Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Alessio, E.' 'Fronzoni, Giovanna' 'Iengo, Elisabetta' 'Mestroni, Stefano' 'Stener, Mauro' 'Zangrando, Ennio' _publ_contact_author_name 'Prof E Alessio' _publ_contact_author_address ; Prof E Alessio Dipartimento di Scienze Chimiche Universita di Trieste Via L Giorgieri 1 Trieste 34127 ITALY ; data_1 _database_code_CSD 153388 _audit_creation_method SHELXL _chemical_name_systematic ; (mu-oxo)-bis[bis(1,4-pyrazine)-dichloro-oxo-rhenium(v)] hemi acetone solvate ; _chemical_name_common ? _chemical_formula_moiety '((C4 H4 N2)4 (Cl 1-)2 O3 Re2 ), 0.5(C3 H6 O)' _chemical_formula_structural '((C4 H4 N2)2 (Cl)2 O Re) O ((Re O (C4 H4 N2)2 (Cl)2) 0.5(O C3 H6)' _chemical_formula_analytical ? _chemical_formula_sum 'C17.50 H19 Cl4 N8 O3.50 Re2' _chemical_formula_weight 911.61 _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 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _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 9.399(1) _cell_length_b 10.244(2) _cell_length_c 15.691(3) _cell_angle_alpha 105.41(1) _cell_angle_beta 96.36(1) _cell_angle_gamma 100.50(1) _cell_volume 1411.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13 _cell_measurement_theta_max 19 _exptl_crystal_description ? _exptl_crystal_colour 'emerald green' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.145 _exptl_crystal_density_method ? _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 8.981 _exptl_absorpt_correction_type 'psi scan' _exptl_absorpt_correction_T_min 0.3544 _exptl_absorpt_correction_T_max 1.0000 _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_type 'Enraf Nonius CAD4' _diffrn_measurement_method '\w/2\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 66 _diffrn_standards_decay_% 2 _diffrn_standards_decay_corr_max 1.043 _diffrn_standards_decay_corr_min 0.985 _diffrn_reflns_number 6348 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 26.98 _reflns_number_total 6118 _reflns_number_observed 4841 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 (Enraf-Nonius)' _computing_cell_refinement 'CELDIM (Enraf-Nonius)' _computing_data_reduction 'WinGX 1.63 (Farrugia, 1999)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3/Windows (Farrugia,1997)' _computing_publication_material 'WinGX 1.63 (Farrugia, 1999)' _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^)+(0.1000P)^2^ ] 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_number_reflns 6118 _refine_ls_number_parameters 334 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_obs 0.0493 _refine_ls_wR_factor_all 0.1480 _refine_ls_wR_factor_obs 0.1429 _refine_ls_goodness_of_fit_all 1.134 _refine_ls_goodness_of_fit_obs 1.240 _refine_ls_restrained_S_all 1.134 _refine_ls_restrained_S_obs 1.240 _refine_ls_shift/esd_max 0.000 _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 Re2 Re 0.58981(4) 0.07069(3) 0.35127(2) 0.03543(13) Uani 1 d . . Re1 Re 0.93197(4) 0.20456(3) 0.25901(2) 0.03539(13) Uani 1 d . . Cl1 Cl 1.0297(3) 0.3772(3) 0.3981(2) 0.0474(5) Uani 1 d . . Cl3 Cl 0.6531(3) -0.1445(2) 0.3385(2) 0.0503(6) Uani 1 d . . Cl4 Cl 0.4538(3) -0.0145(3) 0.2029(2) 0.0557(7) Uani 1 d . . Cl2 Cl 1.0557(3) 0.0484(3) 0.3041(2) 0.0545(6) Uani 1 d . . O2 O 0.7617(6) 0.1390(5) 0.3061(4) 0.0323(13) Uani 1 d . . O3 O 0.4435(8) 0.0481(7) 0.4034(5) 0.048(2) Uani 1 d . . O1 O 1.0569(8) 0.2653(7) 0.1998(5) 0.051(2) Uani 1 d . . N4 N 0.7238(8) 0.1487(7) 0.4805(5) 0.037(2) Uani 1 d . . N2 N 0.8019(8) 0.3412(7) 0.2204(5) 0.036(2) Uani 1 d . . N3 N 0.5479(8) 0.2751(7) 0.3629(6) 0.039(2) Uani 1 d . . N1 N 0.8313(9) 0.0400(8) 0.1379(6) 0.043(2) Uani 1 d . . N6 N 0.6427(11) 0.5240(9) 0.1706(7) 0.058(2) Uani 1 d . . N7 N 0.4891(11) 0.5373(10) 0.3850(8) 0.063(3) Uani 1 d . . N5 N 0.7116(14) -0.1758(12) -0.0172(8) 0.080(3) Uani 1 d . . N8 N 0.8968(12) 0.2507(9) 0.6500(7) 0.060(3) Uani 1 d . . C1 C 0.7685(13) -0.0822(10) 0.1429(8) 0.053(3) Uani 1 d . . H1 H 0.7637(13) -0.0970(10) 0.1986(8) 0.063 Uiso 1 calc R . C2 C 0.7086(15) -0.1906(12) 0.0642(8) 0.066(3) Uani 1 d . . H2 H 0.6647(15) -0.2766(12) 0.0692(8) 0.079 Uiso 1 calc R . C3 C 0.7736(17) -0.0464(14) -0.0186(8) 0.072(4) Uani 1 d . . H3 H 0.7731(17) -0.0282(14) -0.0736(8) 0.087 Uiso 1 calc R . C4 C 0.8370(14) 0.0587(12) 0.0578(8) 0.060(3) Uani 1 d . . H4 H 0.8846(14) 0.1441(12) 0.0535(8) 0.073 Uiso 1 calc R . C5 C 0.8637(11) 0.4773(9) 0.2353(7) 0.043(2) Uani 1 d . . H5 H 0.9613(11) 0.5112(9) 0.2629(7) 0.052 Uiso 1 calc R . C6 C 0.7881(13) 0.5640(11) 0.2115(8) 0.052(3) Uani 1 d . . H6 H 0.8358(13) 0.6564(11) 0.2231(8) 0.062 Uiso 1 calc R . C7 C 0.5839(12) 0.3906(11) 0.1565(7) 0.054(3) Uani 1 d . . H7 H 0.4859(12) 0.3573(11) 0.1296(7) 0.065 Uiso 1 calc R . C8 C 0.6606(12) 0.2978(10) 0.1798(7) 0.047(2) Uani 1 d . . H8 H 0.6140(12) 0.2050(10) 0.1672(7) 0.057 Uiso 1 calc R . C9 C 0.4162(11) 0.2924(11) 0.3385(8) 0.049(2) Uani 1 d . . H9 H 0.3400(11) 0.2148(11) 0.3131(8) 0.059 Uiso 1 calc R . C10 C 0.3887(13) 0.4201(11) 0.3493(9) 0.059(3) Uani 1 d . . H10 H 0.2933(13) 0.4263(11) 0.3306(9) 0.070 Uiso 1 calc R . C11 C 0.6253(12) 0.5221(9) 0.4107(8) 0.052(3) Uani 1 d . . H11 H 0.7007(12) 0.6003(9) 0.4367(8) 0.062 Uiso 1 calc R . C12 C 0.6534(11) 0.3926(10) 0.3990(7) 0.043(2) Uani 1 d . . H12 H 0.7487(11) 0.3851(10) 0.4165(7) 0.051 Uiso 1 calc R . C13 C 0.6690(12) 0.2079(9) 0.5523(7) 0.044(2) Uani 1 d . . H13 H 0.5714(12) 0.2148(9) 0.5455(7) 0.053 Uiso 1 calc R . C14 C 0.7541(14) 0.2587(10) 0.6358(8) 0.058(3) Uani 1 d . . H14 H 0.7125(14) 0.2999(10) 0.6843(8) 0.069 Uiso 1 calc R . C15 C 0.9482(12) 0.1905(11) 0.5782(8) 0.054(3) Uani 1 d . . H15 H 1.0455(12) 0.1824(11) 0.5849(8) 0.065 Uiso 1 calc R . C16 C 0.8641(11) 0.1390(10) 0.4937(7) 0.045(2) Uani 1 d . . H16 H 0.9055(11) 0.0970(10) 0.4454(7) 0.054 Uiso 1 calc R . O4 O 0.8308(23) 0.3568(17) 0.0197(9) 0.068(5) Uani 0.50 d P . C17 C 0.8185(20) 0.3581(15) -0.0559(12) 0.041(4) Uani 0.50 d PD . C19 C 0.9017(21) 0.2778(22) -0.1166(13) 0.046(5) Uani 0.50 d PD . C18 C 0.7075(34) 0.4253(25) -0.0973(17) 0.077(9) Uani 0.50 d PD . 