#============================================================================== data_global #============================================================================== _publ_contact_author 'Harry L. Anderson' _publ_contact_author_email 'harry.anderson@chem.ox.ac.uk' loop_ _publ_author_name _publ_author_address 'Roche, C\'ecile' ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA. UK. ; 'Luo, Qianfu' ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA. UK. ; 'Gil-Ram\'irez, Guzm\'an' ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA. UK. ; 'Jiang, Hua-Wei' ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA. UK. ; 'Kohn, Daniel R.' ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA. UK. ; 'Xiong, Yaoyao' ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA. UK. ; 'Thompson, Amber L.' ; Chemical Crystallography Department, Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA. UK. ; 'Anderson, Harry L.' ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA. UK. ; _publ_requested_journal 'Journal of Organic Chemistry' _journal_volume '?' _journal_page_first '?' _journal_page_last '?' _journal_year '2017' _ccdc_journal_depnumber '?' _publ_section_title ; Unexpected interactions between alkyl straps and pyridyl ligands in sulfur-strapped porphyrin nanorings ; _publ_section_abstract ; Strapped – or 'basket-handle' – porphyrins have been investigated previously as hemoglobin mimics and catalysts. The facial selectivity of their interactions with axial ligands is a sensitive test for non-covalent bonding. Here the binding of pyridyl ligands to zinc porphyrins with thioester-linked alkyl straps is investigated in solution by NMR spectra and in the solid state by X-ray crystallography. We expected that coordination of the axial ligand would occur on the less hindered face of the porphyrin, away from the strap. Surprisingly, attractive interactions between the strap and the ligand direct axial coordination to the strapped face of the porphyrin, except when the strap is short and tight. The strapped porphyrins were incorporated into \p-conjugated 6-porphyrin nanorings using template-directed synthesis. The strap, and the sulfur substituents, are located either inside or outside the porphyrin nanoring, depending on the length of the strap. Six-porphyrin nanorings with outwardly pointing sulfur anchors were prepared for exploring quantum interference effects in single-molecule charge transport. ; #============================================================================== data_6a #============================================================================== _audit_creation_date "2017-01-25" _audit_creation_method CRYSTALS_ver_14.61_build_6019 _oxford_structure_analysis_title '6706 (005drk16)' _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 15.8256(2) _cell_length_b 16.3140(2) _cell_length_c 29.6844(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7663.88(16) _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'P c a 21 ' _symmetry_space_group_name_Hall 'P 2c -2ac' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x+1/2,y,z+1/2' 'x+1/2,-y,z' '-x,-y,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' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 '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' 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' _cell_formula_units_Z 8 # Given Formula = C46 H35 Br2 N5 O2 S2 Zn1 # Dc = 1.70 Fooo = 3952.00 Mu = 28.85 M = 979.14 # Found Formula = C46 H37 N5 O2 S2 Zn1 # Dc = 1.42 FOOO = 3408.00 Mu = 7.97 M = 821.34 _chemical_formula_sum 'C46 H37 N5 O2 S2 Zn1' _chemical_formula_moiety 'C46 H37 N5 O2 S2 Zn1' _chemical_compound_source . _chemical_formula_weight 821.34 _cell_measurement_reflns_used 28188 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description 'block' _exptl_crystal_colour 'clear_intense_purple' _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 3408 _exptl_absorpt_coefficient_mu 0.797 # Sheldrick geometric approximatio 0.79 0.85 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.85 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '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 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _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 150 _diffrn_reflns_number 92249 _reflns_number_total 52097 _diffrn_reflns_av_R_equivalents 0.044 # Number of reflections without Friedels Law is 17184 # Number of reflections with Friedels Law is 52097 # Theoretical number of reflections is about 8814 _diffrn_reflns_theta_min 5.132 _diffrn_reflns_theta_max 27.512 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.962 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _reflns_limit_h_min 0 _reflns_limit_h_max 20 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min -38 _reflns_limit_l_max 38 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom,iterative # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.29 _refine_diff_density_max 0.34 # 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>-3.0\s(I) _refine_ls_number_reflns 17184 _refine_ls_number_restraints 1 _refine_ls_number_parameters 1010 _oxford_refine_ls_R_factor_ref 0.0407 _refine_ls_wR_factor_ref 0.0757 _refine_ls_goodness_of_fit_ref 1.0000 _refine_ls_shift/su_max 0.0017020 _refine_ls_shift/su_mean 0.0000406 # The values computed with all filters except I/sigma _oxford_reflns_number_all 17184 _refine_ls_R_factor_all 0.0407 _refine_ls_wR_factor_all 0.0757 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 15482 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_gt 0.0706 _refine_ls_abs_structure_Flack 0.187(6) _refine_ls_abs_structure_details 'Flack (1983), 0 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 #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: 25.7 40.3 24.2 10.2 2.39 ; # 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. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. 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 atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Zn1 Zn 0.688584(17) 0.613708(16) 0.499974(17) 0.0199 1.0000 Uani . . . . . . N1 N 0.72750(13) 0.71910(13) 0.46614(7) 0.0223 1.0000 Uani . . . . . . N2 N 0.70965(14) 0.67167(13) 0.56111(7) 0.0235 1.0000 Uani . . . . . . N3 N 0.69204(13) 0.50376(13) 0.53477(7) 0.0207 1.0000 Uani . . . . . . N4 N 0.70731(13) 0.55103(12) 0.44042(7) 0.0193 1.0000 Uani . . . . . . N5 N 0.55636(12) 0.64436(13) 0.49879(8) 0.0239 1.0000 Uani . . . . . . C1 C 0.72863(16) 0.73007(16) 0.42026(9) 0.0236 1.0000 Uani . . . . . . C2 C 0.73599(18) 0.81735(17) 0.41036(10) 0.0310 1.0000 Uani . . . . . . C3 C 0.7400(2) 0.85651(18) 0.45052(10) 0.0337 1.0000 Uani . . . . . . C4 C 0.73434(17) 0.79514(16) 0.48539(9) 0.0260 1.0000 Uani . . . . . . C5 C 0.73145(19) 0.81089(17) 0.53153(10) 0.0302 1.0000 Uani . . . . . . C6 C 0.71856(18) 0.75402(17) 0.56641(9) 0.0268 1.0000 Uani . . . . . . C7 C 0.7097(2) 0.77522(19) 0.61349(9) 0.0350 1.0000 Uani . . . . . . C8 C 0.69376(19) 0.70518(19) 0.63585(9) 0.0339 1.0000 Uani . . . . . . C9 C 0.69537(16) 0.63928(18) 0.60317(9) 0.0256 1.0000 Uani . . . . . . C10 C 0.68672(16) 0.55586(17) 0.61275(8) 0.0254 1.0000 Uani . . . . . . C11 C 0.68978(15) 0.49263(16) 0.58052(8) 0.0237 1.0000 Uani . . . . . . C12 C 0.69206(16) 0.40587(17) 0.59073(9) 0.0270 1.0000 Uani . . . . . . C13 C 0.69512(16) 0.36595(16) 0.55102(9) 0.0254 1.0000 Uani . . . . . . C14 C 0.69554(15) 0.42738(16) 0.51606(9) 0.0223 1.0000 Uani . . . . . . C15 C 0.70077(16) 0.41064(16) 0.47012(9) 0.0227 1.0000 Uani . . . . . . C16 C 0.70686(15) 0.46788(16) 0.43535(8) 0.0220 1.0000 Uani . . . . . . C17 C 0.71511(16) 0.44705(16) 0.38805(9) 0.0238 1.0000 Uani . . . . . . C18 C 0.71963(16) 0.51867(16) 0.36525(9) 0.0247 1.0000 Uani . . . . . . C19 C 0.71505(15) 0.58373(16) 0.39812(8) 0.0212 1.0000 Uani . . . . . . C20 C 0.72116(16) 0.66803(16) 0.38811(8) 0.0227 1.0000 Uani . . . . . . C21 C 0.52686(19) 0.6998(2) 0.46903(10) 0.0398 1.0000 Uani . . . . . . C22 C 0.4444(2) 0.7269(2) 0.47012(12) 0.0485 1.0000 Uani . . . . . . C23 C 0.38982(16) 0.69739(19) 0.50149(12) 0.0387 1.0000 Uani . . . . . . C24 C 0.41929(19) 0.6405(2) 0.53196(11) 0.0385 1.0000 Uani . . . . . . C25 C 0.50223(18) 0.61613(18) 0.52969(9) 0.0311 1.0000 Uani . . . . . . C31 C 0.71962(17) 0.69068(15) 0.33938(9) 0.0247 1.0000 Uani . . . . . . C32 C 0.79356(19) 0.70795(18) 0.31564(10) 0.0331 1.0000 Uani . . . . . . C33 C 0.7917(2) 0.72650(19) 0.27005(10) 0.0373 1.0000 Uani . . . . . . C34 C 0.7158(2) 0.72624(18) 0.24716(10) 0.0386 1.0000 Uani . . . . . . C35 C 0.6420(2) 0.70812(17) 0.26934(9) 0.0328 1.0000 Uani . . . . . . C36 C 0.64309(18) 0.69053(16) 0.31537(9) 0.0270 1.0000 Uani . . . . . . C41 C 0.68006(18) 0.52895(17) 0.66113(9) 0.0275 1.0000 Uani . . . . . . C42 C 0.75103(19) 0.5319(2) 0.68836(9) 0.0351 1.0000 Uani . . . . . . C43 C 0.7502(2) 0.5011(2) 0.73225(9) 0.0385 1.0000 Uani . . . . . . C44 C 0.6765(2) 0.46788(19) 0.74910(10) 0.0392 1.0000 Uani . . . . . . C45 C 0.6038(2) 0.46615(19) 0.72295(9) 0.0362 1.0000 Uani . . . . . . C46 C 0.60508(17) 0.49608(17) 0.67919(9) 0.0286 1.0000 Uani . . . . . . S1 S 0.54628(4) 0.67429(4) 0.34422(3) 0.0300 1.0000 Uani . . . . . . S2 S 0.51075(4) 0.49687(4) 0.64667(3) 0.0302 1.0000 Uani . . . . . . O1 O 0.55619(14) 0.53481(13) 0.29882(7) 0.0370 1.0000 Uani . . . . . . O2 O 0.52269(16) 0.33472(14) 0.65522(9) 0.0481 1.0000 Uani . . . . . . C51 C 0.51972(17) 0.57133(18) 0.32825(9) 0.0292 1.0000 Uani . . . . . . C52 C 0.45139(18) 0.5362(2) 0.35729(10) 0.0364 1.0000 Uani . . . . . . C53 C 0.49125(17) 0.49437(18) 0.39873(9) 0.0308 1.0000 Uani . . . . . . C54 C 0.42785(18) 0.4611(2) 0.43222(10) 0.0350 1.0000 Uani . . . . . . C55 C 0.47262(17) 0.4214(2) 0.47200(10) 0.0318 1.0000 Uani . . . . . . C56 C 0.41616(17) 0.40337(19) 0.51275(9) 0.0323 1.0000 Uani . . . . . . C57 C 0.47030(18) 0.38246(19) 0.55368(10) 0.0333 1.0000 Uani . . . . . . C58 C 0.42302(18) 0.3822(2) 0.59913(10) 0.0361 1.0000 Uani . . . . . . C59 C 0.48733(18) 0.39064(18) 0.63654(9) 0.0319 1.0000 Uani . . . . . . Zn101 Zn 0.510191(17) 0.097487(17) 0.247850(17) 0.0217 1.0000 Uani . . . . . . N101 N 0.52775(14) 0.16986(13) 0.19189(7) 0.0241 1.0000 Uani . . . . . . N102 N 0.53272(14) 0.19604(13) 0.28932(7) 0.0249 1.0000 Uani . . . . . . N103 N 0.53393(14) 0.02278(13) 0.30346(7) 0.0246 1.0000 Uani . . . . . . N104 N 0.52969(14) -0.00362(13) 0.20569(7) 0.0241 1.0000 Uani . . . . . . N105 N 0.37809(13) 0.08341(12) 0.25134(8) 0.0243 1.0000 Uani . . . . . . C101 C 0.53378(17) 0.14651(17) 0.14743(9) 0.0268 1.0000 Uani . . . . . . C102 C 0.5392(2) 0.21840(18) 0.11917(10) 0.0337 1.0000 Uani . . . . . . C103 C 0.5371(2) 0.28393(18) 0.14691(10) 0.0369 1.0000 Uani . . . . . . C104 C 0.53022(18) 0.25364(17) 0.19230(9) 0.0288 1.0000 Uani . . . . . . C105 C 0.53075(19) 0.30251(17) 0.23084(10) 0.0317 1.0000 Uani . . . . . . C106 C 0.53485(18) 0.27568(17) 0.27551(9) 0.0275 1.0000 Uani . . . . . . C107 C 0.5454(2) 0.32947(17) 0.31395(10) 0.0329 1.0000 Uani . . . . . . C108 C 0.5501(2) 0.28070(18) 0.35079(9) 0.0319 1.0000 Uani . . . . . . C109 C 0.54217(17) 0.19683(16) 0.33556(9) 0.0256 1.0000 Uani . . . . . . C110 C 0.54621(16) 0.12734(17) 0.36275(9) 0.0256 1.0000 Uani . . . . . . C111 C 0.54331(16) 0.04575(17) 0.34754(9) 0.0248 1.0000 Uani . . . . . . C112 C 0.54796(18) -0.02653(17) 0.37548(9) 0.0289 1.0000 Uani . . . . . . C113 C 0.54074(19) -0.09219(17) 0.34812(10) 0.0314 1.0000 Uani . . . . . . C114 C 0.53155(17) -0.06121(16) 0.30292(9) 0.0252 1.0000 Uani . . . . . . C115 C 0.52519(19) -0.10929(17) 0.26417(10) 0.0295 1.0000 Uani . . . . . . C116 C 0.52728(17) -0.08387(16) 0.21944(9) 0.0262 1.0000 Uani . . . . . . C117 C 0.5312(2) -0.13734(17) 0.18091(10) 0.0339 1.0000 Uani . . . . . . C118 C 0.53705(19) -0.08891(18) 0.14410(10) 0.0319 1.0000 Uani . . . . . . C119 C 0.53463(17) -0.00456(16) 0.15976(8) 0.0250 1.0000 Uani . . . . . . C120 C 0.53713(17) 0.06490(17) 0.13227(9) 0.0267 1.0000 Uani . . . . . . C121 C 0.33473(18) 0.0674(2) 0.21405(10) 0.0346 1.0000 Uani . . . . . . C122 C 0.2530(2) 0.0373(2) 0.21532(11) 0.0443 1.0000 Uani . . . . . . C123 C 0.21682(19) 0.0226(2) 0.25638(11) 0.0407 1.0000 Uani . . . . . . C124 C 0.26044(19) 0.0415(2) 0.29525(11) 0.0361 1.0000 Uani . . . . . . C125 C 0.34037(18) 0.07118(18) 0.29134(9) 0.0308 1.0000 Uani . . . . . . C131 C 0.54550(18) 0.05298(17) 0.08213(9) 0.0284 1.0000 Uani . . . . . . C132 C 0.4754(2) 0.0623(2) 0.05432(10) 0.0395 1.0000 Uani . . . . . . C133 C 0.4826(2) 0.0554(2) 0.00756(10) 0.0466 1.0000 Uani . . . . . . C134 C 0.5605(2) 0.0384(2) -0.01153(10) 0.0438 1.0000 Uani . . . . . . C135 C 0.6309(2) 0.02911(19) 0.01523(9) 0.0349 1.0000 Uani . . . . . . C136 C 0.62384(18) 0.03623(17) 0.06195(9) 0.0290 1.0000 Uani . . . . . . C141 C 0.55197(18) 0.14023(16) 0.41293(9) 0.0281 1.0000 Uani . . . . . . C142 C 0.48123(19) 0.16838(19) 0.43647(10) 0.0346 1.0000 Uani . . . . . . C143 C 0.4844(2) 0.1816(2) 0.48270(11) 0.0431 1.0000 Uani . . . . . . C144 C 0.5583(2) 0.1679(2) 0.50579(11) 0.0457 1.0000 Uani . . . . . . C145 C 0.6288(2) 0.1400(2) 0.48354(10) 0.0410 1.0000 Uani . . . . . . C146 C 0.62643(19) 0.12616(17) 0.43743(9) 0.0305 1.0000 Uani . . . . . . S101 S 0.71591(5) 0.02740(5) 0.09570(3) 0.0321 1.0000 Uani . . . . . . S102 S 0.71846(5) 0.08940(5) 0.40964(3) 0.0333 1.0000 Uani . . . . . . O101 O 0.72837(16) 0.17944(14) 0.06586(8) 0.0429 1.0000 Uani . . . . . . O102 O 0.74465(16) 0.24926(14) 0.40711(8) 0.0490 1.0000 Uani . . . . . . C151 C 0.75364(19) 0.1323(2) 0.09337(10) 0.0347 1.0000 Uani . . . . . . C152 C 0.8134(2) 0.1527(2) 0.13112(11) 0.0429 1.0000 Uani . . . . . . C153 C 0.7610(2) 0.1933(2) 0.16942(11) 0.0430 1.0000 Uani . . . . . . C154 C 0.8106(2) 0.2084(2) 0.21203(11) 0.0444 1.0000 Uani . . . . . . C155 C 0.7544(2) 0.2453(2) 0.24850(14) 0.0448 1.0000 Uani . . . . . . C156 C 0.7947(2) 0.2502(2) 0.29530(11) 0.0450 1.0000 Uani . . . . . . C157 C 0.8137(2) 0.1673(2) 0.31492(11) 0.0429 1.0000 Uani . . . . . . C158 C 0.8421(2) 0.1694(2) 0.36386(11) 0.0456 1.0000 Uani . . . . . . C159 C 0.76886(19) 0.18413(18) 0.39466(9) 0.0330 1.0000 Uani . . . . . . H21 H 0.7371 0.8403 0.3821 0.0371 1.0000 Uiso R . . . . . H31 H 0.7454 0.9113 0.4555 0.0412 1.0000 Uiso R . . . . . H51 H 0.7393 0.8651 0.5404 0.0367 1.0000 Uiso R . . . . . H71 H 0.7145 0.8261 0.6256 0.0425 1.0000 Uiso R . . . . . H81 H 0.6836 0.6993 0.6668 0.0394 1.0000 Uiso R . . . . . H121 H 0.6913 0.3832 0.6193 0.0309 1.0000 Uiso R . . . . . H131 H 0.6952 0.3106 0.5474 0.0310 1.0000 Uiso R . . . . . H151 H 0.7002 0.3559 0.4623 0.0264 1.0000 Uiso R . . . . . H171 H 0.7179 0.3951 0.3760 0.0293 1.0000 Uiso R . . . . . H181 H 0.7242 0.5260 0.3336 0.0303 1.0000 Uiso R . . . . . H211 H 0.5633 0.7197 0.4466 0.0480 1.0000 Uiso R . . . . . H221 H 0.4271 0.7646 0.4491 0.0587 1.0000 Uiso R . . . . . H231 H 0.3341 0.7155 0.5027 0.0469 1.0000 Uiso R . . . . . H241 H 0.3846 0.6198 0.5535 0.0457 1.0000 Uiso R . . . . . H251 H 0.5238 0.5784 0.5504 0.0381 1.0000 Uiso R . . . . . H321 H 0.8453 0.7056 0.3314 0.0392 1.0000 Uiso R . . . . . H331 H 0.8423 0.7388 0.2554 0.0443 1.0000 Uiso R . . . . . H341 H 0.7144 0.7383 0.2165 0.0462 1.0000 Uiso R . . . . . H351 H 0.5903 0.7078 0.2538 0.0384 1.0000 Uiso R . . . . . H421 H 0.8011 0.5516 0.6763 0.0419 1.0000 Uiso R . . . . . H431 H 0.7994 0.5028 0.7493 0.0457 1.0000 Uiso R . . . . . H441 H 0.6763 0.4455 0.7778 0.0468 1.0000 Uiso R . . . . . H451 H 0.5534 0.4443 0.7339 0.0436 1.0000 Uiso R . . . . . H521 H 0.4206 0.4955 0.3405 0.0441 1.0000 Uiso R . . . . . H522 H 0.4137 0.5785 0.3664 0.0441 1.0000 Uiso R . . . . . H531 H 0.5279 0.4513 0.3884 0.0368 1.0000 Uiso R . . . . . H532 H 0.5271 0.5328 0.4139 0.0373 1.0000 Uiso R . . . . . H541 H 0.3928 0.4223 0.4164 0.0422 1.0000 Uiso R . . . . . H542 H 0.3928 0.5063 0.4421 0.0425 1.0000 Uiso R . . . . . H551 H 0.4979 0.3711 0.4621 0.0381 1.0000 Uiso R . . . . . H552 H 0.5165 0.4566 0.4825 0.0375 1.0000 Uiso R . . . . . H561 H 0.3780 0.3589 0.5054 0.0384 1.0000 Uiso R . . . . . H562 H 0.3823 0.4515 0.5195 0.0388 1.0000 Uiso R . . . . . H571 H 0.4960 0.3299 0.5489 0.0411 1.0000 Uiso R . . . . . H572 H 0.5144 0.4238 0.5563 0.0397 1.0000 Uiso R . . . . . H581 H 0.3913 0.3307 0.6032 0.0430 1.0000 Uiso R . . . . . H582 H 0.3849 0.4295 0.6009 0.0433 1.0000 Uiso R . . . . . H1021 H 0.5434 0.2194 0.0874 0.0404 1.0000 Uiso R . . . . . H1031 H 0.5401 0.3377 0.1387 0.0439 1.0000 Uiso R . . . . . H1051 H 0.5299 0.3597 0.2267 0.0377 1.0000 Uiso R . . . . . H1071 H 0.5488 0.3852 0.3125 0.0393 1.0000 Uiso R . . . . . H1081 H 0.5590 0.2974 0.3801 0.0376 1.0000 Uiso R . . . . . H1121 H 0.5540 -0.0269 0.4057 0.0344 1.0000 Uiso R . . . . . H1131 H 0.5431 -0.1479 0.3563 0.0374 1.0000 Uiso R . . . . . H1151 H 0.5234 -0.1662 0.2695 0.0356 1.0000 Uiso R . . . . . H1171 H 0.5297 -0.1934 0.1817 0.0411 1.0000 Uiso R . . . . . H1181 H 0.5419 -0.1071 0.1140 0.0373 1.0000 Uiso R . . . . . H1211 H 0.3611 0.0757 0.1865 0.0418 1.0000 Uiso R . . . . . H1221 H 0.2233 0.0278 0.1886 0.0533 1.0000 Uiso R . . . . . H1231 H 0.1626 -0.0005 0.2580 0.0495 1.0000 Uiso R . . . . . H1241 H 0.2377 0.0341 0.3235 0.0429 1.0000 Uiso R . . . . . H1251 H 0.3719 0.0816 0.3170 0.0376 1.0000 Uiso R . . . . . H1321 H 0.4226 0.0752 0.0667 0.0476 1.0000 Uiso R . . . . . H1331 H 0.4351 0.0624 -0.0107 0.0560 1.0000 Uiso R . . . . . H1341 H 0.5652 0.0329 -0.0426 0.0527 1.0000 Uiso R . . . . . H1351 H 0.6847 0.0187 0.0024 0.0423 1.0000 Uiso R . . . . . H1421 H 0.4316 0.1780 0.4212 0.0413 1.0000 Uiso R . . . . . H1431 H 0.4354 0.1993 0.4971 0.0516 1.0000 Uiso R . . . . . H1441 H 0.5614 0.1787 0.5368 0.0549 1.0000 Uiso R . . . . . H1451 H 0.6788 0.1301 0.4989 0.0485 1.0000 Uiso R . . . . . H1521 H 0.8404 0.1035 0.1419 0.0515 1.0000 Uiso R . . . . . H1522 H 0.8553 0.1920 0.1203 0.0520 1.0000 Uiso R . . . . . H1531 H 0.7130 0.1561 0.1763 0.0520 1.0000 Uiso R . . . . . H1532 H 0.7375 0.2449 0.1596 0.0522 1.0000 Uiso R . . . . . H1541 H 0.8335 0.1550 0.2233 0.0547 1.0000 Uiso R . . . . . H1542 H 0.8572 0.2467 0.2054 0.0548 1.0000 Uiso R . . . . . H1551 H 0.7045 0.2088 0.2515 0.0538 1.0000 Uiso R . . . . . H1552 H 0.7354 0.2997 0.2388 0.0542 1.0000 Uiso R . . . . . H1561 H 0.8479 0.2819 0.2933 0.0538 1.0000 Uiso R . . . . . H1562 H 0.7574 0.2793 0.3159 0.0538 1.0000 Uiso R . . . . . H1571 H 0.8580 0.1402 0.2972 0.0527 1.0000 Uiso R . . . . . H1572 H 0.7623 0.1346 0.3129 0.0516 1.0000 Uiso R . . . . . H1581 H 0.8663 0.1167 0.3721 0.0553 1.0000 Uiso R . . . . . H1582 H 0.8830 0.2131 0.3685 0.0551 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 Zn1 0.02047(12) 0.02116(12) 0.01804(11) -0.00089(12) 0.00010(11) 0.00097(11) N1 0.0238(10) 0.0200(10) 0.0231(10) 0.0002(8) 0.0000(8) 0.0006(8) N2 0.0273(11) 0.0220(11) 0.0212(10) -0.0030(8) -0.0026(8) -0.0004(8) N3 0.0219(10) 0.0216(10) 0.0186(9) -0.0003(8) 0.0000(8) 0.0016(8) N4 0.0205(10) 0.0200(10) 0.0174(9) -0.0025(8) 0.0001(7) 0.0023(8) N5 0.0219(9) 0.0284(10) 0.0214(9) -0.0033(10) -0.0006(9) 0.0022(8) C1 0.0206(12) 0.0265(13) 0.0238(12) 0.0027(10) 0.0008(10) 0.0004(10) C2 0.0378(15) 0.0274(14) 0.0276(13) 0.0063(11) 0.0000(11) -0.0054(11) C3 0.0430(17) 0.0236(13) 0.0345(15) 0.0015(11) -0.0018(12) -0.0073(12) C4 0.0265(13) 0.0241(12) 0.0273(13) -0.0008(10) -0.0014(10) -0.0026(10) C5 0.0377(16) 0.0226(13) 0.0303(14) -0.0059(11) 0.0009(12) -0.0026(11) C6 0.0285(13) 0.0263(13) 0.0256(13) -0.0027(10) 0.0006(10) -0.0017(11) C7 0.0477(18) 0.0304(15) 0.0269(14) -0.0092(12) -0.0014(12) -0.0035(13) C8 0.0420(17) 0.0369(16) 0.0226(13) -0.0051(11) 0.0017(11) -0.0035(13) C9 0.0247(13) 0.0343(14) 0.0178(11) -0.0048(10) 0.0004(9) -0.0011(11) C10 0.0226(12) 0.0346(14) 0.0190(12) 0.0008(10) -0.0008(10) -0.0013(11) C11 0.0206(11) 0.0292(13) 0.0212(11) 0.0021(10) 0.0010(9) 0.0015(10) C12 0.0261(12) 0.0313(14) 0.0237(12) 0.0069(10) 0.0014(10) 0.0027(11) C13 0.0262(12) 0.0207(12) 0.0291(13) 0.0034(10) 0.0034(10) 0.0031(10) C14 0.0189(11) 0.0225(12) 0.0256(12) 0.0019(9) 0.0002(9) 0.0023(9) C15 0.0241(12) 0.0190(12) 0.0249(12) -0.0020(10) 0.0018(10) 0.0033(9) C16 0.0194(11) 0.0257(13) 0.0211(12) -0.0006(10) 0.0002(9) 0.0010(9) C17 0.0250(12) 0.0236(12) 0.0227(12) -0.0054(10) 0.0000(10) 0.0035(10) C18 0.0226(12) 0.0298(13) 0.0216(11) -0.0029(10) 0.0014(9) 0.0007(10) C19 0.0190(11) 0.0273(13) 0.0172(11) -0.0013(9) 0.0001(9) 0.0022(10) C20 0.0199(11) 0.0261(12) 0.0220(12) 0.0021(10) 0.0003(9) 0.0009(10) C21 0.0271(14) 0.059(2) 0.0335(15) 0.0093(14) 0.0022(11) 0.0055(13) C22 0.0303(16) 0.069(2) 0.0461(19) 0.0116(17) -0.0071(14) 0.0143(16) C23 0.0203(12) 0.0492(17) 0.0465(16) -0.0097(16) -0.0017(13) 0.0032(11) C24 0.0267(14) 0.0500(18) 0.0387(15) -0.0067(14) 0.0087(12) -0.0046(13) C25 0.0301(14) 0.0360(15) 0.0273(13) -0.0016(11) 0.0019(11) 0.0011(12) C31 0.0299(13) 0.0213(12) 0.0231(12) 0.0002(10) 0.0009(10) 0.0009(10) C32 0.0347(15) 0.0340(15) 0.0305(14) 0.0019(11) 0.0023(11) -0.0007(12) C33 0.0455(18) 0.0315(15) 0.0349(15) 0.0022(12) 0.0140(13) -0.0022(13) C34 0.0602(18) 0.0334(14) 0.0222(12) 0.0055(13) 0.0072(14) 0.0086(13) C35 0.0450(17) 0.0309(14) 0.0225(13) 0.0002(11) -0.0022(12) 0.0070(12) C36 0.0353(14) 0.0236(13) 0.0221(12) 0.0015(10) 0.0001(10) 0.0042(11) C41 0.0320(14) 0.0294(13) 0.0211(12) -0.0017(10) 0.0027(10) -0.0022(11) C42 0.0367(15) 0.0464(17) 0.0223(13) 0.0001(12) -0.0021(11) -0.0065(13) C43 0.0453(17) 0.0480(17) 0.0223(12) 0.0002(13) -0.0046(12) -0.0039(14) C44 0.0530(18) 0.0448(16) 0.0199(12) 0.0022(13) 0.0024(13) -0.0006(14) C45 0.0425(17) 0.0370(16) 0.0292(14) 0.0002(12) 0.0097(12) -0.0062(13) C46 0.0329(14) 0.0287(13) 0.0242(12) -0.0015(11) 0.0039(11) 0.0003(11) S1 0.0272(3) 0.0322(4) 0.0307(3) -0.0017(3) -0.0004(3) 0.0047(3) S2 0.0297(3) 0.0288(3) 0.0321(3) 0.0007(3) 0.0031(3) 0.0011(3) O1 0.0411(12) 0.0376(11) 0.0323(11) -0.0040(9) -0.0023(9) -0.0015(9) O2 0.0567(15) 0.0317(11) 0.0559(14) 0.0118(10) -0.0155(12) -0.0058(11) C51 0.0244(13) 0.0335(14) 0.0298(13) 0.0023(11) -0.0095(10) 0.0023(11) C52 0.0260(14) 0.0441(17) 0.0392(16) 0.0031(13) -0.0056(12) -0.0040(12) C53 0.0236(12) 0.0380(15) 0.0307(13) -0.0038(11) -0.0028(10) -0.0013(11) C54 0.0223(13) 0.0468(17) 0.0360(15) 0.0007(13) -0.0026(11) -0.0040(12) C55 0.0234(13) 0.0411(16) 0.0309(14) -0.0047(12) -0.0010(11) -0.0037(11) C56 0.0219(12) 0.0405(16) 0.0346(14) -0.0007(11) -0.0005(10) -0.0041(11) C57 0.0292(14) 0.0345(15) 0.0362(15) -0.0033(12) -0.0013(11) -0.0015(12) C58 0.0291(14) 0.0418(16) 0.0374(15) 0.0046(13) 0.0000(12) -0.0056(12) C59 0.0333(14) 0.0325(14) 0.0301(13) 0.0032(11) 0.0038(11) -0.0049(12) Zn101 0.02436(14) 0.02014(12) 0.02046(12) -0.00113(11) 0.00103(12) 0.00047(11) N101 0.0282(11) 0.0230(11) 0.0212(10) 0.0006(8) 0.0027(8) 0.0005(9) N102 0.0292(11) 0.0206(11) 0.0248(11) -0.0026(8) 0.0005(9) -0.0017(8) N103 0.0275(11) 0.0229(11) 0.0234(11) 0.0014(8) -0.0017(9) 0.0009(9) N104 0.0251(10) 0.0229(11) 0.0241(10) -0.0019(9) 0.0025(9) -0.0005(8) N105 0.0255(10) 0.0238(10) 0.0234(10) -0.0001(9) 0.0010(9) 0.0012(8) C101 0.0271(13) 0.0301(14) 0.0233(12) -0.0002(11) 0.0039(10) 0.0013(10) C102 0.0468(17) 0.0305(14) 0.0239(13) 0.0034(11) 0.0058(12) 0.0047(13) C103 0.0555(19) 0.0237(14) 0.0317(15) 0.0052(12) 0.0028(14) 0.0039(13) C104 0.0356(15) 0.0226(13) 0.0283(13) 0.0010(10) 0.0025(11) 0.0031(11) C105 0.0391(16) 0.0195(13) 0.0365(15) -0.0005(11) 0.0058(12) 0.0029(11) C106 0.0330(14) 0.0223(13) 0.0271(13) -0.0019(10) 0.0023(11) 0.0021(11) C107 0.0457(17) 0.0185(13) 0.0345(15) -0.0033(11) 0.0028(13) -0.0005(11) C108 0.0422(16) 0.0288(14) 0.0247(13) -0.0078(11) 0.0001(11) 0.0000(12) C109 0.0264(13) 0.0265(13) 0.0238(12) -0.0040(10) 0.0007(10) -0.0001(10) C110 0.0221(12) 0.0308(14) 0.0240(12) -0.0017(11) 0.0010(10) -0.0022(10) C111 0.0206(11) 0.0295(13) 0.0245(12) 0.0018(10) 0.0008(10) 0.0000(10) C112 0.0321(14) 0.0325(14) 0.0221(12) 0.0042(10) 0.0017(10) -0.0035(11) C113 0.0385(15) 0.0252(14) 0.0305(14) 0.0055(11) 0.0013(12) -0.0006(12) C114 0.0259(13) 0.0226(13) 0.0271(13) 0.0021(10) -0.0007(10) -0.0016(10) C115 0.0366(15) 0.0195(13) 0.0323(14) -0.0004(11) 0.0027(11) -0.0010(11) C116 0.0296(13) 0.0201(12) 0.0288(13) -0.0019(10) 0.0023(11) 0.0006(10) C117 0.0458(17) 0.0215(13) 0.0345(15) -0.0067(11) 0.0017(13) -0.0034(12) C118 0.0358(15) 0.0312(15) 0.0288(14) -0.0096(11) 0.0028(12) -0.0008(12) C119 0.0262(12) 0.0246(13) 0.0241(12) -0.0033(10) 0.0020(10) -0.0016(10) C120 0.0258(13) 0.0306(14) 0.0235(12) -0.0013(11) -0.0012(10) 0.0001(11) C121 0.0290(14) 0.0508(18) 0.0239(13) 0.0006(12) 0.0006(11) 0.0059(13) C122 0.0309(16) 0.065(2) 0.0367(17) -0.0174(16) -0.0089(12) 0.0013(15) C123 0.0286(13) 0.0397(16) 0.054(2) -0.0047(14) 0.0020(13) -0.0036(12) C124 0.0309(15) 0.0393(17) 0.0381(16) 0.0071(13) 0.0068(12) 0.0014(12) C125 0.0313(14) 0.0373(15) 0.0238(13) 0.0000(11) 0.0042(11) 0.0027(11) C131 0.0357(14) 0.0276(13) 0.0219(12) -0.0046(10) 0.0034(11) -0.0025(11) C132 0.0356(16) 0.0522(19) 0.0307(15) -0.0060(13) -0.0028(12) -0.0009(14) C133 0.0496(18) 0.062(2) 0.0284(16) -0.0032(14) -0.0117(13) -0.0037(16) C134 0.061(2) 0.0499(19) 0.0205(13) -0.0063(12) 0.0006(13) -0.0045(16) C135 0.0418(16) 0.0367(15) 0.0261(13) -0.0046(11) 0.0044(12) -0.0002(13) C136 0.0353(14) 0.0254(13) 0.0264(13) -0.0041(10) 0.0029(11) 0.0024(11) C141 0.0328(14) 0.0257(13) 0.0257(13) -0.0003(10) -0.0004(11) -0.0034(11) C142 0.0331(15) 0.0386(16) 0.0321(14) -0.0043(12) 0.0011(12) -0.0043(12) C143 0.0518(19) 0.0435(18) 0.0342(15) -0.0092(14) 0.0139(14) -0.0032(15) C144 0.063(2) 0.0488(19) 0.0248(15) -0.0062(14) 0.0037(14) -0.0044(16) C145 0.0501(18) 0.0458(18) 0.0271(13) -0.0004(13) -0.0085(13) -0.0024(15) C146 0.0357(14) 0.0298(14) 0.0260(13) -0.0005(11) 0.0002(11) -0.0027(11) S101 0.0335(3) 0.0334(4) 0.0294(3) 0.0013(3) 0.0022(3) 0.0043(3) S102 0.0329(4) 0.0314(4) 0.0356(4) -0.0008(3) -0.0026(3) 0.0025(3) O101 0.0541(14) 0.0374(12) 0.0373(11) 0.0062(10) -0.0055(10) -0.0089(10) O102 0.0623(16) 0.0352(12) 0.0495(14) -0.0071(10) 0.0162(12) -0.0053(11) C151 0.0360(15) 0.0424(17) 0.0255(13) 0.0019(13) 0.0068(11) -0.0037(13) C152 0.0365(16) 0.052(2) 0.0397(17) 0.0018(14) -0.0013(13) -0.0058(15) C153 0.0391(17) 0.058(2) 0.0320(16) -0.0030(14) 0.0010(13) 0.0043(15) C154 0.0368(17) 0.052(2) 0.0440(18) -0.0051(15) 0.0004(14) -0.0037(15) C155 0.0456(16) 0.0447(16) 0.0440(16) -0.0035(18) -0.0010(15) 0.0018(15) C156 0.052(2) 0.0441(18) 0.0391(17) -0.0120(14) -0.0016(15) 0.0036(15) C157 0.0471(18) 0.0426(18) 0.0388(16) -0.0037(14) 0.0102(14) 0.0001(15) C158 0.0425(18) 0.049(2) 0.0452(18) -0.0034(16) 0.0073(15) -0.0032(15) C159 0.0368(16) 0.0340(15) 0.0281(14) -0.0049(12) -0.0036(12) 0.0009(12) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 0.20564(5) 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 . N1 . 