#------------------------------------------------------------------------------
#$Date: 2016-10-08 00:57:19 +0300 (Sat, 08 Oct 2016) $
#$Revision: 187046 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/63/7226359.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_7226359
loop_
_publ_author_name
'Martins, Felipe Terra'
'da Silva, Cleiton Moreira'
'Vasconcelos, Géssica Adriana'
'Gontijo Vaz, Boniek'
'Vieira, Tarcisio da Silva'
'Queiroz Júnior, Luiz Henrique Keng'
'de Fátima, Ângelo'
_publ_section_title
;
 Lower rim dimerization of a calixarene through the encapsulation of
 sodium ions
;
_journal_issue                   37
_journal_name_full               CrystEngComm
_journal_page_first              6987
_journal_paper_doi               10.1039/C6CE01387B
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C78 H74 N2 Na4 O26'
_chemical_formula_weight         1547.35
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           106
_space_group_name_Hall           'P 4c -2ab'
_space_group_name_H-M_alt        'P 42 b c'
_symmetry_space_group_name_Hall  'P 4c -2ab'
_symmetry_space_group_name_H-M   'P 42 b c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2016-08-10 deposited with the CCDC.
2016-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.0771(7)
_cell_length_b                   21.0771(7)
_cell_length_c                   16.6303(5)
_cell_measurement_reflns_used    24382
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.29
_cell_volume                     7387.9(4)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_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  0.1284
_diffrn_reflns_av_unetI/netI     0.1274
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            24383
_diffrn_reflns_point_group_measured_fraction_full 0.868
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.404
_diffrn_reflns_theta_min         2.288
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Blessing, R. H. (1995) Acta Cryst., A51, 33-38'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details
;
 Flack x determined using 858 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.6(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     497
_refine_ls_number_reflns         5868
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1725
_refine_ls_R_factor_gt           0.0662
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0975P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1548
_refine_ls_wR_factor_ref         0.2141
_reflns_Friedel_coverage         0.664
_reflns_Friedel_fraction_full    0.725
_reflns_Friedel_fraction_max     0.716
_reflns_number_gt                2790
_reflns_number_total             5868
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ce01387b2.cif
_cod_data_source_block           pol_calix4tube_4
_cod_depositor_comments
'Adding full bibliography for 7226356--7226359.cif.'
_cod_original_cell_volume        7387.9(5)
_cod_database_code               7226359
_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.
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z+1/2'
'y, -x, z+1/2'
'-x, -y, z'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+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
Na2 Na 1.0000 0.5000 0.5257(4) 0.067 Uani 1 2 d S T P
Na3 Na 1.0000 0.5000 0.7629(8) 0.174 Uani 1 2 d S T P
Na1 Na 0.96053(17) 0.34776(17) 0.5397(2) 0.047 Uani 1 1 d . . .
O5 O 1.0326(3) 0.4084(3) 0.4287(5) 0.078 Uani 1 1 d . . .
C2 C 1.0057(5) 0.1968(5) 0.3741(5) 0.045 Uani 1 1 d . . .
C1 C 1.0359(4) 0.2158(4) 0.4460(5) 0.043 Uani 1 1 d . . .
C6 C 1.0666(5) 0.1759(5) 0.4964(6) 0.050 Uani 1 1 d . . .
C7 C 1.0910(5) 0.1975(5) 0.5811(5) 0.051 Uani 1 1 d . . .
H7A H 1.1309 0.1765 0.5930 0.061 Uiso 1 1 calc R U .
H7B H 1.0983 0.2429 0.5810 0.061 Uiso 1 1 calc R U .
C3 C 1.0106(5) 0.1317(5) 0.3567(6) 0.056 Uani 1 1 d . . .
H3 H 0.9928 0.1159 0.3097 0.067 Uiso 1 1 calc R U .
O1 O 1.0354(3) 0.2815(3) 0.4615(3) 0.042 Uani 1 1 d . . .
C5 C 1.0690(5) 0.1127(5) 0.4768(6) 0.055 Uani 1 1 d . . .
H5 H 1.0898 0.0845 0.5108 0.066 Uiso 1 1 calc R U .
C30 C 1.0831(5) 0.3813(5) 0.4257(6) 0.058 Uani 1 1 d . . .
O6 O 1.1367(3) 0.4100(3) 0.4169(5) 0.072 Uani 1 1 d . . .
