data_4975 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Assignment of selectively 13C-labeled cellopentaose synthesized using an engineered glycosynthase ; _BMRB_accession_number 4975 _BMRB_flat_file_name bmr4975.str _Entry_type original _Submission_date 2001-03-20 _Accession_date 2001-03-20 _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 Brun Emmanuel . . 2 Brummer Harry . III 3 Mackenzie Lloyd . . 4 Withers Stephen G. . 5 McIntosh Lawrence P. . 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" 7 "13C chemical shifts" 6 "coupling constants" 8 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2001-10-08 original author . stop_ save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; Letter to the Editor: Assignment of selectively 13C-labeled cellopentaose synthesized using an engineered glycosynthase ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID ? loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Brun Emmanuel . . 2 Brumer Harry . III 3 Mackenzie Lloyd F. . 4 Withers Stephen G. . 5 McIntosh Lawrence P. . stop_ _Journal_abbreviation 'J. Biomol. NMR' _Journal_volume 21 _Journal_issue 1 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 67 _Page_last 68 _Year 2001 _Details . loop_ _Keyword carbohydrate isotope transglycosylation 'NMR assignment' stop_ save_ ####################################### # Cited references within the entry # ####################################### save_ref_1 _Saveframe_category citation _Citation_full ; L.F. MacKenzie, Q. Wang, R.A.J. Warren, S.G. Withers, "Glycosynthases: Mutant Glycosidases for Oligosaccharide Synthesis" J.A.C.S. 120, 5583-5584 (1998) ; _Citation_title . _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID ? _Journal_abbreviation . _Journal_name_full . _Journal_volume . _Journal_issue . _Journal_CSD . _Book_title . _Book_chapter_title . _Book_volume . _Book_series . _Book_publisher . _Book_publisher_city . _Book_ISBN . _Conference_title . _Conference_site . _Conference_state_province . _Conference_country . _Conference_start_date . _Conference_end_date . _Conference_abstract_number . _Thesis_institution . _Thesis_institution_city . _Thesis_institution_country . _Page_first . _Page_last . _Year . _Details . save_ ################################## # Molecular system description # ################################## save_system_cellopentaose _Saveframe_category molecular_system _Mol_system_name B-D-glucospyranosyl-(1,4)-B-D-glucospyranosyl-(1,4)-B-D-glucospyranosyl-(1,4)-B-D-glucospyranosyl-(1,4)-B-D-glucospyranose _Abbreviation_common cellopentaose _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label cellopentaose $cellopentaose stop_ _System_molecular_weight . _System_physical_state native _System_oligomer_state monomer _System_paramagnetic no _System_thiol_state 'not present' _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_cellopentaose _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class carbohydrate _Name_common cellopentaose _Abbreviation_common G5 _Molecular_mass . _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 5 _Mol_residue_sequence XXXXX loop_ _Residue_seq_code _Residue_label 1 GLC 2 GLC 3 GLC 4 GLC 5 GLC stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ###################### # Polymer residues # ###################### save_chem_comp_GLC _Saveframe_category polymer_residue _Mol_type SACCHARIDE _Name_common ALPHA-D-GLUCOSE _BMRB_code . _PDB_code GLC _Standard_residue_derivative . _Molecular_mass 180.156 _Mol_paramagnetic . _Details ; Information obtained from PDB's Chemical Component Dictionary at http://wwpdb-remediation.rutgers.edu/downloads.html Downloaded on Thu Jul 21 10:17:14 2011 ; 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 . ? O1 O1 O . 0 . ? O2 O2 O . 0 . ? O3 O3 O . 0 . ? O4 O4 O . 0 . ? O5 O5 O . 0 . ? O6 O6 O . 0 . ? H1 H1 H . 0 . ? H2 H2 H . 0 . ? H3 H3 H . 0 . ? H4 H4 H . 0 . ? H5 H5 H . 0 . ? H61 H61 H . 