Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name "Prof Dermot O'Hare" _publ_contact_author_address ; Chemistry Research Laboratory Oxford University Mansfield Road Oxford OX1 3TA ; _publ_contact_author_email DERMOT.OHARE@CHEM.OX.AC.UK _publ_section_title ; Structural variation in organically templated uranium sulfate-fluorides ; loop_ _publ_author_name "Dermot O'Hare" 'Ben E. Cockbain' 'Michael Doran' data_USFO-2 _database_code_depnum_ccdc_archive 'CCDC 263735' _audit_creation_date 04-16-12 _audit_creation_method CRYSTALS_ver_12-03-99 #============================================================= _cell_length_a 6.9105(2) _cell_angle_alpha 72.6594(14) _cell_length_b 9.6605(2) _cell_angle_beta 87.0683(13) _cell_length_c 10.1033(2) _cell_angle_gamma 77.9568(12) _cell_volume 629.62(3) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _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 '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 'S ' 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B 'F ' 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 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 '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 '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 _cell_formula_units_Z 2 _chemical_formula_sum ' C6 H16 F2 N2 O6 S1 U1 ' _chemical_formula_moiety ' C6 H16 F2 N2 O6 S1 U1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 520.29 _cell_measurement_reflns_used 2638 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_max 0.16 _exptl_crystal_density_diffrn 2.744 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 480.000 _exptl_absorpt_coefficient_mu 13.103 # Sheldrick geometric definitions 0.16 0.59 _diffrn_measurement_device_type ; 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 ; USER DEFINED STRUCTURE SOLUTION ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.16 _exptl_absorpt_correction_T_max 0.59 _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 5199 _reflns_number_total 2859 _diffrn_reflns_av_R_equivalents 0.02 # Number of reflections with Friedels Law is 2859 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 2890 _diffrn_reflns_theta_min 5.165 _diffrn_reflns_theta_max 27.491 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.941 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _reflns_limit_h_min -8 _reflns_limit_h_max 8 _reflns_limit_k_min -11 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 13 _refine_diff_density_min -1.59 _refine_diff_density_max 1.50 _refine_ls_number_reflns 2602 _refine_ls_number_parameters 164 #_refine_ls_R_factor_ref 0.0229 _refine_ls_wR_factor_ref 0.0567 _refine_ls_goodness_of_fit_ref 0.8970 #_reflns_number_all 2859 _refine_ls_R_factor_all 0.0262 _refine_ls_wR_factor_all 0.0599 # 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 2602 _refine_ls_R_factor_gt 0.0229 _refine_ls_wR_factor_gt 0.0567 _refine_ls_shift/su_max 0.001035 _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 11.7 17.9 10.4 4.48 1.49 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; User-defined structure solution reference 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 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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 H1 H 0.9800 1.4663 -0.6408 0.0177 1.0000 Uiso . H2 H 1.2713 1.2071 -0.6451 0.0168 1.0000 Uiso . H3 H 1.3161 1.3717 -0.6662 0.0168 1.0000 Uiso . H4 H 1.3943 1.2124 -0.4334 0.0174 1.0000 Uiso . H5 H 1.2253 1.3589 -0.4349 0.0174 1.0000 Uiso . H6 H 1.1444 1.0740 -0.4165 0.0151 1.0000 Uiso . H7 H 0.8644 1.3333 -0.4004 0.0181 1.0000 Uiso . H8 H 0.8109 1.1712 -0.3785 0.0181 1.0000 Uiso . H9 H 0.7331 1.3311 -0.6106 0.0201 1.0000 Uiso . H10 H 0.8952 1.1813 -0.6100 0.0201 1.0000 Uiso . H11 H 0.8531 1.4376 -0.8457 0.0189 1.0000 Uiso . H12 H 1.0328 1.2949 -0.8355 0.0189 1.0000 Uiso . H13 H 1.0816 1.4600 -0.8678 0.0189 1.0000 Uiso . H14 H 1.0480 1.0583 -0.1859 0.0159 1.0000 Uiso . H15 H 1.1170 1.2140 -0.2011 0.0159 1.0000 Uiso . H16 H 1.2811 1.0679 -0.2080 0.0159 1.0000 Uiso . N1 N 0.9937(7) 1.3924(5) -0.8157(4) 0.0153 1.0000 Uani . N2 N 1.1421(6) 1.1231(5) -0.2326(4) 0.0139 1.0000 Uani . C1 C 1.0146(8) 1.3699(5) -0.6629(5) 0.0141 1.0000 Uani . C2 C 1.2304(7) 1.3005(6) -0.6183(5) 0.0146 1.0000 Uani . C3 C 1.2551(7) 1.2647(6) -0.4612(5) 0.0142 1.0000 Uani . C4 C 1.1135(7) 1.1660(5) -0.3867(5) 0.0130 1.0000 Uani . C5 C 0.8993(7) 1.2398(6) -0.4275(5) 0.0163 1.0000 Uani . C6 C 0.8717(8) 1.2758(6) -0.5844(5) 0.0170 1.0000 Uani . F1 F 0.1045(4) 0.6680(3) 0.1233(3) 0.0186 1.0000 Uani . F2 F 0.6681(4) 0.5331(3) -0.0243(3) 0.0148 1.0000 Uani . O1 O 0.3190(5) 0.7640(4) -0.1355(4) 0.0159 1.0000 Uani . O2 O 0.5026(6) 0.6191(4) 0.2118(4) 0.0197 1.0000 Uani . O3 O 0.6625(5) 0.8281(4) -0.0141(4) 0.0138 1.0000 Uani . O4 O 0.7439(5) 1.0673(4) -0.0585(4) 0.0150 1.0000 Uani . O5 O 0.5525(5) 1.0197(4) -0.2281(4) 0.0170 1.0000 Uani . O6 O 0.8989(5) 0.9052(4) -0.1888(4) 0.0150 1.0000 Uani . U1 U 0.40361(2) 0.695837(19) 0.039901(18) 0.0096 1.0000 Uani . S1 S 0.71172(17) 0.95589(13) -0.12679(12) 0.0100 1.0000 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 N1 0.017(2) 0.016(2) 0.015(2) -0.0038(16) -0.0005(16) -0.0083(16) N2 0.0143(19) 0.017(2) 0.0086(19) -0.0003(16) 0.0020(15) -0.0052(16) C1 0.017(2) 0.012(2) 0.014(2) -0.0047(18) -0.0026(18) -0.0039(18) C2 0.015(2) 0.018(2) 0.010(2) 0.0009(18) 0.0003(17) -0.0078(19) C3 0.013(2) 0.017(2) 0.014(2) -0.0039(18) -0.0008(17) -0.0070(18) C4 0.015(2) 0.013(2) 0.010(2) -0.0018(17) 0.0007(17) -0.0021(17) C5 0.010(2) 0.025(3) 0.013(2) -0.004(2) -0.0014(17) -0.0025(19) C6 0.014(2) 0.022(2) 0.016(2) -0.0017(19) -0.0006(18) -0.0094(19) F1 0.0143(14) 0.0158(14) 0.0278(17) -0.0091(13) 0.0081(12) -0.0055(11) F2 0.0111(13) 0.0123(13) 0.0223(15) -0.0076(11) 0.0038(11) -0.0025(11) O1 0.0162(17) 0.0165(17) 0.0158(17) -0.0050(14) -0.0006(13) -0.0048(14) O2 0.0236(19) 0.0201(19) 0.0161(18) -0.0030(15) -0.0021(15) -0.0090(15) O3 0.0136(16) 0.0122(16) 0.0160(17) -0.0026(13) -0.0010(13) -0.0055(13) O4 0.0148(17) 0.0102(16) 0.0231(18) -0.0094(14) 0.0017(14) -0.0030(13) O5 0.0134(17) 0.0203(18) 0.0155(18) -0.0020(14) -0.0015(13) -0.0038(14) O6 0.0099(16) 0.0178(17) 0.0190(18) -0.0092(14) 0.0058(13) -0.0020(13) U1 0.00935(11) 0.0084(1) 0.01174(11) -0.00353(6) 0.00096(6) -0.00260(6) S1 0.0102(5) 0.0098(5) 0.0114(5) -0.0044(4) 0.0023(4) -0.0038(4) _refine_ls_extinction_coef 8.0(11) _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 H1 . C1 . 1.000 no H2 . C2 . 1.000 no H3 . C2 . 1.000 no H4 . C3 . 1.000 no H5 . C3 . 1.000 no H6 . C4 . 1.000 no H7 . C5 . 1.000 no H8 . C5 . 1.000 no H9 . C6 . 1.000 no H10 . C6 . 1.000 no H11 . N1 . 1.000 no H12 . N1 . 1.000 no H13 . N1 . 1.000 no H14 . N2 . 1.000 no H15 . N2 . 1.000 no H16 . N2 . 1.000 no N1 . C1 . 1.504(6) yes N2 . C4 . 1.499(6) yes C1 . C2 . 1.533(7) yes C1 . C6 . 1.515(7) yes C2 . C3 . 1.531(7) yes C3 . C4 . 1.522(7) yes C4 . C5 . 1.522(7) yes C5 . C6 . 1.531(7) yes F1 . U1 . 2.230(3) yes F2 . U1 . 2.349(3) yes F2 . U1 2_665 2.416(3) yes O1 . U1 . 1.779(4) yes O2 . U1 . 1.782(4) yes O3 . U1 . 2.360(3) yes O3 . S1 . 1.495(4) yes O4 . U1 2_675 2.361(3) yes O4 . S1 . 1.497(4) yes O5 . S1 . 1.447(4) yes O6 . S1 . 1.463(3) 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 H11 . N1 . H12 . 109.475 no H11 . N1 . H13 . 109.476 no H12 . N1 . H13 . 109.476 no H11 . N1 . C1 . 109.5 no H12 . N1 . C1 . 109.6 no H13 . N1 . C1 . 109.2 no H14 . N2 . H15 . 109.475 no H14 . N2 . H16 . 109.476 no H15 . N2 . H16 . 109.476 no H14 . N2 . C4 . 109.5 no H15 . N2 . C4 . 109.7 no H16 . N2 . C4 . 109.2 no H1 . C1 . N1 . 111.2 no H1 . C1 . C2 . 107.6 no N1 . C1 . C2 . 109.1(4) yes H1 . C1 . C6 . 107.0 no N1 . C1 . C6 . 109.3(4) yes C2 . C1 . C6 . 112.6(4) yes H2 . C2 . H3 . 109.467 no H2 . C2 . C1 . 109.2 no H3 . C2 . C1 . 109.1 no H2 . C2 . C3 . 109.1 no H3 . C2 . C3 . 109.2 no C1 . C2 . C3 . 110.8(4) yes H4 . C3 . H5 . 109.467 no H4 . C3 . C2 . 109.4 no H5 . C3 . C2 . 109.4 no H4 . C3 . C4 . 109.4 no H5 . C3 . C4 . 109.3 no C2 . C3 . C4 . 109.9(4) yes H6 . C4 . N2 . 108.4 no H6 . C4 . C3 . 107.6 no N2 . C4 . C3 . 110.9(4) yes H6 . C4 . C5 . 107.4 no N2 . C4 . C5 . 110.9(4) yes C3 . C4 . C5 . 111.5(4) yes H7 . C5 . H8 . 109.467 no H7 . C5 . C4 . 109.3 no H8 . C5 . C4 . 109.3 no H7 . C5 . C6 . 109.5 no H8 . C5 . C6 . 109.3 no C4 . C5 . C6 . 109.9(4) yes H9 . C6 . H10 . 109.467 no H9 . C6 . C1 . 109.0(3) no H10 . C6 . C1 . 109.1 no H9 . C6 . C5 . 108.9 no H10 . C6 . C5 . 109.2 no C1 . C6 . C5 . 111.1(4) yes U1 . F2 . U1 2_665 116.08(12) yes U1 . O3 . S1 . 137.8(2) yes U1 2_675 O4 . S1 . 140.8(2) yes F1 . U1 . F2 . 132.24(11) yes F1 . U1 . F2 2_665 69.1(1) yes F2 . U1 . F2 2_665 63.92(12) yes F1 . U1 . O1 . 93.52(15) yes F2 . U1 . O1 . 89.39(14) yes F2 2_665 U1 . O1 . 83.31(14) yes F1 . U1 . O2 . 89.29(16) yes F2 . U1 . O2 . 86.55(15) yes F2 2_665 U1 . O2 . 94.97(15) yes O1 . U1 . O2 . 175.94(17) yes F1 . U1 . O3 . 152.15(12) yes F2 . U1 . O3 . 75.21(11) yes F2 2_665 U1 . O3 . 138.72(11) yes O1 . U1 . O3 . 91.02(15) yes O2 . U1 . O3 . 87.85(15) yes F1 . U1 . O4 2_675 76.64(12) yes F2 . U1 . O4 2_675 151.05(11) yes F2 2_665 U1 . O4 2_675 143.43(11) yes O1 . U1 . O4 2_675 86.36(15) yes O2 . U1 . O4 2_675 97.15(16) yes O3 . U1 . O4 2_675 76.24(12) yes O3 . S1 . O4 . 106.6(2) yes O3 . S1 . O5 . 111.0(2) yes O4 . S1 . O5 . 110.5(2) yes O3 . S1 . O6 . 108.6(2) yes O4 . S1 . O6 . 107.7(2) yes O5 . S1 . O6 . 