2,3-Di-O-picolinyl building blocks as glycosyl donors with switchable stereoselectivity.
Yasomanee, Jagodige P.; Parameswar, Archana R.; Pornsuriyasak, Papapida; Rath, Nigam P.; Demchenko, Alexei V.; Organic & biomolecular chemistry 14 (2016) 3159–3169; doi:10.1039/c6ob00107f

data_7154973
_publ_section_title
;
 2,3-Di-O-picolinyl building blocks as glycosyl donors with switchable
 stereoselectivity.
;
_journal_issue                   11
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              3159
_journal_page_last               3169
_journal_paper_doi               10.1039/c6ob00107f
_journal_volume                  14
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C27 H30 Br2 N2 O5 Pd S'
_chemical_formula_sum            'C27 H30 Br2 N2 O5 Pd S'
_chemical_formula_weight         760.81
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2014-09-02 deposited with the CCDC.
2016-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.222(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.3369(4)
_cell_length_b                   20.8048(10)
_cell_length_c                   8.5721(4)
_cell_measurement_reflns_used    9134
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.05
_cell_measurement_theta_min      2.57
_cell_volume                     1376.38(12)
_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 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_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  0.0407
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            47319
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.634
_diffrn_reflns_theta_min         1.958
_exptl_absorpt_coefficient_mu    3.694
_exptl_absorpt_correction_T_max  0.4305
_exptl_absorpt_correction_T_min  0.3967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs v2014/3'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.266
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.157
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
; 
 Flack x determined using 2661 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.002(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         6319
_refine_ls_number_restraints     151
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0262
_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^)+(0.0306P)^2^+0.9116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0592
_reflns_Friedel_coverage         0.935
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                5897
_reflns_number_total             6319
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ob00107f2.cif
_cod_data_source_block           d13811
_cod_depositor_comments          'Adding full bibliography for 7154973.cif.'
_cod_database_code               7154973
_shelx_estimated_absorpt_t_min   0.440
_shelx_estimated_absorpt_t_max   0.595
_shelxl_version_number           2014-3
_shelx_res_checksum              40511