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_4330927
_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_moiety         'C52 H76 N4 P6'
_chemical_formula_sum            'C52 H76 N4 P6'
_chemical_formula_weight         942.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.954(3)
_cell_length_b                   12.954(3)
_cell_length_c                   35.031(12)
_cell_measurement_reflns_used    9033
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.87
_cell_measurement_theta_min      2.22
_cell_volume                     5878(3)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0562
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            71003
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.217
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          .3226
_exptl_crystal_size_mid          .3014
_exptl_crystal_size_min          .2821
_platon_squeeze_details
;
The unit cell contains 4 toluene molecules which have been treated as a diffuse 
contribution to the overall scattering without specific atom positions by 
SQUEEZE/PLATON.
;
_refine_diff_density_max         0.871
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 'Flack (1983), 3049 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.02(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         7296
_refine_ls_number_restraints     2064
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0631
_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^)+(0.0958P)^2^+4.9800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1631
_refine_ls_wR_factor_ref         0.1689
_reflns_number_gt                6406
_reflns_number_total             7296
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301758k_si_001_8.cif
_cod_data_source_block           Compound_8
_cod_original_cell_volume        5878.4(28)
_cod_database_code               4330927