# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound_1 _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety '(C5 H5 Cl1 N1 1+)2, (U O3 C4 H2 N4 S4 2-)' _chemical_formula_sum 'C14 H12 Cl2 N6 O3 S4 U' _exptl_crystal_recrystallization_method 'Slow Aqueous Evaporation' _chemical_melting_point ? _exptl_crystal_description Prism _exptl_crystal_colour Yellow _diffrn_ambient_temperature 100(2) _chemical_formula_weight 749.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.466(5) _cell_length_b 9.033(3) _cell_length_c 18.952(7) _cell_angle_alpha 90 _cell_angle_beta 95.102(5) _cell_angle_gamma 90 _cell_volume 2296.2(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4341 _cell_measurement_theta_min 5.425 _cell_measurement_theta_max 54.942 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.168 _exptl_crystal_F_000 1408 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.145 _exptl_crystal_size_mid 0.084 _exptl_crystal_size_min 0.062 _exptl_absorpt_coefficient_mu 7.694 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5832 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'SADABS, G. Sheldrick (1999)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focused sealed X-ray tube' _diffrn_source_type ? _diffrn_measurement_device_type 'Bruker ApexII CCD' _diffrn_measurement_method 'Omega and Phi Scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15404 _diffrn_reflns_av_unetI/netI 0.0544 _diffrn_reflns_av_R_equivalents 0.0773 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.158 _diffrn_reflns_theta_max 28.428 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 2874 _reflns_number_gt 2515 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'APEX II (Bruker AXS, 2013)' _computing_cell_refinement 'SAINT (Bruker AXS, 2013)' _computing_data_reduction 'SAINT (Bruker AXS, 2013)' _computing_structure_solution 'SIR92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Crystal Maker v.8.2.2 (Palmer 2009)' _computing_publication_material 'WINGX (Farrugia, 2012)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0110P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 2874 _refine_ls_number_parameters 141 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0561 _refine_ls_wR_factor_gt 0.0541 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.5000 0.43072(2) 0.2500 0.01122(7) Uani 1 2 d S T P . . Cl1 Cl 0.30380(8) 0.14580(12) 0.34385(6) 0.0231(2) Uani 1 1 d . . . . . S1 S 0.37731(9) 0.62911(12) -0.00214(6) 0.0211(2) Uani 1 1 d . . . . . OW1 O 0.5000 0.7056(5) 0.2500 0.0199(10) Uani 1 2 d S T P . . S2 S 0.38059(8) -0.06884(12) 0.13808(5) 0.0212(2) Uani 1 1 d . . . . . O1 O 0.3783(2) 0.4325(3) 0.27823(14) 0.0157(6) Uani 1 1 d . . . . . N1 N 0.4381(3) 0.5254(3) 0.13290(18) 0.0143(7) Uani 1 1 d . . . . . N2 N 0.4489(3) 0.2126(4) 0.18027(18) 0.0193(8) Uani 1 1 d . . . . . N3 N 0.3579(3) -0.2982(4) 0.43607(19) 0.0222(8) Uani 1 1 d . . . . . H3 H 0.3688 -0.3848 0.4540 0.027 Uiso 1 1 calc R U . . . C1 C 0.4135(3) 0.5673(5) 0.0778(2) 0.0165(8) Uani 1 1 d . . . . . C2 C 0.4219(3) 0.0944(4) 0.1639(2) 0.0164(9) Uani 1 1 d . . . . . C3 C 0.3231(3) -0.2876(5) 0.3694(2) 0.0215(9) Uani 1 1 d . . . . . H3A H 0.3106 -0.3730 0.3427 0.026 Uiso 1 1 calc R U . . . C4 C 0.3048(3) -0.1508(5) 0.3386(2) 0.0196(9) Uani 1 1 d . . . . . H4 H 0.2804 -0.1424 0.2913 0.023 Uiso 1 1 calc R U . . . C5 C 0.3241(3) -0.0261(5) 0.3806(2) 0.0172(9) Uani 1 1 d . . . . . C6 C 0.3599(3) -0.0400(5) 0.4511(2) 0.0208(10) Uani 1 1 d . . . . . H6 H 0.3719 0.0431 0.4796 0.025 Uiso 1 1 calc R U . . . C7 C 0.3772(4) -0.1785(5) 0.4776(2) 0.0261(11) Uani 1 1 d . . . . . H7 H 0.4024 -0.1908 0.5245 0.031 Uiso 1 1 calc R U . . . OWH1 H 0.530(4) 0.768(5) 0.282(2) 0.031(14) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.01188(11) 0.00780(10) 0.01402(10) 0.000 0.00130(7) 0.000 Cl1 0.0233(6) 0.0178(5) 0.0283(6) 0.0061(5) 0.0031(5) -0.0007(4) S1 0.0292(6) 0.0141(5) 0.0187(5) -0.0008(4) -0.0042(5) 0.0020(5) OW1 0.032(3) 0.008(2) 0.019(2) 0.000 -0.003(2) 0.000 S2 0.0296(6) 0.0109(5) 0.0217(5) -0.0016(5) -0.0062(4) -0.0025(5) O1 0.0158(14) 0.0138(14) 0.0177(13) 0.0008(12) 0.0034(11) -0.0014(12) N1 0.0147(18) 0.0086(16) 0.0200(18) 0.0025(14) 0.0040(14) 0.0019(13) N2 0.019(2) 0.0152(18) 0.0240(19) -0.0027(16) 0.0016(15) 0.0005(15) N3 0.021(2) 0.0161(19) 0.030(2) 0.0025(16) 0.0075(16) 0.0053(16) C1 0.017(2) 0.0093(18) 0.023(2) -0.0040(19) 0.0041(16) 0.0021(18) C2 0.018(2) 0.015(2) 0.016(2) -0.0009(16) 0.0026(16) 0.0006(17) C3 0.016(2) 0.018(2) 0.031(2) -0.008(2) 0.0032(18) 0.0018(18) C4 0.016(2) 0.024(2) 0.019(2) -0.0044(18) 0.0000(17) 0.0029(18) C5 0.013(2) 0.018(2) 0.022(2) 0.0015(17) 0.0066(17) 0.0022(16) C6 0.028(2) 0.018(2) 0.017(2) -0.0047(17) 0.0025(18) 0.0010(18) C7 0.034(3) 0.024(3) 0.021(2) 0.0000(19) 0.006(2) 0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O1 1.769(3) . ? U1 O1 1.769(3) 2_655 ? U1 N2 2.437(4) 2_655 ? U1 N2 2.437(4) . ? U1 N1 2.454(3) 2_655 ? U1 N1 2.454(3) . ? U1 OW1 2.483(4) . ? Cl1 C5 1.713(4) . ? S1 C1 1.647(4) . ? OW1 OWH1 0.91(4) . ? S2 C2 1.635(4) . ? N1 C1 1.132(5) . ? N2 C2 1.161(5) . ? N3 C3 1.311(6) . ? N3 C7 1.349(6) . ? N3 H3 0.8600 . ? C3 C4 1.379(6) . ? C3 H3A 0.9300 . ? C4 C5 1.391(6) . ? C4 H4 0.9300 . ? C5 C6 1.386(6) . ? C6 C7 1.361(6) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 U1 O1 178.98(18) . 2_655 ? O1 U1 N2 93.89(12) . 2_655 ? O1 U1 N2 86.94(12) 2_655 2_655 ? O1 U1 N2 86.94(12) . . ? O1 U1 N2 93.88(12) 2_655 . ? N2 U1 N2 72.12(17) 2_655 . ? O1 U1 N1 88.45(12) . 2_655 ? O1 U1 N1 91.20(12) 2_655 2_655 ? N2 U1 N1 74.61(11) 2_655 2_655 ? N2 U1 N1 146.00(11) . 2_655 ? O1 U1 N1 91.20(12) . . ? O1 U1 N1 88.45(12) 2_655 . ? N2 U1 N1 145.99(11) 2_655 . ? N2 U1 N1 74.61(11) . . ? N1 U1 N1 139.19(15) 2_655 . ? O1 U1 OW1 89.49(9) . . ? O1 U1 OW1 89.49(9) 2_655 . ? N2 U1 OW1 143.94(8) 2_655 . ? N2 U1 OW1 143.94(8) . . ? N1 U1 OW1 69.60(8) 2_655 . ? N1 U1 OW1 69.60(8) . . ? U1 OW1 OWH1 129(3) . . ? C1 N1 U1 176.9(3) . . ? C2 N2 U1 162.7(3) . . ? C3 N3 C7 122.5(4) . . ? C3 N3 H3 118.8 . . ? C7 N3 H3 118.8 . . ? N1 C1 S1 179.6(4) . . ? N2 C2 S2 177.5(4) . . ? N3 C3 C4 120.6(4) . . ? N3 C3 H3A 119.7 . . ? C4 C3 H3A 119.7 . . ? C3 C4 C5 117.8(4) . . ? C3 C4 H4 121.1 . . ? C5 C4 H4 121.1 . . ? C6 C5 C4 120.6(4) . . ? C6 C5 Cl1 120.2(3) . . ? C4 C5 Cl1 119.1(3) . . ? C7 C6 C5 118.2(4) . . ? C7 C6 H6 120.9 . . ? C5 C6 H6 120.9 . . ? N3 C7 C6 120.3(4) . . ? N3 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 N3 C3 C4 0.2(7) . . . . ? N3 C3 C4 C5 -0.3(6) . . . . ? C3 C4 C5 C6 -0.3(6) . . . . ? C3 C4 C5 Cl1 179.2(3) . . . . ? C4 C5 C6 C7 1.0(6) . . . . ? Cl1 C5 C6 C7 -178.5(3) . . . . ? C3 N3 C7 C6 0.6(7) . . . . ? C5 C6 C7 N3 -1.2(7) . . . . ? _refine_diff_density_max 0.781 _refine_diff_density_min -1.041 _refine_diff_density_rms 0.164 _shelxl_version_number 2013-4 _shelx_res_file ; TITL Cc in Cc New: C2/c CELL 0.71073 13.4660 9.0330 18.9520 90.000 95.102 90.000 ZERR 4.00 0.0050 0.0030 0.0070 0.000 0.005 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C CL N O S U H UNIT 56 8 24 12 16 4 48 MERG 2 FMAP 2 PLAN 20 ACTA 50.00 HTAB BOND $H CONF L.S. 12 WGHT 0.011000 FVAR 0.03845 U1 6 0.500000 0.430722 0.250000 10.50000 0.01188 0.00780 = 0.01402 0.00000 0.00130 0.00000 CL1 2 0.303796 0.145802 0.343855 11.00000 0.02329 0.01779 = 0.02828 0.00607 0.00307 -0.00068 S1 5 0.377312 0.629115 -0.002135 11.00000 0.02924 0.01415 = 0.01874 -0.00083 -0.00425 0.00195 OW1 4 0.500000 0.705648 0.250000 10.50000 0.03225 0.00769 = 0.01887 0.00000 -0.00258 0.00000 S2 5 0.380590 -0.068838 0.138076 11.00000 0.02959 0.01088 = 0.02174 -0.00161 -0.00623 -0.00254 O1 4 0.378288 0.432466 0.278235 11.00000 0.01576 0.01381 = 0.01775 0.00083 0.00341 -0.00137 N1 3 0.438057 0.525447 0.132901 11.00000 0.01471 0.00860 = 0.02001 0.00250 0.00402 0.00190 N2 3 0.448886 0.212601 0.180269 11.00000 0.01877 0.01520 = 0.02398 -0.00267 0.00161 0.00051 N3 3 0.357856 -0.298227 0.436067 11.00000 0.02130 0.01614 = 0.03001 0.00255 0.00753 0.00526 AFIX 43 H3 7 0.368786 -0.384791 0.453992 11.00000 -1.20000 AFIX 0 C1 1 0.413472 0.567303 0.077793 11.00000 0.01707 0.00932 = 0.02339 -0.00404 0.00410 0.00213 C2 1 0.421938 0.094366 0.163893 11.00000 0.01817 0.01482 = 0.01630 -0.00091 0.00257 0.00057 C3 1 0.323057 -0.287564 0.369425 11.00000 0.01610 0.01809 = 0.03057 -0.00768 0.00321 0.00181 AFIX 43 H3A 7 0.310562 -0.372985 0.342709 11.00000 -1.20000 AFIX 0 C4 1 0.304811 -0.150843 0.338576 11.00000 0.01586 0.02384 = 0.01875 -0.00445 0.00003 0.00289 AFIX 43 H4 7 0.280439 -0.142363 0.291274 11.00000 -1.20000 AFIX 0 C5 1 0.324074 -0.026066 0.380569 11.00000 0.01297 0.01774 = 0.02193 0.00154 0.00662 0.00219 C6 1 0.359937 -0.039965 0.451106 11.00000 0.02762 0.01820 = 0.01677 -0.00474 0.00249 0.00104 AFIX 43 H6 7 0.371902 0.043134 0.479567 11.00000 -1.20000 AFIX 0 C7 1 0.377151 -0.178535 0.477558 11.00000 0.03368 0.02446 = 0.02074 0.00003 0.00598 0.00443 AFIX 43 H7 7 0.402353 -0.190769 0.524492 11.00000 -1.20000 AFIX 0 OWH1 7 0.530105 0.768438 0.282483 11.00000 0.03095 HKLF 4 REM Cc in Cc New: C2/c REM R1 = 0.0281 for 2515 Fo > 4sig(Fo) and 0.0354 for all 2874 data REM 141 parameters refined using 0 restraints END WGHT 0.0110 0.0000 REM Instructions for potential hydrogen bonds EQIV $1 x, -y, z+1/2 HTAB N3 S1_$1 EQIV $2 x, y-1, z HTAB C3 O1_$2 EQIV $3 -x+1/2, y-1/2, -z+1/2 HTAB C4 O1_$3 EQIV $4 x, -y+1, z+1/2 HTAB C6 S1_$4 HTAB C6 S2_$1 EQIV $5 -x+1, y+1, -z+1/2 HTAB OW1 S2_$5 REM Highest difference peak 0.781, deepest hole -1.041, 1-sigma level 0.164 Q1 1 0.4211 0.4903 0.1016 11.00000 0.05 0.78 Q2 1 0.5458 0.5551 0.2595 11.00000 0.05 0.71 Q3 1 0.3316 0.0678 0.3446 11.00000 0.05 0.69 Q4 1 0.4203 0.2337 0.2416 11.00000 0.05 0.64 Q5 1 0.5010 0.4934 0.3118 11.00000 0.05 0.63 Q6 1 0.4227 -0.2283 0.5391 11.00000 0.05 0.62 Q7 1 0.3895 0.0313 0.1372 11.00000 0.05 0.60 Q8 1 0.4448 0.4543 0.1911 11.00000 0.05 0.59 Q9 1 0.6234 0.7819 0.2677 11.00000 0.05 0.58 Q10 1 0.4509 0.4590 0.1422 11.00000 0.05 0.58 Q11 1 0.4013 0.3718 0.2257 11.00000 0.05 0.56 Q12 1 0.3525 -0.0709 0.4065 11.00000 0.05 0.56 Q13 1 0.4163 0.5774 0.1380 11.00000 0.05 0.54 Q14 1 0.3258 0.5290 -0.0060 11.00000 0.05 0.53 Q15 1 0.3080 0.1431 0.2731 11.00000 0.05 0.52 Q16 1 0.4464 0.3185 0.2623 11.00000 0.05 0.51 Q17 1 0.3746 0.4269 0.3146 11.00000 0.05 0.51 Q18 1 0.4188 0.4927 0.2711 11.00000 0.05 0.50 Q19 1 0.5977 0.8963 0.2531 11.00000 0.05 0.50 Q20 1 0.4397 0.6525 0.0425 11.00000 0.05 0.50 ; _shelx_res_checksum 74462 _shelx_hkl_file ; 2 0 0 127.23 6.87 -2 0 0 124.57 7.37 2 0 0 120.11 6.71 2 0 0 118.07 6.99 4 0 0 10.25 1.06 -4 0 0 8.17 0.95 4 0 0 7.30 0.89 -6 0 0 117.63 7.63 6 0 0 113.91 7.16 6 0 0 125.25 7.27 -8 0 0 104.07 6.50 8 0 0 87.81 6.05 8 0 0 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9 42.83 3.14 -1 3 9 38.85 3.24 1 3 -9 45.45 3.09 1 -3 9 83.25 5.69 1 -3 9 79.61 6.07 -1 -3 -9 93.83 5.65 -1 -3 -9 95.32 5.38 1 3 9 80.72 5.73 -1 3 -9 83.61 5.40 1 3 9 79.99 5.49 -3 -3 -9 113.52 7.84 3 -3 9 134.89 8.24 3 -3 9 131.12 8.85 3 -3 9 131.63 7.16 3 3 9 133.17 8.02 3 3 9 135.81 8.27 -3 3 -9 114.51 7.69 3 3 9 135.01 7.94 -5 -3 -9 70.91 4.38 5 -3 9 58.44 4.63 5 -3 9 63.98 3.93 -5 -3 -9 56.22 4.37 -5 3 -9 61.44 4.14 5 3 9 65.38 4.60 5 3 9 61.99 4.27 7 -3 9 14.77 2.23 7 -3 9 8.28 1.32 -7 -3 -9 7.72 1.50 -7 -3 -9 8.06 1.29 -7 3 -9 13.23 1.31 -7 3 -9 15.25 2.22 7 3 9 11.73 1.96 7 3 9 9.31 1.39 -9 -3 -9 35.18 2.87 -9 -3 -9 38.24 3.28 9 -3 9 27.99 2.79 9 -3 9 31.77 3.35 9 3 9 39.46 3.48 -9 3 -9 27.70 3.18 11 -3 9 48.78 4.57 -11 -3 -9 55.79 4.46 11 -3 9 48.74 4.19 11 3 9 53.19 4.60 -11 3 -9 48.27 4.66 -13 -3 -9 23.91 3.43 13 -3 9 29.67 3.91 -13 3 -9 23.99 3.54 13 3 9 29.53 3.97 15 -3 9 7.45 2.24 -15 -3 -9 14.93 2.80 15 3 9 13.06 2.84 -15 3 -9 7.74 2.23 16 -4 -9 27.63 3.98 16 4 -9 23.62 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11.34 3.24 -3 -5 -21 7.93 2.28 3 5 21 12.50 2.63 -3 5 -21 10.17 2.21 -5 -5 -21 7.53 2.16 5 -5 21 10.70 2.63 5 5 21 7.07 1.99 -5 5 -21 5.52 2.05 6 -6 -21 0.04 1.55 -6 6 21 0.31 1.28 -4 -6 21 7.22 2.56 4 -6 -21 5.19 2.01 -4 6 21 6.28 2.10 4 6 -21 6.83 2.02 2 -6 -21 9.72 2.40 -2 -6 21 12.78 3.14 2 6 -21 6.29 1.92 -2 6 21 11.80 2.72 0 -6 -21 2.71 1.66 0 -6 21 1.89 1.89 0 -6 21 3.40 1.89 0 6 21 3.97 1.69 0 6 -21 3.10 1.49 2 -6 21 -0.02 1.44 -2 -6 -21 -0.66 1.25 2 -6 21 -0.14 1.64 2 6 21 0.53 1.26 -2 6 -21 0.73 1.26 10 0 -22 22.36 3.22 -10 0 22 18.78 4.09 -8 0 22 5.81 2.51 8 0 -22 3.27 1.54 -6 0 22 23.54 4.03 6 0 -22 24.85 2.94 -4 0 22 38.01 4.89 4 0 -22 41.85 3.88 2 0 -22 5.68 1.55 -2 0 22 8.65 2.47 0 0 -22 8.55 1.87 0 0 22 8.75 2.61 2 0 22 10.19 2.78 -2 0 -22 19.55 2.68 -4 0 -22 51.45 4.36 4 0 22 51.91 5.59 -6 0 -22 24.54 3.59 -9 -1 22 9.16 2.95 9 -1 -22 14.90 2.59 -9 1 22 16.19 3.60 9 1 -22 13.89 2.58 -7 -1 22 18.61 3.76 7 -1 -22 22.67 2.75 7 -1 -22 23.25 3.11 7 1 -22 22.56 3.25 5 -1 -22 16.45 2.50 -5 -1 22 11.47 2.93 5 -1 -22 12.45 2.03 -5 1 22 12.28 3.08 5 1 -22 8.64 2.00 3 -1 -22 18.99 2.53 -3 -1 22 18.81 3.64 3 -1 -22 15.83 2.59 -3 1 22 16.34 3.44 3 1 -22 16.32 2.53 1 -1 -22 11.98 1.91 1 -1 -22 9.49 1.95 -1 -1 22 10.64 2.78 -1 1 22 9.18 2.48 1 1 -22 9.93 1.99 -1 -1 -22 10.69 1.98 -1 -1 -22 13.76 1.99 1 -1 22 13.60 3.02 -1 1 -22 11.90 2.15 1 1 22 12.00 2.87 -3 -1 -22 26.96 2.85 3 -1 22 26.77 4.36 -3 -1 -22 19.94 2.50 3 1 22 19.71 3.67 -3 1 -22 25.96 2.88 -5 -1 -22 9.12 1.68 -5 -1 -22 7.40 1.74 -7 -1 -22 12.36 2.51 7 -1 22 21.20 3.35 -7 1 -22 12.41 2.51 8 -2 -22 4.37 1.54 -8 -2 22 4.07 2.14 8 -2 -22 2.92 1.55 8 -2 -22 3.00 1.44 8 2 -22 1.43 1.26 -8 2 22 3.12 2.19 -6 -2 22 4.00 2.31 6 -2 -22 5.86 1.84 6 -2 -22 7.98 1.90 6 -2 -22 6.72 1.56 6 2 -22 4.93 1.75 -6 2 22 6.58 2.50 4 -2 -22 12.05 2.31 -4 -2 22 11.44 2.97 4 -2 -22 13.16 2.13 4 2 -22 8.01 2.00 -4 2 22 13.55 3.08 2 -2 -22 9.51 2.06 2 -2 -22 10.88 1.89 -2 -2 22 9.85 2.76 -2 2 22 4.53 2.13 2 2 -22 11.73 2.17 0 -2 -22 2.05 1.18 0 -2 22 1.73 1.86 0 -2 -22 2.16 0.98 0 2 22 2.79 1.77 0 2 -22 1.08 0.99 -2 -2 -22 6.70 1.51 -2 -2 -22 6.21 1.71 2 -2 22 6.78 2.42 -2 2 -22 7.00 1.79 2 2 22 3.90 1.90 -4 -2 -22 13.21 2.23 4 -2 22 20.71 3.72 -4 -2 -22 11.99 1.86 4 2 22 11.10 2.79 -4 2 -22 18.82 2.68 6 -2 22 6.29 2.05 -6 2 -22 4.59 1.83 9 -3 -22 7.75 1.99 9 -3 -22 5.65 2.05 -9 -3 22 5.75 2.56 9 -3 -22 11.39 2.06 9 3 -22 6.37 1.93 -9 3 22 4.87 2.58 7 -3 -22 0.77 1.00 -7 -3 22 -1.13 1.47 7 -3 -22 0.08 1.29 7 -3 -22 -0.18 1.05 -7 3 22 0.69 1.78 7 3 -22 -0.24 1.00 -5 -3 22 1.47 1.77 5 -3 -22 0.40 0.92 5 -3 -22 1.21 1.18 5 -3 -22 1.92 1.45 5 3 -22 0.40 1.05 -5 3 22 -0.13 1.51 -3 -3 22 -0.78 1.22 3 -3 -22 -0.56 1.04 3 3 -22 0.32 1.05 -3 3 22 -0.27 1.50 1 -3 -22 3.93 1.65 -1 -3 22 4.00 2.10 -1 3 22 4.19 1.68 1 3 -22 3.01 1.29 -1 3 22 0.99 1.52 1 -3 22 6.78 2.54 -1 -3 -22 2.95 1.53 -1 3 -22 5.11 1.60 1 3 22 4.61 1.74 1 3 22 4.49 1.99 3 -3 22 0.60 1.61 -3 3 -22 1.38 1.13 -5 -3 -22 1.08 1.05 -5 -3 -22 0.66 0.79 5 -3 22 1.14 1.35 -5 3 -22 1.28 1.44 8 -4 -22 4.34 2.01 -6 -4 22 -0.45 1.68 6 -4 -22 0.45 1.38 -6 4 22 -0.88 1.59 6 4 -22 0.00 1.11 -6 4 22 1.87 1.56 -4 -4 22 4.64 2.12 4 -4 -22 1.76 1.43 -4 4 22 1.42 1.72 -4 4 22 3.19 1.72 4 4 -22 2.09 1.48 2 -4 -22 0.60 1.20 -2 -4 22 -0.61 1.31 -2 4 22 -0.46 1.03 2 4 -22 -0.12 0.90 0 -4 -22 0.11 1.18 0 -4 22 1.24 1.70 0 4 -22 0.91 1.12 0 4 22 1.27 1.26 2 -4 22 0.61 1.56 -2 -4 -22 0.29 1.16 2 4 22 0.58 1.17 -2 4 -22 1.27 1.10 4 -4 22 0.58 1.41 -4 -4 -22 2.89 1.71 -4 4 -22 2.37 1.37 4 4 22 1.49 1.25 5 -5 -22 5.14 2.04 -5 -5 22 5.60 2.46 5 5 -22 6.46 2.10 -5 5 22 7.80 2.14 3 -5 -22 5.17 2.12 -3 -5 22 7.07 2.50 3 5 -22 4.37 1.85 -3 5 22 4.68 1.86 -1 -5 22 1.59 1.70 1 -5 -22 2.80 1.68 1 5 -22 1.37 1.27 -1 5 22 1.17 1.32 -1 -5 -22 3.85 1.94 1 -5 22 4.26 2.27 1 5 22 3.00 1.72 -1 5 -22 1.99 1.31 3 -5 22 2.06 2.00 3 -5 22 3.10 1.73 -3 -5 -22 2.79 1.69 3 5 22 5.62 1.86 -3 5 -22 5.07 1.79 2 -6 -22 18.98 3.58 -2 6 22 18.20 3.29 8 0 -23 -0.54 0.91 -8 0 23 0.71 1.95 -6 0 23 -0.01 1.36 6 0 -23 -0.03 0.89 -4 0 23 1.69 1.78 4 0 -23 0.32 0.87 2 0 -23 -0.33 0.82 -2 0 23 0.31 1.56 0 0 -23 0.74 0.93 0 0 23 0.33 1.51 -2 0 -23 -0.43 0.73 2 0 23 0.81 1.64 4 0 23 -0.69 1.41 -4 0 -23 -0.40 0.88 -6 0 -23 -0.53 0.84 -7 -1 23 0.80 1.59 7 -1 -23 -0.97 0.87 7 -1 -23 0.68 1.07 7 1 -23 -0.01 1.05 -7 1 23 1.06 1.80 -5 -1 23 0.93 1.72 5 -1 -23 0.06 0.84 5 -1 -23 0.07 0.97 5 1 -23 0.41 1.07 -5 1 23 -0.58 1.44 -3 -1 23 6.54 2.37 3 -1 -23 7.25 1.78 3 -1 -23 5.85 1.51 -3 1 23 3.05 2.04 3 1 -23 8.08 1.93 1 -1 -23 3.38 1.24 -1 -1 23 2.93 2.13 1 -1 -23 5.08 1.53 -1 1 23 3.65 1.89 1 1 -23 1.62 1.21 -1 -1 -23 2.17 1.09 -1 -1 -23 1.86 1.03 1 -1 23 2.16 1.81 -1 1 -23 1.42 1.06 1 1 23 1.41 1.78 -3 -1 -23 0.51 0.87 -3 -1 -23 -0.61 0.74 3 -1 23 0.25 1.46 3 1 23 0.16 1.35 -3 1 -23 -0.15 0.97 8 -2 -23 3.66 1.41 8 -2 -23 3.76 1.55 -8 -2 23 2.77 2.08 -8 2 23 3.20 2.36 8 2 -23 4.30 1.79 -6 -2 23 9.30 2.79 6 -2 -23 8.73 2.00 6 -2 -23 9.97 1.83 6 2 -23 9.38 2.13 -6 2 23 4.96 2.40 4 -2 -23 16.40 2.72 4 -2 -23 14.86 2.30 -4 -2 23 18.33 3.72 4 2 -23 14.95 2.73 -4 2 23 11.23 2.95 -2 -2 23 19.12 3.61 2 -2 -23 15.77 2.60 2 -2 -23 18.31 2.42 2 2 -23 25.33 3.32 -2 2 23 14.01 3.29 0 -2 -23 3.75 1.29 0 -2 -23 2.38 1.24 0 -2 23 -0.79 1.54 0 2 23 1.86 1.83 0 2 -23 1.50 1.14 -2 -2 -23 3.59 1.17 -2 -2 -23 1.27 1.01 2 -2 23 3.98 2.06 -2 2 -23 2.76 1.24 2 2 23 4.19 1.95 -4 -2 -23 23.03 3.09 -4 -2 -23 20.31 2.51 4 -2 23 15.07 3.51 -4 2 -23 19.01 2.91 7 -3 -23 11.74 2.01 -7 -3 23 9.27 3.08 7 -3 -23 10.92 2.34 7 -3 -23 10.34 2.45 -7 3 23 7.23 2.74 7 3 -23 9.71 2.23 -5 -3 23 11.10 3.19 5 -3 -23 11.35 2.03 5 -3 -23 10.95 2.36 5 -3 -23 14.10 2.70 -5 3 23 9.55 2.89 5 3 -23 10.95 2.32 3 -3 -23 24.55 2.88 3 -3 -23 30.37 3.35 -3 -3 23 24.32 4.33 -3 3 23 18.58 3.76 3 3 -23 23.08 3.29 -1 -3 23 24.58 4.22 -1 3 23 21.72 3.69 1 3 -23 29.11 3.24 1 -3 23 10.33 2.93 -1 3 -23 13.99 2.55 3 -3 23 2.85 2.19 -3 -3 -23 5.82 1.44 -3 -3 -23 6.39 1.77 -3 3 -23 4.06 1.51 6 -4 -23 10.83 2.62 -6 4 23 12.63 3.20 6 4 -23 18.76 2.99 -4 -4 23 32.26 5.00 4 -4 -23 37.27 4.04 -4 4 23 30.48 4.25 4 4 -23 25.47 3.71 2 -4 -23 14.45 2.88 -2 -4 23 12.40 3.22 -2 4 23 11.06 2.64 2 4 -23 13.00 2.51 0 -4 23 6.88 2.59 0 -4 -23 6.79 2.17 0 4 23 8.69 2.34 0 4 -23 6.54 1.96 2 -4 23 13.59 3.40 -2 -4 -23 11.66 2.65 -2 4 -23 14.20 2.53 2 4 23 12.43 2.67 -3 5 23 2.63 1.75 1 -5 -23 12.98 2.89 -1 -5 23 7.93 2.82 -1 5 23 13.94 2.82 1 5 -23 15.11 2.87 -6 0 24 5.75 2.50 6 0 -24 7.03 1.98 -4 0 24 15.97 3.50 4 0 -24 12.02 2.34 -2 0 24 9.73 2.86 2 0 -24 12.53 2.32 0 0 -24 23.40 3.24 0 0 24 27.10 4.38 -2 0 -24 20.17 3.03 2 0 24 20.02 3.74 4 0 24 7.91 2.71 -4 0 -24 8.13 1.91 -7 -1 24 9.67 2.88 7 -1 -24 8.76 2.23 -7 1 24 8.48 2.83 7 1 -24 11.20 2.41 -5 -1 24 4.85 2.24 5 -1 -24 3.41 1.41 5 -1 -24 2.41 1.40 5 1 -24 3.38 1.48 -5 1 24 2.77 2.07 3 -1 -24 14.08 2.27 3 -1 -24 11.03 2.27 -3 -1 24 10.83 3.11 -3 1 24 13.87 3.32 3 1 -24 14.94 2.60 -1 -1 24 28.00 4.67 1 -1 -24 31.75 2.96 1 -1 -24 31.26 3.35 -1 1 24 27.41 4.35 1 1 -24 32.77 3.52 1 -1 24 4.53 2.16 -1 -1 -24 7.58 1.79 -1 -1 -24 5.97 1.49 1 1 24 7.02 2.32 -1 1 -24 7.38 1.85 -3 -1 -24 6.19 1.73 3 -1 24 5.75 2.52 -3 -1 -24 3.63 1.26 -3 1 -24 7.14 1.90 3 1 24 4.26 2.08 6 -2 -24 8.32 1.87 -6 -2 24 6.24 2.63 6 -2 -24 7.17 1.91 -6 2 24 5.34 2.39 6 2 -24 3.38 1.58 4 -2 -24 4.50 1.64 4 -2 -24 2.13 1.10 -4 -2 24 0.42 1.78 4 2 -24 6.24 1.91 -4 2 24 4.38 2.31 -2 -2 24 3.10 2.18 2 -2 -24 4.76 1.61 2 -2 -24 6.13 1.53 2 2 -24 3.87 1.59 -2 2 24 2.62 2.02 0 -2 -24 3.88 1.48 0 -2 24 7.11 2.55 0 -2 -24 7.09 1.56 0 2 24 7.18 2.47 0 2 -24 6.87 1.91 2 -2 24 2.28 1.95 -2 -2 -24 5.45 1.68 -2 -2 -24 6.97 1.55 -2 2 -24 7.91 1.87 2 2 24 4.26 2.14 5 -3 -24 0.16 1.07 5 -3 -24 -0.06 1.17 -5 3 24 3.02 2.30 5 3 -24 0.72 1.30 3 -3 -24 2.61 1.44 3 -3 -24 3.24 1.25 -3 -3 24 0.59 1.76 3 3 -24 2.17 1.36 -3 3 24 2.35 2.02 -1 -3 24 1.31 1.99 1 -3 -24 -0.01 0.93 1 -3 -24 0.60 0.89 -1 3 24 -0.50 1.39 1 3 -24 2.88 1.45 -1 -3 -24 0.11 1.07 1 -3 24 3.51 2.15 -1 -3 -24 -0.32 0.85 -1 3 -24 1.62 1.26 4 0 -25 -1.02 0.97 -4 0 25 1.10 1.96 -2 0 25 -1.65 1.58 2 0 -25 -0.44 1.02 0 0 25 1.41 1.79 0 0 -25 -0.06 0.94 3 -1 -25 1.46 1.12 -3 -1 25 0.87 1.89 3 -1 -25 0.42 1.12 3 1 -25 1.19 1.40 -3 1 25 1.33 1.94 1 -1 -25 0.67 1.06 1 -1 -25 0.69 0.99 -1 -1 25 1.55 1.96 -1 1 25 -0.26 1.60 1 1 -25 -0.52 0.97 -1 -1 -25 4.63 1.42 2 -2 -25 -0.48 0.90 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 30014 _symmetry_cell_setting monoclinic _symmetry_space_group_name_h-m 'C 2/c' _symmetry_int_tables_number 15 _chemical_absolute_configuration ? _database_code_depnum_ccdc_archive 'CCDC 967154' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound_2 _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety '(C5 H5 N1 Br1 1+)2, (U1 O3 C4 H2 N4 S4 2-), (H2 O1)' _chemical_formula_sum 'C14 H14 Br2 N6 O4 S4 U' _chemical_properties_physical thermochromic _exptl_crystal_recrystallization_method 'Slow Aqueous Evaporation' _chemical_melting_point ? _exptl_crystal_description Prism _exptl_crystal_colour 'Orange (293(2)K) Yellow (100(2)K)' _diffrn_ambient_temperature 100(2) _chemical_formula_weight 857.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 57 _space_group_name_H-M_alt 'P b c m' _space_group_name_Hall '-P 2c 2b' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 6.4685(13) _cell_length_b 15.007(3) _cell_length_c 25.732(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2497.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8479 _cell_measurement_theta_min 5.429 _cell_measurement_theta_max 56.642 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.267 _exptl_crystal_F_000 1576 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.125 _exptl_crystal_size_mid 0.083 _exptl_crystal_size_min 0.080 _exptl_absorpt_coefficient_mu 10.064 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5276 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'SADABS, G. Sheldrick (1999)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focused sealed X-ray tube' _diffrn_measurement_device_type 'Bruker ApexII CCD' _diffrn_measurement_method 'Omega and Phi Scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 31174 _diffrn_reflns_av_unetI/netI 0.0274 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.715 _diffrn_reflns_theta_max 28.421 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 3212 _reflns_number_gt 2830 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'APEX II (Bruker AXS, 2013)' _computing_cell_refinement 'SAINT (Bruker AXS, 2013)' _computing_data_reduction 'SAINT (Bruker AXS, 2013)' _computing_structure_solution 'SIR92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Crystal Maker v.8.2.2 (Palmer 2009)' _computing_publication_material 'WINGX (Farrugia, 2012)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0225P)^2^+6.0525P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3212 _refine_ls_number_parameters 148 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0549 _refine_ls_wR_factor_gt 0.0526 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1534(6) 0.1950(2) 0.11925(14) 0.0163(7) Uani 1 1 d . . . . . C2 C 0.2729(5) -0.0690(2) 0.17645(13) 0.0150(7) Uani 1 1 d . . . . . C5 C 0.7811(6) 0.9455(3) 0.11350(16) 0.0242(8) Uani 1 1 d . . . . . H5 H 0.8186 0.8875 0.1220 0.029 Uiso 1 1 calc R U . . . C6 C 0.7766(6) 0.9717(3) 0.06246(16) 0.0254(9) Uani 1 1 d . . . . . H6 H 0.8086 0.9318 0.0360 0.030 Uiso 1 1 calc R U . . . C7 C 0.7232(6) 1.0587(3) 0.05120(14) 0.0210(8) Uani 1 1 d . . . . . C8 C 0.6736(6) 1.1183(3) 0.09088(15) 0.0208(7) Uani 1 1 d . . . . . H8 H 0.6375 1.1769 0.0834 0.025 Uiso 1 1 calc R U . . . C9 C 0.6793(6) 1.0883(3) 0.14101(15) 0.0204(7) Uani 1 1 d . . . . . H9 H 0.6467 1.1268 0.1681 0.024 Uiso 1 1 calc R U . . . N1 N 0.1327(5) 0.1826(2) 0.16407(12) 0.0203(7) Uani 1 1 d . . . . . N2 N 0.2512(5) 0.0011(2) 0.19408(13) 0.0233(7) Uani 1 1 d . . . . . N5 N 0.7315(5) 1.0037(2) 0.15134(12) 0.0201(7) Uani 1 1 d . . . . . H5A H 0.7335 0.9861 0.1831 0.024 Uiso 1 1 calc R U . . . O1 O -0.0948(5) 0.0870(2) 0.2500 0.0164(7) Uani 1 2 d S T P . . O2 O 0.4227(5) 0.1652(2) 0.2500 0.0188(8) Uani 1 2 d S T P . . OW1 O -0.0132(6) 0.2789(2) 0.2500 0.0191(8) Uani 1 2 d S T P . . OW2 O 0.2942(6) 0.4084(3) 0.2500 0.0238(8) Uani 1 2 d S T P . . S1 S 0.17640(18) 0.21257(7) 0.05792(4) 0.0283(2) Uani 1 1 d . . . . . S2 S 0.30732(19) -0.16806(7) 0.15214(4) 0.0326(3) Uani 1 1 d . . . . . Br1 Br 0.71268(6) 1.09859(3) -0.01801(2) 0.03017(10) Uani 1 1 d . . . . . U1 U 0.16381(3) 0.12640(2) 0.2500 0.01124(6) Uani 1 2 d S T P . . 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 0.0179(17) 0.0141(16) 0.0171(17) -0.0007(13) -0.0021(14) 0.0011(14) C2 0.0151(16) 0.0178(17) 0.0120(16) 0.0009(13) 0.0002(13) -0.0033(13) C5 0.0165(18) 0.0228(19) 0.033(2) -0.0085(17) -0.0071(16) 0.0030(15) C6 0.0169(18) 0.031(2) 0.029(2) -0.0113(17) -0.0008(16) 0.0024(16) C7 0.0165(17) 0.031(2) 0.0153(17) -0.0048(15) -0.0028(14) -0.0055(15) C8 0.0197(18) 0.0226(18) 0.0202(18) -0.0030(15) -0.0013(14) -0.0020(15) C9 0.0190(18) 0.0210(17) 0.0211(18) -0.0068(15) -0.0006(15) -0.0026(15) N1 0.0222(17) 0.0212(16) 0.0175(15) 0.0004(12) -0.0007(13) 0.0030(13) N2 0.0241(17) 0.0189(16) 0.0267(18) -0.0047(14) 0.0042(14) 0.0025(14) N5 0.0143(14) 0.0267(17) 0.0194(16) -0.0010(13) -0.0045(12) -0.0012(13) O1 0.0098(16) 0.0210(18) 0.0184(18) 0.000 0.000 0.0007(14) O2 0.0148(18) 0.0219(19) 0.0197(18) 0.000 0.000 -0.0008(15) OW1 0.027(2) 0.0150(18) 0.0155(18) 0.000 0.000 0.0059(15) OW2 0.021(2) 0.0220(19) 0.029(2) 0.000 0.000 0.0027(16) S1 0.0389(6) 0.0346(5) 0.0113(4) 0.0052(4) 0.0007(4) -0.0045(5) S2 0.0473(7) 0.0151(5) 0.0353(6) -0.0096(4) 0.0199(5) -0.0077(4) Br1 0.0277(2) 0.0448(2) 0.01800(19) -0.00475(17) 0.00107(15) -0.00916(18) U1 0.01233(9) 0.01125(9) 0.01014(9) 0.000 0.000 0.00078(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.176(5) . ? C1 S1 1.607(4) . ? C2 N2 1.155(4) . ? C2 S2 1.628(4) . ? C5 N5 1.347(5) . ? C5 C6 1.371(6) . ? C5 H5 0.9300 . ? C6 C7 1.382(6) . ? C6 H6 0.9300 . ? C7 C8 1.394(5) . ? C7 Br1 1.880(4) . ? C8 C9 1.367(5) . ? C8 H8 0.9300 . ? C9 N5 1.339(5) . ? C9 H9 0.9300 . ? N1 U1 2.375(3) . ? N2 U1 2.434(3) . ? N5 H5A 0.8600 . ? O1 U1 1.775(3) . ? O2 U1 1.773(4) . ? OW1 U1 2.559(3) . ? U1 N1 2.375(3) 6_556 ? U1 N2 2.434(3) 6_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 S1 178.7(4) . . ? N2 C2 S2 179.0(4) . . ? N5 C5 C6 120.1(4) . . ? N5 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C7 118.5(4) . . ? C5 C6 H6 120.8 . . ? C7 C6 H6 120.8 . . ? C6 C7 C8 120.6(4) . . ? C6 C7 Br1 120.6(3) . . ? C8 C7 Br1 118.8(3) . . ? C9 C8 C7 118.3(4) . . ? C9 C8 H8 120.9 . . ? C7 C8 H8 120.9 . . ? N5 C9 C8 120.4(3) . . ? N5 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C1 N1 U1 163.7(3) . . ? C2 N2 U1 164.7(3) . . ? C9 N5 C5 122.1(3) . . ? C9 N5 H5A 119.0 . . ? C5 N5 H5A 119.0 . . ? O2 U1 O1 179.71(16) . . ? O2 U1 N1 87.90(9) . . ? O1 U1 N1 92.20(9) . . ? O2 U1 N1 87.90(9) . 6_556 ? O1 U1 N1 92.20(9) . 6_556 ? N1 U1 N1 137.19(15) . 6_556 ? O2 U1 N2 91.96(12) . . ? O1 U1 N2 87.80(12) . . ? N1 U1 N2 75.14(11) . . ? N1 U1 N2 147.59(11) 6_556 . ? O2 U1 N2 91.96(12) . 6_556 ? O1 U1 N2 87.80(12) . 6_556 ? N1 U1 N2 147.60(11) . 6_556 ? N1 U1 N2 75.14(11) 6_556 6_556 ? N2 U1 N2 72.48(16) . 