# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Stephen Liddle' _publ_contact_author_email STEPHEN.LIDDLE@NOTTINGHAM.AC.UK _publ_section_title ; Synthesis and Structure of [{N(CH2CH2NSiMe3)3}URe(?5-C5H5)2]: A Heterobimetallic Complex with an Unsupported Uranium-Rhenium Bond ; loop_ _publ_author_name 'Stephen Liddle' 'Benedict M. Gardner' 'William Lewis' 'Jonathan McMaster' # Attachment '3.cif' data_utreni _database_code_depnum_ccdc_archive 'CCDC 723115' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H47 I N4 O Si3 U' _chemical_formula_sum 'C19 H47 I N4 O Si3 U' _chemical_formula_weight 796.81 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 43 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 12.8637(3) _cell_length_b 12.8637(3) _cell_length_c 36.1910(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5988.7(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11530 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 25.84 _exptl_crystal_description Block _exptl_crystal_colour 'Pale green' _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3072 _exptl_absorpt_coefficient_mu 6.588 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.15 _exptl_absorpt_correction_T_max 0.49 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 53401 _diffrn_reflns_av_R_equivalents 0.074 _diffrn_reflns_av_sigmaI/netI 0.056 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.51 _reflns_number_total 6891 _reflns_number_gt 5977 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36A (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Sheldrick, 2008)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al., 2004); PLATON (Spek, 2003)' _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^)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, Me from difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.003(4) _refine_ls_number_reflns 6891 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0530 _refine_ls_wR_factor_gt 0.0490 _refine_ls_goodness_of_fit_ref 1.06 _refine_ls_restrained_S_all 1.06 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.469790(16) 0.883580(15) 0.435014(5) 0.01147(5) Uani 1 1 d . . . I1 I 0.48120(3) 0.79595(3) 0.515979(9) 0.02423(10) Uani 1 1 d . . . N1 N 0.4779(4) 1.0555(3) 0.42537(10) 0.0162(10) Uani 1 1 d . . . N2 N 0.6101(3) 0.8421(3) 0.40179(10) 0.0162(10) Uani 1 1 d . . . N3 N 0.2987(3) 0.8752(3) 0.42161(10) 0.0145(9) Uani 1 1 d . . . N4 N 0.4400(3) 0.9140(3) 0.36552(10) 0.0161(10) Uani 1 1 d . . . Si1 Si 0.50263(12) 1.15478(12) 0.45650(4) 0.0191(3) Uani 1 1 d . . . C1 C 0.3915(5) 1.2478(5) 0.45727(15) 0.0341(15) Uani 1 1 d . . . H1A H 0.3849 1.2811 0.4330 0.051 Uiso 1 1 calc R . . H1B H 0.4039 1.3010 0.4761 0.051 Uiso 1 1 calc R . . H1C H 0.3272 1.2102 0.4630 0.051 Uiso 1 1 calc R . . C2 C 0.6247(5) 1.2267(5) 0.44478(16) 0.0382(17) Uani 1 1 d . . . H2A H 0.6836 1.1784 0.4450 0.057 Uiso 1 1 calc R . . H2B H 0.6364 1.2818 0.4630 0.057 Uiso 1 1 calc R . . H2C H 0.6180 1.2577 0.4202 0.057 Uiso 1 1 calc R . . C3 C 0.5186(4) 1.1013(4) 0.50441(13) 0.0253(13) Uani 1 1 