data_6627 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Structure of cyclotide Kalata B1 in DPC micelles solution ; _BMRB_accession_number 6627 _BMRB_flat_file_name bmr6627.str _Entry_type original _Submission_date 2005-05-12 _Accession_date 2005-05-12 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details ; Both 1H chemical shifts for DPC solution, and 1H 13C chemical shifts for D2O solution (natural abundance) ; loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Shenkarev Zakhar O. . 2 Nadezhdin Kirill D. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 2 coupling_constants 2 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 251 "13C chemical shifts" 111 "coupling constants" 100 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2006-08-07 original author . stop_ loop_ _Related_BMRB_accession_number _Relationship 5114 'structure of KB1 in aqueous solution (ladder)' 5609 'NMR structure of [Ala1,15]kalata B1 (knot)' stop_ _Original_release_date 2006-08-07 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title 'Conformation and mode of membrane interaction in cyclotides' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 16817894 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Shenkarev Zakhar O. . 2 Nadezhdin Kirill D. . 3 Sobol Vladimir A. . 4 Sobol Alexander G. . 5 Skjeldal Lars . . 6 Arseniev Alexander S. . stop_ _Journal_abbreviation 'FEBS J.' _Journal_volume 273 _Journal_issue 12 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 2658 _Page_last 2672 _Year 2006 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'Kalata B1' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label 'Kalata B1' $KB1 stop_ _System_molecular_weight 2892 _System_physical_state native _System_oligomer_state protein _System_paramagnetic no _System_thiol_state 'all disulfide bound' loop_ _Biological_function antimicrobial antiviral cytotoxic 'defence peptide' hemolitic insecticidal stop_ _Database_query_date . _Details 'cyclotide in DPC (or aqueous) solution' save_ ######################## # Monomeric polymers # ######################## save_KB1 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common 'Kalata B1' _Molecular_mass . _Mol_thiol_state 'all disulfide bound' loop_ _Biological_function antimicrobial antiviral cytotoxic 'defence peptide' hemolitic insecticidal stop_ _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 29 _Mol_residue_sequence ; CGETCVGGTCNTPGCTCSWP VCTRNGLPV ; loop_ _Residue_seq_code _Residue_label 1 CYS 2 GLY 3 GLU 4 THR 5 CYS 6 VAL 7 GLY 8 GLY 9 THR 10 CYS 11 ASN 12 THR 13 PRO 14 GLY 15 CYS 16 THR 17 CYS 18 SER 19 TRP 20 PRO 21 VAL 22 CYS 23 THR 24 ARG 25 ASN 26 GLY 27 LEU 28 PRO 29 VAL 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 $KB1 'Oldenlandia affinis' 60225 Eukaryota Viridiplantae Rubiaceae Oldenlandia 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 $KB1 'Purified from the natural source' . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type micelle _Details 'DPC micelles P:D=1.60' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $KB1 3.6 mM . DPC 216 mM '[U-98% 2D]' D2O 10 % . H2O 90 % . stop_ save_ save_sample_2 _Saveframe_category sample _Sample_type solution _Details 'D2O 100%' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $KB1 3.6 mM . D2O 100 % . stop_ save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_Varian_600MHz_UNITY _Saveframe_category NMR_spectrometer _Manufacturer Varian _Model UNITY _Field_strength 600 _Details . save_ save_Bruker_500MHz_DRX _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model DRX _Field_strength 500 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_NOESY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D NOESY' _Sample_label . save_ save_2D_TOCSY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D TOCSY' _Sample_label . save_ save_DQF_COSY_3 _Saveframe_category NMR_applied_experiment _Experiment_name 'DQF COSY' _Sample_label . save_ save_1H13C_HSQC_4 _Saveframe_category NMR_applied_experiment _Experiment_name '1H13C HSQC' _Sample_label . save_ save_HMBC_5 _Saveframe_category NMR_applied_experiment _Experiment_name HMBC _Sample_label . save_ save_NOESY_-_infit_6 _Saveframe_category NMR_applied_experiment _Experiment_name 'NOESY - infit' _Sample_label . save_ save_COSY_-acme_7 _Saveframe_category NMR_applied_experiment _Experiment_name 'COSY -acme' _Sample_label . save_ save_long-range_band_selective_HMQC_8 _Saveframe_category NMR_applied_experiment _Experiment_name 'long-range band selective HMQC' _Sample_label . save_ save_quantitative_J_correlation_9 _Saveframe_category NMR_applied_experiment _Experiment_name 'quantitative J correlation' _Sample_label . save_ save_1H13C_HSQC _Saveframe_category NMR_applied_experiment _Experiment_name 1H13C_HSQC _BMRB_pulse_sequence_accession_number . _Details . save_ ####################### # Sample conditions # ####################### save_conditions_1 _Saveframe_category sample_conditions _Details 'for DPC micelles solution' loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 0 0 M pH 2.8 0.1 pH temperature 313 1 K stop_ save_ save_conditions_2 _Saveframe_category sample_conditions _Details 'for D2O solution' loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 0 0 M pH 2.8 0.1 pH temperature 313 1 K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chemical_shift_referencing _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 H2O C 13 protons ppm 4.65 internal indirect . . . 