# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name A.N.Alsobrook B.G.Hauser J.T.Hupp 'Evgeny V.Alekseev' ; W.Depmeier ; T.E.Albrecht-Schmitt _publ_contact_author_name 'Thomas E. Albrecht-Schmitt' _publ_contact_author_email talbrec1@nd.edu # Attachment '- co1.cif' data_Co2[(UO2)6(PO3CH2CO2)3O3(OH)(H2O)2]*16H2O _database_code_depnum_ccdc_archive 'CCDC 794932' #TrackingRef '- co1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Co2[(UO2)6(PO3CH2CO2)3O3(OH)(H2O)2]*16H2O _chemical_formula_sum 'C6 H42 Co2 O49 P3 U6' _chemical_formula_weight 2537.35 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'I m -3' _symmetry_space_group_name_Hall '-I 2 2 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-z, -x, -y' '-z, x, y' 'z, x, -y' 'z, -x, y' '-y, -z, -x' 'y, -z, x' '-y, z, x' 'y, z, -x' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-z+1/2, -x+1/2, -y+1/2' '-z+1/2, x+1/2, y+1/2' 'z+1/2, x+1/2, -y+1/2' 'z+1/2, -x+1/2, y+1/2' '-y+1/2, -z+1/2, -x+1/2' 'y+1/2, -z+1/2, x+1/2' '-y+1/2, z+1/2, x+1/2' 'y+1/2, z+1/2, -x+1/2' _cell_length_a 26.3861(3) _cell_length_b 26.3861(3) _cell_length_c 26.3861(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 18370.7(4) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3461 _cell_measurement_theta_min 1.89 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.08715 _exptl_crystal_size_mid 0.05055 _exptl_crystal_size_min 0.01730 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 3.670 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 17936 _exptl_absorpt_coefficient_mu 22.012 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.274 _exptl_absorpt_correction_T_max 0.683 _exptl_absorpt_process_details SHELXPREP _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX' _diffrn_measurement_method '0.3 /w wxposure' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number na _diffrn_standards_interval_count na _diffrn_standards_interval_time na _diffrn_standards_decay_% 0 _diffrn_reflns_number 110457 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.0133 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3763 _reflns_number_gt 3461 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement 'SMART, SAINT' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXCIF-97 (Sheldrick, 2000)' _refine_special_details ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 1744.2 512.9 2 0.500 0.000 0.171 34.6 10.3 3 0.347 0.000 0.250 9.4 8.4 4 0.653 0.000 0.250 9.2 8.2 5 0.329 -0.001 0.500 34.4 9.6 6 0.671 -0.001 0.500 34.4 9.4 7 0.347 0.000 0.749 9.3 7.7 8 0.653 0.000 0.750 9.1 7.5 9 0.500 0.000 0.828 34.6 8.6 10 0.000 0.171 0.500 34.7 9.3 11 0.250 0.153 0.500 9.2 7.8 12 0.750 0.153 0.500 9.4 7.8 13 0.500 0.500 0.500 1743.8 512.7 14 0.500 0.249 0.153 9.1 7.7 15 0.000 0.250 0.347 9.4 8.1 16 0.000 0.250 0.653 9.2 8.0 17 0.500 0.249 0.847 9.2 7.9 18 0.500 0.328 0.000 34.6 9.4 19 0.250 0.347 0.000 9.4 8.1 20 0.749 0.347 0.000 9.2 8.0 21 0.000 0.500 0.329 34.6 8.6 22 0.000 0.500 0.671 34.6 10.3 23 0.171 0.499 0.000 34.3 9.4 24 0.829 0.499 0.000 34.4 9.6 25 0.153 0.500 0.250 9.1 7.5 26 0.847 0.500 0.249 9.3 7.7 27 0.153 0.500 0.750 9.2 8.2 28 0.847 0.500 0.750 9.4 8.4 29 0.500 0.671 0.000 34.7 9.3 30 0.250 0.653 0.000 9.2 7.8 31 0.750 0.653 0.000 9.1 7.7 32 0.500 0.750 0.153 9.2 8.0 33 0.000 0.749 0.347 9.2 7.9 34 0.000 0.749 0.653 9.1 7.7 35 0.500 0.750 0.847 9.4 8.1 36 0.000 0.828 0.500 34.7 9.4 37 0.249 0.847 0.500 9.2 8.0 38 0.750 0.847 0.500 9.4 8.1 _platon_squeeze_details 'The water atoms in cages which are in non-disordered (or slightly disordered) were modeled in anisotropic mode. All other where refined as isotropic atoms' 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^)+(0.0176P)^2^+226.1683P] 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 0 _refine_ls_number_reflns 3763 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0209 _refine_ls_R_factor_gt 0.0176 _refine_ls_wR_factor_ref 0.0429 _refine_ls_wR_factor_gt 0.0420 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.009 _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 U1 U 0.069577(6) 0.364696(7) 0.0000 0.01063(4) Uani 1 2 d S . . U2 U 0.0000 0.350441(6) 0.131630(6) 0.00723(4) Uani 1 2 d S . . U3 U 0.071558(5) 0.347245(5) 0.261491(4) 0.00958(3) Uani 1 1 d . . . Co1 Co 0.0000 0.5000 0.14032(3) 0.01160(19) Uani 1 4 d S . . Co2 Co 0.18721(3) 0.18721(3) 0.18721(3) 0.0289(3) Uani 0.75 3 d SP . . Co3 Co 0.2500 0.2500 0.2500 0.0246(3) Uani 1 6 d S . . P1 P 0.12444(3) 0.35657(3) 0.13238(3) 0.01081(18) Uani 1 1 d . . . C1 C 0.16934(13) 0.30770(14) 0.11539(13) 0.0163(8) Uani 1 1 d . . . H2A H 0.1517 0.2757 0.1115 0.020 Uiso 1 1 calc R . . H2B H 0.1849 0.3161 0.0832 0.020 Uiso 1 1 calc R . . C2 C 0.21009(13) 0.30235(13) 0.15560(13) 0.0132(7) Uani 1 1 d . . . O1 O 0.15402(9) 0.40226(10) 0.14864(10) 0.0174(6) Uani 1 1 d . . . O2 O 0.08895(9) 0.33597(10) 0.17353(9) 0.0147(5) Uani 1 1 d . . . O3 O 0.08842(9) 0.36601(11) 0.08813(9) 0.0196(6) Uani 1 1 d . . . O4 O 0.23990(9) 0.33851(9) 0.16282(10) 0.0151(5) Uani 1 1 d . . . O5 O 0.21239(10) 0.26171(10) 0.18061(10) 0.0197(6) Uani 1 1 d . . . O6 O 0.08820(15) 0.29972(15) 0.0000 0.0246(9) Uani 1 2 d S . . O7 O 0.05762(14) 0.43180(14) 0.0000 0.0185(8) Uani 1 2 d S . . O8 O 0.0000 0.28209(13) 0.12703(13) 0.0144(8) Uani 1 2 d S . . O9 O 0.0000 0.41942(13) 0.13703(13) 0.0139(8) Uani 1 2 d S . . O10 O 0.06661(10) 0.27945(10) 0.26776(10) 0.0198(6) Uani 1 1 d . . . O11 O 0.07931(10) 0.41449(9) 0.25377(10) 0.0180(6) Uani 1 1 d . . . O12 O 0.0000 0.35240(15) 0.04882(13) 0.0176(8) Uani 1 2 d S . . O13 O 0.15630(14) 0.39553(16) 0.0000 0.0231(9) Uani 1 2 d S . . O14 O 0.0000 0.34755(14) 0.21473(13) 0.0140(8) Uani 1 2 d S . . O15 O 0.0000 0.3604(2) 0.31190(15) 0.0358(12) Uani 1 2 d S . . OW1 O 0.0422(3) 0.5000 0.2052(3) 0.0235(19) Uani 0.50 2 d SP . . OW1A O 0.0672(3) 0.5000 0.1858(3) 0.0186(17) Uani 0.50 2 d SP . . OW2 O 0.0547(2) 0.5000 0.0850(2) 0.0746(18) Uani 1 2 d S . . OW3 O 0.13503(12) 0.13503(12) 0.13503(12) 0.075(2) Uani 1 3 d S . . OW4 O 0.11213(16) 0.2053(2) 0.1719(2) 0.0805(16) Uani 1 1 d . . . OW5 O 0.24213(19) 0.3455(2) 0.0000 0.0460(13) Uani 1 2 d S . . OW6 O 0.1811(4) 0.5000 0.0227(3) 0.039(2) Uani 0.50 2 d SP . . OW7 O 0.0225(4) 0.2098(4) 0.2020(3) 0.084(3) Uani 0.50 1 d P . . OW8 O 0.1182(7) 0.2010(7) 0.0000 0.099(5) Uiso 0.50 2 d SP . . OW9 O 0.0000 0.2210(10) 0.0397(10) 0.060(6) Uiso 0.25 2 d SP . . OW10 O 0.0646(8) 0.1724(8) 0.0910(8) 0.078(6) Uiso 0.25 1 d P . . OW11 O 0.0227(6) 0.2044(6) 0.0572(6) 0.053(4) Uiso 0.25 1 d P . . OW12 O 0.0866(10) 0.0866(10) 0.0866(10) 0.105(14) Uiso 0.25 3 d SP . . OW13 O 0.1134(11) 0.1740(11) 0.0571(11) 0.123(9) Uiso 0.25 1 d P . . 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 U1 0.00725(7) 0.01940(9) 0.00523(7) 0.000 0.000 0.00177(7) U2 0.00814(7) 0.00847(7) 0.00507(7) -0.00018(6) 0.000 0.000 U3 0.01031(6) 0.01229(6) 0.00613(5) 0.00039(4) -0.00068(4) -0.00007(4) Co1 0.0183(4) 0.0090(4) 0.0075(4) 0.000 0.000 0.000 Co2 0.0289(3) 0.0289(3) 0.0289(3) -0.0009(3) -0.0009(3) -0.0009(3) Co3 0.0246(3) 0.0246(3) 0.0246(3) 0.0143(4) 0.0143(4) 0.0143(4) P1 0.0067(3) 0.0177(4) 0.0081(4) 0.0005(3) 0.0000(3) -0.0017(3) C1 0.0147(16) 0.0228(18) 0.0114(16) -0.0036(14) -0.0006(13) 0.0007(14) C2 0.0114(15) 0.0170(16) 0.0112(15) 0.0000(13) 0.0028(13) 0.0019(13) O1 0.0093(11) 0.0151(12) 0.0279(14) 0.0032(11) -0.0018(10) -0.0013(10) O2 0.0112(11) 0.0227(13) 0.0103(11) -0.0025(10) 0.0013(9) -0.0053(10) O3 0.0114(11) 0.0392(16) 0.0083(11) 0.0017(11) -0.0006(9) 0.0014(11) O4 0.0131(11) 0.0132(11) 0.0192(12) 0.0014(10) -0.0021(10) 0.0001(10) O5 0.0260(14) 0.0138(12) 0.0193(13) 0.0045(10) 0.0038(11) 0.0005(11) O6 0.024(2) 0.0223(19) 0.027(2) 0.000 0.000 0.0083(17) O7 0.0168(17) 0.0198(18) 0.0189(18) 0.000 0.000 0.0000(15) O8 0.0178(17) 0.0084(15) 0.0170(17) -0.0057(13) 0.000 0.000 O9 0.0182(17) 0.0106(15) 0.0129(16) -0.0004(13) 0.000 0.000 O10 0.0250(13) 0.0144(12) 0.0199(13) 0.0074(10) -0.0068(11) -0.0046(11) O11 0.0248(13) 0.0108(11) 0.0184(13) -0.0009(10) -0.0061(11) 