# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Peter Klufers' _publ_contact_author_email KLUEF@CUP.UNI-MUENCHEN.DE _publ_section_title ; Oxidorhenium(V) Complexes with L-Histidine and Pyranosides ; loop_ _publ_author_name 'Peter Klufers' 'Philipp Grimminger' data_jn213 _database_code_depnum_ccdc_archive 'CCDC 737570' ################################################################################ # start Validation Reply Form _vrf_PLAT245_jn213 ; PROBLEM: U(iso) H981 Smaller than U(eq) C98 by ... 0.05 AngSq RESPONSE: one common isotropic displacement factor was refined for all H atoms to account for comparable thermal motions. ; _vrf_PLAT601_jn213 ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 73.00 A**3 RESPONSE: situation was checked several times, no significant solvent accessible voids were identified. ; # end Validation Reply Form ################################################################################ #:---------------------------------------------------------------------------- #:------------------------------CRYSTAL SOURCE-------------------------------- #:---------------------------------------------------------------------------- _audit_update_record 12-FEB-07 _chemical_name_common ReO(His)(MeaDManp) _chemical_compound_source ; 0.833 g (1.0 mmol) of the Rhenium(V)-oxo-complex trans-ReOCl3(PPh3)2 were stirred with 0.388 g (2.0 mmol) methyl-\a-D-mannopyranoside, 0.155 g (1.0 mmol) L-histidine and 0.303 g (3.0 mmol) triethylamine in 250 ml methanol. After stirring for 2 hours at 50 \%C the yellow suspension turned into a blue solution. Then the volume was reduced in vakuo to 30 ml. A blue powder of (I) was filtered off and recrystallised in methanol. ; _exptl_crystal_description platelet _exptl_crystal_colour violet _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_method 'not measured' _exptl_crystal_density_meas ? _exptl_special_details ? #:---------------------------------------------------------------------------- #:---------------------------DATA COLLECTION---------------------------------- #:---------------------------------------------------------------------------- _audit_author_name 'Albrecht, S.' _audit_creation_date 30-Juni-05 _diffrn_ambient_temperature 200(2) _diffrn_source_type 'FR 591 generator' _diffrn_source_power 4.125 _diffrn_source_voltage 55.00 _diffrn_source_current 75.00 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation 0.35 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD; rotation images; thick slices' _diffrn_detector_area_resol_mean 9 _kl_diffrn_measurement_scan_angle phi/omega-scan _kl_diffrn_measurement_scan_step_degree 2.0 _kl_diffrn_measurement_scan_time_per_degree 30 _kl_diffrn_measurement_detector_distance 35 _diffrn_special_details ? _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_UB_11 -0.0024377 _diffrn_orient_matrix_UB_12 -0.0815764 _diffrn_orient_matrix_UB_13 0.0615719 _diffrn_orient_matrix_UB_21 0.0423847 _diffrn_orient_matrix_UB_22 0.0108926 _diffrn_orient_matrix_UB_23 0.0601631 _diffrn_orient_matrix_UB_31 -0.0090113 _diffrn_orient_matrix_UB_32 0.0733015 _diffrn_orient_matrix_UB_33 0.0595824 loop_ _reflns_scale_group_code _reflns_scale_meas_F 1 1.0 _cell_length_a 25.2622(4) _cell_length_b 9.0735(2) _cell_length_c 10.4724(2) _cell_angle_alpha 90.00 _cell_angle_beta 114.2054(9) _cell_angle_gamma 90.00 _cell_volume 2189.40(7) _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 14780 _cell_measurement_theta_min 3.134 _cell_measurement_theta_max 27.485 _cell_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.0239 -1 0 0 0.0260 -29 -1 13 0.0780 30 -1 -19 0.0650 15 28 3 0.0550 -15 -22 0 0.0550 #:---------------------------------------------------------------------------- #:---------------------------ABSORPTION CORRECTION---------------------------- #:---------------------------------------------------------------------------- _exptl_absorpt_coefficient_mu 5.610 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4851 _exptl_absorpt_correction_T_max 0.7705 _exptl_absorpt_process_details ; Crystal faces optimized with XShape, rev. 1.02, STOE (Darmstadt, Germany) Absorption correction with XRed, rev 1.09, STOE (Darmstadt, Germany) ; #:---------------------------------------------------------------------------- #:------------------------REFLECTION DATA ANALYSIS---------------------------- #:---------------------------------------------------------------------------- _diffrn_reflns_number 19131 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.992 #:---------------------------------------------------------------------------- #:---------------------STRUCTURE SOLUTION AND REFINEMENT---------------------- #:---------------------------------------------------------------------------- _symmetry_cell_setting monoclinic #triclinic, monoclinic, orthorhombic, tetragonal #rhombohedral, trigonal, hexagonal, cubic _symmetry_space_group_name_H-M 'C 2' _symmetry_space_group_name_Hall 'C 2y' _symmetry_Int_Tables_number 5 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' 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' _reflns_number_total 4484 _reflns_number_gt 4106 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _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^)+(0.0172P)^2^+1.8116P] 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 refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.041(14) _refine_ls_number_reflns 4484 _refine_ls_number_parameters 234 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0879 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.542 _refine_diff_density_min -1.782 _refine_diff_density_rms 0.185 _refine_special_details ? #:---------------------------------------------------------------------------- #:-----------------------------REFERENCES------------------------------------- #:---------------------------------------------------------------------------- _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution ; A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A. Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for crystal structure determination and refinement; J. Appl. Crystallogr. 1999, 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ? _computing_publication_material ? #:---------------------------------------------------------------------------- #:---------------------TABLES AND GEOMETRICAL DATA---------------------------- #:---------------------------------------------------------------------------- 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 0.212308(5) 0.69413(3) 0.140783(10) 0.01552(5) Uani 1 1 d . . . O1 O 0.24601(12) 0.8551(3) 0.1422(3) 0.0237(6) Uani 1 1 d . . . C11 C 0.05610(16) 0.7538(5) -0.2036(4) 0.0227(9) Uani 1 1 d . . . H11 H 0.0645 0.7004 -0.2768 0.046(3) Uiso 1 1 calc R . . O11 O -0.00203(11) 0.7247(3) -0.2247(3) 0.0259(9) Uani 1 1 d . . . C21 C 0.09368(13) 0.6882(9) -0.0605(3) 0.0180(7) Uani 1 1 d . . . H21 H 0.0780 0.5891 -0.0525 0.046(3) Uiso 1 1 calc R . . O21 O 0.15249(10) 0.6712(4) -0.0493(2) 0.0188(8) Uani 1 1 d . . . C31 C 0.09568(17) 0.7854(5) 0.0618(4) 0.0188(8) Uani 1 1 d . . . H31 H 0.0601 0.7661 0.0789 0.046(3) Uiso 1 1 calc R . . O31 O 0.14608(11) 0.7373(3) 0.1828(2) 0.0190(7) Uani 1 1 d . . . C41 C 0.09902(17) 0.9494(5) 0.0354(4) 0.0201(8) Uani 1 1 d . . . H41 H 0.1390 0.9740 0.0445 0.046(3) Uiso 1 1 calc R . . O41 O 0.08802(18) 1.0250(4) 0.1405(4) 0.0255(9) Uani 1 1 d . . . H841 H 0.0844 1.1156 0.1222 0.046(3) Uiso 1 1 calc R . . C51 C 0.05535(18) 0.9921(5) -0.1098(4) 0.0205(9) Uani 1 1 d . . . H51 H 0.0156 0.9679 -0.1168 0.046(3) Uiso 1 1 calc R . . O51 O 0.06602(12) 0.9045(3) -0.2126(3) 0.0214(6) Uani 1 1 d . . . C61 C 0.05600(18) 1.1520(4) -0.1484(4) 0.0258(10) Uani 1 1 d . . . H612 H 0.0280 1.1677 -0.2466 0.046(3) Uiso 1 1 calc R . . H611 H 0.0439 1.2142 -0.0874 0.046(3) Uiso 1 1 calc R . . O61 O 0.11267(11) 1.1939(7) -0.1330(3) 0.0359(6) Uani 1 1 d . . . H861 H 0.1130 1.2844 -0.1496 0.046(3) Uiso 1 1 calc R . . C71 C -0.0444(2) 0.7724(6) -0.3559(5) 0.0394(12) Uani 1 1 d . . . H711 H -0.0420 0.8796 -0.3633 0.046(3) Uiso 1 1 calc R . . H712 H -0.0831 0.7453 -0.3634 0.046(3) Uiso 1 1 calc R . . H713 H -0.0373 0.7251 -0.4315 0.046(3) Uiso 1 1 calc R . . C12 C 0.23869(18) 0.3673(4) 0.1750(4) 0.0185(8) Uani 1 1 d . . . O121 O 0.19581(12) 0.4590(3) 0.1496(3) 0.0208(6) Uani 1 1 d . . . O122 O 0.23751(13) 0.2366(3) 0.2014(3) 0.0282(7) Uani 1 1 d . . . C22 C 0.29293(17) 0.4385(4) 0.1736(4) 0.0188(8) Uani 1 1 d . . . H22 H 0.3117 0.3688 0.1309 0.046(3) Uiso 1 1 calc R . . N22 N 0.27433(14) 0.5719(4) 0.0861(3) 0.0187(7) Uani 1 1 d . . . H222 H 0.2574 0.5458 -0.0070 0.046(3) Uiso 1 1 calc R . . H221 H 0.3060 0.6302 0.1001 0.046(3) Uiso 1 1 calc R . . C32 C 0.33591(19) 0.4752(5) 0.3239(4) 0.0261(10) Uani 1 1 d . . . H321 H 0.3538 0.3824 0.3720 0.046(3) Uiso 1 1 calc R . . H322 H 0.3673 0.5375 0.3196 0.046(3) Uiso 1 1 calc R . . C42 C 0.30912(17) 0.5547(5) 0.4111(4) 0.0212(9) Uani 1 1 d . . . N52 N 0.26154(14) 0.6466(3) 0.3529(3) 0.0205(8) Uani 1 1 d . . . C62 C 0.24993(15) 0.6955(10) 0.4590(3) 0.0288(8) Uani 1 1 d . . . H62 H 0.2190 0.7602 0.4496 0.046(3) Uiso 1 1 calc R . . N72 N 0.28753(17) 0.6411(4) 0.5787(4) 0.0300(9) Uani 1 1 d . . . H772 H 0.2884 0.6600 0.6620 0.046(3) Uiso 1 1 calc R . . C82 C 0.3252(2) 0.5498(5) 0.5512(4) 0.0276(10) Uani 1 1 d . . . H82 H 0.3562 0.4945 0.6175 0.046(3) Uiso 1 1 calc R . . O98 O 0.0983(2) 0.3236(5) 0.1536(6) 0.0496(13) Uani 1 1 d . . . H898 H 0.1282 0.3597 0.1498 0.046(3) Uiso 1 1 calc R . . C98 C 0.0818(4) 0.4072(8) 0.2354(10) 0.093(3) Uani 1 1 d . . . H981 H 0.1131 0.4759 0.2884 0.046(3) Uiso 1 1 calc R . . H982 H 0.0732 0.3444 0.3006 0.046(3) Uiso 1 1 calc R . . H983 H 0.0470 0.4630 0.1774 0.046(3) Uiso 1 1 calc R . . O99 O 0.1229(2) 0.4533(5) 0.7557(4) 0.0570(11) Uani 1 1 d . . . H899 H 0.1415 0.5114 0.8213 0.046(3) Uiso 1 1 calc R . . C99 C 0.1381(4) 0.4807(11) 0.6373(7) 0.089(3) Uani 1 1 d . . . H991 H 0.1027 0.4846 0.5507 0.046(3) Uiso 1 1 calc R . . H992 H 0.1631 0.4010 0.6309 0.046(3) Uiso 1 1 calc R . . H993 H 0.1588 0.5747 0.6510 0.046(3) Uiso 1 1 calc R . . 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 0.01724(7) 0.01457(7) 0.01460(7) 0.00109(11) 0.00637(5) 0.00148(11) O1 0.0226(14) 0.0186(16) 0.0249(15) 0.0028(12) 0.0046(12) -0.0010(12) C11 0.0167(19) 0.026(2) 0.022(2) 0.0009(16) 0.0047(16) -0.0031(16) O11 0.0171(12) 0.035(3) 0.0225(13) -0.0002(12) 0.0046(10) -0.0038(13) C21 0.0165(14) 0.0179(18) 0.0217(15) 0.004(3) 0.0099(12) 0.007(3) O21 0.0173(11) 0.025(2) 0.0147(11) 0.0002(13) 0.0069(9) -0.0002(14) C31 0.0164(18) 0.021(2) 0.0182(19) -0.0010(15) 0.0063(16) 0.0003(16) O31 0.0198(13) 0.0225(18) 0.0145(12) 0.0036(10) 0.0067(10) 0.0054(11) C41 0.021(2) 0.023(2) 0.0174(19) 0.0002(16) 0.0085(16) 0.0042(17) O41 0.036(2) 0.0189(19) 0.0200(16) 0.0015(14) 0.0097(15) 0.0049(15) C51 0.0184(19) 0.024(2) 0.020(2) 0.0019(17) 0.0085(16) 0.0056(17) O51 0.0228(14) 0.0226(16) 0.0200(14) -0.0017(12) 0.0101(11) -0.0002(12) C61 0.030(2) 0.018(3) 0.027(2) 0.0039(15) 0.0087(17) 0.0055(16) O61 0.0355(14) 0.0209(13) 0.0551(16) 0.007(3) 0.0223(12) 0.003(3) C71 0.025(2) 0.054(3) 0.030(3) 0.001(2) 0.001(2) 0.002(2) C12 0.030(2) 0.014(2) 0.0134(18) 0.0005(15) 0.0100(16) 0.0040(17) O121 0.0222(14) 0.0162(15) 0.0275(15) 0.0003(11) 0.0138(12) -0.0002(12) O122 0.0391(17) 0.020(2) 0.0289(15) 0.0055(11) 0.0176(14) 0.0034(12) C22 0.024(2) 0.019(2) 0.0137(18) 0.0017(15) 0.0076(16) 0.0077(17) N22 0.0209(17) 0.0185(18) 0.0191(16) -0.0002(14) 0.0106(14) 0.0011(14) C32 0.025(2) 0.035(3) 0.017(2) 0.0011(18) 0.0073(18) 0.009(2) C42 0.022(2) 0.021(2) 0.0183(19) -0.0001(16) 0.0057(17) 0.0033(17) N52 0.0227(17) 0.020(2) 