# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_free_calix4tube_1
_database_code_depnum_ccdc_archive 'CCDC 1433706'
_audit_update_record             
;
2016-07-19 deposited with the CCDC.
2016-08-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C73 H67 Na3 O26'
_chemical_formula_weight         1429.24

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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'

_cell_length_a                   14.174(4)
_cell_length_b                   18.194(5)
_cell_length_c                   26.052(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6718(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    48173
_cell_measurement_theta_min      1.56
_cell_measurement_theta_max      26.60

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2984
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_process_details   
'Blessing, R. H. (1995) Acta Cryst., A51, 33-38'
_exptl_absorpt_correction_T_min  0.895
_exptl_absorpt_correction_T_max  0.993

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_reflns_number            48173
_diffrn_reflns_av_unetI/netI     0.1235
_diffrn_reflns_av_R_equivalents  0.1126
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.563
_diffrn_reflns_theta_max         26.600
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             13078
_reflns_number_gt                5959
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.786
_reflns_Friedel_fraction_max     0.905
_reflns_Friedel_fraction_full    0.998

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1021P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2016 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.3(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         13078
_refine_ls_number_parameters     909
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1782
_refine_ls_R_factor_gt           0.0677
_refine_ls_wR_factor_ref         0.2110
_refine_ls_wR_factor_gt          0.1638
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_restrained_S_all      0.984
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Na1 Na 0.6282(2) 0.49512(17) 0.93514(10) 0.0477(7) Uani 1 1 d . . . . .
Na3 Na 0.3146(2) 0.4996(2) 0.75920(10) 0.0579(8) Uani 1 1 d . . . . .
Na2 Na 0.4907(2) 0.4843(2) 0.83751(13) 0.0677(10) Uani 1 1 d . . . . .
C16A C 0.6492(6) 0.3918(5) 1.0504(3) 0.050(2) Uani 1 1 d . . . . .
C12A C 1.0097(7) 0.3668(6) 0.9961(4) 0.079(3) Uani 1 1 d . . . . .
H12A H 1.0676 0.3535 1.0100 0.095 Uiso 1 1 calc R U . . .
O1A O 0.7396(4) 0.5923(3) 0.91743(18) 0.0515(14) Uani 1 1 d . . . . .
O6A O 0.6799(5) 0.6192(4) 0.7869(2) 0.080(2) Uani 1 1 d . . . . .
H6O H 0.6524 0.5932 0.7660 0.120 Uiso 1 1 calc R U . . .
O5A O 0.6519(5) 0.5251(4) 0.8397(2) 0.0679(17) Uani 1 1 d . . . . .
C7A C 0.9152(6) 0.5130(5) 0.9067(3) 0.059(2) Uani 1 1 d . . . . .
H7A1 H 0.8622 0.5088 0.8833 0.071 Uiso 1 1 calc R U . . .
H7A2 H 0.9722 0.5176 0.8863 0.071 Uiso 1 1 calc R U . . .
C6A C 0.9030(6) 0.5821(5) 0.9400(3) 0.055(2) Uani 1 1 d . . . . .
C1A C 0.8159(6) 0.6160(5) 0.9469(3) 0.051(2) Uani 1 1 d . . . . .
C2A C 0.8015(6) 0.6732(5) 0.9819(3) 0.058(2) Uani 1 1 d . . . . .
C29A C 0.7335(7) 0.6311(5) 0.8695(3) 0.062(2) Uani 1 1 d . . . . .
H29A H 0.7965 0.6428 0.8574 0.075 Uiso 1 1 calc R U . . .
H29B H 0.6998 0.6770 0.8746 0.075 Uiso 1 1 calc R U . . .
C30A C 0.6837(6) 0.5863(6) 0.8300(3) 0.058(2) Uani 1 1 d . . . . .
C3A C 0.8810(8) 0.6973(6) 1.0078(4) 0.078(3) Uani 1 1 d . . . . .
H3A H 0.8748 0.7355 1.0312 0.093 Uiso 1 1 calc R U . . .
C4A C 0.9676(8) 0.6672(7) 1.0003(4) 0.089(4) Uani 1 1 d . . . . .
H4A H 1.0193 0.6857 1.0181 0.107 Uiso 1 1 calc R U . . .
C5A C 0.9797(7) 0.6097(6) 0.9666(4) 0.083(3) Uani 1 1 d . . . . .
H5A H 1.0393 0.5895 0.9617 0.099 Uiso 1 1 calc R U . . .
O2A O 0.7590(4) 0.4129(3) 0.92225(18) 0.0472(13) Uani 1 1 d . . . . .
O8A O 0.6443(6) 0.3189(5) 0.8216(3) 0.139(4) Uani 1 1 d . . . . .
O7A O 0.5878(5) 0.3902(4) 0.8815(2) 0.0755(19) Uani 1 1 d . . . . .
C10A C 0.8436(6) 0.3438(5) 0.9851(3) 0.056(2) Uani 1 1 d . . . . .
C32A C 0.6543(8) 0.3600(6) 0.8595(4) 0.078(3) Uani 1 1 d . . . . .
C14A C 0.7565(6) 0.3031(5) 1.0020(3) 0.055(2) Uani 1 1 d . . . . .
H14A H 0.7715 0.2520 1.0086 0.066 Uiso 1 1 calc R U . . .
H14B H 0.7088 0.3051 0.9754 0.066 Uiso 1 1 calc R U . . .
C9A C 0.8425(5) 0.4009(5) 0.9488(3) 0.049(2) Uani 1 1 d . . . . .
C8A C 0.9211(6) 0.4450(5) 0.9394(3) 0.055(2) Uani 1 1 d . . . . .
C13A C 1.0046(6) 0.4262(6) 0.9635(4) 0.069(3) Uani 1 1 d . . . . .
H13A H 1.0584 0.4542 0.9576 0.083 Uiso 1 1 calc R U . . .
C11A C 0.9310(7) 0.3271(5) 1.0082(4) 0.068(3) Uani 1 1 d . . . . .
H11A H 0.9351 0.2889 1.0319 0.081 Uiso 1 1 calc R U . . .
C31A C 0.7529(6) 0.3700(6) 0.8763(3) 0.066(3) Uani 1 1 d . . . . .
H31A H 0.7812 0.3222 0.8824 0.080 Uiso 1 1 calc R U . . .
H31B H 0.7884 0.3940 0.8493 0.080 Uiso 1 1 calc R U . . .
O10A O 0.3846(5) 0.3500(4) 0.9533(3) 0.081(2) Uani 1 1 d . . . . .
H10O H 0.3434 0.3727 0.9379 0.121 Uiso 1 1 calc R U . . .
C33A C 0.5271(6) 0.3575(5) 0.9957(4) 0.062(2) Uani 1 1 d . . . . .
H33A H 0.5007 0.3427 1.0284 0.074 Uiso 1 1 calc R U . . .
H33B H 0.5498 0.3137 0.9783 0.074 Uiso 1 1 calc R U . . .
O3A O 0.6034(3) 0.4065(3) 1.00404(19) 0.0471(13) Uani 1 1 d . . . . .
O9A O 0.4571(5) 0.4572(4) 0.9514(3) 0.086(2) Uani 1 1 d . . . . .
C34A C 0.4527(6) 0.3933(6) 0.9640(3) 0.059(2) Uani 1 1 d . . . . .
C21A C 0.5515(6) 0.4932(5) 1.0907(3) 0.055(2) Uani 1 1 d . . . . .
H21A H 0.5095 0.4902 1.1200 0.066 Uiso 1 1 calc R U . . .
H21B H 0.5140 0.4873 1.0598 0.066 Uiso 1 1 calc R U . . .
C15A C 0.7194(6) 0.3392(5) 1.0509(3) 0.049(2) Uani 1 1 d . . . . .
C17A C 0.6233(6) 0.4317(5) 1.0937(3) 0.055(2) Uani 1 1 d . . . . .
C18A C 0.6679(7) 0.4143(5) 1.1390(3) 0.068(3) Uani 1 1 d . . . . .
H18A H 0.6524 0.4396 1.1688 0.082 Uiso 1 1 calc R U . . .
C19A C 0.7349(7) 0.3599(6) 1.1407(3) 0.072(3) Uani 1 1 d . . . . .
H19A H 0.7638 0.3487 1.1718 0.086 Uiso 1 1 calc R U . . .
C20A C 0.7599(7) 0.3222(5) 1.0977(4) 0.072(3) Uani 1 1 d . . . . .
H20A H 0.8045 0.2848 1.0999 0.087 Uiso 1 1 calc R U . . .
O4A O 0.5774(4) 0.5819(3) 0.99917(18) 0.0486(13) Uani 1 1 d . . . . .
O11A O 0.5093(5) 0.5896(4) 0.9029(2) 0.0734(19) Uani 1 1 d . . . . .
O12A O 0.3674(5) 0.6238(4) 0.9324(2) 0.081(2) Uani 1 1 d . . . . .
H12' H 0.3520 0.6215 0.9021 0.121 Uiso 1 1 calc R U . . .
C24A C 0.6702(7) 0.6702(5) 1.0439(3) 0.062(2) Uani 1 1 d . . . . .
C22A C 0.5987(6) 0.5687(5) 1.0899(3) 0.056(2) Uani 1 1 d . . . . .
C23A C 0.6165(6) 0.6053(5) 1.0455(3) 0.051(2) Uani 1 1 d . . . . .
C35A C 0.4855(6) 0.6102(5) 0.9924(3) 0.057(2) Uani 1 1 d . . . . .
H35A H 0.4836 0.6610 1.0038 0.068 Uiso 1 1 calc R U . . .
H35B H 0.4413 0.5823 1.0131 0.068 Uiso 1 1 calc R U . . .
C36A C 0.4574(6) 0.6060(5) 0.9371(4) 0.059(2) Uani 1 1 d . . . . .
C28A C 0.7050(7) 0.7033(5) 0.9937(3) 0.061(2) Uani 1 1 d . . . . .
H28A H 0.6617 0.6911 0.9661 0.074 Uiso 1 1 calc R U . . .
H28B H 0.7079 0.7564 0.9966 0.074 Uiso 1 1 calc R U . . .
C25A C 0.6997(8) 0.6982(6) 1.0901(3) 0.076(3) Uani 1 1 d . . . . .
H25A H 0.7359 0.7408 1.0907 0.092 Uiso 1 1 calc R U . . .
C26A C 0.6768(9) 0.6647(7) 1.1351(4) 0.088(3) Uani 1 1 d . . . . .
H26A H 0.6941 0.6862 1.1661 0.105 Uiso 1 1 calc R U . . .
C27A C 0.6284(8) 0.5995(6) 1.1353(4) 0.077(3) Uani 1 1 d . . . . .
H27A H 0.6156 0.5760 1.1662 0.093 Uiso 1 1 calc R U . . .
O5B O 0.4608(4) 0.5578(4) 0.7581(2) 0.0685(17) Uani 1 1 d . . . . .
O6B O 0.5980(5) 0.5558(5) 0.7168(2) 0.106(3) Uani 1 1 d . . . . .
O1B O 0.3664(4) 0.5110(4) 0.67370(19) 0.0625(16) Uani 1 1 d . . . . .
C2B C 0.3137(6) 0.4368(5) 0.6027(3) 0.055(2) Uani 1 1 d . . . . .
C1B C 0.3251(6) 0.5074(6) 0.6246(3) 0.054(2) Uani 1 1 d . . . . .
C6B C 0.2971(6) 0.5703(5) 0.6012(3) 0.056(2) Uani 1 1 d . . . . .
C7B C 0.2982(7) 0.6438(5) 0.6290(3) 0.069(3) Uani 1 1 d . . . . .
H7B1 H 0.3458 0.6430 0.6557 0.082 Uiso 1 1 calc R U . . .
H7B2 H 0.3141 0.6826 0.6050 0.082 Uiso 1 1 calc R U . . .
C30B C 0.5082(8) 0.5471(6) 0.7206(4) 0.071(3) Uani 1 1 d . . . . .
C29B C 0.4653(6) 0.5216(6) 0.6702(3) 0.074(3) Uani 1 1 d . . . . .
H29C H 0.4784 0.5579 0.6439 0.088 Uiso 1 1 calc R U . . .
H29D H 0.4949 0.4758 0.6599 0.088 Uiso 1 1 calc R U . . .
C5B C 0.2653(6) 0.5661(6) 0.5516(3) 0.063(2) Uani 1 1 d . . . . .
H5B H 0.2488 0.6090 0.5343 0.076 Uiso 1 1 calc R U . . .
C4B C 0.2572(7) 0.4986(7) 0.5266(3) 0.073(3) Uani 1 1 d . . . . .
H4B H 0.2364 0.4968 0.4928 0.087 Uiso 1 1 calc R U . . .
C3B C 0.2801(7) 0.4344(6) 0.5522(3) 0.069(3) Uani 1 1 d . . . . .
H3B H 0.2730 0.3893 0.5357 0.083 Uiso 1 1 calc R U . . .
O2B O 0.2567(4) 0.6254(3) 0.7369(2) 0.0545(15) Uani 1 1 d . . . . .
O7B O 0.3119(5) 0.6249(4) 0.8348(2) 0.0777(19) Uani 1 1 d . . . . .
O8B O 0.3832(7) 0.7290(5) 0.8311(3) 0.133(4) Uani 1 1 d . . . . .
H8B H 0.3939 0.7609 0.8096 0.200 Uiso 1 1 calc R U . . .
C8B C 0.2038(7) 0.6590(5) 0.6523(3) 0.058(2) Uani 1 1 d . . . . .
C9B C 0.1823(6) 0.6465(4) 0.7042(3) 0.049(2) Uani 1 1 d . . . . .
C31B C 0.3102(7) 0.6869(5) 0.7552(3) 0.072(3) Uani 1 1 d . . . . .
H31C H 0.2739 0.7316 0.7509 0.086 Uiso 1 1 calc R U . . .
H31D H 0.3677 0.6916 0.7352 0.086 Uiso 1 1 calc R U . . .
C32B C 0.3343(8) 0.6767(6) 0.8104(4) 0.077(3) Uani 1 1 d . . . . .
C14B C 0.0702(7) 0.6290(5) 0.7778(3) 0.067(3) Uani 1 1 d . . . . .
H14C H 0.0289 0.6654 0.7930 0.080 Uiso 1 1 calc R U . . .
H14D H 0.1273 0.6266 0.7982 0.080 Uiso 1 1 calc R U . . .
C10B C 0.0948(7) 0.6519(5) 0.7239(3) 0.057(2) Uani 1 1 d . . . . .
C13B C 0.1294(7) 0.6848(5) 0.6223(3) 0.062(3) Uani 1 1 d . . . . .
H13B H 0.1403 0.6959 0.5880 0.074 Uiso 1 1 calc R U . . .
C12B C 0.0396(8) 0.6943(5) 0.6422(4) 0.068(3) Uani 1 1 d . . . . .
H12B H -0.0079 0.7136 0.6216 0.082 Uiso 1 1 calc R U . . .
C11B C 0.0204(7) 0.6758(5) 0.6917(4) 0.065(3) Uani 1 1 d . . . . .
H11B H -0.0409 0.6787 0.7042 0.077 Uiso 1 1 calc R U . . .
O3B O 0.1650(4) 0.4935(3) 0.79902(17) 0.0529(14) Uani 1 1 d . . . . .
O9B O 0.3339(4) 0.4535(4) 0.8428(2) 0.0711(18) Uani 1 1 d . . . . .
O10B O 0.2532(5) 0.4137(5) 0.9121(2) 0.090(2) Uani 1 1 d . . . . .
C15B C 0.0217(6) 0.5545(5) 0.7781(3) 0.053(2) Uani 1 1 d . . . . .
C21B C 0.0910(7) 0.3522(5) 0.7780(4) 0.070(3) Uani 1 1 d . . . . .
H21C H 0.1463 0.3599 0.7994 0.083 Uiso 1 1 calc R U . . .
H21D H 0.0554 0.3117 0.7924 0.083 Uiso 1 1 calc R U . . .
C17B C 0.0315(6) 0.4200(5) 0.7786(3) 0.056(2) Uani 1 1 d . . . . .
C16B C 0.0710(6) 0.4884(5) 0.7842(3) 0.052(2) Uani 1 1 d . . . . .
C33B C 0.1712(6) 0.4870(5) 0.8547(3) 0.064(2) Uani 1 1 d . . . . .
H33C H 0.1177 0.4593 0.8675 0.076 Uiso 1 1 calc R U . . .
H33D H 0.1697 0.5354 0.8701 0.076 Uiso 1 1 calc R U . . .
C34B C 0.2615(7) 0.4485(6) 0.8690(3) 0.066(3) Uani 1 1 d . . . . .
C20B C -0.0760(7) 0.5486(7) 0.7693(3) 0.071(3) Uani 1 1 d . . . . .
H20B H -0.1120 0.5909 0.7652 0.086 Uiso 1 1 calc R U . . .
C19B C -0.1187(7) 0.4808(7) 0.7667(3) 0.075(3) Uani 1 1 d . . . . .
H19B H -0.1837 0.4774 0.7623 0.090 Uiso 1 1 calc R U . . .
C18B C -0.0650(7) 0.4176(6) 0.7705(3) 0.070(3) Uani 1 1 d . . . . .
H18B H -0.0945 0.3722 0.7676 0.084 Uiso 1 1 calc R U . . .
O4B O 0.2824(4) 0.3707(3) 0.7386(2) 0.0605(16) Uani 1 1 d . . . . .
O11B O 0.4619(5) 0.3982(5) 0.7637(3) 0.0765(19) Uani 1 1 d . . . . .
O12B O 0.4769(7) 0.2847(5) 0.7978(4) 0.149(5) Uani 1 1 d . . . . .
H12O H 0.5285 0.3007 0.8067 0.223 Uiso 1 1 calc R U . . .
C36B C 0.4299(8) 0.3361(7) 0.7742(5) 0.084(3) Uani 1 1 d . . . . .
C35B C 0.3340(8) 0.3108(5) 0.7610(4) 0.087(3) Uani 1 1 d . . . . .
H35C H 0.3376 0.2703 0.7369 0.105 Uiso 1 1 calc R U . . .
H35D H 0.3019 0.2937 0.7916 0.105 Uiso 1 1 calc R U . . .
C23B C 0.2119(6) 0.3472(5) 0.7058(4) 0.055(2) Uani 1 1 d . . . . .
C24B C 0.2345(7) 0.3395(5) 0.6536(4) 0.061(2) Uani 1 1 d . . . . .
C28B C 0.3275(6) 0.3664(5) 0.6318(4) 0.065(3) Uani 1 1 d . . . . .
H28C H 0.3720 0.3743 0.6596 0.077 Uiso 1 1 calc R U . . .
H28D H 0.3535 0.3293 0.6092 0.077 Uiso 1 1 calc R U . . .
C22B C 0.1218(7) 0.3328(5) 0.7248(4) 0.062(2) Uani 1 1 d . . . . .
C27B C 0.0553(7) 0.3061(5) 0.6901(4) 0.068(3) Uani 1 1 d . . . . .
H27B H -0.0056 0.2961 0.7015 0.081 Uiso 1 1 calc R U . . .
C26B C 0.0780(8) 0.2940(5) 0.6393(4) 0.076(3) Uani 1 1 d . . . . .
H26B H 0.0337 0.2733 0.6174 0.091 Uiso 1 1 calc R U . . .
C25B C 0.1653(8) 0.3124(5) 0.6210(4) 0.070(3) Uani 1 1 d . . . . .
H25B H 0.1785 0.3066 0.5863 0.084 Uiso 1 1 calc R U . . .
O1S O 0.6649(17) 0.4683(12) 0.6379(8) 0.324(11) Uiso 1 1 d D . . . .
H1OS H 0.6309 0.5076 0.6568 0.487 Uiso 1 1 d R U . . .
C1S C 0.653(2) 0.4792(16) 0.5860(9) 0.294(15) Uiso 1 1 d D . . . .
H1SA H 0.6808 0.5326 0.5746 0.441 Uiso 1 1 d R U . . .
H1SB H 0.5800 0.4765 0.5769 0.441 Uiso 1 1 d R U . . .
H1SC H 0.6904 0.4361 0.5652 0.441 Uiso 1 1 d R U . . .
O1W O 0.6405(10) 0.3574(6) 0.7133(5) 0.217(7) Uani 1 1 d . . . . .
H1W H 0.6555 0.3669 0.6824 0.326 Uiso 1 1 d R U . . .
H2W H 0.5859 0.3751 0.7186 0.326 Uiso 1 1 d R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Na1 O4A 2.408(6) . ?
Na1 O2A 2.405(6) . ?
Na1 O1A 2.415(6) . ?
Na1 O7A 2.434(7) . ?
Na1 O3A 2.439(6) . ?
Na1 O11A 2.550(7) . ?
Na1 O9A 2.558(8) . ?
Na1 O5A 2.568(7) . ?
Na1 Na2 3.210(4) . ?
Na3 O5B 2.328(7) . ?
Na3 O9B 2.350(6) . ?
Na3 O1B 2.355(6) . ?
Na3 O3B 2.363(6) . ?
Na3 O4B 2.449(7) . ?
Na3 O2B 2.500(6) . ?
Na3 O11B 2.788(8) . ?
Na3 O7B 3.013(8) . ?
Na3 C30B 3.048(12) . ?
Na3 C34B 3.101(10) . ?
Na3 Na2 3.236(4) . ?
Na2 O9B 2.296(7) . ?
Na2 O5A 2.403(8) . ?
Na2 O7A 2.477(8) . ?
Na2 O5B 2.500(7) . ?
Na2 O11B 2.514(8) . ?
Na2 O11A 2.577(7) . ?
C16A C15A 1.382(11) . ?
C16A C17A 1.389(11) . ?
C16A O3A 1.398(9) . ?
C12A C11A 1.366(13) . ?
C12A C13A 1.376(13) . ?
C12A H12A 0.9300 . ?
O1A C1A 1.394(9) . ?
O1A C29A 1.438(9) . ?
O6A C30A 1.273(10) . ?
O6A H6O 0.8200 . ?
O5A C30A 1.227(10) . ?
C7A C8A 1.505(12) . ?
C7A C6A 1.537(12) . ?
C7A H7A1 0.9700 . ?
C7A H7A2 0.9700 . ?
C6A C5A 1.384(13) . ?
C6A C1A 1.391(12) . ?
C1A C2A 1.399(13) . ?
C2A C3A 1.383(13) . ?
C2A C28A 1.506(13) . ?
C29A C30A 1.490(12) . ?
C29A H29A 0.9700 . ?
C29A H29B 0.9700 . ?
C3A C4A 1.359(15) . ?
C3A H3A 0.9300 . ?
C4A C5A 1.377(15) . ?
C4A H4A 0.9300 . ?
C5A H5A 0.9300 . ?
O2A C9A 1.388(9) . ?
O2A C31A 1.431(10) . ?
O8A C32A 1.247(11) . ?
O7A C32A 1.233(11) . ?
C10A C9A 1.406(12) . ?
C10A C11A 1.411(12) . ?
C10A C14A 1.506(12) . ?
C32A C31A 1.476(14) . ?
C14A C15A 1.526(11) . ?
C14A H14A 0.9700 . ?
C14A H14B 0.9700 . ?
C9A C8A 1.396(12) . ?
C8A C13A 1.383(12) . ?
C13A H13A 0.9300 . ?
C11A H11A 0.9300 . ?
C31A H31A 0.9700 . ?
C31A H31B 0.9700 . ?
O10A C34A 1.277(10) . ?
O10A H10O 0.8200 . ?
C33A O3A 1.418(10) . ?
C33A C34A 1.491(12) . ?
C33A H33A 0.9700 . ?
C33A H33B 0.9700 . ?
O9A C34A 1.209(11) . ?
C21A C17A 1.514(12) . ?
C21A C22A 1.527(13) . ?
C21A H21A 0.9700 . ?
C21A H21B 0.9700 . ?
C15A C20A 1.384(11) . ?
C17A C18A 1.376(12) . ?
C18A C19A 1.372(13) . ?
C18A H18A 0.9300 . ?
C19A C20A 1.360(13) . ?
C19A H19A 0.9300 . ?
C20A H20A 0.9300 . ?
O4A C23A 1.395(9) . ?
O4A C35A 1.411(9) . ?
O11A C36A 1.193(10) . ?
O12A C36A 1.322(10) . ?
O12A H12' 0.8200 . ?
C24A C25A 1.374(12) . ?
C24A C23A 1.406(12) . ?
C24A C28A 1.522(12) . ?
C22A C23A 1.358(11) . ?
C22A C27A 1.374(12) . ?
C35A C36A 1.498(12) . ?
C35A H35A 0.9700 . ?
C35A H35B 0.9700 . ?
C28A H28A 0.9700 . ?
C28A H28B 0.9700 . ?
C25A C26A 1.361(14) . ?
C25A H25A 0.9300 . ?
C26A C27A 1.370(14) . ?
C26A H26A 0.9300 . ?
C27A H27A 0.9300 . ?
O5B C30B 1.201(11) . ?
O6B C30B 1.286(12) . ?
O1B C1B 1.409(9) . ?
O1B C29B 1.418(10) . ?
C2B C3B 1.400(12) . ?
C2B C1B 1.414(12) . ?
C2B C28B 1.502(13) . ?
C1B C6B 1.357(12) . ?
C6B C5B 1.371(12) . ?
C6B C7B 1.520(13) . ?
C7B C8B 1.494(13) . ?
C7B H7B1 0.9700 . ?
C7B H7B2 0.9700 . ?
C30B C29B 1.519(13) . ?
C29B H29C 0.9700 . ?
C29B H29D 0.9700 . ?
C5B C4B 1.394(14) . ?
C5B H5B 0.9300 . ?
C4B C3B 1.384(14) . ?
C4B H4B 0.9300 . ?
C3B H3B 0.9300 . ?
O2B C9B 1.410(9) . ?
O2B C31B 1.433(10) . ?
O7B C32B 1.181(11) . ?
O8B C32B 1.295(12) . ?
O8B H8B 0.8200 . ?
C8B C13B 1.393(12) . ?
C8B C9B 1.405(12) . ?
C9B C10B 1.346(12) . ?
C31B C32B 1.491(13) . ?
C31B H31C 0.9700 . ?
C31B H31D 0.9700 . ?
C14B C10B 1.503(12) . ?
C14B C15B 1.521(13) . ?
C14B H14C 0.9700 . ?
C14B H14D 0.9700 . ?
C10B C11B 1.416(12) . ?
C13B C12B 1.386(13) . ?
C13B H13B 0.9300 . ?
C12B C11B 1.359(13) . ?
C12B H12B 0.9300 . ?
C11B H11B 0.9300 . ?
O3B C16B 1.391(9) . ?
O3B C33B 1.457(9) . ?
O9B C34B 1.235(11) . ?
O10B C34B 1.295(11) . ?
C15B C16B 1.400(12) . ?
C15B C20B 1.408(13) . ?
C21B C22B 1.496(13) . ?
C21B C17B 1.495(13) . ?
C21B H21C 0.9700 . ?
C21B H21D 0.9700 . ?
C17B C16B 1.371(12) . ?
C17B C18B 1.385(13) . ?
C33B C34B 1.506(13) . ?
C33B H33C 0.9700 . ?
C33B H33D 0.9700 . ?
C20B C19B 1.376(15) . ?
C20B H20B 0.9300 . ?
C19B C18B 1.382(14) . ?
C19B H19B 0.9300 . ?
C18B H18B 0.9300 . ?
O4B C23B 1.382(10) . ?
O4B C35B 1.436(11) . ?
O11B C36B 1.248(14) . ?
O12B C36B 1.303(13) . ?
O12B H12O 0.8200 . ?
C36B C35B 1.476(15) . ?
C35B H35C 0.9700 . ?
C35B H35D 0.9700 . ?
C23B C22B 1.396(13) . ?
C23B C24B 1.402(13) . ?
C24B C25B 1.388(13) . ?
C24B C28B 1.517(13) . ?
C28B H28C 0.9700 . ?
C28B H28D 0.9700 . ?
C22B C27B 1.392(12) . ?
C27B C26B 1.379(14) . ?
C27B H27B 0.9300 . ?
C26B C25B 1.367(14) . ?
C26B H26B 0.9300 . ?
C25B H25B 0.9300 . ?
O1S C1S 1.377(13) . ?
O1S H1OS 0.9931 . ?
C1S H1SA 1.0889 . ?
C1S H1SB 1.0642 . ?
C1S H1SC 1.0886 . ?
O1W H1W 0.8500 . ?
O1W H2W 0.8499 . ?

