#------------------------------------------------------------------------------ #$Date: 2026-06-30 01:17:23 +0100 (Tue, 30 Jun 2026) $ #$Revision: 306684 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/11/7721187.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_7721187 loop_ _publ_author_name 'Jacobs, Frederick J. F.' 'Fourie, Eleanor' 'Brink, Alice' _publ_section_title ; Engineering the rhenium metalation of phenanthroline imino complexes for variable structure activity relationships. ; _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_paper_doi 10.1039/d6dt00636a _journal_year 2026 _chemical_formula_moiety 'C46 H28 N6 O8 Re2, 1.437(C3 H7 N O), 0.563(H2 O1)' _chemical_formula_sum 'C50.31 H39.19 N7.43 O10 Re2' _chemical_formula_weight 1280.28 _chemical_name_common fac-[Re(CO)3(Phen5MeSal)]2 _chemical_name_systematic fac-bis{2-([1,10-Phenanthrolin-5-ylimino]methyl)phenol-N,N'}-hexacarbonyl-di-rhenium(I)] _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2023-12-07 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2026-06-02 deposited with the CCDC. 2026-06-15 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 102.8830(10) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 10.0739(4) _cell_length_b 21.6296(8) _cell_length_c 11.0985(4) _cell_measurement_reflns_used 59425 _cell_measurement_temperature 100.00 _cell_measurement_theta_max 0.7457 _cell_measurement_theta_min 0.6345 _cell_volume 2357.43(15) _computing_cell_refinement 'APEX5 (Bruker, 2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 100.00 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker D8 Venture 4K Kappa Photon III C28 diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_unetI/netI 0.0236 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 58555 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.335 _diffrn_reflns_theta_min 2.074 _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _exptl_absorpt_coefficient_mu 5.198 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6345 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1477 before and 0.0601 after correction. The Ratio of minimum to maximum transmission is 0.8509. The \l/2 correction factor is Not present. ; _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.804 _exptl_crystal_description prism _exptl_crystal_F_000 1246 _exptl_crystal_size_max 0.105 _exptl_crystal_size_mid 0.058 _exptl_crystal_size_min 0.027 _refine_diff_density_max 1.638 _refine_diff_density_min -2.079 _refine_diff_density_rms 0.128 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 322 _refine_ls_number_reflns 5871 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.080 _refine_ls_R_factor_all 0.0328 _refine_ls_R_factor_gt 0.0288 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0180P)^2^+10.8709P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.0659 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5242 _reflns_number_total 