#------------------------------------------------------------------------------ #$Date: 2021-10-15 02:06:48 +0300 (Fri, 15 Oct 2021) $ #$Revision: 269960 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/85/7708566.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_7708566 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 H18 F4 I2 N2 O4' _chemical_formula_sum 'C22 H18 F4 I2 N2 O4' _chemical_formula_weight 704.18 _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 2021-04-27 _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 90 _cell_angle_beta 91.420(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.8812(3) _cell_length_b 32.4911(7) _cell_length_c 7.4264(2) _cell_measurement_reflns_used 4276 _cell_measurement_temperature 120.00(10) _cell_measurement_theta_max 76.2330 _cell_measurement_theta_min 4.4510 _cell_volume 2383.52(11) _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)' _computing_structure_solution 'ShelXT (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 0.997 _diffrn_measured_fraction_theta_max 0.991 _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 -116.00 -19.00 1.00 1.00 -- -41.90 -37.00 -60.00 97 2 \w -68.00 28.00 1.00 1.00 -- -41.90 77.00 90.00 96 3 \w 26.00 61.00 1.00 1.00 -- 41.90 -77.00 120.00 35 4 \w 46.00 109.00 1.00 1.00 -- 112.00-111.00 120.00 63 5 \w 40.00 139.00 1.00 1.00 -- 112.00 -61.00 150.00 99 6 \w 29.00 101.00 1.00 1.00 -- 112.00 -94.00 -30.00 72 7 \w 104.00 171.00 1.00 1.00 -- 112.00 111.00 120.00 67 8 \w 90.00 178.00 1.00 1.00 -- 112.00 45.00 -60.00 88 ; _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 -0.1558583000 _diffrn_orient_matrix_UB_12 0.0002969000 _diffrn_orient_matrix_UB_13 0.0058946000 _diffrn_orient_matrix_UB_21 -0.0002805000 _diffrn_orient_matrix_UB_22 0.0469258000 _diffrn_orient_matrix_UB_23 -0.0301650000 _diffrn_orient_matrix_UB_31 -0.0084821000 _diffrn_orient_matrix_UB_32 -0.0068178000 _diffrn_orient_matrix_UB_33 -0.2050241000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_unetI/netI 0.0536 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 8490 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.128 _diffrn_reflns_theta_min 2.720 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 21.304 _exptl_absorpt_correction_T_max 0.700 _exptl_absorpt_correction_T_min 0.079 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020) Numerical absorption correction based on gaussian integration over a multifaceted crystal model 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 1.962 _exptl_crystal_description plate _exptl_crystal_F_000 1352 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DCM/petroleum ether' _exptl_crystal_size_max 0.322 _exptl_crystal_size_mid 0.138 _exptl_crystal_size_min 0.034 _refine_diff_density_max 2.364 _refine_diff_density_min -1.233 _refine_diff_density_rms 0.175 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.204 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 309 _refine_ls_number_reflns 4646 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.204 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0475 _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^)+(0.0493P)^2^+14.2794P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1319 _refine_ls_wR_factor_ref 0.1368 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4085 _reflns_number_total 4646 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt03324g2.cif _cod_data_source_block 1F _cod_database_code 7708566 _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 98.94 _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.a Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C17(H17A,H17B) 2.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C5(H5), C6(H6), C12(H12), C13(H13), C15(H15), C16(H16) 2.c Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C18(H18A,H18B,H18C) ; _shelx_res_file ; TITL oie072_numabs_a.res in P2(1)/c REM Old TITL OIE072_numabs in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.076, Rweak 0.097, Alpha 0.048, Orientation as input REM Formula found by SHELXT: C22 N3 O3 F4 I2 CELL 1.54184 9.8812 32.4911 7.4264 90 91.42 90 ZERR 4 0.0003 0.0007 0.0002 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H F I N O UNIT 88 72 16 8 8 16 L.S. 4 PLAN 20 BOND $H list 4 fmap 2 53 acta SHEL 50 0.81 REM REM REM WGHT 0.049300 14.279399 FVAR 0.25700 I1 4 0.162773 0.522357 0.687022 11.00000 0.02141 0.02555 = 0.01822 0.00321 0.00132 -0.00118 I2 4 0.345094 0.509996 0.212574 11.00000 0.02188 0.02229 = 0.02011 -0.00238 0.00259 -0.00021 F33 3 0.418825 0.678472 0.107163 11.00000 0.03273 0.03749 = 0.03301 0.00087 0.01360 -0.00968 F34 3 0.284475 0.749252 0.153627 11.00000 0.04726 0.02632 = 0.04366 0.01116 0.00041 -0.00680 F35 3 0.064710 0.751767 0.363833 11.00000 0.04844 0.02336 = 0.05474 -0.00431 -0.00005 0.01126 F36 3 -0.022679 0.683704 0.528129 11.00000 0.03493 0.03466 = 0.03721 -0.00459 0.01563 0.00853 O28 6 0.201315 0.584146 0.570276 11.00000 0.01867 0.03099 = 0.03262 0.01337 -0.00159 0.00005 O29 6 -0.016517 0.598116 0.508752 11.00000 0.01756 0.03577 = 0.03617 0.00955 0.00824 -0.00089 O31 6 0.278592 0.574760 0.184032 11.00000 