#------------------------------------------------------------------------------ #$Date: 2021-10-15 02:06:48 +0300 (Fri, 15 Oct 2021) $ #$Revision: 269960 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/85/7708567.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_7708567 loop_ _publ_author_name 'Kramer, Eric' 'Yu, Shilin' 'Ward, Jas S.' 'Rissanen, Kari' _publ_section_title ; Dihypoiodites Stabilised by 4-ethylpyridine through O-I-N Halogen Bonds ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT03324G _journal_year 2021 _chemical_formula_moiety 'C22 H22 I2 N2 O4' _chemical_formula_sum 'C22 H22 I2 N2 O4' _chemical_formula_weight 632.21 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2021-04-28 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-08-24 deposited with the CCDC. 2021-10-14 downloaded from the CCDC. ; _cell_angle_alpha 84.321(8) _cell_angle_beta 87.332(8) _cell_angle_gamma 71.188(6) _cell_formula_units_Z 2 _cell_length_a 8.0109(5) _cell_length_b 9.0287(6) _cell_length_c 16.548(2) _cell_measurement_reflns_used 3812 _cell_measurement_temperature 120.00(10) _cell_measurement_theta_max 75.0000 _cell_measurement_theta_min 2.6210 _cell_volume 1127.25(18) _computing_cell_refinement 'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 120.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.1977 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -115.00 -13.00 1.00 5.00 -- -41.40 -57.00 30.00 102 2 \w -115.00 -13.00 1.00 5.00 -- -41.40 -57.00 120.00 102 3 \w -70.00 32.00 1.00 5.00 -- -41.40 57.00 -90.00 102 4 \w 6.00 82.00 1.00 5.00 -- 41.40 -99.00 -30.00 76 5 \w 84.00 178.00 1.00 25.00 -- 112.00 30.00 -30.00 94 6 \w 36.00 109.00 1.00 25.00 -- 112.00-111.00 0.00 73 7 \w 40.00 141.00 1.00 25.00 -- 112.00 -61.00-180.00 101 8 \w 36.00 140.00 1.00 25.00 -- 112.00 -30.00 0.00 104 9 \w 29.00 107.00 1.00 25.00 -- 112.00 -94.00 150.00 78 10 \w 103.00 178.00 1.00 25.00 -- 112.00 77.00 -60.00 75 11 \w 36.00 109.00 1.00 25.00 -- 112.00-111.00 60.00 73 12 \w 39.00 138.00 1.00 25.00 -- 112.00 -45.00 -90.00 99 13 \w 36.00 109.00 1.00 25.00 -- 112.00-111.00 -60.00 73 14 \w 59.00 178.00 1.00 25.00 -- 112.00 15.00 -90.00 119 15 \w 61.00 146.00 1.00 25.00 -- 112.00 178.00-180.00 85 16 \w -115.00 -13.00 1.00 5.00 -- -41.40 -57.00 -90.00 102 17 \w -86.00 -6.00 1.00 5.00 -- -41.40 125.00 60.00 80 18 \w -116.00 -17.00 1.00 5.00 -- -41.40 -37.00-180.00 99 19 \w 6.00 32.00 1.00 5.00 -- 41.40 85.00 -95.89 26 20 \w 84.00 178.00 1.00 25.00 -- 112.00 30.00 150.00 94 21 \w 80.00 121.00 1.00 25.00 -- 112.00 73.00 -7.68 41 22 \w 84.00 178.00 1.00 25.00 -- 112.00 30.00 60.00 94 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.1895537000 _diffrn_orient_matrix_UB_12 0.0072678000 _diffrn_orient_matrix_UB_13 -0.0004446000 _diffrn_orient_matrix_UB_21 -0.0067453000 _diffrn_orient_matrix_UB_22 0.0380415000 _diffrn_orient_matrix_UB_23 -0.0928587000 _diffrn_orient_matrix_UB_31 -0.0728556000 _diffrn_orient_matrix_UB_32 0.1767808000 _diffrn_orient_matrix_UB_33 0.0114966000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.1200 _diffrn_reflns_av_unetI/netI 0.1121 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 12079 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.117 _diffrn_reflns_theta_min 2.684 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 22.170 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.27050 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.863 _exptl_crystal_description plate _exptl_crystal_F_000 612 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DCM' _exptl_crystal_size_max 0.173 _exptl_crystal_size_mid 0.059 _exptl_crystal_size_min 0.013 _refine_diff_density_max 2.110 _refine_diff_density_min -1.524 _refine_diff_density_rms 0.276 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 323 _refine_ls_number_reflns 4411 _refine_ls_number_restraints 222 _refine_ls_restrained_S_all 0.989 _refine_ls_R_factor_all 0.1026 _refine_ls_R_factor_gt 0.0818 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1441P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2177 _refine_ls_wR_factor_ref 0.2436 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3134 _reflns_number_total 4411 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt03324g2.cif _cod_data_source_block 2 _cod_original_cell_volume 1127.23(18) _cod_database_code 7708567 _shelxl_version_number 2014/6 _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. ; _reflns_odcompleteness_completeness 99.24 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 71.98 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints N11 \\sim N41 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04 3. Others Sof(C44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=Sof(N41)=Sof(C42)=Sof(H42)= Sof(C43)=Sof(H43)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(C48)=Sof(H48A)=Sof(H48B)= Sof(H48C)=1-FVAR(1) Sof(C14)=Sof(C13)=Sof(H13)=Sof(C12)=Sof(H12)=Sof(N11)=Sof(C16)=Sof(H16)= Sof(C15)=Sof(H15)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)= Sof(H18C)=FVAR(1) 4.a Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C17(H17A,H17B), C47(H47A,H47B) 4.