#------------------------------------------------------------------------------
#$Date: 2016-03-21 11:03:27 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178678 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/89/4078990.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_4078990
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            'C40 H68 F N9 O12 Si8'
_chemical_formula_weight         1110.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 93.831(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.4378(11)
_cell_length_b                   8.7798(4)
_cell_length_c                   26.8273(10)
_cell_measurement_reflns_used    3785
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     6213.2(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 '4096x4096pixels / 62x62mm'
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type
'Bruker-Nonius APEX II CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            26421
_diffrn_reflns_theta_full        27.71
_diffrn_reflns_theta_max         27.71
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    0.232
_exptl_absorpt_correction_T_max  0.9963
_exptl_absorpt_correction_T_min  0.9639
_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    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
;
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         7115
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0541
_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)+(0.0589P)²+15.8814P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1436
_reflns_number_gt                5824
_reflns_number_total             7115
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300277g_si_001.cif
_cod_data_source_block           EY225
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4078990
loop_
_symmetry_equiv_pos_as_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_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
Si1 Si 0.19956(2) 0.90394(8) 0.06613(2) 0.01900(15) Uani 1 1 d .
F1 F 0.2500 0.7500 0.0000 0.0227(4) Uani 1 2 d S
O1 O 0.24676(6) 1.01210(19) 0.05310(6) 0.0208(3) Uani 1 1 d .
Si2 Si 0.29535(2) 1.01528(8) 0.01948(2) 0.01895(15) Uani 1 1 d .
O2 O 0.27963(6) 1.01379(19) -0.04007(6) 0.0218(3) Uani 1 1 d .
Si3 Si 0.25159(2) 0.90883(8) -0.08348(2) 0.01968(15) Uani 1 1 d .
O3 O 0.19205(6) 0.8786(2) -0.07562(6) 0.0220(4) Uani 1 1 d .
Si4 Si 0.15598(2) 0.79782(8) -0.03684(2) 0.01875(15) Uani 1 1 d .
O4 O 0.16016(6) 0.8748(2) 0.01830(6) 0.0213(3) Uani 1 1 d .
O5 O 0.16248(6) 0.61377(19) -0.03519(6) 0.0214(3) Uani 1 1 d .
O6 O 0.21826(6) 0.7480(2) 0.09415(6) 0.0220(3) Uani 1 1 d .
C11 C 0.16303(9) 1.0153(3) 0.11034(9) 0.0261(5) Uani 1 1 d .
H11A H 0.1475 1.1041 0.0924 0.031 Uiso 1 1 calc R
H11B H 0.1352 0.9510 0.1215 0.031 Uiso 1 1 calc R
N11 N 0.14409(11) 1.2611(4) 0.20906(10) 0.0526(7) Uani 1 1 d .
C12 C 0.19458(10) 1.0722(3) 0.15631(10) 0.0310(6) Uani 1 1 d .
H12A H 0.2059 0.9838 0.1771 0.037 Uiso 1 1 calc R
H12B H 0.2252 1.1242 0.1454 0.037 Uiso 1 1 calc R
C13 C 0.16654(11) 1.1776(4) 0.18668(10) 0.0370(6) Uani 1 1 d .
C21 C 0.32508(9) 1.2042(3) 0.03262(9) 0.0243(5) Uani 1 1 d .
H21A H 0.3025 1.2838 0.0174 0.029 Uiso 1 1 calc R
H21B H 0.3273 1.2208 0.0692 0.029 Uiso 1 1 calc R
N21 N 0.44853(13) 1.1107(5) 0.07369(19) 0.0951(16) Uani 1 1 d .
C22 C 0.37800(9) 1.2259(3) 0.01374(10) 0.0284(5) Uani 1 1 d .
H22A H 0.3790 1.1779 -0.0196 0.034 Uiso 1 1 calc R
H22B H 0.3845 1.3361 0.0098 0.034 Uiso 1 1 calc R
C23 C 0.41783(11) 1.1607(4) 0.04712(15) 0.0497(9) Uani 1 1 d .
C31 C 0.25234(10) 1.0258(3) -0.14120(9) 0.0271(5) Uani 1 1 d .
H31A H 0.2321 1.1189 -0.1364 0.032 Uiso 1 1 calc R
H31B H 0.2877 1.0585 -0.1452 0.032 Uiso 1 1 calc R
N31 N 0.29696(16) 0.7585(4) -0.22705(13) 0.0716(10) Uani 1 1 d .
