Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _audit_creation_method CRYSTALS_ver_12-03-99 _publ_contact_author_name 'Sofia I. Pascu' _publ_contact_author_address ; Inorganic Chemistry Laboratory University of Oxford South Parks Road Oxford OX1 3QR UNITED KINGDOM ; _publ_contact_author_email sofia.pascu@chem.ox.ac.uk _publ_contact_author_fax '(01865) 285200' _publ_contact_author_phone '(01865) 285201' _publ_section_title ; Designing Zn(II) and Cu(II) derivatives as probes for in vitro fluorescence imaging ; loop_ _publ_author_name 'Sofia I. Pascu' 'Franklin I Aigbirhio' 'Helen M. Betts' 'Martin Christlieb' 'Grant C. Churchill' ; T.D.Conry ; 'Jonathan R. Dilworth' 'Tzveta Pokrovska' 'Philip A. Waghorn' 'John E. Warren' data_1 _database_code_depnum_ccdc_archive 'CCDC 642484' _audit_creation_date 07-03-27 _audit_creation_method CRYSTALS_ver_12.80 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 8.4135(2) _cell_length_b 18.9038(5) _cell_length_c 12.3095(3) _cell_angle_alpha 90 _cell_angle_beta 95.7293(12) _cell_angle_gamma 90 _cell_volume 1948.01(8) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421 1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C20 H18 N6 Ni1 S2' _chemical_formula_moiety 'C20 H18 N6 Ni1 S2' _chemical_compound_source ? _chemical_formula_weight 465.25 _cell_measurement_reflns_used 4384 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 1.231 # Sheldrick geometric approximatio 0.78 0.88 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.88 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'Nonius (1997-2001). COLLECT.' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 8655 _reflns_number_total 4417 _diffrn_reflns_av_R_equivalents 0.021 # Number of reflections with Friedels Law is 4417 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 4448 _diffrn_reflns_theta_min 5.103 _diffrn_reflns_theta_max 27.453 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.630 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 24 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _oxford_diffrn_Wilson_B_factor 1.83 _oxford_diffrn_Wilson_scale 20.36 _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.39 _refine_diff_density_max 0.66 _refine_ls_number_reflns 2853 _refine_ls_number_restraints 16 _refine_ls_number_parameters 280 #_refine_ls_R_factor_ref 0.0306 _refine_ls_wR_factor_ref 0.0364 _refine_ls_goodness_of_fit_ref 1.1304 #_reflns_number_all 4417 _refine_ls_R_factor_all 0.0579 _refine_ls_wR_factor_all 0.0567 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 2853 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_gt 0.0364 _refine_ls_shift/su_max 0.009443 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.431 0.261 0.237 ; # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ni1 Ni 0.64669(4) 0.367098(16) 0.46041(2) 0.0208 1.0000 Uani . . . . . . N1 N 0.6392(2) 0.43962(11) 0.56388(16) 0.0212 1.0000 Uani . . . . . . N2 N 0.5640(3) 0.43685(11) 0.65764(16) 0.0235 1.0000 Uani . . . . . . N3 N 0.4236(3) 0.36018(11) 0.75500(17) 0.0265 1.0000 Uani . . . . . . N4 N 0.7612(2) 0.43216(11) 0.38373(16) 0.0216 1.0000 Uani . . . . . . N5 N 0.8168(3) 0.42130(11) 0.28438(17) 0.0251 1.0000 Uani . . . . . . N6 N 0.8170(3) 0.33731(12) 0.15062(18) 0.0306 1.0000 Uani . . . . . . C1 C 0.7160(3) 0.49632(13) 0.53931(19) 0.0210 1.0000 Uani . . . . . . C2 C 0.7878(3) 0.49153(13) 0.43576(19) 0.0209 1.0000 Uani . . . . . . C3 C 0.8710(3) 0.55774(13) 0.4192(2) 0.0230 1.0000 Uani . . . . . . C4 C 0.9600(3) 0.58417(14) 0.3405(2) 0.0268 1.0000 Uani . . . . . . C5 C 1.0205(3) 0.65357(15) 0.3543(2) 0.0322 1.0000 Uani . . . . . . C6 C 0.9953(3) 0.69469(14) 0.4434(2) 0.0324 1.0000 Uani . . . . . . C7 C 0.9041(3) 0.66879(14) 0.5261(2) 0.0265 1.0000 Uani . . . . . . C8 C 0.8653(3) 0.70397(14) 0.6219(2) 0.0321 1.0000 Uani . . . . . . C9 C 0.7737(3) 0.67167(15) 0.6935(2) 0.0316 1.0000 Uani . . . . . . C10 C 0.7147(3) 0.60188(14) 0.6774(2) 0.0272 1.0000 Uani . . . . . . C11 C 0.7516(3) 0.56601(13) 0.5859(2) 0.0228 1.0000 Uani . . . . . . C12 C 0.8450(3) 0.59992(13) 0.51133(19) 0.0228 1.0000 Uani . . . . . . C13 C 0.7763(3) 0.35757(13) 0.2490(2) 0.0242 1.0000 Uani . . . . . . C14 C 0.9206(4) 0.37912(16) 0.0871(2) 0.0356 1.0000 Uani . . . . . . C17 C 0.5022(3) 0.37290(13) 0.66726(19) 0.0225 1.0000 Uani . . . . . . C18 C 0.3991(3) 0.41585(15) 0.8348(2) 0.0288 1.0000 Uani . . . . . . C19 C 0.3251(4) 0.38642(17) 0.9294(3) 0.0416 1.0000 Uani . . . . . . C20 C 0.3894(6) 0.3913(2) 1.0306(3) 0.0603 1.0000 Uani . . . . . . S1 S 0.52068(8) 0.30410(3) 0.57269(5) 0.0256 1.0000 Uani . . . . . . S2 S 0.66952(8) 0.29651(3) 0.32231(5) 0.0262 1.0000 Uani . . . . . . C150 C 0.8409(11) 0.4250(7) 0.0104(8) 0.0428 0.3000 Uani D U . . . . C151 C 0.8600(7) 0.3789(3) -0.0308(5) 0.0559 0.7000 Uani D U . . . . C160 C 0.8388(16) 0.4044(8) -0.0948(10) 0.0441 0.3000 Uani D U . . . . C161 C 0.8307(9) 0.4367(3) -0.0939(5) 0.0559 0.7000 Uani D U . . . . H41 H 0.9796 0.5572 0.2788 0.0395 1.0000 Uiso . . . . . . H51 H 1.0816 0.6726 0.3005 0.0474 1.0000 Uiso . . . . . . H61 H 1.0392 0.7398 0.4495 0.0461 1.0000 Uiso . . . . . . H81 H 0.9038 0.7505 0.6363 0.0462 1.0000 Uiso . . . . . . H91 H 0.7488 0.6959 0.7563 0.0449 1.0000 Uiso . . . . . . H101 H 0.6522 0.5807 0.7291 0.0391 1.0000 Uiso . . . . . . H181 H 0.5025 0.4375 0.8595 0.0440 1.0000 Uiso . . . . . . H182 H 0.3285 0.4531 0.7983 0.0445 1.0000 Uiso . . . . . . H191 H 0.2252 0.3630 0.9151 0.0628 1.0000 Uiso . . . . . . H201 H 0.4900 0.4144 1.0457 0.0909 1.0000 Uiso . . . . . . H202 H 0.3383 0.3723 1.0882 0.0917 1.0000 Uiso . . . . . . H8 H 0.3776 0.3194 0.7615 0.0398 1.0000 Uiso . . . . . . H10 H 0.7818 0.2966 0.1248 0.0458 1.0000 Uiso . . . . . . H14 H 0.9710 0.4176 0.1286 0.0677 1.0000 Uiso . . . . . . H15 H 1.0293 0.3602 0.0834 0.0679 1.0000 Uiso . . . . . . H1501 H 0.7882 0.4702 0.0316 0.0564 0.3000 Uiso . . . . . . H1601 H 0.7845 0.4360 -0.1549 0.0573 0.3000 Uiso . . . . . . H1602 H 0.8931 0.3609 -0.1148 0.0573 0.3000 Uiso . . . . . . H1511 H 0.8390 0.3316 -0.0676 0.0715 0.7000 Uiso . . . . . . H1611 H 0.8499 0.4850 -0.0612 0.0719 0.7000 Uiso . . . . . . H1612 H 0.7894 0.4321 -0.1726 0.0719 0.7000 Uiso . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.02419(17) 0.01708(16) 0.02133(15) -0.00017(12) 0.00270(11) -0.00087(13) N1 0.0194(10) 0.0219(10) 0.0221(9) 0.0013(8) 0.0008(8) 0.0011(8) N2 0.0239(11) 0.0245(10) 0.0223(10) 0.0033(8) 0.0028(8) 0.0001(9) N3 0.0306(12) 0.0259(11) 0.0234(10) 0.0039(9) 0.0049(8) -0.0017(9) N4 0.0236(11) 0.0188(10) 0.0229(10) 0.0004(8) 0.0041(8) 0.0023(8) N5 0.0290(12) 0.0238(11) 0.0229(10) -0.0001(8) 0.0051(8) 0.0028(9) N6 0.0404(13) 0.0266(11) 0.0256(11) -0.0035(9) 0.0077(10) 0.0015(10) C1 0.0218(12) 0.0192(11) 0.0215(11) -0.0022(9) 0.0004(9) -0.0012(9) C2 0.0198(12) 0.0198(11) 0.0229(11) 0.0022(9) 0.0007(9) -0.0003(9) C3 0.0205(12) 0.0225(12) 0.0249(12) 0.0019(9) -0.0025(9) 0.0033(9) C4 0.0252(13) 0.0272(13) 0.0276(13) 0.0045(10) 0.0010(10) 0.0016(10) C5 0.0275(14) 0.0306(14) 0.0379(15) 0.0116(11) 0.0004(11) -0.0025(11) C6 0.0304(14) 0.0214(13) 0.0440(15) 0.0058(12) -0.0032(12) -0.0043(11) C7 0.0237(13) 0.0179(12) 0.0361(14) -0.0015(10) -0.0060(10) 0.0011(10) C8 0.0319(15) 0.0219(13) 0.0401(15) -0.0053(11) -0.0089(12) -0.0018(11) C9 0.0346(15) 0.0265(14) 0.0321(13) -0.0081(11) -0.0043(11) 0.0031(11) C10 0.0288(13) 0.0279(13) 0.0242(12) -0.0012(10) -0.0001(10) 0.0040(11) C11 0.0220(12) 0.0208(12) 0.0250(11) 0.0022(9) -0.0015(9) 0.0000(10) C12 0.0215(12) 0.0218(12) 0.0242(12) 0.0027(9) -0.0026(10) 0.0027(10) C13 0.0231(12) 0.0234(12) 0.0254(12) -0.0007(10) -0.0005(9) 0.0043(10) C14 0.0386(16) 0.0386(16) 0.0307(13) -0.0009(12) 0.0094(12) -0.0023(13) C17 0.0203(11) 0.0234(12) 0.0232(11) 0.0028(10) -0.0015(9) 0.0022(10) C18 0.0312(14) 0.0280(13) 0.0275(13) -0.0003(10) 0.0047(11) 0.0000(11) C19 0.0522(19) 0.0347(16) 0.0414(16) -0.0051(13) 0.0216(14) -0.0071(14) C20 0.108(3) 0.047(2) 0.0291(16) 0.0044(14) 0.0236(18) 0.017(2) S1 0.0291(3) 0.0208(3) 0.0271(3) 0.0012(2) 0.0044(2) -0.0030(2) S2 0.0318(3) 0.0204(3) 0.0267(3) -0.0035(2) 0.0038(2) -0.0018(3) C150 0.016(3) 0.061(6) 0.053(5) 0.014(4) 0.008(3) 0.004(4) C151 0.050(2) 0.079(3) 0.039(2) 0.024(2) 0.0037(18) -0.004(2) C160 0.018(4) 0.062(6) 0.052(5) 0.014(4) 0.007(3) 0.002(4) C161 0.049(2) 0.079(3) 0.040(2) 0.025(2) 0.0049(18) -0.001(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2201(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ni1 . N1 . 