#------------------------------------------------------------------------------ #$Date: 2019-11-11 20:29:26 +0200 (Mon, 11 Nov 2019) $ #$Revision: 227273 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/58/4035861.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_4035861 loop_ _publ_author_name 'Bookser, Brett C.' 'Weinhouse, Michael I.' 'Burns, Aaron C.' 'Valiere, Andrew N.' 'Valdez, Lino J.' 'Stanczak, Pawel' 'Na, Jim' 'Rheingold, Arnold L.' 'Moore, Curtis E.' 'Dyck, Brian' _publ_section_title ; Solvent-Controlled, Site-Selective N-Alkylation Reactions of Azolo-Fused Ring Heterocycles at N1-, N2-, and N3-Positions, Including Pyrazolo[3,4- d]pyrimidines, Purines, [1,2,3]Triazolo[4,5]pyridines, and Related Deaza-Compounds. ; _journal_issue 12 _journal_name_full 'The Journal of organic chemistry' _journal_page_first 6334 _journal_page_last 6353 _journal_paper_doi 10.1021/acs.joc.8b00540 _journal_volume 83 _journal_year 2018 _chemical_formula_moiety 'C28 H36 I3 N16 Na3 O6' _chemical_formula_sum 'C28 H36 I3 N16 Na3 O6' _chemical_formula_weight 1142.40 _space_group_crystal_system orthorhombic _space_group_IT_number 60 _space_group_name_Hall '-P 2n 2ab' _space_group_name_H-M_alt 'P b c n' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_date 2017-10-09 _audit_creation_method ; Olex2 1.2-beta (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 16.1345(9) _cell_length_b 17.9552(8) _cell_length_c 13.8025(7) _cell_measurement_reflns_used 9949 _cell_measurement_temperature 100.0 _cell_measurement_theta_max 26.370 _cell_measurement_theta_min 2.249 _cell_volume 3998.6(4) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2016)' _computing_data_collection 'APEX3 v2016.1-0 (Bruker, 2016)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2016)' _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_temperature 100.0 _diffrn_detector 'Bruker APEX-II CCD' _diffrn_detector_area_resol_mean 8.258 _diffrn_detector_type 'CCD Area Detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device 'Kappa Four-Circle Diffractometer' _diffrn_measurement_device_type 'Bruker APEX II Ultra' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'Double Bounce Multilayer Mirrors' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_unetI/netI 0.0345 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 26596 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 26.388 _diffrn_reflns_theta_min 2.249 _diffrn_source 'Micro Focus Rotating Anode' _diffrn_source_type 'Bruker TXS' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.440 _exptl_absorpt_correction_T_max 0.2602 _exptl_absorpt_correction_T_min 0.2112 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0886 before and 0.0623 after correction. The Ratio of minimum to maximum transmission is 0.8117. The \l/2 correction factor is Not present.' _exptl_crystal_colour Colorless _exptl_crystal_colour_primary Colorless _exptl_crystal_density_diffrn 1.898 _exptl_crystal_description Block _exptl_crystal_F_000 2224 _exptl_crystal_size_max 0.157 _exptl_crystal_size_mid 0.053 _exptl_crystal_size_min 0.049 _refine_diff_density_max 0.723 _refine_diff_density_min -0.583 _refine_diff_density_rms 0.092 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 266 _refine_ls_number_reflns 4089 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all 0.0288 _refine_ls_R_factor_gt 0.0226 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0168P)^2^+3.5957P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.0547 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3554 _reflns_number_total 4089 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jo8b00540_si_011.cif _cod_data_source_block Dart196 _cod_depositor_comments ; The following automatic conversions were performed: data item '_diffrn_radiation_probe' value 'X-ray' was changed to 'x-ray' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas ; _cod_database_code 4035861 _shelx_shelxl_version_number 2017/1 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.890 _shelx_estimated_absorpt_t_min 0.701 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances O1S-H1SA = O1S-H1SB 0.95 with sigma of 0.02 H1SB-H1SA 1.4 with sigma of 0.02 3.a Aromatic/amide H refined with riding coordinates: C6B(H6B), C6(H6), C3B(H3B), C3(H3) 3.b Idealised Me refined as rotating group: C9B(H9BA,H9BB,H9BC), C9(H9A,H9B,H9C), C8B(H8BA,H8BB,H8BC), C8(H8A,H8B,H8C) ; _shelx_res_file ; TITL dart196_a.res in Pbcn dart196.res created by SHELXL-2017/1 at 14:04:39 on 09-Oct-2017 REM Old TITL Dart196 in Pbcn REM SHELXT solution in Pbcn REM R1 0.074, Rweak 0.001, Alpha 0.023, Orientation as input REM Formula found by SHELXT: C42 N8 Na3 I3 CELL 0.71073 16.1345 17.9552 13.8025 90 90 90 ZERR 4 0.0009 0.0008 0.0007 0 0 0 LATT 1 SYMM 0.5-X,0.5-Y,0.5+Z SYMM -X,+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H I N Na O UNIT 112 144 12 64 12 24 EQIV $1 1-X,+Y,0.5-Z DFIX 0.95 O1S H1Sa O1S H1Sb DFIX 1.4 H1Sb H1Sa L.S. 10 PLAN 20 SIZE 0.157 0.053 0.049 TEMP -173.15 HTAB O1S N7 HTAB O1S N7_$1 BOND $H list 4 fmap 2 acta 50 REM REM REM WGHT 0.016800 3.595700 FVAR 0.14203 I2 3 0.500000 0.675210 0.750000 10.50000 0.01808 0.01879 = 0.02218 0.00000 -0.00484 0.00000 I1 3 0.463884 0.759510 0.072869 11.00000 