5871 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00636a2.cif _cod_data_source_block mo_v1_22ffj11_0m _cod_database_code 7721187 _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 0.872 _shelx_estimated_absorpt_t_min 0.611 _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,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(O1) = Uanis(O1B) Uanis(O3) = Uanis(O1A) Uanis(N1A) = Uanis(C1A) 3. Others Fixed Sof: N1A(0.71834) O1A(0.71834) C1A(0.71834) H1A(0.71834) C4A(0.71834) H4AA(0.71834) H4AB(0.71834) H4AC(0.71834) C3A(0.71834) H3AA(0.71834) H3AB(0.71834) H3AC(0.71834) O1B(0.28166) H1BA(0.28166) H1BB(0.28166) 4.a Free rotating group: O1B(H1BA,H1BB) 4.b Aromatic/amide H refined with riding coordinates: C10(H10), C15(H15), C4(H4), C14(H14), C21(H21), C13(H13), C18(H18), C16(H16), C5(H5), C6(H6), C19(H19), C1A(H1A) 4.c Idealised Me refined as rotating group: C23(H23A,H23B,H23C), C4A(H4AA,H4AB,H4AC), C3A(H3AA,H3AB,H3AC) ; _shelx_res_file ; TITL mo_v1_22ffj11_0m_a.res in P2(1)/c mo_v1_22ffj11_0m.res created by SHELXL-2018/3 at 10:58:27 on 07-Dec-2023 CELL 0.71073 10.0739 21.6296 11.0985 90 102.883 90 ZERR 2 0.0004 0.0008 0.0004 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O Re UNIT 100.62 78.37 14.87 20 4 EADP O1 O1B EADP O3 O1A EADP N1A C1A L.S. 4 PLAN 20 SIZE 0.027 0.058 0.105 TEMP -173.15 CONF MORE -1 BOND BOND $H LIST 4 fmap 2 acta MERG 2 OMIT -1 1 2 OMIT 1 1 0 REM REM REM WGHT 0.018000 10.870900 FVAR 0.25616 RE1 5 0.202525 0.483456 0.856568 11.00000 0.02052 0.02072 = 0.01308 -0.00150 0.00728 -0.00176 O4 4 0.351723 0.414389 0.847037 11.00000 0.01944 0.02100 = 0.01892 -0.00340 0.00727 -0.00248 N2 3 0.358461 0.543205 0.810586 11.00000 0.01902 0.02024 = 0.01308 -0.00146 0.00539 -0.00106 O1 4 0.010640 0.593252 0.852685 11.00000 0.03160 0.03248 = 0.03137 -0.00527 0.00826 0.00620 N1 3 0.173633 0.473593 0.657687 11.00000 0.02166 0.01717 = 0.01445 -0.00228 0.00629 -0.00048 O2 4 0.272240 0.501610 1.137647 11.00000 0.04201 0.03979 = 0.01495 -0.00179 0.00810 0.00373 O3 4 -0.042061 0.400921 0.868524 11.00000 0.03304 0.04234 = 0.06077 0.00278 0.02205 -0.00384 C12 1 0.252647 0.509344 0.478909 11.00000 0.01944 0.02144 = 0.01444 -0.00121 0.00439 0.00193 C11 1 0.257641 0.509235 0.606397 11.00000 0.02311 0.01906 = 0.01377 -0.00124 0.00680 0.00020 N3 3 0.486236 0.369122 0.535870 11.00000 0.02283 0.02273 = 0.01729 0.00037 0.00778 -0.00145 C9 1 0.354348 0.547213 0.686640 11.00000 0.02143 0.01918 = 0.01145 -0.00085 0.00493 0.00238 C2 1 0.247430 0.493380 1.032450 11.00000 0.02540 0.02423 = 0.02191 0.00094 0.00934 0.00198 C10 1 0.339269 0.550748 0.430695 11.00000 0.02834 0.02601 = 0.01144 -0.00088 0.00879 0.00038 AFIX 43 H10 2 0.332265 0.552481 0.343972 11.00000 -1.20000 AFIX 0 C1 1 0.083218 0.551907 0.853015 11.00000 0.02963 0.02599 = 0.01379 -0.00045 0.00747 -0.00224 C8 1 0.431368 0.587648 0.506459 11.00000 0.01929 0.02135 = 0.01680 0.00080 0.00809 0.00145 C7 1 0.441510 