The synthesis and molecular structures of the crystalline 1-aza-2-phospha(V)allyllithium compounds [Li(LL ′ )(OEt2)2] and [Li(LL ′ )]2 [LL ′ = CH(SiMe3)P(Ph)2NSiMe3] and the preparation and characterisation of the new phosphinimines CH(R1)(R2)P(Ph)2 NSiMe3 [R1 = R2 = SiMe3; R1 = H, R2 = Si(Me)2NEt2] †
Hitchcock, Peter B.; Lappert, Michael F.; Uiterweerd, Patrick G. H.; Wang, Zhong-Xia; Journal of the Chemical Society, Dalton Transactions  (1999) 3413–; doi:10.1039/a905464b

data_7027678
_publ_section_title
;
 The synthesis and molecular structures of the crystalline
 1-aza-2-phospha(V)allyllithium compounds
 [Li(LL&#x200A;&#x2032;&#x200A;)(OEt2)2] and
 [Li(LL&#x200A;&#x2032;&#x200A;)]2
 [LL&#x200A;&#x2032;&#x2005;=&#x2005;CH(SiMe3)P(Ph)2&#xE006;NSiMe3] and
 the preparation and characterisation of the new phosphinimines
 CH(R1)(R2)P(Ph)2&#xE006; NSiMe3
 [R1&#x2005;=&#x2005;R2&#x2005;=&#x2005;SiMe3; R1&#x2005;=&#x2005;H,
 R2&#x2005;=&#x2005;Si(Me)2NEt2]&#x200A;&#x2020;
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_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3413
_journal_paper_doi               10.1039/a905464b
_journal_year                    1999
_chemical_formula_structural     '[{Li(Me3SiNPPh2CHSiMe3)}2]'
_chemical_formula_sum            'C38 H58 Li2 N2 P2 Si4'
_chemical_formula_weight         731.04
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                100.750(10)
_cell_angle_beta                 94.930(10)
_cell_angle_gamma                108.830(10)
_cell_formula_units_Z            2
_cell_length_a                   10.988(2)
_cell_length_b                   11.478(2)
_cell_length_c                   18.753(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     2171.9(7)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_molecular_graphics    'CAMERON (Watkin and Pearce,1993)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       ' Enraf-Nonius CAD4'
_diffrn_measurement_method       \w--2\q
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1017
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7615
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.237
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.037
_refine_ls_goodness_of_fit_obs   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         7614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_restrained_S_obs      1.074
_refine_ls_R_factor_all          0.1154
_refine_ls_R_factor_obs          0.0638
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0780P)^2^+0.1748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1762
_refine_ls_wR_factor_obs         0.1434
_reflns_number_observed          4860
_reflns_number_total             7615
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            905464bsup1.cif
_cod_data_source_block           complex7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0780P)^2^+0.1748P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0780P)^2^+0.1748P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2171.9(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7027678