#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:51:08 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179493 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/90/4339068.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_4339068
loop_
_publ_author_name
'Wei, Meilin'
'He, Cheng'
'Sun, Qiaozhen'
'Meng, Qingjin'
'Duan, Chunying'
_publ_section_title
;
 Zeolite ionic crystals assembled through direct incorporation of
 polyoxometalate clusters within 3D metal-organic frameworks.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5957
_journal_page_last               5966
_journal_paper_doi               10.1021/ic070274o
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C144 H187 N36 Ni4 O171 P3 W36'
_chemical_formula_weight         12104.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           204
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-I 2 2 3'
_symmetry_space_group_name_H-M   'I m -3'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   23.1330(11)
_cell_length_b                   23.1330(11)
_cell_length_c                   23.1330(11)
_cell_measurement_reflns_used    5704
_cell_measurement_temperature    293(2)
_cell_measurement_theta_min      2.228.45
_cell_volume                     12379.3(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1031
_diffrn_reflns_av_sigmaI/netI    0.0789
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31414
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    17.079
_exptl_absorpt_correction_T_max  0.46
_exptl_absorpt_correction_T_min  0.17
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Crystal Faces, Bruker(2005)'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    3.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             10984
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.660
_refine_diff_density_min         -7.033
_refine_diff_density_rms         0.454
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2553
_refine_ls_number_restraints     246
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0743
_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)+(0.1800P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2362
_refine_ls_wR_factor_ref         0.2498
_reflns_number_gt                1610
_reflns_number_total             1976
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070274osi20070211_065642.cif
_cod_data_source_block           sad
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according
to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'Im-3  '
_cod_database_code               4339068
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'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'
'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, x+1/2, -y+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, x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-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'
'-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, -x+1/2, y+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, -x+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
_atom_site_disorder_group
W1 W 0.39126(3) 0.07665(2) 0.42300(3) 0.01723(16) Uani 1 1 d U .
W2 W 0.5000 0.15366(5) 0.5000 0.0136(2) Uani 1 4 d SU .
W3 W 0.5000 0.0000 0.34565(5) 0.0226(3) Uani 1 4 d SU .
P1 P 0.5000 0.0000 0.5000 0.0127(18) Uani 1 8 d SU .
O1 O 0.4676(11) 0.0519(12) 0.5000 0.0168(18) Uiso 0.50 2 d SPU 1
O1' O 0.4573(12) 0.0000 0.4459(11) 0.016(2) Uiso 0.50 2 d SPU 2
O2 O 0.3646(7) 0.0801(6) 0.5000 0.023(2) Uani 1 2 d SU .
O3 O 0.4432(5) 0.1380(5) 0.4436(4) 0.0241(17) Uani 1 1 d U .
O4 O 0.5000 0.2238(9) 0.5000 0.029(5) Uani 1 4 d SU .
O5 O 0.5000 0.0000 0.2721(9) 0.025(3) Uani 1 4 d SU .
O6 O 0.3390(5) 0.1116(5) 0.3886(5) 0.040(3) Uani 1 1 d U .
O8 O 0.4569(9) 0.0562(9) 0.3747(9) 0.020(2) Uiso 0.50 1 d PU 1
O7 O 0.3776(13) 0.0000 0.4314(12) 0.018(2) Uiso 0.50 2 d SPU 1
O8' O 0.4357(9) 0.0595(9) 0.3550(9) 0.020(2) Uiso 0.50 1 d PU 2
O7' O 0.3507(12) 0.0000 0.4097(12) 0.016(3) Uiso 0.50 2 d SPU 2
Ni1 Ni 0.2500 0.2500 0.2500 0.0103(8) Uani 1 6 d SU .
O9 O 0.2092(4) 0.2756(4) 0.1765(4) 0.0148(15) Uani 1 1 d U .
N1 N 0.1508(5) 0.2773(5) 0.1764(5) 0.0132(16) Uani 1 1 d U .
C1 C 0.1237(6) 0.2468(6) 0.1372(6) 0.0151(17) Uani 1 1 d U .
H1A H 0.1442 0.2247 0.1107 0.018 Uiso 1 1 calc R .
C2 C 0.0646(6) 0.2483(6) 0.1358(6) 0.0172(19) Uani 1 1 d U .
H2A H 0.0454 0.2245 0.1097 0.021 Uiso 1 1 calc R .
C3 C 0.0325(5) 0.2832(6) 0.1713(6) 0.0118(18) Uani 1 1 d U .
