Phosphaalkene vs. phosphinidene: the nature of the P-C bond in carbonyl-decorated carbene > PPh adducts
Roberta R. Rodrigues; Christopher L. Dorsey; Chelsee A. Arceneaux; Todd W. Hudnall; Chem.Commun. 50 (2014) 162–; doi:10.1039/c3cc45134h

data_7110172
_publ_section_title
;
 Phosphaalkene vs. phosphinidene: the nature of the P-C bond in
 carbonyl-decorated carbene > PPh adducts
;
_journal_name_full               Chem.Commun.
_journal_page_first              162
_journal_paper_doi               10.1039/c3cc45134h
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C24 H28 N2 O2 Cl - S O3 C F3'
_chemical_formula_sum            'C25 H28 Cl F3 N2 O5 S'
_chemical_formula_weight         561.00
_chemical_name_common            'DAC-Cl Triflate'
_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                 96.361(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7462(8)
_cell_length_b                   16.7795(16)
_cell_length_c                   18.8733(18)
_cell_measurement_temperature    223(2)
_cell_volume                     2752.7(5)
_computing_cell_refinement       'SHELXS-97 (Sheldrick, 1990)'
_computing_data_collection       'SHELXS-97 (Sheldrick, 1990)'
_computing_data_reduction        'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13546
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.479
_exptl_crystal_size_mid          0.354
_exptl_crystal_size_min          0.322
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         4821
_refine_ls_number_restraints     279
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.066
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0795P)^2^+1.0507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1476
_refine_ls_wR_factor_ref         0.1707
_reflns_number_gt                3075
_reflns_number_total             4821
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc45134h.txt
_cod_data_source_block           1ClOTf
_cod_original_cell_volume        2752.7(4)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7110172