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_4112097
_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         'C92 H94 Ge2, 2(C2 H5 O C2 H5)0.5'
_chemical_formula_sum            'C96 H104 Ge2 O'
_chemical_formula_weight         1418.97
_chemical_name_systematic
;

 ?

;
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_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                87.3680(10)
_cell_angle_beta                 79.4960(10)
_cell_angle_gamma                66.6180(10)
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_cell_length_a                   13.7999(8)
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_cell_length_c                   20.3401(12)
_cell_measurement_reflns_used    5512
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.16
_cell_measurement_theta_min      2.46
_cell_volume                     3847.0(4)
_computing_cell_refinement       'SAINT (7.06a) (Bruker, 2004)'
_computing_data_collection       'Apex2 (1.0.27) Bruker, 2004)'
_computing_data_reduction        'SAINT (7.06a) (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34752
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.830
_exptl_absorpt_correction_T_max  0.8856
_exptl_absorpt_correction_T_min  0.7014
_exptl_absorpt_correction_type   'empirical, SADABS (multi-scan)'
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_meas      0
_exptl_crystal_description       Rod
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     970
_refine_ls_number_reflns         17678
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0618P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1119
_reflns_number_gt                12284
_reflns_number_total             17678
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja055372ssi20050819_054957.cif
_cod_data_source_block           1233ffmi
_cod_database_code               4112097