#------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_global #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2015-05-01 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ? #============================================================================== # # SUBMISSION DETAILS _publ_requested_journal 'Crystal Growth and Design' # Name and address of author for correspondence _publ_contact_author_name 'Forbes, Tori M' _publ_contact_author_address ; Department of Chemistry W372 Chemistry Building The University of Iowa Iowa City, IA 52242-1294 USA ; _publ_contact_author_email 'tori-forbes@uiowa.edu' _publ_contact_author_fax '1-319-335-1270' _publ_contact_author_phone '1-319-384-1908' _publ_section_abstract ; Porous hybrid materials such as metal organic nanotubes are of interest due to synthetic tunability, possibility for 1-D flow, and confinement of solvent molecules. In the current study, the stability and solvent selectivity of two porous metal organic nanotube (UIDA and UPDC) were analyszed using X-ray diffraction, gas chromatography/mass spec, thermogravimetricanalysis, and Infrared specroscopy. The fine details of the structural characterization, such as the presence of secondary solvent molecules were found to be important to the overall properties of the materials as evidenced by the increased stability of the UIDA compound when formed from solvent mixture containing acetone. Careful analysis of the UPDC compound indicated that the ligated solvent molecule can exchanged, which may impact the overall hydration state of the material. Overall, the UIDA compound displays complete selectivity to water, but the UPDC compound can also absorb amounts of THF, methanol, ethanol, and cyclohexane. The selectivity of the compounds may be related to the different gating mechanisms resulting from the flexibility of the overall crystalline lattice. ; #============================================================================== # # TITLE AND AUTHOR LIST _publ_section_title ;Structural features in metal organic nanotube crystals that influence stability and solvent uptake. ; _publ_section_title_footnote ; ? ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Jayasinghe, Ashini S.' ? ;Department of Chemistry W372 Chemistry Building The University of Iowa Iowa City, IA 52242-1294 USA ; 'Unruh, Daniel K.' ? ;Department of Chemistry W372 Chemistry Building The University of Iowa Iowa City, IA 52242-1294 USA ; 'Kral, Andrew' ? ;Department of Chemistry W372 Chemistry Building The University of Iowa Iowa City, IA 52242-1294 USA ; 'Libo, Anna' ? ;Department of Chemistry W372 Chemistry Building The University of Iowa Iowa City, IA 52242-1294 USA ; 'Forbes, Tori M' ? ;Department of Chemistry W372 Chemistry Building The University of Iowa Iowa City, IA 52242-1294 USA ; #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_p-1_a _audit_creation_date 2015-05-01T12:34:51-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_formula_sum 'C10 H25 N3 O14 U' _chemical_formula_weight 649.36 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.5215(10) _cell_length_b 12.771(2) _cell_length_c 13.063(2) _cell_angle_alpha 110.962(5) _cell_angle_beta 90.309(5) _cell_angle_gamma 98.608(5) _cell_volume 1002.