Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name ; Dermot O'Hare ; 'Jong-Young Kim' 'Alexander J. Norquist' _publ_contact_author_name ; Prof Dermot O'Hare ; _publ_contact_author_address ; Inorganic Chemistry Lab University of Oxford South Parks Rd Oxford UNITED KINGDOM ; _publ_contact_author_email DERMOT.OHARE@CHEM.OX.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Incorporation of uranium(VI) into metal-organic framework solids, [UO2(C4H4O4)]?H2O, [UO2F(C5H6O4)]?2H2O, and [(UO2)1.5(C8H4O4)2]2[(CH3)2NCOH2]?H2O ; data_[UO2(C4H4O4)]H2O_(1) _database_code_CSD 210317 _audit_creation_date 03-02-04 _audit_creation_method CRYSTALS_ver_12-03-99 #============================================================= _cell_length_a 7.5720(5) _cell_angle_alpha 90 _cell_length_b 10.7786(8) _cell_angle_beta 90.773(5) _cell_length_c 9.5090(6) _cell_angle_gamma 90 _cell_volume 776.01(9) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'U ' -10.6730 9.6540 36.0228 0.5293 23.4128 3.3253 14.9491 16.0927 4.1880 100.6130 13.3966 International_Tables_Vol_IV_Table_2.2B 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 3 _chemical_formula_sum ' C5.33 H5.33 O9.33 U1.33 ' _chemical_formula_moiety '[UO2(C4H4O4)] H2O' _chemical_compound_source ; ? ; _chemical_formula_weight 536.13 _cell_measurement_reflns_used 1802 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description ' octahedral ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_max 0.08 _exptl_crystal_density_diffrn 3.442 _exptl_crystal_density_meas 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 704.000 _exptl_absorpt_coefficient_mu 20.915 # Sheldrick geometric definitions 0.43 0.43 _diffrn_measurement_device_type ; Enraf Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.43 _exptl_absorpt_correction_T_max 0.43 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 3481 _reflns_number_total 1768 _diffrn_reflns_av_R_equivalents 0.03 # Number of reflections with Friedels Law is 1768 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 1794 _diffrn_reflns_theta_min 5.130 _diffrn_reflns_theta_max 27.561 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.424 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _reflns_limit_h_min -9 _reflns_limit_h_max 9 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 12 _refine_diff_density_min -1.60 _refine_diff_density_max 3.87 _refine_ls_number_reflns 1201 _refine_ls_number_parameters 110 #_refine_ls_R_factor_ref 0.0389 _refine_ls_wR_factor_ref 0.0830 _refine_ls_goodness_of_fit_ref 0.8913 #_reflns_number_all 1768 _refine_ls_R_factor_all 0.0689 _refine_ls_wR_factor_all 0.0936 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 1201 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_gt 0.0830 _refine_ls_shift/su_max 0.000048 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method = Prince modified Chebychev polynomial, (Watkin, 1994) W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 4.14 4.10 2.01 -0.492E-01 0.113 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 COLLECT Software, Nonius BV 