d . . . H3A H 0.4523 1.0722 0.5128 0.038 Uiso 1 1 calc R . . H3B H 0.5400 1.1572 0.5211 0.038 Uiso 1 1 calc R . . H3C H 0.5716 1.0467 0.5042 0.038 Uiso 1 1 calc R . . C4 C 0.4549(5) 1.0950(4) 0.38759(13) 0.0225(13) Uani 1 1 d . . . H4A H 0.4923 1.1613 0.3836 0.027 Uiso 1 1 calc R . . H4B H 0.3795 1.1090 0.3854 0.027 Uiso 1 1 calc R . . C5 C 0.4869(4) 1.0182(4) 0.35833(13) 0.0223(12) Uani 1 1 d . . . H5A H 0.4641 1.0436 0.3338 0.027 Uiso 1 1 calc R . . H5B H 0.5636 1.0121 0.3580 0.027 Uiso 1 1 calc R . . Si2 Si 0.73628(12) 0.85836(12) 0.41780(4) 0.0187(3) Uani 1 1 d . . . C6 C 0.8102(4) 0.7344(5) 0.41545(16) 0.0284(14) Uani 1 1 d . . . H6A H 0.7843 0.6865 0.4344 0.043 Uiso 1 1 calc R . . H6B H 0.8841 0.7483 0.4198 0.043 Uiso 1 1 calc R . . H6C H 0.8012 0.7032 0.3910 0.043 Uiso 1 1 calc R . . C7 C 0.8069(5) 0.9593(5) 0.39076(15) 0.0358(16) Uani 1 1 d . . . H7A H 0.8120 0.9373 0.3649 0.054 Uiso 1 1 calc R . . H7B H 0.8769 0.9684 0.4010 0.054 Uiso 1 1 calc R . . H7C H 0.7690 1.0253 0.3922 0.054 Uiso 1 1 calc R . . C8 C 0.7320(5) 0.9051(5) 0.46660(15) 0.0371(17) Uani 1 1 d . . . H8A H 0.6916 0.9695 0.4679 0.056 Uiso 1 1 calc R . . H8B H 0.8029 0.9181 0.4753 0.056 Uiso 1 1 calc R . . H8C H 0.6993 0.8521 0.4822 0.056 Uiso 1 1 calc R . . C9 C 0.6060(5) 0.8210(5) 0.36161(13) 0.0245(13) Uani 1 1 d . . . H9A H 0.6336 0.7505 0.3567 0.029 Uiso 1 1 calc R . . H9B H 0.6508 0.8716 0.3485 0.029 Uiso 1 1 calc R . . C10 C 0.4968(4) 0.8286(4) 0.34687(13) 0.0204(13) Uani 1 1 d . . . H10A H 0.4989 0.8416 0.3199 0.024 Uiso 1 1 calc R . . H10B H 0.4601 0.7620 0.3511 0.024 Uiso 1 1 calc R . . Si3 Si 0.19473(12) 0.92483(13) 0.44596(4) 0.0212(4) Uani 1 1 d . . . C11 C 0.1377(5) 1.0406(5) 0.42155(16) 0.046(2) Uani 1 1 d . . . H11A H 0.1913 1.0941 0.4186 0.069 Uiso 1 1 calc R . . H11B H 0.0800 1.0686 0.4361 0.069 Uiso 1 1 calc R . . H11C H 0.1122 1.0194 0.3972 0.069 Uiso 1 1 calc R . . C12 C 0.2362(5) 0.9709(5) 0.49272(14) 0.0363(16) Uani 1 1 d . . . H12A H 0.2619 0.9118 0.5072 0.054 Uiso 1 1 calc R . . H12B H 0.1767 1.0023 0.5054 0.054 Uiso 1 1 calc R . . H12C H 0.2916 1.0226 0.4901 0.054 Uiso 1 1 calc R . . C13 C 0.0912(5) 0.8249(6) 0.45188(19) 0.056(2) Uani 1 1 d . . . H13A H 0.0694 0.7993 0.4276 0.084 Uiso 1 1 calc R . . H13B H 0.0315 0.8560 0.4646 0.084 Uiso 1 1 calc R . . H13C H 0.1182 0.7670 0.4666 0.084 Uiso 1 1 calc R . . C14 C 0.2733(4) 0.8414(5) 0.38341(13) 0.0224(13) Uani 1 1 d . . . H14A H 0.1973 0.8457 0.3793 0.027 Uiso 1 1 calc R . . H14B H 0.2950 0.7682 0.3798 0.027 Uiso 1 1 calc R . . C15 C 0.3288(4) 0.9101(4) 0.35617(13) 0.0227(13) Uani 1 1 d . . . H15A H 0.3198 0.8823 0.3309 0.027 Uiso 1 1 calc R . . H15B H 0.2990 0.9810 0.3570 0.027 Uiso 1 1 calc R . . O1 O 0.4432(3) 0.6890(3) 0.42505(9) 0.0183(9) Uani 1 1 d . . . C16 C 0.3553(4) 0.6347(4) 0.44030(14) 0.0196(12) Uani 1 1 d . . . H16A H 0.3049 0.6175 0.4206 0.023 Uiso 1 1 calc R . . H16B H 0.3199 0.6785 0.4589 0.023 Uiso 1 1 calc R . . C17 C 0.3954(5) 0.5374(4) 0.45785(15) 0.0259(13) Uani 1 1 d . . . H17A H 0.3427 0.4814 0.4572 0.031 Uiso 1 1 calc R . . H17B H 0.4164 