data_5276 #Corrected using PDB structure: 1KMAA # #N.B. (Observed* = Observed shift + Offset correction) # #After reference correction, the following residues still #have a HA chemical shift difference (obs*-pred) greater than 0.7ppm: #NUM AA CS Observed* Predicted # 1 F HA 4.09 4.86 # #After reference correction, the following residues still #have a CA chemical shift difference (obs*-pred) greater than 5.0ppm: #NUM AA CS Observed* Predicted # 48 C CA 54.67 59.68 # #After reference correction, the following residues still #have a CB chemical shift difference (obs*-pred) greater than 5.0ppm: #NUM AA CS Observed* Predicted # 16 C CB 38.35 47.34 # 27 C CB 35.55 41.23 # #After reference correction, the following residues still #have a N chemical shift difference (obs*-pred) greater than 10.0ppm: #NUM AA CS Observed* Predicted # 44 H N 109.21 122.77 # #After reference correction, the following residues still #have a HN chemical shift difference (obs*-pred) greater than 2.0ppm: #NUM AA CS Observed* Predicted # 3 G H 8.03 10.08 # #The average CS difference between predicted and observed: #HA CA CB CO N HN #0.06 1.67 1.35 1.56 -2.69 -0.01 # #bmr5276.str.corr chemical shifts have been re-referenced with the following #offsets (these values have been added to the original bmr5276.str file): #HA CA CB CO N HN #N/A +1.51 +1.51 +1.56 -2.69 N/A # #The 95% confidence intervals for the above recommended offsets are: # HA CA CB CO N HN #+/-0.04 +/-0.31 +/-0.25 +/-0.36 +/-0.72 +/-0.12 # #The Correlation Coefficients between predicted and observed #chemical shifts are: #HA CA CB CO N HN #0.830 0.961 0.983 0.660 0.587 0.232 # #The RMSD between predicted and observed* (reference #corrected) chemical shifts are: #HA CA CB CO N HN #0.130 1.101 0.812 1.197 2.324 0.408 # ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; NMR Structure of the Domain-I of the Kazal-type Thrombin Inhibitor Dipetalin ; loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Schlott B. . . 2 Wohnert J. . . 3 Icke C. . . 4 Hartmann M. . . 5 Ramachandran R. . . 6 Guhrs K.-H. . . 7 Glusa E. . . 8 Flemming J. . . 9 Gorlach M. . . 10 Grosse F. . . 11 Ohlenschlager O. . . stop_ _BMRB_accession_number 5276 _BMRB_flat_file_name bmr5276.str _Entry_type new _Submission_date 2002-02-06 _Accession_date 2002-02-06 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 coupling_constants 1 stop_ loop_ _Data_type _Data_type_count '1H chemical shifts' 269 '15N chemical shifts' 53 '13C chemical shifts' 183 'coupling constants' 50 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2004-07-12 update BMRB "Links to related BMRB entries inserted" 2002-09-11 original author "Original release" stop_ loop_ _Related_BMRB_accession_number _Relationship 6242 "two-domain Thrombin inhibitor Dipetalin" stop_ save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_title ; Interaction of Kazal-type Inhibitor Domains with Serine Proteinases: Biochemical and Structural Studies ; _Citation_status published _Citation_type journal _MEDLINE_UI_code 22047862 _PubMed_ID 12051857 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Schlott B. . . 2 Wohnert J. . . 3 Icke C. . . 4 Hartmann M. . . 5 Ramachandran R. . . 6 Guhrs K-H. . . 7 Glusa E. . . 8 Flemming J. . . 