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_4306079
_publ_contact_author             'Prof. Dr. Herbert 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            'C37 H87 Li3 N3 O3 P3 Si'
_chemical_formula_weight         763.92
_chemical_name_common            '[MeSi(NPtBu2)3Li3(Et2O)3]'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1371(7)
_cell_length_b                   17.0011(10)
_cell_length_c                   25.8204(16)
_cell_measurement_reflns_used    13609
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.87
_cell_measurement_theta_min      2.32
_cell_volume                     4888.9(5)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            46209
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.179
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS-2004/1
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.038
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.157
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         9632
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0492
_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^)+(0.1150P)^2^+0.3242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1573
_reflns_number_gt                8591
_reflns_number_total             9632
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800995h_si_001_3.cif
_cod_data_source_block           7
_cod_database_code               4306079