# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- 5CIF.cif' #============================================================================== #FILL IN SECTIONS BELOW AS APPROPRIATE INSTEAD OF CAPITALISED GENERALITIES _publ_contact_author_name 'Paul D. Beer' _publ_contact_author_address ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA, UK. ; _publ_contact_author_email paul.beer@chem.ox.ac.uk _publ_section_title ; Triazole- and triazolium-containing porphyrin-cages for optical anion sensing ; loop_ _publ_author_name _publ_author_address 'Lydia C. Gilday' ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA, UK. ; 'Nicholas G. White' ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford, OX1 3TA, UK. ; 'Paul D. Beer' ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA, UK. ; _publ_section_abstract ; Triazole and triazolium groups have been integrated into a zinc(II) metalloporphyrin-based structural framework to produce two porphyrin-cages for anion sensing applications. UV/visible spectroscopic titration investigations reveal both host systems exhibit strong anion binding affinities, with the positively-charged triazolium-porphyrin cage capable of colorimetric sensing halides, fluoride and chloride, and oxoanions in acetone/water solvent mixtures. ; #============================================================================== data_COMPOUNDNAME _database_code_depnum_ccdc_archive 'CCDC 863074' #TrackingRef '- 5CIF.cif' #============================================================================== _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. ; _refine_special_details ; ? ; #--------------------------------------------------------------- # _oxford_ data items, April 2010: # There is some uncertainty about the correct way of forming local data # names, e.g. # _atom_site_special_shape_oxford # or # _oxford_atom_site_special_shape # see: # http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace # A reserved prefix, e.g. foo, must be used in the following way # " If the data file contains items defined in a DDL1 dictionary, the # local data names assigned under the reserved prefix must contain it as # their first component, e.g. _foo_atom_site_my_item. " # However, this seems to say the opposite: # http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html # According to advice from the IUCr, CRYSTALS is correct #--------------------------------------------------------------- # End of 'script/refcif.dat' #end of refcif _cell_length_a 14.7594(2) _cell_length_b 19.6725(2) _cell_length_c 26.8029(3) _cell_angle_alpha 90 _cell_angle_beta 99.6681(11) _cell_angle_gamma 90 _cell_volume 7671.81(16) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_space_group_name_Hall '-P 2ybc' 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 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' _cell_formula_units_Z 4 # Given Formula = C82 H70 N16 O12 # Dc = 1.27 Fooo = 3328.00 Mu = 7.21 M = 1471.56 # Found Formula = C85 H76 N16 O13 Zn1 # Dc = 1.38 FOOO = 3328.00 Mu = 10.79 M = 1595.02 _chemical_formula_sum 'C85 H76 N16 O13 Zn' _chemical_formula_moiety 'C73 H52 N16 O9 Zn, 4(C3 H6 O)' _chemical_compound_source synthesized _chemical_formula_weight 1595.02 _cell_measurement_reflns_used 22816 _cell_measurement_theta_min 3 _cell_measurement_theta_max 77 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_min 0.07 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 3328 _exptl_absorpt_coefficient_mu 1.079 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlis, (Oxford Diffraction, 2002)' _exptl_absorpt_correction_T_min 0.59304 _exptl_absorpt_correction_T_max 1.00 _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 'CrysAlis, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis, (Oxford Diffraction, 2002)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_ambient_temperature 150 _diffrn_reflns_number 56994 _reflns_number_total 16008 _diffrn_reflns_av_R_equivalents 0.0427 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 16008 # Theoretical number of reflections is about 26610 _diffrn_reflns_theta_min 3.345 _diffrn_reflns_theta_max 76.929 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 75.391 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _reflns_limit_h_min -18 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 24 _reflns_limit_l_min 0 _reflns_limit_l_max 33 _oxford_diffrn_Wilson_B_factor 1.83 _oxford_diffrn_Wilson_scale 0.20 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.58 _refine_diff_density_max 0.77 # 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 13286 _refine_ls_number_restraints 0 _refine_ls_number_parameters 1036 _oxford_refine_ls_R_factor_ref 0.0639 _refine_ls_wR_factor_ref 0.1612 _refine_ls_goodness_of_fit_ref 1.0464 _refine_ls_shift/su_max 0.0015985 _refine_ls_shift/su_mean 0.0000287 # The values computed from all data _oxford_reflns_number_all 13286 _refine_ls_R_factor_all 0.0639 _refine_ls_wR_factor_all 0.1612 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 11544 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_gt 0.1563 # 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 # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.06P)^2^ +20.16P] ,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. Oxford Diffraction, (2010). CrysAlisPro. Oxford Diffraction, (2010). Supernova User Manual. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. ; # 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 0.38318(3) 0.67538(2) 0.711878(16) 0.0204 1.0000 Uani . . . . . . O2 O 0.44594(16) 0.57365(12) 0.73584(9) 0.0279 1.0000 Uani . . . . . . C3 C 0.4253(2) 0.51414(17) 0.74094(13) 0.0277 1.0000 Uani . . . . . . C4 C 0.4970(3) 0.46280(19) 0.76120(16) 0.0360 1.0000 Uani . . . . . . C5 C 0.3295(3) 0.4883(2) 0.72522(19) 0.0461 1.0000 Uani . . . . . . N6 N 0.24869(18) 0.64534(13) 0.69219(10) 0.0215 1.0000 Uani . . . . . . C7 C 0.2112(2) 0.61399(16) 0.64787(12) 0.0231 1.0000 Uani . . . . . . C8 C 0.2523(2) 0.60847(15) 0.60446(13) 0.0225 1.0000 Uani . . . . . . C9 C 0.3379(2) 0.63593(16) 0.59912(12) 0.0221 1.0000 Uani . . . . . . N10 N 0.39728(18) 0.66826(13) 0.63646(10) 0.0203 1.0000 Uani . . . . . . C11 C 0.4684(2) 0.69225(16) 0.61421(12) 0.0220 1.0000 Uani . . . . . . C12 C 0.5429(2) 0.73047(16) 0.63877(13) 0.0223 1.0000 Uani . . . . . . C13 C 0.5580(2) 0.74834(16) 0.69020(13) 0.0221 1.0000 Uani . . . . . . N14 N 0.50077(18) 0.73373(13) 0.72430(10) 0.0207 1.0000 Uani . . . . . . C15 C 0.5412(2) 0.76123(16) 0.76968(12) 0.0218 1.0000 Uani . . . . . . C16 C 0.6276(2) 0.79260(16) 0.76404(13) 0.0242 1.0000 Uani . . . . . . C17 C 0.6369(2) 0.78480(17) 0.71529(13) 0.0256 1.0000 Uani . . . . . . C18 C 0.5025(2) 0.76253(15) 0.81402(12) 0.0217 1.0000 Uani . . . . . . C19 C 0.5554(2) 0.79851(16) 0.85893(12) 0.0230 1.0000 Uani . . . . . . C20 C 0.5208(2) 0.85884(16) 0.87660(12) 0.0238 1.0000 Uani . . . . . . C21 C 0.5684(2) 0.89237(17) 0.91863(13) 0.0261 1.0000 Uani . . . . . . C22 C 0.6516(3) 0.86612(19) 0.94289(14) 0.0329 1.0000 Uani . . . . . . C23 C 0.6871(3) 0.8069(2) 0.92530(15) 0.0355 1.0000 Uani . . . . . . C24 C 0.6388(2) 0.77339(18) 0.88385(14) 0.0287 1.0000 Uani . . . . . . C25 C 0.5302(3) 0.95576(18) 0.93988(14) 0.0331 1.0000 Uani . . . . . . N26 N 0.4578(2) 0.98916(14) 0.90460(11) 0.0285 1.0000 Uani . . . . . . N27 N 0.3685(2) 0.97726(18) 0.90693(13) 0.0417 1.0000 Uani . . . . . . N28 N 0.3200(2) 1.01028(18) 0.86952(13) 0.0396 1.0000 Uani . . . . . . C29 C 0.3770(2) 1.04312(17) 0.84244(13) 0.0275 1.0000 Uani . . . . . . C30 C 0.4652(3) 1.02901(17) 0.86508(13) 0.0279 1.0000 Uani . . . . . . C31 C 0.3431(2) 1.08785(17) 0.79822(13) 0.0279 1.0000 Uani . . . . . . O32 O 0.29312(17) 1.04505(12) 0.75775(9) 0.0275 1.0000 Uani . . . . . . C33 C 0.2807(2) 1.07220(16) 0.71132(13) 0.0229 1.0000 Uani . . . . . . O34 O 0.31121(17) 1.12623(12) 0.70090(9) 0.0298 1.0000 Uani . . . . . . C35 C 0.2190(2) 1.02936(15) 0.67396(13) 0.0226 1.0000 Uani . . . . . . C36 C 0.2297(2) 1.02732(16) 0.62300(13) 0.0230 1.0000 Uani . . . . . . C37 C 0.1633(2) 0.99630(16) 0.58745(13) 0.0252 1.0000 Uani . . . . . . C38 C 0.0848(2) 0.96788(15) 0.60160(13) 0.0223 1.0000 Uani . . . . . . C39 C 0.0740(2) 0.96951(15) 0.65225(13) 0.0225 1.0000 Uani . . . . . . C40 C 0.1417(2) 0.99979(16) 0.68801(13) 0.0225 1.0000 Uani . . . . . . C41 C -0.0134(2) 0.94365(16) 0.66709(13) 0.0245 1.0000 Uani . . . . . . O42 O -0.02614(16) 0.96959(12) 0.71140(9) 0.0265 1.0000 Uani . . . . . . C43 C -0.1154(2) 0.95594(18) 0.72641(14) 0.0292 1.0000 Uani . . . . . . C44 C -0.1129(2) 0.89572(17) 0.75984(13) 0.0249 1.0000 Uani . . . . . . N45 N -0.0993(2) 0.90192(16) 0.81113(12) 0.0355 1.0000 Uani . . . . . . N46 N -0.1023(2) 0.84087(17) 0.83113(12) 0.0371 1.0000 Uani . . . . . . N47 N -0.11788(19) 0.79624(14) 0.79261(11) 0.0258 1.0000 Uani . . . . . . C48 C -0.1246(2) 0.82865(18) 0.74776(13) 0.0255 1.0000 Uani . . . . . . C49 C -0.1275(2) 0.72366(18) 0.80226(15) 0.0301 1.0000 Uani . . . . . . C50 C -0.0367(2) 0.68736(17) 0.81635(13) 0.0253 1.0000 Uani . . . . . . C51 C -0.0261(2) 0.64160(17) 0.85663(13) 0.0254 1.0000 Uani . . . . . . C52 C 0.0546(2) 0.60450(17) 0.86933(13) 0.0267 1.0000 Uani . . . . . . C53 C 0.1245(2) 0.61226(17) 0.84142(13) 0.0250 1.0000 Uani . . . . . . C54 C 0.1161(2) 0.65811(16) 0.80120(12) 0.0230 1.0000 Uani . . . . . . C55 C 0.0354(2) 0.69523(17) 0.78885(13) 0.0257 1.0000 Uani . . . . . . C56 C 0.1951(2) 0.66628(16) 0.77307(12) 0.0218 1.0000 Uani . . . . . . C57 C 0.1837(2) 0.64250(16) 0.72344(13) 0.0223 1.0000 Uani . . . . . . C58 C 0.1036(2) 0.60750(18) 0.69760(13) 0.0268 1.0000 Uani . . . . . . C59 C 0.1207(2) 0.58931(17) 0.65161(13) 0.0269 1.0000 Uani . . . . . . C60 C 0.2759(2) 0.69503(16) 0.79985(12) 0.0227 1.0000 Uani . . . . . . N61 N 0.35530(18) 0.70635(13) 0.78105(10) 0.0210 1.0000 Uani . . . . . . C62 C 0.4153(2) 0.73750(15) 0.81877(12) 0.0220 1.0000 Uani . . . . . . C63 C 0.3733(2) 0.74367(17) 0.86330(13) 0.0268 1.0000 Uani . . . . . . C64 C 0.2875(2) 0.71844(18) 0.85149(13) 0.0279 1.0000 Uani . . . . . . O65 O -0.06603(18) 0.90641(13) 0.64085(10) 0.0355 1.0000 Uani . . . . . . C66 C 0.0093(2) 0.94614(16) 0.55949(12) 0.0237 1.0000 Uani . . . . . . O67 O 0.02849(16) 0.88704(11) 0.53920(9) 0.0261 1.0000 Uani . . . . . . C68 C -0.0359(2) 0.86835(17) 0.49380(13) 0.0277 1.0000 Uani . . . . . . C69 C -0.0268(2) 0.79452(17) 0.48367(12) 0.0235 1.0000 Uani . . . . . . N70 N -0.0867(2) 0.74911(15) 0.49737(14) 0.0378 1.0000 Uani . . . . . . N71 N -0.0667(2) 0.68827(16) 0.48185(15) 0.0431 1.0000 Uani . . . . . . N72 N 0.0057(2) 0.69523(14) 0.45847(11) 0.0288 1.0000 Uani . . . . . . C73 C 0.0326(3) 0.75943(18) 0.45871(13) 0.0297 1.0000 Uani . . . . . . C74 C 0.0444(3) 0.6348(2) 0.43770(15) 0.0416 1.0000 Uani . . . . . . C75 C 0.0962(3) 0.59040(18) 0.47827(13) 0.0291 1.0000 Uani . . . . . . C76 C 0.0924(3) 0.52070(19) 0.47247(15) 0.0335 1.0000 Uani . . . . . . C77 C 0.1393(3) 0.47875(18) 0.50985(16) 0.0378 1.0000 Uani . . . . . . C78 C 0.1909(3) 0.50655(18) 0.55310(14) 0.0312 1.0000 Uani . . . . . . C79 C 0.1968(2) 0.57698(17) 0.55854(13) 0.0243 1.0000 Uani . . . . . . C80 C 0.1491(2) 0.61779(17) 0.52115(13) 0.0270 1.0000 Uani . . . . . . O81 O -0.05634(17) 