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
_geom_angle_publ_flag
O4A Na1 O2A 137.3(2) . . ?
O4A Na1 O1A 81.2(2) . . ?
O2A Na1 O1A 85.7(2) . . ?
O4A Na1 O7A 147.3(3) . . ?
O2A Na1 O7A 67.3(2) . . ?
O1A Na1 O7A 128.2(2) . . ?
O4A Na1 O3A 83.14(19) . . ?
O2A Na1 O3A 78.62(19) . . ?
O1A Na1 O3A 136.0(2) . . ?
O7A Na1 O3A 82.6(2) . . ?
O4A Na1 O11A 65.7(2) . . ?
O2A Na1 O11A 152.0(2) . . ?
O1A Na1 O11A 82.8(2) . . ?
O7A Na1 O11A 100.6(2) . . ?
O3A Na1 O11A 126.4(2) . . ?
O4A Na1 O9A 77.2(2) . . ?
O2A Na1 O9A 125.9(2) . . ?
O1A Na1 O9A 148.1(2) . . ?
O7A Na1 O9A 70.1(3) . . ?
O3A Na1 O9A 64.1(2) . . ?
O11A Na1 O9A 67.0(2) . . ?
O4A Na1 O5A 124.8(2) . . ?
O2A Na1 O5A 84.0(2) . . ?
O1A Na1 O5A 64.8(2) . . ?
O7A Na1 O5A 69.0(2) . . ?
O3A Na1 O5A 150.7(2) . . ?
O11A Na1 O5A 67.9(2) . . ?
O9A Na1 O5A 110.0(2) . . ?
O4A Na1 Na2 114.03(18) . . ?
O2A Na1 Na2 108.61(16) . . ?
O1A Na1 Na2 106.88(16) . . ?
O7A Na1 Na2 49.76(18) . . ?
O3A Na1 Na2 117.07(17) . . ?
O11A Na1 Na2 51.60(17) . . ?
O9A Na1 Na2 62.52(19) . . ?
O5A Na1 Na2 47.57(17) . . ?
O5B Na3 O9B 94.0(2) . . ?
O5B Na3 O1B 70.7(2) . . ?
O9B Na3 O1B 150.7(3) . . ?
O5B Na3 O3B 145.7(3) . . ?
O9B Na3 O3B 71.4(2) . . ?
O1B Na3 O3B 134.4(2) . . ?
O5B Na3 O4B 126.8(3) . . ?
O9B Na3 O4B 83.3(2) . . ?
O1B Na3 O4B 86.3(2) . . ?
O3B Na3 O4B 83.4(2) . . ?
O5B Na3 O2B 82.7(2) . . ?
O9B Na3 O2B 125.4(3) . . ?
O1B Na3 O2B 78.6(2) . . ?
O3B Na3 O2B 81.4(2) . . ?
O4B Na3 O2B 139.9(2) . . ?
O5B Na3 O11B 68.6(2) . . ?
O9B Na3 O11B 68.8(2) . . ?
O1B Na3 O11B 82.2(2) . . ?
O3B Na3 O11B 128.5(2) . . ?
O4B Na3 O11B 61.0(2) . . ?
O2B Na3 O11B 149.4(3) . . ?
O5B Na3 O7B 71.1(2) . . ?
O9B Na3 O7B 70.4(2) . . ?
O1B Na3 O7B 123.8(2) . . ?
O3B Na3 O7B 74.8(2) . . ?
O4B Na3 O7B 150.0(2) . . ?
O2B Na3 O7B 56.97(19) . . ?
O11B Na3 O7B 118.8(2) . . ?
O5B Na3 C30B 20.8(2) . . ?
O9B Na3 C30B 107.6(3) . . ?
O1B Na3 C30B 51.8(2) . . ?
O3B Na3 C30B 165.0(3) . . ?
O4B Na3 C30B 111.5(3) . . ?
O2B Na3 C30B 87.7(3) . . ?
O11B Na3 C30B 61.8(3) . . ?
O7B Na3 C30B 90.7(3) . . ?
O5B Na3 C34B 111.3(2) . . ?
O9B Na3 C34B 20.9(2) . . ?
O1B Na3 C34B 167.1(3) . . ?
O3B Na3 C34B 50.5(2) . . ?
O4B Na3 C34B 82.5(3) . . ?
O2B Na3 C34B 114.1(3) . . ?
O11B Na3 C34B 86.8(3) . . ?
O7B Na3 C34B 67.7(2) . . ?
C30B Na3 C34B 127.4(3) . . ?
O5B Na3 Na2 50.22(18) . . ?
O9B Na3 Na2 45.18(18) . . ?
O1B Na3 Na2 111.29(18) . . ?
O3B Na3 Na2 114.29(16) . . ?
O4B Na3 Na2 101.53(18) . . ?
O2B Na3 Na2 118.56(18) . . ?
O11B Na3 Na2 48.64(17) . . ?
O7B Na3 Na2 70.26(15) . . ?
C30B Na3 Na2 62.5(2) . . ?
C34B Na3 Na2 65.1(2) . . ?
O9B Na2 O5A 173.9(3) . . ?
O9B Na2 O7A 110.0(3) . . ?
O5A Na2 O7A 71.0(2) . . ?
O9B Na2 O5B 90.9(2) . . ?
O5A Na2 O5B 90.9(2) . . ?
O7A Na2 O5B 147.8(3) . . ?
O9B Na2 O11B 74.7(2) . . ?
O5A Na2 O11B 111.4(2) . . ?
O7A Na2 O11B 90.8(3) . . ?
O5B Na2 O11B 70.9(3) . . ?
O9B Na2 O11A 103.9(3) . . ?
O5A Na2 O11A 70.0(2) . . ?
O7A Na2 O11A 98.7(2) . . ?
O5B Na2 O11A 99.6(2) . . ?
O11B Na2 O11A 170.2(3) . . ?
O9B Na2 Na1 123.7(2) . . ?
O5A Na2 Na1 52.06(16) . . ?
O7A Na2 Na1 48.60(17) . . ?
O5B Na2 Na1 136.6(2) . . ?
O11B Na2 Na1 138.0(2) . . ?
O11A Na2 Na1 50.86(16) . . ?
O9B Na2 Na3 46.54(17) . . ?
O5A Na2 Na3 136.2(2) . . ?
O7A Na2 Na3 141.2(2) . . ?
O5B Na2 Na3 45.69(16) . . ?
O11B Na2 Na3 56.34(18) . . ?
O11A Na2 Na3 115.58(19) . . ?
Na1 Na2 Na3 164.28(15) . . ?
C15A C16A C17A 123.1(7) . . ?
C15A C16A O3A 118.3(7) . . ?
C17A C16A O3A 118.6(8) . . ?
C11A C12A C13A 121.1(9) . . ?
C11A C12A H12A 119.5 . . ?
C13A C12A H12A 119.5 . . ?
C1A O1A C29A 112.0(6) . . ?
C1A O1A Na1 128.9(4) . . ?
C29A O1A Na1 119.1(5) . . ?
C30A O6A H6O 109.5 . . ?
C30A O5A Na2 128.6(6) . . ?
C30A O5A Na1 116.1(6) . . ?
Na2 O5A Na1 80.4(2) . . ?
C8A C7A C6A 111.1(7) . . ?
C8A C7A H7A1 109.4 . . ?
C6A C7A H7A1 109.4 . . ?
C8A C7A H7A2 109.4 . . ?
C6A C7A H7A2 109.4 . . ?
H7A1 C7A H7A2 108.0 . . ?
C5A C6A C1A 118.2(9) . . ?
C5A C6A C7A 119.4(9) . . ?
C1A C6A C7A 122.3(8) . . ?
C6A C1A O1A 118.7(8) . . ?
C6A C1A C2A 122.8(8) . . ?
O1A C1A C2A 118.4(8) . . ?
C3A C2A C1A 115.8(9) . . ?
C3A C2A C28A 121.7(9) . . ?
C1A C2A C28A 122.4(8) . . ?
O1A C29A C30A 111.1(7) . . ?
O1A C29A H29A 109.4 . . ?
C30A C29A H29A 109.4 . . ?
O1A C29A H29B 109.4 . . ?
C30A C29A H29B 109.4 . . ?
H29A C29A H29B 108.0 . . ?
O5A C30A O6A 126.3(8) . . ?
O5A C30A C29A 121.9(8) . . ?
O6A C30A C29A 111.8(8) . . ?
C4A C3A C2A 122.6(11) . . ?
C4A C3A H3A 118.7 . . ?
C2A C3A H3A 118.7 . . ?
C3A C4A C5A 120.7(10) . . ?
C3A C4A H4A 119.7 . . ?
C5A C4A H4A 119.7 . . ?
C4A C5A C6A 119.8(10) . . ?
C4A C5A H5A 120.1 . . ?
C6A C5A H5A 120.1 . . ?
C9A O2A C31A 112.4(6) . . ?
C9A O2A Na1 133.3(5) . . ?
C31A O2A Na1 114.2(5) . . ?
C32A O7A Na1 115.9(7) . . ?
C32A O7A Na2 121.3(6) . . ?
Na1 O7A Na2 81.6(2) . . ?
C9A C10A C11A 117.2(8) . . ?
C9A C10A C14A 123.4(7) . . ?
C11A C10A C14A 119.3(8) . . ?
O7A C32A O8A 123.2(11) . . ?
O7A C32A C31A 122.1(9) . . ?
O8A C32A C31A 114.7(10) . . ?
C10A C14A C15A 108.4(7) . . ?
C10A C14A H14A 110.0 . . ?
C15A C14A H14A 110.0 . . ?
C10A C14A H14B 110.0 . . ?
C15A C14A H14B 110.0 . . ?
H14A C14A H14B 108.4 . . ?
O2A C9A C8A 120.3(7) . . ?
O2A C9A C10A 117.5(7) . . ?
C8A C9A C10A 122.3(7) . . ?
C13A C8A C9A 117.5(8) . . ?
C13A C8A C7A 120.6(8) . . ?
C9A C8A C7A 121.8(7) . . ?
C12A C13A C8A 121.3(9) . . ?
C12A C13A H13A 119.4 . . ?
C8A C13A H13A 119.4 . . ?
C12A C11A C10A 120.2(9) . . ?
C12A C11A H11A 119.9 . . ?
C10A C11A H11A 119.9 . . ?
O2A C31A C32A 111.9(8) . . ?
O2A C31A H31A 109.2 . . ?
C32A C31A H31A 109.2 . . ?
O2A C31A H31B 109.2 . . ?
C32A C31A H31B 109.2 . . ?
H31A C31A H31B 107.9 . . ?
C34A O10A H10O 109.5 . . ?
O3A C33A C34A 110.5(7) . . ?
O3A C33A H33A 109.6 . . ?
C34A C33A H33A 109.6 . . ?
O3A C33A H33B 109.6 . . ?
C34A C33A H33B 109.6 . . ?
H33A C33A H33B 108.1 . . ?
C16A O3A C33A 111.5(6) . . ?
C16A O3A Na1 134.1(4) . . ?
C33A O3A Na1 114.4(5) . . ?
C34A O9A Na1 110.7(6) . . ?
O9A C34A O10A 124.9(9) . . ?
O9A C34A C33A 122.3(8) . . ?
O10A C34A C33A 112.8(9) . . ?
C17A C21A C22A 111.8(7) . . ?
C17A C21A H21A 109.3 . . ?
C22A C21A H21A 109.3 . . ?
C17A C21A H21B 109.3 . . ?
C22A C21A H21B 109.3 . . ?
H21A C21A H21B 107.9 . . ?
C16A C15A C20A 117.5(8) . . ?
C16A C15A C14A 122.6(7) . . ?
C20A C15A C14A 119.8(8) . . ?
C18A C17A C16A 117.0(9) . . ?
C18A C17A C21A 121.6(8) . . ?
C16A C17A C21A 121.4(7) . . ?
C19A C18A C17A 120.8(9) . . ?
C19A C18A H18A 119.6 . . ?
C17A C18A H18A 119.6 . . ?
C20A C19A C18A 121.2(9) . . ?
C20A C19A H19A 119.4 . . ?
C18A C19A H19A 119.4 . . ?
C19A C20A C15A 120.3(9) . . ?
C19A C20A H20A 119.8 . . ?
C15A C20A H20A 119.8 . . ?
C23A O4A C35A 111.3(6) . . ?
C23A O4A Na1 132.9(5) . . ?
C35A O4A Na1 115.4(4) . . ?
C36A O11A Na1 109.3(6) . . ?
C36A O11A Na2 128.0(6) . . ?
Na1 O11A Na2 77.5(2) . . ?
C36A O12A H12' 109.5 . . ?
C25A C24A C23A 116.7(9) . . ?
C25A C24A C28A 120.6(9) . . ?
C23A C24A C28A 122.3(8) . . ?
C23A C22A C27A 118.4(9) . . ?
C23A C22A C21A 122.2(8) . . ?
C27A C22A C21A 119.3(8) . . ?
C22A C23A O4A 120.9(8) . . ?
C22A C23A C24A 122.6(8) . . ?
O4A C23A C24A 116.4(7) . . ?
O4A C35A C36A 110.3(7) . . ?
O4A C35A H35A 109.6 . . ?
C36A C35A H35A 109.6 . . ?
O4A C35A H35B 109.6 . . ?
C36A C35A H35B 109.6 . . ?
H35A C35A H35B 108.1 . . ?
O11A C36A O12A 126.0(9) . . ?
O11A C36A C35A 124.6(8) . . ?
O12A C36A C35A 109.5(8) . . ?
C2A C28A C24A 108.9(7) . . ?
C2A C28A H28A 109.9 . . ?
C24A C28A H28A 109.9 . . ?
C2A C28A H28B 109.9 . . ?
C24A C28A H28B 109.9 . . ?
H28A C28A H28B 108.3 . . ?
C26A C25A C24A 121.2(10) . . ?
C26A C25A H25A 119.4 . . ?
C24A C25A H25A 119.4 . . ?
C25A C26A C27A 120.6(9) . . ?
C25A C26A H26A 119.7 . . ?
C27A C26A H26A 119.7 . . ?
C22A C27A C26A 120.3(10) . . ?
C22A C27A H27A 119.9 . . ?
C26A C27A H27A 119.9 . . ?
C30B O5B Na3 115.7(6) . . ?
C30B O5B Na2 119.4(7) . . ?
Na3 O5B Na2 84.1(2) . . ?
C1B O1B C29B 111.0(6) . . ?
C1B O1B Na3 136.5(5) . . ?
C29B O1B Na3 112.4(4) . . ?
C3B C2B C1B 116.5(8) . . ?
C3B C2B C28B 119.5(9) . . ?
C1B C2B C28B 123.8(8) . . ?
C6B C1B O1B 119.3(8) . . ?
C6B C1B C2B 123.5(7) . . ?
O1B C1B C2B 117.1(8) . . ?
C1B C6B C5B 118.2(9) . . ?
C1B C6B C7B 121.7(8) . . ?
C5B C6B C7B 120.1(8) . . ?
C8B C7B C6B 110.4(8) . . ?
C8B C7B H7B1 109.6 . . ?
C6B C7B H7B1 109.6 . . ?
C8B C7B H7B2 109.6 . . ?
C6B C7B H7B2 109.6 . . ?
H7B1 C7B H7B2 108.1 . . ?
O5B C30B O6B 126.5(9) . . ?
O5B C30B C29B 121.9(9) . . ?
O6B C30B C29B 111.6(9) . . ?
O6B C30B Na3 162.0(7) . . ?
C29B C30B Na3 80.7(6) . . ?
O1B C29B C30B 112.5(8) . . ?
O1B C29B H29C 109.1 . . ?
C30B C29B H29C 109.1 . . ?
O1B C29B H29D 109.1 . . ?
C30B C29B H29D 109.1 . . ?
H29C C29B H29D 107.8 . . ?
C6B C5B C4B 121.0(9) . . ?
C6B C5B H5B 119.5 . . ?
C4B C5B H5B 119.5 . . ?
C3B C4B C5B 120.1(7) . . ?
C3B C4B H4B 120.0 . . ?
C5B C4B H4B 120.0 . . ?
C4B C3B C2B 120.4(9) . . ?
C4B C3B H3B 119.8 . . ?
C2B C3B H3B 119.8 . . ?
C9B O2B C31B 112.6(6) . . ?
C9B O2B Na3 129.4(4) . . ?
C31B O2B Na3 117.6(5) . . ?
C32B O7B Na3 104.4(6) . . ?
C32B O8B H8B 109.5 . . ?
C13B C8B C9B 115.4(9) . . ?
C13B C8B C7B 120.8(8) . . ?
C9B C8B C7B 123.7(8) . . ?
C10B C9B C8B 123.8(8) . . ?
C10B C9B O2B 118.5(7) . . ?
C8B C9B O2B 117.7(8) . . ?
O2B C31B C32B 110.2(8) . . ?
O2B C31B H31C 109.6 . . ?
C32B C31B H31C 109.6 . . ?
O2B C31B H31D 109.6 . . ?
C32B C31B H31D 109.6 . . ?
H31C C31B H31D 108.1 . . ?
O7B C32B O8B 120.5(10) . . ?
O7B C32B C31B 123.8(10) . . ?
O8B C32B C31B 115.7(10) . . ?
C10B C14B C15B 110.9(7) . . ?
C10B C14B H14C 109.5 . . ?
C15B C14B H14C 109.5 . . ?
C10B C14B H14D 109.5 . . ?
C15B C14B H14D 109.5 . . ?
H14C C14B H14D 108.1 . . ?
C9B C10B C11B 118.8(8) . . ?
C9B C10B C14B 123.3(8) . . ?
C11B C10B C14B 117.8(9) . . ?
C12B C13B C8B 121.8(8) . . ?
C12B C13B H13B 119.1 . . ?
C8B C13B H13B 119.1 . . ?
C11B C12B C13B 120.5(9) . . ?
C11B C12B H12B 119.7 . . ?
C13B C12B H12B 119.7 . . ?
C12B C11B C10B 119.3(9) . . ?
C12B C11B H11B 120.3 . . ?
C10B C11B H11B 120.3 . . ?
C16B O3B C33B 109.2(6) . . ?
C16B O3B Na3 137.8(4) . . ?
C33B O3B Na3 112.7(5) . . ?
C34B O9B Na2 148.7(6) . . ?
C34B O9B Na3 116.2(6) . . ?
Na2 O9B Na3 88.3(3) . . ?
C16B C15B C20B 116.4(9) . . ?
C16B C15B C14B 122.8(8) . . ?
C20B C15B C14B 120.8(9) . . ?
C22B C21B C17B 111.6(8) . . ?
C22B C21B H21C 109.3 . . ?
C17B C21B H21C 109.3 . . ?
C22B C21B H21D 109.3 . . ?
C17B C21B H21D 109.3 . . ?
H21C C21B H21D 108.0 . . ?
C16B C17B C18B 116.6(9) . . ?
C16B C17B C21B 121.3(8) . . ?
C18B C17B C21B 122.0(9) . . ?
C17B C16B O3B 118.8(8) . . ?
C17B C16B C15B 124.3(8) . . ?
O3B C16B C15B 116.9(8) . . ?
O3B C33B C34B 109.7(7) . . ?
O3B C33B H33C 109.7 . . ?
C34B C33B H33C 109.7 . . ?
O3B C33B H33D 109.7 . . ?
C34B C33B H33D 109.7 . . ?
H33C C33B H33D 108.2 . . ?
O9B C34B O10B 126.2(9) . . ?
O9B C34B C33B 122.3(8) . . ?
O10B C34B C33B 111.4(8) . . ?
O10B C34B Na3 165.7(7) . . ?
C33B C34B Na3 80.7(5) . . ?
C19B C20B C15B 120.6(10) . . ?
C19B C20B H20B 119.7 . . ?
C15B C20B H20B 119.7 . . ?
C20B C19B C18B 120.0(10) . . ?
C20B C19B H19B 120.0 . . ?
C18B C19B H19B 120.0 . . ?
C19B C18B C17B 122.0(10) . . ?
C19B C18B H18B 119.0 . . ?
C17B C18B H18B 119.0 . . ?
C23B O4B C35B 112.7(7) . . ?
C23B O4B Na3 124.5(5) . . ?
C35B O4B Na3 122.8(5) . . ?
C36B O11B Na2 117.1(7) . . ?
C36B O11B Na3 109.6(6) . . ?
Na2 O11B Na3 75.0(2) . . ?
C36B O12B H12O 109.5 . . ?
O11B C36B O12B 124.6(10) . . ?
O11B C36B C35B 124.5(10) . . ?
O12B C36B C35B 110.9(12) . . ?
O4B C35B C36B 109.1(9) . . ?
O4B C35B H35C 109.9 . . ?
C36B C35B H35C 109.9 . . ?
O4B C35B H35D 109.9 . . ?
C36B C35B H35D 109.9 . . ?
H35C C35B H35D 108.3 . . ?
O4B C23B C22B 120.0(8) . . ?
O4B C23B C24B 117.7(8) . . ?
C22B C23B C24B 122.3(9) . . ?
C25B C24B C23B 117.9(9) . . ?
C25B C24B C28B 120.0(9) . . ?
C23B C24B C28B 121.9(8) . . ?
C2B C28B C24B 110.6(7) . . ?
C2B C28B H28C 109.5 . . ?
C24B C28B H28C 109.5 . . ?
C2B C28B H28D 109.5 . . ?
C24B C28B H28D 109.5 . . ?
H28C C28B H28D 108.1 . . ?
C27B C22B C23B 117.0(9) . . ?
C27B C22B C21B 119.1(9) . . ?
C23B C22B C21B 123.5(8) . . ?
C26B C27B C22B 121.3(10) . . ?
C26B C27B H27B 119.3 . . ?
C22B C27B H27B 119.3 . . ?
C25B C26B C27B 120.5(10) . . ?
C25B C26B H26B 119.8 . . ?
C27B C26B H26B 119.8 . . ?
C26B C25B C24B 120.8(10) . . ?
C26B C25B H25B 119.6 . . ?
C24B C25B H25B 119.6 . . ?
C1S O1S H1OS 109.0 . . ?
O1S C1S H1SA 110.5 . . ?
O1S C1S H1SB 109.2 . . ?
H1SA C1S H1SB 109.4 . . ?
O1S C1S H1SC 109.0 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.3 . . ?
H1W O1W H2W 107.7 . . ?

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_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C8A C7A C6A C5A 75.4(10) . . . . ?
C8A C7A C6A C1A -100.8(9) . . . . ?
C5A C6A C1A O1A 175.1(8) . . . . ?
C7A C6A C1A O1A -8.6(11) . . . . ?
C5A C6A C1A C2A -4.3(13) . . . . ?
C7A C6A C1A C2A 171.9(7) . . . . ?
C29A O1A C1A C6A -88.5(9) . . . . ?
Na1 O1A C1A C6A 88.3(8) . . . . ?
C29A O1A C1A C2A 91.0(8) . . . . ?
Na1 O1A C1A C2A -92.2(8) . . . . ?
C6A C1A C2A C3A 3.3(12) . . . . ?
O1A C1A C2A C3A -176.2(7) . . . . ?
C6A C1A C2A C28A -172.6(8) . . . . ?
O1A C1A C2A C28A 8.0(11) . . . . ?
C1A O1A C29A C30A 154.6(8) . . . . ?
Na1 O1A C29A C30A -22.5(10) . . . . ?
Na2 O5A C30A O6A -63.0(13) . . . . ?
Na1 O5A C30A O6A -161.8(8) . . . . ?
Na2 O5A C30A C29A 117.4(9) . . . . ?
Na1 O5A C30A C29A 18.6(12) . . . . ?
O1A C29A C30A O5A 1.3(13) . . . . ?
O1A C29A C30A O6A -178.3(8) . . . . ?
C1A C2A C3A C4A -0.5(14) . . . . ?
C28A C2A C3A C4A 175.3(10) . . . . ?
C2A C3A C4A C5A -1.1(17) . . . . ?
C3A C4A C5A C6A 0.0(17) . . . . ?
C1A C6A C5A C4A 2.6(15) . . . . ?
C7A C6A C5A C4A -173.8(9) . . . . ?
Na1 O7A C32A O8A -161.3(10) . . . . ?
Na2 O7A C32A O8A -65.3(14) . . . . ?
Na1 O7A C32A C31A 18.7(13) . . . . ?
Na2 O7A C32A C31A 114.7(9) . . . . ?
C9A C10A C14A C15A -94.7(10) . . . . ?
C11A C10A C14A C15A 81.9(10) . . . . ?
C31A O2A C9A C8A 91.7(10) . . . . ?
Na1 O2A C9A C8A -84.3(9) . . . . ?
C31A O2A C9A C10A -88.8(9) . . . . ?
Na1 O2A C9A C10A 95.2(9) . . . . ?
C11A C10A C9A O2A 174.0(7) . . . . ?
C14A C10A C9A O2A -9.4(12) . . . . ?
C11A C10A C9A C8A -6.6(13) . . . . ?
C14A C10A C9A C8A 170.1(8) . . . . ?
O2A C9A C8A C13A -174.3(8) . . . . ?
C10A C9A C8A C13A 6.3(13) . . . . ?
O2A C9A C8A C7A 9.1(12) . . . . ?
C10A C9A C8A C7A -170.4(8) . . . . ?
C6A C7A C8A C13A -79.9(10) . . . . ?
C6A C7A C8A C9A 96.7(10) . . . . ?
C11A C12A C13A C8A -4.1(16) . . . . ?
C9A C8A C13A C12A -0.9(14) . . . . ?
C7A C8A C13A C12A 175.8(9) . . . . ?
C13A C12A C11A C10A 3.8(16) . . . . ?
C9A C10A C11A C12A 1.5(14) . . . . ?
C14A C10A C11A C12A -175.3(9) . . . . ?
C9A O2A C31A C32A 157.8(8) . . . . ?
Na1 O2A C31A C32A -25.5(10) . . . . ?
O7A C32A C31A O2A 4.6(15) . . . . ?
O8A C32A C31A O2A -175.4(9) . . . . ?
C15A C16A O3A C33A 85.9(9) . . . . ?
C17A C16A O3A C33A -95.3(9) . . . . ?
C15A C16A O3A Na1 -92.8(9) . . . . ?
C17A C16A O3A Na1 86.0(9) . . . . ?
C34A C33A O3A C16A 151.1(7) . . . . ?
C34A C33A O3A Na1 -29.9(9) . . . . ?
Na1 O9A C34A O10A -147.3(8) . . . . ?
Na1 O9A C34A C33A 34.7(11) . . . . ?
O3A C33A C34A O9A -5.0(14) . . . . ?
O3A C33A C34A O10A 176.7(7) . . . . ?
C17A C16A C15A C20A 5.2(13) . . . . ?
O3A C16A C15A C20A -176.1(8) . . . . ?
C17A C16A C15A C14A -171.6(8) . . . . ?
O3A C16A C15A C14A 7.2(11) . . . . ?
C10A C14A C15A C16A 95.6(9) . . . . ?
C10A C14A C15A C20A -81.0(10) . . . . ?
C15A C16A C17A C18A -3.1(13) . . . . ?
O3A C16A C17A C18A 178.1(7) . . . . ?
C15A C16A C17A C21A 174.9(8) . . . . ?
O3A C16A C17A C21A -3.8(12) . . . . ?
C22A C21A C17A C18A 77.1(10) . . . . ?
C22A C21A C17A C16A -100.9(9) . . . . ?
C16A C17A C18A C19A 0.1(13) . . . . ?
C21A C17A C18A C19A -177.9(9) . . . . ?
C17A C18A C19A C20A 0.6(15) . . . . ?
C18A C19A C20A C15A 1.5(16) . . . . ?
C16A C15A C20A C19A -4.3(14) . . . . ?
C14A C15A C20A C19A 172.6(9) . . . . ?
C17A C21A C22A C23A 96.1(9) . . . . ?
C17A C21A C22A C27A -80.7(10) . . . . ?
C27A C22A C23A O4A -171.4(8) . . . . ?
C21A C22A C23A O4A 11.8(12) . . . . ?
C27A C22A C23A C24A 5.1(14) . . . . ?
C21A C22A C23A C24A -171.8(8) . . . . ?
C35A O4A C23A C22A 84.8(9) . . . . ?
Na1 O4A C23A C22A -87.7(9) . . . . ?
C35A O4A C23A C24A -91.9(9) . . . . ?
Na1 O4A C23A C24A 95.6(8) . . . . ?
C25A C24A C23A C22A -4.0(14) . . . . ?
C28A C24A C23A C22A 168.7(9) . . . . ?
C25A C24A C23A O4A 172.6(8) . . . . ?
C28A C24A C23A O4A -14.7(12) . . . . ?
C23A O4A C35A C36A 161.5(7) . . . . ?
Na1 O4A C35A C36A -24.6(9) . . . . ?
Na1 O11A C36A O12A -146.9(8) . . . . ?
Na2 O11A C36A O12A -57.9(13) . . . . ?
Na1 O11A C36A C35A 33.9(11) . . . . ?
Na2 O11A C36A C35A 122.9(8) . . . . ?
O4A C35A C36A O11A -8.6(13) . . . . ?
O4A C35A C36A O12A 172.1(7) . . . . ?
C3A C2A C28A C24A -75.6(10) . . . . ?
C1A C2A C28A C24A 100.0(9) . . . . ?
C25A C24A C28A C2A 80.9(11) . . . . ?
C23A C24A C28A C2A -91.4(10) . . . . ?
C23A C24A C25A C26A -0.6(15) . . . . ?
C28A C24A C25A C26A -173.4(10) . . . . ?
C24A C25A C26A C27A 4.0(18) . . . . ?
C23A C22A C27A C26A -1.6(15) . . . . ?
C21A C22A C27A C26A 175.4(10) . . . . ?
C25A C26A C27A C22A -2.9(18) . . . . ?
C29B O1B C1B C6B -87.8(10) . . . . ?
Na3 O1B C1B C6B 94.9(10) . . . . ?
C29B O1B C1B C2B 93.3(9) . . . . ?
Na3 O1B C1B C2B -83.9(10) . . . . ?
C3B C2B C1B C6B 6.4(13) . . . . ?
C28B C2B C1B C6B -168.1(8) . . . . ?
C3B C2B C1B O1B -174.8(7) . . . . ?
C28B C2B C1B O1B 10.7(12) . . . . ?
O1B C1B C6B C5B 174.1(7) . . . . ?
C2B C1B C6B C5B -7.2(13) . . . . ?
O1B C1B C6B C7B -7.4(12) . . . . ?
C2B C1B C6B C7B 171.3(8) . . . . ?
C1B C6B C7B C8B -93.9(10) . . . . ?
C5B C6B C7B C8B 84.6(10) . . . . ?
Na3 O5B C30B O6B -159.9(10) . . . . ?
Na2 O5B C30B O6B -61.8(14) . . . . ?
Na3 O5B C30B C29B 21.1(13) . . . . ?
Na2 O5B C30B C29B 119.2(9) . . . . ?
Na2 O5B C30B Na3 98.1(7) . . . . ?
C1B O1B C29B C30B 163.8(8) . . . . ?
Na3 O1B C29B C30B -18.3(11) . . . . ?
O5B C30B C29B O1B -1.4(15) . . . . ?
O6B C30B C29B O1B 179.4(9) . . . . ?
Na3 C30B C29B O1B 13.1(8) . . . . ?
C1B C6B C5B C4B 3.3(14) . . . . ?
C7B C6B C5B C4B -175.3(8) . . . . ?
C6B C5B C4B C3B 1.0(14) . . . . ?
C5B C4B C3B C2B -1.7(14) . . . . ?
C1B C2B C3B C4B -1.8(13) . . . . ?
C28B C2B C3B C4B 173.0(8) . . . . ?
C6B C7B C8B C13B -78.7(10) . . . . ?
C6B C7B C8B C9B 98.9(9) . . . . ?
C13B C8B C9B C10B 5.9(12) . . . . ?
C7B C8B C9B C10B -171.8(8) . . . . ?
C13B C8B C9B O2B -175.6(7) . . . . ?
C7B C8B C9B O2B 6.6(12) . . . . ?
C31B O2B C9B C10B -98.6(9) . . . . ?
Na3 O2B C9B C10B 88.1(9) . . . . ?
C31B O2B C9B C8B 82.9(9) . . . . ?
Na3 O2B C9B C8B -90.5(8) . . . . ?
C9B O2B C31B C32B 139.3(8) . . . . ?
Na3 O2B C31B C32B -46.5(10) . . . . ?
Na3 O7B C32B O8B -146.4(10) . . . . ?
Na3 O7B C32B C31B 33.2(13) . . . . ?
O2B C31B C32B O7B 0.2(16) . . . . ?
O2B C31B C32B O8B 179.8(10) . . . . ?
C8B C9B C10B C11B -4.0(13) . . . . ?
O2B C9B C10B C11B 177.6(7) . . . . ?
C8B C9B C10B C14B 171.8(8) . . . . ?
O2B C9B C10B C14B -6.6(12) . . . . ?
C15B C14B C10B C9B -101.7(10) . . . . ?
C15B C14B C10B C11B 74.1(10) . . . . ?
C9B C8B C13B C12B -2.5(13) . . . . ?
C7B C8B C13B C12B 175.3(9) . . . . ?
C8B C13B C12B C11B -2.7(14) . . . . ?
C13B C12B C11B C10B 4.9(14) . . . . ?
C9B C10B C11B C12B -1.6(13) . . . . ?
C14B C10B C11B C12B -177.7(8) . . . . ?
C10B C14B C15B C16B 92.6(10) . . . . ?
C10B C14B C15B C20B -83.9(10) . . . . ?
C22B C21B C17B C16B -90.2(10) . . . . ?
C22B C21B C17B C18B 85.9(11) . . . . ?
C18B C17B C16B O3B 171.7(7) . . . . ?
C21B C17B C16B O3B -12.0(11) . . . . ?
C18B C17B C16B C15B -5.4(12) . . . . ?
C21B C17B C16B C15B 170.9(8) . . . . ?
C33B O3B C16B C17B -82.9(9) . . . . ?
Na3 O3B C16B C17B 90.5(9) . . . . ?
C33B O3B C16B C15B 94.4(8) . . . . ?
Na3 O3B C16B C15B -92.2(9) . . . . ?
C20B C15B C16B C17B 4.7(12) . . . . ?
C14B C15B C16B C17B -171.9(8) . . . . ?
C20B C15B C16B O3B -172.4(7) . . . . ?
C14B C15B C16B O3B 11.0(11) . . . . ?
C16B O3B C33B C34B 146.5(8) . . . . ?
Na3 O3B C33B C34B -28.7(9) . . . . ?
Na2 O9B C34B O10B -54(2) . . . . ?
Na3 O9B C34B O10B 167.6(8) . . . . ?
Na2 O9B C34B C33B 122.8(11) . . . . ?
Na3 O9B C34B C33B -15.5(12) . . . . ?
Na2 O9B C34B Na3 138.3(16) . . . . ?
O3B C33B C34B O9B 30.6(13) . . . . ?
O3B C33B C34B O10B -152.1(8) . . . . ?
O3B C33B C34B Na3 20.0(6) . . . . ?
C16B C15B C20B C19B -0.4(12) . . . . ?
C14B C15B C20B C19B 176.2(8) . . . . ?
C15B C20B C19B C18B -2.8(13) . . . . ?
C20B C19B C18B C17B 2.0(14) . . . . ?
C16B C17B C18B C19B 1.9(13) . . . . ?
C21B C17B C18B C19B -174.4(8) . . . . ?
Na2 O11B C36B O12B -69.6(14) . . . . ?
Na3 O11B C36B O12B -152.3(10) . . . . ?
Na2 O11B C36B C35B 111.1(11) . . . . ?
Na3 O11B C36B C35B 28.4(13) . . . . ?
C23B O4B C35B C36B 153.4(9) . . . . ?
Na3 O4B C35B C36B -28.3(12) . . . . ?
O11B C36B C35B O4B -4.9(16) . . . . ?
O12B C36B C35B O4B 175.7(9) . . . . ?
C35B O4B C23B C22B 89.1(10) . . . . ?
Na3 O4B C23B C22B -89.2(9) . . . . ?
C35B O4B C23B C24B -91.6(10) . . . . ?
Na3 O4B C23B C24B 90.2(8) . . . . ?
O4B C23B C24B C25B 176.8(7) . . . . ?
C22B C23B C24B C25B -3.9(13) . . . . ?
O4B C23B C24B C28B -9.1(12) . . . . ?
C22B C23B C24B C28B 170.3(8) . . . . ?
C3B C2B C28B C24B -81.0(10) . . . . ?
C1B C2B C28B C24B 93.4(10) . . . . ?
C25B C24B C28B C2B 70.3(10) . . . . ?
C23B C24B C28B C2B -103.8(9) . . . . ?
O4B C23B C22B C27B -177.1(8) . . . . ?
C24B C23B C22B C27B 3.6(13) . . . . ?
O4B C23B C22B C21B 9.9(13) . . . . ?
C24B C23B C22B C21B -169.5(8) . . . . ?
C17B C21B C22B C27B -70.9(11) . . . . ?
C17B C21B C22B C23B 102.1(10) . . . . ?
C23B C22B C27B C26B 0.3(14) . . . . ?
C21B C22B C27B C26B 173.7(9) . . . . ?
C22B C27B C26B C25B -4.0(15) . . . . ?
C27B C26B C25B C24B 3.7(15) . . . . ?
C23B C24B C25B C26B 0.1(14) . . . . ?
C28B C24B C25B C26B -174.1(9) . . . . ?

