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#$Date: 2016-03-21 19:10:27 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178838 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/92/4109203.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_4109203
loop_
_publ_author_name
'Michael A. Shestopalov'
'Yuri V. Mironov'
'Konstantin A. Brylev'
'Svetlana G. Kozlova'
'Vladimir E. Fedorov'
'Hartmut Spies'
'Hans-Jürgen Pietzsch'
'Holger Stephan'
'Gerhard Geipel'
'Gerd Bernhard'
_publ_contact_author_address
;Nikolaev Institute of Inorganic Chemistry,
SB Russian Academy of Sciences,
Akad. Lavrentiev prospekt 3,
Novosibirsk 90,
630090 Russia
;
_publ_contact_author_email       fed@che.nsk.su
_publ_contact_author_fax         '007 383 3309489'
_publ_contact_author_name        'Prof. Vladimir E. Fedorov'
_publ_contact_author_phone       '007 383 3309253'
_publ_section_title
;
 Cluster Core Controlled Reactions of Substitution of Terminal Bromide
 Ligands by Triphenylphosphine in Octahedral Rhenium Chalcobromide
 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3714
_journal_page_last               3721
_journal_paper_doi               10.1021/ja0668062
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         cis-[{Re6S6Be2}(PPh3)2Br4]
_chemical_formula_sum            'C36 H30 Br6 P2 Re6 S6'
_chemical_formula_weight         2313.56
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 105.38(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.302(2)
_cell_length_b                   20.292(4)
_cell_length_c                   12.108(2)
_cell_measurement_reflns_used    1221
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.27
_cell_measurement_theta_min      2.66
_cell_volume                     2440.5(9)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2004)'
_computing_publication_material  'SHELXTL (Bruker, 2004)'
_computing_structure_refinement  'SHELXTL (Bruker, 2004)'
_computing_structure_solution    'SHELXTL (Bruker, 2004)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD area-detector'
_diffrn_measurement_method       'φ 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  0.1789
_diffrn_reflns_av_sigmaI/netI    0.0686
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12764
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.88
_diffrn_reflns_theta_min         2.31
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.081
_exptl_absorpt_correction_T_max  0.403
_exptl_absorpt_correction_T_min  0.118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.148
_exptl_crystal_description       prism
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.368
_refine_diff_density_min         -1.943
_refine_diff_density_rms         0.442
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.789
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         4626
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.787
_refine_ls_R_factor_all          0.2121
_refine_ls_R_factor_gt           0.0700
_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)+(0.0829P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1575
_refine_ls_wR_factor_ref         0.1934
_reflns_number_gt                1662
_reflns_number_total             4626
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ja0668062si20061208_071712_6.cif
_cod_data_source_block           compound5
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4109203
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
Re1 Re 0.57628(11) 0.68518(6) 0.21630(9) 0.0378(3) Uani 1 1 d .
Re2 Re 0.36303(10) 0.68451(6) 0.04445(9) 0.0411(3) Uani 1 1 d .
Re3 Re 0.57916(15) 0.7500 0.03164(13) 0.0394(5) Uani 1 2 d S
Re4 Re 0.36290(15) 0.7500 0.23172(13) 0.0407(5) Uani 1 2 d S
Br5 Br 0.1472(5) 0.7500 0.0569(4) 0.0679(14) Uani 1 2 d S
Br3 Br 0.7327(5) 0.7500 -0.1002(4) 0.0655(14) Uani 1 2 d S
Br6 Br 0.3658(5) 0.7500 -0.1431(4) 0.0615(14) Uani 1 2 d S
Br2 Br 0.2248(3) 0.59536(18) -0.0744(3) 0.0653(10) Uani 1 1 d .
Br4 Br 0.2173(5) 0.7500 0.3708(4) 0.0652(14) Uani 1 2 d S
S1 S 0.7690(9) 0.7500 0.2027(7) 0.030(2) Uani 1 2 d S
S3 S 0.3696(7) 0.6292(3) 0.2243(5) 0.0343(17) Uani 1 1 d .
