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_4330922
_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 O3 P2'
_chemical_formula_sum            'C52 H76 N4 O3 P2'
_chemical_formula_weight         867.11
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.922(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.186(4)
_cell_length_b                   17.938(4)
_cell_length_c                   17.738(4)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    135(2)
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      2.22
_cell_volume                     5039(2)
_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      135(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0768
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            48892
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker: 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          .3426
_exptl_crystal_size_mid          .3007
_exptl_crystal_size_min          .2844
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         8872
_refine_ls_number_restraints     290
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+4.4044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1300
_reflns_number_gt                6034
_reflns_number_total             8872
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301758k_si_001_3.cif
_cod_data_source_block           Compound_3
_cod_database_code               4330922