Reactions of Terminal Alkynes with a Bulky Dialkylaluminum Hydride: Hydroalumination versus Deprotonation
Uhl, Werner; Er, Elif; Hepp, Alexander; Kösters, Jutta; Grunenberg, Jörg; Organometallics 27 (2008) 3346–; doi:10.1021/om800190f

data_4071494
_publ_section_title
;
 Reactions of Terminal Alkynes with a Bulky Dialkylaluminum Hydride:
 Hydroalumination versus Deprotonation
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3346
_journal_paper_doi               10.1021/om800190f
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C22 H45 Al Si4'
_chemical_formula_weight         448.92
_chemical_melting_point          >360&#x00B0;
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           110
_symmetry_space_group_name_Hall  'I 4bw -2c'
_symmetry_space_group_name_H-M   'I 41 c d'
_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            8
_cell_length_a                   15.4927(4)
_cell_length_b                   15.4927(4)
_cell_length_c                   23.7644(6)
_cell_measurement_reflns_used    'all measured'
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.06
_cell_measurement_theta_min      4.04
_cell_volume                     5704.0(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0823
_diffrn_reflns_av_sigmaI/netI    0.0586
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            15692
_diffrn_reflns_theta_full        70.24
_diffrn_reflns_theta_max         70.24
_diffrn_reflns_theta_min         5.49
_exptl_absorpt_coefficient_mu    2.259
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.486
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.046
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.39(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2536
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.0961
_reflns_number_gt                2204
_reflns_number_total             2536
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800190f-file001.cif
_cod_data_source_block           sad
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constr.' was replaced with the
value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_sg_symbol_H-M      'I 4bw -2c'
_cod_database_code               4071494