_publ_requested_journal 'J. Am. Chem. Soc.' _publ_contact_author_name 'Oakley, Richard T.' _publ_contact_author_address ; Department of Chemistry University of Waterloo 200 University Avenue Waterloo, Ontario N2L 3G1 Canada ; _publ_contact_author_email oakley@uwaterloo.ca _publ_contact_author_fax '(519) 888-4582' _publ_contact_author_phone '(519) 746-0435' loop_ _publ_author_name _publ_author_address 'Aaron Mailman' ; Department of Chemistry University of Waterloo Waterloo, Ontario N2L 3G1 Canada ; 'Joanne Wong' ; Department of Chemistry University of Waterloo Waterloo, Ontario N2L 3G1 Canada ; 'Steve Winter' ; Department of Chemistry University of Waterloo Waterloo, Ontario N2L 3G1 Canada ; 'Rob Claridge' ; Department of Chemistry University of Waterloo Waterloo, Ontario N2L 3G1 Canada ; 'Craig Robertson' ; Department of Chemistry University of Liverpool Liverpool, Liverpool L69 7ZD UK ; 'Abdeljalil Assoud' ; Department of Chemistry University of Waterloo Waterloo, Ontario N2L 3G1 Canada ; 'Wenjun Yong' ; Department of Earth Sciences University of Western Ontario London, Ontario N6A 5B7, Canada ; 'Eden Steven' ; Department of Physics Florida State University Tallahassee, Florida 32310 United States ; 'Paul Dube' ; Brockhouse Institute for Materials Research McMaster University Hamilton, Ontario L8S 4MI Canada ; 'John Tse' ; Department of Physics University of Saskatchewan Saskatoon, Saskatchewan S7N 5E2, Canada ; 'Serge Desgreniers' ; Department of Physics University of Ottawa Ottawa, Ontario K1N 6N5, Canada ; 'Richard Secco' ; Department of Earth Sciences University of Western Ontario London, Ontario N6A 5B7, Canada ; 'Richard Oakley' ; Department of Chemistry University of Waterloo Waterloo, Ontario N2L 3G1 Canada ; data_NO2BBO(MeCN) _database_code_depnum_ccdc_archive 'CCDC XXXXXXX' _audit_creation_date 2016-06-03 _audit_creation_method ; Olex2 1.2 (compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C6 N3 O3 S4, C2 H3 N' _chemical_formula_sum 'C8 H3 N4 O3 S4' _chemical_formula_weight 331.38 _chemical_melting_point ? 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' _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. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 3.4719(3) _cell_length_b 30.764(4) _cell_length_c 11.0663(13) _cell_angle_alpha 90 _cell_angle_beta 90.2099(7) _cell_angle_gamma 90 _cell_volume 1182.0(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 891 _cell_measurement_temperature 100 _cell_measurement_theta_max 25.395 _cell_measurement_theta_min 2.691 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.811 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6682 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1073 before and 0.0564 after correction. The Ratio of minimum to maximum transmission is 0.8964. