#------------------------------------------------------------------------------ #$Date: 2019-11-11 20:28:41 +0200 (Mon, 11 Nov 2019) $ #$Revision: 227270 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/58/4035858.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_4035858 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_absolute_configuration ad _chemical_formula_moiety 'C14 H28 N8 Na2 O8, 2(C7 H8 N4 O), 2(I)' _chemical_formula_sum 'C28 H44 I2 N16 Na2 O10' _chemical_formula_weight 1064.57 _space_group_crystal_system orthorhombic _space_group_IT_number 43 _space_group_name_Hall 'F 2 -2d' _space_group_name_H-M_alt 'F d d 2' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary dual _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 8 _cell_length_a 27.7776(14) _cell_length_b 44.788(3) _cell_length_c 6.8825(4) _cell_measurement_reflns_used 3374 _cell_measurement_temperature 100 _cell_measurement_theta_max 22.291 _cell_measurement_theta_min 2.337 _cell_volume 8562.5(9) _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_collection 'APEX3 v2016.1-0 (Bruker, 2016)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _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 1.000 _diffrn_measured_fraction_theta_max 0.998 _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 0.0642 _diffrn_reflns_av_unetI/netI 0.0687 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_k_max 54 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 16912 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 25.420 _diffrn_reflns_theta_min 1.725 _diffrn_source 'Micro Focus Rotating Anode' _diffrn_source_type 'Bruker TXS' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.558 _exptl_absorpt_correction_T_max 0.0916 _exptl_absorpt_correction_T_min 0.0667 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.0652 before and 0.0579 after correction. The Ratio of minimum to maximum transmission is 0.7282. The \l/2 correction factor is 0.00150.' _exptl_crystal_colour Orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.652 _exptl_crystal_description Plank _exptl_crystal_F_000 4256 _exptl_crystal_size_max 0.053 _exptl_crystal_size_mid 0.021 _exptl_crystal_size_min 0.005 _refine_diff_density_max 0.373 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.085 _refine_ls_abs_structure_details ; Flack x determined using 1141 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.028(19) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 285 _refine_ls_number_reflns 3922 _refine_ls_number_restraints 11 _refine_ls_restrained_S_all 1.001 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0370 _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^)+(0.0201P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.0611 _reflns_Friedel_coverage 0.825 _reflns_Friedel_fraction_full 0.993 _reflns_Friedel_fraction_max 0.986 _reflns_number_gt 3145 _reflns_number_total 3922 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jo8b00540_si_010.cif _cod_data_source_block Dart113 _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. data item '_exptl_crystal_colour_primary' value 'Orange' was changed to 'orange' 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_original_cell_volume 8562.6(8) _cod_database_code 4035858 _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 0.992 _shelx_estimated_absorpt_t_min 0.922 _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, All O(H) groups, All O(H,H) groups 2. Restrained distances O2S-H2S = O1S-H1S 0.95 with sigma of 0.02 H2S-H2S_$1 1.45 with sigma of 0.02 H1S_$1-H1S 1.45 with sigma of 0.02 O3S-H3SA = O3S-H3SB 0.95 with sigma of 0.02 H3SB-H3SA 1.45 with sigma of 0.02 H4SA-H4SB 1.45 with sigma of 0.02 O4S-H4SA = O4S-H4SB 0.95 with sigma of 0.02 3.a Aromatic/amide H refined with riding coordinates: C3(H3), C6(H6), C3B(H3B), C6B(H6B) 3.b Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,H9BC) ; _shelx_res_file ; TITL Dart113 in Fdd2 #43 dart113.res created by SHELXL-2017/1 at 14:48:21 on 09-Oct-2017 REM SHELXT solution in Fdd2 REM R1 0.106, Rweak 0.017, Alpha 0.004, Orientation as input REM Flack x = 0.019 ( 0.019 ) from Parsons' quotients REM Formula found by SHELXT: C17 N7 O3 Na I CELL 0.71073 27.7776 44.7884 6.8825 90 90 90 ZERR 8 0.0014 0.0027 0.0004 0 0 0 LATT -4 SYMM -X,-Y,+Z SYMM 0.25+X,0.25-Y,0.25+Z SYMM 0.25-X,0.25+Y,0.25+Z SFAC C H I N Na O UNIT 224 352 16 128 16 80 EQIV $1 1-X,1-Y,+Z EQIV $2 +X,+Y,-1+Z EQIV $3 +X,+Y,1+Z DFIX 0.95 O2S H2S O1S H1S DFIX 1.45 H2S H2S_$1 DFIX 1.45 H1S_$1 H1S DFIX 0.95 