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_4110679
_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            'C37 H28 I2 O P2'
_chemical_formula_weight         804.33
_chemical_name_common            'ethyl(2-furyl)diphenylphosphonium iodide'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_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                69.132(3)
_cell_angle_beta                 80.813(3)
_cell_angle_gamma                83.241(3)
_cell_formula_units_Z            2
_cell_length_a                   10.2558(16)
_cell_length_b                   12.515(2)
_cell_length_c                   15.051(2)
_cell_measurement_reflns_used    146
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      29.62
_cell_measurement_theta_min      1.46
_cell_volume                     1778.1(5)
_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 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.0137
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13956
_diffrn_reflns_theta_full        29.62
_diffrn_reflns_theta_max         29.62
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    1.885
_exptl_absorpt_correction_T_max  0.7043
_exptl_absorpt_correction_T_min  0.6017
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       platelet
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.178
_refine_diff_density_min         -1.101
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    calculated
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         9753
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0476P)^2^+4.0324P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1295
_reflns_number_gt                7654
_reflns_number_total             9753
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja057085usi20051026_025032.cif
_cod_data_source_block           c1408
_cod_database_code               4110679