0.0012(10) O12 0.0097(15) 0.037(2) 0.0065(15) 0.0010(15) 0.000 0.000 O13 0.0123(17) 0.031(2) 0.026(2) 0.000 0.000 0.0008(16) O14 0.0089(15) 0.0230(18) 0.0101(16) -0.0014(14) 0.000 0.000 O15 0.0119(18) 0.083(4) 0.0123(19) -0.002(2) 0.000 0.000 OW1 0.035(4) 0.018(4) 0.018(4) 0.000 -0.018(3) 0.000 OW1A 0.020(4) 0.014(3) 0.022(4) 0.000 0.000(3) 0.000 OW2 0.108(4) 0.017(2) 0.098(4) 0.000 0.089(3) 0.000 OW3 0.075(2) 0.075(2) 0.075(2) -0.0362(16) -0.0362(16) -0.0362(16) OW4 0.040(2) 0.091(3) 0.110(4) 0.025(3) -0.031(2) -0.024(2) OW5 0.044(3) 0.057(3) 0.038(3) 0.000 0.000 0.036(2) OW6 0.051(6) 0.031(5) 0.035(5) 0.000 -0.012(4) 0.000 OW7 0.099(7) 0.092(6) 0.060(5) -0.036(5) -0.029(5) 0.039(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 U1 O6 1.783(4) . ? U1 O7 1.798(4) . ? U1 O12 2.266(2) 26 ? U1 O12 2.266(2) . ? U1 O3 2.378(2) . ? U1 O3 2.378(2) 26 ? U1 O13 2.429(4) . ? U1 U1 3.6718(3) 3 ? U1 U2 3.94653(17) 26 ? U1 U2 3.94653(17) . ? U2 O8 1.808(3) . ? U2 O9 1.826(3) . ? U2 O12 2.186(3) . ? U2 O14 2.194(3) . ? U2 O2 2.622(2) 28 ? U2 O2 2.622(2) . ? U2 O3 2.632(2) 28 ? U2 O3 2.632(2) . ? U2 P1 3.2875(8) 28 ? U2 P1 3.2875(8) . ? U2 U3 3.91322(18) . ? U2 U3 3.91322(19) 28 ? U3 O11 1.798(2) . ? U3 O10 1.801(3) . ? U3 O14 2.2556(18) . ? U3 O15 2.335(2) . ? U3 O1 2.336(2) 45 ? U3 O2 2.385(2) . ? U3 O4 2.388(2) 45 ? U3 U3 3.7763(2) 28 ? Co1 OW1 2.041(7) . ? Co1 OW1 2.041(7) 2_565 ? Co1 OW2 2.053(5) 2_565 ? Co1 OW2 2.053(5) . ? Co1 O9 2.128(3) . ? Co1 O9 2.128(3) 2_565 ? Co1 OW1A 2.140(8) 2_565 ? Co1 OW1A 2.140(8) . ? Co2 OW4 2.077(4) 5 ? Co2 OW4 2.077(4) . ? Co2 OW4 2.077(4) 9 ? Co2 O5 2.082(3) 9 ? Co2 O5 2.082(3) . ? Co2 O5 2.082(3) 5 ? Co2 OW3 2.385(6) . ? Co2 Co3 2.8698(14) . ? Co3 O5 2.105(3) 9 ? Co3 O5 2.105(3) . ? Co3 O5 2.105(3) 5 ? Co3 O5 2.105(3) 37 ? Co3 O5 2.105(3) 45 ? Co3 O5 2.105(3) 41 ? Co3 Co2 2.8698(14) 37 ? P1 O1 1.499(3) . ? P1 O3 1.526(3) . ? P1 O2 1.533(2) . ? P1 C1 1.808(4) . ? C1 C2 1.517(5) . ? C2 O4 1.251(4) . ? C2 O5 1.261(4) . ? O1 U3 2.336(2) 41 ? O4 U3 2.388(2) 41 ? O12 U1 2.266(2) 3 ? O14 U3 2.2556(18) 28 ? O15 U3 2.335(2) 28 ? OW1 OW1A 0.835(10) . ? OW6 OW6 1.201(18) 26 ? OW7 OW7 1.186(19) 28 ? OW8 OW13 1.67(3) 26 ? OW8 OW13 1.67(3) . ? OW9 OW11 0.87(2) 28 ? OW9 OW11 0.87(2) . ? OW10 OW13 1.57(3) . ? OW10 OW11 1.65(3) . ? OW11 OW11 1.20(3) 28 ? 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 O6 U1 O7 174.11(17) . . ? O6 U1 O12 94.91(15) . 26 ? O7 U1 O12 89.93(14) . 26 ? O6 U1 O12 94.91(15) . . ? O7 U1 O12 89.93(14) . . ? O12 U1 O12 69.28(14) 26 . ? O6 U1 O3 87.50(7) . . ? O7 U1 O3 91.28(7) . . ? O12 U1 O3 136.66(9) 26 . ? O12 U1 O3 67.40(9) . . ? O6 U1 O3 87.50(7) . 26 ? O7 U1 O3 91.28(7) . 26 ? O12 U1 O3 67.40(9) 26 26 ? O12 U1 O3 136.66(9) . 26 ? O3 U1 O3 155.80(12) . 26 ? O6 U1 O13 93.58(16) . . ? O7 U1 O13 80.53(15) . . ? O12 U1 O13 144.22(8) 26 . ? O12 U1 O13 144.22(8) . . ? O3 U1 O13 78.35(6) . . ? O3 U1 O13 78.35(6) 26 . ? O6 U1 U1 106.00(13) . 3 ? O7 U1 U1 79.90(12) . 3 ? O12 U1 U1 35.89(7) 26 3 ? O12 U1 U1 35.89(7) . 3 ? O3 U1 U1 102.07(6) . 3 ? O3 U1 U1 102.07(6) 26 3 ? O13 U1 U1 160.43(10) . 3 ? O6 U1 U2 92.10(6) . 26 ? O7 U1 U2 90.70(6) . 26 ? O12 U1 U2 27.03(7) 26 26 ? O12 U1 U2 96.30(7) . 26 ? O3 U1 U2 163.57(6) . 26 ? O3 U1 U2 40.37(6) 26 26 ? O13 U1 U2 118.050(8) . 26 ? U1 U1 U2 62.278(2) 3 26 ? O6 U1 U2 92.10(6) . . ? O7 U1 U2 90.70(6) . . ? O12 U1 U2 96.30(7) 26 . ? O12 U1 U2 27.03(7) . . ? O3 U1 U2 40.37(6) . . ? O3 U1 U2 163.57(6) 26 . ? O13 U1 U2 118.050(8) . . ? U1 U1 U2 62.278(2) 3 . ? U2 U1 U2 123.301(5) 26 . ? O8 U2 O9 179.37(15) . . ? O8 U2 O12 87.51(15) . . ? O9 U2 O12 93.12(15) . . ? O8 U2 O14 91.86(15) . . ? O9 U2 O14 87.51(14) . . ? O12 U2 O14 179.37(14) . . ? O8 U2 O2 83.28(7) . 28 ? O9 U2 O2 96.44(7) . 28 ? O12 U2 O2 115.14(5) . 28 ? O14 U2 O2 64.76(5) . 28 ? O8 U2 O2 83.28(7) . . ? O9 U2 O2 96.44(7) . . ? O12 U2 O2 115.14(5) . . ? O14 U2 O2 64.76(5) . . ? O2 U2 O2 127.03(10) 28 . ? O8 U2 O3 97.26(8) . 28 ? O9 U2 O3 83.02(8) . 28 ? O12 U2 O3 63.92(6) . 28 ? O14 U2 O3 116.18(6) . 28 ? O2 U2 O3 54.07(7) 28 28 ? O2 U2 O3 178.86(8) . 28 ? O8 U2 O3 97.26(8) . . ? O9 U2 O3 83.02(8) . . ? O12 U2 O3 63.92(6) . . ? O14 U2 O3 116.18(6) . . ? O2 U2 O3 178.86(8) 28 . ? O2 U2 O3 54.07(7) . . ? O3 U2 O3 124.82(11) 28 . ? O8 U2 P1 92.837(16) . 28 ? O9 U2 P1 87.161(16) . 28 ? O12 U2 P1 90.278(16) . 28 ? O14 U2 P1 89.753(16) . 28 ? O2 U2 P1 27.21(5) 28 28 ? O2 U2 P1 153.97(5) . 28 ? O3 U2 P1 27.09(5) 28 28 ? O3 U2 P1 151.66(6) . 28 ? O8 U2 P1 92.837(16) . . ? O9 U2 P1 87.161(16) . . ? O12 U2 P1 90.278(16) . . ? O14 U2 P1 89.753(16) . . ? O2 U2 P1 153.97(5) 28 . ? O2 U2 P1 27.21(5) . . ? O3 U2 P1 151.66(6) 28 . ? O3 U2 P1 27.09(5) . . ? P1 U2 P1 174.32(3) 28 . ? O8 U2 U3 92.14(10) . . ? O9 U2 U3 87.32(9) . . ? O12 U2 U3 151.151(2) . . ? O14 U2 U3 28.854(3) . . ? O2 U2 U3 93.42(5) 28 . ? O2 U2 U3 36.47(5) . . ? O3 U2 U3 144.37(5) 28 . ? O3 U2 U3 87.57(5) . . ? P1 U2 U3 118.535(15) 28 . ? P1 U2 U3 60.914(15) . . ? O8 U2 U3 92.14(10) . 28 ? O9 U2 U3 87.32(9) . 28 ? O12 U2 U3 151.151(2) . 28 ? O14 U2 U3 28.854(3) . 28 ? O2 U2 U3 36.47(5) 28 28 ? O2 U2 U3 93.42(5) . 28 ? O3 U2 U3 87.57(5) 28 28 ? O3 U2 U3 144.37(5) . 28 ? P1 U2 U3 60.914(15) 28 28 ? P1 U2 U3 118.535(15) . 28 ? U3 U2 U3 57.698(4) . 28 ? O11 U3 O10 177.31(13) . . ? O11 U3 O14 91.70(12) . . ? O10 U3 O14 89.60(12) . . ? O11 U3 O15 90.58(16) . . ? O10 U3 O15 92.09(16) . . ? O14 U3 O15 68.55(11) . . ? O11 U3 O1 91.64(11) . 45 ? O10 U3 O1 88.85(11) . 45 ? O14 U3 O1 140.29(9) . 45 ? O15 U3 O1 71.86(10) . 45 ? O11 U3 O2 89.47(10) . . ? O10 U3 O2 88.83(10) . . ? O14 U3 O2 68.23(9) . . ? O15 U3 O2 136.76(10) . . ? O1 U3 O2 151.35(8) 45 . ? O11 U3 O4 89.71(10) . 45 ? O10 U3 O4 87.89(11) . 45 ? O14 U3 O4 145.47(9) . 45 ? O15 U3 O4 145.96(10) . 45 ? O1 U3 O4 74.10(8) 45 45 ? O2 U3 O4 77.28(8) . 45 ? O11 U3 U3 96.54(9) . 28 ? O10 U3 U3 85.84(9) . 28 ? O14 U3 U3 33.16(7) . 28 ? O15 U3 U3 36.05(8) . 28 ? O1 U3 U3 107.20(6) 45 28 ? O2 U3 U3 101.10(6) . 28 ? O4 U3 U3 173.56(6) 45 28 ? O11 U3 U2 86.24(8) . . ? O10 U3 U2 93.83(8) . . ? O14 U3 U2 28.00(7) . . ? O15 U3 U2 96.05(8) . . ? O1 U3 U2 167.73(6) 45 . ? O2 U3 U2 40.82(6) . . ? O4 U3 U2 117.93(6) 45 . ? U3 U3 U2 61.151(2) 28 . ? OW1 Co1 OW1 66.1(5) . 2_565 ? OW1 Co1 OW2 168.4(3) . 2_565 ? OW1 Co1 OW2 102.3(3) 2_565 2_565 ? OW1 Co1 OW2 102.3(3) . . ? OW1 Co1 OW2 168.4(3) 2_565 . ? OW2 Co1 OW2 89.3(4) 2_565 . ? OW1 Co1 O9 91.96(8) . . ? OW1 Co1 O9 91.96(8) 2_565 . ? OW2 Co1 O9 88.34(7) 2_565 . ? OW2 Co1 O9 88.34(7) . . ? OW1 Co1 O9 91.96(8) . 2_565 ? OW1 Co1 O9 91.96(8) 2_565 2_565 ? OW2 Co1 O9 88.34(7) 2_565 2_565 ? OW2 Co1 O9 88.34(7) . 2_565 ? O9 Co1 O9 175.32(19) . 2_565 ? OW1 Co1 OW1A 88.9(4) . 2_565 ? OW1 Co1 OW1A 22.9(3) 2_565 2_565 ? OW2 Co1 OW1A 79.4(3) 2_565 2_565 ? OW2 Co1 OW1A 168.7(3) . 2_565 ? O9 Co1 OW1A 91.31(5) . 2_565 ? O9 Co1 OW1A 91.31(5) 2_565 2_565 ? OW1 Co1 OW1A 22.9(3) . . ? OW1 Co1 OW1A 88.9(4) 2_565 . ? OW2 Co1 OW1A 168.7(3) 2_565 . ? OW2 Co1 OW1A 79.4(3) . . ? O9 Co1 OW1A 91.31(5) . . ? O9 Co1 OW1A 91.31(5) 2_565 . ? OW1A Co1 OW1A 111.8(4) 2_565 . ? OW4 Co2 OW4 94.5(2) 5 . ? OW4 Co2 OW4 94.5(2) 5 9 ? OW4 Co2 OW4 94.5(2) . 9 ? OW4 Co2 O5 91.77(17) 5 9 ? OW4 Co2 O5 168.99(18) . 9 ? OW4 Co2 O5 94.10(16) 9 9 ? OW4 Co2 O5 168.99(18) 5 . ? OW4 Co2 O5 94.10(16) . . ? OW4 Co2 O5 91.77(17) 9 . ? O5 Co2 O5 78.72(12) 9 . ? OW4 Co2 O5 94.10(16) 5 5 ? OW4 Co2 O5 91.77(17) . 5 ? OW4 Co2 O5 168.99(18) 9 5 ? O5 Co2 O5 78.72(12) 9 5 ? O5 Co2 O5 78.72(12) . 5 ? OW4 Co2 OW3 57.95(16) 5 . ? OW4 Co2 OW3 57.95(16) . . ? OW4 Co2 OW3 57.95(16) 9 . ? O5 Co2 OW3 132.92(8) 9 . ? O5 Co2 OW3 132.92(8) . . ? O5 Co2 OW3 132.92(8) 5 . ? OW4 Co2 Co3 122.05(16) 5 . ? OW4 Co2 Co3 122.05(16) . . ? OW4 Co2 Co3 122.05(16) 9 . ? O5 Co2 Co3 47.08(8) 9 . ? O5 Co2 Co3 47.08(8) . . ? O5 Co2 Co3 47.08(8) 5 . ? OW3 Co2 Co3 180.0(2) . . ? O5 Co3 O5 77.70(11) 9 . ? O5 Co3 O5 77.70(11) 9 5 ? O5 Co3 O5 77.70(11) . 5 ? O5 Co3 O5 102.30(11) 9 37 ? O5 Co3 O5 180.00(7) . 37 ? O5 Co3 O5 102.30(11) 5 37 ? O5 Co3 O5 180.00(13) 9 45 ? O5 Co3 O5 102.30(11) . 