data_11550 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Active-Site Structure of the Thermophilic Foc-Subunit Ring in Membranes Elucidated by Solid-State NMR ; _BMRB_accession_number 11550 _BMRB_flat_file_name bmr11550.str _Entry_type original _Submission_date 2014-02-10 _Accession_date 2014-02-11 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details 'Thermophilic Foc-Subunit Ring in Membranes' loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Kang Su-Jin . . 2 Yasuto Todokoro . . 3 Akustu Hideo . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 spectral_peak_list 4 stop_ loop_ _Data_type _Data_type_count "13C chemical shifts" 19 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2017-08-03 original BMRB . stop_ _Original_release_date 2014-02-11 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; Active-site structure of the thermophilic foc-subunit ring in membranes elucidated by solid-state NMR ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 24461014 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Kang Su-Jin . . 2 Yasuto Todokoro . . 3 Ikuko Yumen . . 4 Bo Shen . . 5 Iku Iwasaki . . 6 Toshiharu Suzuki . . 7 Atsushi Miyagi . . 8 Masasuke Yoshida . . 9 Toshimichi Fujiwara . . 10 Akutsu Hideo . . stop_ _Journal_abbreviation 'Biophys J.' _Journal_volume 106 _Journal_issue 2 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 390 _Page_last 398 _Year 2014 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'thermophilic Fo subunit c ring in membranes' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label Foc-subunit_1 $subunit_c_of_thermophilic_FoF1_ATP_synthase Foc-subunit_2 $subunit_c_of_thermophilic_FoF1_ATP_synthase Foc-subunit_3 $subunit_c_of_thermophilic_FoF1_ATP_synthase Foc-subunit_4 $subunit_c_of_thermophilic_FoF1_ATP_synthase Foc-subunit_5 $subunit_c_of_thermophilic_FoF1_ATP_synthase Foc-subunit_6 $subunit_c_of_thermophilic_FoF1_ATP_synthase Foc-subunit_7 $subunit_c_of_thermophilic_FoF1_ATP_synthase Foc-subunit_8 $subunit_c_of_thermophilic_FoF1_ATP_synthase Foc-subunit_9 $subunit_c_of_thermophilic_FoF1_ATP_synthase Foc-subunit_10 $subunit_c_of_thermophilic_FoF1_ATP_synthase 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_subunit_c_of_thermophilic_FoF1_ATP_synthase _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common 'subunit c of thermophilic FoF1 ATP synthase' _Molecular_mass . _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 72 _Mol_residue_sequence ; MHLGVLAAAIAVGLGALGAG IGNGLIVSRTIEGIARQPEL RPVLQTTMFIGVALVEALPI IGVVFSFIYLGR ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 1 MET 2 2 HIS 3 3 LEU 4 4 GLY 5 5 VAL 6 6 LEU 7 7 ALA 8 8 ALA 9 9 ALA 10 10 ILE 11 11 ALA 12 12 VAL 13 13 GLY 14 14 LEU 15 15 GLY 16 16 ALA 17 17 LEU 18 18 GLY 19 19 ALA 20 20 GLY 21 21 ILE 22 22 GLY 23 23 ASN 