Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_reox1 _database_code_CSD 158606 _journal_coden_Cambridge 186 loop_ _publ_author_name 'Anulewicz-Ostrowska, Romana' 'Czerwieniec, Rafal' 'Kapturkiewicz, Andrzej' 'Nowacki, Jacek' _publ_contact_author_name 'Andrzej Kapturkiewicz' _publ_contact_author_addres ; Institute of Physical Chemistry, Polish Academy of Sciences, 01-224 Warsaw, Kasprzaka 44/52, Poland ; _publ_contact_author_email 'akaptur@ichf.edu.pl' _publ_requestet_journal 'J.Chem.Soc. Dalton Transactions' _publ_section_title ; Monomeric and dimeric Re(I)(tricarbonyl)(8-Quinolinato) complexes ; _audit_creation_method SHELXL _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C17 H11 N2 O4 Re' _chemical_formula_weight 493.48 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.0890(10) _cell_length_b 9.418(2) _cell_length_c 12.493(2) _cell_angle_alpha 87.77(3) _cell_angle_beta 82.66(3) _cell_angle_gamma 75.22(3) _cell_volume 799.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.049 _exptl_crystal_density_method ? _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 7.619 _exptl_absorpt_correction_type NUMERICAL _exptl_absorpt_correction_T_min 0.0679 _exptl_absorpt_correction_T_max 0.2189 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3884 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0132 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 28.72 _reflns_number_total 3884 _reflns_number_observed 3575 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+1.3804P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0065(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3884 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0277 _refine_ls_R_factor_obs 0.0248 _refine_ls_wR_factor_all 0.0622 _refine_ls_wR_factor_obs 0.0595 _refine_ls_goodness_of_fit_all 1.152 _refine_ls_goodness_of_fit_obs 1.152 _refine_ls_restrained_S_all 1.152 _refine_ls_restrained_S_obs 1.152 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re1 Re 0.33201(2) 0.69096(2) 0.748338(12) 0.03471(7) Uani 1 d . . N1 N 0.5090(4) 0.8342(4) 0.6768(2) 0.0309(6) Uani 1 d . . C1 C 0.6981(6) 0.8032(5) 0.6412(4) 0.0422(9) Uani 1 d . . H1 H 0.7711(6) 0.7063(5) 0.6446(4) 0.066(17) Uiso 1 calc R . C2 C 0.7941(6) 0.9087(6) 0.5987(4) 0.0476(10) Uani 1 d . . H2 H 0.9286(6) 0.8822(6) 0.5766(4) 0.049(14) Uiso 1 calc R . C3 C 0.6910(7) 1.0491(5) 0.5899(3) 0.0449(10) Uani 1 d . . H3 H 0.7540(7) 1.1197(5) 0.5607(3) 0.055(15) Uiso 1 calc R . C4 C 0.4881(6) 1.0893(4) 0.6248(3) 0.0354(8) Uani 1 d . . C5 C 0.3665(7) 1.2327(5) 0.6187(4) 0.0449(10) Uani 1 d . . H5 H 0.4187(7) 1.3083(5) 0.5885(4) 0.059(16) Uiso 1 calc R . C6 C 0.1730(8) 1.2600(5) 0.6572(4) 0.0475(10) Uani 1 d . . H6 H 0.0941(8) 1.3550(5) 0.6524(4) 0.064(17) Uiso 1 calc R . C7 C 0.0883(7) 1.1495(5) 0.7038(4) 0.0422(9) Uani 1 d . . H7 H -0.0446(7) 1.1723(5) 0.7300(4) 0.056(15) Uiso 1 calc R . C8 C 0.2010(5) 1.0067(4) 0.7111(3) 0.0313(7) Uani 1 d . . C9 C 0.4024(5) 0.9773(4) 0.6700(3) 0.0291(7) Uani 1 d . . O1 O 0.1303(4) 0.8978(3) 0.7543(2) 0.0354(6) Uani 1 d . . N2 N 0.3982(5) 0.7629(4) 0.9020(3) 0.0379(7) Uani 1 d . . C10 C 0.2609(8) 0.8492(6) 0.9707(4) 0.0538(12) Uani 1 d . . H10 H 0.1341(8) 0.8812(6) 0.9518(4) 0.070(18) Uiso 1 calc R . C11 C 0.2973(11) 0.8932(7) 1.0679(4) 0.071(2) Uani 1 d . . H11 H 0.1974(11) 0.9537(7) 1.1134(4) 0.103(26) Uiso 1 calc R . C12 C 0.4830(13) 