0.251449530 H2O H 1 protons ppm 4.65 internal 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_chem_shift_list_1 _Saveframe_category assigned_chemical_shifts _Details 'DPC micelles' loop_ _Experiment_label '2D NOESY' '2D TOCSY' 'DQF COSY' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $conditions_1 _Chem_shift_reference_set_label $chemical_shift_referencing _Mol_system_component_name 'Kalata B1' _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 CYS H H 7.65 0.02 1 2 1 1 CYS HA H 4.51 0.02 1 3 1 1 CYS HB2 H 3.36 0.02 2 4 1 1 CYS HB3 H 3.07 0.02 2 5 2 2 GLY H H 8.65 0.02 1 6 2 2 GLY HA2 H 3.77 0.02 2 7 2 2 GLY HA3 H 3.91 0.02 2 8 3 3 GLU H H 7.10 0.02 1 9 3 3 GLU HA H 4.90 0.02 1 10 3 3 GLU HB2 H 2.14 0.02 2 11 3 3 GLU HB3 H 1.87 0.02 2 12 3 3 GLU HG2 H 2.73 0.02 2 13 3 3 GLU HG3 H 2.59 0.02 2 14 4 4 THR H H 8.50 0.02 1 15 4 4 THR HA H 4.54 0.02 1 16 4 4 THR HB H 4.50 0.02 1 17 4 4 THR HG2 H 1.15 0.02 1 18 5 5 CYS H H 8.32 0.02 1 19 5 5 CYS HA H 5.06 0.02 1 20 5 5 CYS HB2 H 2.76 0.02 2 21 5 5 CYS HB3 H 3.36 0.02 2 22 6 6 VAL H H 9.33 0.02 1 23 6 6 VAL HA H 3.64 0.02 1 24 6 6 VAL HB H 2.21 0.02 1 25 6 6 VAL HG1 H 1.16 0.02 2 26 6 6 VAL HG2 H 1.02 0.02 2 27 7 7 GLY H H 9.02 0.02 1 28 7 7 GLY HA2 H 4.35 0.02 2 29 7 7 GLY HA3 H 3.83 0.02 2 30 8 8 GLY H H 8.09 0.02 1 31 8 8 GLY HA2 H 4.13 0.02 2 32 8 8 GLY HA3 H 4.50 0.02 2 33 9 9 THR H H 7.94 0.02 1 34 9 9 THR HA H 4.71 0.02 1 35 9 9 THR HB H 4.06 0.02 1 36 9 9 THR HG2 H 1.18 0.02 1 37 10 10 CYS H H 8.71 0.02 1 38 10 10 CYS HA H 4.66 0.02 1 39 10 10 CYS HB2 H 2.84 0.02 2 40 10 10 CYS HB3 H 3.03 0.02 2 41 11 11 ASN H H 9.31 0.02 1 42 11 11 ASN HA H 4.79 0.02 1 43 11 11 ASN HB2 H 2.87 0.02 1 44 11 11 ASN HB3 H 2.87 0.02 1 45 11 11 ASN HD21 H 7.63 0.02 2 46 11 11 ASN HD22 H 6.95 0.02 2 47 12 12 THR H H 8.15 0.02 1 48 12 12 THR HA H 4.58 0.02 1 49 12 12 THR HB H 4.19 0.02 1 50 12 12 THR HG2 H 1.37 0.02 1 51 13 13 PRO HA H 4.30 0.02 1 52 13 13 PRO HB2 H 1.95 0.02 2 53 13 13 PRO HB3 H 2.35 0.02 2 54 13 13 PRO HG2 H 2.17 0.02 2 55 13 13 PRO HG3 H 2.05 0.02 2 56 13 13 PRO HD2 H 3.75 0.02 2 57 13 13 PRO HD3 H 4.14 0.02 2 58 14 14 GLY H H 8.72 0.02 1 59 14 14 GLY HA2 H 3.75 0.02 2 60 14 14 GLY HA3 H 4.20 0.02 2 61 15 15 CYS H H 7.69 0.02 1 62 15 15 CYS HA H 5.38 0.02 1 63 15 15 CYS HB2 H 3.82 0.02 2 64 15 15 CYS HB3 H 2.70 0.02 2 65 16 16 THR H H 9.48 0.02 1 66 16 16 THR HA H 4.58 0.02 1 67 16 16 THR HB H 4.10 0.02 1 68 16 16 THR HG2 H 1.17 0.02 1 69 17 17 CYS H H 8.89 0.02 1 70 17 17 CYS HA H 4.71 0.02 1 71 17 17 CYS HB2 H 2.88 0.02 2 72 17 17 CYS HB3 H 3.17 0.02 2 73 18 18 SER H H 8.85 0.02 1 74 18 18 SER HA H 4.80 0.02 1 75 18 18 SER HB2 H 3.94 0.02 2 76 18 18 SER HB3 H 3.88 0.02 2 77 19 19 TRP H H 7.72 0.02 1 78 19 19 TRP HA H 4.04 0.02 1 79 19 19 TRP HB2 H 3.29 0.02 1 80 19 19 TRP HB3 H 3.29 0.02 1 81 19 19 TRP HD1 H 7.45 0.02 1 82 19 19 TRP