# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Clifford Kubiak' _publ_contact_author_email ckubiak@ucsd.edu loop_ _publ_author_name 'Eric Benson' 'Clifford Kubiak' data_[Re(bpy)(CO)3]2 _database_code_depnum_ccdc_archive 'CCDC 876407' #TrackingRef '- Bensons_Xtals.cif' _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety ? _chemical_formula_sum 'C26 H16 N4 O6 Re2' _chemical_formula_weight 852.83 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z+1/2' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x, -y, z-1/2' 7 '-x+1/2, -y+1/2, -z' 8 'x+1/2, -y+1/2, z-1/2' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _cell_length_a 9.620(3) _cell_length_b 19.620(6) _cell_length_c 12.933(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.710(4) _cell_angle_gamma 90.00 _cell_volume 2371.5(13) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2803 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.88 _cell_measurement_theta_min 2.41 _exptl_absorpt_coefficient_mu 10.252 _exptl_absorpt_correction_T_max 0.4589 _exptl_absorpt_correction_T_min 0.1119 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details TWINABS _exptl_crystal_colour green _exptl_crystal_density_diffrn 2.389 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description Plate _exptl_crystal_F_000 1592 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.09 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0638 _diffrn_reflns_av_sigmaI/netI 0.0707 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2666 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 28.63 _diffrn_reflns_theta_min 2.08 _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.960 _diffrn_measured_fraction_theta_max 0.874 _diffrn_measurement_device_type 'Bruker APEX CCD' _diffrn_measurement_method '\f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _reflns_number_gt 2015 _reflns_number_total 2666 _reflns_threshold_expression >2\s(I) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 2.355 _refine_diff_density_min -2.666 _refine_diff_density_rms 0.307 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 173 _refine_ls_number_reflns 2666 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0755 _refine_ls_R_factor_gt 0.0489 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1094 _refine_ls_wR_factor_ref 0.1197 _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^ > 2\s(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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.47896(4) 0.63815(2) 0.62823(3) 0.01858(15) Uani 1 1 d . . . O1 O 0.3294(8) 0.5037(4) 0.6533(6) 0.0281(17) Uani 1 1 d . . . O2 O 0.2069(7) 0.7180(4) 0.6339(6) 0.0233(16) Uani 1 1 d . . . O3 O 0.3581(9) 0.6294(4) 0.3884(6) 0.0285(18) Uani 1 1 d . . . N1 N 0.6879(8) 0.5960(4) 0.6311(6) 0.0204(18) Uani 1 1 d . . . N2 N 0.6120(9) 0.7261(5) 0.6329(6) 0.023(2) Uani 1 1 d . . . C1 C 0.3862(10) 0.5543(6) 0.6452(8) 0.023(2) Uani 1 1 d . . . C2 C 0.3090(11) 0.6892(5) 0.6355(8) 0.022(2) Uani 1 1 d . . . C3 C 0.4081(10) 0.6338(5) 0.4753(9) 0.023(2) Uani 1 1 d . . . C4 C 0.7137(12) 0.5304(7) 0.6236(8) 0.030(3) Uani 1 1 d . . . H4 H 0.6389 0.4988 0.6237 0.036 Uiso 1 1 calc R . . C5 C 0.8460(11) 0.5058(6) 0.6156(8) 0.028(2) Uani 1 1 d . . . H5 H 0.8609 0.4581 0.6112 0.033 Uiso 1 1 calc R . . C6 C 0.9568(11) 0.5512(6) 0.6138(7) 0.024(2) Uani 1 1 d . . . H6 H 1.0485 0.5356 0.6087 0.029 Uiso 1 1 calc R . . C7 C 0.9281(12) 0.6185(6) 0.6199(9) 0.030(3) Uani 1 1 d . . . H7 H 1.0018 0.6503 0.6180 0.035 Uiso 1 1 calc R . . C8 C 0.8012(11) 0.6422(5) 0.6283(8) 0.019(2) Uani 1 1 d . . . C9 C 0.7541(11) 0.7139(5) 0.6331(8) 0.021(2) Uani 1 1 d . . . C10 C 0.8498(11) 0.7689(5) 0.6364(8) 0.024(2) Uani 1 1 d . . . H10 H 0.9459 0.7600 0.6336 0.029 Uiso 1 1 calc R . . C11 C 0.8060(12) 0.8350(5) 0.6434(9) 0.024(2) Uani 1 1 d . . . H11 H 0.8707 0.8721 0.6477 0.029 Uiso 1 1 calc R . . C12 C 0.6626(12) 0.8456(5) 0.6441(8) 0.024(2) Uani 1 1 d . . . H12 H 0.6279 0.8905 0.6485 0.029 Uiso 1 1 calc R . . C13 C 0.5716(11) 0.7907(5) 0.6383(8) 0.024(2) Uani 1 1 d . . . H13 H 0.4744 0.7995 0.6381 0.029 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 0.0162(2) 0.0175(2) 0.0234(2) -0.00084(18) 0.00716(15) -0.0014(2) O1 0.028(4) 0.026(5) 0.032(4) -0.003(3) 0.011(3) -0.006(4) O2 0.017(3) 0.013(4) 0.043(4) -0.002(3) 0.012(3) 0.001(3) O3 0.034(4) 0.036(5) 0.015(4) -0.004(3) 0.004(3) -0.008(4) N1 0.021(4) 0.022(5) 0.020(4) 0.008(4) 0.008(3) 0.008(4) N2 0.022(4) 0.030(5) 0.016(4) -0.002(4) 0.003(4) -0.013(4) C1 0.015(4) 0.034(7) 0.018(5) 0.005(4) 0.001(4) -0.001(5) C2 0.029(6) 0.010(5) 0.028(5) 0.003(4) 0.013(4) -0.009(5) C3 0.018(5) 0.013(5) 0.036(7) -0.001(4) 0.003(4) -0.002(4) C4 0.023(5) 0.038(7) 0.031(6) -0.006(5) 0.013(5) 0.007(5) C5 0.021(5) 0.029(7) 0.033(6) -0.006(5) 0.006(4) 0.005(5) C6 0.024(5) 0.026(6) 0.025(6) -0.010(4) 0.010(4) -0.005(5) C7 0.024(5) 0.032(7) 0.033(7) -0.011(5) 0.008(5) 0.011(5) C8 0.023(5) 0.024(5) 0.012(5) -0.004(4) 0.006(4) -0.001(5) C9 0.033(6) 0.016(6) 0.016(5) 0.001(4) 0.009(4) 0.006(4) C10 0.020(5) 0.026(6) 0.021(5) -0.002(4) -0.006(4) -0.013(4) C11 0.025(5) 0.013(5) 0.036(6) -0.005(4) 0.009(5) -0.010(4) C12 0.030(5) 0.011(5) 0.029(6) 0.000(4) 0.003(5) 0.001(4) C13 0.026(5) 0.020(6) 0.028(6) 0.004(4) 0.011(5) 0.002(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Re1 3.0791(13) 2_656 ? Re1 N1 2.165(8) . ? Re1 N2 2.141(8) . ? Re1 C1 1.909(11) . ? Re1 C2 1.939(11) . ? Re1 C3 1.935(11) . ? O1 C1 1.150(12) . ? O2 C2 1.129(12) . ? O3 C3 1.116(13) . ? N1 C4 1.319(15) . ? N1 C8 1.424(13) . ? N2 C9 1.387(13) . ? N2 C13 1.333(13) . ? C4 H4 0.9500 . ? C4 C5 1.389(14) . ? C5 H5 0.9500 . ? C5 C6 1.394(15) . ? C6 H6 0.9500 . ? C6 C7 1.355(15) . ? C7 H7 0.9500 . ? C7 C8 1.335(14) . ? C8 C9 1.484(14) . ? C9 C10 1.412(15) . ? C10 H10 0.9500 . ? C10 C11 1.374(15) . ? C11 H11 0.9500 . ? C11 C12 1.397(15) . ? C12 H12 0.9500 . ? C12 C13 1.378(14) . ? C13 H13 0.9500 . ? 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 N1 Re1 Re1 94.9(2) . 2_656 ? N2 Re1 Re1 92.2(2) . 2_656 ? N2 Re1 N1 76.2(3) . . ? C1 Re1 Re1 80.4(3) . 2_656 ? C1 Re1 N1 97.2(4) . . ? C1 Re1 N2 169.7(4) . . ? C1 Re1 C2 91.0(4) . . ? C1 Re1 C3 91.1(4) . . ? C2 Re1 Re1 81.9(3) . 2_656 ? C2 Re1 N1 170.6(4) . . ? C2 Re1 N2 95.0(4) . . ? C3 Re1 Re1 167.1(3) . 2_656 ? C3 Re1 N1 95.8(4) . . ? C3 Re1 N2 97.4(4) . . ? C3 Re1 C2 88.6(4) . . ? C4 N1 Re1 124.2(7) . . ? C4 N1 C8 117.4(9) . . ? C8 N1 Re1 118.1(7) . . ? C9 N2 Re1 116.3(7) . . ? C13 N2 Re1 126.0(7) . . ? C13 N2 C9 117.6(9) . . ? O1 C1 Re1 178.6(9) . . ? O2 C2 Re1 176.2(9) . . ? O3 C3 Re1 174.8(9) . . ? N1 C4 H4 118.7 . . ? N1 C4 C5 122.5(11) . . ? C5 C4 H4 118.7 . . ? C4 C5 H5 120.1 . . ? C4 C5 C6 119.8(11) . . ? C6 C5 H5 120.1 . . ? C5 C6 H6 121.5 . . ? C7 C6 C5 117.0(10) . . ? C7 C6 H6 121.5 . . ? C6 C7 H7 118.4 . . ? C8 C7 C6 123.2(12) . . ? C8 C7 H7 118.4 . . ? N1 C8 C9 111.0(9) . . ? C7 C8 N1 120.1(10) . . ? C7 C8 C9 128.9(11) . . ? N2 C9 C8 118.3(9) . . ? N2 C9 C10 120.2(9) . . ? C10 C9 C8 121.5(10) . . ? C9 C10 H10 119.5 . . ? C11 C10 C9 121.1(10) . . ? C11 C10 H10 119.5 . . ? C10 C11 H11 121.3 . . ? C10 C11 C12 117.3(9) . . ? C12 C11 H11 121.3 . . ? C11 C12 H12 120.0 . . ? C13 C12 C11 120.0(9) . . ? C13 C12 H12 120.0 . . ? N2 C13 C12 123.8(10) . . ? N2 C13 H13 118.1 . . ? C12 C13 H13 118.1 . . ? data_[Re(bpy)(CO)3]2_[K(18-crown-6)(Et2O)] _database_code_depnum_ccdc_archive 'CCDC 876408' #TrackingRef '- Bensons_Xtals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H50 K N4 O13 Re2' _chemical_formula_weight 1304.50 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.9201(8) _cell_length_b 12.4212(12) _cell_length_c 38.087(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.7410(10) _cell_angle_gamma 90.00 _cell_volume 4198.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9621 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 25.38 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.829 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2244 _exptl_absorpt_coefficient_mu 5.924 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5888 _exptl_absorpt_correction_T_max 0.8660 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 32169 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.44 _reflns_number_total 7756 _reflns_number_gt 6688 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; SQUEEZE found two voids containing one disordered Diethyl ether molecules. Their formula was added to the formula for the unit-cell and its electron density removed. 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^)+(0.0000P)^2^+67.8282P] 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_number_reflns 7756 _refine_ls_number_parameters 508 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1083 _refine_ls_wR_factor_gt 0.1050 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.165 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.000 93 37 ' ' 2 0.500 1.000 0.500 93 37 ' ' _platon_squeeze_details ; Two voids were found each containing one disordered Diethyl ether molecule. Their formula was added to the formula for the unit-cell and its electron density removed. ; 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 0.77723(4) 0.66030(3) 0.386181(10) 0.02018(10) Uani 1 1 d . . . Re2 Re 0.87207(4) 0.47534(3) 0.336005(10) 0.01956(10) Uani 1 1 d . . . K1 K 0.6178(2) 0.2295(2) 0.43580(6) 0.0403(6) Uani 1 1 d . . . O1 O 0.9676(9) 0.5337(7) 0.4443(2) 0.046(2) Uani 1 1 d . . . O2 O 0.5276(9) 0.5022(7) 0.4028(2) 0.050(2) Uani 1 1 d . . . O3 O 0.7004(9) 0.8248(6) 0.4417(2) 0.043(2) Uani 1 1 d . . . O4 O 1.1790(8) 0.5422(6) 0.3741(2) 0.0361(18) Uani 1 1 d . . . O5 O 0.8095(9) 0.3358(6) 0.39932(19) 0.0408(19) Uani 1 1 d . . . O6 O 1.0322(8) 0.2805(6) 0.30693(19) 0.0325(17) Uani 1 1 d . . . O7 O 0.3043(7) 0.2582(5) 0.42381(18) 0.0275(16) Uani 1 1 d . . . O8 O 0.4751(8) 0.3538(6) 0.48304(17) 0.0337(17) Uani 1 1 d . . . O9 O 0.7627(8) 0.2643(6) 0.50412(18) 0.0328(17) Uani 1 1 d . . . O10 O 0.9144(7) 0.1551(5) 0.45249(17) 0.0277(15) Uani 1 1 d . . . O11 O 0.7404(7) 0.0728(5) 0.39222(17) 0.0235(15) Uani 1 1 d . . . O12 O 0.4645(7) 0.1708(5) 0.37058(17) 0.0243(15) Uani 1 1 d . . . N1 N 0.9431(8) 0.7603(6) 0.3655(2) 0.0219(17) Uani 1 1 d . . . N2 N 0.6624(9) 0.7341(6) 0.3406(2) 0.0230(18) Uani 1 1 d . . . N3 N 0.8816(8) 0.5825(6) 0.29281(19) 0.0176(16) Uani 1 1 d . . . N4 N 0.6479(8) 0.4758(6) 0.3101(2) 0.0223(17) Uani 1 1 d . . . C1 