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C5(H5), C6(H6), C13(H13), C12(H12), C16(H16), C15(H15), C22(H22), C24(H24), C25(H25), C26(H26), C45(H45), C46(H46), C42(H42), C43(H43) 4.c Fitted hexagon refined as free rotating group: C14(C13,C12,N11,C16,C15), C44(C45,C46,N41,C42,C43) 4.d Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C18(H18A,H18B,H18C), C48(H48A,H48B,H48C) ; _shelx_res_file ; TITL oie068_a.res in P-1 REM Old TITL OIE068 in P-1 REM SHELXT solution in P-1 REM R1 0.153, Rweak 0.006, Alpha 0.045, Orientation as input REM Formula found by SHELXT: C21 N3 O4 I2 CELL 1.54184 8.0109 9.0287 16.5477 84.321 87.332 71.188 ZERR 2 0.0005 0.0006 0.002 0.008 0.008 0.006 LATT 1 SFAC C H I N O UNIT 44 44 4 4 8 SIMU 0.02 0.04 1.7 N11 N41 C12 C13 C14 C15 C16 C17 C18 C42 C43 C44 C45 C46 = C47 C48 L.S. 4 PLAN 20 BOND $H list 4 fmap 2 53 acta SHEL 50 0.81 REM REM REM WGHT 0.144100 FVAR 0.29937 0.67626 I1 3 0.496996 0.589791 0.862937 11.00000 0.04288 0.04947 = 0.05834 -0.02060 -0.00215 -0.01536 I2 3 0.397202 -0.213332 0.531776 11.00000 0.03797 0.04625 = 0.05045 -0.01098 -0.00337 -0.01340 O28 5 0.585692 0.369901 0.806795 11.00000 0.03645 0.04936 = 0.09420 -0.03909 0.00305 -0.00524 O29 5 0.861243 0.314310 0.848865 11.00000 0.04514 0.05423 = 0.06308 -0.01426 0.00361 -0.02533 O31 5 0.605439 -0.166927 0.594882 11.00000 0.04050 0.04884 = 0.05800 -0.01574 -0.00978 -0.01514 O32 5 0.401349 -0.004039 0.670311 11.00000 0.04757 0.05814 = 0.06375 -0.02353 0.00001 -0.01755 N1 4 0.383774 0.826200 0.916874 11.00000 0.04298 0.04805 = 0.04659 -0.00640 0.00022 -0.02038 C2 1 0.290680 0.840077 0.985568 11.00000 0.04604 0.04722 = 0.05450 -0.00886 -0.00185 -0.02237 AFIX 43 H2 2 0.274070 0.751077 1.013350 11.00000 -1.20000 AFIX 0 C3 1 0.216637 0.985655 1.017369 11.00000 0.04968 0.05351 = 0.04211 -0.00261 -0.00231 -0.02134 AFIX 43 H3 2 0.154098 0.991790 1.066377 11.00000 -1.20000 AFIX 0 C4 1 0.235648 1.117988 0.977031 11.00000 0.04265 0.04423 = 0.04899 -0.00459 -0.01887 -0.01073 C5 1 0.331942 1.103937 0.906548 11.00000 0.06349 0.04454 = 0.05207 0.00436 -0.01560 -0.01745 AFIX 43 H5 2 0.350702 1.191636 0.878308 11.00000 -1.20000 AFIX 0 C6 1 0.402333 0.955922 0.877124 11.00000 0.04485 0.05367 = 0.04962 -0.01152 0.00660 -0.00984 AFIX 43 H6 2 0.464419 0.947735 0.827972 11.00000 -1.20000 AFIX 0 C7 1 0.154942 1.280744 1.007264 11.00000 0.05341 0.04500 = 0.06324 -0.01015 -0.02160 -0.00881 AFIX 23 H7A 2 0.242872 1.334090 1.001166 11.00000 -1.20000 H7B 2 0.057488 1.340123 0.972380 11.00000 -1.20000 AFIX 0 C8 1 0.088484 1.284959 1.093997 11.00000 0.04635 0.05089 = 0.06635 -0.01443 -0.00746 -0.00681 AFIX 137 H8A 2 -0.011753 1.248249 1.099170 11.00000 -1.50000 H8B 2 0.054751 1.390755 1.109028 11.00000 -1.50000 H8C 2 0.180122 1.218556 1.129040 11.00000 -1.50000 AFIX 66 PART 1 C14 1 -0.047690 -0.380485 0.391462 21.00000 0.03776 0.04877 = 0.04773 -0.00834 0.00050 -0.01462 C13 1 0.131869 -0.449209 0.377128 21.00000 0.03853 0.04971 = 0.04499 -0.01771 0.00795 -0.00983 AFIX 43 H13 2 0.170955 -0.529679 0.342901 21.00000 -1.20000 AFIX 65 C12 1 0.253008 -0.397660 0.413950 21.00000 0.03612 0.03515 = 0.04930 -0.01363 0.00682 -0.01643 AFIX 43 H12 2 0.373145 -0.443641 0.404359 21.00000 -1.20000 AFIX 65 N11 4 0.194590 -0.277387 0.465106 21.00000 0.03993 0.03934 = 0.05048 -0.01021 -0.00121 -0.01450 C16 1 0.015032 -0.208663 0.479440 21.00000 0.03750 0.04717 = 0.05338 -0.00942 -0.00850 -0.01046 AFIX 43 H16 2 -0.024053 -0.128192 0.513667 21.00000 -1.20000 AFIX 65 C15 1 -0.106109 -0.260210 0.442619 21.00000 0.03579 0.05155 = 0.05155 -0.00726 0.00913 -0.01148 AFIX 43 H15 2 -0.226246 -0.214229 0.452210 21.00000 -1.20000 AFIX 0 C17 1 -0.184953 -0.438309 0.356509 21.00000 0.04393 0.04929 = 0.06129 -0.00332 0.00047 -0.02103 AFIX 23 H17A 2 -0.174707 -0.542675 0.381415 21.00000 -1.20000 H17B 2 -0.302048 -0.369012 0.368697 21.00000 -1.20000 AFIX 0 C18 1 -0.159871 -0.442806 0.265490 21.00000 0.05278 0.07841 = 0.07149 -0.01643 -0.01276 -0.03740 AFIX 137 H18A 2 -0.250312 -0.475604 0.244049 21.00000 -1.50000 H18B 2 -0.046334 -0.515653 0.253613 21.00000 -1.50000 H18C 2 -0.167051 -0.340013 0.241057 21.00000 -1.50000 AFIX 0 PART 0 C21 1 0.793582 0.142398 0.765144 11.00000 0.04622 0.04774 = 0.04817 -0.01265 0.00278 -0.02105 C22 1 0.659682 0.103297 0.729945 11.00000 0.03336 0.04298 = 0.04909 -0.00090 0.00054 -0.01176 AFIX 43 H22 2 0.542262 0.164128 0.735856 11.00000 -1.20000 AFIX 0 C23 1 0.705280 -0.028991 0.685635 11.00000 0.03955 0.03329 = 0.03889 -0.00216 -0.00344 -0.00531 C24 1 0.878010 -0.121559 0.677325 11.00000 0.04136 0.04859 = 0.05111 -0.01489 0.00306 -0.02014 AFIX 43 H24 2 0.905659 -0.210804 0.649173 11.00000 -1.20000 AFIX 0 C25 1 1.013489 -0.080294 0.711840 11.00000 0.03172 0.06260 = 0.05900 -0.02447 0.00417 -0.01158 AFIX 43 H25 2 1.130960 -0.140773 0.705658 11.00000 -1.20000 AFIX 0 C26 1 0.968235 0.053160 0.755546 11.00000 0.03717 0.05470 = 0.06395 -0.00870 -0.00495 -0.02140 AFIX 43 H26 2 1.056334 0.081638 0.778160 11.00000 -1.20000 AFIX 0 C27 1 0.753041 0.285401 0.812187 11.00000 0.04516 0.05491 = 0.05329 -0.01993 0.01286 -0.02106 C30 1 0.552331 -0.072315 0.648019 11.00000 0.02806 0.04113 = 0.03781 0.00682 0.00925 -0.00388 PART 2 AFIX 66 C44 1 -0.012816 -0.366393 0.353220 -21.00000 0.04446 0.04668 = 0.05018 -0.01300 0.00582 -0.01076 C45 1 -0.082915 -0.256822 0.409360 -21.00000 0.03464 0.05051 = 0.05121 -0.00528 -0.00149 -0.01273 AFIX 43 H45 2 -0.204235 -0.208414 0.412937 -21.00000 -1.20000 AFIX 65 C46 1 0.028313 -0.219601 0.460154 -21.00000 0.03441 0.03934 = 0.04567 -0.01452 0.00517 -0.01019 AFIX 43 H46 2 -0.018589 -0.146291 0.497715 -21.00000 -1.20000 AFIX 65 N41 4 0.209640 -0.291952 0.454808 -21.00000 0.03153 0.03533 = 0.05799 -0.00707 -0.00411 -0.02350 C42 1 0.279741 -0.401523 0.398669 -21.00000 0.04242 0.04051 = 0.05709 -0.00563 0.00207 -0.01339 AFIX 43 H42 2 0.401062 -0.449930 0.395092 -21.00000 -1.20000 AFIX 65 C43 1 0.168516 -0.438745 0.347874 -21.00000 0.04306 0.04304 = 0.04286 -0.02350 0.00295 -0.01420 AFIX 43 H43 2 0.215418 -0.512056 0.310313 -21.00000 -1.20000 AFIX 0 C47 1 -0.132959 -0.405921 