#------------------------------------------------------------------------------
#$Date: 2021-03-02 08:04:16 +0200 (Tue, 02 Mar 2021) $
#$Revision: 262343 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/87/2108776.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_2108776
loop_
_publ_author_name
'Safari, Fatemeh'
'Katrusiak, Andrzej'
_publ_section_title
;
 Structure--property relationships of molecular shape and orientation with
 compression and expansion of xylitol
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520621000445
_journal_volume                  77
_journal_year                    2021
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C5 H12 O5'
_chemical_formula_sum            'C5 H12 O5'
_chemical_formula_weight         152.15
_chemical_name_common            xylitol
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.204(2)
_cell_length_b                   8.854(2)
_cell_length_c                   8.6809(7)
_cell_measurement_reflns_used    805
_cell_measurement_temperature    296.0(5)
_cell_measurement_theta_max      20.3060
_cell_measurement_theta_min      3.2740
_cell_volume                     630.6(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.355
_diffrn_measured_fraction_theta_max 0.316
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.355
_diffrn_reflns_Laue_measured_fraction_max 0.316
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2619
_diffrn_reflns_point_group_measured_fraction_full 0.374
_diffrn_reflns_point_group_measured_fraction_max 0.329
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.283
_diffrn_reflns_theta_min         3.287
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_description       prism
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.113
_refine_diff_density_min         -0.131
_refine_diff_density_rms         0.030
_refine_ls_abs_structure_details
;
 Flack x determined using 141 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -1.4(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         467
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0381P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0681
_refine_ls_wR_factor_ref         0.0765
_reflns_Friedel_coverage         0.749
_reflns_Friedel_fraction_full    0.404
_reflns_Friedel_fraction_max     0.349
_reflns_number_gt                377
_reflns_number_total             467
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            um5047sup1.cif
_cod_data_source_block           Xylitol0_96GPa
_cod_database_code               2108776
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 C4-C3
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C3(H3A), C2(H2A), C4(H4A)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C5(H5A,H5B)
4.c Tetrahedral OH refined with riding coordinates:
 O2(H2), O1(H1)
4.d Idealised tetrahedral OH refined as rotating group:
 O4(H4), O3(H3), O5(H5)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_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_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O4 O 0.4743(7) 0.6414(7) 0.6198(4) 0.0327(16) Uani 1 1 d . . . . .
H4 H 0.517113 0.595187 0.690941 0.049 Uiso 1 1 calc GR . . . .
O2 O 0.8621(7) 0.5708(5) 0.3055(4) 0.0345(15) Uani 1 1 d . . . . .
H2 H 0.908398 0.648302 0.333141 0.052 Uiso 1 1 calc R . . . .
O3 O 0.5648(8) 0.7135(6) 0.3134(4) 0.0345(14) Uani 1 1 d . . . . .
H3 H 0.571989 0.713761 0.219157 0.052 Uiso 1 1 calc GR . . . .
O1 O 0.9253(9) 0.3258(7) 0.5080(4) 0.0376(17) Uani 1 1 d . . . . .
H1 H 0.988519 0.395549 0.490910 0.056 Uiso 1 1 calc R . . . .
O5 O 0.1573(8) 0.5325(7) 0.5401(5) 0.0366(17) Uani 1 1 d . . . . .
H5 H 0.139862 0.607349 0.593221 0.055 Uiso 1 1 calc GR . . . .
C3 C 0.5752(11) 0.5614(9) 0.3688(6) 0.028(2) Uani 1 1 d D . . . .
H3A H 0.548859 0.493888 0.282871 0.034 Uiso 1 1 calc R . . . .
C2 C 0.7473(12) 0.5268(9) 0.4195(7) 0.030(2) Uani 1 1 d . U . . .
H2A H 0.770415 0.581089 0.515373 0.035 Uiso 1 1 calc R . . . .
C1 C 0.7706(12) 0.3607(10) 0.4455(8) 0.032(2) Uani 1 1 d . . . . .
H1A H 0.686646 0.324602 0.515009 0.039 Uiso 1 1 calc R . . . .
H1B H 0.757769 0.308051 0.348256 0.039 Uiso 1 1 calc R . . . .
C4 C 0.4455(11) 0.5393(9) 0.4927(6) 0.0286(19) Uani 1 1 d D . . . .
H4A H 0.451795 0.435240 0.530780 0.034 Uiso 1 1 calc R . . . .
C5 C 0.2780(11) 0.5662(9) 0.4297(8) 0.032(2) Uani 1 1 d . . . . .
H5A H 0.267959 0.671074 0.398625 0.038 Uiso 1 1 calc R . . . .
H5B H 0.261608 0.503742 0.339215 0.038 Uiso 1 1 calc R . . . .
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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 C3 C2 110.2(6) . . ?
O3 C3 C4 108.4(5) . . ?
C2 C3 C4 114.9(6) . . ?
O2 C2 C3 111.2(5) . . ?
O2 C2 C1 106.8(6) . . ?
C1 C2 C3 111.2(7) . . ?
O1 C1 C2 112.7(7) . . ?
O4 C4 C3 110.1(6) . . ?
O4 C4 C5 109.2(6) . . ?
C5 C4 C3 111.2(5) . . ?
O5 C5 C4 111.2(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O4 C4 1.446(8) . ?
O2 C2 1.420(10) . ?
O3 C3 1.433(8) . ?
O1 C1 1.415(9) . ?
O5 C5 1.410(8) . ?
C3 C2 1.510(10) . ?
C3 C4 1.526(10) . ?
C2 C1 1.500(11) . ?
C4 C5 1.498(10) . ?

_cod_database_fobs_code 2108776