0.01530 0.01403 = 0.02149 0.00044 0.00200 -0.00176 NA2 5 0.503958 0.595693 0.522757 11.00000 0.01217 0.01579 = 0.01793 -0.00085 0.00136 0.00047 NA1 5 0.500000 0.662438 0.250000 10.50000 0.01420 0.02088 = 0.02473 0.00000 0.00003 0.00000 O1B 6 0.891910 0.548532 0.391221 11.00000 0.00905 0.01549 = 0.02032 -0.00073 0.00342 -0.00154 O1 6 0.107417 0.512589 0.348704 11.00000 0.01104 0.01485 = 0.02431 0.00116 0.00090 -0.00198 O1S 6 0.503624 0.526766 0.372971 11.00000 0.01139 0.03705 = 0.02135 -0.01337 -0.00186 0.00270 H1SA 2 0.547742 0.512745 0.338202 11.00000 0.02610 H1SB 2 0.461663 0.512813 0.334849 11.00000 0.02977 N7B 4 0.652647 0.561552 0.496821 11.00000 0.01215 0.01324 = 0.01445 0.00011 -0.00188 0.00133 N7 4 0.352598 0.511616 0.263999 11.00000 0.01135 0.01495 = 0.01362 0.00024 -0.00078 0.00095 N5B 4 0.782787 0.618592 0.449529 11.00000 0.01253 0.01224 = 0.01705 0.00030 0.00098 0.00003 N5 4 0.224734 0.448553 0.303651 11.00000 0.01460 0.01336 = 0.01194 -0.00030 -0.00116 -0.00100 N1B 4 0.649270 0.428073 0.477984 11.00000 0.01217 0.01415 = 0.01211 0.00086 0.00025 0.00174 N1 4 0.346872 0.644670 0.276996 11.00000 0.01454 0.01310 = 0.01506 0.00058 -0.00041 0.00004 N2B 4 0.709902 0.379418 0.449899 11.00000 0.01362 0.01058 = 0.01265 -0.00014 0.00008 0.00129 N2 4 0.283950 0.691157 0.302627 11.00000 0.01582 0.01077 = 0.01519 0.00201 -0.00052 0.00061 C6B 1 0.703564 0.617832 0.483892 11.00000 0.01260 0.01434 = 0.01543 -0.00311 -0.00203 0.00042 AFIX 43 H6B 2 0.681854 0.665197 0.501118 11.00000 -1.20000 AFIX 0 C6 1 0.305787 0.452285 0.276365 11.00000 0.01253 0.01385 = 0.01307 -0.00148 -0.00303 0.00165 AFIX 43 H6 2 0.332087 0.405807 0.264681 11.00000 -1.20000 AFIX 0 C7AB 1 0.688141 0.494303 0.474049 11.00000 0.01280 0.01372 = 0.00921 0.00016 -0.00206 0.00029 C7A 1 0.311829 0.577041 0.282938 11.00000 0.01331 0.01591 = 0.00757 0.00127 -0.00153 0.00078 C3AB 1 0.770914 0.486677 0.442267 11.00000 0.01240 0.01277 = 0.00944 -0.00065 -0.00202 0.00109 C3A 1 0.228001 0.580849 0.311932 11.00000 0.01089 0.01397 = 0.01231 0.00086 -0.00022 0.00163 C4B 1 0.815606 0.553770 0.427974 11.00000 0.01078 0.01746 = 0.00951 0.00007 -0.00194 -0.00140 C4 1 0.186134 0.511678 0.321365 11.00000 0.01261 0.01457 = 0.00915 0.00072 -0.00137 -0.00255 C3B 1 0.782397 0.410728 0.428523 11.00000 0.01148 0.01529 = 0.01291 -0.00076 -0.00141 0.00086 AFIX 43 H3B 2 0.831627 0.386289 0.408156 11.00000 -1.20000 AFIX 0 C3 1 0.212760 0.656807 0.324011 11.00000 0.01476 0.01752 = 0.01392 -0.00068 -0.00045 0.00120 AFIX 43 H3 2 0.162196 0.679435 0.343434 11.00000 -1.20000 AFIX 0 C9B 1 0.935270 0.618294 0.371335 11.00000 0.01402 0.01893 = 0.02305 0.00122 0.00170 -0.00669 AFIX 137 H9BA 2 0.903158 0.647800 0.324871 11.00000 -1.50000 H9BB 2 0.990045 0.607433 0.344100 11.00000 -1.50000 H9BC 2 0.941696 0.646453 0.431693 11.00000 -1.50000 AFIX 0 C9 1 0.066610 0.440516 0.358205 11.00000 0.01200 0.01730 = 0.02660 0.00035 0.00048 -0.00519 AFIX 137 H9A 2 0.067713 0.414647 0.295698 11.00000 -1.50000 H9B 2 0.008994 0.447943 0.378498 11.00000 -1.50000 H9C 2 0.095692 0.410510 0.406804 11.00000 -1.50000 AFIX 0 C8B 1 0.689251 0.299986 0.442130 11.00000 0.01718 0.01025 = 0.02034 0.00136 -0.00133 -0.00161 AFIX 137 H8BA 2 0.660812 0.283807 0.501232 11.00000 -1.50000 H8BB 2 0.740243 0.271029 0.433811 11.00000 -1.50000 H8BC 2 0.652917 0.292115 0.386161 11.00000 -1.50000 AFIX 0 C8 1 0.299027 0.771464 0.303200 11.00000 0.02288 0.00993 = 0.02581 0.00157 0.00217 -0.00042 AFIX 137 H8A 2 0.340466 0.783424 0.352724 11.00000 -1.50000 H8B 2 0.247243 0.797703 0.317755 11.00000 -1.50000 H8C 2 0.319475 0.787083 0.239505 11.00000 -1.50000 AFIX 0 HKLF 4 REM dart196_a.res in Pbcn REM R1 = 0.0226 for 3554 Fo > 4sig(Fo) and 0.0288 for all 4089 data REM 266 parameters refined using 3 restraints END WGHT 0.0168 3.5953 REM Highest difference peak 0.723, deepest hole -0.583, 1-sigma level 0.092 Q1 1 0.5399 0.6968 0.7025 11.00000 0.05 0.72 Q2 1 0.2075 0.5483 0.3379 11.00000 0.05 0.48 Q3 1 0.4716 0.7305 -0.0065 11.00000 0.05 0.40 Q4 1 0.7372 0.4988 0.4573 11.00000 0.05 0.37 Q5 1 0.7965 0.5170 0.4541 11.00000 0.05 0.37 Q6 1 0.5151 0.7360 0.0867 11.00000 0.05 0.36 Q7 1 0.6665 0.4028 0.4605 11.00000 0.05 0.36 Q8 1 0.2667 0.5798 0.2939 11.00000 0.05 0.35 Q9 1 0.5005 0.6643 0.8454 11.00000 0.05 0.35 Q10 1 0.7838 0.4568 0.4425 11.00000 0.05 0.35 Q11 1 0.7918 0.5128 0.4219 11.00000 0.05 0.34 Q12 1 0.4576 0.7490 0.1628 11.00000 0.05 0.34 Q13 1 0.3954 0.5248 0.2444 11.00000 0.05 0.34 Q14 1 0.2181 0.6109 0.3381 11.00000 0.05 0.33 Q15 1 0.8483 0.5525 0.3842 11.00000 0.05 0.33 Q16 1 0.5461 0.7085 0.6273 11.00000 0.05 0.33 Q17 1 0.5000 0.7319 0.7500 10.50000 0.05 0.32 Q18 1 0.3227 0.6096 0.2680 11.00000 0.05 0.32 Q19 1 0.4567 0.8134 0.0711 11.00000 0.05 0.32 Q20 1 0.3698 0.7134 0.3794 11.00000 0.05 0.31 ; _shelx_res_checksum 68443 _shelx_hkl_file ; 1 0 0 0.10 0.20 1 0 0 0.00 0.20 2 0 0 463.25 27.90 2 0 0 504.55 27.90 -2 0 0 398.16 27.80 3 0 0 0.90 0.70 -3 0 0 -0.60 0.70 3 0 0 1.20 0.80 -3 0 0 -0.40 0.60 4 0 0 7357.06 416.06 4 0 0 6679.73 415.86 -4 0 0 6291.07 417.86 -4 0 0 7212.98 415.96 5 0 0 3.60 1.20 -5 0 0 1.90 1.10 5 0 0 0.20 1.00 -5 0 0 0.60 1.00 6 0 0 3811.52 229.48 -6 0 0 3589.54 229.48 6 0 0 3963.00 229.68 7 0 0 1.20 1.20 7 0 0 0.30 1.10 -7 