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_4106946
_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            'C40 H71 Ge N5 P2'
_chemical_formula_weight         756.55
_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                85.4800(10)
_cell_angle_beta                 81.329(2)
_cell_angle_gamma                70.6260(10)
_cell_formula_units_Z            2
_cell_length_a                   9.8517(4)
_cell_length_b                   10.3538(4)
_cell_length_c                   22.4488(10)
_cell_measurement_reflns_used    9802
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.28
_cell_volume                     2134.46(15)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            38146
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         5.13
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_T_max  0.7556
_exptl_absorpt_correction_T_min  0.6288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         10483
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+1.1287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0838
_reflns_number_gt                9306
_reflns_number_total             10483
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2073577_si_004.cif
_cod_data_source_block           6b
_cod_database_code               4106946