0.8465(8) 1.0966(5) 0.079(2) Uani 1 d . . H12 H 0.5114(13) 0.8744(8) 1.1621(5) 0.062(16) Uiso 1 calc R . C13 C 0.6252(11) 0.7590(7) 1.0283(5) 0.073(2) Uani 1 d . . H13 H 0.7525(11) 0.7263(7) 1.0463(5) 0.089(23) Uiso 1 calc R . C14 C 0.5797(8) 0.7191(6) 0.9322(4) 0.0552(12) Uani 1 d . . H14 H 0.6786(8) 0.6591(6) 0.8859(4) 0.066(18) Uiso 1 calc R . C15 C 0.1528(6) 0.5859(5) 0.8200(4) 0.0442(9) Uani 1 d . . O15 O 0.0418(6) 0.5270(5) 0.8623(4) 0.0702(11) Uani 1 d . . C16 C 0.2733(6) 0.6342(4) 0.6135(4) 0.0397(9) Uani 1 d . . O16 O 0.2372(7) 0.6000(4) 0.5341(3) 0.0640(10) Uani 1 d . . C17 C 0.5368(6) 0.5127(5) 0.7452(3) 0.0394(8) Uani 1 d . . O17 O 0.6645(6) 0.4084(4) 0.7404(4) 0.0707(11) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.03113(10) 0.02959(9) 0.04082(10) 0.00090(6) -0.00520(6) -0.00273(6) N1 0.0258(14) 0.036(2) 0.0308(14) -0.0005(12) -0.0066(11) -0.0056(12) C1 0.033(2) 0.047(2) 0.043(2) 0.002(2) -0.005(2) -0.003(2) C2 0.029(2) 0.065(3) 0.049(2) 0.005(2) -0.004(2) -0.014(2) C3 0.047(2) 0.055(3) 0.039(2) 0.002(2) -0.007(2) -0.025(2) C4 0.046(2) 0.035(2) 0.030(2) -0.0014(14) -0.010(2) -0.015(2) C5 0.061(3) 0.031(2) 0.046(2) 0.002(2) -0.010(2) -0.017(2) C6 0.060(3) 0.026(2) 0.052(2) 0.002(2) -0.005(2) -0.004(2) C7 0.040(2) 0.032(2) 0.049(2) 0.000(2) -0.003(2) 0.000(2) C8 0.031(2) 0.029(2) 0.032(2) -0.0015(13) -0.0052(14) -0.0046(14) C9 0.033(2) 0.029(2) 0.026(2) -0.0022(13) -0.0093(13) -0.0069(14) O1 0.0274(12) 0.0293(13) 0.0458(15) 0.0027(11) -0.0014(11) -0.0020(10) N2 0.037(2) 0.039(2) 0.035(2) 0.0024(13) -0.0046(13) -0.0056(14) C10 0.054(3) 0.059(3) 0.042(2) -0.003(2) 0.005(2) -0.006(2) C11 0.101(5) 0.073(4) 0.036(2) -0.007(2) 0.009(3) -0.025(4) C12 0.130(6) 0.080(4) 0.036(3) 0.004(3) -0.021(3) -0.040(4) C13 0.088(4) 0.078(4) 0.059(3) 0.009(3) -0.042(3) -0.019(3) C14 0.055(3) 0.056(3) 0.053(3) -0.002(2) -0.019(2) -0.004(2) C15 0.035(2) 0.040(2) 0.053(2) 0.002(2) -0.007(2) -0.002(2) O15 0.056(2) 0.068(3) 0.087(3) 0.013(2) 0.010(2) -0.028(2) C16 0.039(2) 0.026(2) 0.052(2) 0.007(2) -0.009(2) -0.005(2) O16 0.090(3) 0.055(2) 0.055(2) -0.002(2) -0.029(2) -0.024(2) C17 0.035(2) 0.038(2) 0.043(2) 0.000(2) -0.004(2) -0.005(2) O17 0.059(2) 0.034(2) 0.105(3) -0.005(2) -0.009(2) 0.014(2) _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 C16 1.913(5) . ? Re1 C15 1.917(5) . ? Re1 C17 1.917(4) . ? Re1 O1 2.099(3) . ? Re1 N1 2.162(3) . ? Re1 N2 2.204(4) . ? N1 C1 1.319(5) . ? N1 C9 1.373(5) . ? C1 C2 1.394(7) . ? C1 H1 0.93 . ? C2 C3 1.346(7) . ? C2 H2 0.93 . ? C3 C4 1.406(6) . ? C3 H3 0.93 . ? C4 C5 1.410(6) . ? C4 C9 1.411(5) . ? C5 C6 1.356(7) . ? C5 H5 0.93 . ? C6 C7 1.402(6) . ? C6 H6 0.93 . ? C7 C8 1.384(5) . ? C7 H7 0.93 . ? C8 O1 1.321(5) . ? C8 C9 1.415(5) . ? N2 C10 1.335(6) . ? N2 C14 1.345(6) . ? C10 C11 1.374(8) . ? C10 H10 0.93 . ? C11 C12 1.367(10) . ? C11 H11 0.93 . ? C12 C13 1.354(10) . ? C12 H12 0.93 . ? C13 C14 1.372(7) . ? C13 H13 0.93 . ? C14 H14 0.93 . ? C15 O15 1.140(6) . ? C16 O16 1.134(6) . ? C17 O17 1.151(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 Re1 C15 88.4(2) . . ? C16 Re1 C17 87.8(2) . . ? C15 Re1 C17 88.8(2) . . ? C16 Re1 O1 95.83(15) . . ? C15 Re1 O1 96.06(15) . . ? C17 Re1 O1 173.97(14) . . ? C16 Re1 N1 94.77(15) . . ? C15 Re1 N1 172.7(2) . . ? C17 Re1 N1 97.8(2) . . ? O1 Re1 N1 77.15(11) . . ? C16 Re1 N2 178.36(14) . . ? C15 Re1 N2 92.6(2) . . ? C17 Re1 N2 93.5(2) . . ? O1 