data_25928 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; NMR solution structure of vitamin B12 conjugates of PYY3-36 ; _BMRB_accession_number 25928 _BMRB_flat_file_name bmr25928.str _Entry_type original _Submission_date 2016-09-15 _Accession_date 2016-09-15 _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 Doyle R. P. . 2 Henry K. E. . 3 Roth C. L. . 4 Kerwood D. J . 5 Allis D. G. . 6 Holz G. G. . 7 Zubieta J. . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 190 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2016-09-15 original BMRB . stop_ _Original_release_date 2016-09-15 save_ ############################# # Citation for this entry # ############################# save_citations _Saveframe_category entry_citation _Citation_full . _Citation_title ; Solution Structure and Constrained Molecular Dynamics Study of Vitamin B12 Conjugates of the Anorectic Peptide PYY(3-36) ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 27027248 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Henry Kelly E. . 2 Kerwood Deborah J. . 3 Allis Damian G. . 4 Workinger Jayme L. . 5 Bonaccorso Ron L. . 6 Holz George G. . 7 Roth Christian L. . 8 Zubieta Jon A. . 9 Doyle Robert P. . stop_ _Journal_abbreviation ChemMedChem _Journal_volume 11 _Journal_issue 9 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 1015 _Page_last 1021 _Year 2016 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'vitamin B12 conjugate of PYY3-36' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label 'vitamin B12 conjugate of PYY3-36' $vitamin_B12_conjugate_of_PYY3-36 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_vitamin_B12_conjugate_of_PYY3-36 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common vitamin_B12_conjugate_of_PYY3-36 _Molecular_mass 4007.475 _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 35 _Mol_residue_sequence ; IXPEAPGEDASPEELNRYYA SLRHYLNLVVTRQRY ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 3 ILE 2 4 LCT 3 6 PRO 4 7 GLU 5 8 ALA 6 9 PRO 7 10 GLY 8 11 GLU 9 12 ASP 10 13 ALA 11 14 SER 12 15 PRO 13 16 GLU 14 17 GLU 15 18 LEU 16 19 ASN 17 20 ARG 18 21 TYR 19 22 TYR 20 23 ALA 21 24 SER 22 25 LEU 23 26 ARG 24 27 HIS 25 28 TYR 26 29 LEU 27 30 ASN 28 31 LEU 29 32 VAL 30 33 VAL 31 34 THR 32 35 ARG 33 36 GLN 34 37 ARG 35 38 TYR stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ###################### # Polymer residues # ###################### save_chem_comp_LCT _Saveframe_category polymer_residue _Mol_type NON-POLYMER _Name_common N-[5-(4-nitrophenyl)-1,3,4-thiadiazol-2-yl]acetamide _BMRB_code LCT _PDB_code LCT _Standard_residue_derivative . _Molecular_mass 264.261 _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 . ? O34 O34 O . 