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_4112900
_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            'C76 H98 Ge2 Li2 O4'
_chemical_formula_weight         1234.60
_chemical_name_common            '[Li(THF)3(Et2O)][Li(HGeDipp*)2]'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 114.4310(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.6448(14)
_cell_length_b                   17.6953(14)
_cell_length_c                   12.6498(10)
_cell_measurement_reflns_used    7124
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      30.1
_cell_measurement_theta_min      2.3
_cell_volume                     3799.8(5)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART 5.054 (Bruker, 2003)'
_computing_data_reduction        'SAINT 6.36A (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL 5.1 (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      91(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0649
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17563
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.66
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.833
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.05 (Sheldrick, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.079
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.995
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         3568
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0866
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1544P)^2^+24.6758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2484
_refine_ls_wR_factor_ref         0.2612
_reflns_number_gt                2997
_reflns_number_total             3570
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja047090isi20040526_024739.cif
_cod_data_source_block           ar26
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4112900