# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Mihail Barboiu' _publ_contact_author_email BARBOIU@IEMM.UNIV-MONTP2.FR _publ_section_title ; Self-sorting of equilibrating metallosupramolecular DCLs via constitutional crystallization. ; loop_ _publ_author_name 'Mihail Barboiu' 'Florina Dumitru' 'Yves-Maire Legrand' 'Eddy Petit' 'Arie van der Lee' # Attachment 'chemcom_barboiu.cif' #Self-sorting of equilibrating metallosupramolecular DCLs via constitutional #crystallization data_1 _database_code_depnum_ccdc_archive 'CCDC 715275' _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; All non-H atoms refined anisotropically The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; _cell_length_a 21.72580(13) _cell_length_b 10.8837(5) _cell_length_c 23.8728(6) _cell_angle_alpha 90 _cell_angle_beta 103.488(4) _cell_angle_gamma 90 _cell_volume 5489.2(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1 ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -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' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol 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' 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' Pb -3.3944 10.1111 31.0617 0.6902 13.0637 2.3576 18.4420 8.6180 5.9696 47.2579 13.4118 '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 # Given Formula = C29.50 H22.50 F3 N4.50 O3 Pb0.50 S0.50 # Dc = 0.80 Fooo = 2712.00 Mu = 15.97 M = 332.33 # Found Formula = C59 H45 F6 N9 O6 Pb1 S2 # Dc = 1.65 FOOO = 2712.00 Mu = 32.32 M = 680.69 _chemical_formula_sum 'C59 H45 F6 N9 O6 Pb1 S2' _chemical_formula_moiety 'C57 H45 N9 Pb, 2(C F3 O3 S)' _chemical_compound_source ? _chemical_formula_weight 1361.38 _cell_measurement_reflns_used 31170 _cell_measurement_theta_min 2.5869 _cell_measurement_theta_max 32.4305 _cell_measurement_temperature 173 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_max 0.31 _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2712 _exptl_absorpt_coefficient_mu 3.232 _exptl_absorpt_correction_T_min 0.82188 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_detector_area_resol_mean 8.4205 _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_measurement_device 'Oxford Diffraction XCALIBUR' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _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 173 _diffrn_reflns_number 53652 _reflns_number_total 9071 _diffrn_reflns_av_R_equivalents 0.025 # Number of reflections with Friedels Law is 9071 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 9917 _diffrn_orient_matrix_UB_11 -0.0202412809 _diffrn_orient_matrix_UB_12 0.0089249008 _diffrn_orient_matrix_UB_13 0.0190394915 _diffrn_orient_matrix_UB_21 -0.0144649921 _diffrn_orient_matrix_UB_22 -0.0577062239 _diffrn_orient_matrix_UB_23 -0.0083049471 _diffrn_orient_matrix_UB_31 0.0225322014 _diffrn_orient_matrix_UB_32 -0.0289594615 _diffrn_orient_matrix_UB_33 0.0224178998 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -54.00 61.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 30.0000 -79.0000 0.0000 0.0000 0.0000 115 #__ type_ start__ end____ width___ exp.time_ 2 omega -54.00 61.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 30.0000 -79.0000 90.0000 0.0000 0.0000 115 #__ type_ start__ end____ width___ exp.time_ 3 omega -54.00 61.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 30.0000 -79.0000 180.0000 0.0000 0.0000 115 #__ type_ start__ end____ width___ exp.time_ 4 omega -54.00 61.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 30.0000 -79.0000 270.0000 0.0000 0.0000 115 #__ type_ start__ end____ width___ exp.time_ 5 omega -111.00 10.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -25.0000 -80.0000 100.0000 0.0000 0.0000 121 #__ type_ start__ end____ width___ exp.time_ 6 omega -116.00 71.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -25.0000 -10.0000 180.0000 0.0000 0.0000 187 #__ type_ start__ end____ width___ exp.time_ 7 omega -110.00 12.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -25.0000 -80.0000 0.0000 0.0000 0.0000 122 ; _diffrn_reflns_theta_min 2.593 _diffrn_reflns_theta_max 32.479 _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 30.205 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 34 _reflns_limit_h_min -32 _reflns_limit_h_max 30 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 36 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.49 _refine_diff_density_max 0.86 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 7973 _refine_ls_number_restraints 0 _refine_ls_number_parameters 378 _oxford_refine_ls_R_factor_ref 0.0209 _refine_ls_wR_factor_ref 0.0202 _refine_ls_goodness_of_fit_ref 1.0782 _refine_ls_shift/su_max 0.001756 # The values computed from all data _oxford_reflns_number_all 9071 _refine_ls_R_factor_all 0.0286 _refine_ls_wR_factor_all 0.0204 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 7973 _refine_ls_R_factor_gt 0.0209 _refine_ls_wR_factor_gt 0.0202 # 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 constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _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: 4.94 -5.69 3.35 -0.790 -0.154 ; # 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. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. 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. Oxford Diffraction, (2002). CrysAlis RED. Oxford Diffraction, (2002). Xcalibur User Manual. 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Pb1 Pb 0.5000 0.562998(8) 0.2500 0.0179 1.0000 Uani S T . . . . . S2 S 0.21578(3) 0.49664(5) 0.42226(2) 0.0371 1.0000 Uani . . . . . . . O3 O 0.23405(11) 0.59862(16) 0.45925(7) 0.0642 1.0000 Uani . . . . . . . O4 O 0.16997(12) 0.5204(2) 0.37063(8) 0.0725 1.0000 Uani . . . . . . . O5 O 0.26728(12) 0.4206(3) 0.41465(14) 0.0926 1.0000 Uani . . . . . . . C6 C 0.17490(13) 0.3979(2) 0.46279(11) 0.0502 1.0000 Uani . . . . . . . F7 F 0.15676(11) 0.29323(17) 0.43556(9) 0.0842 1.0000 Uani . . . . . . . F8 F 0.12269(11) 0.4509(2) 0.47081(11) 0.1018 1.0000 Uani . . . . . . . F9 F 0.21031(12) 0.3719(2) 0.51423(8) 0.0912 1.0000 Uani . . . . . . . N10 N 0.59412(6) 0.45553(12) 0.32893(5) 0.0203 1.0000 Uani . . . . . . . C11 C 0.60504(8) 0.48966(15) 0.38441(7) 0.0223 1.0000 Uani . . . . . . . C12 C 0.65637(8) 0.44529(18) 0.42631(7) 0.0293 1.0000 Uani . . . . . . . C13 C 0.69701(9) 0.36215(18) 0.41039(8) 0.0313 1.0000 Uani . . . . . . . C14 C 0.68591(9) 0.32575(16) 0.35331(8) 0.0289 1.0000 Uani . . . . . . . C15 C 0.63405(8) 0.37450(14) 0.31389(7) 0.0219 1.0000 Uani . . . . . . . C16 C 0.61999(8) 0.33214(15) 0.25349(7) 0.0243 1.0000 Uani . . . . . . . N17 N 0.56910(7) 0.36083(14) 0.21705(6) 0.0253 1.0000 Uani . . . . . . . C18 C 0.56050(9) 0.31561(16) 0.15946(7) 0.0268 1.0000 Uani . . . . . . . C19 C 0.50196(10) 0.26545(18) 0.13273(8) 0.0329 1.0000 Uani . . . . . . . C20 C 0.49127(12) 0.2230(2) 0.07615(9) 0.0417 1.0000 Uani . . . . . . . C21 C 0.53817(13) 0.2330(2) 0.04631(8) 0.0448 1.0000 Uani . . . . . . . C22 C 0.59607(12) 0.2831(2) 0.07239(9) 0.0411 1.0000 Uani . . . . . . . C23 C 0.60781(10) 0.32430(18) 0.12931(8) 0.0331 1.0000 Uani . . . . . . . H24 H 0.6469 0.3580 0.1469 0.0500 1.0000 Uiso R . . . . . . H25 H 0.6279 0.2918 0.0530 0.0500 1.0000 Uiso R . . . . . . H26 H 0.5312 0.2045 0.0086 0.0500 1.0000 Uiso R . . . . . . H27 H 0.4523 0.1882 0.0585 0.0500 1.0000 Uiso R . . . . . . H28 H 0.4703 0.2591 0.1532 0.0500 1.0000 Uiso R . . . . . . H29 H 0.6501 0.2812 0.2426 0.0500 1.0000 Uiso R . . . . . . H30 H 0.7123 0.2694 0.3411 0.0500 1.0000 Uiso R . . . . . . H31 H 0.7315 0.3305 0.4378 0.0500 1.0000 Uiso R . . . . . . H32 H 0.6626 0.4718 0.4643 0.0500 1.0000 Uiso R . . . . . . C33 C 0.55960(8) 0.57405(16) 0.40128(6) 0.0244 1.0000 Uani . . . . . . . N34 N 0.51489(7) 0.62489(14) 0.36523(6) 0.0260 1.0000 Uani . . . . . . . C35 C 0.47149(8) 0.69994(16) 0.38692(6) 0.0248 1.0000 Uani . . . . . . . C36 C 0.47399(9) 0.82679(17) 0.38298(7) 0.0303 1.0000 Uani . . . . . . . C37 C 0.43036(11) 0.8981(2) 0.40291(9) 0.0378 1.0000 Uani . . . . . . . C38 C 0.38437(10) 0.8435(2) 0.42581(9) 0.0407 1.0000 Uani . . . . . . . C39 C 0.38173(10) 0.7170(2) 0.42952(9) 0.0410 1.0000 Uani . . . . . . . C40 C 0.42577(10) 0.64501(19) 0.41039(8) 0.0343 1.0000 Uani . . . . . . . H41 H 0.4247 0.5595 0.4136 0.0500 1.0000 Uiso R . . . . . . H42 H 0.3501 0.6788 0.4448 0.0500 1.0000 Uiso R . . . . . . H43 H 0.3550 0.8921 0.4385 0.0500 1.0000 Uiso R . . . . . . H44 H 0.4323 0.9841 0.4004 0.0500 1.0000 Uiso R . . . . . . H45 H 0.5049 0.8638 0.3674 0.0500 1.0000 Uiso R . . . . . . H46 H 0.5644 0.5894 0.4409 0.0500 1.0000 Uiso R . . . . . . N47 N 0.5000 0.81478(18) 0.2500 0.0174 1.0000 Uani S T . . . . . C48 C 0.55414(7) 0.87845(14) 0.26448(7) 0.0194 1.0000 Uani . . . . . . . C49 C 0.55614(8) 1.00651(15) 0.26654(7) 0.0237 