0.298689 -21.00000 0.03745 0.05615 = 0.05919 -0.01419 -0.00991 -0.02867 AFIX 23 H47A 2 -0.206176 -0.309823 0.269819 -21.00000 -1.20000 H47B 2 -0.062364 -0.472207 0.258710 -21.00000 -1.20000 AFIX 0 C48 1 -0.246877 -0.486499 0.342037 -21.00000 0.04809 0.06329 = 0.06353 -0.02390 -0.01929 -0.02946 AFIX 137 H48A 2 -0.274291 -0.553496 0.306796 -21.00000 -1.50000 H48B 2 -0.353959 -0.410250 0.358809 -21.00000 -1.50000 H48C 2 -0.187129 -0.548622 0.388950 -21.00000 -1.50000 AFIX 0 HKLF 4 REM oie068_a.res in P-1 REM R1 = 0.0818 for 3134 Fo > 4sig(Fo) and 0.1026 for all 4411 data REM 323 parameters refined using 222 restraints END WGHT 0.1441 0.0000 REM Highest difference peak 2.110, deepest hole -1.524, 1-sigma level 0.276 Q1 1 0.3831 -0.2229 0.5922 11.00000 0.05 2.11 Q2 1 0.4072 -0.1990 0.4634 11.00000 0.05 1.99 Q3 1 0.1367 -0.2073 0.5248 11.00000 0.05 1.97 Q4 1 0.2407 -0.2210 0.5384 11.00000 0.05 1.96 Q5 1 0.6352 0.5825 0.8593 11.00000 0.05 1.95 Q6 1 0.6571 -0.2197 0.5345 11.00000 0.05 1.91 Q7 1 0.2249 1.4057 1.1367 11.00000 0.05 1.86 Q8 1 0.5066 0.6052 0.8005 11.00000 0.05 1.83 Q9 1 0.2533 0.5950 0.8598 11.00000 0.05 1.82 Q10 1 0.5224 -0.2367 0.5267 11.00000 0.05 1.81 Q11 1 0.3359 0.5850 0.8675 11.00000 0.05 1.77 Q12 1 -0.1082 1.4118 1.1359 11.00000 0.05 1.72 Q13 1 0.4775 0.5754 0.9309 11.00000 0.05 1.72 Q14 1 -0.0098 -0.2205 0.5365 11.00000 0.05 1.70 Q15 1 -0.0058 1.4063 1.1415 11.00000 0.05 1.63 Q16 1 -0.1637 -0.2140 0.5297 11.00000 0.05 1.56 Q17 1 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7 -3 98.35 13.49 -2 -7 3 82.48 31.07 2 7 -3 95.31 42.61 2 7 -3 116.77 23.28 2 7 -3 103.68 21.75 2 7 -2 63.27 10.44 2 7 -2 45.51 14.01 -2 -7 2 87.13 30.45 2 7 -2 21.08 20.00 2 7 -2 37.67 12.10 2 7 -2 49.37 16.59 2 7 -1 -1.03 4.27 2 7 -1 0.93 2.57 -2 -7 1 -4.49 6.93 2 7 -1 10.29 15.81 2 7 -1 -0.72 4.79 2 7 -1 4.09 5.17 2 7 0 -5.78 4.76 2 7 0 -0.63 2.69 2 7 0 5.59 5.27 2 7 0 1.47 3.02 2 7 0 -0.57 6.79 2 7 1 210.43 47.12 2 7 1 167.26 16.88 2 7 1 124.89 20.86 2 7 1 158.40 24.34 2 7 1 193.55 25.61 2 7 2 18.26 16.31 2 7 2 8.78 4.06 2 7 2 10.07 5.09 2 7 2 8.32 5.36 2 7 2 14.80 7.59 2 7 3 41.18 10.58 2 7 3 68.79 29.08 2 7 3 45.17 8.76 -2 -7 -3 17.91 19.19 2 7 3 23.90 8.09 2 7 3 34.96 10.32 2 7 4 575.42 32.12 -2 -7 -4 423.04 80.06 2 7 4 532.55 37.03 2 7 4 516.21 43.78 2 7 4 586.64 45.26 2 7 5 14.70 5.98 2 7 5 14.14 5.50 -2 -7 -5 -3.52 11.64 2 7 5 0.70 4.23 2 7 5 8.60 5.87 2 7 6 285.86 23.81 -2 -7 -6 259.42 67.99 2 7 6 320.15 34.60 2 7 7 204.74 19.99 -2 -7 -7 247.75 68.99 2 7 7 297.40 33.87 2 7 8 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28.08 9.50 4 5 -13 32.13 7.63 -4 -5 13 28.17 16.00 4 5 -13 13.70 7.48 4 5 -12 12.62 7.79 -4 -5 12 26.92 15.74 4 5 -12 14.98 8.61 4 5 -12 27.38 12.12 -4 -5 11 48.14 20.19 4 5 -11 77.42 21.37 4 5 -11 77.74 17.72 -4 -5 10 8.21 11.49 4 5 -10 3.66 6.37 -4 -5 9 17.30 14.16 4 5 -9 28.68 14.02 -4 -5 8 59.26 26.70 -4 -5 8 30.48 14.83 4 5 -8 45.12 14.87 -4 -5 7 139.09 42.47 -4 -5 7 123.96 29.74 4 5 -7 103.46 22.14 -4 -5 6 20.72 13.34 4 5 -6 61.53 15.19 -4 -5 5 4.55 11.95 4 5 -5 12.26 9.15 -4 -5 4 384.16 65.48 -4 -5 3 46.88 23.08 -4 -5 2 486.98 67.83 4 5 -2 512.55 57.92 4 5 -1 1174.08 86.48 -4 -5 1 1159.99 97.93 4 5 0 -0.91 5.97 -4 -5 0 5.65 8.24 4 5 1 341.34 47.54 -4 -5 -1 376.86 50.50 4 5 2 284.44 43.93 -4 -5 -2 285.03 42.23 4 5 3 88.36 25.48 -4 -5 -3 101.56 24.64 4 5 4 663.77 73.83 -4 -5 -5 71.22 29.72 4 5 5 30.30 17.85 -4 -5 -6 57.40 25.50 4 5 6 96.69 32.01 -4 -5 -7 178.84 53.54 4 5 7 199.60 48.76 4 5 8 200.25 19.76 -4 -5 -8 172.78 56.22 -4 -5 -8 209.68 17.10 4 5 9 24.33 7.33 -4 -5 -9 59.49 34.33 4 5 9 43.76 23.20 -4 -5 -9 39.18 8.16 4 5 10 30.91 8.19 -4 -5 -10 32.46 27.06 4 5 10 10.68 14.40 -4 -5 -10 25.12 7.09 -4 -5 -11 122.53 15.03 4 5 11 205.85 20.40 -4 -5 -12 71.49 11.82 4 5 12 83.92 13.01 -4 -5 -13 8.43 3.94 4 5 13 8.91 4.26 -4 -5 -14 275.78 21.97 4 5 14 263.89 20.46 4 5 15 5.08 2.51 -4 -5 -15 4.36 2.64 4 5 15 6.81 3.21 4 5 16 34.07 5.17 -4 -5 -16 46.33 7.73 4 5 16 35.22 6.16 -4 -5 -17 89.12 9.59 4 5 17 72.09 7.55 -4 -5 -18 -0.36 0.95 4 5 18 1.92 1.38 4 5 18 -1.69 1.64 4 6 -15 45.33 6.38 -4 -6 15 14.33 5.81 4 6 -14 -1.90 2.06 -4 -6 14 -3.14 4.86 4 6 -13 29.18 6.51 -4 -6 13 2.28 4.63 4 6 -12 60.67 9.72 -4 -6 12 37.62 15.29 4 6 -12 25.02 10.67 4 6 -12 40.22 13.82 4 6 -11 7.77 4.82 4 6 -11 -4.45 6.25 4 6 -11 8.13 5.85 -4 -6 10 49.72 21.05 4 6 -10 44.00 16.65 4 6 -10 53.77 16.28 -4 -6 9 21.91 12.00 4 6 -9 40.01 15.39 4 6 -9 37.17 15.13 -4 -6 8 8.56 10.54 4 6 -8 23.84 13.14 -4 -6 7 110.77 29.89 4 6 -7 147.72 25.25 -4 -6 6 1.15 3.93 -4 -6 6 20.10 12.89 4 6 -6 10.59 8.59 -4 -6 5 30.05 19.53 4 6 -5 57.69 16.07 -4 -6 4 310.79 60.30 4 6 -4 329.65 32.93 -4 -6 3 56.21 26.35 4 6 -3 25.32 10.46 -4 -6 2 41.45 20.65 4 6 -2 17.30 7.62 4 6 -1 21.08 12.12 -4 -6 1 22.65 14.27 4 6 0 525.73 65.82 -4 -6 0 533.49 66.85 -4 -6 -1 15.27 11.00 4 6 1 8.04 9.51 4 6 2 83.34 26.85 4 6 3 498.49 66.29 4 6 4 1.65 6.01 4 6 4 2.75 2.43 4 6 4 1.94 3.10 4 6 5 470.02 29.81 4 6 5 430.95 37.06 4 6 6 393.50 66.73 4 6 6 308.57 25.07 -4 -6 -6 290.66 69.84 4 6 6 375.14 35.47 4 6 7 32.83 8.24 4 6 7 62.91 28.51 -4 -6 -7 4.74 11.26 4 6 7 38.01 12.47 4 6 8 203.99 19.70 4 6 8 313.66 65.91 -4 -6 -8 236.73 68.27 4 6 8 280.37 31.77 4 6 9 51.19 10.23 4 6 9 143.42 23.68 4 6 10 15.50 5.82 4 6 11 243.13 22.68 4 6 11 219.01 20.39 4 6 12 8.45 3.84 -4 -6 -12 8.28 3.99 4 6 12 9.67 4.62 4 6 13 6.56 3.72 -4 -6 -13 5.23 2.93 4 6 13 6.90 3.64 4 6 14 34.44 6.64 -4 -6 -14 30.59 6.71 4 6 14 36.99 7.39 4 6 15 84.30 8.78 -4 -6 -15 97.38 10.95 4 6 15 87.27 10.06 4 6 15 61.75 11.94 4 6 16 0.99 1.00 -4 -6 -16 0.65 1.55 4 6 16 1.15 1.20 