45 ? O5 Co3 O5 102.30(11) 5 45 ? O5 Co3 O5 77.70(11) 37 45 ? O5 Co3 O5 102.30(11) 9 41 ? O5 Co3 O5 102.30(11) . 41 ? O5 Co3 O5 180.0(2) 5 41 ? O5 Co3 O5 77.70(11) 37 41 ? O5 Co3 O5 77.70(11) 45 41 ? O5 Co3 Co2 46.41(7) 9 . ? O5 Co3 Co2 46.41(7) . . ? O5 Co3 Co2 46.41(7) 5 . ? O5 Co3 Co2 133.59(7) 37 . ? O5 Co3 Co2 133.59(7) 45 . ? O5 Co3 Co2 133.59(7) 41 . ? O5 Co3 Co2 133.59(7) 9 37 ? O5 Co3 Co2 133.59(7) . 37 ? O5 Co3 Co2 133.59(7) 5 37 ? O5 Co3 Co2 46.41(7) 37 37 ? O5 Co3 Co2 46.41(7) 45 37 ? O5 Co3 Co2 46.41(7) 41 37 ? Co2 Co3 Co2 180.00(5) . 37 ? O1 P1 O3 114.34(16) . . ? O1 P1 O2 113.60(15) . . ? O3 P1 O2 102.67(14) . . ? O1 P1 C1 107.67(16) . . ? O3 P1 C1 109.56(16) . . ? O2 P1 C1 108.84(16) . . ? O1 P1 U2 124.15(10) . . ? O3 P1 U2 51.79(10) . . ? O2 P1 U2 51.46(9) . . ? C1 P1 U2 128.17(12) . . ? C2 C1 P1 110.9(2) . . ? O4 C2 O5 122.6(3) . . ? O4 C2 C1 118.8(3) . . ? O5 C2 C1 118.7(3) . . ? P1 O1 U3 138.42(15) . 41 ? P1 O2 U3 139.69(14) . . ? P1 O2 U2 101.33(12) . . ? U3 O2 U2 102.70(9) . . ? P1 O3 U1 151.17(15) . . ? P1 O3 U2 101.12(12) . . ? U1 O3 U2 103.81(9) . . ? C2 O4 U3 137.0(2) . 41 ? C2 O5 Co2 146.2(2) . . ? C2 O5 Co3 127.1(2) . . ? Co2 O5 Co3 86.51(10) . . ? U2 O9 Co1 177.9(2) . . ? U2 O12 U1 124.87(7) . 3 ? U2 O12 U1 124.87(7) . . ? U1 O12 U1 108.23(14) 3 . ? U2 O14 U3 123.15(7) . . ? U2 O14 U3 123.15(7) . 28 ? U3 O14 U3 113.67(14) . 28 ? U3 O15 U3 107.89(16) 28 . ? OW1A OW1 Co1 85.3(8) . . ? OW1 OW1A Co1 71.9(8) . . ? OW13 OW8 OW13 129(2) 26 . ? OW11 OW9 OW11 86(3) 28 . ? OW13 OW10 OW11 103.1(17) . . ? OW9 OW11 OW11 46.8(16) . 28 ? OW9 OW11 OW10 179(2) . . ? OW11 OW11 OW10 132.0(9) 28 . ? OW10 OW13 OW8 126(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.002 _refine_diff_density_min -1.357 _refine_diff_density_rms 0.150 # Attachment 'web_deposit_cif_file_1_AndreaN.Alsobrook_1285604678.cif' data_Cd2[(UO2)6(PO3CH2CO2)3O3(OH)(H2O)2]*16H2O _database_code_depnum_ccdc_archive 'CCDC 794933' #TrackingRef 'web_deposit_cif_file_1_AndreaN.Alsobrook_1285604678.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Cd2[(UO2)6(PO3CH2CO2)3O3(OH)(H2O)2]*16H2O _chemical_formula_sum 'C6 H42 Cd2 O49 P3 U6' _chemical_formula_weight 2644.29 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'I m -3' _symmetry_space_group_name_Hall '-I 2 2 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-z, -x, -y' '-z, x, y' 'z, x, -y' 'z, -x, y' '-y, -z, -x' 'y, -z, x' '-y, z, x' 'y, z, -x' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-z+1/2, -x+1/2, -y+1/2' '-z+1/2, x+1/2, y+1/2' 'z+1/2, x+1/2, -y+1/2' 'z+1/2, -x+1/2, y+1/2' '-y+1/2, -z+1/2, -x+1/2' 'y+1/2, -z+1/2, x+1/2' '-y+1/2, z+1/2, x+1/2' 'y+1/2, z+1/2, -x+1/2' _cell_length_a 26.404(2) _cell_length_b 26.404(2) _cell_length_c 26.404(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 18407(3) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3204 _cell_measurement_theta_min 1.89 _cell_measurement_theta_max 27.47 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.04928 _exptl_crystal_size_mid 0.04724 _exptl_crystal_size_min 0.04077 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 3.817 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 18608 _exptl_absorpt_coefficient_mu 22.172 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.349 _exptl_absorpt_correction_T_max 0.405 _exptl_absorpt_process_details SHELXPREP _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX' _diffrn_measurement_method '0.3 /w exposure' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number na _diffrn_standards_interval_count na _diffrn_standards_interval_time na _diffrn_standards_decay_% 0 _diffrn_reflns_number 109885 _diffrn_reflns_av_R_equivalents 0.0757 _diffrn_reflns_av_sigmaI/netI 0.0204 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 27.46 _reflns_number_total 3759 _reflns_number_gt 3204 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement 'SMART, SAINT' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXCIF-97 (Sheldrick, 2000)' _refine_special_details ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 1690.9 502.7 2 0.500 0.000 0.167 28.3 13.0 3 0.333 0.000 0.500 28.2 12.3 4 0.667 0.000 0.500 28.3 12.3 5 0.500 0.000 0.833 28.3 11.1 6 0.000 0.167 0.500 28.2 12.4 7 0.500 0.500 0.500 1690.8 502.7 8 0.500 0.333 0.000 28.3 12.1 9 0.000 0.500 0.333 28.3 11.1 10 0.000 0.500 0.667 28.3 13.0 11 0.167 0.500 0.000 28.2 12.3 12 0.833 0.500 0.000 28.2 12.2 13 0.500 0.667 0.000 28.3 12.4 14 0.000 0.833 0.500 28.3 12.1 _platon_squeeze_details 'The water atoms in cages which are in non-disordered (or slightly disordered) were modeled in anisotropic mode. All other where refined as isotropic atoms' 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^)+(0.0194P)^2^+472.6401P] 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 0 _refine_ls_number_reflns 3759 _refine_ls_number_parameters 238 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0330 _refine_ls_R_factor_gt 0.0239 _refine_ls_wR_factor_ref 0.0565 _refine_ls_wR_factor_gt 0.0531 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.022 _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 U1 U 0.069221(12) 0.363231(14) 0.0000 0.01356(8) Uani 1 2 d S . . U2 U 0.0000 0.346684(12) 0.131842(11) 0.00895(7) Uani 1 2 d S . . U3 U 0.071934(9) 0.344815(9) 0.261803(8) 0.01020(6) Uani 1 1 d . . . Cd1 Cd 0.0000 0.5000 0.14387(4) 0.0358(3) Uani 1 4 d S . . Cd2 Cd 0.17908(3) 0.17908(3) 0.17908(3) 0.0335(3) Uani 0.75 3 d SP . . Cd3 Cd 0.2500 0.2500 0.2500 0.0333(4) Uani 1 6 d S . . P1 P 0.12415(6) 0.35680(6) 0.13216(6) 0.0120(3) Uani 1 1 d . . . C1 C 0.1698(3) 0.3109(3) 0.1114(3) 0.0177(14) Uani 1 1 d . . . H2A H 0.1527 0.2793 0.1038 0.021 Uiso 1 1 calc R . . H2B H 0.1860 0.3228 0.0807 0.021 Uiso 1 1 calc R . . C2 C 0.2094(2) 0.3019(3) 0.1517(2) 0.0147(13) Uani 1 1 d . . . O1 O 0.15295(16) 0.40231(17) 0.14997(18) 0.0162(9) Uani 1 1 d . . . O2 O 0.08991(17) 0.33361(17) 0.17312(17) 0.0157(9) Uani 1 1 d . . . O3 O 0.08767(17) 0.3671(2) 0.08849(17) 0.0227(11) Uani 1 1 d . . . O4 O 0.23846(17) 0.33771(16) 0.16369(17) 0.0147(9) Uani 1 1 d . . . O5 O 0.21135(19) 0.25888(18) 0.17312(19) 0.0219(11) Uani 1 1 d . . . O6 O 0.0899(3) 0.2989(3) 0.0000 0.0327(19) Uani 1 2 d S . . O7 O 0.0560(3) 0.4297(3) 0.0000 0.0246(16) Uani 1 2 d S . . O8 O 0.0000 0.2789(2) 0.1277(2) 0.0180(14) Uani 1 2 d S . . O9 O 0.0000 0.4157(2) 0.1376(3) 0.0188(14) Uani 1 2 d S . . O10 O 0.06731(18) 0.27719(18) 0.26833(18) 0.0191(10) Uani 1 1 d . . . O11 O 0.07908(18) 0.41209(17) 0.25481(18) 0.0182(10) Uani 1 1 d . . . O12 O 0.0000 0.3481(3) 0.0484(2) 0.0193(15) Uani 1 2 d S . . O13 O 0.1561(3) 0.3958(3) 0.0000 0.0325(19) Uani 1 2 d S . . O14 O 0.0000 0.3448(2) 0.2146(2) 0.0130(13) Uani 1 2 d S . . O15 O 0.0000 0.3565(3) 0.3122(3) 0.0306(19) Uani 1 2 d S . . OW1 O 0.0336(8) 0.5000 0.2192(7) 0.047(5) Uani 0.50 2 d SP . . OW1A O 0.0809(7) 0.5000 0.1887(7) 0.036(4) Uani 0.50 2 d SP . . OW2 O 0.0517(10) 0.5000 0.0741(10) 0.064(6) Uiso 0.50 2 d SP . . OW2A O 0.0726(9) 0.5000 0.0950(9) 0.054(5) Uiso 0.50 2 d SP . . OW3 O 0.0977(3) 0.2119(4) 0.1712(4) 0.082(3) Uani 1 1 d . . . OW4 O 0.2414(5) 0.3477(6) 0.0000 0.088(5) Uani 1 2 d S . . OW5 O 0.0837(3) 0.0837(3) 0.0837(3) 0.067(4) Uani 1 3 d S . . OW6 O 0.1757(9) 0.5000 0.0300(8) 0.064(6) Uiso 0.50 2 d SP . . OW7 O 0.0000 0.1935(11) 0.2154(11) 0.085(8) Uiso 0.50 2 d SP . . OW8 O 0.0000 0.2217(14) 0.0330(13) 0.118(11) Uiso 0.50 2 d SP . . OW9 O 0.051(2) 0.183(2) 0.077(2) 0.12(2) Uiso 0.20 1 d P . . OW10 O 0.1953(19) 0.0338(19) 0.113(2) 0.092(15) Uiso 0.20 1 d P . . OW11 O 0.1315(8) 0.1315(8) 0.1315(8) 0.080(10) Uiso 0.50 3 d SP . . OW12 O 0.2108(11) 0.4419(11) 0.0000 0.094(9) Uiso 0.50 2 d SP . . OW13 O 0.100(4) 0.092(4) 0.0000 0.05(3) Uiso 0.10 2 d SP . . OW14 O 0.067(4) 0.095(4) 0.0000 0.05(3) Uiso 0.10 2 d SP . . OW15 O 0.1165(14) 0.1571(13) 0.1157(14) 0.069(9) Uiso 0.25 1 d P . . 