6_556 ? O2 U1 OW1 97.40(15) . . ? O1 U1 OW1 82.89(14) . . ? N1 U1 OW1 69.18(8) . . ? N1 U1 OW1 69.18(8) 6_556 . ? N2 U1 OW1 142.63(8) . . ? N2 U1 OW1 142.63(8) 6_556 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C8 H8 S2 0.93 2.94 3.575(4) 126.4 7_675 C9 H9 O2 0.93 2.62 3.457(4) 149.9 1_565 N5 H5A O1 0.86 2.55 3.044(4) 117.8 1_665 N5 H5A OW2 0.86 2.09 2.919(4) 162.9 7_665 C8 H8 S2 0.93 2.94 3.575(4) 126.4 7_675 C9 H9 O2 0.93 2.62 3.457(4) 149.9 1_565 N5 H5A O1 0.86 2.55 3.044(4) 117.8 1_665 N5 H5A OW2 0.86 2.09 2.919(4) 162.9 7_665 _refine_diff_density_max 1.391 _refine_diff_density_min -1.016 _refine_diff_density_rms 0.138 _shelxl_version_number 2013-4 _shelx_res_file ; TITL Pbcm in Pbcm CELL 0.71073 6.4685 15.0067 25.7319 90.000 90.000 90.000 ZERR 4.00 0.0013 0.0029 0.0049 0.000 0.000 0.000 LATT 1 SYMM - X, - Y, 1/2 + Z SYMM X, 1/2 - Y, - Z SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O S BR U UNIT 56 40 24 16 16 8 4 MERG 2 EQIV $1 -x+1, y+3/2, z HTAB C8 S2_$1 EQIV $2 x, y+1, z HTAB C9 O2_$2 EQIV $3 x+1, y+1, z HTAB N5 O1_$3 EQIV $4 -x+1, y+1/2, z HTAB N5 OW2_$4 HTAB C8 S2_$1 HTAB C9 O2_$2 HTAB N5 O1_$3 HTAB N5 OW2_$4 HTAB OW2 OW1 FMAP 2 PLAN 10 ACTA 50.00 BOND $H L.S. 24 WGHT 0.022500 6.052500 FVAR 0.04378 C1 1 0.153376 0.194954 0.119247 11.00000 0.01789 0.01406 = 0.01708 -0.00070 -0.00214 0.00107 C2 1 0.272875 -0.069030 0.176451 11.00000 0.01511 0.01776 = 0.01199 0.00093 0.00018 -0.00328 C5 1 0.781148 0.945533 0.113499 11.00000 0.01647 0.02275 = 0.03340 -0.00852 -0.00712 0.00297 AFIX 43 H5 2 0.818565 0.887500 0.122003 11.00000 -1.20000 AFIX 0 C6 1 0.776563 0.971702 0.062455 11.00000 0.01687 0.03068 = 0.02862 -0.01126 -0.00081 0.00237 AFIX 43 H6 2 0.808643 0.931777 0.036016 11.00000 -1.20000 AFIX 0 C7 1 0.723198 1.058737 0.051199 11.00000 0.01647 0.03130 = 0.01528 -0.00478 -0.00283 -0.00547 C8 1 0.673588 1.118276 0.090883 11.00000 0.01970 0.02256 = 0.02023 -0.00300 -0.00126 -0.00195 AFIX 43 H8 2 0.637531 1.176893 0.083433 11.00000 -1.20000 AFIX 0 C9 1 0.679311 1.088278 0.141014 11.00000 0.01900 0.02098 = 0.02109 -0.00677 -0.00063 -0.00258 AFIX 43 H9 2 0.646743 1.126791 0.168119 11.00000 -1.20000 AFIX 0 N1 3 0.132705 0.182587 0.164071 11.00000 0.02216 0.02122 = 0.01749 0.00036 -0.00074 0.00304 N2 3 0.251238 0.001125 0.194079 11.00000 0.02414 0.01892 = 0.02671 -0.00473 0.00418 0.00245 N5 3 0.731547 1.003741 0.151338 11.00000 0.01430 0.02665 = 0.01942 -0.00104 -0.00447 -0.00116 AFIX 43 H5A 2 0.733474 0.986076 0.183128 11.00000 -1.20000 AFIX 0 O1 4 -0.094846 0.086988 0.250000 10.50000 0.00982 0.02102 = 0.01843 0.00000 0.00000 0.00069 O2 4 0.422734 0.165215 0.250000 10.50000 0.01475 0.02188 = 0.01967 0.00000 0.00000 -0.00076 OW1 4 -0.013179 0.278895 0.250000 10.50000 0.02682 0.01499 = 0.01551 0.00000 0.00000 0.00590 OW2 4 0.294196 0.408375 0.250000 10.50000 0.02083 0.02196 = 0.02853 0.00000 0.00000 0.00267 S1 5 0.176395 0.212573 0.057916 11.00000 0.03893 0.03464 = 0.01134 0.00516 0.00074 -0.00453 S2 5 0.307317 -0.168064 0.152136 11.00000 0.04733 0.01510 = 0.03529 -0.00959 0.01988 -0.00768 BR1 6 0.712681 1.098595 -0.018012 11.00000 0.02768 0.04484 = 0.01800 -0.00475 0.00107 -0.00916 U1 7 0.163810 0.126400 0.250000 10.50000 0.01233 0.01125 = 0.01014 0.00000 0.00000 0.00078 HKLF 4 REM Pbcm in Pbcm REM R1 = 0.0243 for 2830 Fo > 4sig(Fo) and 0.0313 for all 3212 data REM 148 parameters refined using 0 restraints END WGHT 0.0225 6.0532 REM Highest difference peak 1.391, deepest hole -1.016, 1-sigma level 0.138 Q1 1 0.1893 0.3616 0.2500 10.50000 0.05 1.39 Q2 1 0.2276 0.1700 0.2500 10.50000 0.05 1.30 Q3 1 0.0461 0.0825 0.2500 10.50000 0.05 0.91 Q4 1 0.2378 0.0850 0.2500 10.50000 0.05 0.89 Q5 1 0.0567 0.1793 0.2500 10.50000 0.05 0.82 Q6 1 0.4087 0.3753 0.2500 10.50000 0.05 0.80 Q7 1 -0.0766 0.2859 0.2771 11.00000 0.05 0.69 Q8 1 0.7504 1.0440 -0.0105 11.00000 0.05 0.63 Q9 1 0.3604 0.1979 0.2500 10.50000 0.05 0.60 Q10 1 0.2393 0.1374 0.2972 11.00000 0.05 0.57 ; _shelx_res_checksum 30126 _shelx_hkl_file ; -1 0 0 44.26 1.97 -1 0 0 44.46 2.00 1 0 0 55.36 2.01 -2 0 0 927.89 36.80 2 0 0 1000.00 36.67 -2 0 0 976.75 36.90 -3 0 0 20.47 1.00 3 0 0 21.28 1.22 -3 0 0 22.71 1.14 -3 0 0 22.13 1.27 -4 0 0 0.43 0.47 4 0 0 -0.14 0.40 -4 0 0 0.53 0.24 -5 0 0 10.15 1.09 5 0 0 9.91 0.83 5 0 0 11.02 1.10 -6 0 0 50.04 2.74 6 0 0 47.94 2.63 6 0 0 51.47 2.41 -7 0 0 77.60 3.97 7 0 0 78.73 3.91 -8 0 0 11.88 1.56 8 0 0 9.93 1.47 0 1 0 -0.04 0.02 0 -1 0 -0.03 0.03 0 1 0 -0.04 0.03 0 1 0 -0.03 0.04 0 -1 0 -0.09 0.03 0 -1 0 -0.01 0.04 1 -1 0 14.39 0.67 1 1 0 14.72 0.64 -1 -1 0 12.65 0.65 -1 1 0 12.89 0.59 -1 -1 0 14.91 0.60 1 -1 0 12.62 0.59 1 1 0 14.10 0.71 2 1 0 338.65 13.85 -2 1 0 369.36 13.95 -2 1 0 364.95 13.95 -2 1 0 350.71 13.89 -2 -1 0 361.31 13.90 2 -1 0 370.28 13.85 -2 -1 0 375.64 13.86 -3 -1 0 29.09 1.52 -3 -1 0 30.34 1.39 3 -1 0 30.14 1.50 3 1 0 28.50 1.52 -3 1 0 29.49 1.31 4 -1 0 242.09 9.65 -4 -1 0 245.21 9.56 -4 1 0 241.38 9.47 4 1 0 244.20 9.69 4 -1 0 243.19 9.58 -4 -1 0 245.17 9.72 -4 1 0 245.93 9.76 -4 -1 0 239.01 9.51 5 1 0 60.32 2.62 -5 -1 0 55.89 2.52 5 -1 0 59.83 2.68 5 -1 0 60.05 2.88 5 1 0 58.76 2.90 -5 -1 0 57.30 2.91 -5 1 0 60.85 2.97 -6 1 0 9.33 1.22 -6 -1 0 6.79 1.05 6 -1 0 10.18 0.94 6 -1 0 10.24 1.20 6 1 0 8.22 1.14 -7 1 0 12.42 1.50 7 -1 0 11.63 1.40 7 1 0 10.86 1.35 -7 -1 0 10.04 1.36 -8 -1 0 7.32 1.29 -8 1 0 6.06 1.26 8 -1 0 5.23 1.13 8 1 0 4.63 1.17 0 2 0 15.90 0.75 0 2 0 15.61 0.72 0 2 0 16.50 0.66 0 -2 0 16.45 0.72 -1 2 0 19.71 0.93 -1 -2 0 19.63 0.89 1 -2 0 20.29 0.88 -1 -2 0 20.51 0.81 1 -2 0 20.14 0.94 1 2 0 20.53 0.94 1 2 0 19.71 0.83 1 2 0 18.94 0.91 -1 2 0 19.14 0.86 2 2 0 69.29 2.87 2 -2 0 70.50 2.92 2 2 0 71.06 2.95 -2 -2 0 71.27 2.90 2 -2 0 67.94 2.88 -2 2 0 68.15 2.79 -2 2 0 71.74 2.97 -2 -2 0 72.47 2.79 -3 -2 0 19.00 1.15 -3 2 0 19.89 1.23 -3 -2 0 20.68 1.01 3 -2 0 19.43 1.10 3 -2 0 21.79 1.17 3 2 0 19.13 1.20 -3 2 0 19.50 0.92 4 2 0 36.34 1.94 -4 2 0 33.60 1.58 -4 -2 0 36.04 1.71 -4 -2 0 37.11 1.89 4 -2 0 36.95 1.88 4 -2 0 38.52 1.82 -4 2 0 38.33 2.01 -5 -2 0 8.40 1.00 5 -2 0 8.80 0.87 5 -2 0 7.93 0.94 -5 -2 0 8.59 0.70 5 2 0 7.82 0.97 5 2 0 9.29 0.74 -5 2 0 9.75 1.10 6 2 0 17.41 1.58 6 -2 0 15.96 1.23 -6 2 0 14.67 1.55 -6 -2 0 13.86 1.39 6 -2 0 18.58 1.47 -7 2 0 -0.48 0.70 -7 -2 0 0.33 0.70 7 -2 0 -0.14 0.66 7 2 0 0.05 0.73 -8 2 0 0.33 0.88 8 -2 0 1.70 0.97 8 2 0 0.81 0.94 -8 -2 0 2.61 1.05 0 -3 0 0.09 0.13 0 3 0 0.09 0.12 0 -3 0 -0.01 0.08 0 3 0 0.00 0.07 0 3 0 0.04 0.18 1 3 0 74.67 2.96 -1 -3 0 66.17 2.88 -1 3 0 73.00 2.90 -1 3 0 71.19 2.92 1 -3 0 72.33 2.95 1 -3 0 75.77 2.83 -1 -3 0 72.48 2.81 1 3 0 74.05 2.90 -2 3 0 95.93 3.67 2 -3 0 96.52 3.72 2 3 0 91.66 3.79 -2 -3 0 79.34 3.70 -2 3 0 94.74 3.81 2 -3 0 87.25 3.78 2 3 0 94.60 3.76 -2 -3 0 98.51 3.61 -3 -3 0 32.67 1.43 3 -3 0 32.58 1.60 -3 -3 0 32.47 1.62 3 -3 0 34.05 1.63 -3 3 0 35.02 1.74 -3 3 0 32.57 1.42 3 3 0 30.70 1.67 4 3 0 104.58 4.65 -4 3 0 109.67 4.33 -4 -3 0 109.82 4.40 -4 -3 0 110.18 4.64 -4 3 0 107.29 4.72 4 -3 0 106.42 4.56 4 -3 0 111.41 4.58 -5 3 0 25.14 1.72 5 -3 0 23.95 1.57 5 -3 0 28.12 1.54 5 3 0 23.36 1.60 -5 -3 0 25.82 1.66 6 -3 0 20.40 1.56 -6 3 0 19.56 1.61 6 3 0 22.21 1.69 6 -3 0 19.64 1.41 -6 -3 0 21.55 1.66 7 -3 0 4.92 0.88 -7 3 0 4.78 1.08 -7 -3 0 7.04 1.20 7 -3 0 5.80 1.07 7 3 0 4.33 1.04 8 -3 0 0.57 0.83 8 3 0 -0.68 0.81 -8 -3 0 -0.14 0.76 -8 3 0 0.02 0.94 0 -4 0 386.18 14.16 0 4 0 364.51 14.11 0 4 0 364.38 13.98 0 4 0 362.89 14.28 -1 -4 0 0.68 0.21 -1 -4 0 0.83 0.15 1 4 0 1.12 0.24 1 -4 0 0.55 0.23 1 4 0 0.60 0.28 -1 4 0 0.74 0.24 1 -4 0 0.65 0.15 -1 4 0 0.39 0.21 -2 4 0 82.03 3.33 2 -4 0 83.62 3.32 -2 -4 0 85.07 3.22 2 -4 0 82.56 3.45 2 4 0 81.04 3.41 -2 -4 0 83.02 3.37 2 4 0 76.62 3.40 -2 4 0 83.43 3.43 -3 -4 0 5.77 0.63 3 -4 0 7.95 0.71 -3 4 0 7.13 0.50 -3 4 0 5.56 0.67 3 4 0 7.35 0.81 3 -4 0 6.48 0.70 -3 -4 0 6.54 0.44 3 4 0 6.94 0.64 -4 4 0 22.93 1.10 4 -4 0 22.87 1.35 4 4 0 23.19 1.48 4 -4 0 22.68 1.34 -4 -4 0 23.45 1.15 -4 -4 0 22.55 1.40 -4 4 0 23.09 1.51 -5 4 0 9.29 1.11 5 -4 0 8.28 0.90 -5 -4 0 7.80 0.97 5 -4 0 7.97 0.94 5 4 0 7.54 0.99 6 -4 0 46.76 2.60 -6 -4 0 50.03 2.72 6 -4 0 49.52 2.51 6 4 0 47.82 2.71 -6 4 0 49.62 2.81 7 4 0 35.68 2.39 -7 -4 0 36.64 2.42 -7 4 0 36.48 2.46 7 -4 0 33.89 2.21 7 -4 0 35.71 2.12 -8 -4 0 12.83 1.65 8 -4 0 13.63 1.57 8 4 0 8.43 1.40 -8 4 0 9.05 1.44 0 5 0 -0.06 0.22 0 5 0 -0.37 0.17 0 5 0 0.00 0.09 0 -5 0 -0.02 0.17 1 5 0 20.10 0.98 -1 -5 0 22.18 0.94 1 -5 0 21.41 0.89 1 -5 0 21.71 1.10 -1 5 0 21.19 1.06 1 5 0 21.47 1.10 -1 -5 0 20.59 1.02 -1 5 0 20.58 1.06 2 -5 0 64.07 2.57 -2 -5 0 59.84 2.62 2 5 0 62.32 2.68 -2 5 0 61.95 2.70 -2 5 0 62.02 2.62 2 -5 0 64.07 2.74 -2 -5 0 62.08 2.47 2 5 0 62.87 2.70 -3 5 0 5.55 0.50 3 5 0 8.78 0.84 3 5 0 5.59 0.60 3 -5 0 6.27 0.63 -3 -5 0 5.07 0.62 3 -5 0 5.17 0.64 -3 -5 0 5.98 0.40 -3 5 0 5.79 0.71 4 5 0 28.29 1.69 4 -5 0 28.77 1.63 4 -5 0 28.98 1.57 -4 5 0 26.13 1.69 -4 5 0 28.71 1.35 -4 -5 0 31.36 1.65 -4 -5 0 28.82 1.32 5 -5 0 12.50 1.15 5 5 0 12.81 1.35 -5 5 0 13.06 1.36 5 -5 0 13.95 1.21 -5 -5 0 13.26 1.26 6 -5 0 2.31 0.70 6 -5 0 1.05 0.63 6 5 0 2.23 0.84 -6 -5 0 1.32 0.67 -6 5 0 2.84 0.88 7 -5 0 3.03 0.81 7 -5 0 3.53 0.88 -7 -5 0 1.99 0.92 -7 5 0 3.54 1.00 7 5 0 2.21 1.01 8 -5 0 18.03 1.81 8 5 0 19.42 2.02 -8 -5 0 18.67 1.96 -8 5 0 19.77 2.05 0 6 0 6.23 0.59 0 6 0 6.88 0.53 0 -6 0 6.76 0.48 0 6 0 5.64 0.32 -1 -6 0 -0.25 0.18 1 -6 0 -0.24 0.23 -1 -6 0 -0.24 0.12 -1 6 0 0.03 0.21 1 6 0 -0.04 0.17 -1 6 0 0.00 0.23 1 -6 0 -0.01 0.11 1 6 0 0.05 0.28 2 6 0 8.33 0.70 2 6 0 8.12 0.68 2 -6 0 7.99 0.54 -2 -6 0 7.70 0.63 -2 6 0 7.77 0.72 2 -6 0 6.88 0.69 -2 -6 0 8.34 0.46 -2 6 0 8.24 0.62 -3 6 0 14.17 0.85 3 6 0 12.48 0.94 -3 6 0 14.66 1.02 3 6 0 14.94 1.04 3 -6 0 13.70 0.89 -3 -6 0 14.35 0.94 3 -6 0 13.12 1.02 -4 -6 0 7.56 0.53 4 6 0 7.44 0.95 -4 -6 0 7.37 0.82 -4 6 0 8.04 0.99 4 -6 0 8.74 0.85 -4 6 0 8.48 0.62 4 -6 0 6.66 0.84 4 6 0 7.67 0.80 -5 -6 0 9.07 1.08 5 6 0 11.76 1.28 5 -6 0 12.54 1.17 -5 6 0 11.58 1.24 5 -6 0 9.10 1.01 6 -6 0 0.64 0.63 6 -6 0 0.54 0.64 6 6 0 1.06 0.79 -6 6 0 0.88 0.75 -6 -6 0 0.98 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1.49 0.79 0 -4 31 1.02 0.86 0 4 31 1.88 1.07 -1 4 31 -0.21 1.02 1 4 -31 -1.12 0.72 1 -4 31 0.75 0.83 -1 -4 -31 0.67 0.81 1 -4 31 0.63 0.83 1 4 31 -0.93 0.87 1 4 31 0.86 0.76 -1 -4 31 0.25 0.98 1 -4 -31 -0.37 0.75 -1 4 -31 0.79 0.87 1 -4 -31 0.09 0.64 2 -4 31 1.37 0.81 -2 4 31 -1.05 1.04 2 4 -31 0.94 0.88 -2 -4 -31 1.14 0.85 -2 -4 31 -0.21 1.02 2 -4 -31 0.18 0.81 -2 4 -31 1.30 1.00 2 4 31 1.16 0.90 2 -4 -31 1.38 0.76 2 4 31 0.61 0.79 -3 -4 -31 2.77 1.06 3 4 -31 4.26 1.09 3 -4 31 3.70 1.04 -3 4 31 2.94 1.35 -3 4 -31 5.02 1.19 -3 -4 31 3.12 1.19 3 -4 -31 1.87 1.01 3 -4 -31 1.69 0.86 3 4 31 1.26 0.89 0 5 -31 0.10 0.76 0 -5 -31 0.17 0.79 0 5 31 -0.71 0.61 0 5 31 -0.31 0.99 0 5 -31 0.17 0.80 0 -5 31 0.80 0.89 -1 5 31 4.35 1.26 1 5 -31 5.48 1.19 -1 -5 -31 4.69 1.13 1 -5 31 6.12 1.13 1 5 31 6.41 1.07 1 -5 -31 4.37 0.95 -1 -5 31 3.97 1.21 1 -5 -31 6.54 1.24 -1 5 -31 4.48 1.15 1 5 31 5.19 1.23 2 -5 31 2.60 0.93 -2 -5 -31 3.73 1.07 2 5 -31 3.88 1.08 -2 5 31 1.82 1.32 2 -5 -31 2.17 0.94 -2 5 -31 3.21 1.09 2 5 31 3.83 1.15 2 5 31 4.06 1.02 -2 -5 31 2.98 1.22 2 -5 -31 3.16 1.06 3 -5 31 0.30 0.82 -3 5 31 -0.24 1.09 3 5 -31 0.81 0.90 -3 -5 -31 1.23 0.93 3 5 31 1.21 0.88 -3 -5 31 -0.90 0.93 -3 5 -31 -0.22 0.84 3 -5 -31 0.14 0.86 0 -6 31 8.37 1.45 0 -6 -31 10.15 1.42 0 6 31 11.31 1.69 0 6 -31 10.97 1.43 1 6 -31 4.37 1.08 -1 6 31 3.64 1.38 -1 -6 -31 5.16 1.15 1 -6 31 8.60 1.27 1 6 31 4.97 1.28 -1 -6 31 4.85 1.30 -1 6 -31 5.77 1.24 1 6 31 4.93 1.01 1 -6 -31 5.92 1.24 2 -6 31 2.20 0.85 -2 6 31 1.02 1.29 2 6 -31 1.07 0.94 -2 -6 -31 1.50 0.92 2 6 31 0.75 0.80 -2 6 -31 1.46 0.98 -2 -6 31 -1.97 0.89 2 6 31 1.58 0.97 2 -6 -31 0.77 0.91 0 7 -31 -0.90 0.71 0 -7 31 -0.85 0.83 0 7 31 1.38 1.12 0 -7 -31 0.12 0.83 1 7 -31 2.82 1.02 -1 -7 -31 2.04 0.99 -1 7 31 4.17 1.42 1 -7 31 4.47 1.06 1 -7 -31 2.95 1.06 1 7 31 3.14 1.23 -1 7 -31 4.64 1.21 -1 -7 31 2.16 1.07 -2 -7 -31 5.22 1.20 2 -7 31 4.43 1.03 2 7 -31 3.80 1.14 -2 7 31 5.49 1.45 2 7 31 4.24 1.14 -2 7 -31 3.87 1.21 -2 -7 31 3.04 1.26 2 -7 -31 4.04 1.12 0 -8 -31 -0.47 0.81 0 8 -31 -0.04 0.83 0 8 31 -0.44 1.01 0 -8 31 -0.95 0.81 -1 8 31 0.01 1.16 1 8 -31 0.55 0.87 -1 -8 -31 -0.41 0.82 1 -8 31 0.98 0.82 -1 -8 31 1.20 1.06 1 -8 -31 -0.05 0.87 1 8 31 -0.54 0.94 0 0 -32 15.31 1.67 0 0 32 17.82 1.91 0 0 -32 19.89 1.75 1 0 -32 12.87 1.58 -1 0 32 13.85 1.76 -1 0 -32 13.30 1.61 1 0 32 15.21 1.56 1 0 -32 15.16 1.60 1 0 32 11.36 1.50 2 0 32 -0.34 0.72 -2 0 -32 0.79 0.87 -2 0 32 0.37 0.93 2 0 -32 -1.20 0.68 3 0 -32 43.01 2.65 -3 0 32 38.60 2.93 -3 0 -32 38.64 2.79 3 0 32 42.78 2.68 0 1 32 0.26 0.94 0 1 -32 -1.40 0.63 0 1 -32 1.16 0.91 0 -1 32 -1.26 0.85 0 -1 -32 0.54 0.83 1 -1 32 30.42 2.20 1 -1 32 33.50 2.21 -1 1 32 22.23 2.30 -1 -1 -32 28.73 2.26 1 1 -32 29.76 2.19 1 1 -32 31.28 2.25 -1 -1 32 28.06 2.40 1 1 32 25.86 2.18 -1 1 -32 29.96 2.28 1 -1 -32 28.82 2.08 1 -1 -32 29.78 2.26 1 1 32 30.90 2.07 2 1 -32 10.88 1.46 -2 -1 -32 8.49 1.35 -2 1 32 8.75 1.65 2 -1 32 9.76 1.30 2 -1 -32 11.76 1.43 -2 1 -32 9.13 1.46 -2 -1 32 10.59 1.69 2 -1 -32 10.27 1.43 2 1 32 11.28 1.38 -3 -1 -32 -1.00 0.92 3 1 -32 1.82 0.93 -3 1 32 1.25 1.26 3 -1 32 2.43 0.99 -3 1 -32 1.94 1.10 -3 -1 32 -1.16 1.12 3 -1 -32 2.42 1.02 3 1 32 -1.04 0.77 0 2 -32 8.33 1.26 0 -2 32 6.65 1.29 0 2 -32 3.27 0.91 0 -2 -32 4.72 1.06 0 2 32 6.31 1.15 0 2 32 8.81 1.44 1 2 -32 0.48 0.90 1 -2 32 0.34 0.87 1 2 -32 -0.31 0.76 1 -2 32 0.80 0.82 -1 2 32 -0.84 0.85 -1 -2 -32 0.51 0.85 1 2 32 -0.08 0.82 -1 2 -32 1.17 0.87 1 -2 -32 -0.25 0.83 1 -2 -32 0.03 0.65 -1 -2 32 1.04 1.01 1 2 32 -0.69 0.69 -2 -2 -32 0.45 0.91 2 -2 32 2.29 0.94 2 2 -32 2.41 0.93 -2 2 32 0.95 1.23 2 -2 -32 1.75 0.90 -2 2 -32 2.39 1.09 2 -2 -32 2.70 0.92 -2 -2 32 2.27 1.12 2 2 32 1.90 0.92 -3 2 32 0.94 1.28 3 2 -32 0.02 0.78 -3 -2 -32 1.51 0.98 -3 -2 32 -0.42 1.14 3 2 32 1.28 0.91 3 -2 -32 0.18 0.82 -3 2 -32 3.27 1.17 0 -3 -32 -1.37 0.70 0 3 32 1.19 0.79 0 3 32 -0.37 0.95 0 3 -32 -0.17 0.73 0 3 -32 0.74 0.81 0 -3 32 -0.67 0.86 -1 3 32 23.62 2.34 1 -3 32 30.48 2.19 1 3 -32 27.06 2.12 -1 -3 -32 27.48 2.25 1 -3 32 31.56 2.20 -1 -3 32 26.99 2.47 1 -3 -32 28.10 2.01 1 3 32 32.17 2.12 1 3 32 26.82 2.27 -1 3 -32 34.30 2.47 1 -3 -32 27.29 2.20 2 3 -32 -0.05 0.83 -2 -3 -32 0.15 0.84 2 -3 32 1.40 0.85 -2 3 32 2.14 1.30 -2 3 -32 0.88 0.95 2 3 32 2.05 0.90 -2 -3 32 0.91 1.01 2 -3 -32 1.92 0.91 2 -3 -32 0.51 0.77 0 -4 -32 5.94 1.24 0 4 32 5.62 1.10 0 4 -32 5.24 1.23 0 4 -32 5.71 1.13 0 4 32 7.03 1.47 0 -4 32 5.01 1.19 -1 4 32 5.28 1.32 -1 -4 -32 5.86 1.15 1 -4 32 7.27 1.22 1 4 -32 7.50 1.23 1 4 32 5.87 1.15 1 -4 -32 6.44 1.27 -1 -4 32 6.13 1.34 1 -4 -32 7.95 1.16 -1 4 -32 3.94 1.13 1 4 32 6.48 1.33 -2 4 32 -1.11 1.11 -2 -4 -32 -0.33 0.80 2 -4 32 0.02 0.78 2 4 -32 -1.09 0.69 -2 -4 32 -0.70 0.90 2 4 32 -1.46 0.72 2 -4 -32 0.86 0.90 2 -4 -32 -0.42 0.67 -2 4 -32 1.30 0.98 0 -5 32 -0.38 0.84 0 -5 -32 -0.70 0.78 0 5 -32 0.04 0.77 0 5 32 0.16 0.66 0 5 32 -1.03 0.99 1 5 -32 2.93 0.99 -1 -5 -32 3.27 1.05 -1 5 32 4.64 1.37 1 -5 32 4.17 1.08 -1 -5 32 4.70 1.32 1 5 32 3.10 0.94 1 5 32 2.61 1.10 -1 5 -32 3.23 1.15 1 -5 -32 4.37 1.11 2 5 -32 11.55 1.55 -2 5 32 11.80 1.91 2 -5 32 15.25 1.59 -2 -5 -32 8.40 1.45 2 -5 -32 12.75 1.68 -2 -5 32 7.57 1.55 2 5 32 10.74 1.51 2 5 32 11.01 1.41 -2 5 -32 12.52 1.69 0 -6 -32 11.87 1.64 0 6 32 12.83 1.84 0 -6 32 10.16 1.53 0 6 -32 12.84 1.56 -1 6 32 0.44 1.16 1 6 -32 1.89 0.97 1 -6 32 1.64 0.86 -1 -6 -32 1.36 0.98 -1 6 -32 0.59 0.98 1 -6 -32 0.32 0.89 -1 -6 32 2.51 1.17 1 6 32 0.65 1.02 1 6 32 1.96 0.87 0 -7 -32 -1.04 0.76 0 7 -32 0.17 0.81 0 7 32 0.18 1.11 0 -7 32 1.62 0.96 -1 7 32 17.49 2.18 1 -7 32 25.31 2.00 1 7 -32 19.50 1.93 -1 -7 -32 26.30 2.15 1 -7 -32 20.81 2.04 -1 7 -32 22.33 2.11 1 7 32 20.21 2.18 -1 -7 32 18.81 2.07 0 0 -33 1.52 0.95 0 0 33 1.23 1.02 1 0 33 0.39 0.79 -1 0 -33 0.37 0.84 1 0 33 0.20 0.87 1 0 -33 0.81 0.87 -1 0 33 0.75 1.09 1 0 -33 0.17 0.79 2 0 -33 -0.21 0.77 -2 0 -33 -0.08 0.88 -2 0 33 -0.46 1.08 2 0 33 1.63 0.89 0 1 -33 1.17 0.91 0 1 33 0.13 0.91 0 -1 33 -0.85 0.98 0 1 -33 0.66 0.79 0 -1 -33 -0.53 0.82 -1 1 33 5.36 1.35 -1 -1 -33 3.98 1.11 1 1 -33 3.48 1.02 1 -1 33 4.57 1.08 1 1 -33 3.63 1.02 1 -1 33 3.79 1.10 1 1 33 4.98 1.05 -1 1 -33 3.09 1.06 1 -1 -33 2.95 1.01 1 1 33 4.49 1.17 -1 -1 33 2.90 1.26 1 -1 -33 3.20 0.96 2 1 -33 9.74 1.38 -2 1 33 9.50 1.73 -2 -1 -33 9.13 1.47 2 -1 33 9.90 1.37 2 1 33 9.64 1.37 2 -1 -33 11.81 1.46 -2 -1 33 7.25 1.53 -2 1 -33 9.17 1.46 0 2 -33 35.75 2.48 0 2 33 37.32 2.36 0 -2 -33 33.88 2.54 0 2 33 33.56 2.60 0 2 -33 32.47 2.30 0 -2 33 36.63 2.55 -1 -2 -33 4.33 1.09 1 -2 33 4.72 1.15 1 -2 33 4.97 1.17 -1 2 33 4.18 1.37 1 2 -33 2.99 0.98 1 -2 -33 3.05 1.03 -1 2 -33 4.42 1.14 1 2 33 2.91 1.08 -1 -2 33 5.09 1.25 1 -2 -33 2.21 0.96 1 2 33 3.73 0.98 -2 2 33 9.31 1.74 2 -2 33 12.86 1.55 -2 -2 -33 6.63 1.30 2 2 -33 10.16 1.44 -2 -2 33 7.06 1.58 2 2 33 10.11 1.44 -2 2 -33 12.37 1.63 2 -2 -33 9.96 1.47 2 -2 -33 7.36 1.27 0 3 -33 -0.52 0.87 0 3 33 0.32 1.04 0 3 -33 0.53 0.81 0 3 33 0.10 0.74 0 -3 33 2.10 1.01 0 -3 -33 0.26 0.81 -1 3 33 5.39 1.46 -1 -3 -33 4.86 1.17 1 -3 33 4.83 1.14 1 3 -33 2.55 0.96 1 -3 -33 3.82 0.96 -1 3 -33 4.12 1.16 -1 -3 33 1.61 1.02 1 -3 -33 4.50 1.15 1 3 33 4.54 1.23 1 3 33 4.70 1.02 -2 3 33 5.94 1.57 -2 -3 -33 7.31 1.39 2 3 -33 6.46 1.28 2 -3 33 10.08 1.37 -2 3 -33 6.37 1.35 2 3 33 8.52 1.34 2 -3 -33 4.55 1.07 2 -3 -33 6.62 1.27 -2 -3 33 8.82 1.60 0 4 33 1.29 0.85 0 -4 33 0.92 0.98 0 4 33 2.13 1.12 0 -4 -33 1.47 0.98 0 4 -33 2.09 0.89 0 4 -33 2.08 1.03 -1 4 33 -0.62 1.06 1 4 -33 1.42 0.93 -1 -4 -33 2.12 1.00 1 -4 33 -0.19 0.84 -1 4 -33 -0.30 0.86 -1 -4 33 0.66 0.89 1 4 33 -1.87 0.81 1 -4 -33 1.08 0.92 1 4 33 -0.37 0.69 1 -4 -33 0.09 0.74 0 5 -33 -0.51 0.78 0 5 33 0.19 1.10 0 -5 33 1.19 0.95 0 -5 -33 0.28 0.86 0 5 33 1.98 0.78 1 5 -33 3.74 1.06 1 -5 33 4.51 1.16 -1 -5 -33 2.40 1.00 -1 5 33 4.64 1.44 1 5 33 3.42 1.15 1 5 33 1.46 0.88 -1 -5 33 1.36 1.14 1 -5 -33 2.48 1.02 -1 5 -33 6.27 1.26 0 0 -34 23.04 2.17 0 0 34 29.33 2.35 -1 0 34 1.40 1.15 1 0 -34 3.52 1.01 1 0 34 2.88 1.08 -1 0 -34 1.43 0.97 1 0 -34 3.49 1.11 1 0 34 2.44 0.90 0 1 -34 0.58 0.87 0 -1 -34 0.53 0.85 0 -1 34 -0.45 0.93 0 1 34 0.80 0.82 0 1 34 -0.26 0.98 1 -1 34 2.18 1.00 -1 1 34 1.17 1.12 1 -1 34 2.11 0.93 -1 -1 -34 0.15 0.90 1 1 -34 2.63 1.00 1 1 -34 0.91 0.98 1 1 34 2.54 0.90 1 -1 -34 1.46 0.97 -1 -1 34 0.53 1.09 1 1 34 2.56 1.11 1 -1 -34 0.33 0.82 -1 1 -34 1.68 0.99 0 -2 -34 4.15 1.19 0 2 -34 2.48 1.00 0 -2 34 3.89 1.22 0 2 -34 3.73 1.02 0 2 34 1.40 0.94 0 2 34 2.56 1.24 -1 -2 -34 0.82 0.88 1 2 -34 -0.16 0.80 -1 2 34 -0.04 1.11 1 -2 34 0.60 0.85 -1 2 -34 0.83 0.97 1 2 34 0.09 0.95 -1 -2 34 -0.13 1.02 1 -2 -34 0.10 0.84 1 2 34 0.32 0.75 1 -2 -34 0.69 0.79 0 3 34 -0.44 0.95 0 3 -34 -0.11 0.94 0 3 34 -1.15 0.77 0 -3 -34 0.00 0.90 0 -3 34 -1.00 0.90 0 3 -34 0.89 0.88 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 75850 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_h-m 'P b c m' _symmetry_int_tables_number 57 _chemical_absolute_configuration ? _database_code_depnum_ccdc_archive 'CCDC 967155' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound_3 _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety '(C5 H5 I N 1+)2,(U O3 C4 H2 N4 S4 2-),(H2 O)' _chemical_formula_sum 'C14 H14 I2 N6 O4 S4 U' _chemical_properties_physical thermochromic _exptl_crystal_recrystallization_method 'Slow Aqueous Evaporation' _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour 'Orange (293(2)K) Yellow (100(2)K)' _diffrn_ambient_temperature 100(2) _chemical_formula_weight 950.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.6151(18) _cell_length_b 14.993(4) _cell_length_c 25.896(7) _cell_angle_alpha 90 _cell_angle_beta 91.068(4) _cell_angle_gamma 90 _cell_volume 2567.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7627 _cell_measurement_theta_min 5.434 _cell_measurement_theta_max 57.987 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.448 _exptl_crystal_F_000 1720 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.122 _exptl_crystal_size_mid 0.077 _exptl_crystal_size_min 0.062 _exptl_absorpt_coefficient_mu 9.082 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5827 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_process_details 'SADABS, G. Sheldrick (1999)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_measurement_device_type 'Bruker ApexII CCD' _diffrn_measurement_method 'Omega and Phi Scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 36812 _diffrn_reflns_av_unetI/netI 0.0529 _diffrn_reflns_av_R_equivalents 0.0642 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.570 _diffrn_reflns_theta_max 30.404 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.940 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.940 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.940 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 7328 _reflns_number_gt 5970 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'APEX II (Bruker AXS, 2013)' _computing_cell_refinement 'SAINT (Bruker AXS, 2013)' _computing_data_reduction 'SAINT (Bruker AXS, 2013)' _computing_structure_solution 'SIR92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Crystal Maker v.8.2.2 (Palmer 2009)' _computing_publication_material 'WINGX (Farrugia, 2012)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+115.1768P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 7328 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0736 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1333 _refine_ls_wR_factor_gt 0.1276 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.150 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6522(16) 0.8051(7) 0.8864(4) 0.016(2) Uani 1 1 d . . . . . C2 C 0.7825(17) 1.0709(8) 0.8234(4) 0.017(2) Uani 1 1 d . . . . . C3 C 0.7582(16) 1.0628(7) 0.6770(4) 0.0141(19) Uani 1 1 d . . . . . C4 C 0.6512(15) 0.8013(7) 0.6263(4) 0.0131(19) Uani 1 1 d . . . . . C5 C 0.2965(17) 1.0419(8) -0.1074(4) 0.019(2) Uani 1 1 d . . . . . H5 H 0.3427 1.0991 -0.1146 0.023 Uiso 1 1 calc R U . . . C6 C 0.2842(17) 1.0137(8) -0.0572(4) 0.020(2) Uani 1 1 d . . . . . H6 H 0.3207 1.0517 -0.0302 0.024 Uiso 1 1 calc R U . . . C7 C 0.2169(15) 0.9281(8) -0.0470(4) 0.017(2) Uani 1 1 d . . . . . C8 C 0.1660(15) 0.8728(7) -0.0881(4) 0.016(2) Uani 1 1 d . . . . . H8 H 0.1245 0.8145 -0.0820 0.019 Uiso 1 1 calc R U . . . C9 C 0.1770(16) 0.9042(8) -0.1380(4) 0.020(2) Uani 1 1 d . . . . . H9 H 0.1395 0.8679 -0.1657 0.023 Uiso 1 1 calc R U . . . C10 C 0.2572(17) 0.4376(8) 1.1254(4) 0.020(2) Uani 1 1 d . . . . . H10 H 0.2805 0.3787 1.1352 0.024 Uiso 1 1 calc R U . . . C11 C 0.2659(17) 0.4626(7) 1.0739(4) 0.019(2) Uani 1 1 d . . . . . H11 H 0.2963 0.4211 1.0485 0.023 Uiso 1 1 calc R U . . . C12 C 0.2278(15) 0.5516(8) 1.0611(4) 0.016(2) Uani 1 1 d . . . . . C13 C 0.1820(18) 0.6116(8) 1.0988(4) 0.022(2) Uani 1 1 d . . . . . H13 H 0.1553 0.6708 1.0902 0.027 Uiso 1 1 calc R U . . . C14 C 0.1755(17) 0.5846(8) 1.1490(4) 0.018(2) Uani 1 1 d . . . . . H14 H 0.1438 0.6252 1.1748 0.022 Uiso 1 1 calc R U . . . N1 N 0.6332(15) 0.8158(7) 0.8415(4) 0.0188(19) Uani 1 1 d . . . . . N2 N 0.7480(15) 0.9973(6) 0.8110(4) 0.0191(19) Uani 1 1 d . . . . . N3 N 0.7453(15) 0.9963(7) 0.6998(4) 0.022(2) Uani 1 1 d . . . . . N4 N 0.6215(15) 0.8143(7) 0.6706(4) 0.0192(19) Uani 1 1 d . . . . . N5 N 0.2418(14) 0.9870(7) -0.1462(4) 0.0183(19) Uani 1 1 d . . . . . H5A H 0.2488 1.0060 -0.1774 0.022 Uiso 1 1 calc R U . . . N6 N 0.2148(14) 0.4996(7) 1.1609(4) 0.0189(19) Uani 1 1 d . . . . . H6A H 0.2128 0.4839 1.1929 0.023 Uiso 1 1 calc R U . . . O1 O 0.4064(11) 0.9110(5) 0.7557(3) 0.0143(14) Uani 1 1 d . . . . . O2 O 0.9119(12) 0.8340(6) 0.7556(3) 0.0215(17) Uani 1 1 d . . . . . OW1 O 0.4862(11) 0.7181(5) 0.7548(3) 0.0144(14) Uani 1 1 d . . . . . OW2 O 0.7902(12) 0.5919(5) 0.7402(3) 0.0177(15) Uani 1 1 d . . . . . S1 S 0.6745(5) 0.7891(2) 0.94747(10) 0.0230(6) Uani 1 1 d . . . . . S2 S 0.8399(5) 1.17301(19) 0.83880(11) 0.0223(6) Uani 1 1 d . . . . . S3 S 0.7736(5) 1.1577(2) 0.64634(11) 0.0233(6) Uani 1 1 d . . . . . S4 S 0.6895(5) 0.7846(2) 0.56605(11) 0.0262(6) Uani 1 1 d . . . . . I1 I 0.19684(11) 0.88243(5) 0.02845(3) 0.01939(16) Uani 1 1 d . . . . . I2 I 0.23389(11) 0.58964(5) 0.98357(3) 0.01983(16) Uani 1 1 d . . . . . U1 U 0.65864(6) 0.87120(2) 0.75542(2) 0.01003(9) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.013(5) 0.016(5) 0.019(5) 0.001(4) 0.003(4) 0.000(4) C2 0.021(5) 0.020(5) 0.009(4) -0.005(4) -0.004(4) 0.004(4) C3 0.014(5) 0.014(5) 0.014(5) 0.000(4) 0.005(4) -0.001(4) C4 0.011(5) 0.012(5) 0.016(5) -0.001(4) 0.000(4) -0.003(4) C5 0.021(5) 0.019(5) 0.019(5) 0.000(4) 0.003(4) -0.002(4) C6 0.020(6) 0.019(5) 0.020(5) -0.008(4) 0.003(4) -0.002(4) C7 0.010(5) 0.030(6) 0.011(4) 0.000(4) 0.002(4) 0.005(4) C8 0.013(5) 0.011(5) 0.025(5) 0.002(4) 0.002(4) 0.004(4) C9 0.009(5) 0.029(6) 0.021(5) -0.002(5) -0.001(4) -0.004(4) C10 0.018(5) 0.018(5) 0.024(6) -0.002(4) -0.003(4) 0.005(4) C11 0.017(5) 0.015(5) 0.025(6) -0.010(4) -0.004(4) 0.009(4) C12 0.007(4) 0.028(6) 0.014(5) -0.003(4) 0.002(4) -0.004(4) C13 0.023(6) 0.024(6) 0.020(5) -0.003(4) -0.002(4) -0.005(5) C14 0.018(5) 0.016(5) 0.020(5) -0.005(4) -0.001(4) 0.002(4) N1 0.021(5) 0.019(5) 0.016(4) 0.004(4) 0.001(4) -0.003(4) N2 0.020(5) 0.014(4) 0.023(5) 0.004(4) -0.002(4) -0.002(4) N3 0.024(5) 0.019(5) 0.022(5) 0.003(4) 0.000(4) -0.002(4) N4 0.020(5) 0.018(5) 0.019(5) -0.001(4) -0.001(4) -0.005(4) N5 0.018(4) 0.021(5) 0.017(4) 0.002(4) 0.006(3) 0.005(4) N6 0.013(4) 0.026(5) 0.018(4) 0.000(4) -0.004(3) 0.004(4) O1 0.010(3) 0.010(3) 0.022(4) -0.001(3) -0.002(3) -0.002(3) O2 0.017(4) 0.038(5) 0.010(3) 0.004(3) 0.001(3) -0.002(4) OW1 0.014(4) 0.014(4) 0.016(3) 0.003(3) -0.001(3) -0.003(3) OW2 0.020(4) 0.013(4) 0.020(4) 0.001(3) 0.004(3) 0.001(3) S1 0.0285(15) 0.0303(16) 0.0101(12) 0.0050(11) -0.0001(10) 0.0019(12) S2 0.0352(16) 0.0107(12) 0.0210(13) -0.0038(10) -0.0051(11) 0.0027(11) S3 0.0343(16) 0.0161(13) 0.0198(13) 0.0069(11) 0.0100(11) 0.0078(12) S4 0.0341(17) 0.0322(17) 0.0124(12) -0.0048(11) 0.0035(11) 0.0023(13) I1 0.0215(3) 0.0236(4) 0.0131(3) -0.0002(3) 0.0010(2) 0.0036(3) I2 0.0220(4) 0.0243(4) 0.0132(3) -0.0009(3) 0.0012(2) -0.0061(3) U1 0.01088(16) 0.00928(16) 0.00994(16) 0.00066(13) 0.00063(11) -0.00017(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.178(14) . ? C1 S1 1.603(11) . ? C2 N2 1.170(15) . ? C2 S2 1.625(12) . ? C3 N3 1.163(14) . ? C3 S3 1.633(11) . ? C4 N4 1.184(14) . ? C4 S4 1.604(11) . ? C5 N5 1.343(15) . ? C5 C6 1.371(16) . ? C5 H5 0.9300 . ? C6 C7 1.385(16) . ? C6 H6 0.9300 . ? C7 C8 1.386(15) . ? C7 I1 2.077(10) . ? C8 C9 1.378(15) . ? C8 H8 0.9300 . ? C9 N5 1.332(15) . ? C9 H9 0.9300 . ? C10 N6 1.341(15) . ? C10 C11 1.388(16) . ? C10 H10 0.9300 . ? C11 C12 1.397(16) . ? C11 H11 0.9300 . ? C12 C13 1.365(16) . ? C12 I2 2.089(11) . ? C13 C14 1.363(16) . ? C13 H13 0.9300 . ? C14 N6 1.336(15) . ? C14 H14 0.9300 . ? N1 U1 2.388(9) . ? N2 U1 2.442(10) . ? N3 U1 2.440(10) . ? N4 U1 2.365(9) . ? N5 H5A 0.8600 . ? N6 H6A 0.8600 . ? O1 U1 1.773(7) . ? O2 U1 1.765(8) . ? OW1 U1 2.564(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 S1 178.8(11) . . ? N2 C2 S2 177.2(11) . . ? N3 C3 S3 178.3(10) . . ? N4 C4 S4 179.3(11) . . ? N5 C5 C6 120.0(11) . . ? N5 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C7 119.4(10) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C6 C7 C8 118.8(10) . . ? C6 C7 I1 120.7(8) . . ? C8 C7 I1 120.4(9) . . ? C9 C8 C7 119.9(11) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? N5 C9 C8 119.4(11) . . ? N5 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? N6 C10 C11 119.0(11) . . ? N6 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C10 C11 C12 118.4(10) . . ? C10 C11 H11 120.8 . . ? C12 C11 H11 120.8 . . ? C13 C12 C11 120.1(11) . . ? C13 C12 I2 121.0(9) . . ? C11 C12 I2 118.8(8) . . ? C14 C13 C12 119.8(12) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? N6 C14 C13 119.6(11) . . ? N6 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C1 N1 U1 163.8(9) . . ? C2 N2 U1 159.3(9) . . ? C3 N3 U1 168.4(9) . . ? C4 N4 U1 160.6(8) . . ? C9 N5 C5 122.4(10) . . ? C9 N5 H5A 118.8 . . ? C5 N5 H5A 118.8 . . ? C14 N6 C10 123.1(10) . . ? C14 N6 H6A 118.5 . . ? C10 N6 H6A 118.5 . . ? O2 U1 O1 178.7(4) . . ? O2 U1 N4 88.4(3) . . ? O1 U1 N4 92.5(3) . . ? O2 U1 N1 88.3(3) . . ? O1 U1 N1 91.8(3) . . ? N4 U1 N1 137.2(3) . . ? O2 U1 N3 90.7(4) . . ? O1 U1 N3 88.6(3) . . ? N4 U1 N3 75.6(3) . . ? N1 U1 N3 147.1(3) . . ? O2 U1 N2 91.3(4) . . ? O1 U1 N2 87.4(3) . . ? N4 U1 N2 147.8(3) . . ? N1 U1 N2 74.9(3) . . ? N3 U1 N2 72.3(3) . . ? O2 U1 OW1 98.0(3) . . ? O1 U1 OW1 83.3(3) . . ? N4 U1 OW1 68.5(3) . . ? N1 U1 OW1 69.8(3) . . ? N3 U1 OW1 142.6(3) . . ? N2 U1 OW1 143.1(3) . . ? _refine_diff_density_max 5.291 _refine_diff_density_min -3.046 _refine_diff_density_rms 0.347 _shelxl_version_number 2013-4 _shelx_res_file ; TITL P21onc in P2(1)/c CELL 0.71073 6.6151 14.9927 25.8958 90.000 91.068 90.000 ZERR 4.00 0.0018 0.0039 0.0068 0.000 0.004 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O S I U UNIT 56 40 24 16 16 8 4 MERG 2 FMAP 2 ACTA 50 HTAB BOND $H PLAN 25 L.S. 24 WGHT 0.000000 115.176796 FVAR 0.03890 C1 1 0.652191 0.805133 0.886434 11.00000 0.01274 0.01552 = 0.01938 0.00107 0.00330 -0.00050 C2 1 0.782472 1.070914 0.823400 11.00000 0.02074 0.02016 = 0.00942 -0.00467 -0.00374 0.00405 C3 1 0.758153 1.062819 0.676969 11.00000 0.01415 0.01400 = 0.01437 0.00047 0.00509 -0.00081 C4 1 0.651151 0.801312 0.626268 11.00000 0.01122 0.01224 = 0.01584 -0.00105 0.00042 -0.00329 C5 1 0.296480 1.041915 -0.107409 11.00000 0.02101 0.01893 = 0.01850 0.00009 0.00316 -0.00173 AFIX 43 H5 2 0.342704 1.099080 -0.114605 11.00000 -1.20000 AFIX 0 C6 1 0.284186 1.013697 -0.057210 11.00000 0.02038 0.01878 = 0.02022 -0.00803 0.00347 -0.00155 AFIX 43 H6 2 0.320692 1.051703 -0.030229 11.00000 -1.20000 AFIX 0 C7 1 0.216944 0.928114 -0.047011 11.00000 0.01046 0.02978 = 0.01058 -0.00022 0.00230 0.00460 C8 1 0.166037 0.872759 -0.088110 11.00000 0.01258 0.01102 = 0.02508 0.00204 0.00194 0.00380 AFIX 43 H8 2 0.124547 0.814492 -0.082027 11.00000 -1.20000 AFIX 0 C9 1 0.176984 0.904177 -0.138006 11.00000 0.00922 0.02869 = 0.02068 -0.00231 -0.00053 -0.00442 AFIX 43 H9 2 0.139487 0.867883 -0.165689 11.00000 -1.20000 AFIX 0 C10 1 0.257228 0.437583 1.125447 11.00000 0.01791 0.01776 = 0.02359 -0.00227 -0.00315 0.00505 AFIX 43 H10 2 0.280513 0.378717 1.135194 11.00000 -1.20000 AFIX 0 C11 1 0.265871 0.462606 1.073935 11.00000 0.01710 0.01474 = 0.02547 -0.00961 -0.00354 0.00856 AFIX 43 H11 2 0.296253 0.421101 1.048543 11.00000 -1.20000 AFIX 0 C12 1 0.227849 0.551612 1.061146 11.00000 0.00680 0.02821 = 0.01400 -0.00304 0.00228 -0.00445 C13 1 0.182016 0.611630 1.098791 11.00000 0.02295 0.02378 = 0.01953 -0.00305 -0.00213 -0.00473 AFIX 43 H13 2 0.155345 0.670759 1.090215 11.00000 -1.20000 AFIX 0 C14 1 0.175457 0.584636 1.148991 11.00000 0.01788 0.01636 = 0.01969 -0.00514 -0.00144 0.00224 AFIX 43 H14 2 0.143785 0.625173 1.174792 11.00000 -1.20000 AFIX 0 N1 3 0.633228 0.815758 0.841516 11.00000 0.02069 0.01940 = 0.01626 0.00380 0.00141 -0.00266 N2 3 0.747983 0.997313 0.811013 11.00000 0.02048 0.01358 = 0.02313 0.00423 -0.00235 -0.00214 N3 3 0.745274 0.996325 0.699809 11.00000 0.02435 0.01892 = 0.02183 0.00253 -0.00021 -0.00210 N4 3 0.621466 0.814312 0.670589 11.00000 0.02011 0.01846 = 0.01914 -0.00126 -0.00072 -0.00454 N5 3 0.241774 0.987011 -0.146201 11.00000 0.01752 0.02073 = 0.01691 0.00178 0.00559 0.00461 AFIX 43 H5A 2 0.248829 1.006016 -0.177449 11.00000 -1.20000 AFIX 0 N6 3 0.214794 0.499587 1.160931 11.00000 0.01339 0.02555 = 0.01750 -0.00024 -0.00430 0.00425 AFIX 43 H6A 2 0.212790 0.483911 1.192863 11.00000 -1.20000 AFIX 0 O1 4 0.406352 0.911046 0.755713 11.00000 0.01047 0.01031 = 0.02197 -0.00088 -0.00237 -0.00222 O2 4 0.911869 0.833993 0.755647 11.00000 0.01688 0.03786 = 0.00967 0.00399 0.00106 -0.00163 OW1 4 0.486203 0.718068 0.754845 11.00000 0.01373 0.01365 = 0.01591 0.00293 -0.00070 -0.00333 OW2 4 0.790200 0.591869 0.740162 11.00000 0.02022 0.01296 = 0.02005 0.00127 0.00383 0.00142 S1 5 0.674511 0.789055 0.947473 11.00000 0.02854 0.03027 = 0.01009 0.00501 -0.00010 0.00191 S2 5 0.839883 1.173014 0.838801 11.00000 0.03519 0.01067 = 0.02097 -0.00376 -0.00514 0.00269 S3 5 0.773557 1.157716 0.646338 11.00000 0.03428 0.01614 = 0.01984 0.00691 0.00998 0.00776 S4 5 0.689527 0.784570 0.566050 11.00000 0.03414 0.03217 = 0.01245 -0.00483 0.00353 0.00227 I1 6 0.196838 0.882435 0.028448 11.00000 0.02147 0.02360 = 0.01311 -0.00018 0.00098 0.00355 I2 6 0.233885 0.589644 0.983566 11.00000 0.02203 0.02435 = 0.01316 -0.00094 0.00123 -0.00609 U1 7 0.658644 0.871200 0.755425 11.00000 0.01088 0.00928 = 0.00994 0.00066 0.00063 -0.00017 HKLF 4 REM P21onc in P2(1)/c REM R1 = 0.0570 for 5970 Fo > 4sig(Fo) and 0.0736 for all 7328 data REM 280 parameters refined using 0 restraints END WGHT 0.0000 115.2038 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, y-1/2, -z+1/2 HTAB C8 S3_$1 EQIV $2 x-1, y, z-1 HTAB C9 O2_$2 EQIV $3 -x+1, -y+1, -z+2 HTAB C11 I2_$3 EQIV $4 -x+1, -y+2, -z+2 HTAB C13 S2_$4 EQIV $5 x, y, z-1 HTAB N5 O1_$5 EQIV $6 -x+1, y+1/2, -z+1/2 HTAB N5 OW2_$6 EQIV $7 x, -y+3/2, z+1/2 HTAB N6 O1_$7 HTAB N6 OW2_$3 REM Highest difference peak 5.291, deepest hole -3.046, 1-sigma level 0.347 Q1 1 0.6575 0.8687 0.7220 11.00000 0.05 5.29 Q2 1 0.1956 0.6234 0.9576 11.00000 0.05 4.63 Q3 1 0.2341 0.9127 0.0022 11.00000 0.05 2.82 Q4 1 0.6605 0.8745 0.7903 11.00000 0.05 2.72 Q5 1 1.0173 0.8750 0.7604 11.00000 0.05 2.47 Q6 1 0.4180 0.5855 0.9811 11.00000 0.05 2.46 Q7 1 0.5203 1.1226 -0.0279 11.00000 0.05 2.36 Q8 1 0.1985 0.6324 1.0004 11.00000 0.05 2.15 Q9 1 0.0876 0.5790 0.9814 11.00000 0.05 1.98 Q10 1 0.3466 0.8796 0.0318 11.00000 0.05 1.90 Q11 1 0.4968 0.8334 0.7598 11.00000 0.05 1.57 Q12 1 0.5122 0.9175 0.7622 11.00000 0.05 1.54 Q13 1 0.8524 0.8784 0.7538 11.00000 0.05 1.51 Q14 1 0.2284 1.0950 -0.0095 11.00000 0.05 1.47 Q15 1 0.2387 1.0820 -0.0221 11.00000 0.05 1.33 Q16 1 0.9133 0.8184 0.7305 11.00000 0.05 1.32 Q17 1 0.2446 0.8190 0.0104 11.00000 0.05 1.32 Q18 1 0.4425 0.7160 0.7253 11.00000 0.05 1.26 Q19 1 0.7793 0.9082 0.7223 11.00000 0.05 1.26 Q20 1 0.5956 0.6190 0.7223 11.00000 0.05 1.24 Q21 1 0.2000 1.1225 -0.0401 11.00000 0.05 1.23 Q22 1 0.0368 0.8648 0.0331 11.00000 0.05 1.21 Q23 1 0.1016 0.8741 0.0133 11.00000 0.05 1.21 Q24 1 0.5328 0.9153 0.9298 11.00000 0.05 1.20 Q25 1 0.7587 1.1776 0.8014 11.00000 0.05 1.20 ; _shelx_res_checksum 24503 _shelx_hkl_file ; 1 0 0 26.74 1.12 1 0 0 26.69 1.25 1 0 0 27.07 1.25 -1 0 0 26.91 1.21 2 0 0 1000.00 36.52 2 0 0 985.92 36.85 -2 0 0 894.61 36.12 2 0 0 993.56 34.95 3 0 0 6.83 0.59 3 0 0 6.16 0.79 3 0 0 6.08 0.77 -3 0 0 7.02 0.79 -4 0 0 2.60 0.60 4 0 0 3.09 0.68 4 0 0 4.05 0.53 4 0 0 4.32 0.76 5 0 0 25.03 1.37 5 0 0 26.07 1.86 -5 0 0 24.75 1.66 -6 0 0 31.31 2.26 6 0 0 35.11 2.43 -6 0 0 34.56 2.15 7 0 0 94.79 5.04 -7 0 0 95.25 4.92 -8 0 0 1.11 1.10 8 0 0 0.09 1.06 9 0 0 28.49 3.20 0 -1 0 0.06 0.06 0 -1 0 0.06 0.09 0 -1 0 0.04 0.06 0 1 0 -0.11 0.05 0 1 0 0.17 0.09 0 1 0 -0.01 0.03 0 1 0 -0.01 0.06 1 -1 0 0.13 0.19 -1 -1 0 0.53 0.14 1 -1 0 0.25 0.22 -1 -1 0 0.44 0.21 1 1 0 0.33 0.20 -1 1 0 0.34 0.14 -1 1 0 0.03 0.22 1 1 0 0.14 0.22 -1 1 0 0.55 0.15 2 -1 0 338.33 13.04 2 -1 0 350.36 12.23 2 -1 0 330.57 12.88 -2 -1 0 319.18 12.99 -2 -1 0 322.71 12.67 -2 1 0 334.71 12.81 2 1 0 338.07 12.93 2 1 0 354.02 12.32 3 -1 0 51.97 2.10 -3 -1 0 51.91 2.31 3 -1 0 49.45 2.44 -3 -1 0 52.89 2.46 3 -1 0 50.71 2.48 -3 1 0 50.14 2.43 3 1 0 54.20 2.52 3 1 0 51.66 2.19 4 -1 0 231.14 9.03 4 -1 0 220.70 8.28 -4 -1 