C 0.8975(12) 0.5846(8) 0.4219(3) 0.030(2) Uani 1 1 d . . . C2 C 0.6202(12) 0.5644(9) 0.3961(3) 0.032(2) Uani 1 1 d . . . C3 C 0.7279(12) 0.7618(8) 0.4199(3) 0.028(2) Uani 1 1 d . . . C4 C 1.0853(10) 0.7754(8) 0.3808(3) 0.029(2) Uani 1 1 d . . . H4 H 1.1158 0.7383 0.4021 0.035 Uiso 1 1 calc R . . C5 C 1.1881(13) 0.8423(10) 0.3668(4) 0.046(3) Uani 1 1 d . . . H5 H 1.2873 0.8508 0.3781 0.055 Uiso 1 1 calc R . . C6 C 1.1399(14) 0.8981(9) 0.3349(3) 0.041(3) Uani 1 1 d . . . H6 H 1.2081 0.9440 0.3244 0.050 Uiso 1 1 calc R . . C7 C 0.9999(14) 0.8861(8) 0.3198(3) 0.038(3) Uani 1 1 d . . . H7 H 0.9683 0.9230 0.2985 0.045 Uiso 1 1 calc R . . C8 C 0.8999(11) 0.8190(7) 0.3353(2) 0.0222(15) Uani 1 1 d . . . C9 C 0.7440(11) 0.8050(7) 0.3220(2) 0.0222(15) Uani 1 1 d . . . C10 C 0.6728(14) 0.8597(9) 0.2920(3) 0.037(3) Uani 1 1 d . . . H10 H 0.7300 0.9061 0.2786 0.045 Uiso 1 1 calc R . . C11 C 0.5222(15) 0.8456(10) 0.2822(3) 0.047(3) Uani 1 1 d . . . H11 H 0.4741 0.8828 0.2624 0.057 Uiso 1 1 calc R . . C12 C 0.4399(13) 0.7756(10) 0.3019(3) 0.041(3) Uani 1 1 d . . . H12 H 0.3347 0.7663 0.2959 0.050 Uiso 1 1 calc R . . C13 C 0.5128(11) 0.7210(9) 0.3297(3) 0.029(2) Uani 1 1 d . . . H13 H 0.4567 0.6712 0.3420 0.035 Uiso 1 1 calc R . . C14 C 1.0615(12) 0.5164(8) 0.3599(3) 0.030(2) Uani 1 1 d . . . C15 C 0.8390(10) 0.3891(8) 0.3751(3) 0.026(2) Uani 1 1 d . . . C16 C 0.9639(11) 0.3563(8) 0.3158(3) 0.026(2) Uani 1 1 d . . . C17 C 1.0087(10) 0.6353(7) 0.2844(2) 0.019(2) Uani 1 1 d . . . H17 H 1.0974 0.6308 0.3004 0.023 Uiso 1 1 calc R . . C18 C 1.0139(11) 0.6936(8) 0.2544(3) 0.028(2) Uani 1 1 d . . . H18 H 1.1055 0.7264 0.2493 0.034 Uiso 1 1 calc R . . C19 C 0.8855(12) 0.7049(8) 0.2312(3) 0.031(2) Uani 1 1 d . . . H19 H 0.8874 0.7471 0.2104 0.037 Uiso 1 1 calc R . . C20 C 0.7545(11) 0.6546(8) 0.2386(2) 0.026(2) Uani 1 1 d . . . H20 H 0.6656 0.6619 0.2228 0.032 Uiso 1 1 calc R . . C21 C 0.7525(10) 0.5920(7) 0.2696(2) 0.019(2) Uani 1 1 d . . . C22 C 0.6245(10) 0.5373(7) 0.2796(2) 0.020(2) Uani 1 1 d . . . C23 C 0.4784(11) 0.5435(8) 0.2608(3) 0.026(2) Uani 1 1 d . . . H23 H 0.4626 0.5867 0.2401 0.031 Uiso 1 1 calc R . . C24 C 0.3607(10) 0.4874(8) 0.2724(3) 0.028(2) Uani 1 1 d . . . H24 H 0.2635 0.4898 0.2597 0.033 Uiso 1 1 calc R . . C25 C 0.3863(11) 0.4263(9) 0.3033(3) 0.030(2) Uani 1 1 d . . . H25 H 0.3061 0.3873 0.3119 0.036 Uiso 1 1 calc R . . C26 C 0.5270(10) 0.4229(8) 0.3209(3) 0.025(2) Uani 1 1 d . . . H26 H 0.5414 0.3814 0.3419 0.030 Uiso 1 1 calc R . . C27 C 0.2488(11) 0.3463(9) 0.4439(3) 0.033(2) Uani 1 1 d . . . H27A H 0.1375 0.3437 0.4427 0.039 Uiso 1 1 calc R . . H27B H 0.2785 0.4161 0.4341 0.039 Uiso 1 1 calc R . . C28 C 0.3160(12) 0.3348(9) 0.4812(3) 0.036(3) Uani 1 1 d . . . H28A H 0.2689 0.3871 0.4963 0.044 Uiso 1 1 calc R . . H28B H 0.2968 0.2614 0.4898 0.044 Uiso 1 1 calc R . . C29 C 0.5431(12) 0.3572(10) 0.5185(3) 0.036(3) Uani 1 1 d . . . H29A H 0.5162 0.2918 0.5313 0.044 Uiso 1 1 calc R . . H29B H 0.5067 0.4208 0.5308 0.044 Uiso 1 1 calc R . . C30 C 0.7114(13) 0.3634(9) 0.5178(3) 0.036(3) Uani 1 1 d . . . H30A H 0.7374 0.4241 0.5027 0.044 Uiso 1 1 calc R . . H30B H 0.7606 0.3757 0.5419 0.044 Uiso 1 1 calc R . . C31 C 0.9217(12) 0.2613(9) 0.5048(3) 0.039(3) Uani 1 1 d . . . H31A H 0.9683 0.2678 0.5294 0.047 Uiso 1 1 calc R . . H31B H 0.9568 0.3222 0.4910 0.047 Uiso 1 1 calc R . . C32 C 0.9674(12) 0.1566(9) 0.4892(3) 0.037(3) Uani 1 1 d . . . H32A H 1.0785 0.1493 0.4922 0.044 Uiso 1 1 calc R . . H32B H 0.9235 0.0956 0.5014 0.044 Uiso 1 1 calc R . . C33 C 0.9485(12) 0.0555(7) 0.4357(3) 0.030(2) Uani 1 1 d . . . H33A H 0.8941 -0.0047 0.4458 0.036 Uiso 1 1 calc R . . H33B H 1.0580 0.0406 0.4396 0.036 Uiso 1 1 calc R . . C34 C 0.9016(11) 0.0654(9) 0.3977(3) 0.030(2) Uani 1 1 d . . . H34A H 0.9475 0.1305 0.3883 0.037 Uiso 1 1 calc R . . H34B H 0.9364 0.0019 0.3851 0.037 Uiso 1 1 calc R . . C35 C 0.6903(11) 0.0876(9) 0.3560(2) 0.028(2) Uani 1 1 d . . . H35A H 0.7320 0.0306 0.3416 0.033 Uiso 1 1 calc R . . H35B H 0.7243 0.1584 0.3478 0.033 Uiso 1 1 calc R . . C36 C 0.5202(11) 0.0822(8) 0.3523(3) 0.026(2) Uani 1 1 d . . . H36A H 0.4811 0.0852 0.3270 0.032 Uiso 1 1 calc R . . H36B H 0.4866 0.0138 0.3623 0.032 Uiso 1 1 calc R . . C37 C 0.3034(10) 0.1725(8) 0.3677(3) 0.030(2) Uani 1 1 d . . . H37A H 0.2649 0.1061 0.3780 0.036 Uiso 1 1 calc R . . H37B H 0.2627 0.1764 0.3426 0.036 Uiso 1 1 calc R . . C38 C 0.2539(11) 0.2705(8) 0.3874(3) 0.030(2) Uani 1 1 d . . . H38A H 0.2975 0.3365 0.3781 0.035 Uiso 1 1 calc R . . H38B H 0.1427 0.2769 0.3843 0.035 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 0.02104(19) 0.0215(2) 0.01822(19) -0.00086(16) 0.00290(14) -0.00479(16) Re2 0.01975(19) 0.01542(19) 0.0225(2) 0.00049(15) -0.00303(14) 0.00112(16) K1 0.0211(11) 0.0709(19) 0.0290(13) -0.0127(12) 0.0037(9) 0.0111(12) O1 0.057(5) 0.051(5) 0.024(4) -0.001(4) -0.016(4) -0.001(4) O2 0.054(5) 0.055(6) 0.044(5) -0.017(4) 0.027(4) -0.037(5) O3 0.057(5) 0.035(5) 0.040(5) -0.013(4) 0.027(4) -0.018(4) O4 0.027(4) 0.026(4) 0.052(5) -0.010(4) -0.014(3) 0.001(3) O5 0.071(6) 0.017(4) 0.033(4) 0.013(3) 0.000(4) -0.010(4) O6 0.031(4) 0.026(4) 0.038(4) -0.009(3) -0.009(3) 0.003(3) O7 0.027(4) 0.021(4) 0.035(4) 0.003(3) 0.006(3) 0.009(3) O8 0.041(4) 0.038(4) 0.024(4) 0.002(3) 0.013(3) 0.004(4) O9 0.037(4) 0.030(4) 0.032(4) -0.004(3) 0.004(3) -0.001(3) O10 0.034(4) 0.017(3) 0.032(4) -0.003(3) -0.002(3) 0.011(3) O11 0.017(3) 0.022(4) 0.031(4) 0.003(3) 0.002(3) 0.006(3) O12 0.016(3) 0.024(4) 0.033(4) -0.004(3) 0.000(3) 0.001(3) N1 0.022(4) 0.019(4) 0.024(4) -0.005(3) 0.003(3) -0.004(3) N2 0.022(4) 0.022(4) 0.025(4) -0.010(3) 0.002(3) 0.000(3) N3 0.020(4) 0.011(4) 0.022(4) -0.004(3) 0.002(3) 0.001(3) N4 0.018(4) 0.017(4) 0.031(5) -0.001(4) 0.001(3) 0.000(3) C1 0.038(6) 0.020(5) 0.031(6) -0.013(5) 0.003(5) -0.014(5) C2 0.036(6) 0.030(6) 0.031(6) -0.013(5) 0.014(5) -0.004(5) C3 0.034(6) 0.019(5) 0.033(6) -0.001(5) 0.005(5) -0.012(4) C4 0.012(5) 0.021(5) 0.055(7) -0.012(5) 0.003(4) 0.006(4) C5 0.036(6) 0.032(7) 0.073(9) -0.023(7) 0.020(6) -0.015(6) C6 0.046(7) 0.017(6) 0.067(9) -0.013(6) 0.033(6) -0.015(5) C7 0.059(8) 0.014(5) 0.044(7) -0.009(5) 0.029(6) -0.012(5) C8 0.034(4) 0.011(3) 0.022(4) -0.006(3) 0.008(3) 0.006(3) C9 0.034(4) 0.011(3) 0.022(4) -0.006(3) 0.008(3) 0.006(3) C10 0.057(8) 0.028(6) 0.027(6) 0.001(5) 0.004(5) 0.018(6) C11 0.069(9) 0.044(7) 0.026(6) -0.011(6) -0.011(6) 0.033(7) C12 0.037(6) 0.041(7) 0.043(7) -0.021(6) -0.009(5) 0.018(6) C13 0.019(5) 0.032(6) 0.036(6) -0.016(5) -0.003(4) 0.009(4) C14 0.046(7) 0.007(5) 0.033(6) 0.005(4) -0.005(5) 0.005(5) C15 0.006(4) 0.031(6) 0.041(6) -0.001(5) 0.005(4) 0.007(4) C16 0.021(5) 0.026(6) 0.030(5) 0.004(4) -0.002(4) 0.001(4) C17 0.011(4) 0.024(5) 0.023(5) -0.003(4) 0.001(4) 0.002(4) C18 0.025(5) 0.027(6) 0.034(6) -0.004(5) 0.007(4) -0.006(4) C19 0.041(6) 0.028(6) 0.024(5) -0.001(4) 0.008(5) 0.004(5) C20 0.029(5) 0.025(5) 0.024(5) -0.002(4) -0.003(4) 0.009(5) C21 0.026(5) 0.012(5) 0.019(5) -0.005(4) 0.001(4) 0.008(4) C22 0.023(5) 0.015(5) 0.022(5) -0.008(4) 0.001(4) 0.008(4) C23 0.028(5) 0.023(6) 0.025(5) -0.009(4) -0.004(4) 0.005(4) C24 0.010(4) 0.035(6) 0.037(6) -0.015(5) -0.005(4) 0.002(4) C25 0.018(5) 0.036(6) 0.036(6) -0.008(5) 0.007(4) -0.008(4) C26 0.024(5) 0.022(5) 0.029(5) -0.006(4) 0.007(4) -0.004(4) C27 0.026(5) 0.033(6) 0.043(6) 0.007(5) 0.016(5) 0.008(5) C28 0.045(7) 0.032(6) 0.035(6) 0.003(5) 0.016(5) -0.001(5) C29 0.042(6) 0.040(7) 0.027(6) 0.002(5) 0.006(5) 0.001(5) C30 0.049(7) 0.029(6) 0.030(6) -0.007(5) -0.001(5) 0.004(5) C31 0.038(6) 0.038(7) 0.040(7) -0.013(5) -0.001(5) -0.009(5) C32 0.036(6) 0.032(6) 0.039(6) 0.005(5) -0.011(5) 0.009(5) C33 0.036(6) 0.010(5) 0.043(7) -0.006(4) -0.006(5) 0.011(4) C34 0.024(5) 0.028(6) 0.040(6) -0.006(5) 0.003(5) 0.013(4) C35 0.031(6) 0.032(6) 0.020(5) -0.006(4) 0.004(4) -0.001(5) C36 0.029(5) 0.022(5) 0.028(5) -0.006(4) 0.002(4) -0.002(4) C37 0.018(5) 0.029(6) 0.041(6) 0.004(5) -0.007(4) -0.001(4) C38 0.023(5) 0.023(5) 0.042(6) -0.002(5) 0.002(5) 0.005(4) _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 C3 1.883(10) . ? Re1 C1 1.897(12) . ? Re1 C2 1.906(10) . ? Re1 N2 2.133(8) . ? Re1 N1 2.142(7) . ? Re1 Re2 3.1574(6) . ? Re2 C15 1.881(10) . ? Re2 C16 1.891(10) . ? Re2 C14 1.906(11) . ? Re2 N3 2.124(7) . ? Re2 N4 2.140(8) . ? K1 O5 2.659(8) . ? K1 O8 2.775(7) . ? K1 O12 2.810(7) . ? K1 O7 2.811(7) . ? K1 O10 2.814(7) . ? K1 O9 2.820(8) . ? K1 O11 2.846(7) . ? O1 C1 1.188(13) . ? O2 C2 1.177(12) . ? O3 C3 1.185(12) . ? O4 C14 1.176(12) . ? O5 C15 1.187(12) . ? O6 C16 1.189(12) . ? O7 C38 1.422(12) . ? O7 C27 1.450(12) . ? O8 C29 1.425(12) . ? O8 C28 1.433(13) . ? O9 C31 1.416(13) . ? O9 C30 1.430(12) . ? O10 C32 1.431(12) . ? O10 C33 1.439(11) . ? O11 C35 1.419(11) . ? O11 C34 1.435(11) . ? O12 C36 1.418(11) . ? O12 C37 1.430(11) . ? N1 C4 1.354(12) . ? N1 C8 1.385(12) . ? N2 C13 1.367(12) . ? N2 C9 1.382(12) . ? N3 C17 1.375(11) . ? N3 C21 1.385(12) . ? N4 C26 1.361(11) . ? N4 C22 1.387(12) . ? C4 C5 1.382(15) . ? C4 H4 0.9500 . ? C5 C6 1.428(18) . ? C5 H5 0.9500 . ? C6 C7 1.330(17) . ? C6 H6 0.9500 . ? C7 C8 1.395(13) . ? C7 H7 0.9500 . ? C8 C9 1.441(14) . ? C9 C10 1.424(14) . ? C10 C11 1.369(17) . ? C10 H10 0.9500 . ? C11 C12 1.401(18) . ? C11 H11 0.9500 . ? C12 C13 1.367(15) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C17 C18 1.358(13) . ? C17 H17 0.9500 . ? C18 C19 1.381(14) . ? C18 H18 0.9500 . ? C19 C20 1.379(14) . ? C19 H19 0.9500 . ? C20 C21 1.416(13) . ? C20 H20 0.9500 . ? C21 C22 1.414(13) . ? C22 C23 1.426(13) . ? C23 C24 1.369(13) . ? C23 H23 0.9500 . ? C24 C25 1.400(15) . ? C24 H24 0.9500 . ? C25 C26 1.364(14) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.493(15) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.506(15) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.503(15) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.471(14) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.512(13) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.518(14) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? 