HE1 H 11.02 0.02 1 83 19 19 TRP HE3 H 7.49 0.02 1 84 19 19 TRP HZ2 H 7.48 0.02 1 85 19 19 TRP HZ3 H 6.99 0.02 1 86 19 19 TRP HH2 H 7.10 0.02 1 87 20 20 PRO HA H 3.47 0.02 1 88 20 20 PRO HB2 H 1.73 0.02 2 89 20 20 PRO HB3 H -0.38 0.02 2 90 20 20 PRO HG2 H 1.21 0.02 1 91 20 20 PRO HG3 H 1.21 0.02 1 92 20 20 PRO HD2 H 3.15 0.02 2 93 20 20 PRO HD3 H 3.40 0.02 2 94 21 21 VAL H H 8.65 0.02 1 95 21 21 VAL HA H 4.35 0.02 1 96 21 21 VAL HB H 1.92 0.02 1 97 21 21 VAL HG1 H 0.86 0.02 2 98 21 21 VAL HG2 H 0.86 0.02 2 99 22 22 CYS H H 7.57 0.02 1 100 22 22 CYS HA H 5.17 0.02 1 101 22 22 CYS HB2 H 3.21 0.02 2 102 22 22 CYS HB3 H 2.85 0.02 2 103 23 23 THR H H 10.02 0.02 1 104 23 23 THR HA H 5.10 0.02 1 105 23 23 THR HB H 3.78 0.02 1 106 23 23 THR HG2 H 0.93 0.02 1 107 24 24 ARG H H 8.68 0.02 1 108 24 24 ARG HA H 4.80 0.02 1 109 24 24 ARG HB2 H 1.73 0.02 1 110 24 24 ARG HB3 H 1.73 0.02 1 111 24 24 ARG HG2 H 1.50 0.02 2 112 24 24 ARG HG3 H 1.73 0.02 2 113 24 24 ARG HD2 H 3.20 0.02 1 114 24 24 ARG HD3 H 3.20 0.02 1 115 24 24 ARG HE H 6.98 0.02 1 116 25 25 ASN H H 9.48 0.02 1 117 25 25 ASN HA H 4.43 0.02 1 118 25 25 ASN HB2 H 2.88 0.02 2 119 25 25 ASN HB3 H 3.15 0.02 2 120 25 25 ASN HD21 H 7.58 0.02 2 121 25 25 ASN HD22 H 6.91 0.02 2 122 26 26 GLY H H 8.69 0.02 1 123 26 26 GLY HA2 H 4.28 0.02 2 124 26 26 GLY HA3 H 3.62 0.02 2 125 27 27 LEU H H 7.69 0.02 1 126 27 27 LEU HA H 5.10 0.02 1 127 27 27 LEU HB2 H 2.03 0.02 2 128 27 27 LEU HB3 H 1.41 0.02 2 129 27 27 LEU HG H 1.79 0.02 1 130 27 27 LEU HD1 H 1.05 0.02 2 131 27 27 LEU HD2 H 0.97 0.02 2 132 28 28 PRO HA H 5.16 0.02 1 133 28 28 PRO HB2 H 2.55 0.02 2 134 28 28 PRO HB3 H 1.66 0.02 2 135 28 28 PRO HG2 H 2.11 0.02 1 136 28 28 PRO HG3 H 2.11 0.02 1 137 28 28 PRO HD2 H 3.70 0.02 2 138 28 28 PRO HD3 H 3.83 0.02 2 139 29 29 VAL H H 8.04 0.02 1 140 29 29 VAL HA H 4.65 0.02 1 141 29 29 VAL HB H 2.63 0.02 1 142 29 29 VAL HG1 H 0.88 0.02 2 143 29 29 VAL HG2 H 0.93 0.02 2 stop_ save_ save_chem_shift_list_2 _Saveframe_category assigned_chemical_shifts _Details 'D2O solution' loop_ _Experiment_label '1H13C HSQC' HMBC stop_ loop_ _Sample_label $sample_2 stop_ _Sample_conditions_label $conditions_2 _Chem_shift_reference_set_label $chemical_shift_referencing _Mol_system_component_name 'Kalata B1' _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 CYS HA H 4.49 0.02 1 2 1 1 CYS HB2 H 3.36 0.02 2 3 1 1 CYS HB3 H 3.02 0.02 2 4 1 1 CYS C C 174.2 0.5 1 5 1 1 CYS CA C 59.2 0.5 1 6 1 1 CYS CB C 48.9 0.5 1 7 2 2 GLY HA2 H 3.76 0.02 2 8 2 2 GLY HA3 H 3.88 0.02 2 9 2 2 GLY C C 173.5 0.5 1 10 2 2 GLY CA C 46.4 0.5 1 11 3 3 GLU HA H 4.81 0.02 1 12 3 3 GLU HB2 H 2.10 0.02 2 13 3 3 GLU HB3 H 1.91 0.02 2 14 3 3 GLU HG2 H 2.55 0.02 1 15 3 3 GLU HG3 H 2.55 0.02 1 16 3 3 GLU C C 174.6 0.5 1 17 3 3 GLU CA C 54.4 0.5 1 18 