# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2015

####################################################################### 
# 
# 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_940SF_0ms_a
_database_code_depnum_ccdc_archive 'CCDC 1431112'
_audit_update_record             
;
2015-10-13 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C12 H24 K O6, C10 H8
;
_chemical_formula_sum            'C22 H32 K O6'
_chemical_formula_weight         431.57

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'
K K 0.2009 0.2494 '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'
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                   8.7069(8)
_cell_length_b                   9.1354(8)
_cell_length_c                   15.4095(14)
_cell_angle_alpha                98.5060(15)
_cell_angle_beta                 91.6650(15)
_cell_angle_gamma                113.2050(14)
_cell_volume                     1108.98(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2719
_cell_measurement_theta_max      29.48
_cell_measurement_theta_min      2.46

_exptl_crystal_description       block
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_F_000             462
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    0.274
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6507
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus tube, MoK\a'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11412
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.342
_diffrn_reflns_theta_max         29.563
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             5873
_reflns_number_gt                4238
_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-2014/6 (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)+(0.0412P)²+0.3077P] 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_number_reflns         5873
_refine_ls_number_parameters     262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0513
_refine_ls_wR_factor_ref         0.1081
_refine_ls_wR_factor_gt          0.0943
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_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
K1 K 0.65809(5) 0.51429(5) 0.76092(3) 0.01773(10) Uani 1 1 d . . . . .
O1 O 0.66102(15) 0.78514(15) 0.68694(8) 0.0178(3) Uani 1 1 d . . . . .
O2 O 0.95635(15) 0.80951(14) 0.78334(8) 0.0175(3) Uani 1 1 d . . . . .
O3 O 0.93378(15) 0.55275(15) 0.87255(8) 0.0197(3) Uani 1 1 d . . . . .
O4 O 0.68361(15) 0.23547(15) 0.81002(8) 0.0182(3) Uani 1 1 d . . . . .
O5 O 0.38307(16) 0.20509(15) 0.71690(8) 0.0195(3) Uani 1 1 d . . . . .
O6 O 0.42131(15) 0.46319(15) 0.62452(8) 0.0194(3) Uani 1 1 d . . . . .
C1 C 0.4317(2) 0.4570(2) 0.96563(11) 0.0158(4) Uani 1 1 d . . . . .
C2 C 0.4105(2) 0.5405(2) 0.89875(12) 0.0209(4) Uani 1 1 d . . . . .
H2 H 0.3239 0.4846 0.8521 0.025 Uiso 1 1 calc R U . . .
C3 C 0.5139(3) 0.7031(2) 0.89969(13) 0.0241(4) Uani 1 1 d . . . . .
H3 H 0.4946 0.7574 0.8552 0.029 Uiso 1 1 calc R U . . .
C4 C 0.6448(3) 0.7852(2) 0.96569(13) 0.0237(4) Uani 1 1 d . . . . .
H4 H 0.7154 0.8954 0.9659 0.028 Uiso 1 1 calc R U . . .
C5 C 0.6734(2) 0.7068(2) 1.03174(12) 0.0205(4) Uani 1 1 d . . . . .
H5 H 0.7648 0.7641 1.0757 0.025 Uiso 1 1 calc R U . . .
C6 C 1.0067(2) 0.5539(2) 0.54055(11) 0.0130(3) Uani 1 1 d . . . . .
C7 C 0.9296(2) 0.4858(2) 0.61334(11) 0.0163(4) Uani 1 1 d . . . . .
H7 H 0.9404 0.5550 0.6677 0.020 Uiso 1 1 calc R U . . .
C8 C 0.8378(2) 0.3185(2) 0.60668(12) 0.0202(4) Uani 1 1 d . . . . .
H8 H 0.7853 0.2760 0.6559 0.024 Uiso 1 1 calc R U . . .
C9 C 0.8236(2) 0.2154(2) 0.52846(12) 0.0186(4) Uani 1 1 d . . . . .
H9 H 0.7608 0.1023 0.5240 0.022 Uiso 1 1 calc R U . . .
C10 C 0.9019(2) 0.2780(2) 0.45584(11) 0.0162(4) Uani 1 1 d . . . . .
H10 H 0.8934 0.2058 0.4030 0.019 Uiso 1 1 calc R U . . .
C11 C 0.8223(2) 0.9128(2) 0.68662(12) 0.0198(4) Uani 1 1 d . . . . .
H11A H 0.8091 1.0116 0.6758 0.024 Uiso 1 1 calc R U . . .
H11B H 0.8828 0.8812 0.6389 0.024 Uiso 1 1 calc R U . . .
C12 C 0.9208(2) 0.9460(2) 0.77424(12) 0.0200(4) Uani 1 1 d . . . . .
H12A H 1.0269 1.0431 0.7778 0.024 Uiso 1 1 calc R U . . .
H12B H 0.8551 0.9663 0.8224 0.024 Uiso 1 1 calc R U . . .
C13 C 1.0544(2) 0.8324(2) 0.86372(12) 0.0186(4) Uani 1 1 d . . . . .
H13A H 0.9930 0.8500 0.9145 0.022 Uiso 1 1 calc R U . . .
H13B H 1.1615 0.9285 0.8675 0.022 Uiso 1 1 calc R U . . .
C14 C 1.0886(2) 0.6838(2) 0.86553(12) 0.0201(4) Uani 1 1 d . . . . .
H14A H 1.1370 0.6582 0.8109 0.024 Uiso 1 1 calc R U . . .
H14B H 1.1699 0.7024 0.9165 0.024 Uiso 1 1 calc R U . . .
C15 C 0.9537(2) 0.4077(2) 0.88156(12) 0.0198(4) Uani 1 1 d . . . . .
H15A H 1.0328 0.4275 0.9338 0.024 Uiso 1 1 calc R U . . .
H15B H 0.9996 0.3707 0.8287 0.024 Uiso 1 1 calc R U . . .
C16 C 0.7844(2) 0.2811(2) 0.89202(11) 0.0192(4) Uani 1 1 d . . . . .
H16A H 0.7967 0.1857 0.9091 0.023 Uiso 1 1 calc R U . . .
H16B H 0.7305 0.3248 0.9387 0.023 Uiso 1 1 calc R U . . .
C17 C 0.5249(2) 0.1056(2) 0.81174(12) 0.0208(4) Uani 1 1 d . . . . .
H17A H 0.4650 0.1354 0.8602 0.025 Uiso 1 1 calc R U . . .
H17B H 0.5415 0.0081 0.8219 0.025 Uiso 1 1 calc R U . . .
C18 C 0.4237(2) 0.0711(2) 0.72505(12) 0.0211(4) Uani 1 1 d . . . . .
H18A H 0.4890 0.0529 0.6762 0.025 Uiso 1 1 calc R U . . .
H18B H 0.3195 -0.0278 0.7219 0.025 Uiso 1 1 calc R U . . .
C19 C 0.2945(2) 0.1844(2) 0.63350(12) 0.0220(4) Uani 1 1 d . . . . .
H19A H 0.1862 0.0890 0.6271 0.026 Uiso 1 1 calc R U . . .
H19B H 0.3612 0.1656 0.5855 0.026 Uiso 1 1 calc R U . . .
C20 C 0.2634(2) 0.3325(2) 0.62697(12) 0.0213(4) Uani 1 1 d . . . . .
H20A H 0.1893 0.3138 0.5728 0.026 Uiso 1 1 calc R U . . .
H20B H 0.2076 0.3587 0.6785 0.026 Uiso 1 1 calc R U . . .
C21 C 0.4015(2) 0.6031(2) 0.60472(12) 0.0209(4) Uani 1 1 d . . . . .
H21A H 0.3421 0.6411 0.6507 0.025 Uiso 1 1 calc R U . . .
H21B H 0.3339 0.5761 0.5473 0.025 Uiso 1 1 calc R U . . .
C22 C 0.5712(2) 0.7330(2) 0.60113(12) 0.0198(4) Uani 1 1 d . . . . .
H22A H 0.6344 0.6911 0.5592 0.024 Uiso 1 1 calc R U . . .
H22B H 0.5592 0.8256 0.5802 0.024 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
K1 O6 2.7542(13) . ?
K1 O3 2.7857(14) . ?
K1 O4 2.8488(13) . ?
K1 O5 2.8603(13) . ?
K1 O1 2.8651(13) . ?
K1 O2 2.8792(13) . ?
K1 H8 3.0897 . ?
K1 C2 3.1205(19) . ?
K1 C3 3.146(2) . ?
O1 C11 1.430(2) . ?
O1 C22 1.431(2) . ?
O2 C12 1.422(2) . ?
O2 C13 1.424(2) . ?
O3 C14 1.427(2) . ?
O3 C15 1.429(2) . ?
O4 C16 1.425(2) . ?
O4 C17 1.427(2) . ?
O5 C18 1.423(2) . ?
O5 C19 1.428(2) . ?
O6 C20 1.428(2) . ?
O6 C21 1.429(2) . ?
C1 C2 1.418(3) . ?
C1 C5 1.421(2) 2_667 ?
C1 C1 1.449(3) 2_667 ?
C2 C3 1.399(3) . ?
C3 C4 1.389(3) . ?
C4 C5 1.397(3) . ?
C5 C1 1.421(2) 2_667 ?
C6 C10 1.416(2) 2_766 ?
C6 C7 1.420(2) . ?
C6 C6 1.442(3) 2_766 ?
C7 C8 1.404(3) . ?
C8 C9 1.386(3) . ?
C9 C10 1.404(2) . ?
C10 C6 1.416(2) 2_766 ?
C11 C12 1.502(3) . ?
C13 C14 1.504(3) . ?
C15 C16 1.505(3) . ?
C17 C18 1.500(3) . ?
C19 C20 1.498(3) . ?
C21 C22 1.496(2) . ?

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
O6 K1 O3 168.69(4) . . ?
O6 K1 O4 117.05(4) . . ?
O3 K1 O4 60.87(4) . . ?
O6 K1 O5 60.87(4) . . ?
O3 K1 O5 119.99(4) . . ?
O4 K1 O5 59.70(4) . . ?
O6 K1 O1 60.99(4) . . ?
O3 K1 O1 118.97(4) . . ?
O4 K1 O1 170.48(4) . . ?
O5 K1 O1 121.00(4) . . ?
O6 K1 O2 117.23(4) . . ?
O3 K1 O2 60.03(4) . . ?
O4 K1 O2 118.33(4) . . ?
O5 K1 O2 171.53(4) . . ?
O1 K1 O2 59.39(4) . . ?
O6 K1 H8 91.7 . . ?
O3 K1 H8 78.5 . . ?
O4 K1 H8 51.4 . . ?
O5 K1 H8 71.6 . . ?
O1 K1 H8 119.1 . . ?
O2 K1 H8 100.6 . . ?
O6 K1 C2 90.78(5) . . ?
O3 K1 C2 100.45(5) . . ?
O4 K1 C2 95.55(4) . . ?
O5 K1 C2 77.79(4) . . ?
O1 K1 C2 93.81(5) . . ?
O2 K1 C2 110.66(5) . . ?
H8 K1 C2 143.3 . . ?
O6 K1 C3 95.33(5) . . ?
O3 K1 C3 95.39(5) . . ?
O4 K1 C3 115.37(4) . . ?
O5 K1 C3 102.16(5) . . ?
O1 K1 C3 74.09(4) . . ?
O2 K1 C3 86.14(5) . . ?
H8 K1 C3 166.8 . . ?
C2 K1 C3 25.79(5) . . ?
C11 O1 C22 111.30(13) . . ?
C11 O1 K1 115.93(10) . . ?
C22 O1 K1 110.77(10) . . ?
C12 O2 C13 112.66(13) . . ?
C12 O2 K1 112.53(10) . . ?
C13 O2 K1 111.18(9) . . ?
C14 O3 C15 112.97(14) . . ?
C14 O3 K1 116.81(10) . . ?
C15 O3 K1 115.79(10) . . ?
C16 O4 C17 112.10(13) . . ?
C16 O4 K1 109.21(10) . . ?
C17 O4 K1 113.58(10) . . ?
C18 O5 C19 112.02(14) . . ?
C18 O5 K1 114.85(10) . . ?
C19 O5 K1 112.40(10) . . ?
C20 O6 C21 111.89(14) . . ?
C20 O6 K1 114.65(10) . . ?
C21 O6 K1 116.47(10) . . ?
C2 C1 C5 123.40(17) . 2_667 ?
C2 C1 C1 118.2(2) . 2_667 ?
C5 C1 C1 118.4(2) 2_667 2_667 ?
C3 C2 C1 121.71(18) . . ?
C3 C2 K1 78.12(11) . . ?
C1 C2 K1 105.73(12) . . ?
C4 C3 C2 119.92(18) . . ?
C4 C3 K1 104.62(13) . . ?
C2 C3 K1 76.09(11) . . ?
C3 C4 C5 120.47(18) . . ?
C4 C5 C1 121.26(18) . 2_667 ?
C10 C6 C7 123.17(15) 2_766 . ?
C10 C6 C6 118.48(18) 2_766 2_766 ?
C7 C6 C6 118.35(19) . 2_766 ?
C8 C7 C6 121.44(16) . . ?
C9 C8 C7 120.12(16) . . ?
C8 C9 C10 120.01(16) . . ?
C9 C10 C6 121.58(16) . 2_766 ?
O1 C11 C12 109.06(14) . . ?
O2 C12 C11 108.80(15) . . ?
O2 C13 C14 108.32(14) . . ?
O3 C14 C13 108.28(15) . . ?
O3 C15 C16 108.12(15) . . ?
O4 C16 C15 108.31(14) . . ?
O4 C17 C18 108.70(14) . . ?
O5 C18 C17 108.98(15) . . ?
O5 C19 C20 109.55(15) . . ?
O6 C20 C19 108.25(15) . . ?
O6 C21 C22 108.86(15) . . ?
O1 C22 C21 109.69(14) . . ?

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
C5 C1 C2 C3 178.31(18) 2_667 . . . ?
C1 C1 C2 C3 -2.2(3) 2_667 . . . ?
C5 C1 C2 K1 -96.13(17) 2_667 . . . ?
C1 C1 C2 K1 83.4(2) 2_667 . . . ?
C1 C2 C3 C4 2.2(3) . . . . ?
K1 C2 C3 C4 -99.06(18) . . . . ?
C1 C2 C3 K1 101.28(17) . . . . ?
C2 C3 C4 C5 -0.5(3) . . . . ?
K1 C3 C4 C5 -82.65(18) . . . . ?
C3 C4 C5 C1 -1.2(3) . . . 2_667 ?
C10 C6 C7 C8 178.97(18) 2_766 . . . ?
C6 C6 C7 C8 -1.9(3) 2_766 . . . ?
C6 C7 C8 C9 1.3(3) . . . . ?
C7 C8 C9 C10 0.4(3) . . . . ?
C8 C9 C10 C6 -1.4(3) . . . 2_766 ?
C22 O1 C11 C12 -171.66(15) . . . . ?
K1 O1 C11 C12 -43.87(17) . . . . ?
C13 O2 C12 C11 178.13(14) . . . . ?
K1 O2 C12 C11 -55.21(15) . . . . ?
O1 C11 C12 O2 66.79(18) . . . . ?
C12 O2 C13 C14 -178.48(14) . . . . ?
K1 O2 C13 C14 54.15(15) . . . . ?
C15 O3 C14 C13 -175.53(14) . . . . ?
K1 O3 C14 C13 46.43(16) . . . . ?
O2 C13 C14 O3 -67.80(17) . . . . ?
C14 O3 C15 C16 177.74(14) . . . . ?
K1 O3 C15 C16 -43.77(16) . . . . ?
C17 O4 C16 C15 175.04(15) . . . . ?
K1 O4 C16 C15 -58.19(15) . . . . ?
O3 C15 C16 O4 69.83(18) . . . . ?
C16 O4 C17 C18 177.06(15) . . . . ?
K1 O4 C17 C18 52.68(16) . . . . ?
C19 O5 C18 C17 176.71(14) . . . . ?
K1 O5 C18 C17 46.90(16) . . . . ?
O4 C17 C18 O5 -67.02(18) . . . . ?
C18 O5 C19 C20 -177.00(14) . . . . ?
K1 O5 C19 C20 -45.94(16) . . . . ?
C21 O6 C20 C19 171.02(14) . . . . ?
K1 O6 C20 C19 -53.51(16) . . . . ?
O5 C19 C20 O6 67.09(18) . . . . ?
C20 O6 C21 C22 -178.64(14) . . . . ?
K1 O6 C21 C22 46.76(17) . . . . ?
C11 O1 C22 C21 -178.28(15) . . . . ?
K1 O1 C22 C21 51.19(16) . . . . ?
O6 C21 C22 O1 -66.44(19) . . . . ?

_refine_diff_density_max         0.349
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.061

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_942SF_0mS_a
_database_code_depnum_ccdc_archive 'CCDC 1431113'
_audit_update_record             
;
2015-10-13 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
K H24 C12 O6, 2(C4 H8 O), C14 H10
;
_chemical_formula_sum            'C34 H50 K O8'
_chemical_formula_weight         625.84

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'
K K 0.2009 0.2494 '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      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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+1/2, -z'

_cell_length_a                   13.0082(8)
_cell_length_b                   18.1719(11)
_cell_length_c                   15.3774(10)
_cell_angle_alpha                90
_cell_angle_beta                 112.4700(10)
_cell_angle_gamma                90
_cell_volume                     3359.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6599
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      25.45

_exptl_crystal_description       block
_exptl_crystal_colour            blue-purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_F_000             1348
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    0.206
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6643
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus tube, MoK\a'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'φ and ο scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35792
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.433
_diffrn_reflns_theta_max         27.534
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             14982
_reflns_number_gt                11167
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    1.000

_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-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0329P)²+0.2748P] 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 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.42(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         14982
_refine_ls_number_parameters     776
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0444
_refine_ls_wR_factor_ref         0.0878
_refine_ls_wR_factor_gt          0.0767
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_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
K1 K 0.09896(6) 0.75660(4) 0.27966(6) 0.01842(16) Uani 1 1 d . . . . .
K2 K 0.39814(6) 0.23018(4) 0.22103(6) 0.01885(17) Uani 1 1 d . . . . .
O5 O -0.01211(18) 0.63126(12) 0.31784(16) 0.0216(6) Uani 1 1 d . . . . .
O4 O -0.12869(16) 0.75464(13) 0.22363(16) 0.0198(5) Uani 1 1 d . . . . .
O6 O 0.22140(18) 0.64607(13) 0.40716(16) 0.0225(5) Uani 1 1 d . . . . .
O10 O 0.34037(18) 0.09163(13) 0.27323(16) 0.0224(6) Uani 1 1 d . . . . .
O14 O 0.23112(19) 0.32402(12) 0.10438(17) 0.0238(6) Uani 1 1 d . . . . .
O9 O 0.17844(18) 0.20141(12) 0.19133(17) 0.0223(6) Uani 1 1 d . . . . .
O3 O -0.02564(18) 0.86314(12) 0.14696(17) 0.0225(6) Uani 1 1 d . . . . .
O1 O 0.32616(17) 0.75057(13) 0.33099(16) 0.0224(6) Uani 1 1 d . . . . .
O2 O 0.21041(18) 0.87717(13) 0.23650(16) 0.0224(6) Uani 1 1 d . . . . .
O13 O 0.45603(19) 0.37105(13) 0.17302(17) 0.0272(6) Uani 1 1 d . . . . .
O11 O 0.56786(18) 0.13900(14) 0.34334(17) 0.0275(6) Uani 1 1 d . . . . .
O12 O 0.61857(18) 0.26561(15) 0.25946(17) 0.0294(6) Uani 1 1 d . . . . .
O7 O 0.0806(2) 0.67887(15) 0.1245(2) 0.0363(7) Uani 1 1 d . . . . .
O16 O 0.3925(2) 0.30327(15) 0.3693(2) 0.0426(8) Uani 1 1 d . . . . .
O8 O 0.1018(2) 0.84214(15) 0.4236(2) 0.0417(8) Uani 1 1 d . . . . .
O15 O 0.4018(2) 0.16450(15) 0.0669(2) 0.0423(8) Uani 1 1 d . . . . .
C59 C 0.9685(3) 0.21759(19) 0.2968(2) 0.0175(8) Uani 1 1 d . . . . .
C55 C 0.8745(3) 0.10170(19) 0.2293(2) 0.0219(8) Uani 1 1 d . . . . .
H55 H 0.8199 0.0752 0.1797 0.026 Uiso 1 1 calc R U . . .
C47 C 0.6550(2) 0.81475(19) 0.2983(2) 0.0174(8) Uani 1 1 d . . . . .
C54 C 0.5416(3) 0.67565(19) 0.2599(2) 0.0186(8) Uani 1 1 d . . . . .
C45 C 0.6344(3) 0.68820(19) 0.3485(2) 0.0180(8) Uani 1 1 d . . . . .
C58 C 1.0355(3) 0.1772(2) 0.3760(2) 0.0225(8) Uani 1 1 d . . . . .
H58 H 1.0906 0.2022 0.4268 0.027 Uiso 1 1 calc R U . . .
C52 C 0.5634(2) 0.80239(19) 0.2096(2) 0.0171(7) Uani 1 1 d . . . . .
C2 C 0.3183(3) 0.85695(19) 0.2391(2) 0.0226(8) Uani 1 1 d . . . . .
H2A H 0.3596 0.9014 0.2340 0.027 Uiso 1 1 calc R U . . .
H2B H 0.3105 0.8239 0.1857 0.027 Uiso 1 1 calc R U . . .
C67 C 0.8165(3) 0.2188(2) 0.1405(2) 0.0195(8) Uani 1 1 d . . . . .
H67 H 0.7618 0.1932 0.0900 0.023 Uiso 1 1 calc R U . . .
C53 C 0.5094(3) 0.73382(19) 0.1940(2) 0.0183(7) Uani 1 1 d . . . . .
H53 H 0.4481 0.7262 0.1363 0.022 Uiso 1 1 calc R U . . .
C51 C 0.5334(3) 0.86021(19) 0.1426(2) 0.0206(8) Uani 1 1 d . . . . .
H51 H 0.4731 0.8532 0.0841 0.025 Uiso 1 1 calc R U . . .
C50 C 0.5898(3) 0.9268(2) 0.1603(3) 0.0265(9) Uani 1 1 d . . . . .
H50 H 0.5689 0.9643 0.1137 0.032 Uiso 1 1 calc R U . . .
C49 C 0.6772(3) 0.9386(2) 0.2462(3) 0.0253(9) Uani 1 1 d . . . . .
H49 H 0.7156 0.9843 0.2583 0.030 Uiso 1 1 calc R U . . .
C6 C -0.1881(3) 0.8013(2) 0.1455(2) 0.0237(8) Uani 1 1 d . . . . .
H6A H -0.2650 0.8091 0.1419 0.028 Uiso 1 1 calc R U . . .
H6B H -0.1920 0.7780 0.0861 0.028 Uiso 1 1 calc R U . . .
C68 C 0.8841(3) 0.17851(19) 0.2200(2) 0.0179(8) Uani 1 1 d . . . . .
C61 C 0.9091(3) 0.33469(19) 0.2092(2) 0.0200(8) Uani 1 1 d . . . . .
C48 C 0.7080(3) 0.88449(19) 0.3139(3) 0.0220(8) Uani 1 1 d . . . . .
H48 H 0.7666 0.8941 0.3727 0.026 Uiso 1 1 calc R U . . .
C21 C 0.1509(3) 0.12627(19) 0.1987(3) 0.0235(8) Uani 1 1 d . . . . .
H21A H 0.1487 0.0986 0.1426 0.028 Uiso 1 1 calc R U . . .
H21B H 0.0766 0.1230 0.2023 0.028 Uiso 1 1 calc R U . . .
C65 C 0.7590(3) 0.3358(2) 0.0524(3) 0.0248(8) Uani 1 1 d . . . . .
H65 H 0.7063 0.3103 0.0005 0.030 Uiso 1 1 calc R U . . .
C46 C 0.6870(3) 0.7570(2) 0.3644(2) 0.0199(8) Uani 1 1 d . . . . .
H46 H 0.7472 0.7651 0.4227 0.024 Uiso 1 1 calc R U . . .
C7 C -0.1830(3) 0.68612(18) 0.2195(3) 0.0211(8) Uani 1 1 d . . . . .
H7A H -0.1815 0.6567 0.1658 0.025 Uiso 1 1 calc R U . . .
H7B H -0.2617 0.6945 0.2105 0.025 Uiso 1 1 calc R U . . .
C8 C -0.1240(3) 0.6457(2) 0.3096(3) 0.0224(8) Uani 1 1 d . . . . .
H8A H -0.1233 0.6758 0.3635 0.027 Uiso 1 1 calc R U . . .
H8B H -0.1628 0.5988 0.3097 0.027 Uiso 1 1 calc R U . . .
C22 C 0.2367(3) 0.0942(2) 0.2852(3) 0.0252(8) Uani 1 1 d . . . . .
H22A H 0.2442 0.1248 0.3405 0.030 Uiso 1 1 calc R U . . .
H22B H 0.2144 0.0439 0.2958 0.030 Uiso 1 1 calc R U . . .
C11 C 0.3283(3) 0.6346(2) 0.4028(3) 0.0256(8) Uani 1 1 d . . . . .
H11A H 0.3193 0.6112 0.3422 0.031 Uiso 1 1 calc R U . . .
H11B H 0.3734 0.6015 0.4544 0.031 Uiso 1 1 calc R U . . .
C57 C 1.0235(3) 0.1016(2) 0.3821(3) 0.0271(9) Uani 1 1 d . . . . .
H57 H 1.0705 0.0756 0.4363 0.032 Uiso 1 1 calc R U . . .
C41 C 0.4894(3) 0.6064(2) 0.2440(3) 0.0246(8) Uani 1 1 d . . . . .
H41 H 0.4284 0.5978 0.1863 0.029 Uiso 1 1 calc R U . . .
C5 C -0.1284(3) 0.8733(2) 0.1590(3) 0.0243(8) Uani 1 1 d . . . . .
H5A H -0.1751 0.9095 0.1126 0.029 Uiso 1 1 calc R U . . .
H5B H -0.1137 0.8925 0.2229 0.029 Uiso 1 1 calc R U . . .
C23 C 0.4260(3) 0.0601(2) 0.3529(3) 0.0288(9) Uani 1 1 d . . . . .
H23A H 0.4082 0.0081 0.3605 0.035 Uiso 1 1 calc R U . . .
H23B H 0.4329 0.0873 0.4107 0.035 Uiso 1 1 calc R U . . .
C3 C 0.1450(3) 0.9129(2) 0.1517(3) 0.0252(8) Uani 1 1 d . . . . .
H3A H 0.1357 0.8805 0.0974 0.030 Uiso 1 1 calc R U . . .
H3B H 0.1820 0.9588 0.1446 0.030 Uiso 1 1 calc R U . . .
C56 C 0.9426(3) 0.0641(2) 0.3086(3) 0.0254(9) Uani 1 1 d . . . . .
H56 H 0.9341 0.0125 0.3131 0.030 Uiso 1 1 calc R U . . .
C12 C 0.3856(3) 0.7068(2) 0.4117(3) 0.0258(9) Uani 1 1 d . . . . .
H12A H 0.3884 0.7323 0.4694 0.031 Uiso 1 1 calc R U . . .
H12B H 0.4629 0.6990 0.4163 0.031 Uiso 1 1 calc R U . . .
C35 C 0.4230(3) 0.0690(2) -0.0293(3) 0.0264(9) Uani 1 1 d . . . . .
H35A H 0.3812 0.0824 -0.0960 0.032 Uiso 1 1 calc R U . . .
H35B H 0.4370 0.0153 -0.0247 0.032 Uiso 1 1 calc R U . . .
C18 C 0.1273(3) 0.9299(2) 0.5434(3) 0.0268(8) Uani 1 1 d . . . . .
H18A H 0.1362 0.9839 0.5512 0.032 Uiso 1 1 calc R U . . .
H18B H 0.1647 0.9058 0.6054 0.032 Uiso 1 1 calc R U . . .
C60 C 0.9774(3) 0.2943(2) 0.2878(2) 0.0202(8) Uani 1 1 d . . . . .
H60 H 1.0328 0.3201 0.3376 0.024 Uiso 1 1 calc R U . . .
C1 C 0.3796(3) 0.81865(19) 0.3301(3) 0.0240(8) Uani 1 1 d . . . . .
H1A H 0.4576 0.8097 0.3374 0.029 Uiso 1 1 calc R U . . .
H1B H 0.3804 0.8498 0.3832 0.029 Uiso 1 1 calc R U . . .
C19 C 0.0048(3) 0.90819(19) 0.4987(3) 0.0234(8) Uani 1 1 d . . . . .
H19A H -0.0286 0.9036 0.5465 0.028 Uiso 1 1 calc R U . . .
H19B H -0.0387 0.9440 0.4501 0.028 Uiso 1 1 calc R U . . .
C42 C 0.5241(3) 0.5504(2) 0.3097(3) 0.0320(10) Uani 1 1 d . . . . .
H42 H 0.4875 0.5040 0.2967 0.038 Uiso 1 1 calc R U . . .
C34 C 0.5311(3) 0.11236(19) 0.0128(3) 0.0275(9) Uani 1 1 d . . . . .
H34A H 0.5846 0.0879 0.0696 0.033 Uiso 1 1 calc R U . . .
H34B H 0.5661 0.1194 -0.0335 0.033 Uiso 1 1 calc R U . . .
C43 C 0.6129(3) 0.5621(2) 0.3950(3) 0.0304(9) Uani 1 1 d . . . . .
H43 H 0.6368 0.5237 0.4402 0.036 Uiso 1 1 calc R U . . .
C10 C 0.1646(3) 0.5785(2) 0.4032(3) 0.0257(9) Uani 1 1 d . . . . .
H10A H 0.2073 0.5476 0.4581 0.031 Uiso 1 1 calc R U . . .
H10B H 0.1569 0.5514 0.3453 0.031 Uiso 1 1 calc R U . . .
C32 C 0.0973(3) 0.23796(19) 0.1127(2) 0.0246(9) Uani 1 1 d . . . . .
H32A H 0.0226 0.2326 0.1151 0.030 Uiso 1 1 calc R U . . .
H32B H 0.0953 0.2157 0.0533 0.030 Uiso 1 1 calc R U . . .
C62 C 0.9156(3) 0.4123(2) 0.2010(3) 0.0272(9) Uani 1 1 d . . . . .
H62 H 0.9692 0.4391 0.2508 0.033 Uiso 1 1 calc R U . . .
C66 C 0.8265(3) 0.2956(2) 0.1325(2) 0.0197(8) Uani 1 1 d . . . . .
C33 C 0.4903(3) 0.1845(2) 0.0370(3) 0.0342(10) Uani 1 1 d . . . . .
H33A H 0.5509 0.2100 0.0881 0.041 Uiso 1 1 calc R U . . .
H33B H 0.4625 0.2172 -0.0187 0.041 Uiso 1 1 calc R U . . .
C17 C 0.1722(3) 0.9018(2) 0.4723(3) 0.0293(9) Uani 1 1 d . . . . .
H17A H 0.1708 0.9413 0.4276 0.035 Uiso 1 1 calc R U . . .
H17B H 0.2498 0.8846 0.5044 0.035 Uiso 1 1 calc R U . . .
C44 C 0.6663(3) 0.6293(2) 0.4141(3) 0.0260(9) Uani 1 1 d . . . . .
H44 H 0.7261 0.6363 0.4730 0.031 Uiso 1 1 calc R U . . .
C30 C 0.2630(3) 0.3986(2) 0.1049(3) 0.0298(9) Uani 1 1 d . . . . .
H30A H 0.2707 0.4220 0.1653 0.036 Uiso 1 1 calc R U . . .
H30B H 0.2053 0.4257 0.0533 0.036 Uiso 1 1 calc R U . . .
C25 C 0.6693(3) 0.1481(2) 0.3283(3) 0.0344(10) Uani 1 1 d . . . . .
H25A H 0.6597 0.1294 0.2653 0.041 Uiso 1 1 calc R U . . .
H25B H 0.7296 0.1197 0.3760 0.041 Uiso 1 1 calc R U . . .
C9 C 0.0517(3) 0.5950(2) 0.4036(3) 0.0264(9) Uani 1 1 d . . . . .
H9A H 0.0145 0.5487 0.4092 0.032 Uiso 1 1 calc R U . . .
H9B H 0.0589 0.6268 0.4578 0.032 Uiso 1 1 calc R U . . .
C20 C 0.0121(3) 0.8346(2) 0.4560(3) 0.0307(9) Uani 1 1 d . . . . .
H20A H 0.0283 0.7950 0.5036 0.037 Uiso 1 1 calc R U . . .
H20B H -0.0584 0.8230 0.4029 0.037 Uiso 1 1 calc R U . . .
C37 C 0.4524(3) 0.3694(2) 0.4010(3) 0.0295(9) Uani 1 1 d . . . . .
H37A H 0.4590 0.3964 0.3475 0.035 Uiso 1 1 calc R U . . .
H37B H 0.5282 0.3586 0.4473 0.035 Uiso 1 1 calc R U . . .
C4 C 0.0335(3) 0.93014(19) 0.1548(3) 0.0252(8) Uani 1 1 d . . . . .
H4A H 0.0433 0.9550 0.2147 0.030 Uiso 1 1 calc R U . . .
H4B H -0.0087 0.9634 0.1023 0.030 Uiso 1 1 calc R U . . .
C63 C 0.8453(3) 0.4498(2) 0.1219(3) 0.0323(10) Uani 1 1 d . . . . .
H63 H 0.8502 0.5018 0.1185 0.039 Uiso 1 1 calc R U . . .
C31 C 0.1272(3) 0.3173(2) 0.1160(3) 0.0275(9) Uani 1 1 d . . . . .
H31A H 0.0684 0.3443 0.0651 0.033 Uiso 1 1 calc R U . . .
H31B H 0.1338 0.3387 0.1770 0.033 Uiso 1 1 calc R U . . .
C16 C 0.0224(3) 0.6102(2) 0.1121(3) 0.0307(9) Uani 1 1 d . . . . .
H16A H -0.0483 0.6122 0.0563 0.037 Uiso 1 1 calc R U . . .
H16B H 0.0056 0.5984 0.1681 0.037 Uiso 1 1 calc R U . . .
C24 C 0.5335(3) 0.0647(2) 0.3373(3) 0.0319(9) Uani 1 1 d . . . . .
H24A H 0.5915 0.0350 0.3854 0.038 Uiso 1 1 calc R U . . .
H24B H 0.5226 0.0446 0.2745 0.038 Uiso 1 1 calc R U . . .
C40 C 0.3029(3) 0.2999(2) 0.4013(3) 0.0345(10) Uani 1 1 d . . . . .
H40A H 0.3251 0.2717 0.4608 0.041 Uiso 1 1 calc R U . . .
H40B H 0.2370 0.2761 0.3537 0.041 Uiso 1 1 calc R U . . .
C29 C 0.3718(3) 0.4020(2) 0.0924(3) 0.0326(10) Uani 1 1 d . . . . .
H29A H 0.3664 0.3743 0.0355 0.039 Uiso 1 1 calc R U . . .
H29B H 0.3904 0.4538 0.0846 0.039 Uiso 1 1 calc R U . . .
C64 C 0.7676(3) 0.4112(2) 0.0476(3) 0.0311(9) Uani 1 1 d . . . . .
H64 H 0.7203 0.4369 -0.0068 0.037 Uiso 1 1 calc R U . . .
C13 C 0.1678(3) 0.6727(2) 0.0895(3) 0.0311(9) Uani 1 1 d . . . . .
H13A H 0.2415 0.6779 0.1415 0.037 Uiso 1 1 calc R U . . .
H13B H 0.1602 0.7114 0.0421 0.037 Uiso 1 1 calc R U . . .
C26 C 0.6994(3) 0.2272(2) 0.3356(3) 0.0356(10) Uani 1 1 d . . . . .
H26A H 0.7018 0.2473 0.3962 0.043 Uiso 1 1 calc R U . . .
H26B H 0.7740 0.2333 0.3332 0.043 Uiso 1 1 calc R U . . .
C28 C 0.5637(3) 0.3749(2) 0.1687(3) 0.0327(10) Uani 1 1 d . . . . .
H28A H 0.5838 0.4269 0.1640 0.039 Uiso 1 1 calc R U . . .
H28B H 0.5633 0.3484 0.1123 0.039 Uiso 1 1 calc R U . . .
C27 C 0.6464(3) 0.3409(2) 0.2551(3) 0.0330(10) Uani 1 1 d . . . . .
H27A H 0.7218 0.3447 0.2540 0.040 Uiso 1 1 calc R U . . .
H27B H 0.6464 0.3673 0.3114 0.040 Uiso 1 1 calc R U . . .
C36 C 0.3615(3) 0.0930(2) 0.0325(3) 0.0309(10) Uani 1 1 d . . . . .
H36A H 0.2803 0.0945 -0.0046 0.037 Uiso 1 1 calc R U . . .
H36B H 0.3761 0.0582 0.0854 0.037 Uiso 1 1 calc R U . . .
C14 C 0.1557(3) 0.5966(2) 0.0451(3) 0.0359(10) Uani 1 1 d . . . . .
H14A H 0.1092 0.5982 -0.0230 0.043 Uiso 1 1 calc R U . . .
H14B H 0.2291 0.5751 0.0544 0.043 Uiso 1 1 calc R U . . .
C39 C 0.2782(3) 0.3789(2) 0.4163(3) 0.0419(11) Uani 1 1 d . . . . .
H39A H 0.2248 0.4009 0.3575 0.050 Uiso 1 1 calc R U . . .
H39B H 0.2476 0.3829 0.4661 0.050 Uiso 1 1 calc R U . . .
C15 C 0.0990(4) 0.5538(2) 0.0985(3) 0.0434(11) Uani 1 1 d . . . . .
H15A H 0.0570 0.5114 0.0615 0.052 Uiso 1 1 calc R U . . .
H15B H 0.1534 0.5361 0.1597 0.052 Uiso 1 1 calc R U . . .
C38 C 0.3895(4) 0.4148(3) 0.4459(4) 0.0544(14) Uani 1 1 d . . . . .
H38A H 0.4277 0.4145 0.5153 0.065 Uiso 1 1 calc R U . . .
H38B H 0.3821 0.4663 0.4234 0.065 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
K1 O8 2.694(3) . ?
K1 O7 2.703(3) . ?
K1 O4 2.750(2) . ?
K1 O1 2.754(2) . ?
K1 O3 2.830(2) . ?
K1 O6 2.833(2) . ?
K1 O2 2.842(2) . ?
K1 O5 2.875(2) . ?
K1 C5 3.534(3) . ?
K2 O16 2.663(3) . ?
K2 O15 2.670(3) . ?
K2 O9 2.766(2) . ?
K2 O12 2.773(2) . ?
K2 O14 2.805(2) . ?
K2 O11 2.825(2) . ?
K2 O10 2.830(2) . ?
K2 O13 2.844(2) . ?
O5 C9 1.424(4) . ?
O5 C8 1.436(4) . ?
O4 C7 1.421(4) . ?
O4 C6 1.431(4) . ?
O6 C10 1.422(4) . ?
O6 C11 1.432(4) . ?
O10 C23 1.424(4) . ?
O10 C22 1.430(4) . ?
O14 C30 1.417(4) . ?
O14 C31 1.435(4) . ?
O9 C21 1.427(4) . ?
O9 C32 1.429(4) . ?
O3 C4 1.420(4) . ?
O3 C5 1.430(4) . ?
O1 C1 1.422(4) . ?
O1 C12 1.427(4) . ?
O2 C3 1.414(4) . ?
O2 C2 1.436(4) . ?
O13 C29 1.419(4) . ?
O13 C28 1.429(4) . ?
O11 C24 1.415(4) . ?
O11 C25 1.433(4) . ?
O12 C26 1.423(4) . ?
O12 C27 1.423(4) . ?
O7 C16 1.434(4) . ?
O7 C13 1.435(4) . ?
O16 C37 1.415(4) . ?
O16 C40 1.429(4) . ?
O8 C17 1.431(4) . ?
O8 C20 1.439(4) . ?
O15 C36 1.426(5) . ?
O15 C33 1.441(4) . ?
C59 C58 1.404(5) . ?
C59 C60 1.411(5) . ?
C59 C68 1.454(4) . ?
C55 C56 1.384(5) . ?
C55 C68 1.413(5) . ?
C55 H55 0.9500 . ?
C47 C46 1.409(5) . ?
C47 C48 1.419(5) . ?
C47 C52 1.445(4) . ?
C54 C41 1.406(5) . ?
C54 C53 1.412(5) . ?
C54 C45 1.452(5) . ?
C45 C46 1.401(5) . ?
C45 C44 1.421(5) . ?
C58 C57 1.389(5) . ?
C58 H58 0.9500 . ?
C52 C53 1.405(5) . ?
C52 C51 1.418(5) . ?
C2 C1 1.492(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C67 C68 1.408(5) . ?
C67 C66 1.411(5) . ?
C67 H67 0.9500 . ?
C53 H53 0.9500 . ?
C51 C50 1.387(5) . ?
C51 H51 0.9500 . ?
C50 C49 1.391(5) . ?
C50 H50 0.9500 . ?
C49 C48 1.375(5) . ?
C49 H49 0.9500 . ?
C6 C5 1.496(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C61 C60 1.403(5) . ?
C61 C62 1.421(5) . ?
C61 C66 1.442(5) . ?
C48 H48 0.9500 . ?
C21 C22 1.490(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C65 C64 1.380(5) . ?
C65 C66 1.414(5) . ?
C65 H65 0.9500 . ?
C46 H46 0.9500 . ?
C7 C8 1.496(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C11 C12 1.489(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C57 C56 1.393(5) . ?
C57 H57 0.9500 . ?
C41 C42 1.383(5) . ?
C41 H41 0.9500 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C23 C24 1.509(5) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C3 C4 1.503(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C56 H56 0.9500 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C35 C36 1.521(5) . ?
C35 C34 1.524(5) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C18 C17 1.512(5) . ?
C18 C19 1.527(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C60 H60 0.9500 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C19 C20 1.509(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C42 C43 1.394(5) . ?
C42 H42 0.9500 . ?
C34 C33 1.512(5) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C43 C44 1.379(5) . ?
C43 H43 0.9500 . ?
C10 C9 1.500(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C32 C31 1.489(5) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C62 C63 1.390(5) . ?
C62 H62 0.9500 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C44 H44 0.9500 . ?
C30 C29 1.501(5) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C25 C26 1.482(6) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C37 C38 1.503(5) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C63 C64 1.391(5) . ?
C63 H63 0.9500 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C16 C15 1.497(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C40 C39 1.508(6) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C64 H64 0.9500 . ?
C13 C14 1.524(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C28 C27 1.487(6) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C14 C15 1.512(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C39 C38 1.492(6) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?

