#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:36:43 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180189 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/85/7108586.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_7108586
loop_
_publ_author_name
'Katsuhiko Takeuchi'
'Douglas W. Stephan'
_publ_section_title
;
 Silyl-migrations in frustrated Lewis pair chemistry: reactions of
 (CH3)3Si)3P and B(C6F4H)3 with H2 and CO2
;
_journal_name_full               Chem.Commun.
_journal_page_first              11304
_journal_paper_doi               10.1039/c2cc36470k
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C30 H39 B F12 P Si4'
_chemical_formula_weight         781.75
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   14.0075(12)
_cell_length_b                   14.0075(12)
_cell_length_c                   34.296(4)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.284
_cell_measurement_theta_min      2.902
_cell_volume                     5827.7(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0779
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            2998
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2418
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.291
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0707P)²+10.8148P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1461
_reflns_number_gt                2674
_reflns_number_total             2998
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc36470k.txt
_cod_data_source_block           kt002twin
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7108586
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
P1 P 0.3333 0.6667 0.04210(5) 0.0150(3) Uani 1 3 d S
Si1 Si 0.3333 0.6667 -0.02499(5) 0.0204(4) Uani 1 3 d S
Si2 Si 0.25312(9) 0.48790(9) 0.06475(4) 0.0233(2) Uani 1 1 d .
C19 C 0.4262(5) 0.8095(4) -0.04134(14) 0.0364(11) Uani 1 1 d .
H19A H 0.4214 0.8136 -0.0692 0.055 Uiso 1 1 calc R
H19B H 0.5006 0.8316 -0.0341 0.055 Uiso 1 1 calc R
H19C H 0.4048 0.8578 -0.0292 0.055 Uiso 1 1 calc R
C22 C 0.3567(5) 0.4424(4) 0.05865(16) 0.0383(11) Uani 1 1 d .
H22A H 0.3233 0.3654 0.0648 0.057 Uiso 1 1 calc R
H22B H 0.4178 0.4840 0.0759 0.057 Uiso 1 1 calc R
H22C H 0.3824 0.4545 0.0322 0.057 Uiso 1 1 calc R
C23 C 0.1271(4) 0.3989(4) 0.03523(16) 0.0387(11) Uani 1 1 d .
H23A H 0.1483 0.3922 0.0092 0.058 Uiso 1 1 calc R
H23B H 0.0811 0.4316 0.0344 0.058 Uiso 1 1 calc R
H23C H 0.0872 0.3272 0.0469 0.058 Uiso 1 1 calc R
C24 C 0.2187(5) 0.4887(4) 0.11740(13) 0.0350(11) Uani 1 1 d .
H24A H 0.1669 0.5143 0.1199 0.052 Uiso 1 1 calc R
H24B H 0.2846 0.5369 0.1316 0.052 Uiso 1 1 calc R
H24C H 0.1869 0.4154 0.1277 0.052 Uiso 1 1 calc R
F1 F 0.1395(2) -0.0673(2) 0.19678(8) 0.0331(6) Uani 1 1 d .
F2 F 0.3440(2) -0.0132(3) 0.17967(9) 0.0382(7) Uani 1 1 d .
F3 F 0.3359(3) 0.1866(3) 0.06989(10) 0.0496(9) Uani 1 1 d .
F4 F 0.1327(3) 0.1369(3) 0.08718(9) 0.0443(8) Uani 1 1 d .
C1 C 0.1247(3) 0.0327(3) 0.14344(11) 0.0215(7) Uani 1 1 d .
C2 C 0.1847(3) -0.0034(3) 0.16497(12) 0.0237(8) Uani 1 1 d .
C3 C 0.2919(4) 0.0234(4) 0.15606(13) 0.0256(9) Uani 1 1 d .
C4 C 0.3460(4) 0.0876(4) 0.12481(14) 0.0274(9) Uani 1 1 d .
H4 H 0.4182 0.1067 0.1190 0.033 Uiso 1 1 calc R
C5 C 0.2877(4) 0.1233(4) 0.10205(14) 0.0296(9) Uani 1 1 d .
C6 C 0.1816(4) 0.0969(4) 0.11172(13) 0.0270(9) Uani 1 1 d .
B1 B 0.0000 0.0000 0.1573(2) 0.0230(15) Uani 1 3 d S
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'
B B 0.0013 0.0007 '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'
P P 0.1023 0.0942 '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
Si1 P1 Si2 109.68(5) . 3_565
Si1 P1 Si2 109.68(5) . 2_665
Si2 P1 Si2 109.26(5) 3_565 2_665
Si1 P1 Si2 109.68(5) . .
Si2 P1 Si2 109.26(5) 3_565 .
Si2 P1 Si2 109.26(5) 2_665 .
C19 Si1 C19 111.20(15) 2_665 .
C19 Si1 C19 111.20(15) 2_665 3_565
C19 Si1 C19 111.20(15) . 3_565
C19 Si1 P1 107.68(16) 2_665 .
C19 Si1 P1 107.68(16) . .
C19 Si1 P1 107.68(16) 3_565 .
C22 Si2 C23 110.4(3) . .
C22 Si2 C24 110.9(2) . .
