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_4112901
_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 K2'
_chemical_formula_weight         1020.59
_chemical_name_common            '[(Dipp*GeH2)]K2'
_chemical_name_systematic
; 
 ? 
;
_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                 101.959(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.4599(11)
_cell_length_b                   18.3736(18)
_cell_length_c                   13.3713(13)
_cell_measurement_reflns_used    956
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      30.216
_cell_measurement_theta_min      2.676
_cell_volume                     2754.3(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_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  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30753
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.91
_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    1.278
_exptl_absorpt_correction_T_max  0.7878
_exptl_absorpt_correction_T_min  0.6647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.04 (Sheldrick 2002)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       block
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.906
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.875
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         6308
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.875
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0497P)^2^+3.3002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0848
_reflns_number_gt                5460
_reflns_number_total             6308
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja047090isi20040526_024805.cif
_cod_data_source_block           ar126
_cod_database_code               4112901