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
O8 K1 O7 174.63(10) . . ?
O8 K1 O4 86.55(8) . . ?
O7 K1 O4 89.73(8) . . ?
O8 K1 O1 96.39(8) . . ?
O7 K1 O1 87.45(8) . . ?
O4 K1 O1 176.65(8) . . ?
O8 K1 O3 91.25(8) . . ?
O7 K1 O3 83.58(8) . . ?
O4 K1 O3 62.07(7) . . ?
O1 K1 O3 119.33(7) . . ?
O8 K1 O6 90.74(9) . . ?
O7 K1 O6 94.41(8) . . ?
O4 K1 O6 117.44(7) . . ?
O1 K1 O6 61.03(7) . . ?
O3 K1 O6 177.91(8) . . ?
O8 K1 O2 84.20(8) . . ?
O7 K1 O2 94.46(8) . . ?
O4 K1 O2 121.41(7) . . ?
O1 K1 O2 60.68(7) . . ?
O3 K1 O2 60.46(7) . . ?
O6 K1 O2 120.40(7) . . ?
O8 K1 O5 98.02(8) . . ?
O7 K1 O5 83.36(8) . . ?
O4 K1 O5 59.25(7) . . ?
O1 K1 O5 118.55(7) . . ?
O3 K1 O5 119.67(7) . . ?
O6 K1 O5 59.38(6) . . ?
O2 K1 O5 177.75(8) . . ?
O8 K1 C5 80.27(9) . . ?
O7 K1 C5 94.38(9) . . ?
O4 K1 C5 42.14(7) . . ?
O1 K1 C5 139.92(8) . . ?
O3 K1 C5 22.69(7) . . ?
O6 K1 C5 157.65(8) . . ?
O2 K1 C5 79.28(7) . . ?
O5 K1 C5 101.39(7) . . ?
O16 K2 O15 176.60(10) . . ?
O16 K2 O9 82.58(8) . . ?
O15 K2 O9 97.85(8) . . ?
O16 K2 O12 93.81(8) . . ?
O15 K2 O12 85.71(8) . . ?
O9 K2 O12 176.31(8) . . ?
O16 K2 O14 88.64(9) . . ?
O15 K2 O14 88.64(9) . . ?
O9 K2 O14 60.69(7) . . ?
O12 K2 O14 118.70(8) . . ?
O16 K2 O11 89.59(9) . . ?
O15 K2 O11 93.11(9) . . ?
O9 K2 O11 119.62(7) . . ?
O12 K2 O11 60.86(8) . . ?
O14 K2 O11 178.14(8) . . ?
O16 K2 O10 95.95(8) . . ?
O15 K2 O10 87.17(8) . . ?
O9 K2 O10 60.60(7) . . ?
O12 K2 O10 120.74(8) . . ?
O14 K2 O10 119.84(7) . . ?
O11 K2 O10 60.93(7) . . ?
O16 K2 O13 82.53(8) . . ?
O15 K2 O13 94.34(8) . . ?
O9 K2 O13 119.12(7) . . ?
O12 K2 O13 59.44(7) . . ?
O14 K2 O13 60.27(7) . . ?
O11 K2 O13 118.92(7) . . ?
O10 K2 O13 178.48(8) . . ?
C9 O5 C8 112.3(2) . . ?
C9 O5 K1 113.29(18) . . ?
C8 O5 K1 114.13(18) . . ?
C7 O4 C6 112.4(2) . . ?
C7 O4 K1 118.88(17) . . ?
C6 O4 K1 115.26(17) . . ?
C10 O6 C11 111.7(2) . . ?
C10 O6 K1 115.89(19) . . ?
C11 O6 K1 111.70(18) . . ?
C23 O10 C22 111.6(3) . . ?
C23 O10 K2 113.37(19) . . ?
C22 O10 K2 111.92(19) . . ?
C30 O14 C31 111.6(3) . . ?
C30 O14 K2 115.1(2) . . ?
C31 O14 K2 113.89(19) . . ?
C21 O9 C32 112.7(3) . . ?
C21 O9 K2 116.27(18) . . ?
C32 O9 K2 115.75(18) . . ?
C4 O3 C5 112.4(2) . . ?
C4 O3 K1 112.53(19) . . ?
C5 O3 K1 107.52(19) . . ?
C1 O1 C12 112.9(3) . . ?
C1 O1 K1 115.98(18) . . ?
C12 O1 K1 115.91(17) . . ?
C3 O2 C2 112.3(2) . . ?
C3 O2 K1 112.87(19) . . ?
C2 O2 K1 112.11(19) . . ?
C29 O13 C28 112.5(3) . . ?
C29 O13 K2 113.0(2) . . ?
C28 O13 K2 114.7(2) . . ?
C24 O11 C25 112.8(3) . . ?
C24 O11 K2 111.68(19) . . ?
C25 O11 K2 111.0(2) . . ?
C26 O12 C27 112.9(3) . . ?
C26 O12 K2 116.1(2) . . ?
C27 O12 K2 118.3(2) . . ?
C16 O7 C13 109.6(3) . . ?
C16 O7 K1 115.9(2) . . ?
C13 O7 K1 123.8(2) . . ?
C37 O16 C40 109.4(3) . . ?
C37 O16 K2 121.8(2) . . ?
C40 O16 K2 124.5(2) . . ?
C17 O8 C20 109.4(3) . . ?
C17 O8 K1 132.2(2) . . ?
C20 O8 K1 118.1(2) . . ?
C36 O15 C33 109.6(3) . . ?
C36 O15 K2 127.5(2) . . ?
C33 O15 K2 117.3(2) . . ?
C58 C59 C60 123.7(3) . . ?
C58 C59 C68 118.3(3) . . ?
C60 C59 C68 117.9(3) . . ?
C56 C55 C68 121.7(3) . . ?
C56 C55 H55 119.2 . . ?
C68 C55 H55 119.2 . . ?
C46 C47 C48 123.6(3) . . ?
C46 C47 C52 118.4(3) . . ?
C48 C47 C52 118.1(3) . . ?
C41 C54 C53 123.6(3) . . ?
C41 C54 C45 118.5(3) . . ?
C53 C54 C45 117.9(3) . . ?
C46 C45 C44 123.9(3) . . ?
C46 C45 C54 118.7(3) . . ?
C44 C45 C54 117.4(3) . . ?
C57 C58 C59 121.8(3) . . ?
C57 C58 H58 119.1 . . ?
C59 C58 H58 119.1 . . ?
C53 C52 C51 123.5(3) . . ?
C53 C52 C47 118.5(3) . . ?
C51 C52 C47 118.0(3) . . ?
O2 C2 C1 108.2(3) . . ?
O2 C2 H2A 110.1 . . ?
C1 C2 H2A 110.1 . . ?
O2 C2 H2B 110.1 . . ?
C1 C2 H2B 110.1 . . ?
H2A C2 H2B 108.4 . . ?
C68 C67 C66 122.8(3) . . ?
C68 C67 H67 118.6 . . ?
C66 C67 H67 118.6 . . ?
C52 C53 C54 123.3(3) . . ?
C52 C53 H53 118.3 . . ?
C54 C53 H53 118.3 . . ?
C50 C51 C52 121.7(3) . . ?
C50 C51 H51 119.1 . . ?
C52 C51 H51 119.1 . . ?
C51 C50 C49 120.0(3) . . ?
C51 C50 H50 120.0 . . ?
C49 C50 H50 120.0 . . ?
C48 C49 C50 120.3(3) . . ?
C48 C49 H49 119.9 . . ?
C50 C49 H49 119.9 . . ?
O4 C6 C5 108.4(3) . . ?
O4 C6 H6A 110.0 . . ?
C5 C6 H6A 110.0 . . ?
O4 C6 H6B 110.0 . . ?
C5 C6 H6B 110.0 . . ?
H6A C6 H6B 108.4 . . ?
C67 C68 C55 123.4(3) . . ?
C67 C68 C59 118.6(3) . . ?
C55 C68 C59 118.0(3) . . ?
C60 C61 C62 123.7(3) . . ?
C60 C61 C66 118.4(3) . . ?
C62 C61 C66 117.9(3) . . ?
C49 C48 C47 121.9(3) . . ?
C49 C48 H48 119.0 . . ?
C47 C48 H48 119.0 . . ?
O9 C21 C22 108.7(3) . . ?
O9 C21 H21A 110.0 . . ?
C22 C21 H21A 110.0 . . ?
O9 C21 H21B 110.0 . . ?
C22 C21 H21B 110.0 . . ?
H21A C21 H21B 108.3 . . ?
C64 C65 C66 121.6(4) . . ?
C64 C65 H65 119.2 . . ?
C66 C65 H65 119.2 . . ?
C45 C46 C47 123.3(3) . . ?
C45 C46 H46 118.4 . . ?
C47 C46 H46 118.4 . . ?
O4 C7 C8 108.6(3) . . ?
O4 C7 H7A 110.0 . . ?
C8 C7 H7A 110.0 . . ?
O4 C7 H7B 110.0 . . ?
C8 C7 H7B 110.0 . . ?
H7A C7 H7B 108.4 . . ?
O5 C8 C7 108.4(3) . . ?
O5 C8 H8A 110.0 . . ?
C7 C8 H8A 110.0 . . ?
O5 C8 H8B 110.0 . . ?
C7 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
O10 C22 C21 108.6(3) . . ?
O10 C22 H22A 110.0 . . ?
C21 C22 H22A 110.0 . . ?
O10 C22 H22B 110.0 . . ?
C21 C22 H22B 110.0 . . ?
H22A C22 H22B 108.3 . . ?
O6 C11 C12 109.2(3) . . ?
O6 C11 H11A 109.8 . . ?
C12 C11 H11A 109.8 . . ?
O6 C11 H11B 109.8 . . ?
C12 C11 H11B 109.8 . . ?
H11A C11 H11B 108.3 . . ?
C58 C57 C56 119.9(3) . . ?
C58 C57 H57 120.0 . . ?
C56 C57 H57 120.0 . . ?
C42 C41 C54 122.1(4) . . ?
C42 C41 H41 119.0 . . ?
C54 C41 H41 119.0 . . ?
O3 C5 C6 109.3(3) . . ?
O3 C5 K1 49.79(15) . . ?
C6 C5 K1 80.42(19) . . ?
O3 C5 H5A 109.8 . . ?
C6 C5 H5A 109.8 . . ?
K1 C5 H5A 159.6 . . ?
O3 C5 H5B 109.8 . . ?
C6 C5 H5B 109.8 . . ?
K1 C5 H5B 83.4 . . ?
H5A C5 H5B 108.3 . . ?
O10 C23 C24 108.0(3) . . ?
O10 C23 H23A 110.1 . . ?
C24 C23 H23A 110.1 . . ?
O10 C23 H23B 110.1 . . ?
C24 C23 H23B 110.1 . . ?
H23A C23 H23B 108.4 . . ?
O2 C3 C4 108.3(3) . . ?
O2 C3 H3A 110.0 . . ?
C4 C3 H3A 110.0 . . ?
O2 C3 H3B 110.0 . . ?
C4 C3 H3B 110.0 . . ?
H3A C3 H3B 108.4 . . ?
C55 C56 C57 120.3(3) . . ?
C55 C56 H56 119.8 . . ?
C57 C56 H56 119.8 . . ?
O1 C12 C11 109.0(3) . . ?
O1 C12 H12A 109.9 . . ?
C11 C12 H12A 109.9 . . ?
O1 C12 H12B 109.9 . . ?
C11 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
C36 C35 C34 101.9(3) . . ?
C36 C35 H35A 111.4 . . ?
C34 C35 H35A 111.4 . . ?
C36 C35 H35B 111.4 . . ?
C34 C35 H35B 111.4 . . ?
H35A C35 H35B 109.2 . . ?
C17 C18 C19 102.3(3) . . ?
C17 C18 H18A 111.3 . . ?
C19 C18 H18A 111.3 . . ?
C17 C18 H18B 111.3 . . ?
C19 C18 H18B 111.3 . . ?
H18A C18 H18B 109.2 . . ?
C61 C60 C59 123.5(3) . . ?
C61 C60 H60 118.2 . . ?
C59 C60 H60 118.2 . . ?
O1 C1 C2 109.0(3) . . ?
O1 C1 H1A 109.9 . . ?
C2 C1 H1A 109.9 . . ?
O1 C1 H1B 109.9 . . ?
C2 C1 H1B 109.9 . . ?
H1A C1 H1B 108.3 . . ?
C20 C19 C18 101.3(3) . . ?
C20 C19 H19A 111.5 . . ?
C18 C19 H19A 111.5 . . ?
C20 C19 H19B 111.5 . . ?
C18 C19 H19B 111.5 . . ?
H19A C19 H19B 109.3 . . ?
C41 C42 C43 119.8(4) . . ?
C41 C42 H42 120.1 . . ?
C43 C42 H42 120.1 . . ?
C33 C34 C35 101.5(3) . . ?
C33 C34 H34A 111.5 . . ?
C35 C34 H34A 111.5 . . ?
C33 C34 H34B 111.5 . . ?
C35 C34 H34B 111.5 . . ?
H34A C34 H34B 109.3 . . ?
C44 C43 C42 120.3(4) . . ?
C44 C43 H43 119.8 . . ?
C42 C43 H43 119.8 . . ?
O6 C10 C9 108.8(3) . . ?
O6 C10 H10A 109.9 . . ?
C9 C10 H10A 109.9 . . ?
O6 C10 H10B 109.9 . . ?
C9 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
O9 C32 C31 108.8(3) . . ?
O9 C32 H32A 109.9 . . ?
C31 C32 H32A 109.9 . . ?
O9 C32 H32B 109.9 . . ?
C31 C32 H32B 109.9 . . ?
H32A C32 H32B 108.3 . . ?
C63 C62 C61 121.5(4) . . ?
C63 C62 H62 119.2 . . ?
C61 C62 H62 119.2 . . ?
C67 C66 C65 122.7(3) . . ?
C67 C66 C61 118.8(3) . . ?
C65 C66 C61 118.5(3) . . ?
O15 C33 C34 105.0(3) . . ?
O15 C33 H33A 110.7 . . ?
C34 C33 H33A 110.7 . . ?
O15 C33 H33B 110.7 . . ?
C34 C33 H33B 110.7 . . ?
H33A C33 H33B 108.8 . . ?
O8 C17 C18 106.7(3) . . ?
O8 C17 H17A 110.4 . . ?
C18 C17 H17A 110.4 . . ?
O8 C17 H17B 110.4 . . ?
C18 C17 H17B 110.4 . . ?
H17A C17 H17B 108.6 . . ?
C43 C44 C45 121.9(4) . . ?
C43 C44 H44 119.0 . . ?
C45 C44 H44 119.0 . . ?
O14 C30 C29 109.1(3) . . ?
O14 C30 H30A 109.9 . . ?
C29 C30 H30A 109.9 . . ?
O14 C30 H30B 109.9 . . ?
C29 C30 H30B 109.9 . . ?
H30A C30 H30B 108.3 . . ?
O11 C25 C26 109.5(3) . . ?
O11 C25 H25A 109.8 . . ?
C26 C25 H25A 109.8 . . ?
O11 C25 H25B 109.8 . . ?
C26 C25 H25B 109.8 . . ?
H25A C25 H25B 108.2 . . ?
O5 C9 C10 108.3(3) . . ?
O5 C9 H9A 110.0 . . ?
C10 C9 H9A 110.0 . . ?
O5 C9 H9B 110.0 . . ?
C10 C9 H9B 110.0 . . ?
H9A C9 H9B 108.4 . . ?
O8 C20 C19 105.1(3) . . ?
O8 C20 H20A 110.7 . . ?
C19 C20 H20A 110.7 . . ?
O8 C20 H20B 110.7 . . ?
C19 C20 H20B 110.7 . . ?
H20A C20 H20B 108.8 . . ?
O16 C37 C38 107.4(3) . . ?
O16 C37 H37A 110.2 . . ?
C38 C37 H37A 110.2 . . ?
O16 C37 H37B 110.2 . . ?
C38 C37 H37B 110.2 . . ?
H37A C37 H37B 108.5 . . ?
O3 C4 C3 108.4(3) . . ?
O3 C4 H4A 110.0 . . ?
C3 C4 H4A 110.0 . . ?
O3 C4 H4B 110.0 . . ?
C3 C4 H4B 110.0 . . ?
H4A C4 H4B 108.4 . . ?
C62 C63 C64 120.0(4) . . ?
C62 C63 H63 120.0 . . ?
C64 C63 H63 120.0 . . ?
O14 C31 C32 109.0(3) . . ?
O14 C31 H31A 109.9 . . ?
C32 C31 H31A 109.9 . . ?
O14 C31 H31B 109.9 . . ?
C32 C31 H31B 109.9 . . ?
H31A C31 H31B 108.3 . . ?
O7 C16 C15 105.6(3) . . ?
O7 C16 H16A 110.6 . . ?
C15 C16 H16A 110.6 . . ?
O7 C16 H16B 110.6 . . ?
C15 C16 H16B 110.6 . . ?
H16A C16 H16B 108.8 . . ?
O11 C24 C23 109.3(3) . . ?
O11 C24 H24A 109.8 . . ?
C23 C24 H24A 109.8 . . ?
O11 C24 H24B 109.8 . . ?
C23 C24 H24B 109.8 . . ?
H24A C24 H24B 108.3 . . ?
O16 C40 C39 105.2(3) . . ?
O16 C40 H40A 110.7 . . ?
C39 C40 H40A 110.7 . . ?
O16 C40 H40B 110.7 . . ?
C39 C40 H40B 110.7 . . ?
H40A C40 H40B 108.8 . . ?
O13 C29 C30 108.8(3) . . ?
O13 C29 H29A 109.9 . . ?
C30 C29 H29A 109.9 . . ?
O13 C29 H29B 109.9 . . ?
C30 C29 H29B 109.9 . . ?
H29A C29 H29B 108.3 . . ?
C65 C64 C63 120.4(4) . . ?
C65 C64 H64 119.8 . . ?
C63 C64 H64 119.8 . . ?
O7 C13 C14 106.1(3) . . ?
O7 C13 H13A 110.5 . . ?
C14 C13 H13A 110.5 . . ?
O7 C13 H13B 110.5 . . ?
C14 C13 H13B 110.5 . . ?
H13A C13 H13B 108.7 . . ?
O12 C26 C25 108.8(3) . . ?
O12 C26 H26A 109.9 . . ?
C25 C26 H26A 109.9 . . ?
O12 C26 H26B 109.9 . . ?
C25 C26 H26B 109.9 . . ?
H26A C26 H26B 108.3 . . ?
O13 C28 C27 109.0(3) . . ?
O13 C28 H28A 109.9 . . ?
C27 C28 H28A 109.9 . . ?
O13 C28 H28B 109.9 . . ?
C27 C28 H28B 109.9 . . ?
H28A C28 H28B 108.3 . . ?
O12 C27 C28 109.3(3) . . ?
O12 C27 H27A 109.8 . . ?
C28 C27 H27A 109.8 . . ?
O12 C27 H27B 109.8 . . ?
C28 C27 H27B 109.8 . . ?
H27A C27 H27B 108.3 . . ?
O15 C36 C35 106.7(3) . . ?
O15 C36 H36A 110.4 . . ?
C35 C36 H36A 110.4 . . ?
O15 C36 H36B 110.4 . . ?
C35 C36 H36B 110.4 . . ?
H36A C36 H36B 108.6 . . ?
C15 C14 C13 102.2(3) . . ?
C15 C14 H14A 111.3 . . ?
C13 C14 H14A 111.3 . . ?
C15 C14 H14B 111.3 . . ?
C13 C14 H14B 111.3 . . ?
H14A C14 H14B 109.2 . . ?
C38 C39 C40 103.0(3) . . ?
C38 C39 H39A 111.2 . . ?
C40 C39 H39A 111.2 . . ?
C38 C39 H39B 111.2 . . ?
C40 C39 H39B 111.2 . . ?
H39A C39 H39B 109.1 . . ?
C16 C15 C14 102.3(3) . . ?
C16 C15 H15A 111.3 . . ?
C14 C15 H15A 111.3 . . ?
C16 C15 H15B 111.3 . . ?
C14 C15 H15B 111.3 . . ?
H15A C15 H15B 109.2 . . ?
C39 C38 C37 104.8(3) . . ?
C39 C38 H38A 110.8 . . ?
C37 C38 H38A 110.8 . . ?
C39 C38 H38B 110.8 . . ?
C37 C38 H38B 110.8 . . ?
H38A C38 H38B 108.9 . . ?

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
C41 C54 C45 C46 179.7(3) . . . . ?
C53 C54 C45 C46 0.2(4) . . . . ?
C41 C54 C45 C44 -0.4(4) . . . . ?
C53 C54 C45 C44 -179.8(3) . . . . ?
C60 C59 C58 C57 179.7(3) . . . . ?
C68 C59 C58 C57 0.5(5) . . . . ?
C46 C47 C52 C53 1.0(4) . . . . ?
C48 C47 C52 C53 -179.2(3) . . . . ?
C46 C47 C52 C51 -178.5(3) . . . . ?
C48 C47 C52 C51 1.3(4) . . . . ?
C3 O2 C2 C1 -179.0(3) . . . . ?
K1 O2 C2 C1 -50.6(3) . . . . ?
C51 C52 C53 C54 178.1(3) . . . . ?
C47 C52 C53 C54 -1.4(4) . . . . ?
C41 C54 C53 C52 -178.6(3) . . . . ?
C45 C54 C53 C52 0.8(4) . . . . ?
C53 C52 C51 C50 -179.2(3) . . . . ?
C47 C52 C51 C50 0.4(5) . . . . ?
C52 C51 C50 C49 -1.1(5) . . . . ?
C51 C50 C49 C48 0.1(5) . . . . ?
C7 O4 C6 C5 176.7(3) . . . . ?
K1 O4 C6 C5 -42.8(3) . . . . ?
C66 C67 C68 C55 179.5(3) . . . . ?
C66 C67 C68 C59 -0.6(5) . . . . ?
C56 C55 C68 C67 -180.0(3) . . . . ?
C56 C55 C68 C59 0.2(5) . . . . ?
C58 C59 C68 C67 179.9(3) . . . . ?
C60 C59 C68 C67 0.6(4) . . . . ?
C58 C59 C68 C55 -0.2(4) . . . . ?
C60 C59 C68 C55 -179.6(3) . . . . ?
C50 C49 C48 C47 1.6(5) . . . . ?
C46 C47 C48 C49 177.5(3) . . . . ?
C52 C47 C48 C49 -2.3(5) . . . . ?
C32 O9 C21 C22 -177.0(3) . . . . ?
K2 O9 C21 C22 46.1(3) . . . . ?
C44 C45 C46 C47 179.5(3) . . . . ?
C54 C45 C46 C47 -0.6(5) . . . . ?
C48 C47 C46 C45 -179.8(3) . . . . ?
C52 C47 C46 C45 0.0(5) . . . . ?
C6 O4 C7 C8 -172.3(3) . . . . ?
K1 O4 C7 C8 48.7(3) . . . . ?
C9 O5 C8 C7 178.0(3) . . . . ?
K1 O5 C8 C7 47.3(3) . . . . ?
O4 C7 C8 O5 -62.6(3) . . . . ?
C23 O10 C22 C21 -178.9(3) . . . . ?
K2 O10 C22 C21 52.8(3) . . . . ?
O9 C21 C22 O10 -66.4(3) . . . . ?
C10 O6 C11 C12 -177.4(3) . . . . ?
K1 O6 C11 C12 50.9(3) . . . . ?
C59 C58 C57 C56 -0.6(5) . . . . ?
C53 C54 C41 C42 179.2(3) . . . . ?
C45 C54 C41 C42 -0.2(5) . . . . ?
C4 O3 C5 C6 177.4(3) . . . . ?
K1 O3 C5 C6 -58.2(3) . . . . ?
C4 O3 C5 K1 -124.4(3) . . . . ?
O4 C6 C5 O3 70.2(3) . . . . ?
O4 C6 C5 K1 29.0(2) . . . . ?
C22 O10 C23 C24 -176.0(3) . . . . ?
K2 O10 C23 C24 -48.4(3) . . . . ?
C2 O2 C3 C4 178.7(3) . . . . ?
K1 O2 C3 C4 50.8(3) . . . . ?
C68 C55 C56 C57 -0.3(5) . . . . ?
C58 C57 C56 C55 0.5(5) . . . . ?
C1 O1 C12 C11 -175.7(3) . . . . ?
K1 O1 C12 C11 47.1(3) . . . . ?
O6 C11 C12 O1 -66.2(4) . . . . ?
C62 C61 C60 C59 178.0(3) . . . . ?
C66 C61 C60 C59 -1.2(5) . . . . ?
C58 C59 C60 C61 -178.9(3) . . . . ?
C68 C59 C60 C61 0.3(5) . . . . ?
C12 O1 C1 C2 174.2(3) . . . . ?
K1 O1 C1 C2 -48.7(3) . . . . ?
O2 C2 C1 O1 66.7(3) . . . . ?
C17 C18 C19 C20 37.3(4) . . . . ?
C54 C41 C42 C43 0.5(5) . . . . ?
C36 C35 C34 C33 -37.5(4) . . . . ?
C41 C42 C43 C44 0.0(5) . . . . ?
C11 O6 C10 C9 -177.4(3) . . . . ?
K1 O6 C10 C9 -47.9(3) . . . . ?
C21 O9 C32 C31 174.6(3) . . . . ?
K2 O9 C32 C31 -48.2(3) . . . . ?
C60 C61 C62 C63 -179.5(3) . . . . ?
C66 C61 C62 C63 -0.2(5) . . . . ?
C68 C67 C66 C65 179.6(3) . . . . ?
C68 C67 C66 C61 -0.3(5) . . . . ?
C64 C65 C66 C67 177.7(3) . . . . ?
C64 C65 C66 C61 -2.4(5) . . . . ?
C60 C61 C66 C67 1.2(4) . . . . ?
C62 C61 C66 C67 -178.1(3) . . . . ?
C60 C61 C66 C65 -178.7(3) . . . . ?
C62 C61 C66 C65 2.0(4) . . . . ?
C36 O15 C33 C34 -20.1(4) . . . . ?
K2 O15 C33 C34 135.7(3) . . . . ?
C35 C34 C33 O15 35.9(4) . . . . ?
C20 O8 C17 C18 3.6(4) . . . . ?
K1 O8 C17 C18 177.1(2) . . . . ?
C19 C18 C17 O8 -26.0(4) . . . . ?
C42 C43 C44 C45 -0.7(5) . . . . ?
C46 C45 C44 C43 -179.2(3) . . . . ?
C54 C45 C44 C43 0.9(5) . . . . ?
C31 O14 C30 C29 -179.9(3) . . . . ?
K2 O14 C30 C29 48.2(3) . . . . ?
C24 O11 C25 C26 179.9(3) . . . . ?
K2 O11 C25 C26 53.7(3) . . . . ?
C8 O5 C9 C10 176.8(3) . . . . ?
K1 O5 C9 C10 -52.1(3) . . . . ?
O6 C10 C9 O5 67.0(4) . . . . ?
C17 O8 C20 C19 20.9(4) . . . . ?
K1 O8 C20 C19 -153.7(2) . . . . ?
C18 C19 C20 O8 -36.1(4) . . . . ?
C40 O16 C37 C38 -7.0(5) . . . . ?
K2 O16 C37 C38 150.7(3) . . . . ?
C5 O3 C4 C3 173.9(3) . . . . ?
K1 O3 C4 C3 52.4(3) . . . . ?
O2 C3 C4 O3 -70.6(4) . . . . ?
C61 C62 C63 C64 -1.2(5) . . . . ?
C30 O14 C31 C32 178.8(3) . . . . ?
K2 O14 C31 C32 -48.8(3) . . . . ?
O9 C32 C31 O14 64.4(4) . . . . ?
C13 O7 C16 C15 18.8(4) . . . . ?
K1 O7 C16 C15 -127.1(3) . . . . ?
C25 O11 C24 C23 -179.5(3) . . . . ?
K2 O11 C24 C23 -53.7(3) . . . . ?
O10 C23 C24 O11 70.1(4) . . . . ?
C37 O16 C40 C39 24.7(4) . . . . ?
K2 O16 C40 C39 -132.3(3) . . . . ?
C28 O13 C29 C30 -177.6(3) . . . . ?
K2 O13 C29 C30 50.6(3) . . . . ?
O14 C30 C29 O13 -66.7(4) . . . . ?
C66 C65 C64 C63 1.1(5) . . . . ?
C62 C63 C64 C65 0.8(5) . . . . ?
C16 O7 C13 C14 4.9(4) . . . . ?
K1 O7 C13 C14 147.6(2) . . . . ?
C27 O12 C26 C25 -174.1(3) . . . . ?
K2 O12 C26 C25 44.6(3) . . . . ?
O11 C25 C26 O12 -66.6(4) . . . . ?
C29 O13 C28 C27 -179.6(3) . . . . ?
K2 O13 C28 C27 -48.6(3) . . . . ?
C26 O12 C27 C28 174.5(3) . . . . ?
K2 O12 C27 C28 -45.1(3) . . . . ?
O13 C28 C27 O12 61.3(4) . . . . ?
C33 O15 C36 C35 -4.4(4) . . . . ?
K2 O15 C36 C35 -157.0(2) . . . . ?
C34 C35 C36 O15 26.6(4) . . . . ?
O7 C13 C14 C15 -26.1(4) . . . . ?
O16 C40 C39 C38 -32.2(5) . . . . ?
O7 C16 C15 C14 -34.7(4) . . . . ?
C13 C14 C15 C16 36.5(4) . . . . ?
C40 C39 C38 C37 27.5(5) . . . . ?
O16 C37 C38 C39 -13.6(5) . . . . ?