1.877(2) yes Ni1 . N4 . 1.874(2) yes Ni1 . C1 . 2.672(2) yes Ni1 . C2 . 2.666(2) yes Ni1 . S1 . 2.1784(7) yes Ni1 . S2 . 2.1846(7) yes N1 . N2 . 1.372(3) yes N1 . C1 . 1.302(3) yes N2 . C17 . 1.326(3) yes N3 . C17 . 1.343(3) yes N3 . C18 . 1.468(3) yes N3 . H8 . 0.869 no N4 . N5 . 1.368(3) yes N4 . C2 . 1.301(3) yes N5 . C13 . 1.314(3) yes N6 . C13 . 1.347(3) yes N6 . C14 . 1.460(4) yes N6 . H10 . 0.873 no C1 . C2 . 1.467(3) yes C1 . C11 . 1.456(3) yes C2 . C3 . 1.458(3) yes C3 . C4 . 1.376(4) yes C3 . C12 . 1.421(4) yes C4 . C5 . 1.411(4) yes C4 . H41 . 0.943 no C5 . C6 . 1.378(4) yes C5 . H51 . 0.949 no C6 . C7 . 1.421(4) yes C6 . H61 . 0.930 no C7 . C8 . 1.420(4) yes C7 . C12 . 1.399(4) yes C8 . C9 . 1.371(4) yes C8 . H81 . 0.947 no C9 . C10 . 1.416(4) yes C9 . H91 . 0.941 no C10 . C11 . 1.377(4) yes C10 . H101 . 0.953 no C11 . C12 . 1.419(3) yes C13 . S2 . 1.765(3) yes C14 . C150 . 1.403(11) yes C14 . C151 . 1.490(6) yes C14 . H14 . 0.963 no C14 . H15 . 0.987 no C17 . S1 . 1.763(3) yes C18 . C19 . 1.482(4) yes C18 . H181 . 0.981 no C18 . H182 . 1.000 no C19 . C20 . 1.311(5) yes C19 . H191 . 0.951 no C20 . H201 . 0.954 no C20 . H202 . 0.936 no C150 . C151 . 1.029(13) yes C150 . C160 . 1.351(2) yes C150 . C161 . 1.297(13) yes C150 . H1501 . 1.010 no C151 . C160 . 0.925(14) yes C151 . C161 . 1.3489(19) yes C151 . H1602 . 1.148 no C151 . H1511 . 1.010 no C160 . H1601 . 1.023 no C160 . H1602 . 0.982 no C160 . H1612 . 1.134 no C161 . H1601 . 0.811 no C161 . H1611 . 1.003 no C161 . H1612 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Ni1 . N4 . 85.19(9) yes N1 . Ni1 . C1 . 26.63(8) yes N4 . Ni1 . C1 . 58.58(8) yes N1 . Ni1 . C2 . 58.54(8) yes N4 . Ni1 . C2 . 26.69(8) yes C1 . Ni1 . C2 . 31.91(7) yes N1 . Ni1 . S1 . 85.26(6) yes N4 . Ni1 . S1 . 170.21(7) yes C1 . Ni1 . S1 . 111.81(5) yes C2 . Ni1 . S1 . 143.62(5) yes N1 . Ni1 . S2 . 170.36(7) yes N4 . Ni1 . S2 . 85.38(6) yes C1 . Ni1 . S2 . 143.95(6) yes C2 . Ni1 . S2 . 112.06(5) yes S1 . Ni1 . S2 . 104.24(3) yes Ni1 . N1 . N2 . 126.35(16) yes Ni1 . N1 . C1 . 113.13(16) yes N2 . N1 . C1 . 120.5(2) yes N1 . N2 . C17 . 109.1(2) yes C17 . N3 . C18 . 121.5(2) yes C17 . N3 . H8 . 119.5 no C18 . N3 . H8 . 118.7 no Ni1 . N4 . N5 . 126.21(16) yes Ni1 . N4 . C2 . 112.97(16) yes N5 . N4 . C2 . 120.8(2) yes N4 . N5 . C13 . 109.5(2) yes C13 . N6 . C14 . 123.1(2) yes C13 . N6 . H10 . 118.1 no C14 . N6 . H10 . 118.8 no N1 . C1 . Ni1 . 40.24(11) yes N1 . C1 . C2 . 114.1(2) yes Ni1 . C1 . C2 . 73.84(13) yes N1 . C1 . C11 . 137.8(2) yes Ni1 . C1 . C11 . 177.99(17) yes C2 . C1 . C11 . 108.1(2) yes C1 . C2 . N4 . 114.5(2) yes C1 . C2 . Ni1 . 74.25(13) yes N4 . C2 . Ni1 . 40.34(12) yes C1 . C2 . C3 . 108.3(2) yes N4 . C2 . C3 . 137.2(2) yes Ni1 . C2 . C3 . 177.07(18) yes C2 . C3 . C4 . 135.5(2) yes C2 . C3 . C12 . 104.8(2) yes C4 . C3 . C12 . 119.7(2) yes C3 . C4 . C5 . 117.9(2) yes C3 . C4 . H41 . 121.5 no C5 . C4 . H41 . 120.6 no C4 . C5 . C6 . 122.5(3) yes C4 . C5 . H51 . 118.8 no C6 . C5 . H51 . 118.7 no C5 . C6 . C7 . 120.8(2) yes C5 . C6 . H61 . 119.3 no C7 . C6 . H61 . 119.8 no C6 . C7 . C8 . 128.2(3) yes C6 . C7 . C12 . 116.0(2) yes C8 . C7 . C12 . 115.8(2) yes C7 . C8 . C9 . 121.1(2) yes C7 . C8 . H81 . 119.2 no C9 . C8 . H81 . 119.8 no C8 . C9 . C10 . 122.4(2) yes C8 . C9 . H91 . 119.8 no C10 . C9 . H91 . 117.7 no C9 . C10 . C11 . 117.9(2) yes C9 . C10 . H101 . 120.5 no C11 . C10 . H101 . 121.5 no C1 . C11 . C10 . 135.5(2) yes C1 . C11 . C12 . 105.0(2) yes C10 . C11 . C12 . 119.4(2) yes C3 . C12 . C11 . 113.7(2) yes C3 . C12 . C7 . 123.0(2) yes C11 . C12 . C7 . 123.3(2) yes N6 . C13 . N5 . 118.5(2) yes N6 . C13 . S2 . 117.5(2) yes N5 . C13 . S2 . 123.95(19) yes N6 . C14 . C150 . 115.2(5) yes N6 . C14 . C151 . 110.8(3) yes C150 . C14 . C151 . 41.5(5) yes N6 . C14 . H14 . 112.3 no C150 . C14 . H14 . 92.6 no C151 . C14 . H14 . 127.5 no N6 . C14 . H15 . 115.7 no C150 . C14 . H15 . 125.1 no C151 . C14 . H15 . 100.5 no H14 . C14 . H15 . 86.4 no N3 . C17 . N2 . 117.6(2) yes N3 . C17 . S1 . 118.82(19) yes N2 . C17 . S1 . 123.53(19) yes N3 . C18 . C19 . 110.8(2) yes N3 . C18 . H181 . 109.1 no C19 . C18 . H181 . 110.0 no N3 . C18 . H182 . 108.7 no C19 . C18 . H182 . 109.9 no H181 . C18 . H182 . 108.3 no C18 . C19 . C20 . 123.7(3) yes C18 . C19 . H191 . 117.6 no C20 . C19 . H191 . 118.8 no C19 . C20 . H201 . 119.4 no C19 . C20 . H202 . 121.1 no H201 . C20 . H202 . 119.5 no C17 . S1 . Ni1 . 95.53(8) yes C13 . S2 . Ni1 . 95.00(9) yes C14 . C150 . C151 . 73.8(8) yes C14 . C150 . C160 . 115.3(12) yes C151 . C150 . C160 . 43.2(8) yes C14 . C150 . C161 . 138.8(11) yes C151 . C150 . C161 . 69.8(7) yes C160 . C150 . C161 . 26.8(6) yes C14 . C150 . H1501 . 122.8 no C151 . C150 . H1501 . 159.9 no C160 . C150 . H1501 . 122.0 no C161 . C150 . H1501 . 97.2 no C14 . C151 . C150 . 64.7(7) yes C14 . C151 . C160 . 147.8(9) yes C150 . C151 . C160 . 87.3(8) yes C14 . C151 . C161 . 125.7(6) yes C150 . C151 . C161 . 64.5(7) yes C160 . C151 . C161 . 23.1(8) yes C14 . C151 . H1602 . 142.0 no C150 . C151 . H1602 . 139.3 no C160 . C151 . H1602 . 55.3 no C161 . C151 . H1602 . 76.6 no C14 . C151 . H1511 . 117.8 no C150 . C151 . H1511 . 160.4 no C160 . C151 . H1511 . 93.9 no C161 . C151 . H1511 . 116.5 no H1602 . C151 . H1511 . 51.8 no C150 . C160 . C151 . 49.5(8) yes C150 . C160 . H1601 . 119.2 no C151 . C160 . H1601 . 162.6 no C150 . C160 . H1602 . 121.3 no C151 . C160 . H1602 . 73.9 no H1601 . C160 . H1602 . 119.5 no C150 . C160 . H1612 . 130.2 no C151 . C160 . H1612 . 169.5 no H1601 . C160 . H1612 . 11.2 no H1602 . C160 . H1612 . 108.4 no C151 . C161 . C150 . 45.7(6) yes C151 . C161 . H1601 . 124.2 no C150 . C161 . H1601 . 153.2 no C151 . C161 . H1611 . 119.5 no C150 . C161 . H1611 . 76.5 no H1601 . C161 . H1611 . 115.5 no C151 . C161 . H1612 . 120.8 no C150 . C161 . H1612 . 157.9 no H1601 . C161 . H1612 . 9.1 no H1611 . C161 . H1612 . 119.6 no C160 . H1601 . C161 . 37.0 no C151 . H1602 . C160 . 50.7 no C160 . H1612 . C161 . 32.8 no #===END ###################################### ## denoted 2.DABCO in text ## ###################################### data_2 _database_code_depnum_ccdc_archive 'CCDC 642485' _audit_creation_date 07-03-31 _audit_creation_method CRYSTALS_ver_12.80 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 13.7520(10) _cell_length_b 15.1762(11) _cell_length_c 15.7383(11) _cell_angle_alpha 82.3090(10) _cell_angle_beta 74.4080(10) _cell_angle_gamma 68.6340(10) _cell_volume 2944.0(4) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Zn 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 _chemical_formula_sum 'C58 H72 N16 O1.50 S4 Zn2' _chemical_formula_moiety 'C58 H72 N16 O1.50 S4 Zn2' _chemical_compound_source ? _chemical_formula_weight 1276.34 _cell_measurement_reflns_used 31331 _cell_measurement_theta_min 1 _cell_measurement_theta_max 30 _cell_measurement_temperature 150 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_min 0.01 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_max 0.02 _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 1.014 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_radiation_wavelength 0.6709 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART APEX2 CCD diffractometer' _diffrn_measurement_method 'fine-slice \w scans' _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 31331 _reflns_number_total 15676 _diffrn_reflns_av_R_equivalents 0.044 # Number of reflections with Friedels Law is 15676 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 15970 _diffrn_reflns_theta_min 1.307 _diffrn_reflns_theta_max 28.330 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.214 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -17 _reflns_limit_h_max 18 _reflns_limit_k_min -20 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.08 _refine_diff_density_max 1.77 _refine_ls_number_reflns 8727 _refine_ls_number_restraints 15 _refine_ls_number_parameters 757 #_refine_ls_R_factor_ref 0.0627 _refine_ls_wR_factor_ref 0.0714 _refine_ls_goodness_of_fit_ref 1.0479 #_reflns_number_all 15643 _refine_ls_R_factor_all 0.1018 _refine_ls_wR_factor_all 0.0853 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 8727 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_gt 0.0714 _refine_ls_shift/su_max 0.039186 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.987 0.830 0.673 ; # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # Insert your own references if required - in alphabetical order _publ_section_references ; Data collection: APEX2, Bruker AXS Inc., Madison, USA, 2004 Data reduction (frames integration): SAINT, Bruker AXS Inc., Madison, USA, 2004 Cell refinement: SAINT, Bruker AXS Inc., Madison, USA, 2004 Absorption correction: SADABS, Bruker AXS Inc., Madison, USA, 2004 Station 9.8: R. J. Cernik, W. Clegg, C. R. A. Catlow, G. Bushnell-Wye, J. V. Flaherty, G. N. Greaves, M. Hamichi, I. Burrows, D. J. Taylor and S. J. Teat, J. Synchotron Radiation 1997, 4, 279-286; 7, 40. Synchrotron chemical crystallography: W. Clegg, J. Chem. Soc., Dalton Trans. 