Synthesis, Structure, and Properties of a Stable 1,2-Dibromodialumane(4) Bearing a Bulky Aryl Substituent
Agou, Tomohiro; Nagata, Koichi; Sakai, Heisuke; Furukawa, Yukio; Tokitoh, Norihiro; Organometallics 31 (2012) 3806–; doi:10.1021/om300237q

data_4078301
_publ_section_title
;
 Synthesis, Structure, and Properties of a Stable 1,2-Dibromodialumane(4)
 Bearing a Bulky Aryl Substituent
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              3806
_journal_paper_doi               10.1021/om300237q
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C24 H51 Al Br2 O Si4'
_chemical_formula_sum            'C24 H51 Al Br2 O Si4'
_chemical_formula_weight         654.81
_chemical_name_common            BbpAlBrOEt2
_chemical_name_systematic
'2,6-bis(bis(trimethylsilyl)methyl)phenyl-dibromoalumane diethylether complex'
_chemical_properties_physical
'air-sensitive, moisture-sensitive, oxygen-sensitive'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2012-03-05 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.1654(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.54330(10)
_cell_length_b                   27.0804(4)
_cell_length_c                   13.4611(2)
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      2.14
_cell_volume                     3443.57(8)
_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    SIR2004
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku VariMax Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            29893
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.14
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku Mercury'
_exptl_absorpt_coefficient_mu    2.533
_exptl_absorpt_correction_T_max  0.9279
_exptl_absorpt_correction_T_min  0.7857
_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    1.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1368
_exptl_crystal_recrystallization_method hexane
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         6391
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+1.7060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0661
_reflns_number_gt                5645
_reflns_number_total             6391
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300237q_si_002.cif
_cod_data_source_block           BbpAlBr2OEt2
_cod_depositor_comments
;
  Moved the _audit_creation_method data item out of the loop.

  Antanas Vaitkus,
  2019-03-01
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4078301