O3S H3Sa O3S H3Sb DFIX 1.45 H3Sb H3Sa DFIX 1.45 H4Sa H4Sb DFIX 0.95 O4S H4Sa O4S H4Sb L.S. 10 PLAN 20 SIZE 0.053 0.021 0.005 TEMP -173.15 HTAB O1S N7B HTAB O3S I1 HTAB O3S N1B_$2 HTAB O2S N7B_$2 HTAB O4S O3S_$3 BOND $H fmap 2 53 acta 50 REM REM REM WGHT 0.020100 FVAR 0.07706 NA1 5 0.456350 0.475149 0.356467 11.00000 0.02503 0.02011 = 0.03235 0.00070 0.00078 0.00039 O1 6 0.685904 0.405538 0.307308 11.00000 0.02579 0.02392 = 0.03122 0.00008 0.00476 0.00902 O1S 6 0.500000 0.500000 0.595889 10.50000 0.02734 0.02203 = 0.01656 0.00000 0.00000 0.01006 H1S 2 0.481777 0.511315 0.680157 11.00000 -1.50000 O2S 6 0.500000 0.500000 0.107435 10.50000 0.02388 0.01536 = 0.02254 0.00000 0.00000 0.00425 H2S 2 0.485910 0.513555 0.025178 11.00000 -1.50000 O3S 6 0.408994 0.457857 0.083500 11.00000 0.02376 0.02195 = 0.06981 -0.00714 -0.00352 -0.00411 H3SA 2 0.379907 0.447753 0.103769 11.00000 -1.50000 H3SB 2 0.397592 0.475713 0.027031 11.00000 -1.50000 O4S 6 0.422630 0.446669 0.618362 11.00000 0.03314 0.04911 = 0.03062 -0.00640 0.00319 -0.00742 H4SA 2 0.393364 0.444054 0.555157 11.00000 -1.50000 H4SB 2 0.414284 0.458403 0.722697 11.00000 -1.50000 N1 4 0.530711 0.442873 0.318893 11.00000 0.02967 0.01529 = 0.02842 0.00033 0.00521 -0.00147 N2 4 0.531487 0.413573 0.270575 11.00000 0.02680 0.01716 = 0.02331 0.00041 -0.00224 0.00166 N5 4 0.674862 0.455857 0.364787 11.00000 0.02104 0.02033 = 0.02514 -0.00020 0.00450 0.00337 N7 4 0.594841 0.477802 0.376484 11.00000 0.02603 0.01373 = 0.02749 0.00244 0.00268 -0.00090 C3 1 0.575767 0.401868 0.257134 11.00000 0.02549 0.01908 = 0.02584 0.00742 0.00001 0.00512 AFIX 43 H3 2 0.583736 0.381832 0.225227 11.00000 -1.20000 AFIX 0 C3A 1 0.607401 0.424639 0.298737 11.00000 0.02500 0.02011 = 0.01923 0.00094 0.00431 0.00269 C4 1 0.657278 0.429473 0.322933 11.00000 0.02574 0.02413 = 0.01924 -0.00324 -0.00022 0.00243 C6 1 0.642065 0.478560 0.386484 11.00000 0.03424 0.01860 = 0.02282 0.00141 0.00096 -0.00378 AFIX 43 H6 2 0.655517 0.497644 0.412596 11.00000 -1.20000 AFIX 0 C7A 1 0.577714 0.449889 0.333552 11.00000 0.02510 0.02397 = 0.01912 0.00220 -0.00209 -0.00455 C8 1 0.485645 0.398161 0.237574 11.00000 0.02936 0.01999 = 0.04364 0.00381 -0.00141 -0.00981 AFIX 137 H8A 2 0.467606 0.397130 0.359760 11.00000 -1.50000 H8B 2 0.491910 0.377903 0.190087 11.00000 -1.50000 H8C 2 0.466777 0.409150 0.140816 11.00000 -1.50000 AFIX 0 C9 1 0.735879 0.409438 0.365372 11.00000 0.02124 0.03223 = 0.05051 -0.00646 0.00109 0.00600 AFIX 137 H9A 2 0.752934 0.421025 0.266121 11.00000 -1.50000 H9B 2 0.751181 0.389841 0.379405 11.00000 -1.50000 H9C 2 0.737180 0.420074 0.489695 11.00000 -1.50000 AFIX 0 O1B 6 0.355785 0.610775 0.732903 11.00000 0.03492 0.03214 = 0.03483 -0.00358 -0.00249 0.01355 N1B 4 0.377310 0.511348 0.889110 11.00000 0.02554 0.04043 = 0.03024 0.00957 -0.00332 0.00207 N2B 4 0.329535 0.519193 0.880941 11.00000 0.01996 0.05143 = 0.02748 0.01100 0.00022 -0.00050 N5B 4 0.433371 0.592736 0.759064 11.00000 0.03102 0.02728 = 0.02469 -0.00617 -0.00426 0.00958 N7B 4 0.448467 0.541193 0.842848 11.00000 0.02607 0.02787 = 0.02569 -0.00207 -0.00078 0.00739 C3AB 1 0.366529 0.560766 0.818475 11.00000 0.02523 0.02902 = 0.02252 -0.00352 -0.00136 0.00801 C3B 1 0.321420 0.547382 0.839328 11.00000 0.02839 0.04332 = 0.02231 0.00891 0.00096 0.01493 AFIX 43 H3B 2 0.290938 0.556782 0.826072 11.00000 -1.20000 AFIX 0 C4B 1 0.386310 0.588334 0.770144 11.00000 0.03859 0.03557 = 0.02081 -0.00407 -0.00193 0.01102 C6B 1 0.461208 0.568464 0.796263 11.00000 0.02536 0.03438 = 0.02749 -0.00532 -0.00162 0.00584 AFIX 43 H6B 2 0.494926 0.571730 0.787179 11.00000 -1.20000 AFIX 0 C7AB 1 0.399172 0.537119 0.852149 11.00000 0.02173 0.03911 = 0.01798 0.00138 0.00318 0.00830 C8B 1 0.293770 0.495589 0.910683 11.00000 0.03152 0.06501 = 0.04665 0.02059 0.00122 -0.00650 AFIX 137 H8BA 2 0.297478 0.480319 0.809807 11.00000 -1.50000 H8BB 2 0.261356 0.504155 0.903360 11.00000 -1.50000 H8BC 2 0.298552 0.486506 1.038777 11.00000 -1.50000 AFIX 0 C9B 1 0.376484 0.639125 0.672293 11.00000 0.04593 0.03192 = 0.05070 -0.00041 -0.00281 0.01452 AFIX 137 H9BA 2 0.398023 0.635843 0.561560 11.00000 -1.50000 H9BB 2 0.394736 0.647807 0.780259 11.00000 -1.50000 H9BC 2 0.350636 0.652821 0.634237 11.00000 -1.50000 AFIX 0 I1 3 0.312230 0.434054 0.385930 11.00000 0.02598 0.02106 = 0.04681 0.00290 -0.00261 -0.00150 HKLF 4 REM Dart113 in Fdd2 #43 REM R1 = 0.0370 for 3145 Fo > 4sig(Fo) and 0.0575 for all 3922 data REM 285 parameters refined using 11 restraints END WGHT 0.0204 0.0000 REM Highest difference peak 