1.0000 Uani . . . . . . . C50 C 0.500000(7) 1.0712(2) 0.250000(7) 0.0256 1.0000 Uani S T . . . . . H51 H 0.5000 1.1568 0.2500 0.0500 1.0000 Uiso RS . . . . . . H52 H 0.5952 1.0467 0.2787 0.0500 1.0000 Uiso R . . . . . . C53 C 0.61404(7) 0.80927(15) 0.27636(7) 0.0210 1.0000 Uani . . . . . . . N54 N 0.61634(6) 0.69686(13) 0.26250(6) 0.0215 1.0000 Uani . . . . . . . C55 C 0.67739(7) 0.64134(15) 0.27354(7) 0.0216 1.0000 Uani . . . . . . . C56 C 0.69335(8) 0.57604(19) 0.22886(7) 0.0299 1.0000 Uani . . . . . . . C57 C 0.75172(10) 0.5181(2) 0.23791(9) 0.0401 1.0000 Uani . . . . . . . C58 C 0.79343(9) 0.5225(2) 0.29172(9) 0.0370 1.0000 Uani . . . . . . . C59 C 0.77737(8) 0.58761(17) 0.33601(8) 0.0301 1.0000 Uani . . . . . . . C60 C 0.71964(8) 0.64848(16) 0.32723(7) 0.0248 1.0000 Uani . . . . . . . H61 H 0.7090 0.6919 0.3573 0.0500 1.0000 Uiso R . . . . . . H62 H 0.8053 0.5904 0.3721 0.0500 1.0000 Uiso R . . . . . . H63 H 0.8327 0.4814 0.2985 0.0500 1.0000 Uiso R . . . . . . H64 H 0.7627 0.4749 0.2076 0.0500 1.0000 Uiso R . . . . . . H65 H 0.6648 0.5734 0.1927 0.0500 1.0000 Uiso R . . . . . . H66 H 0.6511 0.8528 0.2933 0.0500 1.0000 Uiso 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 Pb1 0.01874(3) 0.01855(3) 0.01507(3) 0.0000 0.00098(2) 0.0000 S2 0.0452(3) 0.0343(2) 0.0285(2) 0.00171(18) 0.00173(19) -0.0073(2) O3 0.0999(16) 0.0378(9) 0.0366(8) 0.0021(7) -0.0210(9) -0.0217(9) O4 0.0904(16) 0.0764(14) 0.0334(9) 0.0002(9) -0.0204(9) -0.0149(12) O5 0.0779(16) 0.0866(18) 0.135(2) 0.0226(17) 0.0693(17) 0.0164(14) C6 0.0638(15) 0.0476(12) 0.0474(12) -0.0163(10) 0.0295(12) -0.0169(11) F7 0.1190(16) 0.0553(10) 0.0953(14) -0.0325(10) 0.0597(13) -0.0487(11) F8 0.0834(14) 0.1164(19) 0.1290(19) -0.0391(16) 0.0725(14) -0.0109(13) F9 0.144(2) 0.0797(13) 0.0482(10) 0.0213(9) 0.0186(11) -0.0294(13) N10 0.0235(6) 0.0189(6) 0.0165(5) 0.0003(4) 0.0004(4) 0.0008(5) C11 0.0250(7) 0.0215(7) 0.0177(6) 0.0004(5) -0.0004(5) 0.0002(6) C12 0.0334(8) 0.0320(8) 0.0178(6) 0.0017(7) -0.0038(6) 0.0026(7) C13 0.0302(8) 0.0313(8) 0.0260(8) 0.0037(7) -0.0065(6) 0.0063(7) C14 0.0300(8) 0.0244(8) 0.0285(8) 0.0015(6) -0.0007(6) 0.0078(6) C15 0.0242(7) 0.0184(7) 0.0212(7) 0.0003(5) 0.0014(5) 0.0010(5) C16 0.0290(8) 0.0199(7) 0.0229(7) -0.0012(5) 0.0038(6) 0.0044(6) N17 0.0311(7) 0.0246(6) 0.0188(6) -0.0039(5) 0.0028(5) 0.0050(5) C18 0.0377(9) 0.0215(7) 0.0189(6) -0.0029(6) 0.0016(6) 0.0103(6) C19 0.0382(10) 0.0310(9) 0.0247(8) -0.0040(7) -0.0024(7) 0.0099(7) C20 0.0518(12) 0.0377(10) 0.0272(9) -0.0082(8) -0.0079(8) 0.0101(9) C21 0.0716(15) 0.0390(11) 0.0188(8) -0.0050(7) 0.0005(9) 0.0147(10) C22 0.0641(14) 0.0355(10) 0.0261(9) -0.0004(7) 0.0154(9) 0.0130(10) C23 0.0447(10) 0.0294(8) 0.0253(8) -0.0026(7) 0.0083(7) 0.0088(8) C33 0.0287(7) 0.0270(8) 0.0158(6) -0.0032(6) 0.0014(5) 0.0003(6) N34 0.0311(7) 0.0271(7) 0.0188(6) -0.0032(5) 0.0038(5) 0.0047(6) C35 0.0280(7) 0.0286(8) 0.0154(6) -0.0046(6) 0.0000(5) 0.0032(6) C36 0.0378(9) 0.0292(8) 0.0239(7) -0.0024(6) 0.0072(7) 0.0015(7) C37 0.0479(11) 0.0302(9) 0.0336(9) -0.0045(7) 0.0062(8) 0.0094(8) C38 0.0340(10) 0.0512(13) 0.0356(10) -0.0102(9) 0.0052(8) 0.0137(9) C39 0.0306(9) 0.0555(13) 0.0383(10) -0.0074(9) 0.0111(8) -0.0041(9) C40 0.0380(10) 0.0326(9) 0.0326(9) -0.0056(7) 0.0087(7) -0.0052(8) N47 0.0168(7) 0.0155(7) 0.0197(8) 0.0000 0.0036(6) 0.0000 C48 0.0179(6) 0.0195(7) 0.0201(6) 0.0003(5) 0.0030(5) -0.0004(5) C49 0.0235(7) 0.0189(7) 0.0264(7) -0.0001(6) 0.0012(6) -0.0031(6) C50 0.0273(10) 0.0159(9) 0.0302(10) 0.0000 -0.0003(8) 0.0000 C53 0.0159(6) 0.0213(7) 0.0252(7) 0.0022(6) 0.0037(5) -0.0015(5) N54 0.0163(5) 0.0226(6) 0.0248(6) -0.0003(5) 0.0029(5) 0.0016(5) C55 0.0164(6) 0.0216(7) 0.0266(7) 0.0004(6) 0.0048(5) 0.0008(5) C56 0.0252(7) 0.0398(10) 0.0232(7) -0.0032(7) 0.0026(6) 0.0095(7) C57 0.0344(10) 0.0573(13) 0.0294(9) -0.0031(9) 0.0091(7) 0.0197(9) C58 0.0243(8) 0.0514(11) 0.0353(9) 0.0011(8) 0.0070(7) 0.0158(8) C59 0.0212(7) 0.0367(10) 0.0292(8) -0.0001(7) -0.0007(6) 0.0045(6) C60 0.0214(7) 0.0268(8) 0.0253(7) -0.0038(6) 0.0036(6) 0.0013(6) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.6301(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 Pb1 . N10 5_655 2.7024(12) yes Pb1 . N34 5_655 2.7768(14) yes Pb1 . N54 5_655 2.8720(13) yes Pb1 . N17 5_655 2.8748(14) yes Pb1 . N10 . 2.7024(12) yes Pb1 . N17 . 2.8748(14) yes Pb1 . N34 . 2.7768(14) yes Pb1 . N47 . 2.7403(19) yes Pb1 . N54 . 2.8720(13) yes S2 . O3 . 1.4162(17) yes S2 . O4 . 1.4157(18) yes S2 . O5 . 1.437(2) yes S2 . C6 . 1.811(2) yes C6 . F7 . 1.325(3) yes C6 . F8 . 1.326(3) yes C6 . F9 . 1.319(3) yes N10 . C11 . 1.3425(19) yes N10 . C15 . 1.343(2) yes C11 . C12 . 1.399(2) yes C11 . C33 . 1.472(2) yes C12 . C13 . 1.378(3) yes C12 . H32 . 0.931 no C13 . C14 . 1.385(3) yes C13 . H31 . 0.937 no C14 . C15 . 1.394(2) yes C14 . H30 . 0.932 no C15 . C16 . 1.476(2) yes C16 . N17 . 1.276(2) yes C16 . H29 . 0.939 no N17 . C18 . 1.431(2) yes C18 . C19 . 1.394(3) yes C18 . C23 . 1.389(3) yes C19 . C20 . 1.395(3) yes C19 . H28 . 0.935 no C20 . C21 . 1.377(4) yes C20 . H27 . 0.934 no C21 . C22 . 1.379(4) yes C21 . H26 . 0.930 no C22 . C23 . 1.397(3) yes C22 . H25 . 0.923 no C23 . H24 . 0.930 no C33 . N34 . 1.265(2) yes C33 . H46 . 0.943 no N34 . C35 . 1.432(2) yes C35 . C36 . 1.386(3) yes C35 . C40 . 1.385(3) yes C36 . C37 . 1.392(3) yes C36 . H45 . 0.932 no C37 . C38 . 1.380(3) yes C37 . H44 . 0.939 no C38 . C39 . 1.382(3) yes C38 . H43 . 0.932 no C39 . C40 . 1.393(3) yes C39 . H42 . 0.944 no C40 . H41 . 0.934 no N47 . C48 5_655 1.3392(18) yes N47 . C48 . 1.3392(18) yes C48 . C49 . 1.395(2) yes C48 . C53 . 1.473(2) yes C49 . C50 . 1.384(2) yes C49 . H52 . 0.939 no C50 . H51 . 0.932 no C53 . N54 . 1.271(2) yes C53 . H66 . 0.940 no N54 . C55 . 1.4250(19) yes C55 . C56 . 1.391(2) yes C55 . C60 . 1.394(2) yes C56 . C57 . 1.388(2) yes C56 . H65 . 0.939 no C57 . C58 . 1.389(3) yes C57 . H64 . 0.938 no C58 . C59 . 1.384(3) yes C58 . H63 . 0.943 no C59 . C60 . 1.390(2) yes C59 . H62 . 0.932 no C60 . H61 . 0.932 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 N10 5_655 Pb1 . N34 5_655 61.31(4) yes N10 5_655 Pb1 . N54 5_655 69.06(4) yes N34 5_655 Pb1 . N54 5_655 82.97(4) yes N10 5_655 Pb1 . N17 5_655 60.06(4) yes N34 5_655 Pb1 . N17 5_655 120.60(4) yes N54 5_655 Pb1 . N17 5_655 85.04(4) yes N10 5_655 Pb1 . N10 . 128.71(5) yes N34 5_655 Pb1 . N10 . 133.64(4) yes N54 5_655 Pb1 . N10 . 142.80(4) yes N17 5_655 Pb1 . N10 . 80.59(4) yes N10 5_655 Pb1 . N17 . 80.59(4) yes N34 5_655 Pb1 . N17 . 82.08(4) yes N54 5_655 Pb1 . N17 . 149.64(4) yes N17 5_655 Pb1 . N17 . 80.12(6) yes N10 . Pb1 . N17 . 60.06(4) yes N10 5_655 Pb1 . N34 . 133.64(4) yes N34 5_655 Pb1 . N34 . 151.92(6) yes N54 5_655 Pb1 . N34 . 82.89(4) yes N17 5_655 Pb1 . N34 . 82.08(4) yes N10 . Pb1 . N34 . 61.31(4) yes N10 5_655 Pb1 . N47 . 115.65(3) yes N34 5_655 Pb1 . N47 . 75.96(3) yes N54 5_655 Pb1 . N47 . 59.52(3) yes N17 5_655 Pb1 . N47 . 139.94(3) yes N10 . Pb1 . N47 . 115.65(3) yes N10 5_655 Pb1 . N54 . 142.80(4) yes N34 5_655 Pb1 . N54 . 82.89(4) yes N54 5_655 Pb1 . N54 . 119.04(5) yes N17 5_655 Pb1 . N54 . 149.64(4) yes N10 . Pb1 . N54 . 69.06(4) yes N17 . Pb1 . N34 . 120.60(4) yes N17 . Pb1 . N47 . 139.94(3) yes N34 . Pb1 . N47 . 75.96(3) yes N17 . Pb1 . N54 . 85.04(4) yes N34 . Pb1 . N54 . 82.97(4) yes N47 . Pb1 . N54 . 59.52(3) yes O3 . S2 . O4 . 115.96(13) yes O3 . S2 . O5 . 114.64(17) yes O4 . S2 . O5 . 113.90(17) yes O3 . S2 . C6 . 103.46(12) yes O4 . S2 . C6 . 103.93(14) yes O5 . S2 . C6 . 102.67(14) yes S2 . C6 . F7 . 112.00(17) yes S2 . C6 . F8 . 111.2(2) yes F7 . C6 . F8 . 106.2(2) yes S2 . C6 . F9 . 111.88(19) yes F7 . C6 . F9 . 108.3(3) yes F8 . C6 . F9 . 107.0(2) yes Pb1 . N10 . C11 . 119.93(10) yes Pb1 . N10 . C15 . 121.91(10) yes C11 . N10 . C15 . 117.96(13) yes N10 . C11 . C12 . 122.54(15) yes N10 . C11 . C33 . 117.85(13) yes C12 . C11 . C33 . 119.58(14) yes C11 . C12 . C13 . 118.99(15) yes C11 . C12 . H32 . 120.1 no C13 . C12 . H32 . 121.0 no C12 . C13 . C14 . 118.91(15) yes C12 . C13 . H31 . 120.6 no C14 . C13 . H31 . 120.5 no C13 . C14 . C15 . 118.89(16) yes C13 . C14 . H30 . 121.1 no C15 . C14 . H30 . 120.0 no C14 . C15 . N10 . 122.70(15) yes C14 . C15 . C16 . 119.42(15) yes N10 . C15 . C16 . 117.82(13) yes C15 . C16 . N17 . 122.59(15) yes C15 . C16 . H29 . 117.2 no N17 . C16 . H29 . 120.2 no C16 . N17 . Pb1 . 115.18(11) yes C16 . N17 . C18 . 117.98(15) yes Pb1 . N17 . C18 . 124.52(10) yes N17 . C18 . C19 . 118.37(17) yes N17 . C18 . C23 . 121.86(17) yes C19 . C18 . C23 . 119.73(16) yes C18 . C19 . C20 . 120.1(2) yes C18 . C19 . H28 . 119.6 no C20 . C19 . H28 . 120.3 no C19 . C20 . C21 . 119.9(2) yes C19 . C20 . H27 . 119.9 no C21 . C20 . H27 . 120.1 no C20 . C21 . C22 . 120.29(18) yes C20 . C21 . H26 . 120.1 no C22 . C21 . H26 . 119.6 no C21 . C22 . C23 . 