Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Roger Alberto' _publ_contact_author_address ; Institute of Inorganic Chemistry University of Zurich Winterthurerstrasse 190 Zürich 8057 SWITZERLAND ; _publ_contact_author_email ARIEL@ACI.UNIZH.CH _publ_section_title ; A new [2+1] mixed ligand concept based on [99(m)Tc(OH2)3(CO)3]+: A basic study ; loop_ _publ_author_name 'Roger Alberto' 'Monika Kundig' 'Stefan Mundwiler' 'Kirstin Ortner' data_5 _database_code_depnum_ccdc_archive 'CCDC 228229' _audit_creation_method SHELXL-97 _chemical_name_systematic 'Re(I)(2,4-Pyridinedicarboxylicacid)(water)(CO)3 x 2 H2O' _chemical_name_common 'Re(i)(2,4-Pyridinedicarboxylicacid)(water)(CO)3 x 2 H2O' _chemical_melting_point ? _chemical_formula_moiety 'C10 H6 N O8 Re x 2(H2 O)' _chemical_formula_sum 'C10 H10 N O10 Re' _chemical_formula_weight 490.39 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.3056(7) _cell_length_b 23.3953(10) _cell_length_c 24.7252(16) _cell_angle_alpha 90.00 _cell_angle_beta 98.380(8) _cell_angle_gamma 90.00 _cell_volume 5897.7(6) _cell_formula_units_Z 16 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3712 _exptl_absorpt_coefficient_mu 8.292 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.2409 _exptl_absorpt_correction_T_max 0.5945 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method '/f oscillation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 50-200 _diffrn_standards_interval_count image _diffrn_standards_interval_time 5.7 _diffrn_standards_decay_% 0 _diffrn_reflns_number 45230 _diffrn_reflns_av_R_equivalents 0.0674 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 28.02 _reflns_number_total 14181 _reflns_number_gt 9218 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS, Stoe, 1999)' _computing_cell_refinement 'IPDS, Stoe, 1999)' _computing_data_reduction 'X-Red, Stoe, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Zortep (Zsolnai, 1994), Platon (Spek, 1993)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14181 _refine_ls_number_parameters 835 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0780 _refine_ls_wR_factor_gt 0.0722 _refine_ls_goodness_of_fit_ref 0.847 _refine_ls_restrained_S_all 0.847 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.18479(2) 0.337395(10) -0.080768(9) 0.02075(6) Uani 1 1 d . . . Re2 Re -0.20217(2) 0.170846(10) 0.059594(9) 0.02065(6) Uani 1 1 d . . . Re3 Re 0.29108(2) 0.579545(10) 0.066568(9) 0.01993(6) Uani 1 1 d . . . Re4 Re 0.32297(2) 0.086663(10) 0.073672(9) 0.02138(6) Uani 1 1 d . . . C1 C -0.0510(6) 0.2951(3) -0.1555(2) 0.0214(12) Uani 1 1 d . . . C2 C 0.0321(6) 0.2417(3) -0.1434(2) 0.0191(11) Uani 1 1 d . . . C3 C -0.0079(7) 0.1881(3) -0.1637(2) 0.0244(13) Uani 1 1 d . . . H3 H -0.0887 0.1836 -0.1872 0.029 Uiso 1 1 calc R . . C4 C 0.0727(8) 0.1412(3) -0.1488(3) 0.0287(15) Uani 1 1 d . . . C5 C 0.0288(7) 0.0815(3) -0.1684(3) 0.0291(15) Uani 1 1 d . . . C6 C 0.1921(7) 0.1500(3) -0.1149(2) 0.0271(14) Uani 1 1 d . . . H6 H 0.2493 0.1187 -0.1047 0.033 Uiso 1 1 calc R . . C7 C 0.2258(7) 0.2044(3) -0.0965(2) 0.0242(13) Uani 1 1 d . . . H7 H 0.3074 0.2101 -0.0737 0.029 Uiso 1 1 calc R . . C8 C 0.3585(6) 0.3246(3) -0.0414(3) 0.0266(13) Uani 1 1 d . . . C9 C 0.2073(7) 0.4175(3) -0.0632(3) 0.0291(14) Uani 1 1 d . . . C10 C 0.1175(7) 0.3246(3) -0.0132(2) 0.0273(14) Uani 1 1 d . . . C21 C 0.0362(6) 0.2025(3) 0.1387(2) 0.0197(11) Uani 1 1 d . . . C22 C -0.0349(6) 0.2595(3) 0.1272(2) 0.0221(12) Uani 1 1 d . . . C23 C 0.0085(7) 0.3095(3) 0.1534(2) 0.0259(14) Uani 1 1 d . . . H23 H 0.0892 0.3103 0.1775 0.031 Uiso 1 1 calc R . . C24 C -0.0674(8) 0.3590(3) 0.1441(2) 0.0279(15) Uani 1 1 d . . . C25 C -0.0223(8) 0.4138(3) 0.1730(3) 0.0308(15) Uani 1 1 d . . . C26 C -0.1854(8) 0.3554(3) 0.1090(2) 0.0271(14) Uani 1 1 d . . . H26 H -0.2399 0.3881 0.1025 0.032 Uiso 1 1 calc R . . C27 C -0.2238(7) 0.3040(3) 0.0834(2) 0.0260(14) Uani 1 1 d . . . H27 H -0.3043 0.3022 0.0593 0.031 Uiso 1 1 calc R . . C28 C -0.3616(7) 0.1863(3) 0.0117(3) 0.0274(13) Uani 1 1 d . . . C29 C -0.2331(6) 0.0912(3) 0.0437(2) 0.0267(13) Uani 1 1 d . . . C30 C -0.1121(7) 0.1778(3) -0.0025(2) 0.0257(14) Uani 1 1 d . . . C31 C 0.5291(6) 0.5471(3) 0.1456(2) 0.0210(12) Uani 1 1 d . . . C32 C 0.4603(7) 0.4907(3) 0.1324(2) 0.0218(12) Uani 1 1 d . . . C33 C 0.5058(7) 0.4396(3) 0.1575(2) 0.0226(13) Uani 1 1 d . . . H33 H 0.5860 0.4385 0.1818 0.027 Uiso 1 1 calc R . . C34 C 0.4314(7) 0.3901(3) 0.1460(2) 0.0228(13) Uani 1 1 d . . . C35 C 0.4815(8) 0.3349(3) 0.1727(3) 0.0310(15) Uani 1 1 d . . . C36 C 0.3161(7) 0.3933(3) 0.1091(3) 0.0281(14) Uani 1 1 d . . . H36 H 0.2642 0.3601 0.1003 0.034 Uiso 1 1 calc R . . C37 C 0.2781(7) 0.4455(3) 0.0855(2) 0.0262(14) Uani 1 1 d . . . H37 H 0.1995 0.4473 0.0602 0.031 Uiso 1 1 calc R . . C38 C 0.1294(7) 0.5649(3) 0.0186(3) 0.0286(14) Uani 1 1 d . . . C39 C 0.2577(7) 0.6605(3) 0.0532(2) 0.0257(13) Uani 1 1 d . . . C40 C 0.3809(7) 0.5727(3) 0.0041(2) 0.0248(13) Uani 1 1 d . . . C41 C 0.5575(7) 0.0438(3) 0.1483(2) 0.0232(13) Uani 1 1 d . . . C42 C 0.4729(7) -0.0087(3) 0.1376(2) 0.0227(13) Uani 1 1 d . . . C43 C 0.5111(7) -0.0622(3) 0.1599(2) 0.0236(13) Uani 1 1 d . . . H43 H 0.5928 -0.0668 0.1828 0.028 Uiso 1 1 calc R . . C44 C 0.4274(7) -0.1081(3) 0.1477(2) 0.0256(14) Uani 1 1 d . . . C45 C 0.4696(8) -0.1664(3) 0.1692(3) 0.0313(15) Uani 1 1 d . . . C46 C 0.3071(8) -0.0994(3) 0.1148(3) 0.0289(15) Uani 1 1 d . . . H46 H 0.2472 -0.1301 0.1066 0.035 Uiso 1 1 calc R . . C47 C 0.2768(7) -0.0453(3) 0.0945(2) 0.0262(14) Uani 1 1 d . . . H47 H 0.1948 -0.0397 0.0721 0.031 Uiso 1 1 calc R . . C48 C 0.1502(7) 0.0744(3) 0.0343(3) 0.0316(14) Uani 1 1 d . . . C49 C 0.3035(7) 0.1670(3) 0.0545(3) 0.0307(14) Uani 1 1 d . . . C50 C 0.3904(7) 0.0729(3) 0.0066(2) 0.0257(14) Uani 1 1 d . . . N1 N 0.1472(5) 0.2498(2) -0.10972(19) 0.0200(10) Uani 1 1 d . . . N2 N -0.1493(5) 0.2566(2) 0.09215(18) 0.0215(10) Uani 1 1 d . . . N3 N 0.3474(5) 0.4937(2) 0.09683(19) 0.0206(10) Uani 1 1 d . . . N4 N 0.3572(5) -0.0005(2) 0.10479(19) 0.0202(10) Uani 1 1 d . . . O1 O -0.0065(4) 0.34021(19) -0.13009(16) 0.0247(9) Uani 1 1 d . . . O2 O -0.1553(5) 0.2924(2) -0.18713(18) 0.0341(11) Uani 1 1 d . . . O3 O -0.0773(6) 0.0745(2) -0.1958(2) 0.0412(13) Uani 1 1 d . . . O4 O 0.1140(8) 0.0431(3) -0.1506(3) 0.058(2) Uani 1 1 d . . . H4 H 0.097(8) 0.015(4) -0.161(3) 0.03(2) Uiso 1 1 d . . . O5 O 0.2348(5) 0.3519(2) -0.16309(19) 0.0303(10) Uani 1 1 d . . . H5A H 0.288(9) 0.374(4) -0.164(3) 0.04(2) Uiso 1 1 d . . . H5B H 0.237(10) 0.326(5) -0.181(4) 0.05(3) Uiso 1 1 d . . . O6 O 0.4587(5) 0.3169(2) -0.0172(2) 0.0424(13) Uani 1 1 d . . . O7 O 0.2239(7) 0.4656(2) -0.0526(2) 0.0471(15) Uani 1 1 d . . . O8 O 0.0767(6) 0.3158(2) 0.02660(19) 0.0370(13) Uani 1 1 d . . . O21 O -0.0223(4) 0.15838(19) 0.11553(17) 0.0250(9) Uani 1 1 d . . . O22 O 0.1428(5) 0.2007(2) 0.16892(18) 0.0307(10) Uani 1 1 d . . . O23 O 0.0851(6) 0.4159(2) 0.2015(2) 0.0442(14) Uani 1 1 d . . . O24 O -0.1071(7) 0.4549(2) 0.1640(2) 0.0417(14) Uani 1 1 d . . . H24 H -0.086(11) 0.485(5) 0.176(4) 0.07(3) Uiso 1 1 d . . . O25 O -0.2832(5) 0.1650(2) 0.13602(19) 0.0325(10) Uani 1 1 d . . . H25A H -0.366(10) 0.149(4) 0.137(3) 0.05(2) Uiso 1 1 d . . . H25B H -0.272(12) 0.191(5) 0.163(5) 0.08(4) Uiso 1 1 d . . . O26 O -0.4553(5) 0.1937(2) -0.0194(2) 0.0420(12) Uani 1 1 d . . . O27 O -0.2504(6) 0.0429(2) 0.0357(2) 0.0420(13) Uani 1 1 d . . . O28 O -0.0565(6) 0.1830(2) -0.03928(19) 