#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:14:00 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178554 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/62/4066267.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_4066267
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            'C20 H60 Ge9'
_chemical_formula_weight         953.99
_chemical_name_systematic
;
 ?
;
_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                 106.31(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.164(3)
_cell_length_b                   9.2516(19)
_cell_length_c                   24.439(5)
_cell_measurement_reflns_used    4213
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.484
_cell_measurement_theta_min      4.931
_cell_volume                     3724.6(14)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            12160
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    7.162
_exptl_absorpt_correction_T_max  0.3937
_exptl_absorpt_correction_T_min  0.1825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.996
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3776
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0387
_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/[σ²(Fo²)+(0.0480P)²+5.3029P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0942
_reflns_number_gt                3042
_reflns_number_total             3776
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100377n_si_001.cif
_cod_data_source_block           4_701j
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3724.5(13)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4066267
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.0782(6) 1.0794(10) 0.3809(5) 0.043(3) Uani 0.544(7) 1 d P A 1
H1A H -0.1271 1.1102 0.3910 0.064 Uiso 0.544(7) 1 calc PR A 1
H1B H -0.0745 1.1315 0.3469 0.064 Uiso 0.544(7) 1 calc PR A 1
H1C H -0.0302 1.1004 0.4127 0.064 Uiso 0.544(7) 1 calc PR A 1
C2 C -0.1880(6) 0.8500(14) 0.3023(5) 0.051(3) Uani 0.544(7) 1 d P A 1
H2A H -0.1905 0.7501 0.2885 0.077 Uiso 0.544(7) 1 calc PR A 1
H2B H -0.1888 0.9164 0.2709 0.077 Uiso 0.544(7) 1 calc PR A 1
H2C H -0.2348 0.8693 0.3167 0.077 Uiso 0.544(7) 1 calc PR A 1
C3 C -0.1074(7) 0.7765(13) 0.4309(5) 0.055(3) Uani 0.544(7) 1 d P A 1
H3A H -0.1577 0.8145 0.4369 0.082 Uiso 0.544(7) 1 calc PR A 1
H3B H -0.0625 0.7911 0.4654 0.082 Uiso 0.544(7) 1 calc PR A 1
H3C H -0.1138 0.6730 0.4222 0.082 Uiso 0.544(7) 1 calc PR A 1
C11 C -0.1171(7) 1.0687(14) 0.3309(6) 0.043(3) Uani 0.456(7) 1 d P A 2
H11A H -0.1394 1.0568 0.2896 0.064 Uiso 0.456(7) 1 calc PR A 2
H11B H -0.0700 1.1332 0.3388 0.064 Uiso 0.456(7) 1 calc PR A 2
H11C H -0.1587 1.1105 0.3467 0.064 Uiso 0.456(7) 1 calc PR A 2
C22 C -0.1701(7) 0.7484(14) 0.3487(6) 0.051(4) Uani 0.456(7) 1 d P A 2
H22A H -0.2142 0.7856 0.3629 0.076 Uiso 0.456(7) 1 calc PR A 2
H22B H -0.1517 0.6551 0.3666 0.076 Uiso 0.456(7) 1 calc PR A 2
H22C H -0.1897 0.7359 0.3072 0.076 Uiso 0.456(7) 1 calc PR A 2
C33 C -0.0533(7) 0.9199(17) 0.4488(5) 0.051(4) Uani 0.456(7) 1 d P A 2
H33A H -0.0993 0.9649 0.4588 0.076 Uiso 0.456(7) 1 calc PR A 2
H33B H -0.0067 0.9857 0.4587 0.076 Uiso 0.456(7) 1 calc PR A 2
H33C H -0.0389 0.8293 0.4701 0.076 Uiso 0.456(7) 1 calc PR A 2
Ge1 Ge 0.03447(3) 0.78316(5) 0.34199(2) 0.02556(14) Uani 1 1 d . A .
Ge2 Ge -0.08378(3) 0.87938(5) 0.36619(2) 0.02948(14) Uani 1 1 d . . .
Ge3 Ge 0.09041(3) 0.59839(6) 0.41328(3) 0.03676(16) Uani 1 1 d . . .
Ge4 Ge 0.13892(3) 0.96590(5) 0.35392(2) 0.03020(15) Uani 1 1 d . . .
Ge5 Ge 0.0000 0.65825(7) 0.2500 0.0344(2) Uani 1 2 d S . .
C4 C 0.1913(4) 0.5144(8) 0.4060(3) 0.065(2) Uani 1 1 d . A .