4 6 16 4.71 2.23 -4 -6 -17 0.22 0.69 4 6 17 -0.15 0.85 4 6 17 -2.38 2.50 4 6 18 53.58 4.58 4 6 18 35.78 5.18 4 7 -14 1.77 1.36 4 7 -13 17.56 4.31 4 7 -12 1.84 1.80 4 7 -12 5.04 4.95 4 7 -11 16.75 5.21 -4 -7 11 11.64 4.60 4 7 -11 18.90 9.26 4 7 -11 10.31 6.70 4 7 -10 6.26 3.88 -4 -7 10 7.43 8.32 4 7 -10 -6.36 6.46 4 7 -10 2.38 5.52 4 7 -9 34.70 7.93 4 7 -9 33.50 9.34 -4 -7 9 5.97 8.23 4 7 -9 4.45 4.95 4 7 -9 15.03 8.93 4 7 -8 32.93 8.83 4 7 -8 41.71 12.07 -4 -7 8 21.25 13.13 4 7 -8 16.82 9.82 4 7 -8 23.24 10.38 4 7 -7 21.98 11.64 -4 -7 7 10.73 10.36 4 7 -7 5.03 5.32 4 7 -7 15.70 8.70 -4 -7 6 100.15 24.94 4 7 -6 119.27 22.69 4 7 -6 103.18 21.70 4 7 -5 65.47 18.56 -4 -7 5 71.05 23.63 4 7 -5 51.48 14.07 4 7 -5 51.93 14.34 4 7 -4 105.36 26.58 4 7 -4 47.79 13.56 -4 -7 3 496.49 76.58 4 7 -3 490.65 50.67 4 7 -3 394.25 35.60 -4 -7 2 9.18 12.11 4 7 -2 24.08 11.52 4 7 -2 10.39 6.32 -4 -7 1 97.56 31.84 4 7 -1 125.42 26.27 4 7 -1 65.33 14.16 4 7 0 233.28 49.19 4 7 0 189.52 16.94 4 7 0 267.92 33.29 4 7 0 210.34 24.16 4 7 1 16.65 12.53 4 7 1 19.23 6.40 4 7 1 22.36 9.74 4 7 1 15.50 7.21 4 7 1 14.32 7.58 4 7 2 312.14 57.30 4 7 2 227.72 19.54 4 7 2 252.91 28.51 4 7 2 220.99 25.60 4 7 2 224.26 27.60 4 7 3 87.68 30.72 4 7 3 84.12 12.14 4 7 3 122.76 18.45 4 7 3 105.65 18.40 4 7 3 122.23 19.39 4 7 4 87.60 12.82 4 7 4 66.63 13.02 4 7 4 74.84 15.59 4 7 5 0.51 8.77 4 7 5 3.50 1.99 -4 -7 -5 13.22 16.08 4 7 5 5.79 2.85 4 7 6 92.29 13.69 4 7 6 65.87 15.74 4 7 7 38.86 9.52 4 7 7 47.39 13.80 4 7 8 10.29 5.28 4 7 8 14.94 5.45 4 7 8 17.20 8.63 4 7 9 219.99 21.59 4 7 9 213.15 28.54 4 7 10 56.37 10.60 4 7 10 23.46 6.33 4 7 10 39.47 12.41 4 7 11 10.08 4.23 4 7 11 8.26 4.05 4 7 11 1.72 3.32 4 7 12 310.69 21.59 4 7 12 243.52 18.88 4 7 13 5.86 3.05 4 7 13 7.21 3.04 4 7 13 3.39 2.46 4 7 14 22.76 4.77 4 7 14 21.97 4.94 4 7 14 13.40 5.79 4 7 15 123.26 8.92 4 7 15 114.72 9.88 4 7 15 103.78 13.22 4 7 16 2.70 1.46 4 7 16 0.73 1.33 4 7 17 19.32 2.83 4 8 -12 25.17 4.35 4 8 -11 19.87 4.64 4 8 -10 14.50 4.51 4 8 -10 -5.82 6.44 4 8 -9 11.75 7.22 4 8 -9 26.96 8.77 4 8 -8 6.20 3.34 4 8 -8 1.97 3.57 4 8 -8 -5.21 6.50 4 8 -8 1.77 4.57 4 8 -7 32.68 8.93 4 8 -7 41.28 12.20 4 8 -7 5.06 7.20 4 8 -7 14.11 7.01 4 8 -6 85.74 12.51 4 8 -6 50.64 14.45 4 8 -6 36.39 13.35 4 8 -6 84.64 18.26 4 8 -5 3.72 4.54 4 8 -5 1.82 4.00 4 8 -5 4.26 7.70 4 8 -4 6.93 9.92 4 8 -4 -1.49 2.86 4 8 -4 -3.07 4.17 4 8 -3 7.45 9.20 4 8 -3 7.85 4.98 4 8 -3 6.69 3.54 4 8 -2 117.71 18.84 4 8 -2 130.18 25.00 4 8 -2 88.65 18.69 4 8 -1 3.16 3.17 4 8 -1 -1.39 3.48 4 8 -1 1.46 3.38 4 8 0 17.19 6.04 4 8 0 14.37 8.67 4 8 0 6.90 4.06 4 8 0 4.21 5.10 4 8 1 100.73 13.38 4 8 1 109.12 19.99 4 8 1 76.04 15.16 4 8 1 61.01 14.44 4 8 2 23.30 7.09 4 8 2 23.81 9.47 4 8 2 13.01 7.45 4 8 2 20.57 8.78 4 8 2 18.98 8.10 4 8 3 134.76 16.10 4 8 3 76.48 16.32 4 8 3 97.52 17.44 4 8 3 106.42 19.77 4 8 3 109.46 17.80 4 8 4 116.98 15.35 4 8 4 119.98 17.32 4 8 4 126.60 19.33 4 8 4 130.74 20.69 4 8 5 46.18 9.90 4 8 5 28.34 9.61 4 8 5 32.01 10.12 4 8 6 278.77 24.03 4 8 6 257.08 29.04 4 8 6 257.72 28.81 4 8 7 78.43 12.75 4 8 7 80.85 16.65 4 8 7 103.11 17.85 4 8 8 4.55 4.48 4 8 8 3.50 2.47 4 8 8 2.25 4.21 4 8 9 210.98 20.06 4 8 9 169.82 21.49 4 8 9 200.74 25.11 4 8 10 7.81 3.82 4 8 10 3.15 2.11 4 8 10 0.53 2.56 4 8 11 4.34 2.16 4 8 11 6.02 3.07 4 8 11 7.45 5.48 4 8 12 66.34 8.77 4 8 12 52.69 7.57 4 8 12 53.72 11.21 4 8 13 70.66 8.02 4 8 13 56.72 9.97 4 8 14 0.62 0.69 4 8 14 0.91 1.45 4 8 14 -1.61 2.02 4 8 15 0.11 0.60 4 9 -8 32.74 8.44 4 9 -8 16.33 7.38 4 9 -7 33.71 9.16 4 9 -7 7.62 5.09 4 9 -6 4.33 6.65 4 9 -6 -5.79 4.64 4 9 -5 129.03 21.05 4 9 -5 52.48 14.25 4 9 -4 19.05 8.95 4 9 -4 19.19 8.99 4 9 -3 32.43 14.54 4 9 -3 -2.76 6.12 4 9 -2 73.93 18.67 4 9 -2 87.48 11.67 4 9 -2 53.95 14.10 4 9 -1 3.71 3.23 4 9 -1 11.44 10.08 4 9 -1 6.64 6.50 4 9 0 74.00 11.63 4 9 0 78.54 18.38 4 9 0 34.92 11.18 4 9 1 68.53 10.86 4 9 1 81.51 17.25 4 9 1 67.51 15.74 4 9 2 186.17 18.41 4 9 2 158.84 22.30 4 9 3 14.62 4.94 4 9 3 11.09 5.54 4 9 4 31.10 7.91 4 9 4 13.18 5.75 4 9 4 11.17 9.29 4 9 5 140.05 16.05 4 9 5 99.11 16.15 4 9 5 115.48 19.70 4 9 5 92.12 14.04 4 9 6 29.29 7.46 4 9 6 15.22 6.51 4 9 6 29.28 9.59 4 9 7 70.75 12.89 4 9 7 80.03 14.69 4 9 8 67.92 10.71 4 9 8 51.41 10.50 4 9 8 52.73 12.02 4 9 9 -1.71 2.64 4 9 9 0.77 2.70 4 9 9 2.27 2.58 4 9 10 246.39 18.07 4 9 11 23.35 5.00 4 9 12 4.40 2.22 4 9 13 106.19 7.43 4 10 -6 11.50 4.91 4 10 -5 -0.77 3.11 4 10 -5 11.23 6.43 4 10 -4 48.18 11.91 4 10 -4 23.09 7.94 4 10 -3 -0.36 3.96 4 10 -3 0.45 2.72 4 10 -2 7.04 7.96 4 10 -2 -1.28 4.39 4 10 -1 85.33 10.49 4 10 -1 53.52 13.73 4 10 -1 45.33 12.98 4 10 0 -3.71 2.85 4 10 0 3.84 4.97 4 10 1 18.08 5.59 4 10 1 13.74 8.00 4 10 2 86.89 11.32 4 10 2 73.90 14.35 4 10 3 7.44 4.00 4 10 3 6.91 4.28 4 10 4 94.86 12.32 4 10 4 59.86 10.74 4 10 5 57.63 9.61 4 10 6 -1.60 2.11 4 10 7 55.44 8.84 4 10 8 0.89 1.54 4 10 9 13.51 3.98 4 10 10 12.74 3.22 4 10 11 16.11 2.98 4 11 -3 2.84 2.84 4 11 -2 4.55 4.45 4 11 -1 9.97 5.11 4 11 0 24.87 7.33 4 11 1 1.61 1.91 4 11 2 -0.79 1.93 4 11 2 4.67 2.24 4 11 3 49.30 7.30 4 11 4 0.61 1.02 4 11 5 25.74 5.24 4 11 6 27.47 4.88 4 11 7 4.56 1.78 -5 7 5 39.99 6.90 -5 7 4 -2.02 2.62 -5 7 3 8.33 3.76 -5 7 2 49.22 8.54 -5 7 1 1.55 2.04 -5 7 0 53.11 9.17 -5 7 -1 31.19 6.98 -5 7 -2 -2.12 3.02 -5 7 -3 63.45 9.77 -5 7 -4 7.62 3.32 -5 7 -5 1.56 1.74 -5 6 9 5.29 2.07 -5 6 8 104.23 9.90 -5 6 7 4.37 2.59 -5 6 7 7.14 4.14 -5 6 6 26.12 6.45 -5 6 5 51.78 9.38 -5 6 4 11.88 4.76 -5 6 3 50.22 9.71 -5 6 2 9.03 4.56 -5 6 1 17.86 5.59 -5 6 0 26.51 7.13 -5 6 -1 10.43 4.40 -5 6 -2 29.92 7.97 -5 6 -3 0.78 2.72 -5 6 -4 97.26 14.57 -5 6 -5 14.75 5.83 -5 6 -6 4.76 3.06 -5 6 -7 36.10 7.91 -5 6 -8 11.88 4.24 -5 6 -9 10.74 3.18 -5 5 13 3.13 1.47 -5 5 12 -1.07 1.68 -5 5 11 37.78 5.91 -5 5 10 16.70 4.67 -5 5 9 5.22 3.40 -5 5 8 2.13 3.21 -5 5 8 0.48 3.02 -5 5 7 120.22 15.18 -5 5 7 104.66 13.81 -5 5 6 -2.63 2.29 -5 5 6 -1.58 3.18 -5 5 5 8.34 4.35 -5 5 5 13.82 6.47 -5 5 4 107.49 14.89 -5 5 4 82.61 14.23 -5 5 3 0.33 1.91 -5 5 3 -7.19 3.31 -5 5 2 74.35 16.10 -5 5 2 79.29 13.20 -5 5 1 129.11 21.26 -5 5 1 131.01 17.08 -5 5 0 1.63 3.45 -5 5 0 4.01 4.95 -5 5 -1 178.75 25.48 -5 5 -1 171.96 20.16 -5 5 -2 31.17 8.86 -5 5 -2 24.19 8.85 -5 5 -3 -0.59 2.27 -5 5 -3 0.48 3.54 -5 5 -4 37.12 10.01 -5 5 -4 24.02 9.22 -5 5 -5 5.62 4.31 -5 5 -6 -2.38 3.36 -5 5 -7 22.29 7.69 -5 5 -8 29.78 8.86 -5 5 -9 3.44 3.53 -5 5 -10 2.57 2.98 -5 5 -11 42.13 7.14 -5 4 14 2.70 1.40 -5 4 13 98.73 9.29 -5 4 12 18.69 4.66 -5 4 11 7.66 3.72 -5 4 10 246.89 20.48 -5 4 9 -2.83 3.54 -5 4 9 4.12 3.03 -5 4 8 11.73 5.34 -5 4 8 15.49 6.10 -5 4 7 168.00 18.29 -5 4 7 103.24 16.43 -5 4 6 24.22 8.55 -5 4 6 30.97 7.90 -5 4 5 34.92 7.93 -5 4 4 34.88 8.68 -5 4 4 34.43 10.28 -5 4 3 37.34 9.02 -5 4 3 40.43 11.63 -5 4 2 22.21 6.96 -5 4 2 22.38 8.53 -5 4 1 15.36 5.31 -5 4 1 16.22 6.69 -5 4 0 135.56 21.16 -5 4 0 121.29 16.44 -5 4 -1 0.99 3.05 -5 4 -1 3.35 3.54 -5 4 -2 178.67 25.58 -5 4 -2 166.08 20.19 -5 4 -3 92.68 17.94 -5 4 -3 81.15 14.64 -5 4 -4 2.53 2.70 -5 4 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206.08 38.76 8 6 4 239.86 34.79 8 6 4 271.01 26.15 -8 -6 -5 4.89 2.28 8 6 5 8.87 6.75 -8 -6 -5 13.59 12.11 8 6 5 7.45 3.80 -8 -6 -6 8.35 2.68 8 6 6 1.67 3.67 -8 -6 -6 7.60 7.65 8 6 6 4.14 3.05 8 6 7 110.16 11.04 -8 -6 -7 141.22 12.09 -8 -6 -7 113.54 26.76 8 6 7 113.05 16.04 -8 -6 -8 11.63 3.62 8 6 8 6.62 3.03 -8 -6 -8 17.05 4.29 8 6 8 6.56 5.69 -8 -6 -8 15.40 10.11 8 6 8 7.55 3.78 -8 -6 -9 3.27 1.69 8 6 9 6.57 3.03 -8 -6 -9 6.08 2.35 8 6 9 1.43 2.37 -8 -6 -9 2.27 5.52 8 6 9 0.96 2.48 8 6 10 17.97 3.85 -8 -6 -10 16.52 3.64 -8 -6 -10 27.93 5.49 8 6 10 20.90 5.66 8 6 11 26.20 3.98 -8 -6 -11 32.77 4.52 -8 -6 -11 35.45 5.68 8 6 11 18.49 4.33 8 6 12 9.37 2.10 8 7 -8 1.39 0.90 -8 -7 8 6.42 4.48 8 7 -8 3.30 2.43 -8 -7 7 21.07 9.02 8 7 -7 34.23 7.70 8 7 -6 -0.77 2.87 -8 -7 6 2.14 3.99 8 7 -6 -0.17 2.25 -8 -7 5 13.52 7.97 8 7 -5 25.21 7.34 -8 -7 4 51.35 14.94 -8 -7 4 27.73 9.47 8 7 -4 71.38 13.07 -8 -7 3 -3.45 5.18 -8 -7 3 1.22 3.28 8 7 -3 -3.33 4.45 -8 -7 2 45.36 13.86 8 7 -2 91.52 14.71 -8 -7 1 9.11 8.48 8 7 -1 18.45 7.14 8 7 0 4.50 5.31 -8 -7 0 2.11 5.09 8 7 0 0.69 3.89 8 7 1 134.53 17.35 8 7 1 91.37 21.26 -8 -7 -1 60.25 17.69 8 7 1 102.19 15.58 8 7 2 3.28 2.66 8 7 2 -4.45 6.50 -8 -7 -2 -2.20 6.40 8 7 2 0.49 2.26 8 7 3 21.32 9.56 -8 -7 -3 11.99 9.96 8 7 3 32.35 8.68 8 7 4 22.85 10.61 -8 -7 -4 12.47 9.48 8 7 4 15.65 5.54 8 7 5 37.75 11.87 -8 -7 -5 40.84 15.15 8 7 5 74.52 12.66 8 7 6 2.20 3.17 -8 -7 -6 10.38 8.02 8 7 6 9.53 4.05 8 7 7 0.74 1.27 -8 -7 -7 -3.28 5.82 8 7 7 0.53 1.93 8 7 8 74.41 7.58 -8 -7 -8 86.22 19.45 8 7 8 60.61 10.11 8 7 9 0.56 0.94 8 7 9 -1.16 1.82 8 7 10 20.67 3.47 -8 -7 -10 10.81 5.70 8 7 10 15.25 4.30 8 8 -6 15.08 4.30 -8 -8 6 0.98 3.23 8 8 -6 8.99 3.72 8 8 -5 -0.26 1.57 -8 -8 5 -3.51 4.38 8 8 -5 -0.58 1.42 8 8 -4 4.90 2.47 -8 -8 4 -3.10 5.04 8 8 -4 0.38 1.52 -8 -8 3 50.12 14.42 -8 -8 3 25.48 7.93 8 8 -3 69.02 11.13 8 8 -3 88.75 13.68 8 8 -2 -4.36 4.94 -8 -8 2 -8.29 8.55 -8 -8 2 -2.21 3.10 8 8 -2 -0.37 1.81 8 8 -1 35.01 8.70 -8 -8 1 23.83 9.95 -8 -8 1 10.51 6.33 8 8 -1 25.17 6.82 -8 -8 0 32.51 10.43 8 8 0 56.37 10.02 8 8 0 66.65 11.44 8 8 1 -1.87 3.55 -8 -8 -1 0.01 4.37 8 8 1 -0.76 1.75 8 8 2 120.08 12.52 8 8 2 105.65 14.47 -8 -8 -3 16.94 10.16 8 8 3 22.43 6.90 -8 -8 -4 -4.75 6.78 8 8 4 -0.75 2.84 -8 -8 -5 36.69 13.00 8 8 5 58.84 10.43 -8 -8 -6 -5.95 5.32 8 8 6 -1.15 2.28 -8 -8 -7 -3.01 4.08 8 8 7 0.10 2.17 -8 -8 -8 12.84 6.62 8 8 8 4.13 2.58 -8 -8 -9 4.61 3.57 8 8 9 9.82 3.19 8 9 -3 1.35 1.90 8 9 -2 -3.89 2.57 8 9 -2 -1.82 1.93 8 9 -1 14.01 4.27 -8 -9 1 12.56 5.42 8 9 -1 18.99 5.09 8 9 0 -3.74 2.49 -8 -9 0 -7.06 5.05 -8 -9 0 3.66 3.69 8 9 0 -0.58 1.54 -8 -9 -1 0.21 5.15 -8 -9 -1 2.50 3.35 8 9 1 10.32 3.74 -8 -9 -2 10.22 7.29 -8 -9 -2 3.89 4.48 8 9 2 5.72 3.34 -8 -9 -3 7.72 5.09 8 9 3 17.65 4.83 -8 -9 -4 2.62 3.90 8 9 4 3.62 2.06 -8 -9 -5 1.31 2.79 8 9 5 0.70 1.04 -8 -9 -6 14.89 6.87 8 9 6 27.36 5.36 -9 1 4 15.37 3.85 -9 1 3 5.68 2.63 -9 1 0 23.69 6.35 -9 1 -1 6.56 3.53 -9 1 -2 0.17 1.69 -9 1 -3 39.41 8.14 -9 1 -4 9.03 4.20 -9 0 6 11.11 2.78 -9 0 5 14.13 3.97 9 0 -5 21.54 6.92 9 0 -4 1.26 3.18 9 0 -3 94.36 15.20 9 0 -2 48.76 10.91 -9 0 1 -0.75 1.80 9 0 -1 -1.65 4.74 -9 0 0 119.81 11.95 -9 0 0 91.08 11.98 -9 0 -1 2.40 2.45 -9 0 -1 2.87 3.00 -9 0 -2 5.74 2.45 -9 0 -2 3.13 2.89 -9 0 -3 46.25 7.29 -9 0 -3 51.86 9.81 -9 0 -4 17.69 4.22 -9 0 -4 20.27 6.05 -9 0 -5 3.08 2.89 -9 0 -6 1.56 2.14 -9 0 -7 24.72 5.74 9 1 -7 -3.34 2.81 -9 -1 6 14.70 3.26 9 1 -6 18.83 6.19 9 1 -5 6.01 4.90 9 1 -4 8.49 5.48 9 1 -3 28.42 7.84 -9 -1 2 32.76 6.52 9 1 -2 22.79 7.61 -9 -1 1 16.03 4.71 -9 -1 1 13.25 4.21 -9 -1 0 8.06 3.55 -9 -1 0 15.67 4.83 -9 -1 -1 92.27 12.27 -9 -1 -1 127.33 13.23 -9 -1 -2 24.98 6.86 9 1 2 27.53 10.04 -9 -1 -2 26.34 5.86 -9 -1 -3 18.75 5.77 -9 -1 -3 26.19 5.70 -9 -1 -4 166.74 17.79 -9 -1 -4 195.06 15.65 -9 -1 -5 11.94 4.85 9 1 5 15.69 7.29 -9 -1 -5 9.38 3.46 -9 -1 -6 29.98 7.40 9 1 6 15.04 7.09 -9 -1 -6 25.22 5.00 -9 -1 -7 42.42 8.34 9 1 7 21.07 7.54 -9 -1 -8 3.14 2.21 9 1 8 -2.82 2.99 9 2 -8 -0.69 1.72 9 2 -7 42.44 9.66 9 2 -6 4.15 4.52 9 2 -5 60.51 12.42 9 2 -4 87.32 15.57 -9 -2 3 -1.18 2.03 9 2 -3 3.32 3.89 9 2 -2 82.23 17.81 -9 -2 2 114.56 11.94 9 2 -1 21.50 10.15 -9 -2 1 10.91 