S4 S 0.5705(8) 0.7500 0.3892(6) 0.0171(18) Uani 1 2 d S
S2 S 0.5679(6) 0.6296(3) 0.0367(5) 0.0332(17) Uani 1 1 d .
P1 P 0.7352(7) 0.5983(3) 0.3209(6) 0.0386(18) Uani 1 1 d .
C11 C 0.829(2) 0.6269(8) 0.4656(14) 0.058(9) Uani 1 1 d G
C12 C 0.7586(17) 0.6363(9) 0.547(2) 0.077(12) Uani 1 1 d G
H12 H 0.6666 0.6279 0.5291 0.093 Uiso 1 1 calc R
C13 C 0.825(3) 0.6584(10) 0.6563(17) 0.082(11) Uani 1 1 d GU
H13 H 0.7778 0.6647 0.7110 0.099 Uiso 1 1 calc R
C14 C 0.963(3) 0.6710(10) 0.6835(15) 0.118(16) Uani 1 1 d GU
H14 H 1.0072 0.6858 0.7564 0.142 Uiso 1 1 calc R
C15 C 1.0335(17) 0.6616(10) 0.602(2) 0.096(13) Uani 1 1 d G
H15 H 1.1255 0.6700 0.6200 0.115 Uiso 1 1 calc R
C16 C 0.967(2) 0.6395(10) 0.4928(18) 0.066(10) Uani 1 1 d G
H16 H 1.0143 0.6332 0.4381 0.079 Uiso 1 1 calc R
C21 C 0.656(2) 0.5165(8) 0.346(2) 0.061(9) Uani 1 1 d G
C22 C 0.699(2) 0.4817(13) 0.4482(16) 0.082(11) Uani 1 1 d G
H22 H 0.7602 0.5008 0.5106 0.098 Uiso 1 1 calc R
C23 C 0.651(2) 0.4185(12) 0.4569(19) 0.101(15) Uani 1 1 d G
H23 H 0.6798 0.3952 0.5253 0.121 Uiso 1 1 calc R
C24 C 0.560(2) 0.3900(8) 0.364(2) 0.090(12) Uani 1 1 d G
H24 H 0.5274 0.3477 0.3695 0.108 Uiso 1 1 calc R
C25 C 0.517(2) 0.4247(11) 0.2615(19) 0.101(13) Uani 1 1 d GU
H25 H 0.4555 0.4057 0.1990 0.121 Uiso 1 1 calc R
C26 C 0.565(2) 0.4880(10) 0.2527(15) 0.079(13) Uani 1 1 d G
H26 H 0.5359 0.5112 0.1844 0.095 Uiso 1 1 calc R
C31 C 0.8651(17) 0.5706(9) 0.2499(15) 0.057(9) Uani 1 1 d G
C32 C 0.8874(17) 0.6027(8) 0.1551(15) 0.060(9) Uani 1 1 d G
H32 H 0.8319 0.6374 0.1215 0.072 Uiso 1 1 calc R
C33 C 0.9925(19) 0.5829(10) 0.1107(13) 0.063(10) Uani 1 1 d G
H33 H 1.0074 0.6044 0.0474 0.076 Uiso 1 1 calc R
C34 C 1.0754(16) 0.5310(10) 0.1611(18) 0.075(11) Uani 1 1 d G
H34 H 1.1457 0.5178 0.1314 0.090 Uiso 1 1 calc R
C35 C 1.0531(17) 0.4990(8) 0.2558(17) 0.071(10) Uani 1 1 d GU
H35 H 1.1085 0.4643 0.2895 0.086 Uiso 1 1 calc R
C36 C 0.948(2) 0.5187(9) 0.3002(13) 0.054(8) Uani 1 1 d GU
H36 H 0.9331 0.4973 0.3636 0.064 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'
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 '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
S1 Re1 S2 91.5(2) . .
S1 Re1 S3 174.6(2) . .
S2 Re1 S3 89.7(2) . .
S1 Re1 S4 88.5(2) . .
S2 Re1 S4 174.6(2) . .
