#------------------------------------------------------------------------------ #$Date: 2022-12-14 01:15:54 +0200 (Wed, 14 Dec 2022) $ #$Revision: 279877 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/81/1568120.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_1568120 loop_ _publ_author_name 'Cohen, Seth M.' 'Karges, Johannes' 'Giardini , Miriam' 'Blacque, Olivier' 'Woodworth, Brendon' 'Siqueira-Neto , Jair' _publ_section_title ; Enantioselective Inhibition of the SARS-CoV-2 Main Protease with Rhenium(I) Picolinic Acid Complexes ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D2SC05473F _journal_year 2022 _chemical_formula_moiety 'C9 H6 N O7 Re' _chemical_formula_sum 'C9 H6 N O7 Re' _chemical_formula_weight 426.35 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2021-03-16 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _audit_update_record ; 2022-09-06 deposited with the CCDC. 2022-12-13 downloaded from the CCDC. ; _cell_angle_alpha 88.048(3) _cell_angle_beta 76.353(3) _cell_angle_gamma 84.465(4) _cell_formula_units_Z 2 _cell_length_a 7.2397(3) _cell_length_b 8.0044(4) _cell_length_c 9.5362(2) _cell_measurement_reflns_used 10143 _cell_measurement_temperature 160(1) _cell_measurement_theta_max 78.7350 _cell_measurement_theta_min 4.7610 _cell_volume 534.48(4) _computing_cell_refinement 'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL (Sheldrick, 2015b)' _computing_structure_solution 'SHELXT (Sheldrick, 2015a)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 160(1) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 5.8140 _diffrn_detector_type 'Pilatus 200K' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.996 _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 29.00 125.00 0.50 0.12 -- 51.79 77.00 0.00 192 2 \w 92.00 178.00 0.50 0.49 -- 107.75 61.00 120.00 172 3 \w 95.00 178.00 0.50 0.49 -- 107.75 16.00 144.00 166 4 \w 40.00 132.00 0.50 0.12 -- 51.79 16.00 144.00 184 5 \w 29.00 125.00 0.50 0.12 -- 51.79 77.00 -60.00 192 6 \w 29.00 125.00 0.50 0.12 -- 51.79 77.00-120.00 192 7 \w 95.00 178.00 0.50 0.49 -- 107.75 45.00-180.00 166 8 \w 34.00 130.00 0.50 0.49 -- 107.75 -77.00 60.00 192 9 \w 37.00 124.00 0.50 0.49 -- 107.75 -61.00 60.00 174 10 \w 37.00 124.00 0.50 0.49 -- 107.75 -61.00 150.00 174 11 \w 32.00 120.00 0.50 0.49 -- 107.75 -45.00 60.00 176 12 \w 37.00 124.00 0.50 0.49 -- 107.75 -61.00 -60.00 174 13 \w -21.00 67.00 0.50 0.12 -- 51.79 -57.00-180.00 176 14 \w 34.00 130.00 0.50 0.49 -- 107.75 -77.00-180.00 192 15 \w 28.00 120.00 0.50 0.49 -- 107.75 -16.00 -25.00 184 16 \w 30.00 120.00 0.50 0.49 -- 107.75 -30.00-180.00 180 17 \w 28.00 120.00 0.50 0.49 -- 107.75 -15.00-180.00 184 18 \w -27.00 65.00 0.50 0.12 -- 51.79 -16.00 -25.00 184 19 \w 31.00 106.00 0.50 0.49 -- 107.75 -94.00 -30.00 150 20 \w 31.00 106.00 0.50 0.49 -- 107.75 -94.00 30.00 150 21 \w 31.00 109.00 0.50 0.49 -- 107.75-111.00 30.00 156 22 \w 31.00 106.00 0.50 0.49 -- 107.75 -94.00 60.00 150 23 \w 31.00 109.00 0.50 0.49 -- 107.75-111.00 -60.00 156 24 \w 31.00 109.00 0.50 0.49 -- 107.75-111.00-120.00 