2.084(2) yes Zn1 . N2 . 2.073(2) yes Zn1 . N3 . 2.071(2) yes Zn1 . N4 . 2.064(2) yes Zn1 . N5 . 2.1518(19) yes N1 . C1 . 1.374(3) yes N1 . C4 . 1.370(3) yes N2 . C6 . 1.360(3) yes N2 . C9 . 1.374(3) yes N3 . C11 . 1.371(3) yes N3 . C14 . 1.365(3) yes N4 . C16 . 1.365(3) yes N4 . C19 . 1.370(3) yes N5 . C21 . 1.347(4) yes N5 . C25 . 1.337(3) yes C1 . C2 . 1.459(4) yes C1 . C20 . 1.396(4) yes C2 . C3 . 1.354(4) yes C2 . H21 . 0.919 no C3 . C4 . 1.443(4) yes C3 . H31 . 0.910 no C4 . C5 . 1.394(4) yes C5 . C6 . 1.405(4) yes C5 . H51 . 0.932 no C6 . C7 . 1.446(4) yes C7 . C8 . 1.345(4) yes C7 . H71 . 0.908 no C8 . C9 . 1.448(4) yes C8 . H81 . 0.938 no C9 . C10 . 1.397(4) yes C10 . C11 . 1.408(4) yes C10 . C41 . 1.505(4) yes C11 . C12 . 1.448(4) yes C12 . C13 . 1.347(4) yes C12 . H121 . 0.926 no C13 . C14 . 1.443(4) yes C13 . H131 . 0.909 no C14 . C15 . 1.393(4) yes C15 . C16 . 1.395(4) yes C15 . H151 . 0.922 no C16 . C17 . 1.451(3) yes C17 . C18 . 1.352(4) yes C17 . H171 . 0.920 no C18 . C19 . 1.444(4) yes C18 . H181 . 0.949 no C19 . C20 . 1.410(4) yes C20 . C31 . 1.493(3) yes C21 . C22 . 1.379(4) yes C21 . H211 . 0.939 no C22 . C23 . 1.358(5) yes C22 . H221 . 0.919 no C23 . C24 . 1.377(5) yes C23 . H231 . 0.931 no C24 . C25 . 1.373(4) yes C24 . H241 . 0.908 no C25 . H251 . 0.936 no C31 . C32 . 1.395(4) yes C31 . C36 . 1.405(4) yes C32 . C33 . 1.387(4) yes C32 . H321 . 0.945 no C33 . C34 . 1.380(5) yes C33 . H331 . 0.932 no C34 . C35 . 1.373(4) yes C34 . H341 . 0.931 no C35 . C36 . 1.396(4) yes C35 . H351 . 0.938 no C36 . S1 . 1.775(3) yes C41 . C42 . 1.385(4) yes C41 . C46 . 1.408(4) yes C42 . C43 . 1.396(4) yes C42 . H421 . 0.927 no C43 . C44 . 1.381(4) yes C43 . H431 . 0.930 no C44 . C45 . 1.388(4) yes C44 . H441 . 0.928 no C45 . C46 . 1.388(4) yes C45 . H451 . 0.932 no C46 . S2 . 1.778(3) yes S1 . C51 . 1.795(3) yes S2 . C59 . 1.798(3) yes O1 . C51 . 1.205(4) yes O2 . C59 . 1.205(4) yes C51 . C52 . 1.497(4) yes C52 . C53 . 1.542(4) yes C52 . H521 . 0.961 no C52 . H522 . 0.951 no C53 . C54 . 1.513(4) yes C53 . H531 . 0.961 no C53 . H532 . 0.958 no C54 . C55 . 1.522(4) yes C54 . H541 . 0.963 no C54 . H542 . 0.968 no C55 . C56 . 1.532(4) yes C55 . H551 . 0.959 no C55 . H552 . 0.953 no C56 . C57 . 1.525(4) yes C56 . H561 . 0.970 no C56 . H562 . 0.972 no C57 . C58 . 1.543(4) yes C57 . H571 . 0.960 no C57 . H572 . 0.974 no C58 . C59 . 1.513(4) yes C58 . H581 . 0.987 no C58 . H582 . 0.980 no Zn101 . N101 . 2.057(2) yes Zn101 . N102 . 2.056(2) yes Zn101 . N103 . 2.086(2) yes Zn101 . N104 . 2.093(2) yes Zn101 . N105 . 2.106(2) yes N101 . C101 . 1.377(3) yes N101 . C104 . 1.367(3) yes N102 . C106 . 1.363(3) yes N102 . C109 . 1.381(3) yes N103 . C111 . 1.369(3) yes N103 . C114 . 1.371(3) yes N104 . C116 . 1.372(3) yes N104 . C119 . 1.366(3) yes N105 . C121 . 1.328(4) yes N105 . C125 . 1.344(3) yes C101 . C102 . 1.444(4) yes C101 . C120 . 1.406(4) yes C102 . C103 . 1.350(4) yes C102 . H1021 . 0.947 no C103 . C104 . 1.439(4) yes C103 . H1031 . 0.911 no C104 . C105 . 1.394(4) yes C105 . C106 . 1.398(4) yes C105 . H1051 . 0.941 no C106 . C107 . 1.449(4) yes C107 . C108 . 1.355(4) yes C107 . H1071 . 0.912 no C108 . C109 . 1.447(4) yes C108 . H1081 . 0.924 no C109 . C110 . 1.393(4) yes C110 . C111 . 1.406(4) yes C110 . C141 . 1.507(4) yes C111 . C112 . 1.443(4) yes C112 . C113 . 1.349(4) yes C112 . H1121 . 0.901 no C113 . C114 . 1.441(4) yes C113 . H1131 . 0.941 no C114 . C115 . 1.396(4) yes C115 . C116 . 1.392(4) yes C115 . H1151 . 0.942 no C116 . C117 . 1.440(4) yes C117 . C118 . 1.352(4) yes C117 . H1171 . 0.915 no C118 . C119 . 1.453(4) yes C118 . H1181 . 0.945 no C119 . C120 . 1.397(4) yes C120 . C131 . 1.507(4) yes C121 . C122 . 1.384(4) yes C121 . H1211 . 0.929 no C122 . C123 . 1.368(5) yes C122 . H1221 . 0.935 no C123 . C124 . 1.380(4) yes C123 . H1231 . 0.939 no C124 . C125 . 1.359(4) yes C124 . H1241 . 0.920 no C125 . H1251 . 0.926 no C131 . C132 . 1.391(4) yes C131 . C136 . 1.404(4) yes C132 . C133 . 1.397(4) yes C132 . H1321 . 0.937 no C133 . C134 . 1.385(5) yes C133 . H1331 . 0.934 no C134 . C135 . 1.376(4) yes C134 . H1341 . 0.929 no C135 . C136 . 1.396(4) yes C135 . H1351 . 0.948 no C136 . S101 . 1.774(3) yes C141 . C142 . 1.397(4) yes C141 . C146 . 1.404(4) yes C142 . C143 . 1.390(4) yes C142 . H1421 . 0.920 no C143 . C144 . 1.375(5) yes C143 . H1431 . 0.929 no C144 . C145 . 1.374(5) yes C144 . H1441 . 0.939 no C145 . C146 . 1.388(4) yes C145 . H1451 . 0.927 no C146 . S102 . 1.778(3) yes S101 . C151 . 1.815(3) yes S102 . C159 . 1.795(3) yes O101 . C151 . 1.190(4) yes O102 . C159 . 1.188(4) yes C151 . C152 . 1.504(4) yes C152 . C153 . 1.556(5) yes C152 . H1521 . 0.963 no C152 . H1522 . 0.977 no C153 . C154 . 1.509(4) yes C153 . H1531 . 0.994 no C153 . H1532 . 0.966 no C154 . C155 . 1.525(5) yes C154 . H1541 . 0.999 no C154 . H1542 . 0.987 no C155 . C156 . 1.531(5) yes C155 . H1551 . 0.993 no C155 . H1552 . 0.981 no C156 . C157 . 1.502(5) yes C156 . H1561 . 0.990 no C156 . H1562 . 0.974 no C157 . C158 . 1.521(5) yes C157 . H1571 . 0.982 no C157 . H1572 . 0.976 no C158 . C159 . 1.496(4) yes C158 . H1581 . 0.972 no C158 . H1582 . 0.972 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Zn1 . N2 . 89.89(8) yes N1 . Zn1 . N3 . 161.30(8) yes N2 . Zn1 . N3 . 87.37(8) yes N1 . Zn1 . N4 . 87.34(8) yes N2 . Zn1 . N4 . 162.31(8) yes N3 . Zn1 . N4 . 89.67(8) yes N1 . Zn1 . N5 . 95.03(8) yes N2 . Zn1 . N5 . 93.71(8) yes N3 . Zn1 . N5 . 103.60(8) yes N4 . Zn1 . N5 . 103.93(8) yes Zn1 . N1 . C1 . 126.08(17) yes Zn1 . N1 . C4 . 124.71(17) yes C1 . N1 . C4 . 107.1(2) yes Zn1 . N2 . C6 . 124.64(18) yes Zn1 . N2 . C9 . 126.39(17) yes C6 . N2 . C9 . 107.0(2) yes Zn1 . N3 . C11 . 127.47(17) yes Zn1 . N3 . C14 . 126.06(16) yes C11 . N3 . C14 . 106.5(2) yes Zn1 . N4 . C16 . 125.89(17) yes Zn1 . N4 . C19 . 127.24(16) yes C16 . N4 . C19 . 106.6(2) yes Zn1 . N5 . C21 . 120.24(18) yes Zn1 . N5 . C25 . 122.12(18) yes C21 . N5 . C25 . 117.3(2) yes N1 . C1 . C2 . 109.1(2) yes N1 . C1 . C20 . 125.6(2) yes C2 . C1 . C20 . 125.2(2) yes C1 . C2 . C3 . 106.7(2) yes C1 . C2 . H21 . 125.6 no C3 . C2 . H21 . 127.7 no C2 . C3 . C4 . 107.5(2) yes C2 . C3 . H31 . 127.6 no C4 . C3 . H31 . 124.9 no C3 . C4 . N1 . 109.5(2) yes C3 . C4 . C5 . 125.4(3) yes N1 . C4 . C5 . 125.0(2) yes C4 . C5 . C6 . 127.4(2) yes C4 . C5 . H51 . 116.7 no C6 . C5 . H51 . 115.9 no C5 . C6 . N2 . 125.6(2) yes C5 . C6 . C7 . 124.6(3) yes N2 . C6 . C7 . 109.8(2) yes C6 . C7 . C8 . 107.0(3) yes C6 . C7 . H71 . 126.4 no C8 . C7 . H71 . 126.7 no C7 . C8 . C9 . 107.3(2) yes C7 . C8 . H81 . 127.0 no C9 . C8 . H81 . 125.7 no C8 . C9 . N2 . 109.0(2) yes C8 . C9 . C10 . 125.8(2) yes N2 . C9 . C10 . 125.1(2) yes C9 . C10 . C11 . 124.9(2) yes C9 . C10 . C41 . 119.0(2) yes C11 . C10 . C41 . 115.9(2) yes C10 . C11 . N3 . 125.3(2) yes C10 . C11 . C12 . 125.1(2) yes N3 . C11 . C12 . 109.6(2) yes C11 . C12 . C13 . 106.9(2) yes C11 . C12 . H121 . 125.6 no C13 . C12 . H121 . 127.6 no C12 . C13 . C14 . 107.1(2) yes C12 . C13 . H131 . 125.7 no C14 . C13 . H131 . 127.2 no C13 . C14 . N3 . 109.9(2) yes C13 . C14 . C15 . 124.6(2) yes N3 . C14 . C15 . 125.4(2) yes C14 . C15 . C16 . 126.7(2) yes C14 . C15 . H151 . 115.8 no C16 . C15 . H151 . 117.6 no C15 . C16 . N4 . 125.7(2) yes C15 . C16 . C17 . 124.4(2) yes N4 . C16 . C17 . 109.8(2) yes C16 . C17 . C18 . 106.7(2) yes C16 . C17 . H171 . 126.6 no C18 . C17 . H171 . 126.7 no C17 . C18 . C19 . 107.1(2) yes C17 . C18 . H181 . 127.5 no C19 . C18 . H181 . 125.4 no C18 . C19 . N4 . 109.7(2) yes C18 . C19 . C20 . 124.8(2) yes N4 . C19 . C20 . 125.4(2) yes C19 . C20 . C1 . 124.7(2) yes C19 . C20 . C31 . 116.4(2) yes C1 . C20 . C31 . 119.0(2) yes N5 . C21 . C22 . 121.9(3) yes N5 . C21 . H211 . 119.0 no C22 . C21 . H211 . 119.1 no C21 . C22 . C23 . 120.3(3) yes C21 . C22 . H221 . 118.7 no C23 . C22 . H221 . 121.0 no C22 . C23 . C24 . 118.3(3) yes C22 . C23 . H231 . 121.1 no C24 . C23 . H231 . 120.6 no C23 . C24 . C25 . 119.1(3) yes C23 . C24 . H241 . 120.5 no C25 . C24 . H241 . 120.4 no C24 . C25 . N5 . 123.1(3) yes C24 . C25 . H251 . 120.5 no N5 . C25 . H251 . 116.4 no C20 . C31 . C32 . 121.7(2) yes C20 . C31 . C36 . 120.3(2) yes C32 . C31 . C36 . 117.9(2) yes C31 . C32 . C33 . 121.3(3) yes C31 . C32 . H321 . 117.9 no C33 . C32 . H321 . 120.8 no C32 . C33 . C34 . 119.9(3) yes C32 . C33 . H331 . 118.9 no C34 . C33 . H331 . 121.2 no C33 . C34 . C35 . 120.3(3) yes C33 . C34 . H341 . 120.1 no C35 . C34 . H341 . 119.6 no C34 . C35 . C36 . 120.2(3) yes C34 . C35 . H351 . 120.4 no C36 . C35 . H351 . 119.4 no C31 . C36 . C35 . 120.5(3) yes C31 . C36 . S1 . 119.96(19) yes C35 . C36 . S1 . 119.5(2) yes C10 . C41 . C42 . 119.4(2) yes C10 . C41 . C46 . 122.2(2) yes C42 . C41 . C46 . 118.3(2) yes C41 . C42 . C43 . 121.7(3) yes C41 . C42 . H421 . 118.7 no C43 . C42 . H421 . 119.5 no C42 . C43 . C44 . 119.1(3) yes C42 . C43 . H431 . 119.3 no C44 . C43 . H431 . 121.5 no C43 . C44 . C45 . 120.4(3) yes C43 . C44 . H441 . 119.3 no C45 . C44 . H441 . 120.3 no C44 . C45 . C46 . 120.2(3) yes C44 . C45 . H451 . 121.4 no C46 . C45 . H451 . 118.3 no C41 . C46 . C45 . 120.2(3) yes C41 . C46 . S2 . 119.9(2) yes C45 . C46 . S2 . 119.9(2) yes C36 . S1 . C51 . 102.37(13) yes C46 . S2 . C59 . 104.89(13) yes S1 . C51 . O1 . 122.8(2) yes S1 . C51 . C52 . 112.1(2) yes O1 . C51 . C52 . 125.0(3) yes C51 . C52 . C53 . 109.5(2) yes C51 . C52 . H521 . 109.4 no C53 . C52 . H521 . 108.3 no C51 . C52 . H522 . 109.8 no C53 . C52 . H522 . 110.4 no H521 . C52 . H522 . 109.3 no C52 . C53 . C54 . 114.3(2) yes C52 . C53 . H531 . 108.4 no C54 . C53 . H531 . 110.3 no C52 . C53 . H532 . 109.1 no C54 . C53 . H532 . 108.5 no H531 . C53 . H532 . 105.8 no C53 . C54 . C55 . 110.7(2) yes C53 . C54 . H541 . 107.2 no C55 . C54 . H541 . 111.6 no C53 . C54 . H542 . 107.8 no C55 . C54 . H542 . 110.8 no H541 . C54 . H542 . 108.6 no C54 . C55 . C56 . 115.0(2) yes C54 . C55 . H551 . 108.6 no C56 . C55 . H551 . 108.8 no C54 . C55 . H552 . 109.7 no C56 . C55 . H552 . 106.4 no H551 . C55 . H552 . 108.2 no C55 . C56 . C57 . 110.1(2) yes C55 . C56 . H561 . 109.2 no C57 . C56 . H561 . 111.3 no C55 . C56 . H562 . 109.2 no C57 . C56 . H562 . 109.1 no H561 . C56 . H562 . 107.9 no C56 . C57 . C58 . 115.1(2) yes C56 . C57 . H571 . 108.6 no C58 . C57 . H571 . 109.4 no C56 . C57 . H572 . 108.1 no C58 . C57 . H572 . 106.3 no H571 . C57 . H572 . 109.1 no C57 . C58 . C59 . 108.4(2) yes C57 . C58 . H581 . 110.9 no C59 . C58 . H581 . 109.2 no C57 . C58 . H582 . 110.1 no C59 . C58 . H582 . 107.7 no H581 . C58 . H582 . 110.5 no C58 . C59 . S2 . 110.4(2) yes C58 . C59 . O2 . 125.6(3) yes S2 . C59 . O2 . 123.9(2) yes N101 . Zn101 . N102 . 90.64(9) yes N101 . Zn101 . N103 . 161.83(9) yes N102 . Zn101 . N103 . 87.24(9) yes N101 . Zn101 . N104 . 87.10(8) yes N102 . Zn101 . N104 . 161.54(8) yes N103 . Zn101 . N104 . 89.21(9) yes N101 . Zn101 . N105 . 103.67(9) yes N102 . Zn101 . N105 . 103.18(9) yes N103 . Zn101 . N105 . 94.37(8) yes N104 . Zn101 . N105 . 95.15(8) yes Zn101 . N101 . C101 . 128.65(18) yes Zn101 . N101 . C104 . 124.77(18) yes C101 . N101 . C104 . 106.5(2) yes Zn101 . N102 . C106 . 124.74(18) yes Zn101 . N102 . C109 . 128.40(17) yes C106 . N102 . C109 . 106.7(2) yes Zn101 . N103 . C111 . 128.02(17) yes Zn101 . N103 . C114 . 124.74(18) yes C111 . N103 . C114 . 106.7(2) yes Zn101 . N104 . C116 . 124.74(17) yes Zn101 . N104 . C119 . 127.89(18) yes C116 . N104 . C119 . 106.7(2) yes Zn101 . N105 . C121 . 119.57(18) yes Zn101 . N105 . C125 . 120.04(18) yes C121 . N105 . C125 . 118.5(2) yes N101 . C101 . C102 . 109.6(2) yes N101 . C101 . C120 . 124.8(2) yes C102 . C101 . C120 . 125.5(2) yes C101 . C102 . C103 . 106.7(2) yes C101 . C102 . H1021 . 126.7 no C103 . C102 . H1021 . 126.6 no C102 . C103 . C104 . 107.5(3) yes C102 . C103 . H1031 . 126.6 no C104 . C103 . H1031 . 125.8 no C103 . C104 . N101 . 109.7(2) yes C103 . C104 . C105 . 124.8(3) yes N101 . C104 . C105 . 125.4(3) yes C104 . C105 . C106 . 126.8(3) yes C104 . C105 . H1051 . 117.4 no C106 . C105 . H1051 . 115.7 no C105 . C106 . N102 . 125.6(2) yes C105 . C106 . C107 . 124.2(2) yes N102 . C106 . C107 . 110.1(2) yes C106 . C107 . C108 . 106.6(2) yes C106 . C107 . H1071 . 125.0 no C108 . C107 . H1071 . 128.4 no C107 . C108 . C109 . 107.4(2) yes C107 . C108 . H1081 . 126.6 no C109 . C108 . H1081 . 126.0 no C108 . C109 . N102 . 109.2(2) yes C108 . C109 . C110 . 125.8(2) yes N102 . C109 . C110 . 125.0(2) yes C109 . C110 . C111 . 125.6(2) yes C109 . C110 . C141 . 117.5(2) yes C111 . C110 . C141 . 116.8(2) yes C110 . C111 . N103 . 124.7(2) yes C110 . C111 . C112 . 126.0(2) yes N103 . C111 . C112 . 109.3(2) yes C111 . C112 . C113 . 107.4(2) yes C111 . C112 . H1121 . 125.6 no C113 . C112 . H1121 . 127.1 no C112 . C113 . C114 . 106.9(2) yes C112 . C113 . H1131 . 127.5 no C114 . C113 . H1131 . 125.6 no C113 . C114 . N103 . 109.7(2) yes C113 . C114 . C115 . 125.3(2) yes N103 . C114 . C115 . 125.0(2) yes C114 . C115 . C116 . 128.1(2) yes C114 . C115 . H1151 . 114.7 no C116 . C115 . H1151 . 117.0 no C115 . C116 . N104 . 124.7(2) yes C115 . C116 . C117 . 125.3(2) yes N104 . C116 . C117 . 109.9(2) yes C116 . C117 . C118 . 106.9(2) yes C116 . C117 . H1171 . 125.7 no C118 . C117 . H1171 . 127.4 no C117 . C118 . C119 . 107.0(2) yes C117 . C118 . H1181 . 125.9 no C119 . C118 . H1181 . 127.0 no C118 . C119 . N104 . 109.4(2) yes C118 . C119 . C120 . 125.5(2) yes N104 . C119 . C120 . 125.1(2) yes C101 . C120 . C119 . 125.4(2) yes C101 . C120 . C131 . 116.2(2) yes C119 . C120 . C131 . 118.3(2) yes N105 . C121 . C122 . 122.0(3) yes N105 . C121 . H1211 . 118.2 no C122 . C121 . H1211 . 119.8 no C121 . C122 . C123 . 118.5(3) yes C121 . C122 . H1221 . 120.3 no C123 . C122 . H1221 . 121.1 no C122 . C123 . C124 . 119.8(3) yes C122 . C123 . H1231 . 120.0 no C124 . C123 . H1231 . 120.2 no C123 . C124 . C125 . 118.3(3) yes C123 . C124 . H1241 . 122.5 no C125 . C124 . H1241 . 119.3 no C124 . C125 . N105 . 122.8(3) yes C124 . C125 . H1251 . 119.8 no N105 . C125 . H1251 . 117.3 no C120 . C131 . C132 . 120.1(3) yes C120 . C131 . C136 . 121.6(3) yes C132 . C131 . C136 . 118.2(3) yes C131 . C132 . C133 . 121.1(3) yes C131 . C132 . H1321 . 120.1 no C133 . C132 . H1321 . 118.8 no C132 . C133 . C134 . 119.7(3) yes C132 . C133 . H1331 . 120.0 no C134 . C133 . H1331 . 120.3 no C133 . C134 . C135 . 120.4(3) yes C133 . C134 . H1341 . 119.7 no C135 . C134 . H1341 . 119.9 no C134 . C135 . C136 . 120.0(3) yes C134 . C135 . H1351 . 121.0 no C136 . C135 . H1351 . 119.0 no C131 . C136 . C135 . 120.7(3) yes C131 . C136 . S101 . 120.0(2) yes C135 . C136 . S101 . 119.3(2) yes C110 . C141 . C142 . 119.4(2) yes C110 . C141 . C146 . 122.7(2) yes C142 . C141 . C146 . 117.9(3) yes C141 . C142 . C143 . 121.1(3) yes C141 . C142 . H1421 . 119.5 no C143 . C142 . H1421 . 119.4 no C142 . C143 . C144 . 119.8(3) yes C142 . C143 . H1431 . 118.1 no C144 . C143 . H1431 . 122.1 no C143 . C144 . C145 . 120.4(3) yes C143 . C144 . H1441 . 120.2 no C145 . C144 . H1441 . 119.4 no C144 . C145 . C146 . 120.4(3) yes C144 . C145 . H1451 . 120.9 no C146 . C145 . H1451 . 118.7 no C141 . C146 . C145 . 120.5(3) yes C141 . C146 . S102 . 120.2(2) yes C145 . C146 . S102 . 119.3(2) yes C136 . S101 . C151 . 99.91(14) yes C146 . S102 . C159 . 100.86(14) yes S101 . C151 . O101 . 121.6(2) yes S101 . C151 . C152 . 112.7(2) yes O101 . C151 . C152 . 125.5(3) yes C151 . C152 . C153 . 107.6(3) yes C151 . C152 . H1521 . 110.1 no C153 . C152 . H1521 . 110.3 no C151 . C152 . H1522 . 109.0 no C153 . C152 . H1522 . 108.8 no H1521 . C152 . H1522 . 110.9 no C152 . C153 . C154 . 113.8(3) yes C152 . C153 . H1531 . 107.3 no C154 . C153 . H1531 . 109.0 no C152 . C153 . H1532 . 110.9 no C154 . C153 . H1532 . 108.2 no H1531 . C153 . H1532 . 107.4 no C153 . C154 . C155 . 110.8(3) yes C153 . C154 . H1541 . 109.1 no C155 . C154 . H1541 . 108.6 no C153 . C154 . H1542 . 108.9 no C155 . C154 . H1542 . 109.1 no H1541 . C154 . H1542 . 110.3 no C154 . C155 . C156 . 115.0(3) yes C154 . C155 . H1551 . 106.8 no C156 . C155 . H1551 . 106.4 no C154 . C155 . H1552 . 109.1 no C156 . C155 . H1552 . 110.4 no H1551 . C155 . H1552 . 109.0 no C155 . C156 . C157 . 112.9(3) yes C155 . C156 . H1561 . 109.1 no C157 . C156 . H1561 . 108.9 no C155 . C156 . H1562 . 110.0 no C157 . C156 . H1562 . 108.5 no H1561 . C156 . H1562 . 107.3 no C156 . C157 . C158 . 114.2(3) yes C156 . C157 . H1571 . 109.9 no C158 . C157 . H1571 . 108.2 no C156 . C157 . H1572 . 107.6 no C158 . C157 . H1572 . 108.4 no H1571 . C157 . H1572 . 108.4 no C157 . C158 . C159 . 111.0(3) yes C157 . C158 . H1581 . 109.7 no C159 . C158 . H1581 . 107.1 no C157 . C158 . H1582 . 110.3 no C159 . C158 . H1582 . 108.1 no H1581 . C158 . H1582 . 110.5 no C158 . C159 . S102 . 110.9(2) yes C158 . C159 . O102 . 125.7(3) yes S102 . C159 . O102 . 123.3(2) 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 C13 . H131 . O101 2_655 145 0.91 2.52 3.304(4) yes C15 . H151 . O102 . 147 0.92 2.49 3.303(4) yes C17 . H171 . O102 . 136 0.92 2.59 3.309(4) yes C107 . H1071 . O1 . 173 0.91 2.48 3.384(4) yes C117 . H1171 . O2 4_654 154 0.91 2.57 3.417(4) yes C123 . H1231 . N103 3_455 147 0.94 2.47 3.298(4) yes C145 . H1451 . O101 2_655 144 0.93 2.60 3.390(4) yes _iucr_refine_instructions_details ; # # Punched on 25/01/17 at 11:57:28 # #LIST 12 BLOCK SCALE X'S U'S CONT ENANTIO RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 15,X'S) H ( 151,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 33,X'S) H ( 331,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 43,X'S) H ( 431,X'S) RIDE C ( 44,X'S) H ( 441,X'S) RIDE C ( 45,X'S) H ( 451,X'S) RIDE C ( 52,X'S) H ( 521,X'S) H ( 522,X'S) RIDE C ( 53,X'S) H ( 531,X'S) H ( 532,X'S) RIDE C ( 54,X'S) H ( 541,X'S) H ( 542,X'S) RIDE C ( 55,X'S) H ( 551,X'S) H ( 552,X'S) RIDE C ( 56,X'S) H ( 561,X'S) H ( 562,X'S) RIDE C ( 57,X'S) H ( 571,X'S) H ( 572,X'S) RIDE C ( 58,X'S) H ( 581,X'S) H ( 582,X'S) RIDE C ( 102,X'S) H (1021,X'S) RIDE C ( 103,X'S) H (1031,X'S) RIDE C ( 105,X'S) H (1051,X'S) RIDE C ( 107,X'S) H (1071,X'S) RIDE C ( 108,X'S) H (1081,X'S) RIDE C ( 112,X'S) H (1121,X'S) RIDE C ( 113,X'S) H (1131,X'S) RIDE C ( 115,X'S) H (1151,X'S) RIDE C ( 117,X'S) H (1171,X'S) RIDE C ( 118,X'S) H (1181,X'S) RIDE C ( 121,X'S) H (1211,X'S) RIDE C ( 122,X'S) H (1221,X'S) RIDE C ( 123,X'S) H (1231,X'S) RIDE C ( 124,X'S) H (1241,X'S) RIDE C ( 125,X'S) H (1251,X'S) RIDE C ( 132,X'S) H (1321,X'S) RIDE C ( 133,X'S) H (1331,X'S) RIDE C ( 134,X'S) H (1341,X'S) RIDE C ( 135,X'S) H (1351,X'S) RIDE C ( 142,X'S) H (1421,X'S) RIDE C ( 143,X'S) H (1431,X'S) RIDE C ( 144,X'S) H (1441,X'S) RIDE C ( 145,X'S) H (1451,X'S) RIDE C ( 152,X'S) H (1521,X'S) H (1522,X'S) RIDE C ( 153,X'S) H (1531,X'S) H (1532,X'S) RIDE C ( 154,X'S) H (1541,X'S) H (1542,X'S) RIDE C ( 155,X'S) H (1551,X'S) H (1552,X'S) RIDE C ( 156,X'S) H (1561,X'S) H (1562,X'S) RIDE C ( 157,X'S) H (1571,X'S) H (1572,X'S) RIDE C ( 158,X'S) H (1581,X'S) H (1582,X'S) END # # Punched on 25/01/17 at 11:57:28 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; #============================================================================== data_6b #============================================================================== _audit_creation_date "2017-01-24" _audit_creation_method CRYSTALS_ver_14.61_build_6019 _oxford_structure_analysis_title '6543' _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 20.7707(1) _cell_length_b 12.2277(1) _cell_length_c 15.6407(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3972.39(5) _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'P n a 21 ' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,z+1/2' '-x+1/2,y+1/2,z+1/2' 'x+1/2,-y+1/2,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 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0311 0.0180 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 0.0492 0.0322 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' Zn -1.5491 0.6778 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' S 0.3331 0.5567 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 = C46.75 H42.50 N4.25 O4.25 S2 Zn1 # Dc = 1.44 Fooo = 1795.00 Mu = 22.64 M = 861.39 # Found Formula = C47 H39 N5 O2 S2 Zn1 # Dc = 1.40 FOOO = 1736.00 Mu = 22.11 M = 835.37 _chemical_formula_sum 'C47 H39 N5 O2 S2 Zn1' _chemical_formula_moiety 'C47 H39 N5 O2 S2 Zn1' _chemical_compound_source . _chemical_formula_weight 835.37 _cell_measurement_reflns_used 23853 _cell_measurement_theta_min 4 _cell_measurement_theta_max 76 _cell_measurement_temperature 150 _exptl_crystal_description 'plate' _exptl_crystal_colour 'metallic_dark_purple' _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_max 0.10 _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 2.211 # Sheldrick geometric approximatio 0.84 0.96 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro, (Agilent, 2011)' _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.96 _diffrn_measurement_device_type 'Oxford Diffraction SuperNova' _diffrn_measurement_device 'Area' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54180 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlisPro, (Agilent, 2011)' _computing_data_reduction 'CrysAlisPro, (Agilent, 2011)' _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 150 _diffrn_reflns_number 44155 _reflns_number_total 7913 _diffrn_reflns_av_R_equivalents 0.029 # Number of reflections without Friedels Law is 7913 # Number of reflections with Friedels Law is 4300 # Theoretical number of reflections is about 4154 _diffrn_reflns_theta_min 4.195 _diffrn_reflns_theta_max 76.122 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 76.122 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min 0 _reflns_limit_h_max 25 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min -19 _reflns_limit_l_max 19 _oxford_diffrn_Wilson_B_factor 2.89 _oxford_diffrn_Wilson_scale 0.03 _atom_sites_solution_primary Other #heavy,direct,difmap,geom,iterative # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.19 _refine_diff_density_max 0.25 # 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>-3.0\s(I) _refine_ls_number_reflns 7885 _refine_ls_number_restraints 473 _refine_ls_number_parameters 585 _oxford_refine_ls_R_factor_ref 0.0269 _refine_ls_wR_factor_ref 0.0678 _refine_ls_goodness_of_fit_ref 1.0008 _refine_ls_shift/su_max 0.0034301 _refine_ls_shift/su_mean 0.0001889 # The values computed with all filters except I/sigma _oxford_reflns_number_all 7885 _refine_ls_R_factor_all 0.0269 _refine_ls_wR_factor_all 0.0678 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 7569 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_gt 0.0652 _refine_ls_abs_structure_Flack -0.012(11) _refine_ls_abs_structure_details 'Flack (1983), 3613 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 #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^) + ( 0.04P)^2^ + 0.87P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # 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. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Agilent (2011). CrysAlisPro. Oxford Diffraction, (2010). Supernova User Manual. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. 