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 C3 Re1 C1 89.8(4) . . ? C3 Re1 C2 93.2(4) . . ? C1 Re1 C2 85.5(5) . . ? C3 Re1 N2 98.1(4) . . ? C1 Re1 N2 171.4(4) . . ? C2 Re1 N2 97.3(4) . . ? C3 Re1 N1 94.5(4) . . ? C1 Re1 N1 100.9(4) . . ? C2 Re1 N1 169.9(4) . . ? N2 Re1 N1 75.2(3) . . ? C3 Re1 Re2 174.3(3) . . ? C1 Re1 Re2 84.7(3) . . ? C2 Re1 Re2 85.0(3) . . ? N2 Re1 Re2 87.5(2) . . ? N1 Re1 Re2 87.9(2) . . ? C15 Re2 C16 89.1(4) . . ? C15 Re2 C14 88.7(4) . . ? C16 Re2 C14 90.2(4) . . ? C15 Re2 N3 172.4(3) . . ? C16 Re2 N3 97.0(3) . . ? C14 Re2 N3 95.7(4) . . ? C15 Re2 N4 98.8(3) . . ? C16 Re2 N4 103.7(4) . . ? C14 Re2 N4 164.2(4) . . ? N3 Re2 N4 75.5(3) . . ? C15 Re2 Re1 82.1(3) . . ? C16 Re2 Re1 165.6(3) . . ? C14 Re2 Re1 78.2(3) . . ? N3 Re2 Re1 92.69(19) . . ? N4 Re2 Re1 89.0(2) . . ? O5 K1 O8 115.1(2) . . ? O5 K1 O12 87.0(2) . . ? O8 K1 O12 120.2(2) . . ? O5 K1 O7 122.2(2) . . ? O8 K1 O7 61.4(2) . . ? O12 K1 O7 60.04(19) . . ? O5 K1 O10 69.0(2) . . ? O8 K1 O10 121.2(2) . . ? O12 K1 O10 118.6(2) . . ? O7 K1 O10 167.4(2) . . ? O5 K1 O9 98.5(2) . . ? O8 K1 O9 60.9(2) . . ? O12 K1 O9 173.2(2) . . ? O7 K1 O9 119.2(2) . . ? O10 K1 O9 60.5(2) . . ? O5 K1 O11 74.3(2) . . ? O8 K1 O11 170.6(2) . . ? O12 K1 O11 59.22(19) . . ? O7 K1 O11 115.2(2) . . ? O10 K1 O11 60.00(19) . . ? O9 K1 O11 118.4(2) . . ? C15 O5 K1 152.6(7) . . ? C38 O7 C27 110.0(7) . . ? C38 O7 K1 112.6(5) . . ? C27 O7 K1 113.4(6) . . ? C29 O8 C28 112.2(7) . . ? C29 O8 K1 116.8(6) . . ? C28 O8 K1 113.1(6) . . ? C31 O9 C30 111.9(8) . . ? C31 O9 K1 112.2(6) . . ? C30 O9 K1 109.5(6) . . ? C32 O10 C33 112.4(7) . . ? C32 O10 K1 115.4(6) . . ? C33 O10 K1 114.7(6) . . ? C35 O11 C34 111.3(7) . . ? C35 O11 K1 112.1(5) . . ? C34 O11 K1 113.4(5) . . ? C36 O12 C37 111.9(7) . . ? C36 O12 K1 118.2(5) . . ? C37 O12 K1 117.4(5) . . ? C4 N1 C8 117.1(8) . . ? C4 N1 Re1 125.0(7) . . ? C8 N1 Re1 117.8(6) . . ? C13 N2 C9 117.9(9) . . ? C13 N2 Re1 124.8(7) . . ? C9 N2 Re1 117.2(6) . . ? C17 N3 C21 117.6(8) . . ? C17 N3 Re2 125.2(6) . . ? C21 N3 Re2 116.9(6) . . ? C26 N4 C22 117.5(8) . . ? C26 N4 Re2 126.2(7) . . ? C22 N4 Re2 116.3(6) . . ? O1 C1 Re1 177.0(9) . . ? O2 C2 Re1 177.3(11) . . ? O3 C3 Re1 178.1(10) . . ? N1 C4 C5 123.2(11) . . ? N1 C4 H4 118.4 . . ? C5 C4 H4 118.4 . . ? C4 C5 C6 117.7(11) . . ? C4 C5 H5 121.2 . . ? C6 C5 H5 121.2 . . ? C7 C6 C5 120.3(10) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.8 . . ? C6 C7 C8 119.7(11) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? N1 C8 C7 122.0(10) . . ? N1 C8 C9 114.0(8) . . ? C7 C8 C9 124.0(10) . . ? N2 C9 C10 120.0(10) . . ? N2 C9 C8 115.9(8) . . ? C10 C9 C8 124.2(9) . . ? C11 C10 C9 120.3(11) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 119.2(11) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C13 C12 C11 119.2(11) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 N2 123.4(11) . . ? C12 C13 H13 118.3 . . ? N2 C13 H13 118.3 . . ? O4 C14 Re2 179.1(9) . . ? O5 C15 Re2 176.2(8) . . ? O6 C16 Re2 172.0(8) . . ? C18 C17 N3 123.3(9) . . ? C18 C17 H17 118.4 . . ? N3 C17 H17 118.4 . . ? C17 C18 C19 119.8(9) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C20 C19 C18 119.3(10) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C19 C20 C21 120.0(9) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? N3 C21 C22 115.4(8) . . ? N3 C21 C20 120.1(8) . . ? C22 C21 C20 124.6(9) . . ? N4 C22 C21 115.7(8) . . ? N4 C22 C23 120.3(8) . . ? C21 C22 C23 124.0(9) . . ? C24 C23 C22 120.1(9) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 118.8(9) . . ? C23 C24 H24 120.6 . . ? C25 C24 H24 120.6 . . ? C26 C25 C24 119.7(9) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? N4 C26 C25 123.6(10) . . ? N4 C26 H26 118.2 . . ? C25 C26 H26 118.2 . . ? O7 C27 C28 107.7(8) . . ? O7 C27 H27A 110.2 . . ? C28 C27 H27A 110.2 . . ? O7 C27 H27B 110.2 . . ? C28 C27 H27B 110.2 . . ? H27A C27 H27B 108.5 . . ? O8 C28 C27 109.4(8) . . ? O8 C28 H28A 109.8 . . ? C27 C28 H28A 109.8 . . ? O8 C28 H28B 109.8 . . ? C27 C28 H28B 109.8 . . ? H28A C28 H28B 108.2 . . ? O8 C29 C30 108.4(8) . . ? O8 C29 H29A 110.0 . . ? C30 C29 H29A 110.0 . . ? O8 C29 H29B 110.0 . . ? C30 C29 H29B 110.0 . . ? H29A C29 H29B 108.4 . . ? O9 C30 C29 108.6(9) . . ? O9 C30 H30A 110.0 . . ? C29 C30 H30A 110.0 . . ? O9 C30 H30B 110.0 . . ? C29 C30 H30B 110.0 . . ? H30A C30 H30B 108.4 . . ? O9 C31 C32 109.1(9) . . ? O9 C31 H31A 109.9 . . ? C32 C31 H31A 109.9 . . ? O9 C31 H31B 109.9 . . ? C32 C31 H31B 109.9 . . ? H31A C31 H31B 108.3 . . ? O10 C32 C31 108.7(9) . . ? O10 C32 H32A 110.0 . . ? C31 C32 H32A 110.0 . . ? O10 C32 H32B 110.0 . . ? C31 C32 H32B 110.0 . . ? H32A C32 H32B 108.3 . . ? O10 C33 C34 108.2(8) . . ? O10 C33 H33A 110.1 . . ? C34 C33 H33A 110.1 . . ? O10 C33 H33B 110.1 . . ? C34 C33 H33B 110.1 . . ? H33A C33 H33B 108.4 . . ? O11 C34 C33 109.3(8) . . ? O11 C34 H34A 109.8 . . ? C33 C34 H34A 109.8 . . ? O11 C34 H34B 109.8 . . ? C33 C34 H34B 109.8 . . ? H34A C34 H34B 108.3 . . ? O11 C35 C36 107.5(7) . . ? O11 C35 H35A 110.2 . . ? C36 C35 H35A 110.2 . . ? O11 C35 H35B 110.2 . . ? C36 C35 H35B 110.2 . . ? H35A C35 H35B 108.5 . . ? O12 C36 C35 108.5(8) . . ? O12 C36 H36A 110.0 . . ? C35 C36 H36A 110.0 . . ? O12 C36 H36B 110.0 . . ? C35 C36 H36B 110.0 . . ? H36A C36 H36B 108.4 . . ? O12 C37 C38 108.3(8) . . ? O12 C37 H37A 110.0 . . ? C38 C37 H37A 110.0 . . ? O12 C37 H37B 110.0 . . ? C38 C37 H37B 110.0 . . ? H37A C37 H37B 108.4 . . ? O7 C38 C37 108.5(8) . . ? O7 C38 H38A 110.0 . . ? C37 C38 H38A 110.0 . . ? O7 C38 H38B 110.0 . . ? C37 C38 H38B 110.0 . . ? H38A C38 H38B 108.4 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.960 _refine_diff_density_min -2.675 _refine_diff_density_rms 0.191 data_[Re(bpy)(CO)3]2_[K(THF)2] _database_code_depnum_ccdc_archive 'CCDC 876409' #TrackingRef '- Bensons_Xtals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H32 K N4 O8 Re2' _chemical_formula_weight 1036.14 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.8574(5) _cell_length_b 11.5882(7) _cell_length_c 32.4500(18) _cell_angle_alpha 90.00 _cell_angle_beta 95.504(3) _cell_angle_gamma 90.00 _cell_volume 3315.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9884 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 25.35 _exptl_crystal_description plate _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.076 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1988 _exptl_absorpt_coefficient_mu 7.480 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5217 _exptl_absorpt_correction_T_max 0.9290 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23718 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 25.38 _reflns_number_total 6067 _reflns_number_gt 5576 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0150P)^2^+10.3819P] 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_number_reflns 6067 _refine_ls_number_parameters 441 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0508 _refine_ls_wR_factor_gt 0.0429 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.140 _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 0.067724(19) 0.318293(15) 0.089524(5) 0.01333(5) Uani 1 1 d . C . Re2 Re 0.197594(18) 0.091535(14) 0.132038(5) 0.01337(5) Uani 1 1 d . C . K1 K -0.31468(11) -0.02022(8) 0.03243(3) 0.0230(2) Uani 1 1 d . . . O1 O -0.2282(3) 0.1795(3) 0.08378(10) 0.0251(7) Uani 1 1 d . . . O2 O 0.1513(4) 0.1938(3) 0.01130(10) 0.0288(8) Uani 1 1 d . . . O3 O -0.0873(4) 0.5164(3) 0.03983(11) 0.0370(9) Uani 1 1 d . . . O4 O -0.0136(4) -0.0213(3) 0.06339(11) 0.0325(9) Uani 1 1 d . . . O5 O 0.4327(4) 0.0934(3) 0.06832(10) 0.0250(7) Uani 1 1 d . . . O6 O 0.3207(4) -0.1423(3) 0.16329(11) 0.0318(8) Uani 1 1 d . . . O7 O -0.5881(3) -0.1552(3) 0.02176(10) 0.0224(7) Uani 1 1 d . . . O8 O -0.2768(4) -0.1655(4) 0.09451(11) 0.0402(10) Uani 1 1 d . C . N1 N 0.0493(4) 0.3975(3) 0.14828(10) 0.0125(7) Uani 1 1 d . . . N2 N 0.2822(4) 0.3981(3) 0.10539(11) 0.0154(8) Uani 1 1 d . . . N3 N 0.0383(4) 0.1152(3) 0.17654(11) 0.0144(7) Uani 1 1 d . . . N4 N 0.3118(4) 0.1979(3) 0.17862(11) 0.0139(7) Uani 1 1 d . . . C1 C -0.1164(5) 0.2322(4) 0.08620(13) 0.0167(9) Uani 1 1 d . . . C2 C 0.1178(5) 0.2418(4) 0.04048(14) 0.0204(10) Uani 1 1 d . . . C3 C -0.0250(5) 0.4432(4) 0.05905(14) 0.0236(10) Uani 1 1 d . . . C4 C 0.4043(5) 0.3888(4) 0.08333(15) 0.0229(10) Uani 1 1 d . . . H4 H 0.3941 0.3442 0.0587 0.028 Uiso 1 1 calc R . . C5 C 0.5406(5) 0.4398(4) 0.09450(16) 0.0268(11) Uani 1 1 d . . . H5 H 0.6231 0.4298 0.0781 0.032 Uiso 1 1 calc R . . C6 C 0.5572(5) 0.5071(4) 0.13038(16) 0.0245(11) Uani 1 1 d . . . H6 H 0.6511 0.5436 0.1388 0.029 Uiso 1 1 calc R . . C7 C 0.4363(5) 0.5193(4) 0.15309(14) 0.0192(10) Uani 1 1 d . . . H7 H 0.4454 0.5661 0.1772 0.023 Uiso 1 1 calc R . . C8 C 0.2988(5) 0.4633(4) 0.14105(13) 0.0143(9) Uani 1 1 d . . . C9 C 0.1695(5) 0.4660(3) 0.16400(12) 0.0116(8) Uani 1 1 d . . . C10 C 0.1597(5) 0.5306(4) 0.20027(13) 0.0159(9) Uani 1 1 d . . . H10 H 0.2430 0.5772 0.2107 0.019 Uiso 1 1 calc R . . C11 C 0.0324(5) 0.5273(4) 0.22067(13) 0.0158(9) Uani 1 1 d . . . H11 H 0.0260 0.5710 0.2452 0.019 Uiso 1 1 calc R . . C12 C -0.0888(5) 0.4582(4) 0.20475(13) 0.0165(9) Uani 1 1 d . . . H12 H -0.1791 0.4545 0.2183 0.020 Uiso 1 1 calc R . . C13 C -0.0759(5) 0.3959(4) 0.16950(13) 0.0153(9) Uani 1 1 d . . . H13 H -0.1589 0.3488 0.1592 0.018 Uiso 1 1 calc R . . C14 C 0.0652(5) 0.0194(4) 0.08986(15) 0.0214(10) Uani 1 1 d . . . C15 C 0.3446(5) 0.0950(4) 0.09304(14) 0.0175(9) Uani 1 1 d . . . C16 C 0.2736(5) -0.0522(4) 0.15320(14) 0.0208(10) Uani 1 1 d . . . C17 C -0.1041(5) 0.0695(4) 0.17403(14) 0.0187(10) Uani 1 1 d . . . H17 H -0.1383 0.0264 0.1500 0.022 Uiso 1 1 calc R . . C18 C -0.1998(5) 0.0825(4) 0.20416(14) 0.0220(10) Uani 1 1 d . . . H18 H -0.2982 0.0491 0.2010 0.026 Uiso 1 1 calc R . . C19 C -0.1517(5) 0.1455(4) 0.23969(14) 0.0220(10) Uani 1 1 d . . . H19 H -0.2164 0.1547 0.2612 0.026 Uiso 1 1 calc R . . C20 C -0.0109(5) 0.1935(4) 0.24315(13) 0.0186(10) Uani 1 1 d . . . H20 H 0.0226 0.2376 0.2670 0.022 Uiso 1 1 calc R . . C21 C 0.0855(5) 0.1780(4) 0.21144(13) 0.0164(9) Uani 1 1 d . . . C22 C 0.2352(5) 0.2241(4) 0.21243(13) 0.0148(9) Uani 1 1 d . . . C23 C 0.3040(5) 0.2944(4) 0.24434(14) 0.0207(10) Uani 1 1 d . . . H23 H 0.2491 0.3151 0.2670 0.025 Uiso 1 1 calc R . . C24 C 0.4481(5) 0.3327(4) 0.24288(15) 0.0238(10) Uani 1 1 d . . . H24 H 0.4940 0.3811 0.2642 0.029 Uiso 1 1 calc R . . C25 C 0.5289(5) 0.3000(4) 0.20949(14) 0.0211(10) Uani 1 1 d . . . H25 H 0.6315 0.3229 0.2085 0.025 Uiso 1 1 calc R . . C26 C 0.4577(5) 0.2353(4) 0.17887(14) 0.0177(9) Uani 1 1 d . . . H26 H 0.5125 0.2147 0.1562 0.021 Uiso 1 1 calc R . . C27 C -0.5448(7) -0.2641(5) 0.00635(18) 0.0388(14) Uani 1 1 d . B . H27A H -0.4402 -0.2849 0.0173 0.047 Uiso 1 1 calc R A 1 H27B H -0.5521 -0.2646 -0.0243 0.047 Uiso 1 1 calc R A 1 C28A C -0.645(2) -0.3489(14) 0.0101(5) 0.0460(19) Uani 0.50 1 d P B 2 H28A H -0.5959 -0.4255 0.0127 0.055 Uiso 0.50 1 calc PR B 2 H28B H -0.7256 -0.3498 -0.0133 0.055 Uiso 0.50 1 calc PR B 2 C28B C -0.665(2) -0.3479(14) 0.0232(5) 0.0460(19) Uani 0.50 1 d P B 1 H28C H -0.7174 -0.3909 -0.0003 0.055 Uiso 0.50 1 calc PR B 1 H28D H -0.6111 -0.4047 0.0422 0.055 Uiso 0.50 1 calc PR B 1 C29A C -0.717(2) -0.3041(13) 0.0574(4) 0.0460(19) Uani 0.50 1 d P B 2 H29A H -0.8184 -0.3352 0.0611 0.055 Uiso 0.50 1 calc PR B 2 H29B H -0.6452 -0.3186 0.0823 0.055 Uiso 0.50 1 calc PR B 2 C29B C -0.749(2) -0.3013(13) 0.0398(4) 0.0460(19) Uani 0.50 1 d P B 1 H29C H -0.7750 -0.3479 0.0637 0.055 Uiso 0.50 1 calc PR B 1 H29D H -0.8430 -0.2898 0.0211 0.055 Uiso 0.50 1 calc PR B 1 C30A C -0.719(2) -0.1740(16) 0.0424(5) 0.0460(19) Uani 0.50 1 d P . 