Synthesis, Structure, and Bonding Properties of 5-Carbaphosphatranes: A New Class of Main Group Atrane
Junji Kobayashi; Kei Goto; Takayuki Kawashima; Michael W. Schmidt; Shigeru Nagase; Journal of the American Chemical Society 124 (2002) 3703–3712; doi:10.1021/ja011458j

data_4114715
_publ_contact_author_address
;
Department of Chemistry,
Graduate School of Science,
the University of Tokyo
7-3-1 Hongo, Bunkyo-ku,
Tokyo 113-0033, Japan. 
;
_publ_contact_author_email       ' takayuki@chem.s.u-tokyo.ac.jp '
_publ_contact_author_fax         ' +81-3-5800-6899 '
_publ_contact_author_name        ' Takayuki Kawashima'
_publ_contact_author_phone       ' +81-3-5841-4342 '
_publ_section_title
;
 Synthesis, Structure, and Bonding Properties of 5-Carbaphosphatranes: A
 New Class of Main Group Atrane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3703
_journal_page_last               3712
_journal_paper_doi               10.1021/ja011458j
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C31 H37 O3 P'
_chemical_formula_weight         488.58
_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                 93.842(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.9630(10)
_cell_length_b                   11.2780(10)
_cell_length_c                   15.2690(10)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    123.2
_cell_measurement_theta_max      0.0
_cell_measurement_theta_min      0.0
_cell_volume                     2742.7(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 0.010000
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Mac Science DIP2030 Image Plate'
_diffrn_measurement_method       \w
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4985
_diffrn_reflns_theta_full        25.61
_diffrn_reflns_theta_max         25.61
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_T_max  0.9622
_exptl_absorpt_correction_T_min  0.9381
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.176
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         4985
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0793P)^2^+1.7661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1435
_refine_ls_wR_factor_ref         0.1483
_reflns_number_gt                4242
_reflns_number_total             4985
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja011458j.cif
_cod_data_source_block           C31H37O3P
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               4114715