C23 Si2 C24 111.5(3) . .
C22 Si2 P1 107.03(18) . .
C23 Si2 P1 109.06(18) . .
C24 Si2 P1 107.79(17) . .
Si1 C19 H19A 109.5 . .
Si1 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
Si1 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
Si2 C22 H22A 109.5 . .
Si2 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
Si2 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
Si2 C23 H23A 109.5 . .
Si2 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
Si2 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
Si2 C24 H24A 109.5 . .
Si2 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
Si2 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
C6 C1 C2 113.5(4) . .
C6 C1 B1 126.6(4) . .
C2 C1 B1 119.8(4) . .
F1 C2 C3 116.3(4) . .
F1 C2 C1 120.1(4) . .
C3 C2 C1 123.6(4) . .
F2 C3 C4 119.7(4) . .
F2 C3 C2 118.8(4) . .
C4 C3 C2 121.4(4) . .
C3 C4 C5 116.6(4) . .
C3 C4 H4 121.7 . .
C5 C4 H4 121.7 . .
F3 C5 C6 119.0(4) . .
F3 C5 C4 119.9(4) . .
C6 C5 C4 121.0(4) . .
F4 C6 C5 115.7(4) . .
F4 C6 C1 120.5(4) . .
C5 C6 C1 123.8(4) . .
C1 B1 C1 111.9(3) 3 .
C1 B1 C1 111.9(3) 3 2
C1 B1 C1 111.9(3) . 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 Si1 2.301(3) .
P1 Si2 2.3071(12) 3_565
P1 Si2 2.3071(12) 2_665
P1 Si2 2.3071(12) .
Si1 C19 1.846(5) 2_665
Si1 C19 1.846(5) .
Si1 C19 1.846(5) 3_565
Si2 C22 1.865(5) .
Si2 C23 1.870(5) .
Si2 C24 1.870(5) .
C19 H19A 0.9600 .
C19 H19B 0.9600 .
C19 H19C 0.9600 .
C22 H22A 0.9600 .
C22 H22B 0.9600 .
C22 H22C 0.9600 .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C24 H24A 0.9600 .
C24 H24B 0.9600 .
C24 H24C 0.9600 .
F1 C2 1.351(5) .
F2 C3 1.350(5) .
F3 C5 1.364(5) .
F4 C6 1.369(5) .
C1 C6 1.382(6) .
C1 C2 1.390(5) .
C1 B1 1.640(5) .
C2 C3 1.388(6) .
C3 C4 1.360(6) .
C4 C5 1.390(7) .
C4 H4 0.9300 .
C5 C6 1.381(6) .
B1 C1 1.640(5) 3
B1 C1 1.640(5) 2
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_4
Si2 P1 Si1 C19 -46.80(19) 3_565 2_665
Si2 P1 Si1 C19 -166.80(19) 2_665 2_665
Si2 P1 Si1 C19 73.20(19) . 2_665
Si2 P1 Si1 C19 73.20(19) 3_565 .
Si2 P1 Si1 C19 -46.80(19) 2_665 .
Si2 P1 Si1 C19 -166.80(19) . .
Si2 P1 Si1 C19 -166.80(19) 3_565 3_565
Si2 P1 Si1 C19 73.20(19) 2_665 3_565
Si2 P1 Si1 C19 -46.80(19) . 3_565
Si1 P1 Si2 C22 76.5(2) . .
Si2 P1 Si2 C22 -163.30(19) 3_565 .
Si2 P1 Si2 C22 -43.8(2) 2_665 .
Si1 P1 Si2 C23 -42.93(19) . .
Si2 P1 Si2 C23 77.3(2) 3_565 .
Si2 P1 Si2 C23 -163.2(2) 2_665 .
Si1 P1 Si2 C24 -164.15(18) . .
Si2 P1 Si2 C24 -43.9(2) 3_565 .
Si2 P1 Si2 C24 75.60(19) 2_665 .
C6 C1 C2 F1 -179.8(4) . .
B1 C1 C2 F1 1.4(6) . .
C6 C1 C2 C3 1.0(6) . .
B1 C1 C2 C3 -177.8(4) . .
F1 C2 C3 F2 -1.4(6) . .
C1 C2 C3 F2 177.8(4) . .
F1 C2 C3 C4 -179.7(4) . .
C1 C2 C3 C4 -0.5(7) . .
F2 C3 C4 C5 -179.3(4) . .
C2 C3 C4 C5 -1.0(7) . .
C3 C4 C5 F3 -179.0(4) . .
C3 C4 C5 C6 1.8(7) . .
F3 C5 C6 F4 0.6(7) . .
C4 C5 C6 F4 179.8(4) . .
F3 C5 C6 C1 179.4(4) . .
C4 C5 C6 C1 -1.4(7) . .
C2 C1 C6 F4 178.7(4) . .
B1 C1 C6 F4 -2.7(7) . .
C2 C1 C6 C5 -0.1(7) . .
B1 C1 C6 C5 178.6(4) . .
C6 C1 B1 C1 100.2(4) . 3
C2 C1 B1 C1 -81.2(7) . 3
C6 C1 B1 C1 -26.4(7) . 2
C2 C1 B1 C1 152.2(4) . 2
