# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2002data_global #==================================================================== _journal_coden_Cambridge 182 loop_ _publ_author_name 'Wolfgang Runde' 'Thomas E. Albrecht-Schmitt' 'Amanda C. Bean' 'Brian L. Scott' _publ_contact_author_name 'Dr Wolfgang Runde' _publ_contact_author_address ; Dr Wolfgang Runde Chemistry Division Los Alamos National Laboratory MS J514 Los Alamos NM 87544 UNITED STATES OF AMERICA ; _publ_contact_author_email runde@lanl.gov _publ_contact_author_fax '(505) 665-4955' _publ_contact_author_phone '(505) 667-3350' _publ_requested_journal 'Chemical Communications' #==================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Structural Characterization of the First Hydrothermally Synthesized Plutonium Compound, PuO2(IO3)2·H2O ; # TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; Crystal structure of PuO2(IO3)2·H2O ; _publ_section_comment ; ? ; _publ_section_references ; ? ; #==================================================================== data_final _database_code_CSD 197636 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_structural PuO2(IO3)2·H2O _chemical_formula_sum 'H2 I2 O9 Pu' _chemical_formula_weight 623.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pu Pu -9.4100 4.3056 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pn2(1)a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' 'x+1/2, y, -z+1/2' '-x+1/2, y+1/2, z+1/2' _cell_length_a 7.3199(12) _cell_length_b 9.4725(16) _cell_length_c 11.636(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 806.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rectangular block' _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.136 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 11.869 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.083 _exptl_absorpt_correction_T_max 0.241 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 P4/CCD/PC' _diffrn_measurement_method '0.3 degree a and w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3786 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0177 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 23.24 _reflns_number_total 1139 _reflns_number_gt 1138 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement 'SMART, SAINT' _computing_data_reduction SMART _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-97 (Sheldrick, 1997)' _computing_publication_material 'SHELCIF-97 (Sheldrick, 1997)' _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^)+(0.0225P)^2^+6.4980P] 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 SHELXL _refine_ls_extinction_coef 0.00511(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.36(3) _refine_ls_number_reflns 1139 _refine_ls_number_parameters 111 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0184 _refine_ls_R_factor_gt 0.0184 _refine_ls_wR_factor_ref 0.0442 _refine_ls_wR_factor_gt 0.0442 _refine_ls_goodness_of_fit_ref 1.195 _refine_ls_restrained_S_all 1.194 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 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 -0.81774(4) 0.56353(3) -0.02430(3) 0.00697(15) Uani 