data_19112 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Structural characterization by NMR of a double phosphorylated chimeric peptide vaccine for treatment of Alzheimer's disease ; _BMRB_accession_number 19112 _BMRB_flat_file_name bmr19112.str _Entry_type original _Submission_date 2013-03-27 _Accession_date 2013-03-27 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details . loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Matzapetakis Manolis . . 2 Ramirez-Gualito Karla . . 3 Richter Monique . . 4 Berger Stefan . . 5 Singer David . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 101 "13C chemical shifts" 66 "15N chemical shifts" 20 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2013-05-03 original author . stop_ _Original_release_date 2013-05-03 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title 'Structural characterization by NMR of a double phosphorylated chimeric Peptide vaccine for treatment of Alzheimer's disease' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 23624647 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Ramirez-Gualito Karla . . 2 Richter Monique . . 3 Matzapetakis Manolis . . 4 Singer David . . 5 Berger Stefan . . stop_ _Journal_abbreviation Molecules _Journal_volume 18 _Journal_issue 5 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 4929 _Page_last 4941 _Year 2013 _Details . loop_ _Keyword 'NMR spectroscopy' 'Alzheimer's disease' 'peptide vaccine' 'B cell epitope' 'Tau protein' stop_ save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name MS1 _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label TAU231 $TAU231 stop_ _System_molecular_weight 2827.0347 _System_physical_state unfolded _System_oligomer_state ? _System_paramagnetic no _System_thiol_state 'not present' _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_TAU231 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common TAU231 _Molecular_mass 2984.9 _Mol_thiol_state 'not present' loop_ _Biological_function 'Peptide vaccine' stop_ _Details 'T22 and S26 are phosphorylated.' ############################## # Polymer residue sequence # ############################## _Residue_count 28 _Mol_residue_sequence ; QDAYNAGGGHNGVFDGPSLV RXPPKXPS ; loop_ _Residue_seq_code _Residue_label 1 GLN 2 ASP 3 ALA 4 TYR 5 ASN 6 ALA 7 GLY 8 GLY 9 GLY 10 HIS 11 ASN 12 GLY 13 VAL 14 PHE 15 ASP 16 GLY 17 PRO 18 SER 19 LEU 20 VAL 21 ARG 22 TPO 23 PRO 24 PRO 25 LYS 26 SEP 27 PRO 28 SER stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ###################### # Polymer residues # ###################### save_chem_comp_TPO _Saveframe_category polymer_residue _Mol_type 'L-PEPTIDE LINKING' _Name_common PHOSPHOTHREONINE _BMRB_code TPO _PDB_code TPO _Standard_residue_derivative . _Molecular_mass 199.099 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons C C C . 0 . ? CA CA C . 0 . ? CB CB C . 0 . ? CG2 CG2 C . 0 . ? H H H . 0 . ? H2 H2 H . 0 . ? HA HA H . 0 . ? HB HB H . 