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type _atom_site_attached_hydrogens # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom U1 U 0.24200(6) 0.73790(4) 0.14527(5) 0.0136 1.0000 Uani . O2 O 0.2318(13) 0.7220(11) 0.402(1) 0.0299 1.0000 Uani . O3 O 0.4973(13) 0.6293(11) 0.2292(11) 0.0304 1.0000 Uani . O4 O 0.1169(14) 0.602(1) 0.1341(11) 0.0299 1.0000 Uani . O5 O 0.5843(13) 0.692(1) 0.4424(11) 0.0283 1.0000 Uani . C1 C 0.6032(18) 0.6236(13) 0.3339(14) 0.0198 1.0000 Uani . O7 O 0.5849(13) 0.3222(9) 0.053(1) 0.0241 1.0000 Uani . O1 O 0.3613(13) 0.875(1) 0.1526(11) 0.0282 1.0000 Uani . O6 O 0.5180(14) 0.342(1) 0.2758(12) 0.0314 1.0000 Uani . C2 C 0.753(2) 0.5361(13) 0.3272(15) 0.0204 1.0000 Uani . C4 C 0.6109(18) 0.3705(12) 0.1725(16) 0.0225 1.0000 Uani . C3 C 0.7604(19) 0.4618(12) 0.1919(16) 0.0190 1.0000 Uani . H1 H 0.8661 0.5850 0.3387 0.0251 1.0000 Uiso . H2 H 0.7447 0.4766 0.4085 0.0251 1.0000 Uiso . H4 H 0.8761 0.4149 0.1906 0.0229 1.0000 Uiso . H3 H 0.7586 0.5214 0.1109 0.0229 1.0000 Uiso . 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 0.0149(3) 0.0167(3) 0.0091(2) -0.0000(2) 0.00030(14) 0.0011(2) O2 0.023(5) 0.046(6) 0.020(5) 0.001(5) 0.001(4) 0.012(5) O3 0.022(6) 0.052(7) 0.017(5) -0.009(5) -0.004(4) 0.012(5) O4 0.027(6) 0.040(6) 0.022(5) 0.003(5) -0.006(4) -0.006(5) O5 0.020(5) 0.037(6) 0.027(6) -0.011(5) -0.008(4) 0.001(4) C1 0.014(7) 0.033(7) 0.013(6) -0.006(5) 0.006(5) -0.007(5) O7 0.024(5) 0.028(5) 0.021(5) -0.002(4) 0.002(4) -0.002(4) O1 0.018(5) 0.043(6) 0.023(5) -0.005(4) 0.001(4) 0.001(4) O6 0.024(6) 0.039(6) 0.032(6) -0.001(5) 0.005(5) -0.016(5) C2 0.017(7) 0.025(7) 0.019(8) -0.001(5) -0.006(6) 0.000(5) C4 0.019(7) 0.019(7) 0.030(8) 0.004(6) 0.000(6) 0.001(5) C3 0.014(7) 0.014(6) 0.029(8) -0.007(5) 0.008(6) -0.002(5) _refine_ls_extinction_coef 8.0(13) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag U1 . O2 . 2.451(9) yes U1 . O3 . 2.39(1) yes U1 . O4 . 1.747(11) yes U1 . O5 4_464 2.38(1) yes U1 . O7 2_665 2.40(1) yes U1 . O1 . 1.736(11) yes U1 . O6 3_555 2.39(1) yes O3 . C1 . 1.272(17) yes O5 . C1 . 1.277(16) yes C1 . C2 . 1.48(2) yes O7 . C4 . 1.264(17) yes O6 . C4 . 1.254(17) yes C2 . C3 . 1.518(18) yes C2 . H1 . 1.009 no C2 . H2 . 1.008 no C4 . C3 . 1.509(18) yes C3 . H4 . 1.011 no C3 . H3 . 1.003 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O2 . U1 . O3 . 70.7(3) yes O2 . U1 . O4 . 88.7(4) yes O3 . U1 . O4 . 92.6(5) yes O2 . U1 . O5 4_464 143.9(3) yes O3 . U1 . O5 4_464 145.3(4) yes O4 . U1 . O5 4_464 87.2(4) yes O2 . U1 . O7 2_665 142.1(3) yes O3 . U1 . O7 2_665 71.4(3) yes O4 . U1 . O7 2_665 91.6(4) yes O5 4_464 U1 . O7 2_665 73.9(4) yes O2 . U1 . O1 . 92.5(4) yes O3 . U1 . O1 . 89.2(4) yes O4 . U1 . O1 . 178.1(5) yes O5 4_464 U1 . O1 . 91.0(4) yes O7 2_665 U1 . O1 . 88.4(4) yes O2 . U1 . O6 3_555 71.5(3) yes O3 . U1 . O6 3_555 142.2(4) yes O4 . U1 . O6 3_555 88.0(5) yes O5 4_464 U1 . O6 3_555 72.5(4) yes O7 2_665 U1 . O6 3_555 146.4(3) yes O1 . U1 . O6 3_555 91.0(4) yes U1 . O3 . C1 . 141.7(9) yes U1 4_565 O5 . C1 . 141.1(9) yes O3 . C1 . O5 . 