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Blades _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 2.151 _exptl_crystal_F_000 620 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 8.168 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_absorpt_correction_T_min 0.4636 _exptl_absorpt_correction_T_max 0.7461 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'sealed tube' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_number 7944 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.673 _diffrn_reflns_theta_max 22.633 _diffrn_reflns_theta_full 22.633 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _reflns_number_total 2639 _reflns_number_gt 2212 _reflns_threshold_expression 'I > 2\s(I)' #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'APEX2 (Bruker AXS, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'CrystalMaker v2.5.0' _computing_publication_material 'Bruker SHELXTL' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_hydrogens mixed #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0476P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 2639 _refine_ls_number_parameters 277 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0757 _refine_ls_wR_factor_gt 0.071 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 0.924 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.237 _refine_diff_density_min -1.892 _refine_diff_density_rms 0.161 #----------------------------------------------------------------------------# # 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' 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_calc_flag _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.05911(5) 0.43329(3) 0.21893(3) 0.01787(14) Uani 1 d . . O1 O -0.0386(9) 0.4204(5) 0.3395(5) 0.0225(15) Uani 1 d . . O2 O 0.3746(8) 0.5267(5) 0.3090(5) 0.0195(14) Uani 1 d . . O3 O 0.7543(9) 0.7184(5) 0.8091(5) 0.0247(15) Uani 1 d . . O4 O 0.0428(9) 0.6303(5) 0.2811(5) 0.0239(15) Uani 1 d . . O5 O -0.1960(9) 0.2785(5) 0.1135(5) 0.0256(15) Uani 1 d . . O6 O -0.0974(9) 0.7824(5) 0.2976(5) 0.0296(17) Uani 1 d . . O7 O -0.4083(9) 0.1982(5) -0.0371(5) 0.0248(15) Uani 1 d . . O8 O 0.6615(10) 0.6197(6) 0.4114(5) 0.0355(18) Uani 1 d . . O9 O 0.6294(9) 0.8638(5) 0.7875(5) 0.0269(16) Uani 1 d . . O10 O 0.1471(9) 0.4429(5) 0.0945(5) 0.0242(15) Uani 1 d . . O11 O 0.1756(10) 0.8900(5) 0.6711(5) 0.0300(16) Uani 1 d . . O12 O -0.4056(10) 0.8846(5) 0.2543(5) 0.0300(16) Uani 1 d . . O13 O 0.7204(10) 1.0881(5) 0.5903(6) 0.0364(18) Uani 1 d . . O14 O 0.8129(10) 0.8750(5) 0.5361(5) 0.0323(17) Uani 1 d . . N1 N -0.2770(11) 0.4836(5) 0.1615(6) 0.0186(17) Uani 1 d . . H1 H -0.3794 0.4755 0.216 