# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_apx1716a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H20 Cl4 Np O4' _chemical_formula_weight 559.06 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' Np Np -11.4937 4.1493 '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/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.509(3) _cell_length_b 7.2429(12) _cell_length_c 14.850(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.662(2) _cell_angle_gamma 90.00 _cell_volume 1600.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 7.159 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3285 _exptl_absorpt_correction_T_max 0.6733 _exptl_absorpt_process_details 'SADABS v. 1 (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _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_detector_area_resol_mean ? _diffrn_reflns_number 17379 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 28.43 _reflns_number_total 3808 _reflns_number_gt 3246 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 7.0 (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_data_reduction 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.14, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.14, (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^)+(0.0203P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3808 _refine_ls_number_parameters 158 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0219 _refine_ls_wR_factor_ref 0.0433 _refine_ls_wR_factor_gt 0.0408 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Np1 Np 0.248687(8) 0.526121(17) 0.278953(9) 0.01329(4) Uani 1 1 d . . . Cl1 Cl 0.34093(6) 0.70171(13) 0.20098(7) 0.0245(2) Uani 1 1 d . . . Cl2 Cl 0.36195(6) 0.44648(12) 0.46307(6) 0.02295(19) Uani 1 1 d . . . Cl3 Cl 0.16893(6) 0.22605(12) 0.29116(7) 0.0249(2) Uani 1 1 d . . . Cl4 Cl 0.11428(6) 0.72543(12) 0.15599(6) 0.02430(19) Uani 1 1 d . . . O1 O 0.15519(16) 0.6137(3) 0.37208(18) 0.0243(6) Uani 1 1 d . . . O2 O 0.29331(16) 0.8272(3) 0.37301(17) 0.0233(6) Uani 1 1 d . . . O3 O 0.19626(14) 0.3518(3) 0.11173(16) 0.0201(5) Uani 1 1 d . . . O4 O 0.36190(14) 0.2998(3) 0.26617(17) 0.0186(5) Uani 1 1 d . . . C1 C 0.0636(3) 0.5568(6) 0.3433(4) 0.0410(11) Uani 1 1 d . . . H1A H 0.0494 0.5696 0.3993 0.061 Uiso 1 1 calc R . . H1B H 0.0565 0.4302 0.3223 0.061 Uiso 1 1 calc R . . H1C H 0.0238 0.6329 0.2893 0.061 Uiso 1 1 calc R . . C2 C 0.1648(3) 0.8028(5) 0.4053(3) 0.0338(10) Uani 1 1 d . . . H2A H 0.1426 0.8163 0.4557 0.041 Uiso 1 1 calc R . . H2B H 0.1297 0.8828 0.3496 0.041 Uiso 1 1 calc R . . C3 C 0.2605(3) 0.8561(6) 0.4475(3) 0.0341(10) Uani 1 1 d . . . H3A H 0.2671 0.9850 0.4672 0.041 Uiso 1 1 calc R . . H3B H 0.2950 