Photo-mediated synthesis of 1,2-dideoxy-2-phosphinylated carbohydrates from glycals: the reduction of glycosyl radicals to glycosyl anions
Li, Hai; Yu, Kai-Cheng; Su, Jia-Kun; Ouyang, Wei; Fan, Nai-Li; Hu, Xiang-Guo; Green Chemistry 24 (2022) 8280–8291; doi:10.1039/D2GC01513G

data_7245196
_publ_section_title
;
 Photo-mediated synthesis of 1,2-dideoxy-2-phosphinylated carbohydrates
 from glycals: the reduction of glycosyl radicals to glycosyl anions
;
_journal_issue                   21
_journal_name_full               'Green Chemistry'
_journal_page_first              8280
_journal_page_last               8291
_journal_paper_doi               10.1039/D2GC01513G
_journal_volume                  24
_journal_year                    2022
_chemical_absolute_configuration s
_chemical_formula_moiety         C23H27O6P
_chemical_formula_sum            'C23 H27 O6 P'
_chemical_formula_weight         430.41
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_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-11-20 deposited with the CCDC.	2022-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
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_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.88
_cell_measurement_theta_min      2.19
_cell_volume                     4322.2(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
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_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
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_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0434
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_h_max       11
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_diffrn_reflns_limit_k_max       11
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_diffrn_reflns_number            33464
_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.496
_diffrn_reflns_theta_min         2.187
_exptl_absorpt_coefficient_mu    0.164
_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
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_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_exptl_transmission_factor_max   1.0000
_exptl_transmission_factor_min   0.6181
_refine_diff_density_max         0.196
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_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   -0.01(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         4035
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0262P)^2^+2.5918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.0988
_reflns_Friedel_coverage         0.636
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3724
_reflns_number_total             4035
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2gc01513g2.cif
_cod_data_source_block           A
_cod_depositor_comments
'Adding full bibliography for 7245196--7245197.cif.'
_cod_database_code               7245196
_shelx_shelxl_version_number     2014/7
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_shelx_estimated_absorpt_t_max   0.976
_shelx_res_checksum              99953