0.585781 0.638620 11.00000 0.02077 0.01974 = 0.01500 -0.00027 0.00517 0.00090 C15 1 0.088132 0.435520 0.584461 11.00000 0.01871 0.02232 = 0.01809 -0.00137 0.00460 -0.00285 AFIX 43 H15 2 0.029940 0.410179 0.619977 11.00000 -1.20000 AFIX 0 C22 1 0.318391 0.359372 0.796643 11.00000 0.01794 0.01826 = 0.01668 -0.00079 0.00373 -0.00105 C3 1 0.052814 0.430555 0.868788 11.00000 0.02340 0.02872 = 0.02019 -0.00322 0.00957 0.00087 C4 1 0.448614 0.577338 0.887872 11.00000 0.02442 0.02289 = 0.01527 -0.00146 0.00536 -0.00241 AFIX 43 H4 2 0.453008 0.574229 0.974055 11.00000 -1.20000 AFIX 0 C14 1 0.080352 0.431252 0.457824 11.00000 0.02264 0.02287 = 0.01784 -0.00506 0.00379 -0.00074 AFIX 43 H14 2 0.019427 0.402692 0.409125 11.00000 -1.20000 AFIX 0 C21 1 0.235999 0.318405 0.845843 11.00000 0.02374 0.02397 = 0.01531 0.00025 0.00581 -0.00169 AFIX 43 H21 2 0.206086 0.330021 0.917981 11.00000 -1.20000 AFIX 0 C13 1 0.160739 0.468324 0.403645 11.00000 0.02551 0.02428 = 0.01405 -0.00483 0.00515 -0.00141 AFIX 43 H13 2 0.154802 0.466487 0.317083 11.00000 -1.20000 AFIX 0 C17 1 0.365205 0.340282 0.690521 11.00000 0.02016 0.01898 = 0.01745 -0.00014 0.00516 -0.00019 C20 1 0.197277 0.261619 0.792064 11.00000 0.02437 0.02546 = 0.02217 0.00394 0.00610 -0.00220 C18 1 0.327281 0.282090 0.638821 11.00000 0.02661 0.02193 = 0.02042 -0.00212 0.00774 0.00043 AFIX 43 H18 2 0.360501 0.268900 0.569372 11.00000 -1.20000 AFIX 0 C16 1 0.445483 0.381906 0.635206 11.00000 0.02196 0.02014 = 0.01726 0.00031 0.00657 0.00168 AFIX 43 H16 2 0.469749 0.420773 0.673710 11.00000 -1.20000 AFIX 0 C5 1 0.537179 0.617642 0.846867 11.00000 0.02482 0.02535 = 0.01820 -0.00338 0.00392 -0.00435 AFIX 43 H5 2 0.599599 0.641945 0.904590 11.00000 -1.20000 AFIX 0 C6 1 0.533918 0.622136 0.722167 11.00000 0.02301 0.02374 = 0.01904 -0.00041 0.00722 -0.00378 AFIX 43 H6 2 0.593679 0.649577 0.693386 11.00000 -1.20000 AFIX 0 C19 1 0.242711 0.243487 0.686552 11.00000 0.03038 0.02101 = 0.02469 0.00058 0.00542 -0.00188 AFIX 43 H19 2 0.215366 0.204856 0.648257 11.00000 -1.20000 AFIX 0 C23 1 0.108367 0.218721 0.845796 11.00000 0.04570 0.03336 = 0.03096 -0.00168 0.01448 -0.01802 AFIX 137 H23A 2 0.165186 0.187769 0.897675 11.00000 -1.50000 H23B 2 0.044083 0.197939 0.778738 11.00000 -1.50000 H23C 2 0.057833 0.242472 0.896026 11.00000 -1.50000 AFIX 0 PART 1 N1A 3 -0.251103 0.259856 0.457968 10.71834 0.02730 0.05720 = 0.06910 0.01312 0.01540 0.00439 O1A 4 -0.192875 0.332702 0.326044 10.71834 0.03304 0.04234 = 0.06077 0.00278 0.02205 -0.00384 C1A 1 -0.260632 0.287010 0.348930 10.71834 0.02730 0.05720 = 0.06910 0.01312 0.01540 0.00439 AFIX 43 H1A 2 -0.325281 0.270189 0.281258 10.71834 -1.20000 AFIX 0 C4A 1 -0.165489 0.291156 0.549547 10.71834 0.04376 0.06451 = 0.11484 -0.01000 0.03620 -0.00338 AFIX 137 H4AA 2 -0.131108 0.327980 0.515018 10.71834 -1.50000 H4AB 2 -0.088923 0.264421 0.587233 10.71834 -1.50000 H4AC 2 -0.214653 0.303653 0.612476 10.71834 -1.50000 