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 Re2 0.0318(2) 0.0265(2) 0.0469(2) 0.01154(15) 0.0047(2) 0.00374(13) Re1 0.0328(2) 0.0322(2) 0.0398(2) 0.00971(15) 0.00550(15) 0.00537(14) Cl1 0.0372(12) 0.0482(13) 0.0456(13) 0.0042(10) -0.0003(10) 0.0002(9) Cl3 0.0579(15) 0.0304(10) 0.067(2) 0.0169(11) 0.0169(13) 0.0139(10) Cl4 0.0467(14) 0.0456(13) 0.061(2) 0.0082(12) -0.0097(12) -0.0015(10) Cl2 0.0462(14) 0.0557(14) 0.072(2) 0.0253(13) 0.0140(13) 0.0252(11) O2 0.026(3) 0.033(3) 0.040(3) 0.011(3) 0.004(2) 0.010(2) O3 0.039(4) 0.039(3) 0.072(5) 0.023(3) 0.013(3) 0.008(3) O1 0.045(4) 0.044(4) 0.064(5) 0.015(3) 0.019(4) 0.007(3) N4 0.036(4) 0.026(3) 0.053(5) 0.020(3) 0.007(3) 0.007(3) N2 0.035(4) 0.032(4) 0.041(4) 0.013(3) 0.007(3) 0.007(3) N3 0.036(4) 0.028(3) 0.054(5) 0.010(3) 0.010(4) 0.010(3) N1 0.044(4) 0.034(4) 0.045(5) 0.004(3) 0.003(4) 0.008(3) N6 0.054(5) 0.043(5) 0.073(7) 0.017(4) -0.007(5) 0.008(4) N7 0.057(6) 0.051(5) 0.101(8) 0.034(5) 0.037(6) 0.032(4) N5 0.089(9) 0.070(7) 0.061(7) 0.001(5) 0.001(6) 0.002(6) N8 0.081(7) 0.039(4) 0.053(6) 0.014(4) -0.002(5) 0.002(4) C1 0.060(7) 0.040(5) 0.051(6) 0.006(5) 0.007(5) 0.008(5) C2 0.079(9) 0.047(6) 0.053(7) -0.003(5) 0.000(6) 0.000(6) C3 0.101(11) 0.075(8) 0.031(6) 0.012(5) 0.003(6) 0.007(8) C4 0.070(8) 0.049(6) 0.057(7) 0.015(5) 0.005(6) 0.001(5) C5 0.042(5) 0.035(5) 0.049(6) 0.012(4) 0.009(4) -0.001(4) C6 0.064(7) 0.037(5) 0.056(6) 0.017(5) 0.011(5) 0.011(5) C7 0.048(6) 0.055(6) 0.051(6) 0.013(5) -0.017(5) 0.008(5) C8 0.050(6) 0.039(5) 0.047(6) 0.016(4) -0.003(5) -0.003(4) C9 0.033(5) 0.046(5) 0.069(7) 0.022(5) 0.008(5) 0.005(4) C10 0.046(6) 0.047(6) 0.097(9) 0.034(6) 0.024(6) 0.023(5) C11 0.056(6) 0.027(4) 0.069(7) 0.010(5) 0.012(5) 0.004(4) C12 0.034(5) 0.043(5) 0.055(6) 0.018(4) 0.009(4) 0.012(4) C13 0.052(6) 0.033(4) 0.051(6) 0.013(4) 0.016(5) 0.012(4) C14 0.075(8) 0.034(5) 0.059(7) 0.010(5) 0.010(6) 0.007(5) C15 0.046(6) 0.060(6) 0.056(7) 0.027(5) -0.007(5) 0.003(5) C16 0.046(5) 0.045(5) 0.049(6) 0.019(4) 0.014(4) 0.015(4) O4 0.127(16) 0.072(10) 0.028(7) 0.021(7) 0.039(9) 0.050(10) C17 0.061(12) 0.019(7) 0.041(10) 0.009(7) 0.008(9) 0.006(7) C19 0.038(10) 0.065(13) 0.035(10) 0.010(9) 0.019(8) 0.009(9) C18 0.136(26) 0.053(13) 0.056(15) 0.016(11) 0.009(15) 0.056(15) _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 Re2 O3 1.688(7) . ? Re2 O2 1.926(5) . ? Re2 N4 2.131(8) . ? Re2 N3 2.165(7) . ? Re2 Cl3 2.350(2) . ? Re2 Cl4 2.381(3) . ? Re1 O1 1.706(7) . ? Re1 O2 1.921(5) . ? Re1 N1 2.161(8) . ? Re1 N2 2.175(7) . ? Re1 Cl2 2.348(2) . ? Re1 Cl1 2.377(2) . ? N4 C13 1.334(12) . ? N4 C16 1.338(12) . ? N2 C8 1.347(12) . ? N2 C5 1.356(11) . ? N3 C9 1.312(12) . ? N3 C12 1.353(12) . ? N1 C1 1.310(13) . ? N1 C4 1.325(14) . ? N6 C7 1.326(13) . ? N6 C6 1.381(14) . ? N7 C10 1.326(15) . ? N7 C11 1.348(14) . ? N5 C2 1.33(2) . ? N5 C3 1.35(2) . ? N8 C15 1.32(2) . ? N8 C14 1.36(2) . ? C1 C2 1.401(15) . ? C3 C4 1.37(2) . ? C5 C6 1.335(15) . ? C7 C8 1.390(14) . ? C9 C10 1.350(14) . ? C11 C12 1.369(13) . ? C13 C14 1.37(2) . ? C15 C16 1.380(15) . ? O4 C17 1.18(2) . ? C17 C19 1.48(2) . ? C17 C18 1.53(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Re2 O2 167.3(3) . . ? O3 Re2 N4 87.8(3) . . ? O2 Re2 N4 86.2(3) . . ? O3 Re2 N3 84.8(3) . . ? O2 Re2 N3 84.1(3) . . ? N4 Re2 N3 89.8(3) . . ? O3 Re2 Cl3 98.9(2) . . ? O2 Re2 Cl3 92.1(2) . . ? N4 Re2 Cl3 88.6(2) . . ? N3 Re2 Cl3 175.9(2) . . ? O3 Re2 Cl4 95.8(3) . . ? O2 Re2 Cl4 90.3(2) . . ? N4 Re2 Cl4 176.4(2) . . ? N3 Re2 Cl4 90.7(2) . . ? Cl3 Re2 Cl4 90.75(10) . . ? O1 Re1 O2 168.0(3) . . ? O1 Re1 N1 88.1(3) . . ? O2 Re1 N1 84.9(3) . . ? O1 Re1 N2 86.3(3) . . ? O2 Re1 N2 84.0(2) . . ? N1 Re1 N2 90.9(3) . . ? O1 Re1 Cl2 98.1(3) . . ? O2 Re1 Cl2 91.5(2) . . ? N1 Re1 Cl2 88.2(2) . . ? N2 Re1 Cl2 175.5(2) . . ? O1 Re1 Cl1 96.3(3) . . ? O2 Re1 Cl1 90.8(2) . . ? N1 Re1 Cl1 175.6(2) . . ? N2 Re1 Cl1 89.8(2) . . ? Cl2 Re1 Cl1 90.82(10) . . ? Re1 O2 Re2 179.0(3) . . ? C13 N4 C16 117.2(9) . . ? C13 N4 Re2 120.6(7) . . ? C16 N4 Re2 122.1(7) . . ? C8 N2 C5 116.6(8) . . ? C8 N2 Re1 123.5(6) . . ? C5 N2 Re1 119.9(6) . . ? C9 N3 C12 115.9(8) . . ? C9 N3 Re2 121.6(6) . . ? C12 N3 Re2 122.5(6) . . ? C1 N1 C4 119.1(9) . . ? C1 N1 Re1 119.8(7) . . ? C4 N1 Re1 121.0(7) . . ? C7 N6 C6 114.0(9) . . ? C10 N7 C11 115.4(9) . . ? C2 N5 C3 114.8(10) . . ? C15 N8 C14 115.6(10) . . ? N1 C1 C2 119.8(11) . . ? N5 C2 C1 122.9(11) . . ? N5 C3 C4 122.6(11) . . ? N1 C4 C3 120.6(11) . . ? C6 C5 N2 121.7(10) . . ? C5 C6 N6 123.5(9) . . ? N6 C7 C8 123.6(10) . . ? N2 C8 C7 120.6(8) . . ? N3 C9 C10 121.6(10) . . ? N7 C10 C9 124.0(11) . . ? N7 C11 C12 120.5(9) . . ? N3 C12 C11 122.5(9) . . ? N4 C13 C14 121.2(10) . . ? N8 C14 C13 122.1(11) . . ? N8 C15 C16 123.0(11) . . ? N4 C16 C15 120.8(10) . . ? O4 C17 C19 118.9(17) . . ? O4 C17 C18 123.3(19) . . ? C19 C17 C18 117.4(18) . . ? 