0.5498 0.4838 0.031 Uiso 1 1 calc R . . C18 C 0.4889(5) 0.5108(4) 0.43381(16) 0.0286(14) Uani 1 1 d . . . H18A H 0.5401 0.4679 0.4474 0.034 Uiso 1 1 calc R . . H18B H 0.4677 0.4740 0.4110 0.034 Uiso 1 1 calc R . . C19 C 0.5316(5) 0.6180(4) 0.42536(15) 0.0282(14) Uani 1 1 d . . . H19A H 0.5824 0.6392 0.4445 0.034 Uiso 1 1 calc R . . H19B H 0.5668 0.6183 0.4010 0.034 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 U1 0.01279(10) 0.01149(10) 0.01013(7) 0.00037(8) -0.00033(8) -0.00067(9) I1 0.0316(2) 0.0267(2) 0.01432(16) 0.00458(14) -0.00225(16) -0.00342(19) N1 0.021(3) 0.015(2) 0.0124(19) 0.0010(16) 0.0008(18) -0.001(2) N2 0.016(2) 0.022(2) 0.011(2) 0.0009(17) -0.0013(18) -0.001(2) N3 0.013(2) 0.018(2) 0.0125(19) -0.0005(19) -0.0018(17) 0.002(2) N4 0.013(2) 0.018(3) 0.017(2) 0.0010(18) -0.0030(18) -0.0016(18) Si1 0.0255(10) 0.0127(8) 0.0192(7) -0.0006(6) -0.0009(6) -0.0026(6) C1 0.047(4) 0.025(4) 0.030(3) -0.006(3) -0.001(3) 0.013(3) C2 0.048(5) 0.029(4) 0.037(4) -0.008(3) 0.004(3) -0.020(3) C3 0.033(4) 0.021(3) 0.021(3) -0.005(2) 0.000(3) 0.000(3) C4 0.034(4) 0.013(3) 0.021(3) 0.004(2) -0.006(3) -0.007(2) C5 0.025(3) 0.020(3) 0.022(3) 0.005(2) -0.001(2) 0.000(3) Si2 0.0144(8) 0.0205(9) 0.0213(7) 0.0021(7) 0.0025(6) -0.0013(6) C6 0.019(3) 0.032(4) 0.034(3) -0.001(3) -0.001(3) 0.003(3) C7 0.034(4) 0.041(4) 0.032(3) 0.008(3) 0.005(3) -0.007(4) C8 0.025(4) 0.053(5) 0.033(3) -0.007(3) -0.006(3) 0.004(3) C9 0.026(3) 0.027(3) 0.020(3) -0.003(2) 0.002(3) 0.005(3) C10 0.024(3) 0.024(3) 0.013(2) -0.003(2) 0.001(2) 0.003(3) Si3 0.0137(8) 0.0298(9) 0.0201(8) -0.0010(7) 0.0006(6) 0.0019(7) C11 0.048(5) 0.055(5) 0.036(4) -0.001(3) -0.003(3) 0.026(4) C12 0.030(4) 0.058(5) 0.021(3) -0.008(3) 0.002(3) 0.019(4) C13 0.034(5) 0.072(6) 0.063(5) -0.010(4) 0.017(4) -0.023(4) C14 0.020(3) 0.031(4) 0.016(3) 0.000(2) -0.003(2) -0.003(3) C15 0.032(4) 0.023(4) 0.013(3) 0.000(2) -0.008(2) -0.002(3) O1 0.014(2) 0.021(2) 0.0196(19) -0.0014(15) 0.0007(15) -0.0004(17) C16 0.026(3) 0.007(3) 0.026(3) 0.001(2) -0.002(2) -0.007(2) C17 0.029(3) 0.018(3) 0.031(3) 0.004(3) 0.004(3) -0.004(3) C18 0.035(4) 0.017(3) 0.034(3) 0.002(3) -0.001(3) -0.002(3) C19 0.026(3) 0.020(3) 0.039(3) -0.004(3) 0.005(3) 0.003(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 U1 I1 3.1430(4) . ? U1 O1 2.552(4) . ? U1 N1 2.241(4) . ? U1 N2 2.233(4) . ? U1 N3 2.256(4) . ? U1 N4 2.574(4) . ? N1 C4 1.488(6) . ? N1 Si1 1.733(4) . ? N2 C9 1.480(6) . ? N2 Si2 1.737(5) . ? N3 C14 1.486(6) . ? N3 Si3 1.724(4) . ? N4 C15 1.471(7) . ? N4 C10 1.483(6) . ? N4 C5 1.492(7) . ? Si1 C1 1.865(6) . ? Si1 C2 1.872(6) . ? Si1 C3 1.876(5) . ? C4 C5 1.506(7) . ? Si2 C6 1.858(6) . ? Si2 C7 1.863(6) . ? Si2 C8 1.866(6) . ? C9 C10 1.505(7) . ? Si3 C13 1.863(7) . ? Si3 C12 1.870(5) . ? Si3 C11 1.880(6) . ? C14 C15 1.505(7) . ? O1 C16 1.439(6) . ? O1 C19 1.458(6) . ? C16 C17 1.495(7) . ? C17 C18 1.523(8) . ? C18 C19 1.516(7) . ? 