0.373, deepest hole -0.340, 1-sigma level 0.085 Q1 1 0.3125 0.5711 0.7266 11.00000 0.05 0.37 Q2 1 0.3091 0.4106 0.5102 11.00000 0.05 0.32 Q3 1 0.3483 0.5100 0.9005 11.00000 0.05 0.31 Q4 1 0.3270 0.5920 0.8022 11.00000 0.05 0.31 Q5 1 0.4499 0.4912 0.8104 11.00000 0.05 0.31 Q6 1 0.3028 0.4628 0.2658 11.00000 0.05 0.30 Q7 1 0.4378 0.6791 0.8391 11.00000 0.05 0.30 Q8 1 0.8121 0.4310 0.4000 11.00000 0.05 0.30 Q9 1 0.3164 0.4567 0.4932 11.00000 0.05 0.29 Q10 1 0.3062 0.5091 0.8782 11.00000 0.05 0.29 Q11 1 0.3192 0.4848 1.2366 11.00000 0.05 0.29 Q12 1 0.2502 0.5679 0.8872 11.00000 0.05 0.28 Q13 1 0.2819 0.4251 0.2407 11.00000 0.05 0.28 Q14 1 0.2615 0.4599 1.1326 11.00000 0.05 0.28 Q15 1 0.3505 0.6670 0.6933 11.00000 0.05 0.28 Q16 1 0.4315 0.4306 0.5430 11.00000 0.05 0.28 Q17 1 0.3118 0.4161 0.2569 11.00000 0.05 0.27 Q18 1 0.3006 0.6583 0.6345 11.00000 0.05 0.27 Q19 1 0.3698 0.6124 0.5497 11.00000 0.05 0.27 Q20 1 0.3605 0.4619 0.6372 11.00000 0.05 0.26 ; _shelx_res_checksum 80493 _shelx_hkl_file ; 0 0 2 -10.50 10.20 0 0 2 -2.70 10.40 0 0 4 3604.54 132.49 0 0 4 3880.91 134.69 0 0 6 8.00 14.10 0 0 6 37.90 17.90 0 0 8 157.98 29.10 0 0 8 138.89 29.40 0 0 -8 157.48 26.90 -2 0 0 0.00 1.50 2 0 0 0.20 1.60 -2 0 0 -3.20 1.60 2 0 2 3186.88 111.39 2 0 2 3384.86 111.19 2 0 2 3313.17 111.39 -2 0 2 3336.17 110.29 -2 0 4 -5.60 12.00 -2 0 4 4.30 12.50 2 0 4 0.00 11.10 2 0 4 -7.10 12.40 -2 0 6 291.87 33.00 2 0 6 269.77 32.70 -2 0 6 339.27 34.70 2 0 6 244.58 32.30 -2 0 -6 264.77 30.00 2 0 8 10.90 17.20 -2 0 8 -17.80 13.70 -2 0 -8 0.20 16.70 2 0 8 5.00 18.50 -2 0 8 -5.10 17.90 -4 0 0 1241.38 42.30 4 0 0 1204.38 42.00 -4 0 0 1224.28 41.80 -4 0 -2 0.70 9.80 -4 0 -2 1.60 9.20 -4 0 -2 -13.40 9.80 -4 0 2 -1.30 8.70 4 0 2 -2.70 10.70 4 0 2 13.20 11.50 4 0 2 -17.70 8.60 4 0 4 20.10 15.60 4 0 4 12.30 12.80 -4 0 4 25.40 13.30 4 0 6 14.20 16.60 -4 0 6 0.50 14.60 -4 0 -6 11.90 17.10 -4 0 6 9.70 16.10 4 0 -6 5.10 12.80 4 0 6 -2.10 12.00 4 0 8 -4.20 17.50 4 0 8 -26.80 15.50 -4 0 8 11.10 17.70 -4 0 -8 20.50 19.70 -4 0 8 5.30 17.60 -6 0 0 3.60 6.90 -6 0 0 -3.00 9.00 6 0 0 -9.10 8.30 -6 0 -2 1768.72 65.99 -6 0 -2 1744.53 64.99 -6 0 -2 1790.92 65.59 6 0 2 1788.42 65.59 6 0 2 1752.32 64.49 -6 0 2 1834.12 62.29 6 0 -2 1784.32 57.19 6 0 2 1615.24 65.39 6 0 4 12.60 13.60 6 0 4 8.70 11.20 -6 0 4 -9.70 11.50 6 0 6 189.78 29.50 -6 0 6 165.28 26.60 -6 0 6 193.48 28.00 -6 0 -6 116.49 24.90 6 0 -6 170.78 20.70 6 0 6 157.08 26.10 -6 0 -8 -21.00 16.90 6 0 8 -8.50 18.90 -6 0 8 -15.60 14.90 6 0 8 32.80 20.90 -6 0 8 17.90 18.20 -8 0 0 3637.94 117.99 8 0 0 3530.45 118.49 -8 0 0 3611.74 118.19 -8 0 -2 -14.50 10.50 -8 0 -2 0.60 10.00 8 0 2 4.80 10.50 -8 0 -2 -17.60 9.30 8 0 -2 -0.50 4.10 8 0 2 -11.90 10.20 8 0 2 1.10 9.60 8 0 4 1018.50 51.99 -8 0 4 1092.89 49.60 8 0 4 1042.30 51.59 8 0 6 -0.30 15.70 -8 0 -6 -26.50 14.20 8 0 -6 24.70 11.90 -8 0 6 16.30 16.90 8 0 6 -8.10 15.40 -8 0 8 56.99 22.20 8 0 8 111.19 27.10 8 0 8 42.10 24.10 -8 0 8 56.99 21.30 -8 0 -8 56.29 23.50 10 0 0 -8.50 9.70 -10 0 0 2.80 2.40 -10 0 0 4.60 10.50 -10 0 0 -5.00 7.00 10 0 2 410.06 23.60 -10 0 -2 296.37 22.50 10 0 2 414.66 25.70 -10 0 -2 318.27 24.00 -10 0 -2 326.97 25.10 10 0 -2 327.97 14.40 10 0 2 447.66 23.90 10 0 4 2.00 12.30 10 0 -4 -10.20 5.20 10 0 4 7.80 14.10 -10 0 4 -11.30 10.50 10 0 6 201.28 28.30 10 0 6 103.09 23.40 -10 0 -6 143.89 27.00 -10 0 6 130.19 23.30 -12 0 0 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133.09 17.80 2 14 2 154.38 18.10 -2 -14 2 144.89 17.40 -2 14 -2 169.58 19.40 -2 -14 2 155.88 16.40 2 14 2 131.49 18.60 2 -14 -2 130.09 17.10 2 -14 -2 138.29 13.90 -2 14 -2 157.78 19.30 2 14 -4 445.16 32.70 2 14 -4 419.46 27.40 -2 14 4 456.25 32.60 -2 14 4 423.76 29.30 -2 14 -4 434.26 32.40 2 14 4 425.36 32.10 2 14 4 452.65 32.80 -2 14 -4 410.36 29.90 -2 14 6 163.28 26.40 2 14 -6 179.88 22.40 2 -14 6 186.78 27.90 -2 14 6 185.28 25.90 2 -14 6 165.18 29.00 -2 14 -6 201.58 26.20 2 14 6 151.38 28.00 -2 -14 6 157.88 26.50 2 14 6 176.18 27.00 -2 14 8 64.39 23.80 2 -14 8 47.90 23.60 2 14 8 29.80 21.80 -2 -14 8 23.60 23.00 4 -14 0 341.27 23.90 4 14 0 380.16 25.40 -4 -14 0 317.47 22.40 -4 -14 0 305.87 20.60 4 -14 0 353.86 15.80 4 -14 0 342.27 22.70 -4 14 0 347.57 23.70 -4 -14 0 307.47 21.60 -4 14 0 376.06 24.00 4 14 0 356.16 22.40 4 -14 2 45.50 14.80 4 -14 2 122.29 18.50 4 14 -2 97.09 13.90 -4 14 2 128.19 18.60 4 14 -2 104.29 15.80 -4 -14 -2 76.29 16.00 -4 -14 -2 84.29 15.30 -4 14 2 94.89 11.90 4 14 2 93.49 15.40 -4 14 -2 76.19 18.30 4 -14 -2 65.59 13.20 -4 -14 2 107.19 14.00 -4 -14 2 88.69 13.90 -4 14 -2 109.19 