Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name "O'Hare, Dermot" _publ_contact_author_address ; Chemistry Research Laboratory University of Oxford Oxford OX1 3TA UK ; _publ_contact_author_email dermot.ohare@chem.ox.ac.uk _publ_contact_author_fax 44(1865)285131 _publ_contact_author_phone 44(1865)285130 #------------------ TITLE AND AUTHOR LIST------------------------------------# _publ_section_title ; [(CH3)2NH(CH2)2NH(CH3)2][(UO2)2F2(HPO4)2]: A new organically templated layered uranium phosphate fluoride - Synthesis, structure, characterization, and ion-exchange reactions ; _publ_author_address ; Chemistry Research Laboratory University of Oxford Oxford OX1 3TA UK ; loop_ _publ_author_name 'Kang Min Ok' 'Michael B. Doran' "Dermot O'Hare" data_[TMEDAH2][(UO2)2F2(HPO4)2] _database_code_depnum_ccdc_archive 'CCDC 644037' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; N,N,N',N'-Tetramethylethylenediammonium Uranylphosphatefluoride ; _chemical_formula_sum 'C3 H10 F N O6 P U' _chemical_formula_weight 444.12 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _cell_length_a 8.2189(16) _cell_length_b 12.760(3) _cell_length_c 8.6282(17) _cell_angle_alpha 90 _cell_angle_beta 98.62(3) _cell_angle_gamma 90 _cell_volume 894.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 3.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 18.339 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.08 _exptl_absorpt_correction_T_max 0.23 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_ambient_temperature 150.0(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_unetI/netI 0.0426 _diffrn_reflns_number 3634 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 5.27 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 2031 _reflns_number_gt 1803 _reflns_threshold_expression >3\(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0198P)^2^+1.1455P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2031 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0289 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0551 _refine_ls_wR_factor_gt 0.0529 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.57 _refine_diff_density_min -1.679 _refine_diff_density_rms 0.229 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' 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 0.451807(19) 0.300039(13) 0.072930(18) 0.00694(10) Uani 1 1 d . . . P1 P 0.46573(15) 0.04370(10) 0.23818(13) 0.0080(3) Uani 1 1 d . . . F1 F 0.4778(4) 0.2097(2) -0.1535(3) 0.0153(7) Uani 1 1 d . . . O1 O 0.2408(4) 0.2657(3) 0.0655(4) 0.0130(7) Uani 1 1 d . . . O2 O 0.6613(4) 0.3347(3) 0.0805(4) 0.0129(7) Uani 1 1 d . . . O3 O 0.5418(4) 0.1259(3) 0.1421(4) 0.0115(7) Uani 1 1 d . . . O4 O 0.3670(4) 0.0914(3) 0.3546(3) 0.0103(7) Uani 1 1 d . . . O5 O 0.3368(4) -0.0225(3) 0.1210(4) 0.0117(7) Uani 1 1 d . . . H5 H 0.3841 -0.0504 0.0546 0.018 Uiso 1 1 calc R . . O6 O 0.5984(4) -0.0322(3) 0.3155(3) 0.0089(7) Uani 1 1 d . . . N1 N 1.0824(5) 0.4966(4) 0.2171(5) 0.0145(9) Uani 1 1 d . . . C1 C 0.9759(6) 0.4688(5) 0.0679(5) 0.0153(11) Uani 