#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:36:45 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178787 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/41/4104164.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_4104164
loop_
_publ_author_name
'Harald Wagner'
'Judith Baumgartner'
'Thomas Müller'
'Christoph Marschner'
_publ_section_title
;
 Shuttling Germanium Atoms into Branched Polysilanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5022
_journal_page_last               5023
_journal_paper_doi               10.1021/ja809270m
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C22 H66 Ge4 Si6'
_chemical_formula_weight         789.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.20(3)
_cell_angle_beta                 103.02(3)
_cell_angle_gamma                114.18(3)
_cell_formula_units_Z            1
_cell_length_a                   9.1291(18)
_cell_length_b                   9.1306(18)
_cell_length_c                   13.694(3)
_cell_measurement_reflns_used    3760
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.552
_cell_measurement_theta_min      4.922
_cell_volume                     1003.5(5)
_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 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7787
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    3.156
_exptl_absorpt_correction_T_max  0.5180
_exptl_absorpt_correction_T_min  0.3962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             410
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.909
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         3968
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0349
_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)+(0.0494P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0901
_reflns_number_gt                3408
_reflns_number_total             3968
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja809270m_si_001_2.cif
_cod_data_source_block           8_632j
_cod_original_cell_volume        1003.5(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4104164
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.84268(4) 0.29929(4) 0.27699(2) 0.01321(10) Uani 1 1 d .
Ge2 Ge 1.05038(4) 0.47478(4) 0.42867(2) 0.01725(11) Uani 1 1 d .
Si1 Si 0.62228(10) 0.07378(10) 0.31248(6) 0.01625(19) Uani 1 1 d .
Si2 Si 0.73133(10) 0.44992(10) 0.17052(6) 0.01617(19) Uani 1 1 d .
Si3 Si 0.98431(10) 0.20135(10) 0.18397(6) 0.01740(19) Uani 1 1 d .
C1 C 0.4777(4) 0.1425(4) 0.3554(3) 0.0241(7) Uani 1 1 d .
H1A H 0.3897 0.0499 0.3727 0.036 Uiso 1 1 calc R
H1B H 0.4276 0.1876 0.3008 0.036 Uiso 1 1 calc R
H1C H 0.5397 0.2259 0.4151 0.036 Uiso 1 1 calc R
C2 C 0.7082(4) -0.0292(4) 0.4099(2) 0.0255(7) Uani 1 1 d .
H2A H 0.7740 0.0481 0.4721 0.038 Uiso 1 1 calc R
H2B H 0.7791 -0.0686 0.3840 0.038 Uiso 1 1 calc R
H2C H 0.6162 -0.1210 0.4246 0.038 Uiso 1 1 calc R
C3 C 0.4982(4) -0.0788(4) 0.1947(2) 0.0262(8) Uani 1 1 d .
H3A H 0.4115 -0.1736 0.2112 0.039 Uiso 1 1 calc R
H3B H 0.5721 -0.1126 0.1678 0.039 Uiso 1 1 calc R
H3C H 0.4463 -0.0297 0.1438 0.039 Uiso 1 1 calc R
C4 C 0.5432(4) 0.3054(4) 0.0699(2) 0.0239(7) Uani 1 1 d .
H4A H 0.4561 0.2406 0.1016 0.036 Uiso 1 1 calc R
H4B H 0.5735 0.2333 0.0324 0.036 Uiso 1 1 calc R
H4C H 0.5018 0.3669 0.0232 0.036 Uiso 1 1 calc R
C5 C 0.8865(4) 0.5838(4) 0.1061(3) 0.0267(7) Uani 1 1 d .
H5A H 0.8398 0.6487 0.0660 0.040 Uiso 1 1 calc R
H5B H 0.9123 0.5167 0.0614 0.040 Uiso 1 1 calc R
H5C H 0.9885 0.6562 0.1572 0.040 Uiso 1 1 calc R
C6 C 0.6670(4) 0.5792(4) 0.2436(2) 0.0237(7) Uani 1 1 d .
H6A H 0.7650 0.6603 0.2937 0.036 Uiso 1 1 calc R
H6B H 0.5866 0.5110 0.2784 0.036 Uiso 1 1 calc R
H6C H 0.6156 0.6342 0.1971 0.036 Uiso 1 1 calc R
C7 C 1.1892(4) 0.3681(4) 0.1814(3) 0.0257(7) Uani 1 1 d .
H7A H 1.2622 0.4062 0.2505 0.039 Uiso 1 1 calc R
H7B H 1.1709 0.4583 0.1535 0.039 Uiso 1 1 calc R
H7C H 1.2414 0.3271 0.1390 0.039 Uiso 1 1 calc R
C8 C 0.8555(4) 0.1208(4) 0.0497(2) 0.0261(8) Uani 1 1 d .
H8A H 0.8401 0.2088 0.0169 0.039 Uiso 1 1 calc R
H8B H 0.7467 0.0348 0.0492 0.039 Uiso 1 1 calc R
H8C H 0.9125 0.0766 0.0130 0.039 Uiso 1 1 calc R
C9 C 1.0206(4) 0.0309(4) 0.2404(3) 0.0269(8) Uani 1 1 d .
H9A H 1.0831 -0.0040 0.2028 0.040 Uiso 1 1 calc R
H9B H 0.9133 -0.0604 0.2362 0.040 Uiso 1 1 calc R
H9C H 1.0844 0.0683 0.3115 0.040 Uiso 1 1 calc R
C10 C 1.2100(4) 0.3829(4) 0.4748(2) 0.0251(7) Uani 1 1 d .