_refine_diff_density_max         0.377
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.063

_shelxl_version_number           2014-3


# start Validation Reply Form
_vrf_PLAT417_free_calix4tube_1   
;
PROBLEM: Short Inter D-H..H-D       H1W    ..  H8B     ..       2.07 Ang.  
RESPONSE: Concerning these hydrogens, the electronic density peak regarding these atoms was first found from the difference Fourier map so that their position was fixed according to stereochemical assumption in which bond length and angle follow the riding model. Furthermore, they are correctly pointed towards their hydrogen bonding acceptor oxygen. Therefore, there is no problem of assigning their position.
;
_vrf_PLAT340_free_calix4tube_1   
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01336 Ang.  
RESPONSE: This error message appears because of the low amount of observed refelctions (Ratio Observed / Unique Reflections is only 47%). In this way, a large amount of unobserved reflections in practice are being used in the refinement, resulting in low precision on atom positions.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_free_calix4tube_2
_database_code_depnum_ccdc_archive 'CCDC 1433707'
_audit_update_record             
;
2016-08-19 deposited with the CCDC.
2016-08-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C288 H246 Na12 O97'
_chemical_formula_weight         5534.74

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'
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   14.840(2)
_cell_length_b                   17.911(3)
_cell_length_c                   31.010(5)
_cell_angle_alpha                79.663(11)
_cell_angle_beta                 86.268(11)
_cell_angle_gamma                82.469(12)
_cell_volume                     8032(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    45357
_cell_measurement_theta_min      1.39
_cell_measurement_theta_max      25.39

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2882
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'Blessing, R. H. (1995) Acta Cryst., A51, 33-38'
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_T_max  0.994