Re1 N2 82.82(12) . . ? N1 Re1 N2 84.02(12) . . ? C1 N1 C9 117.8(3) . . ? C1 N1 Re1 129.6(3) . . ? C9 N1 Re1 112.6(2) . . ? N1 C1 C2 123.2(4) . . ? N1 C1 H1 118.4(3) . . ? C2 C1 H1 118.4(3) . . ? C3 C2 C1 119.6(4) . . ? C3 C2 H2 120.2(3) . . ? C1 C2 H2 120.2(3) . . ? C2 C3 C4 120.0(4) . . ? C2 C3 H3 120.0(3) . . ? C4 C3 H3 120.0(3) . . ? C3 C4 C5 124.6(4) . . ? C3 C4 C9 117.1(4) . . ? C5 C4 C9 118.3(4) . . ? C6 C5 C4 119.7(4) . . ? C6 C5 H5 120.1(3) . . ? C4 C5 H5 120.1(3) . . ? C5 C6 C7 122.0(4) . . ? C5 C6 H6 119.0(3) . . ? C7 C6 H6 119.0(3) . . ? C8 C7 C6 120.5(4) . . ? C8 C7 H7 119.7(2) . . ? C6 C7 H7 119.7(3) . . ? O1 C8 C7 123.5(4) . . ? O1 C8 C9 118.8(3) . . ? C7 C8 C9 117.7(4) . . ? N1 C9 C4 122.2(3) . . ? N1 C9 C8 116.1(3) . . ? C4 C9 C8 121.7(3) . . ? C8 O1 Re1 115.2(2) . . ? C10 N2 C14 116.5(4) . . ? C10 N2 Re1 122.2(3) . . ? C14 N2 Re1 121.3(3) . . ? N2 C10 C11 123.3(6) . . ? N2 C10 H10 118.3(3) . . ? C11 C10 H10 118.3(4) . . ? C12 C11 C10 118.8(6) . . ? C12 C11 H11 120.6(4) . . ? C10 C11 H11 120.6(4) . . ? C13 C12 C11 119.1(5) . . ? C13 C12 H12 120.5(4) . . ? C11 C12 H12 120.5(4) . . ? C12 C13 C14 119.4(6) . . ? C12 C13 H13 120.3(4) . . ? C14 C13 H13 120.3(4) . . ? N2 C14 C13 122.9(5) . . ? N2 C14 H14 118.6(3) . . ? C13 C14 H14 118.6(4) . . ? O15 C15 Re1 178.0(4) . . ? O16 C16 Re1 179.3(4) . . ? O17 C17 Re1 177.2(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 Re1 N1 C1 -87.3(4) . . . . ? C15 Re1 N1 C1 156.7(11) . . . . ? C17 Re1 N1 C1 1.2(4) . . . . ? O1 Re1 N1 C1 177.8(4) . . . . ? N2 Re1 N1 C1 93.9(4) . . . . ? C16 Re1 N1 C9 93.3(3) . . . . ? C15 Re1 N1 C9 -22.8(13) . . . . ? C17 Re1 N1 C9 -178.3(3) . . . . ? O1 Re1 N1 C9 -1.6(2) . . . . ? N2 Re1 N1 C9 -85.6(2) . . . . ? C9 N1 C1 C2 0.9(6) . . . . ? Re1 N1 C1 C2 -178.6(3) . . . . ? N1 C1 C2 C3 -2.0(7) . . . . ? C1 C2 C3 C4 0.9(7) . . . . ? C2 C3 C4 C5 -179.7(4) . . . . ? C2 C3 C4 C9 1.0(6) . . . . ? C3 C4 C5 C6 -178.5(4) . . . . ? C9 C4 C5 C6 0.9(6) . . . . ? C4 C5 C6 C7 0.3(7) . . . . ? C5 C6 C7 C8 -0.7(7) . . . . ? C6 C7 C8 O1 179.9(4) . . . . ? C6 C7 C8 C9 -0.1(6) . . . . ? C1 N1 C9 C4 1.2(5) . . . . ? Re1 N1 C9 C4 -179.3(3) . . . . ? C1 N1 C9 C8 -178.7(3) . . . . ? Re1 N1 C9 C8 0.9(4) . . . . ? C3 C4 C9 N1 -2.1(5) . . . . ? C5 C4 C9 N1 178.5(3) . . . . ? C3 C4 C9 C8 177.7(3) . . . . ? C5 C4 C9 C8 -1.6(5) . . . . ? O1 C8 C9 N1 1.1(5) . . . . ? C7 C8 C9 N1 -178.9(3) . . . . ? O1 C8 C9 C4 -178.7(3) . . . . ? C7 C8 C9 C4 1.2(5) . . . . ? C7 C8 O1 Re1 177.4(3) . . . . ? C9 C8 O1 Re1 -2.6(4) . . . . ? C16 Re1 O1 C8 -91.3(3) . . . . ? C15 Re1 O1 C8 179.7(3) . . . . ? C17 Re1 O1 C8 35.5(14) . . . . ? N1 Re1 O1 C8 2.3(2) . . . . ? N2 Re1 O1 C8 87.8(3) . . . . ? C16 Re1 N2 C10 68.0(53) . . . . ? C15 Re1 N2 C10 -62.8(4) . . . . ? C17 Re1 N2 C10 -151.8(4) . . . . ? O1 Re1 N2 C10 33.0(4) . . . . ? N1 Re1 N2 C10 110.7(4) . . . . ? C16 Re1 N2 C14 -113.3(52) . . . . ? C15 Re1 N2 C14 115.9(4) . . . . ? C17 Re1 N2 C14 26.9(4) . . . . ? O1 Re1 N2 C14 -148.3(4) . . . . ? N1 Re1 N2 C14 -70.6(4) . . . . ? C14 N2 C10 C11 -0.1(8) . . . . ? Re1 N2 C10 C11 178.7(4) . . . . ? N2 C10 C11 C12 -0.1(9) . . . . ? C10 C11 C12 C13 0.3(10) . . . . ? C11 C12 C13 C14 -0.1(10) . . . . ? C10 N2 C14 C13 0.2(8) . . . . ? Re1 N2 C14 C13 -178.5(5) . . . . ? C12 C13 C14 N2 -0.1(10) . . . . ? C16 Re1 C15 O15 -85.2(130) . . . . ? C17 Re1 C15 O15 -173.0(130) . . . . ? O1 Re1 C15 O15 