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour black _exptl_crystal_colour_primary black _exptl_crystal_density_diffrn 1.862 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description needle _exptl_crystal_F_000 668 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.015 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0589 _diffrn_reflns_av_unetI/netI 0.0353 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 19168 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.987 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 26.411 _diffrn_reflns_theta_min 2.267 _diffrn_ambient_temperature 99.93 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type 'D8 Venture' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_special_details ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1954 _reflns_number_total 2414 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution ? _refine_diff_density_max 0.755 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.076 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 173 _refine_ls_number_reflns 2414 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0360 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+1.5325P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0757 _refine_ls_wR_factor_ref 0.0818 _refine_special_details 'platon squeeze used to remove dissordered acetonitrile in 1-D channel' _olex2_refinement_description ; 1. Fixed Uiso At 1.5 times of: All C(H,H,H) groups 2.a Idealised Me refined as rotating group: C8(H8A,H8B,H8C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? 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 S4 S 0.85079(19) 0.06458(2) 0.24181(6) 0.01837(17) Uani 1 1 d . . . . . S3 S 0.7889(2) 0.04887(2) 0.05962(6) 0.02173(17) Uani 1 1 d . . . . . S2 S 1.23981(18) 0.23521(2) 0.35145(5) 0.01628(16) Uani 1 1 d . . . . . S1 S 1.28417(19) 0.27839(2) 0.20734(6) 0.01802(17) Uani 1 1 d . . . . . O1 O 1.0061(6) 0.18134(6) -0.07281(16) 0.0241(4) Uani 1 1 d . . . . . O2 O 1.1525(6) 0.16864(6) 0.48990(17) 0.0259(5) Uani 1 1 d . . . . . C3 C 1.0389(7) 0.15035(9) 0.2923(2) 0.0164(5) Uani 1 1 d . . . . . N2 N 0.8646(7) 0.09627(7) 0.00144(19) 0.0203(5) Uani 1 1 d . . . . . N1 N 1.1920(6) 0.24551(7) 0.09667(19) 0.0177(5) Uani 1 1 d . . . . . O3 O 0.9472(6) 0.10268(7) 0.44834(17) 0.0300(5) Uani 1 1 d . . . . . C4 C 0.9483(7) 0.11802(8) 0.2063(2) 0.0163(5) Uani 1 1 d . . . . . C2 C 1.1249(7) 0.19317(8) 0.2546(2) 0.0151(5) Uani 1 1 d . . . . . N3 N 1.0476(6) 0.14003(7) 0.41775(19) 0.0183(5) Uani 1 1 d . . . . . C5 C 0.9410(7) 0.12787(9) 