9 Gorlach M. . . 10 Grosse F. . . 11 Ohlenschlager O. . . stop_ _Journal_abbreviation "J. Mol. Biol." _Journal_volume 318 _Journal_issue 2 _Page_first 533 _Page_last 546 _Year 2002 loop_ _Keyword "disulphide-rich small alpha+beta fold" "Kazal-type" stop_ save_ ################################## # Molecular system description # ################################## save_system_DIPETALIN _Saveframe_category molecular_system _Mol_system_name DIPETALIN _Abbreviation_common DIPETALIN _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label DIPETALIN $DIPETALIN stop_ _System_physical_state native _System_oligomer_state monomer _System_paramagnetic no _System_thiol_state 'all disulfide bound' loop_ _Database_name _Database_accession_code _Database_entry_mol_name _Database_entry_details PDB 1KMA ? . stop_ save_ ######################## # Monomeric polymers # ######################## save_DIPETALIN _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common DIPETALIN _Name_variant . _Abbreviation_common DIPETALIN _Mol_thiol_state 'all disulfide bound' ############################## # Polymer residue sequence # ############################## _Residue_count 55 _Mol_residue_sequence ; FQGNPCECPRALHRVCGSDG NTYSNPCMLTCAKHEGNPDL VQVHEGPCDEHDHDF ; loop_ _Residue_seq_code _Residue_label 1 PHE 2 GLN 3 GLY 4 ASN 5 PRO 6 CYS 7 GLU 8 CYS 9 PRO 10 ARG 11 ALA 12 LEU 13 HIS 14 ARG 15 VAL 16 CYS 17 GLY 18 SER 19 ASP 20 GLY 21 ASN 22 THR 23 TYR 24 SER 25 ASN 26 PRO 27 CYS 28 MET 29 LEU 30 THR 31 CYS 32 ALA 33 LYS 34 HIS 35 GLU 36 GLY 37 ASN 38 PRO 39 ASP 40 LEU 41 VAL 42 GLN 43 VAL 44 HIS 45 GLU 46 GLY 47 PRO 48 CYS 49 ASP 50 GLU 51 HIS 52 ASP 53 HIS 54 ASP 55 PHE stop_ _Sequence_homology_query_date 2004-07-29 _Sequence_homology_query_revised_last_date 2004-07-24 loop_ _Database_name _Database_accession_code _Database_entry_mol_name _Sequence_query_to_submitted_percentage _Sequence_subject_length _Sequence_identity _Sequence_positive _Sequence_homology_expectation_value PDB 1KMA "A Chain A, Nmr Structure Of The Domain-I OfThe Kazal-Type Thrombin Inhibitor Dipetalin" 100.00 55 100 100 2e-30 EMBL CAA10384.1 "dipetalogastin [Dipetalogaster maximus]" 15.99 344 100 100 2e-30 SWISS-PROT O96790 "DPGN_DIPMA Serine protease inhibitordipetalogastin precursor (Dipetalin)" 15.67 351 100 100 2e-30 stop_ save_ ######################################## # Molecular bond linkage definitions # ######################################## save_crosslink_bond_definitions _Saveframe_category crosslink_bonds loop_ _Bond_order _Bond_type _Atom_one_mol_system_component_name _Atom_one_residue_seq_code _Atom_one_residue_label _Atom_one_atom_name _Atom_two_mol_system_component_name _Atom_two_residue_seq_code _Atom_two_residue_label _Atom_two_atom_name single disulfide DIPETALIN 6 CYS SG DIPETALIN 31 CYS SG single disulfide DIPETALIN 8 CYS SG DIPETALIN 27 CYS SG single disulfide DIPETALIN 16 CYS SG DIPETALIN 48 CYS SG stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $DIPETALIN "Dipetalogaster maximus" 72496 Eukaryota Metazoa Dipetalogaster maximus stop_ save_ ######################### # Experimental source # ######################### save_experimental_source _Saveframe_category experimental_source loop_ _Mol_label _Production_method _Host_organism_name_common _Genus _Species _Strain _Vector_name $DIPETALIN 'recombinant technology' "E. COLI" Escherichia coli TG1 pMEX6 stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $DIPETALIN 1 mM "[U-15N]" "phosphate buffer" 50 mM . NaCl 100 mM . EDTA 0.1 mM . D2O 6 % . H2O 94 % . stop_ save_ save_sample_2 _Saveframe_category sample _Sample_type solution loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $DIPETALIN 1.37 mM "[U-15N; U-13C]" "phosphate buffer" 50 mM . NaCl 100 mM . EDTA 0.1 mM . D2O 6 % . H2O 94 % . stop_ save_ ############################ # Computer software used # ############################ save_DYANA _Saveframe_category software _Name DYANA _Version 1.5 loop_ _Task "structure solution" stop_ _Details Guentert save_ save_OPAL _Saveframe_category software _Name OPAL _Version 2.6 loop_ _Task refinement stop_ _Details Luginbuehl save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_NMR_spectrometer _Saveframe_category NMR_spectrometer _Manufacturer Varian _Model INOVA _Field_strength 600 save_ ############################# # NMR applied experiments # ############################# save_NMR_applied_experiment _Saveframe_category NMR_applied_experiment _Experiment_name ; 3D 15N-separated NOESY 3D 13C-separated NOESY HNHA ; save_ ####################### # Sample conditions # ####################### save_sample_cond_1 _Saveframe_category sample_conditions loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 6.68 . n/a temperature 288 . K pressure 1 . atm stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chemical_shift_reference _Saveframe_category chemical_shift_reference loop_ _Mol_common_name _Atom_type _Atom_isotope_number _Atom_group _Chem_shift_units _Chem_shift_value _Reference_method _Reference_type _External_reference_sample_geometry _External_reference_location _External_reference_axis _Indirect_shift_ratio DSS H 1 "methyl protons" ppm 0.00 external direct . . . 1.0 NH4Cl N 15 nitrogen ppm 24.93 external direct . . . 1.0 DIOXANE C 13 "methylene carbons" ppm 67.80 external direct . . . 1.0 stop_ save_ ################################### # Assigned chemical shift lists # ################################### ################################################################### # Chemical Shift Ambiguity Index Value Definitions # # # # Index Value Definition # # # # 1 Unique # # 2 Ambiguity of geminal atoms or geminal methyl # # proton groups # # 3 Aromatic atoms on opposite sides of the ring # # (e.g. Tyr HE1 and HE2 protons) # # 4 Intraresidue ambiguities (e.g. Lys HG and # # HD protons) # # 5 Interresidue ambiguities (Lys 12 vs. Lys 27) # # 9 Ambiguous, specific ambiguity not defined # # # ################################################################### save_chemical_shift_set_1 _Saveframe_category assigned_chemical_shifts loop_ _Sample_label $sample_1 $sample_2 stop_ _Sample_conditions_label $sample_cond_1 _Chem_shift_reference_set_label $chemical_shift_reference _Mol_system_component_name DIPETALIN loop_ _Atom_shift_assign_ID _Residue_seq_code _Residue_label _Atom_name _Atom_type _Chem_shift_value _Chem_shift_value_error _Chem_shift_ambiguity_code 1 1 PHE CA C 57.31 0.2 1 2 1 PHE HA H 4.03 0.02 1 3 1 PHE CB C 35.81 0.2 1 4 1 PHE HB2 H 1.96 0.02 1 5 1 PHE HB3 H 