C4 C 0.0639(5) 0.3169(6) 0.2097(6) 0.0110(18) Uani 1 1 d U .
H4A H 0.0440 0.3414 0.2347 0.013 Uiso 1 1 calc R .
C5 C 0.1248(6) 0.3154(6) 0.2124(6) 0.0127(17) Uani 1 1 d U .
H5A H 0.1458 0.3390 0.2373 0.015 Uiso 1 1 calc R .
O1W O 0.6056(12) 0.3342(12) 0.5000 0.077(4) Uani 1 2 d SU .
O3W O 0.5000 0.353(3) 0.463(3) 0.10(2) Uiso 0.50 2 d SP .
O4W O 0.5000 0.5000 0.5000 0.23(9) Uiso 1 24 d S .
O2W O 0.6009(7) 0.3991(7) 0.3991(7) 0.056(7) Uani 1 3 d S .
C7 C 0.7530(11) 0.1552(14) 0.5000 0.053(9) Uani 1 2 d S .
H7C H 0.7768 0.1584 0.5339 0.063 Uiso 0.50 1 d PR .
H7A H 0.7339 0.1184 0.5000 0.063 Uiso 1 2 d SR .
C6 C 0.7116(11) 0.1981(11) 0.5000 0.035(6) Uani 1 2 d S .
N2 N 0.6743(14) 0.2362(10) 0.5000 0.055(8) Uani 1 2 d S .
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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
O6 W1 O7 113.7(10) . .
O6 W1 O2 101.2(6) . .
O7 W1 O2 83.3(10) . .
O6 W1 O8' 95.6(8) . .
O7 W1 O8' 88.8(11) . .
O2 W1 O8' 163.2(8) . .
O6 W1 O3 102.4(5) . .
O7 W1 O3 143.7(10) . .
O2 W1 O3 86.5(5) . .
O8' W1 O3 91.2(7) . .
O6 W1 O8 114.4(8) . .
O7 W1 O8 87.7(11) . .
O2 W1 O8 144.0(8) . .
O8' W1 O8 20.1(8) . .
O3 W1 O8 80.4(7) . .
O6 W1 O7' 90.9(8) . .
O7 W1 O7' 23.1(10) . .
O2 W1 O7' 91.7(9) . .
O8' W1 O7' 86.7(10) . .
O3 W1 O7' 166.6(8) . .
O8 W1 O7' 93.5(10) . .
O6 W1 O1' 158.5(7) . .
O7 W1 O1' 50.5(10) . .
O2 W1 O1' 91.8(8) . .
O8' W1 O1' 71.8(9) . .
O3 W1 O1' 95.3(6) . .
O8 W1 O1' 56.6(9) . .
O7' W1 O1' 71.5(9) . .
O4 W2 O3 101.1(3) . 26_556
O4 W2 O3 101.1(3) . .
O3 W2 O3 87.5(6) 26_556 .
O4 W2 O3 101.1(3) . 3_656
O3 W2 O3 88.2(6) 26_556 3_656
O3 W2 O3 157.9(7) . 3_656
O4 W2 O3 101.1(3) . 28_655
O3 W2 O3 157.9(7) 26_556 28_655
O3 W2 O3 88.2(6) . 28_655
O3 W2 O3 87.5(6) 3_656 28_655
O4 W2 O1 162.3(6) . .
O3 W2 O1 66.8(5) 26_556 .
O3 W2 O1 66.8(5) . .
O3 W2 O1 91.6(6) 3_656 .
O3 W2 O1 91.6(6) 28_655 .
O4 W2 O1 162.3(6) . 3_656
O3 W2 O1 91.6(6) 26_556 3_656
O3 W2 O1 91.6(6) . 3_656
O3 W2 O1 66.8(5) 3_656 3_656
O3 W2 O1 66.8(5) 28_655 3_656
O1 W2 O1 35.3(12) . 3_656
O5 W3 O8 112.3(7) . 27
O5 W3 O8 112.3(7) . .
O8 W3 O8 94.5(13) 27 .
O5 W3 O8 112.3(7) . 28_655
O8 W3 O8 135.4(14) 27 28_655
O8 W3 O8 68.6(13) . 28_655
O5 W3 O8 112.3(7) . 2_655
O8 W3 O8 68.6(13) 27 2_655
O8 W3 O8 135.4(14) . 2_655
O8 W3 O8 94.5(13) 28_655 2_655
O5 W3 O8' 96.1(6) . 27
O8 W3 O8' 18.7(8) 27 27
O8 W3 O8' 92.5(8) . 27
O8 W3 O8' 150.1(10) 28_655 27
O8 W3 O8' 82.8(9) 2_655 27
O5 W3 O8' 96.1(6) . .
