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#$Date: 2018-08-16 02:26:01 +0300 (Thu, 16 Aug 2018) $
#$Revision: 209759 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/35/7113590.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_7113590
loop_
_publ_author_name
'Burford, Neil'
'Ragogna, Paul J.'
'McDonald, Robert'
'Ferguson, Michael J.'
_publ_section_title
;
 Homoatomic P →  P coordination: A versatile synthetic approach to
 polyphosphorus dications
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   16
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2066
_journal_page_last               2067
_journal_paper_doi               10.1039/b304984a
_journal_year                    2003
_chemical_formula_moiety         'C32 H36 F6 O6 P4 S2'
_chemical_formula_sum            'C32 H36 F6 O6 P4 S2'
_chemical_formula_weight         818.61
_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                96.528(3)
_cell_angle_beta                 93.131(3)
_cell_angle_gamma                99.431(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6372(12)
_cell_length_b                   13.5443(19)
_cell_length_c                   15.742(2)
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.045
_cell_measurement_theta_min      2.397
_cell_volume                     1799.9(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0679
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11460
_diffrn_reflns_theta_full        26.32
_diffrn_reflns_theta_max         26.32
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    0.400
_exptl_absorpt_correction_T_max  0.9649
_exptl_absorpt_correction_T_min  0.7896
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.797
_refine_diff_density_min         -1.087
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1151
_refine_ls_R_factor_gt           0.0741
_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)+(0.0910P)²+3.3707P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1764
_refine_ls_wR_factor_ref         0.2012
_reflns_number_gt                4743
_reflns_number_total             7168
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7103837
_cod_data_source_file            b304984a.txt
_cod_data_source_block           dal0248
_cod_original_cell_volume        1799.8(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7113590
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
P1 P 0.31313(12) 0.08220(8) 0.45711(7) 0.0248(3) Uani 1 1 d .
P2 P 0.45679(12) 0.21404(8) 0.41233(7) 0.0261(3) Uani 1 1 d .
C1 C 0.4319(5) 0.0174(3) 0.5228(3) 0.0264(9) Uani 1 1 d .
H1A H 0.4745 0.0632 0.5754 0.032 Uiso 1 1 calc R
H1B H 0.3641 -0.0419 0.5403 0.032 Uiso 1 1 calc R
C2 C 0.1559(5) 0.1126(3) 0.5204(3) 0.0310(10) Uani 1 1 d .
H2A H 0.0963 0.0506 0.5369 0.037 Uiso 1 1 calc R
H2B H 0.0858 0.1459 0.4868 0.037 Uiso 1 1 calc R
H2C H 0.2001 0.1579 0.5721 0.037 Uiso 1 1 calc R
C3 C 0.2346(5) -0.0040(4) 0.3644(3) 0.0357(11) Uani 1 1 d .
H3A H 0.1693 -0.0632 0.3821 0.043 Uiso 1 1 calc R
H3B H 0.3212 -0.0251 0.3332 0.043 Uiso 1 1 calc R
H3C H 0.1704 0.0292 0.3270 0.043 Uiso 1 1 calc R
C11 C 0.5944(5) 0.2534(3) 0.5070(3) 0.0243(9) Uani 1 1 d .
C12 C 0.7536(5) 0.2597(3) 0.4927(3) 0.0312(10) Uani 1 1 d .
H12 H 0.7837 0.2451 0.4361 0.037 Uiso 1 1 calc R
C13 C 0.8675(5) 0.2868(3) 0.5597(3) 0.0360(11) Uani 1 1 d .
H13 H 0.9754 0.2909 0.5491 0.043 Uiso 1 1 calc R
C14 C 0.8252(5) 0.3082(4) 0.6423(3) 0.0384(11) Uani 1 1 d .
H14 H 0.9038 0.3271 0.6885 0.046 Uiso 1 1 calc R
C15 C 0.6666(6) 0.3018(4) 0.6576(3) 0.0378(11) Uani 1 1 d .
H15 H 0.6373 0.3153 0.7145 0.045 Uiso 1 1 calc R
C16 C 0.5521(5) 0.2761(3) 0.5908(3) 0.0328(10) Uani 1 1 d .