17.50 4 14 2 106.69 18.10 4 -14 -2 90.29 15.30 4 14 -4 395.96 24.60 -4 14 4 424.36 31.40 -4 14 4 406.16 28.00 4 -14 4 405.36 30.20 4 14 4 434.26 31.60 -4 14 -4 443.06 34.70 4 -14 -4 433.06 31.70 -4 14 -4 394.46 29.30 4 14 4 397.16 31.10 4 14 -6 38.40 13.20 4 -14 6 23.60 18.70 -4 14 6 24.00 14.30 -4 14 6 41.20 18.30 4 -14 6 23.40 19.70 4 14 6 26.00 20.00 -4 -14 6 34.80 20.00 -4 14 -6 19.10 17.00 4 14 6 33.20 19.40 -6 14 0 1906.41 70.79 6 14 0 1910.91 67.29 6 -14 0 1976.70 71.59 -6 14 0 1902.11 71.59 6 14 0 1906.31 72.39 -6 -14 0 1881.01 71.79 6 -14 0 2003.40 60.79 -6 -14 0 1898.81 69.29 6 -14 0 1917.21 69.69 -6 -14 0 1830.82 68.19 6 -14 2 19.60 10.40 6 -14 2 10.20 12.60 6 14 -2 25.10 9.60 6 -14 2 12.40 12.00 -6 -14 -2 14.90 11.40 -6 -14 -2 8.40 12.10 6 14 -2 7.00 10.40 -6 14 2 29.40 7.70 -6 14 2 5.90 10.90 -6 14 2 14.00 12.60 6 -14 -2 3.30 9.20 -6 -14 2 18.10 8.20 6 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41.20 8 -14 4 69.19 18.00 -8 14 4 95.49 15.70 8 14 -4 87.59 11.80 -8 14 4 84.49 18.80 8 14 4 76.49 18.20 8 -14 -4 87.89 15.80 -8 14 -4 82.79 20.90 8 -14 -4 97.19 16.00 8 14 4 83.59 19.50 -8 14 -4 87.89 20.40 8 -14 6 270.87 35.30 8 -14 6 301.37 35.40 -8 14 6 312.17 32.00 -8 14 6 289.97 32.60 8 14 6 322.87 36.40 8 14 6 335.77 36.90 -8 14 -6 320.47 36.20 10 14 0 1170.68 54.89 10 -14 0 1193.98 39.00 10 -14 0 1146.39 50.99 -10 -14 0 1163.48 45.90 -10 14 0 1187.98 50.99 10 -14 0 1217.38 47.20 -10 14 0 1194.78 49.90 10 14 0 1189.28 40.50 -10 -14 0 1206.48 52.89 10 -14 2 7.30 11.90 -10 14 2 33.50 12.10 -10 14 2 18.50 6.40 10 -14 2 16.30 9.80 -10 14 2 31.90 12.70 -10 -14 -2 44.80 12.60 -10 -14 2 47.40 8.80 10 -14 -2 26.90 9.50 10 14 2 48.00 15.20 -10 14 -2 27.40 14.30 10 14 2 11.60 11.20 -10 -14 2 22.00 9.30 -10 14 -2 41.20 14.40 10 -14 -2 45.60 12.80 10 -14 4 415.46 32.50 -10 14 4 386.66 25.40 10 -14 4 419.46 32.70 10 14 -4 371.86 17.30 -10 14 4 440.06 30.80 10 -14 -4 448.96 27.60 10 14 4 337.57 33.00 10 14 4 383.26 32.40 -10 14 -4 403.46 35.40 -10 14 -4 423.16 33.60 10 -14 -4 413.86 26.50 10 -14 6 0.70 19.80 10 -14 6 22.40 18.00 -10 14 6 35.90 18.30 -10 14 6 6.90 12.10 10 14 6 -17.00 16.00 -10 14 -6 -18.30 17.70 10 14 6 17.70 17.90 -10 14 -6 14.90 19.30 12 14 0 415.26 31.10 12 -14 0 410.46 27.50 -12 14 0 422.16 30.10 -12 -14 0 441.76 23.10 -12 14 0 411.46 17.10 12 -14 0 442.26 18.40 12 -14 0 459.25 24.10 -12 14 0 469.65 28.00 -12 -14 -2 49.10 13.30 -12 14 2 58.89 13.50 12 -14 2 41.30 14.20 -12 14 2 44.50 13.80 12 -14 2 47.20 11.40 -12 14 2 45.30 8.10 12 14 2 43.60 12.30 12 14 2 59.49 16.80 -12 -14 2 39.80 7.90 12 -14 -2 47.00 9.70 12 14 2 41.40 11.20 -12 14 -2 49.70 16.10 -12 14 -2 67.59 19.50 12 -14 -2 46.60 12.70 -12 -14 2 33.40 9.30 -12 14 4 48.90 16.20 12 -14 4 68.39 20.20 12 -14 4 66.49 17.80 -12 14 4 77.29 13.90 -12 14 -4 38.80 18.50 12 14 4 97.39 21.60 12 -14 -4 78.79 15.30 12 14 4 101.59 20.50 -12 14 -4 73.19 20.30 12 -14 6 -26.40 12.40 -12 14 6 7.60 16.50 12 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166.38 21.70 -18 14 2 198.68 15.60 18 -14 2 178.28 18.90 18 -14 -2 221.58 22.90 18 14 2 243.98 30.40 -18 14 -2 199.78 24.70 -18 14 -2 220.98 30.30 -18 14 -2 229.68 19.20 -18 -14 2 194.08 14.50 -18 -14 2 190.28 13.50 18 14 2 215.78 10.60 -18 14 4 189.68 23.90 18 -14 4 236.48 27.50 18 -14 4 177.38 25.20 -18 14 -4 199.48 31.50 -18 14 -4 182.68 30.50 18 14 4 240.38 25.30 18 14 4 163.78 28.80 18 -14 6 -9.10 17.30 18 -14 6 28.10 20.80 -18 14 6 19.50 14.20 -18 14 6 19.60 12.50 -18 14 -6 -12.00 19.30 -18 14 -6 13.50 22.50 18 14 6 9.00 21.10 -18 -14 6 34.00 15.80 18 14 6 5.00 17.10 -20 14 0 136.49 14.10 20 14 0 138.49 23.30 -20 14 0 137.39 19.30 -20 14 0 145.89 22.50 20 -14 0 136.29 14.90 -20 -14 0 131.09 13.70 -20 14 2 7.80 7.40 20 -14 2 -1.20 9.30 -20 14 2 10.40 11.20 -20 14 2 15.60 12.40 20 -14 2 10.40 11.60 20 -14 2 20.60 9.80 -20 -14 2 6.20 7.10 -20 14 -2 -1.40 14.00 20 14 2 25.80 17.80 -20 14 -2 1.90 15.50 -20 -14 2 -7.80 5.90 -20 -14 2 -0.60 6.80 20 -14 4 94.79 20.40 -20 14 4 115.39 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421.66 36.00 26 14 0 415.36 40.70 -26 14 0 481.85 32.10 26 -14 2 69.69 17.80 -26 14 2 40.20 15.70 26 14 2 65.09 25.60 -26 14 -2 53.99 22.40 -26 14 -2 78.49 20.50 26 -14 4 111.59 23.50 -26 14 -4 116.29 24.70 26 14 4 109.19 29.20 -26 14 -4 124.89 30.00 -28 -14 0 28.70 17.00 -28 14 0 26.80 17.20 28 14 0 62.19 23.90 -28 -14 -2 1.80 20.30 -28 14 -2 29.50 18.60 28 14 2 0.90 18.20 -28 14 -2 13.50 18.70 -28 14 -4 -1.50 19.20 30 14 0 52.79 24.40 -30 14 0 29.30 17.50 -30 -14 -2 85.89 25.30 -30 