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_4112090
_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         'C136 H148 Ge4 N12, 2.25 C4H10O'
_chemical_formula_sum            'C147 H170.5 Ge4 N12 O2.25'
_chemical_formula_weight         2431.81
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.0570(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.3869(9)
_cell_length_b                   29.4879(13)
_cell_length_c                   25.0943(11)
_cell_measurement_reflns_used    7153
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      23.70
_cell_measurement_theta_min      2.24
_cell_volume                     14029.4(11)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            96096
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_T_max  0.8857
_exptl_absorpt_correction_T_min  0.8424
_exptl_absorpt_correction_type   'empirical, SADABS (multi-scan)'
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            'Pale Yellow'
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_density_meas      0
_exptl_crystal_description       Block
_exptl_crystal_F_000             5130
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.856
_refine_diff_density_min         -1.053
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1617
_refine_ls_number_reflns         24669
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_gt           0.0633
_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^)+(0.1001P)^2^+1.4654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1647
_refine_ls_wR_factor_ref         0.1814
_reflns_number_gt                15875
_reflns_number_total             24669
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja055372ssi20050805_073544.cif
_cod_data_source_block           1232ffmi
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C147 H170.50 Ge4 N12 O2.25'
_cod_database_code               4112090