0 0 1.00 1.20 8 0 0 61.19 5.60 8 0 0 66.59 5.70 9 0 0 1.60 1.30 9 0 0 -1.50 1.10 -11 0 0 1.10 1.60 -12 0 0 157.68 12.50 -13 0 0 1.50 2.00 -14 0 0 26.90 5.10 -15 0 0 1.20 2.30 -16 0 0 54.89 7.60 -17 0 0 1.50 2.40 -18 0 0 66.89 9.00 -19 0 0 -0.40 2.70 -20 0 0 204.28 17.60 2 1 0 0.00 0.40 2 -1 0 0.60 0.50 -2 -1 0 -0.40 0.30 2 1 0 0.60 0.50 -2 1 0 0.00 0.50 -3 1 0 149.09 9.80 3 1 0 136.69 9.50 -3 -1 0 147.19 9.60 3 1 0 146.69 9.50 3 -1 0 155.88 9.80 4 -1 0 1.40 1.20 4 1 0 0.50 0.90 4 1 0 0.30 0.90 -4 1 0 0.20 1.20 -4 -1 0 0.90 1.10 -5 -1 0 1571.24 99.19 5 -1 0 1604.84 99.29 5 1 0 1598.44 99.19 5 -1 0 1861.51 99.59 -5 1 0 1567.94 99.39 5 1 0 1567.14 99.09 -6 1 0 3.10 1.50 6 -1 0 1.40 1.20 -6 -1 0 1.30 1.20 6 1 0 -0.50 1.00 6 1 0 -0.20 1.00 6 -1 0 -1.00 1.00 7 1 0 3006.20 190.58 7 -1 0 3264.17 190.78 -7 -1 0 3414.36 190.88 -7 1 0 2805.82 190.78 7 -1 0 3404.36 191.08 7 1 0 2958.50 190.68 8 1 0 -0.70 1.30 -8 1 0 0.90 1.30 8 -1 0 -0.90 1.10 -8 -1 0 -1.50 0.90 8 1 0 1.00 1.30 8 -1 0 1.10 1.40 9 -1 0 6.70 2.20 9 1 0 11.20 2.50 9 1 0 5.30 1.90 -9 -1 0 -0.20 1.30 9 -1 0 2.10 1.90 10 1 0 1.10 1.60 -10 1 0 0.80 1.20 10 1 0 -0.10 1.70 -11 -1 0 512.85 32.50 -11 1 0 469.45 32.40 -12 -1 0 0.00 1.30 -12 1 0 1.40 1.80 -13 1 0 250.77 18.80 -13 -1 0 266.97 18.90 -14 1 0 0.50 1.80 -14 -1 0 -0.80 2.00 -15 -1 0 462.95 32.70 -15 1 0 497.15 33.10 -16 1 0 -1.50 2.00 -16 -1 0 2.10 2.70 -17 1 0 4.50 2.80 -17 -1 0 3.20 2.70 -18 -1 0 6.20 3.50 -18 1 0 3.30 3.20 -19 -1 0 80.09 10.10 -19 1 0 72.29 9.80 -20 -1 0 3.40 3.70 -20 1 0 -0.80 3.00 -1 2 0 -0.30 0.40 -1 -2 0 0.00 0.20 1 2 0 -0.10 0.20 1 -2 0 -0.10 0.30 1 2 0 0.20 0.30 -2 2 0 5475.95 314.47 2 2 0 5180.38 313.77 -2 -2 0 4713.33 314.67 2 -2 0 5372.46 314.37 -3 2 0 0.00 0.80 3 2 0 0.00 0.50 -3 -2 0 -0.50 0.60 3 -2 0 0.00 0.80 3 2 0 -1.00 0.50 -4 2 0 2613.04 167.28 4 2 0 2819.22 166.78 -4 -2 0 2984.80 166.98 4 2 0 2757.02 166.88 4 -2 0 2610.54 167.28 -5 -2 0 -1.00 0.90 5 2 0 0.30 0.90 -5 2 0 0.00 0.90 5 -2 0 -0.20 1.00 5 2 0 2.70 1.00 6 -2 0 278.57 17.10 6 2 0 219.18 16.30 -6 2 0 240.28 17.00 6 2 0 252.07 16.50 -6 -2 0 281.67 16.80 7 -2 0 -1.20 1.10 7 2 0 -2.20 0.80 7 2 0 0.10 0.80 -7 2 0 1.50 1.40 7 -2 0 -0.10 1.00 -7 -2 0 2.40 1.40 8 2 0 33.50 4.00 -8 2 0 26.60 4.10 8 -2 0 31.60 4.30 8 -2 0 33.20 4.20 8 2 0 34.50 4.00 -8 -2 0 31.00 4.10 9 -2 0 0.70 1.80 -9 -2 0 -0.90 1.50 9 2 0 3.40 1.60 9 2 0 0.30 1.00 -9 2 0 -1.30 1.10 10 2 0 354.36 25.10 10 2 0 409.46 25.60 -10 2 0 424.96 26.20 -10 -2 0 352.56 25.60 -11 -2 0 -1.00 1.30 -11 -2 0 0.20 1.70 -11 2 0 0.90 1.50 -12 -2 0 571.24 37.40 -12 2 0 570.84 37.60 -13 2 0 -0.40 1.70 -13 -2 0 0.20 1.80 -14 2 0 419.56 27.20 -14 -2 0 348.07 26.30 -15 -2 0 1.40 2.20 -15 2 0 0.90 2.10 -16 -2 0 294.07 20.70 -16 2 0 250.17 20.30 -17 2 0 1.70 2.80 -17 -2 0 -0.10 2.50 -18 2 0 96.49 11.70 -18 -2 0 113.49 10.90 -19 2 0 0.50 2.90 -19 -2 0 3.60 3.30 -20 -2 0 -0.70 2.90 0 -3 0 0.80 0.40 0 3 0 0.10 0.40 0 3 0 0.20 0.30 -1 3 0 628.84 39.20 1 -3 0 606.84 39.50 1 3 0 663.03 39.20 -1 -3 0 650.73 39.10 1 3 0 631.34 39.00 -1 -3 0 635.84 39.20 -1 3 0 657.13 39.50 1 -3 0 679.83 39.50 2 -3 0 0.80 0.80 2 3 0 0.70 0.60 -2 3 0 -0.20 0.70 -2 -3 0 1.00 0.60 -3 3 0 78.69 6.10 -3 -3 0 86.59 5.80 3 -3 0 73.49 6.00 3 3 0 89.49 5.70 4 3 0 0.30 0.70 -4 3 0 0.80 1.10 4 3 0 -0.20 0.80 -4 -3 0 0.50 1.00 4 -3 0 2.50 1.30 -5 -3 0 401.06 25.50 5 -3 0 425.36 26.00 5 3 0 391.66 25.20 5 3 0 414.76 25.20 -5 3 0 379.16 25.80 6 3 0 1.40 1.00 -6 -3 0 0.70 1.10 6 -3 0 -0.40 1.10 -6 3 0 0.00 1.20 6 3 0 0.00 0.90 -7 -3 0 189.88 13.70 7 3 0 211.28 13.50 -7 3 0 192.08 14.20 7 3 0 204.58 13.60 7 -3 0 198.78 14.10 8 3 0 -0.90 0.90 -8 -3 0 -1.00 0.90 -8 3 0 -0.70 1.20 8 -3 0 0.60 1.50 8 3 0 1.20 1.30 -9 3 0 1156.98 76.99 9 3 0 1209.08 76.29 -9 -3 0 1300.57 76.79 -9 3 0 1198.08 76.99 9 3 0 1318.47 76.49 -10 3 0 1.00 1.70 -10 -3 0 2.10 1.70 -10 3 0 1.50 1.70 10 3 0 -0.10 1.30 10 3 0 1.50 1.50 -11 3 0 647.64 39.80 11 3 0 550.84 39.20 -11 -3 0 602.54 39.20 -11 -3 0 623.64 39.40 -12 -3 0 0.70 1.60 -12 3 0 -0.70 1.50 -12 -3 0 -1.60 1.70 -13 -3 0 294.87 19.70 -13 3 0 268.57 20.00 -13 -3 0 250.27 19.50 -14 -3 0 0.90 1.90 -14 3 0 -1.20 1.10 -15 3 0 125.09 11.90 -15 -3 0 149.88 12.10 -16 -3 0 1.60 2.10 -16 3 0 -1.40 1.80 -17 -3 0 346.87 24.00 -17 3 0 298.57 23.80 -18 3 0 -1.90 2.40 -18 -3 0 -0.40 2.60 -19 3 0 148.59 13.70 -19 -3 0 135.49 13.10 0 4 0 1665.93 100.29 0 -4 0 1665.63 100.59 0 4 0 1655.23 100.59 -1 -4 0 -0.70 0.40 1 -4 0 -0.80 0.80 -1 4 0 1.20 0.60 1 4 0 0.50 0.50 -1 4 0 0.60 1.00 1 -4 0 -0.30 0.60 -1 -4 0 -0.20 0.60 -1 4 0 1.00 0.70 -2 4 0 1343.77 79.39 2 4 0 1266.87 79.09 2 4 0 1291.57 78.99 -2 4 0 1313.67 79.69 2 -4 0 1337.27 79.69 -2 -4 0 1286.07 79.29 -3 4 0 -0.30 0.70 -3 -4 0 1.50 0.90 3 -4 0 -0.10 0.80 3 4 0 0.20 0.70 -3 4 0 0.40 1.00 4 4 0 17.20 2.10 -4 4 0 20.10 2.90 4 -4 0 16.00 2.60 -4 -4 0 19.00 2.30 -5 4 0 1.80 1.40 5 4 0 -0.70 0.80 -5 -4 0 0.80 1.00 5 4 0 1.40 0.80 5 -4 0 -0.40 0.90 6 4 0 4.80 1.30 -6 4 0 6.00 1.90 6 4 0 5.40 1.30 -6 -4 0 5.20 1.60 6 -4 0 4.50 1.70 -7 -4 0 0.50 1.10 -7 4 0 0.00 1.10 7 -4 0 2.00 1.40 7 4 0 -0.90 0.70 7 4 0 1.00 0.90 -8 4 0 178.98 14.00 -8 -4 0 194.88 13.70 8 4 0 184.48 13.20 -8 4 0 233.38 14.50 8 4 0 195.28 13.30 -9 4 0 -0.20 1.30 9 4 0 0.90 1.40 -9 -4 0 2.20 1.60 9 4 0 1.60 1.10 -9 4 0 1.70 1.60 -10 4 0 885.61 49.00 10 4 0 702.53 47.30 -10 -4 0 750.12 47.90 10 4 0 769.02 47.50 -10 4 0 680.73 48.00 11 4 0 -0.50 1.40 11 4 0 -1.10 1.70 -11 -4 0 0.00 1.20 -11 4 0 -0.80 1.60 -11 -4 0 1.50 1.80 -11 4 0 0.80 1.80 -12 4 0 922.81 59.99 -12 -4 0 942.91 59.79 -12 -4 0 953.60 59.59 -13 4 0 2.50 2.40 -13 -4 0 -1.70 1.70 -13 -4 0 -0.60 1.60 -14 -4 0 2112.89 136.39 -14 4 0 2266.37 136.99 -14 -4 0 2231.68 136.39 -15 -4 0 -0.70 1.80 -15 4 0 -0.40 2.20 -15 -4 0 -1.80 1.80 -16 4 0 338.57 26.50 -16 -4 0 406.46 26.70 -17 -4 0 1.10 2.40 -17 4 0 1.70 2.60 -18 4 0 376.36 27.60 -18 -4 0 373.76 27.20 -19 -4 0 0.30 2.70 -19 4 0 1.60 2.40 0 5 0 1.10 0.40 0 5 0 -0.10 0.80 0 -5 0 0.00 0.50 0 5 0 1.00 0.70 -1 -5 0 8.70 1.40 1 -5 0 8.60 1.50 -1 5 0 9.60 1.20 1 -5 0 8.50 1.70 -1 -5 0 8.40 1.20 -1 5 0 8.30 1.50 1 5 0 8.50 1.10 -1 5 0 10.60 1.90 -2 -5 0 0.50 0.70 2 5 0 0.40 0.50 -2 5 0 0.50 0.90 2 -5 0 1.20 1.10 2 5 0 0.60 0.60 -2 5 0 1.00 0.70 2 -5 0 1.30 1.00 3 5 0 81.09 5.60 3 -5 0 85.09 6.30 -3 5 0 94.29 6.50 3 5 0 79.19 5.40 -3 5 0 71.29 5.90 -3 -5 0 88.69 6.00 4 5 0 -0.50 0.70 -4 5 0 -0.40 0.80 -4 5 0 0.60 1.10 4 -5 0 2.10 1.20 -4 -5 0 -0.60 0.60 -5 5 0 154.28 11.80 5 5 0 177.08 10.80 5 5 0 179.98 11.00 -5 5 0 156.48 11.50 -5 -5 0 157.98 11.30 5 -5 0 161.38 11.80 -6 5 0 1.10 1.20 6 5 0 -0.10 0.70 -6 5 0 -0.50 1.20 6 5 0 0.10 0.80 6 -5 0 0.70 1.30 -6 -5 0 0.00 1.00 -7 5 0 14.50 3.00 -7 -5 0 14.60 2.60 7 5 0 15.20 2.30 7 -5 0 14.30 3.00 -7 5 0 12.20 2.50 7 5 0 11.50 2.00 -8 5 0 0.00 1.50 8 5 0 -0.50 1.00 -8 -5 0 1.70 1.30 8 5 0 1.10 1.30 -8 5 0 2.00 1.30 -9 5 0 161.98 13.10 -9 -5 0 155.38 12.50 9 5 0 182.08 12.20 -9 5 0 205.68 13.40 9 5 0 170.58 12.10 -10 5 0 -0.80 1.30 -10 -5 0 0.80 1.60 10 5 0 3.00 1.70 -10 -5 0 0.30 1.30 10 5 0 0.40 1.40 -10 5 0 1.00 1.80 -11 5 0 97.69 9.20 -11 -5 0 96.29 8.70 -11 -5 0 113.59 9.20 11 5 0 114.59 8.50 11 5 0 103.99 8.50 -11 5 0 110.79 9.60 -12 5 0 -0.20 1.90 -12 -5 0 1.10 1.80 -12 -5 0 3.10 1.90 -13 -5 0 485.95 31.50 -13 -5 0 458.15 31.50 -13 5 0 458.95 31.90 -14 5 0 1.50 2.30 -14 -5 0 2.60 2.20 -14 -5 0 -0.40 2.20 -15 -5 0 191.48 17.00 -15 -5 0 235.28 17.20 -15 5 0 246.38 18.00 -16 -5 0 2.00 2.40 -16 -5 0 -3.20 1.90 -16 5 0 -1.40 2.30 -17 5 0 136.99 12.90 -17 -5 0 155.58 13.00 -18 -5 0 0.20 2.70 -18 5 0 0.30 2.70 -19 5 0 24.80 6.30 -19 -5 0 26.90 5.80 0 -6 0 687.53 42.80 0 -6 0 751.22 43.00 0 6 0 720.53 42.90 0 6 0 703.43 42.40 0 6 0 619.64 43.30 1 6 0 -0.40 0.60 -1 -6 0 1.20 0.80 -1 6 0 1.40 0.90 -1 6 0 0.80 0.60 -1 -6 0 0.60 0.60 1 -6 0 -0.50 0.70 -1 6 0 3.60 1.50 -2 6 0 270.17 16.30 -2 -6 0 241.08 16.30 -2 -6 0 265.27 15.60 -2 6 0 259.27 16.60 2 -6 0 259.17 16.60 2 6 0 249.88 15.80 2 -6 0 230.78 16.80 3 6 0 -0.50 0.40 3 6 0 0.20 0.70 -3 6 0 0.40 0.80 -3 -6 0 -0.10 0.80 3 -6 0 1.00 1.00 3 -6 0 1.70 1.10 -3 6 0 0.40 1.10 -4 6 0 138.89 9.90 4 6 0 136.29 9.40 -4 6 0 132.89 10.30 4 -6 0 159.28 10.40 -4 -6 0 148.79 9.80 5 -6 0 2.80 1.50 5 6 0 0.00 0.80 -5 -6 0 -0.60 0.90 -5 6 0 -0.10 1.20 -5 6 0 0.40 1.10 -6 6 0 174.88 11.70 -6 -6 0 166.08 10.90 6 -6 0 162.98 11.50 6 6 0 134.69 10.10 6 6 0 149.88 10.00 -6 6 0 141.49 10.90 -7 6 0 -1.10 1.00 -7 -6 0 -0.20 1.10 -7 6 0 -0.50 1.20 7 6 0 -0.50 1.00 7 6 0 0.10 0.90 -8 -6 0 773.82 50.19 -8 6 0 837.82 50.79 8 6 0 770.12 49.70 8 6 0 803.02 49.70 -8 6 0 828.52 51.19 9 6 0 -0.10 1.10 -9 -6 0 -0.60 0.90 -9 6 0 -0.90 0.80 9 6 0 0.30 1.10 -9 -6 0 -0.60 1.10 -9 6 0 -0.50 1.50 -10 -6 0 1333.27 83.29 -10 6 0 1389.76 84.19 10 6 0 1395.76 82.89 -10 6 0 1288.47 84.29 10 6 0 1377.46 82.79 -10 -6 0 1274.47 83.49 11 6 0 -0.40 1.30 -11 -6 0 0.30 1.60 -11 6 0 0.10 1.60 11 6 0 -0.20 1.60 -11 6 0 -0.10 1.70 -11 -6 0 0.30 1.60 12 6 0 1482.05 89.99 -12 -6 0 1386.66 90.29 -12 -6 0 1376.16 90.59 -12 6 0 1682.23 92.09 12 6 0 1425.26 89.79 -12 6 0 1393.56 91.09 -13 -6 0 1.10 2.10 -13 6 0 1.40 2.30 -13 -6 0 2.10 2.00 -14 6 0 859.41 56.99 -14 -6 0 924.51 56.89 -14 -6 0 863.11 56.39 -15 -6 0 -1.20 2.10 -15 6 0 0.40 2.10 -15 -6 0 1.20 2.10 -16 -6 0 917.11 56.99 -16 -6 0 812.12 55.99 -16 6 0 885.71 57.09 -17 -6 0 -4.50 2.50 -17 6 0 -2.30 2.20 -17 -6 0 -2.10 1.80 -18 -6 0 332.17 24.10 -18 6 0 317.97 24.70 -19 -6 0 2.00 3.00 -19 6 0 0.40 2.60 0 7 0 0.70 0.50 0 7 0 0.80 1.40 0 -7 0 -0.20 0.80 0 7 0 0.10 0.80 0 -7 0 -0.20 0.60 -1 7 0 460.35 28.00 -1 -7 0 457.25 28.40 -1 7 0 462.15 28.60 1 -7 0 459.65 28.50 -1 -7 0 447.86 28.10 1 7 0 455.65 28.10 -1 7 0 429.36 29.00 2 -7 0 0.30 1.00 -2 -7 0 -0.10 0.60 -2 -7 0 0.70 0.80 2 -7 0 0.80 1.00 -2 7 0 0.80 1.10 -2 7 0 0.30 0.80 2 7 0 0.20 0.50 -3 7 0 405.56 27.90 3 -7 0 476.75 28.30 3 7 0 429.46 26.80 3 7 0 438.56 27.10 -3 -7 0 447.06 26.80 -3 7 0 435.36 27.60 -3 -7 0 416.96 27.50 3 -7 0 463.15 28.10 -4 -7 0 0.60 0.90 4 -7 0 -0.80 1.10 -4 7 0 -1.10 0.80 4 7 0 -0.40 0.40 4 7 0 0.10 0.70 -4 7 0 -0.80 0.80 -5 7 0 116.59 9.10 5 7 0 127.79 8.50 -5 -7 0 127.29 9.00 -5 7 0 121.09 9.60 5 -7 0 127.79 9.60 -6 -7 0 0.40 1.00 6 -7 0 0.70 1.30 -6 7 0 -0.40 1.20 6 7 0 0.40 0.60 6 7 0 -0.50 0.70 -6 7 0 1.90 1.70 7 7 0 0.30 0.80 -7 7 0 -1.70 1.00 -7 -7 0 1.40 1.40 7 7 0 0.40 1.00 -7 7 0 0.20 1.50 -8 -7 0 0.30 1.20 8 7 0 -1.20 0.90 -8 -7 0 -0.60 1.00 -8 7 0 -1.20 1.40 -8 7 0 -0.50 1.20 8 7 0 0.70 1.10 -9 -7 0 13.50 2.60 -9 7 0 13.20 3.40 -9 7 0 16.40 3.30 9 7 0 12.30 