#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:57:19 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178797 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/51/4105171.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4105171
loop_
_publ_author_name
'Upadhyayula S. Raghavender'
'Subrayashastry Aravinda'
'Narayanaswamy Shamala'
'Rajkishor Rai'
'Padmanabhan Balaram'
_publ_section_title
;
 Characterization of Water Wires inside Hydrophobic Tubular Peptide
 Structures
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15130
_journal_page_last               15132
_journal_paper_doi               10.1021/ja9038906
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C29 H51 N5 O8.17'
_chemical_formula_weight         600.41
_chemical_name_common            Boc-D-Pro-Aib-Val-Aib-Val-OMe
_chemical_name_systematic
; 
 t-Butyloxycarbonyl-D-prolyl-alpha-aminoisobutyryl-valyl
-alpha-aminoisobutyryl-valyl-methyl ester
;
_space_group_IT_number           170
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 65'
_symmetry_space_group_name_H-M   'P 65'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   24.3161(3)
_cell_length_b                   24.3161(3)
_cell_length_c                   10.48050(10)
_cell_measurement_temperature    293(2)
_cell_volume                     5366.62(11)
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type
'BRUKER AXS SMART APEXII ULTRA CCD with Cu source'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0187
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18429
_diffrn_reflns_theta_full        72.06
_diffrn_reflns_theta_max         72.06
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'color less'
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_description       rods
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -10(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    'riding over the heavy atom'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         3632
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          1.265
_refine_ls_shift/su_mean         0.043
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1654P)²+0.2146P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1844
_refine_ls_wR_factor_ref         0.1855
_reflns_number_gt                3309
_reflns_number_total             3632
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9038906_si_004.cif
_cod_data_source_block           dpuv5b
_cod_original_cell_volume        5366.61(11)
_cod_database_code               4105171
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'-x, -y, z+1/2'
'y, -x+y, z+1/6'
'x-y, x, z+5/6'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.8063(2) 0.7353(2) -0.3975(5) 0.0766(10) Uani 1 1 d .
C2 C 0.7530(3) 0.6987(4) -0.3057(7) 0.1086(19) Uani 1 1 d .
H2A H 0.7701 0.6970 -0.2241 0.163 Uiso 1 1 calc R
H2B H 0.7265 0.6564 -0.3372 0.163 Uiso 1 1 calc R
H2C H 0.7283 0.7194 -0.2968 0.163 Uiso 1 1 calc R
C3 C 0.7789(4) 0.7386(4) -0.5247(8) 0.126(2) Uani 1 1 d .
H3A H 0.8128 0.7620 -0.5841 0.190 Uiso 1 1 calc R
H3B H 0.7546 0.7596 -0.5143 0.190 Uiso 1 1 calc R
H3C H 0.7519 0.6964 -0.5564 0.190 Uiso 1 1 calc R
C4 C 0.8552(3) 0.7999(2) -0.3461(9) 0.116(2) Uani 1 1 d .
H4A H 0.8879 0.8218 -0.4087 0.173 Uiso 1 1 calc R
H4B H 0.8737 0.7945 -0.2695 0.173 Uiso 1 1 calc R
H4C H 0.8350 0.8243 -0.3275 0.173 Uiso 1 1 calc R
O O 0.83717(15) 0.69913(15) -0.4271(3) 0.0740(7) Uani 1 1 d .
C0' C 0.86442(15) 0.68165(15) -0.3364(3) 0.0534(6) Uani 1 1 d .
O0 O 0.87735(12) 0.70274(12) -0.2276(3) 0.0657(6) Uani 1 1 d .
N1 N 0.87672(13) 0.63696(13) -0.3802(3) 0.0543(6) Uani 1 1 d .
C1A C 0.90878(13) 0.61269(14) -0.3021(3) 0.0506(6) Uani 1 1 d .
H1A H 0.9531 0.6458 -0.2887 0.061 Uiso 1 1 calc R
C1' C 0.87566(12) 0.58827(13) -0.1735(3) 0.0472(6) Uani 1 1 d .