0.98074(12) 0.54368(10) 0.0319 1.0000 Uani . . . . . . C82 C 0.3093(2) 1.06141(17) 0.60435(13) 0.0267 1.0000 Uani . . . . . . O83 O 0.38932(16) 1.04275(12) 0.63172(10) 0.0287 1.0000 Uani . . . . . . C84 C 0.4696(3) 1.08280(19) 0.62471(18) 0.0398 1.0000 Uani . . . . . . C85 C 0.5476(2) 1.03670(17) 0.61818(14) 0.0288 1.0000 Uani . . . . . . N86 N 0.6240(2) 1.03365(18) 0.65437(13) 0.0394 1.0000 Uani . . . . . . N87 N 0.6837(2) 0.99313(17) 0.63845(13) 0.0376 1.0000 Uani . . . . . . N88 N 0.64598(19) 0.97098(14) 0.59219(11) 0.0256 1.0000 Uani . . . . . . C89 C 0.5611(3) 0.99666(18) 0.57855(14) 0.0308 1.0000 Uani . . . . . . C90 C 0.6988(3) 0.92609(18) 0.56438(15) 0.0334 1.0000 Uani . . . . . . C91 C 0.6824(2) 0.85118(17) 0.57166(13) 0.0262 1.0000 Uani . . . . . . C92 C 0.6214(2) 0.82617(17) 0.60139(13) 0.0241 1.0000 Uani . . . . . . C93 C 0.6100(2) 0.75626(17) 0.60727(12) 0.0240 1.0000 Uani . . . . . . C94 C 0.6623(2) 0.71143(17) 0.58322(13) 0.0269 1.0000 Uani . . . . . . C95 C 0.7227(3) 0.73658(18) 0.55345(14) 0.0309 1.0000 Uani . . . . . . C96 C 0.7323(3) 0.80577(19) 0.54736(14) 0.0313 1.0000 Uani . . . . . . O97 O 0.2986(2) 1.09943(15) 0.56892(11) 0.0426 1.0000 Uani . . . . . . C98 C 0.4530(2) 0.67357(17) 0.56113(13) 0.0257 1.0000 Uani . . . . . . C99 C 0.3730(2) 0.63801(17) 0.55198(13) 0.0258 1.0000 Uani . . . . . . O100 O 0.8461(2) 0.68816(18) 0.68329(13) 0.0577 1.0000 Uani . . . . . . C101 C 0.8858(3) 0.6793(2) 0.64789(16) 0.0402 1.0000 Uani . . . . . . C102 C 0.9487(3) 0.7317(2) 0.63268(18) 0.0487 1.0000 Uani . . . . . . C103 C 0.8751(3) 0.6137(2) 0.61834(19) 0.0498 1.0000 Uani . . . . . . O104 O 0.3626(2) 0.95008(15) 0.52533(12) 0.0484 1.0000 Uani . . . . . . C105 C 0.3446(3) 0.9012(2) 0.49735(16) 0.0424 1.0000 Uani . . . . . . C106 C 0.2516(4) 0.8938(3) 0.46547(19) 0.0588 1.0000 Uani . . . . . . C107 C 0.4147(4) 0.8481(3) 0.4925(2) 0.0576 1.0000 Uani . . . . . . O108 O 0.1157(2) 0.84076(18) 0.73474(14) 0.0597 1.0000 Uani . . . . . . C109 C 0.1719(3) 0.8614(2) 0.76982(18) 0.0460 1.0000 Uani . . . . . . C110 C 0.2707(3) 0.8719(2) 0.7657(2) 0.0516 1.0000 Uani . . . . . . C111 C 0.1452(4) 0.8782(4) 0.8191(2) 0.0782 1.0000 Uani . . . . . . O112 O 0.2606(3) 0.7902(2) 0.55380(15) 0.0725 1.0000 Uani . . . . . . C113 C 0.2583(4) 0.8076(2) 0.5974(2) 0.0556 1.0000 Uani . . . . . . C114 C 0.3375(4) 0.8458(3) 0.6276(2) 0.0678 1.0000 Uani . . . . . . C115 C 0.1786(4) 0.7914(3) 0.6219(2) 0.0679 1.0000 Uani . . . . . . H41 H 0.4778 0.4350 0.7870 0.0545 1.0000 Uiso R . . . . . H43 H 0.5532 0.4847 0.7750 0.0545 1.0000 Uiso R . . . . . H42 H 0.5075 0.4346 0.7334 0.0546 1.0000 Uiso R . . . . . H52 H 0.3146 0.4573 0.7499 0.0687 1.0000 Uiso R . . . . . H51 H 0.2863 0.5243 0.7205 0.0688 1.0000 Uiso R . . . . . H53 H 0.3261 0.4653 0.6936 0.0687 1.0000 Uiso R . . . . . H161 H 0.6693 0.8131 0.7902 0.0298 1.0000 Uiso R . . . . . H171 H 0.6855 0.8000 0.7003 0.0299 1.0000 Uiso R . . . . . H201 H 0.4647 0.8768 0.8594 0.0280 1.0000 Uiso R . . . . . H221 H 0.6840 0.8894 0.9714 0.0392 1.0000 Uiso R . . . . . H231 H 0.7436 0.7898 0.9411 0.0419 1.0000 Uiso R . . . . . H241 H 0.6624 0.7340 0.8726 0.0344 1.0000 Uiso R . . . . . H252 H 0.5798 0.9888 0.9492 0.0390 1.0000 Uiso R . . . . . H251 H 0.5043 0.9441 0.9693 0.0396 1.0000 Uiso R . . . . . H301 H 0.5205 1.0442 0.8558 0.0340 1.0000 Uiso R . . . . . H311 H 0.3021 1.1226 0.8080 0.0343 1.0000 Uiso R . . . . . H312 H 0.3954 1.1085 0.7867 0.0348 1.0000 Uiso R . . . . . H371 H 0.1701 0.9945 0.5533 0.0281 1.0000 Uiso R . . . . . H401 H 0.1336 1.0024 0.7218 0.0272 1.0000 Uiso R . . . . . H431 H -0.1282 0.9942 0.7458 0.0340 1.0000 Uiso R . . . . . H432 H -0.1622 0.9516 0.6960 0.0338 1.0000 Uiso R . . . . . H481 H -0.1337 0.8072 0.7163 0.0302 1.0000 Uiso R . . . . . H492 H -0.1616 0.7193 0.8299 0.0350 1.0000 Uiso R . . . . . H491 H -0.1622 0.7037 0.7722 0.0346 1.0000 Uiso R . . . . . H511 H -0.0726 0.6363 0.8756 0.0296 1.0000 Uiso R . . . . . H521 H 0.0628 0.5744 0.8972 0.0319 1.0000 Uiso R . . . . . H531 H 0.1787 0.5860 0.8501 0.0291 1.0000 Uiso R . . . . . H551 H 0.0300 0.7271 0.7616 0.0305 1.0000 Uiso R . . . . . H581 H 0.0487 0.6001 0.7106 0.0319 1.0000 Uiso R . . . . . H591 H 0.0824 0.5649 0.6258 0.0328 1.0000 Uiso R . . . . . H631 H 0.3999 0.7617 0.8944 0.0315 1.0000 Uiso R . . . . . H641 H 0.2428 0.7157 0.8731 0.0321 1.0000 Uiso R . . . . . H681 H -0.0976 0.8794 0.4983 0.0326 1.0000 Uiso R . . . . . H682 H -0.0202 0.8952 0.4655 0.0330 1.0000 Uiso R . . . . . H731 H 0.0817 0.7761 0.4446 0.0352 1.0000 Uiso R . . . . . H742 H 0.0876 0.6506 0.4165 0.0484 1.0000 Uiso R . . . . . H741 H -0.0052 0.6094 0.4184 0.0481 1.0000 Uiso R . . . . . H761 H 0.0578 0.5019 0.4423 0.0393 1.0000 Uiso R . . . . . H771 H 0.1357 0.4317 0.5059 0.0427 1.0000 Uiso R . . . . . H781 H 0.2229 0.4793 0.5783 0.0373 1.0000 Uiso R . . . . . H801 H 0.1529 0.6655 0.5250 0.0326 1.0000 Uiso R . . . . . H842 H 0.4874 1.1120 0.6538 0.0482 1.0000 Uiso R . . . . . H841 H 0.4539 1.1109 0.5947 0.0477 1.0000 Uiso R . . . . . H891 H 0.5220 0.9879 0.5487 0.0362 1.0000 Uiso R . . . . . H901 H 0.7637 0.9363 0.5759 0.0399 1.0000 Uiso R . . . . . H902 H 0.6819 0.9371 0.5289 0.0396 1.0000 Uiso R . . . . . H921 H 0.5859 0.8562 0.6173 0.0293 1.0000 Uiso R . . . . . H941 H 0.6575 0.6645 0.5878 0.0322 1.0000 Uiso R . . . . . H951 H 0.7588 0.7062 0.5380 0.0371 1.0000 Uiso R . . . . . H961 H 0.7728 0.8216 0.5269 0.0372 1.0000 Uiso R . . . . . H981 H 0.4914 0.6847 0.5378 0.0314 1.0000 Uiso R . . . . . H991 H 0.3457 0.6196 0.5207 0.0309 1.0000 Uiso R . . . . . H1023 H 1.0075 0.7130 0.6303 0.0726 1.0000 Uiso R . . . . . H1021 H 0.9584 