_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_reflns_number            45357
_diffrn_reflns_av_unetI/netI     0.3544
_diffrn_reflns_av_R_equivalents  0.1181
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         1.385
_diffrn_reflns_theta_max         25.391
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measured_fraction_theta_full 0.939
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_Laue_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_point_group_measured_fraction_full 0.939
_reflns_number_total             27303
_reflns_number_gt                5220
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1511P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         27303
_refine_ls_number_parameters     1735
_refine_ls_number_restraints     1992
_refine_ls_R_factor_all          0.3084
_refine_ls_R_factor_gt           0.1435
_refine_ls_wR_factor_ref         0.4050
_refine_ls_wR_factor_gt          0.3559
_refine_ls_goodness_of_fit_ref   0.878
_refine_ls_restrained_S_all      0.931
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Na6 Na 0.2960(5) 0.7743(4) 0.99288(14) 0.154(2) Uani 1 1 d . U . . .
Na1 Na 0.4713(3) 0.6759(2) 0.63861(10) 0.0606(10) Uani 1 1 d . U . . .
Na4 Na 0.2703(3) 0.8486(2) 1.18847(13) 0.0876(12) Uani 1 1 d . U . . .
Na2 Na 0.6453(3) 0.7090(2) 0.57386(11) 0.0695(11) Uani 1 1 d . U . . .
Na3 Na 0.7877(3) 0.74692(19) 0.48995(10) 0.0589(10) Uani 1 1 d . U . . .
Na5 Na 0.2714(6) 0.8119(6) 1.09059(19) 0.237(3) Uani 1 1 d . U . . .
O1A O 0.3599(5) 0.7896(4) 0.6411(2) 0.0765(18) Uani 1 1 d . U . . .
C2A C 0.2852(9) 0.8166(5) 0.7087(4) 0.070(3) Uani 1 1 d . U . . .
C1A C 0.2814(9) 0.7998(6) 0.6688(4) 0.069(3) Uani 1 1 d . U . . .
C6A C 0.2070(10) 0.7906(6) 0.6526(4) 0.081(3) Uani 1 1 d . U . . .
C7A C 0.2003(9) 0.7571(8) 0.6105(4) 0.116(4) Uani 1 1 d . U . . .
H7A1 H 0.1478 0.7843 0.5949 0.139 Uiso 1 1 calc R U . . .
H7A2 H 0.2539 0.7667 0.5917 0.139 Uiso 1 1 calc R U . . .
C29A C 0.3970(9) 0.8618(7) 0.6228(4) 0.106(4) Uani 1 1 d . U . . .
H29C H 0.3543 0.9049 0.6288 0.127 Uiso 1 1 calc R U . . .
H29D H 0.4536 0.8636 0.6364 0.127 Uiso 1 1 calc R U . . .
C3A C 0.2037(10) 0.8307(7) 0.7335(4) 0.095(4) Uani 1 1 d . U . . .
H3A H 0.2043 0.8425 0.7614 0.114 Uiso 1 1 calc R U . . .
C4A C 0.1269(9) 0.8267(7) 0.7159(4) 0.088(4) Uani 1 1 d . U . . .
H4A H 0.0723 0.8401 0.7307 0.106 Uiso 1 1 calc R U . . .
C5A C 0.1249(9) 0.8034(6) 0.6761(4) 0.089(3) Uani 1 1 d . U . . .
H5A H 0.0703 0.7964 0.6652 0.107 Uiso 1 1 calc R U . . .
O6A O 0.4379(8) 0.9404(6) 0.5610(3) 0.185(5) Uani 1 1 d . U . . .
H6A H 0.4467 0.9491 0.5343 0.277 Uiso 1 1 calc R U . . .
O5A O 0.403(2) 0.8259(10) 0.5540(5) 0.392(16) Uani 1 1 d . U . . .
C30A C 0.4136(18) 0.8664(16) 0.5739(7) 0.198(8) Uani 1 1 d . U . . .
O2A O 0.3506(6) 0.6369(4) 0.6038(2) 0.087(2) Uani 1 1 d . U . . .
O7A O 0.5012(6) 0.6745(5) 0.5659(2) 0.118(3) Uani 1 1 d . U . . .
C8A C 0.1927(10) 0.6763(10) 0.6172(4) 0.098(3) Uani 1 1 d . U . . .
C9A C 0.2656(10) 0.6135(9) 0.6210(4) 0.092(3) Uani 1 1 d . U . . .
C31A C 0.3607(9) 0.6416(7) 0.5562(3) 0.094(3) Uani 1 1 d . U . . .
H31A H 0.3539 0.5924 0.5487 0.113 Uiso 1 1 calc R U . . .
H31B H 0.3134 0.6790 0.5423 0.113 Uiso 1 1 calc R U . . .
C32A C 0.4440(10) 0.6620(7) 0.5411(3) 0.087(3) Uani 1 1 d . U . . .
C14A C 0.3404(9) 0.4809(7) 0.6379(4) 0.100(3) Uani 1 1 d . U . . .
H14C H 0.3897 0.5016 0.6194 0.121 Uiso 1 1 calc R U . . .
H14D H 0.3291 0.4343 0.6285 0.121 Uiso 1 1 calc R U . . .
C10A C 0.2558(9) 0.5381(9) 0.6330(4) 0.098(3) Uani 1 1 d . U . . .
C13A C 0.1089(10) 0.6468(10) 0.6314(4) 0.120(4) Uani 1 1 d . U . . .
H13A H 0.0567 0.6812 0.6333 0.145 Uiso 1 1 calc R U . . .
C12A C 0.1013(10) 0.5667(11) 0.6429(5) 0.121(5) Uani 1 1 d . U . . .
H12A H 0.0437 0.5512 0.6489 0.145 Uiso 1 1 calc R U . . .
C11A C 0.1714(10) 0.5149(10) 0.6453(5) 0.125(5) Uani 1 1 d . U . . .
H11A H 0.1651 0.4636 0.6551 0.150 Uiso 1 1 calc R U . . .
O8A O 0.4562(7) 0.6698(5) 0.5003(2) 0.140(4) Uani 1 1 d . U . . .
O3A O 0.4878(5) 0.5416(4) 0.6711(2) 0.0720(18) Uani 1 1 d . U . . .
O10A O 0.7118(6) 0.5005(4) 0.6279(2) 0.099(3) Uani 1 1 d . U . . .
H10A H 0.7517 0.5271 0.6179 0.148 Uiso 1 1 calc R U . . .
C21A C 0.5117(8) 0.5437(6) 0.7605(3) 0.087(3) Uani 1 1 d . U . . .
H21C H 0.5469 0.5140 0.7844 0.104 Uiso 1 1 calc R U . . .
H21D H 0.5539 0.5606 0.7366 0.104 Uiso 1 1 calc R U . . .
C17A C 0.4482(9) 0.4921(6) 0.7447(4) 0.086(3) Uani 1 1 d . U . . .
C18A C 0.3969(10) 0.4440(8) 0.7722(5) 0.109(4) Uani 1 1 d . U . . .
H18A H 0.4043 0.4378 0.8023 0.130 Uiso 1 1 calc R U . . .
C19A C 0.3396(12) 0.4071(8) 0.7587(6) 0.120(5) Uani 1 1 d . U . . .
H19A H 0.3106 0.3720 0.7789 0.144 Uiso 1 1 calc R U . . .
C20A C 0.3208(11) 0.4173(7) 0.7181(5) 0.117(4) Uani 1 1 d . U . . .
H20A H 0.2741 0.3933 0.7100 0.141 Uiso 1 1 calc R U . . .
C15A C 0.3679(9) 0.4628(7) 0.6860(5) 0.095(3) Uani 1 1 d . U . . .
C16A C 0.4299(8) 0.4992(6) 0.7011(4) 0.071(3) Uani 1 1 d . U . . .
C33A C 0.5704(8) 0.4943(6) 0.6578(4) 0.093(3) Uani 1 1 d . U . . .
H33E H 0.5928 0.4583 0.6831 0.112 Uiso 1 1 calc R U . . .
H33F H 0.5548 0.4652 0.6364 0.112 Uiso 1 1 calc R U . . .
C34A C 0.6442(9) 0.5411(8) 0.6384(3) 0.075(3) Uani 1 1 d . U . . .
O9A O 0.6262(5) 0.6090(4) 0.6349(2) 0.091(2) Uani 1 1 d . U . . .
O11A O 0.5784(5) 0.7644(3) 0.63578(18) 0.0634(16) Uani 1 1 d . U . . .
O4A O 0.4999(5) 0.6941(3) 0.70935(17) 0.0600(17) Uani 1 1 d . U . . .
O12A O 0.6939(6) 0.7886(4) 0.6711(2) 0.096(3) Uani 1 1 d . U . . .
H12' H 0.7106 0.8077 0.6463 0.144 Uiso 1 1 calc R U . . .
C36A C 0.6182(8) 0.7588(6) 0.6692(3) 0.073(3) Uani 1 1 d . U . . .
C35A C 0.5852(8) 0.7224(6) 0.7128(3) 0.087(4) Uani 1 1 d . U . . .
H35C H 0.6298 0.6805 0.7249 0.104 Uiso 1 1 calc R U . . .
H35D H 0.5772 0.7594 0.7326 0.104 Uiso 1 1 calc R U . . .
C23A C 0.4506(8) 0.6833(6) 0.7485(3) 0.066(3) Uani 1 1 d . U . . .
C24A C 0.3962(8) 0.7405(7) 0.7592(3) 0.073(3) Uani 1 1 d . U . . .
C28A C 0.3728(8) 0.8145(6) 0.7303(3) 0.086(3) Uani 1 1 d . U . . .
H28C H 0.4211 0.8230 0.7080 0.103 Uiso 1 1 calc R U . . .
H28D H 0.3678 0.8553 0.7474 0.103 Uiso 1 1 calc R U . . .
C22A C 0.4611(9) 0.6088(7) 0.7749(3) 0.084(3) Uani 1 1 d . U . . .
C25A C 0.3454(8) 0.7325(7) 0.8041(3) 0.096(4) Uani 1 1 d . U . . .
H25A H 0.3075 0.7727 0.8133 0.115 Uiso 1 1 calc R U . . .
C26A C 0.3610(10) 0.6576(8) 0.8308(4) 0.112(5) Uani 1 1 d . U . . .
H26A H 0.3365 0.6493 0.8594 0.134 Uiso 1 1 calc R U . . .
C27A C 0.4101(9) 0.6007(7) 0.8149(3) 0.094(4) Uani 1 1 d . U . . .
H27A H 0.4109 0.5519 0.8314 0.112 Uiso 1 1 calc R U . . .
O1B O 0.7164(5) 0.8305(3) 0.42732(17) 0.0543(16) Uani 1 1 d . U . . .
C5B C 0.7931(7) 0.9786(6) 0.3408(3) 0.064(3) Uani 1 1 d . U . . .
H5B H 0.8076 1.0284 0.3373 0.077 Uiso 1 1 calc R U . . .
C7B C 0.7853(7) 0.9766(5) 0.4238(3) 0.064(2) Uani 1 1 d . U . . .
H7B1 H 0.7695 1.0315 0.4165 0.077 Uiso 1 1 calc R U . . .
H7B2 H 0.7450 0.9572 0.4479 0.077 Uiso 1 1 calc R U . . .
C6B C 0.7732(6) 0.9388(6) 0.3832(3) 0.052(2) Uani 1 1 d . U . . .
C1B C 0.7498(7) 0.8655(6) 0.3873(3) 0.054(2) Uani 1 1 d . U . . .
C29B C 0.6217(7) 0.8453(6) 0.4309(3) 0.072(3) Uani 1 1 d . U . . .
H29E H 0.5954 0.8203 0.4103 0.086 Uiso 1 1 calc R U . . .
H29F H 0.6038 0.8999 0.4230 0.086 Uiso 1 1 calc R U . . .
C30B C 0.5842(10) 0.8181(8) 0.4762(5) 0.129(5) Uani 1 1 d . U . . .
O5B O 0.6358(5) 0.7884(5) 0.5068(2) 0.119(3) Uani 1 1 d . U . . .
O6B O 0.4974(7) 0.8343(8) 0.4782(4) 0.250(8) Uani 1 1 d . U . . .
H6B H 0.4777 0.8195 0.5032 0.375 Uiso 1 1 calc R U . . .
C4B C 0.7913(7) 0.9464(6) 0.3068(3) 0.072(3) Uani 1 1 d . U . . .
H4B H 0.7975 0.9757 0.2790 0.086 Uiso 1 1 calc R U . . .
C3B C 0.7796(7) 0.8650(7) 0.3105(3) 0.075(3) Uani 1 1 d . U . . .
H3B H 0.7839 0.8418 0.2858 0.090 Uiso 1 1 calc R U . . .
C2B C 0.7621(6) 0.8243(6) 0.3515(3) 0.055(2) Uani 1 1 d . U . . .
O2B O 0.8449(5) 0.8637(3) 0.49849(17) 0.0607(16) Uani 1 1 d . U . . .
O7B O 0.7714(5) 0.7795(4) 0.56817(19) 0.0828(19) Uani 1 1 d . U . . .
O8B O 0.7531(6) 0.8730(4) 0.6076(2) 0.093(3) Uani 1 1 d . U . . .
C14B C 1.0281(7) 0.8127(6) 0.5175(3) 0.072(3) Uani 1 1 d . U . . .
H14E H 1.0710 0.8275 0.5358 0.086 Uiso 1 1 calc R U . . .
H14F H 0.9752 0.7994 0.5360 0.086 Uiso 1 1 calc R U . . .
C10B C 0.9993(8) 0.8799(5) 0.4819(3) 0.059(2) Uani 1 1 d . U . . .
C9B C 0.9084(8) 0.9031(6) 0.4721(3) 0.062(2) Uani 1 1 d . U . . .
C8B C 0.8822(8) 0.9588(5) 0.4373(3) 0.062(3) Uani 1 1 d . U . . .
C11B C 1.0630(8) 0.9231(6) 0.4558(3) 0.076(3) Uani 1 1 d . U . . .
H11B H 1.1237 0.9131 0.4631 0.091 Uiso 1 1 calc R U . . .
C12B C 1.0408(8) 0.9777(5) 0.4208(3) 0.074(3) Uani 1 1 d . U . . .
H12B H 1.0851 1.0012 0.4027 0.089 Uiso 1 1 calc R U . . .
C13B C 0.9445(8) 0.9983(6) 0.4129(3) 0.070(3) Uani 1 1 d . U . . .
H13B H 0.9259 1.0388 0.3909 0.084 Uiso 1 1 calc R U . . .
C31B C 0.8173(9) 0.9013(6) 0.5357(3) 0.093(4) Uani 1 1 d . U . . .
H31C H 0.7725 0.9450 0.5269 0.111 Uiso 1 1 calc R U . . .
H31D H 0.8696 0.9197 0.5457 0.111 Uiso 1 1 calc R U . . .
C32B C 0.7769(7) 0.8466(6) 0.5734(3) 0.063(3) Uani 1 1 d . U . . .
C33B C 0.9308(7) 0.6455(5) 0.5541(3) 0.057(2) Uani 1 1 d . U . . .
H33A H 0.9790 0.6030 0.5564 0.069 Uiso 1 1 calc R U . . .
H33B H 0.9420 0.6781 0.5745 0.069 Uiso 1 1 calc R U . . .
O3B O 0.9320(4) 0.6893(3) 0.50906(18) 0.0570(15) Uani 1 1 d . U . . .
C18B C 1.1504(8) 0.6239(6) 0.4564(3) 0.072(3) Uani 1 1 d . U . . .
H18B H 1.1771 0.5833 0.4432 0.086 Uiso 1 1 calc R U . . .
O9B O 0.7749(5) 0.6343(3) 0.54377(18) 0.0578(16) Uani 1 1 d . U . . .
O10B O 0.8449(5) 0.5709(4) 0.6024(2) 0.097(3) Uani 1 1 d . U . . .
C34B C 0.8425(9) 0.6163(6) 0.5657(3) 0.069(3) Uani 1 1 d . U . . .
C16B C 1.0233(8) 0.6878(6) 0.4906(3) 0.057(2) Uani 1 1 d . U . . .
C15B C 1.0712(8) 0.7436(6) 0.4990(3) 0.066(3) Uani 1 1 d . U . . .
C21B C 0.9911(7) 0.5794(5) 0.4553(3) 0.059(3) Uani 1 1 d . U . . .
H21E H 1.0249 0.5294 0.4550 0.071 Uiso 1 1 calc R U . . .
H21F H 0.9409 0.5736 0.4769 0.071 Uiso 1 1 calc R U . . .
C17B C 1.0534(7) 0.6331(5) 0.4681(3) 0.051(2) Uani 1 1 d . U . . .
C19B C 1.2008(8) 0.6776(7) 0.4658(3) 0.079(3) Uani 1 1 d . U . . .
H19B H 1.2625 0.6736 0.4577 0.094 Uiso 1 1 calc R U . . .
C20B C 1.1652(8) 0.7353(7) 0.4859(3) 0.076(3) Uani 1 1 d . U . . .
H20B H 1.2021 0.7703 0.4915 0.091 Uiso 1 1 calc R U . . .
C25B C 0.8975(8) 0.6837(6) 0.3265(3) 0.067(3) Uani 1 1 d . U . . .
H25B H 0.8801 0.7077 0.2986 0.081 Uiso 1 1 calc R U . . .
O4B O 0.8086(4) 0.6558(3) 0.44070(17) 0.0581(16) Uani 1 1 d . U . . .
C28B C 0.7471(7) 0.7391(6) 0.3595(3) 0.062(2) Uani 1 1 d . U . . .
H28E H 0.7120 0.7265 0.3867 0.074 Uiso 1 1 calc R U . . .
H28F H 0.7143 0.7284 0.3357 0.074 Uiso 1 1 calc R U . . .
C24B C 0.8400(8) 0.6925(5) 0.3619(3) 0.064(3) Uani 1 1 d . U . . .
C23B C 0.8657(7) 0.6534(5) 0.4041(3) 0.052(2) Uani 1 1 d . U . . .
C22B C 0.9541(8) 0.6118(5) 0.4101(3) 0.058(2) Uani 1 1 d . U . . .
C27B C 1.0076(8) 0.6071(6) 0.3715(3) 0.072(3) Uani 1 1 d . U . . .
H27B H 1.0653 0.5796 0.3733 0.086 Uiso 1 1 calc R U . . .
C26B C 0.9771(8) 0.6419(6) 0.3312(3) 0.072(3) Uani 1 1 d . U . . .
H26B H 1.0138 0.6357 0.3063 0.086 Uiso 1 1 calc R U . . .
C35B C 0.7747(7) 0.5828(6) 0.4551(3) 0.070(3) Uani 1 1 d . U . . .
H35E H 0.7897 0.5515 0.4325 0.084 Uiso 1 1 calc R U . . .
H35F H 0.8053 0.5568 0.4813 0.084 Uiso 1 1 calc R U . . .
C36B C 0.6772(12) 0.5895(10) 0.4644(5) 0.112(4) Uani 1 1 d . U . . .
O11B O 0.6303(7) 0.6519(7) 0.4595(5) 0.198(6) Uani 1 1 d . U . . .
O12B O 0.6416(7) 0.5320(5) 0.4782(3) 0.146(4) Uani 1 1 d . U . . .
H12O H 0.5866 0.5434 0.4817 0.219 Uiso 1 1 calc R U . . .
O1C O 0.1791(5) 0.9697(4) 1.1949(2) 0.087(2) Uani 1 1 d . U . . .
C30C C 0.1483(15) 0.9448(14) 1.1238(4) 0.214(5) Uani 1 1 d . U . . .
O6C O 0.0965(13) 1.0025(10) 1.0905(4) 0.310(9) Uani 1 1 d . U . . .
H6C H 0.0976 0.9860 1.0674 0.466 Uiso 1 1 calc R U . . .
C29C C 0.1259(10) 1.0074(7) 1.1571(4) 0.130(4) Uani 1 1 d . U . . .
H29A H 0.1462 1.0562 1.1442 0.156 Uiso 1 1 calc R U . . .
H29B H 0.0615 1.0151 1.1650 0.156 Uiso 1 1 calc R U . . .
C1C C 0.1591(9) 1.0071(6) 1.2321(4) 0.076(3) Uani 1 1 d . U . . .
C6C C 0.2226(10) 1.0568(7) 1.2378(4) 0.092(3) Uani 1 1 d . U . . .
C7C C 0.3086(9) 1.0643(6) 1.2099(4) 0.105(4) Uani 1 1 d . U . . .
H7C1 H 0.3184 1.1177 1.2024 0.126 Uiso 1 1 calc R U . . .
H7C2 H 0.3040 1.0449 1.1830 0.126 Uiso 1 1 calc R U . . .
C2C C 0.0867(9) 0.9914(6) 1.2581(4) 0.082(3) Uani 1 1 d . U . . .
C5C C 0.1969(11) 1.0944(8) 1.2735(4) 0.120(4) Uani 1 1 d . U . . .
H5C H 0.2354 1.1275 1.2799 0.144 Uiso 1 1 calc R U . . .
C4C C 0.1198(11) 1.0864(8) 1.2996(5) 0.118(4) Uani 1 1 d . U . . .
H4C H 0.1043 1.1153 1.3216 0.142 Uiso 1 1 calc R U . . .
C3C C 0.0667(10) 1.0340(8) 1.2919(4) 0.110(4) Uani 1 1 d . U . . .
H3C H 0.0149 1.0263 1.3098 0.132 Uiso 1 1 calc R U . . .
O5C O 0.1486(11) 0.8568(10) 1.1405(5) 0.236(6) Uiso 1 1 d . U . . .
O2C O 0.3972(5) 0.9200(4) 1.1956(2) 0.092(2) Uani 1 1 d . U . . .
C8C C 0.3883(9) 1.0186(7) 1.2358(4) 0.090(3) Uani 1 1 d . U . . .
C9C C 0.4248(9) 0.9520(8) 1.2305(4) 0.085(3) Uani 1 1 d . U . . .
C10C C 0.4941(8) 0.9028(8) 1.2570(4) 0.089(3) Uani 1 1 d . U . . .
C14C C 0.5253(7) 0.8251(7) 1.2524(4) 0.088(3) Uani 1 1 d . U . . .
H14A H 0.5897 0.8131 1.2578 0.106 Uiso 1 1 calc R U . . .
H14B H 0.5155 0.8168 1.2231 0.106 Uiso 1 1 calc R U . . .
C31C C 0.4609(11) 0.9233(8) 1.1601(4) 0.132(5) Uani 1 1 d D U . . .
H31G H 0.4722 0.9759 1.1504 0.158 Uiso 1 1 calc R U . . .
H31H H 0.5178 0.8937 1.1698 0.158 Uiso 1 1 calc R U . . .
C13C C 0.4237(11) 1.0507(9) 1.2707(5) 0.127(4) Uani 1 1 d . U . . .
H13C H 0.3993 1.0984 1.2768 0.152 Uiso 1 1 calc R U . . .
C12C C 0.4983(11) 1.0055(10) 1.2956(5) 0.131(5) Uani 1 1 d . U . . .
H12C H 0.5279 1.0249 1.3159 0.157 Uiso 1 1 calc R U . . .
C11C C 0.5198(10) 0.9405(9) 1.2882(5) 0.123(5) Uani 1 1 d . U . . .
H11C H 0.5615 0.9110 1.3074 0.147 Uiso 1 1 calc R U . . .
O7C O 0.3154(12) 0.9315(9) 1.1188(3) 0.246(4) Uani 1 1 d D U . . .
O8C O 0.4676(8) 0.9580(7) 1.0850(4) 0.192(5) Uiso 1 1 d D U . . .
C32C C 0.432(2) 0.8954(16) 1.1254(7) 0.265(10) Uiso 1 1 d D U . . .
O3C O 0.3685(5) 0.7549(4) 1.2329(2) 0.0796(19) Uani 1 1 d . U . . .
C15C C 0.4689(9) 0.7750(7) 1.2870(4) 0.088(3) Uani 1 1 d . U . . .
C16C C 0.3909(9) 0.7420(6) 1.2794(4) 0.073(3) Uani 1 1 d . U . . .
C33C C 0.4096(9) 0.6902(7) 1.2156(4) 0.110(4) Uani 1 1 d . U . . .
H33C H 0.4750 0.6911 1.2137 0.132 Uiso 1 1 calc R U . . .
H33D H 0.3973 0.6447 1.2361 0.132 Uiso 1 1 calc R U . . .
C21C C 0.2456(9) 0.6854(6) 1.2994(3) 0.087(3) Uani 1 1 d . U . . .
H21A H 0.2457 0.6811 1.2687 0.105 Uiso 1 1 calc R U . . .
H21B H 0.2364 0.6360 1.3168 0.105 Uiso 1 1 calc R U . . .
C17C C 0.3383(10) 0.7070(7) 1.3095(4) 0.090(3) Uani 1 1 d . U . . .
C18C C 0.3640(10) 0.6932(6) 1.3541(4) 0.091(4) Uani 1 1 d . U . . .
H18C H 0.3257 0.6699 1.3759 0.109 Uiso 1 1 calc R U . . .
C19C C 0.4414(11) 0.7130(8) 1.3652(5) 0.119(5) Uani 1 1 d . U . . .
H19C H 0.4605 0.7003 1.3938 0.143 Uiso 1 1 calc R U . . .
C20C C 0.4913(10) 0.7524(7) 1.3328(4) 0.104(4) Uani 1 1 d . U . . .
H20C H 0.5453 0.7665 1.3408 0.125 Uiso 1 1 calc R U . . .
O9C O 0.3869(9) 0.7667(9) 1.1490(4) 0.218(4) Uani 1 1 d . U . . .
O10C O 0.4252(13) 0.6393(11) 1.1543(4) 0.367(14) Uani 1 1 d . U . . .
H10C H 0.4030 0.6449 1.1302 0.550 Uiso 1 1 calc R U . . .
C34C C 0.3826(19) 0.6841(17) 1.1759(10) 0.224(9) Uiso 1 1 d . U . . .
O4C O 0.1507(5) 0.7969(4) 1.2338(2) 0.0816(19) Uani 1 1 d . U . . .
C28C C 0.0319(8) 0.9292(7) 1.2555(3) 0.086(3) Uani 1 1 d . U . . .
H28A H 0.0389 0.9166 1.2263 0.103 Uiso 1 1 calc R U . . .
H28B H -0.0319 0.9461 1.2612 0.103 Uiso 1 1 calc R U . . .
C24C C 0.0626(9) 0.8585(7) 1.2891(3) 0.079(3) Uani 1 1 d . U . . .
C25C C 0.0351(9) 0.8592(7) 1.3332(3) 0.092(3) Uani 1 1 d . U . . .
H25C H -0.0076 0.8971 1.3418 0.110 Uiso 1 1 calc R U . . .
C26C C 0.0758(10) 0.7998(8) 1.3630(4) 0.098(4) Uani 1 1 d . U . . .
H26C H 0.0566 0.7983 1.3923 0.117 Uiso 1 1 calc R U . . .
C27C C 0.1394(10) 0.7445(8) 1.3544(4) 0.093(4) Uani 1 1 d . U . . .
H27C H 0.1645 0.7070 1.3766 0.111 Uiso 1 1 calc R U . . .
C22C C 0.1674(8) 0.7453(7) 1.3098(4) 0.081(3) Uani 1 1 d . U . . .
C23C C 0.1255(9) 0.8036(7) 1.2789(4) 0.077(3) Uani 1 1 d . U . . .
C35C C 0.0900(10) 0.7573(8) 1.2170(3) 0.122(4) Uani 1 1 d . U . . .
H35A H 0.0298 0.7860 1.2158 0.146 Uiso 1 1 calc R U . . .
H35B H 0.0863 0.7078 1.2353 0.146 Uiso 1 1 calc R U . . .
O11C O 0.2364(12) 0.7155(7) 1.1679(3) 0.206(3) Uani 1 1 d . U . . .
O12C O 0.0682(11) 0.7084(10) 1.1565(4) 0.297(9) Uani 1 1 d . U . . .
H12E H 0.0861 0.6999 1.1321 0.445 Uiso 1 1 calc R U . . .
C36C C 0.1266(18) 0.7481(16) 1.1716(6) 0.234(7) Uani 1 1 d . U . . .
O1D O 0.3138(8) 0.8764(6) 0.9404(3) 0.151(3) Uani 1 1 d . U . . .
C7D C 0.4795(11) 0.8572(9) 0.8977(4) 0.134(4) Uani 1 1 d . U . . .
H7D1 H 0.5286 0.8868 0.8860 0.161 Uiso 1 1 calc R U . . .
H7D2 H 0.4692 0.8620 0.9283 0.161 Uiso 1 1 calc R U . . .
C6D C 0.3927(13) 0.8943(8) 0.8734(4) 0.117(4) Uani 1 1 d . U . . .
C1D C 0.3128(14) 0.8943(10) 0.8955(5) 0.136(5) Uani 1 1 d . U . . .
C2D C 0.2461(15) 0.9209(10) 0.8722(5) 0.150(5) Uani 1 1 d . U . . .
C5D C 0.4011(12) 0.9217(7) 0.8277(4) 0.123(5) Uani 1 1 d . U . . .
H5D H 0.4575 0.9193 0.8127 0.147 Uiso 1 1 calc R U . . .
C4D C 0.3246(14) 0.9513(9) 0.8069(5) 0.132(5) Uani 1 1 d . U . . .
H4D H 0.3278 0.9744 0.7776 0.158 Uiso 1 1 calc R U . . .
C3D C 0.2484(14) 0.9477(10) 0.8272(5) 0.147(6) Uani 1 1 d . U . . .
H3D H 0.1948 0.9627 0.8123 0.176 Uiso 1 1 calc R U . . .
C29D C 0.3246(16) 0.9447(11) 0.9572(5) 0.212(5) Uani 1 1 d . U . . .
H29G H 0.3602 0.9747 0.9348 0.254 Uiso 1 1 calc R U . . .
H29H H 0.2644 0.9732 0.9580 0.254 Uiso 1 1 calc R U . . .
O6D O 0.319(3) 0.9850(13) 1.0219(6) 0.57(2) Uani 1 1 d D U . . .
H6D H 0.3482 0.9792 1.0441 0.860 Uiso 1 1 calc R U . . .
O5D O 0.3600(12) 0.8668(10) 1.0200(4) 0.247(4) Uani 1 1 d D U . . .
C30D C 0.361(2) 0.9464(17) 0.9957(9) 0.279(8) Uani 1 1 d . U . . .
C14D C 0.4728(14) 0.5867(11) 0.9605(5) 0.179(6) Uani 1 1 d . U . . .
H14G H 0.4636 0.6043 0.9885 0.214 Uiso 1 1 calc R U . . .
H14H H 0.5216 0.5447 0.9638 0.214 Uiso 1 1 calc R U . . .
C10D C 0.5048(11) 0.6485(11) 0.9286(4) 0.127(4) Uani 1 1 d . U . . .
C9D C 0.4843(11) 0.7275(11) 0.9282(5) 0.126(4) Uani 1 1 d . U . . .
C8D C 0.5095(11) 0.7796(10) 0.8957(5) 0.117(4) Uani 1 1 d . U . . .
C11D C 0.5602(12) 0.6196(10) 0.8901(4) 0.149(5) Uani 1 1 d . U . . .
H11D H 0.5772 0.5682 0.8886 0.178 Uiso 1 1 calc R U . . .
C12D C 0.5813(11) 0.6782(11) 0.8586(5) 0.145(5) Uani 1 1 d . U . . .
H12D H 0.6189 0.6649 0.8353 0.174 Uiso 1 1 calc R U . . .
C13D C 0.5534(11) 0.7564(10) 0.8569(5) 0.138(5) Uani 1 1 d . U . . .
H13D H 0.5630 0.7918 0.8316 0.165 Uiso 1 1 calc R U . . .
O2D O 0.4520(8) 0.7419(7) 0.9686(3) 0.164(3) Uani 1 1 d . U . . .
C31D C 0.5032(14) 0.7495(14) 0.9955(6) 0.249(5) Uani 1 1 d D U . . .
H31E H 0.5276 0.7978 0.9863 0.299 Uiso 1 1 calc R U . . .
H31F H 0.5537 0.7090 0.9967 0.299 Uiso 1 1 calc R U . . .
C32D C 0.452(2) 0.7475(19) 1.0486(11) 0.436(14) Uiso 1 1 d G U . . .
O7D O 0.3545(14) 0.6988(10) 1.0618(3) 0.267(4) Uani 1 1 d DG U . . .
O8D O 0.463(3) 0.822(3) 1.0796(13) 0.78(3) Uiso 1 1 d DG U . . .
H8D H 0.4198 0.8248 1.0974 1.171 Uiso 1 1 calc R U . . .
C21D C 0.1333(15) 0.6272(12) 0.9565(6) 0.195(6) Uani 1 1 d . U . . .
H21G H 0.1332 0.6396 0.9857 0.234 Uiso 1 1 calc R U . . .
H21H H 0.0857 0.5951 0.9561 0.234 Uiso 1 1 calc R U . . .
C17D C 0.2200(19) 0.5871(12) 0.9460(5) 0.184(5) Uani 1 1 d D U . . .
C16D C 0.3058(18) 0.5928(11) 0.9627(6) 0.165(5) Uani 1 1 d D U . . .
C15D C 0.3895(17) 0.5558(13) 0.9525(6) 0.175(6) Uani 1 1 d D U . . .
C18D C 0.2351(14) 0.5251(11) 0.9186(6) 0.199(6) Uani 1 1 d D U . . .
H18D H 0.1835 0.5135 0.9070 0.238 Uiso 1 1 calc R U . . .
C19D C 0.3154(17) 0.4834(11) 0.9086(6) 0.201(7) Uani 1 1 d D U . . .
H19D H 0.3158 0.4442 0.8925 0.241 Uiso 1 1 calc R U . . .
C20D C 0.4026(15) 0.5014(11) 0.9237(6) 0.193(6) Uani 1 1 d D U . . .
H20D H 0.4596 0.4792 0.9152 0.232 Uiso 1 1 calc R U . . .
O3D O 0.2964(9) 0.6407(7) 0.9941(3) 0.186(3) Uani 1 1 d . U . . .
C33D C 0.2712(19) 0.6058(14) 1.0373(5) 0.273(9) Uani 1 1 d D U . . .
H33G H 0.3279 0.5733 1.0442 0.328 Uiso 1 1 d R U . . .
H33H H 0.2226 0.5737 1.0400 0.328 Uiso 1 1 d R U . . .
O10D O 0.242(3) 0.664(3) 1.1120(12) 0.67(2) Uiso 1 1 d D U . . .
C34D C 0.235(3) 0.6601(18) 1.0692(11) 0.400(12) Uiso 1 1 d D U . . .
O9D O 0.1847(12) 0.7258(9) 1.0563(3) 0.239(4) Uani 1 1 d D U . . .
O11D O 0.1940(13) 0.8900(9) 1.0194(3) 0.230(4) Uani 1 1 d D U . . .
C28D C 0.1520(13) 0.9099(11) 0.8933(5) 0.166(5) Uani 1 1 d . U . . .
H28G H 0.1082 0.9499 0.8787 0.199 Uiso 1 1 calc R U . . .
H28H H 0.1520 0.9164 0.9237 0.199 Uiso 1 1 calc R U . . .
C24D C 0.1190(13) 0.8303(14) 0.8920(5) 0.169(5) Uani 1 1 d D U . . .
C23D C 0.1373(14) 0.7798(14) 0.9236(6) 0.177(5) Uani 1 1 d . U . . .
O4D O 0.1556(8) 0.7791(8) 0.9648(3) 0.179(3) Uani 1 1 d . U . . .
C25D C 0.0869(14) 0.8335(12) 0.8491(5) 0.187(7) Uani 1 1 d D U . . .
H25D H 0.0759 0.8772 0.8280 0.224 Uiso 1 1 calc R U . . .
C35D C 0.1008(14) 0.8212(14) 0.9858(6) 0.234(5) Uani 1 1 d D U . . .
H35G H 0.0581 0.7868 0.9999 0.281 Uiso 1 1 calc R U . . .
H35H H 0.0674 0.8553 0.9627 0.281 Uiso 1 1 calc R U . . .
C22D C 0.1152(15) 0.7008(16) 0.9229(6) 0.203(6) Uani 1 1 d D U . . .
C26D C 0.0752(16) 0.7590(12) 0.8446(6) 0.207(8) Uani 1 1 d D U . . .
H26D H 0.0541 0.7501 0.8186 0.249 Uiso 1 1 calc R U . . .
C27D C 0.0957(19) 0.6960(12) 0.8800(6) 0.272(9) Uani 1 1 d D U . . .
H27D H 0.0959 0.6471 0.8737 0.327 Uiso 1 1 calc R U . . .
O12D O 0.040(3) 0.887(4) 1.0546(16) 0.94(4) Uiso 1 1 d D U . . .
C36D C 0.1075(18) 0.8755(17) 1.0218(9) 0.294(11) Uiso 1 1 d D U . . .
O1W O 0.4575(11) 0.5437(9) 0.4565(5) 0.111(5) Uiso 0.5 1 d . . P . .
H1W H 0.4723 0.5972 0.4495 0.166 Uiso 0.5 1 d R U P . .
H2W H 0.3906 0.5438 0.4565 0.166 Uiso 0.5 1 d R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Na6 O1D 2.250(12) . ?
Na6 O4D 2.296(13) . ?
Na6 O5D 2.317(16) . ?
Na6 O3D 2.386(14) . ?
Na6 O2D 2.417(13) . ?
Na6 O7D 2.458(13) . ?
Na6 O11D 2.625(16) . ?
Na6 O9D 2.586(15) . ?
Na6 C32D 2.91(4) . ?
Na6 C35D 2.92(2) . ?
Na6 C34D 3.01(4) . ?
Na6 C31D 3.05(2) . ?
Na1 O7A 2.274(7) . ?
Na1 O4A 2.348(6) . ?
Na1 O11A 2.375(7) . ?
Na1 O2A 2.390(8) . ?
Na1 O3A 2.423(7) . ?
Na1 O9A 2.455(9) . ?
Na1 O1A 2.458(8) . ?
Na1 C36A 3.079(13) . ?
Na1 Na2 3.217(5) . ?
Na4 O4C 2.371(9) . ?
Na4 O3C 2.372(8) . ?
Na4 O5C 2.387(15) . ?
Na4 O1C 2.435(9) . ?
Na4 O2C 2.453(9) . ?
Na4 O7C 2.499(12) . ?
Na4 O9C 2.520(12) . ?
Na4 O11C 2.691(12) . ?
Na4 C30C 2.946(17) . ?
Na4 C32C 3.10(3) . ?
Na4 Na5 3.218(7) . ?
Na2 O5B 2.300(8) . ?
Na2 O7A 2.342(9) . ?
Na2 O7B 2.372(8) . ?
Na2 O9A 2.391(8) . ?
Na2 O9B 2.429(8) . ?
Na2 O11A 2.416(7) . ?
Na2 Na3 3.275(5) . ?
Na3 O3B 2.317(7) . ?
Na3 O5B 2.336(9) . ?
Na3 O9B 2.396(6) . ?
Na3 O4B 2.407(7) . ?
Na3 O2B 2.420(7) . ?
Na3 O1B 2.438(6) . ?
Na3 O7B 2.584(7) . ?
Na3 C34B 3.071(11) . ?
Na5 O5C 2.463(17) . ?
Na5 O7D 2.504(18) . ?
Na5 O9C 2.527(15) . ?
Na5 O5D 2.585(17) . ?
Na5 O9D 2.540(18) . ?
Na5 O11D 2.635(16) . ?
Na5 O7C 2.627(18) . ?
Na5 O11C 2.753(16) . ?
Na5 O10D 2.69(5) . ?
Na5 O8D 2.87(4) . ?
Na5 C32D 3.08(3) . ?
Na5 C30C 3.09(2) . ?
O1A C1A 1.413(12) . ?
O1A C29A 1.477(12) . ?
C2A C1A 1.332(13) . ?
C2A C3A 1.408(15) . ?
C2A C28A 1.494(14) . ?
C1A C6A 1.284(14) . ?
C6A C5A 1.391(15) . ?
C6A C7A 1.547(15) . ?
C7A C8A 1.442(16) . ?
C7A H7A1 0.9700 . ?
C7A H7A2 0.9700 . ?
C29A C30A 1.51(2) . ?
C29A H29C 0.9700 . ?
C29A H29D 0.9700 . ?
C3A C4A 1.310(15) . ?
C3A H3A 0.9300 . ?
C4A C5A 1.375(14) . ?
C4A H4A 0.9300 . ?
C5A H5A 0.9300 . ?
O6A C30A 1.40(2) . ?
O6A H6A 0.8200 . ?
O5A C30A 1.06(3) . ?
O2A C9A 1.422(14) . ?
O2A C31A 1.461(11) . ?
O7A C32A 1.250(12) . ?
C8A C13A 1.428(18) . ?
C8A C9A 1.449(17) . ?
C9A C10A 1.359(17) . ?
C31A C32A 1.364(15) . ?
C31A H31A 0.9700 . ?
C31A H31B 0.9700 . ?
C32A O8A 1.251(11) . ?
C14A C10A 1.510(17) . ?
C14A C15A 1.538(16) . ?
C14A H14C 0.9700 . ?
C14A H14D 0.9700 . ?
C10A C11A 1.380(17) . ?
C13A C12A 1.432(19) . ?
C13A H13A 0.9300 . ?
C12A C11A 1.296(18) . ?
C12A H12A 0.9300 . ?
C11A H11A 0.9300 . ?
O3A C16A 1.411(12) . ?
O3A C33A 1.477(12) . ?
O10A C34A 1.222(12) . ?
O10A H10A 0.8200 . ?
C21A C22A 1.428(14) . ?
C21A C17A 1.559(15) . ?
C21A H21C 0.9700 . ?
C21A H21D 0.9700 . ?
C17A C18A 1.370(16) . ?
C17A C16A 1.377(14) . ?
C18A C19A 1.276(17) . ?
C18A H18A 0.9300 . ?
C19A C20A 1.284(16) . ?
C19A H19A 0.9300 . ?
C20A C15A 1.383(17) . ?
C20A H20A 0.9300 . ?
C15A C16A 1.348(15) . ?
C33A C34A 1.497(15) . ?
C33A H33E 0.9700 . ?
C33A H33F 0.9700 . ?
C34A O9A 1.198(12) . ?
O11A C36A 1.209(10) . ?
O4A C23A 1.372(11) . ?
O4A C35A 1.442(11) . ?
O12A C36A 1.314(12) . ?
O12A H12' 0.8200 . ?
C36A C35A 1.475(13) . ?
C35A H35C 0.9700 . ?
C35A H35D 0.9700 . ?
C23A C24A 1.298(13) . ?
C23A C22A 1.430(13) . ?
C24A C28A 1.474(13) . ?
C24A C25A 1.531(14) . ?
C28A H28C 0.9700 . ?
C28A H28D 0.9700 . ?
C22A C27A 1.404(14) . ?
C25A C26A 1.444(16) . ?
C25A H25A 0.9300 . ?
C26A C27A 1.325(15) . ?
C26A H26A 0.9300 . ?
C27A H27A 0.9300 . ?
O1B C1B 1.378(10) . ?
O1B C29B 1.397(11) . ?
C5B C4B 1.292(12) . ?
C5B C6B 1.412(11) . ?
C5B H5B 0.9300 . ?
C7B C8B 1.501(13) . ?
C7B C6B 1.563(12) . ?
C7B H7B1 0.9700 . ?
C7B H7B2 0.9700 . ?
C6B C1B 1.383(12) . ?
C1B C2B 1.431(12) . ?
C29B C30B 1.498(14) . ?
C29B H29E 0.9700 . ?
C29B H29F 0.9700 . ?
C30B O5B 1.255(13) . ?
C30B O6B 1.283(13) . ?
O6B H6B 0.8200 . ?
C4B C3B 1.474(13) . ?
C4B H4B 0.9300 . ?
C3B C2B 1.373(11) . ?
C3B H3B 0.9300 . ?
C2B C28B 1.545(12) . ?
O2B C9B 1.388(11) . ?
O2B C31B 1.449(10) . ?
O7B C32B 1.255(10) . ?
O8B C32B 1.251(10) . ?
C14B C15B 1.508(13) . ?
C14B C10B 1.517(12) . ?
C14B H14E 0.9700 . ?
C14B H14F 0.9700 . ?
C10B C9B 1.396(13) . ?
C10B C11B 1.420(13) . ?
C9B C8B 1.369(12) . ?
C8B C13B 1.348(12) . ?
C11B C12B 1.349(12) . ?
C11B H11B 0.9300 . ?
C12B C13B 1.453(14) . ?
C12B H12B 0.9300 . ?
C13B H13B 0.9300 . ?
C31B C32B 1.528(13) . ?
C31B H31C 0.9700 . ?
C31B H31D 0.9700 . ?
C33B C34B 1.475(13) . ?
C33B O3B 1.473(9) . ?
C33B H33A 0.9700 . ?
C33B H33B 0.9700 . ?
O3B C16B 1.435(11) . ?
C18B C19B 1.373(14) . ?
C18B C17B 1.457(13) . ?
C18B H18B 0.9300 . ?
O9B C34B 1.224(11) . ?
O10B C34B 1.275(10) . ?
C16B C17B 1.316(12) . ?
C16B C15B 1.370(13) . ?
C15B C20B 1.423(14) . ?
C21B C22B 1.526(11) . ?
C21B C17B 1.535(12) . ?
C21B H21E 0.9700 . ?
C21B H21F 0.9700 . ?
C19B C20B 1.335(13) . ?
C19B H19B 0.9300 . ?
C20B H20B 0.9300 . ?
C25B C26B 1.315(13) . ?
C25B C24B 1.364(13) . ?
C25B H25B 0.9300 . ?
O4B C23B 1.375(10) . ?
O4B C35B 1.448(10) . ?
C28B C24B 1.514(13) . ?
C28B H28E 0.9700 . ?
C28B H28F 0.9700 . ?
C24B C23B 1.421(11) . ?
C23B C22B 1.426(13) . ?
C22B C27B 1.402(12) . ?
C27B C26B 1.371(12) . ?
C27B H27B 0.9300 . ?
C26B H26B 0.9300 . ?
C35B C36B 1.450(17) . ?
C35B H35E 0.9700 . ?
C35B H35F 0.9700 . ?
C36B O12B 1.216(14) . ?
C36B O11B 1.227(16) . ?
O12B H12O 0.8200 . ?
O1C C1C 1.432(13) . ?
O1C C29C 1.466(11) . ?
C30C O5C 1.57(2) . ?
C30C O6C 1.498(19) . ?
C30C C29C 1.64(2) . ?
O6C H6C 0.8200 . ?
C29C H29A 0.9700 . ?
C29C H29B 0.9700 . ?
C1C C2C 1.329(15) . ?
C1C C6C 1.419(15) . ?
C6C C5C 1.402(16) . ?
C6C C7C 1.500(16) . ?
C7C C8C 1.531(16) . ?
C7C H7C1 0.9700 . ?
C7C H7C2 0.9700 . ?
C2C C3C 1.398(15) . ?
C2C C28C 1.479(15) . ?
C5C C4C 1.366(17) . ?
C5C H5C 0.9300 . ?
C4C C3C 1.362(17) . ?
C4C H4C 0.9300 . ?
C3C H3C 0.9300 . ?
O2C C31C 1.400(13) . ?
O2C C9C 1.418(13) . ?
C8C C9C 1.277(15) . ?
C8C C13C 1.469(16) . ?
C9C C10C 1.457(16) . ?
C10C C11C 1.374(16) . ?
C10C C14C 1.437(15) . ?
C14C C15C 1.546(15) . ?
C14C H14A 0.9700 . ?
C14C H14B 0.9700 . ?
C31C C32C 1.381(10) . ?
C31C H31G 0.9700 . ?
C31C H31H 0.9700 . ?
C13C C12C 1.460(19) . ?
C13C H13C 0.9300 . ?
C12C C11C 1.224(17) . ?
C12C H12C 0.9300 . ?
C11C H11C 0.9300 . ?
O7C C32C 1.77(3) . ?
O8C C32C 1.64(3) . ?
O3C C33C 1.414(12) . ?
O3C C16C 1.473(11) . ?
C15C C16C 1.417(15) . ?
C15C C20C 1.454(14) . ?
C16C C17C 1.302(15) . ?
C33C C34C 1.35(3) . ?
C33C H33C 0.9700 . ?
C33C H33D 0.9700 . ?
C21C C22C 1.533(15) . ?
C21C C17C 1.542(15) . ?
C21C H21A 0.9700 . ?
C21C H21B 0.9700 . ?
C17C C18C 1.428(14) . ?
C18C C19C 1.327(16) . ?
C18C H18C 0.9300 . ?
C19C C20C 1.357(17) . ?
C19C H19C 0.9300 . ?
C20C H20C 0.9300 . ?
O9C C34C 1.57(3) . ?
O10C C34C 1.22(3) . ?
O10C H10C 0.8200 . ?
O4C C35C 1.395(11) . ?
O4C C23C 1.447(12) . ?
C28C C24C 1.528(14) . ?
C28C H28A 0.9700 . ?
C28C H28B 0.9700 . ?
C24C C23C 1.331(14) . ?
C24C C25C 1.403(14) . ?
C25C C26C 1.380(15) . ?
C25C H25C 0.9300 . ?
C26C C27C 1.326(16) . ?
C26C H26C 0.9300 . ?
C27C C22C 1.417(14) . ?
C27C H27C 0.9300 . ?
C22C C23C 1.393(14) . ?
C35C C36C 1.50(2) . ?
C35C H35A 0.9700 . ?
C35C H35B 0.9700 . ?
O11C C36C 1.66(3) . ?
O12C C36C 1.345(19) . ?
O12C H12E 0.8200 . ?
O1D C1D 1.373(14) . ?
O1D C29D 1.444(17) . ?
C7D C8D 1.415(17) . ?
C7D C6D 1.545(18) . ?
C7D H7D1 0.9700 . ?
C7D H7D2 0.9700 . ?
C6D C1D 1.33(2) . ?
C6D C5D 1.417(16) . ?
C1D C2D 1.25(2) . ?
C2D C3D 1.392(18) . ?
C2D C28D 1.53(2) . ?
C5D C4D 1.342(19) . ?
C5D H5D 0.9300 . ?
C4D C3D 1.26(2) . ?
C4D H4D 0.9300 . ?
C3D H3D 0.9300 . ?
C29D C30D 1.35(2) . ?
C29D H29G 0.9700 . ?
C29D H29H 0.9700 . ?
O6D C30D 1.24(3) . ?
O6D H6D 0.8200 . ?
O5D C30D 1.49(3) . ?
C14D C10D 1.452(19) . ?
C14D C15D 1.47(2) . ?
C14D H14G 0.9700 . ?
C14D H14H 0.9700 . ?
C10D C9D 1.406(19) . ?
C10D C11D 1.53(2) . ?
C9D C8D 1.316(18) . ?
C9D O2D 1.366(16) . ?
C8D C13D 1.434(18) . ?
C11D C12D 1.354(18) . ?
C11D H11D 0.9300 . ?
C12D C13D 1.400(19) . ?
C12D H12D 0.9300 . ?
C13D H13D 0.9300 . ?
O2D C31D 1.201(15) . ?
C31D C32D 1.76(3) . ?
C31D H31E 0.9700 . ?
C31D H31F 0.9700 . ?
C32D O7D 1.772(17) . ?
C32D O8D 1.805(17) . ?
O8D H8D 0.8200 . ?
C21D C17D 1.44(3) . ?
C21D C22D 1.53(3) . ?
C21D H21G 0.9700 . ?
C21D H21H 0.9700 . ?
C17D C16D 1.43(3) . ?
C17D C18D 1.501(16) . ?
C16D C15D 1.375(16) . ?
C16D O3D 1.40(2) . ?
C15D C20D 1.42(2) . ?
C18D C19D 1.370(16) . ?
C18D H18D 0.9300 . ?
C19D C20D 1.50(2) . ?
C19D H19D 0.9300 . ?
C20D H20D 0.9300 . ?
O3D C33D 1.422(16) . ?
C33D C34D 1.536(17) . ?
C33D H33G 0.9700 . ?
C33D H33H 0.9700 . ?
O10D C34D 1.355(19) . ?
C34D O9D 1.317(18) . ?
O11D C36D 1.338(17) . ?
C28D C24D 1.57(2) . ?
C28D H28G 0.9700 . ?
C28D H28H 0.9700 . ?
C24D C23D 1.23(2) . ?
C24D C25D 1.432(15) . ?
C23D O4D 1.321(17) . ?
C23D C22D 1.50(3) . ?
O4D C35D 1.265(19) . ?
C25D C26D 1.401(16) . ?
C25D H25D 0.9300 . ?
C35D C36D 1.622(17) . ?
C35D H35G 0.9700 . ?
C35D H35H 0.9700 . ?
C22D C27D 1.400(15) . ?
C26D C27D 1.442(15) . ?
C26D H26D 0.9300 . ?
C27D H27D 0.9300 . ?
O12D C36D 1.399(18) . ?
O1W H1W 0.9929 . ?
O1W H2W 0.9929 . ?

