data_18897 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; NMR structure of the glycosylated conotoxin CcTx from Conus consors ; _BMRB_accession_number 18897 _BMRB_flat_file_name bmr18897.str _Entry_type original _Submission_date 2012-12-13 _Accession_date 2012-12-13 _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 Hocking Henry G. . 2 Gerwig G. J. . 3 Favreau P. . . 4 Stocklin R. . . 5 Kamerling J. P. . 6 Boelens R. . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 2 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 199 "13C chemical shifts" 126 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2013-01-29 original author . stop_ _Original_release_date 2013-01-29 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title 'Structure of the O-Glycosylated Conopeptide CcTx from Conus consors Venom.' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 23281027 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Hocking Henry G. . 2 Gerwig Gerrit J. . 3 Dutertre Sebastien . . 4 Violette Aude . . 5 Favreau Philipe . . 6 Stocklin Reto . . 7 Kamerling Johannis P. . 8 Boelens Rolf . . stop_ _Journal_abbreviation Chemistry _Journal_name_full 'Chemistry (Weinheim an der Bergstrasse, Germany)' _Journal_volume 19 _Journal_issue 3 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 870 _Page_last 879 _Year 2013 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'NMR structure of the glycosylated conotoxin CcTx from Conus consors' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label polysaccharide $polysaccharide 'CONOTOXIN CCTX' $CONOTOXIN_CCTX stop_ _System_molecular_weight 4206.561 _System_physical_state native _System_oligomer_state ? _System_paramagnetic no _System_thiol_state 'all disulfide bound' _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_polysaccharide _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class carbohydrate _Name_common polysaccharide _Molecular_mass . _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 5 _Mol_residue_sequence XXXXX loop_ _Residue_seq_code _Residue_label 1 A2G 2 NDG 3 GXL 4 GAL 5 GXL stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ save_CONOTOXIN_CCTX _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common CONOTOXIN_CCTX _Molecular_mass 3223.6702 _Mol_thiol_state 'all disulfide bound' _Details . _Residue_count 30 _Mol_residue_sequence ; AXWLVPSQITTCCGYNXGTM CXSCMCTNTC ; loop_ _Residue_seq_code _Residue_label 1 ALA 2 HYP 3 TRP 4 LEU 5 VAL 6 PRO 7 SER 8 GLN 9 ILE 10 THR 11 THR 12 CYS 13 CYS 14 GLY 15 TYR 16 ASN 17 HYP 18 GLY 19 THR 