##############################################################################
# #
# This CIF contains the data in a paper accepted for publication in #
# Acta Crystallographica Section E. It conforms to the requirements of #
# Notes for Authors for Acta Crystallographica Section E, and has been #
# peer reviewed under the auspices of the IUCr Commission on Journals. #
# #
# Full details of the Crystallographic Information File format #
# are given in the paper "The Crystallographic Information File (CIF): #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H. #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. #
# #
# The current version of the core CIF dictionary is obtainable from #
# ftp://ftp.iucr.org/pub/cif_core.dic. #
# #
# Software is freely available for graphical display of the structure(s) #
# in this CIF. For information consult the CIF software page #
# http://www.iucr.org/resources/cif/software. #
# #
# This file may be used for bona fide research purposes within the #
# scientific community so long as proper attribution is given to the journal #
# article from which it was obtained. #
# #
##############################################################################
data_global
_audit_creation_method 'by CrystalStructure 4.1'
_journal_date_recd_electronic 2015-03-19
_journal_date_accepted 2015-04-02
_journal_name_full 'Acta Crystallographica, Section E'
_journal_year 2015
_journal_volume 71
_journal_issue 5
_journal_page_first o289
_journal_page_last o290
_journal_paper_category HO
_journal_paper_doi 10.1107/S2056989015006623
_journal_coeditor_code IS5394
_publ_contact_author_name 'Tomohiko Ishii'
_publ_contact_author_address
;
Department of Advanced Materials Science
Faculty of Engineering
Kagawa University
2217-20, Hayashicho, Takamatsu
Kagawa 761-0396
Japan
;
_publ_contact_author_email tishii@eng.kagawa-u.ac.jp
_publ_contact_author_fax '+81-87-864-2414'
_publ_contact_author_phone '+81-87-864-2414'
_publ_section_title
;
Crystal structure of \b-D,L-psicose
;
loop_
_publ_author_name
_publ_author_address
'Ishii, Tomohiko'
;
Department of Advanced Materials Science
Faculty of Engineering
Kagawa University
2217-20 Hayashi-cho, Takamatsu
Kagawa 761-0396
Japan
;
'Sakane, Genta'
;
Department of Chemistry
Faculty of Science
Okayama University of Science
1-1 Ridaicho, Kita-ku
Okayama 700-0005
Japan
;
'Yoshihara, Akihide'
;
Rare Sugar Research Center
Faculty of Agriculture
Kagawa University
2393 Ikenobe
Kagawa 761-0795
Japan
;
'Fukada, Kazuhiro'
;
Department of Applied Biological Science
Faculty of Agriculture
Kagawa University
2393 Ikenobe
Kagawa 761-0795
Japan
;
'Senoo, Tatsuya'
;
Department of Advanced Materials Science
Faculty of Engineering
Kagawa University
2217-20 Hayashi-cho, Takamatsu
Kagawa 761-0396
Japan
;
data_I
_database_code_depnum_ccdc_archive 'CCDC 1057484'
_chemical_formula_moiety 'C6 H12 O6'
_chemical_formula_sum 'C6 H12 O6'
_chemical_formula_iupac 'C6 H12 O6'
_chemical_formula_weight 180.16
_chemical_melting_point ?
_space_group_crystal_system orthorhombic
_space_group_name_H-M_alt 'P n a 21'
_space_group_name_Hall 'P 2c -2n'
loop_
_symmetry_equiv_pos_site_id
_space_group_symop_operation_xyz
1 '+X,+Y,+Z'
2 '1/2-X,1/2+Y,1/2+Z'
3 '1/2+X,1/2-Y,+Z'
4 '-X,-Y,1/2+Z'
_cell_length_a 11.2629(5)
_cell_length_b 5.3552(3)
_cell_length_c 12.6538(6)
_cell_angle_alpha 90.0000
_cell_angle_beta 90.0000
_cell_angle_gamma 90.0000
_cell_volume 763.21(6)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 5584
_cell_measurement_theta_min 3.50
_cell_measurement_theta_max 68.47
_cell_measurement_temperature 296
_exptl_crystal_description block
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.100
_exptl_crystal_size_mid 0.100
_exptl_crystal_size_min 0.100
_exptl_crystal_density_diffrn 1.568
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 384.00
_exptl_absorpt_coefficient_mu 1.248
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1995)
;
_exptl_absorpt_correction_T_min 0.442
_exptl_absorpt_correction_T_max 0.883
_diffrn_ambient_temperature 296
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54187
_diffrn_measurement_device_type 'Rigaku R-AXIS RAPID'
_diffrn_measurement_method \w
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number 12119
_diffrn_reflns_av_R_equivalents 0.1387
_diffrn_reflns_theta_min 6.999
_diffrn_reflns_theta_max 68.179
_diffrn_reflns_theta_full 67.687
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_limit_l_max 15
_diffrn_standards_number 0
_diffrn_standards_interval_count .
_diffrn_standards_decay_% ?
_refine_special_details
;
Refinement was performed using all reflections. The weighted R-factor
(wR) and goodness of fit (S) are based on F^2^.
R-factor (gt) are based on F. The threshold expression of
F^2^ > 2.0 \s(F^2^) is used only for calculating R-factor
(gt).
