data_11006 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; The Glycosylated EGF-Like Repeats 12 From Mouse NOTCH-1, NMR, Minimized Average Structure ; _BMRB_accession_number 11006 _BMRB_flat_file_name bmr11006.str _Entry_type new _Submission_date 2007-08-24 _Accession_date 2007-08-24 _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 Hiruma-Shimizu Kazumi H. . 2 Shimizu Hiroki . . 3 Nishimura Shin-Ichiro . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 2 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 232 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2010-10-22 original author . stop_ save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title 'Chemical Synthesis, Folding, and Structural Insights into O-Fucosylated Epidermal Growth Factor-like Repeat 12 of Mouse Notch-1 Receptor' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 20883017 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Hiruma-Shimizu Kazumi H. . 2 Hosoguchi Kensaku . . 3 Liu Yan . . 4 Fujitani Naoki . . 5 Ohta Takashi . . 6 Hinou Hiroshi . . 7 Matsushita Takahiko . . 8 Shimizu Hiroki . . 9 Feizi Ten . . 10 Nishimura Shin-Ichiro . . stop_ _Journal_abbreviation 'J. Am. Chem. Soc.' _Journal_name_full 'Journal of the American Chemical Society' _Journal_volume 132 _Journal_issue 42 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 14857 _Page_last 14865 _Year 2010 _Details . loop_ _Keyword NOTCH 'EGF-LIKE DOMAIN' GLYCOPROTEIN 'O-LINKED FUCOSE' FRINGE RECEPTOR 'LIGAND BINDING' stop_ save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'Extracellular domain of mouse NOTCH 1EGF12' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label 'EGF12 peptide' $mouse_NOTCH-1_EGF12 'NAG b1-3 FUC' $disaccharide stop_ _System_molecular_weight 4561 _System_physical_state native _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . loop_ _Biological_function 'cell surface receptor' stop_ _Database_query_date . _Details ; This extracellular domain of NOTCH-1 protein contains 36 tandem EGF repeats. Each EGF repeats are numbered from 1 to 36. The EGF12 repeat contains O-linked fucose at Thr-15. ; save_ ######################## # Monomeric polymers # ######################## save_mouse_NOTCH-1_EGF12 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common mouse_NOTCH-1_EGF12 _Molecular_mass 4211.66 _Mol_thiol_state 'all disulfide bound' loop_ _Biological_function 'signaling receptor' stop_ _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 38 _Mol_residue_sequence ; DVNECISNPCQNDATCLDQI GEFQCICMPGYEGVYCEX ; loop_ _Residue_seq_code _Residue_label 1 ASP 2 VAL 3 ASN 4 GLU 5 CYS 6 ILE 7 SER 8 ASN 9 PRO 10 CYS 11 GLN 12 ASN 13 ASP 14 