0.0167(16) -0.0012(12) 0.0061(13) 0.0042(13) C62 0.0323(19) 0.032(2) 0.0212(17) 0.002(4) 0.0099(15) 0.013(4) N72 0.042(2) 0.032(2) 0.0160(17) -0.0029(14) 0.0115(16) 0.0081(16) C82 0.031(2) 0.029(3) 0.017(2) -0.0003(18) 0.0044(17) 0.009(2) O98 0.049(3) 0.031(3) 0.089(3) -0.016(2) 0.049(3) -0.017(2) C98 0.132(7) 0.047(4) 0.162(8) -0.047(5) 0.123(7) -0.044(5) O99 0.076(3) 0.037(2) 0.060(3) -0.0108(19) 0.030(2) -0.004(2) C99 0.090(6) 0.125(8) 0.041(4) 0.006(4) 0.016(4) 0.059(6) 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 O1 1.688(3) . ? Re O31 1.936(3) . ? Re O21 1.955(2) . ? Re N52 2.098(3) . ? Re N22 2.179(3) . ? Re O121 2.183(3) . ? C11 O51 1.401(5) . ? C11 O11 1.417(5) . ? C11 C21 1.527(6) . ? C11 H11 1.0000 . ? O11 C71 1.419(5) . ? C21 O21 1.450(4) . ? C21 C31 1.539(6) . ? C21 H21 1.0000 . ? C31 O31 1.447(4) . ? C31 C41 1.523(6) . ? C31 H31 1.0000 . ? C41 O41 1.417(5) . ? C41 C51 1.518(5) . ? C41 H41 1.0000 . ? O41 H841 0.8400 . ? C51 O51 1.449(5) . ? C51 C61 1.508(6) . ? C51 H51 1.0000 . ? C61 O61 1.425(5) . ? C61 H612 0.9900 . ? C61 H611 0.9900 . ? O61 H861 0.8400 . ? C71 H711 0.9800 . ? C71 H712 0.9800 . ? C71 H713 0.9800 . ? C12 O122 1.221(5) . ? C12 O121 1.304(5) . ? C12 C22 1.520(6) . ? C22 N22 1.474(5) . ? C22 C32 1.538(6) . ? C22 H22 1.0000 . ? N22 H222 0.9200 . ? N22 H221 0.9200 . ? C32 C42 1.523(6) . ? C32 H321 0.9900 . ? C32 H322 0.9900 . ? C42 C82 1.353(6) . ? C42 N52 1.382(5) . ? N52 C62 1.336(5) . ? C62 N72 1.320(6) . ? C62 H62 0.9500 . ? N72 C82 1.378(6) . ? N72 H772 0.8800 . ? C82 H82 0.9500 . ? O98 C98 1.333(7) . ? O98 H898 0.8400 . ? C98 H981 0.9800 . ? C98 H982 0.9800 . ? C98 H983 0.9800 . ? O99 C99 1.462(8) . ? O99 H899 0.8400 . ? C99 H991 0.9800 . ? C99 H992 0.9800 . ? C99 H993 0.9800 . ? 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 O1 Re O31 107.61(12) . . ? O1 Re O21 106.11(14) . . ? O31 Re O21 82.75(10) . . ? O1 Re N52 95.21(13) . . ? O31 Re N52 89.62(12) . . ? O21 Re N52 158.64(14) . . ? O1 Re N22 91.62(14) . . ? O31 Re N22 160.73(12) . . ? O21 Re N22 90.96(12) . . ? N52 Re N22 89.77(12) . . ? O1 Re O121 161.79(12) . . ? O31 Re O121 89.44(10) . . ? O21 Re O121 81.82(13) . . ? N52 Re O121 78.16(11) . . ? N22 Re O121 71.60(12) . . ? O51 C11 O11 111.9(3) . . ? O51 C11 C21 112.9(4) . . ? O11 C11 C21 105.5(3) . . ? O51 C11 H11 108.8 . . ? O11 C11 H11 108.8 . . ? C21 C11 H11 108.8 . . ? C11 O11 C71 114.6(3) . . ? O21 C21 C11 109.0(3) . . ? O21 C21 C31 108.1(3) . . ? C11 C21 C31 112.9(5) . . ? O21 C21 H21 108.9 . . ? C11 C21 H21 108.9 . . ? C31 C21 H21 108.9 . . ? C21 O21 Re 114.18(19) . . ? O31 C31 C41 111.1(3) . . ? O31 C31 C21 105.9(3) . . ? C41 C31 C21 113.2(4) . . ? O31 C31 H31 108.9 . . ? C41 C31 H31 108.9 . . ? C21 C31 H31 108.9 . . ? C31 O31 Re 113.2(2) . . ? O41 C41 C51 111.2(3) . . ? O41 C41 C31 106.8(3) . . ? C51 C41 C31 111.1(3) . . ? O41 C41 H41 109.2 . . ? C51 C41 H41 109.2 . . ? C31 C41 H41 109.2 . . ? C41 O41 H841 109.5 . . ? O51 C51 C61 107.6(3) . . ? O51 C51 C41 108.9(3) . . ? C61 C51 C41 115.5(4) . . ? O51 C51 H51 108.2 . . ? C61 C51 H51 108.2 . . ? C41 C51 H51 108.2 . . ? C11 O51 C51 113.1(3) . . ? O61 C61 C51 110.3(4) . . ? O61 C61 H612 109.6 . . ? C51 C61 H612 109.6 . . ? O61 C61 H611 109.6 . . ? C51 C61 H611 109.6 . . ? H612 C61 H611 108.1 . . ? C61 O61 H861 109.5 . . ? O11 C71 H711 109.5 . . ? O11 C71 H712 109.5 . . ? H711 C71 H712 109.5 . . ? O11 C71 H713 109.5 . . ? H711 C71 H713 109.5 . . ? H712 C71 H713 109.5 . . ? O122 C12 O121 124.8(4) . . ? O122 C12 C22 121.4(4) . . ? O121 C12 C22 113.8(3) . . ? C12 O121 Re 118.4(3) . . ? N22 C22 C12 107.2(3) . . ? N22 C22 C32 111.7(3) . . ? C12 C22 C32 110.1(3) . . ? N22 C22 H22 109.3 . . ? C12 C22 H22 109.3 . . ? C32 C22 H22 109.3 . . ? C22 N22 Re 109.5(2) . . ? C22 N22 H222 109.8 . . ? Re N22 H222 109.8 . . ? C22 N22 H221 109.8 . . ? Re N22 H221 109.8 . . ? H222 N22 H221 108.2 . . ? C42 C32 C22 114.5(3) . . ? C42 C32 H321 108.6 . . ? C22 C32 H321 108.6 . . ? C42 C32 H322 108.6 . . ? C22 C32 H322 108.6 . . ? H321 C32 H322 107.6 . . ? C82 C42 N52 108.5(4) . . ? C82 C42 C32 128.7(4) . . ? N52 C42 C32 122.7(3) . . ? C62 N52 C42 106.3(3) . . ? C62 N52 Re 125.1(3) . . ? C42 N52 Re 128.4(3) . . ? N72 C62 N52 110.4(5) . . ? N72 C62 H62 124.8 . . ? N52 C62 H62 124.8 . . ? C62 N72 C82 108.4(4) . . ? C62 N72 H772 125.8 . . ? C82 N72 H772 125.8 . . ? C42 C82 N72 106.3(4) . . ? C42 C82 H82 126.8 . . ? N72 C82 H82 126.8 . . ? C98 O98 H898 109.5 . . ? O98 C98 H981 109.5 . . ? O98 C98 H982 109.5 . . ? H981 C98 H982 109.5 . . ? O98 C98 H983 109.5 . . ? H981 C98 H983 109.5 . . ? H982 C98 H983 109.5 . . ? C99 O99 H899 109.5 . . ? O99 C99 H991 109.5 . . ? O99 C99 H992 109.5 . . ? H991 C99 H992 109.5 . . ? O99 C99 H993 109.5 . . ? H991 C99 H993 109.5 . . ? H992 C99 H993 109.5 . . ? 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 O51 C11 O11 C71 59.1(5) . . . . ? C21 C11 O11 C71 -177.7(4) . . . . ? O51 C11 C21 O21 -75.2(6) . . . . ? O11 C11 C21 O21 162.2(4) . . . . ? O51 C11 C21 C31 44.9(5) . . . . ? O11 C11 C21 C31 -77.7(5) . . . . ? C11 C21 O21 Re 148.3(3) . . . . ? C31 C21 O21 Re 25.3(6) . . . . ? O1 Re O21 C21 -109.4(4) . . . . ? O31 Re O21 C21 -3.1(4) . . . . ? N52 Re O21 C21 66.8(6) . . . . ? N22 Re O21 C21 158.6(4) . . . . ? O121 Re O21 C21 87.4(4) . . . . ? O21 C21 C31 O31 -40.7(5) . . . . ? C11 C21 C31 O31 -161.4(3) . . . . ? O21 C21 C31 C41 81.1(5) . . . . ? C11 C21 C31 C41 -39.5(5) . . . . ? C41 C31 O31 Re -83.1(3) . . . . ? C21 C31 O31 Re 40.1(4) . . . . ? O1 Re O31 C31 82.6(2) . . . . ? O21 Re O31 C31 -22.1(2) . . . . ? N52 Re O31 C31 177.9(2) . . . . ? N22 Re O31 C31 -93.8(4) . . . . ? O121 Re O31 C31 -103.9(2) . . . . ? O31 C31 C41 O41 -73.4(4) . . . . ? C21 C31 C41 O41 167.7(3) . . . . ? O31 C31 C41 C51 165.2(3) . . . . ? C21 C31 C41 C51 46.3(4) . . . . ? O41 C41 C51 O51 -176.1(3) . . . . ? C31 C41 C51 O51 -57.3(4) . . . . ? O41 