AFIX 0 C3A 1 -0.333329 0.211322 0.475363 10.71834 0.08322 0.09774 = 0.10297 -0.00117 0.02237 -0.06054 AFIX 137 H3AA 2 -0.382244 0.195560 0.394894 10.71834 -1.50000 H3AB 2 -0.399021 0.225596 0.522438 10.71834 -1.50000 H3AC 2 -0.277233 0.178273 0.521137 10.71834 -1.50000 AFIX 6 PART 2 O1B 4 -0.152742 0.338049 0.455661 10.28166 0.03160 0.03248 = 0.03137 -0.00527 0.00826 0.00620 H1BA 2 -0.204181 0.370290 0.434160 10.28166 -1.50000 H1BB 2 -0.134603 0.334317 0.535741 10.28166 -1.50000 AFIX 0 HKLF 4 REM mo_v1_22ffj11_0m_a.res in P2(1)/c REM wR2 = 0.0659, GooF = S = 1.080, Restrained GooF = 1.080 for all data REM R1 = 0.0288 for 5242 Fo > 4sig(Fo) and 0.0328 for all 5871 data REM 322 parameters refined using 0 restraints END WGHT 0.0180 10.8709 REM Highest difference peak 1.638, deepest hole -2.079, 1-sigma level 0.128 Q1 1 -0.1751 0.3397 0.3956 11.00000 0.05 1.31 Q2 1 0.1253 0.4912 0.8260 11.00000 0.05 1.19 Q3 1 -0.2253 0.2425 0.4593 11.00000 0.05 0.82 Q4 1 -0.2912 0.2462 0.3172 11.00000 0.05 0.80 Q5 1 0.2531 0.5305 0.9180 11.00000 0.05 0.78 Q6 1 -0.2087 0.3012 0.4389 11.00000 0.05 0.67 Q7 1 0.1649 0.5323 0.9034 11.00000 0.05 0.66 Q8 1 0.2439 0.5048 0.8400 11.00000 0.05 0.64 Q9 1 0.3922 0.5285 0.4242 11.00000 0.05 0.61 Q10 1 -0.3472 0.2369 0.4007 11.00000 0.05 0.60 Q11 1 0.1298 0.4384 0.8828 11.00000 0.05 0.56 Q12 1 0.1111 0.4436 0.8407 11.00000 0.05 0.55 Q13 1 0.2513 0.5774 0.9111 11.00000 0.05 0.55 Q14 1 0.2136 0.4272 0.8779 11.00000 0.05 0.53 Q15 1 -0.3640 0.2154 0.4873 11.00000 0.05 0.52 Q16 1 0.2985 0.4830 0.9342 11.00000 0.05 0.51 Q17 1 0.1890 0.4276 0.8451 11.00000 0.05 0.50 Q18 1 -0.1784 0.3015 0.5780 11.00000 0.05 0.44 Q19 1 0.0154 0.5006 0.2800 11.00000 0.05 0.44 Q20 1 0.4625 0.4910 0.4843 11.00000 0.05 0.43 ; _shelx_res_checksum 4989 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.20253(2) 0.48346(2) 0.85657(2) 0.01755(5) Uani 1 1 d . . . . . O4 O 0.3517(3) 0.41439(12) 0.8470(2) 0.0193(5) Uani 1 1 d . . . . . N2 N 0.3585(3) 0.54320(15) 0.8106(3) 0.0172(6) Uani 1 1 d . . . . . O1 O 0.0106(3) 0.59325(15) 0.8527(3) 0.0316(7) Uani 1 1 d . . . . . N1 N 0.1736(3) 0.47359(14) 0.6577(3) 0.0174(6) Uani 1 1 d . . . . . O2 O 0.2722(3) 0.50161(15) 1.1376(3) 0.0320(7) Uani 1 1 d . . . . . O3 O -0.0421(4) 0.40092(17) 0.8685(4) 0.0436(7) Uani 1 1 d . . . . . C12 C 0.2526(4) 0.50934(18) 0.4789(3) 0.0183(7) Uani 1 1 d . . . . . C11 C 0.2576(4) 0.50923(17) 0.6064(3) 0.0182(7) Uani 1 1 d . . . . . N3 N 0.4862(3) 0.36912(15) 0.5359(3) 0.0204(6) Uani 1 1 d . . . . . C9 C 0.3543(4) 0.54721(17) 0.6866(3) 0.0172(7) Uani 1 1 d . . . . . C2 C 0.2474(4) 0.49338(19) 1.0325(4) 0.0232(8) Uani 1 1 d . . . . . C10 C 0.3393(4) 0.55075(19) 0.4307(3) 0.0212(8) Uani 1 1 d . . . . . H10 H 0.332265 0.552481 0.343972 0.025 Uiso 1 1 calc R U . . . C1 C 0.0832(4) 0.55191(19) 0.8530(3) 0.0227(8) Uani 1 1 d . . . . . C8 C 0.4314(4) 0.58765(18) 0.5065(3) 0.0185(7) Uani 1 1 d . . . . . C7 C 0.4415(4) 