#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2006172.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_2006172
loop_
_publ_author_name
'G\"orbitz, C. H.'
_publ_section_title
;
Cyclic Water Pentamers in
L-Leucyl-L-alanine Tetrahydrate
;
_journal_issue 6
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first 736
_journal_page_last 739
_journal_volume 53
_journal_year 1997
_chemical_formula_iupac 'C9 H18 N2 O3 , 4H2 O'
_chemical_formula_sum 'C9 H26 N2 O7'
_chemical_formula_weight 274.32
_chemical_name_systematic
;
L-leucyl-L-alanine tetrahydrate
;
_space_group_IT_number 19
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'P 2ac 2ab'
_symmetry_space_group_name_H-M 'P 21 21 21'
_audit_creation_method SHELXL
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 6.1863(2)
_cell_length_b 12.5481(4)
_cell_length_c 19.8831(6)
_cell_measurement_reflns_used 19345
_cell_measurement_temperature 150(2)
_cell_volume 1543.45(8)
_computing_cell_refinement 'SAINT (Siemens, 1995)'
_computing_data_collection 'SMART (Siemens, 1995)'
_computing_data_reduction SAINT
_computing_molecular_graphics SHELXTL
_computing_publication_material SHELXTL
_computing_structure_refinement SHELXTL
_computing_structure_solution 'SHELXTL (Sheldrick, 1994)'
_diffrn_ambient_temperature 150(2)
_diffrn_measurement_device 'Siemens SMART CCD diffractometer'
_diffrn_measurement_method
'Sets of exsposures each taken over 0.6\% \w rotation'
_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 0.0251
_diffrn_reflns_av_sigmaI/netI 0.0268
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_l_max 34
_diffrn_reflns_limit_l_min -33
_diffrn_reflns_number 23659
_diffrn_reflns_theta_max 38.24
_diffrn_reflns_theta_min 1.92
_diffrn_standards_decay_% none
_exptl_absorpt_coefficient_mu 0.100
_exptl_absorpt_correction_T_max 0.990
_exptl_absorpt_correction_T_min 0.946
_exptl_absorpt_correction_type 'multi-scan (SADABS; Sheldrick, 1996)'
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 1.181
_exptl_crystal_density_meas 'not measured'
_exptl_crystal_description Block
_exptl_crystal_F_000 600
_exptl_crystal_size_max 0.50
_exptl_crystal_size_mid 0.35
_exptl_crystal_size_min 0.10
_refine_diff_density_max 0.348
_refine_diff_density_min -0.164
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_all 1.142
_refine_ls_goodness_of_fit_obs 1.137
_refine_ls_hydrogen_treatment refall
_refine_ls_matrix_type full
_refine_ls_number_parameters 224
_refine_ls_number_reflns 7987
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.147
_refine_ls_restrained_S_obs 1.137
_refine_ls_R_factor_all 0.0455
_refine_ls_R_factor_obs 0.0380
_refine_ls_shift/esd_max -0.009
_refine_ls_shift/esd_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.0365P)^2^+0.1600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all 0.0905
_refine_ls_wR_factor_obs 0.0857
_reflns_number_observed 7250
_reflns_number_total 7988
_reflns_observed_criterion >2sigma(I)
_[local]_cod_data_source_file ab1443.cif
_[local]_cod_data_source_block lax2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana
;
_cod_database_code 2006172
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
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 0.0168(2) 0.0212(3) 0.0420(4) -0.0046(2) 0.0057(2) -0.0116(2)
O2 0.0118(2) 0.0263(3) 0.0225(3) -0.0013(2) 0.0019(2) 0.0013(2)
O3 0.0180(2) 0.0283(3) 0.0192(2) 0.0033(2) 0.0007(2) 0.0081(2)
O40 0.0168(2) 0.0199(3) 0.0292(3) -0.0016(2) 0.0042(2) -0.0068(2)
O50 0.0279(3) 0.0345(3) 0.0209(3) -0.0018(3) 0.0033(2) 0.0023(2)
O60 0.0251(3) 0.0321(3) 0.0211(3) 0.0023(2) -0.0003(2) 0.0042(2)
