data_17870 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Di-O-GalNAc glycosylated Mucin sequence based on MUC2 Mucin glycoprotein tandem repeat ; _BMRB_accession_number 17870 _BMRB_flat_file_name bmr17870.str _Entry_type original _Submission_date 2011-08-18 _Accession_date 2011-08-18 _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 Borgert Andrew . . 2 Heimburg-Molinaro Jamie . . 3 Lasanajak Yi . . 4 Ju Tongzhong . . 5 Liu Mian . . 6 Thompson Pamela . . 7 Ragupathi Govind . . 8 Barany George . . 9 Cummings Richard . . 10 Smith David . . 11 Live David . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 3 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 65 "13C chemical shifts" 37 "15N chemical shifts" 6 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2012-06-29 update BMRB 'update entry citation' 2012-03-27 original author 'original release' stop_ loop_ _Related_BMRB_accession_number _Relationship 17868 'Mucin sequence based on MUC2 Mucin glycoprotein tandem repeat' 17869 'Tri-O-GalNAc glycosylated Mucin sequence based on MUC2 Mucin glycoprotein tandem repeat' 17872 'Mucin sequence based on MUC2 Mucin glycoprotein tandem repeat' 17873 'Mucin sequence based on MUC2 Mucin glycoprotein tandem repeat' 17874 'Mono-O-GalNAc glycosylated Mucin sequence based on MUC2 Mucin glycoprotein tandem repeat' 17875 'Mono-O-GalNAc glycosylated Mucin sequence based on MUC2 Mucin glycoprotein tandem repeat' stop_ save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title 'Deciphering structural elements of mucin glycoprotein recognition.' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 22444368 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Borgert Andrew . . 2 Heimburg-Molinaro Jamie . . 3 Song Xuezheng . . 4 Lasanajak Yi . . 5 Ju Tongzhong . . 6 Liu Mian . . 7 Thompson Pamela . . 8 Ragupathi Govind . . 9 Barany George . . 10 Smith David F. . 11 Cummings Richard D. . 12 Live David . . stop_ _Journal_abbreviation 'ACS Chem. Biol.' _Journal_name_full 'ACS chemical biology' _Journal_volume 7 _Journal_issue 6 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 1031 _Page_last 1039 _Year 2012 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'MUC2_Mucin_Domain_Peptide, SUGAR (2-MER)' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label MUC2_Mucin_Domain_Peptide $MUC2_Mucin_Domain_Peptide 'SUGAR (2-MER), 1' $A2G 'SUGAR (2-MER), 2' $A2G 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_MUC2_Mucin_Domain_Peptide _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common MUC2_Mucin_Domain_Peptide _Molecular_mass 781.948 _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 9 _Mol_residue_sequence XPTTTPLKX loop_ _Residue_seq_code _Residue_label 1 ACE 2 PRO 3 THR 4 THR 5 THR 6 PRO 7 LEU 8 LYS 9 NH2 stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ###################### # Polymer residues # ###################### save_chem_comp_ACE _Saveframe_category polymer_residue _Mol_type non-polymer _Name_common 'ACETYL GROUP' _BMRB_code . _PDB_code ACE _Standard_residue_derivative . _Molecular_mass 44.053 _Mol_paramagnetic . _Details ; Information obtained from PDB's Chemical Component Dictionary at http://wwpdb-remediation.rutgers.edu/downloads.html Downloaded on Thu Aug 25 10:53:14 2011 ; loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons C C C . 