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 U1 0.00832(15) 0.02652(19) 0.00583(15) 0.000 0.000 0.00159(13) U2 0.00975(15) 0.01084(15) 0.00625(14) 0.00037(12) 0.000 0.000 U3 0.01164(11) 0.01261(11) 0.00635(11) 0.00075(8) -0.00044(8) -0.00089(9) Cd1 0.0730(10) 0.0130(5) 0.0214(6) 0.000 0.000 0.000 Cd2 0.0335(3) 0.0335(3) 0.0335(3) 0.0003(3) 0.0003(3) 0.0003(3) Cd3 0.0333(4) 0.0333(4) 0.0333(4) 0.0158(4) 0.0158(4) 0.0158(4) P1 0.0087(7) 0.0193(8) 0.0080(7) 0.0006(6) -0.0003(6) -0.0023(6) C1 0.017(3) 0.021(3) 0.016(3) -0.004(3) 0.004(3) 0.002(3) C2 0.011(3) 0.020(3) 0.013(3) -0.001(3) 0.005(2) 0.001(3) O1 0.008(2) 0.016(2) 0.025(2) 0.000(2) -0.0015(18) -0.0019(18) O2 0.016(2) 0.019(2) 0.012(2) -0.0008(18) 0.0035(18) -0.0065(19) O3 0.012(2) 0.046(3) 0.010(2) -0.001(2) -0.0006(18) 0.004(2) O4 0.012(2) 0.013(2) 0.019(2) -0.0002(18) -0.0032(18) 0.0015(18) O5 0.025(3) 0.015(2) 0.026(3) 0.006(2) 0.007(2) 0.001(2) O6 0.038(5) 0.038(5) 0.023(4) 0.000 0.000 0.021(4) O7 0.028(4) 0.028(4) 0.018(4) 0.000 0.000 -0.007(3) O8 0.022(4) 0.014(3) 0.018(3) -0.004(3) 0.000 0.000 O9 0.019(3) 0.015(3) 0.022(4) 0.001(3) 0.000 0.000 O10 0.021(2) 0.015(2) 0.021(2) 0.0041(19) -0.006(2) -0.0026(19) O11 0.022(2) 0.015(2) 0.018(2) -0.0019(19) -0.0041(19) 0.0001(19) O12 0.011(3) 0.038(4) 0.009(3) 0.005(3) 0.000 0.000 O13 0.020(4) 0.050(5) 0.028(4) 0.000 0.000 -0.011(4) O14 0.006(3) 0.020(3) 0.013(3) 0.003(3) 0.000 0.000 O15 0.012(3) 0.062(6) 0.018(4) -0.007(4) 0.000 0.000 OW1 0.088(15) 0.016(8) 0.036(10) 0.000 -0.028(10) 0.000 OW1A 0.051(11) 0.014(7) 0.043(10) 0.000 0.006(9) 0.000 OW3 0.059(5) 0.081(6) 0.105(7) 0.002(6) -0.030(5) -0.014(5) OW4 0.098(10) 0.125(11) 0.041(6) 0.000 0.000 0.080(9) OW5 0.067(4) 0.067(4) 0.067(4) -0.013(4) -0.013(4) -0.013(4) _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 U1 O6 1.783(8) . ? U1 O7 1.789(7) . ? U1 O12 2.265(4) 26 ? U1 O12 2.265(4) . ? U1 O3 2.389(5) 26 ? U1 O3 2.389(5) . ? U1 O13 2.450(7) . ? U1 U1 3.6554(7) 3 ? U1 U2 3.9559(4) 26 ? U1 U2 3.9559(4) . ? U2 O8 1.794(6) . ? U2 O9 1.829(7) . ? U2 O14 2.187(6) . ? U2 O12 2.205(6) . ? U2 O2 2.635(5) . ? U2 O2 2.635(5) 28 ? U2 O3 2.638(5) 28 ? U2 O3 2.638(5) . ? U2 P1 3.2888(16) 28 ? U2 P1 3.2888(16) . ? U2 U3 3.9223(5) . ? U2 U3 3.9223(5) 28 ? U3 O11 1.796(5) . ? U3 O10 1.798(5) . ? U3 O14 2.271(3) . ? U3 O15 2.339(4) . ? U3 O1 2.355(4) 45 ? U3 O4 2.396(4) 45 ? U3 O2 2.407(4) . ? U3 U3 3.7986(5) 28 ? Cd1 OW1 2.179(17) 2_565 ? Cd1 OW1 2.179(17) . ? Cd1 O9 2.231(7) . ? Cd1 O9 2.231(7) 2_565 ? Cd1 OW2 2.29(2) 2_565 ? Cd1 OW2 2.29(2) . ? Cd1 OW2A 2.31(2) 2_565 ? Cd1 OW2A 2.31(2) . ? Cd1 OW1A 2.442(18) . ? Cd1 OW1A 2.442(18) 2_565 ? Cd2 OW11 2.18(4) . ? Cd2 O5 2.278(5) 9 ? Cd2 O5 2.278(5) . ? Cd2 O5 2.278(5) 5 ? Cd2 OW3 2.326(9) 5 ? Cd2 OW3 2.326(9) . ? Cd2 OW3 2.326(9) 9 ? Cd2 OW15 2.42(4) 9 ? Cd2 OW15 2.42(4) 5 ? Cd2 OW15 2.42(4) . ? Cd2 Cd3 3.2435(15) . ? Cd3 O5 2.284(5) 9 ? Cd3 O5 2.284(5) . ? Cd3 O5 2.284(5) 5 ? Cd3 O5 2.284(5) 37 ? Cd3 O5 2.284(5) 41 ? Cd3 O5 2.284(5) 45 ? Cd3 Cd2 3.2435(15) 37 ? P1 O1 1.498(5) . ? P1 O3 1.527(5) . ? P1 O2 1.537(5) . ? P1 C1 1.794(7) . ? C1 C2 1.512(9) . ? C2 O4 1.257(8) . ? C2 O5 1.270(8) . ? O1 U3 2.355(4) 41 ? O4 U3 2.396(4) 41 ? O12 U1 2.265(4) 3 ? O14 U3 2.271(3) 28 ? O15 U3 2.339(4) 28 ? OW1 OW1A 1.49(3) . ? OW1 OW1 1.78(4) 2_565 ? OW2 OW2A 0.78(3) . ? OW6 OW6 1.58(4) 26 ? OW8 OW8 1.74(7) 26 ? OW10 OW10 1.79(10) 27 ? OW11 OW15 0.89(3) 9 ? OW11 OW15 0.89(3) 5 ? OW11 OW15 0.89(3) . ? OW13 OW14 0.88(12) . ? OW15 OW15 1.53(6) 9 ? OW15 OW15 1.53(6) 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 O6 U1 O7 173.5(4) . . ? O6 U1 O12 94.5(3) . 26 ? O7 U1 O12 90.9(3) . 26 ? O6 U1 O12 94.5(3) . . ? O7 U1 O12 90.9(3) . . ? O12 U1 O12 68.6(3) 26 . ? O6 U1 O3 88.77(14) . 26 ? O7 U1 O3 89.87(14) . 26 ? O12 U1 O3 67.72(18) 26 26 ? O12 U1 O3 136.34(18) . 26 ? O6 U1 O3 88.77(14) . . ? O7 U1 O3 89.87(14) . . ? O12 U1 O3 136.34(18) 26 . ? O12 U1 O3 67.72(18) . . ? O3 U1 O3 155.9(2) 26 . ? O6 U1 O13 92.8(4) . . ? O7 U1 O13 80.7(3) . . ? O12 U1 O13 144.83(15) 26 . ? O12 U1 O13 144.83(15) . . ? O3 U1 O13 78.11(12) 26 . ? O3 U1 O13 78.11(12) . . ? O6 U1 U1 107.8(3) . 3 ? O7 U1 U1 78.7(2) . 3 ? O12 U1 U1 36.20(13) 26 3 ? O12 U1 U1 36.20(13) . 3 ? O3 U1 U1 101.77(11) 26 3 ? O3 U1 U1 101.77(11) . 3 ? O13 U1 U1 159.4(2) . 3 ? O6 U1 U2 92.06(13) . 26 ? O7 U1 U2 91.04(11) . 26 ? O12 U1 U2 27.34(13) 26 26 ? O12 U1 U2 95.96(14) . 26 ? O3 U1 U2 40.39(11) 26 26 ? O3 U1 U2 163.66(11) . 26 ? O13 U1 U2 118.122(15) . 26 ? U1 U1 U2 62.483(5) 3 26 ? O6 U1 U2 92.06(13) . . ? O7 U1 U2 91.04(11) . . ? O12 U1 U2 95.96(14) 26 . ? O12 U1 U2 27.34(13) . . ? O3 U1 U2 163.66(11) 26 . ? O3 U1 U2 40.39(11) . . ? O13 U1 U2 118.122(15) . . ? U1 U1 U2 62.483(5) 3 . ? U2 U1 U2 123.278(10) 26 . ? O8 U2 O9 178.8(3) . . ? O8 U2 O14 92.2(3) . . ? O9 U2 O14 86.6(3) . . ? O8 U2 O12 87.5(3) . . ? O9 U2 O12 93.8(3) . . ? O14 U2 O12 179.7(3) . . ? O8 U2 O2 83.94(13) . . ? O9 U2 O2 95.53(13) . . ? O14 U2 O2 65.38(10) . . ? O12 U2 O2 114.57(10) . . ? O8 U2 O2 83.94(13) . 28 ? O9 U2 O2 95.53(13) . 28 ? O14 U2 O2 65.38(10) . 28 ? O12 U2 O2 114.57(10) . 28 ? O2 U2 O2 128.57(19) . 28 ? O8 U2 O3 100.23(15) . 28 ? O9 U2 O3 80.33(15) . 28 ? O14 U2 O3 116.01(11) . 28 ? O12 U2 O3 64.07(11) . 28 ? O2 U2 O3 175.43(15) . 28 ? O2 U2 O3 54.25(14) 28 28 ? O8 U2 O3 100.23(15) . . ? O9 U2 O3 80.33(15) . . ? O14 U2 O3 116.01(11) . . ? O12 U2 O3 64.07(11) . . ? O2 U2 O3 54.25(14) . . ? O2 U2 O3 175.43(15) 28 . ? O3 U2 O3 122.7(2) 28 . ? O8 U2 P1 94.66(3) . 28 ? O9 U2 P1 85.34(3) . 28 ? O14 U2 P1 89.96(3) . 28 ? O12 U2 P1 90.07(3) . 28 ? O2 U2 P1 155.17(10) . 28 ? O2 U2 P1 27.33(10) 28 28 ? O3 U2 P1 27.12(10) 28 28 ? O3 U2 P1 149.21(11) . 28 ? O8 U2 P1 94.66(3) . . ? O9 U2 P1 85.34(3) . . ? O14 U2 P1 89.96(3) . . ? O12 U2 P1 90.07(3) . . ? O2 U2 P1 27.33(10) . . ? O2 U2 P1 155.17(10) 28 . ? O3 U2 P1 149.21(11) 28 . ? O3 U2 P1 27.12(10) . . ? P1 U2 P1 170.68(6) 28 . ? O8 U2 U3 92.34(18) . . ? O9 U2 U3 86.58(19) . . ? O14 U2 U3 28.966(5) . . ? O12 U2 U3 151.037(4) . . ? O2 U2 U3 36.89(9) . . ? O2 U2 U3 94.17(9) 28 . ? O3 U2 U3 143.81(10) 28 . ? O3 U2 U3 87.55(10) . . ? P1 U2 U3 118.78(3) 28 . ? P1 U2 U3 61.06(3) . . ? O8 U2 U3 92.34(18) . 28 ? O9 U2 U3 86.58(19) . 28 ? O14 U2 U3 28.966(5) . 28 ? O12 U2 U3 151.037(4) . 28 ? O2 U2 U3 94.17(9) . 28 ? O2 U2 U3 36.89(9) 28 28 ? O3 U2 U3 87.55(10) 28 28 ? O3 U2 U3 143.81(10) . 28 ? P1 U2 U3 61.06(3) 28 28 ? P1 U2 U3 118.78(3) . 28 ? U3 U2 U3 57.924(8) . 28 ? O11 U3 O10 177.8(2) . . ? O11 U3 O14 91.8(2) . . ? O10 U3 O14 89.7(2) . . ? O11 U3 O15 90.8(3) . . ? O10 U3 O15 91.2(3) . . ? O14 U3 O15 68.45(19) . . ? O11 U3 O1 90.58(19) . 45 ? O10 U3 O1 89.20(19) . 45 ? O14 U3 O1 139.95(17) . 45 ? O15 U3 O1 71.55(18) . 45 ? O11 U3 O4 89.30(19) . 45 ? O10 U3 O4 88.55(19) . 45 ? O14 U3 O4 146.20(17) . 45 ? O15 U3 O4 145.34(18) . 45 ? O1 U3 O4 73.79(15) 45 45 ? O11 U3 O2 90.05(18) . . ? O10 U3 O2 89.12(19) . . ? O14 U3 O2 68.37(17) . . ? O15 U3 O2 136.82(18) . . ? O1 U3 O2 151.61(15) 45 . ? O4 U3 O2 77.84(15) 45 . ? O11 U3 U3 96.03(15) . 28 ? O10 U3 U3 86.11(15) . 28 ? O14 U3 U3 33.26(13) . 28 ? O15 U3 U3 35.70(14) . 28 ? O1 U3 U3 106.78(11) 45 28 ? O4 U3 U3 174.62(11) 45 28 ? O2 U3 U3 101.37(11) . 28 ? O11 U3 U2 87.04(15) . . ? O10 U3 U2 93.64(15) . . ? O14 U3 U2 27.79(13) . . ? O15 U3 U2 95.88(15) . . ? O1 U3 U2 167.19(11) 45 . ? O4 U3 U2 118.73(10) 45 . ? O2 U3 U2 41.07(11) . . ? U3 U3 U2 61.038(4) 28 . ? OW1 Cd1 OW1 48.1(12) 2_565 . ? OW1 Cd1 O9 93.91(16) 2_565 . ? OW1 Cd1 O9 93.91(16) . . ? OW1 Cd1 O9 93.91(16) 2_565 2_565 ? OW1 Cd1 O9 93.91(16) . 2_565 ? O9 Cd1 O9 171.4(4) . 2_565 ? OW1 Cd1 OW2 119.4(9) 2_565 2_565 ? OW1 Cd1 OW2 167.5(9) . 2_565 ? O9 Cd1 OW2 86.56(15) . 2_565 ? O9 Cd1 OW2 86.56(15) 2_565 2_565 ? OW1 Cd1 OW2 167.5(9) 2_565 . ? OW1 Cd1 OW2 119.4(9) . . ? O9 Cd1 OW2 86.56(15) . . ? O9 Cd1 OW2 86.56(15) 2_565 . ? OW2 Cd1 OW2 73.1(13) 2_565 . ? OW1 Cd1 OW2A 99.9(8) 2_565 2_565 ? OW1 Cd1 OW2A 148.0(8) . 2_565 ? O9 Cd1 OW2A 87.61(11) . 2_565 ? O9 Cd1 OW2A 87.61(11) 2_565 2_565 ? OW2 Cd1 OW2A 19.5(7) 2_565 2_565 ? OW2 Cd1 OW2A 92.6(11) . 