#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:14:00 +0100 (lun 21 de mar de 2016) $
#$Revision: 178554 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/62/4066266.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4066266
loop_
_publ_author_name
'Hlina, Johann'
'Baumgartner, Judith'
'Marschner, Christoph'
_publ_section_title
;
 Polygermane Building Blocks†
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5289
_journal_paper_doi               10.1021/om100377n
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C18 H54 Ge8'
_chemical_formula_weight         851.33
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   15.968(2)
_cell_length_b                   15.968(2)
_cell_length_c                   11.190(2)
_cell_measurement_reflns_used    4154
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.519
_cell_measurement_theta_min      4.655
_cell_volume                     2470.9(6)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SMART APEX'
_diffrn_measurement_method       'ω scans'
_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  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0164
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6662
_diffrn_reflns_theta_full        26.34
_diffrn_reflns_theta_max         26.34
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    7.197
_exptl_absorpt_correction_T_max  0.3270
_exptl_absorpt_correction_T_min  0.1873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1254
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     43
_refine_ls_number_reflns         1129
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0179
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0248P)²+4.4056P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0458
_refine_ls_wR_factor_ref         0.0465
_reflns_number_gt                1054
_reflns_number_total             1129
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100377n_si_001.cif
_cod_data_source_block           3_648j
_cod_original_cell_volume        2470.9(7)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4066266
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ge1 Ge 0.0000 0.0000 0.60979(3) 0.01673(10) Uani 1 3 d S
Ge2 Ge -0.161458(15) -0.091003(15) 0.696897(19) 0.02137(9) Uani 1 1 d .
C1 C -0.20835(18) -0.22949(16) 0.7184(2) 0.0370(6) Uani 1 1 d .
H1A H -0.2381 -0.2499 0.7975 0.056 Uiso 1 1 calc R
H1B H -0.1540 -0.2414 0.7119 0.056 Uiso 1 1 calc R
H1C H -0.2563 -0.2664 0.6567 0.056 Uiso 1 1 calc R
C2 C -0.25770(17) -0.07965(19) 0.6019(2) 0.0360(5) Uani 1 1 d .
H2A H -0.2678 -0.1144 0.5262 0.054 Uiso 1 1 calc R
H2B H -0.2348 -0.0113 0.5855 0.054 Uiso 1 1 calc R
H2C H -0.3188 -0.1076 0.6461 0.054 Uiso 1 1 calc R
C3 C -0.16048(19) -0.0399(2) 0.8564(2) 0.0387(6) Uani 1 1 d .
H3A H -0.1453 0.0274 0.8497 0.058 Uiso 1 1 calc R
H3B H -0.1114 -0.0430 0.9058 0.058 Uiso 1 1 calc R
H3C H -0.2242 -0.0786 0.8935 0.058 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ge1 0.01537(13) 0.01537(13) 0.01947(19) 0.000 0.000 0.00768(6)
Ge2 0.01813(13) 0.01933(13) 0.02545(14) 0.00279(8) 0.00394(8) 0.00846(9)
C1 0.0336(13) 0.0244(12) 0.0477(15) 0.0102(10) 0.0069(11) 0.0104(10)
C2 0.0219(11) 0.0401(14) 0.0464(14) 0.0068(11) 0.0018(10) 0.0158(10)
C3 0.0402(14) 0.0433(15) 0.0273(12) 0.0007(10) 0.0111(10) 0.0170(12)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Ge2 Ge1 Ge2 105.130(12) . 3
Ge2 Ge1 Ge2 105.129(12) . 2
Ge2 Ge1 Ge2 105.130(11) 3 2
Ge2 Ge1 Ge1 113.526(10) . 10_556
Ge2 Ge1 Ge1 113.526(10) 3 10_556
Ge2 Ge1 Ge1 113.526(10) 2 10_556
C2 Ge2 C3 107.50(11) . .
C2 Ge2 C1 107.29(11) . .
C3 Ge2 C1 106.04(11) . .
C2 Ge2 Ge1 111.94(7) . .
C3 Ge2 Ge1 109.24(8) . .
C1 Ge2 Ge1 114.45(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ge1 Ge2 2.4418(4) .
Ge1 Ge2 2.4418(4) 3
Ge1 Ge2 2.4418(4) 2
Ge1 Ge1 2.4571(8) 10_556
Ge2 C2 1.950(2) .
Ge2 C3 1.959(2) .
Ge2 C1 1.963(2) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
Ge2 Ge1 Ge2 C2 89.39(9) 3
Ge2 Ge1 Ge2 C2 -159.93(9) 2
Ge1 Ge1 Ge2 C2 -35.27(9) 10_556
Ge2 Ge1 Ge2 C3 -29.55(9) 3
Ge2 Ge1 Ge2 C3 81.13(9) 2
Ge1 Ge1 Ge2 C3 -154.21(9) 10_556
Ge2 Ge1 Ge2 C1 -148.26(9) 3
Ge2 Ge1 Ge2 C1 -37.57(9) 2
Ge1 Ge1 Ge2 C1 87.08(9) 10_556
