Towards the complete synthetic O-antigen of Vibrio cholerae O1, serotype inaba: improved synthesis of the conjugation-ready upstream terminal hexasaccharide determinant
Mukherjee, Mana Mohan; Xu, Peng; Stevens, Edwin D.; Kováč, Pavol; RSC Advances 9 (2019) 36440–; doi:10.1039/C9RA08232H

data_7235004
_publ_section_title
;
 Towards the complete synthetic O-antigen of Vibrio cholerae O1, serotype
 inaba: improved synthesis of the conjugation-ready upstream terminal
 hexasaccharide determinant
;
_journal_issue                   62
_journal_name_full               'RSC Advances'
_journal_page_first              36440
_journal_paper_doi               10.1039/C9RA08232H
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C44 H59 N9 O10 Si'
_chemical_formula_sum            'C44 H59 N9 O10 Si'
_chemical_formula_weight         902.09
_chemical_melting_point          352
_chemical_name_systematic
2-(trimethylsilyl)ethyl-4-azido-3-O-benzyl-4,6-dideoxy-alpha-D-mannopyranosyl-(1->2)-4-azido-3-O-benzyl-4,6-dideoxy-alpha-D-mannopyranosyl-(1->2)-4-azido-3-O-benzyl-4,6-dideoxy-alpha-D-mannopyranoside
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-07-10 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.067(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.530(3)
_cell_length_b                   16.862(4)
_cell_length_c                   25.697(6)
_cell_measurement_reflns_used    51631
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      34.607
_cell_measurement_theta_min      2.209
_cell_volume                     4947(2)
_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-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.969
_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  0.0362
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            72975
_diffrn_reflns_point_group_measured_fraction_full 0.942
_diffrn_reflns_point_group_measured_fraction_max 0.772
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         47.954
_diffrn_reflns_theta_min         1.449
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_T_max  0.7470
_exptl_absorpt_correction_T_min  0.7038
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_description       needle
_exptl_crystal_F_000             1920
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ethanol'
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.376
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 17080 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1167
_refine_ls_number_reflns         72975
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+0.3909P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1171
_reflns_Friedel_coverage         0.560
_reflns_Friedel_fraction_full    0.881
_reflns_Friedel_fraction_max     0.566
_reflns_number_gt                56235
_reflns_number_total             72975
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra08232h2.cif
_cod_data_source_block           Kovac3M_0m_a
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7235004
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.958
_shelx_estimated_absorpt_t_max   0.968
_shelx_res_checksum              10222