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 N2 U1 N1 96.56(16) . . ? N2 U1 N3 131.38(14) . . ? N1 U1 N3 93.38(16) . . ? N2 U1 O1 78.33(13) . . ? N1 U1 O1 162.19(12) . . ? N3 U1 O1 78.01(14) . . ? N2 U1 N4 68.30(14) . . ? N1 U1 N4 72.83(13) . . ? N3 U1 N4 69.64(13) . . ? O1 U1 N4 89.49(12) . . ? N2 U1 I1 112.25(10) . . ? N1 U1 I1 119.80(9) . . ? N3 U1 I1 103.23(10) . . ? O1 U1 I1 77.65(7) . . ? N4 U1 I1 166.52(10) . . ? C4 N1 Si1 112.5(3) . . ? C4 N1 U1 118.1(3) . . ? Si1 N1 U1 129.4(2) . . ? C9 N2 Si2 112.5(3) . . ? C9 N2 U1 123.0(3) . . ? Si2 N2 U1 123.2(2) . . ? C14 N3 Si3 114.4(3) . . ? C14 N3 U1 115.4(3) . . ? Si3 N3 U1 129.0(2) . . ? C15 N4 C10 110.5(4) . . ? C15 N4 C5 112.5(4) . . ? C10 N4 C5 112.8(4) . . ? C15 N4 U1 111.4(3) . . ? C10 N4 U1 105.0(3) . . ? C5 N4 U1 104.3(3) . . ? N1 Si1 C1 110.0(3) . . ? N1 Si1 C2 111.8(2) . . ? C1 Si1 C2 109.2(3) . . ? N1 Si1 C3 110.5(2) . . ? C1 Si1 C3 107.8(3) . . ? C2 Si1 C3 107.4(3) . . ? N1 C4 C5 111.6(4) . . ? N4 C5 C4 110.9(4) . . ? N2 Si2 C6 111.1(2) . . ? N2 Si2 C7 111.4(2) . . ? C6 Si2 C7 108.9(3) . . ? N2 Si2 C8 109.1(2) . . ? C6 Si2 C8 109.5(3) . . ? C7 Si2 C8 106.7(3) . . ? N2 C9 C10 111.7(4) . . ? N4 C10 C9 110.3(4) . . ? N3 Si3 C13 111.0(3) . . ? N3 Si3 C12 111.0(2) . . ? C13 Si3 C12 108.5(3) . . ? N3 Si3 C11 110.8(3) . . ? C13 Si3 C11 108.8(3) . . ? C12 Si3 C11 106.6(3) . . ? N3 C14 C15 109.4(4) . . ? N4 C15 C14 109.3(4) . . ? C16 O1 C19 107.8(4) . . ? C16 O1 U1 121.8(3) . . ? C19 O1 U1 120.6(3) . . ? O1 C16 C17 107.3(4) . . ? C16 C17 C18 102.6(4) . . ? C19 C18 C17 101.3(4) . . ? O1 C19 C18 106.8(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.06 _refine_diff_density_min -0.73 _refine_diff_density_rms 0.14 data_uretrn _database_code_depnum_ccdc_archive 'CCDC 723116' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H49 N4 Re Si3 U' _chemical_formula_sum 'C25 H49 N4 Re Si3 U' _chemical_formula_weight 914.18 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' Si Si 0.0817 0.0704 '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' U U -9.6767 9.6646 '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 15.805(2) _cell_length_b 10.2483(12) _cell_length_c 19.910(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.734(2) _cell_angle_gamma 90.00 _cell_volume 3168.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5311 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 27.28 _exptl_crystal_description Plate _exptl_crystal_colour Red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.916 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 9.055 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.12 _exptl_absorpt_correction_T_max 0.64 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 19270 _diffrn_reflns_av_R_equivalents 0.0584 _diffrn_reflns_av_sigmaI/netI 0.0729 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.53 _reflns_number_total 7190 _reflns_number_gt 5416 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0361P)^2^+0.8064P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, Me from difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7190 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0948 _refine_ls_wR_factor_gt 0.0857 