#------------------------------------------------------------------------------ #$Date: 2023-09-22 00:56:58 +0300 (Fri, 22 Sep 2023) $ #$Revision: 286448 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/13/21/7132145.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_7132145 loop_ _publ_author_name 'Xu, Yijue' 'Calabrese, Miriam' 'Demitri, Nicola' 'Pizzi, Andrea' 'Nag, Tamali' 'Hung, Ivan' 'Gan, Zhehong' 'Resnati, Giuseppe' 'Bryce, David L.' _publ_section_title ; Non-Covalent Matere Bonds in Perrhenates Probed via Ultrahigh Field Rhenium-185/187 NMR and Zero-Field NQR Spectroscopy ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/D3CC04090A _journal_year 2023 _chemical_formula_moiety 'C7 H16 N O2, Re O4' _chemical_formula_sum 'C7 H16 N O6 Re' _chemical_formula_weight 396.41 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2023-08-18 deposited with the CCDC. 2023-09-21 downloaded from the CCDC. ; _cell_angle_alpha 79.13(3) _cell_angle_beta 71.47(3) _cell_angle_gamma 67.85(3) _cell_formula_units_Z 2 _cell_length_a 7.313(2) _cell_length_b 8.956(2) _cell_length_c 10.153(2) _cell_measurement_reflns_used 1514 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.812 _cell_measurement_theta_min 2.161 _cell_volume 582.2(3) _computing_cell_refinement 'XDS (Kabsch, 2010)' _computing_data_collection 'Elettra XRD2 Data Collection SW' _computing_data_reduction 'XDS (Kabsch, 2010)' _computing_molecular_graphics 'Ortep3 for Windows - Coot' _computing_publication_material 'enCIFer - publCIF' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.960 _diffrn_measured_fraction_theta_max 0.960 _diffrn_measurement_device_type ; 'Arinax MD2s Goniometer, Pilatus 6M detector' ; _diffrn_measurement_method 'Rotating crystal' _diffrn_radiation_type Synchrotron _diffrn_radiation_wavelength 0.620 _diffrn_reflns_av_R_equivalents 0.1587 _diffrn_reflns_av_unetI/netI 0.2208 _diffrn_reflns_Laue_measured_fraction_full 0.960 _diffrn_reflns_Laue_measured_fraction_max 0.960 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 4770 _diffrn_reflns_point_group_measured_fraction_full 0.960 _diffrn_reflns_point_group_measured_fraction_max 0.960 _diffrn_reflns_theta_full 21.000 _diffrn_reflns_theta_max 21.000 _diffrn_reflns_theta_min 2.724 _diffrn_source 'Elettra Synchrotron - XRD2 BL' _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 7.282 _exptl_absorpt_correction_type none _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 2.261 _exptl_crystal_description 'Thin needles' _exptl_crystal_F_000 376 _exptl_crystal_size_max 0.050 _exptl_crystal_size_mid 0.020 _exptl_crystal_size_min 0.020 _refine_diff_density_max 6.573 _refine_diff_density_min -4.117 _refine_diff_density_rms 0.636 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 137 _refine_ls_number_reflns 1814 _refine_ls_number_restraints 107 _refine_ls_restrained_S_all 1.223 _refine_ls_R_factor_all 0.1151 _refine_ls_R_factor_gt 0.1033 _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^)+(0.0799P)^2^+11.2667P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1802 _refine_ls_wR_factor_ref 