2 H30A H -0.8111 -0.1589 0.0235 0.055 Uiso 0.50 1 calc PR . 2 H30B H -0.7190 -0.1215 0.0665 0.055 Uiso 0.50 1 calc PR . 2 C30B C -0.682(2) -0.1765(16) 0.0560(5) 0.0460(19) Uani 0.50 1 d P B 1 H30C H -0.7630 -0.1178 0.0572 0.055 Uiso 0.50 1 calc PR B 1 H30D H -0.6212 -0.1819 0.0831 0.055 Uiso 0.50 1 calc PR B 1 C31A C -0.3591(11) -0.1655(8) 0.1272(3) 0.0218(11) Uani 0.545(7) 1 d PD C 2 H31A H -0.4534 -0.2107 0.1210 0.026 Uiso 0.545(7) 1 calc PR C 2 H31B H -0.3864 -0.0858 0.1345 0.026 Uiso 0.545(7) 1 calc PR C 2 C31B C -0.3030(15) -0.1922(10) 0.1400(4) 0.0356(14) Uani 0.506(8) 1 d P C 1 H31C H -0.3300 -0.1214 0.1548 0.043 Uiso 0.506(8) 1 calc PR C 1 H31D H -0.3843 -0.2502 0.1416 0.043 Uiso 0.506(8) 1 calc PR C 1 C32A C -0.2566(11) -0.2217(8) 0.1630(3) 0.0218(11) Uani 0.545(7) 1 d PD C 2 H32A H -0.2370 -0.1674 0.1864 0.026 Uiso 0.545(7) 1 calc PR C 2 H32B H -0.3038 -0.2926 0.1729 0.026 Uiso 0.545(7) 1 calc PR C 2 C32B C -0.1523(17) -0.2387(11) 0.1577(4) 0.0356(14) Uani 0.506(8) 1 d P C 1 H32C H -0.0861 -0.1756 0.1694 0.043 Uiso 0.506(8) 1 calc PR C 1 H32D H -0.1654 -0.2959 0.1797 0.043 Uiso 0.506(8) 1 calc PR C 1 C33A C -0.1106(12) -0.2498(11) 0.1438(4) 0.0218(11) Uani 0.455(7) 1 d PD C 2 H33A H -0.0314 -0.1911 0.1511 0.026 Uiso 0.455(7) 1 calc PR C 2 H33B H -0.0713 -0.3268 0.1525 0.026 Uiso 0.455(7) 1 calc PR C 2 C33B C -0.0882(14) -0.2924(10) 0.1230(4) 0.0356(14) Uani 0.494(8) 1 d P C 1 H33C H -0.0746 -0.3763 0.1279 0.043 Uiso 0.494(8) 1 calc PR C 1 H33D H 0.0119 -0.2581 0.1192 0.043 Uiso 0.494(8) 1 calc PR C 1 C34A C -0.1615(14) -0.2474(11) 0.0983(3) 0.0218(11) Uani 0.455(7) 1 d PD C 2 H34A H -0.0772 -0.2246 0.0821 0.026 Uiso 0.455(7) 1 calc PR C 2 H34B H -0.1999 -0.3239 0.0886 0.026 Uiso 0.455(7) 1 calc PR C 2 C34B C -0.1943(16) -0.2725(11) 0.0860(4) 0.0356(14) Uani 0.494(8) 1 d P C 1 H34C H -0.2656 -0.3380 0.0814 0.043 Uiso 0.494(8) 1 calc PR C 1 H34D H -0.1387 -0.2630 0.0612 0.043 Uiso 0.494(8) 1 calc PR C 1 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 0.01293(9) 0.01439(9) 0.01247(9) -0.00309(7) 0.00011(6) 0.00028(7) Re2 0.00980(9) 0.01280(9) 0.01771(9) -0.00212(7) 0.00235(6) -0.00032(6) K1 0.0165(5) 0.0196(5) 0.0316(6) -0.0018(4) -0.0046(4) 0.0004(4) O1 0.0145(17) 0.0234(18) 0.036(2) -0.0082(15) -0.0031(14) -0.0006(14) O2 0.0285(19) 0.038(2) 0.0204(17) -0.0141(16) 0.0027(14) 0.0032(16) O3 0.047(2) 0.034(2) 0.029(2) 0.0068(17) 0.0011(17) 0.0159(18) O4 0.0169(17) 0.033(2) 0.046(2) -0.0235(18) -0.0070(16) 0.0013(15) O5 0.0193(17) 0.0234(18) 0.0342(19) -0.0014(15) 0.0119(15) -0.0022(14) O6 0.042(2) 0.0221(19) 0.033(2) 0.0106(16) 0.0163(17) 0.0154(17) O7 0.0214(17) 0.0211(17) 0.0254(17) -0.0046(14) 0.0066(14) -0.0004(14) O8 0.035(2) 0.058(3) 0.028(2) 0.0071(18) 0.0041(16) 0.0256(19) N1 0.0115(17) 0.0142(18) 0.0116(17) -0.0008(14) 0.0001(14) 0.0012(14) N2 0.0184(19) 0.0115(18) 0.0167(18) -0.0016(15) 0.0042(15) -0.0017(15) N3 0.0137(18) 0.0121(18) 0.0178(19) -0.0003(15) 0.0031(15) 0.0002(14) N4 0.0116(18) 0.0122(18) 0.0172(18) 0.0023(14) -0.0018(14) -0.0002(14) C1 0.018(2) 0.013(2) 0.018(2) -0.0036(18) -0.0012(18) 0.0064(19) C2 0.013(2) 0.027(3) 0.021(2) -0.002(2) -0.0027(18) -0.0032(19) C3 0.029(3) 0.024(3) 0.018(2) -0.002(2) 0.002(2) 0.003(2) C4 0.026(3) 0.018(2) 0.026(3) -0.005(2) 0.012(2) -0.002(2) C5 0.022(3) 0.022(3) 0.039(3) -0.007(2) 0.015(2) -0.003(2) C6 0.017(2) 0.016(2) 0.042(3) -0.001(2) 0.007(2) -0.0042(19) C7 0.017(2) 0.012(2) 0.028(3) -0.0026(19) 0.0008(19) -0.0004(18) C8 0.013(2) 0.011(2) 0.019(2) 0.0025(17) 0.0011(17) -0.0010(17) C9 0.014(2) 0.0066(19) 0.014(2) 0.0010(16) -0.0004(16) 0.0007(16) C10 0.017(2) 0.010(2) 0.021(2) -0.0019(17) -0.0009(18) -0.0005(17) C11 0.023(2) 0.013(2) 0.012(2) -0.0051(17) 0.0015(17) 0.0035(18) C12 0.017(2) 0.014(2) 0.020(2) -0.0013(18) 0.0046(18) 0.0005(18) C13 0.014(2) 0.014(2) 0.018(2) 0.0011(17) 0.0014(17) 0.0009(17) C14 0.013(2) 0.014(2) 0.038(3) -0.007(2) 0.007(2) 0.0040(18) C15 0.014(2) 0.011(2) 0.027(2) -0.0038(18) -0.0009(19) -0.0026(17) C16 0.019(2) 0.023(3) 0.021(2) 0.001(2) 0.0073(19) -0.002(2) C17 0.013(2) 0.019(2) 0.024(2) 0.0021(19) 0.0017(18) -0.0012(18) C18 0.016(2) 0.021(2) 0.030(3) 0.007(2) 0.0071(19) 0.0018(19) C19 0.021(2) 0.022(2) 0.024(2) 0.009(2) 0.0114(19) 0.006(2) C20 0.024(2) 0.015(2) 0.017(2) 0.0045(18) 0.0031(18) 0.0061(19) C21 0.018(2) 0.014(2) 0.017(2) 0.0038(18) 0.0002(17) 0.0026(18) C22 0.017(2) 0.011(2) 0.015(2) 0.0044(17) -0.0019(17) 0.0031(17) C23 0.026(3) 0.017(2) 0.018(2) 0.0014(18) -0.0002(19) 0.0045(19) C24 0.028(3) 0.016(2) 0.025(3) 0.0005(19) -0.009(2) -0.001(2) C25 0.015(2) 0.019(2) 0.027(3) 0.005(2) -0.0078(19) -0.0009(18) C26 0.013(2) 0.018(2) 0.022(2) 0.0039(19) 0.0009(18) -0.0008(18) C27 0.047(3) 0.026(3) 0.048(3) -0.003(3) 0.024(3) 0.008(3) C28A 0.076(5) 0.033(2) 0.035(7) -0.005(4) 0.039(3) -0.010(3) C28B 0.076(5) 0.033(2) 0.035(7) -0.005(4) 0.039(3) -0.010(3) C29A 0.076(5) 0.033(2) 0.035(7) -0.005(4) 0.039(3) -0.010(3) C29B 0.076(5) 0.033(2) 0.035(7) -0.005(4) 0.039(3) -0.010(3) C30A 0.076(5) 0.033(2) 0.035(7) -0.005(4) 0.039(3) -0.010(3) C30B 0.076(5) 0.033(2) 0.035(7) -0.005(4) 0.039(3) -0.010(3) C31A 0.025(3) 0.023(3) 0.017(3) 0.009(2) -0.001(2) -0.001(2) C31B 0.044(4) 0.032(3) 0.032(4) 0.006(3) 0.006(3) -0.001(3) C32A 0.025(3) 0.023(3) 0.017(3) 0.009(2) -0.001(2) -0.001(2) C32B 0.044(4) 0.032(3) 0.032(4) 0.006(3) 0.006(3) -0.001(3) C33A 0.025(3) 0.023(3) 0.017(3) 0.009(2) -0.001(2) -0.001(2) C33B 0.044(4) 0.032(3) 0.032(4) 0.006(3) 0.006(3) -0.001(3) C34A 0.025(3) 0.023(3) 0.017(3) 0.009(2) -0.001(2) -0.001(2) C34B 0.044(4) 0.032(3) 0.032(4) 0.006(3) 0.006(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C3 1.895(5) . ? Re1 C1 1.906(5) . ? Re1 C2 1.911(5) . ? Re1 N2 2.131(4) . ? Re1 N1 2.136(3) . ? Re1 Re2 3.1348(3) . ? Re2 C16 1.900(5) . ? Re2 C15 1.901(4) . ? Re2 C14 1.907(5) . ? Re2 N4 2.129(3) . ? Re2 N3 2.131(3) . ? K1 O8 2.622(4) . ? K1 O4 2.758(3) . ? K1 O7 2.771(3) 3_455 ? K1 O7 2.876(3) . ? K1 O1 2.912(3) . ? K1 O2 2.924(3) 3 ? K1 O5 2.932(3) 1_455 ? K1 C30A 3.346(17) 3_455 ? K1 C34B 3.515(13) . ? K1 C27 3.539(6) . ? K1 K1 3.7553(19) 3_455 ? O1 C1 1.159(5) . ? O2 C2 1.161(5) . ? O2 K1 2.924(3) 3 ? O3 C3 1.161(6) . ? O4 C14 1.155(5) . ? O5 C15 1.172(5) . ? O5 K1 2.932(3) 1_655 ? O6 C16 1.159(6) . ? O7 C30A 1.41(2) . ? O7 C27 1.424(6) . ? O7 C30B 1.471(19) . ? O7 K1 2.771(3) 3_455 ? O8 C31A 1.342(10) . ? O8 C34A 1.391(13) . ? O8 C34B 1.479(14) . ? O8 C31B 1.549(13) . ? N1 C13 1.360(5) . ? N1 C9 1.385(5) . ? N2 C4 1.357(6) . ? N2 C8 1.379(5) . ? N3 C17 1.363(5) . ? N3 C21 1.377(5) . ? N4 C26 1.362(5) . ? N4 C22 1.378(5) . ? C4 C5 1.362(7) . ? C4 H4 0.9500 . ? C5 C6 1.397(7) . ? C5 H5 0.9500 . ? C6 C7 1.365(6) . ? C6 H6 0.9500 . ? C7 C8 1.402(6) . ? C7 H7 0.9500 . ? C8 C9 1.425(6) . ? C9 C10 1.405(6) . ? C10 C11 1.362(6) . ? C10 H10 0.9500 . ? C11 C12 1.397(6) . ? C11 H11 0.9500 . ? C12 C13 1.367(6) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C17 C18 1.363(6) . ? C17 H17 0.9500 . ? C18 C19 1.396(7) . ? C18 H18 0.9500 . ? C19 C20 1.361(6) . ? C19 H19 0.9500 . ? C20 C21 1.410(6) . ? C20 H20 0.9500 . ? C21 C22 1.427(6) . ? C22 C23 1.409(6) . ? C23 C24 1.357(7) . ? C23 H23 0.9500 . ? C24 C25 1.407(7) . ? C24 H24 0.9500 . ? C25 C26 1.352(6) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28A 1.338(16) . ? C27 C28B 1.574(14) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28A C29A 1.792(19) . ? C28A H28A 0.9900 . ? C28A H28B 0.9900 . ? C28B C29B 1.10(2) . ? C28B H28C 0.9900 . ? C28B H28D 0.9900 . ? C29A C30A 1.58(3) . ? C29A H29A 0.9900 . ? C29A H29B 0.9900 . ? C29B C30B 1.63(3) . ? C29B H29C 0.9900 . ? C29B H29D 0.9900 . ? C30A K1 3.346(17) 3_455 ? C30A H30A 0.9900 . ? C30A H30B 0.9900 . ? C30B H30C 0.9900 . ? C30B H30D 0.9900 . ? C31A C32A 1.547(10) . ? C31A H31A 0.9900 . ? C31A H31B 0.9900 . ? C31B C32B 1.501(18) . ? C31B H31C 0.9900 . ? C31B H31D 0.9900 . ? C32A C33A 1.523(13) . ? C32A H32A 0.9900 . ? C32A H32B 0.9900 . ? C32B C33B 1.450(18) . ? C32B H32C 0.9900 . ? C32B H32D 0.9900 . ? C33A C34A 1.501(13) . ? C33A H33A 0.9900 . ? C33A H33B 0.9900 . ? C33B C34B 1.468(17) . ? C33B H33C 0.9900 . ? C33B H33D 0.9900 . ? C34A H34A 0.9900 . ? C34A H34B 0.9900 . ? C34B H34C 0.9900 . ? C34B H34D 0.9900 . ? 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 C3 Re1 C1 92.57(19) . . ? C3 Re1 C2 92.49(19) . . ? C1 Re1 C2 88.60(18) . . ? C3 Re1 N2 97.25(18) . . ? C1 Re1 N2 168.20(16) . . ? C2 Re1 N2 97.46(16) . . ? C3 Re1 N1 94.07(16) . . ? C1 Re1 N1 97.90(15) . . ? C2 Re1 N1 170.54(16) . . ? N2 Re1 N1 74.96(13) . . ? C3 Re1 Re2 172.85(14) . . ? C1 Re1 Re2 82.06(13) . . ? C2 Re1 Re2 82.70(14) . . ? N2 Re1 Re2 88.64(9) . . ? N1 Re1 Re2 91.36(9) . . ? C16 Re2 C15 91.03(18) . . ? C16 Re2 C14 92.71(19) . . ? C15 Re2 C14 86.82(18) . . ? C16 Re2 N4 97.07(17) . . ? C15 Re2 N4 98.70(16) . . ? C14 Re2 N4 168.65(16) . . ? C16 Re2 N3 95.89(16) . . ? C15 Re2 N3 171.27(16) . . ? C14 Re2 N3 98.13(16) . . ? N4 Re2 N3 75.20(13) . . ? C16 Re2 Re1 174.99(14) . . ? C15 Re2 Re1 86.27(13) . . ? C14 Re2 Re1 82.94(14) . . ? N4 Re2 Re1 87.51(9) . . ? N3 Re2 Re1 87.21(9) . . ? O8 K1 O4 70.69(12) . . ? O8 K1 O7 165.41(11) . 3_455 ? O4 K1 O7 117.73(11) . 3_455 ? O8 K1 O7 77.72(11) . . ? O4 K1 O7 144.58(11) . . ? O7 K1 O7 96.65(9) 3_455 . ? O8 K1 O1 93.64(12) . . ? O4 K1 O1 66.61(9) . . ? O7 K1 O1 80.13(10) 3_455 . ? O7 K1 O1 132.36(9) . . ? O8 K1 O2 84.18(11) . 3 ? O4 K1 O2 70.56(10) . 3 ? O7 K1 O2 109.56(10) 3_455 3 ? O7 K1 O2 91.02(9) . 3 ? O1 K1 O2 135.18(10) . 3 ? O8 K1 O5 91.68(10) . 1_455 ? O4 K1 O5 127.26(10) . 