3.71 -9 -2 0 -0.16 1.95 9 2 0 0.69 3.83 -9 -2 0 0.54 1.94 -9 -2 -1 54.74 8.81 9 2 1 40.09 11.92 -9 -2 -1 74.70 9.98 -9 -2 -2 4.38 2.39 9 2 2 5.51 6.60 -9 -2 -2 5.02 2.69 -9 -2 -3 -0.78 2.33 9 2 3 1.70 4.43 -9 -2 -3 0.62 1.83 -9 -2 -4 20.84 5.92 9 2 4 13.91 7.46 -9 -2 -4 22.28 5.74 -9 -2 -5 85.17 11.87 9 2 5 60.68 15.87 -9 -2 -6 -3.80 3.80 9 2 6 1.75 4.17 -9 -2 -6 0.67 1.44 -9 -2 -7 3.16 2.79 9 2 7 -2.99 4.13 -9 -2 -7 4.75 2.25 -9 -2 -8 41.71 7.98 -9 -2 -8 46.28 6.76 -9 -2 -9 0.78 1.29 -9 -2 -9 0.28 0.96 9 2 9 0.99 2.67 9 3 -8 7.90 4.04 9 3 -7 8.13 4.67 9 3 -6 6.64 4.36 9 3 -5 8.04 5.31 9 3 -4 5.10 4.08 -9 -3 3 23.71 5.25 9 3 -3 43.30 13.87 9 3 -3 31.24 8.97 -9 -3 2 0.91 2.02 9 3 -2 1.83 2.49 9 3 -1 63.07 17.18 -9 -3 1 99.33 11.02 9 3 0 38.15 13.50 -9 -3 0 32.91 6.16 9 3 1 16.80 8.46 -9 -3 -1 20.84 5.19 9 3 2 191.78 28.80 -9 -3 -2 275.84 18.56 -9 -3 -3 10.04 3.39 9 3 3 9.38 5.57 -9 -3 -3 8.59 3.77 -9 -3 -4 22.26 6.01 9 3 4 12.94 7.84 -9 -3 -4 35.95 6.78 -9 -3 -5 106.03 12.77 9 3 5 81.93 18.73 -9 -3 -5 124.07 12.61 -9 -3 -6 3.71 2.61 9 3 6 0.84 3.84 -9 -3 -6 5.65 2.22 -9 -3 -7 13.44 4.51 9 3 7 2.24 4.44 -9 -3 -7 16.30 4.42 -9 -3 -8 19.72 5.35 9 3 8 5.45 5.11 -9 -3 -8 17.59 4.18 -9 -3 -9 9.67 3.27 9 3 9 3.60 2.84 -9 -3 -9 8.35 2.81 -9 -3 -10 6.16 2.60 -9 -3 -10 4.42 1.58 9 4 -7 27.63 7.16 9 4 -6 31.61 7.98 -9 -4 5 -6.54 6.27 9 4 -5 3.64 4.30 -9 -4 4 31.71 10.63 9 4 -4 52.68 11.55 -9 -4 3 8.33 2.86 9 4 -3 12.32 10.75 -9 -4 3 18.53 9.08 9 4 -3 7.73 4.05 -9 -4 2 1.16 0.97 9 4 -2 1.54 4.48 -9 -4 2 4.15 4.69 9 4 -2 -0.82 3.23 -9 -4 1 115.11 11.07 9 4 -1 87.62 19.67 -9 -4 1 106.05 21.71 -9 -4 1 51.34 16.44 9 4 -1 89.17 14.29 9 4 0 -4.41 6.89 -9 -4 0 -9.24 7.78 -9 -4 0 4.17 1.66 9 4 1 3.97 3.99 -9 -4 -1 5.45 4.40 -9 -4 -1 5.14 2.64 9 4 2 21.32 10.59 -9 -4 -2 8.34 9.33 -9 -4 -2 25.80 5.24 9 4 3 65.56 17.26 -9 -4 -3 27.83 12.79 9 4 4 16.96 9.60 -9 -4 -4 8.36 7.70 -9 -4 -4 12.18 3.93 -9 -4 -5 -2.36 2.54 9 4 5 4.79 5.89 -9 -4 -5 0.46 1.18 -9 -4 -6 79.70 9.81 -9 -4 -6 92.07 9.91 -9 -4 -7 2.35 1.88 9 4 7 -1.69 4.61 -9 -4 -7 -0.05 1.27 -9 -4 -8 16.95 4.22 9 4 8 10.33 5.83 -9 -4 -8 21.38 4.37 -9 -4 -9 102.50 10.09 -9 -4 -9 97.27 8.83 -9 -4 -10 -0.42 0.68 9 4 10 -1.26 1.98 -9 -5 6 1.76 5.23 -9 -5 5 28.59 9.65 9 5 -5 55.04 9.25 -9 -5 4 15.93 9.63 9 5 -4 0.85 2.87 -9 -5 3 23.02 9.63 9 5 -3 32.47 8.05 -9 -5 2 63.21 7.12 9 5 -2 67.69 17.28 -9 -5 2 67.23 16.95 -9 -5 2 41.91 14.42 9 5 -2 62.24 10.84 -9 -5 1 0.22 1.61 9 5 -1 0.39 6.51 -9 -5 1 -0.17 5.24 9 5 -1 -2.44 3.46 -9 -5 0 83.61 20.42 9 5 0 119.01 23.61 9 5 0 114.64 14.70 -9 -5 -1 21.37 4.44 9 5 1 23.40 9.93 -9 -5 -1 23.50 12.16 9 5 1 24.83 6.64 9 5 2 -0.80 4.24 -9 -5 -2 4.74 7.28 -9 -5 -2 3.49 1.37 9 5 3 79.71 18.00 -9 -5 -3 54.92 16.63 9 5 4 -4.79 5.52 -9 -5 -4 -4.43 5.27 -9 -5 -4 1.20 1.10 9 5 5 2.46 3.71 -9 -5 -5 -0.29 3.46 9 5 6 25.54 9.77 -9 -5 -6 27.93 9.71 -9 -5 -6 35.78 5.56 9 5 7 8.74 6.01 -9 -5 -7 24.51 4.48 9 5 8 4.24 3.48 -9 -5 -8 -3.64 1.88 9 5 9 -1.35 2.06 -9 -5 -9 1.54 1.19 9 6 -6 22.44 4.90 -9 -6 6 4.09 3.57 -9 -6 5 11.16 6.86 -9 -6 4 -7.35 7.05 -9 -6 3 19.06 9.13 -9 -6 2 4.21 5.42 -9 -6 2 0.87 2.54 9 6 -2 -1.85 2.90 -9 -6 1 9.74 6.48 9 6 -1 7.55 3.74 9 6 0 9.68 8.60 -9 -6 0 5.88 6.27 9 6 0 12.50 4.94 9 6 1 31.97 12.27 -9 -6 -1 19.73 9.45 9 6 1 42.95 8.52 9 6 2 21.74 10.64 -9 -6 -2 11.01 8.22 9 6 2 12.80 4.42 -9 -6 -3 1.34 0.88 9 6 3 -4.74 5.42 -9 -6 -3 0.15 4.34 9 6 4 31.60 11.08 -9 -6 -4 27.80 11.19 -9 -6 -5 7.89 2.37 9 6 5 4.59 5.35 -9 -6 -5 7.19 5.60 -9 -6 -6 16.54 3.28 9 6 6 2.53 2.64 -9 -6 -6 13.27 7.64 -9 -6 -7 91.70 7.12 -9 -6 -7 69.12 13.13 9 6 7 59.81 11.57 -9 -7 4 15.97 6.63 9 7 -4 42.15 6.86 9 7 -3 3.75 3.29 -9 -7 3 -2.82 6.06 9 7 -2 32.00 6.35 -9 -7 2 39.88 11.39 -9 -7 2 14.90 6.45 9 7 -2 34.87 6.78 9 7 -1 16.68 4.80 -9 -7 1 11.04 6.03 -9 -7 1 7.11 4.86 9 7 -1 19.34 5.26 9 7 0 2.22 1.78 9 7 0 -0.13 1.38 9 7 1 63.24 9.39 9 7 1 63.98 7.90 -9 -7 -2 -0.11 3.33 9 7 2 -1.29 2.30 9 7 3 1.09 2.98 -9 -7 -3 -4.97 4.72 9 7 3 -1.13 1.82 9 7 4 18.25 7.13 -9 -7 -4 22.27 9.22 9 7 4 30.48 5.94 9 7 5 9.80 5.13 -9 -7 -5 8.91 5.71 9 7 5 17.74 4.32 -9 -7 -6 -1.99 3.05 -9 -8 1 -6.03 5.08 -9 -8 0 23.81 8.59 -9 -8 -1 -2.03 3.07 -9 -8 -1 0.47 2.08 -9 -8 -2 38.01 10.25 -9 -8 -2 17.44 6.43 -9 -8 -3 2.36 2.41 -9 -8 -4 1.05 2.47 10 2 0 -0.48 2.24 10 2 1 52.64 8.31 10 3 -1 13.00 4.46 10 3 0 8.14 3.49 -10 -3 -1 1.24 0.85 10 3 1 -3.49 2.84 -10 -3 -2 112.27 9.07 10 3 2 57.21 8.81 -10 -3 -3 5.86 2.02 -10 -4 -1 1.12 0.70 10 4 1 -8.88 5.00 -10 -4 -2 37.82 4.76 10 4 2 21.98 7.29 -10 -4 -3 23.37 3.68 10 4 3 4.30 4.08 10 5 2 -1.69 2.70 TITL OIE068 in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 8.010927 9.028686 16.547700 84.3209 87.3318 71.1879 ZERR 2.00 0.000491 0.000605 0.002047 0.0080 0.0078 0.0058 LATT 1 SFAC C H N O I UNIT 44.00 44.00 4.00 8.00 4.