#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:36:45 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178787 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/41/4104163.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_4104163
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 Ge2 Si8'
_chemical_formula_weight         700.65
_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                103.20(3)
_cell_angle_beta                 91.95(3)
_cell_angle_gamma                114.33(3)
_cell_formula_units_Z            1
_cell_length_a                   9.1381(18)
_cell_length_b                   9.1761(18)
_cell_length_c                   13.632(3)
_cell_measurement_reflns_used    3504
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.546
_cell_measurement_theta_min      4.911
_cell_volume                     1003.4(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 0.974
_diffrn_measured_fraction_theta_max 0.974
_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  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0487
_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       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7916
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    1.747
_exptl_absorpt_correction_T_max  0.6791
_exptl_absorpt_correction_T_min  0.5273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             374
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.063
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         4009
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0298P)²+7.1485P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1191
_reflns_number_gt                3375
_reflns_number_total             4009
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja809270m_si_001_1.cif
_cod_data_source_block           6_271j
_cod_original_cell_volume        1003.4(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4104163
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 0.69739(5) 0.15527(5) 0.21854(3) 0.01514(13) Uani 1 1 d .
Si1 Si 0.52379(14) -0.05050(14) 0.06898(9) 0.0182(3) Uani 1 1 d .
Si2 Si 0.92653(14) 0.37657(15) 0.18666(9) 0.0186(3) Uani 1 1 d .
Si3 Si 0.79598(15) 0.01580(15) 0.31324(9) 0.0202(3) Uani 1 1 d .
Si4 Si 0.55018(14) 0.26831(15) 0.32820(9) 0.0190(3) Uani 1 1 d .
C1 C 0.3252(5) -0.1663(6) 0.1142(4) 0.0257(10) Uani 1 1 d .
H1A H 0.2525 -0.2601 0.0581 0.039 Uiso 1 1 calc R
H1B H 0.2745 -0.0913 0.1368 0.039 Uiso 1 1 calc R
H1C H 0.3460 -0.2074 0.1709 0.039 Uiso 1 1 calc R
C2 C 0.6146(6) -0.2006(6) 0.0233(4) 0.0282(10) Uani 1 1 d .
H2A H 0.6333 -0.2442 0.0794 0.042 Uiso 1 1 calc R
H2B H 0.7180 -0.1431 -0.0002 0.042 Uiso 1 1 calc R
H2C H 0.5398 -0.2923 -0.0330 0.042 Uiso 1 1 calc R
C3 C 0.8616(6) 0.5252(6) 0.1454(4) 0.0269(10) Uani 1 1 d .
H12A H 0.9544 0.6099 0.1259 0.040 Uiso 1 1 calc R
H12B H 0.8214 0.5786 0.2018 0.040 Uiso 1 1 calc R
H12C H 0.7750 0.4646 0.0871 0.040 Uiso 1 1 calc R
C4 C 1.0776(5) 0.4968(6) 0.3053(4) 0.0291(10) Uani 1 1 d .
H11A H 1.1150 0.4232 0.3290 0.044 Uiso 1 1 calc R
H11B H 1.0264 0.5423 0.3582 0.044 Uiso 1 1 calc R
H11C H 1.1704 0.5878 0.2906 0.044 Uiso 1 1 calc R
C5 C 1.0326(6) 0.2935(6) 0.0892(4) 0.0278(10) Uani 1 1 d .
H13A H 0.9565 0.2276 0.0263 0.042 Uiso 1 1 calc R
H13B H 1.0724 0.2234 0.1153 0.042 Uiso 1 1 calc R
H13C H 1.1244 0.3861 0.0752 0.042 Uiso 1 1 calc R
C6 C 0.8765(6) 0.1450(6) 0.4488(4) 0.0284(10) Uani 1 1 d .
H7A H 0.9272 0.0922 0.4844 0.043 Uiso 1 1 calc R
H7B H 0.7870 0.1539 0.4833 0.043 Uiso 1 1 calc R
H7C H 0.9573 0.2561 0.4493 0.043 Uiso 1 1 calc R
C7 C 0.9670(6) -0.0203(6) 0.2562(4) 0.0301(11) Uani 1 1 d .
H5A H 1.0612 0.0865 0.2647 0.045 Uiso 1 1 calc R
H5B H 0.9323 -0.0770 0.1835 0.045 Uiso 1 1 calc R
H5C H 0.9966 -0.0891 0.2907 0.045 Uiso 1 1 calc R
C8 C 0.6299(6) -0.1899(6) 0.3158(4) 0.0287(10) Uani 1 1 d .
H6A H 0.5898 -0.2615 0.2461 0.043 Uiso 1 1 calc R
H6B H 0.5407 -0.1724 0.3461 0.043 Uiso 1 1 calc R
H6C H 0.6726 -0.2428 0.3564 0.043 Uiso 1 1 calc R
C9 C 0.4157(6) 0.1127(6) 0.3930(4) 0.0306(11) Uani 1 1 d .
H8A H 0.3491 0.1579 0.4325 0.046 Uiso 1 1 calc R
H8B H 0.4829 0.0888 0.4387 0.046 Uiso 1 1 calc R
H8C H 0.3450 0.0101 0.3417 0.046 Uiso 1 1 calc R
C10 C 0.4207(6) 0.3347(6) 0.2573(4) 0.0250(10) Uani 1 1 d .