0 . ? O O O . 0 . ? CH3 CH3 C . 0 . ? H H H . 0 . ? H1 H1 H . 0 . ? H2 H2 H . 0 . ? H3 H3 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 DOUB C O ? ? SING C CH3 ? ? SING C H ? ? SING CH3 H1 ? ? SING CH3 H2 ? ? SING CH3 H3 ? ? stop_ save_ save_chem_comp_NH2 _Saveframe_category polymer_residue _Mol_type non-polymer _Name_common 'AMINO GROUP' _BMRB_code . _PDB_code NH2 _Standard_residue_derivative . _Molecular_mass 16.023 _Mol_paramagnetic . _Details ; Information obtained from PDB's Chemical Component Dictionary at http://wwpdb-remediation.rutgers.edu/downloads.html Downloaded on Thu Aug 25 10:51:49 2011 ; loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons N N N . 0 . ? HN1 HN1 H . 0 . ? HN2 HN2 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 HN1 ? ? SING N HN2 ? ? stop_ save_ ############# # Ligands # ############# save_A2G _Saveframe_category ligand _Mol_type "non-polymer (SACCHARIDE)" _Name_common "A2G (N-ACETYL-2-DEOXY-2-AMINO-GALACTOSE)" _BMRB_code . _PDB_code A2G _Molecular_mass 221.208 _Mol_charge 0 _Mol_paramagnetic . _Mol_aromatic no _Details ; Information obtained from PDB's Chemical Component Dictionary at http://wwpdb-remediation.rutgers.edu/downloads.html Downloaded on Thu Aug 25 10:48:35 2011 ; loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons O O O . 0 . ? C1 C1 C . 0 . ? O1 O1 O . 0 . ? C2 C2 C . 0 . ? N2 N2 N . 0 . ? C3 C3 C . 0 . ? O3 O3 O . 0 . ? C4 C4 C . 0 . ? O4 O4 O . 0 . ? C5 C5 C . 0 . ? C6 C6 C . 0 . ? O6 O6 O . 0 . ? C7 C7 C . 0 . ? O7 O7 O . 0 . ? C8 C8 C . 0 . ? H1 H1 H . 0 . ? HO1 HO1 H . 0 . ? H2 H2 H . 0 . ? HN2 HN2 H . 0 . ? H3 H3 H . 0 . ? HO3 HO3 H . 0 . ? H4 H4 H . 0 . ? HO4 HO4 H . 0 . ? H5 H5 H . 0 . ? H6 H6 H . 0 . ? H8 H8 H . 0 . ? H8A H8A H . 0 . ? H8B H8B H . 0 . ? H14 H14 H . 0 . ? H15 H15 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 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_ _Mol_thiol_state . _Sequence_homology_query_date . save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $MUC2_Mucin_Domain_Peptide Human 9606 Eukaryota Metazoa Homo sapiens 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 $MUC2_Mucin_Domain_Peptide 'chemical synthesis' . . . . . 'Synthesized via solid phase peptide synthesis' $A2G 'obtained from a vendor' . . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_h2o _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Concentration_min_value _Concentration_max_value _Isotopic_labeling $MUC2_Mucin_Domain_Peptide . mM 2 10 'natural abundance' $A2G . mM 2 10 'natural abundance' H2O 90 % . . 'natural abundance' D2O 10 % . . 'natural abundance' stop_ save_ save_sample_d2o _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Concentration_min_value _Concentration_max_value _Isotopic_labeling $MUC2_Mucin_Domain_Peptide . mM 2 10 'natural abundance' $A2G . mM 2 10 'natural abundance' D2O 100 % . . 