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 U1 U 0.229417(17) 0.76525(2) 0.389812(14) 0.02082(8) Uani 1 1 d . . . N1 N 0.1122(4) 0.8738(6) 0.3316(3) 0.0266(14) Uani 1 1 d . . . Si1 Si 0.01390(14) 0.9024(2) 0.35544(11) 0.0256(4) Uani 1 1 d . . . C1 C 0.0199(5) 0.8548(7) 0.4467(4) 0.0294(17) Uani 1 1 d . . . H1A H 0.0630 0.9088 0.4759 0.044 Uiso 1 1 calc R . . H1B H 0.0364 0.7627 0.4526 0.044 Uiso 1 1 calc R . . H1C H -0.0364 0.8677 0.4595 0.044 Uiso 1 1 calc R . . C2 C -0.0197(6) 1.0771(8) 0.3462(4) 0.037(2) Uani 1 1 d . . . H2A H 0.0300 1.1331 0.3629 0.056 Uiso 1 1 calc R . . H2B H -0.0648 1.0935 0.3729 0.056 Uiso 1 1 calc R . . H2C H -0.0419 1.0964 0.2979 0.056 Uiso 1 1 calc R . . C3 C -0.0755(5) 0.8059(8) 0.3028(4) 0.0331(18) Uani 1 1 d . . . H3A H -0.0764 0.8221 0.2542 0.050 Uiso 1 1 calc R . . H3B H -0.1306 0.8326 0.3143 0.050 Uiso 1 1 calc R . . H3C H -0.0662 0.7128 0.3126 0.050 Uiso 1 1 calc R . . C4 C 0.1196(5) 0.9359(8) 0.2656(4) 0.0349(19) Uani 1 1 d . . . H4A H 0.0681 0.9901 0.2492 0.042 Uiso 1 1 calc R . . H4B H 0.1229 0.8676 0.2309 0.042 Uiso 1 1 calc R . . C5 C 0.2009(5) 1.0215(7) 0.2750(4) 0.0339(19) Uani 1 1 d . . . H5A H 0.2075 1.0603 0.2307 0.041 Uiso 1 1 calc R . . H5B H 0.1966 1.0931 0.3075 0.041 Uiso 1 1 calc R . . N2 N 0.3199(4) 0.9175(6) 0.4470(3) 0.0271(14) Uani 1 1 d . . . Si2 Si 0.32995(14) 1.0161(2) 0.51837(11) 0.0280(5) Uani 1 1 d . . . C6 C 0.2212(6) 1.0668(9) 0.5358(5) 0.046(2) Uani 1 1 d . . . H6A H 0.1990 0.9987 0.5625 0.069 Uiso 1 1 calc R . . H6B H 0.1812 1.0792 0.4924 0.069 Uiso 1 1 calc R . . H6C H 0.2269 1.1487 0.5617 0.069 Uiso 1 1 calc R . . C7 C 0.3911(5) 0.9339(8) 0.5966(4) 0.036(2) Uani 1 1 d . . . H7A H 0.4439 0.8954 0.5862 0.055 Uiso 1 1 calc R . . H7B H 0.3554 0.8651 0.6112 0.055 Uiso 1 1 calc R . . H7C H 0.4059 0.9981 0.6334 0.055 Uiso 1 1 calc R . . C8 C 0.3883(6) 1.1721(8) 0.5078(5) 0.043(2) Uani 1 1 d . . . H8A H 0.4463 1.1521 0.5001 0.065 Uiso 1 1 calc R . . H8B H 0.3922 1.2251 0.5492 0.065 Uiso 1 1 calc R . . H8C H 0.3567 1.2206 0.4685 0.065 Uiso 1 1 calc R . . C9 C 0.3875(5) 0.9395(8) 0.4051(4) 0.0345(19) Uani 1 1 d . . . H9A H 0.4097 0.8545 0.3923 0.041 Uiso 1 1 calc R . . H9B H 0.4361 0.9887 0.4321 0.041 Uiso 1 1 calc R . . C10 C 0.3502(6) 1.0154(9) 0.3411(4) 0.044(2) Uani 1 1 d . . . H10A H 0.3292 1.1015 0.3534 0.053 Uiso 1 1 calc R . . H10B H 0.3948 1.0294 0.3129 0.053 Uiso 1 1 calc R . . N3 N 0.3052(4) 0.6654(6) 0.3202(3) 0.0288(15) Uani 1 1 d . . . Si3 Si 0.39060(16) 0.5563(2) 0.32723(12) 0.0346(5) Uani 1 1 d . . . C11 C 0.3570(7) 0.4018(9) 0.2781(6) 0.057(3) Uani 1 1 d . . . H11A H 0.3101 0.3603 0.2962 0.086 Uiso 1 1 calc R . . H11B H 0.4062 0.3421 0.2828 0.086 Uiso 1 1 calc R . . H11C H 0.3373 0.4229 0.2297 0.086 Uiso 1 1 calc R . . C12 C 0.4285(6) 0.5147(10) 0.4187(5) 0.053(3) Uani 1 1 d . . . H12A H 0.3811 0.4756 0.4373 0.080 Uiso 1 1 calc R . . H12B H 0.4482 0.5941 0.4444 0.080 Uiso 1 1 calc R . . H12C H 0.4763 0.4524 0.4228 0.080 Uiso 1 1 calc R . . C13 C 0.4838(6) 0.6274(9) 0.2938(5) 0.047(2) Uani 1 1 d . . . H13A H 0.5020 0.7089 0.3181 0.070 Uiso 1 1 calc