data_20086 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Helical Agonist of Nociceptin (NOP) Receptor ; _BMRB_accession_number 20086 _BMRB_flat_file_name bmr20086.str _Entry_type new _Submission_date 2009-07-23 _Accession_date 2009-07-23 _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 Hill Timothy A. . 2 Fairlie David P. . 3 Hoang Huy N. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 coupling_constants 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 80 "coupling constants" 17 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2011-07-08 update BMRB 'update entry citation' 2011-06-03 original author 'orginial release' stop_ loop_ _Related_BMRB_accession_number _Relationship 20087 'nociceptin analogue' 20088 'nociceptin analogue' 20089 'nociceptin analogue' stop_ save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title 'Novel Helix-Constrained Nociceptin Derivatives Are Potent Agonists and Antagonists of ERK Phosphorylation and Thermal Analgesia in Mice.' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 21067234 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Harrison Rosemary S. . 2 Ruiz-Gomez Gloria . . 3 Hill Timothy A. . 4 Chow Shiao Y. . 5 Shepherd Nicholas E. . 6 Lohman Rink-Jan . . 7 Abbenante Giovanni . . 8 Hoang Huy N. . 9 Fairlie David P. . stop_ _Journal_abbreviation 'J. Med. Chem.' _Journal_name_full 'Journal of medicinal chemistry' _Journal_volume 53 _Journal_issue 23 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 8400 _Page_last 8408 _Year 2010 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'nociceptin Antagonist' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label 'Nociceptin Antagonist' $Nociceptin_Antagonist 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_Nociceptin_Antagonist _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common Nociceptin_Antagonist _Molecular_mass . _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 18 _Mol_residue_sequence FGGFTGKRKSDRKKANQD loop_ _Residue_seq_code _Residue_label 1 PHE 2 GLY 3 GLY 4 PHE 5 THR 6 GLY 7 LYS 8 ARG 9 LYS 10 SER 11 ASP 12 ARG 13 LYS 14 LYS 15 ALA 16 ASN 17 GLN 18 ASP stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $Nociceptin_Antagonist . . . . . . 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 $Nociceptin_Antagonist 'recombinant technology' . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $Nociceptin_Antagonist 3 mM 'natural abundance' H2O 90 % 'natural abundance' D2O 10 % 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_X-PLOR_NIH _Saveframe_category software _Name X-PLOR_NIH _Version . loop_ _Vendor _Address _Electronic_address 'Schwieters, Kuszewski, Tjandra and Clore' . . stop_ loop_ _Task 'geometry optimization' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 600 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-1H_NOESY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H 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 temperature 288 . K pH 3.5 . pH 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 direct . . . 