;
_reflns_number_total 1400
_reflns_number_gt 1295
_reflns_threshold_expression F^2^>2\s(F^2^)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all 0.0511
_refine_ls_R_factor_gt 0.0475
_refine_ls_wR_factor_gt 0.1007
_refine_ls_wR_factor_ref 0.1017
_refine_ls_goodness_of_fit_ref 1.040
_refine_ls_number_reflns 1400
_refine_ls_number_parameters 116
_refine_ls_number_restraints 1
_refine_ls_hydrogen_treatment constr
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0359P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_refine_ls_shift/su_max 0.000
_refine_diff_density_max 0.25
_refine_diff_density_min -0.23
_refine_ls_extinction_method SHELXL
_refine_ls_extinction_coef 0.039(3)
_refine_ls_abs_structure_details
;
Flack (1983), 666 Friedel pairs
;
_refine_ls_abs_structure_Flack 0.1(4)
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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
'H' 'H' 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
'O' 'O' 0.0492 0.0322
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
_computing_data_collection
;
RAPID-AUTO (Rigaku, 2009)
;
_computing_cell_refinement
;
RAPID-AUTO (Rigaku, 2009)
;
_computing_data_reduction
;
RAPID-AUTO (Rigaku, 2009)
;
_computing_structure_solution
;
SIR2011 (Burla et al., 2012)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_molecular_graphics
;
CrystalStructure (Rigaku, 2014)
;
_computing_publication_material
;
CrystalStructure (Rigaku, 2014)
;
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_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O O1 0.6428(2) 1.0475(5) 0.0101(2) 0.0321(7) Uani d . 1 . .
O O2 0.8138(2) 1.3225(4) 0.1244(2) 0.0283(6) Uani d . 1 . .
O O3 0.9712(2) 0.7407(4) 0.0986(2) 0.0278(6) Uani d . 1 . .
O O4 1.12635(19) 0.9941(5) 0.2360(2) 0.0306(7) Uani d . 1 . .
O O5 0.9520(3) 0.6941(5) 0.3201(2) 0.0368(7) Uani d . 1 . .
O O6 0.75926(19) 0.9487(5) 0.2068(2) 0.0243(6) Uani d . 1 . .
C C1 0.7610(3) 0.9600(8) 0.0218(3) 0.0275(8) Uani d . 1 . .
C C2 0.8199(3) 1.0614(6) 0.1199(3) 0.0211(7) Uani d . 1 . .
C C3 0.9525(3) 0.9956(6) 0.1238(3) 0.0223(7) Uani d . 1 . .
C C4 1.0049(3) 1.0665(7) 0.2306(2) 0.0233(8) Uani d . 1 . .
C C5 0.9337(3) 0.9564(7) 0.3210(3) 0.0266(8) Uani d . 1 . .
C C6 0.8044(3) 1.0258(7) 0.3083(3) 0.0289(8) Uani d . 1 . .
H H1B 0.80695 1.00892 -0.03968 0.0330 Uiso calc R 1 . .
H H1C 0.76042 0.77904 0.02497 0.0330 Uiso calc R 1 . .
H H1A 0.59772 0.95756 0.04384 0.0386 Uiso calc R 1 . .
H H2A 0.75043 1.36467 0.15074 0.0340 Uiso calc R 1 . .
H H3A 0.92832 0.65324 0.13561 0.0333 Uiso calc R 1 . .
H H3B 0.99273 1.0959 0.06985 0.0268 Uiso calc R 1 . .
H H4B 1.00147 1.24872 0.23691 0.0280 Uiso calc R 1 . .
H H4A 1.1313 0.84167 0.23198 0.0367 Uiso calc R 1 . .
H H5A 0.92192 0.63218 0.37294 0.0442 Uiso calc R 1 . .
H H5B 0.96322 1.0246 0.38792 0.0319 Uiso calc R 1 . .
H H6A 0.75828 0.94707 0.36378 0.0347 Uiso calc R 1 . .
H H6B 0.79566 1.20525 0.31544 0.0347 Uiso calc R 1 . .
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 0.0232(14) 0.0431(18) 0.0301(13) -0.0019(11) -0.0058(11) 0.0126(12)
O2 0.0238(12) 0.0228(13) 0.0384(14) 0.0010(9) 0.0057(11) 0.0025(13)
O3 0.0252(12) 0.0240(13) 0.0340(14) 0.0013(10) 0.0068(10) -0.0020(11)
O4 0.0193(12) 0.0265(14) 0.0459(17) 0.0004(10) -0.0022(10) 0.0013(12)
