Reactions of the Heavier Group 14 Element Alkyne Analogues Ar'EEAr' (Ar' = C6H3-2,6(C6H3-2,6-Pri2)2; E = Ge, Sn) with Unsaturated Molecules: Probing the Character of the EE Multiple Bonds
Chunming Cui; Marilyn M. Olmstead; James C. Fettinger; Geoffrey H. Spikes; Philip P. Power; Journal of the American Chemical Society 127 (2005) 17530–17541; doi:10.1021/ja055372s

data_4112096
_publ_section_title
;
 Reactions of the Heavier Group 14 Element Alkyne Analogues Ar'EEAr' (Ar'
 = C6H3-2,6(C6H3-2,6-Pri2)2; E = Ge, Sn) with Unsaturated Molecules:
 Probing the Character of the EE Multiple Bonds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17530
_journal_page_last               17541
_journal_paper_doi               10.1021/ja055372s
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C72 H104 Ge2 N4 Si3, C6 H14'
_chemical_formula_sum            'C78 H118 Ge2 N4 Si3'
_chemical_formula_weight         1341.21
_chemical_name_common            Dipp*Ge(CHSiMe3)(n2CHSiMe3)2GeDipp*.n-hexane
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.746(3)
_cell_angle_beta                 80.117(3)
_cell_angle_gamma                83.322(4)
_cell_formula_units_Z            2
_cell_length_a                   12.8515(9)
_cell_length_b                   14.9117(11)
_cell_length_c                   20.4565(15)
_cell_measurement_reflns_used    986
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      2.4
_cell_volume                     3795.9(5)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART 5.054 (Bruker, 2002)'
_computing_data_reduction        'SAINT 6.45A (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_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  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            41348
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.60
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.882
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       plate
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.271
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.062
_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     827
_refine_ls_number_reflns         17358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0446P)^2^+2.2180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                13971
_reflns_number_total             17358
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja055372ssi20050805_074850.cif
_cod_data_source_block           mn1592
_cod_database_code               4112096