Synthesis and structural characterisation of the first tris(diacylpnictido)phosphines, P[E{C(O)R}2]3, E = P or As, R = But or Ph
Jones, Cameron; Junk, Peter C.; Williams, Thomas C.; Journal of the Chemical Society, Dalton Transactions  (2002) 2417–; doi:10.1039/b203709m

data_7702820
_publ_section_title
;
 Synthesis and structural characterisation of the first
 tris(diacylpnictido)phosphines, P[E{C(O)R}2]3, E = P or As, R = But or Ph
;
_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2417
_journal_paper_doi               10.1039/b203709m
_journal_year                    2002
_chemical_formula_sum            'C46 H40 O7 P4'
_chemical_formula_weight         828.66
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                97.21(3)
_cell_angle_beta                 112.28(3)
_cell_angle_gamma                116.39(3)
_cell_formula_units_Z            2
_cell_length_a                   12.930(3)
_cell_length_b                   14.012(3)
_cell_length_c                   14.939(3)
_cell_measurement_temperature    150(2)
_cell_volume                     2097.6(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.0676
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41030
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    0.231
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   'Sortav (Blessing)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         9595
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0324P)^2^+0.9508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0956
_reflns_number_gt                7499
_reflns_number_total             9595
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b203709m.txt
_cod_data_source_block           compound_6
_cod_original_cell_volume        2097.8(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7702820