20 MET 21 CYS 22 HYP 23 SER 24 CYS 25 MET 26 CYS 27 THR 28 ASN 29 THR 30 CYS stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date 2014-11-09 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 PDB 4B1Q "Nmr Structure Of The Glycosylated Conotoxin Cctx From Conus Consors" 93.33 30 100.00 100.00 4.74e-08 stop_ save_ ###################### # Polymer residues # ###################### save_chem_comp_A2G _Saveframe_category polymer_residue _Mol_type SACCHARIDE _Name_common N-ACETYL-2-DEOXY-2-AMINO-GALACTOSE _BMRB_code A2G _PDB_code A2G _Standard_residue_derivative . _Molecular_mass 221.208 _Mol_paramagnetic . _Details . 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 . ? H1 H1 H . 0 . ? H14 H14 H . 0 . ? H15 H15 H . 0 . ? H2 H2 H . 0 . ? H3 H3 H . 0 . ? H4 H4 H . 0 . ? H5 H5 H . 0 . ? H6 H6 H . 0 . ? H8 H8 H . 0 . ? H8A H8A H . 0 . ? H8B H8B H . 0 . ? HN2 HN2 H . 0 . ? HO1 HO1 H . 0 . ? HO3 HO3 H . 0 . ? HO4 HO4 H . 0 . ? N2 N2 N . 0 . ? O O O . 0 . ? O1 O1 O . 0 . ? O3 O3 O . 0 . ? O4 O4 O . 0 . ? O6 O6 O . 0 . ? O7 O7 O . 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 O C5 ? ? SING C1 O ? ? SING C1 C2 ? ? SING C1 H1 ? ? SING O1 C1 ? ? SING O1 HO1 ? ? SING C2 C3 ? ? SING C2 H2 ? ? SING N2 C2 ? ? SING N2 HN2 ? ? SING C3 C4 ? ? SING C3 O3 ? ? SING C3 H3 ? ? SING O3 HO3 ? ? SING C4 O4 ? ? SING C4 H4 ? ? SING O4 HO4 ? ? SING C5 C4 ? ? SING C5 C6 ? ? SING C5 H5 ? ? SING C6 O6 ? ? SING C6 H6 ? ? SING C7 N2 ? ? DOUB O7 C7 ? ? SING C8 C7 ? ? SING C8 H8 ? ? SING C8 H8A ? ? SING C8 H8B ? ? SING C6 H14 ? ? SING O6 H15 ? ? stop_ save_ save_chem_comp_NDG _Saveframe_category polymer_residue _Mol_type D-SACCHARIDE _Name_common 2-(ACETYLAMINO)-2-DEOXY-A-D-GLUCOPYRANOSE _BMRB_code NDG _PDB_code NDG _Standard_residue_derivative . _Molecular_mass 221.208 _Mol_paramagnetic . _Details . 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 . ? H1 H1 H . 0 . ? H1L H1L H . 0 . ? H2 H2 H . 0 . ? H3 H3 H . 0 . ? H4 H4 H . 0 . ? H5 H5 H . 0 . ? H6 H6 H . 0 . ? H6C1 H6C1 H . 0 . ? H6C2 H6C2 H . 0 . ? H8C1 H8C1 H . 0 . ? H8C2 H8C2 H . 0 . ? H8C3 H8C3 H . 0 . ? HA HA H . 0 . ? HB HB H . 0 . ? HC HC H . 0 . ? N2 N2 N . 0 . ? O O O . 0 . ? O1L O1L O . 0 . ? O3 O3 O . 0 . ? O4 O4 O . 0 . ? O6 O6 O . 0 . ? O7 O7 O . 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 O ? ? SING C1 O1L ? ? 