0.58578(17) 0.6386(3) 0.0183(7) Uani 1 1 d . . . . . C15 C 0.0881(4) 0.43552(18) 0.5845(3) 0.0196(7) Uani 1 1 d . . . . . H15 H 0.029940 0.410179 0.619977 0.024 Uiso 1 1 calc R U . . . C22 C 0.3184(4) 0.35937(17) 0.7966(3) 0.0176(7) Uani 1 1 d . . . . . C3 C 0.0528(4) 0.43056(19) 0.8688(4) 0.0234(8) Uani 1 1 d . . . . . C4 C 0.4486(4) 0.57734(18) 0.8879(3) 0.0207(7) Uani 1 1 d . . . . . H4 H 0.453008 0.574229 0.974055 0.025 Uiso 1 1 calc R U . . . C14 C 0.0804(4) 0.43125(18) 0.4578(3) 0.0212(8) Uani 1 1 d . . . . . H14 H 0.019427 0.402692 0.409125 0.025 Uiso 1 1 calc R U . . . C21 C 0.2360(4) 0.31841(18) 0.8458(3) 0.0208(8) Uani 1 1 d . . . . . H21 H 0.206086 0.330021 0.917981 0.025 Uiso 1 1 calc R U . . . C13 C 0.1607(4) 0.46832(18) 0.4036(3) 0.0212(8) Uani 1 1 d . . . . . H13 H 0.154802 0.466487 0.317083 0.025 Uiso 1 1 calc R U . . . C17 C 0.3652(4) 0.34028(17) 0.6905(3) 0.0187(7) Uani 1 1 d . . . . . C20 C 0.1973(4) 0.26162(19) 0.7921(4) 0.0239(8) Uani 1 1 d . . . . . C18 C 0.3273(4) 0.28209(18) 0.6388(4) 0.0226(8) Uani 1 1 d . . . . . H18 H 0.360501 0.268900 0.569372 0.027 Uiso 1 1 calc R U . . . C16 C 0.4455(4) 0.38191(18) 0.6352(3) 0.0194(7) Uani 1 1 d . . . . . H16 H 0.469749 0.420773 0.673710 0.023 Uiso 1 1 calc R U . . . C5 C 0.5372(4) 0.61764(19) 0.8469(4) 0.0229(8) Uani 1 1 d . . . . . H5 H 0.599599 0.641945 0.904590 0.028 Uiso 1 1 calc R U . . . C6 C 0.5339(4) 0.62214(18) 0.7222(3) 0.0215(8) Uani 1 1 d . . . . . H6 H 0.593679 0.649577 0.693386 0.026 Uiso 1 1 calc R U . . . C19 C 0.2427(4) 0.24349(19) 0.6866(4) 0.0255(8) Uani 1 1 d . . . . . H19 H 0.215366 0.204856 0.648257 0.031 Uiso 1 1 calc R U . . . C23 C 0.1084(5) 0.2187(2) 0.8458(4) 0.0357(11) Uani 1 1 d . . . . . H23A H 0.165186 0.187769 0.897675 0.054 Uiso 1 1 calc R U . . . H23B H 0.044083 0.197939 0.778738 0.054 Uiso 1 1 calc R U . . . H23C H 0.057833 0.242472 0.896026 0.054 Uiso 1 1 calc R U . . . N1A N -0.2511(6) 0.2599(3) 0.4580(7) 0.0505(13) Uani 0.7183 1 d . . P A 1 O1A O -0.1929(5) 0.3327(2) 0.3260(5) 0.0436(7) Uani 0.7183 1 d . . P A 1 C1A C -0.2606(8) 0.2870(4) 0.3489(9) 0.0505(13) Uani 0.7183 1 d . . P A 1 H1A H -0.325281 0.270189 0.281258 0.061 Uiso 0.7183 1 calc R U P A 1 C4A C -0.1655(10) 0.2912(5) 0.5495(11) 0.071(3) Uani 0.7183 1 d . . P A 1 H4AA H -0.131108 0.327980 0.515018 0.107 Uiso 0.7183 1 calc R U P A 1 H4AB H -0.088923 0.264421 0.587233 0.107 Uiso 0.7183 1 calc R U P A 1 H4AC H -0.214653 0.303653 0.612476 0.107 Uiso 0.7183 1 calc R U P A 1 C3A C -0.3333(12) 0.2113(6) 0.4754(12) 0.094(4) Uani 0.7183 1 d . . P A 1 H3AA H -0.382244 0.195560 0.394894 0.142 Uiso 0.7183 1 calc R U P A 1 H3AB H -0.399021 0.225596 0.522438 0.142 Uiso 0.7183 1 calc R U P A 1 H3AC H -0.277233 0.178273 0.521137 0.142 Uiso 0.7183 1 calc R U P A 1 O1B O -0.1527(12) 0.3380(5) 0.4557(11) 0.0316(7) Uani 0.2817 1 d G . P B 2 H1BA H -0.204181 0.370290 0.434160 0.047 Uiso 0.2817 1 d G U P B 2 H1BB H -0.134603 0.334317 