14 -2 73.59 23.50 30 14 2 91.49 27.50 32 14 0 -5.70 18.90 -32 14 0 11.10 15.80 -1 15 1 46.80 13.00 -1 15 1 38.10 9.10 -1 15 1 41.40 13.20 1 15 -1 41.60 14.00 1 -15 1 37.50 13.70 1 -15 1 35.20 11.60 1 15 -1 42.00 12.70 -1 -15 -1 39.00 10.60 -1 -15 -1 43.00 11.80 -1 -15 -1 30.50 12.20 -1 -15 1 28.20 12.00 1 -15 -1 32.90 8.10 1 15 1 32.80 12.60 -1 -15 1 37.20 10.70 -1 15 -1 40.20 13.00 1 -15 -1 59.39 14.00 -1 -15 1 56.59 13.10 -1 15 -1 27.50 12.60 1 15 1 49.20 11.10 1 -15 -1 50.09 12.60 -1 15 3 101.99 18.50 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47.00 15.40 0 -20 0 27.70 12.90 0 -20 0 17.00 9.10 0 -20 -2 -0.90 8.10 0 -20 -2 -10.60 11.80 0 -20 2 -7.90 11.70 0 20 -2 -1.90 12.80 0 20 2 -17.20 8.90 0 20 2 3.50 12.30 0 20 -2 -7.60 13.00 0 -20 -2 10.80 11.60 0 -20 2 -4.40 10.60 0 20 4 206.58 27.90 0 20 -4 153.08 23.20 0 20 4 204.48 23.20 0 20 -4 252.27 25.60 0 20 6 -14.40 12.90 0 20 -6 20.40 14.60 0 20 6 -1.20 16.80 2 20 0 845.22 39.30 2 -20 0 787.82 39.90 -2 20 0 776.12 40.80 2 20 0 786.02 40.60 2 -20 0 819.02 40.20 -2 20 0 833.12 40.70 2 20 0 848.62 40.50 2 -20 0 864.01 35.10 -2 -20 0 870.91 41.20 -2 -20 0 802.32 37.90 -2 -20 0 896.31 40.50 2 20 -2 47.70 16.20 -2 20 2 46.20 14.40 -2 -20 -2 43.20 15.00 2 -20 2 34.70 13.80 2 20 -2 33.50 13.70 -2 -20 -2 18.00 10.60 -2 20 2 22.00 9.80 -2 -20 2 30.20 13.70 2 20 2 35.30 12.20 2 20 2 43.40 15.40 -2 -20 2 53.39 13.70 -2 20 -2 28.30 14.70 -2 20 -2 14.50 14.10 2 -20 -2 50.09 15.00 2 -20 -2 21.80 11.80 2 -20 -2 35.50 9.50 2 20 -4 228.08 26.20 2 20 -4 255.37 24.00 -2 20 4 204.98 23.50 -2 20 4 212.08 26.90 -2 -20 4 224.78 23.40 2 20 4 178.38 23.10 -2 20 -4 238.38 25.90 2 20 4 206.28 26.80 -2 20 -4 185.08 25.30 -2 20 6 64.99 22.00 -2 20 6 6.30 15.30 2 -20 6 24.30 18.50 2 20 -6 59.69 17.30 -2 20 -6 43.70 19.10 2 20 6 35.30 18.10 2 20 6 64.29 22.40 4 -20 0 65.89 15.40 4 -20 0 56.89 9.00 -4 20 0 84.49 17.60 -4 -20 0 55.89 14.70 -4 -20 0 50.59 12.60 4 20 0 40.00 15.10 4 -20 0 75.49 15.70 4 20 0 33.90 12.50 4 20 0 28.60 13.50 -4 20 0 52.89 15.40 -4 -20 0 60.79 16.10 -4 20 2 1386.26 51.29 4 -20 2 1375.56 58.89 -4 20 2 1357.66 59.49 -4 20 2 1312.17 58.49 4 20 -2 1344.87 56.69 -4 -20 -2 1355.06 57.69 4 20 -2 1385.56 55.49 4 -20 -2 1397.16 50.99 4 20 2 1317.67 58.59 -4 -20 2 1453.65 55.09 -4 20 -2 1268.17 59.09 4 20 2 1341.17 57.99 -4 -20 2 1336.57 56.59 4 -20 -2 1444.16 59.19 -4 20 -2 1361.46 58.99 4 -20 -2 1361.56 57.69 4 20 -4 -13.00 11.50 -4 20 4 3.70 9.80 4 20 -4 4.90 14.60 -4 20 4 29.30 15.40 -4 20 -4 19.90 18.20 4 20 4 3.30 11.90 -4 20 -4 -0.10 14.70 -4 -20 4 13.50 11.50 4 20 4 -3.40 15.70 4 -20 6 156.28 26.40 4 20 -6 185.38 21.90 -4 20 6 157.48 23.50 -4 20 6 169.18 29.50 -4 20 -6 214.08 28.70 4 20 6 118.09 24.30 4 20 6 206.88 32.10 -6 -20 0 2011.90 77.89 -6 -20 0 2019.90 79.49 6 -20 0 2126.19 68.39 6 -20 0 2069.79 79.09 6 -20 0 2118.39 80.39 6 20 0 2110.69 80.09 -6 20 0 2111.79 81.19 -6 -20 0 2150.08 78.59 6 20 0 2062.19 76.09 -6 20 0 2018.00 80.99 6 20 -2 79.39 14.20 -6 20 2 92.89 10.60 -6 20 2 59.79 15.60 -6 20 2 47.90 14.80 6 20 -2 55.89 14.50 -6 -20 2 77.69 13.80 6 -20 -2 88.09 18.10 -6 20 -2 113.09 19.20 6 -20 -2 60.19 14.10 6 20 2 68.29 15.20 -6 20 -2 67.19 17.00 6 20 2 85.59 17.60 -6 -20 2 65.29 14.50 6 -20 4 394.76 31.50 -6 20 4 329.07 24.90 6 20 -4 360.06 24.50 -6 20 4 344.57 32.60 6 20 -4 325.77 27.70 -6 -20 4 324.07 23.40 -6 20 -4 354.66 34.10 6 20 4 383.56 31.90 6 20 4 292.07 30.90 -6 20 -4 319.07 33.00 6 -20 6 23.20 16.50 6 -20 6 26.70 19.10 -6 20 6 58.49 22.40 6 20 -6 23.00 21.00 -6 20 6 24.50 14.60 6 20 6 14.70 18.50 6 20 6 30.30 18.80 -6 20 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-20 2 91.29 13.70 -10 20 2 115.69 18.70 -10 20 2 67.89 16.90 10 20 -2 73.39 11.50 -10 20 2 105.29 8.50 -10 20 -2 95.09 19.20 10 20 2 75.89 17.50 -10 20 -2 113.69 22.90 10 20 2 92.89 17.10 -10 -20 2 61.79 13.50 10 -20 -2 79.59 15.20 -10 -20 2 65.19 12.30 10 20 -4 284.97 18.20 -10 20 4 261.47 21.70 -10 20 4 230.78 27.00 10 -20 4 252.27 27.60 -10 20 -4 250.07 30.20 10 20 4 297.47 31.10 10 20 4 246.88 30.70 -10 20 -4 312.57 36.00 -10 20 6 15.90 16.70 -10 20 6 21.10 13.80 10 -20 6 20.10 17.60 10 -20 6 32.10 20.40 -10 20 -6 22.90 18.80 -10 20 -6 30.00 23.10 10 20 6 -11.50 15.40 10 20 6 26.70 18.60 -12 -20 0 267.97 21.80 12 20 0 324.67 31.40 -12 20 0 320.17 26.60 -12 -20 0 333.57 25.10 12 20 0 306.57 17.60 -12 20 0 332.37 27.90 12 -20 0 296.17 22.20 -12 20 2 1039.80 49.90 -12 20 2 1032.90 50.29 12 -20 2 1045.10 44.50 -12 20 2 1105.09 35.70 -12 20 2 1078.49 35.60 -12 20 -2 1152.18 54.99 12 20 