0.1859 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1534 _reflns_number_total 1814 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3cc04090a2.cif _cod_data_source_block 5 _cod_database_code 7132145 _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_min 0.712 _shelx_estimated_absorpt_t_max 0.868 _shelx_res_file ; TITL X4ESxT-28Feb152301_a.res in P-1 XDS_ASCII_scaled1b_unmerged_tw.res created by SHELXL-2019/3 at 13:40:48 on 18-Aug-2023 REM Old TITL X4ESxT-28Feb152301 in P1 REM SHELXT solution in P-1: R1 0.108, Rweak 0.014, Alpha 0.122 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C10 N2 O S I CELL 0.62000 7.31340 8.95560 10.15310 79.1316 71.4703 67.8486 ZERR 2.00 0.00146 0.00179 0.00203 0.0300 0.0300 0.0300 LATT 1 SFAC C N O Re H DISP H 0.00000 0.00000 0.66 DISP C 0.00201 0.00119 8.75 DISP N 0.00416 0.00245 14.28 DISP O 0.00771 0.00451 22.87 DISP RE -0.50077 5.80803 20973.66 UNIT 14 2 12 2 32 L.S. 10 LIST 4 BOND $H CONF MERG 2 FMAP 2 REM PLAN 25 SHEL 180 0.865 ACTA WPDB -2 TEMP -173.15 SIZE 0.05 0.02 0.02 PLAN 20 REM hfix_ACH 23 c2 c3 REM hfix_ACH 33 c6 c8 c9 c10 SIMU_* 0.01 REM ISOR_* 0.01 SADI_2 0.01 re o12 re o13 re o14 re o15 SADI_2 0.01 o12 o13 o12 o14 o12 o15 o13 o14 o13 o15 o14 o15 DFIX_REO 2.00 0.01 re o12 DANG_REO 2.85 0.01 O12 o13 SADI_1 0.01 n1 c8 n1 c9 n1 c10 SADI_1 0.01 c8 c9 c9 c10 c10 c8 WGHT 0.079900 11.266700 BASF 0.00843 FVAR 9.98703 RESI 2 REO RE 4 0.166255 0.791673 0.330606 11.00000 0.01032 0.01116 = 0.01686 -0.00568 0.00253 0.00013 O12 3 0.277237 0.584414 0.283290 11.00000 0.03272 0.03089 = 0.05875 -0.01355 0.00860 -0.00555 O13 3 0.131867 0.918678 0.178501 11.00000 0.03641 0.03940 = 0.03138 0.01568 -0.01530 -0.01055 O14 3 -0.071582 0.815895 0.455974 11.00000 0.04042 0.04663 = 0.06174 -0.02037 0.00681 -0.01502 O15 3 0.335407 0.831726 0.398104 11.00000 0.03617 0.04964 = 0.04405 -0.02105 -0.01407 -0.00237 REM AFIX 6 RESI 1 ACH O7 3 0.737939 0.604738 0.109333 11.00000 0.04918 0.03249 = 0.04996 -0.00314 -0.00693 -0.01693 C5 1 0.782573 0.510164 0.208694 11.00000 0.02012 0.02464 = 0.04131 -0.00328 -0.00676 -0.00848 C6 1 0.781167 0.551776 0.346762 11.00000 0.03096 0.01285 = 0.05228 -0.00001 -0.01614 -0.00918 AFIX 33 H6A 5 0.823633 0.452086 0.405815 11.00000 -1.50000 H6B 5 0.876484 0.610463 0.330680 11.00000 -1.50000 H6C 5 0.642473 0.619734 0.393225 11.00000 -1.50000 AFIX 0 O4 3 0.835319 0.347879 0.207927 11.00000 0.01727 0.01961 = 0.03943 -0.00025 -0.00494 -0.01514 C3 1 0.827958 0.292431 0.084703 11.00000 0.01902 0.01608 = 0.02966 -0.00010 -0.00083 -0.00998 AFIX 23 H3A 5 0.921248 0.179141 0.073435 11.00000 -1.20000 H3B 5 0.874553 0.359905 0.001075 11.00000 -1.20000 AFIX 0 C2 1 0.606434 0.303360 0.098417 11.00000 0.02046 0.00802 = 0.02121 0.00085 -0.00431 -0.00448 AFIX 23 H2A 5 0.512476 0.411550 0.128448 11.00000 -1.20000 H2B 5 0.597093 0.295885 0.004861 11.00000 -1.20000 AFIX 0 N1 2 0.529309 0.176752 0.198552 11.00000 0.01552 0.00864 = 0.01734 -0.00227 -0.00848 -0.00044 C10 1 0.311108 0.229419 0.195130 11.00000 0.02197 0.01311 = 0.03196 0.00096 -0.00957 0.00034 AFIX 33 H10A 5 0.306369 