0 . ? HG21 HG21 H . 0 . ? HG22 HG22 H . 0 . ? HG23 HG23 H . 0 . ? HOP2 HOP2 H . 0 . ? HOP3 HOP3 H . 0 . ? HXT HXT H . 0 . ? N N N . 0 . ? O O O . 0 . ? O1P O1P O . 0 . ? O2P O2P O . 0 . ? O3P O3P O . 0 . ? OG1 OG1 O . 0 . ? OXT OXT O . 0 . ? P P P . 0 . ? stop_ loop_ _Bond_order _Bond_atom_one_atom_name _Bond_atom_two_atom_name _PDB_bond_atom_one_atom_name _PDB_bond_atom_two_atom_name SING N CA ? ? SING N H ? ? SING N H2 ? ? SING CA CB ? ? SING CA C ? ? SING CA HA ? ? SING CB CG2 ? ? SING CB OG1 ? ? SING CB HB ? ? SING CG2 HG21 ? ? SING CG2 HG22 ? ? SING CG2 HG23 ? ? SING OG1 P ? ? DOUB P O1P ? ? SING P O2P ? ? SING P O3P ? ? SING O2P HOP2 ? ? SING O3P HOP3 ? ? DOUB C O ? ? SING C OXT ? ? SING OXT HXT ? ? stop_ save_ save_chem_comp_SEP _Saveframe_category polymer_residue _Mol_type 'L-PEPTIDE LINKING' _Name_common PHOSPHOSERINE _BMRB_code SEP _PDB_code SEP _Standard_residue_derivative . _Molecular_mass 185.072 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons C C C . 0 . ? CA CA C . 0 . ? CB CB C . 0 . ? H H H . 0 . ? H2 H2 H . 0 . ? HA HA H . 0 . ? HB2 HB2 H . 0 . ? HB3 HB3 H . 0 . ? HOP2 HOP2 H . 0 . ? HOP3 HOP3 H . 0 . ? HXT HXT H . 0 . ? N N N . 0 . ? O O O . 0 . ? O1P O1P O . 0 . ? O2P O2P O . 0 . ? O3P O3P O . 0 . ? OG OG O . 0 . ? OXT OXT O . 0 . ? P P P . 0 . ? stop_ loop_ _Bond_order _Bond_atom_one_atom_name _Bond_atom_two_atom_name _PDB_bond_atom_one_atom_name _PDB_bond_atom_two_atom_name SING N CA ? ? SING N H ? ? SING N H2 ? ? SING CA CB ? ? SING CA C ? ? SING CA HA ? ? SING CB OG ? ? SING CB HB2 ? ? SING CB HB3 ? ? SING OG P ? ? DOUB C O ? ? SING C OXT ? ? SING OXT HXT ? ? DOUB P O1P ? ? SING P O2P ? ? SING P O3P ? ? SING O2P HOP2 ? ? SING O3P HOP3 ? ? stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $TAU231 . . . . . . 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 $TAU231 'chemical synthesis' . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $TAU231 1 mM 'natural abundance' D2O 10 % 'natural abundance' DSS 0.1 mM 'natural abundance' 'sodium phosphate' 200 mM 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_CcpNmr_Analysis _Saveframe_category software _Name CcpNmr_Analysis _Version 2.2 loop_ _Vendor _Address _Electronic_address CCPN 'Department of Biochemistry, Cambridge CB2 1GA, UK' http://www.ccpn.ac.uk stop_ loop_ _Task 'chemical shift assignment' stop_ _Details 'The CCPN NMR assignment and data analysis application' save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_Avance700 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 700 _Details . save_ save_Avance800 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 800 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-15N_HSQC_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample save_ save_2D_DQF-COSY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D DQF-COSY' _Sample_label $sample save_ save_2D_1H-1H_NOESY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample save_ save_2D_1H-1H_TOCSY_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample save_ save_2D_1H-1H_ROESY_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H ROESY' _Sample_label $sample save_ save_2D_1H-13C_HSQC_6 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $sample save_ save_2D_1H-13C_HMBC_7 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HMBC' _Sample_label $sample save_ save_NMR_spectrometer_expt _Saveframe_category NMR_applied_experiment _Experiment_name . _BMRB_pulse_sequence_accession_number . _Details . save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units temperature 300 . K pH 5.8 . pH pressure 1 . atm 'ionic strength' 0.2 . M stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chemical_shift_reference_1 _Saveframe_category chemical_shift_reference _Details . 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 internal direct . . . 1.000000000 DSS C 13 'methyl protons' ppm 0.00 na indirect . . . 0.251449530 DSS N 15 'methyl protons' ppm 0.00 na indirect . . . 0.101329118 stop_ save_ ################################### # Assigned chemical shift lists # ################################### ################################################################### # Chemical Shift Ambiguity Index Value Definitions # # # # The values other than 1 are used for those atoms with different # # chemical shifts that cannot be assigned to stereospecific atoms # # or to specific residues or chains. # # # # Index Value Definition # # # # 1 Unique (including isolated methyl protons, # # geminal atoms, and geminal methyl # # groups with identical chemical shifts) # # (e.g. ILE HD11, HD12, HD13 protons) # # 2 Ambiguity of geminal atoms or geminal methyl # # proton groups (e.g. ASP HB2 and HB3 # # protons, LEU CD1 and CD2 carbons, or # # LEU HD11, HD12, HD13 and HD21, HD22, # # HD23 methyl protons) # # 3 Aromatic atoms on opposite sides of # # symmetrical rings (e.g. TYR HE1 and HE2 # # protons) # # 4 Intraresidue ambiguities (e.g. LYS HG and # # HD protons or TRP HZ2 and HZ3 protons) # # 5 Interresidue ambiguities (LYS 12 vs. LYS 27) # # 6 Intermolecular ambiguities (e.g. ASP 31 CA # # in monomer 1 and ASP 31 CA in monomer 2 # # of an asymmetrical homodimer, duplex # # DNA assignments, or other assignments # # that may apply to atoms in one or more # # molecule in the molecular assembly) # # 9 Ambiguous, specific ambiguity not defined # # # ################################################################### save_assigned_chem_shift_list _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-15N HSQC' '2D DQF-COSY' '2D 1H-1H NOESY' '2D 1H-1H TOCSY' '2D 1H-13C HSQC' '2D 1H-13C HMBC' stop_ loop_ _Sample_label $sample stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name TAU231 _Text_data_format . _Text_data . loop_ _Atom_shift_assign_ID _Residue_author_seq_code _Residue_seq_code _Residue_label _Atom_name _Atom_type _Chem_shift_value _Chem_shift_value_error _Chem_shift_ambiguity_code 1 3 3 ALA H H 8.384 0.001 1 2 3 3 ALA HA H 4.248 0.008 1 3 3 3 ALA HB H 1.291 0.014 1 4 3 3 ALA CA C 53.394 0.061 1 5 3 3 ALA CB C 19.780 0.097 1 6 3 3 ALA N N 124.155 . 