1_455 ? O7 K1 O5 73.74(9) 3_455 1_455 ? O7 K1 O5 68.06(9) . 1_455 ? O1 K1 O5 65.45(9) . 1_455 ? O2 K1 O5 159.06(10) 3 1_455 ? O8 K1 C30A 167.5(3) . 3_455 ? O4 K1 C30A 96.8(3) . 3_455 ? O7 K1 C30A 24.4(4) 3_455 3_455 ? O7 K1 C30A 114.2(3) . 3_455 ? O1 K1 C30A 81.0(3) . 3_455 ? O2 K1 C30A 91.6(3) 3 3_455 ? O5 K1 C30A 96.3(4) 1_455 3_455 ? O8 K1 C34B 22.4(2) . . ? O4 K1 C34B 65.1(2) . . ? O7 K1 C34B 170.2(2) 3_455 . ? O7 K1 C34B 79.6(2) . . ? O1 K1 C34B 109.1(2) . . ? O2 K1 C34B 61.8(2) 3 . ? O5 K1 C34B 112.6(2) 1_455 . ? C30A K1 C34B 151.1(4) 3_455 . ? O8 K1 C27 72.50(14) . . ? O4 K1 C27 126.72(12) . . ? O7 K1 C27 107.30(12) 3_455 . ? O7 K1 C27 22.77(10) . . ? O1 K1 C27 152.33(11) . . ? O2 K1 C27 68.60(11) 3 . ? O5 K1 C27 90.56(11) 1_455 . ? C30A K1 C27 116.9(3) 3_455 . ? C34B K1 C27 66.1(2) . . ? O8 K1 K1 123.45(10) . 3_455 ? O4 K1 K1 165.35(10) . 3_455 ? O7 K1 K1 49.53(7) 3_455 3_455 ? O7 K1 K1 47.13(7) . 3_455 ? O1 K1 K1 112.93(7) . 3_455 ? O2 K1 K1 105.11(8) 3 3_455 ? O5 K1 K1 60.48(7) 1_455 3_455 ? C30A K1 K1 69.1(3) 3_455 3_455 ? C34B K1 K1 126.1(2) . 3_455 ? C27 K1 K1 60.87(10) . 3_455 ? C1 O1 K1 129.3(3) . . ? C2 O2 K1 154.5(3) . 3 ? C14 O4 K1 139.8(3) . . ? C15 O5 K1 149.7(3) . 1_655 ? C30A O7 C27 107.0(8) . . ? C30A O7 C30B 20.6(10) . . ? C27 O7 C30B 107.9(8) . . ? C30A O7 K1 101.3(7) . 3_455 ? C27 O7 K1 120.3(3) . 3_455 ? C30B O7 K1 115.9(8) . 3_455 ? C30A O7 K1 138.3(7) . . ? C27 O7 K1 105.8(3) . . ? C30B O7 K1 122.1(7) . . ? K1 O7 K1 83.35(9) 3_455 . ? C31A O8 C34A 112.3(7) . . ? C31A O8 C34B 117.5(7) . . ? C34A O8 C34B 21.9(6) . . ? C31A O8 C31B 26.4(5) . . ? C34A O8 C31B 87.5(7) . . ? C34B O8 C31B 97.6(7) . . ? C31A O8 K1 124.6(5) . . ? C34A O8 K1 123.0(5) . . ? C34B O8 K1 115.1(5) . . ? C31B O8 K1 147.3(5) . . ? C13 N1 C9 117.2(3) . . ? C13 N1 Re1 125.6(3) . . ? C9 N1 Re1 116.9(3) . . ? C4 N2 C8 117.4(4) . . ? C4 N2 Re1 125.1(3) . . ? C8 N2 Re1 117.5(3) . . ? C17 N3 C21 117.4(4) . . ? C17 N3 Re2 125.3(3) . . ? C21 N3 Re2 117.2(3) . . ? C26 N4 C22 117.7(4) . . ? C26 N4 Re2 125.0(3) . . ? C22 N4 Re2 117.1(3) . . ? O1 C1 Re1 179.3(4) . . ? O2 C2 Re1 178.2(4) . . ? O3 C3 Re1 176.8(4) . . ? N2 C4 C5 123.8(4) . . ? N2 C4 H4 118.1 . . ? C5 C4 H4 118.1 . . ? C4 C5 C6 118.9(4) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C7 C6 C5 118.9(4) . . ? C7 C6 H6 120.6 . . ? C5 C6 H6 120.6 . . ? C6 C7 C8 120.5(4) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? N2 C8 C7 120.5(4) . . ? N2 C8 C9 115.1(4) . . ? C7 C8 C9 124.4(4) . . ? N1 C9 C10 120.5(4) . . ? N1 C9 C8 115.0(4) . . ? C10 C9 C8 124.5(4) . . ? C11 C10 C9 120.8(4) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 118.6(4) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? C13 C12 C11 119.3(4) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? N1 C13 C12 123.6(4) . . ? N1 C13 H13 118.2 . . ? C12 C13 H13 118.2 . . ? O4 C14 Re2 177.7(4) . . ? O5 C15 Re2 177.4(4) . . ? O6 C16 Re2 175.2(4) . . ? C18 C17 N3 123.4(4) . . ? C18 C17 H17 118.3 . . ? N3 C17 H17 118.3 . . ? C17 C18 C19 119.2(4) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C20 C19 C18 119.1(4) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C19 C20 C21 120.1(4) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? N3 C21 C20 120.7(4) . . ? N3 C21 C22 115.1(4) . . ? C20 C21 C22 124.2(4) . . ? N4 C22 C23 120.1(4) . . ? N4 C22 C21 115.3(4) . . ? C23 C22 C21 124.6(4) . . ? C24 C23 C22 120.4(4) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 119.2(4) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C26 C25 C24 118.7(4) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C25 C26 N4 123.8(4) . . ? C25 C26 H26 118.1 . . ? N4 C26 H26 118.1 . . ? C28A C27 O7 114.5(7) . . ? C28A C27 C28B 16.3(9) . . ? O7 C27 C28B 102.2(6) . . ? C28A C27 K1 159.5(6) . . ? O7 C27 K1 51.4(2) . . ? C28B C27 K1 143.2(6) . . ? C28A C27 H27A 113.4 . . ? O7 C27 H27A 111.3 . . ? C28B C27 H27A 111.3 . . ? K1 C27 H27A 67.1 . . ? C28A C27 H27B 96.1 . . ? O7 C27 H27B 111.3 . . ? C28B C27 H27B 111.3 . . ? K1 C27 H27B 103.0 . . ? H27A C27 H27B 109.2 . . ? C27 C28A C29A 99.0(11) . . ? C27 C28A H28A 112.0 . . ? C29A C28A H28A 112.0 . . ? C27 C28A H28B 112.0 . . ? C29A C28A H28B 112.0 . . ? H28A C28A H28B 109.6 . . ? C29B C28B C27 112.3(16) . . ? C29B C28B H28C 109.1 . . ? C27 C28B H28C 109.1 . . ? C29B C28B H28D 109.1 . . ? C27 C28B H28D 109.1 . . ? H28C C28B H28D 107.9 . . ? C30A C29A C28A 90.5(12) . . ? C30A C29A H29A 113.6 . . ? C28A C29A H29A 113.6 . . ? C30A C29A H29B 113.6 . . ? C28A C29A H29B 113.6 . . ? H29A C29A H29B 110.8 . . ? C28B C29B C30B 110.3(17) . . ? C28B C29B H29C 109.6 . . ? C30B C29B H29C 109.6 . . ? C28B C29B H29D 109.6 . . ? C30B C29B H29D 109.6 . . ? H29C C29B H29D 108.1 . . ? O7 C30A C29A 107.8(16) . . ? O7 C30A K1 54.3(6) . 3_455 ? C29A C30A K1 149.7(12) . 3_455 ? O7 C30A H30A 110.1 . . ? C29A C30A H30A 110.1 . . ? K1 C30A H30A 63.6 3_455 . ? O7 C30A H30B 110.1 . . ? C29A C30A H30B 110.1 . . ? K1 C30A H30B 99.6 3_455 . ? H30A C30A H30B 108.5 . . ? O7 C30B C29B 96.9(12) . . ? O7 C30B H30C 112.4 . . ? C29B C30B H30C 112.4 . . ? O7 C30B H30D 112.4 . . ? C29B C30B H30D 112.4 . . ? H30C C30B H30D 109.9 . . ? O8 C31A C32A 105.6(7) . . ? O8 C31A H31A 110.6 . . ? C32A C31A H31A 110.6 . . ? O8 C31A H31B 110.6 . . ? C32A C31A H31B 110.6 . . ? H31A C31A H31B 108.8 . . ? C32B C31B O8 103.1(9) . . ? C32B C31B H31C 111.1 . . ? O8 C31B H31C 111.1 . . ? C32B C31B H31D 111.1 . . ? O8 C31B H31D 111.1 . . ? H31C C31B H31D 109.1 . . ? C33A C32A C31A 104.1(8) . . ? C33A C32A H32A 110.9 . . ? C31A C32A H32A 110.9 . . ? C33A C32A H32B 110.9 . . ? C31A C32A H32B 110.9 . . ? H32A C32A H32B 109.0 . . ? C33B C32B C31B 105.0(10) . . ? C33B C32B H32C 110.8 . . ? C31B C32B H32C 110.8 . . ? C33B C32B H32D 110.8 . . ? C31B C32B H32D 110.8 . . ? H32C C32B H32D 108.8 . . ? C34A C33A C32A 102.2(8) . . ? C34A C33A H33A 111.3 . . ? C32A C33A H33A 111.3 . . ? C34A C33A H33B 111.3 . . ? C32A C33A H33B 111.3 . . ? H33A C33A H33B 109.2 . . ? C32B C33B C34B 107.4(11) . . ? C32B C33B H33C 110.2 . . ? C34B C33B H33C 110.2 . . ? C32B C33B H33D 110.2 . . ? C34B C33B H33D 110.2 . . ? H33C C33B H33D 108.5 . . ? O8 C34A C33A 104.4(9) . . ? O8 C34A H34A 110.9 . . ? C33A C34A H34A 110.9 . . ? O8 C34A H34B 110.9 . . ? C33A C34A H34B 110.9 . . ? H34A C34A H34B 108.9 . . ? C33B C34B O8 105.6(10) . . ? C33B C34B K1 132.4(8) . . ? O8 C34B K1 42.5(4) . . ? C33B C34B H34C 110.6 . . ? O8 C34B H34C 110.6 . . ? K1 C34B H34C 113.8 . . ? C33B C34B H34D 110.6 . . ? O8 C34B H34D 110.6 . . ? K1 C34B H34D 69.9 . . ? H34C C34B H34D 108.7 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.639 _refine_diff_density_min -0.791 _refine_diff_density_rms 0.147 data_[Re(bpy)(CO)3][K(18-crown-6)(THF)] _database_code_depnum_ccdc_archive 'CCDC 876410' #TrackingRef '- Bensons_Xtals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H40 K N2 O10 Re' _chemical_formula_weight 801.94 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 23.3023(13) _cell_length_b 18.0705(9) _cell_length_c 16.0034(8) _cell_angle_alpha 90.00 _cell_angle_beta 73.240(3) _cell_angle_gamma 90.00 _cell_volume 6452.5(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9894 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 25.51 _exptl_crystal_description plate _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.651 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3216 _exptl_absorpt_coefficient_mu 3.952 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5054 _exptl_absorpt_correction_T_max 0.6933 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 44779 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.56 _reflns_number_total 11977 _reflns_number_gt 8870 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0131P)^2^+15.2106P] 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 11977 _refine_ls_number_parameters 798 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0537 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0636 _refine_ls_wR_factor_gt 0.0578 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.027 _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 0.529238(8) 0.972710(9) 0.244532(13) 0.02222(5) Uani 1 1 d . A . Re2 Re 0.973008(8) 0.465442(9) 0.255980(12) 0.02195(5) Uani 1 1 d . . . K1 K 0.71472(5) 1.13356(6) 0.25154(8) 0.0361(3) Uani 1 1 d . . . K2 K 0.77968(4) 0.60224(6) 0.25807(7) 0.0311(2) Uani 1 1 d . . . O3 O 0.65461(18) 1.0022(2) 0.2571(4) 0.0784(17) Uani 1 1 d . A . O1 O 0.57659(16) 0.85374(18) 0.1036(2) 0.0382(9) Uani 1 1 d . A . O2 O 0.5086(2) 0.84320(19) 0.3730(2) 0.0650(14) Uani 1 1 d . A . O4 O 0.78185(16) 1.0910(2) 0.0823(3) 0.0557(11) Uani 1 1 d . A . O5 O 0.82605(15) 1.06803(19) 0.2263(3) 0.0523(11) Uani 1 1 d . A . O6 O 0.74581(17) 1.0771(2) 0.3961(3) 0.0487(10) Uani 1 1 d . A . O7 O 0.64497(17) 1.1737(2) 0.4191(2) 0.0455(9) Uani 1 1 d . A . O8 O 0.60789(14) 1.20315(17) 0.2714(2) 0.0374(9) Uani 1 1 d . A . O9 O 0.68535(15) 1.18852(19) 0.1016(2) 0.0407(9) Uani 1 1 d . A . O30A O 0.7689(2) 1.2594(3) 0.2950(3) 0.0411(12) Uani 0.734(6) 1 d P A 1 O30B O 0.7383(6) 1.2957(8) 0.2292(11) 0.0411(12) Uani 0.266(6) 1 d P A 2 O31 O 0.84687(16) 0.47323(19) 0.2378(3) 0.0560(12) Uani 1 1 d . . . O32 O 0.93392(18) 0.34679(18) 0.3994(2) 0.0458(10) Uani 1 1 d . . . O33 O 1.01154(16) 0.34186(17) 0.1201(2) 0.0409(9) Uani 1 1 d . . . O34 O 0.80699(14) 0.66227(19) 0.4076(2) 0.0353(8) Uani 1 1 d . . . O35 O 0.71840(14) 0.55121(19) 0.4262(2) 0.0375(8) Uani 1 1 d . . . O36 O 0.67253(14) 0.53176(17) 0.2865(2) 0.0356(8) Uani 1 1 d . . . O37 O 0.74642(14) 0.54842(19) 0.1121(2) 0.0359(8) Uani 1 1 d . . . O38 O 0.84089(14) 0.65417(18) 0.0897(2) 0.0369(8) Uani 1 1 d . . . O39 O 0.87975(15) 0.68942(18) 0.2358(2) 0.0367(8) Uani 1 1 d . . . O10 O 0.7137(2) 0.7263(2) 0.2577(3) 0.0735(15) Uani 1 1 d . B . N1 N 0.50485(15) 1.05346(18) 0.1692(2) 0.0206(8) Uani 1 1 d . . . N2 N 0.47740(16) 1.0476(2) 0.3341(2) 0.0251(9) Uani 1 1 d . . . N3 N 0.98892(15) 0.54969(18) 0.3350(2) 0.0207(8) Uani 1 1 d . . . N4 N 1.01880(15) 0.54622(18) 0.1692(2) 0.0201(8) Uani 1 1 d . . . C3 C 0.6065(3) 0.9905(3) 0.2521(4) 0.0443(15) Uani 1 1 d . . . C1 C 0.5588(2) 0.9000(3) 0.1555(3) 0.0288(11) Uani 1 1 d . . . C2 C 0.5175(3) 0.8926(3) 0.3240(3) 0.0377(13) Uani 1 1 d . . . C4 C 0.4608(2) 1.0393(3) 0.4238(3) 0.0357(12) Uani 1 1 d . . . H4 H 0.4709 0.9943 0.4468 0.043 Uiso 1 1 calc R . . C5 C 0.4312(2) 1.0910(3) 0.4806(3) 0.0421(14) Uani 1 1 d . . . H5 H 0.4203 1.0820 0.5416 