# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Diwu, Juan' 'Albrecht-Schmitt, Thomas' _publ_contact_author_name 'Albrecht-Schmitt, Thomas' _publ_contact_author_email talbrec1@nd.edu _publ_section_title ; Chiral Uranium Phosphonates Constructed from Achiral Units with High Porosity Frameworks ; # Attachment '- final.cif' data_UC1P2N-1 _database_code_depnum_ccdc_archive 'CCDC 867168' #TrackingRef '- final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'uranium methylenediphosphonate' _chemical_melting_point n/a _chemical_formula_moiety UO2[CH2(PO3)2].(C2H4N2H6)(H2O) _chemical_formula_sum 'C H0 O8 P2 U' _chemical_formula_weight 439.98 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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P3(1)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' _cell_length_a 11.883(2) _cell_length_b 11.883(2) _cell_length_c 18.066(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2209.3(7) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5744 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 25.99 _exptl_crystal_description primatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.080 _exptl_crystal_size_mid 0.020 _exptl_crystal_size_min 0.020 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.984 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 11.241 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.764 _exptl_absorpt_correction_T_max 0.799 _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 'Imus microdocused' _diffrn_radiation_monochromator 'Quazar optics' _diffrn_measurement_device_type 'Bruker APEXII' _diffrn_measurement_method '0.3 wide w/ exposures' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26086 _diffrn_reflns_av_R_equivalents 0.1190 _diffrn_reflns_av_sigmaI/netI 0.0758 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 27.58 _reflns_number_total 3413 _reflns_number_gt 2692 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0245P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.009(11) _refine_ls_number_reflns 3413 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0683 _refine_ls_wR_factor_gt 0.0652 _refine_ls_goodness_of_fit_ref 0.887 _refine_ls_restrained_S_all 0.887 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.14348(3) 0.58572(3) 0.042278(17) 0.03020(9) Uani 1 1 d . . . P1 P 0.4871(3) 0.8240(3) 0.03114(12) 0.0357(6) Uani 1 1 d . . . P2 P 0.1758(2) 0.5146(2) 0.23389(11) 0.0300(5) Uani 1 1 d . . . O4 O 0.2118(5) 0.7347(6) -0.0592(3) 0.0316(12) Uani 1 1 d . . . O7 O 0.0909(5) 0.6736(6) 