10.5(130) . . . . ? N1 Re1 C15 O15 31.2(138) . . . . ? N2 Re1 C15 O15 93.6(130) . . . . ? C15 Re1 C16 O16 3.1(310) . . . . ? C17 Re1 C16 O16 92.0(310) . . . . ? O1 Re1 C16 O16 -92.8(310) . . . . ? N1 Re1 C16 O16 -170.3(310) . . . . ? N2 Re1 C16 O16 -127.7(294) . . . . ? C16 Re1 C17 O17 80.5(86) . . . . ? C15 Re1 C17 O17 169.0(86) . . . . ? O1 Re1 C17 O17 -46.6(92) . . . . ? N1 Re1 C17 O17 -14.0(86) . . . . ? N2 Re1 C17 O17 -98.4(86) . . . . ? _refine_diff_density_max 0.711 _refine_diff_density_min -1.083 _refine_diff_density_rms 0.112 data_reox2 _database_code_CSD 158607 _journal_coden_Cambridge 186 loop_ _publ_author_name 'Anulewicz-Ostrowska, Romana' 'Czerwieniec, Rafal' 'Kapturkiewicz, Andrzej' 'Nowacki, Jacek' _publ_contact_author_name 'Andrzej Kapturkiewicz' _publ_contact_author_addres ; Institute of Physical Chemistry, Polish Academy of Sciences, 01-224 Warsaw, Kasprzaka 44/52, Poland ; _publ_contact_author_email 'akaptur@ichf.edu.pl' _publ_requestet_journal 'J.Chem.Soc. Dalton Transactions' _publ_section_title ; Monomeric and dimeric Re(I)(tricarbonyl)(8-Quinolinato) complexes ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H12 N2 O8 Re2' _chemical_formula_weight 829.97 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting OTHORHOMBIC _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.785(2) _cell_length_b 14.327(3) _cell_length_c 16.454(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2306.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.67 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.386 _exptl_crystal_density_method ? _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 10.540 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.3151 _exptl_absorpt_correction_T_max 0.6476 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5546 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0532 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 28.80 _reflns_number_total 5546 _reflns_number_observed 4592 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _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 0.00 _refine_ls_number_reflns 5541 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_obs 0.0403 _refine_ls_wR_factor_all 0.0917 _refine_ls_wR_factor_obs 0.0826 _refine_ls_goodness_of_fit_all 1.058 _refine_ls_goodness_of_fit_obs 1.066 _refine_ls_restrained_S_all 1.071 _refine_ls_restrained_S_obs 1.066 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re1 Re 1.01598(4) 0.02306(3) 0.83034(2) 0.03049(10) Uani 1 d . . Re2 Re 0.73850(4) 0.12785(3) 0.74403(2) 0.03165(11) Uani 1 d . . O1 O 0.9576(6) 0.1447(4) 0.7556(4) 0.0297(14) Uani 1 d . . O2 O 0.8128(7) -0.0089(5) 0.7866(4) 0.036(2) Uani 1 d . . C111 C 0.9760(12) 0.0817(8) 0.9306(7) 0.040(3) Uani 1 d . . O111 O 0.9611(11) 0.1148(6) 0.9941(5) 0.061(2) Uani 1 d . . C221 C 1.0413(12) -0.0877(9) 0.8913(7) 0.044(3) Uani 1 d . . O221 O 1.0557(10) -0.1533(6) 0.9304(6) 0.063(3) Uani 1 d . . C331 C 1.2020(11) 0.0506(8) 0.8556(8) 0.039(3) Uani 1 d . . O331 O 1.3120(9) 0.0669(7) 0.8704(6) 0.061(3) Uani 1 d . . C112 C 0.6763(10) 0.1588(8) 0.8505(7) 0.037(3) Uani 1 d . . O112 O 0.6361(10) 0.1810(8) 0.9129(5) 0.065(3) Uani 1 d . . C222 C 0.6873(11) 0.2501(9) 0.7108(8) 0.043(3) Uani 1 d . . O222 O 0.6554(10) 0.3240(6) 0.6936(6) 0.064(3) Uani 1 d . . C332 C 0.5565(12) 0.0887(8) 0.7172(8) 0.043(3) Uani 1 d . . O332 O 0.4503(8) 0.0654(9) 