data_18537 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; 1H and 13C chemical shifts for collagelin ; _BMRB_accession_number 18537 _BMRB_flat_file_name bmr18537.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" 83 "13C chemical shifts" 41 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2012-12-21 original author . stop_ loop_ _Related_BMRB_accession_number _Relationship 18538 '1H and 13C NMR of GPVI mimetic' stop_ _Original_release_date 2012-12-21 save_ ############################# # Citation for this entry # ############################# save_Collagelin_NMR _Saveframe_category entry_citation _Citation_full . _Citation_title 'Collagelin 1H and 13C NMR data' _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 'Herve du Penhoat' Catherine . . 2 Gnanagurunathan Nimalta . . 3 Guenin Erwann . . 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 . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name collagelin _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label collagelin $collagelin stop_ _System_molecular_weight 2178.4 _System_physical_state native _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_collagelin _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common collagelin _Molecular_mass 2178.4 _Mol_thiol_state 'all disulfide bound' loop_ _Biological_function 'GPVI mimetic' stop_ _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 23 _Mol_residue_sequence ; SGSGCGPRVMHGLHLGDDEG PCX ; loop_ _Residue_seq_code _Residue_label 1 SER 2 GLY 3 SER 4 GLY 5 CYS 6 GLY 7 PRO 8 ARG 9 VAL 10 MET 11 HIS 12 GLY 13 LEU 14 HIS 15 LEU 16 GLY 17 ASP 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 $collagelin . . . . . . 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 $collagelin 'obtained from a vendor' . . . . . 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 $collagelin 3 mM 'natural abundance' H2O 93 % 'natural abundance' D2O 7 % '[U-100% 2H]' 'sodium phosphate' 20 mM 'natural abundance' 'sodium azide' 5 uM 'natural abundance' 'sodium chloride' 50 mM '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 . . 'Koradi, Billeter and Wuthrich' . . 'Bartels et al.' . . 'Delaglio, Grzesiek, Vuister, Zhu, Pfeifer and Bax' . . 'Delaglio, Grzesiek, Vuister, Zhu, Pfeifer and Bax' . . stop_ loop_ _Task 'structure solution' processing refinement 'peak picking' '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_ save_2D_1H-1H_TOCSY_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample_1 save_ save_2D_1H-1H_NOESY_6 _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 collagelin _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 4.208 0.005 1 2 1 1 SER HB2 H 3.997 0.005 1 3 1 1 SER HB3 H 3.997 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 8.732 0.005 1 7 2 2 GLY HA2 H 4.070 0.005 1 8 2 2 GLY HA3 H 4.070 0.005 1 9 2 2 GLY CA C 45.7 0.1 1 10 3 3 SER H H 8.438 0.005 1 11 3 3 SER HA H 4.479 0.005 1 12 3 3 SER HB2 H 3.873 0.005 1 13 3 3 SER HB3 H 3.873 0.005 1 14 3 3 SER CA C 59.0 0.1 1 15 3 3 SER CB C 64.5 0.1 1 16 4 4 GLY H H 8.507 0.005 1 17 4 4 GLY HA2 H 3.990 0.005 1 18 4 4 GLY HA3 H 3.990 0.005 1 19 4 4 GLY CA C 45.9 0.1 1 20 5 5 CYS H H 8.339 0.005 1 21 5 5 CYS HA H 4.725 0.005 