Exploring the reactivity of white phosphorus with electrophilic carbenes: synthesis of a P4 cage and P8 clusters
Caleb D. Martin; Cory M. Weinstein; Curtis E. Moore; Arnold L. Rheingold; Guy Bertrand; Chem.Commun. 49 (2013) 4486–; doi:10.1039/c3cc42041h

data_7109273
_publ_section_title
;
 Exploring the reactivity of white phosphorus with electrophilic carbenes:
 synthesis of a P4 cage and P8 clusters
;
_journal_name_full               Chem.Commun.
_journal_page_first              4486
_journal_paper_doi               10.1039/c3cc42041h
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C27 H26 N2 O2 P4, 1/3(C H Cl3)'
_chemical_formula_sum            'C27.33 H26.33 Cl N2 O2 P4'
_chemical_formula_weight         534.38
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            18
_cell_length_a                   34.4341(10)
_cell_length_b                   34.4341(10)
_cell_length_c                   11.4555(4)
_cell_measurement_reflns_used    38590
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.37
_cell_volume                     11763.1(6)
_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      100(2)
_diffrn_detector_area_resol_mean '512 x 512'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1185
_diffrn_reflns_av_sigmaI/netI    0.0823
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            38581
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    0.421
_exptl_absorpt_correction_T_max  0.9600
_exptl_absorpt_correction_T_min  0.9452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5004
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
SQUEEZE found 3 voids containing 2 disordered molecules of chloroform in each. Their
formula was added to the formula for the unit cell and the electron density removed.
;
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         5356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_gt           0.0645
_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^)+(0.0701P)^2^+22.8677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1495
_reflns_number_gt                3775
_reflns_number_total             5356
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc42041h.txt
_cod_data_source_block           gbcm6
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7109273