Hydroalumination of dialkynylgermanes—synthesis of alkenyl‒alkynylgermanes with intramolecular aluminium‒carbon interactions
Uhl, Werner; Rohling, Martina; Kösters, Jutta; New Journal of Chemistry 34 (2010) 1630–; doi:10.1039/c0nj00050g

data_7053460
_publ_section_title
;
 Hydroalumination of dialkynylgermanes---synthesis of
 alkenyl--alkynylgermanes with intramolecular aluminium--carbon
 interactions
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1630
_journal_paper_doi               10.1039/c0nj00050g
_journal_volume                  34
_journal_year                    2010
_chemical_formula_sum            'C42 H59 Al Ge Si4'
_chemical_formula_weight         775.82
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                74.1410(10)
_cell_angle_beta                 81.1020(10)
_cell_angle_gamma                79.0390(10)
_cell_formula_units_Z            4
_cell_length_a                   11.8818(2)
_cell_length_b                   17.6370(3)
_cell_length_c                   23.2730(3)
_cell_measurement_reflns_used    8969
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      72.387
_cell_measurement_theta_min      2.875
_cell_volume                     4578.53(13)
_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      243(2)
_diffrn_measured_fraction_theta_full 0.858
_diffrn_measured_fraction_theta_max 0.858
_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  0.0566
_diffrn_reflns_av_sigmaI/netI    0.0820
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27196
_diffrn_reflns_theta_full        72.58
_diffrn_reflns_theta_max         72.58
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    2.281
_exptl_absorpt_correction_T_max  0.7559
_exptl_absorpt_correction_T_min  0.5780
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.943
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.240
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     944
_refine_ls_number_reflns         15605
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.239
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0760
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1990
_refine_ls_wR_factor_ref         0.2104
_reflns_number_gt                12009
_reflns_number_total             15605
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0nj00050g.txt
_cod_data_source_block           sad1_7
_cod_original_cell_volume        4578.53(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7053460