2_565 ? OW1 Cd1 OW2A 148.0(8) 2_565 . ? OW1 Cd1 OW2A 99.9(8) . . ? O9 Cd1 OW2A 87.61(11) . . ? O9 Cd1 OW2A 87.61(11) 2_565 . ? OW2 Cd1 OW2A 92.6(11) 2_565 . ? OW2 Cd1 OW2A 19.5(7) . . ? OW2A Cd1 OW2A 112.1(12) 2_565 . ? OW1 Cd1 OW1A 85.1(8) 2_565 . ? OW1 Cd1 OW1A 37.0(7) . . ? O9 Cd1 OW1A 92.07(9) . . ? O9 Cd1 OW1A 92.07(9) 2_565 . ? OW2 Cd1 OW1A 155.5(8) 2_565 . ? OW2 Cd1 OW1A 82.5(8) . . ? OW2A Cd1 OW1A 175.1(7) 2_565 . ? OW2A Cd1 OW1A 62.9(7) . . ? OW1 Cd1 OW1A 37.0(7) 2_565 2_565 ? OW1 Cd1 OW1A 85.1(8) . 2_565 ? O9 Cd1 OW1A 92.07(9) . 2_565 ? O9 Cd1 OW1A 92.07(9) 2_565 2_565 ? OW2 Cd1 OW1A 82.5(8) 2_565 2_565 ? OW2 Cd1 OW1A 155.5(8) . 2_565 ? OW2A Cd1 OW1A 62.9(7) 2_565 2_565 ? OW2A Cd1 OW1A 175.1(7) . 2_565 ? OW1A Cd1 OW1A 122.0(8) . 2_565 ? OW11 Cd2 O5 135.24(13) . 9 ? OW11 Cd2 O5 135.24(13) . . ? O5 Cd2 O5 75.1(2) 9 . ? OW11 Cd2 O5 135.24(13) . 5 ? O5 Cd2 O5 75.1(2) 9 5 ? O5 Cd2 O5 75.1(2) . 5 ? OW11 Cd2 OW3 68.3(2) . 5 ? O5 Cd2 OW3 83.1(3) 9 5 ? O5 Cd2 OW3 156.0(3) . 5 ? O5 Cd2 OW3 89.7(3) 5 5 ? OW11 Cd2 OW3 68.3(2) . . ? O5 Cd2 OW3 156.0(3) 9 . ? O5 Cd2 OW3 89.7(3) . . ? O5 Cd2 OW3 83.1(3) 5 . ? OW3 Cd2 OW3 107.2(2) 5 . ? OW11 Cd2 OW3 68.3(2) . 9 ? O5 Cd2 OW3 89.7(3) 9 9 ? O5 Cd2 OW3 83.1(3) . 9 ? O5 Cd2 OW3 156.0(3) 5 9 ? OW3 Cd2 OW3 107.2(2) 5 9 ? OW3 Cd2 OW3 107.2(2) . 9 ? OW11 Cd2 OW15 21.4(8) . 9 ? O5 Cd2 OW15 115.4(8) 9 9 ? O5 Cd2 OW15 132.9(9) . 9 ? O5 Cd2 OW15 150.8(8) 5 9 ? OW3 Cd2 OW15 66.1(9) 5 9 ? OW3 Cd2 OW15 88.6(8) . 9 ? OW3 Cd2 OW15 52.9(9) 9 9 ? OW11 Cd2 OW15 21.4(8) . 5 ? O5 Cd2 OW15 132.9(9) 9 5 ? O5 Cd2 OW15 150.8(8) . 5 ? O5 Cd2 OW15 115.4(8) 5 5 ? OW3 Cd2 OW15 52.9(9) 5 5 ? OW3 Cd2 OW15 66.1(9) . 5 ? OW3 Cd2 OW15 88.6(8) 9 5 ? OW15 Cd2 OW15 36.9(14) 9 5 ? OW11 Cd2 OW15 21.4(8) . . ? O5 Cd2 OW15 150.8(8) 9 . ? O5 Cd2 OW15 115.4(8) . . ? O5 Cd2 OW15 132.9(9) 5 . ? OW3 Cd2 OW15 88.6(8) 5 . ? OW3 Cd2 OW15 52.9(9) . . ? OW3 Cd2 OW15 66.1(9) 9 . ? OW15 Cd2 OW15 36.9(14) 9 . ? OW15 Cd2 OW15 36.9(14) 5 . ? OW11 Cd2 Cd3 180.0(13) . . ? O5 Cd2 Cd3 44.76(13) 9 . ? O5 Cd2 Cd3 44.76(13) . . ? O5 Cd2 Cd3 44.76(13) 5 . ? OW3 Cd2 Cd3 111.7(2) 5 . ? OW3 Cd2 Cd3 111.7(2) . . ? OW3 Cd2 Cd3 111.7(2) 9 . ? OW15 Cd2 Cd3 158.6(8) 9 . ? OW15 Cd2 Cd3 158.6(8) 5 . ? OW15 Cd2 Cd3 158.6(8) . . ? O5 Cd3 O5 74.93(18) 9 . ? O5 Cd3 O5 74.93(18) 9 5 ? O5 Cd3 O5 74.93(18) . 5 ? O5 Cd3 O5 105.07(18) 9 37 ? O5 Cd3 O5 180.000(1) . 37 ? O5 Cd3 O5 105.07(18) 5 37 ? O5 Cd3 O5 105.07(18) 9 41 ? O5 Cd3 O5 105.07(18) . 41 ? O5 Cd3 O5 180.0(3) 5 41 ? O5 Cd3 O5 74.93(18) 37 41 ? O5 Cd3 O5 180.0(2) 9 45 ? O5 Cd3 O5 105.07(18) . 45 ? O5 Cd3 O5 105.07(18) 5 45 ? O5 Cd3 O5 74.93(18) 37 45 ? O5 Cd3 O5 74.93(18) 41 45 ? O5 Cd3 Cd2 44.62(12) 9 . ? O5 Cd3 Cd2 44.62(12) . . ? O5 Cd3 Cd2 44.62(12) 5 . ? O5 Cd3 Cd2 135.38(12) 37 . ? O5 Cd3 Cd2 135.38(12) 41 . ? O5 Cd3 Cd2 135.38(12) 45 . ? O5 Cd3 Cd2 135.38(12) 9 37 ? O5 Cd3 Cd2 135.38(12) . 37 ? O5 Cd3 Cd2 135.38(12) 5 37 ? O5 Cd3 Cd2 44.62(12) 37 37 ? O5 Cd3 Cd2 44.62(12) 41 37 ? O5 Cd3 Cd2 44.62(12) 45 37 ? Cd2 Cd3 Cd2 180.00(2) . 37 ? O1 P1 O3 114.5(3) . . ? O1 P1 O2 113.4(3) . . ? O3 P1 O2 103.4(3) . . ? O1 P1 C1 107.2(3) . . ? O3 P1 C1 108.3(3) . . ? O2 P1 C1 109.9(3) . . ? O1 P1 U2 124.89(19) . . ? O3 P1 U2 51.97(18) . . ? O2 P1 U2 51.91(18) . . ? C1 P1 U2 127.9(2) . . ? C2 C1 P1 110.9(4) . . ? O4 C2 O5 122.5(6) . . ? O4 C2 C1 118.7(6) . . ? O5 C2 C1 118.8(6) . . ? P1 O1 U3 137.3(3) . 41 ? P1 O2 U3 138.7(3) . . ? P1 O2 U2 100.8(2) . . ? U3 O2 U2 102.04(16) . . ? P1 O3 U1 149.3(3) . . ? P1 O3 U2 100.9(2) . . ? U1 O3 U2 103.69(17) . . ? C2 O4 U3 136.3(4) . 41 ? C2 O5 Cd2 147.5(5) . . ? C2 O5 Cd3 120.3(4) . . ? Cd2 O5 Cd3 90.62(17) . . ? U2 O9 Cd1 179.5(4) . . ? U2 O12 U1 124.52(15) . . ? U2 O12 U1 124.52(15) . 3 ? U1 O12 U1 107.6(3) . 3 ? U2 O14 U3 123.24(13) . . ? U2 O14 U3 123.24(13) . 28 ? U3 O14 U3 113.5(3) . 28 ? U3 O15 U3 108.6(3) 28 . ? OW1A OW1 OW1 147.2(9) . 2_565 ? OW1A OW1 Cd1 81.2(10) . . ? OW1 OW1 Cd1 66.0(6) 2_565 . ? OW1 OW1A Cd1 61.8(9) . . ? OW2A OW2 Cd1 82(3) . . ? OW2 OW2A Cd1 79(3) . . ? OW15 OW11 OW15 119.2(12) 9 5 ? OW15 OW11 OW15 119.2(12) 9 . ? OW15 OW11 OW15 119.2(12) 5 . ? OW15 OW11 Cd2 95(4) 9 . ? OW15 OW11 Cd2 95(4) 5 . ? OW15 OW11 Cd2 95(4) . . ? OW11 OW15 OW15 30.4(6) . 9 ? OW11 OW15 OW15 30.4(6) . 5 ? OW15 OW15 OW15 60.000(6) 9 5 ? OW11 OW15 Cd2 63(4) . . ? OW15 OW15 Cd2 71.6(7) 9 . ? OW15 OW15 Cd2 71.6(7) 5 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.669 _refine_diff_density_min -2.567 _refine_diff_density_rms 0.209 # Attachment 'web_deposit_cif_file_2_AndreaN.Alsobrook_1285604678.cif' data_Mn2[(UO2)6(PO3CH2CO2)3O3(OH)(H2O)2]*16H2O _database_code_depnum_ccdc_archive 'CCDC 794934' #TrackingRef 'web_deposit_cif_file_2_AndreaN.Alsobrook_1285604678.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Mn2[(UO2)6(PO3CH2CO2)3O3(OH)(H2O)2]*16H2O _chemical_formula_sum 'C6 H42 Mn2 O49 P3 U6' _chemical_formula_weight 2529.37 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'I m -3' _symmetry_space_group_name_Hall '-I 2 2 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-z, -x, -y' '-z, x, y' 'z, x, -y' 'z, -x, y' '-y, -z, -x' 'y, -z, x' '-y, z, x' 'y, z, -x' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-z+1/2, -x+1/2, -y+1/2' '-z+1/2, x+1/2, y+1/2' 'z+1/2, x+1/2, -y+1/2' 'z+1/2, -x+1/2, y+1/2' '-y+1/2, -z+1/2, -x+1/2' 'y+1/2, -z+1/2, x+1/2' '-y+1/2, z+1/2, x+1/2' 'y+1/2, z+1/2, -x+1/2' _cell_length_a 26.4013(4) _cell_length_b 26.4013(4) _cell_length_c 26.4013(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 18402.5(5) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3462 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 27.46 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.06280 _exptl_crystal_size_mid 0.05631 _exptl_crystal_size_min 0.05388 _exptl_crystal_density_meas nm _exptl_crystal_density_diffrn 3.652 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 17872 _exptl_absorpt_coefficient_mu 21.802 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.265 _exptl_absorpt_correction_T_max 0.309 _exptl_absorpt_process_details SHELXPREP _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 '0.3 /w exposure' _diffrn_measurement_method 'BRUKER APEX' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number nm _diffrn_standards_interval_count nm _diffrn_standards_interval_time nm _diffrn_standards_decay_% 0 _diffrn_reflns_number 110070 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.0120 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 27.46 _reflns_number_total 3759 _reflns_number_gt 3462 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement 'SMART, SAINT' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXCIF-97 (Sheldrick, 2000)' _refine_special_details ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 1681.4 427.9 2 0.500 0.000 0.330 32.5 10.4 3 0.251 0.000 0.342 7.0 7.2 4 0.749 0.000 0.342 6.8 7.2 5 0.169 0.000 0.500 32.5 10.1 6 0.831 0.000 0.500 32.5 10.1 7 0.500 0.000 0.669 32.5 9.9 8 0.251 0.000 0.658 6.8 7.8 9 0.749 0.000 0.658 6.6 7.7 10 0.500 0.169 0.000 32.5 10.6 11 0.500 0.159 0.250 6.7 7.2 12 0.500 0.159 0.750 6.9 8.0 13 0.500 0.500 0.500 1681.2 427.8 14 0.342 0.251 0.000 7.0 7.5 15 0.658 0.251 0.000 6.8 7.4 16 0.158 0.249 0.500 6.6 7.5 17 0.842 0.249 0.500 6.8 7.6 18 0.000 0.330 0.500 32.5 9.8 19 0.000 0.341 0.250 6.9 7.8 20 0.000 0.341 0.749 6.8 7.0 21 0.331 0.500 0.000 32.5 10.1 22 0.669 0.500 0.000 32.5 10.1 23 0.000 0.500 0.169 32.5 9.9 24 0.000 0.500 0.830 32.4 10.4 25 0.249 0.500 0.158 6.6 7.7 26 0.751 0.500 0.158 6.8 7.8 27 0.249 0.500 0.842 6.8 7.2 28 0.751 0.500 0.842 7.0 7.2 29 0.000 0.669 0.500 32.5 10.6 30 0.000 0.658 0.251 6.7 8.0 31 0.000 0.658 0.749 6.6 7.1 32 0.342 0.749 0.000 6.8 7.6 33 0.658 0.749 0.000 6.6 7.5 34 0.158 0.750 0.500 6.8 7.4 35 0.842 0.750 0.500 7.0 7.5 36 0.500 0.830 0.000 32.5 9.8 37 0.500 0.841 0.249 6.8 7.0 38 0.500 0.841 0.750 6.9 7.8 _platon_squeeze_details 'The water atoms in cages which are in non-disordered (or slightly disordered) were modeled in anisotropic mode. All other where refined as isotropic atoms' 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^)+(0.0143P)^2^+263.6979P] 