Facile Activation of Dihydrogen by an Unsaturated Heavier Main Group Compound
Geoffrey H. Spikes; James C. Fettinger; Philip P. Power; Journal of the American Chemical Society 127 (2005) 12232–12233; doi:10.1021/ja053247a

data_4111895
_publ_section_title
;
 Facile Activation of Dihydrogen by an Unsaturated Heavier Main Group
 Compound
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12232
_journal_page_last               12233
_journal_paper_doi               10.1021/ja053247a
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C60 H78 Ge2'
_chemical_formula_sum            'C60 H78 Ge2'
_chemical_formula_weight         944.40
_chemical_melting_point          517
_chemical_name_common            digermane
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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            12
_cell_length_a                   16.3425(11)
_cell_length_b                   45.579(3)
_cell_length_c                   21.2946(14)
_cell_measurement_reflns_used    8234
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      29.77
_cell_measurement_theta_min      2.28
_cell_volume                     15861.8(18)
_computing_cell_refinement       'SAINT (7.16b) (Bruker, 2004)'
_computing_data_collection       'SMART (Version 5.054) (Bruker, 2002)'
_computing_data_reduction        'SAINT (7.16b) (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART1000'
_diffrn_measurement_method       '\w and \f'
_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  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            91162
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.32
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.173
_exptl_absorpt_correction_T_max  0.6589
_exptl_absorpt_correction_T_min  0.5155
_exptl_absorpt_correction_type   'empirical, SADABS (multi-scan)'
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_description       Block
_exptl_crystal_F_000             6024
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.36
_refine_diff_density_max         2.172
_refine_diff_density_min         -1.773
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.331(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1734
_refine_ls_number_reflns         28329
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0622
_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^)+(0.0549P)^2^+51.4333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1501
_reflns_number_gt                24708
_reflns_number_total             28329
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja053247asi20050628_042823.cif
_cod_data_source_block           digermane
_cod_original_cell_volume        15861.7(18)
_cod_database_code               4111895