120.4(2) yes C21 . C22 . H25 . 121.7 no C23 . C22 . H25 . 117.9 no C22 . C23 . C18 . 119.5(2) yes C22 . C23 . H24 . 120.4 no C18 . C23 . H24 . 120.1 no C11 . C33 . N34 . 122.99(14) yes C11 . C33 . H46 . 117.5 no N34 . C33 . H46 . 119.5 no C33 . N34 . Pb1 . 117.47(11) yes C33 . N34 . C35 . 117.98(14) yes Pb1 . N34 . C35 . 124.19(10) yes N34 . C35 . C36 . 120.27(17) yes N34 . C35 . C40 . 119.65(17) yes C36 . C35 . C40 . 120.05(17) yes C35 . C36 . C37 . 119.46(19) yes C35 . C36 . H45 . 120.1 no C37 . C36 . H45 . 120.5 no C36 . C37 . C38 . 120.6(2) yes C36 . C37 . H44 . 119.4 no C38 . C37 . H44 . 120.0 no C37 . C38 . C39 . 119.95(19) yes C37 . C38 . H43 . 119.9 no C39 . C38 . H43 . 120.1 no C38 . C39 . C40 . 119.8(2) yes C38 . C39 . H42 . 120.5 no C40 . C39 . H42 . 119.7 no C39 . C40 . C35 . 120.15(19) yes C39 . C40 . H41 . 120.1 no C35 . C40 . H41 . 119.8 no C48 5_655 N47 . Pb1 . 121.17(10) yes C48 5_655 N47 . C48 . 117.67(19) yes Pb1 . N47 . C48 . 121.17(10) yes N47 . C48 . C49 . 122.99(16) yes N47 . C48 . C53 . 117.94(14) yes C49 . C48 . C53 . 119.02(15) yes C48 . C49 . C50 . 118.71(17) yes C48 . C49 . H52 . 119.6 no C50 . C49 . H52 . 121.6 no C49 . C50 . C49 5_655 118.8(2) yes C49 . C50 . H51 . 120.6 no C49 5_655 C50 . H51 . 120.6 no C48 . C53 . N54 . 121.90(14) yes C48 . C53 . H66 . 117.0 no N54 . C53 . H66 . 121.0 no C53 . N54 . Pb1 . 115.35(10) yes C53 . N54 . C55 . 116.83(13) yes Pb1 . N54 . C55 . 124.24(10) yes N54 . C55 . C56 . 117.55(14) yes N54 . C55 . C60 . 122.09(14) yes C56 . C55 . C60 . 120.34(14) yes C55 . C56 . C57 . 119.66(16) yes C55 . C56 . H65 . 119.4 no C57 . C56 . H65 . 120.9 no C56 . C57 . C58 . 120.25(18) yes C56 . C57 . H64 . 119.6 no C58 . C57 . H64 . 120.1 no C57 . C58 . C59 . 119.86(17) yes C57 . C58 . H63 . 120.8 no C59 . C58 . H63 . 119.4 no C58 . C59 . C60 . 120.55(16) yes C58 . C59 . H62 . 119.8 no C60 . C59 . H62 . 119.6 no C55 . C60 . C59 . 119.31(15) yes C55 . C60 . H61 . 120.5 no C59 . C60 . H61 . 120.1 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C13 . H31 . O3 2_666 125 0.94 2.52 3.152(3) yes C49 . H52 . O4 3_555 126 0.94 2.42 3.074(3) yes C53 . H66 . O4 3_555 130 0.94 2.56 3.247(3) yes #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 715276' _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; One triflate molecule disordered over two parts. The two different parts were refined as rigid bodies with one isotropic temp factor each The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _cell_length_a 8.9330(3) _cell_length_b 10.5894(4) _cell_length_c 30.0903(10) _cell_angle_alpha 81.785(3) _cell_angle_beta 89.709(3) _cell_angle_gamma 87.927(3) _cell_volume 2815.34(17) _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 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' 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' 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' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol 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' _cell_formula_units_Z 2 # Given Formula = C63 F6 N9 O4 S2 Zn2 # Dc = 1.48 Fooo = 1496.00 Mu = 10.03 M = 1255.63 # Found Formula = C46 H40 F12 N8 O18 S4 Zn2 # Dc = 1.75 FOOO = 1496.00 Mu = 11.20 M = 1479.87 _chemical_formula_sum 'C46 H40 F12 N8 O18 S4 Zn2' _chemical_formula_moiety '2(C22 H20 F3 N4 O6 S Zn), 2(C F3 O3 S)' _chemical_compound_source ? _chemical_formula_weight 1479.87 _cell_measurement_reflns_used 8107 _cell_measurement_theta_min 3.6799 _cell_measurement_theta_max 33.6074 _cell_measurement_temperature 173 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_max 0.27 _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 1.120 # Sheldrick geometric approximatio 0.79 0.85 _exptl_absorpt_correction_T_min 0.94192 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_detector_area_resol_mean 16.0143 _diffrn_measurement_device 'Oxford Diffraction XCALIBUR' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_sigmaI/netI 0.087 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _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_orient_matrix_UB_11 -0.0538779135 _diffrn_orient_matrix_UB_12 -0.0234299333 _diffrn_orient_matrix_UB_13 -0.0136635994 _diffrn_orient_matrix_UB_21 0.0049740005 _diffrn_orient_matrix_UB_22 -0.0602581653 _diffrn_orient_matrix_UB_23 0.0136952337 _diffrn_orient_matrix_UB_31 -0.0580543030 _diffrn_orient_matrix_UB_32 0.0198967321 _diffrn_orient_matrix_UB_33 0.0138547070 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 27.47 100.47 1.0000 5.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 32.0000 -140.0000 -40.0000 0.0000 0.0000 73 #__ type_ start__ end____ width___ exp.time_ 2 omega 2.00 103.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 32.0000 70.0000 -140.0000 0.0000 0.0000 101 #__ type_ start__ end____ width___ exp.time_ 3 omega -83.69 -5.69 1.0000 5.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -32.0000 110.0000 -290.0000 0.0000 0.0000 78 #__ type_ start__ end____ width___ exp.time_ 4 phi -180.00 170.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames 0.0000 32.0000 0.0000 - 0.0000 0.0000 350 #__ type_ start__ end____ width___ exp.time_ 5 omega 2.00 103.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 32.0000 70.0000 -20.0000 0.0000 0.0000 101 #__ type_ start__ end____ width___ exp.time_ 6 omega 2.00 103.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 32.0000 70.0000 -270.0000 0.0000 0.0000 101 ; _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 173 _diffrn_reflns_number 58657 _reflns_number_total 20555 _diffrn_reflns_av_R_equivalents 0.070 # Number of reflections with Friedels Law is 20555 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 21912 _diffrn_reflns_theta_min 3.686 _diffrn_reflns_theta_max 33.665 _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 30.635 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min -15 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 46 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -2.13 _refine_diff_density_max 2.20 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 7062 _refine_ls_number_restraints 1036 _refine_ls_number_parameters 761 _oxford_refine_ls_R_factor_ref 0.0689 _refine_ls_wR_factor_ref 0.0738 _refine_ls_goodness_of_fit_ref 0.8913 _refine_ls_shift/su_max 0.000535 # The values computed from all data _oxford_reflns_number_all 20555 _refine_ls_R_factor_all 0.1635 _refine_ls_wR_factor_all 0.1253 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 7062 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_gt 0.0738 # 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 constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _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: 15.3 -7.15 8.18 ; # 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. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. 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. Oxford Diffraction, (2002). CrysAlis RED. Oxford Diffraction, (2002). Xcalibur User Manual. 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Zn1 Zn 0.30135(10) 0.24071(8) 0.40042(3) 0.0233 1.0000 Uani . . . . . . . O2 O 0.5000(6) 0.2688(5) 0.42642(17) 0.0283 1.0000 Uani . . . . . . . O3 O 0.3515(6) 0.0518(4) 0.44985(17) 0.0273 1.0000 Uani . . . . . . . S4 S 0.3223(2) -0.08335(17) 0.45860(6) 0.0206 1.0000 Uani . . . . . . . O5 O 0.1966(6) -0.1228(5) 0.4350(2) 0.0380 1.0000 Uani . . . . . . . O6 O 0.3327(6) -0.1377(5) 0.50517(16) 0.0272 1.0000 Uani . . . . . . . C7 C 0.4833(10) -0.1558(7) 0.4330(3) 0.0332 1.0000 Uani . . . . . . . F8 F 0.6101(6) -0.1337(5) 0.4532(2) 0.0594 1.0000 Uani . . . . . . . F9 F 0.4726(6) -0.2812(4) 0.43617(17) 0.0495 1.0000 Uani . . . . . . . F10 F 0.4938(7) -0.1089(5) 0.39032(17) 0.0626 1.0000 Uani . . . . . . . N11 N 0.1365(6) 0.2815(5) 0.45472(19) 0.0197 1.0000 Uani . . . . . . . C12 C 0.1596(8) 0.3534(6) 0.4905(2) 0.0208 1.0000 Uani . . . . . . . C13 C 0.2623(8) 0.4496(7) 0.4840(2) 0.0244 1.0000 Uani . . . . . . . C14 C 0.2924(9) 0.5215(6) 0.5176(2) 0.0269 1.0000 Uani . . . . . . . C15 C 0.2233(8) 0.4954(7) 0.5583(2) 0.0233 1.0000 Uani . . . . . . . O16 O 0.2582(6) 0.5684(5) 0.59120(18) 0.0316 1.0000 Uani . . . . . . . C17 C 0.1227(9) 0.3977(7) 0.5657(3) 0.0313 1.0000 Uani . . . . . . . C18 C 0.0911(9) 0.3266(7) 0.5320(2) 0.0266 1.0000 Uani . . . . . . . C19 C 0.0135(8) 0.2254(7) 0.4511(2) 0.0219 1.0000 Uani . . . . . . . C20 C -0.0013(8) 0.1500(7) 0.4140(2) 0.0235 1.0000 Uani . . . . . . . N21 N 0.1138(6) 0.1530(5) 0.38585(19) 0.0195 1.0000 Uani . . . . . . . C22 C 0.1177(8) 0.0818(7) 0.3527(2) 0.0206 1.0000 Uani . . . . . . . C23 C 0.0016(8) 0.0052(7) 0.3453(2) 0.0254 1.0000 Uani . . . . . . . C24 C -0.1199(9) 0.0022(8) 0.3738(3) 0.0324 1.0000 Uani . . . . . . . C25 C -0.1241(8) 0.0733(7) 0.4088(2) 0.0259 1.0000 Uani . . . . . . . C26 C 0.2574(8) 0.0889(7) 0.3270(2) 0.0229 1.0000 Uani . . . . . . . N27 N 0.3669(7) 0.1504(5) 0.3397(2) 0.0226 1.0000 Uani . . . . . . . C28 C 0.5060(8) 0.1521(7) 0.3163(2) 0.0198 1.0000 Uani . . . . . . . C29 C 0.5557(9) 0.0507(7) 0.2941(3) 0.0294 1.0000 Uani . . . . . . . C30 C 0.6913(9) 0.0580(8) 0.2711(3) 0.0326 1.0000 Uani . . . . . . . C31 C 0.7747(9) 0.1656(7) 0.2699(3) 0.0293 1.0000 Uani . . . . . . . O32 O 0.9099(6) 0.1764(6) 0.2478(2) 0.0422 1.0000 Uani . . . . . . . C33 C 0.7306(9) 0.2645(7) 0.2933(3) 0.0296 1.0000 Uani . . . . . . . C34 C 0.5957(8) 0.2568(7) 0.3167(2) 0.0250 1.0000 Uani . . . . . . . N35 N 0.2735(8) 0.4320(6) 0.3688(2) 0.0317 1.0000 Uani . . . . . . . C36 C 0.2485(8) 0.5372(7) 0.3589(2) 0.0301 1.0000 Uani . . . . . . . C37 C 0.2131(9) 0.6739(7) 0.3478(3) 0.0435 1.0000 Uani . . . . . . . Zn38 Zn 0.69765(10) 0.26508(9) 0.10167(3) 0.0289 1.0000 Uani . . . . . . . O39 O 0.6526(6) 0.4545(5) 0.05386(18) 0.0329 1.0000 Uani . . . . . . . S40 S 0.6781(2) 0.59076(18) 0.04581(6) 0.0252 1.0000 Uani . . . . . . . O41 O 0.8009(7) 0.6313(6) 0.0699(2) 0.0451 1.0000 Uani . . . . . . . O42 O 0.6674(6) 0.6460(5) -0.00086(19) 0.0352 1.0000 Uani . . . . . . . C43 C 0.5124(11) 0.6576(8) 0.0706(4) 0.0453 1.0000 Uani . . . . . . . F44 F 0.5005(7) 0.6124(5) 0.11373(19) 0.0622 1.0000 Uani . . . . . . . F45 F 0.5183(7) 0.7841(5) 0.0674(2) 0.0620 1.0000 Uani . . . . . . . F46 F 0.3886(6) 0.6316(6) 0.0501(2) 0.0667 1.0000 Uani . . . . . . . O47 O 0.4998(6) 0.2460(5) 0.0743(2) 0.0352 1.0000 Uani . . . . . . . N48 N 0.6992(8) 0.0738(7) 0.1363(2) 0.0361 1.0000 Uani . . . . . . . C49 C 0.6978(12) -0.0306(10) 0.1505(3) 0.0548 1.0000 Uani . . . . . . . C50 C 0.6874(19) -0.1659(11) 0.1682(5) 0.1163 1.0000 Uani . . . . . . . N51 N 0.8599(7) 0.2148(6) 0.0483(2) 0.0270 1.0000 Uani . . . . . . . C52 C 0.9851(9) 0.2690(7) 0.0510(3) 0.0285 1.0000 Uani . . . . . . . C53 C 1.0069(8) 0.3455(7) 0.0872(2) 0.0251 1.0000 Uani . . . . . . . N54 N 0.8920(7) 0.3440(6) 0.1158(2) 0.0290 1.0000 Uani . . . . . . . C55 C 0.8937(9) 0.4110(8) 0.1499(3) 0.0321 1.0000 Uani . . . . . . . C56 C 0.7559(9) 0.4072(8) 0.1770(3) 0.0313 1.0000 Uani . . . . . . . N57 N 0.6433(7) 0.3528(6) 0.1645(2) 0.0268 1.0000 Uani . . . . . . . C58 C 0.5085(9) 0.3550(8) 0.1897(3) 0.0275 1.0000 Uani . . . . . . . C59 C 0.4082(10) 0.2573(8) 0.1882(3) 0.0349 1.0000 Uani . . . . . . . C60 C 0.2771(9) 0.2550(8) 0.2127(3) 0.0362 1.0000 Uani . . . . . . . C61 C 0.2415(10) 0.3490(8) 0.2389(3) 0.0380 1.0000 Uani . . . . . . . O62 O 0.1150(7) 0.3528(6) 0.2642(2) 0.0465 1.0000 Uani . . . . . . . C63 C 0.3403(9) 0.4473(8) 0.2398(3) 0.0346 1.0000 Uani . . . . . . . C64 C 0.4703(9) 0.4508(8) 0.2150(3) 0.0331 1.0000 Uani . . . . . . . C65 C 1.0172(10) 0.4828(10) 0.1579(3) 0.0454 1.0000 Uani . . . . . . . C66 C 1.1354(9) 0.4831(10) 0.1286(3) 0.0478 1.0000 Uani . . . . . . . C67 C 1.1324(10) 0.4138(9) 0.0927(3) 0.0425 1.0000 Uani . . . . . . . C68 C 0.8335(9) 0.1436(7) 0.0125(3) 0.0276 1.0000 Uani . . . . . . . C69 C 0.9058(9) 0.1614(8) -0.0288(3) 0.0315 1.0000 Uani . . . . . . . C70 C 0.8723(9) 0.0879(8) -0.0615(3) 0.0331 1.0000 Uani . . . . . . . C71 C 0.7659(9) -0.0049(7) -0.0531(3) 0.0284 1.0000 Uani . . . . . . . O72 O 0.7262(7) -0.0796(6) -0.0848(2) 0.0392 1.0000 Uani . . . . . . . C73 C 0.6946(9) -0.0253(8) -0.0117(3) 0.0318 1.0000 Uani . . . . . . . C74 C 0.7279(9) 0.0486(7) 0.0207(3) 0.0309 1.0000 Uani . . . . . . . S75 S 0.8210(2) 0.63352(18) 0.29474(6) 0.0299 1.0000 Uani . . . . . . . O76 O 0.8085(7) 0.5968(6) 0.25076(18) 0.0435 1.0000 Uani . . . . . . . O77 O 0.8905(7) 0.7524(5) 0.2974(3) 0.0566 1.0000 Uani . . . . . . . O78 O 0.8668(6) 0.5297(5) 0.32943(18) 0.0395 1.0000 Uani . . . . . . . C79 C 0.6271(9) 0.6650(8) 0.3098(3) 0.0399 1.0000 Uani . . . . . . . F80 F 0.5472(6) 0.5618(5) 0.3115(2) 0.0621 1.0000 Uani . . . . . . . F81 F 0.6157(7) 0.7055(6) 0.3489(2) 0.0765 1.0000 Uani . . . . . . . F82 F 0.5628(7) 0.7541(5) 0.2793(2) 0.0684 1.0000 Uani . . . . . . . H131 H 0.3134 0.4669 0.4558 0.0319 1.0000 Uiso R . . . . . . H141 H 0.3636 0.5898 0.5121 0.0315 1.0000 Uiso R . . . . . . H171 H 0.0753 0.3778 0.5949 0.0391 1.0000 Uiso R . . . . . . H181 H 0.0215 0.2578 0.5370 0.0332 1.0000 Uiso R . . . . . . H191 H -0.0660 0.2321 0.4720 0.0299 1.0000 Uiso R . . . . . . H231 H 0.0068 -0.0468 0.3211 0.0299 1.0000 Uiso R . . . . . . H241 H -0.2036 -0.0544 0.3701 0.0336 1.0000 Uiso R . . . . . . H251 H -0.2079 0.0707 0.4301 0.0296 1.0000 Uiso R . . . . . . H261 H 0.2682 0.0491 0.3005 0.0274 1.0000 Uiso R . . . . . . H291 H 0.4991 -0.0252 0.2950 0.0323 1.0000 Uiso R . . . . . . H301 H 0.7227 -0.0104 0.2554 0.0374 1.0000 Uiso R . . . . . . H331 H 0.7897 0.3414 0.2922 0.0391 1.0000 Uiso R . . . . . . H341 H 0.5625 0.3262 0.3335 0.0361 1.0000 Uiso R . . . . . . H371 H 0.1618 0.7063 0.3712 0.0502 1.0000 Uiso R . . . . . . H372 H 0.3060 0.7188 0.3424 0.0502 1.0000 Uiso R . . . . . . H373 H 0.1561 0.6901 0.3209 0.0502 1.0000 Uiso R . . . . . . H521 H 1.0649 0.2580 0.0300 0.0352 1.0000 Uiso R . . . . . . H561 H 0.7534 0.4450 0.2039 0.0364 1.0000 Uiso R . . . . . . H591 H 0.4279 0.1944 0.1690 0.0379 1.0000 Uiso R . . . . . . H601 H 0.2055 0.1907 0.2106 0.0398 1.0000 Uiso R . . . . . . H631 H 0.3165 0.5152 0.2576 0.0418 1.0000 Uiso R . . . . . . H641 H 0.5383 0.5164 0.2155 0.0411 1.0000 Uiso R . . . . . . H651 H 1.0182 0.5284 0.1823 0.0539 1.0000 Uiso R . . . . . . H661 H 1.2216 0.5232 0.1344 0.0529 1.0000 Uiso R . . . . . . H671 H 1.2171 0.4108 0.0734 0.0472 1.0000 Uiso R . . . . . . H691 H 0.9788 0.2255 -0.0343 0.0395 1.0000 Uiso R . . . . . . H701 H 0.9227 0.1005 -0.0893 0.0369 1.0000 Uiso R . . . . . . H731 H 0.6251 -0.0927 -0.0054 0.0428 1.0000 Uiso R . . . . . . H741 H 0.6779 0.0373 0.0487 0.0371 1.0000 Uiso R . . . . . . H502 H 0.7258 -0.1861 0.1971 0.1263 1.0000 Uiso R . . . . . . H503 H 0.7465 -0.2145 0.1483 0.1263 1.0000 Uiso R . . . . . . H504 H 0.5872 -0.1926 0.1669 0.1263 1.0000 Uiso R . . . . . . S100 S 0.1763(4) 0.9237(3) 0.20724(13) 0.0484(7) 0.5000 Uiso G . . . . . . O101 O 0.2555(6) 0.9042(5) 0.24959(15) 0.0481(7) 0.5000 Uiso G . . . . . . O102 O 0.2697(7) 0.9807(4) 0.17077(17) 0.0481(7) 0.5000 Uiso G . . . . . . O103 O 0.0575(6) 0.9723(5) 0.2367(2) 0.0481(7) 0.5000 Uiso G . . . . . . C104 C 0.1722(5) 0.7601(3) 0.19668(15) 0.0481(7) 0.5000 Uiso G . . . . . . F105 F 0.1196(8) 0.6841(4) 0.23034(19) 0.0481(7) 0.5000 Uiso G . . . . . . F106 F 0.2990(6) 0.7268(5) 0.1837(2) 0.0481(7) 0.5000 Uiso G . . . . . . F107 F 0.0676(7) 0.7594(5) 0.16054(19) 0.0481(7) 0.5000 Uiso G . . . . . . H505 H 0.2223 0.5385 0.6207 0.10(4) 1.0000 Uiso R . . . . . . H507 H 0.9382 0.1063 0.2398 0.04(2) 1.0000 Uiso R . . . . . . H506 H 0.0696 0.2826 0.2691 0.07(3) 1.0000 Uiso R . . . . . . H508 H 0.7790 -0.0642 -0.1109 0.13(4) 1.0000 Uiso R . . . . . . H509 H 0.5370 0.2165 0.4467 0.06(3) 1.0000 Uiso R . . . . . . H512 H 0.4363 0.1897 0.0745 0.08(3) 1.0000 Uiso R . . . . . . H511 H 0.4688 0.2844 0.0519 0.06(3) 1.0000 Uiso R . . . . . . H510 H 0.5705 0.3256 0.4197 0.07(3) 1.0000 Uiso R . . . . . . S200 S 0.0771(5) 0.9316(5) 0.18815(17) 0.0748(11) 0.5000 Uiso G . . . . . . O201 O 0.0162(7) 0.9666(8) 0.2291(2) 0.0748(11) 0.5000 Uiso G . . . . . . O202 O 0.1202(8) 1.0342(6) 0.1545(2) 0.0748(11) 0.5000 Uiso G . . . . . . O203 O -0.0018(7) 0.8306(7) 0.1710(3) 0.0748(11) 0.5000 Uiso G . . . . . . C204 C 0.2545(5) 0.8520(5) 0.20559(19) 0.0748(11) 0.5000 Uiso G . . . . . . F205 F 0.2355(8) 0.7486(6) 0.2355(3) 0.0748(11) 0.5000 Uiso G . . . . . . F206 F 0.3318(7) 0.8164(8) 0.1721(3) 0.0748(11) 0.5000 Uiso G . . . . . . F207 F 0.3403(6) 0.9285(7) 0.2255(3) 0.0748(11) 0.5000 Uiso G . . . . . . 