0.7685 0.6566 0.0722 1.0000 Uiso R . . . . . H1022 H 0.9230 0.7492 0.6003 0.0721 1.0000 Uiso R . . . . . H1031 H 0.8864 0.6221 0.5841 0.0724 1.0000 Uiso R . . . . . H1032 H 0.9174 0.5797 0.6340 0.0720 1.0000 Uiso R . . . . . H1033 H 0.8136 0.5951 0.6162 0.0724 1.0000 Uiso R . . . . . H1063 H 0.2592 0.8909 0.4301 0.0870 1.0000 Uiso R . . . . . H1061 H 0.2152 0.9339 0.4696 0.0868 1.0000 Uiso R . . . . . H1062 H 0.2223 0.8525 0.4755 0.0872 1.0000 Uiso R . . . . . H1071 H 0.4234 0.8458 0.4571 0.0825 1.0000 Uiso R . . . . . H1073 H 0.4723 0.8592 0.5140 0.0818 1.0000 Uiso R . . . . . H1072 H 0.3933 0.8057 0.5029 0.0821 1.0000 Uiso R . . . . . H1102 H 0.3093 0.8484 0.7935 0.0750 1.0000 Uiso R . . . . . H1101 H 0.2862 0.9203 0.7692 0.0753 1.0000 Uiso R . . . . . H1103 H 0.2838 0.8553 0.7335 0.0755 1.0000 Uiso R . . . . . H1113 H 0.1850 0.8565 0.8464 0.1141 1.0000 Uiso R . . . . . H1111 H 0.1492 0.9265 0.8248 0.1137 1.0000 Uiso R . . . . . H1112 H 0.0830 0.8653 0.8191 0.1140 1.0000 Uiso R . . . . . H1141 H 0.3123 0.8878 0.6388 0.0974 1.0000 Uiso R . . . . . H1143 H 0.3816 0.8551 0.6056 0.0970 1.0000 Uiso R . . . . . H1142 H 0.3631 0.8186 0.6572 0.0967 1.0000 Uiso R . . . . . H1152 H 0.1973 0.7641 0.6518 0.0980 1.0000 Uiso R . . . . . H1151 H 0.1521 0.8325 0.6334 0.0986 1.0000 Uiso R . . . . . H1153 H 0.1303 0.7666 0.5996 0.0984 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 0.0212(2) 0.0172(2) 0.0225(2) -0.00041(16) 0.00306(17) -0.00149(16) O2 0.0310(13) 0.0198(12) 0.0335(13) 0.0030(10) 0.0068(10) 0.0024(10) C3 0.0324(19) 0.0243(18) 0.0265(18) 0.0013(14) 0.0056(14) 0.0011(14) C4 0.035(2) 0.0234(18) 0.048(2) 0.0037(16) 0.0045(17) 0.0030(15) C5 0.038(2) 0.029(2) 0.067(3) 0.0127(19) -0.005(2) -0.0054(17) N6 0.0223(14) 0.0172(13) 0.0246(14) 0.0008(11) 0.0027(11) 0.0006(11) C7 0.0255(16) 0.0170(15) 0.0253(17) 0.0007(13) 0.0003(13) 0.0020(13) C8 0.0266(16) 0.0134(14) 0.0263(17) 0.0004(12) 0.0009(13) 0.0018(12) C9 0.0256(16) 0.0168(15) 0.0232(16) 0.0004(12) 0.0014(13) 0.0032(13) N10 0.0225(13) 0.0149(12) 0.0232(14) 0.0009(10) 0.0027(11) -0.0003(10) C11 0.0234(16) 0.0178(15) 0.0251(17) 0.0035(13) 0.0045(13) 0.0023(13) C12 0.0225(16) 0.0169(15) 0.0282(17) 0.0027(13) 0.0061(13) 0.0031(12) C13 0.0242(16) 0.0159(15) 0.0266(17) 0.0031(12) 0.0055(13) 0.0027(12) N14 0.0239(14) 0.0156(12) 0.0227(14) -0.0008(10) 0.0043(11) 0.0002(11) C15 0.0218(16) 0.0159(15) 0.0268(17) 0.0002(12) 0.0014(13) 0.0013(12) C16 0.0239(16) 0.0187(15) 0.0288(18) 0.0001(13) 0.0007(14) -0.0033(13) C17 0.0221(16) 0.0212(16) 0.0340(19) 0.0011(14) 0.0061(14) -0.0022(13) C18 0.0246(16) 0.0135(14) 0.0256(17) -0.0004(12) -0.0003(13) 0.0017(12) C19 0.0241(16) 0.0207(16) 0.0243(17) 0.0011(13) 0.0047(13) -0.0025(13) C20 0.0248(16) 0.0204(16) 0.0245(17) 0.0000(13) -0.0008(13) 0.0000(13) C21 0.0308(18) 0.0219(16) 0.0248(17) 0.0004(13) 0.0020(14) -0.0035(14) C22 0.0338(19) 0.0304(19) 0.0307(19) -0.0021(15) -0.0057(15) -0.0044(15) C23 0.0284(19) 0.040(2) 0.034(2) -0.0017(16) -0.0054(15) 0.0053(16) C24 0.0263(17) 0.0268(18) 0.0314(19) -0.0002(14) 0.0004(14) 0.0028(14) C25 0.044(2) 0.0257(18) 0.0258(18) -0.0030(14) -0.0051(16) 0.0021(16) N26 0.0350(16) 0.0232(14) 0.0258(15) -0.0037(12) 0.0006(12) 0.0012(12) N27 0.0391(19) 0.044(2) 0.043(2) 0.0104(16) 0.0101(15) 0.0033(16) N28 0.0360(18) 0.0419(19) 0.0416(19) 0.0091(15) 0.0086(15) 0.0036(15) C29 0.0323(18) 0.0221(17) 0.0277(18) -0.0048(14) 0.0042(15) -0.0006(14) C30 0.0330(19) 0.0236(17) 0.0263(18) -0.0021(14) 0.0023(14) -0.0043(14) C31 0.0316(18) 0.0218(16) 0.0277(18) -0.0048(14) -0.0027(14) -0.0031(14) O32 0.0337(13) 0.0217(12) 0.0249(12) -0.0015(9) -0.0014(10) -0.0052(10) C33 0.0211(16) 0.0198(16) 0.0275(17) 0.0000(13) 0.0030(13) 0.0054(13) O34 0.0337(13) 0.0201(12) 0.0346(14) 0.0005(10) 0.0030(11) -0.0055(10) C35 0.0226(16) 0.0139(14) 0.0301(18) 0.0021(13) 0.0006(13) 0.0040(12) C36 0.0231(16) 0.0173(15) 0.0284(17) 0.0019(13) 0.0040(13) 0.0038(13) C37 0.0286(18) 0.0202(16) 0.0271(17) -0.0011(13) 0.0054(14) 0.0052(13) C38 0.0249(16) 0.0117(14) 0.0295(17) -0.0029(12) 0.0021(14) 0.0020(12) C39 0.0240(16) 0.0135(14) 0.0292(17) 0.0024(13) 0.0022(13) 0.0002(12) C40 0.0247(16) 0.0189(15) 0.0232(16) 0.0025(13) 0.0017(13) 0.0032(13) C41 0.0260(17) 0.0192(16) 0.0273(17) 0.0020(13) 0.0019(14) 0.0013(13) O42 0.0263(12) 0.0277(12) 0.0264(12) 0.0002(10) 0.0068(10) -0.0040(10) C43 0.0252(17) 0.0282(18) 0.0355(19) 0.0015(15) 0.0086(15) 0.0002(14) C44 0.0202(15) 0.0255(17) 0.0297(18) 0.0006(14) 0.0059(13) 0.0000(13) N45 0.0450(19) 0.0295(16) 0.0315(17) -0.0025(13) 0.0049(14) 0.0002(14) N46 0.0468(19) 0.0374(18) 0.0261(16) -0.0018(13) 0.0038(14) 0.0017(15) N47 0.0217(14) 0.0255(15) 0.0301(15) 0.0015(12) 0.0043(12) -0.0012(11) C48 0.0218(16) 0.0292(18) 0.0251(17) -0.0005(14) 0.0030(13) -0.0010(14) C49 0.0238(17) 0.0290(18) 0.038(2) 0.0073(15) 0.0067(15) -0.0031(14) C50 0.0236(17) 0.0231(16) 0.0286(18) 0.0015(13) 0.0029(14) -0.0025(13) C51 0.0256(17) 0.0237(17) 0.0277(17) -0.0013(14) 0.0065(14) -0.0072(13) C52 0.0343(19) 0.0216(16) 0.0241(17) 0.0033(13) 0.0045(14) -0.0073(14) C53 0.0262(17) 0.0206(16) 0.0270(17) -0.0002(13) 0.0012(14) -0.0034(13) C54 0.0252(17) 0.0203(16) 0.0235(16) -0.0013(13) 0.0044(13) -0.0057(13) C55 0.0261(17) 0.0240(17) 0.0266(17) 0.0046(13) 0.0037(14) -0.0036(14) C56 0.0227(16) 0.0180(15) 0.0248(16) 0.0032(13) 0.0041(13) 0.0010(12) C57 0.0216(16) 0.0181(15) 0.0271(17) 0.0032(13) 0.0036(13) 0.0002(12) C58 0.0198(16) 0.0296(18) 0.0302(18) -0.0002(14) 0.0021(14) -0.0032(14) C59 0.0228(16) 0.0263(17) 0.0295(18) -0.0041(14) -0.0020(14) -0.0019(14) C60 0.0263(17) 0.0170(15) 0.0255(17) 0.0016(13) 