Generation of Weakly Bound Al‒N Lewis Pairs by Hydroalumination of Ynamines and the Activation of Small Molecules: Phenylethyne and Dicyclohexylcarbodiimide
Holtrichter-Rößmann, Thorsten; Rösener, Christian; Hellmann, Johannes; Uhl, Werner; Würthwein, Ernst-Ulrich; Fröhlich, Roland; Wibbeling, Birgit; Organometallics 31 (2012) 3272–; doi:10.1021/om3001179

data_4078104
_publ_section_title
;
 Generation of Weakly Bound Al--N Lewis Pairs by Hydroalumination of
 Ynamines and the Activation of Small Molecules: Phenylethyne and
 Dicyclohexylcarbodiimide
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              3272
_journal_paper_doi               10.1021/om3001179
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C28 H48 Al N Si'
_chemical_formula_weight         453.74
_chemical_melting_point          377
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 96.5550(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.81570(10)
_cell_length_b                   17.2096(2)
_cell_length_c                   17.4767(2)
_cell_measurement_reflns_used    7593
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      72.469
_cell_measurement_theta_min      3.616
_cell_volume                     2932.94(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17060
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         70.00
_diffrn_reflns_theta_min         3.63
_exptl_absorpt_coefficient_mu    1.079
_exptl_absorpt_correction_T_max  0.8295
_exptl_absorpt_correction_T_min  0.7240
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.028
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         5266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0742P)^2^+0.6091P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1191
_reflns_number_gt                4587
_reflns_number_total             5266
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3001179_si_006.cif
_cod_data_source_block           sad1
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4078104