#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:14:33 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179833 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/29/7012911.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_7012911
loop_
_publ_author_name
'Andrei S. Batsanov'
'Stéphanie M. Cornet'
'Keith B. Dillon'
'Andrés E. Goeta'
'Amber L. Thompson'
'Bao Yu Xue'
_publ_section_title
;
 The synthesis and characterisation of some Group 14 compounds
 containing the 2,4,6-(CF3)3C6H2, 2,6-(CF3)2C6H3 or 2,4-(CF3)2C6H3
 ligands
;
_journal_issue                   12
_journal_name_full               'Dalton Trans.'
_journal_page_first              2496
_journal_page_last               2502
_journal_paper_doi               10.1039/b302544f
_journal_year                    2003
_chemical_formula_moiety         'C18 H4 Cl2 F18 Ge'
_chemical_formula_sum            'C18 H4 Cl2 F18 Ge'
_chemical_formula_weight         705.70
_chemical_melting_point          ?
_chemical_name_common
Bis-(2,4,6-tris-trifluoromethyl-phenyl)-dichloro-germane
_chemical_name_systematic
; 
Bis-(2,4,6-tris-trifluoromethyl-phenyl)-dichloro-germane 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 96.433(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3893(6)
_cell_length_b                   30.043(2)
_cell_length_c                   8.6373(6)
_cell_measurement_reflns_used    7656
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      54.790
_cell_measurement_theta_min      4.936
_cell_volume                     2163.2(3)
_computing_cell_refinement       'SMART-NT V5.0 (Bruker, 1998)'
_computing_data_collection       'SMART-NT V5.0 (Bruker, 1998)'
_computing_data_reduction        'SMART-NT V5.0 (Bruker, 1998)'
_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      120(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker SMART CCD 1K area detector'
_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  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            16108
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    1.826
_exptl_absorpt_correction_T_max  0.8677
_exptl_absorpt_correction_T_min  0.5757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (G.M.Sheldrick, 1998)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.167
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         4795
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0405
_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)+(0.0216P)²+5.1440P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0851
_reflns_number_gt                3860
_reflns_number_total             4795
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b302544f.txt
_cod_data_source_block           (1b)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7012911
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Ge Ge 0.74612(4) 0.618770(11) 1.04001(4) 0.01535(9) Uani 1 1 d . . .
Cl1 Cl 0.97859(11) 0.62655(3) 1.16029(11) 0.0276(2) Uani 1 1 d . . .
Cl2 Cl 0.59696(11) 0.60346(3) 1.21993(11) 0.0289(2) Uani 1 1 d . . .
C11 C 0.6267(4) 0.67390(10) 0.9602(4) 0.0169(6) Uani 1 1 d . . .
C12 C 0.4658(4) 0.67011(10) 0.8916(4) 0.0179(7) Uani 1 1 d . . .
C13 C 0.3698(4) 0.70695(11) 0.8538(4) 0.0204(7) Uani 1 1 d . . .
H13 H 0.2647 0.7030 0.8087 0.025 Uiso 1 1 d R . .
C14 C 0.4290(4) 0.74957(11) 0.8827(4) 0.0191(7) Uani 1 1 d . A .
C15 C 0.5858(4) 0.75482(11) 0.9471(4) 0.0204(7) Uani 1 1 d . . .
H15 H 0.6269 0.7833 0.9655 0.024 Uiso 1 1 d R . .
C16 C 0.6834(4) 0.71801(10) 0.9849(4) 0.0171(6) Uani 1 1 d . . .
C17 C 0.3760(4) 0.62710(11) 0.8571(4) 0.0233(7) Uani 1 1 d . . .
F11 F 0.4662(2) 0.59068(6) 0.8705(3) 0.0322(5) Uani 1 1 d . . .
F12 F 0.2996(3) 0.62688(8) 0.7130(3) 0.0475(7) Uani 1 1 d . . .
F13 F 0.2626(3) 0.62189(7) 0.9521(3) 0.0457(7) Uani 1 1 d . . .
C18 C 0.8494(4) 0.72955(11) 1.0626(4) 0.0241(7) Uani 1 1 d . . .
F14 F 0.9668(2) 0.71080(6) 0.9921(2) 0.0250(4) Uani 1 1 d . . .
F15 F 0.8665(3) 0.71664(7) 1.2126(2) 0.0325(5) Uani 1 1 d . . .
F16 F 0.8781(3) 0.77346(7) 1.0637(3) 0.0384(6) Uani 1 1 d . . .
C19 C 0.3214(4) 0.78885(11) 0.8467(4) 0.0243(7) Uani 1 1 d D . .
F17 F 0.2989(7) 0.79850(16) 0.6995(4) 0.091(2) Uani 0.872(7) 1 d PD A 1
F18 F 0.1818(4) 0.78438(11) 0.8985(6) 0.0730(16) Uani 0.872(7) 1 d PD A 1
F19 F 0.3814(4) 0.82629(9) 0.9156(5) 0.0611(14) Uani 0.872(7) 1 d PD A 1
F17A F 0.398(2) 0.8213(5) 0.797(2) 0.032(5) Uiso 0.128(7) 1 d PD A 2
F18A F 0.2155(19) 0.7777(6) 0.726(2) 0.025(5) Uiso 0.128(7) 1 d PD A 2
F19A F 0.249(3) 0.8011(8) 0.959(2) 0.045(6) Uiso 0.128(7) 1 d PD A 2
C21 C 0.7721(4) 0.56786(10) 0.8963(4) 0.0139(6) Uani 1 1 d . . .