3 3 GLU CB C 32.5 0.5 1 19 3 3 GLU CG C 33.5 0.5 1 20 3 3 GLU CD C 180.9 0.5 1 21 4 4 THR HA H 4.59 0.02 1 22 4 4 THR HB H 4.46 0.02 1 23 4 4 THR HG2 H 1.16 0.02 1 24 4 4 THR C C 173.4 0.5 1 25 4 4 THR CA C 60.2 0.5 1 26 4 4 THR CB C 70.6 0.5 1 27 4 4 THR CG2 C 21.6 0.5 1 28 5 5 CYS HA H 4.94 0.02 1 29 5 5 CYS HB2 H 2.97 0.02 2 30 5 5 CYS HB3 H 3.21 0.02 2 31 5 5 CYS C C 175.2 0.5 1 32 5 5 CYS CA C 54.8 0.5 1 33 5 5 CYS CB C 47.2 0.5 1 34 6 6 VAL HA H 3.91 0.02 1 35 6 6 VAL HB H 2.05 0.02 1 36 6 6 VAL HG1 H 1.03 0.02 2 37 6 6 VAL HG2 H 0.97 0.02 2 38 6 6 VAL C C 177.9 0.5 1 39 6 6 VAL CA C 64.9 0.5 1 40 6 6 VAL CB C 32.0 0.5 1 41 6 6 VAL CG1 C 21.1 0.5 1 42 6 6 VAL CG2 C 21.7 0.5 1 43 7 7 GLY HA2 H 4.25 0.02 2 44 7 7 GLY HA3 H 3.87 0.02 2 45 7 7 GLY C C 175.3 0.5 1 46 7 7 GLY CA C 45.8 0.5 1 47 8 8 GLY HA2 H 4.05 0.02 2 48 8 8 GLY HA3 H 4.40 0.02 2 49 8 8 GLY C C 173.5 0.5 1 50 8 8 GLY CA C 45.5 0.5 1 51 9 9 THR HA H 4.72 0.02 1 52 9 9 THR HB H 4.13 0.02 1 53 9 9 THR HG2 H 1.17 0.02 1 54 9 9 THR C C 173.7 0.5 1 55 9 9 THR CA C 60.7 0.5 1 56 9 9 THR CB C 71.4 0.5 1 57 9 9 THR CG2 C 21.2 0.5 1 58 10 10 CYS HA H 4.74 0.02 1 59 10 10 CYS HB2 H 2.83 0.02 2 60 10 10 CYS HB3 H 3.06 0.02 2 61 10 10 CYS CA C 55.3 0.5 1 62 10 10 CYS CB C 45.2 0.5 1 63 11 11 ASN HA H 4.72 0.02 1 64 11 11 ASN HB2 H 2.82 0.02 1 65 11 11 ASN HB3 H 2.82 0.02 1 66 11 11 ASN C C 175.8 0.5 1 67 11 11 ASN CA C 54.2 0.5 1 68 11 11 ASN CB C 39.5 0.5 1 69 11 11 ASN CG C 176.8 0.5 1 70 12 12 THR HA H 4.53 0.02 1 71 12 12 THR HB H 4.21 0.02 1 72 12 12 THR HG2 H 1.34 0.02 1 73 12 12 THR C C 172.5 0.5 1 74 12 12 THR CA C 61.1 0.5 1 75 12 12 THR CB C 69.8 0.5 1 76 12 12 THR CG2 C 21.9 0.5 1 77 13 13 PRO HA H 4.29 0.02 1 78 13 13 PRO HB2 H 2.33 0.02 2 79 13 13 PRO HB3 H 1.93 0.02 2 80 13 13 PRO HG2 H 2.16 0.02 2 81 13 13 PRO HG3 H 2.03 0.02 2 82 13 13 PRO HD2 H 4.15 0.02 2 83 13 13 PRO HD3 H 3.73 0.02 2 84 13 13 PRO C C 177.0 0.5 1 85 13 13 PRO CA C 64.2 0.5 1 86 13 13 PRO CB C 31.9 0.5 1 87 13 13 PRO CG C 27.6 0.5 1 88 13 13 PRO CD C 51.6 0.5 1 89 14 14 GLY HA2 H 3.71 0.02 2 90 14 14 GLY HA3 H 4.20 0.02 2 91 14 14 GLY C C 174.2 0.5 1 92 14 14 GLY CA C 45.2 0.5 1 93 15 15 CYS HA H 5.33 0.02 1 94 15 15 CYS HB2 H 3.82 0.02 2 95 15 15 CYS HB3 H 2.66 0.02 2 96 15 15 CYS C C 173.5 0.5 1 97 15 15 CYS CA C 57.9 0.5 1 98 15 15 CYS CB C 49.8 0.5 1 99 16 16 THR HA H 4.55 0.02 1 100 16 16 THR HB H 4.05 0.02 1 101 16 16 THR HG2 H 1.14 0.02 1 102 16 16 THR C C 174.0 0.5 1 103 16 16 THR CA C 60.3 0.5 1 104 16 16 THR CB C 71.3 0.5 1 105 16 16 THR CG2 C 21.1 0.5 1 106 17 17 CYS HA H 4.61 0.02 1 107 17 17 CYS HB2 H 2.85 0.02 2 108 17 17 CYS HB3 H 3.12 0.02 2 109 17 17 CYS C C 174.5 0.5 1 110 17 17 CYS CA C 56.4 0.5 1 111 17 17 CYS CB C 40.1 0.5 1 112 18 18 SER HA H 4.78 0.02 1 113 18 