24 24 GLY 25 25 LEU 26 26 ILE 27 27 VAL 28 28 SER 29 29 ARG 30 30 THR 31 31 ILE 32 32 GLU 33 33 GLY 34 34 ILE 35 35 ALA 36 36 ARG 37 37 GLN 38 38 PRO 39 39 GLU 40 40 LEU 41 41 ARG 42 42 PRO 43 43 VAL 44 44 LEU 45 45 GLN 46 46 THR 47 47 THR 48 48 MET 49 49 PHE 50 50 ILE 51 51 GLY 52 52 VAL 53 53 ALA 54 54 LEU 55 55 VAL 56 56 GLU 57 57 ALA 58 58 LEU 59 59 PRO 60 60 ILE 61 61 ILE 62 62 GLY 63 63 VAL 64 64 VAL 65 65 PHE 66 66 SER 67 67 PHE 68 68 ILE 69 69 TYR 70 70 LEU 71 71 GLY 72 72 ARG 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 $subunit_c_of_thermophilic_FoF1_ATP_synthase 'Bacillus sp. PS3' 2334 Bacteria . Bacillus . 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 $subunit_c_of_thermophilic_FoF1_ATP_synthase 'recombinant technology' 'bread wheat' Triticum aestivum . pZA01MCS-SP6P stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solid _Details 'solid-state NMR sample in dimyristoyl phosphatidylcholine membrane' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $subunit_c_of_thermophilic_FoF1_ATP_synthase 2.8 mg '[U-100% 13C; U-100% 15N; U-80% 2H]' D2O 100 % . Tris-DCl 10 mM . stop_ save_ ############################ # Computer software used # ############################ save_SPARKY _Saveframe_category software _Name SPARKY _Version . 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 Varian _Model infinity-plus _Field_strength 700 _Details . save_ save_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer Varian _Model infinity-plus _Field_strength 600 _Details . save_ ############################# # NMR applied experiments # ############################# save_DARR_1 _Saveframe_category NMR_applied_experiment _Experiment_name DARR _Sample_label $sample_1 save_ save_DARR_2 _Saveframe_category NMR_applied_experiment _Experiment_name DARR _Sample_label $sample_1 save_ save_Cai+1-(C'Ca)_correlation_3 _Saveframe_category NMR_applied_experiment _Experiment_name "Cai+1-(C'Ca) correlation" _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 'ionic strength' 0.010 . M pH 7.5 . pH pressure 1 . atm temperature 298 . 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 adamantan C 13 'methine carbon' ppm 40.5 external direct . . . 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 _Saveframe_category assigned_chemical_shifts _Details ; _Systematic_chem_shift_offset: SAIL isotope labeling: all ASN CA: 0.04 all ASN CB: 0.27 all GLU CA: 0.07 all GLU CB: 0.40 all GLU CG: 0.35 ; loop_ _Experiment_label DARR "Cai+1-(C'Ca) correlation" 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 Foc-subunit_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 23 23 ASN C C 178.2 0.3 1 2 23 23 ASN CA C 55.3 0.3 1 3 23 23 ASN CB C 36.9 0.4 1 4 23 23 ASN CG C 170.7 0.5 1 5 32 32 GLU C C 178.9 0.3 1 6 32 32 GLU CA C 58.4 0.3 1 7 32 32 GLU CB C 30.0 0.5 