C22 C 0.7860(4) 0.57524(10) 0.7371(4) 0.0151(6) Uani 1 1 d . . .
C23 C 0.7797(4) 0.54073(10) 0.6286(4) 0.0169(6) Uani 1 1 d . . .
H23 H 0.7877 0.5468 0.5242 0.020 Uiso 1 1 d R . .
C24 C 0.7613(4) 0.49720(10) 0.6778(4) 0.0157(6) Uani 1 1 d . . .
C25 C 0.7593(4) 0.48845(10) 0.8342(4) 0.0152(6) Uani 1 1 d . . .
H25 H 0.7530 0.4591 0.8677 0.018 Uiso 1 1 d R . .
C26 C 0.7667(4) 0.52287(10) 0.9426(4) 0.0147(6) Uani 1 1 d . . .
C27 C 0.8097(4) 0.62124(11) 0.6729(4) 0.0206(7) Uani 1 1 d . . .
C28 C 0.7679(4) 0.50758(10) 1.1101(4) 0.0182(7) Uani 1 1 d . . .
C29 C 0.7476(4) 0.46026(10) 0.5591(4) 0.0196(7) Uani 1 1 d . . .
F21 F 0.8910(2) 0.64766(6) 0.7799(2) 0.0234(4) Uani 1 1 d . . .
F22 F 0.6693(3) 0.64179(6) 0.6281(2) 0.0278(5) Uani 1 1 d . . .
F23 F 0.8915(3) 0.62061(7) 0.5490(2) 0.0298(5) Uani 1 1 d . . .
F24 F 0.8376(3) 0.46746(6) 1.1307(2) 0.0258(5) Uani 1 1 d . . .
F25 F 0.8508(2) 0.53485(6) 1.2126(2) 0.0217(4) Uani 1 1 d . . .
F26 F 0.6198(2) 0.50341(7) 1.1516(2) 0.0252(4) Uani 1 1 d . . .
F27 F 0.7386(3) 0.42034(6) 0.6229(2) 0.0341(5) Uani 1 1 d . . .
F28 F 0.6164(3) 0.46500(8) 0.4571(3) 0.0436(6) Uani 1 1 d . . .
F29 F 0.8712(3) 0.45970(8) 0.4756(3) 0.0423(6) Uani 1 1 d . . .
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'
F F 0.0171 0.0103 '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
C21 Ge C11 120.07(12) . . ?
C21 Ge Cl1 103.34(9) . . ?
C11 Ge Cl1 118.17(9) . . ?
C21 Ge Cl2 113.46(9) . . ?
C11 Ge Cl2 96.65(9) . . ?
Cl1 Ge Cl2 104.33(4) . . ?
Cl1 Ge F11 167.77(5) . . ?
Cl2 Ge F21 169.32(5) . . ?
C11 Ge F25 164.49(10) . . ?
C21 Ge F15 152.55(10) . . ?
C16 C11 C12 115.2(3) . . ?
C16 C11 Ge 124.8(2) . . ?
C12 C11 Ge 119.4(2) . . ?
C13 C12 C11 122.4(3) . . ?
C13 C12 C17 111.9(3) . . ?
C11 C12 C17 125.6(3) . . ?
C14 C13 C12 120.5(3) . . ?
C15 C14 C13 119.0(3) . . ?
C15 C14 C19 121.3(3) . . ?
C13 C14 C19 119.7(3) . . ?
C14 C15 C16 120.9(3) . . ?
C15 C16 C11 121.9(3) . . ?
C15 C16 C18 114.1(3) . . ?
C11 C16 C18 123.8(3) . . ?
F11 C17 F13 106.8(3) . . ?
F11 C17 F12 106.6(3) . . ?
F13 C17 F12 105.8(3) . . ?
F11 C17 C12 114.9(3) . . ?
F13 C17 C12 110.8(3) . . ?
F12 C17 C12 111.4(3) . . ?
C17 F11 Ge 103.71(18) . . ?
F14 C18 F16 106.1(3) . . ?
F15 C18 F14 108.2(3) . . ?
F16 C18 F15 106.1(3) . . ?
F14 C18 C16 112.8(3) . . ?
F16 C18 C16 112.5(3) . . ?
F15 C18 C16 110.7(3) . . ?
C18 F15 Ge 80.36(16) . . ?
C18 F14 Ge 81.24(17) . . ?
F19A C19 F17A 110.1(14) . . ?
F19A C19 F17 131.4(11) . . ?
F17A C19 F17 61.2(9) . . ?
F19A C19 F18 40.2(11) . . ?
F17A C19 F18 134.6(9) . . ?
F17 C19 F18 108.7(4) . . ?