121.9(13) yes O3 . C1 . C2 . 118.3(12) yes O5 . C1 . C2 . 119.8(12) yes U1 2_665 O7 . C4 . 137.6(9) yes U1 3_545 O6 . C4 . 146.4(10) yes C1 . C2 . C3 . 114.2(11) yes C1 . C2 . H1 . 108.277 no C3 . C2 . H1 . 109.120 no C1 . C2 . H2 . 108.399 no C3 . C2 . H2 . 108.533 no H1 . C2 . H2 . 108.166 no O7 . C4 . O6 . 121.4(13) yes O7 . C4 . C3 . 119.1(13) yes O6 . C4 . C3 . 119.5(13) yes C2 . C3 . C4 . 114.3(11) yes C2 . C3 . H4 . 108.353 no C4 . C3 . H4 . 108.732 no C2 . C3 . H3 . 108.193 no C4 . C3 . H3 . 108.750 no H4 . C3 . H3 . 108.321 no #===END data_[UO2F(C5H6O4)]2H2O_(2) _database_code_CSD 210318 _audit_creation_date 2003-04-02T10:44:15-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C10 H14 F2 O14 U2' _chemical_formula_weight 872.27 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/m 1' 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' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 11.3572(4) _cell_length_b 18.1700(8) _cell_length_c 7.1855(3) _cell_angle_alpha 90 _cell_angle_beta 119.577(2) _cell_angle_gamma 90 _cell_volume 1289.58(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 4.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 25.212 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.084 _diffrn_reflns_av_unetI/netI 0.0624 _diffrn_reflns_number 5396 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 5.51 _diffrn_reflns_theta_max 27.72 _diffrn_reflns_theta_full 27.72 _diffrn_measured_fraction_theta_full 0.975 _diffrn_measured_fraction_theta_max 0.975 _reflns_number_total 1533 _reflns_number_gt 1382 _reflns_threshold_expression >2sigma(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^)+(0.0599P)^2^+28.4117P] 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 1533 _refine_ls_number_parameters 82 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0613 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1278 _refine_ls_wR_factor_gt 0.1228 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 5.01 _refine_diff_density_min -1.751 _refine_diff_density_rms 0.314 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 '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' F F 0.0171 0.0103 '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 0.11045(3) 0.5 0.0223(2) Uani 1 2 d S . . F1 F 0.1226(8) 0 0.6237(18) 0.032(2) Uani 1 2 d S . . O2 O 0.1358(7) 0.2256(4) 0.6311(15) 0.031(2) Uani 1 1 d . . . O1 O 0.0130(8) 0.1109(4) 0.2633(14) 0.0291(16) Uani 1 1 d . . . O3 O 0.2509(8) 0.1224(4) 0.7193(15) 0.0287(17) Uani 1 1 d . . . O4 O 0.4113(11) 0 0.727(2) 0.030(3) Uani 1 2 d S . . C1 C 0.2489(10) 0.1919(5) 0.732(2) 0.023(2) Uani 1 1 d . . . C2 C 0.3761(10) 0.2348(6) 0.869(2) 0.027(2) Uani 1 1 d . . . C3 C 0.5 0.1904(9) 1 0.043(5) Uani 1 2 d S . . H3A H 0.4839 0.1582 1.0965 0.052 Uiso 0.5 1 calc P . . H3B H 0.5161 0.1582 0.9035 0.052 Uiso 0.5 1 calc P . . O5 O 0.691(3) 0 0.852(9) 0.21(2) Uani 1 2 d S . . H2A H 0.360(12) 0.272(7) 0.77(2) 0.03(3) Uiso 1 1 d . . . H2B H 0.370(14) 0.260(7) 0.99(3) 0.04(4) 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 0.0118(3) 0.0162(3) 0.0346(3) 0 0.0081(2) 