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#$Date: 2016-08-07 11:46:44 +0300 (Sun, 07 Aug 2016) $
#$Revision: 185338 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/03/93/7039382.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_7039382
loop_
_publ_author_name
'Nguyen, H. H.'
'Jegathesh, J. J.'
'Takiden, A.'
'Hauenstein, D.'
'Pham, C. T.'
'Le, C. D.'
'Abram, U.'
_publ_section_title
;
 2,6-Dipicolinoylbis(N,N-dialkylthioureas) as versatile building blocks
 for oligo- and polynuclear architectures.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10771
_journal_page_last               10779
_journal_paper_doi               10.1039/c6dt01389a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         '(C46 H66 Cu2 Dy N10 O12 S4),(Cl),2(C H4 O)'
_chemical_formula_sum            'C48 H74 Cl Cu2 Dy N10 O14 S4'
_chemical_formula_weight         1468.44
_space_group_crystal_system      orthorhombic
_space_group_IT_number           23
_space_group_name_Hall           'I 2 2'
_space_group_name_H-M_alt        'I 2 2 2'
_symmetry_space_group_name_Hall  'I 2 2'
_symmetry_space_group_name_H-M   'I 2 2 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-05-30 deposited with the CCDC.
2016-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.4359(6)
_cell_length_b                   16.1026(10)
_cell_length_c                   18.6442(13)
_cell_measurement_reflns_used    17942
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.18
_cell_measurement_theta_min      2.53
_cell_volume                     3433.3(4)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    ORTEP
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'STOE IPDS T2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0802
_diffrn_reflns_av_unetI/netI     0.0656
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17942
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.185
_diffrn_reflns_theta_min         2.530
_exptl_absorpt_coefficient_mu    1.912
_exptl_absorpt_correction_T_max  .4291
_exptl_absorpt_correction_T_min  .2451
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   X-SHAPE
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       block
_exptl_crystal_F_000             1498
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.902
_refine_diff_density_min         -1.267
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details
;
 Flack x determined using 1573 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.040(7)
_refine_ls_extinction_coef       0.0049(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.880
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         4638
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.880
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0729P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1005
_reflns_Friedel_coverage         0.803
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                4093
_reflns_number_total             4638
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt01389a2.cif
_cod_data_source_block           CuDy_polymer
_cod_depositor_comments
'Adding full bibliography for 7039379--7039383.cif.'
_cod_database_code               7039382
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Dy Dy 0.0000 0.0000 0.0000 0.02354(16) Uani 1 4 d S T P
Cu Cu 0.0000 0.0000 0.19448(5) 0.0398(2) Uani 1 2 d S T P
N1 N 0.0000 0.1586(3) 0.0000 0.0272(10) Uani 1 2 d S T P
C2 C 0.0372(5) 0.2014(3) 0.0572(3) 0.0281(11) Uani 1 1 d . . .
C3 C 0.0404(6) 0.2877(4) 0.0590(4) 0.0363(13) Uani 1 1 d . . .
H3 H 0.0691 0.3157 0.0989 0.044 Uiso 1 1 calc R U .
C4 C 0.0000 0.3310(4) 0.0000 0.0424(17) Uani 1 2 d S T P
H4 H 0.0000 0.3888 0.0000 0.051 Uiso 1 2 calc R U P
S11 S 0.05557(17) 0.08752(11) 0.28187(9) 0.0408(4) Uani 1 1 d . . .
C12 C 0.1468(6) 0.1547(4) 0.2370(4) 0.0353(13) Uani 1 1 d . . .
N13 N 0.1230(5) 0.1878(3) 0.1717(3) 0.0361(11) Uani 1 1 d . . .
C14 C 0.0728(5) 0.1486(3) 0.1195(3) 0.0278(11) Uani 1 1 d . . .
O15 O 0.0508(4) 0.0708(2) 0.1128(2) 0.0287(8) Uani 1 1 d . . .
N16 N 0.2425(5) 0.1846(4) 0.2692(3) 0.0409(13) Uani 1 1 d . . .
C17 C 0.2764(7) 0.1601(5) 0.3419(5) 0.055(2) Uani 1 1 d . . .
H17A H 0.3611 0.1590 0.3452 0.065 Uiso 1 1 calc R U .
H17B H 0.2479 0.1044 0.3514 0.065 Uiso 1 1 calc R U .
C18 C 0.2284(9) 0.2189(7) 0.3983(5) 0.064(2) Uani 1 1 d . . .
H18A H 0.2619 0.2058 0.4441 0.095 Uiso 1 1 calc R U .
