Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_smw89 _database_code_CSD 168965 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Doran, Michael' 'O'Hare, Dermot' 'Walker, Susan M.' _publ_contact_author_name 'Prof Dermot O'Hare' _publ_contact_author_address ; Prof Dermot O'Hare Inorganuc Chemistry University of Oxford South Parks Rd Oxford Oxon OX1 3QR UNITED KINGDOM ; _publ_contact_author_email 'DERMOT.OHARE@CHEM.OX.AC.UK' _publ_section_title ; Synthesis and Characterisation of (C4N2H12)(UO2)2(PO3H)2(PO2(OH)H)2: a three dimensionally connected actinide framework ; _audit_creation_date 2001-07-26T14:56:24-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C4 H12 N2 O8 P2 U2' _chemical_formula_structural 'U2 O8 P2 C4 N2 H12' _chemical_formula_sum 'C4 H18 N2 O16 P4 U2' _chemical_formula_weight 950.14 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.758(5) _cell_length_b 8.180(5) _cell_length_c 18.037(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 106.647(5) _cell_angle_gamma 90.000(5) _cell_volume 1944.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8604 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 3.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 17.042 _exptl_absorpt_correction_type sphere _exptl_absorpt_process_details ; Interpolation using Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3 for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959) p.302; Table 5.3.6 B for muR in the range 2.6-10.0. The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975) A31,146-148) is used with some modification. ; _exptl_absorpt_correction_T_min 0.0104 _exptl_absorpt_correction_T_max 0.0273 _exptl_absorpt_correction_T_ave 0.0206 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_number 8286 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_unetI/netI 0.0678 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.2 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 4467 _reflns_number_gt 3315 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # 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^)+(0.1046P)^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_number_reflns 4467 _refine_ls_number_parameters 255 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.1669 _refine_ls_wR_factor_gt 0.1052 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.353 _refine_diff_density_min -2.379 _refine_diff_density_rms 0.777 #----------------------------------------------------------------------------# # 