_refine_diff_density_max         0.326
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.050

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_947SF_0mS_a
_database_code_depnum_ccdc_archive 'CCDC 1431114'
_audit_update_record             
;
2015-10-13 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H24 O6 Li, C10 H8'
_chemical_formula_sum            'C22 H32 Li O6'
_chemical_formula_weight         399.41

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'
Li Li -0.0003 0.0001 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_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, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   8.6020(3)
_cell_length_b                   21.8870(8)
_cell_length_c                   22.2344(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4186.1(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7581
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      27.46

_exptl_crystal_description       irregular
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_F_000             1720
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.045
_exptl_absorpt_coefficient_mu    0.090
_shelx_estimated_absorpt_T_min   0.7110
_shelx_estimated_absorpt_T_max   0.7456
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7110
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus tube'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            44126
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.832
_diffrn_reflns_theta_max         27.551
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4827
_reflns_number_gt                3792
_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-2014/6 (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)+(0.0365P)²+1.7924P] 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_number_reflns         4827
_refine_ls_number_parameters     262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0368
_refine_ls_wR_factor_ref         0.0918
_refine_ls_wR_factor_gt          0.0810
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.001
_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
Li1 Li 0.4513(3) 0.63971(10) 0.35964(10) 0.0195(4) Uani 1 1 d . . . . .
O1 O 0.40480(10) 0.68654(4) 0.27867(4) 0.01579(19) Uani 1 1 d . . . . .
O2 O 0.52403(10) 0.57626(4) 0.29403(4) 0.0190(2) Uani 1 1 d . . . . .
O3 O 0.49236(10) 0.56274(4) 0.41229(4) 0.0180(2) Uani 1 1 d . . . . .
O4 O 0.20223(10) 0.61281(4) 0.38227(4) 0.01776(19) Uani 1 1 d . . . . .
O5 O 0.37772(10) 0.70335(4) 0.42291(4) 0.01740(19) Uani 1 1 d . . . . .
O6 O 0.64372(10) 0.70919(4) 0.35952(4) 0.0189(2) Uani 1 1 d . . . . .
C1 C 0.46539(16) 0.65484(6) 0.22696(6) 0.0203(3) Uani 1 1 d . . . . .
H1A H 0.5768 0.6645 0.2213 0.024 Uiso 1 1 calc R U . . .
H1B H 0.4081 0.6670 0.1902 0.024 Uiso 1 1 calc R U . . .
C2 C 0.44439(16) 0.58778(6) 0.23883(6) 0.0213(3) Uani 1 1 d . . . . .
H2A H 0.3327 0.5775 0.2426 0.026 Uiso 1 1 calc R U . . .
H2B H 0.4897 0.5632 0.2058 0.026 Uiso 1 1 calc R U . . .
C3 C 0.51557(17) 0.51443(6) 0.31441(6) 0.0247(3) Uani 1 1 d . . . . .
H3A H 0.5834 0.4878 0.2898 0.030 Uiso 1 1 calc R U . . .
H3B H 0.4076 0.4990 0.3118 0.030 Uiso 1 1 calc R U . . .
C4 C 0.57012(17) 0.51556(6) 0.37894(6) 0.0245(3) Uani 1 1 d . . . . .
H4A H 0.5491 0.4755 0.3979 0.029 Uiso 1 1 calc R U . . .
H4B H 0.6837 0.5227 0.3801 0.029 Uiso 1 1 calc R U . . .
C5 C 0.35488(15) 0.54417(6) 0.44443(6) 0.0189(3) Uani 1 1 d . . . . .
H5A H 0.3447 0.5690 0.4814 0.023 Uiso 1 1 calc R U . . .
H5B H 0.3654 0.5008 0.4565 0.023 Uiso 1 1 calc R U . . .
C6 C 0.20961(15) 0.55169(6) 0.40639(6) 0.0193(3) Uani 1 1 d . . . . .
H6A H 0.2110 0.5217 0.3730 0.023 Uiso 1 1 calc R U . . .
H6B H 0.1164 0.5437 0.4313 0.023 Uiso 1 1 calc R U . . .
C7 C 0.13511(15) 0.65553(6) 0.42387(6) 0.0189(3) Uani 1 1 d . . . . .
H7A H 0.1488 0.6407 0.4656 0.023 Uiso 1 1 calc R U . . .
H7B H 0.0224 0.6600 0.4159 0.023 Uiso 1 1 calc R U . . .
C8 C 0.21510(14) 0.71586(6) 0.41605(6) 0.0183(3) Uani 1 1 d . . . . .
H8A H 0.1934 0.7330 0.3757 0.022 Uiso 1 1 calc R U . . .
H8B H 0.1795 0.7454 0.4469 0.022 Uiso 1 1 calc R U . . .
C9 C 0.47089(15) 0.75676(6) 0.43203(6) 0.0195(3) Uani 1 1 d . . . . .
H9A H 0.4634 0.7708 0.4743 0.023 Uiso 1 1 calc R U . . .
H9B H 0.4363 0.7902 0.4053 0.023 Uiso 1 1 calc R U . . .
C10 C 0.63539(15) 0.73819(6) 0.41730(6) 0.0208(3) Uani 1 1 d . . . . .
H10A H 0.7030 0.7748 0.4175 0.025 Uiso 1 1 calc R U . . .
H10B H 0.6740 0.7097 0.4485 0.025 Uiso 1 1 calc R U . . .
C11 C 0.62433(14) 0.75002(6) 0.30934(6) 0.0199(3) Uani 1 1 d . . . . .
H11A H 0.6989 0.7387 0.2773 0.024 Uiso 1 1 calc R U . . .
H11B H 0.6485 0.7922 0.3224 0.024 Uiso 1 1 calc R U . . .
C12 C 0.46011(14) 0.74823(6) 0.28390(6) 0.0171(3) Uani 1 1 d . . . . .
H12A H 0.3897 0.7716 0.3105 0.020 Uiso 1 1 calc R U . . .
H12B H 0.4591 0.7679 0.2438 0.020 Uiso 1 1 calc R U . . .
C13 C 0.23215(14) 0.38590(5) 0.35590(6) 0.0150(2) Uani 1 1 d . . . . .
C14 C 0.09463(15) 0.40107(6) 0.32419(6) 0.0200(3) Uani 1 1 d . . . . .
H14 H 0.0935 0.3981 0.2816 0.024 Uiso 1 1 calc R U . . .
C15 C -0.04020(15) 0.42042(6) 0.35446(7) 0.0246(3) Uani 1 1 d . . . . .
H15 H -0.1318 0.4295 0.3323 0.029 Uiso 1 1 calc R U . . .
C16 C -0.03976(15) 0.42622(6) 0.41638(7) 0.0242(3) Uani 1 1 d . . . . .
H16 H -0.1312 0.4391 0.4367 0.029 Uiso 1 1 calc R U . . .
C17 C 0.09496(15) 0.41312(6) 0.44927(6) 0.0202(3) Uani 1 1 d . . . . .
H17 H 0.0942 0.4184 0.4917 0.024 Uiso 1 1 calc R U . . .
C18 C 0.23240(15) 0.39223(5) 0.42078(5) 0.0152(2) Uani 1 1 d . . . . .
C19 C 0.36990(15) 0.37690(5) 0.45262(6) 0.0186(3) Uani 1 1 d . . . . .
H19 H 0.3720 0.3811 0.4951 0.022 Uiso 1 1 calc R U . . .
C20 C 0.50261(15) 0.35567(6) 0.42272(6) 0.0217(3) Uani 1 1 d . . . . .
H20 H 0.5929 0.3452 0.4450 0.026 Uiso 1 1 calc R U . . .
C21 C 0.50260(15) 0.34986(6) 0.36077(6) 0.0213(3) Uani 1 1 d . . . . .
H21 H 0.5933 0.3359 0.3407 0.026 Uiso 1 1 calc R U . . .
C22 C 0.36932(15) 0.36456(6) 0.32749(6) 0.0185(3) Uani 1 1 d . . . . .
H22 H 0.3710 0.3601 0.2850 0.022 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
Li1 O5 2.078(2) . ?
Li1 O3 2.081(2) . ?
Li1 O2 2.109(2) . ?
Li1 O1 2.110(2) . ?
Li1 O6 2.248(2) . ?
Li1 O4 2.278(2) . ?
O1 C12 1.4362(14) . ?
O1 C1 1.4405(14) . ?
O2 C2 1.4280(15) . ?
O2 C3 1.4288(15) . ?
O3 C4 1.4365(15) . ?
O3 C5 1.4403(15) . ?
O4 C7 1.4364(15) . ?
O4 C6 1.4426(15) . ?
O5 C9 1.4318(15) . ?
O5 C8 1.4335(15) . ?
O6 C10 1.4346(15) . ?
O6 C11 1.4390(15) . ?
C1 C2 1.5023(18) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.510(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.5179(18) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.4990(17) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.5082(18) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.5222(17) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.4166(17) . ?
C13 C22 1.4175(17) . ?
C13 C18 1.4493(17) . ?
C14 C15 1.4061(19) . ?
C14 H14 0.9500 . ?
C15 C16 1.383(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.400(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.4170(17) . ?
C17 H17 0.9500 . ?
C18 C19 1.4187(18) . ?
C19 C20 1.4004(19) . ?
C19 H19 0.9500 . ?
C20 C21 1.3833(19) . ?
C20 H20 0.9500 . ?
C21 C22 1.4019(18) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?

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
O5 Li1 O3 102.33(10) . . ?
O5 Li1 O2 178.83(13) . . ?
O3 Li1 O2 78.80(8) . . ?
O5 Li1 O1 101.20(10) . . ?
O3 Li1 O1 154.85(12) . . ?
O2 Li1 O1 77.64(8) . . ?
O5 Li1 O6 76.80(8) . . ?
O3 Li1 O6 115.03(10) . . ?
O2 Li1 O6 103.07(10) . . ?
O1 Li1 O6 79.04(8) . . ?
O5 Li1 O4 74.78(8) . . ?
O3 Li1 O4 80.00(8) . . ?
O2 Li1 O4 105.17(10) . . ?
O1 Li1 O4 97.81(9) . . ?
O6 Li1 O4 150.19(11) . . ?
C12 O1 C1 113.42(9) . . ?
C12 O1 Li1 108.96(9) . . ?
C1 O1 Li1 112.24(9) . . ?
C2 O2 C3 114.55(10) . . ?
C2 O2 Li1 109.62(9) . . ?
C3 O2 Li1 112.89(9) . . ?
C4 O3 C5 115.82(10) . . ?
C4 O3 Li1 111.76(10) . . ?
C5 O3 Li1 111.60(9) . . ?
C7 O4 C6 112.46(9) . . ?
C7 O4 Li1 110.61(9) . . ?
C6 O4 Li1 106.29(9) . . ?
C9 O5 C8 113.91(9) . . ?
C9 O5 Li1 118.21(10) . . ?
C8 O5 Li1 110.67(9) . . ?
C10 O6 C11 114.44(10) . . ?
C10 O6 Li1 105.15(9) . . ?
C11 O6 Li1 109.61(9) . . ?
O1 C1 C2 106.67(10) . . ?
O1 C1 H1A 110.4 . . ?
C2 C1 H1A 110.4 . . ?
O1 C1 H1B 110.4 . . ?
C2 C1 H1B 110.4 . . ?
H1A C1 H1B 108.6 . . ?
O2 C2 C1 105.42(10) . . ?
O2 C2 H2A 110.7 . . ?
C1 C2 H2A 110.7 . . ?
O2 C2 H2B 110.7 . . ?
C1 C2 H2B 110.7 . . ?
H2A C2 H2B 108.8 . . ?
O2 C3 C4 105.67(11) . . ?
O2 C3 H3A 110.6 . . ?
C4 C3 H3A 110.6 . . ?
O2 C3 H3B 110.6 . . ?
C4 C3 H3B 110.6 . . ?
H3A C3 H3B 108.7 . . ?
O3 C4 C3 110.95(11) . . ?
O3 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
O3 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.0 . . ?
O3 C5 C6 111.64(10) . . ?
O3 C5 H5A 109.3 . . ?
C6 C5 H5A 109.3 . . ?
O3 C5 H5B 109.3 . . ?
C6 C5 H5B 109.3 . . ?
H5A C5 H5B 108.0 . . ?
O4 C6 C5 110.11(10) . . ?
O4 C6 H6A 109.6 . . ?
C5 C6 H6A 109.6 . . ?
O4 C6 H6B 109.6 . . ?
C5 C6 H6B 109.6 . . ?
H6A C6 H6B 108.2 . . ?
O4 C7 C8 108.31(10) . . ?
O4 C7 H7A 110.0 . . ?
C8 C7 H7A 110.0 . . ?
O4 C7 H7B 110.0 . . ?
C8 C7 H7B 110.0 . . ?
H7A C7 H7B 108.4 . . ?
O5 C8 C7 105.51(10) . . ?
O5 C8 H8A 110.6 . . ?
C7 C8 H8A 110.6 . . ?
O5 C8 H8B 110.6 . . ?
C7 C8 H8B 110.6 . . ?
H8A C8 H8B 108.8 . . ?
O5 C9 C10 105.93(10) . . ?
O5 C9 H9A 110.6 . . ?
C10 C9 H9A 110.6 . . ?
O5 C9 H9B 110.6 . . ?
C10 C9 H9B 110.6 . . ?
H9A C9 H9B 108.7 . . ?
O6 C10 C9 111.13(10) . . ?
O6 C10 H10A 109.4 . . ?
C9 C10 H10A 109.4 . . ?
O6 C10 H10B 109.4 . . ?
C9 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
O6 C11 C12 112.32(10) . . ?
O6 C11 H11A 109.1 . . ?
C12 C11 H11A 109.1 . . ?
O6 C11 H11B 109.1 . . ?
C12 C11 H11B 109.1 . . ?
H11A C11 H11B 107.9 . . ?
O1 C12 C11 111.21(10) . . ?
O1 C12 H12A 109.4 . . ?
C11 C12 H12A 109.4 . . ?
O1 C12 H12B 109.4 . . ?
C11 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
C14 C13 C22 123.41(12) . . ?
C14 C13 C18 118.31(11) . . ?
C22 C13 C18 118.28(11) . . ?
C15 C14 C13 121.41(12) . . ?
C15 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
C16 C15 C14 120.13(12) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C15 C16 C17 120.24(12) . . ?
C15 C16 H16 119.9 . . ?
C17 C16 H16 119.9 . . ?
C16 C17 C18 121.55(12) . . ?
C16 C17 H17 119.2 . . ?
C18 C17 H17 119.2 . . ?
C17 C18 C19 123.30(12) . . ?
C17 C18 C13 118.33(11) . . ?
C19 C18 C13 118.37(11) . . ?
C20 C19 C18 121.42(12) . . ?
C20 C19 H19 119.3 . . ?
C18 C19 H19 119.3 . . ?
C21 C20 C19 120.21(12) . . ?
C21 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
C20 C21 C22 120.30(12) . . ?
C20 C21 H21 119.9 . . ?
C22 C21 H21 119.9 . . ?
C21 C22 C13 121.41(12) . . ?
C21 C22 H22 119.3 . . ?
C13 C22 H22 119.3 . . ?

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
C12 O1 C1 C2 160.79(10) . . . . ?
Li1 O1 C1 C2 36.76(13) . . . . ?
C3 O2 C2 C1 178.77(10) . . . . ?
Li1 O2 C2 C1 50.68(13) . . . . ?
O1 C1 C2 O2 -56.95(13) . . . . ?
C2 O2 C3 C4 -166.26(11) . . . . ?
Li1 O2 C3 C4 -39.85(14) . . . . ?
C5 O3 C4 C3 93.83(13) . . . . ?
Li1 O3 C4 C3 -35.46(15) . . . . ?
O2 C3 C4 O3 48.99(14) . . . . ?
C4 O3 C5 C6 -90.89(13) . . . . ?
Li1 O3 C5 C6 38.48(13) . . . . ?
C7 O4 C6 C5 -84.13(13) . . . . ?
Li1 O4 C6 C5 37.03(13) . . . . ?
O3 C5 C6 O4 -52.04(14) . . . . ?
C6 O4 C7 C8 145.11(10) . . . . ?
Li1 O4 C7 C8 26.45(13) . . . . ?
C9 O5 C8 C7 -165.11(10) . . . . ?
Li1 O5 C8 C7 58.84(12) . . . . ?
O4 C7 C8 O5 -54.43(13) . . . . ?
C8 O5 C9 C10 -161.30(10) . . . . ?
Li1 O5 C9 C10 -28.76(14) . . . . ?
C11 O6 C10 C9 72.39(13) . . . . ?
Li1 O6 C10 C9 -47.94(12) . . . . ?
O5 C9 C10 O6 51.45(13) . . . . ?
C10 O6 C11 C12 -99.62(12) . . . . ?
Li1 O6 C11 C12 18.20(14) . . . . ?
C1 O1 C12 C11 -78.51(12) . . . . ?
Li1 O1 C12 C11 47.30(13) . . . . ?
O6 C11 C12 O1 -44.05(14) . . . . ?
C22 C13 C14 C15 178.16(12) . . . . ?
C18 C13 C14 C15 -1.51(18) . . . . ?
C13 C14 C15 C16 1.3(2) . . . . ?
C14 C15 C16 C17 0.3(2) . . . . ?
C15 C16 C17 C18 -1.65(19) . . . . ?
C16 C17 C18 C19 -178.24(12) . . . . ?
C16 C17 C18 C13 1.41(18) . . . . ?
C14 C13 C18 C17 0.16(17) . . . . ?
C22 C13 C18 C17 -179.53(11) . . . . ?
C14 C13 C18 C19 179.82(11) . . . . ?
C22 C13 C18 C19 0.14(17) . . . . ?
C17 C18 C19 C20 179.17(12) . . . . ?
C13 C18 C19 C20 -0.48(18) . . . . ?
C18 C19 C20 C21 0.75(19) . . . . ?
C19 C20 C21 C22 -0.67(19) . . . . ?
C20 C21 C22 C13 0.33(19) . . . . ?
C14 C13 C22 C21 -179.74(12) . . . . ?
C18 C13 C22 C21 -0.07(18) . . . . ?

_refine_diff_density_max         0.316
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.041

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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 
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data_969SF_0mS_a
_database_code_depnum_ccdc_archive 'CCDC 1431115'
_audit_update_record             
;
2015-10-13 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 O2 H10, Na C12 H24 O6, C14 H10'
_chemical_formula_sum            'C30 H44 Na O8'
_chemical_formula_weight         555.64

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'

_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                   11.5114(7)
_cell_length_b                   11.8386(7)
_cell_length_c                   13.6270(8)
_cell_angle_alpha                65.2130(10)
_cell_angle_beta                 70.1690(10)
_cell_angle_gamma                63.7510(10)
_cell_volume                     1484.90(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2520
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      27.32

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_F_000             598
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.101
_shelx_estimated_absorpt_T_min   0.982
_shelx_estimated_absorpt_T_max   0.998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6966
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus tube'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16775
_diffrn_reflns_av_unetI/netI     0.0727
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.676
_diffrn_reflns_theta_max         27.588
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6810
_reflns_number_gt                4442
_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-2014/6 (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)+(0.0335P)²+0.4683P] 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_number_reflns         6810
_refine_ls_number_parameters     354
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0491
_refine_ls_wR_factor_ref         0.1074
_refine_ls_wR_factor_gt          0.0873
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_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
Na01 Na 0.11494(7) 0.28539(7) 0.24423(6) 0.01964(19) Uani 1 1 d . . . . .
O8 O 0.18314(13) 0.04358(13) 0.31363(10) 0.0196(3) Uani 1 1 d . . . . .
O3 O 0.33640(13) 0.23956(13) 0.11500(10) 0.0204(3) Uani 1 1 d . . . . .
O4 O 0.11860(12) 0.22987(13) 0.08266(10) 0.0204(3) Uani 1 1 d . . . . .
O2 O 0.19747(13) 0.48019(13) 0.15003(10) 0.0218(3) Uani 1 1 d . . . . .
O6 O -0.08716(13) 0.27225(13) 0.38952(10) 0.0220(3) Uani 1 1 d . . . . .
O5 O -0.11442(13) 0.40048(13) 0.16389(10) 0.0219(3) Uani 1 1 d . . . . .
O1 O 0.02707(13) 0.46074(13) 0.34518(10) 0.0232(3) Uani 1 1 d . . . . .
O7 O 0.25113(13) 0.17048(13) 0.40210(11) 0.0256(3) Uani 1 1 d . . . . .
C30 C 0.53928(18) 0.61268(19) 0.43066(15) 0.0171(4) Uani 1 1 d . . . . .
C28 C 0.54002(18) 0.42493(19) 0.60459(14) 0.0164(4) Uani 1 1 d . . . . .
C29 C 0.57536(18) 0.53698(19) 0.53461(14) 0.0181(4) Uani 1 1 d . . . . .
H29 H 0.6257 0.5626 0.5586 0.022 Uiso 1 1 calc R U . . .
C25 C 0.46190(19) 0.20323(19) 0.74301(15) 0.0211(5) Uani 1 1 d . . . . .
H25 H 0.4345 0.1299 0.7902 0.025 Uiso 1 1 calc R U . . .
C27 C 0.57925(19) 0.3457(2) 0.70745(15) 0.0209(4) Uani 1 1 d . . . . .
H27 H 0.6332 0.3677 0.7309 0.025 Uiso 1 1 calc R U . . .
C24 C 0.42254(18) 0.27645(19) 0.64224(15) 0.0191(4) Uani 1 1 d . . . . .
H24 H 0.3685 0.2519 0.6212 0.023 Uiso 1 1 calc R U . . .
C26 C 0.54143(19) 0.2370(2) 0.77520(15) 0.0224(5) Uani 1 1 d . . . . .
H26 H 0.5699 0.1856 0.8436 0.027 Uiso 1 1 calc R U . . .
C14 C 0.24191(19) -0.0280(2) 0.40884(15) 0.0221(5) Uani 1 1 d . . . . .
H14A H 0.2937 -0.1215 0.4112 0.026 Uiso 1 1 calc R U . . .
H14B H 0.1727 -0.0275 0.4761 0.026 Uiso 1 1 calc R U . . .
C23 C 1.1403(2) -0.06255(19) -0.02303(17) 0.0219(4) Uani 1 1 d . . . . .
C13 C 0.3299(2) 0.0375(2) 0.40331(16) 0.0241(5) Uani 1 1 d . . . . .
H13A H 0.3736 -0.0111 0.4679 0.029 Uiso 1 1 calc R U . . .
H13B H 0.3988 0.0372 0.3359 0.029 Uiso 1 1 calc R U . . .
C8 C -0.11425(19) 0.3117(2) 0.11761(15) 0.0208(4) Uani 1 1 d . . . . .
H8A H -0.1940 0.3505 0.0853 0.025 Uiso 1 1 calc R U . . .
H8B H -0.1139 0.2259 0.1754 0.025 Uiso 1 1 calc R U . . .
C12 C -0.09287(19) 0.4623(2) 0.42281(16) 0.0237(5) Uani 1 1 d . . . . .
H12A H -0.1694 0.5226 0.3861 0.028 Uiso 1 1 calc R U . . .
H12B H -0.0984 0.4937 0.4817 0.028 Uiso 1 1 calc R U . . .
C10 C -0.21007(19) 0.3126(2) 0.35777(15) 0.0233(5) Uani 1 1 d . . . . .
H10A H -0.2836 0.3400 0.4167 0.028 Uiso 1 1 calc R U . . .
H10B H -0.2159 0.2359 0.3500 0.028 Uiso 1 1 calc R U . . .
C21 C 0.9319(2) -0.01738(19) 0.11241(17) 0.0224(5) Uani 1 1 d . . . . .
C7 C 0.00763(19) 0.2907(2) 0.03011(15) 0.0219(5) Uani 1 1 d . . . . .
H7A H 0.0097 0.2325 -0.0061 0.026 Uiso 1 1 calc R U . . .
H7B H 0.0088 0.3768 -0.0265 0.026 Uiso 1 1 calc R U . . .
C6 C 0.23976(19) 0.1908(2) 0.00933(15) 0.0230(5) Uani 1 1 d . . . . .
H6A H 0.2466 0.2668 -0.0580 0.028 Uiso 1 1 calc R U . . .
H6B H 0.2450 0.1183 -0.0122 0.028 Uiso 1 1 calc R U . . .
C5 C 0.34946(19) 0.1438(2) 0.06967(16) 0.0232(5) Uani 1 1 d . . . . .
H5A H 0.3495 0.0597 0.1299 0.028 Uiso 1 1 calc R U . . .
H5B H 0.4351 0.1255 0.0182 0.028 Uiso 1 1 calc R U . . .
C4 C 0.3547(2) 0.35803(19) 0.03358(16) 0.0231(5) Uani 1 1 d . . . . .
H4A H 0.2919 0.3997 -0.0170 0.028 Uiso 1 1 calc R U . . .
H4B H 0.4455 0.3372 -0.0101 0.028 Uiso 1 1 calc R U . . .
C9 C -0.2254(2) 0.4264(2) 0.25053(15) 0.0242(5) Uani 1 1 d . . . . .
H9A H -0.3061 0.4426 0.2280 0.029 Uiso 1 1 calc R U . . .
H9B H -0.2366 0.5080 0.2623 0.029 Uiso 1 1 calc R U . . .
C22 C 1.0700(2) -0.0759(2) 0.08574(17) 0.0232(5) Uani 1 1 d . . . . .
H22 H 1.1180 -0.1270 0.1441 0.028 Uiso 1 1 calc R U . . .
C3 C 0.33120(19) 0.4499(2) 0.09264(16) 0.0241(5) Uani 1 1 d . . . . .
H3A H 0.3919 0.4070 0.1452 0.029 Uiso 1 1 calc R U . . .
H3B H 0.3465 0.5323 0.0395 0.029 Uiso 1 1 calc R U . . .
C16 C 0.0998(2) -0.0147(2) 0.31194(16) 0.0244(5) Uani 1 1 d . . . . .
H16A H 0.1504 -0.1077 0.3158 0.037 Uiso 1 1 calc R U . . .
H16B H 0.0646 0.0338 0.2437 0.037 Uiso 1 1 calc R U . . .
H16C H 0.0267 -0.0103 0.3752 0.037 Uiso 1 1 calc R U . . .
C11 C -0.0928(2) 0.3225(2) 0.47053(15) 0.0242(5) Uani 1 1 d . . . . .
H11A H -0.0160 0.2640 0.5073 0.029 Uiso 1 1 calc R U . . .
H11B H -0.1737 0.3199 0.5271 0.029 Uiso 1 1 calc R U . . .
C20 C 0.8595(2) -0.0319(2) 0.22132(17) 0.0265(5) Uani 1 1 d . . . . .
H20 H 0.9053 -0.0853 0.2810 0.032 Uiso 1 1 calc R U . . .
C17 C 0.7213(2) 0.1236(2) 0.04982(18) 0.0268(5) Uani 1 1 d . . . . .
H17 H 0.6728 0.1772 -0.0081 0.032 Uiso 1 1 calc R U . . .
C2 C 0.1622(2) 0.5735(2) 0.20495(17) 0.0283(5) Uani 1 1 d . . . . .
H2A H 0.1647 0.6602 0.1503 0.034 Uiso 1 1 calc R U . . .
H2B H 0.2254 0.5414 0.2533 0.034 Uiso 1 1 calc R U . . .
C1 C 0.0260(2) 0.5890(2) 0.27193(16) 0.0272(5) Uani 1 1 d . . . . .
H1A H 0.0008 0.6499 0.3139 0.033 Uiso 1 1 calc R U . . .
H1B H -0.0383 0.6262 0.2234 0.033 Uiso 1 1 calc R U . . .
C18 C 0.6543(2) 0.1079(2) 0.15746(18) 0.0310(5) Uani 1 1 d . . . . .
H18 H 0.5614 0.1506 0.1727 0.037 Uiso 1 1 calc R U . . .
C19 C 0.7236(2) 0.0294(2) 0.24355(18) 0.0304(5) Uani 1 1 d . . . . .
H19 H 0.6777 0.0179 0.3176 0.037 Uiso 1 1 calc R U . . .
C15 C 0.3251(2) 0.2354(2) 0.40828(19) 0.0354(6) Uani 1 1 d . . . . .
H15A H 0.3631 0.1849 0.4751 0.053 Uiso 1 1 calc R U . . .
H15B H 0.2672 0.3251 0.4105 0.053 Uiso 1 1 calc R U . . .
H15C H 0.3961 0.2410 0.3435 0.053 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
Na01 O8 2.4396(15) . ?
Na01 O6 2.5087(14) . ?
Na01 O4 2.5313(15) . ?
Na01 O3 2.5350(14) . ?
Na01 O2 2.5488(15) . ?
Na01 O1 2.6111(15) . ?
Na01 O7 2.6238(15) . ?
Na01 O5 2.7485(16) . ?
O8 C16 1.418(2) . ?
O8 C14 1.423(2) . ?
O3 C4 1.429(2) . ?
O3 C5 1.436(2) . ?
O4 C6 1.425(2) . ?
O4 C7 1.428(2) . ?
O2 C2 1.426(2) . ?
O2 C3 1.428(2) . ?
O6 C11 1.430(2) . ?
O6 C10 1.436(2) . ?
O5 C9 1.433(2) . ?
O5 C8 1.434(2) . ?
O1 C1 1.422(2) . ?
O1 C12 1.424(2) . ?
O7 C15 1.415(2) . ?
O7 C13 1.424(2) . ?
C30 C29 1.410(3) . ?
C30 C24 1.423(3) 2_666 ?
C30 C28 1.449(3) 2_666 ?
C28 C29 1.410(2) . ?
C28 C27 1.415(3) . ?
C28 C30 1.449(3) 2_666 ?
C29 H29 0.9500 . ?
C25 C24 1.385(3) . ?
C25 C26 1.390(3) . ?
C25 H25 0.9500 . ?
C27 C26 1.388(3) . ?
C27 H27 0.9500 . ?
C24 C30 1.423(3) 2_666 ?
C24 H24 0.9500 . ?
C26 H26 0.9500 . ?
C14 C13 1.492(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C23 C22 1.407(3) . ?
C23 C17 1.415(3) 2_755 ?
C23 C21 1.447(3) 2_755 ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C8 C7 1.502(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C12 C11 1.503(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C10 C9 1.515(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C21 C22 1.409(3) . ?
C21 C20 1.414(3) . ?
C21 C23 1.447(3) 2_755 ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C6 C5 1.510(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C4 C3 1.494(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C22 H22 0.9500 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C20 C19 1.387(3) . ?
C20 H20 0.9500 . ?
C17 C18 1.383(3) . ?
C17 C23 1.415(3) 2_755 ?
C17 H17 0.9500 . ?
C2 C1 1.496(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C18 C19 1.393(3) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?

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
O8 Na01 O6 83.19(5) . . ?
O8 Na01 O4 77.28(5) . . ?
O6 Na01 O4 111.40(5) . . ?
O8 Na01 O3 83.31(5) . . ?
O6 Na01 O3 166.49(5) . . ?
O4 Na01 O3 65.64(4) . . ?
O8 Na01 O2 144.37(5) . . ?
O6 Na01 O2 127.58(5) . . ?
O4 Na01 O2 102.40(5) . . ?
O3 Na01 O2 65.16(4) . . ?
O8 Na01 O1 131.50(5) . . ?
O6 Na01 O1 67.04(5) . . ?
O4 Na01 O1 148.30(5) . . ?
O3 Na01 O1 122.91(5) . . ?
O2 Na01 O1 63.23(4) . . ?
O8 Na01 O7 65.48(5) . . ?
O6 Na01 O7 88.25(5) . . ?
O4 Na01 O7 135.47(5) . . ?
O3 Na01 O7 85.90(5) . . ?
O2 Na01 O7 94.80(5) . . ?
O1 Na01 O7 75.82(5) . . ?
O8 Na01 O5 111.68(5) . . ?
O6 Na01 O5 65.71(4) . . ?
O4 Na01 O5 62.64(4) . . ?
O3 Na01 O5 120.14(5) . . ?
O2 Na01 O5 98.84(5) . . ?
O1 Na01 O5 90.51(5) . . ?
O7 Na01 O5 153.80(5) . . ?
C16 O8 C14 111.38(14) . . ?
C16 O8 Na01 117.83(11) . . ?
C14 O8 Na01 119.38(11) . . ?
C4 O3 C5 113.61(14) . . ?
C4 O3 Na01 112.62(10) . . ?
C5 O3 Na01 108.01(10) . . ?
C6 O4 C7 112.01(14) . . ?
C6 O4 Na01 119.86(11) . . ?
C7 O4 Na01 121.94(11) . . ?
C2 O2 C3 112.08(15) . . ?
C2 O2 Na01 119.62(11) . . ?
C3 O2 Na01 115.63(11) . . ?
C11 O6 C10 115.83(15) . . ?
C11 O6 Na01 108.59(11) . . ?
C10 O6 Na01 119.67(10) . . ?
C9 O5 C8 113.01(14) . . ?
C9 O5 Na01 109.59(11) . . ?
C8 O5 Na01 107.24(11) . . ?
C1 O1 C12 113.57(14) . . ?
C1 O1 Na01 112.89(11) . . ?
C12 O1 Na01 114.41(11) . . ?
C15 O7 C13 111.58(16) . . ?
C15 O7 Na01 119.03(12) . . ?
C13 O7 Na01 108.78(11) . . ?
C29 C30 C24 123.61(18) . 2_666 ?
C29 C30 C28 118.37(16) . 2_666 ?
C24 C30 C28 118.01(17) 2_666 2_666 ?
C29 C28 C27 123.42(18) . . ?
C29 C28 C30 118.66(17) . 2_666 ?
C27 C28 C30 117.91(17) . 2_666 ?
C28 C29 C30 122.95(18) . . ?
C28 C29 H29 118.5 . . ?
C30 C29 H29 118.5 . . ?
C24 C25 C26 120.05(18) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C26 C27 C28 122.09(19) . . ?
C26 C27 H27 119.0 . . ?
C28 C27 H27 119.0 . . ?
C25 C24 C30 121.83(19) . 2_666 ?
C25 C24 H24 119.1 . . ?
C30 C24 H24 119.1 2_666 . ?
C27 C26 C25 120.06(19) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
O8 C14 C13 108.08(15) . . ?
O8 C14 H14A 110.1 . . ?
C13 C14 H14A 110.1 . . ?
O8 C14 H14B 110.1 . . ?
C13 C14 H14B 110.1 . . ?
H14A C14 H14B 108.4 . . ?
C22 C23 C17 123.27(19) . 2_755 ?
C22 C23 C21 118.72(18) . 2_755 ?
C17 C23 C21 118.01(18) 2_755 2_755 ?
O7 C13 C14 108.13(16) . . ?
O7 C13 H13A 110.1 . . ?
C14 C13 H13A 110.1 . . ?
O7 C13 H13B 110.1 . . ?
C14 C13 H13B 110.1 . . ?
H13A C13 H13B 108.4 . . ?
O5 C8 C7 107.68(15) . . ?
O5 C8 H8A 110.2 . . ?
C7 C8 H8A 110.2 . . ?
O5 C8 H8B 110.2 . . ?
C7 C8 H8B 110.2 . . ?
H8A C8 H8B 108.5 . . ?
O1 C12 C11 107.24(15) . . ?
O1 C12 H12A 110.3 . . ?
C11 C12 H12A 110.3 . . ?
O1 C12 H12B 110.3 . . ?
C11 C12 H12B 110.3 . . ?
H12A C12 H12B 108.5 . . ?
O6 C10 C9 112.58(15) . . ?
O6 C10 H10A 109.1 . . ?
C9 C10 H10A 109.1 . . ?
O6 C10 H10B 109.1 . . ?
C9 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
C22 C21 C20 123.93(19) . . ?
C22 C21 C23 118.04(18) . 2_755 ?
C20 C21 C23 118.04(19) . 2_755 ?
O4 C7 C8 107.35(15) . . ?
O4 C7 H7A 110.2 . . ?
C8 C7 H7A 110.2 . . ?
O4 C7 H7B 110.2 . . ?
C8 C7 H7B 110.2 . . ?
H7A C7 H7B 108.5 . . ?
O4 C6 C5 107.03(15) . . ?
O4 C6 H6A 110.3 . . ?
C5 C6 H6A 110.3 . . ?
O4 C6 H6B 110.3 . . ?
C5 C6 H6B 110.3 . . ?
H6A C6 H6B 108.6 . . ?
O3 C5 C6 112.44(16) . . ?
O3 C5 H5A 109.1 . . ?
C6 C5 H5A 109.1 . . ?
O3 C5 H5B 109.1 . . ?
C6 C5 H5B 109.1 . . ?
H5A C5 H5B 107.8 . . ?
O3 C4 C3 107.35(15) . . ?
O3 C4 H4A 110.2 . . ?
C3 C4 H4A 110.2 . . ?
O3 C4 H4B 110.2 . . ?
C3 C4 H4B 110.2 . . ?
H4A C4 H4B 108.5 . . ?
O5 C9 C10 112.47(16) . . ?
O5 C9 H9A 109.1 . . ?
C10 C9 H9A 109.1 . . ?
O5 C9 H9B 109.1 . . ?
C10 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
C23 C22 C21 123.23(19) . . ?
C23 C22 H22 118.4 . . ?
C21 C22 H22 118.4 . . ?
O2 C3 C4 107.40(16) . . ?
O2 C3 H3A 110.2 . . ?
C4 C3 H3A 110.2 . . ?
O2 C3 H3B 110.2 . . ?
C4 C3 H3B 110.2 . . ?
H3A C3 H3B 108.5 . . ?
O8 C16 H16A 109.5 . . ?
O8 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O8 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O6 C11 C12 112.91(15) . . ?
O6 C11 H11A 109.0 . . ?
C12 C11 H11A 109.0 . . ?
O6 C11 H11B 109.0 . . ?
C12 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
C19 C20 C21 121.9(2) . . ?
C19 C20 H20 119.1 . . ?
C21 C20 H20 119.1 . . ?
C18 C17 C23 122.2(2) . 2_755 ?
C18 C17 H17 118.9 . . ?
C23 C17 H17 118.9 2_755 . ?
O2 C2 C1 108.61(16) . . ?
O2 C2 H2A 110.0 . . ?
C1 C2 H2A 110.0 . . ?
O2 C2 H2B 110.0 . . ?
C1 C2 H2B 110.0 . . ?
H2A C2 H2B 108.3 . . ?
O1 C1 C2 107.37(16) . . ?
O1 C1 H1A 110.2 . . ?
C2 C1 H1A 110.2 . . ?
O1 C1 H1B 110.2 . . ?
C2 C1 H1B 110.2 . . ?
H1A C1 H1B 108.5 . . ?
C17 C18 C19 119.8(2) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C20 C19 C18 120.1(2) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
O7 C15 H15A 109.5 . . ?
O7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 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
C27 C28 C29 C30 177.89(18) . . . . ?
C30 C28 C29 C30 -1.4(3) 2_666 . . . ?
C24 C30 C29 C28 -178.06(17) 2_666 . . . ?
C28 C30 C29 C28 1.3(3) 2_666 . . . ?
C29 C28 C27 C26 179.14(18) . . . . ?
C30 C28 C27 C26 -1.6(3) 2_666 . . . ?
C26 C25 C24 C30 -0.3(3) . . . 2_666 ?
C28 C27 C26 C25 -0.4(3) . . . . ?
C24 C25 C26 C27 1.3(3) . . . . ?
C16 O8 C14 C13 178.82(15) . . . . ?
Na01 O8 C14 C13 -38.46(18) . . . . ?
C15 O7 C13 C14 173.97(16) . . . . ?
Na01 O7 C13 C14 -52.75(16) . . . . ?
O8 C14 C13 O7 60.74(19) . . . . ?
C9 O5 C8 C7 -178.83(15) . . . . ?
Na01 O5 C8 C7 -57.95(15) . . . . ?
C1 O1 C12 C11 163.66(17) . . . . ?
Na01 O1 C12 C11 32.06(18) . . . . ?
C11 O6 C10 C9 99.51(18) . . . . ?
Na01 O6 C10 C9 -33.6(2) . . . . ?
C6 O4 C7 C8 172.94(15) . . . . ?
Na01 O4 C7 C8 -34.83(19) . . . . ?
O5 C8 C7 O4 62.11(19) . . . . ?
C7 O4 C6 C5 173.23(16) . . . . ?
Na01 O4 C6 C5 20.35(19) . . . . ?
C4 O3 C5 C6 -67.54(19) . . . . ?
Na01 O3 C5 C6 58.16(16) . . . . ?
O4 C6 C5 O3 -52.5(2) . . . . ?
C5 O3 C4 C3 177.03(16) . . . . ?
Na01 O3 C4 C3 53.81(17) . . . . ?
C8 O5 C9 C10 77.1(2) . . . . ?
Na01 O5 C9 C10 -42.42(19) . . . . ?
O6 C10 C9 O5 51.8(2) . . . . ?
C17 C23 C22 C21 -178.62(19) 2_755 . . . ?
C21 C23 C22 C21 1.3(3) 2_755 . . . ?
C20 C21 C22 C23 178.75(19) . . . . ?
C23 C21 C22 C23 -1.3(3) 2_755 . . . ?
C2 O2 C3 C4 -176.91(16) . . . . ?
Na01 O2 C3 C4 41.27(18) . . . . ?
O3 C4 C3 O2 -62.2(2) . . . . ?
C10 O6 C11 C12 -80.8(2) . . . . ?
Na01 O6 C11 C12 57.16(17) . . . . ?
O1 C12 C11 O6 -60.9(2) . . . . ?
C22 C21 C20 C19 178.94(19) . . . . ?
C23 C21 C20 C19 -1.0(3) 2_755 . . . ?
C3 O2 C2 C1 -174.31(16) . . . . ?
Na01 O2 C2 C1 -34.2(2) . . . . ?
C12 O1 C1 C2 173.48(16) . . . . ?
Na01 O1 C1 C2 -54.17(18) . . . . ?
O2 C2 C1 O1 57.1(2) . . . . ?
C23 C17 C18 C19 -0.2(3) 2_755 . . . ?
C21 C20 C19 C18 0.1(3) . . . . ?
C17 C18 C19 C20 0.5(3) . . . . ?