S3 Re1 S4 89.8(2) . .
S1 Re1 P1 88.8(2) . .
S2 Re1 P1 89.4(2) . .
S3 Re1 P1 96.5(2) . .
S4 Re1 P1 96.0(2) . .
S1 Re1 Re2 118.89(19) . .
S2 Re1 Re2 57.20(15) . .
S3 Re1 Re2 57.77(14) . .
S4 Re1 Re2 118.29(18) . .
P1 Re1 Re2 134.54(17) . .
S1 Re1 Re3 58.05(19) . .
S2 Re1 Re3 58.08(15) . .
S3 Re1 Re3 118.62(15) . .
S4 Re1 Re3 117.69(11) . .
P1 Re1 Re3 129.38(17) . .
Re2 Re1 Re3 60.89(5) . .
S1 Re1 Re4 116.88(13) . .
S2 Re1 Re4 117.83(16) . .
S3 Re1 Re4 58.06(16) . .
S4 Re1 Re4 57.64(17) . .
P1 Re1 Re4 140.11(17) . .
Re2 Re1 Re4 60.67(5) . .
Re3 Re1 Re4 90.49(6) . .
S1 Re1 Re1 57.14(12) . 4_575
S2 Re1 Re1 117.64(15) . 4_575
S3 Re1 Re1 117.77(16) . 4_575
S4 Re1 Re1 58.07(10) . 4_575
P1 Re1 Re1 134.66(16) . 4_575
Re2 Re1 Re1 90.30(4) . 4_575
Re3 Re1 Re1 59.62(3) . 4_575
Re4 Re1 Re1 59.75(3) . 4_575
S2 Re2 S3 90.3(2) . .
S2 Re2 Br2 90.82(18) . .
S3 Re2 Br2 93.31(17) . .
S2 Re2 Re1 57.97(14) . .
S3 Re2 Re1 57.88(16) . .
Br2 Re2 Re1 134.07(11) . .
S2 Re2 Br5 176.96(18) . .
S3 Re2 Br5 90.29(18) . .
Br2 Re2 Br5 92.14(11) . .
Re1 Re2 Br5 120.04(11) . .
S2 Re2 Re4 117.90(15) . .
S3 Re2 Re4 57.84(15) . .
Br2 Re2 Re4 136.87(9) . .
Re1 Re2 Re4 59.97(5) . .
Br5 Re2 Re4 60.07(11) . .
S2 Re2 Re3 57.86(16) . .
S3 Re2 Re3 117.52(16) . .
Br2 Re2 Re3 133.71(9) . .
Re1 Re2 Re3 59.68(5) . .
Br5 Re2 Re3 119.31(7) . .
Re4 Re2 Re3 89.40(6) . .
S2 Re2 Br6 89.42(17) . .
S3 Re2 Br6 176.48(17) . .
Br2 Re2 Br6 90.21(11) . .
Re1 Re2 Br6 119.18(11) . .
Br5 Re2 Br6 89.83(13) . .
Re4 Re2 Br6 119.37(7) . .
Re3 Re2 Br6 59.50(11) . .
S2 Re2 Re2 117.53(16) . 4_575
S3 Re2 Re2 117.44(15) . 4_575
Br2 Re2 Re2 136.18(9) . 4_575
Re1 Re2 Re2 89.70(4) . 4_575
Br5 Re2 Re2 59.63(6) . 4_575
Re4 Re2 Re2 59.63(3) . 4_575
Re3 Re2 Re2 59.68(3) . 4_575
Br6 Re2 Re2 59.74(5) . 4_575
S1 Re3 S2 90.65(14) . .
S1 Re3 S2 90.65(14) . 4_575
S2 Re3 S2 173.2(3) . 4_575
S1 Re3 Br3 92.3(2) . .
S2 Re3 Br3 93.31(15) . .
S2 Re3 Br3 93.31(15) 4_575 .
S1 Re3 Re1 57.34(17) . 4_575
S2 Re3 Re1 118.15(15) . 4_575
S2 Re3 Re1 57.47(14) 4_575 4_575
Br3 Re3 Re1 133.99(10) . 4_575
S1 Re3 Re1 57.34(17) . .
