#------------------------------------------------------------------------------
#$Date: 2015-12-13 04:45:11 +0200 (Sun, 13 Dec 2015) $
#$Revision: 171478 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/13/2241396.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2241396
loop_
_publ_author_name
'Zaitsev, Kirill V.'
'Zaitseva, Galina S.'
'Karlov, Sergey S.'
'Korlyukov, Alexander A.'
_publ_section_title
;
 Crystal structure of (tert-butyldimethylsilyl)triphenylgermane,
 Ph₃Ge-SiMe₂(t-Bu)
;
_journal_coeditor_code           IM2474
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1015
_journal_page_last               o1016
_journal_paper_doi               10.1107/S2056989015022872
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C24 H30 Ge Si'
_chemical_formula_moiety         'C24 H30 Ge Si'
_chemical_formula_sum            'C24 H30 Ge Si'
_chemical_formula_weight         419.16
_chemical_name_systematic
;
(tert-Butyldimethylsilyl)triphenylgermane
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.2048(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.5332(6)
_cell_length_b                   14.9825(7)
_cell_length_c                   22.7179(13)
_cell_measurement_reflns_used    8565
_cell_measurement_temperature    120
_cell_measurement_theta_max      31.69
_cell_measurement_theta_min      2.45
_cell_volume                     4423.3(4)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS2014 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD area-detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            32242
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.638
_diffrn_reflns_theta_min         1.867
_exptl_absorpt_coefficient_mu    1.444
_exptl_absorpt_correction_T_max  0.8623
_exptl_absorpt_correction_T_min  0.7195
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2013)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.373
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         7990
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0303P)²+1.8636P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0709
_reflns_number_gt                6137
_reflns_number_total             7990
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            im2474sup1.cif
_cod_data_source_block           I
_cod_database_code               2241396
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Ge Ge1 0.36354(2) 0.03558(2) 0.37248(2) 0.01369(4) Uani d 1
Si Si1 0.26294(3) 0.07258(3) 0.27044(2) 0.01566(8) Uani d 1
C C1 0.19468(11) -0.02626(9) 0.22333(7) 0.0193(3) Uani d 1
C C2 0.14760(13) -0.08808(11) 0.26222(8) 0.0280(3) Uani d 1
H H2A 0.2015 -0.1135 0.2947 0.042 Uiso calc 1
H H2B 0.1099 -0.1350 0.2369 0.042 Uiso calc 1
H H2C 0.1020 -0.0544 0.2794 0.042 Uiso calc 1
C C3 0.10842(13) 0.00982(12) 0.16951(8) 0.0286(4) Uani d 1
H H3A 0.0582 0.0399 0.1849 0.043 Uiso calc 1
H H3B 0.0763 -0.0388 0.1437 0.043 Uiso calc 1
H H3C 0.1368 0.0509 0.1462 0.043 Uiso calc 1