0.7822 0.5062 0.041 Uiso 1 1 calc R . . C4 C 0.3816(3) 0.9085(6) 0.4087(3) 0.0365(10) Uani 1 1 d . . . H4A H 0.3787 1.0361 0.4245 0.055 Uiso 1 1 calc R . . H4B H 0.4025 0.8991 0.3579 0.055 Uiso 1 1 calc R . . H4C H 0.4222 0.8442 0.4675 0.055 Uiso 1 1 calc R . . C5 C 0.1031(2) 0.3210(6) 0.0446(3) 0.0303(9) Uani 1 1 d . . . H5A H 0.0971 0.3070 -0.0223 0.045 Uiso 1 1 calc R . . H5B H 0.0679 0.4244 0.0473 0.045 Uiso 1 1 calc R . . H5C H 0.0824 0.2110 0.0640 0.045 Uiso 1 1 calc R . . C6 C 0.2456(2) 0.1852(5) 0.1155(3) 0.0247(8) Uani 1 1 d . . . H6A H 0.2309 0.1420 0.0484 0.030 Uiso 1 1 calc R . . H6B H 0.2300 0.0891 0.1507 0.030 Uiso 1 1 calc R . . C7 C 0.3433(2) 0.2284(5) 0.1687(3) 0.0239(8) Uani 1 1 d . . . H7A H 0.3783 0.1177 0.1750 0.029 Uiso 1 1 calc R . . H7B H 0.3594 0.3191 0.1312 0.029 Uiso 1 1 calc R . . C8 C 0.4579(2) 0.3270(6) 0.3207(3) 0.0296(9) Uani 1 1 d . . . H8A H 0.4881 0.2106 0.3287 0.044 Uiso 1 1 calc R . . H8B H 0.4713 0.3784 0.3852 0.044 Uiso 1 1 calc R . . H8C H 0.4781 0.4102 0.2842 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Np1 0.01166(6) 0.01573(7) 0.01227(7) 0.00095(5) 0.00499(5) -0.00066(5) Cl1 0.0264(5) 0.0293(5) 0.0227(5) 0.0011(4) 0.0153(4) -0.0058(4) Cl2 0.0219(4) 0.0298(5) 0.0144(4) 0.0040(3) 0.0053(3) 0.0023(4) Cl3 0.0228(4) 0.0203(5) 0.0349(5) 0.0008(4) 0.0155(4) -0.0039(3) Cl4 0.0206(4) 0.0256(5) 0.0207(4) 0.0010(3) 0.0033(4) 0.0062(4) O1 0.0288(14) 0.0229(14) 0.0290(14) 0.0042(11) 0.0199(12) 0.0057(11) O2 0.0279(14) 0.0237(14) 0.0159(13) -0.0039(10) 0.0072(11) -0.0035(11) O3 0.0134(12) 0.0239(14) 0.0173(12) -0.0033(10) 0.0013(10) 0.0015(10) O4 0.0116(11) 0.0276(14) 0.0156(12) -0.0004(10) 0.0048(10) 0.0012(10) C1 0.029(2) 0.045(3) 0.061(3) 0.012(2) 0.031(2) 0.009(2) C2 0.055(3) 0.026(2) 0.036(2) 0.0003(17) 0.034(2) 0.0104(19) C3 0.057(3) 0.027(2) 0.021(2) -0.0046(16) 0.019(2) 0.0054(19) C4 0.036(2) 0.030(2) 0.030(2) -0.0010(18) 0.0020(19) -0.0127(19) C5 0.0171(19) 0.036(2) 0.025(2) -0.0103(17) -0.0027(16) -0.0003(16) C6 0.025(2) 0.026(2) 0.0226(19) -0.0084(15) 0.0092(16) 0.0026(16) C7 0.0218(19) 0.033(2) 0.0194(19) -0.0037(15) 0.0110(16) 0.0056(16) C8 0.0125(18) 0.046(3) 0.029(2) 0.0037(18) 0.0085(16) 0.0021(16) _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 Np1 O2 2.522(2) . ? Np1 O4 2.554(2) . ? Np1 O1 2.559(2) . ? Np1 O3 2.578(2) . ? Np1 Cl3 2.5878(9) . ? Np1 Cl1 2.6085(9) . ? Np1 Cl4 2.6139(9) . ? Np1 Cl2 2.6224(9) . ? O1 C2 1.441(4) . ? O1 C1 1.442(5) . ? O2 C3 1.442(4) . ? O2 C4 1.442(4) . ? O3 C5 1.442(4) . ? O3 C6 1.444(4) . ? O4 C7 1.440(4) . ? O4 C8 1.448(4) . ? C2 C3 1.477(6) . ? C6 C7 1.489(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 O2 Np1 O4 123.27(8) . . ? O2 Np1 O1 