112.3(2) yes #===END data_USFO-3 _database_code_depnum_ccdc_archive 'CCDC 263736' _audit_creation_date 05-22-03 _audit_creation_method CRYSTALS_ver_12-03-99 #============================================================= _cell_length_a 6.9503(1) _cell_angle_alpha 90 _cell_length_b 17.2147(4) _cell_angle_beta 90 _cell_length_c 7.0867(1) _cell_angle_gamma 90 _cell_volume 847.90(3) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P m m n ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y,z x+1/2,-y,-z x,-y+1/2,z -x,y+1/2,-z -x+1/2,-y+1/2,z x+1/2,y+1/2,-z # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _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 'S ' 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 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 'F ' 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 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 '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 '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 _cell_formula_units_Z 2 _chemical_formula_sum ' C6 H14 F2 N2 O12 S2 U2 ' _chemical_formula_moiety ' C6 H14 F2 N2 O12 S2 U2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 884.37 _cell_measurement_reflns_used 1148 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_max 0.12 _exptl_crystal_density_diffrn 3.464 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 788.000 _exptl_absorpt_coefficient_mu 19.406 # Sheldrick geometric definitions 0.46 0.68 _diffrn_measurement_device_type ; 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 0.46 _exptl_absorpt_correction_T_max 0.68 _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 1936 _reflns_number_total 1120 _diffrn_reflns_av_R_equivalents 0.01 # Number of reflections with Friedels Law is 1120 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 969 _diffrn_reflns_theta_min 5.433 _diffrn_reflns_theta_max 27.450 _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 27.450 _diffrn_measured_fraction_theta_full 0.962 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _reflns_limit_h_min 0 _reflns_limit_h_max 9 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 9 _refine_diff_density_min -1.56 _refine_diff_density_max 1.36 _refine_ls_number_reflns 907 _refine_ls_number_parameters 74 #_refine_ls_R_factor_ref 0.0229 _refine_ls_wR_factor_ref 0.0547 _refine_ls_goodness_of_fit_ref 0.8449 #_reflns_number_all 1120 _refine_ls_R_factor_all 0.0335 _refine_ls_wR_factor_all 0.0658 # 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 907 _refine_ls_R_factor_gt 0.0229 _refine_ls_wR_factor_gt 0.0547 _refine_ls_shift/su_max 0.000136 _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 16.8 27.1 17.3 7.80 2.88 ; _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 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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 O1 O 0.7500 -0.1502(3) 0.1487(8) 0.0180 1.0000 Uani . O2 O 0.7500 -0.1197(3) -0.3433(8) 0.0160 1.0000 Uani . O3 O 0.7500 -0.0012(3) -0.0524(8) 0.0162 1.0000 Uani . O4 O 0.5832(7) 0.1054(2) 0.0818(8) 0.0396 1.0000 Uani . O5 O 0.7500 0.0181(4) 0.285(1) 0.0594 1.0000 Uani . U1 U 0.7500 -0.136950(12) -0.09753(3) 0.0078 1.0000 Uani . S1 S 0.7500 0.0560(1) 0.1039(2) 0.0119 1.0000 Uani . F1 F 0.5734(6) -0.2500 -0.1296(7) 0.0157 1.0000 Uani . C1 C 1.158(2) -0.1777(7) 0.361(2) 0.026(3) 0.5000 Uiso . C3 C 1.1317(17) -0.1789(6) 0.4354(18) 0.016(2) 0.5000 Uiso . C4 C 1.032(3) -0.2500 0.370(3) 0.023(4) 0.5000 Uiso . C2 C 1.056(3) -0.2500 0.435(4) 0.034(5) 0.5000 Uiso . N2 N 1.094(3) -0.0955(11) 0.377(3) 0.003(4) 0.2500 Uiso . N1 N 1.064(4) -0.1018(14) 0.415(4) 0.021(7) 0.2500 Uiso . H9 H 1.1904 -0.0600 0.4455 0.0112 0.2500 Uiso . H8 H 1.1171 -0.0886 0.2379 0.0112 0.2500 Uiso . H7 H 0.9631 -0.0793 0.4105 0.0112 0.2500 Uiso . H3 H 1.1434 -0.0573 0.3544 0.0159 0.2500 Uiso . H1 H 1.0601 -0.0954 0.5490 0.0159 0.2500 Uiso . H2 H 0.9326 -0.0992 0.3557 0.0159 0.2500 Uiso . H10 H 1.0898 -0.1871 0.5671 0.0167 0.5000 Uiso . H4 H 1.1550 -0.1811 0.2174 0.0340 0.5000 Uiso . H5 H 1.0486 -0.2500 0.5737 0.0381 0.5000 Uiso . H6 H 0.9215 -0.2500 0.3800 0.0381 0.5000 Uiso . H12 H 1.0138 -0.2500 0.2280 0.0257 0.5000 Uiso . H11 H 0.9010 -0.2500 0.4298 0.0257 0.5000 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 O1 0.036(3) 0.016(2) 0.002(2) -0.0015(19) 0.0000 0.0000 O2 0.022(3) 0.015(2) 0.011(2) -0.004(2) 0.0000 0.0000 O3 0.025(3) 0.010(2) 0.014(3) -0.005(2) 0.0000 0.0000 O4 0.017(2) 0.013(2) 0.088(4) -0.001(2) 0.018(2) 0.0073(17) O5 0.149(9) 0.018(3) 0.011(3) -0.005(2) 0.0000 0.0000 U1 0.00871(15) 0.00539(15) 0.00930(15) -0.00035(8) 0.0000 0.0000 S1 0.0140(8) 0.0070(7) 0.0147(8) -0.0035(6) 0.0000 0.0000 F1 0.0054(19) 0.0082(17) 0.033(2) 0.0000 -0.0006(17) 0.0000 _refine_ls_extinction_coef 12.035 _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 O1 . U1 . 1.760(5) yes O2 . U1 . 1.767(6) yes O3 . U1 . 2.358(5) yes O3 . S1 . 1.482(5) yes O4 . U1 2_655 2.381(4) yes O4 . S1 . 1.447(4) yes O5 . S1 . 1.436(7) yes U1 . F1 . 2.312(2) yes U1 . F1 3_655 2.312(2) yes C1 . C1 3_755 1.28(3) yes C1 . C3 . 0.560(14) yes C1 . C3 3_755 1.554(17) yes C1 . C4 . 1.523(17) yes C1 . C2 . 1.528(19) yes C1 . N2 . 1.49(2) yes C1 . N1 . 1.51(3) yes C1 . H4 . 1.018 no C3 . C3 3_755 1.64(2) yes C3 . C4 . 1.481(16) yes C3 . C2 . 1.334(15) yes C3 . N2 . 1.52(2) yes C3 . N1 . 1.41(3) yes C3 . H10 . 0.988 no C4 . C2 . 0.49(3) yes C4 . H6 . 0.774 no C4 . H12 . 1.012 no C4 . H11 . 1.007 no C2 . H5 . 0.983 no C2 . H6 . 1.012 no C2 . H11 . 1.076 no N2 . N1 . 0.35(3) yes N2 . H9 . 1.030 no N2 . H8 . 1.006 no N2 . H7 . 0.980 no N2 . H3 . 0.760 no N2 . H1 . 1.242 no N2 . H2 . 1.133 no N1 . H9 . 1.155 no N1 . H7 . 0.803 no N1 . H3 . 1.034 no N1 . H1 . 0.960 no N1 . H2 . 1.007 no H9 . H9 3_755 0.829 no H9 . H3 . 0.725 no H7 . H2 . 0.560 no H6 . H11 . 0.380 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 U1 . O3 . S1 . 139.5(3) yes U1 2_655 O4 . S1 . 155.3(3) yes O1 . U1 . O2 . 177.8(2) yes O1 . U1 . O3 . 89.6(2) yes O2 . U1 . O3 . 88.1(2) yes O1 . U1 . O4 2_655 89.03(15) yes O2 . U1 . O4 2_655 90.45(15) yes O3 . U1 . O4 2_655 76.6(1) yes O1 . U1 . O4 4_555 89.03(15) yes O2 . U1 . O4 4_555 90.45(15) yes O3 . U1 . O4 4_555 76.6(1) yes O4 2_655 U1 . O4 4_555 153.1(2) yes O1 . U1 . F1 . 89.35(19) yes O2 . U1 . F1 . 92.54(19) yes O3 . U1 . F1 . 147.91(9) yes O4 2_655 U1 . F1 . 71.35(14) yes O4 4_555 U1 . F1 . 135.48(13) yes O1 . U1 . F1 3_655 89.35(19) yes O2 . U1 . F1 3_655 92.54(19) yes O3 . U1 . F1 3_655 147.91(9) yes O4 2_655 U1 . F1 3_655 135.48(13) yes O4 4_555 U1 . F1 3_655 71.35(14) yes F1 . U1 . F1 3_655 64.14(18) yes O3 . S1 . O4 . 108.0(3) yes O3 . S1 . O4 3_655 108.0(3) yes O4 . S1 . O4 3_655 106.6(4) yes O3 . S1 . O5 . 111.4(3) yes O4 . S1 . O5 . 111.3(3) yes O4 3_655 S1 . O5 . 111.3(3) yes U1 . F1 . U1 5_545 114.63(17) yes C1 3_755 C1 . C3 . 109.1(21) yes C1 3_755 C1 . C3 3_755 19.9(6) yes C3 . C1 . C3 3_755 89.2(23) yes C1 3_755 C1 . C4 . 125.1(8) yes C3 . C1 . C4 . 75.1(20) yes C3 3_755 C1 . C4 . 121.0(12) yes C1 3_755 C1 . C2 . 117.8(10) yes C3 . C1 . C2 . 59.5(19) yes C3 3_755 C1 . C2 . 108.0(13) yes C4 . C1 . C2 . 18.6(10) yes C1 3_755 C1 . N2 . 107.5(9) yes C3 . C1 . N2 . 82.1(21) yes C3 3_755 C1 . N2 . 105.6(12) yes C4 . C1 . N2 . 127.0(14) yes C2 . C1 . N2 . 127.5(15) yes C1 3_755 C1 . N1 . 115.6(12) yes C3 . C1 . N1 . 69.6(21) yes C3 3_755 C1 . N1 . 109.4(14) yes C4 . C1 . N1 . 116.7(16) yes C2 . C1 . N1 . 114.7(16) yes C1 3_755 C1 . H4 . 91.230 no C3 . C1 . H4 . 158.958 no C3 3_755 C1 . H4 . 111.054 no C4 . C1 . H4 . 88.988 no C2 . C1 . H4 . 106.739 no N2 . C1 . N1 . 13.5(11) yes N2 . C1 . H4 . 97.174 no N1 . C1 . H4 . 106.979 no C1 . C3 . C1 3_755 51.0(19) yes C1 . C3 . C3 3_755 70.9(21) yes C1 3_755 C3 . C3 3_755 19.9(6) yes C1 . C3 . C4 . 83.4(21) yes C1 3_755 C3 . C4 . 110.0(11) yes C3 3_755 C3 . C4 . 117.8(8) yes C1 . C3 . C2 . 99.3(22) yes C1 3_755 C3 . C2 . 112.6(13) yes C3 3_755 C3 . C2 . 113.3(11) yes C4 . C3 . C2 . 19.2(11) yes C1 . C3 . N2 . 76.4(20) yes C1 3_755 C3 . N2 . 93.3(11) yes C3 3_755 C3 . N2 . 100.0(9) yes C4 . C3 . N2 . 128.0(13) yes C2 . C3 . N2 . 143.1(15) yes C1 . C3 . N1 . 88.6(22) yes C1 3_755 C3 . N1 . 105.3(14) yes C3 3_755 C3 . N1 . 109.3(13) yes C4 . C3 . N1 . 126.0(15) yes C2 . C3 . N1 . 136.9(18) yes C1 . C3 . H10 . 173.610 no C1 3_755 C3 . H10 . 126.944 no C3 3_755 C3 . H10 . 107.171 no C4 . C3 . H10 . 92.370 no C2 . C3 . H10 . 75.710 no N2 . C3 . N1 . 13.3(12) yes N2 . C3 . H10 . 109.994 no N1 . C3 . H10 . 97.764 no C1 . C4 . C1 5_545 109.7(16) yes C1 . C4 . C3 . 21.4(6) yes C1 5_545 C4 . C3 . 114.9(14) yes C1 . C4 . C3 5_545 114.9(14) yes C1 5_545 C4 . C3 5_545 21.4(6) yes C3 . C4 . C3 5_545 111.5(16) yes C1 . C4 . C2 . 81.3(25) yes C1 5_545 C4 . C2 . 81.3(25) yes C3 . C4 . C2 . 63.2(17) yes C3 5_545 C4 . C2 . 63.2(17) yes C1 . C4 . H6 . 125.150 no C1 5_545 C4 . H6 . 125.150 no C3 . C4 . H6 . 115.753 no C3 5_545 C4 . H6 . 115.753 no C2 . C4 . H6 . 103.889 no C1 . C4 . H12 . 91.822 no C1 5_545 C4 . H12 . 91.822 no C3 . C4 . H12 . 111.787 no C3 5_545 C4 . H12 . 111.787 no C2 . C4 . H12 . 167.927 no C1 . C4 . H11 . 122.543 no C1 5_545 C4 . H11 . 122.543 no C3 . C4 . H11 . 106.837 no C3 5_545 C4 . H11 . 106.837 no C2 . C4 . H11 . 84.322 no H6 . C4 . H12 . 88.184 no H6 . C4 . H11 . 19.567 no H12 . C4 . H11 . 107.751 no C1 . C2 . C1 5_545 109.1(18) yes C1 . C2 . C3 . 21.2(6) yes C1 5_545 C2 . C3 . 