C32 C 0.23205(13) 0.9488(4) -0.19031(10) 0.0428(7) Uani 1 1 d .
H32A H 0.2004 0.8934 -0.1843 0.051 Uiso 1 1 calc R
H32B H 0.2236 1.0285 -0.2156 0.051 Uiso 1 1 calc R
C33 C 0.26881(15) 0.8407(4) -0.21039(11) 0.0493(8) Uani 1 1 d .
C41 C 0.08954(8) 0.8394(3) -0.06002(9) 0.0240(5) Uani 1 1 d .
H41A H 0.0859 0.9502 -0.0660 0.029 Uiso 1 1 calc R
H41B H 0.0822 0.7868 -0.0923 0.029 Uiso 1 1 calc R
N41 N -0.03994(9) 0.8829(4) -0.05360(11) 0.0573(9) Uani 1 1 d .
C42 C 0.05060(9) 0.7891(4) -0.02350(11) 0.0367(7) Uani 1 1 d .
H42A H 0.0511 0.6766 -0.0206 0.044 Uiso 1 1 calc R
H42B H 0.0600 0.8321 0.0100 0.044 Uiso 1 1 calc R
C43 C -0.00073(10) 0.8395(4) -0.04015(11) 0.0401(7) Uani 1 1 d .
N51 N 0.0000 0.4882(3) -0.2500 0.0204(6) Uani 1 2 d S
C51 C -0.02027(9) 0.3862(3) -0.20997(9) 0.0235(5) Uani 1 1 d .
H51A H -0.0470 0.3196 -0.2258 0.028 Uiso 1 1 calc R
H51B H 0.0076 0.3197 -0.1963 0.028 Uiso 1 1 calc R
C52 C -0.04208(10) 0.4718(3) -0.16697(9) 0.0275(5) Uani 1 1 d .
H52A H -0.0645 0.5545 -0.1805 0.033 Uiso 1 1 calc R
H52B H -0.0141 0.5187 -0.1459 0.033 Uiso 1 1 calc R
C53 C -0.07222(10) 0.3655(4) -0.13510(10) 0.0336(6) Uani 1 1 d .
H53A H -0.1007 0.3204 -0.1560 0.040 Uiso 1 1 calc R
H53B H -0.0501 0.2814 -0.1222 0.040 Uiso 1 1 calc R
C54 C -0.09296(11) 0.4507(4) -0.09144(11) 0.0407(7) Uani 1 1 d .
H54A H -0.0647 0.4913 -0.0699 0.061 Uiso 1 1 calc R
H54B H -0.1130 0.3809 -0.0722 0.061 Uiso 1 1 calc R
H54C H -0.1145 0.5349 -0.1042 0.061 Uiso 1 1 calc R
C55 C 0.04191(9) 0.5894(3) -0.22714(9) 0.0217(5) Uani 1 1 d .
H55A H 0.0293 0.6423 -0.1979 0.026 Uiso 1 1 calc R
H55B H 0.0499 0.6680 -0.2519 0.026 Uiso 1 1 calc R
C56 C 0.09047(9) 0.5050(3) -0.21066(9) 0.0256(5) Uani 1 1 d .
H56A H 0.0820 0.4109 -0.1927 0.031 Uiso 1 1 calc R
H56B H 0.1084 0.4754 -0.2404 0.031 Uiso 1 1 calc R
C57 C 0.12484(10) 0.6044(3) -0.17677(10) 0.0316(6) Uani 1 1 d .
H57A H 0.1274 0.7067 -0.1920 0.038 Uiso 1 1 calc R
H57B H 0.1097 0.6166 -0.1442 0.038 Uiso 1 1 calc R
C58 C 0.17724(11) 0.5370(4) -0.16830(11) 0.0396(7) Uani 1 1 d .
H58A H 0.1749 0.4372 -0.1523 0.059 Uiso 1 1 calc R
H58B H 0.1984 0.6048 -0.1467 0.059 Uiso 1 1 calc R
H58C H 0.1924 0.5253 -0.2004 0.059 Uiso 1 1 calc R
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
O4 Si1 O6 113.20(9) . .
O4 Si1 O1 112.62(9) . .
O6 Si1 O1 112.22(9) . .
O4 Si1 C11 104.77(10) . .
O6 Si1 C11 107.69(10) . .
