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_4071495
_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            'C19 H49 Al Si5'
_chemical_formula_weight         445.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_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                97.449(2)
_cell_angle_beta                 95.133(2)
_cell_angle_gamma                105.461(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5540(3)
_cell_length_b                   12.1864(5)
_cell_length_c                   12.5117(5)
_cell_measurement_reflns_used    'all measured'
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      71.86
_cell_measurement_theta_min      3.80
_cell_volume                     1524.87(10)
_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      153(2)
_diffrn_measured_fraction_theta_full 0.843
_diffrn_measured_fraction_theta_max 0.843
_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  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0968
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8315
_diffrn_reflns_theta_full        72.28
_diffrn_reflns_theta_max         72.28
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    2.467
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.042
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.969
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         5070
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1242
_refine_ls_R_factor_gt           0.0846
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2520
_refine_ls_wR_factor_ref         0.2918
_reflns_number_gt                3435
_reflns_number_total             5070
_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      '-P 1'
_cod_database_code               4071495