vic-Diphosphination of Alkenes with Silylphosphine under Visible-Light-Promoted Photoredox Catalysis.
Otomura, Nobutaka; Okugawa, Yuto; Hirano, Koji; Miura, Masahiro; Organic letters 19 (2017) 4802–4805; doi:10.1021/acs.orglett.7b02223

data_1547569
_publ_section_title
;
 vic-Diphosphination of Alkenes with Silylphosphine under
 Visible-Light-Promoted Photoredox Catalysis.
;
_journal_issue                   18
_journal_name_full               'Organic letters'
_journal_page_first              4802
_journal_page_last               4805
_journal_paper_doi               10.1021/acs.orglett.7b02223
_journal_volume                  19
_journal_year                    2017
_chemical_formula_sum            'C33 H28 P2 S2'
_chemical_formula_weight         550.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                95.750(12)
_cell_angle_beta                 95.75(2)
_cell_angle_gamma                107.27(2)
_cell_formula_units_Z            2
_cell_length_a                   10.179(17)
_cell_length_b                   10.178(17)
_cell_length_c                   14.35(2)
_cell_measurement_reflns_used    4635
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.30
_cell_volume                     1399(4)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 13.653
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            8280
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.333
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.854
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.410
_exptl_crystal_size_min          0.320
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.206
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0124P)^2^+1.5001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1099
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5487
_reflns_number_total             6276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b02223_si_002.cif
_cod_data_source_block           shelxl
_cod_database_code               1547569
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.867
_shelx_estimated_absorpt_t_max   0.903
_shelx_res_checksum              39497
_shelx_hkl_checksum              66608