1.96 0.02 1 6 1 PHE C C 176.76 0.2 1 7 2 GLN N N 117.51 0.2 1 8 2 GLN H H 8.37 0.02 1 9 2 GLN CA C 55.81 0.2 1 10 2 GLN HA H 4.18 0.02 1 11 2 GLN CB C 29.41 0.2 1 12 2 GLN HB2 H 1.92 0.02 2 13 2 GLN HB3 H 1.79 0.02 2 14 2 GLN CG C 33.61 0.2 1 15 2 GLN HG2 H 2.16 0.02 1 16 2 GLN HG3 H 2.16 0.02 1 17 2 GLN NE2 N 114.20 0.2 1 18 2 GLN HE21 H 7.48 0.02 2 19 2 GLN HE22 H 6.79 0.02 2 20 2 GLN C C 175.46 0.2 1 21 3 GLY N N 109.11 0.2 1 22 3 GLY H H 8.04 0.02 1 23 3 GLY CA C 44.91 0.2 1 24 3 GLY HA2 H 3.76 0.02 1 25 3 GLY HA3 H 3.76 0.02 1 26 3 GLY C C 173.46 0.2 1 27 4 ASN N N 118.31 0.2 1 28 4 ASN H H 8.29 0.02 1 29 4 ASN CA C 51.11 0.2 1 30 4 ASN HA H 4.88 0.02 1 31 4 ASN CB C 38.71 0.2 1 32 4 ASN HB2 H 2.71 0.02 2 33 4 ASN HB3 H 2.57 0.02 2 34 4 ASN ND2 N 114.40 0.2 1 35 4 ASN HD21 H 7.56 0.02 2 36 4 ASN HD22 H 6.98 0.02 2 37 5 PRO CD C 50.91 0.2 1 38 5 PRO CA C 63.71 0.2 1 39 5 PRO HA H 4.27 0.02 1 40 5 PRO CB C 32.21 0.2 1 41 5 PRO HB2 H 2.08 0.02 2 42 5 PRO HB3 H 1.74 0.02 2 43 5 PRO CG C 27.11 0.2 1 44 5 PRO HG2 H 1.73 0.02 1 45 5 PRO HG3 H 1.73 0.02 1 46 5 PRO HD2 H 3.65 0.02 2 47 5 PRO HD3 H 3.51 0.02 2 48 9 PRO CD C 50.91 0.2 1 49 9 PRO CA C 62.31 0.2 1 50 9 PRO HA H 4.47 0.02 1 51 9 PRO CB C 32.41 0.2 1 52 9 PRO HB2 H 2.37 0.02 2 53 9 PRO HB3 H 1.82 0.02 2 54 9 PRO CG C 27.51 0.2 1 55 9 PRO HG2 H 1.98 0.02 1 56 9 PRO HG3 H 1.98 0.02 1 57 9 PRO HD2 H 3.90 0.02 2 58 9 PRO HD3 H 3.44 0.02 2 59 9 PRO C C 176.46 0.2 1 60 10 ARG N N 118.51 0.2 1 61 10 ARG H H 8.48 0.02 1 62 10 ARG CA C 56.21 0.2 1 63 10 ARG HA H 4.04 0.02 1 64 10 ARG CB C 30.01 0.2 1 65 10 ARG HB2 H 1.79 0.02 2 66 10 ARG HB3 H 1.61 0.02 2 67 10 ARG CG C 27.31 0.2 1 68 10 ARG HG2 H 1.56 0.02 1 69 10 ARG HG3 H 1.56 0.02 1 70 10 ARG CD C 43.11 0.2 1 71 10 ARG HD2 H 3.10 0.02 1 72 10 ARG HD3 H 3.10 0.02 1 73 10 ARG C C 177.16 0.2 1 74 11 ALA N N 120.81 0.2 1 75 11 ALA H H 7.24 0.02 1 76 11 ALA CA C 52.71 0.2 1 77 11 ALA HA H 4.04 0.02 1 78 11 ALA HB H 1.25 0.02 1 79 11 ALA CB C 19.21 0.2 1 80 11 ALA C C 177.16 0.2 1 81 12 LEU N N 123.01 0.2 1 82 12 LEU H H 8.52 0.02 1 83 12 LEU CA C 55.31 0.2 1 84 12 LEU HA H 4.34 0.02 1 85 12 LEU CB C 43.01 0.2 1 86 12 LEU HB2 H 1.64 0.02 2 87 12 LEU HB3 H 1.48 0.02 2 88 12 LEU CG C 27.31 0.2 1 89 12 LEU HG H 1.64 0.02 1 90 12 LEU HD1 H 0.90 0.02 2 91 12 LEU HD2 H 0.84 0.02 2 92 12 LEU CD1 C 24.81 0.2 1 93 12 LEU CD2 C 24.31 0.2 1 94 12 LEU C C 177.36 0.2 1 95 13 HIS N N 125.51 0.2 1 96 13 HIS H H 9.37 0.02 1 97 13 HIS CA C 55.31 0.2 1 98 13 HIS HA H 4.53 0.02 1 99 13 HIS CB C 29.91 0.2 1 100 13 HIS HB2 H 3.02 0.02 2 101 13 HIS HB3 H 2.89 0.02 2 102 13 HIS C C 172.46 0.2 1 103 14 ARG N N 120.21 0.2 1 104 14 ARG H H 8.31 0.02 1 105 14 ARG CA C 58.21 0.2 1 106 14 ARG HA H 4.34 0.02 1 107 14 ARG CB C 31.01 0.2 1 108 14 ARG HB2 H 1.56 0.02 2 109 14 ARG HB3 H 1.14 0.02 2 110 14 ARG CG C 28.61 0.2 1 111 14 ARG HG2 H 1.78 0.02 2 112 14 ARG HG3 H 1.56 0.02 2 113 14 ARG CD C 43.91 0.2 1 114 14 ARG HD2 H 3.01 0.02 1 115 14 ARG HD3 H 3.01 0.02 1 116 14 ARG NE N 112.30 0.2 1 117 14 ARG HE H 8.34 0.02 1 118 14 ARG C C 177.96 0.2 1 119 15 VAL N N 110.71 0.2 1 120 15 VAL H H 8.29 0.02 1 121 15 VAL CA C 59.71 0.2 1 122 15 VAL HA H 4.61 0.02 1 123 15 VAL CB C 36.81 0.2 1 124 15 VAL HB H 1.81 0.02 1 125 15 VAL HG1 