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' 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 0.76746(4) 1.07603(6) 0.45994(3) 0.02348(18) Uani 1 1 d . . . U2 U 0.91195(4) 0.78605(6) 0.73467(3) 0.02339(17) Uani 1 1 d . . . P1 P 1.0049(3) 1.0550(4) 0.6096(2) 0.0231(7) Uani 1 1 d . . . H1 H 1.0272 1.1211 0.6567 0.028 Uiso 1 1 calc R . . P2 P 0.7693(3) 1.1553(4) 0.6578(2) 0.0238(7) Uani 1 1 d . . . H2 H 0.8381 1.2001 0.6758 0.029 Uiso 1 1 calc R . . O5 O 0.9261(7) 1.1573(13) 0.5503(6) 0.029(2) Uani 1 1 d . . . O9 O 0.9546(8) 0.9033(11) 0.6304(6) 0.029(2) Uani 1 1 d . . . O1 O 0.7541(8) 0.8740(12) 0.4910(6) 0.032(2) Uani 1 1 d . . . O6 O 0.8575(8) 0.6211(12) 0.6728(6) 0.032(2) Uani 1 1 d . . . O2 O 0.7736(8) 1.2763(13) 0.4234(6) 0.035(2) Uani 1 1 d . . . O12 O 1.0975(8) 1.0178(14) 0.5853(6) 0.035(2) Uani 1 1 d . . . O3 O 0.7328(7) 1.1770(12) 0.5701(5) 0.027(2) Uani 1 1 d . . . O4 O 0.6985(8) 0.9881(16) 0.3271(7) 0.044(3) Uani 1 1 d . . . N1 N 0.5373(9) 1.3413(14) 0.5361(7) 0.029(3) Uani 1 1 d . . . H1A H 0.5468 1.2831 0.4964 0.034 Uiso 1 1 calc R . . H1B H 0.5553 1.2786 0.5789 0.034 Uiso 1 1 calc R . . C1 C 0.6037(11) 1.497(2) 0.5487(9) 0.035(3) Uani 1 1 d . . . H1C H 0.5995 1.5525 0.5952 0.041 Uiso 1 1 calc R . . H1D H 0.6739 1.4669 0.5558 0.041 Uiso 1 1 calc R . . C2 C 0.5695(10) 0.6118(17) 0.4807(8) 0.025(3) Uani 1 1 d . . . H2A H 0.6111 0.7097 0.4912 0.03 Uiso 1 1 calc R . . H2B H 0.5801 0.5596 0.4353 0.03 Uiso 1 1 calc R . . O7 O 0.9733(8) 0.9486(12) 0.7961(6) 0.030(2) Uani 1 1 d . . . O8 O 0.7755(7) 0.9752(12) 0.6796(6) 0.028(2) Uani 1 1 d . . . O13 O 0.7038(8) 1.2530(12) 0.6946(6) 0.030(2) Uani 1 1 d . . . O11 O 0.9844(8) 0.6074(11) 0.8455(6) 0.027(2) Uani 1 1 d . . . O10 O 1.0765(8) 0.6912(15) 0.7301(7) 0.040(3) Uani 1 1 d . . . O14 O 0.5852(8) 1.1221(12) 0.4266(6) 0.031(2) Uani 1 1 d . . . P3 P 0.9983(3) 0.4261(4) 0.8581(2) 0.0255(8) Uani 1 1 d . . . H3 H 1.0096 0.3776 0.8116 0.031 Uiso 1 1 calc R . . P4 P 0.6784(3) 0.8255(7) 0.2890(3) 0.0461(11) Uani 1 1 d . . . H4 H 0.6795 0.7461 0.33 0.055 Uiso 1 1 calc R . . O17 O 0.4040(8) 1.1563(13) 0.3726(8) 0.041(3) Uani 1 1 d . . . H17 H 0.3984 1.1267 0.4146 0.062 Uiso 1 1 calc R . . N2 N 0.9979(13) 1.3699(18) 0.4546(9) 0.052(4) Uani 1 1 d . . . H2C H 1.0214 1.3178 0.4192 0.063 Uiso 1 1 calc R . . H2D H 0.9578 1.3002 0.4709 0.063 Uiso 1 1 calc R . . O15 O 0.7679(11) 0.783(3) 0.2578(11) 0.085(6) Uani 1 1 d . . . H15 H 0.7905 0.8665 0.2441 0.128 Uiso 1 1 calc R . . C3 C 0.9435(19) 1.501(2) 0.4217(12) 0.059(6) Uani 1 1 d . . . H3A H 0.8856 1.4663 0.3798 0.071 Uiso 1 1 calc R . . H3B H 0.9848 1.5731 0.4007 0.071 Uiso 1 1 calc R . . C4 C 0.9119(16) 0.579(3) 0.476(3) 0.111(15) Uani 1 1 d . . . H4A H 0.867 0.5081 0.4943 0.133 Uiso 1 1 calc R . . H4B H 0.8738 0.6757 0.4537 0.133 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 0.0213(3) 0.0261(3) 0.0227(3) -0.00046(19) 0.0058(2) -0.00067(19) U2 0.0231(3) 0.0248(3) 0.0224(3) 0.00182(19) 0.0066(2) 0.00054(19) P1 0.0241(18) 0.0245(16) 0.0212(18) -0.0018(13) 0.0073(15) -0.0004(14) P2 0.0219(17) 0.0260(17) 0.0239(18) -0.0011(14) 0.0071(14) 0.0001(14) O5 0.026(5) 0.033(5) 0.025(5) 0.005(4) 0.002(4) -0.003(4) O9 0.032(6) 0.029(5) 0.027(5) 0.006(4) 0.011(4) 0.007(4) O1 0.033(6) 0.023(5) 0.035(6) -0.002(4) 0.001(5) -0.007(4) O6 0.042(6) 0.025(5) 0.027(5) -0.006(4) 0.004(5) -0.009(5) O2 0.026(5) 0.043(6) 0.033(6) 0.004(5) 0.004(5) -0.003(5) O12 0.022(5) 0.047(6) 0.037(6) 0.003(5) 0.008(5) 0.001(5) O3 0.026(5) 0.031(5) 0.023(5) 0.003(4) 0.004(4) 0.008(4) O4 0.031(6) 0.068(8) 0.034(6) -0.020(6) 0.010(5) -0.003(6) N1 0.029(6) 0.025(6) 0.032(7) 0.002(5) 0.009(5) 0.002(5) C1 0.025(7) 0.043(9) 0.034(9) -0.009(7) 0.008(6) -0.011(7) C2 0.024(7) 0.025(7) 0.026(7) 0.000(5) 0.007(6) 0.006(6) O7 0.028(5) 0.034(5) 0.026(5) -0.004(4) 0.005(4) -0.006(4) O8 0.028(5) 0.029(5) 0.030(5) 0.005(4) 0.014(4) 0.001(4) O13 0.034(6) 0.027(5) 0.032(6) -0.004(4) 0.013(5) -0.002(4) O11 0.030(5) 0.028(5) 0.021(5) 0.006(4) 0.004(4) 0.002(4) O10 0.025(5) 0.062(8) 0.037(6) 0.024(6) 0.013(5) 0.011(5) O14 0.032(5) 0.031(5) 0.034(6) -0.008(5) 0.013(5) -0.002(5) P3 0.0251(18) 0.0238(17) 0.0262(19) 0.0024(14) 0.0052(15) 0.0008(14) P4 0.028(2) 0.066(3) 0.043(3) -0.023(2) 0.0083(19) -0.003(2) O17 0.023(5) 0.030(6) 0.067(8) -0.011(6) 0.009(5) 0.007(5) N2 0.078(11) 0.040(8) 0.059(10) -0.020(8) 0.052(9) -0.024(8) O15 0.039(8) 0.142(16) 0.077(12) -0.067(12) 0.021(8) -0.008(9) C3 0.083(15) 0.033(10) 0.055(12) 0.003(9) 0.010(11) -0.022(11) C4 0.028(11) 0.034(11) 0.27(5) 0.041(18) 0.042(18) 0.001(9) #----------------------------------------------------------------------------# # 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 1.772(10) . ? U1 O2 1.777(11) . ? U1 O3 2.324(9) . ? U1 O12 2.361(10) 3_776 ? U1 O5 2.413(10) . ? U1 O4 2.420(11) . ? U1 O14 2.435(10) . ? U2 O6 1.775(10) . ? U2 O7 1.781(10) . ? U2 O13 2.324(10) 2_646 ? U2 O9 2.331(10) . ? U2 O8 2.416(10) . ? U2 O10 2.417(10) . ? U2 O11 