2 1008.00 46.40 -12 -20 2 1007.20 42.40 -12 20 -2 1026.70 51.59 12 -20 -2 1055.69 45.60 12 20 2 1000.50 53.69 -12 -20 2 1040.70 45.70 -12 20 4 76.59 17.70 12 -20 4 42.70 14.80 -12 20 4 56.09 12.10 12 20 4 28.50 17.90 12 20 4 71.09 19.90 -12 20 -4 53.59 19.80 -12 20 -4 85.29 23.90 -12 20 6 192.48 24.30 12 -20 6 146.59 29.50 12 -20 6 156.88 28.10 12 20 6 146.99 26.70 -12 20 -6 131.49 27.30 12 20 6 115.19 27.80 -12 20 -6 154.38 30.00 14 20 0 824.22 47.00 -14 -20 0 813.12 38.60 -14 20 0 867.01 44.60 -14 20 0 895.51 45.30 14 -20 0 781.32 38.00 14 -20 2 52.39 12.10 -14 20 2 64.79 17.20 -14 20 2 77.99 17.50 -14 20 -2 80.89 20.50 14 20 2 38.70 13.20 -14 20 -2 36.90 17.30 -14 -20 2 57.19 11.80 -14 -20 2 67.99 13.20 14 20 2 52.79 18.20 14 -20 -2 72.19 12.40 14 20 2 45.10 12.40 14 -20 4 186.28 24.30 -14 20 4 186.08 17.80 -14 20 4 213.28 27.10 14 -20 4 181.78 27.50 14 20 4 194.18 25.80 -14 20 -4 178.68 30.70 14 20 4 174.08 27.40 -14 20 -4 152.38 26.50 -14 20 6 16.30 12.60 14 -20 6 30.00 18.50 14 -20 6 49.60 23.00 -14 20 6 4.60 15.30 14 20 6 23.00 20.80 -14 20 -6 14.00 20.10 -14 20 -6 64.79 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132.09 23.40 -1 23 7 55.39 22.60 1 -23 7 27.50 18.30 1 -23 7 46.10 20.70 -1 23 7 -2.60 14.50 1 23 7 5.00 14.90 1 23 7 26.30 21.50 -1 23 -7 45.40 19.30 3 23 -1 460.15 32.10 -3 23 1 485.05 33.10 -3 23 1 556.04 25.80 -3 23 1 500.05 34.10 3 23 -1 509.45 30.10 3 -23 1 539.75 28.40 -3 -23 -1 456.25 28.60 3 -23 1 477.95 31.80 -3 -23 1 475.75 31.10 3 -23 -1 523.15 24.20 -3 23 -1 459.35 33.10 3 23 1 508.95 31.30 -3 -23 1 551.34 32.00 -3 -23 1 473.65 30.50 -3 23 -1 449.56 32.10 3 23 1 484.45 31.10 3 -23 -1 523.15 32.20 3 23 -3 327.37 25.90 -3 23 3 260.17 22.30 -3 23 3 336.07 32.60 3 23 -3 335.77 28.60 3 23 3 328.07 30.90 3 -23 -3 293.87 21.40 -3 -23 3 302.87 24.70 3 23 3 299.77 28.10 -3 23 -3 356.26 33.60 -3 23 -3 312.37 29.50 3 23 -5 210.28 24.00 -3 23 5 118.29 20.70 -3 23 5 151.78 26.00 3 23 -5 134.59 24.80 3 23 5 188.28 28.30 -3 23 -5 165.38 30.20 3 23 5 164.38 24.60 -3 23 -5 195.68 26.70 -3 23 7 39.70 21.90 3 -23 7 -11.20 17.10 3 -23 7 36.40 21.60 -3 23 7 3.10 14.80 3 23 7 -2.90 14.20 -3 23 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50 0 3.60 19.60 -6 50 0 -10.70 21.30 6 50 -2 208.78 31.60 -6 50 2 211.08 36.10 6 50 2 116.89 30.00 -6 50 -2 199.68 34.50 6 50 2 162.98 27.20 -6 50 -2 206.28 35.50 -8 50 0 -1.50 24.30 -8 50 0 -5.20 18.70 8 50 0 -20.70 19.00 8 50 -2 -22.70 17.50 -8 50 2 -24.00 19.80 8 50 2 14.10 19.70 -8 50 -2 -8.30 22.90 8 50 2 9.10 22.20 -8 50 -2 15.30 24.30 -10 50 0 -3.60 22.50 -10 50 0 -3.40 24.30 10 50 0 -7.70 18.20 -12 50 0 302.27 44.00 -12 50 0 355.86 45.20 1 51 -1 79.89 23.40 -1 51 1 39.40 24.90 1 51 -1 50.49 26.20 -1 51 -1 66.19 28.10 1 51 1 43.70 23.40 -1 51 -1 44.50 22.50 -3 51 1 36.70 25.70 3 51 -1 70.59 23.50 3 51 -1 16.30 23.60 -3 51 -1 43.90 24.30 -3 51 -1 53.19 26.70 3 51 1 -12.90 22.50 5 51 -1 21.40 20.60 -5 51 1 56.69 27.10 -5 51 1 44.60 22.00 5 51 1 1.30 20.00 -5 51 -1 21.50 25.90 -5 51 -1 13.70 20.00 -7 51 1 84.29 29.00 7 51 -1 92.49 24.90 -7 51 1 108.39 27.10 -7 51 -1 104.09 27.40 -7 51 -1 95.69 28.40 7 51 1 101.69 24.60 -9 51 1 59.09 25.20 9 51 -1 56.69 22.50 -9 51 1 69.59 31.60 -9 51 -1 -10.40 24.40 -9 51 -1 62.19 24.50 9 51 1 5.50 20.50 0 52 0 190.38 33.50 0 52 0 106.49 29.00 0 52 -2 38.30 22.90 0 52 2 -0.40 23.30 0 52 -2 -7.50 20.00 -2 52 0 52.99 25.80 -2 52 0 52.79 22.50 2 52 0 48.20 26.50 2 52 -2 116.59 27.50 -2 52 2 75.09 30.70 2 52 -2 62.69 27.30 -2 52 -2 112.89 27.80 2 52 2 53.39 28.10 -2 52 -2 62.89 29.00 -4 52 0 3.30 20.00 4 52 0 -4.20 19.80 -4 52 0 -18.20 23.50 -4 52 2 20.10 23.60 4 52 -2 39.90 25.40 4 52 2 21.80 24.30 -4 52 -2 34.30 25.90 6 52 0 76.29 24.60 -6 52 0 52.39 26.40 -6 52 0 76.59 27.40 8 52 0 256.67 34.20 -8 52 0 246.78 39.60 -8 52 0 230.88 38.30 1 53 -1 32.90 21.70 1 53 -1 16.00 23.90 -1 53 1 9.40 24.00 -1 53 -1 24.50 21.90 1 53 1 9.40 25.50 -1 53 -1 13.20 22.70 3 53 -1 91.69 26.00 -3 53 1 141.69 30.90 3 53 1 80.39 26.90 -3 53 -1 84.39 25.50 -3 53 -1 63.29 26.60 -5 53 1 128.69 34.00 5 53 -1 93.49 25.90 -5 53 -1 151.38 34.70 5 53 1 120.79 30.10 0 54 0 -8.30 23.80 -2 54 0 27.30 24.30 2 54 0 91.59 29.20 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 53373 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' 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 Na1 Na 0.45635(8) 0.47515(5) 0.3565(5) 0.0258(7) Uani 1 1 d . . . O1 O 0.68590(15) 0.40554(10) 0.3073(7) 0.0270(12) Uani 1 1 d . . . O1S O 0.500000 0.500000 0.5959(10) 0.0220(17) Uani 1 