O5 0.0475(17) 0.0309(15) 0.0322(15) 0.0064(12) 0.0101(11) 0.0101(12)
O6 0.0230(12) 0.0297(14) 0.0203(11) -0.0057(10) 0.0027(10) 0.0002(12)
C1 0.025(2) 0.032(2) 0.0254(19) -0.0001(15) -0.0001(14) 0.0024(18)
C2 0.0211(17) 0.0228(17) 0.0195(16) 0.0012(12) 0.0034(14) 0.0043(16)
C3 0.0197(19) 0.0233(17) 0.0239(17) 0.0009(12) 0.0038(14) 0.0042(14)
C4 0.0189(17) 0.025(2) 0.0265(19) 0.0009(13) 0.0000(13) 0.0006(15)
C5 0.030(2) 0.030(2) 0.0201(17) 0.0027(14) -0.0011(15) -0.0001(15)
C6 0.0272(18) 0.039(2) 0.0209(17) 0.0006(15) 0.0055(15) -0.0002(15)
_geom_special_details
;
ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C1 . . 1.419(4) no
O2 C2 . . 1.401(4) no
O3 C3 . . 1.418(4) no
O4 C4 . . 1.423(4) no
O5 C5 . . 1.419(4) no
O6 C2 . . 1.428(4) no
O6 C6 . . 1.442(4) no
C1 C2 . . 1.509(5) no
C2 C3 . . 1.535(5) no
C3 C4 . . 1.523(5) no
C4 C5 . . 1.516(5) no
C5 C6 . . 1.512(5) no
O1 H1A . . 0.820 no
O2 H2A . . 0.820 no
O3 H3A . . 0.820 no
O4 H4A . . 0.820 no
O5 H5A . . 0.820 no
C1 H1B . . 0.970 no
C1 H1C . . 0.970 no
C3 H3B . . 0.980 no
C4 H4B . . 0.980 no
C5 H5B . . 0.980 no
C6 H6A . . 0.970 no
C6 H6B . . 0.970 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 O6 C6 . . . 113.3(2) no
O1 C1 C2 . . . 112.3(3) no
O2 C2 O6 . . . 111.6(3) no
O2 C2 C1 . . . 111.8(3) no
O2 C2 C3 . . . 106.0(3) no
O6 C2 C1 . . . 105.7(3) no
O6 C2 C3 . . . 110.1(3) no
C1 C2 C3 . . . 111.8(3) no
O3 C3 C2 . . . 111.0(3) no
O3 C3 C4 . . . 112.5(3) no
C2 C3 C4 . . . 110.4(3) no
O4 C4 C3 . . . 110.3(3) no
O4 C4 C5 . . . 111.5(3) no
C3 C4 C5 . . . 111.6(3) no
O5 C5 C4 . . . 107.5(3) no
O5 C5 C6 . . . 112.5(3) no
C4 C5 C6 . . . 109.5(3) no
O6 C6 C5 . . . 111.4(3) no
C1 O1 H1A . . . 109.471 no
C2 O2 H2A . . . 109.471 no
C3 O3 H3A . . . 109.470 no
C4 O4 H4A . . . 109.469 no
C5 O5 H5A . . . 109.469 no
O1 C1 H1B . . . 109.152 no
O1 C1 H1C . . . 109.152 no
C2 C1 H1B . . . 109.145 no
C2 C1 H1C . . . 109.145 no
H1B C1 H1C . . . 107.867 no
O3 C3 H3B . . . 107.581 no
C2 C3 H3B . . . 107.578 no
C4 C3 H3B . . . 107.580 no
O4 C4 H4B . . . 107.757 no
C3 C4 H4B . . . 107.761 no
C5 C4 H4B . . . 107.767 no
O5 C5 H5B . . . 109.099 no
C4 C5 H5B . . . 109.103 no
C6 C5 H5B . . . 109.093 no
O6 C6 H6A . . . 109.357 no
O6 C6 H6B . . . 109.357 no
C5 C6 H6A . . . 109.358 no
C5 C6 H6B . . . 109.358 no
H6A C6 H6B . . . 107.992 no
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C2 O6 C6 C5 . . . . -60.7(3) no
C6 O6 C2 O2 . . . . -58.2(3) no
C6 O6 C2 C1 . . . . -179.9(2) no
C6 O6 C2 C3 . . . . 59.2(3) no
O1 C1 C2 O2 . . . . -53.5(4) no
O1 C1 C2 O6 . . . . 68.1(3) no
O1 C1 C2 C3 . . . . -172.1(2) no
O2 C2 C3 O3 . . . . -168.2(2) no
O2 C2 C3 C4 . . . . 66.4(3) no
O6 C2 C3 O3 . . . . 71.0(3) no
O6 C2 C3 C4 . . . . -54.4(3) no
C1 C2 C3 O3 . . . . -46.2(4) no
C1 C2 C3 C4 . . . . -171.7(2) no
O3 C3 C4 O4 . . . . 52.5(3) no
O3 C3 C4 C5 . . . . -72.0(3) no
C2 C3 C4 O4 . . . . 177.1(2) no
C2 C3 C4 C5 . . . . 52.6(3) no
O4 C4 C5 O5 . . . . -54.2(3) no
O4 C4 C5 C6 . . . . -176.7(2) no
C3 C4 C5 O5 . . . . 69.6(3) no
C3 C4 C5 C6 . . . . -52.9(3) no
O5 C5 C6 O6 . . . . -63.8(4) no
C4 C5 C6 O6 . . . . 55.7(4) no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_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
O1 H1A O3 . . 3_465 0.82 1.91 2.715(3) 168 yes