H 0.90 0.02 2 126 15 VAL HG2 H 0.52 0.02 2 127 15 VAL CG1 C 22.01 0.2 1 128 15 VAL CG2 C 18.11 0.2 1 129 15 VAL C C 173.06 0.2 1 130 16 CYS N N 118.41 0.2 1 131 16 CYS H H 8.16 0.02 1 132 16 CYS CA C 54.01 0.2 1 133 16 CYS HA H 5.02 0.02 1 134 16 CYS CB C 38.51 0.2 1 135 16 CYS HB2 H 2.37 0.02 2 136 16 CYS HB3 H 0.97 0.02 2 137 16 CYS C C 175.36 0.2 1 138 17 GLY N N 114.41 0.2 1 139 17 GLY H H 9.32 0.02 1 140 17 GLY CA C 44.71 0.2 1 141 17 GLY HA2 H 4.86 0.02 2 142 17 GLY HA3 H 3.96 0.02 2 143 17 GLY C C 175.76 0.2 1 144 18 SER N N 116.71 0.2 1 145 18 SER H H 9.23 0.02 1 146 18 SER CA C 60.61 0.2 1 147 18 SER HA H 3.96 0.02 1 148 18 SER CB C 62.01 0.2 1 149 18 SER HB2 H 4.09 0.02 2 150 18 SER HB3 H 3.67 0.02 2 151 18 SER C C 173.76 0.2 1 152 19 ASP N N 119.01 0.2 1 153 19 ASP H H 8.10 0.02 1 154 19 ASP CA C 53.11 0.2 1 155 19 ASP HA H 4.39 0.02 1 156 19 ASP CB C 40.31 0.2 1 157 19 ASP HB2 H 2.88 0.02 2 158 19 ASP HB3 H 2.47 0.02 2 159 19 ASP C C 176.66 0.2 1 160 20 GLY N N 107.41 0.2 1 161 20 GLY H H 8.19 0.02 1 162 20 GLY CA C 45.51 0.2 1 163 20 GLY HA2 H 4.01 0.02 2 164 20 GLY HA3 H 3.60 0.02 2 165 20 GLY C C 173.76 0.2 1 166 21 ASN N N 117.61 0.2 1 167 21 ASN H H 8.02 0.02 1 168 21 ASN CA C 51.81 0.2 1 169 21 ASN HA H 4.75 0.02 1 170 21 ASN CB C 39.71 0.2 1 171 21 ASN HB2 H 2.75 0.02 2 172 21 ASN HB3 H 1.96 0.02 2 173 21 ASN ND2 N 116.40 0.2 1 174 21 ASN HD21 H 6.82 0.02 2 175 21 ASN HD22 H 6.87 0.02 2 176 21 ASN C C 173.46 0.2 1 177 22 THR N N 119.61 0.2 1 178 22 THR H H 8.45 0.02 1 179 22 THR CA C 62.41 0.2 1 180 22 THR HA H 4.79 0.02 1 181 22 THR CB C 69.21 0.2 1 182 22 THR HB H 3.85 0.02 1 183 22 THR HG2 H 1.03 0.02 1 184 22 THR CG2 C 22.51 0.2 1 185 22 THR C C 174.66 0.2 1 186 23 TYR N N 126.31 0.2 1 187 23 TYR H H 9.22 0.02 1 188 23 TYR CA C 57.51 0.2 1 189 23 TYR HA H 4.45 0.02 1 190 23 TYR CB C 42.11 0.2 1 191 23 TYR HB2 H 2.72 0.02 2 192 23 TYR HB3 H 2.36 0.02 2 193 23 TYR HE1 H 6.22 0.02 1 194 23 TYR HE2 H 6.22 0.02 1 195 23 TYR C C 176.76 0.2 1 196 24 SER N N 116.11 0.2 1 197 24 SER H H 9.15 0.02 1 198 24 SER CA C 61.91 0.2 1 199 24 SER HA H 3.87 0.02 1 200 24 SER CB C 63.21 0.2 1 201 24 SER HB2 H 3.81 0.02 1 202 24 SER HB3 H 3.81 0.02 1 203 24 SER C C 172.86 0.2 1 204 25 ASN N N 108.21 0.2 1 205 25 ASN H H 7.31 0.02 1 206 25 ASN CA C 51.81 0.2 1 207 25 ASN HA H 5.39 0.02 1 208 25 ASN CB C 37.21 0.2 1 209 25 ASN HB2 H 3.29 0.02 2 210 25 ASN HB3 H 3.06 0.02 2 211 25 ASN ND2 N 114.90 0.2 1 212 25 ASN HD21 H 7.29 0.02 2 213 25 ASN HD22 H 6.34 0.02 2 214 26 PRO CD C 50.41 0.2 1 215 26 PRO CA C 65.91 0.2 1 216 26 PRO HA H 4.04 0.02 1 217 26 PRO CB C 32.21 0.2 1 218 26 PRO HB2 H 2.48 0.02 2 219 26 PRO HB3 H 1.87 0.02 2 220 26 PRO CG C 28.01 0.2 1 221 26 PRO HG2 H 2.05 0.02 2 222 26 PRO HG3 H 1.87 0.02 2 223 26 PRO HD2 H 4.10 0.02 2 224 26 PRO HD3 H 3.90 0.02 2 225 26 PRO C C 177.76 0.2 1 226 27 CYS N N 116.81 0.2 1 227 27 CYS H H 7.92 0.02 1 228 27 CYS CA C 60.01 0.2 1 229 27 CYS HA H 4.14 0.02 1 230 27 CYS CB C 35.71 0.2 1 231 27 CYS HB2 H 3.22 0.02 2 232 27 CYS HB3 H 2.98 0.02 2 233 27 CYS C C 177.16 0.2 1 234 28 MET N N 119.71 0.2 1 235 28 MET H H 8.27 0.02 1 236 28 MET CA C 57.41 0.2 1 237 28 MET HA H 4.22 0.02 1 238 28 MET CB C 32.61 0.2 1 239 28 MET HB2 H 2.76 0.02 2 240 28 MET