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_7004128
_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            'C28 H13 F20 O2 P'
_chemical_formula_weight         792.35
_chemical_melting_point          115
_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                 96.6920(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.6370(2)
_cell_length_b                   37.4070(13)
_cell_length_c                   16.1350(8)
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.4
_cell_volume                     5776.9(4)
_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 0.657
_diffrn_measured_fraction_theta_max 0.657
_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    0.0615
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9091
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    0.254
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.776
_refine_diff_density_min         -1.280
_refine_diff_density_rms         0.291
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         9091
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.1330
_refine_ls_R_factor_gt           0.0839
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1822P)^2^+3.8368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2364
_refine_ls_wR_factor_ref         0.2914
_reflns_number_gt                5924
_reflns_number_total             9091
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b802947d.txt
_cod_data_source_block           compound12a
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7004128