H16 H 0.4445 0.2739 0.6015 0.039 Uiso 1 1 calc R
C21 C 0.3115(5) 0.2986(3) 0.4186(3) 0.0271(9) Uani 1 1 d .
C22 C 0.1750(5) 0.2723(3) 0.3635(3) 0.0297(9) Uani 1 1 d .
H22 H 0.1550 0.2085 0.3292 0.036 Uiso 1 1 calc R
C23 C 0.0688(5) 0.3375(4) 0.3582(3) 0.0350(11) Uani 1 1 d .
H23 H -0.0243 0.3184 0.3210 0.042 Uiso 1 1 calc R
C24 C 0.0978(6) 0.4300(4) 0.4068(3) 0.0393(11) Uani 1 1 d .
H24 H 0.0257 0.4755 0.4026 0.047 Uiso 1 1 calc R
C25 C 0.2319(6) 0.4572(4) 0.4620(3) 0.0423(12) Uani 1 1 d .
H25 H 0.2514 0.5213 0.4957 0.051 Uiso 1 1 calc R
C26 C 0.3385(5) 0.3914(3) 0.4686(3) 0.0338(10) Uani 1 1 d .
H26 H 0.4297 0.4102 0.5072 0.041 Uiso 1 1 calc R
P3 P 0.16578(18) 0.41778(11) 0.06373(9) 0.0487(4) Uani 1 1 d .
P4 P 0.01633(15) 0.28614(12) 0.10663(8) 0.0435(4) Uani 1 1 d .
C4 C 0.0748(7) 0.4872(5) -0.0136(4) 0.0582(15) Uani 1 1 d .
H4A H 0.1479 0.5500 -0.0199 0.070 Uiso 1 1 calc R
H4B H 0.0564 0.4456 -0.0703 0.070 Uiso 1 1 calc R
C5 C 0.2243(8) 0.5056(4) 0.1587(4) 0.0633(18) Uani 1 1 d .
H5A H 0.2924 0.5655 0.1440 0.076 Uiso 1 1 calc R
H5B H 0.2819 0.4738 0.2004 0.076 Uiso 1 1 calc R
H5C H 0.1307 0.5252 0.1837 0.076 Uiso 1 1 calc R
C6 C 0.3338(8) 0.3900(5) 0.0121(4) 0.0638(17) Uani 1 1 d .
H6A H 0.3933 0.4521 -0.0043 0.077 Uiso 1 1 calc R
H6B H 0.3003 0.3416 -0.0393 0.077 Uiso 1 1 calc R
H6C H 0.4006 0.3609 0.0513 0.077 Uiso 1 1 calc R
C31 C -0.1175(5) 0.2452(4) 0.0110(3) 0.0413(12) Uani 1 1 d .
C32 C -0.2777(5) 0.2299(4) 0.0246(3) 0.0402(11) Uani 1 1 d .
H32 H -0.3097 0.2372 0.0814 0.048 Uiso 1 1 calc R
C33 C -0.3902(6) 0.2044(4) -0.0437(3) 0.0421(12) Uani 1 1 d .
H33 H -0.4989 0.1945 -0.0338 0.050 Uiso 1 1 calc R
C34 C -0.3435(6) 0.1932(4) -0.1268(3) 0.0476(13) Uani 1 1 d .
H34 H -0.4207 0.1766 -0.1739 0.057 Uiso 1 1 calc R
C35 C -0.1868(6) 0.2061(4) -0.1414(3) 0.0496(13) Uani 1 1 d .
H35 H -0.1559 0.1975 -0.1984 0.060 Uiso 1 1 calc R
C36 C -0.0732(6) 0.2318(5) -0.0732(3) 0.0504(14) Uani 1 1 d .
H36 H 0.0352 0.2403 -0.0837 0.060 Uiso 1 1 calc R
C41 C 0.1621(5) 0.2022(3) 0.1030(3) 0.0324(10) Uani 1 1 d .
C42 C 0.2918(6) 0.2262(4) 0.1640(3) 0.0376(11) Uani 1 1 d .