2.20 9 7 0 11.20 2.30 -9 -7 0 13.60 2.90 10 7 0 0.00 1.30 -10 7 0 -1.10 1.50 -10 -7 0 -0.70 1.30 -10 -7 0 0.50 1.40 -10 7 0 0.50 1.30 10 7 0 0.40 1.50 -11 -7 0 106.69 9.30 11 7 0 116.09 8.60 -11 -7 0 109.09 8.90 -11 7 0 109.49 9.70 -11 7 0 116.99 10.20 11 7 0 101.39 8.40 -12 7 0 0.60 2.00 12 7 0 1.50 1.40 12 7 0 -0.30 1.50 -12 7 0 1.80 2.10 -12 -7 0 2.40 1.90 -12 -7 0 0.00 1.70 -13 7 0 36.30 5.90 -13 -7 0 44.30 6.10 -13 -7 0 42.00 5.90 -14 -7 0 1.90 2.10 -14 -7 0 -0.70 2.00 -14 7 0 -0.50 1.80 -15 -7 0 33.20 6.10 -15 -7 0 43.20 6.20 -15 7 0 42.00 6.60 -16 7 0 -1.00 2.60 -16 -7 0 0.00 2.40 -16 -7 0 3.90 3.00 -17 7 0 23.10 5.60 -17 -7 0 5.30 3.80 -17 -7 0 19.90 4.60 -18 -7 0 2.10 3.20 -18 7 0 -2.30 2.70 -18 -7 0 0.80 2.40 -19 -7 0 -1.40 2.60 0 8 0 361.06 22.80 0 8 0 387.96 24.40 0 -8 0 372.16 23.60 0 -8 0 372.16 23.50 0 8 0 373.26 23.50 -1 -8 0 -1.20 0.70 -1 8 0 1.00 0.60 -1 -8 0 -0.30 0.70 1 -8 0 -0.40 0.70 -1 8 0 -0.60 1.10 -1 8 0 0.20 1.00 1 8 0 0.80 0.80 2 -8 0 356.26 23.00 -2 -8 0 361.26 22.70 2 8 0 349.96 22.10 -2 8 0 344.27 23.00 -2 -8 0 348.57 22.20 -2 8 0 379.06 22.50 3 -8 0 0.30 1.20 -3 -8 0 0.20 0.20 -3 -8 0 0.20 0.30 -3 -8 0 0.60 0.90 3 8 0 0.10 0.50 -3 8 0 1.20 1.00 3 -8 0 0.70 1.00 -3 8 0 1.80 1.30 4 -8 0 86.59 7.30 -4 8 0 95.89 7.30 -4 -8 0 79.39 5.60 4 8 0 85.19 5.60 4 8 0 78.89 6.00 -4 -8 0 98.69 6.80 -4 8 0 86.69 6.60 4 -8 0 86.39 7.00 -5 8 0 -0.10 1.10 5 8 0 0.60 0.70 -5 -8 0 3.10 1.40 5 -8 0 1.70 1.40 5 8 0 0.20 0.80 -5 8 0 -0.40 1.00 -5 -8 0 -0.60 0.50 -6 -8 0 93.69 7.40 -6 8 0 99.49 7.70 -6 8 0 109.79 8.40 -6 -8 0 92.39 6.70 6 8 0 93.89 6.40 6 8 0 87.79 6.70 7 8 0 0.20 1.00 -7 -8 0 0.10 0.90 7 8 0 1.00 0.90 -7 -8 0 0.10 1.20 -7 8 0 0.00 1.50 -7 8 0 -0.80 1.20 8 8 0 451.35 28.50 -8 8 0 447.46 30.30 -8 -8 0 486.15 29.60 8 8 0 466.65 28.40 -8 -8 0 436.86 28.80 -8 8 0 428.36 29.80 -9 8 0 1.90 1.90 9 8 0 -0.40 1.20 -9 8 0 -0.10 1.50 -9 -8 0 0.30 1.40 9 8 0 -0.40 0.80 -9 -8 0 0.90 1.20 10 8 0 691.43 44.30 -10 -8 0 655.93 44.80 -10 -8 0 663.73 45.30 -10 8 0 822.62 46.90 -10 8 0 753.82 46.10 10 8 0 704.43 44.30 11 8 0 -1.30 1.20 -11 8 0 1.80 1.80 -11 -8 0 2.60 1.80 -11 8 0 -1.60 1.70 -11 -8 0 0.90 1.80 11 8 0 2.10 1.50 -12 8 0 1233.98 82.39 -12 8 0 1210.38 81.99 -12 -8 0 1260.37 81.69 12 8 0 1510.35 83.09 12 8 0 1309.77 80.39 -12 -8 0 1307.07 81.19 -13 -8 0 0.60 2.10 -13 8 0 -0.70 2.00 -13 -8 0 1.10 1.70 -14 -8 0 873.81 54.89 -14 -8 0 805.22 55.19 -14 8 0 885.11 55.99 -15 8 0 -0.20 2.50 -15 -8 0 -1.60 2.30 -15 -8 0 2.60 2.30 -16 8 0 574.34 41.00 -16 -8 0 580.34 40.60 -16 -8 0 647.74 40.40 -17 -8 0 0.50 2.90 -17 8 0 2.10 3.10 -17 -8 0 0.70 2.40 -18 -8 0 254.67 22.50 -18 8 0 323.47 23.40 -18 -8 0 301.97 22.20 0 9 0 0.20 0.50 0 9 0 -1.50 1.20 0 -9 0 -0.60 0.80 0 9 0 0.40 1.00 0 -9 0 0.80 0.90 -1 9 0 1288.27 81.69 1 -9 0 1317.17 80.79 -1 9 0 1307.47 80.19 -1 -9 0 1336.87 80.49 -1 -9 0 1339.37 80.89 1 -9 0 1412.66 80.99 1 9 0 1279.37 80.39 -1 9 0 1274.67 80.89 -2 9 0 -0.80 0.60 -2 -9 0 0.60 1.00 2 9 0 -0.20 0.60 2 -9 0 0.80 1.00 -2 -9 0 0.00 0.70 -2 9 0 -0.20 1.10 -3 9 0 880.21 54.49 3 -9 0 984.30 56.49 -3 9 0 876.41 55.29 -3 -9 0 865.51 54.69 3 9 0 865.71 53.79 3 -9 0 860.31 55.09 -4 -9 0 0.60 0.40 -4 -9 0 -0.20 1.00 4 9 0 0.30 0.40 -4 9 0 -1.20 0.80 -4 9 0 -1.00 1.10 4 -9 0 0.30 1.10 -4 -9 0 0.00 0.30 -5 9 0 468.85 29.10 -5 -9 0 439.66 27.80 -5 -9 0 463.25 29.00 -5 9 0 408.36 29.50 5 -9 0 501.95 29.90 5 9 0 458.45 28.10 5 9 0 437.06 27.60 6 9 0 0.40 0.80 6 9 0 0.20 0.70 -6 -9 0 2.70 1.50 -6 9 0 2.50 1.60 -6 9 0 -0.10 1.40 -6 -9 0 -0.30 0.70 6 9 0 0.80 0.60 7 9 0 302.97 19.20 -7 9 0 313.67 20.80 7 9 0 309.17 19.50 -7 -9 0 295.47 19.60 -7 -9 0 291.07 20.40 7 9 0 314.97 19.20 -7 9 0 310.47 21.30 -8 9 0 -0.90 1.40 -8 -9 0 -0.40 1.30 8 9 0 -0.90 1.00 -8 9 0 -1.80 1.10 -8 -9 0 0.20 1.00 8 9 0 0.00 0.80 9 9 0 0.90 1.20 -9 9 0 2.70 1.90 -9 9 0 4.10 2.30 -9 -9 0 1.90 1.70 -9 -9 0 0.70 1.10 9 9 0 1.90 1.30 -10 9 0 -2.10 1.50 10 9 0 0.70 1.30 -10 -9 0 -0.90 1.10 10 9 0 -0.40 1.30 -10 -9 0 -0.60 1.50 -10 9 0 0.00 2.00 11 9 0 3.10 1.80 -11 -9 0 4.20 2.00 -11 9 0 5.00 2.80 -11 -9 0 0.50 1.80 11 9 0 0.50 1.70 -11 9 0 0.80 2.20 -12 -9 0 0.90 1.50 -12 9 0 -0.40 2.10 -12 -9 0 2.30 2.30 -12 9 0 -1.70 2.00 -13 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10 15 65.79 11.20 4 10 -15 73.09 11.60 -4 -10 15 86.19 10.40 0 11 15 -3.20 3.30 -1 11 15 104.79 13.40 1 11 15 113.89 13.40 0 0 -16 543.85 39.20 0 0 16 538.95 39.00 -1 0 16 10.20 5.30 -1 0 -16 15.90 5.60 1 0 -16 19.40 6.00 2 0 -16 131.99 16.00 -2 0 16 129.29 15.30 -3 0 -16 77.79 11.40 3 0 -16 75.49 12.00 -3 0 16 78.29 11.30 -4 0 -16 361.46 27.90 4 0 -16 342.07 28.80 -4 0 16 392.86 29.00 -5 0 -16 34.20 7.30 5 0 -16 36.70 8.30 -5 0 16 39.00 8.00 -6 0 16 30.70 7.80 6 0 -16 45.20 9.20 -6 0 -16 39.40 7.80 -7 0 -16 395.36 28.90 -7 0 16 362.96 29.90 0 1 -16 6.40 4.40 0 1 16 -0.50 4.00 0 -1 16 -3.90 2.70 0 -1 -16 0.20 3.70 -1 -1 -16 9.70 5.10 1 1 -16 1.00 3.70 -1 1 16 1.10 4.00 1 1 16 9.70 4.80 -1 -1 16 -0.10 3.80 1 -1 -16 1.50 4.10 -1 1 -16 3.00 3.60 -2 -1 -16 18.70 5.90 -2 1 16 9.60 4.40 2 1 -16 7.50 5.10 -2 -1 16 11.50 5.60 -2 1 -16 18.00 5.80 2 -1 -16 18.00 6.10 -3 -1 -16 72.29 10.70 -3 1 16 74.39 11.20 3 1 -16 69.09 11.30 -3 -1 16 68.19 10.80 3 -1 -16 83.69 12.30 -3 1 -16 72.19 10.70 4 1 -16 -2.00 3.90 -4 1 16 1.50 4.40 -4 -1 -16 2.70 3.50 -4 1 -16 2.20 3.90 4 -1 -16 -1.30 4.10 -4 -1 16 -0.50 4.00 -5 1 16 12.70 5.60 -5 -1 -16 1.80 4.20 5 1 -16 18.20 6.60 -5 1 -16 10.40 5.00 -5 -1 16 1.70 4.20 5 -1 -16 22.00 6.70 -6 -1 -16 10.40 4.20 -6 1 16 4.30 5.00 6 1 -16 22.40 7.40 6 -1 -16 10.90 5.80 -6 1 -16 13.90 5.20 -6 -1 16 6.90 5.00 -7 -1 -16 72.99 10.60 -7 1 16 58.69 11.90 -7 -1 16 73.39 11.40 -7 1 -16 64.39 10.30 0 2 -16 189.48 18.40 0 -2 16 213.58 18.30 0 2 16 200.78 18.40 0 -2 -16 206.28 18.30 -1 2 16 5.70 4.60 1 2 -16 1.60 4.30 -1 -2 -16 1.50 3.90 -1 -2 16 1.00 3.60 1 2 16 0.80 3.70 1 -2 -16 3.40 4.30 -1 2 -16 0.70 3.90 2 2 -16 164.88 16.10 -2 2 16 138.19 16.30 -2 -2 -16 149.49 15.10 2 -2 -16 161.08 15.70 -2 -2 16 183.98 16.10 -2 2 -16 133.19 15.90 -3 2 16 95.39 13.40 3 2 -16 131.09 15.80 -3 -2 -16 136.29 15.10 -3 -2 16 107.39 13.70 3 -2 -16 100.49 14.10 -3 2 -16 127.59 14.60 4 2 -16 69.69 10.90 -4 2 16 44.00 9.10 -4 -2 -16 52.49 9.00 -4 2 -16 52.09 9.40 4 -2 -16 40.50 8.90 -4 -2 16 63.29 10.20 -5 -2 -16 283.87 22.00 5 2 -16 289.97 23.80 -5 2 16 255.37 22.70 5 -2 -16 263.97 22.80 -5 2 -16 255.97 22.00 -5 -2 16 254.27 22.50 -6 -2 -16 43.90 8.50 -6 2 16 38.50 8.70 6 2 -16 43.70 9.50 6 -2 -16 68.69 11.30 -6 2 -16 58.49 9.40 -6 -2 16 47.90 9.10 -7 -2 -16 59.69 9.10 -7 -2 16 60.19 10.20 -7 2 -16 36.80 7.80 0 3 -16 4.40 4.40 0 3 16 0.30 3.70 0 -3 -16 -0.20 3.60 1 3 -16 31.60 7.80 -1 3 16 14.40 5.90 -1 -3 -16 12.50 5.40 1 -3 -16 20.00 6.40 1 3 16 23.50 6.50 -1 3 -16 35.10 8.20 -1 -3 16 31.40 6.90 -2 -3 -16 21.80 6.10 -2 3 16 18.80 5.90 2 3 -16 12.30 5.50 -2 -3 16 12.90 5.30 -2 3 -16 13.70 6.10 2 -3 -16 27.90 7.00 3 3 -16 25.60 7.00 -3 3 16 13.70 5.80 -3 -3 -16 14.30 4.90 -3 3 -16 18.40 6.40 -3 -3 16 18.70 5.80 3 -3 -16 15.30 6.30 -4 3 16 -1.60 4.00 -4 -3 -16 2.80 3.10 4 3 -16 4.00 4.90 -4 3 -16 6.10 4.90 -4 -3 16 1.70 4.10 4 -3 -16 7.10 5.00 -5 -3 -16 139.69 15.20 -5 3 16 123.59 15.80 5 3 -16 124.89 16.40 -5 3 -16 134.99 15.40 5 -3 -16 150.78 16.90 -5 -3 16 136.09 15.70 -6 -3 -16 5.10 4.10 -6 3 16 3.50 5.30 6 3 -16 3.70 5.20 -6 3 -16 7.10 4.80 6 -3 -16 10.00 6.00 -6 -3 16 10.50 4.90 -7 -3 16 23.40 6.90 0 4 16 30.30 7.40 0 4 -16 57.79 9.70 0 -4 -16 47.40 8.90 -1 -4 -16 12.60 5.20 -1 4 16 5.10 4.70 1 4 -16 8.20 5.00 1 4 16 3.40 4.10 1 -4 -16 12.30 5.80 -1 -4 16 10.30 4.80 -1 4 -16 7.30 5.10 -2 -4 -16 19.80 5.30 -2 4 16 18.40 5.70 2 4 -16 24.10 6.70 -2 4 -16 29.80 7.10 -2 -4 16 19.60 5.50 2 -4 -16 22.20 6.80 -3 4 16 53.19 9.50 3 4 -16 47.60 9.50 -3 -4 -16 68.49 10.10 -3 -4 16 49.10 9.20 -3 4 -16 48.20 9.10 3 -4 -16 46.20 9.00 -4 4 16 11.50 5.80 -4 -4 -16 2.50 3.70 4 4 -16 13.10 6.20 -4 -4 16 10.30 5.30 -4 4 -16 8.60 5.10 4 -4 -16 10.30 5.10 -5 4 16 70.69 11.70 5 4 -16 86.39 13.10 -5 -4 -16 98.69 11.70 5 -4 -16 79.69 12.20 -5 4 -16 77.99 11.30 -5 -4 16 87.29 12.20 -6 -4 -16 8.60 4.50 6 -4 -16 9.20 5.40 -6 -4 16 7.30 4.70 -6 4 -16 9.90 5.10 0 -5 -16 -7.20 2.30 0 5 16 -3.10 2.00 0 5 -16 -1.40 4.00 1 5 -16 76.49 11.10 -1 -5 -16 52.59 8.80 -1 5 16 64.09 10.30 1 5 16 42.00 7.90 -1 5 -16 47.00 9.10 1 -5 -16 52.29 9.50 2 5 -16 3.20 4.40 -2 -5 -16 2.10 3.60 -2 5 16 5.60 4.00 2 -5 -16 -0.30 4.30 -2 -5 16 0.30 2.90 -2 5 -16 9.00 4.70 -3 5 16 19.40 6.40 3 5 -16 23.50 7.40 -3 -5 -16 23.90 6.30 -3 5 -16 22.50 6.80 -3 -5 16 34.70 7.20 3 -5 -16 24.90 6.70 -4 -5 -16 3.10 3.20 -4 5 16 1.90 4.60 4 5 -16 3.80 4.60 -4 5 -16 -0.40 3.90 4 -5 -16 5.70 5.30 -4 -5 16 -0.10 3.50 -5 -5 -16 39.00 7.40 -5 5 -16 44.00 8.70 5 -5 -16 35.80 8.20 -5 -5 16 44.60 8.40 -6 -5 16 25.60 6.80 0 6 -16 -0.50 4.20 0 6 16 0.90 3.40 0 -6 -16 2.10 4.00 -1 -6 -16 3.10 3.70 1 6 -16 2.90 5.00 -1 6 16 1.40 3.30 1 6 16 -0.30 3.20 -1 6 -16 4.40 4.50 1 -6 -16 -1.40 3.30 2 6 -16 19.70 6.60 -2 -6 -16 17.80 5.50 -2 6 16 6.60 4.80 -2 -6 16 -0.20 2.90 -2 6 -16 3.60 4.50 2 -6 -16 10.70 5.20 3 6 -16 22.30 7.30 -3 -6 -16 54.69 8.90 -3 6 16 40.20 8.70 -3 -6 16 42.70 8.20 3 -6 -16 37.40 8.10 -3 6 -16 43.90 8.50 -4 -6 -16 36.30 7.40 4 6 -16 51.49 14.00 -4 6 16 25.20 7.90 -4 6 -16 63.39 11.30 4 -6 -16 32.70 7.80 -4 -6 16 33.50 7.70 -5 -6 -16 110.69 13.00 -5 -6 16 102.39 13.10 0 -7 -16 1.70 3.50 0 7 16 0.50 4.20 0 7 -16 -1.60 4.60 -1 -7 -16 21.00 5.70 -1 7 16 23.00 6.20 1 7 -16 38.10 8.30 -1 7 -16 9.30 5.10 1 7 16 13.10 5.20 1 -7 -16 19.30 6.30 -2 -7 -16 2.90 3.90 -2 7 16 5.00 5.00 2 7 -16 8.70 5.40 2 -7 -16 -2.30 3.70 -3 7 16 15.90 7.10 -3 -7 -16 21.70 6.40 3 -7 -16 18.70 6.60 -3 -7 16 21.20 5.90 -4 -7 -16 8.10 4.90 -4 -7 16 4.70 4.10 4 -7 -16 1.90 3.80 0 8 16 -1.30 3.10 0 -8 -16 -0.70 3.60 -1 8 16 6.40 5.80 -1 -8 -16 12.90 4.90 1 8 16 16.10 5.30 1 -8 -16 6.90 5.00 -2 -8 -16 -1.40 3.50 2 -8 -16 0.90 3.60 0 0 -17 -6.10 3.30 0 0 17 4.50 4.10 1 0 -17 -4.40 3.70 -1 0 -17 0.70 4.50 -1 0 17 -1.80 3.70 -2 0 17 -6.80 3.60 -2 0 -17 -6.20 3.80 2 0 -17 0.40 4.70 -3 0 -17 1.00 4.20 0 -1 17 0.20 2.70 0 1 -17 6.60 4.80 0 -1 -17 1.20 4.30 1 1 -17 51.69 10.20 -1 -1 -17 52.99 9.40 1 -1 -17 66.39 10.90 -1 1 -17 66.99 11.20 -1 -1 17 54.49 10.00 -2 -1 -17 0.20 4.00 -2 -1 17 4.90 5.00 2 -1 -17 8.90 5.80 -2 1 -17 0.80 4.50 -3 -1 -17 19.60 6.00 -3 1 -17 7.60 4.90 3 -1 -17 4.00 5.20 0 -2 -17 78.59 12.00 0 2 -17 91.09 14.70 1 2 -17 -1.70 3.60 -1 -2 -17 8.30 4.80 -1 2 -17 2.10 4.50 1 -2 -17 2.40 4.60 -1 -2 17 2.90 4.40 -2 -2 -17 71.49 11.10 -2 2 -17 54.99 11.30 2 -2 -17 62.99 11.10 -2 -2 17 78.19 11.40 0 -3 -17 -0.80 3.60 -1 -3 17 178.18 17.10 -2 -3 17 2.70 4.