0 . ? C32 C32 C . 0 . ? C36 C36 C . 0 . ? N30 N30 N . 0 . ? C22 C22 C . 0 . ? N23 N23 N . 0 . ? N24 N24 N . 0 . ? S21 S21 S . 0 . ? C19 C19 C . 0 . ? N13 N13 N . 1 . ? O15 O15 O . -1 . ? O17 O17 O . 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 . ? H7 H7 H . 0 . ? H8 H8 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 C1 C2 ? ? SING C1 C6 ? ? SING C2 C3 ? ? SING C2 N13 ? ? DOUB C3 C4 ? ? SING C4 C5 ? ? DOUB C5 C6 ? ? SING C5 C19 ? ? DOUB O34 C32 ? ? SING C32 C36 ? ? SING C32 N30 ? ? SING N30 C22 ? ? DOUB C22 N23 ? ? SING C22 S21 ? ? SING N23 N24 ? ? DOUB N24 C19 ? ? SING S21 C19 ? ? SING N13 O15 ? ? DOUB N13 O17 ? ? SING C1 H1 ? ? SING C3 H2 ? ? SING C4 H3 ? ? SING C6 H4 ? ? SING C36 H5 ? ? SING C36 H6 ? ? SING C36 H7 ? ? SING N30 H8 ? ? stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $vitamin_B12_conjugate_of_PYY3-36 . . . . . . 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 $vitamin_B12_conjugate_of_PYY3-36 'chemical synthesis' . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details '90% H2O, 10% D2O' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $vitamin_B12_conjugate_of_PYY3-36 1 mM 'natural abundance' H2O 90 % 'natural abundance' D2O 10 % 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_TOPSPIN _Saveframe_category software _Name TOPSPIN _Version 1.3 loop_ _Vendor _Address _Electronic_address 'Bruker Biospin' . . stop_ loop_ _Task 'chemical shift assignment' 'chemical shift calculation' collection stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model DRX _Field_strength 500 _Details . save_ ############################# # NMR applied experiments # ############################# save_NOESY_1 _Saveframe_category NMR_applied_experiment _Experiment_name NOESY _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_DQF-COSY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D DQF-COSY' _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 pH 5.5 .1 pH temperature 273 . 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 water H 1 protons ppm 4.769 internal direct . . . 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 . loop_ _Experiment_label NOESY '2D 1H-1H TOCSY' '2D DQF-COSY' 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 'vitamin B12 conjugate of PYY3-36' _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 3 1 ILE HA H 3.89 0.02 1 2 3 1 ILE HB H 1.94 0.02 1 3 3 1 ILE HG12 H 1.19 0.02 2 4 3 1 ILE HG13 H 1.47 0.02 2 5 3 1 ILE HG2 H 0.97 0.02 1 6 3 1 ILE HD1 H 0.87 0.02 1 7 6 3 PRO HA H 4.38 0.02 1 8 6 3 PRO HB2 H 2.31 0.02 2 9 6 3 PRO HB3 H 2.31 0.02 2 10 6 3 PRO HG2 H 1.88 0.02 2 11 6 3 PRO HG3 H 1.88 0.02 2 12 6 3 PRO HD2 H 3.33 0.02 2 13 6 3 PRO HD3 H 3.56 0.02 2 14 7 4 GLU H H 8.35 0.02 