0 F1 0.014(4) 0.017(4) 0.050(7) 0 0.005(5) 0 O2 0.012(3) 0.018(3) 0.052(6) 0.000(3) 0.007(4) 0.004(3) O1 0.030(4) 0.030(4) 0.029(4) -0.004(4) 0.016(4) -0.001(3) O3 0.017(4) 0.016(3) 0.045(5) 0.002(3) 0.010(4) -0.001(3) O4 0.018(5) 0.031(5) 0.043(8) 0 0.016(6) 0 C1 0.009(4) 0.021(4) 0.034(6) 0.001(4) 0.006(5) 0.003(3) C2 0.017(5) 0.018(4) 0.037(7) -0.001(5) 0.006(5) -0.003(4) C3 0.021(8) 0.024(8) 0.070(15) 0 0.012(9) 0 O5 0.12(3) 0.14(3) 0.42(7) 0 0.18(4) 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 1.778(8) . ? U1 O1 1.778(8) 2_556 ? U1 F1 2.353(5) 5_556 ? U1 F1 2.353(5) . ? U1 O2 2.492(7) . ? U1 O2 2.492(7) 2_556 ? U1 O3 2.494(8) 2_556 ? U1 O3 2.494(8) . ? U1 C1 2.883(10) . ? U1 C1 2.883(10) 2_556 ? U1 U1 4.0138(10) 5_556 ? F1 U1 2.353(5) 5_556 ? O2 C1 1.278(12) . ? O3 C1 1.267(11) . ? C1 C2 1.502(14) . ? C2 C3 1.486(13) . ? C3 C2 1.486(13) 2_657 ? 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 179.5(5) . 2_556 ? O1 U1 F1 87.4(4) . 5_556 ? O1 U1 F1 93.0(4) 2_556 5_556 ? O1 U1 F1 93.0(4) . . ? O1 U1 F1 87.4(4) 2_556 . ? F1 U1 F1 62.9(4) 5_556 . ? O1 U1 O2 91.7(3) . . ? O1 U1 O2 87.9(3) 2_556 . ? F1 U1 O2 178.3(2) 5_556 . ? F1 U1 O2 115.6(2) . . ? O1 U1 O2 87.9(3) . 2_556 ? O1 U1 O2 91.7(3) 2_556 2_556 ? F1 U1 O2 115.6(2) 5_556 2_556 ? F1 U1 O2 178.3(2) . 2_556 ? O2 U1 O2 65.8(3) . 2_556 ? O1 U1 O3 90.2(3) . 2_556 ? O1 U1 O3 89.7(3) 2_556 2_556 ? F1 U1 O3 63.7(2) 5_556 2_556 ? F1 U1 O3 126.3(2) . 2_556 ? O2 U1 O3 117.8(2) . 2_556 ? O2 U1 O3 52.2(2) 2_556 2_556 ? O1 U1 O3 89.7(3) . . ? O1 U1 O3 90.2(3) 2_556 . ? F1 U1 O3 126.3(2) 5_556 . ? F1 U1 O3 63.7(2) . . ? O2 U1 O3 52.2(2) . . ? O2 U1 O3 117.8(2) 2_556 . ? O3 U1 O3 170.0(3) 2_556 . ? O1 U1 C1 91.8(4) . . ? O1 U1 C1 88.0(4) 2_556 . ? F1 U1 C1 152.3(3) 5_556 . ? F1 U1 C1 89.5(3) . . ? O2 U1 C1 26.2(2) . . ? O2 U1 C1 92.0(2) 2_556 . ? O3 U1 C1 144.0(2) 2_556 . ? O3 U1 C1 26.0(2) . . ? O1 U1 C1 88.0(4) . 2_556 ? O1 U1 C1 91.8(4) 2_556 2_556 ? F1 U1 C1 89.5(3) 5_556 2_556 ? F1 U1 C1 152.3(3) . 2_556 ? O2 U1 C1 92.0(2) . 2_556 ? O2 U1 C1 26.2(2) 2_556 2_556 ? O3 U1 C1 26.0(2) 2_556 2_556 ? O3 U1 C1 144.0(2) . 2_556 ? C1 U1 C1 118.2(4) . 2_556 ? O1 U1 U1 90.2(2) . 5_556 ? O1 U1 U1 90.2(2) 2_556 5_556 ? F1 U1 U1 31.46(18) 5_556 5_556 ? F1 U1 U1 31.46(18) . 5_556 ? O2 U1 U1 147.10(16) . 5_556 ? O2 U1 U1 147.10(16) 2_556 5_556 ? O3 U1 U1 94.99(15) 2_556 5_556 ? O3 U1 U1 94.99(15) . 5_556 ? C1 U1 U1 120.88(18) . 5_556 ? C1 U1 U1 120.88(18) 2_556 5_556 ? U1 F1 U1 117.1(4) 5_556 . ? C1 O2 U1 94.2(6) . . ? C1 O3 U1 94.4(6) . . ? O3 C1 O2 119.0(9) . . ? O3 C1 C2 121.2(9) . . ? O2 C1 C2 119.7(8) . . ? O3 C1 U1 59.6(5) . . ? O2 C1 U1 59.5(5) . . ? C2 C1 U1 175.2(8) . . ? C3 C2 C1 115.9(9) . . ? C2 C3 C2 114.3(13) 2_657 . ? #===END data_[(UO2)1.5(ISP)2]2[HDMF]H2O_(3) _database_code_CSD 210319 _audit_creation_date 03-02-04 _audit_creation_method CRYSTALS_ver_12-03-99 #============================================================= _cell_length_a 9.9344(2) _cell_angle_alpha 90 _cell_length_b 15.6519(3) _cell_angle_beta 104.4136(7) _cell_length_c 14.7961(3) _cell_angle_gamma 