0.0807(2) 0.0171(6) Uani 1 1 d . . . . . N4 N 0.6288(8) -0.02710(9) 0.2039(3) 0.0380(7) Uani 1 1 d . . . . . C1 C 1.1153(7) 0.20467(8) 0.1295(2) 0.0158(5) Uani 1 1 d . . . . . C6 C 1.0185(7) 0.17223(8) 0.0354(2) 0.0170(6) Uani 1 1 d . . . . . C8 C 0.5357(18) -0.10713(16) 0.2700(4) 0.0928(18) Uani 1 1 d . . . A 2 H8A H 0.6499 -0.1266 0.2100 0.139 Uiso 1 1 calc GR . . A 2 H8B H 0.2595 -0.1132 0.2768 0.139 Uiso 1 1 calc GR . . A 2 H8C H 0.6603 -0.1118 0.3486 0.139 Uiso 1 1 calc GR . . A 2 C7 C 0.5921(11) -0.06157(13) 0.2321(3) 0.0427(9) Uani 1 1 d . . . A 2 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 S4 0.0182(4) 0.0233(4) 0.0136(3) 0.0008(3) 0.0006(2) 0.0032(3) S3 0.0276(4) 0.0224(4) 0.0152(3) -0.0029(3) -0.0007(3) 0.0064(3) S2 0.0166(4) 0.0243(4) 0.0079(3) -0.0010(2) -0.0002(2) 0.0022(3) S1 0.0215(4) 0.0227(4) 0.0099(3) 0.0000(3) 0.0012(2) 0.0026(3) O1 0.0361(12) 0.0262(11) 0.0101(9) -0.0008(8) -0.0019(8) 0.0076(9) O2 0.0359(12) 0.0285(11) 0.0133(10) -0.0012(8) -0.0035(8) -0.0032(9) C3 0.0127(13) 0.0271(15) 0.0093(12) 0.0014(10) 0.0005(9) 0.0050(10) N2 0.0243(13) 0.0225(12) 0.0140(11) -0.0029(9) -0.0003(9) 0.0089(9) N1 0.0196(12) 0.0240(12) 0.0094(10) -0.0009(9) -0.0006(9) 0.0055(9) O3 0.0414(13) 0.0325(12) 0.0161(10) 0.0049(9) 0.0000(9) -0.0074(10) C4 0.0123(13) 0.0236(14) 0.0131(13) 0.0004(10) 0.0012(10) 0.0068(10) C2 0.0109(13) 0.0239(14) 0.0104(12) -0.0009(10) -0.0004(9) 0.0058(10) N3 0.0201(12) 0.0233(12) 0.0114(11) 0.0013(9) 0.0003(9) 0.0017(9) C5 0.0152(14) 0.0240(14) 0.0120(13) -0.0022(11) -0.0007(10) 0.0073(11) N4 0.0414(17) 0.0293(16) 0.0432(17) -0.0086(13) -0.0039(13) -0.0023(13) C1 0.0126(13) 0.0227(14) 0.0120(12) 0.0015(10) -0.0006(10) 0.0078(10) C6 0.0184(14) 0.0217(14) 0.0109(13) -0.0015(10) 0.0001(10) 0.0098(11) C8 0.151(5) 0.070(3) 0.057(3) 0.033(3) -0.008(3) -0.011(3) C7 0.049(2) 0.056(2) 0.0227(18) -0.0032(16) -0.0063(15) -0.0022(18) _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 S4 S3 2.0837(10) . ? S4 C4 1.724(3) . ? S3 N2 1.616(2) . ? S2 S1 2.0817(9) . ? S2 C2 1.725(3) . ? S1 N1 1.619(2) . ? O1 C6 1.231(3) . ? O2 N3 1.242(3) . ? C3 C4 1.411(4) . ? C3 C2 1.414(4) . ? C3 N3 1.424(3) . ? N2 C5 1.335(3) . ? N1 C1 1.335(3) . ? O3 N3 1.248(3) . ? C4 C5 1.424(3) . ? C2 C1 1.429(3) . ? C5 C6 1.478(4) . ? N4 C7 1.113(4) . ? C1 C6 1.480(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C8 C7 1.476(6) . ? 