# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2006 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 # Attachment 'B609525A.cif' #------------------ SUBMISSION DETAILS --------------------------------------# # Name and address of author for correspondence _publ_contact_author_name "Dermot O'Hare" _publ_contact_author_address ; Inorganic Chemistry Laboratory University of Oxford Oxford OX1 3QR 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 ; [N(CH3)4][(UO2)2F5]: A New Organically Templated Microporous Uranium Oxide Fluoride (MUF-2) ; _publ_author_address ; Inorganic Chemistry Laboratory University of Oxford Oxford OX1 3QR UK ; loop_ _publ_author_name 'Kang Min Ok' 'Michael B. Doran' "Dermot O'Hare" data_[N(CH3)4][(UO2)2F5] _database_code_depnum_ccdc_archive 'CCDC 613404' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; Tetramethylammonium Uranium oxide fluoride ; _chemical_formula_sum 'C4 H12 F5 N O4 U2' _chemical_formula_weight 709.21 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+1/4, x+3/4, z+1/4' 'y+1/4, -x+1/4, z+3/4' '-x+1/2, y, -z+1/2' 'x, -y, -z' 'y+1/4, x+3/4, -z+1/4' '-y+1/4, -x+1/4, -z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+3/4, x+5/4, z+3/4' 'y+3/4, -x+3/4, z+5/4' '-x+1, y+1/2, -z+1' 'x+1/2, -y+1/2, -z+1/2' 'y+3/4, x+5/4, -z+3/4' '-y+3/4, -x+3/4, -z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-1/4, -x-3/4, -z-1/4' '-y-1/4, x-1/4, -z-3/4' 'x-1/2, -y, z-1/2' '-x, y, z' '-y-1/4, -x-3/4, z-1/4' 'y-1/4, x-1/4, z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y+1/4, -x-1/4, -z+1/4' '-y+1/4, x+1/4, -z-1/4' 'x, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' '-y+1/4, -x-1/4, z+1/4' 'y+1/4, x+1/4, z-1/4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I 41/a m d' _cell_length_a 7.2721(10) _cell_length_b 7.2721(10) _cell_length_c 23.632(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1249.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 3.770 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 25.945 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.060 _exptl_absorpt_correction_T_max 0.075 #----------------------------------------------------------------------------# # 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 0.0358 _diffrn_reflns_av_unetI/netI 0.0396 _diffrn_reflns_number 1259 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 5.14 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_standards_decay_% 0 _reflns_number_total 418 _reflns_number_gt 340 _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^)+(0.0189P)^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_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.00185(14) _refine_ls_number_reflns 418 _refine_ls_number_parameters 28 