ALA 15 THR 16 CYS 17 LEU 18 ASP 19 GLN 20 ILE 21 GLY 22 GLU 23 PHE 24 GLN 25 CYS 26 ILE 27 CYS 28 MET 29 PRO 30 GLY 31 TYR 32 GLU 33 GLY 34 VAL 35 TYR 36 CYS 37 GLU 38 ILE_NH2 stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date 2014-11-10 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 17527 NEUROGENIC_LOCUS_NOTCH_HOMOLOG_PROTEIN_1_EGF12_domain 97.37 38 100.00 100.00 2.98e-17 BMRB 17528 NEUROGENIC_LOCUS_NOTCH_HOMOLOG_PROTEIN_1_EGF12_domain 97.37 38 100.00 100.00 2.98e-17 PDB 2RQZ "Structure Of Sugar Modified Epidermal Growth Factor-Like Repeat 12 Of Mouse Notch-1 Receptor" 97.37 38 100.00 100.00 2.98e-17 PDB 2RR0 "Structure Of Epidermal Growth Factor-Like Repeat 12 Of Mouse Notch-1 Receptor" 97.37 38 100.00 100.00 2.98e-17 PDB 2RR2 "Structure Of O-Fucosylated Epidermal Growth Factor-Like Repeat 12 Of Mouse Notch-1 Receptor" 97.37 38 100.00 100.00 2.98e-17 stop_ save_ save_disaccharide _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class carbohydrate _Name_common disaccharide _Molecular_mass . _Mol_thiol_state 'not present' _Details . _Residue_count 2 _Mol_residue_sequence XX loop_ _Residue_seq_code _Residue_label 1 FUC 2 NAG stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ###################### # Polymer residues # ###################### save_chem_comp_ILE_NH2 _Saveframe_category polymer_residue _Mol_type 'L-peptide linking' _Name_common 'L-ISOLEUCINAMIDE AMIDE' _Abbreviation_common ILE _BMRB_code ILE_NH2 _PDB_code . _Standard_residue_derivative ILE _Molecular_mass 129.180 _Mol_paramagnetic no _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons N N N . 0 . ? NT NT N . 0 . ? CA CA C . 0 . ? C C C . 0 . ? O O O . 0 . ? CB CB C . 0 . ? CG1 CG1 C . 0 . ? CG2 CG2 C . 0 . ? CD1 CD1 C . 0 . ? H H H . 0 . ? HA HA H . 0 . ? HB HB H . 0 . ? HG12 HG12 H . 0 . ? HG13 HG13 H . 0 . ? HG21 HG21 H . 0 . ? HG22 HG22 H . 0 . ? HG23 HG23 H . 0 . ? HD11 HD11 H . 0 . ? HD12 HD12 H . 0 . ? HD13 HD13 H . 0 . ? HT1 HT1 H . 0 . ? HT2 HT2 H . 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 CA C ? ? SING CA CB ? ? SING CA HA ? ? DOUB C O ? ? SING CB CG1 ? ? SING CB CG2 ? ? SING CB HB ? ? SING CG1 CD1 ? ? SING CG1 HG12 ? ? SING CG1 HG13 ? ? SING CG2 HG21 ? ? SING CG2 HG22 ? ? SING CG2 HG23 ? ? SING CD1 HD11 ? ? SING CD1 HD12 ? ? SING CD1 HD13 ? ? SING C N2 ? ? SING NT HT1 ? ? SING NT HT2 ? ? stop_ save_ save_chem_comp_FUC _Saveframe_category polymer_residue _Mol_type saccharide _Name_common ALPHA-L-FUCOSE _BMRB_code . _PDB_code FUC _Standard_residue_derivative . _Molecular_mass 164.156 _Mol_paramagnetic . _Details ; Information obtained from PDB's Chemical Component Dictionary at http://wwpdb-remediation.rutgers.edu/downloads.html Downloaded on Tue Jun 9 14:11:51 2009 ; loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons C1 C1 C . 