0.051 Uiso 1 1 calc R . . C6 C 0.4165(2) 1.1590(3) 0.4480(3) 0.0390(13) Uani 1 1 d . . . H6 H 0.3969 1.1969 0.4869 0.047 Uiso 1 1 calc R . . C7 C 0.4308(2) 1.1693(3) 0.3608(3) 0.0333(12) Uani 1 1 d . . . H7 H 0.4213 1.2150 0.3386 0.040 Uiso 1 1 calc R . . C8 C 0.46003(19) 1.1128(2) 0.3016(3) 0.0240(11) Uani 1 1 d . . . C9 C 0.47418(18) 1.1157(2) 0.2111(3) 0.0226(10) Uani 1 1 d . . . C30 C 0.4599(2) 1.1745(2) 0.1629(3) 0.0270(11) Uani 1 1 d . . . H10 H 0.4388 1.2162 0.1928 0.032 Uiso 1 1 calc R . . C31 C 0.4757(2) 1.1727(2) 0.0745(3) 0.0294(11) Uani 1 1 d . . . H11 H 0.4664 1.2128 0.0423 0.035 Uiso 1 1 calc R . . C32 C 0.5064(2) 1.1097(2) 0.0313(3) 0.0259(11) Uani 1 1 d . . . H12 H 0.5177 1.1067 -0.0306 0.031 Uiso 1 1 calc R . . C33 C 0.51949(19) 1.0538(2) 0.0789(3) 0.0220(10) Uani 1 1 d . . . H13 H 0.5401 1.0121 0.0485 0.026 Uiso 1 1 calc R . . C34 C 0.8436(2) 1.0778(3) 0.0729(5) 0.0623(19) Uani 1 1 d . . . H14A H 0.8643 1.1254 0.0738 0.075 Uiso 1 1 calc R A . H14B H 0.8623 1.0535 0.0161 0.075 Uiso 1 1 calc R . . C35 C 0.8501(3) 1.0302(3) 0.1442(5) 0.067(2) Uani 1 1 d . A . H15A H 0.8285 0.9830 0.1445 0.080 Uiso 1 1 calc R . . H15B H 0.8930 1.0187 0.1355 0.080 Uiso 1 1 calc R . . C36 C 0.8340(3) 1.0273(3) 0.2973(6) 0.067(2) Uani 1 1 d . . . H16A H 0.8771 1.0174 0.2883 0.080 Uiso 1 1 calc R A . H16B H 0.8128 0.9792 0.3020 0.080 Uiso 1 1 calc R . . C37 C 0.8096(3) 1.0706(3) 0.3779(5) 0.060(2) Uani 1 1 d . A . H17A H 0.8193 1.0457 0.4272 0.072 Uiso 1 1 calc R . . H17B H 0.8280 1.1204 0.3709 0.072 Uiso 1 1 calc R . . C38 C 0.7186(3) 1.1162(3) 0.4735(4) 0.0600(18) Uani 1 1 d . . . H18A H 0.7365 1.1661 0.4709 0.072 Uiso 1 1 calc R A . H18B H 0.7249 1.0896 0.5241 0.072 Uiso 1 1 calc R . . C39 C 0.6534(3) 1.1225(3) 0.4833(4) 0.0575(17) Uani 1 1 d . A . H19A H 0.6369 1.0734 0.4748 0.069 Uiso 1 1 calc R . . H19B H 0.6320 1.1403 0.5426 0.069 Uiso 1 1 calc R . . C10 C 0.5835(3) 1.1818(3) 0.4222(4) 0.0540(16) Uani 1 1 d . . . H20A H 0.5600 1.1999 0.4804 0.065 Uiso 1 1 calc R A . H20B H 0.5668 1.1335 0.4115 0.065 Uiso 1 1 calc R . . C11 C 0.5797(2) 1.2357(3) 0.3541(4) 0.0468(15) Uani 1 1 d . A . H21A H 0.5372 1.2470 0.3592 0.056 Uiso 1 1 calc R . . H21B H 0.6002 1.2823 0.3608 0.056 Uiso 1 1 calc R . . C12 C 0.5995(2) 1.2442(3) 0.2001(4) 0.0424(14) Uani 1 1 d . . . H22A H 0.6218 1.2915 0.1937 0.051 Uiso 1 1 calc R A . H22B H 0.5565 1.2553 0.2100 0.051 Uiso 1 1 calc R . . C13 C 0.6224(2) 1.1981(3) 0.1203(4) 0.0471(15) Uani 1 1 d . A . H23A H 0.6024 1.1493 0.1294 0.056 Uiso 1 1 calc R . . H23B H 0.6132 1.2225 0.0704 0.056 Uiso 1 1 calc R . . C14 C 0.7075(3) 1.1428(4) 0.0274(4) 0.0640(18) Uani 1 1 d . . . H24A H 0.6996 1.1660 -0.0242 0.077 Uiso 1 1 calc R A . H24B H 0.6871 1.0942 0.0373 0.077 Uiso 1 1 calc R . . C15 C 0.7734(3) 1.1325(4) 0.0115(5) 0.0682(19) Uani 1 1 d . A . H25A H 0.7906 1.1057 -0.0441 0.082 Uiso 1 1 calc R . . H25B H 0.7935 1.1811 0.0077 0.082 Uiso 1 1 calc R . . C16A C 0.7479(3) 1.3257(5) 0.2625(6) 0.0411(12) Uani 0.734(6) 1 d P A 1 H26A H 0.7566 1.3703 0.2926 0.049 Uiso 0.734(6) 1 calc PR A 1 H26B H 0.7043 1.3231 0.2697 0.049 Uiso 0.734(6) 1 calc PR A 1 C16B C 0.7581(9) 1.3115(15) 0.3021(16) 0.0411(12) Uani 0.266(6) 1 d P A 2 H26C H 0.7328 1.2879 0.3560 0.049 Uiso 0.266(6) 1 calc PR A 2 H26D H 0.7611 1.3653 0.3115 0.049 Uiso 0.266(6) 1 calc PR A 2 C17 C 0.7843(3) 1.3258(4) 0.1644(4) 0.0492(16) Uani 1 1 d . . . H27A H 0.7649 1.2951 0.1290 0.059 Uiso 0.734(6) 1 calc PR A 1 H27B H 0.7903 1.3766 0.1402 0.059 Uiso 0.734(6) 1 calc PR A 1 H27C H 0.796(10) 1.370(12) 0.146(15) 0.059 Uiso 0.266(6) 1 d P A 2 H27D H 0.797(10) 1.266(12) 0.156(13) 0.059 Uiso 0.266(6) 1 d P A 2 C18 C 0.8431(2) 1.2917(3) 0.1698(3) 0.0403(13) Uani 1 1 d . A . H28A H 0.8543 1.2485 0.1303 0.048 Uiso 1 1 calc R . . H28B H 0.8760 1.3284 0.1544 0.048 Uiso 1 1 calc R . . C19 C 0.8300(2) 1.2685(4) 0.2628(4) 0.0545(17) Uani 1 1 d . . . H29A H 0.8508 1.2215 0.2671 0.065 Uiso 0.734(6) 1 calc PR A 1 H29B H 0.8440 1.3068 0.2967 0.065 Uiso 0.734(6) 1 calc PR A 1 H29C H 0.852(10) 1.307(11) 0.302(14) 0.065 Uiso 0.266(6) 1 d P A 2 H29D H 0.831(9) 1.205(11) 0.297(14) 0.065 Uiso 0.266(6) 1 d P A 2 C20 C 0.8956(2) 0.4704(2) 0.2451(3) 0.0322(12) Uani 1 1 d . . . C21 C 0.9487(2) 0.3919(3) 0.3456(3) 0.0320(12) Uani 1 1 d . . . C22 C 0.9954(2) 0.3878(2) 0.1732(3) 0.0278(11) Uani 1 1 d . . . C23 C 1.03596(19) 0.5403(2) 0.0791(3) 0.0264(11) Uani 1 1 d . . . H33 H 1.0290 0.4946 0.0543 0.032 Uiso 1 1 calc R . . C24 C 1.0618(2) 0.5953(3) 0.0247(3) 0.0284(11) Uani 1 1 d . . . H34 H 1.0734 0.5876 -0.0367 0.034 Uiso 1 1 calc R . . C25 C 1.0717(2) 0.6649(2) 0.0595(3) 0.0280(11) Uani 1 1 d . . . H35 H 1.0889 0.7049 0.0222 0.034 Uiso 1 1 calc R . . C26 C 1.05572(18) 0.6726(2) 0.1473(3) 0.0230(10) Uani 1 1 d . . . H36 H 1.0618 0.7188 0.1719 0.028 Uiso 1 1 calc R . . C27 C 1.03039(19) 0.6135(2) 0.2029(3) 0.0224(10) Uani 1 1 d . . . C28 C 1.01462(19) 0.6146(2) 0.2950(3) 0.0228(10) Uani 1 1 d . . . C29 C 1.02367(19) 0.6756(2) 0.3458(3) 0.0243(10) Uani 1 1 d . . . H39 H 1.0414 0.7197 0.3173 0.029 Uiso 1 1 calc R . . C40 C 1.0075(2) 0.6721(2) 0.4337(3) 0.0262(11) Uani 1 1 d . . . H40 H 1.0137 0.7130 0.4674 0.031 Uiso 1 1 calc R . . C41 C 0.9808(2) 0.6057(2) 0.4748(3) 0.0278(11) Uani 1 1 d . . . H41 H 0.9686 0.6017 0.5367 0.033 Uiso 1 1 calc R . . C42 C 0.97299(19) 0.5486(2) 0.4255(3) 0.0249(10) Uani 1 1 d . . . H42 H 0.9554 0.5047 0.4545 0.030 Uiso 1 1 calc R . . C43 C 0.7944(2) 0.6088(3) 0.4746(3) 0.0439(14) Uani 1 1 d . . . H43A H 0.8041 0.6289 0.5264 0.053 Uiso 1 1 calc R . . H43B H 0.8193 0.5643 0.4547 0.053 Uiso 1 1 calc R . . C44 C 0.7295(2) 0.5886(3) 0.4981(3) 0.0456(14) Uani 1 1 d . . . H44A H 0.7191 0.5562 0.5502 0.055 Uiso 1 1 calc R . . H44B H 0.7045 0.6338 0.5120 0.055 Uiso 1 1 calc R . . C45 C 0.6561(2) 0.5422(3) 0.4387(3) 0.0373(12) Uani 1 1 d . . . H45A H 0.6370 0.5911 0.4384 0.045 Uiso 1 1 calc R . . H45B H 0.6374 0.5184 0.4958 0.045 Uiso 1 1 calc R . . C46 C 0.6464(2) 0.4949(3) 0.3667(3) 0.0385(13) Uani 1 1 d . . . H46A H 0.6654 0.4459 0.3666 0.046 Uiso 1 1 calc R . . H46B H 0.6030 0.4875 0.3753 0.046 Uiso 1 1 calc R . . C47 C 0.6601(2) 0.4972(3) 0.2145(4) 0.0392(13) Uani 1 1 d . . . H47A H 0.6164 0.4894 0.2269 0.047 Uiso 1 1 calc R . . H47B H 0.6802 0.4484 0.2035 0.047 Uiso 1 1 calc R . . C48 C 0.6820(2) 0.5450(3) 0.1372(4) 0.0417(13) Uani 1 1 d . . . H48A H 0.6686 0.5250 0.0884 0.050 Uiso 1 1 calc R . . H48B H 0.6652 0.5954 0.1506 0.050 Uiso 1 1 calc R . . C49 C 0.7693(2) 0.5921(3) 0.0369(3) 0.0423(13) Uani 1 1 d . . . H49A H 0.7478 0.6399 0.0437 0.051 Uiso 1 1 calc R . . H49B H 0.7633 0.5664 -0.0146 0.051 Uiso 1 1 calc R . . C50 C 0.8345(2) 0.6052(3) 0.0239(3) 0.0437(14) Uani 1 1 d . . . H50A H 0.8549 0.5578 0.0275 0.052 Uiso 1 1 calc R . . H50B H 0.8529 0.6270 -0.0345 0.052 Uiso 1 1 calc R . . C51 C 0.9015(2) 0.6708(3) 0.0848(4) 0.0428(14) Uani 1 1 d . . . H51A H 0.9220 0.6921 0.0269 0.051 Uiso 1 1 calc R . . H51B H 0.9227 0.6249 0.0921 0.051 Uiso 1 1 calc R . . C52 C 0.9027(2) 0.7242(3) 0.1542(4) 0.0414(13) Uani 1 1 d . . . H52A H 0.9443 0.7408 0.1470 0.050 Uiso 1 1 calc R . . H52B H 0.8781 0.7681 0.1505 0.050 Uiso 1 1 calc R . . C53 C 0.8817(2) 0.7344(3) 0.3075(4) 0.0416(13) Uani 1 1 d . . . H53A H 0.8523 0.7752 0.3149 0.050 Uiso 1 1 calc R . . H53B H 0.9221 0.7563 0.2969 0.050 Uiso 1 1 calc R . . C54 C 0.8673(2) 0.6881(3) 0.3869(4) 0.0398(13) Uani 1 1 d . . . H54A H 0.8950 0.6453 0.3774 0.048 Uiso 1 1 calc R . . H54B H 0.8728 0.7174 0.4363 0.048 Uiso 1 1 calc R . . C55 C 0.7203(3) 0.7789(3) 0.1933(4) 0.0508(15) Uani 1 1 d . B . H55A H 0.6821 0.7862 0.1789 0.061 Uiso 1 1 calc R . . H55B H 0.7515 0.7636 0.1398 0.061 Uiso 1 1 calc R . . C56 C 0.7382(4) 0.8477(3) 0.2293(4) 0.084(3) Uani 1 1 d . . . H56C H 0.7193 0.8912 0.2102 0.101 Uiso 0.568(11) 1 calc PR B 2 H56D H 0.7823 0.8539 0.2085 0.101 Uiso 0.568(11) 1 calc PR B 2 H56A H 0.7344 0.8928 0.1962 0.101 Uiso 0.432(11) 1 calc PR B 1 H56B H 0.7784 0.8451 0.2388 0.101 Uiso 0.432(11) 1 calc PR B 1 C57A C 0.7176(6) 0.8414(6) 0.3278(7) 0.045(2) Uani 0.568(11) 1 d P B 2 H57A H 0.6874 0.8796 0.3542 0.054 Uiso 0.568(11) 1 calc PR B 2 H57B H 0.7517 0.8455 0.3528 0.054 Uiso 0.568(11) 1 calc PR B 2 C57B C 0.6811(8) 0.8355(8) 0.3212(10) 0.045(2) Uani 0.432(11) 1 d P B 1 H57C H 0.6842 0.8697 0.3681 0.054 Uiso 0.432(11) 1 calc PR B 1 H57D H 0.6417 0.8422 0.3102 0.054 Uiso 0.432(11) 1 calc PR B 1 C58 C 0.6900(3) 0.7631(4) 0.3412(4) 0.0558(17) Uani 1 1 d . . . H58A H 0.6518 0.7401 0.3750 0.067 Uiso 0.432(11) 1 calc PR B 1 H58B H 0.7189 0.7602 0.3759 0.067 Uiso 0.432(11) 1 calc PR B 1 H58C H 0.691(5) 0.740(6) 0.392(7) 0.067 Uiso 0.568(11) 1 d P B 2 H58D H 0.648(5) 0.796(6) 0.331(7) 0.067 Uiso 0.568(11) 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.02450(10) 0.02083(9) 0.02308(11) 0.00313(8) -0.00965(8) -0.00239(8) Re2 0.02264(10) 0.02169(9) 0.02215(11) -0.00227(8) -0.00747(8) -0.00392(7) K1 0.0239(6) 0.0333(6) 0.0551(8) -0.0095(5) -0.0179(5) 0.0012(4) K2 0.0259(5) 0.0414(6) 0.0251(6) -0.0049(5) -0.0058(4) -0.0023(5) O3 0.048(3) 0.033(2) 0.177(5) -0.004(3) -0.070(3) -0.0012(19) O1 0.051(2) 0.0292(18) 0.030(2) 0.0004(16) -0.0058(17) 0.0091(16) O2 0.143(4) 0.026(2) 0.028(2) 0.0057(17) -0.029(3) -0.013(2) O4 0.029(2) 0.053(2) 0.077(3) -0.018(2) -0.002(2) -0.0005(18) O5 0.027(2) 0.039(2) 0.094(3) 0.001(2) -0.021(2) 0.0018(16) O6 0.048(2) 0.047(2) 0.065(3) 0.001(2) -0.038(2) -0.0123(18) O7 0.049(2) 0.049(2) 0.043(2) -0.0024(18) -0.0198(19) -0.0040(18) O8 0.0272(19) 0.0380(19) 0.047(2) -0.0013(17) -0.0103(17) 0.0021(15) O9 0.036(2) 0.047(2) 0.043(2) -0.0044(18) -0.0172(18) -0.0083(16) O30A 0.024(2) 0.040(3) 0.055(3) 0.004(2) -0.0042(19) -0.0004(18) O30B 0.024(2) 0.040(3) 0.055(3) 0.004(2) -0.0042(19) -0.0004(18) O31 0.026(2) 0.041(2) 0.107(4) -0.010(2) -0.028(2) 0.0024(16) O32 0.082(3) 0.0311(19) 0.028(2) 0.0065(17) -0.022(2) -0.0215(19) O33 0.060(2) 0.0244(17) 0.031(2) -0.0041(16) -0.0008(18) 0.0044(16) O34 0.0228(18) 0.053(2) 0.031(2) -0.0026(17) -0.0097(15) 0.0009(15) O35 0.0218(17) 0.057(2) 0.032(2) -0.0049(17) -0.0064(15) 0.0017(16) O36 0.0290(18) 0.044(2) 0.036(2) -0.0015(16) -0.0121(16) -0.0028(15) O37 0.0303(19) 0.048(2) 0.032(2) -0.0071(17) -0.0119(16) 0.0088(16) O38 0.0292(19) 0.049(2) 0.030(2) -0.0052(17) -0.0031(15) 0.0069(16) O39 0.0309(19) 0.046(2) 0.031(2) 0.0019(17) -0.0067(16) -0.0055(16) O10 0.106(4) 0.035(2) 0.056(3) 0.001(2) 0.016(3) 0.008(2) N1 0.0180(19) 0.0195(18) 