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0316 _refine_ls_R_factor_gt 0.0209 _refine_ls_wR_factor_ref 0.0465 _refine_ls_wR_factor_gt 0.0436 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.629 _refine_diff_density_min -1.118 _refine_diff_density_rms 0.216 #----------------------------------------------------------------------------# # 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' 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 0.75 0.028507(15) 0.00883(19) Uani 1 4 d S . . F1 F 0 0.4390(6) 0.05092(17) 0.0162(10) Uani 1 2 d S . . F2 F 0 0.75 0.125 0.0152(18) Uani 1 8 d S . . N1 N 0.5 0.25 0.125 0.012(3) Uani 1 8 d S . . O1 O 0.2433(7) 0.75 0.02792(19) 0.0161(12) Uani 1 2 d S . . C1 C 0.5 0.4175(13) 0.0886(4) 0.032(2) Uani 1 2 d S . . H1A H 0.3922 0.4174 0.0651 0.047 Uiso 0.5 1 calc PR . . H1B H 0.6078 0.4175 0.0651 0.047 Uiso 0.5 1 calc PR . . H1C H 0.4999 0.5252 0.112 0.047 Uiso 1 2 calc SR . . 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 0.0134(3) 0.0065(3) 0.0066(2) 0 0 0 F1 0.031(3) 0.007(2) 0.011(2) 0.0004(18) 0 0 F2 0.017(3) 0.017(3) 0.011(4) 0 0 0 N1 0.011(4) 0.011(4) 0.014(6) 0 0 0 O1 0.015(3) 0.018(3) 0.015(3) 0 -0.001(2) 0 C1 0.042(6) 0.022(5) 0.031(5) 0.001(4) 0 0 #----------------------------------------------------------------------------# # 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 O1 1.769(5) 10_464 ? U1 O1 1.769(5) . ? U1 F2 2.2803(6) . ? U1 F1 2.323(4) 10_464 ? U1 F1 2.323(4) . ? U1 F1 2.327(4) 17_565 ? U1 U1 3.8777(5) 17_565 ? F1 U1 2.327(4) 17_565 ? F2 U1 2.2803(6) 27_465 ? N1 C1 1.491(9) 10_554 ? N1 C1 1.491(9) 20_656 ? N1 C1 1.491(9) . ? N1 C1 1.491(9) 27_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 O1 U1 O1 179.1(3) 10_464 . ? O1 U1 F2 90.45(14) 10_464 . ? O1 U1 F2 90.45(14) . . ? O1 U1 F1 90.10(3) 10_464 10_464 ? O1 U1 F1 90.10(3) . 10_464 ? F2 U1 F1 76.82(10) . 10_464 ? O1 U1 F1 90.10(3) 10_464 . ? O1 U1 F1 90.10(3) . . ? F2 U1 F1 76.82(10) . . ? F1 U1 F1 153.6(2) 10_464 . ? O1 U1 F1 89.64(12) 10_464 17_565 ? O1 U1 F1 89.64(12) . 17_565 ? F2 U1 F1 143.78(10) . 17_565 ? F1 U1 F1 139.40(11) 10_464 17_565 ? F1 U1 F1 66.96(17) . 17_565 ? O1 U1 F1 89.64(12) 10_464 26 ? O1 U1 F1 89.64(12) . 26 ? F2 U1 F1 143.78(10) . 26 ? F1 U1 F1 66.96(17) 10_464 26 ? F1 U1 F1 139.40(11) . 26 ? F1 U1 F1 72.4(2) 17_565 26 ? O1 U1 U1 89.84(5) 10_464 17_565 ? O1 U1 U1 89.84(5) . 17_565 ? F2 U1 U1 110.332(11) . 17_565 ? F1 U1 U1 172.85(10) 10_464 17_565 ? F1 U1 U1 33.52(10) . 17_565 ? F1 U1 U1 33.45(10) 17_565 17_565 ? F1 U1 U1 105.89(11) 26 17_565 ? O1 U1 U1 89.84(5) 10_464 17_575 ? O1 U1 U1 89.84(5) . 17_575 ? F2 U1 U1 110.332(11) . 17_575 ? F1 U1 U1 33.52(10) 10_464 17_575 ? F1 U1 U1 172.85(10) . 