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 O1 Re1 O2 Re2 57.3(156) . . . . ? N1 Re1 O2 Re2 2.4(151) . . . . ? N2 Re1 O2 Re2 93.8(151) . . . . ? Cl2 Re1 O2 Re2 -85.6(151) . . . . ? Cl1 Re1 O2 Re2 -176.5(1000) . . . . ? O3 Re2 O2 Re1 -148.2(146) . . . . ? N4 Re2 O2 Re1 149.9(151) . . . . ? N3 Re2 O2 Re1 -119.9(151) . . . . ? Cl3 Re2 O2 Re1 61.5(151) . . . . ? Cl4 Re2 O2 Re1 -29.3(151) . . . . ? O3 Re2 N4 C13 -26.7(7) . . . . ? O2 Re2 N4 C13 142.1(6) . . . . ? N3 Re2 N4 C13 58.1(7) . . . . ? Cl3 Re2 N4 C13 -125.7(6) . . . . ? Cl4 Re2 N4 C13 155.2(26) . . . . ? O3 Re2 N4 C16 152.3(7) . . . . ? O2 Re2 N4 C16 -38.9(7) . . . . ? N3 Re2 N4 C16 -123.0(7) . . . . ? Cl3 Re2 N4 C16 53.3(7) . . . . ? Cl4 Re2 N4 C16 -25.8(33) . . . . ? O1 Re1 N2 C8 126.5(8) . . . . ? O2 Re1 N2 C8 -46.4(8) . . . . ? N1 Re1 N2 C8 38.4(8) . . . . ? Cl2 Re1 N2 C8 -39.5(31) . . . . ? Cl1 Re1 N2 C8 -137.2(8) . . . . ? O1 Re1 N2 C5 -52.1(7) . . . . ? O2 Re1 N2 C5 135.1(7) . . . . ? N1 Re1 N2 C5 -140.1(7) . . . . ? Cl2 Re1 N2 C5 141.9(23) . . . . ? Cl1 Re1 N2 C5 44.2(7) . . . . ? O3 Re2 N3 C9 -49.2(9) . . . . ? O2 Re2 N3 C9 136.8(9) . . . . ? N4 Re2 N3 C9 -137.0(9) . . . . ? Cl3 Re2 N3 C9 156.9(27) . . . . ? Cl4 Re2 N3 C9 46.6(8) . . . . ? O3 Re2 N3 C12 127.9(8) . . . . ? O2 Re2 N3 C12 -46.1(8) . . . . ? N4 Re2 N3 C12 40.1(8) . . . . ? Cl3 Re2 N3 C12 -26.0(37) . . . . ? Cl4 Re2 N3 C12 -136.3(8) . . . . ? O1 Re1 N1 C1 147.9(8) . . . . ? O2 Re1 N1 C1 -41.9(8) . . . . ? N2 Re1 N1 C1 -125.8(8) . . . . ? Cl2 Re1 N1 C1 49.7(8) . . . . ? Cl1 Re1 N1 C1 -27.4(33) . . . . ? O1 Re1 N1 C4 -29.3(9) . . . . ? O2 Re1 N1 C4 140.9(9) . . . . ? N2 Re1 N1 C4 57.0(9) . . . . ? Cl2 Re1 N1 C4 -127.5(9) . . . . ? Cl1 Re1 N1 C4 155.4(25) . . . . ? C4 N1 C1 C2 -0.1(17) . . . . ? Re1 N1 C1 C2 -177.3(9) . . . . ? C3 N5 C2 C1 -1.8(21) . . . . ? N1 C1 C2 N5 -0.2(20) . . . . ? C2 N5 C3 C4 4.2(22) . . . . ? C1 N1 C4 C3 2.4(18) . . . . ? Re1 N1 C4 C3 179.6(10) . . . . ? N5 C3 C4 N1 -4.7(23) . . . . ? C8 N2 C5 C6 0.4(14) . . . . ? Re1 N2 C5 C6 179.1(8) . . . . ? N2 C5 C6 N6 0.2(18) . . . . ? C7 N6 C6 C5 -0.2(17) . . . . ? C6 N6 C7 C8 -0.6(18) . . . . ? C5 N2 C8 C7 -1.1(15) . . . . ? Re1 N2 C8 C7 -179.7(8) . . . . ? N6 C7 C8 N2 1.2(18) . . . . ? C12 N3 C9 C10 -0.2(16) . . . . ? Re2 N3 C9 C10 177.1(9) . . . . ? C11 N7 C10 C9 0.1(19) . . . . ? N3 C9 C10 N7 -0.2(20) . . . . ? C10 N7 C11 C12 0.5(17) . . . . ? C9 N3 C12 C11 0.8(15) . . . . ? Re2 N3 C12 C11 -176.4(8) . . . . ? N7 C11 C12 N3 -1.0(17) . . . . ? C16 N4 C13 C14 1.1(13) . . . . ? Re2 N4 C13 C14 -179.9(7) . . . . ? C15 N8 C14 C13 -0.2(15) . . . . ? N4 C13 C14 N8 -0.5(15) . . . . ? C14 N8 C15 C16 0.3(15) . . . . ? C13 N4 C16 C15 -1.0(13) . . . . ? Re2 N4 C16 C15 180.0(7) . . . . ? N8 C15 C16 N4 0.3(16) . . . . ? N1 Re1 Re2 N4 152.4(3) . . . . ? N2 Re1 Re2 N3 -26.1(3) . . . . ? Cl1 Re1 Re2 Cl4 154.26(10) . . . . ? Cl2 Re1 Re2 Cl3 -24.15(11) . . . . ? _refine_diff_density_max 1.527 _refine_diff_density_min -1.943 _refine_diff_density_rms 0.272 #===END data_3 _database_code_CSD 153389 _audit_creation_method SHELXL _chemical_name_systematic ; bis(1,4-pyrazine)-dichloro-ethoxy-oxo-rhenium(V) ; _chemical_name_common ? _chemical_formula_moiety '(C4 H4 N2)2 (Cl 1-)2 (O C2 H5 1-) O Re' _chemical_formula_structural '(C4 H4 N2)2 (Cl)2 (O C2 H5) O Re' _chemical_formula_analytical ? _chemical_formula_sum 'C10 H13 Cl2 N4 O2 Re' _chemical_formula_weight 478.34 _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' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 21/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 11.804(3) _cell_length_b 9.061(3) _cell_length_c 14.253(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.67(2) _cell_angle_gamma 90.00 _cell_volume 1467.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 16 _exptl_crystal_description ? _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.165 _exptl_crystal_density_method ? _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 8.645 _exptl_absorpt_correction_type 'psi scan' _exptl_absorpt_correction_T_min 74.56 _exptl_absorpt_correction_T_max 99.90 _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 'KUMA K4' _diffrn_measurement_method '\w/2\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 4000 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3574 _diffrn_reflns_av_R_equivalents 0.0726 _diffrn_reflns_av_sigmaI/netI 0.1221 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 30.06 _reflns_number_total 3340 _reflns_number_gt 1750 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KM4 package' _computing_cell_refinement 'KM4 package' _computing_data_reduction 'KM4 package' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3/Windows (Farrugia,1997)' _computing_publication_material 'WinGX 1.63 (Farrugia, 1999)' _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^)+(0.1105P)^2^] 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 3340 _refine_ls_number_parameters 173 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1516 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.2165 _refine_ls_wR_factor_gt 0.1823 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.038 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re Re 0.07478(6) -0.00673(9) 0.28402(5) 0.0316(2) Uani 1 d . . . Cl1 Cl 0.0527(6) -0.1637(6) 0.4155(4) 0.0529(16) Uani 1 d . . . Cl2 Cl 0.0766(6) 0.1494(7) 0.1521(5) 0.0579(17) Uani 1 d . . . O1 O 0.2146(12) -0.0639(19) 0.3122(12) 0.050(4) Uani 1 d . . . O2 O -0.0778(11) 0.0494(15) 0.2731(10) 0.038(3) Uani 1 d . . . N1 N 0.0137(15) -0.1838(18) 0.1824(13) 0.036(4) Uani 1 d . . . N2 N -0.0773(14) -0.413(2) 0.0629(14) 0.042(4) Uani 1 d . . . C1 C 0.0657(17) -0.313(2) 0.1962(18) 0.046(6) Uani 1 d . . . H1 H 0.1303 -0.3291 0.2494 0.055 Uiso 1 calc R . . C2 C 0.0216(19) -0.426(2) 0.1290(16) 0.040(5) Uani 1 d . . . H2 H 0.0648 -0.5122 0.1320 0.049 Uiso 1 calc R . . C3 C -0.132(2) -0.285(3) 0.0538(16) 0.045(5) Uani 1 d . . . H3 H -0.2031 -0.2727 0.0061 0.054 Uiso 1 calc R . . C4 C -0.0850(17) -0.171(2) 0.1149(13) 0.038(5) Uani 1 d . . . H4 H -0.1248 -0.0814 0.1079 0.046 Uiso 1 calc R . . N3 N 0.1327(15) 0.1737(18) 0.3775(13) 0.038(4) Uani 1 d . . . N4 N 0.202(2) 0.425(3) 0.4999(15) 0.064(6) Uani 1 d U . . C5 C 0.0723(18) 0.305(2) 0.3631(18) 0.047(6) Uani 1 d . . . H5 H 0.0052 0.3152 0.3113 0.056 Uiso 1 calc R . . C6 C 0.111(2) 0.422(2) 0.4251(17) 0.059(8) Uani 1 d U . . H6 H 0.0665 0.5082 0.4118 0.071 Uiso 1 calc R . . C7 C 0.262(2) 0.294(3) 0.5127(17) 0.046(6) Uani 1 d U . . H7 H 0.3313 0.2881 0.5628 0.055 Uiso 1 calc R . . C8 C 0.2266(18) 0.172(3) 0.4561(16) 0.044(5) Uani 1 d . . . H8 H 0.2689 0.0852 0.4723 0.053 Uiso 1 calc R . . C9 C -0.181(2) 0.051(3) 0.313(2) 0.069(8) Uani 1 d U . . H9A H -0.1638 -0.0105 0.3706 0.083 Uiso 1 calc R . . H9B H -0.1924 0.1508 0.3328 0.083 Uiso 1 calc R . . C10 C -0.286(2) 0.003(5) 0.252(3) 0.130(16) Uani 1 d U . . H10A H -0.2843 0.0151 0.1850 0.194 Uiso 1 calc R . . H10B H -0.3497 0.0606 0.2628 0.194 Uiso 1 calc R . . H10C H -0.2979 -0.0989 0.2640 0.194 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re 0.0263(3) 0.0239(3) 0.0365(4) -0.0054(5) -0.0053(2) 0.0004(4) Cl1 0.072(4) 0.040(3) 0.038(3) 0.006(2) 0.000(3) 0.002(3) Cl2 0.067(4) 0.049(3) 0.052(4) 0.008(3) 0.005(3) -0.020(3) O1 0.030(7) 0.065(10) 0.065(11) 0.008(8) 0.028(8) 0.004(7) O2 0.029(7) 0.033(7) 0.040(8) 0.022(6) -0.009(6) -0.011(5) N1 0.035(9) 0.033(9) 0.039(10) -0.010(8) 0.006(8) -0.001(7) N2 0.027(8) 0.043(10) 0.049(11) -0.009(9) -0.001(8) -0.011(8) C1 0.030(10) 0.019(8) 0.072(16) 0.000(10) -0.013(10) 0.003(8) C2 0.042(12) 0.022(9) 0.053(14) -0.011(9) 0.005(10) -0.008(8) C3 0.036(11) 0.063(15) 0.037(12) -0.013(11) 0.012(10) 0.005(11) C4 0.039(11) 0.045(12) 0.017(9) 0.004(9) -0.015(8) 0.005(9) N3 0.032(9) 0.027(8) 0.040(10) -0.003(7) -0.015(8) -0.006(7) N4 0.065(13) 0.070(13) 0.046(11) -0.016(10) -0.005(10) -0.044(11) C5 0.038(11) 0.017(8) 0.069(16) -0.002(9) -0.013(11) 0.005(8) C6 0.074(16) 0.032(11) 0.043(12) -0.005(10) -0.035(12) 0.022(11) C7 0.039(12) 0.041(11) 0.044(12) -0.015(10) -0.011(10) -0.005(9) C8 0.032(11) 0.049(13) 0.046(13) 0.010(11) 0.002(9) -0.002(10) C9 0.061(17) 0.065(17) 0.08(2) 0.006(15) 0.014(15) -0.009(14) C10 0.053(16) 0.23(4) 0.12(3) -0.02(3) 0.049(18) -0.05(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 Re O1 1.672(14) . ? Re O2 1.837(14) . ? Re N3 2.103(16) . ? Re N1 2.152(16) . ? Re Cl2 2.357(6) . ? Re Cl1 2.423(6) . ? O2 C9 1.48(3) . ? N1 C4 1.30(2) . ? N1 C1 1.31(2) . ? N2 C2 1.29(2) . ? N2 C3 1.31(3) . ? C1 C2 1.40(3) . ? C3 C4 1.37(3) . ? N3 C8 1.35(2) . ? N3 C5 1.37(2) . ? N4 C6 1.29(3) . ? N4 C7 1.37(3) . ? C5 C6 1.37(3) . ? C7 C8 1.36(3) . ? C9 C10 1.38(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Re O2 171.0(6) . . ? O1 Re N3 87.6(8) . . ? O2 Re N3 89.0(7) . . ? O1 Re N1 93.4(7) . . ? O2 Re N1 90.4(6) . . ? N3 Re N1 177.1(7) . . ? O1 Re Cl2 99.0(6) . . ? O2 Re Cl2 89.2(4) . . ? N3 Re Cl2 88.1(5) . . ? N1 Re Cl2 89.1(5) . . ? O1 Re Cl1 86.4(6) . . ? O2 Re Cl1 85.4(4) . . ? N3 Re Cl1 92.9(5) . . ? N1 Re Cl1 89.8(5) . . ? Cl2 Re Cl1 174.5(2) . . ? C9 O2 Re 149.7(15) . . ? C4 N1 C1 118.8(18) . . ? C4 N1 Re 120.1(14) . . ? C1 N1 Re 120.3(14) . . ? C2 N2 C3 118.5(18) . . ? N1 C1 C2 118.3(19) . . ? N2 C2 C1 121.8(19) . . ? N2 C3 C4 120(2) . . ? N1 C4 C3 122(2) . . ? C8 N3 C5 114.1(18) . . ? C8 N3 Re 125.0(15) . . ? C5 N3 Re 120.8(13) . . ? C6 N4 C7 112.3(19) . . ? C6 C5 N3 120.2(18) . . ? N4 C6 C5 127(2) . . ? C8 C7 N4 124(2) . . ? N3 C8 C7 122(2) . . ? C10 C9 O2 117(3) . . ? 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 O1 Re O2 C9 -14(6) . . . . ? N3 Re O2 C9 -82(3) . . . . ? N1 Re O2 C9 101(3) . . . . ? Cl2 Re O2 C9 -170(3) . . . . ? Cl1 Re O2 C9 11(3) . . . . ? O1 Re N1 C4 -158.7(18) . . . . ? O2 Re N1 C4 29.5(18) . . . . ? N3 Re N1 C4 -47(14) . . . . ? Cl2 Re N1 C4 -59.7(17) . . . . ? Cl1 Re N1 C4 114.9(17) . . . . ? O1 Re N1 C1 31.4(19) . . . . ? O2 Re N1 C1 -140.4(19) . . . . ? N3 Re N1 C1 143(13) . . . . ? Cl2 Re N1 C1 130.4(18) . . . . ? Cl1 Re N1 C1 -55.0(19) . . . . ? C4 N1 C1 C2 9(4) . . . . ? Re N1 C1 C2 178.9(16) . . . . ? C3 N2 C2 C1 6(4) . . . . ? N1 C1 C2 N2 -10(4) . . . . ? C2 N2 C3 C4 -1(3) . . . . ? C1 N1 C4 C3 -4(3) . . . . ? Re N1 C4 C3 -174.4(17) . . . . ? N2 C3 C4 N1 0(4) . . . . ? O1 Re N3 C8 -29.0(19) . . . . ? O2 Re N3 C8 142.7(19) . . . . ? N1 Re N3 C8 -140(13) . . . . ? Cl2 Re N3 C8 -128.1(19) . . . . ? Cl1 Re N3 C8 57.3(19) . . . . ? O1 Re N3 C5 153.0(19) . . . . ? O2 Re N3 C5 -35.3(19) . . . . ? N1 Re N3 C5 42(15) . . . . ? Cl2 Re N3 C5 53.9(18) . . . . ? Cl1 Re N3 C5 -120.7(18) . . . . ? C8 N3 C5 C6 1(4) . . . . ? Re N3 C5 C6 180(2) . . . . ? C7 N4 C6 C5 1(5) . . . . ? N3 C5 C6 N4 0(5) . . . . ? C6 N4 C7 C8 -3(4) . . . . ? C5 N3 C8 C7 -4(3) . . . . ? Re N3 C8 C7 178.2(18) . . . . ? N4 C7 C8 N3 5(4) . . . . ? Re O2 C9 C10 -127(3) . . . . ? C1 N1 N3 C8 2(3) . . . . ? C4 N1 N3 C5 -6(2) . . . . ? _refine_diff_density_max 2.143 _refine_diff_density_min -2.300 _refine_diff_density_rms 0.351 #===END data_5 _database_code_CSD 153390 