#------------------------------------------------------------------------------
#$Date: 2016-03-21 11:03:27 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178678 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/89/4078993.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_4078993
loop_
_publ_author_name
'El Aziz, Youssef'
'Bassindale, Alan R.'
'Taylor, Peter G.'
'Horton, Peter N.'
'Stephenson, Richard A.'
'Hursthouse, Michael B.'
_publ_section_title
;
 Facile Synthesis of Novel Functionalized Silsesquioxane Nanostructures
 Containing an Encapsulated Fluoride Anion
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              6032
_journal_paper_doi               10.1021/om300277g
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C32 H52 F N9 O12 Si8'
_chemical_formula_weight         998.55
_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                106.0410(10)
_cell_angle_beta                 98.0060(10)
_cell_angle_gamma                96.1230(10)
_cell_formula_units_Z            1
_cell_length_a                   8.6557(2)
_cell_length_b                   11.7528(2)
_cell_length_c                   12.4208(2)
_cell_measurement_reflns_used    5302
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     1188.45(4)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
'Bruker-Nonius Roper CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26888
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    0.294
_exptl_absorpt_correction_T_max  0.9655
_exptl_absorpt_correction_T_min  0.8317
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       slab
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5461
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0342
_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)+(0.0588P)²+0.4876P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1083
_reflns_number_gt                4914
_reflns_number_total             5461
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300277g_si_001.cif
_cod_data_source_block           EY250
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4078993
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.56330(5) 0.93355(4) 0.28966(3) 0.01150(11) Uani 1 1 d . . .
Si2 Si 0.57373(5) 0.78096(4) 0.45337(3) 0.01168(11) Uani 1 1 d . . .
Si3 Si 0.75215(5) 0.99723(4) 0.64713(3) 0.01131(11) Uani 1 1 d . . .
Si4 Si 0.25886(5) 0.85101(4) 0.51535(3) 0.01150(11) Uani 1 1 d . . .
O1 O 0.38245(13) 0.96086(10) 0.27817(9) 0.0142(2) Uani 1 1 d . . .
O2 O 0.69291(13) 1.04985(10) 0.36044(9) 0.0143(2) Uani 1 1 d . . .
O3 O 0.58240(13) 0.81896(9) 0.33764(9) 0.0142(2) Uani 1 1 d . . .
O4 O 0.70563(13) 0.86186(9) 0.56094(9) 0.0141(2) Uani 1 1 d . . .
O5 O 0.39570(13) 0.77010(10) 0.48147(9) 0.0147(2) Uani 1 1 d . . .
O6 O 0.18934(12) 0.90600(10) 0.41561(9) 0.0142(2) Uani 1 1 d . . .
C11 C 0.60290(19) 0.89548(15) 0.14125(13) 0.0165(3) Uani 1 1 d . . .
H11A H 0.6136 0.9695 0.1178 0.020 Uiso 1 1 calc R . .
H11B H 0.7047 0.8643 0.1396 0.020 Uiso 1 1 calc R . .
C12 C 0.4734(2) 0.80226(16) 0.05498(14) 0.0216(3) Uani 1 1 d . . .
H12A H 0.4757 0.7241 0.0702 0.026 Uiso 1 1 calc R . .
H12B H 0.3693 0.8265 0.0662 0.026 Uiso 1 1 calc R . .
C13 C 0.4900(2) 0.78752(16) -0.06455(15) 0.0225(4) Uani 1 1 d . . .
N14 N 0.5023(2) 0.77608(15) -0.15726(13) 0.0299(4) Uani 1 1 d . . .
C21 C 0.62468(19) 0.62656(14) 0.42926(13) 0.0161(3) Uani 1 1 d . . .
H21A H 0.7335 0.6280 0.4129 0.019 Uiso 1 1 calc R . .
H21B H 0.6249 0.6050 0.5009 0.019 Uiso 1 1 calc R . .
C22 C 0.5152(2) 0.52702(15) 0.33254(15) 0.0199(3) Uani 1 1 d . . .
H22A H 0.5354 0.4478 0.3394 0.024 Uiso 1 1 calc R . .
H22B H 0.4038 0.5338 0.3396 0.024 Uiso 1 1 calc R . .