0.02506 0.02676 = 0.02982 -0.00831 -0.00059 0.00095 O32 6 0.467694 0.601672 0.313115 11.00000 0.01669 0.03317 = 0.03910 -0.00568 0.00167 0.00062 N1 5 0.147012 0.459486 0.806074 11.00000 0.01370 0.02237 = 0.02522 -0.00037 0.00263 -0.00472 N11 5 0.385681 0.443526 0.244345 11.00000 0.02209 0.02016 = 0.01782 -0.00384 0.00581 -0.00004 C2 1 0.248505 0.433124 0.795588 11.00000 0.01705 0.02614 = 0.02292 -0.00029 0.00188 -0.00219 AFIX 43 H2 2 0.328206 0.441470 0.742447 11.00000 -1.20000 AFIX 0 C3 1 0.239001 0.393136 0.862208 11.00000 0.01713 0.02583 = 0.02163 0.00080 0.00289 0.00411 AFIX 43 H3 2 0.311485 0.375096 0.852056 11.00000 -1.20000 AFIX 0 C4 1 0.122147 0.380320 0.943163 11.00000 0.02185 0.03033 = 0.01437 -0.00002 -0.00089 -0.00066 C5 1 0.017425 0.409032 0.956217 11.00000 0.01479 0.03204 = 0.02281 0.00458 0.00319 -0.00338 AFIX 43 H5 2 -0.061820 0.401904 1.013594 11.00000 -1.20000 AFIX 0 C6 1 0.031267 0.447758 0.884496 11.00000 0.01323 0.03394 = 0.02458 -0.00128 0.00669 -0.00053 AFIX 43 H6 2 -0.040387 0.466236 0.890054 11.00000 -1.20000 AFIX 0 C7 1 0.101317 0.337708 1.017245 11.00000 0.03135 0.02951 = 0.02931 0.00641 -0.00160 -0.00431 AFIX 23 H7A 2 0.009436 0.329158 0.987297 11.00000 -1.20000 H7B 2 0.109949 0.338999 1.147517 11.00000 -1.20000 AFIX 0 C8 1 0.197081 0.305152 0.950951 11.00000 0.04048 0.02893 = 0.06994 0.00889 0.01151 0.00568 AFIX 137 H8A 2 0.190891 0.303773 0.821882 11.00000 -1.50000 H8B 2 0.173184 0.278954 1.000786 11.00000 -1.50000 H8C 2 0.288055 0.312030 0.988035 11.00000 -1.50000 AFIX 0 C12 1 0.501318 0.426623 0.187915 11.00000 0.02123 0.03388 = 0.02041 -0.00060 0.00361 -0.00462 AFIX 43 H12 2 0.562544 0.442962 0.127168 11.00000 -1.20000 AFIX 0 C13 1 0.531483 0.385972 0.217431 11.00000 0.02772 0.02668 = 0.02213 -0.00355 -0.00145 0.00280 AFIX 43 H13 2 0.612112 0.375148 0.176072 11.00000 -1.20000 AFIX 0 C14 1 0.442816 0.360904 0.308358 11.00000 0.02865 0.02923 = 0.01898 -0.00051 -0.00200 0.00153 C15 1 0.321669 0.378377 0.362989 11.00000 0.03190 0.03320 = 0.02072 0.00031 0.00353 -0.00667 AFIX 43 H15 2 0.258040 0.362434 0.421336 11.00000 -1.20000 AFIX 0 C16 1 0.296884 0.419600 0.329722 11.00000 0.02052 0.02833 = 0.02086 -0.00214 0.00567 -0.00086 AFIX 43 H16 2 0.216259 0.431110 0.367628 11.00000 -1.20000 AFIX 0 C17 1 0.481246 0.316884 0.346750 11.00000 0.03437 0.02737 = 0.03257 0.00111 0.00402 0.00288 AFIX 23 H17A 2 0.480343 0.302030 0.233427 11.00000 -1.20000 H17B 2 0.573561 0.316505 0.394289 11.00000 -1.20000 AFIX 0 C18 1 0.394003 0.293897 0.475429 11.00000 0.04807 0.04310 = 0.08817 0.03457 0.01353 0.00625 AFIX 137 H18A 2 0.302765 0.292859 0.428128 11.00000 -1.50000 H18B 2 0.395468 0.307729 0.589690 11.00000 -1.50000 H18C 2 0.428001 0.266408 0.490731 11.00000 -1.50000 AFIX 0 C21 1 0.153488 0.643395 0.404032 11.00000 0.01839 0.02587 = 0.01709 -0.00144 -0.00081 -0.00143 C22 1 0.268298 0.642165 0.296829 11.00000 0.02148 0.01803 = 0.01882 -0.00093 -0.00028 -0.00056 C23 1 0.309789 0.678011 0.214594 11.00000 0.02519 0.03106 = 0.01950 0.00053 0.00167 -0.00277 C24 1 0.242018 0.714802 0.233754 11.00000 0.03449 0.01919 = 0.02650 0.00439 -0.00508 -0.00637 C25 1 0.129078 0.715841 0.339500 11.00000 0.03815 0.01736 = 0.02913 -0.00068 -0.00378 0.00390 C26 1 0.087142 0.680242 0.422583 11.00000 0.02352 0.03126 = 0.01826 -0.00438 0.00210 0.00182 C27 1 0.103897 0.605199 0.501685 11.00000 0.02309 0.02744 = 0.01572 -0.00147 0.00494 -0.00094 C30 1 0.349275 0.603242 0.267076 11.00000 0.02369 0.03228 = 0.01807 -0.00188 0.00998 -0.00424 HKLF 4 REM oie072_numabs_a.res in P2(1)/c REM R1 = 0.0475 for 4085 Fo > 4sig(Fo) and 0.0538 for all 4646 data REM 309 parameters refined using 0 restraints END WGHT 0.0493 14.2930 REM Highest difference peak 2.364, deepest hole -1.233, 1-sigma level 0.175 Q1 1 0.3414 0.5385 0.2162 11.00000 0.05 2.36 Q2 1 0.1628 0.5028 0.6889 11.00000 0.05 1.62 Q3 1 0.3498 0.4819 0.2087 11.00000 0.05 1.61 Q4 1 0.0743 0.5245 0.7992 11.00000 0.05 1.15 Q5 1 0.1596 0.5578 0.6911 11.00000 0.05 1.14 Q6 1 0.4735 0.5010 0.2529 11.00000 0.05 0.99 Q7 1 0.2561 0.5075 0.2979 11.00000 0.05 0.96 Q8 1 0.2441 0.5222 0.5932 11.00000 0.05 0.92 Q9 1 0.1801 0.4603 0.6558 11.00000 0.05 0.91 Q10 1 0.4331 0.5080 0.1295 11.00000 0.05 0.82 Q11 1 0.0199 0.4759 0.8449 11.00000 0.05 0.75 Q12 1 0.3472 0.4396 0.1634 11.00000 0.05 0.72 Q13 1 0.0357 0.5330 0.6650 11.00000 0.05 0.71 Q14 1 0.4981 0.4808 -0.0016 11.00000 0.05 0.67 Q15 1 0.2157 0.5137 0.1819 11.00000 0.05 0.67 Q16 1 0.2533 0.4416 0.5420 11.00000 0.05 0.63 Q17 1 0.3594 0.5777 0.0960 11.00000 0.05 0.62 Q18 1 0.1335 0.5185 0.5832 11.00000 0.05 0.61 Q19 1 0.2402 0.5148 0.1284 11.00000 0.05 0.60 Q20 1 0.4097 0.4566 0.2926 11.00000 0.05 0.60 ; _shelx_res_checksum 64453 _shelx_hkl_file ; 1 0 0 38.15 1.88 2 0 0 1167.90 14.41 3 0 0 20.43 3.43 3 0 0 22.10 2.52 4 0 0 1071.51 28.44 5 0 0 11.28 3.68 6 0 0 3592.56 71.51 7 0 0 15.78 4.85 8 0 0 0.68 2.66 8 0 0 9.95 5.19 9 0 0 10.91 4.88 -10 0 0 903.50 55.30 -11 0 0 74.60 13.77 -12 0 0 497.23 24.61 1 1 0 626.08 10.58 -1 1 0 659.93 8.41 2 1 0 17.36 2.48 2 -1 0 22.60 2.15 3 1 0 3.97 1.16 3 1 0 1.13 1.16 4 1 0 3.35 1.84 4 1 0 4.68 1.31 4 -1 0 6.95 2.59 5 -1 0 5.41 2.46 5 