# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name _publ_author_address J.N.H.Reek ; van 't Hoff Institute for Molecular Sciences University of Amsterdam Science Park 904 1098 XH Amsterdam The Netherlands ; V.Bocokic ; van 't Hoff Institute for Molecular Sciences University of Amsterdam Science Park 904 1098 XH Amsterdam The Netherlands ; A.Spek ; Bijvoet Center for Biomolecular Research Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; M.Lutz ; Bijvoet Center for Biomolecular Research Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; _publ_contact_author_name 'Martin Lutz' _publ_contact_author_address ; Bijvoet Center for Biomolecular Research Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; _publ_contact_author_email m.lutz@uu.nl _publ_contact_author_fax '[+31] 30 2533940' _publ_contact_author_phone '[+31] 30 2533902' _publ_section_title ; Bis-(thiosemicarbazonato) Zn(II) Complexes as Building Blocks for Construction of Supramolecular Catalysts ; # Attachment '- final_reek_et_al_deposit.cif' #TrackingRef '- final_reek_et_al_deposit.cif' data_s3940a _database_code_depnum_ccdc_archive 'CCDC 799011' #TrackingRef '- final_reek_et_al_deposit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H32 N7 P S2 Zn' _chemical_formula_sum 'C31 H32 N7 P S2 Zn' _chemical_formula_weight 663.10 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' P P 0.1023 0.0942 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1142(8) _cell_length_b 11.1774(9) _cell_length_c 13.0986(8) _cell_angle_alpha 81.434(3) _cell_angle_beta 84.669(4) _cell_angle_gamma 78.433(2) _cell_volume 1573.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4702 _cell_measurement_theta_min 1.58 _cell_measurement_theta_max 22.87 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.998 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.47 _exptl_absorpt_correction_T_max 0.94 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13454 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0623 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 21.00 _reflns_number_total 3373 _reflns_number_gt 2429 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement Peakref _computing_data_reduction 'EvalCCD, Sadabs' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0791P)^2^+16.5407P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3373 _refine_ls_number_parameters 383 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1219 _refine_ls_R_factor_gt 0.0867 _refine_ls_wR_factor_ref 0.2191 _refine_ls_wR_factor_gt 0.1990 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.72593(12) 0.23572(12) 0.55889(10) 0.0434(5) Uani 1 1 d . . . S1 S 0.8605(3) 0.3822(3) 0.5357(2) 0.0466(9) Uani 1 1 d . . . S2 S 0.7159(3) 0.1084(3) 0.7196(2) 0.0615(10) Uani 1 1 d . . . P1 P 0.9758(3) 0.1511(3) 0.1594(2) 0.0430(8) Uani 1 1 d . . . N1 N 0.8499(9) 0.5606(9) 0.3795(8) 0.047(3) Uani 1 1 d . . . H1 H 0.9181 0.5641 0.4071 0.057 Uiso 1 1 calc R . . N2 N 0.6835(8) 0.4658(8) 0.3936(7) 0.036(2) Uani 1 1 d . . . N3 N 0.6340(8) 0.3727(8) 0.4484(6) 0.036(2) Uani 1 1 d . . . N4 N 0.5499(9) 0.1967(9) 0.5590(7) 0.046(3) Uani 1 1 d . . . N5 N 0.5126(9) 0.0983(9) 0.6211(8) 0.054(3) Uani 1 1 d . . . N6 N 0.5542(10) -0.0452(9) 0.7642(8) 0.059(3) Uani 1 1 d . . . N7 N 0.8169(7) 0.1157(8) 0.4554(6) 0.031(2) Uani 1 1 d . . . C1 C 0.8225(11) 0.6474(11) 0.2902(10) 0.048(3) Uani 1 1 d . . . C2 C 0.7038(12) 0.6865(11) 0.2549(10) 0.058(4) Uani 1 1 d . . . H2 H 0.6368 0.6534 0.2906 0.070 Uiso 1 1 calc R . . C3 C 0.6842(14) 0.7734(12) 0.1681(10) 0.065(4) Uani 1 1 d . . . H3 H 0.6034 0.8001 0.1451 0.077 Uiso 1 1 calc R . . C4 C 0.7802(18) 0.8217(13) 0.1144(11) 0.073(4) Uani 1 1 d . . . H4 H 0.7667 0.8800 0.0540 0.088 Uiso 1 1 calc R . . C5 C 0.8965(17) 0.7835(14) 0.1504(11) 0.075(5) Uani 1 1 d . . . H5 H 0.9632 0.8183 0.1162 0.090 Uiso 1 1 calc R . . C6 C 0.9163(13) 0.6956(12) 0.2354(11) 0.063(4) Uani 1 1 d . . . H6 H 0.9978 0.6674 0.2566 0.075 Uiso 1 1 calc R . . C7 C 0.7893(10) 0.4742(11) 0.4289(9) 0.040(3) Uani 1 1 d . . . C8 C 0.5264(10) 0.3586(10) 0.4257(8) 0.036(3) Uani 1 1 d . . . C9 C 0.4788(10) 0.2560(11) 0.4884(9) 0.043(3) Uani 1 1 d . . . C10 C 0.4543(10) 0.4424(11) 0.3441(8) 0.047(3) Uani 1 1 d . . . H10A H 0.5012 0.5051 0.3117 0.070 Uiso 1 1 calc R . . H10B H 0.3759 0.4826 0.3754 0.070 Uiso 1 1 calc R . . H10C H 0.4383 0.3946 0.2916 0.070 Uiso 1 1 calc R . . C11 C 0.3588(11) 0.2228(11) 0.4692(10) 0.061(4) Uani 1 1 d . . . H11A H 0.3555 0.1392 0.5034 0.092 Uiso 1 1 calc R . . H11B H 0.3526 0.2263 0.3947 0.092 Uiso 1 1 calc R . . H11C H 0.2902 0.2812 0.4971 0.092 Uiso 1 1 calc R . . C12 C 0.5870(11) 0.0542(13) 0.6966(10) 0.057(4) Uani 1 1 d . . . C13 C 0.4398(13) -0.0865(12) 0.7483(11) 0.070(4) Uani 1 1 d . . . H13A H 0.3685 -0.0253 0.7681 0.105 Uiso 1 1 calc R . . H13B H 0.4371 -0.1658 0.7911 0.105 Uiso 1 1 calc R . . H13C H 0.4380 -0.0957 0.6753 0.105 Uiso 1 1 calc R . . C14 C 0.6173(14) -0.1039(15) 0.8517(10) 0.085(5) Uani 1 1 d . . . H14A H 0.6962 -0.0769 0.8496 0.128 Uiso 1 1 calc R . . H14B H 0.6319 -0.1933 0.8520 0.128 Uiso 1 1 calc R . . H14C H 0.5676 -0.0822 0.9145 0.128 Uiso 1 1 calc R . . C15 C 0.9235(9) 0.0906(9) 0.2895(7) 0.031(3) Uani 1 1 d . . . C16 C 0.8540(9) 0.1623(10) 0.3601(8) 0.037(3) Uani 1 1 d . . . H16 H 0.8316 0.2486 0.3397 0.045 Uiso 1 1 calc R . . C17 C 0.8441(9) -0.0062(11) 0.4824(8) 0.038(3) Uani 1 1 d . . . H17 H 0.8155 -0.0402 0.5489 0.045 Uiso 1 1 calc R . . C18 C 0.9120(10) -0.0842(10) 0.4177(9) 0.042(3) Uani 1 1 d . . . H18 H 0.9302 -0.1706 0.4389 0.050 Uiso 1 1 calc R . . C19 C 0.9532(10) -0.0344(11) 0.3214(9) 0.040(3) Uani 1 1 d . . . H19 H 1.0025 -0.0867 0.2764 0.048 Uiso 1 1 calc R . . C20 C 1.0484(11) 0.2762(10) 0.1792(8) 0.044(3) Uani 1 1 d . . . C21 C 1.0774(14) 0.3523(13) 0.0935(10) 0.075(4) Uani 1 1 d . . . H21 H 1.0537 0.3409 0.0283 0.089 Uiso 1 1 calc R . . C22 C 1.1406(18) 0.4465(15) 0.0986(12) 0.106(6) Uani 1 1 d . . . H22 H 1.1601 0.4980 0.0373 0.127 Uiso 1 1 calc R . . C23 C 1.1750(14) 0.4651(13) 0.1927(12) 0.075(4) Uani 1 1 d . . . H23 H 1.2185 0.5291 0.1966 0.090 Uiso 1 1 calc R . . C24 C 1.1462(11) 0.3914(12) 0.2792(10) 0.055(3) Uani 1 1 d . . . H24 H 1.1676 0.4051 0.3445 0.065 Uiso 1 1 calc R . . C25 C 1.0847(10) 0.2949(11) 0.2731(8) 0.045(3) Uani 1 1 d . . . H25 H 1.0678 0.2417 0.3341 0.054 Uiso 1 1 calc R . . C26 C 0.8332(11) 0.2306(11) 0.1029(8) 0.047(3) Uani 1 1 d . . . C27 C 0.7618(13) 0.3379(12) 0.1357(9) 0.062(4) Uani 1 1 d . . . H27 H 0.7893 0.3759 0.1871 0.074 Uiso 1 1 calc R . . C28 C 0.6502(15) 0.3883(14) 0.0923(11) 0.080(5) Uani 1 1 d . . . H28 H 0.6003 0.4595 0.1161 0.097 Uiso 1 1 calc R . . C29 C 0.6110(15) 0.3365(17) 0.0155(11) 0.086(5) Uani 1 1 d . . . H29 H 0.5348 0.3721 -0.0137 0.103 Uiso 1 1 calc R . . C30 C 0.6827(15) 0.2328(16) -0.0192(11) 0.081(5) Uani 1 1 d . . . H30 H 0.6564 0.1983 -0.0733 0.097 Uiso 1 1 calc R . . C31 C 0.7935(12) 0.1784(12) 0.0245(9) 0.056(3) Uani 1 1 d . . . H31 H 0.8418 0.1062 0.0012 0.067 Uiso 1 1 calc R . . 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 0.0402(9) 0.0500(9) 0.0359(8) -0.0142(6) -0.0064(6) 0.0095(7) S1 0.0403(18) 0.0438(19) 0.059(2) -0.0200(15) -0.0219(15) 0.0028(15) S2 0.063(2) 0.079(3) 0.0402(19) -0.0040(17) -0.0042(16) -0.0125(19) P1 0.052(2) 0.043(2) 0.0348(17) -0.0111(14) -0.0032(15) -0.0059(16) N1 0.038(6) 0.042(6) 0.061(7) -0.012(6) -0.011(5) 0.002(5) N2 0.026(6) 0.037(6) 0.045(6) -0.019(5) -0.004(5) 0.008(5) N3 0.039(6) 0.029(6) 0.037(5) -0.011(4) 0.000(5) 0.001(5) N4 0.047(6) 0.037(6) 0.041(6) -0.002(5) 0.013(5) 0.011(5) N5 0.044(6) 0.052(7) 0.057(7) -0.012(6) 0.004(6) 0.010(5) N6 0.060(8) 0.048(7) 0.066(8) -0.002(6) 0.020(6) -0.016(6) N7 0.034(5) 0.028(6) 0.031(6) -0.002(4) -0.010(4) -0.002(4) C1 0.042(8) 0.048(8) 0.059(8) -0.029(7) 0.003(7) -0.010(7) C2 0.059(10) 0.046(8) 0.072(10) -0.011(7) -0.002(7) -0.014(7) C3 0.075(10) 0.057(9) 0.060(9) -0.006(8) -0.008(8) -0.008(8) C4 0.124(15) 0.055(9) 0.050(9) -0.010(7) -0.011(10) -0.036(10) C5 0.112(14) 0.085(12) 0.048(9) -0.018(9) 0.000(9) -0.064(11) C6 0.076(10) 0.065(10) 0.061(10) -0.029(8) -0.005(8) -0.034(8) C7 0.028(7) 0.041(8) 0.052(7) -0.025(6) -0.003(6) 0.009(6) C8 0.027(7) 0.045(8) 0.037(7) -0.022(6) -0.005(6) 0.007(6) C9 0.034(7) 0.042(8) 0.048(8) -0.006(6) 0.010(6) 0.001(6) C10 0.030(7) 0.059(8) 0.051(7) -0.013(6) -0.011(6) -0.002(6) C11 0.049(9) 0.054(9) 0.077(10) -0.005(7) -0.002(7) -0.008(7) C12 0.044(8) 0.071(10) 0.056(9) -0.028(8) 0.005(7) 0.002(7) C13 0.068(10) 0.065(10) 0.072(10) -0.013(8) 0.013(8) -0.009(8) C14 0.080(11) 0.106(13) 0.053(9) 0.014(9) 0.013(8) -0.007(10) C15 0.034(6) 0.025(7) 0.033(6) -0.012(5) 0.001(5) 0.001(5) C16 0.035(7) 0.039(7) 0.034(7) -0.003(6) -0.012(5) 0.006(6) C17 0.033(7) 0.046(8) 0.037(7) 0.002(6) -0.006(5) -0.016(6) C18 0.037(7) 0.033(7) 0.058(9) -0.015(6) -0.008(6) -0.001(6) C19 0.039(7) 0.044(8) 0.039(7) -0.022(6) -0.006(6) 0.001(6) C20 0.057(8) 0.039(7) 0.029(7) 0.006(6) -0.010(6) 0.000(6) C21 0.118(13) 0.066(10) 0.056(9) -0.013(8) -0.025(9) -0.043(9) C22 0.171(19) 0.090(13) 0.065(11) 0.029(9) -0.035(11) -0.059(13) C23 0.094(12) 0.055(9) 0.082(11) 0.002(9) -0.040(9) -0.022(8) C24 0.052(8) 0.056(9) 0.059(9) -0.024(8) -0.026(7) 0.002(7) C25 0.044(7) 0.058(9) 0.032(7) -0.009(6) -0.010(6) -0.001(6) C26 0.069(9) 0.047(8) 0.024(6) -0.008(6) -0.011(6) -0.002(7) C27 0.081(10) 0.062(9) 0.033(7) -0.003(7) -0.015(7) 