C4 C 1.0417(5) 0.0906(5) 0.4085(7) 0.062 Uani 1 1 d . . .
H4 H 1.0438 0.0476 0.3964 0.075 Uiso 1 1 calc R U .
C29 C 1.0905(5) 0.3118(5) 0.4290(8) 0.069 Uani 1 1 d . . .
H29A H 1.0983 0.2957 0.3753 0.083 Uiso 1 1 calc R U .
H29B H 1.1270 0.3014 0.4620 0.083 Uiso 1 1 calc R U .
O7 O 1.0462(4) 0.4045(3) 0.6009(4) 0.070 Uani 1 1 d . . .
C8 C 1.0433(5) 0.1811(5) 0.6438(5) 0.048 Uani 1 1 d . . .
C9 C 0.9974(5) 0.2245(4) 0.6720(5) 0.046 Uani 1 1 d . . .
O2 O 1.0044(3) 0.2880(3) 0.6466(3) 0.044 Uani 1 1 d . . .
C31 C 1.0441(5) 0.3223(4) 0.7016(5) 0.052 Uani 1 1 d . . .
H31A H 1.0811 0.2969 0.7148 0.062 Uiso 1 1 calc R U .
H31B H 1.0210 0.3304 0.7510 0.062 Uiso 1 1 calc R U .
C32 C 1.0651(5) 0.3844(5) 0.6654(7) 0.058 Uani 1 1 d . . .
C14 C 0.8934(5) 0.2527(5) 0.7398(5) 0.057 Uani 1 1 d . . .
H14A H 0.9067 0.2960 0.7299 0.069 Uiso 1 1 calc R U .
H14B H 0.8809 0.2491 0.7957 0.069 Uiso 1 1 calc R U .
C10 C 0.9477(5) 0.2076(5) 0.7224(5) 0.047 Uani 1 1 d . . .
C11 C 0.9482(6) 0.1454(5) 0.7511(6) 0.064 Uani 1 1 d . . .
H11 H 0.9167 0.1327 0.7868 0.076 Uiso 1 1 calc R U .
C12 C 0.9929(5) 0.1030(5) 0.7287(6) 0.059 Uani 1 1 d . . .
H12 H 0.9916 0.0619 0.7489 0.071 Uiso 1 1 calc R U .
C13 C 1.0404(5) 0.1201(5) 0.6764(6) 0.054 Uani 1 1 d . . .
H13 H 1.0713 0.0905 0.6625 0.065 Uiso 1 1 calc R U .
O8 O 1.1074(4) 0.4111(4) 0.7119(4) 0.082 Uani 1 1 d . . .
H8 H 1.1180 0.4452 0.6925 0.123 Uiso 1 1 calc R U .
C21 C 0.7698(5) 0.2883(5) 0.4788(6) 0.064 Uani 1 1 d . . .
H21A H 0.7248 0.2911 0.4671 0.076 Uiso 1 1 calc R U .
H21B H 0.7864 0.3312 0.4824 0.076 Uiso 1 1 calc R U .
C17 C 0.7796(5) 0.2538(5) 0.5612(6) 0.059 Uani 1 1 d . . .
C16 C 0.8239(5) 0.2718(4) 0.6164(6) 0.050 Uani 1 1 d . . .
C15 C 0.8379(5) 0.2360(5) 0.6857(6) 0.057 Uani 1 1 d . . .
O3 O 0.8575(3) 0.3282(3) 0.6047(3) 0.048 Uani 1 1 d . . .
C33 C 0.8223(5) 0.3833(5) 0.6314(6) 0.062 Uani 1 1 d . . .
H33A H 0.7942 0.3712 0.6750 0.074 Uiso 1 1 calc R U .
H33B H 0.7963 0.3989 0.5875 0.074 Uiso 1 1 calc R U .
C34 C 0.8661(5) 0.4361(5) 0.6600(6) 0.059 Uani 1 1 d . . .
O9 O 0.9229(4) 0.4233(4) 0.6729(6) 0.094 Uani 1 1 d . . .
O10 O 0.8399(3) 0.4886(3) 0.6679(5) 0.073 Uani 1 1 d . . .
C18 C 0.7453(5) 0.1989(6) 0.5783(7) 0.074 Uani 1 1 d . . .
H18 H 0.7141 0.1860 0.5423 0.089 Uiso 1 1 calc R U .
