#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/10/12/4101259.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_4101259
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 O4'
_chemical_formula_weight         218.25
_chemical_name_common            Leu-Ser
_chemical_name_systematic
;
 L-Leucyl-L-Serine
;
_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                   18.138(2)
_cell_length_b                   18.138(2)
_cell_length_c                   6.163(1)
_cell_measurement_reflns_used    5846
_cell_measurement_temperature    293(2)
_cell_volume                     1755.9(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0103
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            20062
_diffrn_reflns_theta_full        28.73
_diffrn_reflns_theta_max         28.73
_diffrn_reflns_theta_min         3.55
_exptl_absorpt_coefficient_mu    0.097
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.111
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.2(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2977
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0289
_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)+(0.0608P)²+0.0358P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0815
_reflns_number_gt                2868
_reflns_number_total             2977
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja060474jsi20060127_030544.cif
_cod_data_source_block           ls
_cod_original_sg_symbol_H-M      P65
_cod_database_code               4101259
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'x-y, x, z+5/6'
'y, -x+y, z+1/6'
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 0.44467(6) 0.08350(5) -0.32699(13) 0.02851(17) Uani 1 1 d .
H1 H 0.4917 0.1226 -0.4210 0.034 Uiso 1 1 calc R
N1 N 0.45075(5) 0.00538(4) -0.29691(12) 0.02830(15) Uani 1 1 d .
H1A H 0.4203 -0.0231 -0.1816 0.042 Uiso 1 1 calc R
H1B H 0.5049 0.0199 -0.2769 0.042 Uiso 1 1 calc R
H1C H 0.4306 -0.0273 -0.4143 0.042 Uiso 1 1 calc R
C2 C 0.45761(6) 0.12499(6) -0.10416(15) 0.03001(17) Uani 1 1 d .
O1 O 0.44675(6) 0.08389(5) 0.06290(12) 0.04128(18) Uani 1 1 d .
N2 N 0.47813(6) 0.20678(5) -0.10983(13) 0.03258(17) Uani 1 1 d .
H2 H 0.4929 0.2337 -0.2312 0.039 Uiso 1 1 calc R
C3 C 0.47608(6) 0.25104(5) 0.08382(13) 0.02870(17) Uani 1 1 d .
H3 H 0.4222 0.2146 0.1590 0.034 Uiso 1 1 calc R
C4 C 0.47844(6) 0.33419(5) 0.02087(15) 0.02937(17) Uani 1 1 d .
O2 O 0.47972(6) 0.35214(5) -0.17377(12) 0.04369(19) Uani 1 1 d .
O3 O 0.48253(6) 0.38007(5) 0.17821(13) 0.04173(18) Uani 1 1 d .
C5 C 0.36085(7) 0.06270(6) -0.43806(17) 0.0374(2) Uani 1 1 d .
H5A H 0.3598 0.1154 -0.4537 0.045 Uiso 1 1 calc R
H5B H 0.3613 0.0421 -0.5830 0.045 Uiso 1 1 calc R
C6 C 0.27804(8) -0.00222(10) -0.3277(3) 0.0578(3) Uani 1 1 d .
H6 H 0.2848 -0.0494 -0.2748 0.069 Uiso 1 1 calc R
C7 C 0.25505(13) 0.0354(3) -0.1366(4) 0.1128(11) Uani 1 1 d .
H7A H 0.2539 0.0853 -0.1830 0.169 Uiso 1 1 calc R
H7B H 0.2967 0.0504 -0.0240 0.169 Uiso 1 1 calc R
H7C H 0.2000 -0.0058 -0.0822 0.169 Uiso 1 1 calc R
C8 C 0.20695(10) -0.03690(12) -0.4976(4) 0.0777(5) Uani 1 1 d .
H8A H 0.1549 -0.0799 -0.4329 0.117 Uiso 1 1 calc R
H8B H 0.2220 -0.0612 -0.6159 0.117 Uiso 1 1 calc R
H8C H 0.1993 0.0086 -0.5506 0.117 Uiso 1 1 calc R
C9 C 0.54877(7) 0.26867(7) 0.23941(15) 0.0360(2) Uani 1 1 d .
H9A H 0.5583 0.2206 0.2388 0.043 Uiso 1 1 calc R
H9B H 0.6006 0.3184 0.1903 0.043 Uiso 1 1 calc R
O4 O 0.53000(7) 0.28268(6) 0.45330(12) 0.0454(2) Uani 1 1 d .
H4 H 0.5197 0.3218 0.4531 0.068 Uiso 1 1 calc R
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 106.93(7)
N1 C1 C5 110.99(7)
C2 C1 C5 114.34(8)
O1 C2 N2 124.52(8)
O1 C2 C1 121.10(7)
N2 C2 C1 114.34(8)
C2 N2 C3 121.54(7)
N2 C3 C9 111.97(8)
N2 C3 C4 109.87(7)
C9 C3 C4 110.79(8)
O2 C4 O3 125.87(9)
O2 C4 C3 119.30(8)
O3 C4 C3 114.76(8)
C6 C5 C1 117.56(9)
C7 C6 C5 112.52(16)
C7 C6 C8 110.52(15)
C5 C6 C8 108.28(14)
O4 C9 C3 111.22(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N1 1.4869(11)
C1 C2 1.5267(12)
C1 C5 1.5326(14)
C2 O1 1.2279(12)
C2 N2 1.3372(11)
N2 C3 1.4492(11)
C3 C9 1.5292(13)
C3 C4 1.5371(11)
C4 O2 1.2401(13)
C4 O3 1.2555(12)
C5 C6 1.5286(17)
C6 C7 1.520(3)
C6 C8 1.531(2)
C9 O4 1.4158(12)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 5360279
