data_18538 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; 1H and 13C NMR of GPVI mimetic ; _BMRB_accession_number 18538 _BMRB_flat_file_name bmr18538.str _Entry_type original _Submission_date 2012-06-20 _Accession_date 2012-06-20 _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 Gnanagurunathan Nimalta . . 2 Guenin Erwann . . 3 'Herve du Penhoat' Catherine . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 119 "13C chemical shifts" 57 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2012-12-21 original author . stop_ loop_ _Related_BMRB_accession_number _Relationship 18537 'Collagelin 1H and 13C NMR data' stop_ _Original_release_date 2012-12-21 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title '1H and 13C NMR of GPVI mimetic' _Citation_status 'in preparation' _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID ? loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Gnanagurunathan Nimalta . . 2 Guenin Erwann . . 3 'Herve du Penhoat' Catherine . . stop_ _Journal_abbreviation 'Not known' _Journal_volume . _Journal_issue . _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first . _Page_last . _Year . _Details . loop_ _Keyword 'GPVI peptide mimetic' stop_ save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'GPVI peptide mimetic' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label 'GPVI peptide mimetic' $GPVI_peptide_mimetic stop_ _System_molecular_weight . _System_physical_state native _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_GPVI_peptide_mimetic _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common GPVI_peptide_mimetic _Molecular_mass 2302.8 _Mol_thiol_state 'all disulfide bound' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 23 _Mol_residue_sequence ; SGSGCGPRFMHGLQLWADEG PCX ; loop_ _Residue_seq_code _Residue_label 1 SER 2 GLY 3 SER 4 GLY 5 CYS 6 GLY 7 PRO 8 ARG 9 PHE 10 MET 11 HIS 12 GLY 13 LEU 14 GLN 15 LEU 16 TRP 17 ALA 18 ASP 19 GLU 20 GLY 21 PRO 22 CYS 23 NH2 stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ###################### # Polymer residues # ###################### save_chem_comp_NH2 _Saveframe_category polymer_residue _Mol_type NON-POLYMER _Name_common 'AMINO GROUP' _BMRB_code NH2 _PDB_code NH2 _Standard_residue_derivative . _Molecular_mass 16.023 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons HN1 HN1 H . 0 . ? HN2 HN2 H . 0 . ? N N N . 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 HN1 ? ? SING N HN2 ? ? stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $GPVI_peptide_mimetic . . . . . . 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 $GPVI_peptide_mimetic 'chemical synthesis' . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $GPVI_peptide_mimetic 3 mM 'natural abundance' H2O 93 % 'natural abundance' D2O 7 % '[U-100% 2H]' 'sodium chloride' 50 mM 'natural abundance' 'sodium phosphate' 20 mM 'natural abundance' 'sodium azide' 5 uM 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_DYANA _Saveframe_category software _Name DYANA _Version 'version 1.5' loop_ _Vendor _Address _Electronic_address 'Guntert, Braun and Wuthrich' . . Guntert . . 'Bartels et al.' . . 'Koradi, Billeter and Wuthrich' . . 'Delaglio, Grzesiek, Vuister, Zhu, Pfeifer and Bax' . . 