O1 O 0.81766(10) 0.55566(11) -0.1662(3) 0.0617(6) Uani 1 1 d .
C1B C 0.9060(2) 0.5595(2) -0.3850(4) 0.0752(10) Uani 1 1 d .
H1B1 H 0.9469 0.5735 -0.4250 0.090 Uiso 1 1 calc R
H1B2 H 0.8954 0.5225 -0.3331 0.090 Uiso 1 1 calc R
C1G C 0.8584(5) 0.5443(4) -0.4798(7) 0.138(3) Uani 1 1 d .
H1G1 H 0.8177 0.5104 -0.4500 0.165 Uiso 1 1 calc R
H1G2 H 0.8695 0.5304 -0.5576 0.165 Uiso 1 1 calc R
C1D C 0.8549(2) 0.6047(2) -0.5047(4) 0.0786(11) Uani 1 1 d .
H1D1 H 0.8830 0.6298 -0.5734 0.094 Uiso 1 1 calc R
H1D2 H 0.8120 0.5950 -0.5239 0.094 Uiso 1 1 calc R
N2 N 0.91430(10) 0.60439(12) -0.0731(2) 0.0494(5) Uani 1 1 d .
H2 H 0.9542 0.6299 -0.0854 0.059 Uiso 1 1 calc R
C2A C 0.89320(13) 0.58138(15) 0.0564(3) 0.0518(6) Uani 1 1 d .
C2' C 0.84490(11) 0.59971(13) 0.1047(3) 0.0443(5) Uani 1 1 d .
O2 O 0.80894(10) 0.56980(12) 0.1929(2) 0.0589(5) Uani 1 1 d .
C2B C 0.8629(3) 0.5092(2) 0.0623(6) 0.0913(15) Uani 1 1 d .
H2B1 H 0.8268 0.4900 0.0064 0.137 Uiso 1 1 calc R
H2B2 H 0.8495 0.4950 0.1481 0.137 Uiso 1 1 calc R
H2B3 H 0.8933 0.4973 0.0361 0.137 Uiso 1 1 calc R
C2G C 0.95062(17) 0.6147(3) 0.1432(4) 0.0923(16) Uani 1 1 d .
H2G1 H 0.9682 0.6598 0.1369 0.138 Uiso 1 1 calc R
H2G2 H 0.9820 0.6039 0.1178 0.138 Uiso 1 1 calc R
H2G3 H 0.9380 0.6014 0.2297 0.138 Uiso 1 1 calc R
N3 N 0.84594(10) 0.65010(11) 0.0517(3) 0.0481(5) Uani 1 1 d .
H3 H 0.8724 0.6699 -0.0089 0.058 Uiso 1 1 calc R
C3A C 0.80282(14) 0.67251(14) 0.0947(4) 0.0571(7) Uani 1 1 d .
H3A1 H 0.8026 0.6721 0.1882 0.069 Uiso 1 1 calc R
C3' C 0.73432(13) 0.62859(13) 0.0492(3) 0.0499(6) Uani 1 1 d .
O3 O 0.69164(11) 0.63780(11) 0.0872(3) 0.0670(6) Uani 1 1 d .
C3B C 0.8348(2) 0.74467(19) 0.0499(6) 0.0827(11) Uani 1 1 d .
H3B1 H 0.8473 0.7488 -0.0401 0.099 Uiso 1 1 calc R
C3G C 0.7923(3) 0.7715(2) 0.0718(10) 0.121(2) Uani 1 1 d .
H3G1 H 0.7547 0.7488 0.0209 0.182 Uiso 1 1 calc R
H3G2 H 0.8140 0.8156 0.0483 0.182 Uiso 1 1 calc R
H3G3 H 0.7808 0.7674 0.1603 0.182 Uiso 1 1 calc R
C3D C 0.8940(3) 0.7811(2) 0.1360(12) 0.144(4) Uani 1 1 d .