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 0.0200(5) 0.0261(4) 0.0251(5) -0.0073(4) 0.0018(4) -0.0054(4) O2 0.025(3) 0.029(3) 0.029(3) 0.007(2) -0.007(2) -0.011(2) O3 0.030(3) 0.017(2) 0.034(3) 0.000(2) -0.005(2) -0.001(2) S4 0.0185(9) 0.0208(8) 0.0221(9) -0.0016(7) -0.0004(7) -0.0021(7) O5 0.033(3) 0.036(3) 0.044(3) 0.001(3) -0.016(3) -0.012(3) O6 0.035(3) 0.030(3) 0.013(2) 0.006(2) -0.001(2) 0.002(2) C7 0.050(6) 0.022(4) 0.026(4) 0.002(3) 0.009(4) 0.005(4) F8 0.024(3) 0.064(4) 0.092(5) -0.019(3) 0.006(3) 0.006(3) F9 0.076(4) 0.025(3) 0.046(3) -0.004(2) 0.014(3) 0.010(2) F10 0.100(5) 0.046(3) 0.034(3) 0.010(2) 0.034(3) 0.024(3) N11 0.020(3) 0.023(3) 0.017(3) -0.006(2) -0.001(2) -0.001(2) C12 0.020(4) 0.020(3) 0.023(4) -0.003(3) -0.003(3) -0.003(3) C13 0.029(4) 0.025(4) 0.019(3) -0.004(3) 0.006(3) -0.006(3) C14 0.036(4) 0.020(3) 0.027(4) -0.007(3) 0.003(3) -0.012(3) C15 0.024(4) 0.027(4) 0.021(3) -0.009(3) -0.001(3) -0.004(3) O16 0.040(3) 0.033(3) 0.025(3) -0.010(2) 0.005(2) -0.015(2) C17 0.030(4) 0.034(4) 0.032(4) -0.011(3) 0.005(3) -0.015(3) C18 0.028(4) 0.028(4) 0.025(4) -0.006(3) 0.007(3) -0.014(3) C19 0.018(4) 0.028(4) 0.022(4) -0.009(3) -0.003(3) 0.002(3) C20 0.018(4) 0.026(4) 0.027(4) -0.008(3) -0.002(3) 0.001(3) N21 0.016(3) 0.024(3) 0.018(3) -0.002(2) 0.003(2) 0.001(2) C22 0.017(3) 0.029(4) 0.015(3) -0.001(3) -0.003(3) -0.003(3) C23 0.027(4) 0.033(4) 0.019(3) -0.011(3) 0.004(3) -0.001(3) C24 0.027(4) 0.039(4) 0.033(4) -0.010(3) -0.003(3) -0.010(3) C25 0.018(4) 0.036(4) 0.024(4) -0.007(3) 0.005(3) -0.004(3) C26 0.025(4) 0.025(3) 0.019(3) -0.004(3) 0.000(3) 0.001(3) N27 0.022(3) 0.022(3) 0.024(3) -0.005(2) 0.003(3) 0.000(2) C28 0.023(4) 0.025(3) 0.012(3) -0.001(2) 0.002(2) -0.001(3) C29 0.027(4) 0.032(4) 0.030(4) -0.009(3) 0.001(3) -0.003(3) C30 0.028(4) 0.036(4) 0.035(4) -0.009(3) 0.005(3) -0.002(3) C31 0.025(4) 0.032(4) 0.028(4) 0.003(3) 0.013(3) -0.001(3) O32 0.033(3) 0.040(3) 0.052(4) -0.002(3) 0.026(3) -0.001(2) C33 0.027(4) 0.023(3) 0.039(4) -0.002(3) 0.001(3) -0.003(3) C34 0.022(4) 0.021(3) 0.032(4) -0.004(3) 0.006(3) -0.001(3) N35 0.035(4) 0.028(3) 0.033(4) -0.005(3) 0.006(3) -0.002(3) C36 0.030(4) 0.034(4) 0.028(4) -0.006(3) -0.005(3) -0.002(3) C37 0.035(4) 0.019(3) 0.075(6) 0.003(4) -0.003(4) -0.002(3) Zn38 0.0228(5) 0.0336(5) 0.0301(5) -0.0038(4) 0.0032(4) -0.0023(4) O39 0.037(3) 0.027(3) 0.035(3) -0.003(2) -0.002(3) -0.006(2) S40 0.0249(11) 0.0239(9) 0.0263(10) -0.0010(8) -0.0012(8) -0.0026(8) O41 0.037(4) 0.043(4) 0.055(4) -0.002(3) -0.015(3) -0.014(3) O42 0.033(3) 0.037(3) 0.035(3) -0.001(3) 0.006(3) 0.000(3) C43 0.045(6) 0.030(5) 0.059(7) 0.001(4) 0.016(5) 0.003(4) F44 0.082(4) 0.056(4) 0.044(3) 0.004(3) 0.031(3) 0.007(3) F45 0.080(4) 0.034(3) 0.069(4) 0.000(3) 0.029(3) 0.015(3) F46 0.031(3) 0.077(4) 0.089(5) -0.003(4) 0.007(3) 0.004(3) O47 0.026(3) 0.039(3) 0.039(4) 0.001(3) 0.001(3) -0.008(3) N48 0.038(4) 0.038(4) 0.030(4) 0.004(3) 0.002(3) 0.000(3) C49 0.066(7) 0.052(6) 0.044(5) 0.007(4) -0.008(5) -0.019(5) C50 0.179(16) 0.044(7) 0.113(12) 0.042(7) -0.051(11) -0.034(8) N51 0.020(4) 0.027(3) 0.034(4) -0.003(3) -0.001(3) 0.001(3) C52 0.027(5) 0.025(4) 0.033(4) -0.002(3) 0.012(4) 0.002(3) C53 0.019(4) 0.032(4) 0.022(4) 0.003(3) 0.005(3) 0.004(3) N54 0.022(4) 0.037(4) 0.026(4) 0.000(3) 0.001(3) 0.002(3) C55 0.017(4) 0.053(5) 0.025(4) -0.002(4) 0.004(3) 0.003(3) C56 0.027(4) 0.049(5) 0.018(4) -0.007(3) 0.006(3) 0.001(4) N57 0.018(3) 0.036(4) 0.024(3) 0.000(3) 0.002(3) 0.000(3) C58 0.021(4) 0.041(4) 0.022(4) -0.009(3) 0.002(3) 0.002(3) C59 0.039(5) 0.029(4) 0.037(5) -0.006(4) 0.012(4) -0.001(4) C60 0.030(4) 0.041(4) 0.038(5) -0.007(4) 0.011(4) -0.005(3) C61 0.032(4) 0.042(5) 0.038(5) -0.001(4) 0.007(4) 0.003(4) O62 0.035(3) 0.060(4) 0.046(4) -0.012(3) 0.023(3) -0.001(3) C63 0.030(4) 0.039(4) 0.037(4) -0.015(3) 0.013(3) -0.002(3) C64 0.026(4) 0.044(4) 0.031(4) -0.008(3) 0.007(3) -0.007(3) C65 0.027(4) 0.074(7) 0.039(5) -0.023(5) -0.007(4) -0.011(4) C66 0.017(4) 0.090(7) 0.042(5) -0.023(5) 0.005(4) -0.014(4) C67 0.023(5) 0.061(6) 0.045(6) -0.015(5) -0.001(4) -0.003(4) C68 0.024(4) 0.025(4) 0.034(4) -0.001(3) 0.005(3) 0.001(3) C69 0.029(4) 0.038(4) 0.029(4) -0.005(3) 0.003(3) -0.008(3) C70 0.031(4) 0.042(4) 0.025(4) 0.001(3) 0.006(3) -0.006(3) C71 0.029(4) 0.023(4) 0.033(4) -0.003(3) 0.004(3) -0.003(3) O72 0.041(3) 0.047(3) 0.030(3) -0.005(3) 0.004(3) -0.017(3) C73 0.028(4) 0.036(4) 0.031(4) -0.001(3) 0.012(3) -0.009(3) C74 0.026(4) 0.033(4) 0.035(4) -0.005(3) 0.005(3) -0.008(3) S75 0.0302(9) 0.0329(9) 0.0270(9) -0.0044(7) 0.0059(7) -0.0066(7) O76 0.053(4) 0.052(3) 0.026(3) -0.007(2) 0.006(2) -0.002(3) O77 0.045(4) 0.032(3) 0.097(5) -0.023(3) 0.011(3) -0.015(3) O78 0.042(3) 0.043(3) 0.034(3) -0.013(2) 0.000(2) 0.004(2) C79 0.044(5) 0.033(4) 0.045(5) -0.014(4) -0.001(4) 0.002(3) F80 0.043(3) 0.039(3) 0.106(5) -0.011(3) 0.012(3) -0.012(2) F81 0.076(4) 0.091(5) 0.072(4) -0.047(4) 0.030(3) 0.003(4) F82 0.059(4) 0.046(3) 0.094(5) 0.006(3) -0.008(3) 0.016(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 2.150(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 . O2 . 1.992(5) yes Zn1 . O3 . 2.347(5) yes Zn1 . N11 . 2.271(6) yes Zn1 . N21 . 2.024(6) yes Zn1 . N27 . 2.245(6) yes Zn1 . N35 . 2.117(7) yes O2 . H509 . 0.826 no O2 . H510 . 0.889 no O3 . S4 . 1.451(5) yes S4 . O5 . 1.437(5) yes S4 . O6 . 1.439(5) yes S4 . C7 . 1.824(8) yes C7 . F8 . 1.332(10) yes C7 . F9 . 1.325(8) yes C7 . F10 . 1.314(9) yes N11 . C12 . 1.425(8) yes N11 . C19 . 1.280(8) yes C12 . C13 . 1.388(9) yes C12 . C18 . 1.386(10) yes C13 . C14 . 1.381(9) yes C13 . H131 . 0.960 no C14 . C15 . 1.366(10) yes C14 . H141 . 0.976 no C15 . O16 . 1.384(8) yes C15 . C17 . 1.389(10) yes O16 . H505 . 0.958 no C17 . C18 . 1.382(10) yes C17 . H171 . 0.973 no C18 . H181 . 0.970 no C19 . C20 . 1.470(9) yes C19 . H191 . 0.954 no C20 . N21 . 1.328(9) yes C20 . C25 . 1.411(9) yes N21 . C22 . 1.334(8) yes C22 . C23 . 1.378(9) yes C22 . C26 . 1.462(10) yes C23 . C24 . 1.379(10) yes C23 . H231 . 0.974 no C24 . C25 . 1.377(10) yes C24 . H241 . 0.992 no C25 . H251 . 0.982 no C26 . N27 . 1.284(9) yes C26 . H261 . 0.957 no N27 . C28 . 1.425(9) yes C28 . C29 . 1.402(9) yes C28 . C34 . 1.393(9) yes C29 . C30 . 1.391(10) yes C29 . H291 . 0.962 no C30 . C31 . 1.380(10) yes C30 . H301 . 0.952 no C31 . O32 . 1.375(8) yes C31 . C33 . 1.388(10) yes O32 . H507 . 0.843 no C33 . C34 . 1.391(10) yes C33 . H331 . 0.983 no C34 . H341 . 0.987 no N35 . C36 . 1.126(9) yes C36 . C37 . 1.462(10) yes C37 . H371 . 0.937 no C37 . H372 . 0.973 no C37 . H373 . 0.949 no Zn38 . O39 . 2.319(5) yes Zn38 . O47 . 1.983(6) yes Zn38 . N48 . 2.141(7) yes Zn38 . N51 . 2.265(6) yes Zn38 . N54 . 2.027(6) yes Zn38 . N57 . 2.265(6) yes O39 . S40 . 1.454(5) yes S40 . O41 . 1.430(6) yes S40 . O42 . 1.444(6) yes S40 . C43 . 1.820(9) yes C43 . F44 . 1.322(11) yes C43 . F45 . 1.332(10) yes C43 . F46 . 1.325(11) yes O47 . H512 . 0.836 no O47 . H511 . 0.782 no N48 . C49 . 1.127(11) yes C49 . C50 . 1.462(14) yes C50 . H502 . 0.929 no C50 . H503 . 0.983 no C50 . H504 . 0.951 no N51 . C52 . 1.283(9) yes N51 . C68 . 1.426(10) yes C52 . C53 . 1.467(10) yes C52 . H521 . 0.965 no C53 . N54 . 1.335(9) yes C53 . C67 . 1.379(11) yes N54 . C55 . 1.328(10) yes C55 . C56 . 1.470(11) yes C55 . C65 . 1.403(11) yes C56 . N57 . 1.262(10) yes C56 . H561 . 0.953 no N57 . C58 . 1.420(9) yes C58 . C59 . 1.399(11) yes C58 . C64 . 1.385(10) yes C59 . C60 . 1.382(11) yes C59 . H591 . 0.952 no C60 . C61 . 1.383(11) yes C60 . H601 . 0.959 no C61 . O62 . 1.361(9) yes C61 . C63 . 1.392(11) yes O62 . H506 . 0.854 no C63 . C64 . 1.376(10) yes C63 . H631 . 0.974 no C64 . H641 . 0.941 no C65 . C66 . 1.373(12) yes C65 . H651 . 0.935 no C66 . C67 . 1.389(12) yes C66 . H661 . 0.922 no C67 . H671 . 0.953 no C68 . C69 . 1.388(11) yes C68 . C74 . 1.399(10) yes C69 . C70 . 1.381(11) yes C69 . H691 . 0.955 no C70 . C71 . 1.388(11) yes C70 . H701 . 0.942 no C71 . O72 . 1.379(9) yes C71 . C73 . 1.389(11) yes O72 . H508 . 0.911 no C73 . C74 . 1.374(11) yes C73 . H731 . 0.961 no C74 . H741 . 0.945 no S75 . O76 . 1.438(5) yes S75 . O77 . 1.437(5) yes S75 . O78 . 1.453(6) yes S75 . C79 . 1.819(8) yes C79 . F80 . 1.321(9) yes C79 . F81 . 1.309(9) yes C79 . F82 . 1.335(10) yes S100 . O101 . 1.44585(5) yes S100 . O102 . 1.45036(5) yes S100 . O103 . 1.50264(5) yes S100 . C104 . 1.80696(7) yes C104 . F105 . 1.298 yes C104 . F106 . 1.252 yes C104 . F107 . 1.43788(5) yes S200 . O201 . 1.436 yes S200 . O202 . 1.43724(6) yes S200 . O203 . 1.45735(5) yes S200 . C204 . 1.81219(7) yes C204 . F205 . 1.33035(5) yes C204 . F206 . 1.311 yes C204 . F207 . 1.338 yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O2 . Zn1 . O3 . 76.47(19) yes O2 . Zn1 . N11 . 103.7(2) yes O3 . Zn1 . N11 . 83.12(19) yes O2 . Zn1 . N21 . 160.6(2) yes O3 . Zn1 . N21 . 84.3(2) yes N11 . Zn1 . N21 . 75.9(2) yes O2 . Zn1 . N27 . 102.0(2) yes O3 . Zn1 . N27 . 93.0(2) yes N11 . Zn1 . N27 . 152.4(2) yes N21 . Zn1 . N27 . 76.5(2) yes O2 . Zn1 . N35 . 93.8(2) yes O3 . Zn1 . N35 . 166.3(2) yes N11 . Zn1 . N35 . 90.1(2) yes N21 . Zn1 . N35 . 105.6(2) yes N27 . Zn1 . N35 . 98.4(2) yes Zn1 . O2 . H509 . 120.6 no Zn1 . O2 . H510 . 134.7 no H509 . O2 . H510 . 104.5 no Zn1 . O3 . S4 . 144.0(3) yes O3 . S4 . O5 . 115.5(3) yes O3 . S4 . O6 . 114.3(3) yes O5 . S4 . O6 . 114.9(3) yes O3 . S4 . C7 . 102.7(3) yes O5 . S4 . C7 . 103.6(4) yes O6 . S4 . C7 . 103.6(3) yes S4 . C7 . F8 . 111.0(5) yes S4 . C7 . F9 . 111.3(6) yes F8 . C7 . F9 . 107.4(7) yes S4 . C7 . F10 . 110.6(6) yes F8 . C7 . F10 . 108.1(7) yes F9 . C7 . F10 . 108.2(6) yes Zn1 . N11 . C12 . 127.8(5) yes Zn1 . N11 . C19 . 111.0(4) yes C12 . N11 . C19 . 121.1(6) yes N11 . C12 . C13 . 118.1(6) yes N11 . C12 . C18 . 122.9(6) yes C13 . C12 . C18 . 118.9(6) yes C12 . C13 . C14 . 121.2(7) yes C12 . C13 . H131 . 119.7 no C14 . C13 . H131 . 119.2 no C13 . C14 . C15 . 119.6(6) yes C13 . C14 . H141 . 119.8 no C15 . C14 . H141 . 