0.229839 0.099674 11.00000 -1.50000 H10B 5 0.246144 0.154422 0.256594 11.00000 -1.50000 H10C 5 0.237669 0.338545 0.226878 11.00000 -1.50000 AFIX 0 C9 1 0.538012 0.175752 0.343719 11.00000 0.02744 0.01457 = 0.01337 0.00640 -0.00077 -0.01590 AFIX 33 H9A 5 0.681446 0.141127 0.345314 11.00000 -1.50000 H9B 5 0.464913 0.284798 0.375689 11.00000 -1.50000 H9C 5 0.473388 0.100674 0.405405 11.00000 -1.50000 AFIX 0 C8 1 0.643571 0.011126 0.148327 11.00000 0.02162 0.01341 = 0.03157 -0.00371 -0.00123 -0.00384 AFIX 33 H8A 5 0.637513 0.012276 0.053079 11.00000 -1.50000 H8B 5 0.787014 -0.021977 0.149461 11.00000 -1.50000 H8C 5 0.581036 -0.065416 0.209539 11.00000 -1.50000 AFIX 0 HKLF 5 REM X4ESxT-28Feb152301_a.res in P-1 REM wR2 = 0.1859, GooF = S = 1.117, Restrained GooF = 1.223 for all data REM R1 = 0.1033 for 1534 Fo > 4sig(Fo) and 0.1151 for all 1814 data REM 137 parameters refined using 107 restraints END WGHT 0.0764 10.7378 REM Highest difference peak 6.573, deepest hole -4.117, 1-sigma level 0.636 Q1 1 0.1515 0.8548 0.3884 11.00000 0.05 6.57 Q2 1 0.2541 0.6440 0.2715 11.00000 0.05 4.53 Q3 1 0.1070 0.7728 0.3052 11.00000 0.05 4.50 Q4 1 0.0966 0.9815 0.4876 11.00000 0.05 2.28 Q5 1 0.1893 0.6408 0.1651 11.00000 0.05 2.10 Q6 1 -0.0449 0.8486 0.3954 11.00000 0.05 1.75 Q7 1 -0.0045 0.8847 0.4875 11.00000 0.05 1.74 Q8 1 0.2744 0.8922 0.1598 11.00000 0.05 1.62 Q9 1 0.7567 0.6987 0.4162 11.00000 0.05 1.61 Q10 1 0.4133 0.8086 0.2931 11.00000 0.05 1.60 Q11 1 0.2227 1.0499 0.1181 11.00000 0.05 1.54 Q12 1 0.3250 0.4844 0.1363 11.00000 0.05 1.52 Q13 1 -0.0702 0.7821 0.3652 11.00000 0.05 1.49 Q14 1 0.2788 0.9252 0.3838 11.00000 0.05 1.47 Q15 1 0.0925 0.8364 0.1040 11.00000 0.05 1.42 Q16 1 0.4273 0.4604 0.0194 11.00000 0.05 1.42 Q17 1 0.5376 0.2188 -0.1277 11.00000 0.05 1.33 Q18 1 0.9289 0.6419 0.4427 11.00000 0.05 1.32 Q19 1 0.4468 0.2626 -0.0103 11.00000 0.05 1.32 Q20 1 0.3560 0.4682 0.0445 11.00000 0.05 1.30 ; _shelx_res_checksum 64830 _shelx_hkl_file ; 1 0 0 335255 47194 1 2 0 0 1230484 173078 1 3 0 0 1714731 239981 1 4 0 0 262912 37015 1 5 0 0 142006 20711 1 6 0 0 600726 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8 364847 98746 1 -1 -6 8 259703 880128 1 0 -6 8 128357 110953 1 1 7 -7 233754 96136 -2 1 -6 8 233754 96136 1 2 8 -6 3542 61014 -2 2 -6 8 3542 61014 1 3 9 -5 87213 649300 -2 3 -6 8 87213 649300 1 -4 -5 8 351294 201701 1 -2 -5 8 189411 99925 1 0 -5 8 8529 86078 1 1 -5 8 89110 145972 1 2 -5 8 217238 156832 1 3 8 -5 37128 61201 -2 3 -5 8 37128 61201 1 4 9 -4 70950 31448 -2 4 -5 8 70950 31448 1 -4 -4 8 35441 8839 1 -3 -4 8 334289 100766 1 -2 -4 8 192441 85108 1 0 -4 8 510988 120718 1 1 -4 8 158447 69829 1 2 -4 8 186296 639450 1 3 -4 8 305651 100093 1 4 -4 8 26393 48385 1 5 -4 8 31606 10349 1 -4 -3 8 129068 85361 1 -3 -3 8 20301 5050 1 -2 -3 8 461488 125600 1 1 -3 8 392459 94369 1 2 -3 8 317705 77532 1 3 -3 8 -10165 46386 1 4 -3 8 75725 98465 1 5 -3 8 200281 65104 1 6 -3 8 10452 4714 1 -4 -2 8 219217 77280 1 -3 -2 8 353387 72291 1 -2 -2 8 1064 28201 1 0 -2 8 786264 189916 1 1 -2 8 28285 86035 1 2 -2 8 243877 63642 1 3 -2 8 204058 