H3D1 H 0.9221 0.7646 0.1234 0.216 Uiso 1 1 calc R
H3D2 H 0.8810 0.7759 0.2238 0.216 Uiso 1 1 calc R
H3D3 H 0.9155 0.8254 0.1144 0.216 Uiso 1 1 calc R
N4 N 0.72296(10) 0.57855(10) -0.0224(2) 0.0468(5) Uani 1 1 d .
H4 H 0.7546 0.5783 -0.0585 0.056 Uiso 1 1 calc R
C4A C 0.65948(13) 0.52415(14) -0.0426(3) 0.0531(6) Uani 1 1 d .
C4' C 0.62680(13) 0.49492(16) 0.0853(3) 0.0566(7) Uani 1 1 d .
O4 O 0.56876(11) 0.46632(17) 0.0940(4) 0.0910(11) Uani 1 1 d .
C4B C 0.61764(17) 0.5429(2) -0.1209(5) 0.0787(11) Uani 1 1 d .
H4B1 H 0.6134 0.5750 -0.0758 0.118 Uiso 1 1 calc R
H4B2 H 0.5764 0.5063 -0.1332 0.118 Uiso 1 1 calc R
H4B3 H 0.6371 0.5592 -0.2023 0.118 Uiso 1 1 calc R
C4G C 0.66725(17) 0.47333(18) -0.1125(5) 0.0738(10) Uani 1 1 d .
H4G1 H 0.6874 0.4896 -0.1933 0.111 Uiso 1 1 calc R
H4G2 H 0.6263 0.4366 -0.1260 0.111 Uiso 1 1 calc R
H4G3 H 0.6929 0.4618 -0.0621 0.111 Uiso 1 1 calc R
N5 N 0.66407(11) 0.49834(13) 0.1827(3) 0.0571(6) Uani 1 1 d .
H5 H 0.7046 0.5188 0.1726 0.069 Uiso 1 1 calc R
C5A C 0.63798(14) 0.46860(14) 0.3043(3) 0.0558(7) Uani 1 1 d .
H5A H 0.5979 0.4290 0.2904 0.067 Uiso 1 1 calc R
C5' C 0.62605(15) 0.51264(16) 0.3885(4) 0.0592(7) Uani 1 1 d .
O5 O 0.66425(17) 0.56641(14) 0.4103(4) 0.0957(11) Uani 1 1 d .
C5B C 0.6847(2) 0.4540(2) 0.3757(4) 0.0720(9) Uani 1 1 d .
H5B H 0.7247 0.4942 0.3856 0.086 Uiso 1 1 calc R
C5G C 0.6986(3) 0.4094(3) 0.2994(8) 0.1109(19) Uani 1 1 d .
H5G1 H 0.7145 0.4274 0.2167 0.166 Uiso 1 1 calc R
H5G2 H 0.6604 0.3693 0.2897 0.166 Uiso 1 1 calc R
H5G3 H 0.7299 0.4034 0.3432 0.166 Uiso 1 1 calc R
C5D C 0.6604(5) 0.4283(5) 0.5085(7) 0.143(3) Uani 1 1 d .
H5D1 H 0.6527 0.4579 0.5545 0.214 Uiso 1 1 calc R
H5D2 H 0.6916 0.4224 0.5530 0.214 Uiso 1 1 calc R
H5D3 H 0.6216 0.3883 0.5018 0.214 Uiso 1 1 calc R
O1M O 0.56725(12) 0.48211(16) 0.4368(3) 0.0774(7) Uani 1 1 d .
C1M C 0.5516(3) 0.5173(3) 0.5252(5) 0.0914(14) Uani 1 1 d .
H1M1 H 0.5085 0.4913 0.5533 0.137 Uiso 1 1 calc R
H1M2 H 0.5562 0.5546 0.4840 0.137 Uiso 1 1 calc R
H1M3 H 0.5795 0.5294 0.5974 0.137 Uiso 1 1 calc R
O1W O 0.998(3) 0.994(2) -0.042(16) 0.26(6) Uani 0.17 1 d P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O C1 C2 109.5(4) . .
O C1 C3 102.7(4) . .
C2 C1 C3 109.0(5) . .