H4A H 0.2329 0.5897 0.4118 0.098 Uiso 1 1 calc R . .
H4B H 0.1820 0.4728 0.3678 0.098 Uiso 1 1 calc R . .
H4C H 0.2095 0.4384 0.4347 0.098 Uiso 1 1 calc R . .
C5 C 0.1184(5) 0.6767(9) 0.4900(3) 0.086(3) Uani 1 1 d . A .
H5A H 0.0704 0.7220 0.4969 0.128 Uiso 1 1 calc R . .
H5B H 0.1614 0.7490 0.4943 0.128 Uiso 1 1 calc R . .
H5C H 0.1375 0.5985 0.5176 0.128 Uiso 1 1 calc R . .
C6 C 0.0145(5) 0.4400(9) 0.4097(4) 0.118(4) Uani 1 1 d . A .
H6A H 0.0402 0.3655 0.4375 0.177 Uiso 1 1 calc R . .
H6B H -0.0006 0.3983 0.3713 0.177 Uiso 1 1 calc R . .
H6C H -0.0342 0.4763 0.4186 0.177 Uiso 1 1 calc R . .
C7 C 0.1680(4) 1.0450(9) 0.4302(3) 0.067(2) Uani 1 1 d . A .
H7A H 0.2065 1.1246 0.4328 0.100 Uiso 1 1 calc R . .
H7B H 0.1931 0.9694 0.4576 0.100 Uiso 1 1 calc R . .
H7C H 0.1191 1.0811 0.4389 0.100 Uiso 1 1 calc R . .
C8 C 0.2378(5) 0.8837(9) 0.3426(5) 0.125(4) Uani 1 1 d . A .
H8A H 0.2272 0.8512 0.3030 0.188 Uiso 1 1 calc R . .
H8B H 0.2552 0.8012 0.3683 0.188 Uiso 1 1 calc R . .
H8C H 0.2806 0.9572 0.3508 0.188 Uiso 1 1 calc R . .
C9 C 0.1032(4) 1.1273(8) 0.3032(3) 0.088(3) Uani 1 1 d . A .
H9A H 0.0639 1.1847 0.3163 0.132 Uiso 1 1 calc R . .
H9B H 0.0775 1.0915 0.2646 0.132 Uiso 1 1 calc R . .
H9C H 0.1500 1.1877 0.3029 0.132 Uiso 1 1 calc R . .
C10 C 0.0917(5) 0.5296(6) 0.2502(3) 0.065(2) Uani 1 1 d . A .
H10A H 0.0916 0.4467 0.2751 0.098 Uiso 1 1 calc R . .
H10B H 0.1428 0.5828 0.2643 0.098 Uiso 1 1 calc R . .
H10C H 0.0863 0.4955 0.2114 0.098 Uiso 1 1 calc R . .
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
Ge4 Ge1 Ge2 110.78(3) . .
Ge4 Ge1 Ge3 105.90(3) . .
Ge2 Ge1 Ge3 105.70(3) . .
Ge4 Ge1 Ge5 114.83(3) . .
Ge2 Ge1 Ge5 113.11(3) . .
Ge3 Ge1 Ge5 105.69(3) . .
C22 Ge2 C1 132.5(5) . .
C22 Ge2 C11 111.3(6) . .
C1 Ge2 C11 37.0(5) . .
C22 Ge2 C33 108.8(6) . .
C1 Ge2 C33 68.4(6) . .
C11 Ge2 C33 103.9(6) . .
C22 Ge2 C3 62.9(6) . .
C1 Ge2 C3 109.3(5) . .
C11 Ge2 C3 132.7(5) . .
C33 Ge2 C3 48.0(6) . .
C22 Ge2 C2 42.9(6) . .
C1 Ge2 C2 105.4(5) . .
C11 Ge2 C2 72.4(5) . .
C33 Ge2 C2 137.1(4) . .
C3 Ge2 C2 102.4(5) . .
C22 Ge2 Ge1 111.6(4) . .
C1 Ge2 Ge1 113.9(3) . .
C11 Ge2 Ge1 112.3(3) . .
C33 Ge2 Ge1 108.6(3) . .
C3 Ge2 Ge1 112.9(3) . .
C2 Ge2 Ge1 112.2(3) . .
C5 Ge3 C6 107.8(4) . .
C5 Ge3 C4 104.6(3) . .
C6 Ge3 C4 107.2(4) . .
C5 Ge3 Ge1 111.7(2) . .
C6 Ge3 Ge1 111.8(2) . .
C4 Ge3 Ge1 113.3(2) . .