1 22 5 5 CYS HB2 H 2.956 0.005 1 23 5 5 CYS HB3 H 3.236 0.005 1 24 5 5 CYS CB C 42.0 0.1 1 25 6 6 GLY H H 8.392 0.005 1 26 6 6 GLY HA2 H 4.095 0.005 1 27 6 6 GLY HA3 H 4.095 0.005 1 28 6 6 GLY CA C 45.3 0.1 1 29 7 7 PRO HA H 4.394 0.005 1 30 7 7 PRO HB2 H 1.892 0.005 1 31 7 7 PRO HB3 H 2.258 0.005 1 32 7 7 PRO HG2 H 1.998 0.005 1 33 7 7 PRO HG3 H 1.998 0.005 1 34 7 7 PRO HD2 H 3.616 0.005 1 35 7 7 PRO HD3 H 3.616 0.005 1 36 7 7 PRO CA C 64.0 0.1 1 37 7 7 PRO CB C 32.6 0.1 1 38 7 7 PRO CG C 27.7 0.1 1 39 7 7 PRO CD C 50.3 0.1 1 40 8 8 ARG H H 8.348 0.005 1 41 8 8 ARG HA H 4.305 0.005 1 42 8 8 ARG HB2 H 1.759 0.005 1 43 8 8 ARG HB3 H 1.819 0.005 1 44 8 8 ARG HG2 H 1.590 0.005 2 45 8 8 ARG HG3 H 1.618 0.005 2 46 8 8 ARG HD2 H 3.178 0.005 1 47 8 8 ARG HD3 H 3.178 0.005 1 48 8 8 ARG HE H 7.159 0.005 1 49 8 8 ARG HH11 H 6.960 0.010 1 50 8 8 ARG HH12 H 7.065 0.010 1 51 8 8 ARG HH21 H 6.960 0.010 1 52 8 8 ARG HH22 H 7.065 0.010 1 53 8 8 ARG CA C 56.8 0.1 1 54 8 8 ARG CB C 31.2 0.1 1 55 8 8 ARG CG C 27.6 0.1 1 56 8 8 ARG CD C 43.9 0.1 1 57 9 9 VAL H H 8.014 0.005 1 58 9 9 VAL HA H 4.092 0.005 1 59 9 9 VAL HB H 1.995 0.005 1 60 9 9 VAL HG1 H 0.822 0.005 1 61 9 9 VAL HG2 H 0.865 0.005 1 62 9 9 VAL CA C 62.7 0.1 1 63 9 9 VAL CB C 33.3 0.1 1 64 9 9 VAL CG1 C 21.7 0.1 1 65 9 9 VAL CG2 C 21.1 0.1 1 66 10 10 MET H H 8.364 0.005 1 67 10 10 MET HA H 4.438 0.005 1 68 10 10 MET HB2 H 1.925 0.005 1 69 10 10 MET HB3 H 1.925 0.005 1 70 10 10 MET HG2 H 2.428 0.005 2 71 10 10 MET HG3 H 2.509 0.005 2 72 10 10 MET HE H 2.020 0.005 1 73 10 10 MET CA C 55.8 0.1 1 74 10 10 MET CB C 33.4 0.1 1 75 10 10 MET CG C 32.4 0.1 1 76 10 10 MET CE C 17.4 0.1 1 77 11 11 HIS H H 8.497 0.005 1 78 11 11 HIS HA H 4.684 0.005 1 79 11 11 HIS HB2 H 3.190 0.005 2 80 11 11 HIS HB3 H 3.290 0.005 2 81 11 11 HIS HD2 H 7.294 0.005 1 82 11 11 HIS HE1 H 8.602 0.005 1 83 11 11 HIS CA C 55.8 0.1 1 84 11 11 HIS CB C 29.4 0.1 1 85 11 11 HIS CD2 C 120.6 0.1 1 86 12 12 GLY H H 8.410 0.005 1 87 12 12 GLY HA2 H 3.845 0.005 2 88 12 12 GLY HA3 H 3.975 0.005 2 89 12 12 GLY CA C 45.7 0.1 1 90 13 13 LEU H H 8.105 0.005 1 91 13 13 LEU HA H 4.281 0.005 1 92 13 13 LEU HB2 H 1.550 0.005 1 93 13 13 LEU HB3 H 1.439 0.005 1 94 13 13 LEU HG H 1.502 0.005 1 95 13 13 LEU HD1 H 0.818 0.005 2 96 13 13 LEU HD2 H 0.882 0.005 2 97 13 13 LEU CA C 55.7 0.1 1 98 13 13 LEU CB C 43.1 0.1 1 99 13 13 LEU CG C 27.4 0.1 1 100 13 13 LEU CD1 C 24.0 0.1 2 101 13 13 LEU CD2 C 25.3 0.1 2 102 14 14 HIS H H 8.533 0.005 1 103 14 14 HIS HA H 4.694 0.005 1 104 14 14 HIS HB2 H 3.168 0.005 2 105 14 14 HIS HB3 H 3.271 0.005 2 106 14 14 HIS HD2 H 7.270 0.005 1 107 14 14 HIS HE1 H 8.585 0.005 1 108 14 14 HIS CA C 55.4 0.1 1 109 14 14 HIS CB C 29.2 0.1 1 110 14 14 HIS CD2 C 120.6 0.1 1 111 15 15 LEU H H 8.327 0.005 1 112 15 15 LEU HA H 4.327 0.005 1 113 15 15 LEU HB2 H 1.551 0.005 2 114 15 15 LEU HB3 H 1.608 0.005 2 115 15 15 LEU HG H 1.551 0.005 1 116 15 15 LEU HD1 H 0.834 0.005 2 117 15 15 LEU HD2 H 0.879 0.005 2 118 15 15 LEU CA C 55.9 0.1 1 119 15 15 LEU CB C 42.9 0.1 1 120 15 15 LEU CG C 27.4 0.1 1 121 15 15 LEU CD1 C 24.0 0.1 2 122 15 15 LEU CD2 C 25.5 0.1 2 123 16 16 GLY H H 8.468 0.005 1 124 16 16 GLY HA2 H 3.903 0.005 2 stop_ save_