Catalytic Conversion of a Chitin-Derived Sugar Alcohol to an Amide-Containing Isosorbide Analog
Sagawa, Takuya; Kobayashi, Hirokazu; Murata, Chinatsu; Shichibu, Yukatsu; Konishi, Katsuaki; Fukuoka, Atsushi; ACS Sustainable Chemistry & Engineering 7 (2019) 14883–; doi:10.1021/acssuschemeng.9b02985

data_4515218
_publ_section_title
;
 Catalytic Conversion of a Chitin-Derived Sugar Alcohol to an
 Amide-Containing Isosorbide Analog
;
_journal_issue                   17
_journal_name_full               'ACS Sustainable Chemistry &amp; Engineering'
_journal_page_first              14883
_journal_paper_doi               10.1021/acssuschemeng.9b02985
_journal_volume                  7
_journal_year                    2019
_chemical_absolute_configuration syn
_chemical_formula_sum            'C8 H13 N O4'
_chemical_formula_weight         187.19
_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   difmap
_cell_angle_alpha                90
_cell_angle_beta                 109.041(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.217(2)
_cell_length_b                   7.746(3)
_cell_length_c                   9.321(3)
_cell_measurement_reflns_used    124
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.0562
_cell_measurement_theta_min      4.3736
_cell_volume                     424.3(3)
_computing_cell_refinement       'APEX3 v2017.3-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 833)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0157
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2349
_diffrn_reflns_theta_full        26.71
_diffrn_reflns_theta_max         26.71
_diffrn_reflns_theta_min         2.31
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.118
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             200
_exptl_crystal_size_max          0.383
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.172
_refine_diff_density_min         -0.170
_refine_ls_abs_structure_details
;

Flack x determined using 616 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.3(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         1683
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0357
_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^)+(0.0272P)^2^+0.0883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0685
_reflns_number_gt                1552
_reflns_number_total             1683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sc9b02985_si_002.cif
_cod_data_source_block           exp832
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               4515218
_shelx_res_checksum              38956
_shelx_hkl_checksum              60900