######################### # Spectral peak lists # ######################### 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 30946 _Spectral_peak_list.ID 1 _Spectral_peak_list.Name . _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.Chem_shift_reference_ID 1 _Spectral_peak_list.Chem_shift_reference_label $chem_shift_reference_1 _Spectral_peak_list.Experiment_ID 2 _Spectral_peak_list.Experiment_name '2D 1H-1H TOCSY' _Spectral_peak_list.Experiment_class . _Spectral_peak_list.Experiment_type . _Spectral_peak_list.Number_of_spectral_dimensions 2 _Spectral_peak_list.Chemical_shift_list . _Spectral_peak_list.Assigned_chem_shift_list_ID 1 _Spectral_peak_list.Assigned_chem_shift_list_label $assigned_chemical_shifts_1 _Spectral_peak_list.Details ; A combined overlay of 1H-1H 2D COSY, TOCSY, and ROESY experiments were used to assign the proton chemical shifts. Peaks were picked within the TOCSY spectrum as peak height maxima allowed for the most precise measurement of shifts between the experiments employed. Peaks denoted (ROE) in the list were found in the 2D 1H-1H ROESY spectrum. ; _Spectral_peak_list.Text_data_format text _Spectral_peak_list.Text_data ; Notes on peak picking and annotation: 1) Chemical shifts were calculated only from non-ROE peaks, using TOCSY maxima and in cases of overlap, the centerpoint of a phase-sensitve COSY crosspeak 2) Diastereotopic protons and methyl groups were annotate such that the more upfield of the pair was labeled 1 and the more downfield labeled 2. If superimposed and not resolvable in the f2 dimension, then the group was labeled 12. e.g. For leucine methyl groups, resolved: HD1 and HD2. For leucine beta protons, not resolved - HB12. 3) Peaks that were solely chosen from the ROESY spectrum are indicated with (ROE) in parentheses. No ROE peaks that also included a TOCSY peak were used to generate the NMR ensemble or any of the associated restraints. f2 (ppm) f1 (ppm) Annotation 1 0.85 4.26 Leu(9)HD1-HA 2 0.85 7.10 Leu(9)HD1-Tyr(8)H2,6 (ROE) 3 0.85 6.84 Leu(9)HD1-Tyr(8)H3,5 (ROE) 4 0.86 1.53 Leu(9)HD1-HB/ G 5 0.86 8.08 Leu(9)HD1-HN 6 0.89 4.29 Leu(10)HD1-HA 7 0.89 7.98 Leu(10)HD1-HN 8 0.89 7.56 Leu(10)HD1-Trp(1)H4 (ROE) 9 0.89 6.85 Leu(9)HD2-Tyr(8)H3,5 (ROE) 10 