2000, 3223-3232. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of G\"ottingen, Federal Republic of Germany. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Zn1 Zn 0.00389(4) 0.80144(3) 0.04809(3) 0.0367 1.0000 Uani . . . . . . Zn2 Zn 0.16165(4) 0.79901(3) 0.47024(3) 0.0323 1.0000 Uani . . . . . . S1 S 0.2019(2) 0.82548(13) 0.03546(13) 0.0850 1.0000 Uani . . . . . . S2 S -0.05406(10) 0.85600(7) -0.07998(7) 0.0395 1.0000 Uani . . . . . . S101 S -0.04477(12) 0.80659(10) 0.48148(10) 0.0582 1.0000 Uani . . . . . . S102 S 0.17906(8) 0.84216(8) 0.59916(7) 0.0391 1.0000 Uani . . . . . . N1 N -0.0621(3) 0.6978(2) 0.0483(2) 0.0372 1.0000 Uani . . . . . . N2 N -0.1314(3) 0.7117(2) -0.0041(2) 0.0401 1.0000 Uani . . . . . . N3 N -0.1995(3) 0.8030(3) -0.1159(2) 0.0407 1.0000 Uani . . . . . . N4 N 0.1099(3) 0.6255(3) 0.1597(3) 0.0443 1.0000 Uani . . . . . . N5 N 0.1112(3) 0.7070(3) 0.1100(3) 0.0446 1.0000 Uani . . . . . . N6 N 0.2797(4) 0.6765(3) 0.1385(3) 0.0545 1.0000 Uani . . . . . . N7 N -0.1061(3) 0.9016(2) 0.1414(2) 0.0332 1.0000 Uani . . . . . . N8 N -0.2405(3) 1.0278(3) 0.2512(3) 0.0426 1.0000 Uani . . . . . . N101 N 0.2147(3) 0.6240(3) 0.3629(3) 0.0401 1.0000 Uani . . . . . . N102 N 0.1437(3) 0.6993(3) 0.4115(3) 0.0404 1.0000 Uani . . . . . . N103 N 0.0077(3) 0.6587(3) 0.3810(3) 0.0472 1.0000 Uani . . . . . . N104 N 0.3215(3) 0.7124(2) 0.4613(2) 0.0329 1.0000 Uani . . . . . . N105 N 0.3814(3) 0.7361(2) 0.5052(2) 0.0353 1.0000 Uani . . . . . . N106 N 0.3702(3) 0.8277(3) 0.6136(3) 0.0443 1.0000 Uani . . . . . . N107 N 0.1790(3) 0.9064(2) 0.3729(2) 0.0302 1.0000 Uani . . . . . . N108 N 0.2043(3) 1.0352(2) 0.2526(2) 0.0363 1.0000 Uani . . . . . . C1 C -0.0413(4) 0.6187(3) 0.0955(3) 0.0381 1.0000 Uani . . . . . . C2 C 0.0367(4) 0.5915(3) 0.1539(3) 0.0447 1.0000 Uani . . . . . . C3 C 0.0290(4) 0.5036(3) 0.2011(3) 0.0417 1.0000 Uani . . . . . . C4 C 0.0751(4) 0.4480(4) 0.2668(4) 0.0521 1.0000 Uani . . . . . . C5 C 0.0497(5) 0.3658(4) 0.2994(4) 0.0604 1.0000 Uani . . . . . . C6 C -0.0168(4) 0.3385(3) 0.2654(4) 0.0588 1.0000 Uani . . . . . . C7 C -0.0641(4) 0.3926(3) 0.1957(3) 0.0480 1.0000 Uani . . . . . . C8 C -0.1312(4) 0.3736(3) 0.1536(4) 0.0553 1.0000 Uani . . . . . . C9 C -0.1723(4) 0.4358(3) 0.0903(4) 0.0493 1.0000 Uani . . . . . . C10 C -0.1506(4) 0.5214(3) 0.0641(3) 0.0435 1.0000 Uani . . . . . . C11 C -0.0833(4) 0.5408(3) 0.1043(3) 0.0387 1.0000 Uani . . . . . . C12 C -0.0402(4) 0.4769(3) 0.1687(3) 0.0428 1.0000 Uani . . . . . . C13 C -0.1321(3) 0.7841(3) -0.0624(3) 0.0348 1.0000 Uani . . . . . . C14 C -0.2653(4) 0.7449(4) -0.1121(3) 0.0495 1.0000 Uani . . . . . . C15 C -0.3251(5) 0.7785(4) -0.1814(4) 0.0586 1.0000 Uani . . . . . . C16 C -0.4311(6) 0.8080(5) -0.1643(6) 0.0790 1.0000 Uani . . . . . . C17 C 0.2000(4) 0.7268(4) 0.1004(3) 0.0526 1.0000 Uani . . . . . . C18 C 0.3826(5) 0.6896(5) 0.1205(4) 0.0604 1.0000 Uani . . . . . . C19 C 0.4602(6) 0.6391(6) 0.0416(5) 0.0817 1.0000 Uani . . . . . . C20 C 0.5552(7) 0.5781(7) 0.0427(7) 0.1015 1.0000 Uani . . . . . . C21 C -0.1008(4) 0.8691(4) 0.2343(3) 0.0509 1.0000 Uani . . . . . . C22 C -0.0829(5) 0.9909(4) 0.1232(4) 0.0585 1.0000 Uani . . . . . . C23 C -0.2172(4) 0.9220(4) 0.1349(4) 0.0561 1.0000 Uani . . . . . . C24 C -0.1828(4) 0.9437(4) 0.2983(3) 0.0484 1.0000 Uani . . . . . . C25 C -0.1612(5) 1.0653(4) 0.1897(4) 0.0540 1.0000 Uani . . . . . . C26 C -0.2962(4) 0.9994(4) 0.1986(4) 0.0538 1.0000 Uani . . . . . . C101 C 0.3145(3) 0.6027(3) 0.3634(3) 0.0345 1.0000 Uani . . . . . . C102 C 0.3713(3) 0.6389(3) 0.4124(3) 0.0320 1.0000 Uani . . . . . . C103 C 0.4831(3) 0.5741(3) 0.3977(3) 0.0312 1.0000 Uani . . . . . . C104 C 0.5719(3) 0.5650(3) 0.4287(3) 0.0368 1.0000 Uani . . . . . . C105 C 0.6674(4) 0.4892(3) 0.4004(3) 0.0447 1.0000 Uani . . . . . . C106 C 0.6765(4) 0.4244(3) 0.3443(3) 0.0463 1.0000 Uani . . . . . . C107 C 0.5902(4) 0.4314(3) 0.3093(3) 0.0404 1.0000 Uani . . . . . . C108 C 0.5873(4) 0.3714(3) 0.2484(4) 0.0510 1.0000 Uani . . . . . . C109 C 0.4946(5) 0.3862(4) 0.2240(4) 0.0546 1.0000 Uani . . . . . . C110 C 0.3970(4) 0.4609(4) 0.2574(3) 0.0468 1.0000 Uani . . . . . . C111 C 0.3973(4) 0.5214(3) 0.3148(3) 0.0364 1.0000 Uani . . . . . . C112 C 0.4951(3) 0.5065(3) 0.3387(3) 0.0339 1.0000 Uani . . . . . . C113 C 0.0385(3) 0.7124(3) 0.4197(3) 0.0400 1.0000 Uani . . . . . . C114 C -0.1027(4) 0.6638(4) 0.3936(4) 0.0549 1.0000 Uani . . . . . . C115 C -0.1316(4) 0.5920(4) 0.4620(4) 0.0573 1.0000 Uani . . . . . . C116 C -0.2122(6) 0.6141(6) 0.5302(5) 0.0769 1.0000 Uani . . . . . . C117 C 0.3212(3) 0.7971(3) 0.5681(3) 0.0354 1.0000 Uani . . . . . . C118 C 0.4874(4) 0.7971(4) 0.5977(4) 0.0508 1.0000 Uani . . . . . . C119 C 0.5307(7) 0.8634(7) 0.5446(7) 0.0954 1.0000 Uani . . . . . . C120 C 0.6011(9) 0.8959(8) 0.5520(9) 0.1216 1.0000 Uani . . . . . . C121 C 0.2653(5) 0.9397(4) 0.3815(4) 0.0551 1.0000 Uani . . . . . . C122 C 0.0795(4) 0.9900(3) 0.3808(3) 0.0491 1.0000 Uani . . . . . . C123 C 0.2084(4) 0.8704(3) 0.2835(3) 0.0472 1.0000 Uani . . . . . . C124 C 0.2752(5) 1.0200(4) 0.3129(4) 0.0606 1.0000 Uani . . . . . . C125 C 0.0930(4) 1.0640(3) 0.3061(3) 0.0522 1.0000 Uani . . . . . . C126 C 0.2288(5) 0.9467(3) 0.2122(3) 0.0516 1.0000 Uani . . . . . . C201 C 0.6487(7) 0.7777(6) 0.3112(7) 0.1032 1.0000 Uani D . . . . . C202 C 0.7068(5) 0.6967(5) 0.2579(5) 0.0743 1.0000 Uani D . . . . . C203 C 0.6337(6) 0.6929(5) 0.2037(5) 0.0757 1.0000 Uani D . . . . . C204 C 0.5313(5) 0.7709(5) 0.2369(6) 0.0805 1.0000 Uani D . . . . . C205 C 0.4271(13) 0.9959(12) 0.0192(13) 0.0701 0.5000 Uani D . . . . . C206 C 0.5330(14) 0.9654(12) 0.0506(15) 0.0761 0.5000 Uani D . . . . . C207 C 0.5970(13) 1.0238(13) -0.0104(17) 0.0968 0.5000 Uani D . . . . . C209 C 0.4438(14) 1.0648(12) -0.0598(13) 0.0711 0.5000 Uani D . . . . . O1 O 0.5568(4) 0.8307(4) 0.2818(5) 0.1163 1.0000 Uani D . . . . . O2 O 0.5243(6) 1.0976(5) -0.0505(5) 0.0579 0.5000 Uani D . . . . . H41 H 0.1236 0.4655 0.2890 0.0684 1.0000 Uiso . . . . . . H51 H 0.0792 0.3293 0.3458 0.0771 1.0000 Uiso . . . . . . H61 H -0.0306 0.2833 0.2877 0.0729 1.0000 Uiso . . . . . . H81 H -0.1480 0.3180 0.1691 0.0711 1.0000 Uiso . . . . . . H91 H -0.2167 0.4197 0.0630 0.0700 1.0000 Uiso . . . . . . H101 H -0.1807 0.5626 0.0206 0.0612 1.0000 Uiso . . . . . . H141 H -0.3159 0.7506 -0.0546 0.0789 1.0000 Uiso . . . . . . H142 H -0.2191 0.6796 -0.1201 0.0792 1.0000 Uiso . . . . . . H151 H -0.2865 0.7784 -0.2407 0.0920 1.0000 Uiso . . . . . . H161 H -0.4688 0.8300 -0.2096 0.1180 1.0000 Uiso . . . . . . H162 H -0.4727 0.8089 -0.1046 0.1178 1.0000 Uiso . . . . . . H181 H 0.3698 0.7576 0.1079 0.0921 1.0000 Uiso . . . . . . H182 H 0.4122 0.6713 0.1729 0.0918 1.0000 Uiso . . . . . . H191 H 0.4390 0.6523 -0.0117 0.1250 1.0000 Uiso . . . . . . H201 H 0.5785 0.5628 0.0949 0.1540 1.0000 Uiso . . . . . . H202 H 0.6011 0.5479 -0.0084 0.1542 1.0000 Uiso . . . . . . H211 H -0.0300 0.8624 0.2388 0.0723 1.0000 Uiso . . . . . . H212 H -0.1125 0.8077 0.2483 0.0727 1.0000 Uiso . . . . . . H221 H -0.0085 0.9784 0.1240 0.0870 1.0000 Uiso . . . . . . H222 H -0.0912 1.0146 0.0638 0.0874 1.0000 Uiso . . . . . . H231 H -0.2228 