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 C4 S4 S3 91.17(9) . . ? N2 S3 S4 99.20(9) . . ? C2 S2 S1 91.16(9) . . ? N1 S1 S2 99.55(8) . . ? C4 C3 C2 120.3(2) . . ? C4 C3 N3 120.3(2) . . ? C2 C3 N3 119.4(2) . . ? C5 N2 S3 115.33(19) . . ? C1 N1 S1 114.89(18) . . ? C3 C4 S4 124.2(2) . . ? C3 C4 C5 120.8(2) . . ? C5 C4 S4 115.0(2) . . ? C3 C2 S2 124.32(19) . . ? C3 C2 C1 120.8(2) . . ? C1 C2 S2 114.9(2) . . ? O2 N3 C3 118.3(2) . . ? O2 N3 O3 124.0(2) . . ? O3 N3 C3 117.7(2) . . ? N2 C5 C4 119.3(2) . . ? N2 C5 C6 119.1(2) . . ? C4 C5 C6 121.6(2) . . ? N1 C1 C2 119.5(2) . . ? N1 C1 C6 119.2(2) . . ? C2 C1 C6 121.3(2) . . ? O1 C6 C5 122.3(2) . . ? O1 C6 C1 122.6(2) . . ? C5 C6 C1 115.2(2) . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? N4 C7 C8 178.9(5) . . ? 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 S4 S3 N2 C5 0.7(2) . . . . ? S4 C4 C5 N2 -0.4(3) . . . . ? S4 C4 C5 C6 179.97(19) . . . . ? S3 S4 C4 C3 -177.8(2) . . . . ? S3 S4 C4 C5 0.71(18) . . . . ? S3 N2 C5 C4 -0.3(3) . . . . ? S3 N2 C5 C6 179.31(18) . . . . ? S2 S1 N1 C1 1.16(19) . . . . ? S2 C2 C1 N1 -0.1(3) . . . . ? S2 C2 C1 C6 -179.56(19) . . . . ? S1 S2 C2 C3 -178.3(2) . . . . ? S1 S2 C2 C1 0.72(18) . . . . ? S1 N1 C1 C2 -0.8(3) . . . . ? S1 N1 C1 C6 178.62(18) . . . . ? C3 C4 C5 N2 178.2(2) . . . . ? C3 C4 C5 C6 -1.4(4) . . . . ? C3 C2 C1 N1 179.0(2) . . . . ? C3 C2 C1 C6 -0.5(4) . . . . ? N2 C5 C6 O1 1.8(4) . . . . ? N2 C5 C6 C1 -177.7(2) . . . . ? N1 C1 C6 O1 0.1(4) . . . . ? N1 C1 C6 C5 179.6(2) . . . . ? C4 C3 C2 S2 -179.94(19) . . . . ? C4 C3 C2 C1 1.1(4) . . . . ? C4 C3 N3 O2 175.5(2) . . . . ? C4 C3 N3 O3 -4.8(3) . . . . ? C4 C5 C6 O1 -178.6(2) . . . . ? C4 C5 C6 C1 1.9(3) . . . . ? C2 C3 C4 S4 178.33(19) . . . . ? C2 C3 C4 C5 -0.1(4) . . . . ? C2 C3 N3 O2 -4.0(3) . . . . ? C2 C3 N3 O3 175.7(2) . . . . ? C2 C1 C6 O1 179.6(2) . . . . ? C2 C1 C6 C5 -1.0(3) . . . . ? N3 C3 C4 S4 -1.2(3) . . . . ? N3 C3 C4 C5 -179.6(2) . . . . ? N3 C3 C2 S2 -0.4(3) . . . . ? N3 C3 C2 C1 -179.4(2) . . . . ? _shelx_res_file ; final_sq.res created by SHELXL-2014/7 TITL zeefinal in P2(1)/n CELL 0.71073 3.4719 30.7642 11.0663 90 90.2099 90 ZERR 4 0.0003 0.0037 0.0013 0 0.0007 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O S UNIT 32 12 16 12 16 L.S. 50 0 7 PLAN 20 TEMP -173.22 BOND MORE -1 BOND $H CONF ABIN fmap 2 acta 52 REM REM REM WGHT 0.033000 1.532500 FVAR 0.17711 S4 5 0.850793 0.064582 0.241814 11.00000 0.01817 0.02332 = 0.01361 0.00080 0.00059 0.00317 S3 5 0.788894 0.048873 0.059617 11.00000 0.02759 0.02245 = 0.01516 -0.00288 -0.00072 0.00636 S2 5 1.239815 0.235210 0.351447 11.00000 0.01664 0.02429 = 0.00793 -0.00098 -0.00016 0.00221 S1 5 1.284168 0.278391 0.207339 11.00000 0.02147 0.02272 = 0.00989 -0.00002 0.00118 0.00263 O1 4 1.006063 0.181336 -0.072809 11.00000 0.03610 0.02617 = 0.01010 -0.00075 -0.00186 0.00758 O2 4 1.152491 0.168641 0.489903 11.00000 0.03592 0.02853 = 0.01332 -0.00120 -0.00351 -0.00315 C3 1 1.038944 0.150348 0.292298 11.00000 0.01271 0.02709 = 