0.0955(3) 0.0334(14) Uani 1 1 d . . . O6 O 0.2064(6) 0.5209(6) 0.1513(3) 0.0336(14) Uani 1 1 d . . . O5 O -0.0344(5) 0.3866(5) 0.0819(3) 0.0284(14) Uani 1 1 d . . . O3 O -0.0311(6) 0.5355(5) -0.0396(3) 0.0326(15) Uani 1 1 d . . . O8 O 0.1991(6) 0.4969(6) -0.0097(3) 0.0384(16) Uani 1 1 d . . . O2 O 0.3565(6) 0.7439(6) 0.0694(3) 0.0430(17) Uani 1 1 d . . . O1 O 0.5848(7) 0.7886(8) 0.0599(4) 0.065(2) Uani 1 1 d . . . C1 C 0.4556(8) 0.7843(9) -0.0662(4) 0.034(2) Uani 1 1 d . . . H1A H 0.5373 0.8332 -0.0946 0.040 Uiso 1 1 calc R . . H1B H 0.4227 0.6904 -0.0734 0.040 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 U1 0.0361(2) 0.0355(2) 0.01497(12) 0.00162(15) 0.00219(15) 0.01489(18) P1 0.0325(14) 0.0441(16) 0.0258(12) 0.0066(12) -0.0034(11) 0.0157(12) P2 0.0370(14) 0.0410(15) 0.0148(10) -0.0005(10) -0.0018(9) 0.0216(13) O4 0.029(3) 0.035(3) 0.024(3) 0.003(3) -0.001(3) 0.011(3) O7 0.039(4) 0.046(4) 0.019(3) 0.004(3) -0.005(2) 0.023(3) O6 0.046(4) 0.044(4) 0.017(3) 0.008(3) 0.008(3) 0.028(3) O5 0.025(3) 0.028(3) 0.020(3) 0.009(2) 0.008(2) 0.005(3) O3 0.034(4) 0.028(4) 0.025(3) 0.003(3) -0.006(3) 0.007(3) O8 0.034(4) 0.056(4) 0.018(3) 0.003(3) 0.007(3) 0.017(3) O2 0.039(4) 0.047(4) 0.022(3) 0.009(3) 0.002(3) 0.006(3) O1 0.066(5) 0.103(7) 0.049(4) 0.010(4) -0.014(4) 0.061(5) C1 0.033(5) 0.038(6) 0.029(5) -0.008(4) -0.001(4) 0.017(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 O7 1.748(6) . ? U1 O8 1.769(6) . ? U1 O2 2.328(6) . ? U1 O5 2.362(5) . ? U1 O6 2.368(5) . ? U1 O3 2.369(5) . ? U1 O4 2.391(5) . ? P1 O1 1.512(7) . ? P1 O2 1.522(6) . ? P1 O3 1.525(6) 4_565 ? P1 C1 1.811(8) . ? P2 O5 1.514(6) 6 ? P2 O4 1.527(6) 2_665 ? P2 O6 1.529(5) . ? P2 C1 1.780(9) 2_665 ? O4 P2 1.527(6) 3_564 ? O5 P2 1.514(6) 6 ? O3 P1 1.525(6) 4_455 ? C1 P2 1.780(9) 3_564 ? 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 O7 U1 O8 178.6(2) . . ? O7 U1 O2 88.4(2) . . ? O8 U1 O2 90.8(3) . . ? O7 U1 O5 91.4(2) . . ? O8 U1 O5 88.7(2) . . ? O2 U1 O5 144.28(18) . . ? O7 U1 O6 90.1(2) . . ? O8 U1 O6 88.5(2) . . ? O2 U1 O6 72.2(2) . . ? O5 U1 O6 72.0(2) . . ? O7 U1 O3 88.0(2) . . ? O8 U1 O3 93.4(2) . . ? O2 U1 O3 142.80(19) . . ? O5 U1 O3 72.82(19) . . ? O6 U1 O3 144.8(2) . . ? O7 U1 O4 94.0(2) . . ? O8 U1 O4 86.8(2) . . ? O2 U1 O4 74.59(19) . . ? O5 U1 O4 140.96(17) . . ? O6 U1 O4 146.4(2) . . ? O3 U1 O4 68.77(18) . . ? O1 P1 O2 110.8(4) . . ? O1 P1 O3 111.8(4) . 4_565 ? O2 P1 O3 110.6(4) . 4_565 ? O1 P1 C1 110.4(4) . . ? O2 P1 C1 105.3(4) . . ? O3 P1 C1 107.7(4) 4_565 . ? O5 P2 O4 111.4(3) 6 2_665 ? O5 P2 O6 112.9(3) 6 . ? O4 P2 O6 107.2(3) 2_665 . ? O5 P2 C1 108.4(4) 6 2_665 ? O4 P2 C1 106.5(4) 2_665 2_665 ? O6 P2 C1 110.2(4) . 