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_4306077
_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 H48 N P'
_chemical_formula_weight         453.66
_chemical_name_common            '[{(2,4,6-C3H7)(C6H2)}2PNH2]'
_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                106.199(3)
_cell_angle_beta                 95.848(4)
_cell_angle_gamma                98.495(3)
_cell_formula_units_Z            2
_cell_length_a                   9.631(3)
_cell_length_b                   10.779(3)
_cell_length_c                   14.484(5)
_cell_measurement_reflns_used    15983
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.07
_cell_measurement_theta_min      2.43
_cell_volume                     1411.8(8)
_computing_cell_refinement       'SAINT V7.23A'
_computing_data_collection       'APEX2 v2.1-0'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0150
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            28805
_diffrn_reflns_theta_full        26.07
_diffrn_reflns_theta_max         26.07
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS-2004/1
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.067
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         5572
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0618P)^2^+1.1681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1281
_reflns_number_gt                5033
_reflns_number_total             5572
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800995h_si_001_1.cif
_cod_data_source_block           2
_cod_original_cell_volume        1411.9(8)
_cod_database_code               4306077