C20 C 0.8007(6) 0.1821(6) 0.7006(8) 0.080 Uani 1 1 d . . .
H20 H 0.8064 0.1587 0.7475 0.096 Uiso 1 1 calc R U .
C19 C 0.7550(6) 0.1640(6) 0.6439(11) 0.116 Uani 1 1 d . . .
H19 H 0.7312 0.1274 0.6522 0.139 Uiso 1 1 calc R U .
C25 C 0.8650(6) 0.1835(6) 0.2946(7) 0.077 Uani 1 1 d . . .
H25 H 0.8852 0.1596 0.2552 0.093 Uiso 1 1 calc R U .
O11 O 0.9078(3) 0.4388(3) 0.4893(4) 0.050 Uani 1 1 d . . .
C26 C 0.8036(7) 0.1727(7) 0.3113(9) 0.100 Uani 1 1 d . . .
H26 H 0.7815 0.1430 0.2809 0.120 Uiso 1 1 calc R U .
C24 C 0.8989(5) 0.2305(5) 0.3358(6) 0.053 Uani 1 1 d . . .
C28 C 0.9698(5) 0.2387(5) 0.3220(6) 0.052 Uani 1 1 d . . .
H28A H 0.9797 0.2293 0.2663 0.063 Uiso 1 1 calc R U .
H28B H 0.9817 0.2823 0.3326 0.063 Uiso 1 1 calc R U .
C23 C 0.8650(5) 0.2662(4) 0.3906(6) 0.050 Uani 1 1 d . . .
C22 C 0.8024(5) 0.2539(5) 0.4128(7) 0.065 Uani 1 1 d . . .
C36 C 0.8878(5) 0.4344(5) 0.4226(7) 0.060 Uani 1 1 d . . .
O12 O 0.8686(5) 0.4790(4) 0.3756(5) 0.106 Uani 1 1 d . . .
H12O H 0.8691 0.5129 0.3999 0.159 Uiso 1 1 calc R U .
O4 O 0.8944(3) 0.3192(3) 0.4282(4) 0.047 Uani 1 1 d . . .
C27 C 0.7722(6) 0.2040(6) 0.3720(7) 0.083 Uani 1 1 d . . .
H27 H 0.7311 0.1922 0.3860 0.100 Uiso 1 1 calc R U .
C35 C 0.8868(7) 0.3738(5) 0.3746(6) 0.073 Uani 1 1 d . . .
H35A H 0.8469 0.3703 0.3458 0.088 Uiso 1 1 calc R U .
H35B H 0.9209 0.3743 0.3354 0.088 Uiso 1 1 calc R U .
N1S N 0.8428(5) 0.0448(5) 0.5325(8) 0.096 Uani 1 1 d . . .
C1S C 0.8812(11) 0.0980(11) 0.504(2) 0.242 Uani 1 1 d . . .
H1S1 H 0.8670 0.1106 0.4516 0.363 Uiso 1 1 calc R U .
H1S2 H 0.8768 0.1331 0.5406 0.363 Uiso 1 1 calc R U .
H1S3 H 0.9249 0.0855 0.5015 0.363 Uiso 1 1 calc R U .
C3S C 0.8504(16) 0.0194(12) 0.5969(11) 0.276 Uani 1 1 d . . .
H3S H 0.8759 0.0455 0.6284 0.331 Uiso 1 1 calc R U .
O1S O 0.8393(7) -0.0200(8) 0.6299(8) 0.212 Uani 1 1 d . . .
C2S C 0.7940(11) 0.0287(13) 0.4804(12) 0.217 Uani 1 1 d . . .
H2S1 H 0.7966 0.0544 0.4328 0.326 Uiso 1 1 calc R U .
H2S2 H 0.7977 -0.0153 0.4659 0.326 Uiso 1 1 calc R U .
H2S3 H 0.7539 0.0357 0.5064 0.326 Uiso 1 1 calc R U .
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'
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'
Na Na 0.0362 0.0249 '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'
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
O11 Na2 O11 151.0(4) . 4_765
O11 Na2 O7 103.6(2) . 4_765
O11 Na2 O7 90.5(2) 4_765 4_765
O11 Na2 O7 90.5(2) . .
O11 Na2 O7 103.6(2) 4_765 .
O7 Na2 O7 121.5(4) 4_765 .