18 SER HB2 H 3.86 0.02 1 114 18 18 SER HB3 H 3.86 0.02 1 115 18 18 SER C C 174.1 0.5 1 116 18 18 SER CA C 56.5 0.5 1 117 18 18 SER CB C 61.3 0.5 1 118 19 19 TRP HA H 4.10 0.02 1 119 19 19 TRP HB2 H 3.28 0.02 1 120 19 19 TRP HB3 H 3.28 0.02 1 121 19 19 TRP HD1 H 7.31 0.02 1 122 19 19 TRP HE3 H 7.46 0.02 1 123 19 19 TRP HZ2 H 7.54 0.02 1 124 19 19 TRP HZ3 H 7.14 0.02 1 125 19 19 TRP HH2 H 7.26 0.02 1 126 19 19 TRP C C 175.3 0.5 1 127 19 19 TRP CA C 59.1 0.5 1 128 19 19 TRP CB C 29.9 0.5 1 129 19 19 TRP CG C 110.5 0.5 1 130 19 19 TRP CD1 C 128.0 0.5 1 131 19 19 TRP CD2 C 129.1 0.5 1 132 19 19 TRP CE2 C 139.0 0.5 1 133 19 19 TRP CE3 C 121.4 0.5 1 134 19 19 TRP CZ2 C 114.3 0.5 1 135 19 19 TRP CZ3 C 122.1 0.5 1 136 19 19 TRP CH2 C 124.7 0.5 1 137 20 20 PRO HA H 3.46 0.02 1 138 20 20 PRO HB2 H 1.71 0.02 2 139 20 20 PRO HB3 H -0.095 0.02 2 140 20 20 PRO HD2 H 3.26 0.02 1 141 20 20 PRO HD3 H 3.26 0.02 1 142 20 20 PRO CA C 65.0 0.5 1 143 20 20 PRO CB C 32.3 0.5 1 144 20 20 PRO CD C 48.9 0.5 1 145 21 21 VAL HA H 4.26 0.02 1 146 21 21 VAL HB H 1.95 0.02 1 147 21 21 VAL HG1 H 0.87 0.02 2 148 21 21 VAL HG2 H 0.85 0.02 2 149 21 21 VAL CA C 61.8 0.5 1 150 21 21 VAL CB C 35.2 0.5 1 151 21 21 VAL CG1 C 21.4 0.5 1 152 21 21 VAL CG2 C 20.9 0.5 1 153 22 22 CYS HA H 5.14 0.02 1 154 22 22 CYS HB2 H 3.24 0.02 2 155 22 22 CYS HB3 H 2.78 0.02 2 156 22 22 CYS CA C 56.8 0.5 1 157 22 22 CYS CB C 43.8 0.5 1 158 23 23 THR HA H 5.07 0.02 1 159 23 23 THR HB H 3.73 0.02 1 160 23 23 THR HG2 H 0.90 0.02 1 161 23 23 THR C C 174.5 0.5 1 162 23 23 THR CA C 51.7 0.5 1 163 23 23 THR CB C 72.5 0.5 1 164 23 23 THR CG2 C 21.2 0.5 1 165 24 24 ARG HA H 4.78 0.02 1 166 24 24 ARG HB2 H 1.71 0.02 1 167 24 24 ARG HB3 H 1.71 0.02 1 168 24 24 ARG HG2 H 1.40 0.02 2 169 24 24 ARG HD2 H 3.18 0.02 1 170 24 24 ARG HD3 H 3.18 0.02 1 171 24 24 ARG C C 176.7 0.5 1 172 24 24 ARG CA C 55.6 0.5 1 173 24 24 ARG CB C 32.9 0.5 1 174 24 24 ARG CG C 24.1 0.5 1 175 24 24 ARG CD C 43.7 0.5 1 176 25 25 ASN HA H 4.41 0.02 1 177 25 25 ASN HB2 H 3.11 0.02 2 178 25 25 ASN HB3 H 2.86 0.02 2 179 25 25 ASN C C 174.8 0.5 1 180 25 25 ASN CA C 54.5 0.5 1 181 25 25 ASN CB C 37.7 0.5 1 182 25 25 ASN CG C 178.0 0.5 1 183 26 26 GLY HA2 H 4.26 0.02 2 184 26 26 GLY HA3 H 3.61 0.02 2 185 26 26 GLY C C 173.8 0.5 1 186 26 26 GLY CA C 45.0 0.5 1 187 27 27 LEU HA H 5.09 0.02 1 188 27 27 LEU HB2 H 1.95 0.02 2 189 27 27 LEU HB3 H 1.49 0.02 2 190 27 27 LEU HG H 1.72 0.02 1 191 27 27 LEU HD1 H 1.00 0.02 2 192 27 27 LEU HD2 H 0.93 0.02 2 193 27 27 LEU C C 173.4 0.5 1 194 27 27 LEU CA C 59.6 0.5 1 195 27 27 LEU CB C 43.9 0.5 1 196 27 27 LEU CG C 26.8 0.5 1 197 27 27 LEU CD1 C 25.3 0.5 1 198 27 27 LEU CD2 C 22.6 0.5 1 199 28 28 PRO HA H 5.08 0.02 1 200 28 28 PRO HB2 H 2.48 0.02 2 201 28 28 PRO HB3 H 1.73 0.02 2 202 28 