H10A H 1.2502 0.3608 0.4179 0.038 Uiso 1 1 calc R
H10B H 1.1553 0.2816 0.5010 0.038 Uiso 1 1 calc R
H10C H 1.3043 0.4605 0.5287 0.038 Uiso 1 1 calc R
C11 C 1.1727(4) 0.6816(4) 0.3827(2) 0.0215(7) Uani 1 1 d .
H11A H 1.2711 0.7509 0.4372 0.032 Uiso 1 1 calc R
H11B H 1.1002 0.7368 0.3649 0.032 Uiso 1 1 calc R
H11C H 1.2075 0.6600 0.3232 0.032 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'
Si Si 0.0817 0.0704 '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_3
Si1 Ge1 Si2 109.70(4) .
Si1 Ge1 Si3 108.81(4) .
Si2 Ge1 Si3 106.73(4) .
Si1 Ge1 Ge2 113.54(4) .
Si2 Ge1 Ge2 110.89(3) .
Si3 Ge1 Ge2 106.89(3) .
C10 Ge2 C11 106.77(14) .
C10 Ge2 Ge1 108.28(10) .
C11 Ge2 Ge1 105.30(10) .
C10 Ge2 Ge2 108.76(10) 2_766
C11 Ge2 Ge2 109.89(10) 2_766
Ge1 Ge2 Ge2 117.33(3) 2_766
C1 Si1 C2 111.29(15) .
C1 Si1 C3 107.38(16) .
C2 Si1 C3 107.84(15) .
C1 Si1 Ge1 109.77(11) .
C2 Si1 Ge1 110.18(11) .
C3 Si1 Ge1 110.32(11) .
C6 Si2 C5 108.45(16) .
C6 Si2 C4 108.23(14) .
C5 Si2 C4 107.99(16) .
C6 Si2 Ge1 111.54(11) .
C5 Si2 Ge1 111.24(11) .
C4 Si2 Ge1 109.28(11) .
C8 Si3 C7 107.99(16) .
C8 Si3 C9 107.52(16) .
C7 Si3 C9 109.25(16) .
C8 Si3 Ge1 110.10(11) .
C7 Si3 Ge1 110.93(11) .
C9 Si3 Ge1 110.95(11) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ge1 Si1 2.3765(13) .
Ge1 Si2 2.3838(11) .
Ge1 Si3 2.3866(10) .
Ge1 Ge2 2.4409(14) .
Ge2 C10 1.963(3) .
Ge2 C11 1.973(3) .
Ge2 Ge2 2.4418(9) 2_766
Si1 C1 1.866(3) .
Si1 C2 1.873(3) .
Si1 C3 1.881(3) .
Si2 C6 1.866(3) .
Si2 C5 1.873(3) .
Si2 C4 1.878(3) .
Si3 C8 1.875(3) .
Si3 C7 1.876(3) .
Si3 C9 1.878(3) .
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
Si1 Ge1 Ge2 C10 84.10(11) .
Si2 Ge1 Ge2 C10 -151.86(11) .
Si3 Ge1 Ge2 C10 -35.89(11) .
Si1 Ge1 Ge2 C11 -161.98(11) .
Si2 Ge1 Ge2 C11 -37.94(11) .
Si3 Ge1 Ge2 C11 78.03(11) .
Si1 Ge1 Ge2 Ge2 -39.40(4) 2_766
Si2 Ge1 Ge2 Ge2 84.64(4) 2_766
Si3 Ge1 Ge2 Ge2 -159.39(3) 2_766
Si2 Ge1 Si1 C1 -49.39(12) .
Si3 Ge1 Si1 C1 -165.81(11) .
Ge2 Ge1 Si1 C1 75.30(12) .
Si2 Ge1 Si1 C2 -172.29(11) .
Si3 Ge1 Si1 C2 71.29(12) .
Ge2 Ge1 Si1 C2 -47.61(12) .
Si2 Ge1 Si1 C3 68.75(13) .
Si3 Ge1 Si1 C3 -47.67(13) .
Ge2 Ge1 Si1 C3 -166.57(12) .
Si1 Ge1 Si2 C6 77.52(12) .
Si3 Ge1 Si2 C6 -164.75(12) .
Ge2 Ge1 Si2 C6 -48.68(12) .
Si1 Ge1 Si2 C5 -161.25(12) .
Si3 Ge1 Si2 C5 -43.53(13) .
Ge2 Ge1 Si2 C5 72.54(13) .
Si1 Ge1 Si2 C4 -42.11(12) .
Si3 Ge1 Si2 C4 75.62(12) .
Ge2 Ge1 Si2 C4 -168.31(11) .
Si1 Ge1 Si3 C8 74.69(13) .
Si2 Ge1 Si3 C8 -43.62(13) .
Ge2 Ge1 Si3 C8 -162.33(12) .
Si1 Ge1 Si3 C7 -165.84(12) .
Si2 Ge1 Si3 C7 75.85(13) .
Ge2 Ge1 Si3 C7 -42.86(12) .
Si1 Ge1 Si3 C9 -44.22(13) .
Si2 Ge1 Si3 C9 -162.52(12) .
Ge2 Ge1 Si3 C9 78.77(12) .