O11 Na2 O5 91.6(3) . 4_765
O11 Na2 O5 70.2(2) 4_765 4_765
O7 Na2 O5 67.7(2) 4_765 4_765
O7 Na2 O5 169.7(3) . 4_765
O11 Na2 O5 70.2(2) . .
O11 Na2 O5 91.6(3) 4_765 .
O7 Na2 O5 169.7(3) 4_765 .
O7 Na2 O5 67.7(2) . .
O5 Na2 O5 103.6(4) 4_765 .
O11 Na2 Na1 137.41(17) . 4_765
O11 Na2 Na1 45.49(16) 4_765 4_765
O7 Na2 Na1 45.77(17) 4_765 4_765
O7 Na2 Na1 129.0(2) . 4_765
O5 Na2 Na1 52.72(18) 4_765 4_765
O5 Na2 Na1 133.8(2) . 4_765
O11 Na2 Na1 45.49(16) . .
O11 Na2 Na1 137.41(17) 4_765 .
O7 Na2 Na1 129.0(2) 4_765 .
O7 Na2 Na1 45.77(17) . .
O5 Na2 Na1 133.8(2) 4_765 .
O5 Na2 Na1 52.72(18) . .
Na1 Na2 Na1 171.9(2) 4_765 .
O11 Na2 Na3 104.5(2) . .
O11 Na2 Na3 104.5(2) 4_765 .
O7 Na2 Na3 60.8(2) 4_765 .
O7 Na2 Na3 60.8(2) . .
O5 Na2 Na3 128.2(2) 4_765 .
O5 Na2 Na3 128.2(2) . .
Na1 Na2 Na3 85.97(12) 4_765 .
Na1 Na2 Na3 85.97(12) . .
O9 Na3 O9 113.7(6) 4_765 .
O9 Na3 Na2 56.9(3) 4_765 .
O9 Na3 Na2 56.9(3) . .
O2 Na1 O11 151.6(3) . .
O2 Na1 O7 69.6(2) . .
O11 Na1 O7 95.7(3) . .
O2 Na1 O4 132.4(2) . .
O11 Na1 O4 70.0(2) . .
O7 Na1 O4 153.3(3) . .
O2 Na1 O3 85.7(2) . .
O11 Na1 O3 82.9(2) . .
O7 Na1 O3 124.3(3) . .
O4 Na1 O3 77.6(2) . .
O2 Na1 O1 81.1(2) . .
O11 Na1 O1 124.7(2) . .
O7 Na1 O1 91.4(3) . .
O4 Na1 O1 79.7(2) . .
O3 Na1 O1 134.3(2) . .
O2 Na1 O5 122.9(3) . .
O11 Na1 O5 68.9(2) . .
O7 Na1 O5 68.4(3) . .
O4 Na1 O5 85.3(3) . .
O3 Na1 O5 150.8(3) . .
O1 Na1 O5 63.3(2) . .
O2 Na1 O9 79.7(3) . .
O11 Na1 O9 72.0(2) . .
O7 Na1 O9 66.4(3) . .
O4 Na1 O9 125.6(3) . .
O3 Na1 O9 60.3(2) . .
O1 Na1 O9 154.6(3) . .
O5 Na1 O9 115.1(3) . .
O2 Na1 C36 170.2(3) . .
O11 Na1 C36 20.4(2) . .
O7 Na1 C36 110.4(3) . .
O4 Na1 C36 51.0(3) . .
O3 Na1 C36 86.4(3) . .
O1 Na1 C36 108.6(3) . .
O5 Na1 C36 64.4(3) . .
O9 Na1 C36 91.3(3) . .
O2 Na1 Na2 118.0(2) . .
O11 Na1 Na2 46.44(17) . .
O7 Na1 Na2 50.1(2) . .
O4 Na1 Na2 109.5(2) . .
O3 Na1 Na2 114.42(19) . .
O1 Na1 Na2 110.4(2) . .
O5 Na1 Na2 50.0(2) . .
O9 Na1 Na2 65.4(2) . .
C36 Na1 Na2 60.5(2) . .
C30 O5 Na2 127.4(7) . .
C30 O5 Na1 107.4(7) . .
Na2 O5 Na1 77.3(2) . .
C3 C2 C1 114.7(9) . .
C3 C2 C28 120.7(9) . .
C1 C2 C28 124.6(9) . .
C6 C1 O1 120.2(8) . .
C6 C1 C2 124.3(9) . .
O1 C1 C2 115.5(8) . .