124.4(18) yes C1 . C2 . C3 5_545 124.4(18) yes C1 5_545 C2 . C3 5_545 21.2(6) yes C3 . C2 . C3 5_545 133.3(22) yes C1 . C2 . C4 . 80.1(25) yes C1 5_545 C2 . C4 . 80.1(25) yes C3 . C2 . C4 . 97.6(20) yes C3 5_545 C2 . C4 . 97.6(20) yes C1 . C2 . H5 . 111.609 no C1 5_545 C2 . H5 . 111.609 no C3 . C2 . H5 . 91.076 no C3 5_545 C2 . H5 . 91.076 no C4 . C2 . H5 . 157.741 no C1 . C2 . H6 . 107.241 no C1 5_545 C2 . H6 . 107.241 no C3 . C2 . H6 . 111.455 no C3 5_545 C2 . H6 . 111.455 no C4 . C2 . H6 . 47.933 no C1 . C2 . H11 . 116.951 no C1 5_545 C2 . H11 . 116.951 no C3 . C2 . H11 . 113.315 no C3 5_545 C2 . H11 . 113.315 no C4 . C2 . H11 . 68.613 no H5 . C2 . H6 . 109.807 no H5 . C2 . H11 . 89.127 no H6 . C2 . H11 . 20.680 no C1 . N2 . C3 . 21.5(6) yes C1 . N2 . N1 . 86.7(63) yes C3 . N2 . N1 . 66.8(61) yes C1 . N2 . H9 . 113.954 no C3 . N2 . H9 . 108.697 no N1 . N2 . H9 . 101.844 no C1 . N2 . H8 . 89.373 no C3 . N2 . H8 . 110.622 no N1 . N2 . H8 . 150.252 no H9 . N2 . H8 . 106.669 no C1 . N2 . H7 . 124.647 no C3 . N2 . H7 . 111.392 no N1 . N2 . H7 . 50.561 no H9 . N2 . H7 . 108.650 no H8 . N2 . H7 . 110.655 no C1 . N2 . H3 . 132.170 no C3 . N2 . H3 . 142.998 no N1 . N2 . H3 . 133.395 no H9 . N2 . H3 . 44.717 no H8 . N2 . H3 . 67.534 no C1 . N2 . H1 . 97.760 no C3 . N2 . H1 . 76.526 no N1 . N2 . H1 . 31.865 no H9 . N2 . H1 . 70.034 no H8 . N2 . H1 . 172.852 no C1 . N2 . H2 . 103.534 no C3 . N2 . H2 . 98.948 no N1 . N2 . H2 . 60.490 no H9 . N2 . H2 . 137.758 no H8 . N2 . H2 . 92.014 no H7 . N2 . H3 . 102.931 no H7 . N2 . H1 . 65.526 no H3 . N2 . H1 . 106.877 no H7 . N2 . H2 . 29.620 no H3 . N2 . H2 . 117.923 no H1 . N2 . H2 . 86.775 no C1 . N1 . C3 . 21.8(7) yes C1 . N1 . N2 . 79.8(62) yes C3 . N1 . N2 . 99.9(66) yes C1 . N1 . H9 . 105.067 no C3 . N1 . H9 . 108.263 no N2 . N1 . H9 . 60.765 no C1 . N1 . H7 . 141.903 no C3 . N1 . H7 . 138.231 no N2 . N1 . H7 . 109.613 no H9 . N1 . H7 . 111.710 no C1 . N1 . H3 . 107.917 no C3 . N1 . H3 . 124.167 no N2 . N1 . H3 . 32.256 no H9 . N1 . H3 . 38.185 no H7 . N1 . H3 . 95.356 no C1 . N1 . H1 . 111.336 no C3 . N1 . H1 . 90.830 no N2 . N1 . H1 . 136.950 no H9 . N1 . H1 . 76.246 no H7 . N1 . H1 . 87.263 no C1 . N1 . H2 . 109.089 no C3 . N1 . H2 . 112.719 no N2 . N1 . H2 . 101.758 no H9 . N1 . H2 . 137.789 no H7 . N1 . H2 . 33.709 no H3 . N1 . H1 . 109.850 no H3 . N1 . H2 . 106.238 no H1 . N1 . H2 . 112.198 no N2 . H9 . N1 . 17.391 no N2 . H9 . H9 3_755 130.643 no N1 . H9 . H9 3_755 139.330 no N2 . H9 . H3 . 47.482 no N1 . H9 . H3 . 61.849 no H9 3_755 H9 . H3 . 116.782 no N2 . H7 . N1 . 19.826 no N2 . H7 . H2 . 90.505 no N1 . H7 . H2 . 93.515 no N2 . H3 . N1 . 14.349 no N2 . H3 . H9 . 87.802 no N1 . H3 . H9 . 79.967 no N2 . H1 . N1 . 11.185 no N2 . H2 . N1 . 17.753 no N2 . H2 . H7 . 59.875 no N1 . H2 . H7 . 52.776 no C4 . H6 . C2 . 28.178 no C4 . H6 . H11 . 117.460 no C2 . H6 . H11 . 89.283 no C4 . H11 . C2 . 27.064 no C4 . H11 . H6 . 42.973 no C2 . H11 . H6 . 70.037 no #===END data_USFO-4 _database_code_depnum_ccdc_archive 'CCDC 263737' _audit_creation_date 05-24-03 _audit_creation_method CRYSTALS_ver_12-03-99 #============================================================= _cell_length_a 13.5775(3) _cell_angle_alpha 90 _cell_length_b 14.6180(4) _cell_angle_beta 90 _cell_length_c 8.1168(2) _cell_angle_gamma 90 _cell_volume 1610.99(7) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n m a ' 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 x,-y+1/2,z -x,y+1/2,-z -x+1/2,-y,z+1/2 x+1/2,y,-z+1/2 # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _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 'S ' 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 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 'F ' 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 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 '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 '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 _cell_formula_units_Z 4 _chemical_formula_sum ' C3 H12 F2 N2 O13 S2 U2 ' _chemical_formula_moiety ' C3 H12 F2 N2 O13 S2 U2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 862.32 _cell_measurement_reflns_used 6633 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 3.555 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1528.000 _exptl_absorpt_coefficient_mu 20.427 # Sheldrick geometric definitions 0.44 0.66 _diffrn_measurement_device_type ; 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 ; USER DEFINED STRUCTURE SOLUTION ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.44 _exptl_absorpt_correction_T_max 0.66 _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 13326 _reflns_number_total 1964 _diffrn_reflns_av_R_equivalents 0.03 # Number of reflections with Friedels Law is 1964 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 1845 _diffrn_reflns_theta_min 5.106 _diffrn_reflns_theta_max 27.481 _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 27.481 _diffrn_measured_fraction_theta_full 0.941 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _reflns_limit_h_min 0 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 10 _refine_diff_density_min -1.05 _refine_diff_density_max 1.12 _refine_ls_number_reflns 1123 _refine_ls_number_parameters 108 #_refine_ls_R_factor_ref 0.0206 _refine_ls_wR_factor_ref 0.0464 _refine_ls_goodness_of_fit_ref 0.9248 #_reflns_number_all 1964 _refine_ls_R_factor_all 0.0624 _refine_ls_wR_factor_all 0.0552 # 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 1123 _refine_ls_R_factor_gt 0.0206 _refine_ls_wR_factor_gt 0.0464 _refine_ls_shift/su_max 0.000829 _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 8.51 10.9 8.17 2.63 1.41 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; User-defined structure solution reference 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 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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 H1 H 0.4063 0.1644 0.5787 0.0233 0.5000 Uiso . H2 H 0.3315 0.2453 0.6385 0.0233 0.5000 Uiso . H3 H 0.4647 0.3433 0.6607 0.0273 0.5000 Uiso . H4 H 0.4790 0.1873 0.8679 0.0250 0.5000 Uiso . H5 H 0.5298 0.2861 0.9078 0.0250 0.5000 Uiso . H6 H 0.4100 0.2772 0.8993 0.0250 0.5000 Uiso . H7 H 0.4451 0.2495 0.3420 0.0217 0.5000 Uiso . H8 H 0.3269 0.2299 0.3518 0.0217 0.5000 Uiso . H9 H 0.3703 0.3303 0.4019 0.0217 0.5000 Uiso . H10 H 0.5903 0.1914 0.6163 0.0183 0.5000 Uiso . H11 H 0.5728 0.2724 0.4808 0.0183 0.5000 Uiso . H12 H 0.6242 0.2961 0.6577 0.0183 0.5000 Uiso . U1 U 0.304941(18) 0.512179(15) 0.12774(3) 0.0110 1.0000 Uani . S1 S 0.55373(15) 0.45267(13) 0.2480(2) 0.0137 1.0000 Uani . F1 F 0.2794(3) 0.4518(3) 0.3875(5) 0.0142 1.0000 Uani . O1 O 0.3002(5) 0.6267(3) 0.2007(7) 0.0176 1.0000 Uani . O2 O 0.3124(4) 0.3982(3) 0.0569(7) 0.0165 1.0000 Uani . O3 O 0.6307(4) 0.5086(4) 0.3249(7) 0.0199 1.0000 Uani . O4 O 0.5791(4) 0.4358(4) 0.0713(6) 0.0166 1.0000 Uani . O5 O 0.4613(4) 0.5072(5) 0.2536(7) 0.0261 1.0000 Uani . O6 O 0.5424(6) 0.3662(5) 0.3300(8) 0.0401 1.0000 Uani . O7 O 0.1882(7) 0.2500 0.3462(15) 0.0374 1.0000 Uani . N1 N 0.3829(8) 0.2631(11) 0.4057(13) 0.017(3) 0.5000 Uiso . N2 N 0.5745(7) 0.2582(16) 0.6013(12) 0.015(3) 0.5000 Uiso . C1 C 0.3940(11) 0.2325(11) 0.5798(17) 0.028(5) 0.5000 Uiso . C2 C 0.4763(9) 0.2772(9) 0.6722(16) 0.021(4) 0.5000 Uiso . C3 C 0.4741(9) 0.255(3) 0.8515(15) 0.024(4) 0.5000 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 0.00895(12) 0.01560(13) 0.00837(12) -0.0011(1) -0.00004(12) -0.0012(1) S1 0.0114(8) 0.0215(8) 0.0081(7) 0.0017(8) -0.0012(6) -0.0032(7) F1 0.011(2) 0.024(2) 0.0081(18) 0.0015(18) 0.0003(17) 0.0002(14) O1 0.020(3) 0.014(2) 0.019(3) -0.005(2) 0.004(3) -0.006(2) O2 0.021(3) 0.014(2) 0.014(2) -0.0065(19) -0.004(2) -0.001(2) O3 0.011(2) 0.030(3) 0.019(3) -0.008(2) -0.004(2) 0.000(2) O4 0.017(3) 0.027(3) 0.006(2) -0.005(2) 0.003(2) -0.007(2) O5 0.013(3) 0.049(4) 0.016(3) -0.011(3) -0.001(2) 0.010(2) O6 0.066(5) 0.034(4) 0.021(4) 0.016(3) -0.009(3) -0.017(3) O7 0.007(4) 0.041(5) 0.064(8) 0.0000 -0.008(5) 0.0000 _refine_ls_extinction_coef 8.410 _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 H1 . C1 . 1.008 no H2 . H2 5_555 0.137 no H2 . C1 . 0.991 no H2 . C1 5_555 1.026 no H3 . C2 . 0.983 no H4 . C3 . 1.002 no H4 . C3 5_555 0.854 no H5 . C3 . 0.993 no H5 . C3 5_555 1.070 no H6 . H6 5_555 0.795 no H6 . C3 . 1.006 no H6 . C3 5_555 1.063 no H7 . H7 5_555 0.015 no H7 . N1 . 1.011 no H7 . N1 5_555 1.008 no H8 . H8 5_555 0.587 no H8 . N1 . 1.002 no H8 . N1 5_555 0.883 no H9 . N1 . 0.998 no H10 . H12 5_555 0.598 no H10 . N2 . 1.006 no H10 . N2 5_555 0.777 no H11 . H11 5_555 0.655 no H11 . N2 . 1.000 no H11 . N2 5_555 1.075 no H12 . N2 . 0.986 no H12 . N2 5_555 1.138 no U1 . F1 . 2.312(4) yes U1 . F1 7_564 2.322(4) yes U1 . O1 . 1.778(5) yes U1 . O2 . 1.765(5) yes U1 . O3 8_455 2.397(5) yes U1 . O4 2_665 2.380(5) yes U1 . O5 . 2.358(5) yes S1 . O3 . 1.467(6) yes S1 . O4 . 1.495(5) yes S1 . O5 . 1.487(6) yes S1 . O6 . 1.437(6) yes N1 . N1 5_555 0.38(3) yes N1 . C1 . 1.490(13) yes N1 . C1 5_555 1.423(14) yes N2 . N2 5_555 0.24(5) yes N2 . C2 . 1.479(13) yes N2 . C2 5_555 1.542(16) yes C1 . C1 5_555 0.51(3) yes C1 . C2 . 1.496(15) yes C1 . C2 5_555 1.353(16) yes C2 . C2 5_555 0.80(3) yes C2 . C3 . 1.491(14) yes C2 . C3 5_555 1.53(2) yes C3 . C3 5_555 0.15(9) 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 H2 5_555 H2 . C1 . 100.933 no H2 5_555 H2 . C1 5_555 71.541 no C1 . H2 . C1 5_555 29.392 no C3 . H4 . C3 5_555 1.485 no C3 . H5 . C3 5_555 7.144 no H6 5_555 H6 . C3 . 