1 8 32 32 GLU CD C 183.1 0.5 1 9 32 32 GLU CG C 34.5 0.3 1 10 39 39 GLU C C 177.8 0.4 1 11 39 39 GLU CA C 57.8 0.2 1 12 39 39 GLU CB C 30.7 0.6 1 13 39 39 GLU CD C 182.6 0.3 1 14 39 39 GLU CG C 35.8 0.2 1 15 56 56 GLU C C 177.6 0.4 1 16 56 56 GLU CA C 57.3 0.4 1 17 56 56 GLU CB C 27.4 0.6 1 18 56 56 GLU CD C 174.5 0.7 1 19 56 56 GLU CG C 31.0 1.1 1 stop_ save_ save_spectral_peak_list_1 _Saveframe_category spectral_peak_list _Details . _Experiment_label DARR _Number_of_spectral_dimensions 2 loop_ _Expt_dimension_ID _Atom_type _Spectral_region 1 C 'Ca, Cb, Cg, Cd, Co' 2 C 'Ca, Cb, Cg, Cd, Co' stop_ _Sample_label $sample_1 _Sample_conditions_label $sample_conditions_1 _Text_data_format "NMR-STAR v3" _Text_data ; >>save_spectral_peak_list_1 >> _Spectral_peak_list.Sf_category spectral_peak_list >> _Spectral_peak_list.Sf_framecode spectral_peak_list_1 >> _Spectral_peak_list.Entry_ID 11550 >> _Spectral_peak_list.ID 1 >> _Spectral_peak_list.Sample_ID 1 >> _Spectral_peak_list.Sample_label $sample_1 >> _Spectral_peak_list.Sample_condition_list_ID 1 >> _Spectral_peak_list.Sample_condition_list_label $sample_conditions_1 >> _Spectral_peak_list.Experiment_ID 1 >> _Spectral_peak_list.Experiment_name DARR >> _Spectral_peak_list.Number_of_spectral_dimensions 2 >> _Spectral_peak_list.Details . >> _Spectral_peak_list.Text_data_format text >> _Spectral_peak_list.Text_data >>; >>Assignment w1 w2 >> >> 23Nca-cb 55.3 36.9 >> N23cg-cb 169.950 36.9 >> N23co-ca 177.694 55.3 >> N23co-ca 170.025 55.3 >> N23co-cb 177.694 36.9 >> E32cd-cg 182.204 34.5 >> E39cd-cg 181.377 35.8 >> E56cd-cg 173.333 31.0 >>; >> >> loop_ >> _Spectral_dim.ID >> _Spectral_dim.Atom_type >> _Spectral_dim.Atom_isotope_number >> _Spectral_dim.Spectral_region >> _Spectral_dim.Magnetization_linkage_ID >> _Spectral_dim.Under_sampling_type >> _Spectral_dim.Sweep_width >> _Spectral_dim.Sweep_width_units >> _Spectral_dim.Center_frequency_offset >> _Spectral_dim.Encoding_code >> _Spectral_dim.Encoded_source_dimension_ID >> _Spectral_dim.Entry_ID >> _Spectral_dim.Spectral_peak_list_ID >> >> 1 C 13 'Ca, Cb, Cg, Cd, Co' . . 100000 . . . . 11550 1 >> 2 C 13 'Ca, Cb, Cg, Cd, Co' . . 100000 . . . . 11550 1 >> >> stop_ >> >>save_ >> ; save_ save_spectral_peak_list_2 _Saveframe_category spectral_peak_list _Details . _Experiment_label DARR _Number_of_spectral_dimensions 2 loop_ _Expt_dimension_ID _Atom_type _Spectral_region 1 C 'Ca, Cb, Cg, Cd, Co' 2 C 'Ca, Cb, Cg, Cd, Co' stop_ _Sample_label $sample_1 _Sample_conditions_label $sample_conditions_1 _Text_data_format "NMR-STAR v3" _Text_data ; >>save_spectral_peak_list_2 >> _Spectral_peak_list.Sf_category spectral_peak_list >> _Spectral_peak_list.Sf_framecode spectral_peak_list_2 >> _Spectral_peak_list.Entry_ID 11550 >> _Spectral_peak_list.ID 2 >> _Spectral_peak_list.Sample_ID 1 >> _Spectral_peak_list.Sample_label $sample_1 >> _Spectral_peak_list.Sample_condition_list_ID 1 >> _Spectral_peak_list.Sample_condition_list_label $sample_conditions_1 >> _Spectral_peak_list.Experiment_ID 1 >> _Spectral_peak_list.Experiment_name DARR >> _Spectral_peak_list.Number_of_spectral_dimensions 2 >> _Spectral_peak_list.Details . >> _Spectral_peak_list.Text_data_format text >> _Spectral_peak_list.Text_data >>; >>Assignment w1 w2 >> >> 23Nca-cb 55.3 36.9 >> 23Ncb-ca 36.9 55.3 >> 23Ncg-ca 170.540 55.3 >> 23Ncg-cb 170.474 36.9 >> 23Ncg-co 170.540 178.248 >> 23Nco-ca 178.281 55.455 >> 23Nco-cb 178.215 36.9 >> 32Eca-cb 58.4 30.0 >> 32Ecb-ca 30.0 58.4 >> 32Ecd-ca 182.912 58.4 >> 32Ecd-cg 182.912 34.5 >> 32Ecg-ca 34.449 58.4 >> 32Eco-ca 178.612 58.4 >> 32Eco-cb 178.545 30.0 >> 32Eco-cg 178.744 34.5 >> 39Ecb-ca 30.7 57.8 >> 39Ecd-cg 182.184 35.8 >> 39Eco-ca 177.421 57.8 >> 39Eco-cb 177.487 30.7 >> 39Eco-cg 177.487 35.8 >> 56Eca-cb 57.3 27.4 >> 56Ecb-ca 27.4 57.3 >> 56Ecd-ca 174.708 57.3 >> 56Ecd-cb 174.774 27.4 >> 56Ecd-cg 174.708 31.0 >> 56Eco-ca 177.090 57.3 >> 56Eco-cb 177.156 27.4 >> 56Eco-cg 177.156 31.0 >>; >> >> loop_ >> _Spectral_dim.ID >> _Spectral_dim.Atom_type >> _Spectral_dim.Atom_isotope_number >> _Spectral_dim.Spectral_region >> _Spectral_dim.Magnetization_linkage_ID >> _Spectral_dim.Under_sampling_type >> _Spectral_dim.Sweep_width >> _Spectral_dim.Sweep_width_units >> _Spectral_dim.Center_frequency_offset >> _Spectral_dim.Encoding_code >> _Spectral_dim.Encoded_source_dimension_ID >> _Spectral_dim.Entry_ID >> _Spectral_dim.Spectral_peak_list_ID >> >> 1 C 13 'Ca, Cb, Cg, Cd, Co' . . 100000 . . . . 11550 2 >> 2 C 13 'Ca, Cb, Cg, Cd, Co' . . 100000 . . . . 11550 2 >> >> stop_ >> >>save_ >> ; save_ save_spectral_peak_list_3 _Saveframe_category spectral_peak_list _Details . _Experiment_label DARR _Number_of_spectral_dimensions 2 loop_ _Expt_dimension_ID _Atom_type _Spectral_region 1 C 'Ca, Cb, Cg, Cd, Co' 2 C 'Ca, Cb, Cg, Cd, Co' stop_ _Sample_label $sample_1 _Sample_conditions_label $sample_conditions_1 _Text_data_format "NMR-STAR v3" _Text_data ; >>save_spectral_peak_list_3 >> _Spectral_peak_list.Sf_category spectral_peak_list >> _Spectral_peak_list.Sf_framecode spectral_peak_list_3 >> _Spectral_peak_list.Entry_ID 11550 >> _Spectral_peak_list.ID 3 >> _Spectral_peak_list.Sample_ID 1 >> _Spectral_peak_list.Sample_label $sample_1 >> _Spectral_peak_list.Sample_condition_list_ID 1 >> _Spectral_peak_list.Sample_condition_list_label $sample_conditions_1 >> _Spectral_peak_list.Experiment_ID 1 >> _Spectral_peak_list.Experiment_name DARR >> _Spectral_peak_list.Number_of_spectral_dimensions 2 >> _Spectral_peak_list.Details . >> _Spectral_peak_list.Text_data_format text >> _Spectral_peak_list.Text_data >>; >>Assignment w1 w2 >> >> N23cb-ca 36.9 55.3 >> N23cg-ca 