#------------------------------------------------------------------------------
#$Date: 2022-06-17 01:56:31 +0300 (Fri, 17 Jun 2022) $
#$Revision: 276073 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/05/7710511.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_7710511
loop_
_publ_author_name
'Wohltmann, Wiebke Marie'
'Schmidtmann, Marc'
'Müller, Thomas'
_publ_section_title
;
 Covalent triflates as synthons for silolyl- and germolyl cations
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01446G
_journal_year                    2022
_chemical_formula_structural     GeClC4(CH3)2(Si(CH3)3)2(C6H5)
_chemical_formula_sum            'C18 H29 Cl Ge Si2'
_chemical_formula_weight         409.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-05-03 deposited with the CCDC.	2022-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.931(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1665(12)
_cell_length_b                   6.7319(5)
_cell_length_c                   19.8527(14)
_cell_measurement_reflns_used    9339
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.05
_cell_measurement_theta_min      2.56
_cell_volume                     2128.2(3)
_computing_cell_refinement       'Bruker SAINT V8.40A'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT V8.40A'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Photon III CPAD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            69223
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.033
_diffrn_reflns_theta_min         1.503
_diffrn_source                   'I\mS microfocus'
_exptl_absorpt_coefficient_mu    1.673
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.069
_refine_diff_density_min         -1.075
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.236
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         6239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.236
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0678
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0400P)²+14.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1669
_refine_ls_wR_factor_ref         0.1709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5522
_reflns_number_total             6239
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt01446g3.cif
_cod_data_source_block           ww69
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7710511
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_min   0.851
_shelx_estimated_absorpt_t_max   0.921
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.46978(3) 0.41451(7) 0.20827(2) 0.01643(12) Uani 1 1 d . . . . .
Cl1 Cl 0.46088(8) 0.73161(16) 0.22724(6) 0.0276(2) Uani 1 1 d . . . . .
Si1 Si 0.35265(8) 0.38494(19) 0.05043(6) 0.0204(2) Uani 1 1 d . . . . .
Si2 Si 0.49487(7) 0.25927(18) 0.37313(6) 0.0184(2) Uani 1 1 d . . . . .
C1 C 0.3756(2) 0.3190(6) 0.1428(2) 0.0175(8) Uani 1 1 d . . . . .
C2 C 0.3370(2) 0.1887(6) 0.1784(2) 0.0171(7) Uani 1 1 d . . . . .
C3 C 0.3677(3) 0.1681(6) 0.2549(2) 0.0167(7) Uani 1 1 d . . . . .
C4 C 0.4374(3) 0.2680(6) 0.2832(2) 0.0167(7) Uani 1 1 d . . . . .
C5 C 0.2655(3) 0.0544(7) 0.1466(2) 0.0257(9) Uani 1 1 d . . . . .
H5A H 0.215775 0.082271 0.167094 0.039 Uiso 1 1 calc R U . . .
H5B H 0.282053 -0.084707 0.154819 0.039 Uiso 1 1 calc R U . . .
H5C H 0.252488 0.078932 0.097220 0.039 Uiso 1 1 calc R U . . .
C6 C 0.3172(3) 0.0357(7) 0.2939(2) 0.0215(8) Uani 1 1 d . . . . .
H6A H 0.341934 0.037464 0.342566 0.032 Uiso 1 1 calc R U . . .
H6B H 0.317599 -0.100352 0.276434 0.032 Uiso 1 1 calc R U . . .
H6C H 0.259219 0.084164 0.287993 0.032 Uiso 1 1 calc R U . . .
C7 C 0.4160(4) 0.6107(8) 0.0387(3) 0.0328(11) Uani 1 1 d . . . . .
H7A H 0.475587 0.583140 0.054952 0.049 Uiso 1 1 calc R U . . .
H7B H 0.398038 0.721352 0.064852 0.049 Uiso 1 1 calc R U . . .
H7C H 0.407471 0.646069 -0.009909 0.049 Uiso 1 1 calc R U . . .
C8 C 0.2404(3) 0.4535(11) 0.0233(3) 0.0426(15) Uani 1 1 d . . . . .
H8A H 0.230875 0.494168 -0.024822 0.064 Uiso 1 1 calc R U . . .
H8B H 0.226331 0.563650 0.051544 0.064 Uiso 1 1 calc R U . . .