52193 1 4 -2 8 16752 39061 1 5 -2 8 161886 27528 1 6 -2 8 173753 37545 1 -4 -1 8 56741 136334 1 -3 -1 8 113967 23559 1 -2 -1 8 491558 233480 1 -1 -1 8 74417 15658 1 0 -1 8 60022 160368 1 1 -1 8 1302640 295060 1 2 -1 8 64989 107333 1 3 -1 8 123479 15995 1 4 -1 8 487969 58549 1 5 -1 8 29097 9008 1 6 -1 8 80899 3115 1 7 -1 8 112299 23824 1 -4 0 8 291154 59006 1 -3 0 8 167523 33926 1 -2 0 8 91675 18689 1 -1 0 8 387324 78037 1 0 0 8 248738 48748 1 1 0 8 13091 3199 1 2 0 8 488645 28837 1 3 0 8 291233 13872 1 4 0 8 20772 10860 1 5 0 8 252042 60275 1 6 0 8 118715 23795 1 7 0 8 2189 337 1 -4 1 8 5809 5809 1 -2 1 8 261387 52698 1 -1 1 8 78037 15910 1 0 1 8 370319 74165 1 1 1 8 448742 31021 1 2 1 8 2257 4924 1 3 1 8 374986 51816 1 4 1 8 304124 25002 1 5 1 8 5788 4122 1 6 1 8 113737 17879 1 7 1 8 156161 22793 1 -4 2 8 269064 23812 1 -3 2 8 17594 22308 1 -2 2 8 461882 52067 1 -1 2 8 413072 72313 1 0 2 8 28845 7534 1 1 2 8 387558 15864 1 2 2 8 543783 18060 1 3 2 8 2686 842 1 4 2 8 441454 100659 1 5 2 8 194887 35219 1 6 2 8 13035 2285 1 7 2 8 118905 8399 1 -3 3 8 615852 119287 1 -2 3 8 45907 15490 1 -1 3 8 213487 43017 1 0 3 8 649510 46721 1 2 3 8 226558 8039 1 3 3 8 489602 24455 1 4 3 8 62398 2273 1 5 3 8 168353 51725 1 6 3 8 327541 45006 1 7 3 8 54556 7360 1 8 3 8 78037 20204 1 -3 4 8 75750 20242 1 -2 4 8 451898 18676 1 -1 4 8 177350 12872 1 0 4 8 89973 3471 1 1 4 8 769725 33583 1 2 4 8 114989 16502 1 3 4 8 148115 10535 1 4 4 8 507683 19278 1 5 4 8 67215 3409 1 6 4 8 19841 3820 1 7 4 8 257346 15360 1 8 4 8 39229 9681 1 -2 5 8 9257 2020 1 -1 5 8 391203 29506 1 0 5 8 340518 68356 1 1 5 8 28706 6230 1 2 5 8 391396 27828 1 3 5 8 288598 20128 1 4 5 8 28422 2555 1 5 5 8 419167 11978 1 6 5 8 185199 21972 1 7 5 8 7171 5637 1 8 5 8 171480 11617 1 -2 6 8 281713 30309 1 -1 6 8 12744 1679 1 0 6 8 330332 11449 1 1 6 8 415438 12733 1 2 6 8 23390 2914 1 3 6 8 259634 13681 1 4 6 8 430557 12054 1 5 6 8 3067 863 1 6 6 8 150697 12523 1 7 6 8 266774 12291 1 8 6 8 -6145 10716 1 -1 7 8 299526 21073 1 0 7 8 104251 5177 1 1 7 8 189645 6590 1 2 7 8 369579 13730 1 3 7 8 70761 5091 1 4 7 8 128561 12082 1 5 7 8 298193 12684 1 6 7 8 72379 9044 1 7 7 8 56402 13132 1 8 7 8 138138 19657 1 0 8 8 424271 26896 1 1 8 8 145034 15286 1 2 8 8 36000 3159 1 3 8 8 287894 18056 1 4 8 8 126514 8138 1 5 8 8 9113 4023 1 6 8 8 260880 16429 1 7 8 8 52711 3931 1 2 9 8 187558 29344 1 3 9 8 3000 471 1 4 9 8 210316 15430 1 5 9 8 150463 13281 1 6 9 8 1346 5423 1 0 -6 9 689 130628 1 1 -6 9 152495 131956 1 -2 -5 9 27780 182339 1 1 -5 9 91498 110912 1 2 -5 9 63601 89237 1 3 -5 9 332784 92138 1 -3 -4 9 25591 235711 1 0 -4 9 15658 147572 1 1 -4 9 234196 70461 1 2 -4 9 124506 84435 1 3 -4 9 27063 79773 1 4 -4 9 60897 96797 1 -3 -3 9 170301 37461 1 -2 -3 9 23824 242025 1 0 -3 9 205826 127873 1 1 -3 9 -84 134355 1 3 -3 9 174594 51772 1 4 -3 9 6 24827 1 5 -3 9 91115 6836 1 -4 -2 9 -266 50257 1 -3 -2 9 137926 28841 1 -2 -2 9 185875 464603 1 0 -2 9 420660 250948 1 1 -2 9 159610 157000 1 3 -2 9 84752 64947 1 4 -2 9 122502 11491 1 5 -2 9 2280 6398 1 6 -2 9 98525 22687 1 -4 -1 9 305580 62514 1 -3 -1 