#------------------------------------------------------------------------------
#$Date: 2016-05-06 04:19:40 +0200 (vie 06 de may de 2016) $
#$Revision: 182798 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/48/7224884.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7224884
loop_
_publ_author_name
'Patyk, Ewa'
'Jenczak, Anna'
'Katrusiak, Andrzej'
_publ_section_title
;
 Giant strain geared to transformable H-bonded network in compressed
 β-d-mannose.
;
_journal_issue                   16
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              11474
_journal_page_last               11479
_journal_paper_doi               10.1039/c6cp01286h
_journal_volume                  18
_journal_year                    2016
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C6 H12 O6'
_chemical_formula_sum            'C6 H12 O6'
_chemical_formula_weight         180.16
_chemical_melting_point          400
_chemical_name_common            β-D-mannose
_chemical_name_systematic        β-D-mannopyranose
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-02-04 deposited with the CCDC.
2016-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.58(3)
_cell_length_b                   8.401(8)
_cell_length_c                   17.20(5)
_cell_measurement_reflns_used    128
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      17.1230
_cell_measurement_theta_min      4.9900
_cell_volume                     662(5)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies,Version 1.171.37.31'
_computing_data_collection
'CrysAlisPro, Agilent Technologies,Version 1.171.37.31'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies,Version 1.171.37.31'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         2350000
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 16.2413
_diffrn_measured_fraction_theta_full 0.282
_diffrn_measured_fraction_theta_max 0.271
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2644
_diffrn_reflns_av_unetI/netI     0.2946
_diffrn_reflns_Laue_measured_fraction_full 0.282
_diffrn_reflns_Laue_measured_fraction_max 0.271
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            1474
_diffrn_reflns_point_group_measured_fraction_full 0.272
_diffrn_reflns_point_group_measured_fraction_max 0.260
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.754
_diffrn_reflns_theta_min         4.853
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.164
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
; 
 Flack x determined using 22 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   6.7(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         331
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1668
_refine_ls_R_factor_gt           0.1163
_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)+(0.0989P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2375
_refine_ls_wR_factor_ref         0.2857
_reflns_Friedel_coverage         0.561
_reflns_Friedel_fraction_full    0.257
_reflns_Friedel_fraction_max     0.242
_reflns_number_gt                144
_reflns_number_total             331
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6cp01286h6.cif
_cod_data_source_block           bman6_2350MPa
_cod_depositor_comments
'Adding full bibliography for 7224879--7224889.cif.'
_cod_original_cell_volume        662(4)
_cod_database_code               7224884
_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. 
;
_shelx_res_file
; 
      bman6.res created by SHELXL-2014/7 
  
  
TITL a in P2(1)2(1)2(1) 
CELL 0.71073   4.5848   8.4006  17.2002  90.000  90.000  90.000 
ZERR    4.00   0.0265   0.0077   0.0543   0.000   0.000   0.000 
LATT -1 
SYMM 0.5-X, -Y, 0.5+Z 
SYMM -X, 0.5+Y, 0.5-Z 
SYMM 0.5+X, 0.5-Y, -Z 
SFAC C H O 
UNIT 24 48 24 
  
L.S. 100 
BOND 
FMAP 2 
PLAN 20 
ACTA 
dfix 1.5000 0.02 c1 c2 
dfix 1.5000 0.02 c3 c4 
dfix 1.5000 0.02 c5 c6 
dfix 1.5000 0.02 c2 c3 
dfix 1.4500 0.02 o3 c3 
EQIV $1 1-X, -0.5+Y, 0.5-Z 
EQIV $2 1-X, 0.5+Y, 0.5-Z 
EQIV $3 0.5+X, 1.5-Y, -Z 
EQIV $4 0.5+X, 0.5-Y, -Z 
EQIV $5 -X, -0.5+Y, 0.5-Z 
EQIV $6 -0.5+X, 1.5-Y, -Z 
EQIV $7 X, 1+Y, Z 
EQIV $8 X, -1+Y, Z 
EQIV $9 -1+X, Y, Z 
EQIV $10 -X, 0.5+Y, 0.5-Z 
EQIV $11 -0.5+X, 0.5-Y, -Z 
  
RTAB oho1 O1 O3_$1 
RTAB oho1 H8 O3_$1 
RTAB oho1 O1 H8 O3_$1 
RTAB oho1 C1 O1 O3_$1 
RTAB oho1 O1 O3_$1 c3_$1 
  
RTAB oho2 O1 O6_$2 
RTAB oho2 H8 O6_$2 
RTAB oho2 O1 H8 O6_$2 
RTAB oho2 C1 O1 O6_$2 
RTAB oho2 O1 O6_$2 c6_$2 
  