0 220.05 9.04 4 -1 0 209.85 9.05 -4 -1 0 218.01 8.75 4 1 0 217.31 8.37 4 1 0 221.80 9.06 -4 1 0 234.37 8.93 5 -1 0 66.93 2.78 -5 -1 0 72.01 3.38 5 -1 0 62.77 3.37 5 -1 0 67.41 3.38 -5 -1 0 66.62 3.15 5 1 0 62.66 3.37 5 1 0 62.20 2.84 -5 1 0 64.25 3.24 6 -1 0 7.57 1.25 -6 -1 0 5.96 1.00 -6 -1 0 5.25 1.10 -6 1 0 10.73 1.36 6 1 0 7.30 1.24 7 -1 0 6.16 1.42 -7 -1 0 7.76 1.38 -7 1 0 8.53 1.49 7 1 0 7.82 1.53 -7 1 0 9.92 1.43 -8 -1 0 8.94 1.61 8 -1 0 9.89 1.80 -8 1 0 7.08 1.58 8 1 0 7.50 1.65 9 -1 0 0.86 1.33 9 1 0 0.85 1.21 0 -2 0 13.69 0.78 0 -2 0 14.49 0.70 0 2 0 14.64 0.71 0 2 0 15.15 0.76 -1 -2 0 14.53 0.86 1 -2 0 16.39 0.90 1 -2 0 16.47 0.80 1 2 0 15.93 0.88 -1 2 0 17.14 0.74 1 2 0 15.88 0.87 -1 2 0 15.82 0.91 2 -2 0 61.70 2.83 -2 -2 0 71.43 2.93 -2 -2 0 67.88 2.69 2 -2 0 65.46 2.95 2 2 0 66.46 2.76 -2 2 0 70.81 2.97 2 2 0 67.19 2.94 -2 2 0 68.99 2.59 -2 2 0 69.20 2.62 3 -2 0 16.97 1.14 -3 -2 0 16.72 1.13 -3 -2 0 16.46 0.96 3 -2 0 15.52 1.16 3 2 0 15.25 0.98 3 2 0 18.43 1.22 -3 2 0 18.06 1.22 -4 -2 0 45.65 2.32 4 -2 0 44.77 2.30 -4 -2 0 38.12 2.03 4 -2 0 43.07 2.33 4 2 0 40.76 2.33 4 2 0 44.87 2.03 -4 2 0 41.70 2.31 5 -2 0 9.55 1.25 5 -2 0 11.50 1.37 -5 -2 0 9.74 1.03 -5 -2 0 10.14 1.23 5 2 0 11.30 1.38 -5 2 0 9.61 1.20 5 2 0 10.83 1.02 6 -2 0 25.90 2.01 6 -2 0 23.73 1.96 -6 -2 0 20.64 1.78 -6 2 0 20.60 1.82 6 2 0 19.56 2.08 -7 -2 0 0.50 0.77 7 -2 0 0.39 0.78 7 2 0 -0.21 0.86 -7 2 0 0.17 0.74 -8 -2 0 1.93 1.13 8 -2 0 2.72 1.20 8 2 0 3.97 1.46 -8 2 0 1.82 1.02 9 -2 0 0.24 1.29 9 2 0 -0.66 1.21 0 -3 0 0.18 0.32 0 -3 0 -0.01 0.21 0 3 0 0.19 0.29 0 3 0 -0.10 0.19 1 -3 0 162.11 6.59 1 -3 0 167.90 6.38 -1 -3 0 181.25 6.59 -1 3 0 169.24 6.18 1 3 0 165.03 6.34 -1 3 0 155.67 6.48 1 3 0 161.96 6.49 2 -3 0 92.72 3.83 2 -3 0 86.47 3.64 -2 -3 0 87.50 3.76 -2 -3 0 88.47 3.39 -2 3 0 88.95 3.80 -2 3 0 86.42 3.38 2 3 0 92.20 3.78 2 3 0 89.55 3.62 3 -3 0 72.45 3.38 3 -3 0 72.00 3.24 -3 -3 0 73.89 3.34 -3 -3 0 65.80 2.95 -3 3 0 75.97 2.88 3 3 0 73.63 3.38 3 3 0 78.98 3.16 -3 3 0 79.38 3.43 -4 -3 0 93.57 3.94 4 -3 0 96.81 4.42 4 -3 0 98.33 4.31 -4 -3 0 95.18 4.34 -4 3 0 99.17 4.41 4 3 0 96.87 4.02 4 3 0 97.02 4.43 -4 3 0 94.16 3.73 5 -3 0 38.73 2.33 -5 -3 0 34.69 1.88 -5 -3 0 34.93 2.20 5 -3 0 38.45 2.28 5 3 0 39.98 2.40 5 3 0 37.25 1.97 -5 3 0 36.81 2.31 -6 -3 0 17.60 1.82 6 -3 0 19.34 1.99 6 -3 0 19.01 1.90 6 3 0 13.46 1.35 -6 3 0 14.99 1.70 6 3 0 18.16 1.95 7 -3 0 6.01 1.36 -7 -3 0 4.56 1.20 7 -3 0 5.22 1.31 -7 3 0 5.49 1.27 7 3 0 2.86 1.19 -8 -3 0 1.51 1.04 8 -3 0 -0.04 1.04 -8 3 0 2.03 1.11 8 3 0 1.30 1.18 -8 3 0 1.89 1.06 9 -3 0 3.78 1.55 0 -4 0 465.93 18.26 0 -4 0 489.96 17.94 0 4 0 465.11 17.41 0 4 0 475.92 17.81 1 -4 0 0.77 0.28 -1 -4 0 0.68 0.37 1 -4 0 1.20 0.42 1 4 0 1.22 0.44 1 4 0 0.95 0.18 -1 4 0 0.00 0.35 1 4 0 1.06 0.34 1 4 0 0.75 0.17 -1 4 0 1.08 0.36 2 -4 0 115.90 4.80 2 -4 0 120.75 5.05 -2 -4 0 125.47 5.01 -2 4 0 120.11 4.57 -2 4 0 120.24 5.01 2 4 0 117.33 4.97 2 4 0 120.55 4.84 -3 -4 0 2.46 0.61 -3 -4 0 1.22 0.24 3 -4 0 2.26 0.60 3 -4 0 1.52 0.46 -3 4 0 1.82 0.34 3 4 0 1.84 0.54 -3 4 0 1.18 0.59 3 4 0 1.36 0.52 4 -4 0 16.86 1.36 -4 -4 0 15.28 1.27 4 -4 0 14.50 1.21 -4 -4 0 15.39 0.89 -4 4 0 15.83 0.87 4 4 0 15.05 1.17 -4 4 0 15.17 1.50 4 4 0 14.73 1.31 5 -4 0 32.05 2.03 5 -4 0 28.91 2.10 -5 -4 0 31.12 2.11 5 4 0 35.30 2.29 -5 4 0 37.22 2.29 5 4 0 30.77 1.86 6 -4 0 36.17 2.39 -6 -4 0 33.31 2.39 6 -4 0 37.42 2.50 6 4 0 33.07 2.51 -6 4 0 34.14 2.44 6 4 0 35.00 2.06 -7 -4 0 54.09 3.34 7 -4 0 54.94 3.43 7 -4 0 52.25 3.31 7 4 0 48.22 3.42 -7 4 0 52.92 3.37 8 -4 0 1.68 1.25 -8 -4 0 3.49 1.34 -8 4 0 4.53 1.35 8 4 0 2.77 1.32 0 -5 0 -0.15 0.37 0 -5 0 -0.52 0.24 0 5 0 0.27 0.38 0 5 0 0.29 0.28 1 -5 0 7.89 0.87 -1 -5 0 8.44 0.85 1 -5 0 8.06 0.60 -1 5 0 7.78 0.80 1 5 0 7.96 0.75 1 5 0 7.10 0.49 -1 5 0 8.55 0.77 1 5 0 8.53 0.93 2 -5 0 89.06 3.95 2 -5 0 89.02 3.68 -2 -5 0 91.33 3.92 -2 5 0 85.44 3.92 2 5 0 90.68 3.85 2 5 0 93.12 3.89 -2 5 0 87.76 3.55 -3 -5 0 11.52 1.15 3 -5 0 11.25 1.16 3 -5 0 10.06 0.87 -3 5 0 10.90 1.23 -3 5 0 9.49 0.69 3 5 0 10.31 1.11 3 5 0 11.34 1.14 4 -5 0 35.30 2.05 -4 -5 0 38.16 1.59 -4 -5 0 38.81 2.19 4 -5 0 40.65 2.28 -4 5 0 37.58 2.31 -4 5 0 38.14 1.70 4 5 0 38.70 2.28 4 5 0 36.73 2.07 5 -5 0 10.90 1.41 -5 -5 0 10.67 1.35 5 -5 0 9.27 1.23 -5 5 0 10.09 1.45 5 5 0 9.51 1.36 5 5 0 10.14 1.20 6 -5 0 1.63 0.78 -6 -5 0 2.26 0.87 6 -5 0 2.38 0.96 6 5 0 1.82 0.92 -6 5 0 1.25 0.94 6 5 0 3.00 0.82 7 -5 0 1.86 0.93 7 -5 0 -0.09 0.76 -7 -5 0 1.48 0.98 -7 5 0 -0.28 0.84 7 5 0 -0.42 0.86 8 -5 0 19.31 2.37 -8 -5 0 12.78 2.01 8 5 0 16.09 2.23 -8 5 0 16.39 2.13 0 -6 0 8.85 0.71 0 -6 0 9.13 0.98 0 6 0 9.21 0.93 0 6 0 8.16 0.70 1 -6 0 0.36 0.44 -1 -6 0 0.55 0.42 1 -6 0 0.19 0.29 -1 6 0 0.20 0.38 -1 6 0 -0.07 0.36 1 6 0 -0.23 0.40 1 6 0 0.40 0.24 1 6 0 -0.08 0.29 -2 -6 0 16.35 1.24 2 -6 0 17.00 1.01 2 -6 0 15.56 1.23 2 6 0 17.89 1.20 2 6 0 19.04 1.34 -2 6 0 15.33 1.04 -2 6 0 18.41 1.31 3 -6 0 13.48 1.02 3 -6 0 13.22 1.22 -3 -6 0 13.59 1.16 -3 6 0 14.91 0.91 -3 6 0 14.61 1.28 3 6 0 13.54 1.33 3 6 0 12.91 1.28 -4 -6 0 22.12 1.67 4 -6 0 24.77 1.78 4 -6 0 24.16 1.55 4 6 0 25.37 1.78 -4 6 0 22.85 1.81 -4 6 0 25.10 1.27 4 6 0 25.67 1.73 -5 -6 0 12.64 1.48 5 -6 0 10.71 1.43 5 -6 0 9.37 1.22 -5 6 0 14.37 1.78 5 6 0 14.26 1.62 5 6 0 9.57 1.27 6 -6 0 4.87 1.20 -6 -6 0 6.78 1.24 6 -6 0 6.83 1.19 6 6 0 7.67 1.42 -6 6 0 7.98 1.42 6 6 0 6.81 1.12 7 -6 0 1.45 0.97 7 -6 0 2.64 1.06 -7 -6 0 2.62 1.08 -7 6 0 2.45 1.15 7 6 0 3.82 1.28 -8 -6 0 -0.36 0.87 8 -6 0 1.03 1.13 8 6 0 1.08 1.10 -8 6 0 -1.29 0.89 0 -7 0 0.47 0.34 0 -7 0 -0.35 0.42 0 7 0 0.67 0.47 0 7 0 -0.50 0.29 -1 -7 0 26.70 1.71 1 -7 0 31.47 1.44 1 -7 0 29.16 1.74 1 7 0 24.20 1.67 1 7 0 27.03 1.33 -1 7 0 26.14 1.58 -1 7 0 28.17 1.59 -2 -7 0 33.26 1.94 2 -7 0 31.70 1.64 2 -7 0 37.35 2.08 -2 7 0 36.01 1.76 2 7 0 32.94 2.01 2 7 0 34.48 1.86 -2 7 0 33.56 1.97 3 -7 0 18.68 1.21 -3 -7 0 19.46 1.46 3 -7 0 18.60 1.48 -3 7 0 18.65 1.16 3 7 0 17.93 1.49 -3 7 0 21.10 1.56 3 7 0 18.83 1.40 4 -7 0 42.26 2.52 4 -7 0 40.69 2.19 -4 -7 0 42.85 2.43 -4 7 0 40.15 1.93 4 7 0 42.66 2.45 4 7 0 41.02 2.44 -4 7 0 38.57 2.52 5 -7 0 24.26 1.77 -5 -7 0 22.74 1.84 5 -7 0 23.62 1.95 5 7 0 23.85 1.83 -5 7 0 24.88 2.07 5 7 0 23.21 1.98 -6 -7 0 6.49 1.27 6 -7 0 6.01 1.31 6 -7 0 5.50 1.13 6 7 0 6.35 1.30 6 7 0 4.79 1.07 -6 7 0 5.31 1.34 -7 -7 0 1.70 1.12 7 -7 0 1.05 0.98 7 7 0 2.92 1.20 -7 7 0 4.18 1.35 -8 -7 0 0.57 1.09 8 -7 0 0.86 1.15 8 7 0 0.82 1.12 -8 7 0 0.34 1.20 0 -8 0 95.95 4.32 0 -8 0 95.71 3.98 0 8 0 89.34 4.11 0 8 0 96.74 4.04 -1 -8 0 6.42 0.94 -1 -8 0 5.87 0.77 1 -8 0 8.71 0.80 1 -8 0 8.04 1.04 -1 8 0 7.28 0.92 1 8 0 8.22 1.08 1 8 0 7.33 0.69 -1 8 0 6.01 0.84 -2 -8 0 32.46 1.95 2 -8 0 29.53 1.94 2 -8 0 30.79 1.56 2 8 0 30.43 1.75 -2 8 0 26.20 1.80 -2 8 0 28.52 1.65 2 8 0 33.17 2.01 3 -8 0 13.89 1.48 -3 -8 0 14.17 1.43 3 -8 0 12.92 1.01 -3 8 0 13.03 1.50 -3 8 0 12.99 1.03 3 8 0 13.14 1.48 3 8 0 12.33 1.31 4 -8 0 14.03 1.58 -4 -8 0 12.88 1.46 4 -8 0 11.23 1.15 4 8 0 10.84 1.42 -4 8 0 13.51 1.63 -4 8 0 11.56 0.95 4 8 0 10.05 1.33 5 -8 0 2.10 0.86 5 -8 0 1.52 0.69 -5 -8 0 2.29 0.92 5 8 0 1.11 0.80 5 8 0 0.09 0.68 -5 8 0 0.87 0.91 6 -8 0 46.35 3.05 -6 -8 0 40.31 2.78 6 8 0 45.09 3.05 6 8 0 41.31 2.74 -6 8 0 42.11 3.05 -7 -8 0 17.91 2.26 7 -8 0 23.07 2.53 7 8 0 19.72 2.40 -7 8 0 20.00 2.46 -8 -8 0 5.59 1.55 8 -8 0 7.19 1.71 -8 8 0 6.72 1.80 8 8 0 6.30 1.77 0 -9 0 0.30 0.52 0 -9 0 0.08 0.35 0 9 0 -0.11 0.44 0 9 0 0.00 0.35 1 -9 0 64.84 3.23 1 -9 0 63.14 2.78 -1 -9 0 64.08 3.21 -1 -9 0 54.80 2.84 -1 9 0 63.13 2.98 1 9 0 62.44 2.72 1 9 0 63.39 3.14 -1 9 0 60.25 2.99 -2 -9 0 25.36 1.79 2 -9 0 25.01 1.38 2 -9 0 27.16 1.86 -2 9 0 25.36 1.59 -2 9 0 23.03 1.71 2 9 0 25.75 1.62 2 9 0 23.91 1.83 3 -9 0 3.84 0.89 3 -9 0 2.75 0.58 -3 -9 0 3.23 0.85 3 9 0 4.63 1.00 -3 9 0 2.23 0.77 -3 9 0 4.65 0.76 3 9 0 4.35 0.84 4 -9 0 10.85 1.12 4 -9 0 12.95 1.59 -4 -9 0 11.12 1.45 -4 9 0 11.19 1.50 4 9 0 10.75 1.48 4 9 0 9.89 1.31 -5 -9 0 1.88 0.95 5 -9 0 5.34 1.23 5 9 0 3.39 1.04 -5 9 0 4.05 1.22 5 9 0 3.47 0.99 6 -9 0 0.47 0.89 -6 -9 0 2.66 1.00 -6 9 0 1.99 1.19 6 9 0 0.91 0.92 6 9 0 2.97 1.09 -7 -9 0 -0.92 0.84 7 -9 0 -0.32 1.00 -7 9 0 0.58 1.18 7 9 0 -0.37 0.95 -8 -9 0 12.41 2.11 -8 9 0 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11 0 16.45 1.57 -1 11 0 17.44 1.45 1 11 0 17.04 1.16 -2 -11 0 50.40 2.71 2 -11 0 52.88 3.04 -2 -11 0 53.42 3.05 -2 11 0 47.01 2.80 -2 11 0 47.94 2.64 2 11 0 52.02 2.97 -3 -11 0 0.27 0.77 3 -11 0 -0.14 0.71 -3 11 0 -0.74 0.62 3 11 0 -0.59 0.65 -3 11 0 0.52 0.56 3 11 0 1.06 0.64 -4 -11 0 31.48 2.43 4 -11 0 34.78 2.55 -4 11 0 32.34 2.50 4 11 0 35.15 2.34 4 11 0 33.09 2.52 5 -11 0 9.39 1.56 -5 -11 0 6.05 1.33 5 11 0 6.79 1.38 -5 11 0 5.31 1.30 5 11 0 6.55 1.42 6 -11 0 0.96 1.03 -6 -11 0 2.81 1.17 -6 11 0 0.18 1.13 6 11 0 0.95 1.04 6 11 0 2.06 1.12 7 -11 0 0.26 1.08 -7 -11 0 -0.09 0.97 7 11 0 -0.05 1.10 7 11 0 0.56 1.15 -7 11 0 0.43 1.24 0 -12 0 31.98 1.85 0 -12 0 29.31 2.24 0 12 0 33.90 1.97 0 12 0 35.08 2.26 -1 -12 0 28.07 1.74 -1 -12 0 26.62 2.08 1 -12 0 23.52 2.00 1 12 0 24.56 1.60 -1 12 0 24.84 1.80 1 12 0 25.63 2.00 -1 12 0 23.14 1.83 -2 -12 0 0.66 0.85 2 -12 0 1.76 0.81 -2 -12 0 1.07 0.66 2 12 0 1.02 0.74 -2 12 0 1.16 0.76 -2 12 0 2.76 0.80 -3 -12 0 58.84 3.16 3 -12 0 58.26 3.47 -3 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33 -1.10 0.87 0 -3 -33 16.27 2.00 0 -3 -33 13.55 1.90 0 -3 -33 16.83 2.35 0 -3 33 16.59 2.36 0 3 33 18.19 2.51 0 3 -33 17.36 2.14 -1 -3 -33 3.52 1.43 -1 -3 -33 3.15 1.21 -1 -3 -33 2.30 1.06 1 -3 33 4.76 1.60 1 3 33 2.26 1.28 -1 3 -33 2.14 1.09 -2 -3 -33 0.03 1.21 2 -3 33 1.23 1.29 -2 -3 -33 0.83 1.02 -2 -3 -33 1.94 1.12 -2 3 -33 1.68 0.97 2 3 33 3.26 1.35 -3 -3 -33 0.69 1.19 3 3 33 0.19 1.17 -3 -4 33 2.74 1.34 -2 -4 33 -0.44 0.98 2 -4 -33 0.71 1.08 -2 4 33 -0.90 0.97 -1 -4 33 5.33 1.47 1 -4 -33 4.58 1.51 1 4 -33 2.84 1.18 -1 4 33 4.98 1.63 0 -4 -33 -0.36 0.95 0 -4 33 -0.01 1.10 0 -4 -33 1.99 1.04 0 -4 -33 0.52 0.94 0 4 33 1.81 1.31 0 4 -33 2.23 1.04 -1 -4 -33 2.48 1.35 1 -4 33 3.50 1.41 -1 -4 -33 4.32 1.23 -1 -4 -33 3.58 1.19 1 4 33 4.40 1.48 -1 4 -33 3.62 1.31 -2 -4 -33 1.26 1.04 -2 -4 -33 -0.65 1.16 -2 -4 -33 0.39 0.89 2 -4 33 -0.44 1.13 2 4 33 0.37 1.06 -2 4 -33 0.84 0.95 -3 -4 -33 1.54 1.27 3 4 33 0.11 1.23 -3 -5 33 2.54 1.28 2 -5 -33 32.38 3.30 -2 -5 33 32.65 2.84 -2 5 33 29.88 3.50 -1 -5 33 1.68 1.26 1 -5 -33 2.88 1.42 1 5 -33 1.33 1.07 -1 5 33 3.07 1.53 0 -5 33 39.98 3.39 0 -5 -33 43.16 3.13 0 -5 -33 44.09 3.62 0 -5 -33 49.80 3.19 0 5 33 45.32 3.56 0 5 -33 53.29 3.36 -1 -5 -33 -0.01 0.90 1 -5 33 2.96 1.33 -1 -5 -33 0.23 0.89 -1 -5 -33 1.04 1.28 -1 5 -33 0.38 0.89 1 5 33 -0.75 1.04 -2 -5 -33 5.26 1.46 -2 -5 -33 6.08 1.79 2 5 33 7.34 1.87 3 5 33 0.77 1.23 -3 -6 33 0.22 1.00 -2 -6 33 15.25 2.16 -1 -6 33 3.82 1.42 1 -6 -33 5.52 1.70 -1 6 33 3.85 1.58 1 6 -33 3.66 1.32 0 -6 33 15.60 2.31 0 -6 -33 8.65 1.99 0 6 -33 9.83 1.85 0 6 33 8.92 1.94 -1 -6 -33 0.75 1.25 1 -6 33 1.27 1.37 -1 6 -33 0.15 1.04 1 6 33 0.08 1.12 -2 -6 -33 37.37 3.90 2 6 33 40.54 3.40 -2 -7 33 10.35 1.83 2 7 -33 5.74 1.51 -1 -7 33 0.17 1.09 1 7 -33 -0.57 0.92 0 -7 33 13.02 2.16 0 -7 -33 11.44 2.51 0 7 33 15.80 2.49 0 7 -33 13.20 2.02 1 7 33 5.54 1.77 2 7 33 -0.57 1.17 2 8 -33 0.95 1.11 1 8 -33 12.74 2.07 0 8 33 1.31 1.43 1 8 33 7.00 1.57 1 8 33 10.36 2.06 1 9 33 -0.91 1.06 3 0 -34 3.96 1.38 2 0 -34 4.80 1.34 -2 0 34 2.41 1.30 1 0 -34 27.00 2.73 -1 0 34 22.59 2.66 0 0 -34 1.43 1.11 0 0 34 2.04 1.28 0 0 -34 1.41 1.11 1 0 34 4.44 1.46 -1 0 -34 3.93 1.30 -2 0 -34 10.60 1.80 2 0 34 10.02 2.04 3 -1 -34 4.19 1.52 3 1 -34 1.80 1.07 2 -1 -34 -0.32 0.99 -2 -1 34 0.01 1.03 -2 1 34 -0.51 1.00 2 1 -34 0.16 0.89 -1 -1 34 -1.35 0.95 1 -1 -34 0.41 0.93 1 1 -34 -1.19 0.78 1 1 -34 0.43 0.95 -1 1 34 -0.81 0.98 0 -1 -34 2.52 1.12 0 -1 -34 0.50 1.08 0 -1 34 2.73 1.34 0 1 34 5.97 1.66 0 1 -34 5.07 1.25 -1 -1 -34 9.45 1.83 -1 -1 -34 4.46 1.32 1 -1 34 8.39 1.93 -1 1 -34 7.99 1.56 1 1 34 7.13 1.76 -2 -1 -34 0.22 0.93 2 -1 34 0.10 1.16 -2 -1 -34 2.02 1.04 2 1 34 0.84 1.25 -2 1 -34 -0.75 0.83 3 2 -34 0.90 1.08 -2 -2 34 -0.25 1.01 2 -2 -34 0.45 1.08 1 -2 -34 4.12 1.41 -1 -2 34 3.24 1.46 -1 2 34 4.30 1.61 1 2 -34 2.87 1.14 0 -2 -34 -0.04 0.99 0 -2 34 1.05 1.11 0 -2 -34 -0.80 0.74 0 2 34 -1.19 0.91 0 2 -34 0.70 0.91 -1 -2 -34 1.70 1.32 -1 -2 -34 0.42 0.88 -1 -2 -34 1.74 1.01 1 -2 34 4.84 1.63 1 2 34 0.90 1.12 -1 2 -34 2.08 1.08 -2 -2 -34 1.58 1.12 -2 -2 -34 3.45 1.50 -2 -2 -34 2.86 1.20 2 2 34 3.30 1.41 -2 -3 34 1.98 1.28 2 -3 -34 2.39 1.35 1 -3 -34 1.43 1.22 -1 -3 34 3.03 1.40 -1 3 34 0.72 1.14 1 3 -34 0.58 0.90 0 -3 -34 8.31 1.55 0 -3 -34 10.16 1.92 0 -3 -34 8.04 1.58 0 -3 34 7.35 1.74 0 3 34 8.56 1.87 0 3 -34 7.11 1.45 1 -3 34 8.88 1.90 -1 -3 -34 11.13 1.76 -1 -3 -34 7.22 1.61 -1 -3 -34 8.51 1.92 -1 3 -34 7.31 1.58 1 3 34 9.91 2.06 -2 -3 -34 -0.34 0.91 -2 -3 -34 0.93 1.24 -2 -3 -34 1.54 1.18 2 3 34 -0.66 1.14 -2 -4 34 16.08 2.51 1 -4 -34 27.63 3.08 -1 -4 34 33.03 3.27 -1 4 34 31.53 3.30 1 4 -34 32.21 2.68 0 -4 34 3.18 1.41 0 -4 -34 0.50 0.93 0 -4 -34 0.80 1.22 0 -4 -34 -0.62 0.83 0 4 34 1.36 1.22 0 4 -34 -0.74 0.87 -1 -4 -34 7.56 1.60 -1 -4 -34 7.06 1.83 -1 -4 -34 8.87 1.69 1 4 34 6.67 1.65 -1 4 -34 8.89 1.66 -2 -4 -34 14.59 2.35 2 4 34 16.37 2.44 1 -5 -34 3.12 1.51 -1 -5 34 2.42 1.41 1 5 -34 1.71 1.10 0 -5 -34 15.57 2.47 0 5 -34 14.91 2.11 0 5 34 17.31 2.54 -1 -5 -34 17.39 2.33 -1 -5 -34 19.28 2.45 -1 -5 -34 22.33 2.85 1 5 34 15.77 2.44 2 5 34 -0.78 1.13 1 6 -34 -0.04 0.89 0 6 -34 -1.58 0.72 -1 -6 -34 0.99 1.13 -1 -6 -34 -0.19 0.90 1 6 34 0.10 1.27 2 0 -35 0.41 1.00 1 0 -35 -0.08 0.99 0 0 -35 0.85 0.89 -1 0 -35 -1.00 0.82 2 -1 -35 0.62 1.12 2 1 -35 0.86 1.01 1 -1 -35 1.03 1.06 0 -1 -35 0.89 1.04 0 -1 -35 1.17 1.19 0 1 -35 -0.56 0.85 -1 -1 -35 13.05 1.96 -1 1 -35 16.59 2.20 3 2 -35 9.77 2.01 2 -2 -35 3.13 1.49 1 -2 -35 56.42 3.97 0 -2 -35 0.07 0.93 0 -2 -35 0.50 1.14 0 2 -35 0.45 1.03 -1 -2 -35 28.36 2.92 -1 -2 -35 31.87 3.09 -1 -2 -35 30.56 3.17 -1 2 -35 27.91 2.84 1 -3 -35 1.09 1.18 1 3 -35 0.56 0.94 0 -3 -35 1.46 1.07 0 -3 -35 3.46 1.49 0 3 -35 4.48 1.31 -1 -3 -35 7.99 1.94 -1 -3 -35 8.80 1.69 -1 -3 -35 8.13 1.62 -2 -3 -35 0.17 1.22 1 4 -35 2.75 1.25 0 -4 -35 1.37 1.37 0 4 -35 0.44 1.02 -1 -4 -35 2.91 1.49 -1 -4 -35 3.21 1.28 -1 -4 -35 2.29 1.20 1 5 -35 1.68 1.15 -1 -5 -35 16.04 2.34 1 0 -36 15.45 2.37 0 0 -36 2.43 1.14 1 -1 -36 1.57 1.25 0 -1 -36 20.66 2.48 0 -1 -36 21.84 2.68 0 1 -36 19.82 2.49 1 -2 -36 1.69 1.35 0 -2 -36 -1.51 0.80 0 -2 -36 0.52 1.19 0 2 -36 1.16 1.08 -1 -2 -36 1.62 1.37 1 4 -36 2.92 1.37 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 2048 _symmetry_cell_setting monoclinic _symmetry_space_group_name_h-m 'P 21/c' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? _database_code_depnum_ccdc_archive 'CCDC 967156' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound_3RT _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety '(C5 H5 I N 1+)2,(U O3 C4 H2 N4 S4 2-),(H2 O)' _chemical_formula_sum 'C14 H14 I2 N6 O4 S4 U' _chemical_properties_physical thermochromic _exptl_crystal_recrystallization_method 'Slow Aqueous Evaporation' _chemical_melting_point ? _exptl_crystal_description Prism _exptl_crystal_colour 'Orange (293(2)K) Yellow (100(2)K)' _diffrn_ambient_temperature 293(2) _chemical_formula_weight 950.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 57 _space_group_name_H-M_alt 'P b c m' _space_group_name_Hall '-P 2c 2b' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 6.7452(4) _cell_length_b 15.1032(8) _cell_length_c 25.9377(14) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2642.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3790 _cell_measurement_theta_min 5.394 _cell_measurement_theta_max 44.268 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.379 _exptl_crystal_F_000 1720 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.128 _exptl_crystal_size_mid 0.083 _exptl_crystal_size_min 0.053 _exptl_absorpt_coefficient_mu 8.826 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5821 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_process_details 'SADABS, G. Sheldrick (1999)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_measurement_device_type 'Bruker ApexII CCD' _diffrn_measurement_method 'Omega and Phi Scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26739 _diffrn_reflns_av_unetI/netI 0.0425 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.697 _diffrn_reflns_theta_max 30.323 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.963 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.963 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.963 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 3910 _reflns_number_gt 2658 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'APEX II (Bruker AXS, 2013)' _computing_cell_refinement 'SAINT (Bruker AXS, 2013)' _computing_data_reduction 'SAINT (Bruker AXS, 2013)' _computing_structure_solution 'SIR92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Crystal Maker v.8.2.2 (Palmer 2009)' _computing_publication_material 'WINGX (Farrugia, 2012)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+4.5113P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3910 _refine_ls_number_parameters 148 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0720 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0752 _refine_ls_wR_factor_gt 0.0648 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6572(8) 0.3061(4) 0.8790(2) 0.0478(13) Uani 1 1 d . . . . . C2 C 0.7643(8) 0.5683(4) 0.8223(2) 0.0466(13) Uani 1 1 d . . . . . C3 C 0.1748(9) 0.4100(5) 0.8575(2) 0.0618(16) Uani 1 1 d . . . . . H3 H 0.1413 0.3716 0.8309 0.074 Uiso 1 1 calc R U . . . C4 C 0.1741(9) 0.3811(4) 0.9070(2) 0.0570(14) Uani 1 1 d . . . . . H4 H 0.1408 0.3228 0.9146 0.068 Uiso 1 1 calc R U . . . C5 C 0.2230(8) 0.4389(4) 0.9457(2) 0.0530(14) Uani 1 1 d . . . . . C6 C 0.2711(9) 0.5247(4) 0.9339(3) 0.0655(17) Uani 1 1 d . . . . . H6 H 0.3027 0.5646 0.9600 0.079 Uiso 1 1 calc R U . . . C7 C 0.2720(10) 0.5511(5) 0.8837(3) 0.0681(18) Uani 1 1 d . . . . . H7 H 0.3063 0.6089 0.8751 0.082 Uiso 1 1 calc R U . . . N1 N 0.6335(8) 0.3188(3) 0.83534(17) 0.0613(13) Uani 1 1 d . . . . . N2 N 0.7454(8) 0.4992(3) 0.8051(2) 0.0680(14) Uani 1 1 d . . . . . N3 N 0.2235(7) 0.4936(4) 0.8471(2) 0.0617(13) Uani 1 1 d . . . . . H3A H 0.2235 0.5110 0.8156 0.074 Uiso 1 1 calc R U . . . O1 O 0.4149(8) 0.4111(3) 0.7500 0.0520(13) Uani 1 2 d S T P . . O2 O 0.9098(8) 0.3383(4) 0.7500 0.0588(14) Uani 1 2 d S T P . . OW1 O 0.5026(8) 0.2201(3) 0.7500 0.0536(14) Uani 1 2 d S T P . . OW2 O 0.8064(9) 0.0914(4) 0.7500 0.0676(16) Uani 1 2 d S T P . . S1 S 0.6837(3) 0.28651(14) 0.93915(6) 0.0797(5) Uani 1 1 d . . . . . S2 S 0.7942(4) 0.66619(11) 0.84522(7) 0.0893(7) Uani 1 1 d . . . . . I1 I 0.21818(7) 0.39716(3) 1.02238(2) 0.07331(15) Uani 1 1 d . . . . . U1 U 0.66311(4) 0.37449(2) 0.7500 0.03907(9) Uani 1 2 d S T P . . 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 0.049(3) 0.052(3) 0.042(3) 0.003(2) 0.003(3) -0.007(3) C2 0.049(3) 0.051(3) 0.039(3) -0.004(2) -0.006(2) 0.002(3) C3 0.057(4) 0.073(4) 0.055(4) -0.016(3) -0.007(3) 0.002(3) C4 0.060(4) 0.062(4) 0.049(3) -0.006(3) 0.001(3) 0.006(3) C5 0.041(3) 0.070(4) 0.048(3) -0.012(3) -0.001(2) 0.011(3) C6 0.061(4) 0.066(4) 0.070(5) -0.022(3) 0.005(3) -0.004(3) C7 0.070(4) 0.065(4) 0.069(5) -0.006(4) 0.015(4) -0.010(3) N1 0.080(4) 0.066(3) 0.038(3) 0.003(2) -0.002(2) -0.009(3) N2 0.085(4) 0.054(3) 0.065(3) -0.009(3) -0.008(3) -0.005(3) N3 0.050(3) 0.081(4) 0.054(3) 0.006(3) 0.006(2) 0.008(3) O1 0.053(3) 0.062(3) 0.041(3) 0.000 0.000 0.005(3) O2 0.059(3) 0.063(3) 0.054(3) 0.000 0.000 0.007(3) OW1 0.070(4) 0.041(3) 0.050(3) 0.000 0.000 -0.013(3) OW2 0.069(4) 0.070(4) 0.064(4) 0.000 0.000 -0.007(3) S1 0.0987(14) 0.1031(14) 0.0372(8) 0.0145(8) -0.0030(9) 0.0055(11) S2 0.1417(19) 0.0491(9) 0.0773(13) -0.0188(9) -0.0407(12) 0.0169(11) I1 0.0762(3) 0.0942(3) 0.0495(2) -0.0080(2) -0.0032(2) 0.0189(2) U1 0.04409(16) 0.04013(15) 0.03298(14) 0.000 0.000 -0.00065(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.159(6) . ? C1 S1 1.599(6) . ? C2 N2 1.141(6) . ? C2 S2 1.607(6) . ? C3 N3 1.332(8) . ? C3 C4 1.355(8) . ? C3 H3 0.9300 . ? C4 C5 1.370(8) . ? C4 H4 0.9300 . ? C5 C6 1.371(8) . ? C5 I1 2.087(6) . ? C6 C7 1.363(9) . ? C6 H6 0.9300 . ? C7 N3 1.327(8) . ? C7 H7 0.9300 . ? N1 U1 2.376(5) . ? N2 U1 2.430(5) . ? N3 H3A 0.8600 . ? O1 U1 1.763(5) . ? O2 U1 1.751(5) . ? OW1 U1 2.570(5) . ? U1 N1 2.376(5) 6_557 ? U1 N2 2.430(5) 6_557 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 S1 178.1(6) . . ? N2 C2 S2 178.5(6) . . ? N3 C3 C4 119.8(6) . . ? N3 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C3 C4 C5 119.2(6) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C4 C5 C6 119.8(6) . . ? C4 C5 I1 120.1(5) . . ? C6 C5 I1 120.1(4) . . ? C7 C6 C5 119.3(6) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? N3 C7 C6 119.4(6) . . ? N3 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C1 N1 U1 163.0(5) . . ? C2 N2 U1 164.6(5) . . ? C7 N3 C3 122.5(6) . . ? C7 N3 H3A 118.8 . . ? C3 N3 H3A 118.8 . . ? O2 U1 O1 179.9(2) . . ? O2 U1 N1 88.24(14) . . ? O1 U1 N1 91.78(14) . . ? O2 U1 N1 88.24(14) . 6_557 ? O1 U1 N1 91.78(14) . 6_557 ? N1 U1 N1 137.3(2) . 6_557 ? O2 U1 N2 91.4(2) . 6_557 ? O1 U1 N2 88.52(19) . 6_557 ? N1 U1 N2 147.34(18) . 6_557 ? N1 U1 N2 75.26(17) 6_557 6_557 ? O2 U1 N2 91.4(2) . . ? O1 U1 N2 88.52(19) . . ? N1 U1 N2 75.25(17) . . ? N1 U1 N2 147.35(18) 6_557 . ? N2 U1 N2 72.1(3) 6_557 . ? O2 U1 OW1 96.7(2) . . ? O1 U1 OW1 83.3(2) . . ? N1 U1 OW1 69.12(12) . . ? N1 U1 OW1 69.12(12) 6_557 . ? N2 U1 OW1 143.09(13) 6_557 . ? N2 U1 OW1 143.09(13) . . ? _refine_diff_density_max 1.043 _refine_diff_density_min -1.197 _refine_diff_density_rms 0.140 _shelxl_version_number 2013-4 _shelx_res_file ; TITL Pbcm in Pbcm CELL 0.71073 6.7452 15.1032 25.9377 90.000 90.000 90.000 ZERR 4.00 0.0004 0.0008 0.0014 0.000 0.000 0.000 LATT 1 SYMM - X, - Y, 1/2 + Z SYMM X, 1/2 - Y, - Z SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O S I U UNIT 56 40 24 16 16 8 4 MERG 2 HTAB Bond $H ACTA 50 FMAP 2 PLAN 25 L.S. 24 WGHT 0.025200 4.511300 FVAR 0.04028 C1 1 0.657200 0.306135 0.878960 11.00000 0.04921 0.05208 = 0.04226 0.00301 0.00339 -0.00684 C2 1 0.764299 0.568272 0.822308 11.00000 0.04939 0.05139 = 0.03909 -0.00387 -0.00641 0.00229 C3 1 0.174778 0.410038 0.857515 11.00000 0.05726 0.07280 = 0.05536 -0.01550 -0.00681 0.00172 AFIX 43 H3 2 0.141324 0.371606 0.830886 11.00000 -1.20000 AFIX 0 C4 1 0.174090 0.381142 0.906977 11.00000 0.06009 0.06154 = 0.04934 -0.00571 0.00091 0.00591 AFIX 43 H4 2 0.140830 0.322820 0.914560 11.00000 -1.20000 AFIX 0 C5 1 0.223000 0.438904 0.945686 11.00000 0.04090 0.07025 = 0.04788 -0.01172 -0.00073 0.01072 C6 1 0.271065 0.524742 0.933943 11.00000 0.06061 0.06598 = 0.06979 -0.02188 0.00502 -0.00356 AFIX 43 H6 2 0.302744 0.564594 0.960006 11.00000 -1.20000 AFIX 0 C7 1 0.271972 0.551117 0.883687 11.00000 0.06996 0.06543 = 0.06902 -0.00648 0.01545 -0.00966 AFIX 43 H7 2 0.306277 0.608905 0.875101 11.00000 -1.20000 AFIX 0 N1 3 0.633500 0.318799 0.835337 11.00000 0.08021 0.06568 = 0.03796 0.00349 -0.00248 -0.00936 N2 3 0.745425 0.499240 0.805131 11.00000 0.08500 0.05381 = 0.06519 -0.00948 -0.00817 -0.00522 N3 3 0.223494 0.493633 0.847133 11.00000 0.04962 0.08105 = 0.05449 0.00586 0.00629 0.00842 AFIX 43 H3A 2 0.223517 0.510981 0.815553 11.00000 -1.20000 AFIX 0 O1 4 0.414916 0.411053 0.750000 10.50000 0.05271 0.06225 = 0.04096 0.00000 0.00000 0.00486 O2 4 0.909792 0.338291 0.750000 10.50000 0.05907 0.06344 = 0.05400 0.00000 0.00000 0.00690 OW1 4 0.502622 0.220142 0.750000 10.50000 0.07030 0.04063 = 0.04985 0.00000 0.00000 -0.01295 OW2 4 0.806406 0.091372 0.750000 10.50000 0.06853 0.07016 = 0.06416 0.00000 0.00000 -0.00714 S1 5 0.683723 0.286510 0.939155 11.00000 0.09867 0.10314 = 0.03724 0.01447 -0.00301 0.00547 S2 5 0.794173 0.666195 0.845224 11.00000 0.14171 0.04906 = 0.07727 -0.01883 -0.04069 0.01685 I1 6 0.218183 0.397155 1.022376 11.00000 0.07624 0.09421 = 0.04950 -0.00799 -0.00320 0.01887 U1 7 0.663109 0.374493 0.750000 10.50000 0.04409 0.04013 = 0.03298 0.00000 0.00000 -0.00065 HKLF 4 REM Pbcm in Pbcm REM R1 = 0.0358 for 2658 Fo > 4sig(Fo) and 0.0720 for all 3910 data REM 148 parameters refined using 0 restraints END WGHT 0.0244 4.6176 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, y-1/2, z HTAB C4 S2_$1 EQIV $2 -x+1, -y+1, -z+2 HTAB C6 I1_$2 HTAB N3 O1 EQIV $3 -x+1, y+1/2, z HTAB N3 OW2_$3 REM Highest difference peak 1.043, deepest hole -1.197, 1-sigma level 0.140 Q1 1 0.6624 0.4292 0.7500 10.50000 0.05 1.04 Q2 1 0.7559 0.3080 0.7500 10.50000 0.05 1.00 Q3 1 0.2525 0.4473 1.0180 11.00000 0.05 0.86 Q4 1 0.6490 0.3016 0.7500 10.50000 0.05 0.70 Q5 1 0.5101 0.4182 0.7500 10.50000 0.05 0.70 Q6 1 0.6819 0.1425 0.7500 10.50000 0.05 0.67 Q7 1 0.5042 0.3344 0.7500 10.50000 0.05 0.61 Q8 1 0.7165 0.3383 0.7081 11.00000 0.05 0.59 Q9 1 0.5961 0.1858 0.7500 10.50000 0.05 0.58 Q10 1 0.9313 0.3146 0.7500 10.50000 0.05 0.58 Q11 1 0.2230 0.3856 1.0413 11.00000 0.05 0.57 Q12 1 0.8330 0.6780 0.8215 11.00000 0.05 0.55 Q13 1 0.5831 0.3377 0.7920 11.00000 0.05 0.55 Q14 1 0.1206 0.3956 1.0191 11.00000 0.05 0.54 Q15 1 0.7580 0.3742 0.7500 10.50000 0.05 0.53 Q16 1 0.9349 0.4286 0.7500 10.50000 0.05 0.53 Q17 1 0.8381 0.1565 0.7325 11.00000 0.05 0.51 Q18 1 0.8473 0.3638 0.7325 11.00000 0.05 0.51 Q19 1 0.5906 0.4135 0.7096 11.00000 0.05 0.50 Q20 1 0.4373 0.1960 0.7194 11.00000 0.05 0.50 Q21 1 0.1804 0.3815 0.7500 10.50000 0.05 0.50 Q22 1 0.8208 0.7187 0.8608 11.00000 0.05 0.49 Q23 1 0.7143 0.3709 0.8393 11.00000 0.05 0.49 Q24 1 0.3372 0.3630 1.0183 11.00000 0.05 0.49 Q25 1 0.4731 0.3747 0.7327 11.00000 0.05 0.48 ; _shelx_res_checksum 89314 _shelx_hkl_file ; 1 0 0 28.08 0.82 1 0 0 29.36 0.83 1 0 0 29.50 0.79 2 0 0 1000.00 21.95 2 0 0 972.57 21.40 2 0 0 999.92 22.67 3 0 0 7.04 0.44 3 0 0 6.66 0.48 3 0 0 7.30 0.53 4 0 0 9.56 0.58 4 0 0 7.64 0.73 4 0 0 8.93 0.65 5 0 0 6.39 0.77 5 0 0 6.77 0.78 5 0 0 6.79 0.65 6 0 0 8.00 0.78 6 0 0 10.68 1.06 6 0 0 10.04 1.01 -7 0 0 18.17 1.24 7 0 0 15.77 1.22 7 0 0 17.26 1.25 -8 0 0 0.31 0.45 0 -1 0 -0.05 0.03 0 -1 0 -0.04 0.01 0 1 0 -0.02 0.03 0 1 0 -0.02 0.02 0 -1 0 -0.02 0.02 0 1 0 -0.03 0.03 -1 -1 0 0.25 0.11 1 -1 0 0.27 0.12 1 -1 0 0.40 0.11 1 1 0 0.46 0.13 1 1 0 0.31 0.08 2 1 0 279.47 6.17 2 -1 0 279.50 6.35 2 1 0 274.73 6.45 2 1 0 278.83 6.33 2 -1 0 288.85 6.40 2 -1 0 273.79 6.25 3 -1 0 39.69 1.38 3 -1 0 40.54 1.34 3 -1 0 41.31 1.30 3 1 0 40.07 1.21 3 1 0 43.59 1.41 3 1 0 40.91 1.38 4 1 0 125.85 3.54 4 -1 0 125.34 3.36 4 -1 0 133.98 3.53 4 1 0 131.03 3.29 4 1 0 131.18 3.53 4 -1 0 129.69 3.51 5 -1 0 33.54 1.45 5 1 0 34.82 1.30 5 -1 0 31.84 1.32 5 1 0 33.03 1.48 5 1 0 32.50 1.45 5 -1 0 32.89 1.47 6 1 0 4.53 0.72 6 -1 0 3.91 0.67 6 1 0 4.15 0.59 6 -1 0 3.71 0.57 6 -1 0 3.55 0.67 -7 -1 0 2.24 0.57 7 1 0 3.08 0.71 -7 1 0 2.43 0.63 7 -1 0 3.46 0.76 -7 -1 0 3.56 0.68 8 -1 0 0.17 0.45 -8 -1 0 0.34 0.44 -8 1 0 -0.02 0.48 8 1 0 2.42 0.76 0 2 0 26.44 0.72 0 -2 0 25.43 0.74 0 2 0 26.33 0.71 1 2 0 16.07 0.42 1 2 0 15.15 0.58 1 -2 0 16.69 0.58 1 -2 0 15.91 0.55 -1 2 0 16.39 0.52 -1 -2 0 15.85 0.58 -1 -2 0 16.43 0.44 -2 -2 0 63.78 1.70 2 -2 0 57.34 1.61 2 2 0 61.48 1.47 2 -2 0 57.29 1.67 2 2 0 58.13 1.70 -2 2 0 59.48 1.56 3 2 0 12.65 0.55 3 -2 0 12.34 0.70 3 2 0 13.04 0.71 3 -2 0 12.22 0.63 -3 -2 0 13.84 0.71 3 -2 0 13.55 0.66 4 -2 0 19.04 0.99 4 2 0 18.56 0.79 4 -2 0 19.61 0.93 -4 -2 0 19.66 0.98 4 2 0 18.95 0.99 4 -2 0 18.59 0.90 5 -2 0 3.79 0.53 -5 -2 0 5.01 0.66 5 2 0 5.17 0.72 5 -2 0 4.49 0.67 5 2 0 5.68 0.57 -6 -2 0 3.94 0.66 6 2 0 4.15 0.71 6 2 0 2.97 0.49 -6 2 0 3.00 0.55 6 -2 0 3.56 0.61 6 -2 0 4.18 0.71 -7 2 0 -0.15 0.34 -7 -2 0 0.12 0.32 -7 2 0 -0.52 0.30 7 -2 0 0.30 0.44 7 2 0 -0.08 0.37 -8 -2 0 -0.04 0.40 -8 2 0 0.09 0.49 8 2 0 0.31 0.54 8 -2 0 0.02 0.40 0 -3 0 -0.08 0.11 0 3 0 0.07 0.09 0 3 0 0.01 0.11 -1 3 0 143.47 3.36 -1 -3 0 145.96 3.43 1 3 0 142.01 3.18 -1 -3 0 145.40 3.17 1 3 0 151.52 3.50 1 -3 0 145.31 3.37 1 -3 0 143.52 3.42 -2 3 0 80.92 2.04 2 3 0 79.50 1.87 2 3 0 81.47 2.22 2 -3 0 80.95 2.17 -2 -3 0 78.98 2.15 2 -3 0 80.17 2.12 -3 3 0 55.94 1.61 3 3 0 57.13 1.48 3 -3 0 55.65 1.70 3 3 0 56.12 1.81 3 -3 0 52.94 1.75 -3 -3 0 54.31 1.73 -4 3 0 67.06 2.03 -4 -3 0 72.73 2.25 4 -3 0 68.90 2.25 4 3 0 70.16 2.28 4 3 0 69.78 1.91 4 -3 0 70.03 2.14 -5 3 0 26.78 1.16 5 -3 0 26.74 1.23 5 3 0 24.46 1.30 5 3 0 26.14 1.04 -5 -3 0 25.78 1.28 5 -3 0 26.77 1.36 6 3 0 5.84 0.61 -6 3 0 5.44 0.70 -6 -3 0 5.00 0.75 6 -3 0 5.08 0.77 6 3 0 4.84 0.79 7 -3 0 2.45 0.64 -7 -3 0 2.28 0.56 7 3 0 2.59 0.72 -7 3 0 3.26 0.73 8 3 0 -0.07 0.50 8 -3 0 0.00 0.49 -8 -3 0 -0.24 0.41 -8 3 0 -0.33 0.49 -9 3 0 -0.14 0.56 0 4 0 456.42 10.33 0 4 0 471.58 10.50 0 -4 0 459.51 10.20 -1 4 0 0.54 0.14 1 -4 0 0.44 0.16 1 4 0 0.51 0.11 1 -4 0 0.54 0.19 -1 -4 0 0.29 0.18 1 4 0 0.62 0.19 2 -4 0 115.94 2.89 2 4 0 112.07 3.00 -2 -4 0 114.65 2.94 -2 4 0 114.18 2.82 2 4 0 115.40 2.56 2 -4 0 110.37 2.92 -3 -4 0 2.18 0.38 3 4 0 2.24 0.42 3 -4 0 2.48 0.38 3 -4 0 2.96 0.46 -3 4 0 2.80 0.34 3 4 0 2.63 0.25 -4 -4 0 6.14 0.70 -4 4 0 5.19 0.52 4 4 0 5.56 0.38 4 -4 0 6.02 0.71 4 4 0 5.18 0.65 4 -4 0 4.91 0.59 5 -4 0 5.76 0.69 5 4 0 5.74 0.52 -5 4 0 5.48 0.60 -5 -4 0 5.79 0.75 5 4 0 5.94 0.80 5 -4 0 5.63 0.74 6 -4 0 12.52 1.20 -6 4 0 11.96 0.85 6 4 0 10.52 1.11 -6 -4 0 10.98 1.09 -7 4 0 10.24 1.23 7 4 0 9.40 1.16 -7 -4 0 8.55 1.04 7 -4 0 9.57 1.15 -8 4 0 1.35 0.71 -8 -4 0 0.02 0.47 8 4 0 0.69 0.62 -9 4 0 2.36 0.89 9 4 0 2.59 0.88 0 -5 0 0.00 0.15 0 5 0 -0.08 0.12 1 -5 0 7.27 0.48 -1 -5 0 7.32 0.48 -1 5 0 6.65 0.36 1 5 0 6.11 0.29 -1 5 0 6.16 0.45 1 5 0 5.87 0.44 -2 -5 0 48.35 1.58 2 5 0 49.27 1.62 2 -5 0 51.40 1.53 -2 5 0 49.61 1.40 2 5 0 49.84 1.17 2 -5 0 45.83 1.55 3 -5 0 6.22 0.66 -3 5 0 5.66 0.43 3 -5 0 5.17 0.55 3 5 0 5.76 0.29 3 5 0 5.68 0.64 -3 -5 0 5.62 0.61 -4 5 0 20.01 0.91 4 5 0 20.15 1.11 4 5 0 19.00 0.71 4 -5 0 20.49 1.02 -4 -5 0 20.13 1.07 4 -5 0 19.80 1.10 -5 -5 0 5.72 0.74 5 -5 0 7.06 0.88 5 5 0 6.98 0.83 -5 5 0 6.85 0.70 -6 5 0 0.20 0.43 -6 -5 0 0.42 0.36 6 5 0 -0.03 0.34 6 -5 0 0.52 0.38 7 5 0 1.15 0.59 7 -5 0 -0.14 0.43 -7 -5 0 1.98 0.63 -7 5 0 1.45 0.61 -8 -5 0 1.80 0.67 8 5 0 1.61 0.72 -8 5 0 2.61 0.84 9 5 0 0.09 0.66 -9 5 0 0.45 0.76 0 -6 0 17.62 0.79 0 6 0 16.03 0.69 -1 -6 0 0.16 0.19 -1 6 0 -0.14 0.17 1 -6 0 0.00 0.17 1 6 0 0.01 0.09 1 6 0 0.10 0.18 -1 6 0 0.25 0.14 2 -6 0 11.76 0.72 2 6 0 13.17 0.41 -2 -6 0 15.17 0.78 -2 6 0 12.51 0.57 2 6 0 13.01 0.76 3 6 0 7.91 0.33 3 -6 0 8.51 0.79 -3 6 0 8.61 0.52 3 6 0 9.35 0.70 -3 -6 0 8.70 0.79 3 -6 0 8.93 0.62 4 6 0 8.12 0.89 -4 -6 0 6.40 0.73 4 -6 0 7.88 0.84 -4 6 0 7.28 0.55 4 6 0 7.41 0.38 5 -6 0 3.31 0.64 -5 6 0 4.55 0.58 5 6 0 4.11 0.71 -5 -6 0 4.11 0.65 -6 6 0 1.75 0.54 6 -6 0 1.07 0.48 -6 -6 0 0.97 0.44 6 6 0 0.47 0.44 7 6 0 -0.43 0.40 -7 -6 0 0.08 0.37 7 -6 0 0.59 0.53 -7 6 0 -0.19 0.43 -8 6 0 -0.57 0.44 8 6 0 0.04 0.48 -8 -6 0 -0.03 0.48 9 6 0 -0.52 0.65 -9 6 0 1.57 0.83 0 7 0 0.05 0.17 0 -7 0 0.20 0.20 1 7 0 14.46 0.54 -1 -7 0 14.90 0.79 -1 7 0 14.64 0.64 -1 7 0 12.32 0.72 1 -7 0 13.93 0.77 1 7 0 14.05 0.73 -2 7 0 29.61 1.26 2 -7 0 29.24 1.25 2 7 0 31.25 0.83 -2 -7 0 32.15 1.28 2 7 0 30.39 1.27 -2 7 0 32.20 1.04 -3 -7 0 11.95 0.80 -3 7 0 12.58 0.88 -3 7 0 11.83 0.62 3 -7 0 13.66 0.86 3 7 0 12.34 0.39 3 7 0 12.49 0.83 4 7 0 27.09 1.36 -4 7 0 26.62 1.07 -4 7 0 23.59 1.32 4 -7 0 24.14 1.30 -4 -7 0 22.68 1.22 -5 7 0 9.86 1.10 5 -7 0 13.34 1.23 