data_1127 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Static and Transient Hydrogen-Bonding Interactions in Recombinant Desulfatohirudin Studied by 1H Nuclear Magnetic Resonance Measurements of Amide Proton Exchange Rates and pH-Dependent Chemical Shifts ; _BMRB_accession_number 1127 _BMRB_flat_file_name bmr1127.str _Entry_type update _Submission_date 1995-07-31 _Accession_date 1996-04-13 _Entry_origination BMRB _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 Haruyama Hideyuki . . 2 Qian Yan-qiu . . 3 Wuthrich Kurt . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 23 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2010-06-14 revision BMRB 'Complete natural source information' 1999-06-14 revision BMRB 'Converted to BMRB NMR-STAR V 2.1 format' 1996-04-13 revision BMRB 'Link to the Protein Data Bank added' 1996-03-25 reformat BMRB 'Converted to the BMRB 1996-03-01 STAR flat-file format' 1995-07-31 original BMRB 'Last release in original BMRB flat-file format' stop_ save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full ; Haruyama, Hideyuki, Qian, Yan-qiu, Wuthrich, Kurt, "Static and Transient Hydrogen-Bonding Interactions in Recombinant Desulfatohirudin Studied by 1H Nuclear Magnetic Resonance Measurements of Amide Proton Exchange Rates and pH-Dependent Chemical Shifts," Biochemistry 28, 4312-4317 (1989). ; _Citation_title ; Static and Transient Hydrogen-Bonding Interactions in Recombinant Desulfatohirudin Studied by 1H Nuclear Magnetic Resonance Measurements of Amide Proton Exchange Rates and pH-Dependent Chemical Shifts ; _Citation_status published _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 Haruyama Hideyuki . . 2 Qian Yan-qiu . . 3 Wuthrich Kurt . . stop_ _Journal_abbreviation Biochemistry _Journal_volume 28 _Journal_issue . _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 4312 _Page_last 4317 _Year 1989 _Details . save_ ################################## # Molecular system description # ################################## save_system_desulfatohirudin _Saveframe_category molecular_system _Mol_system_name desulfatohirudin _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label desulfatohirudin $desulfatohirudin stop_ _System_molecular_weight . _System_oligomer_state ? _System_paramagnetic ? _System_thiol_state . _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_desulfatohirudin _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common desulfatohirudin _Molecular_mass . _Mol_thiol_state . _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 65 _Mol_residue_sequence ; VVYTDCTESGQNLCLCEGSN VCGQGNKCILGSDGEKNQCV TGEGTPKPQSHNDGDFEEIP EEYLQ ; loop_ _Residue_seq_code _Residue_label 1 VAL 2 VAL 3 TYR 4 THR 5 ASP 6 CYS 7 THR 8 GLU 9 SER 10 GLY 11 GLN 12 ASN 13 LEU 14 CYS 15 LEU 16 CYS 17 GLU 18 GLY 19 SER 20 ASN 21 VAL 22 CYS 23 GLY 24 GLN 25 GLY 26 ASN 27 LYS 28 CYS 29 ILE 30 LEU 31 GLY 32 SER 33 ASP 34 GLY 35 GLU 36 LYS 37 ASN 38 GLN 39 CYS 40 VAL 41 THR 42 GLY 43 GLU 44 GLY 45 THR 46 PRO 47 LYS 48 PRO 49 GLN 50 SER 51 HIS 52 ASN 53 ASP 54 GLY 55 ASP 56 PHE 57 GLU 58 GLU 59 ILE 60 PRO 61 GLU 62 GLU 63 TYR 64 LEU 65 GLN stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date 2015-09-23 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 BMRB 1128 desulfatohirudin 100.00 65 100.00 100.00 1.24e-37 BMRB 1129 desulfatohirudin 100.00 65 100.00 100.00 1.24e-37 BMRB 27 hirudin 100.00 65 98.46 98.46 1.87e-36 PDB 1HIC "The Nmr Solution Structure Of Hirudin(1-51) And Comparison With Corresponding Three-Dimensional Structures Determined Using The" 76.92 51 100.00 100.00 5.88e-26 PDB 1HRT "The Structure Of A Complex Of Bovine Alpha-Thrombin And Recombinant Hirudin At 2.8 Angstroms Resolution" 100.00 65 100.00 100.00 1.24e-37 PDB 2HIR "Solution