S2 Re3 Re1 57.47(14) . .
S2 Re3 Re1 118.15(15) 4_575 .
Br3 Re3 Re1 133.99(10) . .
Re1 Re3 Re1 60.75(6) 4_575 .
S1 Re3 Br6 176.4(2) . .
S2 Re3 Br6 89.14(14) . .
S2 Re3 Br6 89.14(14) 4_575 .
Br3 Re3 Br6 91.25(16) . .
Re1 Re3 Br6 119.78(10) 4_575 .
Re1 Re3 Br6 119.78(10) . .
S1 Re3 Re2 116.72(18) . .
S2 Re3 Re2 56.50(15) . .
S2 Re3 Re2 117.12(16) 4_575 .
Br3 Re3 Re2 135.88(10) . .
Re1 Re3 Re2 90.11(6) 4_575 .
Re1 Re3 Re2 59.43(5) . .
Br6 Re3 Re2 60.34(9) . .
S1 Re3 Re2 116.72(18) . 4_575
S2 Re3 Re2 117.12(16) . 4_575
S2 Re3 Re2 56.50(15) 4_575 4_575
Br3 Re3 Re2 135.88(10) . 4_575
Re1 Re3 Re2 59.43(5) 4_575 4_575
Re1 Re3 Re2 90.11(6) . 4_575
Br6 Re3 Re2 60.34(9) . 4_575
Re2 Re3 Re2 60.64(6) . 4_575
S3 Re4 S3 174.1(3) . 4_575
S3 Re4 S4 90.07(15) . .
S3 Re4 S4 90.07(15) 4_575 .
S3 Re4 Br4 92.96(15) . .
S3 Re4 Br4 92.96(15) 4_575 .
S4 Re4 Br4 91.8(2) . .
S3 Re4 Re1 117.92(16) . 4_575
S3 Re4 Re1 57.44(15) 4_575 4_575
S4 Re4 Re1 58.65(15) . 4_575
Br4 Re4 Re1 134.86(10) . 4_575
S3 Re4 Re1 57.44(15) . .
S3 Re4 Re1 117.92(16) 4_575 .
S4 Re4 Re1 58.65(15) . .
Br4 Re4 Re1 134.86(10) . .
Re1 Re4 Re1 60.51(6) 4_575 .
S3 Re4 Re2 57.12(14) . .
S3 Re4 Re2 117.83(15) 4_575 .
S4 Re4 Re2 118.01(15) . .
Br4 Re4 Re2 135.14(10) . .
Re1 Re4 Re2 90.00(6) 4_575 .
Re1 Re4 Re2 59.37(5) . .
S3 Re4 Re2 117.83(15) . 4_575
S3 Re4 Re2 57.12(14) 4_575 4_575
S4 Re4 Re2 118.01(16) . 4_575
Br4 Re4 Re2 135.14(10) . 4_575
Re1 Re4 Re2 59.37(5) 4_575 4_575
Re1 Re4 Re2 90.00(6) . 4_575
Re2 Re4 Re2 60.74(7) . 4_575
S3 Re4 Br5 89.80(15) . .
S3 Re4 Br5 89.80(15) 4_575 .
S4 Re4 Br5 177.5(2) . .
Br4 Re4 Br5 90.71(16) . .
Re1 Re4 Br5 119.33(10) 4_575 .
Re1 Re4 Br5 119.33(10) . .
Re2 Re4 Br5 59.96(9) . .
Re2 Re4 Br5 59.96(9) 4_575 .
Re2 Br5 Re2 60.74(11) 4_575 .
Re2 Br5 Re4 59.97(10) 4_575 .
Re2 Br5 Re4 59.97(10) . .
Re3 Br6 Re2 60.16(10) . .
Re3 Br6 Re2 60.16(10) . 4_575
Re2 Br6 Re2 60.52(11) . 4_575
Re1 S1 Re1 65.7(2) . 4_575
Re1 S1 Re3 64.6(2) . .