0.535741 0.047 Uiso 0.2817 1 d G U P B 2 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 0.02052(8) 0.02072(8) 0.01308(7) -0.00150(5) 0.00728(5) -0.00176(6) O4 0.0194(13) 0.0210(13) 0.0189(12) -0.0034(10) 0.0073(10) -0.0025(10) N2 0.0190(15) 0.0202(15) 0.0131(14) -0.0015(11) 0.0054(12) -0.0011(12) O1 0.0316(16) 0.0325(16) 0.0314(16) -0.0053(13) 0.0083(13) 0.0062(13) N1 0.0217(16) 0.0172(15) 0.0144(14) -0.0023(11) 0.0063(12) -0.0005(12) O2 0.0420(19) 0.0398(18) 0.0149(13) -0.0018(12) 0.0081(13) 0.0037(14) O3 0.0330(15) 0.0423(17) 0.061(2) 0.0028(14) 0.0221(14) -0.0038(13) C12 0.0194(17) 0.0214(18) 0.0144(16) -0.0012(14) 0.0044(13) 0.0019(14) C11 0.0231(18) 0.0191(17) 0.0138(16) -0.0012(13) 0.0068(13) 0.0002(14) N3 0.0228(17) 0.0227(16) 0.0173(15) 0.0004(12) 0.0078(12) -0.0015(13) C9 0.0214(18) 0.0192(17) 0.0114(15) -0.0008(13) 0.0049(13) 0.0024(14) C2 0.025(2) 0.0242(19) 0.0219(19) 0.0009(15) 0.0093(15) 0.0020(16) C10 0.028(2) 0.0260(19) 0.0114(15) -0.0009(14) 0.0088(14) 0.0004(16) C1 0.030(2) 0.026(2) 0.0138(16) -0.0004(14) 0.0075(15) -0.0022(17) C8 0.0193(18) 0.0213(18) 0.0168(17) 0.0008(14) 0.0081(14) 0.0015(14) C7 0.0208(18) 0.0197(17) 0.0150(16) -0.0003(13) 0.0052(14) 0.0009(14) C15 0.0187(18) 0.0223(18) 0.0181(17) -0.0014(14) 0.0046(14) -0.0028(14) C22 0.0179(17) 0.0183(17) 0.0167(16) -0.0008(13) 0.0037(14) -0.0010(14) C3 0.023(2) 0.029(2) 0.0202(18) -0.0032(15) 0.0096(15) 0.0009(16) C4 0.0244(19) 0.0229(18) 0.0153(16) -0.0015(14) 0.0054(14) -0.0024(15) C14 0.0226(19) 0.0229(19) 0.0178(17) -0.0051(14) 0.0038(14) -0.0007(15) C21 0.0237(19) 0.0240(19) 0.0153(16) 0.0003(14) 0.0058(14) -0.0017(15) C13 0.026(2) 0.0243(19) 0.0141(16) -0.0048(14) 0.0052(14) -0.0014(15) C17 0.0202(18) 0.0190(17) 0.0174(17) -0.0001(14) 0.0052(14) -0.0002(14) C20 0.024(2) 0.025(2) 0.0222(19) 0.0039(15) 0.0061(16) -0.0022(16) C18 0.027(2) 0.0219(19) 0.0204(18) -0.0021(15) 0.0077(16) 0.0004(15) C16 0.0220(19) 0.0201(18) 0.0173(17) 0.0003(14) 0.0066(14) 0.0017(15) C5 0.025(2) 0.025(2) 0.0182(18) -0.0034(15) 0.0039(15) -0.0043(16) C6 0.0230(19) 0.0237(19) 0.0190(18) -0.0004(15) 0.0072(15) -0.0038(15) C19 0.030(2) 0.0210(19) 0.0247(19) 0.0006(15) 0.0054(17) -0.0019(16) C23 0.046(3) 0.033(2) 0.031(2) -0.0017(19) 0.014(2) -0.018(2) N1A 0.027(2) 0.057(3) 0.069(4) 0.013(3) 0.015(2) 0.004(2) O1A 0.0330(15) 0.0423(17) 0.061(2) 0.0028(14) 0.0221(14) -0.0038(13) C1A 0.027(2) 0.057(3) 0.069(4) 0.013(3) 0.015(2) 0.004(2) C4A 0.044(5) 0.065(6) 0.115(9) -0.010(6) 0.036(6) -0.003(4) C3A 0.083(8) 0.098(9) 0.103(9) -0.001(7) 0.022(7) -0.061(7) O1B 0.0316(16) 0.0325(16) 0.0314(16) -0.0053(13) 0.0083(13) 0.0062(13) 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' N N 0.0061 0.0033 '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' Re Re -1.0185 7.2310 '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 O4 Re1 N2 81.46(11) . . ? O4 Re1 N1 79.48(11) . . ? N1 Re1 N2 76.15(12) . . ? C2 Re1 O4 96.88(14) . . ? C2 