2_665 ? P2 O4 U1 137.0(3) 3_564 . ? P2 O6 U1 136.2(3) . . ? P2 O5 U1 135.1(3) 6 . ? P1 O3 U1 135.5(3) 4_455 . ? P1 O2 U1 140.1(3) . . ? P2 C1 P1 110.2(4) 3_564 . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 -0.013 -0.008 -0.002 1229 556 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.684 _refine_diff_density_min -0.702 _refine_diff_density_rms 0.134 #==============END===================== data_KUC1P2-1 _database_code_depnum_ccdc_archive 'CCDC 867169' #TrackingRef '- final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Potassium tetraethylamine uranyl methylenediphosphonate hydrate' _chemical_melting_point N/A _chemical_formula_moiety 'K[N(C2H5)4](UO2)3[CH2(PO3)2]2(H2O)2 1.5H2O' _chemical_formula_sum 'C4 H8 K2 O43 P8 U6' _chemical_formula_weight 2498.24 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' K K 0.2009 0.2494 '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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 23.613(3) _cell_length_b 9.0805(11) _cell_length_c 12.8303(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2751.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 106(2) _cell_measurement_reflns_used 6644 _cell_measurement_theta_min 1.59 _cell_measurement_theta_max 28.64 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.110 _exptl_crystal_size_mid 0.015 _exptl_crystal_size_min 0.011 _exptl_crystal_density_meas N/A _exptl_crystal_density_diffrn 3.016 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2172 _exptl_absorpt_coefficient_mu 18.075 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.729 _exptl_absorpt_correction_T_max 0.820 _exptl_absorpt_process_details SHELTXPREP _exptl_special_details ; ? ; _diffrn_ambient_temperature 106(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Imus microfocused' _diffrn_radiation_monochromator 'Quazar optics' _diffrn_measurement_device_type 'BRUKER apex II' _diffrn_measurement_method '0.5 wide w/ exposures' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6644 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0592 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 28.64 _reflns_number_total 6644 _reflns_number_gt 5839 _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^)+(0.0353P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.426(10) _refine_ls_number_reflns 6644 _refine_ls_number_parameters 279 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0887 _refine_ls_wR_factor_gt 