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 0 _refine_ls_number_reflns 3759 _refine_ls_number_parameters 237 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0218 _refine_ls_R_factor_gt 0.0185 _refine_ls_wR_factor_ref 0.0411 _refine_ls_wR_factor_gt 0.0400 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.005 _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 U1 U 0.368223(8) 0.151088(8) 0.5000 0.00729(5) Uani 1 2 d S . . U2 U 0.5000 0.136448(9) 0.569392(8) 0.01065(5) Uani 1 2 d S . . U3 U 0.238374(6) 0.153871(6) 0.571742(6) 0.00892(4) Uani 1 1 d . . . Mn1 Mn 0.31712(4) 0.31712(4) 0.68288(4) 0.0201(3) Uani 0.75 3 d SP . . Mn2 Mn 0.2500 0.2500 0.7500 0.0207(4) Uani 1 6 d S . . Mn3 Mn 0.35820(5) 0.0000 0.5000 0.0169(3) Uani 1 4 d S . . P1 P 0.36764(4) 0.14336(4) 0.62424(4) 0.0097(2) Uani 1 1 d . . . C1 C 0.38649(17) 0.19118(17) 0.66918(17) 0.0147(9) Uani 1 1 d . . . H1AA H 0.4183 0.1815 0.6847 0.018 Uiso 1 1 calc R . . H1BA H 0.3916 0.2231 0.6517 0.018 Uiso 1 1 calc R . . C2 C 0.34654(16) 0.19805(17) 0.71009(16) 0.0127(8) Uani 1 1 d . . . O1 O 0.23246(12) 0.22161(12) 0.56690(13) 0.0177(7) Uani 1 1 d . . . O2 O 0.5000 0.1044(2) 0.65589(17) 0.0250(11) Uani 1 2 d S . . O3 O 0.5000 0.20118(19) 0.58952(19) 0.0241(11) Uani 1 2 d S . . O4 O 0.41169(11) 0.13346(13) 0.58788(12) 0.0182(7) Uani 1 1 d . . . O5 O 0.24557(12) 0.08671(12) 0.57954(12) 0.0168(7) Uani 1 1 d . . . O6 O 0.35073(12) 0.09778(12) 0.65347(11) 0.0158(6) Uani 1 1 d . . . O7 O 0.33700(12) 0.16193(12) 0.73932(11) 0.0144(6) Uani 1 1 d . . . O8 O 0.32636(11) 0.16519(12) 0.58933(11) 0.0139(6) Uani 1 1 d . . . O9 O 0.18794(19) 0.1416(2) 0.5000 0.0301(13) Uani 1 2 d S . . O10 O 0.5000 0.06982(18) 0.55659(17) 0.0180(10) Uani 1 2 d S . . O11 O 0.37231(17) 0.21931(16) 0.5000 0.0151(9) Uani 1 2 d S . . O12 O 0.45123(17) 0.15032(19) 0.5000 0.0174(10) Uani 1 2 d S . . O13 O 0.36320(17) 0.08204(16) 0.5000 0.0142(9) Uani 1 2 d S . . O14 O 0.28544(15) 0.15288(17) 0.5000 0.0124(9) Uani 1 2 d S . . O15 O 0.32348(12) 0.23966(12) 0.71236(12) 0.0180(7) Uani 1 1 d . . . OW1 O 0.2888(4) 0.0000 0.5398(4) 0.028(2) Uani 0.50 2 d SP . . OW1A O 0.3120(4) 0.0000 0.5730(4) 0.023(2) Uani 0.50 2 d SP . . OW2 O 0.3293(3) 0.2938(3) 0.6054(2) 0.103(3) Uani 1 1 d . . . OW3 O 0.4158(4) 0.0000 0.5584(4) 0.096(4) Uani 1 2 d S . . OW4 O 0.3658(7) 0.3658(7) 0.6342(7) 0.121(11) Uiso 0.50 3 d SP . . OW5 O 0.5000 0.1546(3) 0.7412(2) 0.0451(17) Uani 1 2 d S . . OW6 O 0.5255(5) 0.0000 0.6790(6) 0.068(4) Uani 0.60 2 d SP . . OW7 O 0.2980(5) 0.2938(5) 0.5240(5) 0.091(4) Uiso 0.50 1 d P . . OW8 O 0.4654(9) 0.2787(9) 0.5000 0.078(7) Uiso 0.40 2 d SP . . OW9 O 0.4372(10) 0.2997(10) 0.4775(9) 0.054(6) Uiso 0.20 1 d P . . OW10 O 0.4552(9) 0.3063(9) 0.6132(9) 0.062(6) Uiso 0.25 1 d P . . OW11 O 0.5000 0.3001(15) 0.6156(15) 0.103(11) Uiso 0.30 2 d SP . . OW12 O 0.4104(10) 0.3301(10) 0.4434(9) 0.091(7) Uiso 0.30 1 d P . . OW13 O 0.3696(19) 0.3646(19) 0.4613(18) 0.132(17) Uiso 0.20 1 d P . . 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 U1 0.00553(10) 0.00840(10) 0.00795(10) 0.000 0.000 0.00005(7) U2 0.00526(10) 0.01997(12) 0.00673(10) -0.00228(8) 0.000 0.000 U3 0.00588(7) 0.01051(8) 0.01038(8) -0.00006(5) 0.00053(5) 0.00031(5) Mn1 0.0201(3) 0.0201(3) 0.0201(3) 0.0031(4) 0.0031(4) -0.0031(4) Mn2 0.0207(4) 0.0207(4) 0.0207(4) -0.0093(5) -0.0093(5) 0.0093(5) Mn3 0.0112(6) 0.0088(6) 0.0308(8) 0.000 0.000 0.000 P1 0.0067(5) 0.0162(5) 0.0063(5) 0.0006(4) 0.0002(4) 0.0003(4) C1 0.012(2) 0.017(2) 0.015(2) -0.0022(17) 0.0029(17) -0.0028(17) C2 0.0098(19) 0.017(2) 0.0113(19) -0.0039(16) -0.0021(16) 0.0010(16) O1 0.0182(16) 0.0128(15) 0.0221(17) 0.0015(13) 0.0035(13) 0.0063(13) O2 0.028(3) 0.037(3) 0.009(2) 0.001(2) 0.000 0.000 O3 0.020(2) 0.026(3) 0.027(3) -0.010(2) 0.000 0.000 O4 0.0083(15) 0.036(2) 0.0101(15) -0.0048(14) -0.0001(12) 0.0009(14) O5 0.0185(16) 0.0108(15) 0.0211(17) -0.0004(13) 0.0046(13) -0.0003(12) O6 0.0240(17) 0.0147(15) 0.0087(14) -0.0004(12) 0.0016(13) 0.0037(13) O7 0.0173(16) 0.0149(15) 0.0109(14) -0.0014(12) -0.0004(12) 0.0004(12) O8 0.0076(14) 0.0216(16) 0.0125(15) 0.0042(12) -0.0021(12) -0.0014(12) O9 0.013(2) 0.065(4) 0.012(2) 0.000 0.000 -0.001(2) O10 0.018(2) 0.021(2) 0.015(2) 0.0000(19) 0.000 0.000 O11 0.016(2) 0.010(2) 0.019(2) 0.000 0.000 -0.0023(17) O12 0.010(2) 0.036(3) 0.006(2) 0.000 0.000 0.0010(19) O13 0.015(2) 0.008(2) 0.020(2) 0.000 0.000 0.0003(17) O14 0.0072(19) 0.019(2) 0.011(2) 0.000 0.000 -0.0012(17) O15 0.0191(16) 0.0167(16) 0.0182(17) -0.0002(13) -0.0009(13) 0.0038(13) OW1 0.029(6) 0.018(5) 0.037(6) 0.000 0.018(5) 0.000 OW1A 0.027(6) 0.020(5) 0.023(5) 0.000 0.001(5) 0.000 OW2 0.127(6) 0.138(7) 0.044(3) 0.026(4) 0.042(4) 0.035(5) OW3 0.123(8) 0.021(3) 0.143(9) 0.000 -0.107(7) 0.000 OW5 0.036(3) 0.057(4) 0.042(4) -0.034(3) 0.000 0.000 OW6 0.060(8) 0.044(7) 0.099(11) 0.000 -0.035(7) 0.000 _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 U1 O11 1.804(4) . ? U1 O13 1.828(4) . ? U1 O14 2.186(4) . ? U1 O12 2.192(4) . ? U1 O4 2.630(3) 26_556 ? U1 O4 2.630(3) . ? U1 O8 2.631(3) 26_556 ? U1 O8 2.631(3) . ? U1 P1 3.2865(10) 26_556 ? U1 P1 3.2865(10) . ? U1 U3 3.9173(2) 26_556 ? U1 U3 3.9173(2) . ? U2 O3 1.790(5) . ? U2 O10 1.791(5) . ? U2 O12 2.269(3) . ? U2 O12 2.269(3) 3_656 ? U2 O4 2.383(3) . ? U2 O4 2.383(3) 28_655 ? U2 O2 2.436(5) . ? U2 U2 3.6641(4) 26_556 ? U2 U1 3.9509(2) 3_656 ? U3 O5 1.795(3) . ? U3 O1 1.800(3) . ? U3 O14 2.265(2) . ? U3 O9 2.338(3) . ? U3 O6 2.348(3) 44_455 ? U3 O8 2.388(3) . ? U3 O7 2.393(3) 44_455 ? U3 U3 3.7882(3) 26_556 ? Mn1 OW2 2.160(6) . ? Mn1 OW2 2.160(6) 8_656 ? Mn1 OW2 2.160(6) 11_566 ? Mn1 O15 2.194(3) 11_566 ? Mn1 O15 2.194(3) . ? Mn1 O15 2.194(3) 8_656 ? Mn1 OW4 2.23(3) . ? Mn1 Mn2 3.0692(17) . ? Mn2 O15 2.197(3) 44_455 ? Mn2 O15 2.197(3) 8_656 ? Mn2 O15 2.197(3) 11_566 ? Mn2 O15 2.197(3) . ? Mn2 O15 2.197(3) 37_556 ? Mn2 O15 2.197(3) 47_545 ? Mn2 Mn1 3.0692(17) 37_556 ? Mn3 OW1 2.112(10) 26_556 ? Mn3 OW1 2.112(10) . ? Mn3 OW3 2.167(7) 26_556 ? Mn3 OW3 2.167(7) . ? Mn3 O13 2.170(4) . ? Mn3 O13 2.170(4) 27 ? Mn3 OW1A 2.282(10) 26_556 ? Mn3 OW1A 2.282(10) . ? P1 O6 1.498(3) . ? P1 O4 1.530(3) . ? P1 O8 1.539(3) . ? P1 C1 1.803(5) . ? C1 C2 1.520(6) . ? C1 H1AA 0.9700 . ? C1 H1BA 0.9700 . ? C2 O7 1.252(5) . ? C2 O15 1.257(5) . ? O6 U3 2.348(3) 47_545 ? O7 U3 2.393(3) 47_545 ? O9 U3 2.338(3) 26_556 ? O12 U2 2.269(3) 26_556 ? O14 U3 2.265(2) 26_556 ? OW1 OW1A 1.070(15) . ? OW6 OW6 1.34(3) 2_655 ? OW7 OW7 1.27(3) 26_556 ? OW8 OW9 1.10(3) . ? OW8 OW9 1.10(3) 26_556 ? OW9 OW9 1.19(5) 26_556 ? OW9 OW12 1.40(3) . ? OW10 OW11 1.20(2) . ? OW10 OW13 1.78(5) 31_556 ? OW11 OW10 1.20(2) 28_655 ? OW12 OW13 1.49(5) . ? OW13 OW10 1.78(5) 34_565 ? 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 O11 U1 O13 179.3(2) . . ? O11 U1 O14 92.19(18) . . ? O13 U1 O14 87.08(18) . . ? O11 U1 O12 87.10(19) . . ? O13 U1 O12 93.63(19) . . ? O14 U1 O12 179.29(18) . . ? O11 U1 O4 98.66(10) . 26_556 ? O13 U1 O4 81.67(10) . 26_556 ? O14 U1 O4 116.11(7) . 26_556 ? O12 U1 O4 64.03(7) . 26_556 ? O11 U1 O4 98.66(10) . . ? O13 U1 O4 81.67(10) . . ? O14 U1 O4 116.11(7) . . ? O12 U1 O4 64.03(7) . . ? O4 U1 O4 123.82(13) 26_556 . ? O11 U1 O8 83.33(9) . 26_556 ? O13 U1 O8 96.36(9) . 26_556 ? O14 U1 O8 64.98(7) . 26_556 ? O12 U1 O8 114.92(7) . 26_556 ? O4 U1 O8 54.37(9) 26_556 26_556 ? O4 U1 O8 177.62(10) . 26_556 ? O11 U1 O8 83.33(9) . . ? O13 U1 O8 96.36(9) . . ? O14 U1 O8 64.98(7) . . ? O12 U1 O8 114.92(7) . . ? O4 U1 O8 177.62(10) 26_556 . ? O4 U1 O8 54.37(9) . . ? O8 U1 O8 127.38(13) 26_556 . ? O11 U1 P1 93.57(2) . 26_556 ? O13 U1 P1 86.43(2) . 26_556 ? O14 U1 P1 89.81(2) . 26_556 ? O12 U1 P1 90.23(2) . 26_556 ? O4 U1 P1 27.20(7) 26_556 26_556 ? O4 U1 P1 150.64(7) . 26_556 ? O8 U1 P1 27.40(7) 26_556 26_556 ? O8 U1 P1 154.35(7) . 26_556 ? O11 U1 P1 93.57(2) . . ? O13 U1 P1 86.43(2) . . ? O14 U1 P1 89.81(2) . . ? O12 U1 P1 90.23(2) . . ? O4 U1 P1 150.64(7) 26_556 . ? O4 U1 P1 27.20(7) . . ? O8 U1 P1 154.35(7) 26_556 . ? O8 U1 P1 27.40(7) . . ? P1 U1 P1 172.86(4) 26_556 . ? O11 U1 U3 91.93(12) . 