#------------------------------------------------------------------------------
#$Date: 2019-06-20 14:25:37 +0300 (Thu, 20 Jun 2019) $
#$Revision: 216253 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/16/1551642.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_1551642
loop_
_publ_author_name
'INADA, Aya'
'KANAZAWA, Hitoshi'
'UEKUSA, Hidehiro'
_publ_section_title
;
 Crystal Structure of <font size=-1>L</font>-Isoleucine
 N-Carboxy Anhydride
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              17
_journal_paper_doi               10.2116/xraystruct.31.17
_journal_volume                  31
_journal_year                    2015
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C7 H11 N O3'
_chemical_formula_sum            'C7 H11 N O3'
_chemical_formula_weight         157.17
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'by CrystalStructure 4.0'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.4713(3)
_cell_length_b                   6.7196(3)
_cell_length_c                   17.9369(7)
_cell_measurement_reflns_used    8122
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      68.03
_cell_measurement_theta_min      4.93
_cell_volume                     779.98(6)
_computing_cell_refinement       'RAPID-AUTO (RIGAKU)'
_computing_data_collection       'RAPID-AUTO (RIGAKU)'
_computing_data_reduction        'RAPID-AUTO (RIGAKU)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_pressure         101.3
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'R-AXIS RAPID-II'
_diffrn_measurement_method       ω-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8122
_diffrn_reflns_theta_full        68.03
_diffrn_reflns_theta_max         68.03
_diffrn_reflns_theta_min         4.93
_exptl_absorpt_coefficient_mu    0.883
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.232
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         1409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0592P)²+0.2827P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1332
_reflns_number_gt                1221
_reflns_number_total             1409
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            31_17_1.txt
_cod_data_source_block           shelxl
_cod_database_code               1551642
_shelxl_version_number           97
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
C1 C -0.1089(5) -0.1462(4) 0.59007(15) 0.0348(7) Uani 1 1 d .
C2 C -0.0007(5) 0.0283(3) 0.69066(14) 0.0303(6) Uani 1 1 d .
C3 C 0.1898(4) -0.0253(4) 0.64661(14) 0.0299(7) Uani 1 1 d .
C4 C 0.3039(4) 0.1585(4) 0.61539(15) 0.0324(7) Uani 1 1 d .
C5 C 0.1553(5) 0.2961(4) 0.57404(16) 0.0388(8) Uani 1 1 d .
C6 C 0.4257(4) 0.2656(4) 0.67557(15) 0.0357(7) Uani 1 1 d .
C7 C 0.5651(5) 0.4290(5) 0.64400(17) 0.0442(8) Uani 1 1 d .
H1 H 0.169(5) -0.193(4) 0.5434(19) 0.042 Uiso 1 1 d .
H3 H 0.2858 -0.1070 0.6778 0.036 Uiso 1 1 calc R
H4 H 0.4061 0.1088 0.5779 0.039 Uiso 1 1 calc R
H5A H 0.2334 0.4036 0.5502 0.047 Uiso 1 1 calc R
H5B H 0.0562 0.3529 0.6094 0.047 Uiso 1 1 calc R
H5C H 0.0808 0.2201 0.5359 0.047 Uiso 1 1 calc R
H6A H 0.5118 0.1677 0.7027 0.043 Uiso 1 1 calc R
H6B H 0.3282 0.3254 0.7117 0.043 Uiso 1 1 calc R
H7A H 0.4868 0.5534 0.6401 0.053 Uiso 1 1 calc R
H7B H 0.6144 0.3896 0.5945 0.053 Uiso 1 1 calc R
H7C H 0.6836 0.4488 0.6772 0.053 Uiso 1 1 calc R
N1 N 0.0983(4) -0.1473(4) 0.58848(13) 0.0353(6) Uani 1 1 d .
O1 O -0.2343(4) -0.2147(3) 0.54785(12) 0.0492(7) Uani 1 1 d .
O2 O -0.1728(3) -0.0416(3) 0.65333(10) 0.0338(5) Uani 1 1 d .
O3 O -0.0181(3) 0.1198(3) 0.74778(9) 0.0353(5) Uani 1 1 d .
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 0.0091 '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 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
C2 O2 C1 109.0(2)
C1 N1 C3 112.9(3)
C1 N1 H1 119.2(18)
C3 N1 H1 125.4(18)
O1 C1 N1 131.3(3)
O1 C1 O2 120.3(3)
N1 C1 O2 108.4(3)
O3 C2 O2 120.8(3)
O3 C2 C3 130.3(3)
O2 C2 C3 108.89(19)
N1 C3 C2 100.2(2)
N1 C3 C4 112.7(2)
C2 C3 C4 112.9(2)
N1 C3 H3 110.2
C2 C3 H3 110.2
C4 C3 H3 110.2
C6 C4 C5 112.7(2)
C6 C4 C3 111.7(2)
C5 C4 C3 111.1(2)
C6 C4 H4 107.0
C5 C4 H4 107.0
C3 C4 H4 107.0
C4 C5 H5A 109.5
C4 C5 H5B 109.5
H5A C5 H5B 109.5
C4 C5 H5C 109.5
H5A C5 H5C 109.5
H5B C5 H5C 109.5
C4 C6 C7 112.5(2)
C4 C6 H6A 109.1
C7 C6 H6A 109.1
C4 C6 H6B 109.1
C7 C6 H6B 109.1
H6A C6 H6B 107.8
C6 C7 H7A 109.5
C6 C7 H7B 109.5
H7A C7 H7B 109.5
C6 C7 H7C 109.5
H7A C7 H7C 109.5
H7B C7 H7C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
O1 C1 1.202(3)
O2 C2 1.382(3)
O2 C1 1.398(3)
O3 C2 1.200(3)
N1 C1 1.341(4)
N1 C3 1.452(3)
N1 H1 0.98(3)
C2 C3 1.508(4)
C3 C4 1.544(4)
C3 H3 1.0000
C4 C6 1.518(4)
C4 C5 1.526(4)
C4 H4 1.0000
C5 H5A 0.9800
C5 H5B 0.9800
C5 H5C 0.9800
C6 C7 1.530(4)
C6 H6A 0.9900
C6 H6B 0.9900
C7 H7A 0.9800
C7 H7B 0.9800
C7 H7C 0.9800
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1 O1 0.98(3) 1.86(4) 2.831(4) 172(3) 2_546 y
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
C3 N1 C1 O1 173.0(3)
C3 N1 C1 O2 -6.0(4)
C2 O2 C1 O1 -177.5(2)
C2 O2 C1 N1 1.6(3)
C1 O2 C2 O3 -178.5(2)
C1 O2 C2 C3 3.1(3)
C1 N1 C3 C2 7.4(3)
C1 N1 C3 C4 -112.9(3)
O3 C2 C3 N1 175.8(3)
O2 C2 C3 N1 -6.1(2)
O3 C2 C3 C4 -64.1(4)
O2 C2 C3 C4 114.1(2)
N1 C3 C4 C6 -171.2(2)
C2 C3 C4 C6 76.1(3)
N1 C3 C4 C5 62.1(3)
C2 C3 C4 C5 -50.6(3)
C5 C4 C6 C7 -62.7(3)
C3 C4 C6 C7 171.4(2)