0.0397(13) Uani 1 1 d . . . O31 O 0.4705(4) 0.59168(19) 0.12301(16) 0.0252(9) Uani 1 1 d . . . O32 O 0.6349(5) 0.5498(2) 0.17675(18) 0.0286(10) Uani 1 1 d . . . O33 O 0.5857(6) 0.3318(2) 0.2017(2) 0.0404(13) Uani 1 1 d . . . O34 O 0.3964(7) 0.2926(2) 0.1611(2) 0.0464(15) Uani 1 1 d . . . H34 H 0.4261 0.2627 0.1773 0.070 Uiso 1 1 calc R . . O35 O 0.2104(6) 0.5839(2) 0.1430(2) 0.0347(11) Uani 1 1 d . . . H35A H 0.147(10) 0.603(4) 0.140(4) 0.05(3) Uiso 1 1 d . . . H35B H 0.225(8) 0.563(4) 0.163(3) 0.02(2) Uiso 1 1 d . . . O36 O 0.0356(5) 0.5588(2) -0.0121(2) 0.0410(13) Uani 1 1 d . . . O37 O 0.2378(6) 0.7085(2) 0.0472(2) 0.0426(13) Uani 1 1 d . . . O38 O 0.4345(6) 0.5683(3) -0.03307(19) 0.0403(13) Uani 1 1 d . . . O41 O 0.5148(4) 0.08965(19) 0.12293(16) 0.0241(9) Uani 1 1 d . . . O42 O 0.6628(5) 0.0412(2) 0.17994(19) 0.0333(11) Uani 1 1 d . . . O43 O 0.5769(6) -0.1754(2) 0.1946(2) 0.0418(13) Uani 1 1 d . . . O44 O 0.3784(7) -0.2058(2) 0.1555(2) 0.0471(15) Uani 1 1 d . . . H44 H 0.3754 -0.2278 0.1822 0.071 Uiso 1 1 calc R . . O45 O 0.2727(5) 0.1026(2) 0.15578(19) 0.0276(10) Uani 1 1 d . . . H45A H 0.214(10) 0.132(5) 0.157(4) 0.06(3) Uiso 1 1 d . . . H45B H 0.275(10) 0.084(4) 0.177(4) 0.05(3) Uiso 1 1 d . . . O46 O 0.0493(6) 0.0648(3) 0.0090(3) 0.0489(14) Uani 1 1 d . . . O47 O 0.2909(7) 0.2143(2) 0.0430(2) 0.0498(15) Uani 1 1 d . . . O48 O 0.4316(6) 0.0650(2) -0.03352(19) 0.0399(13) Uani 1 1 d . . . O50 O 0.2284(5) -0.2464(2) -0.20862(17) 0.0336(11) Uani 1 1 d . . . O51 O 0.2617(6) 0.0137(2) 0.21905(18) 0.0355(12) Uani 1 1 d . . . O52 O 0.4753(5) 0.19281(19) 0.20024(19) 0.0347(11) Uani 1 1 d . . . O53 O -0.0328(5) -0.0551(2) -0.29418(19) 0.0359(11) Uani 1 1 d . . . O54 O -0.2424(6) -0.2372(2) -0.27422(18) 0.0358(11) Uani 1 1 d . . . O55 O 0.4176(5) -0.18570(19) -0.31146(18) 0.0310(10) Uani 1 1 d . . . O56 O 0.2689(5) -0.0025(2) -0.28502(18) 0.0347(11) Uani 1 1 d . . . O57 O 0.0748(5) -0.06564(19) -0.18249(19) 0.0322(10) 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 0.02246(12) 0.01609(11) 0.02363(11) -0.00233(8) 0.00315(9) -0.00189(9) Re2 0.02195(12) 0.01706(11) 0.02311(11) -0.00172(8) 0.00387(9) -0.00159(9) Re3 0.02036(12) 0.01642(11) 0.02307(11) 0.00195(8) 0.00337(9) 0.00170(9) Re4 0.02376(12) 0.01654(11) 0.02389(11) 0.00178(8) 0.00368(9) 0.00223(9) C1 0.019(3) 0.022(3) 0.024(3) -0.001(2) 0.004(2) 0.002(2) C2 0.018(3) 0.019(3) 0.020(2) 0.001(2) 0.002(2) 0.002(2) C3 0.025(3) 0.022(3) 0.026(3) -0.003(2) 0.003(2) -0.003(3) C4 0.032(4) 0.025(4) 0.030(3) 0.000(2) 0.005(3) 0.000(3) C5 0.033(4) 0.019(3) 0.036(3) -0.005(2) 0.008(3) -0.004(3) C6 0.036(4) 0.013(3) 0.031(3) -0.002(2) 0.003(3) 0.004(3) C7 0.021(3) 0.019(3) 0.032(3) 0.000(2) 0.001(2) 0.002(2) C8 0.024(3) 0.022(3) 0.036(3) -0.007(2) 0.009(3) -0.007(2) C9 0.033(3) 0.024(3) 0.031(3) -0.001(2) 0.003(3) 0.001(3) C10 0.030(4) 0.027(3) 0.025(3) -0.002(2) 0.002(3) 0.000(3) C21 0.019(3) 0.016(3) 0.025(3) -0.002(2) 0.006(2) 0.002(2) C22 0.021(3) 0.022(3) 0.024(3) 0.000(2) 0.004(2) 0.000(2) C23 0.028(4) 0.022(3) 0.028(3) -0.007(2) 0.005(3) -0.003(3) C24 0.038(4) 0.019(3) 0.027(3) 0.000(2) 0.007(3) 0.002(3) C25 0.042(4) 0.019(3) 0.032(3) -0.001(2) 0.011(3) -0.005(3) C26 0.034(4) 0.016(3) 0.031(3) -0.001(2) 0.002(3) 0.008(3) C27 0.028(3) 0.022(3) 0.025(3) 0.001(2) -0.005(3) 0.002(3) C28 0.029(3) 0.018(3) 0.036(3) 0.001(2) 0.006(3) 0.004(2) C29 0.029(3) 0.023(3) 0.027(3) -0.003(2) 0.002(2) -0.003(3) C30 0.029(3) 0.018(3) 0.029(3) 0.000(2) 0.000(3) 0.003(3) C31 0.020(3) 0.020(3) 0.025(3) 0.004(2) 0.007(2) -0.002(2) C32 0.025(3) 0.019(3) 0.021(3) -0.004(2) 0.002(2) 0.002(2) C33 0.018(3) 0.024(3) 0.025(3) 0.002(2) 0.001(2) 0.001(2) C34 0.025(3) 0.018(3) 0.025(3) -0.002(2) 0.002(2) 0.000(3) C35 0.038(4) 0.023(4) 0.032(3) 0.004(3) 0.006(3) 0.000(3) C36 0.031(4) 0.017(3) 0.036(3) 0.001(2) 0.005(3) -0.004(3) C37 0.027(3) 0.025(3) 0.026(3) 0.003(2) 0.005(3) -0.002(3) C38 0.027(3) 0.020(3) 0.039(3) 0.007(2) 0.009(3) 0.001(3) C39 0.031(3) 0.021(3) 0.026(3) 0.003(2) 0.006(2) 0.003(3) C40 0.028(3) 0.019(3) 0.026(3) -0.003(2) 0.000(3) 0.002(3) C41 0.024(3) 0.020(3) 0.026(3) 0.000(2) 0.004(2) 0.002(2) C42 0.026(3) 0.022(3) 0.021(3) -0.004(2) 0.005(2) 0.001(3) C43 0.023(3) 0.022(3) 0.026(3) 0.005(2) 0.005(2) 0.003(3) C44 0.027(4) 0.020(3) 0.030(3) 0.002(2) 0.004(3) 0.001(3) C45 0.037(4) 0.024(4) 0.034(3) 0.002(3) 0.008(3) 0.001(3) C46 0.035(4) 0.020(3) 0.031(3) -0.005(2) 0.005(3) -0.006(3) C47 0.029(3) 0.026(3) 0.023(3) 0.001(2) 0.001(2) -0.002(3) C48 0.030(3) 0.032(4) 0.032(3) 0.005(3) 0.003(3) -0.001(3) C49 0.034(4) 0.022(3) 0.036(3) 0.001(3) 0.004(3) 0.000(3) C50 0.026(3) 0.024(3) 0.028(3) -0.004(2) 0.005(3) 0.003(3) N1 0.021(3) 0.013(2) 0.026(2) 0.0010(18) 0.0020(19) 0.0008(19) N2 0.028(3) 0.017(2) 0.019(2) 0.0004(17) 0.004(2) -0.001(2) N3 0.021(3) 0.016(2) 0.025(2) 0.0001(17) 0.004(2) 0.000(2) N4 0.022(3) 0.013(2) 0.025(2) -0.0007(17) 0.001(2) 0.002(2) O1 0.025(2) 0.020(2) 0.028(2) -0.0006(16) -0.0022(17) 0.0034(17) O2 0.034(3) 0.033(3) 0.032(2) -0.0073(18) -0.008(2) 0.007(2) O3 0.031(3) 0.030(3) 0.062(3) -0.010(2) 0.002(2) -0.008(2) O4 0.061(4) 0.017(3) 0.087(5) -0.004(3) -0.023(3) -0.001(3) O5 0.037(3) 0.029(3) 0.028(2) -0.0063(19) 0.012(2) -0.011(2) O6 0.027(3) 0.033(3) 0.063(3) 0.001(2) -0.009(2) 0.000(2) O7 0.069(4) 0.023(3) 0.051(3) -0.010(2) 0.015(3) -0.012(3) O8 0.043(3) 0.039(3) 0.031(2) 0.0012(19) 0.014(2) -0.002(3) O21 0.023(2) 0.020(2) 0.030(2) 0.0010(16) -0.0039(17) 0.0022(17) O22 0.028(2) 0.024(2) 0.037(2) -0.0071(18) -0.005(2) 0.0006(19) O23 0.037(3) 0.027(3) 0.065(3) -0.012(2) -0.003(3) 0.000(2) O24 0.053(4) 0.019(3) 0.048(3) -0.008(2) -0.007(3) 0.004(3) O25 0.034(3) 0.037(3) 0.031(2) -0.007(2) 0.019(2) -0.007(2) O26 0.030(3) 0.039(3) 0.053(3) 0.000(2) -0.006(2) 0.002(2) O27 0.052(3) 0.025(3) 0.048(3) -0.004(2) 0.002(3) -0.010(2) O28 0.045(3) 0.042(3) 0.035(2) 0.003(2) 0.018(2) -0.003(3) O31 0.029(2) 0.018(2) 0.027(2) -0.0023(15) -0.0042(17) 0.0005(18) O32 0.027(2) 0.025(2) 0.031(2) 0.0025(17) -0.0044(19) -0.0036(19) O33 0.037(3) 0.026(3) 0.054(3) 0.009(2) -0.006(2) 0.001(2) O34 0.056(4) 0.018(3) 0.060(3) 0.008(2) -0.009(3) -0.005(3) O35 0.042(3) 0.033(3) 0.034(3) 0.012(2) 0.019(2) 0.016(2) O36 0.028(3) 0.033(3) 0.056(3) 0.000(2) -0.013(2) -0.001(2) O37 0.060(4) 0.023(3) 0.044(3) 0.008(2) 0.006(3) 0.008(2) O38 0.048(3) 0.043(3) 0.033(2) -0.003(2) 0.017(2) 0.002(3) O41 0.024(2) 0.022(2) 0.0255(19) 0.0007(15) -0.0004(16) 0.0012(18) O42 0.031(3) 0.028(3) 0.038(2) 0.0090(18) -0.005(2) -0.002(2) O43 0.038(3) 0.023(3) 0.063(3) 0.010(2) 0.004(3) 0.004(2) O44 0.055(4) 0.024(3) 0.057(3) 0.005(2) -0.007(3) -0.006(3) O45 0.038(3) 0.024(2) 0.022(2) 0.0023(18) 0.0117(19) 0.008(2) O46 0.033(3) 0.039(3) 0.070(4) -0.004(3) -0.008(3) 0.004(2) O47 0.068(4) 0.026(3) 0.055(3) 0.010(2) 0.010(3) 0.007(3) O48 0.054(4) 0.036(3) 0.033(2) 0.000(2) 0.018(2) -0.001(3) O50 0.039(3) 0.033(3) 0.029(2) -0.0007(18) 0.006(2) -0.001(2) O51 0.045(3) 0.031(3) 0.031(2) -0.0047(18) 0.010(2) -0.011(2) O52 0.044(3) 0.020(2) 0.040(3) 0.0002(18) 0.007(2) -0.002(2) O53 0.046(3) 0.023(2) 0.039(3) 0.0015(18) 0.005(2) 0.001(2) O54 0.047(3) 0.031(3) 0.030(2) 0.0029(18) 0.004(2) -0.010(2) O55 0.037(3) 0.019(2) 0.035(2) 0.0028(17) 0.001(2) -0.0040(19) O56 0.041(3) 0.034(3) 0.029(2) -0.0025(18) 0.007(2) 0.002(2) O57 0.033(3) 0.022(2) 0.040(2) 0.0029(18) 0.000(2) 0.0015(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C10 