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_4109466
_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         'C24 H24 N O3 P, H2 O'
_chemical_formula_sum            'C24 H26 N O4 P'
_chemical_formula_weight         423.43
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 113.583(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.996(4)
_cell_length_b                   10.762(2)
_cell_length_c                   23.331(5)
_cell_measurement_reflns_used    6630
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      3.78
_cell_volume                     4371.3(15)
_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 0.989
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega and phi 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  0.0516
_diffrn_reflns_av_sigmaI/netI    0.0587
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            42433
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         30.74
_diffrn_reflns_theta_min         3.76
_exptl_absorpt_coefficient_mu    0.156
_exptl_absorpt_correction_T_max  0.9846
_exptl_absorpt_correction_T_min  0.9105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs (Bruker)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_description       cut-plate
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         12666
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0402P)^2^+2.0918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1104
_reflns_number_gt                8859
_reflns_number_total             12666
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja071990ssi20070321_024041.cif
_cod_data_source_block           kw806
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4109466