0.010(8) C28 0.099(13) 0.072(11) 0.054(9) 0.005(8) -0.011(9) 0.017(9) C29 0.076(11) 0.125(15) 0.045(9) 0.016(10) -0.026(8) 0.001(11) C30 0.086(12) 0.112(14) 0.049(9) -0.011(9) -0.031(9) -0.016(11) C31 0.063(9) 0.071(9) 0.038(7) -0.010(7) 0.000(7) -0.023(8) _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 Zn1 N4 2.088(10) . ? Zn1 N7 2.098(8) . ? Zn1 N3 2.115(9) . ? Zn1 S2 2.366(3) . ? Zn1 S1 2.400(3) . ? S1 C7 1.758(12) . ? S2 C12 1.730(14) . ? P1 C20 1.809(12) . ? P1 C26 1.818(12) . ? P1 C15 1.825(10) . ? N1 C7 1.342(14) . ? N1 C1 1.417(15) . ? N1 H1 0.8800 . ? N2 C7 1.327(13) . ? N2 N3 1.355(12) . ? N3 C8 1.302(13) . ? N4 C9 1.289(14) . ? N4 N5 1.376(13) . ? N5 C12 1.322(15) . ? N6 C12 1.400(16) . ? N6 C14 1.405(16) . ? N6 C13 1.479(16) . ? N7 C17 1.335(13) . ? N7 C16 1.340(13) . ? C1 C6 1.365(17) . ? C1 C2 1.403(17) . ? C2 C3 1.384(17) . ? C2 H2 0.9500 . ? C3 C4 1.380(19) . ? C3 H3 0.9500 . ? C4 C5 1.38(2) . ? C4 H4 0.9500 . ? C5 C6 1.373(18) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C8 C9 1.467(16) . ? C8 C10 1.491(15) . ? C9 C11 1.507(16) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C19 1.379(14) . ? C15 C16 1.390(14) . ? C16 H16 0.9500 . ? C17 C18 1.374(14) . ? C17 H17 0.9500 . ? C18 C19 1.377(15) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.359(16) . ? C20 C25 1.386(15) . ? C21 C22 1.390(19) . ? C21 H21 0.9500 . ? C22 C23 1.38(2) . ? C22 H22 0.9500 . ? C23 C24 1.351(18) . ? C23 H23 0.9500 . ? C24 C25 1.403(16) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C31 1.398(16) . ? C26 C27 1.401(16) . ? C27 C28 1.390(19) . ? C27 H27 0.9500 . ? C28 C29 1.38(2) . ? C28 H28 0.9500 . ? C29 C30 1.38(2) . ? C29 H29 0.9500 . ? C30 C31 1.393(18) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? 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 N4 Zn1 N7 98.2(3) . . ? N4 Zn1 N3 74.6(4) . . ? N7 Zn1 N3 97.4(3) . . ? N4 Zn1 S2 79.6(3) . . ? N7 Zn1 S2 104.4(3) . . ? N3 Zn1 S2 148.2(3) . . ? N4 Zn1 S1 150.0(3) . . ? N7 Zn1 S1 99.5(2) . . ? N3 Zn1 S1 79.2(3) . . ? S2 Zn1 S1 118.71(12) . . ? C7 S1 Zn1 95.6(4) . . ? C12 S2 Zn1 95.7(5) . . ? C20 P1 C26 103.1(5) . . ? C20 P1 C15 104.1(5) . . ? C26 P1 C15 102.9(5) . . ? C7 N1 C1 130.9(10) . . ? C7 N1 H1 114.6 . . ? C1 N1 H1 114.6 . . ? C7 N2 N3 112.1(9) . . ? C8 N3 N2 118.5(9) . . ? C8 N3 Zn1 116.5(7) . . ? N2 N3 Zn1 124.7(7) . . ? C9 N4 N5 117.8(10) . . ? C9 N4 Zn1 118.7(8) . . ? N5 N4 Zn1 122.8(7) . . ? C12 N5 N4 111.5(11) . . ? C12 N6 C14 124.8(12) . . ? C12 N6 C13 118.4(11) . . ? C14 N6 C13 116.6(11) . . ? C17 N7 C16 118.3(9) . . ? C17 N7 Zn1 122.3(7) . . ? C16 N7 Zn1 119.4(7) . . ? C6 C1 C2 118.0(13) . . ? C6 C1 N1 118.5(12) . . ? C2 C1 N1 123.4(11) . . ? C3 C2 C1 119.9(13) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 121.1(14) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 118.5(14) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C6 C5 C4 120.4(14) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C1 C6 C5 122.0(14) . . ? C1 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? N2 C7 N1 118.1(10) . . ? N2 C7 S1 126.6(10) . . ? N1 C7 S1 115.3(9) . . ? N3 C8 C9 115.3(10) . . ? N3 C8 C10 122.8(10) . . ? C9 C8 C10 121.9(11) . . ? N4 C9 C8 113.9(11) . . ? N4 C9 C11 123.8(11) . . ? C8 C9 C11 122.3(11) . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 N6 115.0(12) . . ? N5 C12 S2 126.6(11) . . ? N6 C12 S2 118.4(10) . . ? N6 C13 H13A 109.5 . . ? N6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N6 C14 H14A 109.5 . . ? N6 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N6 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C19 C15 C16 116.8(10) . . ? C19 C15 P1 118.9(8) . . ? C16 C15 P1 124.3(8) . . ? N7 C16 C15 123.3(10) . . ? N7 C16 H16 118.4 . . ? C15 C16 H16 118.4 . . ? N7 C17 C18 122.5(10) . . ? N7 C17 H17 118.8 . . ? C18 C17 H17 118.8 . . ? C19 C18 C17 118.5(10) . . ? C19 C18 H18 120.7 . . ? C17 C18 H18 120.7 . . ? C18 C19 C15 120.6(10) . . ? C18 C19 H19 119.7 . . ? C15 C19 H19 119.7 . . ? C21 C20 C25 117.7(11) . . ? C21 C20 P1 116.8(9) . . ? C25 C20 P1 125.3(9) . . ? C20 C21 C22 121.8(12) . . ? C20 C21 H21 119.1 . . ? C22 C21 H21 119.1 . . ? C23 C22 C21 119.9(14) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C24 C23 C22 119.4(13) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C25 120.3(11) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C20 C25 C24 120.8(11) . . ? C20 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C31 C26 C27 119.5(11) . . ? C31 C26 P1 117.1(9) . . ? C27 C26 P1 123.3(9) . . ? C28 C27 C26 119.4(12) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C29 C28 C27 121.0(14) . . ? C29 C28 H28 119.5 . . ? C27 C28 H28 119.5 . . ? C28 C29 C30 119.9(14) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C29 C30 C31 120.5(13) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C30 C31 C26 119.7(13) . . ? C30 C31 H31 120.1 . . ? C26 C31 H31 120.1 . . ? 