Redox Reactions of a Stable Dialkylphosphinyl Radical
Hirakawa, Fumiya; Ichikawa, Hitomi; Ishida, Shintaro; Iwamoto, Takeaki; Organometallics 34 (2015) 2714–; doi:10.1021/acs.organomet.5b00323

data_4087563
_publ_section_title
;
 Redox Reactions of a Stable Dialkylphosphinyl Radical
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2714
_journal_paper_doi               10.1021/acs.organomet.5b00323
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C28 H64 K O6 P Si4'
_chemical_formula_weight         679.22
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                94.352(3)
_cell_angle_beta                 92.112(4)
_cell_angle_gamma                101.411(4)
_cell_formula_units_Z            2
_cell_length_a                   9.908(3)
_cell_length_b                   10.852(3)
_cell_length_c                   18.585(5)
_cell_measurement_reflns_used    4735
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.10
_cell_measurement_theta_min      2.20
_cell_volume                     1950.4(10)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0167
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9826
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.921
_exptl_absorpt_coefficient_mu    0.334
_exptl_absorpt_correction_T_max  0.9516
_exptl_absorpt_correction_T_min  0.9516
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_description       block
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.791
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         7432
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+3.5878P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1292
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5960
_reflns_number_total             7432
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00323_si_002.cif
_cod_data_source_block           compound_[K(18-c-6)]+1-
_cod_original_cell_volume        1950.3(9)
_cod_database_code               4087563
_shelx_estimated_absorpt_t_min   0.952
_shelx_estimated_absorpt_t_max   0.952
_shelxl_version_number           2014-3
_shelx_res_checksum              85706
_shelx_hkl_checksum              47194