0.0064(13) 0.0000(13) N61 0.0219(13) 0.0175(13) 0.0233(14) 0.0002(11) 0.0029(11) -0.0014(11) C62 0.0265(17) 0.0155(15) 0.0232(16) -0.0002(12) 0.0017(13) 0.0005(13) C63 0.0322(18) 0.0226(17) 0.0249(17) -0.0030(13) 0.0027(14) -0.0048(14) C64 0.0299(18) 0.0275(18) 0.0282(18) -0.0015(14) 0.0106(14) -0.0037(14) O65 0.0323(14) 0.0355(14) 0.0387(15) -0.0088(12) 0.0059(11) -0.0116(11) C66 0.0283(17) 0.0195(16) 0.0239(16) -0.0004(13) 0.0064(14) 0.0003(14) O67 0.0297(12) 0.0187(11) 0.0277(12) -0.0050(9) -0.0020(10) 0.0009(9) C68 0.0315(18) 0.0218(17) 0.0265(18) -0.0031(14) -0.0043(14) -0.0004(14) C69 0.0255(16) 0.0206(16) 0.0229(16) -0.0012(13) -0.0003(13) -0.0025(13) N70 0.0346(17) 0.0223(15) 0.059(2) -0.0024(14) 0.0157(16) 0.0005(13) N71 0.0350(18) 0.0212(16) 0.073(3) -0.0058(16) 0.0083(17) -0.0050(13) N72 0.0373(17) 0.0229(14) 0.0236(15) -0.0041(12) -0.0024(12) 0.0080(12) C73 0.0334(19) 0.0265(18) 0.0303(19) 0.0008(14) 0.0086(15) 0.0019(15) C74 0.060(3) 0.031(2) 0.030(2) -0.0098(16) -0.0024(18) 0.0182(19) C75 0.0327(18) 0.0281(18) 0.0254(17) -0.0065(14) 0.0018(15) 0.0056(15) C76 0.034(2) 0.0289(19) 0.034(2) -0.0108(15) -0.0041(16) 0.0019(15) C77 0.042(2) 0.0194(17) 0.047(2) -0.0087(16) -0.0071(18) 0.0004(16) C78 0.0344(19) 0.0217(17) 0.035(2) 0.0000(15) -0.0014(16) 0.0033(15) C79 0.0228(16) 0.0242(17) 0.0259(17) -0.0028(13) 0.0044(13) -0.0005(13) C80 0.0351(19) 0.0179(16) 0.0270(18) -0.0038(13) 0.0026(15) 0.0021(14) O81 0.0307(13) 0.0257(12) 0.0360(14) -0.0080(10) -0.0036(11) 0.0064(11) C82 0.0282(18) 0.0227(17) 0.0295(18) -0.0011(14) 0.0056(14) -0.0019(14) O83 0.0228(12) 0.0219(12) 0.0428(14) 0.0016(10) 0.0098(11) -0.0017(9) C84 0.0280(19) 0.0255(19) 0.069(3) -0.0022(18) 0.0178(19) -0.0056(15) C85 0.0259(17) 0.0224(17) 0.039(2) 0.0004(15) 0.0078(15) -0.0061(14) N86 0.0352(18) 0.0412(19) 0.0406(19) -0.0103(15) 0.0034(15) 0.0018(15) N87 0.0280(16) 0.0402(18) 0.0426(19) -0.0066(15) 0.0004(14) 0.0029(14) N88 0.0250(14) 0.0207(14) 0.0323(16) 0.0029(12) 0.0076(12) -0.0013(11) C89 0.0295(18) 0.0276(18) 0.034(2) 0.0026(15) 0.0010(15) -0.0017(15) C90 0.036(2) 0.0258(18) 0.043(2) 0.0020(16) 0.0205(17) 0.0001(15) C91 0.0270(17) 0.0230(17) 0.0290(18) 0.0015(14) 0.0059(14) -0.0008(14) C92 0.0246(16) 0.0228(16) 0.0252(17) -0.0003(13) 0.0054(13) 0.0012(13) C93 0.0233(16) 0.0256(17) 0.0231(16) 0.0016(13) 0.0035(13) 0.0004(13) C94 0.0314(18) 0.0203(16) 0.0299(18) 0.0000(14) 0.0074(15) 0.0010(14) C95 0.0335(19) 0.0274(18) 0.0332(19) -0.0021(15) 0.0092(15) 0.0031(15) C96 0.0323(19) 0.0299(19) 0.0339(19) 0.0013(15) 0.0121(15) -0.0005(15) O97 0.0449(16) 0.0422(16) 0.0394(16) 0.0160(13) 0.0032(13) -0.0098(13) C98 0.0284(17) 0.0242(17) 0.0254(17) 0.0018(13) 0.0067(14) 0.0016(14) C99 0.0303(18) 0.0231(16) 0.0230(17) -0.0006(13) 0.0016(14) 0.0011(14) O100 0.068(2) 0.058(2) 0.0498(19) -0.0196(16) 0.0185(17) -0.0177(17) C101 0.038(2) 0.041(2) 0.038(2) -0.0065(18) -0.0019(18) 0.0023(18) C102 0.057(3) 0.039(2) 0.048(3) -0.0006(19) 0.006(2) 0.000(2) C103 0.040(2) 0.046(3) 0.060(3) -0.020(2) -0.002(2) 0.003(2) O104 0.0525(18) 0.0420(17) 0.0473(17) -0.0069(14) -0.0018(14) -0.0061(14) C105 0.048(2) 0.042(2) 0.034(2) 0.0036(18) -0.0015(18) -0.0068(19) C106 0.063(3) 0.052(3) 0.052(3) 0.001(2) -0.018(2) -0.007(2) C107 0.063(3) 0.053(3) 0.055(3) 0.002(2) 0.006(2) 0.005(2) O108 0.057(2) 0.055(2) 0.065(2) 0.0083(17) 0.0026(18) -0.0054(17) C109 0.047(3) 0.036(2) 0.053(3) 0.014(2) 0.005(2) 0.0034(19) C110 0.050(3) 0.037(2) 0.069(3) 0.011(2) 0.012(2) 0.004(2) C111 0.054(3) 0.120(5) 0.062(3) -0.002(3) 0.013(3) 0.005(3) O112 0.095(3) 0.069(2) 0.059(2) 0.0041(19) 0.026(2) 0.008(2) C113 0.076(3) 0.036(2) 0.057(3) 0.014(2) 0.018(3) 0.016(2) C114 0.082(4) 0.053(3) 0.068(3) 0.009(3) 0.010(3) 0.014(3) C115 0.086(4) 0.054(3) 0.070(4) 0.024(3) 0.030(3) 0.027(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 1.943(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 . O2 . 2.253(2) yes Zn1 . N6 . 2.053(3) yes Zn1 . N10 . 2.071(3) yes Zn1 . N14 . 2.061(3) yes Zn1 . N61 . 2.058(3) yes O2 . C3 . 1.223(4) yes C3 . C4 . 1.497(5) yes C3 . C5 . 1.495(5) yes C4 . H41 . 0.959 no C4 . H43 . 0.954 no C4 . H42 . 0.961 no C5 . H52 . 0.950 no C5 . H51 . 0.948 no C5 . H53 . 0.954 no N6 . C7 . 1.370(4) yes N6 . C57 . 1.376(4) yes C7 . C8 . 1.404(5) yes C7 . C59 . 1.440(5) yes C8 . C9 . 1.403(5) yes C8 . C79 . 1.494(5) yes C9 . N10 . 1.371(4) yes C9 . C99 . 1.445(5) yes N10 . C11 . 1.375(4) yes C11 . C12 . 1.401(5) yes C11 . C98 . 1.450(5) yes C12 . C13 . 1.404(5) yes C12 . C93 . 1.494(5) yes C13 . N14 . 1.376(4) yes C13 . C17 . 1.435(5) yes N14 . C15 . 1.373(4) yes C15 . C16 . 1.448(5) yes C15 . C18 . 1.403(5) yes C16 . C17 . 1.346(5) yes C16 . H161 . 0.941 no C17 . H171 . 0.927 no C18 . C19 . 1.498(4) yes C18 . C62 . 1.403(5) yes C19 . C20 . 1.406(5) yes C19 . C24 . 1.389(5) yes C20 . C21 . 1.390(5) yes C20 . H201 . 0.945 no C21 . C22 . 1.390(5) yes C21 . C25 . 1.518(5) yes C22 . C23 . 1.391(5) yes C22 . H221 . 0.949 no C23 . C24 . 1.383(5) yes C23 . H231 . 0.933 no C24 . H241 . 0.921 no C25 . N26 . 1.460(5) yes C25 . H252 . 0.980 no C25 . H251 . 0.960 no N26 . N27 . 1.350(5) yes N26 . C30 . 1.337(5) yes N27 . N28 . 1.303(5) yes N28 . C29 . 1.363(5) yes C29 . C30 . 1.370(5) yes C29 . C31 . 1.493(5) yes C30 . H301 . 0.941 no C31 . O32 . 1.470(4) yes C31 . H311 . 0.978 no C31 . H312 . 0.967 no O32 . C33 . 1.338(4) yes C33 . O34 . 1.205(4) yes C33 . C35 . 1.495(5) yes C35 . C36 . 1.402(5) yes C35 . C40 . 1.388(5) yes C36 . C37 . 1.388(5) yes C36 . C82 . 1.509(5) yes C37 . C38 . 1.395(5) yes C37 . H371 . 0.938 no C38 . C39 . 1.394(5) yes C38 . C66 . 1.509(5) yes C39 . C40 . 