#------------------------------------------------------------------------------
#$Date: 2017-10-13 13:42:48 +0200 (vie 13 de oct de 2017) $
#$Revision: 201982 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/12/4101261.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_4101261
loop_
_publ_author_name
'Soldatov, Dmitriy V'
'Moudrakovski, Igor L'
'Grachev, Eugeny V'
'Ripmeester, John A'
_publ_section_title
;
 Micropores in crystalline dipeptides as seen from the crystal
 structure, He pycnometry, and 129Xe NMR spectroscopy.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6737
_journal_page_last               6744
_journal_paper_doi               10.1021/ja060474j
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C9 H18 N2 O3'
_chemical_formula_weight         202.25
_chemical_name_common            Ile-Ala
_chemical_name_systematic
;
 L-Isoleucyl-L-Alanine
;
_space_group_IT_number           169
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 61'
_symmetry_space_group_name_H-M   'P 61'
_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                   14.481(2)
_cell_length_b                   14.481(2)
_cell_length_c                   10.037(1)
_cell_measurement_reflns_used    7219
_cell_measurement_temperature    293(2)
_cell_volume                     1822.8(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'SMART CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0147
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            21121
_diffrn_reflns_theta_full        28.73
_diffrn_reflns_theta_max         28.73
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    0.083
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.167
_refine_diff_density_min         -0.142
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.7(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         3112
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0594P)²+0.1348P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0950
_reflns_number_gt                2862
_reflns_number_total             3112
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja060474jsi20060127_030631.cif
_cod_data_source_block           ia
_cod_original_sg_symbol_H-M      P61
_cod_database_code               4101261
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'x-y, x, z+1/6'
'y, -x+y, 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 0.48645(9) 0.22187(8) 1.37238(12) 0.0301(2) Uani 1 1 d .
H1 H 0.4882 0.1773 1.4447 0.036 Uiso 1 1 calc R
N1 N 0.53114(8) 0.33290(7) 1.42251(10) 0.02942(18) Uani 1 1 d .
H1A H 0.5921 0.3526 1.4650 0.044 Uiso 1 1 calc R
H1B H 0.4849 0.3359 1.4783 0.044 Uiso 1 1 calc R
H1C H 0.5431 0.3767 1.3542 0.044 Uiso 1 1 calc R
C2 C 0.56155(9) 0.22751(9) 1.26218(12) 0.0305(2) Uani 1 1 d .
O1 O 0.62341(8) 0.31449(7) 1.21117(11) 0.0450(2) Uani 1 1 d .
N2 N 0.55477(8) 0.13701(7) 1.22450(10) 0.0335(2) Uani 1 1 d .
H2 H 0.5122 0.0786 1.2651 0.040 Uiso 1 1 calc R
C3 C 0.61962(10) 0.13631(9) 1.11393(12) 0.0352(2) Uani 1 1 d .
H3 H 0.6264 0.1901 1.0492 0.042 Uiso 1 1 calc R
C4 C 0.56613(9) 0.02760(9) 1.04353(12) 0.0321(2) Uani 1 1 d .
O2 O 0.50897(10) -0.05207(8) 1.11079(12) 0.0570(3) Uani 1 1 d .
O3 O 0.59057(8) 0.02874(7) 0.92358(9) 0.0413(2) Uani 1 1 d .
C5 C 0.37101(10) 0.17491(12) 1.32480(16) 0.0465(3) Uani 1 1 d .
H5 H 0.3521 0.1086 1.2775 0.056 Uiso 1 1 calc R
C6 C 0.29594(13) 0.14538(15) 1.4436(2) 0.0675(5) Uani 1 1 d .
H6A H 0.3102 0.1034 1.5054 0.101 Uiso 1 1 calc R
H6B H 0.2235 0.1049 1.4135 0.101 Uiso 1 1 calc R
H6C H 0.3068 0.2092 1.4869 0.101 Uiso 1 1 calc R
C7 C 0.35793(16) 0.24838(19) 1.2257(2) 0.0731(5) Uani 1 1 d .