O C1 C4 109.3(4) . .
C2 C1 C4 112.6(5) . .
C3 C1 C4 113.4(5) . .
C0' O C1 121.9(3) . .
O0 C0' O 126.2(3) . .
O0 C0' N1 122.8(3) . .
O C0' N1 111.0(3) . .
C0' N1 C1A 121.4(3) . .
C0' N1 C1D 124.5(3) . .
C1A N1 C1D 114.0(3) . .
N1 C1A C1B 102.6(3) . .
N1 C1A C1' 111.8(2) . .
C1B C1A C1' 112.3(3) . .
O1 C1' N2 123.7(3) . .
O1 C1' C1A 121.2(3) . .
N2 C1' C1A 115.1(2) . .
C1G C1B C1A 107.6(3) . .
C1B C1G C1D 107.1(5) . .
N1 C1D C1G 100.5(3) . .
C1' N2 C2A 124.1(2) . .
N2 C2A C2G 107.4(2) . .
N2 C2A C2B 110.7(3) . .
C2G C2A C2B 112.1(4) . .
N2 C2A C2' 111.6(2) . .
C2G C2A C2' 106.3(3) . .
C2B C2A C2' 108.7(3) . .
O2 C2' N3 122.5(2) . .
O2 C2' C2A 119.8(3) . .
N3 C2' C2A 117.6(2) . .
C2' N3 C3A 121.5(3) . .
N3 C3A C3' 111.9(2) . .
N3 C3A C3B 105.8(3) . .
C3' C3A C3B 115.8(3) . .
O3 C3' N4 122.5(3) . .
O3 C3' C3A 119.5(3) . .
N4 C3' C3A 117.8(2) . .
C3G C3B C3D 108.0(5) . .
C3G C3B C3A 111.9(4) . .
C3D C3B C3A 105.1(5) . .
C3' N4 C4A 123.4(2) . .
N4 C4A C4G 107.4(2) . .
N4 C4A C4' 111.1(3) . .
C4G C4A C4' 106.7(3) . .
N4 C4A C4B 111.3(3) . .
C4G C4A C4B 110.6(3) . .
C4' C4A C4B 109.6(3) . .
O4 C4' N5 122.0(3) . .
O4 C4' C4A 120.6(3) . .
N5 C4' C4A 117.2(2) . .
C4' N5 C5A 121.8(2) . .
N5 C5A C5' 110.4(3) . .
N5 C5A C5B 110.7(3) . .
C5' C5A C5B 107.5(3) . .
O5 C5' O1M 124.7(4) . .
O5 C5' C5A 124.5(3) . .
O1M C5' C5A 110.8(3) . .
C5G C5B C5D 111.6(5) . .
C5G C5B C5A 111.2(4) . .
C5D C5B C5A 111.1(4) . .
C5' O1M C1M 116.3(4) . .
O1W O1W O1W 175.7(14) 6_654 5_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O 1.447(5) .
C1 C2 1.499(8) .
C1 C3 1.509(8) .
C1 C4 1.518(8) .
O C0' 1.344(4) .
C0' O0 1.225(5) .
C0' N1 1.344(4) .
N1 C1A 1.444(4) .
N1 C1D 1.477(4) .
C1A C1B 1.530(4) .
C1A C1' 1.530(4) .
C1' O1 1.227(4) .
C1' N2 1.332(4) .
C1B C1G 1.427(7) .
C1G C1D 1.536(7) .
N2 C2A 1.460(4) .
C2A C2G 1.517(5) .
C2A C2B 1.528(5) .
C2A C2' 1.535(4) .
C2' O2 1.229(4) .
C2' N3 1.334(4) .
N3 C3A 1.473(4) .
C3A C3' 1.537(4) .
C3A C3B 1.594(5) .
C3' O3 1.232(4) .
C3' N4 1.335(4) .
C3B C3G 1.490(7) .
C3B C3D 1.548(8) .
N4 C4A 1.461(3) .
C4A C4G 1.527(5) .
C4A C4' 1.539(5) .