O1 Si1 C11 105.62(11) . .
Si2 O1 Si1 141.23(11) . .
O1 Si2 O2 112.81(8) . .
O1 Si2 O5 113.56(9) . 7_565
O2 Si2 O5 112.06(9) . 7_565
O1 Si2 C21 104.54(10) . .
O2 Si2 C21 105.72(10) . .
O5 Si2 C21 107.38(10) 7_565 .
Si2 O2 Si3 141.66(11) . .
O3 Si3 O2 113.55(9) . .
O3 Si3 O6 112.04(9) . 7_565
O2 Si3 O6 113.64(9) . 7_565
O3 Si3 C31 105.24(10) . .
O2 Si3 C31 104.70(11) . .
O6 Si3 C31 106.77(11) 7_565 .
Si4 O3 Si3 140.53(11) . .
O3 Si4 O4 113.29(9) . .
O3 Si4 O5 112.75(9) . .
O4 Si4 O5 112.87(9) . .
O3 Si4 C41 106.42(10) . .
O4 Si4 C41 103.19(10) . .
O5 Si4 C41 107.46(10) . .
Si1 O4 Si4 142.13(11) . .
Si2 O5 Si4 140.32(11) 7_565 .
Si1 O6 Si3 140.41(11) . 7_565
C12 C11 Si1 114.14(17) . .
C12 C11 H11A 108.7 . .
Si1 C11 H11A 108.7 . .
C12 C11 H11B 108.7 . .
Si1 C11 H11B 108.7 . .
H11A C11 H11B 107.6 . .
C13 C12 C11 112.7(2) . .
C13 C12 H12A 109.0 . .
C11 C12 H12A 109.0 . .
C13 C12 H12B 109.0 . .
C11 C12 H12B 109.0 . .
H12A C12 H12B 107.8 . .
N11 C13 C12 178.1(3) . .
C22 C21 Si2 115.61(18) . .
C22 C21 H21A 108.4 . .
Si2 C21 H21A 108.4 . .
C22 C21 H21B 108.4 . .
Si2 C21 H21B 108.4 . .
H21A C21 H21B 107.4 . .
C23 C22 C21 112.8(2) . .
C23 C22 H22A 109.0 . .
C21 C22 H22A 109.0 . .
C23 C22 H22B 109.0 . .
C21 C22 H22B 109.0 . .
H22A C22 H22B 107.8 . .
N21 C23 C22 179.0(5) . .
C32 C31 Si3 116.5(2) . .
C32 C31 H31A 108.2 . .
Si3 C31 H31A 108.2 . .
C32 C31 H31B 108.2 . .
Si3 C31 H31B 108.2 . .
H31A C31 H31B 107.3 . .
C33 C32 C31 113.0(3) . .
C33 C32 H32A 109.0 . .
C31 C32 H32A 109.0 . .
C33 C32 H32B 109.0 . .
C31 C32 H32B 109.0 . .
H32A C32 H32B 107.8 . .
N31 C33 C32 178.4(4) . .
C42 C41 Si4 112.92(17) . .
C42 C41 H41A 109.0 . .
Si4 C41 H41A 109.0 . .
C42 C41 H41B 109.0 . .
Si4 C41 H41B 109.0 . .
H41A C41 H41B 107.8 . .
C43 C42 C41 111.4(2) . .
C43 C42 H42A 109.3 . .
C41 C42 H42A 109.3 . .
C43 C42 H42B 109.3 . .
C41 C42 H42B 109.3 . .
H42A C42 H42B 108.0 . .
N41 C43 C42 177.8(4) . .
C55 N51 C55 108.3(3) 2_554 .
C55 N51 C51 110.32(13) 2_554 .
C55 N51 C51 109.95(13) . .
C55 N51 C51 109.95(13) 2_554 2_554
C55 N51 C51 110.32(13) . 2_554
C51 N51 C51 108.0(3) . 2_554
C52 C51 N51 114.4(2) . .
C52 C51 H51A 108.7 . .
N51 C51 H51A 108.7 . .
C52 C51 H51B 108.7 . .
N51 C51 H51B 108.7 . .
H51A C51 H51B 107.6 . .
C51 C52 C53 111.2(2) . .
C51 C52 H52A 109.4 . .
C53 C52 H52A 109.4 . .
C51 C52 H52B 109.4 . .
C53 C52 H52B 109.4 . .
