Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Nadia Carmen Mosch-Zanetti' _publ_contact_author_address ; Institut fur Anorganische Chemie Universitat Gottingen Tammannstrasse 4 Göttingen 37077 GERMANY ; _publ_contact_author_email NMOESCH@GWDG.DE _publ_section_title ; Rhenium oxo compounds containing h2-pyrazolate ligands ; loop_ _publ_author_name 'Nadia Carmen Mosch-Zanetti' 'Jorg Magull' 'Roland Pfoh' 'Anna Sachse' 'Denis Vidovic' data_as3 _database_code_depnum_ccdc_archive 'CCDC 261127' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H21 N2 O3 Re' _chemical_formula_weight 427.51 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 ? _symmetry_space_group_name_H-M ? 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 11.2384(4) _cell_length_b 9.0653(4) _cell_length_c 14.5734(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.253(3) _cell_angle_gamma 90.00 _cell_volume 1472.85(10) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.928 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 8.253 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25266 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0133 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 24.79 _reflns_number_total 2524 _reflns_number_gt 2460 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0180P)^2^+2.7477P] 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 2524 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0168 _refine_ls_R_factor_gt 0.0160 _refine_ls_wR_factor_ref 0.0393 _refine_ls_wR_factor_gt 0.0388 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 0.912249(10) 0.562459(13) 0.604925(8) 0.02547(6) Uani 1 1 d . . . O1 O 1.0140(2) 0.4638(3) 0.6762(2) 0.0486(7) Uani 1 1 d . . . O2 O 0.9917(2) 0.6534(3) 0.53025(17) 0.0369(5) Uani 1 1 d . . . O3 O 0.8558(2) 0.6912(3) 0.67226(17) 0.0436(6) Uani 1 1 d . . . N1 N 0.7587(2) 0.5173(3) 0.51081(16) 0.0205(5) Uani 1 1 d . . . N2 N 0.7928(2) 0.3993(3) 0.56858(16) 0.0194(5) Uani 1 1 d . . . C1 C 0.6900(2) 0.4672(3) 0.43593(19) 0.0182(6) Uani 1 1 d . . . C2 C 0.6772(2) 0.3124(3) 0.44628(19) 0.0194(6) Uani 1 1 d . . . C3 C 0.7467(2) 0.2731(3) 0.52915(19) 0.0191(6) Uani 1 1 d . . . C4 C 0.6355(3) 0.5727(3) 0.3616(2) 0.0228(6) Uani 1 1 d . . . C5 C 0.6868(3) 0.7277(3) 0.3818(2) 0.0357(8) Uani 1 1 d . . . H5A H 0.7737 0.7260 0.3806 0.054 Uiso 1 1 calc R . . H5B H 0.6696 0.7597 0.4430 0.054 Uiso 1 1 calc R . . H5C H 0.6498 0.7966 0.3348 0.054 Uiso 1 1 calc R . . C6 C 0.6642(3) 0.5241(4) 0.2661(2) 0.0311(7) Uani 1 1 d . . . H6A H 0.7513 0.5181 0.2666 0.047 Uiso 1 1 calc R . . H6B H 0.6311 0.5959 0.2195 0.047 Uiso 1 1 calc R . . H6C H 0.6285 0.4270 0.2511 0.047 Uiso 1 1 calc R . . C7 C 0.4992(3) 0.5775(4) 0.3640(2) 0.0314(7) Uani 1 1 d . . . H7A H 0.4622 0.6435 0.3153 0.047 Uiso 1 1 calc R . . H7B H 0.4826 0.6139 0.4244 0.047 Uiso 1 1 calc R . . H7C H 0.4659 0.4780 0.3538 0.047 Uiso 1 1 calc R . . C8 C 0.6014(3) 0.2119(4) 0.3809(2) 0.0299(7) Uani 1 1 d . . . H8A H 0.6224 0.2250 0.3182 0.045 Uiso 1 1 calc R . . H8B H 0.5165 0.2359 0.3817 0.045 Uiso 1 1 calc R . . H8C H 0.6158 0.1092 0.4003 0.045 Uiso 1 1 calc R . . C9 C 0.7757(3) 0.1252(3) 0.5742(2) 0.0262(6) Uani 1 1 d . . . C10 C 0.8406(3) 0.0313(4) 0.5071(3) 