O2 H2A O4 . . 3_475 0.82 1.92 2.724(3) 166 yes
O3 H3A O2 . . 1_545 0.82 2.20 2.874(3) 140 yes
O3 H3A O5 . . . 0.82 2.36 2.822(4) 117 yes
O4 H4A O6 . . 3_565 0.82 2.14 2.829(3) 141 yes
O5 H5A O1 . . 2_645 0.82 1.94 2.746(4) 169 yes
_shelx_hkl_file
;
0 0 1 63.39 11.01
0 0 1 92.94 12.27
0 0 1 49.49 8.61
0 0 1 79.21 9.60
0 0 1 60.34 9.98
0 0 1 70.06 10.46
0 0 -1 60.77 9.77
0 0 -1 66.73 12.10
0 0 -1 89.24 13.10
0 0 -1 62.75 9.66
0 0 -1 69.77 9.75
0 0 -1 60.70 8.25
0 0 -1 72.46 12.14
0 0 -1 139.04 16.06
0 0 -1 56.13 9.73
0 0 241323.6710753.21
0 0 234949.63 9118.31
0 0 236954.62 9630.51
0 0 227989.67 7306.82
0 0 246847.1212219.20
0 0 232437.20 8441.23
0 0 222472.06 5837.82
0 0 223077.93 6025.56
0 0 -221660.74 5660.15
0 0 -236614.92 9525.89
0 0 -234897.28 9094.52
0 0 -244148.7011501.12
0 0 -216898.24 4417.96
0 0 -235472.28 9250.68
0 0 -224856.03 6466.76
0 0 -220463.45 5356.13
0 0 3 7.12 8.31
0 0 3 24.73 7.51
0 0 3 3.48 13.97
0 0 3 5.89 11.57
0 0 3 8.49 15.53
0 0 3 7.92 12.64
0 0 3 6.73 12.92
0 0 3 6.20 8.79
0 0 -3 -0.01 11.39
0 0 -3 8.54 9.42
0 0 -3 17.94 8.34
0 0 -3 6.17 11.08
0 0 -3 5.92 6.14
0 0 -3 4.91 15.92
0 0 -3 6.79 12.75
0 0 419746.17 4796.70
0 0 420309.96 4918.85
0 0 416127.92 3888.92
0 0 420153.49 4868.25
0 0 415777.58 3796.92
0 0 420921.98 5067.19
0 0 415756.83 3821.12
0 0 -420173.13 4857.60
0 0 -413318.34 3248.99
0 0 -418480.51 4467.76
0 0 -416958.19 4108.35
0 0 -415447.35 3769.82
0 0 -411639.67 2803.71
0 0 -413002.58 3157.06
0 0 5 48.67 25.75
0 0 5 37.14 31.15
0 0 5 32.81 27.26
0 0 5 30.87 17.17
0 0 5 50.12 25.83
0 0 5 41.15 34.99
0 0 5 36.99 29.41
0 0 -5 56.94 21.63
0 0 -5 45.03 27.04
0 0 -5 42.51 24.80
0 0 -5 38.15 21.80
0 0 -5 39.60 34.26
0 0 -5 63.66 12.24
0 0 -5 41.57 16.90
0 0 -5 48.02 23.36
0 0 6 5310.08 1083.98
0 0 6 5543.32 1142.68
0 0 6 5150.90 1065.40
0 0 6 6151.96 1276.62
0 0 6 5133.11 1072.39
0 0 6 4378.45 907.86
0 0 6 5216.96 1074.98
0 0 -6 4937.89 998.64
0 0 -6 4257.77 885.44
0 0 -6 4456.45 930.52
0 0 -6 5259.06 1071.23
0 0 -6 5449.23 1137.86
0 0 -6 4115.31 833.18
0 0 -6 3109.39 662.50
0 0 7 8.55 16.26
0 0 7 0.14 27.92
0 0 7 -0.31 28.14
0 0 7 -0.04 25.03
0 0 7 -0.17 30.80
0 0 7 1.10 25.97
0 0 -7 14.54 17.88
0 0 -7 31.21 46.88
0 0 -7 2.88 26.78
0 0 -7 4.45 12.13
0 0 -7 1.90 15.61
0 0 -7 4.58 30.96
0 0 -7 0.79 19.46
0 0 810389.47 2535.58
0 0 812728.53 3058.11
0 0 813363.01 3282.20
0 0 812492.15 3050.30
0 0 814474.37 3513.39
0 0 815871.45 3842.47
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-11 -1 -4 302.15 86.97
-11 -1 -4 286.06 114.93
-11 -1 -4 252.90 92.35
11 -1 -4 309.80 81.27
11 -1 -4 348.93 98.24
11 1 -4 311.64 113.58
11 -1 -4 297.26 90.53
11 1 5 970.57 214.40
11 -1 5 879.94 205.62
11 1 5 859.58 218.85
-11 1 5 689.41 171.87
11 -1 5 933.71 189.87
11 -1 5 982.93 242.69
-11 -1 5 1228.24 298.12
-11 1 -5 671.75 158.90
11 -1 -5 924.68 203.23
11 1 -5 863.62 210.90
-11 1 -5 634.54 346.67
11 1 -5 957.06 223.02
11 -1 -5 934.26 200.25
-11 -1 -5 737.53 179.08
-11 -1 -5 780.68 172.16
11 -1 -5 888.03 202.41
11 -1 -5 865.94 191.44
11 -1 6 180.04 79.05
11 -1 6 191.03 56.80
11 -1 6 222.19 102.65
-11 -1 6 197.40 74.97
11 1 6 211.55 82.07
11 1 6 181.69 93.12
11 -1 -6 206.04 75.85
-11 -1 -6 158.67 61.66
-11 1 -6 213.73 78.27
11 -1 -6 611.38 118.24
11 -1 -6 190.72 72.34
11 -1 -6 201.39 73.56
-11 -1 -6 170.42 85.30