C9 Ge4 C7 106.1(4) . .
C9 Ge4 C8 110.1(4) . .
C7 Ge4 C8 106.6(4) . .
C9 Ge4 Ge1 111.85(18) . .
C7 Ge4 Ge1 111.25(19) . .
C8 Ge4 Ge1 110.8(3) . .
C10 Ge5 C10 105.8(5) . 2
C10 Ge5 Ge1 105.92(17) . 2
C10 Ge5 Ge1 107.2(2) 2 2
C10 Ge5 Ge1 107.2(2) . .
C10 Ge5 Ge1 105.92(17) 2 .
Ge1 Ge5 Ge1 123.66(4) 2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 Ge2 1.882(9) .
C2 Ge2 2.035(10) .
C3 Ge2 1.982(10) .
C11 Ge2 1.965(12) .
C22 Ge2 1.868(11) .
C33 Ge2 1.975(12) .
Ge1 Ge4 2.4215(8) .
Ge1 Ge2 2.4362(8) .
Ge1 Ge3 2.4372(8) .
Ge1 Ge5 2.4480(8) .
Ge3 C5 1.940(7) .
Ge3 C6 1.946(7) .
Ge3 C4 1.951(6) .
Ge4 C9 1.928(6) .
Ge4 C7 1.933(6) .
Ge4 C8 1.949(6) .
Ge5 C10 1.972(6) .
Ge5 C10 1.972(6) 2
Ge5 Ge1 2.4480(8) 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_4
Ge4 Ge1 Ge2 C22 172.8(5) .
Ge3 Ge1 Ge2 C22 -72.9(5) .
Ge5 Ge1 Ge2 C22 42.2(5) .
Ge4 Ge1 Ge2 C1 6.8(4) .
Ge3 Ge1 Ge2 C1 121.1(4) .
Ge5 Ge1 Ge2 C1 -123.8(4) .
Ge4 Ge1 Ge2 C11 47.1(5) .
Ge3 Ge1 Ge2 C11 161.3(5) .
Ge5 Ge1 Ge2 C11 -83.5(5) .
Ge4 Ge1 Ge2 C33 -67.2(5) .
Ge3 Ge1 Ge2 C33 47.0(5) .
Ge5 Ge1 Ge2 C33 162.2(5) .
Ge4 Ge1 Ge2 C3 -118.6(4) .
Ge3 Ge1 Ge2 C3 -4.3(4) .
Ge5 Ge1 Ge2 C3 110.9(4) .
Ge4 Ge1 Ge2 C2 126.3(4) .
Ge3 Ge1 Ge2 C2 -119.4(4) .
Ge5 Ge1 Ge2 C2 -4.2(4) .
Ge4 Ge1 Ge3 C5 59.6(3) .
Ge2 Ge1 Ge3 C5 -58.0(3) .
Ge5 Ge1 Ge3 C5 -178.2(3) .
Ge4 Ge1 Ge3 C6 -179.5(4) .
Ge2 Ge1 Ge3 C6 62.9(4) .
Ge5 Ge1 Ge3 C6 -57.3(4) .
Ge4 Ge1 Ge3 C4 -58.2(2) .
Ge2 Ge1 Ge3 C4 -175.8(2) .
Ge5 Ge1 Ge3 C4 64.0(2) .
Ge2 Ge1 Ge4 C9 -62.9(3) .
Ge3 Ge1 Ge4 C9 -177.1(3) .
Ge5 Ge1 Ge4 C9 66.7(3) .
Ge2 Ge1 Ge4 C7 55.5(3) .
Ge3 Ge1 Ge4 C7 -58.7(3) .
Ge5 Ge1 Ge4 C7 -174.9(3) .
Ge2 Ge1 Ge4 C8 173.9(4) .
Ge3 Ge1 Ge4 C8 59.7(4) .
Ge5 Ge1 Ge4 C8 -56.5(4) .
Ge4 Ge1 Ge5 C10 72.1(2) .
Ge2 Ge1 Ge5 C10 -159.4(2) .
Ge3 Ge1 Ge5 C10 -44.2(2) .
Ge4 Ge1 Ge5 C10 -175.3(2) 2
Ge2 Ge1 Ge5 C10 -46.8(2) 2
Ge3 Ge1 Ge5 C10 68.4(2) 2
Ge4 Ge1 Ge5 Ge1 -51.33(2) 2
Ge2 Ge1 Ge5 Ge1 77.17(3) 2
Ge3 Ge1 Ge5 Ge1 -167.66(2) 2
