Functionalization of Aminophosphanes: Synthesis and X-Ray Crystal Structure of Novel Dilithium and Trilithium Complexes Containing Silicon-Fused Heteronuclear SiN2PLi Five-Membered Rings
Anukul Jana; Gerald Schwab; Herbert W. Roesky; Dietmar Stalke; Inorganic Chemistry 47 (2008) 8990–8994; doi:10.1021/ic800995h

data_4306078
_publ_contact_author             'Prof. Dr. Herbert W. Roesky'
_publ_contact_author_email       hroesky@gwdg.de
_publ_section_title
;
Functionalization of Aminophosphanes: Synthesis and X-Ray Crystal Structure
of Novel Dilithium and Trilithium Complexes Containing Silicon-Fused
Heteronuclear SiN2PLi Five-Membered Rings
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8990
_journal_page_last               8994
_journal_paper_doi               10.1021/ic800995h
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C30 H66 Li2 N2 O3 P2 Si'
_chemical_formula_weight         606.76
_chemical_name_common            '[Me2Si(NPtBu2)2Li2(THF)3]'
_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-97
_cell_angle_alpha                87.7880(10)
_cell_angle_beta                 72.9230(10)
_cell_angle_gamma                73.4670(10)
_cell_formula_units_Z            4
_cell_length_a                   11.7583(6)
_cell_length_b                   18.0055(9)
_cell_length_c                   19.3288(10)
_cell_measurement_reflns_used    21262
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      2.36
_cell_volume                     3745.5(3)
_computing_cell_refinement       'SAINT V7.23A'
_computing_data_collection       'APEX2 v2.0-2'
_computing_data_reduction        'SAINT V7.23A'
_computing_molecular_graphics    'XP in SHELXTL ver. 6.12'
_computing_publication_material  'XP in SHELXTL ver. 6.12'
_computing_structure_refinement  'SHELXL in SHELXTL ver. 6.12'
_computing_structure_solution    'SHELXS in SHELXTL ver. 6.12'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker Smart Apex II with D8-Goniometer'
_diffrn_measurement_method       'omega 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  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            59281
_diffrn_reflns_theta_full        27.92
_diffrn_reflns_theta_max         27.92
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS-2004/1
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     818
_refine_ls_number_reflns         16997
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+1.6032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1197
_reflns_number_gt                13606
_reflns_number_total             16997
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800995h_si_001_2.cif
_cod_data_source_block           6
_cod_database_code               4306078