Germanium and Tin Analogues of Alkynes and Their Reduction Products
Lihung Pu; Andrew D. Phillips; Anne F. Richards; Matthias Stender; Richard S. Simons; Marilyn M. Olmstead; Philip P. Power; Journal of the American Chemical Society 125 (2003) 11626–11636; doi:10.1021/ja035711m

data_4114192
_publ_section_title
;
 Germanium and Tin Analogues of Alkynes and Their Reduction Products
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11626
_journal_page_last               11636
_journal_paper_doi               10.1021/ja035711m
_journal_volume                  125
_journal_year                    2003
_chemical_absolute_configuration ad
_chemical_formula_sum            'C90 H116 Na2 Sn2'
_chemical_formula_weight         1481.19
_chemical_name_common            (NaSnBert*)~2~^.^3benzene
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.720(4)
_cell_length_b                   16.720(4)
_cell_length_c                   29.616(6)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      16.8
_cell_measurement_theta_min      4.9
_cell_volume                     8279(3)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens XDISK'
_computing_molecular_graphics    'SHELXTL 5.03, 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      140(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens R3m/v'
_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  0.0529
_diffrn_reflns_av_sigmaI/netI    0.1304
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6018
_diffrn_reflns_theta_full        22.53
_diffrn_reflns_theta_max         22.53
_diffrn_reflns_theta_min         1.40
_diffrn_standards_decay_%        5.1
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  0.8801
_exptl_absorpt_correction_T_min  0.8586
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;XABS2: an empirical absorption correction program. Parkin, S.; Moezzi,
 B.; Hope, H. J. Appl. Cryst. 1995, 28, 53-56.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       bipyramid
_exptl_crystal_F_000             3112
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         5429
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1210
_refine_ls_R_factor_gt           0.0604
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+0.6186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.1122
_reflns_number_gt                3387
_reflns_number_total             5429
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja035711msi20030421_060217_8.cif
_cod_data_source_block           mn885
_cod_database_code               4114192