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 N4 Zn1 S1 C7 -39.0(6) . . . . ? N7 Zn1 S1 C7 86.2(4) . . . . ? N3 Zn1 S1 C7 -9.5(4) . . . . ? S2 Zn1 S1 C7 -161.5(3) . . . . ? N4 Zn1 S2 C12 13.4(5) . . . . ? N7 Zn1 S2 C12 -82.5(5) . . . . ? N3 Zn1 S2 C12 49.3(6) . . . . ? S1 Zn1 S2 C12 168.0(4) . . . . ? C7 N2 N3 C8 176.1(8) . . . . ? C7 N2 N3 Zn1 -10.5(10) . . . . ? N4 Zn1 N3 C8 -8.0(7) . . . . ? N7 Zn1 N3 C8 88.5(7) . . . . ? S2 Zn1 N3 C8 -44.7(9) . . . . ? S1 Zn1 N3 C8 -173.2(7) . . . . ? N4 Zn1 N3 N2 178.5(8) . . . . ? N7 Zn1 N3 N2 -85.0(7) . . . . ? S2 Zn1 N3 N2 141.7(6) . . . . ? S1 Zn1 N3 N2 13.3(7) . . . . ? N7 Zn1 N4 C9 -86.1(8) . . . . ? N3 Zn1 N4 C9 9.3(8) . . . . ? S2 Zn1 N4 C9 170.6(8) . . . . ? S1 Zn1 N4 C9 39.4(11) . . . . ? N7 Zn1 N4 N5 84.0(8) . . . . ? N3 Zn1 N4 N5 179.4(8) . . . . ? S2 Zn1 N4 N5 -19.3(7) . . . . ? S1 Zn1 N4 N5 -150.5(6) . . . . ? C9 N4 N5 C12 -173.4(9) . . . . ? Zn1 N4 N5 C12 16.5(12) . . . . ? N4 Zn1 N7 C17 -74.2(8) . . . . ? N3 Zn1 N7 C17 -149.6(8) . . . . ? S2 Zn1 N7 C17 7.1(8) . . . . ? S1 Zn1 N7 C17 130.2(7) . . . . ? N4 Zn1 N7 C16 108.6(8) . . . . ? N3 Zn1 N7 C16 33.3(8) . . . . ? S2 Zn1 N7 C16 -170.1(7) . . . . ? S1 Zn1 N7 C16 -47.0(7) . . . . ? C7 N1 C1 C6 -157.8(11) . . . . ? C7 N1 C1 C2 22.1(17) . . . . ? C6 C1 C2 C3 -1.3(17) . . . . ? N1 C1 C2 C3 178.8(11) . . . . ? C1 C2 C3 C4 0.7(19) . . . . ? C2 C3 C4 C5 -1(2) . . . . ? C3 C4 C5 C6 3(2) . . . . ? C2 C1 C6 C5 2.6(18) . . . . ? N1 C1 C6 C5 -177.5(11) . . . . ? C4 C5 C6 C1 -3(2) . . . . ? N3 N2 C7 N1 178.1(8) . . . . ? N3 N2 C7 S1 -1.8(12) . . . . ? C1 N1 C7 N2 -2.0(16) . . . . ? C1 N1 C7 S1 177.9(8) . . . . ? Zn1 S1 C7 N2 9.9(9) . . . . ? Zn1 S1 C7 N1 -170.0(7) . . . . ? N2 N3 C8 C9 -179.9(8) . . . . ? Zn1 N3 C8 C9 6.1(11) . . . . ? N2 N3 C8 C10 -1.7(14) . . . . ? Zn1 N3 C8 C10 -175.6(7) . . . . ? N5 N4 C9 C8 -179.6(8) . . . . ? Zn1 N4 C9 C8 -9.0(12) . . . . ? N5 N4 C9 C11 -0.9(15) . . . . ? Zn1 N4 C9 C11 169.7(8) . . . . ? N3 C8 C9 N4 1.8(13) . . . . ? C10 C8 C9 N4 -176.5(9) . . . . ? N3 C8 C9 C11 -177.0(9) . . . . ? C10 C8 C9 C11 4.7(15) . . . . ? N4 N5 C12 N6 179.1(8) . . . . ? N4 N5 C12 S2 0.2(14) . . . . ? C14 N6 C12 N5 -177.8(11) . . . . ? C13 N6 C12 N5 -2.8(15) . . . . ? C14 N6 C12 S2 1.3(16) . . . . ? C13 N6 C12 S2 176.3(8) . . . . ? Zn1 S2 C12 N5 -12.4(11) . . . . ? Zn1 S2 C12 N6 168.7(8) . . . . ? C20 P1 C15 C19 -129.5(9) . . . . ? C26 P1 C15 C19 123.3(9) . . . . ? C20 P1 C15 C16 50.9(10) . . . . ? C26 P1 C15 C16 -56.3(10) . . . . ? C17 N7 C16 C15 -2.7(15) . . . . ? Zn1 N7 C16 C15 174.6(8) . . . . ? C19 C15 C16 N7 0.6(15) . . . . ? P1 C15 C16 N7 -179.8(8) . . . . ? C16 N7 C17 C18 2.4(15) . . . . ? Zn1 N7 C17 C18 -174.8(7) . . . . ? N7 C17 C18 C19 -0.1(16) . . . . ? C17 C18 C19 C15 -2.0(16) . . . . ? C16 C15 C19 C18 1.8(15) . . . . ? P1 C15 C19 C18 -177.8(8) . . . . ? C26 P1 C20 C21 -61.8(11) . . . . ? C15 P1 C20 C21 -168.9(10) . . . . ? C26 P1 C20 C25 123.3(10) . . . . ? C15 P1 C20 C25 16.2(11) . . . . ? C25 C20 C21 C22 0(2) . . . . ? P1 C20 C21 C22 -175.7(13) . . . . ? C20 C21 C22 C23 0(3) . . . . ? C21 C22 C23 C24 0(3) . . . . ? C22 C23 C24 C25 2(2) . . . . ? C21 C20 C25 C24 1.7(17) . . . . ? P1 C20 C25 C24 176.7(9) . . . . ? C23 C24 C25 C20 -2.5(18) . . . . ? C20 P1 C26 C31 141.6(9) . . . . ? C15 P1 C26 C31 -110.4(9) . . . . ? C20 P1 C26 C27 -39.9(12) . . . . ? C15 P1 C26 C27 68.1(11) . . . . ? C31 C26 C27 C28 2.3(19) . . . . ? P1 C26 C27 C28 -176.2(10) . . . . ? C26 C27 C28 C29 -2(2) . . . . ? C27 C28 C29 C30 0(2) . . . . ? C28 C29 C30 C31 1(2) . . . . ? C29 C30 C31 C26 -1(2) . . . . ? C27 C26 C31 C30 -0.8(18) . . . . ? P1 C26 C31 C30 177.8(10) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 21.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.226 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.110 #===END data_s3939a _database_code_depnum_ccdc_archive 'CCDC 799012' #TrackingRef '- final_reek_et_al_deposit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H32 N7 P S2 Zn, C7 H8' _chemical_formula_sum 'C38 H40 N7 P S2 Zn' _chemical_formula_weight 755.23 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' P P 0.1023 0.0942 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9582(3) _cell_length_b 13.0266(2) _cell_length_c 13.1409(3) _cell_angle_alpha 115.9892(8) _cell_angle_beta 93.8687(10) _cell_angle_gamma 107.0963(9) _cell_volume 1855.38(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 102858 