Synthesis and Structure of Stable Tri-tert-butylgermyl-Substituted Stannylene and Germylene
Setaka, Wataru; Sakamoto, Kenkichi; Kira, Mitsuo; Power, Philip P.; Organometallics 20 (2001) 4460–; doi:10.1021/om010591h

data_4077412
_publ_section_title
;
 Synthesis and Structure of Stable Tri-tert-butylgermyl-Substituted
 Stannylene and Germylene
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              4460
_journal_paper_doi               10.1021/om010591h
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C42 H62 Ge Sn'
_chemical_formula_weight         758.20
_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
_cell_angle_alpha                91.260(2)
_cell_angle_beta                 95.308(2)
_cell_angle_gamma                94.727(3)
_cell_formula_units_Z            4
_cell_length_a                   11.5028(16)
_cell_length_b                   15.748(2)
_cell_length_c                   21.351(3)
_cell_measurement_temperature    120(2)
_cell_volume                     3836.3(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0851
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22726
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    1.461
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.276
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         15601
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.934
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0621P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1228
_reflns_number_gt                10254
_reflns_number_total             15601
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om010591h.cif
_cod_data_source_block           sgd1
_cod_original_cell_volume        3836.5(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077412