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 73241 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.637 _oxdiff_exptl_absorpt_empirical_full_min 0.337 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 0.49700(9) 0.58979(9) 0.86294(5) 0.0489(3) Uani 1 1 d . . . . . I2 I 0.39720(9) -0.21333(9) 0.53178(4) 0.0443(3) Uani 1 1 d . . . . . O28 O 0.5857(11) 0.3699(11) 0.8068(7) 0.060(3) Uani 1 1 d . . . . . O29 O 0.8612(11) 0.3143(11) 0.8489(6) 0.051(2) Uani 1 1 d . . . . . O31 O 0.6054(11) -0.1669(10) 0.5949(5) 0.048(2) Uani 1 1 d . . . . . O32 O 0.4013(12) -0.0040(11) 0.6703(6) 0.055(2) Uani 1 1 d . . . . . N1 N 0.3838(13) 0.8262(12) 0.9169(6) 0.044(2) Uani 1 1 d . . . . . C2 C 0.2907(16) 0.8401(15) 0.9856(8) 0.047(3) Uani 1 1 d . . . . . H2 H 0.2741 0.7511 1.0133 0.057 Uiso 1 1 calc R . . . . C3 C 0.2166(16) 0.9857(15) 1.0174(7) 0.047(3) Uani 1 1 d . . . . . H3 H 0.1541 0.9918 1.0664 0.057 Uiso 1 1 calc R . . . . C4 C 0.2356(15) 1.1180(15) 0.9770(8) 0.045(3) Uani 1 1 d . . . . . C5 C 0.3319(19) 1.1039(16) 0.9065(8) 0.053(3) Uani 1 1 d . . . . . H5 H 0.3507 1.1916 0.8783 0.064 Uiso 1 1 calc R . . . . C6 C 0.4023(17) 0.9559(16) 0.8771(8) 0.051(3) Uani 1 1 d . . . . . H6 H 0.4644 0.9477 0.8280 0.061 Uiso 1 1 calc R . . . . C7 C 0.1549(18) 1.2807(16) 1.0073(9) 0.054(3) Uani 1 1 d . . . . . H7A H 0.2429 1.3341 1.0012 0.065 Uiso 1 1 calc R . . . . H7B H 0.0575 1.3401 0.9724 0.065 Uiso 1 1 calc R . . . . C8 C 0.0885(17) 1.2850(16) 1.0940(9) 0.056(3) Uani 1 1 d . . . . . H8A H -0.0118 1.2482 1.0992 0.084 Uiso 1 1 calc GR . . . . H8B H 0.0548 1.3908 1.1090 0.084 Uiso 1 1 calc GR . . . . H8C H 0.1801 1.2186 1.1290 0.084 Uiso 1 1 calc GR . . . . C14 C -0.0477(16) -0.3805(17) 0.3915(11) 0.044(4) Uani 0.68(2) 1 d . U P A 1 C13 C 0.1319(17) -0.4492(17) 0.3771(9) 0.045(4) Uani 0.68(2) 1 d G U P A 1 H13 H 0.1710 -0.5297 0.3429 0.054 Uiso 0.68(2) 1 calc R . P A 1 C12 C 0.2530(15) -0.398(3) 0.4139(11) 0.039(3) Uani 0.68(2) 1 d G U P A 1 H12 H 0.3731 -0.4436 0.4044 0.046 Uiso 0.68(2) 1 calc R . P A 1 N11 N 0.195(2) -0.277(3) 0.4651(13) 0.042(4) Uani 0.68(2) 1 d G U P A 1 C16 C 0.015(2) -0.209(2) 0.4794(12) 0.046(4) Uani 0.68(2) 1 d G U P A 1 H16 H -0.0241 -0.1282 0.5137 0.055 Uiso 0.68(2) 1 calc R . P A 1 C15 C -0.1061(17) -0.2602(18) 0.4426(10) 0.047(4) Uani 0.68(2) 1 d G U P A 1 H15 H -0.2262 -0.2142 0.4522 0.056 Uiso 0.68(2) 1 calc R . P A 1 C17 C -0.185(3) -0.438(2) 0.3565(13) 0.050(4) Uani 0.68(2) 1 d . U P A 1 H17A H -0.1747 -0.5427 0.3814 0.060 Uiso 0.68(2) 1 calc R . P A 1 H17B H -0.3020 -0.3690 0.3687 0.060 Uiso 0.68(2) 1 calc R . P A 1 C18 C -0.160(3) -0.443(3) 0.2655(15) 0.063(5) Uani 0.68(2) 1 d . U P A 1 H18A H -0.2503 -0.4756 0.2440 0.094 Uiso 0.68(2) 1 calc GR . P A 1 H18B H -0.0463 -0.5157 0.2536 0.094 Uiso 0.68(2) 1 calc GR . P A 1 H18C H -0.1671 -0.3400 0.2411 0.094 Uiso 0.68(2) 1 calc GR . P A 1 C21 C 0.7936(16) 0.1424(15) 0.7651(8) 0.045(3) Uani 1 1 d . . . . . C22 C 0.6597(15) 0.1033(14) 0.7299(7) 0.042(2) Uani 1 1 d . . . . . H22 H 0.5423 0.1641 0.7359 0.051 Uiso 1 1 calc R . . . . C23 C 0.7053(15) -0.0290(13) 0.6856(7) 0.039(2) Uani 1 1 d . . . . . C24 C 0.8780(15) -0.1216(15) 0.6773(8) 0.045(3) Uani 1 1 d . . . . . H24 H 0.9057 -0.2108 0.6492 0.054 Uiso 1 1 calc R . . . . C25 C 1.0135(15) -0.0803(16) 0.7118(8) 0.051(3) Uani 1 1 d . . . . . H25 H 1.1310 -0.1408 0.7057 0.061 Uiso 1 1 calc R . . . . C26 C 0.9682(15) 0.0532(16) 0.7555(8) 0.050(3) Uani 1 1 d . . . . . H26 H 1.0563 0.0816 0.7782 0.060 Uiso 1 1 calc R . . . . C27 C 0.7530(16) 0.2854(16) 0.8122(8) 0.049(3) Uani 1 1 d . . . . . C30 C 0.5523(13) -0.0723(13) 0.6480(7) 0.038(2) Uani 1 1 d . . . . . C44 C -0.013(4) -0.366(4) 0.353(2) 0.048(5) Uani 0.32(2) 1 d . U P A 2 C45 C -0.083(4) -0.257(4) 0.409(2) 0.046(5) Uani 0.32(2) 1 d G U P A 2 H45 H -0.2042 -0.2084 0.4129 0.055 Uiso 0.32(2) 1 calc R . P A 2 C46 C 0.028(5) -0.220(5) 0.460(2) 0.040(5) Uani 0.32(2) 1 d G U P A 2 H46 H -0.0186 -0.1463 0.4977 0.048 Uiso 0.32(2) 1 calc R . P A 2 N41 N 0.210(5) -0.292(6) 0.455(3) 0.038(5) Uani 0.32(2) 1 d G U P A 2 C42 C 0.280(3) -0.402(6) 0.399(2) 0.047(6) Uani 0.32(2) 1 d G U P A 2 H42 H 0.4011 -0.4499 0.3951 0.056 Uiso 0.32(2) 1 calc R . P A 2 C43 C 0.169(4) -0.439(4) 0.348(2) 0.042(6) Uani 0.32(2) 1 d G U P A 2 H43 H 0.2154 -0.5121 0.3103 0.050 Uiso 0.32(2) 1 calc R . P A 2 C47 C -0.133(5) -0.406(5) 0.299(3) 0.047(6) Uani 0.32(2) 1 d . U P A 2 H47A H -0.2062 -0.3098 0.2698 0.056 Uiso 0.32(2) 1 calc R . P A 2 H47B H -0.0624 -0.4722 0.2587 0.056 Uiso 0.32(2) 1 calc R . P A 2 C48 C -0.247(5) -0.486(5) 0.342(3) 0.054(8) Uani 0.32(2) 1 d . U P A 2 H48A H -0.2743 -0.5535 0.3068 0.080 Uiso 0.32(2) 1 calc GR . P A 2 H48B H -0.3540 -0.4103 0.3588 0.080 Uiso 0.32(2) 1 calc GR . P A 2 H48C H -0.1871 -0.5486 0.3889 0.080 Uiso 0.32(2) 1 calc GR . P A 2 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 0.0429(4) 0.0495(5) 0.0583(5) -0.0206(4) -0.0021(3) -0.0154(3) I2 0.0380(4) 0.0463(5) 0.0504(4) -0.0110(3) -0.0034(3) -0.0134(3) O28 0.036(4) 0.049(5) 0.094(7) -0.039(5) 0.003(4) -0.005(4) O29 0.045(4) 0.054(5) 0.063(5) -0.014(4) 0.004(4) -0.025(4) O31 0.040(4) 0.049(5) 0.058(5) -0.016(4) -0.010(4) -0.015(4) O32 0.048(5) 0.058(5) 0.064(6) -0.024(5) 0.000(4) -0.018(4) N1 0.043(5) 0.048(6) 0.047(5) -0.006(4) 0.000(4) -0.020(4) C2 0.046(6) 0.047(7) 0.054(7) -0.009(5) -0.002(5) -0.022(5) C3 0.050(6) 0.054(7) 0.042(6) -0.003(5) -0.002(5) -0.021(6) C4 0.043(6) 0.044(6) 0.049(6) -0.005(5) -0.019(5) -0.011(5) C5 0.063(8) 0.045(7) 0.052(7) 0.004(5) -0.016(6) -0.017(6) C6 0.045(6) 0.054(7) 0.050(6) -0.012(6) 0.007(5) -0.010(5) C7 0.053(7) 0.045(7) 0.063(8) -0.010(6) -0.022(6) -0.009(6) C8 0.046(7) 0.051(7) 0.066(8) -0.014(6) -0.007(6) -0.007(6) C14 0.038(7) 0.049(7) 0.048(8) -0.008(7) 0.000(6) -0.015(6) C13 0.039(7) 0.050(7) 0.045(9) -0.018(7) 0.008(6) -0.010(6) C12 0.036(6) 0.035(6) 0.049(8) -0.014(6) 0.007(6) -0.016(6) N11 0.040(6) 0.039(7) 0.050(7) -0.010(6) -0.001(6) -0.014(6) C16 0.037(7) 0.047(7) 0.053(9) -0.009(7) -0.009(7) -0.010(6) C15 0.036(7) 0.052(7) 0.052(9) -0.007(7) 0.009(7) -0.011(6) C17 0.044(8) 0.049(8) 0.061(9) -0.003(7) 0.000(7) -0.021(7) C18 0.053(10) 0.078(13) 0.071(13) -0.016(11) -0.013(9) -0.037(10) C21 0.046(6) 0.048(7) 0.048(6) -0.013(5) 0.003(5) -0.021(5) C22 0.033(5) 0.043(6) 0.049(6) -0.001(5) 0.001(4) -0.012(5) C23 0.040(5) 0.033(5) 0.039(5) -0.002(4) -0.003(4) -0.005(4) C24 0.041(6) 0.049(7) 0.051(6) -0.015(5) 0.003(5) -0.020(5) C25 