0.9432 0.0743 0.0831 1.0000 Uiso . . . . . . H232 H -0.2346 0.8627 0.1503 0.0831 1.0000 Uiso . . . . . . H241 H -0.1473 0.9629 0.3343 0.0712 1.0000 Uiso . . . . . . H242 H -0.2364 0.9185 0.3371 0.0714 1.0000 Uiso . . . . . . H251 H -0.1230 1.0863 0.2224 0.0787 1.0000 Uiso . . . . . . H252 H -0.1980 1.1205 0.1561 0.0792 1.0000 Uiso . . . . . . H261 H -0.3300 1.0539 0.1637 0.0791 1.0000 Uiso . . . . . . H262 H -0.3524 0.9774 0.2382 0.0790 1.0000 Uiso . . . . . . H1041 H 0.5673 0.6093 0.4677 0.0525 1.0000 Uiso . . . . . . H1051 H 0.7280 0.4824 0.4210 0.0605 1.0000 Uiso . . . . . . H1061 H 0.7415 0.3736 0.3291 0.0600 1.0000 Uiso . . . . . . H1081 H 0.6509 0.3198 0.2248 0.0697 1.0000 Uiso . . . . . . H1091 H 0.4943 0.3460 0.1828 0.0792 1.0000 Uiso . . . . . . H1101 H 0.3333 0.4679 0.2404 0.0698 1.0000 Uiso . . . . . . H1141 H -0.1523 0.7291 0.4127 0.0876 1.0000 Uiso . . . . . . H1142 H -0.1130 0.6527 0.3378 0.0880 1.0000 Uiso . . . . . . H1151 H -0.0882 0.5276 0.4540 0.0891 1.0000 Uiso . . . . . . H1161 H -0.2566 0.6769 0.5404 0.1147 1.0000 Uiso . . . . . . H1162 H -0.2264 0.5653 0.5712 0.1153 1.0000 Uiso . . . . . . H1191 H 0.5038 0.8873 0.4919 0.1403 1.0000 Uiso . . . . . . H1201 H 0.6313 0.8782 0.6018 0.1992 1.0000 Uiso . . . . . . H1202 H 0.6214 0.9415 0.5116 0.1990 1.0000 Uiso . . . . . . H1211 H 0.2484 0.9629 0.4402 0.0947 1.0000 Uiso . . . . . . H1212 H 0.3330 0.8870 0.3717 0.0951 1.0000 Uiso . . . . . . H1221 H 0.0635 1.0177 0.4377 0.0614 1.0000 Uiso . . . . . . H1222 H 0.0206 0.9693 0.3795 0.0620 1.0000 Uiso . . . . . . H1231 H 0.2716 0.8126 0.2784 0.0687 1.0000 Uiso . . . . . . H1232 H 0.1473 0.8565 0.2757 0.0694 1.0000 Uiso . . . . . . H1241 H 0.2538 1.0784 0.3446 0.1042 1.0000 Uiso . . . . . . H1242 H 0.3490 1.0057 0.2789 0.1040 1.0000 Uiso . . . . . . H1251 H 0.0729 1.1256 0.3313 0.0650 1.0000 Uiso . . . . . . H1252 H 0.0447 1.0707 0.2681 0.0655 1.0000 Uiso . . . . . . H1261 H 0.3028 0.9249 0.1783 0.0723 1.0000 Uiso . . . . . . H1262 H 0.1811 0.9579 0.1719 0.0721 1.0000 Uiso . . . . . . H2011 H 0.6920 0.8151 0.3073 0.1530 1.0000 Uiso . . . . . . H2012 H 0.6291 0.7559 0.3735 0.1533 1.0000 Uiso . . . . . . H2031 H 0.6624 0.7029 0.1404 0.1061 1.0000 Uiso . . . . . . H2032 H 0.6226 0.6319 0.2127 0.1062 1.0000 Uiso . . . . . . H2041 H 0.5020 0.8073 0.1868 0.1163 1.0000 Uiso . . . . . . H2042 H 0.4768 0.7451 0.2759 0.1160 1.0000 Uiso . . . . . . H8 H 0.5068 0.7910 0.6546 0.0727 1.0000 Uiso . . . . . . H12 H 0.3320 0.8669 0.6550 0.0665 1.0000 Uiso . . . . . . H28 H -0.2045 0.8506 -0.1541 0.0626 1.0000 Uiso . . . . . . H45 H 0.2732 0.6271 0.1708 0.0825 1.0000 Uiso . . . . . . H78 H 0.0577 0.6157 0.3466 0.0727 1.0000 Uiso . . . . . . H87 H 0.5201 0.7359 0.5689 0.0731 1.0000 Uiso . . . . . . H2091 H 0.3758 1.1197 -0.0618 0.0945 0.5000 Uiso . . . . . . H2092 H 0.4687 1.0321 -0.1187 0.0945 0.5000 Uiso . . . . . . H2051 H 0.3622 1.0265 0.0653 0.0778 0.5000 Uiso . . . . . . H2052 H 0.4178 0.9384 -0.0011 0.0778 0.5000 Uiso . . . . . . H2061 H 0.5168 0.9810 0.1145 0.0850 0.5000 Uiso . . . . . . H2062 H 0.5740 0.8956 0.0452 0.0850 0.5000 Uiso . . . . . . H2071 H 0.6307 1.0517 0.0251 0.1149 0.5000 Uiso . . . . . . H2072 H 0.6577 0.9835 -0.0562 0.1149 0.5000 Uiso . . . . . . H2021 H 0.7745 0.7036 0.2185 0.0896 1.0000 Uiso . . . . . . H2022 H 0.7258 0.6375 0.2961 0.0896 1.0000 Uiso . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0457(3) 0.0289(2) 0.0345(3) 0.00190(18) -0.0152(2) -0.0087(2) Zn2 0.0327(2) 0.0277(2) 0.0354(2) -0.00139(17) -0.01060(19) -0.00735(17) S1 0.1392(17) 0.0628(9) 0.0744(11) 0.0166(8) -0.0541(12) -0.0457(11) S2 0.0528(6) 0.0361(5) 0.0361(5) 0.0060(4) -0.0168(5) -0.0209(5) S101 0.0612(8) 0.0515(7) 0.0574(8) -0.0058(6) -0.0165(6) -0.0114(6) S102 0.0336(5) 0.0405(5) 0.0389(5) -0.0076(4) -0.0087(4) -0.0056(4) N1 0.048(2) 0.0298(16) 0.0325(17) -0.0032(13) -0.0080(15) -0.0125(15) N2 0.051(2) 0.0313(17) 0.0376(18) 0.0001(14) -0.0074(16) -0.0167(16) N3 0.051(2) 0.0382(18) 0.0389(19) 0.0028(15) -0.0118(16) -0.0230(16) N4 0.052(2) 0.0362(18) 0.0385(19) -0.0019(15) -0.0114(17) -0.0082(17) N5 0.055(2) 0.0364(18) 0.043(2) 0.0018(15) -0.0164(18) -0.0142(17) N6 0.059(3) 0.064(3) 0.050(2) 0.009(2) -0.021(2) -0.029(2) N7 0.0369(18) 0.0303(16) 0.0348(17) -0.0015(13) -0.0109(14) -0.0125(14) N8 0.045(2) 0.0429(19) 0.041(2) -0.0067(16) -0.0092(16) -0.0151(16) N101 0.0342(18) 0.0406(19) 0.044(2) 0.0017(15) -0.0087(15) -0.0133(15) N102 0.0365(19) 0.0393(18) 0.047(2) 0.0002(15) -0.0141(16) -0.0131(15) N103 0.040(2) 0.053(2) 0.053(2) -0.0042(18) -0.0108(17) -0.0209(18) N104 0.0296(16) 0.0327(15) 0.0326(16) 0.0009(13) -0.0093(13) -0.0057(13) N105 0.0323(17) 0.0352(17) 0.0373(18) -0.0013(14) -0.0145(14) -0.0060(13) N106 0.0348(19) 0.048(2) 0.052(2) -0.0133(17) -0.0153(17) -0.0087(16) N107 0.0294(16) 0.0271(14) 0.0315(16) -0.0030(12) -0.0097(13) -0.0042(12) N108 0.0383(18) 0.0349(17) 0.0342(17) 0.0055(14) -0.0129(15) -0.0103(14) C1 0.047(2) 0.0256(17) 0.036(2) -0.0019(15) -0.0061(18) -0.0089(16) C2 0.052(3) 0.038(2) 0.041(2) -0.0017(18) -0.006(2) -0.015(2) C3 0.041(2) 0.0307(19) 0.044(2) -0.0003(17) -0.0018(18) -0.0074(17) C4 0.046(3) 0.040(2) 0.057(3) 0.004(2) -0.009(2) -0.004(2) C5 0.054(3) 0.037(2) 0.068(3) 0.017(2) -0.006(3) -0.003(2) C6 0.051(3) 0.031(2) 0.069(3) 0.016(2) 0.003(3) -0.004(2) C7 0.043(2) 0.0241(18) 0.057(3) 0.0026(18) 0.009(2) -0.0049(17) C8 0.043(3) 0.034(2) 0.074(3) -0.007(2) 0.012(2) -0.0125(19) C9 0.048(3) 0.033(2) 0.061(3) -0.009(2) 0.001(2) -0.0143(19) C10 0.042(2) 0.038(2) 0.043(2) -0.0088(18) 0.0028(19) -0.0111(18) C11 0.040(2) 0.0257(17) 0.038(2) -0.0039(15) 0.0043(17) -0.0065(16) C12 0.042(2) 0.0286(19) 0.042(2) -0.0004(16) 0.0037(18) -0.0043(17) C13 0.042(2) 0.0290(18) 0.0332(19) -0.0041(15) -0.0097(17) -0.0112(16) C14 0.063(3) 0.047(3) 0.048(3) -0.003(2) -0.013(2) -0.030(2) C15 0.061(3) 0.061(3) 0.066(3) 0.003(3) -0.024(3) -0.031(3) C16 0.072(4) 0.077(4) 0.103(5) -0.017(4) -0.042(4) -0.023(3) C17 0.058(3) 0.072(3) 0.041(2) -0.006(2) -0.016(2) -0.033(3) C18 0.057(3) 0.082(4) 0.056(3) -0.008(3) -0.019(3) -0.034(3) C19 0.066(4) 0.122(6) 0.073(4) -0.022(4) -0.010(3) -0.049(4) C20 0.065(5) 0.120(7) 0.131(7) -0.053(6) -0.019(5) -0.031(5) C21 0.056(3) 0.055(3) 0.036(2) 0.002(2) -0.017(2) -0.011(2) C22 0.072(4) 0.038(2) 0.059(3) -0.015(2) 0.013(3) -0.028(2) C23 0.046(3) 0.066(3) 0.059(3) -0.022(3) -0.019(2) -0.011(2) C24 0.053(3) 0.057(3) 0.036(2) -0.003(2) -0.012(2) -0.019(2) C25 0.067(3) 0.044(2) 0.048(3) -0.011(2) 0.008(2) -0.028(2) C26 0.042(3) 0.060(3) 0.058(3) -0.017(2) -0.020(2) -0.006(2) C101 0.033(2) 0.0334(19) 0.035(2) 0.0038(15) -0.0090(16) -0.0108(16) C102 0.0297(19) 0.0309(18) 0.0331(19) 0.0028(15) -0.0096(15) -0.0075(15) C103 0.0271(18) 0.0270(17) 0.0335(19) 0.0030(14) -0.0041(15) -0.0061(14) C104 0.031(2) 0.038(2) 0.039(2) 0.0033(16) -0.0082(16) -0.0101(16) C105 0.032(2) 0.044(2) 0.052(3) 0.009(2) -0.0099(19) -0.0095(18) C106 0.030(2) 0.041(2) 0.053(3) 0.006(2) -0.0024(19) -0.0026(18) C107 0.039(2) 0.0301(19) 0.044(2) -0.0012(16) 0.0012(18) -0.0102(16) C108 0.055(3) 0.037(2) 0.053(3) -0.011(2) 0.006(2) -0.017(2) C109 0.069(3) 0.043(2) 0.053(3) -0.011(2) -0.005(2) -0.024(2) C110 0.053(3) 0.050(3) 0.045(2) 0.001(2) -0.012(2) -0.027(2) C111 0.040(2) 0.0343(19) 0.037(2) 0.0023(15) -0.0115(17) -0.0157(17) C112 0.0326(19) 0.0279(18) 0.038(2) 0.0026(15) -0.0057(16) -0.0099(15) C113 0.030(2) 0.047(2) 0.041(2) 0.0115(18) -0.0134(17) -0.0120(18) C114 0.049(3) 0.070(3) 0.058(3) 0.009(3) -0.024(2) -0.031(3) C115 0.048(3) 0.065(3) 0.067(3) 0.004(3) -0.024(3) -0.023(2) C116 0.074(4) 0.093(5) 0.072(4) 0.006(4) -0.019(4) -0.041(4) C117 0.031(2) 0.0350(19) 0.036(2) 0.0019(16) -0.0106(16) -0.0066(16) C118 0.041(2) 0.056(3) 0.057(3) -0.007(2) -0.020(2) -0.012(2) C119 0.067(4) 0.101(6) 0.122(7) 0.002(5) -0.030(4) -0.030(4) C120 0.108(7) 0.127(8) 0.170(10) 0.017(7) -0.064(7) -0.072(7) C121 0.061(3) 0.064(3) 0.065(3) 0.028(3) -0.040(3) -0.042(3) C122 0.043(2) 0.036(2) 0.046(2) 0.0101(19) -0.003(2) 0.0020(19) C123 0.064(3) 0.038(2) 0.037(2) -0.0045(18) -0.006(2) -0.018(2) C124 0.076(4) 0.061(3) 0.071(4) 0.029(3) -0.046(3) -0.044(3) C125 0.047(3) 0.045(2) 0.041(2) 0.008(2) -0.004(2) 0.003(2) C126 0.068(3) 0.041(2) 0.037(2) 0.0001(19) -0.002(2) -0.016(2) C201 0.105(6) 0.082(5) 0.132(7) -0.043(5) -0.066(6) -0.002(4) C202 0.056(3) 0.072(4) 0.091(5) -0.009(3) -0.015(3) -0.018(3) C203 0.067(4) 0.081(4) 0.076(4) -0.014(3) -0.011(3) -0.023(3) C204 0.057(4) 0.075(4) 0.116(6) -0.001(4) -0.029(4) -0.026(3) C205 0.063(9) 0.058(8) 0.074(11) 0.000(7) 0.003(7) -0.018(7) C206 0.094(14) 0.046(10) 0.070(10) 0.004(7) -0.011(9) -0.011(9) C207 0.071(12) 0.115(19) 0.105(15) -0.025(13) -0.014(10) -0.031(11) C209 0.064(9) 0.059(13) 0.085(12) -0.011(9) -0.009(8) -0.019(10) O1 0.069(3) 0.092(4) 0.186(7) -0.056(4) -0.012(4) -0.021(3) O2 0.050(4) 0.068(5) 0.062(4) 0.003(4) -0.020(3) -0.025(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1740(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 . S1 . 