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_4114188
_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            'C60 H74 Ge2 K'
_chemical_formula_weight         979.47
_chemical_name_common            Dipp*GeGeDipp*K
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 93.599(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6822(13)
_cell_length_b                   19.393(2)
_cell_length_c                   26.455(3)
_cell_measurement_reflns_used    912
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      30.4
_cell_measurement_theta_min      2.27
_cell_volume                     5469.6(11)
_computing_cell_refinement       'Bruker SAINT 6.33B (Bruker 2002)'
_computing_data_collection       'Bruker SMART 5.054 (Bruker 2002)'
_computing_data_reduction        'Bruker SAINT 6.33B (Bruker 2002)'
_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      91(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART 1000'
_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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            52864
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_time
;
frames measured at beginning and end of data collection 
;
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    1.210
_exptl_absorpt_correction_T_max  0.7281
_exptl_absorpt_correction_T_min  0.6368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.04 (Bruker 2002)'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_description       block
_exptl_crystal_F_000             2068
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         10685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0455P)^2^+5.2600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0983
_reflns_number_gt                9047
_reflns_number_total             10685
_reflns_threshold_expression     I>2/s(I)
_cod_data_source_file            ja035711msi20030421_060217_4.cif
_cod_data_source_block           test1
_cod_original_cell_volume        5469.7(11)
_cod_database_code               4114188