Sodium phosphaethynolate, Na(OCP), as a “P” transfer reagent for the synthesis of N-heterocyclic carbene supported P3 and PAsP radicals
Tondreau, Aaron M.; Benkő, Zoltán; Harmer, Jeffrey R.; Grützmacher, Hansjörg; Chemical Science 5 (2014) 1545–; doi:10.1039/c3sc53140f

data_1513841
_publ_section_title
;
 Sodium phosphaethynolate, Na(OCP), as a &#x201C;P&#x201D; transfer
 reagent for the synthesis of N-heterocyclic carbene supported P3 and PAsP
 radicals
;
_journal_issue                   4
_journal_name_full               'Chemical Science'
_journal_page_first              1545
_journal_paper_doi               10.1039/c3sc53140f
_journal_volume                  5
_journal_year                    2014
_chemical_formula_moiety         'C33 H55 N2 P7 Si2'
_chemical_formula_sum            'C72 H116 Cl N4 O3 P7 Si2'
_chemical_formula_weight         1394.11
_chemical_name_common
'di(N,N bis(2,6 diisopropylphenyl) imidazolium) chloride bis(trimethylsilyl)heptaphosphide tritetrahydrofuran'
_chemical_name_systematic
'di(N,N bis(2,6 diisopropylphenyl) imidazolium) chloride bis(trimethylsilyl)heptaphosphide tritetrahydrofuran'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 90.8200(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.3995(3)
_cell_length_b                   12.1255(2)
_cell_length_c                   29.5997(5)
_cell_measurement_reflns_used    9854
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.86
_cell_measurement_theta_min      2.24
_cell_volume                     8038.6(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep 3v2'
_computing_publication_material  'Ortep 3v2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            104129
_diffrn_reflns_theta_full        30.55
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_min         1.38
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.261
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6728
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3000
_exptl_crystal_recrystallization_method 'Saturated THF solution at  -30C'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.924
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.311
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     844
_refine_ls_number_reflns         23887
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.311
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1249
_reflns_number_gt                17711
_reflns_number_total             23887
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc53140f.txt
_cod_data_source_block           sadp21n
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1513841