data_18952 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Serine 16 phosphorylated phospholamban pentamer, Hybrid solution and solid-state NMR structural ensemble ; _BMRB_accession_number 18952 _BMRB_flat_file_name bmr18952.str _Entry_type original _Submission_date 2013-01-15 _Accession_date 2013-01-15 _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 Vostrikov Vitaly V. . 2 Verardi Raffaello . . 3 Veglia Gianluigi . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 49 "15N chemical shifts" 49 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2013-12-04 update author 'update entry citation' 2013-10-24 original author 'original release' stop_ save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title 'Structural Dynamics and Topology of Phosphorylated Phospholamban Homopentamer Reveal Its Role in the Regulation of Calcium Transport' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 24207128 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Vostrikov Vitaly V. . 2 Mote Kaustubh R. . 3 Verardi Raffaello . . 4 Veglia Gianluigi . . stop_ _Journal_abbreviation Structure _Journal_volume 21 _Journal_issue 12 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 2119 _Page_last 2130 _Year 2013 _Details 'doi 10.1016/j.str.2013.09.008' save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name Phospholamban _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label Phospholamban_1 $Phospholamban Phospholamban_2 $Phospholamban Phospholamban_3 $Phospholamban Phospholamban_4 $Phospholamban Phospholamban_5 $Phospholamban PHOSPHOSERINE $entity_SEP 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_Phospholamban _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common entity _Molecular_mass 6179.515 _Mol_thiol_state . _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 52 _Mol_residue_sequence ; MEKVQYLTRSAIRRAXTIEM PQQARQNLQNLFINFCLILI CLLLICIIVMLL ; loop_ _Residue_seq_code _Residue_label 1 MET 2 GLU 3 LYS 4 VAL 5 GLN 6 TYR 7 LEU 8 THR 9 ARG 10 SER 11 ALA 12 ILE 13 ARG 14 ARG 15 ALA 16 SEP 17 THR 18 ILE 19 GLU 20 MET 21 PRO 22 GLN 23 GLN 24 ALA 25 ARG 26 GLN 27 ASN 28 LEU 29 GLN 30 ASN 31 LEU 32 PHE 33 ILE 34 ASN 35 PHE 36 CYS 37 LEU 38 ILE 39 LEU 40 ILE 41 CYS 42 LEU 43 LEU 44 LEU 45 ILE 46 CYS 47 ILE 48 ILE 49 VAL 50 MET 51 LEU 52 LEU stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date 2015-08-19 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 2KYV "Hybrid Solution And Solid-state Nmr Structure Ensemble Of Phospholamban Pentamer" 100.00 52 98.08 98.08 3.95e-25 PDB 2M3B "Serine 16 Phosphorylated Phospholamban Pentamer, Hybrid Solution And Solid-state Nmr Structural Ensemble" 100.00 52 100.00 100.00 5.12e-25 DBJ BAB22237 "unnamed protein product [Mus musculus]" 100.00 52 98.08 98.08 3.95e-25 DBJ BAC30680 "unnamed protein product [Mus musculus]" 100.00 52 98.08 98.08 3.95e-25 DBJ BAC34880 "unnamed protein product [Mus musculus]" 100.00 52 98.08 98.08 3.95e-25 DBJ BAE25168 "unnamed protein product [Mus musculus]" 100.00 52 98.08 98.08 3.95e-25 EMBL CAA50394 "phospholamban [Rattus norvegicus]" 100.00 52 98.08 98.08 3.95e-25 EMBL CAA68730 "phospholamban [Oryctolagus cuniculus]" 100.00 