9 14561 32410 1 -2 -1 9 197270 92643 1 -1 -1 9 261892 53456 1 0 -1 9 6225 17047 1 2 -1 9 359459 144205 1 3 -1 9 55671 8418 1 4 -1 9 147498 48279 1 5 -1 9 188810 45879 1 6 -1 9 22602 3409 1 -2 0 9 94439 19272 1 -1 0 9 75428 15574 1 0 0 9 564154 219632 1 1 0 9 157222 108806 1 2 0 9 43009 15637 1 3 0 9 478696 24328 1 4 0 9 57586 22939 1 5 0 9 44789 11668 1 6 0 9 157706 26199 1 7 0 9 33003 6898 1 -3 1 9 32915 7324 1 -1 1 9 377983 84267 1 0 1 9 10439 2610 1 1 1 9 455714 25855 1 2 1 9 418727 22462 1 3 1 9 1214 19989 1 4 1 9 403674 25541 1 5 1 9 271680 52984 1 6 1 9 6499 2107 1 7 1 9 178046 9176 1 -3 2 9 408191 63895 1 -2 2 9 7529 7997 1 -1 2 9 320789 20631 1 0 2 9 501223 100430 1 1 2 9 5977 3451 1 2 2 9 309792 12375 1 3 2 9 392928 27612 1 5 2 9 167438 49129 1 6 2 9 290128 67531 1 7 2 9 15790 5170 1 -3 3 9 169195 16836 1 -2 3 9 542966 111710 1 -1 3 9 150410 27317 1 0 3 9 257078 17257 1 1 3 9 578755 115919 1 2 3 9 108979 9008 1 3 3 9 192048 9807 1 4 3 9 396965 24960 1 5 3 9 75245 155485 1 6 3 9 89520 18084 1 7 3 9 186434 41106 1 -2 4 9 41854 11584 1 -1 4 9 432121 28827 1 0 4 9 214719 30642 1 1 4 9 32848 4389 1 2 4 9 478426 71562 1 4 4 9 51351 10607 1 5 4 9 299741 24384 1 6 4 9 80081 15908 1 7 4 9 17005 4253 1 8 4 9 121307 24329 1 -2 5 9 169553 24443 1 -1 5 9 1337 3406 1 1 5 9 370779 13233 1 2 5 9 14838 2569 1 3 5 9 382454 15589 1 4 5 9 128540 13772 1 5 5 9 1453 828 1 6 5 9 262426 13995 1 7 5 9 167774 36271 1 8 5 9 5417 16422 1 -1 6 9 246516 17825 1 0 6 9 4277 998 1 1 6 9 231965 12964 1 2 6 9 380819 32000 1 3 6 9 2883 4174 1 4 6 9 188762 12364 1 5 6 9 326018 20135 1 6 6 9 3943 1432 1 7 6 9 126912 10961 1 0 7 9 294391 15195 1 1 7 9 51280 2231 1 2 7 9 138605 5027 1 3 7 9 227247 16532 1 4 7 9 47807 3137 1 5 7 9 62404 3662 1 6 7 9 315757 16233 1 7 7 9 18521 4463 1 1 8 9 304696 22412 1 2 8 9 166564 14656 1 3 8 9 33446 4673 1 4 8 9 250714 18826 1 5 8 9 110775 9514 1 6 8 9 16704 2538 1 3 9 9 192665 29563 1 4 9 9 -132 2442 1 5 9 9 128394 27894 1 0 -5 10 92937 217443 1 1 -5 10 163651 191431 1 0 -4 10 67178 229397 1 2 -4 10 222999 147319 1 3 -4 10 91927 147656 1 -2 -3 10 92021 21094 1 0 -3 10 245897 199007 1 1 -3 10 214329 182003 1 2 -3 10 -14564 158095 1 3 -3 10 184865 119960 1 4 -3 10 47007 81994 1 -2 -2 10 169361 35400 1 -1 -2 10 230239 50257 1 0 -2 10 -136712 367036 1 1 -2 10 129809 221316 1 2 -2 10 134608 174174 1 3 -2 10 14395 148498 1 4 -2 10 43666 50972 1 5 -2 10 188566 39650 1 -3 -1 10 231923 47731 1 -2 -1 10 48800 14269 1 -1 -1 10 85614 17763 1 0 -1 10 334221 87760 1 1 -1 10 60381 71850 1 2 -1 10 65073 13217 1 3 -1 10 72229 176362 1 4 -1 10 56403 33042 1 5 -1 10 78896 14227 1 6 -1 10 209995 46511 1 -2 0 10 231165 47058 1 -1 0 10 68356 14143 1 0 0 10 22731 5051 1 1 0 10 294870 84879 1 2 0 10 149017 11942 1 3 0 10 34289 7407 1 4 0 10 248204 54117 1 5 0 10 95310 39397 1 6 0 10 15081 4745 1 -2 1 10 9934 3536 1 -1 1 10 306907 36619 1 0 1 10 149929 30474 1 1 1 10 2061 18879 1 2 1 10 271043 106189 1 3 1 10 139739 31568 1 4 1 10 2714 4638 1 5 1 10 142550 32607 1 6 1 10 137957 28350 1 7 1 10 110 1693 1 -2 2 10 282348 57581 1 -1 2 10 5166 4978 