Re1 N2 98.82(15) . . ? C2 Re1 N1 174.12(15) . . ? C2 Re1 C3 90.32(17) . . ? C1 Re1 O4 172.19(14) . . ? C1 Re1 N2 91.07(15) . . ? C1 Re1 N1 96.58(14) . . ? C1 Re1 C2 86.47(16) . . ? C1 Re1 C3 87.86(18) . . ? C3 Re1 O4 99.14(14) . . ? C3 Re1 N2 170.72(14) . . ? C3 Re1 N1 94.81(14) . . ? C22 O4 Re1 122.2(2) . . ? C9 N2 Re1 114.2(2) . . ? C4 N2 Re1 127.1(2) . . ? C4 N2 C9 118.5(3) . . ? C11 N1 Re1 114.5(2) . . ? C15 N1 Re1 127.1(3) . . ? C15 N1 C11 118.3(3) . . ? C11 C12 C10 119.3(3) . . ? C11 C12 C13 117.8(3) . . ? C13 C12 C10 123.0(3) . . ? N1 C11 C12 122.5(3) . . ? N1 C11 C9 117.9(3) . . ? C12 C11 C9 119.6(3) . . ? C16 N3 C8 118.0(3) . 3_666 ? N2 C9 C11 117.0(3) . . ? N2 C9 C7 122.6(3) . . ? C7 C9 C11 120.3(3) . . ? O2 C2 Re1 177.3(4) . . ? C12 C10 H10 119.2 . . ? C8 C10 C12 121.5(3) . . ? C8 C10 H10 119.2 . . ? O1 C1 Re1 179.0(3) . . ? N3 C8 C7 116.5(3) 3_666 . ? C10 C8 N3 123.9(3) . 3_666 ? C10 C8 C7 119.6(3) . . ? C9 C7 C8 119.6(3) . . ? C9 C7 C6 117.6(3) . . ? C6 C7 C8 122.8(3) . . ? N1 C15 H15 118.6 . . ? N1 C15 C14 122.7(4) . . ? C14 C15 H15 118.6 . . ? O4 C22 C21 121.2(3) . . ? O4 C22 C17 120.6(3) . . ? C21 C22 C17 118.2(3) . . ? O3 C3 Re1 175.1(4) . . ? N2 C4 H4 118.9 . . ? N2 C4 C5 122.2(3) . . ? C5 C4 H4 118.9 . . ? C15 C14 H14 120.1 . . ? C13 C14 C15 119.9(4) . . ? C13 C14 H14 120.1 . . ? C22 C21 H21 119.1 . . ? C20 C21 C22 121.8(3) . . ? C20 C21 H21 119.1 . . ? C12 C13 H13 120.6 . . ? C14 C13 C12 118.8(3) . . ? C14 C13 H13 120.6 . . ? C22 C17 C16 119.6(3) . . ? C18 C17 C22 119.3(3) . . ? C18 C17 C16 121.1(3) . . ? C21 C20 C19 119.6(4) . . ? C21 C20 C23 120.9(4) . . ? C19 C20 C23 119.5(4) . . ? C17 C18 H18 119.3 . . ? C19 C18 C17 121.5(4) . . ? C19 C18 H18 119.3 . . ? N3 C16 C17 123.2(4) . . ? N3 C16 H16 118.4 . . ? C17 C16 H16 118.4 . . ? C4 C5 H5 120.1 . . ? C6 C5 C4 119.8(4) . . ? C6 C5 H5 120.1 . . ? C7 C6 H6 120.4 . . ? C5 C6 C7 119.2(4) . . ? C5 C6 H6 120.4 . . ? C20 C19 H19 120.2 . . ? C18 C19 C20 119.7(4) . . ? C18 C19 H19 120.2 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C1A N1A C4A 111.5(8) . . ? C1A N1A C3A 122.7(9) . . ? C4A N1A C3A 125.2(9) . . ? N1A C1A H1A 116.6 . . ? O1A C1A N1A 126.7(9) . . ? O1A C1A H1A 116.6 . . ? N1A C4A H4AA 109.5 . . ? N1A C4A H4AB 109.5 . . ? N1A C4A H4AC 109.5 . . ? H4AA C4A H4AB 109.5 . . ? H4AA C4A H4AC 109.5 . . ? H4AB C4A H4AC 109.5 . . ? N1A C3A H3AA 109.5 . . ? N1A C3A H3AB 109.5 . . ? N1A C3A H3AC 109.5 . . ? H3AA C3A H3AB 109.5 . . ? H3AA C3A H3AC 109.5 . . ? H3AB C3A H3AC 109.5 . . ? H1BA O1B H1BB 109.3 . . ? 