Strong evidence for stereoselective 1,3-additions of transient nitrilium phosphane-ylide complexes: synthesis of the first 1-aza-3-phosphabuta-1,3-diene complexes
Streubel, Rainer; Schiemann, Udo; Hoffmann, Nils; Jones, Peter G.; Chemical Communications  (2001) 1334–; doi:10.1039/b102250b

data_7114734
_publ_section_title
;
 Strong evidence for stereoselective 1,3-additions of transient nitrilium
 phosphane-ylide complexes: synthesis of the first
 1-aza-3-phosphabuta-1,3-diene complexes
;
_journal_issue                   15
_journal_name_full               'Chemical Communications'
_journal_page_first              1334
_journal_paper_doi               10.1039/b102250b
_journal_year                    2001
_chemical_formula_sum            'C25 H46 Cl N2 O5 P2 Si4 W'
_chemical_formula_weight         848.24
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.16(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.854(2)
_cell_length_b                   11.864(2)
_cell_length_c                   29.372(4)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     3772.3(11)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'Stoe REDU4'
_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_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Stoe STADI-4'
_diffrn_measurement_method       \w-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  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            9019
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         3.21
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.378
_exptl_absorpt_correction_T_max  0.797
_exptl_absorpt_correction_T_min  0.716
_exptl_absorpt_correction_type   Psi-scans
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'multifaceted, equidimensional'
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.163
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         6639
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+3.9743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0724
_reflns_number_gt                5607
_reflns_number_total             6639
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b102250b.txt
_cod_data_source_block           rapyd
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7114734