_refine_diff_density_max         0.250
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.053

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_970SF_0mSa_a
_database_code_depnum_ccdc_archive 'CCDC 1431116'
_audit_update_record             
;
2015-10-13 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Na C16 O8 H34, C20 H12'
_chemical_formula_sum            'C36 H46 Na O8'
_chemical_formula_weight         629.72

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   22.1045(7)
_cell_length_b                   12.5068(4)
_cell_length_c                   16.0000(9)
_cell_angle_alpha                90
_cell_angle_beta                 132.18
_cell_angle_gamma                90
_cell_volume                     3277.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9400
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      27.58

_exptl_crystal_description       Prism
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_F_000             1348
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.100
_shelx_estimated_absorpt_T_min   0.982
_shelx_estimated_absorpt_T_max   0.998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7039
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus tube'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17897
_diffrn_reflns_av_unetI/netI     0.0125
_diffrn_reflns_av_R_equivalents  0.0158
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.049
_diffrn_reflns_theta_max         27.608
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3809
_reflns_number_gt                3414
_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-2014/6 (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)+(0.0526P)²+2.0870P] 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_number_reflns         3809
_refine_ls_number_parameters     205
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0954
_refine_ls_wR_factor_gt          0.0920
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.001
_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 0.5000 0.85602(4) 0.2500 0.01555(13) Uani 1 2 d S T P . .
O1 O 0.61552(5) 0.74979(6) 0.43331(6) 0.02020(17) Uani 1 1 d . . . . .
O2 O 0.51890(4) 0.89750(6) 0.42924(6) 0.01863(16) Uani 1 1 d . . . . .
O3 O 0.40351(4) 0.76747(6) 0.24919(6) 0.01908(16) Uani 1 1 d . . . . .
O4 O 0.58385(5) 1.01449(6) 0.31788(6) 0.02462(18) Uani 1 1 d . . . . .
C1 C 0.62394(7) 0.65542(8) 0.39208(9) 0.0221(2) Uani 1 1 d . . . . .
H1A H 0.5710 0.6176 0.3392 0.027 Uiso 1 1 calc R U . . .
H1B H 0.6643 0.6067 0.4554 0.027 Uiso 1 1 calc R U . . .
C2 C 0.59019(7) 0.72545(9) 0.49315(9) 0.0210(2) Uani 1 1 d . . . . .
H2A H 0.6330 0.6837 0.5619 0.025 Uiso 1 1 calc R U . . .
H2B H 0.5395 0.6825 0.4451 0.025 Uiso 1 1 calc R U . . .
C3 C 0.57556(7) 0.82976(9) 0.52459(9) 0.0222(2) Uani 1 1 d . . . . .
H3A H 0.5544 0.8145 0.5617 0.027 Uiso 1 1 calc R U . . .
H3B H 0.6282 0.8680 0.5795 0.027 Uiso 1 1 calc R U . . .
C4 C 0.43712(7) 0.89564(8) 0.38439(9) 0.0200(2) Uani 1 1 d . . . . .
H4A H 0.4063 0.9555 0.3304 0.024 Uiso 1 1 calc R U . . .
H4B H 0.4383 0.9075 0.4466 0.024 Uiso 1 1 calc R U . . .
C5 C 0.39234(7) 0.79201(9) 0.32511(9) 0.0205(2) Uani 1 1 d . . . . .
H5A H 0.4145 0.7338 0.3809 0.025 Uiso 1 1 calc R U . . .
H5B H 0.3335 0.8001 0.2832 0.025 Uiso 1 1 calc R U . . .
C6 C 0.34781(7) 0.68848(9) 0.16751(9) 0.0223(2) Uani 1 1 d . . . . .
H6A H 0.2919 0.7183 0.1128 0.027 Uiso 1 1 calc R U . . .
H6B H 0.3472 0.6260 0.2050 0.027 Uiso 1 1 calc R U . . .
C7 C 0.54188(9) 1.10615(9) 0.30783(12) 0.0348(3) Uani 1 1 d . . . . .
H7A H 0.5717 1.1716 0.3189 0.042 Uiso 1 1 calc R U . . .
H7B H 0.5379 1.1047 0.3658 0.042 Uiso 1 1 calc R U . . .
C8 C 0.66226(8) 1.00381(13) 0.42813(10) 0.0400(3) Uani 1 1 d . . . . .
H8A H 0.6958 1.0662 0.4451 0.060 Uiso 1 1 calc R U . . .
H8B H 0.6887 0.9388 0.4318 0.060 Uiso 1 1 calc R U . . .
H8C H 0.6562 0.9991 0.4834 0.060 Uiso 1 1 calc R U . . .
C9 C 0.55145(6) 0.55263(8) 0.60830(8) 0.0160(2) Uani 1 1 d . . . . .
C10 C 0.60437(7) 0.60616(8) 0.71335(9) 0.0216(2) Uani 1 1 d . . . . .
H10 H 0.5819 0.6499 0.7353 0.026 Uiso 1 1 calc R U . . .
C11 C 0.68858(7) 0.59599(9) 0.78505(9) 0.0243(2) Uani 1 1 d . . . . .
H11 H 0.7227 0.6346 0.8541 0.029 Uiso 1 1 calc R U . . .
C12 C 0.72344(6) 0.53078(9) 0.75766(9) 0.0224(2) Uani 1 1 d . . . . .
H12 H 0.7812 0.5241 0.8084 0.027 Uiso 1 1 calc R U . . .
C13 C 0.67392(6) 0.47367(8) 0.65451(9) 0.0187(2) Uani 1 1 d . . . . .
C14 C 0.70825(7) 0.40552(9) 0.62503(10) 0.0248(2) Uani 1 1 d . . . . .
H14 H 0.7656 0.3943 0.6768 0.030 Uiso 1 1 calc R U . . .
C15 C 0.65866(7) 0.35517(9) 0.52116(10) 0.0270(2) Uani 1 1 d . . . . .
H15 H 0.6825 0.3103 0.5020 0.032 Uiso 1 1 calc R U . . .
C16 C 0.57456(7) 0.36915(9) 0.44439(9) 0.0228(2) Uani 1 1 d . . . . .
H16 H 0.5420 0.3346 0.3732 0.027 Uiso 1 1 calc R U . . .
C17 C 0.53627(6) 0.43371(8) 0.46992(8) 0.0159(2) Uani 1 1 d . . . . .
C18 C 0.58654(6) 0.48608(8) 0.57741(8) 0.01519(19) Uani 1 1 d . . . . .


_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 O3 2.3956(7) . ?
Na1 O3 2.3956(7) 2_655 ?
Na1 O4 2.4166(9) . ?
Na1 O4 2.4166(9) 2_655 ?
Na1 O1 2.6135(8) 2_655 ?
Na1 O1 2.6135(8) . ?
Na1 O2 2.6570(7) . ?
Na1 O2 2.6570(7) 2_655 ?
O1 C1 1.4240(12) . ?
O1 C2 1.4293(11) . ?
O2 C4 1.4287(12) . ?
O2 C3 1.4310(12) . ?
O3 C5 1.4260(12) . ?
O3 C6 1.4279(12) . ?
O4 C7 1.4143(15) . ?
O4 C8 1.4240(15) . ?
C1 C6 1.5065(15) 2_655 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.5092(15) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.5161(15) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C1 1.5065(15) 2_655 ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C7 1.501(3) 2_655 ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.4147(14) . ?
C9 C18 1.4330(13) . ?
C9 C17 1.4479(14) 5_666 ?
C10 C11 1.3891(16) . ?
C10 H10 0.9500 . ?
C11 C12 1.3800(16) . ?
C11 H11 0.9500 . ?
C12 C13 1.4164(15) . ?
C12 H12 0.9500 . ?
C13 C14 1.4161(15) . ?
C13 C18 1.4412(14) . ?
C14 C15 1.3834(17) . ?
C14 H14 0.9500 . ?
C15 C16 1.3887(16) . ?
C15 H15 0.9500 . ?
C16 C17 1.4140(14) . ?
C16 H16 0.9500 . ?
C17 C18 1.4337(13) . ?
C17 C9 1.4479(14) 5_666 ?

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
O3 Na1 O3 124.93(4) . 2_655 ?
O3 Na1 O4 142.47(3) . . ?
O3 Na1 O4 88.01(3) 2_655 . ?
O3 Na1 O4 88.01(3) . 2_655 ?
O3 Na1 O4 142.47(3) 2_655 2_655 ?
O4 Na1 O4 69.80(4) . 2_655 ?
O3 Na1 O1 64.11(2) . 2_655 ?
O3 Na1 O1 88.09(3) 2_655 2_655 ?
O4 Na1 O1 142.93(3) . 2_655 ?
O4 Na1 O1 92.06(3) 2_655 2_655 ?
O3 Na1 O1 88.08(3) . . ?
O3 Na1 O1 64.12(2) 2_655 . ?
O4 Na1 O1 92.06(3) . . ?
O4 Na1 O1 142.93(3) 2_655 . ?
O1 Na1 O1 118.90(4) 2_655 . ?
O3 Na1 O2 65.81(2) . . ?
O3 Na1 O2 126.17(2) 2_655 . ?
O4 Na1 O2 80.64(3) . . ?
O4 Na1 O2 80.92(3) 2_655 . ?
O1 Na1 O2 129.61(2) 2_655 . ?
O1 Na1 O2 63.95(2) . . ?
O3 Na1 O2 126.18(2) . 2_655 ?
O3 Na1 O2 65.81(2) 2_655 2_655 ?
O4 Na1 O2 80.92(3) . 2_655 ?
O4 Na1 O2 80.65(3) 2_655 2_655 ?
O1 Na1 O2 63.95(2) 2_655 2_655 ?
O1 Na1 O2 129.61(2) . 2_655 ?
O2 Na1 O2 157.48(4) . 2_655 ?
C1 O1 C2 111.45(8) . . ?
C1 O1 Na1 103.56(6) . . ?
C2 O1 Na1 109.45(6) . . ?
C4 O2 C3 115.62(7) . . ?
C4 O2 Na1 103.04(5) . . ?
C3 O2 Na1 115.20(6) . . ?
C5 O3 C6 113.11(8) . . ?
C5 O3 Na1 123.96(6) . . ?
C6 O3 Na1 122.84(6) . . ?
C7 O4 C8 112.14(10) . . ?
C7 O4 Na1 111.53(7) . . ?
C8 O4 Na1 114.08(7) . . ?
O1 C1 C6 107.72(8) . 2_655 ?
O1 C1 H1A 110.2 . . ?
C6 C1 H1A 110.2 2_655 . ?
O1 C1 H1B 110.2 . . ?
C6 C1 H1B 110.2 2_655 . ?
H1A C1 H1B 108.5 . . ?
O1 C2 C3 107.89(8) . . ?
O1 C2 H2A 110.1 . . ?
C3 C2 H2A 110.1 . . ?
O1 C2 H2B 110.1 . . ?
C3 C2 H2B 110.1 . . ?
H2A C2 H2B 108.4 . . ?
O2 C3 C2 112.73(8) . . ?
O2 C3 H3A 109.0 . . ?
C2 C3 H3A 109.0 . . ?
O2 C3 H3B 109.0 . . ?
C2 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
O2 C4 C5 113.74(8) . . ?
O2 C4 H4A 108.8 . . ?
C5 C4 H4A 108.8 . . ?
O2 C4 H4B 108.8 . . ?
C5 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
O3 C5 C4 107.65(8) . . ?
O3 C5 H5A 110.2 . . ?
C4 C5 H5A 110.2 . . ?
O3 C5 H5B 110.2 . . ?
C4 C5 H5B 110.2 . . ?
H5A C5 H5B 108.5 . . ?
O3 C6 C1 107.46(8) . 2_655 ?
O3 C6 H6A 110.2 . . ?
C1 C6 H6A 110.2 2_655 . ?
O3 C6 H6B 110.2 . . ?
C1 C6 H6B 110.2 2_655 . ?
H6A C6 H6B 108.5 . . ?
O4 C7 C7 108.20(8) . 2_655 ?
O4 C7 H7A 110.1 . . ?
C7 C7 H7A 110.1 2_655 . ?
O4 C7 H7B 110.1 . . ?
C7 C7 H7B 110.1 2_655 . ?
H7A C7 H7B 108.4 . . ?
O4 C8 H8A 109.5 . . ?
O4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C18 118.51(9) . . ?
C10 C9 C17 122.03(9) . 5_666 ?
C18 C9 C17 119.42(9) . 5_666 ?
C11 C10 C9 121.24(10) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C12 C11 C10 121.07(10) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C11 C12 C13 120.57(10) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C14 C13 C12 121.59(10) . . ?
C14 C13 C18 119.32(9) . . ?
C12 C13 C18 119.08(9) . . ?
C15 C14 C13 120.30(10) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.8 . . ?
C14 C15 C16 121.04(10) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C15 C16 C17 121.45(10) . . ?
C15 C16 H16 119.3 . . ?
C17 C16 H16 119.3 . . ?
C16 C17 C18 118.39(9) . . ?
C16 C17 C9 122.11(9) . 5_666 ?
C18 C17 C9 119.50(8) . 5_666 ?
C9 C18 C17 121.08(9) . . ?
C9 C18 C13 119.48(9) . . ?
C17 C18 C13 119.43(9) . . ?

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
C2 O1 C1 C6 -178.94(8) . . . 2_655 ?
Na1 O1 C1 C6 63.49(8) . . . 2_655 ?
C1 O1 C2 C3 -175.02(8) . . . . ?
Na1 O1 C2 C3 -61.06(9) . . . . ?
C4 O2 C3 C2 99.23(10) . . . . ?
Na1 O2 C3 C2 -20.92(10) . . . . ?
O1 C2 C3 O2 55.05(11) . . . . ?
C3 O2 C4 C5 -70.40(11) . . . . ?
Na1 O2 C4 C5 56.17(8) . . . . ?
C6 O3 C5 C4 -164.50(8) . . . . ?
Na1 O3 C5 C4 12.07(11) . . . . ?
O2 C4 C5 O3 -48.77(11) . . . . ?
C5 O3 C6 C1 -169.56(8) . . . 2_655 ?
Na1 O3 C6 C1 13.83(11) . . . 2_655 ?
C8 O4 C7 C7 -175.89(10) . . . 2_655 ?
Na1 O4 C7 C7 -46.54(12) . . . 2_655 ?
C18 C9 C10 C11 0.73(15) . . . . ?
C17 C9 C10 C11 -176.97(9) 5_666 . . . ?
C9 C10 C11 C12 -1.91(16) . . . . ?
C10 C11 C12 C13 0.94(16) . . . . ?
C11 C12 C13 C14 -179.41(10) . . . . ?
C11 C12 C13 C18 1.14(15) . . . . ?
C12 C13 C14 C15 -176.56(10) . . . . ?
C18 C13 C14 C15 2.88(15) . . . . ?
C13 C14 C15 C16 -0.75(17) . . . . ?
C14 C15 C16 C17 -1.06(17) . . . . ?
C15 C16 C17 C18 0.65(15) . . . . ?
C15 C16 C17 C9 -178.73(10) . . . 5_666 ?
C10 C9 C18 C17 -177.12(9) . . . . ?
C17 C9 C18 C17 0.64(15) 5_666 . . . ?
C10 C9 C18 C13 1.34(13) . . . . ?
C17 C9 C18 C13 179.10(8) 5_666 . . . ?
C16 C17 C18 C9 179.96(9) . . . . ?
C9 C17 C18 C9 -0.64(15) 5_666 . . . ?
C16 C17 C18 C13 1.49(14) . . . . ?
C9 C17 C18 C13 -179.10(8) 5_666 . . . ?
C14 C13 C18 C9 178.27(9) . . . . ?
C12 C13 C18 C9 -2.27(14) . . . . ?
C14 C13 C18 C17 -3.24(14) . . . . ?
C12 C13 C18 C17 176.22(9) . . . . ?

_refine_diff_density_max         0.380
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.039

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_1005SF_0mS_a
_database_code_depnum_ccdc_archive 'CCDC 1431117'
_audit_update_record             
;
2015-10-13 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H38 O8 K, C12 H10'
_chemical_formula_sum            'C32 H48 K O8'
_chemical_formula_weight         599.80

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   12.8923(12)
_cell_length_b                   18.0166(17)
_cell_length_c                   15.2947(14)
_cell_angle_alpha                90
_cell_angle_beta                 114.036(2)
_cell_angle_gamma                90
_cell_volume                     3244.5(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2856
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      21.56

_exptl_crystal_description       rod
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_F_000             1292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    0.211
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6451
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus tube'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35433
_diffrn_reflns_av_unetI/netI     0.0947
_diffrn_reflns_av_R_equivalents  0.1015
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.750
_diffrn_reflns_theta_max         27.565
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7460
_reflns_number_gt                4130
_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-2014/6 (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)+(0.0707P)²+1.5629P] 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_number_reflns         7460
_refine_ls_number_parameters     380
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1340
_refine_ls_R_factor_gt           0.0607
_refine_ls_wR_factor_ref         0.1708
_refine_ls_wR_factor_gt          0.1330
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.001
_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
K1 K 0.84583(5) 0.76749(4) 0.52295(5) 0.02118(17) Uani 1 1 d . . . . .
O1 O 0.99406(17) 0.66566(12) 0.65291(15) 0.0237(5) Uani 1 1 d . . . . .
O2 O 0.75899(17) 0.63347(12) 0.56891(15) 0.0248(5) Uani 1 1 d . . . . .
O3 O 0.61633(17) 0.75058(12) 0.47720(14) 0.0240(5) Uani 1 1 d . . . . .
O4 O 0.69371(17) 0.87134(12) 0.39762(14) 0.0237(5) Uani 1 1 d . . . . .
O5 O 0.93360(16) 0.89964(11) 0.47766(14) 0.0222(5) Uani 1 1 d . . . . .
O6 O 1.07686(17) 0.77885(12) 0.56904(14) 0.0241(5) Uani 1 1 d . . . . .
O7 O 0.85197(19) 0.68555(12) 0.37754(16) 0.0321(6) Uani 1 1 d . . . . .
O8 O 0.850(3) 0.8453(15) 0.674(3) 0.040(5) Uani 0.53(10) 1 d D U P A 1
O9 O 0.822(3) 0.8598(17) 0.6522(16) 0.033(4) Uani 0.47(10) 1 d D U P A 2
C1 C 0.9487(3) 0.59393(18) 0.6521(2) 0.0267(7) Uani 1 1 d . . . . .
H1A H 1.0006 0.5653 0.7080 0.032 Uiso 1 1 calc R U . . .
H1B H 0.9414 0.5673 0.5932 0.032 Uiso 1 1 calc R U . . .
C2 C 0.8346(3) 0.60002(19) 0.6555(2) 0.0275(8) Uani 1 1 d . . . . .
H2A H 0.8066 0.5501 0.6624 0.033 Uiso 1 1 calc R U . . .
H2B H 0.8400 0.6307 0.7109 0.033 Uiso 1 1 calc R U . . .
C3 C 0.6450(3) 0.63686(18) 0.5614(2) 0.0277(8) Uani 1 1 d . . . . .
H3A H 0.6430 0.6631 0.6176 0.033 Uiso 1 1 calc R U . . .
H3B H 0.6152 0.5860 0.5599 0.033 Uiso 1 1 calc R U . . .
C4 C 0.5735(3) 0.67706(18) 0.4720(2) 0.0286(8) Uani 1 1 d . . . . .
H4A H 0.5757 0.6510 0.4158 0.034 Uiso 1 1 calc R U . . .
H4B H 0.4937 0.6786 0.4649 0.034 Uiso 1 1 calc R U . . .
C5 C 0.5430(3) 0.79735(18) 0.4022(2) 0.0265(7) Uani 1 1 d . . . . .
H5A H 0.4670 0.7994 0.4036 0.032 Uiso 1 1 calc R U . . .
H5B H 0.5343 0.7774 0.3393 0.032 Uiso 1 1 calc R U . . .
C6 C 0.5939(3) 0.87370(18) 0.4162(2) 0.0263(7) Uani 1 1 d . . . . .
H6A H 0.5385 0.9091 0.3720 0.032 Uiso 1 1 calc R U . . .
H6B H 0.6134 0.8905 0.4826 0.032 Uiso 1 1 calc R U . . .
C7 C 0.7432(3) 0.94287(17) 0.4031(2) 0.0255(7) Uani 1 1 d . . . . .
H7A H 0.7571 0.9663 0.4655 0.031 Uiso 1 1 calc R U . . .
H7B H 0.6912 0.9752 0.3515 0.031 Uiso 1 1 calc R U . . .
C8 C 0.8533(3) 0.93362(18) 0.3926(2) 0.0262(7) Uani 1 1 d . . . . .
H8A H 0.8418 0.9021 0.3364 0.031 Uiso 1 1 calc R U . . .
H8B H 0.8819 0.9826 0.3830 0.031 Uiso 1 1 calc R U . . .
C9 C 1.0405(3) 0.88697(19) 0.4718(2) 0.0264(8) Uani 1 1 d . . . . .
C10 C 1.1185(3) 0.85154(18) 0.5644(2) 0.0254(7) Uani 1 1 d . . . . .
H10A H 1.1965 0.8485 0.5673 0.030 Uiso 1 1 calc R U . . .
H10B H 1.1207 0.8817 0.6193 0.030 Uiso 1 1 calc R U . . .
C11 C 1.1480(3) 0.73935(18) 0.6535(2) 0.0274(7) Uani 1 1 d . . . . .
H11A H 1.1490 0.7651 0.7110 0.033 Uiso 1 1 calc R U . . .
H11B H 1.2267 0.7375 0.6579 0.033 Uiso 1 1 calc R U . . .
C12 C 1.1033(3) 0.66297(18) 0.6492(2) 0.0270(7) Uani 1 1 d . . . . .
H12A H 1.0967 0.6386 0.5891 0.032 Uiso 1 1 calc R U . . .
H12B H 1.1564 0.6335 0.7036 0.032 Uiso 1 1 calc R U . . .
C13 C 0.7622(3) 0.8325(2) 0.7078(3) 0.0393(9) Uani 1 1 d D . . . .
H13A H 0.7899 0.7977 0.7627 0.047 Uiso 1 1 calc R U . A 1
H13B H 0.6946 0.8103 0.6563 0.047 Uiso 1 1 calc R U . A 1
C14 C 0.7312(3) 0.9059(2) 0.7384(3) 0.0368(9) Uani 1 1 d . . . . .
H14A H 0.7079 0.8996 0.7921 0.044 Uiso 1 1 calc R U . . .
H14B H 0.6694 0.9308 0.6846 0.044 Uiso 1 1 calc R U . . .
C15 C 0.8423(3) 0.94925(19) 0.7696(2) 0.0315(8) Uani 1 1 d . . . . .
H15A H 0.8279 1.0031 0.7584 0.038 Uiso 1 1 calc R U . . .
H15B H 0.8909 0.9408 0.8382 0.038 Uiso 1 1 calc R U . . .
C16 C 0.8965(3) 0.9175(2) 0.7061(2) 0.0345(9) Uani 1 1 d D . . . .
H16A H 0.8813 0.9505 0.6505 0.041 Uiso 1 1 calc R U . A 1
H16B H 0.9798 0.9139 0.7426 0.041 Uiso 1 1 calc R U . A 1
C17 C 0.7952(3) 0.61565(17) 0.3600(2) 0.0261(7) Uani 1 1 d . . . . .
H17A H 0.7285 0.6161 0.2977 0.031 Uiso 1 1 calc R U . . .
H17B H 0.7693 0.6039 0.4111 0.031 Uiso 1 1 calc R U . . .
C18 C 0.8814(4) 0.5598(2) 0.3592(3) 0.0505(11) Uani 1 1 d . . . . .
H18A H 0.9273 0.5413 0.4245 0.061 Uiso 1 1 calc R U . . .
H18B H 0.8440 0.5172 0.3173 0.061 Uiso 1 1 calc R U . . .
C19 C 0.9528(3) 0.6018(2) 0.3210(3) 0.0460(10) Uani 1 1 d . . . . .
H19A H 0.9242 0.5958 0.2508 0.055 Uiso 1 1 calc R U . . .
H19B H 1.0326 0.5846 0.3509 0.055 Uiso 1 1 calc R U . . .
C20 C 0.9435(3) 0.68173(19) 0.3470(2) 0.0324(8) Uani 1 1 d . . . . .
H20A H 1.0154 0.6981 0.3991 0.039 Uiso 1 1 calc R U . . .
H20B H 0.9276 0.7142 0.2908 0.039 Uiso 1 1 calc R U . . .
C21 C 0.3435(3) 0.76583(18) 0.5181(2) 0.0238(7) Uani 1 1 d . . . . .
C22 C 0.2619(3) 0.78494(19) 0.4234(2) 0.0283(8) Uani 1 1 d . . . . .
H22 H 0.2117 0.7477 0.3851 0.034 Uiso 1 1 calc R U . . .
C23 C 0.2547(3) 0.8556(2) 0.3868(2) 0.0311(8) Uani 1 1 d . . . . .
H23 H 0.2005 0.8654 0.3237 0.037 Uiso 1 1 calc R U . . .
C24 C 0.3250(3) 0.9131(2) 0.4398(2) 0.0328(8) Uani 1 1 d . . . . .
H24 H 0.3187 0.9618 0.4142 0.039 Uiso 1 1 calc R U . . .
C25 C 0.4051(3) 0.8963(2) 0.5322(2) 0.0315(8) Uani 1 1 d . . . . .
H25 H 0.4539 0.9344 0.5697 0.038 Uiso 1 1 calc R U . . .
C26 C 0.4149(3) 0.82614(18) 0.5699(2) 0.0266(7) Uani 1 1 d . . . . .
H26 H 0.4710 0.8172 0.6325 0.032 Uiso 1 1 calc R U . . .
C27 C 0.3522(2) 0.69261(18) 0.5569(2) 0.0225(7) Uani 1 1 d . . . . .
C28 C 0.2786(3) 0.63308(19) 0.5052(2) 0.0295(8) Uani 1 1 d . . . . .
H28 H 0.2211 0.6428 0.4434 0.035 Uiso 1 1 calc R U . . .
C29 C 0.2883(3) 0.5624(2) 0.5422(3) 0.0346(8) Uani 1 1 d . . . . .
H29 H 0.2380 0.5249 0.5048 0.042 Uiso 1 1 calc R U . . .
C30 C 0.3694(3) 0.5443(2) 0.6325(3) 0.0341(8) Uani 1 1 d . . . . .
H30 H 0.3752 0.4954 0.6573 0.041 Uiso 1 1 calc R U . . .
C31 C 0.4428(3) 0.60138(19) 0.6857(2) 0.0296(8) Uani 1 1 d . . . . .
H31 H 0.4988 0.5908 0.7479 0.035 Uiso 1 1 calc R U . . .
C32 C 0.4352(3) 0.67166(18) 0.6499(2) 0.0241(7) Uani 1 1 d . . . . .
H32 H 0.4870 0.7082 0.6880 0.029 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
K1 O8 2.681(17) . ?
K1 O9 2.697(19) . ?
K1 O7 2.697(2) . ?
K1 O3 2.766(2) . ?
K1 O6 2.775(2) . ?
K1 O1 2.806(2) . ?
K1 O4 2.821(2) . ?
K1 O5 2.840(2) . ?
K1 O2 2.867(2) . ?
O1 C1 1.416(4) . ?
O1 C12 1.434(3) . ?
O2 C2 1.420(4) . ?
O2 C3 1.428(3) . ?
O3 C4 1.425(4) . ?
O3 C5 1.427(4) . ?
O4 C7 1.425(4) . ?
O4 C6 1.427(3) . ?
O5 C8 1.429(4) . ?
O5 C9 1.436(3) . ?
O6 C10 1.428(4) . ?
O6 C11 1.432(4) . ?
O7 C17 1.426(4) . ?
O7 C20 1.437(4) . ?
O8 C16 1.433(11) . ?
O8 C13 1.445(10) . ?
O9 C16 1.431(11) . ?
O9 C13 1.442(11) . ?
C1 C2 1.496(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.488(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.501(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.502(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.504(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.483(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.510(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.527(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.521(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.502(5) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.482(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.512(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C27 1.432(4) . ?
C21 C26 1.436(4) . ?
C21 C22 1.443(4) . ?
C22 C23 1.378(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.398(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.403(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.373(5) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.437(4) . ?
C27 C32 1.439(4) . ?
C28 C29 1.378(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.389(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.411(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.367(4) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?