71.286 no H6 5_555 H6 . C3 5_555 63.633 no C3 . H6 . C3 5_555 7.653 no H7 5_555 H7 . N1 . 78.645 no H7 5_555 H7 . N1 5_555 100.492 no N1 . H7 . N1 5_555 21.847 no H8 5_555 H8 . N1 . 61.070 no H8 5_555 H8 . N1 5_555 83.353 no N1 . H8 . N1 5_555 22.283 no H12 5_555 H10 . N2 . 86.411 no H12 5_555 H10 . N2 5_555 90.713 no N2 . H10 . N2 5_555 4.328 no H11 5_555 H11 . N2 . 77.991 no H11 5_555 H11 . N2 5_555 65.424 no N2 . H11 . N2 5_555 12.567 no H10 5_555 H12 . N2 . 51.957 no H10 5_555 H12 . N2 5_555 61.955 no N2 . H12 . N2 5_555 10.006 no F1 . U1 . F1 7_564 141.12(4) yes F1 . U1 . O1 . 92.9(2) yes F1 7_564 U1 . O1 . 92.8(2) yes F1 . U1 . O2 . 86.9(2) yes F1 7_564 U1 . O2 . 88.2(2) yes O1 . U1 . O2 . 178.7(3) yes F1 . U1 . O3 8_455 72.39(16) yes F1 7_564 U1 . O3 8_455 69.68(16) yes O1 . U1 . O3 8_455 86.1(2) yes O2 . U1 . O3 8_455 95.1(2) yes F1 . U1 . O4 2_665 147.15(17) yes F1 7_564 U1 . O4 2_665 71.56(17) yes O1 . U1 . O4 2_665 87.1(2) yes O2 . U1 . O4 2_665 92.4(2) yes O3 8_455 U1 . O4 2_665 140.20(19) yes F1 . U1 . O5 . 74.21(19) yes F1 7_564 U1 . O5 . 144.62(19) yes O1 . U1 . O5 . 85.3(3) yes O2 . U1 . O5 . 93.4(2) yes O3 8_455 U1 . O5 . 144.95(19) yes O4 2_665 U1 . O5 . 73.1(2) yes O3 . S1 . O4 . 109.6(3) yes O3 . S1 . O5 . 106.8(4) yes O4 . S1 . O5 . 108.2(4) yes O3 . S1 . O6 . 111.7(4) yes O4 . S1 . O6 . 108.9(4) yes O5 . S1 . O6 . 111.5(5) yes U1 . F1 . U1 7_565 138.90(19) yes U1 8_555 O3 . S1 . 141.6(3) yes U1 2_665 O4 . S1 . 138.7(3) yes U1 . O5 . S1 . 139.8(4) yes H7 . N1 . H7 5_555 0.864 no H7 . N1 . H8 . 108.450 no H7 5_555 N1 . H8 . 108.956 no H7 . N1 . H8 5_555 119.344 no H7 5_555 N1 . H8 5_555 119.321 no H8 . N1 . H8 5_555 35.577 no H7 . N1 . H9 . 108.716 no H7 5_555 N1 . H9 . 107.859 no H8 . N1 . H9 . 109.467 no H8 5_555 N1 . H9 . 73.952 no H7 . N1 . N1 5_555 78.645 no H7 5_555 N1 . N1 5_555 79.508 no H8 . N1 . N1 5_555 61.070 no H8 5_555 N1 . N1 5_555 96.647 no H9 . N1 . N1 5_555 170.004 no H7 . N1 . C1 . 109.954 no H7 5_555 N1 . C1 . 110.296 no H8 . N1 . C1 . 110.186 no H8 5_555 N1 . C1 . 126.250 no H9 . N1 . C1 . 110.032 no H7 . N1 . C1 5_555 115.364 no H7 5_555 N1 . C1 5_555 115.398 no H8 . N1 . C1 5_555 122.394 no H8 5_555 N1 . C1 5_555 125.280 no H9 . N1 . C1 5_555 90.220 no N1 5_555 N1 . C1 . 72.5(8) yes N1 5_555 N1 . C1 5_555 92.6(11) yes C1 . N1 . C1 5_555 20.1(13) yes H10 . N2 . H10 5_555 147.300 no H10 . N2 . H11 . 108.964 no H10 5_555 N2 . H11 . 87.845 no H10 . N2 . H11 5_555 73.225 no H10 5_555 N2 . H11 5_555 122.878 no H11 . N2 . H11 5_555 36.584 no H10 . N2 . H12 . 110.087 no H10 5_555 N2 . H12 . 37.330 no H11 . N2 . H12 . 110.651 no H11 5_555 N2 . H12 . 132.122 no H10 . N2 . H12 5_555 31.634 no H10 5_555 N2 . H12 5_555 115.772 no H11 . N2 . H12 5_555 123.518 no H11 5_555 N2 . H12 5_555 95.066 no H12 . N2 . H12 5_555 78.475 no H10 . N2 . N2 5_555 14.186 no H10 5_555 N2 . N2 5_555 161.486 no H11 . N2 . N2 5_555 102.009 no H11 5_555 N2 . N2 5_555 65.424 no H12 . N2 . N2 5_555 124.234 no H10 . N2 . C2 . 109.115 no H10 5_555 N2 . C2 . 90.544 no H11 . N2 . C2 . 108.710 no H11 5_555 N2 . C2 . 114.387 no H12 . N2 . C2 . 109.282 no H10 . N2 . C2 5_555 79.266 no H10 5_555 N2 . C2 5_555 119.899 no H11 . N2 . C2 5_555 114.522 no H11 5_555 N2 . C2 5_555 100.451 no H12 . N2 . C2 5_555 127.377 no H12 5_555 N2 . N2 5_555 45.760 no H12 5_555 N2 . C2 . 120.608 no N2 5_555 N2 . C2 . 100.8(10) yes H12 5_555 N2 . C2 5_555 97.372 no N2 5_555 N2 . C2 5_555 70.4(9) yes C2 . N2 . C2 5_555 30.5(10) yes H1 . C1 . H2 . 109.482 no H1 . C1 . H2 5_555 116.984 no H2 . C1 . H2 5_555 7.525 no H1 . C1 . N1 . 107.707 no H2 . C1 . N1 . 108.193 no H2 5_555 C1 . N1 . 105.163 no H1 . C1 . N1 5_555 93.065 no H2 . C1 . N1 5_555 112.209 no H2 5_555 C1 . N1 5_555 111.042 no N1 . C1 . N1 5_555 14.9(13) yes H1 . C1 . C1 5_555 170.438 no H2 . C1 . C1 5_555 79.067 no H2 5_555 C1 . C1 5_555 71.541 no N1 . C1 . C1 5_555 72.5(8) yes N1 5_555 C1 . C1 5_555 87.4(11) yes H1 . C1 . C2 . 108.177 no H2 . C1 . C2 . 108.410 no H2 5_555 C1 . C2 . 104.287 no N1 . C1 . C2 . 114.8(10) yes N1 5_555 C1 . C2 . 123.8(12) yes H1 . C1 . C2 5_555 76.414 no H2 . C1 . C2 5_555 117.436 no H2 5_555 C1 . C2 5_555 117.328 no N1 . C1 . C2 5_555 129.8(12) yes N1 5_555 C1 . C2 5_555 130.0(13) yes C1 5_555 C1 . C2 . 64.1(8) yes C1 5_555 C1 . C2 5_555 96.0(10) yes C2 . C1 . C2 5_555 31.9(11) yes H3 . C2 . N2 . 106.959 no H3 . C2 . N2 5_555 115.606 no N2 . C2 . N2 5_555 8.8(17) yes H3 . C2 . C1 . 105.239 no N2 . C2 . C1 . 113.3(10) yes N2 5_555 C2 . C1 . 108.2(12) yes H3 . C2 . C1 5_555 85.312 no N2 . C2 . C1 5_555 120.6(11) yes N2 5_555 C2 . C1 5_555 118.2(11) yes C1 . C2 . C1 5_555 19.9(14) yes H3 . C2 . C2 5_555 169.297 no N2 . C2 . C2 5_555 79.2(10) yes N2 5_555 C2 . C2 5_555 70.4(9) yes C1 . C2 . C2 5_555 64.1(8) yes C1 5_555 C2 . C2 5_555 84.0(10) yes H3 . C2 . C3 . 107.615 no N2 . C2 . C3 . 110.9(10) yes N2 5_555 C2 . C3 . 108.0(12) yes C1 . C2 . C3 . 112.3(12) yes C1 5_555 C2 . C3 . 120.1(12) yes H3 . C2 . C3 5_555 113.006 no N2 . C2 . C3 5_555 109.2(12) yes N2 5_555 C2 . C3 5_555 105.5(13) yes C1 . C2 . C3 5_555 109.1(15) yes C1 5_555 C2 . C3 5_555 118.6(14) yes C2 5_555 C2 . C3 . 77.5(17) yes C2 5_555 C2 . C3 5_555 72.0(17) yes C3 . C2 . C3 5_555 5.5(32) yes H4 . C3 . H4 5_555 161.491 no H4 . C3 . H5 . 109.917 no H4 5_555 C3 . H5 . 54.572 no H4 . C3 . H5 5_555 48.668 no H4 5_555 C3 . H5 5_555 115.747 no H5 . C3 . H5 5_555 61.477 no H4 . C3 . H6 . 108.823 no H4 5_555 C3 . H6 . 71.958 no H5 . C3 . H6 . 109.560 no H5 5_555 C3 . H6 . 128.880 no H4 . C3 . H6 5_555 64.267 no H4 5_555 C3 . H6 5_555 116.315 no H5 . C3 . H6 5_555 131.152 no H5 5_555 C3 . H6 5_555 99.925 no H6 . C3 . H6 5_555 45.081 no H4 . C3 . C2 . 110.035 no H4 5_555 C3 . C2 . 86.393 no H5 . C3 . C2 . 109.567 no H5 5_555 C3 . C2 . 121.663 no H6 . C3 . C2 . 108.917 no H4 . C3 . C2 5_555 79.608 no H4 5_555 C3 . C2 5_555 116.789 no H5 . C3 . C2 5_555 124.310 no H5 5_555 C3 . C2 5_555 102.613 no H6 . C3 . C2 5_555 118.859 no H4 . C3 . C3 5_555 8.512 no H4 5_555 C3 . C3 5_555 170.003 no H5 . C3 . C3 5_555 117.166 no H5 5_555 C3 . C3 5_555 55.689 no H6 . C3 . C3 5_555 108.714 no H6 5_555 C3 . C2 . 117.948 no H6 5_555 C3 . C2 5_555 103.045 no C2 . C3 . C2 5_555 30.5(10) yes H6 5_555 C3 . C3 5_555 63.633 no C2 . C3 . C3 5_555 102.5(17) yes C2 5_555 C3 . C3 5_555 72.0(17) yes #===END data_USFO-5 _database_code_depnum_ccdc_archive 'CCDC 263738' _audit_creation_date 05-14-03 _audit_creation_method CRYSTALS_ver_12-03-99 #============================================================= _cell_length_a 8.4354(2) _cell_angle_alpha 90 _cell_length_b 15.5581(4) _cell_angle_beta 96.666(1) _cell_length_c 14.8442(6) _cell_angle_gamma 90 _cell_volume 1935.0(1) _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 # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _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 '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 'S ' 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B 'F ' 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 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 '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 '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 _cell_formula_units_Z 4 _chemical_formula_sum ' C5 H17 F2 N2 O14 S2 U2 ' _chemical_formula_moiety ' C5 H17 F2 N2 O14 S2 U2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 907.38 _cell_measurement_reflns_used 4172 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 3.115 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1628.000 _exptl_absorpt_coefficient_mu 17.019 # Sheldrick geometric definitions 0.03 0.18 _diffrn_measurement_device_type ; 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 0.03 _exptl_absorpt_correction_T_max 0.18 _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 8054 _reflns_number_total 4368 _diffrn_reflns_av_R_equivalents 0.02 # Number of reflections with Friedels Law is 4368 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 4422 _diffrn_reflns_theta_min 5.215 _diffrn_reflns_theta_max 27.449 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.900 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _refine_diff_density_min -2.17 _refine_diff_density_max 3.35 _refine_ls_number_reflns 2915 _refine_ls_number_parameters 254 #_refine_ls_R_factor_ref 0.0351 _refine_ls_wR_factor_ref 0.0812 _refine_ls_goodness_of_fit_ref 0.8841 #_reflns_number_all 4368 _refine_ls_R_factor_all 0.0575 _refine_ls_wR_factor_all 0.0927 # 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 2915 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_gt 0.0812 _refine_ls_shift/su_max 0.000586 _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 23.8 36.1 21.8 8.18 2.59 ; _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 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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 H1 H -0.609 -0.3830 0.4743 0.0393 1.0000 Uiso . H2 H -0.402 -0.3832 0.5000 0.0393 1.0000 Uiso . H3 H -0.117 -0.1217 0.4964 0.0378 1.0000 Uiso . H4 H 0.084 -0.1118 0.4856 0.0378 1.0000 Uiso . H5 H 0.2292 0.0508 0.8449 0.0359 1.0000 Uiso . H6 H 0.3705 0.0834 0.7289 0.0363 1.0000 Uiso . H7 H 0.2247 0.0541 0.6531 0.0363 1.0000 Uiso . H8 H 0.4028 -0.0574 0.7815 0.0271 1.0000 Uiso . H9 H 0.4169 -0.0553 0.6728 0.0271 1.0000 Uiso . H10 H 0.1554 -0.1006 0.6428 0.0400 1.0000 Uiso . H11 H 0.2601 -0.1683 0.7095 0.0400 1.0000 Uiso . H12 H 0.1546 -0.1195 