0 . ? C2 C2 C . 0 . ? C3 C3 C . 0 . ? C4 C4 C . 0 . ? C5 C5 C . 0 . ? C6 C6 C . 0 . ? O1 O1 O . 0 . ? O2 O2 O . 0 . ? O3 O3 O . 0 . ? O4 O4 O . 0 . ? O5 O5 O . 0 . ? H1 H1 H . 0 . ? H2 H2 H . 0 . ? H3 H3 H . 0 . ? H4 H4 H . 0 . ? H5 H5 H . 0 . ? H61 H61 H . 0 . ? H62 H62 H . 0 . ? H63 H63 H . 0 . ? HO1 HO1 H . 0 . ? HO2 HO2 H . 0 . ? HO3 HO3 H . 0 . ? HO4 HO4 H . 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 C1 C2 ? ? SING C1 O1 ? ? SING C1 O5 ? ? SING C1 H1 ? ? SING C2 C3 ? ? SING C2 O2 ? ? SING C2 H2 ? ? SING C3 C4 ? ? SING C3 O3 ? ? SING C3 H3 ? ? SING C4 C5 ? ? SING C4 O4 ? ? SING C4 H4 ? ? SING C5 C6 ? ? SING C5 O5 ? ? SING C5 H5 ? ? SING C6 H61 ? ? SING C6 H62 ? ? SING C6 H63 ? ? SING O1 HO1 ? ? SING O2 HO2 ? ? SING O3 HO3 ? ? SING O4 HO4 ? ? stop_ save_ save_chem_comp_NAG _Saveframe_category polymer_residue _Mol_type D-saccharide _Name_common N-ACETYL-D-GLUCOSAMINE _BMRB_code . _PDB_code NAG _Standard_residue_derivative . _Molecular_mass 221.208 _Mol_paramagnetic . _Details ; Information obtained from PDB's Chemical Component Dictionary at http://wwpdb-remediation.rutgers.edu/downloads.html Downloaded on Tue Jun 9 15:20:37 2009 ; loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons C1 C1 C . 0 . ? C2 C2 C . 0 . ? C3 C3 C . 0 . ? C4 C4 C . 0 . ? C5 C5 C . 0 . ? C6 C6 C . 0 . ? C7 C7 C . 0 . ? C8 C8 C . 0 . ? N2 N2 N . 0 . ? O1 O1 O . 0 . ? O3 O3 O . 0 . ? O4 O4 O . 0 . ? O5 O5 O . 0 . ? O6 O6 O . 0 . ? O7 O7 O . 0 . ? H1 H1 H . 0 . ? H2 H2 H . 0 . ? H3 H3 H . 0 . ? H4 H4 H . 0 . ? H5 H5 H . 0 . ? H61 H61 H . 0 . ? H62 H62 H . 0 . ? H81 H81 H . 0 . ? H82 H82 H . 0 . ? H83 H83 H . 0 . ? HN2 HN2 H . 0 . ? HO1 HO1 H . 0 . ? HO3 HO3 H . 0 . ? HO4 HO4 H . 0 . ? HO6 HO6 H . 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 C1 C2 ? ? SING C1 O1 ? ? SING C1 O5 ? ? SING C1 H1 ? ? SING C2 C3 ? ? SING C2 N2 ? ? SING C2 H2 ? ? SING C3 C4 ? ? SING C3 O3 ? ? SING C3 H3 ? ? SING C4 C5 ? ? SING C4 O4 ? ? SING C4 H4 ? ? SING C5 C6 ? ? SING C5 O5 ? ? SING C5 H5 ? ? SING C6 O6 ? ? SING C6 H61 ? ? SING C6 H62 ? ? SING C7 C8 ? ? SING C7 N2 ? ? DOUB C7 O7 ? ? SING C8 H81 ? ? SING C8 H82 ? ? SING C8 H83 ? ? SING N2 HN2 ? ? SING O1 HO1 ? ? SING O3 HO3 ? ? SING O4 HO4 ? ? SING O6 HO6 ? ? stop_ save_ ######################################## # Molecular bond linkage definitions # ######################################## save_crosslink_bonds _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 'EGF12 peptide' 5 CYS SG 'EGF12 peptide' 16 CYS SG single disulfide 'EGF12 peptide' 10 CYS SG 'EGF12 peptide' 25 CYS