-11 1 -6 156.65 158.93
11 1 -6 197.15 86.32
11 1 -6 652.83 186.22
11 1 7 146.19 82.75
11 1 7 159.91 69.85
-11 1 7 114.01 60.33
11 -1 7 161.96 89.30
11 -1 7 140.11 68.23
11 1 -7 152.74 82.88
-11 1 -7 102.64 65.45
-11 -1 -7 130.78 81.55
11 -1 -7 144.23 56.41
11 -1 -7 149.24 59.96
11 -1 -7 148.40 66.73
-11 -1 -7 122.13 53.21
11 1 -7 149.40 74.75
11 -1 8 72.55 65.23
-11 1 8 44.69 45.33
11 1 8 52.73 60.34
11 1 8 75.98 51.23
11 -1 8 56.87 48.20
11 -1 -8 48.59 50.44
11 1 -8 69.26 102.85
11 -1 -8 2.74 36.24
-11 -1 -8 33.17 32.79
-11 -1 -8 53.58 64.88
11 -1 -8 55.71 60.76
-11 1 -8 32.94 52.64
11 -2 0 117.53 86.86
-11 2 0 218.52 148.77
11 -2 0 130.12 76.88
11 2 0 110.46 69.71
-11 -2 0 144.60 71.05
11 2 0 506.29 117.07
-11 -2 0 126.31 119.45
11 -2 1 421.40 129.35
11 2 1 407.12 111.52
11 2 1 439.06 126.09
11 -2 1 408.85 133.76
-11 -2 1 496.04 194.32
-11 2 -1 234.77 167.96
11 2 -1 376.42 96.13
11 2 -1 404.50 118.09
-11 -2 -1 369.05 107.57
11 -2 -1 391.92 131.53
11 -2 -1 397.73 124.64
11 2 -1 495.45 133.02
-11 -2 -1 448.00 163.39
11 -2 2 76.73 70.87
11 -2 2 71.61 60.78
11 2 2 81.62 59.33
-11 2 2 54.66 205.98
11 2 2 65.07 45.96
-11 -2 2 84.82 192.54
-11 2 -2 65.65 110.82
-11 -2 -2 74.12 77.94
11 2 -2 65.32 40.12
11 -2 -2 71.57 63.51
11 -2 -2 69.86 65.61
11 2 -2 55.93 52.76
-11 -2 -2 56.11 52.44
11 2 -2 75.48 61.23
-11 2 3 116.49 178.24
11 2 3 113.09 48.68
11 -2 3 135.15 80.93
-11 -2 3 110.41 82.13
11 2 3 116.94 65.10
11 -2 3 122.43 68.70
-11 -2 -3 93.39 75.15
11 2 -3 119.91 46.39
-11 -2 -3 104.74 62.54
-11 2 -3 82.28 117.32
11 2 -3 130.14 70.63
11 -2 -3 125.86 75.76
11 2 -3 115.75 63.70
11 -2 -3 124.65 70.64
11 -2 4 36.96 55.82
11 -2 4 26.91 46.54
11 2 4 18.80 73.52
11 2 4 23.17 28.00
-11 2 4 53.92 92.05
11 2 4 0.37 41.21
-11 -2 4 26.47 59.31
11 2 -4 22.49 26.96
-11 2 -4 7.71 86.27
11 -2 -4 31.49 51.59
11 2 -4 22.22 43.45
11 -2 -4 23.03 51.53
-11 -2 -4 23.43 44.75
11 2 -4 20.85 48.38
11 2 5 809.21 186.70
-11 -2 5 985.46 229.04
11 -2 5 900.65 203.03
11 -2 5 1016.62 233.36
11 2 5 791.13 153.22
-11 -2 -5 903.94 204.55
11 -2 -5 833.16 252.29
-11 2 -5 308.48 181.68
11 2 -5 796.56 154.77
11 2 -5 949.09 274.38
11 2 -5 846.99 235.83
-11 -2 -5 706.60 222.27
11 -2 -5 904.74 213.03
11 -2 6 72.21 29.94
11 -2 6 81.90 52.45
11 2 6 71.37 51.83
11 -2 6 92.73 63.60
11 2 6 64.37 22.61
-11 -2 6 97.72 60.01
11 2 -6 88.79 61.37
-11 2 -6 100.29 170.16
-11 -2 -6 83.66 63.38
11 -2 -6 73.63 32.67
11 2 -6 72.93 41.60
-11 -2 -6 71.21 103.83
11 -2 -6 82.13 62.49
11 -2 -6 92.21 65.10
11 -2 7 41.66 40.35
11 -2 7 48.19 47.90
-11 2 7 34.59 54.65
11 -2 -7 39.97 48.38
-11 -2 -7 42.96 60.04
11 2 -7 75.82 47.48
11 2 -7 36.36 46.57
-11 -2 -7 0.17 90.12
11 -2 -7 51.25 23.23
11 3 0 97.27 70.85
11 3 0 139.02 71.82
11 -3 0 87.85 61.42
11 -3 0 112.69 84.66
11 3 0 144.50 44.45
-11 -3 0 123.70 72.17
-11 3 0 54.43 99.35
11 3 1 244.30 58.52
11 3 1 -4.64 66.17
11 -3 1 270.96 85.88
11 -3 1 297.35 109.85
-11 3 1 149.36 115.21
11 3 1 304.79 94.45
-11 -3 1 310.68 107.11
11 3 -1 319.12 99.12
11 -3 -1 315.83 114.55
-11 -3 -1 288.48 86.67
-11 3 -1 169.38 124.00
11 3 -1 233.44 60.40
-11 -3 -1 293.14 103.75
11 3 -1 306.27 92.88
11 -3 -1 277.56 90.75
-11 -3 2 260.26 106.12
11 -3 2 233.35 112.11
-11 3 2 187.68 200.31
11 -3 2 281.12 168.18
11 3 2 244.70 81.27
11 3 2 177.30 46.17
