Dehydration of raffinose pentahydrate: structures of raffinose 5-, 4.433-, 4.289- and 4.127-hydrate at 93K
Viriyarattanasak, Chotika; Shiro, Motoo; Munekawa, Shigeru; Franks, Felix; Ikeda, Satomi; Kajiwara, Kazuhito; Acta Crystallographica Section C 71 (2015) –; doi:10.1107/S2053229615017374

data_2020210
_publ_section_title
;
 Dehydration of raffinose pentahydrate: structures of raffinose 5-,
 4.433-, 4.289- and 4.127-hydrate at 93K
;
_journal_coeditor_code           SK3602
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229615017374
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C18 H32 O16 , 4.127H2 O'
_chemical_formula_moiety         'C18 H32 O16, 4.127(H2 O)'
_chemical_formula_sum            'C18 H40.254 O20.127'
_chemical_formula_weight         578.84
_chemical_name_systematic
;<i>O</i>-\a-<i>D</i>-Galactopyranosyl-(1 \\rightarrow 6)-\a-<i>D</i>-glucopyranosyl-(1 \\rightarrow 2)-\b-<i>D</i>-fructofuranose
4.127-hydrate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   8.93444(16)
_cell_length_b                   12.3196(2)
_cell_length_c                   23.6037(4)
_cell_measurement_reflns_used    13668
_cell_measurement_temperature    93
_cell_measurement_theta_max      68.19
_cell_measurement_theta_min      4.05
_cell_volume                     2598.03(8)
_computing_cell_refinement
;
RAPID-AUTO (Rigaku, 1998)
;
_computing_data_collection
;
RAPID-AUTO (Rigaku, 1998)
;
_computing_data_reduction
;
RAPID-AUTO (Rigaku, 1998)
;
_computing_molecular_graphics
;
CrystalStructure (Rigaku, 2010)
and <i>ORTEPII</i> (Johnson, 1976)
;
_computing_publication_material
;
CrystalStructure (Rigaku, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS2013 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            30344
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.219
_diffrn_reflns_theta_min         5.190
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.200
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_correction_T_min  0.702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1237.20
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.19
_refine_diff_density_min         -0.24
_refine_ls_abs_structure_details
;
Flack x parameter determined using 1859 quotients [(I^+^) - (I^-^)]/[(I^+^) +
(I^-^)] (Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     362
_refine_ls_number_reflns         4750
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0435P)^2^+0.8903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0897
_reflns_number_gt                4509
_reflns_number_total             4752
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            sk3602sup1.cif
_cod_data_source_block           IV
_cod_original_cell_volume        2598.03(9)
_cod_database_code               2020210
_cod_database_fobs_code          2020210
_shelx_hkl_checksum              92546
_shelx_res_checksum              44945
_shelxl_version_number           2.014