0.7014(7) 0.087(4) Uani 1 d . . N11 N 1.0493(8) -0.0504(6) 0.7159(5) 0.030(2) Uani 1 d . . C11 C 1.1648(10) -0.0619(8) 0.6761(7) 0.037(2) Uani 1 d . . H11 H 1.2424(10) -0.0311(8) 0.6947(7) 0.001(17) Uiso 1 calc R . C21 C 1.1758(14) -0.1192(9) 0.6060(7) 0.051(3) Uani 1 d . . H21 H 1.2575(14) -0.1248(9) 0.5775(7) 0.044(31) Uiso 1 calc R . C31 C 1.0611(14) -0.1657(8) 0.5826(8) 0.050(3) Uani 1 d . . H31 H 1.0652(14) -0.2037(8) 0.5369(8) 0.012(22) Uiso 1 calc R . C41 C 0.9380(13) -0.1585(8) 0.6243(7) 0.040(3) Uani 1 d . . C51 C 0.8188(13) -0.2076(9) 0.6030(8) 0.046(3) Uani 1 d . . H51 H 0.8200(13) -0.2513(9) 0.5612(8) 0.076(48) Uiso 1 calc R . C61 C 0.7009(13) -0.1896(8) 0.6450(8) 0.051(4) Uani 1 d . . H61 H 0.6217(13) -0.2214(8) 0.6307(8) 0.068(44) Uiso 1 calc R . C71 C 0.6954(11) -0.1256(8) 0.7083(7) 0.040(3) Uani 1 d . . H71 H 0.6142(11) -0.1154(8) 0.7363(7) 0.008(20) Uiso 1 calc R . C81 C 0.8126(12) -0.0772(7) 0.7289(6) 0.033(2) Uani 1 d . . C91 C 0.9370(11) -0.0968(7) 0.6891(6) 0.034(2) Uani 1 d . . N12 N 0.8203(9) 0.0980(6) 0.6230(5) 0.030(2) Uani 1 d . . C12 C 0.7505(13) 0.0682(7) 0.5586(6) 0.038(2) Uani 1 d . . H12 H 0.6602(13) 0.0493(7) 0.5648(6) 0.181(99) Uiso 1 calc R . C22 C 0.8114(12) 0.0651(9) 0.4809(7) 0.047(3) Uani 1 d . . H22 H 0.7614(12) 0.0434(9) 0.4367(7) 0.032(27) Uiso 1 calc R . C32 C 0.9410(13) 0.0932(9) 0.4704(7) 0.045(3) Uani 1 d . . H32 H 0.9805(13) 0.0915(9) 0.4190(7) 0.021(24) Uiso 1 calc R . C42 C 1.0163(12) 0.1249(8) 0.5371(7) 0.042(3) Uani 1 d . . C52 C 1.1503(13) 0.1575(10) 0.5324(8) 0.052(3) Uani 1 d . . H52 H 1.1938(13) 0.1598(10) 0.4822(8) 0.107(63) Uiso 1 calc R . C62 C 1.2200(13) 0.1866(9) 0.6014(8) 0.052(3) Uani 1 d . . H62 H 1.3096(13) 0.2078(9) 0.5974(8) 0.091(55) Uiso 1 calc R . C72 C 1.1544(12) 0.1839(9) 0.6773(8) 0.046(3) Uani 1 d . . H82 H 1.2012(12) 0.2034(9) 0.7235(8) 0.017(25) Uiso 1 calc R . C82 C 1.0223(9) 0.1529(6) 0.6843(5) 0.025(2) Uani 1 d . . C92 C 0.9510(10) 0.1252(8) 0.6130(6) 0.032(2) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0277(2) 0.0349(2) 0.0289(2) -0.0010(2) -0.0025(2) -0.0014(2) Re2 0.0252(2) 0.0385(2) 0.0313(2) 0.0000(2) 0.0010(2) 0.0019(2) O1 0.024(3) 0.037(4) 0.028(3) 0.004(3) -0.003(3) 0.000(3) O2 0.023(3) 0.041(5) 0.044(4) 0.005(3) 0.002(3) 0.001(3) C111 0.042(6) 0.045(6) 0.032(6) 0.003(5) 0.000(5) 0.003(5) O111 0.077(7) 0.066(6) 0.040(5) -0.017(5) 0.008(5) 0.000(5) C221 0.041(7) 0.060(8) 0.031(6) -0.010(6) -0.006(5) -0.003(6) O221 0.066(6) 0.049(5) 0.074(7) 0.033(5) -0.020(5) -0.002(4) C331 0.030(6) 0.031(6) 0.056(8) -0.004(5) -0.005(5) 0.001(4) O331 0.041(5) 0.061(6) 0.080(7) -0.013(5) -0.012(5) -0.006(4) C112 0.026(5) 0.048(7) 0.038(7) 0.000(5) 0.010(4) 0.009(5) O112 0.066(6) 0.094(8) 0.035(5) -0.007(5) 0.014(5) 0.004(6) C222 0.031(6) 0.048(7) 0.049(7) 0.003(6) 0.006(5) 0.009(5) O222 0.078(7) 0.048(6) 0.066(7) 0.010(5) -0.009(5) 0.019(5) C332 0.040(7) 0.037(6) 0.052(7) 0.002(5) -0.015(5) 0.007(5) O332 0.018(4) 0.137(10) 0.106(8) 0.053(8) -0.013(5) -0.020(5) N11 0.031(5) 0.027(4) 0.033(5) -0.002(3) -0.006(4) -0.003(3) C11 0.029(5) 0.036(6) 0.047(7) -0.006(6) -0.005(5) 0.007(4) C21 0.058(8) 0.061(8) 0.035(6) -0.009(6) 0.003(6) 0.020(7) C31 0.071(9) 0.032(6) 0.046(8) -0.012(6) 0.006(7) -0.006(6) C41 0.051(7) 0.037(6) 0.031(6) 0.005(5) -0.007(5) -0.004(5) C51 0.049(7) 0.039(7) 0.051(8) 0.001(6) -0.007(6) 0.008(6) C61 0.051(8) 0.036(6) 0.067(9) 