Synthesis, Structure, and Reactivity of N-Benzoyl Iminophosphoranes Ortho Lithiated at the Benzoyl Group
David Aguilar; Ignacio Fernández; Luciano Cuesta; Víctor Yañez-Rodríguez; Tatiana Soler; Rafael Navarro; Esteban P. Urriolabeitia; Fernando López Ortiz; Journal of Organic Chemistry 75 (2010) 6452–6462; doi:10.1021/jo101151s

data_4025694
_publ_section_title
;
 Synthesis, Structure, and Reactivity of N-Benzoyl Iminophosphoranes Ortho
 Lithiated at the Benzoyl Group
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6452
_journal_page_last               6462
_journal_paper_doi               10.1021/jo101151s
_journal_volume                  75
_journal_year                    2010
_chemical_formula_moiety         'C28 H28 N O P Sn'
_chemical_formula_sum            'C28 H28 N O P Sn'
_chemical_formula_weight         544.17
_chemical_name_systematic
; 
 ? 
;
_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                 105.175(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7495(11)
_cell_length_b                   24.5625(18)
_cell_length_c                   8.8304(6)
_cell_measurement_reflns_used    1169
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      16.2531
_cell_measurement_theta_min      2.9045
_cell_volume                     2668.9(4)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.19 (release 28-02-2008 CrysAlis171 .NET)
(compiled Feb 28 2008,12:10:31)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.19 (release 28-02-2008 CrysAlis171 .NET)
(compiled Feb 28 2008,12:10:31)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.19 (release 28-02-2008 CrysAlis171 .NET)
(compiled Feb 28 2008,12:10:31)
;
_computing_molecular_graphics
;
SHELXTL  Rel. 6.12/V (Sheldrick, Acta Cryst. 2008, A64, 112-122)
;
_computing_publication_material
;
SHELX-97 (Sheldrick, Acta Cryst. 2008, A64, 112-122)' 
;
_computing_structure_refinement
;
SHELXL-97 (Sheldrick, Acta Cryst. 2008, A64, 112-122) 
;
_computing_structure_solution
;
SHELXL-97 (Sheldrick, Acta Cryst. 2008, A64, 112-122) 
;
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 16.3990
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur2'
_diffrn_measurement_method       '\w and \f scans'
_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  0.2490
_diffrn_reflns_av_sigmaI/netI    0.3996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            24496
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    1.036
_exptl_absorpt_correction_T_max  0.9897
_exptl_absorpt_correction_T_min  0.8365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.19 (release 28-02-2008 CrysAlis171 .NET)
(compiled Feb 28 2008,12:10:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         4698
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.2341
_refine_ls_R_factor_gt           0.0787
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0130P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1225
_reflns_number_gt                1523
_reflns_number_total             4698
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo101151s_si_002.cif
_cod_data_source_block           sq
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4025694