1 15 7 4 GLU HA H 4.26 0.02 1 16 7 4 GLU HB2 H 1.99 0.02 2 17 7 4 GLU HB3 H 1.88 0.02 2 18 7 4 GLU HG2 H 2.42 0.02 2 19 7 4 GLU HG3 H 2.42 0.02 2 20 8 5 ALA H H 8.32 0.02 1 21 8 5 ALA HA H 3.70 0.02 1 22 8 5 ALA HB H 1.14 0.02 1 23 9 6 PRO HA H 4.30 0.02 1 24 9 6 PRO HB2 H 1.77 0.02 2 25 9 6 PRO HB3 H 2.11 0.02 2 26 9 6 PRO HG2 H 1.67 0.02 2 27 9 6 PRO HG3 H 1.67 0.02 2 28 9 6 PRO HD2 H 2.97 0.02 2 29 9 6 PRO HD3 H 2.97 0.02 2 30 10 7 GLY H H 8.22 0.02 1 31 10 7 GLY HA2 H 3.90 0.02 2 32 10 7 GLY HA3 H 3.98 0.02 2 33 11 8 GLU H H 8.33 0.02 1 34 11 8 GLU HA H 4.13 0.02 1 35 11 8 GLU HB2 H 2.02 0.02 2 36 11 8 GLU HB3 H 2.02 0.02 2 37 11 8 GLU HG2 H 2.42 0.02 2 38 11 8 GLU HG3 H 2.42 0.02 2 39 12 9 ASP H H 8.56 0.02 1 40 12 9 ASP HA H 4.66 0.02 1 41 12 9 ASP HB2 H 2.78 0.02 2 42 12 9 ASP HB3 H 2.87 0.02 2 43 13 10 ALA H H 7.51 0.02 1 44 13 10 ALA HA H 4.20 0.02 1 45 13 10 ALA HB H 1.32 0.02 1 46 14 11 SER H H 8.31 0.02 1 47 14 11 SER HA H 4.74 0.02 1 48 14 11 SER HB2 H 4.02 0.02 2 49 14 11 SER HB3 H 4.34 0.02 2 50 15 12 PRO HA H 4.28 0.02 1 51 15 12 PRO HB2 H 2.41 0.02 2 52 15 12 PRO HB3 H 1.96 0.02 2 53 15 12 PRO HG2 H 2.19 0.02 2 54 15 12 PRO HG3 H 2.19 0.02 2 55 15 12 PRO HD2 H 3.90 0.02 2 56 15 12 PRO HD3 H 3.90 0.02 2 57 16 13 GLU H H 8.38 0.02 1 58 16 13 GLU HA H 4.17 0.02 1 59 16 13 GLU HB2 H 1.98 0.02 2 60 16 13 GLU HB3 H 2.11 0.02 2 61 16 13 GLU HG2 H 2.42 0.02 2 62 16 13 GLU HG3 H 2.42 0.02 2 63 17 14 GLU H H 7.88 0.02 1 64 17 14 GLU HA H 4.02 0.02 1 65 17 14 GLU HB2 H 2.28 0.02 2 66 17 14 GLU HB3 H 2.28 0.02 2 67 17 14 GLU HG2 H 2.43 0.02 2 68 17 14 GLU HG3 H 2.43 0.02 2 69 18 15 LEU H H 8.36 0.02 1 70 18 15 LEU HA H 3.98 0.02 1 71 18 15 LEU HB2 H 1.81 0.02 2 72 18 15 LEU HB3 H 1.81 0.02 2 73 18 15 LEU HG H 1.54 0.02 1 74 18 15 LEU HD1 H 0.81 0.02 2 75 18 15 LEU HD2 H 0.81 0.02 2 76 19 16 ASN H H 8.41 0.02 1 77 19 16 ASN HA H 4.55 0.02 1 78 19 16 ASN HB2 H 2.90 0.02 2 79 19 16 ASN HB3 H 2.90 0.02 2 80 19 16 ASN HD21 H 7.62 0.02 2 81 19 16 ASN HD22 H 6.95 0.02 2 82 20 17 ARG H H 7.99 0.02 1 83 20 17 ARG HA H 4.12 0.02 1 84 20 17 ARG HB2 H 1.82 0.02 2 85 20 17 ARG HB3 H 1.93 0.02 2 86 20 17 ARG HG2 H 1.62 0.02 2 87 20 17 ARG HG3 H 1.62 0.02 2 88 20 17 ARG HD2 H 3.22 0.02 2 89 20 17 ARG HD3 H 3.22 0.02 2 90 20 17 ARG HE H 7.32 0.02 1 91 21 18 TYR H H 8.04 0.02 1 92 21 18 TYR HA H 4.34 0.02 1 93 21 18 TYR HB2 H 3.11 0.02 2 94 21 18 TYR HB3 H 2.97 0.02 2 95 21 18 TYR HD1 H 6.70 0.02 3 96 21 18 TYR HD2 H 6.70 0.02 3 97 21 18 TYR HE1 H 6.56 0.02 3 98 21 18 TYR HE2 H 6.56 0.02 3 99 22 19 TYR H H 8.63 0.02 1 100 22 19 TYR HA H 4.05 0.02 1 101 22 19 TYR HB2 H 2.98 0.02 2 102 22 19 TYR HB3 H 3.10 0.02 2 103 22 19 TYR HD1 H 7.13 0.02 3 104 22 19 TYR HD2 H 7.13 0.02 3 