52 98.08 98.08 3.95e-25 GB AAA31445 "phospholamban [Oryctolagus cuniculus]" 100.00 52 98.08 98.08 3.95e-25 GB AAA41849 "phospholamban [Rattus norvegicus]" 100.00 52 98.08 98.08 3.95e-25 GB AAB21903 "phospholamban [Rattus sp.]" 100.00 52 98.08 98.08 3.95e-25 GB AAB23706 "phospholamban [Mus sp.]" 100.00 52 98.08 98.08 3.95e-25 GB AAH61097 "Phospholamban [Mus musculus]" 100.00 52 98.08 98.08 3.95e-25 REF NP_001076090 "cardiac phospholamban [Oryctolagus cuniculus]" 100.00 52 98.08 98.08 3.95e-25 REF NP_001135399 "cardiac phospholamban [Mus musculus]" 100.00 52 98.08 98.08 3.95e-25 REF NP_001177823 "phospholamban [Macaca mulatta]" 100.00 52 98.08 98.08 3.95e-25 REF NP_073198 "cardiac phospholamban [Rattus norvegicus]" 100.00 52 98.08 98.08 3.95e-25 REF NP_075618 "cardiac phospholamban [Mus musculus]" 100.00 52 98.08 98.08 3.95e-25 SP P61014 "RecName: Full=Cardiac phospholamban; Short=PLB" 100.00 52 98.08 98.08 3.95e-25 SP P61015 "RecName: Full=Cardiac phospholamban; Short=PLB" 100.00 52 98.08 98.08 3.95e-25 SP P61016 "RecName: Full=Cardiac phospholamban; Short=PLB" 100.00 52 98.08 98.08 3.95e-25 stop_ save_ ###################### # Polymer residues # ###################### save_chem_comp_SEP _Saveframe_category polymer_residue _Mol_type 'L-PEPTIDE LINKING' _Name_common PHOSPHOSERINE _BMRB_code SEP _PDB_code SEP _Standard_residue_derivative . _Molecular_mass 185.072 _Mol_paramagnetic no _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons N N N . 0 . ? CA CA C . 0 . ? CB CB C . 0 . ? OG OG O . 0 . ? C C C . 0 . ? O O O . 0 . ? OXT OXT O . 0 . ? P P P . 0 . ? O1P O1P O . 0 . ? O2P O2P O . 0 . ? O3P O3P O . 0 . ? H H H . 0 . ? H2 H2 H . 0 . ? HA HA H . 0 . ? HB2 HB2 H . 0 . ? HB3 HB3 H . 0 . ? HXT HXT H . 0 . ? HOP2 HOP2 H . 0 . ? HOP3 HOP3 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 CA ? ? SING N H ? ? SING N H2 ? ? SING CA CB ? ? SING CA C ? ? SING CA HA ? ? SING CB OG ? ? SING CB HB2 ? ? SING CB HB3 ? ? SING OG P ? ? DOUB C O ? ? SING C OXT ? ? SING OXT HXT ? ? DOUB P O1P ? ? SING P O2P ? ? SING P O3P ? ? SING O2P HOP2 ? ? SING O3P HOP3 ? ? stop_ save_ ############# # Ligands # ############# save_SEP _Saveframe_category ligand _Mol_type non-polymer _Name_common PHOSPHOSERINE _Molecular_mass 185.072 _Details . _Mol_thiol_state 'not present' _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 $Phospholamban rabbit 9986 Eukaryota Metazoa Oryctolagus cuniculus 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 $Phospholamban 'recombinant technology' . Escherichia coli 'BL21 DE3' pMAL-c2X 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 $Phospholamban 0.1 mM '[U-100% 13C; U-100% 15N]' DPC 300 mM [U-2H] 'sodium phosphate' 20 mM 'natural abundance' 'sodium chloride' 120 mM 'natural abundance' beta-mercaptoethanol 10 mM 'natural abundance' 'sodium azide' 0.02 % 'natural abundance' H2O 95 % 'natural abundance' D2O 5 % 'natural abundance' stop_ save_ save_sample_2 _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $Phospholamban 0.15 mM '[U-13C; U-15N; U-2H]' DPC 300 mM 'natural abundance' 'sodium phosphate' 20 mM 'natural abundance' 'sodium chloride' 120 mM 'natural abundance' beta-mercaptoethanol 10 mM 