A saccharide-based crystalline sponge for hydrophilic guests
Guo-Hong Ning; Kazuki Matsumura; Yasuhide Inokuma; Makoto Fujita; Chem.Commun. 52 (2016) 7013–; doi:

data_7119149
_publ_section_title
;
 A saccharide-based crystalline sponge for hydrophilic guests
;
_journal_name_full               Chem.Commun.
_journal_page_first              7013
_journal_volume                  52
_journal_year                    2016
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C18 H25 Na O12, C3 H8 O, 0.5(H2 O)' 
_chemical_formula_sum            'C21 H34 Na O13.5'
_chemical_formula_weight         525.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-03-28 deposited with the CCDC.
2016-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.390(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.6503(15)
_cell_length_b                   24.440(6)
_cell_length_c                   14.717(3)
_cell_measurement_reflns_used    7273
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.71
_cell_measurement_theta_min      2.82
_cell_volume                     2344.9(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19037
_diffrn_reflns_point_group_measured_fraction_full 0.881
_diffrn_reflns_point_group_measured_fraction_max 0.783
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.686
_diffrn_reflns_theta_min         1.411
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6521
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       needle
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
; 
 Flack x determined using 2994 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.03(16)
_refine_ls_extinction_coef       0.0017(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         9458
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+0.4969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0912
_reflns_Friedel_coverage         0.658
_reflns_Friedel_fraction_full    0.757
_reflns_Friedel_fraction_max     0.636
_reflns_number_gt                8327
_reflns_number_total             9458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc03026b2.cif
_cod_data_source_block           p21
_cod_depositor_comments
;

2023-11-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C42 H68 Na2 O27'
_cod_original_formula_weight         1050.94
_cod_original_formula_moiety         '2(C18 H25 Na O12), 2(C3 H8 O), H2 O' 
_cod_original_formula_units_Z            2
_cod_database_code               7119149
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.977
_shelx_estimated_absorpt_t_max   0.996
_shelx_res_checksum              62854
_shelx_hkl_checksum              19817