C41 C51 C61 62.7(5) . . . . ? C31 C41 C51 C61 -178.5(3) . . . . ? O11 C11 O51 C51 60.1(4) . . . . ? C21 C11 O51 C51 -58.9(4) . . . . ? C61 C51 O51 C11 -169.0(3) . . . . ? C41 C51 O51 C11 65.0(4) . . . . ? O51 C51 C61 O61 -66.3(4) . . . . ? C41 C51 C61 O61 55.6(5) . . . . ? O122 C12 O121 Re 169.5(3) . . . . ? C22 C12 O121 Re -8.6(4) . . . . ? O1 Re O121 C12 2.7(5) . . . . ? O31 Re O121 C12 -157.1(3) . . . . ? O21 Re O121 C12 120.1(3) . . . . ? N52 Re O121 C12 -67.4(3) . . . . ? N22 Re O121 C12 26.4(3) . . . . ? O122 C12 C22 N22 157.5(3) . . . . ? O121 C12 C22 N22 -24.3(4) . . . . ? O122 C12 C22 C32 -80.8(5) . . . . ? O121 C12 C22 C32 97.4(4) . . . . ? C12 C22 N22 Re 45.3(3) . . . . ? C32 C22 N22 Re -75.4(3) . . . . ? O1 Re N22 C22 134.9(2) . . . . ? O31 Re N22 C22 -48.5(5) . . . . ? O21 Re N22 C22 -119.0(3) . . . . ? N52 Re N22 C22 39.7(3) . . . . ? O121 Re N22 C22 -37.9(2) . . . . ? N22 C22 C32 C42 70.9(5) . . . . ? C12 C22 C32 C42 -48.1(5) . . . . ? C22 C32 C42 C82 150.0(5) . . . . ? C22 C32 C42 N52 -29.4(6) . . . . ? C82 C42 N52 C62 0.1(6) . . . . ? C32 C42 N52 C62 179.6(5) . . . . ? C82 C42 N52 Re -176.4(3) . . . . ? C32 C42 N52 Re 3.1(6) . . . . ? O1 Re N52 C62 85.4(5) . . . . ? O31 Re N52 C62 -22.2(5) . . . . ? O21 Re N52 C62 -90.9(6) . . . . ? N22 Re N52 C62 177.0(5) . . . . ? O121 Re N52 C62 -111.7(5) . . . . ? O1 Re N52 C42 -98.7(4) . . . . ? O31 Re N52 C42 153.7(4) . . . . ? O21 Re N52 C42 85.0(5) . . . . ? N22 Re N52 C42 -7.1(4) . . . . ? O121 Re N52 C42 64.2(3) . . . . ? C42 N52 C62 N72 0.7(7) . . . . ? Re N52 C62 N72 177.3(3) . . . . ? N52 C62 N72 C82 -1.2(7) . . . . ? N52 C42 C82 N72 -0.8(5) . . . . ? C32 C42 C82 N72 179.7(4) . . . . ? C62 N72 C82 C42 1.2(6) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? #?# use this item for nonbonding or very weakly bonding contacts, e.g.: #?# Sb1 N13 3.906(13) . . ? #?# Mn Mn 3.253(2) . 2 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag #?# Do not(!) delete the #s to obtain a table header: # #D H A D - H H...A D...A D - H...A symm(A) publ_flag N22 H221 O61 0.92 2.02 2.910(5) 161.5 4_545 ? N22 H222 O1 0.92 2.21 2.973(4) 139.3 4_545 ? N72 H772 O122 0.88 1.93 2.765(4) 157.8 4_556 ? O41 H841 O98 0.84 1.92 2.719(6) 157.8 1_565 ? O61 H861 O99 0.84 1.90 2.685(7) 155.9 1_564 ? O98 H898 O121 0.84 1.93 2.768(5) 174.6 . ? O99 H899 O21 0.84 1.92 2.717(5) 156.7 1_556 ? _geom_special_details ? #:---------------------------------------------------------------------------- #:--------------------------ARCHIVING AND CHECKING---------------------------- #:---------------------------------------------------------------------------- _audit_block_code Re_O_His_MeaDManp_jn213_grimminger _audit_creation_method 'form98_non/compatible with shelxl97-2' _chemical_name_systematic ? _chemical_formula_moiety 'C13 H20 N3 O9 Re, 2(C H4 O)' _chemical_formula_sum 'C15 H28 N3 O11 Re' _chemical_formula_weight 612.60 _chemical_melting_point ? _chemical_absolute_configuration syn _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.859 _exptl_crystal_F_000 1208 ################################################################################ data_ln077 _database_code_depnum_ccdc_archive 'CCDC 737571' ################################################################################ # start Validation Reply Form _vrf_PLAT220_ln077 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.17 Ratio RESPONSE: alert is caused by disordered solvent molecule and thus may be neglected ; _vrf_PLAT222_ln077 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 6.25 Ratio RESPONSE: alert is caused by disordered solvent molecule and thus may be neglected ; _vrf_PLAT601_ln077 ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 128.00 A**3 RESPONSE: situation checked several times, no significant solvent accessible voids were identified ; _vrf_ABSTM02_ln077 ; PROBLEM: The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.586 0.884 Tmin and Tmax expected: 0.393 0.884 RR = 1.490 Please check that your absorption correction is appropriate. RESPONSE: absorption correction was done with SADABS, the absorption correction method is appropriate ; _vrf_PLAT213_ln077 ; PROBLEM: Atom C61 has ADP max/min Ratio ............. 3.10 prola RESPONSE: alert is associated with conformationally flexible end group of carbohydrate. ; _vrf_PLAT342_ln077 ; PROBLEM: Low Bond Precision on C-C Bonds (x 1000) Ang ... 11 RESPONSE: situation checked, e.g. absorption correction was applied correctly ; _vrf_PLAT060_ln077 ; PROBLEM: Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.47 RESPONSE: absorption correction was done with SADABS, the absorption correction method is appropriate, transmission factors were reported correctly ; _vrf_PLAT077_ln077 ; PROBLEM: Unitcell contains non-integer number of atoms .. ? RESPONSE: due to a crystal packing error, refinement necessitated the presence/modelling of sub-occupied rhenium scattering sites ; _vrf_PLAT223_ln077 ; PROBLEM: Large Solvent/Anion H Ueq(max)/Ueq(min) ... 3.81 Ratio RESPONSE: alert is associated with disordered solvent molecule and thus may be neglected ; _vrf_PLAT234_ln077 ; PROBLEM: Large Hirshfeld Difference O11 -- C61 .. 0.17 Ang. RESPONSE: scattering sites assigend correctly ; _vrf_PLAT480_ln077 ; PROBLEM: Long H...A H-Bond Reported H772 .. O122 .. 