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
O8 K1 O7 176.9(11) . . ?
O9 K1 O7 173.2(9) . . ?
O8 K1 O3 85.4(7) . . ?
O9 K1 O3 79.7(5) . . ?
O7 K1 O3 96.82(7) . . ?
O8 K1 O6 95.7(7) . . ?
O9 K1 O6 101.6(5) . . ?
O7 K1 O6 82.01(7) . . ?
O3 K1 O6 177.91(7) . . ?
O8 K1 O1 87.9(11) . . ?
O9 K1 O1 97.6(8) . . ?
O7 K1 O1 89.20(7) . . ?
O3 K1 O1 117.18(6) . . ?
O6 K1 O1 61.15(6) . . ?
O8 K1 O4 90.1(11) . . ?
O9 K1 O4 80.4(8) . . ?
O7 K1 O4 92.78(7) . . ?
O3 K1 O4 61.65(6) . . ?
O6 K1 O4 120.06(6) . . ?
O1 K1 O4 177.81(6) . . ?
O8 K1 O5 84.3(5) . . ?
O9 K1 O5 80.7(4) . . ?
O7 K1 O5 96.28(7) . . ?
O3 K1 O5 121.47(6) . . ?
O6 K1 O5 60.47(6) . . ?
O1 K1 O5 119.79(6) . . ?
O4 K1 O5 60.93(6) . . ?
O8 K1 O2 95.9(5) . . ?
O9 K1 O2 99.5(4) . . ?
O7 K1 O2 83.50(7) . . ?
O3 K1 O2 59.00(6) . . ?
O6 K1 O2 119.07(6) . . ?
O1 K1 O2 59.80(6) . . ?
O4 K1 O2 119.49(6) . . ?
O5 K1 O2 179.52(6) . . ?
C1 O1 C12 112.2(2) . . ?
C1 O1 K1 115.50(17) . . ?
C12 O1 K1 112.98(17) . . ?
C2 O2 C3 112.8(2) . . ?
C2 O2 K1 113.43(17) . . ?
C3 O2 K1 115.85(17) . . ?
C4 O3 C5 112.9(2) . . ?
C4 O3 K1 117.82(17) . . ?
C5 O3 K1 115.37(16) . . ?
C7 O4 C6 112.3(2) . . ?
C7 O4 K1 112.89(16) . . ?
C6 O4 K1 108.55(16) . . ?
C8 O5 C9 111.7(2) . . ?
C8 O5 K1 111.62(16) . . ?
C9 O5 K1 111.71(17) . . ?
C10 O6 C11 112.7(2) . . ?
C10 O6 K1 116.19(16) . . ?
C11 O6 K1 114.77(16) . . ?
C17 O7 C20 108.8(2) . . ?
C17 O7 K1 116.96(17) . . ?
C20 O7 K1 126.75(19) . . ?
C16 O8 C13 107.4(8) . . ?
C16 O8 K1 129.1(11) . . ?
C13 O8 K1 118.9(10) . . ?
C16 O9 C13 107.7(8) . . ?
C16 O9 K1 128.1(12) . . ?
C13 O9 K1 118.1(10) . . ?
O1 C1 C2 109.9(3) . . ?
O1 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
O1 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
O2 C2 C1 108.1(2) . . ?
O2 C2 H2A 110.1 . . ?
C1 C2 H2A 110.1 . . ?
O2 C2 H2B 110.1 . . ?
C1 C2 H2B 110.1 . . ?
H2A C2 H2B 108.4 . . ?
O2 C3 C4 109.1(2) . . ?
O2 C3 H3A 109.9 . . ?
C4 C3 H3A 109.9 . . ?
O2 C3 H3B 109.9 . . ?
C4 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?
O3 C4 C3 108.7(3) . . ?
O3 C4 H4A 110.0 . . ?
C3 C4 H4A 110.0 . . ?
O3 C4 H4B 110.0 . . ?
C3 C4 H4B 110.0 . . ?
H4A C4 H4B 108.3 . . ?
O3 C5 C6 108.5(3) . . ?
O3 C5 H5A 110.0 . . ?
C6 C5 H5A 110.0 . . ?
O3 C5 H5B 110.0 . . ?
C6 C5 H5B 110.0 . . ?
H5A C5 H5B 108.4 . . ?
O4 C6 C5 108.8(2) . . ?
O4 C6 H6A 109.9 . . ?
C5 C6 H6A 109.9 . . ?
O4 C6 H6B 109.9 . . ?
C5 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
O4 C7 C8 108.3(2) . . ?
O4 C7 H7A 110.0 . . ?
C8 C7 H7A 110.0 . . ?
O4 C7 H7B 110.0 . . ?
C8 C7 H7B 110.0 . . ?
H7A C7 H7B 108.4 . . ?
O5 C8 C7 108.4(2) . . ?
O5 C8 H8A 110.0 . . ?
C7 C8 H8A 110.0 . . ?
O5 C8 H8B 110.0 . . ?
C7 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
O5 C9 C10 107.4(2) . . ?
O6 C10 C9 108.4(2) . . ?
O6 C10 H10A 110.0 . . ?
C9 C10 H10A 110.0 . . ?
O6 C10 H10B 110.0 . . ?
C9 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
O6 C11 C12 109.1(3) . . ?
O6 C11 H11A 109.9 . . ?
C12 C11 H11A 109.9 . . ?
O6 C11 H11B 109.9 . . ?
C12 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
O1 C12 C11 109.7(2) . . ?
O1 C12 H12A 109.7 . . ?
C11 C12 H12A 109.7 . . ?
O1 C12 H12B 109.7 . . ?
C11 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
O9 C13 C14 98.9(13) . . ?
O8 C13 C14 108.5(9) . . ?
O8 C13 H13A 110.0 . . ?
C14 C13 H13A 110.0 . . ?
O8 C13 H13B 110.0 . . ?
C14 C13 H13B 110.0 . . ?
H13A C13 H13B 108.4 . . ?
C13 C14 C15 102.2(3) . . ?
C13 C14 H14A 111.3 . . ?
C15 C14 H14A 111.3 . . ?
C13 C14 H14B 111.3 . . ?
C15 C14 H14B 111.3 . . ?
H14A C14 H14B 109.2 . . ?
C16 C15 C14 103.0(3) . . ?
C16 C15 H15A 111.2 . . ?
C14 C15 H15A 111.2 . . ?
C16 C15 H15B 111.2 . . ?
C14 C15 H15B 111.2 . . ?
H15A C15 H15B 109.1 . . ?
O9 C16 C15 105.2(9) . . ?
O8 C16 C15 109.0(5) . . ?
O8 C16 H16A 109.9 . . ?
C15 C16 H16A 109.9 . . ?
O8 C16 H16B 109.9 . . ?
C15 C16 H16B 109.9 . . ?
H16A C16 H16B 108.3 . . ?
O7 C17 C18 105.6(3) . . ?
O7 C17 H17A 110.6 . . ?
C18 C17 H17A 110.6 . . ?
O7 C17 H17B 110.6 . . ?
C18 C17 H17B 110.6 . . ?
H17A C17 H17B 108.8 . . ?
C19 C18 C17 104.0(3) . . ?
C19 C18 H18A 111.0 . . ?
C17 C18 H18A 111.0 . . ?
C19 C18 H18B 111.0 . . ?
C17 C18 H18B 111.0 . . ?
H18A C18 H18B 109.0 . . ?
C18 C19 C20 104.7(3) . . ?
C18 C19 H19A 110.8 . . ?
C20 C19 H19A 110.8 . . ?
C18 C19 H19B 110.8 . . ?
C20 C19 H19B 110.8 . . ?
H19A C19 H19B 108.9 . . ?
O7 C20 C19 107.1(3) . . ?
O7 C20 H20A 110.3 . . ?
C19 C20 H20A 110.3 . . ?
O7 C20 H20B 110.3 . . ?
C19 C20 H20B 110.3 . . ?
H20A C20 H20B 108.5 . . ?
C27 C21 C26 123.0(3) . . ?
C27 C21 C22 122.5(3) . . ?
C26 C21 C22 114.5(3) . . ?
C23 C22 C21 121.9(3) . . ?
C23 C22 H22 119.0 . . ?
C21 C22 H22 119.0 . . ?
C22 C23 C24 121.9(3) . . ?
C22 C23 H23 119.0 . . ?
C24 C23 H23 119.0 . . ?
C23 C24 C25 117.5(3) . . ?
C23 C24 H24 121.2 . . ?
C25 C24 H24 121.2 . . ?
C26 C25 C24 121.7(3) . . ?
C26 C25 H25 119.1 . . ?
C24 C25 H25 119.1 . . ?
C25 C26 C21 122.4(3) . . ?
C25 C26 H26 118.8 . . ?
C21 C26 H26 118.8 . . ?
C21 C27 C28 122.5(3) . . ?
C21 C27 C32 123.5(3) . . ?
C28 C27 C32 114.0(3) . . ?
C29 C28 C27 122.3(3) . . ?
C29 C28 H28 118.8 . . ?
C27 C28 H28 118.8 . . ?
C28 C29 C30 122.1(3) . . ?
C28 C29 H29 119.0 . . ?
C30 C29 H29 119.0 . . ?
C29 C30 C31 117.3(3) . . ?
C29 C30 H30 121.3 . . ?
C31 C30 H30 121.3 . . ?
C32 C31 C30 121.5(3) . . ?
C32 C31 H31 119.3 . . ?
C30 C31 H31 119.3 . . ?
C31 C32 C27 122.8(3) . . ?
C31 C32 H32 118.6 . . ?
C27 C32 H32 118.6 . . ?

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
C12 O1 C1 C2 -179.7(2) . . . . ?
K1 O1 C1 C2 -48.2(3) . . . . ?
C3 O2 C2 C1 175.5(3) . . . . ?
K1 O2 C2 C1 -50.3(3) . . . . ?
O1 C1 C2 O2 66.2(3) . . . . ?
C2 O2 C3 C4 176.3(3) . . . . ?
K1 O2 C3 C4 43.2(3) . . . . ?
C5 O3 C4 C3 -170.4(2) . . . . ?
K1 O3 C4 C3 51.1(3) . . . . ?
O2 C3 C4 O3 -61.1(3) . . . . ?
C4 O3 C5 C6 178.1(2) . . . . ?
K1 O3 C5 C6 -42.3(3) . . . . ?
C7 O4 C6 C5 176.1(2) . . . . ?
K1 O4 C6 C5 -58.4(3) . . . . ?
O3 C5 C6 O4 69.4(3) . . . . ?
C6 O4 C7 C8 174.3(2) . . . . ?
K1 O4 C7 C8 51.2(3) . . . . ?
C9 O5 C8 C7 178.3(2) . . . . ?
K1 O5 C8 C7 52.5(3) . . . . ?
O4 C7 C8 O5 -71.1(3) . . . . ?
C8 O5 C9 C10 179.8(3) . . . . ?
K1 O5 C9 C10 -54.4(3) . . . . ?
C11 O6 C10 C9 177.9(2) . . . . ?
K1 O6 C10 C9 -46.7(3) . . . . ?
O5 C9 C10 O6 67.8(3) . . . . ?
C10 O6 C11 C12 -176.0(2) . . . . ?
K1 O6 C11 C12 48.0(3) . . . . ?
C1 O1 C12 C11 -178.1(3) . . . . ?
K1 O1 C12 C11 49.2(3) . . . . ?
O6 C11 C12 O1 -65.5(3) . . . . ?
C16 O9 C13 C14 45(3) . . . . ?
K1 O9 C13 C14 -159.8(16) . . . . ?
C16 O8 C13 C14 16(4) . . . . ?
K1 O8 C13 C14 -142.2(17) . . . . ?
O9 C13 C14 C15 -45.4(13) . . . . ?
O8 C13 C14 C15 -29(2) . . . . ?
C13 C14 C15 C16 30.2(3) . . . . ?
C13 O9 C16 C15 -27(3) . . . . ?
K1 O9 C16 C15 -178.2(18) . . . . ?
C13 O8 C16 C15 4(4) . . . . ?
K1 O8 C16 C15 160(2) . . . . ?
C14 C15 C16 O9 -3.3(17) . . . . ?
C14 C15 C16 O8 -22(2) . . . . ?
C20 O7 C17 C18 24.5(4) . . . . ?
K1 O7 C17 C18 -127.4(2) . . . . ?
O7 C17 C18 C19 -31.8(4) . . . . ?
C17 C18 C19 C20 26.5(4) . . . . ?
C17 O7 C20 C19 -7.7(4) . . . . ?
K1 O7 C20 C19 140.8(2) . . . . ?
C18 C19 C20 O7 -12.4(4) . . . . ?
C27 C21 C22 C23 -179.7(3) . . . . ?
C26 C21 C22 C23 0.2(4) . . . . ?
C21 C22 C23 C24 -0.9(5) . . . . ?
C22 C23 C24 C25 0.8(5) . . . . ?
C23 C24 C25 C26 0.0(5) . . . . ?
C24 C25 C26 C21 -0.7(5) . . . . ?
C27 C21 C26 C25 -179.5(3) . . . . ?
C22 C21 C26 C25 0.6(4) . . . . ?
C26 C21 C27 C28 178.5(3) . . . . ?
C22 C21 C27 C28 -1.5(4) . . . . ?
C26 C21 C27 C32 -2.0(4) . . . . ?
C22 C21 C27 C32 177.9(3) . . . . ?
C21 C27 C28 C29 179.0(3) . . . . ?
C32 C27 C28 C29 -0.5(4) . . . . ?
C27 C28 C29 C30 0.7(5) . . . . ?
C28 C29 C30 C31 -0.2(5) . . . . ?
C29 C30 C31 C32 -0.5(5) . . . . ?
C30 C31 C32 C27 0.7(5) . . . . ?
C21 C27 C32 C31 -179.7(3) . . . . ?
C28 C27 C32 C31 -0.2(4) . . . . ?

_refine_diff_density_max         0.763
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.071

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_1006SF_0mS_a
_database_code_depnum_ccdc_archive 'CCDC 1431118'
_audit_update_record             
;
2015-10-13 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H40 Li O8, C12 H10'
_chemical_formula_sum            'C32 H50 Li O8'
_chemical_formula_weight         569.66

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'
Li Li -0.0003 0.0001 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   12.1048(8)
_cell_length_b                   17.6109(12)
_cell_length_c                   15.2132(10)
_cell_angle_alpha                90
_cell_angle_beta                 103.6700(10)
_cell_angle_gamma                90
_cell_volume                     3151.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3743
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      28.04

_exptl_crystal_description       rod
_exptl_crystal_colour            purple-blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_F_000             1236
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.900
_exptl_crystal_size_mid          0.370
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.084
_shelx_estimated_absorpt_T_min   0.928
_shelx_estimated_absorpt_T_max   0.988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6861
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus tube'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32260
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.731
_diffrn_reflns_theta_max         27.591
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             7229
_reflns_number_gt                5349
_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-2014/6 (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)+(0.0426P)²+1.0932P] 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_number_reflns         7229
_refine_ls_number_parameters     374
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.1030
_refine_ls_wR_factor_gt          0.0901
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_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
Li1 Li 0.6871(2) 0.38727(14) 0.21582(17) 0.0292(6) Uani 1 1 d . . . . .
O1 O 0.80260(7) 0.32987(5) 0.12266(6) 0.0209(2) Uani 1 1 d . . . . .
O2 O 0.59741(7) 0.40640(5) 0.08206(6) 0.0199(2) Uani 1 1 d . . . . .
O3 O 0.52401(7) 0.43429(5) 0.23342(6) 0.0198(2) Uani 1 1 d . . . . .
O4 O 0.66298(7) 0.41776(5) 0.41334(6) 0.0206(2) Uani 1 1 d . . . . .
O5 O 0.85826(7) 0.32254(5) 0.45369(6) 0.0229(2) Uani 1 1 d . . . . .
O6 O 0.94848(8) 0.32139(5) 0.30028(6) 0.0217(2) Uani 1 1 d . . . . .
O7 O 0.63829(8) 0.28294(5) 0.23772(7) 0.0237(2) Uani 1 1 d D . . . .
O8 O 0.77495(8) 0.48221(5) 0.23718(6) 0.0271(2) Uani 1 1 d . . . . .
C1 C 0.75082(11) 0.35233(8) 0.03240(9) 0.0226(3) Uani 1 1 d . . . . .
H1A H 0.7726 0.3169 -0.0111 0.027 Uiso 1 1 calc R U . . .
H1B H 0.7762 0.4040 0.0207 0.027 Uiso 1 1 calc R U . . .
C2 C 0.62418(11) 0.35126(8) 0.02140(9) 0.0231(3) Uani 1 1 d . . . . .
H2A H 0.5852 0.3638 -0.0417 0.028 Uiso 1 1 calc R U . . .
H2B H 0.5991 0.3002 0.0358 0.028 Uiso 1 1 calc R U . . .
C3 C 0.47792(11) 0.41218(8) 0.07622(9) 0.0220(3) Uani 1 1 d . . . . .
H3A H 0.4461 0.3617 0.0849 0.026 Uiso 1 1 calc R U . . .
H3B H 0.4381 0.4319 0.0161 0.026 Uiso 1 1 calc R U . . .
C4 C 0.46291(11) 0.46563(8) 0.14929(9) 0.0198(3) Uani 1 1 d . . . . .
H4A H 0.4932 0.5164 0.1399 0.024 Uiso 1 1 calc R U . . .
H4B H 0.3813 0.4708 0.1488 0.024 Uiso 1 1 calc R U . . .
C5 C 0.50975(11) 0.47846(8) 0.30884(9) 0.0228(3) Uani 1 1 d . . . . .
H5A H 0.4292 0.4939 0.2993 0.027 Uiso 1 1 calc R U . . .
H5B H 0.5566 0.5250 0.3136 0.027 Uiso 1 1 calc R U . . .
C6 C 0.54415(11) 0.43393(8) 0.39461(9) 0.0233(3) Uani 1 1 d . . . . .
H6A H 0.5269 0.4634 0.4452 0.028 Uiso 1 1 calc R U . . .
H6B H 0.5006 0.3859 0.3887 0.028 Uiso 1 1 calc R U . . .
C7 C 0.69829(11) 0.37715(8) 0.49569(9) 0.0230(3) Uani 1 1 d . . . . .
H7A H 0.6627 0.3262 0.4894 0.028 Uiso 1 1 calc R U . . .
H7B H 0.6739 0.4045 0.5447 0.028 Uiso 1 1 calc R U . . .
C8 C 0.82524(11) 0.36936(8) 0.51894(9) 0.0234(3) Uani 1 1 d . . . . .
H8A H 0.8608 0.4200 0.5197 0.028 Uiso 1 1 calc R U . . .
H8B H 0.8512 0.3465 0.5798 0.028 Uiso 1 1 calc R U . . .
C9 C 0.97779(11) 0.32430(8) 0.46013(9) 0.0231(3) Uani 1 1 d . . . . .
H9A H 1.0188 0.3001 0.5173 0.028 Uiso 1 1 calc R U . . .
H9B H 1.0040 0.3775 0.4601 0.028 Uiso 1 1 calc R U . . .
C10 C 1.00214(11) 0.28252(8) 0.38115(9) 0.0227(3) Uani 1 1 d . . . . .
H10A H 1.0852 0.2801 0.3867 0.027 Uiso 1 1 calc R U . . .
H10B H 0.9727 0.2300 0.3796 0.027 Uiso 1 1 calc R U . . .
C11 C 0.97696(11) 0.28933(8) 0.22282(9) 0.0219(3) Uani 1 1 d . . . . .
H11A H 0.9487 0.2365 0.2142 0.026 Uiso 1 1 calc R U . . .
H11B H 1.0606 0.2884 0.2314 0.026 Uiso 1 1 calc R U . . .
C12 C 0.92441(11) 0.33581(8) 0.14122(9) 0.0238(3) Uani 1 1 d . . . . .
H12A H 0.9474 0.3896 0.1520 0.029 Uiso 1 1 calc R U . . .
H12B H 0.9515 0.3175 0.0884 0.029 Uiso 1 1 calc R U . . .
C13 C 0.71350(12) 0.21875(8) 0.25829(11) 0.0299(3) Uani 1 1 d . . . . .
H13A H 0.7646 0.2243 0.3192 0.036 Uiso 1 1 calc R U . . .
H13B H 0.7605 0.2143 0.2134 0.036 Uiso 1 1 calc R U . . .
C14 C 0.63885(13) 0.14959(8) 0.25482(12) 0.0340(4) Uani 1 1 d . . . . .
H14A H 0.6670 0.1168 0.3083 0.041 Uiso 1 1 calc R U . . .
H14B H 0.6368 0.1196 0.1994 0.041 Uiso 1 1 calc R U . . .
C15 C 0.52085(12) 0.18122(8) 0.25446(10) 0.0268(3) Uani 1 1 d D . . . .
H15A H 0.4678 0.1745 0.1946 0.032 Uiso 0.876(3) 1 calc R U P A 1
H15B H 0.4886 0.1562 0.3011 0.032 Uiso 0.876(3) 1 calc R U P A 1
H15C H 0.4601 0.1486 0.2186 0.032 Uiso 0.124(3) 1 calc R U P A 2
H15D H 0.5100 0.1859 0.3167 0.032 Uiso 0.124(3) 1 calc R U P A 2
C16 C 0.54364(14) 0.26346(9) 0.27563(13) 0.0262(4) Uani 0.876(3) 1 d D . P A 1
H16A H 0.4762 0.2945 0.2480 0.031 Uiso 0.876(3) 1 calc R U P A 1
H16B H 0.5630 0.2719 0.3418 0.031 Uiso 0.876(3) 1 calc R U P A 1
C36 C 0.5218(8) 0.2583(6) 0.2108(8) 0.0262(4) Uani 0.124(3) 1 d D . P A 2
H36A H 0.4966 0.2544 0.1442 0.031 Uiso 0.124(3) 1 calc R U P A 2
H36B H 0.4711 0.2941 0.2327 0.031 Uiso 0.124(3) 1 calc R U P A 2
C17 C 0.75894(12) 0.54532(8) 0.17548(10) 0.0254(3) Uani 1 1 d . . . . .
H17A H 0.6908 0.5749 0.1795 0.030 Uiso 1 1 calc R U . . .
H17B H 0.7495 0.5273 0.1125 0.030 Uiso 1 1 calc R U . . .
C18 C 0.86458(12) 0.59320(8) 0.20378(10) 0.0271(3) Uani 1 1 d . . . . .
H18A H 0.8492 0.6471 0.1866 0.033 Uiso 1 1 calc R U . . .
H18B H 0.9265 0.5741 0.1772 0.033 Uiso 1 1 calc R U . . .
C19 C 0.89300(15) 0.58308(9) 0.30553(11) 0.0389(4) Uani 1 1 d . . . . .
H19A H 0.9745 0.5931 0.3322 0.047 Uiso 1 1 calc R U . . .
H19B H 0.8464 0.6170 0.3341 0.047 Uiso 1 1 calc R U . . .
C20 C 0.86387(13) 0.50050(9) 0.31620(10) 0.0322(4) Uani 1 1 d . . . . .
H20A H 0.9313 0.4679 0.3192 0.039 Uiso 1 1 calc R U . . .
H20B H 0.8368 0.4931 0.3721 0.039 Uiso 1 1 calc R U . . .
C21 C 0.21869(10) 0.39691(8) 0.22830(9) 0.0190(3) Uani 1 1 d . . . . .
C22 C 0.21998(11) 0.35250(8) 0.14930(9) 0.0214(3) Uani 1 1 d . . . . .
H22 H 0.2485 0.3021 0.1569 0.026 Uiso 1 1 calc R U . . .
C23 C 0.18126(11) 0.38048(9) 0.06282(9) 0.0249(3) Uani 1 1 d . . . . .
H23 H 0.1834 0.3488 0.0127 0.030 Uiso 1 1 calc R U . . .
C24 C 0.13877(11) 0.45449(9) 0.04721(10) 0.0275(3) Uani 1 1 d . . . . .
H24 H 0.1120 0.4735 -0.0125 0.033 Uiso 1 1 calc R U . . .
C25 C 0.13710(11) 0.49944(8) 0.12262(10) 0.0260(3) Uani 1 1 d . . . . .
H25 H 0.1090 0.5499 0.1136 0.031 Uiso 1 1 calc R U . . .
C26 C 0.17494(11) 0.47267(8) 0.20938(10) 0.0229(3) Uani 1 1 d . . . . .
H26 H 0.1721 0.5053 0.2585 0.027 Uiso 1 1 calc R U . . .
C27 C 0.25534(10) 0.36774(8) 0.31844(9) 0.0203(3) Uani 1 1 d . . . . .
C28 C 0.25367(12) 0.41167(9) 0.39742(10) 0.0267(3) Uani 1 1 d . . . . .
H28 H 0.2273 0.4626 0.3902 0.032 Uiso 1 1 calc R U . . .
C29 C 0.28916(13) 0.38223(10) 0.48371(10) 0.0356(4) Uani 1 1 d . . . . .
H29 H 0.2871 0.4136 0.5341 0.043 Uiso 1 1 calc R U . . .
C30 C 0.32809(13) 0.30727(10) 0.49872(11) 0.0377(4) Uani 1 1 d . . . . .
H30 H 0.3526 0.2875 0.5583 0.045 Uiso 1 1 calc R U . . .
C31 C 0.32962(12) 0.26283(9) 0.42325(10) 0.0308(3) Uani 1 1 d . . . . .
H31 H 0.3552 0.2118 0.4317 0.037 Uiso 1 1 calc R U . . .
C32 C 0.29490(11) 0.29107(8) 0.33671(10) 0.0233(3) Uani 1 1 d . . . . .
H32 H 0.2972 0.2587 0.2872 0.028 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
Li1 O8 1.967(3) . ?
Li1 O7 1.982(3) . ?
Li1 O2 2.095(3) . ?
Li1 O3 2.214(3) . ?
Li1 O1 2.434(3) . ?
O1 C1 1.4242(16) . ?
O1 C12 1.4380(15) . ?
O2 C2 1.4287(16) . ?
O2 C3 1.4316(15) . ?
O3 C4 1.4291(15) . ?
O3 C5 1.4301(16) . ?
O4 C7 1.4178(16) . ?
O4 C6 1.4275(15) . ?
O5 C8 1.4186(16) . ?
O5 C9 1.4273(16) . ?
O6 C11 1.4206(16) . ?
O6 C10 1.4236(16) . ?
O7 C36 1.440(10) . ?
O7 C13 1.4389(16) . ?
O7 C16 1.4407(18) . ?
O8 C17 1.4380(16) . ?
O8 C20 1.4478(16) . ?
C1 C2 1.5023(19) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.5001(19) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.4948(19) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.4995(18) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.496(2) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.4975(19) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.510(2) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.532(2) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.495(2) . ?
C15 C36 1.512(10) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 H15C 0.9900 . ?
C15 H15D 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C17 C18 1.5071(18) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.515(2) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.514(2) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C27 1.4331(19) . ?
C21 C22 1.4371(19) . ?
C21 C26 1.4391(19) . ?
C22 C23 1.3791(19) . ?
C22 H22 0.9500 . ?
C23 C24 1.401(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.398(2) . ?
C24 H24 0.9500 . ?
C25 C26 1.374(2) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.433(2) . ?
C27 C32 1.4376(19) . ?
C28 C29 1.382(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.402(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.393(2) . ?
C30 H30 0.9500 . ?
C31 C32 1.377(2) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?

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
O8 Li1 O7 158.61(14) . . ?
O8 Li1 O2 99.18(11) . . ?
O7 Li1 O2 101.88(11) . . ?
O8 Li1 O3 97.18(11) . . ?
O7 Li1 O3 90.97(10) . . ?
O2 Li1 O3 77.61(9) . . ?
O8 Li1 O1 94.95(11) . . ?
O7 Li1 O1 87.01(10) . . ?
O2 Li1 O1 74.82(9) . . ?
O3 Li1 O1 151.29(12) . . ?
C1 O1 C12 111.49(10) . . ?
C1 O1 Li1 105.28(9) . . ?
C12 O1 Li1 124.00(10) . . ?
C2 O2 C3 112.85(10) . . ?
C2 O2 Li1 111.94(10) . . ?
C3 O2 Li1 110.83(10) . . ?
C4 O3 C5 111.92(10) . . ?
C4 O3 Li1 108.88(10) . . ?
C5 O3 Li1 125.49(10) . . ?
C7 O4 C6 110.86(10) . . ?
C8 O5 C9 112.83(10) . . ?
C11 O6 C10 112.04(10) . . ?
C36 O7 C13 110.6(4) . . ?
C13 O7 C16 104.36(11) . . ?
C36 O7 Li1 122.8(4) . . ?
C13 O7 Li1 124.52(11) . . ?
C16 O7 Li1 125.78(11) . . ?
C17 O8 C20 109.21(10) . . ?
C17 O8 Li1 124.40(10) . . ?
C20 O8 Li1 126.39(11) . . ?
O1 C1 C2 107.99(11) . . ?
O1 C1 H1A 110.1 . . ?
C2 C1 H1A 110.1 . . ?
O1 C1 H1B 110.1 . . ?
C2 C1 H1B 110.1 . . ?
H1A C1 H1B 108.4 . . ?
O2 C2 C1 107.51(11) . . ?
O2 C2 H2A 110.2 . . ?
C1 C2 H2A 110.2 . . ?
O2 C2 H2B 110.2 . . ?
C1 C2 H2B 110.2 . . ?
H2A C2 H2B 108.5 . . ?
O2 C3 C4 107.22(10) . . ?
O2 C3 H3A 110.3 . . ?
C4 C3 H3A 110.3 . . ?
O2 C3 H3B 110.3 . . ?
C4 C3 H3B 110.3 . . ?
H3A C3 H3B 108.5 . . ?
O3 C4 C3 107.08(10) . . ?
O3 C4 H4A 110.3 . . ?
C3 C4 H4A 110.3 . . ?
O3 C4 H4B 110.3 . . ?
C3 C4 H4B 110.3 . . ?
H4A C4 H4B 108.6 . . ?
O3 C5 C6 110.70(11) . . ?
O3 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
O3 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
O4 C6 C5 109.79(11) . . ?
O4 C6 H6A 109.7 . . ?
C5 C6 H6A 109.7 . . ?
O4 C6 H6B 109.7 . . ?
C5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
O4 C7 C8 109.44(11) . . ?
O4 C7 H7A 109.8 . . ?
C8 C7 H7A 109.8 . . ?
O4 C7 H7B 109.8 . . ?
C8 C7 H7B 109.8 . . ?
H7A C7 H7B 108.2 . . ?
O5 C8 C7 109.30(11) . . ?
O5 C8 H8A 109.8 . . ?
C7 C8 H8A 109.8 . . ?
O5 C8 H8B 109.8 . . ?
C7 C8 H8B 109.8 . . ?
H8A C8 H8B 108.3 . . ?
O5 C9 C10 108.85(11) . . ?
O5 C9 H9A 109.9 . . ?
C10 C9 H9A 109.9 . . ?
O5 C9 H9B 109.9 . . ?
C10 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
O6 C10 C9 108.74(11) . . ?
O6 C10 H10A 109.9 . . ?
C9 C10 H10A 109.9 . . ?
O6 C10 H10B 109.9 . . ?
C9 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
O6 C11 C12 109.36(11) . . ?
O6 C11 H11A 109.8 . . ?
C12 C11 H11A 109.8 . . ?
O6 C11 H11B 109.8 . . ?
C12 C11 H11B 109.8 . . ?
H11A C11 H11B 108.2 . . ?
O1 C12 C11 109.76(11) . . ?
O1 C12 H12A 109.7 . . ?
C11 C12 H12A 109.7 . . ?
O1 C12 H12B 109.7 . . ?
C11 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
O7 C13 C14 106.47(11) . . ?
O7 C13 H13A 110.4 . . ?
C14 C13 H13A 110.4 . . ?
O7 C13 H13B 110.4 . . ?
C14 C13 H13B 110.4 . . ?
H13A C13 H13B 108.6 . . ?
C13 C14 C15 104.86(12) . . ?
C13 C14 H14A 110.8 . . ?
C15 C14 H14A 110.8 . . ?
C13 C14 H14B 110.8 . . ?
C15 C14 H14B 110.8 . . ?
H14A C14 H14B 108.9 . . ?
C16 C15 C14 103.13(12) . . ?
C36 C15 C14 103.0(4) . . ?
C16 C15 H15A 111.1 . . ?
C14 C15 H15A 111.1 . . ?
C16 C15 H15B 111.1 . . ?
C14 C15 H15B 111.1 . . ?
H15A C15 H15B 109.1 . . ?
C36 C15 H15C 111.2 . . ?
C14 C15 H15C 111.2 . . ?
C36 C15 H15D 111.2 . . ?
C14 C15 H15D 111.2 . . ?
H15C C15 H15D 109.1 . . ?
O7 C16 C15 105.56(13) . . ?
O7 C16 H16A 110.6 . . ?
C15 C16 H16A 110.6 . . ?
O7 C16 H16B 110.6 . . ?
C15 C16 H16B 110.6 . . ?
H16A C16 H16B 108.8 . . ?
O7 C36 C15 104.7(6) . . ?
O7 C36 H36A 110.8 . . ?
C15 C36 H36A 110.8 . . ?
O7 C36 H36B 110.8 . . ?
C15 C36 H36B 110.8 . . ?
H36A C36 H36B 108.9 . . ?
O8 C17 C18 105.76(11) . . ?
O8 C17 H17A 110.6 . . ?
C18 C17 H17A 110.6 . . ?
O8 C17 H17B 110.6 . . ?
C18 C17 H17B 110.6 . . ?
H17A C17 H17B 108.7 . . ?
C17 C18 C19 101.45(12) . . ?
C17 C18 H18A 111.5 . . ?
C19 C18 H18A 111.5 . . ?
C17 C18 H18B 111.5 . . ?
C19 C18 H18B 111.5 . . ?
H18A C18 H18B 109.3 . . ?
C20 C19 C18 102.71(12) . . ?
C20 C19 H19A 111.2 . . ?
C18 C19 H19A 111.2 . . ?
C20 C19 H19B 111.2 . . ?
C18 C19 H19B 111.2 . . ?
H19A C19 H19B 109.1 . . ?
O8 C20 C19 105.73(12) . . ?
O8 C20 H20A 110.6 . . ?
C19 C20 H20A 110.6 . . ?
O8 C20 H20B 110.6 . . ?
C19 C20 H20B 110.6 . . ?
H20A C20 H20B 108.7 . . ?
C27 C21 C22 122.89(12) . . ?
C27 C21 C26 122.67(12) . . ?
C22 C21 C26 114.43(12) . . ?
C23 C22 C21 122.34(13) . . ?
C23 C22 H22 118.8 . . ?
C21 C22 H22 118.8 . . ?
C22 C23 C24 121.50(14) . . ?
C22 C23 H23 119.2 . . ?
C24 C23 H23 119.2 . . ?
C25 C24 C23 117.63(13) . . ?
C25 C24 H24 121.2 . . ?
C23 C24 H24 121.2 . . ?
C26 C25 C24 121.86(14) . . ?
C26 C25 H25 119.1 . . ?
C24 C25 H25 119.1 . . ?
C25 C26 C21 122.24(13) . . ?
C25 C26 H26 118.9 . . ?
C21 C26 H26 118.9 . . ?
C21 C27 C28 123.10(13) . . ?
C21 C27 C32 122.37(13) . . ?
C28 C27 C32 114.52(12) . . ?
C29 C28 C27 122.06(15) . . ?
C29 C28 H28 119.0 . . ?
C27 C28 H28 119.0 . . ?
C28 C29 C30 121.67(15) . . ?
C28 C29 H29 119.2 . . ?
C30 C29 H29 119.2 . . ?
C31 C30 C29 117.64(14) . . ?
C31 C30 H30 121.2 . . ?
C29 C30 H30 121.2 . . ?
C32 C31 C30 121.65(15) . . ?
C32 C31 H31 119.2 . . ?
C30 C31 H31 119.2 . . ?
C31 C32 C27 122.45(14) . . ?
C31 C32 H32 118.8 . . ?
C27 C32 H32 118.8 . . ?

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
C12 O1 C1 C2 -174.92(11) . . . . ?
Li1 O1 C1 C2 -37.99(13) . . . . ?
C3 O2 C2 C1 178.51(11) . . . . ?
Li1 O2 C2 C1 -55.64(14) . . . . ?
O1 C1 C2 O2 63.00(14) . . . . ?
C2 O2 C3 C4 174.35(11) . . . . ?
Li1 O2 C3 C4 47.89(14) . . . . ?
C5 O3 C4 C3 -176.37(10) . . . . ?
Li1 O3 C4 C3 40.59(13) . . . . ?
O2 C3 C4 O3 -58.91(13) . . . . ?
C4 O3 C5 C6 163.24(11) . . . . ?
Li1 O3 C5 C6 -61.09(16) . . . . ?
C7 O4 C6 C5 178.53(11) . . . . ?
O3 C5 C6 O4 64.78(14) . . . . ?
C6 O4 C7 C8 -173.21(11) . . . . ?
C9 O5 C8 C7 168.28(11) . . . . ?
O4 C7 C8 O5 -66.20(14) . . . . ?
C8 O5 C9 C10 -172.03(11) . . . . ?
C11 O6 C10 C9 174.22(10) . . . . ?
O5 C9 C10 O6 63.43(14) . . . . ?
C10 O6 C11 C12 -176.20(10) . . . . ?
C1 O1 C12 C11 -161.66(11) . . . . ?
Li1 O1 C12 C11 70.95(15) . . . . ?
O6 C11 C12 O1 -66.16(14) . . . . ?
C36 O7 C13 C14 -7.0(5) . . . . ?
C16 O7 C13 C14 33.54(16) . . . . ?
Li1 O7 C13 C14 -171.15(13) . . . . ?
O7 C13 C14 C15 -13.65(17) . . . . ?
C13 C14 C15 C16 -10.49(17) . . . . ?
C13 C14 C15 C36 27.9(5) . . . . ?
C13 O7 C16 C15 -40.87(16) . . . . ?
Li1 O7 C16 C15 164.23(12) . . . . ?
C14 C15 C16 O7 31.26(16) . . . . ?
C13 O7 C36 C15 25.0(8) . . . . ?
Li1 O7 C36 C15 -170.5(3) . . . . ?
C14 C15 C36 O7 -32.1(7) . . . . ?
C20 O8 C17 C18 17.82(16) . . . . ?
Li1 O8 C17 C18 -162.79(13) . . . . ?
O8 C17 C18 C19 -34.77(15) . . . . ?
C17 C18 C19 C20 37.96(16) . . . . ?
C17 O8 C20 C19 6.79(17) . . . . ?
Li1 O8 C20 C19 -172.59(14) . . . . ?
C18 C19 C20 O8 -28.30(17) . . . . ?
C27 C21 C22 C23 177.99(12) . . . . ?
C26 C21 C22 C23 -0.60(18) . . . . ?
C21 C22 C23 C24 0.3(2) . . . . ?
C22 C23 C24 C25 0.1(2) . . . . ?
C23 C24 C25 C26 -0.3(2) . . . . ?
C24 C25 C26 C21 0.0(2) . . . . ?
C27 C21 C26 C25 -178.19(12) . . . . ?
C22 C21 C26 C25 0.41(18) . . . . ?
C22 C21 C27 C28 -179.67(12) . . . . ?
C26 C21 C27 C28 -1.20(19) . . . . ?
C22 C21 C27 C32 -0.90(19) . . . . ?
C26 C21 C27 C32 177.57(12) . . . . ?
C21 C27 C28 C29 179.81(13) . . . . ?
C32 C27 C28 C29 0.95(19) . . . . ?
C27 C28 C29 C30 -0.5(2) . . . . ?
C28 C29 C30 C31 -0.2(2) . . . . ?
C29 C30 C31 C32 0.3(2) . . . . ?
C30 C31 C32 C27 0.2(2) . . . . ?
C21 C27 C32 C31 -179.67(12) . . . . ?
C28 C27 C32 C31 -0.80(18) . . . . ?