0.8336 0.0462 1.0000 Uiso . H13 H -0.0420 -0.0037 0.8169 0.0347 1.0000 Uiso . H14 H -0.0258 -0.0018 0.7084 0.0347 1.0000 Uiso . H15 H -0.004 0.1314 0.8230 0.0322 0.5000 Uiso . H16 H 0.016 0.1316 0.7148 0.0322 0.5000 Uiso . H17 H 0.149 0.1793 0.7864 0.0322 0.5000 Uiso . H18 H -0.140 -0.1410 0.7935 0.0292 0.5000 Uiso . H19 H -0.118 -0.1253 0.6869 0.0292 0.5000 Uiso . H20 H -0.045 -0.2117 0.7386 0.0292 0.5000 Uiso . C1 C 0.1614(14) 0.0537(8) 0.7853(8) 0.0345 1.0000 Uani . C2 C 0.2788(14) 0.0420(9) 0.7152(7) 0.0355 1.0000 Uani . C3 C 0.2124(15) -0.1090(9) 0.7049(8) 0.0404 1.0000 Uani . C4 C 0.0955(17) -0.0999(9) 0.7747(8) 0.0438 1.0000 Uani . C5 C 0.075(3) 0.1285(14) 0.7765(15) 0.0300 0.5000 Uani . C6 C -0.066(3) -0.1497(14) 0.7463(14) 0.0283 0.5000 Uani . O1 O -0.5076(9) -0.1992(5) 0.6144(5) 0.0225 1.0000 Uani . O2 O -0.4772(8) -0.1914(5) 0.3800(4) 0.0220 1.0000 Uani . O3 O -0.3031(8) -0.0808(4) 0.5157(5) 0.0230 1.0000 Uani . O5 O -0.506(1) -0.3519(5) 0.4885(5) 0.0310 1.0000 Uani . O4 O -0.3513(8) 0.0700(4) 0.5039(5) 0.0211 1.0000 Uani . O6 O 0.0695(9) -0.3042(5) 0.6083(5) 0.0273 1.0000 Uani . O7 O -0.0567(9) -0.3080(5) 0.3737(5) 0.0292 1.0000 Uani . O8 O -0.1472(8) -0.4305(4) 0.4996(4) 0.0212 1.0000 Uani . O10 O -0.011(1) -0.1493(5) 0.4910(5) 0.0287 1.0000 Uani . O9 O -0.1921(8) -0.5796(4) 0.5217(5) 0.0224 1.0000 Uani . O11 O -0.3786(9) -0.0026(5) 0.6441(5) 0.0260 1.0000 Uani . O12 O -0.1190(8) 0.0174(5) 0.5942(5) 0.0243 1.0000 Uani . O13 O -0.3454(9) -0.4753(5) 0.5903(5) 0.0250 1.0000 Uani . O14 O -0.0668(9) -0.4934(5) 0.6455(5) 0.0266 1.0000 Uani . U1 U -0.49283(4) -0.19665(2) 0.49706(2) 0.0159 1.0000 Uani . U2 U 0.00667(4) -0.30529(2) 0.49143(2) 0.0160 1.0000 Uani . S1 S -0.2900(3) 0.00166(15) 0.56762(15) 0.0162 1.0000 Uani . S2 S -0.1847(3) -0.49428(14) 0.56820(15) 0.0157 1.0000 Uani . F2 F -0.2406(6) -0.2563(4) 0.5209(4) 0.0249 1.0000 Uani . F1 F -0.7534(6) -0.2434(4) 0.4664(4) 0.0237 1.0000 Uani . N2 N 0.3428(11) -0.0472(6) 0.7200(6) 0.0297 1.0000 Uani . N1 N 0.0328(11) -0.0107(8) 0.7702(6) 0.0358 1.0000 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 C1 0.027(6) 0.045(7) 0.033(6) 0.002(5) 0.009(5) 0.004(5) C2 0.035(6) 0.050(8) 0.023(5) 0.004(5) 0.008(5) -0.006(6) C3 0.036(7) 0.054(8) 0.031(5) -0.005(5) 0.004(5) -0.011(6) C4 0.052(8) 0.053(9) 0.029(5) -0.003(5) 0.017(5) -0.015(7) C5 0.034(13) 0.021(11) 0.03(1) -0.002(8) -0.007(9) -0.009(9) C6 0.041(14) 0.02(1) 0.03(1) 0.007(8) 0.010(9) 0.002(9) O1 0.019(4) 0.021(4) 0.028(3) 0.002(3) 0.007(3) -0.001(3) O2 0.022(4) 0.023(4) 0.022(3) 0.002(3) 0.007(3) -0.001(3) O3 0.020(4) 0.016(3) 0.034(4) -0.003(3) 0.008(3) -0.001(3) O5 0.026(4) 0.012(3) 0.053(5) 0.005(3) -0.002(3) 0.003(3) O4 0.023(4) 0.007(3) 0.034(4) 0.000(3) 0.007(3) 0.004(3) O6 0.028(4) 0.028(4) 0.024(3) -0.001(3) -0.003(3) 0.007(3) O7 0.030(4) 0.025(4) 0.032(4) 0.000(3) 0.001(3) -0.003(3) O8 0.024(4) 0.018(4) 0.021(3) 0.007(3) 0.003(3) 0.001(3) O10 0.020(4) 0.014(3) 0.054(5) -0.002(3) 0.013(3) 0.003(3) O9 0.021(4) 0.012(3) 0.034(4) -0.008(3) 0.002(3) 0.005(3) O11 0.029(4) 0.030(4) 0.020(3) -0.001(3) 0.007(3) -0.001(3) O12 0.016(3) 0.030(4) 0.026(3) 0.004(3) 0.001(3) 0.001(3) O13 0.023(4) 0.028(4) 0.025(3) 0.001(3) 0.008(3) 0.001(3) O14 0.031(4) 0.025(4) 0.024(4) 0.000(3) 0.001(3) 0.002(3) U1 0.01288(19) 0.01296(19) 0.0220(2) 0.00071(13) 0.00275(13) -0.00004(16) U2 0.01199(19) 0.01255(19) 0.02320(19) 0.00031(14) 0.00039(12) -0.00030(16) S1 0.013(1) 0.016(1) 0.019(1) -0.0014(7) 0.0020(8) -0.0002(8) S2 0.014(1) 0.013(1) 0.020(1) 0.0012(8) 0.0026(8) 0.0014(8) F2 0.011(3) 0.020(3) 0.043(3) 0.001(2) 0.002(3) -0.003(2) F1 0.013(3) 0.016(3) 0.043(3) -0.003(2) 0.002(2) 0.001(2) N2 0.028(5) 0.038(6) 0.024(4) 0.001(4) 0.009(4) -0.007(4) N1 0.020(4) 0.076(8) 0.011(4) -0.006(4) 0.003(3) -0.014(5) _refine_ls_extinction_coef 17.6(15) _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 H1 . O5 . 0.999 no H2 . O5 . 1.000 no H3 . O10 . 0.999 no H4 . O10 . 0.999 no H5 . C1 . 0.998 no H6 . C2 . 1.009 no H7 . C2 . 0.998 no H8 . N2 . 1.004 no H9 . N2 . 1.000 no H10 . C3 . 0.997 no H11 . C3 . 1.005 no H12 . C4 . 1.003 no H13 . N1 . 0.996 no H14 . N1 . 1.000 no H15 . C5 . 1.010 no H16 . C5 . 0.992 no H17 . C5 . 1.009 no H18 . C6 . 0.998 no H19 . C6 . 1.012 no H20 . C6 . 0.991 no C1 . C2 . 1.528(15) yes C1 . C5 . 1.37(3) yes C1 . N1 . 1.475(15) yes C2 . N2 . 1.488(17) yes C3 . C4 . 1.518(16) yes C3 . N2 . 1.458(15) yes C4 . C6 . 1.58(3) yes C4 . N1 . 1.484(19) yes O1 . U1 . 1.761(7) yes O2 . U1 . 1.760(6) yes O3 . U1 . 2.405(7) yes O3 . S1 . 1.495(7) yes O5 . U1 . 2.420(7) yes O4 . U1 2_456 2.368(6) yes O4 . S1 . 1.476(7) yes O6 . U2 . 1.754(7) yes O7 . U2 . 1.767(7) yes O8 . U2 . 2.351(7) yes O8 . S2 . 1.482(7) yes O10 . U2 . 2.432(7) yes O9 . U2 2_546 2.401(7) yes O9 . S2 . 1.494(7) yes O11 . S1 . 1.432(7) yes O12 . S1 . 1.471(7) yes O13 . S2 . 1.462(7) yes O14 . S2 . 1.429(8) yes U1 . F2 . 2.311(5) yes U1 . F1 . 2.310(5) yes U2 . F2 . 2.310(5) yes U2 . F1 1_655 2.310(6) 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 H5 . C1 . C2 . 104.4 no H5 . C1 . C5 . 111.5 no C2 . C1 . C5 . 114.7(14) yes H5 . C1 . N1 . 116.1 no C2 . C1 . N1 . 109.8(10) yes C5 . C1 . N1 . 100.8(13) yes H6 . C2 . H7 . 108.891 no H6 . C2 . C1 . 109.2 no H7 . C2 . C1 . 110.1 no H6 . C2 . N2 . 108.7 no H7 . C2 . N2 . 110.1 no C1 . C2 . N2 . 109.8(9) yes H10 . C3 . H11 . 109.242 no H10 . C3 . C4 . 109.7 no H11 . C3 . C4 . 109.0 no H10 . C3 . N2 . 109.3 no H11 . C3 . N2 . 107.8 no C4 . C3 . N2 . 111.8(10) yes H12 . C4 . C3 . 105.6 no H12 . C4 . C6 . 114.1 no C3 . C4 . C6 . 112.3(12) yes H12 . C4 . N1 . 117.6 no C3 . C4 . N1 . 108.3(10) yes C6 . C4 . N1 . 98.9(12) yes H15 . C5 . H16 . 109.337 no H15 . C5 . H17 . 107.988 no H16 . C5 . H17 . 109.437 no H15 . C5 . C1 . 110.9 no H16 . C5 . C1 . 109.6 no H17 . C5 . C1 . 109.5 no H18 . C6 . H19 . 108.638 no H18 . C6 . H20 . 110.411 no H19 . C6 . H20 . 109.231 no H18 . C6 . C4 . 109.5 no H19 . C6 . C4 . 108.6 no H20 . C6 . C4 . 110.4 no U1 . O3 . S1 . 135.3(4) yes H1 . O5 . H2 . 121.832 no H1 . O5 . U1 . 121.8 no H2 . O5 . U1 . 116.4 no U1 2_456 O4 . S1 . 139.1(4) yes U2 . O8 . S2 . 138.9(4) yes H3 . O10 . H4 . 118.866 no H3 . O10 . U2 . 118.92 no H4 . O10 . U2 . 122.21 no U2 2_546 O9 . S2 . 135.0(4) yes O1 . U1 . O2 . 178.6(3) yes O1 . U1 . O3 . 91.5(3) yes O2 . U1 . O3 . 87.3(3) yes O1 . U1 . O5 . 91.2(3) yes O2 . U1 . O5 . 90.2(3) yes O3 . U1 . O5 . 141.2(3) yes O1 . U1 . O4 2_456 85.5(3) yes O2 . U1 . O4 2_456 93.5(3) yes O3 . U1 . O4 2_456 74.9(2) yes O5 . U1 . O4 2_456 143.9(3) yes O1 . U1 . F2 . 90.5(3) yes O2 . U1 . F2 . 89.8(3) yes O3 . U1 . F2 . 72.2(2) yes O5 . U1 . F2 . 69.1(2) yes O4 2_456 U1 . F2 . 146.7(2) yes O1 . U1 . F1 . 90.7(3) yes O2 . U1 . F1 . 89.9(3) yes O3 . U1 . F1 . 149.8(2) yes O5 . U1 . F1 . 68.9(2) yes O4 2_456 U1 . F1 . 75.3(2) yes F2 . U1 . F1 . 137.9(2) yes O6 . U2 . O7 . 179.2(3) yes O6 . U2 . O8 . 93.6(3) yes O7 . U2 . O8 . 85.8(3) yes O6 . U2 . O10 . 90.2(3) yes O7 . U2 . O10 . 90.6(3) yes O8 . U2 . O10 . 142.4(2) yes O6 . U2 . O9 2_546 87.9(3) yes O7 . U2 . O9 2_546 91.6(3) yes O8 . U2 . O9 2_546 75.8(2) yes O10 . U2 . O9 2_546 141.7(3) yes O6 . U2 . F2 . 89.2(3) yes O7 . U2 . F2 . 91.1(3) yes O8 . U2 . F2 . 75.4(2) yes O10 . U2 . F2 . 67.3(2) yes O9 2_546 U2 . F2 . 150.8(2) yes O6 . U2 . F1 1_655 89.1(3) yes O7 . U2 . F1 1_655 91.2(3) yes O8 . U2 . F1 1_655 148.5(2) yes O10 . U2 . F1 1_655 68.8(2) yes O9 2_546 U2 . F1 1_655 73.0(2) yes F2 . U2 . F1 1_655 136.0(2) yes O3 . S1 . O4 . 106.7(4) yes O3 . S1 . O11 . 110.8(4) yes O4 . S1 . O11 . 111.4(4) yes O3 . S1 . O12 . 107.0(4) yes O4 . S1 . O12 . 108.1(4) yes O11 . S1 . O12 . 112.4(4) yes O8 . S2 . O9 . 106.2(4) yes O8 . S2 . O13 . 107.2(4) yes O9 . S2 . O13 . 107.1(4) yes O8 . S2 . O14 . 111.2(4) yes O9 . S2 . O14 . 111.5(4) yes O13 . S2 . O14 . 113.3(4) yes U1 . F2 . U2 . 159.9(3) yes U1 . F1 . U2 1_455 158.6(3) yes H8 . N2 . H9 . 109.129 no H8 . N2 . C2 . 109.5 no H9 . N2 . C2 . 109.7 no H8 . N2 . C3 . 109.1 no H9 . N2 . C3 . 109.3 no C2 . N2 . C3 . 110.2(10) yes H13 . N1 . H14 . 109.800 no H13 . N1 . C1 . 109.6 no H14 . N1 . C1 . 108.8 no H13 . N1 . C4 . 108.7 no H14 . N1 . C4 . 107.9 no C1 . N1 . C4 . 