17_575 ? F1 U1 U1 105.89(11) 17_565 17_575 ? F1 U1 U1 33.45(10) 26 17_575 ? U1 U1 U1 139.34(2) 17_565 17_575 ? U1 F1 U1 113.04(17) . 17_565 ? U1 F2 U1 180 . 27_465 ? C1 N1 C1 109.5(4) 10_554 20_656 ? C1 N1 C1 109.5(7) 10_554 . ? C1 N1 C1 109.5(4) 20_656 . ? C1 N1 C1 109.5(4) 10_554 27_565 ? C1 N1 C1 109.5(7) 20_656 27_565 ? C1 N1 C1 109.5(4) . 27_565 ? _chemical_name_common 'Tetramethylammonium Uranium oxide fluoride' #===END data_[N(CH3)4][(UO2)(NO3)3] _database_code_depnum_ccdc_archive 'CCDC 613405' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; Tetramethylammonium uranium oxide nitrate ; _chemical_formula_sum 'C4 H12 N4 O11 U' _chemical_formula_weight 530.21 #----------------------------------------------------------------------------# # 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 7.7670(16) _cell_length_b 16.964(3) _cell_length_c 11.255(2) _cell_angle_alpha 90 _cell_angle_beta 105.98(3) _cell_angle_gamma 90 _cell_volume 1425.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 2.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976.0 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 11.444 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.35 _exptl_absorpt_correction_T_max 0.50 #----------------------------------------------------------------------------# # 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 0.0371 _diffrn_reflns_av_unetI/netI 0.0597 _diffrn_reflns_number 5971 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 5.16 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 3221 _reflns_number_gt 2403 _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^)+(0.0282P)^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_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0027(2) _refine_ls_number_reflns 3221 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0655 _refine_ls_wR_factor_gt 0.0585 _refine_ls_goodness_of_fit_ref 0.89 _refine_ls_restrained_S_all 0.89 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.257 _refine_diff_density_min -1.001 _refine_diff_density_rms 0.166 #----------------------------------------------------------------------------# # 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' 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 -0.00161(3) 0.725478(11) 0.007579(16) 0.02194(10) Uani 1 1 d . . . O1 O -0.1297(5) 0.7639(2) -0.1346(3) 0.0284(9) Uani 1 1 d . . . O2 O 0.1243(5) 0.6869(2) 0.1500(3) 0.0329(9) Uani 1 1 d . . . O3 O -0.3170(6) 0.8580(2) 0.1714(4) 0.0451(12) Uani 1 1 d . . . O4 O -0.0782(6) 0.8455(2) 0.1063(4) 0.0379(11) Uani 1 1 d . . . O5 O -0.2586(6) 0.7472(2) 0.0915(4) 0.0307(9) Uani 1 1 d . . . O6 O 0.4230(6) 0.8253(3) -0.0866(4) 0.0516(12) Uani 1 1 d . . . O7 O 0.2631(6) 0.7217(2) -0.0734(4) 0.0369(10) Uani 1 1 d . . . O8 O 0.2106(6) 