1 0 2.09 1.69 6 1 0 161.24 16.44 6 -1 0 175.44 16.83 7 1 0 2.51 3.37 7 -1 0 -2.31 2.41 8 1 0 0.26 2.56 8 -1 0 1.34 2.45 8 1 0 4.11 4.35 8 -1 0 5.54 3.99 9 1 0 6.96 3.51 9 -1 0 6.68 3.98 -10 1 0 195.56 25.81 -10 -1 0 144.98 23.89 -11 -1 0 52.69 11.47 -11 1 0 55.00 10.94 -12 -1 0 49.55 8.22 0 2 0 7594.31 64.92 1 2 0 54.63 3.50 -1 2 0 49.26 2.32 -2 2 0 1703.52 20.02 2 2 0 1674.61 24.71 3 2 0 2.25 1.12 4 2 0 2254.61 41.77 4 2 0 2246.18 29.06 5 2 0 164.04 13.22 5 -2 0 167.14 12.96 6 2 0 4890.74 82.28 6 -2 0 4812.92 81.47 7 -2 0 70.94 11.96 7 2 0 56.06 10.11 8 2 0 0.23 2.75 8 -2 0 4.64 3.05 8 2 0 3.35 2.69 8 -2 0 6.98 5.29 9 2 0 18.36 5.95 -10 2 0 1199.30 59.83 10 2 0 1158.60 44.46 -10 -2 0 1259.31 68.44 -11 2 0 77.85 13.00 -11 -2 0 79.00 14.79 -12 -2 0 523.90 28.88 0 3 0 2.03 2.59 -1 3 0 44.19 2.55 1 3 0 49.72 3.89 -2 3 0 2.87 0.89 2 3 0 1.91 1.31 3 3 0 5.99 2.01 4 3 0 950.29 19.62 4 3 0 1008.22 28.32 5 3 0 711.21 27.37 5 -3 0 661.76 26.21 6 3 0 25.15 7.94 6 -3 0 6.93 5.08 7 -3 0 289.20 23.36 7 3 0 279.94 22.62 8 -3 0 32.73 9.33 8 3 0 27.82 6.66 8 3 0 35.16 9.14 9 3 0 2.66 3.28 -10 3 0 237.63 26.19 -10 -3 0 281.14 34.27 -11 3 0 53.41 10.03 -11 -3 0 50.78 12.47 -12 -3 0 30.35 7.28 0 4 0 2850.38 54.29 1 4 0 33.30 3.56 -1 4 0 31.08 2.65 2 4 0 1887.77 29.55 -2 4 0 1813.30 20.44 -3 4 0 87.72 5.91 3 4 0 80.01 7.22 4 4 0 3092.99 51.08 5 4 0 97.33 10.34 6 -4 0 2332.03 58.04 6 4 0 2255.92 57.59 7 -4 0 113.92 14.71 7 4 0 123.15 15.36 8 4 0 83.18 13.96 8 -4 0 66.27 13.14 8 4 0 61.52 10.57 9 4 0 108.03 14.32 -9 4 0 123.21 19.96 -10 -4 0 1095.40 67.21 10 4 0 998.80 42.23 -10 4 0 998.52 49.88 -11 -4 0 18.40 7.63 -12 -4 0 478.65 29.43 0 5 0 2.59 2.35 -1 5 0 1682.51 23.37 1 5 0 1602.11 28.03 2 5 0 538.85 16.83 -2 5 0 524.74 11.66 3 5 0 2.00 1.49 -3 5 0 1.68 1.08 4 5 0 3.31 2.10 5 5 0 479.66 23.35 6 -5 0 7.72 5.00 6 5 0 2.57 2.43 7 -5 0 439.05 29.11 7 5 0 379.17 26.85 8 5 0 -0.52 3.49 8 -5 0 -9.52 5.02 9 5 0 40.27 9.96 -9 5 0 20.60 7.45 -10 -5 0 115.17 22.50 -10 5 0 72.04 13.87 -11 -5 0 174.25 21.32 -12 -5 0 20.53 6.15 0 6 0 2129.93 49.42 -1 6 0 142.22 8.04 1 6 0 138.04 9.58 2 6 0 296.31 13.20 -2 6 0 269.39 9.20 -3 6 0 2.77 1.08 3 6 0 1.32 1.22 4 6 0 3926.14 59.84 5 6 0 79.83 9.79 6 -6 0 1973.80 54.55 6 6 0 1901.00 53.91 7 6 0 34.47 8.49 7 -6 0 39.65 8.84 8 -6 0 74.22 14.02 8 6 0 59.43 11.84 8 6 0 60.28 10.92 9 6 0 18.48 6.46 -10 -6 0 646.62 46.12 10 6 0 693.09 36.28 -11 -6 0 25.70 8.33 -12 -6 0 359.19 22.45 0 7 0 -0.50 2.54 -1 7 0 1057.81 24.55 1 7 0 1080.68 28.89 2 7 0 18.00 3.60 -2 7 0 13.23 2.44 3 7 0 10.03 3.09 -3 7 0 11.18 2.30 4 7 0 203.49 13.87 5 7 0 1948.52 48.66 6 -7 0 4.12 3.53 6 7 0 1.47 2.06 7 7 0 299.20 24.45 7 -7 0 325.24 26.28 8 7 0 135.83 18.76 8 7 0 151.27 17.79 9 7 0 10.12 4.68 -10 -7 0 51.17 13.80 10 7 0 89.55 14.86 -11 -7 0 493.57 32.91 -12 -7 0 15.41 4.95 0 8 0 1583.22 44.05 -1 8 0 68.44 7.11 1 8 0 67.41 8.61 -2 8 0 724.52 18.71 2 8 0 782.38 25.20 -3 8 0 200.74 9.73 3 8 0 194.54 12.92 -4 8 0 1493.41 29.93 4 8 0 1497.79 39.40 5 8 0 196.63 15.95 6 8 0 1237.75 45.11 7 8 0 162.14 18.60 7 -8 0 189.70 20.79 8 8 0 13.27 6.21 8 8 0 24.85 7.49 9 8 0 92.03 14.15 10 8 0 776.91 40.22 -10 -8 0 717.51 44.97 -11 -8 0 49.44 10.20 -12 -8 0 135.71 12.52 0 9 0 1.30 2.28 1 9 0 3526.23 66.55 -1 9 0 3141.85 52.84 2 9 0 312.42 17.22 -2 9 0 304.49 13.44 3 9 0 1.73 1.99 -3 9 0 0.67 0.70 4 9 0 7.37 3.01 -4 9 0 6.99 2.30 5 9 0 1328.72 42.82 6 9 0 103.20 13.71 7 -9 0 923.84 45.26 7 9 0 918.13 43.39 7 9 0 889.15 43.78 8 9 0 315.51 29.06 8 9 0 327.00 27.66 9 9 0 267.30 25.45 10 9 0 139.95 18.18 -10 -9 0 148.69 21.16 -11 -9 0 391.38 27.11 -12 -9 0 6.05 2.57 0 10 0 3776.76 70.75 1 10 0 409.13 22.99 -1 10 0 444.33 22.04 2 10 0 19.57 5.05 -2 10 0 22.34 4.19 -3 10 0 453.96 16.49 3 10 0 502.96 23.59 4 10 0 198.59 15.68 5 10 0 37.86 7.75 6 10 0 1151.54 46.45 7 10 0 396.49 29.75 7 10 0 392.06 30.22 7 -10 0 390.83 31.24 8 10 0 16.35 6.75 8 10 0 6.53 4.36 9 10 0 387.29 31.93 10 10 0 93.13 15.37 -10 -10 0 115.15 17.20 -11 -10 0 23.30 7.07 -12 -10 0 64.86 7.68 0 11 0 -0.16 2.21 1 11 0 1725.97 49.21 -1 11 0 2001.33 50.63 -2 11 0 69.05 7.91 2 11 0 76.89 10.13 -3 11 0 338.69 15.51 3 11 0 346.03 20.77 4 11 0 384.42 22.69 5 11 0 2425.99 63.13 6 11 0 3.81 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7.65 5.88 -2 13 -7 19.03 8.62 -2 -13 -7 1.39 4.09 -3 13 -7 108.35 15.45 -3 -13 -7 146.47 18.44 -4 -13 -7 82.09 13.44 -5 -13 -7 19.76 6.36 -6 -13 -7 32.30 7.04 -7 -13 -7 32.29 4.99 7 -14 -7 56.79 7.26 6 -14 -7 50.84 9.45 5 -14 -7 231.39 23.35 4 14 -7 675.95 45.05 4 -14 -7 772.64 43.41 3 14 -7 491.49 40.26 3 -14 -7 516.48 33.58 2 -14 -7 44.00 8.08 2 14 -7 41.47 12.11 1 14 -7 2.83 6.08 0 14 -7 268.85 28.54 -1 14 -7 250.96 26.89 -1 -14 -7 247.38 24.04 -2 14 -7 754.33 44.37 -2 -14 -7 759.73 43.28 -3 14 -7 163.85 19.16 -3 -14 -7 195.83 21.36 -4 14 -7 -0.23 1.91 -4 -14 -7 7.94 4.83 -5 -14 -7 21.09 6.40 -6 -14 -7 170.29 14.50 7 -15 -7 159.70 10.86 6 -15 -7 132.16 13.56 5 -15 -7 39.77 8.50 4 -15 -7 14.59 6.36 4 15 -7 8.64 6.59 3 -15 -7 20.16 6.88 3 15 -7 13.50 8.43 2 15 -7 200.60 25.09 2 -15 -7 160.83 15.97 1 15 -7 162.82 22.57 0 15 -7 268.87 28.61 -1 15 -7 6.87 4.98 -2 -15 -7 9.59 5.34 -2 15 -7 3.90 4.27 -3 15 -7 32.82 8.78 -3 -15 -7 48.06 10.09 -4 15 -7 133.93 14.58 -4 -15 -7 186.29 18.75 -5 -15 -7 48.54 8.68 -6 -15 -7 46.15 7.29 6 -16 -7 31.70 6.10 5 -16 -7 223.82 19.03 4 16 -7 423.08 29.04 4 -16 -7 462.27 28.81 3 16 -7 633.81 43.68 3 -16 -7 596.76 32.34 2 16 -7 163.03 23.71 2 -16 -7 147.97 15.05 1 16 -7 3.40 5.16 0 16 -7 153.02 21.37 -1 16 -7 136.32 19.65 -2 16 -7 522.71 36.31 -2 -16 -7 532.70 31.51 -3 16 -7 142.86 17.49 -3 -16 -7 157.00 17.06 -4 16 -7 17.18 5.57 -4 -16 -7 20.70 5.60 -5 -16 -7 38.08 7.10 -6 -16 -7 240.14 15.00 6 -17 -7 119.33 10.49 5 -17 -7 70.21 9.74 4 -17 -7 -1.21 3.59 4 17 -7 0.41 1.66 3 -17 -7 11.50 4.99 3 17 -7 1.91 2.87 2 17 -7 500.65 39.13 2 -17 -7 469.14 25.87 1 17 -7 154.31 21.92 0 17 -7 301.35 29.69 -1 17 -7 0.43 3.35 -2 -17 -7 48.13 9.11 -2 17 -7 42.02 10.59 -3 17 -7 -0.27 3.56 -3 -17 -7 4.58 3.35 -4 17 -7 185.07 16.52 -4 -17 -7 224.83 18.22 -5 -17 -7 85.98 10.18 -6 -17 -7 99.49 8.81 6 -18 -7 2.50 1.68 5 -18 -7 291.19 18.33 4 18 -7 157.64 14.62 4 -18 -7 185.19 15.85 3 18 -7 193.36 20.22 3 -18 -7 195.05 16.69 2 18 -7 366.86 31.41 2 -18 -7 353.48 21.67 1 18 -7 4.45 4.74 0 18 -7 100.36 17.76 -1 18 -7 191.12 23.27 -2 18 -7 332.65 28.66 -2 -18 -7 291.43 20.01 -3 18 -7 86.13 13.74 -3 -18 -7 94.06 11.55 -4 -18 -7 54.49 8.49 -4 18 -7 45.89 7.77 -5 -18 -7 61.39 7.99 -6 -18 -7 131.18 9.10 6 -19 -7 62.24 6.17 5 -19 -7 136.60 11.40 4 -19 -7 11.82 4.25 3 -19 -7 33.38 6.90 3 19 -7 33.41 8.23 2 19 -7 362.48 28.65 2 -19 -7 343.29 20.37 1 19 -7 58.17 12.45 0 19 -7 161.76 20.57 -1 19 -7 134.06 18.64 -2 19 -7 116.17 16.60 -3 19 -7 4.75 3.19 -3 -19 -7 2.89 2.57 -4 -19 -7 370.37 20.09 -5 -19 -7 55.98 7.08 5 -20 -7 177.87 12.06 4 -20 -7 119.77 11.12 3 20 -7 108.39 12.89 3 -20 -7 106.65 11.09 2 20 -7 59.30 10.62 2 -20 -7 63.79 8.51 1 20 -7 93.11 14.43 0 20 -7 2.18 3.46 -1 20 -7 441.15 31.07 -2 20 -7 188.84 19.27 -3 20 -7 9.53 4.51 -3 -20 -7 1.75 1.05 -4 -20 -7 76.10 8.43 -5 -20 -7 45.29 5.61 5 -21 -7 123.60 9.11 4 -21 -7 25.24 4.77 3 -21 -7 1.68 2.05 3 21 -7 1.63 2.16 2 21 -7 159.89 16.47 2 -21 -7 160.90 12.90 1 21 -7 47.92 9.58 0 21 -7 24.67 7.25 -1 21 -7 204.75 19.76 -2 21 -7 123.62 14.60 -3 21 -7 -2.84 3.23 -3 -21 -7 -2.02 2.25 -4 -21 -7 267.40 14.19 4 -22 -7 81.26 7.77 3 -22 -7 26.25 4.84 3 22 -7 22.68 4.66 2 22 -7 127.19 13.64 2 -22 -7 122.82 10.54 1 22 -7 55.12 9.94 0 22 -7 -1.80 2.40 -1 22 -7 309.05 22.59 -2 22 -7 120.07 13.12 -3 22 -7 1.53 1.62 4 -23 -7 25.29 4.06 3 -23 -7 5.46 2.27 3 23 -7 8.37 2.67 2 23 -7 278.62 18.37 2 -23 -7 280.65 14.88 1 23 -7 114.86 12.79 0 23 -7 61.59 9.69 -1 23 -7 173.17 15.65 -2 23 -7 56.61 8.44 -3 23 -7 -0.92 1.40 3 -24 -7 1.88 1.15 2 24 -7 167.42 12.90 2 -24 -7 160.54 10.26 1 24 -7 240.65 16.95 0 24 -7 8.55 3.79 -1 24 -7 230.42 16.59 -2 24 -7 98.91 10.14 -3 24 -7 12.47 2.86 2 25 -7 136.27 10.25 1 25 -7 108.73 10.47 0 25 -7 24.92 5.11 -1 25 -7 128.93 11.47 -2 25 -7 39.36 5.77 1 26 -7 219.23 13.25 0 26 -7 80.12 8.40 -1 26 -7 84.91 8.34 -2 26 -7 47.92 5.50 0 27 -7 7.42 2.25 -1 27 -7 73.97 6.86 4 0 -8 3.80 3.92 3 0 -8 193.15 20.36 2 0 -8 989.12 47.11 1 0 -8 366.27 29.23 0 0 -8 737.52 41.28 -1 0 -8 96.64 14.44 -2 0 -8 15.60 5.79 -2 0 -8 26.18 7.71 -3 0 -8 508.04 32.45 -4 0 -8 500.13 30.06 -5 0 -8 235.80 18.61 4 -1 -8 7.84 4.04 4 1 -8 5.92 3.87 3 -1 -8 30.85 11.64 3 1 -8 6.74 11.31 2 -1 -8 63.36 16.42 2 1 -8 114.77 20.87 1 -1 -8 45.75 13.92 1 1 -8 83.50 18.58 0 -1 -8 46.43 16.05 0 1 -8 86.76 19.99 -1 -1 -8 -4.79 3.73 -1 1 -8 5.63 4.99 -1 -1 -8 10.56 6.68 -2 -1 -8 1.10 2.24 -2 1 -8 3.76 1.71 -2 1 -8 -0.96 3.32 -2 -1 -8 1.60 3.25 -3 1 -8 12.83 6.65 -3 -1 -8 20.76 10.17 -4 1 -8 26.94 11.02 -4 -1 -8 45.87 10.32 -5 -1 -8 12.30 6.80 4 -2 -8 1.43 3.51 4 2 -8 4.94 3.52 3 -2 -8 132.73 16.55 3 2 -8 146.77 17.80 2 -2 -8 745.13 40.48 2 2 -8 848.91 43.93 1 -2 -8 347.98 28.09 1 2 -8 340.08 28.30 0 -2 -8 692.61 39.64 0 2 -8 745.71 42.19 -1 -2 -8 44.55 10.11 -1 2 -8 42.59 10.48 -1 -2 -8 38.95 9.52 -2 -2 -8 15.48 5.70 -2 2 -8 15.91 5.68 -2 -2 -8 14.84 5.90 -3 2 -8 282.70 23.95 -3 -2 -8 292.80 24.51 -4 -2 -8 548.55 31.50 -5 -2 -8 321.10 21.68 4 3 -8 10.41 5.31 3 -3 -8 14.07 6.56 3 3 -8 8.02 5.12 2 -3 -8 53.01 18.55 2 3 -8 60.14 16.07 1 -3 -8 160.44 20.55 1 3 -8 161.11 22.42 0 3 -8 62.86 17.49 0 -3 -8 31.64 11.89 -1 -3 -8 45.93 10.17 -1 3 -8 49.94 10.91 -1 -3 -8 59.76 12.16 -2 -3 -8 3.30 2.48 -2 3 -8 7.97 5.20 -2 -3 -8 -0.55 3.39 -3 -3 -8 12.91 7.17 -4 -3 -8 81.17 13.26 -5 -3 -8 33.29 8.13 4 4 -8 31.01 8.50 3 -4 -8 7.66 4.99 3 4 -8 7.10 4.30 2 -4 -8 618.96 36.48 2 4 -8 628.73 38.42 1 -4 -8 457.72 31.95 1 4 -8 462.87 33.75 0 -4 -8 384.93 28.90 0 4 -8 385.58 30.75 -1 -4 -8 45.09 10.30 -1 4 -8 39.67 10.56 -1 -4 -8 42.82 10.01 -2 -4 -8 11.69 4.94 -2 4 -8 16.41 6.34 -2 -4 -8 17.00 6.61 -3 -4 -8 197.37 20.21 -4 -4 -8 557.23 31.67 -5 -4 -8 341.66 22.32 4 5 -8 46.42 9.95 3 -5 -8 2.23 3.54 3 5 -8 -0.26 2.68 2 -5 -8 82.57 14.06 2 5 -8 120.25 23.09 1 -5 -8 127.34 17.42 1 5 -8 141.92 20.22 0 -5 -8 63.86 12.43 0 5 -8 78.20 14.86 -1 -5 -8 91.12 13.37 -1 5 -8 111.62 16.78 -1 -5 -8 102.41 15.47 -2 -5 -8 16.24 5.56 -2 5 -8 16.04 6.74 -2 -5 -8 24.30 7.75 -3 5 -8 21.55 5.33 -3 -5 -8 36.36 8.95 -4 -5 -8 193.19 18.95 -5 -5 -8 151.40 15.06 -6 -5 -8 20.36 4.62 4 6 -8 0.50 3.00 3 6 -8 3.31 3.77 2 -6 -8 671.32 37.31 2 6 -8 719.87 41.66 1 -6 -8 355.91 27.84 1 6 -8 403.10 31.87 0 -6 -8 271.56 23.93 0 6 -8 270.79 25.87 -1 -6 -8 30.19 7.36 -1 6 -8 26.98 8.71 -1 -6 -8 28.58 7.93 -2 6 -8 124.22 15.92 -2 -6 -8 140.86 17.68 -3 -6 -8 67.07 12.28 -3 6 -8 32.24 8.04 -4 -6 -8 490.03 29.17 -5 -6 -8 258.03 19.16 4 7 -8 6.66 4.34 3 7 -8 10.73 4.81 2 -7 -8 343.75 26.68 2 7 -8 331.97 28.64 1 -7 -8 477.37 31.53 1 7 -8 504.23 35.05 0 -7 -8 145.18 17.46 0 7 -8 157.28 20.07 -1 -7 -8 82.09 12.81 -1 7 -8 86.37 14.56 -1 -7 -8 75.58 13.06 -2 7 -8 44.58 9.55 -2 -7 -8 59.15 11.38 -3 7 -8 147.81 14.81 -3 -7 -8 202.35 19.77 -4 -7 -8 109.16 14.13 -5 -7 -8 296.63 20.38 4 8 -8 5.81 4.56 3 8 -8 0.03 3.72 2 8 -8 165.20 20.15 1 8 -8 85.49 15.80 0 8 -8 102.75 16.19 -1 8 -8 84.19 14.28 -1 -8 -8 80.34 13.25 -2 8 -8 56.99 10.95 -2 -8 -8 86.56 13.59 -3 8 -8 24.58 6.27 -3 -8 -8 51.51 10.02 -4 -8 -8 356.15 24.32 -5 -8 -8 263.78 18.81 4 9 -8 12.70 5.58 3 9 -8 86.97 14.26 2 9 -8 74.35 13.50 1 9 -8 362.07 29.93 0 9 -8 67.32 12.94 -1 9 -8 156.35 19.20 -1 -9 -8 146.23 17.52 -2 9 -8 103.66 14.21 -2 -9 -8 127.97 16.04 -3 9 -8 61.82 9.65 -3 -9 -8 89.41 12.66 -4 -9 -8 186.79 17.48 -5 -9 -8 269.06 18.74 4 10 -8 7.82 2.69 3 10 -8 7.63 5.19 2 10 -8 113.90 16.58 1 10 -8 214.33 23.58 0 10 -8 32.56 8.76 -1 10 -8 221.01 22.28 -2 10 -8 70.12 11.66 -2 -10 -8 94.35 13.75 -3 10 -8 -0.96 2.85 -3 -10 -8 4.04 3.90 -4 -10 -8 166.79 16.12 -5 -10 -8 73.92 9.11 4 11 -8 15.40 4.97 3 11 -8 70.56 12.69 2 11 -8 211.55 22.33 1 11 -8 449.42 32.39 0 11 -8 48.42 10.77 -1 11 -8 93.76 14.32 -2 11 -8 12.14 5.30 -2 -11 -8 17.86 5.28 -3 11 -8 67.35 9.59 -3 -11 -8 99.19 12.72 -4 -11 -8 278.78 19.45 -5 -11 -8 201.74 13.73 4 12 -8 75.12 9.59 3 12 -8 113.79 15.98 2 12 -8 204.66 22.00 1 12 -8 16.85 7.96 0 12 -8 7.41 4.62 -1 12 -8 144.70 17.48 -2 12 -8 77.88 11.75 -2 -12 -8 79.97 10.73 -3 12 -8 11.70 3.99 -3 -12 -8 17.35 5.38 -4 -12 -8 14.00 4.62 -5 -12 -8 42.14 5.82 4 13 -8 3.10 2.24 3 13 -8 79.53 12.28 2 13 -8 301.68 26.31 1 13 -8 679.96 39.18 0 13 -8 68.13 12.38 -1 13 -8 66.11 11.86 -2 -13 -8 45.47 7.41 -2 13 -8 45.16 9.16 -3 13 -8 65.31 8.54 -3 -13 -8 88.04 10.14 -4 -13 -8 400.86 19.81 3 14 -8 156.01 15.83 2 14 -8 67.18 12.32 1 14 -8 4.80 5.64 0 14 -8 2.72 2.93 -1 14 -8 128.23 15.91 -2 14 -8 91.84 12.39 -3 -14 -8 46.97 6.91 -3 14 -8 38.57 6.59 -4 -14 -8 2.15 1.24 3 15 -8 56.06 8.85 2 15 -8 173.09 18.03 1 15 -8 559.42 34.57 0 15 -8 187.60 19.83 -1 15 -8 73.58 12.21 -2 15 -8 51.85 9.09 -3 15 -8 89.52 9.15 -3 -15 -8 107.30 9.20 3 16 -8 163.52 13.30 2 16 -8 33.86 7.39 1 16 -8 1.65 3.50 0 16 -8 66.71 11.23 -1 16 -8 90.00 12.67 -2 16 -8 102.96 12.06 3 17 -8 142.84 11.07 2 17 -8 59.31 8.67 1 17 -8 497.58 27.83 0 17 -8 72.64 10.95 -1 17 -8 22.26 6.02 -2 17 -8 6.53 3.28 2 18 -8 -0.17 1.28 1 18 -8 1.56 2.32 0 18 -8 284.07 19.79 -1 18 -8 146.12 13.62 -2 18 -8 109.05 10.30 2 19 -8 56.73 6.99 1 19 -8 286.04 17.72 0 19 -8 189.91 14.86 -1 19 -8 9.29 3.33 -2 19 -8 12.52 3.01 1 20 -8 69.40 7.99 0 20 -8 282.08 16.53 -1 20 -8 88.76 8.80 1 21 -8 87.77 7.92 0 21 -8 73.85 7.56 1 0 -9 -0.55 2.19 0 0 -9 33.10 8.65 2 1 -9 139.07 13.85 1 -1 -9 2.22 3.00 1 1 -9 -1.61 3.26 0 -1 -9 365.37 22.33 0 1 -9 357.49 22.34 -1 1 -9 124.92 12.08 2 2 -9 13.93 7.43 1 2 -9 3.30 3.92 0 2 -9 39.39 9.02 -1 2 -9 13.20 5.31 2 3 -9 108.60 12.34 1 3 -9 29.93 6.91 0 3 -9 286.27 20.00 -1 3 -9 43.70 7.39 2 4 -9 8.93 5.06 1 4 -9 21.33 5.75 0 4 -9 78.05 11.68 -1 4 -9 59.78 8.41 2 5 -9 124.07 12.89 1 5 -9 4.41 3.63 0 5 -9 439.15 24.43 -1 5 -9 23.74 5.55 2 6 -9 18.55 5.64 1 6 -9 6.06 4.01 0 6 -9 45.22 8.58 -1 6 -9 209.31 15.07 2 7 -9 85.25 10.28 1 7 -9 39.18 7.29 0 7 -9 132.48 13.07 -1 7 -9 12.66 4.47 2 8 -9 1.53 1.50 1 8 -9 4.26 3.22 0 8 -9 10.68 3.43 -1 8 -9 170.17 13.03 2 9 -9 0.19 1.86 1 9 -9 59.33 8.58 0 9 -9 82.11 9.89 1 10 -9 3.08 2.42 0 10 -9 101.57 10.64 1 11 -9 125.70 10.96 0 11 -9 82.18 9.01 0 0 0 0.00 0.00 TITL OIE072_numabs in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 9.881168 32.491150 7.426430 90.0000 91.4203 90.0000 ZERR 4.00 0.000283 0.000736 0.000176 0.0000 0.0023 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O F I UNIT 88.00 72.00 8.00 16.00 16.00 8.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 52811 _ins_header ; TITL OIE072_numabs in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 9.881168 32.491150 7.426430 90.0000 91.4203 90.0000 ZERR 4.00 0.000283 0.000736 0.000176 0.0000 0.0023 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O F I UNIT 88.00 72.00 8.00 16.00 16.00 8.00 TREF HKLF 4 END ; _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 1.467 _oxdiff_exptl_absorpt_empirical_full_min 0.741 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 0.16277(5) 0.52236(2) 0.68702(6) 0.02171(14) Uani 1 1 d . . . . . I2 I 0.34509(5) 0.51000(2) 0.21257(6) 0.02139(14) Uani 1 1 d . . . . . F33 F 0.4188(5) 0.67847(16) 0.1072(6) 0.0342(11) Uani 1 1 d . . . . . F34 F 0.2845(6) 0.74925(15) 0.1536(7) 0.0391(12) Uani 1 1 d . . . . . F35 F 0.0647(6) 0.75177(15) 0.3638(8) 0.0422(13) Uani 1 1 d . . . . . F36 F -0.0227(5) 0.68370(15) 0.5281(7) 