0.00934 0.00142 0.00046 0.00501 N2 3 0.864583 0.096270 0.001445 11.00000 0.02430 0.02252 = 0.01402 -0.00289 -0.00033 0.00892 N1 3 1.191953 0.245515 0.096668 11.00000 0.01962 0.02403 = 0.00941 -0.00091 -0.00057 0.00546 O3 4 0.947192 0.102676 0.448340 11.00000 0.04145 0.03253 = 0.01607 0.00489 0.00002 -0.00742 C4 1 0.948317 0.118020 0.206330 11.00000 0.01226 0.02361 = 0.01309 0.00043 0.00125 0.00684 C2 1 1.124905 0.193174 0.254626 11.00000 0.01090 0.02391 = 0.01039 -0.00092 -0.00043 0.00582 N3 3 1.047623 0.140032 0.417748 11.00000 0.02006 0.02335 = 0.01141 0.00133 0.00030 0.00165 C5 1 0.941049 0.127872 0.080650 11.00000 0.01515 0.02403 = 0.01204 -0.00215 -0.00067 0.00728 N4 3 0.628792 -0.027097 0.203927 11.00000 0.04145 0.02931 = 0.04321 -0.00860 -0.00385 -0.00226 C1 1 1.115317 0.204666 0.129522 11.00000 0.01259 0.02270 = 0.01195 0.00147 -0.00057 0.00776 C6 1 1.018494 0.172226 0.035449 11.00000 0.01845 0.02169 = 0.01092 -0.00146 0.00010 0.00977 PART 2 C8 1 0.535702 -0.107126 0.270046 11.00000 0.15113 0.06966 = 0.05748 0.03256 -0.00773 -0.01097 AFIX 137 H8A 2 0.649856 -0.126609 0.209960 11.00000 -1.50000 H8B 2 0.259515 -0.113194 0.276780 11.00000 -1.50000 H8C 2 0.660287 -0.111817 0.348576 11.00000 -1.50000 AFIX 0 C7 1 0.592111 -0.061569 0.232118 11.00000 0.04904 0.05632 = 0.02274 -0.00316 -0.00629 -0.00222 HKLF 4 REM zeefinal in P2(1)/n REM R1 = 0.0360 for 1954 Fo > 4sig(Fo) and 0.0534 for all 2414 data REM 173 parameters refined using 0 restraints END WGHT 0.0330 1.5326 REM Highest difference peak 0.755, deepest hole -0.365, 1-sigma level 0.076 Q1 1 0.5379 -0.0230 0.3171 11.00000 0.05 0.75 Q2 1 1.0274 0.1488 0.0582 11.00000 0.05 0.32 Q3 1 1.0547 0.1753 0.2781 11.00000 0.05 0.29 Q4 1 1.1016 0.1871 0.0833 11.00000 0.05 0.27 Q5 1 1.0674 0.2000 0.1929 11.00000 0.05 0.27 Q6 1 0.8693 0.0958 0.2201 11.00000 0.05 0.26 Q7 1 0.9737 0.2291 0.1191 11.00000 0.05 0.26 Q8 1 1.3120 0.2652 0.2624 11.00000 0.05 0.25 Q9 1 0.4871 0.0660 0.0594 11.00000 0.05 0.25 Q10 1 1.0043 0.1469 0.3546 11.00000 0.05 0.24 Q11 1 1.0634 0.2102 0.2998 11.00000 0.05 0.24 Q12 1 1.5415 0.2276 0.3401 11.00000 0.05 0.24 Q13 1 0.2765 -0.1121 0.3626 11.00000 0.05 0.24 Q14 1 0.1709 -0.0054 0.1667 11.00000 0.05 0.23 Q15 1 0.6649 0.0796 0.4015 11.00000 0.05 0.22 Q16 1 1.0255 0.1660 -0.0958 11.00000 0.05 0.22 Q17 1 1.2532 0.2118 0.2986 11.00000 0.05 0.22 Q18 1 0.6197 0.1035 0.4772 11.00000 0.05 0.22 Q19 1 1.4118 0.1298 0.2020 11.00000 0.05 0.22 Q20 1 1.0910 -0.0088 0.2591 11.00000 0.05 0.22 ; _shelx_res_checksum 59623 _shelx_hkl_file ; -1 0 0 0.00 0.30 -2 0 0 48.41 1.96 -3 0 0 -0.07 0.99 -4 0 0 6.20 2.03 -1 -1 0 342.31 7.70 1 1 0 347.45 7.72 -1 1 0 338.94 7.67 -2 -1 0 0.51 0.60 -2 1 0 -0.06 