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_4327622
_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            'C24 H40 Br Li Mg N2 O2 Si2'
_chemical_formula_weight         555.92
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 94.625(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6817(11)
_cell_length_b                   11.7292(15)
_cell_length_c                   22.157(3)
_cell_measurement_reflns_used    49
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      12.53
_cell_measurement_theta_min      2.53
_cell_volume                     3026.0(6)
_computing_cell_refinement       'BRUKER XSCANS'
_computing_data_collection       'BRUKER XSCANS'
_computing_data_reduction        'BRUKER XSCANS'
_computing_molecular_graphics    'BRUKER SHELXTL'
_computing_publication_material  'BRUKER SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      299(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       'Omega/2Theta 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  0.0716
_diffrn_reflns_av_sigmaI/netI    0.1379
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            4326
_diffrn_reflns_theta_full        21.00
_diffrn_reflns_theta_max         21.00
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        4.62
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.479
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4247
_exptl_absorpt_correction_type   empirical/difabs
_exptl_absorpt_process_details
; 
 empirical absorption correction was applied using DIFABS
 (N. Walker, D. Stuart, Acta Crystallogr., Sect. A 1983, 39, 158).
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         3243
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.1737
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          2.847
_refine_ls_shift/su_mean         0.151
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1538
_reflns_number_gt                1563
_reflns_number_total             3243
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0002962B_3.cif
_cod_data_source_block           4
_cod_database_code               4327622