R . . H13B H 0.4665 0.6453 0.2448 0.070 Uiso 1 1 calc R . . H13C H 0.5318 0.5653 0.3010 0.070 Uiso 1 1 calc R . . C14 C 0.2731(6) 0.7177(8) 0.2512(4) 0.036(2) Uani 1 1 d . . . H14A H 0.2094 0.7151 0.2412 0.043 Uiso 1 1 calc R . . H14B H 0.2946 0.6634 0.2168 0.043 Uiso 1 1 calc R . . C15 C 0.3039(6) 0.8576(8) 0.2470(4) 0.035(2) Uani 1 1 d . . . H15A H 0.3674 0.8593 0.2522 0.042 Uiso 1 1 calc R . . H15B H 0.2790 0.8950 0.2018 0.042 Uiso 1 1 calc R . . N4 N 0.2767(4) 0.9365(7) 0.3020(3) 0.0303(15) Uani 1 1 d . . . Re1 Re 0.17393(2) 0.53576(3) 0.468796(15) 0.02294(9) Uani 1 1 d . . . C16 C 0.1632(5) 0.6247(8) 0.5680(4) 0.0300(18) Uani 1 1 d . . . H16A H 0.1088 0.6530 0.5825 0.036 Uiso 1 1 calc R . . C17 C 0.2187(5) 0.7047(7) 0.5366(4) 0.0253(16) Uani 1 1 d . . . H17A H 0.2086 0.7987 0.5241 0.030 Uiso 1 1 calc R . . C18 C 0.2922(5) 0.6311(7) 0.5288(4) 0.0279(17) Uani 1 1 d . . . H18A H 0.3429 0.6636 0.5102 0.034 Uiso 1 1 calc R . . C19 C 0.2813(6) 0.5024(8) 0.5541(4) 0.0342(19) Uani 1 1 d . . . H19A H 0.3241 0.4298 0.5573 0.041 Uiso 1 1 calc R . . C20 C 0.2039(6) 0.4995(8) 0.5803(4) 0.036(2) Uani 1 1 d . . . H20A H 0.1826 0.4246 0.6047 0.043 Uiso 1 1 calc R . . C21 C 0.1566(6) 0.3561(8) 0.4055(4) 0.040(2) Uani 1 1 d . . . H21A H 0.1949 0.2776 0.4117 0.048 Uiso 1 1 calc R . . C22 C 0.0827(6) 0.3756(8) 0.4347(4) 0.035(2) Uani 1 1 d . . . H22A H 0.0602 0.3127 0.4655 0.042 Uiso 1 1 calc R . . C23 C 0.0440(5) 0.4941(8) 0.4118(4) 0.0332(18) Uani 1 1 d . . . H23A H -0.0110 0.5291 0.4224 0.040 Uiso 1 1 calc R . . C24 C 0.0917(5) 0.5482(8) 0.3643(4) 0.0314(18) Uani 1 1 d . . . H24A H 0.0770 0.6299 0.3372 0.038 Uiso 1 1 calc R . . C25 C 0.1620(6) 0.4632(8) 0.3602(4) 0.0338(19) Uani 1 1 d . . . H25A H 0.2054 0.4744 0.3300 0.041 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 U1 0.02119(15) 0.02348(14) 0.01732(14) 0.00176(11) 0.00241(10) -0.00137(11) N1 0.023(4) 0.028(3) 0.029(4) 0.005(3) 0.005(3) 0.004(3) Si1 0.0233(11) 0.0248(11) 0.0274(11) -0.0009(9) 0.0017(9) 0.0010(8) C1 0.024(4) 0.030(4) 0.034(5) 0.000(4) 0.004(3) 0.003(3) C2 0.037(5) 0.032(4) 0.043(5) 0.003(4) 0.005(4) 0.007(4) C3 0.029(5) 0.030(4) 0.037(5) -0.003(4) -0.002(4) -0.002(3) C4 0.035(5) 0.041(5) 0.027(4) 0.008(4) 0.003(4) 0.010(4) C5 0.045(5) 0.025(4) 0.034(5) 0.006(3) 0.012(4) 0.004(4) N2 0.025(4) 0.033(3) 0.022(3) 0.003(3) 0.002(3) -0.001(3) Si2 0.0244(12) 0.0285(11) 0.0302(12) -0.0046(9) 0.0028(9) -0.0034(9) C6 0.036(5) 0.038(5) 0.067(7) -0.017(5) 0.017(5) 0.000(4) C7 0.034(5) 0.046(5) 0.030(4) -0.006(4) 0.008(4) -0.016(4) C8 0.044(6) 0.025(4) 0.059(6) -0.003(4) 0.007(5) -0.002(4) C9 0.026(4) 0.045(5) 0.032(5) -0.003(4) 0.004(3) -0.007(4) C10 0.052(6) 0.048(5) 0.037(5) 0.006(4) 0.019(4) -0.009(5) N3 0.032(4) 0.032(4) 0.025(3) 0.001(3) 0.011(3) 0.000(3) Si3 0.0364(14) 0.0375(13) 0.0329(13) 0.0030(11) 0.0146(10) 0.0053(10) C11 0.060(7) 0.039(5) 0.079(8) -0.011(5) 0.027(6) 0.009(5) C12 0.051(6) 0.069(7) 0.042(6) 0.016(5) 0.016(5) 0.031(5) C13 0.036(5) 0.051(6) 0.059(6) 0.001(5) 0.021(5) -0.002(4) C14 0.040(5) 0.049(5) 0.021(4) 0.002(4) 0.011(4) 