-11 -3 -2 232.99 67.96
11 -3 -2 237.75 85.90
11 3 -2 262.89 91.91
-11 -3 -2 229.18 93.87
11 3 -2 197.37 53.69
11 3 -2 238.54 81.38
-11 3 -2 144.53 115.90
11 -3 -2 263.93 102.77
-11 -3 3 222.88 95.13
11 -3 3 240.17 94.44
11 3 3 190.86 68.42
11 -3 3 182.81 63.81
11 3 -3 155.11 43.74
-11 -3 -3 177.20 85.58
11 3 -3 211.66 80.33
11 3 -3 195.92 105.74
-11 3 -3 93.92 106.70
-11 -3 -3 147.84 39.06
11 -3 -3 191.31 78.21
11 -3 -3 196.94 132.79
-11 -3 4 92.62 113.45
11 -3 4 73.17 40.63
11 3 4 76.43 44.55
11 -3 4 77.91 57.30
-11 -3 -4 60.19 35.34
11 -3 -4 81.76 64.21
11 -3 -4 72.37 52.40
11 3 -4 53.58 20.81
11 3 -4 81.35 45.18
-11 -3 -4 69.55 62.41
-11 3 -4 41.70 87.06
11 3 -4 75.58 56.31
11 3 5 491.38 105.36
11 -3 5 448.53 116.53
-11 -3 5 535.51 132.89
11 -3 5 344.70 71.79
-11 -3 -5 402.35 83.69
11 -3 -5 463.87 119.24
11 -3 -5 543.20 141.09
11 3 -5 530.99 125.00
-11 -3 -5 417.83 122.87
11 3 -5 491.62 106.43
12 0 0 221.64 76.22
-12 0 0 321.38 277.71
-12 0 1 1398.70 718.64
12 0 1 976.10 221.68
-12 0 -1 1296.44 490.36
12 0 -1 847.04 185.53
12 0 -1 959.74 190.26
12 0 -1 1120.22 271.58
12 0 2 59.02 59.34
-12 0 2 39.87 88.96
12 0 2 141.85 85.26
12 0 -2 56.79 36.41
12 0 -2 45.56 38.95
12 0 -2 64.96 63.26
-12 0 -2 88.45 194.88
12 0 3 938.86 224.18
-12 0 3 1018.84 262.84
12 0 3 614.54 190.23
-12 0 -3 1606.26 484.31
12 0 -3 1128.30 257.48
12 0 -3 1156.48 230.27
12 0 -3 1227.77 244.74
12 0 4 713.09 192.24
-12 0 4 714.28 191.10
12 0 4 833.64 203.56
-12 0 -4 496.50 214.79
12 0 -4 723.60 162.16
12 0 -4 726.42 148.86
12 0 -4 708.64 182.57
-12 0 5 1044.58 234.00
12 0 5 833.98 212.02
12 0 5 930.73 223.04
12 0 -5 739.91 145.00
12 0 -5 853.63 204.79
12 0 -5 827.29 183.92
-12 0 -5 621.89 153.27
12 0 6 691.71 186.88
12 0 6 812.12 202.79
12 0 -6 788.57 183.74
12 0 7 1393.15 316.87
12 0 7 1616.29 355.41
12 0 -7 1450.60 312.51
12 0 -7 1513.49 323.99
12 -1 0 482.88 138.07
-12 -1 0 390.29 148.37
12 -1 0 465.88 107.73
-12 1 0 437.82 358.44
12 1 0 494.90 111.27
12 -1 0 377.64 148.37
-12 1 1 287.77 290.80
12 -1 1 266.09 103.92
12 -1 1 236.80 65.00
12 -1 1 474.23 111.77
12 1 1 254.07 66.29
-12 -1 1 214.26 119.85
12 1 1 678.97 160.56
-12 -1 -1 200.84 109.48
-12 1 -1 234.12 312.76
12 -1 -1 252.02 98.17
12 1 -1 260.84 77.75
12 -1 -1 258.00 71.48
12 -1 -1 345.70 123.46
12 -1 2 20.91 42.36
12 -1 2 18.47 24.94
12 1 2 18.97 21.54
12 1 2 20.67 26.08
-12 1 2 28.89 156.31
12 -1 2 24.87 54.32
12 1 2 39.36 57.97
-12 -1 2 22.54 71.34
12 1 -2 26.65 37.50
-12 1 -2 164.68 209.51
-12 -1 -2 21.12 55.89
12 -1 -2 23.11 44.49
12 -1 -2 20.90 33.73
12 -1 -2 24.47 30.81
12 1 -2 23.55 49.07
12 -1 3 29.94 42.05
-12 -1 3 36.07 79.39
12 1 3 29.48 55.91
12 1 3 28.63 31.95
12 -1 3 29.94 57.61
-12 1 3 36.88 128.03
-12 -1 -3 22.36 50.15
12 1 -3 59.33 55.01
12 1 -3 26.57 45.94
12 -1 -3 28.65 31.29
12 -1 -3 24.74 43.84
-12 1 -3 30.31 196.67
12 -1 -3 25.60 34.74
-12 1 4 0.01 51.75
-12 -1 4 17.04 129.69
12 -1 4 40.72 39.50
12 1 4 0.40 29.52
12 -1 4 16.82 53.88
12 1 4 0.77 47.88
12 -1 -4 9.22 30.16
-12 1 -4 9.49 142.62
12 1 -4 11.12 45.96
-12 -1 -4 11.29 38.84
12 -1 -4 25.30 23.58
12 1 -4 11.35 42.78
12 -1 -4 43.54 39.02
12 -1 -4 14.41 28.06
12 -1 5 -0.28 50.18
12 -1 5 281.20 159.30
-12 -1 5 230.40 80.15
12 1 5 235.47 95.13
-12 1 -5 247.12 177.91
12 -1 -5 245.11 62.12