H42 H 0.3031 0.2859 0.2034 0.045 Uiso 1 1 calc R
C43 C 0.4019(6) 0.1644(4) 0.1673(3) 0.0413(12) Uani 1 1 d .
H43 H 0.4910 0.1829 0.2075 0.050 Uiso 1 1 calc R
C44 C 0.3843(6) 0.0755(4) 0.1127(4) 0.0467(13) Uani 1 1 d .
H44 H 0.4590 0.0317 0.1165 0.056 Uiso 1 1 calc R
C45 C 0.2583(6) 0.0509(4) 0.0528(4) 0.0528(14) Uani 1 1 d .
H45 H 0.2472 -0.0097 0.0145 0.063 Uiso 1 1 calc R
C46 C 0.1466(6) 0.1136(4) 0.0475(4) 0.0469(13) Uani 1 1 d .
H46 H 0.0597 0.0956 0.0059 0.056 Uiso 1 1 calc R
S1 S -0.23609(15) 0.05089(11) 0.27278(8) 0.0413(3) Uani 1 1 d .
S2 S 0.26614(15) 0.39071(12) -0.24240(9) 0.0477(4) Uani 1 1 d .
F11 F -0.2566(5) -0.0918(5) 0.1451(2) 0.122(2) Uani 1 1 d .
F12 F -0.0195(4) -0.0214(4) 0.1896(2) 0.0946(15) Uani 1 1 d .
F13 F -0.1500(6) -0.1258(3) 0.2603(3) 0.0970(14) Uani 1 1 d .
F21 F 0.3693(5) 0.5765(3) -0.1784(3) 0.1030(15) Uani 1 1 d .
F22 F 0.4627(5) 0.5329(3) -0.2978(3) 0.0867(13) Uani 1 1 d .
F23 F 0.2259(6) 0.5602(4) -0.2968(4) 0.1145(18) Uani 1 1 d .
O11 O -0.1332(4) 0.0710(3) 0.3501(2) 0.0429(8) Uani 1 1 d .
O12 O -0.3961(4) 0.0065(4) 0.2843(2) 0.0630(12) Uani 1 1 d .
O13 O -0.2216(6) 0.1264(4) 0.2177(3) 0.0900(17) Uani 1 1 d .
O21 O 0.2321(4) 0.3431(3) -0.3291(2) 0.0613(11) Uani 1 1 d .
O22 O 0.1294(5) 0.3953(4) -0.1945(3) 0.0787(15) Uani 1 1 d .
O23 O 0.3975(5) 0.3654(4) -0.1957(3) 0.0684(12) Uani 1 1 d .
C10 C -0.1648(7) -0.0552(7) 0.2142(4) 0.069(2) Uani 1 1 d .
C20 C 0.3320(7) 0.5215(5) -0.2547(4) 0.0624(17) 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'
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
C3 P1 C2 110.0(2) .
C3 P1 C1 107.4(2) .
C2 P1 C1 106.3(2) .
C3 P1 P2 107.45(17) .
C2 P1 P2 114.14(16) .
C1 P1 P2 111.33(15) .
C11 P2 C21 106.54(19) .
C11 P2 P1 98.62(14) .
C21 P2 P1 98.07(14) .
C1 C1 P1 113.2(4) 2_656
C12 C11 C16 118.9(4) .
C12 C11 P2 115.8(3) .
C16 C11 P2 125.3(3) .
C13 C12 C11 120.7(4) .
C12 C13 C14 120.2(4) .
C13 C14 C15 119.7(4) .
C16 C15 C14 120.5(4) .
C15 C16 C11 120.0(4) .
C26 C21 C22 118.8(4) .
C26 C21 P2 122.9(3) .
C22 C21 P2 117.9(3) .
C23 C22 C21 121.0(4) .
C24 C23 C22 119.8(4) .
C23 C24 C25 120.0(4) .
C24 C25 C26 120.5(5) .
C21 C26 C25 119.8(4) .
C6 P3 C5 110.3(3) .
C6 P3 C4 102.0(3) .
C5 P3 C4 106.2(3) .
C6 P3 P4 114.9(2) .