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 O ? ? SING C5 H5 ? ? SING C6 O6 ? ? SING C6 H6C1 ? ? SING C6 H6C2 ? ? SING C7 C8 ? ? DOUB C7 O7 ? ? SING C7 N2 ? ? SING C8 H8C1 ? ? SING C8 H8C2 ? ? SING C8 H8C3 ? ? SING O3 HB ? ? SING O4 HC ? ? SING O6 H6 ? ? SING N2 HA ? ? SING O1L H1L ? ? stop_ save_ save_chem_comp_GXL _Saveframe_category polymer_residue _Mol_type NON-POLYMER _Name_common ALPHA-L-GALACTOPYRANOSE _BMRB_code GXL _PDB_code GXL _Standard_residue_derivative . _Molecular_mass 180.156 _Mol_paramagnetic . _Details . 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 . ? H1 H1 H . 0 . ? H2 H2 H . 0 . ? H3 H3 H . 0 . ? H4 H4 H . 0 . ? H5 H5 H . 0 . ? H6 H6 H . 0 . ? H6C1 H6C1 H . 0 . ? H6C2 H6C2 H . 0 . ? HA HA H . 0 . ? HB HB H . 0 . ? HC HC H . 0 . ? HD HD H . 0 . ? O1 O1 O . 0 . ? O2 O2 O . 0 . ? O3 O3 O . 0 . ? O4 O4 O . 0 . ? O5 O5 O . 0 . ? O6 O6 O . 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 HA ? ? 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 H6C1 ? ? SING C6 H6C2 ? ? SING O1 HB ? ? SING O2 H2 ? ? SING O3 HC ? ? SING O4 HD ? ? SING O6 H6 ? ? stop_ save_ save_chem_comp_GAL _Saveframe_category polymer_residue _Mol_type D-SACCHARIDE _Name_common BETA-D-GALACTOSE _BMRB_code GAL _PDB_code GAL _Standard_residue_derivative . _Molecular_mass 180.156 _Mol_paramagnetic . _Details . 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 . ? 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 . ? HO1 HO1 H . 0 . ? HO2 HO2 H . 0 . ? HO3 HO3 H . 0 . ? HO4 HO4 H . 0 . ? HO6 HO6 H . 0 . ? O1 O1 O . 0 . ? O2 O2 O . 0 . ? O3 O3 O . 0 . ? O4 O4 O . 0 . ? O5 O5 O . 0 . ? O6 O6 O . 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 O6 ? ? SING C6 H61 ? ? SING C6 H62 ? ? SING O1 HO1 ? ? SING O2 HO2 ? ? SING O3 HO3 ? ? SING O4 HO4 ? ? SING O6 HO6 ? ? stop_ save_ save_chem_comp_HYP _Saveframe_category polymer_residue _Mol_type 'L-PEPTIDE LINKING' _Name_common 4-HYDROXYPROLINE _BMRB_code HYP _PDB_code HYP _Standard_residue_derivative . _Molecular_mass 131.130 _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 . ? CD CD C . 0 . ? CG CG C . 0 . ? H H H . 0 . ? HA HA H . 0 . ? HB2 HB2 H . 0 . ? HB3 HB3 H . 0 . ? HD1 HD1 H . 0 . ? HD22 HD22 H . 0 . ? HD23 HD23 H . 0 . ? HG HG H . 0 . ? HXT HXT H . 0 . ? N N N . 0 . ? O O O . 0 . ? OD1 OD1 O . 0 . ? OXT OXT O . 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 CD ? ? SING N H ? ? SING CA C ? ? SING CA CB ? ? SING CA HA ? ? DOUB C O ? ? SING C OXT ? ? SING CB CG ? ? SING CB HB2 ? ? SING CB HB3 ? ? SING CG CD ? ? SING CG OD1 ? ? SING CG HG ? ? SING CD HD22 ? ? SING CD HD23 ? ? SING OD1 HD1 ? ? SING OXT HXT ? ? 