2.447(9) . ? P1 O12 1.492(10) . ? P1 O9 1.519(10) . ? P1 O5 1.535(10) . ? P2 O13 1.495(10) . ? P2 O8 1.521(10) . ? P2 O3 1.527(10) . ? O12 U1 2.361(10) 3_776 ? O4 P4 1.486(13) . ? N1 C2 1.464(18) 3_676 ? N1 C1 1.546(19) . ? C1 C2 1.51(2) 1_565 ? C2 N1 1.464(18) 3_676 ? C2 C1 1.51(2) 1_545 ? O13 U2 2.324(10) 2_656 ? O11 P3 1.504(10) . ? O10 P4 1.502(12) 4_676 ? O14 P3 1.504(11) 4_575 ? P3 O14 1.504(11) 4_676 ? P3 O17 1.549(11) 4_676 ? P4 O10 1.502(12) 4_575 ? P4 O15 1.534(14) . ? O17 P3 1.549(10) 4_575 ? N2 C3 1.34(3) . ? N2 C4 1.54(4) 3_776 ? C3 C4 1.35(4) 1_565 ? C4 C3 1.35(4) 1_545 ? C4 N2 1.54(4) 3_776 ? 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 O2 176.1(5) . . ? O1 U1 O3 89.8(4) . . ? O2 U1 O3 91.9(4) . . ? O1 U1 O12 88.2(5) . 3_776 ? O2 U1 O12 92.6(4) . 3_776 ? O3 U1 O12 141.8(4) . 3_776 ? O1 U1 O5 101.5(4) . . ? O2 U1 O5 82.4(4) . . ? O3 U1 O5 72.1(3) . . ? O12 U1 O5 71.0(4) 3_776 . ? O1 U1 O4 89.4(5) . . ? O2 U1 O4 87.3(5) . . ? O3 U1 O4 146.5(4) . . ? O12 U1 O4 71.7(4) 3_776 . ? O5 U1 O4 140.6(3) . . ? O1 U1 O14 91.7(4) . . ? O2 U1 O14 85.4(4) . . ? O3 U1 O14 73.0(3) . . ? O12 U1 O14 145.3(4) 3_776 . ? O5 U1 O14 142.4(3) . . ? O4 U1 O14 73.6(4) . . ? O6 U2 O7 176.8(5) . . ? O6 U2 O13 91.4(4) . 2_646 ? O7 U2 O13 91.3(4) . 2_646 ? O6 U2 O9 87.9(4) . . ? O7 U2 O9 90.6(4) . . ? O13 U2 O9 149.5(4) 2_646 . ? O6 U2 O8 95.2(4) . . ? O7 U2 O8 87.2(4) . . ? O13 U2 O8 74.1(3) 2_646 . ? O9 U2 O8 75.6(3) . . ? O6 U2 O10 88.0(5) . . ? O7 U2 O10 88.8(5) . . ? O13 U2 O10 141.0(4) 2_646 . ? O9 U2 O10 69.5(3) . . ? O8 U2 O10 144.8(3) . . ? O6 U2 O11 93.4(4) . . ? O7 U2 O11 85.9(4) . . ? O13 U2 O11 70.4(3) 2_646 . ? O9 U2 O11 140.1(3) . . ? O8 U2 O11 143.6(3) . . ? O10 U2 O11 70.7(3) . . ? O12 P1 O9 113.2(6) . . ? O12 P1 O5 113.5(6) . . ? O9 P1 O5 109.7(6) . . ? O13 P2 O8 113.5(5) . . ? O13 P2 O3 109.7(6) . . ? O8 P2 O3 111.0(6) . . ? P1 O5 U1 129.9(6) . . ? P1 O9 U2 140.7(6) . . ? P1 O12 U1 171.9(7) . 3_776 ? P2 O3 U1 139.2(6) . . ? P4 O4 U1 133.8(8) . . ? C2 N1 C1 109.3(11) 3_676 . ? C2 C1 N1 111.1(12) 1_565 . ? N1 C2 C1 113.0(12) 3_676 1_545 ? P2 O8 U2 134.9(6) . . ? P2 O13 U2 154.3(6) . 2_656 ? P3 O11 U2 135.8(6) . . ? P4 O10 U2 134.3(7) 4_676 . ? P3 O14 U1 133.0(6) 4_575 . ? O14 P3 O11 114.8(6) 4_676 . ? O14 P3 O17 104.8(6) 4_676 4_676 ? O11 P3 O17 112.2(6) . 4_676 ? O4 P4 O10 114.9(7) . 4_575 ? O4 P4 O15 108.1(8) . . ? O10 P4 O15 113.8(8) 4_575 . ? C3 N2 C4 111.1(15) . 3_776 ? N2 C3 C4 108(2) . 1_565 ? C3 C4 N2 111.5(18) 1_545 3_776 ?