2.829(2) yes Zn1 . S2 . 2.3063(11) yes Zn1 . N1 . 2.082(4) yes Zn1 . N5 . 2.010(4) yes Zn1 . N7 . 2.117(3) yes Zn2 . S101 . 2.7568(16) yes Zn2 . S102 . 2.3095(12) yes Zn2 . N102 . 1.994(4) yes Zn2 . N104 . 2.087(3) yes Zn2 . N107 . 2.116(3) yes S1 . C17 . 1.701(6) yes S2 . C13 . 1.741(4) yes S101 . C113 . 1.697(5) yes S102 . C117 . 1.768(4) yes N1 . N2 . 1.365(5) yes N1 . C1 . 1.303(5) yes N2 . C13 . 1.331(5) yes N3 . C13 . 1.346(6) yes N3 . C14 . 1.462(6) yes N3 . H28 . 0.870 no N4 . N5 . 1.375(5) yes N4 . C2 . 1.314(7) yes N5 . C17 . 1.328(7) yes N6 . C17 . 1.328(7) yes N6 . C18 . 1.448(7) yes N6 . H45 . 0.866 no N7 . C21 . 1.493(6) yes N7 . C22 . 1.477(6) yes N7 . C23 . 1.473(6) yes N8 . C24 . 1.460(6) yes N8 . C25 . 1.479(6) yes N8 . C26 . 1.463(6) yes N101 . N102 . 1.365(5) yes N101 . C101 . 1.293(6) yes N102 . C113 . 1.358(6) yes N103 . C113 . 1.318(6) yes N103 . C114 . 1.452(6) yes N103 . H78 . 0.871 no N104 . N105 . 1.369(5) yes N104 . C102 . 1.302(5) yes N105 . C117 . 1.329(6) yes N106 . C117 . 1.327(6) yes N106 . C118 . 1.465(6) yes N106 . H12 . 0.863 no N107 . C121 . 1.490(6) yes N107 . C122 . 1.477(5) yes N107 . C123 . 1.477(6) yes N108 . C124 . 1.475(6) yes N108 . C125 . 1.469(6) yes N108 . C126 . 1.452(6) yes C1 . C2 . 1.508(7) yes C1 . C11 . 1.471(6) yes C2 . C3 . 1.462(6) yes C3 . C4 . 1.382(7) yes C3 . C12 . 1.389(7) yes C4 . C5 . 1.411(8) yes C4 . H41 . 0.959 no C5 . C6 . 1.376(9) yes C5 . H51 . 0.945 no C6 . C7 . 1.434(8) yes C6 . H61 . 0.928 no C7 . C8 . 1.396(8) yes C7 . C12 . 1.419(6) yes C8 . C9 . 1.366(8) yes C8 . H81 . 0.938 no C9 . C10 . 1.422(6) yes C9 . H91 . 0.947 no C10 . C11 . 1.381(7) yes C10 . H101 . 0.938 no C11 . C12 . 1.399(6) yes C14 . C15 . 1.467(8) yes C14 . H141 . 0.975 no C14 . H142 . 0.967 no C15 . C16 . 1.320(9) yes C15 . H151 . 0.941 no C16 . H161 . 0.947 no C16 . H162 . 0.960 no C18 . C19 . 1.488(9) yes C18 . H181 . 0.983 no C18 . H182 . 0.980 no C19 . C20 . 1.301(12) yes C19 . H191 . 0.935 no C20 . H201 . 0.932 no C20 . H202 . 0.933 no C21 . C24 . 1.527(7) yes C21 . H211 . 0.963 no C21 . H212 . 0.987 no C22 . C25 . 1.534(7) yes C22 . H221 . 0.974 no C22 . H222 . 0.977 no C23 . C26 . 1.537(7) yes C23 . H231 . 0.979 no C23 . H232 . 0.997 no C24 . H241 . 0.971 no C24 . H242 . 0.982 no C25 . H251 . 0.977 no C25 . H252 . 0.977 no C26 . H261 . 0.968 no C26 . H262 . 0.985 no C101 . C102 . 1.502(6) yes C101 . C111 . 1.471(6) yes C102 . C103 . 1.467(5) yes C103 . C104 . 1.389(6) yes C103 . C112 . 1.410(6) yes C104 . C105 . 1.402(6) yes C104 . H1041 . 0.944 no C105 . C106 . 1.360(8) yes C105 . H1051 . 0.940 no C106 . C107 . 1.402(7) yes C106 . H1061 . 0.939 no C107 . C108 . 1.426(7) yes C107 . C112 . 1.398(6) yes C108 . C109 . 1.362(8) yes C108 . H1081 . 0.960 no C109 . C110 . 1.426(8) yes C109 . H1091 . 0.950 no C110 . C111 . 1.374(6) yes C110 . H1101 . 0.949 no C111 . C112 . 1.424(6) yes C114 . C115 . 1.509(8) yes C114 . H1141 . 1.007 no C114 . H1142 . 0.973 no C115 . C116 . 1.295(9) yes C115 . H1151 . 0.945 no C116 . H1161 . 0.934 no C116 . H1162 . 0.956 no C118 . C119 . 1.417(11) yes C118 . H8 . 0.985 no C118 . H87 . 0.984 no C119 . C120 . 1.273(12) yes C119 . H1191 . 0.971 no C120 . H1201 . 0.947 no C120 . H1202 . 0.942 no C121 . C124 . 1.536(7) yes C121 . H1211 . 0.972 no C121 . H1212 . 0.971 no C122 . C125 . 1.535(6) yes C122 . H1221 . 0.977 no C122 . H1222 . 0.977 no C123 . C126 . 1.548(7) yes C123 . H1231 . 0.978 no C123 . H1232 . 0.979 no C124 . H1241 . 0.985 no C124 . H1242 . 0.970 no C125 . H1251 . 0.981 no C125 . H1252 . 0.979 no C126 . H1261 . 0.970 no C126 . H1262 . 0.988 no C201 . C202 . 1.433(10) yes C201 . O1 . 1.390(7) yes C201 . H2011 . 0.948 no C201 . H2012 . 0.989 no C202 . C203 . 1.503(10) yes C202 . H2021 . 1.002 no C202 . H2022 . 1.002 no C203 . C204 . 1.487(10) yes C203 . H2031 . 0.982 no C203 . H2032 . 0.978 no C204 . O1 . 1.408(7) yes C204 . H2041 . 0.990 no C204 . H2042 . 0.997 no C205 . H2072 2_675 1.103 no C205 . O2 2_675 1.414(18) yes C205 . C206 2_675 1.26(3) yes C205 . C206 . 1.554(9) yes C205 . C209 . 1.538(9) yes C205 . H2051 . 0.990 no C205 . H2052 . 1.028 no C206 . H2092 2_675 1.071 no C206 . O2 2_675 1.44(2) yes C206 . C207 . 1.538(9) yes C206 . H2061 . 1.012 no C206 . H2062 . 1.006 no C207 . H2051 2_675 1.117 no C207 . C209 2_675 1.78(2) yes C207 . H2052 2_675 0.572 no C207 . O2 . 1.408(9) yes C207 . H2071 . 1.027 no C207 . H2072 . 1.006 no C209 . H2061 2_675 1.074 no C209 . H2062 2_675 0.612 no C209 . O2 . 1.415(9) yes C209 . H2091 . 1.005 no C209 . H2092 . 1.025 no O2 . H2052 2_675 1.226 no O2 . H2062 2_675 1.299 no H2091 . H2062 2_675 0.750 no H2051 . H2072 2_675 0.420 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 . Zn1 . S2 . 110.69(5) yes S1 . Zn1 . N1 . 141.90(11) yes S2 . Zn1 . N1 . 83.88(10) yes S1 . Zn1 . N5 . 60.55(12) yes S2 . Zn1 . N5 . 149.12(12) yes N1 . Zn1 . N5 . 88.55(15) yes S1 . Zn1 . N7 . 103.16(10) yes S2 . Zn1 . N7 . 103.43(9) yes N1 . Zn1 . N7 . 107.36(13) yes N5 . Zn1 . N7 . 107.40(15) yes S101 . Zn2 . S102 . 112.17(4) yes S101 . Zn2 . N102 . 62.22(11) yes S102 . Zn2 . N102 . 145.69(11) yes S101 . Zn2 . N104 . 146.26(10) yes S102 . Zn2 . N104 . 82.72(10) yes N102 . Zn2 . N104 . 88.12(14) yes S101 . Zn2 . N107 . 102.28(9) yes S102 . Zn2 . N107 . 107.18(9) yes N102 . Zn2 . N107 . 107.04(14) yes N104 . Zn2 . N107 . 101.60(13) yes Zn1 . S1 . C17 . 72.20(19) yes Zn1 . S2 . C13 . 93.32(14) yes Zn2 . S101 . C113 . 73.69(16) yes Zn2 . S102 . C117 . 93.39(15) yes Zn1 . N1 . N2 . 119.0(3) yes Zn1 . N1 . C1 . 124.2(3) yes N2 . N1 . C1 . 116.7(4) yes N1 . N2 . C13 . 112.9(4) yes C13 . N3 . C14 . 121.6(4) yes C13 . N3 . H28 . 120.1 no C14 . N3 . H28 . 118.3 no N5 . N4 . C2 . 115.9(4) yes N4 . N5 . Zn1 . 132.0(3) yes N4 . N5 . C17 . 114.2(4) yes Zn1 . N5 . C17 . 113.8(3) yes C17 . N6 . C18 . 125.1(5) yes C17 . N6 . H45 . 117.3 no C18 . N6 . H45 . 117.0 no Zn1 . N7 . C21 . 113.0(3) yes Zn1 . N7 . C22 . 109.4(3) yes C21 . N7 . C22 . 108.0(4) yes Zn1 . N7 . C23 . 110.5(3) yes C21 . N7 . C23 . 107.6(4) yes C22 . N7 . C23 . 108.2(4) yes C24 . N8 . C25 . 108.6(4) yes C24 . N8 . C26 . 108.3(4) yes C25 . N8 . C26 . 107.7(4) yes N102 . N101 . C101 . 115.8(4) yes N101 . N102 . Zn2 . 133.2(3) yes N101 . N102 . C113 . 114.7(4) yes Zn2 . N102 . C113 . 112.0(3) yes C113 . N103 . C114 . 124.9(4) yes C113 . N103 . H78 . 117.4 no C114 . N103 . H78 . 117.7 no Zn2 . N104 . N105 . 118.9(2) yes Zn2 . N104 . C102 . 124.4(3) yes N105 . N104 . C102 . 116.6(3) yes N104 . N105 . C117 . 112.7(3) yes C117 . N106 . C118 . 122.9(4) yes C117 . N106 . H12 . 119.3 no C118 . N106 . H12 . 117.8 no Zn2 . N107 . C121 . 110.3(2) yes Zn2 . N107 . C122 . 112.4(3) yes C121 . N107 . C122 . 107.1(4) yes Zn2 . N107 . C123 . 110.6(3) yes C121 . N107 . C123 . 108.1(4) yes C122 . N107 . C123 . 108.1(3) yes C124 . N108 . C125 . 107.5(4) yes C124 . N108 . C126 . 109.1(4) yes C125 . N108 . C126 . 108.7(4) yes N1 . C1 . C2 . 122.9(4) yes N1 . C1 . C11 . 130.4(4) yes C2 . C1 . C11 . 106.6(4) yes C1 . C2 . N4 . 132.3(4) yes C1 . C2 . C3 . 105.7(4) yes N4 . C2 . C3 . 121.5(4) yes C2 . C3 . C4 . 133.0(5) yes C2 . C3 . C12 . 107.7(4) yes C4 . C3 . C12 . 119.3(4) yes C3 . C4 . C5 . 118.9(5) yes C3 . C4 . H41 . 119.9 no C5 . C4 . H41 . 121.2 no C4 . C5 . C6 . 121.5(5) yes C4 . C5 . H51 . 118.6 no C6 . C5 . H51 . 119.9 no C5 . C6 . C7 . 121.5(5) yes C5 . C6 . H61 . 119.2 no C7 . C6 . H61 . 119.3 no C6 . C7 . C8 . 