Electronic Properties of Furyl Substituents at Phosphorus and Their Influence on 31P NMR Chemical Shifts
Marco Ackermann; Aurelia Pascariu; Thomas Höcher; Hans-Ullrich Siehl; Stefan Berger; Journal of the American Chemical Society 128 (2006) 8434–8440; doi:10.1021/ja057085u

data_4110678
_publ_section_title
;
 Electronic Properties of Furyl Substituents at Phosphorus and Their
 Influence on 31P NMR Chemical Shifts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8434
_journal_page_last               8440
_journal_paper_doi               10.1021/ja057085u
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C14 H14 I O3 P'
_chemical_formula_weight         388.12
_chemical_name_common            'ethyltris(2-furyl)phosphonium iodide'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 112.290(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3806(12)
_cell_length_b                   14.7084(16)
_cell_length_c                   11.1375(12)
_cell_measurement_reflns_used    112
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.31
_cell_measurement_theta_min      2.41
_cell_volume                     1573.4(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'BRUKER SHELXTL Plus'
_computing_publication_material  'WINGX v1.64.05 (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.900
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type  'Bruker CCD'
_diffrn_measurement_method       'omega 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  0.0162
_diffrn_reflns_av_sigmaI/netI    0.0160
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9870
_diffrn_reflns_theta_full        29.31
_diffrn_reflns_theta_max         29.31
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    2.137
_exptl_absorpt_correction_T_max  0.6745
_exptl_absorpt_correction_T_min  0.4819
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_description       prism
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    calc
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3886
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0235
_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^)+(0.0351P)^2^+0.3842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0618
_reflns_number_gt                3315
_reflns_number_total             3886
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja057085usi20051026_025000.cif
_cod_data_source_block           c1481
_cod_database_code               4110678