H8C H 0.204885 0.338766 0.028858 0.064 Uiso 1 1 calc R U . . .
C9 C 0.3806(4) 0.1769(8) -0.0022(3) 0.0349(12) Uani 1 1 d . . . . .
H9A H 0.440563 0.146929 0.010846 0.052 Uiso 1 1 calc R U . . .
H9C H 0.368489 0.214118 -0.050625 0.052 Uiso 1 1 calc R U . . .
H9B H 0.347609 0.059317 0.005282 0.052 Uiso 1 1 calc R U . . .
C10 C 0.5921(3) 0.4118(9) 0.3787(3) 0.0347(11) Uani 1 1 d . . . . .
H10A H 0.627280 0.357746 0.347569 0.052 Uiso 1 1 calc R U . . .
H10B H 0.623163 0.408599 0.425666 0.052 Uiso 1 1 calc R U . . .
H10C H 0.576833 0.549259 0.365850 0.052 Uiso 1 1 calc R U . . .
C11 C 0.4294(3) 0.3635(8) 0.4336(2) 0.0256(9) Uani 1 1 d . . . . .
H11A H 0.420440 0.505754 0.424689 0.038 Uiso 1 1 calc R U . . .
H11B H 0.458415 0.344305 0.480747 0.038 Uiso 1 1 calc R U . . .
H11C H 0.375105 0.295196 0.427152 0.038 Uiso 1 1 calc R U . . .
C12 C 0.5252(3) -0.0010(7) 0.3977(3) 0.0305(11) Uani 1 1 d . . . . .
H12A H 0.474550 -0.082076 0.395856 0.046 Uiso 1 1 calc R U . . .
H12B H 0.557529 -0.003006 0.444239 0.046 Uiso 1 1 calc R U . . .
H12C H 0.559623 -0.054954 0.365889 0.046 Uiso 1 1 calc R U . . .
C13 C 0.5815(3) 0.3727(7) 0.1871(2) 0.0186(8) Uani 1 1 d . . . . .
C14 C 0.6026(3) 0.1851(7) 0.1690(3) 0.0267(9) Uani 1 1 d . . . . .
H14 H 0.562615 0.080721 0.166014 0.032 Uiso 1 1 calc R U . . .
C15 C 0.6830(3) 0.1476(9) 0.1550(3) 0.0342(11) Uani 1 1 d . . . . .
H15 H 0.697761 0.017609 0.142634 0.041 Uiso 1 1 calc R U . . .
C16 C 0.7409(3) 0.3002(10) 0.1591(3) 0.0342(12) Uani 1 1 d . . . . .
H16 H 0.795765 0.275011 0.150076 0.041 Uiso 1 1 calc R U . . .
C17 C 0.7190(3) 0.4879(9) 0.1761(3) 0.0350(12) Uani 1 1 d . . . . .
H17 H 0.758553 0.592915 0.178083 0.042 Uiso 1 1 calc R U . . .
C18 C 0.6397(3) 0.5257(8) 0.1905(3) 0.0270(10) Uani 1 1 d . . . . .
H18 H 0.625140 0.655955 0.202649 0.032 Uiso 1 1 calc R U . . .
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
C4 Ge1 C1 93.52(17) . . ?
C4 Ge1 C13 118.55(17) . . ?
C1 Ge1 C13 117.37(18) . . ?
C4 Ge1 Cl1 109.45(13) . . ?
C1 Ge1 Cl1 111.99(13) . . ?
C13 Ge1 Cl1 105.72(14) . . ?
C9 Si1 C8 110.2(3) . . ?
C9 Si1 C1 110.5(2) . . ?
C8 Si1 C1 111.3(2) . . ?
C9 Si1 C7 110.7(3) . . ?
C8 Si1 C7 106.9(3) . . ?
C1 Si1 C7 107.2(2) . . ?
C12 Si2 C10 108.7(2) . . ?
C12 Si2 C4 110.2(2) . . ?
C10 Si2 C4 108.4(2) . . ?
C12 Si2 C11 109.8(3) . . ?
C10 Si2 C11 108.6(2) . . ?
C4 Si2 C11 111.0(2) . . ?
C2 C1 Si1 129.9(3) . . ?
C2 C1 Ge1 104.2(3) . . ?
Si1 C1 Ge1 125.7(2) . . ?