RTAB oho3 O2 O5_$2 
RTAB oho3 H9 O5_$2 
RTAB oho3 O2 H9 O5_$2 
RTAB oho3 C2 O2 O5_$2 
  
RTAB oho4 O2 O1_$2 
RTAB oho4 H9 O1_$2 
RTAB oho4 O2 H9 O1_$2 
RTAB oho4 C2 O2 O1_$2 
RTAB oho4 O2 O1_$2 c1_$2 
  
RTAB oho5 O3 O4_$3 
RTAB oho5 H10 O4_$3 
RTAB oho5 O3 H10 O4_$3 
RTAB oho5 C3 O3 O4_$3 
RTAB oho5 O3 O4_$3 c4_$3 
  
RTAB oho6 O3 O4_$6 
RTAB oho6 H10 O4_$6 
RTAB oho6 O3 H10 O4_$6 
RTAB oho6 C3 O3 O4_$6 
RTAB oho6 O3 O4_$6 c4_$6 
  
RTAB oho7 O3 O3_$6 
RTAB oho7 H10 O3_$6 
RTAB oho7 O3 H10 O3_$6 
RTAB oho7 C3 O3 O3_$6 
RTAB oho7 O3 O3_$6 c3_$6 
  
RTAB oo1 O3 O6_$7 
RTAB oo1 H10 O6_$7 
RTAB oo1 O3 H10 O6_$7 
RTAB oo1 C3 O3 O6_$7 
RTAB oo1 O3 O6_$7 c6_$7 
  
RTAB oho8 O4 O6_$4 
RTAB oho8 H11 O6_$4 
RTAB oho8 O4 H11 O6_$4 
RTAB oho8 C4 O4 O6_$4 
RTAB oho8 O4 O6_$4 c6_$4 
  
RTAB oho9 O4 O3_$6 
RTAB oho9 H11 O3_$6 
RTAB oho9 O4 H11 O3_$6 
RTAB oho9 C4 O4 O3_$6 
RTAB oho9 O4 O3_$6 c3_$6 
  
RTAB oh10 O6 O1_$5 
RTAB oh10 H12 O1_$5 
RTAB oh10 O6 H12 O1_$5 
RTAB oh10 C6 O6 O1_$5 
RTAB oh10 O6 O1_$5 c1_$5 
  
RTAB oo2 O6 O3_$8 
RTAB oo2 H12 O3_$8 
RTAB oo2 O6 H12 O3_$8 
RTAB oo2 C6 O6 O3_$8 
RTAB oo2 O6 O3_$8 c3_$8 
  
RTAB cho1 C1 O2_$9 
RTAB cho1 H1 O2_$9 
RTAB cho1 C1 H1 O2_$9 
RTAB cho1 C1 O2_$9 c2_$9 
  
RTAB cho2 C2 O1_$10 
RTAB cho2 H2 O1_$10 
RTAB cho2 C2 H2 O1_$10 
RTAB cho2 C2 O1_$10 c1_$10 
  
RTAB cho3 C2 O2_$9 
RTAB cho3 H2 O2_$9 
RTAB cho3 C2 H2 O2_$9 
RTAB cho3 C2 O2_$9 c2_$9 
  
RTAB cho4 C2 O2_$2 
RTAB cho4 H2 O2_$2 
RTAB cho4 C2 H2 O2_$2 
RTAB cho4 C2 O2_$2 c2_$2 
  
RTAB cho5 C2 O5_$10 
RTAB cho5 H2 O5_$10 
RTAB cho5 C2 H2 O5_$10 
  
RTAB cho6 C3 O2_$9 
RTAB cho6 H3 O2_$9 
RTAB cho6 C3 H3 O2_$9 
RTAB cho6 C3 O2_$9 c2_$9 
  
RTAB cho7 C3 O3_$6 
RTAB cho7 H3 O3_$6 
RTAB cho7 C3 H3 O3_$6 
RTAB cho7 C3 O3_$6 c3_$6 
  
RTAB cho8 C3 O4_$6 
RTAB cho8 H3 O4_$6 
RTAB cho8 C3 H3 O4_$6 
RTAB cho8 C3 O4_$6 c4_$6 
  
RTAB cho9 C3 O6_$7 
RTAB cho9 H3 O6_$7 
RTAB cho9 C3 H3 O6_$7 
RTAB cho9 C3 O6_$7 c6_$7 
  
RTAB ch10 C4 O3_$3 
RTAB ch10 H4 O3_$3 
RTAB ch10 C4 H4 O3_$3 
RTAB ch10 C4 O3_$3 c3_$3 
  