1 0 2 10 149929 30390 1 1 2 10 501702 62000 1 2 2 10 29530 5682 1 3 2 10 262688 13880 1 4 2 10 67346 884842 1 5 2 10 6693 1498 1 6 2 10 84302 17767 1 7 2 10 141592 22938 1 -2 3 10 138275 19783 1 -1 3 10 445229 88518 1 0 3 10 110027 6987 1 1 3 10 138059 28033 1 2 3 10 468324 53203 1 3 3 10 48841 5640 1 4 3 10 79226 6903 1 5 3 10 253288 100317 1 6 3 10 93617 50896 1 7 3 10 72221 3534 1 -1 4 10 37835 3907 1 0 4 10 448592 68482 1 1 4 10 196683 25507 1 2 4 10 44785 9428 1 3 4 10 385102 45164 1 4 4 10 142304 18604 1 5 4 10 30318 2399 1 6 4 10 250956 107446 1 7 4 10 91422 4967 1 -1 5 10 209727 21138 1 0 5 10 4783 2979 1 1 5 10 337199 31957 1 2 5 10 291274 53245 1 3 5 10 178 2082 1 4 5 10 274348 9280 1 5 5 10 191028 26811 1 6 5 10 453 1560 1 7 5 10 150706 40366 1 0 6 10 260138 13932 1 1 6 10 842 6566 1 2 6 10 172051 11274 1 3 6 10 262692 38724 1 4 6 10 11269 927 1 5 6 10 160521 16132 1 6 6 10 197857 54466 1 7 6 10 10712 1810 1 1 7 10 298346 32302 1 2 7 10 46003 2694 1 3 7 10 90199 11206 1 4 7 10 184893 33526 1 5 7 10 33684 2895 1 6 7 10 54639 9187 1 3 8 10 81187 12661 1 4 8 10 7336 6543 1 5 8 10 191217 25796 1 0 -3 11 45627 316021 1 1 -3 11 85193 297080 1 2 -3 11 22393 277213 1 3 -3 11 -842 96473 1 -1 -2 11 145299 30895 1 0 -2 11 127456 30306 1 2 -2 11 58928 261134 1 3 -2 11 40374 63895 1 4 -2 11 3436 29184 1 -1 -1 11 8418 3536 1 0 -1 11 100009 20877 1 1 -1 11 201717 41779 1 2 -1 11 22403 71850 1 3 -1 11 62403 14558 1 4 -1 11 150346 40497 1 5 -1 11 6188 10863 1 -1 0 11 243287 49752 1 0 0 11 59685 12543 1 1 0 11 37608 47973 1 2 0 11 242271 35499 1 3 0 11 68962 6413 1 4 0 11 33352 4171 1 5 0 11 175168 31358 1 -1 1 11 3393 6013 1 0 1 11 253389 51351 1 1 1 11 208811 97356 1 2 1 11 2189 13132 1 3 1 11 252543 45181 1 4 1 11 154622 23885 1 5 1 11 788 3148 1 6 1 11 165229 29500 1 -1 2 11 345266 47605 1 0 2 11 1599 5977 1 1 2 11 204320 22350 1 2 2 11 327744 68398 1 3 2 11 18103 12837 1 4 2 11 104965 4753 1 5 2 11 230880 13465 1 6 2 11 3534 21719 1 -1 3 11 77195 16247 1 0 3 11 490111 99167 1 1 3 11 49163 10354 1 2 3 11 128740 7955 1 3 3 11 232138 21677 1 4 3 11 45973 32761 1 5 3 11 49395 15700 1 6 3 11 142720 26517 1 0 4 11 26758 3054 1 1 4 11 272499 55560 1 3 4 11 25556 1745 1 4 4 11 248473 34767 1 5 4 11 103035 5346 1 6 4 11 34324 64484 1 1 5 11 -484 3757 1 2 5 11 301121 61285 1 4 5 11 1221 2396 1 5 5 11 194323 7661 1 6 5 11 168877 15153 1 1 6 11 295092 29994 1 2 6 11 942 2830 1 3 6 11 119664 21593 1 4 6 11 219221 17384 1 5 6 11 27697 2147 1 6 6 11 150729 30448 1 3 7 11 47326 8755 1 4 7 11 63744 4778 1 5 7 11 258079 32904 1 1 -1 12 104424 23666 1 2 -1 12 91895 75526 1 3 -1 12 13392 5514 1 1 0 12 103678 70229 1 2 0 12 29998 9302 1 3 0 12 182113 14161 1 4 0 12 104493 40113 1 0 1 12 2373 82330 1 1 1 12 256899 89672 1 2 1 12 104275 10060 1 3 1 12 1412 20263 1 4 1 12 147620 60787 1 5 1 12 94617 21746 1 1 2 12 6313 7104 1 2 2 12 197814 11735 1 3 2 12 163839 49499 1 4 2 12 2250 43905 1 5 2 12 85583 54598 1 1 3 12 291440 59601 1 2 3 12 60483 11870 1 3 3 12 57868 3712 1 4 3 12 181325 188232 1 5 3 12 37678 13782 1 2 4 12 193167 16458 1 3 4 12 117100 