O70 0.0319(3) 0.0390(4) 0.0284(4) -0.0036(3) -0.0026(3) 0.0024(3)
N1 0.0153(2) 0.0174(3) 0.0161(2) 0.0023(2) -0.0005(2) -0.0014(2)
N2 0.0111(2) 0.0147(2) 0.0177(2) 0.0001(2) 0.0003(2) -0.0022(2)
C1 0.0143(2) 0.0157(3) 0.0185(3) 0.0015(2) 0.0011(2) -0.0026(2)
C2 0.0210(3) 0.0197(3) 0.0191(3) 0.0038(2) -0.0003(2) 0.0017(2)
C3 0.0267(3) 0.0218(3) 0.0174(3) 0.0051(3) 0.0030(3) 0.0013(2)
C4 0.0291(4) 0.0564(7) 0.0360(5) -0.0098(5) 0.0084(4) -0.0083(5)
C5 0.0441(5) 0.0331(5) 0.0179(3) -0.0008(4) 0.0014(3) 0.0019(3)
C6 0.0137(2) 0.0152(3) 0.0198(3) 0.0002(2) 0.0006(2) -0.0026(2)
C7 0.0127(2) 0.0156(3) 0.0142(2) 0.0009(2) 0.0006(2) -0.0005(2)
C8 0.0203(3) 0.0251(4) 0.0258(3) 0.0013(3) -0.0041(3) -0.0115(3)
C9 0.0127(2) 0.0127(2) 0.0161(3) 0.0000(2) 0.0000(2) -0.0009(2)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
O1 0.50375(10) 0.28280(5) 0.81683(4) 0.02667(13) Uani d . 1 O
O2 0.14186(9) 0.48564(5) 0.87024(3) 0.02019(11) Uani d . 1 O
O3 0.35644(10) 0.53549(5) 0.78543(3) 0.02186(11) Uani d . 1 O
O40 1.31092(10) 0.09838(5) 0.78972(3) 0.02198(11) Uani d . 1 O
H401 1.396(3) 0.0645(14) 0.7638(8) 0.041(4) Uiso d . 1 H
H402 1.375(3) 0.1601(14) 0.7967(8) 0.038(4) Uiso d . 1 H
O50 0.90250(13) 0.17615(6) 0.93207(3) 0.02779(13) Uani d . 1 O
H501 0.808(4) 0.1594(17) 0.9586(11) 0.064(6) Uiso d . 1 H
H502 1.006(4) 0.1364(16) 0.9360(9) 0.056(5) Uiso d . 1 H
O60 0.56313(11) 0.13037(6) 1.01698(3) 0.02611(13) Uani d . 1 O
H601 0.597(3) 0.0928(14) 1.0492(9) 0.040(4) Uiso d . 1 H
H602 0.516(5) 0.188(2) 1.0331(14) 0.106(9) Uiso d . 1 H
O70 1.25613(13) 0.04658(7) 0.92882(4) 0.0331(2) Uani d . 1 O
H701 1.294(3) 0.0558(14) 0.8910(10) 0.047(4) Uiso d . 1 H
H702 1.360(3) 0.0715(14) 0.9523(9) 0.049(5) Uiso d . 1 H
N1 0.89304(10) 0.17493(5) 0.78995(3) 0.01624(10) Uani d . 1 N
H1 1.021(3) 0.1568(11) 0.7835(7) 0.027(3) Uiso d . 1 H
H2 0.873(2) 0.1657(11) 0.8337(7) 0.026(3) Uiso d . 1 H
H3 0.801(2) 0.1354(11) 0.7643(7) 0.027(3) Uiso d . 1 H
N2 0.70061(9) 0.42701(5) 0.84481(3) 0.01451(10) Uani d . 1 N
H4 0.829(3) 0.4561(11) 0.8483(7) 0.030(3) Uiso d . 1 H
C1 0.86784(11) 0.29109(6) 0.77393(4) 0.01616(11) Uani d . 1 C
H11 0.9939(18) 0.3280(5) 0.7862(2) 0.019 Uiso calc R 1 H
C2 0.82447(13) 0.30629(6) 0.69839(4) 0.01992(13) Uani d . 1 C
H21 0.6999(12) 0.2638(4) 0.68607(13) 0.024 Uiso calc R 1 H
H22 0.7879(4) 0.3803(7) 0.69052(9) 0.024 Uiso calc R 1 H
C3 1.01332(14) 0.27607(7) 0.65201(4) 0.02198(14) Uani d . 1 C
H31 1.0683(8) 0.2073(10) 0.6660(2) 0.026 Uiso calc R 1 H
C4 1.1969(2) 0.35682(11) 0.65626(6) 0.0405(3) Uani d . 1 C
H41 1.2458(14) 0.3636(7) 0.7042(5) 0.061(3) Uiso calc R 1 H
H42 1.1449(8) 0.4279(8) 0.6397(6) 0.061(3) Uiso calc R 1 H
H43 1.3211(16) 0.3321(5) 0.6277(6) 0.061(3) Uiso calc R 1 H
C5 0.9321(2) 0.26640(9) 0.57966(5) 0.0317(2) Uani d . 1 C
H51 0.8240(16) 0.2084(8) 0.57685(12) 0.045(2) Uiso calc R 1 H
H52 1.0551(12) 0.2501(8) 0.5495(3) 0.045(2) Uiso calc R 1 H
H53 0.8647(16) 0.3344(7) 0.5657(2) 0.045(2) Uiso calc R 1 H
C6 0.67605(11) 0.33310(6) 0.81430(4) 0.01625(11) Uani d . 1 C
C7 0.52355(11) 0.46874(6) 0.88598(3) 0.01419(10) Uani d . 1 C
H71 0.4822(5) 0.4145(7) 0.9192(4) 0.017 Uiso calc R 1 H
C8 0.59936(13) 0.56854(7) 0.92318(5) 0.02371(15) Uani d . 1 C
H81 0.7319(15) 0.5530(3) 0.9473(4) 0.037(2) Uiso calc R 1 H
H82 0.4889(12) 0.5908(5) 0.9548(4) 0.037(2) Uiso calc R 1 H
H83 0.6254(14) 0.6252(6) 0.8911(3) 0.037(2) Uiso calc R 1 H
C9 0.32399(10) 0.49722(5) 0.84317(4) 0.01384(10) Uani d . 1 C
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
_geom_angle_publ_flag
C1 N1 H1 109.3(9) ?