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
_geom_angle_publ_flag
O1D Na6 O4D 85.3(5) . . ?
O1D Na6 O5D 68.6(5) . . ?
O4D Na6 O5D 130.1(6) . . ?
O1D Na6 O3D 135.1(4) . . ?
O4D Na6 O3D 81.9(5) . . ?
O5D Na6 O3D 145.8(6) . . ?
O1D Na6 O2D 79.7(4) . . ?
O4D Na6 O2D 135.9(4) . . ?
O5D Na6 O2D 81.7(6) . . ?
O3D Na6 O2D 80.3(5) . . ?
O1D Na6 O7D 144.7(7) . . ?
O4D Na6 O7D 128.4(7) . . ?
O5D Na6 O7D 79.7(6) . . ?
O3D Na6 O7D 68.8(5) . . ?
O2D Na6 O7D 80.8(5) . . ?
O1D Na6 O11D 74.3(4) . . ?
O4D Na6 O11D 73.7(5) . . ?
O5D Na6 O11D 58.9(6) . . ?
O3D Na6 O11D 140.1(6) . . ?
O2D Na6 O11D 138.5(6) . . ?
O7D Na6 O11D 102.7(5) . . ?
O1D Na6 O9D 141.3(6) . . ?
O4D Na6 O9D 71.7(5) . . ?
O5D Na6 O9D 102.9(5) . . ?
O3D Na6 O9D 73.0(5) . . ?
O2D Na6 O9D 138.1(5) . . ?
O7D Na6 O9D 59.7(6) . . ?
O11D Na6 O9D 69.6(5) . . ?
O1D Na6 C32D 108.2(7) . . ?
O4D Na6 C32D 165.3(7) . . ?
O5D Na6 C32D 54.0(7) . . ?
O3D Na6 C32D 92.0(7) . . ?
O2D Na6 C32D 55.0(5) . . ?
O7D Na6 C32D 37.3(6) . . ?
O11D Na6 C32D 103.8(6) . . ?
O9D Na6 C32D 93.8(6) . . ?
O1D Na6 C35D 86.1(6) . . ?
O4D Na6 C35D 24.5(4) . . ?
O5D Na6 C35D 108.8(7) . . ?
O3D Na6 C35D 98.5(6) . . ?
O2D Na6 C35D 157.8(5) . . ?
O7D Na6 C35D 119.7(7) . . ?
O11D Na6 C35D 50.3(6) . . ?
O9D Na6 C35D 60.2(6) . . ?
C32D Na6 C35D 146.9(6) . . ?
O1D Na6 C34D 167.0(7) . . ?
O4D Na6 C34D 87.6(9) . . ?
O5D Na6 C34D 108.6(8) . . ?
O3D Na6 C34D 54.0(6) . . ?
O2D Na6 C34D 112.8(7) . . ?
O7D Na6 C34D 40.8(8) . . ?
O11D Na6 C34D 93.3(6) . . ?
O9D Na6 C34D 25.8(6) . . ?
C32D Na6 C34D 78.1(9) . . ?
C35D Na6 C34D 82.9(9) . . ?
O1D Na6 C31D 86.5(6) . . ?
O4D Na6 C31D 157.5(5) . . ?
O5D Na6 C31D 64.9(6) . . ?
O3D Na6 C31D 89.3(6) . . ?
O2D Na6 C31D 21.6(3) . . ?
O7D Na6 C31D 65.7(7) . . ?
O11D Na6 C31D 123.8(7) . . ?
O9D Na6 C31D 125.4(5) . . ?
C32D Na6 C31D 34.3(5) . . ?
C35D Na6 C31D 171.7(7) . . ?
C34D Na6 C31D 104.0(9) . . ?
O7A Na1 O4A 156.3(3) . . ?
O7A Na1 O11A 89.2(3) . . ?
O4A Na1 O11A 69.0(2) . . ?
O7A Na1 O2A 66.8(3) . . ?
O4A Na1 O2A 136.9(3) . . ?
O11A Na1 O2A 147.3(3) . . ?
O7A Na1 O3A 103.5(3) . . ?
O4A Na1 O3A 84.1(2) . . ?
O11A Na1 O3A 127.9(3) . . ?
O2A Na1 O3A 81.1(3) . . ?
O7A Na1 O9A 75.7(3) . . ?
O4A Na1 O9A 87.9(3) . . ?
O11A Na1 O9A 70.4(3) . . ?
O2A Na1 O9A 120.6(3) . . ?
O3A Na1 O9A 64.6(3) . . ?
O7A Na1 O1A 104.7(3) . . ?
O4A Na1 O1A 82.5(2) . . ?
O11A Na1 O1A 83.3(3) . . ?
O2A Na1 O1A 81.9(3) . . ?
O3A Na1 O1A 137.8(3) . . ?
O9A Na1 O1A 153.7(3) . . ?
O7A Na1 C36A 106.8(3) . . ?
O4A Na1 C36A 50.0(3) . . ?
O11A Na1 C36A 20.9(2) . . ?
O2A Na1 C36A 167.5(3) . . ?
O3A Na1 C36A 111.2(3) . . ?
O9A Na1 C36A 65.6(3) . . ?
O1A Na1 C36A 89.8(3) . . ?
O7A Na1 Na2 46.7(2) . . ?
O4A Na1 Na2 109.7(2) . . ?
O11A Na1 Na2 48.36(18) . . ?
O2A Na1 Na2 113.4(2) . . ?
O3A Na1 Na2 108.7(2) . . ?
O9A Na1 Na2 47.54(19) . . ?
O1A Na1 Na2 113.5(2) . . ?
C36A Na1 Na2 61.6(2) . . ?
O4C Na4 O3C 85.6(3) . . ?
O4C Na4 O5C 75.0(4) . . ?
O3C Na4 O5C 139.8(5) . . ?
O4C Na4 O1C 83.0(3) . . ?
O3C Na4 O1C 137.4(3) . . ?
O5C Na4 O1C 75.4(4) . . ?
O4C Na4 O2C 137.8(3) . . ?
O3C Na4 O2C 78.4(3) . . ?
O5C Na4 O2C 138.0(5) . . ?
O1C Na4 O2C 83.1(3) . . ?
O4C Na4 O7C 147.2(5) . . ?
O3C Na4 O7C 126.0(5) . . ?
O5C Na4 O7C 74.2(5) . . ?
O1C Na4 O7C 78.4(4) . . ?
O2C Na4 O7C 66.2(4) . . ?
O4C Na4 O9C 122.1(5) . . ?
O3C Na4 O9C 63.4(4) . . ?
O5C Na4 O9C 97.7(5) . . ?
O1C Na4 O9C 151.9(4) . . ?
O2C Na4 O9C 84.7(4) . . ?
O7C Na4 O9C 73.6(5) . . ?
O4C Na4 O11C 68.4(4) . . ?
O3C Na4 O11C 76.1(4) . . ?
O5C Na4 O11C 64.1(5) . . ?
O1C Na4 O11C 134.8(4) . . ?
O2C Na4 O11C 141.1(5) . . ?
O7C Na4 O11C 107.4(4) . . ?
O9C Na4 O11C 57.7(5) . . ?
O4C Na4 C30C 94.5(5) . . ?
O3C Na4 C30C 170.2(5) . . ?
O5C Na4 C30C 32.1(5) . . ?
O1C Na4 C30C 52.1(4) . . ?
O2C Na4 C30C 107.6(5) . . ?
O7C Na4 C30C 52.9(5) . . ?
O9C Na4 C30C 108.8(5) . . ?
O11C Na4 C30C 94.8(6) . . ?
O4C Na4 C32C 172.5(5) . . ?
O3C Na4 C32C 91.2(6) . . ?
O5C Na4 C32C 103.5(6) . . ?
O1C Na4 C32C 103.9(6) . . ?
O2C Na4 C32C 47.4(4) . . ?
O7C Na4 C32C 34.9(6) . . ?
O9C Na4 C32C 50.5(6) . . ?
O11C Na4 C32C 104.3(6) . . ?
C30C Na4 C32C 87.6(7) . . ?
O4C Na4 Na5 111.9(3) . . ?
O3C Na4 Na5 110.9(3) . . ?
O5C Na4 Na5 49.5(4) . . ?
O1C Na4 Na5 111.5(3) . . ?
O2C Na4 Na5 110.3(3) . . ?
O7C Na4 Na5 52.9(4) . . ?
O9C Na4 Na5 50.5(3) . . ?
O11C Na4 Na5 54.7(3) . . ?
C30C Na4 Na5 60.0(4) . . ?
C32C Na4 Na5 63.0(4) . . ?
O5B Na2 O7A 89.9(3) . . ?
O5B Na2 O7B 74.5(3) . . ?
O7A Na2 O7B 162.1(3) . . ?
O5B Na2 O9A 164.2(4) . . ?
O7A Na2 O9A 75.8(3) . . ?
O7B Na2 O9A 120.6(3) . . ?
O5B Na2 O9B 88.4(3) . . ?
O7A Na2 O9B 116.9(3) . . ?
O7B Na2 O9B 72.2(3) . . ?
O9A Na2 O9B 92.2(3) . . ?
O5B Na2 O11A 115.7(3) . . ?
O7A Na2 O11A 86.6(3) . . ?
O7B Na2 O11A 92.1(3) . . ?
O9A Na2 O11A 70.8(2) . . ?
O9B Na2 O11A 147.2(3) . . ?
O5B Na2 Na1 123.2(3) . . ?
O7A Na2 Na1 44.94(19) . . ?
O7B Na2 Na1 139.0(2) . . ?
O9A Na2 Na1 49.3(2) . . ?
O9B Na2 Na1 137.1(2) . . ?
O11A Na2 Na1 47.27(18) . . ?
O5B Na2 Na3 45.5(2) . . ?
O7A Na2 Na3 122.1(2) . . ?
O7B Na2 Na3 51.49(17) . . ?
O9A Na2 Na3 138.8(2) . . ?
O9B Na2 Na3 46.84(16) . . ?
O11A Na2 Na3 139.7(2) . . ?
Na1 Na2 Na3 166.47(16) . . ?
O3B Na3 O5B 152.6(3) . . ?
O3B Na3 O9B 70.8(2) . . ?
O5B Na3 O9B 88.3(3) . . ?
O3B Na3 O4B 81.2(2) . . ?
O5B Na3 O4B 114.4(3) . . ?
O9B Na3 O4B 82.4(2) . . ?
O3B Na3 O2B 84.6(2) . . ?
O5B Na3 O2B 95.4(3) . . ?
O9B Na3 O2B 128.3(2) . . ?
O4B Na3 O2B 138.8(3) . . ?
O3B Na3 O1B 137.9(3) . . ?
O5B Na3 O1B 68.7(3) . . ?
O9B Na3 O1B 144.5(3) . . ?
O4B Na3 O1B 83.1(2) . . ?
O2B Na3 O1B 82.1(2) . . ?
O3B Na3 O7B 85.6(2) . . ?
O5B Na3 O7B 70.0(3) . . ?
O9B Na3 O7B 69.1(2) . . ?
O4B Na3 O7B 151.3(2) . . ?
O2B Na3 O7B 64.2(2) . . ?
O1B Na3 O7B 122.7(3) . . ?
O3B Na3 C34B 51.2(3) . . ?
O5B Na3 C34B 104.5(3) . . ?
O9B Na3 C34B 21.7(3) . . ?
O4B Na3 C34B 89.0(2) . . ?
O2B Na3 C34B 111.3(3) . . ?
O1B Na3 C34B 165.9(3) . . ?
O7B Na3 C34B 63.1(3) . . ?
O3B Na3 Na2 108.92(19) . . ?
O9B Na3 Na2 47.68(18) . . ?
O4B Na3 Na2 115.6(2) . . ?
O2B Na3 Na2 105.6(2) . . ?
O1B Na3 Na2 113.1(2) . . ?
O7B Na3 Na2 45.92(18) . . ?
C34B Na3 Na2 60.2(2) . . ?
O5C Na5 O7D 146.0(8) . . ?
O5C Na5 O9C 95.6(4) . . ?
O7D Na5 O9C 80.3(5) . . ?
O5C Na5 O5D 138.2(7) . . ?
O7D Na5 O5D 74.0(6) . . ?
O9C Na5 O5D 106.7(6) . . ?
O5C Na5 O9D 98.2(6) . . ?
O7D Na5 O9D 59.8(6) . . ?
O9C Na5 O9D 125.3(7) . . ?
O5D Na5 O9D 97.0(4) . . ?
O5C Na5 O11D 93.9(6) . . ?
O7D Na5 O11D 101.2(4) . . ?
O9C Na5 O11D 160.2(7) . . ?
O5D Na5 O11D 55.8(5) . . ?
O9D Na5 O11D 70.2(5) . . ?
O5C Na5 O7C 70.8(5) . . ?
O7D Na5 O7C 136.5(7) . . ?
O9C Na5 O7C 71.3(5) . . ?
O5D Na5 O7C 83.2(5) . . ?
O9D Na5 O7C 161.8(7) . . ?
O11D Na5 O7C 95.6(6) . . ?
O5C Na5 O11C 62.2(5) . . ?
O7D Na5 O11C 88.4(5) . . ?
O9C Na5 O11C 56.8(5) . . ?
O5D Na5 O11C 158.3(6) . . ?
O9D Na5 O11C 84.5(5) . . ?
O11D Na5 O11C 142.6(6) . . ?
O7C Na5 O11C 102.1(3) . . ?
O5C Na5 O10D 94.1(10) . . ?
O7D Na5 O10D 51.8(10) . . ?
O9C Na5 O10D 80.6(10) . . ?
O5D Na5 O10D 123.7(9) . . ?
O9D Na5 O10D 45.9(8) . . ?
O11D Na5 O10D 116.0(9) . . ?
O7C Na5 O10D 146.2(8) . . ?
O11C Na5 O10D 45.2(7) . . ?
O5C Na5 O8D 134.9(8) . . ?
O7D Na5 O8D 68.5(8) . . ?
O9C Na5 O8D 54.0(10) . . ?
O5D Na5 O8D 52.7(10) . . ?
O9D Na5 O8D 126.0(8) . . ?
O11D Na5 O8D 107.8(11) . . ?
O7C Na5 O8D 68.2(9) . . ?
O11C Na5 O8D 109.4(11) . . ?
O10D Na5 O8D 109.9(15) . . ?
O5C Na5 C32D 166.0(9) . . ?
O7D Na5 C32D 35.2(4) . . ?
O9C Na5 C32D 70.4(8) . . ?
O5D Na5 C32D 50.0(8) . . ?
O9D Na5 C32D 90.9(7) . . ?
O11D Na5 C32D 99.3(9) . . ?
O7C Na5 C32D 102.8(7) . . ?
O11C Na5 C32D 108.5(9) . . ?
O10D Na5 C32D 84.6(12) . . ?
O8D Na5 C32D 35.1(4) . . ?
O5C Na5 C30C 30.2(5) . . ?
O7D Na5 C30C 173.4(7) . . ?
O9C Na5 C30C 104.4(4) . . ?
O5D Na5 C30C 108.6(6) . . ?
O9D Na5 C30C 113.6(6) . . ?
O11D Na5 C30C 76.1(4) . . ?
O7C Na5 C30C 50.1(5) . . ?
O11C Na5 C30C 90.4(5) . . ?
O10D Na5 C30C 123.7(11) . . ?
O8D Na5 C30C 118.0(10) . . ?
C32D Na5 C30C 150.7(8) . . ?
C1A O1A C29A 113.2(8) . . ?
C1A O1A Na1 130.0(6) . . ?
C29A O1A Na1 113.1(6) . . ?
C1A C2A C3A 119.2(13) . . ?
C1A C2A C28A 122.8(11) . . ?
C3A C2A C28A 117.9(11) . . ?
C6A C1A C2A 123.1(13) . . ?
C6A C1A O1A 114.7(11) . . ?
C2A C1A O1A 122.2(12) . . ?
C1A C6A C5A 119.5(12) . . ?
C1A C6A C7A 125.1(13) . . ?
C5A C6A C7A 115.0(12) . . ?
C8A C7A C6A 115.5(10) . . ?
C8A C7A H7A1 108.4 . . ?
C6A C7A H7A1 108.4 . . ?
C8A C7A H7A2 108.4 . . ?
C6A C7A H7A2 108.4 . . ?
H7A1 C7A H7A2 107.5 . . ?
C30A C29A O1A 109.0(14) . . ?
C30A C29A H29C 109.9 . . ?
O1A C29A H29C 109.9 . . ?
C30A C29A H29D 109.9 . . ?
O1A C29A H29D 109.9 . . ?
H29C C29A H29D 108.3 . . ?
C4A C3A C2A 118.0(13) . . ?
C4A C3A H3A 121.0 . . ?
C2A C3A H3A 121.0 . . ?
C3A C4A C5A 121.8(13) . . ?
C3A C4A H4A 119.1 . . ?
C5A C4A H4A 119.1 . . ?
C4A C5A C6A 118.1(12) . . ?
C4A C5A H5A 121.0 . . ?
C6A C5A H5A 121.0 . . ?
C30A O6A H6A 109.5 . . ?
O5A C30A O6A 129(2) . . ?
O5A C30A C29A 129(2) . . ?
O6A C30A C29A 102.0(19) . . ?
C9A O2A C31A 112.3(8) . . ?
C9A O2A Na1 131.0(6) . . ?
C31A O2A Na1 116.6(7) . . ?
C32A O7A Na1 123.1(8) . . ?
C32A O7A Na2 148.4(8) . . ?
Na1 O7A Na2 88.4(3) . . ?
C13A C8A C7A 121.9(15) . . ?
C13A C8A C9A 108.9(16) . . ?
C7A C8A C9A 127.8(15) . . ?
C10A C9A O2A 120.7(14) . . ?
C10A C9A C8A 125.9(16) . . ?
O2A C9A C8A 112.7(14) . . ?
C32A C31A O2A 110.7(10) . . ?
C32A C31A H31A 109.5 . . ?
O2A C31A H31A 109.5 . . ?
C32A C31A H31B 109.5 . . ?
O2A C31A H31B 109.5 . . ?
H31A C31A H31B 108.1 . . ?
O7A C32A O8A 123.3(13) . . ?
O7A C32A C31A 122.4(10) . . ?
O8A C32A C31A 114.2(12) . . ?
C10A C14A C15A 110.3(10) . . ?
C10A C14A H14C 109.6 . . ?
C15A C14A H14C 109.6 . . ?
C10A C14A H14D 109.6 . . ?
C15A C14A H14D 109.6 . . ?
H14C C14A H14D 108.1 . . ?
C9A C10A C11A 120.8(16) . . ?
C9A C10A C14A 118.4(13) . . ?
C11A C10A C14A 120.3(16) . . ?
C8A C13A C12A 123.1(16) . . ?
C8A C13A H13A 118.4 . . ?
C12A C13A H13A 118.4 . . ?
C11A C12A C13A 122.7(16) . . ?
C11A C12A H12A 118.7 . . ?
C13A C12A H12A 118.6 . . ?
C12A C11A C10A 118.1(18) . . ?
C12A C11A H11A 120.9 . . ?
C10A C11A H11A 120.9 . . ?
C16A O3A C33A 112.8(7) . . ?
C16A O3A Na1 130.5(6) . . ?
C33A O3A Na1 116.7(6) . . ?
C34A O10A H10A 109.5 . . ?
C22A C21A C17A 111.6(11) . . ?
C22A C21A H21C 109.3 . . ?
C17A C21A H21C 109.3 . . ?
C22A C21A H21D 109.3 . . ?
C17A C21A H21D 109.3 . . ?
H21C C21A H21D 108.0 . . ?
C18A C17A C16A 113.7(13) . . ?
C18A C17A C21A 124.3(13) . . ?
C16A C17A C21A 121.5(11) . . ?
C19A C18A C17A 123.3(17) . . ?
C19A C18A H18A 118.3 . . ?
C17A C18A H18A 118.3 . . ?
C18A C19A C20A 121.7(19) . . ?
C18A C19A H19A 119.1 . . ?
C20A C19A H19A 119.1 . . ?
C19A C20A C15A 121.9(18) . . ?
C19A C20A H20A 119.0 . . ?
C15A C20A H20A 119.0 . . ?
C16A C15A C20A 114.8(15) . . ?
C16A C15A C14A 122.3(13) . . ?
C20A C15A C14A 122.2(13) . . ?
C15A C16A C17A 124.3(13) . . ?
C15A C16A O3A 119.7(12) . . ?
C17A C16A O3A 115.7(11) . . ?
C34A C33A O3A 112.5(10) . . ?
C34A C33A H33E 109.1 . . ?
O3A C33A H33E 109.1 . . ?
C34A C33A H33F 109.1 . . ?
O3A C33A H33F 109.1 . . ?
H33E C33A H33F 107.8 . . ?
O9A C34A O10A 132.7(13) . . ?
O9A C34A C33A 116.3(12) . . ?
O10A C34A C33A 111.0(11) . . ?
C34A O9A Na2 130.8(7) . . ?
C34A O9A Na1 124.5(8) . . ?
Na2 O9A Na1 83.2(3) . . ?
C36A O11A Na1 114.5(6) . . ?
C36A O11A Na2 122.0(7) . . ?
Na1 O11A Na2 84.4(2) . . ?
C23A O4A C35A 113.0(7) . . ?
C23A O4A Na1 132.3(6) . . ?
C35A O4A Na1 114.7(5) . . ?
C36A O12A H12' 109.5 . . ?
O11A C36A O12A 123.4(10) . . ?
O11A C36A C35A 124.4(11) . . ?
O12A C36A C35A 112.1(9) . . ?
O12A C36A Na1 162.2(7) . . ?
C35A C36A Na1 82.2(6) . . ?
O4A C35A C36A 109.9(8) . . ?
O4A C35A H35C 109.7 . . ?
C36A C35A H35C 109.7 . . ?
O4A C35A H35D 109.7 . . ?
C36A C35A H35D 109.7 . . ?
H35C C35A H35D 108.2 . . ?
C24A C23A O4A 118.5(10) . . ?
C24A C23A C22A 123.6(11) . . ?
O4A C23A C22A 117.9(10) . . ?
C23A C24A C28A 125.4(10) . . ?
C23A C24A C25A 120.1(10) . . ?
C28A C24A C25A 114.4(11) . . ?
C24A C28A C2A 111.3(9) . . ?
C24A C28A H28C 109.4 . . ?
C2A C28A H28C 109.4 . . ?
C24A C28A H28D 109.4 . . ?
C2A C28A H28D 109.4 . . ?
H28C C28A H28D 108.0 . . ?
C27A C22A C23A 115.8(11) . . ?
C27A C22A C21A 120.5(11) . . ?
C23A C22A C21A 123.3(10) . . ?
C26A C25A C24A 114.8(11) . . ?
C26A C25A H25A 122.6 . . ?
C24A C25A H25A 122.6 . . ?
C27A C26A C25A 120.3(11) . . ?
C27A C26A H26A 119.9 . . ?
C25A C26A H26A 119.9 . . ?
C26A C27A C22A 124.8(12) . . ?
C26A C27A H27A 117.6 . . ?
C22A C27A H27A 117.6 . . ?
C1B O1B C29B 111.2(7) . . ?
C1B O1B Na3 133.3(6) . . ?
C29B O1B Na3 115.4(5) . . ?
C4B C5B C6B 120.6(11) . . ?
C4B C5B H5B 119.7 . . ?
C6B C5B H5B 119.7 . . ?
C8B C7B C6B 109.7(8) . . ?
C8B C7B H7B1 109.7 . . ?
C6B C7B H7B1 109.7 . . ?
C8B C7B H7B2 109.7 . . ?
C6B C7B H7B2 109.7 . . ?
H7B1 C7B H7B2 108.2 . . ?
C1B C6B C5B 118.5(9) . . ?
C1B C6B C7B 122.4(8) . . ?
C5B C6B C7B 119.0(9) . . ?
O1B C1B C6B 119.2(8) . . ?
O1B C1B C2B 119.2(9) . . ?
C6B C1B C2B 121.6(9) . . ?
O1B C29B C30B 112.6(9) . . ?
O1B C29B H29E 109.1 . . ?
C30B C29B H29E 109.1 . . ?
O1B C29B H29F 109.1 . . ?
C30B C29B H29F 109.1 . . ?
H29E C29B H29F 107.8 . . ?
O5B C30B O6B 128.2(13) . . ?
O5B C30B C29B 121.3(12) . . ?
O6B C30B C29B 110.4(11) . . ?
C30B O5B Na2 144.7(8) . . ?
C30B O5B Na3 119.2(9) . . ?
Na2 O5B Na3 89.9(3) . . ?
C30B O6B H6B 109.5 . . ?
C5B C4B C3B 122.2(10) . . ?
C5B C4B H4B 118.9 . . ?
C3B C4B H4B 118.9 . . ?
C2B C3B C4B 118.2(10) . . ?
C2B C3B H3B 120.9 . . ?
C4B C3B H3B 120.9 . . ?
C3B C2B C1B 117.4(10) . . ?
C3B C2B C28B 123.0(9) . . ?
C1B C2B C28B 119.4(8) . . ?
C9B O2B C31B 109.5(7) . . ?
C9B O2B Na3 128.6(5) . . ?
C31B O2B Na3 121.9(6) . . ?
C32B O7B Na2 131.4(7) . . ?
C32B O7B Na3 119.4(6) . . ?
Na2 O7B Na3 82.6(2) . . ?
C15B C14B C10B 112.3(8) . . ?
C15B C14B H14E 109.1 . . ?
C10B C14B H14E 109.1 . . ?
C15B C14B H14F 109.2 . . ?
C10B C14B H14F 109.2 . . ?
H14E C14B H14F 107.9 . . ?
C9B C10B C11B 115.1(9) . . ?
C9B C10B C14B 122.4(10) . . ?
C11B C10B C14B 122.5(10) . . ?
C8B C9B O2B 121.0(10) . . ?
C8B C9B C10B 122.9(10) . . ?
O2B C9B C10B 116.0(9) . . ?
C13B C8B C9B 120.2(11) . . ?
C13B C8B C7B 117.5(9) . . ?
C9B C8B C7B 122.3(10) . . ?
C12B C11B C10B 123.9(11) . . ?
C12B C11B H11B 118.0 . . ?
C10B C11B H11B 118.0 . . ?
C11B C12B C13B 117.0(10) . . ?
C11B C12B H12B 121.5 . . ?
C13B C12B H12B 121.5 . . ?
C8B C13B C12B 120.3(10) . . ?
C8B C13B H13B 119.8 . . ?
C12B C13B H13B 119.8 . . ?
O2B C31B C32B 111.0(8) . . ?
O2B C31B H31C 109.4 . . ?
C32B C31B H31C 109.4 . . ?
O2B C31B H31D 109.4 . . ?
C32B C31B H31D 109.4 . . ?
H31C C31B H31D 108.0 . . ?
O7B C32B O8B 125.2(10) . . ?
O7B C32B C31B 118.7(9) . . ?
O8B C32B C31B 116.2(9) . . ?
C34B C33B O3B 110.8(8) . . ?
C34B C33B H33A 109.5 . . ?
O3B C33B H33A 109.5 . . ?
C34B C33B H33B 109.5 . . ?
O3B C33B H33B 109.5 . . ?
H33A C33B H33B 108.1 . . ?
C16B O3B C33B 110.6(6) . . ?
C16B O3B Na3 138.1(5) . . ?
C33B O3B Na3 111.2(5) . . ?
C19B C18B C17B 117.2(11) . . ?
C19B C18B H18B 121.4 . . ?
C17B C18B H18B 121.4 . . ?
C34B O9B Na3 112.0(6) . . ?
C34B O9B Na2 117.7(6) . . ?
Na3 O9B Na2 85.5(2) . . ?
O9B C34B O10B 124.2(11) . . ?
O9B C34B C33B 124.9(9) . . ?
O10B C34B C33B 110.9(11) . . ?
O9B C34B Na3 46.3(5) . . ?
O10B C34B Na3 163.6(8) . . ?
C33B C34B Na3 79.8(5) . . ?
C17B C16B C15B 126.4(12) . . ?
C17B C16B O3B 117.8(10) . . ?
C15B C16B O3B 115.8(10) . . ?
C16B C15B C20B 115.3(11) . . ?
C16B C15B C14B 123.5(11) . . ?
C20B C15B C14B 121.1(10) . . ?
C22B C21B C17B 110.1(7) . . ?
C22B C21B H21E 109.6 . . ?
C17B C21B H21E 109.6 . . ?
C22B C21B H21F 109.6 . . ?
C17B C21B H21F 109.6 . . ?
H21E C21B H21F 108.2 . . ?
C16B C17B C18B 117.1(10) . . ?
C16B C17B C21B 122.6(10) . . ?
C18B C17B C21B 120.4(10) . . ?
C20B C19B C18B 122.9(13) . . ?
C20B C19B H19B 118.5 . . ?
C18B C19B H19B 118.5 . . ?
C19B C20B C15B 120.6(12) . . ?
C19B C20B H20B 119.7 . . ?
C15B C20B H20B 119.7 . . ?
C26B C25B C24B 121.1(10) . . ?
C26B C25B H25B 119.4 . . ?
C24B C25B H25B 119.4 . . ?
C23B O4B C35B 110.4(7) . . ?
C23B O4B Na3 129.9(5) . . ?
C35B O4B Na3 118.0(5) . . ?
C24B C28B C2B 107.3(8) . . ?
C24B C28B H28E 110.2 . . ?
C2B C28B H28E 110.2 . . ?
C24B C28B H28F 110.2 . . ?
C2B C28B H28F 110.2 . . ?
H28E C28B H28F 108.5 . . ?
C25B C24B C23B 119.0(11) . . ?
C25B C24B C28B 124.6(9) . . ?
C23B C24B C28B 116.3(10) . . ?
O4B C23B C22B 117.5(8) . . ?
O4B C23B C24B 122.0(10) . . ?
C22B C23B C24B 120.5(10) . . ?
C27B C22B C23B 115.3(9) . . ?
C27B C22B C21B 121.8(10) . . ?
C23B C22B C21B 122.8(9) . . ?
C26B C27B C22B 121.7(11) . . ?
C26B C27B H27B 119.1 . . ?
C22B C27B H27B 119.1 . . ?
C25B C26B C27B 122.1(11) . . ?
C25B C26B H26B 119.0 . . ?
C27B C26B H26B 119.0 . . ?
C36B C35B O4B 113.3(11) . . ?
C36B C35B H35E 108.9 . . ?
O4B C35B H35E 108.9 . . ?
C36B C35B H35F 108.9 . . ?
O4B C35B H35F 108.9 . . ?
H35E C35B H35F 107.7 . . ?
O12B C36B O11B 119.4(17) . . ?
O12B C36B C35B 119.0(16) . . ?
O11B C36B C35B 121.6(15) . . ?
C36B O12B H12O 109.5 . . ?
C1C O1C C29C 112.4(9) . . ?
C1C O1C Na4 130.2(6) . . ?
C29C O1C Na4 117.0(7) . . ?
O5C C30C O6C 134.5(17) . . ?
O5C C30C C29C 122.0(12) . . ?
O6C C30C C29C 86.6(15) . . ?
O5C C30C Na4 53.9(7) . . ?
O6C C30C Na4 171.2(16) . . ?
C29C C30C Na4 89.6(6) . . ?
O5C C30C Na5 52.1(10) . . ?
O6C C30C Na5 117.4(10) . . ?
C29C C30C Na5 151.6(10) . . ?
Na4 C30C Na5 64.3(5) . . ?
C30C O6C H6C 109.5 . . ?
O1C C29C C30C 101.3(11) . . ?
O1C C29C H29A 111.5 . . ?
C30C C29C H29A 111.5 . . ?
O1C C29C H29B 111.5 . . ?
C30C C29C H29B 111.5 . . ?
H29A C29C H29B 109.3 . . ?
C2C C1C C6C 126.6(13) . . ?
C2C C1C O1C 118.9(11) . . ?
C6C C1C O1C 114.5(12) . . ?
C1C C6C C5C 111.6(13) . . ?
C1C C6C C7C 123.2(12) . . ?
C5C C6C C7C 125.2(13) . . ?
C6C C7C C8C 108.7(10) . . ?
C6C C7C H7C1 109.9 . . ?
C8C C7C H7C1 109.9 . . ?
C6C C7C H7C2 109.9 . . ?
C8C C7C H7C2 109.9 . . ?
H7C1 C7C H7C2 108.3 . . ?
C1C C2C C3C 116.3(13) . . ?
C1C C2C C28C 124.5(12) . . ?
C3C C2C C28C 119.0(13) . . ?
C4C C5C C6C 125.5(15) . . ?
C4C C5C H5C 117.3 . . ?
C6C C5C H5C 117.3 . . ?
C5C C4C C3C 116.9(15) . . ?
C5C C4C H4C 121.5 . . ?
C3C C4C H4C 121.5 . . ?
C4C C3C C2C 122.8(15) . . ?
C4C C3C H3C 118.6 . . ?
C2C C3C H3C 118.6 . . ?
C30C O5C Na4 94.0(10) . . ?
C30C O5C Na5 97.7(12) . . ?
Na4 O5C Na5 83.1(5) . . ?
C31C O2C C9C 112.5(10) . . ?
C31C O2C Na4 114.3(7) . . ?
C9C O2C Na4 132.8(6) . . ?
C9C C8C C13C 116.4(14) . . ?
C9C C8C C7C 124.7(13) . . ?
C13C C8C C7C 118.9(14) . . ?
C8C C9C O2C 118.9(13) . . ?
C8C C9C C10C 127.0(14) . . ?
O2C C9C C10C 114.1(12) . . ?
C11C C10C C14C 126.1(13) . . ?
C11C C10C C9C 109.6(14) . . ?
C14C C10C C9C 124.3(12) . . ?
C10C C14C C15C 105.7(10) . . ?
C10C C14C H14A 110.6 . . ?
C15C C14C H14A 110.6 . . ?
C10C C14C H14B 110.6 . . ?
C15C C14C H14B 110.6 . . ?
H14A C14C H14B 108.7 . . ?
C32C C31C O2C 112.2(18) . . ?
C32C C31C H31G 109.2 . . ?
O2C C31C H31G 109.2 . . ?
C32C C31C H31H 109.2 . . ?
O2C C31C H31H 109.2 . . ?
H31G C31C H31H 107.9 . . ?
C12C C13C C8C 118.1(15) . . ?
C12C C13C H13C 121.0 . . ?
C8C C13C H13C 121.0 . . ?
C11C C12C C13C 116.1(16) . . ?
C11C C12C H12C 122.0 . . ?
C13C C12C H12C 122.0 . . ?
C12C C11C C10C 132.4(18) . . ?
C12C C11C H11C 113.8 . . ?
C10C C11C H11C 113.8 . . ?
C32C O7C Na4 91.2(11) . . ?
C32C O7C Na5 95.3(10) . . ?
Na4 O7C Na5 77.7(5) . . ?
C31C C32C O8C 99.0(18) . . ?
C31C C32C O7C 108(2) . . ?
O8C C32C O7C 93.9(15) . . ?
C31C C32C Na4 85.4(15) . . ?
O8C C32C Na4 146.7(16) . . ?
O7C C32C Na4 53.8(9) . . ?
C33C O3C C16C 106.9(7) . . ?
C33C O3C Na4 118.8(6) . . ?
C16C O3C Na4 133.8(6) . . ?
C16C C15C C20C 109.5(12) . . ?
C16C C15C C14C 126.6(11) . . ?
C20C C15C C14C 123.8(12) . . ?
C17C C16C C15C 125.9(12) . . ?
C17C C16C O3C 120.5(11) . . ?
C15C C16C O3C 113.5(11) . . ?
C34C C33C O3C 115.8(17) . . ?
C34C C33C H33C 108.3 . . ?
O3C C33C H33C 108.3 . . ?
C34C C33C H33D 108.3 . . ?
O3C C33C H33D 108.3 . . ?
H33C C33C H33D 107.4 . . ?
C22C C21C C17C 111.3(10) . . ?
C22C C21C H21A 109.4 . . ?
C17C C21C H21A 109.4 . . ?
C22C C21C H21B 109.4 . . ?
C17C C21C H21B 109.4 . . ?
H21A C21C H21B 108.0 . . ?
C16C C17C C18C 118.7(13) . . ?
C16C C17C C21C 122.6(11) . . ?
C18C C17C C21C 118.5(12) . . ?
C19C C18C C17C 121.6(14) . . ?
C19C C18C H18C 119.2 . . ?
C17C C18C H18C 119.2 . . ?
C18C C19C C20C 117.0(14) . . ?
C18C C19C H19C 121.5 . . ?
C20C C19C H19C 121.5 . . ?
C19C C20C C15C 126.5(14) . . ?
C19C C20C H20C 116.8 . . ?
C15C C20C H20C 116.8 . . ?
C34C O9C Na4 103.4(13) . . ?
C34C O9C Na5 116.3(14) . . ?
Na4 O9C Na5 79.2(4) . . ?
C34C O10C H10C 109.5 . . ?
O10C C34C C33C 121(2) . . ?
O10C C34C O9C 107(2) . . ?
C33C C34C O9C 103(2) . . ?
C35C O4C C23C 110.7(8) . . ?
C35C O4C Na4 120.6(6) . . ?
C23C O4C Na4 128.6(6) . . ?
C2C C28C C24C 110.2(9) . . ?
C2C C28C H28A 109.6 . . ?
C24C C28C H28A 109.6 . . ?
C2C C28C H28B 109.6 . . ?
C24C C28C H28B 109.6 . . ?
H28A C28C H28B 108.1 . . ?
C23C C24C C25C 119.6(11) . . ?
C23C C24C C28C 121.7(11) . . ?
C25C C24C C28C 117.7(12) . . ?
C26C C25C C24C 115.5(13) . . ?
C26C C25C H25C 122.2 . . ?
C24C C25C H25C 122.2 . . ?
C27C C26C C25C 126.8(13) . . ?
C27C C26C H26C 116.6 . . ?
C25C C26C H26C 116.6 . . ?
C26C C27C C22C 116.9(13) . . ?
C26C C27C H27C 121.5 . . ?
C22C C27C H27C 121.5 . . ?
C23C C22C C27C 117.3(13) . . ?
C23C C22C C21C 124.9(11) . . ?
C27C C22C C21C 117.6(11) . . ?
C24C C23C C22C 123.8(12) . . ?
C24C C23C O4C 121.5(10) . . ?
C22C C23C O4C 114.5(11) . . ?
O4C C35C C36C 106.3(13) . . ?
O4C C35C H35A 110.5 . . ?
C36C C35C H35A 110.5 . . ?
O4C C35C H35B 110.5 . . ?
C36C C35C H35B 110.5 . . ?
H35A C35C H35B 108.7 . . ?
C36C O11C Na4 87.1(10) . . ?
C36C O11C Na5 95.0(11) . . ?
Na4 O11C Na5 72.5(4) . . ?
C36C O12C H12E 109.5 . . ?
O12C C36C C35C 105.2(17) . . ?
O12C C36C O11C 117(2) . . ?
C35C C36C O11C 115.2(16) . . ?
C1D O1D C29D 108.2(12) . . ?
C1D O1D Na6 137.7(10) . . ?
C29D O1D Na6 114.0(9) . . ?
C8D C7D C6D 117.7(12) . . ?
C8D C7D H7D1 107.9 . . ?
C6D C7D H7D1 107.9 . . ?
C8D C7D H7D2 107.9 . . ?
C6D C7D H7D2 107.9 . . ?
H7D1 C7D H7D2 107.2 . . ?
C1D C6D C5D 122.7(16) . . ?
C1D C6D C7D 118.8(14) . . ?
C5D C6D C7D 118.3(16) . . ?
C2D C1D C6D 113.8(17) . . ?
C2D C1D O1D 128.1(18) . . ?
C6D C1D O1D 117.4(17) . . ?
C1D C2D C3D 127(2) . . ?
C1D C2D C28D 116.6(16) . . ?
C3D C2D C28D 115.4(18) . . ?
C4D C5D C6D 117.5(17) . . ?
C4D C5D H5D 121.3 . . ?
C6D C5D H5D 121.3 . . ?
C3D C4D C5D 119.9(18) . . ?
C3D C4D H4D 120.0 . . ?
C5D C4D H4D 120.0 . . ?
C4D C3D C2D 119(2) . . ?
C4D C3D H3D 120.6 . . ?
C2D C3D H3D 120.6 . . ?
C30D C29D O1D 125(2) . . ?
C30D C29D Na6 88.0(15) . . ?
C30D C29D H29G 106.0 . . ?
O1D C29D H29G 106.0 . . ?
Na6 C29D H29G 140.1 . . ?
C30D C29D H29H 106.0 . . ?
O1D C29D H29H 106.0 . . ?
Na6 C29D H29H 105.3 . . ?
H29G C29D H29H 106.3 . . ?
C30D O6D H6D 109.5 . . ?
C30D O5D Na6 122.7(13) . . ?
C30D O5D Na5 131.5(16) . . ?
Na6 O5D Na5 81.5(6) . . ?
O6D C30D C29D 120(3) . . ?
O6D C30D O5D 102(3) . . ?
C29D C30D O5D 104(2) . . ?
C10D C14D C15D 119.3(16) . . ?
C10D C14D H14G 107.5 . . ?