C1 C6 C5 118.3(9) . .
C1 C6 C7 122.3(9) . .
C5 C6 C7 118.9(9) . .
C8 C7 C6 109.9(8) . .
C8 C7 H7A 109.7 . .
C6 C7 H7A 109.7 . .
C8 C7 H7B 109.7 . .
C6 C7 H7B 109.7 . .
H7A C7 H7B 108.2 . .
C4 C3 C2 121.1(10) . .
C4 C3 H3 119.4 . .
C2 C3 H3 119.4 . .
C1 O1 C29 111.3(7) . .
C1 O1 Na1 130.9(5) . .
C29 O1 Na1 117.6(5) . .
C4 C5 C6 121.0(10) . .
C4 C5 H5 119.5 . .
C6 C5 H5 119.5 . .
O5 C30 O6 123.6(10) . .
O5 C30 C29 124.1(10) . .
O6 C30 C29 112.3(9) . .
C5 C4 C3 120.5(10) . .
C5 C4 H4 119.7 . .
C3 C4 H4 119.7 . .
O1 C29 C30 111.8(8) . .
O1 C29 H29A 109.2 . .
C30 C29 H29A 109.2 . .
O1 C29 H29B 109.3 . .
C30 C29 H29B 109.2 . .
H29A C29 H29B 107.9 . .
C32 O7 Na1 116.5(7) . .
C32 O7 Na2 145.8(7) . .
Na1 O7 Na2 84.1(2) . .
C13 C8 C9 115.9(9) . .
C13 C8 C7 120.9(9) . .
C9 C8 C7 123.1(9) . .
C10 C9 C8 123.5(8) . .
C10 C9 O2 120.2(8) . .
C8 C9 O2 116.3(8) . .
C9 O2 C31 110.3(6) . .
C9 O2 Na1 133.6(5) . .
C31 O2 Na1 116.0(5) . .
O2 C31 C32 110.7(8) . .
O2 C31 H31A 109.5 . .
C32 C31 H31A 109.5 . .
O2 C31 H31B 109.5 . .
C32 C31 H31B 109.5 . .
H31A C31 H31B 108.1 . .
O7 C32 O8 126.3(10) . .
O7 C32 C31 123.9(9) . .
O8 C32 C31 109.8(9) . .
C10 C14 C15 108.9(8) . .
C10 C14 H14A 109.9 . .
C15 C14 H14A 109.9 . .
C10 C14 H14B 109.9 . .
C15 C14 H14B 109.9 . .
H14A C14 H14B 108.3 . .
C9 C10 C11 116.3(9) . .
C9 C10 C14 121.6(9) . .
C11 C10 C14 121.9(9) . .
C12 C11 C10 122.1(10) . .
C12 C11 H11 118.9 . .
C10 C11 H11 118.9 . .
C11 C12 C13 120.6(10) . .
C11 C12 H12 119.7 . .
C13 C12 H12 119.7 . .
C12 C13 C8 121.2(10) . .
C12 C13 H13 119.4 . .
C8 C13 H13 119.4 . .
C32 O8 H8 109.5 . .
C22 C21 C17 111.0(9) . .
C22 C21 H21A 109.4 . .
C17 C21 H21A 109.4 . .
C22 C21 H21B 109.4 . .
C17 C21 H21B 109.4 . .
H21A C21 H21B 108.0 . .
C16 C17 C18 116.7(10) . .
C16 C17 C21 123.3(10) . .
C18 C17 C21 119.8(9) . .
C17 C16 O3 119.4(9) . .
C17 C16 C15 123.0(10) . .
O3 C16 C15 117.6(9) . .
C20 C15 C16 117.5(11) . .
C20 C15 C14 120.9(10) . .
C16 C15 C14 121.5(9) . .
C16 O3 C33 112.4(7) . .
C16 O3 Na1 130.6(5) . .
C33 O3 Na1 116.9(6) . .
O3 C33 C34 111.8(8) . .
O3 C33 H33A 109.3 . .
C34 C33 H33A 109.3 . .
O3 C33 H33B 109.3 . .
C34 C33 H33B 109.3 . .
H33A C33 H33B 107.9 . .
O10 C34 O9 126.9(10) . .
O10 C34 C33 114.5(10) . .
O9 C34 C33 118.6(10) . .
C34 O9 Na3 122.5(7) . .
C34 O9 Na1 104.8(7) . .