0.0436(9) Uani 1 1 d . . . H10A H 0.8620 -0.0648 0.5354 0.065 Uiso 1 1 calc R . . H10B H 0.9136 0.0823 0.4943 0.065 Uiso 1 1 calc R . . H10C H 0.7874 0.0168 0.4492 0.065 Uiso 1 1 calc R . . C11 C 0.8578(4) 0.1450(4) 0.6648(3) 0.0526(11) Uani 1 1 d . . . H11A H 0.8171 0.2050 0.7073 0.079 Uiso 1 1 calc R . . H11B H 0.9318 0.1945 0.6527 0.079 Uiso 1 1 calc R . . H11C H 0.8774 0.0482 0.6926 0.079 Uiso 1 1 calc R . . C12 C 0.6611(3) 0.0454(3) 0.5947(3) 0.0322(7) Uani 1 1 d . . . H12A H 0.6216 0.1036 0.6388 0.048 Uiso 1 1 calc R . . H12B H 0.6822 -0.0519 0.6212 0.048 Uiso 1 1 calc R . . H12C H 0.6066 0.0337 0.5372 0.048 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 0.02808(8) 0.02409(8) 0.02225(8) 0.00015(5) -0.00455(5) -0.00915(5) O1 0.0432(15) 0.0438(15) 0.0511(17) 0.0096(13) -0.0242(13) -0.0159(12) O2 0.0343(12) 0.0330(13) 0.0433(14) -0.0008(10) 0.0047(10) -0.0149(10) O3 0.0618(16) 0.0382(14) 0.0306(13) -0.0124(11) 0.0048(11) -0.0142(12) N1 0.0243(12) 0.0171(12) 0.0198(12) 0.0017(10) 0.0011(10) -0.0024(10) N2 0.0175(11) 0.0198(12) 0.0198(12) 0.0013(10) -0.0021(9) -0.0018(9) C1 0.0163(13) 0.0204(14) 0.0181(14) -0.0017(11) 0.0030(11) 0.0005(11) C2 0.0155(12) 0.0209(14) 0.0225(14) -0.0028(12) 0.0045(10) -0.0010(11) C3 0.0149(12) 0.0193(14) 0.0237(14) -0.0007(11) 0.0048(11) -0.0017(10) C4 0.0255(15) 0.0255(15) 0.0173(15) 0.0010(11) 0.0023(12) 0.0011(12) C5 0.052(2) 0.0234(16) 0.0301(17) 0.0075(13) -0.0026(15) -0.0013(15) C6 0.0316(16) 0.0415(19) 0.0210(16) 0.0022(14) 0.0058(13) 0.0034(14) C7 0.0286(16) 0.0409(19) 0.0245(17) 0.0066(14) 0.0024(13) 0.0109(14) C8 0.0326(16) 0.0247(16) 0.0309(17) -0.0065(13) -0.0021(13) -0.0039(13) C9 0.0215(14) 0.0196(15) 0.0366(17) 0.0038(13) 0.0005(13) -0.0012(12) C10 0.0383(19) 0.0209(16) 0.076(3) 0.0069(17) 0.0228(19) 0.0057(14) C11 0.054(2) 0.034(2) 0.062(3) 0.0235(19) -0.027(2) -0.0079(17) C12 0.0294(17) 0.0262(16) 0.042(2) 0.0092(14) 0.0072(15) -0.0023(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 Re O1 1.699(3) . ? Re O3 1.698(2) . ? Re O2 1.705(2) . ? Re N2 2.022(2) . ? Re N1 2.104(2) . ? N1 C1 1.334(4) . ? N1 N2 1.385(3) . ? N2 C3 1.354(4) . ? C1 C2 1.421(4) . ? C1 C4 1.516(4) . ? C2 C3 1.399(4) . ? C2 C8 1.502(4) . ? C3 C9 1.511(4) . ? C4 C5 1.533(4) . ? C4 C6 1.533(4) . ? C4 C7 1.537(4) . ? C9 C11 1.522(5) . ? C9 C12 1.539(4) . ? C9 C10 1.548(5) . ? 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 O3 106.25(14) . . ? O1 Re O2 106.17(13) . . ? O3 Re O2 107.50(12) . . ? O1 Re N2 98.54(11) . . ? O3 Re N2 111.69(11) . . ? O2 Re N2 124.78(10) . . ? O1 Re N1 136.84(11) . . ? O3 Re N1 100.07(11) . . ? O2 Re N1 97.51(10) . . ? N2 Re N1 39.15(9) . . ? C1 N1 N2 108.7(2) . . ? C1 N1 Re 160.3(2) . . ? N2 N1 Re 67.22(14) . . ? C3 N2 N1 109.4(2) . . ? C3 N2 Re 159.2(2) . . ? N1 N2 Re 73.62(14) . . ? N1 C1 C2 107.8(2) . . ? N1 C1 C4 120.6(2) . . ? C2 C1 C4 131.4(3) . . ? C3 C2 C1 106.8(2) . . ? C3 C2 C8 127.1(3) . . ? C1 C2 C8 126.1(3) . . ? N2 C3 C2 107.1(2) . . ? N2 C3 C9 121.0(2) . . ? C2 C3 C9 131.9(3) . . ? C1 C4 C5 109.4(2) . . ? C1 C4 C6 110.8(2) . . ? C5 C4 C6 108.7(3) . . ? C1 C4 C7 108.4(2) . . ? C5 C4 C7 108.8(3) . . ? C6 C4 C7 110.7(3) . . ? C3 C9 C11 110.3(3) . . ? C3 C9 C12 111.2(2) . . ? C11 C9 C12 