'Delaglio, Grzesiek, Vuister, Zhu, Pfeifer and Bax' . . stop_ loop_ _Task 'structure solution' processing 'peak picking' refinement 'chemical shift assignment' 'chemical shift assignment' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Varian _Model UnityPlus _Field_strength 500 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-13C_HSQC_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $sample_1 save_ save_2D_DQF-COSY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D DQF-COSY' _Sample_label $sample_1 save_ save_2D_1H-1H_TOCSY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample_1 save_ save_2D_1H-1H_NOESY_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_1 save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units temperature 273 . K pH 5.4 0.1 pH pressure 1 . atm 'ionic strength' 70 . mM 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 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_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-13C HSQC' '2D DQF-COSY' '2D 1H-1H TOCSY' '2D 1H-1H NOESY' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name 'GPVI peptide mimetic' _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 1 1 SER HA H 4.198 0.005 1 2 1 1 SER HB2 H 3.999 0.005 1 3 1 1 SER HB3 H 3.999 0.005 1 4 1 1 SER CA C 58.0 0.1 1 5 1 1 SER CB C 63.5 0.1 1 6 2 2 GLY H H 8.715 0.005 1 7 2 2 GLY HA2 H 4.063 0.005 1 8 2 2 GLY HA3 H 4.063 0.005 1 9 2 2 GLY CA C 45.7 0.1 1 10 3 3 SER H H 8.412 0.005 1 11 3 3 SER HA H 4.455 0.005 1 12 3 3 SER HB2 H 3.851 0.005 1 13 3 3 SER HB3 H 3.851 0.005 1 14 3 3 SER CA C 58.9 0.1 1 15 3 3 SER CB C 64.5 0.1 1 16 4 4 GLY H H 8.422 0.005 1 17 4 4 GLY HA2 H 3.917 0.005 1 18 4 4 GLY HA3 H 3.917 0.005 1 19 4 4 GLY CA C 45.8 0.1 1 20 5 5 CYS H H 8.282 0.005 1 21 5 5 CYS HA H 4.712 0.005 1 22 5 5 CYS HB2 H 2.900 0.005 2 23 5 5 CYS HB3 H 3.144 0.005 2 24 5 5 CYS CA C 57.8 0.1 1 25 5 5 CYS CB C 42.0 0.1 1 26 6 6 GLY H H 8.381 0.005 1 27 6 6 GLY HA2 H 4.092 0.005 1 28 6 6 GLY HA3 H 4.092 0.005 1 29 6 6 GLY CA C 45.3 0.1 1 30 7 7 PRO HA H 4.333 0.005 1 31 7 7 PRO HB2 H 1.757 0.005 2 32 7 7 PRO HB3 H 2.137 0.005 2 33 7 7 PRO HG2 H 1.964 0.005 1 34 7 7 PRO HG3 H 1.964 0.005 1 35 7 7 PRO HD2 H 3.589 0.005 1 36 7 7 PRO HD3 H 3.589 0.005 1 37 7 7 PRO CA C 63.9 0.1 1 38 7 7 PRO CB C 32.6 0.1 1 39 7 7 PRO CG C 27.7 0.1 1 40 7 7 PRO CD C 50.3 0.1 1 41 8 8 ARG H H 8.304 0.005 1 42 8 8 ARG HA H 4.105 0.005 1 43 8 8 ARG HB2 H 1.564 0.005 1 44 8 8 ARG HB3 H 1.564 0.005 1 45 8 8 ARG HG2 H 1.346 0.005 1 46 8 8 ARG HG3 H 1.346 0.005 1 47 8 8 ARG HD2 H 3.004 0.005 1 48 8 8 ARG HD3 H 3.004 0.005 1 49 8 8 ARG HE H 7.020 0.005 1 50 8 8 ARG CA C 56.9 0.1 1 51 8 8 ARG CB C 31.3 0.1 1 52 8 8 ARG CG C 27.5 0.1 1 53 8 8 ARG CD C 43.9 0.1 1 54 9 9 PHE H H 8.056 0.005 1 55 9 9 PHE HA H 4.713 0.005 1 56 9 9 PHE HB2 H 2.861 0.005 2 57 9 9 PHE HB3 H 3.015 0.005 2 58 9 9 PHE HD1 H 7.096 0.005 1 59 9 9 PHE HD2 H 7.096 0.005 1 60 9 9 PHE HE1 H 7.245 0.005 1 61 9 9 PHE HE2 H 7.245 0.005 1 62 9 9 PHE CB C 40.6 0.1 1 63 10 10 MET H H 8.235 0.005 1 64 10 10 MET HA H 4.409 0.005 1 65 10 10 MET HB2 H 1.830 0.005 1 66 10 10 MET HB3 H 1.913 0.005 1 67 10 10 MET HG2 H 2.311 0.005 2 68 10 10 MET HG3 H 2.359 0.005 2 69 10 10 MET HE H 2.002 0.005 1 70 10 10 MET CA C 55.8 0.1 1 71 10 10 MET CB C 33.7 0.1 1 72 10 10 MET CG C 32.4 0.1 1 73 10 10 MET CE C 17.3 0.1 1 74 11 11 HIS H H 8.603 