0.0354(12) Uani 1 1 d . . . . . O28 O 0.2013(5) 0.58415(18) 0.5703(8) 0.0275(12) Uani 1 1 d . . . . . O29 O -0.0165(5) 0.59812(18) 0.5088(8) 0.0297(13) Uani 1 1 d . . . . . O31 O 0.2786(6) 0.57476(17) 0.1840(7) 0.0272(12) Uani 1 1 d . . . . . O32 O 0.4677(5) 0.60167(18) 0.3131(8) 0.0296(13) Uani 1 1 d . . . . . N1 N 0.1470(6) 0.4595(2) 0.8061(8) 0.0204(13) Uani 1 1 d . . . . . N11 N 0.3857(6) 0.44353(19) 0.2443(8) 0.0199(13) Uani 1 1 d . . . . . C2 C 0.2485(8) 0.4331(2) 0.7956(10) 0.0220(15) Uani 1 1 d . . . . . H2 H 0.3282 0.4415 0.7424 0.026 Uiso 1 1 calc R . . . . C3 C 0.2390(7) 0.3931(2) 0.8622(10) 0.0215(15) Uani 1 1 d . . . . . H3 H 0.3115 0.3751 0.8521 0.026 Uiso 1 1 calc R . . . . C4 C 0.1221(8) 0.3803(2) 0.9432(9) 0.0222(15) Uani 1 1 d . . . . . C5 C 0.0174(7) 0.4090(2) 0.9562(10) 0.0232(16) Uani 1 1 d . . . . . H5 H -0.0618 0.4019 1.0136 0.028 Uiso 1 1 calc R . . . . C6 C 0.0313(8) 0.4478(3) 0.8845(10) 0.0238(16) Uani 1 1 d . . . . . H6 H -0.0404 0.4662 0.8901 0.029 Uiso 1 1 calc R . . . . C7 C 0.1013(9) 0.3377(3) 1.0172(11) 0.0301(18) Uani 1 1 d . . . . . H7A H 0.0094 0.3292 0.9873 0.036 Uiso 1 1 calc R . . . . H7B H 0.1099 0.3390 1.1475 0.036 Uiso 1 1 calc R . . . . C8 C 0.1971(11) 0.3052(3) 0.9510(16) 0.046(2) Uani 1 1 d . . . . . H8A H 0.1909 0.3038 0.8219 0.069 Uiso 1 1 calc GR . . . . H8B H 0.1732 0.2790 1.0008 0.069 Uiso 1 1 calc GR . . . . H8C H 0.2881 0.3120 0.9880 0.069 Uiso 1 1 calc GR . . . . C12 C 0.5013(8) 0.4266(3) 0.1879(10) 0.0251(16) Uani 1 1 d . . . . . H12 H 0.5625 0.4430 0.1272 0.030 Uiso 1 1 calc R . . . . C13 C 0.5315(8) 0.3860(2) 0.2174(10) 0.0255(16) Uani 1 1 d . . . . . H13 H 0.6121 0.3751 0.1761 0.031 Uiso 1 1 calc R . . . . C14 C 0.4428(8) 0.3609(3) 0.3084(10) 0.0257(16) Uani 1 1 d . . . . . C15 C 0.3217(9) 0.3784(3) 0.3630(11) 0.0286(17) Uani 1 1 d . . . . . H15 H 0.2580 0.3624 0.4213 0.034 Uiso 1 1 calc R . . . . C16 C 0.2969(8) 0.4196(2) 0.3297(10) 0.0231(15) Uani 1 1 d . . . . . H16 H 0.2163 0.4311 0.3676 0.028 Uiso 1 1 calc R . . . . C17 C 0.4812(9) 0.3169(3) 0.3468(12) 0.0314(19) Uani 1 1 d . . . . . H17A H 0.4803 0.3020 0.2334 0.038 Uiso 1 1 calc R . . . . H17B H 0.5736 0.3165 0.3943 0.038 Uiso 1 1 calc R . . . . C18 C 0.3940(12) 0.2939(3) 0.4754(18) 0.060(3) Uani 1 1 d . . . . . H18A H 0.3028 0.2929 0.4281 0.089 Uiso 1 1 calc GR . . . . H18B H 0.3955 0.3077 0.5897 0.089 Uiso 1 1 calc GR . . . . H18C H 0.4280 0.2664 0.4907 0.089 Uiso 1 1 calc GR . . . . C21 C 0.1535(7) 0.6434(2) 0.4040(10) 0.0205(15) Uani 1 1 d . . . . . C22 C 0.2683(8) 0.6422(2) 0.2968(9) 0.0195(14) Uani 1 1 d . . . . . C23 C 0.3098(8) 0.6780(3) 0.2146(10) 0.0252(16) Uani 1 1 d . . . . . C24 C 0.2420(9) 0.7148(2) 0.2338(11) 0.0268(17) Uani 1 1 d . . . . . C25 C 0.1291(9) 0.7158(2) 0.3395(11) 0.0283(17) Uani 1 1 d . . . . . C26 C 0.0871(8) 0.6802(3) 0.4226(10) 0.0243(16) Uani 1 1 d . . . . . C27 C 0.1039(8) 0.6052(2) 0.5017(10) 0.0220(15) Uani 1 1 d . . . . . C30 C 0.3493(8) 0.6032(3) 0.2671(10) 0.0245(16) Uani 1 1 d . . . . . 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 0.0214(3) 0.0255(3) 0.0182(2) 0.00321(17) 0.00132(17) -0.00118(17) I2 0.0219(3) 0.0223(2) 0.0201(2) -0.00238(16) 0.00259(17) -0.00021(17) F33 0.033(3) 0.037(3) 0.033(3) 0.001(2) 0.014(2) -0.010(2) F34 0.047(3) 0.026(2) 0.044(3) 0.011(2) 0.000(2) -0.007(2) F35 0.048(3) 0.023(2) 0.055(3) -0.004(2) 0.000(3) 0.011(2) F36 0.035(3) 0.035(3) 0.037(3) -0.005(2) 0.016(2) 0.009(2) O28 0.019(3) 0.031(3) 0.033(3) 0.013(2) -0.002(2) 0.000(2) O29 0.018(3) 0.036(3) 0.036(3) 0.010(3) 0.008(2) -0.001(2) O31 0.025(3) 0.027(3) 0.030(3) -0.008(2) -0.001(2) 0.001(2) O32 0.017(3) 0.033(3) 0.039(3) -0.006(3) 0.002(2) 0.001(2) N1 0.014(3) 0.022(3) 0.025(3) 0.000(2) 0.003(2) -0.005(2) N11 0.022(3) 0.020(3) 0.018(3) -0.004(2) 0.006(2) 0.000(2) C2 0.017(4) 0.026(4) 0.023(4) 0.000(3) 0.002(3) -0.002(3) C3 0.017(4) 0.026(4) 0.022(4) 0.001(3) 0.003(3) 0.004(3) C4 0.022(4) 0.030(4) 0.014(3) 0.000(3) -0.001(3) -0.001(3) C5 0.015(4) 0.032(4) 0.023(4) 0.005(3) 0.003(3) -0.003(3) C6 0.013(4) 0.034(4) 0.025(4) -0.001(3) 0.007(3) -0.001(3) C7 0.031(5) 0.030(4) 0.029(4) 0.006(3) -0.002(3) -0.004(4) C8 0.040(6) 0.029(5) 0.070(7) 0.009(5) 0.012(5) 0.006(4) C12 0.021(4) 0.034(4) 0.020(4) -0.001(3) 0.004(3) -0.005(3) C13 0.028(4) 0.027(4) 0.022(4) -0.004(3) -0.001(3) 0.003(3) C14 0.029(4) 0.029(4) 0.019(4) -0.001(3) -0.002(3) 0.002(3) C15 0.032(5) 0.033(4) 0.021(4) 0.000(3) 0.004(3) -0.007(4) C16 0.021(4) 0.028(4) 0.021(4) -0.002(3) 0.006(3) -0.001(3) C17 0.034(5) 0.027(4) 0.033(5) 0.001(3) 0.004(4) 0.003(4) C18 0.048(7) 0.043(6) 0.088(9) 0.035(6) 0.014(6) 0.006(5) C21 0.018(4) 0.026(4) 0.017(3) -0.001(3) -0.001(3) -0.001(3) C22 0.021(4) 0.018(3) 0.019(3) -0.001(3) 0.000(3) -0.001(3) C23 0.025(4) 0.031(4) 0.020(4) 0.001(3) 0.002(3) -0.003(3) C24 0.034(5) 0.019(4) 0.026(4) 0.004(3) -0.005(3) -0.006(3) C25 0.038(5) 0.017(4) 0.029(4) -0.001(3) -0.004(3) 0.004(3) C26 0.024(4) 0.031(4) 0.018(4) -0.004(3) 0.002(3) 0.002(3) C27 0.023(4) 0.027(4) 0.016(3) -0.001(3) 0.005(3) -0.001(3) C30 0.024(4) 0.032(4) 0.018(4) -0.002(3) 0.010(3) -0.004(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' F F 0.0727 