1.397(5) yes C39 . C41 . 1.501(5) yes C40 . H401 . 0.935 no C41 . O42 . 1.335(4) yes C41 . O65 . 1.205(4) yes O42 . C43 . 1.465(4) yes C43 . C44 . 1.482(5) yes C43 . H431 . 0.951 no C43 . H432 . 0.981 no C44 . N45 . 1.361(5) yes C44 . C48 . 1.363(5) yes N45 . N46 . 1.319(5) yes N46 . N47 . 1.345(4) yes N47 . C48 . 1.349(4) yes N47 . C49 . 1.462(4) yes C48 . H481 . 0.931 no C49 . C50 . 1.509(5) yes C49 . H492 . 0.967 no C49 . H491 . 0.963 no C50 . C51 . 1.394(5) yes C50 . C55 . 1.401(5) yes C51 . C52 . 1.389(5) yes C51 . H511 . 0.925 no C52 . C53 . 1.382(5) yes C52 . H521 . 0.944 no C53 . C54 . 1.395(5) yes C53 . H531 . 0.947 no C54 . C55 . 1.389(5) yes C54 . C56 . 1.500(4) yes C55 . H551 . 0.957 no C56 . C57 . 1.394(5) yes C56 . C60 . 1.403(5) yes C57 . C58 . 1.442(5) yes C58 . C59 . 1.348(5) yes C58 . H581 . 0.944 no C59 . H591 . 0.948 no C60 . N61 . 1.370(4) yes C60 . C64 . 1.441(5) yes N61 . C62 . 1.372(4) yes C62 . C63 . 1.440(5) yes C63 . C64 . 1.347(5) yes C63 . H631 . 0.932 no C64 . H641 . 0.949 no C66 . O67 . 1.334(4) yes C66 . O81 . 1.201(4) yes O67 . C68 . 1.460(4) yes C68 . C69 . 1.488(5) yes C68 . H681 . 0.963 no C68 . H682 . 0.984 no C69 . N70 . 1.351(5) yes C69 . C73 . 1.375(5) yes N70 . N71 . 1.317(4) yes N71 . N72 . 1.333(5) yes N72 . C73 . 1.324(5) yes N72 . C74 . 1.469(4) yes C73 . H731 . 0.932 no C74 . C75 . 1.500(5) yes C74 . H742 . 0.974 no C74 . H741 . 0.962 no C75 . C76 . 1.380(5) yes C75 . C80 . 1.385(5) yes C76 . C77 . 1.390(5) yes C76 . H761 . 0.956 no C77 . C78 . 1.388(5) yes C77 . H771 . 0.932 no C78 . C79 . 1.394(5) yes C78 . H781 . 0.927 no C79 . C80 . 1.382(5) yes C80 . H801 . 0.944 no C82 . O83 . 1.333(4) yes C82 . O97 . 1.198(4) yes O83 . C84 . 1.461(4) yes C84 . C85 . 1.499(5) yes C84 . H842 . 0.969 no C84 . H841 . 0.972 no C85 . N86 . 1.359(5) yes C85 . C89 . 1.364(5) yes N86 . N87 . 1.312(5) yes N87 . N88 . 1.344(4) yes N88 . C89 . 1.343(5) yes N88 . C90 . 1.463(4) yes C89 . H891 . 0.922 no C90 . C91 . 1.511(5) yes C90 . H901 . 0.975 no C90 . H902 . 0.967 no C91 . C92 . 1.388(5) yes C91 . C96 . 1.388(5) yes C92 . C93 . 1.398(5) yes C92 . H921 . 0.939 no C93 . C94 . 1.398(5) yes C94 . C95 . 1.384(5) yes C94 . H941 . 0.935 no C95 . C96 . 1.381(5) yes C95 . H951 . 0.942 no C96 . H961 . 0.929 no C98 . C99 . 1.358(5) yes C98 . H981 . 0.938 no C99 . H991 . 0.939 no O100 . C101 . 1.208(5) yes C101 . C102 . 1.489(6) yes C101 . C103 . 1.508(6) yes C102 . H1023 . 0.953 no C102 . H1021 . 0.963 no C102 . H1022 . 0.951 no C103 . H1031 . 0.974 no C103 . H1032 . 0.963 no C103 . H1033 . 0.972 no O104 . C105 . 1.220(5) yes C105 . C106 . 1.497(6) yes C105 . C107 . 1.492(7) yes C106 . H1063 . 0.976 no C106 . H1061 . 0.970 no C106 . H1062 . 0.980 no C107 . H1071 . 0.979 no C107 . H1073 . 0.968 no C107 . H1072 . 0.949 no O108 . C109 . 1.215(6) yes C109 . C110 . 1.495(6) yes C109 . C111 . 1.477(7) yes C110 . H1102 . 0.975 no C110 . H1101 . 0.981 no C110 . H1103 . 0.972 no C111 . H1113 . 0.957 no C111 . H1111 . 0.963 no C111 . H1112 . 0.953 no O112 . C113 . 1.222(6) yes C113 . C114 . 1.508(8) yes C113 . C115 . 1.475(7) yes C114 . H1141 . 0.971 no C114 . H1143 . 0.967 no C114 . H1142 . 0.978 no C115 . H1152 . 0.967 no C115 . H1151 . 0.970 no C115 . H1153 . 0.978 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O2 . Zn1 . N6 . 98.69(10) yes O2 . Zn1 . N10 . 96.56(9) yes N6 . Zn1 . N10 . 88.91(11) yes O2 . Zn1 . N14 . 98.86(10) yes N6 . Zn1 . N14 . 162.45(10) yes N10 . Zn1 . N14 . 88.59(10) yes O2 . Zn1 . N61 . 98.10(10) yes N6 . Zn1 . N61 . 89.19(11) yes N10 . Zn1 . N61 . 165.33(10) yes N14 . Zn1 . N61 . 88.85(10) yes Zn1 . O2 . C3 . 141.6(2) yes O2 . C3 . C4 . 120.8(3) yes O2 . C3 . C5 . 122.4(3) yes C4 . C3 . C5 . 116.7(3) yes C3 . C4 . H41 . 111.7 no C3 . C4 . H43 . 110.6 no H41 . C4 . H43 . 108.8 no C3 . C4 . H42 . 107.7 no H41 . C4 . H42 . 109.5 no H43 . C4 . H42 . 108.5 no C3 . C5 . H52 . 109.9 no C3 . C5 . H51 . 111.5 no H52 . C5 . H51 . 110.1 no C3 . C5 . H53 . 108.5 no H52 . C5 . H53 . 109.3 no H51 . C5 . H53 . 107.5 no Zn1 . N6 . C7 . 125.8(2) yes Zn1 . N6 . C57 . 126.7(2) yes C7 . N6 . C57 . 106.7(3) yes N6 . C7 . C8 . 125.8(3) yes N6 . C7 . C59 . 109.6(3) yes C8 . C7 . C59 . 124.5(3) yes C7 . C8 . C9 . 125.2(3) yes C7 . C8 . C79 . 117.5(3) yes C9 . C8 . C79 . 117.0(3) yes C8 . C9 . N10 . 125.5(3) yes C8 . C9 . C99 . 124.2(3) yes N10 . C9 . C99 . 110.2(3) yes C9 . N10 . Zn1 . 125.9(2) yes C9 . N10 . C11 . 106.5(3) yes Zn1 . N10 . C11 . 127.5(2) yes N10 . C11 . C12 . 125.2(3) yes N10 . C11 . C98 . 109.4(3) yes C12 . C11 . C98 . 125.4(3) yes C11 . C12 . C13 . 125.4(3) yes C11 . C12 . C93 . 117.3(3) yes C13 . C12 . C93 . 117.3(3) yes C12 . C13 . N14 . 125.9(3) yes C12 . C13 . C17 . 124.6(3) yes N14 . C13 . C17 . 109.5(3) yes C13 . N14 . Zn1 . 127.1(2) yes C13 . N14 . C15 . 106.4(3) yes Zn1 . N14 . C15 . 126.3(2) yes N14 . C15 . C16 . 109.6(3) yes N14 . C15 . C18 . 125.4(3) yes C16 . C15 . C18 . 124.9(3) yes C15 . C16 . C17 . 106.8(3) yes C15 . C16 . H161 . 125.6 no C17 . C16 . H161 . 127.7 no C13 . C17 . C16 . 107.8(3) yes C13 . C17 . H171 . 125.7 no C16 . C17 . H171 . 126.5 no C15 . C18 . C19 . 117.2(3) yes C15 . C18 . C62 . 125.5(3) yes C19 . C18 . C62 . 117.1(3) yes C18 . C19 . C20 . 120.0(3) yes C18 . C19 . C24 . 121.2(3) yes C20 . C19 . C24 . 118.8(3) yes C19 . C20 . C21 . 120.7(3) yes C19 . C20 . H201 . 119.3 no C21 . C20 . H201 . 120.0 no C20 . C21 . C22 . 119.3(3) yes C20 . C21 . C25 . 121.7(3) yes C22 . C21 . C25 . 119.0(3) yes C21 . C22 . C23 . 120.4(3) yes C21 . C22 . H221 . 118.9 no C23 . C22 . H221 . 120.7 no C22 . C23 . C24 . 119.9(3) yes C22 . C23 . H231 . 