0.022 Uiso 1 calc . . N2 N 0.4655(11) 0.7451(6) 0.5837(6) 0.0214(18) Uani 1 d . . H2A H 0.5728 0.7876 0.5649 0.026 Uiso 1 calc . . H2B H 0.3862 0.7935 0.628 0.026 Uiso 1 calc . . N3 N 0.8284(11) 1.0348(6) 0.9633(6) 0.0237(19) Uani 1 d . . H3A H 0.7705 0.9686 0.9095 0.028 Uiso 1 calc . . H3B H 0.7479 1.0882 0.9665 0.028 Uiso 1 calc . . C1 C -0.3232(13) 0.2832(7) 0.0418(8) 0.022(2) Uani 1 d . . C2 C 0.4740(14) 0.6030(7) 0.3968(7) 0.019(2) Uani 1 d . . C3 C 0.6533(13) 0.7624(8) 0.7556(7) 0.020(2) Uani 1 d . . C4 C -0.0954(14) 0.6776(8) 0.2547(7) 0.022(2) Uani 1 d . . C5 C -0.3656(13) 0.3995(7) 0.0528(7) 0.019(2) Uani 1 d . . H5A H -0.3019 0.4214 -0.0067 0.023 Uiso 1 calc . . H5B H -0.5173 0.3984 0.0464 0.023 Uiso 1 calc . . C6 C 0.3364(12) 0.6690(7) 0.4814(7) 0.020(2) Uani 1 d . . H6A H 0.2643 0.7153 0.4509 0.024 Uiso 1 calc . . H6B H 0.2299 0.6155 0.4994 0.024 Uiso 1 calc . . C7 C -0.2593(13) 0.6022(7) 0.1673(8) 0.022(2) Uani 1 d . . H7A H -0.3946 0.6286 0.1844 0.027 Uiso 1 calc . . H7B H -0.2223 0.6064 0.0954 0.027 Uiso 1 calc . . C8 C 0.8288(13) 1.0178(7) 1.0705(8) 0.025(2) Uani 1 d . . H8A H 0.6853 0.9919 1.0855 0.03 Uiso 1 calc . . H8B H 0.8835 1.0904 1.1305 0.03 Uiso 1 calc . . C9 C 1.0353(13) 1.0707(7) 0.9347(8) 0.025(2) Uani 1 d . . H9A H 1.0969 1.145 0.9904 0.03 Uiso 1 calc . . H9B H 1.027 1.0796 0.8626 0.03 Uiso 1 calc . . C10 C 0.5491(14) 0.6838(7) 0.6449(7) 0.022(2) Uani 1 d . . H10A H 0.6515 0.6395 0.6009 0.026 Uiso 1 calc . . H10B H 0.435 0.6294 0.6564 0.026 Uiso 1 calc . . H11A H 0.080(11) 0.895(7) 0.618(6) 0.05 Uiso 1 d . . H11B H 0.278(11) 0.957(5) 0.694(7) 0.05 Uiso 1 d . . H12A H -0.304(12) 0.846(7) 0.274(6) 0.05 Uiso 1 d . . H12B H -0.444(14) 0.845(7) 0.178(3) 0.05 Uiso 1 d . . H13A H 0.834(8) 1.148(6) 0.624(7) 0.05 Uiso 1 d . . H13B H 0.607(9) 1.100(7) 0.638(6) 0.05 Uiso 1 d . . H14A H 0.777(15) 0.949(4) 0.548(7) 0.05 Uiso 1 d . . H14B H 0.836(15) 0.842(7) 0.460(3) 0.05 Uiso 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 0.0141(2) 0.0178(2) 0.0179(2) 0.00286(14) 0.00028(13) 0.00048(13) O1 0.023(3) 0.026(3) 0.017(4) 0.008(3) -0.001(3) -0.001(3) O2 0.023(3) 0.018(3) 0.013(4) 0.000(3) -0.002(3) 0.003(3) O3 0.021(4) 0.030(4) 0.020(4) 0.004(3) -0.007(3) 0.006(3) O4 0.021(4) 0.020(3) 0.024(4) 0.001(3) -0.005(3) 0.001(3) O5 0.024(4) 0.024(3) 0.026(4) 0.004(3) -0.007(3) 0.006(3) O6 0.027(4) 0.014(4) 0.038(4) -0.003(3) -0.004(3) 0.002(3) O7 0.022(3) 0.019(3) 0.026(4) 0.001(3) -0.006(3) -0.002(3) O8 0.018(4) 0.049(4) 0.022(4) -0.005(3) 0.000(3) -0.004(3) O9 0.037(4) 0.015(4) 0.023(4) 0.000(3) -0.008(3) 0.002(3) O10 0.020(3) 0.030(4) 0.023(4) 0.009(3) 0.006(3) 0.005(3) O11 0.028(4) 0.029(4) 0.031(4) 0.008(3) 0.002(3) 0.005(3) O12 0.029(4) 0.030(4) 0.029(4) 0.007(3) 0.001(3) 0.009(3) O13 0.031(4) 0.026(4) 0.042(5) 0.003(3) 0.009(3) -0.002(3) O14 0.028(4) 0.025(4) 0.034(4) 0.002(3) 0.004(3) -0.002(3) N1 0.026(4) 0.012(4) 0.012(4) -0.001(3) -0.002(3) 0.002(3) N2 0.025(4) 0.019(4) 0.017(5) 