0.56 -3 -1 0 24.60 2.06 -3 1 0 24.66 2.07 -4 -1 0 5.41 2.13 -4 1 0 6.78 1.96 -1 -2 0 46.49 1.14 1 -2 0 50.05 1.14 -1 -2 0 46.39 1.52 -1 -2 0 46.17 1.13 1 2 0 48.23 1.16 1 2 0 51.26 1.20 1 2 0 47.08 1.56 -2 -2 0 24.50 1.46 -2 2 0 23.03 1.42 -3 -2 0 3.37 1.16 -3 2 0 4.47 1.19 -4 2 0 28.78 3.19 1 -3 0 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-0.01 0.00 -2 33 4 0.11 0.00 2 33 4 -0.29 0.00 -2 34 4 0.15 0.00 2 34 4 0.37 0.00 -1 36 4 0.62 0.00 1 36 4 0.30 0.00 -1 37 4 -0.07 0.00 0 37 4 0.29 0.00 1 37 4 0.53 0.00 0 38 4 0.03 0.00 -4 1 5 0.22 0.00 -4 2 5 -0.18 0.00 -4 3 5 0.20 0.00 -4 5 5 0.17 0.00 -4 6 5 -0.46 0.00 4 6 5 -2.38 0.00 -4 7 5 0.12 0.00 4 7 5 -1.00 0.00 -4 8 5 -0.51 0.00 4 8 5 -2.30 0.00 -4 9 5 0.06 0.00 4 9 5 -0.70 0.00 -4 10 5 -0.47 0.00 4 10 5 -1.86 0.00 -4 11 5 0.00 0.00 4 11 5 -0.39 0.00 -4 12 5 -0.36 0.00 4 12 5 -1.25 0.00 3 24 5 0.93 0.00 -3 25 5 0.06 0.00 3 25 5 -0.04 0.00 -3 26 5 0.32 0.00 3 26 5 0.70 0.00 -2 32 5 0.06 0.00 2 32 5 0.20 0.00 -2 33 5 -0.14 0.00 2 33 5 -0.10 0.00 -1 35 5 -0.82 0.00 1 35 5 -0.34 0.00 -1 36 5 -0.08 0.00 0 36 5 -0.28 0.00 1 36 5 -0.97 0.00 0 37 5 0.03 0.00 -4 0 6 -0.07 0.00 4 0 6 1.45 0.00 -4 1 6 0.07 0.00 4 1 6 0.43 0.00 -4 2 6 -0.07 0.00 4 2 6 1.39 0.00 -4 3 6 0.21 0.00 4 3 6 1.19 0.00 -4 4 6 -0.06 0.00 4 4 6 1.22 0.00 -4 5 6 0.32 0.00 4 5 6 1.64 0.00 -4 6 6 -0.04 0.00 4 6 6 0.95 0.00 -4 7 6 0.39 0.00 4 7 6 1.71 0.00 -4 8 6 0.00 0.00 4 8 6 0.64 0.00 -4 9 6 0.40 0.00 -3 23 6 -0.16 0.00 3 23 6 -0.86 0.00 -3 24 6 -0.02 0.00 3 24 6 -0.03 0.00 -3 25 6 -0.19 0.00 -2 30 6 0.08 0.00 2 30 6 -0.09 0.00 -2 31 6 -0.39 0.00 2 31 6 -0.18 0.00 -1 34 6 0.82 0.00 1 34 6 0.23 0.00 -1 35 6 0.23 0.00 0 35 6 0.19 0.00 1 35 6 1.24 0.00 0 36 6 -0.06 0.00 -3 20 7 -0.12 0.00 3 20 7 0.52 0.00 -3 21 7 -0.20 0.00 3 21 7 0.18 0.00 -3 22 7 -0.07 0.00 3 22 7 0.63 0.00 -3 23 7 -0.09 0.00 2 28 7 0.37 0.00 -2 29 7 0.09 0.00 2 29 7 0.18 0.00 -2 30 7 0.69 0.00 2 30 7 0.23 0.00 -1 32 7 -0.18 0.00 1 32 7 -1.25 0.00 -1 33 7 -0.70 0.00 1 33 7 -0.05 0.00 -1 34 7 -0.25 0.00 0 34 7 -0.13 0.00 0 35 7 0.04 0.00 -3 17 8 0.15 0.00 3 17 8 0.27 0.00 -3 18 8 0.22 0.00 3 18 8 -0.25 0.00 -3 19 8 0.18 0.00 3 19 8 -0.08 0.00 -3 20 8 0.23 0.00 3 20 8 -0.26 0.00 -2 26 8 -0.21 0.00 2 26 8 -0.18 0.00 -2 27 8 -0.83 0.00 2 27 8 -0.33 0.00 -2 28 8 -0.13 0.00 2 28 8 -0.17 0.00 -1 31 8 0.03 0.00 1 31 8 0.78 0.00 -1 32 8 0.53 0.00 0 32 8 0.13 0.00 1 32 8 -0.06 0.00 0 33 8 0.17 0.00 3 12 9 -0.98 0.00 -3 13 9 -0.09 0.00 3 13 9 -0.09 0.00 -3 14 9 0.10 0.00 3 14 9 -0.82 0.00 -3 15 9 -0.12 0.00 3 15 9 0.08 0.00 -3 16 9 -0.02 0.00 3 16 9 -0.54 0.00 -2 24 9 0.56 0.00 2 24 9 0.14 0.00 -2 25 9 0.10 0.00 2 25 9 0.11 0.00 -2 26 9 0.60 0.00 -1 28 9 0.22 0.00 1 