Na3 O9 Na1 126.2(4) . .
C19 C18 C17 123.1(12) . .
C19 C18 H18 118.4 . .
C17 C18 H18 118.4 . .
C19 C20 C15 119.1(12) . .
C19 C20 H20 120.5 . .
C15 C20 H20 120.5 . .
C18 C19 C20 120.4(12) . .
C18 C19 H19 119.8 . .
C20 C19 H19 119.8 . .
C26 C25 C24 120.7(12) . .
C26 C25 H25 119.7 . .
C24 C25 H25 119.7 . .
C36 O11 Na1 115.6(6) . .
C36 O11 Na2 124.1(7) . .
Na1 O11 Na2 88.1(2) . .
C25 C26 C27 122.3(12) . .
C25 C26 H26 118.9 . .
C27 C26 H26 118.9 . .
C23 C24 C25 116.4(11) . .
C23 C24 C28 123.1(9) . .
C25 C24 C28 120.5(10) . .
C2 C28 C24 110.7(8) . .
C2 C28 H28A 109.5 . .
C24 C28 H28A 109.5 . .
C2 C28 H28B 109.5 . .
C24 C28 H28B 109.5 . .
H28A C28 H28B 108.1 . .
C24 C23 C22 124.3(9) . .
C24 C23 O4 119.5(9) . .
C22 C23 O4 116.2(9) . .
C23 C22 C27 116.1(10) . .
C23 C22 C21 122.9(9) . .
C27 C22 C21 120.9(10) . .
O11 C36 O12 128.3(10) . .
O11 C36 C35 124.4(9) . .
O12 C36 C35 107.1(9) . .
O12 C36 Na1 166.7(8) . .
C35 C36 Na1 80.7(5) . .
C36 O12 H12O 109.5 . .
C23 O4 C35 107.6(7) . .
C23 O4 Na1 142.2(5) . .
C35 O4 Na1 109.7(5) . .
C26 C27 C22 119.7(12) . .
C26 C27 H27 120.2 . .
C22 C27 H27 120.2 . .
O4 C35 C36 110.0(8) . .
O4 C35 H35A 109.7 . .
C36 C35 H35A 109.7 . .
O4 C35 H35B 109.7 . .
C36 C35 H35B 109.7 . .
H35A C35 H35B 108.2 . .
C3S N1S C2S 123(2) . .
C3S N1S C1S 124(2) . .
C2S N1S C1S 113.4(17) . .
N1S C1S H1S1 109.5 . .
N1S C1S H1S2 109.5 . .
H1S1 C1S H1S2 109.5 . .
N1S C1S H1S3 109.5 . .
H1S1 C1S H1S3 109.5 . .
H1S2 C1S H1S3 109.5 . .
O1S C3S N1S 144(4) . .
O1S C3S H3S 108.2 . .
N1S C3S H3S 108.2 . .
N1S C2S H2S1 109.5 . .
N1S C2S H2S2 109.5 . .
H2S1 C2S H2S2 109.5 . .
N1S C2S H2S3 109.5 . .
H2S1 C2S H2S3 109.5 . .
H2S2 C2S H2S3 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Na2 O11 2.409(6) .
Na2 O11 2.410(6) 4_765
Na2 O7 2.562(8) 4_765
Na2 O7 2.562(8) .
Na2 O5 2.608(9) 4_765
Na2 O5 2.608(9) .
Na2 Na1 3.323(4) 4_765
Na2 Na1 3.323(4) .
Na2 Na3 3.946(15) .
Na3 O9 2.739(10) 4_765
Na3 O9 2.739(10) .
Na1 O2 2.366(6) .
Na1 O11 2.371(7) .
Na1 O7 2.394(8) .
Na1 O4 2.397(7) .
Na1 O3 2.461(7) .
Na1 O1 2.476(7) .
Na1 O5 2.710(9) .
Na1 O9 2.841(10) .
Na1 C36 3.079(10) .
O5 C30 1.210(11) .
C2 C3 1.406(12) .
C2 C1 1.414(13) .
C2 C28 1.450(14) .
C1 C6 1.352(13) .
C1 O1 1.408(10) .
C6 C5 1.374(13) .
C6 C7 1.566(13) .
C7 C8 1.489(13) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C3 C4 1.385(14) .
C3 H3 0.9300 .
O1 C29 1.431(11) .
C5 C4 1.355(14) .