0.001(3) -0.003(3) 0.007(3) N3 0.026(5) 0.017(4) 0.022(5) 0.000(3) -0.006(3) 0.003(3) C1 0.011(5) 0.024(5) 0.030(6) 0.011(5) 0.004(4) 0.001(4) C2 0.020(6) 0.023(5) 0.015(6) 0.009(4) 0.000(4) -0.002(4) C3 0.012(5) 0.027(6) 0.019(6) 0.006(5) 0.005(4) 0.001(4) C4 0.021(5) 0.035(6) 0.016(6) 0.016(5) 0.012(4) 0.003(4) C5 0.019(5) 0.018(5) 0.019(6) 0.004(4) -0.002(4) 0.006(4) C6 0.010(5) 0.026(5) 0.019(6) 0.001(4) 0.001(4) 0.001(4) C7 0.022(5) 0.018(5) 0.027(6) 0.010(4) -0.001(4) 0.000(4) C8 0.017(5) 0.024(5) 0.027(6) 0.001(4) 0.003(4) 0.001(4) C9 0.027(5) 0.027(5) 0.018(6) 0.008(4) 0.004(4) -0.002(4) C10 0.028(5) 0.021(5) 0.012(5) -0.001(4) 0.000(4) 0.009(4) #----------------------------------------------------------------------------# # 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 1.754(6) . ? U1 O10 1.765(6) . ? U1 O2 2.297(5) . ? U1 O3 2.361(6) 2_666 ? U1 O5 2.370(6) . ? U1 O4 2.371(6) . ? U1 N1 2.555(7) . ? O2 C2 1.299(10) . ? O3 C3 1.275(11) . ? O3 U1 2.360(6) 2_666 ? O4 C4 1.266(11) . ? O5 C1 1.271(10) . ? O6 C4 1.255(10) . ? O7 C1 1.250(10) . ? O8 C2 1.211(10) . ? O9 C3 1.245(10) . ? O11 H11A 0.96(2) . ? O11 H11B 0.96(2) . ? O12 H12A 0.97(2) . ? O12 H12B 0.96(2) . ? O13 H13A 0.96(2) . ? O13 H13B 0.96(2) . ? O14 H14A 0.96(2) . ? O14 H14B 0.96(2) . ? N1 C7 1.475(10) . ? N1 C5 1.489(10) . ? N1 H1 1 . ? N2 C10 1.456(11) . ? N2 C6 1.500(10) . ? N2 H2A 0.91 . ? N2 H2B 0.91 . ? N3 C9 1.454(11) . ? N3 C8 1.491(11) . ? N3 H3A 0.91 . ? N3 H3B 0.91 . ? C1 C5 1.509(12) . ? C2 C6 1.520(12) . ? C3 C10 1.519(12) . ? C4 C7 1.505(12) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 C9 1.521(12) 2_777 ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 C8 1.521(12) 2_777 ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? 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 O10 177.5(3) . . ? O1 U1 O2 91.5(2) . . ? O10 U1 O2 91.0(2) . . ? O1 U1 O3 91.8(2) . 2_666 ? O10 U1 O3 88.6(2) . 2_666 ? O2 U1 O3 78.20(19) . 2_666 ? O1 U1 O5 89.6(2) . . ? O10 U1 O5 88.1(2) . . ? O2 U1 O5 158.10(19) . . ? O3 U1 O5 79.91(19) 2_666 . ? O1 U1 O4 92.7(2) . . ? O10 U1 O4 88.1(2) . . ? O2 U1 O4 73.26(19) . . ? O3 U1 O4 151.2(2) 2_666 . ? O5 U1 O4 128.5(2) . . ? O1 U1 N1 93.5(3) . . ? O10 U1 N1 84.7(2) . . ? O2 U1 N1 138.0(2) . . ? O3 U1 N1 143.13(19) 2_666 . ? O5 U1 N1 63.7(2) . . ? O4 U1 N1 64.86(19) . . ? C2 O2 U1 147.4(5) . . ? C3 O3 U1 140.9(6) . 2_666 ? C4 O4 U1 127.4(5) . . ? C1 O5 U1 123.7(5) . . ? H11A O11 H11B 108(4) . . ? H12A O12 H12B 107(4) . . ? H13A O13 H13B 108(4) . . ? H14A O14 H14B 107(4) . . ? C7 N1 C5 112.8(7) . . ? C7 N1 U1 114.1(5) . . ? C5 N1 U1 111.0(5) . . ? C7 N1 H1 106.1 . . ? C5 N1 H1 106.1 . . ? U1 N1 H1 106.1 . . ? C10 N2 C6 113.6(7) . . ? C10 N2 H2A 108.8 . . ? C6 N2 H2A 108.8 . . ? C10 N2 H2B 108.8 . . ? C6 N2 H2B 108.8 . . ? H2A N2 H2B 107.7 . . ? C9 N3 C8 112.9(7) . . ? C9 N3 H3A 109 . . ? C8 N3 H3A 109 . . ? C9 N3 H3B 109 . . ? C8 N3 H3B 109 . . ? H3A N3 H3B 107.8 . . ? O7 C1 O5 