1.924(7) . ? Re1 C9 1.930(7) . ? Re1 C8 1.931(7) . ? Re1 O1 2.163(4) . ? Re1 N1 2.186(5) . ? Re1 O5 2.198(5) . ? Re2 C30 1.914(7) . ? Re2 C28 1.915(6) . ? Re2 C29 1.921(6) . ? Re2 O21 2.165(4) . ? Re2 O25 2.178(4) . ? Re2 N2 2.200(5) . ? Re3 C40 1.918(7) . ? Re3 C38 1.930(7) . ? Re3 C39 1.944(6) . ? Re3 O31 2.166(4) . ? Re3 O35 2.175(5) . ? Re3 N3 2.191(5) . ? Re4 C50 1.916(6) . ? Re4 C48 1.922(7) . ? Re4 C49 1.942(7) . ? Re4 O41 2.167(4) . ? Re4 N4 2.190(5) . ? Re4 O45 2.199(4) . ? C1 O2 1.236(8) . ? C1 O1 1.279(7) . ? C1 C2 1.519(8) . ? C2 N1 1.360(8) . ? C2 C3 1.389(9) . ? C3 C4 1.393(10) . ? C4 C6 1.399(10) . ? C4 C5 1.526(10) . ? C5 O3 1.210(9) . ? C5 O4 1.286(10) . ? C6 C7 1.380(9) . ? C7 N1 1.347(8) . ? C8 O6 1.131(8) . ? C9 O7 1.162(8) . ? C10 O8 1.143(8) . ? C21 O22 1.236(8) . ? C21 O21 1.287(7) . ? C21 C22 1.528(8) . ? C22 N2 1.359(8) . ? C22 C23 1.379(9) . ? C23 C24 1.398(10) . ? C24 C26 1.390(10) . ? C24 C25 1.508(9) . ? C25 O23 1.223(10) . ? C25 O24 1.297(10) . ? C26 C27 1.389(9) . ? C27 N2 1.349(8) . ? C28 O26 1.156(8) . ? C29 O27 1.156(8) . ? C30 O28 1.149(8) . ? C31 O32 1.242(8) . ? C31 O31 1.291(7) . ? C31 C32 1.511(9) . ? C32 N3 1.354(8) . ? C32 C33 1.397(9) . ? C33 C34 1.394(9) . ? C34 C36 1.390(10) . ? C34 C35 1.507(9) . ? C35 O33 1.203(9) . ? C35 O34 1.326(10) . ? C36 C37 1.387(9) . ? C37 N3 1.342(9) . ? C38 O36 1.147(8) . ? C39 O37 1.148(8) . ? C40 O38 1.145(8) . ? C41 O42 1.243(8) . ? C41 O41 1.288(8) . ? C41 C42 1.507(9) . ? C42 N4 1.355(8) . ? C42 C43 1.399(9) . ? C43 C44 1.383(10) . ? C44 C46 1.395(10) . ? C44 C45 1.505(10) . ? C45 O43 1.208(10) . ? C45 O44 1.324(10) . ? C46 C47 1.379(9) . ? C47 N4 1.337(8) . ? C48 O46 1.155(9) . ? C49 O47 1.143(9) . ? C50 O48 1.150(8) . ? 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 C10 Re1 C9 90.1(3) . . ? C10 Re1 C8 87.9(3) . . ? C9 Re1 C8 88.0(3) . . ? C10 Re1 O1 94.6(2) . . ? C9 Re1 O1 99.6(2) . . ? C8 Re1 O1 172.0(2) . . ? C10 Re1 N1 94.0(2) . . ? C9 Re1 N1 173.4(2) . . ? C8 Re1 N1 97.3(2) . . ? O1 Re1 N1 74.96(18) . . ? C10 Re1 O5 172.5(2) . . ? C9 Re1 O5 91.3(2) . . ? C8 Re1 O5 99.5(2) . . ? O1 Re1 O5 77.91(18) . . ? N1 Re1 O5 84.01(19) . . ? C30 Re2 C28 87.8(3) . . ? C30 Re2 C29 90.2(3) . . ? C28 Re2 C29 87.4(3) . . ? C30 Re2 O21 93.1(2) . . ? C28 Re2 O21 176.7(2) . . ? C29 Re2 O21 95.8(2) . . ? C30 Re2 O25 173.4(3) . . ? C28 Re2 O25 98.4(2) . . ? C29 Re2 O25 92.4(2) . . ? O21 Re2 O25 80.68(19) . . ? C30 Re2 N2 95.3(2) . . ? C28 Re2 N2 101.4(2) . . ? C29 Re2 N2 169.7(2) . . ? O21 Re2 N2 75.26(18) . . ? O25 Re2 N2 81.16(19) . . ? C40 Re3 C38 88.0(3) . . ? C40 Re3 C39 92.2(3) . . ? C38 Re3 C39 87.3(3) . . ? C40 Re3 O31 93.6(2) . . ? C38 Re3 O31 176.8(2) . . ? C39 Re3 O31 95.4(2) . . ? C40 Re3 O35 173.3(3) . . ? C38 Re3 O35 97.9(3) . . ? C39 Re3 O35 91.2(2) . . ? O31 Re3 O35 80.4(2) . . ? C40 Re3 N3 93.7(2) . . ? C38 Re3 N3 102.1(2) . . ? C39 Re3 N3 169.1(2) . . ? O31 Re3 N3 75.02(18) . . ? O35 Re3 N3 82.1(2) . . ? C50 Re4 C48 87.9(3) . . ? C50 Re4 C49 89.4(3) . . ? C48 Re4 C49 88.0(3) . . ? C50 Re4 O41 94.3(2) . . ? C48 Re4 O41 172.5(2) . . ? C49 Re4 O41 99.2(2) . . ? C50 Re4 N4 95.0(3) . . ? C48 Re4 N4 97.4(3) . . ? C49 Re4 N4 173.1(2) . . ? O41 Re4 N4 75.27(18) . . ? C50 Re4 O45 172.5(2) . . ? C48 Re4 O45 99.6(3) . . ? C49 Re4 O45 91.8(2) . . ? O41 Re4 O45 78.13(18) . . ? N4 Re4 O45 83.14(19) . . ? O2 C1 O1 124.6(6) . . ? O2 C1 C2 119.8(5) . . ? O1 C1 C2 115.5(5) . . ? N1 C2 C3 122.2(5) . . ? N1 C2 C1 114.9(5) . . ? C3 C2 C1 122.8(5) . . ? C2 C3 C4 118.8(6) . . ? C3 C4 C6 118.7(6) . . ? C3 C4 C5 120.0(6) . . ? C6 C4 C5 121.2(6) . . ? O3 C5 O4 127.8(7) . . ? O3 C5 C4 120.2(7) . . ? O4 C5 C4 111.9(6) . . ? C7 C6 C4 119.4(6) . . ? N1 C7 C6 122.3(6) . . ? O6 C8 Re1 178.2(6) . . ? O7 C9 Re1 178.4(7) . . ? O8 C10 Re1 178.3(6) . . ? O22 C21 O21 124.0(6) . . ? O22 C21 C22 120.2(5) . . ? O21 C21 C22 115.9(5) . . ? N2 C22 C23 122.3(6) . . ? N2 C22 C21 115.0(5) . . ? C23 C22 C21 122.6(6) . . ? C22 C23 C24 119.3(6) . . ? C26 C24 C23 118.0(6) . . ? C26 C24 C25 122.0(6) . . ? C23 C24 C25 120.0(6) . . ? O23 C25 O24 126.9(7) . . ? O23 C25 C24 119.9(7) . . ? O24 C25 C24 113.3(7) . . ? C27 C26 C24 120.2(6) . . ? N2 C27 C26 121.4(6) . . ? O26 C28 Re2 176.0(6) . . ? O27 C29 Re2 178.1(5) . . ? O28 C30 Re2 178.5(6) . . ? O32 C31 O31 122.8(6) . . ? O32 C31 C32 121.3(5) . . ? O31 C31 C32 115.9(5) . . ? N3 C32 C33 122.3(6) . . ? N3 C32 C31 115.3(5) . . ? C33 C32 C31 122.4(5) . . ? C34 C33 C32 118.8(6) . . ? C36 C34 C33 118.8(6) . . ? C36 C34 C35 122.5(6) . . ? C33 C34 C35 118.7(6) . . ? O33 C35 O34 126.0(7) . . ? O33 C35 C34 122.1(7) . . ? O34 C35 C34 111.8(6) . . ? C37 C36 C34 119.0(6) . . ? N3 C37 C36 122.9(6) . . ? O36 C38 Re3 175.8(6) . . ? O37 C39 Re3 177.6(5) . . ? O38 C40 Re3 179.6(6) . . ? O42 C41 O41 123.4(6) . . ? O42 C41 C42 120.1(6) . . ? O41 C41 C42 116.5(5) . . ? N4 C42 C43 122.3(6) . . ? N4 C42 C41 115.2(5) . . ? C43 C42 C41 122.5(6) . . ? C44 C43 C42 118.5(6) . . ? C43 C44 C46 119.1(6) . . ? C43 C44 C45 119.2(6) . . ? C46 C44 C45 121.7(6) . . ? O43 C45 O44 124.9(7) . . ? O43 C45 C44 122.5(7) . . ? O44 C45 C44 112.5(6) . . ? C47 C46 C44 118.8(6) . . ? N4 C47 C46 123.3(6) . . ? O46 C48 Re4 176.2(7) . . ? O47 C49 Re4 179.4(7) . . ? O48 C50 Re4 179.5(7) . . ? C7 N1 C2 118.6(5) . . ? C7 N1 Re1 126.0(4) . . ? C2 N1 Re1 115.4(4) . . ? C27 N2 C22 118.8(5) . . ? C27 N2 Re2 125.9(4) . . ? C22 N2 Re2 115.1(4) . . ? C37 N3 C32 118.2(5) . . ? C37 N3 Re3 126.3(4) . . ? C32 N3 Re3 115.4(4) . . ? C47 N4 C42 118.0(5) . . ? C47 N4 Re4 126.9(4) . . ? C42 N4 Re4 115.1(4) . . ? C1 O1 Re1 118.9(4) . . ? C21 O21 Re2 118.5(4) . . ? C31 O31 Re3 118.3(4) . . ? C41 O41 Re4 117.8(4) . . ? 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 O2 C1 C2 N1 177.6(6) . . . . ? O1 C1 C2 N1 -4.0(8) . . . . ? O2 C1 C2 C3 -4.3(9) . . . . ? O1 C1 C2 C3 174.0(6) . . . . ? N1 C2 C3 C4 0.2(9) . . . . ? C1 C2 C3 C4 -177.7(6) . . . . ? C2 C3 C4 C6 -1.3(10) . . . . ? C2 C3 C4 C5 177.4(6) . . . . ? C3 C4 C5 O3 -1.8(10) . . . . ? C6 C4 C5 O3 176.8(7) . . . . ? C3 C4 C5 O4 -179.4(7) . . . . ? C6 C4 C5 O4 -0.8(10) . . . . ? C3 C4 C6 C7 1.0(10) . . . . ? C5 C4 C6 C7 -177.7(6) . . . . ? C4 C6 C7 N1 0.4(10) . . . . ? C10 Re1 C8 O6 4(18) . . . . ? C9 Re1 C8 O6 94(18) . . . . ? O1 Re1 C8 O6 -105(18) . . . . ? N1 Re1 C8 O6 -90(18) . . . . ? O5 Re1 C8 O6 -175(100) . . . . ? C10 Re1 C9 O7 118(21) . . . . ? C8 Re1 C9 O7 30(21) . . . . ? O1 Re1 C9 O7 -147(21) . . . . ? N1 Re1 C9 O7 -113(20) . . . . ? O5 Re1 C9 O7 -69(21) . . . . ? C9 Re1 C10 O8 171(22) . . . . ? C8 Re1 C10 O8 -101(22) . . . . ? O1 Re1 C10 O8 71(22) . . . . ? N1 Re1 C10 O8 -4(22) . . . . ? O5 Re1 C10 O8 70(23) . . . . ? O22 C21 C22 N2 178.2(6) . . . . ? O21 C21 C22 N2 -2.3(8) . . . . ? O22 C21 C22 C23 -6.4(9) . . . . ? O21 C21 C22 C23 173.2(6) . . . . ? N2 C22 C23 C24 0.3(10) . . . . ? C21 C22 C23 C24 -174.8(6) . . . . ? C22 C23 C24 C26 0.9(10) . . . . ? C22 C23 C24 C25 179.1(6) . . . . ? C26 C24 C25 O23 -176.5(7) . . . . ? C23 C24 C25 O23 5.4(11) . . . . ? C26 C24 C25 O24 3.4(10) . . . . ? C23 C24 C25 O24 -174.7(6) . . . . ? C23 C24 C26 C27 -1.4(10) . . . . ? C25 C24 C26 C27 -179.5(6) . . . . ? C24 C26 C27 N2 0.6(10) . . . . ? C30 Re2 C28 O26 41(9) . . . . ? C29 Re2 C28 O26 -49(9) . . . . ? O21 Re2 C28 O26 146(7) . . . . ? O25 Re2 C28 O26 -141(9) . . . . ? N2 Re2 C28 O26 136(9) . . . . ? C30 Re2 C29 O27 130(20) . . . . ? C28 Re2 C29 O27 -142(20) . . . . ? O21 Re2 C29 O27 