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_4106945
_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            'C42 H77 Ge N5 P2 Si'
_chemical_formula_weight         814.71
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 95.3190(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0149(4)
_cell_length_b                   13.3330(5)
_cell_length_c                   28.4929(9)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      2.78
_cell_volume                     4544.8(3)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            53670
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         5.18
_exptl_absorpt_coefficient_mu    0.804
_exptl_absorpt_correction_T_max  0.9384
_exptl_absorpt_correction_T_min  0.8304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_description       plate
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         13204
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+1.3427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0954
_reflns_number_gt                10340
_reflns_number_total             13204
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2073577_si_003.cif
_cod_data_source_block           6a
_cod_database_code               4106945