0.003(6) -0.028(7) -0.014(5) C71 0.034(6) 0.043(6) 0.044(6) 0.007(6) 0.002(5) -0.008(5) C81 0.055(7) 0.026(5) 0.018(5) -0.004(4) -0.001(4) -0.001(5) C91 0.037(6) 0.029(5) 0.035(6) -0.001(4) -0.003(5) 0.001(4) N12 0.032(4) 0.036(5) 0.022(4) 0.006(4) -0.002(3) -0.003(4) C12 0.041(6) 0.041(6) 0.033(5) -0.007(4) 0.004(5) -0.001(6) C22 0.050(7) 0.061(8) 0.029(6) -0.005(6) -0.017(5) 0.001(6) C32 0.049(7) 0.058(8) 0.028(6) -0.011(5) 0.001(5) 0.006(6) C42 0.042(6) 0.045(6) 0.038(6) 0.001(5) 0.003(5) 0.008(6) C52 0.041(7) 0.069(9) 0.045(8) 0.003(6) 0.014(6) -0.007(6) C62 0.038(7) 0.059(8) 0.060(8) 0.006(7) 0.007(6) -0.005(6) C72 0.042(6) 0.049(7) 0.047(7) 0.007(6) -0.004(6) -0.009(5) C82 0.022(4) 0.024(4) 0.030(5) 0.010(4) 0.000(4) 0.003(4) C92 0.027(5) 0.038(6) 0.030(5) 0.004(5) 0.003(4) 0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C111 1.892(11) . ? Re1 C221 1.894(13) . ? Re1 C331 1.908(11) . ? Re1 O2 2.164(7) . ? Re1 N11 2.182(8) . ? Re1 O1 2.209(6) . ? Re2 C222 1.902(13) . ? Re2 C112 1.906(11) . ? Re2 C332 1.918(12) . ? Re2 O1 2.165(6) . ? Re2 N12 2.188(8) . ? Re2 O2 2.204(7) . ? O1 C82 1.338(11) . ? O2 C81 1.362(12) . ? C111 O111 1.156(13) . ? C221 O221 1.147(14) . ? C331 O331 1.128(13) . ? C112 O112 1.144(13) . ? C222 O222 1.139(14) . ? C332 O332 1.123(13) . ? N11 C11 1.316(13) . ? N11 C91 1.358(12) . ? C11 C21 1.42(2) . ? C11 H11 0.93 . ? C21 C31 1.36(2) . ? C21 H21 0.93 . ? C31 C41 1.39(2) . ? C31 H31 0.93 . ? C41 C91 1.385(15) . ? C41 C51 1.41(2) . ? C51 C61 1.37(2) . ? C51 H51 0.93 . ? C61 C71 1.39(2) . ? C61 H61 0.93 . ? C71 C81 1.383(15) . ? C71 H71 0.93 . ? C81 C91 1.411(14) . ? N12 C12 1.332(13) . ? N12 C92 1.347(12) . ? C12 C22 1.410(15) . ? C12 H12 0.93 . ? C22 C32 1.34(2) . ? C22 H22 0.93 . ? C32 C42 1.40(2) . ? C32 H32 0.93 . ? C42 C52 1.39(2) . ? C42 C92 1.404(14) . ? C52 C62 1.39(2) . ? C52 H52 0.93 . ? C62 C72 1.40(2) . ? C62 H62 0.93 . ? C72 C82 1.371(14) . ? C72 H82 0.93 . ? C82 C92 1.422(14) . ? 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 C111 Re1 C221 86.4(5) . . ? C111 Re1 C331 85.1(5) . . ? C221 Re1 C331 86.2(5) . . ? C111 Re1 O2 101.2(4) . . ? C221 Re1 O2 96.8(4) . . ? C331 Re1 O2 173.1(4) . . ? C111 Re1 N11 176.0(4) . . ? C221 Re1 N11 91.9(4) . . ? C331 Re1 N11 98.3(4) . . ? O2 Re1 N11 75.4(3) . . ? C111 Re1 O1 94.7(4) . . ? C221 Re1 O1 172.0(4) . . ? C331 Re1 O1 101.8(4) . . ? O2 Re1 O1 75.2(2) . . ? N11 Re1 O1 86.5(3) . . ? C222 Re2 C112 88.0(5) . . ? C222 Re2 C332 87.6(5) . . ? C112 Re2 C332 89.0(5) . . ? C222 Re2 O1 100.6(4) . . ? C112 Re2 O1 102.1(4) . . ? C332 Re2 O1 166.3(4) . . ? C222 Re2 N12 90.9(4) . . ? C112 Re2 N12 176.6(4) . . ? C332 Re2 N12 94.2(4) . . ? O1 Re2 N12 74.9(3) . . ? C222 Re2 O2 175.4(4) . . ? C112 Re2 O2 91.2(4) . . ? C332 Re2 O2 96.9(4) . . ? O1 Re2 O2 75.2(2) . . ? N12 Re2 O2 89.7(3) . . ? C82 O1 Re2 113.7(6) . . ? C82 O1 Re1 115.8(5) . . ? Re2 O1 Re1 102.5(2) . . ? C81 O2 Re1 112.7(6) . . ? C81 O2 Re2 114.6(6) . . ? Re1 O2 Re2 102.7(3) . . ? O111 C111 Re1 174.7(11) . . ? O221 C221 Re1 177.8(11) . . ? O331 C331 Re1 179.9(12) . . ? O112 C112 Re2 176.8(11) . . ? O222 C222 Re2 177.7(11) . . ? O332 C332 Re2 179.6(13) . . ? C11 N11 C91 118.2(9) . . ? C11 N11 Re1 128.1(7) . . ? C91 N11 Re1 113.3(7) . . ? N11 C11 C21 122.7(11) . . ? N11 C11 H11 118.6(6) . . ? C21 C11 H11 118.6(7) . . ? C31 C21 C11 116.8(12) . . ? C31 C21 H21 121.6(8) . . ? C11 C21 H21 