SG single disulfide 'EGF12 peptide' 27 CYS SG 'EGF12 peptide' 36 CYS SG single coordination 'EGF12 peptide' 15 THR OG1 'NAG b1-3 FUC' 1 FUC C1 single coordination 'NAG b1-3 FUC' 1 FUC O3 'NAG b1-3 FUC' 2 NAG C1 stop_ loop_ _Deleted_atom_mol_system_component_name _Deleted_atom_residue_seq_code _Deleted_atom_residue_label _Deleted_atom_name 'EGF12 peptide' 5 CYS HG 'EGF12 peptide' 10 CYS HG 'EGF12 peptide' 15 THR HG1 'EGF12 peptide' 16 CYS HG 'EGF12 peptide' 25 CYS HG 'EGF12 peptide' 27 CYS HG 'EGF12 peptide' 36 CYS HG 'NAG b1-3 FUC' 1 FUC HO1,O1 'NAG b1-3 FUC' 1 FUC HO3 'NAG b1-3 FUC' 2 NAG HO1 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 _Details $mouse_NOTCH-1_EGF12 'house mouse' 10090 Eukaryota Metazoa Mus musculus BALB/c NP_032740 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 _Details $mouse_NOTCH-1_EGF12 'chemical synthesis' . . . . . 'Details are included in the publication.' stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details 'This sample is a glycopeptide.' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $mouse_NOTCH-1_EGF12 0.55 mM 'natural abundance' $disaccharide 0.55 mM 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_NMRPipe _Saveframe_category software _Name NMRPipe _Version 2.4 loop_ _Vendor _Address _Electronic_address 'Delaglio, Grzesiek, Vuister, Zhu, Pfeifer and Bax' . . stop_ loop_ _Task processing stop_ _Details ; I used NMRPipe software for data processing then used SPARKY software to assign the chemical shift. ; save_ save_SPARKY _Saveframe_category software _Name SPARKY _Version 3.110 loop_ _Vendor _Address _Electronic_address Goddard . . stop_ loop_ _Task 'chemical shift assignment' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 600 _Details 'with cryo probe' save_ ############################# # NMR applied experiments # ############################# save_2D_DQF-COSY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D DQF-COSY' _Sample_label $sample_1 save_ save_2D_1H-1H_TOCSY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample_1 save_ save_2D_1H-1H_NOESY_3 _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 300 . K pH 5.3 . pH pressure 1 . atm 'ionic strength' 0 . M stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chemical_shift_reference_1 _Saveframe_category chemical_shift_reference _Details ; Digital lock system by Brucker instrument was used to set chemical shift reference. The DHO signal showed 4.704 ppm at 300K. ; 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 TMS H 1 'methyl protons' ppm 0 external indirect . 'separate tube (no insert) similar to the experimental sample tube' . 