156 25 \w -83.00 -9.00 0.50 0.49 -- -86.25 111.00 -90.00 148 26 \w -65.00 28.00 0.50 0.12 -- -51.79 16.00 144.00 186 27 \w -99.00 -6.00 0.50 0.49 -- -86.25 16.00 144.00 186 28 \w -132.00 -39.00 0.50 0.12 -- -51.79 -16.00 -25.00 186 29 \w -166.00 -73.00 0.50 0.49 -- -86.25 -16.00 -25.00 186 30 \w -125.00 -29.00 0.50 0.12 -- -51.79 -77.00 -90.00 192 31 \w -125.00 -29.00 0.50 0.12 -- -51.79 -77.00 90.00 192 32 \w -124.00 -37.00 0.50 0.12 -- -51.79 -57.00 150.00 174 33 \w -126.00 -73.00 0.50 0.12 -- -51.79-125.00 30.00 106 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, Pilatus 200K' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.1277555000 _diffrn_orient_matrix_UB_12 -0.1609001000 _diffrn_orient_matrix_UB_13 0.0179445000 _diffrn_orient_matrix_UB_21 -0.1756919000 _diffrn_orient_matrix_UB_22 -0.1016280000 _diffrn_orient_matrix_UB_23 0.0301875000 _diffrn_orient_matrix_UB_31 0.0340836000 _diffrn_orient_matrix_UB_32 -0.0343341000 _diffrn_orient_matrix_UB_33 -0.1625018000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_unetI/netI 0.0215 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 10649 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.492 _diffrn_reflns_theta_min 4.772 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 22.569 _exptl_absorpt_correction_T_max 0.714 _exptl_absorpt_correction_T_min 0.115 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.649 _exptl_crystal_description needle _exptl_crystal_F_000 396 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.542 _refine_diff_density_min -1.160 _refine_diff_density_rms 0.171 _refine_ls_extinction_coef 0.00099(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 166 _refine_ls_number_reflns 2165 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.126 _refine_ls_R_factor_all 0.0226 _refine_ls_R_factor_gt 0.0218 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+0.7536P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.0589 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2116 _reflns_number_total 2165 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d2sc05473f2.cif _cod_data_source_block 38 _cod_database_code 1568120 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.661 _shelx_estimated_absorpt_t_min 0.074 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All O(H) groups, All O(H,H) groups 2.a Rotating group: O4(H4A,H4B), O5(H5) 2.b Aromatic/amide H refined with riding coordinates: C5(H5A), C6(H6), C7(H7) ; _shelx_res_file ; TITL joha1603_a.res in P-1 joha1603.res created by SHELXL-2018/3 at 10:57:34 on 16-Mar-2021 CELL 1.54184 7.239716 8.004352 9.536214 88.048 76.3532 84.4654 ZERR 2 0.000345 0.000365 0.00021 0.003 0.0032 0.0038 LATT 1 SFAC C H N O Re UNIT 18 12 2 14 2 EQIV $1 1-X,-Y,1-Z EQIV $2 1-X,1-Y,1-Z EQIV $3 +X,-1+Y,+Z EQIV $4 -1+X,+Y,1+Z L.S. 10 0 0 PLAN 20 SIZE 0.02 0.04 0.24 TEMP -113.1(10) CONF HTAB O4 O2_$1 HTAB O4 O7_$2 HTAB O5 O6_$3 HTAB C5 O6_$3 HTAB C6 O1_$4 list 4 MORE -1 BOND $H fmap 2 53 acta OMIT -2 2 10 OMIT 2 1 11 REM REM REM WGHT 0.039000 0.753600 EXTI 0.000985 FVAR 4.51154 RE1 5 