5 7 0 12.52 1.19 -5 -7 0 13.02 0.98 6 7 0 1.41 0.53 -6 -7 0 2.03 0.57 6 -7 0 2.54 0.68 -6 7 0 1.02 0.55 -7 7 0 0.21 0.57 -7 -7 0 2.26 0.64 7 7 0 1.75 0.66 7 -7 0 1.86 0.70 -8 -7 0 -0.26 0.38 8 7 0 0.27 0.55 -8 7 0 0.44 0.61 0 8 0 73.98 2.13 0 -8 0 72.25 2.26 1 8 0 5.86 0.60 -1 8 0 6.48 0.64 1 -8 0 5.66 0.63 -1 8 0 4.61 0.45 -1 -8 0 4.97 0.61 1 8 0 5.45 0.34 2 8 0 19.62 0.63 -2 -8 0 19.41 1.02 -2 8 0 21.10 0.82 -2 8 0 19.55 1.03 2 -8 0 20.42 1.06 2 8 0 20.22 1.03 3 8 0 12.91 0.89 3 -8 0 13.14 0.92 -3 -8 0 11.80 0.85 -3 8 0 13.90 0.92 -3 8 0 12.75 0.64 4 -8 0 5.26 0.77 -4 -8 0 4.30 0.67 4 8 0 4.11 0.68 -4 8 0 3.93 0.47 -4 8 0 3.98 0.71 -5 8 0 -0.37 0.27 5 8 0 0.55 0.38 -5 -8 0 0.31 0.33 5 -8 0 -0.16 0.31 6 -8 0 9.68 1.15 -6 -8 0 8.74 1.05 6 8 0 9.19 1.14 -6 8 0 9.90 1.26 7 8 0 2.09 0.74 7 -8 0 4.16 0.91 -7 8 0 0.26 0.60 -7 -8 0 2.09 0.66 8 8 0 1.66 0.81 -8 8 0 0.91 0.63 -8 -8 0 -0.11 0.50 0 -9 0 0.25 0.24 0 9 0 0.05 0.19 1 -9 0 39.41 1.60 -1 9 0 41.57 1.41 1 9 0 47.67 1.28 -1 9 0 41.37 1.56 -1 -9 0 39.48 1.60 1 9 0 42.66 1.56 2 -9 0 9.09 0.88 -2 9 0 8.29 0.84 2 9 0 7.96 0.80 2 9 0 6.98 0.39 -2 9 0 9.24 0.55 -2 -9 0 9.04 0.88 -3 -9 0 3.58 0.61 3 9 0 3.30 0.59 -3 9 0 3.10 0.39 -3 9 0 4.03 0.69 3 -9 0 3.83 0.63 4 9 0 3.41 0.65 4 -9 0 2.21 0.57 -4 9 0 2.12 0.62 -4 -9 0 3.05 0.60 5 9 0 0.57 0.46 -5 9 0 0.59 0.51 -5 -9 0 0.65 0.44 5 -9 0 0.98 0.46 -6 -9 0 -0.36 0.38 -6 9 0 0.46 0.51 6 9 0 -0.38 0.39 6 -9 0 1.03 0.59 -7 9 0 0.60 0.57 7 -9 0 1.06 0.65 7 9 0 0.99 0.57 -7 -9 0 0.01 0.45 8 9 0 0.44 0.66 -8 9 0 0.53 0.71 -8 -9 0 0.35 0.57 0 -10 0 39.58 1.60 0 10 0 36.75 1.43 -1 -10 0 0.19 0.27 -1 10 0 0.10 0.21 1 -10 0 -0.11 0.21 1 10 0 0.11 0.25 1 10 0 -0.07 0.13 2 -10 0 15.98 1.04 -2 10 0 17.19 0.82 -2 10 0 19.26 1.11 2 10 0 17.20 1.05 -2 -10 0 17.24 1.05 -3 -10 0 1.67 0.45 3 -10 0 1.99 0.51 -3 10 0 2.19 0.35 -3 10 0 3.14 0.64 3 10 0 3.52 0.64 4 10 0 1.70 0.52 -4 -10 0 1.93 0.57 4 -10 0 1.27 0.48 -4 10 0 1.31 0.51 -5 -10 0 3.19 0.70 5 10 0 2.89 0.69 5 -10 0 3.83 0.83 -5 10 0 2.69 0.76 6 10 0 0.42 0.51 -6 -10 0 0.42 0.43 -6 10 0 0.24 0.55 6 -10 0 -0.27 0.49 7 -10 0 0.52 0.64 -7 10 0 1.60 0.76 -7 -10 0 0.42 0.50 7 10 0 1.87 0.77 8 10 0 -0.28 0.71 -8 -10 0 -0.59 0.55 0 -11 0 0.22 0.27 0 11 0 0.26 0.26 0 11 0 0.03 0.17 -1 -11 0 8.23 0.89 1 -11 0 10.46 1.00 -1 11 0 9.17 0.65 1 11 0 8.88 0.53 1 11 0 8.29 0.82 -2 11 0 25.24 1.34 -2 11 0 25.34 1.07 2 11 0 28.01 1.40 2 -11 0 24.59 1.36 -2 -11 0 24.29 1.34 -3 11 0 0.45 0.37 -3 -11 0 0.01 0.29 3 -11 0 0.12 0.33 3 11 0 -0.12 0.31 4 -11 0 12.61 1.28 4 11 0 12.15 1.22 -4 -11 0 11.67 1.18 -4 11 0 11.84 1.26 -5 -11 0 3.54 0.73 5 11 0 3.60 0.83 5 -11 0 3.22 0.81 -5 11 0 4.85 0.98 -6 11 0 -0.23 0.55 6 11 0 0.72 0.63 -6 -11 0 1.26 0.61 6 -11 0 0.17 0.55 7 11 0 0.74 0.68 -7 -11 0 0.13 0.48 7 -11 0 0.28 0.68 -7 11 0 0.33 0.67 -8 -11 0 0.38 0.69 0 12 0 11.76 0.69 0 12 0 12.50 0.85 0 -12 0 12.01 1.12 -1 -12 0 11.17 1.07 1 -12 0 12.57 1.18 1 12 0 10.01 0.93 -1 12 0 8.84 0.70 -2 12 0 0.60 0.30 2 -12 0 0.58 0.41 2 12 0 0.77 0.43 -2 -12 0 0.70 0.41 3 12 0 22.31 1.41 -3 -12 0 21.29 1.35 -3 12 0 28.90 1.58 3 -12 0 21.22 1.38 4 -12 0 7.87 1.04 4 12 0 6.06 0.92 -4 -12 0 6.07 0.90 -4 12 0 6.34 1.03 -5 -12 0 2.16 0.66 5 12 0 2.06 0.67 5 -12 0 3.56 0.81 -5 12 0 3.33 0.85 -6 -12 0 8.02 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1 5 -34 0.91 0.68 1 -5 34 1.98 0.85 -1 5 -34 1.79 0.82 2 5 -34 1.34 0.83 0 -6 34 0.79 0.59 0 6 -34 0.35 0.62 1 6 -34 1.27 0.75 1 -6 34 -0.33 0.61 2 6 -34 -0.29 0.62 1 -7 34 0.51 0.68 0 0 35 0.15 0.58 -1 0 35 0.30 0.67 1 0 35 -0.01 0.70 -1 0 -35 -0.06 0.60 -2 0 -35 -0.21 0.53 -2 0 35 0.45 0.67 -3 0 35 -0.53 0.51 0 1 35 1.04 0.73 0 -1 35 0.43 0.65 0 1 -35 -0.79 0.52 1 -1 35 3.62 1.01 -1 -1 -35 2.51 0.85 -1 1 35 1.74 0.81 -1 1 -35 4.58 1.06 -1 -1 35 3.82 0.99 -2 1 35 1.28 0.78 -2 -1 -35 0.86 0.81 -2 1 -35 -0.15 0.63 -2 -1 35 0.82 0.74 0 -2 35 0.94 0.77 0 2 -35 0.30 0.60 0 2 35 -0.40 0.55 1 -2 35 1.52 0.81 -1 2 35 1.19 0.82 -1 -2 35 1.07 0.69 -1 2 -35 1.03 0.69 -2 -2 -35 -0.82 0.58 -2 -2 35 -0.19 0.58 0 3 -35 -0.37 0.55 0 -3 35 0.68 0.67 1 -3 35 1.13 0.72 1 3 -35 1.06 0.75 -1 3 -35 1.59 0.88 -1 -3 35 1.72 0.82 -2 -3 -35 0.41 0.76 0 4 -35 -0.06 0.65 0 -4 35 0.48 0.61 1 -4 35 -0.13 0.60 1 4 -35 0.44 0.71 -1 -4 35 -0.08 0.61 0 -5 35 -0.68 0.54 1 5 -35 4.41 1.13 1 -5 35 3.51 0.99 -1 0 -36 0.01 0.68 -1 1 -36 0.98 0.74 0 2 -36 0.11 0.63 -1 -2 36 0.05 0.60 0 3 -36 -0.34 0.58 -1 -3 36 0.20 0.58 1 4 -36 0.55 0.81 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 36265 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_h-m 'P b c m' _symmetry_int_tables_number 57 _chemical_absolute_configuration ? _database_code_depnum_ccdc_archive 'CCDC 967157' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound_4 _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety '(C6 H5 N2 S1 1+)2, (U O3 C4 H2 N4 S4 2-), 4(H2 O)' _chemical_formula_sum 'C16 H20 N8 O7 S6 U' _chemical_properties_physical thermochromic _exptl_crystal_recrystallization_method 'Slow Aqueous Evaporation' _chemical_melting_point ? _exptl_crystal_description Prism _exptl_crystal_colour 'Orange (293(2)K) Yellow (100(2)K)' _diffrn_ambient_temperature 100(2) _chemical_formula_weight 866.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.407(3) _cell_length_b 8.8724(17) _cell_length_c 24.900(5) _cell_angle_alpha 90 _cell_angle_beta 102.363(3) _cell_angle_gamma 90 _cell_volume 2893.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6848 _cell_measurement_theta_min 5.546 _cell_measurement_theta_max 59.896 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.967 _exptl_crystal_F_000 1624 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.175 _exptl_crystal_size_min 0.075 _exptl_absorpt_coefficient_mu 6.093 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5443 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_process_details 'SADABS, G. Sheldrick (1999)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focused sealed X-ray tube' _diffrn_measurement_device_type 'Bruker ApexII CCD' _diffrn_measurement_method 'Omega and Phi Scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15491 _diffrn_reflns_av_unetI/netI 0.0642 _diffrn_reflns_av_R_equivalents 0.0707 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.674 _diffrn_reflns_theta_max 30.430 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.926 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.926 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.926 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 4076 _reflns_number_gt 3882 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'APEX II (Bruker AXS, 2013)' _computing_cell_refinement 'SAINT (Bruker AXS, 2013)' _computing_data_reduction 'SAINT (Bruker AXS, 2013)' _computing_structure_solution 'SIR92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Crystal Maker v.8.2.2 (Palmer 2009)' _computing_publication_material 'WINGX (Farrugia, 2012)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0295P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4076 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0775 _refine_ls_wR_factor_gt 0.0765 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4037(3) 0.1815(4) 0.11145(14) 0.0144(7) Uani 1 1 d . . . . . C2 C 0.4364(3) -0.2521(4) 0.15680(14) 0.0146(7) Uani 1 1 d . . . . . C8 C 0.6536(3) 0.5379(4) 0.07266(16) 0.0187(8) Uani 1 1 d . . . . . H8 H 0.6515 0.6325 0.0564 0.022 Uiso 1 1 calc R U . . . C7 C 0.6394(3) 0.4103(4) 0.04033(16) 0.0204(8) Uani 1 1 d . . . . . H7 H 0.6271 0.4177 0.0022 0.024 Uiso 1 1 calc R U . . . C6 C 0.6438(3) 0.2694(4) 0.06601(14) 0.0113(6) Uani 1 1 d . . . . . C5 C 0.6603(3) 0.2615(4) 0.12280(14) 0.0145(7) Uani 1 1 d . . . . . H5 H 0.6628 0.1688 0.1405 0.017 Uiso 1 1 calc R U . . . C4 C 0.6731(3) 0.3937(4) 0.15255(15) 0.0164(7) Uani 1 1 d . . . . . H4 H 0.6837 0.3905 0.1907 0.020 Uiso 1 1 calc R U . . . C3 C 0.6355(3) -0.0261(4) 0.06873(15) 0.0158(7) Uani 1 1 d . . . . . N1 N 0.4259(3) 0.1480(4) 0.15760(13) 0.0224(7) Uani 1 1 d . . . . . N2 N 0.4588(2) -0.1622(3) 0.19212(12) 0.0175(6) Uani 1 1 d . . . . . N4 N 0.6704(2) 0.5260(4) 0.12710(13) 0.0149(6) Uani 1 1 d . . . . . H4A H 0.6799 0.6068 0.1466 0.018 Uiso 1 1 calc R U . . . N3 N 0.6396(3) -0.1187(4) 0.10112(14) 0.0219(7) Uani 1 1 d . . . . . O1 O 0.6236(2) 0.0625(3) 0.23526(12) 0.0160(5) Uani 1 1 d . . . . . OW1 O 0.5000 0.3340(4) 0.2500 0.0241(9) Uani 1 2 d S T P . . S1 S 0.36805(8) 0.22702(11) 0.04706(4) 0.0206(2) Uani 1 1 d . . . . . S2 S 0.40734(7) -0.38318(11) 0.11048(4) 0.01862(19) Uani 1 1 d . . . . . S3 S 0.62962(7) 0.11247(10) 0.02148(3) 0.01559(18) Uani 1 1 d . . . . . U1 U 0.5000 0.06292(2) 0.2500 0.00872(6) Uani 1 2 d S T P . . OW2 O 0.68623(19) 0.7215(3) 0.21744(10) 0.0149(5) Uani 1 1 d . . . . . OW3 O 0.3215(2) -0.5323(3) 0.20876(11) 0.0163(5) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0134(17) 0.0142(16) 0.0155(16) 0.0015(13) 0.0028(13) 0.0002(13) C2 0.0159(17) 0.0165(17) 0.0117(15) 0.0014(13) 0.0038(13) -0.0013(14) C8 0.030(2) 0.0121(16) 0.0153(17) 0.0028(13) 0.0072(15) 0.0002(15) C7 0.035(2) 0.0140(17) 0.0115(16) 0.0002(13) 0.0028(16) 0.0015(16) C6 0.0124(16) 0.0088(15) 0.0127(15) -0.0018(12) 0.0024(12) -0.0008(12) C5 0.0256(19) 0.0056(14) 0.0135(15) 0.0005(12) 0.0066(14) 0.0004(13) C4 0.0201(19) 0.0191(18) 0.0103(15) -0.0036(13) 0.0039(13) 0.0011(15) C3 0.0187(18) 0.0103(15) 0.0175(17) -0.0066(14) 0.0020(14) -0.0020(14) N1 0.0237(18) 0.0247(18) 0.0159(15) 0.0025(13) -0.0022(13) -0.0044(14) N2 0.0196(16) 0.0154(15) 0.0169(14) -0.0033(11) 0.0027(12) -0.0033(12) N4 0.0173(16) 0.0120(13) 0.0166(14) -0.0028(12) 0.0063(12) -0.0002(12) N3 0.033(2) 0.0125(15) 0.0195(16) -0.0010(13) 0.0039(14) 0.0004(14) O1 0.0142(14) 0.0173(14) 0.0168(13) -0.0006(9) 0.0039(11) -0.0021(9) OW1 0.022(2) 0.0111(18) 0.033(2) 0.000 -0.0074(16) 0.000 S1 0.0294(5) 0.0205(5) 0.0099(4) 0.0019(3) -0.0003(3) 0.0018(4) S2 0.0200(5) 0.0224(5) 0.0139(4) -0.0081(3) 0.0045(3) -0.0052(4) S3 0.0238(5) 0.0107(4) 0.0113(4) -0.0021(3) 0.0016(3) -0.0004(3) U1 0.00869(10) 0.00919(10) 0.00770(9) 0.000 0.00049(6) 0.000 OW2 0.0168(13) 0.0125(12) 0.0146(11) -0.0011(9) 0.0016(9) 0.0006(9) OW3 0.0149(13) 0.0172(12) 0.0173(12) -0.0020(10) 0.0045(10) 0.0007(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.162(5) . ? C1 S1 1.623(4) . ? C2 N2 1.178(5) . ? C2 S2 1.625(4) . ? C8 N4 1.330(5) . ? C8 C7 1.378(5) . ? C8 H8 0.9300 . ? C7 C6 1.400(5) . ? C7 H7 0.9300 . ? C6 C5 1.385(5) . ? C6 S3 1.764(3) . ? C5 C4 1.379(5) . ? C5 H5 0.9300 . ? C4 N4 1.330(5) . ? C4 H4 0.9300 . ? C3 N3 1.144(5) . ? C3 S3 1.692(4) . ? N1 U1 2.423(3) . ? N2 U1 2.456(3) . ? N4 H4A 0.8600 . ? O1 U1 1.772(3) . ? OW1 U1 2.405(4) . ? U1 O1 1.772(3) 2_655 ? U1 N1 2.423(3) 2_655 ? U1 N2 2.456(3) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 S1 177.8(3) . . ? N2 C2 S2 177.0(3) . . ? N4 C8 C7 120.1(3) . . ? N4 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C7 C6 118.7(3) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? C5 C6 C7 119.6(3) . . ? C5 C6 S3 125.0(3) . . ? C7 C6 S3 115.4(3) . . ? C4 C5 C6 118.7(3) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? N4 C4 C5 120.5(3) . . ? N4 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? N3 C3 S3 179.3(4) . . ? C1 N1 U1 169.9(3) . . ? C2 N2 U1 168.1(3) . . ? C8 N4 C4 122.5(3) . . ? C8 N4 H4A 118.8 . . ? C4 N4 H4A 118.8 . . ? C3 S3 C6 98.83(16) . . ? O1 U1 O1 179.76(14) 2_655 . ? O1 U1 OW1 90.12(7) 2_655 . ? O1 U1 OW1 90.12(7) . . ? O1 U1 N1 90.89(12) 2_655 2_655 ? O1 U1 N1 89.19(12) . 2_655 ? OW1 U1 N1 71.86(8) . 2_655 ? O1 U1 N1 89.18(12) 2_655 . ? O1 U1 N1 90.89(12) . . ? OW1 U1 N1 71.86(8) . . ? N1 U1 N1 143.71(17) 2_655 . ? O1 U1 N2 90.99(11) 2_655 . ? O1 U1 N2 88.81(11) . . ? OW1 U1 N2 144.43(7) . . ? N1 U1 N2 143.66(11) 2_655 . ? N1 U1 N2 72.61(11) . . ? O1 U1 N2 88.81(11) 2_655 2_655 ? O1 U1 N2 90.99(11) . 2_655 ? OW1 U1 N2 144.42(7) . 2_655 ? N1 U1 N2 72.61(11) 2_655 2_655 ? N1 U1 N2 143.66(11) . 2_655 ? N2 U1 N2 71.15(15) . 2_655 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C8 H8 S1 0.93 2.82 3.599(4) 141.7 5_665 C7 H7 S2 0.93 2.76 3.680(4) 169.6 5_655 _refine_diff_density_max 1.160 _refine_diff_density_min -1.066 _refine_diff_density_rms 0.190 _shelxl_version_number 2013-4 _shelx_res_file ; TITL C2onc in C2/c CELL 0.71073 13.4066 8.8724 24.8999 90.000 102.363 90.000 ZERR 4.00 0.0025 0.0017 0.0046 0.000 0.003 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O S U UNIT 64 40 32 28 24 4 MERG 2 EQIV $1 x, y+1, z HTAB C8 N4_$1 EQIV $2 -x+1, -y+1, -z HTAB C8 S1_$2 EQIV $3 -x+1, -y, -z HTAB C7 S2_$3 HTAB C7 OW3 HTAB N4 N4_$1 HTAB N4 OW2_$1 FMAP 2 PLAN 10 ACTA 50 BOND $H L.S. 12 WGHT 0.029500 FVAR 0.03429 C1 1 0.403654 0.181543 0.111451 11.00000 0.01343 0.01421 = 0.01551 0.00152 0.00278 0.00023 C2 1 0.436444 -0.252130 0.156797 11.00000 0.01594 0.01651 = 0.01175 0.00142 0.00381 -0.00135 C8 1 0.653614 0.537876 0.072662 11.00000 0.02978 0.01209 = 0.01531 0.00283 0.00725 0.00019 AFIX 43 H8 2 0.651482 0.632479 0.056372 11.00000 -1.20000 AFIX 0 C7 1 0.639371 0.410289 0.040332 11.00000 0.03469 0.01397 = 0.01145 0.00024 0.00282 0.00149 AFIX 43 H7 2 0.627093 0.417686 0.002224 11.00000 -1.20000 AFIX 0 C6 1 0.643760 0.269355 0.066013 11.00000 0.01235 0.00877 = 0.01272 -0.00179 0.00242 -0.00081 C5 1 0.660322 0.261461 0.122804 11.00000 0.02557 0.00558 = 0.01346 0.00051 0.00661 0.00038 AFIX 43 H5 2 0.662759 0.168809 0.140504 11.00000 -1.20000 AFIX 0 C4 1 0.673120 0.393736 0.152552 11.00000 0.02009 0.01912 = 0.01034 -0.00365 0.00393 0.00112 AFIX 43 H4 2 0.683731 0.390485 0.190687 11.00000 -1.20000 AFIX 0 C3 1 0.635467 -0.026106 0.068735 11.00000 0.01873 0.01026 = 0.01754 -0.00660 0.00201 -0.00200 N1 3 0.425872 0.147968 0.157598 11.00000 0.02367 0.02472 = 0.01585 0.00252 -0.00222 -0.00441 N2 3 0.458840 -0.162213 0.192119 11.00000 0.01962 0.01537 = 0.01693 -0.00335 0.00273 -0.00333 N4 3 0.670400 0.525954 0.127104 11.00000 0.01728 0.01203 = 0.01660 -0.00283 0.00633 -0.00018 AFIX 43 H4A 2 0.679852 0.606794 0.146591 11.00000 -1.20000 AFIX 0 N3 3 0.639648 -0.118725 0.101118 11.00000 0.03302 0.01249 = 0.01952 -0.00096 0.00389 0.00037 O1 4 0.623584 0.062503 0.235256 11.00000 0.01417 0.01732 = 0.01677 -0.00056 0.00387 -0.00212 OW1 4 0.500000 0.333968 0.250000 10.50000 0.02224 0.01115 = 0.03290 0.00000 -0.00737 0.00000 S1 5 0.368054 0.227022 0.047065 11.00000 0.02941 0.02051 = 0.00993 0.00187 -0.00026 0.00183 S2 5 0.407342 -0.383175 0.110482 11.00000 0.01997 0.02239 = 0.01390 -0.00805 0.00451 -0.00521 S3 5 0.629622 0.112474 0.021484 11.00000 0.02382 0.01073 = 0.01128 -0.00209 0.00162 -0.00036 U1 6 0.500000 0.062917 0.250000 10.50000 0.00869 0.00919 = 0.00770 0.00000 0.00049 0.00000 OW2 4 0.686230 0.721489 0.217443 11.00000 0.01681 0.01249 = 0.01459 -0.00107 0.00155 0.00060 OW3 4 0.321490 -0.532281 0.208757 11.00000 0.01493 0.01716 = 0.01728 -0.00203 0.00451 0.00074 HKLF 4 REM C2onc in C2/c REM R1 = 0.0317 for 3882 Fo > 4sig(Fo) and 0.0338 for all 4076 data REM 173 parameters refined using 0 restraints END WGHT 0.0295 0.0000 REM Highest difference peak 1.160, deepest hole -1.066, 1-sigma level 0.190 Q1 1 0.5413 0.3780 0.2591 11.00000 0.05 1.16 Q2 1 0.6207 0.7514 0.2131 11.00000 0.05 1.14 Q3 1 0.5744 0.0636 0.2286 11.00000 0.05 1.09 Q4 1 0.3239 -0.4979 0.1780 11.00000 0.05 1.06 Q5 1 0.3876 -0.4315 0.1301 11.00000 0.05 1.00 Q6 1 0.5747 0.0637 0.2678 11.00000 0.05 0.98 Q7 1 0.2671 -0.5960 0.2041 11.00000 0.05 0.94 Q8 1 0.6969 0.6741 0.2418 11.00000 0.05 0.78 Q9 1 0.5530 -0.0391 0.2515 11.00000 0.05 0.73 Q10 1 0.4570 -0.0942 0.2095 11.00000 0.05 0.70 ; _shelx_res_checksum 82693 _shelx_hkl_file ; 2 0 0 87.35 7.70 2 0 0 86.00 7.69 -2 0 0 75.73 8.75 -2 0 0 88.34 7.70 -4 0 0 79.01 7.16 4 0 0 80.20 7.17 4 0 0 75.21 7.19 6 0 0 162.75 14.63 -6 0 0 158.24 14.62 8 0 0 96.49 8.92 -10 0 0 26.68 2.96 10 0 0 26.43 2.66 12 0 0 27.13 2.55 -12 0 0 22.22 2.74 -14 0 0 21.06 2.52 16 0 0 28.38 3.33 -16 0 0 36.15 3.80 -1 -1 0 108.33 9.38 1 -1 0 101.35 9.47 -1 -1 0 97.73 9.47 1 -1 0 103.60 9.39 1 1 0 104.15 10.72 1 1 0 106.14 9.38 -3 -1 0 131.92 11.68 -3 1 0 110.92 13.25 3 1 0 135.16 13.24 3 1 0 132.81 11.61 -5 -1 0 11.85 1.13 5 -1 0 11.54 1.09 5 -1 0 12.23 1.20 -5 1 0 12.13 1.09 5 1 0 11.86 1.31 5 1 0 11.67 1.18 -5 1 0 11.06 1.32 7 -1 0 88.86 8.29 -7 -1 0 92.48 8.25 7 1 0 87.49 8.28 9 -1 0 88.34 7.39 -9 -1 0 70.98 7.24 -9 1 0 79.49 8.33 9 1 0 81.90 7.35 -11 -1 0 2.80 0.57 11 -1 0 2.49 0.57 11 1 0 3.09 0.60 -11 1 0 2.62 0.57 -13 -1 0 16.16 2.00 13 -1 0 14.39 1.91 -13 1 0 19.02 2.02 13 1 0 14.67 1.79 -15 -1 0 40.44 4.95 15 -1 0 47.53 4.47 15 1 0 43.04 4.42 -15 1 0 47.66 4.99 17 -1 0 14.44 1.89 -17 -1 0 15.13 2.11 -17 1 0 11.26 1.99 17 1 0 19.13 2.08 0 -2 0 20.14 1.73 0 -2 0 17.38 1.80 0 2 0 16.77 2.02 0 2 0 20.37 1.73 2 -2 0 18.85 1.87 -2 -2 0 20.82 1.91 -2 2 0 22.60 2.20 2 2 0 20.39 2.14 2 2 0 19.11 1.85 4 -2 0 37.95 3.40 -4 -2 0 33.44 3.40 4 2 0 37.88 3.85 4 2 0 36.64 3.37 -6 -2 0 52.50 4.56 6 -2 0 45.85 4.49 6 -2 0 51.01 4.58 6 2 0 47.11 4.54 -6 2 0 47.58 5.20 6 2 0 50.77 5.17 -8 -2 0 24.22 2.32 8 -2 0 26.13 2.42 8 2 0 22.76 2.36 -10 -2 0 21.82 2.56 10 -2 0 23.95 2.33 -10 2 0 22.72 2.59 10 2 0 22.73 2.29 -12 -2 0 33.02 3.14 12 -2 0 23.30 2.75 -12 2 0 29.78 3.13 12 2 0 23.09 2.74 14 -2 0 7.22 1.18 -14 -2 0 8.78 1.30 14 2 0 8.81 1.22 -14 2 0 7.21 1.25 -16 -2 0 7.12 1.30 16 -2 0 6.87 1.21 16 2 0 7.33 1.20 -16 2 0 7.77 1.30 1 -3 0 0.58 0.11 -1 -3 0 0.68 0.20 1 -3 0 0.64 0.19 -1 3 0 0.50 0.18 1 3 0 0.41 0.15 -3 -3 0 30.67 3.22 3 -3 0 34.73 3.17 -3 3 0 35.04 3.69 3 3 0 34.84 3.62 3 3 0 34.66 3.12 -5 -3 0 16.40 1.56 5 -3 0 17.49 1.51 5 -3 0 15.32 1.54 5 3 0 14.98 1.49 5 3 0 13.59 1.71 7 -3 0 4.42 0.44 7 -3 0 3.22 0.55 -7 -3 0 3.73 0.54 7 3 0 3.79 0.54 7 3 0 3.06 0.57 -7 3 0 5.50 0.76 9 -3 0 16.19 1.72 -9 -3 0 16.15 1.64 9 3 0 16.21 1.89 -9 3 0 16.88 1.96 9 3 0 16.41 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37.68 3.76 9 -1 -4 57.17 5.42 9 -1 -4 50.50 5.29 -9 -1 4 59.83 6.10 -9 1 4 69.46 6.16 9 1 -4 55.07 5.33 9 1 -4 58.33 5.40 7 -1 -4 54.29 5.12 7 -1 -4 53.22 5.05 7 1 -4 55.74 5.11 7 1 -4 56.71 5.08 5 -1 -4 53.38 4.40 5 1 -4 47.37 4.40 5 1 -4 48.14 5.00 -5 1 4 41.12 5.01 5 1 -4 47.73 4.41 3 -1 -4 60.23 5.40 3 1 -4 61.25 5.44 -3 1 4 53.06 6.16 3 1 -4 62.03 5.40 3 1 -4 58.79 6.14 -1 -1 4 187.29 16.17 1 -1 -4 198.70 16.31 1 1 -4 172.91 16.30 1 1 -4 155.02 18.45 -1 1 4 180.38 16.17 -1 1 4 183.87 18.46 -1 1 4 171.87 16.31 -1 -1 -4 165.00 15.66 1 -1 4 168.51 15.54 -1 1 -4 182.53 17.76 -1 1 -4 168.64 15.65 1 1 4 171.18 17.74 1 1 4 173.37 15.54 -3 -1 -4 11.91 1.05 3 -1 4 9.67 1.07 -3 1 -4 11.10 1.02 -3 1 -4 11.09 1.22 3 1 4 10.75 1.20 3 1 4 10.16 1.07 5 -1 4 16.50 1.55 -5 -1 -4 15.95 1.45 5 -1 4 14.24 1.42 5 1 4 14.21 1.52 -5 1 -4 17.85 1.74 7 -1 4 74.25 6.37 -7 -1 -4 65.48 6.25 7 1 4 72.25 6.36 -7 1 -4 63.42 7.19 -9 -1 -4 44.27 5.02 9 -1 4 49.99 4.50 -9 1 -4 45.40 5.04 9 1 4 48.82 4.49 11 -1 4 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-29 28.74 3.15 4 4 -29 31.59 3.17 -4 4 29 31.30 3.12 -2 -4 29 25.10 2.71 2 -4 -29 24.62 2.75 2 4 -29 26.27 2.75 -2 4 29 29.80 2.77 0 -4 29 8.30 1.19 0 -4 -29 8.34 1.17 0 4 29 8.38 1.17 0 4 -29 6.04 1.03 -2 -4 -29 18.83 2.13 2 -4 29 21.75 2.21 2 4 29 18.29 2.16 4 4 29 30.18 3.15 -9 -5 29 7.41 1.06 9 -5 -29 4.58 1.03 -9 5 29 4.87 0.96 -7 -5 29 15.19 1.72 7 -5 -29 17.05 1.87 7 5 -29 14.32 1.90 -7 5 29 13.49 1.82 5 -5 -29 13.61 1.84 -5 -5 29 15.87 1.72 -5 5 29 15.27 1.76 5 5 -29 14.94 1.90 3 -5 -29 11.40 1.52 -3 -5 29 10.40 1.45 3 5 -29 11.39 1.52 -3 5 29 12.69 1.53 -1 -5 29 16.40 1.88 1 -5 -29 17.33 1.94 1 5 -29 16.56 1.88 1 -5 29 16.23 2.18 -1 -5 -29 19.43 2.11 -1 5 -29 20.25 2.08 -3 -5 -29 10.57 1.42 -8 -6 29 8.57 1.22 -6 -6 29 29.52 3.01 -4 -6 29 5.13 0.82 4 6 -29 3.71 0.85 2 -6 -29 0.64 0.53 -2 -6 29 0.83 0.43 2 6 -29 0.54 0.42 0 -6 29 13.74 1.70 0 6 -29 12.33 1.67 12 0 -30 23.34 2.54 -10 0 30 24.12 2.39 10 0 -30 19.44 2.32 -8 0 30 13.50 1.73 8 0 -30 14.05 1.77 6 0 -30 5.64 0.95 -6 0 30 6.46 1.01 -4 0 30 7.34 1.10 4 0 -30 6.99 1.09 2 0 -30 48.32 4.84 -2 0 30 51.07 4.84 0 0 -30 40.87 3.90 0 0 30 37.80 3.90 2 0 30 5.29 0.91 -2 0 -30 4.79 0.82 4 0 30 13.56 1.79 -11 -1 30 10.10 1.46 11 -1 -30 11.06 1.47 11 1 -30 10.45 1.45 -11 1 30 8.91 1.40 -9 -1 30 27.45 3.07 9 -1 -30 30.12 3.14 9 1 -30 29.85 3.13 -9 1 30 33.91 3.16 7 -1 -30 13.84 1.57 -7 -1 30 11.85 1.62 7 1 -30 12.18 1.67 -7 1 30 14.35 1.58 -5 -1 30 9.59 1.36 5 -1 -30 9.09 1.34 -5 1 30 11.12 1.42 5 1 -30 11.31 1.42 -3 -1 30 13.43 1.57 3 -1 -30 13.21 1.54 3 1 -30 12.72 1.54 -3 1 30 14.20 1.58 -1 -1 30 11.12 1.56 1 -1 -30 13.98 1.51 1 1 -30 12.49 1.47 -1 1 30 13.05 1.62 -1 -1 -30 18.10 1.88 1 -1 30 16.68 1.89 -1 1 -30 15.50 1.84 1 1 30 17.74 1.92 -3 -1 -30 14.64 1.80 3 -1 30 20.48 2.00 3 1 30 16.19 1.90 12 -2 -30 9.88 1.56 10 -2 -30 3.19 0.79 -10 -2 30 4.40 0.82 10 2 -30 4.08 0.85 -10 2 30 3.94 0.86 8 -2 -30 4.70 0.84 -8 -2 30 2.84 0.68 8 2 -30 3.93 0.82 -8 2 30 3.32 0.71 -6 -2 30 14.22 1.69 6 -2 -30 15.57 1.87 6 2 -30 14.43 1.71 -6 2 30 14.78 1.83 4 -2 -30 23.13 2.39 -4 -2 30 21.07 2.35 4 2 -30 21.93 2.38 -4 2 30 22.79 2.37 2 -2 -30 8.46 1.24 -2 -2 30 7.63 1.16 -2 2 30 8.22 1.21 2 2 -30 9.82 1.26 0 -2 -30 1.97 0.55 0 -2 30 3.10 0.64 0 2 30 1.49 0.51 0 2 -30 1.54 0.47 -2 -2 -30 14.02 1.67 2 -2 30 15.06 1.88 2 2 30 16.57 1.75 -2 2 -30 13.43 1.64 4 2 30 12.22 1.66 11 -3 -30 3.10 0.79 -9 -3 30 0.63 0.37 9 -3 -30 -0.01 0.35 -9 3 30 -0.06 0.34 9 3 -30 -0.14 0.32 -7 -3 30 0.57 0.38 7 -3 -30 1.43 0.50 -7 3 30 0.93 0.43 7 3 -30 0.57 0.43 -5 -3 30 14.70 1.61 5 -3 -30 11.54 1.64 -5 3 30 13.25 1.70 5 3 -30 14.30 1.62 -3 -3 30 6.28 1.00 3 -3 -30 6.01 0.96 3 3 -30 5.04 0.92 -3 3 30 7.02 1.02 -1 -3 30 0.87 0.47 1 -3 -30 0.73 0.36 -1 3 30 0.83 0.42 1 3 -30 0.69 0.39 -1 -3 -30 1.68 0.52 1 -3 30 2.44 0.59 1 3 30 1.61 0.55 -1 3 -30 2.68 0.59 3 -3 30 2.35 0.69 -3 -3 -30 3.67 0.71 3 3 30 2.89 0.70 -10 -4 30 1.18 0.45 -10 4 30 -0.40 0.33 -8 -4 30 0.91 0.45 8 -4 -30 0.54 0.41 -8 4 30 1.12 0.47 8 4 -30 1.50 0.57 -6 -4 30 0.52 0.37 6 -4 -30 1.03 0.47 6 4 -30 0.24 0.35 -6 4 30 0.81 0.43 -4 -4 30 0.60 0.39 4 -4 -30 1.17 0.51 4 4 -30 0.24 0.36 -4 4 30 0.75 0.44 2 -4 -30 1.22 0.48 -2 -4 30 1.02 0.43 2 4 -30 0.80 0.44 -2 4 30 0.94 0.45 0 -4 -30 0.00 0.34 0 -4 30 0.30 0.36 0 4 -30 0.39 0.36 0 4 30 0.48 0.42 2 -4 30 0.60 0.45 -2 -4 -30 0.36 0.39 2 4 30 0.36 0.43 4 4 30 0.92 0.52 -9 -5 30 6.21 1.04 -9 5 30 5.54 1.00 -7 -5 30 5.89 0.96 -7 5 30 4.23 0.86 -5 -5 30 1.96 0.55 5 -5 -30 2.19 0.64 5 5 -30 2.14 0.65 -5 5 30 1.67 0.55 3 -5 -30 2.21 0.61 -3 -5 30 1.68 0.53 -3 5 30 1.97 0.58 3 5 -30 2.95 0.67 1 -5 -30 1.23 0.50 -1 -5 30 1.24 0.49 1 5 -30 1.59 0.52 -1 -5 -30 1.17 0.48 1 -5 30 0.99 0.51 -1 5 -30 0.70 0.41 -8 -6 30 7.38 1.14 -6 -6 30 9.34 1.31 -4 -6 30 4.44 0.81 -2 -6 30 8.39 1.19 0 6 -30 14.56 1.85 -10 0 31 -0.18 0.35 10 0 -31 0.15 0.35 -8 0 31 0.31 0.35 8 0 -31 0.05 0.33 -6 0 31 -0.42 0.24 6 0 -31 0.12 0.34 -4 0 31 0.05 0.28 4 0 -31 -0.11 0.26 -2 0 31 0.77 0.40 2 0 -31 0.25 0.35 0 0 -31 0.11 0.32 0 0 31 0.54 0.35 -2 0 -31 -0.34 0.27 2 0 31 -0.17 0.32 9 -1 -31 6.46 1.14 -9 -1 31 7.10 1.16 -9 1 31 10.80 1.34 9 1 -31 8.28 1.20 -7 -1 31 8.38 1.17 7 -1 -31 6.16 1.04 7 1 -31 6.71 1.08 -7 1 31 6.05 1.06 5 -1 -31 0.42 0.35 -5 -1 31 0.61 0.36 -5 1 31 0.57 0.40 5 1 -31 0.43 0.38 3 -1 -31 1.84 0.52 -3 -1 31 1.45 0.51 -3 1 31 2.55 0.60 3 1 -31 2.12 0.57 -1 -1 31 7.91 1.09 1 -1 -31 6.20 0.99 -1 1 31 5.89 1.00 1 1 -31 6.93 1.04 1 -1 31 2.30 0.60 -1 1 -31 1.99 0.50 1 1 31 1.53 0.53 3 1 31 1.06 0.51 10 -2 -31 1.55 0.55 -8 -2 31 7.81 1.18 8 -2 -31 7.16 1.12 -8 2 31 6.36 1.10 8 2 -31 8.49 1.21 -6 -2 31 14.67 1.77 6 -2 -31 14.96 1.80 6 2 -31 12.11 1.71 -6 2 31 12.90 1.71 4 -2 -31 9.81 1.42 -4 -2 31 11.17 1.45 4 2 -31 11.62 1.45 -4 2 31 9.46 1.38 2 -2 -31 9.48 1.32 -2 -2 31 10.50 1.37 2 2 -31 10.25 1.39 -2 2 31 9.78 1.38 0 -2 31 13.17 1.65 0 -2 -31 11.69 1.55 0 2 31 11.15 1.55 0 2 -31 13.40 1.60 2 -2 31 4.99 0.93 -2 -2 -31 4.98 0.88 2 2 31 4.99 0.95 9 -3 -31 7.00 1.17 -9 -3 31 7.06 1.11 -9 3 31 7.80 1.19 -7 -3 31 23.43 2.59 7 -3 -31 23.85 2.67 -7 3 31 24.86 2.62 7 3 -31 26.57 2.67 5 -3 -31 20.79 2.30 -5 -3 31 22.89 2.27 5 3 -31 19.53 2.27 -5 3 31 19.48 2.25 3 -3 -31 1.63 0.52 -3 -3 31 1.32 0.50 -3 3 31 1.03 0.46 3 3 -31 0.88 0.44 -1 -3 31 9.83 1.33 1 -3 -31 6.56 1.14 -1 3 31 10.01 1.32 1 3 -31 9.50 1.26 1 -3 31 46.54 4.66 -1 -3 -31 45.62 4.63 1 3 31 45.21 4.64 -1 3 -31 51.11 4.65 -3 -3 -31 19.92 2.19 3 3 31 20.03 2.27 -8 -4 31 22.66 2.16 -8 4 31 15.80 2.06 6 -4 -31 15.73 2.22 -6 -4 31 23.17 2.17 -6 4 31 18.95 2.13 6 4 -31 18.23 2.16 4 -4 -31 13.19 1.71 -4 -4 31 13.18 1.67 -4 4 31 13.23 1.70 4 4 -31 13.13 1.72 2 -4 -31 10.93 1.53 -2 -4 31 14.51 1.65 2 4 -31 11.07 1.51 -2 4 31 10.91 1.53 0 -4 -31 17.32 2.03 0 -4 31 18.63 2.07 0 4 31 18.06 2.08 0 4 -31 19.46 2.06 -2 -4 -31 20.06 2.34 2 4 31 23.89 2.45 -7 -5 31 9.70 1.35 -7 5 31 9.85 1.44 -5 -5 31 10.57 1.46 -5 5 31 11.66 1.52 -3 -5 31 21.24 2.41 3 5 -31 24.03 2.50 -1 -5 31 13.16 1.76 1 5 -31 15.08 1.71 -8 0 32 3.19 0.71 8 0 -32 3.51 0.76 -6 0 32 25.96 2.77 6 0 -32 26.56 2.78 -4 0 32 35.69 3.45 4 0 -32 32.01 3.42 2 0 -32 14.73 1.79 -2 0 32 16.83 1.84 0 0 -32 7.09 1.11 0 0 32 9.10 1.26 -2 0 -32 13.98 1.62 -7 -1 32 7.44 1.20 7 -1 -32 8.24 1.23 7 1 -32 6.33 1.12 -7 1 32 9.75 1.30 -5 -1 32 12.34 1.74 5 -1 -32 14.81 1.70 -5 1 32 15.99 1.74 5 1 -32 14.74 1.70 3 -1 -32 13.24 1.74 -3 -1 32 12.76 1.72 -3 1 32 15.93 1.71 3 1 -32 14.59 1.66 -1 -1 32 9.65 1.28 1 -1 -32 7.77 1.16 1 1 -32 8.91 1.23 -1 1 32 7.67 1.19 1 -1 32 21.41 2.40 -1 -1 -32 23.16 2.37 1 1 32 22.41 2.40 -1 1 -32 20.97 2.33 8 -2 -32 16.50 1.99 -8 -2 32 20.33 2.05 -8 2 32 18.02 2.00 8 2 -32 14.52 2.16 6 -2 -32 7.94 1.28 -6 -2 32 9.03 1.28 6 2 -32 10.20 1.39 -6 2 32 9.14 1.33 4 -2 -32 3.71 0.75 -4 -2 32 3.41 0.73 -4 2 32 3.17 0.72 4 2 -32 3.83 0.76 -2 -2 32 13.31 1.61 2 -2 -32 12.51 1.58 2 2 -32 10.88 1.49 -2 2 32 10.64 1.51 0 -2 -32 6.55 1.06 0 -2 32 7.39 1.14 0 2 -32 8.35 1.16 0 2 32 6.98 1.12 -2 -2 -32 4.98 0.86 -7 -3 32 2.22 0.61 -7 3 32 3.71 0.79 5 -3 -32 6.07 0.98 -5 -3 32 4.82 0.88 -5 3 32 3.13 0.78 5 3 -32 4.49 0.90 -3 -3 32 1.27 0.52 3 -3 -32 1.28 0.54 -3 3 32 1.07 0.48 3 3 -32 2.45 0.61 -1 -3 32 2.61 0.65 1 -3 -32 2.43 0.65 1 3 -32 1.72 0.56 -1 3 32 2.78 0.67 -1 -3 -32 2.43 0.64 -1 3 -32 3.12 0.66 1 3 32 1.78 0.60 -6 -4 32 1.03 0.51 -6 4 32 2.67 0.69 -4 -4 32 1.28 0.52 -4 4 32 1.16 0.52 -2 -4 32 2.26 0.70 2 4 -32 1.07 0.52 -2 4 32 2.26 0.63 0 4 32 1.22 0.55 0 4 -32 1.00 0.44 -5 5 32 0.74 0.49 6 0 -33 0.11 0.34 -6 0 33 0.23 0.36 -4 0 33 0.64 0.40 4 0 -33 0.32 0.39 -2 0 33 0.59 0.40 2 0 -33 0.08 0.32 0 0 -33 0.31 0.35 -7 1 33 0.72 0.48 5 -1 -33 7.58 1.11 -5 -1 33 5.75 1.07 5 1 -33 7.57 1.14 -5 1 33 6.80 1.09 -3 -1 33 4.76 0.88 3 -1 -33 4.24 0.83 -3 1 33 4.09 0.83 3 1 -33 3.94 0.82 1 -1 -33 0.42 0.41 -1 -1 33 0.39 0.38 1 1 -33 0.45 0.37 -1 1 33 0.87 0.45 -1 -1 -33 2.93 0.70 -1 1 -33 4.14 0.79 -6 2 33 13.25 1.75 4 -2 -33 19.89 2.13 -4 -2 33 20.22 2.16 -4 2 33 16.79 2.09 4 2 -33 19.30 2.15 2 -2 -33 2.96 0.67 -2 2 33 3.27 0.76 2 2 -33 3.61 0.76 0 -2 -33 0.85 0.43 0 2 -33 0.40 0.41 -2 -2 -33 7.79 1.13 -5 3 33 7.09 1.13 -3 3 33 36.05 3.67 -1 3 33 20.64 2.36 1 3 -33 22.06 2.35 -4 4 33 16.99 1.96 -2 4 33 14.84 1.93 0 0 -34 28.69 3.00 1 1 -34 21.98 2.40 -1 1 -34 7.09 1.12 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 43645 _symmetry_cell_setting monoclinic _symmetry_space_group_name_h-m 'C 2/c' _symmetry_int_tables_number 15 _chemical_absolute_configuration ? _database_code_depnum_ccdc_archive 'CCDC 967158' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound_5 _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety '(C6 H8 N1 1+)2, (U O3 C4 H2 N4 S4 2-) ' _chemical_formula_sum 'C16 H18 N6 O3 S4 U' _exptl_crystal_recrystallization_method 'Slow Aqueous Evaporation' _chemical_melting_point ? _exptl_crystal_description Prism _exptl_crystal_colour Yellow _diffrn_ambient_temperature 100(2) _chemical_formula_weight 708.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.654(2) _cell_length_b 9.0207(14) _cell_length_c 17.766(3) _cell_angle_alpha 90 _cell_angle_beta 92.078(2) _cell_angle_gamma 90 _cell_volume 2347.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6119 _cell_measurement_theta_min 4.588 _cell_measurement_theta_max 59.688 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.000 _exptl_crystal_F_000 1336 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.142 _exptl_crystal_size_mid 0.119 _exptl_crystal_size_min 0.085 _exptl_absorpt_coefficient_mu 7.301 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.6120 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_process_details 'SADABS, G. Sheldrick (1999)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_measurement_device_type 'Bruker ApexII CCD' _diffrn_measurement_method 'Omega and Phi Scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12086 _diffrn_reflns_av_unetI/netI 0.0319 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.294 _diffrn_reflns_theta_max 30.237 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.938 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.938 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.938 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 3284 _reflns_number_gt 3049 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'APEX II (Bruker AXS, 2013)' _computing_cell_refinement 'SAINT (Bruker AXS, 2013)' _computing_data_reduction 'SAINT (Bruker AXS, 2013)' _computing_structure_solution 'SIR92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Crystal Maker v.8.2.2 (Palmer 2009)' _computing_publication_material 'WINGX (Farrugia, 2012)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0155P)^2^+5.9979P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3284 _refine_ls_number_parameters 138 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0264 _refine_ls_R_factor_gt 0.0223 _refine_ls_wR_factor_ref 0.0460 _refine_ls_wR_factor_gt 0.0449 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.08341(19) 0.9207(3) 0.57519(16) 0.0137(5) Uani 1 1 d . . . . . C2 C -0.0683(2) 1.3933(3) 0.83704(16) 0.0146(5) Uani 1 1 d . . . . . C3 C 0.7956(2) 0.7919(3) 0.62686(18) 0.0197(6) Uani 1 1 d . . . . . H3 H 0.7721 0.8775 0.6480 0.024 Uiso 1 1 calc R U . . . C4 C 0.77544(19) 0.6550(3) 0.65652(17) 0.0172(6) Uani 1 1 d . . . . . H4 H 0.7385 0.6483 0.6979 0.021 Uiso 1 1 calc R U . . . C5 C 0.81036(19) 0.5266(3) 0.62456(16) 0.0144(5) Uani 1 1 d . . . . . C6 C 0.8645(2) 0.5430(3) 0.56165(18) 0.0215(6) Uani 1 1 d . . . . . H6 H 0.8876 0.4596 0.5383 0.026 Uiso 1 1 calc R U . . . C7 C 0.8834(2) 0.6809(4) 0.53444(18) 0.0241(7) Uani 1 1 d . . . . . H7 H 0.9199 0.6912 0.4930 0.029 Uiso 1 1 calc R U . . . C8 C 0.7923(2) 0.3770(3) 0.65764(18) 0.0212(6) Uani 1 1 d . . . . . H8A H 0.7711 0.3107 0.6185 0.032 Uiso 1 1 calc R U . . . H8B H 0.7466 0.3856 0.6948 0.032 Uiso 1 1 calc R U . . . H8C H 0.8476 0.3388 0.6809 0.032 Uiso 1 1 calc R U . . . N1 N 0.06178(17) 0.9590(3) 0.63466(14) 0.0162(5) Uani 1 1 d . . . . . N2 N -0.04171(17) 1.2754(3) 0.82154(14) 0.0168(5) Uani 1 1 d . . . . . N3 N 0.84913(18) 0.8015(3) 0.56763(15) 0.0200(5) Uani 1 1 d . . . . . H3A H 0.8620 0.8876 0.5502 0.024 Uiso 1 1 calc R U . . . O1 O -0.11170(13) 1.0554(2) 0.70819(11) 0.0161(4) Uani 1 1 d . . . . . OW1 O 0.0000 0.7781(3) 0.7500 0.0226(7) Uani 1 2 d S T P . . S1 S 0.11420(6) 0.86563(8) 0.49235(4) 0.01911(15) Uani 1 1 d . . . . . S2 S -0.10687(6) 1.55634(8) 0.86052(4) 0.02167(15) Uani 1 1 d . . . . . U1 U 0.0000 1.05536(2) 0.7500 0.00992(4) Uani 1 2 d S T P . . 