RTAB ch11 C6 O6_$4 
RTAB ch11 H6 O6_$4 
RTAB ch11 C6 H6 O6_$4 
RTAB ch11 C6 O6_$4 c6_$4 
  
RTAB ch12 C6 O3_$8 
RTAB ch12 H7 O3_$8 
RTAB ch12 C6 H7 O3_$8 
RTAB ch12 C6 O3_$8 c3_$8 
  
RTAB hh1 H1 H9_$9 
RTAB hh2 H3 H4_$9 
RTAB hh3 H3 H10_$6 
RTAB hh4 H3 H11_$6 
RTAB hh5 H4 H10_$3 
RTAB hh6 H5 H7_$9 
RTAB hh7 H6 H7_$11 
RTAB hh8 H7 H8_$1 
RTAB hh9 H8 H9_$1 
RTAB hh10 H8 H12_$10 
RTAB hh11 H10 H11_$3 
RTAB hh12 H10 H11_$6 
RTAB hh13 H11 H12_$4 
WGHT    0.098900 
FVAR       1.20616   0.05150   0.05751 
C1    1    0.119804    0.562453    0.214596    11.00000   21.00000 
AFIX  13 
H1    2   -0.092410    0.550952    0.210735    11.00000   -1.20000 
AFIX   0 
C2    1    0.221960    0.711371    0.175381    11.00000   21.00000 
AFIX  13 
H2    2    0.121716    0.805316    0.196045    11.00000   -1.20000 
AFIX   0 
C3    1    0.146374    0.684208    0.089862    11.00000   21.00000 
AFIX  13 
H3    2   -0.065170    0.683843    0.081700    11.00000   -1.20000 
AFIX   0 
C4    1    0.278031    0.537145    0.062744    11.00000   21.00000 
AFIX  13 
H4    2    0.488091    0.553449    0.069651    11.00000   -1.20000 
AFIX   0 
C5    1    0.204002    0.390535    0.116116    11.00000   21.00000 
AFIX  13 
H5    2   -0.007208    0.374301    0.112397    11.00000   -1.20000 
AFIX   0 
C6    1    0.342222    0.239313    0.091115    11.00000   21.00000 
AFIX  23 
H6    2    0.274483    0.215510    0.038969    11.00000   -1.20000 
H7    2    0.551012    0.256826    0.087981    11.00000   -1.20000 
AFIX   0 
O1    3    0.210434    0.557664    0.290505    11.00000   31.00000 
AFIX  83 
H8    2    0.376754    0.592991    0.293612    11.00000   -1.50000 
AFIX   0 
O2    3    0.523268    0.729513    0.178632    11.00000   31.00000 
AFIX  83 
H9    2    0.565405    0.791742    0.213603    11.00000   -1.50000 
AFIX   0 
O3    3    0.286939    0.817281    0.047616    11.00000   31.00000 
AFIX  83 
H10   2    0.162879    0.867294    0.023480    11.00000   -1.50000 
AFIX   0 
O4    3    0.248017    0.500476   -0.012453    11.00000   31.00000 
AFIX  83 
H11   2    0.106728    0.547765   -0.030369    11.00000   -1.50000 
AFIX   0 
O5    3    0.263071    0.421296    0.192863    11.00000   31.00000 
O6    3    0.296107    0.108557    0.135893    11.00000   31.00000 
AFIX  83 
H12   2    0.120363    0.095832    0.142191    11.00000   -1.50000 
  
AFIX   0 
HKLF 4 
  
REM  a in P2(1)2(1)2(1) 
REM R1 =  0.1163 for     144 Fo > 4sig(Fo)  and  0.1668 for all     331 data 
REM     39 parameters refined using      5 restraints 
  
