#------------------------------------------------------------------------------
#$Date: 2008-04-03 13:11:48 +0300 (Thu, 03 Apr 2008) $
#$Revision: 326 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/2206486.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_2206486
loop_
_publ_author_name
'Smith, Joanne H.'
'Dann, Sandra E.'
'Elsegood, Mark R. J.'
'Dale, Sophie H.'
'Blatchford, Chris. G'
_publ_section_title
;
\a-Lactose monohydrate: a redetermination at 150 K
;
_journal_coeditor_code           LH6465
_journal_issue                   8
_journal_name_full               'Acta Crystallographica, Section E'
_journal_page_first              o2499
_journal_page_last               o2501
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C12 H22 O11, H2 O'
_chemical_formula_moiety         'C12 H22 O11, H2 O'
_chemical_formula_sum            'C12 H24 O12'
_chemical_formula_weight         360.31
_chemical_melting_point          220
_chemical_name_common            '\a-lactose monohydrate'
_chemical_name_systematic
;
\a-4-O-(\b-D-galactopyranosido)-D-glucopyranose
;
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 21'
_atom_sites_solution_hydrogens   'Geom except H12A&B coords freely refined'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.911(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   4.7830(5)
_cell_length_b                   21.540(2)
_cell_length_c                   7.7599(8)
_cell_measurement_reflns_used    3523
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.17
_cell_measurement_theta_min      2.73
_cell_volume                     768.85(14)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2000)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6697
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.91
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.141
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         1864
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0332
_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/[\s^2^(Fo^2^)+(0.0394P)^2^+0.1957P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0788
_reflns_number_gt                1692
_reflns_number_total             1864
_reflns_threshold_expression     I>2\s(I)
_[local]_cod_data_source_file    lh6465.cif
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
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 0.0000 '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'
O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_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_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
O1 -0.0485(4) -0.06111(7) 0.7307(2) 0.0172(3) Uani d . 1 O
C1' 0.1611(5) -0.01414(11) 0.7705(3) 0.0168(5) Uani d . 1 C
H1' 0.3530 -0.0304 0.7625 0.020 Uiso calc R 1 H
C2' 0.0574(5) 0.03808(11) 0.6356(3) 0.0182(5) Uani d . 1 C
H2' -0.1467 0.0494 0.6322 0.022 Uiso calc R 1 H
O2 0.0640(4) 0.01591(9) 0.4648(2) 0.0222(4) Uani d . 1 O
H2A -0.1065 0.0093 0.4019 0.033 Uiso calc R 1 H
C3' 0.2515(5) 0.09504(11) 0.6874(3) 0.0189(5) Uani d . 1 C
H3' 0.4489 0.0855 0.6738 0.023 Uiso calc R 1 H
O3 0.1249(4) 0.14411(8) 0.5683(2) 0.0242(4) Uani d . 1 O
H3A 0.2572 0.1660 0.5474 0.036 Uiso calc R 1 H
C4' 0.2784(5) 0.11279(11) 0.8832(3) 0.0189(5) Uani d . 1 C
H4' 0.4201 0.1477 0.9200 0.023 Uiso calc R 1 H
O4 0.0032(4) 0.13101(8) 0.9035(3) 0.0228(4) Uani d . 1 O
H4A -0.0208 0.1692 0.8833 0.034 Uiso calc R 1 H
C5' 0.3853(5) 0.05660(12) 1.0023(3) 0.0179(5) Uani d . 1 C