HB3 H 2.69 0.02 2 241 28 MET CG C 31.91 0.2 1 242 28 MET HG2 H 2.19 0.02 1 243 28 MET HG3 H 2.19 0.02 1 244 28 MET HE H 2.06 0.02 1 245 28 MET CE C 17.21 0.2 1 246 28 MET C C 179.36 0.2 1 247 29 LEU N N 122.91 0.2 1 248 29 LEU H H 7.17 0.02 1 249 29 LEU CA C 59.61 0.2 1 250 29 LEU HA H 2.88 0.02 1 251 29 LEU CB C 40.81 0.2 1 252 29 LEU HB2 H 1.61 0.02 2 253 29 LEU HB3 H 0.85 0.02 2 254 29 LEU CG C 27.61 0.2 1 255 29 LEU HG H 0.80 0.02 1 256 29 LEU HD1 H 0.50 0.02 2 257 29 LEU HD2 H 0.44 0.02 2 258 29 LEU CD1 C 27.01 0.2 1 259 29 LEU CD2 C 23.71 0.2 1 260 29 LEU C C 177.86 0.2 1 261 30 THR N N 116.41 0.2 1 262 30 THR H H 8.14 0.02 1 263 30 THR CA C 66.81 0.2 1 264 30 THR HA H 3.48 0.02 1 265 30 THR CB C 67.91 0.2 1 266 30 THR HB H 4.22 0.02 1 267 30 THR HG2 H 1.08 0.02 1 268 30 THR CG2 C 22.91 0.2 1 269 30 THR C C 176.26 0.2 1 270 31 CYS N N 119.51 0.2 1 271 31 CYS H H 8.51 0.02 1 272 31 CYS CA C 58.41 0.2 1 273 31 CYS HA H 4.14 0.02 1 274 31 CYS CB C 39.81 0.2 1 275 31 CYS HB2 H 3.27 0.02 2 276 31 CYS HB3 H 3.13 0.02 2 277 31 CYS C C 176.16 0.2 1 278 32 ALA N N 120.91 0.2 1 279 32 ALA H H 7.44 0.02 1 280 32 ALA CA C 55.01 0.2 1 281 32 ALA HA H 4.05 0.02 1 282 32 ALA HB H 1.40 0.02 1 283 32 ALA CB C 18.31 0.2 1 284 32 ALA C C 180.46 0.2 1 285 33 LYS N N 120.91 0.2 1 286 33 LYS H H 8.06 0.02 1 287 33 LYS CA C 57.51 0.2 1 288 33 LYS HA H 4.24 0.02 1 289 33 LYS CB C 33.31 0.2 1 290 33 LYS HB2 H 1.91 0.02 2 291 33 LYS HB3 H 1.53 0.02 2 292 33 LYS CG C 30.21 0.2 1 293 33 LYS HG2 H 1.53 0.02 2 294 33 LYS HG3 H 1.41 0.02 2 295 33 LYS CD C 23.91 0.2 1 296 33 LYS HD2 H 1.61 0.02 2 297 33 LYS HD3 H 0.96 0.02 2 298 33 LYS CE C 42.11 0.2 1 299 33 LYS HE2 H 2.93 0.02 2 300 33 LYS HE3 H 2.84 0.02 2 301 33 LYS C C 179.06 0.2 1 302 34 HIS N N 116.11 0.2 1 303 34 HIS H H 7.76 0.02 1 304 34 HIS CA C 57.81 0.2 1 305 34 HIS HA H 4.33 0.02 1 306 34 HIS CB C 29.91 0.2 1 307 34 HIS HB2 H 3.24 0.02 2 308 34 HIS HB3 H 3.08 0.02 2 309 34 HIS C C 176.46 0.2 1 310 35 GLU N N 118.81 0.2 1 311 35 GLU H H 8.02 0.02 1 312 35 GLU CA C 56.21 0.2 1 313 35 GLU HA H 4.26 0.02 1 314 35 GLU CB C 29.11 0.2 1 315 35 GLU HB2 H 2.08 0.02 2 316 35 GLU HB3 H 1.91 0.02 2 317 35 GLU CG C 36.51 0.2 1 318 35 GLU HG2 H 2.34 0.02 2 319 35 GLU HG3 H 2.15 0.02 2 320 35 GLU C C 177.16 0.2 1 321 36 GLY N N 103.41 0.2 1 322 36 GLY H H 7.54 0.02 1 323 36 GLY CA C 46.11 0.2 1 324 36 GLY HA2 H 4.08 0.02 2 325 36 GLY HA3 H 3.91 0.02 2 326 36 GLY C C 173.66 0.2 1 327 37 ASN N N 115.41 0.2 1 328 37 ASN H H 7.57 0.02 1 329 37 ASN CA C 50.81 0.2 1 330 37 ASN HA H 5.19 0.02 1 331 37 ASN CB C 39.11 0.2 1 332 37 ASN HB2 H 2.68 0.02 2 333 37 ASN HB3 H 2.58 0.02 2 334 37 ASN ND2 N 114.50 0.2 1 335 37 ASN HD21 H 7.68 0.02 2 336 37 ASN HD22 H 6.87 0.02 2 337 38 PRO CD C 50.41 0.2 1 338 38 PRO CA C 64.61 0.2 1 339 38 PRO HA H 4.16 0.02 1 340 38 PRO CB C 32.01 0.2 1 341 38 PRO HB2 H 2.23 0.02 2 342 38 PRO HB3 H 1.84 0.02 2 343 38 PRO CG C 27.01 0.2 1 344 38 PRO HG2 H 1.90 0.02 2 345 38 PRO HG3 H 1.82 0.02 2 346 38 PRO HD2 H 3.69 0.02 2 347 38 PRO HD3 H 3.39 0.02 2 348 38 PRO C C 177.66 0.2 1 349 39 ASP N N 116.01 0.2 1 350 39 ASP H H 7.98 0.02 1 351 39 ASP CA C 54.01 0.2 1 352 39 ASP HA H 4.49 0.02 1 353 39 ASP CB C 40.81 0.2 1 354 39 ASP HB2 H 2.67 0.02 2 355 39 