H18B H 0.1449 0.2132 0.4008 0.095 Uiso 1 1 calc R U .
H18C H 0.2478 0.2750 0.3857 0.095 Uiso 1 1 calc R U .
C19 C 0.3201(7) 0.2426(5) 0.2329(5) 0.0531(19) Uani 1 1 d . . .
H19A H 0.3585 0.2773 0.2683 0.064 Uiso 1 1 calc R U .
H19B H 0.2744 0.2784 0.2018 0.064 Uiso 1 1 calc R U .
C20 C 0.4102(10) 0.1987(8) 0.1894(8) 0.096(5) Uani 1 1 d . . .
H20A H 0.4604 0.2388 0.1669 0.144 Uiso 1 1 calc R U .
H20B H 0.3725 0.1657 0.1533 0.144 Uiso 1 1 calc R U .
H20C H 0.4559 0.1634 0.2201 0.144 Uiso 1 1 calc R U .
O31 O 0.1929(4) 0.0594(3) -0.0287(3) 0.0348(9) Uani 1 1 d . . .
C32 C 0.2480(5) 0.0000 0.0000 0.0326(14) Uani 1 2 d S T P
C33 C 0.3781(5) 0.0000 0.0000 0.0308(13) Uani 1 2 d S T P
C34 C 0.4391(4) 0.0744(3) -0.0019(6) 0.0373(11) Uani 1 1 d . . .
H34 H 0.3988 0.1243 -0.0056 0.045 Uiso 1 1 calc R U .
O41 O 0.1952(8) -0.0736(6) 0.1740(5) 0.091(2) Uani 1 1 d . . .
H41 H 0.1516 -0.0952 0.2033 0.136 Uiso 1 1 d R U .
C42 C 0.3076(13) -0.0477(10) 0.2022(8) 0.103(5) Uani 1 1 d . . .
H42A H 0.3257 -0.0797 0.2442 0.154 Uiso 1 1 calc R U .
H42B H 0.3045 0.0102 0.2145 0.154 Uiso 1 1 calc R U .
H42C H 0.3669 -0.0564 0.1666 0.154 Uiso 1 1 calc R U .
O61 O 0.2123(13) 0.4659(10) 0.0605(13) 0.091(6) Uani 0.5 1 d . . P
H61 H 0.2303 0.5127 0.0470 0.137 Uiso 0.5 1 calc R U P
C61 C 0.3079(19) 0.4261(11) 0.0836(8) 0.055(4) Uani 0.5 1 d . . P
H61A H 0.3663 0.4659 0.0973 0.083 Uiso 0.5 1 calc R U P
H61B H 0.3379 0.3915 0.0459 0.083 Uiso 0.5 1 calc R U P
H61C H 0.2881 0.3922 0.1242 0.083 Uiso 0.5 1 calc R U P
Cl Cl 0.0000 0.5000 0.1396(4) 0.0711(15) Uani 0.5 2 d S T P
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 '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'
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
_geom_angle_site_symmetry_3
O15 Dy O15 62.60(18) 3 4
O15 Dy O15 124.85(18) 3 2
O15 Dy O15 152.7(2) 4 2
O15 Dy O15 152.7(2) 3 .
O15 Dy O15 124.85(18) 4 .
O15 Dy O15 62.60(18) 2 .
O15 Dy O31 77.45(15) 3 .
O15 Dy O31 81.15(15) 4 .
O15 Dy O31 125.21(15) 2 .
O15 Dy O31 78.15(15) . .
O15 Dy O31 81.15(15) 3 2
O15 Dy O31 77.45(15) 4 2
O15 Dy O31 78.15(15) 2 2
O15 Dy O31 125.21(15) . 2
O31 Dy O31 154.9(2) . 2
O15 Dy O31 78.15(15) 3 3
O15 Dy O31 125.21(15) 4 3
O15 Dy O31 81.15(15) 2 3
O15 Dy O31 77.45(15) . 3
O31 Dy O31 52.8(2) . 3
O31 Dy O31 134.3(2) 2 3
O15 Dy O31 125.21(15) 3 4
O15 Dy O31 78.15(15) 4 4
O15 Dy O31 77.45(15) 2 4
O15 Dy O31 81.15(15) . 4
O31 Dy O31 134.3(2) . 4
O31 Dy O31 52.8(2) 2 4
O31 Dy O31 154.9(2) 3 4
O15 Dy N1 117.57(9) 3 .
O15 Dy N1 62.43(9) 4 .
O15 Dy N1 117.57(9) 2 .