90 _cell_volume 2228.26(8) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 _chemical_absolute_configuration ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'U ' -9.6767 9.6646 36.0228 0.5293 23.4128 3.3253 14.9491 16.0927 4.1880 100.6130 13.3966 International_Tables_Vol_IV_Table_2.2B 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 8 _chemical_formula_sum ' C9 H5 N0.50 O6.50 U0.75 ' _chemical_formula_moiety [(UO2)1.5(ISP)2]2[HDMF]H2O _chemical_compound_source ; ? ; _chemical_formula_weight 402.66 _cell_measurement_reflns_used 5023 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description ' rod ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 2.400 _exptl_crystal_density_meas 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1468.000 _exptl_absorpt_coefficient_mu 10.969 # Sheldrick geometric definitions 0.42 0.42 _diffrn_measurement_device_type ; Enraf Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.42 _exptl_absorpt_correction_T_max 0.42 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 9840 _reflns_number_total 5039 _diffrn_reflns_av_R_equivalents 0.02 # Number of reflections with Friedels Law is 5039 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 5096 _diffrn_reflns_theta_min 5.181 _diffrn_reflns_theta_max 27.456 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.563 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _refine_diff_density_min -1.31 _refine_diff_density_max 1.25 _refine_ls_number_reflns 3941 _refine_ls_number_parameters 323 #_refine_ls_R_factor_ref 0.0234 _refine_ls_wR_factor_ref 0.0532 _refine_ls_goodness_of_fit_ref 0.9290 #_reflns_number_all 5039 _refine_ls_R_factor_all 0.0369 _refine_ls_wR_factor_all 0.0631 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 3941 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_gt 0.0532 _refine_ls_shift/su_max 0.001156 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method = Prince modified Chebychev polynomial, (Watkin, 1994) W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 20.5 32.8 21.9 10.2 3.96 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 COLLECT Software, Nonius BV 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type _atom_site_attached_hydrogens # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom U2 U 0.0000 0.0000 1.0000 0.0150 1.0000 Uani . O9 O 0.0545(4) 0.1073(3) 1.0017(3) 0.0255 1.0000 Uani . C8 C 0.2036(5) -0.0476(3) 0.9016(3) 0.0188 1.0000 Uani . O10 O 0.2335(4) -0.0451(3) 0.9898(2) 0.0250 1.0000 Uani . O11 O -0.0800(4) 0.0292(3) 1.1439(2) 0.0223 1.0000 Uani . C4 C 0.3126(5) -0.0705(3) 0.8528(3) 0.0177 1.0000 Uani . C3 C 0.2816(5) -0.0785(3) 0.7560(3) 0.0177 1.0000 Uani . C2 C 0.3875(5) -0.0970(4) 0.7124(3) 0.0186 1.0000 Uani . C1 C 0.3576(5) -0.1055(4) 0.6096(3) 0.0205 1.0000 Uani . O4 O 0.2328(4) -0.1023(3) 0.5603(3) 0.0263 1.0000 Uani . O3 O 0.4549(4) -0.1169(3) 0.5689(3) 0.0236 1.0000 Uani . C7 C 0.5232(5) -0.1070(4) 0.7656(4) 0.0258 1.0000 Uani . C5 C 0.4494(5) -0.0825(4) 0.9056(3) 0.0222 1.0000 Uani . U1 U 0.296869(17) -0.123472(12) 0.411933(12) 