C23 C 0.5410(3) 0.53563(17) 0.22151(16) 0.0339(5) Uani 1 1 d . . .
N24 N 0.5650(4) 0.5441(2) 0.13631(17) 0.0729(9) Uani 1 1 d . . .
C31 C 0.92436(18) 0.99104(14) 0.75219(13) 0.0153(3) Uani 1 1 d . . .
H31A H 1.0149 0.9729 0.7131 0.018 Uiso 1 1 calc R . .
H31B H 0.9555 1.0700 0.8106 0.018 Uiso 1 1 calc R . .
C32 C 0.8837(2) 0.89442(16) 0.81006(15) 0.0231(4) Uani 1 1 d . . .
H32A H 0.7960 0.9150 0.8517 0.028 Uiso 1 1 calc R . .
H32B H 0.8468 0.8166 0.7509 0.028 Uiso 1 1 calc R . .
C33 C 1.0186(2) 0.88219(18) 0.88984(16) 0.0274(4) Uani 1 1 d . . .
N34 N 1.1239(2) 0.87220(19) 0.95153(16) 0.0411(5) Uani 1 1 d . . .
C41 C 0.09254(18) 0.74500(14) 0.52874(13) 0.0144(3) Uani 1 1 d . . .
H41A H 0.0056 0.7895 0.5513 0.017 Uiso 1 1 calc R . .
H41B H 0.0524 0.6848 0.4539 0.017 Uiso 1 1 calc R . .
C42 C 0.1427(2) 0.68041(16) 0.61719(16) 0.0233(4) Uani 1 1 d . . .
H42A H 0.2217 0.6292 0.5904 0.028 Uiso 1 1 calc R . .
H42B H 0.1934 0.7407 0.6899 0.028 Uiso 1 1 calc R . .
C43 C 0.0087(2) 0.60620(15) 0.63687(15) 0.0222(3) Uani 1 1 d . . .
N44 N -0.0987(2) 0.55011(15) 0.65112(14) 0.0306(4) Uani 1 1 d . . .
F1 F 0.5000 1.0000 0.5000 0.0173(3) Uani 1 2 d S . .
N1 N 1.0004(18) 0.4958(13) 0.0042(13) 0.0144(10) Uani 0.50 1 d PD A -1
C1 C 0.9945(5) 0.4506(3) -0.1236(3) 0.0252(7) Uani 0.50 1 d PD A -1
H1A H 1.0974 0.4256 -0.1375 0.030 Uiso 0.50 1 calc PR A -1
H1B H 0.9810 0.5179 -0.1557 0.030 Uiso 0.50 1 calc PR A -1
C2 C 0.864(2) 0.3465(17) -0.1876(13) 0.041(4) Uani 0.50 1 d PD A -1
H2A H 0.8827 0.2762 -0.1624 0.061 Uiso 0.50 1 calc PR A -1
H2B H 0.8650 0.3276 -0.2694 0.061 Uiso 0.50 1 calc PR A -1
H2C H 0.7620 0.3686 -0.1720 0.061 Uiso 0.50 1 calc PR A -1
C3 C 0.8455(4) 0.5355(3) 0.0301(3) 0.0235(7) Uani 0.50 1 d PD A -1
H3A H 0.8519 0.5620 0.1137 0.028 Uiso 0.50 1 calc PR A -1
H3B H 0.7607 0.4656 -0.0015 0.028 Uiso 0.50 1 calc PR A -1
C4 C 0.7998(10) 0.6363(7) -0.0169(11) 0.0440(19) Uani 0.50 1 d PD A -1
H4A H 0.8812 0.7070 0.0155 0.066 Uiso 0.50 1 calc PR A -1
H4B H 0.6985 0.6564 0.0035 0.066 Uiso 0.50 1 calc PR A -1
H4C H 0.7901 0.6105 -0.0999 0.066 Uiso 0.50 1 calc PR A -1
C5 C 1.1368(4) 0.5988(3) 0.0497(3) 0.0182(6) Uani 0.50 1 d PD A -1
H5A H 1.1198 0.6594 0.0093 0.022 Uiso 0.50 1 calc PR A -1
H5B H 1.2356 0.5682 0.0324 0.022 Uiso 0.50 1 calc PR A -1