1.00000 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 '2D 1H-1H 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 'Nociceptin Antagonist' _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 PHE HA H 4.20 0.025 1 2 1 1 PHE HB2 H 3.01 0.0035 2 3 1 1 PHE HB3 H 3.04 0.0035 2 4 2 2 GLY H H 8.48 0.0035 1 5 2 2 GLY HA2 H 3.79 0.025 1 6 3 3 GLY H H 7.81 0.0035 1 7 3 3 GLY HA2 H 3.67 0.025 1 8 4 4 PHE H H 8.19 0.0035 1 9 4 4 PHE HA H 4.51 0.025 1 10 4 4 PHE HB2 H 2.93 0.0035 2 11 4 4 PHE HB3 H 2.86 0.0035 2 12 5 5 THR H H 8.11 0.0035 1 13 5 5 THR HA H 4.01 0.025 1 14 5 5 THR HB H 3.98 0.025 1 15 6 6 GLY H H 7.87 0.0035 1 16 6 6 GLY HA2 H 3.98 0.025 1 17 7 7 LYS H H 7.91 0.0035 1 18 7 7 LYS HA H 4.00 0.025 1 19 7 7 LYS HB2 H 1.62 0.025 1 20 7 7 LYS HD2 H 1.27 0.025 2 21 7 7 LYS HD3 H 1.35 0.025 2 22 7 7 LYS HE2 H 2.78 0.025 2 23 7 7 LYS HE3 H 3.38 0.025 2 24 7 7 LYS HG2 H 1.09 0.025 1 25 8 8 ARG H H 8.24 0.0035 1 26 8 8 ARG HA H 3.88 0.025 1 27 8 8 ARG HB2 H 1.64 0.025 1 28 8 8 ARG HD2 H 2.92 0.025 1 29 8 8 ARG HG2 H 1.39 0.025 2 30 8 8 ARG HG3 H 1.50 0.025 2 31 9 9 LYS H H 7.67 0.0035 1 32 9 9 LYS HA H 3.85 0.025 1 33 9 9 LYS HB2 H 1.66 0.025 1 34 9 9 LYS HD2 H 1.46 0.025 2 35 9 9 LYS HD3 H 1.52 0.025 2 36 9 9 LYS HE2 H 2.74 0.025 1 37 9 9 LYS HG2 H 1.13 0.025 2 38 9 9 LYS HG3 H 1.19 0.025 2 39 10 10 SER H H 8.01 0.0035 1 40 10 10 SER HA H 3.70 0.025 1 41 10 10 SER HB2 H 3.60 0.025 1 42 11 11 ASP H H 8.62 0.0035 1 43 11 11 ASP HA H 4.54 0.025 1 44 11 11 ASP HB2 H 2.64 0.025 2 45 11 11 ASP HB3 H 2.52 0.025 2 46 12 12 ARG H H 7.63 0.0035 1 47 12 12 ARG HA H 4.04 0.025 1 48 12 12 ARG HB2 H 1.66 0.025 1 49 12 12 ARG HE H 7.06 0.0035 1 50 12 12 ARG HG2 H 1.54 0.025 1 51 12 12 ARG HG3 H 1.44 0.025 1 52 13 13 LYS H H 7.85 0.0035 1 53 13 13 LYS HA H 4.03 0.025 1 54 13 13 LYS HB2 H 1.69 0.025 1 55 13 13 LYS HD2 H 1.48 0.025 1 56 13 13 LYS HE2 H 2.82 0.025 1 57 13 13 LYS HG2 H 1.16 0.025 2 58 13 13 LYS HG3 H 1.22 0.025 2 59 14 14 LYS H H 7.89 0.0035 1 60 14 14 LYS HA H 3.99 0.025 1 61 14 14 LYS HB2 H 2.47 0.025 1 62 14 14 LYS HD2 H 1.63 0.025 1 63 14 14 LYS HE2 H 2.58 0.025 2 64 14 14 LYS HE3 H 3.30 0.025 2 65 14 14 LYS HG2 H 1.20 0.025 2 66 14 14 LYS HG3 H 1.38 0.025 2 67 15 15 ALA H H 8.03 0.0035 1 68 15 15 ALA HA H 3.87 0.025 1 69 15 15 ALA HB H 1.25 0.025 1 70 16 16 ASN H H 7.78 0.0035 1 71 16 16 ASN HA H 4.34 0.025 1 72 16 16 ASN HB2 H 2.66 0.025 1 73 17 17 GLN H H 7.95 0.0035 1 74 17 17 GLN HA H 3.92 0.025 1 75 17 17 GLN HB2 H 2.20 0.0035 1 76 17 17 GLN HG2 H 2.13 0.0035 1 77 18 18 ASP H H 8.16 0.0035 1 78 18 18 ASP HA H 4.43 0.025 1 79 18 18 ASP HB2 H 2.69 0.025 2 80 18 18 ASP HB3 H 2.44 0.035 2 stop_ save_ ######################## # Coupling constants # ######################## save_coupling_constant_list_1 _Saveframe_category coupling_constants _Details . loop_ _Experiment_label '2D DQF-COSY' stop_ _Sample_conditions_label $sample_conditions_1 _Spectrometer_frequency_1H 600 _Mol_system_component_name 'Nociceptin Antagonist' _Text_data_format . _Text_data . loop_ _Coupling_constant_ID _Coupling_constant_code _Atom_one_residue_seq_code _Atom_one_residue_label _Atom_one_name _Atom_two_residue_seq_code _Atom_two_residue_label _Atom_two_name _Coupling_constant_value _Coupling_constant_min_value _Coupling_constant_max_value _Coupling_constant_value_error 1 3JHNHA 2 GLY H 2 GLY HA 5.5 . . . 2 3JHNHA 3 GLY H 3 GLY HA 6.0 . . . 3 3JHNHA 4 PHE H 4 PHE HA 6.9 . . . 4 3JHNHA 5 THR H 5 THR HA 6.8 . . . 5 3JHNHA 6 GLY H 6 GLY HA 6.2 . . . 6 3JHNHA 7 LYS H 7 LYS HA 3.9 . . . 7 3JHNHA 8 ARG H 8 ARG HA 4.0 . . . 8 3JHNHA 9 LYS H 9 LYS HA 5.4 . . . 9 3JHNHA 10 SER H 10 SER HA 4.5 . . . 10 3JHNHA 11 ASP H 11 ASP HA 4.7 . . . 11 3JHNHA 12 ARG H 12 ARG HA 5.2 . . . 12 3JHNHA 13 LYS H 13 LYS HA 6.0 . . . 13 3JHNHA 14 LYS H 14 LYS HA 4.6 . . . 14 3JHNHA 15 ALA H 15 ALA HA 4.7 . . . 15 3JHNHA 16 ASN H 16 ASN HA 5.0 . . . 16 3JHNHA 17 GLN H 17 GLN HA 5.7 . . . 17 3JHNHA 18 ASP H 18 ASP HA 6.9 . . . stop_ save_