C5 P3 P4 105.5(2) .
C4 P3 P4 117.6(2) .
C31 P4 C41 106.4(2) .
C31 P4 P3 99.74(19) .
C41 P4 P3 97.31(15) .
C4 C4 P3 111.7(6) 2_565
C32 C31 C36 118.5(4) .
C32 C31 P4 115.8(4) .
C36 C31 P4 125.7(4) .
C33 C32 C31 120.8(5) .
C32 C33 C34 119.6(5) .
C35 C34 C33 120.5(5) .
C34 C35 C36 120.2(5) .
C35 C36 C31 120.3(5) .
C46 C41 C42 118.4(4) .
C46 C41 P4 123.8(4) .
C42 C41 P4 117.6(4) .
C43 C42 C41 120.8(5) .
C42 C43 C44 120.4(4) .
C45 C44 C43 119.6(5) .
C44 C45 C46 120.8(5) .
C41 C46 C45 120.0(5) .
O13 S1 O11 116.4(3) .
O13 S1 O12 114.6(3) .
O11 S1 O12 114.5(2) .
O13 S1 C10 104.9(4) .
O11 S1 C10 102.2(2) .
O12 S1 C10 101.6(3) .
O23 S2 O21 116.5(3) .
O23 S2 O22 114.7(3) .
O21 S2 O22 114.4(2) .
O23 S2 C20 102.8(3) .
O21 S2 C20 103.4(3) .
O22 S2 C20 102.3(3) .
F13 C10 F11 109.8(7) .
F13 C10 F12 106.6(6) .
F11 C10 F12 108.0(5) .
F13 C10 S1 112.8(4) .
F11 C10 S1 111.0(5) .
F12 C10 S1 108.4(5) .
F23 C20 F21 108.6(6) .
F23 C20 F22 107.1(6) .
F21 C20 F22 106.4(5) .
F23 C20 S2 112.6(4) .
F21 C20 S2 110.7(5) .
F22 C20 S2 111.2(5) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 C3 1.788(4) .
P1 C2 1.801(4) .
P1 C1 1.810(4) .
P1 P2 2.2092(16) .
P2 C11 1.826(4) .
P2 C21 1.831(4) .
C1 C1 1.522(8) 2_656
C11 C12 1.396(6) .
C11 C16 1.402(6) .
C12 C13 1.377(6) .
C13 C14 1.382(7) .
C14 C15 1.394(7) .
C15 C16 1.377(6) .
C21 C26 1.384(6) .
C21 C22 1.396(6) .
C22 C23 1.380(6) .
C23 C24 1.370(7) .
C24 C25 1.382(7) .
C25 C26 1.389(7) .
P3 C6 1.774(7) .
P3 C5 1.795(5) .
P3 C4 1.839(6) .
P3 P4 2.217(2) .
P4 C31 1.822(5) .
P4 C41 1.828(5) .
C4 C4 1.465(12) 2_565
C31 C32 1.397(7) .
C31 C36 1.400(7) .
C32 C33 1.382(7) .
C33 C34 1.390(7) .
C34 C35 1.372(7) .
C35 C36 1.387(7) .
C41 C46 1.385(7) .
C41 C42 1.405(6) .
C42 C43 1.368(7) .
C43 C44 1.379(7) .
C44 C45 1.371(7) .
C45 C46 1.390(7) .
S1 O13 1.409(4) .
S1 O11 1.439(3) .
S1 O12 1.444(4) .
S1 C10 1.829(7) .
S2 O23 1.428(4) .
S2 O21 1.435(4) .
S2 O22 1.441(4) .
S2 C20 1.805(7) .
F11 C10 1.309(6) .
F12 C10 1.356(7) .
F13 C10 1.282(8) .
F21 C20 1.333(7) .
F22 C20 1.345(8) .
F23 C20 1.312(7) .
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_4
C3 P1 P2 C11 -152.5(2) .
C2 P1 P2 C11 85.2(2) .
C1 P1 P2 C11 -35.2(2) .
C3 P1 P2 C21 99.3(2) .
C2 P1 P2 C21 -23.0(2) .