1 7 4 4 TYR H H 8.274 0.001 1 8 4 4 TYR HA H 4.480 0.009 1 9 4 4 TYR HB3 H 2.994 0.01 1 10 4 4 TYR HD1 H 7.104 0.008 3 11 4 4 TYR HD2 H 7.104 0.008 3 12 4 4 TYR HE1 H 6.819 0.012 3 13 4 4 TYR HE2 H 6.819 0.012 3 14 4 4 TYR CA C 58.820 . 1 15 4 4 TYR CB C 39.281 0.064 1 16 4 4 TYR CG C 131.466 0.099 1 17 4 4 TYR CD1 C 133.875 0.14 3 18 4 4 TYR CD2 C 133.875 0.14 3 19 4 4 TYR CE1 C 118.922 0.151 3 20 4 4 TYR CE2 C 118.922 0.151 3 21 4 4 TYR N N 119.694 . 1 22 6 6 ALA H H 8.234 0.004 1 23 6 6 ALA HA H 4.246 0.003 1 24 6 6 ALA HB H 1.398 0.007 1 25 6 6 ALA CA C 53.641 0.014 1 26 6 6 ALA N N 124.996 . 1 27 7 7 GLY H H 8.380 0.001 1 28 7 7 GLY HA3 H 3.963 0.003 1 29 7 7 GLY CA C 46.057 . 1 30 7 7 GLY N N 107.905 . 1 31 8 8 GLY H H 8.239 0.004 1 32 8 8 GLY HA3 H 3.953 0.002 1 33 8 8 GLY CA C 45.873 . 1 34 8 8 GLY N N 108.691 . 1 35 9 9 GLY H H 8.307 0.001 1 36 9 9 GLY HA3 H 3.876 0.001 1 37 9 9 GLY CA C 45.816 . 1 38 9 9 GLY N N 108.495 . 1 39 10 10 HIS H H 8.436 0.004 1 40 10 10 HIS HA H 4.702 0.003 1 41 10 10 HIS HB2 H 3.123 0.009 2 42 10 10 HIS HB3 H 3.253 0.012 2 43 10 10 HIS HD2 H 7.214 0.006 1 44 10 10 HIS HE1 H 8.432 0.006 1 45 10 10 HIS CA C 56.156 0.067 1 46 10 10 HIS CB C 29.800 0.004 1 47 10 10 HIS CG C 132.655 0.025 1 48 10 10 HIS CD2 C 120.735 0.06 1 49 10 10 HIS CE1 C 137.315 0.081 1 50 10 10 HIS N N 118.373 . 1 51 11 11 ASN H H 8.651 0.002 1 52 11 11 ASN HA H 4.702 0.002 1 53 11 11 ASN HB2 H 2.759 0.011 2 54 11 11 ASN HB3 H 2.866 0.009 2 55 11 11 ASN CA C 54.145 0.017 1 56 11 11 ASN CB C 39.498 0.036 1 57 11 11 ASN N N 120.196 . 1 58 12 12 GLY H H 8.449 0.003 1 59 12 12 GLY HA3 H 3.919 0.001 1 60 12 12 GLY CA C 45.988 . 1 61 12 12 GLY N N 109.375 . 1 62 13 13 VAL H H 7.858 0.003 1 63 13 13 VAL HA H 4.049 0.002 1 64 13 13 VAL HB H 1.965 0.007 1 65 13 13 VAL HG2 H 0.809 0.009 1 66 13 13 VAL CA C 63.080 0.048 1 67 13 13 VAL CB C 33.256 . 1 68 13 13 VAL CG2 C 21.586 0.028 1 69 13 13 VAL N N 119.458 . 1 70 14 14 PHE H H 8.406 0.002 1 71 14 14 PHE HA H 4.679 0.002 1 72 14 14 PHE HB2 H 2.970 0.006 2 73 14 14 PHE HB3 H 3.159 0.01 2 74 14 14 PHE HD1 H 7.247 0.028 3 75 14 14 PHE HD2 H 7.247 0.028 3 76 14 14 PHE HE1 H 7.280 0.026 3 77 14 14 PHE HE2 H 7.280 0.026 3 78 14 14 PHE HZ H 7.265 . 1 79 14 14 PHE CA C 58.112 . 1 80 14 14 PHE CB C 40.304 0.016 1 81 14 14 PHE CG C 139.889 0.016 1 82 14 14 PHE CD1 C 132.450 . 3 83 14 14 PHE CD2 C 132.450 . 3 84 14 14 PHE CE1 C 131.936 . 3 85 14 14 PHE CE2 C 131.936 . 3 86 14 14 PHE CZ C 130.508 0.198 1 87 14 14 PHE N N 123.887 . 1 88 15 15 ASP H H 8.233 0.002 1 89 15 15 ASP HA H 4.646 0.003 1 90 15 15 ASP HB2 H 2.716 0.041 2 91 15 15 ASP HB3 H 2.636 0.025 2 92 15 15 ASP CA C 54.762 0.088 1 93 15 15 ASP N N 122.855 . 1 94 16 16 GLY H H 7.784 0.002 1 95 16 16 GLY HA2 H 4.051 0.003 2 96 16 16 GLY HA3 H 3.998 0.005 2 97 16 16 GLY CA C 45.536 . 