'natural abundance' 'sodium azide' 0.02 % 'natural abundance' H2O 95 % 'natural abundance' D2O 5 % 'natural abundance' stop_ save_ save_sample_3 _Saveframe_category sample _Sample_type 'oriented membrane film' _Details 'Multiple samples with selective 15N labeling' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $Phospholamban 4 mg '[U-100% 15N]' DOPC 38 mg 'natural abundance' DOPE 9 mg 'natural abundance' D2O 100 % 'natural abundance' stop_ save_ save_sample_4 _Saveframe_category sample _Sample_type membrane _Details 'Physical mixture of 13C/15N-Leu and 13C/15N-Ile samples' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $Phospholamban 1 mg '[U-100% 13C; U-100% 15N]' DOPC 12 mg 'natural abundance' DOPE 3 mg 'natural abundance' MOPS 20 mM 'natural abundance' 'sodium chloride' 50 mM 'natural abundance' 'sodium azide' 0.02 % 'natural abundance' D2O 100 % 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_NMRPipe _Saveframe_category software _Name NMRPipe _Version 7.4 loop_ _Vendor _Address _Electronic_address 'Delaglio, Grzesiek, Vuister, Zhu, Pfeifer and Bax' . . stop_ loop_ _Task processing stop_ _Details . save_ save_SPARKY _Saveframe_category software _Name SPARKY _Version 3.114 loop_ _Vendor _Address _Electronic_address Goddard . . stop_ loop_ _Task 'data analysis' stop_ _Details . save_ save_Molprobity _Saveframe_category software _Name MolProbity _Version . loop_ _Vendor _Address _Electronic_address 'David C. Richardson' . . stop_ loop_ _Task 'data analysis' stop_ _Details . save_ save_PSVS _Saveframe_category software _Name PSVS _Version . loop_ _Vendor _Address _Electronic_address 'Bhattacharya and Montelione' . . stop_ loop_ _Task 'data analysis' stop_ _Details . save_ save_X-PLOR_NIH _Saveframe_category software _Name 'X-PLOR NIH' _Version 2.33 loop_ _Vendor _Address _Electronic_address 'Schwieters, Kuszewski, Tjandra and Clore' . . stop_ loop_ _Task 'structure solution' stop_ _Details . save_ save_TALOS _Saveframe_category software _Name TALOS _Version . loop_ _Vendor _Address _Electronic_address 'Cornilescu, Delaglio and Bax' . . stop_ loop_ _Task 'data analysis' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Varian _Model INOVA _Field_strength 600 _Details . save_ save_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer Varian _Model INOVA _Field_strength 700 _Details . save_ save_spectrometer_3 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model DMX _Field_strength 600 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-15N_HSQC_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample_1 save_ save_3D_1H-15N_NOESY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 1H-15N NOESY' _Sample_label $sample_1 save_ save_3D_1H-15N_NOESY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 1H-15N NOESY' _Sample_label $sample_2 save_ save_2D_PISEMA_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D PISEMA' _Sample_label $sample_3 save_ save_2D_DARR_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D DARR' _Sample_label $sample_4 save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 6 . pH temperature 273 . K stop_ save_ save_sample_conditions_2 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 7 . pH temperature 273 . K stop_ save_ save_sample_conditions_3 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 7 . 