ASP HB3 H 2.42 0.02 2 356 39 ASP C C 175.56 0.2 1 357 40 LEU N N 122.21 0.2 1 358 40 LEU H H 7.34 0.02 1 359 40 LEU CA C 56.41 0.2 1 360 40 LEU HA H 3.74 0.02 1 361 40 LEU CB C 42.91 0.2 1 362 40 LEU HB2 H 1.62 0.02 2 363 40 LEU HB3 H 1.26 0.02 2 364 40 LEU CG C 23.01 0.2 1 365 40 LEU HG H 0.91 0.02 1 366 40 LEU HD1 H 1.04 0.02 2 367 40 LEU HD2 H 0.65 0.02 2 368 40 LEU CD1 C 26.81 0.2 1 369 40 LEU CD2 C 27.11 0.2 1 370 40 LEU C C 175.56 0.2 1 371 41 VAL N N 119.21 0.2 1 372 41 VAL H H 8.42 0.02 1 373 41 VAL CA C 58.91 0.2 1 374 41 VAL HA H 4.45 0.02 1 375 41 VAL CB C 36.51 0.2 1 376 41 VAL HB H 1.97 0.02 1 377 41 VAL HG1 H 0.75 0.02 2 378 41 VAL HG2 H 0.70 0.02 2 379 41 VAL CG1 C 21.41 0.2 1 380 41 VAL CG2 C 18.61 0.2 1 381 41 VAL C C 174.66 0.2 1 382 42 GLN N N 122.01 0.2 1 383 42 GLN H H 8.74 0.02 1 384 42 GLN CA C 56.21 0.2 1 385 42 GLN HA H 4.08 0.02 1 386 42 GLN CB C 29.71 0.2 1 387 42 GLN HB2 H 1.76 0.02 2 388 42 GLN HB3 H 1.61 0.02 2 389 42 GLN CG C 43.21 0.2 1 390 42 GLN HG2 H 3.10 0.02 1 391 42 GLN HG3 H 3.10 0.02 1 392 42 GLN NE2 N 112.90 0.2 1 393 42 GLN HE21 H 7.21 0.02 2 394 42 GLN HE22 H 6.78 0.02 2 395 42 GLN C C 176.16 0.2 1 396 43 VAL N N 124.11 0.2 1 397 43 VAL H H 9.07 0.02 1 398 43 VAL CA C 63.61 0.2 1 399 43 VAL HA H 4.14 0.02 1 400 43 VAL CB C 32.71 0.2 1 401 43 VAL HB H 1.76 0.02 1 402 43 VAL HG1 H 0.90 0.02 2 403 43 VAL HG2 H 0.69 0.02 2 404 43 VAL CG1 C 21.91 0.2 1 405 43 VAL CG2 C 20.41 0.2 1 406 43 VAL C C 176.36 0.2 1 407 44 HIS N N 109.21 0.2 1 408 44 HIS H H 7.05 0.02 1 409 44 HIS CA C 55.31 0.2 1 410 44 HIS HA H 4.87 0.02 1 411 44 HIS CB C 29.71 0.2 1 412 44 HIS HB2 H 3.61 0.02 2 413 44 HIS HB3 H 3.21 0.02 2 414 44 HIS C C 173.56 0.2 1 415 45 GLU N N 118.81 0.2 1 416 45 GLU H H 9.19 0.02 1 417 45 GLU CA C 57.31 0.2 1 418 45 GLU HA H 4.36 0.02 1 419 45 GLU CB C 31.21 0.2 1 420 45 GLU HB2 H 2.18 0.02 2 421 45 GLU HB3 H 2.04 0.02 2 422 45 GLU CG C 37.11 0.2 1 423 45 GLU HG2 H 2.35 0.02 2 424 45 GLU HG3 H 2.16 0.02 2 425 45 GLU C C 178.56 0.2 1 426 46 GLY N N 113.71 0.2 1 427 46 GLY H H 8.43 0.02 1 428 46 GLY CA C 44.91 0.2 1 429 46 GLY HA2 H 4.40 0.02 2 430 46 GLY HA3 H 3.57 0.02 2 431 47 PRO CD C 49.11 0.2 1 432 47 PRO CA C 61.51 0.2 1 433 47 PRO HA H 4.24 0.02 1 434 47 PRO CB C 32.41 0.2 1 435 47 PRO HB2 H 1.94 0.02 1 436 47 PRO HB3 H 1.94 0.02 1 437 47 PRO CG C 27.41 0.2 1 438 47 PRO HG2 H 1.88 0.02 2 439 47 PRO HG3 H 1.77 0.02 2 440 47 PRO HD2 H 3.52 0.02 2 441 47 PRO HD3 H 3.26 0.02 2 442 47 PRO C C 174.36 0.2 1 443 48 CYS N N 117.31 0.2 1 444 48 CYS H H 8.19 0.02 1 445 48 CYS CA C 54.51 0.2 1 446 48 CYS HA H 4.51 0.02 1 447 48 CYS CB C 37.51 0.2 1 448 48 CYS HB2 H 3.10 0.02 2 449 48 CYS HB3 H 2.45 0.02 2 450 48 CYS C C 174.96 0.2 1 451 49 ASP N N 120.81 0.2 1 452 49 ASP H H 8.77 0.02 1 453 49 ASP CA C 53.91 0.2 1 454 49 ASP HA H 4.53 0.02 1 455 49 ASP CB C 41.71 0.2 1 456 49 ASP HB2 H 2.57 0.02 1 457 49 ASP HB3 H 2.57 0.02 1 458 49 ASP C C 176.26 0.2 1 459 50 GLU N N 119.91 0.2 1 460 50 GLU H H 8.51 0.02 1 461 50 GLU CA C 57.21 0.2 1 462 50 GLU HA H 4.02 0.02 1 463 50 GLU CB C 29.71 0.2 1 464 50 GLU HB2 H 1.75 0.02 2 465 50 GLU HB3 H 1.59 0.02 2 466 50 GLU CG C 43.11 0.2 1 467 50 GLU HG2 H 3.08 0.02 2 468 50 GLU HG3 H 3.00 0.02 2 469 50 GLU C C 176.76 0.2 1 