_refine_diff_density_max         0.258
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.040

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_1008SF_0mS_a
_database_code_depnum_ccdc_archive 'CCDC 1431119'
_audit_update_record             
;
2015-10-13 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H40 Na O8, C12 H10'
_chemical_formula_sum            'C32 H50 Na O8'
_chemical_formula_weight         585.71

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   12.7772(13)
_cell_length_b                   17.6539(18)
_cell_length_c                   15.1994(15)
_cell_angle_alpha                90
_cell_angle_beta                 112.120(2)
_cell_angle_gamma                90
_cell_volume                     3176.1(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2897
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      21.33

_exptl_crystal_description       rod
_exptl_crystal_colour            blue-purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_F_000             1268
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    0.098
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6531
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus tube'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24404
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.783
_diffrn_reflns_theta_max         23.691
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.835
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.835
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.835
_reflns_number_total             4798
_reflns_number_gt                3149
_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-2014/6 (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)+(0.0563P)²+0.0157P] 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_number_reflns         4798
_refine_ls_number_parameters     380
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0424
_refine_ls_wR_factor_ref         0.1110
_refine_ls_wR_factor_gt          0.0931
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.001
_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 0.84894(8) 0.23680(5) 0.52779(6) 0.0306(3) Uani 1 1 d . . . . .
O1 O 0.99410(13) 0.34011(9) 0.65855(11) 0.0271(4) Uani 1 1 d . . . . .
O2 O 1.07409(13) 0.22062(8) 0.57944(11) 0.0262(4) Uani 1 1 d . . . . .
O3 O 0.93413(13) 0.10470(8) 0.48098(10) 0.0246(4) Uani 1 1 d . . . . .
O4 O 0.70193(13) 0.13931(9) 0.40483(10) 0.0251(4) Uani 1 1 d . . . . .
O5 O 0.62459(12) 0.26172(9) 0.48112(10) 0.0247(4) Uani 1 1 d . . . . .
O6 O 0.76392(13) 0.37552(9) 0.57708(10) 0.0259(4) Uani 1 1 d . . . . .
O7 O 0.83346(14) 0.16368(9) 0.64967(11) 0.0343(5) Uani 1 1 d . . . . .
O8 O 0.86527(14) 0.30930(9) 0.40568(12) 0.0336(4) Uani 1 1 d . . . . .
C1 C 1.1033(2) 0.34107(14) 0.65325(17) 0.0295(6) Uani 1 1 d . . . . .
H1A H 1.1557 0.3720 0.7057 0.035 Uiso 1 1 calc R U . . .
H1B H 1.0985 0.3639 0.5923 0.035 Uiso 1 1 calc R U . . .
C2 C 1.1462(2) 0.26167(14) 0.66034(16) 0.0278(6) Uani 1 1 d . . . . .
H2A H 1.2245 0.2616 0.6622 0.033 Uiso 1 1 calc R U . . .
H2B H 1.1464 0.2377 0.7192 0.033 Uiso 1 1 calc R U . . .
C3 C 1.1176(2) 0.14727(13) 0.57345(17) 0.0278(6) Uani 1 1 d . . . . .
H3A H 1.1169 0.1152 0.6266 0.033 Uiso 1 1 calc R U . . .
H3B H 1.1965 0.1513 0.5772 0.033 Uiso 1 1 calc R U . . .
C4 C 1.04473(19) 0.11300(13) 0.48082(16) 0.0256(6) Uani 1 1 d . . . . .
H4A H 1.0429 0.1461 0.4277 0.031 Uiso 1 1 calc R U . . .
H4B H 1.0750 0.0630 0.4728 0.031 Uiso 1 1 calc R U . . .
C5 C 0.85719(19) 0.07341(13) 0.39444(16) 0.0259(6) Uani 1 1 d . . . . .
H5A H 0.8844 0.0234 0.3827 0.031 Uiso 1 1 calc R U . . .
H5B H 0.8502 0.1073 0.3406 0.031 Uiso 1 1 calc R U . . .
C6 C 0.7459(2) 0.06532(13) 0.40388(17) 0.0262(6) Uani 1 1 d . . . . .
H6A H 0.6934 0.0358 0.3499 0.031 Uiso 1 1 calc R U . . .
H6B H 0.7552 0.0383 0.4635 0.031 Uiso 1 1 calc R U . . .
C7 C 0.59786(19) 0.13719(14) 0.41956(17) 0.0266(6) Uani 1 1 d . . . . .
H7A H 0.6113 0.1185 0.4843 0.032 Uiso 1 1 calc R U . . .
H7B H 0.5441 0.1024 0.3732 0.032 Uiso 1 1 calc R U . . .
C8 C 0.5498(2) 0.21523(13) 0.40723(16) 0.0275(6) Uani 1 1 d . . . . .
H8A H 0.5421 0.2356 0.3444 0.033 Uiso 1 1 calc R U . . .
H8B H 0.4740 0.2144 0.4109 0.033 Uiso 1 1 calc R U . . .
C9 C 0.5799(2) 0.33579(13) 0.47971(17) 0.0284(6) Uani 1 1 d . . . . .
H9A H 0.5003 0.3326 0.4742 0.034 Uiso 1 1 calc R U . . .
H9B H 0.5823 0.3646 0.4246 0.034 Uiso 1 1 calc R U . . .
C10 C 0.6498(2) 0.37472(14) 0.57012(18) 0.0292(6) Uani 1 1 d . . . . .
H10A H 0.6225 0.4272 0.5702 0.035 Uiso 1 1 calc R U . . .
H10B H 0.6439 0.3475 0.6250 0.035 Uiso 1 1 calc R U . . .
C11 C 0.8379(2) 0.41077(14) 0.66166(17) 0.0310(6) Uani 1 1 d . . . . .
H11A H 0.8409 0.3810 0.7178 0.037 Uiso 1 1 calc R U . . .
H11B H 0.8105 0.4624 0.6672 0.037 Uiso 1 1 calc R U . . .
C12 C 0.9520(2) 0.41470(13) 0.65715(17) 0.0286(6) Uani 1 1 d . . . . .
H12A H 0.9475 0.4409 0.5982 0.034 Uiso 1 1 calc R U . . .
H12B H 1.0037 0.4438 0.7120 0.034 Uiso 1 1 calc R U . . .
C13 C 0.9021(2) 0.10075(14) 0.69776(17) 0.0325(7) Uani 1 1 d . . . . .
H13A H 0.9783 0.1184 0.7393 0.039 Uiso 1 1 calc R U . . .
H13B H 0.9101 0.0643 0.6512 0.039 Uiso 1 1 calc R U . . .
C14 C 0.8427(2) 0.06328(14) 0.75701(17) 0.0306(6) Uani 1 1 d . . . . .
H14A H 0.8270 0.0092 0.7398 0.037 Uiso 1 1 calc R U . . .
H14B H 0.8893 0.0670 0.8257 0.037 Uiso 1 1 calc R U . . .
C15 C 0.7329(2) 0.10800(13) 0.73228(18) 0.0313(6) Uani 1 1 d . . . . .
H15A H 0.6698 0.0829 0.6811 0.038 Uiso 1 1 calc R U . . .
H15B H 0.7124 0.1143 0.7885 0.038 Uiso 1 1 calc R U . . .
C16 C 0.7616(2) 0.18327(14) 0.69954(17) 0.0319(6) Uani 1 1 d . . . . .
H16A H 0.6925 0.2094 0.6570 0.038 Uiso 1 1 calc R U . . .
H16B H 0.8016 0.2165 0.7544 0.038 Uiso 1 1 calc R U . . .
C17 C 0.7965(2) 0.37538(13) 0.37076(16) 0.0258(6) Uani 1 1 d D U . . .
H17A H 0.7936 0.4062 0.4242 0.031 Uiso 0.725(13) 1 calc R U P A 1
H17B H 0.7186 0.3606 0.3299 0.031 Uiso 0.725(13) 1 calc R U P A 1
H17C H 0.7606 0.3915 0.4152 0.031 Uiso 0.275(13) 1 calc R U P A 2
H17D H 0.7368 0.3656 0.3077 0.031 Uiso 0.275(13) 1 calc R U P A 2
C18 C 0.8514(4) 0.4201(3) 0.3139(5) 0.0328(14) Uani 0.725(13) 1 d D U P A 1
H18A H 0.8109 0.4117 0.2449 0.039 Uiso 0.725(13) 1 calc R U P A 1
H18B H 0.8513 0.4749 0.3273 0.039 Uiso 0.725(13) 1 calc R U P A 1
C38 C 0.8788(10) 0.4349(6) 0.3642(12) 0.024(3) Uani 0.275(13) 1 d D U P A 2
H38A H 0.8410 0.4706 0.3115 0.028 Uiso 0.275(13) 1 calc R U P A 2
H38B H 0.9113 0.4638 0.4242 0.028 Uiso 0.275(13) 1 calc R U P A 2
C19 C 0.9683(2) 0.39063(14) 0.3458(2) 0.0425(7) Uani 1 1 d D U . . .
H19A H 1.0191 0.4181 0.4026 0.051 Uiso 0.725(13) 1 calc R U P A 1
H19B H 0.9985 0.3944 0.2948 0.051 Uiso 0.725(13) 1 calc R U P A 1
H19C H 1.0442 0.4092 0.3865 0.051 Uiso 0.275(13) 1 calc R U P A 2
H19D H 0.9595 0.3957 0.2785 0.051 Uiso 0.275(13) 1 calc R U P A 2
C20 C 0.9537(2) 0.30901(13) 0.36876(18) 0.0323(6) Uani 1 1 d . . . . .
H20A H 0.9322 0.2773 0.3109 0.039 Uiso 1 1 calc R U . . .
H20B H 1.0247 0.2890 0.4166 0.039 Uiso 1 1 calc R U . . .
C21 C 0.34768(19) 0.23326(13) 0.52461(16) 0.0232(6) Uani 1 1 d . . . . .
C22 C 0.4162(2) 0.17100(14) 0.57493(17) 0.0270(6) Uani 1 1 d . . . . .
H22 H 0.4696 0.1792 0.6375 0.032 Uiso 1 1 calc R U . . .
C23 C 0.4075(2) 0.09971(14) 0.53583(18) 0.0327(7) Uani 1 1 d . . . . .
H23 H 0.4548 0.0603 0.5720 0.039 Uiso 1 1 calc R U . . .
C24 C 0.3304(2) 0.08421(14) 0.44379(18) 0.0337(7) Uani 1 1 d . . . . .
H24 H 0.3248 0.0351 0.4168 0.040 Uiso 1 1 calc R U . . .
C25 C 0.2621(2) 0.14361(15) 0.39332(18) 0.0310(6) Uani 1 1 d . . . . .
H25 H 0.2092 0.1345 0.3308 0.037 Uiso 1 1 calc R U . . .
C26 C 0.2690(2) 0.21479(14) 0.43114(16) 0.0263(6) Uani 1 1 d . . . . .
H26 H 0.2201 0.2532 0.3942 0.032 Uiso 1 1 calc R U . . .
C27 C 0.35723(19) 0.30784(13) 0.56412(16) 0.0230(6) Uani 1 1 d . . . . .
C28 C 0.2882(2) 0.36971(14) 0.51439(16) 0.0269(6) Uani 1 1 d . . . . .
H28 H 0.2327 0.3608 0.4529 0.032 Uiso 1 1 calc R U . . .
C29 C 0.2985(2) 0.44134(14) 0.55134(17) 0.0302(6) Uani 1 1 d . . . . .
H29 H 0.2507 0.4804 0.5147 0.036 Uiso 1 1 calc R U . . .
C30 C 0.3779(2) 0.45836(14) 0.64209(17) 0.0307(6) Uani 1 1 d . . . . .
H30 H 0.3842 0.5079 0.6679 0.037 Uiso 1 1 calc R U . . .
C31 C 0.4470(2) 0.39962(14) 0.69271(17) 0.0283(6) Uani 1 1 d . . . . .
H31 H 0.5019 0.4097 0.7541 0.034 Uiso 1 1 calc R U . . .
C32 C 0.43820(19) 0.32754(14) 0.65657(16) 0.0254(6) Uani 1 1 d . . . . .
H32 H 0.4873 0.2893 0.6939 0.030 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 O8 2.3277(18) . ?
Na1 O7 2.3266(18) . ?
Na1 O2 2.6969(18) . ?
Na1 O4 2.7092(18) . ?
Na1 O5 2.7171(18) . ?
Na1 O3 2.7772(18) . ?
Na1 O1 2.8178(18) . ?
Na1 O6 2.8900(18) . ?
O1 C12 1.420(3) . ?
O1 C1 1.428(3) . ?
O2 C3 1.426(3) . ?
O2 C2 1.426(3) . ?
O3 C4 1.422(3) . ?
O3 C5 1.424(3) . ?
O4 C6 1.424(3) . ?
O4 C7 1.430(3) . ?
O5 C9 1.424(3) . ?
O5 C8 1.428(3) . ?
O6 C11 1.420(3) . ?
O6 C10 1.422(3) . ?
O7 C13 1.433(3) . ?
O7 C16 1.436(3) . ?
O8 C17 1.436(3) . ?
O8 C20 1.438(3) . ?
C1 C2 1.494(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.493(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.489(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.492(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.495(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.487(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.529(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.529(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.512(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C38 1.516(10) . ?
C17 C18 1.522(5) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 H17C 0.9900 . ?
C17 H17D 0.9900 . ?
C18 C19 1.480(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C38 C19 1.496(9) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C19 C20 1.511(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 H19C 0.9900 . ?
C19 H19D 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C27 1.433(3) . ?
C21 C22 1.434(3) . ?
C21 C26 1.435(3) . ?
C22 C23 1.378(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.402(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.395(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.371(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.428(3) . ?
C27 C32 1.439(3) . ?
C28 C29 1.370(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.403(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.391(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.374(3) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?

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
O8 Na1 O7 179.59(8) . . ?
O8 Na1 O2 83.35(6) . . ?
O7 Na1 O2 96.35(6) . . ?
O8 Na1 O4 92.65(6) . . ?
O7 Na1 O4 87.25(6) . . ?
O2 Na1 O4 121.33(6) . . ?
O8 Na1 O5 96.04(6) . . ?
O7 Na1 O5 84.27(6) . . ?
O2 Na1 O5 176.42(6) . . ?
O4 Na1 O5 62.19(5) . . ?
O8 Na1 O3 95.51(6) . . ?
O7 Na1 O3 84.09(6) . . ?
O2 Na1 O3 60.50(5) . . ?
O4 Na1 O3 61.75(5) . . ?
O5 Na1 O3 123.08(6) . . ?
O8 Na1 O1 88.49(6) . . ?
O7 Na1 O1 91.62(6) . . ?
O2 Na1 O1 61.09(5) . . ?
O4 Na1 O1 177.42(6) . . ?
O5 Na1 O1 115.39(6) . . ?
O3 Na1 O1 120.45(6) . . ?
O8 Na1 O6 84.03(6) . . ?
O7 Na1 O6 96.36(6) . . ?
O2 Na1 O6 118.57(6) . . ?
O4 Na1 O6 119.11(6) . . ?
O5 Na1 O6 57.85(5) . . ?
O3 Na1 O6 179.02(6) . . ?
O1 Na1 O6 58.70(5) . . ?
C12 O1 C1 111.15(17) . . ?
C12 O1 Na1 116.42(13) . . ?
C1 O1 Na1 111.45(13) . . ?
C3 O2 C2 112.07(17) . . ?
C3 O2 Na1 118.47(13) . . ?
C2 O2 Na1 118.00(13) . . ?
C4 O3 C5 112.29(16) . . ?
C4 O3 Na1 113.56(13) . . ?
C5 O3 Na1 111.19(13) . . ?
C6 O4 C7 111.78(17) . . ?
C6 O4 Na1 114.59(13) . . ?
C7 O4 Na1 110.66(12) . . ?
C9 O5 C8 111.70(17) . . ?
C9 O5 Na1 122.05(13) . . ?
C8 O5 Na1 116.12(13) . . ?
C11 O6 C10 112.68(18) . . ?
C11 O6 Na1 114.78(13) . . ?
C10 O6 Na1 116.58(13) . . ?
C13 O7 C16 107.90(17) . . ?
C13 O7 Na1 128.10(14) . . ?
C16 O7 Na1 123.35(14) . . ?
C17 O8 C20 108.64(17) . . ?
C17 O8 Na1 121.02(13) . . ?
C20 O8 Na1 128.94(14) . . ?
O1 C1 C2 108.95(19) . . ?
O1 C1 H1A 109.9 . . ?
C2 C1 H1A 109.9 . . ?
O1 C1 H1B 109.9 . . ?
C2 C1 H1B 109.9 . . ?
H1A C1 H1B 108.3 . . ?
O2 C2 C1 108.31(18) . . ?
O2 C2 H2A 110.0 . . ?
C1 C2 H2A 110.0 . . ?
O2 C2 H2B 110.0 . . ?
C1 C2 H2B 110.0 . . ?
H2A C2 H2B 108.4 . . ?
O2 C3 C4 107.97(18) . . ?
O2 C3 H3A 110.1 . . ?
C4 C3 H3A 110.1 . . ?
O2 C3 H3B 110.1 . . ?
C4 C3 H3B 110.1 . . ?
H3A C3 H3B 108.4 . . ?
O3 C4 C3 107.92(18) . . ?
O3 C4 H4A 110.1 . . ?
C3 C4 H4A 110.1 . . ?
O3 C4 H4B 110.1 . . ?
C3 C4 H4B 110.1 . . ?
H4A C4 H4B 108.4 . . ?
O3 C5 C6 107.48(18) . . ?
O3 C5 H5A 110.2 . . ?
C6 C5 H5A 110.2 . . ?
O3 C5 H5B 110.2 . . ?
C6 C5 H5B 110.2 . . ?
H5A C5 H5B 108.5 . . ?
O4 C6 C5 107.91(19) . . ?
O4 C6 H6A 110.1 . . ?
C5 C6 H6A 110.1 . . ?
O4 C6 H6B 110.1 . . ?
C5 C6 H6B 110.1 . . ?
H6A C6 H6B 108.4 . . ?
O4 C7 C8 108.64(19) . . ?
O4 C7 H7A 110.0 . . ?
C8 C7 H7A 110.0 . . ?
O4 C7 H7B 110.0 . . ?
C8 C7 H7B 110.0 . . ?
H7A C7 H7B 108.3 . . ?
O5 C8 C7 108.05(18) . . ?
O5 C8 H8A 110.1 . . ?
C7 C8 H8A 110.1 . . ?
O5 C8 H8B 110.1 . . ?
C7 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
O5 C9 C10 108.11(19) . . ?
O5 C9 H9A 110.1 . . ?
C10 C9 H9A 110.1 . . ?
O5 C9 H9B 110.1 . . ?
C10 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
O6 C10 C9 108.30(19) . . ?
O6 C10 H10A 110.0 . . ?
C9 C10 H10A 110.0 . . ?
O6 C10 H10B 110.0 . . ?
C9 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
O6 C11 C12 107.95(19) . . ?
O6 C11 H11A 110.1 . . ?
C12 C11 H11A 110.1 . . ?
O6 C11 H11B 110.1 . . ?
C12 C11 H11B 110.1 . . ?
H11A C11 H11B 108.4 . . ?
O1 C12 C11 109.18(19) . . ?
O1 C12 H12A 109.8 . . ?
C11 C12 H12A 109.8 . . ?
O1 C12 H12B 109.8 . . ?
C11 C12 H12B 109.8 . . ?
H12A C12 H12B 108.3 . . ?
O7 C13 C14 106.96(19) . . ?
O7 C13 H13A 110.3 . . ?
C14 C13 H13A 110.3 . . ?
O7 C13 H13B 110.3 . . ?
C14 C13 H13B 110.3 . . ?
H13A C13 H13B 108.6 . . ?
C15 C14 C13 104.17(19) . . ?
C15 C14 H14A 110.9 . . ?
C13 C14 H14A 110.9 . . ?
C15 C14 H14B 110.9 . . ?
C13 C14 H14B 110.9 . . ?
H14A C14 H14B 108.9 . . ?
C16 C15 C14 102.7(2) . . ?
C16 C15 H15A 111.2 . . ?
C14 C15 H15A 111.2 . . ?
C16 C15 H15B 111.2 . . ?
C14 C15 H15B 111.2 . . ?
H15A C15 H15B 109.1 . . ?
O7 C16 C15 104.18(19) . . ?
O7 C16 H16A 110.9 . . ?
C15 C16 H16A 110.9 . . ?
O7 C16 H16B 110.9 . . ?
C15 C16 H16B 110.9 . . ?
H16A C16 H16B 108.9 . . ?
O8 C17 C38 104.2(5) . . ?
O8 C17 C18 106.4(2) . . ?
O8 C17 H17A 110.4 . . ?
C18 C17 H17A 110.4 . . ?
O8 C17 H17B 110.4 . . ?
C18 C17 H17B 110.4 . . ?
H17A C17 H17B 108.6 . . ?
O8 C17 H17C 110.9 . . ?
C38 C17 H17C 110.9 . . ?
O8 C17 H17D 110.9 . . ?
C38 C17 H17D 110.9 . . ?
H17C C17 H17D 108.9 . . ?
C19 C18 C17 104.8(3) . . ?
C19 C18 H18A 110.8 . . ?
C17 C18 H18A 110.8 . . ?
C19 C18 H18B 110.8 . . ?
C17 C18 H18B 110.8 . . ?
H18A C18 H18B 108.9 . . ?
C19 C38 C17 104.4(6) . . ?
C19 C38 H38A 110.9 . . ?
C17 C38 H38A 110.9 . . ?
C19 C38 H38B 110.9 . . ?
C17 C38 H38B 110.9 . . ?
H38A C38 H38B 108.9 . . ?
C18 C19 C20 102.3(3) . . ?
C38 C19 C20 106.6(4) . . ?
C18 C19 H19A 111.3 . . ?
C20 C19 H19A 111.3 . . ?
C18 C19 H19B 111.3 . . ?
C20 C19 H19B 111.3 . . ?
H19A C19 H19B 109.2 . . ?
C38 C19 H19C 110.4 . . ?
C20 C19 H19C 110.4 . . ?
C38 C19 H19D 110.4 . . ?
C20 C19 H19D 110.4 . . ?
H19C C19 H19D 108.6 . . ?
O8 C20 C19 105.67(19) . . ?
O8 C20 H20A 110.6 . . ?
C19 C20 H20A 110.6 . . ?
O8 C20 H20B 110.6 . . ?
C19 C20 H20B 110.6 . . ?
H20A C20 H20B 108.7 . . ?
C27 C21 C22 122.8(2) . . ?
C27 C21 C26 122.8(2) . . ?
C22 C21 C26 114.4(2) . . ?
C23 C22 C21 122.4(2) . . ?
C23 C22 H22 118.8 . . ?
C21 C22 H22 118.8 . . ?
C22 C23 C24 121.4(2) . . ?
C22 C23 H23 119.3 . . ?
C24 C23 H23 119.3 . . ?
C25 C24 C23 117.5(2) . . ?
C25 C24 H24 121.3 . . ?
C23 C24 H24 121.3 . . ?
C26 C25 C24 122.0(2) . . ?
C26 C25 H25 119.0 . . ?
C24 C25 H25 119.0 . . ?
C25 C26 C21 122.3(2) . . ?
C25 C26 H26 118.9 . . ?
C21 C26 H26 118.9 . . ?
C28 C27 C21 122.9(2) . . ?
C28 C27 C32 113.9(2) . . ?
C21 C27 C32 123.2(2) . . ?
C29 C28 C27 123.0(2) . . ?
C29 C28 H28 118.5 . . ?
C27 C28 H28 118.5 . . ?
C28 C29 C30 121.5(2) . . ?
C28 C29 H29 119.2 . . ?
C30 C29 H29 119.2 . . ?
C31 C30 C29 117.2(2) . . ?
C31 C30 H30 121.4 . . ?
C29 C30 H30 121.4 . . ?
C32 C31 C30 122.0(2) . . ?
C32 C31 H31 119.0 . . ?
C30 C31 H31 119.0 . . ?
C31 C32 C27 122.3(2) . . ?
C31 C32 H32 118.8 . . ?
C27 C32 H32 118.8 . . ?

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
C12 O1 C1 C2 176.92(18) . . . . ?
Na1 O1 C1 C2 -51.4(2) . . . . ?
C3 O2 C2 C1 171.81(19) . . . . ?
Na1 O2 C2 C1 -45.2(2) . . . . ?
O1 C1 C2 O2 64.4(2) . . . . ?
C2 O2 C3 C4 -172.81(18) . . . . ?
Na1 O2 C3 C4 44.4(2) . . . . ?
C5 O3 C4 C3 179.02(18) . . . . ?
Na1 O3 C4 C3 51.8(2) . . . . ?
O2 C3 C4 O3 -62.8(2) . . . . ?
C4 O3 C5 C6 178.38(18) . . . . ?
Na1 O3 C5 C6 -53.1(2) . . . . ?
C7 O4 C6 C5 -176.44(17) . . . . ?
Na1 O4 C6 C5 -49.5(2) . . . . ?
O3 C5 C6 O4 69.4(2) . . . . ?
C6 O4 C7 C8 -172.77(18) . . . . ?
Na1 O4 C7 C8 58.21(19) . . . . ?
C9 O5 C8 C7 -174.74(18) . . . . ?
Na1 O5 C8 C7 39.0(2) . . . . ?
O4 C7 C8 O5 -65.2(2) . . . . ?
C8 O5 C9 C10 167.89(19) . . . . ?
Na1 O5 C9 C10 -48.2(2) . . . . ?
C11 O6 C10 C9 -179.32(19) . . . . ?
Na1 O6 C10 C9 -43.5(2) . . . . ?
O5 C9 C10 O6 57.5(2) . . . . ?
C10 O6 C11 C12 -174.88(19) . . . . ?
Na1 O6 C11 C12 48.5(2) . . . . ?
C1 O1 C12 C11 179.35(18) . . . . ?
Na1 O1 C12 C11 50.3(2) . . . . ?
O6 C11 C12 O1 -65.3(2) . . . . ?
C16 O7 C13 C14 20.2(3) . . . . ?
Na1 O7 C13 C14 -168.89(15) . . . . ?
O7 C13 C14 C15 3.4(3) . . . . ?
C13 C14 C15 C16 -24.0(2) . . . . ?
C13 O7 C16 C15 -36.0(2) . . . . ?
Na1 O7 C16 C15 152.60(15) . . . . ?
C14 C15 C16 O7 36.6(2) . . . . ?
C20 O8 C17 C38 -33.3(7) . . . . ?
Na1 O8 C17 C38 134.3(6) . . . . ?
C20 O8 C17 C18 -3.5(4) . . . . ?
Na1 O8 C17 C18 164.2(3) . . . . ?
O8 C17 C18 C19 -18.4(5) . . . . ?
O8 C17 C38 C19 29.1(10) . . . . ?
C17 C18 C19 C20 31.7(5) . . . . ?
C17 C38 C19 C20 -15.1(11) . . . . ?
C17 O8 C20 C19 23.8(3) . . . . ?
Na1 O8 C20 C19 -142.59(17) . . . . ?
C18 C19 C20 O8 -34.5(4) . . . . ?
C38 C19 C20 O8 -4.4(8) . . . . ?
C27 C21 C22 C23 -179.1(2) . . . . ?
C26 C21 C22 C23 0.6(3) . . . . ?
C21 C22 C23 C24 0.0(4) . . . . ?
C22 C23 C24 C25 -0.4(4) . . . . ?
C23 C24 C25 C26 0.0(4) . . . . ?
C24 C25 C26 C21 0.7(4) . . . . ?
C27 C21 C26 C25 178.7(2) . . . . ?
C22 C21 C26 C25 -1.0(3) . . . . ?
C22 C21 C27 C28 -179.4(2) . . . . ?
C26 C21 C27 C28 0.9(4) . . . . ?
C22 C21 C27 C32 1.7(4) . . . . ?
C26 C21 C27 C32 -178.0(2) . . . . ?
C21 C27 C28 C29 -178.9(2) . . . . ?
C32 C27 C28 C29 0.1(3) . . . . ?
C27 C28 C29 C30 -0.6(4) . . . . ?
C28 C29 C30 C31 0.8(4) . . . . ?
C29 C30 C31 C32 -0.5(4) . . . . ?
C30 C31 C32 C27 0.0(4) . . . . ?
C28 C27 C32 C31 0.2(3) . . . . ?
C21 C27 C32 C31 179.2(2) . . . . ?

_refine_diff_density_max         0.212
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.044

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_1024SF_0mS_a
_database_code_depnum_ccdc_archive 'CCDC 1431120'
_audit_update_record             
;
2015-10-13 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H34 O8 Na, C10 H8'
_chemical_formula_sum            'C26 H42 Na O8'
_chemical_formula_weight         505.58

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   8.6161(8)
_cell_length_b                   15.7560(14)
_cell_length_c                   19.6860(18)
_cell_angle_alpha                90
_cell_angle_beta                 98.022(2)
_cell_angle_gamma                90
_cell_volume                     2646.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3423
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      24.00

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_F_000             1092
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    0.106
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6566
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus tube'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29172
_diffrn_reflns_av_unetI/netI     0.0779
_diffrn_reflns_av_R_equivalents  0.0790
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.662
_diffrn_reflns_theta_max         28.272
_diffrn_reflns_theta_full        25.242
_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 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6523
_reflns_number_gt                3999
_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-2014/6 (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)+(0.0408P)²+0.2842P] 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_number_reflns         6523
_refine_ls_number_parameters     318
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0487
_refine_ls_wR_factor_ref         0.1037
_refine_ls_wR_factor_gt          0.0853
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.001
_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 0.32483(8) 0.34759(4) 0.25994(3) 0.01710(17) Uani 1 1 d . . . . .
O1 O 0.56613(13) 0.34592(7) 0.20601(6) 0.0167(3) Uani 1 1 d . . . . .
O2 O 0.51067(14) 0.21068(8) 0.28275(6) 0.0185(3) Uani 1 1 d . . . . .
O3 O 0.47103(14) 0.33247(8) 0.37887(6) 0.0193(3) Uani 1 1 d . . . . .
O4 O 0.21705(14) 0.43071(8) 0.34960(6) 0.0178(3) Uani 1 1 d . . . . .
O5 O 0.08932(14) 0.44053(7) 0.20834(6) 0.0195(3) Uani 1 1 d . . . . .
O6 O 0.39814(14) 0.49251(8) 0.21424(6) 0.0169(3) Uani 1 1 d . . . . .
O7 O 0.09035(14) 0.26291(7) 0.27244(6) 0.0188(3) Uani 1 1 d . . . . .
O8 O 0.23524(14) 0.25788(8) 0.15394(6) 0.0197(3) Uani 1 1 d . . . . .
C1 C 0.5595(2) 0.49611(11) 0.20559(9) 0.0188(4) Uani 1 1 d . . . . .
H1A H 0.6233 0.5028 0.2512 0.023 Uiso 1 1 calc R U . . .
H1B H 0.5770 0.5468 0.1780 0.023 Uiso 1 1 calc R U . . .
C2 C 0.6149(2) 0.41879(11) 0.17109(9) 0.0167(4) Uani 1 1 d . . . . .
H2A H 0.5686 0.4175 0.1222 0.020 Uiso 1 1 calc R U . . .
H2B H 0.7305 0.4196 0.1738 0.020 Uiso 1 1 calc R U . . .
C3 C 0.6600(2) 0.27367(11) 0.19793(10) 0.0194(4) Uani 1 1 d . . . . .
H3A H 0.7644 0.2802 0.2257 0.023 Uiso 1 1 calc R U . . .
H3B H 0.6748 0.2673 0.1492 0.023 Uiso 1 1 calc R U . . .
C4 C 0.5777(2) 0.19621(11) 0.22146(9) 0.0196(4) Uani 1 1 d . . . . .
H4A H 0.4938 0.1787 0.1846 0.023 Uiso 1 1 calc R U . . .
H4B H 0.6538 0.1490 0.2293 0.023 Uiso 1 1 calc R U . . .
C5 C 0.6251(2) 0.22344(12) 0.34140(9) 0.0211(4) Uani 1 1 d . . . . .
H5A H 0.7027 0.2663 0.3312 0.025 Uiso 1 1 calc R U . . .
H5B H 0.6812 0.1697 0.3542 0.025 Uiso 1 1 calc R U . . .
C6 C 0.5428(2) 0.25339(12) 0.39919(10) 0.0224(4) Uani 1 1 d . . . . .
H6A H 0.4625 0.2116 0.4084 0.027 Uiso 1 1 calc R U . . .
H6B H 0.6186 0.2605 0.4414 0.027 Uiso 1 1 calc R U . . .
C7 C 0.4111(2) 0.37522(12) 0.43389(9) 0.0218(4) Uani 1 1 d . . . . .
H7A H 0.4978 0.3893 0.4706 0.026 Uiso 1 1 calc R U . . .
H7B H 0.3357 0.3383 0.4535 0.026 Uiso 1 1 calc R U . . .
C8 C 0.3312(2) 0.45477(12) 0.40566(9) 0.0204(4) Uani 1 1 d . . . . .
H8A H 0.2803 0.4836 0.4414 0.025 Uiso 1 1 calc R U . . .
H8B H 0.4084 0.4942 0.3900 0.025 Uiso 1 1 calc R U . . .
C9 C 0.1171(2) 0.49912(11) 0.32432(9) 0.0179(4) Uani 1 1 d . . . . .
H9A H 0.1799 0.5470 0.3103 0.021 Uiso 1 1 calc R U . . .
H9B H 0.0565 0.5193 0.3603 0.021 Uiso 1 1 calc R U . . .
C10 C 0.0082(2) 0.46623(12) 0.26372(10) 0.0201(4) Uani 1 1 d . . . . .
H10A H -0.0509 0.4172 0.2784 0.024 Uiso 1 1 calc R U . . .
H10B H -0.0684 0.5111 0.2473 0.024 Uiso 1 1 calc R U . . .
C11 C 0.1319(2) 0.50984(11) 0.16752(10) 0.0204(4) Uani 1 1 d . . . . .
H11A H 0.1289 0.5637 0.1932 0.024 Uiso 1 1 calc R U . . .
H11B H 0.0567 0.5141 0.1248 0.024 Uiso 1 1 calc R U . . .
C12 C 0.2937(2) 0.49485(12) 0.15056(9) 0.0190(4) Uani 1 1 d . . . . .
H12A H 0.2979 0.4404 0.1258 0.023 Uiso 1 1 calc R U . . .
H12B H 0.3241 0.5411 0.1210 0.023 Uiso 1 1 calc R U . . .
C13 C 0.0677(2) 0.19448(11) 0.22489(9) 0.0193(4) Uani 1 1 d . . . . .
H13A H -0.0368 0.1687 0.2258 0.023 Uiso 1 1 calc R U . . .
H13B H 0.1482 0.1503 0.2376 0.023 Uiso 1 1 calc R U . . .
C14 C 0.0800(2) 0.22733(12) 0.15474(10) 0.0211(4) Uani 1 1 d . . . . .
H14A H 0.0565 0.1814 0.1205 0.025 Uiso 1 1 calc R U . . .
H14B H 0.0036 0.2738 0.1430 0.025 Uiso 1 1 calc R U . . .
C15 C 0.0850(2) 0.23480(12) 0.34073(9) 0.0238(5) Uani 1 1 d . . . . .
H15A H -0.0128 0.2037 0.3427 0.036 Uiso 1 1 calc R U . . .
H15B H 0.0899 0.2839 0.3715 0.036 Uiso 1 1 calc R U . . .
H15C H 0.1744 0.1973 0.3551 0.036 Uiso 1 1 calc R U . . .
C16 C 0.2693(2) 0.26967(13) 0.08601(9) 0.0263(5) Uani 1 1 d . . . . .
H16A H 0.2632 0.2150 0.0621 0.039 Uiso 1 1 calc R U . . .
H16B H 0.3751 0.2931 0.0876 0.039 Uiso 1 1 calc R U . . .
H16C H 0.1931 0.3091 0.0615 0.039 Uiso 1 1 calc R U . . .
C17 C 0.5525(2) 0.53488(12) 0.01122(9) 0.0190(4) Uani 1 1 d . . . . .
C18 C 0.7151(2) 0.51715(12) 0.02615(9) 0.0223(4) Uani 1 1 d . . . . .
H18 H 0.7856 0.5621 0.0405 0.027 Uiso 1 1 calc R U . . .
C19 C 0.7746(2) 0.43528(13) 0.02038(9) 0.0255(5) Uani 1 1 d . . . . .
H19 H 0.8841 0.4254 0.0307 0.031 Uiso 1 1 calc R U . . .
C20 C 0.6745(2) 0.36870(13) -0.00036(9) 0.0248(5) Uani 1 1 d . . . . .
H20 H 0.7151 0.3131 -0.0039 0.030 Uiso 1 1 calc R U . . .
C21 C 0.5129(2) 0.38338(12) -0.01617(9) 0.0224(4) Uani 1 1 d . . . . .
H21 H 0.4455 0.3371 -0.0306 0.027 Uiso 1 1 calc R U . . .
C22 C 0.9905(2) 0.45441(11) 0.49597(9) 0.0183(4) Uani 1 1 d . . . . .
C23 C 0.8673(2) 0.42397(13) 0.44690(10) 0.0240(5) Uani 1 1 d . . . . .
H23 H 0.8537 0.3645 0.4410 0.029 Uiso 1 1 calc R U . . .
C24 C 0.7660(2) 0.47870(14) 0.40721(10) 0.0294(5) Uani 1 1 d . . . . .
H24 H 0.6845 0.4563 0.3747 0.035 Uiso 1 1 calc R U . . .
C25 C 0.7829(2) 0.56524(15) 0.41473(10) 0.0310(5) Uani 1 1 d . . . . .
H25 H 0.7124 0.6023 0.3877 0.037 Uiso 1 1 calc R U . . .
C26 C 0.9041(2) 0.59897(13) 0.46225(10) 0.0247(5) Uani 1 1 d . . . . .
H26 H 0.9154 0.6588 0.4664 0.030 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 O1 2.4630(13) . ?
Na1 O7 2.4619(14) . ?
Na1 O4 2.4800(14) . ?
Na1 O3 2.5104(14) . ?
Na1 O8 2.5492(14) . ?
Na1 O6 2.5654(14) . ?
Na1 O5 2.5921(14) . ?
Na1 O2 2.6866(14) . ?
O1 C3 1.418(2) . ?
O1 C2 1.431(2) . ?
O2 C5 1.424(2) . ?
O2 C4 1.427(2) . ?
O3 C6 1.423(2) . ?
O3 C7 1.431(2) . ?
O4 C8 1.423(2) . ?
O4 C9 1.425(2) . ?
O5 C10 1.433(2) . ?
O5 C11 1.433(2) . ?
O6 C1 1.425(2) . ?
O6 C12 1.438(2) . ?
O7 C15 1.422(2) . ?
O7 C13 1.423(2) . ?
O8 C16 1.421(2) . ?
O8 C14 1.424(2) . ?
C1 C2 1.505(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.516(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.499(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.499(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.503(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.497(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.492(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C21 1.415(3) 3_665 ?
C17 C18 1.419(3) . ?
C17 C17 1.453(4) 3_665 ?
C18 C19 1.399(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.383(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.403(3) . ?
C20 H20 0.9500 . ?
C21 C17 1.415(3) 3_665 ?
C21 H21 0.9500 . ?
C22 C26 1.414(3) 3_766 ?
C22 C23 1.415(3) . ?
C22 C22 1.452(4) 3_766 ?
C23 C24 1.388(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.377(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.405(3) . ?
C25 H25 0.9500 . ?
C26 C22 1.414(3) 3_766 ?
C26 H26 0.9500 . ?

