E-H (E = B, Si, Ge) bond activation of pinacolborane, silanes, and germanes by nucleophilic palladium carbene complexes.
Comanescu, Cezar C.; Iluc, Vlad M.; Chemical communications (Cambridge, England) 52 (2016) 9048–9051; doi:10.1039/c5cc09468b

data_7118689
_publ_section_title
;
 E-H (E = B, Si, Ge) bond activation of pinacolborane, silanes, and
 germanes by nucleophilic palladium carbene complexes.
;
_journal_issue                   58
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9048
_journal_page_last               9051
_journal_paper_doi               10.1039/c5cc09468b
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C31 H44 Ge P2 Pd'
_chemical_formula_weight         657.59
_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
;
2015-11-12 deposited with the CCDC.
2016-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                94.2185(11)
_cell_angle_beta                 93.3363(11)
_cell_angle_gamma                100.7761(11)
_cell_formula_units_Z            2
_cell_length_a                   8.3636(3)
_cell_length_b                   10.0092(4)
_cell_length_c                   18.4078(7)
_cell_measurement_reflns_used    9732
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.868
_cell_measurement_theta_min      2.272
_cell_volume                     1505.62(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'combination of \w- and \f-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  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32263
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.719
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.013
_refine_diff_density_min         -1.472
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         5270
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0181P)^2^+4.0326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0725
_reflns_number_gt                4607
_reflns_number_total             5270
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc09468b3.cif
_cod_data_source_block           cc293
_cod_depositor_comments
'Adding full bibliography for 7118684--7118692.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7118689