108.5(3) . . ? C3 C9 C10 107.8(3) . . ? C11 C9 C10 109.3(3) . . ? C12 C9 C10 109.7(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.79 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.732 _refine_diff_density_min -0.860 _refine_diff_density_rms 0.072 data_g42 _database_code_depnum_ccdc_archive 'CCDC 261128' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H21 N2 O4 Re' _chemical_formula_weight 431.50 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 ? _symmetry_space_group_name_H-M ? 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 9.7531(4) _cell_length_b 10.1836(5) _cell_length_c 15.4082(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.657(3) _cell_angle_gamma 90.00 _cell_volume 1487.10(11) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.927 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 8.179 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30138 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0130 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 24.79 _reflns_number_total 2548 _reflns_number_gt 2486 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0104P)^2^+2.5068P] 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 2548 _refine_ls_number_parameters 177 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0146 _refine_ls_R_factor_gt 0.0139 _refine_ls_wR_factor_ref 0.0321 _refine_ls_wR_factor_gt 0.0318 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.003 _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 0.172851(10) 0.354598(10) 0.535720(7) 0.01846(5) Uani 1 1 d . . . N1 N 0.0199(2) 0.4111(2) 0.74752(15) 0.0209(5) Uani 1 1 d . . . N2 N -0.1177(2) 0.4314(2) 0.70715(15) 0.0208(5) Uani 1 1 d . . . O1 O 0.2086(2) 0.42092(19) 0.64249(12) 0.0235(4) Uani 1 1 d . . . O2 O 0.3220(2) 0.2788(2) 0.52004(14) 0.0329(5) Uani 1 1 d . . . O3 O 0.0415(2) 0.2408(2) 0.52567(16) 0.0400(6) Uani 1 1 d . . . O4 O 0.1247(2) 0.4769(2) 0.45580(14) 0.0379(5) Uani 1 1 d . . . C5 C 0.1740(3) 0.3454(3) 0.89266(18) 0.0198(6) Uani 1 1 d . . . C6 C -0.1959(3) 0.4108(3) 0.76656(17) 0.0188(5) Uani 1 1 d . . . C7 C 0.0312(3) 0.3755(2) 0.83233(17) 0.0179(5) Uani 1 1 d . . . C8 C -0.1040(3) 0.3751(3) 0.84639(18) 0.0194(5) Uani 1 1 d . . . H8A H -0.1292 0.3542 0.9007 0.023 Uiso 1 1 calc R . . C9 C 0.2482(3) 0.2414(3) 0.8480(2) 0.0305(7) Uani 1 1 d . . . H9A H 0.1893 0.1625 0.8360 0.046 Uiso 1 1 calc R . . H9B H 0.3394 0.2192 0.8877 0.046 Uiso 1 1 calc R . . H9C H 0.2632 0.2762 0.7916 0.046 Uiso 1 1 calc R . . C10 C -0.3549(3) 0.4233(3) 0.74161(18) 0.0234(6) Uani 1 1 d . . . C11 C 0.1543(3) 0.2930(3) 0.9820(2) 0.0334(7) Uani 1 1 d . . . H11A H 0.1092 0.3604 1.0112 0.050 Uiso 1 1 calc R . . H11B H 0.2465 0.2705 1.0205 0.050 Uiso 1 1 calc R . . H11C H 0.0947 0.2144 0.9716 0.050 Uiso 1 1 calc R . . C12 C -0.4184(3) 0.2849(3) 0.7391(3) 0.0414(8) Uani 1 1 d . . . H12A H -0.3848 0.2310 0.6957 0.062 Uiso 1 1 calc R . . H12B H -0.5215 0.2906 0.7218 0.062 Uiso 1 1 calc R . . H12C H -0.3892 0.2447 0.7984 0.062 Uiso 1 1 calc R . . C13 C -0.4053(3) 0.4873(3) 0.65000(19) 0.0264(6) Uani 1 1 d . . . H13A H -0.3646 0.5755 0.6512 0.040 Uiso 1 1 calc R . . H13B H -0.5085 0.4936 0.6351 0.040 Uiso 1 1 calc R . . H13C H -0.3751 0.4340 0.6049 0.040 Uiso 1 