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
O1 Na1 O7 142.29(5) . . ?
O1 Na1 O4 137.29(5) . . ?
O7 Na1 O4 79.69(4) . . ?
O1 Na1 O3 93.28(5) . . ?
O7 Na1 O3 99.63(5) . . ?
O4 Na1 O3 64.87(4) . . ?
O1 Na1 O8 79.55(4) . . ?
O7 Na1 O8 67.81(4) . . ?
O4 Na1 O8 140.78(5) . . ?
O3 Na1 O8 140.00(5) . . ?
O1 Na1 O6 66.07(4) . . ?
O7 Na1 O6 139.73(5) . . ?
O4 Na1 O6 85.10(4) . . ?
O3 Na1 O6 107.19(5) . . ?
O8 Na1 O6 105.53(5) . . ?
O1 Na1 O5 119.92(5) . . ?
O7 Na1 O5 74.74(4) . . ?
O4 Na1 O5 68.29(4) . . ?
O3 Na1 O5 133.05(5) . . ?
O8 Na1 O5 82.03(4) . . ?
O6 Na1 O5 64.99(4) . . ?
O1 Na1 O2 62.89(4) . . ?
O7 Na1 O2 91.52(4) . . ?
O4 Na1 O2 125.36(5) . . ?
O3 Na1 O2 63.78(4) . . ?
O8 Na1 O2 78.29(4) . . ?
O6 Na1 O2 127.09(5) . . ?
O5 Na1 O2 159.21(5) . . ?
C3 O1 C2 112.32(12) . . ?
C3 O1 Na1 125.87(10) . . ?
C2 O1 Na1 121.37(10) . . ?
C5 O2 C4 113.09(14) . . ?
C5 O2 Na1 110.57(10) . . ?
C4 O2 Na1 106.79(10) . . ?
C6 O3 C7 112.81(13) . . ?
C6 O3 Na1 119.14(10) . . ?
C7 O3 Na1 118.30(10) . . ?
C8 O4 C9 112.82(13) . . ?
C8 O4 Na1 113.92(10) . . ?
C9 O4 Na1 114.76(10) . . ?
C10 O5 C11 113.66(13) . . ?
C10 O5 Na1 107.44(10) . . ?
C11 O5 Na1 113.74(10) . . ?
C1 O6 C12 113.41(13) . . ?
C1 O6 Na1 111.67(10) . . ?
C12 O6 Na1 100.00(10) . . ?
C15 O7 C13 111.48(13) . . ?
C15 O7 Na1 113.47(10) . . ?
C13 O7 Na1 112.57(10) . . ?
C16 O8 C14 111.87(14) . . ?
C16 O8 Na1 128.26(11) . . ?
C14 O8 Na1 110.86(10) . . ?
O6 C1 C2 113.46(14) . . ?
O6 C1 H1A 108.9 . . ?
C2 C1 H1A 108.9 . . ?
O6 C1 H1B 108.9 . . ?
C2 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
O1 C2 C1 107.45(13) . . ?
O1 C2 H2A 110.2 . . ?
C1 C2 H2A 110.2 . . ?
O1 C2 H2B 110.2 . . ?
C1 C2 H2B 110.2 . . ?
H2A C2 H2B 108.5 . . ?
O1 C3 C4 108.25(14) . . ?
O1 C3 H3A 110.0 . . ?
C4 C3 H3A 110.0 . . ?
O1 C3 H3B 110.0 . . ?
C4 C3 H3B 110.0 . . ?
H3A C3 H3B 108.4 . . ?
O2 C4 C3 113.05(14) . . ?
O2 C4 H4A 109.0 . . ?
C3 C4 H4A 109.0 . . ?
O2 C4 H4B 109.0 . . ?
C3 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
O2 C5 C6 108.19(15) . . ?
O2 C5 H5A 110.1 . . ?
C6 C5 H5A 110.1 . . ?
O2 C5 H5B 110.1 . . ?
C6 C5 H5B 110.1 . . ?
H5A C5 H5B 108.4 . . ?
O3 C6 C5 107.18(14) . . ?
O3 C6 H6A 110.3 . . ?
C5 C6 H6A 110.3 . . ?
O3 C6 H6B 110.3 . . ?
C5 C6 H6B 110.3 . . ?
H6A C6 H6B 108.5 . . ?
O3 C7 C8 107.96(14) . . ?
O3 C7 H7A 110.1 . . ?
C8 C7 H7A 110.1 . . ?
O3 C7 H7B 110.1 . . ?
C8 C7 H7B 110.1 . . ?
H7A C7 H7B 108.4 . . ?
O4 C8 C7 107.26(15) . . ?
O4 C8 H8A 110.3 . . ?
C7 C8 H8A 110.3 . . ?
O4 C8 H8B 110.3 . . ?
C7 C8 H8B 110.3 . . ?
H8A C8 H8B 108.5 . . ?
O4 C9 C10 107.24(14) . . ?
O4 C9 H9A 110.3 . . ?
C10 C9 H9A 110.3 . . ?
O4 C9 H9B 110.3 . . ?
C10 C9 H9B 110.3 . . ?
H9A C9 H9B 108.5 . . ?
O5 C10 C9 112.59(14) . . ?
O5 C10 H10A 109.1 . . ?
C9 C10 H10A 109.1 . . ?
O5 C10 H10B 109.1 . . ?
C9 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
O5 C11 C12 108.90(14) . . ?
O5 C11 H11A 109.9 . . ?
C12 C11 H11A 109.9 . . ?
O5 C11 H11B 109.9 . . ?
C12 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
O6 C12 C11 107.38(15) . . ?
O6 C12 H12A 110.2 . . ?
C11 C12 H12A 110.2 . . ?
O6 C12 H12B 110.2 . . ?
C11 C12 H12B 110.2 . . ?
H12A C12 H12B 108.5 . . ?
O7 C13 C14 108.96(15) . . ?
O7 C13 H13A 109.9 . . ?
C14 C13 H13A 109.9 . . ?
O7 C13 H13B 109.9 . . ?
C14 C13 H13B 109.9 . . ?
H13A C13 H13B 108.3 . . ?
O8 C14 C13 108.38(15) . . ?
O8 C14 H14A 110.0 . . ?
C13 C14 H14A 110.0 . . ?
O8 C14 H14B 110.0 . . ?
C13 C14 H14B 110.0 . . ?
H14A C14 H14B 108.4 . . ?
O7 C15 H15A 109.5 . . ?
O7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O8 C16 H16A 109.5 . . ?
O8 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O8 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C21 C17 C18 123.80(17) 3_665 . ?
C21 C17 C17 118.2(2) 3_665 3_665 ?
C18 C17 C17 118.0(2) . 3_665 ?
C19 C18 C17 121.83(18) . . ?
C19 C18 H18 119.1 . . ?
C17 C18 H18 119.1 . . ?
C20 C19 C18 120.18(19) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C19 C20 C21 119.97(18) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C20 C21 C17 121.82(18) . 3_665 ?
C20 C21 H21 119.1 . . ?
C17 C21 H21 119.1 3_665 . ?
C26 C22 C23 123.71(17) 3_766 . ?
C26 C22 C22 118.1(2) 3_766 3_766 ?
C23 C22 C22 118.2(2) . 3_766 ?
C24 C23 C22 121.79(18) . . ?
C24 C23 H23 119.1 . . ?
C22 C23 H23 119.1 . . ?
C25 C24 C23 120.39(19) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C25 C26 120.24(19) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C25 C26 C22 121.29(18) . 3_766 ?
C25 C26 H26 119.4 . . ?
C22 C26 H26 119.4 3_766 . ?

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
C12 O6 C1 C2 -66.82(19) . . . . ?
Na1 O6 C1 C2 45.24(17) . . . . ?
C3 O1 C2 C1 -156.37(15) . . . . ?
Na1 O1 C2 C1 30.82(18) . . . . ?
O6 C1 C2 O1 -49.8(2) . . . . ?
C2 O1 C3 C4 -166.66(14) . . . . ?
Na1 O1 C3 C4 5.8(2) . . . . ?
C5 O2 C4 C3 -67.77(19) . . . . ?
Na1 O2 C4 C3 54.07(17) . . . . ?
O1 C3 C4 O2 -41.9(2) . . . . ?
C4 O2 C5 C6 169.85(14) . . . . ?
Na1 O2 C5 C6 50.15(16) . . . . ?
C7 O3 C6 C5 -169.87(15) . . . . ?
Na1 O3 C6 C5 44.73(18) . . . . ?
O2 C5 C6 O3 -62.37(19) . . . . ?
C6 O3 C7 C8 -176.97(15) . . . . ?
Na1 O3 C7 C8 -31.25(18) . . . . ?
C9 O4 C8 C7 171.51(14) . . . . ?
Na1 O4 C8 C7 -55.35(15) . . . . ?
O3 C7 C8 O4 55.05(18) . . . . ?
C8 O4 C9 C10 177.42(14) . . . . ?
Na1 O4 C9 C10 44.68(15) . . . . ?
C11 O5 C10 C9 -79.64(18) . . . . ?
Na1 O5 C10 C9 47.12(16) . . . . ?
O4 C9 C10 O5 -63.24(18) . . . . ?
C10 O5 C11 C12 138.86(15) . . . . ?
Na1 O5 C11 C12 15.47(17) . . . . ?
C1 O6 C12 C11 -167.83(14) . . . . ?
Na1 O6 C12 C11 73.16(13) . . . . ?
O5 C11 C12 O6 -61.78(18) . . . . ?
C15 O7 C13 C14 -178.08(14) . . . . ?
Na1 O7 C13 C14 -49.25(16) . . . . ?
C16 O8 C14 C13 164.71(15) . . . . ?
Na1 O8 C14 C13 -45.19(16) . . . . ?
O7 C13 C14 O8 63.97(18) . . . . ?
C21 C17 C18 C19 -179.85(17) 3_665 . . . ?
C17 C17 C18 C19 -0.6(3) 3_665 . . . ?
C17 C18 C19 C20 0.0(3) . . . . ?
C18 C19 C20 C21 0.5(3) . . . . ?
C19 C20 C21 C17 -0.4(3) . . . 3_665 ?
C26 C22 C23 C24 179.65(17) 3_766 . . . ?
C22 C22 C23 C24 -0.2(3) 3_766 . . . ?
C22 C23 C24 C25 -0.1(3) . . . . ?
C23 C24 C25 C26 0.6(3) . . . . ?
C24 C25 C26 C22 -1.0(3) . . . 3_766 ?

_refine_diff_density_max         0.296
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.054

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_1025SF1_0mS
_database_code_depnum_ccdc_archive 'CCDC 1431121'
_audit_update_record             
;
2015-10-13 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H40 Li1 O8, C20 H12'
_chemical_formula_sum            'C40 H52 K O8'
_chemical_formula_weight         699.91

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   17.5120(18)
_cell_length_b                   18.3856(19)
_cell_length_c                   23.115(2)
_cell_angle_alpha                90
_cell_angle_beta                 98.461(2)
_cell_angle_gamma                90
_cell_volume                     7361.5(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9952
_cell_measurement_theta_min      2.215
_cell_measurement_theta_max      26.855

_exptl_crystal_description       Platty
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_F_000             3000
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.016
_exptl_absorpt_coefficient_mu    0.196
_shelx_estimated_absorpt_T_min   0.954
_shelx_estimated_absorpt_T_max   0.997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6580
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus tube'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            58331
_diffrn_reflns_av_unetI/netI     0.0757
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.176
_diffrn_reflns_theta_max         28.389
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             18221
_reflns_number_gt                11429
_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-2014/6 (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)+(0.0681P)²+8.2240P] 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_number_reflns         18221
_refine_ls_number_parameters     903
_refine_ls_number_restraints     93
_refine_ls_R_factor_all          0.1178
_refine_ls_R_factor_gt           0.0656
_refine_ls_wR_factor_ref         0.1784
_refine_ls_wR_factor_gt          0.1549
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.047
_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
K1 K -0.03671(3) 0.23968(3) 0.41149(3) 0.01969(14) Uani 1 1 d . . . . .
K2 K 0.46317(3) 0.24370(3) 0.40276(2) 0.01943(13) Uani 1 1 d . . . . .
O1 O -0.14166(11) 0.27355(11) 0.31392(8) 0.0233(4) Uani 1 1 d . . . . .
O2 O -0.16946(11) 0.15335(10) 0.38667(8) 0.0224(4) Uani 1 1 d . . . . .
O3 O -0.04505(10) 0.10280(11) 0.46906(8) 0.0220(4) Uani 1 1 d . . . . .
O4 O 0.07513(10) 0.20496(10) 0.50528(8) 0.0198(4) Uani 1 1 d . . . . .
O5 O 0.10263(11) 0.32234(10) 0.42912(8) 0.0207(4) Uani 1 1 d . . . . .
O6 O -0.02570(11) 0.37542(10) 0.35453(8) 0.0234(4) Uani 1 1 d . . . . .
O7 O 0.04977(18) 0.15515(13) 0.35251(12) 0.0558(8) Uani 1 1 d . U . . .
O8 O -0.12381(16) 0.31205(18) 0.47959(14) 0.0697(9) Uani 1 1 d D U . . .
O9 O 0.32946(11) 0.22918(10) 0.32002(8) 0.0225(4) Uani 1 1 d . . . . .
O10 O 0.35333(11) 0.35691(11) 0.38635(8) 0.0241(4) Uani 1 1 d . . . . .
O11 O 0.47493(11) 0.35950(11) 0.48118(9) 0.0256(4) Uani 1 1 d . . . . .
O12 O 0.60368(11) 0.26329(10) 0.47996(8) 0.0240(4) Uani 1 1 d . . . . .
O13 O 0.58276(11) 0.13799(11) 0.41150(8) 0.0234(4) Uani 1 1 d . . . . .
O14 O 0.46510(11) 0.14391(10) 0.31348(8) 0.0234(4) Uani 1 1 d . . . . .
O15 O 0.53415(13) 0.34064(14) 0.34485(11) 0.0467(7) Uani 1 1 d . . . . .
O16 O 0.39529(13) 0.13195(14) 0.45265(11) 0.0446(7) Uani 1 1 d . . . . .
C1 C -0.21467(15) 0.23905(17) 0.31368(12) 0.0248(6) Uani 1 1 d . . . . .
H1A H -0.2467 0.2452 0.2750 0.030 Uiso 1 1 calc R U . . .
H1B H -0.2422 0.2615 0.3436 0.030 Uiso 1 1 calc R U . . .
C2 C -0.20195(16) 0.16031(16) 0.32655(12) 0.0240(6) Uani 1 1 d . . . . .
H2A H -0.2515 0.1337 0.3189 0.029 Uiso 1 1 calc R U . . .
H2B H -0.1663 0.1397 0.3013 0.029 Uiso 1 1 calc R U . . .
C3 C -0.16121(16) 0.07987(16) 0.40593(13) 0.0253(6) Uani 1 1 d . . . . .
H3A H -0.1296 0.0524 0.3812 0.030 Uiso 1 1 calc R U . . .
H3B H -0.2125 0.0564 0.4029 0.030 Uiso 1 1 calc R U . . .
C4 C -0.12273(15) 0.07989(16) 0.46820(13) 0.0239(6) Uani 1 1 d . . . . .
H4A H -0.1499 0.1135 0.4917 0.029 Uiso 1 1 calc R U . . .
H4B H -0.1240 0.0305 0.4850 0.029 Uiso 1 1 calc R U . . .
C5 C -0.00230(16) 0.10492(16) 0.52665(12) 0.0237(6) Uani 1 1 d . . . . .
H5A H -0.0007 0.0559 0.5446 0.028 Uiso 1 1 calc R U . . .
H5B H -0.0272 0.1387 0.5515 0.028 Uiso 1 1 calc R U . . .
C6 C 0.07793(16) 0.13029(15) 0.52193(12) 0.0220(6) Uani 1 1 d . . . . .
H6A H 0.1115 0.1243 0.5600 0.026 Uiso 1 1 calc R U . . .
H6B H 0.0997 0.1009 0.4924 0.026 Uiso 1 1 calc R U . . .
C7 C 0.14966(15) 0.23131(15) 0.49819(12) 0.0210(6) Uani 1 1 d . . . . .
H7A H 0.1683 0.2058 0.4652 0.025 Uiso 1 1 calc R U . . .
H7B H 0.1865 0.2217 0.5341 0.025 Uiso 1 1 calc R U . . .
C8 C 0.14515(16) 0.31134(15) 0.48634(12) 0.0204(6) Uani 1 1 d . . . . .
H8A H 0.1189 0.3361 0.5160 0.025 Uiso 1 1 calc R U . . .
H8B H 0.1977 0.3319 0.4883 0.025 Uiso 1 1 calc R U . . .
C9 C 0.09313(17) 0.39743(15) 0.41523(13) 0.0252(6) Uani 1 1 d . . . . .
H9A H 0.1442 0.4213 0.4175 0.030 Uiso 1 1 calc R U . . .
H9B H 0.0639 0.4216 0.4433 0.030 Uiso 1 1 calc R U . . .
C10 C 0.05012(16) 0.40360(16) 0.35461(13) 0.0255(6) Uani 1 1 d . . . . .
H10A H 0.0474 0.4551 0.3421 0.031 Uiso 1 1 calc R U . . .
H10B H 0.0770 0.3757 0.3270 0.031 Uiso 1 1 calc R U . . .
C11 C -0.07071(17) 0.37892(17) 0.29791(13) 0.0283(7) Uani 1 1 d . . . . .
H11A H -0.0456 0.3502 0.2697 0.034 Uiso 1 1 calc R U . . .
H11B H -0.0748 0.4300 0.2842 0.034 Uiso 1 1 calc R U . . .
C12 C -0.14904(17) 0.34928(16) 0.30131(13) 0.0264(7) Uani 1 1 d . . . . .
H12A H -0.1720 0.3745 0.3325 0.032 Uiso 1 1 calc R U . . .
H12B H -0.1831 0.3569 0.2637 0.032 Uiso 1 1 calc R U . . .
C19 C -0.1926(3) 0.4026(3) 0.51994(17) 0.0771(16) Uani 1 1 d . U . . .
H19A H -0.2131 0.3880 0.5559 0.093 Uiso 0.53(2) 1 calc R U P A 1
H19B H -0.2196 0.4472 0.5039 0.093 Uiso 0.53(2) 1 calc R U P A 1
H19C H -0.2178 0.4338 0.4877 0.093 Uiso 0.47(2) 1 calc R U P A 2
H19D H -0.2176 0.4098 0.5552 0.093 Uiso 0.47(2) 1 calc R U P A 2
C13 C 0.0943(3) 0.1900(2) 0.31390(19) 0.0649(13) Uani 1 1 d . U . . .
H13A H 0.1260 0.2293 0.3344 0.078 Uiso 1 1 calc R U . . .
H13B H 0.0602 0.2113 0.2802 0.078 Uiso 1 1 calc R U . . .
C14 C 0.1441(2) 0.1331(2) 0.29403(16) 0.0507(10) Uani 1 1 d . U . . .
H14A H 0.1918 0.1263 0.3223 0.061 Uiso 1 1 calc R U . . .
H14B H 0.1582 0.1450 0.2552 0.061 Uiso 1 1 calc R U . . .
C15 C 0.0934(2) 0.06684(18) 0.29109(14) 0.0370(8) Uani 1 1 d . U . . .
H15A H 0.1245 0.0218 0.2977 0.044 Uiso 1 1 calc R U . . .
H15B H 0.0596 0.0635 0.2529 0.044 Uiso 1 1 calc R U . . .
C18 C -0.1094(3) 0.4141(3) 0.5316(2) 0.0807(16) Uani 1 1 d . U . . .
H18A H -0.0941 0.4361 0.5707 0.097 Uiso 0.660(10) 1 calc R U P A 1
H18B H -0.0921 0.4462 0.5017 0.097 Uiso 0.660(10) 1 calc R U P A 1
H18C H -0.0968 0.4666 0.5319 0.097 Uiso 0.340(10) 1 calc R U P A 2
H18D H -0.0872 0.3926 0.5697 0.097 Uiso 0.340(10) 1 calc R U P A 2
C16 C 0.0469(3) 0.0798(2) 0.3400(2) 0.0661(14) Uani 1 1 d . U . . .
H16A H -0.0072 0.0641 0.3280 0.079 Uiso 1 1 calc R U . . .
H16B H 0.0688 0.0517 0.3751 0.079 Uiso 1 1 calc R U . . .
C17 C -0.0745(3) 0.3370(4) 0.5290(3) 0.0485(19) Uani 0.660(10) 1 d D U P A 1
H17A H -0.0199 0.3384 0.5226 0.058 Uiso 0.660(10) 1 calc R U P A 1
H17B H -0.0794 0.3080 0.5643 0.058 Uiso 0.660(10) 1 calc R U P A 1
C20 C -0.2009(4) 0.3446(7) 0.4772(5) 0.052(3) Uani 0.53(2) 1 d D U P A 1
H20A H -0.2192 0.3640 0.4376 0.063 Uiso 0.53(2) 1 calc R U P A 1
H20B H -0.2384 0.3079 0.4869 0.063 Uiso 0.53(2) 1 calc R U P A 1
C87 C -0.0879(7) 0.3864(7) 0.4955(6) 0.060(4) Uani 0.340(10) 1 d D U P A 2
H87A H -0.0313 0.3802 0.5057 0.072 Uiso 0.340(10) 1 calc R U P A 2
H87B H -0.0972 0.4181 0.4605 0.072 Uiso 0.340(10) 1 calc R U P A 2
C90 C -0.1905(6) 0.3120(8) 0.4998(5) 0.046(3) Uani 0.47(2) 1 d D U P A 2
H90A H -0.1900 0.2790 0.5337 0.055 Uiso 0.47(2) 1 calc R U P A 2
H90B H -0.2341 0.2993 0.4692 0.055 Uiso 0.47(2) 1 calc R U P A 2
C21 C 0.35508(15) 0.77079(15) 0.33814(11) 0.0175(5) Uani 1 1 d . . . . .
C22 C 0.42673(15) 0.80700(16) 0.34067(12) 0.0213(6) Uani 1 1 d . . . . .
H22 H 0.4708 0.7807 0.3329 0.026 Uiso 1 1 calc R U . . .
C23 C 0.43358(16) 0.88031(16) 0.35423(12) 0.0246(6) Uani 1 1 d . . . . .
H23 H 0.4825 0.9032 0.3561 0.030 Uiso 1 1 calc R U . . .
C24 C 0.37077(16) 0.92082(16) 0.36505(12) 0.0234(6) Uani 1 1 d . . . . .
H24 H 0.3770 0.9710 0.3746 0.028 Uiso 1 1 calc R U . . .
C25 C 0.29721(16) 0.88787(15) 0.36202(11) 0.0196(6) Uani 1 1 d . . . . .
C26 C 0.23173(17) 0.92778(15) 0.37277(12) 0.0235(6) Uani 1 1 d . . . . .
H26 H 0.2363 0.9783 0.3811 0.028 Uiso 1 1 calc R U . . .
C27 C 0.16126(17) 0.89368(16) 0.37127(13) 0.0261(6) Uani 1 1 d . . . . .
H27 H 0.1180 0.9210 0.3793 0.031 Uiso 1 1 calc R U . . .
C28 C 0.15253(16) 0.82061(15) 0.35839(13) 0.0231(6) Uani 1 1 d . . . . .
H28 H 0.1033 0.7987 0.3578 0.028 Uiso 1 1 calc R U . . .
C29 C 0.21484(15) 0.77764(14) 0.34604(11) 0.0174(5) Uani 1 1 d . . . . .
C30 C 0.20688(15) 0.70118(15) 0.33188(11) 0.0179(5) Uani 1 1 d . . . . .
C31 C 0.13459(16) 0.66570(16) 0.32312(13) 0.0247(6) Uani 1 1 d . . . . .
H31 H 0.0891 0.6933 0.3246 0.030 Uiso 1 1 calc R U . . .
C32 C 0.12821(17) 0.59184(16) 0.31240(13) 0.0277(7) Uani 1 1 d . . . . .
H32 H 0.0785 0.5699 0.3063 0.033 Uiso 1 1 calc R U . . .
C33 C 0.19251(17) 0.54958(16) 0.31046(12) 0.0246(6) Uani 1 1 d . . . . .
H33 H 0.1871 0.4985 0.3050 0.030 Uiso 1 1 calc R U . . .
C34 C 0.26667(16) 0.58164(15) 0.31657(11) 0.0202(6) Uani 1 1 d . . . . .
C35 C 0.33364(17) 0.54051(15) 0.31296(12) 0.0243(6) Uani 1 1 d . . . . .
H35 H 0.3297 0.4893 0.3079 0.029 Uiso 1 1 calc R U . . .
C36 C 0.40473(17) 0.57360(17) 0.31674(13) 0.0277(7) Uani 1 1 d . . . . .
H36 H 0.4493 0.5447 0.3148 0.033 Uiso 1 1 calc R U . . .
C37 C 0.41259(16) 0.64865(16) 0.32339(12) 0.0230(6) Uani 1 1 d . . . . .
H37 H 0.4621 0.6703 0.3247 0.028 Uiso 1 1 calc R U . . .
C38 C 0.34811(15) 0.69301(15) 0.32824(11) 0.0180(5) Uani 1 1 d . . . . .
C39 C 0.28886(15) 0.81152(14) 0.34834(11) 0.0162(5) Uani 1 1 d . . . . .
C40 C 0.27400(15) 0.65931(14) 0.32567(11) 0.0171(5) Uani 1 1 d . . . . .
C41 C 0.28687(16) 0.29445(16) 0.30495(12) 0.0243(6) Uani 1 1 d . . . . .
H41A H 0.2352 0.2825 0.2836 0.029 Uiso 1 1 calc R U . . .
H41B H 0.3142 0.3250 0.2793 0.029 Uiso 1 1 calc R U . . .
C42 C 0.27892(16) 0.33479(16) 0.36010(13) 0.0252(6) Uani 1 1 d . . . . .
H42A H 0.2453 0.3778 0.3511 0.030 Uiso 1 1 calc R U . . .
H42B H 0.2554 0.3029 0.3871 0.030 Uiso 1 1 calc R U . . .
C43 C 0.35161(17) 0.40173(16) 0.43669(13) 0.0278(7) Uani 1 1 d . . . . .
H43A H 0.3280 0.3749 0.4667 0.033 Uiso 1 1 calc R U . . .
H43B H 0.3205 0.4459 0.4259 0.033 Uiso 1 1 calc R U . . .
C44 C 0.43308(18) 0.42227(16) 0.46024(13) 0.0286(7) Uani 1 1 d . . . . .
H44A H 0.4578 0.4452 0.4290 0.034 Uiso 1 1 calc R U . . .
H44B H 0.4333 0.4578 0.4924 0.034 Uiso 1 1 calc R U . . .
C45 C 0.55247(18) 0.37608(16) 0.50642(13) 0.0286(7) Uani 1 1 d . . . . .
H45A H 0.5524 0.4109 0.5391 0.034 Uiso 1 1 calc R U . . .
H45B H 0.5803 0.3987 0.4767 0.034 Uiso 1 1 calc R U . . .
C46 C 0.59196(19) 0.30726(17) 0.52840(12) 0.0289(7) Uani 1 1 d . . . . .
H46A H 0.6422 0.3186 0.5523 0.035 Uiso 1 1 calc R U . . .
H46B H 0.5599 0.2808 0.5533 0.035 Uiso 1 1 calc R U . . .
C47 C 0.64063(17) 0.19600(16) 0.49826(12) 0.0247(6) Uani 1 1 d . . . . .
H47A H 0.6071 0.1668 0.5203 0.030 Uiso 1 1 calc R U . . .
H47B H 0.6900 0.2054 0.5240 0.030 Uiso 1 1 calc R U . . .
C48 C 0.65509(16) 0.15604(16) 0.44506(13) 0.0253(6) Uani 1 1 d . . . . .
H48A H 0.6855 0.1868 0.4216 0.030 Uiso 1 1 calc R U . . .
H48B H 0.6849 0.1112 0.4563 0.030 Uiso 1 1 calc R U . . .
C49 C 0.59079(16) 0.10758(16) 0.35617(13) 0.0241(6) Uani 1 1 d . . . . .
H49A H 0.6271 0.0660 0.3614 0.029 Uiso 1 1 calc R U . . .
H49B H 0.6116 0.1445 0.3315 0.029 Uiso 1 1 calc R U . . .
C50 C 0.51315(17) 0.08242(16) 0.32708(14) 0.0269(6) Uani 1 1 d . . . . .
H50A H 0.5186 0.0554 0.2909 0.032 Uiso 1 1 calc R U . . .
H50B H 0.4899 0.0494 0.3535 0.032 Uiso 1 1 calc R U . . .
C51 C 0.38971(17) 0.12470(16) 0.28518(13) 0.0282(7) Uani 1 1 d . . . . .
H51A H 0.3630 0.0952 0.3119 0.034 Uiso 1 1 calc R U . . .
H51B H 0.3937 0.0954 0.2498 0.034 Uiso 1 1 calc R U . . .
C52 C 0.34504(17) 0.19225(17) 0.26855(12) 0.0272(7) Uani 1 1 d . . . . .
H52A H 0.3749 0.2244 0.2459 0.033 Uiso 1 1 calc R U . . .
H52B H 0.2958 0.1798 0.2436 0.033 Uiso 1 1 calc R U . . .
C53 C 0.50225(16) 0.38804(16) 0.29859(13) 0.0263(6) Uani 1 1 d . . . . .
H53A H 0.4577 0.4155 0.3093 0.032 Uiso 1 1 calc R U . . .
H53B H 0.4854 0.3605 0.2622 0.032 Uiso 1 1 calc R U . . .
C54 C 0.56852(17) 0.43855(16) 0.29150(15) 0.0290(7) Uani 1 1 d . . . . .
H54A H 0.5711 0.4797 0.3194 0.035 Uiso 1 1 calc R U . . .
H54B H 0.5635 0.4580 0.2512 0.035 Uiso 1 1 calc R U . . .
C55 C 0.63983(16) 0.38949(16) 0.30489(13) 0.0266(7) Uani 1 1 d . . . . .
H55A H 0.6602 0.3762 0.2686 0.032 Uiso 1 1 calc R U . . .
H55B H 0.6811 0.4139 0.3319 0.032 Uiso 1 1 calc R U . . .
C56 C 0.6099(2) 0.3229(2) 0.33332(18) 0.0498(11) Uani 1 1 d . . . . .
H56A H 0.6081 0.2804 0.3068 0.060 Uiso 1 1 calc R U . . .
H56B H 0.6440 0.3109 0.3702 0.060 Uiso 1 1 calc R U . . .
C57 C 0.3209(2) 0.1447(2) 0.4686(2) 0.0574(12) Uani 1 1 d . . . . .
H57A H 0.2822 0.1516 0.4332 0.069 Uiso 1 1 calc R U . . .
H57B H 0.3216 0.1888 0.4932 0.069 Uiso 1 1 calc R U . . .
C58 C 0.30102(18) 0.07879(19) 0.50224(14) 0.0353(8) Uani 1 1 d . . . . .
H58A H 0.2614 0.0487 0.4784 0.042 Uiso 1 1 calc R U . . .
H58B H 0.2817 0.0932 0.5387 0.042 Uiso 1 1 calc R U . . .
C59 C 0.3771(2) 0.03779(19) 0.51569(16) 0.0392(8) Uani 1 1 d . . . . .
H59A H 0.3887 0.0257 0.5578 0.047 Uiso 1 1 calc R U . . .
H59B H 0.3759 -0.0076 0.4926 0.047 Uiso 1 1 calc R U . . .
C60 C 0.43535(19) 0.0903(2) 0.49826(16) 0.0399(9) Uani 1 1 d . . . . .
H60A H 0.4561 0.1218 0.5317 0.048 Uiso 1 1 calc R U . . .
H60B H 0.4787 0.0639 0.4848 0.048 Uiso 1 1 calc R U . . .
C61 C 0.15646(15) 0.31052(16) 0.63734(11) 0.0205(6) Uani 1 1 d . . . . .
C62 C 0.09537(17) 0.36127(17) 0.63468(12) 0.0268(7) Uani 1 1 d . . . . .
H62 H 0.0463 0.3455 0.6426 0.032 Uiso 1 1 calc R U . . .
C63 C 0.10588(18) 0.43355(17) 0.62076(13) 0.0315(7) Uani 1 1 d . . . . .
H63 H 0.0639 0.4665 0.6196 0.038 Uiso 1 1 calc R U . . .
C64 C 0.17567(18) 0.45840(16) 0.60868(13) 0.0288(7) Uani 1 1 d . . . . .
H64 H 0.1813 0.5082 0.5994 0.035 Uiso 1 1 calc R U . . .
C65 C 0.23942(17) 0.41073(16) 0.60989(11) 0.0232(6) Uani 1 1 d . . . . .
C66 C 0.31140(18) 0.43480(17) 0.59723(12) 0.0273(7) Uani 1 1 d . . . . .
H66 H 0.3183 0.4845 0.5880 0.033 Uiso 1 1 calc R U . . .
C67 C 0.37196(17) 0.38690(17) 0.59815(12) 0.0277(7) Uani 1 1 d . . . . .
H67 H 0.4202 0.4040 0.5895 0.033 Uiso 1 1 calc R U . . .
C68 C 0.36359(16) 0.31408(16) 0.61144(12) 0.0239(6) Uani 1 1 d . . . . .
H68 H 0.4061 0.2820 0.6110 0.029 Uiso 1 1 calc R U . . .
C69 C 0.29345(15) 0.28648(15) 0.62557(11) 0.0190(6) Uani 1 1 d . . . . .
C70 C 0.28510(15) 0.21163(15) 0.64335(11) 0.0181(6) Uani 1 1 d . . . . .
C71 C 0.34808(16) 0.16267(15) 0.65062(12) 0.0221(6) Uani 1 1 d . . . . .
H71 H 0.3968 0.1785 0.6420 0.027 Uiso 1 1 calc R U . . .
C72 C 0.34021(16) 0.09230(16) 0.67000(13) 0.0255(7) Uani 1 1 d . . . . .
H72 H 0.3838 0.0610 0.6751 0.031 Uiso 1 1 calc R U . . .
C73 C 0.27005(16) 0.06663(16) 0.68210(12) 0.0232(6) Uani 1 1 d . . . . .
H73 H 0.2657 0.0179 0.6949 0.028 Uiso 1 1 calc R U . . .
C74 C 0.20437(16) 0.11295(15) 0.67543(11) 0.0205(6) Uani 1 1 d . . . . .
C75 C 0.13170(17) 0.08826(17) 0.68732(12) 0.0260(6) Uani 1 1 d . . . . .
H75 H 0.1259 0.0395 0.6995 0.031 Uiso 1 1 calc R U . . .
C76 C 0.06917(17) 0.13480(18) 0.68128(13) 0.0284(7) Uani 1 1 d . . . . .
H76 H 0.0204 0.1173 0.6884 0.034 Uiso 1 1 calc R U . . .
C77 C 0.07664(16) 0.20682(17) 0.66489(12) 0.0256(6) Uani 1 1 d . . . . .
H77 H 0.0329 0.2379 0.6616 0.031 Uiso 1 1 calc R U . . .
C78 C 0.14758(15) 0.23496(15) 0.65295(11) 0.0189(6) Uani 1 1 d . . . . .
C79 C 0.22936(15) 0.33549(15) 0.62434(11) 0.0192(6) Uani 1 1 d . . . . .
C80 C 0.21237(15) 0.18674(15) 0.65677(11) 0.0177(5) Uani 1 1 d . . . . .