128.3(5) yes C6 . C7 . C12 . 114.4(5) yes C8 . C7 . C12 . 117.2(5) yes C7 . C8 . C9 . 120.0(4) yes C7 . C8 . H81 . 119.6 no C9 . C8 . H81 . 120.4 no C8 . C9 . C10 . 123.2(5) yes C8 . C9 . H91 . 117.1 no C10 . C9 . H91 . 119.7 no C9 . C10 . C11 . 117.5(5) yes C9 . C10 . H101 . 120.7 no C11 . C10 . H101 . 121.8 no C1 . C11 . C10 . 134.1(4) yes C1 . C11 . C12 . 106.4(4) yes C10 . C11 . C12 . 119.6(4) yes C7 . C12 . C11 . 122.4(5) yes C7 . C12 . C3 . 124.2(4) yes C11 . C12 . C3 . 113.3(4) yes S2 . C13 . N3 . 115.6(3) yes S2 . C13 . N2 . 128.1(3) yes N3 . C13 . N2 . 116.4(4) yes N3 . C14 . C15 . 109.4(4) yes N3 . C14 . H141 . 109.1 no C15 . C14 . H141 . 109.2 no N3 . C14 . H142 . 109.1 no C15 . C14 . H142 . 110.6 no H141 . C14 . H142 . 109.5 no C14 . C15 . C16 . 122.9(6) yes C14 . C15 . H151 . 118.8 no C16 . C15 . H151 . 118.4 no C15 . C16 . H161 . 122.1 no C15 . C16 . H162 . 120.3 no H161 . C16 . H162 . 117.6 no S1 . C17 . N6 . 122.4(4) yes S1 . C17 . N5 . 113.4(4) yes N6 . C17 . N5 . 124.2(5) yes N6 . C18 . C19 . 112.7(5) yes N6 . C18 . H181 . 107.4 no C19 . C18 . H181 . 107.2 no N6 . C18 . H182 . 110.1 no C19 . C18 . H182 . 111.6 no H181 . C18 . H182 . 107.6 no C18 . C19 . C20 . 123.9(7) yes C18 . C19 . H191 . 117.7 no C20 . C19 . H191 . 118.4 no C19 . C20 . H201 . 120.6 no C19 . C20 . H202 . 120.9 no H201 . C20 . H202 . 118.5 no N7 . C21 . C24 . 110.4(4) yes N7 . C21 . H211 . 106.4 no C24 . C21 . H211 . 108.2 no N7 . C21 . H212 . 110.6 no C24 . C21 . H212 . 111.0 no H211 . C21 . H212 . 110.2 no N7 . C22 . C25 . 110.8(4) yes N7 . C22 . H221 . 109.6 no C25 . C22 . H221 . 111.5 no N7 . C22 . H222 . 108.2 no C25 . C22 . H222 . 109.0 no H221 . C22 . H222 . 107.7 no N7 . C23 . C26 . 110.4(4) yes N7 . C23 . H231 . 109.3 no C26 . C23 . H231 . 109.6 no N7 . C23 . H232 . 108.4 no C26 . C23 . H232 . 109.8 no H231 . C23 . H232 . 109.4 no C21 . C24 . N8 . 111.4(4) yes C21 . C24 . H241 . 110.4 no N8 . C24 . H241 . 108.2 no C21 . C24 . H242 . 110.3 no N8 . C24 . H242 . 107.5 no H241 . C24 . H242 . 109.0 no C22 . C25 . N8 . 110.7(4) yes C22 . C25 . H251 . 111.4 no N8 . C25 . H251 . 110.3 no C22 . C25 . H252 . 107.5 no N8 . C25 . H252 . 110.0 no H251 . C25 . H252 . 107.0 no C23 . C26 . N8 . 111.2(4) yes C23 . C26 . H261 . 108.0 no N8 . C26 . H261 . 108.6 no C23 . C26 . H262 . 110.8 no N8 . C26 . H262 . 109.4 no H261 . C26 . H262 . 108.7 no N101 . C101 . C102 . 133.5(4) yes N101 . C101 . C111 . 120.2(4) yes C102 . C101 . C111 . 106.0(3) yes C101 . C102 . N104 . 122.2(4) yes C101 . C102 . C103 . 107.4(3) yes N104 . C102 . C103 . 130.3(4) yes C102 . C103 . C104 . 135.4(4) yes C102 . C103 . C112 . 107.0(3) yes C104 . C103 . C112 . 117.6(4) yes C103 . C104 . C105 . 118.5(4) yes C103 . C104 . H1041 . 120.1 no C105 . C104 . H1041 . 121.4 no C104 . C105 . C106 . 122.8(4) yes C104 . C105 . H1051 . 119.2 no C106 . C105 . H1051 . 118.1 no C105 . C106 . C107 . 121.2(4) yes C105 . C106 . H1061 . 119.5 no C107 . C106 . H1061 . 119.4 no C106 . C107 . C108 . 128.2(4) yes C106 . C107 . C112 . 115.5(4) yes C108 . C107 . C112 . 116.3(4) yes C107 . C108 . C109 . 120.5(4) yes C107 . C108 . H1081 . 119.8 no C109 . C108 . H1081 . 119.7 no C108 . C109 . C110 . 122.5(5) yes C108 . C109 . H1091 . 119.3 no C110 . C109 . H1091 . 118.2 no C109 . C110 . C111 . 118.7(5) yes C109 . C110 . H1101 . 120.2 no C111 . C110 . H1101 . 121.1 no C101 . C111 . C110 . 134.1(4) yes C101 . C111 . C112 . 107.3(4) yes C110 . C111 . C112 . 118.5(4) yes C111 . C112 . C103 . 112.0(4) yes C111 . C112 . C107 . 123.4(4) yes C103 . C112 . C107 . 124.5(4) yes N102 . C113 . S101 . 112.0(4) yes N102 . C113 . N103 . 122.5(4) yes S101 . C113 . N103 . 125.5(3) yes N103 . C114 . C115 . 112.7(4) yes N103 . C114 . H1141 . 109.0 no C115 . C114 . H1141 . 108.7 no N103 . C114 . H1142 . 108.8 no C115 . C114 . H1142 . 108.6 no H1141 . C114 . H1142 . 108.9 no C114 . C115 . C116 . 123.5(6) yes C114 . C115 . H1151 . 117.5 no C116 . C115 . H1151 . 119.0 no C115 . C116 . H1161 . 121.4 no C115 . C116 . H1162 . 119.5 no H1161 . C116 . H1162 . 119.1 no S102 . C117 . N105 . 126.3(3) yes S102 . C117 . N106 . 115.4(3) yes N105 . C117 . N106 . 118.3(4) yes N106 . C118 . C119 . 112.9(5) yes N106 . C118 . H8 . 108.9 no C119 . C118 . H8 . 106.3 no N106 . C118 . H87 . 109.4 no C119 . C118 . H87 . 109.0 no H8 . C118 . H87 . 110.3 no C118 . C119 . C120 . 131.6(9) yes C118 . C119 . H1191 . 114.9 no C120 . C119 . H1191 . 113.4 no C119 . C120 . H1201 . 120.2 no C119 . C120 . H1202 . 122.5 no H1201 . C120 . H1202 . 117.2 no N107 . C121 . C124 . 110.3(4) yes N107 . C121 . H1211 . 109.8 no C124 . C121 . H1211 . 109.0 no N107 . C121 . H1212 . 108.8 no C124 . C121 . H1212 . 109.3 no H1211 . C121 . H1212 . 109.6 no N107 . C122 . C125 . 110.9(4) yes N107 . C122 . H1221 . 108.5 no C125 . C122 . H1221 . 109.5 no N107 . C122 . H1222 . 108.6 no C125 . C122 . H1222 . 110.7 no H1221 . C122 . H1222 . 108.5 no N107 . C123 . C126 . 110.8(4) yes N107 . C123 . H1231 . 109.2 no C126 . C123 . H1231 . 111.5 no N107 . C123 . H1232 . 107.7 no C126 . C123 . H1232 . 107.7 no H1231 . C123 . H1232 . 110.0 no C121 . C124 . N108 . 111.0(4) yes C121 . C124 . H1241 . 108.1 no N108 . C124 . H1241 . 109.0 no C121 . C124 . H1242 . 110.5 no N108 . C124 . H1242 . 109.6 no H1241 . C124 . H1242 . 108.6 no C122 . C125 . N108 . 110.7(4) yes C122 . C125 . H1251 . 109.5 no N108 . C125 . H1251 . 110.4 no C122 . C125 . H1252 . 109.6 no N108 . C125 . H1252 . 109.0 no H1251 . C125 . H1252 . 107.7 no C123 . C126 . N108 . 110.5(4) yes C123 . C126 . H1261 . 110.2 no N108 . C126 . H1261 . 110.4 no C123 . C126 . H1262 . 108.8 no N108 . C126 . H1262 . 108.3 no H1261 . C126 . H1262 . 108.6 no C202 . C201 . O1 . 108.7(5) yes C202 . C201 . H2011 . 110.4 no O1 . C201 . H2011 . 110.0 no C202 . C201 . H2012 . 108.9 no O1 . C201 . H2012 . 110.4 no H2011 . C201 . H2012 . 108.4 no C201 . C202 . C203 . 106.4(5) yes C201 . C202 . H2021 . 110.2 no C203 . C202 . H2021 . 110.4 no C201 . C202 . H2022 . 110.4 no C203 . C202 . H2022 . 110.4 no H2021 . C202 . H2022 . 109.1 no C202 . C203 . C204 . 104.0(6) yes C202 . C203 . H2031 . 111.8 no C204 . C203 . H2031 . 110.8 no C202 . C203 . H2032 . 111.1 no C204 . C203 . H2032 . 110.8 no H2031 . C203 . H2032 . 108.3 no C203 . C204 . O1 . 106.4(5) yes C203 . C204 . H2041 . 110.2 no O1 . C204 . H2041 . 109.0 no C203 . C204 . H2042 . 110.6 no O1 . C204 . H2042 . 112.1 no H2041 . C204 . H2042 . 108.4 no H2072 2_675 C205 . O2 2_675 104.7 no H2072 2_675 C205 . C206 2_675 127.8 no O2 2_675 C205 . C206 2_675 125(2) yes H2072 2_675 C205 . C206 . 131.5 no O2 2_675 C205 . C206 . 58.0(10) yes C206 2_675 C205 . C206 . 91.4(13) yes H2072 2_675 C205 . C209 . 111.7 no O2 2_675 C205 . C209 . 141.2(16) yes C206 2_675 C205 . C209 . 16.4(13) yes C206 . C205 . C209 . 103.5(6) yes H2072 2_675 C205 . H2051 . 22.3 no O2 2_675 C205 . H2051 . 107.4 no C206 2_675 C205 . H2051 . 127.1 no C206 . C205 . H2051 . 113.2 no C209 . C205 . H2051 . 111.4 no H2072 2_675 C205 . H2052 . 87.7 no O2 2_675 C205 . H2052 . 57.7 no C206 2_675 C205 . H2052 . 105.2 no C206 . C205 . H2052 . 110.6 no C209 . C205 . H2052 . 110.1 no H2051 . C205 . H2052 . 108.0 no C205 . C206 . H2092 2_675 120.9 no C205 . C206 . O2 2_675 56.1(9) yes H2092 2_675 C206 . O2 2_675 104.4 no C205 . C206 . C205 2_675 88.6(13) yes H2092 2_675 C206 . C205 2_675 133.1 no O2 2_675 C206 . C205 2_675 123(2) yes C205 . C206 . C207 . 104.0(6) yes H2092 2_675 C206 . C207 . 112.5 no O2 2_675 C206 . C207 . 143.0(18) yes C205 2_675 C206 . C207 . 20.6(14) yes C205 . C206 . H2061 . 110.3 no H2092 2_675 C206 . H2061 . 12.9 no O2 2_675 C206 . H2061 . 105.3 no C205 2_675 C206 . H2061 . 130.6 no C207 . C206 . H2061 . 111.3 no C205 . C206 . H2062 . 112.1 no H2092 2_675 C206 . H2062 . 96.2 no O2 2_675 C206 . H2062 . 60.9 no C205 2_675 C206 . H2062 . 105.6 no C207 . C206 . H2062 . 111.2 no H2061 . C206 . H2062 . 108.0 no C206 . C207 . H2051 2_675 97.7 no C206 . C207 . C209 2_675 14.6(10) yes H2051 2_675 C207 . C209 2_675 90.7 no C206 . C207 . H2052 2_675 111.1 no H2051 2_675 C207 . H2052 2_675 148.7 no C209 2_675 C207 . H2052 2_675 120.1 no C206 . C207 . O2 . 107.3(7) yes H2051 2_675 C207 . O2 . 100.7 no C209 2_675 C207 . O2 . 121.4(11) yes H2052 2_675 C207 . O2 . 