37(20) . . . . ? O25 Re2 C29 O27 -44(20) . . . . ? N2 Re2 C29 O27 8(21) . . . . ? C28 Re2 C30 O28 117(25) . . . . ? C29 Re2 C30 O28 -155(25) . . . . ? O21 Re2 C30 O28 -60(25) . . . . ? O25 Re2 C30 O28 -41(26) . . . . ? N2 Re2 C30 O28 16(25) . . . . ? O32 C31 C32 N3 -178.4(6) . . . . ? O31 C31 C32 N3 2.2(8) . . . . ? O32 C31 C32 C33 5.1(10) . . . . ? O31 C31 C32 C33 -174.3(6) . . . . ? N3 C32 C33 C34 -0.9(9) . . . . ? C31 C32 C33 C34 175.2(6) . . . . ? C32 C33 C34 C36 1.5(9) . . . . ? C32 C33 C34 C35 179.4(6) . . . . ? C36 C34 C35 O33 174.8(7) . . . . ? C33 C34 C35 O33 -3.0(11) . . . . ? C36 C34 C35 O34 -6.6(10) . . . . ? C33 C34 C35 O34 175.6(6) . . . . ? C33 C34 C36 C37 -0.9(10) . . . . ? C35 C34 C36 C37 -178.7(6) . . . . ? C34 C36 C37 N3 -0.4(10) . . . . ? C40 Re3 C38 O36 -50(9) . . . . ? C39 Re3 C38 O36 43(9) . . . . ? O31 Re3 C38 O36 -169(6) . . . . ? O35 Re3 C38 O36 133(9) . . . . ? N3 Re3 C38 O36 -143(9) . . . . ? C40 Re3 C39 O37 -154(16) . . . . ? C38 Re3 C39 O37 118(16) . . . . ? O31 Re3 C39 O37 -61(16) . . . . ? O35 Re3 C39 O37 20(16) . . . . ? N3 Re3 C39 O37 -32(16) . . . . ? C38 Re3 C40 O38 -86(100) . . . . ? C39 Re3 C40 O38 -174(100) . . . . ? O31 Re3 C40 O38 91(100) . . . . ? O35 Re3 C40 O38 65(100) . . . . ? N3 Re3 C40 O38 16(100) . . . . ? O42 C41 C42 N4 176.6(6) . . . . ? O41 C41 C42 N4 -3.7(8) . . . . ? O42 C41 C42 C43 -3.6(9) . . . . ? O41 C41 C42 C43 176.1(6) . . . . ? N4 C42 C43 C44 0.1(9) . . . . ? C41 C42 C43 C44 -179.7(6) . . . . ? C42 C43 C44 C46 -1.3(9) . . . . ? C42 C43 C44 C45 177.2(6) . . . . ? C43 C44 C45 O43 -3.6(11) . . . . ? C46 C44 C45 O43 174.9(7) . . . . ? C43 C44 C45 O44 178.3(6) . . . . ? C46 C44 C45 O44 -3.2(10) . . . . ? C43 C44 C46 C47 1.3(10) . . . . ? C45 C44 C46 C47 -177.1(6) . . . . ? C44 C46 C47 N4 0.0(10) . . . . ? C50 Re4 C48 O46 36(10) . . . . ? C49 Re4 C48 O46 126(10) . . . . ? O41 Re4 C48 O46 -71(11) . . . . ? N4 Re4 C48 O46 -59(10) . . . . ? O45 Re4 C48 O46 -143(10) . . . . ? C50 Re4 C49 O47 98(61) . . . . ? C48 Re4 C49 O47 10(61) . . . . ? O41 Re4 C49 O47 -168(100) . . . . ? N4 Re4 C49 O47 -132(60) . . . . ? O45 Re4 C49 O47 -89(61) . . . . ? C48 Re4 C50 O48 142(100) . . . . ? C49 Re4 C50 O48 54(90) . . . . ? O41 Re4 C50 O48 -45(90) . . . . ? N4 Re4 C50 O48 -120(90) . . . . ? O45 Re4 C50 O48 -45(91) . . . . ? C6 C7 N1 C2 -1.5(9) . . . . ? C6 C7 N1 Re1 177.3(5) . . . . ? C3 C2 N1 C7 1.2(9) . . . . ? C1 C2 N1 C7 179.3(5) . . . . ? C3 C2 N1 Re1 -177.8(5) . . . . ? C1 C2 N1 Re1 0.3(6) . . . . ? C10 Re1 N1 C7 -83.3(5) . . . . ? C9 Re1 N1 C7 148(2) . . . . ? C8 Re1 N1 C7 5.1(5) . . . . ? O1 Re1 N1 C7 -177.0(5) . . . . ? O5 Re1 N1 C7 103.9(5) . . . . ? C10 Re1 N1 C2 95.6(5) . . . . ? C9 Re1 N1 C2 -33(2) . . . . ? C8 Re1 N1 C2 -176.0(4) . . . . ? O1 Re1 N1 C2 1.9(4) . . . . ? O5 Re1 N1 C2 -77.2(4) . . . . ? C26 C27 N2 C22 0.6(9) . . . . ? C26 C27 N2 Re2 175.4(5) . . . . ? C23 C22 N2 C27 -1.1(9) . . . . ? C21 C22 N2 C27 174.3(5) . . . . ? C23 C22 N2 Re2 -176.4(5) . . . . ? C21 C22 N2 Re2 -1.0(6) . . . . ? C30 Re2 N2 C27 95.6(5) . . . . ? C28 Re2 N2 C27 6.9(6) . . . . ? C29 Re2 N2 C27 -142.1(13) . . . . ? O21 Re2 N2 C27 -172.6(5) . . . . ? O25 Re2 N2 C27 -90.0(5) . . . . ? C30 Re2 N2 C22 -89.4(5) . . . . ? C28 Re2 N2 C22 -178.2(4) . . . . ? C29 Re2 N2 C22 32.8(16) . . . . ? O21 Re2 N2 C22 2.4(4) . . . . ? O25 Re2 N2 C22 85.0(4) . . . . ? C36 C37 N3 C32 0.9(9) . . . . ? C36 C37 N3 Re3 -175.6(5) . . . . ? C33 C32 N3 C37 -0.3(9) . . . . ? C31 C32 N3 C37 -176.7(5) . . . . ? C33 C32 N3 Re3 176.6(5) . . . . ? C31 C32 N3 Re3 0.2(7) . . . . ? C40 Re3 N3 C37 -92.0(5) . . . . ? C38 Re3 N3 C37 -3.3(6) . . . . ? C39 Re3 N3 C37 145.6(12) . . . . ? O31 Re3 N3 C37 175.2(5) . . . . ? O35 Re3 N3 C37 93.1(5) . . . . ? C40 Re3 N3 C32 91.3(5) . . . . ? C38 Re3 N3 C32 -179.9(4) . . . . ? C39 Re3 N3 C32 -31.1(15) . . . . ? O31 Re3 N3 C32 -1.4(4) . . . . ? O35 Re3 N3 C32 -83.5(4) . . . . ? C46 C47 N4 C42 -1.2(9) . . . . ? C46 C47 N4 Re4 178.5(5) . . . . ? C43 C42 N4 C47 1.2(9) . . . . ? C41 C42 N4 C47 -179.0(5) . . . . ? C43 C42 N4 Re4 -178.5(5) . . . . ? C41 C42 N4 Re4 1.3(7) . . . . ? C50 Re4 N4 C47 -86.0(6) . . . . ? C48 Re4 N4 C47 2.5(6) . . . . ? C49 Re4 N4 C47 145(2) . . . . ? O41 Re4 N4 C47 -179.1(5) . . . . ? O45 Re4 N4 C47 101.4(5) . . . . ? C50 Re4 N4 C42 93.7(5) . . . . ? C48 Re4 N4 C42 -177.7(5) . . . . ? C49 Re4 N4 C42 -36(2) . . . . ? O41 Re4 N4 C42 0.6(4) . . . . ? O45 Re4 N4 C42 -78.9(4) . . . . ? O2 C1 O1 Re1 -175.8(5) . . . . ? C2 C1 O1 Re1 5.9(7) . . . . ? C10 Re1 O1 C1 -97.3(5) . . . . ? C9 Re1 O1 C1 171.8(5) . . . . ? C8 Re1 O1 C1 10.7(18) . . . . ? N1 Re1 O1 C1 -4.4(4) . . . . ? O5 Re1 O1 C1 82.6(5) . . . . ? O22 C21 O21 Re2 -175.9(5) . . . . ? C22 C21 O21 Re2 4.5(7) . . . . ? C30 Re2 O21 C21 90.9(5) . . . . ? C28 Re2 O21 C21 -14(4) . . . . ? C29 Re2 O21 C21 -178.6(5) . . . . ? O25 Re2 O21 C21 -87.1(4) . . . . ? N2 Re2 O21 C21 -3.9(4) . . . . ? O32 C31 O31 Re3 177.1(5) . . . . ? C32 C31 O31 Re3 -3.5(7) . . . . ? C40 Re3 O31 C31 -90.1(5) . . . . ? C38 Re3 O31 C31 29(5) . . . . ? C39 Re3 O31 C31 177.4(5) . . . . ? O35 Re3 O31 C31 87.0(5) . . . . ? N3 Re3 O31 C31 2.8(4) . . . . ? O42 C41 O41 Re4 -176.0(5) . . . . ? C42 C41 O41 Re4 4.3(7) . . . . ? C50 Re4 O41 C41 -96.8(5) . . . . ? C48 Re4 O41 C41 10(2) . . . . ? C49 Re4 O41 C41 173.1(5) . . . . ? N4 Re4 O41 C41 -2.7(4) . . . . ? O45 Re4 O41 C41 83.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.02 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.245 _refine_diff_density_min -1.008 _refine_diff_density_rms 0.194 data_compound11 _database_code_depnum_ccdc_archive 'CCDC 228230' _audit_creation_method SHELXL-97 _chemical_name_systematic Rhenium(I)-(pyridine-2.5-dicarboxylicacid)(imidazole)(CO)3 _chemical_name_common '[Re(CO)3(2,5-dipic)(im)]' _chemical_melting_point ? _chemical_formula_moiety 'C13 H8 N3 O7 Re' _chemical_formula_sum 'C13 H8 N3 O7 Re' _chemical_formula_weight 504.42 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5005(8) _cell_length_b 8.6008(9) _cell_length_c 12.6462(13) _cell_angle_alpha 95.120(12) _cell_angle_beta 94.378(12) _cell_angle_gamma 106.362(11) _cell_volume 775.24(14) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 120 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description column _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.161 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 476 _exptl_absorpt_coefficient_mu 7.879 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3654 _exptl_absorpt_correction_T_max 0.6941 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method '/f oscillation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 50-200 _diffrn_standards_interval_count image _diffrn_standards_interval_time 6.8 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11003 _diffrn_reflns_av_R_equivalents 0.0681 _diffrn_reflns_av_sigmaI/netI 0.1102 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 30.39 _reflns_number_total 4253 _reflns_number_gt 2852 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (Stoe, 1999)' _computing_cell_refinement 'IPDS (Stoe, 1999)' _computing_data_reduction 'XRed (Stoe, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Zortep (Zsolnai, 1994), Platon (Spek, 1993)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0233P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4253 _refine_ls_number_parameters 221 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0614 