Re1 S1 Re3 64.6(2) 4_575 .
Re2 S3 Re1 64.34(16) . .
Re2 S3 Re4 65.04(17) . .
Re1 S3 Re4 64.50(17) . .
Re4 S4 Re1 63.71(18) . .
Re4 S4 Re1 63.71(18) . 4_575
Re1 S4 Re1 63.87(19) . 4_575
Re2 S2 Re1 64.82(17) . .
Re2 S2 Re3 65.64(18) . .
Re1 S2 Re3 64.45(18) . .
C11 P1 C31 105.7(10) . .
C11 P1 C21 105.1(10) . .
C31 P1 C21 101.6(8) . .
C11 P1 Re1 111.4(6) . .
C31 P1 Re1 115.6(6) . .
C21 P1 Re1 116.3(8) . .
C12 C11 C16 120.0 . .
C12 C11 P1 118.3(14) . .
C16 C11 P1 121.7(14) . .
C13 C12 C11 120.0 . .
C12 C13 C14 120.0 . .
C13 C14 C15 120.0 . .
C16 C15 C14 120.0 . .
C15 C16 C11 120.0 . .
C22 C21 C26 120.0 . .
C22 C21 P1 122.3(14) . .
C26 C21 P1 117.2(14) . .
C21 C22 C23 120.0 . .
C24 C23 C22 120.0 . .
C23 C24 C25 120.0 . .
C26 C25 C24 120.0 . .
C25 C26 C21 120.0 . .
C32 C31 C36 120.0 . .
C32 C31 P1 122.5(11) . .
C36 C31 P1 117.4(11) . .
C31 C32 C33 120.0 . .
C32 C33 C34 120.0 . .
C35 C34 C33 120.0 . .
C34 C35 C36 120.0 . .
C35 C36 C31 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 S1 2.424(8) .
Re1 S2 2.430(6) .
Re1 S3 2.438(7) .
Re1 S4 2.487(6) .
Re1 P1 2.509(7) .
Re1 Re2 2.5945(17) .
Re1 Re3 2.6010(17) .
Re1 Re4 2.6104(17) .
Re1 Re1 2.630(2) 4_575
Re2 S2 2.410(7) .
Re2 S3 2.435(6) .
Re2 Br2 2.507(3) .
Re2 Br5 2.628(4) .
Re2 Re4 2.6286(17) .
Re2 Re3 2.6326(17) .
Re2 Br6 2.637(4) .
Re2 Re2 2.658(3) 4_575
Re3 S1 2.443(9) .
Re3 S2 2.447(7) .
Re3 S2 2.447(7) 4_575
Re3 Br3 2.528(4) .
Re3 Re1 2.6010(17) 4_575
Re3 Br6 2.615(5) .
Re3 Re2 2.6326(17) 4_575
Re4 S3 2.454(7) .
Re4 S3 2.454(7) 4_575
Re4 S4 2.459(8) .
Re4 Br4 2.535(4) .
Re4 Re1 2.6104(17) 4_575
Re4 Re2 2.6286(17) 4_575
Re4 Br5 2.631(5) .
Br5 Re2 2.628(4) 4_575
Br6 Re2 2.637(4) 4_575
S1 Re1 2.424(8) 4_575
S4 Re1 2.487(6) 4_575
P1 C11 1.856(17) .
P1 C31 1.858(14) .
P1 C21 1.910(17) .
C11 C12 1.3900 .
C11 C16 1.3900 .
C12 C13 1.3900 .
C13 C14 1.3900 .
C14 C15 1.3900 .
C15 C16 1.3900 .
C21 C22 1.3900 .
C21 C26 1.3900 .
C22 C23 1.3900 .
C23 C24 1.3900 .
C24 C25 1.3900 .
C25 C26 1.3900 .
C31 C32 1.3900 .
C31 C36 1.3900 .
C32 C33 1.3900 .
C33 C34 1.3900 .
C34 C35 1.3900 .
C35 C36 1.3900 .
