Stable Tetravalent Phosphonium Enolate Zwitterions
Xue-Feng Zhu; Christopher E. Henry; Ohyun Kwon; Journal of the American Chemical Society 129 (2007) 6722–6723; doi:10.1021/ja071990s

data_4109465
_publ_section_title
;
 Stable Tetravalent Phosphonium Enolate Zwitterions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6722
_journal_page_last               6723
_journal_paper_doi               10.1021/ja071990s
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         '2(C29 H41 O3 P), 0.5(C6 H12) '
_chemical_formula_sum            'C61 H88 O6 P2'
_chemical_formula_weight         979.25
_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                81.392(2)
_cell_angle_beta                 84.224(2)
_cell_angle_gamma                80.184(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4874(16)
_cell_length_b                   13.386(2)
_cell_length_c                   20.289(3)
_cell_measurement_reflns_used    9746
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.31
_cell_measurement_theta_min      3.98
_cell_volume                     2766.7(7)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scan'
_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  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21588
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         26.34
_diffrn_reflns_theta_min         3.77
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  0.9936
_exptl_absorpt_correction_T_min  0.9120
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Bruker)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_description       cut-plate
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         11069
_refine_ls_number_restraints     427
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0642P)^2^+1.0647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1217
_refine_ls_wR_factor_ref         0.1356
_reflns_number_gt                8227
_reflns_number_total             11069
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja071990ssi20070321_024019.cif
_cod_data_source_block           kw606s
_cod_database_code               4109465