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0683 _refine_ls_wR_factor_gt 0.0640 _refine_ls_goodness_of_fit_ref 0.821 _refine_ls_restrained_S_all 0.821 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re Re 0.61909(5) 0.84975(4) 0.80731(2) 0.02355(8) Uani 1 1 d . . . O1 O 0.7835(6) 1.0011(5) 0.6988(3) 0.0229(9) Uani 1 1 d . . . O2 O 0.8076(6) 1.0395(5) 0.5262(3) 0.0251(9) Uani 1 1 d . . . O3 O 0.0717(7) 0.3079(5) 0.5787(3) 0.0281(10) Uani 1 1 d . . . H3A H -0.028(13) 0.218(11) 0.564(6) 0.06(3) Uiso 1 1 d . . . O4 O 0.0649(7) 0.3200(5) 0.4013(3) 0.0315(11) Uani 1 1 d . . . N1 N 0.4923(7) 0.7346(6) 0.6477(4) 0.0187(11) Uani 1 1 d . . . N2 N 0.4381(8) 1.0080(6) 0.7856(4) 0.0244(12) Uani 1 1 d . . . N3 N 0.1848(8) 1.0881(7) 0.7600(4) 0.0302(12) Uani 1 1 d . . . H3B H 0.0690 1.0851 0.7396 0.036 Uiso 1 1 calc R . . C1 C 0.7328(8) 0.9645(7) 0.5977(4) 0.0207(12) Uani 1 1 d . . . C2 C 0.5662(8) 0.8157(6) 0.5656(4) 0.0156(11) Uani 1 1 d . . . C3 C 0.4990(8) 0.7609(7) 0.4591(4) 0.0207(12) Uani 1 1 d . . . H3 H 0.5534 0.8196 0.4037 0.025 Uiso 1 1 calc R . . C4 C 0.3521(9) 0.6202(7) 0.4353(4) 0.0212(13) Uani 1 1 d . . . H4 H 0.3021 0.5822 0.3633 0.025 Uiso 1 1 calc R . . C5 C 0.2780(8) 0.5346(7) 0.5177(4) 0.0189(12) Uani 1 1 d . . . C6 C 0.3510(9) 0.5982(7) 0.6226(4) 0.0203(13) Uani 1 1 d . . . H6 H 0.2975 0.5415 0.6790 0.024 Uiso 1 1 calc R . . C7 C 0.1262(8) 0.3759(7) 0.4926(4) 0.0176(12) Uani 1 1 d . . . C8 C 0.2580(9) 0.9632(8) 0.7476(4) 0.0271(14) Uani 1 1 d . . . H8 H 0.1903 0.8564 0.7158 0.032 Uiso 1 1 calc R . . C9 C 0.3224(11) 1.2217(8) 0.8102(5) 0.0356(16) Uani 1 1 d . . . H9 H 0.3117 1.3276 0.8301 0.043 Uiso 1 1 calc R . . C10 C 0.4784(10) 1.1699(8) 0.8255(5) 0.0300(15) Uani 1 1 d . . . H10 H 0.5967 1.2358 0.8588 0.036 Uiso 1 1 calc R . . C11 C 0.7464(10) 0.9810(9) 0.9373(5) 0.0298(16) Uani 1 1 d . . . O11 O 0.8227(7) 1.0591(6) 1.0156(3) 0.0390(12) Uani 1 1 d . . . C12 C 0.7771(12) 0.7106(9) 0.8224(5) 0.0387(19) Uani 1 1 d . . . O12 O 0.8694(9) 0.6216(7) 0.8361(4) 0.0548(16) Uani 1 1 d . . . C13 C 0.4545(11) 0.7106(9) 0.8873(5) 0.0322(17) Uani 1 1 d . . . O13 O 0.3509(9) 0.6194(6) 0.9335(4) 0.0489(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 Re 0.02341(14) 0.02282(12) 0.01986(11) -0.00104(7) -0.00049(8) 0.00118(10) O1 0.015(2) 0.022(2) 0.026(2) -0.0027(17) -0.0001(17) -0.003(2) O2 0.019(2) 0.020(2) 0.028(2) 0.0053(17) 0.0042(17) -0.008(2) O3 0.027(3) 0.019(2) 0.028(2) 0.0028(17) 0.0016(18) -0.010(2) O4 0.029(3) 0.027(2) 0.026(2) -0.0027(19) -0.0017(19) -0.008(2) N1 0.017(3) 0.019(3) 0.018(2) 0.0033(19) 0.0018(19) 0.001(2) N2 0.021(3) 0.026(3) 0.020(2) -0.001(2) 0.001(2) -0.002(3) N3 0.026(3) 0.037(3) 0.027(3) 0.006(2) 0.000(2) 0.008(3) C1 0.019(3) 0.018(3) 0.025(3) 0.002(2) 0.003(2) 0.005(3) C2 0.016(3) 0.014(3) 0.019(2) 0.002(2) 0.002(2) 0.007(3) C3 0.019(3) 0.022(3) 0.022(3) 0.005(2) 0.005(2) 0.005(3) C4 0.021(4) 0.018(3) 0.020(3) -0.002(2) -0.004(2) 0.003(3) C5 0.015(3) 0.013(3) 0.025(3) -0.001(2) 0.002(2) -0.002(3) C6 0.020(4) 0.018(3) 0.023(3) 0.005(2) 0.005(2) 0.003(3) C7 0.012(3) 0.015(3) 0.023(3) -0.005(2) -0.001(2) 0.003(3) C8 0.027(4) 0.028(3) 0.024(3) 0.001(2) 0.000(3) 0.004(3) C9 0.047(5) 0.026(3) 0.034(3) 0.001(3) 0.004(3) 0.011(4) C10 0.031(4) 0.026(3) 0.028(3) 0.000(3) -0.003(3) 0.002(3) C11 0.028(4) 0.034(4) 0.025(3) 0.002(3) 0.001(3) 0.006(4) O11 0.039(3) 0.044(3) 0.023(2) -0.009(2) -0.005(2) 0.001(3) C12 0.047(5) 0.035(4) 0.021(3) -0.004(3) 0.005(3) -0.006(4) O12 0.071(5) 0.057(4) 0.048(3) 0.005(3) 0.001(3) 0.041(4) C13 0.036(5) 0.029(4) 0.024(3) -0.003(3) -0.003(3) 0.001(4) O13 0.058(4) 0.037(3) 0.040(3) 0.004(2) 0.014(3) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C13 1.885(8) . ? Re C12 1.918(9) . ? Re C11 1.927(7) . ? Re O1 2.185(4) . ? Re N1 2.186(5) . ? Re N2 2.196(5) . ? O1 C1 1.290(7) . ? O2 C1 1.235(7) . ? O3 C7 1.319(7) . ? O4 C7 1.213(6) . ? N1 C6 1.335(8) . ? N1 C2 1.367(7) . ? N2 C8 1.333(8) . ? N2 C10 1.378(8) . ? N3 C8 1.340(8) . ? N3 C9 1.375(9) . ? C1 C2 1.514(8) . ? C2 C3 1.393(7) . ? C3 C4 1.379(8) . ? C4 C5 1.390(8) . ? C5 C6 1.396(8) . ? C5 C7 1.501(8) . ? C9 C10 1.371(9) . ? C11 O11 1.156(7) . ? C12 O12 1.183(9) . ? C13 O13 1.170(9) . ? 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 C13 Re C12 86.8(3) . . ? C13 Re C11 90.0(3) . . ? C12 Re C11 89.5(3) . . ? C13 Re O1 173.2(2) . . ? C12 Re O1 96.0(3) . . ? C11 Re O1 96.3(2) . . ? C13 Re N1 98.2(2) . . ? C12 Re N1 94.4(2) . . ? C11 Re N1 171.1(3) . . ? O1 Re N1 75.38(17) . . ? C13 Re N2 94.0(3) . . ? C12 Re N2 178.5(3) . . ? C11 Re N2 91.7(2) . . ? O1 Re N2 83.03(18) . . ? N1 Re N2 84.32(17) . . ? C1 O1 Re 117.8(4) . . ? C6 N1 C2 117.6(5) . . ? C6 N1 Re 127.4(4) . . ? C2 N1 Re 115.0(4) . . ? C8 N2 C10 105.3(5) . . ? C8 N2 Re 127.5(4) . . ? C10 N2 Re 126.3(4) . . ? C8 N3 C9 108.1(5) . . ? O2 C1 O1 125.9(6) . . ? O2 C1 C2 118.1(5) . . ? O1 C1 C2 116.0(5) . . ? N1 C2 C3 122.4(5) . . ? N1 C2 C1 115.6(5) . . ? C3 C2 C1 122.0(5) . . ? C4 C3 C2 119.0(5) . . ? C3 C4 C5 119.3(5) . . ? C4 C5 C6 118.4(5) . . ? C4 C5 C7 119.9(5) . . ? C6 C5 C7 121.6(5) . . ? N1 C6 C5 123.3(5) . . ? O4 C7 O3 125.6(6) . . ? O4 C7 C5 121.4(5) . . ? O3 C7 C5 113.0(5) . . ? N2 C8 N3 111.2(6) . . ? C10 C9 N3 105.4(5) . . ? C9 C10 N2 109.9(6) . . ? O11 C11 Re 179.7(6) . . ? O12 C12 Re 176.5(6) . . ? O13 C13 Re 177.3(6) . . ? 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 C13 Re O1 C1 -18(2) . . . . ? C12 Re O1 C1 96.1(4) . . . . ? C11 Re O1 C1 -173.8(4) . . . . ? N1 Re O1 C1 3.1(4) . . . . ? N2 Re O1 C1 -82.8(4) . . . . ? C13 Re N1 C6 -5.1(5) . . . . ? C12 Re N1 C6 82.3(5) . . . . ? C11 Re N1 C6 -162.2(15) . . . . ? O1 Re N1 C6 177.4(5) . . . . ? N2 Re N1 C6 -98.3(5) . . . . ? C13 Re N1 C2 173.5(4) . . . . ? C12 Re N1 C2 -99.1(4) . . . . ? C11 Re N1 C2 16.5(19) . . . . ? O1 Re N1 C2 -4.0(3) . . . . ? N2 Re N1 C2 80.3(4) . . . . ? C13 Re N2 C8 -52.8(5) . . . . ? C12 Re N2 C8 71(12) . . . . ? C11 Re N2 C8 -142.9(5) . . . . ? O1 Re N2 C8 121.0(5) . . . . ? N1 Re N2 C8 45.1(5) . . . . ? C13 Re N2 C10 115.0(5) . . . . ? C12 Re N2 C10 -121(12) . . . . ? C11 Re N2 C10 24.9(5) . . . . ? O1 Re N2 C10 -71.2(5) . . . . ? N1 Re N2 C10 -147.1(5) . . . . ? Re O1 C1 O2 178.3(4) . . . . ? Re O1 C1 C2 -1.8(6) . . . . ? C6 N1 C2 C3 0.2(7) . . . . ? Re N1 C2 C3 -178.6(4) . . . . ? C6 N1 C2 C1 -176.8(5) . . . . ? Re N1 C2 C1 4.4(5) . . . . ? O2 C1 C2 N1 178.1(5) . . . . ? O1 C1 C2 N1 -1.8(7) . . . . ? O2 C1 C2 C3 1.1(7) . . . . ? O1 C1 C2 C3 -178.8(5) . . . . ? N1 C2 C3 C4 0.2(8) . . . . ? C1 C2 C3 C4 177.1(5) . . . . ? C2 C3 C4 C5 -1.5(8) . . . . ? C3 C4 C5 C6 2.4(8) . . . . ? C3 C4 C5 C7 -176.2(5) . . . . ? C2 N1 C6 C5 0.7(8) . . . . ? Re N1 C6 C5 179.3(4) . . . . ? C4 C5 C6 N1 -2.1(8) . . . . ? C7 C5 C6 N1 176.5(5) . . . . ? C4 C5 C7 O4 -0.4(8) . . . . ? C6 C5 C7 O4 -179.0(5) . . . . ? C4 C5 C7 O3 179.2(5) . . . . ? C6 C5 C7 O3 0.6(7) . . . . ? C10 N2 C8 N3 1.0(7) . . . . ? Re N2 C8 N3 170.8(4) . . . . ? C9 N3 C8 N2 -1.0(7) . . . . ? C8 N3 C9 C10 0.5(7) . . . . ? N3 C9 C10 N2 0.1(7) . . . . ? C8 N2 C10 C9 -0.6(7) . . . . ? Re N2 C10 C9 -170.6(4) . . . . ? C13 Re C11 O11 40(100) . . . . ? C12 Re C11 O11 -47(100) . . . . ? O1 Re C11 O11 -143(100) . . . . ? N1 Re C11 O11 -163(100) . . . . ? N2 Re C11 O11 134(100) . . . . ? C13 Re C12 O12 -18(11) . . . . ? C11 Re C12 O12 72(11) . . . . ? O1 Re C12 O12 169(11) . . . . ? N1 Re C12 O12 -116(11) . . . . ? N2 Re C12 O12 -141(10) . . . . ? C12 Re C13 O13 -69(14) . . . . ? C11 Re C13 O13 -158(14) . . . . ? O1 Re C13 O13 46(15) . . . . ? N1 Re C13 O13 25(14) . . . . ? N2 Re C13 O13 110(14) . . . . ? 