F19A C19 F18A 110.0(14) . . ?
F17A C19 F18A 104.1(12) . . ?
F17 C19 F18A 43.8(7) . . ?
F18 C19 F18A 72.5(8) . . ?
F19A C19 F19 66.6(12) . . ?
F17A C19 F19 47.8(9) . . ?
F17 C19 F19 104.6(4) . . ?
F18 C19 F19 103.9(4) . . ?
F18A C19 F19 137.7(8) . . ?
F19A C19 C14 113.8(11) . . ?
F17A C19 C14 111.1(9) . . ?
F17 C19 C14 113.5(3) . . ?
F18 C19 C14 113.0(3) . . ?
F18A C19 C14 107.3(8) . . ?
F19 C19 C14 112.4(3) . . ?
C22 C21 C26 115.8(3) . . ?
C22 C21 Ge 120.8(2) . . ?
C26 C21 Ge 123.2(2) . . ?
C23 C22 C21 122.5(3) . . ?
C23 C22 C27 115.5(3) . . ?
C21 C22 C27 122.0(3) . . ?
C24 C23 C22 119.4(3) . . ?
C25 C24 C23 119.6(3) . . ?
C25 C24 C29 121.2(3) . . ?
C23 C24 C29 119.2(3) . . ?
C24 C25 C26 120.9(3) . . ?
C25 C26 C21 121.4(3) . . ?
C25 C26 C28 114.3(3) . . ?
C21 C26 C28 124.3(3) . . ?
F23 C27 F21 107.0(3) . . ?
F23 C27 F22 106.7(3) . . ?
F21 C27 F22 106.7(3) . . ?
F23 C27 C22 112.5(3) . . ?
F21 C27 C22 111.4(3) . . ?
F22 C27 C22 112.2(3) . . ?
F27 C29 F29 107.4(3) . . ?
F27 C29 F28 106.8(3) . . ?
F29 C29 F28 106.2(3) . . ?
F27 C29 C24 112.8(3) . . ?
F29 C29 C24 112.0(3) . . ?
F28 C29 C24 111.4(3) . . ?
F26 C28 F25 108.0(3) . . ?
F26 C28 F24 106.5(2) . . ?
F25 C28 F24 105.9(3) . . ?
F26 C28 C26 112.2(3) . . ?
F25 C28 C26 113.1(3) . . ?
F24 C28 C26 110.8(3) . . ?
C27 F21 Ge 97.78(17) . . ?
C28 F25 Ge 94.79(16) . . ?
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
Ge C21 1.997(3) . ?
Ge C11 2.017(3) . ?
Ge Cl1 2.1174(9) . ?
Ge Cl2 2.1513(9) . ?
Ge F11 2.757(2) . ?
Ge F21 2.809(2) . ?
Ge F25 3.0095(19) . ?
Ge F14 3.3785(19) . ?
Ge F15 3.399(2) . ?
C11 C16 1.416(4) . ?
C11 C12 1.417(4) . ?
C12 C13 1.386(4) . ?
C12 C17 1.508(4) . ?
C13 C14 1.386(5) . ?
C14 C15 1.379(5) . ?
C14 C19 1.497(4) . ?
C15 C16 1.393(4) . ?
C16 C18 1.517(5) . ?
C17 F11 1.328(4) . ?
C17 F13 1.333(4) . ?
C17 F12 1.335(4) . ?
C18 F14 1.339(4) . ?
C18 F16 1.341(4) . ?
C18 F15 1.345(4) . ?
C19 F19A 1.255(16) . ?
C19 F17A 1.270(14) . ?
C19 F17 1.297(5) . ?
C19 F18 1.306(5) . ?
C19 F18A 1.337(14) . ?
C19 F19 1.344(4) . ?
C21 C22 1.410(4) . ?
C21 C26 1.412(4) . ?
C22 C23 1.394(4) . ?
C22 C27 1.510(4) . ?
C23 C24 1.389(4) . ?
C24 C25 1.378(4) . ?
C24 C29 1.507(4) . ?
C25 C26 1.392(4) . ?
C26 C28 1.516(4) . ?
C27 F23 1.335(4) . ?
C27 F21 1.345(4) . ?
C27 F22 1.347(4) . ?
C29 F27 1.325(4) . ?
C29 F29 1.329(4) . ?
C29 F28 1.338(4) . ?
C28 F26 1.337(4) . ?
C28 F25 1.342(4) . ?
C28 F24 1.343(4) . ?
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
C11 C12 C17 F11 -11.2(5) . . . . ?
C21 C22 C27 F21 30.5(4) . . . . ?
C11 C16 C18 F15 -65.3(4) . . . . ?
C21 C26 C28 F25 -31.4(4) . . . . ?
C12 C11 Ge Cl1 -174.4(2) . . . . ?
C12 C11 Ge Cl2 -64.2(2) . . . . ?
C12 C11 Ge C21 57.8(3) . . . . ?
C22 C21 Ge Cl1 -101.8(2) . . . . ?
C22 C21 Ge Cl2 145.9(2) . . . . ?
C22 C21 Ge C11 32.5(3) . . . . ?