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (1,4-pyrazine)-triphenylphosphine-dichloro-ethoxy-oxo-rhenium(V) ; _chemical_name_common ? _chemical_formula_moiety '(C4 H4 N2) (P (C6 H5)3) (Cl 1-)2 (O C2 H5 1-) O Re' _chemical_formula_structural '(C4 H4 N2) (P (C6 H5)3) (Cl)2 (O C2 H5) O Re' _chemical_formula_analytical ? _chemical_formula_sum 'C24 H24 Cl2 N2 O2 P Re' _chemical_formula_weight 660.52 _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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.443(4) _cell_length_b 8.891(1) _cell_length_c 32.297(7) _cell_angle_alpha 90.00 _cell_angle_beta 97.80(2) _cell_angle_gamma 90.00 _cell_volume 4962.5(17) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13 _cell_measurement_theta_max 17 _exptl_crystal_description ? _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2576 _exptl_absorpt_coefficient_mu 5.201 _exptl_absorpt_correction_type 'psi scan' _exptl_absorpt_correction_T_min 0.7272 _exptl_absorpt_correction_T_max 1.0000 _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_type 'Enraf Nonius CAD4' _diffrn_measurement_method '\w/2\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 66 _diffrn_standards_decay_% 3 _diffrn_standards_decay_corr_max 1.059 _diffrn_standards_decay_corr_min 0.911 _diffrn_reflns_number 6440 _diffrn_reflns_av_R_equivalents 0.0550 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 27.97 _reflns_number_total 5953 _reflns_number_gt 5130 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 (Enraf-Nonius)' _computing_cell_refinement 'CELDIM (Enraf-Nonius)' _computing_data_reduction 'WinGX 1.63 (Farrugia, 1999)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3/Windows (Farrugia,1997)' _computing_publication_material 'WinGX 1.63 (Farrugia, 1999)' _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 w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+19.1080P] 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 5953 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.1154 _refine_ls_wR_factor_gt 0.1115 _refine_ls_goodness_of_fit_ref 1.254 _refine_ls_restrained_S_all 1.254 _refine_ls_shift/su_max 0.146 _refine_ls_shift/su_mean 0.002 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re Re 0.043609(12) 0.06631(2) 0.109223(6) 0.03014(9) Uani 1 d . . . P P 0.09563(8) -0.13421(16) 0.15602(4) 0.0299(3) Uani 1 d . . . Cl1 Cl -0.04263(10) -0.10440(18) 0.06888(5) 0.0470(3) Uani 1 d . . . Cl2 Cl 0.13918(10) 0.24139(19) 0.14131(5) 0.0494(4) Uani 1 d . . . O2 O 0.1127(3) 0.0348(5) 0.07069(14) 0.0450(10) Uani 1 d . . . O1 O -0.0192(2) 0.1195(5) 0.14228(12) 0.0386(9) Uani 1 d . . . N1 N -0.0052(3) 0.2476(5) 0.06634(15) 0.0369(10) Uani 1 d . . . N2 N -0.0857(4) 0.4623(7) 0.0146(2) 0.0623(17) Uani 1 d . . . C1 C 0.0278(3) -0.2778(6) 0.16819(16) 0.0335(11) Uani 1 d . . . C2 C 0.0546(4) -0.4154(7) 0.1847(2) 0.0431(13) Uani 1 d . . . H2 H 0.1074 -0.4357 0.1881 0.052 Uiso 1 calc R . . C3 C 0.0040(5) -0.5223(8) 0.1961(2) 0.0530(17) Uani 1 d . . . H3 H 0.0221 -0.6158 0.2059 0.064 Uiso 1 calc R . . C4 C -0.0746(5) -0.4886(9) 0.1928(2) 0.060(2) Uani 1 d . . . H4 H -0.1089 -0.5580 0.2015 0.072 Uiso 1 calc R . . C5 C -0.1011(4) -0.3536(10) 0.1767(3) 0.0595(19) Uani 1 d . . . H5 H -0.1539 -0.3333 0.1737 0.071 Uiso 1 calc R . . C6 C -0.0516(4) -0.2470(8) 0.1647(2) 0.0456(14) Uani 1 d . . . H6 H -0.0706 -0.1547 0.1543 0.055 Uiso 1 calc R . . C7 C 0.1712(3) -0.2289(6) 0.13266(16) 0.0320(11) Uani 1 d . . . C8 C 0.2438(4) -0.1625(9) 0.1356(2) 0.0509(16) Uani 1 d . . . H8 H 0.2534 -0.0723 0.1499 0.061 Uiso 1 calc R . . C9 C 0.3013(4) -0.2302(10) 0.1172(3) 0.0600(19) Uani 1 d . . . H9 H 0.3501 -0.1863 0.1198 0.072 Uiso 1 calc R . . C10 C 0.2883(4) -0.3602(10) 0.0954(2) 0.0582(18) Uani 1 d . . . H10 H 0.3279 -0.4063 0.0835 0.070 Uiso 1 calc R . . C11 C 0.2151(5) -0.4231(8) 0.0911(2) 0.0563(18) Uani 1 d . . . H11 H 0.2053 -0.5103 0.0754 0.068 Uiso 1 calc R . . C12 C 0.1567(4) -0.3590(7) 0.10975(18) 0.0418(13) Uani 1 d . . . H12 H 0.1078 -0.4029 0.1069 0.050 Uiso 1 calc R . . C13 C 0.1388(4) -0.0773(6) 0.20830(17) 0.0360(12) Uani 1 d . . . C14 C 0.1015(4) 0.0326(8) 0.2291(2) 0.0479(15) Uani 1 d . . . H14 H 0.0585 0.0828 0.2154 0.057 Uiso 1 calc R . . C15 C 0.1291(5) 0.0662(9) 0.2702(2) 0.060(2) Uani 1 d . . . H15 H 0.1041 0.1383 0.2844 0.072 Uiso 1 calc R . . C16 C 0.1937(5) -0.0065(10) 0.2904(2) 0.061(2) Uani 1 d . . . H16 H 0.2121 0.0176 0.3180 0.073 Uiso 1 calc R . . C17 C 0.2303(5) -0.1130(10) 0.2702(2) 0.061(2) Uani 1 d . . . H17 H 0.2741 -0.1606 0.2838 0.074 Uiso 1 calc R . . C18 C 0.2026(4) -0.1507(9) 0.2293(2) 0.0531(17) Uani 1 d . . . H18 H 0.2270 -0.2257 0.2158 0.064 Uiso 1 calc R . . C19 C -0.0261(4) 0.2241(8) 0.02590(19) 0.0482(15) Uani 1 d . . . H19 H -0.0136 0.1332 0.0142 0.058 Uiso 1 calc R . . C20 C -0.0660(5) 0.3317(9) 0.0006(2) 0.0585(18) Uani 1 d . . . H20 H -0.0795 0.3103 -0.0276 0.070 Uiso 1 calc R . . C21 C -0.0637(4) 0.4865(8) 0.0552(2) 0.0519(16) Uani 1 d . . . H21 H -0.0759 0.5781 0.0666 0.062 Uiso 1 calc R . . C22 C -0.0236(4) 0.3821(7) 0.0810(2) 0.0417(13) Uani 1 d . . . H22 H -0.0090 0.4050 0.1091 0.050 Uiso 1 calc R . . C23 C 0.1747(7) 0.0943(15) 0.0520(4) 0.099(4) Uani 1 d . . . H23A H 0.1574 0.1881 0.0385 0.119 Uiso 1 calc R . . H23B H 0.2161 0.1187 0.0742 0.119 Uiso 1 calc R . . C24 C 0.2053(8) 0.008(3) 0.0235(5) 0.150(6) Uani 1 d . . . H24A H 0.2268 -0.0819 0.0367 0.225 Uiso 1 calc R . . H24B H 0.2452 0.0636 0.0124 0.225 Uiso 1 calc R . . H24C H 0.1654 -0.0179 0.0011 0.225 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re 