112.1(9) yes #===END data_USFO-6 _database_code_depnum_ccdc_archive 'CCDC 263739' _audit_creation_date 05-14-03 _audit_creation_method CRYSTALS_ver_12-03-99 #============================================================= _cell_length_a 10.8832(2) _cell_angle_alpha 75.6604(8) _cell_length_b 10.9386(2) _cell_angle_beta 73.6101(7) _cell_length_c 16.5325(3) _cell_angle_gamma 89.7726(7) _cell_volume 1824.73(6) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _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 '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 'S ' 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B 'F ' 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 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 '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 '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 _cell_formula_units_Z 2 _chemical_formula_sum ' C12 H36 F4 N4 O25 S4 U4 ' _chemical_formula_moiety ' C12 H36 F4 N4 O25 S4 U4 ' _chemical_compound_source ; ? ; _chemical_formula_weight 1792.80 _cell_measurement_reflns_used 7796 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.16 _exptl_crystal_density_diffrn 3.263 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1608.000 _exptl_absorpt_coefficient_mu 18.039 # Sheldrick geometric definitions 0.11 0.34 _diffrn_measurement_device_type ; 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 ; SHELXS 86 (Sheldrick, 1986) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.11 _exptl_absorpt_correction_T_max 0.34 _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 15248 _reflns_number_total 8296 _diffrn_reflns_av_R_equivalents 0.02 # Number of reflections with Friedels Law is 8296 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 8397 _diffrn_reflns_theta_min 5.122 _diffrn_reflns_theta_max 27.515 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.896 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -13 _reflns_limit_h_max 14 _reflns_limit_k_min -13 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _refine_diff_density_min -2.57 _refine_diff_density_max 3.39 _refine_ls_number_reflns 6969 _refine_ls_number_parameters 479 #_refine_ls_R_factor_ref 0.0387 _refine_ls_wR_factor_ref 0.0945 _refine_ls_goodness_of_fit_ref 0.8816 #_reflns_number_all 8296 _refine_ls_R_factor_all 0.0480 _refine_ls_wR_factor_all 0.0995 # 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 6969 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_gt 0.0945 _refine_ls_shift/su_max 0.000990 _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 27.9 42.3 25.9 9.61 2.82 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; 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. Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. 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 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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 H19 H 0.3132 0.5672 0.4635 0.0336 1.0000 Uiso . H20 H 0.3714 0.4766 0.3989 0.0336 1.0000 Uiso . H21 H 0.4326 0.4819 0.4776 0.0336 1.0000 Uiso . H22 H 0.1767 0.381 0.5030 0.0294 1.0000 Uiso . H23 H 0.2378 0.386 0.5817 0.0294 1.0000 Uiso . H24 H 0.3576 0.2556 0.4541 0.0314 1.0000 Uiso . H25 H 0.3773 0.2390 0.5504 0.0314 1.0000 Uiso . H26 H 0.145 0.157 0.5235 0.0294 1.0000 Uiso . H27 H 0.175 0.132 0.6173 0.0294 1.0000 Uiso . H28 H 0.3285 0.038 0.4771 0.0192 1.0000 Uiso . H29 H 0.3290 -0.004 0.5789 0.0192 1.0000 Uiso . H30 H 0.1222 -0.0519 0.5144 0.0293 1.0000 Uiso . H31 H 0.1133 -0.0852 0.6179 0.0293 1.0000 Uiso . H32 H 0.2882 -0.198 0.4975 0.0016 1.0000 Uiso . H33 H 0.2538 -0.241 0.6037 0.0016 1.0000 Uiso . H34 H 0.0738 -0.2601 0.5074 0.0315 1.0000 Uiso . H35 H 0.1404 -0.3802 0.5548 0.0315 1.0000 Uiso . H36 H 0.0393 -0.3030 0.6137 0.0315 1.0000 Uiso . H1 H 0.3958 0.6432 0.1023 0.0305 1.0000 Uiso . H2 H 0.4720 0.5928 0.0178 0.0305 1.0000 Uiso . H3 H 0.5384 0.7065 0.0427 0.0305 1.0000 Uiso . H4 H 0.378 0.8422 0.0080 0.0266 1.0000 Uiso . H5 H 0.454 0.7918 -0.0765 0.0266 1.0000 Uiso . H6 H 0.2227 0.6574 0.0434 0.0262 1.0000 Uiso . H7 H 0.2880 0.6510 -0.0572 0.0262 1.0000 Uiso . H8 H 0.169 0.867 -0.0088 0.0249 1.0000 Uiso . H9 H 0.229 0.855 -0.1088 0.0249 1.0000 Uiso . H10 H 0.024 0.681 0.0143 0.0271 1.0000 Uiso . H11 H 0.071 0.703 -0.0914 0.0271 1.0000 Uiso . H12 H -0.0528 0.8820 -0.0004 0.0225 1.0000 Uiso . H13 H 0.0050 0.9139 -0.1065 0.0225 1.0000 Uiso . H14 H -0.197 0.725 -0.0077 0.0286 1.0000 Uiso . H15 H -0.146 0.774 -0.1139 0.0286 1.0000 Uiso . H16 H -0.2667 0.9291 0.0004 0.0300 1.0000 Uiso . H17 H -0.2156 0.9787 -0.1058 0.0300 1.0000 Uiso . H18 H -0.3363 0.8725 -0.0595 0.0300 1.0000 Uiso . N1 N 0.2692(8) 0.7084(8) -0.0172(6) 0.0186 1.0000 Uani . N2 N -0.0356(8) 0.8456(8) -0.0523(6) 0.0192 1.0000 Uani . N3 N 0.3131(8) 0.2524(8) 0.5168(6) 0.0180 1.0000 Uani . N4 N 0.1720(8) -0.0780(8) 0.5576(6) 0.0208 1.0000 Uani . C1 C 0.4555(11) 0.6690(11) 0.0413(7) 0.0267 1.0000 Uani . C2 C 0.394(1) 0.7658(11) -0.0156(7) 0.0231 1.0000 Uani . C3 C 0.186(1) 0.807(1) -0.0472(7) 0.0212 1.0000 Uani . C4 C 0.057(1) 0.746(1) -0.0429(7) 0.0219 1.0000 Uani . C5 C -0.160(1) 0.800(1) -0.0582(7) 0.0211 1.0000 Uani . C6 C -0.2520(11) 0.9036(11) -0.0556(7) 0.0254 1.0000 Uani . C7 C 0.3513(12) 0.4843(11) 0.4602(8) 0.0286 1.0000 Uani . C8 C 0.2579(11) 0.378(1) 0.5204(7) 0.0243 1.0000 Uani . C9 C 0.214(1) 0.142(1) 0.5532(7) 0.0223 1.0000 Uani . C10 C 0.2739(11) 0.022(1) 0.5391(7) 0.0229 1.0000 Uani . C11 C 0.2186(11) -0.206(1) 0.5534(7) 0.0245 1.0000 Uani . C12 C 0.1094(11) -0.2944(11) 0.5577(7) 0.0261 1.0000 Uani . O1 O 0.5032(7) 0.7831(6) 0.3772(4) 0.0165 1.0000 Uani . O2 O 0.5030(7) 0.9408(6) 0.1610(4) 0.0176 1.0000 Uani . O3 O 0.7287(7) 0.8634(7) 0.2260(6) 0.0241 1.0000 Uani . O4 O 0.5983(7) 0.0489(6) 0.2871(5) 0.0180 1.0000 Uani . O5 O 0.3140(6) 0.9605(6) 0.3327(4) 0.0141 1.0000 Uani . O6 O 0.6712(7) 0.4915(7) 0.3284(4) 0.0181 1.0000 Uani . O7 O 0.6905(7) 0.5116(7) 0.1076(4) 0.0165 1.0000 Uani . O8 O 0.8241(6) 0.6927(6) 0.1659(4) 0.0122 1.0000 Uani . O9 O -0.1145(7) 0.4194(7) 0.1927(5) 0.0201 1.0000 Uani . O10 O 0.6682(6) 0.2694(6) 0.2445(5) 0.0173 1.0000 Uani . O11 O 0.2370(6) 0.2899(6) 0.3617(4) 0.0138 1.0000 Uani . O13 O 0.4622(6) 0.2026(6) 0.2365(4) 0.0155 1.0000 Uani . O14 O 0.2085(6) 1.1269(6) 0.2556(4) 0.0131 1.0000 Uani . O15 O 0.0722(7) 0.3443(6) 0.2336(4) 0.0156 1.0000 Uani . O16 O 0.0598(7) 0.6489(7) 0.3819(4) 0.0152 1.0000 Uani . O17 O 0.1824(6) 0.7650(6) 0.1515(4) 0.0143 1.0000 Uani . O18 O -0.0068(6) 0.5429(6) 0.2567(4) 0.0151 1.0000 Uani . O19 O 0.9208(6) 0.7854(6) 0.2545(4) 0.0153 1.0000 Uani . O20 O 0.1362(7) 0.9143(6) 0.2809(5) 0.0176 1.0000 Uani . O21 O 0.9266(7) 0.9025(7) 0.1091(5) 0.0202 1.0000 Uani . O22 O 0.4986(7) 0.1868(7) 0.3776(5) 0.0185 1.0000 Uani . O23 O 0.0934(7) 0.5249(7) 0.1087(5) 0.0178 1.0000 Uani . O24 O 0.0994(7) 1.0073(7) 0.4026(4) 0.0187 1.0000 Uani . O25 O 0.0974(8) -0.127(1) 0.7463(6) 0.0346 1.0000 Uani . F1 F 0.5648(6) 0.6817(5) 0.2217(4) 0.0189 1.0000 Uani . F2 F 0.4704(5) 0.4406(5) 0.2523(4) 0.0171 1.0000 Uani . F4 F 0.3225(5) 0.7414(5) 0.2834(4) 0.0189 1.0000 Uani . S1 S 0.8509(2) 0.8106(2) 0.18825(15) 0.0123 1.0000 Uani . S2 S 0.5547(2) 0.1773(2) 0.28905(15) 0.0114 1.0000 Uani . S3 S 0.0130(2) 0.4615(2) 0.19551(15) 0.0125 1.0000 Uani . S4 S 0.1888(2) 1.0018(2) 0.31950(15) 0.0117 1.0000 Uani . U1 U 0.50202(3) 0.86040(3) 0.26820(2) 0.0110 1.0000 Uani . U2 U 0.67967(3) 0.50467(3) 0.21827(2) 0.0108 1.0000 Uani . U3 U 0.28922(3) 0.33227(3) 0.24547(2) 0.0106 1.0000 Uani . U4 U 0.12296(3) 0.70649(3) 0.26659(2) 0.0108 1.0000 Uani . F3 F 0.2395(5) 0.5330(5) 0.2499(4) 0.0176 1.0000 Uani . O12 O 0.3402(7) 0.3721(6) 0.1301(4) 0.0159 1.0000 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 N1 0.019(4) 0.018(4) 0.019(4) -0.010(3) -0.002(3) 0.003(3) N2 0.019(4) 0.016(4) 0.021(4) -0.002(3) -0.005(3) -0.001(3) N3 0.019(4) 0.016(4) 0.020(4) -0.005(3) -0.007(3) 0.002(3) N4 0.017(4) 0.021(4) 0.022(4) -0.006(3) -0.002(3) 0.003(3) C1 0.020(5) 0.027(6) 0.026(5) 0.002(4) -0.004(4) 0.005(4) C2 0.020(5) 0.026(5) 0.020(5) 0.000(4) -0.004(4) -0.005(4) C3 0.022(5) 0.021(5) 0.019(5) -0.003(4) -0.003(4) 0.001(4) C4 0.026(5) 0.018(5) 0.023(5) -0.008(4) -0.006(4) 0.001(4) C5 0.024(5) 0.020(5) 0.026(5) -0.010(4) -0.014(4) 0.002(4) C6 0.023(5) 0.024(5) 0.026(5) -0.005(4) -0.004(4) -0.001(4) C7 0.027(6) 0.020(5) 0.038(6) -0.009(5) -0.007(5) -0.005(4) C8 0.026(5) 0.019(5) 0.029(6) -0.011(4) -0.006(4) -0.004(4) C9 0.022(5) 0.020(5) 0.019(5) -0.004(4) 0.002(4) -0.003(4) C10 0.024(5) 0.023(5) 0.020(5) -0.005(4) -0.005(4) 0.004(4) C11 0.029(6) 0.020(5) 0.025(5) -0.010(4) -0.006(4) 0.003(4) C12 0.024(5) 0.029(6) 0.023(5) -0.011(4) -0.001(4) 0.002(4) O1 0.020(3) 0.016(3) 0.012(3) 0.000(2) -0.006(3) 0.003(3) O2 0.021(4) 0.015(3) 0.012(3) 0.006(2) -0.006(3) -0.001(3) O3 0.012(3) 0.022(4) 0.048(5) -0.022(3) -0.013(3) 0.010(3) O4 0.017(3) 0.012(3) 0.031(4) -0.008(3) -0.014(3) 0.011(3) O5 0.010(3) 0.013(3) 0.022(3) -0.009(3) -0.006(3) 0.004(2) O6 0.022(4) 0.024(4) 0.010(3) -0.009(3) -0.002(3) 0.004(3) O7 0.021(3) 0.020(3) 0.012(3) -0.011(3) -0.006(3) 0.006(3) O8 0.007(3) 0.015(3) 0.016(3) -0.007(2) -0.003(2) -0.000(2) O9 0.014(3) 0.016(3) 0.036(4) -0.013(3) -0.010(3) 0.004(3) O10 0.013(3) 0.007(3) 0.031(4) -0.001(3) -0.009(3) 0.003(2) O11 0.018(3) 0.019(3) 0.002(3) 0.001(2) -0.001(2) -0.003(3) O13 0.015(3) 0.016(3) 0.019(3) -0.007(3) -0.008(3) 0.003(3) O14 0.014(3) 0.010(3) 0.017(3) -0.003(2) -0.008(3) 0.004(2) O15 0.017(3) 0.011(3) 0.022(3) -0.006(3) -0.008(3) 0.000(3) O16 0.022(3) 0.022(3) 0.002(3) -0.003(2) -0.003(2) -0.001(3) O17 0.016(3) 0.014(3) 0.011(3) -0.003(2) -0.002(2) 0.001(3) O18 0.014(3) 0.017(3) 0.019(3) -0.009(3) -0.008(3) 0.005(3) O19 0.015(3) 0.012(3) 0.021(3) -0.008(3) -0.005(3) 0.002(2) O20 0.017(3) 0.010(3) 0.032(4) -0.011(3) -0.010(3) 0.003(3) O21 0.022(4) 0.016(3) 0.021(4) -0.003(3) -0.005(3) -0.004(3) O22 0.019(3) 0.019(3) 0.019(3) -0.008(3) -0.004(3) 0.005(3) O23 0.014(3) 0.016(3) 0.020(3) -0.004(3) -0.000(3) -0.000(3) O24 0.015(3) 0.022(4) 0.017(3) -0.006(3) -0.000(3) 0.009(3) O25 0.018(4) 0.053(6) 0.031(4) -0.008(4) -0.007(3) 0.012(4) F1 0.018(3) 0.011(3) 0.031(3) -0.011(2) -0.007(2) 0.003(2) F2 0.011(3) 0.012(3) 0.031(3) -0.009(2) -0.008(2) 0.006(2) F4 0.011(3) 0.017(3) 0.036(3) -0.015(2) -0.012(2) 0.001(2) S1 0.010(1) 0.0104(9) 0.018(1) -0.0060(8) -0.0051(8) 0.0011(8) S2 0.0087(9) 0.0073(9) 0.0198(11) -0.0052(8) -0.0053(8) 0.0009(7) S3 0.010(1) 0.0104(9) 0.0199(11) -0.0064(8) -0.0060(8) 0.0017(8) S4 0.010(1) 0.0085(9) 0.018(1) -0.0062(8) -0.0045(8) 0.0023(7) U1 0.00879(16) 0.00913(15) 0.01703(17) -0.00514(12) -0.00513(12) 0.00176(11) U2 0.00829(16) 0.00941(16) 0.01641(16) -0.00551(12) -0.00429(12) 0.00134(11) U3 0.00843(16) 0.00893(16) 0.01572(16) -0.00471(11) -0.00439(12) 0.00137(11) U4 0.00901(16) 0.00884(16) 0.01579(17) -0.00494(12) -0.00407(12) 0.00080(11) F3 0.014(3) 0.013(3) 0.036(3) -0.018(2) -0.012(2) 0.012(2) O12 0.021(3) 0.018(3) 0.001(3) 0.003(2) 0.003(2) -0.002(3) _refine_ls_extinction_coef 13.9(14) _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 H19 . C7 . 