1 calc R . . C14 C 0.2613(3) 0.4717(3) 0.9084(2) 0.0327(7) Uani 1 1 d . . . H14A H 0.2136 0.5366 0.9379 0.049 Uiso 1 1 calc R . . H14B H 0.2715 0.5066 0.8510 0.049 Uiso 1 1 calc R . . H14C H 0.3548 0.4526 0.9465 0.049 Uiso 1 1 calc R . . C15 C -0.4008(3) 0.5070(4) 0.8123(2) 0.0445(9) Uani 1 1 d . . . H15A H -0.3566 0.5938 0.8150 0.067 Uiso 1 1 calc R . . H15B H -0.3715 0.4640 0.8706 0.067 Uiso 1 1 calc R . . H15C H -0.5037 0.5167 0.7965 0.067 Uiso 1 1 calc R . . H1 H 0.077(3) 0.418(3) 0.718(2) 0.024(8) Uiso 1 1 d . . . H2 H -0.138(3) 0.461(3) 0.654(2) 0.022(8) 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 Re1 0.01790(7) 0.02293(7) 0.01439(7) 0.00046(4) 0.00352(4) 0.00222(4) N1 0.0153(11) 0.0304(13) 0.0192(12) 0.0056(10) 0.0085(10) 0.0037(10) N2 0.0163(11) 0.0312(13) 0.0144(11) 0.0081(10) 0.0028(9) 0.0046(10) O1 0.0230(10) 0.0313(11) 0.0174(9) 0.0002(8) 0.0074(8) 0.0003(8) O2 0.0293(11) 0.0385(12) 0.0323(12) -0.0077(10) 0.0103(9) 0.0073(10) O3 0.0253(11) 0.0373(12) 0.0508(15) -0.0033(11) -0.0045(10) -0.0079(10) O4 0.0436(13) 0.0500(14) 0.0237(11) 0.0155(10) 0.0151(10) 0.0168(11) C5 0.0161(13) 0.0241(14) 0.0185(14) 0.0023(11) 0.0026(11) -0.0012(11) C6 0.0184(13) 0.0214(13) 0.0175(13) 0.0013(10) 0.0061(10) 0.0010(10) C7 0.0200(13) 0.0180(12) 0.0162(13) 0.0004(10) 0.0055(11) -0.0011(10) C8 0.0205(13) 0.0230(13) 0.0159(13) 0.0033(10) 0.0064(11) -0.0004(11) C9 0.0268(15) 0.0327(16) 0.0293(16) -0.0004(13) 0.0009(13) 0.0100(13) C10 0.0155(13) 0.0340(15) 0.0213(14) 0.0013(12) 0.0054(11) 0.0018(12) C11 0.0231(15) 0.051(2) 0.0234(16) 0.0116(14) 0.0006(12) -0.0012(14) C12 0.0220(16) 0.045(2) 0.054(2) 0.0167(17) 0.0029(14) -0.0057(14) C13 0.0198(14) 0.0329(15) 0.0248(15) 0.0037(12) 0.0018(11) 0.0043(12) C14 0.0272(16) 0.0283(16) 0.0397(18) -0.0001(13) 0.0018(13) -0.0058(13) C15 0.0242(16) 0.080(3) 0.0296(18) -0.0096(18) 0.0062(13) 0.0144(17) _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 O3 1.708(2) . ? Re1 O2 1.714(2) . ? Re1 O1 1.7359(18) . ? Re1 O4 1.736(2) . ? N1 C7 1.335(3) . ? N1 N2 1.355(3) . ? N2 C6 1.339(3) . ? C5 C7 1.512(4) . ? C5 C14 1.530(4) . ? C5 C11 1.530(4) . ? C5 C9 1.534(4) . ? C6 C8 1.389(4) . ? C6 C10 1.513(4) . ? C7 C8 1.386(4) . ? C10 C13 1.527(4) . ? C10 C15 1.530(4) . ? C10 C12 1.537(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 O3 Re1 O2 108.97(11) . . ? O3 Re1 O1 109.18(11) . . ? O2 Re1 O1 108.76(9) . . ? O3 Re1 O4 110.56(11) . . ? O2 Re1 O4 108.64(11) . . ? O1 Re1 O4 110.68(10) . . ? C7 N1 N2 109.6(2) . . ? C6 N2 N1 108.9(2) . . ? C7 C5 C14 109.0(2) . . ? C7 C5 C11 109.3(2) . . ? C14 C5 C11 109.5(2) . . ? C7 C5 C9 109.1(2) . . ? C14 C5 C9 110.3(2) . . ? C11 C5 C9 109.6(2) . . ? N2 C6 C8 107.1(2) . . ? N2 C6 C10 121.9(2) . . ? C8 C6 C10 131.0(2) . . ? N1 C7 C8 107.0(2) . . ? N1 C7 C5 120.5(2) . . ? C8 C7 C5 132.5(2) . . ? C7 C8 C6 107.4(2) . . ? C6 C10 C13 111.0(2) . . ? C6 C10 C15 108.7(2) . . ? C13 C10 C15 109.6(3) . . ? C6 C10 C12 108.2(2) . . ? C13 C10 C12 109.2(2) . . ? C15 C10 C12 110.2(3) . . ? 