121.6(7) . . ? C21 C31 C41 122.6(11) . . ? C21 C31 H31 118.7(8) . . ? C41 C31 H31 118.7(7) . . ? C91 C41 C31 115.7(11) . . ? C91 C41 C51 120.3(12) . . ? C31 C41 C51 124.0(12) . . ? C61 C51 C41 118.6(12) . . ? C61 C51 H51 120.7(7) . . ? C41 C51 H51 120.7(8) . . ? C51 C61 C71 122.5(11) . . ? C51 C61 H61 118.8(7) . . ? C71 C61 H61 118.8(7) . . ? C81 C71 C61 118.9(11) . . ? C81 C71 H71 120.6(6) . . ? C61 C71 H71 120.6(7) . . ? O2 C81 C71 122.1(10) . . ? O2 C81 C91 117.7(9) . . ? C71 C81 C91 120.1(9) . . ? N11 C91 C41 123.8(10) . . ? N11 C91 C81 116.7(9) . . ? C41 C91 C81 119.4(10) . . ? C12 N12 C92 118.9(9) . . ? C12 N12 Re2 126.8(7) . . ? C92 N12 Re2 113.7(7) . . ? N12 C12 C22 121.0(11) . . ? N12 C12 H12 119.5(6) . . ? C22 C12 H12 119.5(7) . . ? C32 C22 C12 120.5(11) . . ? C32 C22 H22 119.8(7) . . ? C12 C22 H22 119.8(7) . . ? C22 C32 C42 119.7(11) . . ? C22 C32 H32 120.2(7) . . ? C42 C32 H32 120.2(7) . . ? C52 C42 C32 124.2(11) . . ? C52 C42 C92 118.4(11) . . ? C32 C42 C92 117.3(11) . . ? C62 C52 C42 121.2(12) . . ? C62 C52 H52 119.4(7) . . ? C42 C52 H52 119.4(7) . . ? C52 C62 C72 119.6(12) . . ? C52 C62 H62 120.2(7) . . ? C72 C62 H62 120.2(7) . . ? C82 C72 C62 121.0(12) . . ? C82 C72 H82 119.5(7) . . ? C62 C72 H82 119.5(7) . . ? O1 C82 C72 123.3(10) . . ? O1 C82 C92 117.8(8) . . ? C72 C82 C92 118.9(10) . . ? N12 C92 C42 122.7(10) . . ? N12 C92 C82 116.5(9) . . ? C42 C92 C82 120.8(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C222 Re2 O1 C82 -71.8(7) . . . . ? C112 Re2 O1 C82 -162.0(6) . . . . ? C332 Re2 O1 C82 54.1(18) . . . . ? N12 Re2 O1 C82 16.3(6) . . . . ? O2 Re2 O1 C82 110.0(6) . . . . ? C222 Re2 O1 Re1 162.5(4) . . . . ? C112 Re2 O1 Re1 72.2(4) . . . . ? C332 Re2 O1 Re1 -71.7(17) . . . . ? N12 Re2 O1 Re1 -109.5(3) . . . . ? O2 Re2 O1 Re1 -15.8(3) . . . . ? C111 Re1 O1 C82 151.3(7) . . . . ? C221 Re1 O1 C82 -110.9(28) . . . . ? C331 Re1 O1 C82 65.3(7) . . . . ? O2 Re1 O1 C82 -108.3(6) . . . . ? N11 Re1 O1 C82 -32.5(6) . . . . ? C111 Re1 O1 Re2 -84.3(4) . . . . ? C221 Re1 O1 Re2 13.5(29) . . . . ? C331 Re1 O1 Re2 -170.3(4) . . . . ? O2 Re1 O1 Re2 16.1(3) . . . . ? N11 Re1 O1 Re2 91.9(3) . . . . ? C111 Re1 O2 C81 -160.0(7) . . . . ? C221 Re1 O2 C81 -72.3(7) . . . . ? C331 Re1 O2 C81 43.0(33) . . . . ? N11 Re1 O2 C81 17.9(6) . . . . ? O1 Re1 O2 C81 108.1(6) . . . . ? C111 Re1 O2 Re2 76.2(4) . . . . ? C221 Re1 O2 Re2 163.8(4) . . . . ? C331 Re1 O2 Re2 -80.9(32) . . . . ? N11 Re1 O2 Re2 -106.0(3) . . . . ? O1 Re1 O2 Re2 -15.8(3) . . . . ? C222 Re2 O2 C81 -128.6(49) . . . . ? C112 Re2 O2 C81 151.3(7) . . . . ? C332 Re2 O2 C81 62.2(8) . . . . ? O1 Re2 O2 C81 -106.4(7) . . . . ? N12 Re2 O2 C81 -32.0(7) . . . . ? C222 Re2 O2 Re1 -6.1(51) . . . . ? C112 Re2 O2 Re1 -86.1(4) . . . . ? C332 Re2 O2 Re1 -175.3(4) . . . . ? O1 Re2 O2 Re1 16.1(3) . . . . ? N12 Re2 O2 Re1 90.6(3) . . . . ? C221 Re1 C111 O111 52.9(112) . . . . ? C331 Re1 C111 O111 -33.6(112) . . . . ? O2 Re1 C111 O111 149.2(111) . . . . ? N11 Re1 C111 O111 117.5(111) . . . . ? O1 Re1 C111 O111 -135.1(112) . . . . ? C111 Re1 C221 O221 0.3(277) . . . . ? C331 Re1 C221 O221 85.6(277) . . . . ? O2 Re1 C221 O221 -100.6(277) . . . . ? N11 Re1 C221 O221 -176.1(277) . . . . ? O1 Re1 C221 O221 -98.1(274) . . . . ? C111 Re1 C331 O331 -143.9(1000) . . . . ? C221 Re1 C331 O331 129.3(1000) . . . . ? O2 Re1 C331 O331 13.5(1000) . . . . ? N11 Re1 C331 O331 38.0(1000) . . . . ? O1 