1.004 no H20 . C7 . 1.000 no H21 . C7 . 1.002 no H22 . C8 . 1.002 no H23 . C8 . 1.004 no H24 . N3 . 1.005 no H25 . N3 . 0.999 no H26 . C9 . 1.000 no H27 . C9 . 1.002 no H28 . C10 . 1.002 no H29 . C10 . 1.002 no H30 . N4 . 1.001 no H31 . N4 . 1.005 no H32 . C11 . 1.000 no H33 . C11 . 1.003 no H34 . C12 . 1.003 no H35 . C12 . 1.004 no H36 . C12 . 1.003 no H1 . C1 . 1.004 no H2 . C1 . 0.999 no H3 . C1 . 1.002 no H4 . C2 . 1.001 no H5 . C2 . 1.004 no H6 . N1 . 1.005 no H7 . N1 . 1.002 no H8 . C3 . 1.006 no H9 . C3 . 1.003 no H10 . C4 . 1.002 no H11 . C4 . 1.003 no H12 . N2 . 1.002 no H13 . N2 . 1.002 no H14 . C5 . 1.007 no H15 . C5 . 1.001 no H16 . C6 . 1.002 no H17 . C6 . 1.001 no H18 . C6 . 1.004 no N1 . C2 . 1.511(13) yes N1 . C3 . 1.486(13) yes N2 . C4 . 1.495(13) yes N2 . C5 . 1.482(13) yes N3 . C8 . 1.501(13) yes N3 . C9 . 1.509(13) yes N4 . C10 . 1.475(14) yes N4 . C11 . 1.500(13) yes C1 . C2 . 1.518(15) yes C3 . C4 . 1.524(15) yes C5 . C6 . 1.507(15) yes C7 . C8 . 1.500(15) yes C9 . C10 . 1.501(15) yes C11 . C12 . 1.509(16) yes O1 . U1 . 1.795(6) yes O2 . U1 . 1.769(6) yes O3 . S1 . 1.481(7) yes O3 . U1 . 2.365(7) yes O4 . S2 . 1.486(7) yes O4 . U1 1_545 2.443(7) yes O5 . S4 . 1.491(7) yes O5 . U1 . 2.419(6) yes O6 . U2 . 1.767(6) yes O7 . U2 . 1.783(6) yes O8 . S1 . 1.479(7) yes O8 . U2 . 2.413(6) yes O9 . S3 . 1.480(7) yes O9 . U2 1_455 2.389(7) yes O10 . S2 . 1.488(7) yes O10 . U2 . 2.499(6) yes O11 . U3 . 1.781(6) yes O13 . S2 . 1.489(7) yes O13 . U3 . 2.346(7) yes O14 . S4 . 1.481(6) yes O14 . U3 1_565 2.365(6) yes O15 . S3 . 1.509(7) yes O15 . U3 . 2.424(7) yes O16 . U4 . 1.781(6) yes O17 . U4 . 1.776(6) yes O18 . S3 . 1.478(7) yes O18 . U4 . 2.349(7) yes O19 . S1 . 1.474(7) yes O19 . U4 1_655 2.403(7) yes O20 . S4 . 1.471(7) yes O20 . U4 . 2.352(6) yes O21 . S1 . 1.465(7) yes O22 . S2 . 1.448(7) yes O23 . S3 . 1.452(7) yes O24 . S4 . 1.457(7) yes F1 . U1 . 2.305(5) yes F1 . U2 . 2.305(5) yes F2 . U2 . 2.256(5) yes F2 . U3 . 2.348(6) yes F4 . U1 . 2.271(5) yes F4 . U4 . 2.311(5) yes U3 . F3 . 2.274(5) yes U3 . O12 . 1.769(6) yes U4 . F3 . 2.308(5) 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 H6 . N1 . H7 . 108.915 no H6 . N1 . C2 . 108.6 no H7 . N1 . C2 . 109.1 no H6 . N1 . C3 . 109.1 no H7 . N1 . C3 . 109.1 no C2 . N1 . C3 . 112.0(8) yes H12 . N2 . H13 . 109.108 no H12 . N2 . C4 . 108.3 no H13 . N2 . C4 . 108.3 no H12 . N2 . C5 . 108.3 no H13 . N2 . C5 . 108.2 no C4 . N2 . C5 . 114.6(8) yes H24 . N3 . H25 . 109.119 no H24 . N3 . C8 . 108.2 no H25 . N3 . C8 . 108.6 no H24 . N3 . C9 . 108.4 no H25 . N3 . C9 . 108.8 no C8 . N3 . C9 . 113.7(8) yes H30 . N4 . H31 . 109.025 no H30 . N4 . C10 . 108.3 no H31 . N4 . C10 . 108.0 no H30 . N4 . C11 . 108.3 no H31 . N4 . C11 . 108.2 no C10 . N4 . C11 . 114.9(8) yes H1 . C1 . H2 . 109.282 no H1 . C1 . H3 . 109.044 no H2 . C1 . H3 . 109.463 no H1 . C1 . C2 . 109.2 no H2 . C1 . C2 . 109.9 no H3 . C1 . C2 . 109.9 no H4 . C2 . H5 . 109.008 no H4 . C2 . N1 . 109.7 no H5 . C2 . N1 . 109.4 no H4 . C2 . C1 . 109.9 no H5 . C2 . C1 . 109.3 no N1 . C2 . C1 . 109.6(9) yes H8 . C3 . H9 . 108.739 no H8 . C3 . N1 . 109.6 no H9 . C3 . N1 . 109.8 no H8 . C3 . C4 . 108.8 no H9 . C3 . C4 . 109.3 no N1 . C3 . C4 . 110.5(8) yes H10 . C4 . H11 . 109.075 no H10 . C4 . N2 . 110.0 no H11 . C4 . N2 . 109.8 no H10 . C4 . C3 . 109.4 no H11 . C4 . C3 . 109.2 no N2 . C4 . C3 . 109.4(8) yes H14 . C5 . H15 . 108.891 no H14 . C5 . N2 . 109.3 no H15 . C5 . N2 . 109.6 no H14 . C5 . C6 . 109.5 no H15 . C5 . C6 . 109.6 no N2 . C5 . C6 . 110.0(8) yes H16 . C6 . H17 . 109.243 no H16 . C6 . H18 . 108.951 no H17 . C6 . H18 . 109.099 no H16 . C6 . C5 . 109.8 no H17 . C6 . C5 . 109.9 no H18 . C6 . C5 . 109.9 no H19 . C7 . H20 . 109.167 no H19 . C7 . H21 . 108.985 no H20 . C7 . H21 . 109.294 no H19 . C7 . C8 . 109.7 no H20 . C7 . C8 . 109.8 no H21 . C7 . C8 . 109.8 no H22 . C8 . H23 . 109.004 no H22 . C8 . N3 . 109.2 no H23 . C8 . N3 . 109.0 no H22 . C8 . C7 . 109.5 no H23 . C8 . C7 . 109.4 no N3 . C8 . C7 . 110.7(9) yes H26 . C9 . H27 . 109.262 no H26 . C9 . N3 . 109.6 no H27 . C9 . N3 . 109.3 no H26 . C9 . C10 . 109.0 no H27 . C9 . C10 . 109.0 no N3 . C9 . C10 . 110.6(9) yes H28 . C10 . H29 . 109.167 no H28 . C10 . N4 . 109.7 no H29 . C10 . N4 . 109.9 no H28 . C10 . C9 . 109.3 no H29 . C10 . C9 . 109.4 no N4 . C10 . C9 . 109.4(9) yes H32 . C11 . H33 . 109.161 no H32 . C11 . N4 . 109.3 no H33 . C11 . N4 . 109.4 no H32 . C11 . C12 . 109.6 no H33 . C11 . C12 . 109.4 no N4 . C11 . C12 . 110.0(9) yes H34 . C12 . H35 . 108.934 no H34 . C12 . H36 . 108.987 no H35 . C12 . H36 . 108.939 no H34 . C12 . C11 . 109.8 no H35 . C12 . C11 . 110.1 no H36 . C12 . C11 . 110.0 no S1 . O3 . U1 . 151.8(5) yes S2 . O4 . U1 1_545 133.6(4) yes S4 . O5 . U1 . 141.4(4) yes S1 . O8 . U2 . 141.8(4) yes S3 . O9 . U2 1_455 134.1(4) yes S2 . O10 . U2 . 128.7(4) yes S2 . O13 . U3 . 130.7(4) yes S4 . O14 . U3 1_565 136.3(4) yes S3 . O15 . U3 . 126.5(4) yes S3 . O18 . U4 . 132.3(4) yes S1 . O19 . U4 1_655 137.2(4) yes S4 . O20 . U4 . 146.7(4) yes U1 . F1 . U2 . 154.2(3) yes U2 . F2 . U3 . 157.3(3) yes U1 . F4 . U4 . 154.8(3) yes O3 . S1 . O8 . 110.0(4) yes O3 . S1 . O19 . 107.2(4) yes O8 . S1 . O19 . 110.7(4) yes O3 . S1 . O21 . 109.6(5) yes O8 . S1 . O21 . 109.2(4) yes O19 . S1 . O21 . 110.2(4) yes O4 . S2 . O10 . 107.7(4) yes O4 . S2 . O13 . 106.8(4) yes O10 . S2 . O13 . 108.1(4) yes O4 . S2 . O22 . 111.5(4) yes O10 . S2 . O22 . 110.2(4) yes O13 . S2 . O22 . 112.3(4) yes O9 . S3 . O15 . 106.7(4) yes O9 . S3 . O18 . 108.1(4) yes O15 . S3 . O18 . 107.6(4) yes O9 . S3 . O23 . 110.9(4) yes O15 . S3 . O23 . 110.7(4) yes O18 . S3 . O23 . 112.6(4) yes O5 . S4 . O14 . 109.9(4) yes O5 . S4 . O20 . 110.1(4) yes O14 . S4 . O20 . 105.9(4) yes O5 . S4 . O24 . 109.7(4) yes O14 . S4 . O24 . 110.6(4) yes O20 . S4 . O24 . 110.6(4) yes O1 . U1 . O2 . 178.2(3) yes O1 . U1 . O3 . 88.0(3) yes O2 . U1 . O3 . 91.4(3) yes O1 . U1 . O4 1_565 87.1(3) yes O2 . U1 . O4 1_565 91.1(3) yes O3 . U1 . O4 1_565 68.5(2) yes O1 . U1 . O5 . 87.3(3) yes O2 . U1 . O5 . 92.3(3) yes O3 . U1 . O5 . 146.7(2) yes O4 1_565 U1 . O5 . 78.3(2) yes O1 . U1 . F1 . 91.3(3) yes O2 . U1 . F1 . 90.0(3) yes O3 . U1 . F1 . 70.7(2) yes O4 1_565 U1 . F1 . 139.3(2) yes O5 . U1 . F1 . 142.3(2) yes O1 . U1 . F4 . 91.3(3) yes O2 . U1 . F4 . 90.2(3) yes O3 . U1 . F4 . 142.6(2) yes O4 1_565 U1 . F4 . 148.8(2) yes O5 . U1 . F4 . 70.5(2) yes F1 . U1 . F4 . 71.9(2) yes O6 . U2 . O7 . 177.6(3) yes O6 . U2 . O8 . 93.1(3) yes O7 . U2 . O8 . 88.1(3) yes O6 . U2 . O9 1_655 91.2(3) yes O7 . U2 . O9 1_655 87.1(3) yes O8 . U2 . O9 1_655 77.7(2) yes O6 . U2 . O10 . 91.0(3) yes O7 . U2 . O10 . 86.8(3) yes O8 . U2 . O10 . 144.1(2) yes O9 1_655 U2 . O10 . 66.6(2) yes O6 . U2 . F1 . 87.6(3) yes O7 . U2 . F1 . 94.7(3) yes O8 . U2 . F1 . 69.9(2) yes O9 1_655 U2 . F1 . 147.4(2) yes O10 . U2 . F1 . 146.0(2) yes O6 . U2 . F2 . 92.6(3) yes O7 . U2 . F2 . 87.6(3) yes O8 . U2 . F2 . 142.0(2) yes O9 1_655 U2 . F2 . 139.7(2) yes O10 . U2 . F2 . 73.3(2) yes F1 . U2 . F2 . 72.9(2) yes O11 . U3 . O13 . 94.3(3) yes O11 . U3 . O14 1_545 86.2(3) yes O13 . U3 . O14 1_545 72.7(2) yes O11 . U3 . O15 . 93.4(3) yes O13 . U3 . O15 . 142.8(2) yes O14 1_545 U3 . O15 . 71.5(2) yes O11 . U3 . F2 . 88.1(3) yes O13 . U3 . F2 . 69.7(2) yes O14 1_545 U3 . F2 . 141.5(2) yes O15 . U3 . F2 . 146.9(2) yes O11 . U3 . F3 . 87.8(3) yes O13 . U3 . F3 . 141.4(2) yes O14 1_545 U3 . F3 . 145.7(2) yes O15 . U3 . F3 . 75.2(2) yes F2 . U3 . F3 . 71.84(19) yes O11 . U3 . O12 . 179.2(3) yes O13 . U3 . O12 . 85.5(3) yes O14 1_545 U3 . O12 . 93.0(3) yes O15 . U3 . O12 . 86.3(3) yes F2 . U3 . O12 . 92.6(3) yes F3 . U3 . O12 . 92.9(3) yes O16 . U4 . O17 . 178.7(3) yes O16 . U4 . O18 . 86.6(3) yes O17 . U4 . O18 . 92.9(3) yes O16 . U4 . O19 1_455 91.6(3) yes O17 . U4 . O19 1_455 87.1(3) yes O18 . U4 . O19 1_455 71.0(2) yes O16 . U4 . O20 . 90.3(3) yes O17 . U4 . O20 . 89.5(3) yes O18 . U4 . O20 . 146.7(2) yes O19 1_455 U4 . O20 . 76.0(2) yes O16 . U4 . F4 . 89.4(3) yes O17 . U4 . F4 . 91.7(3) yes O18 . U4 . F4 . 140.1(2) yes O19 1_455 U4 . F4 . 148.9(2) yes O20 . U4 . F4 . 72.9(2) yes O16 . U4 . F3 . 94.4(3) yes O17 . U4 . F3 . 86.5(3) yes O18 . U4 . F3 . 69.5(2) yes O19 1_455 U4 . F3 . 139.5(2) yes O20 . U4 . F3 . 143.8(2) yes F4 . U4 . F3 . 71.3(2) yes U3 . F3 . U4 . 