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 N1 H1 O1 0.81(3) 1.92(3) 2.725(3) 175(3) . N2 H2 O4 0.85(3) 1.84(3) 2.665(3) 163(3) 3_566 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.79 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.380 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.067 data_nmz584 _database_code_depnum_ccdc_archive 'CCDC 261129' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H54 N4 O8 Re2' _chemical_formula_weight 971.17 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 16.831(3) _cell_length_b 9.6159(19) _cell_length_c 23.936(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.52(3) _cell_angle_gamma 90.00 _cell_volume 3651.3(13) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 6.673 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13124 _diffrn_reflns_av_R_equivalents 0.0525 _diffrn_reflns_av_sigmaI/netI 0.0585 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 24.73 _reflns_number_total 5826 _reflns_number_gt 4588 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0333P)^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 5826 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0707 _refine_ls_wR_factor_gt 0.0650 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _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 Re1 Re 0.262376(15) 0.34477(3) 0.106355(12) 0.02804(8) Uani 1 1 d . . . Re2 Re 0.327970(16) 0.06727(3) 0.356874(13) 0.02972(8) Uani 1 1 d . . . O1 O 0.2510(3) 0.1666(5) 0.1086(3) 0.0428(13) Uani 1 1 d . . . O2 O 0.3709(2) 0.2825(5) 0.0727(2) 0.0277(10) Uani 1 1 d . . . O3 O 0.3472(3) 0.3982(6) 0.1650(2) 0.0415(12) Uani 1 1 d . . . O4 O 0.1776(3) 0.4090(5) 0.1222(2) 0.0407(12) Uani 1 1 d . . . O5 O 0.3347(3) -0.1040(5) 0.3402(2) 0.0376(12) Uani 1 1 d . . . O6 O 0.4248(3) 0.1258(5) 0.4004(2) 0.0372(11) Uani 1 1 d . . . O7 O 0.3977(4) 0.0860(6) 0.2873(3) 0.0541(15) Uani 1 1 d . . . O8 O 0.2718(5) 0.0650(7) 0.4036(4) 0.079(2) Uani 1 1 d . . . N1 N 0.2086(3) 0.3835(5) 0.0142(2) 0.0239(11) Uani 1 1 d . . . N2 N 0.2569(3) 0.4980(5) 0.0416(2) 0.0230(11) Uani 1 1 d . . . N3 N 0.2306(4) 0.1367(6) 0.2834(4) 0.061(2) Uani 1 1 d . . . N4 N 0.2756(4) 0.2527(6) 0.3114(3) 0.059(2) Uani 1 1 d . . . C1 C 0.1379(3) 0.4292(7) -0.0271(3) 0.0231(13) Uani 1 1 d . . . C2 C 0.1423(4) 0.5727(7) -0.0288(3) 0.0250(14) Uani 1 1 d . . . H2A H 0.1023 0.6323 -0.0555 0.030 Uiso 1 1 calc R . . C3 C 0.2160(4) 0.6145(7) 0.0158(3) 0.0243(13) Uani 1 1 d . . . C4 C 0.0706(4) 0.3280(7) -0.0628(3) 0.0284(15) Uani 1 1 d . . . C5 C 0.1079(4) 0.2385(9) -0.1008(4) 0.044(2) Uani 1 1 d . . . H5B H 0.1273 0.2986 -0.1267 0.066 Uiso 1 1 calc R . . H5C H 0.0647 0.1746 -0.1250 0.066 Uiso 1 1 calc R . . H5D H 0.1557 0.1849 -0.0750 0.066 Uiso 1 1 calc R . . C6 C -0.0056(4) 0.4078(9) -0.1014(4) 0.053(2) Uani 1 1 d . . . H6B H 0.0116 0.4715 -0.1273 0.080 Uiso 1 1 calc R . . H6C H -0.0300 0.4611 -0.0763 0.080 Uiso 1 1 calc R . . H6D H -0.0476 0.3423 -0.1258 0.080 Uiso 1 1 calc R . . C7 C 0.0461(5) 0.2322(9) -0.0191(4) 0.049(2) Uani 1 1 d . . . H7A H 0.0968 0.1881 0.0080 0.073 Uiso 1 1 calc R . . H7B H 0.0070 0.1603 -0.0414 0.073 Uiso 1 1 calc R . . H7C H 0.0188 0.2875 0.0037 0.073 Uiso 1 1 calc R . . C8 C 0.2520(4) 0.7560(7) 0.0355(3) 0.0299(15) Uani 1 1 d . . . C9 C 0.2760(7) 0.7692(9) 0.1030(4) 0.065(3) Uani 1 1 d . . . H9A H 0.2256 0.7568 0.1143 0.097 Uiso 1 1 calc R . . H9B H 0.3001 0.8615 0.1155 0.097 Uiso 1 1 calc R . . H9C H 0.3176 