0.011(4) C15 0.041(5) 0.048(5) 0.019(4) 0.009(4) 0.014(4) 0.004(4) N4 0.033(4) 0.041(4) 0.018(3) 0.010(3) 0.007(3) 0.003(3) Re1 0.02665(17) 0.02222(16) 0.01956(15) 0.00055(11) 0.00332(11) -0.00354(12) C16 0.032(5) 0.040(5) 0.019(4) -0.002(3) 0.008(3) -0.004(4) C17 0.034(5) 0.025(4) 0.017(4) -0.004(3) 0.006(3) -0.003(3) C18 0.027(4) 0.029(4) 0.026(4) 0.000(3) -0.001(3) -0.002(3) C19 0.041(5) 0.033(4) 0.027(4) -0.005(4) 0.001(4) 0.002(4) C20 0.059(6) 0.033(4) 0.017(4) 0.008(3) 0.007(4) -0.004(4) C21 0.046(6) 0.028(4) 0.042(5) -0.009(4) -0.001(4) -0.005(4) C22 0.051(6) 0.031(4) 0.023(4) -0.002(3) 0.004(4) -0.009(4) C23 0.027(4) 0.036(5) 0.035(5) 0.000(4) -0.001(3) -0.003(4) C24 0.032(5) 0.032(4) 0.026(4) -0.004(3) -0.007(3) -0.011(3) C25 0.041(5) 0.037(5) 0.023(4) -0.010(4) 0.003(4) -0.007(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 U1 N3 2.241(6) . ? U1 N2 2.274(6) . ? U1 N1 2.282(6) . ? U1 N4 2.680(6) . ? U1 C14 3.007(7) . ? U1 C17 3.023(7) . ? U1 C9 3.040(8) . ? U1 Re1 3.0475(4) . ? N1 C4 1.485(9) . ? N1 Si1 1.732(6) . ? Si1 C1 1.866(8) . ? Si1 C2 1.867(8) . ? Si1 C3 1.876(8) . ? C4 C5 1.539(11) . ? C5 N4 1.498(10) . ? N2 C9 1.491(9) . ? N2 Si2 1.726(7) . ? Si2 C7 1.873(9) . ? Si2 C8 1.877(8) . ? Si2 C6 1.889(8) . ? C9 C10 1.515(12) . ? C10 N4 1.508(11) . ? N3 C14 1.473(10) . ? N3 Si3 1.739(7) . ? Si3 C12 1.858(9) . ? Si3 C13 1.874(8) . ? Si3 C11 1.884(10) . ? C14 C15 1.521(12) . ? C15 N4 1.487(9) . ? Re1 C19 2.192(9) . ? Re1 C23 2.195(8) . ? Re1 C22 2.207(8) . ? Re1 C16 2.210(7) . ? Re1 C20 2.214(8) . ? Re1 C21 2.219(8) . ? Re1 C17 2.228(7) . ? Re1 C24 2.242(8) . ? Re1 C18 2.246(8) . ? Re1 C25 2.260(8) . ? C16 C17 1.427(10) . ? C16 C20 1.436(11) . ? C17 C18 1.419(10) . ? C18 C19 1.434(11) . ? C19 C20 1.417(11) . ? C21 C22 1.413(12) . ? C21 C25 1.432(11) . ? C22 C23 1.397(11) . ? C23 C24 1.426(11) . ? C24 C25 1.426(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 N3 U1 N2 105.4(2) . . ? N3 U1 N1 112.6(2) . . ? N2 U1 N1 107.1(2) . . ? N3 U1 N4 69.5(2) . . ? N2 U1 N4 69.6(2) . . ? N1 U1 N4 69.4(2) . . ? N3 U1 C14 28.1(2) . . ? N2 U1 C14 109.9(2) . . ? N1 U1 C14 85.2(2) . . ? N4 U1 C14 50.8(2) . . ? N3 U1 C17 129.6(2) . . ? N2 U1 C17 78.5(2) . . ? N1 U1 C17 113.8(2) . . ? N4 U1 C17 146.9(2) . . ? C14 U1 C17 156.6(2) . . ? N3 U1 C9 78.8(2) . . ? N2 U1 C9 28.2(2) . . ? N1 U1 C9 109.8(2) . . ? N4 U1 C9 50.0(2) . . ? C14 U1 C9 82.1(2) . . ? C17 U1 C9 102.5(2) . . ? N3 U1 Re1 101.83(16) . . ? N2 U1 Re1 119.06(15) . . ? N1 U1 Re1 110.72(15) . . ? N4 U1 Re1 169.74(14) . . ? C14 U1 Re1 119.08(17) . . ? C17 U1 Re1 43.07(14) . . ? C9 U1 Re1 135.38(16) . . ? C4 N1 Si1 113.1(5) . . ? C4 N1 U1 117.9(5) . . ? Si1 N1 U1 128.9(3) . . ? N1 Si1 C1 109.6(3) . . ? N1 Si1 C2 112.9(3) . . ? C1 Si1 C2 108.0(4) . . ? N1 Si1 C3 112.3(3) . . ? C1 Si1 C3 107.6(4) . . ? C2 Si1 C3 106.2(4) . . ? N1 C4 C5 109.8(7) . . ? N4 C5 C4 107.8(6) . . ? C9 N2 Si2 114.0(5) . . ? C9 N2 U1 105.8(5) . . ? Si2 N2 U1 140.1(3) . . ? N2 Si2 C7 112.1(4) . . ? N2 Si2 C8 112.2(4) . . ? C7 Si2 C8 106.8(4) . . ? N2 Si2 C6 111.4(4) . . ? C7 Si2 C6 