Syntheses and Structural Characterization of a LAl(N3)N[μ-Si(N3)(tBu)]2NAl(N3)L and a Monomeric Aluminum Hydride Amide LAlH(NHAr) (L = HC[(CMe)(NAr)]2, Ar = 2,6-iPr2C6H3)
Zhu, Hongping; Yang, Zhi; Magull, Jörg; Roesky, Herbert W.; Schmidt, Hans-Georg; Noltemeyer, Mathias; Organometallics 24 (2005) 6420–; doi:10.1021/om050698v

data_4076168
_publ_section_title
;
 Syntheses and Structural Characterization of a
 LAl(N3)N[\m-Si(N3)(tBu)]2NAl(N3)L and a Monomeric Aluminum Hydride Amide
 LAlH(NHAr) (L = HC[(CMe)(NAr)]2, Ar = 2,6-iPr2C6H3)
;
_journal_issue                   26
_journal_name_full               Organometallics
_journal_page_first              6420
_journal_paper_doi               10.1021/om050698v
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C48 H68 Al N3'
_chemical_formula_weight         714.03
_chemical_name_systematic
; 
 ? 
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.56(3)
_cell_angle_beta                 90.86(3)
_cell_angle_gamma                110.81(3)
_cell_formula_units_Z            2
_cell_length_a                   10.071(2)
_cell_length_b                   11.630(2)
_cell_length_c                   19.851(4)
_cell_measurement_temperature    200(2)
_cell_volume                     2171.8(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  Stoe-Siemens-Huber
_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  0.0761
_diffrn_reflns_av_sigmaI/netI    0.0587
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9308
_diffrn_reflns_theta_full        22.47
_diffrn_reflns_theta_max         22.47
_diffrn_reflns_theta_min         3.52
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             780
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         5648
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0796P)^2^+0.8460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1464
_reflns_number_gt                4667
_reflns_number_total             5648
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050698vsi20050926_055724.cif
_cod_data_source_block           compound_4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom and difmap' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        2171.7(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4076168