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_4077410
_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            'C36 H52 Ge Sn'
_chemical_formula_weight         676.06
_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                 91.362(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1470(19)
_cell_length_b                   18.340(3)
_cell_length_c                   16.130(3)
_cell_measurement_temperature    120(2)
_cell_volume                     3296.6(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.1031
_diffrn_reflns_av_sigmaI/netI    0.0657
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14099
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    1.691
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.370
_refine_diff_density_min         -1.016
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4563
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1028P)^2^+31.3882P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2012
_refine_ls_wR_factor_ref         0.2088
_reflns_number_gt                3971
_reflns_number_total             4563
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om010591h.cif
_cod_data_source_block           snge7n
_cod_original_cell_volume        3296.7(10)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4077410