C C4 0.26903(13) -0.08070(11) 0.19725(8) 0.0293(4) Uani d 1
H H4A 0.2967 -0.0432 0.1715 0.044 Uiso calc 1
H H4B 0.2327 -0.1298 0.1737 0.044 Uiso calc 1
H H4C 0.3241 -0.1032 0.2303 0.044 Uiso calc 1
C C5 0.16501(12) 0.15374(11) 0.28177(8) 0.0288(4) Uani d 1
H H5A 0.1152 0.1229 0.2971 0.043 Uiso calc 1
H H5B 0.1311 0.1814 0.2433 0.043 Uiso calc 1
H H5C 0.1984 0.1986 0.3107 0.043 Uiso calc 1
C C6 0.34687(14) 0.13018(13) 0.22957(8) 0.0340(4) Uani d 1
H H6A 0.3806 0.1798 0.2536 0.051 Uiso calc 1
H H6B 0.3056 0.1512 0.1905 0.051 Uiso calc 1
H H6C 0.3976 0.0891 0.2235 0.051 Uiso calc 1
C C7 0.48101(10) 0.11767(9) 0.39511(6) 0.0160(3) Uani d 1
C C8 0.46614(12) 0.20997(10) 0.38666(7) 0.0244(3) Uani d 1
H H8 0.3997 0.2322 0.3713 0.029 Uiso calc 1
C C9 0.54855(13) 0.26859(11) 0.40074(8) 0.0287(4) Uani d 1
H H9 0.5371 0.3295 0.3948 0.034 Uiso calc 1
C C10 0.64792(12) 0.23684(11) 0.42370(7) 0.0258(3) Uani d 1
H H10 0.7032 0.2763 0.4332 0.031 Uiso calc 1
C C11 0.66436(11) 0.14632(11) 0.43231(7) 0.0223(3) Uani d 1
H H11 0.7310 0.1247 0.4475 0.027 Uiso calc 1
C C12 0.58171(11) 0.08718(10) 0.41835(6) 0.0185(3) Uani d 1
H H12 0.5939 0.0264 0.4246 0.022 Uiso calc 1
C C13 0.28202(11) 0.05273(9) 0.43088(6) 0.0159(3) Uani d 1
C C14 0.19262(11) 0.00334(10) 0.42642(7) 0.0210(3) Uani d 1
H H14 0.1719 -0.0391 0.3956 0.025 Uiso calc 1
C C15 0.13399(12) 0.01638(11) 0.46710(7) 0.0254(3) Uani d 1
H H15 0.0750 -0.0174 0.4635 0.031 Uiso calc 1
C C16 0.16361(12) 0.07993(11) 0.51311(7) 0.0252(3) Uani d 1
H H16 0.1242 0.0891 0.5402 0.030 Uiso calc 1
C C17 0.25164(12) 0.12936(11) 0.51847(7) 0.0251(3) Uani d 1
H H17 0.2717 0.1719 0.5494 0.030 Uiso calc 1
C C18 0.31062(11) 0.11602(10) 0.47793(7) 0.0203(3) Uani d 1
H H18 0.3700 0.1497 0.4821 0.024 Uiso calc 1
C C19 0.41975(10) -0.08517(9) 0.38053(6) 0.0151(3) Uani d 1
C C20 0.47948(11) -0.11181(10) 0.34217(7) 0.0192(3) Uani d 1
H H20 0.4907 -0.0719 0.3134 0.023 Uiso calc 1
C C21 0.52196(12) -0.19630(10) 0.34629(7) 0.0238(3) Uani d 1
H H21 0.5611 -0.2128 0.3203 0.029 Uiso calc 1
C C22 0.50633(12) -0.25642(10) 0.38912(7) 0.0250(3) Uani d 1
H H22 0.5351 -0.3132 0.3921 0.030 Uiso calc 1
C C23 0.44760(12) -0.23154(10) 0.42747(7) 0.0247(3) Uani d 1
H H23 0.4366 -0.2718 0.4561 0.030 Uiso calc 1
C C24 0.40487(11) -0.14636(10) 0.42328(7) 0.0194(3) Uani d 1
H H24 0.3659 -0.1302 0.4494 0.023 Uiso calc 1
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
C7 Ge1 Si1 107.93(4)
C7 Ge1 C13 107.92(6)
C13 Ge1 Si1 110.34(4)
C19 Ge1 Si1 113.92(4)
C19 Ge1 C7 106.89(6)
C19 Ge1 C13 109.61(6)
C1 Si1 Ge1 114.67(5)
C5 Si1 Ge1 104.47(5)
C5 Si1 C1 109.35(7)
C6 Si1 Ge1 109.08(6)
C6 Si1 C1 110.26(7)
C6 Si1 C5 108.72(9)
C2 C1 Si1 111.05(10)
C2 C1 C4 108.84(13)
C3 C1 Si1 108.38(10)
C3 C1 C2 109.00(13)
C3 C1 C4 108.31(13)
C4 C1 Si1 111.20(10)
C1 C2 H2A 109.5
C1 C2 H2B 109.5
C1 C2 H2C 109.5
H2A C2 H2B 109.5
H2A C2 H2C 109.5
H2B C2 H2C 109.5
C1 C3 H3A 109.5
C1 C3 H3B 109.5
C1 C3 H3C 109.5
H3A C3 H3B 109.5
H3A C3 H3C 109.5
H3B C3 H3C 109.5
C1 C4 H4A 109.5