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 0.0160(13) 0.0077(12) 0.0174(13) 0.0021(10) -0.0013(10) 0.0002(10) C2 0.0176(14) 0.0147(13) 0.0117(12) -0.0006(10) 0.0031(10) -0.0026(11) C3 0.0165(14) 0.0126(13) 0.0299(16) -0.0042(12) -0.0007(12) -0.0001(11) C4 0.0149(13) 0.0161(13) 0.0205(14) -0.0030(12) 0.0013(11) -0.0017(11) C5 0.0133(13) 0.0140(14) 0.0157(13) 0.0019(10) -0.0017(10) -0.0014(10) C6 0.0259(15) 0.0167(14) 0.0222(15) -0.0029(12) 0.0081(12) 0.0003(12) C7 0.0288(17) 0.0225(16) 0.0216(15) 0.0017(13) 0.0079(13) -0.0041(13) C8 0.0230(16) 0.0154(14) 0.0251(16) 0.0050(12) 0.0004(13) 0.0007(12) N1 0.0207(12) 0.0115(11) 0.0165(11) 0.0014(9) 0.0035(9) 0.0007(10) N2 0.0206(13) 0.0138(11) 0.0165(12) -0.0020(9) 0.0054(10) -0.0015(10) N3 0.0226(13) 0.0126(12) 0.0246(13) 0.0030(10) -0.0015(11) -0.0056(10) O1 0.0150(9) 0.0130(9) 0.0201(10) -0.0009(8) 0.0007(8) -0.0009(8) OW1 0.0342(18) 0.0062(13) 0.0280(17) 0.000 0.0101(14) 0.000 S1 0.0326(4) 0.0118(3) 0.0133(3) -0.0010(3) 0.0065(3) 0.0004(3) S2 0.0299(4) 0.0089(3) 0.0271(4) -0.0022(3) 0.0126(3) 0.0009(3) U1 0.01210(7) 0.00619(6) 0.01158(7) 0.000 0.00183(5) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.166(4) . ? C1 S1 1.632(3) . ? C2 N2 1.168(4) . ? C2 S2 1.635(3) . ? C3 N3 1.338(4) . ? C3 C4 1.379(4) . ? C3 H3 0.9300 . ? C4 C5 1.395(4) . ? C4 H4 0.9300 . ? C5 C6 1.401(4) . ? C5 C8 1.499(4) . ? C6 C7 1.366(4) . ? C6 H6 0.9300 . ? C7 N3 1.343(4) . ? C7 H7 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? N1 U1 2.431(2) . ? N2 U1 2.447(2) . ? N3 H3A 0.8600 . ? O1 U1 1.773(2) . ? OW1 U1 2.501(3) . ? U1 O1 1.773(2) 2_556 ? U1 N1 2.431(2) 2_556 ? U1 N2 2.447(2) 2_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 S1 179.4(3) . . ? N2 C2 S2 178.5(3) . . ? N3 C3 C4 119.9(3) . . ? N3 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C3 C4 C5 120.1(3) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 117.6(3) . . ? C4 C5 C8 121.0(3) . . ? C6 C5 C8 121.4(3) . . ? C7 C6 C5 120.4(3) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? N3 C7 C6 119.9(3) . . ? N3 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C1 N1 U1 172.4(2) . . ? C2 N2 U1 162.2(2) . . ? C3 N3 C7 122.2(3) . . ? C3 N3 H3A 118.9 . . ? C7 N3 H3A 118.9 . . ? O1 U1 O1 179.97(13) 2_556 . ? O1 U1 N1 89.25(9) 2_556 . ? O1 U1 N1 90.76(9) . . ? O1 U1 N1 90.76(9) 2_556 2_556 ? O1 U1 N1 89.25(9) . 2_556 ? N1 U1 N1 138.08(11) . 2_556 ? O1 U1 N2 88.46(9) 2_556 2_556 ? O1 U1 N2 91.51(9) . 2_556 ? N1 U1 N2 75.21(8) . 2_556 ? N1 U1 N2 146.70(8) 2_556 2_556 ? O1 U1 N2 91.51(9) 2_556 . ? O1 U1 N2 88.46(9) . . ? N1 U1 N2 146.70(8) . . ? N1 U1 N2 75.21(8) 2_556 . ? N2 U1 N2 71.53(11) 2_556 . ? O1 U1 OW1 90.02(6) 2_556 . ? O1 U1 OW1 90.02(6) . . ? N1 U1 OW1 69.04(6) . . ? N1 U1 OW1 69.04(6) 2_556 . ? N2 U1 OW1 144.24(6) 2_556 . ? N2 U1 OW1 144.23(6) . . ? _refine_diff_density_max 0.895 _refine_diff_density_min -1.608 _refine_diff_density_rms 0.142 _shelxl_version_number 2013-4 _shelx_res_file ; TITL C2onc in C2/c CELL 0.71073 14.6543 9.0207 17.7661 90.000 92.078 90.000 ZERR 8.00 0.0023 0.0014 0.0027 0.000 0.002 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O S U UNIT 64 64 24 12 16 4 MERG 2 FMAP 2 PLAN 25 ACTA 50.00 HTAB BOND $H L.S. 24 WGHT 0.015500 5.997900 FVAR 0.04116 C1 1 0.083414 0.920667 0.575193 11.00000 0.01598 0.00767 = 0.01739 0.00211 -0.00132 0.00019 C2 1 -0.068251 1.393291 0.837036 11.00000 0.01762 0.01468 = 0.01168 -0.00059 0.00313 -0.00260 C3 1 0.795616 0.791931 0.626857 11.00000 0.01651 0.01262 = 0.02987 -0.00424 -0.00067 -0.00009 AFIX 43 H3 2 0.772062 0.877473 0.647987 11.00000 -1.20000 AFIX 0 C4 1 0.775443 0.655025 0.656517 11.00000 0.01495 0.01613 = 0.02052 -0.00304 0.00130 -0.00166 AFIX 43 H4 2 0.738523 0.648275 0.697866 11.00000 -1.20000 AFIX 0 C5 1 0.810360 0.526603 0.624563 11.00000 0.01332 0.01401 = 0.01572 0.00187 -0.00165 -0.00143 C6 1 0.864453 0.543025 0.561648 11.00000 0.02593 0.01671 = 0.02224 -0.00288 0.00812 0.00032 AFIX 43 H6 2 0.887614 0.459555 0.538268 11.00000 -1.20000 AFIX 0 C7 1 0.883380 0.680875 0.534440 11.00000 0.02881 0.02254 = 0.02155 0.00166 0.00791 -0.00412 AFIX 43 H7 2 0.919897 0.691203 0.493028 11.00000 -1.20000 AFIX 0 C8 1 0.792304 0.376976 0.657641 11.00000 0.02299 0.01542 = 0.02508 0.00498 0.00036 0.00067 AFIX 137 H8A 2 0.771145 0.310723 0.618485 11.00000 -1.50000 H8B 2 0.746596 0.385641 0.694756 11.00000 -1.50000 H8C 2 0.847613 0.338769 0.680859 11.00000 -1.50000 AFIX 0 N1 3 0.061784 0.958963 0.634662 11.00000 0.02072 0.01153 = 0.01655 0.00135 0.00346 0.00068 N2 3 -0.041712 1.275448 0.821537 11.00000 0.02061 0.01377 = 0.01648 -0.00200 0.00541 -0.00146 N3 3 0.849131 0.801452 0.567634 11.00000 0.02256 0.01264 = 0.02460 0.00298 -0.00154 -0.00558 AFIX 43 H3A 2 0.862034 0.887612 0.550237 11.00000 -1.20000 AFIX 0 O1 4 -0.111695 1.055417 0.708185 11.00000 0.01501 0.01301 = 0.02014 -0.00088 0.00068 -0.00085 OW1 4 0.000000 0.778072 0.750000 10.50000 0.03418 0.00625 = 0.02804 0.00000 0.01006 0.00000 S1 5 0.114204 0.865625 0.492354 11.00000 0.03261 0.01179 = 0.01335 -0.00095 0.00652 0.00035 S2 5 -0.106873 1.556337 0.860517 11.00000 0.02994 0.00886 = 0.02706 -0.00218 0.01265 0.00086 U1 6 0.000000 1.055360 0.750000 10.50000 0.01210 0.00619 = 0.01158 0.00000 0.00183 0.00000 HKLF 4 REM C2onc in C2/c REM R1 = 0.0223 for 3049 Fo > 4sig(Fo) and 0.0264 for all 3284 data REM 138 parameters refined using 0 restraints END WGHT 0.0155 6.0003 REM Instructions for potential hydrogen bonds EQIV $1 x+1, y, z HTAB C3 O1_$1 EQIV $2 -x+1/2, y-1/2, -z+3/2 HTAB C3 S2_$2 EQIV $3 -x+1, -y+1, -z+1 HTAB C6 S1_$3 EQIV $4 -x+1, -y+2, -z+1 HTAB N3 S1_$4 REM Highest difference peak 0.895, deepest hole -1.608, 1-sigma level 0.142 Q1 1 -0.0692 1.0563 0.7316 11.00000 0.05 0.89 Q2 1 0.0000 0.8148 0.7500 10.50000 0.05 0.81 Q3 1 -0.0270 0.9173 0.7347 11.00000 0.05 0.80 Q4 1 -0.0189 0.7067 0.7783 11.00000 0.05 0.79 Q5 1 -0.0379 1.1763 0.7527 11.00000 0.05 0.69 Q6 1 0.0059 1.0081 0.7175 11.00000 0.05 0.69 Q7 1 0.0000 1.2793 0.7500 10.50000 0.05 0.61 Q8 1 0.0042 1.1004 0.7225 11.00000 0.05 0.60 Q9 1 0.8477 0.5419 0.6012 11.00000 0.05 0.59 Q10 1 -0.0427 1.2616 0.7806 11.00000 0.05 0.55 Q11 1 -0.0440 1.5560 0.8604 11.00000 0.05 0.55 Q12 1 -0.0394 0.8473 0.7674 11.00000 0.05 0.54 Q13 1 -0.0590 0.9803 0.7806 11.00000 0.05 0.53 Q14 1 -0.0411 0.7765 0.7252 11.00000 0.05 0.52 Q15 1 0.0000 0.6812 0.7500 10.50000 0.05 0.52 Q16 1 0.6615 0.3643 0.7394 11.00000 0.05 0.50 Q17 1 0.0729 0.8997 0.6302 11.00000 0.05 0.50 Q18 1 -0.0480 0.8531 0.7189 11.00000 0.05 0.49 Q19 1 -0.0888 1.1060 0.6680 11.00000 0.05 0.47 Q20 1 -0.0109 1.6426 0.8496 11.00000 0.05 0.47 Q21 1 -0.0590 1.2031 0.8642 11.00000 0.05 0.45 Q22 1 -0.0561 1.3560 0.7728 11.00000 0.05 0.44 Q23 1 0.7463 0.3625 0.6589 11.00000 0.05 0.43 Q24 1 -0.0449 1.0334 0.5993 11.00000 0.05 0.43 Q25 1 -0.1311 1.0243 0.7140 11.00000 0.05 0.43 ; _shelx_res_checksum 60799 _shelx_hkl_file ; 2 0 0 214.98 5.20 -4 0 0 4.30 0.31 4 0 0 4.78 0.29 6 0 0 27.78 0.90 -6 0 0 27.70 0.97 -8 0 0 155.35 4.24 8 0 0 155.50 4.03 10 0 0 147.90 3.94 -10 0 0 146.97 4.15 12 0 0 18.02 0.94 -12 0 0 17.61 1.05 -14 0 0 27.78 1.48 14 0 0 25.45 1.27 16 0 0 36.43 1.66 -16 0 0 40.30 1.91 -18 0 0 38.62 2.08 18 0 0 42.37 1.92 20 0 0 22.60 1.61 1 -1 0 159.88 3.77 -1 -1 0 154.12 3.73 1 1 0 150.19 3.84 -1 1 0 151.68 3.86 1 1 0 150.96 4.27 -1 1 0 155.60 4.24 3 -1 0 209.17 5.06 -3 1 0 198.74 5.22 3 1 0 213.16 5.21 3 1 0 204.87 5.70 3 1 0 201.63 5.02 5 -1 0 63.80 1.73 -5 1 0 61.79 1.81 5 1 0 64.64 1.88 5 1 0 61.93 1.69 5 1 0 62.47 1.80 7 -1 0 96.84 2.64 7 1 0 98.96 2.61 -7 1 0 97.56 2.77 9 -1 0 58.08 1.79 -9 -1 0 57.74 1.88 9 1 0 59.36 1.76 -9 1 0 57.43 1.90 11 -1 0 51.73 1.71 -11 -1 0 51.46 1.83 -11 1 0 51.23 1.86 11 1 0 49.72 1.66 13 -1 0 45.62 1.73 -13 -1 0 46.48 1.87 -13 1 0 47.23 1.89 13 1 0 49.08 1.71 -15 -1 0 33.37 1.73 15 -1 0 34.05 1.55 15 1 0 34.23 1.51 -15 1 0 33.73 1.69 -17 -1 0 30.55 1.75 17 -1 0 26.61 1.53 17 1 0 25.65 1.49 -17 1 0 27.53 1.73 -19 -1 0 20.35 1.68 19 -1 0 18.07 1.46 -19 1 0 20.11 1.70 19 1 0 18.21 1.45 0 -2 0 151.39 3.79 0 2 0 153.81 4.31 2 -2 0 104.93 2.64 -2 -2 0 102.88 2.57 2 2 0 101.23 2.63 -2 2 0 102.54 2.93 2 2 0 103.98 2.98 -2 2 0 98.34 2.67 4 -2 0 7.43 0.43 -4 2 0 7.40 0.42 4 2 0 8.55 0.38 4 2 0 7.63 0.46 4 2 0 7.88 0.40 6 -2 0 17.39 0.73 6 2 0 17.77 0.67 6 2 0 18.53 0.74 6 2 0 17.79 0.76 -6 2 0 16.82 0.75 8 -2 0 47.07 1.53 -8 2 0 47.60 1.60 8 2 0 48.07 1.60 8 2 0 47.54 1.47 8 2 0 48.63 1.59 10 -2 0 61.65 2.00 -10 -2 0 64.11 2.09 10 2 0 63.61 1.94 -10 2 0 67.38 2.14 -12 -2 0 33.49 1.29 12 -2 0 32.72 1.39 -12 -2 0 32.13 1.44 -12 2 0 34.47 1.51 12 2 0 34.93 1.33 -14 -2 0 14.66 1.12 14 -2 0 12.35 1.00 -14 2 0 13.37 1.12 14 2 0 13.59 0.97 16 -2 0 26.68 1.48 -16 -2 0 24.12 1.58 16 2 0 24.88 1.40 -16 2 0 26.09 1.59 18 -2 0 13.70 1.25 -18 -2 0 15.69 1.46 -18 2 0 14.39 1.42 18 2 0 15.34 1.27 20 2 0 6.42 0.99 1 -3 0 16.08 0.65 -1 -3 0 17.30 0.62 -1 3 0 15.38 0.70 -1 3 0 15.18 0.57 1 3 0 16.41 0.54 1 3 0 15.86 0.72 -3 -3 0 95.61 2.48 3 -3 0 95.34 2.57 3 3 0 94.24 2.89 3 3 0 98.48 2.53 -3 3 0 97.45 2.82 -3 3 0 91.02 2.57 5 -3 0 43.62 1.35 -5 3 0 39.84 1.33 5 3 0 42.98 1.30 5 3 0 42.86 1.49 5 3 0 41.50 1.26 7 -3 0 1.97 0.36 7 3 0 2.97 0.40 7 3 0 2.46 0.35 -7 3 0 2.54 0.39 7 3 0 2.02 0.30 9 -3 0 5.32 0.57 9 3 0 5.34 0.53 9 3 0 5.75 0.57 9 3 0 5.55 0.50 -9 3 0 5.34 0.57 11 -3 0 5.63 0.66 11 3 0 5.05 0.55 -11 3 0 7.57 0.74 13 -3 0 24.08 1.23 -13 -3 0 22.29 1.26 -13 3 0 23.44 1.34 13 3 0 22.20 1.14 15 -3 0 9.95 1.02 -15 -3 0 7.71 0.96 -15 3 0 10.19 1.09 15 3 0 7.83 0.82 17 -3 0 6.78 0.95 -17 -3 0 7.14 1.09 -17 3 0 8.92 1.10 17 3 0 6.78 0.88 -19 -3 0 2.29 0.96 19 -3 0 4.38 0.93 19 3 0 3.54 0.80 -19 3 0 3.94 0.99 0 -4 0 0.08 0.21 0 4 0 0.12 0.24 0 4 0 0.18 0.16 2 -4 0 14.38 0.67 -2 -4 0 13.52 0.61 -2 4 0 14.64 0.71 -2 4 0 13.80 0.59 2 4 0 13.63 0.75 2 4 0 13.01 0.52 4 -4 0 15.01 0.72 -4 -4 0 13.69 0.61 4 4 0 13.52 0.77 -4 4 0 13.18 0.65 4 4 0 14.35 0.58 -4 4 0 13.11 0.68 6 -4 0 22.90 0.94 6 4 0 21.75 0.85 6 4 0 21.27 1.02 -6 4 0 18.53 0.88 8 -4 0 0.66 0.33 -8 4 0 0.23 0.34 8 4 0 -0.15 0.29 8 4 0 -0.15 0.31 8 4 0 -0.23 0.25 10 -4 0 0.12 0.37 10 4 0 0.23 0.37 10 4 0 0.61 0.39 10 4 0 -0.12 0.30 -10 4 0 -0.26 0.37 -12 -4 0 2.94 0.56 12 -4 0 3.53 0.64 12 4 0 4.06 0.59 -12 4 0 2.58 0.62 14 -4 0 1.81 0.59 -14 -4 0 1.27 0.57 -14 4 0 1.24 0.66 14 4 0 1.17 0.50 16 -4 0 1.98 0.71 -16 -4 0 0.93 0.71 -16 4 0 1.81 0.77 16 4 0 1.66 0.61 18 -4 0 -0.11 0.72 -18 -4 0 -0.15 0.76 -18 4 0 0.69 0.82 18 4 0 0.48 0.60 -1 -5 0 5.85 0.49 1 -5 0 4.70 0.47 -1 5 0 7.13 0.62 -1 5 0 5.33 0.40 1 5 0 4.72 0.52 1 5 0 5.10 0.35 -3 -5 0 2.74 0.35 3 -5 0 2.00 0.38 -3 5 0 2.28 0.32 3 5 0 2.46 0.28 3 5 0 1.95 0.40 -3 5 0 2.32 0.39 5 -5 0 0.55 0.29 -5 -5 0 0.55 0.26 5 5 0 0.99 0.24 -5 5 0 0.73 0.29 5 5 0 1.49 0.40 -5 5 0 0.61 0.29 -7 -5 0 4.33 0.44 7 -5 0 3.54 0.53 -7 5 0 4.04 0.50 7 5 0 4.41 0.59 -7 5 0 2.92 0.40 7 5 0 3.28 0.41 9 -5 0 4.67 0.64 9 5 0 4.85 0.58 9 5 0 5.53 0.69 -9 5 0 4.65 0.63 11 -5 0 0.72 0.50 11 5 0 0.94 0.48 -11 5 0 1.60 0.56 -13 -5 0 0.27 0.49 13 -5 0 0.13 0.51 13 5 0 0.57 0.44 -13 5 0 -0.49 0.54 -15 -5 0 0.67 0.59 15 -5 0 -0.06 0.57 15 5 0 0.13 0.47 -15 5 0 0.48 0.68 -17 -5 0 1.67 0.77 17 -5 0 2.87 0.89 17 5 0 1.75 0.66 -17 5 0 2.45 0.90 0 -6 0 30.42 1.18 0 6 0 30.45 1.35 0 6 0 29.83 1.02 -2 -6 0 43.93 1.52 2 -6 0 47.21 1.59 -2 6 0 46.45 1.76 2 6 0 46.10 1.39 -2 6 0 44.98 1.45 2 6 0 44.51 1.79 -4 -6 0 13.03 0.73 4 -6 0 13.00 0.82 4 6 0 13.27 0.92 -4 6 0 11.78 0.69 -4 6 0 12.57 0.84 4 6 0 13.44 0.62 6 -6 0 8.14 0.79 -6 -6 0 7.63 0.61 6 6 0 7.29 0.56 6 6 0 8.22 0.81 -6 6 0 6.38 0.63 -6 6 0 7.03 0.61 8 -6 0 11.16 0.96 -8 -6 0 9.90 0.74 -8 6 0 10.00 0.86 8 6 0 11.58 0.75 8 6 0 11.41 0.99 -10 -6 0 16.43 0.93 10 -6 0 13.14 1.06 -10 6 0 15.15 1.06 10 6 0 15.80 0.94 10 6 0 15.60 1.14 12 -6 0 12.77 1.13 -12 -6 0 12.86 0.91 12 6 0 11.94 1.09 -12 6 0 13.26 1.11 14 -6 0 5.30 0.86 -14 6 0 5.24 0.83 16 -6 0 3.24 0.82 -16 6 0 3.95 0.89 1 -7 0 22.05 1.07 -1 -7 0 22.11 1.04 -1 7 0 21.76 1.22 1 7 0 20.73 1.21 -1 7 0 22.41 0.88 1 7 0 21.38 0.84 -3 -7 0 38.89 1.46 3 -7 0 38.67 1.54 -3 7 0 39.99 1.39 3 7 0 40.94 1.77 -3 7 0 41.30 1.71 -5 -7 0 92.36 2.77 5 -7 0 91.76 2.90 5 7 0 95.91 3.32 -5 7 0 93.94 2.80 -5 7 0 98.20 3.16 7 -7 0 18.36 1.13 -7 -7 0 18.18 0.96 7 7 0 17.61 1.25 -7 7 0 17.98 1.05 -7 7 0 18.13 1.02 -9 -7 0 13.28 0.91 9 -7 0 13.45 1.15 9 7 0 12.96 1.17 -9 7 0 14.73 1.03 11 -7 0 20.67 1.40 -11 -7 0 20.12 1.17 11 7 0 21.50 1.43 -11 7 0 24.46 1.37 -13 -7 0 42.11 1.73 13 -7 0 40.72 1.96 -13 7 0 42.36 1.97 13 7 0 38.34 1.98 15 -7 0 19.95 1.55 -15 7 0 22.68 1.59 0 -8 0 78.44 2.51 0 8 0 77.25 2.87 -2 -8 0 56.16 1.95 2 -8 0 56.56 2.00 -2 8 0 56.94 2.27 2 8 0 55.00 2.30 4 -8 0 21.93 1.23 -4 -8 0 24.13 1.15 4 8 0 23.19 1.42 -4 8 0 23.43 1.34 6 -8 0 30.68 1.50 -6 -8 0 30.50 1.35 6 8 0 31.88 1.74 -6 8 0 33.93 1.47 -6 8 0 33.95 1.55 8 -8 0 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-3 -20 0.58 0.63 -3 3 -20 0.98 0.65 3 3 20 0.30 0.51 -5 -3 -20 22.18 1.58 5 3 20 21.89 1.45 -5 3 -20 19.53 1.62 -7 -3 -20 8.81 1.16 7 3 20 6.04 0.98 -7 3 -20 6.88 1.12 -9 -3 -20 1.14 0.86 -9 3 -20 2.21 0.89 9 3 20 1.59 0.86 -10 -4 20 1.56 0.69 -8 -4 20 0.19 0.50 8 4 -20 1.19 0.70 -8 4 20 -1.44 0.52 -6 -4 20 -0.19 0.45 -6 4 20 -0.18 0.53 6 4 -20 -0.23 0.60 -4 -4 20 0.57 0.52 4 -4 -20 1.53 0.53 4 4 -20 0.42 0.65 -4 4 20 -0.07 0.52 2 -4 -20 2.78 0.69 2 4 -20 2.81 0.80 -2 4 20 3.92 0.74 0 -4 -20 0.46 0.56 0 4 20 -0.05 0.46 0 4 -20 -0.41 0.54 -2 -4 -20 0.35 0.56 -2 4 -20 0.41 0.69 2 4 20 0.76 0.55 -4 -4 -20 2.29 0.73 4 4 20 4.27 0.81 -4 4 -20 2.68 0.87 -6 -4 -20 1.04 0.70 -6 4 -20 1.47 0.79 6 4 20 1.42 0.71 -8 -4 -20 1.80 0.92 -8 4 -20 1.27 0.78 -9 -5 20 0.88 0.64 9 5 -20 0.68 0.75 -7 -5 20 1.47 0.63 -7 5 20 1.19 0.70 7 5 -20 1.04 0.76 -5 -5 20 0.27 0.55 -5 5 20 0.21 0.58 5 5 -20 0.25 0.64 3 -5 -20 0.39 0.53 -3 -5 20 0.54 0.53 3 5 -20 0.22 0.66 -3 5 20 0.08 0.54 1 -5 -20 0.47 0.51 1 5 -20 0.24 0.64 -1 5 20 -0.06 0.50 -1 -5 -20 -0.95 0.47 -1 5 -20 0.69 0.72 1 5 20 0.50 0.51 -3 -5 -20 -0.30 0.54 -3 5 -20 0.70 0.74 3 5 20 0.66 0.60 -5 -5 -20 0.61 0.72 -5 5 -20 0.86 0.77 5 5 20 0.13 0.67 -7 5 -20 0.41 0.80 -6 -6 20 9.64 1.06 6 6 -20 7.67 1.17 -4 -6 20 4.09 0.80 -4 6 20 3.41 0.84 4 6 -20 4.79 0.99 -2 -6 20 4.08 0.80 2 -6 -20 2.29 0.73 -2 6 20 2.46 0.70 2 6 -20 5.05 0.98 0 -6 -20 3.60 0.84 0 -6 20 4.90 0.88 0 6 -20 2.30 0.87 0 6 20 4.87 0.90 -2 -6 -20 3.73 0.88 -2 6 -20 4.21 0.98 2 6 20 3.75 0.85 -4 -6 -20 4.50 1.02 -4 6 -20 3.92 1.01 -3 -7 20 33.83 1.87 1 -7 -20 10.84 1.25 -1 -7 20 11.22 1.19 1 -7 20 4.64 0.91 -1 -7 -20 4.50 0.96 6 0 -21 0.05 0.47 -6 0 21 0.07 0.43 -4 0 21 0.35 0.41 4 0 -21 0.47 0.48 2 0 -21 0.09 0.48 -2 0 21 0.03 0.38 0 0 21 -0.40 0.40 0 0 -21 -0.13 0.49 2 0 21 0.22 0.45 -2 0 -21 1.50 0.60 4 0 21 0.32 0.50 -4 0 -21 -0.03 0.57 -6 0 -21 -0.19 0.62 6 0 21 0.99 0.58 8 0 21 0.68 0.67 -8 0 -21 -0.32 0.69 10 0 21 0.36 0.69 -11 1 21 5.94 0.93 -9 1 21 7.21 0.96 7 1 -21 0.90 0.51 -7 1 21 0.30 0.48 5 -1 -21 -0.06 0.45 5 1 -21 0.07 0.50 -5 1 21 -0.29 0.40 3 -1 -21 1.75 0.60 3 1 -21 1.90 0.62 -3 1 21 2.15 0.57 1 -1 -21 11.43 1.19 1 1 -21 11.67 1.18 -1 1 21 10.90 1.01 1 -1 21 1.36 0.51 -1 -1 -21 3.51 0.75 -1 1 -21 3.19 0.79 1 1 21 2.18 0.58 3 -1 21 0.44 0.47 -3 -1 -21 0.00 0.55 3 1 21 0.15 0.50 -3 1 -21 0.61 0.58 5 -1 21 0.42 0.53 -5 -1 -21 0.25 0.64 -5 1 -21 0.34 0.66 5 1 21 0.02 0.58 7 -1 21 1.73 0.67 -7 -1 -21 3.64 0.92 -7 1 -21 3.07 0.88 7 1 21 1.92 0.73 9 -1 21 3.16 0.82 -9 -1 -21 4.60 1.13 -9 1 -21 6.53 1.09 9 1 21 3.91 0.90 -10 2 21 12.00 1.22 -8 2 21 18.48 1.41 -6 2 21 4.73 0.82 6 2 -21 3.91 0.80 4 -2 -21 2.51 0.64 -4 2 21 3.57 0.69 4 2 -21 3.65 0.81 2 -2 -21 9.23 1.04 -2 2 21 9.57 1.02 2 2 -21 8.98 1.07 0 -2 -21 18.59 1.38 0 2 21 19.87 1.25 0 2 -21 17.69 1.44 -2 -2 -21 13.33 1.22 2 2 21 10.99 1.06 -2 2 -21 11.73 1.19 -4 -2 -21 7.80 1.05 4 2 21 8.03 0.94 -4 2 -21 9.70 1.16 -6 -2 -21 5.76 0.98 6 2 21 7.06 0.99 -6 2 -21 6.27 1.09 -8 -2 -21 7.80 1.15 -8 2 -21 7.48 1.18 8 2 21 7.06 1.06 -9 -3 21 15.41 1.26 -9 3 21 20.39 1.51 7 3 -21 8.58 1.13 -7 3 21 7.91 1.01 5 -3 -21 9.88 1.09 -5 3 21 11.21 1.19 5 3 -21 8.76 1.10 3 -3 -21 28.00 1.61 -3 3 21 26.13 1.52 3 3 -21 27.45 1.74 1 -3 -21 40.03 1.99 -1 3 21 40.47 1.89 1 3 -21 40.54 2.15 -1 -3 -21 26.97 1.71 1 3 21 31.43 1.63 -1 3 -21 31.11 1.89 -3 -3 -21 10.47 1.17 -3 3 -21 9.98 1.20 3 3 21 9.55 1.07 -5 -3 -21 8.78 1.12 5 3 21 7.68 1.00 -5 3 -21 6.33 1.03 -7 -3 -21 12.47 1.37 7 3 21 11.72 1.29 -7 3 -21 11.46 1.34 -8 -4 21 31.68 1.65 -8 4 21 28.86 1.94 8 4 -21 31.76 2.02 -6 -4 21 34.25 1.74 6 4 -21 30.58 1.98 -6 4 21 32.72 1.86 4 -4 -21 15.42 1.21 4 4 -21 12.55 1.30 -4 4 21 15.95 1.40 2 -4 -21 10.50 1.15 -2 4 21 13.50 1.26 2 4 -21 10.31 1.21 0 -4 -21 19.46 1.47 0 4 -21 23.43 1.70 0 4 21 22.03 1.43 -2 -4 -21 42.65 2.18 2 4 21 41.37 2.02 -2 4 -21 39.80 2.26 -4 -4 -21 16.81 1.51 -4 4 -21 17.95 1.66 4 4 21 19.66 1.47 -6 -4 -21 9.69 1.27 6 4 21 12.02 1.23 -6 4 -21 10.92 1.31 -7 -5 21 11.53 1.13 7 5 -21 10.62 1.29 -5 -5 21 24.01 1.51 -5 5 21 24.16 1.69 5 5 -21 29.55 1.94 3 -5 -21 22.42 1.52 3 5 -21 23.30 1.79 -3 5 21 23.09 1.56 1 -5 -21 17.80 1.42 -1 5 21 15.89 1.34 1 5 -21 19.27 1.63 -1 -5 -21 17.05 1.46 -1 5 -21 19.56 1.69 1 5 21 17.73 1.39 -3 -5 -21 18.52 1.58 3 5 21 20.89 1.55 -3 5 -21 20.89 1.75 -4 -6 21 22.48 1.53 2 -6 -21 6.58 1.00 0 -6 -21 9.63 1.18 6 0 -22 24.10 1.58 -4 0 22 47.04 1.94 4 0 -22 43.81 2.16 -2 0 22 21.51 1.26 2 0 -22 22.59 1.51 0 0 -22 19.05 1.44 0 0 22 16.73 1.17 -2 0 -22 8.56 1.08 2 0 22 7.25 0.87 4 0 22 16.94 1.28 -4 0 -22 17.22 1.49 -6 0 -22 28.50 1.86 6 0 22 25.90 1.60 8 0 22 11.99 1.20 -9 1 22 16.21 1.34 -7 1 22 14.68 1.21 5 -1 -22 11.76 1.20 -5 1 22 11.19 1.11 5 1 -22 11.63 1.21 3 -1 -22 25.03 1.60 -3 1 22 27.17 1.46 3 1 -22 26.15 1.67 1 -1 -22 30.57 1.73 -1 1 22 28.66 1.49 1 1 -22 26.38 1.71 -1 -1 -22 14.14 1.31 1 1 22 15.52 1.15 -1 1 -22 12.87 1.27 -3 -1 -22 11.58 1.23 -3 1 -22 9.97 1.16 3 1 22 10.57 1.06 -5 -1 -22 14.73 1.43 -5 1 -22 16.25 1.49 5 1 22 10.41 1.14 7 -1 22 21.08 1.57 -7 1 -22 23.17 1.87 7 1 22 21.56 1.60 9 -1 22 21.53 1.63 -8 2 22 9.18 1.08 6 2 -22 14.32 1.38 -6 2 22 12.34 1.21 4 -2 -22 12.36 1.18 4 2 -22 16.26 1.38 -4 2 22 13.87 1.15 2 -2 -22 12.66 1.19 2 2 -22 10.35 1.22 -2 2 22 11.61 1.09 0 -2 -22 10.22 1.14 0 2 -22 10.19 1.16 0 2 22 11.11 1.07 -2 -2 -22 12.64 1.25 2 2 22 12.27 1.13 -2 2 -22 11.20 1.21 -4 -2 -22 12.49 1.29 -4 2 -22 9.94 1.18 4 2 22 10.88 1.11 -6 -2 -22 9.85 1.22 -6 2 -22 10.88 1.32 6 2 22 8.48 1.07 -7 3 22 9.63 1.14 7 3 -22 8.13 1.11 -5 3 22 5.57 0.91 5 3 -22 5.51 1.03 3 -3 -22 -0.07 0.45 3 3 -22 -0.03 0.58 -3 3 22 0.42 0.54 1 -3 -22 6.68 0.93 -1 3 22 5.48 0.87 1 3 -22 6.72 1.03 -1 -3 -22 9.20 1.17 -1 3 -22 8.60 1.10 1 3 22 6.92 0.95 -3 -3 -22 5.34 0.95 3 3 22 5.35 0.94 -3 3 -22 8.29 1.16 -5 -3 -22 0.32 0.72 5 3 22 -0.14 0.60 -5 3 -22 0.93 0.81 8 4 -22 8.68 1.25 6 4 -22 3.20 0.90 4 -4 -22 -0.25 0.47 4 4 -22 0.16 0.66 -4 4 22 -0.07 0.51 2 -4 -22 -0.12 0.42 -2 4 22 -0.05 0.50 2 4 -22 1.03 0.76 0 -4 -22 0.57 0.55 0 4 -22 0.89 0.68 0 4 22 0.12 0.53 -2 -4 -22 3.00 0.90 2 4 22 4.24 0.88 -2 4 -22 3.94 0.96 3 -5 -22 0.62 0.57 1 -5 -22 0.08 0.55 -1 -5 -22 -0.25 0.60 2 -6 -22 6.21 1.10 6 0 -23 0.01 0.55 4 0 -23 0.93 0.58 2 0 -23 0.47 0.54 0 0 23 0.10 0.47 0 0 -23 0.27 0.57 -2 0 -23 0.22 0.61 2 0 23 -0.29 0.46 -4 0 -23 0.54 0.68 4 0 23 -1.05 0.50 6 0 23 0.33 0.65 -7 1 23 3.43 0.76 5 -1 -23 4.81 0.86 5 1 -23 4.71 0.87 -5 1 23 4.54 0.79 3 -1 -23 2.78 0.72 -3 1 23 1.99 0.58 3 1 -23 1.34 0.66 1 -1 -23 -0.08 0.54 1 1 -23 0.36 0.58 -1 1 23 0.03 0.44 -1 -1 -23 0.70 0.59 1 1 23 2.29 0.65 -1 1 -23 1.30 0.70 -3 -1 -23 4.42 0.94 -3 1 -23 3.94 0.91 3 1 23 5.02 0.82 5 1 23 1.03 0.69 -6 2 23 15.76 1.28 6 2 -23 14.75 1.43 4 -2 -23 14.73 1.29 4 2 -23 15.38 1.44 -4 2 23 14.55 1.30 2 -2 -23 3.26 0.75 2 2 -23 1.48 0.68 -2 2 23 3.91 0.73 0 -2 -23 1.61 0.65 0 2 23 1.92 0.65 0 2 -23 1.47 0.71 -2 -2 -23 8.40 1.14 2 2 23 8.48 1.02 -2 2 -23 7.75 1.11 4 2 23 13.90 1.25 7 3 -23 15.18 1.50 -5 3 23 10.87 1.24 5 3 -23 12.35 1.38 3 -3 -23 8.15 1.05 3 3 -23 7.47 1.09 -3 3 23 10.74 1.17 1 -3 -23 16.40 1.40 -1 3 23 16.70 1.31 1 3 -23 14.41 1.44 -1 -3 -23 22.47 1.59 -1 3 -23 22.49 1.79 1 3 23 20.80 1.48 3 3 23 19.06 1.51 2 -4 -23 16.23 1.36 0 -4 -23 13.36 1.40 3 -5 -23 6.42 1.01 4 0 -24 19.29 1.52 2 0 -24 16.17 1.42 0 0 -24 23.90 1.76 4 0 24 16.41 1.40 5 -1 -24 10.68 1.21 5 1 -24 10.18 1.22 -5 1 24 9.30 1.03 3 -1 -24 7.01 1.05 3 1 -24 7.99 1.09 -3 1 24 8.14 0.99 1 -1 -24 12.31 1.28 -1 1 24 10.24 1.09 1 1 -24 12.13 1.36 1 1 24 32.64 1.75 3 1 24 15.42 1.28 4 -2 -24 10.23 1.19 -4 2 24 13.65 1.29 2 -2 -24 10.59 1.19 -2 2 24 11.31 1.14 0 2 24 8.88 1.05 2 2 24 6.12 0.93 3 -3 -24 5.38 1.01 -1 1 25 5.29 0.85 1 1 25 4.03 0.88 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 55706 _symmetry_cell_setting monoclinic _symmetry_space_group_name_h-m 'C 2/c' _symmetry_int_tables_number 15 _chemical_absolute_configuration ? _database_code_depnum_ccdc_archive 'CCDC 967159' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound_6 _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety '(C6 H8 N1 1+)2, (U O3 C4 H2 N4 S4 2-)' _chemical_formula_sum 'C16 H18 N6 O3 S4 U' _exptl_crystal_recrystallization_method 'Slow Aqueous Evaporation' _chemical_melting_point ? _exptl_crystal_description Prism _exptl_crystal_colour Yellow _diffrn_ambient_temperature 100(2) _chemical_formula_weight 708.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 11 _space_group_name_H-M_alt 'P 21/m' _space_group_name_Hall '-P 2yb' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 8.761(2) _cell_length_b 16.018(4) _cell_length_c 16.129(4) _cell_angle_alpha 90 _cell_angle_beta 95.282(4) _cell_angle_gamma 90 _cell_volume 2253.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3692 _cell_measurement_theta_min 5.073 _cell_measurement_theta_max 48.472 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.088 _exptl_crystal_F_000 1344 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.107 _exptl_crystal_size_min 0.062 _exptl_absorpt_coefficient_mu 7.603 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5661 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_process_details 'SADABS, G. Sheldrick (1999)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_measurement_device_type 'Bruker ApexII CCD' _diffrn_measurement_method 'Omega and Phi Scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25394 _diffrn_reflns_av_unetI/netI 0.0840 _diffrn_reflns_av_R_equivalents 0.0923 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.268 _diffrn_reflns_theta_max 30.443 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.932 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.932 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.932 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 6584 _reflns_number_gt 5115 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'APEX II (Bruker AXS, 2013)' _computing_cell_refinement 'SAINT (Bruker AXS, 2013)' _computing_data_reduction 'SAINT (Bruker AXS, 2013)' _computing_structure_solution 'SIR92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Crystal Maker v.8.2.2 (Palmer 2009)' _computing_publication_material 'WINGX (Farrugia, 2012)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0240P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 6584 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.0986 _refine_ls_wR_factor_gt 0.0909 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5468(9) 0.2500 0.0494(5) 0.0165(17) Uani 1 2 d S T P . . C2 C 0.9645(9) 0.2500 0.1482(5) 0.0126(15) Uani 1 2 d S T P . . C3 C 0.9989(8) 0.2500 0.3884(4) 0.0098(14) Uani 1 2 d S T P . . C4 C 0.5552(8) 0.2500 0.4831(5) 0.0117(15) Uani 1 2 d S T P . . C5 C 1.0370(6) 0.9660(4) 0.2499(3) 0.0129(11) Uani 1 1 d . . . . . C6 C 0.5873(6) 0.6298(3) 0.2497(3) 0.0123(11) Uani 1 1 d . . . . . C7 C 0.8036(7) -0.0188(4) 0.4135(3) 0.0176(12) Uani 1 1 d . . . . . H7 H 0.8217 -0.0435 0.3632 0.021 Uiso 1 1 calc R U . . . C8 C 0.7154(7) -0.0595(4) 0.4658(4) 0.0191(12) Uani 1 1 d . . . . . H8 H 0.6741 -0.1116 0.4514 0.023 Uiso 1 1 calc R U . . . C9 C 0.6874(6) -0.0220(4) 0.5420(3) 0.0151(12) Uani 1 1 d . . . . . C10 C 0.7545(6) 0.0571(3) 0.5605(3) 0.0146(11) Uani 1 1 d . . . . . H10 H 0.7395 0.0833 0.6106 0.018 Uiso 1 1 calc R U . . . C11 C 0.8403(7) 0.0947(4) 0.5058(4) 0.0202(13) Uani 1 1 d . . . . . H11 H 0.8826 0.1470 0.5180 0.024 Uiso 1 1 calc R U . . . C12 C 0.5982(6) -0.0591(3) 0.5948(3) 0.0095(10) Uani 1 1 d . . . . . H12A H 0.6375 -0.0474 0.6511 0.014 Uiso 1 1 calc R U . . . H12B H 0.5980 -0.1184 0.5858 0.014 Uiso 1 1 calc R U . . . H12C H 0.4955 -0.0382 0.5852 0.014 Uiso 1 1 calc R U . . . C13 C 0.6767(6) 0.5730(4) 0.9793(4) 0.0173(12) Uani 1 1 d . . . . . H13 H 0.6405 0.6203 0.9505 0.021 Uiso 1 1 calc R U . . . C14 C 0.7663(6) 0.5183(3) 0.9423(4) 0.0152(11) Uani 1 1 d . . . . . H14 H 0.7906 0.5280 0.8882 0.018 Uiso 1 1 calc R U . . . C15 C 0.8240(6) 0.4457(3) 0.9859(4) 0.0131(11) Uani 1 1 d . . . . . C16 C 0.7818(7) 0.4354(4) 1.0676(4) 0.0176(12) Uani 1 1 d . . . . . H16 H 0.8171 0.3893 1.0989 0.021 Uiso 1 1 calc R U . . . C17 C 0.6900(7) 0.4923(4) 1.1010(4) 0.0199(13) Uani 1 1 d . . . . . H17 H 0.6620 0.4845 1.1547 0.024 Uiso 1 1 calc R U . . . C18 C 0.9132(5) 0.3910(3) 0.9516(3) 0.0057(9) Uani 1 1 d . . . . . H18A H 0.9705 0.4190 0.9119 0.009 Uiso 1 1 calc R U . . . H18B H 0.8510 0.3482 0.9240 0.009 Uiso 1 1 calc R U . . . H18C H 0.9827 0.3663 0.9942 0.009 Uiso 1 1 calc R U . . . N1 N 0.5371(7) 0.2500 0.1224(4) 0.0159(14) Uani 1 2 d S T P . . N2 N 0.8578(7) 0.2500 0.1857(4) 0.0139(14) Uani 1 2 d S T P . . N3 N 0.8720(8) 0.2500 0.3605(4) 0.0224(16) Uani 1 2 d S T P . . N4 N 0.5572(8) 0.2500 0.4096(4) 0.0178(15) Uani 1 2 d S T P . . N5 N 1.0215(5) 0.8942(3) 0.2396(3) 0.0158(10) Uani 1 1 d . . . . . N6 N 0.7081(5) 0.6607(3) 0.2588(3) 0.0147(10) Uani 1 1 d . . . . . N7 N 0.8649(6) 0.0564(3) 0.4330(3) 0.0219(11) Uani 1 1 d . . . . . H7A H 0.9206 0.0806 0.3989 0.026 Uiso 1 1 calc R U . . . N8 N 0.6391(6) 0.5598(3) 1.0568(3) 0.0182(11) Uani 1 1 d . . . . . H8A H 0.5812 0.5952 1.0789 0.022 Uiso 1 1 calc R U . . . O1 O 0.6369(4) 0.1398(2) 0.2692(2) 0.0168(9) Uani 1 1 d . . . . . O2 O 0.9738(6) 0.7500 0.3564(3) 0.0176(12) Uani 1 2 d S T P . . O3 O 0.8938(6) 0.7500 0.1386(3) 0.0149(12) Uani 1 2 d S T P . . OW1 O 0.3522(6) 0.2500 0.2610(4) 0.0236(14) Uani 1 2 d S T P . . OW2 O 1.2086(6) 0.7500 0.2272(3) 0.0159(12) Uani 1 2 d S T P . . S1 S 0.5555(3) 0.2500 -0.04947(13) 0.0201(4) Uani 1 2 d S T P . . S2 S 1.1099(2) 0.2500 0.09112(12) 0.0140(4) Uani 1 2 d S T P . . S3 S 1.1749(2) 0.2500 0.42978(14) 0.0227(5) Uani 1 2 d S T P . . S4 S 0.5426(3) 0.2500 0.58146(13) 0.0183(4) Uani 1 2 d S T P . . S5 S 1.06069(18) 1.06576(9) 0.26263(9) 0.0180(3) Uani 1 1 d . . . . . S6 S 0.42167(15) 0.58262(9) 0.23438(9) 0.0145(3) Uani 1 1 d . . . . . U1 U 0.63693(3) 0.2500 0.26921(2) 0.00971(8) Uani 1 2 d S T P . . U2 U 0.93156(3) 0.7500 0.24751(2) 0.00930(8) Uani 1 2 d S T P . . 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 0.010(4) 0.017(4) 0.023(5) 0.000 0.008(3) 0.000 C2 0.017(4) 0.007(4) 0.013(4) 0.000 -0.005(3) 0.000 C3 0.011(3) 0.013(4) 0.006(3) 0.000 0.007(3) 0.000 C4 0.011(3) 0.008(4) 0.016(4) 0.000 0.000(3) 0.000 C5 0.011(2) 0.018(3) 0.010(3) 0.002(2) 0.003(2) 0.001(2) C6 0.014(3) 0.013(3) 0.010(3) 0.000(2) 0.004(2) 0.008(2) C7 0.027(3) 0.014(3) 0.012(3) -0.002(2) 0.000(2) 0.001(2) C8 0.023(3) 0.017(3) 0.017(3) -0.001(2) 0.000(2) 0.001(2) C9 0.011(3) 0.020(3) 0.014(3) -0.001(2) 0.002(2) 0.004(2) C10 0.019(3) 0.016(3) 0.009(3) 0.002(2) 0.002(2) 0.001(2) C11 0.028(3) 0.012(3) 0.019(3) 0.000(2) 0.000(3) 0.006(2) C12 0.008(2) 0.013(3) 0.008(2) -0.004(2) 0.0017(19) -0.002(2) C13 0.016(3) 0.020(3) 0.016(3) 0.010(2) 0.001(2) 0.003(2) C14 0.016(3) 0.016(3) 0.014(3) -0.001(2) 0.004(2) -0.003(2) C15 0.012(3) 0.012(3) 0.015(3) -0.005(2) 0.001(2) -0.004(2) C16 0.023(3) 0.015(3) 0.014(3) 0.004(2) -0.002(2) 0.003(2) C17 0.025(3) 0.019(3) 0.016(3) 0.002(2) 0.005(2) 0.002(2) C18 0.004(2) 0.005(2) 0.009(2) -0.0010(18) 0.0042(18) 0.0006(18) N1 0.014(3) 0.019(4) 0.015(3) 0.000 0.003(3) 0.000 N2 0.012(3) 0.018(4) 0.012(3) 0.000 0.006(3) 0.000 N3 0.019(4) 0.034(4) 0.015(4) 0.000 0.005(3) 0.000 N4 0.013(3) 0.028(4) 0.012(3) 0.000 0.001(3) 0.000 N5 0.013(2) 0.012(2) 0.022(3) -0.004(2) 0.003(2) -0.0012(19) N6 0.012(2) 0.016(2) 0.017(2) 0.0028(19) 0.0058(19) -0.0012(19) N7 0.031(3) 0.019(3) 0.017(3) 0.003(2) 0.006(2) -0.006(2) N8 0.018(2) 0.017(3) 0.020(3) -0.003(2) 0.004(2) 0.008(2) O1 0.016(2) 0.016(2) 0.019(2) 0.0039(16) 0.0027(17) 0.0008(16) O2 0.018(3) 0.023(3) 0.012(3) 0.000 0.005(2) 0.000 O3 0.015(3) 0.015(3) 0.016(3) 0.000 0.003(2) 0.000 OW1 0.014(3) 0.041(4) 0.015(3) 0.000 0.000(2) 0.000 OW2 0.016(3) 0.015(3) 0.018(3) 0.000 0.007(2) 0.000 S1 0.0308(12) 0.0175(11) 0.0130(10) 0.000 0.0068(9) 0.000 S2 0.0132(9) 0.0158(10) 0.0139(10) 0.000 0.0056(7) 0.000 S3 0.0105(9) 0.0374(13) 0.0195(11) 0.000 -0.0017(8) 0.000 S4 0.0253(11) 0.0191(11) 0.0105(9) 0.000 0.0028(8) 0.000 S5 0.0279(8) 0.0107(7) 0.0161(7) -0.0006(5) 0.0051(6) -0.0006(6) S6 0.0114(6) 0.0148(7) 0.0174(7) -0.0016(5) 0.0026(5) -0.0026(5) U1 0.00873(14) 0.01165(15) 0.00880(14) 0.000 0.00113(10) 0.000 U2 0.00882(14) 0.00958(14) 0.00978(14) 0.000 0.00231(10) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.188(10) . ? C1 S1 1.604(9) . ? C2 N2 1.160(10) . ? C2 S2 1.638(8) . ? C3 N3 1.160(10) . ? C3 S3 1.622(8) . ? C4 N4 1.188(9) . ? C4 S4 1.601(8) . ? C5 N5 1.167(7) . ? C5 S5 1.623(6) . ? C6 N6 1.165(7) . ? C6 S6 1.635(6) . ? C7 N7 1.344(7) . ? C7 C8 1.361(8) . ? C7 H7 0.9300 . ? C8 C9 1.409(8) . ? C8 H8 0.9300 . ? C9 C12 1.347(7) . ? C9 C10 1.417(8) . ? C10 C11 1.353(8) . ? C10 H10 0.9300 . ? C11 N7 1.360(7) . ? C11 H11 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 N8 1.339(7) . ? C13 C14 1.351(8) . ? C13 H13 0.9300 . ? C14 C15 1.428(8) . ? C14 H14 0.9300 . ? C15 C18 1.328(7) . ? C15 C16 1.411(8) . ? C16 C17 1.359(8) . ? C16 H16 0.9300 . ? C17 N8 1.349(7) . ? C17 H17 0.9300 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? N1 U1 2.447(7) . ? N2 U1 2.457(6) . ? N3 U1 2.419(7) . ? N4 U1 2.430(7) . ? N5 U2 2.448(5) . ? N6 U2 2.445(5) . ? N7 H7A 0.8600 . ? N8 H8A 0.8600 . ? O1 U1 1.765(4) . ? O2 U2 1.761(5) . ? O3 U2 1.757(5) . ? OW1 U1 2.486(6) . ? OW2 U2 2.479(5) . ? U1 O1 1.765(4) 4_565 ? U2 N6 2.445(5) 4_575 ? U2 N5 2.448(5) 4_575 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 S1 178.7(7) . . ? N2 C2 S2 177.3(7) . . ? N3 C3 S3 178.6(7) . . ? N4 C4 S4 176.9(7) . . ? N5 C5 S5 178.9(5) . . ? N6 C6 S6 177.1(5) . . ? N7 C7 C8 121.4(5) . . ? N7 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C7 C8 C9 119.4(6) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C12 C9 C8 121.4(5) . . ? C12 C9 C10 121.0(5) . . ? C8 C9 C10 117.6(5) . . ? C11 C10 C9 120.3(5) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 N7 120.3(6) . . ? C10 C11 H11 119.9 . . ? N7 C11 H11 119.9 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N8 C13 C14 120.9(5) . . ? N8 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C13 C14 C15 120.2(5) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C18 C15 C16 121.8(5) . . ? C18 C15 C14 121.8(5) . . ? C16 C15 C14 116.4(5) . . ? C17 C16 C15 120.4(5) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? N8 C17 C16 120.5(6) . . ? N8 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C1 N1 U1 155.1(6) . . ? C2 N2 U1 178.2(6) . . ? C3 N3 U1 165.5(6) . . ? C4 N4 U1 164.2(6) . . ? C5 N5 U2 162.8(4) . . ? C6 N6 U2 164.5(4) . . ? C7 N7 C11 121.0(5) . . ? C7 N7 H7A 119.5 . . ? C11 N7 H7A 119.5 . . ? C13 N8 C17 121.5(5) . . ? C13 N8 H8A 119.3 . . ? C17 N8 H8A 119.3 . . ? O1 U1 O1 180.0(3) 4_565 . ? O1 U1 N3 90.01(12) 4_565 . ? O1 U1 N3 90.00(13) . . ? O1 U1 N4 89.98(12) 4_565 . ? O1 U1 N4 89.98(12) . . ? N3 U1 N4 74.6(2) . . ? O1 U1 N1 90.01(13) 4_565 . ? O1 U1 N1 90.01(13) . . ? N3 U1 N1 142.9(2) . . ? N4 U1 N1 142.5(2) . . ? O1 U1 N2 90.02(12) 4_565 . ? O1 U1 N2 90.02(12) . . ? N3 U1 N2 70.4(2) . . ? N4 U1 N2 145.0(2) . . ? N1 U1 N2 72.5(2) . . ? O1 U1 OW1 89.98(12) 4_565 . ? O1 U1 OW1 89.98(12) . . ? N3 U1 OW1 145.7(2) . . ? N4 U1 OW1 71.1(2) . . ? N1 U1 OW1 71.4(2) . . ? N2 U1 OW1 143.9(2) . . ? O3 U2 O2 178.7(2) . . ? O3 U2 N6 89.76(18) . 