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_4327621
_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            'C42.5 H68 Li2 N5 Si2'
_chemical_formula_weight         719.08
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                97.030(14)
_cell_angle_beta                 95.118(14)
_cell_angle_gamma                90.331(15)
_cell_formula_units_Z            2
_cell_length_a                   11.645(3)
_cell_length_b                   12.173(3)
_cell_length_c                   15.959(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     2236.0(10)
_computing_cell_refinement       'CAD4 (Enraf-Nonius)'
_computing_data_collection       'CAD4 (Enraf-Nonius)'
_computing_data_reduction        'BEGIN (SDP)'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5294
_diffrn_reflns_theta_full        21.00
_diffrn_reflns_theta_max         21.00
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        0.3
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.9996
_exptl_absorpt_correction_T_min  0.8720
_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    1.068
_exptl_crystal_description       prism
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         4795
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0709
_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^)+(0.1217P)^2^+1.3937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1878
_refine_ls_wR_factor_ref         0.2114
_reflns_number_gt                3460
_reflns_number_total             4795
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0002962B_2.cif
_cod_data_source_block           3
_cod_original_cell_volume        2235.8(9)
_cod_original_formula_sum        'C42.50 H68 Li2 N5 Si2'
_cod_database_code               4327621