#------------------------------------------------------------------------------
#$Date: 2017-10-13 09:09:21 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/20/64/2206486.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
;
 α-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_paper_doi               10.1107/S1600536805021367
_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            'α-lactose monohydrate'
_chemical_name_systematic
;
α-4-O-(β-D-galactopyranosido)-D-glucopyranose
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                     768.84(13)
_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       'ω 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/[σ²(Fo²)+(0.0394P)²+0.1957P] where P = (Fo²+2Fc²)/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>2σ(I)
_cod_data_source_file            lh6465.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (3
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' 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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (3
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' 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_original_cell_volume        768.85(14)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2206486
_cod_database_fobs_code          2206486
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
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_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_
_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_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_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)
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_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 94699