O15 Dy N1 62.43(9) . .
O31 Dy N1 67.17(10) . .
O31 Dy N1 112.83(10) 2 .
O31 Dy N1 112.83(10) 3 .
O31 Dy N1 67.17(10) 4 .
O15 Dy N1 62.43(9) 3 2
O15 Dy N1 117.57(9) 4 2
O15 Dy N1 62.43(9) 2 2
O15 Dy N1 117.57(9) . 2
O31 Dy N1 112.83(10) . 2
O31 Dy N1 67.17(10) 2 2
O31 Dy N1 67.17(10) 3 2
O31 Dy N1 112.83(10) 4 2
N1 Dy N1 180.0 . 2
O15 Dy C32 103.65(10) 3 2
O15 Dy C32 76.35(10) 4 2
O15 Dy C32 76.35(10) 2 2
O15 Dy C32 103.65(10) . 2
O31 Dy C32 153.60(10) . 2
O31 Dy C32 26.40(10) 2 2
O31 Dy C32 153.60(10) 3 2
O31 Dy C32 26.40(10) 4 2
N1 Dy C32 90.0 . 2
N1 Dy C32 90.0 2 2
O15 Dy C32 76.35(10) 3 .
O15 Dy C32 103.65(10) 4 .
O15 Dy C32 103.65(10) 2 .
O15 Dy C32 76.35(10) . .
O31 Dy C32 26.40(10) . .
O31 Dy C32 153.60(10) 2 .
O31 Dy C32 26.40(10) 3 .
O31 Dy C32 153.60(10) 4 .
N1 Dy C32 90.0 . .
N1 Dy C32 90.0 2 .
C32 Dy C32 180.0 2 .
O15 Cu O15 80.1(2) . 2
O15 Cu S11 96.49(13) . .
O15 Cu S11 176.09(12) 2 .
O15 Cu S11 176.09(12) . 2
O15 Cu S11 96.49(13) 2 2
S11 Cu S11 87.00(9) . 2
C2 N1 C2 118.0(6) . 4
C2 N1 Dy 121.0(3) . .
C2 N1 Dy 121.0(3) 4 .
N1 C2 C3 122.9(6) . .
N1 C2 C14 114.4(5) . .
C3 C2 C14 122.8(5) . .
C4 C3 C2 118.4(6) . .
C4 C3 H3 120.8 . .
C2 C3 H3 120.8 . .
C3 C4 C3 119.4(7) . 4
C3 C4 H4 120.3 . .
C3 C4 H4 120.3 4 .
C12 S11 Cu 102.3(2) . .
N16 C12 N13 115.2(6) . .
N16 C12 S11 120.2(5) . .
N13 C12 S11 124.2(5) . .
C14 N13 C12 124.9(5) . .
O15 C14 N13 129.5(6) . .
O15 C14 C2 115.2(5) . .
N13 C14 C2 115.3(5) . .
C14 O15 Cu 122.8(4) . .
C14 O15 Dy 125.5(4) . .
Cu O15 Dy 108.65(17) . .
C12 N16 C19 121.4(6) . .
C12 N16 C17 122.4(6) . .
C19 N16 C17 116.2(6) . .
N16 C17 C18 112.1(7) . .
N16 C17 H17A 109.2 . .
C18 C17 H17A 109.2 . .
N16 C17 H17B 109.2 . .
C18 C17 H17B 109.2 . .
H17A C17 H17B 107.9 . .
C17 C18 H18A 109.5 . .
C17 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C17 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
N16 C19 C20 111.8(8) . .
N16 C19 H19A 109.3 . .
C20 C19 H19A 109.3 . .
N16 C19 H19B 109.3 . .
C20 C19 H19B 109.3 . .
H19A C19 H19B 107.9 . .
C19 C20 H20A 109.5 . .
C19 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
C19 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C32 O31 Dy 93.5(3) . .
O31 C32 O31 120.2(6) 3 .
O31 C32 C33 119.9(3) 3 .
O31 C32 C33 119.9(3) . .
O31 C32 Dy 60.1(3) 3 .
O31 C32 Dy 60.1(3) . .
C33 C32 Dy 180.0 . .
C34 C33 C34 119.6(6) . 3
C34 C33 C32 120.2(3) . .
C34 C33 C32 120.2(3) 3 .
C33 C34 C34 120.1(3) . 4_655
C33 C34 H34 120.0 . .
C34 C34 H34 120.0 4_655 .
C42 O41 H41 114.9 . .
O41 C42 H42A 109.5 . .
O41 C42 H42B 109.5 . .