0.0867 _refine_ls_goodness_of_fit_ref 1.194 _refine_ls_restrained_S_all 1.194 _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 0.266936(18) 0.85402(5) 0.34238(3) 0.01218(10) Uani 1 1 d . . . U2 U 0.431579(17) 0.36509(5) 0.07675(3) 0.01365(10) Uani 1 1 d . . . U3 U 0.171733(19) 1.30505(5) 0.14925(4) 0.01621(11) Uani 1 1 d . . . P1 P 0.33773(12) 0.6784(3) 0.1223(2) 0.0130(6) Uani 1 1 d . . . K1 K 0.21205(13) 0.8855(4) 0.0637(2) 0.0382(9) Uani 1 1 d . . . P3 P 0.55325(14) 0.2284(4) 0.0354(3) 0.0187(7) Uani 1 1 d . . . P4 P 0.31449(12) 0.1689(3) 0.1857(2) 0.0112(6) Uani 1 1 d . . . P5 P 0.25846(14) 1.2527(3) 0.3827(2) 0.0140(6) Uani 1 1 d . . . O18 O 0.3705(3) 0.1834(9) 0.1238(5) 0.0115(17) Uani 1 1 d . . . O17 O 0.2985(3) 0.6907(9) 0.2139(6) 0.0183(19) Uani 1 1 d . . . O16 O 0.4103(3) 0.3395(10) -0.0547(6) 0.0212(19) Uani 1 1 d . . . O15 O 0.2995(4) 0.0084(9) 0.2085(6) 0.0169(18) Uani 1 1 d U . . O14 O 0.1985(3) 0.8456(10) 0.2844(6) 0.023(2) Uani 1 1 d . . . O13 O 0.2133(3) 1.3278(9) 0.3178(6) 0.0189(19) Uani 1 1 d . . . O12 O 0.2676(3) 1.3327(8) 0.4861(6) 0.0170(18) Uani 1 1 d U . . O11 O 0.2673(4) 0.2471(9) 0.1275(6) 0.0176(19) Uani 1 1 d . . . O10 O 0.5814(3) 0.1736(10) -0.0604(6) 0.022(2) Uani 1 1 d . . . O9 O 0.3357(4) 0.8605(11) 0.3995(6) 0.026(2) Uani 1 1 d . . . O8 O 0.1547(3) 1.1206(10) 0.1760(7) 0.026(2) Uani 1 1 d . . . O7 O 0.4967(3) 0.1469(10) 0.0579(6) 0.026(2) Uani 1 1 d . . . O6 O 0.2458(3) 1.0887(9) 0.4023(6) 0.0184(19) Uani 1 1 d U . . O5 O 0.5326(3) 0.3899(10) 0.0294(6) 0.022(2) Uani 1 1 d . . . O4 O 0.3561(3) 0.5178(9) 0.1052(7) 0.019(2) Uani 1 1 d . . . O3 O 0.1882(4) 1.4923(10) 0.1200(7) 0.033(3) Uani 1 1 d . . . O2 O 0.2433(6) 0.6013(10) 0.3858(8) 0.056(4) Uani 1 1 d . . . O1 O 0.3108(3) 0.7418(10) 0.0248(6) 0.021(2) Uani 1 1 d . . . O20 O 0.4539(4) 0.3867(10) 0.2071(6) 0.025(2) Uani 1 1 d . . . C2 C 0.5989(5) 0.2125(14) 0.1429(9) 0.020(3) Uani 1 1 d . . . H2A H 0.6094 0.1079 0.1529 0.024 Uiso 1 1 calc R . . H2B H 0.5793 0.2467 0.2066 0.024 Uiso 1 1 calc R . . O19 O 0.0969(4) 1.3938(14) 0.2720(8) 0.051(3) Uani 1 1 d . . . C1 C 0.3233(5) 0.2627(12) 0.3086(9) 0.014(2) Uani 1 1 d . . . H1A H 0.3545 0.2164 0.3485 0.017 Uiso 1 1 calc R . . H1B H 0.3334 0.3670 0.2960 0.017 Uiso 1 1 calc R . . O1W O 0.1248(6) 1.5666(15) 0.4418(11) 0.074(4) Uiso 1 1 d . . . O2W O 0.0053(14) 1.078(3) 0.451(2) 0.094(11) Uiso 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 0.0201(2) 0.00746(19) 0.00901(18) 0.00029(19) 0.00050(17) -0.00037(17) U2 0.00955(19) 0.0166(2) 0.0148(2) -0.0018(2) 0.00108(17) 