2 d DS T P H1S H 0.4818(18) 0.5113(11) 0.680(6) 0.033 Uiso 1 1 d DR . . O2S O 0.500000 0.500000 0.1074(11) 0.0206(16) Uani 1 2 d DS T P H2S H 0.486(2) 0.5136(8) 0.025(6) 0.031 Uiso 1 1 d DR . . O3S O 0.40899(16) 0.45786(11) 0.0835(9) 0.0385(16) Uani 1 1 d D . . H3SA H 0.3799(15) 0.4478(12) 0.104(12) 0.058 Uiso 1 1 d DR . . H3SB H 0.398(2) 0.4757(10) 0.027(11) 0.058 Uiso 1 1 d DR . . O4S O 0.42263(15) 0.44667(12) 0.6184(10) 0.0376(13) Uani 1 1 d D . . H4SA H 0.3934(15) 0.4441(17) 0.555(9) 0.056 Uiso 1 1 d DR . . H4SB H 0.414(2) 0.4584(16) 0.723(8) 0.056 Uiso 1 1 d DR . . N1 N 0.53071(19) 0.44287(12) 0.3189(8) 0.0245(14) Uani 1 1 d . . . N2 N 0.53149(19) 0.41357(12) 0.2706(8) 0.0224(14) Uani 1 1 d . . . N5 N 0.67486(16) 0.45586(11) 0.3648(10) 0.0222(13) Uani 1 1 d . . . N7 N 0.59484(17) 0.47780(10) 0.3765(10) 0.0224(12) Uani 1 1 d . . . C3 C 0.5758(2) 0.40187(16) 0.2571(10) 0.0235(17) Uani 1 1 d . . . H3 H 0.583736 0.381832 0.225227 0.028 Uiso 1 1 calc R . . C3A C 0.6074(2) 0.42464(15) 0.2987(10) 0.0214(17) Uani 1 1 d . . . C4 C 0.6573(2) 0.42947(15) 0.3229(10) 0.0230(17) Uani 1 1 d . . . C6 C 0.6421(2) 0.47856(14) 0.3865(13) 0.0252(15) Uani 1 1 d . . . H6 H 0.655517 0.497644 0.412596 0.030 Uiso 1 1 calc R . . C7A C 0.5777(2) 0.44989(15) 0.3336(10) 0.0227(17) Uani 1 1 d . . . C8 C 0.4856(2) 0.39816(15) 0.2376(11) 0.0310(19) Uani 1 1 d . . . H8A H 0.467606 0.397130 0.359760 0.046 Uiso 1 1 calc GR . . H8B H 0.491910 0.377903 0.190087 0.046 Uiso 1 1 calc GR . . H8C H 0.466777 0.409150 0.140816 0.046 Uiso 1 1 calc GR . . C9 C 0.7359(2) 0.40944(15) 0.3654(14) 0.0347(19) Uani 1 1 d . . . H9A H 0.752934 0.421025 0.266121 0.052 Uiso 1 1 calc GR . . H9B H 0.751181 0.389841 0.379405 0.052 Uiso 1 1 calc GR . . H9C H 0.737180 0.420074 0.489695 0.052 Uiso 1 1 calc GR . . O1B O 0.35578(17) 0.61077(11) 0.7329(7) 0.0340(13) Uani 1 1 d . . . N1B N 0.37731(18) 0.51135(13) 0.8891(12) 0.0321(14) Uani 1 1 d . . . N2B N 0.32954(17) 0.51919(14) 0.8809(11) 0.0330(15) Uani 1 1 d . . . N5B N 0.4334(2) 0.59274(13) 0.7591(8) 0.0277(15) Uani 1 1 d . . . N7B N 0.44847(18) 0.54119(13) 0.8428(9) 0.0265(15) Uani 1 1 d . . . C3AB C 0.3665(2) 0.56077(16) 0.8185(10) 0.0256(18) Uani 1 1 d . . . C3B C 0.3214(2) 0.54738(17) 0.8393(11) 0.031(2) Uani 1 1 d . . . H3B H 0.290938 0.556782 0.826072 0.038 Uiso 1 1 calc R . . C4B C 0.3863(3) 0.58833(17) 0.7701(11) 0.0317(19) Uani 1 1 d . . . C6B C 0.4612(2) 0.56846(17) 0.7963(10) 0.0291(18) Uani 1 1 d . . . H6B H 0.494926 0.571730 0.787179 0.035 Uiso 1 1 calc R . . C7AB C 0.3992(2) 0.53712(16) 0.8521(11) 0.0263(18) Uani 1 1 d . . . C8B C 0.2938(2) 0.49559(18) 0.9107(14) 0.048(2) Uani 1 1 d . . . H8BA H 0.297478 0.480319 0.809807 0.072 Uiso 1 1 calc GR . . H8BB H 0.261356 0.504155 0.903360 0.072 Uiso 1 1 calc GR . . H8BC H 0.298552 0.486506 1.038777 0.072 Uiso 1 1 calc GR . . C9B C 0.3765(3) 0.63913(16) 0.6723(14) 0.043(2) Uani 1 1 d . . . H9BA H 0.398023 0.635843 0.561560 0.064 Uiso 1 1 calc GR . . H9BB H 0.394736 0.647807 0.780259 0.064 Uiso 1 1 calc GR . . H9BC H 0.350636 0.652821 0.634237 0.064 Uiso 1 1 calc GR . . I1 I 0.31223(2) 0.43405(2) 0.38593(12) 0.03128(14) 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 Na1 0.0250(13) 0.0201(14) 0.0323(19) 0.0007(14) 0.0008(14) 0.0004(11) O1 0.026(2) 0.024(3) 0.031(3) 0.000(2) 0.005(2) 0.009(2) O1S 0.027(4) 0.022(4) 0.017(5) 0.000 0.000 0.010(3) O2S 0.024(3) 0.015(4) 0.023(5) 0.000 0.000 0.004(3) O3S 0.024(2) 0.022(3) 0.070(5) -0.007(3) -0.004(3) -0.004(2) O4S 0.033(3) 0.049(3) 0.031(4) -0.006(3) 0.003(3) -0.007(2) N1 0.030(3) 0.015(3) 0.028(4) 0.000(3) 0.005(3) -0.001(3) N2 0.027(3) 0.017(3) 0.023(4) 0.000(3) -0.002(3) 0.002(3) N5 0.021(3) 0.020(3) 0.025(4) 0.000(3) 0.004(3) 0.003(2) N7 0.026(3) 0.014(3) 0.027(3) 0.002(3) 0.003(4) -0.001(2) C3 0.025(4) 0.019(4) 0.026(4) 0.007(3) 0.000(3) 0.005(3) C3A 0.025(4) 0.020(4) 0.019(4) 0.001(3) 0.004(3) 0.003(3) C4 0.026(4) 0.024(4) 0.019(4) -0.003(3) 0.000(3) 0.002(3) C6 0.034(4) 0.019(4) 0.023(4) 0.001(4) 0.001(5) -0.004(3) C7A 0.025(4) 0.024(4) 0.019(4) 0.002(3) -0.002(3) -0.005(3) C8 0.029(4) 0.020(4) 0.044(5) 0.004(4) -0.001(4) -0.010(3) C9 0.021(4) 0.032(4) 0.051(6) -0.006(5) 0.001(5) 0.006(3) O1B 0.035(3) 0.032(3) 0.035(3) -0.004(3) -0.002(2) 0.014(3) N1B 0.026(3) 0.040(4) 0.030(4) 0.010(4) -0.003(4) 0.002(3) N2B 0.020(3) 0.051(4) 0.027(4) 0.011(4) 0.000(4) -0.001(3) N5B 0.031(4) 0.027(4) 0.025(4) -0.006(3) -0.004(3) 0.010(3) N7B 0.026(3) 0.028(4) 0.026(4) -0.002(3) -0.001(3) 0.007(3) C3AB 0.025(4) 0.029(4) 0.023(4) -0.004(3) -0.001(3) 0.008(3) C3B 0.028(4) 0.043(5) 0.022(5) 0.009(4) 0.001(3) 0.015(4) C4B 0.039(5) 0.036(5) 0.021(5) -0.004(4) -0.002(4) 0.011(4) C6B 0.025(4) 0.034(5) 0.027(4) -0.005(4) -0.002(3) 0.006(4) C7AB 0.022(4) 0.039(5) 0.018(5) 0.001(4) 0.003(3) 0.008(3) C8B 0.032(4) 0.065(6) 0.047(6) 0.021(5) 0.001(5) -0.006(4) C9B 0.046(4) 0.032(5) 0.051(7) 0.000(5) -0.003(4) 0.015(4) I1 0.0260(2) 0.0211(2) 0.0468(3) 0.0029(3) -0.0026(3) -0.0015(2) 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 Na1 Na1 H4SA 148.3(10) 2_665 . O1S Na1 Na1 45.03(14) . 