H42A C42 H42B 109.5 . .
O41 C42 H42C 109.5 . .
H42A C42 H42C 109.5 . .
H42B C42 H42C 109.5 . .
C61 O61 H61 109.5 . .
O61 C61 H61A 109.5 . .
O61 C61 H61B 109.5 . .
H61A C61 H61B 109.5 . .
O61 C61 H61C 109.5 . .
H61A C61 H61C 109.5 . .
H61B C61 H61C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy O15 2.462(4) 3
Dy O15 2.462(4) 4
Dy O15 2.462(4) 2
Dy O15 2.462(4) .
Dy O31 2.463(4) .
Dy O31 2.463(4) 2
Dy O31 2.463(4) 3
Dy O31 2.463(4) 4
Dy N1 2.554(5) .
Dy N1 2.554(5) 2
Dy C32 2.836(6) 2
Dy C32 2.836(6) .
Cu O15 1.988(4) .
Cu O15 1.988(4) 2
Cu S11 2.2459(18) .
Cu S11 2.2460(18) 2
N1 C2 1.339(6) .
N1 C2 1.339(6) 4
C2 C3 1.391(8) .
C2 C14 1.497(8) .
C3 C4 1.381(8) .
C3 H3 0.9300 .
C4 C3 1.381(8) 4
C4 H4 0.9300 .
S11 C12 1.721(7) .
C12 N16 1.337(8) .
C12 N13 1.356(9) .
N13 C14 1.294(8) .
C14 O15 1.284(7) .
N16 C19 1.456(10) .
N16 C17 1.465(10) .
C17 C18 1.519(13) .
C17 H17A 0.9700 .
C17 H17B 0.9700 .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
C19 C20 1.489(14) .
C19 H19A 0.9700 .
C19 H19B 0.9700 .
C20 H20A 0.9600 .
C20 H20B 0.9600 .
C20 H20C 0.9600 .
O31 C32 1.263(5) .
C32 O31 1.263(5) 3
C32 C33 1.489(8) .
C33 C34 1.387(6) .
C33 C34 1.387(6) 3
C34 C34 1.394(9) 4_655
C34 H34 0.9300 .
O41 C42 1.450(16) .
O41 H41 0.8170 .
C42 H42A 0.9600 .
C42 H42B 0.9600 .
C42 H42C 0.9600 .
O61 C61 1.34(3) .
O61 H61 0.8200 .
C61 H61A 0.9600 .
C61 H61B 0.9600 .
C61 H61C 0.9600 .
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
C2 N1 C2 C3 -1.1(4) 4 .
Dy N1 C2 C3 178.9(4) . .
C2 N1 C2 C14 177.8(6) 4 .
Dy N1 C2 C14 -2.2(6) . .
N1 C2 C3 C4 2.1(9) . .
C14 C2 C3 C4 -176.7(5) . .
C2 C3 C4 C3 -1.0(4) . 4
Cu S11 C12 N16 -143.1(5) . .
Cu S11 C12 N13 44.0(6) . .
N16 C12 N13 C14 148.4(6) . .
S11 C12 N13 C14 -38.4(9) . .
C12 N13 C14 O15 -11.3(11) . .
C12 N13 C14 C2 170.0(6) . .
N1 C2 C14 O15 -7.4(7) . .
C3 C2 C14 O15 171.4(6) . .
N1 C2 C14 N13 171.4(5) . .
C3 C2 C14 N13 -9.7(9) . .
N13 C14 O15 Cu 38.0(8) . .
C2 C14 O15 Cu -143.3(4) . .
N13 C14 O15 Dy -163.8(5) . .
C2 C14 O15 Dy 14.8(7) . .
N13 C12 N16 C19 -5.5(10) . .
S11 C12 N16 C19 -179.0(6) . .
N13 C12 N16 C17 175.6(6) . .
S11 C12 N16 C17 2.1(9) . .
C12 N16 C17 C18 -92.7(9) . .
C19 N16 C17 C18 88.4(9) . .
C12 N16 C19 C20 -87.0(11) . .
C17 N16 C19 C20 92.0(10) . .
Dy O31 C32 O31 -0.004(0) . 3
Dy O31 C32 C33 180.0 . .
O31 C32 C33 C34 -152.4(6) 3 .
O31 C32 C33 C34 27.6(6) . .
O31 C32 C33 C34 27.6(6) 3 3
O31 C32 C33 C34 -152.4(6) . 3
C34 C33 C34 C34 -3.3(11) 3 4_655
C32 C33 C34 C34 176.7(11) . 4_655