1.0 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_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $SPARKY stop_ loop_ _Experiment_label '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 'EGF12 peptide' _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 ASP HA H 4.198 0.002 1 2 1 1 ASP HB2 H 2.736 0.001 2 3 1 1 ASP HB3 H 2.585 0 2 4 2 2 VAL H H 8.543 0.002 1 5 2 2 VAL HA H 4.054 0.002 1 6 2 2 VAL HB H 1.983 0.002 1 7 2 2 VAL HG1 H 0.823 0.001 1 8 2 2 VAL HG2 H 0.823 0.001 1 9 3 3 ASN H H 8.448 0.004 1 10 3 3 ASN HA H 4.665 0.001 1 11 3 3 ASN HB2 H 2.682 0.004 1 12 3 3 ASN HB3 H 2.682 0.004 1 13 3 3 ASN HD21 H 6.836 0.001 2 14 3 3 ASN HD22 H 7.507 0.003 2 15 4 4 GLU H H 8.501 0.003 1 16 4 4 GLU HA H 4.221 0.002 1 17 4 4 GLU HB2 H 1.985 0.002 2 18 4 4 GLU HB3 H 1.811 0.004 2 19 4 4 GLU HG2 H 2.285 0.002 2 20 4 4 GLU HG3 H 2.237 0.003 2 21 5 5 CYS H H 8.695 0.001 1 22 5 5 CYS HA H 4.247 0.005 1 23 5 5 CYS HB2 H 3.133 0.002 2 24 5 5 CYS HB3 H 2.852 0.003 2 25 6 6 ILE H H 7.817 0.002 1 26 6 6 ILE HA H 3.84 0.002 1 27 6 6 ILE HB H 1.786 0.002 1 28 6 6 ILE HG12 H 1.401 0.003 2 29 6 6 ILE HG13 H 1.183 0.002 2 30 6 6 ILE HG2 H 0.823 0.002 1 31 6 6 ILE HD1 H 0.787 0 1 32 7 7 SER H H 7.537 0.003 1 33 7 7 SER HA H 4.312 0.002 1 34 7 7 SER HB2 H 3.663 0.002 1 35 7 7 SER HB3 H 3.663 0.002 1 36 8 8 ASN H H 7.978 0.001 1 37 8 8 ASN HA H 4.584 0.002 1 38 8 8 ASN HB2 H 2.851 0.038 2 39 8 8 ASN HB3 H 2.715 0.003 2 40 8 8 ASN HD21 H 6.553 0.002 2 41 8 8 ASN HD22 H 7.338 0.003 2 42 9 9 PRO HA H 4.298 0.003 1 43 9 9 PRO HB2 H 1.732 0.003 2 44 9 9 PRO HB3 H 1.585 0.002 2 45 9 9 PRO HG2 H 1.489 0.004 2 46 9 9 PRO HG3 H 1.157 0.003 2 47 9 9 PRO HD2 H 3.636 0.005 2 48 9 9 PRO HD3 H 3.544 0.002 2 49 10 10 CYS H H 8.042 0.002 1 50 10 10 CYS HA H 4.54 0.003 1 51 10 10 CYS HB2 H 2.724 0.002 2 52 10 10 CYS HB3 H 2.562 0.004 2 53 11 11 GLN H H 8.811 0.003 1 54 11 11 GLN HA H 4.276 0.002 1 55 11 11 GLN HB2 H 2.035 0.003 2 56 11 11 GLN HB3 H 1.583 0.003 2 57 11 11 GLN HG2 H 2.277 0.001 1 58 11 11 GLN HG3 H 2.277 0.001 1 59 11 11 GLN HE21 H 6.701 0.001 2 60 11 11 GLN HE22 H 7.017 0.001 2 61 12 12 ASN H H 8.774 0.002 1 62 12 12 ASN HA H 3.922 0.001 1 63 12 12 ASN HB2 H 2.036 0.002 2 64 12 12 ASN HB3 H 1.33 0.002 2 65 12 12 ASN HD21 H 7.27 0.001 2 66 12 12 ASN HD22 H 8.207 0.001 2 67 13 13 ASP H H 8.574 0.002 1 68 13 13 ASP HA H 4.009 0.002 1 69 13 13 ASP HB2 H 2.93 0.003 2 70 13 13 ASP HB3 H 2.729 0.002 2 71 14 14 ALA H H 6.655 0.002 1 72 14 14 ALA HA H 4.256 0.001 1 73 14 14 ALA HB H 1.291 0.003 1 74 15 15 THR H H 8.422 0.002 1 75 15 15 THR HA H 4.353 0.002 1 76 15 15 THR HB H 3.818 0.003 1 77 15 15 THR HG2 H 1.026 0.002 1 78 16 16 CYS H H 8.986 0.003 1 79 16 16 CYS HA H 5.178 0.005 1 80 16 