Facile Synthesis of an Unsaturated Spiro Germane by Hydroalumination and Intramolecular 1,1-Carbalumination†
Uhl, Werner; Rohling, Martina; Würthwein, Ernst-Ulrich; Ghavtadze, Nugzar; Bergander, Klaus; Organometallics 29 (2010) 5236–; doi:10.1021/om100359k

data_4066223
_publ_section_title
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 Facile Synthesis of an Unsaturated Spiro Germane by Hydroalumination and
 Intramolecular 1,1-Carbalumination&#x2020;
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5236
_journal_paper_doi               10.1021/om100359k
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C60 H98 Al2 Ge Si8'
_chemical_formula_weight         1170.65
_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                80.8230(10)
_cell_angle_beta                 74.1380(10)
_cell_angle_gamma                80.2360(10)
_cell_formula_units_Z            4
_cell_length_a                   14.9993(5)
_cell_length_b                   21.4156(7)
_cell_length_c                   22.9117(8)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.45
_cell_measurement_theta_min      2.159
_cell_volume                     6927.0(4)
_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 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotation anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0676
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            85545
_diffrn_reflns_theta_full        31.37
_diffrn_reflns_theta_max         31.37
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.639
_exptl_absorpt_correction_T_max  0.9687
_exptl_absorpt_correction_T_min  0.8617
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1358
_refine_ls_number_reflns         42936
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1223
_reflns_number_gt                27190
_reflns_number_total             42936
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100359k_si_001.cif
_cod_data_source_block           sad1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4066223