161.4(3) yes #===END data_USFO-7 _database_code_depnum_ccdc_archive 'CCDC 263740' _audit_creation_date 04-03-06 _audit_creation_method CRYSTALS_ver_12-03-99 #============================================================= _cell_length_a 6.7745(2) _cell_angle_alpha 90 _cell_length_b 8.1589(2) _cell_angle_beta 94.556(1) _cell_length_c 14.3661(4) _cell_angle_gamma 90 _cell_volume 791.54(4) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y+1/2,-z # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration unk 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 '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 'S ' 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 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 '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 '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 'F ' 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 2 _chemical_formula_sum ' C3 H14 F2 N2 O13 S2 U2 ' _chemical_formula_moiety ' C3 H14 F2 N2 O13 S2 U2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 864.34 _cell_measurement_reflns_used 1841 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 3.626 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 768.000 _exptl_absorpt_coefficient_mu 20.788 # Sheldrick geometric definitions 0.08 0.19 _diffrn_measurement_device_type ; 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 0.08 _exptl_absorpt_correction_T_max 0.19 _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 3484 _reflns_number_total 3476 _diffrn_reflns_av_R_equivalents 0.00 # Number of reflections with Friedels Law is 3476 # Number of reflections without Friedels Law is 3476 # Theoretical number of reflections is about 1817 _diffrn_reflns_theta_min 5.197 _diffrn_reflns_theta_max 27.493 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.356 _diffrn_measured_fraction_theta_full 0.987 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -8 _reflns_limit_h_max 8 _reflns_limit_k_min -10 _reflns_limit_k_max 10 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _refine_diff_density_min -3.52 _refine_diff_density_max 4.01 _refine_ls_number_reflns 3415 _refine_ls_number_parameters 219 #_refine_ls_R_factor_ref 0.0314 _refine_ls_wR_factor_ref 0.0819 _refine_ls_goodness_of_fit_ref 0.9297 #_reflns_number_all 3476 _refine_ls_R_factor_all 0.0321 _refine_ls_wR_factor_all 0.0825 # 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 3415 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_gt 0.0819 _refine_ls_shift/su_max 0.001064 _refine_ls_abs_structure_Flack 0.028(13) _refine_ls_abs_structure_details 'Flack, 0 Friedel-pairs' _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 28.6 45.9 29.0 13.3 4.41 ; _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 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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 H1 H 0.8361 0.5157 0.7418 0.0364 1.0000 Uiso . H2 H 0.9595 0.4647 0.8398 0.0364 1.0000 Uiso . H3 H 0.9494 0.2754 0.6678 0.0318 1.0000 Uiso . H4 H 1.0882 0.2271 0.7619 0.0318 1.0000 Uiso . H5 H 0.6655 0.2534 0.7564 0.0332 1.0000 Uiso . H6 H 0.8109 0.1866 0.8443 0.0332 1.0000 Uiso . H7 H 1.1357 0.6668 0.7613 0.0388 1.0000 Uiso . H8 H 1.1379 0.5468 0.6703 0.0388 1.0000 Uiso . H9 H 1.2614 0.4958 0.7683 0.0388 1.0000 Uiso . H10 H 0.6571 -0.0354 0.7622 0.0374 1.0000 Uiso . H11 H 0.7508 0.0251 0.6668 0.0374 1.0000 Uiso . H12 H 0.8962 -0.0417 0.7547 0.0374 1.0000 Uiso . N1 N 1.1375(18) 0.5500(15) 0.7398(9) 0.0318 1.0000 Uani . N2 N 0.7717(19) 0.0212(15) 0.7363(9) 0.0325 1.0000 Uani . C1 C 0.959(2) 0.4609(17) 0.7693(11) 0.0304 1.0000 Uani . C2 C 0.9608(18) 0.2794(16) 0.7380(7) 0.0261 1.0000 Uani . C3 C 0.790(2) 0.1914(17) 0.7743(9) 0.0284 1.0000 Uani . F1 F 1.5714(9) 0.0514(8) 0.5497(5) 0.0164 1.0000 Uani . F2 F 1.4529(9) 0.5200(8) 1.0503(5) 0.0153 1.0000 Uani . O4 O 0.8335(12) 0.5967(9) 0.4409(6) 0.0184 1.0000 Uani . O5 O 0.7412(11) 0.345(1) 0.5160(6) 0.0169 1.0000 Uani . O6 O 0.9145(14) 0.3392(12) 0.3741(7) 0.0295 1.0000 Uani . O7 O 1.3872(12) 0.335(1) 0.8752(5) 0.0165 1.0000 Uani . O8 O 1.3925(13) 0.1831(11) 1.1060(7) 0.0260 1.0000 Uani . O9 O 1.0797(13) 0.3835(11) 0.9998(6) 0.0221 1.0000 Uani . O10 O 0.8488(12) 0.563(1) 1.0661(6) 0.0192 1.0000 Uani . O11 O 0.7388(12) 0.2971(11) 1.0046(5) 0.0215 1.0000 Uani . O12 O 0.9556(13) 0.3190(11) 1.1487(6) 0.0250 1.0000 Uani . O13 O 0.6117(16) 0.466(2) 0.2460(7) 0.0473 1.0000 Uani . O1 O 1.3615(12) 0.229(1) 0.3974(5) 0.0168 1.0000 Uani . O2 O 1.4277(12) 0.359(1) 0.6361(5) 0.0163 1.0000 Uani . O3 O 1.0825(11) 0.427(1) 0.5183(6) 0.0158 1.0000 Uani . U1 U 1.39674(5) 0.29304(13) 0.51648(3) 0.0118 1.0000 Uani . U2 U 1.39130(5) 0.25925(13) 0.99169(3) 0.0125 1.0000 Uani . S1 S 0.8918(4) 0.4245(3) 0.46067(18) 0.0129 1.0000 Uani . S2 S 0.9056(4) 0.3891(3) 1.05670(19) 0.0141 1.0000 Uani . H13 H 0.6512 0.4899 0.1815 0.0569 1.0000 Uiso . H14 H 0.6798 0.5461 0.2908 0.0569 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 N1 0.033(6) 0.030(6) 0.036(7) 0.011(5) 0.022(5) 0.014(5) N2 0.037(7) 0.030(6) 0.028(6) -0.007(5) -0.009(5) 0.004(5) C1 0.032(7) 0.027(7) 0.033(7) 0.001(5) 0.012(6) 0.008(5) C2 0.033(6) 0.026(6) 0.020(5) -0.008(5) 0.005(4) 0.010(5) C3 0.029(7) 0.033(7) 0.022(6) -0.013(5) -0.004(5) 0.013(5) F1 0.009(3) 0.016(3) 0.024(3) -0.001(2) 0.000(2) -0.001(2) F2 0.009(3) 0.014(3) 0.023(3) -0.002(2) 0.002(2) 0.004(2) O4 0.018(4) 0.015(4) 0.022(4) 0.002(3) 0.001(3) -0.000(3) O5 0.010(4) 0.018(4) 0.023(4) 0.012(3) 0.002(3) -0.002(3) O6 0.027(5) 0.026(5) 0.035(5) -0.010(4) 0.002(4) 0.011(4) O7 0.018(4) 0.017(4) 0.015(3) -0.001(3) 0.005(3) -0.004(3) O8 0.018(4) 0.015(4) 0.045(6) 0.013(4) 0.006(4) 0.000(3) O9 0.017(4) 0.025(4) 0.027(4) -0.002(3) 0.016(3) 0.004(3) O10 0.012(4) 0.017(4) 0.029(4) -0.005(3) 0.000(3) 0.006(3) O11 0.022(4) 0.017(4) 0.026(4) -0.004(3) 0.006(3) -0.005(3) O12 0.022(4) 0.028(4) 0.026(4) 0.007(3) 0.006(3) -0.005(3) O13 0.031(6) 0.08(1) 0.028(6) 0.001(5) 0.005(5) 0.006(5) O1 0.019(4) 0.019(4) 0.011(3) -0.002(3) -0.004(3) 0.003(3) O2 0.018(4) 0.029(4) 0.002(3) 0.002(3) -0.000(3) 0.002(3) O3 0.003(3) 0.018(4) 0.026(4) -0.000(3) -0.002(3) 0.002(3) U1 0.00957(18) 0.0117(2) 0.01438(19) -0.00027(12) 0.00139(11) -0.00024(12) U2 0.01016(18) 0.0126(2) 0.01474(19) 0.00008(13) 0.00182(11) -0.00028(13) S1 0.0101(11) 0.0119(11) 0.0169(12) -0.0003(8) 0.0013(9) 0.0019(8) S2 0.0093(11) 0.0138(11) 0.0194(13) -0.0002(9) 0.0027(9) -0.0002(9) _refine_ls_extinction_coef 15.5(15) _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 H1 . C1 . 0.997 no H2 . C1 . 1.012 no H3 . C2 . 1.006 no H4 . C2 . 0.999 no H5 . C3 . 1.001 no H6 . C3 . 1.005 no H7 . N1 . 1.002 no H8 . N1 . 0.999 no H9 . N1 . 1.007 no H10 . N2 . 1.000 no H11 . N2 . 0.998 no H12 . N2 . 1.005 no N1 . C1 . 1.502(18) yes N2 . C3 . 1.495(17) yes C1 . C2 . 1.548(19) yes C2 . C3 . 1.49(2) yes F1 . U1 . 2.329(6) yes F1 . U1 2_846 2.329(6) yes F2 . U2 . 2.314(6) yes F2 . U2 2_857 2.321(6) yes O4 . U1 2_756 2.350(8) yes O4 . S1 . 1.481(8) yes O5 . U1 1_455 2.373(8) yes O5 . S1 . 1.489(7) yes O6 . S1 . 1.444(9) yes O7 . U2 . 1.782(8) yes O8 . U2 . 1.76(1) yes O9 . U2 . 2.353(8) yes O9 . S2 . 1.488(8) yes O10 . U2 2_757 2.383(8) yes O10 . S2 . 1.481(8) yes O11 . U2 1_455 2.367(8) yes O11 . S2 . 1.505(8) yes O12 . S2 . 1.455(9) yes O13 . H13 . 1.004 no O13 . H14 . 1.006 no O1 . U1 . 1.787(7) yes O2 . U1 . 1.797(7) yes O3 . U1 . 2.393(7) yes O3 . S1 . 1.478(8) 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 H7 . N1 . H8 . 109.439 no H7 . N1 . H9 . 108.806 no H8 . N1 . H9 . 109.043 no H7 . N1 . C1 . 110.140 no H8 . N1 . C1 . 109.632 no H9 . N1 . C1 . 109.759 no H10 . N2 . H11 . 109.570 no H10 . N2 . H12 . 109.076 no H11 . N2 . H12 . 109.239 no H10 . N2 . C3 . 109.821 no H11 . N2 . C3 . 109.670 no H12 . N2 . C3 . 109.447 no H1 . C1 . H2 . 108.710 no H1 . C1 . N1 . 109.668 no H2 . C1 . N1 . 109.081 no H1 . C1 . C2 . 109.875 no H2 . C1 . C2 . 108.689 no N1 . C1 . C2 . 110.8(11) yes H3 . C2 . H4 . 109.035 no H3 . C2 . C1 . 108.713 no H4 . C2 . C1 . 109.668 no H3 . C2 . C3 . 109.637 no H4 . C2 . C3 . 110.250 no C1 . C2 . C3 . 109.5(10) yes H5 . C3 . H6 . 108.933 no H5 . C3 . N2 . 109.226 no H6 . C3 . N2 . 109.250 no H5 . C3 . C2 . 109.215 no H6 . C3 . C2 . 108.720 no N2 . C3 . C2 . 111.5(11) yes U1 . F1 . U1 2_846 138.1(3) yes U2 . F2 . U2 2_857 138.7(3) yes U1 2_756 O4 . S1 . 140.3(5) yes U1 1_455 O5 . S1 . 142.7(5) yes U2 . O9 . S2 . 142.6(6) yes U2 2_757 O10 . S2 . 141.9(5) yes U2 1_455 O11 . S2 . 143.8(5) yes H13 . O13 . H14 . 108.613 no U1 . O3 . S1 . 136.7(5) yes F1 . U1 . F1 2_856 141.96(5) yes F1 . U1 . O4 2_746 73.0(3) yes F1 2_856 U1 . O4 2_746 143.9(3) yes F1 . U1 . O5 1_655 70.7(2) yes F1 2_856 U1 . O5 1_655 73.3(2) yes O4 2_746 U1 . O5 1_655 142.8(3) yes F1 . U1 . O1 . 88.5(3) yes F1 2_856 U1 . O1 . 83.4(3) yes O4 2_746 U1 . O1 . 90.4(3) yes O5 1_655 U1 . O1 . 96.2(3) yes F1 . U1 . O2 . 92.3(3) yes F1 2_856 U1 . O2 . 96.3(3) yes O4 2_746 U1 . O2 . 89.2(3) yes O5 1_655 U1 . O2 . 84.7(3) yes O1 . U1 . O2 . 178.9(4) yes F1 . U1 . O3 . 145.2(3) yes F1 2_856 U1 . O3 . 72.8(2) yes O4 2_746 U1 . O3 . 72.4(3) yes O5 1_655 U1 . O3 . 142.5(3) yes O1 . U1 . O3 . 95.3(3) yes O2 . U1 . O3 . 83.6(3) yes F2 . U2 . F2 2_847 142.66(6) yes F2 . U2 . O7 . 90.7(3) yes F2 2_847 U2 . O7 . 91.2(3) yes F2 . U2 . O8 . 89.9(4) yes F2 2_847 U2 . O8 . 88.7(4) yes O7 . U2 . O8 . 179.2(4) yes F2 . U2 . O9 . 73.9(3) yes F2 2_847 U2 . O9 . 143.4(3) yes O7 . U2 . O9 . 87.2(3) yes O8 . U2 . O9 . 92.5(4) yes F2 . U2 . O10 2_747 147.4(3) yes F2 2_847 U2 . O10 2_747 69.9(3) yes O7 . U2 . O10 2_747 86.9(3) yes O8 . U2 . O10 2_747 92.3(4) yes O9 . U2 . O10 2_747 73.5(3) yes F2 . U2 . O11 1_655 72.7(3) yes F2 2_847 U2 . O11 1_655 70.1(3) yes O7 . U2 . O11 1_655 88.2(3) yes O8 . U2 . O11 1_655 92.4(4) yes O9 . U2 . O11 1_655 146.2(3) yes O10 2_747 U2 . O11 1_655 139.6(3) yes O4 . S1 . O5 . 109.2(5) yes O4 . S1 . O6 . 109.7(5) yes O5 . S1 . O6 . 112.1(6) yes O4 . S1 . O3 . 107.7(5) yes O5 . S1 . O3 . 108.1(5) yes O6 . S1 . O3 . 109.9(5) yes O9 . S2 . O10 . 107.6(5) yes O9 . S2 . O11 . 107.9(5) yes O10 . S2 . O11 . 109.5(5) yes O9 . S2 . O12 . 110.4(5) yes O10 . S2 . O12 . 109.8(5) yes O11 . S2 . O12 . 111.6(5) yes #===END