Reduction of Digermenes with Alkali Metals: Salts of Formula M2[{Ge(H)Ar'}2] (M = Li, Na, or K, Ar' = Terphenyl) with Three Different Structures
Anne F. Richards; Marcin Brynda; Philip P. Power; Journal of the American Chemical Society 126 (2004) 10530–10531; doi:10.1021/ja047090i

data_4112902
_publ_section_title
;
 Reduction of Digermenes with Alkali Metals: Salts of Formula
 M2[{Ge(H)Ar'}2] (M = Li, Na, or K, Ar' = Terphenyl) with Three Different
 Structures
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10530
_journal_page_last               10531
_journal_paper_doi               10.1021/ja047090i
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C60 H76 Ge2 Na2'
_chemical_formula_weight         988.37
_chemical_name_common            '[Na]2[Dipp*Ge(mu-H)]2'
_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                 100.058(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.6034(15)
_cell_length_b                   17.856(2)
_cell_length_c                   13.1893(17)
_cell_measurement_reflns_used    956
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      30.82
_cell_measurement_theta_min      2.57
_cell_volume                     2690.7(6)
_computing_cell_refinement       'Bruker SAINT+ v. 6.36a'
_computing_data_collection       'Bruker SMART v. 5.626'
_computing_data_reduction        'Bruker SAINT+ v. 6.36a'
_computing_molecular_graphics    'XP, Bruker SHELXTL v. 6.12'
_computing_publication_material  'XCIF, Bruker SHELXTL v. 6.12'
_computing_structure_refinement  'XL, Bruker SHELXTL v. 6.12'
_computing_structure_solution    'XS, Bruker SHELXTL v. 6.12'
_diffrn_ambient_temperature      91(2)
_diffrn_detector_area_resol_mean 8.1
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24701
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        <0.01
_exptl_absorpt_coefficient_mu    1.169
_exptl_absorpt_correction_T_max  0.8350
_exptl_absorpt_correction_T_min  0.7431
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; SAINT+, 2001'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.213
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0648P)^2^+2.2541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1112
_reflns_number_gt                4745
_reflns_number_total             5581
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja047090isi20040526_024822.cif
_cod_data_source_block           t2
_cod_database_code               4112902