Two-coordinate group 14 element(ii) hydrides as reagents for the facile, and sometimes reversible, hydrogermylation/hydrostannylation of unactivated alkenes and alkynes
Hadlington, Terrance J.; Hermann, Markus; Frenking, Gernot; Jones, Cameron; Chem. Sci. 6 (2015) 7249–; doi:10.1039/C5SC03376D

data_1532471
_publ_section_title
;
 Two-coordinate group 14 element(ii) hydrides as reagents for the facile,
 and sometimes reversible, hydrogermylation/hydrostannylation of
 unactivated alkenes and alkynes
;
_journal_issue                   12
_journal_name_full               'Chem. Sci.'
_journal_page_first              7249
_journal_paper_doi               10.1039/C5SC03376D
_journal_volume                  6
_journal_year                    2015
_chemical_formula_sum            'C46 H57 Ge N Si'
_chemical_formula_weight         724.61
_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
_audit_update_record
;
2015-09-07 deposited with the CCDC.
2015-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                97.01(3)
_cell_angle_beta                 91.76(3)
_cell_angle_gamma                92.77(3)
_cell_formula_units_Z            2
_cell_length_a                   10.783(2)
_cell_length_b                   11.465(2)
_cell_length_c                   16.298(3)
_cell_measurement_temperature    100(2)
_cell_volume                     1996.1(6)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'Blu-Ice (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.920
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71080
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25550
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    0.829
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   XDS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0194(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         6617
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0394P)^2^+1.9227P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.0996
_reflns_number_gt                5669
_reflns_number_total             6617
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc03376d2.cif
_cod_data_source_block           compound5
_cod_depositor_comments
'Adding full bibliography for 1532469--1532486.cif.'
_cod_original_cell_volume        1996.1(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1532471