Selective synthesis of 3-deoxy-5-hydroxy-1-amino-carbasugars as potential α-glucosidase inhibitors.
Jiang, Chunfeng; Liu, Quan; Liu, Jiaming; Liu, Kaixuan; Tian, Liangliang; Duan, Mingfei; Wang, Ying; Shen, Zhufang; Xu, Youjun; Organic & biomolecular chemistry 17 (2019) 5381–5391; doi:10.1039/c9ob00762h

data_7156836
_publ_section_title
;
 Selective synthesis of 3-deoxy-5-hydroxy-1-amino-carbasugars as potential
 \a-glucosidase inhibitors.
;
_journal_issue                   21
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              5381
_journal_page_last               5391
_journal_paper_doi               10.1039/c9ob00762h
_journal_volume                  17
_journal_year                    2019
_chemical_absolute_configuration unk
_chemical_formula_sum            'C36 H41 N O4'
_chemical_formula_weight         551.70
_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
;
2019-03-04 deposited with the CCDC.    2019-05-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.625(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.676(4)
_cell_length_b                   5.9027(13)
_cell_length_c                   16.875(4)
_cell_measurement_reflns_used    748
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      18.77
_cell_measurement_theta_min      2.49
_cell_volume                     1510.9(6)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0870
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7530
_diffrn_reflns_point_group_measured_fraction_full 0.918
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        24.943
_diffrn_reflns_theta_max         24.943
_diffrn_reflns_theta_min         1.247
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       Block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_transmission_factor_max   0.864
_exptl_transmission_factor_min   0.864
_refine_diff_density_max         0.134
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
;
 Flack x determined using 754 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -3.2(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         4835
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0492P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1326
_reflns_Friedel_coverage         0.663
_reflns_Friedel_fraction_full    0.820
_reflns_Friedel_fraction_max     0.820
_reflns_number_gt                2806
_reflns_number_total             4835
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ob00762h2.cif
_cod_data_source_block           1_a
_cod_depositor_comments          'Adding full bibliography for 7156836.cif.'
_cod_original_cell_volume        1510.8(6)
_cod_database_code               7156836
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.983
_shelx_estimated_absorpt_t_max   0.986
_shelx_res_checksum              64196