120.6 no C14 . C15 . O16 . 117.8(6) yes C14 . C15 . C17 . 120.0(6) yes O16 . C15 . C17 . 122.1(7) yes C15 . O16 . H505 . 115.8 no C15 . C17 . C18 . 120.4(7) yes C15 . C17 . H171 . 120.0 no C18 . C17 . H171 . 119.5 no C12 . C18 . C17 . 119.8(6) yes C12 . C18 . H181 . 119.3 no C17 . C18 . H181 . 120.9 no N11 . C19 . C20 . 118.2(6) yes N11 . C19 . H191 . 120.7 no C20 . C19 . H191 . 121.1 no C19 . C20 . N21 . 115.5(6) yes C19 . C20 . C25 . 124.0(7) yes N21 . C20 . C25 . 120.4(6) yes C20 . N21 . Zn1 . 119.0(5) yes C20 . N21 . C22 . 121.0(6) yes Zn1 . N21 . C22 . 119.1(5) yes N21 . C22 . C23 . 121.8(6) yes N21 . C22 . C26 . 113.9(6) yes C23 . C22 . C26 . 124.3(6) yes C22 . C23 . C24 . 118.0(6) yes C22 . C23 . H231 . 120.7 no C24 . C23 . H231 . 121.3 no C23 . C24 . C25 . 120.8(7) yes C23 . C24 . H241 . 119.9 no C25 . C24 . H241 . 119.2 no C20 . C25 . C24 . 118.0(7) yes C20 . C25 . H251 . 119.7 no C24 . C25 . H251 . 122.3 no C22 . C26 . N27 . 120.0(6) yes C22 . C26 . H261 . 120.9 no N27 . C26 . H261 . 119.2 no Zn1 . N27 . C26 . 110.3(5) yes Zn1 . N27 . C28 . 129.5(4) yes C26 . N27 . C28 . 120.2(6) yes N27 . C28 . C29 . 122.0(6) yes N27 . C28 . C34 . 118.4(6) yes C29 . C28 . C34 . 119.6(7) yes C28 . C29 . C30 . 119.7(7) yes C28 . C29 . H291 . 121.2 no C30 . C29 . H291 . 119.1 no C29 . C30 . C31 . 119.7(7) yes C29 . C30 . H301 . 119.0 no C31 . C30 . H301 . 121.3 no C30 . C31 . O32 . 121.6(7) yes C30 . C31 . C33 . 121.4(7) yes O32 . C31 . C33 . 116.8(7) yes C31 . O32 . H507 . 110.9 no C31 . C33 . C34 . 118.8(7) yes C31 . C33 . H331 . 121.3 no C34 . C33 . H331 . 119.8 no C28 . C34 . C33 . 120.6(7) yes C28 . C34 . H341 . 119.4 no C33 . C34 . H341 . 120.0 no Zn1 . N35 . C36 . 168.1(6) yes N35 . C36 . C37 . 177.6(8) yes C36 . C37 . H371 . 111.8 no C36 . C37 . H372 . 108.9 no H371 . C37 . H372 . 108.2 no C36 . C37 . H373 . 110.2 no H371 . C37 . H373 . 110.3 no H372 . C37 . H373 . 107.3 no O39 . Zn38 . O47 . 75.1(2) yes O39 . Zn38 . N48 . 166.3(2) yes O47 . Zn38 . N48 . 92.0(3) yes O39 . Zn38 . N51 . 85.5(2) yes O47 . Zn38 . N51 . 102.8(2) yes N48 . Zn38 . N51 . 93.4(2) yes O39 . Zn38 . N54 . 84.9(2) yes O47 . Zn38 . N54 . 160.0(3) yes N48 . Zn38 . N54 . 108.0(3) yes N51 . Zn38 . N54 . 75.3(2) yes O39 . Zn38 . N57 . 93.9(2) yes O47 . Zn38 . N57 . 104.4(2) yes N48 . Zn38 . N57 . 93.5(2) yes N51 . Zn38 . N57 . 151.7(2) yes N54 . Zn38 . N57 . 76.4(2) yes Zn38 . O39 . S40 . 145.5(3) yes O39 . S40 . O41 . 115.3(4) yes O39 . S40 . O42 . 113.9(3) yes O41 . S40 . O42 . 115.4(4) yes O39 . S40 . C43 . 102.3(4) yes O41 . S40 . C43 . 104.6(4) yes O42 . S40 . C43 . 103.1(4) yes S40 . C43 . F44 . 111.4(7) yes S40 . C43 . F45 . 110.8(6) yes F44 . C43 . F45 . 107.2(8) yes S40 . C43 . F46 . 111.3(7) yes F44 . C43 . F46 . 108.2(8) yes F45 . C43 . F46 . 107.7(8) yes Zn38 . O47 . H512 . 138.0 no Zn38 . O47 . H511 . 126.2 no H512 . O47 . H511 . 92.8 no Zn38 . N48 . C49 . 173.2(8) yes N48 . C49 . C50 . 176.9(12) yes C49 . C50 . H502 . 112.8 no C49 . C50 . H503 . 107.4 no H502 . C50 . H503 . 108.1 no C49 . C50 . H504 . 111.0 no H502 . C50 . H504 . 110.9 no H503 . C50 . H504 . 106.3 no Zn38 . N51 . C52 . 111.1(5) yes Zn38 . N51 . C68 . 128.4(5) yes C52 . N51 . C68 . 120.3(7) yes N51 . C52 . C53 . 119.0(7) yes N51 . C52 . H521 . 120.8 no C53 . C52 . H521 . 120.2 no C52 . C53 . N54 . 113.8(7) yes C52 . C53 . C67 . 125.0(7) yes N54 . C53 . C67 . 121.3(7) yes C53 . N54 . Zn38 . 120.0(5) yes C53 . N54 . C55 . 120.9(7) yes Zn38 . N54 . C55 . 118.3(5) yes N54 . C55 . C56 . 115.0(7) yes N54 . C55 . C65 . 121.4(7) yes C56 . C55 . C65 . 123.5(7) yes C55 . C56 . N57 . 119.6(7) yes C55 . C56 . H561 . 119.5 no N57 . C56 . H561 . 120.9 no Zn38 . N57 . C56 . 110.3(5) yes Zn38 . N57 . C58 . 130.5(5) yes C56 . N57 . C58 . 119.2(6) yes N57 . C58 . C59 . 118.6(7) yes N57 . C58 . C64 . 123.0(7) yes C59 . C58 . C64 . 118.4(7) yes C58 . C59 . C60 . 120.2(7) yes C58 . C59 . H591 . 119.9 no C60 . C59 . H591 . 119.8 no C59 . C60 . C61 . 121.1(8) yes C59 . C60 . H601 . 120.6 no C61 . C60 . H601 . 118.2 no C60 . C61 . O62 . 124.5(8) yes C60 . C61 . C63 . 118.5(8) yes O62 . C61 . C63 . 117.0(7) yes C61 . O62 . H506 . 114.8 no C61 . C63 . C64 . 120.6(7) yes C61 . C63 . H631 . 119.8 no C64 . C63 . H631 . 119.6 no C58 . C64 . C63 . 121.1(7) yes C58 . C64 . H641 . 117.6 no C63 . C64 . H641 . 121.3 no C55 . C65 . C66 . 117.3(8) yes C55 . C65 . H651 . 120.9 no C66 . C65 . H651 . 121.8 no C65 . C66 . C67 . 120.9(8) yes C65 . C66 . H661 . 119.3 no C67 . C66 . H661 . 119.5 no C66 . C67 . C53 . 118.1(8) yes C66 . C67 . H671 . 120.4 no C53 . C67 . H671 . 121.4 no N51 . C68 . C69 . 124.7(7) yes N51 . C68 . C74 . 116.2(7) yes C69 . C68 . C74 . 119.1(7) yes C68 . C69 . C70 . 120.5(7) yes C68 . C69 . H691 . 119.1 no C70 . C69 . H691 . 120.4 no C69 . C70 . C71 . 119.8(8) yes C69 . C70 . H701 . 119.6 no C71 . C70 . H701 . 120.6 no C70 . C71 . O72 . 122.2(7) yes C70 . C71 . C73 . 120.4(7) yes O72 . C71 . C73 . 117.4(7) yes C71 . O72 . H508 . 113.6 no C71 . C73 . C74 . 119.6(7) yes C71 . C73 . H731 . 120.1 no C74 . C73 . H731 . 120.2 no C68 . C74 . C73 . 120.6(8) yes C68 . C74 . H741 . 119.0 no C73 . C74 . H741 . 120.3 no O76 . S75 . O77 . 116.6(4) yes O76 . S75 . O78 . 114.1(3) yes O77 . S75 . O78 . 114.8(4) yes O76 . S75 . C79 . 103.1(4) yes O77 . S75 . C79 . 103.4(4) yes O78 . S75 . C79 . 102.2(4) yes S75 . C79 . F80 . 111.6(5) yes S75 . C79 . F81 . 112.1(6) yes F80 . C79 . F81 . 107.8(7) yes S75 . C79 . F82 . 110.5(6) yes F80 . C79 . F82 . 107.0(7) yes F81 . C79 . F82 . 107.6(7) yes O101 . S100 . O102 . 111.815(3) yes O101 . S100 . O103 . 80.488(4) yes O102 . S100 . O103 . 135.349 yes O101 . S100 . C104 . 99.367(4) yes O102 . S100 . C104 . 101.841(4) yes O103 . S100 . C104 . 118.845(3) yes S100 . C104 . F105 . 112.763(3) yes S100 . C104 . F106 . 108.933(3) yes F105 . C104 . F106 . 114.368(3) yes S100 . C104 . F107 . 106.140(4) yes F105 . C104 . F107 . 105.807(4) yes F106 . C104 . F107 . 108.376(3) yes O201 . S200 . O202 . 116.743(3) yes O201 . S200 . C204 . 103.361(3) yes O202 . S200 . O203 . 114.782(3) yes O202 . S200 . C204 . 103.065(4) yes O203 . S200 . C204 . 102.009(4) yes S200 . C204 . F205 . 111.553(3) yes S200 . C204 . F206 . 112.978(3) yes S200 . C204 . F207 . 110.908(3) yes F205 . C204 . F206 . 107.499(4) yes F205 . C204 . F207 . 106.256(4) yes F206 . C204 . F207 . 107.307(3) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C18 . H181 . O5 2_556 163 0.97 2.53 3.465(11) yes C23 . H231 . O77 1_445 140 0.97 2.59 3.397(11) yes C23 . H231 . O103 1_545 141 0.97 2.56 3.368(11) yes C25 . H251 . O6 2_556 152 0.98 2.42 3.318(11) yes C26 . H261 . O101 1_545 163 0.96 2.32 3.250(11) yes C33 . H331 . O78 . 149 0.98 2.54 3.418(11) yes C37 . H373 . O77 1_455 138 0.95 2.52 3.287(11) yes C56 . H561 . O76 . 156 0.95 2.35 3.246(11) yes C67 . H671 . O42 2_765 150 0.95 2.55 3.407(11) yes C70 . H701 . O203 2_665 166 0.94 2.57 3.487(11) yes O16 . H505 . O78 2_666 170 0.96 1.77 2.716(11) yes O32 . H507 . O103 1_645 157 0.84 1.76 2.553(11) yes O32 . H507 . O201 1_645 171 0.84 1.68 2.520(11) yes O62 . H506 . O32 1_455 146 0.85 2.01 2.759(11) yes O72 . H508 . O102 2_665 134 0.91 1.93 2.648(11) yes O72 . H508 . O202 2_665 176 0.91 1.59 2.497(11) yes O2 . H509 . O6 2_656 162 0.83 1.94 2.732(11) yes O47 . H512 . O72 2_655 168 0.84 1.89 2.715(11) yes O47 . H511 . O42 2_665 162 0.78 2.00 2.759(11) yes O2 . H510 . O16 2_666 173 0.89 1.93 2.813(11) yes #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 715277' _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; Inversion twin; flack parameter at exactly 0.5. All atoms, except hydrogen refined anisotropically The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _cell_length_a 15.8406(5) _cell_length_b 16.1462(4) _cell_length_c 40.5039(14) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 10359.5(5) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'F d d 2 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z x,y+1/2,z+1/2 x+1/2,y,z+1/2 x+1/2,y+1/2,z -x+1/4,y+1/4,z+1/4 -x+1/4,y+3/4,z+3/4 -x+3/4,y+1/4,z+3/4 -x+3/4,y+3/4,z+1/4 x+1/4,-y+1/4,z+1/4 x+1/4,-y+3/4,z+3/4 x+3/4,-y+1/4,z+3/4 x+3/4,-y+3/4,z+1/4 -x+1/2,-y,z+1/2 -x+1/2,-y+1/2,z+1 -x+1,-y,z+1 -x+1,-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' 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' 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' 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' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Pb -3.3944 10.1111 31.0617 0.6902 13.0637 2.3576 18.4420 8.6180 5.9696 47.2579 13.4118 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 16 # Given Formula = C6 H5 F0.01 N0.01 O1 Pb0.01 S0.50 # Dc = 0.68 Fooo = 6312.00 Mu = 3.39 M = 266.71 # Found Formula = C8.84 H6.53 F2.53 N1.26 O3.37 Pb0.42 S0.84 # Dc = 2.11 FOOO = 6312.00 