0.0117 1.0000 Uani . O1 O 0.2870(4) -0.0114(3) 0.3971(3) 0.0278 1.0000 Uani . O2 O 0.3043(4) -0.2359(2) 0.4223(3) 0.0250 1.0000 Uani . C16 C 0.5108(5) -0.1289(3) 0.3136(3) 0.0170 1.0000 Uani . O7 O 0.3835(3) -0.1297(3) 0.2688(2) 0.0198 1.0000 Uani . O8 O 0.5424(3) -0.1205(3) 0.4010(2) 0.0229 1.0000 Uani . C12 C 0.6209(5) -0.1416(3) 0.2622(3) 0.0166 1.0000 Uani . C11 C 0.7606(5) -0.1355(4) 0.3096(3) 0.0201 1.0000 Uani . C10 C -0.1366(5) -0.1501(4) 0.2619(4) 0.0201 1.0000 Uani . C9 C 0.0116(5) -0.1405(4) 0.3120(4) 0.0236 1.0000 Uani . O5 O 0.0459(4) -0.1307(4) 0.3993(3) 0.0408 1.0000 Uani . O6 O 0.1060(3) -0.1434(3) 0.2678(2) 0.0201 1.0000 Uani . C15 C -0.1740(5) -0.1727(3) 0.1678(4) 0.0201 1.0000 Uani . C14 C -0.3136(5) -0.1771(4) 0.1207(4) 0.0223 1.0000 Uani . C13 C 0.5847(5) -0.1601(4) 0.1674(4) 0.0212 1.0000 Uani . O12 O -0.1681(4) 0.0274(3) 0.8499(3) 0.0260 1.0000 Uani . C6 C 0.5548(6) -0.1006(4) 0.8628(4) 0.0278 1.0000 Uani . N1 N 0.2463(5) -0.3362(3) 1.0838(5) 0.0380 1.0000 Uani . C17 C 0.2065(7) -0.2469(5) 1.0654(5) 0.0488 1.0000 Uani . O13 O 0.4349(11) -0.4299(8) 1.0432(9) 0.0547 0.5000 Uani . C18 C 0.390(1) -0.3461(8) 1.0621(8) 0.0235 0.5000 Uani . H2 H 0.5995 -0.1194 0.7339 0.0308 1.0000 Uiso . H3 H 0.6521 -0.1103 0.9011 0.0344 1.0000 Uiso . H4 H 0.4710 -0.0772 0.9754 0.0263 1.0000 Uiso . H1 H 0.1845 -0.0712 0.7179 0.0215 1.0000 Uiso . H8 H -0.1002 -0.1858 0.1343 0.0245 1.0000 Uiso . H5 H 0.7870 -0.1214 0.3774 0.0236 1.0000 Uiso . H7 H -0.3405 -0.1931 0.0526 0.0280 1.0000 Uiso . H6 H 0.4846 -0.1603 0.1328 0.0249 1.0000 Uiso . O14 O 0.369(1) -0.3452(5) 1.2697(5) 0.0289 0.5000 Uani . H9 H -0.1398 0.0197 0.7902 0.0315 1.0000 Uiso . H12 H -0.2650 0.0457 0.8487 0.0315 1.0000 Uiso . C19 C 0.3287(17) -0.3320(11) 1.198(1) 0.0471 0.5000 Uani . 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 U2 0.01291(12) 0.02222(14) 0.01079(12) 0.0019(1) 0.00453(9) 0.0021(1) O9 0.027(2) 0.028(2) 0.0230(19) 0.0001(16) 0.0079(16) -0.0018(16) C8 0.018(2) 0.026(3) 0.016(2) 0.0019(19) 0.0102(19) 0.0027(19) O10 0.0192(18) 0.043(2) 0.0134(17) 0.0021(16) 0.0047(14) 0.0062(16) O11 0.0184(17) 0.037(2) 0.0122(16) 0.0015(15) 0.0058(13) 0.0035(15) C4 0.015(2) 0.026(3) 0.013(2) -0.0002(19) 0.0059(18) 0.0035(19) C3 0.013(2) 0.028(3) 0.013(2) -0.0019(19) 0.0036(17) -0.001(2) C2 0.012(2) 0.029(3) 0.015(2) -0.003(2) 0.0025(18) 0.0004(19) C1 0.016(2) 0.034(3) 0.012(2) -0.000(2) 0.0049(18) 0.002(2) O4 0.0145(17) 0.048(3) 0.0154(17) -0.0070(17) 0.0031(14) 0.0024(16) O3 0.0154(17) 0.040(2) 0.0163(17) -0.0058(16) 0.0047(13) 0.0028(16) C7 0.014(2) 0.046(4) 0.017(2) -0.004(2) 0.0037(19) 0.003(2) C5 0.019(2) 0.033(3) 0.015(2) -0.001(2) 0.0036(19) 0.002(2) U1 0.00666(9) 0.0182(1) 0.01058(9) -0.00004(7) 0.00291(6) 0.00059(7) O1 0.031(2) 0.0207(19) 0.032(2) 0.0020(16) 0.0086(17) 0.0057(16) O2 0.035(2) 0.0177(19) 0.0229(18) 0.0010(15) 0.0075(15) -0.0006(16) C16 0.010(2) 0.024(2) 0.018(2) 0.002(2) 0.0057(17) -0.0004(19) O7 0.0108(15) 0.034(2) 0.0164(16) 0.0004(16) 0.0062(13) 0.0007(15) O8 0.0087(15) 0.043(2) 0.0167(17) -0.0027(17) 0.0024(13) -0.0006(16) C12 