2.66 Ang. RESPONSE: the respective hydrogen bond was declared in order to give a complete assignment of possibly interesting inter- and intramolecular contacts and thus might be not taken into consideration for further discussions. ; # end Validation Reply Form ################################################################################ #:---------------------------------------------------------------------------- #:------------------------------CRYSTAL SOURCE-------------------------------- #:---------------------------------------------------------------------------- _audit_update_record 09-AUG-07 _chemical_name_common ReO(His)(MebDRibp) _chemical_compound_source ; 0.833 g (1.0 mmol) of the Rhenium(V)-oxo-complex trans-ReOCl3(PPh3)2 were stirred with 0.328 g (2.0 mmol) methyl-\b-D-ribopyranoside, 0.155 g (1.0 mmol) L-histidine and 0.303 g (3.0 mmol) triethylamine in 100 ml methanol. After stirring for 3 hours at 60 \%C the yellow suspension turned into a blue solution. Then the methanol was removed in vakuo. The remaining blue solid was recrystallised in a mixture of 10 ml methanol and 1 ml of Water. At ambient Temperature blue crystals of (I) formed within 3 days. ; _exptl_crystal_description platelet _exptl_crystal_colour violet _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.02 _exptl_crystal_density_method 'not measured' _exptl_crystal_density_meas ? _exptl_special_details ? #:---------------------------------------------------------------------------- #:---------------------------DATA COLLECTION---------------------------------- #:---------------------------------------------------------------------------- _audit_author_name 'Mayer, P.' _audit_creation_date 12-Feb-07 _diffrn_ambient_temperature 200(2) _diffrn_source_type 'FR 591 generator' _diffrn_source_power 3.025 _diffrn_source_voltage 55.00 _diffrn_source_current 55.00 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'MONTEL, graded multilayered X-ray optics' _diffrn_radiation_collimation 0.20 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD; rotation images; thick slices' _diffrn_detector_area_resol_mean 9 _kl_diffrn_measurement_scan_angle phi/omega-scan _kl_diffrn_measurement_scan_step_degree 2.0 _kl_diffrn_measurement_scan_time_per_degree 8 _kl_diffrn_measurement_detector_distance 30 _diffrn_special_details ? _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_UB_11 0.0940204 _diffrn_orient_matrix_UB_12 -0.0358089 _diffrn_orient_matrix_UB_13 0.0020958 _diffrn_orient_matrix_UB_21 -0.0065008 _diffrn_orient_matrix_UB_22 0.0037137 _diffrn_orient_matrix_UB_23 -0.0675723 _diffrn_orient_matrix_UB_31 0.0225468 _diffrn_orient_matrix_UB_32 0.1503943 _diffrn_orient_matrix_UB_33 0.0021676 loop_ _reflns_scale_group_code _reflns_scale_meas_F 1 1.0 _cell_length_a 10.3763(3) _cell_length_b 6.4665(2) _cell_length_c 14.8657(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.0005(19) _cell_angle_gamma 90.00 _cell_volume 992.00(5) _cell_measurement_temperature 200(2) #?# in K _cell_measurement_reflns_used 22898 _cell_measurement_theta_min 3.134 _cell_measurement_theta_max 27.485 _cell_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 0 0.040000 0 -1 0 0.090000 -1 0 0 0.090000 1 0 0 0.090000 0 0 1 0.010000 0 0 -1 0.010000 loop_ _diffrn_radiation_wavelength_id 0.71073 #:---------------------------------------------------------------------------- #:---------------------------ABSORPTION CORRECTION---------------------------- #:---------------------------------------------------------------------------- _exptl_absorpt_coefficient_mu 6.277 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.58583 _exptl_absorpt_correction_T_max 0.884 _exptl_absorpt_process_details ; Sheldrick, G.M. SADABS. Version 2. Multi-Scan Absorption Correction Program. University of G\"ottingen, Germany, 2001. \m \\times r = 0.048164, Tmin/Tmax = 0.6627 ; #:---------------------------------------------------------------------------- #:------------------------REFLECTION DATA ANALYSIS---------------------------- #:---------------------------------------------------------------------------- _diffrn_reflns_number 17598 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 27.56 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.992 #:---------------------------------------------------------------------------- #:---------------------STRUCTURE SOLUTION AND REFINEMENT---------------------- #:---------------------------------------------------------------------------- _symmetry_cell_setting monoclinic #triclinic, monoclinic, orthorhombic, tetragonal #rhombohedral, trigonal, hexagonal, cubic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' 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' _reflns_number_total 4484 _reflns_number_gt 4106 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _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^)+(0.0488P)^2^+0.6945P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.041(14) _refine_ls_number_reflns 4484 _refine_ls_number_parameters 234 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0879 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.542 _refine_diff_density_min -1.782 _refine_diff_density_rms 0.185 _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. ; #:---------------------------------------------------------------------------- #:-----------------------------REFERENCES------------------------------------- #:---------------------------------------------------------------------------- _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution ; A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A. Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for crystal structure determination and refinement; J. Appl. Crystallogr. 