Mu = 67.71 M = 823.19 _chemical_formula_sum 'C21 H15 F6 N3 O8 Pb S2' _chemical_formula_moiety 'C21 H15 F6 N3 O8 Pb S2' _chemical_compound_source ? _chemical_formula_weight 822.70 _cell_measurement_reflns_used 13820 _cell_measurement_theta_min 3.7328 _cell_measurement_theta_max 29.0416 _cell_measurement_temperature 173 _exptl_crystal_description prism _exptl_crystal_colour orange-red _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.25 _exptl_crystal_density_diffrn 2.111 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 6304.0 _exptl_absorpt_coefficient_mu 6.771 # Sheldrick geometric approximatio 0.26 0.51 # No experimental values of Tmin/max available _exptl_absorpt_correction_T_min 0.53179 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_detector_area_resol_mean 16.0143 _diffrn_measurement_device 'Oxford Diffraction XCALIBUR' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _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_orient_matrix_UB_11 0.0175822520 _diffrn_orient_matrix_UB_12 0.0141244469 _diffrn_orient_matrix_UB_13 -0.0150796924 _diffrn_orient_matrix_UB_21 0.0124856226 _diffrn_orient_matrix_UB_22 -0.0410235507 _diffrn_orient_matrix_UB_23 -0.0038768805 _diffrn_orient_matrix_UB_31 -0.0391939368 _diffrn_orient_matrix_UB_32 -0.0067307707 _diffrn_orient_matrix_UB_33 -0.0079937735 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -12.00 40.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 17.8630 77.0000 90.0000 0.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 2 omega -52.00 0.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 17.8630 -77.0000 270.0000 0.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 3 omega -53.00 -4.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 17.8630 -45.0000 330.0000 0.0000 0.0000 49 #__ type_ start__ end____ width___ exp.time_ 4 omega -53.00 -4.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 17.8630 -45.0000 210.0000 0.0000 0.0000 49 #__ type_ start__ end____ width___ exp.time_ 5 omega -53.00 -4.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 17.8630 -45.0000 120.0000 0.0000 0.0000 49 #__ type_ start__ end____ width___ exp.time_ 6 omega -12.00 40.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 17.8630 77.0000 180.0000 0.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 7 omega 40.00 89.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 17.8630 45.0000 60.0000 0.0000 0.0000 49 #__ type_ start__ end____ width___ exp.time_ 8 omega 40.00 89.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 17.8630 45.0000 210.0000 0.0000 0.0000 49 ; _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 173 _diffrn_reflns_number 20575 _reflns_number_total 5996 _diffrn_reflns_av_R_equivalents 0.026 # Number of reflections with Friedels Law is 3247 # Number of reflections without Friedels Law is 5996 # Theoretical number of reflections is about 3482 _diffrn_reflns_theta_min 3.742 _diffrn_reflns_theta_max 29.120 _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 25.917 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_limit_l_max 54 _reflns_limit_h_min 0 _reflns_limit_h_max 21 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min -53 _reflns_limit_l_max 54 _oxford_diffrn_Wilson_B_factor 1.39 _oxford_diffrn_Wilson_scale 0.85 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.32 _refine_diff_density_max 1.51 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 5996 _refine_ls_number_restraints 452 _refine_ls_number_parameters 378 _oxford_refine_ls_R_factor_ref 0.0386 _refine_ls_wR_factor_ref 0.0393 _refine_ls_goodness_of_fit_ref 0.8163 _refine_ls_shift/su_max 0.001483 # The values computed from all data _oxford_reflns_number_all 5996 _refine_ls_R_factor_all 0.0386 _refine_ls_wR_factor_all 0.0393 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4703 _refine_ls_R_factor_gt 0.0213 _refine_ls_wR_factor_gt 0.0367 _refine_ls_abs_structure_Flack 0.502(4) _refine_ls_abs_structure_details 'Flack (1983), 2749 Friedel-pairs' # 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 ad _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Flack, H. D. (1983). Acta Cryst. A39, 876-881. North, A.C.T., Phillips, D.C. & Mathews, F.S., (1968). Acta Cryst, A24, 351-359. Oxford Diffraction, (2002). CrysAlis RED. Oxford Diffraction, (2002). Xcalibur User Manual. 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Pb1 Pb 0.7500 0.7500 0.58886(3) 0.0204 1.0000 Uani S TU . . . . . O2 O 0.6640(2) 0.8737(2) 0.57481(8) 0.0455 1.0000 Uani . U . . . . . S3 S 0.68112(9) 0.94732(8) 0.59382(4) 0.0348 1.0000 Uani . U . . . . . O4 O 0.6537(4) 1.0212(2) 0.57961(11) 0.0925 1.0000 Uani . U . . . . . O5 O 0.7641(2) 0.9438(4) 0.60787(13) 0.0612 1.0000 Uani . U . . . . . C6 C 0.6155(4) 0.9336(4) 0.62996(17) 0.0554 1.0000 Uani . U . . . . . F7 F 0.6194(2) 1.0007(3) 0.64861(9) 0.0803 1.0000 Uani . U . . . . . F8 F 0.5369(2) 0.9202(3) 0.62143(15) 0.1209 1.0000 Uani . U . . . . . F9 F 0.6407(3) 0.8688(3) 0.64664(11) 0.1115 1.0000 Uani . U . . . . . N10 N 0.7500 0.7500 0.5301(2) 0.0208 1.0000 Uani S TU . . . . . C11 C 0.8176(3) 0.7792(3) 0.51363(10) 0.0247 1.0000 Uani . U . . . . . C12 C 0.8876(4) 0.8104(4) 0.53267(13) 0.0241 1.0000 Uani . U . . . . . N13 N 0.8868(3) 0.8105(3) 0.56409(11) 0.0245 1.0000 Uani . U . . . . . C14 C 0.9543(3) 0.8442(3) 0.58320(11) 0.0231 1.0000 Uani . U . . . . . C15 C 1.0179(3) 0.8913(3) 0.56937(11) 0.0361 1.0000 Uani . U . . . . . C16 C 1.0807(3) 0.9236(3) 0.58870(11) 0.0333 1.0000 Uani . U . . . . . C17 C 1.0785(3) 0.9119(3) 0.62218(12) 0.0281 1.0000 Uani . U . . . . . O18 O 1.1390(2) 0.9441(2) 0.64293(9) 0.0414 1.0000 Uani . U . . . . . C19 C 1.0176(3) 0.8636(4) 0.63653(12) 0.0425 1.0000 Uani . U . . . . . C20 C 0.9547(3) 0.8310(3) 0.61624(11) 0.0400 1.0000 Uani . U . . . . . C21 C 0.8188(3) 0.7790(4) 0.47976(11) 0.0362 1.0000 Uani . U . . . . . C22 C 0.750000(7) 0.750000(7) 0.4607(3) 0.0399 1.0000 Uani S TU . . . . . Pb101 Pb 0.7500 0.2500 0.50042(3) 0.0235 1.0000 Uani S TU . . . . . O102 O 0.6685(2) 0.37728(19) 0.51431(8) 0.0364 1.0000 Uani . U . . . . . S103 S 0.67482(8) 0.44718(7) 0.49156(4) 0.0329 1.0000 Uani . U . . . . . O105 O 0.7532(2) 0.4461(4) 0.47352(12) 0.0469 1.0000 Uani . U . . . . . O104 O 0.6460(3) 0.5244(2) 0.50462(10) 0.0549 1.0000 Uani . U . . . . . C106 C 0.5974(3) 0.4190(4) 0.45972(13) 0.0339 1.0000 Uani . U . . . . . F107 F 0.59361(19) 0.47697(18) 0.43685(7) 0.0484 1.0000 Uani . U . . . . . F109 F 0.61993(18) 0.34909(18) 0.44513(8) 0.0492 1.0000 Uani . U . . . . . F108 F 0.52123(17) 0.4098(2) 0.47269(8) 0.0555 1.0000 Uani . U . . . . . N113 N 0.8844(3) 0.3144(3) 0.52473(11) 0.0248 1.0000 Uani . U . . . . . C112 C 0.8869(4) 0.3129(4) 0.55621(14) 0.0285 1.0000 Uani . U . . . . . C111 C 0.8167(3) 0.2807(3) 0.57548(10) 0.0283 1.0000 Uani . U . . . . . N110 N 0.7500 0.2500 0.5586(2) 0.0284 1.0000 Uani S TU . . . . . C121 C 0.8171(4) 0.2818(3) 0.61022(11) 0.0377 1.0000 Uani . U . . . . . C122 C 0.750000(7) 0.250000(7) 0.6256(3) 0.0423 1.0000 Uani S TU . . . . . C114 C 0.9515(3) 0.3471(3) 0.50594(11) 0.0243 1.0000 Uani . U . . . . . C115 C 1.0202(3) 0.3911(3) 0.51885(11) 0.0354 1.0000 Uani . U . . . . . C116 C 1.0824(3) 0.4216(3) 0.49887(12) 0.0388 1.0000 Uani . U . . . . . C117 C 1.0799(3) 0.4098(3) 0.46458(13) 0.0304 1.0000 Uani . U . . . . . O118 O 1.1372(2) 0.4405(2) 0.44399(9) 0.0439 1.0000 Uani . U . . . . . C119 C 1.0109(3) 0.3675(3) 0.45161(11) 0.0349 1.0000 Uani . U . . . . . C120 C 0.9484(3) 0.3370(3) 0.47186(11) 0.0306 1.0000 Uani . U . . . . . H121 H 0.9347 0.8303 0.5214 0.0288 1.0000 Uiso R . . . . . . H151 H 1.0184 0.9009 0.5468 0.0412 1.0000 Uiso R . . . . . . H161 H 1.1243 0.9538 0.5792 0.0428 1.0000 Uiso R . . . . . . H191 H 1.0181 0.8532 0.6592 0.0519 1.0000 Uiso R . . . . . . H201 H 0.9120 0.7994 0.6258 0.0490 1.0000 Uiso R . . . . . . H211 H 0.8659 0.7982 0.4685 0.0449 1.0000 Uiso R . . . . . . H221 H 0.7500 0.7500 0.4369 0.0532 1.0000 Uiso RS . . . . . . H1121 H 0.9340 0.3327 0.5672 0.0370 1.0000 Uiso R . . . . . . H1211 H 0.8629 0.3036 0.6216 0.0457 1.0000 Uiso R . . . . . . H1221 H 0.7500 0.2500 0.6484 0.0512 1.0000 Uiso RS . . . . . . H1151 H 1.0229 0.4000 0.5415 0.0469 1.0000 Uiso R . . . . . . H1161 H 1.1276 0.4506 0.5081 0.0479 1.0000 Uiso R . . . . . . H1191 H 1.0073 0.3599 0.4289 0.0440 1.0000 Uiso R . . . . . . H1201 H 0.9025 0.3090 0.4627 0.0381 1.0000 Uiso R . . . . . . H1181 H 1.1726 0.4638 0.4552 0.0709 1.0000 Uiso R . . . . . . H181 H 1.1664 0.9824 0.6354 0.0610 1.0000 Uiso 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 Pb1 0.0225(2) 0.0215(3) 0.0171(2) 0.0000 0.0000 0.00070(13) O2 0.065(2) 0.0283(14) 0.043(2) -0.0136(13) -0.0220(16) 0.0215(14) S3 0.0512(7) 0.0228(6) 0.0304(6) -0.0023(5) 0.0026(5) 0.0024(6) O4 0.197(5) 0.026(2) 0.054(3) 0.0033(16) -0.002(3) 