0.010(2) 0.025(3) 0.016(2) -0.0036(19) 0.0062(18) -0.0022(18) C11 0.014(2) 0.032(3) 0.014(2) -0.005(2) 0.0029(18) 0.000(2) C10 0.009(2) 0.029(3) 0.021(2) -0.001(2) 0.0016(18) 0.0031(19) C9 0.009(2) 0.042(3) 0.021(2) 0.001(2) 0.0056(19) 0.001(2) O5 0.0122(17) 0.096(4) 0.0158(19) -0.010(2) 0.0066(14) -0.008(2) O6 0.0080(15) 0.039(2) 0.0149(16) 0.0023(15) 0.0063(13) 0.0002(14) C15 0.012(2) 0.028(3) 0.020(2) -0.000(2) 0.0044(19) 0.0017(19) C14 0.017(2) 0.033(3) 0.019(2) 0.000(2) 0.0070(19) -0.002(2) C13 0.014(2) 0.026(3) 0.022(3) -0.003(2) 0.0006(19) -0.0058(19) O12 0.0195(18) 0.044(2) 0.0154(17) 0.0018(16) 0.0066(14) 0.0066(17) C6 0.016(2) 0.046(4) 0.019(3) -0.006(2) 0.001(2) 0.008(2) N1 0.018(2) 0.024(3) 0.068(4) 0.008(3) 0.001(2) -0.005(2) C17 0.037(3) 0.026(3) 0.068(5) 0.008(4) -0.017(3) -0.006(3) O13 0.042(6) 0.058(7) 0.078(8) 0.009(6) 0.041(6) -0.006(5) C18 0.011(4) 0.035(6) 0.028(5) -0.007(5) 0.013(4) -0.005(4) O14 0.050(5) 0.025(4) 0.015(4) -0.000(3) 0.013(4) 0.012(4) C19 0.052(9) 0.054(9) 0.034(8) -0.001(7) 0.008(6) -0.014(7) _refine_ls_extinction_coef 24.3(34) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag U2 . O9 . 1.764(4) yes U2 . O9 2_557 1.764(4) yes U2 . O10 . 2.465(4) yes U2 . O10 2_557 2.465(4) yes U2 . O11 . 2.493(3) yes U2 . O11 2_557 2.493(3) yes U2 . O12 . 2.461(4) yes U2 . O12 2_557 2.461(4) yes C8 . O10 . 1.265(6) yes C8 . O11 2_557 1.277(6) yes C8 . C4 . 1.487(6) yes C4 . C3 . 1.394(7) yes C4 . C5 . 1.402(7) yes C3 . C2 . 1.394(7) yes C3 . H1 . 0.996 no C2 . C1 . 1.482(7) yes C2 . C7 . 1.391(7) yes C1 . O4 . 1.273(6) yes C1 . O3 . 1.272(6) yes O4 . U1 . 2.455(4) yes O3 . U1 . 2.461(4) yes C7 . C6 . 1.396(7) yes C7 . H2 . 1.005 no C5 . C6 . 1.381(7) yes C5 . H4 . 1.006 no U1 . O1 . 1.768(4) yes U1 . O2 . 1.767(4) yes U1 . O7 . 2.479(3) yes U1 . O8 . 2.485(3) yes U1 . O5 . 2.456(4) yes U1 . O6 . 2.495(3) yes C16 . O7 . 1.273(6) yes C16 . O8 . 1.259(6) yes C16 . C12 . 1.493(6) yes C12 . C11 . 1.394(7) yes C12 . C13 . 1.389(7) yes C11 . C10 1_655 1.398(7) yes C11 . H5 . 0.997 no C10 . C9 . 1.482(7) yes C10 . C15 . 1.394(7) yes C9 . O5 . 1.260(7) yes C9 . O6 . 1.271(6) yes C15 . C14 . 1.390(7) yes C15 . H8 . 1.003 no C14 . C13 1_455 1.385(7) yes C14 . H7 . 1.008 no C13 . H6 . 0.999 no O12 . H9 . 1.000 no O12 . H12 . 1.000 no C6 . H3 . 1.003 no N1 . C17 . 1.460(9) yes N1 . C18 . 1.546(11) yes N1 . C19 . 1.683(16) yes O13 . C18 . 1.436(16) yes O14 . C19 . 1.060(16) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O9 . U2 . O9 2_557 179.993 yes O9 . U2 . O10 . 89.04(16) yes O9 2_557 U2 . O10 . 90.96(16) yes O9 . U2 . O10 2_557 90.96(16) yes O9 2_557 U2 . O10 2_557 89.04(16) yes O10 . U2 . O10 2_557 179.995 yes O9 . U2 . O11 . 88.60(16) yes O9 2_557 U2 . O11 . 91.40(16) yes O10 . U2 . O11 . 127.57(12) yes O10 2_557 U2 . O11 . 52.43(12) yes O9 . U2 . O11 2_557 91.40(16) yes O9 2_557 U2 . O11 2_557 88.60(16) yes O10 . U2 . O11 2_557 52.43(12) yes O10 2_557 U2 . O11 2_557 127.57(12) yes O11 . U2 . O11 2_557 179.995 yes O9 . U2 . O12 . 89.08(16) yes O9 2_557 U2 . O12 . 90.92(16) yes O10 . U2 . O12 . 