# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Andrew Gaunt' _publ_contact_author_address ; C-IIAC, Chemistry Division Los Alamos National Laboratory Los Alamos National Laboratory Mail Stop J-514 Los Alamos New Mexico 87545 UNITED STATES OF AMERICA ; _publ_contact_author_email GAUNT@LANL.GOV _publ_section_title ; An entry route into non-aqueous plutonyl coordination chemistry ; loop_ _publ_author_name A.Gaunt T.W.Hayton M.Neu S.D.Reilly B.L.Scott data_apx360a _database_code_depnum_ccdc_archive 'CCDC 631420' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H16 Cl2 O4 Pu' _chemical_formula_weight 486.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pu Pu -9.4100 4.3056 '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 7.063(3) _cell_length_b 9.720(3) _cell_length_c 10.189(4) _cell_angle_alpha 78.691(4) _cell_angle_beta 79.847(4) _cell_angle_gamma 81.777(3) _cell_volume 670.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 141(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448 _exptl_absorpt_coefficient_mu 5.303 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.23 _exptl_absorpt_correction_T_max 0.73 _exptl_absorpt_process_details 'SADABS 2.03 (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 141(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker D8 with APEXII CCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% '< 2' _diffrn_reflns_number 6571 _diffrn_reflns_av_R_equivalents 0.0698 _diffrn_reflns_av_sigmaI/netI 0.0958 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.35 _reflns_number_total 2452 _reflns_number_gt 1873 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 1.08 (Bruker AXS, 2003)' _computing_cell_refinement 'SAINT+, v. 7.06 (Bruker AXS, 2001)' _computing_data_reduction 'SAINT+, v. 7.06 (Bruker AXS, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.10, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.10, (Bruker AXS, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0512P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2452 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0820 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1132 _refine_ls_wR_factor_gt 0.1038 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pu1 Pu 0.10746(8) 0.86972(6) 0.19092(5) 0.02180(19) Uani 1 1 d . . . Cl1 Cl 0.1157(5) 1.1286(4) 0.0110(4) 0.0324(9) Uani 1 1 d . . . Cl2 Cl 0.2476(6) 0.7177(4) 0.4049(4) 0.0425(10) Uani 1 1 d . . . C1 C 0.232(2) 1.0841(18) 0.3948(16) 0.042(4) Uani 1 1 d . . . H1A H 0.2477 1.0081 0.4708 0.050 Uiso 1 1 calc R . . H1B H 0.0995 1.1287 0.4068 0.050 Uiso 1 1 calc R . . C2 C 0.370(2) 1.1885(19) 0.3851(18) 0.048(5) Uani 1 1 d . . . H2A H 0.3005 1.2820 0.3870 0.057 Uiso 1 1 calc R . . H2B H 0.4423 1.1637 0.4604 0.057 Uiso 1 1 calc R . . C3 C 0.503(3) 1.1861(19) 0.2544(17) 0.050(5) Uani 1 1 d . . . H3A H 0.6350 1.1909 0.2653 0.060 Uiso 1 1 calc R . . H3B H 0.4644 1.2642 0.1855 0.060 Uiso 1 1 calc R . . C4 C 0.481(2) 1.0461(19) 0.2178(19) 0.052(5) Uani 1 1 d . . . H4A H 0.5125 1.0488 0.1208 0.062 Uiso 1 1 calc R . . H4B H 0.5642 0.9699 0.2632 0.062 Uiso 1 1 calc R . . C5 C -0.237(2) 0.6297(18) 0.2851(18) 0.049(5) Uani 1 1 d . . . H5A H -0.3248 0.7099 0.2519 0.059 Uiso 1 1 calc R . . H5B H -0.2558 0.6155 0.3832 0.059 Uiso 