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 O3 H3A O2 0.91(9) 1.68(9) 2.578(6) 172(8) 1_445 N3 H3B O1 0.88 2.07 2.914(7) 161.7 1_455 _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 30.39 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 1.556 _refine_diff_density_min -1.287 _refine_diff_density_rms 0.207 data_4 _database_code_depnum_ccdc_archive 'CCDC 228231' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Tc(i)(water)(1H-imidazole-4-carboxylic acid)(CO)3' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H5 N2 O6 Tc' _chemical_formula_weight 311.13 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' Tc Tc -1.4390 0.7593 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.7875(9) _cell_length_b 7.3430(6) _cell_length_c 12.8952(10) _cell_angle_alpha 90.00 _cell_angle_beta 114.894(8) _cell_angle_gamma 90.00 _cell_volume 1012.45(14) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.041 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 1.437 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5972 _exptl_absorpt_correction_T_max 0.7153 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method '/f oscillation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 50-200 _diffrn_standards_interval_count 'every image' _diffrn_standards_interval_time 4.3 _diffrn_standards_decay_% ? _diffrn_reflns_number 1817 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0145 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 25.90 _reflns_number_total 1817 _reflns_number_gt 1560 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS, Stoe, 1999)' _computing_cell_refinement 'IPDS, Stoe, 1999)' _computing_data_reduction 'X-Red, Stoe, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Zortep (Zsolnai, 1994), Platon (Spek, 1993)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1817 _refine_ls_number_parameters 165 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0284 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0645 _refine_ls_wR_factor_gt 0.0639 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tc1 Tc 0.77493(2) 0.13052(3) 0.504679(18) 0.01848(11) Uani 1 1 d . . . O1 O 0.58000(18) 0.0299(2) 0.41866(16) 0.0195(4) Uani 1 1 d . . . O2 O 0.3803(2) 0.1146(2) 0.31862(17) 0.0233(4) Uani 1 1 d . . . O3 O 0.7149(2) 0.1909(3) 0.64105(18) 0.0195(4) Uani 1 1 d . . . H4 H 0.692(4) 0.115(5) 0.659(3) 0.017(9) Uiso 1 1 d . . . H5 H 0.766(4) 0.235(5) 0.698(3) 0.030(10) Uiso 1 1 d . . . O4 O 0.9111(2) -0.2196(3) 0.6218(2) 0.0441(7) Uani 1 1 d . . . O5 O 1.0266(3) 0.3261(4) 0.6114(3) 0.0476(7) Uani 1 1 d . . . O6 O 0.8272(3) 0.0450(5) 0.2973(2) 0.0551(8) Uani 1 1 d . . . N1 N 0.6658(2) 0.3712(3) 0.4324(2) 0.0202(5) Uani 1 1 d . . . N2 N 0.5694(3) 0.6344(3) 0.3936(2) 0.0251(6) Uani 1 1 d . . . H3 H 0.559(3) 0.748(5) 0.392(3) 0.029(9) Uiso 1 1 d . . . C1 C 0.6812(3) 0.5490(4) 0.4355(3) 0.0241(6) Uani 1 1 d . . . H1 H 0.753(4) 0.611(5) 0.461(4) 0.031(9) Uiso 1 1 d . . . C2 C 0.4782(3) 0.5056(4) 0.3603(3) 0.0227(6) Uani 1 1 d . . . H2 H 0.405(4) 0.528(5) 0.340(3) 0.024(9) Uiso 1 1 d . . . C3 C 0.5386(3) 0.3404(3) 0.3848(2) 0.0170(5) Uani 1 1 d . . . C4 C 0.4947(3) 0.1505(3) 0.3721(2) 0.0169(6) Uani 1 1 d . . . C5 C 0.8583(3) -0.0902(4) 0.5767(3) 0.0275(7) Uani 1 1 d . . . C6 C 0.9332(3) 0.2507(4) 0.5732(3) 0.0294(7) Uani 1 1 d . . . C7 C 0.8086(3) 0.0786(5) 0.3748(3) 0.0320(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 Tc1 0.01570(17) 0.01538(15) 0.02066(15) -0.00195(8) 0.00402(12) 0.00100(8) O1 0.0182(11) 0.0121(9) 0.0224(10) 0.0005(7) 0.0030(9) 0.0009(7) O2 0.0180(12) 0.0177(9) 0.0270(11) 0.0047(8) 0.0023(10) -0.0012(7) O3 0.0194(12) 0.0140(9) 0.0209(11) -0.0026(8) 0.0044(10) -0.0039(8) O4 0.0414(17) 0.0235(12) 0.0430(14) -0.0049(10) -0.0061(13) 0.0126(10) O5 0.0245(16) 0.0489(14) 0.0608(18) -0.0076(13) 0.0095(15) -0.0117(12) O6 0.0469(18) 0.087(2) 0.0358(15) -0.0062(14) 0.0216(14) 0.0107(15) N1 0.0228(15) 0.0145(11) 0.0206(12) 0.0001(8) 0.0066(11) -0.0019(9) N2 0.0367(18) 0.0105(12) 0.0247(13) -0.0009(9) 0.0095(13) -0.0005(9) C1 0.0284(18) 0.0165(13) 0.0233(14) -0.0005(11) 0.0069(14) -0.0050(12) C2 0.0251(19) 0.0160(13) 0.0246(15) 0.0001(11) 0.0082(15) 0.0031(12) C3 0.0181(16) 0.0133(12) 0.0158(13) 0.0009(9) 0.0034(12) -0.0002(10) C4 0.0174(17) 0.0149(12) 0.0155(13) 0.0017(9) 0.0042(13) 0.0000(10) C5 0.0210(18) 0.0246(14) 0.0279(15) -0.0120(12) 0.0014(14) -0.0007(12) C6 0.026(2) 0.0269(15) 0.0326(17) -0.0020(12) 0.0096(16) 0.0010(13) C7 0.0238(19) 0.0405(17) 0.0288(16) -0.0024(14) 0.0084(15) 0.0046(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Tc1 C6 1.911(3) . ? Tc1 C7 1.915(3) . ? Tc1 C5 1.920(3) . ? Tc1 N1 2.154(2) . ? Tc1 O3 2.200(2) . ? Tc1 O1 2.216(2) . ? O1 C4 1.284(3) . ? O2 C4 1.257(4) . ? O4 C5 1.150(4) . ? O5 C6 1.142(4) . ? O6 C7 1.137(4) . ? N1 C1 1.316(3) . ? N1 C3 1.379(4) . ? N2 C1 1.349(4) . ? N2 C2 1.359(4) . ? C2 C3 1.374(4) . ? C3 C4 1.472(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 C6 Tc1 C7 88.56(14) . . ? C6 Tc1 C5 87.98(13) . . ? C7 Tc1 C5 90.14(14) . . ? C6 Tc1 N1 96.32(11) . . ? C7 Tc1 N1 95.22(12) . . ? C5 Tc1 N1 173.20(11) . . ? C6 Tc1 O3 96.74(11) . . ? C7 Tc1 O3 173.85(12) . . ? C5 Tc1 O3 93.15(11) . . ? N1 Tc1 O3 81.14(8) . . ? C6 Tc1 O1 171.96(10) . . ? C7 Tc1 O1 92.81(12) . . ? C5 Tc1 O1 99.93(10) . . ? N1 Tc1 O1 75.67(8) . . ? O3 Tc1 O1 81.52(8) . . ? C4 O1 Tc1 116.54(16) . . ? C1 N1 C3 106.6(2) . . ? C1 N1 Tc1 138.7(2) . . ? C3 N1 Tc1 113.41(16) . . ? C1 N2 C2 108.2(2) . . ? N1 C1 N2 110.5(3) . . ? N2 C2 C3 106.1(3) . . ? C2 C3 N1 108.6(2) . . ? C2 C3 C4 133.4(3) . . ? N1 C3 C4 118.1(2) . . ? O2 C4 O1 124.0(2) . . ? O2 C4 C3 120.3(2) . . ? O1 C4 C3 115.6(3) . . ? O4 C5 Tc1 178.1(3) . . ? O5 C6 Tc1 177.9(3) . . ? O6 C7 Tc1 178.7(3) . . ? 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 C6 Tc1 O1 C4 2.1(8) . . . . ? C7 Tc1 O1 C4 -97.5(2) . . . . ? C5 Tc1 O1 C4 171.85(19) . . . . ? N1 Tc1 O1 C4 -2.84(18) . . . . ? O3 Tc1 O1 C4 80.11(18) . . . . ? C6 Tc1 N1 C1 -7.8(3) . . . . ? C7 Tc1 N1 C1 -96.9(3) . . . . ? C5 Tc1 N1 C1 121.2(9) . . . . ? O3 Tc1 N1 C1 88.1(3) . . . . ? O1 Tc1 N1 C1 171.6(3) . . . . ? C6 Tc1 N1 C3 -172.79(19) . . . . ? C7 Tc1 N1 C3 98.1(2) . . . . ? C5 Tc1 N1 C3 -43.8(10) . . . . ? O3 Tc1 N1 C3 -76.92(18) . . . . ? O1 Tc1 N1 C3 6.52(17) . . . . ? C3 N1 C1 N2 1.0(3) . . . . ? Tc1 N1 C1 N2 -164.7(2) . . . . ? C2 N2 C1 N1 -1.1(3) . . . . ? C1 N2 C2 C3 0.7(3) . . . . ? N2 C2 C3 N1 -0.1(3) . . . . ? N2 C2 C3 C4 178.5(3) . . . . ? C1 N1 C3 C2 -0.5(3) . . . . ? Tc1 N1 C3 C2 169.25(18) . . . . ? C1 N1 C3 C4 -179.4(2) . . . . ? Tc1 N1 C3 C4 -9.7(3) . . . . ? Tc1 O1 C4 O2 178.7(2) . . . . ? Tc1 O1 C4 C3 -1.3(3) . . . . ? C2 C3 C4 O2 8.8(5) . . . . ? N1 C3 C4 O2 -172.6(2) . . . . ? C2 C3 C4 O1 -171.2(3) . . . . ? N1 C3 C4 O1 7.4(4) . . . . ? C6 Tc1 C5 O4 17(9) . . . . ? C7 Tc1 C5 O4 105(9) . . . . ? N1 Tc1 C5 O4 -113(9) . . . . ? O3 Tc1 C5 O4 -80(9) . . . . ? O1 Tc1 C5 O4 -162(9) . . . . ? C7 Tc1 C6 O5 59(8) . . . . ? C5 Tc1 C6 O5 150(8) . . . . ? N1 Tc1 C6 O5 -36(8) . . . . ? O3 Tc1 C6 O5 -118(8) . . . . ? O1 Tc1 C6 O5 -41(9) . . . . ? C6 Tc1 C7 O6 153(15) . . . . ? C5 Tc1 C7 O6 65(15) . . . . ? N1 Tc1 C7 O6 -110(14) . . . . ? O3 Tc1 C7 O6 -57(15) . . . . ? O1 Tc1 C7 O6 -35(15) . . . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 25.90 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 1.068 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.106 data_10 _database_code_depnum_ccdc_archive 'CCDC 228232' _audit_creation_method SHELXL-97 _chemical_name_systematic Re(I)(2,4-Pyridinedicarboxylicacid)(benzylisocyanide)(CO)3 _chemical_name_common Re(i)(2,4-Pyridinedicarboxylicacid)(benzylisocyanide)(CO)3 _chemical_melting_point ? _chemical_formula_moiety 'C18 H11 N2 O7 Re' _chemical_formula_sum 'C18 H11 N2 O7 Re' _chemical_formula_weight 553.49 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.232(11) _cell_length_b 13.240(5) _cell_length_c 14.296(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.13(6) _cell_angle_gamma 90.00 _cell_volume 3744(3) _cell_formula_units_Z 8 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.964 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 6.534 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.2446 _exptl_absorpt_correction_T_max 0.8804 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method '/f oscillation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 50-200 _diffrn_standards_interval_count image _diffrn_standards_interval_time 6 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18625 _diffrn_reflns_av_R_equivalents 0.0607 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 28.03 _reflns_number_total 4500 _reflns_number_gt 3194 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (Stoe, 1999)' _computing_cell_refinement 'IPDS (Stoe, 1999)' _computing_data_reduction 'X-Red (Stoe, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Zortep (Zsolnai, 1994), Platon (Spek, 1993)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4500 _refine_ls_number_parameters 280 _refine_ls_number_restraints 59 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0914 _refine_ls_wR_factor_gt 0.0866 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.913 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re Re -0.336679(12) 0.146719(19) 0.107943(16) 0.03813(9) Uani 1 1 d . . . C1 C -0.3227(3) 0.3069(4) 0.2597(4) 0.0354(12) Uani 1 1 d . . . C2 C -0.3193(4) 0.3626(5) 0.1683(4) 0.0439(15) Uani 1 1 d . . . C3 C -0.3194(3) 0.3581(5) 0.3446(4) 0.0378(12) Uani 1 1 d . . . H3 H -0.3108 0.4287 0.3481 0.045 Uiso 1 1 calc R . . C4 C -0.3289(3) 0.3055(5) 0.4252(4) 0.0371(13) Uani 1 1 d . . . C5 C -0.3295(4) 0.3584(5) 0.5183(4) 0.0454(15) Uani 1 1 d . . . C6 C -0.3391(4) 0.2015(5) 0.4166(4) 0.0439(15) Uani 1 1 d . . . H6 H -0.3455 0.1629 0.4699 0.053 Uiso 1 1 calc R . . C7 C -0.3397(4) 0.1550(5) 0.3301(4) 0.0432(14) Uani 1 1 d . . . H7 H -0.3455 0.0838 0.3257 0.052 Uiso 1 1 calc R . . C8 C -0.2299(3) 0.1485(5) 0.1408(4) 0.0394(12) Uani 1 1 d . . . C21 C -0.0599(7) 0.2248(9) 0.2062(8) 0.055(3) Uiso 0.50 1 d PD A 1 C22 C -0.0643(7) 0.2735(10) 0.2892(9) 0.074(5) Uiso 0.50 1 d PD . 1 C23 C -0.0323(12) 0.3641(13) 0.3131(12) 0.160(17) Uiso 0.50 1 d PD . 1 C24 C 0.0000 0.4094(13) 0.2500 0.160(9) Uiso 1 2 d SD . 1 C25 C 0.0099(14) 0.3579(12) 0.1700(12) 0.101(8) Uiso 0.50 1 d PD . 1 C26 C -0.0227(9) 0.2666(10) 0.1455(10) 0.078(5) Uiso 0.50 1 d PD . 1 C9B C -0.1007(9) 0.1306(13) 0.2100(14) 0.065(5) Uiso 0.50 1 d PDU A 1 C9A C -0.1003(7) 0.1505(13) 0.1580(16) 0.073(5) Uani 0.50 1 d PD A 2 C11 C -0.0663(6) 0.0531(10) 0.1853(9) 0.058(4) Uani 0.50 1 d PD A 2 C12 C -0.0413(7) -0.0063(12) 0.1167(13) 0.083(6) Uani 0.50 1 d PD . 2 C13 C -0.0105(8) -0.1002(15) 0.1521(10) 0.123(12) Uani 0.50 1 d PD . 2 C14 C 0.0000 -0.1332(15) 0.2500 0.120(8) Uani 1 2 d SD . 2 C15 C -0.0270(10) -0.0783(11) 0.3184(16) 0.113(10) Uani 0.50 1 d PD . 2 C16 C -0.0585(7) 0.0132(11) 0.2796(9) 0.058(4) Uani 0.50 1 d PD A 2 C27 C -0.3373(3) 0.1128(6) -0.0247(5) 0.0481(16) Uani 1 1 d . . . O27 O -0.3365(3) 0.0924(4) -0.1019(3) 0.0649(15) Uani 1 1 d . . . C28 C -0.3346(3) 0.0052(6) 0.1358(5) 0.0509(17) Uani 1 1 d . . . O28 O -0.3336(3) -0.0809(4) 0.1526(5) 0.0683(15) Uani 1 1 d . . . C29 C -0.4356(4) 0.1437(7) 0.0835(5) 0.062(2) Uani 1 1 d . . . O29 O -0.4933(3) 0.1370(7) 0.0719(6) 0.105(3) Uani 1 1 d . . . N1 N -0.3324(3) 0.2064(4) 0.2519(3) 0.0353(10) Uani 1 1 d . . . N2 N -0.1720(3) 0.1465(4) 0.1605(5) 0.0550(15) Uani 1 1 d U . . O1 O -0.3299(3) 0.3083(4) 0.0919(3) 0.0476(11) Uani 1 1 d . . . O2 O -0.3093(3) 0.4541(3) 0.1726(3) 0.0661(16) Uani 1 1 d . . . O3 O -0.3437(4) 0.3171(5) 0.5850(4) 0.086(2) Uani 1 1 d . . . O4 O -0.3093(4) 0.4530(4) 0.5165(3) 0.0723(18) Uani 1 1 d . . . H4 H -0.307(5) 0.491(9) 0.577(8) 0.11(4) Uiso 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 Re 0.04040(13) 0.03933(14) 0.03397(12) -0.01134(11) 0.00620(8) 0.00106(12) C1 0.050(3) 0.027(3) 0.029(2) 0.000(2) 0.010(2) 0.000(3) C2 0.072(4) 0.032(3) 0.028(3) 0.001(2) 0.013(3) 0.006(3) C3 0.058(4) 0.027(3) 0.030(2) 0.001(2) 0.011(2) -0.001(3) C4 0.048(3) 0.034(3) 0.030(3) 0.001(2) 0.009(2) -0.004(3) C5 0.069(4) 0.036(3) 0.036(3) -0.004(3) 0.021(3) -0.001(3) C6 0.068(4) 0.034(3) 0.034(3) 0.007(2) 0.019(3) -0.006(3) C7 0.066(4) 0.024(3) 0.041(3) -0.004(2) 0.014(3) -0.006(3) C8 0.041(3) 0.034(3) 0.043(3) 0.002(3) 0.009(2) -0.001(3) C9A 0.029(6) 0.082(13) 0.105(15) 0.015(11) 0.005(8) -0.009(8) C11 0.037(7) 0.053(9) 0.084(10) -0.003(8) 0.015(7) -0.011(6) C12 0.047(9) 0.113(17) 0.088(13) -0.002(11) 0.010(9) -0.024(10) C13 0.023(8) 0.15(2) 0.20(3) -0.07(2) 0.026(13) -0.010(12) C14 0.061(9) 0.107(15) 0.17(2) 0.000 -0.032(12) 0.000 C15 0.058(13) 0.070(15) 0.23(3) -0.024(17) 0.066(17) -0.027(11) C16 0.046(8) 0.059(10) 0.067(9) -0.004(7) 0.008(7) -0.020(7) C27 0.049(4) 0.054(4) 0.037(3) -0.013(3) 0.001(3) 0.011(3) O27 0.076(4) 0.072(4) 0.045(3) -0.019(2) 0.008(2) 0.010(3) C28 0.044(4) 0.055(5) 0.058(4) -0.024(3) 0.018(3) -0.009(3) O28 0.078(4) 0.038(3) 0.095(4) -0.016(3) 0.035(3) -0.013(3) C29 0.044(4) 0.086(6) 0.056(4) -0.028(4) 0.008(3) 0.006(4) O29 0.043(3) 0.153(8) 0.114(6) -0.041(5) 0.007(3) 0.008(4) N1 0.048(3) 0.028(3) 0.030(2) -0.0044(18) 0.0109(19) -0.003(2) N2 0.041(3) 0.037(3) 0.084(4) -0.001(3) 0.007(3) -0.003(3) O1 0.077(3) 0.039(2) 0.0274(19) -0.0018(17) 0.013(2) 0.011(2) O2 0.141(5) 0.030(3) 0.033(2) 0.0042(18) 0.031(3) 0.007(3) O3 0.179(7) 0.049(3) 0.044(3) -0.006(2) 0.058(4) -0.029(4) O4 0.147(6) 0.042(3) 0.037(2) -0.011(2) 0.042(3) -0.020(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C28 1.914(8) . ? Re C27 1.947(6) . ? Re C29 1.958(7) . ? Re C8 2.112(6) . ? Re O1 2.158(5) . ? Re N1 2.189(4) . ? C1 N1 1.347(7) . ? C1 C3 1.379(8) . ? C1 C2 1.514(8) . ? C2 O2 1.227(8) . ? C2 O1 1.288(7) . ? C3 C4 1.394(8) . ? C4 C6 1.394(9) . ? C4 C5 1.506(8) . ? C5 O3 1.185(8) . ? C5 O4 1.319(8) . ? C6 C7 1.379(8) . ? C7 N1 1.342(7) . ? C8 N2 1.146(8) . ? C21 C22 1.371(10) . ? C21 C26 1.378(10) . ? C21 C9B 1.504(15) . ? C22 C23 1.371(11) . ? C22 C25 1.59(3) 2 ? C22 C26 1.81(2) 2 ? C23 C25 0.47(4) 2 ? C23 C24 1.360(11) . ? C23 C26 1.73(3) 2 ? C24 C23 1.360(11) 2 ? C24 C25 1.381(11) . ? C24 C25 1.381(11) 2 ? C25 C23 0.47(4) 2 ? C25 C26 1.387(11) . ? C25 C22 1.59(3) 2 ? C26 C23 1.73(3) 2 ? C26 C22 1.81(2) 2 ? C9B N2 1.48(2) . ? C9A N2 1.460(16) . ? C9A C11 1.475(16) . ? C11 C16 1.425(10) . ? C11 C12 1.431(10) . ? C12 C13 1.434(10) . ? C12 C15 1.77(2) 2 ? C13 C15 0.84(2) 2 ? C13 C14 1.439(10) . ? C14 C15 1.417(11) 2 ? C14 C15 1.417(11) . ? C14 C13 1.439(10) 2 ? C15 C13 0.84(2) 2 ? C15 C16 1.427(11) . ? C15 C12 1.77(2) 2 ? C27 O27 1.139(8) . ? C28 O28 1.165(10) . ? C29 O29 1.147(9) . ? 