C6 C 1.157(2) 0.6591(15) 0.1771(10) 0.028(2) Uani 0.50 1 d PD A -1
H6A H 1.0605 0.6907 0.1950 0.042 Uiso 0.50 1 calc PR A -1
H6B H 1.2459 0.7249 0.2004 0.042 Uiso 0.50 1 calc PR A -1
H6C H 1.1782 0.6005 0.2181 0.042 Uiso 0.50 1 calc PR A -1
C7 C 1.0253(4) 0.3969(3) 0.0582(3) 0.0225(7) Uani 0.50 1 d PD A -1
H7A H 0.9301 0.3351 0.0315 0.027 Uiso 0.50 1 calc PR A -1
H7B H 1.0354 0.4307 0.1417 0.027 Uiso 0.50 1 calc PR A -1
C8 C 1.1680(9) 0.3371(8) 0.0335(11) 0.046(2) Uani 0.50 1 d PD A -1
H8A H 1.1492 0.2881 -0.0463 0.069 Uiso 0.50 1 calc PR A -1
H8B H 1.1866 0.2861 0.0830 0.069 Uiso 0.50 1 calc PR A -1
H8C H 1.2606 0.3984 0.0479 0.069 Uiso 0.50 1 calc PR A -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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
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
O2 Si1 O1 113.76(6) . .
O2 Si1 O3 112.33(6) . .
O1 Si1 O3 111.67(6) . .
O2 Si1 C11 105.21(7) . .
O1 Si1 C11 104.40(7) . .
O3 Si1 C11 108.83(7) . .
O4 Si2 O5 113.58(6) . .
O4 Si2 O3 113.30(6) . .
O5 Si2 O3 112.33(6) . .
O4 Si2 C21 103.97(7) . .
O5 Si2 C21 104.61(7) . .
O3 Si2 C21 108.14(6) . .
O1 Si3 O6 112.69(6) 2_676 2_676
O1 Si3 O4 113.53(6) 2_676 .
O6 Si3 O4 112.72(6) 2_676 .
O1 Si3 C31 105.15(6) 2_676 .
O6 Si3 C31 106.89(7) 2_676 .
O4 Si3 C31 105.02(6) . .
O6 Si4 O2 113.22(6) . 2_676
O6 Si4 O5 112.99(6) . .
O2 Si4 O5 113.61(6) 2_676 .
O6 Si4 C41 105.72(6) . .
O2 Si4 C41 105.08(6) 2_676 .
O5 Si4 C41 105.20(6) . .
Si3 O1 Si1 142.33(7) 2_676 .
Si1 O2 Si4 141.40(7) . 2_676
Si2 O3 Si1 139.70(7) . .
Si2 O4 Si3 141.16(7) . .
Si4 O5 Si2 141.25(7) . .
Si4 O6 Si3 138.90(7) . 2_676
C12 C11 Si1 113.50(11) . .
C12 C11 H11A 108.9 . .
Si1 C11 H11A 108.9 . .
C12 C11 H11B 108.9 . .
Si1 C11 H11B 108.9 . .
H11A C11 H11B 107.7 . .
C13 C12 C11 113.52(14) . .
C13 C12 H12A 108.9 . .
C11 C12 H12A 108.9 . .
C13 C12 H12B 108.9 . .
C11 C12 H12B 108.9 . .
H12A C12 H12B 107.7 . .
N14 C13 C12 179.8(2) . .
C22 C21 Si2 116.20(11) . .
C22 C21 H21A 108.2 . .
Si2 C21 H21A 108.2 . .
C22 C21 H21B 108.2 . .
Si2 C21 H21B 108.2 . .
H21A C21 H21B 107.4 . .
C23 C22 C21 111.09(14) . .
C23 C22 H22A 109.4 . .
C21 C22 H22A 109.4 . .
C23 C22 H22B 109.4 . .
C21 C22 H22B 109.4 . .
H22A C22 H22B 108.0 . .
N24 C23 C22 178.1(3) . .
C32 C31 Si3 110.70(11) . .
C32 C31 H31A 109.5 . .