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 atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Zn1 Zn 0.423299(10) 0.521349(17) 0.40244(4) 0.0315 1.0000 Uani . . . . . . N1 N 0.42901(7) 0.64932(13) 0.31594(11) 0.0341 1.0000 Uani . . . . . . N2 N 0.36070(7) 0.43920(13) 0.32137(11) 0.0339 1.0000 Uani . . . . . . N3 N 0.43830(7) 0.37334(13) 0.46346(11) 0.0345 1.0000 Uani . . . . . . N4 N 0.50678(7) 0.58151(12) 0.45674(12) 0.0351 1.0000 Uani . . . . . . N5 N 0.34936(7) 0.59571(13) 0.47909(11) 0.0340 1.0000 Uani . . . . . . C1 C 0.46452(9) 0.74289(16) 0.32351(14) 0.0373 1.0000 Uani . . . . . . C2 C 0.44227(10) 0.82320(18) 0.26236(15) 0.0431 1.0000 Uani . . . . . . C3 C 0.39374(10) 0.77647(18) 0.21775(15) 0.0436 1.0000 Uani . . . . . . C4 C 0.38519(9) 0.66691(17) 0.25192(13) 0.0375 1.0000 Uani . . . . . . C5 C 0.33957(9) 0.59207(17) 0.22423(13) 0.0384 1.0000 Uani . . . . . . C6 C 0.32831(9) 0.48699(17) 0.25564(13) 0.0359 1.0000 Uani . . . . . . C7 C 0.27948(10) 0.41369(18) 0.22429(13) 0.0413 1.0000 Uani . . . . . . C8 C 0.28231(9) 0.32223(18) 0.27262(14) 0.0409 1.0000 Uani . . . . . . C9 C 0.33372(9) 0.33824(16) 0.33383(13) 0.0360 1.0000 Uani . . . . . . C10 C 0.35264(8) 0.26350(14) 0.39689(15) 0.0371 1.0000 Uani . . . . . . C11 C 0.40290(9) 0.27965(15) 0.45506(14) 0.0369 1.0000 Uani . . . . . . C12 C 0.42595(10) 0.19879(17) 0.51483(17) 0.0449 1.0000 Uani . . . . . . C13 C 0.47512(11) 0.24464(18) 0.55813(16) 0.0463 1.0000 Uani . . . . . . C14 C 0.48253(9) 0.35434(15) 0.52562(15) 0.0388 1.0000 Uani . . . . . . C15 C 0.52927(10) 0.42845(17) 0.55328(15) 0.0412 1.0000 Uani . . . . . . C16 C 0.54099(9) 0.53199(15) 0.52056(15) 0.0377 1.0000 Uani . . . . . . C17 C 0.59309(9) 0.60293(17) 0.54737(15) 0.0426 1.0000 Uani . . . . . . C18 C 0.59000(9) 0.69293(17) 0.49861(15) 0.0415 1.0000 Uani . . . . . . C19 C 0.53551(9) 0.68013(16) 0.44152(14) 0.0367 1.0000 Uani . . . . . . C20 C 0.51522(9) 0.75781(16) 0.38203(14) 0.0381 1.0000 Uani . . . . . . C21 C 0.35996(10) 0.68984(18) 0.51976(16) 0.0454 1.0000 Uani . . . . . . C22 C 0.31303(13) 0.7435(2) 0.56474(19) 0.0609 1.0000 Uani . . . . . . C23 C 0.25214(12) 0.6979(3) 0.56943(18) 0.0618 1.0000 Uani . . . . . . C24 C 0.24051(10) 0.6012(2) 0.52687(18) 0.0570 1.0000 Uani . . . . . . C25 C 0.29014(10) 0.55321(18) 0.48233(16) 0.0452 1.0000 Uani . . . . . . C31 C 0.55093(9) 0.86443(17) 0.38022(15) 0.0421 1.0000 Uani . . . . . . C32 C 0.59425(11) 0.8853(2) 0.31417(17) 0.0516 1.0000 Uani . . . . . . C33 C 0.63095(13) 0.9802(2) 0.31378(18) 0.0577 1.0000 Uani . . . . . . C34 C 0.62428(12) 1.05621(19) 0.37771(17) 0.0543 1.0000 Uani . . . . . . C35 C 0.58030(11) 1.03876(18) 0.44306(19) 0.0505 1.0000 Uani . . . . . . C36 C 0.54428(10) 0.94239(17) 0.44446(17) 0.0446 1.0000 Uani . . . . . . C41 C 0.31574(9) 0.15808(15) 0.40500(16) 0.0401 1.0000 Uani . . . . . . C42 C 0.33358(13) 0.0652(2) 0.3603(2) 0.0610 1.0000 Uani . . . . . . C43 C 0.30151(15) -0.0335(2) 0.3715(2) 0.0649 1.0000 Uani . . . . . . C44 C 0.24958(13) -0.0395(2) 0.42605(18) 0.0571 1.0000 Uani . . . . . . C45 C 0.23003(12) 0.0514(2) 0.47014(16) 0.0500 1.0000 Uani . . . . . . C46 C 0.26360(10) 0.14969(17) 0.46099(14) 0.0403 1.0000 Uani . . . . . . S1 S 0.48573(19) 0.9214(4) 0.51891(19) 0.0432 0.581(5) Uani D . P 1 1 . S2 S 0.24042(3) 0.26447(4) 0.52275(5) 0.0482 1.0000 Uani D . . . . . O1 O 0.5872(2) 0.9395(5) 0.6214(3) 0.0595 0.581(5) Uani D . P 1 1 . O2 O 0.30989(9) 0.15191(19) 0.63464(11) 0.0694 1.0000 Uani D . . . . . C51 C 0.52999(16) 0.9179(3) 0.6167(2) 0.0470 0.581(5) Uani D . P 1 1 . C52 C 0.49273(19) 0.8745(3) 0.6910(2) 0.0515 0.581(5) Uani D . P 1 1 . C53 C 0.5154(2) 0.7587(3) 0.7163(3) 0.0546 0.581(5) Uani D . P 1 1 . C54 C 0.4802(3) 0.7162(4) 0.7953(3) 0.0611 0.581(5) Uani D . P 1 1 . C55 C 0.4137(2) 0.6713(4) 0.7762(4) 0.0694 0.581(5) Uani D . P 1 1 . C56 C 0.4148(2) 0.5589(7) 0.7294(7) 0.0629 0.581(5) Uani D . P 1 1 . C57 C 0.34832(14) 0.5037(4) 0.7241(4) 0.0620 0.581(5) Uani D . P 1 1 . C58 C 0.34924(10) 0.3919(2) 0.67514(16) 0.0615 1.0000 Uani D . . . . . C59 C 0.28489(10) 0.3336(2) 0.67964(14) 0.0764 1.0000 Uani D . . . . . C60 C 0.28247(9) 0.23822(14) 0.61961(10) 0.0604 1.0000 Uani D . . . . . S11 S 0.4921(3) 0.9156(5) 0.5430(3) 0.0445 0.419(5) Uani D . P 1 2 . O11 O 0.6068(3) 0.9230(7) 0.6165(5) 0.0595 0.419(5) Uani D . P 1 2 . C61 C 0.5514(2) 0.8983(4) 0.6254(3) 0.0470 0.419(5) Uani D . P 1 2 . C62 C 0.5237(3) 0.8656(4) 0.7122(3) 0.0612 0.419(5) Uani D . P 1 2 . C63 C 0.4764(3) 0.7700(4) 0.7046(2) 0.0474 0.419(5) Uani D . P 1 2 . C64 C 0.4713(3) 0.7054(5) 0.7887(3) 0.0546 0.419(5) Uani D . P 1 2 . C65 C 0.4134(3) 0.6388(5) 0.7949(3) 0.0535 0.419(5) Uani D . P 1 2 . C66 C 0.4125(4) 0.5439(9) 0.7340(7) 0.0541 0.419(5) Uani D . P 1 2 . C67 C 0.3566(2) 0.4727(6) 0.7445(4) 0.0635 0.419(5) Uani D . P 1 2 . H21 H 0.4577 0.8926 0.2567 0.0518 1.0000 Uiso R . . . . . H31 H 0.3696 0.8071 0.1748 0.0518 1.0000 Uiso R . . . . . H51 H 0.3134 0.6114 0.1782 0.0447 1.0000 Uiso R . . . . . H71 H 0.2515 0.4258 0.1804 0.0501 1.0000 Uiso R . . . . . H81 H 0.2577 0.2580 0.2684 0.0475 1.0000 Uiso R . . . . . H121 H 0.4083 0.1274 0.5211 0.0537 1.0000 Uiso R . . . . . H131 H 0.4987 0.2129 0.6016 0.0571 1.0000 Uiso R . . . . . H151 H 0.5556 0.4045 0.5977 0.0483 1.0000 Uiso R . . . . . H171 H 0.6228 0.5861 0.5907 0.0500 1.0000 Uiso R . . . . . H181 H 0.6181 0.7526 0.4994 0.0490 1.0000 Uiso R . . . . . H211 H 0.4016 0.7191 0.5155 0.0550 1.0000 Uiso R . . . . . H221 H 0.3232 0.8079 0.5931 0.0736 1.0000 Uiso R . . . . . H231 H 0.2194 0.7310 0.6020 0.0731 1.0000 Uiso R . . . . . H241 H 0.2009 0.5653 0.5305 0.0680 1.0000 Uiso R . . . . . H251 H 0.2833 0.4860 0.4531 0.0536 1.0000 Uiso R . . . . . H321 H 0.6002 0.8327 0.2717 0.0608 1.0000 Uiso R . . . . . H331 H 0.6604 0.9920 0.2692 0.0699 1.0000 Uiso R . . . . . H341 H 0.6488 1.1189 0.3778 0.0641 1.0000 Uiso R . . . . . H351 H 0.5745 1.0903 0.4874 0.0606 1.0000 Uiso R . . . . . H421 H 0.3674 0.0694 0.3213 0.0728 1.0000 Uiso R . . . . . H431 H 0.3168 -0.0951 0.3417 0.0786 1.0000 Uiso R . . . . . H441 H 0.2274 -0.1050 0.4329 0.0680 1.0000 Uiso R . . . . . H451 H 0.1945 0.0490 0.5073 0.0594 1.0000 Uiso R . . . . . H521 H 0.4998 0.9217 0.7406 0.0623 0.581(5) Uiso R . P 1 1 . H522 H 0.4477 0.8740 0.6760 0.0612 0.581(5) Uiso R . P 1 1 . H531 H 0.5612 0.7657 0.7308 0.0642 0.581(5) Uiso R . P 1 1 . H532 H 0.5097 0.7075 0.6695 0.0650 0.581(5) Uiso R . P 1 1 . H541 H 0.4775 0.7777 0.8370 0.0731 0.581(5) Uiso R . P 1 1 . H542 H 0.5067 0.6549 0.8193 0.0731 0.581(5) Uiso R . P 1 1 . H551 H 0.3923 0.6581 0.8317 0.0827 0.581(5) Uiso R . P 1 1 . H552 H 0.3885 0.7252 0.7417 0.0831 0.581(5) Uiso R . P 1 1 . H561 H 0.4449 0.5110 0.7595 0.0747 0.581(5) Uiso R . P 1 1 . H562 H 0.4329 0.5696 0.6723 0.0748 0.581(5) Uiso R . P 1 1 . H571 H 0.3331 0.4885 0.7830 0.0739 0.581(5) Uiso R . P 1 1 . H572 H 0.3181 0.5541 0.6969 0.0734 0.581(5) Uiso R . P 1 1 . H583 H 0.3827 0.3462 0.7010 0.0737 0.581(5) Uiso R . P 1 1 . H582 H 0.3596 0.4041 0.6146 0.0733 0.581(5) Uiso R . P 1 1 . H581 H 0.3836 0.3381 0.6818 0.0738 0.419(5) Uiso R . P 1 2 . H584 H 0.3538 0.4258 0.6188 0.0737 0.419(5) Uiso R . P 1 2 . H591 H 0.2794 0.3041 0.7371 0.0915 1.0000 Uiso R . . . . . H592 H 0.2505 0.3872 0.6648 0.0910 1.0000 Uiso R . . . . . H621 H 0.5590 0.8404 0.7462 0.0732 0.419(5) Uiso R . P 1 2 . H622 H 0.5034 0.9272 0.7402 0.0731 0.419(5) Uiso R . P 1 2 . H631 H 0.4892 0.7201 0.6597 0.0570 0.419(5) Uiso R . P 1 2 . H632 H 0.4346 0.7995 0.6904 0.0570 0.419(5) Uiso R . P 1 2 . H641 H 0.4723 0.7590 0.8371 0.0654 0.419(5) Uiso R . P 1 2 . H642 H 0.5091 0.6559 0.7920 0.0652 0.419(5) Uiso R . P 1 2 . H651 H 0.4121 0.6095 0.8523 0.0641 0.419(5) Uiso R . P 1 2 . H652 H 0.3741 0.6842 0.7849 0.0641 0.419(5) Uiso R . P 1 2 . H661 H 0.4511 0.5006 0.7448 0.0647 0.419(5) Uiso R . P 1 2 . H662 H 0.4157 0.5713 0.6756 0.0653 0.419(5) Uiso R . P 1 2 . H671 H 0.3588 0.4353 0.7995 0.0758 0.419(5) Uiso R . P 1 2 . H672 H 0.3181 0.5189 0.7435 0.0760 0.419(5) Uiso R . P 1 2 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02802(10) 0.03193(10) 0.03445(11) -0.00103(11) -0.00036(11) -0.00005(8) N1 0.0312(7) 0.0356(8) 0.0355(8) 0.0001(6) 0.0003(6) 0.0000(6) N2 0.0318(7) 0.0357(8) 0.0342(8) -0.0071(6) 0.0010(6) 0.0001(6) N3 0.0327(7) 0.0325(7) 0.0383(8) 0.0006(6) 0.0008(6) 0.0000(6) N4 0.0296(7) 0.0327(7) 0.0431(9) -0.0017(6) -0.0033(6) 0.0011(6) N5 0.0321(7) 0.0350(8) 0.0349(8) -0.0033(6) 0.0007(6) 0.0038(6) C1 0.0326(8) 0.0354(9) 0.0440(10) 0.0035(8) 0.0040(8) -0.0001(7) C2 0.0415(10) 0.0400(10) 0.0480(11) 0.0081(9) 0.0037(9) -0.0005(8) C3 0.0422(10) 0.0461(11) 0.0424(11) 0.0088(9) 0.0002(8) 0.0035(8) C4 0.0368(9) 0.0420(10) 0.0336(9) 0.0031(8) 0.0017(7) 0.0040(8) C5 0.0354(9) 0.0480(11) 0.0318(9) -0.0017(8) -0.0020(7) 0.0047(7) C6 0.0306(8) 0.0447(10) 0.0325(9) -0.0078(8) 0.0007(7) 0.0024(7) C7 0.0345(9) 0.0528(11) 0.0365(10) -0.0112(9) -0.0017(8) 0.0002(8) C8 0.0351(9) 0.0458(10) 0.0417(11) -0.0133(8) 0.0045(8) -0.0076(8) C9 0.0332(8) 0.0382(9) 0.0367(9) -0.0117(8) 0.0072(7) -0.0025(7) C10 0.0345(8) 0.0367(8) 0.0402(9) -0.0086(9) 0.0102(8) -0.0022(6) C11 0.0360(9) 0.0326(9) 0.0421(10) -0.0014(7) 0.0079(8) 0.0000(7) C12 0.0419(10) 0.0352(9) 0.0576(13) 0.0071(9) 0.0046(9) -0.0010(7) C13 0.0428(11) 0.0406(10) 0.0553(13) 0.0096(9) -0.0024(9) 0.0037(8) C14 0.0369(9) 0.0363(9) 0.0433(10) 0.0049(8) 0.0001(8) 0.0037(7) C15 0.0350(9) 0.0420(10) 0.0466(11) 0.0045(8) -0.0085(8) 0.0041(8) C16 0.0306(8) 0.0372(9) 0.0453(10) -0.0024(8) -0.0046(8) 0.0047(7) C17 0.0312(9) 0.0420(10) 0.0545(12) -0.0057(9) -0.0096(8) 0.0038(7) C18 0.0304(8) 0.0373(9) 0.0567(13) -0.0059(8) -0.0063(8) -0.0004(7) C19 0.0274(8) 0.0359(9) 0.0467(10) -0.0030(8) -0.0003(7) -0.0007(7) C20 0.0300(8) 0.0363(9) 0.0480(12) -0.0012(8) 0.0023(7) 0.0000(7) C21 0.0413(10) 0.0461(10) 0.0487(12) -0.0138(10) -0.0049(9) 0.0023(8) C22 0.0519(13) 0.0627(15) 0.0682(16) -0.0357(13) -0.0102(11) 0.0122(11) C23 0.0426(12) 0.0831(18) 0.0597(15) -0.0325(14) -0.0082(11) 0.0230(11) C24 0.0332(9) 0.0733(15) 0.0645(15) -0.0235(13) 0.0028(10) 0.0039(10) C25 0.0361(9) 0.0437(10) 0.0558(13) -0.0139(9) 0.0049(9) 0.0002(8) C31 0.0314(8) 0.0392(10) 0.0559(14) 0.0072(8) -0.0006(8) -0.0022(7) C32 0.0496(11) 0.0514(12) 0.0538(14) -0.0003(10) 0.0052(10) -0.0103(10) C33 0.0525(13) 0.0623(15) 0.0585(15) 0.0055(12) 0.0083(11) -0.0185(11) C34 0.0487(12) 0.0460(11) 0.0681(17) 0.0117(10) -0.0030(10) -0.0157(9) C35 0.0483(12) 0.0356(10) 0.0675(15) 0.0025(10) 0.0002(10) -0.0038(8) C36 0.0354(9) 0.0338(9) 0.0645(14) 0.0045(9) 0.0039(9) -0.0004(8) C41 0.0394(8) 0.0359(8) 0.0451(10) -0.0058(9) 0.0015(10) -0.0042(7) C42 0.0550(13) 0.0502(13) 0.0777(18) -0.0196(12) 0.0183(12) -0.0082(10) C43 0.0711(17) 0.0394(11) 0.084(2) -0.0215(11) 0.0030(14) -0.0056(11) C44 0.0645(14) 0.0413(11) 0.0656(16) 0.0019(10) -0.0067(12) -0.0183(10) C45 0.0525(12) 0.0494(12) 0.0482(12) 0.0038(10) 0.0012(10) -0.0139(10) C46 0.0437(10) 0.0395(9) 0.0378(10) -0.0005(8) 0.0028(8) -0.0049(8) S1 0.0468(9) 0.0327(7) 0.0501(14) -0.0004(11) 0.0145(10) -0.0001(6) S2 0.0486(3) 0.0498(3) 0.0462(3) -0.0074(2) 0.0145(2) -0.0071(2) O1 0.056(2) 0.066(2) 0.0570(13) -0.0092(13) 0.0099(17) -0.002(2) O2 0.0586(10) 0.1030(15) 0.0466(9) 0.0081(10) 0.0030(8) -0.0219(10) C51 0.050(2) 0.0353(16) 0.0555(14) -0.0094(12) 0.0085(15) -0.0034(15) C52 0.054(2) 0.057(2) 0.044(2) -0.0115(17) -0.0020(18) -0.0176(18) C53 0.048(2) 0.055(2) 0.061(2) -0.0029(18) -0.0101(19) 0.0026(17) C54 0.079(3) 0.047(2) 0.057(3) 0.000(2) -0.019(2) -0.010(2) C55 0.083(3) 0.063(3) 0.062(3) 0.003(2) -0.019(3) -0.009(3) C56 0.064(3) 0.066(3) 0.058(4) 0.002(3) -0.013(3) -0.009(3) C57 0.062(3) 0.085(3) 0.039(2) -0.015(2) -0.004(2) -0.011(2) C58 0.0571(13) 0.0832(16) 0.0441(12) -0.0079(12) 0.0046(10) -0.0132(12) C59 0.0648(15) 0.112(2) 0.0523(14) -0.0269(14) 0.0154(12) -0.0272(15) C60 0.0505(12) 0.0866(15) 0.0441(11) -0.0064(11) 0.0131(9) -0.0214(11) S11 0.0460(12) 0.0374(10) 0.0500(18) 0.0005(15) 0.0139(13) -0.0015(8) O11 0.056(2) 0.066(2) 0.0570(13) -0.0092(13) 0.0099(17) -0.002(2) C61 0.050(2) 0.0353(16) 0.0555(14) -0.0094(12) 0.0085(15) -0.0034(15) C62 0.070(3) 0.064(3) 0.050(3) -0.009(3) -0.015(3) -0.028(3) C63 0.049(3) 0.051(3) 0.042(2) -0.005(2) -0.011(2) -0.005(2) C64 0.067(4) 0.060(4) 0.037(3) -0.009(3) -0.002(3) 0.008(3) C65 0.058(3) 0.068(4) 0.034(3) -0.011(3) 0.000(2) 0.008(3) C66 0.059(4) 0.062(4) 0.041(4) -0.011(3) 0.001(3) 0.006(3) C67 0.059(3) 0.089(4) 0.042(3) -0.007(3) -0.004(3) 0.002(3) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 3.66(2) 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 . N1 . 2.0720(17) yes Zn1 . N2 . 2.0755(16) yes Zn1 . N3 . 2.0696(16) yes Zn1 . N4 . 2.0662(15) yes Zn1 . N5 . 2.1501(15) yes N1 . C1 . 1.366(2) yes N1 . C4 . 1.370(3) yes N2 . C6 . 1.360(3) yes N2 . C9 . 1.370(2) yes N3 . C11 . 1.368(2) yes N3 . C14 . 1.358(3) yes N4 . C16 . 1.367(3) yes N4 . C19 . 1.366(2) yes N5 . C21 . 1.333(3) yes N5 . C25 . 1.336(3) yes C1 . C2 . 1.447(3) yes C1 . C20 . 1.407(3) yes C2 . C3 . 1.353(3) yes C2 . H21 . 0.912 no C3 . C4 . 1.453(3) yes C3 . H31 . 0.918 no C4 . C5 . 1.387(3) yes C5 . C6 . 1.395(3) yes C5 . H51 . 0.934 no C6 . C7 . 1.440(3) yes C7 . C8 . 1.351(3) yes C7 . H71 . 0.911 no C8 . C9 . 1.447(3) yes C8 . H81 . 0.939 no C9 . C10 . 1.401(3) yes C10 . C11 . 1.399(3) yes C10 . C41 . 1.505(2) yes C11 . C12 . 1.443(3) yes C12 . C13 . 1.348(3) yes C12 . H121 . 0.952 no C13 . C14 . 1.443(3) yes C13 . H131 . 0.924 no C14 . C15 . 1.397(3) yes C15 . C16 . 1.387(3) yes C15 . H151 . 0.931 no C16 . C17 . 1.449(3) yes C17 . C18 . 1.340(3) yes C17 . H171 . 0.940 no C18 . C19 . 1.450(3) yes C18 . H181 . 0.934 no C19 . C20 . 1.395(3) yes C20 . C31 . 1.500(3) yes C21 . C22 . 1.369(3) yes C21 . H211 . 0.938 no C22 . C23 . 1.384(4) yes C22 . H221 . 0.929 no C23 . C24 . 1.378(4) yes C23 . H231 . 0.940 no C24 . C25 . 1.376(3) yes C24 . H241 . 0.934 no C25 . H251 . 0.951 no C31 . C32 . 1.394(3) yes C31 . C36 . 1.392(3) yes C32 . C33 . 1.389(3) yes C32 . H321 . 0.932 no C33 . C34 . 1.372(4) yes C33 . H331 . 0.939 no C34 . C35 . 1.387(4) yes C34 . H341 . 0.921 no C35 . C36 . 1.396(3) yes C35 . H351 . 0.944 no C36 . S1 . 1.703(4) yes C36 . S11 . 1.913(5) yes C41 . C42 . 1.384(3) yes C41 . C46 . 1.397(3) yes C42 . C43 . 1.389(4) yes C42 . H421 . 0.931 no C43 . C44 . 1.378(4) yes C43 . H431 . 0.941 no C44 . C45 . 1.370(4) yes C44 . H441 . 0.930 no C45 . C46 . 1.396(3) yes C45 . H451 . 0.940 no C46 . S2 . 1.770(2) yes S1 . C51 . 1.785(4) yes S2 . C60 . 1.7780(18) yes O1 . C51 . 1.219(4) yes O2 . C60 . 1.222(3) yes C51 . C52 . 1.494(4) yes C52 . C53 . 1.543(5) yes C52 . H521 . 0.977 no C52 . H522 . 0.965 no C53 . C54 . 1.527(5) yes C53 . H531 . 0.982 no C53 . H532 . 0.970 no C54 . C55 . 1.515(5) yes C54 . H541 . 0.996 no C54 . H542 . 1.003 no C55 . C56 . 1.557(5) yes C55 . H551 . 0.989 no C55 . H552 . 1.001 no C56 . C57 . 1.539(5) yes C56 . H561 . 0.979 no C56 . H562 . 0.977 no C57 . C58 . 1.567(5) yes C57 . H571 . 0.992 no C57 . H572 . 0.977 no C58 . C59 . 1.517(3) yes C58 . H583 . 0.979 no C58 . H582 . 0.982 no C58 . C59 . 1.517(3) yes C58 . C67 . 1.475(5) yes C58 . H581 . 0.976 no C58 . H584 . 0.979 no C59 . C60 . 1.498(2) yes C59 . H591 . 0.975 no C59 . H592 . 0.997 no S11 . C61 . 1.796(5) yes O11 . C61 . 1.199(5) yes C61 . C62 . 1.527(5) yes C62 . C63 . 1.531(5) yes C62 . H621 . 0.958 no C62 . H622 . 0.969 no C63 . C64 . 1.538(6) yes C63 . H631 . 0.967 no C63 . H632 . 0.966 no C64 . C65 . 1.457(6) yes C64 . H641 . 1.001 no C64 . H642 . 0.993 no C65 . C66 . 1.502(5) yes C65 . H651 . 0.966 no C65 . H652 . 0.999 no C66 . C67 . 1.461(6) yes C66 . H661 . 0.975 no C66 . H662 . 0.975 no C67 . H671 . 0.975 no C67 . H672 . 0.979 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Zn1 . N2 . 90.14(6) yes N1 . Zn1 . N3 . 162.34(6) yes N2 . Zn1 . N3 . 87.30(6) yes N1 . Zn1 . N4 . 87.22(6) yes N2 . Zn1 . N4 . 161.66(6) yes N3 . Zn1 . N4 . 89.74(6) yes N1 . Zn1 . N5 . 94.91(6) yes N2 . Zn1 . N5 . 95.62(6) yes N3 . Zn1 . N5 . 102.72(6) yes N4 . Zn1 . N5 . 102.69(6) yes Zn1 . N1 . C1 . 127.35(14) yes Zn1 . N1 . C4 . 123.89(13) yes C1 . N1 . C4 . 106.89(16) yes Zn1 . N2 . C6 . 124.31(13) yes Zn1 . N2 . C9 . 127.27(14) yes C6 . N2 . C9 . 107.00(16) yes Zn1 . N3 . C11 . 127.39(14) yes Zn1 . N3 . C14 . 125.58(13) yes C11 . N3 . C14 . 106.81(16) yes Zn1 . N4 . C16 . 125.36(13) yes Zn1 . N4 . C19 . 127.53(13) yes C16 . N4 . C19 . 106.93(16) yes Zn1 . N5 . C21 . 120.87(13) yes Zn1 . N5 . C25 . 120.94(13) yes C21 . N5 . C25 . 118.02(17) yes N1 . C1 . C2 . 109.79(18) yes N1 . C1 . C20 . 124.67(18) yes C2 . C1 . C20 . 125.53(18) yes C1 . C2 . C3 . 107.01(19) yes C1 . C2 . H21 . 125.7 no C3 . C2 . H21 . 127.3 no C2 . C3 . C4 . 106.90(19) yes C2 . C3 . H31 . 127.7 no C4 . C3 . H31 . 125.4 no C3 . C4 . N1 . 109.41(18) yes C3 . C4 . C5 . 125.24(19) yes N1 . C4 . C5 . 125.35(18) yes C4 . C5 . C6 . 127.76(19) yes C4 . C5 . H51 . 118.2 no C6 . C5 . H51 . 114.0 no C5 . C6 . N2 . 125.35(18) yes C5 . C6 . C7 . 124.86(19) yes N2 . C6 . C7 . 109.78(18) yes C6 . C7 . C8 . 107.11(18) yes C6 . C7 . H71 . 127.2 no C8 . C7 . H71 . 125.7 no C7 . C8 . C9 . 106.86(18) yes C7 . C8 . H81 . 129.0 no C9 . C8 . H81 . 124.1 no C8 . C9 . N2 . 109.25(18) yes C8 . C9 . C10 . 125.75(18) yes N2 . C9 . C10 . 124.99(18) yes C9 . C10 . C11 . 125.11(17) yes C9 . C10 . C41 . 118.38(18) yes C11 . C10 . C41 . 116.49(19) yes C10 . C11 . N3 . 125.59(18) yes C10 . C11 . C12 . 124.92(18) yes N3 . C11 . C12 . 109.48(18) yes C11 . C12 . C13 . 106.98(18) yes C11 . C12 . H121 . 124.6 no C13 . C12 . H121 . 128.4 no C12 . C13 . C14 . 106.89(19) yes C12 . C13 . H131 . 126.7 no C14 . C13 . H131 . 126.4 no C13 . C14 . N3 . 109.84(17) yes C13 . C14 . C15 . 124.63(19) yes N3 . C14 . C15 . 125.53(18) yes C14 . C15 . C16 . 126.86(19) yes C14 . C15 . H151 . 115.8 no C16 . C15 . H151 . 117.3 no C15 . C16 . N4 . 125.64(18) yes C15 . C16 . C17 . 124.79(19) yes N4 . C16 . C17 . 109.54(17) yes C16 . C17 . C18 . 106.92(18) yes C16 . C17 . H171 . 124.6 no C18 . C17 . H171 . 128.4 no C17 . C18 . C19 . 107.41(18) yes C17 . C18 . H181 . 127.1 no C19 . C18 . H181 . 125.4 no C18 . C19 . N4 . 109.20(18) yes C18 . C19 . C20 . 124.97(18) yes N4 . C19 . C20 . 125.82(18) yes C1 . C20 . C19 . 124.87(18) yes C1 . C20 . C31 . 118.06(17) yes C19 . C20 . C31 . 117.06(17) yes N5 . C21 . C22 . 122.8(2) yes N5 . C21 . H211 . 116.6 no C22 . C21 . H211 . 120.6 no C21 . C22 . C23 . 119.0(2) yes C21 . C22 . H221 . 119.3 no C23 . C22 . H221 . 121.6 no C22 . C23 . C24 . 118.7(2) yes C22 . C23 . H231 . 121.0 no C24 . C23 . H231 . 120.3 no C23 . C24 . C25 . 118.6(2) yes C23 . C24 . H241 . 121.9 no C25 . C24 . H241 . 119.4 no C24 . C25 . N5 . 122.9(2) yes C24 . C25 . H251 . 120.1 no N5 . C25 . H251 . 117.0 no C20 . C31 . C32 . 119.5(2) yes C20 . C31 . C36 . 122.17(19) yes C32 . C31 . C36 . 118.29(19) yes C31 . C32 . C33 . 120.7(2) yes C31 . C32 . H321 . 119.2 no C33 . C32 . H321 . 120.0 no C32 . C33 . C34 . 120.5(2) yes C32 . C33 . H331 . 119.3 no C34 . C33 . H331 . 120.3 no C33 . C34 . C35 . 120.0(2) yes C33 . C34 . H341 . 120.6 no C35 . C34 . H341 . 119.4 no C34 . C35 . C36 . 119.6(2) yes C34 . C35 . H351 . 121.5 no C36 . C35 . H351 . 118.9 no C35 . C36 . C31 . 120.9(2) yes C35 . C36 . S1 . 121.4(2) yes C31 . C36 . S1 . 117.5(2) yes C35 . C36 . C31 . 120.9(2) yes C35 . C36 . S11 . 117.4(3) yes C31 . C36 . S11 . 121.4(2) yes C10 . C41 . C42 . 121.6(2) yes C10 . C41 . C46 . 120.71(18) yes C42 . C41 . C46 . 117.65(19) yes C41 . C42 . C43 . 121.4(2) yes C41 . C42 . H421 . 119.2 no C43 . C42 . H421 . 119.4 no C42 . C43 . C44 . 120.0(2) yes C42 . C43 . H431 . 118.1 no C44 . C43 . H431 . 121.9 no C43 . C44 . C45 . 120.0(2) yes C43 . C44 . H441 . 120.4 no C45 . C44 . H441 . 119.6 no C44 . C45 . C46 . 119.9(2) yes C44 . C45 . H451 . 121.2 no C46 . C45 . H451 . 118.9 no C41 . C46 . C45 . 121.0(2) yes C41 . C46 . S2 . 119.65(15) yes C45 . C46 . S2 . 119.37(17) yes C36 . S1 . C51 . 102.8(2) yes C46 . S2 . C60 . 100.85(9) yes S1 . C51 . O1 . 123.25(6) yes S1 . C51 . C52 . 114.13(6) yes O1 . C51 . C52 . 122.32(6) yes C51 . C52 . C53 . 111.54(7) yes C51 . C52 . H521 . 109.2 no C53 . C52 . H521 . 107.0 no C51 . C52 . H522 . 108.3 no C53 . C52 . H522 . 110.6 no H521 . C52 . H522 . 110.1 no C52 . C53 . C54 . 111.95(7) yes C52 . C53 . H531 . 106.0 no C54 . C53 . H531 . 107.9 no C52 . C53 . H532 . 111.2 no C54 . C53 . H532 . 109.4 no H531 . C53 . H532 . 110.3 no C53 . C54 . C55 . 113.59(7) yes C53 . C54 . H541 . 107.4 no C55 . C54 . H541 . 110.6 no C53 . C54 . H542 . 107.0 no C55 . C54 . H542 . 107.7 no H541 . C54 . H542 . 110.5 no C54 . C55 . C56 . 113.59(7) yes C54 . C55 . H551 . 107.2 no C56 . C55 . H551 . 106.0 no C54 . C55 . H552 . 110.2 no C56 . C55 . H552 . 109.6 no H551 . C55 . H552 . 110.2 no C55 . C56 . C57 . 113.55(7) yes C55 . C56 . H561 . 108.1 no C57 . C56 . H561 . 109.7 no C55 . C56 . H562 . 108.5 no C57 . C56 . H562 . 110.8 no H561 . C56 . H562 . 105.9 no C56 . C57 . C58 . 113.45(7) yes C56 . C57 . H571 . 108.6 no C58 . C57 . H571 . 107.1 no C56 . C57 . H572 . 108.9 no C58 . C57 . H572 . 110.2 no H571 . C57 . H572 . 108.4 no C57 . C58 . C59 . 112.16(7) yes C57 . C58 . H583 . 107.8 no C59 . C58 . H583 . 109.7 no C57 . C58 . H582 . 110.0 no C59 . C58 . H582 . 108.0 no H583 . C58 . H582 . 109.2 no C59 . C58 . C67 . 111.87(7) yes C59 . C58 . H581 . 108.8 no C67 . C58 . H581 . 107.3 no C59 . C58 . H584 . 109.0 no C67 . C58 . H584 . 111.6 no H581 . C58 . H584 . 108.1 no C58 . C59 . C60 . 111.51(5) yes C58 . C59 . H591 . 108.7 no C60 . C59 . H591 . 106.6 no C58 . C59 . H592 . 108.1 no C60 . C59 . H592 . 110.0 no H591 . C59 . H592 . 111.9 no C59 . C60 . S2 . 114.21(4) yes C59 . C60 . O2 . 122.42(4) yes S2 . C60 . O2 . 123.28(4) yes C36 . S11 . C61 . 102.1(3) yes S11 . C61 . O11 . 123.08(6) yes S11 . C61 . C62 . 114.20(7) yes O11 . C61 . C62 . 122.14(6) yes C61 . C62 . C63 . 111.91(7) yes C61 . C62 . H621 . 106.8 no C63 . C62 . H621 . 106.8 no C61 . C62 . H622 . 111.3 no C63 . C62 . H622 . 110.5 no H621 . C62 . H622 . 109.4 no C62 . C63 . C64 . 111.70(7) yes C62 . C63 . H631 . 111.2 no C64 . C63 . H631 . 108.5 no C62 . C63 . H632 . 108.0 no C64 . C63 . H632 . 109.0 no H631 . C63 . H632 . 108.4 no C63 . C64 . C65 . 113.62(7) yes C63 . C64 . H641 . 108.0 no C65 . C64 . H641 . 109.4 no C63 . C64 . H642 . 107.6 no C65 . C64 . H642 . 108.0 no H641 . C64 . H642 . 110.2 no C64 . C65 . C66 . 113.51(7) yes C64 . C65 . H651 . 106.9 no C66 . C65 . H651 . 107.6 no C64 . C65 . H652 . 110.7 no C66 . C65 . H652 . 108.7 no H651 . C65 . H652 . 109.3 no C65 . C66 . C67 . 113.47(7) yes C65 . C66 . H661 . 107.5 no C67 . C66 . H661 . 108.1 no C65 . C66 . H662 . 109.2 no C67 . C66 . H662 . 111.3 no H661 . C66 . H662 . 107.1 no C58 . C67 . C66 . 113.51(7) yes C58 . C67 . H671 . 109.9 no C66 . C67 . H671 . 110.0 no C58 . C67 . H672 . 106.8 no C66 . C67 . H672 . 107.6 no H671 . C67 . H672 . 108.8 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 C24 . H241 . O11 4_465 137 0.93 2.38 3.124(4) yes C54 . H542 . N3 2_665 133 1.00 2.55 3.315(4) yes C64 . H542 . N3 2_665 141 1.07 2.55 3.453(4) yes _iucr_refine_instructions_details ; # # Punched on 24/01/17 at 14:31:00 # #LIST 12 BLOCK SCALE X'S U'S CONT ENANTIO EQUIV PART(1001,OCC) PART(1002,OCC) WEIGHT -1 PART(1002,OCC) RIDE O(1,U'S) O(11,U'S) RIDE C(51,U'S) C(61,U'S) RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 15,X'S) H ( 151,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 33,X'S) H ( 331,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 43,X'S) H ( 431,X'S) RIDE C ( 44,X'S) H ( 441,X'S) RIDE C ( 45,X'S) H ( 451,X'S) RIDE C ( 62,X'S) H ( 621,X'S) H ( 622,X'S) RIDE C ( 63,X'S) H ( 631,X'S) H ( 632,X'S) RIDE C ( 54,X'S) H ( 541,X'S) H ( 542,X'S) RIDE C ( 55,X'S) H ( 551,X'S) H ( 552,X'S) RIDE C ( 56,X'S) H ( 561,X'S) H ( 562,X'S) RIDE C ( 57,X'S) H ( 571,X'S) H ( 572,X'S) RIDE C ( 58,X'S) H ( 581,X'S) H ( 582,X'S) CONT H ( 583,X'S) H ( 584,X'S) RIDE C ( 59,X'S) H ( 591,X'S) H ( 592,X'S) RIDE C ( 52,X'S) H ( 521,X'S) H ( 522,X'S) RIDE C ( 53,X'S) H ( 531,X'S) H ( 532,X'S) RIDE C ( 64,X'S) H ( 641,X'S) H ( 642,X'S) RIDE C ( 65,X'S) H ( 651,X'S) H ( 652,X'S) RIDE C ( 66,X'S) H ( 661,X'S) H ( 662,X'S) RIDE C ( 67,X'S) H ( 671,X'S) H ( 672,X'S) END # # Punched on 24/01/17 at 14:31:00 # #LIST 16 SAME S(1) O(1) C(51) C(52) C(53) C(54) C(55) CONT C(56) C(57) C(58) C(59) C(60) O(2) S(2) AND CONT S(2) O(2) C(60) C(59) C(58) C(57) C(56) CONT C(55) C(54) C(53) C(52) C(51) O(1) S(1) AND CONT S(11) O(11) C(61) C(62) C(63) C(64) C(65) CONT C(66) C(67) C(58) C(59) C(60) O(2) S(2) AND CONT S(2) O(2) C(60) C(59) C(58) C(67) C(66) CONT C(65) C(64) C(63) C(62) C(61) O(11) S(11) SIMU 0.01 S(1) O(1) C(51) C(52) C(53) C(54) C(55) CONT C(56) C(57) C(58) C(59) C(60) O(2) S(2) AND CONT S(2) O(2) C(60) C(59) C(58) C(57) C(56) CONT C(55) C(54) C(53) C(52) C(51) O(1) S(1) AND CONT S(11) O(11) C(61) C(62) C(63) C(64) C(65) CONT C(66) C(67) C(58) C(59) C(60) O(2) S(2) AND CONT S(2) O(2) C(60) C(59) C(58) C(67) C(66) CONT C(65) C(64) C(63) C(62) C(61) O(11) S(11) DELU 0.01 S(1) O(1) C(51) C(52) C(53) C(54) C(55) CONT C(56) C(57) C(58) C(59) C(60) O(2) S(2) AND CONT S(2) O(2) C(60) C(59) C(58) C(57) C(56) CONT C(55) C(54) C(53) C(52) C(51) O(1) S(1) AND CONT S(11) O(11) C(61) C(62) C(63) C(64) C(65) CONT C(66) C(67) C(58) C(59) C(60) O(2) S(2) AND CONT S(2) O(2) C(60) C(59) C(58) C(67) C(66) CONT C(65) C(64) C(63) C(62) C(61) O(11) S(11) END ; #============================================================================== data_6c-I #============================================================================== _audit_creation_date "2017-02-14" _audit_creation_method CRYSTALS_ver_14.61_build_6019 _oxford_structure_analysis_title '6701' _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 9.1845(6) _cell_length_b 49.152(6) _cell_length_c 9.3517(6) _cell_angle_alpha 90 _cell_angle_beta 92.324(5) _cell_angle_gamma 90 _cell_volume 4218.2(6) _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 21/a ' _symmetry_space_group_name_Hall '-P 2yab' 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' 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 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0311 0.0180 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 0.0492 0.0322 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 0.3331 0.5567 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 -1.5491 0.6778 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' _cell_formula_units_Z 4 # Given Formula = C84 H84 N10 O4 S4 Zn2 # Dc = 2.45 Fooo = 3256.00 Mu = 40.79 M = 1556.68 # Found Formula = C49 H43 N5 O2 S2 Zn1 # Dc = 1.36 FOOO = 1800.00 Mu = 20.99 M = 863.42 _chemical_formula_sum 'C49 H43 N5 O2 S2 Zn1' _chemical_formula_moiety 'C49 H43 N5 O2 S2 Zn1' _chemical_compound_source . _chemical_formula_weight 863.42 _cell_measurement_reflns_used 5403 _cell_measurement_theta_min 5 _cell_measurement_theta_max 75 _cell_measurement_temperature 300 _exptl_crystal_description 'plate' _exptl_crystal_colour 'clear_intense_red' _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_max 0.28 _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 2.099 # Sheldrick geometric approximatio 0.69 0.96 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro, (Agilent, 2011)' _exptl_absorpt_correction_T_min 0.73 _exptl_absorpt_correction_T_max 0.96 _diffrn_measurement_device_type 'Oxford Diffraction SuperNova' _diffrn_measurement_device 'Area' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlisPro, (Agilent, 2011)' _computing_data_reduction 'CrysAlisPro, (Agilent, 2011)' _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 300 _diffrn_reflns_number 24727 _reflns_number_total 8714 _diffrn_reflns_av_R_equivalents 0.063 # Number of reflections without Friedels Law is 13862 # Number of reflections with Friedels Law is 8714 # Theoretical number of reflections is about 8842 _diffrn_reflns_theta_min 3.597 _diffrn_reflns_theta_max 76.306 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 74.017 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -59 _diffrn_reflns_limit_k_max 61 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 61 _reflns_limit_l_min 0 _reflns_limit_l_max 11 _oxford_diffrn_Wilson_B_factor 4.76 _oxford_diffrn_Wilson_scale 0.27 _atom_sites_solution_primary Other #heavy,direct,difmap,geom,iterative # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.89 _refine_diff_density_max 0.76 # 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>-3.0\s(I) _refine_ls_number_reflns 8711 _refine_ls_number_restraints 142 _refine_ls_number_parameters 532 _oxford_refine_ls_R_factor_ref 0.1190 _refine_ls_wR_factor_ref 0.2579 _refine_ls_goodness_of_fit_ref 0.9997 _refine_ls_shift/su_max 0.0003297 _refine_ls_shift/su_mean 0.0000196 # The values computed with all filters except I/sigma _oxford_reflns_number_all 8711 _refine_ls_R_factor_all 0.1190 _refine_ls_wR_factor_all 0.2579 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6896 _refine_ls_R_factor_gt 0.1028 _refine_ls_wR_factor_gt 0.2467 # 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 Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr #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^) + ( 0.06P)^2^ +18.71P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # 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. Agilent (2011). CrysAlisPro. Oxford Diffraction, (2010). Supernova User Manual. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. 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 atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Zn1 Zn 0.37414(9) 0.389780(16) 0.31948(9) 0.0550 1.0000 Uani . . . . . . N1 N 0.3846(6) 0.43124(10) 0.3605(6) 0.0556 1.0000 Uani . . . . . . N2 N 0.1851(5) 0.38729(10) 0.4324(5) 0.0547 1.0000 Uani . . . . . . N3 N 0.3924(6) 0.34795(10) 0.3439(6) 0.0614 1.0000 Uani . . . . . . N4 N 0.5891(6) 0.39191(11) 0.2640(5) 0.0573 1.0000 Uani . . . . . . N5 N 0.2662(6) 0.39191(12) 0.1100(6) 0.0619 1.0000 Uani . . . . . . C1 C 0.4895(7) 0.44860(13) 0.3171(7) 0.0568 1.0000 Uani . . . . . . C2 C 0.4446(8) 0.47617(14) 0.3474(9) 0.0718 1.0000 Uani . . . . . . C3 C 0.3161(8) 0.47481(14) 0.4083(9) 0.0730 1.0000 Uani . . . . . . C4 C 0.2760(7) 0.44628(13) 0.4144(8) 0.0618 1.0000 Uani . . . . . . C5 C 0.1461(7) 0.43611(14) 0.4653(8) 0.0674 1.0000 Uani . . . . . . C6 C 0.1044(7) 0.40908(13) 0.4694(7) 0.0583 1.0000 Uani . . . . . . C7 C -0.0385(8) 0.39982(15) 0.5103(8) 0.0702 1.0000 Uani . . . . . . C8 C -0.0404(8) 0.37282(15) 0.4981(7) 0.0669 1.0000 Uani . . . . . . C9 C 0.1012(8) 0.36443(13) 0.4505(7) 0.0605 1.0000 Uani . . . . . . C10 C 0.1506(8) 0.33793(13) 0.4302(7) 0.0623 1.0000 Uani . . . . . . C11 C 0.2862(8) 0.33039(13) 0.3859(8) 0.0645 1.0000 Uani . . . . . . C12 C 0.3420(9) 0.30300(14) 0.3758(9) 0.0787 1.0000 Uani . . . . . . C13 C 0.4758(9) 0.30442(14) 0.3272(9) 0.0803 1.0000 Uani . . . . . . C14 C 0.5075(8) 0.33274(14) 0.3052(8) 0.0688 1.0000 Uani . . . . . . C15 C 0.6341(8) 0.34289(15) 0.2492(9) 0.0738 1.0000 Uani . . . . . . C16 C 0.6715(7) 0.37007(15) 0.2267(8) 0.0663 1.0000 Uani . . . . . . C17 C 0.8017(8) 0.37958(17) 0.1652(9) 0.0793 1.0000 Uani . . . . . . C18 C 0.7988(8) 0.40695(17) 0.1639(8) 0.0719 1.0000 Uani . . . . . . C19 C 0.6630(7) 0.41472(15) 0.2274(7) 0.0611 1.0000 Uani . . . . . . C20 C 0.6179(7) 0.44143(13) 0.2533(7) 0.0578 1.0000 Uani . . . . . . C21 C 0.2344(14) 0.4149(2) 0.0449(11) 0.1228 1.0000 Uani . . . . . . C22 C 0.157(2) 0.4157(3) -0.0817(15) 0.1763 1.0000 Uani . . . . . . C23 C 0.1048(15) 0.3930(3) -0.1417(12) 0.1452 1.0000 Uani . . . . . . C24 C 0.1309(15) 0.3698(3) -0.0751(12) 0.1396 1.0000 Uani . . . . . . C25 C 0.2153(11) 0.3696(2) 0.0491(9) 0.0983 1.0000 Uani . . . . . . C31 C 0.7150(7) 0.46408(14) 0.2102(8) 0.0620 1.0000 Uani . . . . . . C32 C 0.8210(9) 0.47411(19) 0.3089(10) 0.0880 1.0000 Uani . . . . . . C33 C 0.9098(10) 0.4954(2) 0.2722(13) 0.1037 1.0000 Uani . . . . . . C34 C 0.8961(10) 0.5075(2) 0.1409(13) 0.0987 1.0000 Uani . . . . . . C35 C 0.7915(9) 0.49790(19) 0.0426(11) 0.0933 1.0000 Uani . . . . . . C36 C 0.7007(7) 0.47650(16) 0.0756(9) 0.0717 1.0000 Uani . U . . . . C41 C 0.0431(8) 0.31529(14) 0.4566(8) 0.0697 1.0000 Uani . . . . . . C42 C 0.0054(11) 0.30935(18) 0.5976(10) 0.0930 1.0000 Uani . . . . . . C43 C -0.0945(13) 0.2893(2) 0.6241(12) 0.1083 1.0000 Uani . . . . . . C44 C -0.1552(12) 0.2744(2) 0.5152(13) 0.1058 1.0000 Uani . . . . . . C45 C -0.1202(10) 0.27940(17) 0.3764(11) 0.0897 1.0000 Uani . . . . . . C46 C -0.0209(8) 0.29971(14) 0.3473(9) 0.0709 1.0000 Uani . U . . . . S1 S 0.5671(2) 0.46459(5) -0.0493(2) 0.0841 1.0000 Uani . U . . . . S2 S 0.0139(2) 0.30718(4) 0.1680(2) 0.0788 1.0000 Uani . U . . . . O1 O 0.8019(8) 0.45231(18) -0.1914(9) 0.1240 1.0000 Uani . U . . . . O2 O 0.1309(8) 0.25824(12) 0.1876(9) 0.1120 1.0000 Uani . U . . . . C51 C 0.6705(10) 0.4506(2) -0.1889(10) 0.0937 1.0000 Uani D U . . . . C52 C 0.5810(12) 0.4378(2) -0.3082(8) 0.1428 1.0000 Uani D U . . . . C53 C 0.5101(10) 0.4120(2) -0.2547(13) 0.1734 1.0000 Uani D U . . . . C54 C 0.6099(13) 0.3878(2) -0.279(2) 0.2176 1.0000 Uani D U . . . . C55 C 0.5351(12) 0.3614(2) -0.230(3) 0.2498 1.0000 Uani D U . . . . C56 C 0.6398(16) 0.3379(2) -0.238(2) 0.2756 1.0000 Uani D U . . . . C57 C 0.5788(15) 0.3130(3) -0.1575(18) 0.2664 1.0000 Uani D U . . . . C58 C 0.4222(12) 0.3081(3) -0.207(2) 0.2886 1.0000 Uani D U . . . . C59 C 0.3840(13) 0.2783(3) -0.1854(13) 0.2110 1.0000 Uani D U . . . . C60 C 0.3286(10) 0.2744(3) -0.0363(12) 0.2003 1.0000 Uani D U . . . . C61 C 0.1663(10) 0.2810(3) -0.0368(10) 0.1372 1.0000 Uani D U . . . . C62 C 0.1116(9) 0.27762(17) 0.1131(11) 0.0887 1.0000 Uani D U . . . . H21 H 0.4958 0.4920 0.3279 0.0858 1.0000 Uiso R . . . . . H31 H 0.2626 0.4896 0.4416 0.0879 1.0000 Uiso R . . . . . H51 H 0.0806 0.4487 0.4995 0.0809 1.0000 Uiso R . . . . . H71 H -0.1152 0.4107 0.5393 0.0839 1.0000 Uiso R . . . . . H81 H -0.1189 0.3614 0.5176 0.0800 1.0000 Uiso R . . . . . H121 H 0.2927 0.2874 0.3992 0.0951 1.0000 Uiso R . . . . . H131 H 0.5392 0.2900 0.3106 0.0959 1.0000 Uiso R . . . . . H151 H 0.7035 0.3301 0.2250 0.0869 1.0000 Uiso R . . . . . H171 H 0.8764 0.3687 0.1319 0.0937 1.0000 Uiso R . . . . . H181 H 0.8694 0.4187 0.1290 0.0869 1.0000 Uiso R . . . . . H211 H 0.2651 0.4312 0.0864 0.1460 1.0000 Uiso R . . . . . H221 H 0.1395 0.4322 -0.1272 0.1992 1.0000 Uiso R . . . . . H231 H 0.0528 0.3934 -0.2286 0.1778 1.0000 Uiso R . . . . . H241 H 0.0926 0.3536 -0.1126 0.1639 1.0000 Uiso R . . . . . H251 H 0.2384 0.3528 0.0917 0.1161 1.0000 Uiso R . . . . . H321 H 0.8306 0.4663 0.4000 0.1040 1.0000 Uiso R . . . . . H331 H 0.9811 0.5014 0.3383 0.1209 1.0000 Uiso R . . . . . H341 H 0.9546 0.5221 0.1177 0.1199 1.0000 Uiso R . . . . . H351 H 0.7818 0.5059 -0.0475 0.1111 1.0000 Uiso R . . . . . H421 H 0.0493 0.3191 0.6730 0.1109 1.0000 Uiso R . . . . . H431 H -0.1216 0.2863 0.7178 0.1259 1.0000 Uiso R . . . . . H441 H -0.2212 0.2607 0.5356 0.1270 1.0000 Uiso R . . . . . H451 H -0.1622 0.2692 0.3021 0.1080 1.0000 Uiso R . . . . . H521 H 0.5042 0.4501 -0.3378 0.1702 1.0000 Uiso R . . . . . H522 H 0.6420 0.4337 -0.3877 0.1701 1.0000 Uiso R . . . . . H531 H 0.4892 0.4138 -0.1529 0.2054 1.0000 Uiso R . . . . . H532 H 0.4204 0.4088 -0.3122 0.2052 1.0000 Uiso R . . . . . H541 H 0.6991 0.3908 -0.2239 0.2590 1.0000 Uiso R . . . . . H542 H 0.6289 0.3863 -0.3794 0.2590 1.0000 Uiso R . . . . . H551 H 0.5099 0.3630 -0.1305 0.2981 1.0000 Uiso R . . . . . H552 H 0.4497 0.3578 -0.2909 0.2981 1.0000 Uiso R . . . . . H561 H 0.7335 0.3435 -0.1968 0.3282 1.0000 Uiso R . . . . . H562 H 0.6467 0.3337 -0.3383 0.3282 1.0000 Uiso R . . . . . H571 H 0.5847 0.3162 -0.0560 0.3160 1.0000 Uiso R . . . . . H572 H 0.6328 0.2969 -0.1806 0.3159 1.0000 Uiso R . . . . . H581 H 0.3605 0.3191 -0.1478 0.3453 1.0000 Uiso R . . . . . H582 H 0.4087 0.3129 -0.3083 0.3452 1.0000 Uiso R . . . . . H591 H 0.4725 0.2676 -0.1963 0.2541 1.0000 Uiso R . . . . . H592 H 0.3092 0.2729 -0.2560 0.2543 1.0000 Uiso R . . . . . H601 H 0.3816 0.2862 0.0300 0.2421 1.0000 Uiso R . . . . . H602 H 0.3402 0.2555 -0.0106 0.2421 1.0000 Uiso R . . . . . H611 H 0.1522 0.2997 -0.0671 0.1662 1.0000 Uiso R . . . . . H612 H 0.1138 0.2690 -0.1022 0.1662 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 Zn1 0.0591(5) 0.0476(4) 0.0576(5) -0.0021(4) -0.0064(3) 0.0057(4) N1 0.058(3) 0.047(3) 0.062(3) -0.006(2) 0.000(2) 0.002(2) N2 0.059(3) 0.049(3) 0.056(3) 0.003(2) -0.003(2) -0.001(2) N3 0.067(3) 0.048(3) 0.068(3) 0.000(2) -0.013(3) 0.009(2) N4 0.058(3) 0.055(3) 0.058(3) -0.010(2) -0.006(2) 0.009(2) N5 0.066(3) 0.065(3) 0.054(3) 0.001(2) -0.005(2) -0.003(3) C1 0.059(3) 0.053(3) 0.058(3) -0.003(3) -0.001(3) 0.003(3) C2 0.073(4) 0.048(3) 0.095(5) -0.003(3) 0.009(4) -0.002(3) C3 0.068(4) 0.052(4) 0.100(6) -0.008(4) 0.013(4) 0.003(3) C4 0.064(4) 0.046(3) 0.076(4) -0.003(3) 0.008(3) 0.003(3) C5 0.058(4) 0.055(4) 0.090(5) 0.000(3) 0.015(3) 0.007(3) C6 0.059(3) 0.060(4) 0.056(3) 0.004(3) 0.003(3) 0.006(3) C7 0.059(4) 0.069(4) 0.083(5) 0.007(4) 0.008(3) 0.002(3) C8 0.069(4) 0.069(4) 0.062(4) 0.010(3) -0.003(3) -0.013(3) C9 0.071(4) 0.054(3) 0.056(3) 0.006(3) -0.004(3) -0.003(3) C10 0.076(4) 0.053(3) 0.057(4) 0.005(3) -0.011(3) -0.007(3) C11 0.067(4) 0.053(3) 0.071(4) 0.001(3) -0.016(3) 0.000(3) C12 0.084(5) 0.047(3) 0.103(6) 0.004(4) -0.025(4) 0.000(3) C13 0.089(6) 0.050(4) 0.100(6) -0.010(4) -0.025(4) 0.017(4) C14 0.069(4) 0.053(3) 0.083(5) -0.002(3) -0.019(4) 0.015(3) C15 0.073(5) 0.061(4) 0.086(5) -0.013(4) -0.009(4) 0.022(3) C16 0.060(4) 0.063(4) 0.076(4) -0.009(3) 0.000(3) 0.014(3) C17 0.065(4) 0.087(5) 0.087(5) -0.014(4) 0.009(4) 0.019(4) C18 0.062(4) 0.081(5) 0.072(4) -0.001(4) 0.004(3) 0.010(4) C19 0.058(4) 0.069(4) 0.056(3) -0.008(3) -0.003(3) 0.008(3) C20 0.059(3) 0.060(3) 0.053(3) -0.002(3) -0.008(3) -0.001(3) C21 0.182(11) 0.076(6) 0.104(7) 0.017(5) -0.070(8) 0.003(6) C22 0.28(2) 0.117(10) 0.124(10) 0.035(9) -0.094(12) 0.014(12) C23 0.175(12) 0.176(14) 0.078(7) 0.022(8) -0.069(7) -0.015(11) C24 0.168(12) 0.153(12) 0.093(8) 0.002(8) -0.059(8) -0.030(9) C25 0.135(8) 0.091(6) 0.066(5) -0.008(4) -0.024(5) -0.013(6) C31 0.048(3) 0.062(4) 0.076(4) -0.005(3) 0.003(3) 0.004(3) C32 0.065(4) 0.099(6) 0.100(6) -0.013(5) -0.002(4) -0.016(4) C33 0.070(5) 0.114(8) 0.127(9) -0.039(7) 0.008(5) -0.028(5) C34 0.068(5) 0.086(6) 0.144(9) -0.012(6) 0.029(6) -0.020(4) C35 0.069(5) 0.093(6) 0.119(7) 0.021(5) 0.020(5) -0.003(4) C36 0.051(3) 0.073(4) 0.092(4) 0.005(3) 0.016(3) 0.001(3) C41 0.077(4) 0.052(3) 0.079(5) 0.009(3) -0.007(4) -0.003(3) C42 0.124(7) 0.078(5) 0.076(5) 0.010(4) -0.009(5) -0.024(5) C43 0.135(9) 0.083(6) 0.107(8) 0.029(6) 0.013(6) -0.019(6) C44 0.110(7) 0.082(6) 0.126(9) 0.012(6) 0.002(6) -0.033(5) C45 0.094(6) 0.065(5) 0.109(7) 0.001(5) -0.016(5) -0.013(4) C46 0.070(4) 0.051(3) 0.089(5) 0.003(3) -0.021(3) -0.004(3) S1 0.0648(10) 0.1113(16) 0.0757(12) 0.0179(11) -0.0027(8) -0.0018(11) S2 0.0913(13) 0.0585(9) 0.0845(13) 0.0004(9) -0.0226(10) 0.0029(9) O1 0.093(3) 0.148(7) 0.133(6) -0.030(5) 0.028(4) -0.019(4) O2 0.109(5) 0.066(3) 0.160(6) 0.004(3) -0.010(4) 0.016(3) C51 0.090(3) 0.117(7) 0.074(4) 0.017(3) 0.006(3) -0.001(4) C52 0.120(7) 0.228(9) 0.081(6) -0.016(6) 0.011(5) -0.038(7) C53 0.164(12) 0.204(10) 0.153(11) -0.052(9) 0.026(10) -0.060(7) C54 0.176(14) 0.261(11) 0.222(16) 0.076(15) 0.092(12) 0.007(11) C55 0.192(17) 0.222(12) 0.34(2) 0.017(18) 0.041(17) -0.036(10) C56 0.232(18) 0.255(13) 0.34(2) 0.060(19) 0.049(18) 0.005(12) C57 0.205(15) 0.271(14) 0.33(2) 0.068(16) 0.089(16) 0.036(13) C58 0.270(17) 0.275(18) 0.32(2) 0.044(17) 0.024(18) -0.035(17) C59 0.220(13) 0.232(15) 0.186(12) 0.014(15) 0.063(11) 0.054(12) C60 0.178(10) 0.256(16) 0.170(12) -0.011(12) 0.047(9) 0.061(13) C61 0.169(8) 0.126(9) 0.116(6) -0.019(5) 0.008(6) 0.031(8) C62 0.091(5) 0.064(3) 0.109(5) -0.014(3) -0.022(4) 0.000(3) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 2.96(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 . N1 . 2.075(5) yes Zn1 . N2 . 2.072(5) yes Zn1 . N3 . 2.075(5) yes Zn1 . N4 . 2.064(5) yes Zn1 . N5 . 2.162(5) yes N1 . C1 . 1.361(8) yes N1 . C4 . 1.355(8) yes N2 . C6 . 1.356(8) yes N2 . C9 . 1.377(8) yes N3 . C11 . 1.372(9) yes N3 . C14 . 1.356(9) yes N4 . C16 . 1.367(8) yes N4 . C19 . 1.362(9) yes N5 . C21 . 1.313(10) yes N5 . C25 . 1.312(10) yes C1 . C2 . 1.448(9) yes C1 . C20 . 1.389(9) yes C2 . C3 . 1.332(10) yes C2 . H21 . 0.931 no C3 . C4 . 1.452(9) yes C3 . H31 . 0.938 no C4 . C5 . 1.395(9) yes C5 . C6 . 1.384(9) yes C5 . H51 . 0.928 no C6 . C7 . 1.455(9) yes C7 . C8 . 1.332(10) yes C7 . H71 . 0.933 no C8 . C9 . 1.452(10) yes C8 . H81 . 0.938 no C9 . C10 . 1.395(9) yes C10 . C11 . 1.379(10) yes C10 . C41 . 1.515(9) yes C11 . C12 . 1.445(9) yes C12 . C13 . 1.329(12) yes C12 . H121 . 0.921 no C13 . C14 . 1.438(10) yes C13 . H131 . 0.934 no C14 . C15 . 1.387(11) yes C15 . C16 . 1.398(10) yes C15 . H151 . 0.929 no C16 . C17 . 1.426(11) yes C17 . C18 . 1.346(11) yes C17 . H171 . 0.934 no C18 . C19 . 1.454(9) yes C18 . H181 . 0.937 no C19 . C20 . 1.400(9) yes C20 . C31 . 1.492(9) yes C21 . C22 . 1.356(14) yes C21 . H211 . 0.925 no C22 . C23 . 1.330(18) yes C22 . H221 . 0.929 no C23 . C24 . 1.315(17) yes C23 . H231 . 0.926 no C24 . C25 . 1.370(12) yes C24 . H241 . 0.934 no C25 . H251 . 0.939 no C31 . C32 . 1.403(10) yes C31 . C36 . 1.401(10) yes C32 . C33 . 1.378(13) yes C32 . H321 . 0.935 no C33 . C34 . 1.367(15) yes C33 . H331 . 0.930 no C34 . C35 . 1.385(14) yes C34 . H341 . 0.926 no C35 . C36 . 1.385(11) yes C35 . H351 . 0.930 no C36 . S1 . 1.759(8) yes C41 . C42 . 1.407(11) yes C41 . C46 . 1.388(10) yes C42 . C43 . 1.377(12) yes C42 . H421 . 0.931 no C43 . C44 . 1.355(14) yes C43 . H431 . 0.932 no C44 . C45 . 1.372(13) yes C44 . H441 . 0.932 no C45 . C46 . 1.387(11) yes C45 . H451 . 0.929 no C46 . S2 . 1.758(9) yes S1 . C51 . 1.784(10) yes S2 . C62 . 1.793(9) yes O1 . C51 . 1.211(11) yes O2 . C62 . 1.190(11) yes C51 . C52 . 1.497(13) yes C52 . C53 . 1.521(8) yes C52 . H521 . 0.963 no C52 . H522 . 0.971 no C53 . C54 . 1.524(9) yes C53 . H531 . 0.983 no C53 . H532 . 0.977 no C54 . C55 . 1.547(9) yes C54 . H541 . 0.962 no C54 . H542 . 0.965 no C55 . C56 . 1.504(9) yes C55 . H551 . 0.971 no C55 . H552 . 0.967 no C56 . C57 . 1.554(9) yes C56 . H561 . 0.968 no C56 . H562 . 0.965 no C57 . C58 . 1.514(9) yes C57 . H571 . 0.961 no C57 . H572 . 0.966 no C58 . C59 . 1.523(9) yes C58 . H581 . 0.975 no C58 . H582 . 0.976 no C59 . C60 . 1.515(8) yes C59 . H591 . 0.976 no C59 . H592 . 0.970 no C60 . C61 . 1.526(8) yes C60 . H601 . 0.967 no C60 . H602 . 0.966 no C61 . C62 . 1.518(14) yes C61 . H611 . 0.970 no C61 . H612 . 0.966 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Zn1 . N2 . 89.8(2) yes N1 . Zn1 . N3 . 161.8(2) yes N2 . Zn1 . N3 . 87.2(2) yes N1 . Zn1 . N4 . 87.6(2) yes N2 . Zn1 . N4 . 163.9(2) yes N3 . Zn1 . N4 . 90.2(2) yes N1 . Zn1 . N5 . 97.8(2) yes N2 . Zn1 . N5 . 95.8(2) yes N3 . Zn1 . N5 . 100.4(2) yes N4 . Zn1 . N5 . 100.3(2) yes Zn1 . N1 . C1 . 126.0(4) yes Zn1 . N1 . C4 . 125.1(4) yes C1 . N1 . C4 . 108.0(5) yes Zn1 . N2 . C6 . 124.2(4) yes Zn1 . N2 . C9 . 126.6(4) yes C6 . N2 . C9 . 107.4(5) yes Zn1 . N3 . C11 . 126.8(4) yes Zn1 . N3 . C14 . 125.3(5) yes C11 . N3 . C14 . 107.5(6) yes Zn1 . N4 . C16 . 124.7(5) yes Zn1 . N4 . C19 . 126.6(4) yes C16 . N4 . C19 . 107.2(5) yes Zn1 . N5 . C21 . 123.2(6) yes Zn1 . N5 . C25 . 119.7(5) yes C21 . N5 . C25 . 116.7(7) yes N1 . C1 . C2 . 108.5(5) yes N1 . C1 . C20 . 126.4(6) yes C2 . C1 . C20 . 125.1(6) yes C1 . C2 . C3 . 107.5(6) yes C1 . C2 . H21 . 126.4 no C3 . C2 . H21 . 126.1 no C2 . C3 . C4 . 107.2(6) yes C2 . C3 . H31 . 126.0 no C4 . C3 . H31 . 126.8 no C3 . C4 . N1 . 108.7(6) yes C3 . C4 . C5 . 125.5(6) yes N1 . C4 . C5 . 125.7(6) yes C4 . C5 . C6 . 126.5(6) yes C4 . C5 . H51 . 117.1 no C6 . C5 . H51 . 116.4 no C5 . C6 . N2 . 126.6(6) yes C5 . C6 . C7 . 124.2(6) yes N2 . C6 . C7 . 109.2(6) yes C6 . C7 . C8 . 107.3(7) yes C6 . C7 . H71 . 126.6 no C8 . C7 . H71 . 126.0 no C7 . C8 . C9 . 107.5(6) yes C7 . C8 . H81 . 126.1 no C9 . C8 . H81 . 126.4 no C8 . C9 . N2 . 108.6(6) yes C8 . C9 . C10 . 127.4(6) yes N2 . C9 . C10 . 124.0(6) yes C9 . C10 . C11 . 126.5(6) yes C9 . C10 . C41 . 116.5(6) yes C11 . C10 . C41 . 117.0(6) yes C10 . C11 . N3 . 125.3(6) yes C10 . C11 . C12 . 126.7(7) yes N3 . C11 . C12 . 108.0(6) yes C11 . C12 . C13 . 108.0(7) yes C11 . C12 . H121 . 125.5 no C13 . C12 . H121 . 126.5 no C12 . C13 . C14 . 107.2(7) yes C12 . C13 . H131 . 127.5 no C14 . C13 . H131 . 125.3 no C13 . C14 . N3 . 109.3(7) yes C13 . C14 . C15 . 125.4(7) yes N3 . C14 . C15 . 125.2(6) yes C14 . C15 . C16 . 128.0(7) yes C14 . C15 . H151 . 116.3 no C16 . C15 . H151 . 115.7 no C15 . C16 . N4 . 124.8(7) yes C15 . C16 . C17 . 126.1(7) yes N4 . C16 . C17 . 109.1(6) yes C16 . C17 . C18 . 108.4(7) yes C16 . C17 . H171 . 125.9 no C18 . C17 . H171 . 125.8 no C17 . C18 . C19 . 106.0(7) yes C17 . C18 . H181 . 127.3 no C19 . C18 . H181 . 126.7 no C18 . C19 . N4 . 109.3(6) yes C18 . C19 . C20 . 125.5(7) yes N4 . C19 . C20 . 125.1(6) yes C19 . C20 . C1 . 125.0(6) yes C19 . C20 . C31 . 118.0(6) yes C1 . C20 . C31 . 117.0(6) yes N5 . C21 . C22 . 121.8(11) yes N5 . C21 . H211 . 119.3 no C22 . C21 . H211 . 118.9 no C21 . C22 . C23 . 120.9(12) yes C21 . C22 . H221 . 119.9 no C23 . C22 . H221 . 119.2 no C22 . C23 . C24 . 118.1(10) yes C22 . C23 . H231 . 121.0 no C24 . C23 . H231 . 120.9 no C23 . C24 . C25 . 119.6(12) yes C23 . C24 . H241 . 120.2 no C25 . C24 . H241 . 120.2 no C24 . C25 . N5 . 122.8(10) yes C24 . C25 . H251 . 118.4 no N5 . C25 . H251 . 118.8 no C20 . C31 . C32 . 119.4(7) yes C20 . C31 . C36 . 122.2(6) yes C32 . C31 . C36 . 118.4(7) yes C31 . C32 . C33 . 120.3(9) yes C31 . C32 . H321 . 119.4 no C33 . C32 . H321 . 120.3 no C32 . C33 . C34 . 121.4(9) yes C32 . C33 . H331 . 118.9 no C34 . C33 . H331 . 119.7 no C33 . C34 . C35 . 118.9(8) yes C33 . C34 . H341 . 121.0 no C35 . C34 . H341 . 120.1 no C34 . C35 . C36 . 121.3(9) yes C34 . C35 . H351 . 119.7 no C36 . C35 . H351 . 119.0 no C31 . C36 . C35 . 119.7(8) yes C31 . C36 . S1 . 119.3(5) yes C35 . C36 . S1 . 121.0(7) yes C10 . C41 . C42 . 119.4(7) yes C10 . C41 . C46 . 123.0(7) yes C42 . C41 . C46 . 117.6(7) yes C41 . C42 . C43 . 120.6(9) yes C41 . C42 . H421 . 119.2 no C43 . C42 . H421 . 120.2 no C42 . C43 . C44 . 120.5(10) yes C42 . C43 . H431 . 119.2 no C44 . C43 . H431 . 120.3 no C43 . C44 . C45 . 120.7(9) yes C43 . C44 . H441 . 119.2 no C45 . C44 . H441 . 120.1 no C44 . C45 . C46 . 119.7(9) yes C44 . C45 . H451 . 120.3 no C46 . C45 . H451 . 120.0 no C41 . C46 . C45 . 121.0(8) yes C41 . C46 . S2 . 120.0(6) yes C45 . C46 . S2 . 118.9(6) yes C36 . S1 . C51 . 103.7(4) yes C46 . S2 . C62 . 102.5(4) yes S1 . C51 . O1 . 123.2(8) yes S1 . C51 . C52 . 114.5(7) yes O1 . C51 . C52 . 122.2(9) yes C51 . C52 . C53 . 109.56(10) yes C51 . C52 . H521 . 108.9 no C53 . C52 . H521 . 107.6 no C51 . C52 . H522 . 109.9 no C53 . C52 . H522 . 110.3 no H521 . C52 . H522 . 110.5 no C52 . C53 . C54 . 109.53(10) yes C52 . C53 . H531 . 110.2 no C54 . C53 . H531 . 110.9 no C52 . C53 . H532 . 108.3 no C54 . C53 . H532 . 107.0 no H531 . C53 . H532 . 110.7 no C53 . C54 . C55 . 109.48(10) yes C53 . C54 . H541 . 107.7 no C55 . C54 . H541 . 110.5 no C53 . C54 . H542 . 109.8 no C55 . C54 . H542 . 108.9 no H541 . C54 . H542 . 110.5 no C54 . C55 . C56 . 109.52(10) yes C54 . C55 . H551 . 109.9 no C56 . C55 . H551 . 106.8 no C54 . C55 . H552 . 109.7 no C56 . C55 . H552 . 109.7 no H551 . C55 . H552 . 111.2 no C55 . C56 . C57 . 109.53(10) yes C55 . C56 . H561 . 108.9 no C57 . C56 . H561 . 111.2 no C55 . C56 . H562 . 106.4 no C57 . C56 . H562 . 109.8 no H561 . C56 . H562 . 110.9 no C56 . C57 . C58 . 109.50(10) yes C56 . C57 . H571 . 110.1 no C58 . C57 . H571 . 110.2 no C56 . C57 . H572 . 110.0 no C58 . C57 . H572 . 106.8 no H571 . C57 . H572 . 110.2 no C57 . C58 . C59 . 109.52(10) yes C57 . C58 . H581 . 107.6 no C59 . C58 . H581 . 108.2 no C57 . C58 . H582 . 109.9 no C59 . C58 . H582 . 110.2 no H581 . C58 . H582 . 111.3 no C58 . C59 . C60 . 109.51(10) yes C58 . C59 . H591 . 107.7 no C60 . C59 . H591 . 109.9 no C58 . C59 . H592 . 109.3 no C60 . C59 . H592 . 109.7 no H591 . C59 . H592 . 110.7 no C59 . C60 . C61 . 109.54(10) yes C59 . C60 . H601 . 109.6 no C61 . C60 . H601 . 109.9 no C59 . C60 . H602 . 108.2 no C61 . C60 . H602 . 107.7 no H601 . C60 . H602 . 111.8 no C60 . C61 . C62 . 109.49(10) yes C60 . C61 . H611 . 108.8 no C62 . C61 . H611 . 109.2 no C60 . C61 . H612 . 109.5 no C62 . C61 . H612 . 110.0 no H611 . C61 . H612 . 109.9 no C61 . C62 . S2 . 111.3(7) yes C61 . C62 . O2 . 125.6(9) yes S2 . C62 . O2 . 123.0(9) 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 C23 . H231 . C7 1_554 167 0.93 2.57 3.477(14) yes C45 . H451 . O2 3_455 152 0.93 2.53 3.382(14) yes _iucr_refine_instructions_details ; # # Punched on 14/02/17 at 16:48:42 # #LIST 12 BLOCK SCALE X'S U'S RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 15,X'S) H ( 151,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 33,X'S) H ( 331,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 43,X'S) H ( 431,X'S) RIDE C ( 44,X'S) H ( 441,X'S) RIDE C ( 45,X'S) H ( 451,X'S) RIDE C ( 52,X'S) H ( 521,X'S) H ( 522,X'S) RIDE C ( 53,X'S) H ( 531,X'S) H ( 532,X'S) RIDE C ( 54,X'S) H ( 541,X'S) H ( 542,X'S) RIDE C ( 55,X'S) H ( 551,X'S) H ( 552,X'S) RIDE C ( 56,X'S) H ( 561,X'S) H ( 562,X'S) RIDE C ( 57,X'S) H ( 571,X'S) H ( 572,X'S) RIDE C ( 58,X'S) H ( 581,X'S) H ( 582,X'S) RIDE C ( 59,X'S) H ( 591,X'S) H ( 592,X'S) RIDE C ( 60,X'S) H ( 601,X'S) H ( 602,X'S) RIDE C ( 61,X'S) H ( 611,X'S) H ( 612,X'S) END # # Punched on 14/02/17 at 16:48:42 # #LIST 16 DIST 1.54,0.01 = CONT C(52) TO C(53) C(53) TO C(54) C(54) TO C(55) C(55) TO C(56) C(56) TO C(57) CONT C(57) TO C(58) C(58) TO C(59) C(59) TO C(60) C(60) TO C(61) ANGLE 109.5,0.1 = CONT C(51) TO C(52) TO C(53) C(52) TO C(53) TO C(54) C(53) TO C(54) TO C(55) CONT C(54) TO C(55) TO C(56) C(55) TO C(56) TO C(57) C(56) TO C(57) TO C(58) CONT C(57) TO C(58) TO C(59) C(58) TO C(59) TO C(60) C(59) TO C(60) TO C(61) CONT C(60) TO C(61) TO C(62) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) VIBR .0, 0.00200 = S(1) TO C(51) VIBR .0, 0.00500 = C(51) TO C(36) VIBR .0, 0.00200 = S(2) TO C(62) VIBR .0, 0.00500 = C(62) TO C(46) VIBR .0, 0.00200 = O(1) TO C(51) VIBR .0, 0.00200 = O(2) TO C(62) VIBR .0, 0.00200 = C(51) TO C(52) VIBR .0, 0.00500 = O(1) TO S(1) VIBR .0, 0.00500 = C(52) TO S(1) VIBR .0, 0.00500 = C(52) TO O(1) VIBR .0, 0.00200 = C(52) TO C(53) VIBR .0, 0.00500 = C(53) TO C(51) VIBR .0, 0.00200 = C(53) TO C(54) VIBR .0, 0.00500 = C(54) TO C(52) VIBR .0, 0.00200 = C(54) TO C(55) VIBR .0, 0.00500 = C(55) TO C(53) VIBR .0, 0.00200 = C(55) TO C(56) VIBR .0, 0.00500 = C(56) TO C(54) VIBR .0, 0.00200 = C(56) TO C(57) VIBR .0, 0.00500 = C(57) TO C(55) VIBR .0, 0.00200 = C(57) TO C(58) VIBR .0, 0.00500 = C(58) TO C(56) VIBR .0, 0.00200 = C(58) TO C(59) VIBR .0, 0.00500 = C(59) TO C(57) VIBR .0, 0.00200 = C(59) TO C(60) VIBR .0, 0.00500 = C(60) TO C(58) VIBR .0, 0.00200 = C(60) TO C(61) VIBR .0, 0.00500 = C(61) TO C(59) VIBR .0, 0.00200 = C(61) TO C(62) VIBR .0, 0.00500 = C(62) TO C(60) VIBR .0, 0.00500 = S(2) TO C(61) VIBR .0, 0.00500 = O(2) TO C(61) VIBR .0, 0.00500 = O(2) TO S(2) U(IJ) .0, 0.04000 = S(1) TO C(51) U(IJ) .0, 0.04000 = S(2) TO C(62) U(IJ) .0, 0.08000 = O(1) TO C(51) U(IJ) .0, 0.08000 = O(2) TO C(62) U(IJ) .0, 0.04000 = C(51) TO C(52) U(IJ) .0, 0.04000 = C(52) TO C(53) U(IJ) .0, 0.04000 = C(53) TO C(54) U(IJ) .0, 0.04000 = C(54) TO C(55) U(IJ) .0, 0.04000 = C(55) TO C(56) U(IJ) .0, 0.04000 = C(56) TO C(57) U(IJ) .0, 0.04000 = C(57) TO C(58) U(IJ) .0, 0.04000 = C(58) TO C(59) U(IJ) .0, 0.04000 = C(59) TO C(60) U(IJ) .0, 0.04000 = C(60) TO C(61) U(IJ) .0, 0.04000 = C(61) TO C(62) END ; # Manually omitted reflections loop_ _oxford_refln_omitted_index_h _oxford_refln_omitted_index_k _oxford_refln_omitted_index_l _oxford_refln_omitted_flag _oxford_refln_omitted_details 1 4 2 x . 0 12 1 x . 