H10A H 0.3375 0.2375 0.2077 0.038 Uiso 1 1 calc R
H10B H 0.4883 0.4140 0.2216 0.038 Uiso 1 1 calc R
H10C H 0.3682 0.3873 0.3053 0.038 Uiso 1 1 calc R
C11 C 0.6961(6) 0.4552(6) 0.4296(4) 0.0285(10) Uani 1 1 d .
H9A H 0.7616 0.5419 0.3978 0.043 Uiso 1 1 calc R
H9B H 0.7675 0.4241 0.4667 0.043 Uiso 1 1 calc R
H9C H 0.6353 0.4970 0.4770 0.043 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_1
_geom_angle_site_symmetry_3
Si2 Ge1 Si4 108.97(5) . .
Si2 Ge1 Si3 107.64(5) . .
Si4 Ge1 Si3 105.82(5) . .
Si2 Ge1 Si1 115.16(5) . .
Si4 Ge1 Si1 111.72(5) . .
Si3 Ge1 Si1 107.01(5) . .
C2 Si1 C1 108.0(2) . .
C2 Si1 Si1 108.80(17) . 2_655
C1 Si1 Si1 110.07(16) . 2_655
C2 Si1 Ge1 108.13(16) . .
C1 Si1 Ge1 105.28(15) . .
Si1 Si1 Ge1 116.24(8) 2_655 .
C4 Si2 C5 107.1(2) . .
C4 Si2 C3 107.0(2) . .
C5 Si2 C3 111.5(2) . .
C4 Si2 Ge1 110.85(16) . .
C5 Si2 Ge1 110.40(16) . .
C3 Si2 Ge1 109.87(15) . .
C7 Si3 C6 107.6(2) . .
C7 Si3 C8 108.8(2) . .
C6 Si3 C8 108.0(2) . .
C7 Si3 Ge1 110.77(16) . .
C6 Si3 Ge1 110.51(16) . .
C8 Si3 Ge1 111.13(16) . .
C10 Si4 C9 108.3(2) . .
C10 Si4 C11 107.9(2) . .
C9 Si4 C11 108.0(2) . .
C10 Si4 Ge1 111.84(15) . .
C9 Si4 Ge1 110.98(17) . .
C11 Si4 Ge1 109.70(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ge1 Si2 2.3787(16) .
Ge1 Si4 2.3872(14) .
Ge1 Si3 2.3961(14) .
Ge1 Si1 2.4067(18) .
Si1 C2 1.886(5) .
Si1 C1 1.894(5) .
Si1 Si1 2.379(2) 2_655
Si2 C4 1.875(5) .
Si2 C5 1.876(5) .
Si2 C3 1.877(5) .
Si3 C7 1.884(5) .
Si3 C6 1.885(5) .
Si3 C8 1.882(5) .
Si4 C10 1.868(5) .
Si4 C9 1.880(5) .
Si4 C11 1.881(5) .
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
Si2 Ge1 Si1 C2 82.43(17) .
Si4 Ge1 Si1 C2 -152.56(17) .
Si3 Ge1 Si1 C2 -37.16(17) .
Si2 Ge1 Si1 C1 -162.29(16) .
Si4 Ge1 Si1 C1 -37.28(17) .
Si3 Ge1 Si1 C1 78.11(17) .
Si2 Ge1 Si1 Si1 -40.20(10) 2_655
Si4 Ge1 Si1 Si1 84.81(9) 2_655
Si3 Ge1 Si1 Si1 -159.80(8) 2_655
Si4 Ge1 Si2 C4 67.90(18) .
Si3 Ge1 Si2 C4 -46.42(18) .
Si1 Ge1 Si2 C4 -165.67(18) .
Si4 Ge1 Si2 C5 -173.63(16) .
Si3 Ge1 Si2 C5 72.04(17) .
Si1 Ge1 Si2 C5 -47.20(17) .
Si4 Ge1 Si2 C3 -50.21(18) .
Si3 Ge1 Si2 C3 -164.54(17) .
Si1 Ge1 Si2 C3 76.21(18) .
Si2 Ge1 Si3 C7 -45.39(18) .
Si4 Ge1 Si3 C7 -161.79(18) .
Si1 Ge1 Si3 C7 78.94(18) .
Si2 Ge1 Si3 C6 73.72(18) .
Si4 Ge1 Si3 C6 -42.69(18) .
Si1 Ge1 Si3 C6 -161.96(18) .
Si2 Ge1 Si3 C8 -166.42(18) .
Si4 Ge1 Si3 C8 77.17(18) .
Si1 Ge1 Si3 C8 -42.10(18) .
Si2 Ge1 Si4 C10 79.06(18) .
Si3 Ge1 Si4 C10 -165.44(17) .
Si1 Ge1 Si4 C10 -49.32(18) .
Si2 Ge1 Si4 C9 -159.93(18) .
Si3 Ge1 Si4 C9 -44.43(18) .
Si1 Ge1 Si4 C9 71.69(18) .
Si2 Ge1 Si4 C11 -40.67(18) .
Si3 Ge1 Si4 C11 74.83(18) .
Si1 Ge1 Si4 C11 -169.06(18) .