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 26.73 _exptl_crystal_description 'triangular prism' _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 0.855 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.49 _exptl_absorpt_correction_T_max 0.83 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21422 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 24.00 _reflns_number_total 5715 _reflns_number_gt 4719 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement HKL2000 _computing_data_reduction 'HKL2000, denzox, Sadabs' _computing_structure_solution 'SIR-97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0687P)^2^+3.9833P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5715 _refine_ls_number_parameters 447 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1615 _refine_ls_wR_factor_gt 0.1526 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.42321(4) 0.30604(5) 0.11831(5) 0.0485(2) Uani 1 1 d . . . S1 S 0.46833(11) 0.41787(11) 0.32299(12) 0.0606(4) Uani 1 1 d . . . S2 S 0.54861(10) 0.20803(13) 0.03930(13) 0.0622(4) Uani 1 1 d . . . P1 P -0.01713(9) -0.20893(10) -0.04323(11) 0.0425(3) Uani 1 1 d . . . N1 N 0.3858(3) 0.5818(4) 0.4460(4) 0.0589(11) Uani 1 1 d . . . H1 H 0.4144 0.5643 0.4963 0.071 Uiso 1 1 calc R . . N2 N 0.3435(3) 0.5218(3) 0.2493(4) 0.0490(9) Uani 1 1 d . . . N3 N 0.3623(3) 0.4489(3) 0.1447(3) 0.0452(9) Uani 1 1 d . . . N4 N 0.4136(3) 0.3119(3) -0.0404(4) 0.0499(10) Uani 1 1 d . . . N5 N 0.4510(3) 0.2414(4) -0.1318(4) 0.0553(10) Uani 1 1 d . . . N6 N 0.5535(4) 0.1183(4) -0.1871(4) 0.0678(12) Uani 1 1 d . . . N7 N 0.2815(3) 0.1529(3) 0.0741(3) 0.0396(8) Uani 1 1 d . . . C1 C 0.3425(4) 0.6763(5) 0.4964(5) 0.0570(13) Uani 1 1 d . . . C2 C 0.2885(4) 0.7160(5) 0.4331(5) 0.0617(13) Uani 1 1 d . . . H2 H 0.2783 0.6792 0.3510 0.074 Uiso 1 1 calc R . . C3 C 0.2503(5) 0.8099(5) 0.4923(6) 0.0724(16) Uani 1 1 d . . . H3 H 0.2138 0.8373 0.4497 0.087 Uiso 1 1 calc R . . C4 C 0.2639(5) 0.8645(6) 0.6111(6) 0.0776(17) Uani 1 1 d . . . H4 H 0.2358 0.9277 0.6497 0.093 Uiso 1 1 calc R . . C5 C 0.3186(6) 0.8269(7) 0.6740(6) 0.088(2) Uani 1 1 d . . . H5 H 0.3306 0.8657 0.7563 0.106 Uiso 1 1 calc R . . C6 C 0.3556(5) 0.7321(6) 0.6159(6) 0.0795(18) Uani 1 1 d . . . H6 H 0.3909 0.7046 0.6591 0.095 Uiso 1 1 calc R . . C7 C 0.3914(4) 0.5127(4) 0.3343(4) 0.0471(11) Uani 1 1 d . . . C8 C 0.3329(3) 0.4579(4) 0.0537(4) 0.0448(11) Uani 1 1 d . . . C9 C 0.3660(3) 0.3819(4) -0.0537(4) 0.0477(11) Uani 1 1 d . . . C10 C 0.2725(4) 0.5388(4) 0.0508(5) 0.0551(12) Uani 1 1 d . . . H10A H 0.2597 0.5837 0.1280 0.083 Uiso 1 1 calc R . . H10B H 0.2012 0.4886 -0.0058 0.083 Uiso 1 1 calc R . . H10C H 0.3172 0.5970 0.0282 0.083 Uiso 1 1 calc R . . C11 C 0.3522(4) 0.3944(5) -0.1600(5) 0.0596(13) Uani 1 1 d . . . H11A H 0.2740 0.3535 -0.2013 0.089 Uiso 1 1 calc R . . H11B H 0.3972 0.3565 -0.2106 0.089 Uiso 1 1 calc R . . H11C H 0.3763 0.4814 -0.1384 0.089 Uiso 1 1 calc R . . C12 C 0.5124(4) 0.1900(4) -0.0997(5) 0.0565(13) Uani 1 1 d . . . C13 C 0.6169(5) 0.0497(6) -0.1723(6) 0.0835(18) Uani 1 1 d . . . H13A H 0.6058 0.0408 -0.1032 0.125 Uiso 1 1 calc R . . H13B H 0.6957 0.0932 -0.1627 0.125 Uiso 1 1 calc R . . H13C H 0.5923 -0.0314 -0.2409 0.125 Uiso 1 1 calc R . . C14 C 0.5392(5) 0.1115(6) -0.2993(5) 0.0764(16) Uani 1 1 d . . . H14A H 0.5444 0.1918 -0.2903 0.115 Uiso 1 1 calc R . . H14B H 0.4662 0.0507 -0.3472 0.115 Uiso 1 1 calc R . . H14C H 0.5971 0.0875 -0.3370 0.115 Uiso 1 1 calc R . . C15 C 0.1047(3) -0.0675(4) 0.0074(4) 0.0378(10) Uani 1 1 d . . . C16 C 0.1538(4) -0.0411(4) -0.0741(4) 0.0424(10) Uani 1 1 d . . . H16 H 0.1269 -0.0980 -0.1547 0.051 Uiso 1 1 calc R . . C17 C 0.2414(3) 0.0674(4) -0.0375(4) 0.0428(10) Uani 1 1 d . . . H17 H 0.2747 0.0821 -0.0944 0.051 Uiso 1 1 calc R . . C18 C 0.2330(3) 0.1297(4) 0.1525(4) 0.0419(10) Uani 1 1 d . . . H18 H 0.2590 0.1899 0.2322 0.050 Uiso 1 1 calc R . . C19 C 0.1461(3) 0.0212(4) 0.1219(4) 0.0416(10) Uani 1 1 d . . . H19 H 0.1150 0.0083 0.1806 0.050 Uiso 1 1 calc R . . C20 C -0.0072(4) -0.2410(4) 0.0784(4) 0.0431(10) Uani 1 1 d . . . C21 C -0.0641(4) -0.1918(4) 0.1628(5) 0.0559(12) Uani 1 1 d . . . H21 H -0.1037 -0.1440 0.1545 0.067 Uiso 1 1 calc R . . C22 C -0.0639(4) -0.2110(5) 0.2577(5) 0.0604(13) Uani 1 1 d . . . H22 H -0.1014 -0.1748 0.3152 0.072 Uiso 1 1 calc R . . C23 C -0.0095(5) -0.2826(5) 0.2690(5) 0.0654(14) Uani 1 1 d . . . H23 H -0.0090 -0.2952 0.3349 0.078 Uiso 1 1 calc R . . C24 C 0.0435(5) -0.3354(5) 0.1870(5) 0.0716(16) Uani 1 1 d . . . H24 H 0.0795 -0.3863 0.1948 0.086 Uiso 1 1 calc R . . C25 C 0.0453(4) -0.3152(5) 0.0900(5) 0.0598(13) Uani 1 1 d . . . H25 H 0.0826 -0.3523 0.0326 0.072 Uiso 1 1 calc R . . C26 C 0.0289(4) -0.3187(4) -0.1549(4) 