C1 P1 P2 C21 -143.3(2) .
C3 P1 C1 C1 60.1(5) 2_656
C2 P1 C1 C1 177.9(4) 2_656
P2 P1 C1 C1 -57.3(4) 2_656
C21 P2 C11 C12 -135.3(3) .
P1 P2 C11 C12 123.6(3) .
C21 P2 C11 C16 45.3(4) .
P1 P2 C11 C16 -55.8(4) .
C16 C11 C12 C13 0.6(6) .
P2 C11 C12 C13 -178.8(3) .
C11 C12 C13 C14 0.1(7) .
C12 C13 C14 C15 0.2(7) .
C13 C14 C15 C16 -1.1(7) .
C14 C15 C16 C11 1.8(7) .
C12 C11 C16 C15 -1.6(7) .
P2 C11 C16 C15 177.8(4) .
C11 P2 C21 C26 19.8(4) .
P1 P2 C21 C26 121.4(4) .
C11 P2 C21 C22 -167.2(3) .
P1 P2 C21 C22 -65.7(3) .
C26 C21 C22 C23 0.3(6) .
P2 C21 C22 C23 -172.9(3) .
C21 C22 C23 C24 0.8(7) .
C22 C23 C24 C25 -1.0(7) .
C23 C24 C25 C26 0.2(8) .
C22 C21 C26 C25 -1.2(7) .
P2 C21 C26 C25 171.8(4) .
C24 C25 C26 C21 0.9(7) .
C6 P3 P4 C31 -90.1(3) .
C5 P3 P4 C31 148.3(3) .
C4 P3 P4 C31 30.1(3) .
C6 P3 P4 C41 18.0(3) .
C5 P3 P4 C41 -103.6(3) .
C4 P3 P4 C41 138.1(3) .
C6 P3 C4 C4 176.3(6) 2_565
C5 P3 C4 C4 -68.2(7) 2_565
P4 P3 C4 C4 49.6(7) 2_565
C41 P4 C31 C32 129.8(4) .
P3 P4 C31 C32 -129.5(4) .
C41 P4 C31 C36 -52.6(6) .
P3 P4 C31 C36 48.1(5) .
C36 C31 C32 C33 -1.4(8) .
P4 C31 C32 C33 176.3(4) .
C31 C32 C33 C34 0.3(8) .
C32 C33 C34 C35 0.8(8) .
C33 C34 C35 C36 -0.9(9) .
C34 C35 C36 C31 -0.3(9) .
C32 C31 C36 C35 1.4(9) .
P4 C31 C36 C35 -176.1(5) .
C31 P4 C41 C46 -12.6(5) .
P3 P4 C41 C46 -115.1(4) .
C31 P4 C41 C42 171.7(4) .
P3 P4 C41 C42 69.3(4) .
C46 C41 C42 C43 1.3(7) .
P4 C41 C42 C43 177.2(4) .
C41 C42 C43 C44 -2.3(7) .
C42 C43 C44 C45 2.2(8) .
C43 C44 C45 C46 -1.1(9) .
C42 C41 C46 C45 -0.2(8) .
P4 C41 C46 C45 -175.9(4) .
C44 C45 C46 C41 0.2(9) .
O13 S1 C10 F13 171.1(5) .
O11 S1 C10 F13 49.2(5) .
O12 S1 C10 F13 -69.3(5) .
O13 S1 C10 F11 -65.2(6) .
O11 S1 C10 F11 173.0(5) .
O12 S1 C10 F11 54.5(6) .
O13 S1 C10 F12 53.3(5) .
O11 S1 C10 F12 -68.6(5) .
O12 S1 C10 F12 172.9(4) .
O23 S2 C20 F23 -179.9(5) .
O21 S2 C20 F23 58.5(6) .
O22 S2 C20 F23 -60.7(6) .
O23 S2 C20 F21 -58.1(5) .
O21 S2 C20 F21 -179.7(4) .
O22 S2 C20 F21 61.1(5) .
O23 S2 C20 F22 60.0(5) .
O21 S2 C20 F22 -61.7(5) .
O22 S2 C20 F22 179.2(4) .
