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_4114190
_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_formula_sum            'C96 H122 Ge2 K2'
_chemical_formula_weight         1499.32
_chemical_name_common            K2[Bert*Ge]2.4benzene
_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                81.996(7)
_cell_angle_beta                 74.240(7)
_cell_angle_gamma                65.170(7)
_cell_formula_units_Z            1
_cell_length_a                   12.5633(13)
_cell_length_b                   12.8465(12)
_cell_length_c                   15.1597(11)
_cell_measurement_reflns_used    44
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      28.4
_cell_measurement_theta_min      6.5
_cell_volume                     2136.2(4)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens XDISK'
_computing_molecular_graphics    'SHELXTL 5, 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      130(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       2\q-\w
_diffrn_radiation_monochromator  'nickel filter'
_diffrn_radiation_source         'Siemens rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0150
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5640
_diffrn_reflns_theta_full        56.40
_diffrn_reflns_theta_max         56.40
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        4.9
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.055
_exptl_absorpt_correction_T_max  0.4937
_exptl_absorpt_correction_T_min  0.4937
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   XABS2
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         5640
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0545P)^2^+2.3401P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.0994
_reflns_number_gt                5140
_reflns_number_total             5640
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja035711msi20030421_060217_6.cif
_cod_data_source_block           mn1101
_cod_original_cell_volume        2136.2(3)
_cod_database_code               4114190