Crystal structure of the acyclic form of 1-deoxy-1-[(4-methoxyphenyl)(methyl)amino]-<small>D</small>-fructose
Mossine, Valeri V.; Barnes, Charles L.; Mawhinney, Thomas P.; Acta Crystallographica Section E 74 (2018) 127–132; doi:10.1107/S2056989018000099

data_2242311
_publ_section_title
;
 Crystal structure of the acyclic form of
 1-deoxy-1-[(4-methoxyphenyl)(methyl)amino]-<small>D</small>-fructose
;
_journal_coeditor_code           QM2121
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              127
_journal_page_last               132
_journal_paper_doi               10.1107/S2056989018000099
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C14 H21 N O6'
_chemical_formula_moiety         'C14 H21 N O6'
_chemical_formula_sum            'C14 H21 N O6'
_chemical_formula_weight         299.32
_chemical_name_systematic
;
1-Deoxy-1-(<i>N</i>-methyl-<i>p</i>-methoxyphenylamino)-<i>D</i>-fructose
;
_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-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 98.3820(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.8002(15)
_cell_length_b                   5.1439(7)
_cell_length_c                   13.3931(19)
_cell_measurement_reflns_used    3774
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.8
_cell_measurement_theta_min      2.6
_cell_volume                     736.11(18)
_computing_cell_refinement
;
SAINT (Bruker, 1998)
;
_computing_data_collection
;
SMART (Bruker, 1998)
;
_computing_data_reduction
;
SAINT (Bruker, 1998)
;
_computing_molecular_graphics
;
X-Seed (Barbour, 2001) and Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
<i>CIFTAB</i> (Sheldrick, 2008) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2017/1</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8031
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.906
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick (2003)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       Prism
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.150
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1149 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al</i>., 2013)
;
_refine_ls_abs_structure_Flack   0.3(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2993
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0313
_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/[\s^2^(Fo^2^)+(0.0443P)^2^+0.0803P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0815
_reflns_number_gt                2788
_reflns_number_total             2993
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            qm2121sup1.cif
_cod_data_source_block           I
_cod_database_code               2242311
_cod_database_fobs_code          2242311
_shelx_estimated_absorpt_t_min   0.964
_shelx_estimated_absorpt_t_max   0.987
_shelx_hkl_checksum              57816
_shelx_res_checksum              87336