C4A C4B 1.543(4) .
C4' O4 1.226(4) .
C4' N5 1.340(4) .
N5 C5A 1.446(4) .
C5A C5' 1.523(5) .
C5A C5B 1.542(5) .
C5' O5 1.188(5) .
C5' O1M 1.338(4) .
C5B C5G 1.516(7) .
C5B C5D 1.519(8) .
O1M C1M 1.436(6) .
O1W O1W 1.752(4) 6_654
O1W O1W 1.752(4) 5_565
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C2 C1 O C0' -59.9(5)
C3 C1 O C0' -175.5(5)
C4 C1 O C0' 63.9(5)
C1 O C0' O0 -14.5(6)
C1 O C0' N1 165.8(3)
O0 C0' N1 C1A -2.6(5)
O C0' N1 C1A 177.0(3)
O0 C0' N1 C1D 172.1(4)
O C0' N1 C1D -8.2(5)
C0' N1 C1A C1B 174.5(3)
C1D N1 C1A C1B -0.8(4)
C0' N1 C1A C1' 53.9(4)
C1D N1 C1A C1' -121.4(3)
N1 C1A C1' O1 43.8(4)
C1B C1A C1' O1 -71.0(4)
N1 C1A C1' N2 -137.0(3)
C1B C1A C1' N2 108.2(3)
N1 C1A C1B C1G -17.3(6)
C1' C1A C1B C1G 102.9(6)
C1A C1B C1G C1D 28.4(8)
C0' N1 C1D C1G -158.4(5)
C1A N1 C1D C1G 16.7(6)
C1B C1G C1D N1 -27.2(7)
O1 C1' N2 C2A 5.0(5)
C1A C1' N2 C2A -174.2(3)
C1' N2 C2A C2G -175.7(3)
C1' N2 C2A C2B 61.6(4)
C1' N2 C2A C2' -59.6(4)
N2 C2A C2' O2 158.8(3)
C2G C2A C2' O2 -84.4(4)
C2B C2A C2' O2 36.5(4)
N2 C2A C2' N3 -24.2(4)
C2G C2A C2' N3 92.7(3)
C2B C2A C2' N3 -146.5(3)
O2 C2' N3 C3A -1.0(4)
C2A C2' N3 C3A -178.0(3)
C2' N3 C3A C3' -73.9(4)
C2' N3 C3A C3B 159.1(3)
N3 C3A C3' O3 173.4(3)
C3B C3A C3' O3 -65.3(5)
N3 C3A C3' N4 -1.2(4)
C3B C3A C3' N4 120.1(3)
N3 C3A C3B C3G 172.5(5)
C3' C3A C3B C3G 48.0(7)
N3 C3A C3B C3D -70.5(5)
C3' C3A C3B C3D 165.0(5)
O3 C3' N4 C4A -12.0(5)
C3A C3' N4 C4A 162.4(3)
C3' N4 C4A C4G -171.8(3)
C3' N4 C4A C4' -55.4(4)
C3' N4 C4A C4B 67.0(4)
N4 C4A C4' O4 152.9(4)
C4G C4A C4' O4 -90.2(4)
C4B C4A C4' O4 29.5(5)
N4 C4A C4' N5 -31.6(4)
C4G C4A C4' N5 85.3(4)
C4B C4A C4' N5 -155.0(3)
O4 C4' N5 C5A -0.2(6)
C4A C4' N5 C5A -175.7(3)
C4' N5 C5A C5' -85.7(4)
C4' N5 C5A C5B 155.3(3)
N5 C5A C5' O5 -51.1(5)
C5B C5A C5' O5 69.8(5)
N5 C5A C5' O1M 130.3(3)
C5B C5A C5' O1M -108.8(3)
N5 C5A C5B C5G -60.1(4)
C5' C5A C5B C5G 179.2(4)
N5 C5A C5B C5D 174.9(5)
C5' C5A C5B C5D 54.2(6)
O5 C5' O1M C1M -2.8(6)
C5A C5' O1M C1M 175.8(3)