0.661005 0.275463 0.628215 11.00000 0.01610 0.01294 = 0.01301 -0.00027 -0.00032 -0.00388 O1 4 0.948612 0.399653 0.364466 11.00000 0.03601 0.03020 = 0.02240 -0.00006 0.00792 -0.01188 O2 4 0.808881 -0.072986 0.510722 11.00000 0.02391 0.02313 = 0.04963 -0.01741 0.00275 -0.00328 O3 4 0.992371 0.240324 0.776484 11.00000 0.02456 0.03709 = 0.02669 0.00374 -0.01011 -0.00616 O4 4 0.415661 0.316407 0.531373 11.00000 0.02462 0.02153 = 0.01985 0.00306 -0.00852 -0.00676 AFIX 7 H4A 2 0.358994 0.224916 0.537741 11.00000 -1.50000 H4B 2 0.425241 0.346340 0.441454 11.00000 -1.50000 AFIX 0 O5 4 0.457288 -0.058301 0.777452 11.00000 0.03097 0.01193 = 0.02349 -0.00078 0.00250 -0.00387 AFIX 7 H5 2 0.419498 -0.148120 0.817168 11.00000 -1.50000 AFIX 0 O6 4 0.333675 0.655097 0.892941 11.00000 0.02861 0.01232 = 0.02647 -0.00144 0.00263 -0.00530 O7 4 0.540404 0.516179 0.716177 11.00000 0.02090 0.01063 = 0.01657 0.00162 0.00075 -0.00422 N1 3 0.433999 0.220530 0.816953 11.00000 0.01626 0.01287 = 0.01280 -0.00086 -0.00129 -0.00227 C1 1 0.839781 0.356039 0.462498 11.00000 0.02430 0.02059 = 0.02113 -0.00233 -0.00429 -0.00207 C2 1 0.748964 0.057217 0.556380 11.00000 0.01653 0.02252 = 0.02627 -0.00442 -0.00029 -0.00816 C3 1 0.866689 0.254577 0.723244 11.00000 0.02216 0.01672 = 0.02059 0.00279 0.00103 -0.00219 C4 1 0.376948 0.069397 0.862104 11.00000 0.01557 0.01427 = 0.01563 0.00208 -0.00154 -0.00368 C5 1 0.239421 0.048902 0.991236 11.00000 0.02202 0.01341 = 0.01713 0.00557 -0.00110 -0.00476 AFIX 43 H5A 2 0.203552 -0.059815 1.022384 11.00000 -1.20000 AFIX 0 C6 1 0.156900 0.187404 1.072414 11.00000 0.02831 0.01793 = 0.01263 0.00470 0.00418 -0.00654 AFIX 43 H6 2 0.064707 0.175721 1.160540 11.00000 -1.20000 AFIX 0 C7 1 0.212038 0.346285 1.022050 11.00000 0.02224 0.01791 = 0.01824 -0.00481 -0.00098 -0.00210 AFIX 43 H7 2 0.155852 0.444470 1.074512 11.00000 -1.20000 AFIX 0 C8 1 0.347062 0.357008 0.897057 11.00000 0.01736 0.01358 = 0.01559 -0.00037 -0.00391 -0.00342 C9 1 0.409363 0.523634 0.832887 11.00000 0.02042 0.01426 = 0.01604 0.00036 -0.00390 -0.00359 HKLF 4 REM joha1603_a.res in P-1 REM wR2 = 0.0589, GooF = S = 1.126, Restrained GooF = 1.126 for all data REM R1 = 0.0218 for 2116 Fo > 4sig(Fo) and 0.0226 for all 2165 data REM 166 parameters refined using 0 restraints END WGHT 0.0390 0.7537 REM Highest difference peak 1.542, deepest hole -1.160, 1-sigma level 0.171 Q1 1 0.5545 0.3395 0.6350 11.00000 0.05 1.54 Q2 1 0.7816 0.2152 0.6168 11.00000 0.05 1.20 Q3 1 0.5633 0.1839 0.5922 11.00000 0.05 0.93 Q4 1 0.4930 0.2357 0.7435 11.00000 0.05 0.80 Q5 1 0.7635 0.3641 0.6779 11.00000 0.05 0.75 Q6 1 0.7234 0.1352 0.6785 11.00000 0.05 0.74 Q7 1 0.4548 0.2974 0.7232 11.00000 0.05 0.72 Q8 1 0.5818 0.4216 0.5770 11.00000 0.05 0.72 Q9 1 0.8342 0.2992 0.5141 11.00000 0.05 0.68 Q10 1 0.6611 0.4007 0.5403 11.00000 0.05 0.65 Q11 1 0.3547 0.2149 0.7939 11.00000 0.05 0.65 Q12 1 0.1858 0.2494 1.0338 11.00000 0.05 0.65 Q13 1 0.2085 0.4266 0.5837 11.00000 0.05 0.60 Q14 1 0.2195 0.1194 1.0360 11.00000 0.05 0.59 Q15 1 0.6471 0.0799 0.5126 11.00000 0.05 0.56 Q16 1 0.7739 -0.0011 0.4760 11.00000 0.05 0.56 Q17 1 0.8136 -0.1460 0.4917 11.00000 0.05 0.55 Q18 1 0.8891 0.1418 0.6254 11.00000 0.05 0.54 Q19 1 0.9945 -0.1008 0.4441 11.00000 0.05 0.53 Q20 1 0.4036 0.2947 0.8557 11.00000 0.05 0.53 ; _shelx_res_checksum 83606 _shelx_hkl_file ; 0 0 -1 143001. 