1 1 d . . . H1A H 0.8620 0.4830 0.0773 0.018 Uiso 1 1 calc R . . H1B H 0.9862 0.3950 0.0477 0.018 Uiso 1 1 calc R . . C2 C 1.0534(7) 0.6065(5) 0.2697(6) 0.0217(12) Uani 1 1 d . . . H2A H 1.1230 0.6199 0.3730 0.032 Uiso 1 1 calc R . . H2B H 0.9340 0.6152 0.2810 0.032 Uiso 1 1 calc R . . H2C H 1.0830 0.6575 0.1900 0.032 Uiso 1 1 calc R . . C3 C 1.0592(6) 0.4177(5) 0.3401(6) 0.0174(11) Uani 1 1 d . . . H3A H 1.1290 0.4384 0.4440 0.026 Uiso 1 1 calc R . . H3B H 1.0950 0.3450 0.3060 0.026 Uiso 1 1 calc R . . H3C H 0.9370 0.4150 0.3540 0.026 Uiso 1 1 calc R . . H4 H 1.1870 0.5040 0.2010 0.025 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.00963(13) 0.00473(13) 0.00673(13) -0.00014(6) 0.00212(7) -0.00031(6) P1 0.0105(6) 0.0055(6) 0.0083(6) -0.0004(5) 0.0018(5) 0.0004(5) F1 0.0319(18) 0.0039(15) 0.0105(14) -0.0010(11) 0.0047(13) 0.0017(12) O1 0.0145(18) 0.0091(18) 0.0154(17) 0.0004(15) 0.0019(14) -0.0003(15) O2 0.0150(17) 0.0068(18) 0.0164(18) 0.0013(15) 0.0009(14) -0.0010(15) O3 0.0147(17) 0.0089(18) 0.0122(16) 0.0022(13) 0.0066(13) 0.0003(14) O4 0.0157(17) 0.0068(17) 0.0087(15) -0.0039(13) 0.0031(13) -0.0018(14) O5 0.0120(16) 0.0132(19) 0.0100(16) -0.0052(14) 0.0017(13) 0.0018(14) O6 0.0114(16) 0.0060(17) 0.0095(16) 0.0018(13) 0.0019(13) 0.0007(13) N1 0.010(2) 0.018(2) 0.015(2) -0.0029(19) -0.0003(17) -0.0013(19) C1 0.014(2) 0.018(3) 0.013(3) -0.001(2) -0.0010(19) -0.001(2) C2 0.021(3) 0.024(3) 0.019(3) -0.004(2) 0.000(2) 0.000(3) C3 0.017(3) 0.022(3) 0.014(2) 0.005(2) 0.003(2) 0.002(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O2 1.770(3) . ? U1 O1 1.780(3) . ? U1 F1 2.305(3) . ? U1 F1 2.341(3) 4_566 ? U1 O4 2.358(3) 4_565 ? U1 O3 2.389(3) . ? U1 O6 2.408(3) 2_655 ? P1 O4 1.511(3) . ? P1 O3 1.528(3) . ? P1 O6 1.535(3) . ? P1 O5 1.593(3) . ? F1 U1 2.341(3) 4_565 ? O4 U1 2.358(3) 4_566 ? O6 U1 2.408(3) 2_645 ? N1 C1 1.487(6) . ? N1 C3 1.496(7) . ? N1 C2 1.503(7) . ? C1 C1 1.519(10) 3_765 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 U1 O1 179.75(16) . . ? O2 U1 F1 86.75(14) . . ? O1 U1 F1 93.42(14) . . ? O2 U1 F1 92.00(14) . 4_566 ? O1 U1 F1 87.96(13) . 4_566 ? F1 U1 F1 145.25(6) . 4_566 ? O2 U1 O4 92.98(14) . 4_565 ? O1 U1 O4 86.90(14) . 4_565 ? F1 U1 O4 70.77(11) . 4_565 ? F1 U1 O4 143.89(10) 4_566 4_565 ? O2 U1 O3 87.72(14) . . ? O1 U1 O3 92.51(14) . . ? F1 U1 O3 71.47(10) . . ? F1 U1 O3 73.78(10) 4_566 . ? O4 U1 O3 142.13(11) 4_565 . ? O2 U1 O6 89.26(14) . 2_655 ? O1 U1 O6 90.50(14) . 2_655 ? F1 U1 O6 145.73(10) . 2_655 ? F1 U1 O6 68.86(10) 4_566 2_655 ? O4 U1 O6 75.47(11) 4_565 2_655 ? O3 U1 O6 142.38(11) . 2_655 ? O4 P1 O3 112.9(2) . . ? O4 P1 O6 112.50(18) . . ? O3 P1 O6 110.31(19) . . ? O4 P1 O5 105.27(18) . . ? O3 P1 O5 107.90(18) . . ? O6 P1 O5 107.63(19) . . ? U1 F1 U1 151.02(13) . 4_565 ? P1 O3 U1 129.61(18) . . ? P1 O4 U1 130.09(19) . 4_566 ? P1 O6 U1 125.56(18) . 2_645 ? C1 N1 C3 109.4(4) . . ? C1 N1 C2 112.6(4) . . ? C3 N1 C2 111.8(4) . . ? N1 C1 C1 110.8(5) . 3_765 ? #===END _chemical_name_common ;N,N,N',N'-Tetramethylethylenediammonium Uranylphosphatefluoride ;