H5' 0.5796 0.0435 0.9901 0.022 Uiso calc R 1 H
C6' 0.4085(6) 0.06982(12) 1.1971(3) 0.0223(5) Uani d . 1 C
H6'A 0.5526 0.1032 1.2414 0.027 Uiso calc R 1 H
H6'B 0.2181 0.0841 1.2094 0.027 Uiso calc R 1 H
O6 0.4960(4) 0.01480(9) 1.3010(2) 0.0237(4) Uani d . 1 O
H6 0.3859 0.0089 1.3672 0.036 Uiso calc R 1 H
O5 0.1815(4) 0.00615(8) 0.9485(2) 0.0180(3) Uani d . 1 O
C1 -0.0864(5) -0.25161(12) 0.8074(3) 0.0207(5) Uani d . 1 C
H1 -0.0221 -0.2960 0.8191 0.025 Uiso calc R 1 H
O7 -0.3771(4) -0.24879(10) 0.8105(2) 0.0277(4) Uani d . 1 O
H7A -0.4841 -0.2626 0.7136 0.042 Uiso calc R 1 H
C2 0.0961(5) -0.21524(11) 0.9691(3) 0.0178(5) Uani d . 1 C
H2 0.3048 -0.2211 0.9721 0.021 Uiso calc R 1 H
O8 0.0602(4) -0.23976(8) 1.1327(2) 0.0209(4) Uani d . 1 O
H8A -0.0856 -0.2234 1.1546 0.031 Uiso calc R 1 H
C3 0.0325(5) -0.14595(11) 0.9477(3) 0.0175(5) Uani d . 1 C
H3 -0.1683 -0.1379 0.9577 0.021 Uiso calc R 1 H
O9 0.2382(4) -0.11500(8) 1.0912(2) 0.0235(4) Uani d . 1 O
H9A 0.2228 -0.0764 1.0755 0.035 Uiso calc R 1 H
C4 0.0540(5) -0.12383(11) 0.7645(3) 0.0168(5) Uani d . 1 C
H4 0.2609 -0.1262 0.7605 0.020 Uiso calc R 1 H
C5 -0.1351(5) -0.16374(11) 0.6149(3) 0.0174(5) Uani d . 1 C
H5 -0.3432 -0.1599 0.6155 0.021 Uiso calc R 1 H
C6 -0.1058(6) -0.14661(12) 0.4311(3) 0.0225(5) Uani d . 1 C
H6A -0.1494 -0.1019 0.4084 0.027 Uiso calc R 1 H
H6B 0.0965 -0.1540 0.4269 0.027 Uiso calc R 1 H
O11 -0.3010(4) -0.18277(9) 0.2957(2) 0.0262(4) Uani d . 1 O
H11A -0.4400 -0.1604 0.2395 0.039 Uiso calc R 1 H
O10 -0.0445(4) -0.22706(8) 0.6468(2) 0.0186(4) Uani d . 1 O
O12 0.6064(4) 0.20401(9) 0.5314(2) 0.0234(4) Uani d D 1 O
H12A 0.619(7) 0.2294(13) 0.616(3) 0.035 Uiso d D 1 H
H12B 0.764(5) 0.1835(14) 0.548(4) 0.035 Uiso d D 1 H
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 0.0176(8) 0.0132(8) 0.0192(8) 0.0004(6) 0.0023(7) 0.0010(7)
C1' 0.0166(10) 0.0174(11) 0.0170(11) 0.0003(9) 0.0056(9) 0.0010(9)
C2' 0.0184(11) 0.0182(11) 0.0183(12) 0.0015(9) 0.0054(9) 0.0003(9)
O2 0.0227(9) 0.0293(10) 0.0142(8) 0.0004(8) 0.0041(7) 0.0012(7)
C3' 0.0172(11) 0.0193(12) 0.0207(12) 0.0015(9) 0.0063(9) 0.0051(10)
O3 0.0229(9) 0.0221(9) 0.0277(10) 0.0003(7) 0.0069(8) 0.0117(8)
C4' 0.0193(12) 0.0163(12) 0.0211(12) 0.0003(9) 0.0056(9) 0.0007(9)
O4 0.0245(9) 0.0171(9) 0.0289(9) 0.0046(7) 0.0107(8) 0.0028(7)
C5' 0.0161(11) 0.0179(11) 0.0184(11) -0.0015(9) 0.0023(9) -0.0008(9)
C6' 0.0260(12) 0.0208(12) 0.0189(12) -0.0012(10) 0.0040(10) -0.0006(10)
O6 0.0228(9) 0.0310(10) 0.0167(8) 0.0002(8) 0.0044(7) 0.0035(8)
O5 0.0220(8) 0.0166(8) 0.0144(8) -0.0029(7) 0.0032(6) -0.0001(7)
C1 0.0247(12) 0.0176(11) 0.0210(12) -0.0016(10) 0.0081(10) -0.0024(10)
O7 0.0239(9) 0.0367(11) 0.0227(9) -0.0081(8) 0.0065(7) -0.0055(9)
C2 0.0208(11) 0.0144(11) 0.0174(11) -0.0002(9) 0.0039(9) 0.0004(9)
O8 0.0260(9) 0.0173(9) 0.0200(9) 0.0021(7) 0.0070(7) 0.0022(7)
C3 0.0201(11) 0.0157(11) 0.0145(11) 0.0006(8) 0.0012(9) -0.0019(9)
O9 0.0338(10) 0.0141(8) 0.0161(8) -0.0016(7) -0.0041(7) -0.0013(7)
C4 0.0175(11) 0.0156(11) 0.0159(11) 0.0016(9) 0.0022(9) -0.0009(9)
C5 0.0174(11) 0.0181(11) 0.0155(11) 0.0012(9) 0.0025(9) -0.0022(9)
C6 0.0290(13) 0.0220(13) 0.0151(12) -0.0029(10) 0.0037(10) -0.0021(10)
O11 0.0297(10) 0.0268(10) 0.0176(9) 0.0045(8) -0.0013(7) -0.0038(8)
O10 0.0217(8) 0.0167(8) 0.0176(8) 0.0004(6) 0.0055(7) -0.0032(6)
O12 0.0228(9) 0.0235(9) 0.0225(9) 0.0004(7) 0.0039(8) 0.0044(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C1' 1.398(3) Y
O1 C4 1.437(3) Y
C1' O5 1.427(3) ?