Si3 C31 H31A 109.5 . .
C32 C31 H31B 109.5 . .
Si3 C31 H31B 109.5 . .
H31A C31 H31B 108.1 . .
C33 C32 C31 112.68(15) . .
C33 C32 H32A 109.1 . .
C31 C32 H32A 109.1 . .
C33 C32 H32B 109.1 . .
C31 C32 H32B 109.1 . .
H32A C32 H32B 107.8 . .
N34 C33 C32 179.6(2) . .
C42 C41 Si4 111.92(11) . .
C42 C41 H41A 109.2 . .
Si4 C41 H41A 109.2 . .
C42 C41 H41B 109.2 . .
Si4 C41 H41B 109.2 . .
H41A C41 H41B 107.9 . .
C43 C42 C41 112.20(14) . .
C43 C42 H42A 109.2 . .
C41 C42 H42A 109.2 . .
C43 C42 H42B 109.2 . .
C41 C42 H42B 109.2 . .
H42A C42 H42B 107.9 . .
N44 C43 C42 178.1(2) . .
C3 N1 C1 110.5(8) . .
C3 N1 C7 106.7(12) . .
C1 N1 C7 110.6(8) . .
C3 N1 C5 111.7(8) . .
C1 N1 C5 106.3(12) . .
C7 N1 C5 111.0(8) . .
N1 C1 C2 115.3(11) . .
N1 C1 H1A 108.4 . .
C2 C1 H1A 108.4 . .
N1 C1 H1B 108.4 . .
C2 C1 H1B 108.4 . .
H1A C1 H1B 107.5 . .
N1 C3 C4 114.7(8) . .
N1 C3 H3A 108.6 . .
C4 C3 H3A 108.6 . .
N1 C3 H3B 108.6 . .
C4 C3 H3B 108.6 . .
H3A C3 H3B 107.6 . .
N1 C5 C6 113.8(10) . .
N1 C5 H5A 108.8 . .
C6 C5 H5A 108.8 . .
N1 C5 H5B 108.8 . .
C6 C5 H5B 108.8 . .
H5A C5 H5B 107.7 . .
N1 C7 C8 115.2(8) . .
N1 C7 H7A 108.5 . .
C8 C7 H7A 108.5 . .
N1 C7 H7B 108.5 . .
C8 C7 H7B 108.5 . .
H7A C7 H7B 107.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 O2 1.6229(11) .
Si1 O1 1.6260(11) .
Si1 O3 1.6310(11) .
Si1 C11 1.8624(16) .
Si2 O4 1.6230(11) .
Si2 O5 1.6264(11) .
Si2 O3 1.6276(11) .
Si2 C21 1.8666(16) .
Si3 O1 1.6222(11) 2_676
Si3 O6 1.6231(11) 2_676
Si3 O4 1.6252(11) .
Si3 C31 1.8611(16) .
Si4 O6 1.6224(11) .
Si4 O2 1.6235(11) 2_676
Si4 O5 1.6255(11) .
Si4 C41 1.8576(16) .
O1 Si3 1.6222(11) 2_676
O2 Si4 1.6235(11) 2_676
O6 Si3 1.6231(11) 2_676
C11 C12 1.536(2) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 C13 1.476(2) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 N14 1.143(2) .
C21 C22 1.543(2) .
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C22 C23 1.456(3) .
C22 H22A 0.9900 .
C22 H22B 0.9900 .
C23 N24 1.135(3) .
C31 C32 1.538(2) .
C31 H31A 0.9900 .
C31 H31B 0.9900 .
C32 C33 1.469(2) .
C32 H32A 0.9900 .
C32 H32B 0.9900 .
C33 N34 1.144(3) .
C41 C42 1.540(2) .
C41 H41A 0.9900 .
C41 H41B 0.9900 .
C42 C43 1.465(2) .
C42 H42A 0.9900 .
C42 H42B 0.9900 .
C43 N44 1.145(2) .
N1 C3 1.513(15) .
N1 C1 1.520(15) .
N1 C7 1.514(15) .
N1 C5 1.520(15) .
C1 C2 1.521(12) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 C4 1.523(7) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 C6 1.522(12) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 C8 1.511(8) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