28 PRO HG2 H 2.19 0.02 2 203 28 28 PRO HG3 H 2.08 0.02 2 204 28 28 PRO HD2 H 3.83 0.02 2 205 28 28 PRO HD3 H 3.76 0.02 2 206 28 28 PRO C C 175.9 0.5 1 207 28 28 PRO CA C 62.6 0.5 1 208 28 28 PRO CB C 28.0 0.5 1 209 28 28 PRO CG C 27.3 0.5 1 210 28 28 PRO CD C 50.3 0.5 1 211 29 29 VAL HA H 4.67 0.02 1 212 29 29 VAL HB H 2.59 0.02 1 213 29 29 VAL HG1 H 0.90 0.02 2 214 29 29 VAL HG2 H 0.86 0.02 2 215 29 29 VAL C C 176.3 0.5 1 216 29 29 VAL CA C 60.5 0.5 1 217 29 29 VAL CB C 31.3 0.5 1 218 29 29 VAL CG1 C 18.8 0.5 1 219 29 29 VAL CG2 C 21.4 0.5 1 stop_ save_ ######################## # Coupling constants # ######################## save_J_coupling_list_1 _Saveframe_category coupling_constants _Details 'DPC micelles solution' loop_ _Experiment_label 'NOESY - infit' 'COSY -acme' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $conditions_1 _Spectrometer_frequency_1H 600 _Mol_system_component_name 'Kalata B1' _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 1 CYS H 1 CYS HA 7.8 . . 0.5 2 3JHNHA 3 GLU H 3 GLU HA 7.0 . . 0.5 3 3JHNHA 4 THR H 4 THR HA 8.5 . . 0.5 4 3JHNHA 5 CYS H 5 CYS HA 9.0 . . 0.5 5 3JHNHA 6 VAL H 6 VAL HA 5.7 . . 0.5 6 3JHNHA 9 THR H 9 THR HA 9.0 . . 0.5 7 3JHNHA 10 CYS H 10 CYS HA 8.7 . . 0.5 8 3JHNHA 11 ASN H 11 ASN HA 9.4 . . 0.5 9 3JHNHA 12 THR H 12 THR HA 4.5 . . 0.5 10 3JHNHA 15 CYS H 15 CYS HA 9.5 . . 0.5 11 3JHNHA 16 THR H 16 THR HA 9.0 . . 0.5 12 3JHNHA 17 CYS H 17 CYS HA 6.0 . . 0.5 13 3JHNHA 18 SER H 18 SER HA 9.0 . . 0.5 14 3JHNHA 19 TRP H 19 TRP HA 4.0 . . 0.5 15 3JHNHA 21 VAL H 21 VAL HA 9.3 . . 0.5 16 3JHNHA 22 CYS H 22 CYS HA 7.0 . . 0.5 17 3JHNHA 23 THR H 23 THR HA 10.3 . . 0.5 18 3JHNHA 24 ARG H 24 ARG HA 8.9 . . 0.5 19 3JHNHA 25 ASN H 25 ASN HA 6.6 . . 0.5 20 3JHNHA 27 LEU H 27 LEU HA 8.6 . . 0.5 21 3JHNHA 29 VAL H 29 VAL HA 7.8 . . 0.5 22 3JHAHB2 1 CYS HA 1 CYS HB2 12.0 . . 0.5 23 3JHAHB3 1 CYS HA 1 CYS HB3 4.0 . . 0.5 24 3JHAHB2 3 GLU HA 3 GLU HB2 7.0 . . 0.5 25 3JHAHB3 3 GLU HA 3 GLU HB3 7.0 . . 0.5 26 3JHAHB2 5 CYS HA 5 CYS HB2 3.0 . . 0.5 27 3JHAHB3 5 CYS HA 5 CYS HB3 4.0 . . 0.5 28 3JHAHB 6 VAL HA 6 VAL HB 10.5 . . 0.5 29 3JHAHB 9 THR HA 9 THR HB 5.6 . . 0.5 30 3JHAHB2 10 CYS HA 10 CYS HB2 12.0 . . 0.5 31 3JHAHB3 10 CYS HA 10 CYS HB3 4.0 . . 0.5 32 3JHAHB 12 THR HA 12 THR HB 8.7 . . 0.5 33 3JHAHB2 15 CYS HA 15 CYS HB2 12.0 . . 0.5 34 3JHAHB3 15 CYS HA 15 CYS HB3 3.0 . . 0.5 35 3JHAHB 16 THR HA 16 THR HB 5.0 . . 0.5 36 3JHAHB2 17 CYS HA 17 CYS HB2 4.0 . . 0.5 37 3JHAHB3 17 CYS HA 17 CYS HB3 12.0 . . 0.5 38 3JHAHB2 18 SER HA 18 SER HB2 9.5 . . 0.5 39 3JHAHB3 18 SER HA 18 SER HB2 4.7 . . 0.5 40 3JHAHB 21 VAL HA 21 VAL HB 6.7 . . 0.5 41 3JHAHB2 22 CYS HA 22 CYS HB2 14.0 . . 0.5 42 3JHAHB3 22 CYS HA 22 CYS HB3 3.0 . . 0.5 43 3JHAHB 23 THR HA 23 THR HB 3.0 . . 0.5 44 3JHAHB2 25 ASN HA 25 ASN HB2 9.0 . . 