Effects of the alkali metal counter ions on the germanium?germanium double bond length in a heavier group 14 element ethenide salt
Richards, Anne F.; Brynda, Marcin; Power, Philip P.; Chemical Communications  (2004) 1592–1593; doi:10.1039/b401507j

data_7110271
_publ_section_title
;
 Effects of the alkali metal counter ions on the germanium?germanium
 double bond length in a heavier group 14 element ethenide salt
;
_journal_issue                   14
_journal_name_full               'Chemical Communications'
_journal_page_first              1592
_journal_page_last               1593
_journal_paper_doi               10.1039/b401507j
_journal_year                    2004
_chemical_formula_sum            'C64 H88 Ge2 Li2 O5'
_chemical_formula_weight         1096.40
_chemical_name_common            (Jeff*GeLi(OEt2)diox)2
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 98.2720(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.2752(15)
_cell_length_b                   11.5462(8)
_cell_length_c                   23.4339(16)
_cell_measurement_reflns_used    875
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      59.509
_cell_measurement_theta_min      4.583
_cell_volume                     5964.4(7)
_computing_cell_refinement       'Bruker SAINT 6.35A (Bruker 2002)'
_computing_data_collection       'Bruker SMART 5.054 (Bruker 2001)'
_computing_data_reduction        'Bruker SAINT 6.35A (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      90(2)
_diffrn_detector_area_resol_mean 8.3
_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  0.1150
_diffrn_reflns_av_sigmaI/netI    0.1017
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            32323
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.76
_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    1.054
_exptl_absorpt_correction_T_max  0.9521
_exptl_absorpt_correction_T_min  0.8248
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'not applied'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.558
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       0.00044(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6847
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0541P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1212
_reflns_number_gt                4206
_reflns_number_total             6847
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b401507jsup1.cif
_cod_data_source_block           test4
_cod_original_sg_symbol_H-M      'C 2 / c'
_cod_database_code               7110271