C15D C14D H14G 107.5 . . ?
C10D C14D H14H 107.5 . . ?
C15D C14D H14H 107.5 . . ?
H14G C14D H14H 107.0 . . ?
C9D C10D C14D 127.4(17) . . ?
C9D C10D C11D 119.9(15) . . ?
C14D C10D C11D 112.4(17) . . ?
C8D C9D O2D 124.6(18) . . ?
C8D C9D C10D 123.2(18) . . ?
O2D C9D C10D 111.1(15) . . ?
C9D C8D C7D 118.0(17) . . ?
C9D C8D C13D 119.6(18) . . ?
C7D C8D C13D 121.7(16) . . ?
C12D C11D C10D 111.5(17) . . ?
C12D C11D H11D 124.3 . . ?
C10D C11D H11D 124.3 . . ?
C11D C12D C13D 127.9(18) . . ?
C11D C12D H12D 116.0 . . ?
C13D C12D H12D 116.0 . . ?
C12D C13D C8D 117.0(16) . . ?
C12D C13D H13D 121.5 . . ?
C8D C13D H13D 121.5 . . ?
C31D O2D C9D 120.7(16) . . ?
C31D O2D Na6 110.5(13) . . ?
C9D O2D Na6 128.2(8) . . ?
O2D C31D C32D 114(2) . . ?
O2D C31D Na6 47.9(10) . . ?
C32D C31D Na6 68.6(15) . . ?
O2D C31D H31E 108.8 . . ?
C32D C31D H31E 108.8 . . ?
Na6 C31D H31E 110.1 . . ?
O2D C31D H31F 108.8 . . ?
C32D C31D H31F 108.8 . . ?
Na6 C31D H31F 140.7 . . ?
H31E C31D H31F 107.7 . . ?
O7D C32D O8D 116.2 . . ?
O7D C32D C31D 117.9(19) . . ?
O8D C32D C31D 120.9(19) . . ?
O7D C32D Na6 57.2(12) . . ?
O8D C32D Na6 116(2) . . ?
C31D C32D Na6 77.1(16) . . ?
O7D C32D Na5 54.4(8) . . ?
O8D C32D Na5 66.0(10) . . ?
C31D C32D Na5 138(2) . . ?
Na6 C32D Na5 64.7(7) . . ?
C32D O7D Na6 85.5(16) . . ?
C32D O7D Na5 90.4(10) . . ?
Na6 O7D Na5 80.5(5) . . ?
C32D O8D Na5 78.9(10) . . ?
C32D O8D H8D 109.5 . . ?
C17D C21D C22D 109.4(18) . . ?
C17D C21D H21G 109.8 . . ?
C22D C21D H21G 109.8 . . ?
C17D C21D H21H 109.8 . . ?
C22D C21D H21H 109.8 . . ?
H21G C21D H21H 108.2 . . ?
C16D C17D C21D 127(2) . . ?
C16D C17D C18D 107(2) . . ?
C21D C17D C18D 126(2) . . ?
C15D C16D O3D 121(3) . . ?
C15D C16D C17D 128(2) . . ?
O3D C16D C17D 111(2) . . ?
C16D C15D C20D 124(2) . . ?
C16D C15D C14D 120(3) . . ?
C20D C15D C14D 114(2) . . ?
C19D C18D C17D 128(2) . . ?
C19D C18D H18D 115.9 . . ?
C17D C18D H18D 115.9 . . ?
C18D C19D C20D 119(2) . . ?
C18D C19D H19D 120.3 . . ?
C20D C19D H19D 120.3 . . ?
C15D C20D C19D 113.2(19) . . ?
C15D C20D H20D 123.4 . . ?
C19D C20D H20D 123.4 . . ?
C16D O3D C33D 115.3(15) . . ?
C16D O3D Na6 135.7(9) . . ?
C33D O3D Na6 108.6(12) . . ?
O3D C33D C34D 116(2) . . ?
O3D C33D H33G 98.4 . . ?
C34D C33D H33G 117.2 . . ?
O3D C33D H33H 116.5 . . ?
C34D C33D H33H 100.5 . . ?
H33G C33D H33H 108.5 . . ?
C34D O10D Na5 91(3) . . ?
O9D C34D O10D 100(3) . . ?
O9D C34D C33D 122(3) . . ?
O10D C34D C33D 138(3) . . ?
O9D C34D Na6 58.6(19) . . ?
O10D C34D Na6 125(4) . . ?
C33D C34D Na6 80(2) . . ?
O9D C34D Na5 55.8(18) . . ?
O10D C34D Na5 62(3) . . ?
C33D C34D Na5 139(3) . . ?
Na6 C34D Na5 64.1(9) . . ?
C34D O9D Na5 99(2) . . ?
C34D O9D Na6 96(2) . . ?
Na5 O9D Na6 77.5(5) . . ?
C36D O11D Na5 107.4(17) . . ?
C36D O11D Na6 107.9(16) . . ?
Na5 O11D Na6 75.2(5) . . ?
C2D C28D C24D 115.4(16) . . ?
C2D C28D H28G 108.4 . . ?
C24D C28D H28G 108.4 . . ?
C2D C28D H28H 108.4 . . ?
C24D C28D H28H 108.4 . . ?
H28G C28D H28H 107.5 . . ?
C23D C24D C25D 136(2) . . ?
C23D C24D C28D 116(2) . . ?
C25D C24D C28D 107.4(17) . . ?
C24D C23D O4D 134(2) . . ?
C24D C23D C22D 119(2) . . ?
O4D C23D C22D 104.6(17) . . ?
C35D O4D C23D 116.4(17) . . ?
C35D O4D Na6 106.6(12) . . ?
C23D O4D Na6 127.4(11) . . ?
C26D C25D C24D 107.8(18) . . ?
C26D C25D H25D 126.1 . . ?
C24D C25D H25D 126.1 . . ?
O4D C35D C36D 137(2) . . ?
O4D C35D Na6 48.9(10) . . ?
C36D C35D Na6 88.1(14) . . ?
O4D C35D H35G 103.0 . . ?
C36D C35D H35G 103.0 . . ?
Na6 C35D H35G 119.6 . . ?
O4D C35D H35H 103.0 . . ?
C36D C35D H35H 103.0 . . ?
Na6 C35D H35H 130.2 . . ?
H35G C35D H35H 105.1 . . ?
C27D C22D C23D 109(2) . . ?
C27D C22D C21D 119(2) . . ?
C23D C22D C21D 130.2(18) . . ?
C25D C26D C27D 120.4(19) . . ?
C25D C26D H26D 119.8 . . ?
C27D C26D H26D 119.8 . . ?
C22D C27D C26D 127(2) . . ?
C22D C27D H27D 116.7 . . ?
C26D C27D H27D 116.6 . . ?
O11D C36D O12D 128(3) . . ?
O11D C36D C35D 106(2) . . ?
O12D C36D C35D 124(3) . . ?
H1W O1W H2W 109.4 . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3A C2A C1A C6A -4.8(16) . . . . ?
C28A C2A C1A C6A 169.6(10) . . . . ?
C3A C2A C1A O1A 176.0(9) . . . . ?
C28A C2A C1A O1A -9.5(15) . . . . ?
C29A O1A C1A C6A 108.3(11) . . . . ?
Na1 O1A C1A C6A -95.4(10) . . . . ?
C29A O1A C1A C2A -72.5(12) . . . . ?
Na1 O1A C1A C2A 83.8(12) . . . . ?
C2A C1A C6A C5A 4.3(17) . . . . ?
O1A C1A C6A C5A -176.5(9) . . . . ?
C2A C1A C6A C7A -168.3(11) . . . . ?
O1A C1A C6A C7A 10.9(16) . . . . ?
C1A C6A C7A C8A 95.2(16) . . . . ?
C5A C6A C7A C8A -77.7(15) . . . . ?
C1A O1A C29A C30A -130.9(14) . . . . ?
Na1 O1A C29A C30A 68.7(14) . . . . ?
C1A C2A C3A C4A -0.1(16) . . . . ?
C28A C2A C3A C4A -174.8(10) . . . . ?
C2A C3A C4A C5A 5.3(18) . . . . ?
C3A C4A C5A C6A -5.9(17) . . . . ?
C1A C6A C5A C4A 1.0(17) . . . . ?
C7A C6A C5A C4A 174.3(10) . . . . ?
O1A C29A C30A O5A -1(5) . . . . ?
O1A C29A C30A O6A 173.4(13) . . . . ?
C6A C7A C8A C13A 78.0(15) . . . . ?
C6A C7A C8A C9A -86.9(17) . . . . ?
C31A O2A C9A C10A 88.2(13) . . . . ?
Na1 O2A C9A C10A -96.0(12) . . . . ?
C31A O2A C9A C8A -82.8(11) . . . . ?
Na1 O2A C9A C8A 92.9(11) . . . . ?
C13A C8A C9A C10A 4.3(16) . . . . ?
C7A C8A C9A C10A 170.7(12) . . . . ?
C13A C8A C9A O2A 174.7(8) . . . . ?
C7A C8A C9A O2A -18.8(16) . . . . ?
C9A O2A C31A C32A -178.2(12) . . . . ?
Na1 O2A C31A C32A 5.4(13) . . . . ?
Na1 O7A C32A O8A 171.4(9) . . . . ?
Na2 O7A C32A O8A -3(2) . . . . ?
Na1 O7A C32A C31A -5.7(18) . . . . ?
Na2 O7A C32A C31A -179.6(11) . . . . ?
O2A C31A C32A O7A -0.2(19) . . . . ?
O2A C31A C32A O8A -177.5(9) . . . . ?
O2A C9A C10A C11A -173.1(11) . . . . ?
C8A C9A C10A C11A -3.4(19) . . . . ?
O2A C9A C10A C14A 14.1(16) . . . . ?
C8A C9A C10A C14A -176.1(11) . . . . ?
C15A C14A C10A C9A 94.6(14) . . . . ?
C15A C14A C10A C11A -78.2(14) . . . . ?
C7A C8A C13A C12A -173.1(11) . . . . ?
C9A C8A C13A C12A -5.6(16) . . . . ?
C8A C13A C12A C11A 7(2) . . . . ?
C13A C12A C11A C10A -5(2) . . . . ?
C9A C10A C11A C12A 3(2) . . . . ?
C14A C10A C11A C12A 176.0(13) . . . . ?
C22A C21A C17A C18A -75.9(14) . . . . ?
C22A C21A C17A C16A 95.2(13) . . . . ?
C16A C17A C18A C19A 2(2) . . . . ?
C21A C17A C18A C19A 173.8(14) . . . . ?
C17A C18A C19A C20A -5(3) . . . . ?
C18A C19A C20A C15A 7(3) . . . . ?
C19A C20A C15A C16A -4(2) . . . . ?
C19A C20A C15A C14A -174.5(14) . . . . ?
C10A C14A C15A C16A -95.2(15) . . . . ?
C10A C14A C15A C20A 74.3(15) . . . . ?
C20A C15A C16A C17A 1.1(18) . . . . ?
C14A C15A C16A C17A 171.4(11) . . . . ?
C20A C15A C16A O3A 174.2(10) . . . . ?
C14A C15A C16A O3A -15.6(17) . . . . ?
C18A C17A C16A C15A -0.1(17) . . . . ?
C21A C17A C16A C15A -172.1(12) . . . . ?
C18A C17A C16A O3A -173.4(10) . . . . ?
C21A C17A C16A O3A 14.6(15) . . . . ?
C33A O3A C16A C15A -86.2(12) . . . . ?
Na1 O3A C16A C15A 92.9(11) . . . . ?
C33A O3A C16A C17A 87.4(11) . . . . ?
Na1 O3A C16A C17A -93.5(10) . . . . ?
C16A O3A C33A C34A -161.4(9) . . . . ?
Na1 O3A C33A C34A 19.4(11) . . . . ?
O3A C33A C34A O9A -2.5(14) . . . . ?
O3A C33A C34A O10A 179.6(9) . . . . ?
O10A C34A O9A Na2 46.8(19) . . . . ?
C33A C34A O9A Na2 -130.5(9) . . . . ?
O10A C34A O9A Na1 160.6(11) . . . . ?
C33A C34A O9A Na1 -16.7(13) . . . . ?
Na1 O11A C36A O12A 163.0(9) . . . . ?
Na2 O11A C36A O12A 63.8(13) . . . . ?
Na1 O11A C36A C35A -21.2(14) . . . . ?
Na2 O11A C36A C35A -120.3(10) . . . . ?
Na2 O11A C36A Na1 -99.1(7) . . . . ?
C23A O4A C35A C36A -159.5(9) . . . . ?
Na1 O4A C35A C36A 20.3(11) . . . . ?
O11A C36A C35A O4A 0.8(16) . . . . ?
O12A C36A C35A O4A 177.0(9) . . . . ?
Na1 C36A C35A O4A -14.0(8) . . . . ?
C35A O4A C23A C24A 87.3(12) . . . . ?
Na1 O4A C23A C24A -92.4(11) . . . . ?
C35A O4A C23A C22A -93.7(11) . . . . ?
Na1 O4A C23A C22A 86.6(11) . . . . ?
O4A C23A C24A C28A 8.7(17) . . . . ?
C22A C23A C24A C28A -170.3(10) . . . . ?
O4A C23A C24A C25A -175.5(9) . . . . ?
C22A C23A C24A C25A 5.6(17) . . . . ?
C23A C24A C28A C2A 96.5(14) . . . . ?
C25A C24A C28A C2A -79.6(11) . . . . ?
C1A C2A C28A C24A -95.0(12) . . . . ?
C3A C2A C28A C24A 79.5(12) . . . . ?
C24A C23A C22A C27A -1.8(17) . . . . ?
O4A C23A C22A C27A 179.3(10) . . . . ?
C24A C23A C22A C21A 171.6(12) . . . . ?
O4A C23A C22A C21A -7.3(16) . . . . ?
C17A C21A C22A C27A 73.0(13) . . . . ?
C17A C21A C22A C23A -100.1(13) . . . . ?
C23A C24A C25A C26A -2.2(16) . . . . ?
C28A C24A C25A C26A 174.1(11) . . . . ?
C24A C25A C26A C27A -5.1(19) . . . . ?
C25A C26A C27A C22A 10(2) . . . . ?
C23A C22A C27A C26A -6.2(19) . . . . ?
C21A C22A C27A C26A -179.8(13) . . . . ?
C4B C5B C6B C1B -1.5(14) . . . . ?
C4B C5B C6B C7B 174.1(10) . . . . ?
C8B C7B C6B C1B 89.6(11) . . . . ?
C8B C7B C6B C5B -85.8(10) . . . . ?
C29B O1B C1B C6B 90.4(10) . . . . ?
Na3 O1B C1B C6B -92.0(9) . . . . ?
C29B O1B C1B C2B -91.6(10) . . . . ?
Na3 O1B C1B C2B 86.0(10) . . . . ?
C5B C6B C1B O1B -169.8(8) . . . . ?
C7B C6B C1B O1B 14.7(13) . . . . ?
C5B C6B C1B C2B 12.3(13) . . . . ?
C7B C6B C1B C2B -163.2(8) . . . . ?
C1B O1B C29B C30B -171.4(10) . . . . ?
Na3 O1B C29B C30B 10.5(11) . . . . ?
O1B C29B C30B O5B 2.6(19) . . . . ?
O1B C29B C30B O6B 178.7(13) . . . . ?
O6B C30B O5B Na2 27(3) . . . . ?
C29B C30B O5B Na2 -157.2(10) . . . . ?
O6B C30B O5B Na3 169.3(15) . . . . ?
C29B C30B O5B Na3 -15.4(19) . . . . ?
C6B C5B C4B C3B -7.4(16) . . . . ?
C5B C4B C3B C2B 5.8(16) . . . . ?
C4B C3B C2B C1B 4.6(13) . . . . ?
C4B C3B C2B C28B 179.0(9) . . . . ?
O1B C1B C2B C3B 168.5(8) . . . . ?
C6B C1B C2B C3B -13.6(14) . . . . ?
O1B C1B C2B C28B -6.1(13) . . . . ?
C6B C1B C2B C28B 171.8(8) . . . . ?
C15B C14B C10B C9B 106.2(12) . . . . ?
C15B C14B C10B C11B -72.8(12) . . . . ?
C31B O2B C9B C8B -93.0(11) . . . . ?
Na3 O2B C9B C8B 89.6(10) . . . . ?
C31B O2B C9B C10B 89.9(10) . . . . ?
Na3 O2B C9B C10B -87.4(9) . . . . ?
C11B C10B C9B C8B 5.7(15) . . . . ?
C14B C10B C9B C8B -173.5(9) . . . . ?
C11B C10B C9B O2B -177.4(7) . . . . ?
C14B C10B C9B O2B 3.5(14) . . . . ?
O2B C9B C8B C13B 177.7(8) . . . . ?
C10B C9B C8B C13B -5.4(15) . . . . ?
O2B C9B C8B C7B -4.4(14) . . . . ?
C10B C9B C8B C7B 172.4(9) . . . . ?
C6B C7B C8B C13B 76.8(11) . . . . ?
C6B C7B C8B C9B -101.1(11) . . . . ?
C9B C10B C11B C12B -6.6(15) . . . . ?
C14B C10B C11B C12B 172.6(10) . . . . ?
C10B C11B C12B C13B 6.7(16) . . . . ?
C9B C8B C13B C12B 5.4(15) . . . . ?
C7B C8B C13B C12B -172.6(9) . . . . ?
C11B C12B C13B C8B -6.0(15) . . . . ?
C9B O2B C31B C32B -159.0(9) . . . . ?
Na3 O2B C31B C32B 18.6(12) . . . . ?
Na2 O7B C32B O8B 57.9(14) . . . . ?
Na3 O7B C32B O8B 165.3(8) . . . . ?
Na2 O7B C32B C31B -123.3(9) . . . . ?
Na3 O7B C32B C31B -15.9(12) . . . . ?
O2B C31B C32B O7B -0.7(14) . . . . ?
O2B C31B C32B O8B 178.2(9) . . . . ?
C34B C33B O3B C16B -153.8(8) . . . . ?
C34B C33B O3B Na3 29.7(9) . . . . ?
Na3 O9B C34B O10B 162.7(8) . . . . ?
Na2 O9B C34B O10B 66.1(12) . . . . ?
Na3 O9B C34B C33B -15.6(12) . . . . ?
Na2 O9B C34B C33B -112.3(10) . . . . ?
Na2 O9B C34B Na3 -96.6(6) . . . . ?
O3B C33B C34B O9B -9.4(14) . . . . ?
O3B C33B C34B O10B 172.1(8) . . . . ?
O3B C33B C34B Na3 -20.8(6) . . . . ?
C33B O3B C16B C17B 91.5(9) . . . . ?
Na3 O3B C16B C17B -93.4(10) . . . . ?
C33B O3B C16B C15B -87.4(9) . . . . ?
Na3 O3B C16B C15B 87.7(10) . . . . ?
C17B C16B C15B C20B -7.3(14) . . . . ?
O3B C16B C15B C20B 171.5(7) . . . . ?
C17B C16B C15B C14B 168.3(9) . . . . ?
O3B C16B C15B C14B -13.0(13) . . . . ?
C10B C14B C15B C16B -91.2(12) . . . . ?
C10B C14B C15B C20B 84.1(11) . . . . ?
C15B C16B C17B C18B 9.5(14) . . . . ?
O3B C16B C17B C18B -169.2(7) . . . . ?
C15B C16B C17B C21B -171.9(8) . . . . ?
O3B C16B C17B C21B 9.4(12) . . . . ?
C19B C18B C17B C16B -6.5(13) . . . . ?
C19B C18B C17B C21B 174.9(8) . . . . ?
C22B C21B C17B C16B 91.9(10) . . . . ?
C22B C21B C17B C18B -89.5(10) . . . . ?
C17B C18B C19B C20B 2.0(15) . . . . ?
C18B C19B C20B C15B 0.1(16) . . . . ?
C16B C15B C20B C19B 2.0(14) . . . . ?
C14B C15B C20B C19B -173.7(9) . . . . ?
C3B C2B C28B C24B 83.7(11) . . . . ?
C1B C2B C28B C24B -102.0(10) . . . . ?
C26B C25B C24B C23B -2.4(16) . . . . ?
C26B C25B C24B C28B -179.6(10) . . . . ?
C2B C28B C24B C25B -75.3(12) . . . . ?
C2B C28B C24B C23B 107.4(9) . . . . ?
C35B O4B C23B C22B -73.7(9) . . . . ?
Na3 O4B C23B C22B 90.8(9) . . . . ?
C35B O4B C23B C24B 108.4(9) . . . . ?
Na3 O4B C23B C24B -87.1(9) . . . . ?
C25B C24B C23B O4B -175.7(8) . . . . ?
C28B C24B C23B O4B 1.7(13) . . . . ?
C25B C24B C23B C22B 6.4(14) . . . . ?
C28B C24B C23B C22B -176.1(8) . . . . ?
O4B C23B C22B C27B 176.2(7) . . . . ?
C24B C23B C22B C27B -5.9(13) . . . . ?
O4B C23B C22B C21B -7.9(12) . . . . ?
C24B C23B C22B C21B 170.0(8) . . . . ?
C17B C21B C22B C27B 76.8(11) . . . . ?
C17B C21B C22B C23B -98.8(11) . . . . ?
C23B C22B C27B C26B 1.6(14) . . . . ?
C21B C22B C27B C26B -174.3(8) . . . . ?
C24B C25B C26B C27B -2.0(17) . . . . ?
C22B C27B C26B C25B 2.4(16) . . . . ?
C23B O4B C35B C36B -132.8(10) . . . . ?
Na3 O4B C35B C36B 60.6(11) . . . . ?
O4B C35B C36B O12B -177.6(11) . . . . ?
O4B C35B C36B O11B 1(2) . . . . ?
C1C O1C C29C C30C -170.1(12) . . . . ?
Na4 O1C C29C C30C 2.6(13) . . . . ?
O5C C30C C29C O1C 44(2) . . . . ?
O6C C30C C29C O1C -174.0(12) . . . . ?
Na4 C30C C29C O1C -1.9(10) . . . . ?
Na5 C30C C29C O1C -25(3) . . . . ?
C29C O1C C1C C2C 82.6(12) . . . . ?
Na4 O1C C1C C2C -88.9(12) . . . . ?
C29C O1C C1C C6C -99.1(12) . . . . ?
Na4 O1C C1C C6C 89.4(11) . . . . ?
C2C C1C C6C C5C -4.7(18) . . . . ?
O1C C1C C6C C5C 177.1(10) . . . . ?
C2C C1C C6C C7C 172.5(11) . . . . ?
O1C C1C C6C C7C -5.7(16) . . . . ?
C1C C6C C7C C8C -101.6(14) . . . . ?
C5C C6C C7C C8C 75.2(16) . . . . ?
C6C C1C C2C C3C 6.7(18) . . . . ?
O1C C1C C2C C3C -175.2(10) . . . . ?
C6C C1C C2C C28C -168.5(11) . . . . ?
O1C C1C C2C C28C 9.7(17) . . . . ?
C1C C6C C5C C4C -1(2) . . . . ?
C7C C6C C5C C4C -178.3(14) . . . . ?
C6C C5C C4C C3C 4(2) . . . . ?
C5C C4C C3C C2C -2(2) . . . . ?
C1C C2C C3C C4C -3(2) . . . . ?
C28C C2C C3C C4C 172.5(12) . . . . ?
O6C C30C O5C Na4 177(2) . . . . ?
C29C C30C O5C Na4 -62.3(18) . . . . ?
Na5 C30C O5C Na4 83.6(6) . . . . ?
O6C C30C O5C Na5 93(2) . . . . ?
C29C C30C O5C Na5 -145.9(15) . . . . ?
Na4 C30C O5C Na5 -83.6(6) . . . . ?
C6C C7C C8C C9C 100.4(15) . . . . ?
C6C C7C C8C C13C -76.5(14) . . . . ?
C13C C8C C9C O2C -176.3(10) . . . . ?
C7C C8C C9C O2C 6.7(19) . . . . ?
C13C C8C C9C C10C 4(2) . . . . ?
C7C C8C C9C C10C -173.2(11) . . . . ?
C31C O2C C9C C8C 103.3(14) . . . . ?
Na4 O2C C9C C8C -84.6(14) . . . . ?
C31C O2C C9C C10C -76.8(13) . . . . ?
Na4 O2C C9C C10C 95.3(12) . . . . ?
C8C C9C C10C C11C -3.5(19) . . . . ?
O2C C9C C10C C11C 176.6(10) . . . . ?
C8C C9C C10C C14C 172.9(13) . . . . ?
O2C C9C C10C C14C -7.1(17) . . . . ?
C11C C10C C14C C15C 80.3(15) . . . . ?
C9C C10C C14C C15C -95.4(13) . . . . ?
C9C O2C C31C C32C -177.1(18) . . . . ?
Na4 O2C C31C C32C 9(2) . . . . ?
C9C C8C C13C C12C 1.5(19) . . . . ?
C7C C8C C13C C12C 178.6(12) . . . . ?
C8C C13C C12C C11C -7(2) . . . . ?
C13C C12C C11C C10C 8(3) . . . . ?
C14C C10C C11C C12C -179.7(18) . . . . ?
C9C C10C C11C C12C -3(2) . . . . ?
O2C C31C C32C O8C 140.0(14) . . . . ?
O2C C31C C32C O7C 43(2) . . . . ?
O2C C31C C32C Na4 -6.7(15) . . . . ?
Na4 O7C C32C C31C -70.3(19) . . . . ?
Na5 O7C C32C C31C -148.1(17) . . . . ?
Na4 O7C C32C O8C -171.0(9) . . . . ?
Na5 O7C C32C O8C 111.2(9) . . . . ?
Na5 O7C C32C Na4 -77.8(5) . . . . ?
C10C C14C C15C C16C 98.9(13) . . . . ?
C10C C14C C15C C20C -83.5(13) . . . . ?
C20C C15C C16C C17C 10.0(17) . . . . ?
C14C C15C C16C C17C -172.0(12) . . . . ?
C20C C15C C16C O3C -173.9(8) . . . . ?
C14C C15C C16C O3C 4.0(16) . . . . ?
C33C O3C C16C C17C -89.2(13) . . . . ?
Na4 O3C C16C C17C 82.5(12) . . . . ?
C33C O3C C16C C15C 94.5(11) . . . . ?
Na4 O3C C16C C15C -93.8(11) . . . . ?
C16C O3C C33C C34C 167.6(17) . . . . ?
Na4 O3C C33C C34C -6(2) . . . . ?
C15C C16C C17C C18C -6.3(18) . . . . ?
O3C C16C C17C C18C 177.9(8) . . . . ?
C15C C16C C17C C21C 168.7(11) . . . . ?
O3C C16C C17C C21C -7.1(17) . . . . ?
C22C C21C C17C C16C -96.7(13) . . . . ?
C22C C21C C17C C18C 78.3(12) . . . . ?
C16C C17C C18C C19C -2.3(18) . . . . ?
C21C C17C C18C C19C -177.6(12) . . . . ?
C17C C18C C19C C20C 5(2) . . . . ?
C18C C19C C20C C15C 0(2) . . . . ?
C16C C15C C20C C19C -6.6(19) . . . . ?
C14C C15C C20C C19C 175.4(13) . . . . ?
O3C C33C C34C O10C 166(2) . . . . ?
O3C C33C C34C O9C 47(2) . . . . ?
Na4 O9C C34C O10C 168.0(18) . . . . ?
Na5 O9C C34C O10C 84(2) . . . . ?
Na4 O9C C34C C33C -63.4(19) . . . . ?
Na5 O9C C34C C33C -147.8(13) . . . . ?
C1C C2C C28C C24C 96.8(13) . . . . ?
C3C C2C C28C C24C -78.2(14) . . . . ?
C2C C28C C24C C23C -92.2(14) . . . . ?
C2C C28C C24C C25C 76.3(14) . . . . ?
C23C C24C C25C C26C -1.4(17) . . . . ?
C28C C24C C25C C26C -170.2(11) . . . . ?
C24C C25C C26C C27C 2(2) . . . . ?
C25C C26C C27C C22C -1(2) . . . . ?
C26C C27C C22C C23C -0.3(17) . . . . ?
C26C C27C C22C C21C 175.7(12) . . . . ?
C17C C21C C22C C23C 98.8(13) . . . . ?
C17C C21C C22C C27C -76.8(12) . . . . ?
C25C C24C C23C C22C -0.2(19) . . . . ?
C28C C24C C23C C22C 168.1(10) . . . . ?
C25C C24C C23C O4C 174.9(9) . . . . ?
C28C C24C C23C O4C -16.8(17) . . . . ?
C27C C22C C23C C24C 1.1(18) . . . . ?
C21C C22C C23C C24C -174.5(11) . . . . ?
C27C C22C C23C O4C -174.3(9) . . . . ?
C21C C22C C23C O4C 10.0(16) . . . . ?
C35C O4C C23C C24C -83.2(13) . . . . ?
Na4 O4C C23C C24C 93.3(12) . . . . ?
C35C O4C C23C C22C 92.4(12) . . . . ?
Na4 O4C C23C C22C -91.1(10) . . . . ?
C23C O4C C35C C36C -175.4(15) . . . . ?
Na4 O4C C35C C36C 7.7(17) . . . . ?
O4C C35C C36C O12C 178.7(18) . . . . ?
O4C C35C C36C O11C 48(2) . . . . ?
Na4 O11C C36C O12C 168.6(18) . . . . ?
Na5 O11C C36C O12C 96.5(19) . . . . ?
Na4 O11C C36C C35C -67.2(17) . . . . ?
Na5 O11C C36C C35C -139.3(16) . . . . ?
C8D C7D C6D C1D 93(2) . . . . ?
C8D C7D C6D C5D -82.2(18) . . . . ?
C5D C6D C1D C2D 0(3) . . . . ?
C7D C6D C1D C2D -175.3(15) . . . . ?
C5D C6D C1D O1D -171.2(12) . . . . ?
C7D C6D C1D O1D 14(2) . . . . ?
C29D O1D C1D C2D -86(3) . . . . ?
Na6 O1D C1D C2D 90(2) . . . . ?
C29D O1D C1D C6D 83.5(19) . . . . ?
Na6 O1D C1D C6D -101(2) . . . . ?
C6D C1D C2D C3D 1(3) . . . . ?
O1D C1D C2D C3D 171.2(17) . . . . ?
C6D C1D C2D C28D 169.5(16) . . . . ?
O1D C1D C2D C28D -21(3) . . . . ?
C1D C6D C5D C4D 3(2) . . . . ?
C7D C6D C5D C4D 177.7(14) . . . . ?
C6D C5D C4D C3D -6(3) . . . . ?
C5D C4D C3D C2D 7(3) . . . . ?
C1D C2D C3D C4D -5(3) . . . . ?
C28D C2D C3D C4D -173.4(19) . . . . ?
C1D O1D C29D C30D -155(3) . . . . ?
Na6 O1D C29D C30D 29(3) . . . . ?
C1D O1D C29D Na6 176.9(17) . . . . ?
O1D C29D C30D O6D -129(3) . . . . ?
Na6 C29D C30D O6D -111(3) . . . . ?
O1D C29D C30D O5D -16(4) . . . . ?
Na6 C29D C30D O5D 3(2) . . . . ?
Na6 O5D C30D O6D 121(2) . . . . ?
Na5 O5D C30D O6D 12(4) . . . . ?
Na6 O5D C30D C29D -5(3) . . . . ?
Na5 O5D C30D C29D -114(2) . . . . ?
C15D C14D C10D C9D 92(2) . . . . ?
C15D C14D C10D C11D -82(2) . . . . ?
C14D C10D C9D C8D -173.4(16) . . . . ?
C11D C10D C9D C8D 1(2) . . . . ?
C14D C10D C9D O2D 19(2) . . . . ?
C11D C10D C9D O2D -167.2(12) . . . . ?
O2D C9D C8D C7D -18(2) . . . . ?
C10D C9D C8D C7D 175.7(14) . . . . ?
O2D C9D C8D C13D 171.9(14) . . . . ?
C10D C9D C8D C13D 5(2) . . . . ?
C6D C7D C8D C9D -95.4(17) . . . . ?
C6D C7D C8D C13D 75(2) . . . . ?
C9D C10D C11D C12D -1(2) . . . . ?
C14D C10D C11D C12D 173.7(15) . . . . ?
C10D C11D C12D C13D -5(2) . . . . ?
C11D C12D C13D C8D 11(3) . . . . ?
C9D C8D C13D C12D -11(2) . . . . ?
C7D C8D C13D C12D 179.3(14) . . . . ?
C8D C9D O2D C31D -79(2) . . . . ?
C10D C9D O2D C31D 89(2) . . . . ?
C8D C9D O2D Na6 90.9(18) . . . . ?
C10D C9D O2D Na6 -101.2(15) . . . . ?
C9D O2D C31D C32D -167.3(18) . . . . ?
Na6 O2D C31D C32D 21(2) . . . . ?
C9D O2D C31D Na6 172(2) . . . . ?
O2D C31D C32D O7D 25(3) . . . . ?
Na6 C31D C32D O7D 41(2) . . . . ?
O2D C31D C32D O8D -129(3) . . . . ?
Na6 C31D C32D O8D -113(3) . . . . ?
O2D C31D C32D Na6 -16.7(18) . . . . ?
O2D C31D C32D Na5 -42(3) . . . . ?
Na6 C31D C32D Na5 -25.2(17) . . . . ?
O8D C32D O7D Na6 105(3) . . . . ?
C31D C32D O7D Na6 -50(2) . . . . ?
Na5 C32D O7D Na6 80.5(5) . . . . ?
O8D C32D O7D Na5 25(3) . . . . ?
C31D C32D O7D Na5 -131(2) . . . . ?
Na6 C32D O7D Na5 -80.5(5) . . . . ?
O7D C32D O8D Na5 -22(3) . . . . ?
C31D C32D O8D Na5 133(3) . . . . ?
Na6 C32D O8D Na5 42.7(13) . . . . ?
C22D C21D C17D C16D 93(2) . . . . ?
C22D C21D C17D C18D -94(2) . . . . ?
C21D C17D C16D C15D -178.8(19) . . . . ?
C18D C17D C16D C15D 7(2) . . . . ?
C21D C17D C16D O3D 4(3) . . . . ?
C18D C17D C16D O3D -170.8(13) . . . . ?
O3D C16D C15D C20D 174.4(15) . . . . ?
C17D C16D C15D C20D -3(3) . . . . ?
O3D C16D C15D C14D -24(3) . . . . ?
C17D C16D C15D C14D 159.2(19) . . . . ?
C10D C14D C15D C16D -82(3) . . . . ?
C10D C14D C15D C20D 82(2) . . . . ?
C16D C17D C18D C19D -3(3) . . . . ?
C21D C17D C18D C19D -178(2) . . . . ?
C17D C18D C19D C20D -4(3) . . . . ?
C16D C15D C20D C19D -5(3) . . . . ?
C14D C15D C20D C19D -167.8(16) . . . . ?
C18D C19D C20D C15D 8(3) . . . . ?
C15D C16D O3D C33D -95(2) . . . . ?
C17D C16D O3D C33D 83(2) . . . . ?
C15D C16D O3D Na6 94(2) . . . . ?
C17D C16D O3D Na6 -89(2) . . . . ?
C16D O3D C33D C34D -163(3) . . . . ?
Na6 O3D C33D C34D 10(3) . . . . ?
Na5 O10D C34D O9D -43(4) . . . . ?
Na5 O10D C34D C33D 133(7) . . . . ?
Na5 O10D C34D Na6 16(3) . . . . ?
O3D C33D C34D O9D 35(6) . . . . ?
O3D C33D C34D O10D -140(7) . . . . ?
O3D C33D C34D Na6 -8(2) . . . . ?
O3D C33D C34D Na5 -38(4) . . . . ?
O10D C34D O9D Na5 47(4) . . . . ?
C33D C34D O9D Na5 -130(4) . . . . ?
Na6 C34D O9D Na5 -78.2(8) . . . . ?
O10D C34D O9D Na6 125(4) . . . . ?
C33D C34D O9D Na6 -52(5) . . . . ?
Na5 C34D O9D Na6 78.2(8) . . . . ?
C1D C2D C28D C24D -83(2) . . . . ?
C3D C2D C28D C24D 86.2(19) . . . . ?
C2D C28D C24D C23D 91(2) . . . . ?
C2D C28D C24D C25D -79.5(19) . . . . ?
C25D C24D C23D O4D -169(2) . . . . ?
C28D C24D C23D O4D 23(4) . . . . ?
C25D C24D C23D C22D -8(4) . . . . ?
C28D C24D C23D C22D -174.8(19) . . . . ?
C24D C23D O4D C35D 50(4) . . . . ?
C22D C23D O4D C35D -114(2) . . . . ?
C24D C23D O4D Na6 -92(3) . . . . ?
C22D C23D O4D Na6 104.9(18) . . . . ?
C23D C24D C25D C26D 0(4) . . . . ?
C28D C24D C25D C26D 168(2) . . . . ?
C23D O4D C35D C36D -142(3) . . . . ?
Na6 O4D C35D C36D 7(4) . . . . ?
C23D O4D C35D Na6 -149(2) . . . . ?
C24D C23D C22D C27D 14(3) . . . . ?
O4D C23D C22D C27D -179.4(18) . . . . ?
C24D C23D C22D C21D 178(2) . . . . ?
O4D C23D C22D C21D -16(3) . . . . ?
C17D C21D C22D C27D 71(3) . . . . ?
C17D C21D C22D C23D -91(3) . . . . ?
C24D C25D C26D C27D 0(3) . . . . ?
C23D C22D C27D C26D -16(4) . . . . ?
C21D C22D C27D C26D 179(2) . . . . ?
C25D C26D C27D C22D 10(4) . . . . ?
Na5 O11D C36D O12D 58(6) . . . . ?
Na6 O11D C36D O12D 138(5) . . . . ?
Na5 O11D C36D C35D -107.8(19) . . . . ?
Na6 O11D C36D C35D -28(2) . . . . ?
O4D C35D C36D O11D 18(5) . . . . ?
Na6 C35D C36D O11D 24(2) . . . . ?
O4D C35D C36D O12D -148(5) . . . . ?
Na6 C35D C36D O12D -143(5) . . . . ?