0.024(2) 0.0001(16) -0.0050(16) -0.0021(15) N2 0.023(2) 0.029(2) 0.023(2) -0.0023(17) -0.0063(17) -0.0041(16) N3 0.0220(19) 0.0195(17) 0.022(2) -0.0006(16) -0.0080(16) -0.0038(15) N4 0.0209(19) 0.0208(18) 0.020(2) -0.0019(16) -0.0086(16) 0.0026(15) C3 0.048(3) 0.020(2) 0.078(5) 0.000(3) -0.038(3) 0.000(2) C1 0.031(3) 0.026(2) 0.030(3) 0.012(2) -0.011(2) -0.003(2) C2 0.069(4) 0.023(2) 0.024(3) -0.004(2) -0.017(3) -0.006(2) C4 0.043(3) 0.045(3) 0.023(3) -0.001(2) -0.014(2) -0.014(2) C5 0.053(4) 0.050(3) 0.024(3) -0.009(3) -0.012(3) -0.012(3) C6 0.036(3) 0.045(3) 0.032(3) -0.022(3) -0.002(2) -0.010(2) C7 0.029(3) 0.029(3) 0.041(3) -0.013(2) -0.008(2) -0.004(2) C8 0.019(2) 0.023(2) 0.032(3) -0.007(2) -0.011(2) -0.0048(18) C9 0.015(2) 0.018(2) 0.034(3) -0.0060(19) -0.005(2) -0.0027(17) C30 0.027(3) 0.019(2) 0.033(3) -0.002(2) -0.007(2) 0.0026(18) C31 0.031(3) 0.020(2) 0.040(3) 0.008(2) -0.016(2) 0.0010(19) C32 0.029(3) 0.029(2) 0.021(3) 0.007(2) -0.008(2) -0.0043(19) C33 0.023(2) 0.023(2) 0.020(3) -0.0008(19) -0.0049(19) -0.0006(18) C34 0.033(3) 0.052(4) 0.089(5) -0.026(4) 0.002(3) -0.001(3) C35 0.029(3) 0.040(3) 0.127(7) -0.033(4) -0.017(4) 0.010(3) C36 0.038(3) 0.040(3) 0.137(7) 0.018(4) -0.048(4) -0.010(3) C37 0.053(4) 0.045(3) 0.108(6) 0.032(4) -0.064(4) -0.023(3) C38 0.087(5) 0.058(4) 0.054(4) 0.011(3) -0.051(4) -0.026(4) C39 0.083(5) 0.053(4) 0.037(4) -0.006(3) -0.018(3) -0.008(3) C10 0.048(4) 0.064(4) 0.042(4) -0.013(3) 0.000(3) -0.006(3) C11 0.031(3) 0.051(3) 0.059(4) -0.019(3) -0.014(3) 0.007(2) C12 0.036(3) 0.036(3) 0.064(4) 0.001(3) -0.028(3) 0.003(2) C13 0.044(3) 0.049(3) 0.061(4) 0.008(3) -0.036(3) -0.009(3) C14 0.064(4) 0.075(5) 0.055(5) -0.016(4) -0.020(4) -0.004(4) C15 0.065(5) 0.076(5) 0.057(5) -0.011(4) -0.006(4) 0.004(4) C16A 0.024(2) 0.040(3) 0.055(3) 0.004(2) -0.0042(19) -0.0004(18) C16B 0.024(2) 0.040(3) 0.055(3) 0.004(2) -0.0042(19) -0.0004(18) C17 0.048(4) 0.055(4) 0.053(4) 0.016(3) -0.029(3) -0.006(3) C18 0.041(3) 0.040(3) 0.035(3) -0.001(2) -0.004(3) 0.003(2) C19 0.033(3) 0.082(4) 0.056(4) 0.032(3) -0.026(3) -0.018(3) C20 0.030(3) 0.022(2) 0.042(3) -0.004(2) -0.008(2) -0.001(2) C21 0.046(3) 0.028(3) 0.025(3) -0.006(2) -0.016(2) -0.010(2) C22 0.031(3) 0.023(2) 0.029(3) 0.004(2) -0.007(2) -0.002(2) C23 0.023(2) 0.029(2) 0.028(3) -0.001(2) -0.009(2) 0.0026(19) C24 0.023(2) 0.039(3) 0.022(3) 0.001(2) -0.007(2) 0.005(2) C25 0.026(3) 0.032(3) 0.025(3) 0.008(2) -0.006(2) 0.000(2) C26 0.015(2) 0.022(2) 0.033(3) 0.003(2) -0.009(2) -0.0008(17) C27 0.019(2) 0.027(2) 0.021(3) 0.000(2) -0.0059(19) 0.0017(18) C28 0.019(2) 0.025(2) 0.025(3) 0.0002(19) -0.007(2) -0.0008(18) C29 0.020(2) 0.021(2) 0.034(3) -0.001(2) -0.010(2) -0.0014(18) C40 0.025(2) 0.022(2) 0.033(3) -0.007(2) -0.011(2) 0.0002(18) C41 0.030(3) 0.030(2) 0.022(3) -0.004(2) -0.006(2) 0.003(2) C42 0.023(2) 0.028(2) 0.024(3) 0.000(2) -0.006(2) -0.0030(19) C43 0.043(3) 0.061(4) 0.030(3) 0.000(3) -0.013(3) 0.002(3) C44 0.038(3) 0.071(4) 0.026(3) -0.002(3) -0.007(2) -0.009(3) C45 0.024(3) 0.047(3) 0.037(3) 0.001(3) -0.002(2) 0.000(2) C46 0.027(3) 0.042(3) 0.042(3) 0.005(3) -0.003(2) -0.005(2) C47 0.027(3) 0.047(3) 0.046(3) -0.003(3) -0.014(2) -0.001(2) C48 0.030(3) 0.054(3) 0.044(3) -0.006(3) -0.016(3) 0.004(2) C49 0.046(3) 0.049(3) 0.033(3) -0.003(3) -0.012(3) 0.009(3) C50 0.050(3) 0.050(3) 0.024(3) -0.006(3) -0.001(3) 0.009(3) C51 0.028(3) 0.058(3) 0.033(3) 0.003(3) 0.005(2) 0.007(2) C52 0.028(3) 0.047(3) 0.047(4) 0.009(3) -0.006(3) 0.002(2) C53 0.033(3) 0.048(3) 0.049(4) -0.006(3) -0.020(3) -0.002(2) C54 0.031(3) 0.052(3) 0.041(3) -0.008(3) -0.017(3) 0.001(2) C55 0.051(4) 0.064(4) 0.037(4) -0.002(3) -0.011(3) 0.005(3) C56 0.146(8) 0.043(4) 0.050(4) 0.003(3) -0.006(5) 0.015(4) C57A 0.047(6) 0.050(4) 0.036(5) -0.005(4) -0.008(5) 0.004(6) C57B 0.047(6) 0.050(4) 0.036(5) -0.005(4) -0.008(5) 0.004(6) C58 0.063(4) 0.060(4) 0.032(4) 0.000(3) 0.006(3) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C3 1.866(5) . ? Re1 C2 1.894(5) . ? Re1 C1 1.915(5) . ? Re1 N1 2.074(3) . ? Re1 N2 2.085(4) . ? Re2 C20 1.863(5) . ? Re2 C22 1.897(5) . ? Re2 C21 1.917(5) . ? Re2 N3 2.079(3) . ? Re2 N4 2.084(3) . ? K1 O8 2.725(3) . ? K1 O3 2.745(4) . ? K1 O5 2.773(4) . ? K1 O30A 2.785(5) . ? K1 O7 2.801(4) . ? K1 O6 2.807(4) . ? K1 O4 2.816(4) . ? K1 O9 2.857(4) . ? K1 O30B 2.984(14) . ? K1 C16B 3.53(3) . ? K2 O10 2.720(4) . ? K2 O36 2.722(3) . ? K2 O39 2.751(3) . ? K2 O31 2.775(4) . ? K2 O35 2.813(3) . ? K2 O38 2.822(3) . ? K2 O37 2.837(3) . ? K2 O34 2.861(3) . ? O3 C3 1.166(6) . ? O1 C1 1.167(5) . ? O2 C2 1.166(6) . ? O4 C15 1.420(8) . ? O4 C34 1.422(7) . ? O5 C36 1.410(8) . ? O5 C35 1.443(7) . ? O6 C38 1.408(7) . ? O6 C37 1.435(6) . ? O7 C10 1.428(7) . ? O7 C39 1.437(7) . ? O8 C12 1.419(6) . ? O8 C11 1.424(6) . ? O9 C14 1.416(7) . ? O9 C13 1.420(6) . ? O30A C19 1.378(7) . ? O30A C16A 1.447(10) . ? O30B C17 1.372(15) . ? O30B C16B 1.40(3) . ? O31 C20 1.177(6) . ? O32 C21 1.163(5) . ? O33 C22 1.169(5) . ? O34 C43 1.410(6) . ? O34 C54 1.427(6) . ? O35 C45 1.417(5) . ? O35 C44 1.421(6) . ? O36 C47 1.413(6) . ? O36 C46 1.417(6) . ? O37 C49 1.409(6) . ? O37 C48 1.439(6) . ? O38 C50 1.416(6) . ? O38 C51 1.423(6) . ? O39 C52 1.408(6) . ? O39 C53 1.417(6) . ? O10 C55 1.377(7) . ? O10 C58 1.451(7) . ? N1 C33 1.385(5) . ? N1 C9 1.397(5) . ? N2 C4 1.382(6) . ? N2 C8 1.394(6) . ? N3 C28 1.387(5) . ? N3 C42 1.389(5) . ? N4 C23 1.384(6) . ? N4 C27 1.388(5) . ? C4 C5 1.346(7) . ? C4 H4 0.9500 . ? C5 C6 1.415(7) . ? C5 H5 0.9500 . ? C6 C7 1.350(7) . ? C6 H6 0.9500 . ? C7 C8 1.427(6) . ? C7 H7 0.9500 . ? C8 C9 1.391(6) . ? C9 C30 1.408(6) . ? C30 C31 1.355(6) . ? C30 H10 0.9500 . ? C31 C32 1.414(6) . ? C31 H11 0.9500 . ? C32 C33 1.351(6) . ? C32 H12 0.9500 . ? C33 H13 0.9500 . ? C34 C35 1.472(9) . ? C34 H14A 0.9900 . ? C34 H14B 0.9900 . ? C35 H15A 0.9900 . ? C35 H15B 0.9900 . ? C36 C37 1.475(9) . ? C36 H16A 0.9900 . ? C36 H16B 0.9900 . ? C37 H17A 0.9900 . ? C37 H17B 0.9900 . ? C38 C39 1.486(8) . ? C38 H18A 0.9900 . ? C38 H18B 0.9900 . ? C39 H19A 0.9900 . ? C39 H19B 0.9900 . ? C10 C11 1.482(8) . ? C10 H20A 0.9900 . ? C10 H20B 0.9900 . ? C11 H21A 0.9900 . ? C11 H21B 0.9900 . ? C12 C13 1.488(8) . ? C12 H22A 0.9900 . ? C12 H22B 0.9900 . ? C13 H23A 0.9900 . ? C13 H23B 0.9900 . ? C14 C15 1.492(9) . ? C14 H24A 0.9900 . ? C14 H24B 0.9900 . ? C15 H25A 0.9900 . ? C15 H25B 0.9900 . ? C16A C17 1.555(10) . ? C16A H26A 0.9900 . ? C16A H26B 0.9900 . ? C16B C19 1.79(2) . ? C16B H26C 0.9900 . ? C16B H26D 0.9900 . ? C17 C18 1.527(8) . ? C17 H27A 0.9900 . ? C17 H27B 0.9900 . ? C17 H27C 0.9(2) . ? C17 H27D 1.1(2) . ? C18 C19 1.491(7) . ? C18 H27D 1.2(2) . ? C18 H28A 0.9900 . ? C18 H28B 0.9900 . ? C19 H29A 0.9900 . ? C19 H29B 0.9900 . ? C19 H29C 1.2(2) . ? C19 H29D 1.3(2) . ? C23 C24 1.344(6) . ? C23 H33 0.9500 . ? C24 C25 1.422(6) . ? C24 H34 0.9500 . ? C25 C26 1.354(6) . ? C25 H35 0.9500 . ? C26 C27 1.406(6) . ? C26 H36 0.9500 . ? C27 C28 1.413(6) . ? C28 C29 1.421(6) . ? C29 C40 1.350(6) . ? C29 H39 0.9500 . ? C40 C41 1.423(6) . ? C40 H40 0.9500 . ? C41 C42 1.342(6) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.495(7) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.502(7) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.473(7) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.491(7) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.479(7) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.477(7) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.481(9) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57A 1.514(12) . ? C56 C57B 1.689(16) . ? C56 H56C 0.9900 . ? C56 H56D 0.9900 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57A C58 1.544(13) . ? C57A H57A 0.9900 . ? C57A H57B 0.9900 . ? C57B C58 1.378(16) . ? C57B H57C 0.9900 . ? C57B H57D 0.9900 . ? C57B H58D 1.02(11) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C58 H58C 0.91(11) . ? C58 H58D 1.19(11) . ? 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 C3 Re1 C2 92.5(2) . . ? C3 Re1 C1 91.1(2) . . ? C2 Re1 C1 85.78(19) . . ? C3 Re1 N1 110.33(18) . . ? C2 Re1 N1 156.5(2) . . ? C1 Re1 N1 98.64(17) . . ? C3 Re1 N2 102.8(2) . . ? C2 Re1 N2 95.23(18) . . ? C1 Re1 N2 165.94(17) . . ? N1 Re1 N2 75.04(14) . . ? C20 Re2 C22 92.8(2) . . ? C20 Re2 C21 91.0(2) . . ? C22 Re2 C21 88.41(19) . . ? C20 Re2 N3 111.60(17) . . ? C22 Re2 N3 154.84(17) . . ? C21 Re2 N3 96.81(17) . . ? C20 Re2 N4 103.13(17) . . ? C22 Re2 N4 93.90(17) . . ? C21 Re2 N4 165.50(18) . . ? N3 Re2 N4 75.27(14) . . ? O8 K1 O3 87.41(11) . . ? O8 K1 O5 177.34(12) . . ? O3 K1 O5 94.74(11) . . ? O8 K1 O30A 93.37(12) . . ? O3 K1 O30A 164.16(17) . . ? O5 K1 O30A 84.99(13) . . ? O8 K1 O7 60.69(11) . . ? O3 K1 O7 92.48(14) . . ? O5 K1 O7 120.68(13) . . ? O30A K1 O7 74.27(13) . . ? O8 K1 O6 121.06(12) . . ? O3 K1 O6 84.82(13) . . ? O5 K1 O6 60.80(13) . . ? O30A K1 O6 81.23(13) . . ? O7 K1 O6 61.43(12) . . ? O8 K1 O4 118.26(13) . . ? O3 K1 O4 86.08(14) . . ? O5 K1 O4 60.42(13) . . ? O30A K1 O4 107.29(13) . . ? O7 K1 O4 178.29(11) . . ? O6 K1 O4 119.30(13) . . ? O8 K1 O9 60.34(11) . . ? O3 K1 O9 94.82(13) . . ? O5 K1 O9 117.82(13) . . ? O30A K1 O9 99.31(13) . . ? O7 K1 O9 120.05(11) . . ? O6 K1 O9 178.51(12) . . ? O4 K1 O9 59.22(12) . . ? O8 K1 O30B 72.0(3) . . ? O3 K1 O30B 158.1(3) . . ? O5 K1 O30B 105.7(3) . . ? O30A K1 O30B 31.5(3) . . ? O7 K1 O30B 84.0(3) . . ? O6 K1 O30B 111.9(3) . . ? O4 K1 O30B 96.9(3) . . ? O9 K1 O30B 68.8(3) . . ? O8 K1 C16B 82.3(4) . . ? O3 K1 C16B 163.1(4) . . ? O5 K1 C16B 96.0(4) . . ? O30A K1 C16B 11.3(4) . . ? O7 K1 C16B 70.8(4) . . ? O6 K1 C16B 89.0(4) . . ? O4 K1 C16B 110.6(4) . . ? O9 K1 C16B 91.7(4) . . ? O30B K1 C16B 22.9(5) . . ? O10 K2 O36 83.90(12) . . ? O10 K2 O39 89.24(13) . . ? O36 K2 O39 172.80(11) . . ? O10 K2 O31 173.09(14) . . ? O36 K2 O31 94.93(10) . . ? O39 K2 O31 92.15(10) . . ? O10 K2 O35 98.09(11) . . ? O36 K2 O35 59.89(10) . . ? O39 K2 O35 119.28(11) . . ? O31 K2 O35 87.13(12) . . ? O10 K2 O38 81.62(11) . . ? O36 K2 O38 120.14(11) . . ? O39 K2 O38 60.63(10) . . ? O31 K2 O38 93.16(12) . . ? O35 K2 O38 179.69(11) . . ? O10 K2 O37 89.52(13) . . ? O36 K2 O37 61.46(10) . . ? O39 K2 O37 120.82(11) . . ? O31 K2 O37 83.96(11) . . ? O35 K2 O37 119.44(10) . . ? O38 K2 O37 60.68(10) . . ? O10 K2 O34 87.23(13) . . ? O36 K2 O34 116.87(10) . . ? O39 K2 O34 60.43(10) . . ? O31 K2 O34 99.33(12) . . ? O35 K2 O34 59.89(10) . . ? O38 K2 O34 119.97(10) . . ? O37 K2 O34 176.52(10) . . ? C3 