Photooxidation of mixed aryl and biarylphosphines.
Zhang, Dong; Celaje, Jeff A.; Agua, Alon; Doan, Chad; Stewart, Timothy; Bau, Robert; Selke, Matthias; Organic letters 12 (2010) 3100–3103; doi:10.1021/ol101122u

data_1503056
_publ_section_title
;
 Photooxidation of mixed aryl and biarylphosphines.
;
_journal_issue                   13
_journal_name_full               'Organic letters'
_journal_page_first              3100
_journal_page_last               3103
_journal_paper_doi               10.1021/ol101122u
_journal_volume                  12
_journal_year                    2010
_chemical_formula_sum            'C20 H19 O4 P'
_chemical_formula_weight         354.32
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 125.364(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.553(18)
_cell_length_b                   8.908(6)
_cell_length_c                   17.380(12)
_cell_measurement_reflns_used    8180
_cell_measurement_temperature    138(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      1.81
_cell_volume                     3479(4)
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      138(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.0642
_diffrn_reflns_av_sigmaI/netI    0.0760
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8180
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.180
_exptl_absorpt_correction_T_max  0.9770
_exptl_absorpt_correction_T_min  0.9267
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing,R.H.,Acta Crystallogr.1995,A51,33'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_meas      calculated
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3204
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0640
_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^)+(0.1170P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1649
_refine_ls_wR_factor_ref         0.1898
_reflns_number_gt                1967
_reflns_number_total             3204
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol101122u_si_002.cif
_cod_data_source_block           ptriom
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1503056