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 99162 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, 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 I2 I 0.500000 0.67521(2) 0.750000 0.01968(7) Uani 1 2 d S T P I1 I 0.46388(2) 0.75951(2) 0.07287(2) 0.01694(6) Uani 1 1 d . . . Na2 Na 0.50396(6) 0.59569(5) 0.52276(7) 0.0153(2) Uani 1 1 d . . . Na1 Na 0.500000 0.66244(8) 0.250000 0.0199(3) Uani 1 2 d S T P O1B O 0.89191(11) 0.54853(9) 0.39122(13) 0.0150(4) Uani 1 1 d . . . O1 O 0.10742(11) 0.51259(9) 0.34870(13) 0.0167(4) Uani 1 1 d . . . O1S O 0.50362(12) 0.52677(11) 0.37297(14) 0.0233(4) Uani 1 1 d D . . H1SA H 0.5477(12) 0.5127(15) 0.3382(19) 0.026(8) Uiso 1 1 d D . . H1SB H 0.4617(12) 0.5128(16) 0.3348(19) 0.030(9) Uiso 1 1 d D . . N7B N 0.65265(13) 0.56155(11) 0.49682(15) 0.0133(4) Uani 1 1 d . . . N7 N 0.35260(13) 0.51162(11) 0.26400(15) 0.0133(4) Uani 1 1 d . . . N5B N 0.78279(13) 0.61859(11) 0.44953(15) 0.0139(4) Uani 1 1 d . . . N5 N 0.22473(13) 0.44855(11) 0.30365(15) 0.0133(4) Uani 1 1 d . . . N1B N 0.64927(13) 0.42807(11) 0.47798(15) 0.0128(4) Uani 1 1 d . . . N1 N 0.34687(13) 0.64467(11) 0.27700(15) 0.0142(4) Uani 1 1 d . . . N2B N 0.70990(13) 0.37942(11) 0.44990(15) 0.0123(4) Uani 1 1 d . . . N2 N 0.28395(13) 0.69116(10) 0.30263(15) 0.0139(4) Uani 1 1 d . . . C6B C 0.70356(15) 0.61783(13) 0.48389(18) 0.0141(5) Uani 1 1 d . . . H6B H 0.681854 0.665197 0.501118 0.017 Uiso 1 1 calc R . . C6 C 0.30579(15) 0.45228(13) 0.27637(17) 0.0131(5) Uani 1 1 d . . . H6 H 0.332087 0.405807 0.264681 0.016 Uiso 1 1 calc R . . C7AB C 0.68814(15) 0.49430(13) 0.47405(17) 0.0119(5) Uani 1 1 d . . . C7A C 0.31183(15) 0.57704(13) 0.28294(17) 0.0123(5) Uani 1 1 d . . . C3AB C 0.77091(16) 0.48668(13) 0.44227(17) 0.0115(5) Uani 1 1 d . . . C3A C 0.22800(15) 0.58085(13) 0.31193(18) 0.0124(5) Uani 1 1 d . . . C4B C 0.81561(15) 0.55377(13) 0.42797(17) 0.0126(5) Uani 1 1 d . . . C4 C 0.18613(16) 0.51168(13) 0.32136(17) 0.0121(5) Uani 1 1 d . . . C3B C 0.78240(16) 0.41073(13) 0.42852(17) 0.0132(5) Uani 1 1 d . . . H3B H 0.831627 0.386289 0.408156 0.016 Uiso 1 1 calc R . . C3 C 0.21276(16) 0.65681(13) 0.32401(18) 0.0154(5) Uani 1 1 d . . . H3 H 0.162196 0.679435 0.343434 0.018 Uiso 1 1 calc R . . C9B C 0.93527(17) 0.61829(14) 0.37134(19) 0.0187(6) Uani 1 1 d . . . H9BA H 0.903158 0.647800 0.324871 0.028 Uiso 1 1 calc GR . . H9BB H 0.990045 0.607433 0.344100 0.028 Uiso 1 1 calc GR . . H9BC H 0.941696 0.646453 0.431693 0.028 Uiso 1 1 calc GR . . C9 C 0.06661(16) 0.44052(13) 0.3582(2) 0.0186(6) Uani 1 1 d . . . H9A H 0.067713 0.414647 0.295698 0.028 Uiso 1 1 calc GR . . H9B H 0.008994 0.447943 0.378498 0.028 Uiso 1 1 calc GR . . H9C H 0.095692 0.410510 0.406804 0.028 Uiso 1 1 calc GR . . C8B C 0.68925(16) 0.29999(13) 0.44213(19) 0.0159(5) Uani 1 1 d . . . H8BA H 0.660812 0.283807 0.501232 0.024 Uiso 1 1 calc GR . . H8BB H 0.740243 0.271029 0.433811 0.024 Uiso 1 1 calc GR . . H8BC H 0.652917 0.292115 0.386161 0.024 Uiso 1 1 calc GR . . C8 C 0.29903(17) 0.77146(13) 0.3032(2) 0.0195(6) Uani 1 1 d . . . H8A H 0.340466 0.783424 0.352724 0.029 Uiso 1 1 calc GR . . H8B H 0.247243 0.797703 0.317755 0.029 Uiso 1 1 calc GR . . H8C H 0.319475 0.787083 0.239505 0.029 Uiso 1 1 calc GR . . 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 I2 0.01808(14) 0.01879(13) 0.02218(14) 0.000 -0.00484(10) 0.000 I1 0.01530(10) 0.01403(9) 0.02149(11) 0.00044(6) 0.00200(7) -0.00176(6) Na2 0.0122(5) 0.0158(5) 0.0179(5) -0.0008(4) 0.0014(4) 0.0005(4) Na1 0.0142(8) 0.0209(7) 0.0247(8) 0.000 0.0000(6) 0.000 O1B 0.0090(9) 0.0155(8) 0.0203(10) -0.0007(7) 0.0034(8) -0.0015(7) O1 0.0110(9) 0.0148(8) 0.0243(10) 0.0012(7) 0.0009(8) -0.0020(7) O1S 0.0114(10) 0.0371(11) 0.0214(11) -0.0134(9) -0.0019(9) 0.0027(8) N7B 0.0122(11) 0.0132(10) 0.0144(11) 0.0001(8) -0.0019(9) 0.0013(8) N7 0.0113(11) 0.0150(10) 0.0136(11) 0.0002(8) -0.0008(9) 0.0009(8) N5B 0.0125(11) 0.0122(10) 0.0171(12) 0.0003(8) 0.0010(9) 0.0000(8) N5 0.0146(11) 0.0134(10) 0.0119(11) -0.0003(8) -0.0012(9) -0.0010(8) N1B 0.0122(11) 0.0142(10) 0.0121(11) 0.0009(8) 0.0003(9) 0.0017(8) N1 0.0145(12) 0.0131(10) 0.0151(11) 0.0006(8) -0.0004(9) 0.0000(8) N2B 0.0136(11) 0.0106(10) 0.0126(11) -0.0001(8) 0.0001(9) 0.0013(8) N2 0.0158(12) 0.0108(10) 0.0152(11) 0.0020(8) -0.0005(9) 0.0006(8) C6B 0.0126(13) 0.0143(12) 0.0154(13) -0.0031(10) -0.0020(10) 0.0004(10) C6 0.0125(13) 0.0138(12) 0.0131(13) -0.0015(9) -0.0030(10) 0.0017(10) C7AB 0.0128(13) 0.0137(12) 0.0092(12) 0.0002(9) -0.0021(10) 0.0003(10) C7A 0.0133(13) 0.0159(12) 0.0076(12) 0.0013(9) -0.0015(10) 0.0008(10) C3AB 0.0124(13) 0.0128(12) 0.0094(12) -0.0007(9) -0.0020(10) 0.0011(9) C3A 0.0109(12) 0.0140(12) 0.0123(12) 0.0009(9) -0.0002(10) 0.0016(10) C4B 0.0108(13) 0.0175(12) 0.0095(12) 0.0001(9) -0.0019(10) -0.0014(10) C4 0.0126(13) 0.0146(12) 0.0092(12) 0.0007(9) -0.0014(10) -0.0025(10) C3B 0.0115(13) 0.0153(12) 0.0129(12) -0.0008(10) -0.0014(10) 0.0009(10) C3 0.0148(14) 0.0175(12) 0.0139(13) -0.0007(10) -0.0005(11) 0.0012(10) C9B 0.0140(14) 0.0189(13) 0.0231(15) 0.0012(11) 0.0017(11) -0.0067(10) C9 0.0120(13) 0.0173(13) 0.0266(15) 0.0003(11) 0.0005(12) -0.0052(10) C8B 0.0172(14) 0.0103(12) 0.0203(14) 0.0014(10) -0.0013(11) -0.0016(10) C8 0.0229(15) 0.0099(12) 0.0258(15) 0.0016(11) 0.0022(12) -0.0004(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Na2 I2 Na2 131.06(3) . 