16 CYS HB2 H 3.032 0.004 2 81 16 16 CYS HB3 H 2.835 0.002 2 82 17 17 LEU H H 9.324 0.005 1 83 17 17 LEU HA H 4.67 0.002 1 84 17 17 LEU HB2 H 1.507 0.003 1 85 17 17 LEU HB3 H 1.507 0.003 1 86 17 17 LEU HG H 1.413 0.004 1 87 17 17 LEU HD1 H 0.792 0.001 2 88 17 17 LEU HD2 H 0.754 0.001 2 89 18 18 ASP H H 8.522 0.002 1 90 18 18 ASP HA H 4.763 0.001 1 91 18 18 ASP HB2 H 2.673 0.003 2 92 18 18 ASP HB3 H 2.537 0.004 2 93 19 19 GLN H H 8.256 0.002 1 94 19 19 GLN HA H 4.494 0 1 95 19 19 GLN HB2 H 1.746 0.003 1 96 19 19 GLN HB3 H 1.746 0.003 1 97 19 19 GLN HG2 H 2.159 0.003 2 98 19 19 GLN HG3 H 2.025 0.003 2 99 19 19 GLN HE21 H 6.674 0.001 2 100 19 19 GLN HE22 H 7.214 0.003 2 101 20 20 ILE H H 8.449 0.002 1 102 20 20 ILE HA H 3.819 0.002 1 103 20 20 ILE HB H 2.032 0.003 1 104 20 20 ILE HG12 H 1.379 0.003 2 105 20 20 ILE HG13 H 1.011 0.003 2 106 20 20 ILE HG2 H 0.809 0.003 1 107 20 20 ILE HD1 H 0.752 0.003 1 108 21 21 GLY H H 8.527 0.001 1 109 21 21 GLY HA2 H 4.05 0.003 2 110 21 21 GLY HA3 H 3.659 0.001 2 111 22 22 GLU H H 7.536 0.004 1 112 22 22 GLU HA H 4.528 0.008 1 113 22 22 GLU HB2 H 2.124 0.001 2 114 22 22 GLU HB3 H 1.976 0.005 2 115 22 22 GLU HG2 H 1.773 0.006 1 116 22 22 GLU HG3 H 1.773 0.006 1 117 23 23 PHE H H 7.85 0.002 1 118 23 23 PHE HA H 5.225 0.002 1 119 23 23 PHE HB2 H 3.018 0.002 2 120 23 23 PHE HB3 H 2.868 0.034 2 121 23 23 PHE HD1 H 7.152 0.003 1 122 23 23 PHE HD2 H 7.152 0.003 1 123 23 23 PHE HE1 H 6.998 0.003 1 124 23 23 PHE HE2 H 6.998 0.003 1 125 23 23 PHE HZ H 7.097 0.003 1 126 24 24 GLN H H 8.696 0.002 1 127 24 24 GLN HA H 4.289 0.003 1 128 24 24 GLN HB2 H 1.87 0.003 2 129 24 24 GLN HB3 H 1.795 0.001 2 130 24 24 GLN HG2 H 2.094 0.003 1 131 24 24 GLN HG3 H 2.094 0.003 1 132 24 24 GLN HE21 H 6.568 0.002 2 133 24 24 GLN HE22 H 7.279 0.001 2 134 25 25 CYS H H 8.961 0.003 1 135 25 25 CYS HA H 5.387 0.003 1 136 25 25 CYS HB2 H 2.98 0.002 2 137 25 25 CYS HB3 H 2.58 0.002 2 138 26 26 ILE H H 9.514 0.003 1 139 26 26 ILE HA H 4.163 0.003 1 140 26 26 ILE HB H 1.862 0.003 1 141 26 26 ILE HG12 H 1.327 0.003 2 142 26 26 ILE HG13 H 1.163 0.003 2 143 26 26 ILE HG2 H 0.832 0.003 1 144 26 26 ILE HD1 H 0.658 0.002 1 145 27 27 CYS H H 8.366 0.001 1 146 27 27 CYS HA H 4.659 0.001 1 147 27 27 CYS HB2 H 3.346 0.002 2 148 27 27 CYS HB3 H 2.505 0.003 2 149 28 28 MET H H 8.575 0.002 1 150 28 28 MET HA H 4.533 0.042 1 151 28 28 MET HB2 H 1.923 0.002 2 152 28 28 MET HB3 H 2.204 0.002 2 153 28 28 MET HG2 H 2.69 0.003 2 154 28 28 MET HG3 H 2.346 0.003 2 155 28 28 MET HE H 2.121 0.004 1 156 29 29 PRO HA H 4.262 0.002 1 157 29 29 PRO HB2 H 2.232 0.002 2 158 29 29 PRO HB3 H 2.088 0.001 2 159 29 29 PRO HG2 H 1.981 0.001 2 160 29 29 PRO HG3 H 1.77 