Preparation of a Diphosphine with Persistent Phosphinyl Radical Character in Solution: Characterization, Reactivity with O2, S8, Se, Te, and P4, and Electronic Structure Calculations
Nick A. Giffin; Arthur D. Hendsbee; Tracey L. Roemmele; Michael D. Lumsden; Cory C. Pye; Jason D. Masuda; Inorganic Chemistry 51 (2012) 11837–11850; doi:10.1021/ic301758k

data_4330924
_publ_contact_author_address
; The Maritimes Centre for Green Chemistry
  Department of Chemistry
  Saint Mary's University
  923 Robie St
  Halifax, Nova Scotia
  B3H 3C3 
  Canada
;
_publ_contact_author_email       jason.masuda@smu.ca
_publ_contact_author_name        'Jason D. Masuda'
_publ_section_title
;
 Preparation of a Diphosphine with Persistent Phosphinyl Radical Character
 in Solution: Characterization, Reactivity with O2, S8, Se, Te, and P4,
 and Electronic Structure Calculations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11837
_journal_page_last               11850
_journal_paper_doi               10.1021/ic301758k
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C52 H76 N4 P2 Se'
_chemical_formula_weight         898.07
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.160(3)
_cell_angle_beta                 84.262(3)
_cell_angle_gamma                83.823(3)
_cell_formula_units_Z            8
_cell_length_a                   20.648(5)
_cell_length_b                   23.568(6)
_cell_length_c                   24.274(6)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      2.26
_cell_volume                     10801(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0763
_diffrn_reflns_av_sigmaI/netI    0.1492
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            70274
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.789
_exptl_absorpt_correction_T_max  0.9331
_exptl_absorpt_correction_T_min  0.8217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS: Bruker: 2008)'
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_density_method    not-measured
_exptl_crystal_F_000             3840
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
The unit cell contains 5 toluene which have been treated as a diffuse 
contribution to the overall scattering without specific atom positions by 
SQUEEZE/PLATON.
;
_refine_diff_density_max         5.462
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     mutli-scan
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2189
_refine_ls_number_reflns         37157
_refine_ls_number_restraints     2112
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.1588
_refine_ls_R_factor_gt           0.0993
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1661P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2451
_refine_ls_wR_factor_ref         0.2752
_reflns_number_gt                20237
_reflns_number_total             37157
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301758k_si_001_5.cif
_cod_data_source_block           Compound_5
_cod_database_code               4330924