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 'CONOTOXIN CCTX' 13 CYS SG 'CONOTOXIN CCTX' 26 CYS SG single disulfide 'CONOTOXIN CCTX' 12 CYS SG 'CONOTOXIN CCTX' 21 CYS SG single disulfide 'CONOTOXIN CCTX' 24 CYS SG 'CONOTOXIN CCTX' 30 CYS SG stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $CONOTOXIN_CCTX 'Conus consors' 101297 Eukaryota Metazoa Conus consors 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 $CONOTOXIN_CCTX 'purified from the natural source' . . . . . 'Isolated from milked venom' stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details '1.1 mmol/l' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $polysaccharide 1.1 mM '[U-13C; U-15N]' $CONOTOXIN_CCTX 1.1 mM '[U-13C; U-15N]' stop_ save_ ############################ # Computer software used # ############################ save_AutoDep _Saveframe_category software _Name AutoDep _Version 4.3 loop_ _Vendor _Address _Electronic_address PDBe . . stop_ loop_ _Task collection stop_ _Details . save_ save_CCPN_Analysis _Saveframe_category software _Name CCPN_Analysis _Version any loop_ _Vendor _Address _Electronic_address CCPN . . stop_ loop_ _Task 'chemical shift assignment' stop_ _Details . save_ save_CNS _Saveframe_category software _Name CNS _Version any loop_ _Vendor _Address _Electronic_address BRUNGER,ADAMS,CLORE,DELANO,GROS,GROSSE- . . stop_ loop_ _Task 'data analysis' stop_ _Details 'Refinement in explicit water solvent' save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_Bruker_Avance-750 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 750 _Details . save_ ############################# # NMR applied experiments # ############################# save_NOESY_1 _Saveframe_category NMR_applied_experiment _Experiment_name NOESY _Sample_label $sample_1 save_ save_TOCSY_2 _Saveframe_category NMR_applied_experiment _Experiment_name TOCSY _Sample_label $sample_1 save_ save_COSY_3 _Saveframe_category NMR_applied_experiment _Experiment_name COSY _Sample_label $sample_1 save_ save_H2BC_4 _Saveframe_category NMR_applied_experiment _Experiment_name H2BC _Sample_label $sample_1 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 'pH [3.0], temp [292], pressure [0.0], ionStrength [0.0]' loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 0.0 . mM pH 3.000 . pH pressure 1 . atm temperature 292.000 . K 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 0.0 internal indirect . . . 1 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 'Origin nmrStar file /ebi/msd/pdb_root/Processing/prepare/4b1q/ebi/cctxApeptide.bmrb.csh' loop_ _Experiment_label NOESY TOCSY COSY H2BC 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 'CONOTOXIN CCTX' _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 ALA HA H 4.358 . 