1999, 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ? _computing_publication_material ? #:---------------------------------------------------------------------------- #:---------------------TABLES AND GEOMETRICAL DATA---------------------------- #:---------------------------------------------------------------------------- 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 0.192781(16) 0.20210(8) 0.065702(12) 0.02051(8) Uani 0.963(2) 1 d P . . O1 O 0.1790(4) 0.4577(8) 0.0832(3) 0.0301(11) Uani 1 1 d . . . O11 O 0.3575(8) 0.172(2) 0.4448(5) 0.093(3) Uani 1 1 d . . . C11 C 0.2967(8) 0.169(2) 0.3581(6) 0.055(3) Uani 1 1 d . . . H11 H 0.3312 0.2800 0.3206 0.066 Uiso 1 1 calc R . . C21 C 0.3120(9) -0.0404(16) 0.3163(6) 0.050(2) Uani 1 1 d . . . H21 H 0.2736 -0.1443 0.3556 0.059 Uiso 1 1 calc R . . O21 O 0.4425(6) -0.0932(11) 0.3139(4) 0.0535(16) Uani 1 1 d . . . H821 H 0.4802 0.0010 0.2878 0.080 Uiso 1 1 calc R . . C31 C 0.2359(7) -0.0522(11) 0.2235(5) 0.0354(17) Uani 1 1 d . . . H31 H 0.2321 -0.1993 0.2027 0.042 Uiso 1 1 calc R . . O31 O 0.3035(5) 0.0716(8) 0.1606(3) 0.0313(11) Uani 1 1 d . . . C41 C 0.0983(7) 0.0330(13) 0.2210(5) 0.0358(17) Uani 1 1 d . . . H41 H 0.0407 -0.0746 0.2441 0.043 Uiso 1 1 calc R . . O41 O 0.0551(4) 0.0778(7) 0.1287(3) 0.0298(11) Uani 1 1 d . . . C51 C 0.0923(7) 0.229(2) 0.2773(5) 0.047(3) Uani 1 1 d . . . H511 H 0.1316 0.3459 0.2466 0.057 Uiso 1 1 calc R . . H512 H 0.0008 0.2649 0.2835 0.057 Uiso 1 1 calc R . . O51 O 0.1607(5) 0.198(2) 0.3646(3) 0.0580(13) Uani 1 1 d . . . C61 C 0.3762(17) 0.390(3) 0.4775(11) 0.134(7) Uani 1 1 d . . . H611 H 0.4547 0.3982 0.5201 0.200 Uiso 1 1 calc R . . H612 H 0.3011 0.4325 0.5079 0.200 Uiso 1 1 calc R . . H613 H 0.3849 0.4812 0.4259 0.200 Uiso 1 1 calc R . . C12 C 0.1818(6) -0.0970(10) -0.0890(5) 0.0255(14) Uani 1 1 d . . . O121 O 0.1901(4) -0.1010(6) -0.0011(3) 0.0255(10) Uani 1 1 d . . . O122 O 0.2204(5) -0.2365(7) -0.1339(4) 0.0360(13) Uani 1 1 d . . . C22 C 0.1264(6) 0.1024(10) -0.1295(5) 0.0265(13) Uani 1 1 d . . . H22 H 0.0600 0.0707 -0.1813 0.032 Uiso 1 1 calc R . . N22 N 0.0662(4) 0.2159(16) -0.0605(3) 0.0265(12) Uani 1 1 d . . . H221 H -0.0130 0.1586 -0.0527 0.032 Uiso 1 1 calc R . . H222 H 0.0533 0.3514 -0.0781 0.032 Uiso 1 1 calc R . . C32 C 0.2382(6) 0.2311(16) -0.1638(4) 0.031(2) Uani 1 1 d . . . H321 H 0.2570 0.1775 -0.2234 0.038 Uiso 1 1 calc R . . H322 H 0.2103 0.3769 -0.1718 0.038 Uiso 1 1 calc R . . C42 C 0.3599(5) 0.2217(19) -0.0987(4) 0.0325(17) Uani 1 1 d . . . N52 N 0.3570(4) 0.2212(16) -0.0068(4) 0.0272(13) Uani 1 1 d . . . C62 C 0.4790(5) 0.2236(15) 0.0314(4) 0.0272(15) Uani 1 1 d . . . H62 H 0.5056 0.2257 0.0945 0.033 Uiso 1 1 calc R . . N72 N 0.5580(5) 0.2224(15) -0.0348(4) 0.0292(14) Uani 1 1 d . . . H772 H 0.6432 0.2179 -0.0266 0.035 Uiso 1 1 calc R . . C82 C 0.4842(5) 0.2294(13) -0.1183(4) 0.0268(17) Uani 1 1 d . . . H82 H 0.5144 0.2378 -0.1764 0.032 Uiso 1 1 calc R . . O99 O 0.6153(8) 0.2274(19) 0.2710(5) 0.032(2) Uiso 0.50 1 d P . . H899 H 0.6600 0.2358 0.2272 0.048 Uiso 0.50 1 calc PR . . C99 C 0.6813(6) 0.311(4) 0.3451(4) 0.122(11) Uiso 0.50 1 d P . . H991 H 0.7268 0.4352 0.3280 0.183 Uiso 0.50 1 calc PR . . H992 H 0.7444 0.2102 0.3724 0.183 Uiso 0.50 1 calc PR . . H993 H 0.6208 0.3475 0.3889 0.183 Uiso 0.50 1 calc PR . . Re2 Re -0.0249(6) 0.206(4) 0.1847(4) 0.033(3) Uiso 0.0271(11) 1 d PR . . Re3 Re 0.4137(6) 0.206(4) -0.0481(4) 0.017(4) Uiso 0.0157(11) 1 d PR . . Re4 Re 0.2106(6) -0.296(4) 0.2389(4) 0.039(7) Uiso 0.0123(12) 1 d PR . . 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 0.01438(11) 0.01627(11) 0.03076(12) 0.0007(2) 0.00176(7) 0.00124(18) O1 0.027(2) 0.024(3) 0.039(3) -0.001(2) -0.001(2) 0.0028(18) O11 0.077(4) 0.142(10) 0.055(4) -0.048(6) -0.011(3) 0.011(7) C11 0.042(4) 0.076(10) 0.047(4) -0.010(5) 0.003(3) 0.011(5) C21 0.046(5) 0.068(6) 0.035(4) 0.007(4) 0.007(4) 0.013(4) O21 0.044(3) 0.068(4) 0.047(3) 0.013(3) -0.001(3) 0.012(3) C31 0.034(4) 0.026(4) 0.046(4) 0.000(3) 0.005(3) -0.001(3) O31 0.027(2) 0.037(3) 0.030(2) 0.000(2) 0.0054(19) 0.005(2) C41 0.028(4) 0.045(4) 0.035(4) 0.003(3) 0.003(3) -0.007(3) O41 0.024(2) 0.030(3) 0.036(3) -0.001(2) 0.004(2) -0.0002(19) C51 0.033(3) 0.065(8) 0.043(3) -0.003(5) -0.002(3) 0.010(5) O51 0.052(3) 0.081(4) 0.040(2) -0.003(6) -0.001(2) 0.007(6) C61 0.122(13) 0.145(14) 0.130(12) -0.109(12) -0.003(10) -0.013(11) C12 0.016(3) 0.022(3) 0.039(4) 0.002(3) 0.000(3) -0.003(2) O121 0.021(2) 0.016(2) 0.040(3) -0.0022(18) 0.0047(19) 0.0014(17) O122 0.030(2) 0.027(3) 0.050(3) -0.0096(19) -0.001(2) 0.0065(18) C22 0.017(3) 0.019(3) 0.042(4) -0.003(3) -0.001(3) -0.001(2) N22 0.0180(19) 0.021(3) 0.039(2) -0.011(4) -0.0016(17) -0.008(4) C32 0.028(3) 0.034(6) 0.031(3) -0.001(3) 0.000(2) 0.000(3) C42 0.017(2) 0.037(5) 0.043(3) 0.001(4) 0.000(2) 0.002(4) N52 0.0139(19) 0.026(4) 0.040(2) 0.008(3) -0.0006(18) -0.006(3) C62 0.022(2) 0.019(4) 0.040(3) 0.002(3) 0.000(2) -0.001(3) N72 0.017(2) 0.023(4) 0.048(3) -0.002(3) 0.0065(19) -0.004(3) C82 0.021(2) 0.021(5) 0.039(3) -0.010(3) 0.004(2) -0.008(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 O1 1.681(5) . ? Re1 O31 1.919(5) . ? Re1 O41 1.961(5) . ? Re1 N52 2.113(5) . ? Re1 N22 2.177(5) . ? Re1 O121 2.196(4) . ? Re1 Re3 2.987(6) . ? Re1 Re2 3.012(6) . ? O11 C11 1.375(10) . ? O11 C61 1.495(19) . ? C11 O51 1.436(9) . ? C11 C21 1.504(16) . ? C11 H11 1.0000 . ? C21 O21 1.401(10) . ? C21 C31 1.519(11) . ? C21 Re4 2.22(2) . ? C21 H21 1.0000 . ? O21 H821 0.8400 . ? C31 O31 1.464(9) . ? C31 C41 1.528(10) . ? C31 H31 1.0000 . ? C41 O41 1.428(9) . ? C41 C51 1.526(14) . ? C41 H41 1.0000 . ? O41 Re2 1.487(15) . ? C51 O51 1.428(9) . ? C51 H511 0.9900 . ? C51 H512 0.9900 . ? C61 H611 0.9800 . ? C61 H612 0.9800 . ? C61 H613 0.9800 . ? C12 O122 1.214(8) . ? C12 O121 1.301(8) . ? C12 C22 1.511(9) . ? C12 Re2 2.412(15) 2_545 ? O122 Re2 2.122(9) 2_545 ? C22 N22 1.453(9) . ? C22 C32 1.556(10) . ? C22 H22 1.0000 . ? N22 H221 0.9200 . ? N22 H222 0.9200 . ? C32 C42 1.510(8) . ? C32 Re3 2.376(9) . ? C32 H321 0.9900 . ? C32 H322 0.9900 . ? C42 Re3 0.895(8) . ? C42 C82 1.353(8) . ? C42 N52 1.370(9) . ? N52 Re3 0.898(8) . ? N52 C62 1.332(7) . ? C62 N72 1.346(8) . ? C62 H62 0.9500 . ? N72 C82 1.389(8) . ? N72 H772 0.8800 . ? C82 H82 0.9500 . ? O99 C99 1.348(14) . ? O99 H899 0.8400 . ? C99 H991 0.9800 . ? C99 H992 0.9800 . ? C99 H993 0.9800 . ? Re2 O122 2.122(9) 2 ? Re2 C12 2.412(15) 2 ? 