0.6977 0.1223 0.097 Uiso 1 1 calc R . . C10 C 0.3317(5) 0.7759(9) 0.0184(5) 0.056(2) Uani 1 1 d . . . H10A H 0.3758 0.7121 0.0417 0.084 Uiso 1 1 calc R . . H10B H 0.3516 0.8720 0.0266 0.084 Uiso 1 1 calc R . . H10C H 0.3185 0.7562 -0.0239 0.084 Uiso 1 1 calc R . . C11 C 0.1881(4) 0.8692(7) 0.0058(4) 0.046(2) Uani 1 1 d . . . H11A H 0.1375 0.8577 0.0170 0.069 Uiso 1 1 calc R . . H11B H 0.1728 0.8617 -0.0374 0.069 Uiso 1 1 calc R . . H11C H 0.2129 0.9608 0.0187 0.069 Uiso 1 1 calc R . . C12 C 0.1590(4) 0.1787(7) 0.2436(3) 0.0280(15) Uani 1 1 d . . . C13 C 0.1594(4) 0.3233(7) 0.2446(3) 0.0260(14) Uani 1 1 d . . . H13A H 0.1174 0.3826 0.2195 0.031 Uiso 1 1 calc R . . C14 C 0.2324(4) 0.3653(7) 0.2891(3) 0.0264(14) Uani 1 1 d . . . C15 C 0.0949(4) 0.0763(7) 0.2064(3) 0.0307(15) Uani 1 1 d . . . C16 C 0.0293(5) 0.1517(8) 0.1555(4) 0.051(2) Uani 1 1 d . . . H16A H -0.0001 0.2206 0.1716 0.077 Uiso 1 1 calc R . . H16B H -0.0114 0.0842 0.1314 0.077 Uiso 1 1 calc R . . H16C H 0.0574 0.1986 0.1309 0.077 Uiso 1 1 calc R . . C17 C 0.0513(5) 0.0076(9) 0.2460(3) 0.047(2) Uani 1 1 d . . . H17A H 0.0938 -0.0350 0.2803 0.071 Uiso 1 1 calc R . . H17B H 0.0124 -0.0642 0.2234 0.071 Uiso 1 1 calc R . . H17C H 0.0198 0.0779 0.2596 0.071 Uiso 1 1 calc R . . C18 C 0.1382(5) -0.0345(9) 0.1804(4) 0.049(2) Uani 1 1 d . . . H18A H 0.1835 -0.0787 0.2125 0.073 Uiso 1 1 calc R . . H18B H 0.1619 0.0094 0.1526 0.073 Uiso 1 1 calc R . . H18C H 0.0968 -0.1050 0.1596 0.073 Uiso 1 1 calc R . . C19 C 0.2636(4) 0.5127(7) 0.3090(3) 0.0300(15) Uani 1 1 d . . . C20 C 0.1994(6) 0.5859(12) 0.3308(5) 0.077(3) Uiso 1 1 d . . . H20A H 0.1931 0.5345 0.3644 0.116 Uiso 1 1 calc R . . H20B H 0.1450 0.5899 0.2987 0.116 Uiso 1 1 calc R . . H20C H 0.2189 0.6806 0.3434 0.116 Uiso 1 1 calc R . . C21 C 0.2659(6) 0.5954(12) 0.2549(5) 0.072(3) Uiso 1 1 d . . . H21A H 0.2964 0.5420 0.2337 0.108 Uiso 1 1 calc R . . H21B H 0.2947 0.6842 0.2680 0.108 Uiso 1 1 calc R . . H21C H 0.2082 0.6128 0.2286 0.108 Uiso 1 1 calc R . . C22 C 0.3483(7) 0.5116(13) 0.3549(5) 0.083(3) Uiso 1 1 d . . . H22A H 0.3709 0.6064 0.3610 0.124 Uiso 1 1 calc R . . H22B H 0.3859 0.4517 0.3419 0.124 Uiso 1 1 calc R . . H22C H 0.3440 0.4759 0.3921 0.124 Uiso 1 1 calc R . . C23 C 0.3602(4) 0.1957(7) 0.0215(3) 0.0336(16) Uani 1 1 d . . . H23A H 0.3263 0.2439 -0.0153 0.040 Uiso 1 1 calc R . . H23B H 0.3320 0.1072 0.0248 0.040 Uiso 1 1 calc R . . C24 C 0.4501(4) 0.1696(8) 0.0221(4) 0.0407(18) Uani 1 1 d . . . H24A H 0.4770 0.0921 0.0489 0.049 Uiso 1 1 calc R . . H24B H 0.4512 0.1492 -0.0182 0.049 Uiso 1 1 calc R . . C25 C 0.4926(4) 0.3085(8) 0.0451(3) 0.0390(18) Uani 1 1 d . . . H25A H 0.5525 0.2941 0.0693 0.047 Uiso 1 1 calc R . . H25B H 0.4898 0.3713 0.0117 0.047 Uiso 1 1 calc R . . C26 C 0.4447(4) 0.3690(8) 0.0822(4) 0.0413(18) Uani 1 1 d . . . H26A H 0.4800 0.3686 0.1246 0.050 Uiso 1 1 calc R . . H26B H 0.4279 0.4660 0.0701 0.050 Uiso 1 1 calc R . . C27 C 0.3765(5) 0.0114(9) 0.2330(4) 0.048(2) Uani 1 1 d . . . H27A H 0.3195 0.0382 0.2066 0.058 Uiso 1 1 calc R . . H27B H 0.3769 -0.0899 0.2405 0.058 Uiso 1 1 calc R . . C28 C 0.4419(5) 0.0482(9) 0.2049(4) 0.050(2) Uani 1 1 d . . . H28A H 0.4729 -0.0357 0.1997 0.060 Uiso 1 1 calc R . . H28B H 0.4155 0.0930 