120.5 no C24 . C23 . H231 . 119.6 no C19 . C24 . C23 . 120.8(3) yes C19 . C24 . H241 . 119.7 no C23 . C24 . H241 . 119.5 no C21 . C25 . N26 . 113.9(3) yes C21 . C25 . H252 . 109.4 no N26 . C25 . H252 . 107.5 no C21 . C25 . H251 . 109.7 no N26 . C25 . H251 . 106.9 no H252 . C25 . H251 . 109.5 no C25 . N26 . N27 . 120.4(3) yes C25 . N26 . C30 . 128.9(3) yes N27 . N26 . C30 . 110.5(3) yes N26 . N27 . N28 . 107.0(3) yes N27 . N28 . C29 . 109.7(3) yes N28 . C29 . C30 . 107.1(3) yes N28 . C29 . C31 . 123.2(3) yes C30 . C29 . C31 . 129.6(3) yes C29 . C30 . N26 . 105.7(3) yes C29 . C30 . H301 . 128.4 no N26 . C30 . H301 . 125.9 no C29 . C31 . O32 . 107.9(3) yes C29 . C31 . H311 . 109.8 no O32 . C31 . H311 . 109.9 no C29 . C31 . H312 . 108.8 no O32 . C31 . H312 . 109.5 no H311 . C31 . H312 . 110.9 no C31 . O32 . C33 . 115.5(3) yes O32 . C33 . O34 . 124.7(3) yes O32 . C33 . C35 . 111.8(3) yes O34 . C33 . C35 . 123.4(3) yes C33 . C35 . C36 . 120.9(3) yes C33 . C35 . C40 . 119.4(3) yes C36 . C35 . C40 . 119.0(3) yes C35 . C36 . C37 . 120.0(3) yes C35 . C36 . C82 . 122.1(3) yes C37 . C36 . C82 . 117.9(3) yes C36 . C37 . C38 . 120.8(3) yes C36 . C37 . H371 . 120.5 no C38 . C37 . H371 . 118.7 no C37 . C38 . C39 . 119.4(3) yes C37 . C38 . C66 . 116.9(3) yes C39 . C38 . C66 . 123.0(3) yes C38 . C39 . C40 . 119.5(3) yes C38 . C39 . C41 . 119.6(3) yes C40 . C39 . C41 . 120.7(3) yes C39 . C40 . C35 . 121.3(3) yes C39 . C40 . H401 . 119.6 no C35 . C40 . H401 . 119.0 no C39 . C41 . O42 . 111.2(3) yes C39 . C41 . O65 . 123.4(3) yes O42 . C41 . O65 . 125.3(3) yes C41 . O42 . C43 . 116.2(3) yes O42 . C43 . C44 . 112.4(3) yes O42 . C43 . H431 . 105.9 no C44 . C43 . H431 . 106.9 no O42 . C43 . H432 . 109.2 no C44 . C43 . H432 . 112.1 no H431 . C43 . H432 . 110.2 no C43 . C44 . N45 . 121.6(3) yes C43 . C44 . C48 . 129.9(3) yes N45 . C44 . C48 . 108.5(3) yes C44 . N45 . N46 . 108.6(3) yes N45 . N46 . N47 . 107.2(3) yes N46 . N47 . C48 . 110.7(3) yes N46 . N47 . C49 . 120.7(3) yes C48 . N47 . C49 . 128.6(3) yes C44 . C48 . N47 . 105.0(3) yes C44 . C48 . H481 . 130.3 no N47 . C48 . H481 . 124.7 no N47 . C49 . C50 . 113.4(3) yes N47 . C49 . H492 . 107.5 no C50 . C49 . H492 . 108.7 no N47 . C49 . H491 . 107.7 no C50 . C49 . H491 . 110.0 no H492 . C49 . H491 . 109.4 no C49 . C50 . C51 . 118.6(3) yes C49 . C50 . C55 . 122.5(3) yes C51 . C50 . C55 . 118.8(3) yes C50 . C51 . C52 . 120.6(3) yes C50 . C51 . H511 . 120.1 no C52 . C51 . H511 . 119.3 no C51 . C52 . C53 . 119.8(3) yes C51 . C52 . H521 . 120.9 no C53 . C52 . H521 . 119.2 no C52 . C53 . C54 . 120.8(3) yes C52 . C53 . H531 . 118.9 no C54 . C53 . H531 . 120.3 no C53 . C54 . C55 . 119.1(3) yes C53 . C54 . C56 . 118.8(3) yes C55 . C54 . C56 . 122.1(3) yes C50 . C55 . C54 . 120.9(3) yes C50 . C55 . H551 . 120.1 no C54 . C55 . H551 . 119.0 no C54 . C56 . C57 . 117.7(3) yes C54 . C56 . C60 . 116.8(3) yes C57 . C56 . C60 . 125.4(3) yes C56 . C57 . N6 . 125.7(3) yes C56 . C57 . C58 . 125.2(3) yes N6 . C57 . C58 . 109.1(3) yes C57 . C58 . C59 . 107.5(3) yes C57 . C58 . H581 . 125.6 no C59 . C58 . H581 . 126.9 no C7 . C59 . C58 . 107.0(3) yes C7 . C59 . H591 . 124.5 no C58 . C59 . H591 . 128.5 no C56 . C60 . N61 . 125.7(3) yes C56 . C60 . C64 . 125.0(3) yes N61 . C60 . C64 . 109.3(3) yes C60 . N61 . Zn1 . 126.6(2) yes C60 . N61 . C62 . 106.8(3) yes Zn1 . N61 . C62 . 126.4(2) yes C18 . C62 . N61 . 125.4(3) yes C18 . C62 . C63 . 125.1(3) yes N61 . C62 . C63 . 109.5(3) yes C62 . C63 . C64 . 107.0(3) yes C62 . C63 . H631 . 126.8 no C64 . C63 . H631 . 126.2 no C60 . C64 . C63 . 107.4(3) yes C60 . C64 . H641 . 125.7 no C63 . C64 . H641 . 126.9 no C38 . C66 . O67 . 111.8(3) yes C38 . C66 . O81 . 123.6(3) yes O67 . C66 . O81 . 124.3(3) yes C66 . O67 . C68 . 114.0(3) yes O67 . C68 . C69 . 109.4(3) yes O67 . C68 . H681 . 109.6 no C69 . C68 . H681 . 111.1 no O67 . C68 . H682 . 107.7 no C69 . C68 . H682 . 110.0 no H681 . C68 . H682 . 109.0 no C68 . C69 . N70 . 120.8(3) yes C68 . C69 . C73 . 131.6(3) yes N70 . C69 . C73 . 107.5(3) yes C69 . N70 . N71 . 108.8(3) yes N70 . N71 . N72 . 107.2(3) yes N71 . N72 . C73 . 111.1(3) yes N71 . N72 . C74 . 119.2(3) yes C73 . N72 . C74 . 129.7(3) yes C69 . C73 . N72 . 105.4(3) yes C69 . C73 . H731 . 128.6 no N72 . C73 . H731 . 126.0 no N72 . C74 . C75 . 112.3(3) yes N72 . C74 . H742 . 107.2 no C75 . C74 . H742 . 107.8 no N72 . C74 . H741 . 108.3 no C75 . C74 . H741 . 109.7 no H742 . C74 . H741 . 111.5 no C74 . C75 . C76 . 119.3(3) yes C74 . C75 . C80 . 121.5(3) yes C76 . C75 . C80 . 119.1(3) yes C75 . C76 . C77 . 120.2(3) yes C75 . C76 . H761 . 119.1 no C77 . C76 . H761 . 120.7 no C76 . C77 . C78 . 120.3(3) yes C76 . C77 . H771 . 119.8 no C78 . C77 . H771 . 119.9 no C77 . C78 . C79 . 119.7(3) yes C77 . C78 . H781 . 121.4 no C79 . C78 . H781 . 118.9 no C8 . C79 . C78 . 121.0(3) yes C8 . C79 . C80 . 119.9(3) yes C78 . C79 . C80 . 119.1(3) yes C75 . C80 . C79 . 121.6(3) yes C75 . C80 . H801 . 119.5 no C79 . C80 . H801 . 118.9 no C36 . C82 . O83 . 111.3(3) yes C36 . C82 . O97 . 122.3(3) yes O83 . C82 . O97 . 126.4(3) yes C82 . O83 . C84 . 116.3(3) yes O83 . C84 . C85 . 110.1(3) yes O83 . C84 . H842 . 109.4 no C85 . C84 . H842 . 110.1 no O83 . C84 . H841 . 109.1 no C85 . C84 . H841 . 109.2 no H842 . C84 . H841 . 108.9 no C84 . C85 . N86 . 120.3(3) yes C84 . C85 . C89 . 131.0(4) yes N86 . C85 . C89 . 108.6(3) yes C85 . N86 . N87 . 108.4(3) yes N86 . N87 . N88 . 107.5(3) yes N87 . N88 . C89 . 110.6(3) yes N87 . N88 . C90 . 119.5(3) yes C89 . N88 . C90 . 129.9(3) yes C85 . C89 . N88 . 104.9(3) yes C85 . C89 . H891 . 129.2 no N88 . C89 . H891 . 