4_575 ? O2 U2 N6 91.27(18) . 4_575 ? O3 U2 N6 89.76(18) . . ? O2 U2 N6 91.26(18) . . ? N6 U2 N6 71.6(2) 4_575 . ? O3 U2 N5 88.84(13) . 4_575 ? O2 U2 N5 90.74(13) . 4_575 ? N6 U2 N5 145.07(16) 4_575 4_575 ? N6 U2 N5 73.48(15) . 4_575 ? O3 U2 N5 88.84(13) . . ? O2 U2 N5 90.74(13) . . ? N6 U2 N5 73.48(15) 4_575 . ? N6 U2 N5 145.07(15) . . ? N5 U2 N5 141.4(2) 4_575 . ? O3 U2 OW2 87.9(2) . . ? O2 U2 OW2 90.8(2) . . ? N6 U2 OW2 144.13(11) 4_575 . ? N6 U2 OW2 144.13(11) . . ? N5 U2 OW2 70.68(11) 4_575 . ? N5 U2 OW2 70.68(11) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C7 H7 N6 0.93 2.65 3.422(7) 140.4 4_565 C8 H8 S4 0.93 2.94 3.832(6) 162.4 3_656 C10 H10 S6 0.93 2.98 3.799(6) 147.4 2_646 C14 H14 S5 0.93 2.93 3.836(6) 166.4 2_746 C16 H16 N2 0.93 2.64 3.557(7) 168.3 1_556 C17 H17 S6 0.93 3.01 3.631(6) 125.7 1_556 N7 H7A S5 0.86 2.63 3.374(5) 146.2 1_545 N8 H8A S1 0.86 2.78 3.488(5) 141.2 3_666 N8 H8A S6 0.86 2.99 3.601(5) 130.0 1_556 _refine_diff_density_max 1.253 _refine_diff_density_min -1.566 _refine_diff_density_rms 0.244 _shelxl_version_number 2013-4 _shelx_res_file ; TITL P21onm in P2(1)/m CELL 0.71073 8.7611 16.0176 16.1289 90.000 95.282 90.000 ZERR 4.00 0.0023 0.0042 0.0042 0.000 0.004 0.000 LATT 1 SYMM - X, 1/2 + Y, - Z SFAC C H N O S U UNIT 64 72 24 12 16 4 MERG 2 EQIV $1 x, -y+1/2, z HTAB C7 N6_$1 EQIV $2 -x+1, -y, -z+1 HTAB C8 S4_$2 EQIV $3 -x+1, y-1/2, -z+1 HTAB C10 S6_$3 EQIV $4 -x+2, y-1/2, -z+1 HTAB C14 S5_$4 EQIV $5 x, y, z+1 HTAB C16 N2_$5 HTAB C17 S6_$5 EQIV $6 x, y-1, z HTAB N7 S5_$6 EQIV $7 -x+1, -y+1, -z+1 HTAB N8 S1_$7 HTAB N8 S6_$5 FMAP 2 PLAN 10 ACTA 50.00 HTAB 2.00000 BOND $H L.S. 1000 WGHT 0.024000 FVAR 0.05374 C1 1 0.546758 0.250000 0.049427 10.50000 0.01003 0.01713 = 0.02340 0.00000 0.00806 0.00000 C2 1 0.964550 0.250000 0.148179 10.50000 0.01659 0.00708 = 0.01303 0.00000 -0.00497 0.00000 C3 1 0.998899 0.250000 0.388446 10.50000 0.01079 0.01324 = 0.00648 0.00000 0.00685 0.00000 C4 1 0.555192 0.250000 0.483084 10.50000 0.01068 0.00772 = 0.01642 0.00000 -0.00022 0.00000 C5 1 1.037007 0.965953 0.249861 11.00000 0.01081 0.01788 = 0.01038 0.00234 0.00251 0.00071 C6 1 0.587346 0.629785 0.249708 11.00000 0.01382 0.01322 = 0.01049 -0.00019 0.00369 0.00764 C7 1 0.803567 -0.018801 0.413499 11.00000 0.02652 0.01411 = 0.01166 -0.00163 -0.00027 0.00105 AFIX 43 H7 2 0.821728 -0.043543 0.363177 11.00000 -1.20000 AFIX 0 C8 1 0.715410 -0.059498 0.465813 11.00000 0.02304 0.01668 = 0.01736 -0.00102 0.00050 0.00084 AFIX 43 H8 2 0.674065 -0.111556 0.451422 11.00000 -1.20000 AFIX 0 C9 1 0.687412 -0.021993 0.541965 11.00000 0.01130 0.01978 = 0.01436 -0.00123 0.00191 0.00446 C10 1 0.754489 0.057085 0.560538 11.00000 0.01900 0.01598 = 0.00894 0.00205 0.00172 0.00064 AFIX 43 H10 2 0.739458 0.083258 0.610610 11.00000 -1.20000 AFIX 0 C11 1 0.840299 0.094713 0.505797 11.00000 0.02841 0.01235 = 0.01924 -0.00023 -0.00034 0.00636 AFIX 43 H11 2 0.882627 0.147025 0.518000 11.00000 -1.20000 AFIX 0 C12 1 0.598215 -0.059140 0.594808 11.00000 0.00815 0.01276 = 0.00778 -0.00380 0.00174 -0.00161 AFIX 137 H12A 2 0.637545 -0.047370 0.651121 11.00000 -1.50000 H12B 2 0.598047 -0.118379 0.585760 11.00000 -1.50000 H12C 2 0.495471 -0.038151 0.585211 11.00000 -1.50000 AFIX 0 C13 1 0.676651 0.572954 0.979262 11.00000 0.01578 0.02015 = 0.01582 0.01013 0.00111 0.00260 AFIX 43 H13 2 0.640539 0.620343 0.950469 11.00000 -1.20000 AFIX 0 C14 1 0.766334 0.518287 0.942266 11.00000 0.01638 0.01574 = 0.01380 -0.00100 0.00362 -0.00315 AFIX 43 H14 2 0.790597 0.528004 0.888167 11.00000 -1.20000 AFIX 0 C15 1 0.823956 0.445681 0.985931 11.00000 0.01190 0.01227 = 0.01511 -0.00521 0.00055 -0.00367 C16 1 0.781825 0.435353 1.067645 11.00000 0.02300 0.01519 = 0.01382 0.00395 -0.00183 0.00282 AFIX 43 H16 2 0.817131 0.389316 1.098902 11.00000 -1.20000 AFIX 0 C17 1 0.689972 0.492252 1.100975 11.00000 0.02496 0.01903 = 0.01642 0.00249 0.00546 0.00155 AFIX 43 H17 2 0.661977 0.484539 1.154682 11.00000 -1.20000 AFIX 0 C18 1 0.913213 0.390974 0.951638 11.00000 0.00416 0.00486 = 0.00883 -0.00096 0.00425 0.00060 AFIX 137 H18A 2 0.970464 0.418963 0.911944 11.00000 -1.50000 H18B 2 0.850951 0.348167 0.924002 11.00000 -1.50000 H18C 2 0.982721 0.366259 0.994188 11.00000 -1.50000 AFIX 0 N1 3 0.537094 0.250000 0.122439 10.50000 0.01434 0.01876 = 0.01479 0.00000 0.00258 0.00000 N2 3 0.857794 0.250000 0.185693 10.50000 0.01235 0.01824 = 0.01212 0.00000 0.00631 0.00000 N3 3 0.872027 0.250000 0.360496 10.50000 0.01929 0.03372 = 0.01482 0.00000 0.00454 0.00000 N4 3 0.557230 0.250000 0.409556 10.50000 0.01253 0.02838 = 0.01235 0.00000 0.00063 0.00000 N5 3 1.021538 0.894234 0.239594 11.00000 0.01346 0.01214 = 0.02218 -0.00358 0.00331 -0.00122 N6 3 0.708063 0.660692 0.258761 11.00000 0.01211 0.01558 = 0.01721 0.00283 0.00584 -0.00116 N7 3 0.864907 0.056355 0.433009 11.00000 0.03079 0.01860 = 0.01711 0.00303 0.00640 -0.00556 AFIX 43 H7A 2 0.920579 0.080562 0.398936 11.00000 -1.20000 AFIX 0 N8 3 0.639086 0.559808 1.056808 11.00000 0.01782 0.01696 = 0.02009 -0.00341 0.00375 0.00798 AFIX 43 H8A 2 0.581227 0.595230 1.078940 11.00000 -1.20000 AFIX 0 O1 4 0.636872 0.139799 0.269240 11.00000 0.01566 0.01628 = 0.01854 0.00387 0.00266 0.00078 O2 4 0.973766 0.750000 0.356398 10.50000 0.01763 0.02334 = 0.01249 0.00000 0.00501 0.00000 O3 4 0.893833 0.750000 0.138643 10.50000 0.01451 0.01466 = 0.01589 0.00000 0.00292 0.00000 OW1 4 0.352190 0.250000 0.261013 10.50000 0.01437 0.04127 = 0.01477 0.00000 -0.00046 0.00000 OW2 4 1.208552 0.750000 0.227164 10.50000 0.01626 0.01462 = 0.01772 0.00000 0.00690 0.00000 S1 5 0.555490 0.250000 -0.049474 10.50000 0.03078 0.01754 = 0.01301 0.00000 0.00677 0.00000 S2 5 1.109889 0.250000 0.091118 10.50000 0.01320 0.01576 = 0.01391 0.00000 0.00557 0.00000 S3 5 1.174869 0.250000 0.429775 10.50000 0.01053 0.03742 = 0.01955 0.00000 -0.00168 0.00000 S4 5 0.542586 0.250000 0.581462 10.50000 0.02535 0.01912 = 0.01052 0.00000 0.00276 0.00000 S5 5 1.060693 1.065758 0.262630 11.00000 0.02788 0.01066 = 0.01609 -0.00064 0.00511 -0.00060 S6 5 0.421673 0.582621 0.234385 11.00000 0.01140 0.01485 = 0.01735 -0.00161 0.00259 -0.00262 U1 6 0.636929 0.250000 0.269208 10.50000 0.00873 0.01165 = 0.00880 0.00000 0.00113 0.00000 U2 6 0.931562 0.750000 0.247513 10.50000 0.00882 0.00958 = 0.00978 0.00000 0.00231 0.00000 HKLF 4 REM P21onm in P2(1)/m REM R1 = 0.0418 for 5115 Fo > 4sig(Fo) and 0.0591 for all 6584 data REM 300 parameters refined using 0 restraints END WGHT 0.0243 0.0000 REM Instructions for potential hydrogen bonds HTAB C7 N6_$1 HTAB C8 S4_$2 HTAB C10 S6_$3 HTAB C14 S5_$4 HTAB C16 N2_$5 HTAB C17 S6_$5 HTAB N7 S5_$6 HTAB N8 S1_$7 HTAB N8 S6_$5 REM Highest difference peak 1.253, deepest hole -1.566, 1-sigma level 0.244 Q1 1 0.9254 0.7500 0.1826 10.50000 0.05 1.25 Q2 1 0.9038 0.3574 0.9641 11.00000 0.05 1.22 Q3 1 1.1765 0.7500 0.2633 10.50000 0.05 1.21 Q4 1 0.9415 0.7500 0.3131 10.50000 0.05 1.16 Q5 1 0.2721 0.2500 0.2163 10.50000 0.05 1.11 Q6 1 0.9369 0.4137 0.9670 11.00000 0.05 1.10 Q7 1 0.5777 -0.0331 0.6294 11.00000 0.05 1.08 Q8 1 0.8847 0.4073 0.9158 11.00000 0.05 1.08 Q9 1 0.9581 0.3997 0.9579 11.00000 0.05 1.04 Q10 1 1.0914 0.2500 0.1575 10.50000 0.05 1.01 ; _shelx_res_checksum 23910 _shelx_hkl_file ; 1 0 0 6.60 0.69 1 0 0 6.00 0.69 -1 0 0 5.54 0.70 -1 0 0 6.48 0.65 2 0 0 43.49 3.59 -2 0 0 35.19 3.59 -2 0 0 34.30 3.51 2 0 0 31.43 3.50 -3 0 0 77.80 7.75 3 0 0 80.62 7.76 -3 0 0 76.83 7.84 3 0 0 83.14 7.72 4 0 0 100.75 9.64 -4 0 0 104.54 9.67 -4 0 0 88.41 9.77 -5 0 0 1.30 0.62 5 0 0 1.26 0.63 -5 0 0 0.63 0.28 6 0 0 15.70 2.21 -6 0 0 14.64 2.23 -6 0 0 13.97 1.61 7 0 0 72.64 7.11 -7 0 0 62.92 7.20 -8 0 0 13.47 2.36 8 0 0 11.19 2.01 -9 0 0 6.97 1.83 9 0 0 5.11 1.48 10 0 0 22.55 3.47 -10 0 0 21.82 3.58 -11 0 0 6.79 2.05 11 0 0 10.47 2.30 12 0 0 1.51 1.32 0 -1 0 -0.30 0.04 0 -1 0 -0.21 0.06 0 1 0 -0.34 0.03 0 1 0 -0.18 0.09 1 -1 0 10.66 1.17 -1 -1 0 10.87 1.21 -1 -1 0 12.50 1.24 1 -1 0 10.70 1.21 1 -1 0 10.79 1.22 -1 1 0 9.42 1.22 -1 1 0 12.32 1.17 1 1 0 12.28 1.18 1 1 0 14.30 1.19 -2 -1 0 236.12 22.52 2 -1 0 235.58 22.44 2 -1 0 206.77 21.99 2 -1 0 257.14 22.15 2 -1 0 231.96 22.44 -2 -1 0 225.15 22.35 2 1 0 204.91 22.08 -2 1 0 269.55 22.39 3 -1 0 0.43 0.17 3 -1 0 0.47 0.36 -3 -1 0 0.39 0.32 -3 -1 0 0.46 0.23 3 -1 0 0.64 0.35 -3 1 0 0.88 0.39 3 1 0 0.30 0.26 3 1 0 0.93 0.34 4 -1 0 96.40 10.21 4 -1 0 110.72 10.16 -4 -1 0 112.22 10.39 -4 -1 0 113.48 10.25 4 -1 0 94.40 10.14 4 1 0 88.59 10.08 -4 1 0 111.71 10.37 5 -1 0 56.45 5.51 -5 -1 0 58.04 5.60 5 -1 0 53.97 5.71 -5 -1 0 49.98 5.80 5 1 0 55.93 5.67 -5 1 0 57.96 5.85 -6 -1 0 0.12 0.49 -6 -1 0 0.47 0.31 6 -1 0 -0.38 0.50 6 -1 0 0.54 0.28 -6 1 0 0.78 0.58 6 1 0 1.06 0.56 -7 -1 0 1.82 0.92 7 -1 0 0.96 0.70 7 1 0 1.50 0.75 -7 1 0 1.47 0.79 -8 -1 0 4.99 1.41 8 -1 0 3.00 1.10 8 1 0 2.87 1.03 -8 1 0 3.24 1.20 9 -1 0 68.26 7.24 -9 -1 0 60.72 7.30 -9 1 0 66.25 7.40 9 1 0 68.85 7.19 10 -1 0 1.87 1.23 -10 -1 0 0.90 1.05 10 1 0 3.07 1.32 -10 1 0 1.37 1.26 -11 -1 0 4.54 1.88 11 -1 0 8.83 2.19 -11 1 0 10.67 2.51 11 1 0 7.43 1.96 12 1 0 27.04 4.13 0 -2 0 206.59 20.85 0 -2 0 219.07 20.26 0 -2 0 240.53 20.25 0 -2 0 217.54 20.36 0 2 0 186.00 20.64 1 -2 0 0.06 0.12 1 -2 0 0.30 0.20 -1 -2 0 0.36 0.21 1 -2 0 0.01 0.17 -1 -2 0 0.28 0.20 -1 2 0 -0.13 0.18 1 2 0 0.08 0.10 1 2 0 0.09 0.09 -2 -2 0 101.59 10.66 2 -2 0 108.19 10.50 -2 -2 0 108.03 10.73 2 -2 0 100.68 10.63 2 -2 0 105.91 10.56 2 2 0 127.39 10.51 2 2 0 91.80 10.41 -2 2 0 122.80 10.63 -2 2 0 124.36 10.71 -3 -2 0 11.39 1.55 3 -2 0 12.38 1.23 3 -2 0 13.20 1.24 3 -2 0 11.94 1.52 -3 -2 0 12.32 1.38 3 -2 0 11.38 1.54 3 2 0 10.39 1.42 -3 2 0 8.65 1.50 4 -2 0 61.65 6.09 4 -2 0 60.98 6.26 4 -2 0 64.30 6.32 -4 -2 0 53.94 6.32 -4 -2 0 56.66 6.24 4 2 0 75.00 6.24 -4 2 0 71.05 6.45 -5 -2 0 4.49 1.04 -5 -2 0 4.97 0.84 5 -2 0 5.13 0.61 5 -2 0 4.21 1.05 5 2 0 2.90 0.81 -5 2 0 5.97 1.18 6 -2 0 0.95 0.69 -6 -2 0 1.98 0.77 -6 -2 0 1.23 0.46 -6 2 0 1.41 0.70 6 2 0 0.95 0.59 -7 -2 0 61.07 6.61 -7 -2 0 73.25 7.05 7 -2 0 61.02 6.84 7 2 0 75.82 6.84 -7 2 0 58.77 6.91 -8 -2 0 0.06 0.72 8 -2 0 0.38 0.84 -8 2 0 -0.48 0.57 8 2 0 1.54 0.76 -9 -2 0 4.14 1.36 9 -2 0 3.93 1.25 9 2 0 4.42 1.35 -9 2 0 2.31 1.16 -10 -2 0 17.60 3.36 10 -2 0 21.73 3.35 -10 2 0 22.14 3.58 10 2 0 19.74 3.14 -11 -2 0 36.26 5.32 11 -2 0 42.88 5.56 11 2 0 40.74 5.09 -11 2 0 31.52 5.04 12 2 0 -0.18 1.20 0 -3 0 -0.70 0.27 0 -3 0 -0.94 0.14 0 -3 0 -0.80 0.14 0 3 0 -0.80 0.31 1 -3 0 2.24 0.42 1 -3 0 1.95 0.43 1 -3 0 2.12 0.41 -1 -3 0 2.16 0.47 1 3 0 2.19 0.28 1 3 0 2.17 0.28 -1 3 0 2.41 0.51 1 3 0 2.13 0.54 2 -3 0 388.84 38.44 2 -3 0 436.52 39.35 -2 -3 0 429.57 39.48 -2 -3 0 385.96 39.07 2 -3 0 429.19 38.69 2 3 0 414.45 38.35 -2 3 0 368.18 39.06 -3 -3 0 4.86 0.83 3 -3 0 4.99 0.91 3 -3 0 4.97 0.92 -3 -3 0 5.61 0.97 3 -3 0 5.12 0.63 -3 3 0 4.97 0.94 3 3 0 4.46 0.73 -4 -3 0 16.56 2.06 4 -3 0 21.66 2.50 -4 -3 0 16.00 2.28 4 -3 0 19.57 1.86 -4 3 0 20.58 2.27 4 3 0 15.82 2.13 5 -3 0 48.33 5.09 -5 -3 0 49.78 5.19 -5 -3 0 46.70 4.99 -5 3 0 55.61 5.26 5 3 0 45.31 4.93 -6 -3 0 0.76 0.43 6 -3 0 0.74 0.62 -6 -3 0 0.54 0.61 -6 3 0 0.95 0.71 6 3 0 0.05 0.41 -7 -3 0 0.47 0.43 7 -3 0 0.07 0.67 -7 -3 0 -0.42 0.45 -7 3 0 -0.18 0.60 7 3 0 1.11 0.65 -8 -3 0 6.07 1.62 8 -3 0 8.29 1.74 -8 3 0 4.45 1.46 8 3 0 7.13 1.52 9 -3 0 50.65 6.63 -9 -3 0 58.15 6.46 9 3 0 54.23 6.13 -9 3 0 61.07 6.52 -10 -3 0 -1.12 0.67 10 -3 0 -0.01 0.97 -10 3 0 -1.33 0.78 10 3 0 -0.14 0.90 11 -3 0 9.71 2.58 -11 -3 0 12.53 2.76 -11 3 0 10.39 2.65 11 3 0 12.57 2.47 0 -4 0 721.52 68.16 0 4 0 732.42 69.40 1 -4 0 6.90 0.95 -1 -4 0 8.19 1.10 1 -4 0 8.61 0.96 1 -4 0 7.75 1.00 -1 4 0 7.16 1.13 1 4 0 6.65 1.07 2 -4 0 14.06 1.69 2 -4 0 15.68 1.51 -2 -4 0 12.34 1.59 2 -4 0 12.62 1.57 -2 4 0 13.36 1.80 2 4 0 13.99 1.41 2 4 0 12.83 1.76 3 -4 0 10.02 1.40 -3 -4 0 11.72 1.56 3 -4 0 8.08 1.36 3 -4 0 9.52 1.08 -3 -4 0 12.27 1.44 3 4 0 9.78 1.14 -3 4 0 9.35 1.47 4 -4 0 30.49 3.11 4 -4 0 31.44 3.42 -4 -4 0 27.71 3.34 -4 -4 0 33.87 3.51 4 4 0 34.12 3.25 -4 4 0 33.75 3.51 -5 -4 0 1.81 0.73 -5 -4 0 2.38 0.70 5 -4 0 2.28 0.78 5 4 0 4.74 0.86 -5 4 0 3.96 0.97 -6 -4 0 0.55 0.44 6 -4 0 -0.20 0.56 -6 -4 0 0.62 0.63 6 4 0 0.80 0.48 -6 4 0 0.77 0.60 7 -4 0 82.01 8.31 -7 -4 0 76.14 8.10 -7 -4 0 82.70 8.44 7 4 0 69.93 7.98 -7 4 0 95.24 8.52 -8 -4 0 1.10 0.94 8 -4 0 1.64 0.92 -8 4 0 1.36 0.90 8 4 0 3.72 1.05 9 -4 0 1.72 1.09 -9 -4 0 3.75 1.39 -9 4 0 3.47 1.39 9 4 0 2.74 1.15 -10 -4 0 20.29 3.49 10 -4 0 19.58 3.33 10 4 0 21.76 3.12 -10 4 0 17.87 3.22 11 -4 0 16.18 3.16 -11 -4 0 15.02 3.19 -11 4 0 17.24 3.29 0 -5 0 -0.42 0.16 0 -5 0 -0.23 0.30 0 5 0 -0.65 0.31 1 -5 0 2.78 0.56 -1 -5 0 2.79 0.64 1 -5 0 2.62 0.51 1 5 0 2.02 0.59 -1 5 0 3.11 0.70 2 -5 0 188.66 17.74 2 -5 0 202.93 17.39 -2 -5 0 178.58 17.86 2 -5 0 163.57 17.42 2 5 0 189.57 17.75 2 5 0 189.37 17.16 -2 5 0 160.91 17.68 3 -5 0 12.89 1.40 -3 -5 0 12.50 1.71 3 -5 0 12.81 1.72 -3 5 0 14.11 1.88 3 5 0 11.96 1.35 -4 -5 0 128.47 13.17 -4 -5 0 127.23 13.18 4 -5 0 133.64 12.95 4 -5 0 133.41 12.93 4 5 0 145.39 12.74 -4 5 0 126.44 13.15 -5 -5 0 37.10 4.01 -5 -5 0 42.11 3.91 5 -5 0 40.43 3.99 -5 5 0 35.30 4.00 5 5 0 27.67 3.59 -6 -5 0 3.36 0.87 6 -5 0 2.83 1.02 -6 -5 0 3.81 1.12 6 5 0 2.42 0.78 -6 5 0 4.44 1.22 -7 -5 0 0.31 0.51 7 -5 0 1.33 0.81 -7 -5 0 0.00 0.66 7 5 0 -0.31 0.47 -7 5 0 0.16 0.64 8 -5 0 0.79 0.87 -8 -5 0 1.57 1.00 -8 5 0 -0.69 0.76 8 5 0 0.45 0.63 9 -5 0 51.07 6.12 -9 -5 0 52.23 5.84 9 5 0 42.52 5.27 -9 5 0 51.40 6.26 10 -5 0 4.03 1.78 -10 -5 0 3.60 1.51 -10 5 0 4.47 1.66 11 -5 0 7.50 2.30 -11 -5 0 5.63 2.17 -11 5 0 11.52 2.62 0 -6 0 909.35 87.95 0 -6 0 1000.00 85.47 0 6 0 814.42 87.04 1 -6 0 10.48 1.27 -1 -6 0 8.32 1.39 1 -6 0 11.88 1.44 -1 6 0 8.29 1.48 1 6 0 12.54 1.67 -2 -6 0 88.98 10.45 2 -6 0 105.66 10.15 2 -6 0 107.28 10.37 2 6 0 111.03 10.48 -2 6 0 115.68 10.48 -3 -6 0 12.09 1.74 3 -6 0 10.67 1.35 3 -6 0 13.16 1.71 3 6 0 14.34 1.92 -3 6 0 15.59 1.96 3 6 0 10.90 1.25 4 -6 0 78.81 7.44 4 -6 0 79.39 7.60 -4 -6 0 70.17 7.68 -4 6 0 63.48 7.65 4 6 0 80.70 7.33 -5 -6 0 0.64 0.58 5 -6 0 1.09 0.60 5 -6 0 1.00 0.28 -5 -6 0 1.84 0.67 -5 6 0 0.76 0.68 5 6 0 1.48 0.50 -6 -6 0 16.20 2.23 -6 -6 0 14.20 2.32 6 -6 0 19.98 2.53 -6 6 0 13.67 2.35 6 6 0 12.36 1.90 -7 -6 0 51.49 5.89 -7 -6 0 55.51 5.68 7 -6 0 48.72 5.76 7 6 0 53.73 5.50 -7 6 0 51.95 5.88 8 -6 0 6.18 1.59 -8 -6 0 7.26 1.74 8 6 0 4.96 1.26 -8 6 0 5.10 1.61 -9 -6 0 4.80 1.76 9 -6 0 3.76 1.44 -9 6 0 3.37 1.33 10 -6 0 17.84 3.50 -10 -6 0 25.52 4.02 -10 6 0 26.26 3.99 11 -6 0 12.73 2.89 -11 -6 0 18.99 3.49 -11 6 0 13.46 2.88 0 -7 0 -0.15 0.31 0 -7 0 -0.21 0.17 0 7 0 0.01 0.43 1 -7 0 33.73 2.88 1 -7 0 26.71 3.01 -1 -7 0 23.07 3.02 1 7 0 29.76 3.16 -1 7 0 24.27 3.10 2 -7 0 196.26 19.70 2 -7 0 194.90 19.22 -2 -7 0 188.24 19.83 -2 7 0 216.87 19.74 2 7 0 218.55 19.74 3 -7 0 0.49 0.33 3 -7 0 0.67 0.47 -3 -7 0 -0.47 0.36 3 7 0 0.57 0.19 3 7 0 -0.26 0.37 -3 7 0 0.12 0.48 -4 -7 0 43.05 4.42 4 -7 0 41.57 4.33 4 -7 0 40.60 4.11 4 7 0 34.00 3.96 4 7 0 58.77 4.73 -4 7 0 38.04 4.43 -5 -7 0 32.77 3.71 5 -7 0 34.40 3.33 5 -7 0 31.87 3.70 5 7 0 29.95 3.36 -5 7 0 33.64 3.85 -6 -7 0 0.09 0.52 6 -7 0 0.83 0.85 -6 -7 0 0.07 0.67 -6 7 0 0.47 0.69 6 7 0 0.07 0.42 -7 -7 0 1.52 1.01 -7 -7 0 1.31 0.69 7 -7 0 0.25 0.81 -7 7 0 -0.51 0.51 7 7 0 0.35 0.46 -8 -7 0 0.27 0.89 -8 -7 0 2.54 0.94 8 -7 0 3.13 1.25 -8 7 0 0.75 0.86 -9 -7 0 38.63 5.21 9 -7 0 34.15 4.80 -9 7 0 33.65 4.87 10 -7 0 1.76 1.36 -10 -7 0 -0.32 1.01 -10 7 0 -0.56 0.95 11 -7 0 7.46 2.34 -11 -7 0 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20.89 3.55 8 12 3 25.92 4.17 -8 12 -3 22.12 3.96 9 -12 3 2.07 1.44 9 12 3 1.97 1.50 -9 12 -3 1.58 1.37 9 -13 -3 6.94 2.05 -9 -13 3 1.64 1.28 -9 13 3 0.92 1.45 9 13 -3 3.74 1.80 8 -13 -3 58.56 6.89 -8 -13 3 62.79 6.98 -8 13 3 63.29 7.83 8 13 -3 55.07 7.46 7 -13 -3 2.66 1.34 -7 -13 3 3.50 1.42 7 13 -3 4.22 1.70 -7 13 3 3.14 1.61 -6 -13 3 15.37 2.77 6 -13 -3 17.98 2.86 -6 13 3 17.26 3.09 6 13 -3 18.24 3.13 -5 -13 3 40.85 4.65 5 -13 -3 29.38 3.87 -5 13 3 23.05 4.05 5 13 -3 31.32 4.33 4 -13 -3 20.49 3.06 -4 -13 3 27.21 3.67 4 -13 -3 25.37 3.18 -4 13 3 20.12 3.50 4 13 -3 25.36 3.69 -3 -13 3 2.60 1.02 3 -13 -3 0.24 0.64 3 -13 -3 1.58 0.69 3 -13 -3 2.61 0.88 3 13 -3 1.52 1.09 -3 13 3 2.61 1.17 -2 -13 3 6.64 1.43 2 -13 -3 2.88 1.10 2 -13 -3 1.09 0.72 2 -13 -3 2.45 0.76 -2 13 3 2.67 1.14 2 13 -3 5.38 1.42 -1 -13 3 98.75 10.50 1 -13 -3 107.62 10.60 -1 13 3 88.42 10.47 1 13 -3 113.20 10.72 0 -13 -3 12.37 2.20 0 -13 3 8.14 1.77 0 13 3 11.11 2.11 0 13 -3 13.58 2.42 -1 -13 -3 60.85 6.82 1 -13 3 64.75 6.64 -1 13 -3 61.26 6.83 1 13 3 59.22 6.79 2 -13 3 20.23 2.80 -2 -13 -3 18.01 3.14 2 -13 3 24.37 3.07 -2 13 -3 24.84 3.50 2 13 3 27.72 3.55 -3 -13 -3 4.25 1.40 3 -13 3 9.06 1.52 3 -13 3 8.10 1.47 -3 13 -3 5.08 1.52 3 13 3 8.30 1.78 4 -13 3 2.83 1.01 -4 -13 -3 3.49 1.36 -4 13 -3 4.77 1.59 4 13 3 2.93 1.22 5 -13 3 6.78 1.56 -5 -13 -3 6.27 1.73 -5 13 -3 6.42 1.78 5 13 3 8.76 2.06 -6 -13 -3 30.55 4.37 6 -13 3 32.29 4.23 -6 13 -3 26.76 4.44 6 13 3 34.19 4.89 7 -13 3 0.33 1.03 -7 -13 -3 -1.01 0.80 7 13 3 0.48 1.05 -7 13 -3 0.36 1.09 -8 -13 -3 18.83 3.26 8 -13 3 21.99 3.44 8 13 3 24.87 4.16 -8 13 -3 12.78 3.20 9 -13 3 10.94 2.54 -9 13 -3 12.18 2.87 9 13 3 9.21 2.80 9 -14 -3 -1.53 1.10 -9 -14 3 0.31 1.09 9 14 -3 -1.51 0.97 -9 14 3 0.44 1.26 -8 -14 3 4.47 1.69 8 -14 -3 6.07 1.88 -8 14 3 5.89 2.03 8 14 -3 4.73 1.90 7 -14 -3 -0.08 1.13 -7 -14 3 2.29 1.31 -7 14 3 -0.19 0.88 7 14 -3 -0.41 1.02 6 -14 -3 13.66 2.47 -6 -14 3 13.96 2.69 6 14 -3 12.32 2.68 -6 14 3 14.40 2.78 -5 -14 3 5.22 1.53 5 -14 -3 3.86 1.31 -5 14 3 2.98 1.47 5 14 -3 3.31 1.37 4 -14 -3 20.17 2.88 4 -14 -3 18.37 2.68 -4 -14 3 15.55 2.87 4 14 -3 15.86 3.01 -4 14 3 28.84 3.75 -3 -14 3 80.02 9.27 3 -14 -3 91.28 9.22 -3 14 3 90.69 9.37 2 -14 -3 0.53 0.74 -2 -14 3 0.43 0.75 -2 14 3 0.34 0.75 2 14 -3 -0.52 0.66 1 -14 -3 25.23 3.43 -1 -14 3 24.09 3.33 -1 14 3 17.27 3.20 1 14 -3 24.98 3.63 0 -14 -3 0.16 0.80 0 -14 3 0.87 0.71 0 14 -3 1.25 1.02 0 14 3 1.37 0.97 -1 -14 -3 70.66 8.26 1 -14 3 80.49 8.12 -1 14 -3 83.31 8.41 1 14 3 71.68 8.26 2 -14 3 0.68 0.64 -2 -14 -3 0.55 0.93 2 14 3 0.16 0.88 -2 14 -3 -0.67 0.70 3 -14 3 45.29 5.41 3 -14 3 53.80 5.43 -3 -14 -3 51.81 5.87 -3 14 -3 51.22 6.37 3 14 3 48.25 5.77 4 -14 3 36.34 3.90 -4 -14 -3 33.50 4.57 4 14 3 30.30 4.48 -4 14 -3 26.36 4.36 5 -14 3 -0.63 0.62 -5 -14 -3 1.05 1.00 -5 14 -3 0.77 0.94 5 14 3 0.17 0.90 6 -14 3 12.55 2.42 -6 -14 -3 12.80 2.74 6 14 3 17.01 3.14 -6 14 -3 13.17 2.79 7 -14 3 1.22 1.09 -7 -14 -3 -0.65 0.91 7 14 3 -0.34 1.02 -7 14 -3 0.52 1.11 -8 -14 -3 18.80 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55.41 6.21 -4 -5 -4 59.64 6.34 -4 -5 -4 62.76 6.40 -4 5 -4 61.68 6.39 -4 5 -4 62.64 5.96 5 -5 4 67.00 6.51 -5 -5 -4 59.90 6.55 -5 -5 -4 63.67 6.46 5 5 4 56.55 6.21 -5 5 -4 64.31 6.61 -6 -5 -4 4.08 1.01 6 -5 4 6.12 1.38 -6 -5 -4 5.75 1.38 6 5 4 4.45 1.04 -6 5 -4 4.25 1.26 7 -5 4 0.43 0.74 -7 -5 -4 0.30 0.73 -7 -5 -4 0.35 0.61 -7 5 -4 1.41 0.80 7 5 4 0.66 0.63 -8 -5 -4 0.90 0.88 8 -5 4 1.73 0.99 8 5 4 0.91 0.76 -8 5 -4 1.45 0.91 9 -5 4 11.14 2.33 -9 -5 -4 12.28 2.57 9 5 4 11.86 2.17 -9 5 -4 15.28 2.82 -10 -5 -4 4.87 1.83 10 -5 4 4.30 1.64 -10 5 -4 7.32 1.95 -11 -5 -4 4.46 1.93 11 -5 4 5.43 1.81 -11 5 -4 5.29 1.94 -11 -6 4 2.83 1.55 11 -6 -4 4.56 1.99 -11 6 4 5.22 1.94 -10 -6 4 6.69 2.14 10 -6 -4 7.04 2.15 -10 6 4 10.59 2.26 9 -6 -4 37.45 5.07 -9 -6 4 33.93 4.80 -9 6 4 36.78 4.83 -8 -6 4 8.47 1.88 8 -6 -4 6.73 1.80 8 -6 -4 7.67 1.74 -8 -6 4 6.88 1.55 -8 6 4 9.88 1.99 8 6 -4 8.36 1.65 8 6 -4 9.03 1.63 -7 -6 4 76.68 8.17 7 -6 -4 73.71 8.25 -7 -6 4 83.13 8.36 7 -6 -4 76.65 8.30 -7 6 4 76.25 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4.48 3 -8 4 38.04 4.04 -3 8 -4 32.03 4.30 3 8 4 42.18 3.94 3 8 4 43.19 4.45 4 -8 4 23.03 2.82 -4 -8 -4 20.13 2.80 4 -8 4 19.62 2.13 -4 8 -4 21.18 2.90 4 8 4 16.24 2.67 4 8 4 18.95 2.15 -5 -8 -4 6.17 1.37 5 -8 4 4.29 1.17 -5 8 -4 4.27 1.25 5 8 4 6.73 1.50 5 8 4 5.41 0.98 -6 -8 -4 -0.40 0.56 6 -8 4 -0.04 0.77 -6 8 -4 0.42 0.81 7 -8 4 42.89 5.31 -7 -8 -4 51.00 5.17 -7 -8 -4 38.37 4.67 -7 8 -4 35.19 5.08 8 -8 4 0.67 0.95 -8 -8 -4 0.82 1.05 -8 8 -4 -0.29 0.90 9 -8 4 0.88 1.18 -9 -8 -4 1.47 1.18 -9 8 -4 -0.33 0.89 10 -8 4 21.70 3.71 -10 -8 -4 29.87 4.55 -10 8 -4 23.00 3.94 -11 9 4 27.83 4.56 11 9 -4 28.15 4.55 10 -9 -4 1.54 1.37 -10 9 4 0.25 1.11 10 9 -4 1.77 1.32 -9 -9 4 45.51 5.52 9 -9 -4 55.20 6.42 -9 9 4 58.50 6.56 9 9 -4 38.36 5.85 -8 -9 4 0.45 0.76 8 -9 -4 -1.56 0.94 8 -9 -4 1.28 1.04 -8 9 4 0.81 1.14 8 9 -4 0.47 1.07 7 -9 -4 22.62 3.51 7 -9 -4 19.70 3.24 -7 -9 4 25.28 3.43 -7 9 4 22.71 3.50 7 9 -4 27.85 3.69 6 -9 -4 8.30 1.80 6 -9 -4 6.20 1.56 -6 -9 4 12.04 1.95 -6 9 4 7.75 1.75 6 9 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11.82 1.60 1 -7 5 34.46 3.26 1 -7 5 24.96 3.12 -1 -7 -5 31.66 3.53 -1 7 -5 29.29 3.32 1 7 5 37.31 3.40 1 7 5 25.46 3.06 2 -7 5 88.24 8.52 -2 -7 -5 77.09 8.86 2 -7 5 88.44 8.59 2 7 5 97.98 8.40 -2 7 -5 84.30 8.73 2 7 5 75.10 8.65 3 -7 5 9.90 1.78 -3 -7 -5 12.19 2.01 3 -7 5 14.46 1.52 3 7 5 14.03 2.07 -3 7 -5 9.60 1.85 3 7 5 13.15 1.66 -4 -7 -5 4.23 1.14 4 -7 5 3.85 1.04 -4 7 -5 3.19 0.99 4 7 5 4.28 0.84 5 -7 5 2.31 0.87 -5 -7 -5 0.70 0.68 -5 -7 -5 0.32 0.76 -5 7 -5 1.52 0.75 5 7 5 1.82 0.61 -6 -7 -5 110.69 11.12 6 -7 5 107.56 10.82 -6 -7 -5 109.80 10.98 -6 7 -5 97.98 11.01 6 7 5 107.75 10.54 -7 -7 -5 -0.12 0.55 7 -7 5 0.97 0.94 -7 -7 -5 -0.17 0.77 -7 7 -5 0.67 0.85 7 7 5 0.80 0.65 -8 -7 -5 30.85 4.65 8 -7 5 36.62 4.66 -8 7 -5 39.37 5.03 -9 -7 -5 8.33 2.09 9 -7 5 10.64 2.22 -9 7 -5 6.82 2.05 10 -7 5 12.26 2.55 -10 -7 -5 11.67 2.78 -10 7 -5 6.35 1.96 11 8 -5 5.57 1.95 -11 8 5 10.63 2.41 10 -8 -5 27.34 4.33 -10 8 5 34.39 4.61 10 8 -5 24.28 4.19 9 -8 -5 0.88 1.12 -9 -8 5 -0.54 0.68 9 -8 -5 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6.06 8 -9 -5 57.94 6.41 8 -9 -5 54.41 6.58 -8 9 5 51.09 6.20 8 9 -5 55.91 6.33 7 -9 -5 2.15 1.07 7 -9 -5 1.06 1.01 -7 -9 5 2.24 1.13 -7 9 5 2.48 1.17 7 9 -5 3.45 1.33 -6 -9 5 4.02 1.20 6 -9 -5 2.84 1.17 6 -9 -5 3.16 1.18 6 9 -5 5.14 1.49 -6 9 5 1.31 0.91 5 -9 -5 42.56 4.62 -5 -9 5 39.44 4.70 -5 9 5 45.33 4.77 5 9 -5 38.14 4.74 -4 -9 5 34.71 3.55 -4 -9 5 29.05 4.14 4 -9 -5 39.40 4.01 -4 9 5 30.36 4.17 -4 9 5 35.85 3.95 4 9 -5 32.38 4.30 -3 -9 5 0.17 0.47 3 -9 -5 0.13 0.53 -3 -9 5 0.66 0.39 -3 9 5 0.24 0.50 3 9 -5 0.66 0.60 -3 9 5 2.58 0.90 -2 -9 5 4.07 0.72 -2 -9 5 4.03 0.94 2 -9 -5 3.82 1.04 2 9 -5 1.47 0.83 -2 9 5 3.55 1.00 -2 9 5 2.66 0.80 -1 -9 5 125.44 13.76 -1 -9 5 153.49 13.32 1 -9 -5 117.45 13.86 -1 9 5 129.04 13.34 1 9 -5 140.51 13.81 -1 9 5 166.70 13.87 0 -9 5 0.40 0.45 0 -9 -5 1.18 0.64 0 -9 5 0.11 0.37 0 9 -5 -0.28 0.47 0 9 5 -0.41 0.39 0 9 5 1.05 0.44 -1 -9 -5 43.83 5.38 1 -9 5 58.34 5.11 1 -9 5 51.79 5.20 1 9 5 45.36 4.89 -1 9 -5 46.92 5.30 -2 -9 -5 89.80 9.55 2 -9 5 82.08 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2.10 1.34 0 0 21 0.42 1.35 0 0 -21 -0.84 1.06 1 0 21 1.20 1.51 -1 0 -21 0.25 1.16 -2 0 -21 31.98 5.23 2 0 21 37.05 5.86 -4 -1 21 6.59 2.26 -4 1 21 3.74 2.08 3 -1 -21 23.19 3.99 -3 -1 21 12.75 3.25 3 1 -21 24.67 3.93 -3 1 21 17.72 3.68 -2 -1 21 1.12 1.29 2 -1 -21 2.26 1.53 2 1 -21 1.01 1.28 -2 1 21 2.32 1.70 -1 -1 21 5.18 1.95 1 -1 -21 6.65 2.08 1 1 -21 6.56 1.99 -1 1 21 5.41 1.97 0 -1 21 28.88 4.53 0 -1 -21 31.00 4.73 0 1 -21 21.75 4.12 0 1 21 29.25 4.51 1 -1 21 -0.35 1.27 -1 -1 -21 -0.39 1.05 1 1 21 0.23 1.42 -1 1 -21 0.93 1.26 -2 -1 -21 -1.56 0.94 -2 1 -21 1.38 1.38 2 1 21 0.61 1.36 -4 -2 21 0.85 1.38 3 -2 -21 12.99 2.85 -3 -2 21 10.49 2.69 3 2 -21 7.79 2.40 -3 2 21 8.07 2.53 -2 -2 21 24.18 3.83 2 -2 -21 17.73 3.31 2 2 -21 14.35 3.00 -2 2 21 7.90 2.59 1 -2 -21 5.89 2.10 -1 -2 21 8.00 2.47 1 2 -21 10.91 2.41 -1 2 21 3.47 1.91 0 -2 21 2.41 1.52 0 -2 -21 2.15 1.48 0 2 21 1.66 1.52 0 2 -21 -0.38 0.91 1 -2 21 4.12 1.90 -1 -2 -21 6.47 2.22 1 2 21 4.59 1.97 -1 2 -21 6.99 1.95 -2 -2 -21 41.04 5.47 2 2 21 22.90 4.75 -4 -3 21 0.90 1.50 3 -3 -21 35.99 5.34 -3 -3 21 38.08 5.43 -3 3 21 31.23 5.05 3 3 -21 33.45 5.11 -2 -3 21 0.34 1.27 2 -3 -21 -0.63 1.17 2 3 -21 -0.36 1.03 -2 3 21 5.40 2.11 -1 -3 21 13.72 2.96 1 -3 -21 16.52 3.27 -1 3 21 11.03 2.72 1 3 -21 10.38 2.59 0 -3 21 21.05 3.77 0 -3 -21 22.29 4.01 0 3 21 16.75 3.40 0 3 -21 20.43 3.57 -1 -3 -21 3.99 1.85 1 -3 21 2.81 1.80 -1 3 -21 4.15 1.72 1 3 21 2.89 1.67 -2 -3 -21 2.40 1.58 2 3 21 -0.19 1.13 -4 -4 21 -0.24 1.34 3 -4 -21 15.99 3.63 -3 -4 21 6.70 2.27 -3 4 21 7.73 2.48 3 4 -21 12.13 2.76 -2 -4 21 11.91 2.93 2 -4 -21 16.35 3.35 2 4 -21 12.51 2.80 -2 4 21 11.58 2.79 -1 -4 21 8.22 2.43 1 -4 -21 4.86 2.10 1 4 -21 6.47 1.99 -1 4 21 8.98 2.35 0 -4 21 0.79 1.31 0 -4 -21 -1.26 0.91 0 4 21 -0.79 1.12 0 4 -21 0.57 1.05 -1 -4 -21 2.11 1.51 1 -4 21 4.06 1.76 1 4 21 -0.13 1.35 -1 4 -21 0.80 1.12 -2 -4 -21 17.19 3.65 2 4 21 19.58 4.02 -3 -4 -21 0.62 1.39 -3 -5 21 15.63 3.36 -2 -5 21 2.56 1.67 2 -5 -21 2.80 1.69 -2 5 21 2.10 1.60 2 5 -21 0.31 1.14 -1 -5 21 8.29 2.44 1 -5 -21 11.77 2.86 -1 5 21 6.28 2.25 1 5 -21 9.32 2.38 0 -5 -21 13.38 3.31 0 -5 21 17.86 3.36 0 5 21 16.94 3.28 0 5 -21 17.39 3.24 -1 -5 -21 0.25 1.24 -1 5 -21 -0.39 0.94 1 5 21 -0.36 1.25 -2 -5 -21 1.18 1.51 -3 -5 -21 4.93 2.35 -3 -6 21 14.24 3.16 -2 -6 21 6.02 2.09 2 6 -21 12.76 2.86 -2 6 21 5.80 2.26 -1 -6 21 4.77 1.83 1 6 -21 4.06 1.74 -1 6 21 4.15 1.90 0 -6 21 -1.20 1.12 0 6 -21 0.30 1.10 0 6 21 0.89 1.53 1 6 21 0.92 1.42 -1 6 -21 -0.27 1.06 -3 -7 21 8.08 2.58 -2 -7 21 2.00 1.49 -1 -7 21 7.33 2.42 -1 7 21 8.68 2.52 1 7 -21 16.73 3.17 0 7 -21 20.32 3.68 0 7 21 26.34 4.19 1 7 21 1.75 1.51 -2 -8 21 10.13 3.05 0 8 -21 0.11 1.17 1 0 -22 14.20 3.30 0 0 -22 1.38 1.42 -1 0 -22 19.91 3.75 -2 0 -22 2.78 1.62 1 1 -22 24.78 4.59 0 -1 -22 11.55 2.81 0 1 -22 9.10 2.49 -1 -1 -22 7.02 2.36 -1 1 -22 6.62 2.09 -2 -1 -22 -0.71 1.24 1 2 -22 6.62 2.32 0 2 -22 0.55 1.18 -1 -2 -22 17.39 4.12 -1 2 -22 26.98 4.29 -2 -2 -22 -0.32 1.38 0 3 -22 2.31 1.43 -1 3 -22 8.70 2.36 0 4 -22 2.23 1.42 -1 4 -22 23.47 4.01 -1 5 -22 3.33 1.65 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 95908 _symmetry_cell_setting monoclinic _symmetry_space_group_name_h-m 'P 21/m' _symmetry_int_tables_number 11 _chemical_absolute_configuration ? _database_code_depnum_ccdc_archive 'CCDC 967160' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound_7 _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety '(C5 H7 N2 1+)2, (U O3 C4 H2 N4 S4 2-)' _chemical_formula_sum 'C14 H16 N8 O3 S4 U' _exptl_crystal_recrystallization_method 'Slow Evaporation' _chemical_melting_point ? _exptl_crystal_description Prism _exptl_crystal_colour Yellow _diffrn_ambient_temperature 100(2) _chemical_formula_weight 710.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 11 _space_group_name_H-M_alt 'P 21/m' _space_group_name_Hall '-P 2yb' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 8.7580(7) _cell_length_b 16.0178(14) _cell_length_c 16.1291(14) _cell_angle_alpha 90 _cell_angle_beta 95.2530(10) _cell_angle_gamma 90 _cell_volume 2253.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5880 _cell_measurement_theta_min 5.072 _cell_measurement_theta_max 54.778 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.089 _exptl_crystal_F_000 1336 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.154 _exptl_crystal_size_mid 0.070 _exptl_crystal_size_min 0.060 _exptl_absorpt_coefficient_mu 7.607 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.537970 _exptl_absorpt_correction_T_max 0.745686 _exptl_absorpt_process_details 'TWINABS, G. Sheldrick (2008)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_measurement_device_type 'Bruker ApexII CCD' _diffrn_measurement_method 'Omega and Phi Scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 39748 _diffrn_reflns_av_unetI/netI 0.0470 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.268 _diffrn_reflns_theta_max 28.315 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 5798 _reflns_number_gt 4687 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Data were apparently pre-merged, so _diffrn_reflns_number etc. will have to be added later. Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'APEX II (Bruker AXS, 2013)' _computing_cell_refinement 'SAINT (Bruker AXS, 2013)' _computing_data_reduction 'SAINT (Bruker AXS, 2013)' _computing_structure_solution 'SIR92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Crystal Maker v.8.2.2 (Palmer 2009)' _computing_publication_material 'WINGX (Farrugia, 2012)' _refine_special_details ; 'The crystal selected for data' collection of compound 7 was twinned and was treated using Cell Now. The crystal consisted of two non-merohedral twin components with the majority of the collected reflections belonging to the first domain (79%). The twin components are related by 179.9 degree rotation about the 001 axis and the following transformation matrix [-1 0 0 0 -1 0 0 0 1]. The reflection data were assigned to the appropriate domains via Cell_Now, integrated using SAINT, and an absorption correction was applied using SADABS, all contained within the APEXII software suite.' ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0112P)^2^+10.5513P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 5798 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0631 _refine_ls_wR_factor_gt 0.0594 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C5 C 0.5376(5) 0.9661(3) 0.7502(3) 0.0109(9) Uani 1 1 d . . . . . C6 C 0.0883(5) 0.6292(3) 0.7501(3) 0.0120(9) Uani 1 1 d . . . . . C1 C 0.9533(8) 0.7500 1.4491(4) 0.0121(13) Uani 1 2 d S T P . . C2 C 0.5365(7) 0.7500 1.3527(4) 0.0088(12) Uani 1 2 d S T P . . C3 C 0.5004(8) 0.7500 1.1109(4) 0.0116(13) Uani 1 2 d S T P . . C4 C 0.9464(7) 0.7500 1.0165(4) 0.0131(14) Uani 1 2 d S T P . . C7 C 0.3403(6) 0.4058(3) 0.0061(3) 0.0189(10) Uani 1 1 d . . . . . H7 H 0.3839 0.3540 0.0190 0.023 Uiso 1 1 calc R U . . . C8 C 0.2527(6) 0.4433(3) 0.0603(3) 0.0165(10) Uani 1 1 d . . . . . H8 H 0.2360 0.4168 0.1100 0.020 Uiso 1 1 calc R U . . . C9 C 0.1870(5) 0.5221(3) 0.0420(3) 0.0141(10) Uani 1 1 d . . . . . C10 C 0.2166(6) 0.5593(3) -0.0343(3) 0.0191(11) Uani 1 1 d . . . . . H10 H 0.1767 0.6117 -0.0487 0.023 Uiso 1 1 calc R U . . . C11 C 0.3041(6) 0.5181(3) -0.0867(3) 0.0199(11) Uani 1 1 d . . . . . H11 H 0.3221 0.5423 -0.1372 0.024 Uiso 1 1 calc R U . . . C12 C 0.8092(6) 0.9924(3) 0.3987(3) 0.0176(10) Uani 1 1 d . . . . . H12 H 0.8349 0.9852 0.3445 0.021 Uiso 1 1 calc R U . . . C13 C 0.7197(6) 0.9351(3) 0.4325(3) 0.0174(10) Uani 1 1 d . . . . . H13 H 0.6861 0.8884 0.4019 0.021 Uiso 1 1 calc R U . . . C14 C 0.6771(5) 0.9462(3) 0.5143(3) 0.0125(9) Uani 1 1 d . . . . . C15 C 0.7333(5) 1.0176(3) 0.5575(3) 0.0133(9) Uani 1 1 d . . . . . H15 H 0.7083 1.0272 0.6115 0.016 Uiso 1 1 calc R U . . . C16 C 0.8230(5) 1.0723(3) 0.5213(3) 0.0169(10) Uani 1 1 d . . . . . H16 H 0.8590 1.1193 0.5506 0.020 Uiso 1 1 calc R U . . . N5 N 0.5214(4) 0.8943(2) 0.7394(2) 0.0141(8) Uani 1 1 d . . . . . N6 N 0.2082(5) 0.6605(3) 0.7590(3) 0.0163(9) Uani 1 1 d . . . . . N1 N 0.9622(6) 0.7500 1.3778(4) 0.0153(12) Uani 1 2 d S T P . . N2 N 0.6423(7) 0.7500 1.3144(3) 0.0130(11) Uani 1 2 d S T P . . N3 N 0.6291(7) 0.7500 1.1388(4) 0.0172(13) Uani 1 2 d S T P . . N4 N 0.9424(6) 0.7500 1.0894(3) 0.0138(12) Uani 1 2 d S T P . . N7 N 0.3646(5) 0.4432(3) -0.0665(3) 0.0192(9) Uani 1 1 d . . . . . H7A H 0.4200 0.4184 -0.1004 0.023 Uiso 1 1 calc R U . . . N8 N 0.0986(5) 0.5593(3) 0.0941(3) 0.0204(9) Uani 1 1 d . . . . . H8A H 0.0808 0.5351 0.1398 0.024 Uiso 1 1 calc R U . . . H8B H 0.0593 0.6075 0.0819 0.024 Uiso 1 1 calc R U . . . N9 N 0.8618(5) 1.0599(2) 0.4428(2) 0.0158(9) Uani 1 1 d . . . . . H9 H 0.9202 1.0952 0.4208 0.019 Uiso 1 1 calc R U . . . N10 N 0.5868(5) 0.8914(2) 0.5484(2) 0.0170(9) Uani 1 1 d . . . . . H10A H 0.5616 0.8994 0.5981 0.020 Uiso 1 1 calc R U . . . H10B H 0.5538 0.8481 0.5208 0.020 Uiso 1 1 calc R U . . . O2 O 0.4731(5) 0.7500 0.8570(3) 0.0148(10) Uani 1 2 d S T P . . O3 O 0.3928(5) 0.7500 0.6379(3) 0.0115(9) Uani 1 2 d S T P . . O1 O 0.8633(4) 0.6398(2) 1.2305(2) 0.0158(7) Uani 1 1 d . . . . . OW2 O 0.7082(5) 0.7500 0.7271(3) 0.0146(10) Uani 1 2 d S T P . . OW1 O 1.1463(5) 0.7500 1.2387(3) 0.0239(12) Uani 1 2 d S T P . . S5 S 0.56058(16) 1.06576(7) 0.76271(8) 0.0184(3) Uani 1 1 d . . . . . S6 S -0.07808(13) 0.58262(8) 0.73429(7) 0.0144(2) Uani 1 1 d . . . . . S1 S 0.9444(2) 0.7500 1.54952(11) 0.0199(4) Uani 1 2 d S T P . . S2 S 0.38950(19) 0.7500 1.40896(10) 0.0136(3) Uani 1 2 d S T P . . S3 S 0.3255(2) 0.7500 1.07023(12) 0.0214(4) Uani 1 2 d S T P . . S4 S 0.9576(2) 0.7500 0.91821(11) 0.0177(4) Uani 1 2 d S T P . . U2 U 0.43160(3) 0.7500 0.74748(2) 0.00881(6) Uani 1 2 d S T P . . U1 U 0.86303(3) 0.7500 1.23076(2) 0.00926(6) Uani 1 2 d S T P . . 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 C5 0.009(2) 0.015(2) 0.009(2) 0.0023(18) 0.0022(17) -0.0004(17) C6 0.018(2) 0.010(2) 0.009(2) 0.0004(17) 0.0059(18) 0.0023(18) C1 0.013(3) 0.013(3) 0.011(3) 0.000 0.002(3) 0.000 C2 0.010(3) 0.005(3) 0.010(3) 0.000 -0.003(2) 0.000 C3 0.015(3) 0.004(3) 0.016(3) 0.000 0.003(3) 0.000 C4 0.002(3) 0.014(3) 0.023(4) 0.000 0.001(3) 0.000 C7 0.029(3) 0.008(2) 0.019(2) 0.003(2) 0.001(2) -0.002(2) C8 0.019(3) 0.019(3) 0.012(2) -0.0020(19) 0.0003(19) -0.007(2) C9 0.013(2) 0.016(2) 0.013(2) -0.0032(19) -0.0013(18) 0.0017(19) C10 0.020(3) 0.016(3) 0.021(3) 0.004(2) -0.001(2) 0.004(2) C11 0.020(3) 0.022(3) 0.018(3) 0.004(2) 0.003(2) -0.001(2) C12 0.026(3) 0.014(2) 0.014(2) -0.0020(19) 0.009(2) 0.000(2) C13 0.026(3) 0.010(2) 0.016(2) -0.0043(19) 0.002(2) -0.004(2) C14 0.011(2) 0.010(2) 0.016(2) 0.0021(18) -0.0003(18) 0.0002(18) C15 0.014(2) 0.016(2) 0.010(2) -0.0029(18) 0.0026(18) -0.0013(19) C16 0.015(3) 0.013(2) 0.023(3) -0.004(2) 0.003(2) -0.0005(19) N5 0.012(2) 0.014(2) 0.017(2) 0.0010(16) 0.0031(16) 0.0001(16) N6 0.013(2) 0.015(2) 0.021(2) 0.0000(17) 0.0040(17) -0.0025(17) N1 0.012(3) 0.022(3) 0.013(3) 0.000 0.006(2) 0.000 N2 0.018(3) 0.010(3) 0.011(3) 0.000 0.002(2) 0.000 N3 0.018(3) 0.021(3) 0.014(3) 0.000 0.004(2) 0.000 N4 0.006(3) 0.023(3) 0.014(3) 0.000 0.004(2) 0.000 N7 0.023(2) 0.018(2) 0.018(2) -0.0012(18) 0.0094(18) 0.0045(18) N8 0.020(2) 0.024(2) 0.018(2) 0.0026(18) 0.0053(18) 0.0042(18) N9 0.019(2) 0.013(2) 0.016(2) -0.0002(17) 0.0054(17) -0.0049(17) N10 0.021(2) 0.015(2) 0.016(2) -0.0020(17) 0.0041(17) -0.0075(17) O2 0.013(2) 0.017(2) 0.014(2) 0.000 0.0021(19) 0.000 O3 0.015(2) 0.008(2) 0.012(2) 0.000 0.0047(19) 0.000 O1 0.0181(18) 0.0148(17) 0.0150(17) 0.0000(14) 0.0038(13) 0.0019(14) OW2 0.009(2) 0.013(2) 0.023(3) 0.000 0.0075(19) 0.000 OW1 0.010(2) 0.045(3) 0.016(3) 0.000 0.000(2) 0.000 S5 0.0297(7) 0.0096(6) 0.0167(6) -0.0011(5) 0.0061(5) -0.0010(5) S6 0.0117(6) 0.0147(6) 0.0171(6) -0.0013(5) 0.0031(4) -0.0021(5) S1 0.0336(11) 0.0169(9) 0.0102(8) 0.000 0.0073(7) 0.000 S2 0.0099(8) 0.0179(9) 0.0136(8) 0.000 0.0037(6) 0.000 S3 0.0078(8) 0.0377(11) 0.0181(9) 0.000 -0.0018(7) 0.000 S4 0.0239(10) 0.0190(9) 0.0105(8) 0.000 0.0036(7) 0.000 U2 0.00832(12) 0.00896(12) 0.00946(12) 0.000 0.00260(9) 0.000 U1 0.00785(12) 0.01140(12) 0.00869(12) 0.000 0.00164(9) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C5 N5 1.171(6) . ? C5 S5 1.619(5) . ? C6 N6 1.160(6) . ? C6 S6 1.636(5) . ? C1 N1 1.160(8) . ? C1 S1 1.629(6) . ? C2 N2 1.159(8) . ? C2 S2 1.642(7) . ? C3 N3 1.175(8) . ? C3 S3 1.610(7) . ? C4 N4 1.180(8) . ? C4 S4 1.597(7) . ? C7 N7 1.348(6) . ? C7 C8 1.356(7) . ? C7 H7 0.9300 . ? C8 C9 1.408(7) . ? C8 H8 0.9300 . ? C9 N8 1.334(6) . ? C9 C10 1.413(7) . ? C10 C11 1.362(7) . ? C10 H10 0.9300 . ? C11 N7 1.340(6) . ? C11 H11 0.9300 . ? C12 N9 1.352(6) . ? C12 C13 1.353(7) . ? C12 H12 0.9300 . ? C13 C14 1.414(6) . ? C13 H13 0.9300 . ? C14 N10 1.334(6) . ? C14 C15 1.406(6) . ? C15 C16 1.344(6) . ? C15 H15 0.9300 . ? C16 N9 1.356(6) . ? C16 H16 0.9300 . ? N5 U2 2.448(4) . ? N6 U2 2.446(4) . ? N1 U1 2.449(6) . ? N2 U1 2.457(6) . ? N3 U1 2.417(6) . ? N4 U1 2.443(5) . ? N7 H7A 0.8600 . ? N8 H8A 0.8600 . ? N8 H8B 0.8600 . ? N9 H9 0.8600 . ? N10 H10A 0.8600 . ? N10 H10B 0.8600 . ? O2 U2 1.770(5) . ? O3 U2 1.768(4) . ? O1 U1 1.765(3) . ? OW2 U2 2.475(4) . ? OW1 U1 2.472(5) . ? U2 N6 2.446(4) 4_575 ? U2 N5 2.448(4) 4_575 ? U1 O1 1.765(3) 4_575 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 C5 S5 178.6(4) . . ? N6 C6 S6 177.5(4) . . ? N1 C1 S1 178.9(6) . . ? N2 C2 S2 178.6(6) . . ? N3 C3 S3 178.5(6) . . ? N4 C4 S4 178.2(6) . . ? N7 C7 C8 120.5(5) . . ? N7 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C7 C8 C9 120.4(5) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? N8 C9 C8 121.2(4) . . ? N8 C9 C10 121.6(5) . . ? C8 C9 C10 117.2(4) . . ? C11 C10 C9 119.6(5) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? N7 C11 C10 121.1(5) . . ? N7 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? N9 C12 C13 120.9(4) . . ? N9 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C12 C13 C14 120.2(4) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? N10 C14 C15 121.6(4) . . ? N10 C14 C13 121.3(4) . . ? C15 C14 C13 117.0(4) . . ? C16 C15 C14 120.4(4) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 N9 121.2(4) . . ? C15 C16 H16 119.4 . . ? N9 C16 H16 119.4 . . ? C5 N5 U2 162.8(4) . . ? C6 N6 U2 164.8(4) . . ? C1 N1 U1 155.5(5) . . ? C2 N2 U1 178.9(5) . . ? C3 N3 U1 164.8(5) . . ? C4 N4 U1 165.2(5) . . ? C11 N7 C7 121.2(4) . . ? C11 N7 H7A 119.4 . . ? C7 N7 H7A 119.4 . . ? C9 N8 H8A 120.0 . . ? C9 N8 H8B 120.0 . . ? H8A N8 H8B 120.0 . . ? C12 N9 C16 120.3(4) . . ? C12 N9 H9 119.8 . . ? C16 N9 H9 119.8 . . ? C14 N10 H10A 120.0 . . ? C14 N10 H10B 120.0 . . ? H10A N10 H10B 120.0 . . ? O3 U2 O2 179.2(2) . . ? O3 U2 N6 89.65(15) . . ? O2 U2 N6 90.98(15) . . ? O3 U2 N6 89.65(15) . 4_575 ? O2 U2 N6 90.98(15) . 4_575 ? N6 U2 N6 71.78(19) . 4_575 ? O3 U2 N5 88.85(10) . 4_575 ? O2 U2 N5 90.89(11) . 4_575 ? N6 U2 N5 73.37(13) . 4_575 ? N6 U2 N5 145.12(13) 4_575 4_575 ? O3 U2 N5 88.85(10) . . ? O2 U2 N5 90.89(11) . . ? N6 U2 N5 145.12(13) . . ? N6 U2 N5 73.37(13) 4_575 . ? N5 U2 N5 141.42(18) 4_575 . ? O3 U2 OW2 88.16(18) . . ? O2 U2 OW2 91.07(19) . . ? N6 U2 OW2 144.05(9) . . ? N6 U2 OW2 144.05(10) 4_575 . ? N5 U2 OW2 70.72(9) 4_575 . ? N5 U2 OW2 70.72(9) . . ? O1 U1 O1 179.7(2) 4_575 . ? O1 U1 N3 89.99(11) 4_575 . ? O1 U1 N3 89.99(11) . . ? O1 U1 N4 89.85(10) 4_575 . ? O1 U1 N4 89.85(10) . . ? N3 U1 N4 74.05(18) . . ? O1 U1 N1 90.10(11) 4_575 . ? O1 U1 N1 90.10(11) . . ? N3 U1 N1 143.09(19) . . ? N4 U1 N1 142.86(18) . . ? O1 U1 N2 90.14(11) 4_575 . ? O1 U1 N2 90.14(11) . . ? N3 U1 N2 70.81(19) . . ? N4 U1 N2 144.86(19) . . ? N1 U1 N2 72.29(18) . . ? O1 U1 OW1 89.93(11) 4_575 . ? O1 U1 OW1 89.92(11) . . ? N3 U1 OW1 145.28(18) . . ? N4 U1 OW1 71.23(17) . . ? N1 U1 OW1 71.62(17) . . ? N2 U1 OW1 143.91(17) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C15 H15 S5 0.93 2.93 3.841(5) 167.0 . N10 H10A N5 0.86 2.34 3.185(6) 167.7 . _refine_diff_density_max 1.714 _refine_diff_density_min -1.477 _refine_diff_density_rms 0.210 _shelxl_version_number 2013-4 _shelx_res_file ; TITL P21onm in P2(1)/m CELL 0.71073 8.7580 16.0178 16.1291 90.000 95.253 90.000 ZERR 4.00 0.0007 0.0014 0.0014 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, - Z SFAC C H N O S U UNIT 56 56 32 12 16 4 MERG 2 EQIV $1 -x, -y+1, -z+1 HTAB C8 S2_$1 EQIV $2 x-1, y, z-1 HTAB C10 S6_$2 EQIV $3 x, y, z-1 HTAB C11 N2_$3 EQIV $4 -x+1, y+1/2, -z+1 HTAB C12 S2_$4 HTAB C13 N4_$3 HTAB C15 S5 EQIV $5 x, -y+3/2, z-1 HTAB N7 S1_$5 HTAB N8 S2_$1 HTAB N8 N6_$2 HTAB N9 S2_$4 EQIV $6 -x+2, -y+2, -z+2 HTAB N9 S3_$6 HTAB N10 N5 HTAB N10 S4_$3 FMAP 2 PLAN 25 ACTA 50.00 HTAB 2.00000 BOND $H L.S. 24 WGHT 0.011200 10.551301 FVAR 0.05529 C5 1 0.537613 0.966094 0.750174 11.00000 0.00853 0.01511 = 0.00920 0.00229 0.00220 -0.00036 C6 1 0.088345 0.629180 0.750142 11.00000 0.01811 0.01036 = 0.00853 0.00043 0.00585 0.00233 C1 1 0.953251 0.750000 1.449074 10.50000 0.01287 0.01273 = 0.01086 0.00000 0.00205 0.00000 C2 1 0.536486 0.750000 1.352683 10.50000 0.01050 0.00501 = 0.01004 0.00000 -0.00335 0.00000 C3 1 0.500433 0.750000 1.110889 10.50000 0.01497 0.00396 = 0.01634 0.00000 0.00332 0.00000 C4 1 0.946391 0.750000 1.016494 10.50000 0.00227 0.01382 = 0.02303 0.00000 0.00093 0.00000 C7 1 0.340290 0.405823 0.006054 11.00000 0.02929 0.00816 = 0.01892 0.00288 0.00127 -0.00150 AFIX 43 H7 2 0.383910 0.353957 0.018959 11.00000 -1.20000 AFIX 0 C8 1 0.252725 0.443302 0.060325 11.00000 0.01889 0.01886 = 0.01156 -0.00196 0.00029 -0.00701 AFIX 43 H8 2 0.235979 0.416776 0.109977 11.00000 -1.20000 AFIX 0 C9 1 0.186965 0.522143 0.041992 11.00000 0.01304 0.01588 = 0.01281 -0.00315 -0.00129 0.00168 C10 1 0.216648 0.559330 -0.034317 11.00000 0.01990 0.01599 = 0.02107 0.00393 -0.00067 0.00365 AFIX 43 H10 2 0.176692 0.611688 -0.048723 11.00000 -1.20000 AFIX 0 C11 1 0.304092 0.518077 -0.086654 11.00000 0.02050 0.02186 = 0.01768 0.00422 0.00329 -0.00098 AFIX 43 H11 2 0.322105 0.542301 -0.137247 11.00000 -1.20000 AFIX 0 C12 1 0.809206 0.992375 0.398737 11.00000 0.02577 0.01413 = 0.01411 -0.00200 0.00864 -0.00006 AFIX 43 H12 2 0.834872 0.985175 0.344506 11.00000 -1.20000 AFIX 0 C13 1 0.719725 0.935105 0.432491 11.00000 0.02587 0.01013 = 0.01611 -0.00435 0.00170 -0.00378 AFIX 43 H13 2 0.686146 0.888354 0.401850 11.00000 -1.20000 AFIX 0 C14 1 0.677123 0.946158 0.514258 11.00000 0.01059 0.01041 = 0.01614 0.00206 -0.00030 0.00016 C15 1 0.733326 1.017617 0.557482 11.00000 0.01425 0.01624 = 0.00956 -0.00289 0.00257 -0.00135 AFIX 43 H15 2 0.708330 1.027162 0.611485 11.00000 -1.20000 AFIX 0 C16 1 0.822971 1.072255 0.521284 11.00000 0.01511 0.01308 = 0.02259 -0.00400 0.00265 -0.00046 AFIX 43 H16 2 0.858970 1.119342 0.550624 11.00000 -1.20000 AFIX 0 N5 3 0.521383 0.894251 0.739391 11.00000 0.01199 0.01408 = 0.01650 0.00103 0.00310 0.00007 N6 3 0.208207 0.660468 0.758970 11.00000 0.01320 0.01509 = 0.02097 0.00002 0.00398 -0.00248 N1 3 0.962217 0.750000 1.377767 10.50000 0.01182 0.02174 = 0.01305 0.00000 0.00552 0.00000 N2 3 0.642251 0.750000 1.314383 10.50000 0.01809 0.01022 = 0.01084 0.00000 0.00177 0.00000 N3 3 0.629116 0.750000 1.138815 10.50000 0.01752 0.02080 = 0.01360 0.00000 0.00388 0.00000 N4 3 0.942440 0.750000 1.089435 10.50000 0.00567 0.02269 = 0.01360 0.00000 0.00425 0.00000 N7 3 0.364624 0.443152 -0.066471 11.00000 0.02304 0.01761 = 0.01823 -0.00116 0.00937 0.00448 AFIX 43 H7A 2 0.419981 0.418445 -0.100393 11.00000 -1.20000 AFIX 0 N8 3 0.098564 0.559308 0.094081 11.00000 0.02002 0.02363 = 0.01825 0.00264 0.00527 0.00415 AFIX 93 H8A 2 0.080835 0.535108 0.139821 11.00000 -1.20000 H8B 2 0.059289 0.607473 0.081930 11.00000 -1.20000 AFIX 0 N9 3 0.861814 1.059916 0.442758 11.00000 0.01883 0.01272 = 0.01649 -0.00023 0.00536 -0.00491 AFIX 43 H9 2 0.920211 1.095233 0.420847 11.00000 -1.20000 AFIX 0 N10 3 0.586825 0.891394 0.548423 11.00000 0.02114 0.01467 = 0.01569 -0.00202 0.00407 -0.00752 AFIX 93 H10A 2 0.561608 0.899363 0.598106 11.00000 -1.20000 H10B 2 0.553809 0.848108 0.520774 11.00000 -1.20000 AFIX 0 O2 4 0.473112 0.750000 0.856960 10.50000 0.01338 0.01729 = 0.01385 0.00000 0.00211 0.00000 O3 4 0.392798 0.750000 0.637940 10.50000 0.01514 0.00763 = 0.01243 0.00000 0.00466 0.00000 O1 4 0.863283 0.639814 1.230511 11.00000 0.01811 0.01482 = 0.01501 0.00001 0.00380 0.00185 OW2 4 0.708244 0.750000 0.727059 10.50000 0.00871 0.01321 = 0.02285 0.00000 0.00751 0.00000 OW1 4 1.146288 0.750000 1.238684 10.50000 0.01019 0.04488 = 0.01649 0.00000 -0.00026 0.00000 S5 5 0.560582 1.065758 0.762706 11.00000 0.02970 0.00957 = 0.01670 -0.00105 0.00612 -0.00103 S6 5 -0.078076 0.582620 0.734293 11.00000 0.01167 0.01471 = 0.01708 -0.00133 0.00311 -0.00206 S1 5 0.944350 0.750000 1.549523 10.50000 0.03363 0.01690 = 0.01019 0.00000 0.00733 0.00000 S2 5 0.389503 0.750000 1.408957 10.50000 0.00985 0.01793 = 0.01360 0.00000 0.00368 0.00000 S3 5 0.325539 0.750000 1.070233 10.50000 0.00781 0.03773 = 0.01808 0.00000 -0.00178 0.00000 S4 5 0.957591 0.750000 0.918208 10.50000 0.02393 0.01899 = 0.01046 0.00000 0.00361 0.00000 U2 6 0.431596 0.750000 0.747482 10.50000 0.00832 0.00896 = 0.00946 0.00000 0.00260 0.00000 U1 6 0.863034 0.750000 1.230759 10.50000 0.00785 0.01140 = 0.00869 0.00000 0.00164 0.00000 HKLF 4 REM P21onm in P2(1)/m REM R1 = 0.0345 for 4687 Fo > 4sig(Fo) and 0.0497 for all 5798 data REM 298 parameters refined using 0 restraints END WGHT 0.0110 10.6513 REM Instructions for potential hydrogen bonds HTAB C8 S6_$1 HTAB C10 S4_$2 HTAB C11 N6_$3 HTAB C12 S6_$4 HTAB C13 N2_$3 HTAB C15 S5 HTAB N7 S5_$5 HTAB N8 S6_$1 HTAB N8 N4_$2 HTAB N9 S6_$4 HTAB N9 S1_$6 HTAB N10 N5 HTAB N10 S2_$3 REM Highest difference peak 1.714, deepest hole -1.477, 1-sigma level 0.210 Q1 1 0.9974 0.7500 1.2650 10.50000 0.05 1.71 Q2 1 0.8372 0.7500 0.7926 10.50000 0.05 1.48 Q3 1 1.2725 0.7500 1.2784 10.50000 0.05 1.25 Q4 1 0.2986 0.7500 0.7176 10.50000 0.05 1.17 Q5 1 1.2192 0.7500 1.2001 10.50000 0.05 1.12 Q6 1 0.3677 0.7195 1.3197 11.00000 0.05 0.95 Q7 1 0.3211 0.7500 1.1677 10.50000 0.05 0.95 Q8 1 0.8160 0.7500 0.9151 10.50000 0.05 0.93 Q9 1 0.8833 0.7500 1.4171 10.50000 0.05 0.90 Q10 1 0.7857 0.7234 0.7340 11.00000 0.05 0.88 Q11 1 0.7039 0.7087 1.3653 11.00000 0.05 0.84 Q12 1 0.7720 0.7500 1.1509 10.50000 0.05 0.84 Q13 1 0.1296 0.5098 0.2031 11.00000 0.05 0.83 Q14 1 0.6663 1.0802 0.5264 11.00000 0.05 0.82 Q15 1 -0.0288 0.6535 0.6674 11.00000 0.05 0.82 Q16 1 0.2374 0.7500 0.5839 10.50000 0.05 0.81 Q17 1 0.4079 0.7500 1.0983 10.50000 0.05 0.80 Q18 1 0.9391 0.7500 0.7711 10.50000 0.05 0.80 Q19 1 0.7473 0.7500 1.4807 10.50000 0.05 0.79 Q20 1 0.7553 0.7500 1.5434 10.50000 0.05 0.77 Q21 1 0.8992 1.1677 0.4711 11.00000 0.05 0.76 Q22 1 0.4668 0.7500 0.9537 10.50000 0.05 0.75 Q23 1 1.1970 0.7142 1.2588 11.00000 0.05 0.75 Q24 1 1.0704 0.7500 1.0436 10.50000 0.05 0.75 Q25 1 0.3338 0.7500 0.6632 10.50000 0.05 0.75 ; _shelx_res_checksum 52482 _shelx_hkl_file ; 1 0 0 6.96 0.29 2 0 0 38.45 1.58 3 0 0 77.49 3.06 4 0 0 105.08 4.15 5 0 0 0.85 0.38 6 0 0 15.50 1.26 7 0 0 71.29 3.60 8 0 0 13.23 1.40 9 0 0 6.62 1.23 10 0 0 25.24 2.23 11 0 0 15.48 1.96 0 1 0 0.01 0.02 1 1 0 12.92 0.32 2 1 0 250.06 5.55 3 1 0 0.11 0.16 4 1 0 114.33 3.12 5 1 0 56.31 1.80 6 1 0 0.68 0.32 7 1 0 0.35 0.32 8 1 0 4.86 0.66 9 1 0 70.28 2.64 10 1 0 1.51 0.68 11 1 0 7.22 0.99 0 2 0 214.26 6.18 1 2 0 0.13 0.06 2 2 0 115.90 2.21 3 2 0 11.51 0.40 4 2 0 68.49 1.61 5 2 0 4.96 0.36 6 2 0 1.09 0.28 7 2 0 74.86 2.96 8 2 0 0.29 0.44 9 2 0 3.82 0.67 10 2 0 21.28 1.40 11 2 0 35.95 1.94 0 3 0 0.24 0.16 1 3 0 2.20 0.15 2 3 0 444.91 7.63 3 3 0 5.26 0.25 4 3 0 18.99 0.61 5 3 0 56.10 1.43 6 3 0 0.49 0.25 7 3 0 0.33 0.41 8 3 0 8.01 0.78 9 3 0 60.25 2.38 10 3 0 0.34 0.63 11 3 0 11.98 1.42 0 4 0 619.01 17.71 1 4 0 7.37 0.29 2 4 0 13.91 0.38 3 4 0 9.78 0.42 4 4 0 31.64 0.81 5 4 0 3.04 0.26 6 4 0 0.65 0.29 7 4 0 87.69 2.83 8 4 0 1.71 0.61 9 4 0 2.70 0.65 10 4 0 24.01 1.49 11 4 0 20.42 2.32 0 5 0 0.05 0.19 1 5 0 3.01 0.21 2 5 0 206.26 4.25 3 5 0 11.98 0.54 4 5 0 136.53 3.05 5 5 0 40.71 1.20 6 5 0 3.44 0.38 7 5 0 0.24 0.40 8 5 0 0.10 0.55 9 5 0 51.27 1.92 10 5 0 5.51 0.91 11 5 0 7.95 1.74 0 6 0 1000.00 28.53 1 6 0 9.12 0.38 2 6 0 108.88 2.39 3 6 0 13.08 0.46 4 6 0 77.50 2.11 5 6 0 0.83 0.24 6 6 0 16.72 0.75 7 6 0 58.73 1.74 8 6 0 5.34 0.64 9 6 0 5.04 0.82 10 6 0 26.77 1.64 11 6 0 14.27 2.01 0 7 0 0.06 0.24 1 7 0 27.94 0.80 2 7 0 229.43 4.78 3 7 0 0.36 0.14 4 7 0 43.70 1.38 5 7 0 36.64 1.28 6 7 0 0.16 0.27 7 7 0 0.35 0.30 8 7 0 2.22 0.53 9 7 0 40.54 1.95 10 7 0 1.49 1.09 0 8 0 297.32 8.88 1 8 0 0.84 0.20 2 8 0 34.00 0.97 3 8 0 18.70 0.64 4 8 0 43.68 1.41 5 8 0 1.11 0.32 6 8 0 0.31 0.30 7 8 0 61.10 2.31 8 8 0 0.10 0.45 9 8 0 1.02 0.76 10 8 0 13.52 1.88 0 9 0 0.06 0.27 1 9 0 0.29 0.17 2 9 0 147.94 3.27 3 9 0 1.55 0.24 4 9 0 6.79 0.54 5 9 0 53.16 1.71 6 9 0 1.66 0.39 7 9 0 0.60 0.46 8 9 0 5.65 0.80 9 9 0 74.41 3.42 10 9 0 1.05 1.16 0 10 0 451.44 13.39 1 10 0 1.95 0.27 2 10 0 16.80 0.66 3 10 0 22.20 0.78 4 10 0 44.24 1.49 5 10 0 0.90 0.36 6 10 0 3.40 0.59 7 10 0 69.10 2.59 8 10 0 0.49 0.52 9 10 0 8.40 1.57 10 10 0 23.13 2.49 0 11 0 0.19 0.31 1 11 0 3.38 0.34 2 11 0 151.94 3.43 3 11 0 10.35 0.55 4 11 0 104.97 2.90 5 11 0 48.17 1.93 6 11 0 0.17 0.41 7 11 0 1.13 0.55 8 11 0 3.27 0.76 9 11 0 37.40 3.07 0 12 0 306.84 9.42 1 12 0 0.07 0.23 2 12 0 21.27 0.83 3 12 0 14.34 0.83 4 12 0 28.66 1.40 5 12 0 0.64 0.48 6 12 0 5.68 0.75 7 12 0 33.77 1.73 8 12 0 5.77 1.09 9 12 0 2.72 1.30 0 13 0 0.48 0.47 1 13 0 2.42 0.36 2 13 0 119.78 2.88 3 13 0 5.03 0.64 4 13 0 15.78 1.08 5 13 0 18.99 1.24 6 13 0 0.72 0.60 7 13 0 0.08 0.61 8 13 0 0.28 0.82 9 13 0 25.79 2.67 0 14 0 127.53 4.47 1 14 0 5.53 0.48 2 14 0 18.72 1.13 3 14 0 6.01 0.70 4 14 0 16.11 1.12 5 14 0 0.36 0.52 6 14 0 0.26 0.53 7 14 0 36.19 2.26 8 14 0 0.16 0.85 0 15 0 0.30 0.51 1 15 0 3.20 0.47 2 15 0 46.42 1.91 3 15 0 12.87 1.02 4 15 0 13.07 1.07 5 15 0 30.46 1.61 6 15 0 0.38 0.59 7 15 0 0.08 0.81 8 15 0 3.40 1.12 0 16 0 197.39 8.20 1 16 0 3.28 0.51 2 16 0 12.06 0.99 3 16 0 11.31 1.01 4 16 0 21.87 1.39 5 16 0 1.16 0.65 6 16 0 3.91 1.02 7 16 0 47.79 2.74 0 17 0 0.07 0.73 1 17 0 0.81 0.52 2 17 0 100.33 3.42 3 17 0 2.93 0.67 4 17 0 26.00 1.57 5 17 0 26.47 1.60 6 17 0 0.53 0.88 7 17 0 0.86 1.03 0 18 0 98.78 4.87 1 18 0 0.32 0.67 2 18 0 13.44 1.14 3 18 0 6.59 0.89 4 18 0 17.65 1.37 5 18 0 0.46 0.86 6 18 0 2.42 1.03 0 19 0 1.86 1.61 1 19 0 5.83 0.98 2 19 0 52.55 2.69 3 19 0 0.50 0.62 4 19 0 8.92 1.09 5 19 0 13.69 1.51 0 20 0 83.00 7.31 1 20 0 1.96 0.81 2 20 0 4.85 1.05 3 20 0 6.04 1.08 4 20 0 9.76 1.66 0 21 0 0.00 1.59 1 21 0 0.90 1.16 2 21 0 23.14 1.81 -11 0 1 2.99 1.56 -10 0 1 64.26 3.46 -9 0 1 0.00 1.36 -8 0 1 20.42 1.89 -7 0 1 0.81 0.85 -6 0 1 69.80 2.10 -5 0 1 11.72 1.31 -4 0 1 94.23 3.14 -3 0 1 40.21 1.68 -2 0 1 22.33 0.66 -1 0 1 76.70 1.27 0 0 1 0.19 0.04 1 0 1 110.06 1.80 2 0 1 4.08 0.65 3 0 1 54.35 2.02 4 0 1 86.33 3.55 5 0 1 47.37 2.00 6 0 1 21.84 2.02 7 0 1 8.69 0.75 8 0 1 25.38 1.93 9 0 1 21.11 1.58 10 0 1 39.74 3.30 11 0 1 7.61 1.63 -11 1 1 15.43 1.40 -10 1 1 5.85 0.90 -9 1 1 0.75 0.88 -8 1 1 132.04 3.14 -7 1 1 0.00 0.54 -6 1 1 106.39 2.39 -5 1 1 43.94 0.95 -4 1 1 96.31 2.00 -3 1 1 5.09 0.52 -2 1 1 38.46 0.92 -1 1 1 141.48 1.53 0 1 1 0.14 0.03 1 1 1 118.15 1.36 2 1 1 62.15 1.10 3 1 1 29.36 0.62 4 1 1 50.44 1.94 5 1 1 11.24 0.93 6 1 1 55.28 2.29 7 1 1 12.65 0.59 8 1 1 55.58 2.59 9 1 1 13.12 0.95 10 1 1 1.49 0.90 11 1 1 15.92 1.40 -11 2 1 6.72 2.07 -10 2 1 39.84 1.79 -9 2 1 0.68 0.73 -8 2 1 7.37 0.74 -7 2 1 4.75 0.52 -6 2 1 124.15 2.49 -5 2 1 30.90 0.76 -4 2 1 133.03 2.83 -3 2 1 295.73 5.26 -2 2 1 4.65 0.14 -1 2 1 84.09 0.97 0 2 1 0.73 0.06 1 2 1 142.04 1.47 2 2 1 0.09 0.08 3 2 1 193.22 5.12 4 2 1 104.02 2.58 5 2 1 0.00 0.54 6 2 1 49.01 2.17 7 2 1 0.00 0.57 8 2 1 1.67 0.69 9 2 1 3.78 0.76 10 2 1 23.09 1.70 11 2 1 31.84 1.99 -11 3 1 5.18 1.79 -10 3 1 1.28 0.95 -9 3 1 16.81 1.24 -8 3 1 100.77 2.69 -7 3 1 26.49 0.94 -6 3 1 58.49 1.58 -5 3 1 42.04 1.53 -4 3 1 59.00 1.24 -3 3 1 3.39 0.40 -2 3 1 25.45 0.46 -1 3 1 255.80 2.68 0 3 1 15.05 0.29 1 3 1 212.69 2.45 2 3 1 24.44 0.44 3 3 1 38.12 0.74 4 3 1 27.16 1.07 5 3 1 76.98 1.60 6 3 1 45.78 1.55 7 3 1 2.67 0.98 8 3 1 59.69 2.94 9 3 1 8.04 1.06 10 3 1 1.11 0.96 11 3 1 18.02 1.70 -11 4 1 6.81 2.07 -10 4 1 33.54 2.50 -9 4 1 0.00 0.82 -8 4 1 17.04 1.04 -7 4 1 0.55 0.59 -6 4 1 83.45 2.34 -5 4 1 5.45 0.30 -4 4 1 78.45 1.88 -3 4 1 176.70 2.90 -2 4 1 2.79 0.11 -1 4 1 50.70 0.76 0 4 1 3.82 0.19 1 4 1 56.55 0.83 2 4 1 0.47 0.10 3 4 1 120.85 2.34 4 4 1 78.52 1.85 5 4 1 0.33 0.32 6 4 1 30.50 1.91 7 4 1 0.36 0.57 8 4 1 3.54 1.20 9 4 1 2.38 0.82 10 4 1 26.28 2.14 11 4 1 23.16 2.20 -11 5 1 11.14 1.40 -10 5 1 0.98 0.91 -9 5 1 0.00 0.86 -8 5 1 103.75 2.39 -7 5 1 6.42 0.69 -6 5 1 66.78 1.64 -5 5 1 21.31 0.63 -4 5 1 68.07 1.27 -3 5 1 4.32 0.44 -2 5 1 35.42 0.64 -1 5 1 73.27 1.09 0 5 1 12.58 0.34 1 5 1 72.18 1.08 2 5 1 29.27 0.64 3 5 1 36.47 0.70 4 5 1 14.59 0.90 5 5 1 5.85 0.50 6 5 1 31.63 1.41 7 5 1 5.41 0.80 8 5 1 29.88 2.91 9 5 1 11.75 0.95 10 5 1 2.06 1.01 11 5 1 7.85 1.71 -11 6 1 7.75 1.87 -10 6 1 52.27 2.21 -9 6 1 6.99 1.01 -8 6 1 13.84 1.12 -7 6 1 0.78 0.50 -6 6 1 64.67 1.68 -5 6 1 0.52 0.51 -4 6 1 86.70 1.85 -3 6 1 48.99 1.08 -2 6 1 0.32 0.15 -1 6 1 13.62 0.40 0 6 1 0.76 0.14 1 6 1 18.91 0.45 2 6 1 5.46 0.25 3 6 1 51.58 1.05 4 6 1 52.44 1.52 5 6 1 14.07 0.59 6 6 1 32.15 1.54 7 6 1 1.30 0.46 8 6 1 25.77 1.25 9 6 1 18.02 1.14 10 6 1 26.95 2.22 11 6 1 8.51 1.92 -10 7 1 0.46 1.09 -9 7 1 5.37 0.92 -8 7 1 84.66 2.78 -7 7 1 0.30 0.50 -6 7 1 84.76 2.17 -5 7 1 29.29 0.89 -4 7 1 33.71 0.99 -3 7 1 8.55 0.33 -2 7 1 43.75 0.92 -1 7 1 127.63 1.76 0 7 1 0.91 0.16 1 7 1 75.83 1.24 2 7 1 70.93 1.18 3 7 1 14.82 0.37 4 7 1 23.93 0.85 5 7 1 5.45 0.78 6 7 1 54.57 2.06 7 7 1 0.37 0.48 8 7 1 64.09 2.68 9 7 1 2.17 0.97 10 7 1 2.71 1.26 -10 8 1 38.36 2.31 -9 8 1 0.00 0.85 -8 8 1 12.16 0.96 -7 8 1 3.10 0.64 -6 8 1 124.80 2.42 -5 8 1 17.65 0.69 -4 8 1 69.77 1.84 -3 8 1 183.54 3.07 -2 8 1 8.79 0.36 -1 8 1 54.73 1.02 0 8 1 0.12 0.13 1 8 1 103.27 1.51 2 8 1 2.09 0.25 3 8 1 143.33 2.56 4 8 1 71.94 1.70 5 8 1 1.14 0.62 6 8 1 25.75 2.02 7 8 1 0.33 0.57 8 8 1 0.00 0.95 9 8 1 1.88 1.10 10 8 1 18.28 2.51 -10 9 1 2.58 1.46 -9 9 1 7.81 1.24 -8 9 1 89.94 2.82 -7 9 1 20.04 1.01 -6 9 1 42.20 1.68 -5 9 1 23.92 1.21 -4 9 1 47.47 1.46 -3 9 1 3.46 0.41 -2 9 1 26.91 0.76 -1 9 1 139.87 2.16 0 9 1 3.07 0.26 1 9 1 167.96 2.45 2 9 1 27.62 0.76 3 9 1 22.26 0.61 4 9 1 38.00 1.42 5 9 1 40.39 1.29 6 9 1 36.75 1.53 7 9 1 0.26 0.90 8 9 1 41.85 2.82 9 9 1 12.23 1.56 10 9 1 0.00 1.43 -10 10 1 23.19 2.62 -9 10 1 0.00 1.00 -8 10 1 4.81 1.00 -7 10 1 0.33 0.71 -6 10 1 37.53 1.72 -5 10 1 0.00 0.51 -4 10 1 48.88 1.49 -3 10 1 107.72 2.17 -2 10 1 5.92 0.40 -1 10 1 47.28 1.01 0 10 1 2.74 0.28 1 10 1 60.54 1.14 2 10 1 5.60 0.40 3 10 1 54.61 1.74 4 10 1 35.89 1.44 5 10 1 0.84 0.47 6 10 1 37.88 1.72 7 10 1 1.39 0.71 8 10 1 5.05 1.25 9 10 1 5.39 1.30 10 10 1 21.49 2.58 -9 11 1 1.98 1.20 -8 11 1 77.71 2.83 -7 11 1 2.32 0.77 -6 11 1 51.65 1.80 -5 11 1 39.47 1.28 -4 11 1 47.93 1.39 -3 11 1 1.93 0.71 -2 11 1 4.04 0.42 -1 11 1 38.74 0.91 0 11 1 4.06 0.38 1 11 1 14.84 0.74 2 11 1 7.96 0.46 3 11 1 28.44 0.77 4 11 1 8.60 1.10 5 11 1 5.34 1.02 6 11 1 21.67 1.64 7 11 1 1.53 0.78 8 11 1 38.03 3.26 9 11 1 2.12 1.34 -9 12 1 3.17 1.35 -8 12 1 14.12 1.28 -7 12 1 0.98 0.77 -6 12 1 56.85 1.86 -5 12 1 0.37 0.70 -4 12 1 67.38 2.48 -3 12 1 29.42 1.40 -2 12 1 0.47 0.30 -1 12 1 28.05 0.93 0 12 1 0.18 0.33 1 12 1 26.24 0.94 2 12 1 0.16 0.31 3 12 1 31.72 1.30 4 12 1 78.17 2.34 5 12 1 6.63 0.75 6 12 1 14.71 1.64 7 12 1 0.00 0.83 8 12 1 1.92 1.54 9 12 1 6.81 1.66 -9 13 1 5.10 1.42 -8 13 1 59.08 3.20 -7 13 1 4.49 0.90 -6 13 1 42.41 1.93 -5 13 1 12.29 1.08 -4 13 1 10.01 1.08 -3 13 1 1.36 0.67 -2 13 1 36.12 1.24 -1 13 1 76.93 1.93 0 13 1 4.86 0.49 1 13 1 63.00 1.87 2 13 1 27.82 1.13 3 13 1 6.37 0.63 4 13 1 20.86 1.14 5 13 1 12.18 1.07 6 13 1 36.11 1.89 7 13 1 0.33 0.95 8 13 1 52.36 3.60 9 13 1 3.91 1.68 -8 14 1 13.11 1.53 -7 14 1 0.00 0.86 -6 14 1 52.14 1.95 -5 14 1 5.47 0.82 -4 14 1 38.58 1.74 -3 14 1 78.11 2.47 -2 14 1 2.38 0.62 -1 14 1 15.56 1.11 0 14 1 0.70 0.43 1 14 1 40.25 1.15 2 14 1 0.27 0.54 3 14 1 48.79 2.31 4 14 1 32.66 1.71 5 14 1 0.00 0.77 6 14 1 12.46 1.90 7 14 1 1.20 0.97 8 14 1 0.00 1.56 -8 15 1 38.07 2.45 -7 15 1 5.39 1.05 -6 15 1 19.58 1.40 -5 15 1 22.68 1.38 -4 15 1 28.28 1.34 -3 15 1 1.22 0.76 -2 15 1 4.18 0.91 -1 15 1 59.22 1.86 0 15 1 0.79 0.45 1 15 1 53.59 1.74 2 15 1 14.83 0.96 3 15 1 5.79 0.79 4 15 1 7.58 1.22 5 15 1 13.67 1.32 6 15 1 10.79 1.49 7 15 1 1.33 1.11 8 15 1 22.57 2.70 -7 16 1 1.62 1.21 -6 16 1 24.15 1.70 -5 16 1 0.17 0.83 -4 16 1 17.31 1.32 -3 16 1 45.45 1.92 -2 16 1 2.10 0.76 -1 16 1 17.36 1.25 0 16 1 0.00 0.50 1 16 1 25.87 1.17 2 16 1 4.05 0.77 3 16 1 33.48 1.86 4 16 1 18.57 1.35 5 16 1 1.70 0.91 6 16 1 23.68 1.87 7 16 1 0.00 1.37 -7 17 1 0.76 0.62 -6 17 1 28.24 2.07 -5 17 1 7.27 1.05 -4 17 1 14.71 1.13 -3 17 1 9.00 1.15 -2 17 1 10.33 1.05 -1 17 1 20.13 1.33 0 17 1 1.03 0.67 1 17 1 15.52 1.40 2 17 1 8.93 1.04 3 17 1 15.66 1.17 4 17 1 2.41 1.06 5 17 1 1.64 1.09 6 17 1 24.97 2.09 -6 18 1 47.21 2.41 -5 18 1 0.00 0.95 -4 18 1 27.70 1.90 -3 18 1 35.18 1.75 -2 18 1 0.00 0.78 -1 18 1 11.74 1.38 0 18 1 0.15 0.82 1 18 1 16.50 1.41 2 18 1 1.51 0.86 3 18 1 22.35 1.68 4 18 1 37.15 2.12 5 18 1 1.13 1.05 6 18 1 14.15 2.22 -5 19 1 11.53 1.49 -4 19 1 15.26 1.37 -3 19 1 4.97 1.01 -2 19 1 19.72 1.60 -1 19 1 50.10 2.34 0 19 1 2.22 1.39 1 19 1 26.44 2.22 2 19 1 11.82 1.54 3 19 1 0.63 1.10 4 19 1 1.87 1.57 5 19 1 3.81 1.45 -4 20 1 23.02 1.65 -3 20 1 30.97 2.22 -2 20 1 0.00 1.08 -1 20 1 10.07 1.71 0 20 1 0.00 1.32 1 20 1 24.23 2.03 2 20 1 0.57 1.27 3 20 1 25.25 2.45 -2 21 1 1.32 0.62 -1 21 1 19.33 2.37 0 21 1 3.24 1.68 1 21 1 18.76 2.39 -11 0 2 0.00 1.83 -10 0 2 20.10 2.11 -9 0 2 40.77 2.36 -8 0 2 1.79 1.09 -7 0 2 79.45 3.14 -6 0 2 27.03 1.12 -5 0 2 8.66 0.54 -4 0 2 66.01 1.46 -3 0 2 185.20 2.93 -2 0 2 86.79 1.60 -1 0 2 15.52 0.33 0 0 2 208.89 2.49 1 0 2 26.77 0.53 2 0 2 172.48 2.68 3 0 2 264.16 4.07 4 0 2 45.16 1.14 5 0 2 0.50 0.33 6 0 2 16.63 1.10 7 0 2 147.55 4.13 8 0 2 2.67 1.09 9 0 2 10.89 2.16 10 0 2 13.12 2.05 11 0 2 7.44 2.44 -11 1 2 28.66 1.89 -10 1 2 0.09 0.94 -9 1 2 33.43 2.02 -8 1 2 0.34 0.56 -7 1 2 16.42 0.75 -6 1 2 17.19 0.59 -5 1 2 139.90 1.96 -4 1 2 77.04 1.05 -3 1 2 12.04 0.33 -2 1 2 208.81 2.25 -1 1 2 3.12 0.10 0 1 2 12.00 0.18 1 1 2 14.19 0.23 2 1 2 179.39 1.97 3 1 2 37.38 0.60 4 1 2 1.55 0.17 5 1 2 229.96 2.94 6 1 2 10.07 0.56 7 1 2 2.79 0.70 8 1 2 0.31 0.43 9 1 2 59.50 2.15 10 1 2 3.61 1.01 11 1 2 2.44 1.75 -11 2 2 8.78 1.91 -10 2 2 17.45 1.24 -9 2 2 22.86 1.33 -8 2 2 1.59 0.64 -7 2 2 85.10 2.46 -6 2 2 1.82 0.28 -5 2 2 0.05 0.12 -4 2 2 123.28 1.60 -3 2 2 68.65 0.94 -2 2 2 3.14 0.14 -1 2 2 0.56 0.09 0 2 2 352.69 3.62 1 2 2 19.16 0.29 2 2 2 145.74 1.64 3 2 2 128.10 1.56 4 2 2 25.46 0.56 5 2 2 9.00 0.39 6 2 2 0.97 0.23 7 2 2 167.86 2.99 8 2 2 2.90 0.68 9 2 2 8.75 1.37 10 2 2 2.30 1.17 11 2 2 10.46 1.71 -11 3 2 26.44 2.14 -10 3 2 0.00 1.30 -9 3 2 35.42 2.21 -8 3 2 1.42 0.69 -7 3 2 17.36 0.76 -6 3 2 25.92 0.72 -5 3 2 121.95 1.77 -4 3 2 8.15 0.30 -3 3 2 33.59 0.54 -2 3 2 35.90 0.51 -1 3 2 7.04 0.23 0 3 2 0.36 0.08 1 3 2 12.60 0.30 2 3 2 39.34 0.53 3 3 2 36.97 0.61 4 3 2 13.17 0.40 5 3 2 182.39 2.42 6 3 2 5.13 0.40 7 3 2 0.96 0.34 8 3 2 2.59 0.71 9 3 2 51.61 2.08 10 3 2 2.84 1.19 11 3 2 0.00 1.73 -11 4 2 6.12 1.89 -10 4 2 31.32 2.14 -9 4 2 31.28 1.72 -8 4 2 1.39 0.56 -7 4 2 97.93 2.61 -6 4 2 9.19 0.50 -5 4 2 1.56 0.23 -4 4 2 47.86 0.80 -3 4 2 65.56 0.91 -2 4 2 4.64 0.18 -1 4 2 58.72 0.73 0 4 2 76.62 0.95 1 4 2 67.46 0.82 2 4 2 5.30 0.19 3 4 2 57.81 0.83 4 4 2 66.08 0.98 5 4 2 12.57 0.43 6 4 2 0.19 0.17 7 4 2 188.19 3.94 8 4 2 0.20 0.49 9 4 2 12.07 1.63 10 4 2 4.84 1.73 11 4 2 11.79 1.72 -11 5 2 24.50 1.81 -10 5 2 1.56 1.17 -9 5 2 14.02 1.23 -8 5 2 0.39 0.46 -7 5 2 11.38 0.62 -6 5 2 3.29 0.40 -5 5 2 94.68 1.40 -4 5 2 73.29 1.09 -3 5 2 15.23 0.41 -2 5 2 175.31 2.01 -1 5 2 5.27 0.23 0 5 2 4.75 0.21 1 5 2 30.41 0.50 2 5 2 196.64 2.22 3 5 2 43.55 0.73 4 5 2 0.55 0.14 5 5 2 168.15 2.08 6 5 2 0.34 0.27 7 5 2 4.11 0.52 8 5 2 0.61 0.54 9 5 2 36.16 1.38 10 5 2 6.35 1.46 11 5 2 7.74 2.08 -11 6 2 4.43 1.03 -10 6 2 19.07 1.51 -9 6 2 16.28 1.13 -8 6 2 1.11 0.54 -7 6 2 80.80 1.82 -6 6 2 11.71 0.73 -5 6 2 6.15 0.37 -4 6 2 77.12 1.18 -3 6 2 52.14 0.86 -2 6 2 57.77 0.83 -1 6 2 20.05 0.42 0 6 2 152.25 1.79 1 6 2 21.87 0.44 2 6 2 15.97 0.37 3 6 2 113.66 1.53 4 6 2 13.40 0.43 5 6 2 1.33 0.19 6 6 2 21.07 0.85 7 6 2 119.98 2.25 8 6 2 2.11 0.54 9 6 2 8.05 1.18 10 6 2 8.79 1.56 11 6 2 0.00 1.98 -11 7 2 17.99 1.26 -10 7 2 0.15 0.87 -9 7 2 28.80 1.84 -8 7 2 0.05 0.54 -7 7 2 13.71 0.77 -6 7 2 7.51 0.50 -5 7 2 89.55 1.61 -4 7 2 25.70 0.62 -3 7 2 12.63 0.35 -2 7 2 123.61 1.55 -1 7 2 6.64 0.28 0 7 2 6.43 0.28 1 7 2 6.49 0.28 2 7 2 42.54 0.70 3 7 2 21.78 0.42 4 7 2 10.54 0.40 5 7 2 146.47 2.28 6 7 2 6.55 0.49 7 7 2 1.25 0.40 8 7 2 0.00 0.52 9 7 2 37.78 2.27 10 7 2 2.10 1.09 -10 8 2 11.02 1.29 -9 8 2 19.52 1.33 -8 8 2 11.34 0.88 -7 8 2 50.32 1.53 -6 8 2 5.32 0.53 -5 8 2 0.54 0.22 -4 8 2 57.76 1.03 -3 8 2 50.67 0.82 -2 8 2 0.73 0.14 -1 8 2 0.23 0.12 0 8 2 146.20 1.80 1 8 2 10.58 0.38 2 8 2 7.61 0.34 3 8 2 91.97 1.27 4 8 2 39.43 0.79 5 8 2 0.30 0.21 6 8 2 8.32 0.60 7 8 2 132.32 2.48 8 8 2 0.38 0.53 9 8 2 6.93 1.26 10 8 2 8.50 1.44 -10 9 2 0.02 0.81 -9 9 2 42.74 2.13 -8 9 2 1.42 0.61 -7 9 2 6.05 0.61 -6 9 2 30.03 1.03 -5 9 2 104.08 1.94 -4 9 2 8.11 0.40 -3 9 2 13.16 0.41 -2 9 2 41.41 0.74 -1 9 2 4.54 0.27 0 9 2 0.22 0.14 1 9 2 14.75 0.46 2 9 2 14.06 0.45 3 9 2 38.09 0.72 4 9 2 0.29 0.19 5 9 2 134.63 2.41 6 9 2 8.43 0.58 7 9 2 0.12 0.30 8 9 2 3.15 0.72 9 9 2 50.26 2.72 10 9 2 0.99 1.14 -10 10 2 14.77 1.65 -9 10 2 24.97 1.52 -8 10 2 0.05 0.67 -7 10 2 91.72 2.35 -6 10 2 1.87 0.40 -5 10 2 0.02 0.22 -4 10 2 54.53 1.25 -3 10 2 60.19 0.98 -2 10 2 9.70 0.40 -1 10 2 14.21 0.47 0 10 2 105.69 1.55 1 10 2 20.79 0.55 2 10 2 0.71 0.17 3 10 2 68.04 1.15 4 10 2 22.74 0.83 5 10 2 16.68 0.77 6 10 2 3.66 0.44 7 10 2 117.83 2.55 8 10 2 1.96 0.85 9 10 2 6.92 1.38 10 10 2 8.04 1.54 -10 11 2 1.07 0.63 -9 11 2 17.42 1.53 -8 11 2 0.32 0.50 -7 11 2 21.01 1.17 -6 11 2 3.59 0.52 -5 11 2 83.02 1.69 -4 11 2 50.81 1.23 -3 11 2 4.76 0.39 -2 11 2 123.00 1.70 -1 11 2 0.21 0.16 0 11 2 5.36 0.33 1 11 2 4.07 0.30 2 11 2 86.10 1.30 3 11 2 11.60 0.50 4 11 2 6.90 0.52 5 11 2 166.21 2.70 6 11 2 0.26 0.35 7 11 2 4.59 0.79 8 11 2 0.68 0.58 9 11 2 25.50 2.01 -9 12 2 14.00 1.35 -8 12 2 0.57 0.53 -7 12 2 37.54 1.69 -6 12 2 15.94 0.93 -5 12 2 0.42 0.35 -4 12 2 30.50 1.08 -3 12 2 29.70 0.88 -2 12 2 11.43 0.52 -1 12 2 1.79 0.26 0 12 2 109.37 1.58 1 12 2 6.63 0.39 2 12 2 0.06 0.17 3 12 2 50.27 1.19 4 12 2 27.81 0.94 5 12 2 1.11 0.41 6 12 2 3.14 0.55 7 12 2 75.60 2.30 8 12 2 1.70 0.66 9 12 2 5.65 1.27 -9 13 2 13.93 1.76 -8 13 2 0.59 0.70 -7 13 2 4.57 0.78 -6 13 2 8.98 0.87 -5 13 2 34.54 1.35 -4 13 2 14.31 0.78 -3 13 2 0.80 0.30 -2 13 2 38.16 0.92 -1 13 2 4.08 0.35 0 13 2 0.21 0.20 1 13 2 10.13 0.50 2 13 2 19.95 0.68 3 13 2 7.80 0.54 4 13 2 6.53 0.54 5 13 2 53.95 1.61 6 13 2 6.62 0.88 7 13 2 0.97 0.60 8 13 2 0.57 0.68 9 13 