0.0534 '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 -1 -21 0 0.0116 1 21 0 0.0226 0 3 5 0.0688 0 -3 -5 0.0628 4 1 3 0.0928 -4 -1 -3 0.0818 5 -3 -3 0.1418 -6 2 0 0.1589 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 174.1(2) . . ? N11 I2 O31 173.2(2) . . ? C27 O28 I1 120.3(5) . . ? C30 O31 I2 118.3(5) . . ? C2 N1 I1 120.6(5) . . ? C2 N1 C6 119.6(7) . . ? C6 N1 I1 119.8(5) . . ? C12 N11 I2 121.3(5) . . ? C16 N11 I2 119.8(5) . . ? C16 N11 C12 118.8(7) . . ? N1 C2 H2 119.2 . . ? N1 C2 C3 121.7(7) . . ? C3 C2 H2 119.2 . . ? C2 C3 H3 120.0 . . ? C4 C3 C2 120.0(7) . . ? C4 C3 H3 120.0 . . ? C3 C4 C5 117.2(7) . . ? C3 C4 C7 124.1(7) . . ? C5 C4 C7 118.7(7) . . ? C4 C5 H5 119.9 . . ? C6 C5 C4 120.2(7) . . ? C6 C5 H5 119.9 . . ? N1 C6 C5 121.2(7) . . ? N1 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C4 C7 H7A 108.4 . . ? C4 C7 H7B 108.4 . . ? C4 C7 C8 115.6(7) . . ? H7A C7 H7B 107.4 . . ? C8 C7 H7A 108.4 . . ? C8 C7 H7B 108.4 . . ? 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 . . ? N11 C12 H12 119.1 . . ? N11 C12 C13 121.8(7) . . ? C13 C12 H12 119.1 . . ? C12 C13 H13 119.8 . . ? C12 C13 C14 120.5(8) . . ? C14 C13 H13 119.8 . . ? C13 C14 C15 117.4(8) . . ? C13 C14 C17 119.5(8) . . ? C15 C14 C17 123.1(8) . . ? C14 C15 H15 120.3 . . ? C16 C15 C14 119.5(8) . . ? C16 C15 H15 120.3 . . ? N11 C16 C15 122.0(7) . . ? N11 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? C14 C17 H17A 108.2 . . ? C14 C17 H17B 108.2 . . ? H17A C17 H17B 107.3 . . ? C18 C17 C14 116.6(8) . . ? C18 C17 H17A 108.2 . . ? C18 C17 H17B 108.2 . . ? 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(7) . . ? C26 C21 C22 118.5(7) . . ? C26 C21 C27 120.1(7) . . ? C21 C22 C30 122.9(7) . . ? C23 C22 C21 118.7(7) . . ? C23 C22 C30 118.4(7) . . ? F33 C23 C22 121.2(7) . . ? F33 C23 C24 116.5(7) . . ? C24 C23 C22 122.3(8) . . ? F34 C24 C23 121.3(8) . . ? F34 C24 C25 119.9(7) . . ? C23 C24 C25 118.8(7) . . ? F35 C25 C24 119.3(8) . . ? F35 C25 C26 121.3(8) . . ? C26 C25 C24 119.3(7) . . ? F36 C26 C21 121.3(7) . . ? F36 C26 C25 116.2(7) . . ? C21 C26 C25 122.5(8) . . ? O28 C27 C21 112.2(6) . . ? O29 C27 O28 127.7(7) . . ? O29 C27 C21 120.1(7) . . ? O31 C30 C22 112.5(7) . . ? O32 C30 O31 127.2(8) . . ? O32 C30 C22 120.2(7) . . ? 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 2.223(5) . ? I1 N1 2.233(6) . ? I2 O31 2.213(6) . ? I2 N11 2.208(6) . ? F33 C23 1.357(9) . ? F34 C24 1.340(9) . ? F35 C25 1.344(9) . ? F36 C26 1.359(9) . ? O28 C27 1.277(9) . ? O29 C27 1.214(9) . ? O31 C30 1.305(10) . ? O32 C30 1.212(10) . ? N1 C2 1.323(10) . ? N1 C6 1.351(9) . ? N11 C12 1.344(10) . ? N11 C16 1.343(10) . ? C2 H2 0.9300 . ? C2 C3 1.394(11) . ? C3 H3 0.9300 . ? C3 C4 1.379(11) . ? C4 C5 1.398(11) . ? C4 C7 1.506(11) . ? C5 H5 0.9300 . ? C5 C6 1.374(11) . ? C6 H6 0.9300 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 C8 1.510(12) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C12 H12 0.9300 . ? C12 C13 1.370(11) . ? C13 H13 0.9300 . ? C13 C14 1.384(11) . ? C14 C15 1.394(12) . ? C14 C17 1.505(11) . ? C15 H15 0.9300 . ? C15 C16 1.383(12) . ? C16 H16 0.9300 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 C18 1.502(13) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C21 C22 1.403(11) . ? C21 C26 1.374(11) . ? C21 C27 1.524(10) . ? C22 C23 1.382(11) . ? C22 C30 1.516(11) . ? C23 C24 1.379(12) . ? C24 C25 1.381(12) . ? C25 C26 1.379(11) . ? 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 -0.5389 -21.0140 -0.0121 0.0777 -0.9856 0.1503 0.5389 21.0140 0.0121 -0.0777 0.9856 -0.1503 -0.0236 3.1050 4.7726 0.0327 0.0017 -0.9995 0.0236 -3.1050 -4.7726 -0.0327 -0.0017 0.9995 4.3801 1.1062 3.4280 -0.6621 -0.0527 -0.7475 -4.3801 -1.1062 -3.4280 0.6621 0.0527 0.7475 4.7867 -3.3081 -3.2102 -0.7660 -0.0597 0.6401 -6.3826 1.8010 0.2610 0.9969 0.0784 -0.0116 loop_ _hkl_oxdiff_h _hkl_oxdiff_k _hkl_oxdiff_l _hkl_oxdiff_f2 _hkl_oxdiff_sig _hkl_oxdiff_ba 1 0 0 3815.62 188.137 3 2 0 0 116802. 1440.66 3 3 0 0 2042.95 343.020 1 3 0 0 2210.29 252.317 3 4 0 0 107162. 2843.90 1 5 0 0 1128.35 367.977 1 6 0 0 359292. 7151.36 1 7 0 0 1577.66 484.668 1 8 0 0 67.5980 265.934 1 8 0 0 994.899 519.453 8 9 0 0 1091.53 488.497 8 -10 0 0 90359.4 5530.54 7 -11 0 0 7460.28 1377.45 7 -12 0 0 49728.0 2461.70 7 1 1 0 62614.7 1058.46 1 -1 1 0 65999.1 841.191 2 2 1 0 1736.03 248.000 1 2 -1 0 2259.98 214.746 3 3 1 0 397.055 115.752 3 3 1 0 112.828 116.509 1 4 1 0 334.769 183.958 1 4 1 0 467.602 131.140 3 4 -1 0 695.323 259.152 1 5 -1 0 541.503 245.622 1 5 1 0 209.162 168.767 1 6 1 0 16125.1 1643.70 1 6 -1 0 17545.5 1682.92 1 7 1 0 251.285 336.714 1 7 -1 0 -230.797 241.011 1 8 1 0 26.4521 255.703 1 8 -1 0 133.969 245.007 8 8 1 0 410.822 435.038 8 8 -1 0 554.546 399.319 1 9 1 0 695.805 351.029 8 9 -1 0 667.846 398.154 8 -10 1 0 19557.6 2581.41 7 -10 -1 0 14499.5 2388.91 7 -11 -1 0 5269.75 1146.82 7 -11 1 0 5500.56 1094.37 7 -12 -1 0 4955.10 821.980 7 0 2 0 759506. 6492.60 1 1 2 0 5463.51 350.131 1 -1 2 0 4926.04 232.047 2 -2 2 0 170369. 2001.71 2 2 2 0 167478. 2471.07 1 3 2 0 225.436 112.121 1 4 2 0 225483. 4177.57 1 4 2 0 224640. 2905.82 3 5 2 0 16405.4 1321.82 1 5 -2 0 16715.9 1296.53 1 6 2 0 489122. 