0.5 45 3JHAHB3 25 ASN HA 25 ASN HB3 6.0 . . 0.5 46 3JHAHB2 27 LEU HA 27 LEU HB2 13.0 . . 0.5 47 3JHAHB3 27 LEU HA 27 LEU HB3 3.0 . . 0.5 48 3JHB2HG 27 LEU HB2 27 LEU HG 3.0 . . 0.5 49 3JHB3HG 27 LEU HB3 27 LEU HG 12.0 . . 0.5 50 3JHAHB 29 VAL HA 29 VAL HB 4.0 . . 0.5 stop_ save_ save_J_coupling_list_2 _Saveframe_category coupling_constants _Details 'D2O soloution' loop_ _Experiment_label 'long-range band selective HMQC' 'quantitative J correlation' stop_ loop_ _Sample_label $sample_2 stop_ _Sample_conditions_label $conditions_2 _Spectrometer_frequency_1H 500 _Mol_system_component_name 'Kalata B1' _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 1 CYS H 1 CYS HA 7.8 . . 0.5 2 3JHNHA 3 GLU H 3 GLU HA 7.0 . . 0.5 3 3JHNHA 4 THR H 4 THR HA 8.5 . . 0.5 4 3JHNHA 5 CYS H 5 CYS HA 9.0 . . 0.5 5 3JHNHA 6 VAL H 6 VAL HA 5.7 . . 0.5 6 3JHNHA 9 THR H 9 THR HA 9.0 . . 0.5 7 3JHNHA 10 CYS H 10 CYS HA 8.7 . . 0.5 8 3JHNHA 11 ASN H 11 ASN HA 9.4 . . 0.5 9 3JHNHA 12 THR H 12 THR HA 4.5 . . 0.5 10 3JHNHA 15 CYS H 15 CYS HA 9.5 . . 0.5 11 3JHNHA 16 THR H 16 THR HA 9.0 . . 0.5 12 3JHNHA 17 CYS H 17 CYS HA 6.0 . . 0.5 13 3JHNHA 18 SER H 18 SER HA 9.0 . . 0.5 14 3JHNHA 19 TRP H 19 TRP HA 4.0 . . 0.5 15 3JHNHA 21 VAL H 21 VAL HA 9.3 . . 0.5 16 3JHNHA 22 CYS H 22 CYS HA 7.0 . . 0.5 17 3JHNHA 23 THR H 23 THR HA 10.3 . . 0.5 18 3JHNHA 24 ARG H 24 ARG HA 8.9 . . 0.5 19 3JHNHA 25 ASN H 25 ASN HA 6.6 . . 0.5 20 3JHNHA 27 LEU H 27 LEU HA 8.6 . . 0.5 21 3JHNHA 29 VAL H 29 VAL HA 7.8 . . 0.5 22 3JHAHB2 1 CYS HA 1 CYS HB2 12.0 . . 0.5 23 3JHAHB3 1 CYS HA 1 CYS HB3 4.0 . . 0.5 24 3JHAHB2 3 GLU HA 3 GLU HB2 7.0 . . 0.5 25 3JHAHB3 3 GLU HA 3 GLU HB3 7.0 . . 0.5 26 3JHAHB2 5 CYS HA 5 CYS HB2 3.0 . . 0.5 27 3JHAHB3 5 CYS HA 5 CYS HB3 4.0 . . 0.5 28 3JHAHB 6 VAL HA 6 VAL HB 10.5 . . 0.5 29 3JHAHB 9 THR HA 9 THR HB 5.6 . . 0.5 30 3JHAHB2 10 CYS HA 10 CYS HB2 12.0 . . 0.5 31 3JHAHB3 10 CYS HA 10 CYS HB3 4.0 . . 0.5 32 3JHAHB 12 THR HA 12 THR HB 8.7 . . 0.5 33 3JHAHB2 15 CYS HA 15 CYS HB2 12.0 . . 0.5 34 3JHAHB3 15 CYS HA 15 CYS HB3 3.0 . . 0.5 35 3JHAHB 16 THR HA 16 THR HB 5.0 . . 0.5 36 3JHAHB2 17 CYS HA 17 CYS HB2 4.0 . . 0.5 37 3JHAHB3 17 CYS HA 17 CYS HB3 12.0 . . 0.5 38 3JHAHB2 18 SER HA 18 SER HB2 9.5 . . 0.5 39 3JHAHB3 18 SER HA 18 SER HB2 4.7 . . 0.5 40 3JHAHB 21 VAL HA 21 VAL HB 6.7 . . 0.5 41 3JHAHB2 22 CYS HA 22 CYS HB2 14.0 . . 0.5 42 3JHAHB3 22 CYS HA 22 CYS HB3 3.0 . . 0.5 43 3JHAHB 23 THR HA 23 THR HB 3.0 . . 0.5 44 3JHAHB2 25 ASN HA 25 ASN HB2 9.0 . . 0.5 45 3JHAHB3 25 ASN HA 25 ASN HB3 6.0 . . 0.5 46 3JHAHB2 27 LEU HA 27 LEU HB2 13.0 . . 0.5 47 3JHAHB3 27 LEU HA 27 LEU HB3 3.0 . . 0.5 48 3JHB2HG 27 LEU HB2 27 LEU HG 3.0 . . 0.5 49 3JHB3HG 27 LEU HB3 27 LEU HG 12.0 . . 0.5 50 3JHAHB 29 VAL HA 29 VAL HB 4.0 . . 0.5 stop_ save_