115.62(12) yes O10 2_557 U2 . O12 . 64.38(12) yes O11 . U2 . O12 . 116.71(12) yes O9 . U2 . O12 2_557 90.92(16) yes O9 2_557 U2 . O12 2_557 89.08(16) yes O10 . U2 . O12 2_557 64.38(12) yes O10 2_557 U2 . O12 2_557 115.62(12) yes O11 . U2 . O12 2_557 63.29(12) yes O11 2_557 U2 . O12 . 63.29(12) yes O11 2_557 U2 . O12 2_557 116.71(12) yes O12 . U2 . O12 2_557 179.995 yes O10 . C8 . O11 2_557 119.0(4) yes O10 . C8 . C4 . 119.7(4) yes O11 2_557 C8 . C4 . 121.3(4) yes U2 . O10 . C8 . 95.1(3) yes U2 . O11 . C8 2_557 93.5(3) yes C8 . C4 . C3 . 121.3(4) yes C8 . C4 . C5 . 119.0(4) yes C3 . C4 . C5 . 119.7(4) yes C4 . C3 . C2 . 119.7(4) yes C4 . C3 . H1 . 120.452 no C2 . C3 . H1 . 119.862 no C3 . C2 . C1 . 120.8(4) yes C3 . C2 . C7 . 119.9(5) yes C1 . C2 . C7 . 119.3(4) yes C2 . C1 . O4 . 120.2(4) yes C2 . C1 . O3 . 121.1(4) yes O4 . C1 . O3 . 118.7(4) yes C1 . O4 . U1 . 94.3(3) yes C1 . O3 . U1 . 94.1(3) yes C2 . C7 . C6 . 120.8(5) yes C2 . C7 . H2 . 119.650 no C6 . C7 . H2 . 119.510 no C4 . C5 . C6 . 120.9(5) yes C4 . C5 . H4 . 119.355 no C6 . C5 . H4 . 119.785 no O4 . U1 . O3 . 52.91(12) yes O4 . U1 . O1 . 87.60(17) yes O3 . U1 . O1 . 94.48(17) yes O4 . U1 . O2 . 94.09(16) yes O3 . U1 . O2 . 87.52(16) yes O1 . U1 . O2 . 177.91(18) yes O4 . U1 . O7 . 172.58(13) yes O3 . U1 . O7 . 122.17(11) yes O1 . U1 . O7 . 87.34(16) yes O2 . U1 . O7 . 91.10(15) yes O4 . U1 . O8 . 122.20(12) yes O3 . U1 . O8 . 69.81(11) yes O1 . U1 . O8 . 89.92(17) yes O2 . U1 . O8 . 90.23(16) yes O7 . U1 . O8 . 52.38(11) yes O4 . U1 . O5 . 65.82(13) yes O3 . U1 . O5 . 118.10(13) yes O1 . U1 . O5 . 90.69(19) yes O2 . U1 . O5 . 88.88(19) yes O7 . U1 . O5 . 119.67(12) yes O4 . U1 . O6 . 118.03(11) yes O3 . U1 . O6 . 169.23(12) yes O1 . U1 . O6 . 90.66(16) yes O2 . U1 . O6 . 87.46(15) yes O7 . U1 . O6 . 67.46(11) yes O8 . U1 . O5 . 171.98(12) yes O8 . U1 . O6 . 119.73(11) yes O5 . U1 . O6 . 52.27(12) yes O7 . C16 . O8 . 119.9(4) yes O7 . C16 . C12 . 119.4(4) yes O8 . C16 . C12 . 120.6(4) yes U1 . O7 . C16 . 93.8(3) yes U1 . O8 . C16 . 93.8(3) yes C16 . C12 . C11 . 119.9(4) yes C16 . C12 . C13 . 120.3(4) yes C11 . C12 . C13 . 119.8(4) yes C12 . C11 . C10 1_655 119.7(4) yes C12 . C11 . H5 . 120.068 no C10 1_655 C11 . H5 . 120.182 no C11 1_455 C10 . C9 . 119.4(5) yes C11 1_455 C10 . C15 . 120.0(4) yes C9 . C10 . C15 . 120.7(4) yes C10 . C9 . O5 . 120.4(4) yes C10 . C9 . O6 . 120.5(5) yes O5 . C9 . O6 . 119.1(5) yes U1 . O5 . C9 . 95.4(3) yes U1 . O6 . C9 . 93.3(3) yes C10 . C15 . C14 . 119.8(5) yes C10 . C15 . H8 . 119.960 no C14 . C15 . H8 . 120.201 no C15 . C14 . C13 1_455 120.1(5) yes C15 . C14 . H7 . 119.770 no C13 1_455 C14 . H7 . 120.132 no C12 . C13 . C14 1_655 120.4(5) yes C12 . C13 . H6 . 119.593 no C14 1_655 C13 . H6 . 119.969 no U2 . O12 . H9 . 119.981 no U2 . O12 . H12 . 119.974 no H9 . O12 . H12 . 120.043 no C7 . C6 . C5 . 119.0(5) yes C7 . C6 . H3 . 120.667 no C5 . C6 . H3 . 120.300 no C17 . N1 . C18 . 106.1(6) yes C17 . N1 . C19 . 101.0(7) yes C18 . N1 . C19 . 88.1(7) yes N1 . C18 . O13 . 118.7(8) yes N1 . C19 . O14 . 165.0(15) yes