3959.90 13 0 0 -2 1924.12 311.247 13 0 0 -3 50442.4 1934.10 13 0 0 -4 152697. 4755.81 13 0 0 -4 143329. 4104.33 25 0 0 -5 61306.3 2693.27 13 0 0 -5 64125.5 2029.05 25 0 0 -6 5740.03 830.086 13 0 0 -6 5582.93 481.575 14 0 0 -6 5334.00 394.022 23 0 0 -6 4805.04 427.515 25 0 0 -6 5244.22 363.428 21 0 0 -6 6083.45 540.230 24 0 0 7 92118.1 4175.44 30 0 0 -7 86575.5 2945.30 14 0 0 -7 91596.8 4162.70 13 0 0 -7 91680.2 3096.08 24 0 0 -7 84123.0 2875.90 25 0 0 -7 86528.4 2777.38 22 0 0 -7 91042.4 2754.94 21 0 0 -7 88822.6 2798.79 23 0 0 -8 119544. 3666.84 21 0 0 -8 118912. 4023.39 24 0 0 -8 118353. 3808.69 25 0 0 -8 121001. 3731.14 23 0 0 -8 120716. 3657.85 22 0 0 -8 126607. 3953.88 14 0 0 8 121090. 5317.22 6 0 0 -9 21785.3 967.700 21 0 0 -9 19647.3 1014.63 23 0 0 -9 21256.3 1213.85 24 0 0 -9 23967.1 1198.75 14 0 0 -10 1866.39 289.312 23 0 0 -10 2078.31 425.611 24 0 0 -10 1512.45 322.919 14 0 0 -11 49400.4 1601.62 23 0 0 -11 53504.7 1788.88 24 0 1 -11 36725.0 1282.15 24 0 1 -11 31164.4 1151.20 14 0 1 -10 62966.7 2069.70 23 0 1 -10 62805.3 2271.12 24 0 1 -10 64457.4 2249.28 14 0 1 -9 26875.5 1373.66 24 0 1 -9 28024.0 1183.07 23 0 1 -9 28282.2 1253.10 10 0 -1 9 29912.3 2359.80 6 0 1 -9 27824.8 1368.51 14 0 1 -8 127.554 307.981 24 0 1 -8 276.127 193.397 23 0 1 -8 276.933 244.998 10 0 -1 8 547.197 428.218 6 0 1 -8 337.296 304.863 14 0 1 -7 54003.3 1957.51 10 0 -1 7 57187.7 2929.07 30 0 1 -7 53319.3 2037.79 14 0 1 -7 54470.0 3060.84 13 0 1 -7 53340.7 1826.09 23 0 1 -7 53514.8 2080.95 24 0 1 -7 51096.2 1809.23 21 0 1 -7 54914.3 1881.26 22 0 1 -6 130498. 4003.65 10 0 1 -6 134139. 4118.95 24 0 1 -6 128029. 3976.05 25 0 1 -6 139593. 3987.10 22 0 1 -6 135699. 3884.57 23 0 1 -6 134486. 5155.10 13 0 1 -6 133177. 4082.70 14 0 -1 6 141081. 5112.60 30 0 1 -5 120366. 3532.72 25 0 1 -5 121067. 4466.20 13 0 -1 5 119200. 4459.02 30 0 1 -4 58085.1 1814.66 25 0 1 -4 59040.0 2471.15 13 0 -1 4 60165.2 2583.30 30 0 1 -3 137758. 3755.97 28 0 -1 3 135089. 3794.64 18 0 1 -3 140909. 4427.44 13 0 1 -2 402810. 10426.1 1 0 -1 2 364929. 10077.2 18 0 1 -2 375993. 10069.6 28 0 -1 2 375182. 10090.7 26 0 1 -2 381123. 10194.3 33 0 -1 2 378864. 10534.4 30 0 -1 1 169039. 4768.42 18 0 1 -1 178154. 4896.80 31 0 1 -1 177796. 4735.87 33 0 -1 1 172862. 4887.87 30 0 -1 1 169944. 4764.87 26 0 1 0 14831.4 569.554 5 0 -1 0 15458.8 613.227 26 0 1 1 310904. 8121.83 31 0 -1 -1 310214. 8112.00 18 0 1 1 282179. 8037.31 5 0 -1 -1 306151. 8098.52 26 0 -1 -2 228545. 6287.12 26 0 1 2 234082. 6280.29 28 0 -1 -2 230084. 6279.46 18 0 1 3 6606.66 311.348 28 0 -1 -3 6921.37 574.549 13 0 -1 -3 7116.85 327.322 18 0 -1 -4 12996.1 933.075 13 0 -1 -4 13766.1 605.151 25 0 -1 -5 88447.1 3533.73 13 0 -1 -5 92779.1 2781.85 25 0 -1 -6 137521. 4028.52 25 0 -1 -6 130519. 3995.15 22 0 -1 -6 135322. 3974.62 23 0 -1 -6 133770. 