Re1 C331 O331 -50.1(1000) . . . . ? C222 Re2 C112 O112 12.5(193) . . . . ? C332 Re2 C112 O112 -75.1(193) . . . . ? O1 Re2 C112 O112 112.9(193) . . . . ? N12 Re2 C112 O112 83.9(203) . . . . ? O2 Re2 C112 O112 -172.0(193) . . . . ? C112 Re2 C222 O222 3.0(273) . . . . ? C332 Re2 C222 O222 92.2(273) . . . . ? O1 Re2 C222 O222 -98.9(273) . . . . ? N12 Re2 C222 O222 -173.7(273) . . . . ? O2 Re2 C222 O222 -77.1(280) . . . . ? C222 Re2 C332 O332 158.6(1000) . . . . ? C112 Re2 C332 O332 -113.4(1000) . . . . ? O1 Re2 C332 O332 31.4(1000) . . . . ? N12 Re2 C332 O332 67.9(1000) . . . . ? O2 Re2 C332 O332 -22.3(1000) . . . . ? C111 Re1 N11 C11 -156.4(55) . . . . ? C221 Re1 N11 C11 -91.9(9) . . . . ? C331 Re1 N11 C11 -5.5(9) . . . . ? O2 Re1 N11 C11 171.5(9) . . . . ? O1 Re1 N11 C11 95.9(9) . . . . ? C111 Re1 N11 C91 16.4(60) . . . . ? C221 Re1 N11 C91 80.9(7) . . . . ? C331 Re1 N11 C91 167.3(7) . . . . ? O2 Re1 N11 C91 -15.7(7) . . . . ? O1 Re1 N11 C91 -91.2(7) . . . . ? C91 N11 C11 C21 1.0(16) . . . . ? Re1 N11 C11 C21 173.5(8) . . . . ? N11 C11 C21 C31 -2.3(18) . . . . ? C11 C21 C31 C41 -0.1(20) . . . . ? C21 C31 C41 C91 3.4(19) . . . . ? C21 C31 C41 C51 -178.2(12) . . . . ? C91 C41 C51 C61 3.1(18) . . . . ? C31 C41 C51 C61 -175.2(12) . . . . ? C41 C51 C61 C71 -0.7(19) . . . . ? C51 C61 C71 C81 0.9(18) . . . . ? Re1 O2 C81 C71 162.5(8) . . . . ? Re2 O2 C81 C71 -80.4(11) . . . . ? Re1 O2 C81 C91 -18.4(11) . . . . ? Re2 O2 C81 C91 98.6(9) . . . . ? C61 C71 C81 O2 175.5(10) . . . . ? C61 C71 C81 C91 -3.5(16) . . . . ? C11 N11 C91 C41 2.8(15) . . . . ? Re1 N11 C91 C41 -170.8(8) . . . . ? C11 N11 C91 C81 -175.0(9) . . . . ? Re1 N11 C91 C81 11.4(11) . . . . ? C31 C41 C91 N11 -4.9(16) . . . . ? C51 C41 C91 N11 176.6(10) . . . . ? C31 C41 C91 C81 172.8(10) . . . . ? C51 C41 C91 C81 -5.6(16) . . . . ? O2 C81 C91 N11 4.7(14) . . . . ? C71 C81 C91 N11 -176.2(10) . . . . ? O2 C81 C91 C41 -173.2(9) . . . . ? C71 C81 C91 C41 5.9(15) . . . . ? C222 Re2 N12 C12 -84.4(9) . . . . ? C112 Re2 N12 C12 -155.7(62) . . . . ? C332 Re2 N12 C12 3.3(9) . . . . ? O1 Re2 N12 C12 174.9(9) . . . . ? O2 Re2 N12 C12 100.2(9) . . . . ? C222 Re2 N12 C92 86.4(8) . . . . ? C112 Re2 N12 C92 15.1(68) . . . . ? C332 Re2 N12 C92 174.0(8) . . . . ? O1 Re2 N12 C92 -14.3(7) . . . . ? O2 Re2 N12 C92 -89.1(7) . . . . ? C92 N12 C12 C22 0.0(16) . . . . ? Re2 N12 C12 C22 170.3(8) . . . . ? N12 C12 C22 C32 -0.8(18) . . . . ? C12 C22 C32 C42 0.6(19) . . . . ? C22 C32 C42 C52 -178.5(13) . . . . ? C22 C32 C42 C92 0.3(18) . . . . ? C32 C42 C52 C62 -179.0(13) . . . . ? C92 C42 C52 C62 2.2(19) . . . . ? C42 C52 C62 C72 -0.4(21) . . . . ? C52 C62 C72 C82 0.0(19) . . . . ? Re2 O1 C82 C72 165.4(8) . . . . ? Re1 O1 C82 C72 -76.2(10) . . . . ? Re2 O1 C82 C92 -16.5(10) . . . . ? Re1 O1 C82 C92 101.9(8) . . . . ? C62 C72 C82 O1 176.7(10) . . . . ? C62 C72 C82 C92 -1.3(16) . . . . ? C12 N12 C92 C42 1.0(16) . . . . ? Re2 N12 C92 C42 -170.5(8) . . . . ? C12 N12 C92 C82 -177.7(9) . . . . ? Re2 N12 C92 C82 10.8(11) . . . . ? C52 C42 C92 N12 177.7(11) . . . . ? C32 C42 C92 N12 -1.2(16) . . . . ? C52 C42 C92 C82 -3.6(16) . . . . ? C32 C42 C92 C82 177.5(10) . . . . ? O1 C82 C92 N12 3.8(13) . . . . ? C72 C82 C92 N12 -178.1(10) . . . . ? O1 C82 C92 C42 -174.9(9) . . . . ? C72 C82 C92 C42 3.2(15) . . . . ? _refine_diff_density_max 2.081 _refine_diff_density_min -1.321 _refine_diff_density_rms 0.221