0.005 1 75 11 11 HIS HA H 4.534 0.005 1 76 11 11 HIS HB2 H 3.284 0.005 1 77 11 11 HIS HB3 H 3.167 0.005 1 78 11 11 HIS HD2 H 7.245 0.005 1 79 11 11 HIS HE1 H 8.569 0.005 1 80 11 11 HIS CA C 56.0 0.1 1 81 11 11 HIS CB C 28.8 0.1 1 82 12 12 GLY H H 8.396 0.005 1 83 12 12 GLY HA2 H 3.765 0.005 2 84 12 12 GLY HA3 H 4.033 0.005 2 85 12 12 GLY CA C 45.9 0.1 1 86 13 13 LEU H H 7.999 0.005 1 87 13 13 LEU HA H 4.362 0.005 1 88 13 13 LEU HB2 H 1.613 0.005 1 89 13 13 LEU HB3 H 1.566 0.005 1 90 13 13 LEU HG H 1.563 0.005 1 91 13 13 LEU HD1 H 0.848 0.005 2 92 13 13 LEU HD2 H 0.901 0.005 2 93 13 13 LEU CA C 55.4 0.1 1 94 13 13 LEU CB C 43.2 0.1 1 95 13 13 LEU CG C 27.4 0.1 1 96 13 13 LEU CD1 C 24.0 0.1 2 97 13 13 LEU CD2 C 25.4 0.1 2 98 14 14 GLN H H 8.303 0.005 1 99 14 14 GLN HA H 4.149 0.005 1 100 14 14 GLN HB2 H 1.830 0.005 1 101 14 14 GLN HB3 H 1.830 0.005 1 102 14 14 GLN HG2 H 2.122 0.005 1 103 14 14 GLN HG3 H 2.122 0.005 1 104 14 14 GLN HE21 H 6.832 0.010 1 105 14 14 GLN HE22 H 7.387 0.010 1 106 14 14 GLN CA C 56.2 0.1 1 107 14 14 GLN CB C 29.5 0.1 1 108 14 14 GLN CG C 34.3 0.1 1 109 15 15 LEU H H 8.133 0.005 1 110 15 15 LEU HA H 4.268 0.005 1 111 15 15 LEU HB2 H 1.408 0.005 2 112 15 15 LEU HB3 H 1.447 0.005 2 113 15 15 LEU HG H 1.431 0.005 1 114 15 15 LEU HD1 H 0.770 0.005 2 115 15 15 LEU HD2 H 0.820 0.005 2 116 15 15 LEU CA C 55.7 0.1 1 117 15 15 LEU CB C 43.0 0.1 1 118 15 15 LEU CG C 27.4 0.1 1 119 15 15 LEU CD1 C 24.0 0.1 2 120 15 15 LEU CD2 C 25.5 0.1 2 121 16 16 TRP H H 7.941 0.005 1 122 16 16 TRP HA H 4.643 0.005 1 123 16 16 TRP HB2 H 3.143 0.005 2 124 16 16 TRP HB3 H 3.271 0.005 2 125 16 16 TRP HD1 H 7.174 0.005 1 126 16 16 TRP HE1 H 10.025 0.005 1 127 16 16 TRP HE3 H 7.537 0.005 1 128 16 16 TRP HZ2 H 7.436 0.005 1 129 16 16 TRP HZ3 H 7.089 0.005 1 130 16 16 TRP HH2 H 7.186 0.005 1 131 16 16 TRP CA C 57.4 0.1 1 132 16 16 TRP CB C 30.2 0.1 1 133 16 16 TRP CE3 C 121.4 0.1 1 134 16 16 TRP CZ2 C 115.1 0.1 1 135 16 16 TRP CH2 C 125.1 0.1 1 136 17 17 ALA H H 8.169 0.005 1 137 17 17 ALA HA H 4.250 0.005 1 138 17 17 ALA HB H 1.282 0.005 1 139 17 17 ALA CA C 53.0 0.1 1 140 17 17 ALA CB C 19.9 0.1 1 141 18 18 ASP H H 8.244 0.005 1 142 18 18 ASP HA H 4.584 0.005 1 143 18 18 ASP HB2 H 2.873 0.005 1 144 18 18 ASP HB3 H 2.756 0.005 1 145 18 18 ASP CA C 54.0 0.1 1 146 18 18 ASP CB C 39.1 0.1 1 147 19 19 GLU H H 8.024 0.005 1 148 19 19 GLU HA H 4.397 0.005 1 149 19 19 GLU HB2 H 1.913 0.005 2 150 19 19 GLU HB3 H 2.102 0.005 2 151 19 19 GLU HG2 H 2.395 0.005 1 152 19 19 GLU HG3 H 2.395 0.005 1 153 19 19 GLU CA C 56.2 0.1 1 154 19 19 GLU CB C 29.8 0.1 1 155 19 19 GLU CG C 33.5 0.1 1 156 20 20 GLY H H 8.254 0.005 1 157 20 20 GLY HA2 H 3.964 0.005 2 158 20 20 GLY HA3 H 4.105 0.005 2 159 20 20 GLY CA C 45.3 0.1 1 160 21 21 PRO HA H 4.375 0.005 1 161 21 21 PRO HB2 H 1.945 0.005 2 162 21 21 PRO HB3 H 2.252 0.005 2 163 21 21 PRO HG2 H 1.979 0.005 1 164 21 21 PRO HG3 H 1.979 0.005 1 165 21 21 PRO HD2 H 3.642 0.005 1 166 21 21 PRO HD3 H 3.538 0.005 1 167 21 21 PRO CA C 64.2 0.1 1 168 21 21 PRO CB C 32.5 0.1 1 169 21 21 PRO CG C 27.7 0.1 1 170 21 21 PRO CD C 50.3 0.1 1 171 22 22 CYS H H 8.404 0.005 1 172 22 22 CYS HA H 4.540 0.005 1 173 22 22 CYS HB2 H 2.862 0.005 2 174 22 22 CYS HB3 H 3.098 0.005 2 175 22 22 CYS CA C 55.3 0.1 1 176 22 22 CYS CB C 41.2 0.1 1 stop_ save_