0.03285(13) 0.02863(12) 0.02781(12) -0.00112(8) 0.00002(8) 0.00213(8) P 0.0305(6) 0.0295(6) 0.0286(6) -0.0013(5) -0.0001(5) 0.0013(5) Cl1 0.0549(9) 0.0404(7) 0.0422(8) -0.0085(6) -0.0062(6) -0.0048(6) Cl2 0.0523(8) 0.0441(8) 0.0481(8) -0.0010(7) -0.0066(7) -0.0136(7) O2 0.050(3) 0.048(2) 0.038(2) -0.0013(19) 0.0078(19) 0.006(2) O1 0.043(2) 0.040(2) 0.0324(19) -0.0020(17) 0.0020(16) 0.0074(18) N1 0.041(2) 0.034(2) 0.035(2) 0.0035(19) 0.0020(19) 0.004(2) N2 0.072(4) 0.050(3) 0.061(4) 0.020(3) -0.003(3) 0.008(3) C1 0.036(3) 0.038(3) 0.026(2) -0.002(2) 0.003(2) -0.002(2) C2 0.048(3) 0.041(3) 0.040(3) 0.006(2) 0.003(3) -0.001(3) C3 0.076(5) 0.041(3) 0.042(3) 0.003(3) 0.006(3) -0.009(3) C4 0.080(5) 0.054(4) 0.050(4) -0.005(3) 0.016(4) -0.028(4) C5 0.040(3) 0.067(5) 0.074(5) -0.007(4) 0.016(3) -0.006(3) C6 0.043(3) 0.047(3) 0.047(3) 0.007(3) 0.008(3) 0.005(3) C7 0.034(3) 0.035(3) 0.027(2) 0.004(2) 0.0041(19) 0.009(2) C8 0.045(3) 0.055(4) 0.052(4) -0.009(3) 0.006(3) -0.004(3) C9 0.039(3) 0.072(5) 0.071(5) 0.003(4) 0.015(3) 0.000(3) C10 0.057(4) 0.066(5) 0.056(4) 0.003(4) 0.022(3) 0.018(4) C11 0.075(5) 0.045(4) 0.051(4) -0.007(3) 0.016(4) 0.014(3) C12 0.045(3) 0.045(3) 0.034(3) -0.005(3) 0.003(2) 0.001(3) C13 0.041(3) 0.038(3) 0.028(2) 0.001(2) 0.000(2) -0.004(2) C14 0.058(4) 0.042(3) 0.043(3) -0.008(3) 0.005(3) 0.001(3) C15 0.082(6) 0.058(4) 0.041(4) -0.015(3) 0.014(4) -0.007(4) C16 0.082(5) 0.063(5) 0.033(3) -0.003(3) -0.004(3) -0.026(4) C17 0.065(5) 0.069(5) 0.043(4) 0.007(4) -0.020(3) -0.007(4) C18 0.058(4) 0.059(4) 0.038(3) 0.006(3) -0.009(3) 0.005(3) C19 0.065(4) 0.043(3) 0.034(3) 0.003(3) 0.000(3) 0.004(3) C20 0.070(5) 0.055(4) 0.046(4) 0.011(3) -0.007(3) 0.003(4) C21 0.067(4) 0.030(3) 0.057(4) 0.005(3) 0.006(3) 0.004(3) C22 0.045(3) 0.033(3) 0.045(3) -0.004(3) 0.002(3) 0.000(3) C23 0.092(8) 0.117(9) 0.097(8) -0.002(7) 0.046(7) -0.007(7) C24 0.081(8) 0.27(2) 0.102(10) -0.015(13) 0.036(8) -0.013(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re O1 1.697(4) . ? Re O2 1.867(5) . ? Re N1 2.219(5) . ? Re Cl1 2.3942(15) . ? Re Cl2 2.4099(15) . ? Re P 2.4318(14) . ? P C7 1.813(5) . ? P C1 1.820(6) . ? P C13 1.824(6) . ? O2 C23 1.411(12) . ? N1 C19 1.324(8) . ? N1 C22 1.341(8) . ? N2 C20 1.309(10) . ? N2 C21 1.332(10) . ? C1 C2 1.390(8) . ? C1 C6 1.400(8) . ? C2 C3 1.381(9) . ? C3 C4 1.393(12) . ? C4 C5 1.364(12) . ? C5 C6 1.373(10) . ? C7 C12 1.377(8) . ? C7 C8 1.389(9) . ? C8 C9 1.372(10) . ? C9 C10 1.357(12) . ? C10 C11 1.383(12) . ? C11 C12 1.376(10) . ? C13 C18 1.386(9) . ? C13 C14 1.396(9) . ? C14 C15 1.383(10) . ? C15 C16 1.383(12) . ? C16 C17 1.358(13) . ? C17 C18 1.385(9) . ? C19 C20 1.383(9) . ? C21 C22 1.374(9) . ? C23 C24 1.363(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Re O2 172.3(2) . . ? O1 Re N1 87.95(19) . . ? O2 Re N1 85.45(19) . . ? O1 Re Cl1 96.17(15) . . ? O2 Re Cl1 87.52(16) . . ? N1 Re Cl1 87.78(14) . . ? O1 Re Cl2 90.99(15) . . ? O2 Re Cl2 84.97(16) . . ? N1 Re Cl2 89.07(14) . . ? Cl1 Re Cl2 172.06(6) . . ? O1 Re P 91.82(14) . . ? O2 Re P 94.83(15) . . ? N1 Re P 179.28(13) . . ? Cl1 Re P 91.57(5) . . ? Cl2 Re P 91.62(5) . . ? C7 P C1 107.2(3) . . ? C7 P C13 106.4(3) . . ? C1 P C13 101.1(3) . . ? C7 P Re 108.24(17) . . ? C1 P Re 116.72(18) . . ? C13 P Re 116.37(19) . . ? C23 O2 Re 146.1(6) . . ? C19 N1 C22 116.3(5) . . ? C19 N1 Re 122.2(4) . . ? C22 N1 Re 121.1(4) . . ? C20 N2 C21 115.4(6) . . ? C2 C1 C6 118.7(6) . . ? C2 C1 P 120.3(4) . . ? C6 C1 P 120.7(5) . . ? C3 C2 C1 120.9(7) . . ? C2 C3 C4 119.3(7) . . ? C5 C4 C3 119.8(7) . . ? C4 C5 C6 121.4(7) . . ? C5 C6 C1 119.7(6) . . ? C12 C7 C8 119.6(5) . . ? C12 C7 P 121.4(4) . . ? C8 C7 P 118.8(5) . . ? C9 C8 C7 119.8(7) . . ? C10 C9 C8 121.2(7) . . ? C9 C10 C11 118.9(7) . . ? C12 C11 C10 121.2(7) . . ? C11 C12 C7 119.3(6) . . ? C18 C13 C14 119.4(6) . . ? C18 C13 P 121.6(5) . . ? C14 C13 P 118.6(5) . . ? C15 C14 C13 119.3(7) . . ? C14 C15 C16 120.5(7) . . ? C17 C16 C15 120.4(6) . . ? C16 C17 C18 120.1(7) . . ? C17 C18 C13 120.3(7) . . ? N1 C19 C20 121.5(6) . . ? N2 C20 C19 123.0(7) . . ? N2 C21 C22 122.9(7) . . ? N1 C22 C21 120.9(6) . . ? C24 C23 O2 118.2(13) . . ? 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 O1 Re P C7 -179.3(2) . . . . ? O2 Re P C7 -3.1(2) . . . . ? N1 Re P C7 109(11) . . . . ? Cl1 Re P C7 84.5(2) . . . . ? Cl2 Re P C7 -88.2(2) . . . . ? O1 Re P C1 59.8(2) . . . . ? O2 Re P C1 -124.1(2) . . . . ? N1 Re P C1 -11(11) . . . . ? Cl1 Re P C1 -36.4(2) . . . . ? Cl2 Re P C1 150.9(2) . . . . ? O1 Re P C13 -59.6(3) . . . . ? O2 Re P C13 116.5(3) . . . . ? N1 Re P C13 -131(11) . . . . ? Cl1 Re P C13 -155.8(2) . . . . ? Cl2 Re P C13 31.4(2) . . . . ? O1 Re O2 C23 36(2) . . . . ? N1 Re O2 C23 66.5(12) . . . . ? Cl1 Re O2 C23 154.5(12) . . . . ? Cl2 Re O2 C23 -23.0(12) . . . . ? P Re O2 C23 -114.2(12) . . . . ? O1 Re N1 C19 -132.2(5) . . . . ? O2 Re N1 C19 51.7(5) . . . . ? Cl1 Re N1 C19 -36.0(5) . . . . ? Cl2 Re N1 C19 136.7(5) . . . . ? P Re N1 C19 -61(11) . . . . ? O1 Re N1 C22 39.7(5) . . . . ? O2 Re N1 C22 -136.3(5) . . . . ? Cl1 Re N1 C22 136.0(5) . . . . ? Cl2 Re N1 C22 -51.3(5) . . . . ? P Re N1 C22 111(11) . . . . ? C7 P C1 C2 40.8(5) . . . . ? C13 P C1 C2 -70.4(5) . . . . ? Re P C1 C2 162.3(4) . . . . ? C7 P C1 C6 -145.0(5) . . . . ? C13 P C1 C6 103.8(5) . . . . ? Re P C1 C6 -23.5(5) . . . . ? C6 C1 C2 C3 2.3(9) . . . . ? P C1 C2 C3 176.6(5) . . . . ? C1 C2 C3 C4 -3.0(10) . . . . ? C2 C3 C4 C5 2.9(11) . . . . ? C3 C4 C5 C6 -2.1(12) . . . . ? C4 C5 C6 C1 