0.00044(19) U3 0.0146(2) 0.0205(2) 0.0135(2) 0.00036(19) -0.00003(19) 0.00606(18) P1 0.0097(14) 0.0159(17) 0.0135(14) 0.0001(12) -0.0018(11) 0.0010(12) K1 0.0240(15) 0.073(3) 0.0171(14) -0.0169(16) -0.0074(12) 0.0197(16) P3 0.0128(15) 0.0205(18) 0.0229(17) 0.0000(13) 0.0044(12) -0.0061(12) P4 0.0135(14) 0.0111(15) 0.0091(13) 0.0019(11) 0.0012(11) 0.0005(11) P5 0.0229(17) 0.0096(14) 0.0097(14) -0.0005(11) 0.0023(12) 0.0003(13) O18 0.010(4) 0.016(4) 0.008(4) -0.003(3) 0.006(3) -0.005(3) O17 0.018(4) 0.015(4) 0.022(5) -0.003(4) 0.007(4) -0.004(4) O16 0.018(4) 0.030(5) 0.015(4) -0.004(4) -0.005(3) 0.005(4) O15 0.024(4) 0.013(3) 0.014(3) -0.003(3) 0.010(3) -0.005(3) O14 0.023(5) 0.030(5) 0.017(4) -0.008(4) -0.002(4) -0.005(4) O13 0.018(4) 0.025(5) 0.013(4) -0.001(4) 0.006(3) 0.009(4) O12 0.024(3) 0.010(3) 0.016(3) -0.002(3) 0.004(3) 0.005(3) O11 0.022(5) 0.018(4) 0.013(4) 0.002(3) -0.002(4) 0.005(4) O10 0.016(4) 0.031(5) 0.018(4) -0.006(4) 0.010(3) -0.005(4) O9 0.027(5) 0.033(5) 0.018(4) -0.003(4) 0.000(4) -0.005(4) O8 0.021(5) 0.034(6) 0.024(5) 0.010(4) -0.002(4) 0.000(4) O7 0.014(4) 0.033(5) 0.030(5) -0.001(5) 0.006(4) -0.009(4) O6 0.028(4) 0.015(3) 0.012(3) -0.001(3) 0.006(3) 0.000(3) O5 0.016(4) 0.030(5) 0.021(5) -0.002(4) 0.003(4) 0.000(4) O4 0.008(4) 0.016(5) 0.034(5) -0.006(4) 0.005(4) 0.001(3) O3 0.055(7) 0.013(5) 0.031(5) -0.005(4) -0.021(5) 0.010(5) O2 0.139(12) 0.010(5) 0.020(5) -0.002(4) 0.010(6) -0.009(6) O1 0.017(4) 0.035(5) 0.012(4) 0.012(4) -0.005(3) -0.003(4) O20 0.022(5) 0.036(6) 0.018(4) -0.004(4) -0.007(4) -0.008(4) C2 0.019(6) 0.028(7) 0.013(6) 0.007(6) 0.004(5) -0.004(5) O19 0.033(6) 0.087(10) 0.033(6) 0.000(6) 0.003(5) 0.033(6) C1 0.013(6) 0.012(6) 0.017(6) -0.004(5) -0.007(5) 0.008(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 O9 1.783(8) . ? U1 O14 1.780(8) . ? U1 O6 2.320(8) . ? U1 O17 2.339(8) . ? U1 O15 2.347(8) 1_565 ? U1 O12 2.355(7) 3_546 ? U1 O2 2.426(9) . ? U1 K1 3.814(3) . ? U2 O20 1.765(8) . ? U2 O16 1.775(8) . ? U2 O4 2.287(8) . ? U2 O18 2.274(7) . ? U2 O5 2.457(9) 2_665 ? U2 O5 2.472(8) . ? U2 O7 2.519(9) . ? U2 P3 3.174(3) . ? U2 K1 3.845(3) 3_545 ? U2 U2 4.0551(9) 2_665 ? U3 O8 1.756(9) . ? U3 O3 1.784(10) . ? U3 O11 2.334(8) 1_565 ? U3 O1 2.343(8) 3 ? U3 O13 2.384(8) . ? U3 O10 2.427(7) 4_465 ? U3 O19 2.499(10) . ? U3 K1 3.941(3) 3 ? U3 K1 4.078(4) . ? P1 O17 1.501(8) . ? P1 O1 1.517(8) . ? P1 O4 1.537(9) . ? P1 C2 1.814(12) 2_665 ? P1 K1 3.593(4) . ? P1 K1 3.762(5) 3_545 ? K1 O1 2.717(9) . ? K1 O11 2.799(8) 3 ? K1 O14 2.873(8) . ? K1 O8 2.910(10) . ? K1 O16 