28 9 -0.27 0.00 -1 29 9 -0.57 0.00 1 29 9 -0.07 0.00 -1 30 9 0.18 0.00 0 30 9 -0.23 0.00 1 30 9 -0.24 0.00 0 31 9 -0.18 0.00 3 1 10 -0.41 0.00 -3 2 10 0.15 0.00 3 2 10 0.13 0.00 -3 3 10 -1.13 0.00 3 3 10 -0.26 0.00 -3 4 10 0.26 0.00 3 4 10 0.24 0.00 -3 5 10 -0.94 0.00 3 5 10 -0.01 0.00 -3 6 10 0.29 0.00 3 6 10 0.32 0.00 -3 7 10 -0.71 0.00 3 7 10 0.27 0.00 -3 8 10 0.26 0.00 3 8 10 0.35 0.00 -3 9 10 -0.49 0.00 3 9 10 0.50 0.00 -3 10 10 0.19 0.00 3 10 10 0.30 0.00 -3 11 10 -0.30 0.00 3 11 10 0.63 0.00 -2 20 10 -0.18 0.00 2 20 10 -0.02 0.00 -2 21 10 0.07 0.00 2 21 10 0.21 0.00 -2 22 10 -0.06 0.00 2 22 10 0.01 0.00 -2 23 10 -0.08 0.00 -1 26 10 0.47 0.00 1 26 10 0.19 0.00 -1 27 10 -0.36 0.00 0 27 10 0.22 0.00 1 27 10 -0.03 0.00 0 28 10 0.44 0.00 -2 16 11 -0.73 0.00 2 16 11 -0.30 0.00 -2 17 11 0.14 0.00 2 17 11 -0.07 0.00 -2 18 11 -0.63 0.00 2 18 11 -0.37 0.00 -2 19 11 0.05 0.00 -1 22 11 0.49 0.00 1 22 11 -0.04 0.00 -1 23 11 -0.27 0.00 1 23 11 -0.13 0.00 -1 24 11 0.43 0.00 0 24 11 -0.34 0.00 1 24 11 0.01 0.00 0 25 11 -0.63 0.00 0 26 11 -0.20 0.00 -2 8 12 -0.12 0.00 2 8 12 0.24 0.00 -2 9 12 0.55 0.00 2 9 12 0.02 0.00 -2 10 12 -0.10 0.00 2 10 12 0.22 0.00 -2 11 12 0.63 0.00 2 11 12 0.07 0.00 -2 12 12 -0.06 0.00 2 12 12 0.19 0.00 -2 13 12 0.68 0.00 2 13 12 0.16 0.00 -1 17 12 -0.44 0.00 1 17 12 0.13 0.00 -1 18 12 0.11 0.00 1 18 12 -0.01 0.00 -1 19 12 -0.43 0.00 1 19 12 0.07 0.00 -1 20 12 0.11 0.00 0 20 12 0.70 0.00 1 20 12 0.03 0.00 0 21 12 0.52 0.00 0 22 12 0.57 0.00 -1 10 13 -0.02 0.00 1 10 13 -0.28 0.00 -1 11 13 -0.11 0.00 1 11 13 0.34 0.00 -1 12 13 0.03 0.00 1 12 13 -0.18 0.00 -1 13 13 -0.15 0.00 1 13 13 0.18 0.00 -1 14 13 0.10 0.00 0 14 13 -0.38 0.00 1 14 13 -0.09 0.00 -1 15 13 -0.13 0.00 0 15 13 -0.36 0.00 1 15 13 0.06 0.00 0 16 13 -0.43 0.00 0 17 13 -0.36 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 140116) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.062 0.000 0.500 42 12 ' ' 2 -0.060 0.500 0.000 42 12 ' ' # Missing Reflections Below sin(th)/lambda = 0.25 loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta 0 2 0 1.325 0 1 1 1.958 _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL zeefinal in P2(1)/n CELL 3.4670 30.7350 11.0510 90.00 90.22 90.00 SPGR P21/n # Solvent Accessible Volume = 85 # Electrons Found in S.A.V. = 23 # Note: Atoms in Void as Cxxx and Qxxx all others C101 0.500 1.000 0.500 ! 3.16 eA-3 C102 0.252 0.503 0.006 ! 2.65 eA-3 Q103 1.003 0.483 0.163 ! 0.99 eA-3 Q104 0.612 0.969 0.439 ! 0.65 eA-3 Q105 0.857 0.984 0.418 ! 0.58 eA-3 ) ; _shelx_SHELXL_version_number '2014/7' _olex2_exptl_crystal_mounting_method 'mitogen with fomblin' _olex2_submission_special_instructions 'No special instructions were received'