123.7(8) . . ? O7 C1 C5 119.4(8) . . ? O5 C1 C5 116.8(7) . . ? O8 C2 O2 123.1(8) . . ? O8 C2 C6 122.2(8) . . ? O2 C2 C6 114.8(7) . . ? O9 C3 O3 125.4(8) . . ? O9 C3 C10 117.4(8) . . ? O3 C3 C10 117.2(8) . . ? O6 C4 O4 122.6(8) . . ? O6 C4 C7 120.5(9) . . ? O4 C4 C7 116.9(8) . . ? N1 C5 C1 109.4(7) . . ? N1 C5 H5A 109.8 . . ? C1 C5 H5A 109.8 . . ? N1 C5 H5B 109.8 . . ? C1 C5 H5B 109.8 . . ? H5A C5 H5B 108.2 . . ? N2 C6 C2 110.0(7) . . ? N2 C6 H6A 109.7 . . ? C2 C6 H6A 109.7 . . ? N2 C6 H6B 109.7 . . ? C2 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? N1 C7 C4 110.1(7) . . ? N1 C7 H7A 109.6 . . ? C4 C7 H7A 109.6 . . ? N1 C7 H7B 109.6 . . ? C4 C7 H7B 109.6 . . ? H7A C7 H7B 108.2 . . ? N3 C8 C9 109.0(7) . 2_777 ? N3 C8 H8A 109.9 . . ? C9 C8 H8A 109.9 2_777 . ? N3 C8 H8B 109.9 . . ? C9 C8 H8B 109.9 2_777 . ? H8A C8 H8B 108.3 . . ? N3 C9 C8 109.3(7) . 2_777 ? N3 C9 H9A 109.8 . . ? C8 C9 H9A 109.8 2_777 . ? N3 C9 H9B 109.8 . . ? C8 C9 H9B 109.8 2_777 . ? H9A C9 H9B 108.3 . . ? N2 C10 C3 112.6(7) . . ? N2 C10 H10A 109.1 . . ? C3 C10 H10A 109.1 . . ? N2 C10 H10B 109.1 . . ? C3 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag U1 O5 C1 O7 155.6(6) . . . . ? U1 O5 C1 C5 -22.5(11) . . . . ? U1 O2 C2 O8 174.7(7) . . . . ? U1 O2 C2 C6 -4.4(15) . . . . ? U1 O3 C3 O9 -153.8(7) 2_666 . . . ? U1 O3 C3 C10 27.8(13) 2_666 . . . ? U1 O4 C4 O6 175.3(6) . . . . ? U1 O4 C4 C7 -5.4(11) . . . . ? C7 N1 C5 C1 164.1(7) . . . . ? U1 N1 C5 C1 34.6(8) . . . . ? O7 C1 C5 N1 170.5(7) . . . . ? O5 C1 C5 N1 -11.3(11) . . . . ? C10 N2 C6 C2 -69.3(10) . . . . ? O8 C2 C6 N2 -5.3(12) . . . . ? O2 C2 C6 N2 173.8(7) . . . . ? C5 N1 C7 C4 -156.5(7) . . . . ? U1 N1 C7 C4 -28.6(9) . . . . ? O6 C4 C7 N1 -157.6(8) . . . . ? O4 C4 C7 N1 23.1(11) . . . . ? C9 N3 C8 C9 -58.3(9) . . . 2_777 ? C8 N3 C9 C8 58.5(10) . . . 2_777 ? C6 N2 C10 C3 -172.0(7) . . . . ? O9 C3 C10 N2 10.2(11) . . . . ? O3 C3 C10 N2 -171.3(8) . . . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # start Validation Reply Form _vrf_THETM01_I ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: Data collection process was interrupted before a complete data set could be obtained. This material is an intermediate product of a degradation process. Thus, it is not possible to resynthesize the compound. However, due to the weak diffraction of the crystal, even if data collection was continued to a higher theta value there would not have been useful peaks available. ; _vrf_PLAT023_I ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 22.63 Degree RESPONSE: Data collection process was interrupted before a complete data set could be obtained. This material is an intermediate product of a degradation process. Thus, it is not possible to resynthesize the compound. However, due to the weak diffraction of the crystal, even if data collection was continued to a higher theta value there would not have been useful peaks available. ; # end Validation Reply Form # END of CIF