C5 H5 0.9300 .
C30 O6 1.288(11) .
C30 C29 1.474(13) .
C4 H4 0.9300 .
C29 H29A 0.9700 .
C29 H29B 0.9700 .
O7 C32 1.221(12) .
C8 C13 1.397(12) .
C8 C9 1.411(13) .
C9 C10 1.388(13) .
C9 O2 1.412(10) .
O2 C31 1.437(10) .
C31 C32 1.507(13) .
C31 H31A 0.9700 .
C31 H31B 0.9700 .
C32 O8 1.306(12) .
C14 C10 1.516(14) .
C14 C15 1.517(15) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C10 C11 1.394(13) .
C11 C12 1.352(14) .
C11 H11 0.9300 .
C12 C13 1.374(14) .
C12 H12 0.9300 .
C13 H13 0.9300 .
O8 H8 0.8200 .
C21 C22 1.485(14) .
C21 C17 1.565(15) .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C17 C16 1.363(13) .
C17 C18 1.394(15) .
C16 O3 1.397(11) .
C16 C15 1.409(14) .
C15 C20 1.402(15) .
O3 C33 1.448(11) .
C33 C34 1.521(14) .
C33 H33A 0.9700 .
C33 H33B 0.9700 .
C34 O10 1.244(12) .
C34 O9 1.246(13) .
C18 C19 1.331(17) .
C18 H18 0.9300 .
C20 C19 1.401(19) .
C20 H20 0.9300 .
C19 H19 0.9300 .
C25 C26 1.343(17) .
C25 C24 1.401(14) .
C25 H25 0.9300 .
O11 C36 1.191(11) .
C26 C27 1.375(17) .
C26 H26 0.9300 .
C24 C23 1.380(13) .
C24 C28 1.521(14) .
C28 H28A 0.9700 .
C28 H28B 0.9700 .
C23 C22 1.395(14) .
C23 O4 1.422(11) .
C22 C27 1.404(15) .
C36 O12 1.288(11) .
C36 C35 1.507(15) .
O12 H12O 0.8200 .
O4 C35 1.465(11) .
C27 H27 0.9300 .
C35 H35A 0.9700 .
C35 H35B 0.9700 .
N1S C3S 1.209(19) .
N1S C2S 1.39(2) .
N1S C1S 1.46(2) .
C1S H1S1 0.9600 .
C1S H1S2 0.9600 .
C1S H1S3 0.9600 .
C3S O1S 1.02(3) .
C3S H3S 0.9300 .
C2S H2S1 0.9600 .
C2S H2S2 0.9600 .
C2S H2S3 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
C3 C2 C1 C6 -1.2(14)
C28 C2 C1 C6 176.4(9)
C3 C2 C1 O1 175.6(8)
C28 C2 C1 O1 -6.7(13)
O1 C1 C6 C5 -176.3(8)
C2 C1 C6 C5 0.4(15)
O1 C1 C6 C7 12.1(13)
C2 C1 C6 C7 -171.2(9)
C1 C6 C7 C8 95.3(11)
C5 C6 C7 C8 -76.2(11)
C1 C2 C3 C4 1.5(14)
C28 C2 C3 C4 -176.2(9)
C6 C1 O1 C29 85.8(10)
C2 C1 O1 C29 -91.2(10)
C6 C1 O1 Na1 -90.0(10)
C2 C1 O1 Na1 93.0(8)
C1 C6 C5 C4 0.2(15)
C7 C6 C5 C4 172.0(9)
Na2 O5 C30 O6 -54.6(14)
Na1 O5 C30 O6 -141.7(9)
Na2 O5 C30 C29 127.4(10)
Na1 O5 C30 C29 40.3(13)
C6 C5 C4 C3 0.2(16)
C2 C3 C4 C5 -1.1(16)
C1 O1 C29 C30 165.1(8)
Na1 O1 C29 C30 -18.4(12)
O5 C30 C29 O1 -18.7(16)
O6 C30 C29 O1 163.1(9)
C6 C7 C8 C13 82.3(11)
C6 C7 C8 C9 -95.5(11)
C13 C8 C9 C10 -6.7(14)
C7 C8 C9 C10 171.2(9)