0.90 1.61 Leu(3/ 10)HD1-HB/ G 11 0.90 4.26 Leu(9)HD2-HA 12 0.90 7.13 Leu(9)HD2-Tyr(8)H2,6 (ROE) 13 0.91 4.19 Leu(3)HD1-HA 14 0.91 8.32 Leu(3)HD1-HN 15 0.91 7.27 Leu(3)HD1-Trp(1)H6 (ROE) 16 0.91 1.53 Leu(9)HD2-HB/ G 17 0.91 8.07 Leu(9)HD2-HN 18 0.94 6.83 Leu(10)HD2-Tyr(8)H3,5 (ROE) 19 0.95 4.29 Leu(10)HD2-HA 20 0.95 7.98 Leu(10)HD2-HN 21 0.96 8.42 Leu(3)HD2- Asn(4)HN (ROE) 22 0.96 4.19 Leu(3)HD2-HA 23 0.96 8.32 Leu(3)HD2-HN 24 0.96 7.56 Leu(3)HD2-Trp(1)H4 (ROE) 25 0.96 7.27 Leu(3)HD2-Trp(1)H6 26 0.96 7.12 Leu(3)HD2-Tyr(8)H2,6 (ROE) 27 0.96 1.61 Leu(3/ 10)HD2-HB/ G 28 1.16 8.35 Thr(2) HG-HN 29 1.17 4.33 Thr(2) HG-HA 30 1.17 4.11 Thr(2) HG-HB 31 1.17 8.32 Thr(2)HG-Leu(3)HN (ROE) overlap 32 1.19 7.34 Thr(2)HG-Trp(1)H2 (ROE) 33 1.39 4.31 Ala(6)HB-HA 34 1.39 6.84 Leu(9)HB1-Tyr(8)H3,5 (ROE) 35 1.40 8.32 Ala(6)HB-HN overlap 36 1.40 3.88 Ala(6)HB-Ser(5)HB12 (ROE) 37 1.40 8.22 Ala(6)HB-Ser(5)HN (ROE) overlap 38 1.44 3.00 Lys(12/ 13)HG-HE 39 1.45 8.32 Lys(13)HG-HN 40 1.46 8.08 Lys(12)HG-HN 41 1.48 4.29 Lys(12/ 13)HG-HA 42 1.59 4.20 Leu(3)HB/ G-HA 43 1.59 8.44 Leu(3)HB12/ HG-Asn(4)HN (ROE) overlap 44 1.60 8.31 Leu(3)HB/ G-HN 45 1.62 0.93 Leu(all)HB/ G-HD 46 1.62 8.07 Lys(12)HD-HN 47 1.64 7.97 Leu(10)HB/ HG-HN 48 1.66 4.29 Lys(12/ 13)HD-HA 49 1.68 3.00 Lys(12/ 13)HD-HE 50 1.68 8.33 Lys(13)HD-HN 51 1.80 8.08 Lys(12)HB-HN 52 1.81 4.30 Lys(12/ 13)HB-HA 53 1.81 8.31 Lys(13)HB-HN 54 1.83 3.00 Lys(12/ 13)HB-HE 55 2.81 6.91 Asn(4)HB12-NH1 56 2.81 7.58 Asn(4)HB12-NH2 57 2.81 8.27 Asn(4)HB12-Ser(5)HN 58 2.82 4.71 Asn(4)HB12-HA 59 2.82 8.43 Asn(4)HB12-HN 60 3.00 1.83 Lys(12/ 13)HE-HB 61 3.00 1.68 Lys(12/ 13)HE-HD 62 3.00 1.43 Lys(12/ 13)HE-HG 63 3.02 7.11 Tyr(8)HB12-H2,6 (ROE) 64 3.02 4.57 Tyr(8)HB12-HA 65 3.02 8.08 Tyr(8)HB12-Leu(9)HN (ROE) overlap 66 3.03 7.90 Tyr(8)HB12-HN 67 3.41 7.32 Trp(1)HB12-H2 68 3.41 7.60 Trp(1)HB12-H4 69 3.41 4.40 Trp(1)HB12-HA 70 3.42 8.36 Trp(1)HB12-Thr(2)HN (ROE) 71 3.83 7.90 Gly(7)HA12-Tyr(8)HN (ROE) 72 3.85 8.24 Gly(7)HA12-HN 73 3.85 7.11 Gly(7)HA12-Tyr(8)H2,6 (ROE) overlap 74 3.85 1.41 Ser(5)HB1-Ala(6)HB (ROE) 75 3.86 4.38 Ser(5)HB1-HA 76 3.89 8.26 Ser(5)HB12-HN 77 3.92 4.37 Ser(5)HB2-HA 78 3.93 8.24 Gly(11)HA12-HN 79 4.10 1.17 Thr(2) HB-HG 80 4.10 8.35 Thr(2) HB-HN 81 4.11 4.32 Thr(2) HB-HA 