_refine_diff_density_max         0.498
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.100

_shelxl_version_number           2014-3




# start Validation Reply Form
_vrf_RFACR01_free_calix4tube_2   
;
PROBLEM: The value of the weighted R factor is > 0.35
RESPONSE: This error message appears because crystal is very weakly diffracting (Ratio Observed / Unique Reflections is only 19%). In this way, a large amount of almost null reflections not being systematic absence are used in the refinement, yielding a bad statistic figure of merit.
;
_vrf_PLAT026_free_calix4tube_2   
;
PROBLEM: Ratio Observed / Unique Reflections too Low ....         19 %     
RESPONSE: This has resulted in almost all other alerts for this structure and it had occurred because crystal is very weakly diffracting besides loosing quickly solvent when away from mother solution, leading to decrease of long-range order.
;
_vrf_PLAT029_free_calix4tube_2   
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.939 Note  
RESPONSE: This error message appears because crystal is very weakly diffracting even at medium resolution shell (Ratio Observed / Unique Reflections is only 19%). Therefore, high-angle reflections with angles near to 25 were not possible to be measured. 
;
_vrf_PLAT241_free_calix4tube_2   
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of       O10D Check 
RESPONSE: This error message appears because of static disorder mainly involving some carboxyl moieties in the structure probably due to the fact that crystal looses solvent away from mother solution resulting in decrease of long-range order. However, it was not possible a split-atom refinement on the basis of poor quality data from the very weakly diffracting crystal (Ratio Observed / Unique Reflections is only 19%). High correlation between ADPs and SOFs as well as unstable refinements were observed when attempting the classical split-atom approach to these disordered moieties. Therefore, carboxyl hydrogens riding on their parent oxygens had high ADPs compared to all others.
;
_vrf_PLAT242_free_calix4tube_2   
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of       C36D Check 
RESPONSE: This error message appears because of static disorder mainly involving some carboxyl moieties in the structure probably due to the fact that crystal looses solvent away from mother solution resulting in decrease of long-range order. However, it was not possible a split-atom refinement on the basis of poor quality data from the very weakly diffracting crystal (Ratio Observed / Unique Reflections is only 19%). High correlation between ADPs and SOFs as well as unstable refinements were observed when attempting the classical split-atom approach to these disordered moieties. Therefore, carboxyl hydrogens riding on their parent oxygens had high ADPs compared to all others.
;
_vrf_PLAT602_free_calix4tube_2   
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info 
RESPONSE: In this structure, smeared electronic density as low electron density peaks in the difference Fourier map was found, which refer probably to non-stoichiometric loosing solvent molecules. However, their assignment was not possible and the data was squeezed using Platon.
;
_vrf_PLAT084_free_calix4tube_2   
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.41 Report
RESPONSE: This error message appears because crystal is very weakly diffracting (Ratio Observed / Unique Reflections is only 19%). In this way, a large amount of almost null reflections not being systematic absence are used in the refinement, yielding a bad statistic figure of merit.
;
_vrf_PLAT201_free_calix4tube_2   
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         8 Report
RESPONSE: This error message appears because high correlation between ADPs and SOFs and unstable refinements were observed when refining anisotropically the carboxyl/carboxylate oxygens and carbons of calixarene subunits C and D. Therefore, they were refined isotropically.
;
_vrf_PLAT220_free_calix4tube_2   
;
PROBLEM: Non-Solvent Resd 1   O   Ueq(max)/Ueq(min) Range        7.3 Ratio
RESPONSE: This error message appears because of static disorder mainly involving some carboxyl moieties in the structure probably due to the fact that crystal looses solvent away from mother solution resulting in decrease of long-range order. However, it was not possible a split-atom refinement on the basis of poor quality data from the very weakly diffracting crystal (Ratio Observed / Unique Reflections is only 19%). High correlation between ADPs and SOFs as well as unstable refinements were observed when attempting the classical split-atom approach to these disordered moieties.
;
_vrf_PLAT340_free_calix4tube_2   
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.02018 Ang.  
RESPONSE: This error message appears because crystal is very weakly diffracting (Ratio Observed / Unique Reflections is only 19%). In this way, a large amount of unobserved reflections in practice are being used in the refinement, resulting in low precision on atom positions.
;
_vrf_PLAT417_free_calix4tube_2   
;
PROBLEM: Short Inter D-H..H-D       H1W    ..  H12O    ..       2.06 Ang.  
RESPONSE: This error message appears because the close crystal packing. Concerning these hydrogen positions assignment, they were calculated using CALC-OH and carefully checked after their positioning. These hydrogens are suitably pointed towards hydrogen bonding acceptors. Therefore, there is no problem of assigning its position.
;
_vrf_PLAT420_free_calix4tube_2   
;
PROBLEM: D-H Without Acceptor        O6A    -   H6A    ..     Please Check 
RESPONSE: This error message appears because this OH group is only involved in weak contacts instead of classical hydrogen bonds. 
;
_vrf_PLAT334_free_calix4tube_2   
;
PROBLEM: Small Average Benzene  C-C Dist. C15A   -C20A          1.34 Ang.  
RESPONSE: This alert occurs because of the poor quality of extremely weak intensity data leading to high uncertainty in C-C bond lengths.
;
_vrf_PLAT911_free_calix4tube_2   
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L=  0.600       1915 Report
RESPONSE: This error message appears because crystal is very weakly diffracting (Ratio Observed / Unique Reflections is only 19%). It seems to loose quickly solvent when away from mother solution, undergoing decrease of long-
range order, which is refelected in its poor diffracting ability.
;
_vrf_PLAT934_free_calix4tube_2   
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....          5 Check 
RESPONSE: This is caused because of a large amount of almost null reflections not being systematic absence are used in the refinement.
;
_vrf_PLAT990_free_calix4tube_2   
;
PROBLEM: Depricated RES file style based SQUEEZE job ...           ! Note 
RESPONSE: SQUEEZE was applied to intensity data because smeared electronic density as low electron density peaks in the difference Fourier map was found, which refer probably to non-stoichiometric loosing solvent molecules (most probably water and methanol) unable to be properly modeled.
;
# end Validation Reply Form

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 -0.017 0.000 1782 519 ' '
2 0.323 0.924 0.405 151 50 ' '
3 0.677 0.076 0.595 151 50 ' '
_platon_squeeze_details          
;
The unit cell contains an unknown number of solvent molecules (most probably water and methanol) which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. 
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_pol_calix4tube_3
_database_code_depnum_ccdc_archive 'CCDC 1433708'
_audit_update_record             
;
2016-07-19 deposited with the CCDC.
2016-08-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C76 H72 Na4 O26 S2'
_chemical_formula_weight         1557.42

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'
Na Na 0.0362 0.0249 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           106
_space_group_name_H-M_alt        'P 42 b c'
_space_group_name_Hall           'P 4c -2ab'

_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'
'-y, x, z+1/2'
'y, -x, z+1/2'
'-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'