0.1658 0.060 Uiso 1 1 calc R . . C29 C 0.4998(5) 0.1476(11) 0.2482(4) 0.061(2) Uiso 1 1 d . . . H29A H 0.5528 0.1003 0.2713 0.073 Uiso 1 1 calc R . . H29B H 0.5137 0.2274 0.2270 0.073 Uiso 1 1 calc R . . C30 C 0.4553(6) 0.1949(10) 0.2871(5) 0.060(2) Uani 1 1 d . . . H30A H 0.4951 0.2113 0.3276 0.072 Uiso 1 1 calc R . . H30B H 0.4245 0.2824 0.2721 0.072 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 Re1 0.03159(13) 0.02609(14) 0.02627(16) 0.00325(11) 0.00945(10) 0.00175(11) Re2 0.03192(13) 0.02091(13) 0.03457(17) -0.00268(11) 0.00877(11) 0.00170(11) O1 0.049(3) 0.028(3) 0.055(4) 0.007(2) 0.022(2) -0.003(2) O2 0.0257(19) 0.027(2) 0.029(3) -0.007(2) 0.0073(17) -0.0010(19) O3 0.045(3) 0.046(3) 0.030(3) -0.006(2) 0.009(2) 0.009(2) O4 0.048(3) 0.039(3) 0.037(3) -0.001(2) 0.017(2) 0.006(2) O5 0.051(3) 0.016(2) 0.039(3) -0.002(2) 0.006(2) 0.006(2) O6 0.048(3) 0.029(3) 0.029(3) -0.003(2) 0.006(2) 0.005(2) O7 0.074(4) 0.056(4) 0.043(4) -0.022(3) 0.035(3) -0.029(3) O8 0.097(5) 0.077(5) 0.092(6) -0.053(4) 0.071(4) -0.035(4) N1 0.031(2) 0.018(2) 0.026(3) 0.001(2) 0.013(2) -0.003(2) N2 0.026(2) 0.019(3) 0.023(3) -0.001(2) 0.007(2) 0.000(2) N3 0.047(3) 0.017(3) 0.085(6) -0.007(3) -0.022(3) 0.000(3) N4 0.043(3) 0.018(3) 0.080(5) -0.012(3) -0.026(3) -0.001(3) C1 0.027(3) 0.027(3) 0.020(3) -0.006(3) 0.013(2) 0.000(3) C2 0.030(3) 0.022(3) 0.024(4) -0.001(3) 0.012(2) 0.004(3) C3 0.033(3) 0.022(3) 0.024(4) -0.003(3) 0.018(3) 0.000(3) C4 0.028(3) 0.028(3) 0.029(4) -0.012(3) 0.010(3) 0.002(3) C5 0.041(4) 0.049(5) 0.044(5) -0.029(4) 0.018(3) -0.004(4) C6 0.037(4) 0.048(5) 0.059(6) -0.018(4) -0.007(4) 0.007(4) C7 0.047(4) 0.056(5) 0.048(5) -0.023(4) 0.022(4) -0.024(4) C8 0.035(3) 0.018(3) 0.038(4) 0.001(3) 0.014(3) -0.001(3) C9 0.107(7) 0.040(5) 0.042(5) -0.020(4) 0.017(5) -0.015(5) C10 0.045(4) 0.033(4) 0.099(8) 0.008(5) 0.036(4) 0.002(4) C11 0.041(4) 0.018(3) 0.077(6) 0.004(4) 0.017(4) 0.000(3) C12 0.026(3) 0.022(3) 0.035(4) 0.001(3) 0.009(3) -0.003(3) C13 0.033(3) 0.022(3) 0.019(3) 0.004(3) 0.004(3) 0.004(3) C14 0.026(3) 0.025(3) 0.032(4) -0.004(3) 0.013(3) 0.002(3) C15 0.034(3) 0.027(3) 0.031(4) -0.008(3) 0.010(3) -0.010(3) C16 0.046(4) 0.040(4) 0.047(5) 0.003(4) -0.011(4) -0.016(4) C17 0.046(4) 0.060(5) 0.034(5) -0.003(4) 0.011(3) -0.026(4) C18 0.060(5) 0.043(4) 0.050(5) -0.018(4) 0.028(4) -0.006(4) C19 0.032(3) 0.023(3) 0.036(4) -0.006(3) 0.011(3) -0.006(3) C23 0.031(3) 0.028(3) 0.042(4) -0.012(3) 0.011(3) 0.001(3) C24 0.036(3) 0.039(4) 0.046(5) -0.007(4) 0.012(3) 0.005(3) C25 0.045(4) 0.049(5) 0.027(4) -0.004(3) 0.017(3) -0.005(4) C26 0.038(3) 0.036(4) 0.051(5) -0.015(4) 0.016(3) -0.007(3) C27 0.053(4) 0.048(5) 0.043(5) -0.016(4) 0.015(4) -0.013(4) C28 0.050(4) 0.044(5) 0.060(6) -0.003(4) 0.023(4) 0.004(4) C30 0.076(5) 0.057(5) 0.061(6) -0.020(5) 0.042(5) -0.034(5) _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 O4 1.710(5) . ? Re1 O3 1.713(5) . ? Re1 O1 1.726(5) . ? Re1 N2 2.118(5) . ? Re1 N1 2.120(5) . ? Re1 O2 2.308(4) . ? Re2 O8 1.688(6) . ? Re2 O5 1.707(5) . ? Re2 O6 1.709(5) . ? Re2 N3 2.074(6) . ? Re2 N4 2.121(6) . ? Re2 O7 2.343(6) . ? O2 C23 1.443(8) . ? O2 C26 1.449(8) . ? O7 C27 1.421(9) . ? O7 C30 1.427(9) . ? N1 C1 1.341(8) . ? N1 N2 1.396(7) . ? N2 