105 22 19 TYR HE1 H 6.88 0.02 3 106 22 19 TYR HE2 H 6.88 0.02 3 107 23 20 ALA H H 8.05 0.02 1 108 23 20 ALA HA H 4.14 0.02 1 109 23 20 ALA HB H 1.51 0.02 1 110 24 21 SER H H 8.11 0.02 1 111 24 21 SER HA H 4.33 0.02 1 112 24 21 SER HB2 H 3.96 0.02 2 113 24 21 SER HB3 H 4.06 0.02 2 114 25 22 LEU HA H 4.09 0.02 1 115 25 22 LEU HB2 H 1.22 0.02 2 116 25 22 LEU HB3 H 1.22 0.02 2 117 25 22 LEU HG H 1.34 0.02 1 118 25 22 LEU HD1 H 0.83 0.02 2 119 26 23 ARG H H 8.07 0.04 1 120 26 23 ARG HA H 4.01 0.02 1 121 26 23 ARG HB2 H 1.86 0.02 2 122 26 23 ARG HB3 H 1.86 0.02 2 123 26 23 ARG HG2 H 1.58 0.02 2 124 26 23 ARG HG3 H 1.73 0.02 2 125 26 23 ARG HD2 H 3.17 0.02 2 126 26 23 ARG HD3 H 3.17 0.02 2 127 26 23 ARG HE H 7.23 0.02 1 128 27 24 HIS H H 7.96 0.02 1 129 27 24 HIS HA H 4.47 0.02 1 130 27 24 HIS HB2 H 3.32 0.02 2 131 27 24 HIS HB3 H 3.27 0.02 2 132 28 25 TYR H H 8.15 0.02 1 133 28 25 TYR HA H 4.27 0.02 1 134 28 25 TYR HB2 H 3.11 0.02 2 135 28 25 TYR HB3 H 3.11 0.02 2 136 28 25 TYR HD1 H 7.06 0.02 3 137 28 25 TYR HD2 H 7.06 0.02 3 138 29 26 LEU H H 8.37 0.02 1 139 29 26 LEU HA H 4.01 0.02 1 140 29 26 LEU HB2 H 1.73 0.02 2 141 29 26 LEU HB3 H 1.73 0.02 2 142 29 26 LEU HD1 H 0.84 0.02 2 143 30 27 ASN H H 8.03 0.02 1 144 30 27 ASN HA H 4.52 0.02 1 145 30 27 ASN HB2 H 2.81 0.02 2 146 30 27 ASN HB3 H 2.81 0.02 2 147 30 27 ASN HD21 H 7.56 0.02 2 148 30 27 ASN HD22 H 6.89 0.02 2 149 31 28 LEU H H 7.77 0.02 1 150 31 28 LEU HA H 4.18 0.02 1 151 31 28 LEU HB2 H 1.53 0.02 2 152 31 28 LEU HB3 H 1.53 0.02 2 153 31 28 LEU HG H 1.65 0.02 1 154 31 28 LEU HD1 H 0.80 0.02 2 155 32 29 VAL H H 7.91 0.02 1 156 32 29 VAL HA H 3.99 0.02 1 157 32 29 VAL HB H 2.01 0.02 1 158 32 29 VAL HG1 H 0.80 0.02 2 159 33 31 THR H H 7.92 0.02 1 160 33 31 THR HA H 4.22 0.02 1 161 33 31 THR HB H 4.22 0.02 1 162 33 31 THR HG2 H 1.21 0.02 1 163 34 32 ARG H H 8.00 0.02 1 164 34 32 ARG HA H 4.26 0.02 1 165 34 32 ARG HB2 H 1.85 0.02 2 166 34 32 ARG HB3 H 1.79 0.02 2 167 34 32 ARG HG2 H 1.64 0.02 2 168 34 32 ARG HG3 H 1.64 0.02 2 169 34 32 ARG HD2 H 3.16 0.02 2 170 34 32 ARG HD3 H 3.16 0.02 2 171 34 32 ARG HE H 7.16 0.02 1 172 35 33 GLN H H 8.20 0.02 1 173 35 33 GLN HA H 4.22 0.02 1 174 35 33 GLN HB2 H 1.98 0.02 2 175 35 33 GLN HB3 H 1.98 0.02 2 176 35 33 GLN HG2 H 2.33 0.02 2 177 35 33 GLN HG3 H 2.33 0.02 2 178 36 34 ARG H H 8.20 0.02 1 179 36 34 ARG HA H 4.20 0.02 1 180 36 34 ARG HB2 H 1.67 0.02 2 181 36 34 ARG HB3 H 1.67 0.02 2 182 36 34 ARG HG2 H 1.45 0.02 2 183 36 34 ARG HG3 H 1.45 0.02 2 184 36 34 ARG HD2 H 3.11 0.02 2 185 36 34 ARG HD3 H 3.11 0.02 2 186 36 34 ARG HE H 7.11 0.02 1 187 37 35 TYR H H 8.09 0.02 1 188 37 35 TYR HA H 4.55 0.02 1 189 37 35 TYR HB2 H 3.09 0.02 2 190 37 35 TYR HB3 H 2.88 0.02 2 stop_ save_