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 4.7 internal direct . . . 1.0 DSS N 15 'methyl protons' ppm 0.00 na 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 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-15N HSQC' '2D PISEMA' stop_ loop_ _Sample_label $sample_1 $sample_3 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name Phospholamban_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 2 2 GLU H H 9.24 . 1 2 2 2 GLU N N 121.80 . 1 3 3 3 LYS H H 8.27 . 1 4 3 3 LYS N N 120.20 . 1 5 4 4 VAL H H 7.75 . 1 6 4 4 VAL N N 117.60 . 1 7 5 5 GLN H H 8.19 . 1 8 5 5 GLN N N 120.80 . 1 9 6 6 TYR H H 8.02 . 1 10 6 6 TYR N N 119.30 . 1 11 7 7 LEU H H 8.11 . 1 12 7 7 LEU N N 120.40 . 1 13 8 8 THR H H 7.89 . 1 14 8 8 THR N N 111.20 . 1 15 9 9 ARG H H 8.22 . 1 16 9 9 ARG N N 120.70 . 1 17 10 10 SER H H 7.99 . 1 18 10 10 SER N N 114.50 . 1 19 11 11 ALA H H 8.06 . 1 20 11 11 ALA N N 124.00 . 1 21 12 12 ILE H H 7.78 . 1 22 12 12 ILE N N 115.90 . 1 23 13 13 ARG H H 7.91 . 1 24 13 13 ARG N N 121.10 . 1 25 14 14 ARG H H 8.06 . 1 26 14 14 ARG N N 120.27 . 1 27 15 15 ALA H H 8.23 . 1 28 15 15 ALA N N 123.90 . 1 29 16 16 SEP H H 8.42 . 1 30 16 16 SEP N N 113.00 . 1 31 17 17 THR H H 7.82 . 1 32 17 17 THR N N 113.00 . 1 33 18 18 ILE H H 7.72 . 1 34 18 18 ILE N N 122.10 . 1 35 19 19 GLU H H 8.25 . 1 36 19 19 GLU N N 124.80 . 1 37 20 20 MET H H 8.48 . 1 38 20 20 MET N N 122.70 . 1 39 22 22 GLN H H 8.71 . 1 40 22 22 GLN N N 121.60 . 1 41 23 23 GLN H H 8.62 . 1 42 23 23 GLN N N 119.00 . 1 43 24 24 ALA H H 7.84 . 1 44 24 24 ALA N N 122.40 . 1 45 26 26 GLN H H 8.78 . 1 46 26 26 GLN N N 118.34 . 1 47 27 27 ASN H H 8.00 . 1 48 27 27 ASN N N 117.92 . 1 49 28 28 LEU H H 8.21 . 1 50 28 28 LEU N N 121.40 . 1 51 29 29 GLN H H 8.13 . 1 52 29 29 GLN N N 117.93 . 1 53 30 30 ASN H H 8.10 . 1 54 30 30 ASN N N 117.04 . 1 55 31 31 LEU H H 8.06 . 1 56 31 31 LEU N N 121.20 . 1 57 32 32 PHE H H 8.45 . 1 58 32 32 PHE N N 118.31 . 1 59 33 33 ILE H H 8.42 . 1 60 33 33 ILE N N 119.70 . 1 61 34 34 ASN H H 8.03 . 1 62 34 34 ASN N N 117.58 . 1 63 35 35 PHE H H 8.57 . 1 64 35 35 PHE N N 119.40 . 1 65 36 36 CYS H H 8.16 . 1 66 36 36 CYS N N 116.68 . 1 67 37 37 LEU H H 8.17 . 1 68 37 37 LEU N N 118.19 . 1 69 38 38 ILE H H 8.39 . 1 70 38 38 ILE N N 119.70 . 1 71 39 39 LEU H H 7.99 . 1 72 39 39 LEU N N 119.40 . 1 73 40 40 ILE H H 8.14 . 1 74 40 40 ILE N N 119.25 . 1 75 41 41 CYS H H 7.98 . 1 76 41 41 CYS N N 117.80 . 1 77 42 42 LEU H H 8.29 . 1 78 42 42 LEU N N 117.90 . 1 79 43 43 LEU H H 8.39 . 1 80 43 43 LEU N N 119.70 . 1 81 44 44 LEU H H 8.18 . 1 82 44 44 LEU N N 117.80 . 1 83 45 45 ILE H H 8.17 . 1 84 45 45 ILE N N 117.69 . 1 85 46 46 CYS H H 8.15 . 1 86 46 46 CYS N N 117.02 . 1 87 47 47 ILE H H 8.23 . 1 88 47 47 ILE N N 117.30 . 1 89 48 48 ILE H H 8.20 . 1 90 48 48 ILE N N 117.69 . 1 91 49 49 VAL H H 8.34 . 1 92 49 49 VAL N N 115.70 . 1 93 50 50 MET H H 7.92 . 1 94 50 50 MET N N 115.50 . 1 95 51 51 LEU H H 7.88 . 1 96 51 51 LEU N N 118.10 . 1 97 52 52 LEU H H 7.29 . 1 98 52 52 LEU N N 123.40 . 1 stop_ save_