65.55(8) . . ? O4 Np1 O1 146.25(8) . . ? O2 Np1 O3 148.50(8) . . ? O4 Np1 O3 64.24(7) . . ? O1 Np1 O3 127.77(8) . . ? O2 Np1 Cl3 136.30(6) . . ? O4 Np1 Cl3 82.95(6) . . ? O1 Np1 Cl3 74.10(6) . . ? O3 Np1 Cl3 71.79(6) . . ? O2 Np1 Cl1 74.78(6) . . ? O4 Np1 Cl1 72.13(6) . . ? O1 Np1 Cl1 136.37(6) . . ? O3 Np1 Cl1 80.11(6) . . ? Cl3 Np1 Cl1 148.55(3) . . ? O2 Np1 Cl4 82.26(6) . . ? O4 Np1 Cl4 136.85(5) . . ? O1 Np1 Cl4 73.28(6) . . ? O3 Np1 Cl4 76.60(5) . . ? Cl3 Np1 Cl4 102.06(3) . . ? Cl1 Np1 Cl4 84.42(3) . . ? O2 Np1 Cl2 72.98(6) . . ? O4 Np1 Cl2 73.86(5) . . ? O1 Np1 Cl2 79.38(6) . . ? O3 Np1 Cl2 133.39(6) . . ? Cl3 Np1 Cl2 84.08(3) . . ? Cl1 Np1 Cl2 106.28(3) . . ? Cl4 Np1 Cl2 148.88(3) . . ? C2 O1 C1 108.6(3) . . ? C2 O1 Np1 114.7(2) . . ? C1 O1 Np1 124.7(2) . . ? C3 O2 C4 108.3(3) . . ? C3 O2 Np1 115.7(2) . . ? C4 O2 Np1 124.2(2) . . ? C5 O3 C6 108.2(3) . . ? C5 O3 Np1 123.7(2) . . ? C6 O3 Np1 115.06(18) . . ? C7 O4 C8 108.4(3) . . ? C7 O4 Np1 117.44(18) . . ? C8 O4 Np1 122.0(2) . . ? O1 C2 C3 109.4(3) . . ? O2 C3 C2 109.0(3) . . ? O3 C6 C7 107.9(3) . . ? O4 C7 C6 108.6(3) . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.352 _refine_diff_density_min -0.763 _refine_diff_density_rms 0.138 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _database_code_depnum_ccdc_archive 'CCDC 967163' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_apx1670a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H20 Cl4 O4 Pu' _chemical_formula_weight 561.06 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.5060(14) _cell_length_b 7.2420(6) _cell_length_c 14.7911(12) _cell_angle_alpha 90.00 _cell_angle_beta 115.557(1) _cell_angle_gamma 90.00 _cell_volume 1595.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 4.801 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4468 _exptl_absorpt_correction_T_max 0.5138 _exptl_absorpt_process_details 'SADABS v. 1 (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _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_detector_area_resol_mean ? _diffrn_reflns_number 17089 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0168 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 28.35 _reflns_number_total 3752 _reflns_number_gt 3585 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 7.0 (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_data_reduction 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.14, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.14, (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^)+(0.0110P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3752 _refine_ls_number_parameters 158 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0191 _refine_ls_R_factor_gt 0.0174 _refine_ls_wR_factor_ref 0.0405 _refine_ls_wR_factor_gt 0.0402 _refine_ls_goodness_of_fit_ref 1.698 _refine_ls_restrained_S_all 1.698 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pu1 Pu 0.248842(6) 0.526398(14) 0.278511(7) 0.01514(4) Uani 1 1 d . . . Cl1 Cl 0.34079(5) 0.70291(11) 0.20156(5) 0.02838(16) Uani 1 1 d . . . Cl2 Cl 0.36142(5) 0.44624(11) 0.46147(5) 0.02659(16) Uani 1 1 d . . . Cl3 Cl 0.16976(5) 0.22914(10) 0.29298(6) 0.02857(16) Uani 1 1 d . . . Cl4 Cl 0.11595(5) 0.72321(10) 0.15446(5) 0.02763(16) Uani 1 1 d . . . O1 O 0.15493(14) 0.6153(3) 0.37093(15) 0.0302(5) Uani 1 1 d . . . O2 O 0.29349(14) 0.8263(3) 0.37282(14) 0.0284(5) Uani 1 1 d . . . O3 O 0.19597(12) 0.3508(3) 0.11218(14) 0.0222(4) Uani 1 1 d . . . O4 O 0.36177(12) 0.3019(3) 0.26542(13) 0.0220(4) Uani 1 1 d . . . C1 C 0.0626(2) 0.5585(5) 0.3406(3) 0.0464(10) Uani 1 1 d . . . H1A H 0.0478 0.5692 0.3964 0.070 Uiso 1 1 calc R . . H1B H 0.0554 0.4326 0.3182 0.070 Uiso 1 1 calc R . . H1C H 0.0234 0.6362 0.2869 0.070 Uiso 1 1 calc R . . C2 C 0.1643(2) 0.8039(5) 0.4038(3) 0.0394(8) Uani 1 1 d . . . H2A H 0.1412 0.8184 0.4536 0.047 Uiso 1 1 calc R . . H2B H 0.1301 0.8838 0.3475 0.047 Uiso 1 1 calc R . . C3 C 0.2596(3) 0.8555(5) 0.4471(2) 0.0391(8) Uani 1 1 d . . . H3A H 0.2666 0.9842 0.4672 0.047 Uiso 1 1 calc R . . H3B H 0.2933 0.7808 0.5059 0.047 Uiso 1 1 calc R . . C4 C 0.3824(2) 0.9060(5) 0.4103(3) 0.0441(9) Uani 1 1 d . . . H4A H 0.3797 1.0339 0.4257 0.066 Uiso 1 1 calc R . . H4B H 0.4046 0.8952 0.3603 0.066 Uiso 1 1 calc R . . H4C H 0.4219 0.8416 0.4698 0.066 Uiso 1 1 calc R . . C5 C 0.10242(18) 0.3173(5) 0.0460(2) 0.0333(7) Uani 1 1 d . . . H5A H 0.0960 0.2981 -0.0210 0.050 Uiso 1 1 calc R . . H5B H 0.0672 0.4221 0.0471 0.050 Uiso 1 1 calc R . . H5C H 0.0821 0.2096 0.0680 0.050 Uiso 1 1 calc R . . C6 C 0.24564(19) 0.1845(4) 0.1158(2) 0.0279(7) Uani 1 1 d . . . H6A H 0.2306 0.1407 0.0484 0.033 Uiso 1 1 calc R . . H6B H 0.2309 0.0884 0.1519 0.033 Uiso 1 1 calc R . . C7 C 0.34272(19) 0.2301(4) 0.1677(2) 0.0261(6) Uani 1 1 d . . . H7A H 0.3784 0.1203 0.1739 0.031 Uiso 1 1 calc R . . H7B H 0.3578 0.3213 0.1294 0.031 Uiso 1 1 calc R . . C8 C 0.45794(18) 0.3298(5) 0.3194(2) 0.0326(8) Uani 1 1 d . . . H8A H 0.4881 0.2131 0.3288 0.049 Uiso 1 1 calc R . . H8B H 0.4715 0.3843 0.3835 0.049 Uiso 1 1 calc R . . H8C H 0.4779 0.4104 0.2816 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pu1 0.01221(6) 0.01825(6) 0.01412(6) 0.00084(4) 0.00489(4) -0.00096(4) Cl1 0.0289(4) 0.0331(4) 0.0278(4) 0.0028(3) 0.0167(3) -0.0061(3) Cl2 0.0247(4) 0.0342(4) 0.0171(3) 0.0039(3) 0.0054(3) 0.0016(3) Cl3 0.0255(4) 0.0236(4) 0.0396(4) 0.0020(3) 0.0168(3) -0.0036(3) Cl4 