26_556 ? O13 U1 U3 87.43(12) . 26_556 ? O14 U1 U3 28.915(3) . 26_556 ? O12 U1 U3 151.077(4) . 26_556 ? O4 U1 U3 87.63(7) 26_556 26_556 ? O4 U1 U3 144.27(7) . 26_556 ? O8 U1 U3 36.52(6) 26_556 26_556 ? O8 U1 U3 93.62(6) . 26_556 ? P1 U1 U3 60.955(18) 26_556 26_556 ? P1 U1 U3 118.663(19) . 26_556 ? O11 U1 U3 91.93(12) . . ? O13 U1 U3 87.43(12) . . ? O14 U1 U3 28.915(3) . . ? O12 U1 U3 151.077(4) . . ? O4 U1 U3 144.27(7) 26_556 . ? O4 U1 U3 87.63(7) . . ? O8 U1 U3 93.62(6) 26_556 . ? O8 U1 U3 36.52(6) . . ? P1 U1 U3 118.663(19) 26_556 . ? P1 U1 U3 60.955(18) . . ? U3 U1 U3 57.830(5) 26_556 . ? O3 U2 O10 173.6(2) . . ? O3 U2 O12 94.91(19) . . ? O10 U2 O12 90.35(17) . . ? O3 U2 O12 94.91(19) . 3_656 ? O10 U2 O12 90.35(17) . 3_656 ? O12 U2 O12 69.15(18) . 3_656 ? O3 U2 O4 88.32(9) . . ? O10 U2 O4 90.35(9) . . ? O12 U2 O4 67.39(12) . . ? O12 U2 O4 136.54(12) 3_656 . ? O3 U2 O4 88.32(9) . 28_655 ? O10 U2 O4 90.35(9) . 28_655 ? O12 U2 O4 136.54(12) . 28_655 ? O12 U2 O4 67.39(12) 3_656 28_655 ? O4 U2 O4 156.05(15) . 28_655 ? O3 U2 O2 93.1(2) . . ? O10 U2 O2 80.52(19) . . ? O12 U2 O2 144.40(10) . . ? O12 U2 O2 144.40(10) 3_656 . ? O4 U2 O2 78.26(8) . . ? O4 U2 O2 78.26(8) 28_655 . ? O3 U2 U2 107.27(17) . 26_556 ? O10 U2 U2 79.13(15) . 26_556 ? O12 U2 U2 36.16(9) . 26_556 ? O12 U2 U2 36.16(9) 3_656 26_556 ? O4 U2 U2 101.82(7) . 26_556 ? O4 U2 U2 101.82(7) 28_655 26_556 ? O2 U2 U2 159.65(13) . 26_556 ? O3 U2 U1 92.54(8) . . ? O10 U2 U1 90.49(7) . . ? O12 U2 U1 27.14(9) . . ? O12 U2 U1 96.29(9) 3_656 . ? O4 U2 U1 40.25(7) . . ? O4 U2 U1 163.66(8) 28_655 . ? O2 U2 U1 117.955(11) . . ? U2 U2 U1 62.374(3) 26_556 . ? O3 U2 U1 92.54(8) . 3_656 ? O10 U2 U1 90.49(7) . 3_656 ? O12 U2 U1 96.29(9) . 3_656 ? O12 U2 U1 27.14(9) 3_656 3_656 ? O4 U2 U1 163.66(8) . 3_656 ? O4 U2 U1 40.25(7) 28_655 3_656 ? O2 U2 U1 117.955(11) . 3_656 ? U2 U2 U1 62.374(3) 26_556 3_656 ? U1 U2 U1 123.424(6) . 3_656 ? O5 U3 O1 177.25(16) . . ? O5 U3 O14 91.51(15) . . ? O1 U3 O14 89.98(15) . . ? O5 U3 O9 90.90(19) . . ? O1 U3 O9 91.79(19) . . ? O14 U3 O9 68.50(13) . . ? O5 U3 O6 90.93(13) . 44_455 ? O1 U3 O6 89.39(13) . 44_455 ? O14 U3 O6 140.17(12) . 44_455 ? O9 U3 O6 71.71(12) . 44_455 ? O5 U3 O8 89.91(13) . . ? O1 U3 O8 88.50(13) . . ? O14 U3 O8 68.31(11) . . ? O9 U3 O8 136.81(12) . . ? O6 U3 O8 151.45(10) 44_455 . ? O5 U3 O7 89.10(13) . 44_455 ? O1 U3 O7 88.37(13) . 44_455 ? O14 U3 O7 145.81(11) . 44_455 ? O9 U3 O7 145.68(12) . 44_455 ? O6 U3 O7 73.97(11) 44_455 44_455 ? O8 U3 O7 77.51(10) . 44_455 ? O5 U3 U3 96.59(10) . 26_556 ? O1 U3 U3 85.92(11) . 26_556 ? O14 U3 U3 33.27(9) . 26_556 ? O9 U3 U3 35.89(10) . 26_556 ? O6 U3 U3 107.03(8) 44_455 26_556 ? O8 U3 U3 101.22(7) . 26_556 ? O7 U3 U3 174.19(8) 44_455 26_556 ? O5 U3 U1 86.81(10) . . ? O1 U3 U1 93.45(10) . . ? O14 U3 U1 27.81(9) . . ? O9 U3 U1 95.98(10) . . ? O6 U3 U1 167.46(8) 44_455 . ? O8 U3 U1 40.98(7) . . ? O7 U3 U1 118.28(7) 44_455 . ? U3 U3 U1 61.085(3) 26_556 . ? OW2 Mn1 OW2 99.9(3) . 8_656 ? OW2 Mn1 OW2 99.9(3) . 11_566 ? OW2 Mn1 OW2 99.9(3) 8_656 11_566 ? OW2 Mn1 O15 88.0(2) . 11_566 ? OW2 Mn1 O15 163.1(3) 8_656 11_566 ? OW2 Mn1 O15 93.3(2) 11_566 11_566 ? OW2 Mn1 O15 93.3(2) . . ? OW2 Mn1 O15 88.0(2) 8_656 . ? OW2 Mn1 O15 163.1(3) 11_566 . ? O15 Mn1 O15 76.59(14) 11_566 . ? OW2 Mn1 O15 163.1(3) . 8_656 ? OW2 Mn1 O15 93.3(2) 8_656 8_656 ? OW2 Mn1 O15 88.0(2) 11_566 8_656 ? O15 Mn1 O15 76.59(14) 11_566 8_656 ? O15 Mn1 O15 76.59(14) . 8_656 ? OW2 Mn1 OW4 62.1(2) . . ? OW2 Mn1 OW4 62.1(2) 8_656 . ? OW2 Mn1 OW4 62.1(2) 11_566 . ? O15 Mn1 OW4 134.31(9) 11_566 . ? O15 Mn1 OW4 134.31(9) . . ? O15 Mn1 OW4 134.31(9) 8_656 . ? OW2 Mn1 Mn2 117.9(2) . . ? OW2 Mn1 Mn2 117.9(2) 8_656 . ? OW2 Mn1 Mn2 117.9(2) 11_566 . ? O15 Mn1 Mn2 45.69(9) 11_566 . ? O15 Mn1 Mn2 45.69(9) . . ? O15 Mn1 Mn2 45.69(9) 8_656 . ? OW4 Mn1 Mn2 180.0(4) . . ? O15 Mn2 O15 180.00(17) 44_455 8_656 ? O15 Mn2 O15 103.51(13) 44_455 11_566 ? O15 Mn2 O15 76.49(13) 8_656 11_566 ? O15 Mn2 O15 103.51(13) 44_455 . ? O15 Mn2 O15 76.49(13) 8_656 . ? O15 Mn2 O15 76.49(13) 11_566 . ? O15 Mn2 O15 76.49(13) 44_455 37_556 ? O15 Mn2 O15 103.51(13) 8_656 37_556 ? O15 Mn2 O15 103.51(13) 11_566 37_556 ? O15 Mn2 O15 180.000(1) . 37_556 ? O15 Mn2 O15 76.49(13) 44_455 47_545 ? O15 Mn2 O15 103.51(13) 8_656 47_545 ? O15 Mn2 O15 180.000(1) 11_566 47_545 ? O15 Mn2 O15 103.51(13) . 47_545 ? O15 Mn2 O15 76.49(13) 37_556 47_545 ? O15 Mn2 Mn1 134.37(8) 44_455 . ? O15 Mn2 Mn1 45.63(8) 8_656 . ? O15 Mn2 Mn1 45.63(8) 11_566 . ? O15 Mn2 Mn1 45.63(8) . . ? O15 Mn2 Mn1 134.37(8) 37_556 . ? O15 Mn2 Mn1 134.37(8) 47_545 . ? O15 Mn2 Mn1 45.63(8) 44_455 37_556 ? O15 Mn2 Mn1 134.37(8) 8_656 37_556 ? O15 Mn2 Mn1 134.37(8) 11_566 37_556 ? O15 Mn2 Mn1 134.37(8) . 37_556 ? O15 Mn2 Mn1 45.63(8) 37_556 37_556 ? O15 Mn2 Mn1 45.63(8) 47_545 37_556 ? Mn1 Mn2 Mn1 180.00(3) . 37_556 ? OW1 Mn3 OW1 59.7(7) 26_556 . ? OW1 Mn3 OW3 104.8(5) 26_556 26_556 ? OW1 Mn3 OW3 164.4(5) . 26_556 ? OW1 Mn3 OW3 164.4(5) 26_556 . ? OW1 Mn3 OW3 104.8(5) . . ? OW3 Mn3 OW3 90.8(7) 26_556 . ? OW1 Mn3 O13 93.03(11) 26_556 . ? OW1 Mn3 O13 93.03(11) . . ? OW3 Mn3 O13 87.55(9) 26_556 . ? OW3 Mn3 O13 87.55(9) . . ? OW1 Mn3 O13 93.03(11) 26_556 27 ? OW1 Mn3 O13 93.03(11) . 27 ? OW3 Mn3 O13 87.55(9) 26_556 27 ? OW3 Mn3 O13 87.55(9) . 27 ? O13 Mn3 O13 173.0(2) . 27 ? OW1 Mn3 OW1A 27.8(4) 26_556 26_556 ? OW1 Mn3 OW1A 87.5(5) . 26_556 ? OW3 Mn3 OW1A 76.9(4) 26_556 26_556 ? OW3 Mn3 OW1A 167.7(4) . 26_556 ? O13 Mn3 OW1A 91.86(7) . 26_556 ? O13 Mn3 OW1A 91.86(7) 27 26_556 ? OW1 Mn3 OW1A 87.5(5) 26_556 . ? OW1 Mn3 OW1A 27.8(4) . . ? OW3 Mn3 OW1A 167.7(4) 26_556 . ? OW3 Mn3 OW1A 76.9(4) . . ? O13 Mn3 OW1A 91.86(7) . . ? O13 Mn3 OW1A 91.86(7) 27 . ? OW1A Mn3 OW1A 115.4(6) 26_556 . ? O6 P1 O4 114.36(19) . . ? O6 P1 O8 113.47(18) . . ? O4 P1 O8 103.08(17) . . ? O6 P1 C1 107.82(19) . . ? O4 P1 C1 108.83(19) . . ? O8 P1 C1 109.1(2) . . ? O6 P1 U1 124.44(13) . . ? O4 P1 U1 51.76(12) . . ? O8 P1 U1 51.87(12) . . ? C1 P1 U1 127.74(15) . . ? C2 C1 P1 111.1(3) . . ? C2 C1 H1AA 109.4 . . ? P1 C1 H1AA 109.4 . . ? C2 C1 H1BA 109.4 . . ? P1 C1 H1BA 109.4 . . ? H1AA C1 H1BA 108.0 . . ? O7 C2 O15 122.6(4) . . ? O7 C2 C1 119.1(4) . . ? O15 C2 C1 118.3(4) . . ? P1 O4 U2 150.01(19) . . ? P1 O4 U1 101.05(15) . . ? U2 O4 U1 103.91(11) . . ? P1 O6 U3 137.96(19) . 47_545 ? C2 O7 U3 137.0(3) . 47_545 ? P1 O8 U3 139.32(18) . . ? P1 O8 U1 100.74(15) . . ? U3 O8 U1 102.51(11) . . ? U3 O9 U3 108.2(2) . 26_556 ? U1 O12 U2 124.68(10) . . ? U1 O12 U2 124.68(10) . 26_556 ? U2 O12 U2 107.69(18) . 26_556 ? U1 O13 Mn3 179.3(3) . . ? U1 O14 U3 123.27(9) . 26_556 ? U1 O14 U3 123.27(9) . . ? U3 O14 U3 113.46(17) 26_556 . ? C2 O15 Mn1 146.5(3) . . ? C2 O15 Mn2 123.9(3) . . ? Mn1 O15 Mn2 88.69(12) . . ? OW1A OW1 Mn3 84.9(8) . . ? OW1 OW1A Mn3 67.2(7) . . ? OW9 OW8 OW9 65(3) . 26_556 ? OW8 OW9 OW9 57.3(15) . 26_556 ? OW8 OW9 OW12 168(3) . . ? OW9 OW9 OW12 130.1(15) 26_556 . ? OW11 OW10 OW13 91(3) . 31_556 ? OW10 OW11 OW10 163(5) . 28_655 ? OW9 OW12 OW13 121(3) . . ? OW12 OW13 OW10 149(4) . 34_565 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.607 _refine_diff_density_min -1.205 _refine_diff_density_rms 0.150 # Attachment 'web_deposit_cif_file_3_AndreaN.Alsobrook_1285604678.cif' data_r-3 _database_code_depnum_ccdc_archive 'CCDC 794935' #TrackingRef 'web_deposit_cif_file_3_AndreaN.Alsobrook_1285604678.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H12 Cd3 O61 P6 U6' _chemical_formula_sum 'C12 H12 Cd3 O61 P6 U6' _chemical_formula_weight 3083.42 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 18.962(2) _cell_length_b 18.962(2) _cell_length_c 14.0112(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4362.7(10) _cell_formula_units_Z 3 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1937 _cell_measurement_theta_min 1.91 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10265 _exptl_crystal_size_mid 0.08111 _exptl_crystal_size_min 0.06538 _exptl_crystal_density_meas nm _exptl_crystal_density_diffrn 3.