_cell_length_a                   21.041(4)
_cell_length_b                   21.041(4)
_cell_length_c                   16.456(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7286(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    41778
_cell_measurement_theta_min      1.94
_cell_measurement_theta_max      25.13


_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3248
_exptl_absorpt_coefficient_mu    0.181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'Blessing, R. H. (1995) Acta Cryst., A51, 33-38'
_exptl_absorpt_correction_T_min  0.913
_exptl_absorpt_correction_T_max  0.991

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_reflns_number            41778
_diffrn_reflns_av_unetI/netI     0.1843
_diffrn_reflns_av_R_equivalents  0.2484
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.936
_diffrn_reflns_theta_max         25.135
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 0.979
_reflns_number_total             6333
_reflns_number_gt                2947
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.880
_reflns_Friedel_fraction_max     0.946
_reflns_Friedel_fraction_full    0.957

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0581P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 959 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.23(19)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6333
_refine_ls_number_parameters     490
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1946
_refine_ls_R_factor_gt           0.0689
_refine_ls_wR_factor_ref         0.1666
_refine_ls_wR_factor_gt          0.1234
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_restrained_S_all      0.973
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Na1 Na 0.54031(18) 1.15469(17) 0.9433(2) 0.0418(10) Uani 1 1 d . . . . .
Na2 Na 0.5000 1.0000 0.9474(4) 0.0597(16) Uani 1 2 d S T P . .
Na3 Na 0.5000 1.0000 0.6995(7) 0.135(3) Uani 1 2 d S T P . .
O1 O 0.4671(3) 1.2201(3) 1.0282(4) 0.0409(17) Uani 1 1 d . . . . .
O6 O 0.3667(3) 1.0895(3) 1.0718(4) 0.0497(19) Uani 1 1 d . . . . .
O5 O 0.4721(4) 1.0946(3) 1.0683(5) 0.064(2) Uani 1 1 d . . . . .
C2 C 0.4967(5) 1.3063(5) 1.1119(6) 0.040(3) Uani 1 1 d . . . . .
C30 C 0.4201(6) 1.1190(5) 1.0661(6) 0.044(3) Uani 1 1 d . . . . .
C1 C 0.4670(5) 1.2853(5) 1.0424(6) 0.035(2) Uani 1 1 d . . . . .
C6 C 0.4345(5) 1.3259(5) 0.9904(6) 0.038(3) Uani 1 1 d . . . . .
C3 C 0.4934(6) 1.3706(5) 1.1293(6) 0.050(3) Uani 1 1 d . . . . .
H3 H 0.5135 1.3861 1.1756 0.060 Uiso 1 1 calc R U . . .
C29 C 0.4122(5) 1.1894(5) 1.0583(7) 0.054(3) Uani 1 1 d . . . . .
H29A H 0.3769 1.1981 1.0221 0.064 Uiso 1 1 calc R U . . .
H29B H 0.4018 1.2070 1.1112 0.064 Uiso 1 1 calc R U . . .
C7 C 0.4098(5) 1.3046(5) 0.9086(6) 0.047(3) Uani 1 1 d . . . . .
H7A H 0.4028 1.2590 0.9094 0.056 Uiso 1 1 calc R U . . .
H7B H 0.3694 1.3251 0.8978 0.056 Uiso 1 1 calc R U . . .
C5 C 0.4318(5) 1.3896(5) 1.0099(6) 0.052(3) Uani 1 1 d . . . . .
H5 H 0.4102 1.4176 0.9760 0.062 Uiso 1 1 calc R U . . .
C4 C 0.4610(6) 1.4120(6) 1.0791(7) 0.060(3) Uani 1 1 d . . . . .
H4 H 0.4588 1.4550 1.0921 0.071 Uiso 1 1 calc R U . . .
O2 O 0.4937(3) 1.2140(3) 0.8380(4) 0.0342(16) Uani 1 1 d . . . . .
O7 O 0.4519(3) 1.0988(3) 0.8883(4) 0.055(2) Uani 1 1 d . . . . .
O8 O 0.4018(4) 1.0830(4) 0.7710(5) 0.070(3) Uani 1 1 d . . . . .
H8 H 0.3924 1.0488 0.7917 0.105 Uiso 1 1 calc R U . . .
C8 C 0.4555(5) 1.3207(5) 0.8431(5) 0.036(3) Uani 1 1 d . . . . .
C9 C 0.4997(5) 1.2766(4) 0.8134(5) 0.035(2) Uani 1 1 d . . . . .
C32 C 0.4364(5) 1.1149(5) 0.8204(7) 0.042(3) Uani 1 1 d . . . . .
C14 C 0.6012(5) 1.2482(5) 0.7364(6) 0.049(3) Uani 1 1 d . . . . .
H14A H 0.5875 1.2048 0.7462 0.059 Uiso 1 1 calc R U . . .
H14B H 0.6101 1.2525 0.6788 0.059 Uiso 1 1 calc R U . . .
C10 C 0.5479(5) 1.2936(5) 0.7597(5) 0.039(3) Uani 1 1 d . . . . .
C31 C 0.4541(5) 1.1774(5) 0.7842(6) 0.049(3) Uani 1 1 d . . . . .
H31A H 0.4764 1.1703 0.7334 0.059 Uiso 1 1 calc R U . . .
H31B H 0.4157 1.2012 0.7723 0.059 Uiso 1 1 calc R U . . .
C11 C 0.5494(6) 1.3566(5) 0.7332(7) 0.053(3) Uani 1 1 d . . . . .
H11 H 0.5807 1.3694 0.6968 0.064 Uiso 1 1 calc R U . . .
C12 C 0.5063(6) 1.3990(5) 0.7592(7) 0.057(3) Uani 1 1 d . . . . .
H12 H 0.5079 1.4404 0.7395 0.069 Uiso 1 1 calc R U . . .
C13 C 0.4597(5) 1.3830(5) 0.8143(7) 0.048(3) Uani 1 1 d . . . . .
H13 H 0.4311 1.4136 0.8322 0.057 Uiso 1 1 calc R U . . .
O9 O 0.5728(4) 1.0738(4) 0.8106(5) 0.069(2) Uani 1 1 d . . . . .
O3 O 0.6404(3) 1.1730(3) 0.8709(3) 0.0405(18) Uani 1 1 d . . . . .
O10 O 0.6569(3) 1.0105(3) 0.8168(5) 0.059(2) Uani 1 1 d . . . . .
C16 C 0.6753(5) 1.2287(5) 0.8545(7) 0.046(3) Uani 1 1 d . . . . .
C33 C 0.6737(5) 1.1165(5) 0.8454(7) 0.055(3) Uani 1 1 d . . . . .
H33A H 0.7011 1.1020 0.8891 0.066 Uiso 1 1 calc R U . . .
H33B H 0.7003 1.1264 0.7990 0.066 Uiso 1 1 calc R U . . .
C34 C 0.6287(5) 1.0647(5) 0.8232(6) 0.040(3) Uani 1 1 d . . . . .
C15 C 0.6617(6) 1.2610(5) 0.7844(7) 0.048(3) Uani 1 1 d . . . . .
C17 C 0.7235(5) 1.2466(5) 0.9078(7) 0.051(3) Uani 1 1 d . . . . .
C21 C 0.7314(5) 1.2154(6) 0.9907(6) 0.060(4) Uani 1 1 d . . . . .
H21A H 0.7133 1.1731 0.9890 0.072 Uiso 1 1 calc R U . . .
H21B H 0.7764 1.2113 1.0027 0.072 Uiso 1 1 calc R U . . .
C20 C 0.7012(6) 1.3124(6) 0.7641(8) 0.062(4) Uani 1 1 d . . . . .
H20 H 0.6932 1.3359 0.7174 0.074 Uiso 1 1 calc R U . . .
C19 C 0.7513(6) 1.3277(6) 0.8129(10) 0.073(4) Uani 1 1 d . . . . .
H19 H 0.7793 1.3595 0.7965 0.087 Uiso 1 1 calc R U . . .
C18 C 0.7612(6) 1.2984(6) 0.8830(9) 0.070(4) Uani 1 1 d . . . . .
H18 H 0.7938 1.3124 0.9166 0.084 Uiso 1 1 calc R U . . .
O11 O 0.5922(3) 1.0628(3) 0.9932(4) 0.0451(18) Uani 1 1 d . . . . .
O4 O 0.6097(3) 1.1836(3) 1.0527(4) 0.0384(17) Uani 1 1 d . . . . .
C23 C 0.6391(5) 1.2382(5) 1.0846(6) 0.037(3) Uani 1 1 d . . . . .
C36 C 0.6109(5) 1.0672(5) 1.0628(7) 0.044(3) Uani 1 1 d . . . . .
C22 C 0.7002(5) 1.2525(5) 1.0567(7) 0.050(3) Uani 1 1 d . . . . .
O12 O 0.6239(5) 1.0225(4) 1.1107(5) 0.082(3) Uani 1 1 d . . . . .
H12O H 0.6192 0.9884 1.0873 0.124 Uiso 1 1 calc R U . . .
C24 C 0.6075(5) 1.2732(5) 1.1424(6) 0.042(3) Uani 1 1 d . . . . .
C35 C 0.6191(6) 1.1295(5) 1.1047(6) 0.051(3) Uani 1 1 d . . . . .
H35A H 0.5892 1.1319 1.1495 0.061 Uiso 1 1 calc R U . . .
H35B H 0.6616 1.1315 1.1273 0.061 Uiso 1 1 calc R U . . .
C28 C 0.5391(5) 1.2635(5) 1.1635(6) 0.044(3) Uani 1 1 d . . . . .
H28A H 0.5325 1.2730 1.2206 0.053 Uiso 1 1 calc R U . . .
H28B H 0.5276 1.2194 1.1545 0.053 Uiso 1 1 calc R U . . .
C27 C 0.7294(6) 1.3048(6) 1.0918(9) 0.068(4) Uani 1 1 d . . . . .
H27 H 0.7695 1.3171 1.0740 0.081 Uiso 1 1 calc R U . . .
C26 C 0.7000(7) 1.3389(6) 1.1525(8) 0.074(4) Uani 1 1 d . . . . .
H26 H 0.7215 1.3720 1.1778 0.088 Uiso 1 1 calc R U . . .
C25 C 0.6391(6) 1.3243(6) 1.1758(7) 0.062(3) Uani 1 1 d . . . . .
H25 H 0.6189 1.3492 1.2147 0.075 Uiso 1 1 calc R U . . .
S1S S 0.1855(2) 1.0338(2) 0.8968(3) 0.1221(18) Uani 1 1 d . . . . .
O1S O 0.1620(6) 0.9697(5) 0.8767(7) 0.141(5) Uani 1 1 d . . . . .
C2S C 0.1245(7) 1.0764(9) 0.9443(12) 0.145(7) Uani 1 1 d . . . . .
H2S1 H 0.1113 1.0542 0.9924 0.217 Uiso 1 1 calc R U . . .
H2S2 H 0.0892 1.0803 0.9078 0.217 Uiso 1 1 calc R U . . .
H2S3 H 0.1396 1.1179 0.9588 0.217 Uiso 1 1 calc R U . . .
C1S C 0.2302(10) 1.0250(9) 0.9822(13) 0.179(10) Uani 1 1 d . . . . .
H1S1 H 0.2645 0.9961 0.9714 0.269 Uiso 1 1 calc R U . . .
H1S2 H 0.2042 1.0083 1.0251 0.269 Uiso 1 1 calc R U . . .
H1S3 H 0.2471 1.0654 0.9981 0.269 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Na1 O2 2.350(7) . ?
Na1 O11 2.366(8) . ?
Na1 O7 2.379(8) . ?
Na1 O4 2.396(7) . ?
Na1 O3 2.449(7) . ?
Na1 O1 2.494(8) . ?
Na1 O5 2.809(9) . ?
Na1 O9 2.851(9) . ?
Na1 C36 3.075(12) . ?
Na1 C32 3.093(12) . ?
Na1 Na2 3.364(4) . ?
Na2 O11 2.465(7) 2_675 ?
Na2 O11 2.465(7) . ?
Na2 O7 2.508(8) 2_675 ?
Na2 O7 2.508(8) . ?
Na2 O5 2.875(10) 2_675 ?
Na2 O5 2.875(10) . ?
Na2 Na1 3.364(4) 2_675 ?
Na3 O9 2.847(10) . ?
Na3 O9 2.847(10) 2_675 ?
Na3 O8 2.951(10) 2_675 ?
Na3 O5 2.994(11) 8_664 ?
Na3 O5 2.994(11) 7_454 ?
O1 C1 1.391(11) . ?
O1 C29 1.412(11) . ?
O6 C30 1.287(12) . ?
O5 C30 1.210(12) . ?
O5 Na3 2.994(11) 7_455 ?
C2 C1 1.375(13) . ?
C2 C3 1.385(13) . ?
C2 C28 1.526(14) . ?
C30 C29 1.497(13) . ?
C1 C6 1.389(14) . ?
C6 C5 1.380(13) . ?
C6 C7 1.511(14) . ?
C3 C4 1.381(15) . ?
C7 C8 1.484(13) . ?
C5 C4 1.377(15) . ?
O2 C9 1.383(10) . ?
O2 C31 1.440(11) . ?
O7 C32 1.211(12) . ?
O8 C32 1.282(12) . ?
C8 C13 1.398(13) . ?
C8 C9 1.402(13) . ?
C9 C10 1.392(14) . ?
C32 C31 1.491(14) . ?
C14 C15 1.522(15) . ?
C14 C10 1.523(14) . ?
C10 C11 1.397(13) . ?
C11 C12 1.342(15) . ?
C12 C13 1.376(15) . ?
O9 C34 1.209(12) . ?
O3 C16 1.411(11) . ?
O3 C33 1.442(11) . ?
O10 C34 1.289(12) . ?
C16 C15 1.369(14) . ?
C16 C17 1.391(14) . ?
C33 C34 1.489(14) . ?
C15 C20 1.404(15) . ?
C17 C18 1.409(16) . ?
C17 C21 1.523(14) . ?
C21 C22 1.489(14) . ?
C20 C19 1.364(17) . ?
C19 C18 1.324(16) . ?
O11 C36 1.215(12) . ?
O4 C23 1.406(11) . ?
O4 C35 1.437(11) . ?
C23 C24 1.374(13) . ?
C23 C22 1.400(14) . ?
C36 O12 1.259(12) . ?
C36 C35 1.492(14) . ?
C22 C27 1.385(15) . ?
C24 C25 1.379(15) . ?
C24 C28 1.496(15) . ?
C27 C26 1.376(16) . ?
C26 C25 1.372(16) . ?
S1S O1S 1.475(10) . ?
S1S C1S 1.700(19) . ?
S1S C2S 1.749(17) . ?

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
_geom_angle_publ_flag
O2 Na1 O11 151.9(3) . . ?
O2 Na1 O7 69.9(3) . . ?
O11 Na1 O7 95.1(3) . . ?
O2 Na1 O4 132.3(3) . . ?
O11 Na1 O4 70.5(2) . . ?
O7 Na1 O4 152.6(3) . . ?
O2 Na1 O3 85.2(2) . . ?
O11 Na1 O3 84.3(2) . . ?
O7 Na1 O3 124.4(3) . . ?
O4 Na1 O3 78.6(2) . . ?
O2 Na1 O1 82.1(2) . . ?
O11 Na1 O1 122.8(3) . . ?
O7 Na1 O1 90.2(3) . . ?
O4 Na1 O1 79.4(2) . . ?
O3 Na1 O1 135.8(3) . . ?
O2 Na1 O5 124.5(3) . . ?
O11 Na1 O5 67.3(2) . . ?
O7 Na1 O5 69.9(3) . . ?
O4 Na1 O5 82.8(3) . . ?
O3 Na1 O5 150.0(3) . . ?
O1 Na1 O5 61.5(2) . . ?
O2 Na1 O9 81.5(3) . . ?
O11 Na1 O9 70.6(2) . . ?
O7 Na1 O9 66.5(3) . . ?
O4 Na1 O9 125.5(3) . . ?
O3 Na1 O9 61.0(2) . . ?
O1 Na1 O9 155.0(3) . . ?
O5 Na1 O9 114.5(3) . . ?
O2 Na1 C36 172.2(3) . . ?
O11 Na1 C36 21.1(2) . . ?
O7 Na1 C36 109.0(3) . . ?
O4 Na1 C36 51.5(3) . . ?
O3 Na1 C36 89.4(3) . . ?
O1 Na1 C36 105.7(3) . . ?
O5 Na1 C36 60.6(3) . . ?
O9 Na1 C36 91.0(3) . . ?
O2 Na1 C32 50.7(3) . . ?
O11 Na1 C32 109.3(3) . . ?
O7 Na1 C32 20.8(2) . . ?
O4 Na1 C32 172.0(3) . . ?
O3 Na1 C32 109.4(3) . . ?
O1 Na1 C32 94.5(3) . . ?
O5 Na1 C32 89.8(3) . . ?
O9 Na1 C32 60.5(3) . . ?
C36 Na1 C32 126.7(3) . . ?
O2 Na1 Na2 115.0(2) . . ?
O11 Na1 Na2 47.08(19) . . ?
O7 Na1 Na2 48.1(2) . . ?
O4 Na1 Na2 112.6(2) . . ?
O3 Na1 Na2 112.23(19) . . ?
O1 Na1 Na2 111.5(2) . . ?
O5 Na1 Na2 54.6(2) . . ?
O9 Na1 Na2 59.9(2) . . ?
C36 Na1 Na2 62.0(2) . . ?
C32 Na1 Na2 64.7(2) . . ?
O11 Na2 O11 144.4(4) 2_675 . ?
O11 Na2 O7 89.5(2) 2_675 2_675 ?
O11 Na2 O7 104.2(2) . 2_675 ?
O11 Na2 O7 104.2(2) 2_675 . ?
O11 Na2 O7 89.5(2) . . ?
O7 Na2 O7 134.4(5) 2_675 . ?
O11 Na2 O5 65.0(2) 2_675 2_675 ?
O11 Na2 O5 89.9(3) . 2_675 ?
O7 Na2 O5 67.2(2) 2_675 2_675 ?
O7 Na2 O5 157.6(3) . 2_675 ?
O11 Na2 O5 89.9(3) 2_675 . ?
O11 Na2 O5 65.0(2) . . ?
O7 Na2 O5 157.6(3) 2_675 . ?
O7 Na2 O5 67.2(2) . . ?
O5 Na2 O5 92.4(4) 2_675 . ?
O11 Na2 Na1 44.68(17) 2_675 2_675 ?
O11 Na2 Na1 136.33(19) . 2_675 ?
O7 Na2 Na1 44.92(17) 2_675 2_675 ?
O7 Na2 Na1 133.8(2) . 2_675 ?
O5 Na2 Na1 52.81(17) 2_675 2_675 ?
O5 Na2 Na1 129.2(2) . 2_675 ?
O11 Na2 Na1 136.32(19) 2_675 . ?
O11 Na2 Na1 44.68(17) . . ?
O7 Na2 Na1 133.8(2) 2_675 . ?
O7 Na2 Na1 44.92(17) . . ?
O5 Na2 Na1 129.2(2) 2_675 . ?
O5 Na2 Na1 52.81(17) . . ?
Na1 Na2 Na1 177.7(3) 2_675 . ?
O11 Na2 Na3 107.8(2) 2_675 . ?
O11 Na2 Na3 107.8(2) . . ?
O7 Na2 Na3 67.2(2) 2_675 . ?
O7 Na2 Na3 67.2(2) . . ?
O5 Na2 Na3 133.82(19) 2_675 . ?
O5 Na2 Na3 133.82(19) . . ?
Na1 Na2 Na3 88.86(13) 2_675 . ?
Na1 Na2 Na3 88.86(13) . . ?
O11 Na2 Na3 72.2(2) 2_675 7_455 ?
O11 Na2 Na3 72.2(2) . 7_455 ?
O7 Na2 Na3 112.8(2) 2_675 7_455 ?
O7 Na2 Na3 112.8(2) . 7_455 ?
O5 Na2 Na3 46.18(19) 2_675 7_455 ?
O5 Na2 Na3 46.18(19) . 7_455 ?
Na1 Na2 Na3 91.14(13) 2_675 7_455 ?
Na1 Na2 Na3 91.14(13) . 7_455 ?
Na3 Na2 Na3 180.0 . 7_455 ?
O9 Na3 O9 100.1(5) . 2_675 ?
O9 Na3 O8 71.9(3) . 2_675 ?
O9 Na3 O8 78.3(3) 2_675 2_675 ?
O9 Na3 O5 135.6(2) . 8_664 ?
O9 Na3 O5 102.3(2) 2_675 8_664 ?
O8 Na3 O5 150.3(4) 2_675 8_664 ?
O9 Na3 O5 102.3(2) . 7_454 ?
O9 Na3 O5 135.6(2) 2_675 7_454 ?
O8 Na3 O5 72.9(2) 2_675 7_454 ?
O5 Na3 O5 87.7(5) 8_664 7_454 ?
O9 Na3 Na2 50.0(2) . . ?
O9 Na3 Na2 50.0(2) 2_675 . ?
O8 Na3 Na2 66.5(3) 2_675 . ?
O5 Na3 Na2 136.1(2) 8_664 . ?
O5 Na3 Na2 136.1(2) 7_454 . ?
O9 Na3 Na2 130.0(2) . 7_454 ?
O9 Na3 Na2 130.0(2) 2_675 7_454 ?
O8 Na3 Na2 113.5(3) 2_675 7_454 ?
O5 Na3 Na2 43.9(2) 8_664 7_454 ?
O5 Na3 Na2 43.9(2) 7_454 7_454 ?
Na2 Na3 Na2 180.0 . 7_454 ?
C1 O1 C29 113.0(7) . . ?
C1 O1 Na1 129.7(5) . . ?
C29 O1 Na1 116.7(6) . . ?
C30 O5 Na1 104.4(7) . . ?
C30 O5 Na2 117.2(8) . . ?
Na1 O5 Na2 72.6(2) . . ?
C30 O5 Na3 118.7(7) . 7_455 ?
Na1 O5 Na3 136.7(3) . 7_455 ?
Na2 O5 Na3 90.0(3) . 7_455 ?
C1 C2 C3 117.6(10) . . ?
C1 C2 C28 122.6(9) . . ?
C3 C2 C28 119.3(10) . . ?
O5 C30 O6 125.7(11) . . ?
O5 C30 C29 121.5(11) . . ?
O6 C30 C29 112.7(10) . . ?
C2 C1 C6 122.6(10) . . ?
C2 C1 O1 117.2(9) . . ?
C6 C1 O1 120.2(9) . . ?
C5 C6 C1 118.3(10) . . ?
C5 C6 C7 118.7(10) . . ?
C1 C6 C7 122.5(10) . . ?
C4 C3 C2 121.2(11) . . ?
O1 C29 C30 113.1(9) . . ?
C8 C7 C6 110.9(8) . . ?
C4 C5 C6 120.4(11) . . ?
C5 C4 C3 119.8(11) . . ?
C9 O2 C31 112.5(7) . . ?
C9 O2 Na1 133.1(5) . . ?
C31 O2 Na1 114.3(6) . . ?
C32 O7 Na1 115.1(7) . . ?
C32 O7 Na2 134.2(7) . . ?
Na1 O7 Na2 87.0(3) . . ?
C13 C8 C9 117.4(9) . . ?
C13 C8 C7 120.1(9) . . ?
C9 C8 C7 122.2(9) . . ?
O2 C9 C10 119.8(9) . . ?
O2 C9 C8 117.9(9) . . ?
C10 C9 C8 122.3(9) . . ?
O7 C32 O8 126.3(10) . . ?
O7 C32 C31 123.2(10) . . ?
O8 C32 C31 110.4(9) . . ?
O8 C32 Na1 163.4(8) . . ?
C31 C32 Na1 81.2(6) . . ?
C15 C14 C10 112.0(9) . . ?
C9 C10 C11 117.3(10) . . ?
C9 C10 C14 122.3(9) . . ?
C11 C10 C14 120.1(10) . . ?
O2 C31 C32 111.8(8) . . ?
C12 C11 C10 121.1(11) . . ?
C11 C12 C13 121.9(11) . . ?
C12 C13 C8 119.9(10) . . ?
C34 O9 Na3 123.1(7) . . ?
C34 O9 Na1 101.4(7) . . ?
Na3 O9 Na1 133.5(3) . . ?
C16 O3 C33 112.1(8) . . ?
C16 O3 Na1 132.2(6) . . ?
C33 O3 Na1 115.5(6) . . ?
C15 C16 C17 123.3(10) . . ?
C15 C16 O3 117.6(10) . . ?
C17 C16 O3 119.0(10) . . ?
O3 C33 C34 111.4(9) . . ?
O9 C34 O10 125.0(10) . . ?
O9 C34 C33 123.0(10) . . ?
O10 C34 C33 112.0(10) . . ?
C16 C15 C20 117.2(12) . . ?
C16 C15 C14 121.7(10) . . ?
C20 C15 C14 120.5(11) . . ?
C16 C17 C18 115.9(11) . . ?
C16 C17 C21 121.8(10) . . ?
C18 C17 C21 122.1(11) . . ?
C22 C21 C17 112.3(9) . . ?
C19 C20 C15 120.1(12) . . ?
C18 C19 C20 121.5(13) . . ?
C19 C18 C17 121.7(13) . . ?
C36 O11 Na1 114.5(7) . . ?
C36 O11 Na2 125.8(7) . . ?
Na1 O11 Na2 88.2(3) . . ?
C23 O4 C35 111.4(7) . . ?
C23 O4 Na1 139.1(6) . . ?
C35 O4 Na1 109.3(5) . . ?
C24 C23 C22 123.8(10) . . ?
C24 C23 O4 118.9(10) . . ?
C22 C23 O4 117.2(9) . . ?
O11 C36 O12 127.2(11) . . ?
O11 C36 C35 122.7(10) . . ?
O12 C36 C35 110.0(10) . . ?
O12 C36 Na1 162.4(8) . . ?
C35 C36 Na1 80.0(6) . . ?
C27 C22 C23 116.2(10) . . ?
C27 C22 C21 121.7(12) . . ?
C23 C22 C21 122.1(10) . . ?
C23 C24 C25 117.5(11) . . ?
C23 C24 C28 123.6(10) . . ?
C25 C24 C28 118.5(10) . . ?
O4 C35 C36 113.9(8) . . ?
C24 C28 C2 110.7(9) . . ?
C26 C27 C22 121.1(13) . . ?
C25 C26 C27 120.4(12) . . ?
C26 C25 C24 120.8(11) . . ?
O1S S1S C1S 105.7(9) . . ?
O1S S1S C2S 108.8(8) . . ?
C1S S1S C2S 95.4(9) . . ?

_refine_diff_density_max         0.258
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.058

_shelxl_version_number           2014-3


# start Validation Reply Form
_vrf_RINTA01_pol_calix4tube_3    
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: This error message appears because crystal is very weakly diffracting (Ratio Observed / Unique Reflections is only 47%). In this way, a large amount of almost null reflections not being systematic absence are merged to estimate Rint, yielding a bad statistic figure of merit.
;
_vrf_PLAT340_pol_calix4tube_3    
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0112 Ang.  
RESPONSE: This error message appears because crystal is very weakly diffracting (Ratio Observed / Unique Reflections is only 47%). In this way, a large amount of unobserved reflections in practice are being used in the refinement, resulting in low precision on atom positions. 
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_pol_calix4tube_4
_database_code_depnum_ccdc_archive 'CCDC 1440137'
_audit_update_record             
;
2016-08-10 deposited with the CCDC.
2016-08-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C78 H74 N2 Na4 O26'
_chemical_formula_weight         1547.35

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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           106
_space_group_name_H-M_alt        'P 42 b c'
_space_group_name_Hall           'P 4c -2ab'

_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'
'-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'

_cell_length_a                   21.0771(7)
_cell_length_b                   21.0771(7)
_cell_length_c                   16.6303(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7387.9(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    24382
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      25.40

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3232
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'Blessing, R. H. (1995) Acta Cryst., A51, 33-38'
_exptl_absorpt_correction_T_min  0.933
_exptl_absorpt_correction_T_max  0.991

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_reflns_number            24383
_diffrn_reflns_av_unetI/netI     0.1274
_diffrn_reflns_av_R_equivalents  0.1284
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.288
_diffrn_reflns_theta_max         25.404
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_point_group_measured_fraction_full 0.868
_reflns_number_total             5868
_reflns_number_gt                2790
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.664
_reflns_Friedel_fraction_max     0.716
_reflns_Friedel_fraction_full    0.725

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           fullcycle
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0975P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_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)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5868
_refine_ls_number_parameters     497
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1725
_refine_ls_R_factor_gt           0.0662
_refine_ls_wR_factor_ref         0.2141
_refine_ls_wR_factor_gt          0.1548
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001

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
_atom_site_disorder_assembly
_atom_site_disorder_group
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 . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
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_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
_geom_angle_publ_flag
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_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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
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) . . . . ?

_refine_diff_density_max         0.325
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.101

_shelxl_version_number           2014-3


# start Validation Reply Form
_vrf_PLAT340_pol_calix4tube_4    
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01514 Ang.  
RESPONSE: This error message appears because crystal is very weakly diffracting (Ratio Observed / Unique Reflections is only 48%). In this way, a large amount of unobserved reflections in practice are being used in the refinement, resulting in low precision on atom positions. 
;
_vrf_PLAT939_pol_calix4tube_4    
;
PROBLEM: Large Value of Not (SHELXL) Weight Optimized S .     227.44       
RESPONSE: This error is due to poor ratio of observed/unique reflections
;
# end Validation Reply Form