3888.05 21 0 -1 -6 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-7 -6 -5 46626.6 1438.14 11 7 6 5 44008.6 1377.54 3 -7 -6 -5 44818.3 1345.12 15 -7 -6 -6 53044.5 1542.49 9 -7 -6 -6 52774.5 1580.56 11 -7 -7 -2 10273.0 383.031 11 -7 -7 -3 32963.2 1011.89 11 -7 -7 -3 32653.2 998.468 15 8 -3 0 31454.5 1002.62 3 8 -3 0 34115.2 1016.85 2 8 -3 1 17198.8 661.025 3 8 -3 1 17567.7 638.579 2 8 -3 2 7375.84 397.262 3 -8 3 -3 14612.7 568.559 29 8 -3 3 13526.6 550.555 2 8 -3 4 35393.7 1154.95 3 8 -3 4 36109.8 1113.18 2 8 -3 5 9237.34 368.879 3 8 -2 -1 23519.8 772.958 12 8 -2 -1 21179.2 741.509 19 8 -2 -1 22313.1 719.317 2 8 -2 0 81.5879 81.6486 12 8 -2 0 109.187 87.1822 19 8 -2 0 213.658 103.076 2 8 -2 0 36.0057 105.146 3 8 -2 0 58.3427 144.997 25 8 -2 1 7794.50 538.959 25 -8 2 -1 9107.99 437.403 29 8 -2 1 8555.87 466.160 3 8 -2 1 8506.58 430.352 2 8 -2 1 8466.18 393.895 19 8 -2 2 58115.7 1910.41 25 8 -2 2 54147.1 1772.88 3 8 -2 2 53772.6 1719.76 2 -8 2 -3 25688.5 942.081 29 -8 2 -4 152.879 100.848 29 8 -2 4 111.449 118.947 2 8 -2 4 11.8267 136.716 3 8 -2 5 17831.9 651.326 2 8 -2 5 17027.8 666.929 3 -8 2 -5 16531.6 624.847 11 8 -2 6 22721.6 732.024 2 -8 2 -6 25709.1 815.919 11 8 -1 -2 109.293 74.9733 19 8 -1 -2 89.4254 86.8772 12 8 -1 -1 11799.3 616.075 25 8 -1 -1 11739.3 638.686 17 8 -1 -1 11220.7 523.986 19 8 -1 0 55244.2 1816.37 25 8 -1 0 48743.9 1619.20 3 8 -1 0 50431.0 1578.99 2 8 -1 0 52617.7 1847.00 17 8 -1 1 30405.7 1249.01 25 -8 1 -1 29832.1 1060.41 29 8 -1 1 28735.7 1051.66 2 8 -1 1 29403.9 1101.84 3 8 -1 2 21.4253 239.766 17 8 -1 2 132.364 163.672 3 8 -1 2-12.7309 147.911 2 8 -1 2 151.334 211.839 25 8 -1 3 32327.6 1195.04 2 -8 1 -3 35288.7 1210.63 29 -8 1 -4 46084.6 1490.65 11 8 -1 4 46722.9 1583.01 3 -8 1 -4 48110.2 1537.99 29 8 -1 5 6739.63 405.185 2 8 -1 5 7085.09 418.739 3 -8 1 -5 7345.14 422.362 11 8 -1 6 1672.83 178.875 2 8 -1 6 1727.76 164.986 3 -8 1 -6 1666.54 201.044 11 -8 1 -7 19756.5 725.849 11 8 0 -2 46117.0 1576.93 17 8 0 -2 48609.7 1494.89 19 8 0 -1 10555.9 598.474 25 8 0 -1 9584.90 621.268 17 8 0 0 3719.20 313.812 3 8 0 0 4101.78 279.573 2 8 0 0 3488.95 436.932 17 8 0 1 42003.8 1395.81 2 8 0 1 40965.2 1449.64 3 8 0 2 61562.8 1945.02 2 8 0 2 60994.2 1998.00 3 8 0 2 58678.4 2179.94 17 8 0 3 12282.8 628.951 2 8 0 3 12869.2 772.114 17 -8 0 -3 12280.5 613.004 29 8 0 4 2338.10 270.587 2 8 0 4 2003.40 281.654 3 -8 0 -4 2348.00 254.075 11 8 0 5 30868.4 1167.69 2 8 0 5 33494.2 1180.86 3 -8 0 -5 34875.3 1216.88 11 8 0 6 22535.6 850.092 2 8 0 6 21765.5 795.480 3 -8 0 -6 22829.0 896.959 11 -8 0 -7 228.295 75.7358 9 8 0 7 258.899 97.9874 2 -8 0 -7 282.815 127.374 11 8 1 -2 5029.78 411.565 16 8 1 -2 5536.85 399.945 17 8 1 -1 43347.7 1504.75 25 8 1 -1 40326.2 1538.42 17 8 1 0 28380.4 1046.22 3 8 1 0 29942.2 1206.95 25 8 1 0 29694.2 1239.74 17 8 1 1 7200.80 425.188 2 8 1 1 7771.99 486.480 3 8 1 1 7482.04 581.925 25 8 1 1 7567.37 588.540 16 8 1 1 8507.65 626.440 17 8 1 2 11830.2 583.458 2 8 1 2 10795.5 610.838 3 8 1 2 11145.1 725.247 17 8 1 2 10701.3 722.262 25 8 1 3 32417.3 1337.58 17 8 1 3 33003.2 