C1' C2' 1.524(3) ?
C1' H1' 1.0000 ?
C2' O2 1.417(3) ?
C2' C3' 1.524(3) ?
C2' H2' 1.0000 ?
O2 H2A 0.8400 ?
C3' O3 1.425(3) ?
C3' C4' 1.538(3) ?
C3' H3' 1.0000 ?
O3 H3A 0.8400 ?
C4' O4 1.423(3) ?
C4' C5' 1.524(3) ?
C4' H4' 1.0000 ?
O4 H4A 0.8400 ?
C5' O5 1.443(3) ?
C5' C6' 1.512(3) ?
C5' H5' 1.0000 ?
C6' O6 1.430(3) ?
C6' H6'A 0.9900 ?
C6' H6'B 0.9900 ?
O6 H6 0.8400 ?
C1 O7 1.399(3) Y
C1 O10 1.418(3) ?
C1 C2 1.533(3) ?
C1 H1 1.0000 ?
O7 H7A 0.8400 ?
C2 O8 1.428(3) ?
C2 C3 1.523(3) ?
C2 H2 1.0000 ?
O8 H8A 0.8400 ?
C3 O9 1.432(3) ?
C3 C4 1.529(3) ?
C3 H3 1.0000 ?
O9 H9A 0.8400 ?
C4 C5 1.526(3) ?
C4 H4 1.0000 ?
C5 O10 1.432(3) ?
C5 C6 1.516(3) ?
C5 H5 1.0000 ?
C6 O11 1.430(3) ?
C6 H6A 0.9900 ?
C6 H6B 0.9900 ?
O11 H11A 0.8400 ?
O12 H12A 0.842(14) ?
O12 H12B 0.851(14) ?
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' O1 C4 116.88(17) Y
O1 C1' O5 106.85(17) ?
O1 C1' C2' 107.69(18) ?
O5 C1' C2' 111.22(19) ?
O1 C1' H1' 110.3 ?
O5 C1' H1' 110.3 ?
C2' C1' H1' 110.3 ?
O2 C2' C1' 107.89(19) ?
O2 C2' C3' 110.5(2) ?
C1' C2' C3' 110.67(19) ?
O2 C2' H2' 109.3 ?
C1' C2' H2' 109.3 ?
C3' C2' H2' 109.3 ?
C2' O2 H2A 109.5 ?
O3 C3' C2' 107.83(19) ?
O3 C3' C4' 111.2(2) ?
C2' C3' C4' 109.9(2) ?
O3 C3' H3' 109.3 ?
C2' C3' H3' 109.3 ?
C4' C3' H3' 109.3 ?
C3' O3 H3A 109.5 ?
O4 C4' C5' 108.6(2) ?
O4 C4' C3' 110.4(2) ?
C5' C4' C3' 108.96(19) ?
O4 C4' H4' 109.6 ?
C5' C4' H4' 109.6 ?
C3' C4' H4' 109.6 ?
C4' O4 H4A 109.5 ?
O5 C5' C6' 106.82(19) ?
O5 C5' C4' 109.58(18) ?
C6' C5' C4' 112.2(2) ?
O5 C5' H5' 109.4 ?
C6' C5' H5' 109.4 ?
C4' C5' H5' 109.4 ?
O6 C6' C5' 109.7(2) ?
O6 C6' H6'A 109.7 ?
C5' C6' H6'A 109.7 ?
O6 C6' H6'B 109.7 ?
C5' C6' H6'B 109.7 ?
H6'A C6' H6'B 108.2 ?
C6' O6 H6 109.5 ?
C1' O5 C5' 111.85(17) ?
O7 C1 O10 112.3(2) ?
O7 C1 C2 108.01(19) ?
O10 C1 C2 110.05(19) ?
O7 C1 H1 108.8 ?
O10 C1 H1 108.8 ?
C2 C1 H1 108.8 ?
C1 O7 H7A 109.5 ?
O8 C2 C3 113.0(2) ?