0.8321(2) 0.0073(4) 0.0418(11) Uani 1 1 d . . . O9 O -0.1635(6) 0.5031(2) -0.1261(4) 0.0322(9) Uani 1 1 d . . . O10 O -0.2007(5) 0.6085(2) -0.0236(3) 0.0243(8) Uani 1 1 d . . . O11 O 0.0259(5) 0.6012(2) -0.1009(3) 0.0264(9) Uani 1 1 d . . . N1 N -0.2237(7) 0.8181(3) 0.1247(4) 0.0341(12) Uani 1 1 d . . . N2 N 0.3041(7) 0.7949(3) -0.0533(5) 0.0393(13) Uani 1 1 d . . . N3 N -0.1136(6) 0.5679(3) -0.0859(4) 0.0232(10) Uani 1 1 d . . . N4 N 0.3266(6) 0.4792(3) -0.2675(4) 0.0246(10) Uani 1 1 d . . . C1 C 0.1288(8) 0.4655(4) -0.3027(6) 0.0381(14) Uani 1 1 d . . . H1A H 0.1008 0.419 -0.3531 0.057 Uiso 1 1 calc R . . H1B H 0.0685 0.51 -0.3482 0.057 Uiso 1 1 calc R . . H1C H 0.0901 0.4585 -0.2294 0.057 Uiso 1 1 calc R . . C2 C 0.3874(10) 0.4912(3) -0.3818(5) 0.0379(16) Uani 1 1 d . . . H2A H 0.3616 0.4448 -0.4323 0.057 Uiso 1 1 calc R . . H2B H 0.514 0.501 -0.3588 0.057 Uiso 1 1 calc R . . H2C H 0.3255 0.5355 -0.4273 0.057 Uiso 1 1 calc R . . C3 C 0.4212(8) 0.4092(3) -0.2000(5) 0.0345(14) Uani 1 1 d . . . H3A H 0.3929 0.3635 -0.2521 0.052 Uiso 1 1 calc R . . H3B H 0.3834 0.4007 -0.1266 0.052 Uiso 1 1 calc R . . H3C H 0.5481 0.4182 -0.1777 0.052 Uiso 1 1 calc R . . C4 C 0.3678(9) 0.5514(4) -0.1894(6) 0.0409(16) Uani 1 1 d . . . H4A H 0.4944 0.561 -0.1669 0.061 Uiso 1 1 calc R . . H4B H 0.3294 0.544 -0.116 0.061 Uiso 1 1 calc R . . H4C H 0.3059 0.5957 -0.2349 0.061 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 0.02666(13) 0.01618(13) 0.02127(13) -0.00025(9) 0.00372(8) -0.00155(10) O1 0.038(2) 0.022(2) 0.0244(19) 0.0006(16) 0.0073(18) -0.0018(18) O2 0.040(3) 0.026(2) 0.029(2) 0.0027(17) 0.0023(18) 0.0030(19) O3 0.053(3) 0.043(3) 0.037(2) -0.009(2) 0.009(2) 0.022(2) O4 0.053(3) 0.025(2) 0.033(2) -0.0048(17) 0.009(2) 0.001(2) O5 0.036(3) 0.028(2) 0.029(2) -0.0036(17) 0.0113(19) 0.0045(19) O6 0.042(3) 0.057(3) 0.054(3) 0.019(2) 0.010(2) -0.025(3) O7 0.030(2) 0.032(3) 0.051(3) -0.004(2) 0.016(2) -0.0101(19) O8 0.052(3) 0.027(2) 0.046(2) -0.006(2) 0.011(2) -0.013(2) O9 0.032(2) 0.015(2) 0.048(3) -0.0045(18) 0.009(2) -0.0030(19) O10 0.024(2) 0.022(2) 0.030(2) -0.0008(16) 0.0130(17) 0.0010(16) O11 0.028(2) 0.021(2) 0.034(2) -0.0037(16) 0.0151(18) -0.0036(16) N1 0.042(3) 0.036(3) 0.022(2) -0.002(2) 0.003(2) 0.011(3) N2 0.036(3) 0.041(3) 0.037(3) 0.005(2) 0.002(3) -0.016(3) N3 0.022(3) 0.022(3) 0.025(2) 0.001(2) 0.006(2) -0.005(2) N4 0.023(3) 0.019(2) 0.035(3) -0.0060(19) 0.013(2) -0.0007(18) C1 0.023(3) 0.031(3) 0.057(4) -0.015(3) 0.006(3) -0.002(3) C2 0.054(4) 0.032(4) 0.032(3) 0.009(3) 0.020(3) 0.004(3) C3 0.031(4) 0.039(4) 0.036(3) 0.003(3) 0.012(3) 0.000(3) C4 0.036(4) 0.030(4) 0.057(4) -0.026(3) 0.014(3) -0.006(3) #----------------------------------------------------------------------------# # 