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_CNS _Saveframe_category software _Name CNS _Version . loop_ _Vendor _Address _Electronic_address 'Brunger A. T. et.al.' . . stop_ loop_ _Task 'structure solution' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Varian _Model INOVA _Field_strength 600 _Details 'University of Minnesota 600' save_ save_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer Varian _Model INOVA _Field_strength 800 _Details 'University of Minnesota 800' save_ save_spectrometer_3 _Saveframe_category NMR_spectrometer _Manufacturer Varian _Model INOVA _Field_strength 900 _Details 'Univeristy of Georgia 900' save_ ############################# # NMR applied experiments # ############################# save_2D_1H-1H_NOESY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_h2o save_ save_2D_1H-1H_NOESY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_d2o save_ save_3D_TOCSY-NOESY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '3D TOCSY-NOESY' _Sample_label $sample_h2o save_ save_2D_1H-15N_HSQC_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample_h2o save_ save_2D_1H-13C_HSQC_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $sample_h2o save_ save_2D_1H-1H_TOCSY_6 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample_h2o save_ save_2D_1H-1H_COSY_7 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H COSY' _Sample_label $sample_h2o save_ save_2D_1H-1H_COSY_8 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H COSY' _Sample_label $sample_d2o save_ save_2D_1H-13C_HMBC_9 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HMBC' _Sample_label $sample_h2o save_ ####################### # Sample conditions # ####################### save_sample_conditions_all _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units temperature 273 . K pH 4.5 . 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 . 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 internal indirect . . . 0.251449530 DSS N 15 'methyl protons' ppm 0.00 internal indirect . . . 0.101329118 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_ _Experiment_label '2D 1H-15N HSQC' '2D 1H-13C HSQC' '2D 1H-1H TOCSY' '2D 1H-1H COSY' '2D 1H-13C HMBC' stop_ loop_ _Sample_label $sample_h2o $sample_d2o stop_ _Sample_conditions_label $sample_conditions_all _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name MUC2_Mucin_Domain_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 2 2 PRO HA H 4.46 .005 1 2 2 2 PRO HB2 H 2.30 .005 2 3 2 2 PRO HB3 H 1.93 .005 2 4 2 2 PRO HG2 H 1.97 .005 2 5 2 2 PRO HG3 H 1.97 .005 2 6 2 2 PRO HD2 H 3.64 .005 2 7 2 2 PRO HD3 H 3.64 .005 2 8 2 2 PRO CA C 62.78 .005 1 9 2 2 PRO CB C 32.79 .005 1 10 2 2 PRO CG C 27.17 .005 1 11 2 2 PRO CD C 51.48 .005 1 12 3 3 THR H H 8.30 .005 1 13 3 3 THR HA H 4.50 .005 1 14 3 3 THR HB H 4.22 .005 1 15 3 3 THR HG2 H 1.24 .005 1 16 3 3 THR CA C 61.80 .005 1 17 3 3 THR CB C 70.04 .005 1 18 3 3 THR CG2 C 21.73 .005 1 19 3 3 THR N N 114.80 .005 1 20 4 4 THR H H 8.51 .005 1 21 4 4 THR HA H 4.74 .005 1 22 4 4 THR HB H 4.34 .005 1 23 4 4 THR HG2 H 1.25 .005 1 24 4 4 THR CA C 59.81 .005 1 25 4 4 THR CB C 79.33 .005 1 26 4 4 THR CG2 C 21.73 .005 1 27 4 4 THR N N 115.60 .005 1 28 5 5 THR H H 8.67 .005 1 29 5 5 