1 2 1 1 ALA HB H 1.430 0.007 1 3 1 1 ALA CA C 50.640 . 1 4 1 1 ALA CB C 17.385 . 1 5 2 2 HYP HA H 4.599 . 1 6 2 2 HYP HB2 H 2.338 0.002 2 7 2 2 HYP HB3 H 1.933 0.002 2 8 2 2 HYP HG H 4.568 . 1 9 2 2 HYP HD22 H 3.668 . 1 10 2 2 HYP HD23 H 3.668 . 1 11 2 2 HYP CA C 61.534 . 1 12 2 2 HYP CB C 39.630 0.055 1 13 2 2 HYP CG C 72.431 . 1 14 2 2 HYP CD C 57.688 . 1 15 3 3 TRP H H 8.395 0.001 1 16 3 3 TRP HA H 4.677 0.004 1 17 3 3 TRP HB2 H 3.263 0.002 1 18 3 3 TRP HB3 H 3.263 0.002 1 19 3 3 TRP HD1 H 7.246 0.002 1 20 3 3 TRP HE1 H 10.187 . 1 21 3 3 TRP HE3 H 7.668 0.005 1 22 3 3 TRP HZ2 H 7.492 0.004 1 23 3 3 TRP HZ3 H 7.166 0.005 1 24 3 3 TRP HH2 H 7.245 . 1 25 3 3 TRP CA C 56.848 . 1 26 3 3 TRP CB C 29.315 . 1 27 3 3 TRP CG C 111.038 . 1 28 3 3 TRP CD1 C 126.864 . 1 29 3 3 TRP CD2 C 129.435 . 1 30 3 3 TRP CE2 C 138.759 . 1 31 3 3 TRP CE3 C 120.908 . 1 32 3 3 TRP CZ2 C 114.513 . 1 33 3 3 TRP CZ3 C 122.039 . 1 34 3 3 TRP CH2 C 124.611 . 1 35 4 4 LEU H H 8.002 0.003 1 36 4 4 LEU HA H 4.301 0.004 1 37 4 4 LEU HB2 H 1.430 0.007 1 38 4 4 LEU HB3 H 1.430 0.007 1 39 4 4 LEU HG H 1.429 0.01 1 40 4 4 LEU HD1 H 0.790 0.002 2 41 4 4 LEU HD2 H 0.842 . 2 42 4 4 LEU CA C 54.380 . 1 43 4 4 LEU CB C 42.364 . 1 44 4 4 LEU CG C 26.711 . 1 45 4 4 LEU CD1 C 23.448 . 1 46 4 4 LEU CD2 C 24.669 . 1 47 5 5 VAL H H 7.957 0.004 1 48 5 5 VAL HA H 4.224 0.004 1 49 5 5 VAL HB H 1.982 0.004 1 50 5 5 VAL HG1 H 0.938 0.002 2 51 5 5 VAL HG2 H 0.869 0.002 2 52 5 5 VAL CA C 59.583 . 1 53 5 5 VAL CB C 32.518 . 1 54 5 5 VAL CG1 C 20.737 . 1 55 5 5 VAL CG2 C 20.334 . 1 56 6 6 PRO HA H 4.418 0.004 1 57 6 6 PRO HB2 H 2.292 0.002 2 58 6 6 PRO HB3 H 1.912 0.005 2 59 6 6 PRO HG2 H 2.021 0.024 2 60 6 6 PRO HG3 H 1.989 0.003 2 61 6 6 PRO HD2 H 3.833 0.005 2 62 6 6 PRO HD3 H 3.685 . 2 63 6 6 PRO CA C 62.736 . 1 64 6 6 PRO CB C 32.141 0.013 1 65 6 6 PRO CG C 27.185 0.027 1 66 6 6 PRO CD C 50.905 0.007 1 67 7 7 SER H H 8.582 0.001 1 68 7 7 SER HA H 4.512 0.003 1 69 7 7 SER HB2 H 3.971 0.002 2 70 7 7 SER HB3 H 3.750 0.004 2 71 7 7 SER CA C 57.064 . 1 72 7 7 SER CB C 69.506 0.018 1 73 8 8 GLN H H 8.327 0.002 1 74 8 8 GLN HA H 4.416 0.005 1 75 8 8 GLN HB2 H 2.061 0.003 2 76 8 8 GLN HB3 H 1.933 0.002 2 77 8 8 GLN HG2 H 2.320 0.002 1 78 8 8 GLN HG3 H 2.320 0.002 1 79 8 8 GLN HE21 H 7.566 . 1 80 8 8 GLN HE22 H 6.915 0.001 1 81 8 8 GLN CA C 55.238 . 1 82 8 8 GLN CB C 30.105 0.018 1 83 8 8 GLN CG C 33.434 . 1 84 9 9 ILE H H 8.362 0.001 1 85 9 9 ILE HA H 4.307 0.001 1 86 9 9 ILE HB H 1.838 0.001 1 87 9 9 ILE HG12 H 1.529 0.002 2 88 9 9 ILE HG13 H 1.208 . 