0.002 2 161 29 29 PRO HD2 H 3.908 0.003 2 162 29 29 PRO HD3 H 3.594 0.003 2 163 30 30 GLY H H 8.527 0.002 1 164 30 30 GLY HA2 H 3.982 0.003 2 165 30 30 GLY HA3 H 3.371 0.009 2 166 31 31 TYR H H 7.608 0.002 1 167 31 31 TYR HA H 5.064 0.003 1 168 31 31 TYR HB2 H 2.837 0.002 2 169 31 31 TYR HB3 H 2.792 0.003 2 170 31 31 TYR HD1 H 6.837 0.002 1 171 31 31 TYR HD2 H 6.837 0.002 1 172 31 31 TYR HE1 H 6.609 0.003 1 173 31 31 TYR HE2 H 6.609 0.003 1 174 32 32 GLU H H 9.035 0.003 1 175 32 32 GLU HA H 4.811 0.002 1 176 32 32 GLU HB2 H 2.102 0.006 2 177 32 32 GLU HB3 H 2.057 0.007 2 178 32 32 GLU HG2 H 1.877 0.003 1 179 32 32 GLU HG3 H 1.877 0.003 1 180 33 33 GLY H H 8.094 0.053 1 181 33 33 GLY HA2 H 4.846 0.004 2 182 33 33 GLY HA3 H 3.741 0.002 2 183 34 34 VAL H H 9.384 0.001 1 184 34 34 VAL HA H 3.423 0.002 1 185 34 34 VAL HB H 1.525 0.002 1 186 34 34 VAL HG1 H 0.241 0.002 2 187 34 34 VAL HG2 H 0.794 0.001 2 188 35 35 TYR H H 8.462 0.002 1 189 35 35 TYR HA H 5.226 0.003 1 190 35 35 TYR HB2 H 3.645 0.003 2 191 35 35 TYR HB3 H 2.649 0.002 2 192 35 35 TYR HD1 H 6.9 0.002 1 193 35 35 TYR HD2 H 6.9 0.002 1 194 35 35 TYR HE1 H 6.68 0.004 1 195 35 35 TYR HE2 H 6.68 0.004 1 196 36 36 CYS H H 7.873 0.039 1 197 36 36 CYS HA H 3.861 0.002 1 198 36 36 CYS HB2 H 3.215 0.002 2 199 36 36 CYS HB3 H 2.888 0.001 2 200 37 37 GLU HA H 3.968 0.002 1 201 37 37 GLU HB2 H 2.104 0.002 2 202 37 37 GLU HB3 H 1.791 0.002 2 203 37 37 GLU HG2 H 2.527 0.002 2 204 37 37 GLU HG3 H 2.199 0.003 2 205 38 38 ILE_NH2 H H 8.821 0.005 1 206 38 38 ILE_NH2 HA H 4.143 0.002 1 207 38 38 ILE_NH2 HB H 1.575 0.003 1 208 38 38 ILE_NH2 HG12 H 1.439 0.002 1 209 38 38 ILE_NH2 HG13 H 1.439 0.002 1 210 38 38 ILE_NH2 HG21 H 0.955 0.002 1 211 38 38 ILE_NH2 HG22 H 0.955 0.002 1 212 38 38 ILE_NH2 HG23 H 0.955 0.002 1 213 38 38 ILE_NH2 HD11 H 0.79 0.006 1 214 38 38 ILE_NH2 HD12 H 0.79 0.006 1 215 38 38 ILE_NH2 HD13 H 0.79 0.006 1 216 38 38 ILE_NH2 HT1 H 7.152 0.001 2 217 38 38 ILE_NH2 HT2 H 7.733 0.002 2 stop_ save_ save_assigned_chem_shift_list_1_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $SPARKY stop_ loop_ _Experiment_label '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 'NAG b1-3 FUC' _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 FUC H1 H 4.825 0.002 1 2 1 1 FUC H2 H 3.753 0.002 1 3 1 1 FUC H3 H 3.826 0.003 1 4 1 1 FUC H4 H 3.923 0.002 1 5 1 1 FUC H5 H 4.144 0.003 1 6 1 1 FUC H6 H 1.033 0.002 1 7 2 2 NAG H1 H 4.565 0.002 1 8 2 2 NAG H2 H 3.632 0.004 1 9 2 2 NAG H3 H 3.47 0.002 1 10 2 2 NAG H4 H 3.31 0.002 1 11 2 2 NAG H5 H 3.806 0.002 1 12 2 2 NAG H61 H 3.805 0 2 13 2 2 NAG H62 H 3.614 0.003 2 14 2 2 NAG H8 H 1.984 0.001 1 15 2 2 NAG NH2 H 8.189 0.003 1 stop_ save_