Synthesis, structure and isomerization of arylphosphoranes with anti-apicophilic bonding modes using a novel bidentate ligand with two C2F5 groups
Jiang, Xin-Dong; Matsukawa, Shiro; Yamamoto, Yohsuke; Dalton Transactions  (2008) 3678–3687; doi:10.1039/b802947d

data_7004134
_publ_section_title
;
 Synthesis, structure and isomerization of arylphosphoranes with
 anti-apicophilic bonding modes using a novel bidentate ligand with two
 C2F5 groups
;
_journal_issue                   28
_journal_name_full               'Dalton Transactions'
_journal_page_first              3678
_journal_page_last               3687
_journal_paper_doi               10.1039/b802947d
_journal_year                    2008
_chemical_formula_sum            'C31 H19 F20 O2 P'
_chemical_formula_weight         834.43
_chemical_melting_point          190
_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                86.9670(10)
_cell_angle_beta                 87.4260(10)
_cell_angle_gamma                68.0970(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9960(2)
_cell_length_b                   11.9660(3)
_cell_length_c                   14.1910(3)
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      1.4
_cell_volume                     1572.10(6)
_computing_cell_refinement       'HKL(Otwinowski, 1997)'
_computing_data_collection       'HKL(Otwinowski, 1997)'
_computing_data_reduction        'HKL(Otwinowski, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'MacScience DIP2030 Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6952
_diffrn_reflns_theta_full        27.96
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.238
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         6952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0759P)^2^+0.7425P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1256
_reflns_number_gt                6630
_reflns_number_total             6952
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b802947d.txt
_cod_data_source_block           compound13e
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7004134