108.5(4) . . ? C8 Si2 C6 105.6(4) . . ? N2 C9 C10 109.9(7) . . ? N2 C9 U1 46.0(3) . . ? C10 C9 U1 91.9(5) . . ? N4 C10 C9 107.5(6) . . ? C14 N3 Si3 115.9(5) . . ? C14 N3 U1 106.3(5) . . ? Si3 N3 U1 137.7(4) . . ? N3 Si3 C12 109.3(4) . . ? N3 Si3 C13 111.8(4) . . ? C12 Si3 C13 107.8(5) . . ? N3 Si3 C11 111.0(4) . . ? C12 Si3 C11 109.0(5) . . ? C13 Si3 C11 107.8(4) . . ? N3 C14 C15 109.7(7) . . ? N3 C14 U1 45.7(3) . . ? C15 C14 U1 91.6(4) . . ? N4 C15 C14 109.4(6) . . ? C15 N4 C5 111.9(6) . . ? C15 N4 C10 111.8(6) . . ? C5 N4 C10 111.1(7) . . ? C15 N4 U1 106.2(4) . . ? C5 N4 U1 108.3(4) . . ? C10 N4 U1 107.2(4) . . ? C19 Re1 C23 152.2(3) . . ? C19 Re1 C22 119.3(3) . . ? C23 Re1 C22 37.0(3) . . ? C19 Re1 C16 63.2(3) . . ? C23 Re1 C16 108.8(3) . . ? C22 Re1 C16 115.3(3) . . ? C19 Re1 C20 37.5(3) . . ? C23 Re1 C20 119.4(3) . . ? C22 Re1 C20 100.9(3) . . ? C16 Re1 C20 37.9(3) . . ? C19 Re1 C21 107.8(3) . . ? C23 Re1 C21 62.6(3) . . ? C22 Re1 C21 37.2(3) . . ? C16 Re1 C21 145.9(3) . . ? C20 Re1 C21 114.3(3) . . ? C19 Re1 C17 62.6(3) . . ? C23 Re1 C17 128.7(3) . . ? C22 Re1 C17 151.6(3) . . ? C16 Re1 C17 37.5(3) . . ? C20 Re1 C17 62.5(3) . . ? C21 Re1 C17 168.7(3) . . ? C19 Re1 C24 163.5(3) . . ? C23 Re1 C24 37.5(3) . . ? C22 Re1 C24 61.6(3) . . ? C16 Re1 C24 132.7(3) . . ? C20 Re1 C24 156.8(3) . . ? C21 Re1 C24 62.0(3) . . ? C17 Re1 C24 125.6(3) . . ? C19 Re1 C18 37.7(3) . . ? C23 Re1 C18 164.9(3) . . ? C22 Re1 C18 156.7(3) . . ? C16 Re1 C18 62.6(3) . . ? C20 Re1 C18 62.5(3) . . ? C21 Re1 C18 131.7(3) . . ? C17 Re1 C18 37.0(3) . . ? C24 Re1 C18 138.6(3) . . ? C19 Re1 C25 127.2(3) . . ? C23 Re1 C25 62.5(3) . . ? C22 Re1 C25 61.8(3) . . ? C16 Re1 C25 169.6(3) . . ? C20 Re1 C25 150.2(3) . . ? C21 Re1 C25 37.3(3) . . ? C17 Re1 C25 142.7(3) . . ? C24 Re1 C25 36.9(3) . . ? C18 Re1 C25 124.4(3) . . ? C19 Re1 U1 105.3(2) . . ? C23 Re1 U1 102.4(2) . . ? C22 Re1 U1 130.5(2) . . ? C16 Re1 U1 102.7(2) . . ? C20 Re1 U1 128.2(2) . . ? C21 Re1 U1 111.3(2) . . ? C17 Re1 U1 67.88(18) . . ? C24 Re1 U1 69.5(2) . . ? C18 Re1 U1 69.37(19) . . ? C25 Re1 U1 75.0(2) . . ? C17 C16 C20 107.2(7) . . ? C17 C16 Re1 71.9(4) . . ? C20 C16 Re1 71.2(4) . . ? C18 C17 C16 109.0(7) . . ? C18 C17 Re1 72.2(4) . . ? C16 C17 Re1 70.5(4) . . ? C18 C17 U1 79.0(4) . . ? C16 C17 U1 133.7(5) . . ? Re1 C17 U1 69.06(18) . . ? C17 C18 C19 107.2(7) . . ? C17 C18 Re1 70.8(4) . . ? C19 C18 Re1 69.1(5) . . ? C20 C19 C18 108.5(7) . . ? C20 C19 Re1 72.1(5) . . ? C18 C19 Re1 73.2(5) . . ? C19 C20 C16 108.0(7) . . ? C19 C20 Re1 70.4(4) . . ? C16 C20 Re1 70.9(4) . . ? C22 C21 C25 107.5(8) . . ? C22 C21 Re1 70.9(5) . . ? C25 C21 Re1 72.9(4) . . ? C23 C22 C21 109.5(7) . . ? C23 C22 Re1 71.0(5) . . ? C21 C22 Re1 71.8(5) . . ? C22 C23 C24 107.5(7) . . ? C22 C23 Re1 72.0(5) . . ? C24 C23 Re1 73.1(5) . . ? C25 C24 C23 108.3(7) . . ? C25 C24 Re1 72.2(5) . . ? C23 C24 Re1 69.5(5) . . ? C24 C25 C21 107.1(7) . . ? C24 C25 Re1 70.8(4) . . ? C21 C25 Re1 69.8(4) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.675 _refine_diff_density_min -1.293 _refine_diff_density_rms 0.210