O8 W3 O8' 92.5(8) 27 .
O8 W3 O8' 18.7(8) . .
O8 W3 O8' 82.8(9) 28_655 .
O8 W3 O8' 150.1(10) 2_655 .
O8' W3 O8' 84.9(12) 27 .
O5 W3 O8' 96.1(6) . 28_655
O8 W3 O8' 150.1(10) 27 28_655
O8 W3 O8' 82.8(9) . 28_655
O8 W3 O8' 18.7(8) 28_655 28_655
O8 W3 O8' 92.5(8) 2_655 28_655
O8' W3 O8' 167.8(12) 27 28_655
O8' W3 O8' 93.8(12) . 28_655
O5 W3 O8' 96.1(6) . 2_655
O8 W3 O8' 82.8(9) 27 2_655
O8 W3 O8' 150.1(10) . 2_655
O8 W3 O8' 92.5(8) 28_655 2_655
O8 W3 O8' 18.7(8) 2_655 2_655
O8' W3 O8' 93.8(12) 27 2_655
O8' W3 O8' 167.8(12) . 2_655
O8' W3 O8' 84.9(12) 28_655 2_655
O5 W3 O1' 156.9(6) . 2_655
O8 W3 O1' 82.6(8) 27 2_655
O8 W3 O1' 82.6(8) . 2_655
O8 W3 O1' 55.3(7) 28_655 2_655
O8 W3 O1' 55.3(7) 2_655 2_655
O8' W3 O1' 100.9(8) 27 2_655
O8' W3 O1' 100.9(8) . 2_655
O8' W3 O1' 67.5(7) 28_655 2_655
O8' W3 O1' 67.5(7) 2_655 2_655
O5 W3 O1' 156.9(6) . .
O8 W3 O1' 55.3(7) 27 .
O8 W3 O1' 55.3(7) . .
O8 W3 O1' 82.6(8) 28_655 .
O8 W3 O1' 82.6(8) 2_655 .
O8' W3 O1' 67.5(7) 27 .
O8' W3 O1' 67.5(7) . .
O8' W3 O1' 100.9(8) 28_655 .
O8' W3 O1' 100.9(8) 2_655 .
O1' W3 O1' 46.1(12) 2_655 .
O1 P1 O1 116(2) 27 .
O1 P1 O1 180.0(12) 27 3_656
O1 P1 O1 64(2) . 3_656
O1 P1 O1 64(2) 27 25_656
O1 P1 O1 180.000(7) . 25_656
O1 P1 O1 116(2) 3_656 25_656
O1 P1 O1' 70.9(7) 27 26_556
O1 P1 O1' 70.9(7) . 26_556
O1 P1 O1' 109.1(7) 3_656 26_556
O1 P1 O1' 109.1(7) 25_656 26_556
O1 P1 O1' 70.9(7) 27 .
O1 P1 O1' 70.9(7) . .
O1 P1 O1' 109.1(7) 3_656 .
O1 P1 O1' 109.1(7) 25_656 .
O1' P1 O1' 103.5(19) 26_556 .
O1 P1 O1' 109.1(7) 27 25_656
O1 P1 O1' 109.1(7) . 25_656
O1 P1 O1' 70.9(7) 3_656 25_656
O1 P1 O1' 70.9(7) 25_656 25_656
O1' P1 O1' 76.5(19) 26_556 25_656
O1' P1 O1' 180.0(12) . 25_656
O1 P1 O1' 109.1(7) 27 2_655
O1 P1 O1' 109.1(7) . 2_655
O1 P1 O1' 70.9(7) 3_656 2_655
O1 P1 O1' 70.9(7) 25_656 2_655
O1' P1 O1' 180.000(5) 26_556 2_655
O1' P1 O1' 76.5(19) . 2_655
O1' P1 O1' 103.5(19) 25_656 2_655
P1 O1 O1 58.0(11) . 3_656
P1 O1 W2 130.4(15) . .
O1 O1 W2 72.3(6) 3_656 .
P1 O1' W1 124.6(8) . 27
P1 O1' W1 124.6(8) . .
W1 O1' W1 95.2(10) 27 .
P1 O1' W3 118.7(14) . .
W1 O1' W3 92.7(8) 27 .
W1 O1' W3 92.7(8) . .