0 . ? H62 H62 H . 0 . ? HO1 HO1 H . 0 . ? HO2 HO2 H . 0 . ? HO3 HO3 H . 0 . ? HO4 HO4 H . 0 . ? HO6 HO6 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 C1 C2 ? ? SING C1 O1 ? ? SING C1 O5 ? ? SING C1 H1 ? ? SING C2 C3 ? ? SING C2 O2 ? ? SING C2 H2 ? ? SING C3 C4 ? ? SING C3 O3 ? ? SING C3 H3 ? ? SING C4 C5 ? ? SING C4 O4 ? ? SING C4 H4 ? ? SING C5 C6 ? ? SING C5 O5 ? ? SING C5 H5 ? ? SING C6 O6 ? ? SING C6 H61 ? ? SING C6 H62 ? ? SING O1 HO1 ? ? SING O2 HO2 ? ? SING O3 HO3 ? ? SING O4 HO4 ? ? SING O6 HO6 ? ? stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $cellopentaose . . . . . . 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 _Details $cellopentaose 'enzymatic semisynthesis' . . . . . 'Synthesized from a-fluorsyl glucose using an engineered Glycosynthase' stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details '1.5 mg in 550 uL D2O' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $cellopentaose 3.3 mM '[U-95% 13C]-Glc2' stop_ save_ ############################ # Computer software used # ############################ save_Felix _Saveframe_category software _Name Felix _Version 2.3 loop_ _Task processing stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_NMR_spectrometer _Saveframe_category NMR_spectrometer _Manufacturer Varian _Model Unity _Field_strength 500 _Details . save_ ############################# # NMR applied experiments # ############################# save_1H-13C_HSQC_1 _Saveframe_category NMR_applied_experiment _Experiment_name '1H-13C HSQC' _Sample_label $sample_1 save_ save_1H-13C_HCCH-COSY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '1H-13C HCCH-COSY' _Sample_label $sample_1 save_ save_NMR_spec_expt__0_1 _Saveframe_category NMR_applied_experiment _Experiment_name '1H-13C HSQC' _BMRB_pulse_sequence_accession_number . _Details . save_ save_NMR_spec_expt__0_2 _Saveframe_category NMR_applied_experiment _Experiment_name '1H-13C HCCH-COSY' _BMRB_pulse_sequence_accession_number . _Details . save_ ####################### # Sample conditions # ####################### save_condition_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH . . pH temperature 298 0.5 K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chemical_shift_reference _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 DSS H 1 'methyl protons' ppm 0.00 external direct cylindrical external parallel DSS C 13 'methyl protons' ppm 0.00 external indirect cylindrical external parallel 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_cellopentaose_shifts _Saveframe_category assigned_chemical_shifts _Details . loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $condition_1 _Chem_shift_reference_set_label $chemical_shift_reference _Mol_system_component_name cellopentaose _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 . 4 GLC C1 C 105.0 0.05 . 2 . 4 GLC H1 H 4.53 0.02 . 3 . 4 GLC C2 C 75.6 0.05 . 4 . 4 GLC H2 H 3.36 0.02 . 5 . 4 GLC C3 C 76.8 0.05 . 6 . 4 GLC H3 H 3.66 0.02 . 7 . 4 GLC C4 C 81.1 0.05 . 8 . 4 GLC H4 H 3.67 0.02 . 9 . 4 GLC C5 C 77.5 0.05 . 10 . 4 GLC H5 H 3.62 0.02 . 11 . 4 GLC C6 C 62.6 0.05 . 12 . 4 GLC H61 H 3.98 0.02 . 13 . 4 GLC H62 H 3.82 0.02 . stop_ save_ ######################## # Coupling constants # ######################## save_cellopentaose_J_values _Saveframe_category coupling_constants _Details ; Coupling constants were measured from a high-resolution 1H-13C HSQC recorded without 31C-decoupling in the observed dimension. ; loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $condition_1 _Spectrometer_frequency_1H 500 _Mol_system_component_name cellopentaose _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 1JC1H1 4 GLC C1 2 GLC H1 162 . . . 2 1JC1C2 4 GLC C1 2 GLC C2 48 . . . 3 1JC2H2 4 GLC C2 2 GLC H2 148 . . . 4 1JC3H3 4 GLC C3 2 GLC H3 142 . . . 5 1JC4H4 4 GLC C4 2 GLC H4 144 . . . 6 1JC5H5 4 GLC C5 2 GLC H5 142 . . . 7 1JC6H61 4 GLC C6 2 GLC H61 144 . . . 8 1JC6C5 4 GLC C6 2 GLC C5 42 . . . stop_ save_