Synthesis and Structural Characterization of Metalated 1,8-Bis(silylamino)naphthalene Derivatives
Christian H. Galka; Dominique J. M. Trösch; Ina Rüdenauer; Lutz H. Gade; Ian Scowen; Mary McPartlin; Inorganic Chemistry 39 (2000) 4615–4620; doi:10.1021/ic000296+

data_4327620
_publ_contact_author
; 
        Prof. Dr. Lutz H. Gade 
        Laboratoire de Chimie Organometallique et de Catalyse (UMR 7513) 
        Institut LeBel 
        Universite Louis Pasteur 
        4, rue Blaise Pascal 
        67070 Strasbourg 
        France 
;
_publ_contact_author_email       gade@chimie.u-strasbg.fr
_publ_contact_author_fax         '0033 388 416 045'
_publ_contact_author_phone       '0033 388 415 325'
_publ_section_title
;
 Synthesis and Structural Characterization of Metalated
 1,8-Bis(silylamino)naphthalene Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4615
_journal_page_last               4620
_journal_paper_doi               10.1021/ic000296+
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C28 H60 Li2 N8 O2 P2 Si2'
_chemical_formula_weight         672.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 110.603(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.983(2)
_cell_length_b                   11.1727(13)
_cell_length_c                   19.768(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     3924.5(7)
_computing_cell_refinement       'CAD4 (Enraf-Nonius)'
_computing_data_collection       'CAD4 (Enraf-Nonius)'
_computing_data_reduction        'BEGIN (SDP)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CAD4 (Enraf-Nonius)'
_diffrn_measurement_method       'Omega/Theta 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  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       2
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5061
_diffrn_reflns_theta_full        24.94
_diffrn_reflns_theta_max         24.94
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        0.7
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.206
_exptl_absorpt_correction_T_max  0.9994
_exptl_absorpt_correction_T_min  0.8984
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 empirical absorption correction by psi-scans from 10 reflections 
 with chi-angles near 90 degrees 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_description       cube
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3434
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0527P)^2^+4.3623P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1169
_reflns_number_gt                2691
_reflns_number_total             3434
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0002962B_1.cif
_cod_data_source_block           2
_cod_original_cell_volume        3924.5(8)
_cod_database_code               4327620