2.921(8) 3 ? K1 O4 2.956(9) 3 ? K1 O15 2.994(9) 1_565 ? K1 O17 3.317(9) . ? K1 P1 3.762(5) 3 ? K1 P4 3.808(4) 3 ? P3 O10 1.483(8) . ? P3 O7 1.554(8) . ? P3 O5 1.546(9) . ? P3 C2 1.757(12) . ? P4 O11 1.518(8) . ? P4 O15 1.528(8) . ? P4 O18 1.548(7) . ? P4 C1 1.804(11) . ? P4 K1 3.808(4) 3_545 ? P4 K1 3.864(5) 1_545 ? P5 O13 1.515(8) . ? P5 O12 1.528(8) . ? P5 O6 1.539(8) . ? P5 C1 1.805(12) 1_565 ? O16 K1 2.921(8) 3_545 ? O15 U1 2.347(8) 1_545 ? O15 K1 2.994(9) 1_545 ? O12 U1 2.355(7) 3_556 ? O11 U3 2.334(8) 1_545 ? O11 K1 2.799(8) 3_545 ? O10 U3 2.427(7) 4_565 ? O5 U2 2.457(9) 2_665 ? O4 K1 2.956(9) 3_545 ? O1 U3 2.343(8) 3_545 ? C2 P1 1.814(12) 2_665 ? C1 P5 1.805(12) 1_545 ? O2W O2W 1.45(6) 2_575 ? 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 O9 U1 O14 179.3(4) . . ? O9 U1 O6 91.7(4) . . ? O14 U1 O6 89.0(4) . . ? O9 U1 O17 91.2(3) . . ? O14 U1 O17 88.1(3) . . ? O6 U1 O17 152.2(3) . . ? O9 U1 O15 89.0(3) . 1_565 ? O14 U1 O15 91.0(3) . 1_565 ? O6 U1 O15 76.4(3) . 1_565 ? O17 U1 O15 76.0(3) . 1_565 ? O9 U1 O12 86.2(3) . 3_546 ? O14 U1 O12 94.1(3) . 3_546 ? O6 U1 O12 72.0(3) . 3_546 ? O17 U1 O12 135.8(3) . 3_546 ? O15 U1 O12 147.9(3) 1_565 3_546 ? O9 U1 O2 98.4(5) . . ? O14 U1 O2 81.2(4) . . ? O6 U1 O2 138.0(3) . . ? O17 U1 O2 68.6(3) . . ? O15 U1 O2 143.9(3) 1_565 . ? O12 U1 O2 68.2(3) 3_546 . ? O9 U1 K1 133.8(3) . . ? O14 U1 K1 45.8(3) . . ? O6 U1 K1 99.7(2) . . ? O17 U1 K1 59.7(2) . . ? O15 U1 K1 51.7(2) 1_565 . ? O12 U1 K1 139.9(2) 3_546 . ? O2 U1 K1 102.0(3) . . ? O20 U2 O16 178.6(4) . . ? O20 U2 O4 90.8(4) . . ? O16 U2 O4 90.6(3) . . ? O20 U2 O18 91.1(3) . . ? O16 U2 O18 88.7(3) . . ? O4 U2 O18 84.4(3) . . ? O20 U2 O5 91.8(4) . 2_665 ? O16 U2 O5 88.9(3) . 2_665 ? O4 U2 O5 76.0(3) . 2_665 ? O18 U2 O5 160.3(3) . 2_665 ? O20 U2 O5 86.2(3) . . ? O16 U2 O5 93.0(3) . . ? O4 U2 O5 137.4(3) . . ? O18 U2 O5 138.1(3) . . ? O5 U2 O5 61.6(3) 2_665 . ? O20 U2 O7 89.8(4) . . ? O16 U2 O7 88.8(3) . . ? O4 U2 O7 165.4(3) . . ? O18 U2 O7 80.9(3) . . ? O5 U2 O7 118.6(3) 2_665 . ? O5 U2 O7 57.3(3) . . ? O20 U2 P3 86.1(3) . . ? O16 U2 P3 92.7(3) . . ? O4 U2 P3 165.6(2) . . ? O18 U2 P3 109.6(2) . . ? O5 U2 P3 90.1(2) 2_665 . ? O5 U2 P3 28.5(2) . . ? O7 U2 P3 28.86(19) . . ? O20 U2 K1 134.6(3) . 3_545 ? O16 U2 K1 46.5(3) . 3_545 ? O4 U2 K1 50.1(2) . 3_545 ? O18 U2 K1 66.4(2) . 3_545 ? O5 U2 K1 98.29(19) 2_665 3_545 ? O5 U2 K1 137.0(2) . 3_545 ? O7 U2 K1 122.1(2) . 3_545 ? P3 U2 K1 137.63(8) . 3_545 ? O20 U2 U2 72.2(3) . 2_665 ? O16 U2 U2 107.8(3) . 2_665 ? O4 U2 U2 104.7(2) . 2_665 ? O18 U2 U2 160.78(19) . 