2_665 O1S Na1 O2S 91.19(18) . . O1S Na1 O3S 170.03(19) . . O1S Na1 O4S 85.7(2) . . O1S Na1 H4SA 103.4(9) . . O1S Na1 N1 85.44(16) . . O1S Na1 N7 81.77(16) . 2_665 O2S Na1 Na1 46.16(15) . 2_665 O2S Na1 O3S 82.4(2) . . O2S Na1 O4S 172.04(17) . . O2S Na1 H4SA 165.0(9) . . O2S Na1 N1 77.16(14) . . O2S Na1 N7 86.35(16) . 2_665 O3S Na1 Na1 128.07(15) . 2_665 O3S Na1 H4SA 82.7(9) . . O3S Na1 N1 100.4(2) . . O3S Na1 N7 90.2(2) . 2_665 O4S Na1 Na1 130.34(15) . 2_665 O4S Na1 O3S 101.6(2) . . O4S Na1 H4SA 20.7(9) . . O4S Na1 N1 95.26(18) . . O4S Na1 N7 100.5(2) . 2_665 N1 Na1 Na1 77.60(15) . 2_665 N1 Na1 H4SA 107.1(15) . . N1 Na1 N7 158.88(19) . 2_665 N7 Na1 Na1 81.47(14) 2_665 2_665 N7 Na1 H4SA 92.2(15) 2_665 . C4 O1 C9 116.6(5) . . Na1 O1S Na1 89.9(3) 2_665 . Na1 O1S H1S 115(4) 2_665 2_665 Na1 O1S H1S 118(4) . 2_665 Na1 O1S H1S 118(4) 2_665 . Na1 O1S H1S 115(4) . . H1S O1S H1S 102(4) . 2_665 Na1 O2S Na1 87.7(3) 2_665 . Na1 O2S H2S 111(3) 2_665 . Na1 O2S H2S 111(3) . 2_665 Na1 O2S H2S 122(4) . . Na1 O2S H2S 122(4) 2_665 2_665 H2S O2S H2S 104(4) . 2_665 Na1 O3S H3SA 121(5) . . Na1 O3S H3SB 103(5) . . H3SA O3S H3SB 100(3) . . Na1 O4S H4SA 93(5) . . Na1 O4S H4SB 112(6) . . H4SA O4S H4SB 103(4) . . N2 N1 Na1 126.2(4) . . C7A N1 Na1 130.5(4) . . C7A N1 N2 103.2(5) . . N1 N2 C8 118.7(5) . . C3 N2 N1 114.2(5) . . C3 N2 C8 127.0(6) . . C4 N5 C6 116.4(5) . . C6 N7 Na1 122.6(4) . 2_665 C6 N7 C7A 112.4(5) . . C7A N7 Na1 123.3(4) . 2_665 N2 C3 H3 126.8 . . N2 C3 C3A 106.4(6) . . C3A C3 H3 126.8 . . C3 C3A C4 139.9(6) . . C3 C3A C7A 104.7(6) . . C4 C3A C7A 115.3(6) . . O1 C4 C3A 116.8(6) . . N5 C4 O1 121.2(6) . . N5 C4 C3A 122.0(6) . . N5 C6 H6 115.2 . . N7 C6 N5 129.6(6) . . N7 C6 H6 115.2 . . N1 C7A N7 124.5(6) . . N1 C7A C3A 111.4(6) . . N7 C7A C3A 124.2(6) . . 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 . . 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 . . C4B O1B C9B 117.4(6) . . C7AB N1B N2B 102.2(5) . . N1B N2B C8B 117.7(6) . . C3B N2B N1B 114.9(6) . . C3B N2B C8B 127.4(6) . . C4B N5B C6B 115.6(6) . . C6B N7B C7AB 113.7(6) . . C3B C3AB C7AB 103.7(6) . . C4B C3AB C3B 139.4(7) . . C4B C3AB C7AB 116.8(6) . . N2B C3B C3AB 106.3(6) . . N2B C3B H3B 126.8 . . C3AB C3B H3B 126.8 . . O1B C4B C3AB 117.5(7) . . N5B C4B O1B 120.1(7) . . N5B C4B C3AB 122.4(7) . . N5B C6B H6B 115.2 . . N7B C6B N5B 129.6(6) . . N7B C6B H6B 115.2 . . N1B C7AB N7B 125.2(6) . . N1B C7AB C3AB 112.9(6) . . N7B C7AB C3AB 121.9(6) . . 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 . . 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 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Na1 Na1 3.292(5) 2_665 Na1 O1S 2.329(6) . Na1 O2S 2.376(6) . Na1 O3S 2.421(6) . Na1 O4S 2.399(7) . Na1 H4SA 2.62(7) . Na1 N1 2.534(6) . Na1 N7 2.546(5) 2_665 O1 C4 1.339(7) . O1 C9 1.455(7) . O1S H1S 0.92(2) . O1S H1S 0.92(2) 2_665 O2S H2S 0.92(2) . O2S H2S 0.92(2) 2_665 O3S H3SA 0.94(3) . O3S H3SB 0.94(3) . O4S H4SA 0.93(3) . O4S H4SB 0.92(3) . N1 N2 1.354(7) . N1 C7A 1.347(8) . N2 C3 1.340(8) . N2 C8 1.466(8) . N5 C4 1.311(8) . N5 C6 1.373(7) . N7 C6 1.314(7) . N7 C7A 1.370(8) . C3 H3 0.9500 . C3 C3A 1.376(9) . C3A C4 1.412(9) . C3A C7A 1.420(9) . C6 H6 0.9500 . C8 H8A 0.9800 . C8 H8B 0.9800 . C8 H8C 0.9800 . C9 H9A 0.9800 . C9 H9B 0.9800 . C9 H9C 0.9800 . O1B C4B 1.340(8) . O1B C9B 1.455(8) . N1B N2B 1.374(7) . N1B C7AB 1.329(8) . N2B C3B 1.314(8) . N2B C8B 1.465(8) . N5B C4B 1.324(9) . N5B C6B 1.358(8) . N7B C6B 1.311(8) . N7B C7AB 1.383(8) . C3AB C3B 1.396(9) . C3AB C4B 1.392(10) . C3AB C7AB 1.413(9) . C3B H3B 0.9500 . C6B H6B 0.9500 . C8B H8BA 0.9800 . C8B H8BB 0.9800 . C8B H8BC 0.9800 . C9B H9BA 0.9800 . C9B H9BB 0.9800 . C9B H9BC 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 H1S N7B 0.92(2) 1.98(3) 2.888(7) 171(6) . yes O2S H2S N7B 0.92(2) 2.05(3) 2.961(7) 174(6) 1_554 yes O3S H3SA I1 0.94(3) 2.77(5) 3.563(5) 143(7) . yes O3S H3SB N1B 0.94(3) 1.94(3) 2.882(8) 175(8) 1_554 yes O4S H4SB O3S 0.92(3) 2.49(5) 3.262(9) 142(7) 1_556 yes