1 1 d . . . I1 I -0.42509(8) 0.51090(8) 0.21510(6) 0.00816(19) Uani 1 1 d . . . I2 I -1.31468(8) 0.65942(8) -0.13934(5) 0.00783(19) Uani 1 1 d . . . O1 O -0.8184(11) 0.7471(10) -0.0084(8) 0.018(2) Uani 1 1 d . . . O2 O -0.8142(10) 0.3788(10) -0.0381(6) 0.012(2) Uani 1 1 d . . . O3 O -1.1265(10) 0.5642(9) -0.0738(6) 0.0165(16) Uani 1 1 d . . . O4 O -0.6572(10) 0.5196(9) 0.1537(6) 0.0144(18) Uani 1 1 d . . . O5 O -0.5104(10) 0.5408(8) 0.3588(5) 0.0125(16) Uani 1 1 d . . . O6 O -0.4041(12) 0.3207(9) 0.2180(7) 0.0151(18) Uani 1 1 d . . . O7 O -1.3242(10) 0.5619(11) -0.2729(6) 0.0212(19) Uani 1 1 d . . . O8 O -1.4951(10) 0.5687(10) -0.0628(6) 0.0197(17) Uani 1 1 d . . . O1W O -1.0450(19) 0.2937(11) -0.2762(11) 0.062(4) 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 0.0059(2) 0.0102(2) 0.0048(2) 0.00080(16) -0.00005(14) 0.00022(18) I1 0.0055(3) 0.0126(3) 0.0064(3) -0.0004(2) -0.0010(3) -0.0002(3) I2 0.0066(4) 0.0113(4) 0.0056(3) 0.0000(3) 0.0000(2) -0.0005(3) O1 0.028(6) 0.004(5) 0.023(5) 0.000(4) 0.002(4) -0.001(3) O2 0.020(6) 0.006(5) 0.012(5) 0.003(3) 0.002(3) -0.004(3) O3 0.012(3) 0.019(4) 0.018(4) 0.009(4) -0.001(3) -0.003(4) O4 0.010(4) 0.027(5) 0.006(3) 0.000(3) 0.002(3) 0.003(4) O5 0.012(4) 0.024(4) 0.002(3) -0.003(3) -0.001(3) 0.000(3) O6 0.018(4) 0.009(4) 0.019(4) 0.001(3) -0.007(4) 0.003(3) O7 0.034(5) 0.025(4) 0.005(4) -0.009(4) 0.009(3) -0.007(4) O8 0.016(4) 0.024(4) 0.019(4) 0.009(4) 0.011(3) -0.004(4) O1W 0.098(11) 0.018(6) 0.070(8) 0.010(5) -0.052(8) -0.010(6) _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 O1 1.749(10) . ? Pu1 O2 1.757(9) . ? Pu1 O3 2.332(7) . ? Pu1 O7 2.360(7) 3_554 ? Pu1 O5 2.397(7) 3_455 ? Pu1 O8 2.404(7) 1_655 ? Pu1 O4 2.418(8) . ? I1 O5 1.807(6) . ? I1 O6 1.808(8) . ? I1 O4 1.844(7) . ? I1 O4 2.486(7) 3 ? I2 O7 1.810(7) . ? I2 O8 1.810(7) . ? I2 O3 1.815(8) . ? O4 I1 2.486(7) 3_455 ? O5 Pu1 2.397(7) 3 ? O7 Pu1 2.360(7) 3_454 ? O8 Pu1 2.404(7) 1_455 ? 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 Pu1 O2 178.9(4) . . ? O1 Pu1 O3 91.2(3) . . ? O2 Pu1 O3 89.7(3) . . ? O1 Pu1 O7 96.4(4) . 3_554 ? O2 Pu1 O7 84.4(3) . 3_554 ? O3 Pu1 O7 74.6(3) . 3_554 ? O1 Pu1 O5 90.2(4) . 3_455 ? O2 Pu1 O5 89.6(3) . 3_455 ? O3 Pu1 O5 68.2(2) . 3_455 ? O7 Pu1 O5 142.3(2) 3_554 3_455 ? O1 Pu1 O8 90.1(3) . 1_655 ? O2 Pu1 O8 89.3(3) . 1_655 ? O3 Pu1 O8 155.0(3) . 1_655 ? O7 Pu1 O8 80.4(3) 3_554 1_655 ? O5 Pu1 O8 136.8(2) 3_455 1_655 ? O1 Pu1 O4 94.7(4) . . ? O2 Pu1 O4 84.2(3) . . ? O3 Pu1 O4 133.1(2) . . ? O7 Pu1 O4 149.9(3) 3_554 . ? O5 Pu1 O4 65.3(2) 3_455 . ? O8 Pu1 O4 71.7(2) 1_655 . ? O5 I1 O6 99.7(3) . . ? O5 I1 O4 91.9(3) . . ? O6 I1 O4 97.5(4) . . ? O5 I1 O4 72.5(3) . 3 ? O6 I1 O4 87.4(3) . 3 ? O4 I1 O4 164.3(2) . 3 ? O7 I2 O8 98.8(4) . . ? O7 I2 O3 97.9(4) . . ? O8 I2 O3 96.4(3) . . ? I2 O3 Pu1 147.2(4) . . ? I1 O4 Pu1 141.9(4) . . ? I1 O4 I1 119.2(4) . 3_455 ? Pu1 O4 I1 98.5(3) . 3_455 ? I1 O5 Pu1 123.7(3) . 3 ? I2 O7 Pu1 148.7(5) . 3_454 ? I2 O8 Pu1 144.9(4) . 1_455 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.24 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.905 _refine_diff_density_min -1.102 _refine_diff_density_rms 0.212