0.0216(4) 0.0280(4) 0.0256(4) 0.0004(3) 0.0029(3) 0.0055(3) O1 0.0338(12) 0.0280(13) 0.0378(12) 0.0055(10) 0.0240(10) 0.0070(10) O2 0.0355(12) 0.0250(12) 0.0201(10) -0.0034(9) 0.0078(9) -0.0042(9) O3 0.0140(9) 0.0257(11) 0.0223(9) -0.0046(8) 0.0035(8) -0.0001(8) O4 0.0107(9) 0.0329(12) 0.0195(10) -0.0014(8) 0.0038(8) 0.0019(8) C1 0.0337(19) 0.044(2) 0.076(3) 0.014(2) 0.038(2) 0.0116(16) C2 0.057(2) 0.032(2) 0.043(2) 0.0013(15) 0.0343(18) 0.0096(16) C3 0.064(2) 0.0309(19) 0.0228(15) -0.0054(14) 0.0190(16) 0.0027(17) C4 0.043(2) 0.041(2) 0.0323(18) -0.0044(16) 0.0017(16) -0.0183(17) C5 0.0159(15) 0.039(2) 0.0316(16) -0.0100(14) -0.0025(13) -0.0019(13) C6 0.0259(16) 0.0271(17) 0.0285(15) -0.0088(13) 0.0096(13) 0.0044(12) C7 0.0247(15) 0.0324(18) 0.0235(14) -0.0019(12) 0.0127(12) 0.0054(13) C8 0.0114(14) 0.054(2) 0.0285(16) 0.0006(15) 0.0050(12) 0.0018(13) _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 2.514(2) . ? Pu1 O4 2.5429(19) . ? Pu1 O1 2.5524(19) . ? Pu1 O3 2.5651(18) . ? Pu1 Cl3 2.5739(7) . ? Pu1 Cl1 2.5930(7) . ? Pu1 Cl4 2.5956(7) . ? Pu1 Cl2 2.6028(7) . ? O1 C2 1.435(4) . ? O1 C1 1.450(4) . ? O2 C4 1.446(4) . ? O2 C3 1.446(4) . ? O3 C6 1.445(3) . ? O3 C5 1.448(3) . ? O4 C7 1.437(3) . ? O4 C8 1.451(3) . ? C2 C3 1.468(5) . ? C6 C7 1.485(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 O2 Pu1 O4 123.07(6) . . ? O2 Pu1 O1 65.49(7) . . ? O4 Pu1 O1 146.78(6) . . ? O2 Pu1 O3 149.05(6) . . ? O4 Pu1 O3 64.36(6) . . ? O1 Pu1 O3 127.22(6) . . ? O2 Pu1 Cl3 135.58(5) . . ? O4 Pu1 Cl3 83.47(5) . . ? O1 Pu1 Cl3 73.71(5) . . ? O3 Pu1 Cl3 71.95(5) . . ? O2 Pu1 Cl1 74.38(5) . . ? O4 Pu1 Cl1 72.22(5) . . ? O1 Pu1 Cl1 135.76(5) . . ? O3 Pu1 Cl1 81.07(5) . . ? Cl3 Pu1 Cl1 149.62(2) . . ? O2 Pu1 Cl4 82.76(5) . . ? O4 Pu1 Cl4 136.13(4) . . ? O1 Pu1 Cl4 73.54(5) . . ? O3 Pu1 Cl4 76.12(5) . . ? Cl3 Pu1 Cl4 102.34(2) . . ? Cl1 Pu1 Cl4 83.98(3) . . ? O2 Pu1 Cl2 73.07(5) . . ? O4 Pu1 Cl2 73.65(4) . . ? O1 Pu1 Cl2 79.95(5) . . ? O3 Pu1 Cl2 132.96(5) . . ? Cl3 Pu1 Cl2 83.53(2) . . ? Cl1 Pu1 Cl2 106.01(2) . . ? Cl4 Pu1 Cl2 149.77(2) . . ? C2 O1 C1 108.7(2) . . ? C2 O1 Pu1 114.81(17) . . ? C1 O1 Pu1 124.2(2) . . ? C4 O2 C3 108.1(2) . . ? C4 O2 Pu1 124.3(2) . . ? C3 O2 Pu1 115.53(19) . . ? C6 O3 C5 107.9(2) . . ? C6 O3 Pu1 115.16(15) . . ? C5 O3 Pu1 123.62(16) . . ? C7 O4 C8 108.4(2) . . ? C7 O4 Pu1 117.27(15) . . ? C8 O4 Pu1 122.22(17) . . ? O1 C2 C3 109.2(3) . . ? O2 C3 C2 108.9(3) . . ? O3 C6 C7 107.6(2) . . ? O4 C7 C6 108.7(2) . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.316 _refine_diff_density_min -1.253 _refine_diff_density_rms 0.100 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _database_code_depnum_ccdc_archive 'CCDC 967164'