C3 1.351(8) . ? N3 C12 1.324(8) . ? N3 N4 1.390(8) . ? N4 C14 1.314(9) . ? C1 C2 1.383(9) . ? C1 C4 1.521(8) . ? C2 C3 1.399(9) . ? C3 C8 1.500(9) . ? C4 C6 1.515(9) . ? C4 C5 1.531(9) . ? C4 C7 1.550(11) . ? C8 C11 1.529(9) . ? C8 C9 1.536(11) . ? C8 C10 1.539(10) . ? C12 C13 1.391(9) . ? C12 C15 1.512(8) . ? C13 C14 1.391(9) . ? C14 C19 1.531(9) . ? C15 C16 1.526(10) . ? C15 C17 1.528(10) . ? C15 C18 1.535(10) . ? C19 C22 1.480(12) . ? C19 C20 1.520(13) . ? C19 C21 1.530(13) . ? C23 C24 1.530(9) . ? C24 C25 1.529(10) . ? C25 C26 1.501(10) . ? C27 C28 1.512(12) . ? C28 C29 1.505(12) . ? C29 C30 1.450(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Re1 O3 103.8(2) . . ? O4 Re1 O1 104.0(2) . . ? O3 Re1 O1 110.1(3) . . ? O4 Re1 N2 94.4(2) . . ? O3 Re1 N2 102.2(2) . . ? O1 Re1 N2 137.3(2) . . ? O4 Re1 N1 94.0(2) . . ? O3 Re1 N1 138.5(2) . . ? O1 Re1 N1 101.1(2) . . ? N2 Re1 N1 38.47(19) . . ? O4 Re1 O2 171.0(2) . . ? O3 Re1 O2 79.8(2) . . ? O1 Re1 O2 82.1(2) . . ? N2 Re1 O2 76.76(18) . . ? N1 Re1 O2 78.15(17) . . ? O8 Re2 O5 103.8(3) . . ? O8 Re2 O6 103.4(3) . . ? O5 Re2 O6 109.6(2) . . ? O8 Re2 N3 96.1(4) . . ? O5 Re2 N3 102.0(2) . . ? O6 Re2 N3 137.2(3) . . ? O8 Re2 N4 97.0(4) . . ? O5 Re2 N4 137.7(2) . . ? O6 Re2 N4 100.6(2) . . ? N3 Re2 N4 38.7(2) . . ? O8 Re2 O7 174.9(3) . . ? O5 Re2 O7 79.6(2) . . ? O6 Re2 O7 78.8(2) . . ? N3 Re2 O7 79.3(3) . . ? N4 Re2 O7 78.0(3) . . ? C23 O2 C26 108.8(5) . . ? C23 O2 Re1 123.9(3) . . ? C26 O2 Re1 122.2(4) . . ? C27 O7 C30 109.4(6) . . ? C27 O7 Re2 125.3(5) . . ? C30 O7 Re2 124.1(5) . . ? C1 N1 N2 108.8(5) . . ? C1 N1 Re1 142.2(4) . . ? N2 N1 Re1 70.7(3) . . ? C3 N2 N1 108.1(4) . . ? C3 N2 Re1 143.3(4) . . ? N1 N2 Re1 70.8(3) . . ? C12 N3 N4 108.7(6) . . ? C12 N3 Re2 168.3(7) . . ? N4 N3 Re2 72.5(3) . . ? C14 N4 N3 109.1(5) . . ? C14 N4 Re2 168.4(7) . . ? N3 N4 Re2 68.8(4) . . ? N1 C1 C2 107.8(5) . . ? N1 C1 C4 121.0(5) . . ? C2 C1 C4 131.2(6) . . ? C1 C2 C3 107.8(6) . . ? N2 C3 C2 107.4(5) . . ? N2 C3 C8 121.1(5) . . ? C2 C3 C8 131.5(6) . . ? C6 C4 C1 109.8(6) . . ? C6 C4 C5 110.7(6) . . ? C1 C4 C5 108.5(5) . . ? C6 C4 C7 110.5(6) . . ? C1 C4 C7 108.6(5) . . ? C5 C4 C7 108.7(6) . . ? C3 C8 C11 110.6(5) . . ? C3 C8 C9 110.0(6) . . ? C11 C8 C9 109.1(7) . . ? C3 C8 C10 109.0(6) . . ? C11 C8 C10 109.2(6) . . ? C9 C8 C10 108.9(7) . . ? N3 C12 C13 107.2(6) . . ? N3 C12 C15 121.5(6) . . ? C13 C12 C15 131.3(6) . . ? C14 C13 C12 107.5(6) . . ? N4 C14 C13 107.4(6) . . ? N4 C14 C19 123.4(5) . . ? C13 C14 C19 129.1(6) . . ? C12 C15 C16 110.1(6) . . ? C12 C15 C17 108.2(6) . . ? C16 C15 C17 109.4(6) . . ? C12 C15 C18 110.4(5) . . ? C16 C15 C18 108.7(7) . . ? C17 C15 C18 110.0(6) . . ? C22 C19 C20 111.5(8) . . ? C22 C19 C21 110.0(7) . . ? C20 C19 C21 105.8(7) . . ? C22 C19 C14 111.6(7) . . ? C20 C19 C14 109.0(6) . . ? C21 C19 C14 108.7(6) . . ? O2 C23 C24 104.2(5) . . ? C25 C24 C23 101.7(6) . . ? C26 C25 C24 105.9(6) . . ? O2 C26 C25 106.6(5) . . ? O7 C27 C28 106.9(6) . . ? C29 C28 C27 104.0(7) . . ? C30 C29 C28 106.7(7) . . ? O7 C30 C29 105.6(7) . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 24.73 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 1.287 _refine_diff_density_min -0.994 _refine_diff_density_rms 0.132