W1 O2 W1 141.5(9) . 26_556
W2 O3 W1 138.5(6) . .
W3 O8 W1 146.8(12) . .
W1 O7 W1 156.4(18) . 27
W1 O8' W3 128.1(11) . .
W1 O7' W1 121.8(14) . 27
O9 Ni1 O9 90.5(4) 5 45
O9 Ni1 O9 89.5(4) 5 .
O9 Ni1 O9 90.5(4) 45 .
O9 Ni1 O9 89.5(4) 5 9
O9 Ni1 O9 180.0(5) 45 9
O9 Ni1 O9 89.5(4) . 9
O9 Ni1 O9 90.5(4) 5 37
O9 Ni1 O9 89.5(4) 45 37
O9 Ni1 O9 180.0(3) . 37
O9 Ni1 O9 90.5(4) 9 37
O9 Ni1 O9 180.0(5) 5 41
O9 Ni1 O9 89.5(4) 45 41
O9 Ni1 O9 90.5(4) . 41
O9 Ni1 O9 90.5(4) 9 41
O9 Ni1 O9 89.5(4) 37 41
N1 O9 Ni1 118.3(7) . .
C1 N1 O9 117.7(11) . .
C1 N1 C5 124.4(12) . .
O9 N1 C5 117.4(11) . .
N1 C1 C2 118.8(13) . .
N1 C1 H1A 120.6 . .
C2 C1 H1A 120.6 . .
C1 C2 C3 122.8(13) . .
C1 C2 H2A 118.6 . .
C3 C2 H2A 118.6 . .
C2 C3 C4 115.6(12) . .
C2 C3 C3 122.8(8) . 28
C4 C3 C3 121.5(7) . 28
C3 C4 C5 122.5(12) . .
C3 C4 H4A 118.8 . .
C5 C4 H4A 118.8 . .
N1 C5 C4 115.6(12) . .
N1 C5 H5A 122.2 . .
C4 C5 H5A 122.2 . .
C6 C7 H7C 110.0 . .
C6 C7 H7A 108.5 . .
H7C C7 H7A 109.5 . .
N2 C6 C7 180(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O6 1.657(12) .
W1 O7 1.811(6) .
W1 O2 1.887(5) .
W1 O8' 1.92(2) .
W1 O3 1.920(11) .
W1 O8 1.94(2) .
W1 O7' 2.029(14) .
W1 O1' 2.400(18) .
W2 O4 1.62(2) .
W2 O3 1.887(11) 26_556
W2 O3 1.887(11) .
W2 O3 1.887(11) 3_656
W2 O3 1.887(11) 28_655
W2 O1 2.47(3) .
W2 O1 2.47(3) 3_656
W3 O5 1.70(2) .
W3 O8 1.77(2) 27
W3 O8 1.77(2) .
W3 O8 1.77(2) 28_655
W3 O8 1.77(2) 2_655
W3 O8' 2.04(2) 27
W3 O8' 2.04(2) .
W3 O8' 2.04(2) 28_655
W3 O8' 2.04(2) 2_655
W3 O1' 2.52(3) 2_655
W3 O1' 2.52(3) .
P1 O1 1.41(3) 27
P1 O1 1.41(3) .
P1 O1 1.41(3) 3_656
P1 O1 1.41(3) 25_656
P1 O1' 1.59(3) 26_556
P1 O1' 1.59(3) .
P1 O1' 1.59(3) 25_656
P1 O1' 1.59(3) 2_655
O1 O1 1.50(5) 3_656
O1' W1 2.400(18) 27
O2 W1 1.887(5) 26_556
O7 W1 1.811(6) 27
O7' W1 2.029(14) 27
Ni1 O9 2.032(9) 5
Ni1 O9 2.032(9) 45
Ni1 O9 2.032(9) .
Ni1 O9 2.032(9) 9
Ni1 O9 2.032(9) 37
Ni1 O9 2.032(9) 41
O9 N1 1.353(14) .
N1 C1 1.308(18) .
N1 C5 1.354(17) .
C1 C2 1.368(19) .
C1 H1A 0.9300 .
C2 C3 1.370(19) .
C2 H2A 0.9300 .
C3 C4 1.387(19) .
C3 C3 1.50(2) 28
C4 C5 1.412(18) .
C4 H4A 0.9300 .
C5 H5A 0.9300 .
O3W O3W 1.72(13) 26_556
C7 C6 1.38(4) .
C7 H7C 0.9592 .
C7 H7A 0.9590 .
C6 N2 1.23(4) .