C13 C8 C9 O2 173.0(8)
C7 C8 C9 O2 -9.1(13)
C10 C9 O2 C31 90.8(10)
C8 C9 O2 C31 -88.9(9)
C10 C9 O2 Na1 -85.3(10)
C8 C9 O2 Na1 95.0(10)
C9 O2 C31 C32 165.9(8)
Na1 O2 C31 C32 -17.2(10)
Na1 O7 C32 O8 -173.9(9)
Na2 O7 C32 O8 -51.9(19)
Na1 O7 C32 C31 8.7(13)
Na2 O7 C32 C31 130.7(10)
O2 C31 C32 O7 5.7(14)
O2 C31 C32 O8 -172.1(9)
C8 C9 C10 C11 6.0(14)
O2 C9 C10 C11 -173.7(8)
C8 C9 C10 C14 -169.4(8)
O2 C9 C10 C14 10.9(13)
C15 C14 C10 C9 98.1(11)
C15 C14 C10 C11 -77.0(11)
C9 C10 C11 C12 -2.7(15)
C14 C10 C11 C12 172.7(10)
C10 C11 C12 C13 0.4(17)
C11 C12 C13 C8 -1.2(16)
C9 C8 C13 C12 4.1(14)
C7 C8 C13 C12 -173.8(9)
C22 C21 C17 C16 98.8(11)
C22 C21 C17 C18 -76.3(12)
C18 C17 C16 O3 -176.6(8)
C21 C17 C16 O3 8.2(14)
C18 C17 C16 C15 3.4(14)
C21 C17 C16 C15 -171.9(9)
C17 C16 C15 C20 -5.0(15)
O3 C16 C15 C20 175.0(9)
C17 C16 C15 C14 171.6(9)
O3 C16 C15 C14 -8.4(13)
C10 C14 C15 C20 74.4(11)
C10 C14 C15 C16 -102.1(10)
C17 C16 O3 C33 82.3(10)
C15 C16 O3 C33 -97.7(10)
C17 C16 O3 Na1 -93.2(10)
C15 C16 O3 Na1 86.8(9)
C16 O3 C33 C34 150.1(8)
Na1 O3 C33 C34 -33.7(10)
O3 C33 C34 O10 165.9(8)
O3 C33 C34 O9 -14.1(14)
O10 C34 O9 Na3 17.7(16)
C33 C34 O9 Na3 -162.3(8)
O10 C34 O9 Na1 -135.5(10)
C33 C34 O9 Na1 44.5(11)
C16 C17 C18 C19 -1.3(17)
C21 C17 C18 C19 174.1(11)
C16 C15 C20 C19 4.4(16)
C14 C15 C20 C19 -172.2(11)
C17 C18 C19 C20 1(2)
C15 C20 C19 C18 -3(2)
C24 C25 C26 C27 -4(2)
C26 C25 C24 C23 -3.1(17)
C26 C25 C24 C28 174.5(12)
C3 C2 C28 C24 76.6(11)
C1 C2 C28 C24 -100.9(11)
C23 C24 C28 C2 91.1(12)
C25 C24 C28 C2 -86.4(12)
C25 C24 C23 C22 7.1(15)
C28 C24 C23 C22 -170.5(10)
C25 C24 C23 O4 -173.1(9)
C28 C24 C23 O4 9.4(14)
C24 C23 C22 C27 -4.0(16)
O4 C23 C22 C27 176.1(9)
C24 C23 C22 C21 172.6(10)
O4 C23 C22 C21 -7.3(15)
C17 C21 C22 C23 -89.9(13)
C17 C21 C22 C27 86.5(12)
Na1 O11 C36 O12 -165.4(10)
Na2 O11 C36 O12 -59.2(16)
Na1 O11 C36 C35 8.1(14)
Na2 O11 C36 C35 114.3(10)
Na2 O11 C36 Na1 106.2(8)
C24 C23 O4 C35 85.4(11)
C22 C23 O4 C35 -94.7(11)
C24 C23 O4 Na1 -85.5(12)
C22 C23 O4 Na1 94.4(11)
C25 C26 C27 C22 7(2)
C23 C22 C27 C26 -3.1(17)
C21 C22 C27 C26 -179.7(12)
C23 O4 C35 C36 153.5(9)
Na1 O4 C35 C36 -32.4(11)
O11 C36 C35 O4 17.8(16)
O12 C36 C35 O4 -167.5(10)
Na1 C36 C35 O4 23.5(8)
C2S N1S C3S O1S 19(5)
C1S N1S C3S O1S -165(4)
