Syntheses, Structures, and Electronic Properties of the Branched Oligogermanes (Ph3Ge)3GeH and (Ph3Ge)3GeX (X = Cl, Br, I)†
Samanamu, Christian R.; Amadoruge, Monika L.; Yoder, Claude H.; Golen, James A.; Moore, Curtis E.; Rheingold, Arnold L.; Materer, Nicholas F.; Weinert, Charles S.; Organometallics 30 (2011) 1046–; doi:10.1021/om101091c

data_4064028
_publ_section_title
;
 Syntheses, Structures, and Electronic Properties of the Branched
 Oligogermanes (Ph3Ge)3GeH and (Ph3Ge)3GeX (X = Cl, Br, I)&#x2020;
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1046
_journal_paper_doi               10.1021/om101091c
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C80 H0 Cl0 F24 Ge4 O2 P4'
_chemical_formula_weight         1863.04
_chemical_name_common            'COMPOUND 3a'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 95.81
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   13.116
_cell_length_b                   10.450
_cell_length_c                   18.204
_cell_measurement_temperature    293(2)
_cell_volume                     2482.263
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.623
_diffrn_measured_fraction_theta_max 0.623
_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  0.0933
_diffrn_reflns_av_sigmaI/netI    0.1116
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            4949
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         1.12
_exptl_absorpt_coefficient_mu    1.345
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             900
_refine_diff_density_max         0.903
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.51(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         4745
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0748P)^2^+1.5869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1712
_reflns_number_gt                3854
_reflns_number_total             4745
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101091c_si_002.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        2482.1
_cod_database_code               4064028