O3 K1 130.2(3) . . ? C15 O4 C34 111.9(5) . . ? C15 O4 K1 117.2(3) . . ? C34 O4 K1 114.3(4) . . ? C36 O5 C35 112.3(5) . . ? C36 O5 K1 116.1(4) . . ? C35 O5 K1 115.9(3) . . ? C38 O6 C37 113.4(5) . . ? C38 O6 K1 112.6(3) . . ? C37 O6 K1 111.2(3) . . ? C10 O7 C39 112.6(4) . . ? C10 O7 K1 111.1(3) . . ? C39 O7 K1 110.9(3) . . ? C12 O8 C11 113.4(4) . . ? C12 O8 K1 118.7(3) . . ? C11 O8 K1 117.4(3) . . ? C14 O9 C13 110.7(4) . . ? C14 O9 K1 112.5(4) . . ? C13 O9 K1 110.3(3) . . ? C19 O30A C16A 100.8(5) . . ? C19 O30A K1 119.9(4) . . ? C16A O30A K1 111.2(5) . . ? C17 O30B C16B 100.1(14) . . ? C17 O30B K1 123.8(8) . . ? C16B O30B K1 101.1(13) . . ? C20 O31 K2 123.6(3) . . ? C43 O34 C54 112.1(4) . . ? C43 O34 K2 109.2(3) . . ? C54 O34 K2 111.8(3) . . ? C45 O35 C44 111.0(4) . . ? C45 O35 K2 112.9(3) . . ? C44 O35 K2 117.3(3) . . ? C47 O36 C46 113.3(4) . . ? C47 O36 K2 117.7(3) . . ? C46 O36 K2 120.3(3) . . ? C49 O37 C48 111.7(4) . . ? C49 O37 K2 112.7(3) . . ? C48 O37 K2 107.2(3) . . ? C50 O38 C51 114.0(4) . . ? C50 O38 K2 111.7(3) . . ? C51 O38 K2 110.1(3) . . ? C52 O39 C53 113.7(4) . . ? C52 O39 K2 117.2(3) . . ? C53 O39 K2 116.6(3) . . ? C55 O10 C58 107.7(4) . . ? C55 O10 K2 129.0(3) . . ? C58 O10 K2 116.1(4) . . ? C33 N1 C9 115.8(4) . . ? C33 N1 Re1 125.7(3) . . ? C9 N1 Re1 118.4(3) . . ? C4 N2 C8 117.0(4) . . ? C4 N2 Re1 125.2(3) . . ? C8 N2 Re1 117.7(3) . . ? C28 N3 C42 116.3(4) . . ? C28 N3 Re2 117.9(3) . . ? C42 N3 Re2 125.7(3) . . ? C23 N4 C27 116.3(4) . . ? C23 N4 Re2 125.3(3) . . ? C27 N4 Re2 118.3(3) . . ? O3 C3 Re1 179.5(5) . . ? O1 C1 Re1 177.5(4) . . ? O2 C2 Re1 178.1(5) . . ? C5 C4 N2 124.1(5) . . ? C5 C4 H4 117.9 . . ? N2 C4 H4 117.9 . . ? C4 C5 C6 119.0(5) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C7 C6 C5 119.2(5) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C6 C7 C8 121.0(5) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C9 C8 N2 114.5(4) . . ? C9 C8 C7 126.1(4) . . ? N2 C8 C7 119.4(4) . . ? C8 C9 N1 113.8(4) . . ? C8 C9 C30 125.3(4) . . ? N1 C9 C30 120.9(4) . . ? C31 C30 C9 121.1(4) . . ? C31 C30 H10 119.4 . . ? C9 C30 H10 119.4 . . ? C30 C31 C32 118.5(4) . . ? C30 C31 H11 120.7 . . ? C32 C31 H11 120.7 . . ? C33 C32 C31 119.3(4) . . ? C33 C32 H12 120.3 . . ? C31 C32 H12 120.3 . . ? C32 C33 N1 124.3(4) . . ? C32 C33 H13 117.8 . . ? N1 C33 H13 117.8 . . ? O4 C34 C35 110.1(5) . . ? O4 C34 H14A 109.6 . . ? C35 C34 H14A 109.6 . . ? O4 C34 H14B 109.6 . . ? C35 C34 H14B 109.6 . . ? H14A C34 H14B 108.2 . . ? O5 C35 C34 109.2(5) . . ? O5 C35 H15A 109.8 . . ? C34 C35 H15A 109.8 . . ? O5 C35 H15B 109.8 . . ? C34 C35 H15B 109.8 . . ? H15A C35 H15B 108.3 . . ? O5 C36 C37 108.7(5) . . ? O5 C36 H16A 109.9 . . ? C37 C36 H16A 109.9 . . ? O5 C36 H16B 109.9 . . ? C37 C36 H16B 109.9 . . ? H16A C36 H16B 108.3 . . ? O6 C37 C36 109.6(5) . . ? O6 C37 H17A 109.7 . . ? C36 C37 H17A 109.7 . . ? O6 C37 H17B 109.7 . . ? C36 C37 H17B 109.7 . . ? H17A C37 H17B 108.2 . . ? O6 C38 C39 108.6(5) . . ? O6 C38 H18A 110.0 . . ? C39 C38 H18A 110.0 . . ? O6 C38 H18B 110.0 . . ? C39 C38 H18B 110.0 . . ? H18A C38 H18B 108.3 . . ? O7 C39 C38 108.6(5) . . ? O7 C39 H19A 110.0 . . ? C38 C39 H19A 110.0 . . ? O7 C39 H19B 110.0 . . ? C38 C39 H19B 110.0 . . ? H19A C39 H19B 108.3 . . ? O7 C10 C11 108.3(5) . . ? O7 C10 H20A 110.0 . . ? C11 C10 H20A 110.0 . . ? O7 C10 H20B 110.0 . . ? C11 C10 H20B 110.0 . . ? H20A C10 H20B 108.4 . . ? O8 C11 C10 107.7(4) . . ? O8 C11 H21A 110.2 . . ? C10 C11 H21A 110.2 . . ? O8 C11 H21B 110.2 . . ? C10 C11 H21B 110.2 . . ? H21A C11 H21B 108.5 . . ? O8 C12 C13 107.4(4) . . ? O8 C12 H22A 110.2 . . ? C13 C12 H22A 110.2 . . ? O8 C12 H22B 110.2 . . ? C13 C12 H22B 110.2 . . ? H22A C12 H22B 108.5 . . ? O9 C13 C12 110.1(4) . . ? O9 C13 H23A 109.6 . . ? C12 C13 H23A 109.6 . . ? O9 C13 H23B 109.6 . . ? C12 C13 H23B 109.6 . . ? H23A C13 H23B 108.2 . . ? O9 C14 C15 108.9(5) . . ? O9 C14 H24A 109.9 . . ? C15 C14 H24A 109.9 . . ? O9 C14 H24B 109.9 . . ? C15 C14 H24B 109.9 . . ? H24A C14 H24B 108.3 . . ? O4 C15 C14 107.6(5) . . ? O4 C15 H25A 110.2 . . ? C14 C15 H25A 110.2 . . ? O4 C15 H25B 110.2 . . ? C14 C15 H25B 110.2 . . ? H25A C15 H25B 108.5 . . ? O30A C16A C17 102.8(6) . . ? O30A C16A H26A 111.2 . . ? C17 C16A H26A 111.2 . . ? O30A C16A H26B 111.2 . . ? C17 C16A H26B 111.2 . . ? H26A C16A H26B 109.1 . . ? O30B C16B C19 96.9(15) . . ? O30B C16B K1 56.0(11) . . ? C19 C16B K1 79.9(10) . . ? O30B C16B H26C 112.4 . . ? C19 C16B H26C 112.4 . . ? K1 C16B H26C 70.7 . . ? O30B C16B H26D 112.4 . . ? C19 C16B H26D 112.4 . . ? K1 C16B H26D 165.1 . . ? H26C C16B H26D 109.9 . . ? O30B C17 C18 108.4(7) . . ? O30B C17 C16A 32.4(6) . . ? C18 C17 C16A 100.3(5) . . ? O30B C17 H27A 79.8 . . ? C18 C17 H27A 111.7 . . ? C16A C17 H27A 111.7 . . ? O30B C17 H27B 130.8 . . ? C18 C17 H27B 111.7 . . ? C16A C17 H27B 111.7 . . ? H27A C17 H27B 109.5 . . ? O30B C17 H27C 135(10) . . ? C18 C17 H27C 102(10) . . ? C16A C17 H27C 111(10) . . ? H27A C17 H27C 118.2 . . ? H27B C17 H27C 10.6 . . ? O30B C17 H27D 81(10) . . ? C18 C17 H27D 53(10) . . ? C16A C17 H27D 100(10) . . ? H27A C17 H27D 62.5 . . ? H27B C17 H27D 147.5 . . ? H27C C17 H27D 144(10) . . ? C19 C18 C17 104.0(5) . . ? C19 C18 H27D 98(10) . . ? C17 C18 H27D 47(10) . . ? C19 C18 H28A 110.9 . . ? C17 C18 H28A 110.9 . . ? H27D C18 H28A 70.5 . . ? C19 C18 H28B 110.9 . . ? C17 C18 H28B 110.9 . . ? H27D C18 H28B 148.3 . . ? H28A C18 H28B 109.0 . . ? O30A C19 C18 107.3(5) . . ? O30A C19 C16B 32.6(8) . . ? C18 C19 C16B 97.4(9) . . ? O30A C19 H29A 110.2 . . ? C18 C19 H29A 110.3 . . ? C16B C19 H29A 140.9 . . ? O30A C19 H29B 110.3 . . ? C18 C19 H29B 110.3 . . ? C16B C19 H29B 85.8 . . ? H29A C19 H29B 108.5 . . ? O30A C19 H29C 117(10) . . ? C18 C19 H29C 112(10) . . ? C16B C19 H29C 94(10) . . ? H29A C19 H29C 100.2 . . ? H29B C19 H29C 8.8 . . ? O30A C19 H29D 83(9) . . ? C18 C19 H29D 131(9) . . ? C16B C19 H29D 112(9) . . ? H29A C19 H29D 29.4 . . ? H29B C19 H29D 110.3 . . ? H29C C19 H29D 105(10) . . ? O31 C20 Re2 179.5(5) . . ? O32 C21 Re2 179.3(4) . . ? O33 C22 Re2 176.7(4) . . ? C24 C23 N4 124.0(4) . . ? C24 C23 H33 118.0 . . ? N4 C23 H33 118.0 . . ? C23 C24 C25 119.6(4) . . ? C23 C24 H34 120.2 . . ? C25 C24 H34 120.2 . . ? C26 C25 C24 118.1(4) . . ? C26 C25 H35 121.0 . . ? C24 C25 H35 121.0 . . ? C25 C26 C27 121.2(4) . . ? C25 C26 H36 119.4 . . ? C27 C26 H36 119.4 . . ? N4 C27 C26 120.8(4) . . ? N4 C27 C28 113.4(4) . . ? C26 C27 C28 125.8(4) . . ? N3 C28 C27 114.6(4) . . ? N3 C28 C29 120.6(4) . . ? C27 C28 C29 124.8(4) . . ? C40 C29 C28 121.1(4) . . ? C40 C29 H39 119.4 . . ? C28 C29 H39 119.4 . . ? C29 C40 C41 118.4(4) . . ? C29 C40 H40 120.8 . . ? C41 C40 H40 120.8 . . ? C42 C41 C40 119.4(4) . . ? C42 C41 H41 120.3 . . ? C40 C41 H41 120.3 . . ? C41 C42 N3 124.2(4) . . ? C41 C42 H42 117.9 . . ? N3 C42 H42 117.9 . . ? O34 C43 C44 109.4(4) . . ? O34 C43 H43A 109.8 . . ? C44 C43 H43A 109.8 . . ? O34 C43 H43B 109.8 . . ? C44 C43 H43B 109.8 . . ? H43A C43 H43B 108.2 . . ? O35 C44 C43 108.6(4) . . ? O35 C44 H44A 110.0 . . ? C43 C44 H44A 110.0 . . ? O35 C44 H44B 110.0 . . ? C43 C44 H44B 110.0 . . ? H44A C44 H44B 108.3 . . ? O35 C45 C46 109.4(4) . . ? O35 C45 H45A 109.8 . . ? C46 C45 H45A 109.8 . . ? O35 C45 H45B 109.8 . . ? C46 C45 H45B 109.8 . . ? H45A C45 H45B 108.2 . . ? O36 C46 C45 107.9(4) . . ? O36 C46 H46A 110.1 . . ? C45 C46 H46A 110.1 . . ? O36 C46 H46B 110.1 . . ? C45 C46 H46B 110.1 . . ? H46A C46 H46B 108.4 . . ? O36 C47 C48 108.9(4) . . ? O36 C47 H47A 109.9 . . ? C48 C47 H47A 109.9 . . ? O36 C47 H47B 109.9 . . ? C48 C47 H47B 109.9 . . ? H47A C47 H47B 108.3 . . ? O37 C48 C47 110.0(4) . . ? O37 C48 H48A 109.7 . . ? C47 C48 H48A 109.7 . . ? O37 C48 H48B 109.7 . . ? C47 C48 H48B 109.7 . . ? H48A C48 H48B 108.2 . . ? O37 C49 C50 109.1(4) . . ? O37 C49 H49A 109.9 . . ? C50 C49 H49A 109.9 . . ? O37 C49 H49B 109.9 . . ? C50 C49 H49B 109.9 . . ? H49A C49 H49B 108.3 . . ? O38 C50 C49 108.5(4) . . ? O38 C50 H50A 110.0 . . ? C49 C50 H50A 110.0 . . ? O38 C50 H50B 110.0 . . ? C49 C50 H50B 110.0 . . ? H50A C50 H50B 108.4 . . ? O38 C51 C52 109.3(4) . . ? O38 C51 H51A 109.8 . . ? C52 C51 H51A 109.8 . . ? O38 C51 H51B 109.8 . . ? C52 C51 H51B 109.8 . . ? H51A C51 H51B 108.3 . . ? O39 C52 C51 108.7(4) . . ? O39 C52 H52A 109.9 . . ? C51 C52 H52A 109.9 . . ? O39 C52 H52B 109.9 . . ? C51 C52 H52B 109.9 . . ? H52A C52 H52B 108.3 . . ? O39 C53 C54 108.6(4) . . ? O39 C53 H53A 110.0 . . ? C54 C53 H53A 110.0 . . ? O39 C53 H53B 110.0 . . ? C54 C53 H53B 110.0 . . ? H53A C53 H53B 108.4 . . ? O34 C54 C53 110.4(4) . . ? O34 C54 H54A 109.6 . . ? C53 C54 H54A 109.6 . . ? O34 C54 H54B 109.6 . . ? C53 C54 H54B 109.6 . . ? H54A C54 H54B 108.1 . . ? O10 C55 C56 105.8(5) . . ? O10 C55 H55A 110.6 . . ? C56 C55 H55A 110.6 . . ? O10 C55 H55B 110.6 . . ? C56 C55 H55B 110.6 . . ? H55A C55 H55B 108.7 . . ? C55 C56 C57A 107.5(6) . . ? C55 C56 C57B 89.3(7) . . ? C57A C56 C57B 31.8(6) . . ? C55 C56 H56C 110.2 . . ? C57A C56 H56C 110.2 . . ? C57B C56 H56C 93.6 . . ? C55 C56 H56D 110.2 . . ? C57A C56 H56D 110.2 . . ? C57B C56 H56D 142.0 . . ? H56C C56 H56D 108.5 . . ? C55 C56 H56A 113.8 . . ? C57A C56 H56A 124.8 . . ? C57B C56 H56A 113.8 . . ? H56C C56 H56A 20.9 . . ? H56D C56 H56A 88.5 . . ? C55 C56 H56B 113.8 . . ? C57A C56 H56B 82.4 . . ? C57B C56 H56B 113.8 . . ? H56C C56 H56B 127.5 . . ? H56D C56 H56B 28.8 . . ? H56A C56 H56B 111.0 . . ? C56 C57A C58 102.1(7) . . ? C56 C57A H57A 111.4 . . ? C58 C57A H57A 111.4 . . ? C56 C57A H57B 111.4 . . ? C58 C57A H57B 111.4 . . ? H57A C57A H57B 109.2 . . ? C58 C57B C56 101.1(9) . . ? C58 C57B H57C 111.6 . . ? C56 C57B H57C 111.6 . . ? C58 C57B H57D 111.6 . . ? C56 C57B H57D 111.6 . . ? H57C C57B H57D 109.4 . . ? C58 C57B H58D 57(6) . . ? C56 C57B H58D 127(6) . . ? H57C C57B H58D 121.7 . . ? H57D C57B H58D 54.8 . . ? C57B C58 O10 105.3(7) . . ? C57B C58 C57A 35.1(7) . . ? O10 C58 C57A 105.0(6) . . ? C57B C58 H58A 110.7 . . ? O10 C58 H58A 110.7 . . ? C57A C58 H58A 137.2 . . ? C57B C58 H58B 110.7 . . ? O10 C58 H58B 110.7 . . ? C57A C58 H58B 78.6 . . ? H58A C58 H58B 108.8 . . ? C57B C58 H58C 133(7) . . ? O10 C58 H58C 120(7) . . ? C57A C58 H58C 115(7) . . ? H58A C58 H58C 65.1 . . ? H58B C58 H58C 44.2 . . ? C57B C58 H58D 46(5) . . ? O10 C58 H58D 103(5) . . ? C57A C58 H58D 81(5) . . ? H58A C58 H58D 69.3 . . ? H58B C58 H58D 144.4 . . ? H58C C58 H58D 125(9) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.705 _refine_diff_density_min -0.756 _refine_diff_density_rms 0.093