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 1.758(4) . ? U1 O1 1.760(4) . ? U1 O8 2.448(4) . ? U1 O5 2.460(4) . ? U1 O7 2.468(4) . ? U1 O4 2.469(4) . ? U1 O11 2.475(3) . ? U1 O10 2.481(4) . ? U1 N2 2.897(5) . ? U1 N1 2.904(4) . ? U1 N3 2.917(5) . ? O3 N1 1.212(5) . ? O4 N1 1.291(6) . ? O5 N1 1.265(6) . ? O6 N2 1.204(6) . ? O7 N2 1.286(6) . ? O8 N2 1.289(6) . ? O9 N3 1.211(5) . ? O10 N3 1.298(5) . ? O11 N3 1.274(5) . ? N4 C4 1.490(7) . ? N4 C3 1.491(7) . ? N4 C1 1.495(7) . ? N4 C2 1.501(6) . ? 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 179.42(16) . . ? O2 U1 O8 94.06(17) . . ? O1 U1 O8 86.40(16) . . ? O2 U1 O5 90.71(16) . . ? O1 U1 O5 88.76(15) . . ? O8 U1 O5 120.51(14) . . ? O2 U1 O7 90.92(16) . . ? O1 U1 O7 89.64(16) . . ? O8 U1 O7 52.32(13) . . ? O5 U1 O7 172.76(14) . . ? O2 U1 O4 92.26(16) . . ? O1 U1 O4 87.58(15) . . ? O8 U1 O4 68.72(14) . . ? O5 U1 O4 51.84(14) . . ? O7 U1 O4 121.03(14) . . ? O2 U1 O11 91.74(15) . . ? O1 U1 O11 88.35(15) . . ? O8 U1 O11 118.62(12) . . ? O5 U1 O11 120.44(13) . . ? O7 U1 O11 66.56(12) . . ? O4 U1 O11 171.34(14) . . ? O2 U1 O10 89.98(16) . . ? O1 U1 O10 89.62(15) . . ? O8 U1 O10 169.96(11) . . ? O5 U1 O10 68.55(12) . . ? O7 U1 O10 118.51(12) . . ? O4 U1 O10 120.36(12) . . ? O11 U1 O10 51.96(11) . . ? O2 U1 N2 94.63(17) . . ? O1 U1 N2 85.94(16) . . ? O8 U1 N2 26.23(13) . . ? O5 U1 N2 146.57(14) . . ? O7 U1 N2 26.21(13) . . ? O4 U1 N2 94.92(15) . . ? O11 U1 N2 92.40(14) . . ? O10 U1 N2 144.23(13) . . ? O2 U1 N1 92.20(15) . . ? O1 U1 N1 87.40(15) . . ? O8 U1 N1 94.90(15) . . ? O5 U1 N1 25.62(14) . . ? O7 U1 N1 147.22(14) . . ? O4 U1 N1 26.24(14) . . ? O11 U1 N1 145.84(14) . . ? O10 U1 N1 94.12(13) . . ? N2 U1 N1 121.03(16) . . ? O2 U1 N3 91.34(16) . . ? O1 U1 N3 88.49(15) . . ? O8 U1 N3 144.18(12) . . ? O5 U1 N3 94.76(12) . . ? O7 U1 N3 92.25(12) . . ? O4 U1 N3 146.43(13) . . ? O11 U1 N3 25.70(10) . . ? O10 U1 N3 26.27(10) . . ? N2 U1 N3 118.02(13) . . ? N1 U1 N3 120.27(13) . . ? N1 O4 U1 96.0(3) . . ? N1 O5 U1 97.2(3) . . ? N2 O7 U1 95.8(3) . . ? N2 O8 U1 96.7(3) . . ? N3 O10 U1 95.9(3) . . ? N3 O11 U1 96.9(3) . . ? O3 N1 O5 123.6(5) . . ? O3 N1 O4 121.5(5) . . ? O5 N1 O4 114.9(4) . . ? O3 N1 U1 178.4(4) . . ? O5 N1 U1 57.2(2) . . ? O4 N1 U1 57.7(2) . . ? O6 N2 O7 122.2(5) . . ? O6 N2 O8 123.2(5) . . ? O7 N2 O8 114.6(4) . . ? O6 N2 U1 175.3(4) . . ? O7 N2 U1 58.0(2) . . ? O8 N2 U1 57.1(3) . . ? O9 N3 O11 123.3(4) . . ? O9 N3 O10 121.5(4) . . ? O11 N3 O10 115.2(4) . . ? O9 N3 U1 178.7(4) . . ? O11 N3 U1 57.4(2) . . ? O10 N3 U1 57.8(2) . . ? C4 N4 C3 111.0(5) . . ? C4 N4 C1 108.8(4) . . ? C3 N4 C1 109.7(4) . . ? C4 N4 C2 109.1(4) . . ? C3 N4 C2 108.5(4) . . ? C1 N4 C2 109.7(5) . . ? #===END _chemical_name_common 'Tetramethylammonium uranium oxide nitrate'