Novel regio- and stereoselective phosphonyl radical addition to glycals promoted by Mn(II)-air: syntheses of 1,2-dideoxy 2-C-diphenylphosphinylglycopyranosides
Fuyi Zhang; Liming Wang; Cui Zhang; Yufen Zhao; Chem.Commun. 50 (2014) 2046–; doi:10.1039/c3cc48806c

data_7111952
_publ_section_title
;
 Novel regio- and stereoselective phosphonyl radical addition to glycals
 promoted by Mn(II)-air: syntheses of 1,2-dideoxy
 2-C-diphenylphosphinylglycopyranosides
;
_journal_name_full               Chem.Commun.
_journal_page_first              2046
_journal_paper_doi               10.1039/c3cc48806c
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C24 H27 O8 P'
_chemical_formula_weight         474.43
_space_group_IT_number           169
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 61'
_symmetry_space_group_name_H-M   'P 61'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   11.64595(8)
_cell_length_b                   11.64595(8)
_cell_length_c                   31.3727(3)
_cell_measurement_reflns_used    10855
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.8641
_cell_measurement_theta_min      2.8146
_cell_volume                     3684.96(5)
_computing_cell_refinement       'Oxford Diffraction Ltd.'
_computing_data_collection       'Oxford Diffraction Ltd.'
_computing_data_reduction        'Oxford Diffraction Ltd.'
_computing_molecular_graphics    olex2
_computing_publication_material  olex2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            19381
_diffrn_reflns_theta_full        67.22
_diffrn_reflns_theta_max         67.22
_diffrn_reflns_theta_min         4.38
_exptl_absorpt_coefficient_mu    1.382
_exptl_absorpt_correction_T_max  0.8195
_exptl_absorpt_correction_T_min  0.7696
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4240
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0668P)^2^+0.3815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.0995
_reflns_number_gt                4042
_reflns_number_total             4240
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc48806c.txt
_cod_data_source_block           20131015
_cod_original_sg_symbol_H-M      P6(1)
_cod_database_code               7111952