470 51 HIS N N 120.11 0.2 1 471 51 HIS H H 8.07 0.02 1 472 51 HIS CA C 55.91 0.2 1 473 51 HIS HA H 4.50 0.02 1 474 51 HIS CB C 29.31 0.2 1 475 51 HIS HB2 H 3.11 0.02 2 476 51 HIS HB3 H 2.97 0.02 2 477 52 ASP N N 119.41 0.2 1 478 52 ASP H H 8.06 0.02 1 479 52 ASP CA C 54.81 0.2 1 480 52 ASP HA H 4.45 0.02 1 481 52 ASP CB C 41.01 0.2 1 482 52 ASP HB2 H 2.53 0.02 1 483 52 ASP HB3 H 2.53 0.02 1 484 53 HIS N N 117.31 0.2 1 485 53 HIS H H 8.11 0.02 1 486 53 HIS CA C 55.21 0.2 1 487 53 HIS HA H 4.52 0.02 1 488 53 HIS CB C 29.91 0.2 1 489 53 HIS HB2 H 3.04 0.02 2 490 53 HIS HB3 H 2.89 0.02 2 491 54 ASP N N 120.51 0.2 1 492 54 ASP H H 8.22 0.02 1 493 54 ASP CA C 54.41 0.2 1 494 54 ASP HA H 4.48 0.02 1 495 54 ASP CB C 40.81 0.2 1 496 54 ASP HB2 H 2.54 0.02 2 497 54 ASP HB3 H 2.40 0.02 2 498 54 ASP C C 174.96 0.2 1 499 55 PHE N N 123.61 0.2 1 500 55 PHE H H 7.63 0.02 1 501 55 PHE CA C 59.11 0.2 1 502 55 PHE HA H 4.30 0.02 1 503 55 PHE CB C 40.11 0.2 1 504 55 PHE HB2 H 3.01 0.02 2 505 55 PHE HB3 H 2.88 0.02 2 stop_ save_ ######################## # Coupling constants # ######################## save_coupling_constant_set_1 _Saveframe_category coupling_constants loop_ _Sample_label $sample_1 $sample_2 stop_ _Sample_conditions_label $sample_cond_1 _Spectrometer_frequency_1H 600 _Mol_system_component_name DIPETALIN loop_ _Coupling_constant_code _Atom_one_residue_seq_code _Atom_one_residue_label _Atom_one_name _Atom_two_residue_seq_code _Atom_two_residue_label _Atom_two_name _Coupling_constant_value _Coupling_constant_value_error 3JHNHA 2 GLN H 2 GLN HA 6.9 1.5 3JHNHA 3 GLY H 3 GLY HA2 8.1 1.5 3JHNHA 3 GLY H 3 GLY HA3 8.1 1.5 3JHNHA 4 ASN H 4 ASN HA 7.2 1.5 3JHNHA 10 ARG H 10 ARG HA 6.3 1.5 3JHNHA 11 ALA H 11 ALA HA 3.2 1.5 3JHNHA 12 LEU H 12 LEU HA 5.8 1.5 3JHNHA 13 HIS H 13 HIS HA 6.0 1.5 3JHNHA 14 ARG H 14 ARG HA 2.7 1.5 3JHNHA 15 VAL H 15 VAL HA 6.8 1.5 3JHNHA 16 CYS H 16 CYS HA 7.8 1.5 3JHNHA 17 GLY H 17 GLY HA2 5.6 1.5 3JHNHA 17 GLY H 17 GLY HA3 4.0 1.5 3JHNHA 18 SER H 18 SER HA 3.0 1.5 3JHNHA 19 ASP H 19 ASP HA 7.5 1.5 3JHNHA 20 GLY H 20 GLY HA2 6.2 1.5 3JHNHA 20 GLY H 20 GLY HA3 4.2 1.5 3JHNHA 21 ASN H 21 ASN HA 7.7 1.5 3JHNHA 22 THR H 22 THR HA 5.9 1.5 3JHNHA 23 TYR H 23 TYR HA 8.8 1.5 3JHNHA 24 SER H 24 SER HA 2.2 1.5 3JHNHA 25 ASN H 25 ASN HA 3.4 1.5 3JHNHA 27 CYS H 27 CYS HA 3.3 1.5 3JHNHA 28 MET H 28 MET HA 4.2 1.5 3JHNHA 29 LEU H 29 LEU HA 4.1 1.5 3JHNHA 30 THR H 30 THR HA 2.5 1.5 3JHNHA 31 CYS H 31 CYS HA 3.9 1.5 3JHNHA 32 ALA H 32 ALA HA 4.3 1.5 3JHNHA 33 LYS H 33 LYS HA 3.1 1.5 3JHNHA 34 HIS H 34 HIS HA 4.8 1.5 3JHNHA 35 GLU H 35 GLU HA 6.6 1.5 3JHNHA 36 GLY H 36 GLY HA2 4.7 1.5 3JHNHA 36 GLY H 36 GLY HA3 4.9 1.5 3JHNHA 37 ASN H 37 ASN HA 8.0 1.5 3JHNHA 39 ASP H 39 ASP HA 7.5 1.5 3JHNHA 40 LEU H 40 LEU HA 3.3 1.5 3JHNHA 41 VAL H 41 VAL HA 5.6 1.5 3JHNHA 42 GLN H 42 GLN HA 5.6 1.5 3JHNHA 43 VAL H 43 VAL HA 6.1 1.5 3JHNHA 44 HIS H 44 HIS HA 4.3 1.5 3JHNHA 45 GLU H 45 GLU HA 5.6 1.5 3JHNHA 46 GLY H 46 GLY HA2 6.3 1.5 3JHNHA 46 GLY H 46 GLY HA3 3.4 1.5 3JHNHA 48 CYS H 48 CYS HA 4.7 1.5 3JHNHA 49 ASP H 49 ASP HA 6.5 1.5 3JHNHA 50 GLU H 50 GLU HA 4.8 1.5 3JHNHA 52 ASP H 52 ASP HA 6.2 1.5 3JHNHA 53 HIS H 53 HIS HA 7.3 1.5 3JHNHA 54 ASP H 54 ASP HA 6.4 1.5 3JHNHA 55 PHE H 55 PHE HA 5.8 1.5 stop_ save_