Syntheses and Structures of Stable 1-Aminoalumole Derivatives
Agou, Tomohiro; Wasano, Tatsuya; Sasamori, Takahiro; Tokitoh, Norihiro; Organometallics 33 (2014) 6963–; doi:10.1021/om501055f

data_4084814
_publ_section_title
;
 Syntheses and Structures of Stable 1-Aminoalumole Derivatives
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6963
_journal_paper_doi               10.1021/om501055f
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C24 H56 Al Li N2 Si4'
_chemical_formula_sum            'C24 H56 Al Li N2 Si4'
_chemical_formula_weight         518.99
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2815(8)
_cell_length_b                   9.8343(4)
_cell_length_c                   18.6058(8)
_cell_measurement_reflns_used    9023
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      30.3939
_cell_measurement_theta_min      2.1892
_cell_volume                     3162.1(2)
_computing_cell_refinement       HKL2000
_computing_data_collection       CrystalClear
_computing_data_reduction        HKL2000
_computing_molecular_graphics
;
Yadokari-XG 2011 (Wakita Nemoto et al., 2011)
;
_computing_publication_material
;
Yadokari-XG 2011 (Wakita Nemoto et al., 2011)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 14.7059
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  ccd
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_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            25697
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    0.230
_exptl_absorpt_correction_T_max  0.9619
_exptl_absorpt_correction_T_min  0.9237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
MULABS - Empirical Correction for Absorption Anisotropy.
Blessing, R. H., Acta Cryst., A51, 33-38 (1995).
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.170
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5864
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0679
_reflns_number_gt                5734
_reflns_number_total             5864
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501055f_si_002.cif
_cod_data_source_block           AlC4Et4N2TMS4Li
_cod_depositor_comments
'Adding full bibliography for 4084814--4084815.cif.'
_cod_database_code               4084814