82 4.19 8.45 Leu(3)HA-Asn(4)HN (ROE) 83 4.19 1.60 Leu(3)HA-HB/ G 84 4.20 0.93 Leu(3)HA-HD12 85 4.20 8.31 Leu(3)HA-HN 86 4.27 1.65 Leu(10)HA-HB/ G 87 4.27 0.89 Leu(10)HA-HD12 88 4.27 8.07 Leu(9)HA-HN 89 4.27 7.57 Leu(9)HA-Trp(1)H4 (ROE) overlap 90 4.27 8.32 Lys(13)HA-HN 91 4.29 7.97 Leu(10)HA-HN 92 4.29 1.64 Leu(9)HA-HB/ G 93 4.29 0.90 Leu(9)HA-HD 94 4.31 8.32 Ala(6)HA-HN 95 4.32 1.81 Lys(12/ 13)HA-HB 96 4.32 1.68 Lys(12/ 13)HA-HD 97 4.32 1.41 Lys(12/ 13)HA-HG 98 4.32 1.17 Thr(2) HA-HG 99 4.32 8.35 Thr(2) HA-HN 100 4.33 8.07 Lys(12)HA-HN 101 4.33 4.10 Thr(2) HA-HB 102 4.37 3.88 Ser(5)HA-HB12 103 4.37 8.24 Ser(5)HA-HN 104 4.37 8.23 Trp(1)HA-HN 105 4.39 3.42 Trp(1) HA-HB12 106 4.51 3.04 Tyr(8)HA-HB12 107 4.52 7.90 Tyr(8)HA-HN 108 4.71 2.83 Asn(4)HA-HB12 109 6.83 3.02 Tyr(8)H3,5-HB12 110 6.83 7.89 Tyr(8)H3,5-HN (ROE) 111 6.84 3.84 Tyr(8)H3,5-Gly(7)HA12 (ROE) 112 6.84 4.52 Tyr(8)H3,5-HA (ROE) 113 6.84 7.26 Tyr(8)H3,5-Trp(1)H6 (ROE) 114 6.91 2.82 Asn(4)NH1-HB12 115 6.91 7.58 Asn(4)NH1-NH2 116 7.10 3.83 Tyr(8)H2,6-Gly(7)HA12 (ROE) 117 7.10 3.02 Tyr(8)H2,6-HB12 (ROE) 118 7.10 7.89 Tyr(8)H2,6-HN (ROE) 119 7.10 8.08 Tyr(8)H2,6-Leu(9)HA (ROE) overlap 120 7.10 0.88 Tyr(8)H2,6-Leu(9)HD12 121 7.11 2.83 Tyr(8)H2,6-Asn(4)HB12 (ROe) 122 7.11 4.54 Tyr(8)H2,6-HA (ROE) 123 7.15 7.58 Trp(1)H5-H4 124 7.15 7.53 Trp(1)H5-H7 125 7.15 4.21 Trp(1)H5-Leu(3)HA 126 7.15 0.91 Trp(1)H5-Leu9,10,3 HD12 9ROE) 127 7.16 7.28 Trp(1)H5-H6 128 7.25 4.21 Trp(1)H6-Leu(3)HA (ROE) 129 7.27 7.57 Trp(1)H6-H4 130 7.27 7.15 Trp(1)H6-H5 131 7.27 7.54 Trp(1)H6-H7 132 7.28 0.94 Trp(1)H6-Leu(3)HD12 (ROE) 133 7.28 6.82 Trp(1)H6-Tyr(8)H3,5 (ROE) 134 7.32 4.40 Trp(1)H2-HA 135 7.32 0.90 Trp(1)H2-Leu(9)/ Leu(10) HD12 (ROE) 136 7.32 10.23 Trp(1)H2-NH1 137 7.32 3.42 Trp(1)HB12-H2 138 7.51 3.42 Trp(1)H7-HB12 (ROE) 139 7.51 0.94 Trp(1)H7-Leu(3)HD12 (RO) 140 7.52 7.28 Trp(1)H7-H6 141 7.52 4.22 Trp(1)H7-Leu(3)HA (ROE) 142 7.53 7.15 Trp(1)H7-H5 143 7.53 10.22 Trp(1)H7-NH1 (ROE) 144 7.57 7.15 Trp(1)H4-H5 145 7.57 7.29 Trp(1)H4-H7 146 7.57 4.40 Trp(1)H4-HA (ROE) overlap 147 7.57 3.41 Trp(1)H4-HB12 (ROE) overlap 148 7.57 4.27 Trp(1)H4-Leu(9)HA (ROE) overlap 149 7.58 2.81 Asn(4)NH2-HB12 150 7.58 6.91 Asn(4)NH2-NH1 151 7.58 0.90 Asn(4)NH2/ Trp(1)H4-Leu3,9,10 HD12 152 