1 1 calc R . . C6 C -0.268(3) 0.503(2) 0.2382(19) 0.057(5) Uani 1 1 d . . . H6A H -0.3063 0.5265 0.1490 0.069 Uiso 1 1 calc R . . H6B H -0.3667 0.4534 0.3005 0.069 Uiso 1 1 calc R . . C7 C -0.075(3) 0.414(2) 0.234(2) 0.070(6) Uani 1 1 d . . . H7A H -0.0571 0.3611 0.3230 0.085 Uiso 1 1 calc R . . H7B H -0.0607 0.3495 0.1708 0.085 Uiso 1 1 calc R . . C8 C 0.065(2) 0.5261(18) 0.1863(19) 0.051(5) Uani 1 1 d . . . H8A H 0.1819 0.4973 0.2266 0.061 Uiso 1 1 calc R . . H8B H 0.0993 0.5405 0.0885 0.061 Uiso 1 1 calc R . . O1 O 0.3081(14) 0.8030(11) 0.0918(9) 0.033(2) Uani 1 1 d . . . O2 O -0.0935(13) 0.9365(10) 0.2918(10) 0.031(2) Uani 1 1 d . . . O3 O 0.2776(13) 1.0292(10) 0.2657(9) 0.029(2) Uani 1 1 d . . . O4 O -0.0339(14) 0.6522(11) 0.2283(10) 0.035(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pu1 0.0229(3) 0.0272(3) 0.0170(3) -0.0058(2) -0.00272(19) -0.0062(2) Cl1 0.046(2) 0.027(2) 0.028(2) -0.0015(16) -0.0122(17) -0.0134(17) Cl2 0.044(2) 0.047(3) 0.037(2) 0.0024(19) -0.0130(19) -0.010(2) C1 0.036(9) 0.058(12) 0.032(9) -0.019(8) 0.001(8) 0.004(8) C2 0.034(10) 0.050(12) 0.062(12) -0.014(9) -0.013(9) -0.004(8) C3 0.057(11) 0.051(12) 0.042(11) -0.016(9) 0.015(9) -0.026(9) C4 0.037(10) 0.058(13) 0.061(12) -0.017(10) 0.009(9) -0.022(9) C5 0.039(10) 0.047(11) 0.058(12) -0.022(9) 0.026(9) -0.019(8) C6 0.063(13) 0.061(13) 0.055(12) -0.021(10) -0.003(10) -0.023(11) C7 0.099(17) 0.049(13) 0.057(13) -0.015(10) 0.029(12) -0.030(12) C8 0.049(11) 0.046(11) 0.060(12) -0.023(9) -0.001(9) -0.001(9) O1 0.034(6) 0.040(7) 0.024(6) -0.006(5) -0.007(5) 0.002(5) O2 0.032(6) 0.025(6) 0.041(6) -0.009(5) -0.016(5) 0.000(5) O3 0.027(5) 0.037(6) 0.022(5) 0.000(5) -0.003(4) -0.009(5) O4 0.035(6) 0.035(6) 0.040(7) -0.021(5) -0.004(5) -0.001(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 Pu1 O2 1.725(9) . ? Pu1 O1 1.714(9) . ? Pu1 O3 2.397(9) . ? Pu1 O4 2.401(10) . ? Pu1 Cl2 2.645(4) . ? Pu1 Cl1 2.810(4) . ? Pu1 Cl1 2.800(4) 2_575 ? Cl1 Pu1 2.800(4) 2_575 ? C1 O3 1.482(16) . ? C1 C2 1.48(2) . ? C2 C3 1.49(2) . ? C3 C4 1.51(2) . ? C4 O3 1.458(17) . ? C5 O4 1.477(17) . ? C5 C6 1.46(2) . ? C6 C7 1.50(3) . ? C7 C8 1.53(2) . ? C8 O4 1.424(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 O2 Pu1 O1 179.5(5) . . ? O2 Pu1 O3 85.6(4) . . ? O1 Pu1 O3 94.1(4) . . ? O2 Pu1 O4 88.3(4) . . ? O1 Pu1 O4 91.7(4) . . ? O3 Pu1 O4 150.8(3) . . ? O2 Pu1 Cl2 91.5(3) . . ? O1 Pu1 Cl2 88.1(3) . . ? O3 Pu1 Cl2 75.7(2) . . ? O4 Pu1 Cl2 75.9(3) . . ? O2 Pu1 Cl1 91.1(3) . . ? O1 Pu1 Cl1 89.1(3) . . ? O3 Pu1 Cl1 68.6(2) . . ? O4 Pu1 Cl1 140.2(3) . . ? Cl2 Pu1 Cl1 143.91(11) . . ? O2 Pu1 Cl1 90.5(3) . 2_575 ? O1 Pu1 Cl1 89.9(3) . 2_575 ? O3 Pu1 Cl1 138.8(2) . 2_575 ? O4 Pu1 Cl1 69.6(3) . 2_575 ? Cl2 Pu1 Cl1 145.38(12) . 2_575 ? Cl1 Pu1 Cl1 70.55(11) . 2_575 ? Pu1 Cl1 Pu1 109.45(11) . 2_575 ? O3 C1 C2 106.0(12) . . ? C3 C2 C1 107.0(13) . . ? C2 C3 C4 103.7(13) . . ? O3 C4 C3 103.2(13) . . ? O4 C5 C6 104.6(13) . . ? C5 C6 C7 104.5(15) . . ? C8 C7 C6 101.8(15) . . ? O4 C8 C7 106.3(14) . . ? C4 O3 C1 105.2(11) . . ? C4 O3 Pu1 123.4(9) . . ? C1 O3 Pu1 127.7(8) . . ? C5 O4 C8 109.1(11) . . ? C5 O4 Pu1 126.8(8) . . ? C8 O4 Pu1 123.9(9) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.704 _refine_diff_density_min -2.816 _refine_diff_density_rms 0.337