Structure Of Recombinant Hirudin And The Lys-47 (Right Arrow) Glu Mutant. A Nuclear Magnetic Resonance And Hybrid Dist" 100.00 65 100.00 100.00 1.24e-37 PDB 4HIR "Solution Structure Of Recombinant Hirudin And The Lys-47 (Right Arrow) Glu Mutant. A Nuclear Magnetic Resonance And Hybrid Dist" 100.00 65 98.46 100.00 5.66e-37 PDB 4MLF "Crystal Structure For The Complex Of Thrombin Mutant D102n And Hirudin" 100.00 65 100.00 100.00 1.24e-37 PDB 5HIR "Solution Structure Of Recombinant Hirudin And The Lys-47 (Right Arrow) Glu Mutant. A Nuclear Magnetic Resonance And Hybrid Dist" 100.00 65 100.00 100.00 1.24e-37 PDB 6HIR "Solution Structure Of Recombinant Hirudin And The Lys-47 (Right Arrow) Glu Mutant. A Nuclear Magnetic Resonance And Hybrid Dist" 100.00 65 98.46 100.00 5.66e-37 GB AAA72556 "hirudin precursor, partial [synthetic construct]" 100.00 68 100.00 100.00 8.83e-38 GB AAA72772 "hirudin [synthetic construct]" 100.00 66 100.00 100.00 1.01e-37 GB AAA73216 "CTAP-III(Leu21)--hirudin fusion protein [unidentified cloning vector]" 100.00 162 100.00 100.00 3.31e-38 GB AAF85971 "hirudin [synthetic construct]" 100.00 65 100.00 100.00 1.24e-37 GB AAG33034 "PR-S/hirudin fusion protein [synthetic construct]" 100.00 90 100.00 100.00 3.85e-38 PRF 1002207A hirudin 100.00 65 100.00 100.00 1.24e-37 SP P01050 "RecName: Full=Hirudin variant-1; AltName: Full=Hirudin-1; AltName: Full=Hirudin-I; AltName: Full=Lepirudin" 100.00 65 100.00 100.00 1.24e-37 SP P28509 "RecName: Full=Hirudin-3; AltName: Full=Hirudin III" 100.00 65 96.92 98.46 4.98e-36 SP P28511 "RecName: Full=Hirudin-3B'; AltName: Full=Hirudin IIIB'" 100.00 65 96.92 100.00 1.35e-36 stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species _Strain $desulfatohirudin leech 6421 Eukaryota Metazoa Hirudo medicinalis generic 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 $desulfatohirudin 'not available' . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_one _Saveframe_category sample _Sample_type solution _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_list _Saveframe_category NMR_spectrometer _Manufacturer unknown _Model unknown _Field_strength 0 _Details 'spectrometer information not available' save_ ############################# # NMR applied experiments # ############################# save__1 _Saveframe_category NMR_applied_experiment _Sample_label $sample_one save_ ####################### # Sample conditions # ####################### save_sample_condition_set_one _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 4.5 . na temperature 295 . K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chem_shift_reference_par_set_one _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_citation_label _Correction_value_citation_label TSP H . . ppm 0 . . . . . $entry_citation $entry_citation 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_chemical_shift_assignment_data_set_one _Saveframe_category assigned_chemical_shifts _Details . loop_ _Sample_label $sample_one stop_ _Sample_conditions_label $sample_condition_set_one _Chem_shift_reference_set_label $chem_shift_reference_par_set_one _Mol_system_component_name desulfatohirudin _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 . 4 THR H H 9.02 . 1 2 . 6 CYS H H 8.96 . 1 3 . 8 GLU H H 7.36 . 1 4 . 10 GLY H H 9.73 . 1 5 . 11 GLN H H 7.42 . 1 6 . 12 ASN H H 8.16 . 1 7 . 13 LEU H H 9.21 . 1 8 . 14 CYS H H 7.29 . 1 9 . 15 LEU H H 9.05 . 1 10 . 16 CYS H H 7.49 . 1 11 . 20 ASN H H 7.97 . 1 12 . 21 VAL H H 9.08 . 1 13 . 22 CYS H H 8.45 . 1 14 . 26 ASN H H 8.04 . 1 15 . 27 LYS H H 9.3 . 1 16 . 28 CYS H H 9.08 . 1 17 . 29 ILE H H 9.89 . 1 18 . 30 LEU H H 8.46 . 1 19 . 31 GLY H H 8.97 . 1 20 . 35 GLU H H 7.82 . 1 21 . 38 GLN H H 8.47 . 1 22 . 40 VAL H H 9.26 . 1 23 . 42 GLY H H 8.25 . 1 stop_ save_