5467 1 4 4 12 6145 1431 1 5 4 12 144088 33223 1 3 5 12 202383 8786 1 4 5 12 163677 6991 1 ; _shelx_hkl_checksum 46079 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 Re_2 Re 0.16626(8) 0.79167(7) 0.33061(7) 0.0148(4) Uani 1 1 d D U . . . O12_2 O 0.2772(18) 0.5844(8) 0.2833(14) 0.046(4) Uani 1 1 d D U . . . O13_2 O 0.132(2) 0.9187(13) 0.1785(10) 0.038(4) Uani 1 1 d D U . . . O14_2 O -0.0716(14) 0.8159(15) 0.4560(12) 0.052(5) Uani 1 1 d D U . . . O15_2 O 0.3354(15) 0.8317(15) 0.3981(13) 0.044(4) Uani 1 1 d D U . . . O7_1 O 0.738(3) 0.605(2) 0.109(2) 0.045(4) Uani 1 1 d . U . . . C5_1 C 0.783(3) 0.510(3) 0.209(3) 0.029(4) Uani 1 1 d . U . . . C6_1 C 0.781(3) 0.552(2) 0.347(3) 0.031(5) Uani 1 1 d . U . . . H6A_1 H 0.823633 0.452086 0.405815 0.046 Uiso 1 1 calc R U . . . H6B_1 H 0.876484 0.610463 0.330680 0.046 Uiso 1 1 calc R U . . . H6C_1 H 0.642473 0.619734 0.393225 0.046 Uiso 1 1 calc R U . . . O4_1 O 0.8353(19) 0.3479(16) 0.2079(17) 0.024(3) Uani 1 1 d . U . . . C3_1 C 0.828(3) 0.292(2) 0.085(2) 0.022(3) Uani 1 1 d . U . . . H3A_1 H 0.921248 0.179141 0.073435 0.026 Uiso 1 1 calc R U . . . H3B_1 H 0.874553 0.359905 0.001075 0.026 Uiso 1 1 calc R U . . . C2_1 C 0.606(3) 0.303(2) 0.098(2) 0.017(3) Uani 1 1 d . U . . . H2A_1 H 0.512476 0.411550 0.128448 0.021 Uiso 1 1 calc R U . . . H2B_1 H 0.597093 0.295885 0.004861 0.021 Uiso 1 1 calc R U . . . N1_1 N 0.5293(17) 0.1768(16) 0.1986(15) 0.014(3) Uani 1 1 d D U . . . C10_1 C 0.311(2) 0.229(2) 0.195(2) 0.024(4) Uani 1 1 d D U . . . H10A_1 H 0.306369 0.229839 0.099674 0.036 Uiso 1 1 calc R U . . . H10B_1 H 0.246144 0.154422 0.256594 0.036 Uiso 1 1 calc R U . . . H10C_1 H 0.237669 0.338545 0.226878 0.036 Uiso 1 1 calc R U . . . C9_1 C 0.538(2) 0.176(2) 0.3437(16) 0.018(4) Uani 1 1 d D U . . . H9A_1 H 0.681446 0.141127 0.345314 0.027 Uiso 1 1 calc R U . . . H9B_1 H 0.464913 0.284798 0.375689 0.027 Uiso 1 1 calc R U . . . H9C_1 H 0.473388 0.100674 0.405405 0.027 Uiso 1 1 calc R U . . . C8_1 C 0.644(2) 0.0111(19) 0.148(2) 0.024(4) Uani 1 1 d D U . . . H8A_1 H 0.637513 0.012276 0.053079 0.036 Uiso 1 1 calc R U . . . H8B_1 H 0.787014 -0.021977 0.149461 0.036 Uiso 1 1 calc R U . . . H8C_1 H 0.581036 -0.065416 0.209539 0.036 Uiso 1 1 calc R U . . . 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 Re_2 0.0103(5) 0.0112(5) 0.0169(6) -0.0057(4) 0.0025(3) 0.0001(3) O12_2 0.033(8) 0.031(8) 0.059(11) -0.014(8) 0.009(8) -0.006(7) O13_2 0.036(8) 0.039(8) 0.031(9) 0.016(8) -0.015(7) -0.011(7) O14_2 0.040(9) 0.047(9) 0.062(11) -0.020(9) 0.007(8) -0.015(8) O15_2 0.036(8) 0.050(9) 0.044(10) -0.021(8) -0.014(7) -0.002(7) O7_1 0.049(9) 0.032(8) 0.050(11) -0.003(8) -0.007(8) -0.017(7) C5_1 0.020(7) 0.025(7) 0.041(8) -0.003(7) -0.007(6) -0.008(6) C6_1 0.031(9) 0.013(8) 0.052(13) 0.000(9) -0.016(9) -0.009(8) O4_1 0.017(5) 0.020(5) 0.039(7) 0.000(5) -0.005(5) -0.015(4) C3_1 0.019(6) 0.016(6) 0.030(7) 0.000(6) -0.001(6) -0.010(5) C2_1 0.020(6) 0.008(6) 0.021(7) 0.001(6) -0.004(6) -0.004(5) N1_1 0.016(6) 0.009(5) 0.017(7) -0.002(5) -0.008(5) 0.000(5) C10_1 0.022(9) 0.013(8) 0.032(11) 0.001(8) -0.010(8) 