7.89 3.84 Tyr(8)HN-Gly(7)HA12 (ROE) 153 7.89 8.26 Tyr(8)HN-Gly7HN) (ROE) 154 7.89 7.10 Tyr(8)HN-H2,6 (ROE) 155 7.89 4.53 Tyr(8)HN-HA 156 7.89 3.03 Tyr(8)HN-HB12 157 7.90 4.31 Tyr(8)HN-Leu(9)HA (ROE) overlap 158 7.96 3.87 Leu(10)HN-Gly(11)HN (ROE) overlap 159 7.97 4.29 Leu(10)HN-HA 160 7.97 0.93 Leu(10)HN-HD12 161 7.97 1.66 Leu(10)HN-HG/ HB12 162 7.97 8.10 Leu(10)HN-Leu(9)HN (ROE) overlap 163 7.97 4.54 Leu(10)HN-Tyr(8)HA (ROE) 164 8.07 0.88 Leu(9)HN-HD 165 8.07 7.94 Leu(9)HN-Leu(10)HN (ROE) overlap 166 8.07 3.03 Leu(9)HN-Tyr(8)HB12 (ROE) overlap 167 8.07 4.30 Lys(12)HN-HA 168 8.08 4.30 Leu(9)HN-HA 169 8.08 7.10 Leu(9)HN-Tyr(8)H2,6 (ROE) overlap 170 8.08 4.52 Leu(9)HN-Tyr(8)HA (ROE) overlap 171 8.08 1.80 Lys(12)HN-HB 172 8.08 1.59 Lys(12)HN-HD 173 8.08 1.43 Lys(12)HN-HG 174 8.23 4.70 Ser(5)HN-Asn(4)HA (ROE) overlap 175 8.23 2.83 Ser(5)HN-Asn(4)HB12 (ROE) overlap 176 8.23 4.37 Ser(5)HN-HA (overlap) 177 8.23 3.88 Ser(5)HN-HB12 178 8.23 4.37 Trp(1)HN-HA 179 8.24 1.40 Ser(5)HN-Ala(6)HB (ROE) overlap 180 8.26 7.90 Gly(7)HN-Tyr(8)HN (ROE) 181 8.30 1.40 Ala(6)HN-HB 182 8.31 3.89 Ala(6)HN-Ser(5)HB12 (ROE) overlap 183 8.31 2.83 Leu(3)HN-Asn(4)HB12 (ROE) 184 8.31 4.21 Leu(3)HN-HA 185 8.31 0.94 Leu(3)HN-HD12 186 8.31 1.18 Leu(3)HN-Thr(2)HG (ROE) 187 8.31 4.30 Lys(13)HN-HA 188 8.31 1.60 Lys(13)HN-HD 189 8.32 1.81 Lys(13)HN-HB 190 8.32 3.01 Lys(13)HN-HE 191 8.32 1.43 Lys(13)HN-HG 192 8.33 4.28 Ala(6)HN-HA 193 8.35 4.32 Thr(2) HN-HA 194 8.35 4.09 Thr(2) HN-HB 195 8.35 1.17 Thr(2) HN-HG 196 8.35 3.41 Thr(2)-Trp(1)HB12 (ROE) 197 8.43 4.71 Asn(4)HN-HA 198 8.43 2.82 Asn(4)HN-HB12 199 8.43 4.21 Asn(4)HN-Leu(3)HA (ROE) 200 8.43 1.61 Asn(4)HN-Leu(3)HB12/ HG (ROE) overlap 201 10.22 7.32 Trp(1)NH1-H2 202 10.22 7.54 Trp(1)NH1-H7 (ROE) ; loop_ _Spectral_dim.ID _Spectral_dim.Axis_code _Spectral_dim.Spectrometer_frequency _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.Value_first_point _Spectral_dim.Absolute_peak_positions _Spectral_dim.Acquisition _Spectral_dim.Center_frequency_offset _Spectral_dim.Encoding_code _Spectral_dim.Encoded_reduced_dimension_ID _Spectral_dim.Entry_ID _Spectral_dim.Spectral_peak_list_ID 1 . . H 1 H . . 4761.9 Hz . . . 4.69 . . 30946 1 2 . . H 1 H . . 4761.9 Hz . . . 4.69 . . 30946 1 stop_ save_