1 10 0 x . #============================================================================== data_6c-II #============================================================================== _audit_creation_date "2017-02-13" _audit_creation_method CRYSTALS_ver_14.61_build_6019 _oxford_structure_analysis_title '6702' _chemical_name_systematic . _chemical_melting_point 'not measured' loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.120 0.250 -0.043 525 82 ' ' 2 0.107 0.750 0.043 525 82 ' ' 3 -0.116 0.250 0.457 525 82 ' ' 4 0.121 0.750 0.543 525 82 ' ' _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ; The discrete Fourier transform of the void region were treated as contributions to the A and B parts of the calculated structure factors. ; _refine_special_details ; The difference map indicated the presence of diffuse electron density believed to be disordered methanol. SQUEEZE was used leaving a void from which the electron density was removed. ; _cell_length_a 12.1123(2) _cell_length_b 25.4859(5) _cell_length_c 31.6032(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 9755.7(3) _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'P c c n ' _symmetry_space_group_name_Hall '-P 2ab 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 'x,-y+1/2,z+1/2' '-x,y+1/2,-z+1/2' '-x+1/2,-y+1/2,z' 'x+1/2,y+1/2,-z' 'x+1/2,-y,-z+1/2' '-x+1/2,y,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 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0311 0.0180 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 0.0492 0.0322 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 0.3331 0.5567 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 -1.5491 0.6778 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' _cell_formula_units_Z 8 # Given Formula = C48 H48 N5 O2 S2 Zn1 # Dc = 1.17 Fooo = 3592.00 Mu = 18.08 M = 856.45 # Found Formula = C49 H43 N5 O2 S2 Zn1 # Dc = 1.18 FOOO = 3600.00 Mu = 18.15 M = 863.42 _chemical_formula_sum 'C49 H43 N5 O2 S2 Zn1' _chemical_formula_moiety 'C49 H43 N5 O2 S2 Zn1' _chemical_compound_source . _chemical_formula_weight 863.42 _cell_measurement_reflns_used 15666 _cell_measurement_theta_min 4 _cell_measurement_theta_max 76 _cell_measurement_temperature 150 _exptl_crystal_description 'lath' _exptl_crystal_colour 'clear_intense_red' _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.22 _exptl_crystal_density_diffrn 1.176 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 3600 _exptl_absorpt_coefficient_mu 1.815 # Sheldrick geometric approximatio 0.76 0.96 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro, (Agilent, 2011)' _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_T_max 0.96 _diffrn_measurement_device_type 'Oxford Diffraction SuperNova' _diffrn_measurement_device 'Area' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlisPro, (Agilent, 2011)' _computing_data_reduction 'CrysAlisPro, (Agilent, 2011)' _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 150 _diffrn_reflns_number 84406 _reflns_number_total 10136 _diffrn_reflns_av_R_equivalents 0.063 _diffrn_reflns_av_sigmaI/netI 0.0954 # Number of reflections with Friedels Law is 10136 # Theoretical number of reflections is about 20413 _diffrn_reflns_theta_min 4.041 _diffrn_reflns_theta_max 76.165 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 74.642 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 35 _reflns_limit_h_min 0 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 31 _reflns_limit_l_min 0 _reflns_limit_l_max 39 _oxford_diffrn_Wilson_B_factor 2.71 _oxford_diffrn_Wilson_scale 0.42 _atom_sites_solution_primary Other #heavy,direct,difmap,geom,iterative # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.51 _refine_diff_density_max 0.59 # 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>-3.0\s(I) _refine_ls_number_reflns 10088 _refine_ls_number_restraints 0 _refine_ls_number_parameters 532 _oxford_refine_ls_R_factor_ref 0.0668 _refine_ls_wR_factor_ref 0.1297 _refine_ls_goodness_of_fit_ref 1.0486 _refine_ls_shift/su_max 0.0015009 _refine_ls_shift/su_mean 0.0000417 # The values computed with all filters except I/sigma _oxford_reflns_number_all 10098 _refine_ls_R_factor_all 0.0671 _refine_ls_wR_factor_all 0.1302 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 7807 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_gt 0.1157 # 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 Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr #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^) + ( 0.04P)^2^ +12.99P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # 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. Agilent (2011). CrysAlisPro. Oxford Diffraction, (2010). Supernova User Manual. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. 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 atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Zn1 Zn 0.69551(3) 0.585051(13) 0.225451(11) 0.0277 1.0000 Uani . . . . . . N1 N 0.58174(18) 0.62249(8) 0.26447(7) 0.0288 1.0000 Uani . . . . . . N2 N 0.58070(17) 0.58687(9) 0.17636(7) 0.0286 1.0000 Uani . . . . . . N3 N 0.77715(18) 0.52759(8) 0.19170(7) 0.0289 1.0000 Uani . . . . . . N4 N 0.77780(18) 0.56283(9) 0.27992(7) 0.0304 1.0000 Uani . . . . . . N5 N 0.79272(18) 0.65131(9) 0.20718(8) 0.0320 1.0000 Uani . . . . . . C1 C 0.5956(2) 0.63523(10) 0.30628(9) 0.0309 1.0000 Uani . . . . . . C2 C 0.5050(2) 0.66863(11) 0.31976(10) 0.0344 1.0000 Uani . . . . . . C3 C 0.4382(2) 0.67437(11) 0.28608(10) 0.0358 1.0000 Uani . . . . . . C4 C 0.4861(2) 0.64584(10) 0.25121(9) 0.0307 1.0000 Uani . . . . . . C5 C 0.4417(2) 0.64266(10) 0.21076(9) 0.0319 1.0000 Uani . . . . . . C6 C 0.4856(2) 0.61576(10) 0.17600(9) 0.0311 1.0000 Uani . . . . . . C7 C 0.4376(2) 0.61448(12) 0.13439(10) 0.0375 1.0000 Uani . . . . . . C8 C 0.5039(2) 0.58447(12) 0.10990(9) 0.0361 1.0000 Uani . . . . . . C9 C 0.5940(2) 0.56676(10) 0.13642(9) 0.0301 1.0000 Uani . . . . . . C10 C 0.6790(2) 0.53266(11) 0.12368(9) 0.0314 1.0000 Uani . . . . . . C11 C 0.7634(2) 0.51397(10) 0.15019(9) 0.0305 1.0000 Uani . . . . . . C12 C 0.8485(2) 0.47709(11) 0.13788(9) 0.0346 1.0000 Uani . . . . . . C13 C 0.9125(2) 0.46885(11) 0.17225(9) 0.0352 1.0000 Uani . . . . . . C14 C 0.8670(2) 0.50031(10) 0.20610(9) 0.0317 1.0000 Uani . . . . . . C15 C 0.9076(2) 0.50121(11) 0.24731(10) 0.0344 1.0000 Uani . . . . . . C16 C 0.8659(2) 0.52941(10) 0.28131(9) 0.0332 1.0000 Uani . . . . . . C17 C 0.9085(3) 0.52705(12) 0.32388(10) 0.0382 1.0000 Uani . . . . . . C18 C 0.8462(3) 0.55910(11) 0.34781(10) 0.0384 1.0000 Uani . . . . . . C19 C 0.7634(2) 0.58142(10) 0.32012(9) 0.0325 1.0000 Uani . . . . . . C20 C 0.6807(2) 0.61692(10) 0.33273(9) 0.0315 1.0000 Uani . . . . . . C21 C 0.8303(2) 0.68524(12) 0.23597(11) 0.0409 1.0000 Uani . . . . . . C22 C 0.8903(3) 0.72951(13) 0.22456(13) 0.0521 1.0000 Uani . . . . . . C23 C 0.9118(3) 0.73849(14) 0.18260(14) 0.0604 1.0000 Uani . . . . . . C24 C 0.8749(3) 0.70301(15) 0.15276(13) 0.0580 1.0000 Uani . . . . . . C25 C 0.8156(3) 0.66004(12) 0.16645(10) 0.0429 1.0000 Uani . . . . . . C31 C 0.6787(2) 0.63277(11) 0.37827(9) 0.0335 1.0000 Uani . . . . . . C32 C 0.6000(3) 0.61129(13) 0.40549(10) 0.0419 1.0000 Uani . . . . . . C33 C 0.5969(3) 0.62408(14) 0.44797(10) 0.0503 1.0000 Uani . . . . . . C34 C 0.6733(3) 0.65935(14) 0.46432(11) 0.0505 1.0000 Uani . . . . . . C35 C 0.7515(3) 0.68128(13) 0.43823(10) 0.0444 1.0000 Uani . . . . . . C36 C 0.7554(2) 0.66817(11) 0.39542(9) 0.0359 1.0000 Uani . . . . . . C41 C 0.6741(2) 0.51254(12) 0.07914(9) 0.0336 1.0000 Uani . . . . . . C42 C 0.5982(3) 0.47375(13) 0.06818(10) 0.0446 1.0000 Uani . . . . . . C43 C 0.5891(3) 0.45533(16) 0.02738(11) 0.0531 1.0000 Uani . . . . . . C44 C 0.6560(3) 0.47570(17) -0.00402(12) 0.0577 1.0000 Uani . . . . . . C45 C 0.7327(3) 0.51363(15) 0.00587(10) 0.0500 1.0000 Uani . . . . . . C46 C 0.7438(3) 0.53127(13) 0.04722(10) 0.0392 1.0000 Uani . . . . . . S1 S 0.85418(6) 0.69913(3) 0.36235(2) 0.0381 1.0000 Uani . . . . . . S2 S 0.84826(6) 0.57812(3) 0.05846(2) 0.0408 1.0000 Uani . . . . . . O1 O 0.9871(2) 0.64786(11) 0.41457(9) 0.0584 1.0000 Uani . . . . . . O2 O 0.9663(2) 0.49150(10) 0.04661(8) 0.0510 1.0000 Uani . . . . . . C51 C 0.9817(3) 0.67866(13) 0.38583(11) 0.0453 1.0000 Uani . . . . . . C52 C 1.0793(3) 0.70664(14) 0.36630(12) 0.0513 1.0000 Uani . . . . . . C53 C 1.1813(3) 0.67243(16) 0.36250(13) 0.0560 1.0000 Uani . . . . . . C54 C 1.1676(3) 0.62600(15) 0.33298(12) 0.0545 1.0000 Uani . . . . . . C55 C 1.1259(3) 0.63899(14) 0.28890(12) 0.0515 1.0000 Uani . . . . . . C56 C 1.1520(3) 0.59658(13) 0.25684(12) 0.0481 1.0000 Uani . . . . . . C57 C 1.1028(3) 0.60678(14) 0.21355(12) 0.0501 1.0000 Uani . . . . . . C58 C 1.1419(3) 0.57063(14) 0.17830(12) 0.0502 1.0000 Uani . . . . . . C59 C 1.0863(3) 0.58234(15) 0.13627(12) 0.0525 1.0000 Uani . . . . . . C60 C 1.1363(3) 0.55483(17) 0.09806(13) 0.0566 1.0000 Uani . . . . . . C61 C 1.0753(3) 0.56904(16) 0.05682(12) 0.0528 1.0000 Uani . . . . . . C62 C 0.9697(3) 0.53807(14) 0.05264(10) 0.0438 1.0000 Uani . . . . . . H21 H 0.4951 0.6829 0.3468 0.0409 1.0000 Uiso R . . . . . H31 H 0.3738 0.6931 0.2847 0.0423 1.0000 Uiso R . . . . . H51 H 0.3766 0.6605 0.2061 0.0373 1.0000 Uiso R . . . . . H71 H 0.3743 0.6305 0.1257 0.0450 1.0000 Uiso R . . . . . H81 H 0.4952 0.5769 0.0814 0.0420 1.0000 Uiso R . . . . . H121 H 0.8562 0.4625 0.1109 0.0411 1.0000 Uiso R . . . . . H131 H 0.9749 0.4470 0.1737 0.0420 1.0000 Uiso R . . . . . H151 H 0.9693 0.4799 0.2526 0.0408 1.0000 Uiso R . . . . . H171 H 0.9698 0.5071 0.3327 0.0460 1.0000 Uiso R . . . . . H181 H 0.8538 0.5660 0.3774 0.0455 1.0000 Uiso R . . . . . H211 H 0.8152 0.6792 0.2647 0.0482 1.0000 Uiso R . . . . . H221 H 0.9142 0.7523 0.2455 0.0630 1.0000 Uiso R . . . . . H231 H 0.9508 0.7683 0.1742 0.0720 1.0000 Uiso R . . . . . H241 H 0.8882 0.7078 0.1245 0.0701 1.0000 Uiso R . . . . . H251 H 0.7894 0.6363 0.1470 0.0507 1.0000 Uiso R . . . . . H321 H 0.5480 0.5879 0.3946 0.0489 1.0000 Uiso R . . . . . H331 H 0.5435 0.6097 0.4653 0.0597 1.0000 Uiso R . . . . . H341 H 0.6703 0.6678 0.4928 0.0607 1.0000 Uiso R . . . . . H351 H 0.8030 0.7048 0.4490 0.0529 1.0000 Uiso R . . . . . H421 H 0.5523 0.4604 0.0888 0.0524 1.0000 Uiso R . . . . . H431 H 0.5371 0.4300 0.0211 0.0636 1.0000 Uiso R . . . . . H441 H 0.6486 0.4647 -0.0320 0.0688 1.0000 Uiso R . . . . . H451 H 0.7773 0.5271 -0.0151 0.0595 1.0000 Uiso R . . . . . H521 H 1.0963 0.7363 0.3844 0.0619 1.0000 Uiso R . . . . . H522 H 1.0591 0.7192 0.3383 0.0614 1.0000 Uiso R . . . . . H531 H 1.2433 0.6946 0.3523 0.0670 1.0000 Uiso R . . . . . H532 H 1.1986 0.6593 0.3908 0.0669 1.0000 Uiso R . . . . . H541 H 1.2409 0.6091 0.3303 0.0647 1.0000 Uiso R . . . . . H542 H 1.1147 0.6023 0.3463 0.0648 1.0000 Uiso R . . . . . H551 H 1.1588 0.6720 0.2797 0.0617 1.0000 Uiso R . . . . . H552 H 1.0467 0.6437 0.2909 0.0610 1.0000 Uiso R . . . . . H561 H 1.2326 0.5941 0.2545 0.0578 1.0000 Uiso R . . . . . H562 H 1.1227 0.5634 0.2673 0.0579 1.0000 Uiso R . . . . . H571 H 1.1234 0.6427 0.2055 0.0596 1.0000 Uiso R . . . . . H572 H 1.0227 0.6054 0.2160 0.0597 1.0000 Uiso R . . . . . H581 H 1.2203 0.5747 0.1744 0.0601 1.0000 Uiso R . . . . . H582 H 1.1260 0.5345 0.1862 0.0601 1.0000 Uiso R . . . . . H591 H 1.0892 0.6199 0.1311 0.0627 1.0000 Uiso R . . . . . H592 H 1.0091 0.5724 0.1386 0.0624 1.0000 Uiso R . . . . . H601 H 1.2125 0.5660 0.0951 0.0681 1.0000 Uiso R . . . . . H602 H 1.1349 0.5171 0.1027 0.0676 1.0000 Uiso R . . . . . H611 H 1.0579 0.6067 0.0567 0.0625 1.0000 Uiso R . . . . . H612 H 1.1213 0.5601 0.0328 0.0633 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 Zn1 0.02706(17) 0.02319(16) 0.03277(18) 0.00089(14) -0.00041(13) -0.00008(13) N1 0.0264(10) 0.0258(11) 0.0342(12) -0.0001(9) 0.0010(9) -0.0009(8) N2 0.0253(10) 0.0259(10) 0.0348(11) 0.0016(9) -0.0008(8) -0.0030(8) N3 0.0302(11) 0.0237(10) 0.0327(11) -0.0001(9) 0.0017(9) 0.0031(8) N4 0.0319(11) 0.0250(10) 0.0344(12) 0.0007(9) -0.0019(9) 0.0031(8) N5 0.0296(11) 0.0229(10) 0.0436(13) 0.0009(9) -0.0021(9) -0.0013(9) C1 0.0332(13) 0.0232(12) 0.0362(14) -0.0004(10) 0.0032(11) -0.0030(10) C2 0.0356(14) 0.0282(13) 0.0394(15) -0.0027(11) 0.0045(11) 0.0005(11) C3 0.0296(13) 0.0284(13) 0.0495(17) -0.0011(12) 0.0053(12) 0.0015(10) C4 0.0253(12) 0.0248(12) 0.0421(15) 0.0012(11) 0.0024(11) -0.0010(10) C5 0.0212(11) 0.0281(13) 0.0465(16) 0.0025(11) -0.0014(10) 0.0022(10) C6 0.0253(12) 0.0277(13) 0.0402(15) 0.0040(11) -0.0015(10) -0.0017(10) C7 0.0316(14) 0.0376(15) 0.0433(16) 0.0046(13) -0.0059(12) 0.0019(11) C8 0.0349(14) 0.0395(15) 0.0338(14) 0.0047(12) -0.0028(11) -0.0047(12) C9 0.0281(12) 0.0297(13) 0.0324(13) 0.0025(10) -0.0004(10) -0.0057(10) C10 0.0317(13) 0.0301(13) 0.0323(13) 0.0015(11) 0.0024(10) -0.0054(10) C11 0.0319(13) 0.0256(12) 0.0341(14) 0.0015(10) 0.0038(10) -0.0026(10) C12 0.0385(14) 0.0292(13) 0.0361(14) -0.0023(11) 0.0051(12) 0.0015(11) C13 0.0344(14) 0.0323(14) 0.0388(15) -0.0002(11) 0.0040(11) 0.0062(11) C14 0.0323(13) 0.0248(12) 0.0379(15) 0.0016(11) 0.0013(11) 0.0027(10) C15 0.0348(14) 0.0246(12) 0.0438(15) 0.0017(11) -0.0027(12) 0.0060(10) C16 0.0353(14) 0.0267(13) 0.0377(15) 0.0022(11) -0.0010(11) 0.0021(10) C17 0.0399(15) 0.0331(14) 0.0416(16) 0.0014(12) -0.0075(12) 0.0104(12) C18 0.0454(16) 0.0325(14) 0.0373(15) 0.0021(12) -0.0068(12) 0.0055(12) C19 0.0379(14) 0.0262(12) 0.0335(13) 0.0015(11) -0.0026(11) -0.0028(11) C20 0.0335(14) 0.0262(13) 0.0348(14) -0.0012(10) 0.0016(11) -0.0027(10) C21 0.0360(15) 0.0340(15) 0.0527(18) -0.0044(13) -0.0034(13) -0.0029(12) C22 0.0483(18) 0.0347(16) 0.073(2) -0.0085(16) -0.0073(17) -0.0112(14) C23 0.058(2) 0.0394(19) 0.084(3) 0.0093(18) 0.002(2) -0.0211(16) C24 0.065(2) 0.051(2) 0.058(2) 0.0092(17) 0.0092(18) -0.0175(18) C25 0.0478(17) 0.0367(16) 0.0443(17) 0.0005(13) 0.0031(14) -0.0077(13) C31 0.0344(14) 0.0302(13) 0.0360(14) -0.0015(11) -0.0008(11) 0.0028(11) C32 0.0473(17) 0.0394(16) 0.0392(16) -0.0021(13) 0.0001(13) -0.0081(13) C33 0.061(2) 0.054(2) 0.0356(16) 0.0010(14) 0.0096(15) -0.0130(17) C34 0.068(2) 0.0503(19) 0.0336(16) -0.0059(14) 0.0019(15) -0.0056(16) C35 0.0518(18) 0.0387(15) 0.0427(17) -0.0052(13) -0.0040(14) -0.0027(14) C36 0.0388(14) 0.0311(13) 0.0380(15) 0.0006(11) 0.0012(12) 0.0031(12) C41 0.0313(13) 0.0379(14) 0.0318(14) 0.0010(11) -0.0005(10) 0.0023(11) C42 0.0432(17) 0.0483(18) 0.0422(17) -0.0043(14) 0.0025(13) -0.0066(14) C43 0.0467(18) 0.063(2) 0.0498(19) -0.0164(17) -0.0020(15) -0.0126(16) C44 0.054(2) 0.078(3) 0.0408(18) -0.0174(18) -0.0033(15) -0.0058(19) C45 0.0446(18) 0.069(2) 0.0360(16) -0.0031(16) 0.0054(13) -0.0013(16) C46 0.0344(14) 0.0457(17) 0.0376(15) 0.0002(13) 0.0003(12) -0.0019(13) S1 0.0379(4) 0.0343(3) 0.0420(4) 0.0008(3) -0.0011(3) -0.0022(3) S2 0.0405(4) 0.0434(4) 0.0384(4) 0.0023(3) 0.0053(3) -0.0043(3) O1 0.0498(14) 0.0580(15) 0.0673(17) 0.0147(13) -0.0028(12) 0.0105(12) O2 0.0513(13) 0.0528(15) 0.0488(13) -0.0043(11) 0.0069(10) 0.0022(11) C51 0.0472(17) 0.0368(16) 0.0519(19) -0.0023(14) -0.0042(14) 0.0048(13) C52 0.0436(18) 0.0492(19) 0.061(2) -0.0025(16) -0.0048(16) -0.0027(15) C53 0.0418(18) 0.063(2) 0.063(2) 0.0016(18) -0.0024(16) 0.0040(16) C54 0.0448(18) 0.056(2) 0.063(2) 0.0040(17) -0.0021(16) 0.0093(16) C55 0.0430(18) 0.0482(19) 0.063(2) 0.0042(16) -0.0054(15) 0.0047(14) C56 0.0355(15) 0.0455(18) 0.063(2) 0.0052(15) -0.0024(14) 0.0011(13) C57 0.0407(17) 0.0467(18) 0.063(2) 0.0021(16) -0.0033(15) 0.0025(14) C58 0.0331(15) 0.0484(19) 0.069(2) -0.0013(16) 0.0037(15) -0.0013(13) C59 0.0466(18) 0.0497(19) 0.061(2) -0.0008(17) 0.0029(16) 0.0003(15) C60 0.0367(17) 0.066(2) 0.067(2) -0.0111(19) 0.0029(16) -0.0006(16) C61 0.0403(17) 0.064(2) 0.054(2) -0.0029(17) 0.0133(15) -0.0061(15) C62 0.0405(16) 0.056(2) 0.0353(15) 0.0015(14) 0.0040(12) -0.0011(14) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 1.570(6) 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 . N1 . 2.081(2) yes Zn1 . N2 . 2.084(2) yes Zn1 . N3 . 2.064(2) yes Zn1 . N4 . 2.068(2) yes Zn1 . N5 . 2.138(2) yes N1 . C1 . 1.371(4) yes N1 . C4 . 1.368(3) yes N2 . C6 . 1.367(3) yes N2 . C9 . 1.372(4) yes N3 . C11 . 1.367(4) yes N3 . C14 . 1.369(3) yes N4 . C16 . 1.366(3) yes N4 . C19 . 1.367(4) yes N5 . C21 . 1.335(4) yes N5 . C25 . 1.335(4) yes C1 . C2 . 1.452(4) yes C1 . C20 . 1.407(4) yes C2 . C3 . 1.345(4) yes C2 . H21 . 0.937 no C3 . C4 . 1.442(4) yes C3 . H31 . 0.916 no C4 . C5 . 1.389(4) yes C5 . C6 . 1.400(4) yes C5 . H51 . 0.922 no C6 . C7 . 1.438(4) yes C7 . C8 . 1.352(4) yes C7 . H71 . 0.911 no C8 . C9 . 1.448(4) yes C8 . H81 . 0.926 no C9 . C10 . 1.406(4) yes C10 . C11 . 1.405(4) yes C10 . C41 . 1.499(4) yes C11 . C12 . 1.448(4) yes C12 . C13 . 1.351(4) yes C12 . H121 . 0.936 no C13 . C14 . 1.446(4) yes C13 . H131 . 0.940 no C14 . C15 . 1.392(4) yes C15 . C16 . 1.388(4) yes C15 . H151 . 0.938 no C16 . C17 . 1.442(4) yes C17 . C18 . 1.345(4) yes C17 . H171 . 0.942 no C18 . C19 . 1.447(4) yes C18 . H181 . 0.957 no C19 . C20 . 1.408(4) yes C20 . C31 . 1.495(4) yes C21 . C22 . 1.389(4) yes C21 . H211 . 0.939 no C22 . C23 . 1.371(6) yes C22 . H221 . 0.927 no C23 . C24 . 1.381(6) yes C23 . H231 . 0.933 no C24 . C25 . 1.380(4) yes C24 . H241 . 0.915 no C25 . H251 . 0.917 no C31 . C32 . 1.396(4) yes C31 . C36 . 1.404(4) yes C32 . C33 . 1.382(5) yes C32 . H321 . 0.933 no C33 . C34 . 1.390(5) yes C33 . H331 . 0.923 no C34 . C35 . 1.375(5) yes C34 . H341 . 0.927 no C35 . C36 . 1.394(4) yes C35 . H351 . 0.930 no C36 . S1 . 1.773(3) yes C41 . C42 . 1.394(4) yes C41 . C46 . 1.399(4) yes C42 . C43 . 1.377(5) yes C42 . H421 . 0.921 no C43 . C44 . 1.382(5) yes C43 . H431 . 0.923 no C44 . C45 . 1.377(5) yes C44 . H441 . 0.931 no C45 . C46 . 1.389(4) yes C45 . H451 . 0.920 no C46 . S2 . 1.775(3) yes S1 . C51 . 1.791(3) yes S2 . C62 . 1.800(3) yes O1 . C51 . 1.202(4) yes O2 . C62 . 1.203(4) yes C51 . C52 . 1.512(5) yes C52 . C53 . 1.518(5) yes C52 . H521 . 0.969 no C52 . H522 . 0.971 no C53 . C54 . 1.516(5) yes C53 . H531 . 0.992 no C53 . H532 . 0.977 no C54 . C55 . 1.518(5) yes C54 . H541 . 0.990 no C54 . H542 . 0.975 no C55 . C56 . 1.515(5) yes C55 . H551 . 0.974 no C55 . H552 . 0.970 no C56 . C57 . 1.515(5) yes C56 . H561 . 0.981 no C56 . H562 . 0.974 no C57 . C58 . 1.521(5) yes C57 . H571 . 0.982 no C57 . H572 . 0.974 no C58 . C59 . 1.519(5) yes C58 . H581 . 0.963 no C58 . H582 . 0.973 no C59 . C60 . 1.522(5) yes C59 . H591 . 0.971 no C59 . H592 . 0.971 no C60 . C61 . 1.541(5) yes C60 . H601 . 0.971 no C60 . H602 . 0.974 no C61 . C62 . 1.509(5) yes C61 . H611 . 0.982 no C61 . H612 . 0.968 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Zn1 . N2 . 89.38(9) yes N1 . Zn1 . N3 . 161.60(9) yes N2 . Zn1 . N3 . 87.18(9) yes N1 . Zn1 . N4 . 87.22(9) yes N2 . Zn1 . N4 . 161.32(9) yes N3 . Zn1 . N4 . 90.28(9) yes N1 . Zn1 . N5 . 99.35(9) yes N2 . Zn1 . N5 . 98.56(9) yes N3 . Zn1 . N5 . 99.03(9) yes N4 . Zn1 . N5 . 100.12(9) yes Zn1 . N1 . C1 . 126.78(18) yes Zn1 . N1 . C4 . 125.35(19) yes C1 . N1 . C4 . 107.2(2) yes Zn1 . N2 . C6 . 125.47(19) yes Zn1 . N2 . C9 . 126.74(17) yes C6 . N2 . C9 . 107.0(2) yes Zn1 . N3 . C11 . 128.14(18) yes Zn1 . N3 . C14 . 124.70(18) yes C11 . N3 . C14 . 106.7(2) yes Zn1 . N4 . C16 . 125.03(19) yes Zn1 . N4 . C19 . 128.11(18) yes C16 . N4 . C19 . 106.6(2) yes Zn1 . N5 . C21 . 121.0(2) yes Zn1 . N5 . C25 . 120.4(2) yes C21 . N5 . C25 . 118.6(3) yes N1 . C1 . C2 . 109.2(2) yes N1 . C1 . C20 . 125.7(2) yes C2 . C1 . C20 . 125.0(3) yes C1 . C2 . C3 . 106.6(3) yes C1 . C2 . H21 . 126.4 no C3 . C2 . H21 . 127.0 no C2 . C3 . C4 . 108.0(2) yes C2 . C3 . H31 . 127.4 no C4 . C3 . H31 . 124.6 no C3 . C4 . N1 . 109.0(2) yes C3 . C4 . C5 . 125.2(3) yes N1 . C4 . C5 . 125.8(3) yes C4 . C5 . C6 . 127.1(2) yes C4 . C5 . H51 . 116.6 no C6 . C5 . H51 . 116.3 no C5 . C6 . N2 . 125.3(3) yes C5 . C6 . C7 . 125.1(3) yes N2 . C6 . C7 . 109.6(2) yes C6 . C7 . C8 . 107.2(2) yes C6 . C7 . H71 . 127.3 no C8 . C7 . H71 . 125.5 no C7 . C8 . C9 . 107.0(3) yes C7 . C8 . H81 . 127.3 no C9 . C8 . H81 . 125.7 no C8 . C9 . N2 . 109.1(2) yes C8 . C9 . C10 . 125.4(3) yes N2 . C9 . C10 . 125.5(2) yes C9 . C10 . C11 . 124.9(3) yes C9 . C10 . C41 . 116.8(2) yes C11 . C10 . C41 . 118.2(2) yes C10 . C11 . N3 . 125.1(2) yes C10 . C11 . C12 . 125.3(3) yes N3 . C11 . C12 . 109.6(2) yes C11 . C12 . C13 . 107.1(2) yes C11 . C12 . H121 . 125.0 no C13 . C12 . H121 . 127.9 no C12 . C13 . C14 . 106.9(2) yes C12 . C13 . H131 . 126.4 no C14 . C13 . H131 . 126.8 no C13 . C14 . N3 . 109.8(2) yes C13 . C14 . C15 . 124.5(3) yes N3 . C14 . C15 . 125.7(3) yes C14 . C15 . C16 . 127.2(3) yes C14 . C15 . H151 . 116.1 no C16 . C15 . H151 . 116.8 no C15 . C16 . N4 . 125.6(3) yes C15 . C16 . C17 . 124.8(3) yes N4 . C16 . C17 . 109.6(2) yes C16 . C17 . C18 . 107.4(3) yes C16 . C17 . H171 . 125.4 no C18 . C17 . H171 . 127.2 no C17 . C18 . C19 . 106.7(3) yes C17 . C18 . H181 . 127.4 no C19 . C18 . H181 . 125.9 no C18 . C19 . N4 . 109.7(2) yes C18 . C19 . C20 . 125.1(3) yes N4 . C19 . C20 . 125.2(3) yes C19 . C20 . C1 . 124.5(3) yes C19 . C20 . C31 . 117.2(2) yes C1 . C20 . C31 . 118.1(2) yes N5 . C21 . C22 . 121.8(3) yes N5 . C21 . H211 . 119.1 no C22 . C21 . H211 . 119.1 no C21 . C22 . C23 . 119.1(3) yes C21 . C22 . H221 . 119.2 no C23 . C22 . H221 . 121.7 no C22 . C23 . C24 . 119.4(3) yes C22 . C23 . H231 . 120.5 no C24 . C23 . H231 . 120.2 no C23 . C24 . C25 . 118.3(4) yes C23 . C24 . H241 . 121.5 no C25 . C24 . H241 . 120.2 no C24 . C25 . N5 . 122.9(3) yes C24 . C25 . H251 . 119.5 no N5 . C25 . H251 . 117.6 no C20 . C31 . C32 . 119.9(3) yes C20 . C31 . C36 . 122.3(3) yes C32 . C31 . C36 . 117.8(3) yes C31 . C32 . C33 . 121.7(3) yes C31 . C32 . H321 . 119.0 no C33 . C32 . H321 . 119.4 no C32 . C33 . C34 . 119.7(3) yes C32 . C33 . H331 . 120.1 no C34 . C33 . H331 . 120.1 no C33 . C34 . C35 . 119.9(3) yes C33 . C34 . H341 . 119.1 no C35 . C34 . H341 . 121.0 no C34 . C35 . C36 . 120.5(3) yes C34 . C35 . H351 . 120.4 no C36 . C35 . H351 . 119.1 no C31 . C36 . C35 . 120.4(3) yes C31 . C36 . S1 . 120.3(2) yes C35 . C36 . S1 . 119.2(2) yes C10 . C41 . C42 . 120.1(3) yes C10 . C41 . C46 . 122.4(3) yes C42 . C41 . C46 . 117.5(3) yes C41 . C42 . C43 . 121.8(3) yes C41 . C42 . H421 . 119.0 no C43 . C42 . H421 . 119.2 no C42 . C43 . C44 . 119.8(3) yes C42 . C43 . H431 . 119.5 no C44 . C43 . H431 . 120.6 no C43 . C44 . C45 . 119.8(3) yes C43 . C44 . H441 . 120.7 no C45 . C44 . H441 . 119.5 no C44 . C45 . C46 . 120.4(3) yes C44 . C45 . H451 . 119.6 no C46 . C45 . H451 . 120.0 no C41 . C46 . C45 . 120.6(3) yes C41 . C46 . S2 . 121.0(2) yes C45 . C46 . S2 . 118.4(2) yes C36 . S1 . C51 . 101.99(15) yes C46 . S2 . C62 . 100.39(15) yes S1 . C51 . O1 . 123.4(3) yes S1 . C51 . C52 . 111.6(2) yes O1 . C51 . C52 . 125.0(3) yes C51 . C52 . C53 . 113.5(3) yes C51 . C52 . H521 . 107.1 no C53 . C52 . H521 . 108.7 no C51 . C52 . H522 . 109.3 no C53 . C52 . H522 . 108.8 no H521 . C52 . H522 . 109.5 no C52 . C53 . C54 . 114.1(3) yes C52 . C53 . H531 . 108.4 no C54 . C53 . H531 . 109.1 no C52 . C53 . H532 . 107.4 no C54 . C53 . H532 . 108.7 no H531 . C53 . H532 . 109.2 no C53 . C54 . C55 . 115.5(3) yes C53 . C54 . H541 . 107.1 no C55 . C54 . H541 . 108.3 no C53 . C54 . H542 . 106.9 no C55 . C54 . H542 . 108.1 no H541 . C54 . H542 . 110.9 no C54 . C55 . C56 . 112.9(3) yes C54 . C55 . H551 . 109.0 no C56 . C55 . H551 . 109.4 no C54 . C55 . H552 . 107.2 no C56 . C55 . H552 . 109.8 no H551 . C55 . H552 . 108.5 no C55 . C56 . C57 . 113.6(3) yes C55 . C56 . H561 . 107.6 no C57 . C56 . H561 . 109.6 no C55 . C56 . H562 . 108.4 no C57 . C56 . H562 . 108.3 no H561 . C56 . H562 . 109.4 no C56 . C57 . C58 . 115.8(3) yes C56 . C57 . H571 . 107.1 no C58 . C57 . H571 . 107.2 no C56 . C57 . H572 . 108.3 no C58 . C57 . H572 . 110.3 no H571 . C57 . H572 . 107.8 no C57 . C58 . C59 . 112.5(3) yes C57 . C58 . H581 . 109.7 no C59 . C58 . H581 . 107.6 no C57 . C58 . H582 . 108.9 no C59 . C58 . H582 . 108.7 no H581 . C58 . H582 . 109.2 no C58 . C59 . C60 . 115.3(3) yes C58 . C59 . H591 . 108.9 no C60 . C59 . H591 . 107.9 no C58 . C59 . H592 . 108.0 no C60 . C59 . H592 . 108.9 no H591 . C59 . H592 . 107.7 no C59 . C60 . C61 . 111.9(3) yes C59 . C60 . H601 . 108.6 no C61 . C60 . H601 . 107.8 no C59 . C60 . H602 . 109.2 no C61 . C60 . H602 . 110.6 no H601 . C60 . H602 . 108.7 no C60 . C61 . C62 . 110.9(3) yes C60 . C61 . H611 . 109.5 no C62 . C61 . H611 . 109.2 no C60 . C61 . H612 . 109.4 no C62 . C61 . H612 . 107.2 no H611 . C61 . H612 . 110.6 no C61 . C62 . S2 . 112.8(3) yes C61 . C62 . O2 . 124.0(3) yes S2 . C62 . O2 . 123.2(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 C12 . H121 . O2 . 132 0.94 2.54 3.239(5) yes _iucr_refine_instructions_details ; # # Punched on 13/02/17 at 11:01:04 # #LIST 12 BLOCK SCALE X'S U'S RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 15,X'S) H ( 151,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 33,X'S) H ( 331,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 43,X'S) H ( 431,X'S) RIDE C ( 44,X'S) H ( 441,X'S) RIDE C ( 45,X'S) H ( 451,X'S) RIDE C ( 52,X'S) H ( 521,X'S) H ( 522,X'S) RIDE C ( 53,X'S) H ( 531,X'S) H ( 532,X'S) RIDE C ( 54,X'S) H ( 541,X'S) H ( 542,X'S) RIDE C ( 55,X'S) H ( 551,X'S) H ( 552,X'S) RIDE C ( 56,X'S) H ( 561,X'S) H ( 562,X'S) RIDE C ( 57,X'S) H ( 571,X'S) H ( 572,X'S) RIDE C ( 58,X'S) H ( 581,X'S) H ( 582,X'S) RIDE C ( 59,X'S) H ( 591,X'S) H ( 592,X'S) RIDE C ( 60,X'S) H ( 601,X'S) H ( 602,X'S) RIDE C ( 61,X'S) H ( 611,X'S) H ( 612,X'S) END # # Punched on 13/02/17 at 11:01:04 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; #============================================================================== data_7a #============================================================================== _audit_creation_date "2017-01-25" _audit_creation_method CRYSTALS_ver_14.61_build_6019 _oxford_structure_analysis_title '6545' _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 8.6098(2) _cell_length_b 14.9172(3) _cell_length_c 16.4216(4) _cell_angle_alpha 84.6169(18) _cell_angle_beta 83.5040(18) _cell_angle_gamma 81.8061(18) _cell_volume 2067.68(8) _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 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0311 0.0180 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 0.0492 0.0322 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' Zn -1.5491 0.6778 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' S 0.3331 0.5567 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' Br -0.6763 1.2805 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C49.50 H45 Br1 N4.50 O4.50 S1 Zn1 # Dc = 1.53 Fooo = 981.00 Mu = 28.71 M = 952.28 # Found Formula = C46 H35 Br2 N5 O2 S2 Zn1 # Dc = 1.57 FOOO = 988.00 Mu = 43.97 M = 979.14 _chemical_formula_sum 'C46 H35 Br2 N5 O2 S2 Zn1' _chemical_formula_moiety 'C46 H35 Br2 N5 O2 S2 Zn1' _chemical_compound_source . _chemical_formula_weight 979.14 _cell_measurement_reflns_used 23386 _cell_measurement_theta_min 3 _cell_measurement_theta_max 76 _cell_measurement_temperature 150 _exptl_crystal_description 'plate' _exptl_crystal_colour 'clear_intense_red' _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_max 0.18 _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 4.397 # Sheldrick geometric approximatio 0.70 0.92 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro, (Agilent, 2011)' _exptl_absorpt_correction_T_min 0.55 _exptl_absorpt_correction_T_max 0.92 _diffrn_measurement_device_type 'Oxford Diffraction SuperNova' _diffrn_measurement_device 'Area' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54180 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlisPro, (Agilent, 2011)' _computing_data_reduction 'CrysAlisPro, (Agilent, 2011)' _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 150 _diffrn_reflns_number 47763 _reflns_number_total 8608 _diffrn_reflns_av_R_equivalents 0.031 # Number of reflections with Friedels Law is 8608 # Theoretical number of reflections is about 17350 _diffrn_reflns_theta_min 3.002 _diffrn_reflns_theta_max 76.357 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 74.830 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min -18 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _oxford_diffrn_Wilson_B_factor 2.11 _oxford_diffrn_Wilson_scale 0.11 _atom_sites_solution_primary Other #heavy,direct,difmap,geom,iterative # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.55 _refine_diff_density_max 0.89 # 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>-3.0\s(I) _refine_ls_number_reflns 8608 _refine_ls_number_restraints 0 _refine_ls_number_parameters 523 _oxford_refine_ls_R_factor_ref 0.0295 _refine_ls_wR_factor_ref 0.0713 _refine_ls_goodness_of_fit_ref 0.9997 _refine_ls_shift/su_max 0.0016521 _refine_ls_shift/su_mean 0.0000624 # The values computed with all filters except I/sigma _oxford_reflns_number_all 8608 _refine_ls_R_factor_all 0.0295 _refine_ls_wR_factor_all 0.0713 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 7953 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_gt 0.0693 # 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 Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr #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^) + ( 0.04P)^2^ + 1.76P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # 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. Agilent (2011). CrysAlisPro. Oxford Diffraction, (2010). Supernova User Manual. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. 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 atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Zn1 Zn 0.96007(2) 0.734945(14) 0.305108(13) 0.0182 1.0000 Uani . . . . . . N1 N 0.84061(17) 0.79742(10) 0.40606(9) 0.0213 1.0000 Uani . . . . . . N2 N 0.89546(17) 0.61269(10) 0.35952(9) 0.0202 1.0000 Uani . . . . . . N3 N 1.00521(17) 0.67722(10) 0.19409(9) 0.0214 1.0000 Uani . . . . . . N4 N 0.95363(17) 0.86107(10) 0.24108(9) 0.0221 1.0000 Uani . . . . . . N5 N 1.19540(17) 0.72490(10) 0.33531(9) 0.0227 1.0000 Uani . . . . . . C1 C 0.8098(2) 0.88924(12) 0.41455(12) 0.0243 1.0000 Uani . . . . . . C2 C 0.7422(2) 0.90473(13) 0.49701(13) 0.0307 1.0000 Uani . . . . . . C3 C 0.7349(2) 0.82261(13) 0.53842(12) 0.0302 1.0000 Uani . . . . . . C4 C 0.7938(2) 0.75534(12) 0.48105(11) 0.0231 1.0000 Uani . . . . . . C5 C 0.7967(2) 0.66105(12) 0.49560(11) 0.0236 1.0000 Uani . . . . . . C6 C 0.8409(2) 0.59434(12) 0.44015(11) 0.0221 1.0000 Uani . . . . . . C7 C 0.8311(2) 0.49812(12) 0.45611(12) 0.0280 1.0000 Uani . . . . . . C8 C 0.8794(2) 0.45997(12) 0.38494(12) 0.0279 1.0000 Uani . . . . . . C9 C 0.9180(2) 0.53149(12) 0.32419(11) 0.0225 1.0000 Uani . . . . . . C10 C 0.9684(2) 0.51929(12) 0.24120(11) 0.0239 1.0000 Uani . . . . . . C11 C 1.0061(2) 0.58774(12) 0.18089(11) 0.0235 1.0000 Uani . . . . . . C12 C 1.0551(2) 0.57368(13) 0.09544(12) 0.0291 1.0000 Uani . . . . . . C13 C 1.0867(2) 0.65418(13) 0.05807(12) 0.0289 1.0000 Uani . . . . . . C14 C 1.0553(2) 0.71903(12) 0.11973(11) 0.0232 1.0000 Uani . . . . . . C15 C 1.0691(2) 0.81165(12) 0.10761(11) 0.0235 1.0000 Uani . . . . . . C16 C 1.0214(2) 0.87854(12) 0.16270(11) 0.0233 1.0000 Uani . . . . . . C17 C 1.0267(2) 0.97495(13) 0.14599(13) 0.0297 1.0000 Uani . . . . . . C18 C 0.9585(2) 1.01471(13) 0.21400(13) 0.0311 1.0000 Uani . . . . . . C19 C 0.9136(2) 0.94361(12) 0.27363(12) 0.0245 1.0000 Uani . . . . . . C20 C 0.8417(2) 0.95747(12) 0.35298(12) 0.0253 1.0000 Uani . . . . . . C21 C 1.2622(3) 0.79901(14) 0.34140(16) 0.0384 1.0000 Uani . . . . . . C22 C 1.4197(3) 0.79539(17) 0.35314(18) 0.0473 1.0000 Uani . . . . . . C23 C 1.5101(2) 0.71227(18) 0.35872(15) 0.0422 1.0000 Uani . . . . . . C24 C 1.4424(3) 0.63494(16) 0.35382(15) 0.0391 1.0000 Uani . . . . . . C25 C 1.2844(2) 0.64424(13) 0.34166(12) 0.0285 1.0000 Uani . . . . . . C31 C 0.7956(2) 1.05457(12) 0.37226(12) 0.0274 1.0000 Uani . . . . . . C32 C 0.8912(3) 1.09809(15) 0.41384(15) 0.0384 1.0000 Uani . . . . . . C33 C 0.8525(3) 1.18930(16) 0.42814(17) 0.0446 1.0000 Uani . . . . . . C34 C 0.7188(3) 1.23867(14) 0.39948(16) 0.0401 1.0000 Uani . . . . . . C35 C 0.6226(2) 1.19694(13) 0.35766(15) 0.0352 1.0000 Uani . . . . . . C36 C 0.6582(2) 1.10470(13) 0.34569(12) 0.0276 1.0000 Uani . . . . . . C41 C 0.9877(2) 0.42475(12) 0.21396(11) 0.0267 1.0000 Uani . . . . . . C42 C 1.1396(3) 0.37985(13) 0.19636(13) 0.0323 1.0000 Uani . . . . . . C43 C 1.1646(3) 0.29352(14) 0.16833(14) 0.0383 1.0000 Uani . . . . . . C44 C 1.0364(3) 0.25099(14) 0.15800(14) 0.0407 1.0000 Uani . . . . . . C45 C 0.8848(3) 0.29339(14) 0.17586(13) 0.0374 1.0000 Uani . . . . . . C46 C 0.8596(3) 0.38055(13) 0.20321(12) 0.0301 1.0000 Uani . . . . . . Br1 Br 0.71572(3) 0.619192(14) 0.603369(12) 0.0363 1.0000 Uani . . . . . . Br2 Br 1.15661(3) 0.851798(14) 0.000880(12) 0.0314 1.0000 Uani . . . . . . S1 S 0.52163(6) 1.04816(3) 0.30362(3) 0.0304 1.0000 Uani . . . . . . S2 S 0.66335(6) 0.43577(4) 0.22181(3) 0.0349 1.0000 Uani . . . . . . O1 O 0.6236(2) 1.14030(13) 0.16695(11) 0.0532 1.0000 Uani . . . . . . O2 O 0.7272(3) 0.48139(13) 0.06335(10) 0.0563 1.0000 Uani . . . . . . C51 C 0.5474(3) 1.08200(15) 0.19592(14) 0.0364 1.0000 Uani . . . . . . C52 C 0.4716(3) 1.02219(19) 0.14778(17) 0.0498 1.0000 Uani . . . . . . C53 C 0.5993(3) 0.94080(19) 0.12251(18) 0.0520 1.0000 Uani . . . . . . C54 C 0.5297(3) 0.86259(19) 0.09543(18) 0.0506 1.0000 Uani . . . . . . C55 C 0.6529(3) 0.78636(19) 0.07028(18) 0.0504 1.0000 Uani . . . . . . C56 C 0.5927(3) 0.69740(19) 0.05344(17) 0.0520 1.0000 Uani . . . . . . C57 C 0.5089(3) 0.65424(19) 0.12969(18) 0.0514 1.0000 Uani . . . . . . C58 C 0.4806(3) 0.55620(17) 0.12211(16) 0.0449 1.0000 Uani . . . . . . C59 C 0.6323(3) 0.49228(15) 0.12187(14) 0.0390 1.0000 Uani . . . . . . H21 H 0.7087 0.9623 0.5175 0.0370 1.0000 Uiso R . . . . . H31 H 0.6995 0.8113 0.5932 0.0364 1.0000 Uiso R . . . . . H71 H 0.7971 0.4692 0.5071 0.0341 1.0000 Uiso R . . . . . H81 H 0.8880 0.3976 0.3748 0.0327 1.0000 Uiso R . . . . . H121 H 1.0625 0.5183 0.0720 0.0352 1.0000 Uiso R . . . . . H131 H 1.1199 0.6659 0.0034 0.0352 1.0000 Uiso R . . . . . H171 H 1.0691 1.0037 0.0977 0.0359 1.0000 Uiso R . . . . . H181 H 0.9435 1.0763 0.2223 0.0370 1.0000 Uiso R . . . . . H211 H 1.1974 0.8552 0.3378 0.0469 1.0000 Uiso R . . . . . H221 H 1.4640 0.8479 0.3580 0.0574 1.0000 Uiso R . . . . . H231 H 1.6160 0.7082 0.3652 0.0511 1.0000 Uiso R . . . . . H241 H 1.4984 0.5780 0.3580 0.0470 1.0000 Uiso R . . . . . H251 H 1.2346 0.5937 0.3367 0.0336 1.0000 Uiso R . . . . . H321 H 0.9835 1.0657 0.4320 0.0457 1.0000 Uiso R . . . . . H331 H 0.9180 1.2171 0.4566 0.0531 1.0000 Uiso R . . . . . H341 H 0.6916 1.2999 0.4079 0.0484 1.0000 Uiso R . . . . . H351 H 0.5325 1.2296 0.3377 0.0412 1.0000 Uiso R . . . . . H421 H 1.2265 0.4078 0.2039 0.0378 1.0000 Uiso R . . . . . H431 H 1.2684 0.2629 0.1567 0.0458 1.0000 Uiso R . . . . . H441 H 1.0533 0.1937 0.1378 0.0492 1.0000 Uiso R . . . . . H451 H 0.7986 0.2642 0.1703 0.0447 1.0000 Uiso R . . . . . H521 H 0.4304 1.0575 0.1022 0.0596 1.0000 Uiso R . . . . . H522 H 0.3855 0.9989 0.1834 0.0597 1.0000 Uiso R . . . . . H531 H 0.6722 0.9658 0.0759 0.0633 1.0000 Uiso R . . . . . H532 H 0.6589 0.9148 0.1719 0.0634 1.0000 Uiso R . . . . . H541 H 0.4647 0.8879 0.0487 0.0620 1.0000 Uiso R . . . . . H542 H 0.4604 0.8407 0.1435 0.0607 1.0000 Uiso R . . . . . H551 H 0.7175 0.8084 0.0203 0.0601 1.0000 Uiso R . . . . . H552 H 0.7180 0.7705 0.1161 0.0604 1.0000 Uiso R . . . . . H561 H 0.6831 0.6521 0.0327 0.0636 1.0000 Uiso R . . . . . H562 H 0.5154 0.7079 0.0102 0.0638 1.0000 Uiso R . . . . . H571 H 0.5814 0.6577 0.1740 0.0625 1.0000 Uiso R . . . . . H572 H 0.4052 0.6934 0.1426 0.0623 1.0000 Uiso R . . . . . H581 H 0.4105 0.5388 0.1703 0.0541 1.0000 Uiso R . . . . . H582 H 0.4335 0.5521 0.0731 0.0540 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 Zn1 0.01817(11) 0.01640(11) 0.02002(11) -0.00031(8) -0.00258(8) -0.00226(8) N1 0.0206(7) 0.0194(7) 0.0232(7) -0.0020(5) -0.0014(5) -0.0010(5) N2 0.0217(7) 0.0183(7) 0.0206(7) -0.0006(5) -0.0017(5) -0.0033(5) N3 0.0249(7) 0.0188(7) 0.0208(7) 0.0000(5) -0.0026(5) -0.0043(5) N4 0.0233(7) 0.0177(7) 0.0244(7) 0.0008(5) -0.0029(6) -0.0009(5) N5 0.0193(7) 0.0234(7) 0.0255(7) -0.0013(6) -0.0041(6) -0.0023(5) C1 0.0232(8) 0.0203(8) 0.0292(9) -0.0046(7) -0.0022(7) -0.0010(6) C2 0.0335(10) 0.0250(9) 0.0325(10) -0.0082(8) 0.0028(8) -0.0015(7) C3 0.0349(10) 0.0274(9) 0.0265(9) -0.0050(7) 0.0048(8) -0.0021(8) C4 0.0219(8) 0.0245(9) 0.0220(8) -0.0021(7) -0.0010(6) -0.0009(6) C5 0.0229(8) 0.0247(9) 0.0209(8) 0.0023(7) -0.0004(6) 0.0001(7) C6 0.0214(8) 0.0210(8) 0.0228(8) 0.0022(6) -0.0022(6) -0.0016(6) C7 0.0343(10) 0.0215(9) 0.0261(9) 0.0035(7) 0.0012(7) -0.0034(7) C8 0.0346(10) 0.0192(8) 0.0292(9) 0.0009(7) -0.0013(7) -0.0048(7) C9 0.0240(8) 0.0178(8) 0.0259(9) -0.0004(6) -0.0030(7) -0.0041(6) C10 0.0278(9) 0.0199(8) 0.0249(9) -0.0025(7) -0.0033(7) -0.0055(7) C11 0.0271(8) 0.0211(8) 0.0231(8) -0.0033(7) -0.0029(7) -0.0050(7) C12 0.0387(10) 0.0256(9) 0.0233(9) -0.0051(7) -0.0018(7) -0.0043(8) C13 0.0379(10) 0.0276(9) 0.0205(8) -0.0012(7) -0.0011(7) -0.0037(8) C14 0.0248(8) 0.0242(9) 0.0202(8) 0.0005(7) -0.0027(6) -0.0028(7) C15 0.0238(8) 0.0252(9) 0.0206(8) 0.0046(7) -0.0031(6) -0.0038(7) C16 0.0232(8) 0.0206(8) 0.0255(9) 0.0047(7) -0.0051(7) -0.0025(6) C17 0.0341(10) 0.0208(9) 0.0324(10) 0.0057(7) -0.0007(8) -0.0041(7) C18 0.0363(10) 0.0179(8) 0.0376(11) 0.0023(7) -0.0009(8) -0.0030(7) C19 0.0246(8) 0.0171(8) 0.0313(9) 0.0003(7) -0.0049(7) -0.0009(6) C20 0.0240(8) 0.0195(8) 0.0323(10) -0.0025(7) -0.0043(7) -0.0011(6) C21 0.0308(10) 0.0253(10) 0.0620(15) -0.0056(9) -0.0166(10) -0.0032(8) C22 0.0370(12) 0.0407(12) 0.0703(17) 0.0010(11) -0.0230(11) -0.0159(10) C23 0.0224(9) 0.0563(14) 0.0488(13) 0.0023(11) -0.0125(9) -0.0057(9) C24 0.0287(10) 0.0402(12) 0.0458(12) 0.0009(9) -0.0112(9) 0.0076(8) C25 0.0272(9) 0.0242(9) 0.0335(10) 0.0007(7) -0.0062(7) -0.0008(7) C31 0.0316(9) 0.0195(8) 0.0305(9) -0.0025(7) 0.0003(7) -0.0035(7) C32 0.0400(11) 0.0276(10) 0.0494(13) -0.0064(9) -0.0113(10) -0.0037(8) C33 0.0498(13) 0.0315(11) 0.0566(15) -0.0133(10) -0.0076(11) -0.0116(10) C34 0.0404(11) 0.0200(9) 0.0592(14) -0.0115(9) 0.0082(10) -0.0062(8) C35 0.0303(10) 0.0224(9) 0.0497(12) -0.0039(8) 0.0059(9) 0.0001(7) C36 0.0276(9) 0.0216(9) 0.0326(10) -0.0031(7) 0.0021(7) -0.0038(7) C41 0.0395(10) 0.0200(8) 0.0211(8) -0.0010(6) -0.0020(7) -0.0074(7) C42 0.0414(11) 0.0256(9) 0.0305(10) -0.0048(8) -0.0031(8) -0.0047(8) C43 0.0513(13) 0.0258(10) 0.0353(11) -0.0038(8) 0.0000(9) 0.0009(9) C44 0.0668(15) 0.0219(9) 0.0338(11) -0.0056(8) 0.0017(10) -0.0099(9) C45 0.0577(14) 0.0298(10) 0.0289(10) -0.0041(8) -0.0027(9) -0.0198(9) C46 0.0416(11) 0.0264(9) 0.0234(9) 0.0006(7) -0.0019(8) -0.0110(8) Br1 0.05107(13) 0.02642(11) 0.02372(10) 0.00382(8) 0.00949(9) 0.00675(9) Br2 0.04161(12) 0.03059(11) 0.02163(10) 0.00474(7) -0.00047(8) -0.01022(8) S1 0.0277(2) 0.0254(2) 0.0375(3) -0.00106(18) -0.00018(18) -0.00506(17) S2 0.0356(2) 0.0401(3) 0.0309(2) -0.0024(2) -0.00146(19) -0.0135(2) O1 0.0698(12) 0.0536(11) 0.0404(9) 0.0028(8) -0.0009(8) -0.0301(9) O2 0.0767(13) 0.0523(11) 0.0307(8) -0.0037(7) 0.0029(8) 0.0166(9) C51 0.0382(11) 0.0332(11) 0.0372(11) -0.0025(9) 0.0002(9) -0.0057(9) C52 0.0496(14) 0.0589(16) 0.0452(14) -0.0071(11) -0.0078(11) -0.0176(12) C53 0.0452(13) 0.0553(15) 0.0580(16) -0.0120(12) -0.0051(12) -0.0107(11) C54 0.0403(13) 0.0528(15) 0.0593(16) 0.0004(12) -0.0091(11) -0.0079(11) C55 0.0473(14) 0.0545(15) 0.0511(15) -0.0022(12) -0.0057(11) -0.0131(11) C56 0.0559(15) 0.0514(15) 0.0475(14) -0.0086(11) -0.0042(12) -0.0012(12) C57 0.0462(14) 0.0493(14) 0.0577(16) -0.0090(12) -0.0031(12) -0.0014(11) C58 0.0425(12) 0.0454(13) 0.0480(13) -0.0049(10) -0.0086(10) -0.0058(10) C59 0.0505(13) 0.0340(11) 0.0344(11) -0.0074(9) -0.0073(10) -0.0063(9) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 2.705(13) 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 . N1 . 2.0750(15) yes Zn1 . N2 . 2.0748(14) yes Zn1 . N3 . 2.0627(15) yes Zn1 . N4 . 2.0641(14) yes Zn1 . N5 . 2.1214(14) yes N1 . C1 . 1.375(2) yes N1 . C4 . 1.374(2) yes N2 . C6 . 1.370(2) yes N2 . C9 . 1.371(2) yes N3 . C11 . 1.371(2) yes N3 . C14 . 1.372(2) yes N4 . C16 . 1.369(2) yes N4 . C19 . 1.372(2) yes N5 . C21 . 1.333(3) yes N5 . C25 . 1.333(2) yes C1 . C2 . 1.438(3) yes C1 . C20 . 1.399(3) yes C2 . C3 . 1.350(3) yes C2 . H21 . 0.946 no C3 . C4 . 1.441(3) yes C3 . H31 . 0.924 no C4 . C5 . 1.401(3) yes C5 . C6 . 1.396(3) yes C5 . Br1 . 1.9092(17) yes C6 . C7 . 1.448(2) yes C7 . C8 . 1.345(3) yes C7 . H71 . 0.941 no C8 . C9 . 1.439(2) yes C8 . H81 . 0.951 no C9 . C10 . 1.403(3) yes C10 . C11 . 1.400(2) yes C10 . C41 . 1.501(2) yes C11 . C12 . 1.445(3) yes C12 . C13 . 1.345(3) yes C12 . H121 . 0.935 no C13 . C14 . 1.443(3) yes C13 . H131 . 0.920 no C14 . C15 . 1.397(3) yes C15 . C16 . 1.397(3) yes C15 . Br2 . 1.9057(17) yes C16 . C17 . 1.445(2) yes C17 . C18 . 1.349(3) yes C17 . H171 . 0.928 no C18 . C19 . 1.439(3) yes C18 . H181 . 0.931 no C19 . C20 . 1.398(3) yes C20 . C31 . 1.500(2) yes C21 . C22 . 1.384(3) yes C21 . H211 . 0.939 no C22 . C23 . 1.368(4) yes C22 . H221 . 0.932 no C23 . C24 . 1.377(3) yes C23 . H231 . 0.923 no C24 . C25 . 1.382(3) yes C24 . H241 . 0.915 no C25 . H251 . 0.932 no C31 . C32 . 1.388(3) yes C31 . C36 . 1.397(3) yes C32 . C33 . 1.389(3) yes C32 . H321 . 0.934 no C33 . C34 . 1.380(4) yes C33 . H331 . 0.934 no C34 . C35 . 1.379(3) yes C34 . H341 . 0.929 no C35 . C36 . 1.394(3) yes C35 . H351 . 0.931 no C36 . S1 . 1.774(2) yes C41 . C42 . 1.394(3) yes C41 . C46 . 1.398(3) yes C42 . C43 . 1.388(3) yes C42 . H421 . 0.932 no C43 . C44 . 1.382(3) yes C43 . H431 . 0.951 no C44 . C45 . 1.380(4) yes C44 . H441 . 0.932 no C45 . C46 . 1.395(3) yes C45 . H451 . 0.929 no C46 . S2 . 1.778(2) yes S1 . C51 . 1.791(2) yes S2 . C59 . 1.803(2) yes O1 . C51 . 1.195(3) yes O2 . C59 . 1.196(3) yes C51 . C52 . 1.504(3) yes C52 . C53 . 1.570(4) yes C52 . H521 . 0.947 no C52 . H522 . 0.975 no C53 . C54 . 1.508(4) yes C53 . H531 . 1.011 no C53 . H532 . 1.025 no C54 . C55 . 1.495(4) yes C54 . H541 . 1.013 no C54 . H542 . 0.993 no C55 . C56 . 1.550(4) yes C55 . H551 . 0.995 no C55 . H552 . 0.980 no C56 . C57 . 1.510(4) yes C56 . H561 . 1.006 no C56 . H562 . 1.014 no C57 . C58 . 1.535(4) yes C57 . H571 . 1.020 no C57 . H572 . 1.008 no C58 . C59 . 1.503(3) yes C58 . H581 . 0.978 no C58 . H582 . 0.953 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Zn1 . N2 . 88.22(6) yes N1 . Zn1 . N3 . 161.33(6) yes N2 . Zn1 . N3 . 88.84(6) yes N1 . Zn1 . N4 . 88.71(6) yes N2 . Zn1 . N4 . 162.15(6) yes N3 . Zn1 . N4 . 88.46(6) yes N1 . Zn1 . N5 . 100.05(6) yes N2 . Zn1 . N5 . 101.13(6) yes N3 . Zn1 . N5 . 98.61(6) yes N4 . Zn1 . N5 . 96.73(6) yes Zn1 . N1 . C1 . 126.67(12) yes Zn1 . N1 . C4 . 126.63(12) yes C1 . N1 . C4 . 106.28(15) yes Zn1 . N2 . C6 . 126.91(12) yes Zn1 . N2 . C9 . 126.23(12) yes C6 . N2 . C9 . 106.39(14) yes Zn1 . N3 . C11 . 127.15(12) yes Zn1 . N3 . C14 . 126.62(12) yes C11 . N3 . C14 . 105.96(15) yes Zn1 . N4 . C16 . 125.75(12) yes Zn1 . N4 . C19 . 126.45(12) yes C16 . N4 . C19 . 106.35(15) yes Zn1 . N5 . C21 . 121.11(13) yes Zn1 . N5 . C25 . 120.37(13) yes C21 . N5 . C25 . 118.26(16) yes N1 . C1 . C2 . 109.64(16) yes N1 . C1 . C20 . 125.38(17) yes C2 . C1 . C20 . 124.97(17) yes C1 . C2 . C3 . 107.34(17) yes C1 . C2 . H21 . 125.5 no C3 . C2 . H21 . 127.1 no C2 . C3 . C4 . 106.95(17) yes C2 . C3 . H31 . 126.8 no C4 . C3 . H31 . 126.2 no C3 . C4 . N1 . 109.76(16) yes C3 . C4 . C5 . 126.70(17) yes N1 . C4 . C5 . 123.46(16) yes C4 . C5 . C6 . 128.48(16) yes C4 . C5 . Br1 . 115.69(13) yes C6 . C5 . Br1 . 115.67(13) yes C5 . C6 . N2 . 123.50(16) yes C5 . C6 . C7 . 126.78(16) yes N2 . C6 . C7 . 109.67(16) yes C6 . C7 . C8 . 106.83(16) yes C6 . C7 . H71 . 125.4 no C8 . C7 . H71 . 127.8 no C7 . C8 . C9 . 107.39(16) yes C7 . C8 . H81 . 128.0 no C9 . C8 . H81 . 124.6 no C8 . C9 . N2 . 109.70(16) yes C8 . C9 . C10 . 124.63(16) yes N2 . C9 . C10 . 125.66(16) yes C9 . C10 . C11 . 125.72(16) yes C9 . C10 . C41 . 117.96(16) yes C11 . C10 . C41 . 116.30(16) yes C10 . C11 . N3 . 125.38(16) yes C10 . C11 . C12 . 124.66(17) yes N3 . C11 . C12 . 109.94(16) yes C11 . C12 . C13 . 107.04(17) yes C11 . C12 . H121 . 125.1 no C13 . C12 . H121 . 127.8 no C12 . C13 . C14 . 106.97(17) yes C12 . C13 . H131 . 126.5 no C14 . C13 . H131 . 126.5 no C13 . C14 . N3 . 110.06(16) yes C13 . C14 . C15 . 126.51(17) yes N3 . C14 . C15 . 123.42(16) yes C14 . C15 . C16 . 128.17(16) yes C14 . C15 . Br2 . 115.47(14) yes C16 . C15 . Br2 . 116.31(13) yes C15 . C16 . N4 . 123.47(16) yes C15 . C16 . C17 . 126.63(17) yes N4 . C16 . C17 . 109.82(16) yes C16 . C17 . C18 . 106.78(17) yes C16 . C17 . H171 . 126.4 no C18 . C17 . H171 . 126.8 no C17 . C18 . C19 . 107.29(17) yes C17 . C18 . H181 . 127.5 no C19 . C18 . H181 . 125.2 no C18 . C19 . N4 . 109.74(17) yes C18 . C19 . C20 . 124.59(17) yes N4 . C19 . C20 . 125.67(16) yes C1 . C20 . C19 . 125.73(17) yes C1 . C20 . C31 . 118.23(17) yes C19 . C20 . C31 . 116.04(16) yes N5 . C21 . C22 . 122.7(2) yes N5 . C21 . H211 . 117.1 no C22 . C21 . H211 . 120.2 no C21 . C22 . C23 . 118.5(2) yes C21 . C22 . H221 . 121.4 no C23 . C22 . H221 . 120.1 no C22 . C23 . C24 . 119.61(19) yes C22 . C23 . H231 . 120.1 no C24 . C23 . H231 . 120.3 no C23 . C24 . C25 . 118.4(2) yes C23 . C24 . H241 . 122.3 no C25 . C24 . H241 . 119.2 no C24 . C25 . N5 . 122.52(19) yes C24 . C25 . H251 . 121.2 no N5 . C25 . H251 . 116.3 no C20 . C31 . C32 . 121.05(18) yes C20 . C31 . C36 . 120.65(17) yes C32 . C31 . C36 . 118.25(18) yes C31 . C32 . C33 . 121.1(2) yes C31 . C32 . H321 . 119.4 no C33 . C32 . H321 . 119.5 no C32 . C33 . C34 . 120.0(2) yes C32 . C33 . H331 . 119.7 no C34 . C33 . H331 . 120.2 no C33 . C34 . C35 . 119.84(19) yes C33 . C34 . H341 . 121.3 no C35 . C34 . H341 . 118.9 no C34 . C35 . C36 . 120.2(2) yes C34 . C35 . H351 . 120.6 no C36 . C35 . H351 . 119.1 no C31 . C36 . C35 . 120.47(19) yes C31 . C36 . S1 . 119.36(14) yes C35 . C36 . S1 . 120.00(16) yes C10 . C41 . C42 . 118.76(17) yes C10 . C41 . C46 . 122.77(18) yes C42 . C41 . C46 . 118.44(18) yes C41 . C42 . C43 . 121.3(2) yes C41 . C42 . H421 . 119.8 no C43 . C42 . H421 . 118.9 no C42 . C43 . C44 . 119.4(2) yes C42 . C43 . H431 . 121.1 no C44 . C43 . H431 . 119.5 no C43 . C44 . C45 . 120.54(19) yes C43 . C44 . H441 . 119.3 no C45 . C44 . H441 . 120.1 no C44 . C45 . C46 . 120.1(2) yes C44 . C45 . H451 . 120.6 no C46 . C45 . H451 . 119.4 no C41 . C46 . C45 . 120.3(2) yes C41 . C46 . S2 . 120.42(15) yes C45 . C46 . S2 . 119.31(17) yes C36 . S1 . C51 . 103.64(10) yes C46 . S2 . C59 . 101.00(10) yes S1 . C51 . O1 . 123.81(19) yes S1 . C51 . C52 . 110.63(17) yes O1 . C51 . C52 . 125.4(2) yes C51 . C52 . C53 . 107.8(2) yes C51 . C52 . H521 . 108.8 no C53 . C52 . H521 . 113.3 no C51 . C52 . H522 . 108.2 no C53 . C52 . H522 . 109.4 no H521 . C52 . H522 . 109.3 no C52 . C53 . C54 . 113.2(2) yes C52 . C53 . H531 . 106.6 no C54 . C53 . H531 . 109.9 no C52 . C53 . H532 . 109.9 no C54 . C53 . H532 . 105.8 no H531 . C53 . H532 . 111.6 no C53 . C54 . C55 . 112.5(2) yes C53 . C54 . H541 . 106.9 no C55 . C54 . H541 . 111.6 no C53 . C54 . H542 . 106.2 no C55 . C54 . H542 . 109.2 no H541 . C54 . H542 . 110.2 no C54 . C55 . C56 . 116.3(2) yes C54 . C55 . H551 . 108.2 no C56 . C55 . H551 . 109.0 no C54 . C55 . H552 . 106.6 no C56 . C55 . H552 . 106.2 no H551 . C55 . H552 . 110.4 no C55 . C56 . C57 . 112.0(2) yes C55 . C56 . H561 . 110.5 no C57 . C56 . H561 . 108.2 no C55 . C56 . H562 . 112.3 no C57 . C56 . H562 . 106.7 no H561 . C56 . H562 . 106.9 no C56 . C57 . C58 . 114.1(2) yes C56 . C57 . H571 . 103.4 no C58 . C57 . H571 . 111.7 no C56 . C57 . H572 . 107.9 no C58 . C57 . H572 . 109.9 no H571 . C57 . H572 . 109.6 no C57 . C58 . C59 . 111.1(2) yes C57 . C58 . H581 . 107.2 no C59 . C58 . H581 . 108.4 no C57 . C58 . H582 . 110.6 no C59 . C58 . H582 . 109.2 no H581 . C58 . H582 . 110.2 no C58 . C59 . S2 . 112.76(17) yes C58 . C59 . O2 . 124.9(2) yes S2 . C59 . O2 . 122.31(19) 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 C45 . H451 . O1 1_545 162 0.93 2.55 3.448(3) yes C56 . H561 . O2 . 129 1.01 2.53 3.261(3) yes _iucr_refine_instructions_details ; # # Punched on 25/01/17 at 12:33:04 # #LIST 12 BLOCK SCALE X'S U'S RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 33,X'S) H ( 331,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 43,X'S) H ( 431,X'S) RIDE C ( 44,X'S) H ( 441,X'S) RIDE C ( 45,X'S) H ( 451,X'S) RIDE C ( 52,X'S) H ( 521,X'S) H ( 522,X'S) RIDE C ( 53,X'S) H ( 531,X'S) H ( 532,X'S) RIDE C ( 54,X'S) H ( 541,X'S) H ( 542,X'S) RIDE C ( 55,X'S) H ( 551,X'S) H ( 552,X'S) RIDE C ( 56,X'S) H ( 561,X'S) H ( 562,X'S) RIDE C ( 57,X'S) H ( 571,X'S) H ( 572,X'S) RIDE C ( 58,X'S) H ( 581,X'S) H ( 582,X'S) END # # Punched on 25/01/17 at 12:33:04 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; #============================================================================== data_7b #============================================================================== _audit_creation_date "2017-01-25" _audit_creation_method CRYSTALS_ver_14.61_build_6019 _oxford_structure_analysis_title '6544' _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 8.4714(1) _cell_length_b 12.5943(3) _cell_length_c 21.8373(4) _cell_angle_alpha 92.5573(17) _cell_angle_beta 96.0799(15) _cell_angle_gamma 98.6538(15) _cell_volume 2286.02(7) _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 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0311 0.0180 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 0.0492 0.0322 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' Zn -1.5491 0.6778 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' S 0.3331 0.5567 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' Br -0.6763 1.2805 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C11 H10 Br2 Cl3 N1 O1 S1 Zn0.50 # Dc = 0.73 Fooo = 486.00 Mu = 45.41 M = 503.13 # Found Formula = C48 H38.00 Br2 Cl3 N5 O2 S2 Zn1 # Dc = 1.62 FOOO = 1120.00 Mu = 56.31 M = 1112.54 _chemical_formula_sum 'C48 H38 Br2 Cl3 N5 O2 S2 Zn1' _chemical_formula_moiety 'C47 H37 Br2 N5 O2 S2 Zn, C H Cl3' _chemical_compound_source . _chemical_formula_weight 1112.54 _cell_measurement_reflns_used 30570 _cell_measurement_theta_min 4 _cell_measurement_theta_max 76 _cell_measurement_temperature 150 _exptl_crystal_description 'lath' _exptl_crystal_colour 'metallic_dark_purple' _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_max 0.45 _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1119.995 _exptl_absorpt_coefficient_mu 5.631 # Sheldrick geometric approximatio 0.29 0.80 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro, (Agilent, 2011)' _exptl_absorpt_correction_T_min 0.29 _exptl_absorpt_correction_T_max 0.80 _diffrn_measurement_device_type 'Oxford Diffraction SuperNova' _diffrn_measurement_device 'Area' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54180 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlisPro, (Agilent, 2011)' _computing_data_reduction 'CrysAlisPro, (Agilent, 2011)' _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 150 _diffrn_reflns_number 49844 _reflns_number_total 9489 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_av_sigmaI/netI 0.0392 # Number of reflections with Friedels Law is 9489 # Theoretical number of reflections is about 19132 _diffrn_reflns_theta_min 3.557 _diffrn_reflns_theta_max 76.154 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 73.869 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min -15 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 27 _oxford_diffrn_Wilson_B_factor 1.71 _oxford_diffrn_Wilson_scale 0.02 _atom_sites_solution_primary Other #heavy,direct,difmap,geom,iterative # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.07 _refine_diff_density_max 1.71 # 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>-3.0\s(I) _refine_ls_number_reflns 9489 _refine_ls_number_restraints 0 _refine_ls_number_parameters 587 _oxford_refine_ls_R_factor_ref 0.0377 _refine_ls_wR_factor_ref 0.0992 _refine_ls_goodness_of_fit_ref 1.0045 _refine_ls_shift/su_max 0.0008310 _refine_ls_shift/su_mean 0.0000372 # The values computed with all filters except I/sigma _oxford_reflns_number_all 9489 _refine_ls_R_factor_all 0.0377 _refine_ls_wR_factor_all 0.0992 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 9016 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_gt 0.0976 # 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 Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr #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^) + ( 0.06P)^2^ + 3.50P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # 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. Agilent (2011). CrysAlisPro. Oxford Diffraction, (2010). Supernova User Manual. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. 