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 O1 Re1 O31 111.9(2) . . ? O1 Re1 O41 104.5(2) . . ? O31 Re1 O41 83.0(2) . . ? O1 Re1 N52 96.2(3) . . ? O31 Re1 N52 87.0(2) . . ? O41 Re1 N52 159.1(3) . . ? O1 Re1 N22 92.3(3) . . ? O31 Re1 N22 155.9(3) . . ? O41 Re1 N22 91.4(2) . . ? N52 Re1 N22 90.22(18) . . ? O1 Re1 O121 161.8(2) . . ? O31 Re1 O121 85.33(19) . . ? O41 Re1 O121 82.82(18) . . ? N52 Re1 O121 78.1(3) . . ? N22 Re1 O121 70.7(3) . . ? O1 Re1 Re3 99.3(5) . . ? O31 Re1 Re3 89.1(3) . . ? O41 Re1 Re3 156.1(5) . . ? N52 Re1 Re3 4.7(4) . . ? N22 Re1 Re3 86.62(17) . . ? O121 Re1 Re3 74.1(5) . . ? O1 Re1 Re2 79.7(5) . . ? O31 Re1 Re2 90.0(3) . . ? O41 Re1 Re2 25.0(5) . . ? N52 Re1 Re2 173.6(4) . . ? N22 Re1 Re2 94.83(17) . . ? O121 Re1 Re2 107.3(5) . . ? Re3 Re1 Re2 178.2(5) . . ? C11 O11 C61 110.5(13) . . ? O11 C11 O51 107.1(6) . . ? O11 C11 C21 110.1(10) . . ? O51 C11 C21 107.0(9) . . ? O11 C11 H11 110.9 . . ? O51 C11 H11 110.9 . . ? C21 C11 H11 110.9 . . ? O21 C21 C11 112.0(8) . . ? O21 C21 C31 112.1(7) . . ? C11 C21 C31 110.7(7) . . ? O21 C21 Re4 102.3(7) . . ? C11 C21 Re4 145.1(7) . . ? C31 C21 Re4 46.9(6) . . ? O21 C21 H21 107.2 . . ? C11 C21 H21 107.2 . . ? C31 C21 H21 107.2 . . ? Re4 C21 H21 66.8 . . ? C21 O21 H821 109.5 . . ? O31 C31 C21 108.3(6) . . ? O31 C31 C41 107.3(6) . . ? C21 C31 C41 113.6(7) . . ? O31 C31 H31 109.2 . . ? C21 C31 H31 109.2 . . ? C41 C31 H31 109.2 . . ? C31 O31 Re1 114.8(4) . . ? O41 C41 C51 109.3(6) . . ? O41 C41 C31 107.1(6) . . ? C51 C41 C31 112.3(6) . . ? O41 C41 H41 109.4 . . ? C51 C41 H41 109.4 . . ? C31 C41 H41 109.4 . . ? C41 O41 Re2 73.3(6) . . ? C41 O41 Re1 111.8(4) . . ? Re2 O41 Re1 121.1(8) . . ? O51 C51 C41 109.4(10) . . ? O51 C51 H511 109.8 . . ? C41 C51 H511 109.8 . . ? O51 C51 H512 109.8 . . ? C41 C51 H512 109.8 . . ? H511 C51 H512 108.2 . . ? C51 O51 C11 110.9(6) . . ? O11 C61 H611 109.5 . . ? O11 C61 H612 109.5 . . ? H611 C61 H612 109.5 . . ? O11 C61 H613 109.5 . . ? H611 C61 H613 109.5 . . ? H612 C61 H613 109.5 . . ? O122 C12 O121 123.1(6) . . ? O122 C12 C22 123.4(6) . . ? O121 C12 C22 113.5(6) . . ? O122 C12 Re2 61.6(5) . 2_545 ? O121 C12 Re2 123.5(5) . 2_545 ? C22 C12 Re2 90.7(6) . 2_545 ? C12 O121 Re1 115.7(4) . . ? C12 O122 Re2 88.2(6) . 2_545 ? N22 C22 C12 108.9(6) . . ? N22 C22 C32 110.5(6) . . ? C12 C22 C32 108.7(6) . . ? N22 C22 H22 109.5 . . ? C12 C22 H22 109.5 . . ? C32 C22 H22 109.5 . . ? C22 N22 Re1 108.8(4) . . ? C22 N22 H221 109.9 . . ? Re1 N22 H221 109.9 . . ? C22 N22 H222 109.9 . . ? Re1 N22 H222 109.9 . . ? H221 N22 H222 108.3 . . ? C42 C32 C22 111.8(7) . . ? C42 C32 Re3 6.7(3) . . ? C22 C32 Re3 105.5(6) . . ? C42 C32 H321 109.3 . . ? C22 C32 H321 109.3 . . ? Re3 C32 H321 114.6 . . ? C42 C32 H322 109.3 . . ? C22 C32 H322 109.3 . . ? Re3 C32 H322 110.1 . . ? H321 C32 H322 107.9 . . ? Re3 C42 C82 70.2(6) . . ? Re3 C42 N52 40.3(5) . . ? C82 C42 N52 109.6(5) . . ? Re3 C42 C32 161.8(9) . . ? C82 C42 C32 127.8(6) . . ? N52 C42 C32 122.4(5) . . ? Re3 N52 C62 68.4(6) . . ? Re3 N52 C42 40.1(5) . . ? C62 N52 C42 107.9(5) . . ? Re3 N52 Re1 164.2(12) . . ? C62 N52 Re1 124.3(4) . . ? C42 N52 Re1 127.7(4) . . ? N52 C62 N72 108.2(5) . . ? N52 C62 H62 125.9 . . ? N72 C62 H62 125.9 . . ? C62 N72 C82 109.4(5) . . ? C62 N72 H772 125.3 . . ? C82 N72 H772 125.3 . . ? C42 C82 N72 104.8(5) . . ? C42 C82 H82 127.6 . . ? N72 C82 H82 127.6 . . ? C99 O99 H899 109.5 . . ? O99 C99 H991 109.5 . . ? O99 C99 H992 109.5 . . ? H991 C99 H992 109.5 . . ? O99 C99 H993 109.5 . . ? H991 C99 H993 109.5 . . ? H992 C99 H993 109.5 . . ? O41 Re2 O122 117.8(6) . 2 ? O41 Re2 C12 110.2(4) . 2 ? O122 Re2 C12 30.2(3) 2 2 ? O41 Re2 Re1 33.9(4) . . ? O122 Re2 Re1 122.6(3) 2 . ? C12 Re2 Re1 99.1(4) 2 . ? C42 Re3 N52 99.6(9) . . ? C42 Re3 C32 11.4(5) . . ? N52 Re3 C32 88.9(6) . . ? C42 Re3 Re1 91.7(6) . . ? N52 Re3 Re1 11.1(8) . . ? C32 Re3 Re1 80.5(2) . . ? 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 C61 O11 C11 O51 -80.2(12) . . . . ? C61 O11 C11 C21 163.9(10) . . . . ? O11 C11 C21 O21 -58.8(10) . . . . ? O51 C11 C21 O21 -174.8(7) . . . . ? O11 C11 C21 C31 175.3(7) . . . . ? O51 C11 C21 C31 59.3(10) . . . . ? O11 C11 C21 Re4 132.6(11) . . . . ? O51 C11 C21 Re4 16.6(15) . . . . ? O21 C21 C31 O31 -52.9(9) . . . . ? C11 C21 C31 O31 72.9(8) . . . . ? Re4 C21 C31 O31 -139.1(8) . . . . ? O21 C21 C31 C41 -171.9(7) . . . . ? C11 C21 C31 C41 -46.1(10) . . . . ? Re4 C21 C31 C41 101.8(7) . . . . ? C21 C31 O31 Re1 -147.7(5) . . . . ? C41 C31 O31 Re1 -24.8(7) . . . . ? O1 Re1 O31 C31 105.7(5) . . . . ? O41 Re1 O31 C31 2.8(4) . . . . ? N52 Re1 O31 C31 -158.8(5) . . . . ? N22 Re1 O31 C31 -74.9(6) . . . . ? O121 Re1 O31 C31 -80.5(4) . . . . ? Re3 Re1 O31 C31 -154.6(6) . . . . ? Re2 Re1 O31 C31 26.9(6) . . . . ? O31 C31 C41 O41 41.0(7) . . . . ? C21 C31 C41 O41 160.6(7) . . . . ? O31 C31 C41 C51 -79.0(8) . . . . ? C21 C31 C41 C51 40.6(10) . . . . ? C51 C41 O41 Re2 -35.9(9) . . . . ? C31 C41 O41 Re2 -157.8(10) . . . . ? C51 C41 O41 Re1 81.6(6) . . . . ? C31 C41 O41 Re1 -40.3(7) . . . . ? O1 Re1 O41 C41 -88.8(5) . . . . ? O31 Re1 O41 C41 22.0(4) . . . . ? N52 Re1 O41 C41 84.1(7) . . . . ? N22 Re1 O41 C41 178.5(5) . . . . ? O121 Re1 O41 C41 108.2(5) . . . . ? Re3 Re1 O41 C41 93.7(6) . . . . ? Re2 Re1 O41 C41 -83.1(6) . . . . ? O1 Re1 O41 Re2 -5.7(5) . . . . ? O31 Re1 O41 Re2 105.1(5) . . . . ? N52 Re1 O41 Re2 167.2(5) . . . . ? N22 Re1 O41 Re2 -98.4(5) . . . . ? O121 Re1 O41 Re2 -168.7(5) . . . . ? Re3 Re1 O41 Re2 176.7(6) . . . . ? O41 C41 C51 O51 -167.6(6) . . . . ? C31 C41 C51 O51 -48.8(9) . . . . ? C41 C51 O51 C11 65.8(13) . . . . ? O11 C11 O51 C51 170.7(12) . . . . ? C21 C11 O51 C51 -71.3(13) . . . . ? O122 C12 O121 Re1 155.2(5) . . . . ? C22 C12 O121 Re1 -21.6(6) . . . . ? Re2 C12 O121 Re1 -129.3(7) 2_545 . . . ? O1 Re1 O121 C12 14.2(8) . . . . ? O31 Re1 O121 C12 -147.1(4) . . . . ? O41 Re1 O121 C12 129.4(4) . . . . ? N52 Re1 O121 C12 -59.2(4) . . . . ? N22 Re1 O121 C12 35.3(4) . . . . ? Re3 Re1 O121 C12 -56.7(4) . . . . ? Re2 Re1 O121 C12 124.4(4) . . . . ? O121 C12 O122 Re2 113.4(7) . . . 