H52A C52 H52B 108.0 . .
C54 C53 C52 111.0(3) . .
C54 C53 H53A 109.4 . .
C52 C53 H53A 109.4 . .
C54 C53 H53B 109.4 . .
C52 C53 H53B 109.4 . .
H53A C53 H53B 108.0 . .
C53 C54 H54A 109.5 . .
C53 C54 H54B 109.5 . .
H54A C54 H54B 109.5 . .
C53 C54 H54C 109.5 . .
H54A C54 H54C 109.5 . .
H54B C54 H54C 109.5 . .
N51 C55 C56 114.3(2) . .
N51 C55 H55A 108.7 . .
C56 C55 H55A 108.7 . .
N51 C55 H55B 108.7 . .
C56 C55 H55B 108.7 . .
H55A C55 H55B 107.6 . .
C57 C56 C55 110.7(2) . .
C57 C56 H56A 109.5 . .
C55 C56 H56A 109.5 . .
C57 C56 H56B 109.5 . .
C55 C56 H56B 109.5 . .
H56A C56 H56B 108.1 . .
C58 C57 C56 111.8(2) . .
C58 C57 H57A 109.3 . .
C56 C57 H57A 109.3 . .
C58 C57 H57B 109.3 . .
C56 C57 H57B 109.3 . .
H57A C57 H57B 107.9 . .
C57 C58 H58A 109.5 . .
C57 C58 H58B 109.5 . .
H58A C58 H58B 109.5 . .
C57 C58 H58C 109.5 . .
H58A C58 H58C 109.5 . .
H58B C58 H58C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 O4 1.6181(16) .
Si1 O6 1.6234(18) .
Si1 O1 1.6246(17) .
Si1 C11 1.857(2) .
O1 Si2 1.6184(17) .
Si2 O2 1.6235(17) .
Si2 O5 1.6254(17) 7_565
Si2 C21 1.859(3) .
O2 Si3 1.6247(18) .
Si3 O3 1.6239(17) .
Si3 O6 1.6256(18) 7_565
Si3 C31 1.860(2) .
O3 Si4 1.6208(17) .
Si4 O4 1.6235(17) .
Si4 O5 1.6253(18) .
Si4 C41 1.860(2) .
O5 Si2 1.6254(17) 7_565
O6 Si3 1.6256(18) 7_565
C11 C12 1.526(3) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
N11 C13 1.139(4) .
C12 C13 1.466(4) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C21 C22 1.531(3) .
C21 H21A 0.9900 .
C21 H21B 0.9900 .
N21 C23 1.132(5) .
C22 C23 1.454(4) .
C22 H22A 0.9900 .
C22 H22B 0.9900 .
C31 C32 1.545(4) .
C31 H31A 0.9900 .
C31 H31B 0.9900 .
N31 C33 1.149(5) .
C32 C33 1.485(5) .
C32 H32A 0.9900 .
C32 H32B 0.9900 .
C41 C42 1.533(3) .
C41 H41A 0.9900 .
C41 H41B 0.9900 .
N41 C43 1.140(4) .
C42 C43 1.469(4) .
C42 H42A 0.9900 .
C42 H42B 0.9900 .
N51 C55 1.517(3) 2_554
N51 C55 1.517(3) .
N51 C51 1.523(3) .
N51 C51 1.523(3) 2_554
C51 C52 1.522(4) .
C51 H51A 0.9900 .
C51 H51B 0.9900 .
C52 C53 1.526(4) .
C52 H52A 0.9900 .
C52 H52B 0.9900 .
C53 C54 1.523(4) .
C53 H53A 0.9900 .
C53 H53B 0.9900 .
C54 H54A 0.9800 .
C54 H54B 0.9800 .
C54 H54C 0.9800 .
C55 C56 1.522(3) .
C55 H55A 0.9900 .
C55 H55B 0.9900 .
C56 C57 1.518(3) .
C56 H56A 0.9900 .
C56 H56B 0.9900 .
C57 C58 1.510(4) .
C57 H57A 0.9900 .
C57 H57B 0.9900 .
C58 H58A 0.9800 .
C58 H58B 0.9800 .
C58 H58C 0.9800 .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.971 0.250 239 33 ' '
2 0.000 0.029 0.750 239 33 ' '
3 0.500 0.471 0.250 239 33 ' '
4 0.500 0.529 0.750 239 33 ' '