0.0444(10) Uani 1 1 d . . . C27 C -0.0499(4) -0.4071(4) -0.2587(4) 0.0592(14) Uani 1 1 d . . . H27 H -0.1249 -0.4119 -0.2657 0.071 Uiso 1 1 calc R . . C28 C -0.0190(6) -0.4873(5) -0.3509(5) 0.0755(18) Uani 1 1 d . . . H28 H -0.0724 -0.5460 -0.4213 0.091 Uiso 1 1 calc R . . C29 C 0.0872(6) -0.4816(5) -0.3403(6) 0.0790(18) Uani 1 1 d . . . H29 H 0.1080 -0.5358 -0.4045 0.095 Uiso 1 1 calc R . . C30 C 0.1661(5) -0.3992(5) -0.2387(5) 0.0657(14) Uani 1 1 d . . . H30 H 0.2398 -0.3986 -0.2316 0.079 Uiso 1 1 calc R . . C31 C 0.1366(4) -0.3175(4) -0.1474(4) 0.0497(11) Uani 1 1 d . . . H31 H 0.1912 -0.2591 -0.0777 0.060 Uiso 1 1 calc R . . C32 C 0.2438(6) 0.1735(6) 0.4821(5) 0.0763(16) Uani 1 1 d . . . C33 C 0.2622(6) 0.2809(5) 0.4768(5) 0.0783(17) Uani 1 1 d . . . H33 H 0.3357 0.3385 0.5011 0.094 Uiso 1 1 calc R . . C34 C 0.1794(6) 0.3063(6) 0.4384(6) 0.0785(17) Uani 1 1 d . . . H34 H 0.1955 0.3799 0.4337 0.094 Uiso 1 1 calc R . . C35 C 0.0702(5) 0.2261(5) 0.4053(5) 0.0719(15) Uani 1 1 d . . . H35 H 0.0116 0.2451 0.3795 0.086 Uiso 1 1 calc R . . C36 C 0.0487(6) 0.1202(6) 0.4104(5) 0.0808(18) Uani 1 1 d . . . H36 H -0.0255 0.0645 0.3882 0.097 Uiso 1 1 calc R . . C37 C 0.1370(5) 0.0929(5) 0.4489(5) 0.0728(16) Uani 1 1 d . . . H37 H 0.1219 0.0183 0.4515 0.087 Uiso 1 1 calc R . . C38 C 0.3374(7) 0.1456(8) 0.5222(7) 0.107(2) Uani 1 1 d . . . H38A H 0.3462 0.0763 0.4568 0.160 Uiso 1 1 calc R . . H38B H 0.3216 0.1247 0.5841 0.160 Uiso 1 1 calc R . . H38C H 0.4059 0.2174 0.5520 0.160 Uiso 1 1 calc R . . 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 0.0390(3) 0.0407(3) 0.0737(4) 0.0367(3) 0.0039(2) 0.0124(2) S1 0.0648(8) 0.0481(7) 0.0690(8) 0.0306(6) -0.0076(6) 0.0216(6) S2 0.0472(7) 0.0715(9) 0.0893(10) 0.0506(8) 0.0159(7) 0.0307(6) P1 0.0349(6) 0.0424(6) 0.0618(7) 0.0357(6) 0.0068(5) 0.0131(5) N1 0.060(3) 0.061(3) 0.078(3) 0.051(2) 0.011(2) 0.023(2) N2 0.046(2) 0.046(2) 0.067(3) 0.039(2) 0.0103(19) 0.0159(17) N3 0.0379(19) 0.042(2) 0.064(3) 0.0361(19) 0.0066(18) 0.0109(16) N4 0.038(2) 0.045(2) 0.074(3) 0.035(2) 0.0147(19) 0.0127(17) N5 0.044(2) 0.053(2) 0.078(3) 0.039(2) 0.016(2) 0.0176(19) N6 0.058(3) 0.078(3) 0.080(3) 0.043(3) 0.014(2) 0.034(2) N7 0.0379(19) 0.0371(18) 0.052(2) 0.0272(17) 0.0062(16) 0.0154(15) C1 0.049(3) 0.059(3) 0.081(4) 0.048(3) 0.023(3) 0.020(2) C2 0.067(3) 0.049(3) 0.073(3) 0.035(3) 0.005(3) 0.019(3) C3 0.076(4) 0.061(3) 0.094(5) 0.048(3) 0.011(3) 0.028(3) C4 0.083(4) 0.080(4) 0.098(5) 0.054(4) 0.040(4) 0.045(3) C5 0.116(5) 0.122(6) 0.086(4) 0.072(4) 0.057(4) 0.080(5) C6 0.099(5) 0.108(5) 0.089(5) 0.073(4) 0.048(4) 0.066(4) C7 0.042(2) 0.041(2) 0.062(3) 0.032(2) 0.003(2) 0.0098(19) C8 0.032(2) 0.039(2) 0.071(3) 0.037(2) 0.008(2) 0.0086(18) C9 0.035(2) 0.045(2) 0.068(3) 0.037(2) 0.007(2) 0.008(2) C10 0.054(3) 0.056(3) 0.073(3) 0.043(3) 0.013(2) 0.025(2) C11 0.055(3) 0.058(3) 0.071(3) 0.038(3) 0.012(3) 0.017(2) C12 0.038(2) 0.051(3) 0.087(4) 0.041(3) 0.012(2) 0.013(2) C13 0.085(4) 0.088(4) 0.099(5) 0.048(4) 0.024(4) 0.054(4) C14 0.080(4) 0.093(4) 0.072(4) 0.043(3) 0.023(3) 0.046(3) C15 0.033(2) 0.038(2) 0.058(3) 0.032(2) 0.0085(19) 0.0174(17) C16 0.047(2) 0.040(2) 0.045(2) 0.025(2) 0.009(2) 0.0151(19) C17 0.043(2) 0.041(2) 0.057(3) 0.032(2) 0.014(2) 0.0160(19) C18 0.044(2) 0.039(2) 0.048(3) 0.023(2) 0.007(2) 0.0190(19) C19 0.043(2) 0.042(2) 0.051(3) 0.029(2) 0.014(2) 0.0188(19) C20 0.046(2) 0.039(2) 0.056(3) 0.032(2) 0.013(2) 0.0150(19) C21 0.052(3) 0.052(3) 0.075(3) 0.039(3) 0.016(3) 0.020(2) C22 0.063(3) 0.055(3) 0.068(3) 0.036(3) 0.026(3) 0.015(3) C23 0.079(4) 0.062(3) 0.068(3) 0.046(3) 0.019(3) 0.019(3) C24 0.092(4) 0.076(4) 0.085(4) 0.061(3) 0.026(3) 0.043(3) C25 0.066(3) 0.065(3) 0.070(3) 0.043(3) 0.020(3) 0.035(3) C26 0.046(2) 0.035(2) 0.052(3) 0.029(2) 0.005(2) 0.0036(19) C27 0.064(3) 0.052(3) 0.056(3) 0.036(3) 0.004(2) 0.000(2) C28 0.107(5) 0.049(3) 0.045(3) 0.023(3) 0.005(3) -0.002(3) C29 0.112(5) 0.048(3) 0.073(4) 0.028(3) 0.041(4) 0.019(3) C30 0.079(4) 0.045(3) 0.082(4) 0.036(3) 0.033(3) 0.023(3) C31 0.054(3) 0.037(2) 0.060(3) 0.025(2) 0.010(2) 0.016(2) C32 0.090(4) 0.077(4) 0.057(3) 0.029(3) 0.015(3) 0.029(4) C33 0.100(5) 0.058(3) 0.084(4) 0.039(3) 0.028(4) 0.027(3) C34 0.089(5) 0.064(4) 0.086(4) 0.040(3) 0.024(4) 0.027(3) C35 0.088(4) 0.063(3) 0.069(4) 0.030(3) 0.020(3) 0.035(3) C36 0.091(5) 0.064(4) 0.081(4) 0.034(3) 0.028(4) 0.020(3) C37 0.083(4) 0.061(3) 0.073(4) 0.034(3) 0.022(3) 0.021(3) C38 0.120(6) 0.114(6) 0.099(5) 0.049(5) 0.016(5) 0.064(5) _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 Zn1 N7 2.092(3) . ? Zn1 N4 2.117(4) . ? Zn1 N3 2.132(4) . ? Zn1 S1 2.3561(15) . ? Zn1 S2 2.3737(14) . ? S1 C7 1.767(5) . ? S2 C12 1.749(6) . ? P1 