Synthesis and Reactivity of a Phosphine-Stabilized Monogermanium Analogue of Alkynes
Juliette Berthe; Juan Manuel Garcia; Edgar Ocando; Tsuyoshi Kato; Nathalie Saffon-Merceron; Abel De Cózar; Fernando P. Cossío; Antoine Baceiredo; Journal of the American Chemical Society 133 (2011) 15930–15933; doi:10.1021/ja2073577

data_4106943
_publ_section_title
;
 Synthesis and Reactivity of a Phosphine-Stabilized Monogermanium Analogue
 of Alkynes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15930
_journal_page_last               15933
_journal_paper_doi               10.1021/ja2073577
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C46 H87 Ge N7 O P2 Si'
_chemical_formula_weight         916.85
_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                76.4920(10)
_cell_angle_beta                 75.0280(10)
_cell_angle_gamma                82.150(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4194(3)
_cell_length_b                   13.8223(6)
_cell_length_c                   20.0405(5)
_cell_measurement_reflns_used    9232
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      32.27
_cell_measurement_theta_min      2.59
_cell_volume                     2702.18(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      193(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker kappa APEX-II CCD Quazar'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            52913
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         5.11
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  0.7256
_exptl_absorpt_correction_T_min  0.6838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         13232
_refine_ls_number_restraints     170
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0547P)^2^+1.0201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1013
_reflns_number_gt                11480
_reflns_number_total             13232
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2073577_si_001.cif
_cod_data_source_block           3a
_cod_database_code               4106943