0.032(5) 0.063(8) 0.059(7) -0.024(6) 0.004(5) -0.012(5) C26 0.037(6) 0.055(7) 0.064(8) -0.009(6) -0.005(5) -0.021(5) C27 0.045(6) 0.055(7) 0.053(7) -0.020(6) 0.013(5) -0.021(6) C30 0.028(5) 0.041(6) 0.038(5) 0.007(4) 0.009(4) -0.004(4) C44 0.044(9) 0.047(8) 0.050(10) -0.013(9) 0.006(9) -0.011(8) C45 0.035(9) 0.051(9) 0.051(11) -0.005(10) -0.001(10) -0.013(8) C46 0.034(8) 0.039(9) 0.046(11) -0.015(9) 0.005(9) -0.010(8) N41 0.032(8) 0.035(8) 0.058(10) -0.007(8) -0.004(8) -0.024(8) C42 0.042(9) 0.041(9) 0.057(11) -0.006(9) 0.002(9) -0.013(9) C43 0.043(10) 0.043(9) 0.043(12) -0.023(10) 0.003(10) -0.014(9) C47 0.037(11) 0.056(12) 0.059(13) -0.014(11) -0.010(11) -0.029(10) C48 0.048(15) 0.063(17) 0.064(17) -0.024(14) -0.019(14) -0.029(14) 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' 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_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -11 0.0072 0 0 11 0.0062 5 3 0 0.0838 -5 -3 0 0.0838 0 5 2 0.0295 0 -5 -2 0.0295 3 6 2 0.0582 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 O28 I1 N1 175.6(3) . . ? O31 I2 N11 176.2(6) . . ? O31 I2 N41 171.2(11) . . ? C27 O28 I1 118.3(7) . . ? C30 O31 I2 114.8(7) . . ? C2 N1 I1 121.5(8) . . ? C2 N1 C6 118.2(11) . . ? C6 N1 I1 120.3(8) . . ? N1 C2 H2 119.2 . . ? N1 C2 C3 121.5(12) . . ? C3 C2 H2 119.2 . . ? C2 C3 H3 119.8 . . ? C4 C3 C2 120.4(12) . . ? C4 C3 H3 119.8 . . ? C3 C4 C5 118.2(12) . . ? C3 C4 C7 123.1(13) . . ? C5 C4 C7 118.7(13) . . ? C4 C5 H5 120.4 . . ? C4 C5 C6 119.2(13) . . ? C6 C5 H5 120.4 . . ? N1 C6 C5 122.5(12) . . ? N1 C6 H6 118.8 . . ? C5 C6 H6 118.8 . . ? C4 C7 H7A 108.3 . . ? C4 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C8 C7 C4 116.1(12) . . ? C8 C7 H7A 108.3 . . ? C8 C7 H7B 108.3 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C13 C14 C15 120.0 . . ? C13 C14 C17 122.1(11) . . ? C15 C14 C17 117.8(11) . . ? C14 C13 H13 120.0 . . ? C14 C13 C12 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C12 H12 120.0 . . ? N11 C12 C13 120.0 . . ? N11 C12 H12 120.0 . . ? C12 N11 I2 118.4(9) . . ? C12 N11 C16 120.0 . . ? C16 N11 I2 121.4(8) . . ? N11 C16 H16 120.0 . . ? N11 C16 C15 120.0 . . ? C15 C16 H16 120.0 . . ? C14 C15 H15 120.0 . . ? C16 C15 C14 120.0 . . ? C16 C15 H15 120.0 . . ? C14 C17 H17A 109.6 . . ? C14 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? C18 C17 C14 110.5(18) . . ? C18 C17 H17A 109.6 . . ? C18 C17 H17B 109.6 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C22 C21 C27 121.4(11) . . ? C26 C21 C22 120.5(11) . . ? C26 C21 C27 118.0(10) . . ? C21 C22 H22 120.5 . . ? C21 C22 C23 119.0(11) . . ? C23 C22 H22 120.5 . . ? C22 C23 C30 118.0(10) . . ? C24 C23 C22 121.3(10) . . ? C24 C23 C30 120.7(10) . . ? C23 C24 H24 120.2 . . ? C23 C24 C25 119.7(11) . . ? C25 C24 H24 120.2 . . ? C24 C25 H25 120.4 . . ? C26 C25 C24 119.1(11) . . ? C26 C25 H25 120.4 . . ? C21 C26 C25 120.4(10) . . ? C21 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? O28 C27 C21 111.1(10) . . ? O29 C27 O28 125.8(12) . . ? O29 C27 C21 123.1(12) . . ? O31 C30 C23 113.0(9) . . ? O32 C30 O31 129.6(11) . . ? O32 C30 C23 117.3(10) . . ? C45 C44 C43 120.0 . . ? C45 C44 C47 120(3) . . ? C43 C44 C47 120(3) . . ? C44 C45 H45 120.0 . . ? C44 C45 C46 120.0 . . ? C46 C45 H45 120.0 . . ? C45 C46 H46 120.0 . . ? N41 C46 C45 120.0 . . ? N41 C46 H46 120.0 . . ? C46 N41 I2 119.9(19) . . ? C46 N41 C42 120.0 . . ? C42 N41 I2 119.9(19) . . ? N41 C42 H42 120.0 . . ? C43 C42 N41 120.0 . . ? C43 C42 H42 120.0 . . ? C44 C43 H43 120.0 . . ? C42 C43 C44 120.0 . . ? C42 C43 H43 120.0 . . ? C44 C47 H47A 108.9 . . ? C44 C47 H47B 108.9 . . ? H47A C47 H47B 107.7 . . ? C48 C47 C44 113(4) . . ? C48 C47 H47A 108.9 . . ? C48 C47 H47B 108.9 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48B 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? 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 O28 2.169(8) . ? I1 N1 2.287(10) . ? I2 O31 2.179(7) . ? I2 N11 2.255(11) . ? I2 N41 2.33(2) . ? O28 C27 1.314(16) . ? O29 C27 1.189(15) . ? O31 C30 1.250(14) . ? O32 C30 1.225(14) . ? N1 C2 1.324(16) . ? N1 C6 1.333(17) . ? C2 H2 0.9300 . ? C2 C3 1.400(17) . ? C3 H3 0.9300 . ? C3 C4 1.359(19) . ? C4 C5 1.36(2) . ? C4 C7 1.527(17) . ? C5 H5 0.9300 . ? C5 C6 1.399(19) . ? C6 H6 0.9300 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 C8 1.51(2) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C14 C13 1.3900 . ? C14 C15 1.3900 . ? C14 C17 1.52(2) . ? C13 H13 0.9300 . ? C13 C12 1.3900 . ? C12 H12 0.9300 . ? C12 N11 1.3900 . ? N11 C16 1.3900 . ? C16 H16 0.9300 . ? C16 C15 1.3900 . ? C15 H15 0.9300 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 C18 1.51(3) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C21 C22 1.399(16) . ? C21 C26 1.382(17) . ? C21 C27 1.511(16) . ? C22 H22 0.9300 . ? C22 C23 1.402(16) . ? C23 C24 1.375(16) . ? C23 C30 1.572(15) . ? C24 H24 0.9300 . ? C24 C25 1.415(15) . ? C25 H25 0.9300 . ? C25 C26 1.405(18) . ? C26 H26 0.9300 . ? C44 C45 1.3900 . ? C44 C43 1.3900 . ? C44 C47 1.49(5) . ? C45 H45 0.9300 . ? C45 C46 1.3900 . ? C46 H46 0.9300 . ? C46 N41 1.3900 . ? N41 C42 1.3900 . ? C42 H42 0.9300 . ? C42 C43 1.3900 . ? C43 H43 0.9300 . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C47 C48 1.46(6) . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -0.4556 0.4455 -10.5198 -0.0785 0.9969 -0.0090 0.4556 -0.4455 10.5198 0.0785 -0.9969 0.0090 5.1385 2.6198 -0.1424 0.9931 0.0782 0.0871 -5.1385 -2.6198 0.1424 -0.9931 -0.0782 -0.0871 -0.2496 5.4084 2.2325 -0.0090 0.0001 1.0000 0.2496 -5.4084 -2.2325 0.0090 -0.0001 -1.0000 2.5574 5.7482 1.7160 0.5258 0.0421 0.8496