Deoxygenation of Some α-Dicarbonyl Compounds by Tris(diethylamino)phosphine in the Presence of Fullerene C60
Irina P. Romanova; Andrey V. Bogdanov; Vladimir F. Mironov; Gulnara R. Shaikhutdinova; Olga A. Larionova; Shamil K. Latypov; Alsu A. Balandina; Dmitry G. Yakhvarov; Aidar T. Gubaidullin; Alina F. Saifina; Oleg G. Sinyashin; Journal of Organic Chemistry 76 (2011) 2548–2557; doi:10.1021/jo102332e

data_4026193
_publ_contact_author
;
 Structure Determination:

 Dr. Aidar T. Gubaidullin
 Institute of Organic &
 Physical Chemistry
 Arbuzov Str.8
 420088 Kazan
 Russia

 Alina F. Saifina
 Institute of Organic &
 Physical Chemistry
 Arbuzov Str.8
 420088 Kazan
 Russia
;
_publ_contact_author_email       aidar@iopc.knc.ru
_publ_contact_author_fax
;
007 / 843 / 2732253
;
_publ_contact_author_phone
;   
007 / 843 / 2727573
;
_publ_section_title
;
 Deoxygenation of Some \a-Dicarbonyl Compounds by
 Tris(diethylamino)phosphine in the Presence of Fullerene C60
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2548
_journal_page_last               2557
_journal_paper_doi               10.1021/jo102332e
_journal_volume                  76
_journal_year                    2011
_chemical_formula_moiety         'C72 H6 O, 2(C S2)'
_chemical_formula_sum            'C74 H6 O S4'
_chemical_formula_weight         1039.03
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 90.794(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.491(4)
_cell_length_b                   13.676(4)
_cell_length_c                   21.937(6)
_cell_measurement_reflns_used    1166
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.17
_cell_measurement_theta_min      2.31
_cell_volume                     4047(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2439
_diffrn_reflns_av_sigmaI/netI    0.6479
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14929
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.298
_exptl_absorpt_correction_T_max  0.9794
_exptl_absorpt_correction_T_min  0.9029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
G.M. Sheldrick (1998a). SADABS v.2.01, Bruker.
Siemens Area Detector Absorption Correction Program.
Bruker AXS. Madison. Wisconsin. USA
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_description       plate
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.176
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.75(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     713
_refine_ls_number_reflns         6973
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.3680
_refine_ls_R_factor_gt           0.0826
_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^)+(0.0271P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.2354
_reflns_number_gt                1704
_reflns_number_total             6973
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo102332e_si_002.cif
_cod_data_source_block           11
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4026193