2_665 ? O5 U2 U2 34.76(19) 2_665 2_665 ? O5 U2 U2 34.5(2) . 2_665 ? O7 U2 U2 89.37(18) . 2_665 ? P3 U2 U2 60.99(6) . 2_665 ? K1 U2 U2 132.36(5) 3_545 2_665 ? O8 U3 O3 178.9(4) . . ? O8 U3 O11 91.7(3) . 1_565 ? O3 U3 O11 88.8(4) . 1_565 ? O8 U3 O1 89.6(4) . 3 ? O3 U3 O1 89.7(4) . 3 ? O11 U3 O1 70.1(3) 1_565 3 ? O8 U3 O13 90.0(3) . . ? O3 U3 O13 91.1(3) . . ? O11 U3 O13 74.3(3) 1_565 . ? O1 U3 O13 144.4(3) 3 . ? O8 U3 O10 88.1(3) . 4_465 ? O3 U3 O10 90.9(4) . 4_465 ? O11 U3 O10 144.3(3) 1_565 4_465 ? O1 U3 O10 74.1(3) 3 4_465 ? O13 U3 O10 141.4(3) . 4_465 ? O8 U3 O19 91.3(4) . . ? O3 U3 O19 88.8(4) . . ? O11 U3 O19 146.2(3) 1_565 . ? O1 U3 O19 143.5(3) 3 . ? O13 U3 O19 72.0(3) . . ? O10 U3 O19 69.4(3) 4_465 . ? O8 U3 K1 118.1(3) . 3 ? O3 U3 K1 61.7(3) . 3 ? O11 U3 K1 44.40(19) 1_565 3 ? O1 U3 K1 42.4(2) 3 3 ? O13 U3 K1 109.03(19) . 3 ? O10 U3 K1 105.8(2) 4_465 3 ? O19 U3 K1 150.4(3) . 3 ? O8 U3 K1 38.3(3) . . ? O3 U3 K1 141.6(3) . . ? O11 U3 K1 62.0(2) 1_565 . ? O1 U3 K1 58.2(2) 3 . ? O13 U3 K1 103.2(2) . . ? O10 U3 K1 98.8(2) 4_465 . ? O19 U3 K1 129.5(3) . . ? K1 U3 K1 79.86(4) 3 . ? O17 P1 O1 111.0(5) . . ? O17 P1 O4 110.9(5) . . ? O1 P1 O4 111.2(5) . . ? O17 P1 C2 110.8(5) . 2_665 ? O1 P1 C2 105.0(5) . 2_665 ? O4 P1 C2 107.8(5) . 2_665 ? O17 P1 K1 67.3(3) . . ? O1 P1 K1 44.1(3) . . ? O4 P1 K1 134.4(3) . . ? C2 P1 K1 115.2(4) 2_665 . ? O17 P1 K1 110.9(3) . 3_545 ? O1 P1 K1 67.3(4) . 3_545 ? O4 P1 K1 47.7(3) . 3_545 ? C2 P1 K1 137.4(4) 2_665 3_545 ? K1 P1 K1 88.81(7) . 3_545 ? O1 K1 O11 58.3(2) . 3 ? O1 K1 O14 102.5(3) . . ? O11 K1 O14 145.8(3) 3 . ? O1 K1 O8 147.4(3) . . ? O11 K1 O8 147.6(3) 3 . ? O14 K1 O8 63.4(3) . . ? O1 K1 O16 140.6(3) . 3 ? O11 K1 O16 94.2(2) 3 3 ? O14 K1 O16 84.9(2) . 3 ? O8 K1 O16 70.4(3) . 3 ? O1 K1 O4 121.9(3) . 3 ? O11 K1 O4 68.6(2) 3 3 ? O14 K1 O4 135.5(3) . 3 ? O8 K1 O4 79.1(2) . 3 ? O16 K1 O4 59.4(2) 3 3 ? O1 K1 O15 72.6(3) . 1_565 ? O11 K1 O15 126.2(3) 3 1_565 ? O14 K1 O15 60.8(2) . 1_565 ? O8 K1 O15 74.9(2) . 1_565 ? O16 K1 O15 139.5(2) 3 1_565 ? O4 K1 O15 132.8(3) 3 1_565 ? O1 K1 O17 47.4(2) . . ? O11 K1 O17 99.3(2) 3 . ? O14 K1 O17 55.2(2) . . ? O8 K1 O17 112.9(2) . . ? O16 K1 O17 123.7(2) 3 . ? O4 K1 O17 167.9(2) 3 . ? O15 K1 O17 54.1(2) 1_565 . ? O1 K1 P1 22.86(17) . . ? O11 K1 P1 78.72(19) 3 . ? O14 K1 P1 79.61(19) . . ? O8 K1 P1 131.67(19) . . ? O16 K1 P1 138.6(2) 3 . ? O4 K1 P1 144.71(19) 3 . ? O15 K1 P1 59.70(18) 1_565 . ? O17 K1 P1 24.68(14) . . ? O1 K1 P1 119.4(2) . 3 ? O11 K1 P1 79.41(18) 3 3 ? O14 K1 P1 132.8(2) . 3 ? O8 K1 P1 69.49(18) . 