1194.88 2 -8 -1 -3 31428.6 1132.62 11 8 1 4 44991.7 1491.35 2 8 1 4 44168.7 1512.91 3 -8 -1 -4 44901.3 1488.30 11 8 1 5 2268.23 268.794 3 -8 -1 -5 2327.67 273.036 11 8 1 6 10880.7 528.495 2 8 1 6 9930.92 468.177 3 -8 -1 -6 10619.5 551.567 11 8 1 7 29465.8 1016.40 2 -8 -1 -7 31580.5 1086.54 11 -8 -1 -7 31168.6 974.399 9 8 2 -2 28624.3 1053.43 17 8 2 -1 1524.87 263.884 17 8 2 -1 1827.57 298.855 16 8 2 0 8113.21 455.064 3 -8 -2 0 9509.47 491.096 27 8 2 0 7913.79 542.464 25 8 2 0 8645.78 580.291 16 8 2 1 39264.0 1321.74 3 -8 -2 -1 41490.0 1357.34 27 8 2 1 38787.4 1423.91 25 8 2 1 38111.1 1456.06 16 8 2 1 41058.0 1480.12 17 8 2 2 52756.7 1684.74 2 8 2 2 54340.4 1760.32 3 8 2 2 56445.4 1891.64 17 8 2 2 54962.7 1884.10 25 -8 -2 -3 3029.38 275.226 11 8 2 3 3485.83 315.473 2 8 2 3 3621.12 416.431 17 -8 -2 -3 3579.38 333.647 27 8 2 3 3097.23 382.108 25 -8 -2 -4 23137.3 916.787 27 8 2 4 21171.6 895.843 2 8 2 4 20752.2 898.282 3 -8 -2 -4 24441.5 921.958 11 -8 -2 -5 47113.8 1591.63 27 8 2 5 49452.4 1615.26 2 8 2 5 48717.9 1595.80 3 -8 -2 -5 50674.6 1641.83 11 8 2 6 23075.9 811.595 3 -8 -2 -6 23355.9 905.228 11 -8 -2 -6 22788.2 788.288 9 8 2 7 803.827 137.991 2 -8 -2 -7 787.094 113.088 9 8 3 -2 22936.5 880.549 16 8 3 -2 23677.7 869.231 17 8 3 -1 40359.4 1412.87 16 8 3 -1 41113.0 1424.52 17 8 3 0 34533.9 1275.95 16 8 3 0 32319.9 1125.04 3 -8 -3 0 34971.5 1185.21 27 -8 -3 -1 72.6685 107.558 15 8 3 1 118.701 186.932 16 -8 -3 -1 420.468 167.000 27 8 3 1 117.858 216.706 17 8 3 1 261.799 147.298 3 8 3 2 24952.4 1034.48 17 8 3 2 23535.5 874.787 2 8 3 2 24647.4 960.203 3 -8 -3 -3 75105.9 2192.20 15 -8 -3 -3 73348.4 2163.86 11 -8 -3 -3 70393.3 2248.34 27 8 3 3 66400.2 2261.43 17 8 3 3 69886.9 2163.98 2 -8 -3 -4 34781.0 1216.27 11 -8 -3 -4 34787.5 1241.76 27 -8 -3 -4 34697.6 1183.11 15 8 3 4 34184.3 1209.67 2 8 3 4 36029.9 1238.91 3 8 3 5 73.7655 127.985 3 8 3 5-33.8093 132.276 2 -8 -3 -5 133.542 131.255 11 -8 -3 -5 32.1113 119.787 27 8 3 6 24797.5 825.616 3 -8 -3 -6 26354.1 937.074 11 -8 -3 -6 24977.7 820.556 9 -8 -3 -7 13933.2 488.694 9 8 4 -1-26.4943 123.703 16 8 4 0 20905.9 833.018 16 8 4 0 22594.5 774.966 3 -8 -4 -1 60861.6 1842.86 15 -8 -4 -1 60895.1 1933.41 27 8 4 1 65956.6 2009.63 17 8 4 1 60726.0 1877.18 3 8 4 2 4974.46 374.218 17 8 4 2 4627.10 336.475 3 -8 -4 -3 97.0150 99.8799 11 -8 -4 -3 121.732 131.677 27 -8 -4 -3 326.640 111.695 15 8 4 3 133.842 97.7777 2 -8 -4 -4 33064.8 1093.68 11 -8 -4 -4 30040.9 1114.54 27 -8 -4 -4 31892.2 1056.34 15 8 4 4 31842.1 1066.94 2 8 4 4 32126.0 1104.15 3 8 4 5 44295.3 1404.13 2 8 4 5 44718.4 1386.36 3 -8 -4 -5 45430.6 1430.01 11 8 4 6 4077.04 267.640 2 -8 -5 -1 3399.91 199.362 15 8 5 1 3361.27 248.286 17 8 5 1 3067.36 211.650 3 8 5 2 26828.4 918.072 3 -8 -5 -3 40628.7 1237.04 11 -8 -5 -3 43017.8 1280.81 15 -8 -5 -4 9107.90 390.733 11 8 5 4 8712.97 399.739 3 -8 -5 -4 8912.36 371.139 15 -8 -5 -5 3355.84 204.367 11 8 5 5 1784.77 142.078 2 9 0 3 10732.2 409.429 2 9 0 3 10204.8 433.115 3 9 1 2 29381.0 923.780 3 9 1 2 28007.4 849.665 2 9 1 3 11651.0 441.550 2 9 1 3 12056.4 485.894 3 9 1 4 139.609 