2 89 9 9 ILE HG2 H 0.939 0.001 1 90 9 9 ILE HD1 H 0.864 0.002 1 91 9 9 ILE CA C 60.688 . 1 92 9 9 ILE CB C 38.910 . 1 93 9 9 ILE CG1 C 27.491 0.014 1 94 9 9 ILE CG2 C 17.445 . 1 95 9 9 ILE CD1 C 12.926 . 1 96 10 10 THR H H 8.313 0.003 1 97 10 10 THR HA H 4.573 0.003 1 98 10 10 THR HB H 4.356 0.004 1 99 10 10 THR HG2 H 1.202 0.004 1 100 10 10 THR CA C 61.275 . 1 101 10 10 THR CB C 70.172 . 1 102 10 10 THR CG2 C 20.691 . 1 103 11 11 THR H H 8.144 0.002 1 104 11 11 THR HA H 4.453 0.001 1 105 11 11 THR HB H 3.981 0.004 1 106 11 11 THR HG2 H 0.979 0.003 1 107 11 11 THR CA C 60.840 . 1 108 11 11 THR CB C 71.831 . 1 109 11 11 THR CG2 C 21.435 . 1 110 12 12 CYS H H 8.486 0.001 1 111 12 12 CYS HA H 5.136 0.001 1 112 12 12 CYS HB2 H 2.866 0.004 2 113 12 12 CYS HB3 H 2.591 0.01 2 114 12 12 CYS CA C 53.896 . 1 115 12 12 CYS CB C 39.051 0.004 1 116 13 13 CYS H H 9.263 . 1 117 13 13 CYS HA H 4.357 0.005 1 118 13 13 CYS HB2 H 3.448 0.008 2 119 13 13 CYS HB3 H 3.101 0.003 2 120 13 13 CYS CA C 55.112 . 1 121 13 13 CYS CB C 37.301 0.011 1 122 14 14 GLY H H 7.863 0.003 1 123 14 14 GLY HA2 H 4.057 0.004 2 124 14 14 GLY HA3 H 3.490 0.01 2 125 14 14 GLY CA C 44.650 0.025 1 126 15 15 TYR H H 7.742 0.003 1 127 15 15 TYR HA H 4.727 0.002 1 128 15 15 TYR HB2 H 3.042 0.003 2 129 15 15 TYR HB3 H 2.870 0.004 2 130 15 15 TYR HD1 H 7.095 0.004 3 131 15 15 TYR HD2 H 7.095 0.004 3 132 15 15 TYR HE1 H 6.821 0.005 3 133 15 15 TYR HE2 H 6.821 0.005 3 134 15 15 TYR CA C 56.649 . 1 135 15 15 TYR CB C 40.684 0.003 1 136 15 15 TYR CG C 130.593 . 1 137 15 15 TYR CD1 C 133.483 . 3 138 15 15 TYR CD2 C 133.483 . 3 139 15 15 TYR CE1 C 117.912 . 3 140 15 15 TYR CE2 C 117.912 . 3 141 16 16 ASN H H 9.080 0.001 1 142 16 16 ASN HA H 4.495 0.008 1 143 16 16 ASN HB2 H 2.927 0.006 2 144 16 16 ASN HB3 H 2.669 0.005 2 145 16 16 ASN HD21 H 7.675 . 1 146 16 16 ASN HD22 H 6.981 0.001 1 147 16 16 ASN CA C 52.872 . 1 148 16 16 ASN CB C 37.376 0.034 1 149 17 17 HYP HA H 4.793 . 1 150 17 17 HYP HB2 H 2.200 0.004 2 151 17 17 HYP HB3 H 2.064 0.005 2 152 17 17 HYP HG H 4.626 0.006 1 153 17 17 HYP HD22 H 3.829 0.024 2 154 17 17 HYP HD23 H 3.800 0.001 2 155 17 17 HYP CA C 62.341 . 1 156 17 17 HYP CB C 39.100 0.007 1 157 17 17 HYP CG C 72.221 . 1 158 17 17 HYP CD C 57.689 . 1 159 18 18 GLY H H 9.261 0.002 1 160 18 18 GLY HA2 H 4.362 0.002 2 161 18 18 GLY HA3 H 3.767 0.009 2 162 18 18 GLY CA C 44.683 0.008 1 163 19 19 THR H H 7.824 0.005 1 164 19 19 THR HA H 4.610 0.001 1 165 19 19 THR HB H 4.256 0.007 1 166 19 19 THR HG2 H 1.168 0.001 1 167 19 19 THR CA C 60.827 . 1 168 19 19 THR CB C 71.300 . 