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 C28 Re C27 88.4(3) . . ? C28 Re C29 89.7(3) . . ? C27 Re C29 91.4(3) . . ? C28 Re C8 89.3(3) . . ? C27 Re C8 90.9(3) . . ? C29 Re C8 177.5(3) . . ? C28 Re O1 173.2(2) . . ? C27 Re O1 96.5(3) . . ? C29 Re O1 95.0(3) . . ? C8 Re O1 85.8(2) . . ? C28 Re N1 99.4(2) . . ? C27 Re N1 172.0(3) . . ? C29 Re N1 90.7(2) . . ? C8 Re N1 87.2(2) . . ? O1 Re N1 75.62(16) . . ? N1 C1 C3 122.5(5) . . ? N1 C1 C2 116.2(5) . . ? C3 C1 C2 121.1(5) . . ? O2 C2 O1 126.1(5) . . ? O2 C2 C1 118.3(5) . . ? O1 C2 C1 115.5(5) . . ? C1 C3 C4 119.5(6) . . ? C6 C4 C3 117.6(5) . . ? C6 C4 C5 120.6(5) . . ? C3 C4 C5 121.8(6) . . ? O3 C5 O4 125.6(6) . . ? O3 C5 C4 123.0(6) . . ? O4 C5 C4 111.3(5) . . ? C7 C6 C4 119.6(5) . . ? N1 C7 C6 122.6(5) . . ? N2 C8 Re 177.6(6) . . ? C22 C21 C26 120.1(5) . . ? C22 C21 C9B 102.9(10) . . ? C26 C21 C9B 137.1(11) . . ? C21 C22 C23 120.9(5) . . ? C21 C22 C25 118.8(6) . 2 ? C23 C22 C25 16.3(12) . 2 ? C21 C22 C26 100.9(10) . 2 ? C23 C22 C26 63.9(10) . 2 ? C25 C22 C26 47.5(7) 2 2 ? C25 C23 C24 82.6(16) 2 . ? C25 C23 C22 109(3) 2 . ? C24 C23 C22 119.2(5) . . ? C25 C23 C26 39(3) 2 2 ? C24 C23 C26 101.1(14) . 2 ? C22 C23 C26 70.6(10) . 2 ? C23 C24 C23 127.6(14) 2 . ? C23 C24 C25 19.9(17) 2 . ? C23 C24 C25 120.3(6) . . ? C23 C24 C25 120.3(6) 2 2 ? C23 C24 C25 19.9(17) . 2 ? C25 C24 C25 120.8(15) . 2 ? C23 C25 C24 77.5(13) 2 . ? C23 C25 C26 129(4) 2 . ? C24 C25 C26 119.8(5) . . ? C23 C25 C22 55(3) 2 2 ? C24 C25 C22 104.7(16) . 2 ? C26 C25 C22 74.7(14) . 2 ? C21 C26 C25 118.9(5) . . ? C21 C26 C23 118.8(6) . 2 ? C25 C26 C23 12.3(14) . 2 ? C21 C26 C22 107.2(11) . 2 ? C25 C26 C22 57.8(14) . 2 ? C23 C26 C22 45.5(7) 2 2 ? N2 C9B C21 110.6(13) . . ? N2 C9A C11 111.8(12) . . ? C16 C11 C12 117.4(13) . . ? C16 C11 C9A 121.8(14) . . ? C12 C11 C9A 120.8(15) . . ? C11 C12 C13 115.1(16) . . ? C11 C12 C15 106.6(11) . 2 ? C13 C12 C15 27.8(9) . 2 ? C15 C13 C12 99.1(19) 2 . ? C15 C13 C14 71.6(8) 2 . ? C12 C13 C14 124.9(18) . . ? C15 C14 C15 118(2) 2 . ? C15 C14 C13 34.1(10) 2 . ? C15 C14 C13 121.1(18) . . ? C15 C14 C13 121.1(18) 2 2 ? C15 C14 C13 34.1(10) . 2 ? C13 C14 C13 145(2) . 2 ? C13 C15 C14 74.4(8) 2 . ? C13 C15 C16 141(2) 2 . ? C14 C15 C16 111.9(18) . . ? C13 C15 C12 53.1(14) 2 2 ? C14 C15 C12 105.5(12) . 2 ? C16 C15 C12 89.0(11) . 2 ? C11 C16 C15 129.4(16) . . ? O27 C27 Re 178.8(6) . . ? O28 C28 Re 179.7(7) . . ? O29 C29 Re 176.2(9) . . ? C7 N1 C1 118.1(5) . . ? C7 N1 Re 127.6(4) . . ? C1 N1 Re 114.2(3) . . ? C8 N2 C9A 164.3(11) . . ? C8 N2 C9B 164.4(10) . . ? C9A N2 C9B 31.1(9) . . ? C2 O1 Re 117.8(4) . . ? 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 N1 C1 C2 O2 -178.7(7) . . . . ? C3 C1 C2 O2 4.6(10) . . . . ? N1 C1 C2 O1 3.6(9) . . . . ? C3 C1 C2 O1 -173.1(6) . . . . ? N1 C1 C3 C4 -2.3(10) . . . . ? C2 C1 C3 C4 174.1(6) . . . . ? C1 C3 C4 C6 2.1(9) . . . . ? C1 C3 C4 C5 -176.7(6) . . . . ? C6 C4 C5 O3 -6.1(11) . . . . ? C3 C4 C5 O3 172.7(8) . . . . ? C6 C4 C5 O4 170.8(7) . . . . ? C3 C4 C5 O4 -10.4(9) . . . . ? C3 C4 C6 C7 -0.2(10) . . . . ? C5 C4 C6 C7 178.6(6) . . . . ? C4 C6 C7 N1 -1.7(11) . . . . ? C28 Re C8 N2 -24(14) . . . . ? C27 Re C8 N2 -112(14) . . . . ? C29 Re C8 N2 43(18) . . . . ? O1 Re C8 N2 151(14) . . . . ? N1 Re C8 N2 76(14) . . . . ? C26 C21 C22 C23 0.2(16) . . . . ? C9B C21 C22 C23 179.2(15) . . . . ? C26 C21 C22 C25 -18(2) . . . 2 ? C9B C21 C22 C25 160.5(14) . . . 2 ? C26 C21 C22 C26 -65.7(13) . . . 2 ? C9B C21 C22 C26 113.3(11) . . . 2 ? C21 C22 C23 C25 -87(2) . . . 2 ? C26 C22 C23 C25 0.0(14) 2 . . 2 ? C21 C22 C23 C24 5(2) . . . . ? C25 C22 C23 C24 92(2) 2 . . . ? C26 C22 C23 C24 92.2(19) 2 . . . ? C21 C22 C23 C26 -87.2(11) . . . 2 ? C25 C22 C23 C26 0.0(14) 2 . . 2 ? C25 C23 C24 C23 75(3) 2 . . 2 ? C22 C23 C24 C23 -32.7(12) . . . 2 ? C26 C23 C24 C23 41.1(7) 2 . . 2 ? C25 C23 C24 C25 97(4) 2 . . . ? C22 C23 C24 C25 -10(3) . . . . ? C26 C23 C24 C25 64(2) 2 . . . ? C22 C23 C24 C25 -108(3) . . . 2 ? C26 C23 C24 C25 -34(3) 2 . . 2 ? C23 C24 C25 C23 -118(3) . . . 2 ? C25 C24 C25 C23 -94(3) 2 . . 2 ? C23 C24 C25 C26 128(5) 2 . . . ? C23 C24 C25 C26 11(3) . . . . ? C25 C24 C25 C26 33.8(18) 2 . . . ? C23 C24 C25 C22 48(3) 2 . . 2 ? C23 C24 C25 C22 -70(2) . . . 2 ? C25 C24 C25 C22 -46.7(8) 2 . . 2 ? C22 C21 C26 C25 0(3) . . . . ? C9B C21 C26 C25 -178(2) . . . . ? C22 C21 C26 C23 14(2) . . . 2 ? C9B C21 C26 C23 -164.5(17) . . . 2 ? C22 C21 C26 C22 62.2(14) . . . 2 ? C9B C21 C26 C22 -116.3(18) . . . 2 ? C23 C25 C26 C21 93(2) 2 . . . ? C24 C25 C26 C21 -5(3) . . . . ? C22 C25 C26 C21 92.9(17) 2 . . . ? C24 C25 C26 C23 -98(4) . . . 2 ? C22 C25 C26 C23 0.0(18) 2 . . 2 ? C23 C25 C26 C22 0.0(18) 2 . . 2 ? C24 C25 C26 C22 -98(2) . . . 2 ? C22 C21 C9B N2 92.1(14) . . . . ? C26 C21 C9B N2 -89(2) . . . . ? N2 C9A C11 C16 -66.1(19) . . . . ? N2 C9A C11 C12 112.4(16) . . . . ? C16 C11 C12 C13 -0.3(12) . . . . ? C9A C11 C12 C13 -178.9(13) . . . . ? C16 C11 C12 C15 -28.8(13) . . . 2 ? C9A C11 C12 C15 152.7(12) . . . 2 ? C11 C12 C13 C15 -77.9(15) . . . 2 ? C11 C12 C13 C14 -4.0(14) . . . . ? C15 C12 C13 C14 73.8(16) 2 . . . ? C12 C13 C14 C15 -88(2) . . . 2 ? C15 C13 C14 C15 95(2) 2 . . . ? C12 C13 C14 C15 7.1(18) . . . . ? C15 C13 C14 C13 60.7(17) 2 . . 2 ? C12 C13 C14 C13 -27.6(10) . . . 2 ? C15 C14 C15 C13 -104.5(19) 2 . . 2 ? C13 C14 C15 C13 -144(2) . . . 2 ? C15 C14 C15 C16 34.3(9) 2 . . . ? C13 C14 C15 C16 -5.0(19) . . . . ? C13 C14 C15 C16 139(3) 2 . . . ? C15 C14 C15 C12 -61.0(9) 2 . . 2 ? C13 C14 C15 C12 -100.2(14) . . . 2 ? C13 C14 C15 C12 43.6(17) 2 . . 2 ? C12 C11 C16 C15 2(2) . . . . ? C9A C11 C16 C15 -179.4(15) . . . . ? C13 C15 C16 C11 93(3) 2 . . . ? C14 C15 C16 C11 1(2) . . . . ? C12 C15 C16 C11 107.0(16) 2 . . . ? C28 Re C27 O27 -74(37) . . . . ? C29 Re C27 O27 -164(37) . . . . ? C8 Re C27 O27 15(37) . . . . ? O1 Re C27 O27 101(37) . . . . ? N1 Re C27 O27 91(36) . . . . ? C27 Re C28 O28 -88(100) . . . . ? C29 Re C28 O28 3(100) . . . . ? C8 Re C28 O28 -179(100) . . . . ? O1 Re C28 O28 136(100) . . . . ? N1 Re C28 O28 94(100) . . . . ? C28 Re C29 O29 19(10) . . . . ? C27 Re C29 O29 107(10) . . . . ? C8 Re C29 O29 -48(14) . . . . ? O1 Re C29 O29 -156(10) . . . . ? N1 Re C29 O29 -81(10) . . . . ? C6 C7 N1 C1 1.5(10) . . . . ? C6 C7 N1 Re -177.0(5) . . . . ? C3 C1 N1 C7 0.5(9) . . . . ? C2 C1 N1 C7 -176.1(6) . . . . ? C3 C1 N1 Re 179.2(5) . . . . ? C2 C1 N1 Re 2.6(7) . . . . ? C28 Re N1 C7 -11.1(6) . . . . ? C27 Re N1 C7 -176.5(15) . . . . ? C29 Re N1 C7 78.7(6) . . . . ? C8 Re N1 C7 -99.9(6) . . . . ? O1 Re N1 C7 173.7(6) . . . . ? C28 Re N1 C1 170.3(5) . . . . ? C27 Re N1 C1 5.0(19) . . . . ? C29 Re N1 C1 -99.9(5) . . . . ? C8 Re N1 C1 81.5(5) . . . . ? O1 Re N1 C1 -4.9(4) . . . . ? Re C8 N2 C9A 138(13) . . . . ? Re C8 N2 C9B -28(16) . . . . ? C11 C9A N2 C8 -119(3) . . . . ? C11 C9A N2 C9B 53.6(18) . . . . ? C21 C9B N2 C8 -133(3) . . . . ? C21 C9B N2 C9A 53.7(19) . . . . ? O2 C2 O1 Re 174.4(6) . . . . ? C1 C2 O1 Re -8.2(8) . . . . ? C28 Re O1 C2 -36(2) . . . . ? C27 Re O1 C2 -171.3(5) . . . . ? C29 Re O1 C2 96.7(5) . . . . ? C8 Re O1 C2 -80.9(5) . . . . ? N1 Re O1 C2 7.3(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 O4 H4 O2 0.99(12) 1.56(12) 2.549(6) 175(10) 6_566 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.03 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.689 _refine_diff_density_min -0.754 _refine_diff_density_rms 0.178