O8 C2 C1 111.00(19) ?
C3 C2 C1 111.1(2) ?
O8 C2 H2 107.1 ?
C3 C2 H2 107.1 ?
C1 C2 H2 107.1 ?
C2 O8 H8A 109.5 ?
O9 C3 C2 107.30(19) ?
O9 C3 C4 111.76(19) ?
C2 C3 C4 110.1(2) ?
O9 C3 H3 109.2 ?
C2 C3 H3 109.2 ?
C4 C3 H3 109.2 ?
C3 O9 H9A 109.5 ?
O1 C4 C5 106.83(18) ?
O1 C4 C3 110.87(19) ?
C5 C4 C3 110.79(19) ?
O1 C4 H4 109.4 ?
C5 C4 H4 109.4 ?
C3 C4 H4 109.4 ?
O10 C5 C6 107.02(19) ?
O10 C5 C4 108.48(18) ?
C6 C5 C4 113.0(2) ?
O10 C5 H5 109.4 ?
C6 C5 H5 109.4 ?
C4 C5 H5 109.4 ?
O11 C6 C5 110.4(2) ?
O11 C6 H6A 109.6 ?
C5 C6 H6A 109.6 ?
O11 C6 H6B 109.6 ?
C5 C6 H6B 109.6 ?
H6A C6 H6B 108.1 ?
C6 O11 H11A 109.5 ?
C1 O10 C5 113.47(18) ?
H12A O12 H12B 110(2) ?
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
C4 O1 C1' O5 -93.4(2)
C4 O1 C1' C2' 147.00(19)
O1 C1' C2' O2 -67.6(2)
O5 C1' C2' O2 175.61(17)
O1 C1' C2' C3' 171.40(18)
O5 C1' C2' C3' 54.6(3)
O2 C2' C3' O3 67.0(2)
C1' C2' C3' O3 -173.61(19)
O2 C2' C3' C4' -171.67(19)
C1' C2' C3' C4' -52.2(3)
O3 C3' C4' O4 55.1(3)
C2' C3' C4' O4 -64.3(2)
O3 C3' C4' C5' 174.24(19)
C2' C3' C4' C5' 54.9(2)
O4 C4' C5' O5 60.5(2)
C3' C4' C5' O5 -59.8(2)
O4 C4' C5' C6' -57.9(3)
C3' C4' C5' C6' -178.2(2)
O5 C5' C6' O6 57.2(2)
C4' C5' C6' O6 177.2(2)
O1 C1' O5 C5' -177.84(17)
C2' C1' O5 C5' -60.6(2)
C6' C5' O5 C1' -174.86(18)
C4' C5' O5 C1' 63.4(2)
O7 C1 C2 O8 57.8(3)
O10 C1 C2 O8 -179.21(18)
O7 C1 C2 C3 -68.7(3)
O10 C1 C2 C3 54.2(3)
O8 C2 C3 O9 62.2(3)
C1 C2 C3 O9 -172.33(19)
O8 C2 C3 C4 -175.98(19)
C1 C2 C3 C4 -50.5(2)
C1' O1 C4 C5 -143.26(19)
C1' O1 C4 C3 95.9(2)
O9 C3 C4 O1 -69.7(2)
C2 C3 C4 O1 171.10(19)
O9 C3 C4 C5 171.83(19)
C2 C3 C4 C5 52.7(2)
O1 C4 C5 O10 -178.42(18)
C3 C4 C5 O10 -57.6(2)
O1 C4 C5 C6 63.1(2)
C3 C4 C5 C6 -176.0(2)
O10 C5 C6 O11 64.3(2)
C4 C5 C6 O11 -176.3(2)
O7 C1 O10 C5 58.4(3)
C2 C1 O10 C5 -62.0(2)
C6 C5 O10 C1 -174.31(18)
C4 C5 O10 C1 63.5(2)
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
O2 H2A O6 1_454 0.84 1.85 2.665(2) 163
O3 H3A O12 . 0.84 1.89 2.722(3) 168
O4 H4A O8 2_557 0.84 1.97 2.806(3) 173
O6 H6 O2 1_556 0.84 1.90 2.707(2) 161
O7 H7A O12 2_546 0.84 1.97 2.772(2) 161
O8 H8A O11 1_556 0.84 1.91 2.700(3) 157
O9 H9A O5 . 0.84 2.02 2.819(2) 159
O11 H11A O9 1_454 0.84 1.92 2.755(2) 174
O12 H12B O3 1_655 0.851(14) 1.893(15) 2.740(3) 174(4)
O12 H12A O8 2_657 0.842(14) 2.23(2) 2.920(2) 140(3)