1 169 19 19 THR CG2 C 21.021 . 1 170 20 20 MET H H 8.333 0.002 1 171 20 20 MET HA H 4.692 0.002 1 172 20 20 MET HB2 H 2.003 0.001 1 173 20 20 MET HB3 H 2.003 0.001 1 174 20 20 MET HG2 H 2.541 0.001 2 175 20 20 MET HG3 H 2.493 0.003 2 176 20 20 MET HE H 2.072 0.002 1 177 20 20 MET CA C 54.607 . 1 178 20 20 MET CB C 35.313 . 1 179 20 20 MET CG C 31.543 0.002 1 180 20 20 MET CE C 16.765 . 1 181 21 21 CYS H H 8.735 0.001 1 182 21 21 CYS HA H 5.042 0.001 1 183 21 21 CYS HB2 H 3.800 . 2 184 21 21 CYS HB3 H 3.175 0.003 2 185 21 21 CYS CA C 53.653 . 1 186 21 21 CYS CB C 46.949 0.015 1 187 22 22 HYP HA H 4.697 0.006 1 188 22 22 HYP HB2 H 2.497 0.001 2 189 22 22 HYP HB3 H 2.342 0.003 2 190 22 22 HYP HG H 4.699 0.005 1 191 22 22 HYP HD22 H 3.865 0.001 2 192 22 22 HYP HD23 H 3.785 0.001 2 193 22 22 HYP CA C 61.523 . 1 194 22 22 HYP CB C 40.139 0.014 1 195 22 22 HYP CG C 72.578 . 1 196 22 22 HYP CD C 58.179 0.007 1 197 23 23 SER H H 8.929 . 1 198 23 23 SER HA H 4.311 0.003 1 199 23 23 SER HB2 H 3.956 0.007 1 200 23 23 SER HB3 H 3.956 0.007 1 201 23 23 SER CA C 61.334 . 1 202 23 23 SER CB C 62.423 . 1 203 24 24 CYS H H 8.610 0.001 1 204 24 24 CYS HA H 4.265 0.003 1 205 24 24 CYS HB2 H 3.080 0.003 2 206 24 24 CYS HB3 H 2.957 0.009 2 207 24 24 CYS CA C 57.164 . 1 208 24 24 CYS CB C 39.715 0.003 1 209 25 25 MET H H 8.262 0.001 1 210 25 25 MET HA H 4.313 0.002 1 211 25 25 MET HB2 H 2.284 0.001 2 212 25 25 MET HB3 H 2.224 0.001 2 213 25 25 MET HG2 H 2.737 . 2 214 25 25 MET HG3 H 2.662 0.002 2 215 25 25 MET HE H 2.143 . 1 216 25 25 MET CA C 58.267 . 1 217 25 25 MET CB C 32.007 0.013 1 218 25 25 MET CG C 33.096 0.035 1 219 25 25 MET CE C 17.003 . 1 220 26 26 CYS H H 7.970 0.002 1 221 26 26 CYS HA H 4.651 0.002 1 222 26 26 CYS HB2 H 3.485 0.001 2 223 26 26 CYS HB3 H 2.971 0.008 2 224 26 26 CYS CA C 54.868 . 1 225 26 26 CYS CB C 35.656 0.013 1 226 27 27 THR H H 7.314 0.004 1 227 27 27 THR HA H 4.464 0.003 1 228 27 27 THR HB H 4.594 0.007 1 229 27 27 THR HG2 H 1.138 0.003 1 230 27 27 THR CA C 60.126 . 1 231 27 27 THR CB C 68.848 . 1 232 27 27 THR CG2 C 21.712 . 1 233 28 28 ASN H H 7.818 0.001 1 234 28 28 ASN HA H 4.635 0.007 1 235 28 28 ASN HB2 H 3.266 0.001 2 236 28 28 ASN HB3 H 2.769 0.005 2 237 28 28 ASN HD21 H 7.630 . 1 238 28 28 ASN HD22 H 6.870 . 1 239 28 28 ASN CA C 54.236 . 1 240 28 28 ASN CB C 36.936 0.008 1 241 29 29 THR H H 8.347 0.003 1 242 29 29 THR HA H 4.658 0.003 1 243 29 29 THR HB H 4.630 . 1 244 29 29 THR HG2 H 1.152 . 1 245 29 29 THR CA C 60.180 . 1 246 29 29 THR CB C 68.591 . 1 247 29 29 THR CG2 C 21.216 . 