Photochemically generated nitrilium phosphane-ylid tungsten complexes and their reactivity towards alkyne and nitrile derivatives
Streubel, Rainer; Wilkens, Hendrik; Jones, Peter G.; Chemical Communications  (1999) 2127–; doi:10.1039/a905752h

data_7115222
_publ_section_title
;
 Photochemically generated nitrilium phosphane-ylid tungsten complexes and
 their reactivity towards alkyne and nitrile derivatives
;
_journal_issue                   20
_journal_name_full               'Chemical Communications'
_journal_page_first              2127
_journal_paper_doi               10.1039/a905752h
_journal_year                    1999
_chemical_formula_sum            'C23 H29 N2 O7 P Si2 W'
_chemical_formula_weight         716.48
_chemical_name_systematic
;
 ?
;
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.915(3)
_cell_angle_beta                 82.215(3)
_cell_angle_gamma                75.406(3)
_cell_formula_units_Z            2
_cell_length_a                   10.5466(10)
_cell_length_b                   10.7010(11)
_cell_length_c                   13.8717(14)
_cell_measurement_reflns_used    6523
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     1484.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       \w-scan
_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  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15748
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    4.065
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.142
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         7327
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0206
_refine_ls_R_factor_gt           0.0186
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+0.2143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0433
_refine_ls_wR_factor_ref         0.0438
_reflns_number_gt                6896
_reflns_number_total             7327
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            905752h.txt
_cod_data_source_block           wilkum
_cod_database_code               7115222