H7A H 0.3599 0.3071 1.2747 0.088 Uiso 1 1 calc R
H7B H 0.4183 0.2783 1.1653 0.088 Uiso 1 1 calc R
C8 C 0.2570(3) 0.1953(4) 1.1444(4) 0.1331(14) Uani 1 1 d .
H8A H 0.2580 0.1428 1.0870 0.200 Uiso 1 1 calc R
H8B H 0.2519 0.2479 1.0916 0.200 Uiso 1 1 calc R
H8C H 0.1966 0.1613 1.2029 0.200 Uiso 1 1 calc R
C9 C 0.73072(14) 0.1649(2) 1.1588(3) 0.0774(7) Uani 1 1 d .
H9A H 0.7637 0.2329 1.2027 0.116 Uiso 1 1 calc R
H9B H 0.7725 0.1685 1.0827 0.116 Uiso 1 1 calc R
H9C H 0.7263 0.1116 1.2194 0.116 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0338(5) 0.0286(5) 0.0295(5) 0.0006(4) 0.0037(4) 0.0167(4)
N1 0.0346(4) 0.0309(4) 0.0265(4) -0.0009(4) -0.0011(4) 0.0191(4)
C2 0.0318(5) 0.0306(5) 0.0278(5) 0.0011(4) 0.0030(4) 0.0147(4)
O1 0.0511(5) 0.0304(4) 0.0486(5) 0.0057(4) 0.0203(5) 0.0166(4)
N2 0.0397(5) 0.0297(4) 0.0301(5) 0.0008(4) 0.0091(4) 0.0165(4)
C3 0.0355(5) 0.0310(5) 0.0321(6) -0.0044(4) 0.0078(4) 0.0114(4)
C4 0.0339(5) 0.0278(5) 0.0319(6) -0.0015(4) 0.0045(4) 0.0135(4)
O2 0.0680(7) 0.0317(4) 0.0507(6) 0.0024(4) 0.0267(5) 0.0094(4)
O3 0.0571(5) 0.0307(4) 0.0291(4) -0.0010(3) 0.0056(4) 0.0168(4)
C5 0.0338(6) 0.0441(7) 0.0564(8) -0.0136(6) -0.0004(6) 0.0156(5)
C6 0.0402(7) 0.0645(10) 0.0870(13) -0.0108(10) 0.0175(8) 0.0182(7)
C7 0.0607(10) 0.0938(14) 0.0756(13) -0.0096(11) -0.0246(10) 0.0467(10)
C8 0.0907(19) 0.202(4) 0.111(2) -0.025(3) -0.0499(18) 0.076(2)
C9 0.0408(8) 0.1015(16) 0.0831(14) -0.0451(12) -0.0087(8) 0.0305(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
N1 C1 C2 105.91(9)
N1 C1 C5 111.92(9)
C2 C1 C5 112.85(10)
O1 C2 N2 123.39(11)
O1 C2 C1 119.34(10)
N2 C2 C1 117.25(10)
C2 N2 C3 119.80(10)
N2 C3 C9 111.81(13)
N2 C3 C4 111.17(9)
C9 C3 C4 109.85(12)
O2 C4 O3 126.32(11)
O2 C4 C3 117.79(11)
O3 C4 C3 115.75(10)
C6 C5 C1 110.33(14)
C6 C5 C7 112.56(16)
C1 C5 C7 112.30(12)
C8 C7 C5 114.9(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N1 1.4888(14)
C1 C2 1.5245(15)
C1 C5 1.5324(18)
C2 O1 1.2340(15)
C2 N2 1.3197(14)
N2 C3 1.4570(15)
C3 C9 1.515(2)
C3 C4 1.5356(16)
C4 O2 1.2317(15)
C4 O3 1.2527(15)
C5 C6 1.524(2)
C5 C7 1.536(3)
C7 C8 1.507(3)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 5373156