1 248 30 30 CYS H H 8.317 0.003 1 249 30 30 CYS HA H 4.426 . 1 250 30 30 CYS HB2 H 2.902 0.001 2 251 30 30 CYS HB3 H 3.238 0.001 2 252 30 30 CYS CA C 55.470 . 1 253 30 30 CYS CB C 40.392 0.023 1 stop_ save_ save_assigned_chem_shift_list_1_2 _Saveframe_category assigned_chemical_shifts _Details 'Origin nmrStar file /ebi/msd/pdb_root/Processing/prepare/4b1q/ebi/cctxglycan.bmrb.csh' loop_ _Experiment_label NOESY TOCSY COSY H2BC 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 polysaccharide _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 A2G H1 H 4.835 . 1 2 1 1 A2G H2 H 4.286 . 1 3 1 1 A2G H3 H 4.238 . 1 4 1 1 A2G H4 H 4.156 . 1 5 1 1 A2G H5 H 4.066 . 1 6 1 1 A2G H6 H 3.848 . 1 7 1 1 A2G H8 H 2.052 . 1 8 1 1 A2G H8A H 2.052 . 1 9 1 1 A2G H8B H 2.052 . 1 10 1 1 A2G H14 H 3.533 . 1 11 1 1 A2G HN2 H 8.483 . 1 12 1 1 A2G C1 C 100.875 . 1 13 1 1 A2G C2 C 51.393 . 1 14 1 1 A2G C3 C 75.605 . 1 15 1 1 A2G C4 C 71.855 . 1 16 1 1 A2G C5 C 71.278 . 1 17 1 1 A2G C6 C 68.894 . 1 18 2 2 NDG H1 H 4.819 0.001 1 19 2 2 NDG H2 H 3.953 0.003 1 20 2 2 NDG H3 H 3.841 0.004 1 21 2 2 NDG H4 H 3.610 0.001 1 22 2 2 NDG H5 H 3.907 0.002 1 23 2 2 NDG H6C1 H 3.842 0.001 1 24 2 2 NDG H6C2 H 3.842 0.001 1 25 2 2 NDG H8C1 H 2.042 . 1 26 2 2 NDG H8C2 H 2.042 . 1 27 2 2 NDG H8C3 H 2.042 . 1 28 2 2 NDG HA H 8.101 . 1 29 2 2 NDG C1 C 99.152 . 1 30 2 2 NDG C2 C 56.252 . 1 31 2 2 NDG C3 C 72.537 . 1 32 2 2 NDG C4 C 80.598 . 1 33 2 2 NDG C5 C 62.515 . 1 34 2 2 NDG C6 C 73.342 . 1 35 3 3 GXL H1 H 5.030 0.001 1 36 3 3 GXL H2 H 3.833 0.001 1 37 3 3 GXL H3 H 3.972 0.001 1 38 3 3 GXL H4 H 3.813 . 1 39 3 3 GXL H5 H 4.212 0.001 1 40 3 3 GXL H6C1 H 3.674 . 1 41 3 3 GXL H6C2 H 3.674 . 1 42 3 3 GXL C1 C 102.326 . 1 43 3 3 GXL C2 C 70.924 . 1 44 3 3 GXL C3 C 71.588 . 1 45 3 3 GXL C5 C 73.234 . 1 46 3 3 GXL C6 C 63.005 . 1 47 4 4 GAL H1 H 4.603 0.001 1 48 4 4 GAL H2 H 3.724 0.003 1 49 4 4 GAL H3 H 3.789 0.002 1 50 4 4 GAL H4 H 3.818 . 1 51 4 4 GAL H5 H 3.589 0.001 1 52 4 4 GAL H61 H 3.695 0.002 2 53 4 4 GAL H62 H 3.751 0.003 2 54 4 4 GAL C1 C 104.457 . 1 55 4 4 GAL C2 C 77.573 . 1 56 4 4 GAL C3 C 76.265 . 1 57 4 4 GAL C4 C 71.700 . 1 58 4 4 GAL C5 C 77.882 . 1 59 4 4 GAL C6 C 63.675 0.013 1 60 5 5 GXL H1 H 5.340 0.001 1 61 5 5 GXL H2 H 3.789 0.003 1 62 5 5 GXL H3 H 3.676 0.002 1 63 5 5 GXL H4 H 3.859 0.002 1 64 5 5 GXL H5 H 4.240 0.001 1 65 5 5 GXL H6C1 H 3.771 0.004 2 66 5 5 GXL H6C2 H 3.681 0.001 2 67 5 5 GXL C1 C 101.240 . 1 68 5 5 GXL C2 C 70.990 . 1 69 5 5 GXL C3 C 71.840 . 1 70 5 5 GXL C4 C 72.194 . 1 71 5 5 GXL C5 C 72.918 . 1 72 5 5 GXL C6 C 64.315 0.022 1 stop_ save_