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 2.138(3) . ? Re1 N2 2.181(3) . ? Re1 N1 2.172(3) . ? Re1 C2 1.915(4) . ? Re1 C1 1.902(4) . ? Re1 C3 1.922(4) . ? O4 C22 1.326(4) . ? N2 C9 1.370(4) . ? N2 C4 1.326(5) . ? O1 C1 1.155(5) . ? N1 C11 1.360(5) . ? N1 C15 1.330(5) . ? O2 C2 1.152(5) . ? O3 C3 1.150(5) . ? C12 C11 1.405(5) . ? C12 C10 1.435(5) . ? C12 C13 1.413(5) . ? C11 C9 1.425(5) . ? N3 C8 1.399(5) 3_666 ? N3 C16 1.289(5) . ? C9 C7 1.400(5) . ? C10 H10 0.9500 . ? C10 C8 1.363(5) . ? C8 C7 1.448(5) . ? C7 C6 1.400(5) . ? C15 H15 0.9500 . ? C15 C14 1.393(5) . ? C22 C21 1.405(5) . ? C22 C17 1.424(5) . ? C4 H4 0.9500 . ? C4 C5 1.394(5) . ? C14 H14 0.9500 . ? C14 C13 1.370(5) . ? C21 H21 0.9500 . ? C21 C20 1.383(6) . ? C13 H13 0.9500 . ? C17 C18 1.401(5) . ? C17 C16 1.436(5) . ? C20 C19 1.405(6) . ? C20 C23 1.502(6) . ? C18 H18 0.9500 . ? C18 C19 1.380(6) . ? C16 H16 0.9500 . ? C5 H5 0.9500 . ? C5 C6 1.380(5) . ? C6 H6 0.9500 . ? C19 H19 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? N1A C1A 1.329(10) . ? N1A C4A 1.358(12) . ? N1A C3A 1.377(11) . ? O1A C1A 1.259(9) . ? C1A H1A 0.9500 . ? C4A H4AA 0.9800 . ? C4A H4AB 0.9800 . ? C4A H4AC 0.9800 . ? C3A H3AA 0.9800 . ? C3A H3AB 0.9800 . ? C3A H3AC 0.9800 . ? O1B H1BA 0.8699 . ? O1B H1BB 0.8703 . ? 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 O4 C22 C21 -62.2(4) . . . . ? Re1 O4 C22 C17 117.6(3) . . . . ? Re1 N2 C9 C11 -4.4(4) . . . . ? Re1 N2 C9 C7 176.6(3) . . . . ? Re1 N2 C4 C5 -174.9(3) . . . . ? Re1 N1 C11 C12 -179.4(3) . . . . ? Re1 N1 C11 C9 1.1(4) . . . . ? Re1 N1 C15 C14 -177.9(3) . . . . ? O4 C22 C21 C20 178.1(4) . . . . ? O4 C22 C17 C18 -179.5(4) . . . . ? O4 C22 C17 C16 -2.1(6) . . . . ? N2 C9 C7 C8 180.0(3) . . . . ? N2 C9 C7 C6 -1.2(6) . . . . ? N2 C4 C5 C6 -1.0(6) . . . . ? N1 C11 C9 N2 2.3(5) . . . . ? N1 C11 C9 C7 -178.7(3) . . . . ? N1 C15 C14 C13 -1.6(6) . . . . ? C12 C11 C9 N2 -177.3(3) . . . . ? C12 C11 C9 C7 1.8(6) . . . . ? C12 C10 C8 N3 -176.9(4) . . . 3_666 ? C12 C10 C8 C7 -0.7(6) . . . . ? C11 N1 C15 C14 -0.7(6) . . . . ? C11 C12 C10 C8 3.5(6) . . . . ? C11 C12 C13 C14 0.8(6) . . . . ? C11 C9 C7 C8 1.0(5) . . . . ? C11 C9 C7 C6 179.8(4) . . . . ? N3 C8 C7 C9 174.9(3) 3_666 . . . ? N3 C8 C7 C6 -3.8(6) 3_666 . . . ? C9 N2 C4 C5 1.1(6) . . . . ? C9 C7 C6 C5 1.3(6) . . . . ? C10 C12 C11 N1 176.5(3) . . . . ? C10 C12 C11 C9 -4.0(6) . . . . ? C10 C12 C13 C14 -178.9(4) . . . . ? C10 C8 C7 C9 -1.5(6) . . . . ? C10 C8 C7 C6 179.8(4) . . . . ? C8 N3 C16 C17 -177.4(4) 3_666 . . . ? C8 C7 C6 C5 180.0(4) . . . . ? C15 N1 C11 C12 3.1(6) . . . . ? C15 N1 C11 C9 -176.4(3) . . . . ? C15 C14 C13 C12 1.4(6) . . . . ? C22 C21 C20 C19 1.0(6) . . . . ? C22 C21 C20 C23 -179.6(4) . . . . ? C22 C17 C18 C19 1.7(6) . . . . ? C22 C17 C16 N3 -176.7(4) . . . . ? C4 N2 C9 C11 179.1(3) . . . . ? C4 N2 C9 C7 0.1(6) . . . . ? C4 C5 C6 C7 -0.2(6) . . . . ? C21 C22 C17 C18 0.4(6) . . . . ? C21 C22 C17 C16 177.7(3) . . . . ? C21 C20 C19 C18 1.0(6) . . . . ? C13 C12 C11 N1 -3.1(6) . . . . ? C13 C12 C11 C9 176.4(3) . . . . ? C13 C12 C10 C8 -176.9(4) . . . . ? C17 C22 C21 C20 -1.7(6) . . . . ? C17 C18 C19 C20 -2.4(6) . . . . ? C18 C17 C16 N3 0.6(6) . . . . ? C16 C17 C18 C19 -175.6(4) . . . . ? C23 C20 C19 C18 -178.3(4) . . . . ? C4A N1A C1A O1A 5.8(12) . . . . ? C3A N1A C1A O1A 177.5(10) . . . . ?