C20 1.825(4) . ? P1 C26 1.826(5) . ? P1 C15 1.845(4) . ? N1 C7 1.367(6) . ? N1 C1 1.418(7) . ? N1 H1 0.8800 . ? N2 C7 1.309(6) . ? N2 N3 1.374(5) . ? N3 C8 1.295(6) . ? N4 C9 1.302(6) . ? N4 N5 1.376(6) . ? N5 C12 1.332(6) . ? N6 C12 1.382(7) . ? N6 C14 1.434(7) . ? N6 C13 1.439(7) . ? N7 C17 1.337(6) . ? N7 C18 1.340(5) . ? C1 C6 1.384(8) . ? C1 C2 1.400(7) . ? C2 C3 1.386(8) . ? C2 H2 0.9500 . ? C3 C4 1.375(9) . ? C3 H3 0.9500 . ? C4 C5 1.380(8) . ? C4 H4 0.9500 . ? C5 C6 1.381(8) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C8 C10 1.496(6) . ? C8 C9 1.504(7) . ? C9 C11 1.481(7) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C19 1.374(6) . ? C15 C16 1.399(6) . ? C16 C17 1.380(6) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.390(6) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C25 1.387(6) . ? C20 C21 1.396(7) . ? C21 C22 1.375(7) . ? C21 H21 0.9500 . ? C22 C23 1.372(8) . ? C22 H22 0.9500 . ? C23 C24 1.354(8) . ? C23 H23 0.9500 . ? C24 C25 1.411(7) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C31 1.387(7) . ? C26 C27 1.405(6) . ? C27 C28 1.386(8) . ? C27 H27 0.9500 . ? C28 C29 1.352(9) . ? C28 H28 0.9500 . ? C29 C30 1.376(9) . ? C29 H29 0.9500 . ? C30 C31 1.379(7) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C37 1.368(8) . ? C32 C33 1.383(8) . ? C32 C38 1.490(9) . ? C33 C34 1.340(9) . ? C33 H33 0.9500 . ? C34 C35 1.390(8) . ? C34 H34 0.9500 . ? C35 C36 1.357(8) . ? C35 H35 0.9500 . ? C36 C37 1.418(9) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? 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 N7 Zn1 N4 100.56(14) . . ? N7 Zn1 N3 104.76(13) . . ? N4 Zn1 N3 74.77(15) . . ? N7 Zn1 S1 105.71(11) . . ? N4 Zn1 S1 147.03(11) . . ? N3 Zn1 S1 79.50(11) . . ? N7 Zn1 S2 100.04(10) . . ? N4 Zn1 S2 80.04(11) . . ? N3 Zn1 S2 147.29(11) . . ? S1 Zn1 S2 113.89(5) . . ? C7 S1 Zn1 96.27(17) . . ? C12 S2 Zn1 95.64(17) . . ? C20 P1 C26 105.0(2) . . ? C20 P1 C15 102.38(19) . . ? C26 P1 C15 100.22(19) . . ? C7 N1 C1 132.2(4) . . ? C7 N1 H1 113.9 . . ? C1 N1 H1 113.9 . . ? C7 N2 N3 111.4(4) . . ? C8 N3 N2 119.8(4) . . ? C8 N3 Zn1 116.7(3) . . ? N2 N3 Zn1 123.2(3) . . ? C9 N4 N5 118.6(4) . . ? C9 N4 Zn1 118.3(3) . . ? N5 N4 Zn1 123.0(3) . . ? C12 N5 N4 111.5(4) . . ? C12 N6 C14 121.3(4) . . ? C12 N6 C13 123.6(5) . . ? C14 N6 C13 115.0(5) . . ? C17 N7 C18 117.1(4) . . ? C17 N7 Zn1 119.0(3) . . ? C18 N7 Zn1 123.7(3) . . ? C6 C1 C2 118.7(5) . . ? C6 C1 N1 117.0(5) . . ? C2 C1 N1 124.3(5) . . ? C3 C2 C1 119.0(5) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C4 C3 C2 121.6(5) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 119.6(6) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C6 119.3(6) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C5 C6 C1 121.8(6) . . ? C5 C6 H6 119.1 . . ? C1 C6 H6 119.1 . . ? N2 C7 N1 120.2(4) . . ? N2 C7 S1 126.9(4) . . ? N1 C7 S1 112.9(3) . . ? N3 C8 C10 124.6(4) . . ? N3 C8 C9 115.4(4) . . ? C10 C8 C9 120.0(4) . . ? N4 C9 C11 124.4(5) . . ? N4 C9 C8 113.5(4) . . ? C11 C9 C8 121.9(4) . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 N6 114.8(5) . . ? N5 C12 S2 127.1(4) . . ? N6 C12 S2 118.1(4) . . ? N6 C13 H13A 109.5 . . ? N6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N6 C14 H14A 109.5 . . ? N6 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N6 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C19 C15 C16 116.3(4) . . ? C19 C15 P1 123.9(3) . . ? C16 C15 P1 119.5(3) . . ? C17 C16 C15 120.0(4) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? N7 C17 C16 123.2(4) . . ? N7 C17 H17 118.4 . . ? C16 C17 H17 118.4 . . ? N7 C18 C19 122.6(4) . . ? N7 C18 H18 118.7 . . ? C19 C18 H18 118.7 . . ? C15 C19 C18 120.6(4) . . ? C15 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C25 C20 C21 117.9(4) . . ? C25 C20 P1 125.9(4) . . ? C21 C20 P1 116.1(3) . . ? C22 C21 C20 121.4(5) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C23 C22 C21 119.8(5) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C24 C23 C22 120.6(5) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 120.2(5) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C20 C25 C24 120.0(5) . . ? C20 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C31 C26 C27 117.7(5) . . ? C31 C26 P1 125.1(3) . . ? C27 C26 P1 117.1(4) . . ? C28 C27 C26 120.4(5) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C29 C28 C27 119.8(5) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 121.5(6) . . ? C28 C29 H29 119.2 . . ? C30 C29 H29 119.2 . . ? C29 C30 C31 119.0(6) . . ? C29 C30 H30 120.5 . . ? C31 C30 H30 120.5 . . ? C30 C31 C26 121.5(5) . . ? C30 C31 H31 119.3 . . ? C26 C31 H31 119.3 . . ? C37 C32 C33 118.0(6) . . ? C37 C32 C38 120.8(6) . . ? C33 C32 C38 121.2(7) . . ? C34 C33 C32 122.1(7) . . ? C34 C33 H33 119.0 . . ? C32 C33 H33 119.0 . . ? C33 C34 C35 120.7(6) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C36 C35 C34 118.9(6) . . ? C36 C35 H35 120.5 . . ? C34 C35 H35 120.5 . . ? C35 C36 C37 120.0(6) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C32 C37 C36 120.2(6) . . ? C32 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C32 C38 H38A 109.5 . . ? C32 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C32 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? 