12 1 -5 244.81 84.52
12 -1 -5 236.79 71.96
12 -1 -5 223.97 65.19
12 -1 -5 241.18 64.49
12 -1 6 360.28 136.70
-12 1 6 288.59 77.00
12 -1 6 424.57 189.29
12 1 6 362.53 118.96
12 1 -6 367.69 105.75
12 -1 -6 386.14 89.68
12 -1 -6 367.18 90.76
12 -1 -6 363.31 84.13
12 2 0 75.21 38.13
12 -2 0 38.38 103.84
-12 -2 0 27.67 61.51
12 -2 0 63.09 56.01
12 2 0 488.76 128.75
-12 2 0 23.36 226.62
12 2 0 45.70 47.28
12 2 1 376.81 106.67
12 2 1 363.04 85.94
12 2 1 436.58 105.15
-12 2 1 347.58 291.79
-12 -2 1 394.83 127.22
12 -2 1 412.14 110.01
12 -2 1 397.36 122.06
12 2 -1 432.75 113.24
-12 -2 -1 350.68 107.30
-12 2 -1 283.51 340.63
12 2 -1 356.23 81.72
12 -2 -1 397.86 111.49
12 -2 -1 388.37 119.94
12 2 -1 354.93 104.56
12 -2 2 45.77 43.05
12 -2 2 46.75 55.68
-12 -2 2 57.27 61.15
-12 2 2 45.39 145.38
12 2 2 62.73 35.76
12 2 2 -0.31 27.09
12 2 2 38.81 45.51
-12 2 -2 22.28 216.68
12 2 -2 46.34 48.15
12 2 -2 35.89 47.10
12 -2 -2 40.27 55.16
12 2 -2 37.15 39.28
-12 -2 -2 33.55 39.28
12 -2 -2 41.90 75.95
-12 -2 3 479.27 141.90
12 2 3 408.75 107.32
12 -2 3 475.43 132.38
12 2 3 458.03 96.88
12 -2 3 438.85 106.73
-12 2 3 576.81 217.47
12 2 -3 434.69 113.98
-12 -2 -3 417.97 101.42
-12 2 -3 301.73 325.76
12 -2 -3 492.94 125.05
-12 -2 -3 395.41 91.63
12 -2 -3 459.72 127.99
12 2 -3 463.68 125.09
-12 -2 4 18.97 51.04
12 2 4 22.08 34.94
12 -2 4 13.39 29.06
12 -2 4 13.26 45.24
12 2 4 24.73 15.89
12 -2 -4 23.22 39.98
-12 2 -4 10.87 161.12
12 2 -4 21.24 45.00
12 -2 -4 0.48 74.11
12 2 -4 1.00 62.19
-12 -2 -4 15.38 30.00
12 2 5 64.36 40.97
-12 -2 5 81.06 57.62
12 -2 5 75.30 53.30
12 -2 5 47.54 22.85
12 -2 -5 86.52 53.36
12 -2 -5 76.43 50.06
12 2 -5 76.46 53.75
-12 2 -5 73.26 146.69
12 2 -5 71.13 45.04
12 3 0 1712.23 357.99
12 3 0 1599.98 319.12
12 -3 0 1608.03 349.10
12 -3 0 1536.85 323.77
-12 -3 0 1697.08 403.82
-12 3 0 1104.79 451.22
13 0 0 1.66 20.53
-13 0 0 8.69 55.35
-13 0 1 0.17 46.55
13 0 1 1.68 20.38
13 0 -1 0.04 16.77
13 0 -1 0.56 29.29
-13 0 -1 0.42 46.38
-13 0 2 -0.19 43.21
13 0 2 -0.06 31.86
13 0 2 0.92 23.11
13 0 -2 4.62 28.99
13 0 -2 0.05 15.33
-13 0 -2 5.14 44.65
13 0 -2 0.54 9.29
-13 0 3 -2.03 39.33
13 0 3 0.25 30.23
13 0 3 -0.13 24.80
13 0 -3 0.39 27.31
13 0 -3 2.23 28.48
-13 0 -3 3.19 36.99
13 0 4 0.03 51.38
13 0 -4 791.99 157.84
-13 -1 0 33.65 68.01
13 1 0 27.83 23.08
13 1 0 40.36 49.21
13 -1 0 0.09 39.80
13 -1 0 44.87 32.93
-13 1 0 8.79 153.80
13 -1 1 58.44 52.44
13 1 1 53.76 56.31
-13 -1 1 74.33 83.29
-13 1 1 8.68 136.74
13 -1 1 19.52 32.62
13 1 -1 58.42 33.45
13 -1 -1 61.87 35.57
13 1 -1 54.13 53.72
-13 -1 -1 67.08 70.10
-13 1 -1 74.74 174.08
13 -1 -1 66.49 47.63
13 -1 2 39.67 34.59
-13 1 2 36.84 70.02
-13 -1 2 66.28 143.04
13 -1 2 44.86 51.02
13 1 2 39.14 54.29
13 1 -2 40.69 52.06
13 1 -2 41.75 34.67
-13 -1 -2 47.50 59.76
13 -1 -2 38.61 32.37
-13 1 -2 61.38 156.57
13 -1 -2 39.22 42.08
13 -1 3 437.59 121.92
13 1 3 399.34 115.59
-13 -1 3 389.40 114.82
13 -1 3 355.21 86.29
-13 1 3 375.97 119.91
13 -1 -3 440.27 105.10
13 1 -3 428.63 101.58
13 1 -3 419.01 118.36
-13 -1 -3 471.66 161.50
-13 1 -3 562.23 254.98
;
_shelx_hkl_checksum 26783
_shelx_res_file
;
TITL DL-Psicose_CS41
CELL 1.54187 11.26293 5.35518 12.65375 90.000 90.000 90.000
ZERR 4 0.00054 0.00025 0.00063 0.000 0.000 0.000
LATT -1
SYMM .50-X, .50+Y, .50+Z
SYMM .50+X, .50-Y, +Z
