The difference between the reactivity of a terminal phosphinidene and a Li/Cl phosphiniodenoid complex in cycloaddition chemistry – in the importance of template-induced selectivity
Rainer Streubel; Jose Manuel Villalba Franco; Gregor Schnakenburg; Arturo Espinosa Ferao; Chem.Commun. 48 (2012) 5986–; doi:10.1039/c2cc31851b

data_7107824
_publ_section_title
;
 The difference between the reactivity of a terminal phosphinidene and a
 Li/Cl phosphiniodenoid complex in cycloaddition chemistry -- in the
 importance of template-induced selectivity
;
_journal_name_full               Chem.Commun.
_journal_page_first              5986
_journal_paper_doi               10.1039/c2cc31851b
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C18 H26 N O5 P S Si2 W'
_chemical_formula_sum            'C18 H26 N O5 P S Si2 W'
_chemical_formula_weight         639.46
_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                72.585(2)
_cell_angle_beta                 74.551(3)
_cell_angle_gamma                77.633(3)
_cell_formula_units_Z            2
_cell_length_a                   9.2854(4)
_cell_length_b                   9.7913(5)
_cell_length_c                   15.3748(7)
_cell_measurement_reflns_used    4617
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      1.00
_cell_volume                     1271.74(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0913
_diffrn_reflns_av_sigmaI/netI    0.0962
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16486
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    4.807
_exptl_absorpt_correction_T_max  0.6997
_exptl_absorpt_correction_T_min  0.2494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.704
_refine_diff_density_min         -2.811
_refine_diff_density_rms         0.227
_refine_ls_extinction_coef       0.0015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5984
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0239P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0832
_reflns_number_gt                4775
_reflns_number_total             5984
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc31851b.txt
_cod_data_source_block           4
_cod_original_cell_volume        1271.75(10)
_cod_database_code               7107824