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4074 _exptl_absorpt_coefficient_mu 18.011 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.189 _exptl_absorpt_correction_T_max 0.308 _exptl_absorpt_process_details SHELXPREP _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX' _diffrn_measurement_method '0.3 /w exposure' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number na _diffrn_standards_interval_count na _diffrn_standards_interval_time na _diffrn_standards_decay_% 0 _diffrn_reflns_number 17130 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2230 _reflns_number_gt 1937 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement 'SMART, SAINT' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXCIF-97 (Sheldrick, 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^)+(0.0193P)^2^+52.6651P] 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 SHELXL _refine_ls_extinction_coef 0.000038(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2230 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0519 _refine_ls_wR_factor_gt 0.0494 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 U1 U 0.393612(12) -0.034522(13) -0.258795(14) 0.01567(8) Uani 1 1 d . . . Cd1 Cd 0.0000 0.0000 0.0000 0.0161(2) Uani 1 6 d S . . Cd2 Cd 0.0000 0.0000 -0.24159(5) 0.01833(16) Uani 1 3 d S . . P1 P 0.27560(10) 0.04274(9) -0.15464(10) 0.0170(3) Uani 1 1 d . . . O1 O 0.2677(3) 0.1189(3) -0.1575(3) 0.0343(12) Uani 1 1 d . . . O2 O 0.3017(2) 0.0287(2) -0.0567(3) 0.0174(8) Uani 1 1 d . . . O3 O 0.3334(2) 0.0463(2) -0.2334(3) 0.0190(9) Uani 1 1 d . . . O4 O 0.1313(2) -0.0632(2) -0.0164(3) 0.0228(9) Uani 1 1 d . . . O5 O 0.0639(2) -0.0302(2) -0.1188(3) 0.0187(8) Uani 1 1 d . . . O6 O 0.4744(2) 0.0448(3) -0.3228(3) 0.0296(11) Uani 1 1 d . . . O7 O 0.3144(2) -0.1101(2) -0.1891(3) 0.0160(8) Uani 1 1 d . . . O8 O 0.4511(3) 0.0549(3) -0.1107(3) 0.0435(14) Uani 1 1 d . . . O9 O 0.0838(6) 0.1014(7) -0.3358(7) 0.037(3) Uani 0.45 1 d P . . O10 O 0.0000 0.0000 -0.4093(10) 0.027(3) Uiso 0.50 3 d SP . . O11 O -0.0346(5) -0.1341(5) -0.2815(5) 0.031(2) Uani 0.55 1 d P . . C1 C 0.1756(4) -0.0428(4) -0.1779(4) 0.0199(12) Uani 1 1 d . . . H3A H 0.1555 -0.0360 -0.2405 0.024 Uiso 1 1 calc R . . H3B H 0.1778 -0.0938 -0.1795 0.024 Uiso 1 1 calc R . . C2 C 0.1196(4) -0.0467(3) -0.1000(4) 0.0177(12) Uani 1 1 d . . . O1W O 0.1778(5) 0.5657(5) 0.1625(6) 0.0271(19) Uani 0.50 1 d P . . O2W O -0.0951(5) -0.2406(5) -0.3417(5) 0.0186(17) Uani 0.50 1 d P . . 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 U1 0.01061(12) 0.02656(14) 0.00832(11) -0.00196(8) -0.00098(8) 0.00816(10) Cd1 0.0201(3) 0.0201(3) 0.0079(4) 0.000 0.000 0.01007(16) Cd2 0.0233(2) 0.0233(2) 0.0083(3) 0.000 0.000 0.01167(12) P1 0.0319(9) 0.0152(7) 0.0094(6) 0.0026(5) 0.0048(6) 0.0158(7) O1 0.084(4) 0.028(3) 0.0106(19) 0.0010(18) 0.005(2) 0.042(3) O2 0.022(2) 0.016(2) 0.0133(18) 0.0043(15) 0.0043(16) 0.0094(17) O3 0.027(2) 0.014(2) 0.0129(18) 0.0023(15) 0.0074(16) 0.0078(18) O4 0.020(2) 0.024(2) 0.0138(19) 0.0037(17) -0.0013(16) 0.0038(19) O5 0.022(2) 0.022(2) 0.0147(19) 0.0007(16) 0.0020(16) 0.0125(18) O6 0.013(2) 0.046(3) 0.013(2) -0.0025(19) 0.0012(16) 0.002(2) O7 0.016(2) 0.024(2) 0.0127(18) -0.0004(16) 0.0000(15) 0.0131(18) O8 0.022(2) 0.055(3) 0.019(2) -0.019(2) 0.0049(19) -0.006(2) O9 0.033(6) 0.055(7) 0.029(6) 0.026(5) 0.016(5) 0.027(6) O11 0.049(6) 0.028(5) 0.019(4) -0.002(3) -0.007(4) 0.021(4) C1 0.029(3) 0.027(3) 0.011(3) -0.003(2) -0.001(2) 0.019(3) C2 0.026(3) 0.013(3) 0.014(3) 0.000(2) -0.003(2) 0.009(3) O1W 0.031(5) 0.026(5) 0.027(5) 0.003(4) 0.004(4) 0.016(4) O2W 0.022(4) 0.023(4) 0.015(4) -0.001(3) -0.001(3) 0.014(4) _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 U1 O6 1.763(4) . ? U1 O7 1.764(4) . ? U1 O1 2.346(4) 18_544 ? U1 O3 2.350(4) . ? U1 O2 2.375(4) 8_544 ? U1 O4 2.376(4) 8_544 ? U1 O8 2.553(4) . ? Cd1 O5 2.293(4) 11 ? Cd1 O5 2.293(4) 10 ? Cd1 O5 2.293(4) 12 ? Cd1 O5 2.293(4) 3 ? Cd1 O5 2.293(4) . ? Cd1 O5 2.293(4) 2 ? Cd1 Cd2 3.3850(8) 10 ? Cd1 Cd2 3.3850(8) . ? Cd2 O9 2.216(10) 2 ? Cd2 O9 2.216(10) . ? Cd2 O9 2.216(10) 3 ? Cd2 O5 2.334(4) 3 ? Cd2 O5 2.334(4) . ? Cd2 O5 2.334(4) 2 ? Cd2 O10 2.350(15) . ? Cd2 O11 2.355(8) . ? Cd2 O11 2.355(8) 3 ? Cd2 O11 2.355(8) 2 ? P1 O1 1.525(4) . ? P1 O2 1.527(4) . ? P1 O3 1.533(4) . ? P1 C1 1.805(6) . ? O1 U1 2.346(4) 17_554 ? O2 U1 2.375(4) 6 ? O4 C2 1.261(6) . ? O4 U1 2.376(4) 6 ? O5 C2 1.271(7) . ? O9 O11 1.235(13) 2 ? O11 O9 1.235(13) 3 ? C1 C2 1.498(8) . ? C1 H3A 0.9900 . ? C1 H3B 0.9900 . ? 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 O6 U1 O7 176.74(18) . . ? O6 U1 O1 92.32(19) . 18_544 ? O7 U1 O1 86.99(16) . 18_544 ? O6 U1 O3 91.09(18) . . ? O7 U1 O3 87.26(15) . . ? O1 U1 O3 136.91(14) 18_544 . ? O6 U1 O2 90.42(16) . 8_544 ? O7 U1 O2 91.82(15) . 8_544 ? O1 U1 O2 148.78(15) 18_544 8_544 ? O3 U1 O2 74.06(14) . 8_544 ? O6 U1 O4 93.74(18) . 8_544 ? O7 U1 O4 89.15(16) . 8_544 ? O1 U1 O4 74.86(15) 18_544 8_544 ? O3 U1 O4 147.65(14) . 8_544 ? O2 U1 O4 73.94(13) 8_544 8_544 ? O6 U1 O8 86.93(17) . . ? O7 U1 O8 89.85(16) . . ? O1 U1 O8 69.07(18) 18_544 . ? O3 U1 O8 68.25(16) . . ? O2 U1 O8 142.14(17) 8_544 . ? O4 U1 O8 143.92(16) 8_544 . ? O5 Cd1 O5 73.13(15) 11 10 ? O5 Cd1 O5 73.13(15) 11 12 ? O5 Cd1 O5 73.13(15) 10 12 ? O5 Cd1 O5 106.87(15) 11 3 ? O5 Cd1 O5 106.87(15) 10 3 ? O5 Cd1 O5 180.0 12 3 ? O5 Cd1 O5 106.87(15) 11 . ? O5 Cd1 O5 180.0 10 . ? O5 Cd1 O5 106.87(15) 12 . ? O5 Cd1 O5 73.13(15) 3 . ? O5 Cd1 O5 180.0 11 2 ? O5 Cd1 O5 106.87(15) 10 2 ? O5 Cd1 O5 106.87(15) 12 2 ? O5 Cd1 O5 73.13(15) 3 2 ? O5 Cd1 O5 73.13(15) . 2 ? O5 Cd1 Cd2 43.46(9) 11 10 ? O5 Cd1 Cd2 43.46(9) 10 10 ? O5 Cd1 Cd2 43.46(10) 12 10 ? O5 Cd1 Cd2 136.54(10) 3 10 ? O5 Cd1 Cd2 136.54(9) . 10 ? O5 Cd1 Cd2 136.54(9) 2 10 ? O5 Cd1 Cd2 136.54(9) 11 . ? O5 Cd1 Cd2 136.54(9) 10 . ? O5 Cd1 Cd2 136.54(10) 12 . ? O5 Cd1 Cd2 43.46(10) 3 . ? O5 Cd1 Cd2 43.46(9) . . ? O5 Cd1 Cd2 43.46(9) 2 . ? Cd2 Cd1 Cd2 180.0 10 . ? O9 Cd2 O9 88.1(4) 2 . ? O9 Cd2 O9 88.1(4) 2 3 ? O9 Cd2 O9 88.1(4) . 3 ? O9 Cd2 O5 88.9(3) 2 3 ? O9 Cd2 O5 156.9(3) . 3 ? O9 Cd2 O5 114.6(3) 3 3 ? O9 Cd2 O5 156.9(3) 2 . ? O9 Cd2 O5 114.6(3) . . ? O9 Cd2 O5 88.9(3) 3 . ? O5 Cd2 O5 71.64(15) 3 . ? O9 Cd2 O5 114.6(3) 2 2 ? O9 Cd2 O5 88.9(3) . 2 ? O9 Cd2 O5 156.9(3) 3 2 ? O5 Cd2 O5 71.64(15) 3 2 ? O5 Cd2 O5 71.64(15) . 2 ? O9 Cd2 O10 53.4(3) 2 . ? O9 Cd2 O10 53.4(3) . . ? O9 Cd2 O10 53.4(3) 3 . ? O5 Cd2 O10 137.49(9) 3 . ? O5 Cd2 O10 137.49(9) . . ? O5 Cd2 O10 137.49(9) 2 . ? O9 Cd2 O11 86.8(3) 2 . ? O9 Cd2 O11 119.2(4) . . ? O9 Cd2 O11 31.2(3) 3 . ? O5 Cd2 O11 83.5(2) 3 . ? O5 Cd2 O11 79.0(2) . . ? O5 Cd2 O11 146.1(2) 2 . ? O10 Cd2 O11 76.27(19) . . ? O9 Cd2 O11 31.2(3) 2 3 ? O9 Cd2 O11 86.8(3) . 3 ? O9 Cd2 O11 119.2(4) 3 3 ? O5 Cd2 O11 79.0(2) 3 3 ? O5 Cd2 O11 146.1(2) . 3 ? O5 Cd2 O11 83.5(2) 2 3 ? O10 Cd2 O11 76.27(19) . 3 ? O11 Cd2 O11 114.55(14) . 3 ? O9 Cd2 O11 119.2(4) 2 2 ? O9 Cd2 O11 31.2(3) . 2 ? O9 Cd2 O11 86.8(3) 3 2 ? O5 Cd2 O11 146.1(2) 3 2 ? O5 Cd2 O11 83.5(2) . 2 ? O5 Cd2 O11 79.0(2) 2 2 ? O10 Cd2 O11 76.27(19) . 2 ? O11 Cd2 O11 114.55(14) . 2 ? O11 Cd2 O11 114.55(14) 3 2 ? O9 Cd2 Cd1 126.6(3) 2 . ? O9 Cd2 Cd1 126.6(3) . . ? O9 Cd2 Cd1 126.6(3) 3 . ? O5 Cd2 Cd1 42.51(9) 3 . ? O5 Cd2 Cd1 42.51(9) . . ? O5 Cd2 Cd1 42.51(9) 2 . ? O10 Cd2 Cd1 180.000(1) . . ? O11 Cd2 Cd1 103.73(19) . . ? O11 Cd2 Cd1 103.73(19) 3 . ? O11 Cd2 Cd1 103.73(19) 2 . ? O1 P1 O2 112.4(2) . . ? O1 P1 O3 110.3(2) . . ? O2 P1 O3 111.6(2) . . ? O1 P1 C1 106.8(3) . . ? O2 P1 C1 107.0(2) . . ? O3 P1 C1 108.4(2) . . ? P1 O1 U1 143.7(3) . 17_554 ? P1 O2 U1 136.7(2) . 6 ? P1 O3 U1 130.5(2) . . ? C2 O4 U1 138.3(4) . 6 ? C2 O5 Cd1 121.3(3) . . ? C2 O5 Cd2 144.1(4) . . ? Cd1 O5 Cd2 94.02(14) . . ? O11 O9 Cd2 80.7(6) 2 . ? O9 O11 Cd2 68.2(6) 3 . ? C2 C1 P1 108.2(4) . . ? C2 C1 H3A 110.1 . . ? P1 C1 H3A 110.1 . . ? C2 C1 H3B 110.1 . . ? P1 C1 H3B 110.1 . . ? H3A C1 H3B 108.4 . . ? O4 C2 O5 121.6(5) . . ? O4 C2 C1 118.8(5) . . ? O5 C2 C1 119.5(5) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.751 _refine_diff_density_min -1.777 _refine_diff_density_rms 0.190