C1 N1 H2 108.7(9) ?
H1 N1 H2 104.4(13) ?
C1 N1 H3 110.1(9) ?
H1 N1 H3 111.2(13) ?
H2 N1 H3 112.8(13) ?
C6 N2 C7 119.01(6) ?
C6 N2 H4 120.4(9) ?
C7 N2 H4 119.0(9) ?
N1 C1 C6 107.74(6) ?
N1 C1 C2 110.25(6) ?
C6 C1 C2 109.58(6) ?
N1 C1 H11 109.75(4) ?
C6 C1 H11 109.75(4) ?
C2 C1 H11 109.75(4) ?
C3 C2 C1 115.03(6) ?
C3 C2 H21 108.51(5) ?
C1 C2 H21 108.51(4) ?
C3 C2 H22 108.51(4) ?
C1 C2 H22 108.51(4) ?
H21 C2 H22 107.5 ?
C4 C3 C5 110.47(8) ?
C4 C3 C2 111.67(8) ?
C5 C3 C2 109.56(7) ?
C4 C3 H31 108.35(6) ?
C5 C3 H31 108.35(5) ?
C2 C3 H31 108.35(4) ?
C3 C4 H41 109.47(6) ?
C3 C4 H42 109.47(6) ?
H41 C4 H42 109.5 ?
C3 C4 H43 109.47(5) ?
H41 C4 H43 109.5 ?
H42 C4 H43 109.5 ?
C3 C5 H51 109.47(5) ?
C3 C5 H52 109.47(5) ?
H51 C5 H52 109.5 ?
C3 C5 H53 109.47(5) ?
H51 C5 H53 109.5 ?
H52 C5 H53 109.5 ?
O1 C6 N2 121.94(7) ?
O1 C6 C1 120.93(6) ?
N2 C6 C1 117.10(6) ?
N2 C7 C8 109.52(6) ?
N2 C7 C9 111.93(6) ?
C8 C7 C9 108.85(6) ?
N2 C7 H71 108.83(4) ?
C8 C7 H71 108.83(5) ?
C9 C7 H71 108.83(4) ?
C7 C8 H81 109.47(4) ?
C7 C8 H82 109.47(4) ?
H81 C8 H82 109.5 ?
C7 C8 H83 109.47(5) ?
H81 C8 H83 109.5 ?
H82 C8 H83 109.5 ?
O2 C9 O3 125.21(7) ?
O2 C9 C7 117.05(6) ?
O3 C9 C7 117.62(6) ?
H401 O40 H402 105(2) yes
H501 O50 H502 110(2) yes
H601 O60 H602 106(2) yes
H701 O70 H702 104(2) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
O1 C6 1.2397(9)
O2 C9 1.2570(8)
O3 C9 1.2607(9)
O40 H401 0.85(2)
O40 H402 0.88(2)
O50 H501 0.82(2)
O50 H502 0.81(2)
O60 H601 0.82(2)
O60 H602 0.84(3)
O70 H701 0.80(2)
O70 H702 0.85(2)
N1 C1 1.5001(10)
N1 H1 0.836(15)
N1 H2 0.887(14)
N1 H3 0.912(14)
N2 C6 1.3341(9)
N2 C7 1.4642(9)
N2 H4 0.88(2)
C1 C6 1.5264(10)
C1 C2 1.5377(11)
C1 H11 0.940(13)
C2 C3 1.5359(12)
C2 H21 0.968(10)
C2 H22 0.968(9)
C3 C4 1.525(2)
C3 C5 1.5285(13)
C3 H31 0.968(15)
C4 H41 1.004(11)
C4 H42 1.004(11)
C4 H43 1.004(11)
C5 H51 0.990(9)
C5 H52 0.990(9)
C5 H53 0.990(9)
C7 C8 1.5282(11)
C7 C9 1.5414(10)
C7 H71 0.982(12)
C8 H81 0.969(9)
C8 H82 0.969(9)
C8 H83 0.969(9)
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
_geom_torsion_publ_flag
N1 C1 C2 C3 -66.58(8) yes
C6 C1 C2 C3 175.01(7) ?
C1 C2 C3 C4 -72.16(10) yes
C1 C2 C3 C5 165.12(7) yes
C7 N2 C6 O1 3.91(11) ?
C1 C6 N2 C7 -177.94(6) yes
N1 C1 C6 O1 -45.71(10) ?
C2 C1 C6 O1 74.25(9) ?
N1 C1 C6 N2 136.12(7) yes
C2 C1 C6 N2 -103.92(8) ?
C6 N2 C7 C8 172.32(7) ?
C6 N2 C7 C9 -66.88(8) yes
N2 C7 C9 O2 147.74(6) yes
C8 C7 C9 O2 -91.07(8) ?
N2 C7 C9 O3 -35.98(9) yes
C8 C7 C9 O3 85.21(8) ?