#------------------------------------------------------------------------------
#$Date: 2017-10-13 11:03:29 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201974 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/21/31/2213115.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2213115
loop_
_publ_author_name
'Yamashita, Motoi'
'Inomata, Shinsuke'
'Ishikawa, Kouki'
'Kashiwagi, Tatsuki'
'Matsuo, Hiroshi'
'Sawamura, Seiji'
'Kato, Minoru'
_publ_section_title
;
 A high-pressure polymorph of <small>L</small>-α-leucine
;
_journal_coeditor_code           BG2041
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2762
_journal_page_last               o2764
_journal_paper_doi               10.1107/S1600536807018764
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C6 H13 N O2'
_chemical_formula_moiety         'C6 H13 N O2'
_chemical_formula_structural     '(C H3 )2 C H C H2 C H (N H2) C O O H'
_chemical_formula_sum            'C6 H13 N O2'
_chemical_formula_weight         131.17
_chemical_name_common            L-α-leucine
_chemical_name_systematic
;
2-ammonio-4-methylpentanoate
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_cell_angle_alpha                90
_cell_angle_beta                 96.17(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.807(3)
_cell_length_b                   5.9750(10)
_cell_length_c                   14.193(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.6
_cell_measurement_theta_min      28.4
_cell_volume                     742.5(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1988)
;
_computing_data_reduction
;
TEXSAN (Molecular Structure Corporation, 2004)
;
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  TEXSAN
_computing_structure_refinement  TEXSAN
_computing_structure_solution    'SIR92 (Altomare et al.,  1994)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.93
_diffrn_measurement_device_type  'Rigaku AFC-5S'
_diffrn_measurement_method       ω--2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            1570
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         79.47
_diffrn_standards_decay_%        2.89
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al.,  1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_density_meas      1.1675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             288.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.17
_refine_diff_density_min         -0.15
_refine_ls_extinction_coef       0.11(2)
_refine_ls_extinction_method
'Zachariasen (1967) type 2, Gaussian isotropic'
_refine_ls_goodness_of_fit_all   1.502
_refine_ls_goodness_of_fit_ref   1.502
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     83
_refine_ls_number_reflns         834
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.0168
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²) + (0.05(Max(Fo²,0) + 2Fc²)/3)²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1039
_refine_ls_wR_factor_ref         0.1039
_reflns_number_gt                756
_reflns_number_total             834
_reflns_threshold_expression     F²>2σ(F²)
_cod_data_source_file            bg2041.cif
_cod_data_source_block           III
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               2213115
_cod_database_fobs_code          2213115
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,y,-z
1/2+x,1/2+y,z
1/2-x,1/2+y,-z
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
O O1 0.40710(10) 0.592(2) 0.60053(9) 0.0373(3) Uani d 1.00
O O2 0.5502(2) 0.900(2) 0.60720(10) 0.0421(4) Uani d 1.00
N N1 0.7934(2) 0.640(2) 0.57270(10) 0.0308(3) Uani d 1.00
C C1 0.6790(2) 0.559(2) 0.63510(10) 0.0300(4) Uani d 1.00
C C2 0.5317(2) 0.693(2) 0.61210(10) 0.0300(4) Uani d 1.00
C C3 0.7453(2) 0.591(2) 0.73820(10) 0.0395(5) Uani d 1.00