8228.98 1 6 -2 0 481340. 8148.15 1 7 -2 0 7095.04 1196.20 1 7 2 0 5606.24 1011.22 1 8 2 0 23.4297 275.187 1 8 -2 0 464.208 304.963 8 8 2 0 335.107 269.176 8 8 -2 0 697.841 529.307 1 9 2 0 1836.50 594.877 8 -10 2 0 119942. 5984.02 7 10 2 0 115871. 4446.62 8 -10 -2 0 125943. 6844.29 7 -11 2 0 7785.28 1300.25 7 -11 -2 0 7900.65 1479.02 7 -12 -2 0 52395.0 2888.35 7 0 3 0 202.696 258.697 1 -1 3 0 4419.58 255.180 2 1 3 0 4972.50 389.388 1 -2 3 0 287.367 89.0222 2 2 3 0 190.815 131.225 1 3 3 0 599.039 201.379 1 4 3 0 95038.5 1962.26 3 4 3 0 100832. 2832.45 1 5 3 0 71127.7 2736.90 1 5 -3 0 66182.9 2621.26 1 6 3 0 2514.79 794.396 1 6 -3 0 693.410 508.224 1 7 -3 0 28922.7 2336.40 1 7 3 0 27996.6 2261.84 1 8 -3 0 3273.44 933.342 1 8 3 0 2781.99 665.734 8 8 3 0 3516.82 913.712 1 9 3 0 266.124 327.720 8 -10 3 0 23765.1 2618.85 7 -10 -3 0 28116.5 3427.32 7 -11 3 0 5341.21 1003.20 7 -11 -3 0 5078.26 1247.58 7 -12 -3 0 3035.77 728.256 7 0 4 0 285066. 5429.87 1 1 4 0 3330.58 356.349 1 -1 4 0 3108.08 264.964 2 2 4 0 188796. 2954.94 1 -2 4 0 181348. 2044.44 2 -3 4 0 8772.74 591.018 2 3 4 0 8001.36 721.740 1 4 4 0 309330. 5108.13 1 5 4 0 9733.95 1034.03 1 6 -4 0 233226. 5804.10 1 6 4 0 225614. 5760.07 1 7 -4 0 11393.6 1470.69 1 7 4 0 12315.9 1535.73 1 8 4 0 8318.71 1396.42 1 8 -4 0 6627.80 1314.18 1 8 4 0 6152.91 1057.02 8 9 4 0 10803.7 1431.71 8 -9 4 0 12321.9 1996.01 7 -10 -4 0 109551. 6721.44 7 10 4 0 99890.2 4223.40 8 -10 4 0 99861.6 4988.27 7 -11 -4 0 1840.04 762.870 7 -12 -4 0 47869.9 2942.97 7 0 5 0 258.930 235.425 1 -1 5 0 168268. 2337.62 2 1 5 0 160227. 2803.58 1 2 5 0 53890.8 1682.78 1 -2 5 0 52478.7 1166.57 2 3 5 0 200.194 149.179 1 -3 5 0 167.907 107.713 2 4 5 0 330.759 210.315 1 5 5 0 47971.1 2334.85 1 6 -5 0 771.626 500.241 1 6 5 0 256.915 242.744 1 7 -5 0 43909.6 2911.24 1 7 5 0 37920.7 2685.24 1 8 5 0 -51.6991 348.785 1 8 -5 0 -952.569 501.963 1 9 5 0 4027.15 995.781 8 -9 5 0 2060.12 745.140 7 -10 -5 0 11518.2 2250.30 7 -10 5 0 7204.41 1386.90 7 -11 -5 0 17426.9 2131.88 7 -12 -5 0 2053.07 615.476 7 0 6 0 213014. 4942.83 1 -1 6 0 14223.4 804.319 2 1 6 0 13805.5 957.837 1 2 6 0 29633.7 1320.60 1 -2 6 0 26941.4 920.434 2 -3 6 0 276.945 108.395 2 3 6 0 131.650 122.464 1 4 6 0 392653. 5984.13 1 5 6 0 7984.06 979.211 1 6 -6 0 197400. 5455.37 1 6 6 0 190119. 5391.17 1 7 6 0 3446.94 848.974 1 7 -6 0 3965.82 883.763 1 8 -6 0 7423.11 1402.24 1 8 6 0 5943.54 1184.07 1 8 6 0 6028.24 1092.31 8 9 6 0 1848.34 646.522 8 -10 -6 0 64668.0 4612.44 7 10 6 0 69316.3 3628.07 8 -11 -6 0 2570.11 832.988 7 -12 -6 0 35922.7 2245.43 7 0 7 0 -49.6396 254.348 1 -1 7 0 105791. 2455.30 2 1 7 0 108079. 2889.11 1 2 7 0 1799.76 360.521 1 -2 7 0 1322.73 243.779 2 3 7 0 1003.23 309.515 1 -3 7 0 1117.87 229.711 2 4 7 0 20350.9 1386.67 1 5 7 0 194871. 4866.91 1 6 -7 0 412.370 352.724 1 6 7 0 147.193 205.907 1 7 7 0 29922.9 2444.89 1 7 -7 0 32527.3 2628.10 1 8 7 0 13584.3 1876.68 1 8 7 0 15128.0 1778.82 8 9 7 0 1012.25 468.315 8 -10 -7 0 5117.70 1380.33 7 10 7 0 8955.57 1486.32 8 -11 -7 0 49362.2 3291.37 7 -12 -7 0 1540.99 495.255 7 0 8 0 158338. 4404.99 1 -1 8 0 6844.41 711.023 2 1 8 0 6741.31 860.739 1 -2 8 0 72459.6 1871.41 2 2 8 0 78245.5 2520.31 1 -3 8 0 20075.7 973.223 2 3 8 0 19455.8 1291.91 1 -4 8 0 149356. 2993.03 2 4 8 0 149794. 3940.03 1 5 8 0 19664.8 1594.78 1 6 8 0 123787. 4511.58 1 7 8 0 16215.7 1859.74 1 7 -8 0 18972.2 2078.92 1 8 8 0 1327.63 620.998 1 8 8 0 2485.30 748.575 8 9 8 0 9203.58 1415.29 8 10 8 0 77698.2 4022.30 8 -10 -8 0 71757.7 4497.85 7 -11 -8 0 4944.32 1020.23 7 -12 -8 0 13572.3 1252.41 7 0 9 0 130.401 227.659 1 1 9 0 352658. 6655.32 1 -1 9 0 314216. 5284.77 2 2 9 0 31245.0 1722.14 1 -2 9 0 30452.2 1343.98 2 3 9 0 173.385 199.074 1 -3 9 0 67.0174 69.8750 2 4 9 0 737.293 300.892 1 -4 9 0 699.088 230.139 2 5 9 0 132885. 4282.83 1 6 9 0 10320.7 1371.28 1 7 -9 0 92393.6 4526.37 1 7 9 0 91822.3 4339.57 8 7 9 0 88924.1 4378.28 1 8 9 0 31553.7 2906.57 1 8 9 0 32703.2 2765.83 8 9 9 0 26732.8 2545.14 8 10 9 0 13996.2 1818.02 8 -10 -9 0 14870.2 2116.33 7 -11 -9 0 39141.8 2711.55 7 -12 -9 0 605.100 256.848 7 0 10 0 377713. 7076.16 1 1 10 0 40917.0 2299.21 1 -1 10 0 44437.5 2204.10 2 2 10 0 1957.14 505.152 1 -2 10 0 2234.24 418.748 2 -3 10 0 45400.5 1649.29 2 3 10 0 50301.3 2359.54 1 4 10 0 19861.2 1568.17 1 5 10 0 3786.54 775.142 1 6 10 0 115165. 4645.39 1 7 10 0 39653.3 2975.52 8 7 10 0 39210.3 3022.74 1 7 -10 0 39086.9 3124.58 1 8 10 0 1635.41 675.375 1 8 10 0 652.678 436.101 8 9 10 0 38732.7 3193.11 8 10 10 0 9313.93 1537.39 8 -10 -10 0 11516.2 1719.78 7 -11 -10 0 2330.72 706.856 7 -12 -10 0 6486.34 768.418 7 0 11 0 -16.0695 221.068 1 1 11 0 172614. 4921.12 1 -1 11 0 200153. 5063.41 2 -2 11 0 6905.96 791.486 2 2 11 0 7689.88 1013.07 1 -3 11 0 33872.1 1550.75 2 3 11 0 34606.6 2077.33 1 4 11 0 38445.5 2269.37 1 5 11 0 242623. 6313.45 1 6 11 0 381.464 306.656 1 7 11 0 64905.2 3958.05 8 7 -11 0 63490.8 4006.30 1 7 11 0 63964.8 3930.05 1 8 11 0 509.369 238.473 8 9 11 0 34514.9 3116.73 8 10 11 0 7496.26 1421.95 8 -10 -11 0 8895.08 1459.08 7 -11 -11 0 49529.3 2829.32 7 11 11 0 43949.8 2876.27 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