C1 C2 C5 123.9(4) . . ?
C1 C2 C3 118.9(4) . . ?
C5 C2 C3 117.1(4) . . ?
C4 C3 C6 124.6(4) . . ?
C4 C3 C2 118.4(4) . . ?
C6 C3 C2 117.0(3) . . ?
C3 C4 Si2 128.7(3) . . ?
C3 C4 Ge1 104.6(3) . . ?
Si2 C4 Ge1 126.6(2) . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si1 C8 H8A 109.5 . . ?
Si1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si1 C9 H9A 109.5 . . ?
Si1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
Si1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9C C9 H9B 109.5 . . ?
Si2 C10 H10A 109.5 . . ?
Si2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si2 C11 H11A 109.5 . . ?
Si2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si2 C12 H12A 109.5 . . ?
Si2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C18 119.9(4) . . ?
C14 C13 Ge1 118.2(3) . . ?
C18 C13 Ge1 121.9(4) . . ?
C13 C14 C15 120.0(5) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C16 C15 C14 119.8(5) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C17 C16 C15 119.9(5) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C16 C17 C18 120.6(5) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 H17 119.7 . . ?
C17 C18 C13 119.8(5) . . ?
C17 C18 H18 120.1 . . ?
C13 C18 H18 120.1 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 C4 1.931(4) . ?
Ge1 C1 1.933(4) . ?
Ge1 C13 1.944(4) . ?
Ge1 Cl1 2.1767(12) . ?
Si1 C9 1.850(5) . ?
Si1 C8 1.860(5) . ?
Si1 C1 1.861(4) . ?
Si1 C7 1.869(6) . ?
Si2 C12 1.862(5) . ?
Si2 C10 1.864(5) . ?
Si2 C4 1.866(4) . ?
Si2 C11 1.869(5) . ?
C1 C2 1.346(6) . ?
C2 C5 1.517(6) . ?
C2 C3 1.520(6) . ?
C3 C4 1.348(6) . ?
C3 C6 1.509(6) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9C 0.9800 . ?
C9 H9B 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.372(6) . ?
C13 C18 1.389(6) . ?
C14 C15 1.398(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.383(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.370(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.384(7) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
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
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 Si1 C1 C2 -70.5(5) . . . . ?
C8 Si1 C1 C2 52.3(5) . . . . ?
C7 Si1 C1 C2 168.9(4) . . . . ?
C9 Si1 C1 Ge1 104.2(3) . . . . ?
C8 Si1 C1 Ge1 -133.0(3) . . . . ?
C7 Si1 C1 Ge1 -16.5(3) . . . . ?
Si1 C1 C2 C5 3.6(7) . . . . ?
Ge1 C1 C2 C5 -171.9(4) . . . . ?
Si1 C1 C2 C3 -178.3(3) . . . . ?
Ge1 C1 C2 C3 6.2(5) . . . . ?
C1 C2 C3 C4 -6.0(6) . . . . ?
C5 C2 C3 C4 172.2(4) . . . . ?
C1 C2 C3 C6 174.0(4) . . . . ?
C5 C2 C3 C6 -7.8(6) . . . . ?
C6 C3 C4 Si2 5.0(7) . . . . ?
C2 C3 C4 Si2 -175.0(3) . . . . ?
C6 C3 C4 Ge1 -178.2(3) . . . . ?
C2 C3 C4 Ge1 1.8(4) . . . . ?
C12 Si2 C4 C3 55.7(5) . . . . ?
C10 Si2 C4 C3 174.6(4) . . . . ?
C11 Si2 C4 C3 -66.2(5) . . . . ?
C12 Si2 C4 Ge1 -120.5(3) . . . . ?
C10 Si2 C4 Ge1 -1.6(4) . . . . ?
C11 Si2 C4 Ge1 117.7(3) . . . . ?
C18 C13 C14 C15 0.9(7) . . . . ?
Ge1 C13 C14 C15 -178.5(4) . . . . ?
C13 C14 C15 C16 -0.3(8) . . . . ?
C14 C15 C16 C17 -0.7(9) . . . . ?
C15 C16 C17 C18 1.1(9) . . . . ?
C16 C17 C18 C13 -0.5(8) . . . . ?
C14 C13 C18 C17 -0.5(7) . . . . ?
Ge1 C13 C18 C17 178.9(4) . . . . ?