0.035(3) O5 0.0344(17) 0.070(4) 0.079(4) -0.026(3) 0.0089(17) -0.016(2) C6 0.046(2) 0.055(3) 0.065(3) -0.0131(17) 0.026(2) 0.009(3) F7 0.088(2) 0.087(2) 0.066(2) -0.037(2) 0.0249(18) 0.012(2) F8 0.042(2) 0.113(4) 0.207(5) -0.065(3) 0.035(2) -0.014(2) F9 0.167(4) 0.089(3) 0.079(3) 0.037(2) 0.064(3) 0.024(3) N10 0.030(3) 0.014(4) 0.0191(15) 0.0000 0.0000 -0.0042(19) C11 0.035(2) 0.018(2) 0.0207(15) 0.0018(17) 0.0029(14) -0.0047(19) C12 0.027(2) 0.021(3) 0.0247(19) 0.0025(17) 0.0060(15) -0.003(2) N13 0.0280(15) 0.023(2) 0.0224(18) 0.0001(16) 0.0010(13) -0.0053(15) C14 0.0212(19) 0.022(2) 0.0257(16) 0.0015(16) 0.0000(14) 0.0005(16) C15 0.037(3) 0.049(3) 0.022(2) 0.0052(18) 0.0011(16) -0.016(2) C16 0.032(2) 0.039(3) 0.0288(18) 0.0082(19) -0.0002(17) -0.013(2) C17 0.026(2) 0.031(3) 0.0266(18) 0.0018(18) -0.0056(16) -0.0005(19) O18 0.0326(18) 0.058(3) 0.0338(19) 0.0070(17) -0.0094(15) -0.0126(18) C19 0.040(3) 0.064(4) 0.023(2) 0.016(2) -0.0096(18) -0.017(3) C20 0.034(3) 0.059(4) 0.0266(18) 0.006(2) 0.0014(17) -0.021(2) C21 0.038(3) 0.049(3) 0.0215(16) 0.002(2) 0.0074(17) -0.013(3) C22 0.051(5) 0.046(8) 0.022(4) 0.0000 0.0000 -0.013(4) Pb101 0.0290(2) 0.0231(3) 0.0184(2) 0.0000 0.0000 0.00484(13) O102 0.0500(18) 0.0259(14) 0.0333(17) 0.0050(11) 0.0130(14) 0.0124(13) S103 0.0406(7) 0.0227(6) 0.0354(6) 0.0024(5) 0.0077(5) 0.0041(6) O105 0.0344(18) 0.053(3) 0.054(2) 0.0096(19) 0.0097(14) -0.0067(18) O104 0.078(3) 0.0262(19) 0.061(2) -0.0074(14) -0.002(2) 0.0138(18) C106 0.032(2) 0.034(2) 0.036(2) 0.0092(13) 0.0104(14) 0.004(2) F107 0.0547(18) 0.049(2) 0.0419(16) 0.0181(12) 0.0073(13) 0.0159(15) F109 0.0558(17) 0.0405(16) 0.0513(17) -0.0072(13) -0.0054(14) 0.0042(14) F108 0.0288(15) 0.072(2) 0.065(2) 0.0248(17) 0.0123(13) 0.0039(15) N113 0.0338(15) 0.016(2) 0.0242(18) -0.0009(16) -0.0037(13) 0.0049(14) C112 0.036(2) 0.024(3) 0.0254(19) -0.0049(18) -0.0052(16) 0.001(2) C111 0.044(2) 0.021(3) 0.0200(15) 0.0000(18) -0.0025(14) 0.005(2) N110 0.040(3) 0.024(5) 0.0212(16) 0.0000 0.0000 0.000(2) C121 0.072(4) 0.020(3) 0.0210(16) -0.0033(19) -0.005(2) 0.005(3) C122 0.080(6) 0.039(7) 0.008(4) 0.0000 0.0000 0.006(4) C114 0.0283(19) 0.017(2) 0.0274(16) -0.0014(16) -0.0061(14) 0.0066(16) C115 0.035(3) 0.047(3) 0.025(2) -0.0081(18) -0.0077(15) -0.004(2) C116 0.029(2) 0.053(3) 0.0343(19) -0.009(2) -0.0113(17) -0.012(2) C117 0.026(2) 0.030(3) 0.0353(18) -0.0053(19) -0.0025(17) 0.001(2) O118 0.049(2) 0.047(2) 0.036(2) -0.0017(17) -0.0029(16) -0.024(2) C119 0.040(3) 0.039(3) 0.0264(19) -0.0009(18) -0.0066(18) -0.010(2) C120 0.033(2) 0.031(3) 0.0286(17) -0.0029(18) -0.0095(16) -0.008(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.33612(12) 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 Pb1 . O2 14_664 2.484(3) yes Pb1 . N13 14_664 2.580(4) yes Pb1 . O2 . 2.484(3) yes Pb1 . N10 . 2.381(9) yes Pb1 . N13 . 2.580(4) yes O2 . S3 . 1.442(3) yes S3 . O4 . 1.394(4) yes S3 . O5 . 1.433(4) yes S3 . C6 . 1.809(6) yes C6 . F7 . 1.321(8) yes C6 . F8 . 1.310(7) yes C6 . F9 . 1.309(8) yes N10 . C11 14_664 1.346(6) yes N10 . C11 . 1.346(6) yes C11 . C12 . 1.442(7) yes C11 . C21 . 1.372(6) yes C12 . N13 . 1.273(5) yes C12 . H121 . 0.932 no N13 . C14 . 1.428(6) yes C14 . C15 . 1.381(6) yes C14 . C20 . 1.355(6) yes C15 . C16 . 1.368(6) yes C15 . H151 . 0.928 no C16 . C17 . 1.370(6) yes C16 . H161 . 0.929 no C17 . O18 . 1.377(5) yes C17 . C19 . 1.369(7) yes O18 . H181 . 0.813 no C19 . C20 . 1.395(6) yes C19 . H191 . 0.932 no C20 . H201 . 0.931 no C21 . C22 . 1.416(8) yes C21 . H211 . 0.928 no C22 . H221 . 0.964 no Pb101 . O102 14_654 2.491(3) yes Pb101 . N113 14_654 2.566(4) yes Pb101 . O102 . 2.491(3) yes Pb101 . N113 . 2.566(4) yes Pb101 . N110 . 2.357(10) yes O102 . S103 . 1.461(3) yes S103 . O105 . 1.440(4) yes S103 . O104 . 1.429(4) yes S103 . C106 . 1.837(6) yes C106 . F107 . 1.318(6) yes C106 . F109 . 1.323(6) yes C106 . F108 . 1.324(5) yes N113 . C112 . 1.276(5) yes N113 . C114 . 1.410(6) yes C112 . C111 . 1.454(7) yes C112 . H1121 . 0.926 no C111 . N110 . 1.353(7) yes C111 . C121 . 1.407(6) yes C121 . C122 . 1.334(7) yes C121 . H1211 . 0.929 no C122 . H1221 . 0.924 no C114 . C115 . 1.401(6) yes C114 . C120 . 1.391(6) yes C115 . C116 . 1.366(7) yes C115 . H1151 . 0.928 no C116 . C117 . 1.402(7) yes C116 . H1161 . 0.934 no C117 . O118 . 1.328(6) yes C117 . C119 . 1.392(7) yes O118 . H1181 . 0.814 no C119 . C120 . 1.377(7) yes C119 . H1191 . 0.931 no C120 . H1201 . 0.933 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 O2 14_664 Pb1 . N13 14_664 93.85(14) yes O2 14_664 Pb1 . O2 . 153.50(15) yes N13 14_664 Pb1 . O2 . 75.80(14) yes O2 14_664 Pb1 . N10 . 76.75(8) yes N13 14_664 Pb1 . N10 . 67.12(10) yes O2 . Pb1 . N10 . 76.75(8) yes O2 14_664 Pb1 . N13 . 75.80(14) yes N13 14_664 Pb1 . N13 . 134.2(2) yes O2 . Pb1 . N13 . 93.85(14) yes N10 . Pb1 . N13 . 67.12(10) yes Pb1 . O2 . S3 . 115.90(18) yes O2 . S3 . O4 . 115.2(2) yes O2 . S3 . O5 . 110.6(3) yes O4 . S3 . O5 . 118.9(4) yes O2 . S3 . C6 . 102.9(3) yes O4 . S3 . C6 . 105.1(3) yes O5 . S3 . C6 . 101.6(3) yes S3 . C6 . F7 . 109.6(4) yes S3 . C6 . F8 . 110.6(5) yes F7 . C6 . F8 . 109.3(5) yes S3 . C6 . F9 . 109.9(4) yes F7 . C6 . F9 . 110.3(6) yes F8 . C6 . F9 . 107.1(7) yes Pb1 . N10 . C11 14_664 119.7(4) yes Pb1 . N10 . C11 . 119.7(4) yes C11 14_664 N10 . C11 . 120.7(8) yes N10 . C11 . C12 . 118.0(5) yes N10 . C11 . C21 . 120.3(5) yes C12 . C11 . C21 . 121.7(4) yes C11 . C12 . N13 . 121.9(5) yes C11 . C12 . H121 . 118.3 no N13 . C12 . H121 . 119.8 no Pb1 . N13 . C12 . 113.4(4) yes Pb1 . N13 . C14 . 124.2(3) yes C12 . N13 . C14 . 122.4(5) yes N13 . C14 . C15 . 122.4(4) yes N13 . C14 . C20 . 118.6(4) yes C15 . C14 . C20 . 118.9(4) yes C14 . C15 . C16 . 120.5(4) yes C14 . C15 . H151 . 119.8 no C16 . C15 . H151 . 119.7 no C15 . C16 . C17 . 119.7(4) yes C15 . C16 . H161 . 120.3 no C17 . C16 . H161 . 120.0 no C16 . C17 . O18 . 122.3(5) yes C16 . C17 . C19 . 121.1(5) yes O18 . C17 . C19 . 116.5(4) yes C17 . O18 . H181 . 115.5 no C17 . C19 . C20 . 117.9(4) yes C17 . C19 . H191 . 121.0 no C20 . C19 . H191 . 121.1 no C19 . C20 . C14 . 121.7(4) yes C19 . C20 . H201 . 118.8 no C14 . C20 . H201 . 119.5 no C11 . C21 . C22 . 122.4(6) yes C11 . C21 . H211 . 120.1 no C22 . C21 . H211 . 117.5 no C21 14_664 C22 . C21 . 113.8(9) yes C21 14_664 C22 . H221 . 123.1 no C21 . C22 . H221 . 123.1 no O102 14_654 Pb101 . N113 14_654 90.52(13) yes O102 14_654 Pb101 . O102 . 153.89(14) yes N113 14_654 Pb101 . O102 . 79.49(13) yes O102 14_654 Pb101 . N113 . 79.49(13) yes N113 14_654 Pb101 . N113 . 134.9(2) yes O102 . Pb101 . N113 . 90.52(13) yes O102 14_654 Pb101 . N110 . 76.95(7) yes N113 14_654 Pb101 . N110 . 67.43(10) yes O102 . Pb101 . N110 . 76.95(7) yes N113 . Pb101 . N110 . 67.43(10) yes Pb101 . O102 . S103 . 117.36(16) yes O102 . S103 . O105 . 111.7(3) yes O102 . S103 . O104 . 114.7(2) yes O105 . S103 . O104 . 118.3(3) yes O102 . S103 . C106 . 101.9(2) yes O105 . S103 . C106 . 102.5(3) yes O104 . S103 . C106 . 105.3(3) yes S103 . C106 . F107 . 110.3(4) yes S103 . C106 . F109 . 110.2(4) yes F107 . C106 . F109 . 107.7(4) yes S103 . C106 . F108 . 110.9(4) yes F107 . C106 . F108 . 108.4(4) yes F109 . C106 . F108 . 109.1(5) yes Pb101 . N113 . C112 . 113.7(5) yes Pb101 . N113 . C114 . 124.8(3) yes C112 . N113 . C114 . 121.6(5) yes N113 . C112 . C111 . 121.3(6) yes N113 . C112 . H1121 . 119.8 no C111 . C112 . H1121 . 118.8 no C112 . C111 . N110 . 117.2(5) yes C112 . C111 . C121 . 121.9(5) yes N110 . C111 . C121 . 120.9(6) yes Pb101 . N110 . C111 14_654 120.4(4) yes Pb101 . N110 . C111 . 120.4(4) yes C111 14_654 N110 . C111 . 119.3(8) yes C111 . C121 . C122 . 117.3(7) yes C111 . C121 . H1211 . 120.3 no C122 . C121 . H1211 . 122.4 no C121 . C122 . C121 14_654 124.4(10) yes C121 . C122 . H1221 . 117.8 no C121 14_654 C122 . H1221 . 117.8 no N113 . C114 . C115 . 125.0(4) yes N113 . C114 . C120 . 117.7(4) yes C115 . C114 . C120 . 117.2(4) yes C114 . C115 . C116 . 121.4(4) yes C114 . C115 . H1151 . 118.8 no C116 . C115 . H1151 . 119.8 no C115 . C116 . C117 . 121.2(4) yes C115 . C116 . H1161 . 119.7 no C117 . C116 . H1161 . 119.1 no C116 . C117 . O118 . 123.5(5) yes C116 . C117 . C119 . 117.5(5) yes O118 . C117 . C119 . 118.9(4) yes C117 . O118 . H1181 . 106.9 no C117 . C119 . C120 . 121.0(4) yes C117 . C119 . H1191 . 119.2 no C120 . C119 . H1191 . 119.8 no C114 . C120 . C119 . 121.6(4) yes C114 . C120 . H1201 . 118.7 no C119 . C120 . H1201 . 119.7 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C119 . H1191 . O18 11_464 131 0.93 2.53 3.220(7) yes O118 . H1181 . O105 15_664 160 0.81 2.01 2.792(7) yes O18 . H181 . O5 15_674 166 0.81 1.97 2.765(7) yes _vrf_PLAT201_1 ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 44 RESPONSE: This is simply not true, all non-H atoms have been refined anisotropically ; #===END