87.0881 3 9 1 4 195.546 78.0725 2 0 0 0 0.00 0.00 0 TITL joha1603 in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 7.239716 8.004352 9.536214 88.0480 76.3532 84.4654 ZERR 2.00 0.000345 0.000365 0.000210 0.0030 0.0032 0.0038 LATT 1 SFAC C H N O Re UNIT 18.00 12.00 2.00 14.00 2.00 TREF HKLF 4 END ; _shelx_hkl_checksum 3426 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.66101(2) 0.27546(2) 0.62822(2) 0.01436(10) Uani 1 1 d . . . . . O1 O 0.9486(5) 0.3997(4) 0.3645(4) 0.0314(7) Uani 1 1 d . . . . . O2 O 0.8089(5) -0.0730(4) 0.5107(4) 0.0336(8) Uani 1 1 d . . . . . O3 O 0.9924(4) 0.2403(4) 0.7765(3) 0.0286(7) Uani 1 1 d . . . . . O4 O 0.4157(4) 0.3164(4) 0.5314(3) 0.0212(6) Uani 1 1 d . . . . . H4A H 0.358994 0.224916 0.537741 0.032 Uiso 1 1 d R U . . . H4B H 0.425241 0.346340 0.441454 0.032 Uiso 1 1 d R U . . . O5 O 0.4573(4) -0.0583(3) 0.7775(3) 0.0235(6) Uani 1 1 d . . . . . H5 H 0.419498 -0.148120 0.817168 0.035 Uiso 1 1 d R U . . . O6 O 0.3337(4) 0.6551(3) 0.8929(3) 0.0237(6) Uani 1 1 d . . . . . O7 O 0.5404(4) 0.5162(3) 0.7162(3) 0.0167(5) Uani 1 1 d . . . . . N1 N 0.4340(5) 0.2205(4) 0.8170(4) 0.0142(6) Uani 1 1 d . . . . . C1 C 0.8398(6) 0.3560(5) 0.4625(5) 0.0221(8) Uani 1 1 d . . . . . C2 C 0.7490(6) 0.0572(6) 0.5564(5) 0.0220(8) Uani 1 1 d . . . . . C3 C 0.8667(6) 0.2546(5) 0.7232(5) 0.0209(8) Uani 1 1 d . . . . . C4 C 0.3769(5) 0.0694(5) 0.8621(4) 0.0154(7) Uani 1 1 d . . . . . C5 C 0.2394(6) 0.0489(5) 0.9912(4) 0.0180(7) Uani 1 1 d . . . . . H5A H 0.203552 -0.059815 1.022384 0.022 Uiso 1 1 calc R U . . . C6 C 0.1569(6) 0.1874(5) 1.0724(4) 0.0209(8) Uani 1 1 d . . . . . H6 H 0.064707 0.175721 1.160540 0.025 Uiso 1 1 calc R U . . . C7 C 0.2120(6) 0.3463(5) 1.0220(4) 0.0200(8) Uani 1 1 d . . . . . H7 H 0.155852 0.444470 1.074512 0.024 Uiso 1 1 calc R U . . . C8 C 0.3471(5) 0.3570(5) 0.8971(4) 0.0154(7) Uani 1 1 d . . . . . C9 C 0.4094(6) 0.5236(5) 0.8329(4) 0.0168(7) 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 Re1 0.01610(13) 0.01294(13) 0.01301(13) -0.00027(7) -0.00032(7) -0.00388(7) O1 0.0360(18) 0.0302(17) 0.0224(16) -0.0001(13) 0.0079(14) -0.0119(14) O2 0.0239(15) 0.0231(16) 0.050(2) -0.0174(15) 0.0027(14) -0.0033(12) O3 0.0246(16) 0.0371(18) 0.0267(16) 0.0037(13) -0.0101(13) -0.0062(13) O4 0.0246(15) 0.0215(15) 0.0198(14) 0.0031(11) -0.0085(12) -0.0068(12) O5 0.0310(15) 0.0119(13) 0.0235(15) -0.0008(11) 0.0025(12) -0.0039(11) O6 0.0286(15) 0.0123(14) 0.0265(15) -0.0014(11) 0.0026(12) -0.0053(11) O7 0.0209(14) 0.0106(12) 0.0166(13) 0.0016(10) 0.0008(11) -0.0042(10) N1 0.0163(15) 0.0129(15) 0.0128(15) -0.0009(11) -0.0013(12) -0.0023(12) C1 0.024(2) 0.021(2) 0.021(2) -0.0023(16) -0.0043(17) -0.0021(16) C2 0.0165(18) 0.023(2) 0.026(2) -0.0044(16) -0.0003(16) -0.0082(15) C3 0.022(2) 0.0167(19) 0.021(2) 0.0028(15) 0.0010(16) -0.0022(15) C4 0.0156(17) 0.0143(18) 0.0156(18) 0.0021(14) -0.0015(14) -0.0037(14) C5 0.0220(18) 0.0134(17) 0.0171(18) 0.0056(14) -0.0011(15) -0.0048(14) C6 0.028(2) 0.0179(19) 0.0126(18) 0.0047(14) 0.0042(15) -0.0065(16) C7 0.0222(19) 0.0179(19) 