2_545 ? C22 C12 O122 Re2 -70.1(8) . . . 2_545 ? O122 C12 C22 N22 168.6(6) . . . . ? O121 C12 C22 N22 -14.6(7) . . . . ? Re2 C12 C22 N22 112.8(5) 2_545 . . . ? O122 C12 C22 C32 -70.9(8) . . . . ? O121 C12 C22 C32 105.9(6) . . . . ? Re2 C12 C22 C32 -126.7(5) 2_545 . . . ? C12 C22 N22 Re1 43.2(6) . . . . ? C32 C22 N22 Re1 -76.2(7) . . . . ? O1 Re1 N22 C22 132.8(6) . . . . ? O31 Re1 N22 C22 -46.6(8) . . . . ? O41 Re1 N22 C22 -122.6(5) . . . . ? N52 Re1 N22 C22 36.6(6) . . . . ? O121 Re1 N22 C22 -40.7(5) . . . . ? Re3 Re1 N22 C22 33.6(7) . . . . ? Re2 Re1 N22 C22 -147.4(7) . . . . ? N22 C22 C32 C42 78.8(9) . . . . ? C12 C22 C32 C42 -40.8(9) . . . . ? N22 C22 C32 Re3 76.1(8) . . . . ? C12 C22 C32 Re3 -43.4(8) . . . . ? C22 C32 C42 Re3 -22(6) . . . . ? C22 C32 C42 C82 148.2(10) . . . . ? Re3 C32 C42 C82 171(7) . . . . ? C22 C32 C42 N52 -37.6(15) . . . . ? Re3 C32 C42 N52 -15(6) . . . . ? C82 C42 N52 Re3 -12(3) . . . . ? C32 C42 N52 Re3 173(3) . . . . ? Re3 C42 N52 C62 11(3) . . . . ? C82 C42 N52 C62 -1.5(13) . . . . ? C32 C42 N52 C62 -176.6(10) . . . . ? Re3 C42 N52 Re1 -166(3) . . . . ? C82 C42 N52 Re1 -178.1(7) . . . . ? C32 C42 N52 Re1 6.8(17) . . . . ? O1 Re1 N52 Re3 -132(5) . . . . ? O31 Re1 N52 Re3 116(5) . . . . ? O41 Re1 N52 Re3 55(5) . . . . ? N22 Re1 N52 Re3 -40(5) . . . . ? O121 Re1 N52 Re3 30(5) . . . . ? Re2 Re1 N52 Re3 179(8) . . . . ? O1 Re1 N52 C62 86.8(9) . . . . ? O31 Re1 N52 C62 -24.9(9) . . . . ? O41 Re1 N52 C62 -86.3(11) . . . . ? N22 Re1 N52 C62 179.1(9) . . . . ? O121 Re1 N52 C62 -110.7(9) . . . . ? Re3 Re1 N52 C62 -141(6) . . . . ? Re2 Re1 N52 C62 37(5) . . . . ? O1 Re1 N52 C42 -97.1(10) . . . . ? O31 Re1 N52 C42 151.2(10) . . . . ? O41 Re1 N52 C42 89.8(11) . . . . ? N22 Re1 N52 C42 -4.8(10) . . . . ? O121 Re1 N52 C42 65.4(10) . . . . ? Re3 Re1 N52 C42 35(5) . . . . ? Re2 Re1 N52 C42 -147(4) . . . . ? Re3 N52 C62 N72 6.4(19) . . . . ? C42 N52 C62 N72 -0.9(13) . . . . ? Re1 N52 C62 N72 175.8(7) . . . . ? N52 C62 N72 C82 2.9(12) . . . . ? Re3 C42 C82 N72 -5.2(18) . . . . ? N52 C42 C82 N72 3.1(12) . . . . ? C32 C42 C82 N72 177.9(12) . . . . ? C62 N72 C82 C42 -3.7(11) . . . . ? C41 O41 Re2 O122 -146.3(13) . . . 2 ? Re1 O41 Re2 O122 107.9(10) . . . 2 ? C41 O41 Re2 C12 -178.4(10) . . . 2 ? Re1 O41 Re2 C12 75.8(8) . . . 2 ? C41 O41 Re2 Re1 105.7(6) . . . . ? O1 Re1 Re2 O41 174.4(5) . . . . ? O31 Re1 Re2 O41 -73.4(5) . . . . ? N52 Re1 Re2 O41 -135(4) . . . . ? N22 Re1 Re2 O41 82.9(5) . . . . ? O121 Re1 Re2 O41 11.7(5) . . . . ? Re3 Re1 Re2 O41 -132(26) . . . . ? O1 Re1 Re2 O122 82.0(11) . . . 2 ? O31 Re1 Re2 O122 -165.7(11) . . . 2 ? O41 Re1 Re2 O122 -92.3(10) . . . 2 ? N52 Re1 Re2 O122 132(3) . . . 2 ? N22 Re1 Re2 O122 -9.4(11) . . . 2 ? O121 Re1 Re2 O122 -80.6(11) . . . 2 ? Re3 Re1 Re2 O122 136(25) . . . 2 ? O1 Re1 Re2 C12 61.5(6) . . . 2 ? O31 Re1 Re2 C12 173.8(6) . . . 2 ? O41 Re1 Re2 C12 -112.9(6) . . . 2 ? N52 Re1 Re2 C12 112(4) . . . 2 ? N22 Re1 Re2 C12 -29.9(7) . . . 2 ? O121 Re1 Re2 C12 -101.1(6) . . . 2 ? Re3 Re1 Re2 C12 116(26) . . . 2 ? C82 C42 Re3 N52 168(3) . . . . ? C32 C42 Re3 N52 -20(7) . . . . ? C82 C42 Re3 C32 -172(6) . . . . ? N52 C42 Re3 C32 20(7) . . . . ? C82 C42 Re3 Re1 175.7(12) . . . . ? N52 C42 Re3 Re1 7.8(15) . . . . ? C32 C42 Re3 Re1 -12(6) . . . . ? C62 N52 Re3 C42 -169(3) . . . . ? Re1 N52 Re3 C42 45(7) . . . . ? C62 N52 Re3 C32 -173.0(13) . . . . ? C42 N52 Re3 C32 -3.9(15) . . . . ? Re1 N52 Re3 C32 41(6) . . . . ? C62 N52 Re3 Re1 146(5) . . . . ? C42 N52 Re3 Re1 -45(7) . . . . ? C22 C32 Re3 C42 158(6) . . . . ? C42 C32 Re3 N52 160(7) . . . . ? C22 C32 Re3 N52 -41.3(19) . . . . ? C42 C32 Re3 Re1 168(6) . . . . ? C22 C32 Re3 Re1 -33.9(7) . . . . ? O1 Re1 Re3 C42 -87.6(17) . . . . ? O31 Re1 Re3 C42 160.4(17) . . . . ? O41 Re1 Re3 C42 90.0(19) . . . . ? N52 Re1 Re3 C42 -136(7) . . . . ? N22 Re1 Re3 C42 4.1(17) . . . . ? O121 Re1 Re3 C42 75.0(17) . . . . ? Re2 Re1 Re3 C42 -141(25) . . . . ? O1 Re1 Re3 N52 48(5) . . . . ? O31 Re1 Re3 N52 -64(5) . . . . ? O41 Re1 Re3 N52 -134(5) . . . . ? N22 Re1 Re3 N52 140(5) . . . . ? O121 Re1 Re3 N52 -149(5) . . . . ? Re2 Re1 Re3 N52 -5(31) . . . . ? O1 Re1 Re3 C32 -90.0(6) . . . . ? O31 Re1 Re3 C32 157.9(6) . . . . ? O41 Re1 Re3 C32 87.6(8) . . . . ? N52 Re1 Re3 C32 -138(6) . . . . ? N22 Re1 Re3 C32 1.7(6) . . . . ? O121 Re1 Re3 C32 72.5(5) . . . . ? Re2 Re1 Re3 C32 -144(26) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? #?# use this item for nonbonding or very weakly bonding contacts, e.g.: #?# Sb1 N13 3.906(13) . . ? #?# Mn Mn 3.253(2) . 2 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag #?# Do not(!) delete the #s to obtain a table header: # #D H A D - H H...A D...A D - H...A symm(A) publ_flag O21 H821 O99 0.84 2.06 2.856(13) 157.9 . ? N22 H221 O1 0.92 2.17 3.032(8) 156.4 2_545 ? N22 H221 O121 0.92 2.60 3.135(7) 117.9 2 ? N22 H222 O41 0.92 1.95 2.797(10) 152.4 2 ? N72 H772 O121 0.88 2.09 2.851(7) 143.7 2_655 ? N72 H772 O122 0.88 2.66 3.231(7) 123.7 2_655 ? N72 H772 O1 0.88 2.70 3.362(8) 133.4 2_645 ? O99 H899 O122 0.84 1.96 2.801(10) 174.1 2_655 ? _geom_special_details ? #:---------------------------------------------------------------------------- #:--------------------------ARCHIVING AND CHECKING---------------------------- #:---------------------------------------------------------------------------- _audit_block_code Re_O_MebDribp_His_ln077_grimminger _audit_creation_method 'form98_non/compatible with shelxl97-2' _chemical_name_systematic ? _chemical_formula_moiety '2(C12 H18 N3 O8 Re1.02), 0.5(C2 H8 O2)' _chemical_formula_sum 'C25 H40 N6 O17 Re2.04' _chemical_formula_weight 1075.75 _chemical_melting_point ? _chemical_absolute_configuration syn _cell_formula_units_Z 1 _exptl_crystal_density_diffrn 1.801 _exptl_crystal_F_000 518