0.000(7) C9_1 0.027(9) 0.015(8) 0.013(10) 0.006(8) -0.001(7) -0.016(7) C8_1 0.022(8) 0.013(8) 0.032(11) -0.004(8) -0.001(8) -0.004(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0020 0.0012 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0042 0.0025 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0077 0.0045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -0.5008 5.8080 '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' 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 O15_2 Re_2 O14_2 110.8(4) . . ? O15_2 Re_2 O13_2 110.5(4) . . ? O14_2 Re_2 O13_2 110.5(4) . . ? O15_2 Re_2 O12_2 108.9(4) . . ? O14_2 Re_2 O12_2 108.5(4) . . ? O13_2 Re_2 O12_2 107.7(4) . . ? O7_1 C5_1 O4_1 122.3(18) . . ? O7_1 C5_1 C6_1 127.4(19) . . ? O4_1 C5_1 C6_1 110(2) . . ? C5_1 C6_1 H6A_1 109.5 . . ? C5_1 C6_1 H6B_1 109.5 . . ? H6A_1 C6_1 H6B_1 109.5 . . ? C5_1 C6_1 H6C_1 109.5 . . ? H6A_1 C6_1 H6C_1 109.5 . . ? H6B_1 C6_1 H6C_1 109.5 . . ? C5_1 O4_1 C3_1 115.8(18) . . ? O4_1 C3_1 C2_1 110.1(15) . . ? O4_1 C3_1 H3A_1 109.6 . . ? C2_1 C3_1 H3A_1 109.6 . . ? O4_1 C3_1 H3B_1 109.6 . . ? C2_1 C3_1 H3B_1 109.6 . . ? H3A_1 C3_1 H3B_1 108.2 . . ? N1_1 C2_1 C3_1 116.6(15) . . ? N1_1 C2_1 H2A_1 108.1 . . ? C3_1 C2_1 H2A_1 108.1 . . ? N1_1 C2_1 H2B_1 108.1 . . ? C3_1 C2_1 H2B_1 108.1 . . ? H2A_1 C2_1 H2B_1 107.3 . . ? C9_1 N1_1 C10_1 109.8(9) . . ? C9_1 N1_1 C8_1 109.7(9) . . ? C10_1 N1_1 C8_1 109.9(9) . . ? C9_1 N1_1 C2_1 112.9(12) . . ? C10_1 N1_1 C2_1 102.7(14) . . ? C8_1 N1_1 C2_1 111.5(14) . . ? N1_1 C10_1 H10A_1 109.5 . . ? N1_1 C10_1 H10B_1 109.5 . . ? H10A_1 C10_1 H10B_1 109.5 . . ? N1_1 C10_1 H10C_1 109.5 . . ? H10A_1 C10_1 H10C_1 109.5 . . ? H10B_1 C10_1 H10C_1 109.5 . . ? N1_1 C9_1 H9A_1 109.5 . . ? N1_1 C9_1 H9B_1 109.5 . . ? H9A_1 C9_1 H9B_1 109.5 . . ? N1_1 C9_1 H9C_1 109.5 . . ? H9A_1 C9_1 H9C_1 109.5 . . ? H9B_1 C9_1 H9C_1 109.5 . . ? N1_1 C8_1 H8A_1 109.5 . . ? N1_1 C8_1 H8B_1 109.5 . . ? H8A_1 C8_1 H8B_1 109.5 . . ? N1_1 C8_1 H8C_1 109.5 . . ? H8A_1 C8_1 H8C_1 109.5 . . ? H8B_1 C8_1 H8C_1 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re_2 O15_2 1.759(7) . ? Re_2 O14_2 1.762(8) . ? Re_2 O13_2 1.764(7) . ? Re_2 O12_2 1.813(6) . ? O7_1 C5_1 1.23(3) . ? C5_1 O4_1 1.36(3) . ? C5_1 C6_1 1.51(3) . ? C6_1 H6A_1 0.9800 . ? C6_1 H6B_1 0.9800 . ? C6_1 H6C_1 0.9800 . ? O4_1 C3_1 1.45(2) . ? C3_1 C2_1 1.55(2) . ? C3_1 H3A_1 0.9900 . ? C3_1 H3B_1 0.9900 . ? C2_1 N1_1 1.52(3) . ? C2_1 H2A_1 0.9900 . ? C2_1 H2B_1 0.9900 . ? N1_1 C9_1 1.494(13) . ? N1_1 C10_1 1.494(12) . ? N1_1 C8_1 1.496(12) . ? C10_1 H10A_1 0.9800 . ? C10_1 H10B_1 0.9800 . ? C10_1 H10C_1 0.9800 . ? C9_1 H9A_1 0.9800 . ? C9_1 H9B_1 0.9800 . ? C9_1 H9C_1 0.9800 . ? C8_1 H8A_1 0.9800 . ? C8_1 H8B_1 0.9800 . ? C8_1 H8C_1 0.9800 . ? 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 O7_1 C5_1 O4_1 C3_1 -2(3) . . . . ? C6_1 C5_1 O4_1 C3_1 175.7(15) . . . . ? C5_1 O4_1 C3_1 C2_1 -84(2) . . . . ? O4_1 C3_1 C2_1 N1_1 -74.0(18) . . . . ? C3_1 C2_1 N1_1 C9_1 57.4(15) . . . . ? C3_1 C2_1 N1_1 C10_1 175.7(12) . . . . ? C3_1 C2_1 N1_1 C8_1 -66.7(14) . . . . ?