C1 C4 H4B 109.5
C1 C4 H4C 109.5
H4A C4 H4B 109.5
H4A C4 H4C 109.5
H4B C4 H4C 109.5
Si1 C5 H5A 109.5
Si1 C5 H5B 109.5
Si1 C5 H5C 109.5
H5A C5 H5B 109.5
H5A C5 H5C 109.5
H5B C5 H5C 109.5
Si1 C6 H6A 109.5
Si1 C6 H6B 109.5
Si1 C6 H6C 109.5
H6A C6 H6B 109.5
H6A C6 H6C 109.5
H6B C6 H6C 109.5
C8 C7 Ge1 120.48(11)
C12 C7 Ge1 121.93(11)
C12 C7 C8 117.57(13)
C7 C8 H8 119.4
C9 C8 C7 121.19(15)
C9 C8 H8 119.4
C8 C9 H9 119.9
C10 C9 C8 120.28(15)
C10 C9 H9 119.9
C9 C10 H10 120.2
C11 C10 C9 119.52(14)
C11 C10 H10 120.2
C10 C11 H11 119.8
C10 C11 C12 120.39(14)
C12 C11 H11 119.8
C7 C12 H12 119.5
C11 C12 C7 121.06(14)
C11 C12 H12 119.5
C14 C13 Ge1 121.31(10)
C14 C13 C18 117.60(13)
C18 C13 Ge1 121.09(11)
C13 C14 H14 119.3
C15 C14 C13 121.38(14)
C15 C14 H14 119.3
C14 C15 H15 120.0
C16 C15 C14 119.93(15)
C16 C15 H15 120.0
C15 C16 H16 120.1
C17 C16 C15 119.72(14)
C17 C16 H16 120.1
C16 C17 H17 119.8
C16 C17 C18 120.36(14)
C18 C17 H17 119.8
C13 C18 H18 119.5
C17 C18 C13 121.01(14)
C17 C18 H18 119.5
C20 C19 Ge1 118.88(10)
C24 C19 Ge1 123.24(10)
C24 C19 C20 117.87(13)
C19 C20 H20 119.3
C21 C20 C19 121.30(14)
C21 C20 H20 119.3
C20 C21 H21 120.0
C20 C21 C22 120.06(14)
C22 C21 H21 120.0
C21 C22 H22 120.2
C23 C22 C21 119.62(14)
C23 C22 H22 120.2
C22 C23 H23 119.9
C22 C23 C24 120.25(14)
C24 C23 H23 119.9
C19 C24 C23 120.90(14)
C19 C24 H24 119.6
C23 C24 H24 119.6
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ge1 Si1 2.4026(4)
Ge1 C7 1.9618(14)
Ge1 C13 1.9648(14)
Ge1 C19 1.9512(13)
Si1 C1 1.9078(15)
Si1 C5 1.8687(15)
Si1 C6 1.8670(17)
C1 C2 1.536(2)
C1 C3 1.534(2)
C1 C4 1.537(2)
C2 H2A 0.9600
C2 H2B 0.9600
C2 H2C 0.9600
C3 H3A 0.9600
C3 H3B 0.9600
C3 H3C 0.9600
C4 H4A 0.9600
C4 H4B 0.9600
C4 H4C 0.9600
C5 H5A 0.9600
C5 H5B 0.9600
C5 H5C 0.9600
C6 H6A 0.9600
C6 H6B 0.9600
C6 H6C 0.9600
C7 C8 1.403(2)
C7 C12 1.3939(19)
C8 H8 0.9300
C8 C9 1.385(2)
C9 H9 0.9300
C9 C10 1.384(2)
C10 H10 0.9300
C10 C11 1.379(2)
C11 H11 0.9300
C11 C12 1.393(2)
C12 H12 0.9300
C13 C14 1.398(2)
C13 C18 1.400(2)
C14 H14 0.9300
C14 C15 1.389(2)
C15 H15 0.9300
C15 C16 1.388(2)
C16 H16 0.9300
C16 C17 1.379(2)
C17 H17 0.9300
C17 C18 1.391(2)
C18 H18 0.9300
C19 C20 1.4019(19)
C19 C24 1.390(2)
C20 H20 0.9300
C20 C21 1.383(2)
C21 H21 0.9300
C21 C22 1.385(2)
C22 H22 0.9300
C22 C23 1.384(2)
C23 H23 0.9300
C23 C24 1.393(2)
C24 H24 0.9300
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
Ge1 C7 C8 C9 -178.11(13)
Ge1 C7 C12 C11 177.92(11)
Ge1 C13 C14 C15 -178.96(12)
Ge1 C13 C18 C17 178.66(12)
Ge1 C19 C20 C21 179.40(11)
Ge1 C19 C24 C23 -179.38(11)
C7 C8 C9 C10 -0.1(3)
C8 C7 C12 C11 -0.3(2)
C8 C9 C10 C11 0.2(2)
C9 C10 C11 C12 -0.3(2)
C10 C11 C12 C7 0.4(2)
C12 C7 C8 C9 0.2(2)
C13 C14 C15 C16 0.4(2)
C14 C13 C18 C17 -0.3(2)
C14 C15 C16 C17 -0.5(3)
C15 C16 C17 C18 0.2(2)
C16 C17 C18 C13 0.2(2)
C18 C13 C14 C15 0.0(2)
C19 C20 C21 C22 -0.3(2)
C20 C19 C24 C23 -0.4(2)
C20 C21 C22 C23 0.3(2)
C21 C22 C23 C24 -0.3(2)
C22 C23 C24 C19 0.4(2)
C24 C19 C20 C21 0.3(2)

_cod_database_fobs_code 2241396