THR HA H 4.67 .005 1 30 5 5 THR HB H 4.25 .005 1 31 5 5 THR HG2 H 1.28 .005 1 32 5 5 THR CA C 58.40 .005 1 33 5 5 THR CB C 77.07 .005 1 34 5 5 THR CG2 C 21.48 .005 1 35 5 5 THR N N 113.50 .005 1 36 6 6 PRO HA H 4.41 .005 1 37 6 6 PRO HB2 H 2.27 .005 2 38 6 6 PRO HB3 H 1.86 .005 2 39 6 6 PRO HG2 H 2.00 .005 2 40 6 6 PRO HG3 H 2.00 .005 2 41 6 6 PRO HD2 H 3.65 .005 2 42 6 6 PRO HD3 H 3.66 .005 2 43 6 6 PRO CA C 62.41 .005 1 44 6 6 PRO CB C 32.25 .005 1 45 6 6 PRO CG C 27.30 .005 1 46 6 6 PRO CD C 50.57 .005 1 47 7 7 LEU H H 8.19 .005 1 48 7 7 LEU HA H 4.12 .005 1 49 7 7 LEU HB2 H 1.58 .005 2 50 7 7 LEU HB3 H 1.58 .005 2 51 7 7 LEU HG H 1.62 .005 1 52 7 7 LEU HD1 H 0.96 .005 2 53 7 7 LEU HD2 H 0.92 .005 2 54 7 7 LEU CA C 55.56 .005 1 55 8 8 LYS H H 8.36 .005 1 56 8 8 LYS HA H 4.22 .005 1 57 8 8 LYS HB2 H 1.79 .005 2 58 8 8 LYS HB3 H 1.76 .005 2 59 8 8 LYS HG2 H 1.45 .005 2 60 8 8 LYS HG3 H 1.40 .005 2 61 8 8 LYS HD2 H 1.68 .005 2 62 8 8 LYS HD3 H 1.68 .005 2 63 8 8 LYS HE2 H 2.98 .005 2 64 8 8 LYS HE3 H 2.98 .005 2 65 8 8 LYS CA C 56.23 .005 1 66 8 8 LYS CB C 33.05 .005 1 67 8 8 LYS CG C 24.75 .005 1 68 8 8 LYS CD C 29.15 .005 1 69 8 8 LYS CE C 42.17 .005 1 70 8 8 LYS N N 124.60 .005 1 stop_ save_ save_assigned_chem_shift_list_1_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-15N HSQC' '2D 1H-13C HSQC' '2D 1H-1H TOCSY' '2D 1H-1H COSY' '2D 1H-13C HMBC' stop_ loop_ _Sample_label $sample_h2o $sample_d2o stop_ _Sample_conditions_label $sample_conditions_all _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name 'SUGAR (2-MER), 1' _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 10 1 A2G C1 C 101.59 .005 1 2 10 1 A2G C2 C 52.50 .005 1 3 10 1 A2G C3 C 70.97 .005 1 4 10 1 A2G C4 C 71.40 .005 1 5 10 1 A2G C5 C 74.10 .005 1 6 10 1 A2G C6 C 64.20 .005 1 7 10 1 A2G C8 C 25.20 .005 1 8 10 1 A2G H1 H 4.78 .005 1 9 10 1 A2G H14 H 3.72 .005 2 10 10 1 A2G H2 H 4.04 .005 1 11 10 1 A2G H3 H 3.87 .005 1 12 10 1 A2G H4 H 3.95 .005 1 13 10 1 A2G H5 H 3.99 .005 1 14 10 1 A2G H6 H 3.72 .005 2 15 10 1 A2G H8 H 1.99 .005 2 16 10 1 A2G H8A H 1.99 .005 2 17 10 1 A2G H8B H 1.99 .005 2 18 10 1 A2G HN2 H 7.72 .005 1 19 10 1 A2G N2 N 122.80 .005 1 stop_ save_ save_assigned_chem_shift_list_1_3 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-15N HSQC' '2D 1H-13C HSQC' '2D 1H-1H TOCSY' '2D 1H-1H COSY' '2D 1H-13C HMBC' stop_ loop_ _Sample_label $sample_h2o $sample_d2o stop_ _Sample_conditions_label $sample_conditions_all _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name 'SUGAR (2-MER), 2' _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 11 1 A2G C1 C 101.19 .005 1 2 11 1 A2G C2 C 52.57 .005 1 3 11 1 A2G C3 C 71.33 .005 1 4 11 1 A2G C4 C 71.46 .005 1 5 11 1 A2G C5 C 74.17 .005 1 6 11 1 A2G C6 C 64.20 .005 1 7 11 1 A2G C8 C 25.20 .005 1 8 11 1 A2G H1 H 4.98 .005 1 9 11 1 A2G H14 H 3.73 .005 2 10 11 1 A2G H2 H 4.08 .005 1 11 11 1 A2G H3 H 3.87 .005 1 12 11 1 A2G H4 H 3.96 .005 1 13 11 1 A2G H5 H 4.01 .005 1 14 11 1 A2G H6 H 3.73 .005 2 15 11 1 A2G H8 H 2.00 .005 2 16 11 1 A2G H8A H 2.00 .005 2 17 11 1 A2G H8B H 2.00 .005 2 18 11 1 A2G HN2 H 7.79 .005 1 19 11 1 A2G N2 N 122.90 .005 1 stop_ save_