1.4(11) . . . . ? C2 C1 C6 C5 -1.5(10) . . . . ? P C1 C6 C5 -175.7(5) . . . . ? C1 P C7 C12 30.2(5) . . . . ? C13 P C7 C12 137.7(5) . . . . ? Re P C7 C12 -96.5(5) . . . . ? C1 P C7 C8 -154.5(5) . . . . ? C13 P C7 C8 -46.9(5) . . . . ? Re P C7 C8 78.9(5) . . . . ? C12 C7 C8 C9 -2.9(10) . . . . ? P C7 C8 C9 -178.3(6) . . . . ? C7 C8 C9 C10 1.3(12) . . . . ? C8 C9 C10 C11 1.2(12) . . . . ? C9 C10 C11 C12 -2.2(12) . . . . ? C10 C11 C12 C7 0.7(11) . . . . ? C8 C7 C12 C11 1.9(9) . . . . ? P C7 C12 C11 177.2(5) . . . . ? C7 P C13 C18 -24.1(6) . . . . ? C1 P C13 C18 87.7(6) . . . . ? Re P C13 C18 -144.8(5) . . . . ? C7 P C13 C14 162.5(5) . . . . ? C1 P C13 C14 -85.7(5) . . . . ? Re P C13 C14 41.8(6) . . . . ? C18 C13 C14 C15 0.1(10) . . . . ? P C13 C14 C15 173.6(6) . . . . ? C13 C14 C15 C16 1.0(11) . . . . ? C14 C15 C16 C17 -0.6(13) . . . . ? C15 C16 C17 C18 -0.8(13) . . . . ? C16 C17 C18 C13 1.9(13) . . . . ? C14 C13 C18 C17 -1.5(11) . . . . ? P C13 C18 C17 -174.8(6) . . . . ? C22 N1 C19 C20 -1.3(10) . . . . ? Re N1 C19 C20 171.0(6) . . . . ? C21 N2 C20 C19 1.0(12) . . . . ? N1 C19 C20 N2 0.0(13) . . . . ? C20 N2 C21 C22 -0.6(12) . . . . ? C19 N1 C22 C21 1.6(9) . . . . ? Re N1 C22 C21 -170.8(5) . . . . ? N2 C21 C22 N1 -0.7(11) . . . . ? Re O2 C23 C24 178.4(10) . . . . ? _refine_diff_density_max 1.080 _refine_diff_density_min -1.100 _refine_diff_density_rms 0.155 #===END data_7 _database_code_CSD 153391 _audit_creation_method SHELXL _chemical_name_systematic ; trans-dioxo-tetrakis(1,4-pyrazine)-rhenium(V) sodium bis(exafluorophosphate) dihydrate ; _chemical_name_common ? _chemical_formula_moiety '((C4 H4 N2)4 O2 Re 1+), (Na 1+), 2(P F6 1-), 2(H2 O)' _chemical_formula_structural '((C4 H4 N2)4 O2 Re) (P F6) (Na P F6 ) 2(H2 O)' _chemical_formula_analytical ? _chemical_formula_sum 'C16 H20 F12 N8 Na O4 P2 Re' _chemical_formula_weight 887.53 _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' 'P' 'P' 0.1023 0.0942 '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' 'N' 'N' 0.0061 0.0033 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 2/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 9.243(1) _cell_length_b 14.793(2) _cell_length_c 10.560(1) _cell_angle_alpha 90.00 _cell_angle_beta 95.94(2) _cell_angle_gamma 90.00 _cell_volume 1436.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 17 _exptl_crystal_description ? _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.052 _exptl_crystal_density_method ? _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 4.476 _exptl_absorpt_correction_type 'psi scan' _exptl_absorpt_correction_T_min 0.7206 _exptl_absorpt_correction_T_max 1.0000 _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_type 'Enraf Nonius CAD4' _diffrn_measurement_method '\w/2\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 3 _diffrn_standards_decay_corr_max 1.088 _diffrn_standards_decay_corr_min 1.000 _diffrn_reflns_number 4187 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 29.97 _reflns_number_total 4187 _reflns_number_observed 3451 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 (Enraf-Nonius)' _computing_cell_refinement 'CELDIM (Enraf-Nonius)' _computing_data_reduction 'WinGX 1.63 (Farrugia, 1999)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3/Windows (Farrugia,1997)' _computing_publication_material 'WinGX 1.63 (Farrugia, 1999)' _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^)+(0.0617P)^2^] 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_number_reflns 4187 _refine_ls_number_parameters 206 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_obs 0.0396 _refine_ls_wR_factor_all 0.0993 _refine_ls_wR_factor_obs 0.0955 _refine_ls_goodness_of_fit_all 1.033 _refine_ls_goodness_of_fit_obs 1.100 _refine_ls_restrained_S_all 1.033 _refine_ls_restrained_S_obs 1.100 _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 Re Re 0.7500 0.73388(2) 0.7500 0.02414(9) Uani 1 d S . O1 O 0.8905(4) 0.7358(2) 0.8751(3) 0.0325(7) Uani 1 d . . N1 N 0.9058(4) 0.7351(3) 0.6135(4) 0.0291(7) Uani 1 d . . N2 N 1.1027(6) 0.7446(3) 0.4318(5) 0.0477(12) Uani 1 d . . N3 N 0.7500 0.5894(4) 0.7500 0.0282(11) Uani 1 d S . N4 N 0.7500 0.4014(4) 0.7500 0.045(2) Uani 1 d S . N5 N 0.7500 0.8789(4) 0.7500 0.0309(12) Uani 1 d S . N6 N 0.7500 1.0663(4) 0.7500 0.046(2) Uani 1 d S . C1 C 1.0362(7) 0.7717(4) 0.6401(5) 0.0478(14) Uani 1 d . . H1 H 1.0636(7) 0.7941(4) 0.7214(5) 0.057 Uiso 1 calc R . C2 C 1.1317(7) 0.7767(5) 0.5480(6) 0.053(2) Uani 1 d . . H2 H 1.2214(7) 0.8043(5) 0.5691(6) 0.064 Uiso 1 calc R . C3 C 0.9740(7) 0.7062(5) 0.4092(6) 0.055(2) Uani 1 d . . H3 H 0.9487(7) 0.6809(5) 0.3293(6) 0.065 Uiso 1 calc R . C4 C 0.8756(6) 0.7016(5) 0.4974(5) 0.0477(14) Uani 1 d . . H4 H 0.7859(6) 0.6744(5) 0.4754(5) 0.057 Uiso 1 calc R . C5 C 0.8301(7) 0.5416(4) 0.8384(6) 0.052(2) Uani 1 d . . H5 H 0.8899(7) 0.5715(4) 0.9012(6) 0.062 Uiso 1 calc R . C6 C 0.8255(8) 0.4493(4) 0.8379(7) 0.060(2) Uani 1 d . . H6 H 0.8790(8) 0.4187(4) 0.9039(7) 0.072 Uiso 1 calc R . C7 C 0.7821(8) 0.9265(4) 0.8559(5) 0.049(2) Uani 1 d . . H7 H 0.8047(8) 0.8964(4) 0.9327(5) 0.059 Uiso 1 calc R . C8 C 0.7824(9) 1.0193(4) 0.8538(6) 0.059(2) Uani 1 d . . H8 H 0.8067(9) 1.0502(4) 0.9298(6) 0.071 Uiso 1 calc R . P1 P 0.7500 0.96558(15) 0.2500 0.0488(6) Uani 1 d S . P2 P 0.7500 0.4727(2) 0.2500 0.0620(7) Uani 1 d S . Na Na 0.7500 0.2365(2) 0.7500 0.0310(5) Uani 1 d S . F6 F 0.8910(7) 0.4732(5) 0.3471(7) 0.121(2) Uani 1 d . . F4 F 0.8215(7) 0.5467(5) 0.1670(6) 0.116(2) Uani 1 d . . F5 F 0.8200(8) 0.3978(5) 0.1711(8) 0.131(3) Uani 1 d . . F3 F 0.8666(10) 0.9695(9) 0.3559(9) 0.188(5) Uani 1 d . . F2 F 0.8275(14) 0.9043(9) 0.1760(9) 0.239(7) Uani 1 d . . F1 F 0.8216(15) 1.0398(10) 0.1857(10) 0.238(7) Uani 1 d . . OW O 0.9619(6) 0.2232(4) 0.8899(5) 0.0676(15) Uani 1 d G . H9 H 0.9927(76) 0.2414(45) 0.9732(27) 0.081 Uiso 1 d G . H10 H 1.0324(58) 0.1854(46) 0.8606(60) 0.081 Uiso 1 d G . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re 0.02963(13) 0.02225(12) 0.02114(12) 0.000 0.00553(8) 0.000 O1 0.038(2) 0.031(2) 0.028(2) -0.0015(13) 0.0039(13) 0.0022(14) N1 0.034(2) 0.028(2) 0.027(2) -0.0014(15) 0.0099(15) -0.001(2) N2 0.048(3) 0.053(3) 0.045(3) -0.005(2) 0.024(2) -0.005(2) N3 0.030(3) 0.030(3) 0.026(3) 0.000 0.008(2) 0.000 N4 0.057(4) 0.026(3) 0.053(4) 0.000 0.012(3) 0.000 N5 0.045(3) 0.019(3) 0.029(3) 0.000 0.005(2) 0.000 N6 0.072(5) 0.023(3) 0.043(4) 0.000 0.000(3) 0.000 C1 0.044(3) 0.070(4) 0.032(3) -0.014(2) 0.013(2) -0.020(3) C2 0.046(3) 0.071(5) 0.045(3) -0.007(3) 0.018(3) -0.022(3) C3 0.058(4) 0.070(4) 0.038(3) -0.021(3) 0.019(3) -0.018(3) C4 0.048(3) 0.064(4) 0.033(3) -0.017(3) 0.013(2) -0.017(3) C5 0.061(4) 0.036(3) 0.054(4) 0.001(3) -0.018(3) 0.004(3) C6 0.078(5) 0.029(3) 0.068(4) 0.005(3) -0.021(4) 0.007(3) C7 0.089(5) 0.027(3) 0.029(3) -0.001(2) -0.004(3) 0.002(3) C8 0.108(6) 0.032(3) 0.037(3) -0.006(2) 0.000(3) 0.004(3) P1 0.071(2) 0.0311(11) 0.0506(13) 0.000 0.0360(12) 0.000 P2 0.074(2) 0.0443(15) 0.066(2) 0.000 0.0012(14) 0.000 Na 0.0354(13) 0.0267(12) 0.0318(13) 0.000 0.0089(10) 0.000 F6 0.091(4) 0.148(6) 0.111(5) 0.017(4) -0.043(4) -0.004(4) F4 0.117(5) 0.118(5) 0.112(5) 0.049(4) 0.014(4) -0.008(4) F5 0.131(6) 0.108(6) 0.158(7) -0.035(5) 0.026(5) 0.021(4) F3 0.125(7) 0.312(15) 0.125(7) 0.019(8) 0.010(6) 0.011(8) F2 0.294(14) 0.286(15) 0.137(8) -0.058(8) 0.025(7) 0.193(12) F1 0.303(17) 0.247(14) 0.152(10) 0.066(8) -0.040(9) -0.116(13) OW 0.056(3) 0.085(4) 0.056(3) -0.022(3) -0.023(2) 0.019(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 Re O1 1.755(4) . ? Re O1 1.755(4) 2_656 ? Re N3 2.138(6) . ? Re N1 2.141(4) . ? Re N1 2.141(4) 2_656 ? Re N5 2.145(6) . ? N1 C1 1.324(7) . ? N1 C4 1.325(6) . ? N2 C2 1.317(8) . ? N2 C3 1.318(8) . ? N2 Na 2.482(5) 3_766 ? N3 C5 1.332(6) 2_656 ? N3 C5 1.332(6) . ? N4 C6 1.310(8) . ? N4 C6 1.310(7) 2_656 ? N4 Na 2.439(7) . ? N5 C7 1.329(6) . ? N5 C7 1.329(6) 2_656 ? N6 C8 1.306(7) 2_656 ? N6 C8 1.306(7) . ? N6 Na 2.518(7) 1_565 ? C1 C2 1.383(8) . ? C3 C4 1.369(8) . ? C5 C6 1.367(9) . ? C7 C8 1.374(8) . ? P1 F2 1.436(7) 2_655 ? P1 F2 1.436(7) . ? P1 F3 1.472(9) 2_655 ? P1 F3 1.472(9) . ? P1 F1 1.483(11) . ? P1 F1 1.483(10) 2_655 ? P2 F5 1.566(7) . ? P2 F5 1.566(7) 2_655 ? P2 F6 1.573(6) . ? P2 F6 1.573(6) 2_655 ? P2 F4 1.588(6) 2_655 ? P2 F4 1.588(6) . ? Na OW 2.336(4) . ? Na OW 2.336(4) 2_656 ? Na N2 2.482(5) 4_566 ? Na N2 2.482(5) 3_766 ? Na N6 2.518(7) 1_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Re O1 178.1(2) . 2_656 ? O1 Re N3 90.95(11) . . ? O1 Re N3 90.95(11) 2_656 . ? O1 Re N1 90.6(2) . . ? O1 Re N1 89.4(2) 2_656 . ? N3 Re N1 90.49(11) . . ? O1 Re N1 89.4(2) . 2_656 ? O1 Re N1 90.6(2) 2_656 2_656 ? N3 Re N1 90.49(11) . 2_656 ? N1 Re N1 179.0(2) . 2_656 ? O1 Re N5 89.05(11) . . ? O1 Re N5 89.05(11) 2_656 . ? N3 Re N5 180.000(1) . . ? N1 Re N5 89.51(11) . . ? N1 Re N5 89.51(11) 2_656 . ? C1 N1 C4 116.7(4) . . ? C1 N1 Re 121.4(3) . . ? C4 N1 Re 121.9(4) . . ? C2 N2 C3 114.7(5) . . ? C2 N2 Na 127.2(4) . 3_766 ? C3 N2 Na 117.7(4) . 3_766 ? C5 N3 C5 116.0(7) 2_656 . ? C5 N3 Re 122.0(3) 2_656 . ? C5 N3 Re 122.0(4) . . ? C6 N4 C6 114.6(7) . 2_656 ? C6 N4 Na 122.7(4) . . ? C6 N4 Na 122.7(4) 2_656 . ? C7 N5 C7 116.0(6) . 2_656 ? C7 N5 Re 122.0(3) . . ? C7 N5 Re 122.0(3) 2_656 . ? C8 N6 C8 115.7(7) 2_656 . ? C8 N6 Na 122.1(4) 2_656 1_565 ? C8 N6 Na 122.1(4) . 1_565 ? N1 C1 C2 120.4(5) . . ? N2 C2 C1 123.6(6) . . ? N2 C3 C4 123.2(5) . . ? N1 C4 C3 121.3(5) . . ? N3 C5 C6 120.8(6) . . ? N4 C6 C5 123.9(6) . . ? N5 C7 C8 121.1(5) . . ? N6 C8 C7 123.0(6) . . ? F2 P1 F2 101.6(13) 2_655 . ? F2 P1 F3 94.1(6) 2_655 2_655 ? F2 P1 F3 88.8(6) . 2_655 ? F2 P1 F3 88.8(6) 2_655 . ? F2 P1 F3 94.1(6) . . ? F3 P1 F3 175.4(10) 2_655 . ? F2 P1 F1 171.3(10) 2_655 . ? F2 P1 F1 87.0(8) . . ? F3 P1 F1 87.1(6) 2_655 . ? F3 P1 F1 89.6(6) . . ? F2 P1 F1 87.0(8) 2_655 2_655 ? F2 P1 F1 171.3(10) . 2_655 ? F3 P1 F1 89.6(6) 2_655 2_655 ? F3 P1 F1 87.1(6) . 2_655 ? F1 P1 F1 84.4(13) . 2_655 ? F5 P2 F5 89.9(7) . 2_655 ? F5 P2 F6 89.4(4) . . ? F5 P2 F6 91.0(4) 2_655 . ? F5 P2 F6 91.0(4) . 2_655 ? F5 P2 F6 89.4(4) 2_655 2_655 ? F6 P2 F6 179.4(6) . 2_655 ? F5 P2 F4 178.4(5) . 2_655 ? F5 P2 F4 88.6(4) 2_655 2_655 ? F6 P2 F4 90.1(4) . 2_655 ? F6 P2 F4 89.5(4) 2_655 2_655 ? F5 P2 F4 88.6(4) . . ? F5 P2 F4 178.4(5) 2_655 . ? F6 P2 F4 89.6(4) . . ? F6 P2 F4 90.1(4) 2_655 . ? F4 P2 F4 92.9(6) 2_655 . ? OW Na OW 170.3(3) . 2_656 ? OW Na N4 94.9(2) . . ? OW Na N4 94.9(2) 2_656 . ? OW Na N2 90.6(2) . 4_566 ? OW Na N2 90.4(2) 2_656 4_566 ? N4 Na N2 83.55(13) . 4_566 ? OW Na N2 90.4(2) . 3_766 ? OW Na N2 90.6(2) 2_656 3_766 ? N4 Na N2 83.55(13) . 3_766 ? N2 Na N2 167.1(3) 4_566 3_766 ? OW Na N6 85.1(2) . 1_545 ? OW Na N6 85.1(2) 2_656 1_545 ? N4 Na N6 180.0 . 1_545 ? N2 Na N6 96.45(13) 4_566 1_545 ? N2 Na N6 96.45(13) 3_766 1_545 ? 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 C1 N1 N1 C4 -54.7(5) . . 2_656 2_656 ? C5 N3 N5 C7 -25.5(5) . . . . ? _refine_diff_density_max 2.238 _refine_diff_density_min -1.321 _refine_diff_density_rms 0.166