59.9 no C206 . C207 . H2071 . 110.6 no H2051 2_675 C207 . H2071 . 128.8 no C209 2_675 C207 . H2071 . 106.2 no H2052 2_675 C207 . H2071 . 52.0 no O2 . C207 . H2071 . 109.7 no C206 . C207 . H2072 . 111.4 no H2051 2_675 C207 . H2072 . 22.0 no C209 2_675 C207 . H2072 . 100.7 no H2052 2_675 C207 . H2072 . 137.2 no O2 . C207 . H2072 . 110.9 no H2071 . C207 . H2072 . 106.9 no C205 . C209 . H2061 2_675 103.2 no C205 . C209 . C207 2_675 18.0(11) yes H2061 2_675 C209 . C207 2_675 93.0 no C205 . C209 . H2062 2_675 106.8 no H2061 2_675 C209 . H2062 2_675 150.0 no C207 2_675 C209 . H2062 2_675 116.2 no C205 . C209 . O2 . 106.9(7) yes H2061 2_675 C209 . O2 . 103.7 no C207 2_675 C209 . O2 . 124.2(11) yes H2062 2_675 C209 . O2 . 66.5 no C205 . C209 . H2091 . 111.9 no H2061 2_675 C209 . H2091 . 119.9 no C207 2_675 C209 . H2091 . 105.8 no H2062 2_675 C209 . H2091 . 48.1 no O2 . C209 . H2091 . 110.2 no C205 . C209 . H2092 . 111.6 no H2061 2_675 C209 . H2092 . 12.9 no C207 2_675 C209 . H2092 . 98.9 no H2062 2_675 C209 . H2092 . 140.6 no O2 . C209 . H2092 . 109.1 no H2091 . C209 . H2092 . 107.1 no C204 . O1 . C201 . 108.5(5) yes C206 2_675 O2 . C209 . 19.4(9) yes C206 2_675 O2 . C205 2_675 65.9(7) yes C209 . O2 . C205 2_675 85.3(9) yes C206 2_675 O2 . C207 . 88.9(9) yes C209 . O2 . C207 . 108.1(7) yes C205 2_675 O2 . C207 . 23.3(10) yes C206 2_675 O2 . H2052 2_675 106.5 no C209 . O2 . H2052 2_675 124.0 no C205 2_675 O2 . H2052 2_675 45.2 no C207 . O2 . H2052 2_675 23.8 no C206 2_675 O2 . H2062 2_675 42.6 no C209 . O2 . H2062 2_675 25.6 no C205 2_675 O2 . H2062 2_675 104.5 no C207 . O2 . H2062 2_675 124.5 no H2052 2_675 O2 . H2062 2_675 130.7 no #===END ###################################### ## denoted 3 in text ## ###################################### data_3 _database_code_depnum_ccdc_archive 'CCDC 642486' _audit_creation_date 07-06-22 _audit_creation_method CRYSTALS_ver_12.80 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 8.3511(7) _cell_length_b 18.9737(15) _cell_length_c 12.4187(10) _cell_angle_alpha 90 _cell_angle_beta 97.1090(10) _cell_angle_gamma 90 _cell_volume 1952.6(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126 1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C20 H18 Cu1 N6 S2' _chemical_formula_moiety 'C20 H18 Cu1 N6 S2' _chemical_compound_source ? _chemical_formula_weight 470.08 _cell_measurement_reflns_used 22936 _cell_measurement_theta_min 1 _cell_measurement_theta_max 32 _cell_measurement_temperature 150 _exptl_crystal_description needle _exptl_crystal_colour 'dark red' _exptl_crystal_size_min 0.01 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_max 0.02 _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 961.600 _exptl_absorpt_coefficient_mu 1.353 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_radiation_wavelength 0.6709 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART APEX2 CCD diffractometer' _diffrn_measurement_method 'fine-slice \w scans' _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 22936 _reflns_number_total 6356 _diffrn_reflns_av_R_equivalents 0.066 # Number of reflections with Friedels Law is 6356 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 6792 _diffrn_reflns_theta_min 2.087 _diffrn_reflns_theta_max 31.035 _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 29.484 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 27 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.43 _refine_diff_density_max 0.77 _refine_ls_number_reflns 4476 _refine_ls_number_restraints 16 _refine_ls_number_parameters 280 #_refine_ls_R_factor_ref 0.0392 _refine_ls_wR_factor_ref 0.0449 _refine_ls_goodness_of_fit_ref 1.1023 #_reflns_number_all 6344 _refine_ls_R_factor_all 0.0507 _refine_ls_wR_factor_all 0.0527 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 4476 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_gt 0.0449 _refine_ls_shift/su_max 0.003169 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.305 0.224 0.134 ; # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # Insert your own references if required - in alphabetical order _publ_section_references ; Data collection: APEX2, Bruker AXS Inc., Madison, USA, 2004 Data reduction (frames integration): SAINT, Bruker AXS Inc., Madison, USA, 2004 Cell refinement: SAINT, Bruker AXS Inc., Madison, USA, 2004 Absorption correction: SADABS, Bruker AXS Inc., Madison, USA, 2004 Station 9.8: R. J. Cernik, W. Clegg, C. R. A. Catlow, G. Bushnell-Wye, J. V. Flaherty, G. N. Greaves, M. Hamichi, I. Burrows, D. J. Taylor and S. J. Teat, J. Synchotron Radiation 1997, 4, 279-286; 7, 40. Synchrotron chemical crystallography: W. Clegg, J. Chem. Soc., Dalton Trans. 2000, 3223-3232. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Cu1 Cu 0.64608(3) 0.360277(13) 0.46008(2) 0.0205 1.0000 Uani . . . . . . N1 N 0.6355(2) 0.43826(9) 0.56557(14) 0.0200 1.0000 Uani . . . . . . N2 N 0.5619(2) 0.43508(9) 0.65718(14) 0.0213 1.0000 Uani . . . . . . N3 N 0.4273(2) 0.36005(10) 0.75731(15) 0.0246 1.0000 Uani . . . . . . N4 N 0.7616(2) 0.43217(9) 0.38394(14) 0.0206 1.0000 Uani . . . . . . N5 N 0.8182(2) 0.42333(10) 0.28677(14) 0.0235 1.0000 Uani . . . . . . N6 N 0.8232(3) 0.34309(11) 0.14989(16) 0.0315 1.0000 Uani . . . . . . C1 C 0.7097(2) 0.49431(10) 0.53949(15) 0.0194 1.0000 Uani . . . . . . C2 C 0.7835(2) 0.49067(10) 0.43765(16) 0.0196 1.0000 Uani . . . . . . C3 C 0.8655(2) 0.55729(10) 0.42393(16) 0.0207 1.0000 Uani . . . . . . C4 C 0.9560(3) 0.58427(12) 0.34807(18) 0.0241 1.0000 Uani . . . . . . C5 C 1.0167(3) 0.65368(12) 0.3640(2) 0.0284 1.0000 Uani . . . . . . C6 C 0.9885(3) 0.69426(12) 0.4523(2) 0.0292 1.0000 Uani . . . . . . C7 C 0.8957(3) 0.66773(11) 0.53141(18) 0.0237 1.0000 Uani . . . . . . C8 C 0.8543(3) 0.70238(12) 0.6254(2) 0.0297 1.0000 Uani . . . . . . C9 C 0.7612(3) 0.66932(13) 0.69422(19) 0.0292 1.0000 Uani . . . . . . C10 C 0.7031(3) 0.59931(12) 0.67621(17) 0.0253 1.0000 Uani . . . . . . C11 C 0.7425(2) 0.56437(10) 0.58628(16) 0.0199 1.0000 Uani . . . . . . C12 C 0.8365(3) 0.59885(10) 0.51455(17) 0.0212 1.0000 Uani . . . . . . C13 C 0.7815(3) 0.35928(11) 0.24796(17) 0.0232 1.0000 Uani . . . . . . C14 C 0.9242(4) 0.38801(16) 0.0913(2) 0.0387 1.0000 Uani . . . . . . C17 C 0.5035(2) 0.37081(11) 0.66937(16) 0.0218 1.0000 Uani . . . . . . C18 C 0.4046(3) 0.41653(12) 0.83395(18) 0.0268 1.0000 Uani . . . . . . C19 C 0.3301(4) 0.38809(15) 0.9281(2) 0.0406 1.0000 Uani . . . . . . C20 C 0.3973(6) 0.3936(2) 1.0292(2) 0.0589 1.0000 Uani . . . . . . S1 S 0.52367(7) 0.29884(3) 0.58290(4) 0.0245 1.0000 Uani . . . . . . S2 S 0.68043(7) 0.29342(3) 0.31311(5) 0.0267 1.0000 Uani . . . . . . C150 C 0.8495(12) 0.4232(6) 0.0004(6) 0.0429 0.3000 Uani D U . . . . C151 C 0.8749(6) 0.3783(3) -0.0296(3) 0.0483 0.7000 Uani D U . . . . C160 C 0.8530(15) 0.4000(7) -0.1021(7) 0.0451 0.3000 Uani D U . . . . C161 C 0.8379(7) 0.4319(3) -0.0995(4) 0.0496 0.7000 Uani D U . . . . H41 H 0.9772 0.5578 0.2881 0.0339 1.0000 Uiso . . . . . . H51 H 1.0775 0.6728 0.3129 0.0409 1.0000 Uiso . . . . . . H61 H 1.0305 0.7392 0.4589 0.0412 1.0000 Uiso . . . . . . H81 H 0.8905 0.7484 0.6408 0.0416 1.0000 Uiso . . . . . . H91 H 0.7347 0.6929 0.7554 0.0397 1.0000 Uiso . . . . . . H101 H 0.6402 0.5781 0.7224 0.0363 1.0000 Uiso . . . . . . H181 H 0.5065 0.4381 0.8582 0.0389 1.0000 Uiso . . . . . . H182 H 0.3338 0.4523 0.7971 0.0389 1.0000 Uiso . . . . . . H191 H 0.2304 0.3654 0.9140 0.0614 1.0000 Uiso . . . . . . H201 H 0.4973 0.4155 1.0473 0.0854 1.0000 Uiso . . . . . . H202 H 0.3450 0.3751 1.0836 0.0860 1.0000 Uiso . . . . . . H2 H 0.3829 0.3199 0.7649 0.0359 1.0000 Uiso . . . . . . H4 H 0.8035 0.3015 0.1258 0.0458 1.0000 Uiso . . . . . . H141 H 0.9072 0.4384 0.1110 0.0478 0.7000 Uiso . . . . . . H142 H 1.0393 0.3750 0.1101 0.0478 0.7000 Uiso . . . . . . H1501 H 0.7898 0.4687 0.0119 0.0514 0.3000 Uiso . . . . . . H1511 H 0.8707 0.3293 -0.0586 0.0597 0.7000 Uiso . . . . . . H1611 H 0.8425 0.4817 -0.0722 0.0608 0.7000 Uiso . . . . . . H1612 H 0.8081 0.4220 -0.1781 0.0608 0.7000 Uiso . . . . . . H1601 H 0.7979 0.4280 -0.1645 0.0531 0.3000 Uiso . . . . . . H1602 H 0.9113 0.3560 -0.1147 0.0531 0.3000 Uiso . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02534(13) 0.01629(11) 0.02040(12) -0.00074(9) 0.00470(8) -0.00056(9) N1 0.0241(8) 0.0181(7) 0.0181(7) 0.0003(6) 0.0032(6) 0.0008(6) N2 0.0259(8) 0.0214(8) 0.0171(7) 0.0007(6) 0.0047(6) -0.0006(6) N3 0.0289(9) 0.0235(8) 0.0225(8) 0.0028(7) 0.0072(7) -0.0001(7) N4 0.0254(8) 0.0193(7) 0.0174(7) 0.0002(6) 0.0045(6) 0.0015(6) N5 0.0299(9) 0.0225(8) 0.0190(7) 0.0002(6) 0.0069(7) 0.0025(7) N6 0.0481(12) 0.0249(9) 0.0229(9) -0.0050(7) 0.0096(8) 0.0031(8) C1 0.0222(9) 0.0181(8) 0.0175(8) -0.0001(6) 0.0010(7) 0.0001(6) C2 0.0212(9) 0.0186(8) 0.0192(8) 0.0010(6) 0.0035(7) 0.0009(7) C3 0.0217(9) 0.0181(8) 0.0218(9) 0.0023(7) 0.0011(7) -0.0008(7) C4 0.0239(10) 0.0242(9) 0.0241(9) 0.0043(7) 0.0027(7) -0.0009(7) C5 0.0262(10) 0.0268(10) 0.0323(11) 0.0073(8) 0.0038(8) -0.0043(8) C6 0.0292(11) 0.0209(9) 0.0363(12) 0.0066(8) -0.0005(9) -0.0043(8) C7 0.0224(9) 0.0170(8) 0.0305(10) 0.0007(7) -0.0021(8) -0.0011(7) C8 0.0316(11) 0.0211(9) 0.0345(11) -0.0057(8) -0.0032(9) -0.0014(8) C9 0.0326(11) 0.0255(10) 0.0285(10) -0.0086(8) -0.0001(9) 0.0017(8) C10 0.0294(10) 0.0243(9) 0.0219(9) -0.0024(7) 0.0020(8) 0.0001(8) C11 0.0225(9) 0.0173(8) 0.0197(8) -0.0012(6) 0.0013(7) -0.0003(7) C12 0.0240(9) 0.0172(8) 0.0221(9) 0.0001(6) 0.0012(7) -0.0004(7) C13 0.0259(10) 0.0223(9) 0.0211(8) -0.0005(7) 0.0022(7) 0.0054(8) C14 0.0550(16) 0.0397(14) 0.0237(11) 0.0002(10) 0.0139(10) -0.0044(12) C17 0.0223(9) 0.0226(9) 0.0200(8) 0.0020(7) 0.0009(7) 0.0009(7) C18 0.0310(11) 0.0280(10) 0.0221(9) -0.0006(8) 0.0061(8) 0.0024(8) C19 0.0530(16) 0.0365(13) 0.0369(13) -0.0019(11) 0.0236(12) -0.0047(12) C20 0.100(3) 0.0521(19) 0.0283(14) 0.0038(13) 0.0238(16) 0.0187(19) S1 0.0303(3) 0.0183(2) 0.0258(2) 0.00078(18) 0.00708(19) -0.00243(18) S2 0.0330(3) 0.0206(2) 0.0272(2) -0.00499(19) 0.0066(2) -0.0014(2) C150 0.036(4) 0.060(5) 0.033(3) 0.022(3) 0.009(3) 0.007(4) C151 0.0462(19) 0.068(3) 0.0322(16) 0.0060(17) 0.0096(14) 0.0004(18) C160 0.039(4) 0.064(5) 0.033(3) 0.020(4) 0.007(3) 0.006(4) C161 0.046(2) 0.069(3) 0.0351(17) 0.0107(18) 0.0087(15) 0.001(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1661(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu1 . N1 . 1.9855(17) yes Cu1 . N4 . 1.9779(17) yes Cu1 . C1 . 2.755(2) yes Cu1 . C2 . 2.756(2) yes Cu1 . S1 . 2.2620(6) yes Cu1 . S2 . 2.2699(6) yes N1 . N2 . 1.360(2) yes N1 . C1 . 1.292(3) yes N2 . C17 . 1.329(3) yes N3 . C17 . 1.346(3) yes N3 . C18 . 1.461(3) yes N3 . H2 . 0.857 no N4 . N5 . 1.360(2) yes N4 . C2 . 1.296(3) yes N5 . C13 . 1.329(3) yes N6 . C13 . 1.343(3) yes N6 . C14 . 1.456(3) yes N6 . H4 . 0.852 no C1 . C2 . 1.476(3) yes C1 . C11 . 1.463(3) yes C2 . C3 . 1.457(3) yes C3 . C4 . 1.377(3) yes C3 . C12 . 1.419(3) yes C4 . C5 . 1.417(3) yes C4 . H41 . 0.933 no C5 . C6 . 1.384(4) yes C5 . H51 . 0.933 no C6 . C7 . 1.417(3) yes C6 . H61 . 0.922 no C7 . C8 . 1.419(3) yes C7 . C12 . 1.404(3) yes C8 . C9 . 1.375(4) yes C8 . H81 . 0.936 no C9 . C10 . 1.423(3) yes C9 . H91 . 0.932 no C10 . C11 . 1.373(3) yes C10 . H101 . 0.917 no C11 . C12 . 1.418(3) yes C13 . S2 . 1.760(2) yes C14 . C150 . 1.390(9) yes C14 . C151 . 1.518(5) yes C14 . H141 . 1.001 no C14 . H142 . 0.992 no C17 . S1 . 1.758(2) yes C18 . C19 . 1.491(3) yes C18 . H181 . 0.959 no C18 . H182 . 0.976 no C19 . C20 . 1.315(5) yes C19 . H191 . 0.934 no C20 . H201 . 0.935 no C20 . H202 . 0.918 no C150 . C151 . 0.964(11) yes C150 . C160 . 1.351(2) yes C150 . C161 . 1.243(10) yes C150 . H1501 . 1.016 no C151 . C160 . 0.986(10) yes C151 . C161 . 1.3476(19) yes C151 . H1511 . 0.995 no C151 . H1602 . 1.212 no C160 . H1612 . 1.057 no C160 . H1601 . 1.003 no C160 . H1602 . 0.990 no C161 . H1611 . 1.002 no C161 . H1612 . 0.995 no C161 . H1601 . 0.838 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Cu1 . N4 . 82.28(7) yes N1 . Cu1 . C1 . 25.63(6) yes N4 . Cu1 . C1 . 56.68(6) yes N1 . Cu1 . C2 . 56.69(6) yes N4 . Cu1 . C2 . 25.66(6) yes C1 . Cu1 . C2 . 31.06(6) yes N1 . Cu1 . S1 . 83.01(5) yes N4 . Cu1 . S1 . 164.97(5) yes C1 . Cu1 . S1 . 108.51(4) yes C2 . Cu1 . S1 . 139.41(4) yes N1 . Cu1 . S2 . 165.33(5) yes N4 . Cu1 . S2 . 83.30(5) yes C1 . Cu1 . S2 . 139.96(4) yes C2 . Cu1 . S2 . 108.95(4) yes S1 . Cu1 . S2 . 111.52(2) yes Cu1 . N1 . N2 . 125.50(13) yes Cu1 . N1 . C1 . 112.71(14) yes N2 . N1 . C1 . 121.79(17) yes N1 . N2 . C17 . 110.26(17) yes C17 . N3 . C18 . 121.99(18) yes C17 . N3 . H2 . 118.6 no C18 . N3 . H2 . 119.1 no Cu1 . N4 . N5 . 125.65(14) yes Cu1 . N4 . C2 . 112.99(14) yes N5 . N4 . C2 . 121.34(18) yes N4 . N5 . C13 . 110.17(18) yes C13 . N6 . C14 . 123.4(2) yes C13 . N6 . H4 . 118.0 no C14 . N6 . H4 . 117.7 no N1 . C1 . Cu1 . 41.66(10) yes N1 . C1 . C2 . 116.14(17) yes Cu1 . C1 . C2 . 74.49(11) yes N1 . C1 . C11 . 136.07(19) yes Cu1 . C1 . C11 . 177.54(14) yes C2 . C1 . C11 . 107.79(17) yes C1 . C2 . N4 . 115.71(18) yes C1 . C2 . Cu1 . 74.45(11) yes N4 . C2 . Cu1 . 41.35(10) yes C1 . C2 . C3 . 108.17(17) yes N4 . C2 . C3 . 136.12(19) yes Cu1 . C2 . C3 . 176.27(15) yes C2 . C3 . C4 . 135.1(2) yes C2 . C3 . C12 . 105.09(17) yes C4 . C3 . C12 . 119.85(19) yes C3 . C4 . C5 . 117.9(2) yes C3 . C4 . H41 . 121.4 no C5 . C4 . H41 . 120.8 no C4 . C5 . C6 . 122.3(2) yes C4 . C5 . H51 . 118.8 no C6 . C5 . H51 . 118.9 no C5 . C6 . C7 . 120.9(2) yes C5 . C6 . H61 . 119.0 no C7 . C6 . H61 . 120.1 no C6 . C7 . C8 . 128.0(2) yes C6 . C7 . C12 . 116.1(2) yes C8 . C7 . C12 . 115.9(2) yes C7 . C8 . C9 . 120.9(2) yes C7 . C8 . H81 . 119.6 no C9 . C8 . H81 . 119.5 no C8 . C9 . C10 . 122.4(2) yes C8 . C9 . H91 . 119.9 no C10 . C9 . H91 . 117.7 no C9 . C10 . C11 . 117.9(2) yes C9 . C10 . H101 . 121.5 no C11 . C10 . H101 . 120.7 no C1 . C11 . C10 . 135.2(2) yes C1 . C11 . C12 . 105.10(17) yes C10 . C11 . C12 . 119.68(19) yes C3 . C12 . C11 . 113.82(18) yes C3 . C12 . C7 . 122.97(19) yes C11 . C12 . C7 . 123.21(19) yes N6 . C13 . N5 . 117.6(2) yes N6 . C13 . S2 . 116.59(17) yes N5 . C13 . S2 . 125.79(16) yes N6 . C14 . C150 . 117.2(5) yes N6 . C14 . C151 . 108.7(3) yes C150 . C14 . C151 . 38.4(4) yes N6 . C14 . H141 . 109.1 no C150 . C14 . H141 . 71.2 no C151 . C14 . H141 . 109.2 no N6 . C14 . H142 . 109.9 no C150 . C14 . H142 . 129.4 no C151 . C14 . H142 . 109.8 no H141 . C14 . H142 . 110.0 no N3 . C17 . N2 . 116.66(19) yes N3 . C17 . S1 . 117.93(16) yes N2 . C17 . S1 . 125.37(16) yes N3 . C18 . C19 . 110.2(2) yes N3 . C18 . H181 . 109.6 no C19 . C18 . H181 . 110.3 no N3 . C18 . H182 . 108.9 no C19 . C18 . H182 . 109.4 no H181 . C18 . H182 . 108.3 no C18 . C19 . C20 . 123.4(3) yes C18 . C19 . H191 . 118.0 no C20 . C19 . H191 . 118.7 no C19 . C20 . H201 . 121.9 no C19 . C20 . H202 . 119.1 no H201 . C20 . H202 . 119.0 no C17 . S1 . Cu1 . 95.56(7) yes C13 . S2 . Cu1 . 95.07(7) yes C14 . C150 . C151 . 78.0(7) yes C14 . C150 . C160 . 123.3(10) yes C151 . C150 . C160 . 46.9(6) yes C14 . C150 . C161 . 147.7(9) yes C151 . C150 . C161 . 74.0(6) yes C160 . C150 . C161 . 27.2(5) yes C14 . C150 . H1501 . 118.2 no C151 . C150 . H1501 . 160.2 no C160 . C150 . H1501 . 118.5 no C161 . C150 . H1501 . 92.7 no C14 . C151 . C150 . 63.6(6) yes C14 . C151 . C160 . 148.1(8) yes C150 . C151 . C160 . 87.7(7) yes C14 . C151 . C161 . 123.9(5) yes C150 . C151 . C161 . 62.5(6) yes C160 . C151 . C161 . 25.2(6) yes C14 . C151 . H1511 . 117.7 no C150 . C151 . H1511 . 164.7 no C160 . C151 . H1511 . 93.8 no C161 . C151 . H1511 . 118.5 no C14 . C151 . H1602 . 147.0 no C150 . C151 . H1602 . 137.5 no C160 . C151 . H1602 . 52.3 no C161 . C151 . H1602 . 76.4 no H1511 . C151 . H1602 . 50.2 no C150 . C160 . C151 . 45.5(7) yes C150 . C160 . H1612 . 131.8 no C151 . C160 . H1612 . 170.0 no C150 . C160 . H1601 . 119.7 no C151 . C160 . H1601 . 160.4 no H1612 . C160 . H1601 . 12.4 no C150 . C160 . H1602 . 119.5 no C151 . C160 . H1602 . 75.7 no H1612 . C160 . H1602 . 108.6 no H1601 . C160 . H1602 . 120.8 no C151 . C161 . C150 . 43.5(5) yes C151 . C161 . H1611 . 119.9 no C150 . C161 . H1611 . 78.1 no C151 . C161 . H1612 . 119.9 no C150 . C161 . H1612 . 158.8 no H1611 . C161 . H1612 . 120.2 no C151 . C161 . H1601 . 125.8 no C150 . C161 . H1601 . 157.2 no H1611 . C161 . H1601 . 113.7 no H1612 . C161 . H1601 . 10.4 no C160 . H1612 . C161 . 35.0 no C160 . H1601 . C161 . 38.0 no C160 . H1602 . C151 . 52.0 no #===END