3 ? O16 K1 P1 76.52(18) 3 3 ? O4 K1 P1 22.63(17) 3 3 ? O15 K1 P1 110.2(2) 1_565 3 ? O17 K1 P1 159.65(18) . 3 ? P1 K1 P1 139.54(11) . 3 ? O1 K1 P4 74.88(19) . 3 ? O11 K1 P4 20.01(17) 3 3 ? O14 K1 P4 138.2(2) . 3 ? O8 K1 P4 135.92(19) . 3 ? O16 K1 P4 74.35(18) 3 3 ? O4 K1 P4 60.27(18) 3 3 ? O15 K1 P4 145.86(19) 1_565 3 ? O17 K1 P4 108.31(18) . 3 ? P1 K1 P4 92.38(10) . 3 ? P1 K1 P4 77.33(8) 3 3 ? O1 K1 U1 81.06(18) . . ? O11 K1 U1 136.8(2) 3 . ? O14 K1 U1 26.39(16) . . ? O8 K1 U1 75.46(17) . . ? O16 K1 U1 111.25(18) 3 . ? O4 K1 U1 154.57(19) 3 . ? O15 K1 U1 37.98(15) 1_565 . ? O17 K1 U1 37.48(14) . . ? P1 K1 U1 58.94(6) . . ? P1 K1 U1 138.91(11) 3 . ? P4 K1 U1 143.63(12) 3 . ? O10 P3 O7 112.3(5) . . ? O10 P3 O5 114.7(5) . . ? O7 P3 O5 101.0(5) . . ? O10 P3 C2 110.4(5) . . ? O7 P3 C2 110.0(5) . . ? O5 P3 C2 108.1(6) . . ? O10 P3 U2 132.5(4) . . ? O7 P3 U2 51.5(4) . . ? O5 P3 U2 49.7(3) . . ? C2 P3 U2 117.1(4) . . ? O11 P4 O15 111.7(5) . . ? O11 P4 O18 109.5(4) . . ? O15 P4 O18 112.1(5) . . ? O11 P4 C1 107.1(5) . . ? O15 P4 C1 108.1(5) . . ? O18 P4 C1 108.1(5) . . ? O11 P4 K1 39.1(3) . 3_545 ? O15 P4 K1 127.9(3) . 3_545 ? O18 P4 K1 70.4(3) . 3_545 ? C1 P4 K1 120.7(4) . 3_545 ? O11 P4 K1 69.6(3) . 1_545 ? O15 P4 K1 45.3(3) . 1_545 ? O18 P4 K1 112.5(3) . 1_545 ? C1 P4 K1 137.8(4) . 1_545 ? K1 P4 K1 84.28(7) 3_545 1_545 ? O13 P5 O12 111.3(4) . . ? O13 P5 O6 112.9(5) . . ? O12 P5 O6 110.2(4) . . ? O13 P5 C1 106.6(5) . 1_565 ? O12 P5 C1 108.2(5) . 1_565 ? O6 P5 C1 107.4(5) . 1_565 ? P4 O18 U2 137.7(5) . . ? P1 O17 U1 142.7(5) . . ? P1 O17 K1 88.0(4) . . ? U1 O17 K1 82.9(2) . . ? U2 O16 K1 107.4(3) . 3_545 ? P4 O15 U1 141.8(5) . 1_545 ? P4 O15 K1 113.4(4) . 1_545 ? U1 O15 K1 90.3(3) 1_545 1_545 ? U1 O14 K1 107.8(4) . . ? P5 O13 U3 138.5(5) . . ? P5 O12 U1 143.3(5) . 3_556 ? P4 O11 U3 139.1(5) . 1_545 ? P4 O11 K1 120.9(4) . 3_545 ? U3 O11 K1 99.9(3) 1_545 3_545 ? P3 O10 U3 139.1(5) . 4_565 ? U3 O8 K1 119.8(4) . . ? P3 O7 U2 99.6(5) . . ? P5 O6 U1 142.4(5) . . ? P3 O5 U2 137.5(5) . 2_665 ? P3 O5 U2 101.9(4) . . ? U2 O5 U2 110.7(3) 2_665 . ? P1 O4 U2 144.9(5) . . ? P1 O4 K1 109.6(4) . 3_545 ? U2 O4 K1 93.5(3) . 3_545 ? P1 O1 U3 143.6(5) . 3_545 ? P1 O1 K1 113.0(4) . . ? U3 O1 K1 102.0(3) 3_545 . ? P3 C2 P1 110.3(6) . 2_665 ? P5 C1 P4 109.8(6) 1_545 . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 0.000 -0.050 0.446 356 19 ' ' 2 0.500 -0.005 0.554 356 19 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 28.64 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 1.166 _refine_diff_density_min -1.054 _refine_diff_density_rms 0.254