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 N7 Zn1 S1 C7 -91.72(17) . . . . ? N4 Zn1 S1 C7 49.8(3) . . . . ? N3 Zn1 S1 C7 10.81(17) . . . . ? S2 Zn1 S1 C7 159.45(15) . . . . ? N7 Zn1 S2 C12 87.60(18) . . . . ? N4 Zn1 S2 C12 -11.48(18) . . . . ? N3 Zn1 S2 C12 -51.4(3) . . . . ? S1 Zn1 S2 C12 -160.11(16) . . . . ? C7 N2 N3 C8 -171.4(4) . . . . ? C7 N2 N3 Zn1 15.2(5) . . . . ? N7 Zn1 N3 C8 -86.8(3) . . . . ? N4 Zn1 N3 C8 10.4(3) . . . . ? S1 Zn1 N3 C8 169.6(3) . . . . ? S2 Zn1 N3 C8 51.3(4) . . . . ? N7 Zn1 N3 N2 86.8(3) . . . . ? N4 Zn1 N3 N2 -176.0(3) . . . . ? S1 Zn1 N3 N2 -16.8(3) . . . . ? S2 Zn1 N3 N2 -135.1(3) . . . . ? N7 Zn1 N4 C9 94.5(3) . . . . ? N3 Zn1 N4 C9 -8.1(3) . . . . ? S1 Zn1 N4 C9 -48.0(4) . . . . ? S2 Zn1 N4 C9 -167.0(3) . . . . ? N7 Zn1 N4 N5 -82.7(3) . . . . ? N3 Zn1 N4 N5 174.7(3) . . . . ? S1 Zn1 N4 N5 134.8(3) . . . . ? S2 Zn1 N4 N5 15.8(3) . . . . ? C9 N4 N5 C12 170.3(4) . . . . ? Zn1 N4 N5 C12 -12.6(5) . . . . ? N4 Zn1 N7 C17 24.9(3) . . . . ? N3 Zn1 N7 C17 101.8(3) . . . . ? S1 Zn1 N7 C17 -175.2(3) . . . . ? S2 Zn1 N7 C17 -56.7(3) . . . . ? N4 Zn1 N7 C18 -160.7(3) . . . . ? N3 Zn1 N7 C18 -83.9(3) . . . . ? S1 Zn1 N7 C18 -0.9(3) . . . . ? S2 Zn1 N7 C18 117.6(3) . . . . ? C7 N1 C1 C6 -176.8(5) . . . . ? C7 N1 C1 C2 3.0(8) . . . . ? C6 C1 C2 C3 0.2(8) . . . . ? N1 C1 C2 C3 -179.6(5) . . . . ? C1 C2 C3 C4 -0.2(8) . . . . ? C2 C3 C4 C5 1.2(9) . . . . ? C3 C4 C5 C6 -2.1(10) . . . . ? C4 C5 C6 C1 2.1(10) . . . . ? C2 C1 C6 C5 -1.2(9) . . . . ? N1 C1 C6 C5 178.7(6) . . . . ? N3 N2 C7 N1 177.6(4) . . . . ? N3 N2 C7 S1 -1.8(5) . . . . ? C1 N1 C7 N2 -5.9(8) . . . . ? C1 N1 C7 S1 173.5(4) . . . . ? Zn1 S1 C7 N2 -9.2(4) . . . . ? Zn1 S1 C7 N1 171.4(3) . . . . ? N2 N3 C8 C10 -3.6(6) . . . . ? Zn1 N3 C8 C10 170.2(3) . . . . ? N2 N3 C8 C9 175.0(3) . . . . ? Zn1 N3 C8 C9 -11.2(4) . . . . ? N5 N4 C9 C11 -2.1(6) . . . . ? Zn1 N4 C9 C11 -179.4(3) . . . . ? N5 N4 C9 C8 -177.7(3) . . . . ? Zn1 N4 C9 C8 5.0(5) . . . . ? N3 C8 C9 N4 4.2(5) . . . . ? C10 C8 C9 N4 -177.2(4) . . . . ? N3 C8 C9 C11 -171.6(4) . . . . ? C10 C8 C9 C11 7.1(6) . . . . ? N4 N5 C12 N6 -179.6(4) . . . . ? N4 N5 C12 S2 -1.8(6) . . . . ? C14 N6 C12 N5 5.9(7) . . . . ? C13 N6 C12 N5 -176.7(5) . . . . ? C14 N6 C12 S2 -172.1(4) . . . . ? C13 N6 C12 S2 5.3(7) . . . . ? Zn1 S2 C12 N5 11.7(4) . . . . ? Zn1 S2 C12 N6 -170.5(3) . . . . ? C20 P1 C15 C19 -32.9(4) . . . . ? C26 P1 C15 C19 -140.9(3) . . . . ? C20 P1 C15 C16 153.0(3) . . . . ? C26 P1 C15 C16 45.1(4) . . . . ? C19 C15 C16 C17 2.1(6) . . . . ? P1 C15 C16 C17 176.6(3) . . . . ? C18 N7 C17 C16 0.0(6) . . . . ? Zn1 N7 C17 C16 174.7(3) . . . . ? C15 C16 C17 N7 -1.8(6) . . . . ? C17 N7 C18 C19 1.4(6) . . . . ? Zn1 N7 C18 C19 -173.0(3) . . . . ? C16 C15 C19 C18 -0.8(6) . . . . ? P1 C15 C19 C18 -175.0(3) . . . . ? N7 C18 C19 C15 -1.0(6) . . . . ? C26 P1 C20 C25 11.7(5) . . . . ? C15 P1 C20 C25 -92.5(4) . . . . ? C26 P1 C20 C21 -164.0(3) . . . . ? C15 P1 C20 C21 91.7(4) . . . . ? C25 C20 C21 C22 3.1(7) . . . . ? P1 C20 C21 C22 179.2(4) . . . . ? C20 C21 C22 C23 -1.8(7) . . . . ? C21 C22 C23 C24 -0.5(8) . . . . ? C22 C23 C24 C25 1.4(9) . . . . ? C21 C20 C25 C24 -2.1(7) . . . . ? P1 C20 C25 C24 -177.8(4) . . . . ? C23 C24 C25 C20 0.0(9) . . . . ? C20 P1 C26 C31 -68.5(4) . . . . ? C15 P1 C26 C31 37.4(4) . . . . ? C20 P1 C26 C27 115.0(3) . . . . ? C15 P1 C26 C27 -139.1(3) . . . . ? C31 C26 C27 C28 -1.9(6) . . . . ? P1 C26 C27 C28 174.9(4) . . . . ? C26 C27 C28 C29 0.9(8) . . . . ? C27 C28 C29 C30 1.3(9) . . . . ? C28 C29 C30 C31 -2.5(8) . . . . ? C29 C30 C31 C26 1.5(7) . . . . ? C27 C26 C31 C30 0.6(7) . . . . ? P1 C26 C31 C30 -175.9(4) . . . . ? C37 C32 C33 C34 -1.3(9) . . . . ? C38 C32 C33 C34 178.4(6) . . . . ? C32 C33 C34 C35 1.9(10) . . . . ? C33 C34 C35 C36 -1.2(9) . . . . ? C34 C35 C36 C37 -0.1(9) . . . . ? C33 C32 C37 C36 -0.1(9) . . . . ? C38 C32 C37 C36 -179.7(6) . . . . ? C35 C36 C37 C32 0.7(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 S1 0.88 2.61 3.463(4) 163.0 2_666 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.179 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.065 #===END