END 
  
WGHT      0.0992      0.0000 
  
REM Highest difference peak  0.301,  deepest hole -0.307,  1-sigma level  0.086 
Q1    1   0.2223  0.8050  0.0350  11.00000  0.05    0.30 
Q2    1   0.5903  0.4843  0.1880  11.00000  0.05    0.29 
Q3    1   0.2163  0.5318  0.0194  11.00000  0.05    0.25 
Q4    1  -0.2872  0.5809  0.2621  11.00000  0.05    0.23 
Q5    1   0.4421  0.5103 -0.0219  11.00000  0.05    0.23 
Q6    1   0.3000  0.7112  0.2197  11.00000  0.05    0.22 
Q7    1   0.7422  0.7626  0.1607  11.00000  0.05    0.21 
Q8    1   0.7542  0.7973  0.1399  11.00000  0.05    0.20 
Q9    1   0.2412  0.5005 -0.0639  11.00000  0.05    0.20 
Q10   1   0.3062 -0.0549  0.1162  11.00000  0.05    0.19 
Q11   1   0.0845  0.6588  0.0878  11.00000  0.05    0.18 
Q12   1   0.5159  0.5650  0.3160  11.00000  0.05    0.17 
Q13   1   0.3209  0.2079  0.0194  11.00000  0.05    0.17 
Q14   1   0.2720  0.4416  0.2161  11.00000  0.05    0.16 
Q15   1   0.0678  0.3784  0.0356  11.00000  0.05    0.16 
Q16   1   0.1910  0.4201  0.2009  11.00000  0.05    0.16 
Q17   1   0.1253  0.3618  0.0666  11.00000  0.05    0.15 
Q18   1   0.2562  0.3749  0.0841  11.00000  0.05    0.15 
Q19   1   0.0704  0.5639 -0.0535  11.00000  0.05    0.15 
Q20   1   0.0410  0.6773  0.2881  11.00000  0.05    0.15 
;
_shelx_res_checksum              94489
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
C1 C 0.120(8) 0.562(3) 0.2146(19) 0.051(4) Uiso 1 1 d D U
H1 H -0.0924 0.5510 0.2107 0.062 Uiso 1 1 calc R U
C2 C 0.222(11) 0.711(3) 0.1754(15) 0.051(4) Uiso 1 1 d D U
H2 H 0.1217 0.8053 0.1960 0.062 Uiso 1 1 calc R U
C3 C 0.146(7) 0.684(3) 0.0899(15) 0.051(4) Uiso 1 1 d D U
H3 H -0.0652 0.6838 0.0817 0.062 Uiso 1 1 calc R U
C4 C 0.278(9) 0.537(2) 0.063(2) 0.051(4) Uiso 1 1 d D U
H4 H 0.4881 0.5534 0.0697 0.062 Uiso 1 1 calc R U
C5 C 0.204(8) 0.391(2) 0.116(2) 0.051(4) Uiso 1 1 d D U
H5 H -0.0072 0.3743 0.1124 0.062 Uiso 1 1 calc R U
C6 C 0.342(7) 0.239(2) 0.0911(18) 0.051(4) Uiso 1 1 d D U
H6 H 0.2745 0.2155 0.0390 0.062 Uiso 1 1 calc R U
H7 H 0.5510 0.2568 0.0880 0.062 Uiso 1 1 calc R U
O1 O 0.210(6) 0.5577(17) 0.2905(12) 0.058(4) Uiso 1 1 d . U
H8 H 0.3768 0.5930 0.2936 0.086 Uiso 1 1 calc R U
O2 O 0.523(6) 0.7295(17) 0.1786(12) 0.058(4) Uiso 1 1 d . U
H9 H 0.5654 0.7917 0.2136 0.086 Uiso 1 1 calc R U
O3 O 0.287(5) 0.8173(18) 0.0476(10) 0.058(4) Uiso 1 1 d D U
H10 H 0.1629 0.8673 0.0235 0.086 Uiso 1 1 calc R U
O4 O 0.248(6) 0.5005(18) -0.0125(11) 0.058(4) Uiso 1 1 d . U
H11 H 0.1067 0.5478 -0.0304 0.086 Uiso 1 1 calc R U
O5 O 0.263(6) 0.4213(16) 0.1929(12) 0.058(4) Uiso 1 1 d . U
O6 O 0.296(6) 0.1086(15) 0.1359(11) 0.058(4) Uiso 1 1 d . U
H12 H 0.1204 0.0958 0.1422 0.086 Uiso 1 1 calc R U
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
O1 C1 O5 95(2)
O1 C1 C2 111(2)
O5 C1 C2 116(2)
O2 C2 C1 113(3)
O2 C2 C3 106(2)
C1 C2 C3 104(2)
C4 C3 O3 108(2)
C4 C3 C2 110(3)
O3 C3 C2 105(2)
O4 C4 C3 118(3)
O4 C4 C5 111(2)
C3 C4 C5 113(2)
O5 C5 C6 111(3)
O5 C5 C4 112(2)
C6 C5 C4 114(2)
O6 C6 C5 117(2)
C5 O5 C1 109(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 O1 1.37(4)
C1 O5 1.41(3)
C1 C2 1.50(2)
C2 O2 1.39(5)
C2 C3 1.53(2)
C3 C4 1.45(2)
C3 O3 1.48(2)
C4 O4 1.34(4)
C4 C5 1.57(4)
C5 O5 1.37(4)
C5 C6 1.48(2)
C6 O6 1.36(2)