3_656 Na1 I1 Na2 77.26(3) . 3_655 I2 Na2 Na2 124.75(4) . 5_666 I2 Na2 Na1 137.82(3) . . I1 Na2 I2 89.86(2) 3_655 . I1 Na2 Na2 144.95(5) 3_655 5_666 I1 Na2 Na1 49.02(2) 3_655 . Na2 Na2 Na1 97.26(4) 5_666 . O1S Na2 I2 173.46(6) . . O1S Na2 I2 81.23(5) 5_666 . O1S Na2 I1 96.67(6) . 3_655 O1S Na2 I1 168.92(6) 5_666 3_655 O1S Na2 Na2 43.53(5) 5_666 5_666 O1S Na2 Na2 48.76(5) . 5_666 O1S Na2 Na1 140.71(5) 5_666 . O1S Na2 Na1 48.57(6) . . O1S Na2 O1S 92.29(7) . 5_666 O1S Na2 N7B 75.73(7) . . O1S Na2 N1B 84.66(7) . 5_666 N7B Na2 I2 104.45(6) . . N7B Na2 I1 90.60(5) . 3_655 N7B Na2 Na2 76.61(6) . 5_666 N7B Na2 Na1 87.33(5) . . N7B Na2 O1S 85.30(7) . 5_666 N7B Na2 N1B 154.51(7) . 5_666 N1B Na2 I2 93.21(5) 5_666 . N1B Na2 I1 107.95(5) 5_666 3_655 N1B Na2 Na2 78.23(6) 5_666 5_666 N1B Na2 Na1 91.82(5) 5_666 . N1B Na2 O1S 79.30(7) 5_666 5_666 I1 Na1 I1 110.52(4) 3_655 . I1 Na1 Na2 53.713(14) . 3_655 I1 Na1 Na2 53.711(14) 3_655 . I1 Na1 Na2 159.64(4) 3_655 3_655 I1 Na1 Na2 159.64(4) . . Na2 Na1 Na2 144.69(5) 3_655 . O1S Na1 I1 90.39(4) 3_655 . O1S Na1 I1 158.14(5) . . O1S Na1 I1 90.39(4) . 3_655 O1S Na1 I1 158.14(5) 3_655 3_655 O1S Na1 Na2 37.47(4) . . O1S Na1 Na2 107.22(5) 3_655 . O1S Na1 Na2 107.22(5) . 3_655 O1S Na1 Na2 37.47(4) 3_655 3_655 O1S Na1 O1S 69.77(8) 3_655 . N1 Na1 I1 98.09(5) 3_655 . N1 Na1 I1 98.09(5) . 3_655 N1 Na1 I1 90.20(5) 3_655 3_655 N1 Na1 I1 90.20(5) . . N1 Na1 Na2 94.97(5) 3_655 . N1 Na1 Na2 80.59(5) 3_655 3_655 N1 Na1 Na2 94.97(5) . 3_655 N1 Na1 Na2 80.59(5) . . N1 Na1 O1S 80.26(6) 3_655 3_655 N1 Na1 O1S 87.79(7) . 3_655 N1 Na1 O1S 87.78(7) 3_655 . N1 Na1 O1S 80.26(6) . . N1 Na1 N1 165.45(11) 3_655 . C4B O1B C9B 116.92(19) . . C4 O1 C9 116.59(19) . . Na2 O1S Na2 87.71(7) . 5_666 Na2 O1S Na1 93.96(7) . . Na2 O1S Na1 175.86(8) 5_666 . Na2 O1S H1SA 95.5(18) 5_666 . Na2 O1S H1SA 127.1(17) . . Na2 O1S H1SB 130.6(18) . . Na2 O1S H1SB 93.0(19) 5_666 . Na1 O1S H1SA 86.6(18) . . Na1 O1S H1SB 83.0(19) . . H1SA O1S H1SB 102(2) . . C6B N7B Na2 115.49(16) . . C6B N7B C7AB 112.6(2) . . C7AB N7B Na2 130.41(16) . . C6 N7 C7A 113.1(2) . . C4B N5B C6B 116.6(2) . . C4 N5 C6 117.6(2) . . N2B N1B Na2 126.52(14) . 5_666 C7AB N1B Na2 127.55(16) . 5_666 C7AB N1B N2B 102.69(19) . . N2 N1 Na1 133.82(15) . . C7A N1 Na1 122.47(16) . . C7A N1 N2 103.0(2) . . N1B N2B C8B 118.6(2) . . C3B N2B N1B 114.94(19) . . C3B N2B C8B 126.4(2) . . N1 N2 C8 118.8(2) . . C3 N2 N1 114.54(19) . . C3 N2 C8 126.6(2) . . N7B C6B N5B 129.9(2) . . N7B C6B H6B 115.1 . . N5B C6B H6B 115.1 . . N7 C6 N5 128.8(2) . . N7 C6 H6 115.6 . . N5 C6 H6 115.6 . . N7B C7AB C3AB 123.4(2) . . N1B C7AB N7B 125.0(2) . . N1B C7AB C3AB 111.6(2) . . N7 C7A C3A 123.7(2) . . N1 C7A N7 124.1(2) . . N1 C7A C3A 112.2(2) . . C7AB C3AB C4B 116.2(2) . . C3B C3AB C7AB 105.3(2) . . C3B C3AB C4B 138.4(2) . . C7A C3A C4 116.1(2) . . C3 C3A C7A 104.5(2) . . C3 C3A C4 139.5(2) . . O1B C4B C3AB 117.5(2) . . N5B C4B O1B 121.4(2) . . N5B C4B C3AB 121.1(2) . . O1 C4 C3A 118.1(2) . . N5 C4 O1 121.1(2) . . N5 C4 C3A 120.7(2) . . N2B C3B C3AB 105.5(2) . . N2B C3B H3B 127.3 . . C3AB C3B H3B 127.3 . . N2 C3 C3A 105.8(2) . . N2 C3 H3 127.1 . . C3A C3 H3 127.1 . . O1B C9B H9BA 109.5 . . O1B C9B H9BB 109.5 . . O1B C9B H9BC 109.5 . . H9BA C9B H9BB 109.5 . . H9BA C9B H9BC 109.5 . . H9BB C9B H9BC 109.5 . . O1 C9 H9A 109.5 . . O1 C9 H9B 109.5 . . O1 C9 H9C 109.5 . . H9A C9 H9B 109.5 . . H9A C9 H9C 109.5 . . H9B C9 H9C 109.5 . . N2B C8B H8BA 109.5 . . N2B C8B H8BB 109.5 . . N2B C8B H8BC 109.5 . . H8BA C8B H8BB 109.5 . . H8BA C8B H8BC 109.5 . . H8BB C8B H8BC 109.5 . . N2 C8 H8A 109.5 . . N2 C8 H8B 109.5 . . N2 C8 H8C 109.5 . . H8A C8 H8B 109.5 . . H8A C8 H8C 109.5 . . H8B C8 H8C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 I2 Na2 3.4468(10) . I2 Na2 3.4468(10) 3_656 I1 Na2 3.2654(10) 3_655 I1 Na1 3.0585(8) . Na2 Na2 3.4956(19) 5_666 Na2 Na1 3.9514(11) . Na2 O1S 2.410(2) . Na2 O1S 2.631(2) 5_666 Na2 N7B 2.502(2) . Na2 N1B 2.509(2) 5_666 Na1 O1S 2.970(2) . Na1 O1S 2.970(2) 3_655 Na1 N1 2.519(2) 3_655 Na1 N1 2.519(2) . O1B C4B 1.335(3) . O1B C9B 1.461(3) . O1 C4 1.325(3) . O1 C9 1.458(3) . O1S H1SA 0.895(17) . O1S H1SB 0.893(17) . N7B C6B 1.314(3) . N7B C7AB 1.373(3) . N7 C6 1.317(3) . N7 C7A 1.371(3) . N5B C6B 1.363(3) . N5B C4B 1.313(3) . N5 C6 1.363(3) . N5 C4 1.316(3) . N1B N2B 1.368(3) . N1B C7AB 1.346(3) . N1 N2 1.361(3) . N1 C7A 1.342(3) . N2B C3B 1.331(3) . N2B C8B 1.469(3) . N2 C3 1.337(3) . N2 C8 1.462(3) . C6B H6B 0.9500 . C6 H6 0.9500 . C7AB C3AB 1.412(3) . C7A C3A 1.412(3) . C3AB C4B 1.418(3) . C3AB C3B 1.389(3) . C3A C4 1.420(3) . C3A C3 1.396(3) . C3B H3B 0.9500 . C3 H3 0.9500 . C9B H9BA 0.9800 . C9B H9BB 0.9800 . C9B H9BC 0.9800 . C9 H9A 0.9800 . C9 H9B 0.9800 . C9 H9C 0.9800 . C8B H8BA 0.9800 . C8B H8BB 0.9800 . C8B H8BC 0.9800 . C8 H8A 0.9800 . C8 H8B 0.9800 . C8 H8C 0.9800 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O1S H1SA N7 0.895(17) 2.139(18) 3.005(3) 163(3) 3_655 yes O1S H1SB N7 0.893(17) 2.013(17) 2.876(3) 162(3) . yes