170.852 55.3 >> N23cg-cb 170.852 36.9 >> E32cb-ca 30.0 58.4 >> E32cd-cb 183.414 30.0 >> E32cd-cg 183.414 34.5 >> E32cg-ca 34.451 58.4 >> E32co-cb 179.060 30.0 >> E56cb-ca 27.4 57.3 >> E56cd-ca 174.849 57.3 >> E56cg-ca 31.0 57.3 >> E56co-cb 177.704 27.4 >>; >> >> loop_ >> _Spectral_dim.ID >> _Spectral_dim.Atom_type >> _Spectral_dim.Atom_isotope_number >> _Spectral_dim.Spectral_region >> _Spectral_dim.Magnetization_linkage_ID >> _Spectral_dim.Under_sampling_type >> _Spectral_dim.Sweep_width >> _Spectral_dim.Sweep_width_units >> _Spectral_dim.Center_frequency_offset >> _Spectral_dim.Encoding_code >> _Spectral_dim.Encoded_source_dimension_ID >> _Spectral_dim.Entry_ID >> _Spectral_dim.Spectral_peak_list_ID >> >> 1 C 13 'Ca, Cb, Cg, Cd, Co' . . 70000 . . . . 11550 3 >> 2 C 13 'Ca, Cb, Cg, Cd, Co' . . 70000 . . . . 11550 3 >> >> stop_ >> >>save_ >> ; save_ save_spectral_peak_list_4 _Saveframe_category spectral_peak_list _Details . _Experiment_label DARR _Number_of_spectral_dimensions 2 loop_ _Expt_dimension_ID _Atom_type _Spectral_region 1 C 'Ca, Cb, Cg, Cd, Co' 2 C 'Ca, Cb, Cg, Cd, Co' stop_ _Sample_label $sample_1 _Sample_conditions_label $sample_conditions_1 _Text_data_format "NMR-STAR v3" _Text_data ; >>save_spectral_peak_list_4 >> _Spectral_peak_list.Sf_category spectral_peak_list >> _Spectral_peak_list.Sf_framecode spectral_peak_list_4 >> _Spectral_peak_list.Entry_ID 11550 >> _Spectral_peak_list.ID 4 >> _Spectral_peak_list.Sample_ID 1 >> _Spectral_peak_list.Sample_label $sample_1 >> _Spectral_peak_list.Sample_condition_list_ID 1 >> _Spectral_peak_list.Sample_condition_list_label $sample_conditions_1 >> _Spectral_peak_list.Experiment_ID 1 >> _Spectral_peak_list.Experiment_name DARR >> _Spectral_peak_list.Number_of_spectral_dimensions 2 >> _Spectral_peak_list.Details . >> _Spectral_peak_list.Text_data_format text >> _Spectral_peak_list.Text_data >>; >>Assignment w1 w2 >> >> 23Nca-cb 55.3 36.9 >> 23Ncg-cb 170.424 36.9 >> 23Ncg-56Ecb 170.587 27.4 >> 23Ncg-56Ecg 170.342 31.0 >> 23Nco-ca 170.424 55.3 >> 23Nco-cg 178.274 170.628 >> 32Eca-cb 58.4 30.0 >> 32Eca-cg 58.4 34.5 >> 56Eca-cb 57.3 27.4 >> 56Ecd-23Ncg 174.513 170.546 >> 56Ecd-cb 174.840 27.4 >> 56Ecd-cg 174.840 31.0 >>; >> >> loop_ >> _Spectral_dim.ID >> _Spectral_dim.Atom_type >> _Spectral_dim.Atom_isotope_number >> _Spectral_dim.Spectral_region >> _Spectral_dim.Magnetization_linkage_ID >> _Spectral_dim.Under_sampling_type >> _Spectral_dim.Sweep_width >> _Spectral_dim.Sweep_width_units >> _Spectral_dim.Center_frequency_offset >> _Spectral_dim.Encoding_code >> _Spectral_dim.Encoded_source_dimension_ID >> _Spectral_dim.Entry_ID >> _Spectral_dim.Spectral_peak_list_ID >> >> 1 C 13 'Ca, Cb, Cg, Cd, Co' . . 100000 . . . . 11550 4 >> 2 C 13 'Ca, Cb, Cg, Cd, Co' . . 100000 . . . . 11550 4 >> >> stop_ >> >>save_ >> ; save_