C C4 0.6481(3) 0.493(2) 0.8107(2) 0.0534(6) Uani d 1.00
C C5 0.6636(4) 0.239(2) 0.8159(2) 0.0750(9) Uani d 1.00
C C6 0.6968(6) 0.595(2) 0.9079(2) 0.1030(10) Uani d 1.00
H H1 0.6594 0.4026 0.6233 0.0365 Uiso calc 1.00
H H2 0.7558 0.7455 0.7499 0.0486 Uiso calc 1.00
H H3 0.8430 0.5206 0.7466 0.0486 Uiso calc 1.00
H H4 0.5441 0.5268 0.7925 0.0657 Uiso calc 1.00
H H5 0.7669 0.1987 0.8356 0.0911 Uiso calc 1.00
H H6 0.6341 0.1747 0.7551 0.0911 Uiso calc 1.00
H H7 0.5998 0.1798 0.8600 0.0911 Uiso calc 1.00
H H8 0.8005 0.5607 0.9265 0.1220 Uiso calc 1.00
H H9 0.6353 0.5318 0.9531 0.1220 Uiso calc 1.00
H H10 0.6818 0.7507 0.9049 0.1220 Uiso calc 1.00
H H11 0.8854 0.5561 0.5855 0.0376 Uiso calc 1.00
H H12 0.7542 0.6195 0.5083 0.0376 Uiso calc 1.00
H H13 0.8133 0.7930 0.5849 0.0376 Uiso calc 1.00
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
O1 0.0243(6) 0.0374(7) 0.0493(7) -0.0031(5) -0.0006(5) 0.0008(6)
O2 0.0252(7) 0.0277(6) 0.0723(10) 0.0064(5) 0.0009(6) -0.0016(6)
N1 0.0237(7) 0.0275(7) 0.0408(7) 0.0045(6) 0.0018(5) -0.0002(5)
C1 0.0248(8) 0.0271(8) 0.0377(7) 0.0034(6) 0.0014(6) -0.0002(6)
C2 0.0251(8) 0.0283(7) 0.0360(8) 0.0038(6) 0.0006(6) -0.0023(6)
C3 0.0370(10) 0.0400(10) 0.0393(8) 0.0054(8) -0.0062(6) -0.0007(7)
C4 0.0510(10) 0.0670(10) 0.0430(10) 0.0140(10) 0.0085(9) 0.0078(9)
C5 0.093(2) 0.0650(10) 0.066(2) -0.019(2) 0.000(2) 0.0120(10)
C6 0.184(4) 0.083(2) 0.0410(10) 0.007(3) 0.012(2) -0.0040(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.018 0.009
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
N N 0.031 0.018
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
O O 0.049 0.032
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
0 0 4
0 0 5
-2 0 5
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
C1 N1 H11 109.1 no
C1 N1 H12 109.2 no
C1 N1 H13 109.4 no
H11 N1 H12 109.0 no
H11 N1 H13 109.9 no
H12 N1 H13 110.3 no
N1 C1 C2 108.4(7) ?
N1 C1 C3 108.3(2) ?
N1 C1 H1 109.6 no
C2 C1 C3 111.5(5) ?
C2 C1 H1 109.9 no
C3 C1 H1 109.4 no
O1 C2 O2 126.1(7) ?
O1 C2 C1 119.3(11) ?
O2 C2 C1 114.7(5) ?
C1 C3 C4 114.5(5) ?
C1 C3 H2 108.2 no
C1 C3 H3 108.1 no
C4 C3 H2 108.1 no
C4 C3 H3 108.1 no
H2 C3 H3 109.9 no
C3 C4 C5 111.2(3) ?
C3 C4 C6 109.4(3) ?
C3 C4 H4 109.2 no
C5 C4 C6 109.9(3) ?
C5 C4 H4 107.9 no
C6 C4 H4 109.2 no
C4 C5 H5 110.1 no
C4 C5 H6 110.1 no
C4 C5 H7 110.2 no
H5 C5 H6 108.8 no
H5 C5 H7 108.9 no
H6 C5 H7 108.8 no
C4 C6 H8 109.6 no
C4 C6 H9 108.9 no
C4 C6 H10 109.3 no
H8 C6 H9 108.9 no
H8 C6 H10 110.6 no
H9 C6 H10 109.4 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C2 1.248(8) yes
O2 C2 1.250(17) yes
N1 C1 1.493(3) yes
N1 H11 0.955 no
N1 H12 0.951 no
N1 H13 0.941 no
C1 C2 1.530(9) yes
C1 C3 1.528(3) yes
C1 H1 0.960 no
C3 C4 1.526(4) yes
C3 H2 0.942 no
C3 H3 0.954 no
C4 C5 1.525(17) yes
C4 C6 1.526(5) yes
C4 H4 0.947 no
C5 H5 0.954 no
C5 H6 0.954 no
C5 H7 0.954 no
C6 H8 0.946 no
C6 H9 0.960 no
C6 H10 0.941 no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
O1 N1 2.884(2) 2_656
O1 N1 2.893(16) 3_445
O1 C2 3.179(3) 2_656
O1 C1 3.355(2) 2_656
O1 O2 3.357(6) 3_445
O1 N1 3.434(16) 3_455
O1 O1 3.439(3) 2_656
O1 C1 3.503(14) 3_455
O1 O2 3.530(9) 2_656
O2 N1 2.678(9) 3_455
O2 O2 3.078(4) 2_656
O2 N1 3.351(8) 4_656
O2 C2 3.355(7) 2_656
O2 C1 3.467(3) 3_455
N1 C2 3.406(13) 3_545
C2 C2 3.170(4) 2_656
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H13 O1 3_555 0.940 1.972 2.890(10) 165.100 yes
N1 H12 O1 2_656 0.951 1.990 2.884(2) 155.910 yes
N1 H11 O2 3_545 0.955 1.725 2.680(8) 178.977 yes
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
O1 C2 C1 N1 133.1(5)
O1 C2 C1 C3 -107.8(7)
O2 C2 C1 N1 -47.3(6)
O2 C2 C1 C3 71.9(7)
N1 C1 C3 C4 -173.9(9)
C1 C3 C4 C5 76.1(8)
C1 C3 C4 C6 -162.5(8)
C2 C1 C3 C4 67.0(12)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 5880