125.9 no N88 . C90 . C91 . 114.3(3) yes N88 . C90 . H901 . 107.1 no C91 . C90 . H901 . 109.3 no N88 . C90 . H902 . 107.1 no C91 . C90 . H902 . 108.9 no H901 . C90 . H902 . 110.1 no C90 . C91 . C92 . 123.6(3) yes C90 . C91 . C96 . 117.2(3) yes C92 . C91 . C96 . 119.2(3) yes C91 . C92 . C93 . 121.0(3) yes C91 . C92 . H921 . 120.2 no C93 . C92 . H921 . 118.8 no C12 . C93 . C92 . 120.1(3) yes C12 . C93 . C94 . 121.1(3) yes C92 . C93 . C94 . 118.9(3) yes C93 . C94 . C95 . 119.9(3) yes C93 . C94 . H941 . 120.1 no C95 . C94 . H941 . 119.9 no C94 . C95 . C96 . 120.6(3) yes C94 . C95 . H951 . 119.5 no C96 . C95 . H951 . 119.8 no C91 . C96 . C95 . 120.4(3) yes C91 . C96 . H961 . 120.3 no C95 . C96 . H961 . 119.3 no C11 . C98 . C99 . 107.3(3) yes C11 . C98 . H981 . 125.6 no C99 . C98 . H981 . 127.1 no C9 . C99 . C98 . 106.6(3) yes C9 . C99 . H991 . 127.2 no C98 . C99 . H991 . 126.2 no O100 . C101 . C102 . 121.5(4) yes O100 . C101 . C103 . 120.9(4) yes C102 . C101 . C103 . 117.5(4) yes C101 . C102 . H1023 . 111.6 no C101 . C102 . H1021 . 111.6 no H1023 . C102 . H1021 . 107.4 no C101 . C102 . H1022 . 109.2 no H1023 . C102 . H1022 . 107.8 no H1021 . C102 . H1022 . 109.0 no C101 . C103 . H1031 . 109.4 no C101 . C103 . H1032 . 111.3 no H1031 . C103 . H1032 . 109.2 no C101 . C103 . H1033 . 111.5 no H1031 . C103 . H1033 . 108.3 no H1032 . C103 . H1033 . 107.0 no O104 . C105 . C106 . 120.7(4) yes O104 . C105 . C107 . 121.5(4) yes C106 . C105 . C107 . 117.7(4) yes C105 . C106 . H1063 . 108.5 no C105 . C106 . H1061 . 109.2 no H1063 . C106 . H1061 . 108.3 no C105 . C106 . H1062 . 109.2 no H1063 . C106 . H1062 . 110.3 no H1061 . C106 . H1062 . 111.4 no C105 . C107 . H1071 . 108.8 no C105 . C107 . H1073 . 110.0 no H1071 . C107 . H1073 . 110.0 no C105 . C107 . H1072 . 108.6 no H1071 . C107 . H1072 . 110.4 no H1073 . C107 . H1072 . 109.1 no O108 . C109 . C110 . 122.5(5) yes O108 . C109 . C111 . 121.1(5) yes C110 . C109 . C111 . 116.4(5) yes C109 . C110 . H1102 . 109.3 no C109 . C110 . H1101 . 110.0 no H1102 . C110 . H1101 . 106.9 no C109 . C110 . H1103 . 111.2 no H1102 . C110 . H1103 . 109.9 no H1101 . C110 . H1103 . 109.5 no C109 . C111 . H1113 . 111.2 no C109 . C111 . H1111 . 110.2 no H1113 . C111 . H1111 . 107.8 no C109 . C111 . H1112 . 110.0 no H1113 . C111 . H1112 . 110.4 no H1111 . C111 . H1112 . 107.2 no O112 . C113 . C114 . 120.7(5) yes O112 . C113 . C115 . 121.1(6) yes C114 . C113 . C115 . 118.2(5) yes C113 . C114 . H1141 . 106.7 no C113 . C114 . H1143 . 107.8 no H1141 . C114 . H1143 . 111.0 no C113 . C114 . H1142 . 108.8 no H1141 . C114 . H1142 . 109.5 no H1143 . C114 . H1142 . 112.8 no C113 . C115 . H1152 . 110.6 no C113 . C115 . H1151 . 110.8 no H1152 . C115 . H1151 . 105.8 no C113 . C115 . H1153 . 113.0 no H1152 . C115 . H1153 . 107.8 no H1151 . C115 . H1153 . 108.5 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 C5 . H51 . N6 . 148.45(12) 0.948 2.532 3.377(5) yes C31 . H311 . O100 4_656 161.03(11) 0.978 2.583 3.522(5) yes C48 . H481 . O100 1_455 137.27(11) 0.931 2.503 3.250(5) yes C49 . H491 . O100 1_455 139.96(11) 0.963 2.426 3.223(5) yes C52 . H521 . O81 4_546 166.40(10) 0.944 2.443 3.368(5) yes C89 . H891 . O104 . 135.59(12) 0.922 2.446 3.171(5) yes C106 . H1062 . O112 . 127.55(16) 0.980 2.413 3.110(5) yes C107 . H1072 . O112 . 125.27(14) 0.949 2.587 3.229(5) yes C110 . H1101 . O32 . 164.58(13) 0.981 2.477 3.432(5) yes _iucr_refine_instruction_details_constraints ; # # Punched on 24/10/11 at 09:54:12 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 4,X'S) H ( 41,X'S) H ( 43,X'S) H ( 42,X'S) RIDE C ( 5,X'S) H ( 52,X'S) H ( 51,X'S) H ( 53,X'S) RIDE C ( 16,X'S) H ( 161,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 20,X'S) H ( 201,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 ( 252,X'S) H ( 251,X'S) RIDE C ( 30,X'S) H ( 301,X'S) RIDE C ( 31,X'S) H ( 311,X'S) H ( 312,X'S) RIDE C ( 37,X'S) H ( 371,X'S) RIDE C ( 40,X'S) H ( 401,X'S) RIDE C ( 43,X'S) H ( 431,X'S) H ( 432,X'S) RIDE C ( 48,X'S) H ( 481,X'S) RIDE C ( 49,X'S) H ( 492,X'S) H ( 491,X'S) RIDE C ( 51,X'S) H ( 511,X'S) RIDE C ( 52,X'S) H ( 521,X'S) RIDE C ( 53,X'S) H ( 531,X'S) RIDE C ( 55,X'S) H ( 551,X'S) RIDE C ( 58,X'S) H ( 581,X'S) RIDE C ( 59,X'S) H ( 591,X'S) RIDE C ( 63,X'S) H ( 631,X'S) RIDE C ( 64,X'S) H ( 641,X'S) RIDE C ( 68,X'S) H ( 681,X'S) H ( 682,X'S) RIDE C ( 73,X'S) H ( 731,X'S) RIDE C ( 74,X'S) H ( 742,X'S) H ( 741,X'S) RIDE C ( 76,X'S) H ( 761,X'S) RIDE C ( 77,X'S) H ( 771,X'S) RIDE C ( 78,X'S) H ( 781,X'S) RIDE C ( 80,X'S) H ( 801,X'S) RIDE C ( 84,X'S) H ( 842,X'S) H ( 841,X'S) RIDE C ( 89,X'S) H ( 891,X'S) RIDE C ( 90,X'S) H ( 901,X'S) H ( 902,X'S) RIDE C ( 92,X'S) H ( 921,X'S) RIDE C ( 94,X'S) H ( 941,X'S) RIDE C ( 95,X'S) H ( 951,X'S) RIDE C ( 96,X'S) H ( 961,X'S) RIDE C ( 98,X'S) H ( 981,X'S) RIDE C ( 99,X'S) H ( 991,X'S) RIDE C ( 102,X'S) H (1023,X'S) H (1021,X'S) H (1022,X'S) RIDE C ( 103,X'S) H (1031,X'S) H (1032,X'S) H (1033,X'S) RIDE C ( 106,X'S) H (1063,X'S) H (1061,X'S) H (1062,X'S) RIDE C ( 107,X'S) H (1071,X'S) H (1073,X'S) H (1072,X'S) RIDE C ( 110,X'S) H (1102,X'S) H (1101,X'S) H (1103,X'S) RIDE C ( 111,X'S) H (1113,X'S) H (1111,X'S) H (1112,X'S) RIDE C ( 114,X'S) H (1141,X'S) H (1143,X'S) H (1142,X'S) RIDE C ( 115,X'S) H (1152,X'S) H (1151,X'S) H (1153,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 24/10/11 at 09:54:12 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) 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 -2 5 3 x . -1 6 1 x . 2 5 0 x . 3 0 6 x . 0 3 1 x . -1 3 1 x . -1 2 1 x . 1 6 1 x . 1 3 1 x . 1 4 0 x . 1 5 0 x . -2 5 1 x . -1 11 3 x . -2 1 7 x . 2 5 1 x . -3 2 6 x .