0.0182(19) -0.0048(15) -0.0010(15) -0.0021(15) C8 0.0174(18) 0.0136(18) 0.0156(18) -0.0004(14) -0.0039(14) -0.0034(14) C9 0.0204(18) 0.0143(18) 0.0160(18) 0.0004(14) -0.0039(14) -0.0036(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Re Re -5.2083 5.8923 '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 0 1 0.0090 -1 0 -1 0.0090 2 -1 -5 0.0404 -2 1 5 0.0404 0 0 -1 0.0214 0 0 1 0.0214 -1 -4 3 0.0889 1 4 -3 0.0969 -1 -5 -2 0.1081 1 5 2 0.1151 1 0 0 0.0125 -1 0 0 0.0125 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 O4 Re1 N1 80.70(12) . . ? O7 Re1 O4 79.71(11) . . ? O7 Re1 N1 74.79(11) . . ? C1 Re1 O4 94.85(15) . . ? C1 Re1 O7 97.36(14) . . ? C1 Re1 N1 171.50(15) . . ? C2 Re1 O4 97.73(16) . . ? C2 Re1 O7 175.66(13) . . ? C2 Re1 N1 101.40(16) . . ? C2 Re1 C1 86.33(18) . . ? C2 Re1 C3 86.77(18) . . ? C3 Re1 O4 175.30(13) . . ? C3 Re1 O7 95.72(15) . . ? C3 Re1 N1 97.15(15) . . ? C3 Re1 C1 86.74(18) . . ? Re1 O4 H4A 109.6 . . ? Re1 O4 H4B 123.0 . . ? H4A O4 H4B 102.6 . . ? C4 O5 H5 109.3 . . ? C9 O7 Re1 119.5(2) . . ? C4 N1 Re1 127.0(3) . . ? C4 N1 C8 117.9(3) . . ? C8 N1 Re1 115.1(3) . . ? O1 C1 Re1 178.1(4) . . ? O2 C2 Re1 177.4(4) . . ? O3 C3 Re1 178.1(4) . . ? O5 C4 N1 116.0(3) . . ? O5 C4 C5 122.4(4) . . ? N1 C4 C5 121.7(4) . . ? C4 C5 H5A 120.2 . . ? C6 C5 C4 119.6(4) . . ? C6 C5 H5A 120.2 . . ? C5 C6 H6 120.7 . . ? C5 C6 C7 118.6(4) . . ? C7 C6 H6 120.7 . . ? C6 C7 H7 120.6 . . ? C8 C7 C6 118.8(4) . . ? C8 C7 H7 120.6 . . ? N1 C8 C9 114.5(3) . . ? C7 C8 N1 123.4(4) . . ? C7 C8 C9 122.1(3) . . ? O6 C9 O7 124.4(4) . . ? O6 C9 C8 119.8(3) . . ? O7 C9 C8 115.9(3) . . ? 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 Re1 O4 2.181(3) . ? Re1 O7 2.149(3) . ? Re1 N1 2.196(3) . ? Re1 C1 1.927(4) . ? Re1 C2 1.894(4) . ? Re1 C3 1.909(4) . ? O1 C1 1.140(6) . ? O2 C2 1.148(6) . ? O3 C3 1.137(6) . ? O4 H4A 0.8669 . ? O4 H4B 0.8710 . ? O5 H5 0.8400 . ? O5 C4 1.325(5) . ? O6 C9 1.232(5) . ? O7 C9 1.280(5) . ? N1 C4 1.340(5) . ? N1 C8 1.368(5) . ? C4 C5 1.405(5) . ? C5 H5A 0.9500 . ? C5 C6 1.378(6) . ? C6 H6 0.9500 . ? C6 C7 1.405(6) . ? C7 H7 0.9500 . ? C7 C8 1.358(6) . ? C8 C9 1.512(5) . ? 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 O4 H4A O2 0.87 1.94 2.752(4) 155.7 2_656 yes O4 H4B O7 0.87 1.82 2.642(4) 157.8 2_666 yes O5 H5 O6 0.84 1.81 2.652(4) 176.5 1_545 yes C5 H5A O6 0.95 2.62 3.281(5) 127.3 1_545 yes C6 H6 O1 0.95 2.62 3.281(5) 126.8 1_456 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Re1 O7 C9 O6 178.8(3) . . . . ? Re1 O7 C9 C8 -1.6(4) . . . . ? Re1 N1 C4 O5 -5.3(5) . . . . ? Re1 N1 C4 C5 175.0(3) . . . . ? Re1 N1 C8 C7 -175.9(3) . . . . ? Re1 N1 C8 C9 5.8(4) . . . . ? O5 C4 C5 C6 -178.0(4) . . . . ? N1 C4 C5 C6 1.6(6) . . . . ? N1 C8 C9 O6 176.7(4) . . . . ? N1 C8 C9 O7 -3.0(5) . . . . ? C4 N1 C8 C7 2.6(6) . . . . ? C4 N1 C8 C9 -175.7(3) . . . . ? C4 C5 C6 C7 0.7(6) . . . . ? C5 C6 C7 C8 -1.3(6) . . . . ? C6 C7 C8 N1 -0.3(6) . . . . ? C6 C7 C8 C9 177.8(4) . . . . ? C7 C8 C9 O6 -1.6(6) . . . . ? C7 C8 C9 O7 178.7(4) . . . . ? C8 N1 C4 O5 176.5(3) . . . . ? C8 N1 C4 C5 -3.2(6) . . . . ?