1 98 16 16 GLY N N 108.966 . 1 99 17 17 PRO HA H 4.456 0.01 1 100 17 17 PRO HB2 H 2.296 0.005 2 101 17 17 PRO HB3 H 1.929 0.008 2 102 17 17 PRO HG2 H 2.026 0.003 2 103 17 17 PRO HG3 H 2.304 0.001 2 104 17 17 PRO HD2 H 3.633 0.005 2 105 17 17 PRO HD3 H 3.813 0.004 2 106 17 17 PRO CA C 64.187 . 1 107 17 17 PRO CB C 32.840 0.024 1 108 17 17 PRO CG C 28.038 2.404 1 109 17 17 PRO CD C 51.199 0.016 1 110 18 18 SER H H 8.382 0.002 1 111 18 18 SER HA H 4.412 0.002 1 112 18 18 SER HB3 H 3.851 0.012 1 113 18 18 SER CA C 59.038 0.015 1 114 18 18 SER CB C 64.260 . 1 115 18 18 SER N N 115.746 . 1 116 19 19 LEU H H 8.252 0.001 1 117 19 19 LEU HA H 4.359 0.004 1 118 19 19 LEU HB3 H 1.594 0.006 1 119 19 19 LEU HG H 1.598 0.005 1 120 19 19 LEU HD1 H 0.903 0.007 2 121 19 19 LEU HD2 H 0.852 0.007 2 122 19 19 LEU CA C 60.211 . 1 123 19 19 LEU CB C 43.092 0.062 1 124 19 19 LEU CG C 27.643 . 1 125 19 19 LEU CD1 C 25.514 . 2 126 19 19 LEU CD2 C 24.220 . 2 127 19 19 LEU N N 124.652 . 1 128 20 20 VAL H H 8.112 0.006 1 129 20 20 VAL HA H 4.087 0.007 1 130 20 20 VAL HB H 2.033 0.008 1 131 20 20 VAL HG2 H 0.918 0.01 1 132 20 20 VAL CA C 62.878 0.037 1 133 20 20 VAL CB C 33.329 0.093 1 134 20 20 VAL CG2 C 21.819 0.092 1 135 20 20 VAL N N 121.738 . 1 136 21 21 ARG H H 8.396 0.002 1 137 21 21 ARG HA H 4.408 0.014 1 138 21 21 ARG HB2 H 1.751 0.004 2 139 21 21 ARG HB3 H 1.854 0.005 2 140 21 21 ARG HG3 H 1.622 0.005 1 141 21 21 ARG HD2 H 3.190 0.009 1 142 21 21 ARG HE H 7.325 0.004 1 143 21 21 ARG C C 175.286 . 1 144 21 21 ARG CA C 56.388 . 1 145 21 21 ARG CB C 31.830 0.121 1 146 21 21 ARG CG C 27.675 0.013 1 147 21 21 ARG CD C 43.900 . 1 148 21 21 ARG N N 125.856 . 1 149 22 22 TPO H H 8.743 0.001 1 150 22 22 TPO HA H 4.604 0.001 1 151 22 22 TPO HB H 4.476 0.003 1 152 22 22 TPO HG21 H 1.339 0.007 1 153 22 22 TPO HG22 H 1.339 0.007 1 154 22 22 TPO HG23 H 1.339 0.007 1 155 22 22 TPO CA C 60.572 . 1 156 22 22 TPO CB C 73.766 . 1 157 22 22 TPO CG2 C 21.244 . 1 158 22 22 TPO N N 119.675 . 1 159 23 23 PRO HA H 4.658 0.005 1 160 23 23 PRO HB2 H 1.856 0.002 2 161 23 23 PRO HB3 H 2.376 0.003 2 162 23 23 PRO HG2 H 1.998 0.005 2 163 23 23 PRO HG3 H 2.083 0.005 2 164 23 23 PRO HD2 H 3.715 0.003 2 165 23 23 PRO HD3 H 3.945 0.003 2 166 23 23 PRO CA C 62.347 . 1 167 23 23 PRO CB C 31.583 0.002 1 168 23 23 PRO CG C 28.197 . 1 169 23 23 PRO CD C 51.796 0.022 1 170 25 25 LYS H H 8.492 0.002 1 171 25 25 LYS HA H 4.327 0.004 1 172 25 25 LYS HB2 H 1.828 0.003 2 173 25 25 LYS HB3 H 1.758 0.005 2 174 25 25 LYS HG3 H 1.484 0.006 1 175 25 25 LYS HD3 H 1.701 0.01 1 176 25 25 LYS HE3 H 3.017 0.004 1 177 25 25 LYS CA C 56.646 . 1 178 25 25 LYS CB C 33.924 0.014 1 179 25 25 LYS CG C 25.270 0.015 1 180 25 25 LYS CD C 29.606 . 1 181 25 25 LYS CE C 42.772 . 1 182 25 25 LYS N N 122.431 . 1 183 26 26 SEP H H 8.679 0.001 1 184 26 26 SEP HA H 4.833 0.009 1 185 26 26 SEP HB3 H 4.070 0.005 1 186 26 26 SEP CB C 66.117 . 1 187 26 26 SEP N N 118.769 . 1 stop_ save_