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_4112091
_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_sum            'C66 H90 N Si Sn2'
_chemical_formula_weight         1162.86
_chemical_name_common            Dipp*Sn(N-SiMe3)SnDipp*.0.5n-hexane
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 96.47(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.694(4)
_cell_length_b                   18.392(4)
_cell_length_c                   32.292(7)
_cell_measurement_reflns_used    844
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      2.2
_cell_volume                     12802(5)
_computing_cell_refinement       'SMART 5.054 (Bruker, 2002)'
_computing_data_collection       'SMART 5.054 (Bruker, 2002)'
_computing_data_reduction        'SAINT 6.36A (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.135
_diffrn_reflns_av_sigmaI/netI    0.100
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            60542
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.28
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.835
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.05 (Sheldrick, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       plate
_exptl_crystal_F_000             4856
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.790
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.146
_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     637
_refine_ls_number_reflns         11720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1207
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0790P)^2^+80.6413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1433
_refine_ls_wR_factor_ref         0.1736
_reflns_number_gt                7157
_reflns_number_total             11720
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja055372ssi20050805_073641.cif
_cod_data_source_block           ar86
_cod_original_cell_volume        12803(4)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4112091