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 atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Zn1 Zn 0.57417(3) 0.64387(2) 0.270714(13) 0.0146 1.0000 Uani . . . . . . N1 N 0.6753(2) 0.63141(15) 0.36049(9) 0.0165 1.0000 Uani . . . . . . N2 N 0.6751(2) 0.80560(15) 0.27913(9) 0.0172 1.0000 Uani . . . . . . N3 N 0.5458(2) 0.65364(15) 0.17583(9) 0.0169 1.0000 Uani . . . . . . N4 N 0.5546(2) 0.47844(14) 0.25672(9) 0.0169 1.0000 Uani . . . . . . N5 N 0.3407(2) 0.66734(15) 0.28982(9) 0.0190 1.0000 Uani . . . . . . C1 C 0.6823(3) 0.53800(18) 0.39013(10) 0.0186 1.0000 Uani . . . . . . C2 C 0.7379(3) 0.5632(2) 0.45469(11) 0.0236 1.0000 Uani . . . . . . C3 C 0.7651(3) 0.67177(19) 0.46337(11) 0.0231 1.0000 Uani . . . . . . C4 C 0.7276(3) 0.71415(18) 0.40419(10) 0.0177 1.0000 Uani . . . . . . C5 C 0.7504(3) 0.82210(18) 0.39039(10) 0.0196 1.0000 Uani . . . . . . C6 C 0.7296(3) 0.86647(18) 0.33305(10) 0.0185 1.0000 Uani . . . . . . C7 C 0.7632(3) 0.97861(19) 0.32094(11) 0.0247 1.0000 Uani . . . . . . C8 C 0.7276(3) 0.98506(19) 0.25939(12) 0.0254 1.0000 Uani . . . . . . C9 C 0.6717(3) 0.87669(18) 0.23352(11) 0.0191 1.0000 Uani . . . . . . C10 C 0.6224(3) 0.84976(18) 0.17052(10) 0.0191 1.0000 Uani . . . . . . C11 C 0.5650(3) 0.74576(18) 0.14425(10) 0.0185 1.0000 Uani . . . . . . C12 C 0.5162(3) 0.71996(19) 0.07913(11) 0.0217 1.0000 Uani . . . . . . C13 C 0.4659(3) 0.61200(19) 0.07224(10) 0.0212 1.0000 Uani . . . . . . C14 C 0.4858(3) 0.57093(18) 0.13290(10) 0.0175 1.0000 Uani . . . . . . C15 C 0.4578(3) 0.46292(18) 0.14681(10) 0.0185 1.0000 Uani . . . . . . C16 C 0.4947(3) 0.41859(18) 0.20318(11) 0.0183 1.0000 Uani . . . . . . C17 C 0.4858(3) 0.30540(18) 0.21339(11) 0.0224 1.0000 Uani . . . . . . C18 C 0.5424(3) 0.29827(18) 0.27328(12) 0.0227 1.0000 Uani . . . . . . C19 C 0.5836(3) 0.40671(17) 0.30037(11) 0.0183 1.0000 Uani . . . . . . C20 C 0.6437(3) 0.43387(18) 0.36226(10) 0.0187 1.0000 Uani . . . . . . C21 C 0.2835(3) 0.6413(2) 0.34293(12) 0.0256 1.0000 Uani . . . . . . C22 C 0.1341(3) 0.6606(2) 0.35656(14) 0.0337 1.0000 Uani . . . . . . C23 C 0.0405(3) 0.7089(2) 0.31365(15) 0.0354 1.0000 Uani . . . . . . C24 C 0.0990(3) 0.7372(2) 0.25896(14) 0.0322 1.0000 Uani . . . . . . C25 C 0.2492(3) 0.7149(2) 0.24897(12) 0.0246 1.0000 Uani . . . . . . C31 C 0.6668(3) 0.34388(18) 0.40324(10) 0.0202 1.0000 Uani . . . . . . C32 C 0.5390(3) 0.2945(2) 0.43189(13) 0.0294 1.0000 Uani . . . . . . C33 C 0.5568(4) 0.2136(2) 0.47172(14) 0.0355 1.0000 Uani . . . . . . C34 C 0.7044(4) 0.1789(2) 0.48244(13) 0.0324 1.0000 Uani . . . . . . C35 C 0.8334(3) 0.2257(2) 0.45395(13) 0.0296 1.0000 Uani . . . . . . C36 C 0.8163(3) 0.30926(19) 0.41489(11) 0.0220 1.0000 Uani . . . . . . C41 C 0.6300(3) 0.94219(18) 0.12937(10) 0.0212 1.0000 Uani . . . . . . C42 C 0.4928(3) 0.9877(2) 0.11275(12) 0.0263 1.0000 Uani . . . . . . C43 C 0.4999(4) 1.0790(2) 0.07909(13) 0.0326 1.0000 Uani . . . . . . C44 C 0.6464(4) 1.1274(2) 0.06297(13) 0.0357 1.0000 Uani . . . . . . C45 C 0.7839(4) 1.0824(2) 0.07779(13) 0.0326 1.0000 Uani . . . . . . C46 C 0.7748(3) 0.9890(2) 0.11015(11) 0.0242 1.0000 Uani . . . . . . Br1 Br 0.83483(3) 0.922095(19) 0.458346(11) 0.0275 1.0000 Uani . . . . . . Br2 Br 0.36695(3) 0.362221(19) 0.079823(11) 0.0246 1.0000 Uani . . . . . . S1 S 0.98861(7) 0.37384(5) 0.38410(3) 0.0262 1.0000 Uani . . . . . . S2 S 0.95171(7) 0.93101(5) 0.12774(3) 0.0272 1.0000 Uani . . . . . . O1 O 0.8746(2) 0.22533(16) 0.29430(10) 0.0341 1.0000 Uani . . . . . . O2 O 0.8445(3) 0.84188(18) 0.01620(10) 0.0413 1.0000 Uani . . . . . . C51 C 0.9783(3) 0.2998(2) 0.31115(13) 0.0264 1.0000 Uani . . . . . . C52 C 1.1119(3) 0.3448(2) 0.27428(14) 0.0338 1.0000 Uani . . . . . . C53 C 1.0563(4) 0.4287(3) 0.23002(15) 0.0411 1.0000 Uani . . . . . . C54 C 0.9403(4) 0.3778(3) 0.17583(16) 0.0458 1.0000 Uani . . . . . . C55 C 0.8733(3) 0.4619(3) 0.13559(15) 0.0425 1.0000 Uani . . . . . . C56 C 1.0002(3) 0.5369(2) 0.10595(13) 0.0311 1.0000 Uani . . . . . . C57 C 0.9243(3) 0.5962(2) 0.05432(13) 0.0302 1.0000 Uani . . . . . . C58 C 1.0426(3) 0.6770(2) 0.02505(12) 0.0307 1.0000 Uani . . . . . . C59 C 1.0859(3) 0.7842(2) 0.06274(13) 0.0302 1.0000 Uani . . . . . . C60 C 0.9466(3) 0.8468(2) 0.05945(12) 0.0280 1.0000 Uani . . . . . . Cl1 Cl 0.62857(13) 1.06109(8) 0.63191(5) 0.0604 1.0000 Uani . . . . . . Cl2 Cl 0.81719(12) 0.88712(9) 0.62855(5) 0.0612 1.0000 Uani . . . . . . Cl3 Cl 0.7526(12) 0.9680(6) 0.7443(3) 0.0782 0.614(10) Uani . . P 1 1 . C61 C 0.7872(6) 0.9972(4) 0.6703(2) 0.0364 0.614(10) Uani . . P 1 1 . Cl4 Cl 0.7043(16) 0.9720(8) 0.7439(5) 0.0634 0.386(10) Uani . . P 1 2 . C62 C 0.6684(10) 0.9532(6) 0.6637(4) 0.0356 0.386(10) Uani . . P 1 2 . H21 H 0.7526 0.5127 0.4850 0.0285 1.0000 Uiso R . . . . . H31 H 0.7989 0.7109 0.5001 0.0281 1.0000 Uiso R . . . . . H71 H 0.8007 1.0358 0.3495 0.0298 1.0000 Uiso R . . . . . H81 H 0.7363 1.0472 0.2373 0.0302 1.0000 Uiso R . . . . . H121 H 0.5202 0.7692 0.0481 0.0258 1.0000 Uiso R . . . . . H131 H 0.4273 0.5709 0.0363 0.0255 1.0000 Uiso R . . . . . H171 H 0.4490 0.2510 0.1844 0.0275 1.0000 Uiso R . . . . . H181 H 0.5530 0.2358 0.2937 0.0277 1.0000 Uiso R . . . . . H211 H 0.3474 0.6086 0.3710 0.0309 1.0000 Uiso R . . . . . H221 H 0.0998 0.6412 0.3940 0.0403 1.0000 Uiso R . . . . . H231 H -0.0617 0.7219 0.3219 0.0423 1.0000 Uiso R . . . . . H241 H 0.0394 0.7697 0.2300 0.0393 1.0000 Uiso R . . . . . H251 H 0.2911 0.7336 0.2122 0.0289 1.0000 Uiso R . . . . . H321 H 0.4398 0.3181 0.4244 0.0355 1.0000 Uiso R . . . . . H331 H 0.4686 0.1826 0.4911 0.0431 1.0000 Uiso R . . . . . H341 H 0.7161 0.1243 0.5084 0.0388 1.0000 Uiso R . . . . . H351 H 0.9334 0.2014 0.4609 0.0366 1.0000 Uiso R . . . . . H421 H 0.3952 0.9563 0.1248 0.0315 1.0000 Uiso R . . . . . H431 H 0.4062 1.1078 0.0674 0.0386 1.0000 Uiso R . . . . . H441 H 0.6529 1.1914 0.0428 0.0430 1.0000 Uiso R . . . . . H451 H 0.8819 1.1144 0.0664 0.0388 1.0000 Uiso R . . . . . H521 H 1.2040 0.3804 0.3018 0.0414 1.0000 Uiso R . . . . . H522 H 1.1432 0.2863 0.2511 0.0412 1.0000 Uiso R . . . . . H531 H 1.1522 0.4705 0.2143 0.0494 1.0000 Uiso R . . . . . H532 H 0.9970 0.4788 0.2510 0.0494 1.0000 Uiso R . . . . . H541 H 1.0007 0.3305 0.1513 0.0557 1.0000 Uiso R . . . . . H542 H 0.8503 0.3304 0.1915 0.0559 1.0000 Uiso R . . . . . H551 H 0.8183 0.5072 0.1609 0.0510 1.0000 Uiso R . . . . . H552 H 0.7952 0.4222 0.1030 0.0516 1.0000 Uiso R . . . . . H561 H 1.0599 0.5886 0.1376 0.0373 1.0000 Uiso R . . . . . H562 H 1.0747 0.4951 0.0891 0.0367 1.0000 Uiso R . . . . . H571 H 0.8460 0.6343 0.0714 0.0364 1.0000 Uiso R . . . . . H572 H 0.8662 0.5423 0.0228 0.0362 1.0000 Uiso R . . . . . H581 H 1.1419 0.6484 0.0207 0.0362 1.0000 Uiso R . . . . . H582 H 0.9942 0.6905 -0.0163 0.0370 1.0000 Uiso R . . . . . H591 H 1.1772 0.8280 0.0471 0.0359 1.0000 Uiso R . . . . . H592 H 1.1183 0.7741 0.1051 0.0357 1.0000 Uiso R . . . . . H611 H 0.8868 1.0471 0.6724 0.0445 0.614(10) Uiso R . P 1 1 . H621 H 0.5685 0.9020 0.6553 0.0431 0.386(10) Uiso R . P 1 2 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01502(14) 0.01371(14) 0.01450(15) 0.00155(11) -0.00065(10) 0.00135(10) N1 0.0181(8) 0.0144(8) 0.0160(9) 0.0025(7) -0.0017(7) 0.0011(7) N2 0.0179(8) 0.0163(9) 0.0160(9) 0.0021(7) -0.0001(7) -0.0011(7) N3 0.0194(9) 0.0157(8) 0.0153(9) 0.0016(7) 0.0008(7) 0.0026(7) N4 0.0195(9) 0.0137(8) 0.0170(9) 0.0004(7) -0.0004(7) 0.0031(7) N5 0.0154(8) 0.0186(9) 0.0226(9) 0.0015(7) 0.0025(7) 0.0013(7) C1 0.0195(10) 0.0185(10) 0.0176(10) 0.0038(8) -0.0001(8) 0.0031(8) C2 0.0313(12) 0.0219(11) 0.0170(11) 0.0049(9) -0.0020(9) 0.0042(9) C3 0.0284(12) 0.0230(11) 0.0161(11) 0.0014(9) -0.0021(9) 0.0013(9) C4 0.0167(10) 0.0194(10) 0.0158(10) 0.0001(8) -0.0005(8) 0.0014(8) C5 0.0206(10) 0.0192(10) 0.0172(10) -0.0011(8) -0.0003(8) -0.0004(8) C6 0.0194(10) 0.0159(10) 0.0181(10) -0.0007(8) -0.0010(8) -0.0010(8) C7 0.0336(13) 0.0159(11) 0.0214(11) 0.0003(9) -0.0008(9) -0.0036(9) C8 0.0350(13) 0.0159(11) 0.0230(12) 0.0043(9) -0.0007(10) -0.0012(9) C9 0.0223(11) 0.0153(10) 0.0191(11) 0.0038(8) 0.0006(8) 0.0010(8) C10 0.0213(10) 0.0179(10) 0.0183(10) 0.0039(8) 0.0011(8) 0.0031(8) C11 0.0190(10) 0.0195(10) 0.0170(10) 0.0034(8) 0.0008(8) 0.0037(8) C12 0.0252(11) 0.0236(11) 0.0167(11) 0.0042(9) 0.0001(8) 0.0056(9) C13 0.0236(11) 0.0241(11) 0.0152(10) -0.0001(8) -0.0024(8) 0.0054(9) C14 0.0156(9) 0.0201(10) 0.0163(10) 0.0003(8) -0.0002(8) 0.0033(8) C15 0.0178(10) 0.0187(10) 0.0178(10) -0.0027(8) -0.0010(8) 0.0019(8) C16 0.0170(10) 0.0159(10) 0.0206(11) -0.0012(8) -0.0003(8) 0.0007(8) C17 0.0259(11) 0.0157(10) 0.0240(11) -0.0016(9) -0.0020(9) 0.0019(8) C18 0.0256(11) 0.0152(10) 0.0265(12) 0.0029(9) -0.0008(9) 0.0024(8) C19 0.0188(10) 0.0153(10) 0.0205(11) 0.0030(8) 0.0004(8) 0.0026(8) C20 0.0190(10) 0.0173(10) 0.0197(11) 0.0053(8) 0.0009(8) 0.0021(8) C21 0.0262(12) 0.0248(12) 0.0265(12) 0.0053(9) 0.006(1) 0.0032(9) C22 0.0323(14) 0.0334(14) 0.0377(15) 0.0049(11) 0.0164(11) 0.0030(11) C23 0.0218(12) 0.0345(14) 0.0515(17) -0.0010(12) 0.0113(12) 0.0060(10) C24 0.0243(12) 0.0336(14) 0.0401(15) 0.0057(11) -0.0001(11) 0.0110(10) C25 0.0213(11) 0.0283(12) 0.0247(12) 0.0044(9) 0.0018(9) 0.0055(9) C31 0.0264(11) 0.0164(10) 0.0173(10) 0.0030(8) 0.0006(8) 0.0026(8) C32 0.0284(12) 0.0251(12) 0.0372(14) 0.0108(11) 0.0091(11) 0.0060(10) C33 0.0430(16) 0.0291(14) 0.0391(15) 0.0157(12) 0.0190(13) 0.0069(11) C34 0.0472(16) 0.0236(12) 0.0297(13) 0.0135(10) 0.0091(12) 0.0095(11) C35 0.0339(13) 0.0241(12) 0.0319(13) 0.0092(10) -0.0015(11) 0.0097(10) C36 0.0256(11) 0.0185(10) 0.0210(11) 0.0033(9) 0.0002(9) 0.0016(9) C41 0.0299(12) 0.0172(10) 0.0157(10) 0.0021(8) -0.0015(9) 0.0035(9) C42 0.0316(13) 0.0227(11) 0.0243(12) 0.0030(9) 0.0002(10) 0.0052(10) C43 0.0424(15) 0.0277(13) 0.0296(13) 0.0053(11) -0.0021(11) 0.0151(11) C44 0.0546(18) 0.0237(13) 0.0297(14) 0.0123(10) 0.0009(12) 0.0081(12) C45 0.0422(15) 0.0278(13) 0.0276(13) 0.0120(10) 0.0058(11) 0.0009(11) C46 0.0302(12) 0.0220(11) 0.0201(11) 0.0048(9) 0.0014(9) 0.0039(9) Br1 0.04118(15) 0.01855(13) 0.01827(13) -0.00178(9) -0.00527(10) -0.00273(10) Br2 0.03151(14) 0.01952(13) 0.02019(13) -0.00425(9) -0.00633(9) 0.00384(9) S1 0.0216(3) 0.0237(3) 0.0320(3) 0.0057(2) 0.0000(2) 0.0001(2) S2 0.0266(3) 0.0320(3) 0.0228(3) 0.0061(2) 0.0000(2) 0.0044(2) O1 0.0359(10) 0.0279(9) 0.0375(11) 0.0029(8) 0.0064(8) 0.0000(8) O2 0.0442(12) 0.0481(12) 0.0318(11) -0.0035(9) -0.0114(9) 0.0207(10) C51 0.0249(12) 0.0229(12) 0.0323(13) 0.0084(10) 0.0020(10) 0.0053(9) C52 0.0253(12) 0.0399(15) 0.0387(15) 0.0127(12) 0.0075(11) 0.0072(11) C53 0.0386(16) 0.0405(16) 0.0437(17) 0.0088(13) 0.0070(13) 0.0009(13) C54 0.0436(17) 0.0464(18) 0.0450(18) 0.0100(14) 0.0062(14) -0.0038(14) C55 0.0251(13) 0.062(2) 0.0408(17) 0.0180(15) 0.0026(12) 0.0032(13) C56 0.0261(12) 0.0370(14) 0.0308(14) 0.0080(11) 0.0005(10) 0.0068(11) C57 0.0253(12) 0.0342(14) 0.0316(13) 0.0059(11) -0.0001(10) 0.0069(10) C58 0.0314(13) 0.0354(14) 0.0264(13) 0.0042(11) 0.0017(10) 0.0091(11) C59 0.0279(12) 0.0356(14) 0.0276(13) 0.0048(11) 0.0009(10) 0.0073(11) C60 0.0298(13) 0.0292(13) 0.0253(12) 0.0067(10) 0.0015(10) 0.0047(10) Cl1 0.0618(5) 0.0625(6) 0.0601(6) 0.0076(4) 0.0025(4) 0.0217(4) Cl2 0.0545(5) 0.0731(6) 0.0576(5) -0.0005(5) -0.0035(4) 0.0233(5) Cl3 0.138(6) 0.0618(17) 0.0249(11) -0.0023(10) 0.000(2) -0.007(2) C61 0.037(3) 0.031(2) 0.038(3) 0.0042(19) -0.002(2) -0.001(2) Cl4 0.104(5) 0.042(2) 0.0331(19) 0.0087(15) 0.005(2) -0.022(3) C62 0.041(5) 0.032(4) 0.032(4) 0.007(3) 0.004(3) -0.001(3) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 2.96(2) 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 . N1 . 2.0770(18) yes Zn1 . N2 . 2.0792(18) yes Zn1 . N3 . 2.0717(19) yes Zn1 . N4 . 2.0714(18) yes Zn1 . N5 . 2.1241(19) yes N1 . C1 . 1.374(3) yes N1 . C4 . 1.370(3) yes N2 . C6 . 1.373(3) yes N2 . C9 . 1.370(3) yes N3 . C11 . 1.374(3) yes N3 . C14 . 1.369(3) yes N4 . C16 . 1.369(3) yes N4 . C19 . 1.371(3) yes N5 . C21 . 1.339(3) yes N5 . C25 . 1.340(3) yes C1 . C2 . 1.444(3) yes C1 . C20 . 1.398(3) yes C2 . C3 . 1.354(3) yes C2 . H21 . 0.950 no C3 . C4 . 1.443(3) yes C3 . H31 . 0.918 no C4 . C5 . 1.395(3) yes C5 . C6 . 1.399(3) yes C5 . Br1 . 1.907(2) yes C6 . C7 . 1.440(3) yes C7 . C8 . 1.355(3) yes C7 . H71 . 0.926 no C8 . C9 . 1.444(3) yes C8 . H81 . 0.934 no C9 . C10 . 1.406(3) yes C10 . C11 . 1.401(3) yes C10 . C41 . 1.500(3) yes C11 . C12 . 1.446(3) yes C12 . C13 . 1.359(3) yes C12 . H121 . 0.939 no C13 . C14 . 1.446(3) yes C13 . H131 . 0.922 no C14 . C15 . 1.398(3) yes C15 . C16 . 1.399(3) yes C15 . Br2 . 1.909(2) yes C16 . C17 . 1.445(3) yes C17 . C18 . 1.356(3) yes C17 . H171 . 0.907 no C18 . C19 . 1.441(3) yes C18 . H181 . 0.933 no C19 . C20 . 1.401(3) yes C20 . C31 . 1.498(3) yes C21 . C22 . 1.384(4) yes C21 . H211 . 0.927 no C22 . C23 . 1.384(4) yes C22 . H221 . 0.927 no C23 . C24 . 1.381(4) yes C23 . H231 . 0.939 no C24 . C25 . 1.381(3) yes C24 . H241 . 0.917 no C25 . H251 . 0.937 no C31 . C32 . 1.387(3) yes C31 . C36 . 1.402(3) yes C32 . C33 . 1.384(4) yes C32 . H321 . 0.934 no C33 . C34 . 1.386(4) yes C33 . H331 . 0.940 no C34 . C35 . 1.383(4) yes C34 . H341 . 0.920 no C35 . C36 . 1.398(3) yes C35 . H351 . 0.943 no C36 . S1 . 1.773(2) yes C41 . C42 . 1.394(3) yes C41 . C46 . 1.394(3) yes C42 . C43 . 1.389(4) yes C42 . H421 . 0.931 no C43 . C44 . 1.386(4) yes C43 . H431 . 0.938 no C44 . C45 . 1.385(4) yes C44 . H441 . 0.932 no C45 . C46 . 1.395(3) yes C45 . H451 . 0.931 no C46 . S2 . 1.777(3) yes S1 . C51 . 1.797(3) yes S2 . C60 . 1.784(3) yes O1 . C51 . 1.200(3) yes O2 . C60 . 1.204(3) yes C51 . C52 . 1.514(4) yes C52 . C53 . 1.554(4) yes C52 . H521 . 0.970 no C52 . H522 . 0.961 no C53 . C54 . 1.508(5) yes C53 . H531 . 1.001 no C53 . H532 . 0.989 no C54 . C55 . 1.541(5) yes C54 . H541 . 1.011 no C54 . H542 . 0.995 no C55 . C56 . 1.538(4) yes C55 . H551 . 0.977 no C55 . H552 . 0.982 no C56 . C57 . 1.519(4) yes C56 . H561 . 0.971 no C56 . H562 . 0.972 no C57 . C58 . 1.529(4) yes C57 . H571 . 0.970 no C57 . H572 . 0.981 no C58 . C59 . 1.524(4) yes C58 . H581 . 0.975 no C58 . H582 . 0.984 no C59 . C60 . 1.513(4) yes C59 . H591 . 0.981 no C59 . H592 . 0.956 no Cl1 . C61 . 1.818(5) yes Cl1 . C62 . 1.617(8) yes Cl2 . C61 . 1.692(5) yes Cl2 . C62 . 1.826(8) yes Cl3 . C61 . 1.718(9) yes C61 . H611 . 0.968 no Cl4 . C62 . 1.745(14) yes C62 . H621 . 0.979 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Zn1 . N2 . 87.88(7) yes N1 . Zn1 . N3 . 162.16(7) yes N2 . Zn1 . N3 . 88.65(7) yes N1 . Zn1 . N4 . 88.76(7) yes N2 . Zn1 . N4 . 160.00(7) yes N3 . Zn1 . N4 . 88.54(7) yes N1 . Zn1 . N5 . 98.57(7) yes N2 . Zn1 . N5 . 96.29(7) yes N3 . Zn1 . N5 . 99.20(7) yes N4 . Zn1 . N5 . 103.71(7) yes Zn1 . N1 . C1 . 126.42(15) yes Zn1 . N1 . C4 . 126.70(15) yes C1 . N1 . C4 . 106.33(18) yes Zn1 . N2 . C6 . 126.63(15) yes Zn1 . N2 . C9 . 126.25(15) yes C6 . N2 . C9 . 106.03(18) yes Zn1 . N3 . C11 . 126.70(15) yes Zn1 . N3 . C14 . 126.36(15) yes C11 . N3 . C14 . 106.52(18) yes Zn1 . N4 . C16 . 126.29(15) yes Zn1 . N4 . C19 . 126.92(15) yes C16 . N4 . C19 . 106.50(18) yes Zn1 . N5 . C21 . 122.43(16) yes Zn1 . N5 . C25 . 119.42(16) yes C21 . N5 . C25 . 118.1(2) yes N1 . C1 . C2 . 109.8(2) yes N1 . C1 . C20 . 125.5(2) yes C2 . C1 . C20 . 124.7(2) yes C1 . C2 . C3 . 106.9(2) yes C1 . C2 . H21 . 126.2 no C3 . C2 . H21 . 126.9 no C2 . C3 . C4 . 107.0(2) yes C2 . C3 . H31 . 126.4 no C4 . C3 . H31 . 126.6 no C3 . C4 . N1 . 109.93(19) yes C3 . C4 . C5 . 126.8(2) yes N1 . C4 . C5 . 123.1(2) yes C4 . C5 . C6 . 128.9(2) yes C4 . C5 . Br1 . 115.37(17) yes C6 . C5 . Br1 . 115.57(16) yes C5 . C6 . N2 . 123.1(2) yes C5 . C6 . C7 . 126.6(2) yes N2 . C6 . C7 . 110.2(2) yes C6 . C7 . C8 . 106.8(2) yes C6 . C7 . H71 . 127.0 no C8 . C7 . H71 . 126.2 no C7 . C8 . C9 . 106.9(2) yes C7 . C8 . H81 . 127.3 no C9 . C8 . H81 . 125.8 no C8 . C9 . N2 . 110.0(2) yes C8 . C9 . C10 . 124.2(2) yes N2 . C9 . C10 . 125.8(2) yes C9 . C10 . C11 . 125.5(2) yes C9 . C10 . C41 . 115.8(2) yes C11 . C10 . C41 . 118.6(2) yes C10 . C11 . N3 . 125.7(2) yes C10 . C11 . C12 . 124.5(2) yes N3 . C11 . C12 . 109.8(2) yes C11 . C12 . C13 . 106.8(2) yes C11 . C12 . H121 . 125.8 no C13 . C12 . H121 . 127.5 no C12 . C13 . C14 . 106.9(2) yes C12 . C13 . H131 . 127.9 no C14 . C13 . H131 . 125.1 no C13 . C14 . N3 . 109.90(19) yes C13 . C14 . C15 . 126.3(2) yes N3 . C14 . C15 . 123.7(2) yes C14 . C15 . C16 . 128.1(2) yes C14 . C15 . Br2 . 116.18(17) yes C16 . C15 . Br2 . 115.66(16) yes C15 . C16 . N4 . 123.9(2) yes C15 . C16 . C17 . 126.2(2) yes N4 . C16 . C17 . 109.8(2) yes C16 . C17 . C18 . 106.9(2) yes C16 . C17 . H171 . 125.1 no C18 . C17 . H171 . 128.1 no C17 . C18 . C19 . 106.9(2) yes C17 . C18 . H181 . 127.4 no C19 . C18 . H181 . 125.7 no C18 . C19 . N4 . 109.9(2) yes C18 . C19 . C20 . 124.7(2) yes N4 . C19 . C20 . 125.5(2) yes C19 . C20 . C1 . 126.0(2) yes C19 . C20 . C31 . 117.7(2) yes C1 . C20 . C31 . 116.2(2) yes N5 . C21 . C22 . 122.6(2) yes N5 . C21 . H211 . 117.7 no C22 . C21 . H211 . 119.8 no C21 . C22 . C23 . 118.7(3) yes C21 . C22 . H221 . 119.4 no C23 . C22 . H221 . 122.0 no C22 . C23 . C24 . 119.3(2) yes C22 . C23 . H231 . 119.9 no C24 . C23 . H231 . 120.8 no C23 . C24 . C25 . 118.3(3) yes C23 . C24 . H241 . 120.9 no C25 . C24 . H241 . 120.8 no C24 . C25 . N5 . 123.1(2) yes C24 . C25 . H251 . 119.6 no N5 . C25 . H251 . 117.3 no C20 . C31 . C32 . 119.8(2) yes C20 . C31 . C36 . 121.7(2) yes C32 . C31 . C36 . 118.5(2) yes C31 . C32 . C33 . 121.6(2) yes C31 . C32 . H321 . 118.4 no C33 . C32 . H321 . 120.0 no C32 . C33 . C34 . 119.6(3) yes C32 . C33 . H331 . 119.7 no C34 . C33 . H331 . 120.7 no C33 . C34 . C35 . 120.1(2) yes C33 . C34 . H341 . 119.8 no C35 . C34 . H341 . 120.1 no C34 . C35 . C36 . 120.2(2) yes C34 . C35 . H351 . 120.0 no C36 . C35 . H351 . 119.8 no C31 . C36 . C35 . 120.0(2) yes C31 . C36 . S1 . 121.32(18) yes C35 . C36 . S1 . 118.64(19) yes C10 . C41 . C42 . 120.2(2) yes C10 . C41 . C46 . 121.3(2) yes C42 . C41 . C46 . 118.4(2) yes C41 . C42 . C43 . 121.1(3) yes C41 . C42 . H421 . 119.0 no C43 . C42 . H421 . 119.9 no C42 . C43 . C44 . 119.6(3) yes C42 . C43 . H431 . 120.3 no C44 . C43 . H431 . 120.1 no C43 . C44 . C45 . 120.3(2) yes C43 . C44 . H441 . 119.9 no C45 . C44 . H441 . 119.8 no C44 . C45 . C46 . 119.7(3) yes C44 . C45 . H451 . 120.2 no C46 . C45 . H451 . 120.2 no C45 . C46 . C41 . 120.8(2) yes C45 . C46 . S2 . 119.1(2) yes C41 . C46 . S2 . 120.07(18) yes C36 . S1 . C51 . 102.15(11) yes C46 . S2 . C60 . 100.51(12) yes S1 . C51 . O1 . 122.8(2) yes S1 . C51 . C52 . 111.84(19) yes O1 . C51 . C52 . 125.3(3) yes C51 . C52 . C53 . 111.0(2) yes C51 . C52 . H521 . 110.2 no C53 . C52 . H521 . 108.0 no C51 . C52 . H522 . 108.5 no C53 . C52 . H522 . 110.1 no H521 . C52 . H522 . 109.1 no C52 . C53 . C54 . 112.8(3) yes C52 . C53 . H531 . 109.5 no C54 . C53 . H531 . 108.9 no C52 . C53 . H532 . 111.5 no C54 . C53 . H532 . 104.6 no H531 . C53 . H532 . 109.3 no C53 . C54 . C55 . 112.5(3) yes C53 . C54 . H541 . 106.6 no C55 . C54 . H541 . 111.3 no C53 . C54 . H542 . 108.8 no C55 . C54 . H542 . 109.8 no H541 . C54 . H542 . 107.7 no C54 . C55 . C56 . 114.9(2) yes C54 . C55 . H551 . 109.1 no C56 . C55 . H551 . 107.3 no C54 . C55 . H552 . 107.1 no C56 . C55 . H552 . 109.2 no H551 . C55 . H552 . 109.2 no C55 . C56 . C57 . 111.8(2) yes C55 . C56 . H561 . 108.8 no C57 . C56 . H561 . 109.6 no C55 . C56 . H562 . 109.5 no C57 . C56 . H562 . 108.6 no H561 . C56 . H562 . 108.5 no C56 . C57 . C58 . 114.7(2) yes C56 . C57 . H571 . 107.5 no C58 . C57 . H571 . 108.6 no C56 . C57 . H572 . 108.0 no C58 . C57 . H572 . 110.0 no H571 . C57 . H572 . 107.8 no C57 . C58 . C59 . 112.6(2) yes C57 . C58 . H581 . 110.5 no C59 . C58 . H581 . 108.0 no C57 . C58 . H582 . 109.0 no C59 . C58 . H582 . 108.3 no H581 . C58 . H582 . 108.3 no C58 . C59 . C60 . 111.6(2) yes C58 . C59 . H591 . 109.8 no C60 . C59 . H591 . 108.5 no C58 . C59 . H592 . 111.3 no C60 . C59 . H592 . 108.6 no H591 . C59 . H592 . 106.8 no C59 . C60 . S2 . 111.71(19) yes C59 . C60 . O2 . 124.8(3) yes S2 . C60 . O2 . 123.5(2) yes Cl1 . C61 . Cl3 . 111.9(4) yes Cl1 . C61 . Cl2 . 111.5(3) yes Cl3 . C61 . Cl2 . 111.6(4) yes Cl1 . C61 . H611 . 107.8 no Cl3 . C61 . H611 . 108.2 no Cl2 . C61 . H611 . 105.5 no Cl2 . C62 . Cl4 . 114.1(6) yes Cl2 . C62 . Cl1 . 114.8(4) yes Cl4 . C62 . Cl1 . 112.1(6) yes Cl2 . C62 . H621 . 104.5 no Cl4 . C62 . H621 . 105.5 no Cl1 . C62 . H621 . 104.6 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 C23 . H231 . N1 1_455 142 0.94 2.59 3.380(4) yes _iucr_refine_instructions_details ; # # Punched on 25/01/17 at 15:14:36 # #LIST 12 BLOCK SCALE X'S U'S EQUIV PART(1001, OCC) PART(1002, OCC) WEIGHT -1 PART(1002, OCC) RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 33,X'S) H ( 331,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 43,X'S) H ( 431,X'S) RIDE C ( 44,X'S) H ( 441,X'S) RIDE C ( 45,X'S) H ( 451,X'S) RIDE C ( 52,X'S) H ( 521,X'S) H ( 522,X'S) RIDE C ( 53,X'S) H ( 531,X'S) H ( 532,X'S) RIDE C ( 54,X'S) H ( 541,X'S) H ( 542,X'S) RIDE C ( 55,X'S) H ( 551,X'S) H ( 552,X'S) RIDE C ( 56,X'S) H ( 561,X'S) H ( 562,X'S) RIDE C ( 57,X'S) H ( 571,X'S) H ( 572,X'S) RIDE C ( 58,X'S) H ( 581,X'S) H ( 582,X'S) RIDE C ( 59,X'S) H ( 591,X'S) H ( 592,X'S) RIDE C ( 61,X'S) H ( 611,X'S) RIDE C ( 62,X'S) H ( 621,X'S) END # # Punched on 25/01/17 at 15:14:36 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; #============================================================================== data_7c #============================================================================== _audit_creation_date "2017-01-17" _audit_creation_method CRYSTALS_ver_14.61_build_6019 _oxford_structure_analysis_title '6705 (004drk16)' _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 29.0785(1) _cell_length_b 15.1984(1) _cell_length_c 24.2182(2) _cell_angle_alpha 90 _cell_angle_beta 123.5003(3) _cell_angle_gamma 90 _cell_volume 8925.18(10) _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'C 2/c ' _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' 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' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 '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' 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' 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' _cell_formula_units_Z 8 # Given Formula = C49 H51 Br2 N5 O2 S2 Zn1 # Dc = 1.53 Fooo = 4224.00 Mu = 24.81 M = 1031.30 # Found Formula = C49.00 H41.00 Br2 N5 O2 S2 Zn1 # Dc = 1.52 FOOO = 4144.00 Mu = 24.81 M = 1021.22 _chemical_formula_sum 'C49 H41 Br2 N5 O2 S2 Zn1' _chemical_formula_moiety 'C49 H41 Br2 N5 O2 S2 Zn1' _chemical_compound_source . _chemical_formula_weight 1021.22 _cell_measurement_reflns_used 10534 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description 'block' _exptl_crystal_colour 'clear_intense_red' _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_max 0.34 _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 4143.997 _exptl_absorpt_coefficient_mu 2.481 # Sheldrick geometric approximatio 0.45 0.61 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.50 _exptl_absorpt_correction_T_max 0.61 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '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 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _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 150 _diffrn_ambient_pressure 0 _diffrn_reflns_number 107221 _reflns_number_total 10171 _diffrn_reflns_av_R_equivalents 0.023 # Number of reflections without Friedels Law is 19827 # Number of reflections with Friedels Law is 10171 # Theoretical number of reflections is about 10241 _diffrn_reflns_theta_min 5.112 _diffrn_reflns_theta_max 27.489 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.489 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _reflns_limit_h_min -37 _reflns_limit_h_max 31 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 31 _oxford_diffrn_Wilson_B_factor 2.22 _oxford_diffrn_Wilson_scale 57.50 _atom_sites_solution_primary Other #heavy,direct,difmap,geom,iterative # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.87 _refine_diff_density_max 0.96 # 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>-3.0\s(I) _refine_ls_number_reflns 10171 _refine_ls_number_restraints 203 _refine_ls_number_parameters 605 _oxford_refine_ls_R_factor_ref 0.0464 _refine_ls_wR_factor_ref 0.0802 _refine_ls_goodness_of_fit_ref 1.0000 _refine_ls_shift/su_max 0.0017534 _refine_ls_shift/su_mean 0.0000383 # The values computed with all filters except I/sigma _oxford_reflns_number_all 10171 _refine_ls_R_factor_all 0.0464 _refine_ls_wR_factor_all 0.0802 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 8549 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_gt 0.0718 # 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 Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr #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: 34.7 54.5 32.2 13.3 3.11 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. 