Conversion of Tricoordinate to Hexacoordinate Phosphorus. Formation of a Phosphorane-Phosphatrane System1
Natalya V. Timosheva; A. Chandrasekaran; Roberta O. Day; Robert R. Holmes; Journal of the American Chemical Society 124 (2002) 7035–7040; doi:10.1021/ja012579m

data_4114869
_publ_section_title
;
 Conversion of Tricoordinate to Hexacoordinate Phosphorus. Formation of a
 Phosphorane-Phosphatrane System1
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7035
_journal_page_last               7040
_journal_paper_doi               10.1021/ja012579m
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C33 H40 N O5 P'
_chemical_formula_weight         561.63
_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                 105.1107(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.30430(10)
_cell_length_b                   14.7072(2)
_cell_length_c                   19.1561(3)
_cell_measurement_reflns_used    5349
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      4.08
_cell_volume                     3074.67(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Nonius KappaCCD area detector'
_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  0.0197
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10021
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         4.42
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_T_max  0.9560
_exptl_absorpt_correction_T_min  0.9263
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         5252
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0808P)^2^+1.5578P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1570
_reflns_number_gt                4078
_reflns_number_total             5252
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja012579m_3.cif
_cod_data_source_block           ach15p
_cod_database_code               4114869