2 24.72 2.20 -8 14 2 3.45 0.75 -7 14 2 38.91 1.79 -6 14 2 1.40 0.56 -5 14 2 0.14 0.39 -4 14 2 20.21 1.00 -3 14 2 28.71 1.05 -2 14 2 0.58 0.29 -1 14 2 1.46 0.33 0 14 2 48.09 1.07 1 14 2 12.54 0.60 2 14 2 0.35 0.24 3 14 2 43.22 1.21 4 14 2 5.67 0.60 5 14 2 1.75 0.49 6 14 2 0.98 0.59 7 14 2 68.25 2.38 8 14 2 0.30 0.60 -8 15 2 0.23 0.67 -7 15 2 4.81 0.82 -6 15 2 4.54 0.77 -5 15 2 53.90 1.98 -4 15 2 6.13 0.66 -3 15 2 12.63 0.79 -2 15 2 40.03 1.20 -1 15 2 0.18 0.26 0 15 2 2.58 0.41 1 15 2 0.22 0.24 2 15 2 20.95 0.90 3 15 2 20.84 1.00 4 15 2 0.14 0.33 5 15 2 86.41 2.53 6 15 2 1.22 0.68 7 15 2 0.42 0.58 8 15 2 1.05 0.74 -7 16 2 47.15 2.15 -6 16 2 2.21 0.72 -5 16 2 0.84 0.58 -4 16 2 26.05 1.22 -3 16 2 19.52 1.01 -2 16 2 8.97 0.69 -1 16 2 11.57 0.71 0 16 2 46.92 1.28 1 16 2 11.81 0.69 2 16 2 3.64 0.50 3 16 2 27.54 1.17 4 16 2 12.73 0.88 5 16 2 5.48 0.84 6 16 2 3.49 0.79 7 16 2 73.78 2.62 -7 17 2 3.51 0.74 -6 17 2 0.89 0.65 -5 17 2 48.50 1.98 -4 17 2 16.40 1.04 -3 17 2 3.46 0.56 -2 17 2 45.09 1.48 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16.57 0.47 3 0 3 17.61 0.55 4 0 3 84.48 1.63 5 0 3 20.77 0.75 6 0 3 14.69 0.72 7 0 3 1.32 0.33 8 0 3 46.01 1.56 9 0 3 1.66 0.59 10 0 3 38.59 2.00 11 0 3 19.45 1.96 -11 1 3 13.88 1.29 -10 1 3 1.55 0.47 -9 1 3 1.16 0.41 -8 1 3 105.39 1.88 -7 1 3 1.14 0.21 -6 1 3 41.14 0.78 -5 1 3 38.98 0.69 -4 1 3 39.43 0.65 -3 1 3 17.59 0.38 -2 1 3 11.85 0.27 -1 1 3 258.11 2.73 0 1 3 20.85 0.32 1 1 3 142.71 1.51 2 1 3 48.43 0.67 3 1 3 61.08 0.85 4 1 3 18.88 0.45 5 1 3 3.19 0.24 6 1 3 67.37 1.09 7 1 3 10.28 0.50 8 1 3 45.43 1.19 9 1 3 9.90 0.81 10 1 3 18.13 1.16 11 1 3 10.57 1.18 -11 2 3 5.23 0.81 -10 2 3 54.64 1.72 -9 2 3 0.52 0.33 -8 2 3 1.52 0.31 -7 2 3 1.13 0.25 -6 2 3 65.39 1.04 -5 2 3 1.33 0.17 -4 2 3 50.74 0.78 -3 2 3 364.26 3.89 -2 2 3 1.69 0.12 -1 2 3 85.06 0.96 0 2 3 3.45 0.15 1 2 3 281.42 2.66 2 2 3 2.81 0.16 3 2 3 107.60 1.33 4 2 3 87.44 1.18 5 2 3 0.14 0.13 6 2 3 34.22 0.72 7 2 3 1.07 0.25 8 2 3 20.42 0.83 9 2 3 0.48 0.37 10 2 3 30.07 1.55 11 2 3 19.52 1.52 -11 3 3 4.76 0.84 -10 3 3 0.25 0.48 -9 3 3 8.94 0.66 -8 3 3 76.55 1.49 -7 3 3 24.83 0.76 -6 3 3 25.64 0.62 -5 3 3 115.27 1.55 -4 3 3 23.73 0.50 -3 3 3 0.48 0.10 -2 3 3 0.37 0.08 -1 3 3 515.63 5.55 0 3 3 0.09 0.08 1 3 3 232.57 2.63 2 3 3 35.90 0.54 3 3 3 63.68 0.92 4 3 3 19.69 0.47 5 3 3 34.38 0.70 6 3 3 49.46 1.00 7 3 3 7.08 0.48 8 3 3 43.94 1.13 9 3 3 27.10 1.06 10 3 3 1.80 0.59 11 3 3 0.14 0.52 -11 4 3 7.52 1.05 -10 4 3 47.45 2.11 -9 4 3 1.21 0.40 -8 4 3 2.88 0.37 -7 4 3 1.45 0.28 -6 4 3 51.66 1.01 -5 4 3 15.89 0.44 -4 4 3 19.32 0.41 -3 4 3 145.97 1.67 -2 4 3 1.66 0.16 -1 4 3 23.54 0.42 0 4 3 1.40 0.12 1 4 3 89.52 1.23 2 4 3 0.10 0.09 3 4 3 81.99 1.02 4 4 3 41.99 0.68 5 4 3 2.84 0.24 6 4 3 25.98 0.70 7 4 3 0.41 0.24 8 4 3 26.21 0.92 9 4 3 0.40 0.36 10 4 3 18.77 1.57 11 4 3 26.02 1.53 -11 5 3 12.22 0.99 -10 5 3 1.16 0.48 -9 5 3 0.71 0.36 -8 5 3 62.83 1.34 -7 5 3 0.15 0.20 -6 5 3 34.43 0.75 -5 5 3 32.90 0.67 -4 5 3 6.03 0.30 -3 5 3 33.80 0.62 -2 5 3 16.85 0.41 -1 5 3 187.30 2.03 0 5 3 6.36 0.24 1 5 3 103.47 1.21 2 5 3 35.79 0.58 3 5 3 36.47 0.59 4 5 3 4.90 0.27 5 5 3 1.96 0.21 6 5 3 41.21 0.94 7 5 3 1.00 0.26 8 5 3 34.82 0.97 9 5 3 3.61 0.53 10 5 3 12.94 1.06 11 5 3 11.22 1.21 -11 6 3 2.38 0.66 -10 6 3 62.52 1.70 -9 6 3 2.56 0.44 -8 6 3 14.46 0.71 -7 6 3 4.72 0.43 -6 6 3 47.06 0.97 -5 6 3 3.08 0.29 -4 6 3 22.43 0.57 -3 6 3 147.78 1.80 -2 6 3 2.42 0.12 -1 6 3 9.79 0.30 0 6 3 4.00 0.22 1 6 3 59.83 0.85 2 6 3 1.50 0.13 3 6 3 13.68 0.36 4 6 3 63.62 1.10 5 6 3 6.10 0.34 6 6 3 14.65 0.62 7 6 3 4.49 0.44 8 6 3 33.02 1.15 9 6 3 1.32 0.44 10 6 3 37.09 1.55 -11 7 3 8.65 0.93 -10 7 3 0.57 0.44 -9 7 3 1.36 0.42 -8 7 3 90.98 1.86 -7 7 3 3.16 0.40 -6 7 3 29.01 0.79 -5 7 3 18.82 0.66 -4 7 3 27.34 0.64 -3 7 3 5.67 0.25 -2 7 3 14.07 0.38 -1 7 3 188.41 2.21 0 7 3 2.56 0.19 1 7 3 100.16 1.31 2 7 3 51.69 0.80 3 7 3 46.33 0.75 4 7 3 8.02 0.36 5 7 3 1.85 0.29 6 7 3 54.43 1.21 7 7 3 3.21 0.44 8 7 3 29.81 1.18 9 7 3 12.85 0.85 10 7 3 6.53 0.79 -10 8 3 46.87 1.57 -9 8 3 0.44 0.38 -8 8 3 2.26 0.48 -7 8 3 1.60 0.38 -6 8 3 39.37 1.11 -5 8 3 4.16 0.41 -4 8 3 35.04 0.76 -3 8 3 233.98 2.73 -2 8 3 0.31 0.13 -1 8 3 60.47 0.99 0 8 3 0.45 0.13 1 8 3 158.45 1.95 2 8 3 0.16 0.12 3 8 3 119.99 1.57 4 8 3 57.99 1.01 5 8 3 0.19 0.23 6 8 3 42.18 1.12 7 8 3 0.38 0.36 8 8 3 31.23 1.30 9 8 3 0.27 0.45 10 8 3 22.26 1.36 -10 9 3 0.29 0.43 -9 9 3 8.01 0.80 -8 9 3 63.89 1.78 -7 9 3 2.96 0.46 -6 9 3 19.93 0.87 -5 9 3 73.50 1.49 -4 9 3 28.13 0.79 -3 9 3 0.11 0.12 -2 9 3 1.60 0.18 -1 9 3 287.40 3.29 0 9 3 1.35 0.18 1 9 3 113.64 1.59 2 9 3 36.51 0.70 3 9 3 29.26 0.62 4 9 3 16.69 0.58 5 9 3 16.27 0.73 6 9 3 35.41 1.04 7 9 3 1.19 0.40 8 9 3 36.37 1.52 9 9 3 11.65 0.98 10 9 3 2.89 0.71 -10 10 3 34.61 1.61 -9 10 3 0.33 0.46 -8 10 3 2.96 0.54 -7 10 3 1.48 0.42 -6 10 3 42.20 1.22 -5 10 3 2.64 0.38 -4 10 3 5.57 0.46 -3 10 3 114.48 1.68 -2 10 3 10.43 0.42 -1 10 3 28.87 0.65 0 10 3 8.80 0.38 1 10 3 101.12 1.50 2 10 3 9.79 0.41 3 10 3 38.92 0.87 4 10 3 38.30 1.02 5 10 3 4.60 0.44 6 10 3 9.14 0.61 7 10 3 0.56 0.37 8 10 3 7.72 0.93 9 10 3 0.19 0.46 -9 11 3 0.47 0.47 -8 11 3 52.47 1.69 -7 11 3 0.22 0.36 -6 11 3 21.33 1.00 -5 11 3 28.28 0.98 -4 11 3 2.54 0.37 -3 11 3 25.40 0.80 -2 11 3 1.36 0.23 -1 11 3 90.69 1.36 0 11 3 0.10 0.15 1 11 3 49.93 0.91 2 11 3 12.07 0.50 3 11 3 33.12 0.83 4 11 3 5.85 0.48 5 11 3 3.74 0.43 6 11 3 40.50 1.31 7 11 3 3.26 0.60 8 11 3 31.88 1.73 9 11 3 6.53 0.84 -9 12 3 4.47 0.72 -8 12 3 4.64 0.67 -7 12 3 0.92 0.43 -6 12 3 27.94 1.25 -5 12 3 0.34 0.29 -4 12 3 36.81 1.11 -3 12 3 78.17 1.48 -2 12 3 1.54 0.26 -1 12 3 14.75 0.55 0 12 3 0.36 0.18 1 12 3 50.63 1.00 2 12 3 1.87 0.27 3 12 3 11.82 0.64 4 12 3 49.93 1.26 5 12 3 1.09 0.33 6 12 3 11.51 0.88 7 12 3 2.78 0.58 8 12 3 22.33 1.50 9 12 3 1.86 0.67 -9 13 3 1.19 0.55 -8 13 3 60.82 1.92 -7 13 3 2.00 0.52 -6 13 3 17.69 1.02 -5 13 3 29.52 1.23 -4 13 3 23.38 0.98 -3 13 3 2.11 0.38 -2 13 3 3.33 0.34 -1 13 3 107.57 1.71 0 13 3 12.99 0.54 1 13 3 69.84 1.25 2 13 3 27.14 0.81 3 13 3 6.63 0.52 4 13 3 3.48 0.44 5 13 3 10.29 0.85 6 13 3 33.54 1.46 7 13 3 0.45 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0.01 0.20 7 0 4 75.73 1.78 8 0 4 14.03 0.94 9 0 4 8.04 1.19 10 0 4 34.12 2.48 11 0 4 3.51 1.24 -11 1 4 22.53 1.59 -10 1 4 1.44 0.51 -9 1 4 51.27 1.43 -8 1 4 2.60 0.34 -7 1 4 39.54 0.83 -6 1 4 3.54 0.27 -5 1 4 117.84 1.55 -4 1 4 88.18 1.18 -3 1 4 3.90 0.20 -2 1 4 132.30 1.53 -1 1 4 0.09 0.07 0 1 4 19.43 0.36 1 1 4 35.85 0.51 2 1 4 86.30 1.09 3 1 4 26.66 0.51 4 1 4 18.22 0.46 5 1 4 101.07 1.40 6 1 4 5.98 0.35 7 1 4 0.66 0.22 8 1 4 8.85 0.59 9 1 4 26.15 1.30 10 1 4 6.11 0.94 11 1 4 3.79 0.85 -11 2 4 11.60 1.16 -10 2 4 1.36 0.56 -9 2 4 34.88 1.21 -8 2 4 0.26 0.25 -7 2 4 134.81 1.99 -6 2 4 25.92 0.62 -5 2 4 6.78 0.31 -4 2 4 36.60 0.63 -3 2 4 68.72 0.94 -2 2 4 4.15 0.15 -1 2 4 31.83 0.45 0 2 4 69.16 0.88 1 2 4 0.55 0.12 2 2 4 1.76 0.14 3 2 4 42.07 0.67 4 2 4 48.80 0.79 5 2 4 10.57 0.41 6 2 4 1.56 0.22 7 2 4 78.83 1.36 8 2 4 1.37 0.32 9 2 4 1.46 0.51 10 2 4 33.40 1.84 11 2 4 11.80 1.24 -11 3 4 33.65 1.91 -10 3 4 0.12 0.44 -9 3 4 41.68 1.53 -8 3 4 0.42 0.25 -7 3 4 32.44 0.87 -6 3 4 4.81 0.29 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32.56 0.68 -2 6 5 3.16 0.24 -1 6 5 7.05 0.27 0 6 5 0.44 0.12 1 6 5 9.97 0.36 2 6 5 0.12 0.12 3 6 5 2.22 0.21 4 6 5 125.75 1.65 5 6 5 2.77 0.28 6 6 5 30.56 1.02 7 6 5 4.40 0.52 8 6 5 55.08 1.56 9 6 5 2.36 0.51 10 6 5 16.38 1.09 -10 7 5 5.37 0.63 -9 7 5 0.98 0.39 -8 7 5 66.80 1.58 -7 7 5 0.23 0.27 -6 7 5 16.69 0.83 -5 7 5 55.91 1.22 -4 7 5 33.67 0.73 -3 7 5 11.03 0.43 -2 7 5 24.09 0.59 -1 7 5 122.56 1.57 0 7 5 11.46 0.38 1 7 5 38.17 0.72 2 7 5 92.16 1.35 3 7 5 13.32 0.46 4 7 5 4.60 0.33 5 7 5 0.88 0.22 6 7 5 113.25 2.14 7 7 5 0.31 0.30 8 7 5 44.40 1.41 9 7 5 11.37 0.84 10 7 5 9.86 0.89 -10 8 5 36.71 1.54 -9 8 5 0.58 0.40 -8 8 5 0.57 0.38 -7 8 5 5.81 0.58 -6 8 5 74.86 1.67 -5 8 5 4.50 0.40 -4 8 5 6.03 0.42 -3 8 5 153.05 2.07 -2 8 5 13.00 0.48 -1 8 5 0.49 0.13 0 8 5 13.70 0.43 1 8 5 63.76 0.97 2 8 5 0.24 0.14 3 8 5 29.06 0.67 4 8 5 146.57 2.16 5 8 5 1.21 0.32 6 8 5 40.60 1.26 7 8 5 1.03 0.38 8 8 5 24.71 1.18 9 8 5 1.12 0.49 10 8 5 16.79 1.23 -10 9 5 1.75 0.63 -9 9 5 2.53 0.56 -8 9 5 60.15 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6 6 16 0.69 0.60 -7 7 16 14.25 1.08 -6 7 16 12.38 1.05 -5 7 16 1.26 0.53 -4 7 16 45.22 1.98 -3 7 16 0.27 0.41 -2 7 16 0.28 0.41 -1 7 16 26.93 1.24 0 7 16 42.70 1.47 1 7 16 0.26 0.41 2 7 16 3.33 0.68 3 7 16 51.58 1.76 4 7 16 0.49 0.47 5 7 16 9.30 0.89 -7 8 16 1.72 0.70 -6 8 16 41.89 1.86 -5 8 16 1.62 0.63 -4 8 16 0.98 0.56 -3 8 16 4.73 0.66 -2 8 16 37.37 1.44 -1 8 16 0.13 0.36 0 8 16 3.16 0.57 1 8 16 41.36 1.75 2 8 16 0.29 0.53 3 8 16 2.64 0.68 4 8 16 1.84 0.60 5 8 16 19.71 1.46 -6 9 16 2.27 0.75 -5 9 16 1.52 0.68 -4 9 16 33.39 1.72 -3 9 16 0.20 0.42 -2 9 16 0.38 0.42 -1 9 16 24.65 1.23 0 9 16 13.90 0.96 1 9 16 0.91 0.48 2 9 16 0.10 0.54 3 9 16 42.90 1.93 4 9 16 0.65 0.55 5 9 16 4.22 0.99 -6 10 16 16.84 1.44 -5 10 16 1.63 0.65 -4 10 16 2.12 0.70 -3 10 16 0.41 0.53 -2 10 16 50.01 1.67 -1 10 16 2.88 0.57 0 10 16 7.36 0.78 1 10 16 33.05 1.53 2 10 16 7.46 0.94 3 10 16 0.56 0.59 4 10 16 0.06 0.52 -5 11 16 0.31 0.58 -4 11 16 45.03 2.06 -3 11 16 0.22 0.51 -2 11 16 0.11 0.43 -1 11 16 15.84 1.04 0 11 16 33.23 1.49 1 11 16 0.15 0.48 2 11 16 8.30 1.00 3 11 16 53.23 2.11 4 11 16 1.73 0.84 -5 12 16 2.85 2.68 -4 12 16 7.09 0.96 -3 12 16 2.79 0.74 -2 12 16 40.09 1.82 -1 12 16 0.91 0.51 0 12 16 1.84 0.58 1 12 16 36.80 1.68 2 12 16 5.52 0.80 3 12 16 0.94 0.65 -4 13 16 34.08 5.69 -3 13 16 0.25 0.53 -2 13 16 0.40 0.53 -1 13 16 20.67 1.23 0 13 16 19.15 1.25 1 13 16 0.73 0.56 2 13 16 1.80 0.61 -2 14 16 21.40 1.42 -1 14 16 0.85 0.68 0 14 16 2.33 0.64 -7 0 17 21.89 1.73 -6 0 17 5.74 0.87 -5 0 17 22.55 1.40 -4 0 17 3.19 0.80 -3 0 17 59.16 3.05 -2 0 17 4.74 0.81 -1 0 17 1.15 0.60 0 0 17 2.91 0.73 1 0 17 0.36 0.59 2 0 17 41.08 2.29 3 0 17 0.48 0.56 4 0 17 36.67 1.99 5 0 17 21.39 1.79 6 0 17 10.03 1.38 -7 1 17 34.03 1.41 -6 1 17 6.97 0.64 -5 1 17 26.39 1.15 -4 1 17 0.77 0.48 -3 1 17 20.18 1.19 -2 1 17 0.74 0.38 -1 1 17 17.96 1.00 0 1 17 32.62 1.28 1 1 17 0.39 0.42 2 1 17 27.95 1.27 3 1 17 6.95 0.72 4 1 17 19.77 1.08 5 1 17 3.46 0.65 6 1 17 37.52 1.70 -7 2 17 0.67 0.51 -6 2 17 4.13 0.64 -5 2 17 65.21 1.71 -4 2 17 0.22 0.39 -3 2 17 45.10 1.47 -2 2 17 7.68 0.78 -1 2 17 6.98 0.68 0 2 17 6.67 0.69 1 2 17 13.42 0.95 2 2 17 53.43 1.63 3 2 17 0.50 0.43 4 2 17 52.83 1.74 5 2 17 3.35 0.66 6 2 17 1.96 0.67 -7 3 17 33.39 1.66 -6 3 17 4.88 0.68 -5 3 17 10.83 0.88 -4 3 17 2.96 0.54 -3 3 17 47.77 1.51 -2 3 17 0.26 0.40 -1 3 17 23.24 1.36 0 3 17 26.04 1.26 1 3 17 1.07 0.42 2 3 17 27.14 1.26 3 3 17 0.02 0.40 4 3 17 22.54 1.23 5 3 17 1.53 0.57 6 3 17 48.28 1.82 -7 4 17 1.81 0.75 -6 4 17 3.83 0.83 -5 4 17 37.88 1.51 -4 4 17 0.69 0.42 -3 4 17 36.92 1.42 -2 4 17 15.07 1.11 -1 4 17 2.38 0.62 0 4 17 3.37 0.66 1 4 17 3.03 0.54 2 4 17 31.04 1.36 3 4 17 1.09 0.50 4 4 17 40.08 1.71 5 4 17 3.45 0.72 -7 5 17 35.86 1.73 -6 5 17 3.85 0.74 -5 5 17 24.24 1.36 -4 5 17 0.32 0.42 -3 5 17 10.17 0.85 -2 5 17 0.16 0.39 -1 5 17 28.36 1.51 0 5 17 20.71 1.22 1 5 17 0.09 0.41 2 5 17 28.71 1.31 3 5 17 7.06 0.81 4 5 17 15.89 1.11 5 5 17 0.69 0.56 -7 6 17 13.57 1.15 -6 6 17 7.72 0.91 -5 6 17 32.28 1.60 -4 6 17 0.52 0.48 -3 6 17 38.11 1.51 -2 6 17 5.76 0.70 -1 6 17 0.25 0.51 0 6 17 2.30 0.59 1 6 17 0.40 0.51 2 6 17 41.11 1.70 3 6 17 0.39 0.47 4 6 17 31.47 1.54 5 6 17 11.45 1.03 -6 7 17 3.28 0.71 -5 7 17 17.53 1.30 -4 7 17 1.98 0.66 -3 7 17 16.73 1.09 -2 7 17 0.30 0.42 -1 7 17 12.08 0.94 0 7 17 18.28 1.18 1 7 17 0.70 0.55 2 7 17 21.81 1.32 3 7 17 1.74 0.69 4 7 17 22.48 1.32 5 7 17 1.10 0.58 -6 8 17 3.06 0.77 -5 8 17 51.91 2.15 -4 8 17 1.29 0.61 -3 8 17 39.65 1.67 -2 8 17 6.31 0.76 -1 8 17 10.11 0.84 0 8 17 1.36 0.56 1 8 17 14.89 1.12 2 8 17 38.84 1.89 3 8 17 0.07 0.54 4 8 17 47.10 2.00 -6 9 17 7.02 1.14 -5 9 17 9.02 1.05 -4 9 17 0.57 0.57 -3 9 17 36.77 1.82 -2 9 17 0.35 0.47 -1 9 17 26.51 1.32 0 9 17 34.15 1.49 1 9 17 0.81 0.56 2 9 17 28.08 1.64 3 9 17 0.41 0.57 4 9 17 12.98 1.20 -5 10 17 27.93 1.65 -4 10 17 0.33 0.60 -3 10 17 32.80 1.75 -2 10 17 8.48 0.83 -1 10 17 0.65 0.48 0 10 17 9.23 0.86 1 10 17 1.38 0.67 2 10 17 24.03 1.52 3 10 17 0.58 0.59 -4 11 17 0.84 0.57 -3 11 17 10.33 1.13 -2 11 17 0.13 0.52 -1 11 17 8.83 0.85 0 11 17 12.88 1.01 1 11 17 1.57 0.67 2 11 17 21.54 1.46 3 11 17 1.45 1.24 -3 12 17 29.58 1.71 -2 12 17 4.84 0.83 -1 12 17 0.36 0.49 0 12 17 1.21 0.61 1 12 17 1.28 0.60 2 12 17 32.91 3.61 -1 13 17 15.55 1.27 -7 0 18 1.03 0.74 -6 0 18 28.91 1.69 -5 0 18 0.00 0.83 -4 0 18 2.96 1.05 -3 0 18 0.87 0.93 -2 0 18 117.52 3.55 -1 0 18 15.33 1.35 0 0 18 4.81 0.89 1 0 18 51.81 2.53 2 0 18 7.34 1.17 3 0 18 0.08 0.63 4 0 18 0.99 0.73 5 0 18 38.46 2.41 -7 1 18 9.13 0.90 -6 1 18 7.29 0.72 -5 1 18 0.08 0.50 -4 1 18 75.27 2.59 -3 1 18 4.59 0.83 -2 1 18 0.13 0.42 -1 1 18 21.63 1.12 0 1 18 32.22 1.44 1 1 18 14.81 1.01 2 1 18 1.30 0.52 3 1 18 55.80 1.84 4 1 18 0.56 0.49 5 1 18 2.82 0.69 -7 2 18 0.59 0.56 -6 2 18 55.47 2.25 -5 2 18 0.73 0.56 -4 2 18 0.77 0.63 -3 2 18 0.93 0.50 -2 2 18 32.63 1.51 -1 2 18 16.43 1.20 0 2 18 4.82 0.67 1 2 18 30.35 1.43 2 2 18 0.74 0.50 3 2 18 1.94 0.60 4 2 18 4.02 0.72 5 2 18 24.58 1.36 -7 3 18 16.35 1.45 -6 3 18 3.64 0.82 -5 3 18 0.45 0.54 -4 3 18 62.20 1.83 -3 3 18 4.48 0.72 -2 3 18 6.57 0.84 -1 3 18 9.74 0.95 0 3 18 8.63 0.89 1 3 18 4.38 0.67 2 3 18 0.82 0.44 3 3 18 46.43 1.77 4 3 18 0.40 0.52 5 3 18 0.28 0.58 -6 4 18 30.19 1.79 -5 4 18 0.53 0.53 -4 4 18 0.77 0.48 -3 4 18 1.28 0.57 -2 4 18 47.53 1.91 -1 4 18 20.09 1.31 0 4 18 5.65 0.79 1 4 18 42.06 1.77 2 4 18 0.62 0.44 3 4 18 2.10 0.58 4 4 18 2.24 0.68 5 4 18 33.60 1.72 -6 5 18 6.09 0.97 -5 5 18 0.49 0.54 -4 5 18 64.11 1.99 -3 5 18 2.89 0.63 -2 5 18 1.31 0.59 -1 5 18 7.70 0.90 0 5 18 37.87 1.78 1 5 18 14.09 1.14 2 5 18 2.58 0.64 3 5 18 34.88 1.59 4 5 18 0.73 0.56 -6 6 18 33.09 1.68 -5 6 18 0.02 0.55 -4 6 18 6.92 0.80 -3 6 18 1.36 0.54 -2 6 18 63.67 2.20 -1 6 18 22.81 1.42 0 6 18 3.51 0.73 1 6 18 28.73 1.60 2 6 18 5.08 0.80 3 6 18 0.11 0.50 4 6 18 0.44 0.54 -6 7 18 15.23 4.29 -5 7 18 0.32 0.60 -4 7 18 47.00 2.10 -3 7 18 3.30 0.67 -2 7 18 1.61 0.54 -1 7 18 17.49 1.27 0 7 18 21.97 1.40 1 7 18 5.72 0.82 2 7 18 0.59 0.55 3 7 18 57.48 2.22 4 7 18 0.59 0.62 -5 8 18 0.17 0.57 -4 8 18 3.20 0.80 -3 8 18 1.13 0.56 -2 8 18 41.96 1.77 -1 8 18 9.02 0.99 0 8 18 3.70 0.74 1 8 18 29.39 1.57 2 8 18 0.49 0.58 3 8 18 1.84 0.74 -4 9 18 48.17 2.07 -3 9 18 2.03 0.70 -2 9 18 2.20 0.60 -1 9 18 5.80 0.86 0 9 18 11.20 1.04 1 9 18 8.03 0.98 2 9 18 0.22 0.58 3 9 18 40.15 2.03 -4 10 18 0.38 0.65 -3 10 18 0.70 0.59 -2 10 18 36.38 1.66 -1 10 18 13.77 1.08 0 10 18 4.69 0.81 1 10 18 26.61 1.63 2 10 18 0.32 0.62 -3 11 18 1.25 0.72 -2 11 18 0.54 0.58 -1 11 18 6.69 0.80 0 11 18 24.22 1.58 1 11 18 12.95 1.23 -6 0 19 1.65 2.48 -5 0 19 34.43 3.21 -4 0 19 0.00 2.76 -3 0 19 1.63 2.31 -2 0 19 28.31 2.95 -1 0 19 4.75 1.62 0 0 19 4.70 2.26 1 0 19 11.56 2.04 2 0 19 34.36 2.74 3 0 19 0.00 2.41 4 0 19 10.23 2.22 -6 1 19 0.14 2.01 -5 1 19 2.05 1.40 -4 1 19 0.00 1.56 -3 1 19 40.72 2.16 -2 1 19 0.00 1.99 -1 1 19 11.68 1.54 0 1 19 43.85 1.90 1 1 19 0.04 1.61 2 1 19 19.23 1.52 3 1 19 0.42 1.20 4 1 19 9.64 1.52 -6 2 19 6.41 2.01 -5 2 19 47.90 2.41 -4 2 19 3.59 1.86 -3 2 19 9.31 1.85 -2 2 19 29.56 1.82 -1 2 19 29.43 2.17 0 2 19 3.64 1.67 1 2 19 21.10 1.61 2 2 19 27.60 1.72 3 2 19 0.55 1.80 4 2 19 27.33 1.86 -6 3 19 0.00 1.64 -5 3 19 1.92 1.44 -4 3 19 4.16 1.77 -3 3 19 56.76 2.42 -2 3 19 0.98 1.66 -1 3 19 15.36 1.72 0 3 19 34.32 1.89 1 3 19 7.79 2.18 2 3 19 18.70 1.56 3 3 19 1.83 1.23 4 3 19 9.77 1.45 -5 4 19 38.41 2.33 -4 4 19 2.66 1.74 -3 4 19 4.51 1.48 -2 4 19 38.73 2.10 -1 4 19 18.48 1.83 0 4 19 7.41 1.90 1 4 19 14.36 1.58 2 4 19 32.46 1.96 3 4 19 6.36 1.77 4 4 19 13.95 1.19 -5 5 19 2.37 1.52 -4 5 19 0.70 1.51 -3 5 19 26.43 1.79 -2 5 19 3.42 1.61 -1 5 19 10.95 1.59 0 5 19 24.50 1.79 1 5 19 0.00 1.57 2 5 19 19.31 1.65 3 5 19 0.37 1.35 -5 6 19 29.38 1.96 -4 6 19 1.05 1.62 -3 6 19 13.87 1.55 -2 6 19 26.27 1.84 -1 6 19 7.22 1.49 0 6 19 3.02 1.67 1 6 19 0.88 1.48 2 6 19 21.38 1.74 3 6 19 0.00 1.73 -4 7 19 0.00 1.45 -3 7 19 31.84 2.07 -2 7 19 0.00 1.71 -1 7 19 9.69 1.62 0 7 19 34.10 1.98 1 7 19 9.01 1.93 2 7 19 12.40 1.60 -4 8 19 0.74 1.84 -3 8 19 4.85 2.09 -2 8 19 14.83 1.63 -1 8 19 26.23 2.21 0 8 19 2.87 1.54 1 8 19 22.77 1.97 2 8 19 28.77 1.99 -3 9 19 51.99 2.44 -2 9 19 0.00 1.81 -1 9 19 11.94 1.75 0 9 19 38.84 2.11 1 9 19 0.00 2.08 -1 10 19 9.93 3.60 -5 0 20 1.16 1.68 -4 0 20 4.39 1.79 -3 0 20 3.82 3.03 -2 0 20 41.18 3.25 -1 0 20 9.30 2.55 0 0 20 7.98 2.47 1 0 20 44.36 2.88 2 0 20 3.42 1.51 3 0 20 0.00 1.33 -5 1 20 1.31 2.03 -4 1 20 42.11 2.12 -3 1 20 4.46 1.27 -2 1 20 2.11 1.32 -1 1 20 17.58 1.62 0 1 20 11.81 1.30 1 1 20 4.54 1.09 2 1 20 0.48 1.56 3 1 20 46.54 2.00 -5 2 20 1.41 1.15 -4 2 20 0.34 1.13 -3 2 20 4.52 1.95 -2 2 20 25.79 1.78 -1 2 20 10.64 1.38 0 2 20 0.29 1.41 1 2 20 37.65 2.02 2 2 20 1.03 1.09 3 2 20 0.33 0.98 -4 3 20 63.88 2.74 -3 3 20 3.54 1.22 -2 3 20 4.57 0.98 -1 3 20 13.76 1.50 0 3 20 0.00 0.97 1 3 20 2.77 1.10 2 3 20 0.00 2.09 -4 4 20 5.20 1.25 -3 4 20 0.00 1.40 -2 4 20 19.30 1.51 -1 4 20 10.29 1.39 0 4 20 3.84 1.41 1 4 20 26.41 1.64 2 4 20 0.00 1.12 -4 5 20 25.80 1.61 -3 5 20 4.69 1.13 -2 5 20 0.00 1.10 -1 5 20 14.08 1.58 0 5 20 11.20 1.24 1 5 20 1.94 1.13 2 5 20 0.20 1.44 -3 6 20 0.00 1.73 -2 6 20 45.23 2.04 -1 6 20 7.36 1.32 0 6 20 0.00 1.74 1 6 20 42.53 2.03 -2 7 20 2.50 1.13 -1 7 20 14.22 1.63 0 7 20 6.84 1.21 -3 0 21 26.26 2.81 -2 0 21 9.11 2.58 -1 0 21 9.77 3.00 0 0 21 0.57 2.53 1 0 21 0.00 2.06 -3 1 21 13.23 1.83 -2 1 21 4.81 2.09 -1 1 21 15.42 2.23 0 1 21 31.06 2.04 1 1 21 4.68 1.53 -3 2 21 8.20 1.69 -2 2 21 21.06 1.93 -1 2 21 10.39 1.49 0 2 21 0.00 1.57 1 2 21 6.36 1.50 -2 3 21 2.62 1.92 -1 3 21 14.21 1.70 0 3 21 24.03 1.84 -2 4 21 15.16 1.52 -1 4 21 7.79 1.46 0 4 21 0.00 1.40 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 87498 _symmetry_cell_setting monoclinic _symmetry_space_group_name_h-m 'P 21/m' _symmetry_int_tables_number 11 _chemical_absolute_configuration ? _database_code_depnum_ccdc_archive 'CCDC 967161' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound_8 _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety '(C7 H11 N2 1+)2, (U O3 C4 H2 N4 S4 2-)' _chemical_formula_sum 'C18 H24 N8 O3 S4 U' _exptl_crystal_recrystallization_method 'Slow Aqueous Evaporation' _chemical_melting_point ? _exptl_crystal_description Prism _exptl_crystal_colour Yellow _diffrn_ambient_temperature 100(2) _chemical_formula_weight 766.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.3879(15) _cell_length_b 8.6863(10) _cell_length_c 23.486(3) _cell_angle_alpha 90 _cell_angle_beta 98.3050(10) _cell_angle_gamma 90 _cell_volume 2702.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3807 _cell_measurement_theta_min 5.608 _cell_measurement_theta_max 60.667 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.879 _exptl_crystal_F_000 1464 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.387 _exptl_crystal_size_mid 0.285 _exptl_crystal_size_min 0.239 _exptl_absorpt_coefficient_mu 6.350 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4844 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_process_details 'SADABS, G. Sheldrick (1999)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focused sealed X-ray tube' _diffrn_measurement_device_type 'Bruker ApexII CCD' _diffrn_measurement_method 'Omega and Phi Scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14446 _diffrn_reflns_av_unetI/netI 0.0171 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.753 _diffrn_reflns_theta_max 30.334 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.936 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.936 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.936 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 3807 _reflns_number_gt 3756 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'APEX II (Bruker AXS, 2013)' _computing_cell_refinement 'SAINT (Bruker AXS, 2013)' _computing_data_reduction 'SAINT (Bruker AXS, 2013)' _computing_structure_solution 'SIR92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Crystal Maker v.8.2.2 (Palmer 2009)' _computing_publication_material 'WINGX (Farrugia, 2012)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0084P)^2^+4.5197P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3807 _refine_ls_number_parameters 157 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0156 _refine_ls_R_factor_gt 0.0151 _refine_ls_wR_factor_ref 0.0347 _refine_ls_wR_factor_gt 0.0345 _refine_ls_goodness_of_fit_ref 1.215 _refine_ls_restrained_S_all 1.215 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.59414(13) 0.45871(19) 0.38868(8) 0.0135(3) Uani 1 1 d . . . . . C2 C 0.41103(13) -0.0071(2) 0.17340(7) 0.0158(3) Uani 1 1 d . . . . . C3 C 0.63295(16) -0.1886(2) 0.55468(9) 0.0225(4) Uani 1 1 d . . . . . H3 H 0.6316 -0.2946 0.5601 0.027 Uiso 1 1 calc R U . . . C4 C 0.64323(15) -0.0940(2) 0.60149(8) 0.0191(4) Uani 1 1 d . . . . . H4 H 0.6482 -0.1353 0.6383 0.023 Uiso 1 1 calc R U . . . C5 C 0.64628(13) 0.0688(2) 0.59365(8) 0.0155(3) Uani 1 1 d . . . . . C6 C 0.63364(14) 0.1225(2) 0.53581(8) 0.0191(4) Uani 1 1 d . . . . . H6 H 0.6321 0.2278 0.5284 0.023 Uiso 1 1 calc R U . . . C7 C 0.62385(15) 0.0214(2) 0.49144(8) 0.0224(4) Uani 1 1 d . . . . . H7 H 0.6164 0.0585 0.4539 0.027 Uiso 1 1 calc R U . . . C8 C 0.67583(16) 0.1067(3) 0.69730(9) 0.0285(5) Uani 1 1 d . . . . . H8A H 0.6926 0.1905 0.7236 0.043 Uiso 1 1 calc R U . . . H8B H 0.7300 0.0334 0.7016 0.043 Uiso 1 1 calc R U . . . H8C H 0.6152 0.0578 0.7054 0.043 Uiso 1 1 calc R U . . . C9 C 0.66288(19) 0.3319(3) 0.62931(12) 0.0330(5) Uani 1 1 d . . . . . H9A H 0.6718 0.3835 0.6658 0.049 Uiso 1 1 calc R U . . . H9B H 0.6006 0.3646 0.6071 0.049 Uiso 1 1 calc R U . . . H9C H 0.7180 0.3570 0.6090 0.049 Uiso 1 1 calc R U . . . N1 N 0.59219(12) 0.43326(18) 0.33982(7) 0.0172(3) Uani 1 1 d . . . . . N2 N 0.43685(13) 0.11114(19) 0.19394(7) 0.0213(3) Uani 1 1 d . . . . . N3 N 0.62462(13) -0.1319(2) 0.50058(7) 0.0218(3) Uani 1 1 d . . . . . H3A H 0.6198 -0.1940 0.4718 0.026 Uiso 1 1 calc R U . . . N4 N 0.66019(12) 0.1653(2) 0.63840(7) 0.0209(3) Uani 1 1 d . . . . . O1 O 0.61064(10) 0.33494(16) 0.21682(6) 0.0191(3) Uani 1 1 d . . . . . OW1 O 0.5000 0.6216(2) 0.2500 0.0255(4) Uani 1 2 d S T P . . S1 S 0.59470(4) 0.49528(6) 0.45655(2) 0.02296(10) Uani 1 1 d . . . . . S2 S 0.37640(4) -0.17429(5) 0.14580(2) 0.01942(9) Uani 1 1 d . . . . . U1 U 0.5000 0.33647(2) 0.2500 0.01077(3) Uani 1 2 d S T P . . 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 0.0135(7) 0.0100(7) 0.0170(8) 0.0015(6) 0.0021(6) 0.0002(6) C2 0.0182(8) 0.0146(8) 0.0133(7) 0.0025(6) -0.0027(6) 0.0013(7) C3 0.0243(9) 0.0170(9) 0.0261(10) 0.0015(7) 0.0029(8) 0.0004(7) C4 0.0206(9) 0.0196(9) 0.0171(8) 0.0038(7) 0.0030(7) 0.0010(7) C5 0.0110(7) 0.0187(8) 0.0169(8) -0.0008(6) 0.0019(6) 0.0006(6) C6 0.0188(8) 0.0175(8) 0.0205(9) 0.0052(7) 0.0018(7) 0.0011(7) C7 0.0217(9) 0.0297(10) 0.0154(8) 0.0041(7) 0.0014(7) 0.0017(8) C8 0.0198(9) 0.0494(14) 0.0164(9) -0.0085(9) 0.0024(7) -0.0037(9) C9 0.0300(11) 0.0242(11) 0.0452(14) -0.0127(10) 0.0073(10) -0.0046(9) N1 0.0216(8) 0.0129(7) 0.0165(7) -0.0003(5) 0.0011(6) 0.0014(6) N2 0.0268(9) 0.0138(7) 0.0208(8) -0.0005(6) -0.0053(7) -0.0016(6) N3 0.0218(8) 0.0254(8) 0.0178(8) -0.0062(6) 0.0013(6) 0.0008(6) N4 0.0159(7) 0.0254(8) 0.0213(8) -0.0071(7) 0.0026(6) -0.0008(6) O1 0.0163(6) 0.0236(7) 0.0178(6) -0.0053(5) 0.0038(5) -0.0011(5) OW1 0.0419(13) 0.0140(9) 0.0177(9) 0.000 -0.0055(9) 0.000 S1 0.0382(3) 0.0192(2) 0.01256(19) 0.00144(17) 0.00715(18) 0.0015(2) S2 0.0295(2) 0.01181(19) 0.01518(19) -0.00314(15) -0.00259(17) -0.00312(17) U1 0.01284(4) 0.00821(4) 0.01112(4) 0.000 0.00132(3) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.165(2) . ? C1 S1 1.6242(18) . ? C2 N2 1.165(2) . ? C2 S2 1.6305(19) . ? C3 N3 1.352(3) . ? C3 C4 1.363(3) . ? C3 H3 0.9300 . ? C4 C5 1.428(3) . ? C4 H4 0.9300 . ? C5 N4 1.336(2) . ? C5 C6 1.423(3) . ? C6 C7 1.355(3) . ? C6 H6 0.9300 . ? C7 N3 1.349(3) . ? C7 H7 0.9300 . ? C8 N4 1.461(3) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 N4 1.464(3) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? N1 U1 2.4348(16) . ? N2 U1 2.4409(16) . ? N3 H3A 0.8600 . ? O1 U1 1.7707(13) . ? OW1 U1 2.476(2) . ? U1 O1 1.7706(13) 2_655 ? U1 N1 2.4348(16) 2_655 ? U1 N2 2.4408(16) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 S1 178.94(17) . . ? N2 C2 S2 178.78(18) . . ? N3 C3 C4 121.56(18) . . ? N3 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C3 C4 C5 119.63(18) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? N4 C5 C6 121.94(18) . . ? N4 C5 C4 121.55(18) . . ? C6 C5 C4 116.50(17) . . ? C7 C6 C5 120.46(18) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? N3 C7 C6 121.33(18) . . ? N3 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? N4 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N4 C9 H9A 109.5 . . ? N4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 N1 U1 148.78(14) . . ? C2 N2 U1 171.36(15) . . ? C7 N3 C3 120.45(17) . . ? C7 N3 H3A 119.8 . . ? C3 N3 H3A 119.8 . . ? C5 N4 C8 120.74(18) . . ? C5 N4 C9 120.59(18) . . ? C8 N4 C9 118.65(18) . . ? O1 U1 O1 179.14(9) 2_655 . ? O1 U1 N1 91.85(6) 2_655 2_655 ? O1 U1 N1 88.45(6) . 2_655 ? O1 U1 N1 88.45(6) 2_655 . ? O1 U1 N1 91.85(6) . . ? N1 U1 N1 139.60(7) 2_655 . ? O1 U1 N2 90.18(6) 2_655 2_655 ? O1 U1 N2 89.13(6) . 2_655 ? N1 U1 N2 146.82(5) 2_655 2_655 ? N1 U1 N2 73.55(5) . 2_655 ? O1 U1 N2 89.13(6) 2_655 . ? O1 U1 N2 90.18(6) . . ? N1 U1 N2 73.55(5) 2_655 . ? N1 U1 N2 146.83(5) . . ? N2 U1 N2 73.38(8) 2_655 . ? O1 U1 OW1 90.43(4) 2_655 . ? O1 U1 OW1 90.43(4) . . ? N1 U1 OW1 69.80(4) 2_655 . ? N1 U1 OW1 69.80(4) . . ? N2 U1 OW1 143.31(4) 2_655 . ? N2 U1 OW1 143.31(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C3 H3 S1 0.93 3.02 3.574(2) 119.5 1_545 C4 H4 O1 0.93 2.63 3.500(2) 155.6 6_556 C6 H6 S1 0.93 2.87 3.734(2) 154.4 . C8 H8B N1 0.96 2.71 3.363(3) 125.5 7_656 N3 H3A S1 0.86 2.74 3.4056(18) 135.7 1_545 N3 H3A S2 0.86 2.78 3.4556(18) 137.2 2_655 _refine_diff_density_max 0.714 _refine_diff_density_min -1.508 _refine_diff_density_rms 0.081 _shelxl_version_number 2013-4 _shelx_res_file ; TITL C2onc in C2/c CELL 0.71073 13.3879 8.6863 23.4861 90.000 98.305 90.000 ZERR 4.00 0.0015 0.0010 0.0027 0.000 0.001 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O S U UNIT 72 88 32 12 16 4 MERG 2 EQIV $1 x, y-1, z HTAB C3 S1_$1 EQIV $2 x, -y, z+1/2 HTAB C4 O1_$2 HTAB C6 S1 EQIV $3 -x+3/2, -y+1/2, -z+1 HTAB C8 N1_$3 HTAB N3 S1_$1 EQIV $4 -x+1, y, -z+1/2 HTAB N3 S2_$4 FMAP 2 PLAN 25 ACTA 50.00 HTAB 2.00000 BOND $H L.S. 12 WGHT 0.008400 4.519700 FVAR 0.04918 C1 1 0.594138 0.458712 0.388680 11.00000 0.01350 0.00999 = 0.01695 0.00154 0.00206 0.00017 C2 1 0.411034 -0.007061 0.173403 11.00000 0.01824 0.01458 = 0.01326 0.00254 -0.00273 0.00130 C3 1 0.632950 -0.188576 0.554684 11.00000 0.02429 0.01704 = 0.02611 0.00148 0.00293 0.00040 AFIX 43 H3 2 0.631634 -0.294578 0.560093 11.00000 -1.20000 AFIX 0 C4 1 0.643232 -0.093989 0.601494 11.00000 0.02062 0.01955 = 0.01711 0.00382 0.00296 0.00097 AFIX 43 H4 2 0.648231 -0.135305 0.638327 11.00000 -1.20000 AFIX 0 C5 1 0.646283 0.068840 0.593646 11.00000 0.01097 0.01870 = 0.01689 -0.00075 0.00189 0.00064 C6 1 0.633643 0.122534 0.535812 11.00000 0.01881 0.01754 = 0.02052 0.00516 0.00176 0.00114 AFIX 43 H6 2 0.632094 0.227758 0.528426 11.00000 -1.20000 AFIX 0 C7 1 0.623852 0.021444 0.491440 11.00000 0.02174 0.02965 = 0.01542 0.00409 0.00141 0.00170 AFIX 43 H7 2 0.616450 0.058504 0.453916 11.00000 -1.20000 AFIX 0 C8 1 0.675833 0.106738 0.697302 11.00000 0.01977 0.04939 = 0.01642 -0.00848 0.00239 -0.00375 AFIX 137 H8A 2 0.692555 0.190546 0.723600 11.00000 -1.50000 H8B 2 0.730040 0.033392 0.701585 11.00000 -1.50000 H8C 2 0.615185 0.057759 0.705439 11.00000 -1.50000 AFIX 0 C9 1 0.662879 0.331917 0.629309 11.00000 0.03004 0.02416 = 0.04523 -0.01267 0.00729 -0.00464 AFIX 137 H9A 2 0.671809 0.383478 0.665846 11.00000 -1.50000 H9B 2 0.600588 0.364562 0.607137 11.00000 -1.50000 H9C 2 0.718004 0.356958 0.608985 11.00000 -1.50000 AFIX 0 N1 3 0.592194 0.433265 0.339820 11.00000 0.02164 0.01294 = 0.01646 -0.00029 0.00113 0.00141 N2 3 0.436852 0.111137 0.193938 11.00000 0.02680 0.01381 = 0.02077 -0.00054 -0.00526 -0.00164 N3 3 0.624620 -0.131898 0.500580 11.00000 0.02182 0.02538 = 0.01783 -0.00625 0.00132 0.00075 AFIX 43 H3A 2 0.619780 -0.194031 0.471803 11.00000 -1.20000 AFIX 0 N4 3 0.660190 0.165337 0.638397 11.00000 0.01594 0.02539 = 0.02130 -0.00706 0.00265 -0.00077 O1 4 0.610645 0.334937 0.216818 11.00000 0.01632 0.02363 = 0.01776 -0.00530 0.00377 -0.00114 OW1 4 0.500000 0.621557 0.250000 10.50000 0.04190 0.01401 = 0.01769 0.00000 -0.00549 0.00000 S1 5 0.594698 0.495279 0.456546 11.00000 0.03820 0.01916 = 0.01256 0.00144 0.00715 0.00150 S2 5 0.376399 -0.174293 0.145800 11.00000 0.02954 0.01181 = 0.01518 -0.00314 -0.00259 -0.00312 U1 6 0.500000 0.336471 0.250000 10.50000 0.01284 0.00821 = 0.01112 0.00000 0.00132 0.00000 HKLF 4 REM C2onc in C2/c REM R1 = 0.0151 for 3756 Fo > 4sig(Fo) and 0.0156 for all 3807 data REM 157 parameters refined using 0 restraints END WGHT 0.0084 4.4524 REM Instructions for potential hydrogen bonds HTAB C3 S1_$1 HTAB C4 O1_$2 HTAB C6 S1 HTAB N3 S1_$1 HTAB N3 S2_$4 REM Highest difference peak 0.714, deepest hole -1.508, 1-sigma level 0.081 Q1 1 0.5506 0.2736 0.2526 11.00000 0.05 0.71 Q2 1 0.5278 0.6797 0.2798 11.00000 0.05 0.69 Q3 1 0.5000 0.6943 0.2500 10.50000 0.05 0.65 Q4 1 0.5184 0.2865 0.2258 11.00000 0.05 0.55 Q5 1 0.5531 0.4000 0.2505 11.00000 0.05 0.46 Q6 1 0.5353 0.5966 0.2465 11.00000 0.05 0.41 Q7 1 0.5827 0.3775 0.2419 11.00000 0.05 0.40 Q8 1 0.4980 0.0426 0.2325 11.00000 0.05 0.34 Q9 1 0.6322 -0.1409 0.5794 11.00000 0.05 0.33 Q10 1 0.6352 0.0855 0.5632 11.00000 0.05 0.32 Q11 1 0.3967 -0.2015 0.1112 11.00000 0.05 0.32 Q12 1 0.5624 0.3405 0.2098 11.00000 0.05 0.31 Q13 1 0.6292 0.0578 0.5183 11.00000 0.05 0.31 Q14 1 0.6658 -0.0289 0.5971 11.00000 0.05 0.29 Q15 1 0.6673 0.1182 0.6204 11.00000 0.05 0.28 Q16 1 0.6343 -0.1548 0.5288 11.00000 0.05 0.27 Q17 1 0.6387 0.2983 0.2255 11.00000 0.05 0.26 Q18 1 0.3877 0.0630 0.1870 11.00000 0.05 0.26 Q19 1 0.6381 0.4642 0.5397 11.00000 0.05 0.25 Q20 1 0.5152 0.3932 0.2205 11.00000 0.05 0.25 Q21 1 0.6210 -0.0139 0.5975 11.00000 0.05 0.24 Q22 1 0.6669 0.1323 0.6617 11.00000 0.05 0.24 Q23 1 0.6415 -0.0559 0.4988 11.00000 0.05 0.23 Q24 1 0.6395 0.5640 0.4544 11.00000 0.05 0.23 Q25 1 0.7569 0.4003 0.5605 11.00000 0.05 0.22 ; _shelx_res_checksum 17277 _shelx_hkl_file ; -2 0 0 354.58 8.67 2 0 0 311.90 9.72 -4 0 0 178.12 4.47 -4 0 0 169.00 4.09 4 0 0 158.58 4.43 -6 0 0 97.92 2.38 6 0 0 95.78 2.62 -6 0 0 101.85 2.57 -8 0 0 312.89 7.59 8 0 0 318.52 8.28 -8 0 0 308.87 8.22 -10 0 0 118.25 2.94 10 0 0 120.44 3.26 -10 0 0 125.14 3.19 12 0 0 60.43 1.69 -12 0 0 59.04 1.63 -14 0 0 41.17 1.20 14 0 0 42.65 1.26 16 0 0 30.55 1.01 18 0 0 21.20 0.82 1 -1 0 32.76 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15.04 0.61 1 -1 -33 15.21 0.69 -1 1 33 15.75 0.61 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 37924 _symmetry_cell_setting monoclinic _symmetry_space_group_name_h-m 'C 2/c' _symmetry_int_tables_number 15 _chemical_absolute_configuration ? #===End _database_code_depnum_ccdc_archive 'CCDC 967162'