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 atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Zn1 Zn 0.250635(10) 0.534167(16) 0.362732(12) 0.0191 1.0000 Uani . . . . . . N1 N 0.23293(8) 0.48341(12) 0.42847(9) 0.0208 1.0000 Uani . . . . . . N2 N 0.16623(8) 0.54544(12) 0.29373(9) 0.0220 1.0000 Uani . . . . . . N3 N 0.26117(7) 0.53740(12) 0.28456(9) 0.0212 1.0000 Uani . . . . . . N4 N 0.32849(7) 0.47996(12) 0.42063(9) 0.0207 1.0000 Uani . . . . . . N5 N 0.26429(9) 0.66795(13) 0.39281(10) 0.0280 1.0000 Uani . . . . . . C1 C 0.26841(9) 0.44067(14) 0.48671(10) 0.0207 1.0000 Uani . . . . . . C2 C 0.24049(9) 0.41721(15) 0.51876(11) 0.0241 1.0000 Uani . . . . . . C3 C 0.18847(10) 0.44772(15) 0.48039(11) 0.0256 1.0000 Uani . . . . . . C4 C 0.18369(9) 0.48895(15) 0.42362(11) 0.0228 1.0000 Uani . . . . . . C5 C 0.13620(10) 0.52579(17) 0.36902(12) 0.0288 1.0000 Uani . . . . . . C6 C 0.12685(10) 0.55034(17) 0.30796(12) 0.0283 1.0000 Uani . . . . . . C7 C 0.07550(11) 0.5793(2) 0.25045(14) 0.0422 1.0000 Uani . . . . . . C8 C 0.08383(11) 0.5893(2) 0.20121(13) 0.0379 1.0000 Uani . . . . . . C9 C 0.14070(9) 0.56832(15) 0.22859(11) 0.0245 1.0000 Uani . . . . . . C10 C 0.16587(9) 0.57089(15) 0.19304(11) 0.0237 1.0000 Uani . . . . . . C11 C 0.22137(9) 0.55343(13) 0.21898(11) 0.0212 1.0000 Uani . . . . . . C12 C 0.24594(10) 0.55097(14) 0.18100(11) 0.0247 1.0000 Uani . . . . . . C13 C 0.29996(10) 0.53422(15) 0.22343(12) 0.0258 1.0000 Uani . . . . . . C14 C 0.30964(9) 0.52552(14) 0.28826(11) 0.0217 1.0000 Uani . . . . . . C15 C 0.35989(9) 0.50493(16) 0.34704(12) 0.0242 1.0000 Uani . . . . . . C16 C 0.36942(9) 0.48398(14) 0.40860(11) 0.0216 1.0000 Uani . . . . . . C17 C 0.42115(9) 0.45569(16) 0.46691(12) 0.0263 1.0000 Uani . . . . . . C18 C 0.41054(9) 0.43198(16) 0.51243(11) 0.0256 1.0000 Uani . . . . . . C19 C 0.35238(9) 0.44620(14) 0.48310(11) 0.0210 1.0000 Uani . . . . . . C20 C 0.32423(9) 0.42439(14) 0.51340(11) 0.0217 1.0000 Uani . . . . . . C21 C 0.29158(12) 0.69252(19) 0.45612(15) 0.0422 1.0000 Uani . . . . . . C22 C 0.29662(16) 0.7803(2) 0.47471(19) 0.0607 1.0000 Uani . . . . . . C23 C 0.27274(17) 0.8435(2) 0.4266(2) 0.0697 1.0000 Uani . . . . . . C24 C 0.24471(19) 0.8185(2) 0.3616(2) 0.0704 1.0000 Uani . . . . . . C25 C 0.24135(14) 0.73050(18) 0.34667(16) 0.0463 1.0000 Uani . . . . . . C31 C 0.35695(9) 0.37797(15) 0.57871(11) 0.0233 1.0000 Uani . . . . . . C32 C 0.36042(11) 0.28625(17) 0.58066(13) 0.0323 1.0000 Uani . . . . . . C33 C 0.39256(12) 0.24273(19) 0.64047(14) 0.0388 1.0000 Uani . . . . . . C34 C 0.42232(12) 0.2898(2) 0.69919(13) 0.0393 1.0000 Uani . . . . . . C35 C 0.41848(11) 0.38053(19) 0.69856(12) 0.0333 1.0000 Uani . . . . . . C36 C 0.38531(9) 0.42455(16) 0.63842(11) 0.0251 1.0000 Uani . U . . . . C41 C 0.12947(9) 0.59211(16) 0.12050(11) 0.0255 1.0000 Uani . . . . . . C42 C 0.09537(11) 0.52739(18) 0.07592(13) 0.0337 1.0000 Uani . . . . . . C43 C 0.06252(11) 0.5448(2) 0.00824(13) 0.0348 1.0000 Uani . . . . . . C44 C 0.06357(11) 0.6266(2) -0.01530(12) 0.0353 1.0000 Uani . . . . . . C45 C 0.09611(11) 0.69217(18) 0.02831(12) 0.0327 1.0000 Uani . . . . . . C46 C 0.12891(10) 0.67551(16) 0.09598(11) 0.0258 1.0000 Uani . U . . . . Br1 Br 0.075066(12) 0.53814(3) 0.377273(16) 0.0546 1.0000 Uani . . . . . . Br2 Br 0.422175(10) 0.49679(2) 0.340660(13) 0.0362 1.0000 Uani . . . . . . S1 S 0.37677(2) 0.54008(4) 0.63673(3) 0.0301 1.0000 Uani . U . . . . S2 S 0.16905(3) 0.76132(4) 0.15180(3) 0.0302 1.0000 Uani . U . . . . O1 O 0.48025(8) 0.53127(15) 0.67189(12) 0.0471 1.0000 Uani . U . . . . O2 O 0.22061(8) 0.73512(13) 0.09092(9) 0.0377 1.0000 Uani . U . . . . C51 C 0.44276(11) 0.57910(19) 0.65903(13) 0.0351 1.0000 Uani . U . . . . C52 C 0.44480(14) 0.6787(2) 0.65950(19) 0.0517 1.0000 Uani D U . . . . C53 C 0.48693(15) 0.7141(2) 0.64663(16) 0.0534 1.0000 Uani D U . . . . C54 C 0.4565(2) 0.7002(4) 0.5711(3) 0.0443 0.533(6) Uani D U P 1 1 . C55 C 0.4949(2) 0.7258(3) 0.5492(2) 0.0378 0.533(6) Uani D U P 1 1 . C56 C 0.4704(2) 0.7057(4) 0.4763(3) 0.0364 0.533(6) Uani D U P 1 1 . C57 C 0.4272(3) 0.7739(4) 0.4301(3) 0.0406 0.533(6) Uani D U P 1 1 . C58 C 0.3952(3) 0.7436(4) 0.3593(3) 0.0477 0.533(6) Uani D U P 1 1 . C59 C 0.3546(3) 0.8105(4) 0.3087(3) 0.0441 0.533(6) Uani D U P 1 1 . C60 C 0.31379(11) 0.76612(18) 0.24347(13) 0.0389 1.0000 Uani D U . . . . C61 C 0.27008(11) 0.82529(16) 0.18789(13) 0.0362 1.0000 Uani D U . . . . C62 C 0.22252(10) 0.77121(16) 0.13601(12) 0.0290 1.0000 Uani . U . . . . C64 C 0.4886(3) 0.6897(5) 0.5856(3) 0.0483 0.467(6) Uani D U P 1 2 . C65 C 0.4400(3) 0.7277(6) 0.5230(3) 0.0573 0.467(6) Uani D U P 1 2 . C66 C 0.4464(3) 0.7188(6) 0.4647(3) 0.0478 0.467(6) Uani D U P 1 2 . C67 C 0.3979(3) 0.7565(5) 0.4020(3) 0.0435 0.467(6) Uani D U P 1 2 . C68 C 0.4109(3) 0.7776(5) 0.3498(3) 0.0423 0.467(6) Uani D U P 1 2 . C69 C 0.3648(3) 0.8250(4) 0.2878(3) 0.0411 0.467(6) Uani D U P 1 2 . H21 H 0.2557 0.3855 0.5578 0.0284 1.0000 Uiso R . . . . . H31 H 0.1609 0.4423 0.4886 0.0309 1.0000 Uiso R . . . . . H71 H 0.0424 0.5878 0.2478 0.0509 1.0000 Uiso R . . . . . H81 H 0.0583 0.6065 0.1577 0.0450 1.0000 Uiso R . . . . . H121 H 0.2271 0.5602 0.1350 0.0297 1.0000 Uiso R . . . . . H131 H 0.3263 0.5296 0.2135 0.0310 1.0000 Uiso R . . . . . H171 H 0.4550 0.4536 0.4716 0.0317 1.0000 Uiso R . . . . . H181 H 0.4357 0.4112 0.5549 0.0309 1.0000 Uiso R . . . . . H211 H 0.3071 0.6489 0.4884 0.0512 1.0000 Uiso R . . . . . H221 H 0.3161 0.7952 0.5198 0.0728 1.0000 Uiso R . . . . . H231 H 0.2757 0.9028 0.4378 0.0840 1.0000 Uiso R . . . . . H241 H 0.2278 0.8601 0.3279 0.0853 1.0000 Uiso R . . . . . H251 H 0.2221 0.7131 0.3022 0.0558 1.0000 Uiso R . . . . . H321 H 0.3408 0.2544 0.5412 0.0388 1.0000 Uiso R . . . . . H331 H 0.3942 0.1813 0.6409 0.0470 1.0000 Uiso R . . . . . H341 H 0.4445 0.2608 0.7391 0.0465 1.0000 Uiso R . . . . . H351 H 0.4381 0.4132 0.7381 0.0395 1.0000 Uiso R . . . . . H421 H 0.0946 0.4714 0.0917 0.0402 1.0000 Uiso R . . . . . H431 H 0.0400 0.5011 -0.0210 0.0416 1.0000 Uiso R . . . . . H441 H 0.0423 0.6374 -0.0607 0.0417 1.0000 Uiso R . . . . . H451 H 0.0961 0.7488 0.0125 0.0389 1.0000 Uiso R . . . . . H521 H 0.4539 0.6992 0.7019 0.0623 1.0000 Uiso R . . . . . H522 H 0.4090 0.7010 0.6260 0.0626 1.0000 Uiso R . . . . . H532 H 0.4944 0.7759 0.6589 0.0638 0.533(6) Uiso R . P 1 1 . H531 H 0.5213 0.6810 0.6715 0.0634 0.533(6) Uiso R . P 1 1 . H533 H 0.5225 0.6941 0.6842 0.0636 0.467(6) Uiso R . P 1 2 . H534 H 0.4850 0.7780 0.6476 0.0640 0.467(6) Uiso R . P 1 2 . H541 H 0.4237 0.7366 0.5488 0.0532 0.533(6) Uiso R . P 1 1 . H542 H 0.4464 0.6381 0.5595 0.0531 0.533(6) Uiso R . P 1 1 . H552 H 0.5017 0.7888 0.5559 0.0448 0.533(6) Uiso R . P 1 1 . H551 H 0.5296 0.6938 0.5760 0.0450 0.533(6) Uiso R . P 1 1 . H561 H 0.4994 0.7041 0.4681 0.0439 0.533(6) Uiso R . P 1 1 . H562 H 0.4527 0.6497 0.4663 0.0438 0.533(6) Uiso R . P 1 1 . H572 H 0.4462 0.8286 0.4333 0.0491 0.533(6) Uiso R . P 1 1 . H571 H 0.4020 0.7848 0.4433 0.0490 0.533(6) Uiso R . P 1 1 . H581 H 0.4212 0.7273 0.3477 0.0570 0.533(6) Uiso R . P 1 1 . H582 H 0.3744 0.6918 0.3568 0.0572 0.533(6) Uiso R . P 1 1 . H592 H 0.3750 0.8544 0.3015 0.0529 0.533(6) Uiso R . P 1 1 . H591 H 0.3345 0.8386 0.3254 0.0530 0.533(6) Uiso R . P 1 1 . H602 H 0.3337 0.7357 0.2273 0.0468 0.533(6) Uiso R . P 1 1 . H601 H 0.2944 0.7231 0.2534 0.0469 0.533(6) Uiso R . P 1 1 . H603 H 0.3001 0.7424 0.2691 0.0468 0.467(6) Uiso R . P 1 2 . H604 H 0.3235 0.7184 0.2247 0.0467 0.467(6) Uiso R . P 1 2 . H612 H 0.2862 0.8566 0.1681 0.0432 1.0000 Uiso R . . . . . H611 H 0.2571 0.8666 0.2061 0.0429 1.0000 Uiso R . . . . . H641 H 0.5227 0.7108 0.5914 0.0583 0.467(6) Uiso R . P 1 2 . H642 H 0.4863 0.6259 0.5799 0.0579 0.467(6) Uiso R . P 1 2 . H652 H 0.4363 0.7897 0.5314 0.0693 0.467(6) Uiso R . P 1 2 . H651 H 0.4072 0.6950 0.5128 0.0691 0.467(6) Uiso R . P 1 2 . H661 H 0.4792 0.7506 0.4751 0.0573 0.467(6) Uiso R . P 1 2 . H662 H 0.4509 0.6579 0.4581 0.0567 0.467(6) Uiso R . P 1 2 . H672 H 0.3872 0.8110 0.4130 0.0519 0.467(6) Uiso R . P 1 2 . H671 H 0.3676 0.7150 0.3839 0.0517 0.467(6) Uiso R . P 1 2 . H682 H 0.4431 0.8148 0.3705 0.0508 0.467(6) Uiso R . P 1 2 . H681 H 0.4187 0.7222 0.3364 0.0510 0.467(6) Uiso R . P 1 2 . H691 H 0.3536 0.8758 0.3021 0.0489 0.467(6) Uiso R . P 1 2 . H692 H 0.3795 0.8445 0.2625 0.0491 0.467(6) Uiso R . P 1 2 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02031(12) 0.01786(11) 0.02098(12) 0.00166(9) 0.01260(10) 0.00107(9) N1 0.0217(9) 0.0206(9) 0.0206(9) 0.0014(7) 0.0121(7) 0.0014(7) N2 0.0212(9) 0.0224(9) 0.0239(9) 0.0047(7) 0.0134(8) 0.0036(7) N3 0.0221(9) 0.0203(9) 0.0217(9) 0.0027(7) 0.0123(8) 0.0011(7) N4 0.0205(9) 0.0200(9) 0.0244(9) 0.0021(7) 0.0141(8) 0.0012(7) N5 0.0312(10) 0.0221(10) 0.0338(11) -0.0027(8) 0.0198(9) -0.0014(8) C1 0.0268(11) 0.0180(10) 0.0198(10) 0.0006(8) 0.0145(9) 0.0007(8) C2 0.0278(11) 0.0244(11) 0.0226(11) 0.0016(9) 0.0156(9) -0.0010(9) C3 0.0277(11) 0.0290(12) 0.0252(11) 0.0004(9) 0.0179(10) -0.0009(9) C4 0.0232(10) 0.0249(11) 0.0240(10) 0.0006(8) 0.0154(9) 0.0018(8) C5 0.0237(11) 0.0369(13) 0.0322(12) 0.0062(10) 0.0195(10) 0.0062(9) C6 0.0230(11) 0.0349(13) 0.0303(12) 0.0084(10) 0.0168(10) 0.0068(9) C7 0.0275(13) 0.0643(19) 0.0388(15) 0.0206(14) 0.0208(12) 0.0176(13) C8 0.0248(12) 0.0565(18) 0.0290(13) 0.0169(12) 0.0128(11) 0.0141(12) C9 0.0237(11) 0.0245(11) 0.0238(11) 0.0041(9) 0.0122(9) 0.0036(9) C10 0.0275(11) 0.0203(10) 0.0234(11) 0.0027(8) 0.0140(9) 0.0006(9) C11 0.0276(11) 0.0153(10) 0.0220(10) 0.0023(8) 0.0145(9) 0.0002(8) C12 0.0317(12) 0.0203(11) 0.0237(11) 0.0028(8) 0.0163(10) 0.0018(9) C13 0.0325(12) 0.0230(11) 0.0300(12) 0.0025(9) 0.0223(10) 0.0007(9) C14 0.0249(10) 0.0176(10) 0.0273(11) 0.0031(8) 0.0175(9) 0.0016(8) C15 0.0230(10) 0.0240(11) 0.0316(12) 0.0016(9) 0.0190(10) 0.0002(9) C16 0.0200(10) 0.0195(11) 0.0269(11) 0.0009(8) 0.0140(9) -0.0001(8) C17 0.0191(10) 0.0286(12) 0.0287(11) 0.0030(9) 0.0116(9) 0.0009(9) C18 0.0219(11) 0.0271(11) 0.0236(11) 0.0021(9) 0.0100(9) 0.0016(9) C19 0.0222(10) 0.0179(10) 0.0219(10) 0.0004(8) 0.0115(9) -0.0003(8) C20 0.0243(11) 0.0197(10) 0.0218(10) -0.0004(8) 0.0131(9) -0.0008(8) C21 0.0426(15) 0.0336(14) 0.0400(15) -0.0102(12) 0.0163(13) -0.0034(12) C22 0.062(2) 0.048(2) 0.058(2) -0.0278(17) 0.0242(18) -0.0109(16) C23 0.077(3) 0.0264(16) 0.097(3) -0.0235(18) 0.043(2) -0.0050(16) C24 0.092(3) 0.0236(15) 0.082(3) 0.0031(16) 0.040(2) 0.0047(17) C25 0.064(2) 0.0233(13) 0.0466(17) 0.0044(11) 0.0277(16) 0.0030(13) C31 0.0210(10) 0.0280(11) 0.0229(11) 0.0029(9) 0.0134(9) 0.0012(8) C32 0.0386(14) 0.0273(12) 0.0274(12) 0.0024(10) 0.0160(11) 0.0010(10) C33 0.0468(16) 0.0320(14) 0.0346(14) 0.0108(11) 0.0205(13) 0.0063(12) C34 0.0372(14) 0.0493(17) 0.0275(13) 0.0139(12) 0.0154(12) 0.0114(12) C35 0.0303(12) 0.0464(15) 0.0212(11) 0.0011(10) 0.0130(10) 0.0052(11) C36 0.0232(11) 0.0301(12) 0.0241(11) -0.0016(9) 0.0143(9) 0.0015(9) C41 0.0235(11) 0.0303(12) 0.0230(11) 0.0019(9) 0.0130(9) 0.0036(9) C42 0.0332(13) 0.0352(13) 0.0310(13) 0.0008(10) 0.0166(11) -0.0037(11) C43 0.0281(12) 0.0486(16) 0.0264(12) -0.0070(11) 0.0143(10) -0.0045(11) C44 0.0278(12) 0.0534(17) 0.0213(11) 0.0042(11) 0.0113(10) 0.0083(11) C45 0.0343(13) 0.0352(13) 0.0282(12) 0.0106(10) 0.0171(11) 0.0131(11) C46 0.0264(11) 0.0264(11) 0.0244(11) 0.0036(9) 0.0140(10) 0.0061(9) Br1 0.03616(15) 0.0927(3) 0.05140(18) 0.03558(17) 0.03464(14) 0.03134(16) Br2 0.02640(12) 0.05305(16) 0.03772(13) 0.01186(12) 0.02318(11) 0.00602(11) S1 0.0251(3) 0.0305(3) 0.0325(3) -0.0074(2) 0.0144(2) -0.0001(2) S2 0.0422(3) 0.0223(3) 0.0290(3) 0.0013(2) 0.0214(3) 0.0040(2) O1 0.0329(10) 0.0522(12) 0.0609(13) 0.0121(10) 0.0289(10) 0.0051(9) O2 0.0405(10) 0.0407(11) 0.0337(10) -0.0036(8) 0.0216(9) 0.0022(8) C51 0.0279(11) 0.0418(13) 0.0331(13) -0.0012(11) 0.0154(11) -0.0025(9) C52 0.0442(17) 0.0420(14) 0.065(2) -0.0103(15) 0.0282(16) -0.0123(13) C53 0.066(2) 0.0466(17) 0.0509(16) -0.0112(14) 0.0341(16) -0.0213(15) C54 0.027(3) 0.054(4) 0.046(2) 0.004(3) 0.015(2) 0.001(3) C55 0.038(3) 0.028(2) 0.043(2) 0.007(2) 0.020(2) -0.002(2) C56 0.028(3) 0.032(3) 0.043(2) 0.006(2) 0.016(2) 0.004(2) C57 0.034(3) 0.037(3) 0.039(2) 0.005(2) 0.013(2) 0.006(2) C58 0.044(3) 0.030(3) 0.043(3) -0.003(2) 0.007(2) 0.002(2) C59 0.047(3) 0.036(3) 0.033(2) -0.0035(19) 0.012(2) 0.008(2) C60 0.0380(14) 0.0280(13) 0.0361(13) -0.0022(10) 0.0113(10) 0.0032(10) C61 0.0417(13) 0.0212(12) 0.0380(13) 0.0013(9) 0.0171(10) 0.0015(9) C62 0.0344(11) 0.0217(11) 0.0276(11) 0.0056(8) 0.0151(10) 0.0060(9) C64 0.053(4) 0.045(4) 0.043(3) 0.004(3) 0.024(3) -0.003(3) C65 0.058(4) 0.064(5) 0.049(3) 0.011(3) 0.028(3) 0.012(3) C66 0.030(4) 0.065(5) 0.038(3) -0.002(3) 0.012(3) -0.011(4) C67 0.037(4) 0.049(4) 0.032(3) -0.011(3) 0.011(3) -0.011(3) C68 0.035(3) 0.039(4) 0.043(3) -0.001(2) 0.014(2) -0.016(3) C69 0.043(3) 0.038(3) 0.037(3) -0.005(2) 0.019(2) -0.007(2) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 0.13945(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 . N1 . 2.0735(18) yes Zn1 . N2 . 2.0780(19) yes Zn1 . N3 . 2.0787(18) yes Zn1 . N4 . 2.0654(18) yes Zn1 . N5 . 2.122(2) yes N1 . C1 . 1.367(3) yes N1 . C4 . 1.373(3) yes N2 . C6 . 1.368(3) yes N2 . C9 . 1.367(3) yes N3 . C11 . 1.375(3) yes N3 . C14 . 1.374(3) yes N4 . C16 . 1.374(3) yes N4 . C19 . 1.369(3) yes N5 . C21 . 1.333(3) yes N5 . C25 . 1.332(4) yes C1 . C2 . 1.444(3) yes C1 . C20 . 1.398(3) yes C2 . C3 . 1.347(3) yes C2 . H21 . 0.928 no C3 . C4 . 1.446(3) yes C3 . H31 . 0.931 no C4 . C5 . 1.398(3) yes C5 . C6 . 1.399(3) yes C5 . Br1 . 1.905(2) yes C6 . C7 . 1.438(3) yes C7 . C8 . 1.350(4) yes C7 . H71 . 0.937 no C8 . C9 . 1.437(3) yes C8 . H81 . 0.931 no C9 . C10 . 1.405(3) yes C10 . C11 . 1.397(3) yes C10 . C41 . 1.503(3) yes C11 . C12 . 1.443(3) yes C12 . C13 . 1.344(3) yes C12 . H121 . 0.942 no C13 . C14 . 1.440(3) yes C13 . H131 . 0.923 no C14 . C15 . 1.401(3) yes C15 . C16 . 1.395(3) yes C15 . Br2 . 1.905(2) yes C16 . C17 . 1.448(3) yes C17 . C18 . 1.347(3) yes C17 . H171 . 0.928 no C18 . C19 . 1.444(3) yes C18 . H181 . 0.928 no C19 . C20 . 1.408(3) yes C20 . C31 . 1.498(3) yes C21 . C22 . 1.389(4) yes C21 . H211 . 0.930 no C22 . C23 . 1.368(6) yes C22 . H221 . 0.939 no C23 . C24 . 1.366(6) yes C23 . H231 . 0.931 no C24 . C25 . 1.376(4) yes C24 . H241 . 0.930 no C25 . H251 . 0.937 no C31 . C32 . 1.397(3) yes C31 . C36 . 1.399(3) yes C32 . C33 . 1.384(4) yes C32 . H321 . 0.933 no C33 . C34 . 1.387(4) yes C33 . H331 . 0.934 no C34 . C35 . 1.383(4) yes C34 . H341 . 0.925 no C35 . C36 . 1.396(3) yes C35 . H351 . 0.941 no C36 . S1 . 1.771(3) yes C41 . C42 . 1.391(3) yes C41 . C46 . 1.396(3) yes C42 . C43 . 1.393(4) yes C42 . H421 . 0.939 no C43 . C44 . 1.375(4) yes C43 . H431 . 0.927 no C44 . C45 . 1.379(4) yes C44 . H441 . 0.932 no C45 . C46 . 1.391(3) yes C45 . H451 . 0.942 no C46 . S2 . 1.775(2) yes S1 . C51 . 1.783(3) yes S2 . C62 . 1.801(3) yes O1 . C51 . 1.200(3) yes O2 . C62 . 1.196(3) yes C51 . C52 . 1.515(4) yes C52 . C53 . 1.520(4) yes C52 . H521 . 0.960 no C52 . H522 . 0.962 no C53 . C54 . 1.546(6) yes C53 . H532 . 0.972 no C53 . H531 . 0.975 no C53 . C64 . 1.551(6) yes C53 . H533 . 0.976 no C53 . H534 . 0.973 no C54 . C55 . 1.528(6) yes C54 . H541 . 0.969 no C54 . H542 . 0.981 no C55 . C56 . 1.527(6) yes C55 . H552 . 0.973 no C55 . H551 . 0.976 no C56 . C57 . 1.534(6) yes C56 . H561 . 0.966 no C56 . H562 . 0.954 no C57 . C58 . 1.502(7) yes C57 . H572 . 0.977 no C57 . H571 . 0.963 no C58 . C59 . 1.527(6) yes C58 . H581 . 0.972 no C58 . H582 . 0.974 no C59 . C60 . 1.514(5) yes C59 . H592 . 0.971 no C59 . H591 . 0.973 no C60 . C61 . 1.532(3) yes C60 . H602 . 0.975 no C60 . H601 . 0.976 no C60 . C61 . 1.532(3) yes C60 . C69 . 1.548(6) yes C60 . H603 . 0.974 no C60 . H604 . 0.977 no C61 . C62 . 1.500(4) yes C61 . H612 . 0.962 no C61 . H611 . 0.957 no C64 . C65 . 1.505(7) yes C64 . H641 . 0.975 no C64 . H642 . 0.976 no C65 . C66 . 1.528(7) yes C65 . H652 . 0.982 no C65 . H651 . 0.977 no C66 . C67 . 1.503(7) yes C66 . H661 . 0.969 no C66 . H662 . 0.960 no C67 . C68 . 1.539(7) yes C67 . H672 . 0.973 no C67 . H671 . 0.970 no C68 . C69 . 1.532(7) yes C68 . H682 . 0.964 no C68 . H681 . 0.974 no C69 . H691 . 0.971 no C69 . H692 . 0.969 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Zn1 . N2 . 87.97(7) yes N1 . Zn1 . N3 . 158.74(7) yes N2 . Zn1 . N3 . 88.17(7) yes N1 . Zn1 . N4 . 88.51(7) yes N2 . Zn1 . N4 . 160.79(7) yes N3 . Zn1 . N4 . 88.31(7) yes N1 . Zn1 . N5 . 99.88(8) yes N2 . Zn1 . N5 . 96.39(8) yes N3 . Zn1 . N5 . 101.32(8) yes N4 . Zn1 . N5 . 102.82(8) yes Zn1 . N1 . C1 . 127.09(15) yes Zn1 . N1 . C4 . 126.91(15) yes C1 . N1 . C4 . 105.96(18) yes Zn1 . N2 . C6 . 125.69(15) yes Zn1 . N2 . C9 . 126.66(15) yes C6 . N2 . C9 . 106.26(19) yes Zn1 . N3 . C11 . 127.07(14) yes Zn1 . N3 . C14 . 126.80(15) yes C11 . N3 . C14 . 106.13(18) yes Zn1 . N4 . C16 . 126.26(15) yes Zn1 . N4 . C19 . 126.66(14) yes C16 . N4 . C19 . 106.29(18) yes Zn1 . N5 . C21 . 122.89(18) yes Zn1 . N5 . C25 . 118.93(18) yes C21 . N5 . C25 . 118.0(2) yes N1 . C1 . C2 . 110.11(19) yes N1 . C1 . C20 . 125.69(19) yes C2 . C1 . C20 . 124.2(2) yes C1 . C2 . C3 . 107.1(2) yes C1 . C2 . H21 . 125.6 no C3 . C2 . H21 . 127.2 no C2 . C3 . C4 . 106.7(2) yes C2 . C3 . H31 . 126.4 no C4 . C3 . H31 . 126.9 no C3 . C4 . N1 . 110.10(19) yes C3 . C4 . C5 . 126.8(2) yes N1 . C4 . C5 . 123.0(2) yes C4 . C5 . C6 . 128.4(2) yes C4 . C5 . Br1 . 115.61(17) yes C6 . C5 . Br1 . 115.89(17) yes C5 . C6 . N2 . 123.4(2) yes C5 . C6 . C7 . 126.7(2) yes N2 . C6 . C7 . 109.8(2) yes C6 . C7 . C8 . 107.1(2) yes C6 . C7 . H71 . 126.0 no C8 . C7 . H71 . 127.0 no C7 . C8 . C9 . 106.8(2) yes C7 . C8 . H81 . 127.7 no C9 . C8 . H81 . 125.5 no C8 . C9 . N2 . 110.0(2) yes C8 . C9 . C10 . 124.5(2) yes N2 . C9 . C10 . 125.4(2) yes C9 . C10 . C11 . 125.6(2) yes C9 . C10 . C41 . 117.0(2) yes C11 . C10 . C41 . 117.4(2) yes C10 . C11 . N3 . 125.5(2) yes C10 . C11 . C12 . 125.0(2) yes N3 . C11 . C12 . 109.53(19) yes C11 . C12 . C13 . 107.4(2) yes C11 . C12 . H121 . 125.5 no C13 . C12 . H121 . 127.2 no C12 . C13 . C14 . 107.1(2) yes C12 . C13 . H131 . 127.0 no C14 . C13 . H131 . 125.9 no C13 . C14 . N3 . 109.92(19) yes C13 . C14 . C15 . 126.5(2) yes N3 . C14 . C15 . 123.6(2) yes C14 . C15 . C16 . 128.1(2) yes C14 . C15 . Br2 . 115.93(16) yes C16 . C15 . Br2 . 115.79(16) yes C15 . C16 . N4 . 123.5(2) yes C15 . C16 . C17 . 126.6(2) yes N4 . C16 . C17 . 109.58(19) yes C16 . C17 . C18 . 107.1(2) yes C16 . C17 . H171 . 126.2 no C18 . C17 . H171 . 126.7 no C17 . C18 . C19 . 107.0(2) yes C17 . C18 . H181 . 126.9 no C19 . C18 . H181 . 126.0 no C18 . C19 . N4 . 109.98(19) yes C18 . C19 . C20 . 124.6(2) yes N4 . C19 . C20 . 125.3(2) yes C19 . C20 . C1 . 125.3(2) yes C19 . C20 . C31 . 116.63(19) yes C1 . C20 . C31 . 118.05(19) yes N5 . C21 . C22 . 122.1(3) yes N5 . C21 . H211 . 118.2 no C22 . C21 . H211 . 119.7 no C21 . C22 . C23 . 119.0(3) yes C21 . C22 . H221 . 119.8 no C23 . C22 . H221 . 121.2 no C22 . C23 . C24 . 119.1(3) yes C22 . C23 . H231 . 120.7 no C24 . C23 . H231 . 120.3 no C23 . C24 . C25 . 118.9(4) yes C23 . C24 . H241 . 120.9 no C25 . C24 . H241 . 120.2 no C24 . C25 . N5 . 122.9(3) yes C24 . C25 . H251 . 119.2 no N5 . C25 . H251 . 117.9 no C20 . C31 . C32 . 119.9(2) yes C20 . C31 . C36 . 121.5(2) yes C32 . C31 . C36 . 118.7(2) yes C31 . C32 . C33 . 120.5(2) yes C31 . C32 . H321 . 119.4 no C33 . C32 . H321 . 120.1 no C32 . C33 . C34 . 120.3(3) yes C32 . C33 . H331 . 119.4 no C34 . C33 . H331 . 120.3 no C33 . C34 . C35 . 120.1(2) yes C33 . C34 . H341 . 120.4 no C35 . C34 . H341 . 119.5 no C34 . C35 . C36 . 119.6(2) yes C34 . C35 . H351 . 121.0 no C36 . C35 . H351 . 119.4 no C31 . C36 . C35 . 120.6(2) yes C31 . C36 . S1 . 118.88(18) yes C35 . C36 . S1 . 120.45(19) yes C10 . C41 . C42 . 119.7(2) yes C10 . C41 . C46 . 121.8(2) yes C42 . C41 . C46 . 118.4(2) yes C41 . C42 . C43 . 120.7(2) yes C41 . C42 . H421 . 119.4 no C43 . C42 . H421 . 119.8 no C42 . C43 . C44 . 120.1(2) yes C42 . C43 . H431 . 120.0 no C44 . C43 . H431 . 119.9 no C43 . C44 . C45 . 119.9(2) yes C43 . C44 . H441 . 119.7 no C45 . C44 . H441 . 120.3 no C44 . C45 . C46 . 120.4(2) yes C44 . C45 . H451 . 120.2 no C46 . C45 . H451 . 119.4 no C41 . C46 . C45 . 120.4(2) yes C41 . C46 . S2 . 119.66(17) yes C45 . C46 . S2 . 119.92(19) yes C36 . S1 . C51 . 102.06(12) yes C46 . S2 . C62 . 100.47(11) yes S1 . C51 . O1 . 123.3(2) yes S1 . C51 . C52 . 111.4(2) yes O1 . C51 . C52 . 125.3(3) yes C51 . C52 . C53 . 112.6(3) yes C51 . C52 . H521 . 108.6 no C53 . C52 . H521 . 109.1 no C51 . C52 . H522 . 109.1 no C53 . C52 . H522 . 108.8 no H521 . C52 . H522 . 108.6 no C52 . C53 . C54 . 101.2(3) yes C52 . C53 . H532 . 110.5 no C54 . C53 . H532 . 112.3 no C52 . C53 . H531 . 111.0 no C54 . C53 . H531 . 112.5 no H532 . C53 . H531 . 109.2 no C52 . C53 . C64 . 124.3(4) yes C52 . C53 . H533 . 105.0 no C64 . C53 . H533 . 103.9 no C52 . C53 . H534 . 106.5 no C64 . C53 . H534 . 107.1 no H533 . C53 . H534 . 109.6 no C53 . C54 . C55 . 108.9(4) yes C53 . C54 . H541 . 109.0 no C55 . C54 . H541 . 110.2 no C53 . C54 . H542 . 110.9 no C55 . C54 . H542 . 107.8 no H541 . C54 . H542 . 110.1 no C54 . C55 . C56 . 112.7(4) yes C54 . C55 . H552 . 108.3 no C56 . C55 . H552 . 108.2 no C54 . C55 . H551 . 109.2 no C56 . C55 . H551 . 108.6 no H552 . C55 . H551 . 109.9 no C55 . C56 . C57 . 112.3(5) yes C55 . C56 . H561 . 109.8 no C57 . C56 . H561 . 108.9 no C55 . C56 . H562 . 108.3 no C57 . C56 . H562 . 107.9 no H561 . C56 . H562 . 109.7 no C56 . C57 . C58 . 111.5(5) yes C56 . C57 . H572 . 108.5 no C58 . C57 . H572 . 108.7 no C56 . C57 . H571 . 110.0 no C58 . C57 . H571 . 109.0 no H572 . C57 . H571 . 109.1 no C57 . C58 . C59 . 115.4(5) yes C57 . C58 . H581 . 108.4 no C59 . C58 . H581 . 108.5 no C57 . C58 . H582 . 107.0 no C59 . C58 . H582 . 108.1 no H581 . C58 . H582 . 109.3 no C58 . C59 . C60 . 110.8(4) yes C58 . C59 . H592 . 108.9 no C60 . C59 . H592 . 108.9 no C58 . C59 . H591 . 109.5 no C60 . C59 . H591 . 109.0 no H592 . C59 . H591 . 109.8 no C59 . C60 . C61 . 116.6(3) yes C59 . C60 . H602 . 109.5 no C61 . C60 . H602 . 108.3 no C59 . C60 . H601 . 105.6 no C61 . C60 . H601 . 107.3 no H602 . C60 . H601 . 109.3 no C61 . C60 . C69 . 106.4(3) yes C61 . C60 . H603 . 110.2 no C69 . C60 . H603 . 110.1 no C61 . C60 . H604 . 109.9 no C69 . C60 . H604 . 109.9 no H603 . C60 . H604 . 110.3 no C60 . C61 . C62 . 110.4(2) yes C60 . C61 . H612 . 109.4 no C62 . C61 . H612 . 109.3 no C60 . C61 . H611 . 109.1 no C62 . C61 . H611 . 109.3 no H612 . C61 . H611 . 109.3 no C61 . C62 . S2 . 111.89(19) yes C61 . C62 . O2 . 125.0(2) yes S2 . C62 . O2 . 123.1(2) yes C53 . C64 . C65 . 111.3(6) yes C53 . C64 . H641 . 110.3 no C65 . C64 . H641 . 109.5 no C53 . C64 . H642 . 109.7 no C65 . C64 . H642 . 106.6 no H641 . C64 . H642 . 109.3 no C64 . C65 . C66 . 111.8(6) yes C64 . C65 . H652 . 107.9 no C66 . C65 . H652 . 111.0 no C64 . C65 . H651 . 107.6 no C66 . C65 . H651 . 108.7 no H652 . C65 . H651 . 109.7 no C65 . C66 . C67 . 112.0(6) yes C65 . C66 . H661 . 108.7 no C67 . C66 . H661 . 108.1 no C65 . C66 . H662 . 109.6 no C67 . C66 . H662 . 109.6 no H661 . C66 . H662 . 108.7 no C66 . C67 . C68 . 113.0(6) yes C66 . C67 . H672 . 108.1 no C68 . C67 . H672 . 107.9 no C66 . C67 . H671 . 108.8 no C68 . C67 . H671 . 109.8 no H672 . C67 . H671 . 109.2 no C67 . C68 . C69 . 115.1(6) yes C67 . C68 . H682 . 107.8 no C69 . C68 . H682 . 107.8 no C67 . C68 . H681 . 107.6 no C69 . C68 . H681 . 108.5 no H682 . C68 . H681 . 110.0 no C68 . C69 . C60 . 113.2(5) yes C68 . C69 . H691 . 108.0 no C60 . C69 . H691 . 109.1 no C68 . C69 . H692 . 108.1 no C60 . C69 . H692 . 109.0 no H691 . C69 . H692 . 109.4 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 C2 . H21 . O2 5_565 132 0.93 2.44 3.140(6) yes C65 . H541 . C52 . 135 0.98 2.55 3.316(6) yes C67 . H571 . C65 . 120 1.03 1.83 2.513(6) yes _iucr_refine_instructions_details ; # # Punched on 17/01/17 at 15:59:15 # #LIST 12 BLOCK SCALE X'S U'S EQUIV PART(1001,OCC) PART(1002,OCC) WEIGHT -1 PART(1002,OCC) RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 33,X'S) H ( 331,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 43,X'S) H ( 431,X'S) RIDE C ( 44,X'S) H ( 441,X'S) RIDE C ( 45,X'S) H ( 451,X'S) RIDE C ( 52,X'S) H ( 521,X'S) H ( 522,X'S) RIDE C ( 53,X'S) H ( 532,X'S) H ( 531,X'S) CONT H ( 533,X'S) H ( 534,X'S) RIDE C ( 54,X'S) H ( 541,X'S) H ( 542,X'S) RIDE C ( 55,X'S) H ( 552,X'S) H ( 551,X'S) RIDE C ( 56,X'S) H ( 561,X'S) H ( 562,X'S) RIDE C ( 57,X'S) H ( 572,X'S) H ( 571,X'S) RIDE C ( 58,X'S) H ( 581,X'S) H ( 582,X'S) RIDE C ( 59,X'S) H ( 592,X'S) H ( 591,X'S) RIDE C ( 60,X'S) H ( 602,X'S) H ( 601,X'S) CONT H ( 603,X'S) H ( 604,X'S) RIDE C ( 61,X'S) H ( 612,X'S) H ( 611,X'S) RIDE C ( 64,X'S) H ( 641,X'S) H ( 642,X'S) RIDE C ( 65,X'S) H ( 652,X'S) H ( 651,X'S) RIDE C ( 66,X'S) H ( 661,X'S) H ( 662,X'S) RIDE C ( 67,X'S) H ( 672,X'S) H ( 671,X'S) RIDE C ( 68,X'S) H ( 682,X'S) H ( 681,X'S) RIDE C ( 69,X'S) H ( 691,X'S) H ( 692,X'S) END # # Punched on 17/01/17 at 15:59:15 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) DIST 0,0.01 = MEAN CONT C(52) TO C(53) C(53) TO C(54) C(54) TO C(55) C(55) TO C(56) CONT C(56) TO C(57) C(57) TO C(58) C(58) TO C(59) C(59) TO C(60) CONT C(60) TO C(61) C(53) TO C(64) C(64) TO C(65) C(65) TO C(66) CONT C(66) TO C(67) C(67) TO C(68) C(68) TO C(69) C(69) TO C(60) VIBR .0, 0.00200 = S(1) TO C(51) VIBR .0, 0.00500 = C(51) TO C(36) VIBR .0, 0.00200 = S(2) TO C(62) VIBR .0, 0.00500 = C(62) TO C(46) VIBR .0, 0.00200 = O(1) TO C(51) VIBR .0, 0.00200 = O(2) TO C(62) VIBR .0, 0.00200 = C(51) TO C(52) VIBR .0, 0.00500 = O(1) TO S(1) VIBR .0, 0.00500 = C(52) TO S(1) VIBR .0, 0.00500 = C(52) TO O(1) VIBR .0, 0.00200 = C(52) TO C(53) VIBR .0, 0.00500 = C(53) TO C(51) VIBR .0, 0.00200 = C(53) TO C(54) VIBR .0, 0.00500 = C(54) TO C(52) VIBR .0, 0.00200 = C(53) TO C(64) VIBR .0, 0.00500 = C(64) TO C(52) VIBR .0, 0.00200 = C(54) TO C(55) VIBR .0, 0.00500 = C(55) TO C(53) VIBR .0, 0.00200 = C(55) TO C(56) VIBR .0, 0.00500 = C(56) TO C(54) VIBR .0, 0.00200 = C(56) TO C(57) VIBR .0, 0.00500 = C(57) TO C(55) VIBR .0, 0.00200 = C(57) TO C(58) VIBR .0, 0.00500 = C(58) TO C(56) VIBR .0, 0.00200 = C(58) TO C(59) VIBR .0, 0.00500 = C(59) TO C(57) VIBR .0, 0.00200 = C(59) TO C(60) VIBR .0, 0.00500 = C(60) TO C(58) VIBR .0, 0.00200 = C(60) TO C(61) VIBR .0, 0.00500 = C(61) TO C(59) VIBR .0, 0.00200 = C(60) TO C(61) VIBR .0, 0.00200 = C(60) TO C(69) VIBR .0, 0.00500 = C(69) TO C(61) VIBR .0, 0.00200 = C(61) TO C(62) VIBR .0, 0.00500 = C(62) TO C(60) VIBR .0, 0.00500 = S(2) TO C(61) VIBR .0, 0.00500 = O(2) TO C(61) VIBR .0, 0.00500 = O(2) TO S(2) VIBR .0, 0.00200 = C(64) TO C(65) VIBR .0, 0.00500 = C(65) TO C(53) VIBR .0, 0.00200 = C(65) TO C(66) VIBR .0, 0.00500 = C(66) TO C(64) VIBR .0, 0.00200 = C(66) TO C(67) VIBR .0, 0.00500 = C(67) TO C(65) VIBR .0, 0.00200 = C(67) TO C(68) VIBR .0, 0.00500 = C(68) TO C(66) VIBR .0, 0.00200 = C(68) TO C(69) VIBR .0, 0.00500 = C(69) TO C(67) VIBR .0, 0.00500 = C(60) TO C(68) U(IJ) .0, 0.04000 = S(1) TO C(51) U(IJ) .0, 0.04000 = S(2) TO C(62) U(IJ) .0, 0.08000 = O(1) TO C(51) U(IJ) .0, 0.08000 = O(2) TO C(62) U(IJ) .0, 0.04000 = C(51) TO C(52) U(IJ) .0, 0.04000 = C(52) TO C(53) U(IJ) .0, 0.04000 = C(53) TO C(54) U(IJ) .0, 0.04000 = C(53) TO C(64) U(IJ) .0, 0.04000 = C(54) TO C(55) U(IJ) .0, 0.04000 = C(55) TO C(56) U(IJ) .0, 0.04000 = C(56) TO C(57) U(IJ) .0, 0.04000 = C(57) TO C(58) U(IJ) .0, 0.04000 = C(58) TO C(59) U(IJ) .0, 0.04000 = C(59) TO C(60) U(IJ) .0, 0.04000 = C(60) TO C(61) U(IJ) .0, 0.04000 = C(60) TO C(61) U(IJ) .0, 0.04000 = C(60) TO C(69) U(IJ) .0, 0.04000 = C(61) TO C(62) U(IJ) .0, 0.04000 = C(64) TO C(65) U(IJ) .0, 0.04000 = C(65) TO C(66) U(IJ) .0, 0.04000 = C(66) TO C(67) U(IJ) .0, 0.04000 = C(67) TO C(68) U(IJ) .0, 0.04000 = C(68) TO C(69) END ;