SYMM -X, -Y, .50+Z
SFAC C H O
UNIT 24 48 24
OMIT 6 0 0
L.S. 100
FMAP 2
PLAN -15
TWIN
WPDB -2
HTAB
LIST 4
TEMP 23.0
ACTA
SIZE 0.100 0.100 0.100
WGHT 0.035900
EXTI 0.038908
BASF 0.05407
FVAR 2.87476
O1 3 0.642841 1.047517 0.010128 11.00000 0.02322 0.04307 =
0.03010 0.01262 -0.00580 -0.00194
AFIX 147
H1A 2 0.597718 0.957556 0.043845 11.00000 -1.20000
AFIX 0
O2 3 0.813849 1.322544 0.124364 11.00000 0.02381 0.02277 =
0.03835 0.00250 0.00571 0.00099
AFIX 147
H2A 2 0.750435 1.364666 0.150740 11.00000 -1.20000
AFIX 0
O3 3 0.971226 0.740684 0.098578 11.00000 0.02520 0.02405 =
0.03404 -0.00196 0.00682 0.00134
AFIX 147
H3A 2 0.928317 0.653243 0.135610 11.00000 -1.20000
AFIX 0
O4 3 1.126345 0.994145 0.236020 11.00000 0.01926 0.02649 =
0.04595 0.00134 -0.00217 0.00035
AFIX 147
H4A 2 1.131296 0.841675 0.231984 11.00000 -1.20000
AFIX 0
O5 3 0.951990 0.694130 0.320064 11.00000 0.04747 0.03088 =
0.03218 0.01012 0.01015 0.00641
AFIX 147
H5A 2 0.921923 0.632180 0.372939 11.00000 -1.20000
AFIX 0
O6 3 0.759262 0.948664 0.206792 11.00000 0.02295 0.02971 =
0.02033 0.00021 0.00267 -0.00570
C1 1 0.761005 0.960010 0.021770 11.00000 0.02473 0.03231 =
0.02541 0.00239 -0.00015 -0.00009
AFIX 23
H1B 2 0.806947 1.008921 -0.039676 11.00000 -1.20000
H1C 2 0.760421 0.779039 0.024969 11.00000 -1.20000
AFIX 0
C2 1 0.819911 1.061362 0.119910 11.00000 0.02108 0.02276 =
0.01946 0.00433 0.00341 0.00116
C3 1 0.952461 0.995571 0.123798 11.00000 0.01974 0.02333 =
0.02390 0.00421 0.00376 0.00090
AFIX 13
H3B 2 0.992732 1.095895 0.069849 11.00000 -1.20000
AFIX 0
C4 1 1.004903 1.066468 0.230619 11.00000 0.01886 0.02461 =
0.02654 0.00057 0.00003 0.00086
AFIX 13
H4B 2 1.001467 1.248719 0.236915 11.00000 -1.20000
AFIX 0
C5 1 0.933707 0.956356 0.321030 11.00000 0.02973 0.03002 =
0.02013 -0.00014 -0.00112 0.00265
AFIX 13
H5B 2 0.963223 1.024598 0.387916 11.00000 -1.20000
AFIX 0
C6 1 0.804388 1.025849 0.308278 11.00000 0.02719 0.03873 =
0.02092 -0.00018 0.00551 0.00055
AFIX 23
H6A 2 0.758276 0.947073 0.363778 11.00000 -1.20000
H6B 2 0.795658 1.205253 0.315440 11.00000 -1.20000
AFIX 0
HKLF 4
REM DL-Psicose_CS41
REM R1 = 0.0475 for 1295 Fo > 4sig(Fo) and 0.0511 for all 1400 data
REM 116 parameters refined using 1 restraints
END
WGHT 0.0359 0.0000
REM Instructions for potential hydrogen bonds
EQIV $1 x-1/2, -y+3/2, z
HTAB O1 O3_$1
EQIV $2 x-1/2, -y+5/2, z
HTAB O2 O4_$2
EQIV $3 x, y-1, z
HTAB O3 O2_$3
HTAB O3 O5
EQIV $4 x+1/2, -y+3/2, z
HTAB O4 O6_$4
EQIV $5 -x+3/2, y-1/2, z+1/2
HTAB O5 O1_$5
REM Highest difference peak 0.248, deepest hole -0.234, 1-sigma level 0.056
Q1 1 0.8865 1.0281 0.1206 11.00000 0.05 0.25
Q2 1 0.8747 0.9909 0.3038 11.00000 0.05 0.18
Q3 1 0.7820 0.9920 0.2364 11.00000 0.05 0.18
Q4 1 0.9725 1.0153 0.2795 11.00000 0.05 0.17
Q5 1 0.8715 0.7503 0.1199 11.00000 0.05 0.17
Q6 1 0.9647 0.7048 -0.0816 11.00000 0.05 0.16
Q7 1 0.8579 0.5763 0.3244 11.00000 0.05 0.16
Q8 1 1.0555 1.0313 0.2315 11.00000 0.05 0.16
Q9 1 0.9961 1.0406 0.1792 11.00000 0.05 0.15
Q10 1 0.5593 1.1947 0.0192 11.00000 0.05 0.15
Q11 1 0.6816 0.8095 0.4178 11.00000 0.05 0.15
Q12 1 0.7955 1.0104 0.1697 11.00000 0.05 0.15
Q13 1 0.6435 1.0650 -0.0578 11.00000 0.05 0.15
Q14 1 0.8554 0.8023 0.3164 11.00000 0.05 0.14
Q15 1 0.9848 0.7331 0.0145 11.00000 0.05 0.14
;
_shelx_res_checksum 66640