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_4110680
_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            'C16 H16 I O2 P'
_chemical_formula_weight         398.16
_chemical_name_common            'ethylbis(2-furyl)phenylphosphonium iodide'
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.283(2)
_cell_length_b                   11.5693(17)
_cell_length_c                   20.138(3)
_cell_measurement_reflns_used    138
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.29
_cell_measurement_theta_min      1.76
_cell_volume                     3327.7(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL PLUS'
_computing_publication_material  'Bruker SHELXTL PLUS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXs-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_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  0.0151
_diffrn_reflns_av_sigmaI/netI    0.0139
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20355
_diffrn_reflns_theta_full        29.29
_diffrn_reflns_theta_max         29.29
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    2.019
_exptl_absorpt_correction_T_max  0.6882
_exptl_absorpt_correction_T_min  0.4989
_exptl_absorpt_correction_type   SASABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    calculated
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         7767
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+2.4817P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0731
_reflns_number_gt                7146
_reflns_number_total             7767
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja057085usi20051026_025101.cif
_cod_data_source_block           c1548
_cod_original_cell_volume        3327.8(8)
_cod_database_code               4110680