_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
K1 O7 2.679(3) . ?
K1 O8 2.699(3) . ?
K1 O1 2.7627(19) . ?
K1 O4 2.7738(18) . ?
K1 O2 2.8037(19) . ?
K1 O6 2.841(2) . ?
K1 O5 2.8526(19) . ?
K1 O3 2.861(2) . ?
K2 O15 2.646(2) . ?
K2 O16 2.714(2) . ?
K2 O14 2.765(2) . ?
K2 O11 2.784(2) . ?
K2 O9 2.8097(19) . ?
K2 O10 2.822(2) . ?
K2 O12 2.8418(19) . ?
K2 O13 2.842(2) . ?
O1 C12 1.425(3) . ?
O1 C1 1.427(3) . ?
O2 C3 1.423(3) . ?
O2 C2 1.428(3) . ?
O3 C4 1.421(3) . ?
O3 C5 1.429(3) . ?
O4 C7 1.424(3) . ?
O4 C6 1.425(3) . ?
O5 C9 1.422(3) . ?
O5 C8 1.433(3) . ?
O6 C10 1.425(3) . ?
O6 C11 1.426(3) . ?
O7 C16 1.415(4) . ?
O7 C13 1.421(4) . ?
O8 C90 1.321(8) . ?
O8 C17 1.403(6) . ?
O8 C20 1.470(9) . ?
O8 C87 1.527(11) . ?
O9 C41 1.429(3) . ?
O9 C52 1.431(3) . ?
O10 C42 1.414(3) . ?
O10 C43 1.430(3) . ?
O11 C44 1.414(3) . ?
O11 C45 1.430(3) . ?
O12 C46 1.420(3) . ?
O12 C47 1.431(3) . ?
O13 C49 1.422(3) . ?
O13 C48 1.424(3) . ?
O14 C50 1.417(3) . ?
O14 C51 1.429(3) . ?
O15 C53 1.428(3) . ?
O15 C56 1.430(4) . ?
O16 C60 1.405(4) . ?
O16 C57 1.425(4) . ?
C1 C2 1.488(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.497(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.500(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.497(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.494(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.489(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C19 C20 1.447(9) . ?
C19 C18 1.457(7) . ?
C19 C90 1.731(14) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 H19C 0.9900 . ?
C19 H19D 0.9900 . ?
C13 C14 1.478(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.504(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.505(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C18 C87 1.091(13) . ?
C18 C17 1.547(8) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 H18C 0.9900 . ?
C18 H18D 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C87 H87A 0.9900 . ?
C87 H87B 0.9900 . ?
C90 H90A 0.9900 . ?
C90 H90B 0.9900 . ?
C21 C22 1.414(4) . ?
C21 C39 1.429(4) . ?
C21 C38 1.451(4) . ?
C22 C23 1.385(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.381(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.416(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.414(4) . ?
C25 C39 1.442(4) . ?
C26 C27 1.380(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.380(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.410(4) . ?
C28 H28 0.9500 . ?
C29 C39 1.432(4) . ?
C29 C30 1.445(4) . ?
C30 C31 1.412(4) . ?
C30 C40 1.430(4) . ?
C31 C32 1.382(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.374(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.414(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.408(4) . ?
C34 C40 1.446(4) . ?
C35 C36 1.377(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.393(4) . ?
C36 H36 0.9500 . ?
C37 C38 1.411(4) . ?
C37 H37 0.9500 . ?
C38 C40 1.432(4) . ?
C41 C42 1.499(4) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.499(4) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.495(4) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.486(4) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C50 1.499(4) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.488(4) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.514(4) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.535(4) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C56 1.519(5) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 C58 1.508(5) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 C59 1.522(5) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 C60 1.502(5) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C61 C62 1.414(4) . ?
C61 C79 1.429(4) . ?
C61 C78 1.450(4) . ?
C62 C63 1.386(4) . ?
C62 H62 0.9500 . ?
C63 C64 1.371(5) . ?
C63 H63 0.9500 . ?
C64 C65 1.416(4) . ?
C64 H64 0.9500 . ?
C65 C66 1.407(4) . ?
C65 C79 1.440(4) . ?
C66 C67 1.376(4) . ?
C66 H66 0.9500 . ?
C67 C68 1.386(4) . ?
C67 H67 0.9500 . ?
C68 C69 1.411(4) . ?
C68 H68 0.9500 . ?
C69 C79 1.436(4) . ?
C69 C70 1.450(4) . ?
C70 C71 1.414(4) . ?
C70 C80 1.430(4) . ?
C71 C72 1.383(4) . ?
C71 H71 0.9500 . ?
C72 C73 1.383(4) . ?
C72 H72 0.9500 . ?
C73 C74 1.421(4) . ?
C73 H73 0.9500 . ?
C74 C75 1.416(4) . ?
C74 C80 1.437(4) . ?
C75 C76 1.380(4) . ?
C75 H75 0.9500 . ?
C76 C77 1.389(4) . ?
C76 H76 0.9500 . ?
C77 C78 1.410(4) . ?
C77 H77 0.9500 . ?
C78 C80 1.432(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 K1 O8 173.43(10) . . ?
O7 K1 O1 94.21(8) . . ?
O8 K1 O1 89.99(8) . . ?
O7 K1 O4 82.95(8) . . ?
O8 K1 O4 92.99(8) . . ?
O1 K1 O4 176.70(6) . . ?
O7 K1 O2 94.66(8) . . ?
O8 K1 O2 82.86(8) . . ?
O1 K1 O2 61.87(6) . . ?
O4 K1 O2 119.90(6) . . ?
O7 K1 O6 101.06(7) . . ?
O8 K1 O6 85.41(9) . . ?
O1 K1 O6 60.40(6) . . ?
O4 K1 O6 118.43(6) . . ?
O2 K1 O6 120.87(6) . . ?
O7 K1 O5 81.14(8) . . ?
O8 K1 O5 101.48(8) . . ?
O1 K1 O5 116.67(6) . . ?
O4 K1 O5 61.32(5) . . ?
O2 K1 O5 175.53(6) . . ?
O6 K1 O5 58.89(5) . . ?
O7 K1 O3 78.33(7) . . ?
O8 K1 O3 95.19(9) . . ?
O1 K1 O3 120.31(6) . . ?
O4 K1 O3 60.82(5) . . ?
O2 K1 O3 59.97(5) . . ?
O6 K1 O3 179.05(6) . . ?
O5 K1 O3 120.23(5) . . ?
O15 K2 O16 172.91(9) . . ?
O15 K2 O14 90.64(8) . . ?
O16 K2 O14 82.48(7) . . ?
O15 K2 O11 79.58(8) . . ?
O16 K2 O11 107.29(8) . . ?
O14 K2 O11 170.20(6) . . ?
O15 K2 O9 97.24(7) . . ?
O16 K2 O9 81.03(7) . . ?
O14 K2 O9 61.93(6) . . ?
O11 K2 O9 119.36(6) . . ?
O15 K2 O10 78.28(7) . . ?
O16 K2 O10 106.44(7) . . ?
O14 K2 O10 118.17(6) . . ?
O11 K2 O10 60.47(6) . . ?
O9 K2 O10 59.68(6) . . ?
O15 K2 O12 78.73(7) . . ?
O16 K2 O12 102.83(7) . . ?
O14 K2 O12 116.63(6) . . ?
O11 K2 O12 61.31(6) . . ?
O9 K2 O12 175.81(6) . . ?
O10 K2 O12 120.07(6) . . ?
O15 K2 O13 95.77(6) . . ?
O16 K2 O13 79.42(6) . . ?
O14 K2 O13 60.63(6) . . ?
O11 K2 O13 119.57(6) . . ?
O9 K2 O13 120.99(6) . . ?
O10 K2 O13 173.99(6) . . ?
O12 K2 O13 58.75(6) . . ?
C12 O1 C1 112.3(2) . . ?
C12 O1 K1 114.63(15) . . ?
C1 O1 K1 113.02(15) . . ?
C3 O2 C2 113.4(2) . . ?
C3 O2 K1 115.50(15) . . ?
C2 O2 K1 110.37(15) . . ?
C4 O3 C5 113.0(2) . . ?
C4 O3 K1 111.62(15) . . ?
C5 O3 K1 110.73(15) . . ?
C7 O4 C6 111.3(2) . . ?
C7 O4 K1 112.68(14) . . ?
C6 O4 K1 115.17(14) . . ?
C9 O5 C8 111.9(2) . . ?
C9 O5 K1 114.58(15) . . ?
C8 O5 K1 111.97(15) . . ?
C10 O6 C11 112.0(2) . . ?
C10 O6 K1 116.45(15) . . ?
C11 O6 K1 113.51(16) . . ?
C16 O7 C13 108.6(3) . . ?
C16 O7 K1 131.8(2) . . ?
C13 O7 K1 117.5(2) . . ?
C17 O8 C20 110.4(4) . . ?
C90 O8 C87 105.6(7) . . ?
C90 O8 K1 144.3(5) . . ?
C17 O8 K1 107.7(3) . . ?
C20 O8 K1 140.7(4) . . ?
C87 O8 K1 109.5(5) . . ?
C41 O9 C52 110.6(2) . . ?
C41 O9 K2 116.05(15) . . ?
C52 O9 K2 111.68(15) . . ?
C42 O10 C43 112.7(2) . . ?
C42 O10 K2 114.37(16) . . ?
C43 O10 K2 114.28(16) . . ?
C44 O11 C45 112.3(2) . . ?
C44 O11 K2 114.61(16) . . ?
C45 O11 K2 113.81(16) . . ?
C46 O12 C47 111.7(2) . . ?
C46 O12 K2 110.79(16) . . ?
C47 O12 K2 112.84(15) . . ?
C49 O13 C48 112.6(2) . . ?
C49 O13 K2 111.99(15) . . ?
C48 O13 K2 117.81(16) . . ?
C50 O14 C51 112.5(2) . . ?
C50 O14 K2 115.85(16) . . ?
C51 O14 K2 113.19(16) . . ?
C53 O15 C56 105.8(2) . . ?
C53 O15 K2 128.95(18) . . ?
C56 O15 K2 117.28(18) . . ?
C60 O16 C57 105.7(3) . . ?
C60 O16 K2 122.01(19) . . ?
C57 O16 K2 117.4(2) . . ?
O1 C1 C2 108.9(2) . . ?
O1 C1 H1A 109.9 . . ?
C2 C1 H1A 109.9 . . ?
O1 C1 H1B 109.9 . . ?
C2 C1 H1B 109.9 . . ?
H1A C1 H1B 108.3 . . ?
O2 C2 C1 108.0(2) . . ?
O2 C2 H2A 110.1 . . ?
C1 C2 H2A 110.1 . . ?
O2 C2 H2B 110.1 . . ?
C1 C2 H2B 110.1 . . ?
H2A C2 H2B 108.4 . . ?
O2 C3 C4 108.1(2) . . ?
O2 C3 H3A 110.1 . . ?
C4 C3 H3A 110.1 . . ?
O2 C3 H3B 110.1 . . ?
C4 C3 H3B 110.1 . . ?
H3A C3 H3B 108.4 . . ?
O3 C4 C3 107.9(2) . . ?
O3 C4 H4A 110.1 . . ?
C3 C4 H4A 110.1 . . ?
O3 C4 H4B 110.1 . . ?
C3 C4 H4B 110.1 . . ?
H4A C4 H4B 108.4 . . ?
O3 C5 C6 108.0(2) . . ?
O3 C5 H5A 110.1 . . ?
C6 C5 H5A 110.1 . . ?
O3 C5 H5B 110.1 . . ?
C6 C5 H5B 110.1 . . ?
H5A C5 H5B 108.4 . . ?
O4 C6 C5 108.9(2) . . ?
O4 C6 H6A 109.9 . . ?
C5 C6 H6A 109.9 . . ?
O4 C6 H6B 109.9 . . ?
C5 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
O4 C7 C8 109.3(2) . . ?
O4 C7 H7A 109.8 . . ?
C8 C7 H7A 109.8 . . ?
O4 C7 H7B 109.8 . . ?
C8 C7 H7B 109.8 . . ?
H7A C7 H7B 108.3 . . ?
O5 C8 C7 108.3(2) . . ?
O5 C8 H8A 110.0 . . ?
C7 C8 H8A 110.0 . . ?
O5 C8 H8B 110.0 . . ?
C7 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
O5 C9 C10 108.2(2) . . ?
O5 C9 H9A 110.1 . . ?
C10 C9 H9A 110.1 . . ?
O5 C9 H9B 110.1 . . ?
C10 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
O6 C10 C9 108.3(2) . . ?
O6 C10 H10A 110.0 . . ?
C9 C10 H10A 110.0 . . ?
O6 C10 H10B 110.0 . . ?
C9 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
O6 C11 C12 108.9(2) . . ?
O6 C11 H11A 109.9 . . ?
C12 C11 H11A 109.9 . . ?
O6 C11 H11B 109.9 . . ?
C12 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
O1 C12 C11 108.2(2) . . ?
O1 C12 H12A 110.1 . . ?
C11 C12 H12A 110.1 . . ?
O1 C12 H12B 110.1 . . ?
C11 C12 H12B 110.1 . . ?
H12A C12 H12B 108.4 . . ?
C20 C19 C18 103.4(4) . . ?
C18 C19 C90 97.4(4) . . ?
C20 C19 H19A 111.1 . . ?
C18 C19 H19A 111.1 . . ?
C20 C19 H19B 111.1 . . ?
C18 C19 H19B 111.1 . . ?
H19A C19 H19B 109.1 . . ?
C18 C19 H19C 112.3 . . ?
C90 C19 H19C 112.3 . . ?
C18 C19 H19D 112.3 . . ?
C90 C19 H19D 112.3 . . ?
H19C C19 H19D 109.9 . . ?
O7 C13 C14 106.2(3) . . ?
O7 C13 H13A 110.5 . . ?
C14 C13 H13A 110.5 . . ?
O7 C13 H13B 110.5 . . ?
C14 C13 H13B 110.5 . . ?
H13A C13 H13B 108.7 . . ?
C13 C14 C15 102.4(3) . . ?
C13 C14 H14A 111.3 . . ?
C15 C14 H14A 111.3 . . ?
C13 C14 H14B 111.3 . . ?
C15 C14 H14B 111.3 . . ?
H14A C14 H14B 109.2 . . ?
C14 C15 C16 102.7(3) . . ?
C14 C15 H15A 111.2 . . ?
C16 C15 H15A 111.2 . . ?
C14 C15 H15B 111.2 . . ?
C16 C15 H15B 111.2 . . ?
H15A C15 H15B 109.1 . . ?
C87 C18 C19 103.8(7) . . ?
C19 C18 C17 104.4(4) . . ?
C19 C18 H18A 110.9 . . ?
C17 C18 H18A 110.9 . . ?
C19 C18 H18B 110.9 . . ?
C17 C18 H18B 110.9 . . ?
H18A C18 H18B 108.9 . . ?
C87 C18 H18C 111.0 . . ?
C19 C18 H18C 111.0 . . ?
C87 C18 H18D 111.0 . . ?
C19 C18 H18D 111.0 . . ?
H18C C18 H18D 109.0 . . ?
O7 C16 C15 107.5(3) . . ?
O7 C16 H16A 110.2 . . ?
C15 C16 H16A 110.2 . . ?
O7 C16 H16B 110.2 . . ?
C15 C16 H16B 110.2 . . ?
H16A C16 H16B 108.5 . . ?
O8 C17 C18 97.6(4) . . ?
O8 C17 H17A 112.2 . . ?
C18 C17 H17A 112.2 . . ?
O8 C17 H17B 112.2 . . ?
C18 C17 H17B 112.2 . . ?
H17A C17 H17B 109.8 . . ?
C19 C20 O8 105.9(5) . . ?
C19 C20 H20A 110.6 . . ?
O8 C20 H20A 110.6 . . ?
C19 C20 H20B 110.6 . . ?
O8 C20 H20B 110.6 . . ?
H20A C20 H20B 108.7 . . ?
C18 C87 O8 115.2(10) . . ?
C18 C87 H87A 108.5 . . ?
O8 C87 H87A 108.5 . . ?
C18 C87 H87B 108.5 . . ?
O8 C87 H87B 108.5 . . ?
H87A C87 H87B 107.5 . . ?
O8 C90 C19 98.6(6) . . ?
O8 C90 H90A 112.1 . . ?
C19 C90 H90A 112.1 . . ?
O8 C90 H90B 112.1 . . ?
C19 C90 H90B 112.1 . . ?
H90A C90 H90B 109.7 . . ?
C22 C21 C39 118.9(2) . . ?
C22 C21 C38 121.6(2) . . ?
C39 C21 C38 119.4(2) . . ?
C23 C22 C21 121.0(3) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C24 C23 C22 121.4(3) . . ?
C24 C23 H23 119.3 . . ?
C22 C23 H23 119.3 . . ?
C23 C24 C25 120.2(3) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C26 C25 C24 121.7(3) . . ?
C26 C25 C39 119.0(2) . . ?
C24 C25 C39 119.3(3) . . ?
C27 C26 C25 120.3(3) . . ?
C27 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C28 C27 C26 121.2(3) . . ?
C28 C27 H27 119.4 . . ?
C26 C27 H27 119.4 . . ?
C27 C28 C29 121.6(3) . . ?
C27 C28 H28 119.2 . . ?
C29 C28 H28 119.2 . . ?
C28 C29 C39 118.2(2) . . ?
C28 C29 C30 122.6(2) . . ?
C39 C29 C30 119.2(2) . . ?
C31 C30 C40 118.0(2) . . ?
C31 C30 C29 122.4(2) . . ?
C40 C30 C29 119.5(2) . . ?
C32 C31 C30 121.8(3) . . ?
C32 C31 H31 119.1 . . ?
C30 C31 H31 119.1 . . ?
C33 C32 C31 121.1(3) . . ?
C33 C32 H32 119.5 . . ?
C31 C32 H32 119.5 . . ?
C32 C33 C34 120.4(3) . . ?
C32 C33 H33 119.8 . . ?
C34 C33 H33 119.8 . . ?
C35 C34 C33 122.1(3) . . ?
C35 C34 C40 118.8(3) . . ?
C33 C34 C40 119.1(3) . . ?
C36 C35 C34 120.8(3) . . ?
C36 C35 H35 119.6 . . ?
C34 C35 H35 119.6 . . ?
C35 C36 C37 121.2(3) . . ?
C35 C36 H36 119.4 . . ?
C37 C36 H36 119.4 . . ?
C36 C37 C38 121.0(3) . . ?
C36 C37 H37 119.5 . . ?
C38 C37 H37 119.5 . . ?
C37 C38 C40 118.5(2) . . ?
C37 C38 C21 122.2(2) . . ?
C40 C38 C21 119.2(2) . . ?
C21 C39 C29 121.2(2) . . ?
C21 C39 C25 119.2(2) . . ?
C29 C39 C25 119.6(2) . . ?
C30 C40 C38 121.1(2) . . ?
C30 C40 C34 119.3(2) . . ?
C38 C40 C34 119.6(2) . . ?
O9 C41 C42 108.6(2) . . ?
O9 C41 H41A 110.0 . . ?
C42 C41 H41A 110.0 . . ?
O9 C41 H41B 110.0 . . ?
C42 C41 H41B 110.0 . . ?
H41A C41 H41B 108.4 . . ?
O10 C42 C41 108.2(2) . . ?
O10 C42 H42A 110.1 . . ?
C41 C42 H42A 110.1 . . ?
O10 C42 H42B 110.1 . . ?
C41 C42 H42B 110.1 . . ?
H42A C42 H42B 108.4 . . ?
O10 C43 C44 107.9(2) . . ?
O10 C43 H43A 110.1 . . ?
C44 C43 H43A 110.1 . . ?
O10 C43 H43B 110.1 . . ?
C44 C43 H43B 110.1 . . ?
H43A C43 H43B 108.4 . . ?
O11 C44 C43 109.7(2) . . ?
O11 C44 H44A 109.7 . . ?
C43 C44 H44A 109.7 . . ?
O11 C44 H44B 109.7 . . ?
C43 C44 H44B 109.7 . . ?
H44A C44 H44B 108.2 . . ?
O11 C45 C46 108.8(2) . . ?
O11 C45 H45A 109.9 . . ?
C46 C45 H45A 109.9 . . ?
O11 C45 H45B 109.9 . . ?
C46 C45 H45B 109.9 . . ?
H45A C45 H45B 108.3 . . ?
O12 C46 C45 109.1(2) . . ?
O12 C46 H46A 109.9 . . ?
C45 C46 H46A 109.9 . . ?
O12 C46 H46B 109.9 . . ?
C45 C46 H46B 109.9 . . ?
H46A C46 H46B 108.3 . . ?
O12 C47 C48 107.9(2) . . ?
O12 C47 H47A 110.1 . . ?
C48 C47 H47A 110.1 . . ?
O12 C47 H47B 110.1 . . ?
C48 C47 H47B 110.1 . . ?
H47A C47 H47B 108.4 . . ?
O13 C48 C47 108.6(2) . . ?
O13 C48 H48A 110.0 . . ?
C47 C48 H48A 110.0 . . ?
O13 C48 H48B 110.0 . . ?
C47 C48 H48B 110.0 . . ?
H48A C48 H48B 108.3 . . ?
O13 C49 C50 108.8(2) . . ?
O13 C49 H49A 109.9 . . ?
C50 C49 H49A 109.9 . . ?
O13 C49 H49B 109.9 . . ?
C50 C49 H49B 109.9 . . ?
H49A C49 H49B 108.3 . . ?
O14 C50 C49 108.9(2) . . ?
O14 C50 H50A 109.9 . . ?
C49 C50 H50A 109.9 . . ?
O14 C50 H50B 109.9 . . ?
C49 C50 H50B 109.9 . . ?
H50A C50 H50B 108.3 . . ?
O14 C51 C52 109.1(2) . . ?
O14 C51 H51A 109.9 . . ?
C52 C51 H51A 109.9 . . ?
O14 C51 H51B 109.9 . . ?
C52 C51 H51B 109.9 . . ?
H51A C51 H51B 108.3 . . ?
O9 C52 C51 109.8(2) . . ?
O9 C52 H52A 109.7 . . ?
C51 C52 H52A 109.7 . . ?
O9 C52 H52B 109.7 . . ?
C51 C52 H52B 109.7 . . ?
H52A C52 H52B 108.2 . . ?
O15 C53 C54 103.5(2) . . ?
O15 C53 H53A 111.1 . . ?
C54 C53 H53A 111.1 . . ?
O15 C53 H53B 111.1 . . ?
C54 C53 H53B 111.1 . . ?
H53A C53 H53B 109.0 . . ?
C53 C54 C55 103.4(2) . . ?
C53 C54 H54A 111.1 . . ?
C55 C54 H54A 111.1 . . ?
C53 C54 H54B 111.1 . . ?
C55 C54 H54B 111.1 . . ?
H54A C54 H54B 109.0 . . ?
C56 C55 C54 103.8(2) . . ?
C56 C55 H55A 111.0 . . ?
C54 C55 H55A 111.0 . . ?
C56 C55 H55B 111.0 . . ?
C54 C55 H55B 111.0 . . ?
H55A C55 H55B 109.0 . . ?
O15 C56 C55 106.5(3) . . ?
O15 C56 H56A 110.4 . . ?
C55 C56 H56A 110.4 . . ?
O15 C56 H56B 110.4 . . ?
C55 C56 H56B 110.4 . . ?
H56A C56 H56B 108.6 . . ?
O16 C57 C58 106.9(3) . . ?
O16 C57 H57A 110.3 . . ?
C58 C57 H57A 110.3 . . ?
O16 C57 H57B 110.3 . . ?
C58 C57 H57B 110.3 . . ?
H57A C57 H57B 108.6 . . ?
C57 C58 C59 104.0(3) . . ?
C57 C58 H58A 111.0 . . ?
C59 C58 H58A 111.0 . . ?
C57 C58 H58B 111.0 . . ?
C59 C58 H58B 111.0 . . ?
H58A C58 H58B 109.0 . . ?
C60 C59 C58 103.6(3) . . ?
C60 C59 H59A 111.0 . . ?
C58 C59 H59A 111.0 . . ?
C60 C59 H59B 111.0 . . ?
C58 C59 H59B 111.0 . . ?
H59A C59 H59B 109.0 . . ?
O16 C60 C59 105.5(3) . . ?
O16 C60 H60A 110.6 . . ?
C59 C60 H60A 110.6 . . ?
O16 C60 H60B 110.6 . . ?
C59 C60 H60B 110.6 . . ?
H60A C60 H60B 108.8 . . ?
C62 C61 C79 118.2(3) . . ?
C62 C61 C78 122.3(3) . . ?
C79 C61 C78 119.5(2) . . ?
C63 C62 C61 121.1(3) . . ?
C63 C62 H62 119.4 . . ?
C61 C62 H62 119.4 . . ?
C64 C63 C62 121.3(3) . . ?
C64 C63 H63 119.4 . . ?
C62 C63 H63 119.4 . . ?
C63 C64 C65 120.9(3) . . ?
C63 C64 H64 119.6 . . ?
C65 C64 H64 119.6 . . ?
C66 C65 C64 121.9(3) . . ?
C66 C65 C79 119.6(3) . . ?
C64 C65 C79 118.4(3) . . ?
C67 C66 C65 120.5(3) . . ?
C67 C66 H66 119.8 . . ?
C65 C66 H66 119.8 . . ?
C66 C67 C68 121.0(3) . . ?
C66 C67 H67 119.5 . . ?
C68 C67 H67 119.5 . . ?
C67 C68 C69 121.5(3) . . ?
C67 C68 H68 119.2 . . ?
C69 C68 H68 119.2 . . ?
C68 C69 C79 118.3(3) . . ?
C68 C69 C70 122.3(2) . . ?
C79 C69 C70 119.3(2) . . ?
C71 C70 C80 118.3(3) . . ?
C71 C70 C69 121.9(3) . . ?
C80 C70 C69 119.7(2) . . ?
C72 C71 C70 121.4(3) . . ?
C72 C71 H71 119.3 . . ?
C70 C71 H71 119.3 . . ?
C71 C72 C73 121.3(3) . . ?
C71 C72 H72 119.4 . . ?
C73 C72 H72 119.4 . . ?
C72 C73 C74 120.2(3) . . ?
C72 C73 H73 119.9 . . ?
C74 C73 H73 119.9 . . ?
C75 C74 C73 121.5(3) . . ?
C75 C74 C80 119.4(3) . . ?
C73 C74 C80 119.0(3) . . ?
C76 C75 C74 120.3(3) . . ?
C76 C75 H75 119.9 . . ?
C74 C75 H75 119.9 . . ?
C75 C76 C77 120.9(3) . . ?
C75 C76 H76 119.6 . . ?
C77 C76 H76 119.6 . . ?
C76 C77 C78 121.6(3) . . ?
C76 C77 H77 119.2 . . ?
C78 C77 H77 119.2 . . ?
C77 C78 C80 118.3(3) . . ?
C77 C78 C61 122.0(2) . . ?
C80 C78 C61 119.7(2) . . ?
C61 C79 C69 120.9(3) . . ?
C61 C79 C65 120.0(2) . . ?
C69 C79 C65 119.0(3) . . ?
C70 C80 C78 120.8(2) . . ?
C70 C80 C74 119.8(2) . . ?
C78 C80 C74 119.4(2) . . ?

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
C12 O1 C1 C2 179.4(2) . . . . ?
K1 O1 C1 C2 -49.0(2) . . . . ?
C3 O2 C2 C1 174.4(2) . . . . ?
K1 O2 C2 C1 -54.2(2) . . . . ?
O1 C1 C2 O2 71.0(3) . . . . ?
C2 O2 C3 C4 176.9(2) . . . . ?
K1 O2 C3 C4 48.1(3) . . . . ?
C5 O3 C4 C3 -180.0(2) . . . . ?
K1 O3 C4 C3 54.5(2) . . . . ?
O2 C3 C4 O3 -69.3(3) . . . . ?
C4 O3 C5 C6 -179.5(2) . . . . ?
K1 O3 C5 C6 -53.5(2) . . . . ?
C7 O4 C6 C5 -178.0(2) . . . . ?
K1 O4 C6 C5 -48.2(2) . . . . ?
O3 C5 C6 O4 69.3(3) . . . . ?
C6 O4 C7 C8 -174.7(2) . . . . ?
K1 O4 C7 C8 54.2(2) . . . . ?
C9 O5 C8 C7 177.8(2) . . . . ?
K1 O5 C8 C7 47.6(2) . . . . ?
O4 C7 C8 O5 -69.7(3) . . . . ?
C8 O5 C9 C10 178.6(2) . . . . ?
K1 O5 C9 C10 -52.5(3) . . . . ?
C11 O6 C10 C9 -179.7(2) . . . . ?
K1 O6 C10 C9 -46.8(3) . . . . ?
O5 C9 C10 O6 65.6(3) . . . . ?
C10 O6 C11 C12 -179.5(2) . . . . ?
K1 O6 C11 C12 46.1(3) . . . . ?
C1 O1 C12 C11 -175.6(2) . . . . ?
K1 O1 C12 C11 53.7(3) . . . . ?
O6 C11 C12 O1 -66.8(3) . . . . ?
C16 O7 C13 C14 -22.5(5) . . . . ?
K1 O7 C13 C14 172.1(2) . . . . ?
O7 C13 C14 C15 34.5(4) . . . . ?
C13 C14 C15 C16 -32.7(4) . . . . ?
C90 C19 C18 C87 42.7(11) . . . . ?
C20 C19 C18 C17 -36.3(8) . . . . ?
C13 O7 C16 C15 0.8(5) . . . . ?
K1 O7 C16 C15 163.5(2) . . . . ?
C14 C15 C16 O7 20.4(5) . . . . ?
C20 O8 C17 C18 -32.6(8) . . . . ?
K1 O8 C17 C18 137.3(3) . . . . ?
C19 C18 C17 O8 42.3(5) . . . . ?
C18 C19 C20 O8 16.1(10) . . . . ?
C17 O8 C20 C19 12.2(11) . . . . ?
K1 O8 C20 C19 -152.5(4) . . . . ?
C19 C18 C87 O8 -43.2(13) . . . . ?
C90 O8 C87 C18 21.9(16) . . . . ?
K1 O8 C87 C18 -164.7(11) . . . . ?
C87 O8 C90 C19 8.4(10) . . . . ?
K1 O8 C90 C19 -161.0(6) . . . . ?
C18 C19 C90 O8 -28.0(8) . . . . ?
C39 C21 C22 C23 1.6(4) . . . . ?
C38 C21 C22 C23 -175.4(2) . . . . ?
C21 C22 C23 C24 -0.8(4) . . . . ?
C22 C23 C24 C25 -0.5(4) . . . . ?
C23 C24 C25 C26 -179.9(3) . . . . ?
C23 C24 C25 C39 0.8(4) . . . . ?
C24 C25 C26 C27 -178.0(3) . . . . ?
C39 C25 C26 C27 1.2(4) . . . . ?
C25 C26 C27 C28 -1.1(4) . . . . ?
C26 C27 C28 C29 -0.2(4) . . . . ?
C27 C28 C29 C39 1.3(4) . . . . ?
C27 C28 C29 C30 -179.4(3) . . . . ?
C28 C29 C30 C31 7.1(4) . . . . ?
C39 C29 C30 C31 -173.6(2) . . . . ?
C28 C29 C30 C40 -173.7(2) . . . . ?
C39 C29 C30 C40 5.7(4) . . . . ?
C40 C30 C31 C32 3.9(4) . . . . ?
C29 C30 C31 C32 -176.8(3) . . . . ?
C30 C31 C32 C33 0.7(5) . . . . ?
C31 C32 C33 C34 -3.2(4) . . . . ?
C32 C33 C34 C35 -177.9(3) . . . . ?
C32 C33 C34 C40 0.8(4) . . . . ?
C33 C34 C35 C36 177.4(3) . . . . ?
C40 C34 C35 C36 -1.4(4) . . . . ?
C34 C35 C36 C37 -0.9(4) . . . . ?
C35 C36 C37 C38 1.9(4) . . . . ?
C36 C37 C38 C40 -0.5(4) . . . . ?
C36 C37 C38 C21 176.8(3) . . . . ?
C22 C21 C38 C37 3.1(4) . . . . ?
C39 C21 C38 C37 -173.9(2) . . . . ?
C22 C21 C38 C40 -179.5(2) . . . . ?
C39 C21 C38 C40 3.4(4) . . . . ?
C22 C21 C39 C29 179.7(2) . . . . ?
C38 C21 C39 C29 -3.2(4) . . . . ?
C22 C21 C39 C25 -1.2(4) . . . . ?
C38 C21 C39 C25 175.9(2) . . . . ?
C28 C29 C39 C21 178.0(2) . . . . ?
C30 C29 C39 C21 -1.4(4) . . . . ?
C28 C29 C39 C25 -1.1(4) . . . . ?
C30 C29 C39 C25 179.6(2) . . . . ?
C26 C25 C39 C21 -179.3(2) . . . . ?
C24 C25 C39 C21 0.0(4) . . . . ?
C26 C25 C39 C29 -0.2(4) . . . . ?
C24 C25 C39 C29 179.1(2) . . . . ?
C31 C30 C40 C38 173.8(2) . . . . ?
C29 C30 C40 C38 -5.5(4) . . . . ?
C31 C30 C40 C34 -6.1(4) . . . . ?
C29 C30 C40 C34 174.6(2) . . . . ?
C37 C38 C40 C30 178.3(2) . . . . ?
C21 C38 C40 C30 0.9(4) . . . . ?
C37 C38 C40 C34 -1.7(4) . . . . ?
C21 C38 C40 C34 -179.2(2) . . . . ?
C35 C34 C40 C30 -177.4(2) . . . . ?
C33 C34 C40 C30 3.8(4) . . . . ?
C35 C34 C40 C38 2.7(4) . . . . ?
C33 C34 C40 C38 -176.1(2) . . . . ?
C52 O9 C41 C42 -174.4(2) . . . . ?
K2 O9 C41 C42 -45.8(3) . . . . ?
C43 O10 C42 C41 174.7(2) . . . . ?
K2 O10 C42 C41 -52.5(3) . . . . ?
O9 C41 C42 O10 65.2(3) . . . . ?
C42 O10 C43 C44 -179.4(2) . . . . ?
K2 O10 C43 C44 47.7(3) . . . . ?
C45 O11 C44 C43 -177.6(2) . . . . ?
K2 O11 C44 C43 50.5(3) . . . . ?
O10 C43 C44 O11 -65.8(3) . . . . ?
C44 O11 C45 C46 178.9(2) . . . . ?
K2 O11 C45 C46 -48.8(3) . . . . ?
C47 O12 C46 C45 -179.3(2) . . . . ?
K2 O12 C46 C45 -52.6(3) . . . . ?
O11 C45 C46 O12 69.7(3) . . . . ?
C46 O12 C47 C48 -176.3(2) . . . . ?
K2 O12 C47 C48 58.0(2) . . . . ?
C49 O13 C48 C47 172.7(2) . . . . ?
K2 O13 C48 C47 40.0(3) . . . . ?
O12 C47 C48 O13 -64.7(3) . . . . ?
C48 O13 C49 C50 173.5(2) . . . . ?
K2 O13 C49 C50 -51.1(2) . . . . ?
C51 O14 C50 C49 179.7(2) . . . . ?
K2 O14 C50 C49 -47.9(3) . . . . ?
O13 C49 C50 O14 66.8(3) . . . . ?
C50 O14 C51 C52 -175.9(2) . . . . ?
K2 O14 C51 C52 50.4(3) . . . . ?
C41 O9 C52 C51 179.7(2) . . . . ?
K2 O9 C52 C51 48.8(3) . . . . ?
O14 C51 C52 O9 -68.0(3) . . . . ?
C56 O15 C53 C54 -42.4(3) . . . . ?
K2 O15 C53 C54 170.4(2) . . . . ?
O15 C53 C54 C55 34.3(3) . . . . ?
C53 C54 C55 C56 -14.3(3) . . . . ?
C53 O15 C56 C55 33.2(4) . . . . ?
K2 O15 C56 C55 -175.1(2) . . . . ?
C54 C55 C56 O15 -10.5(4) . . . . ?
C60 O16 C57 C58 -32.6(4) . . . . ?
K2 O16 C57 C58 -172.5(2) . . . . ?
O16 C57 C58 C59 12.9(4) . . . . ?
C57 C58 C59 C60 9.8(4) . . . . ?
C57 O16 C60 C59 39.2(4) . . . . ?
K2 O16 C60 C59 176.8(2) . . . . ?
C58 C59 C60 O16 -29.9(4) . . . . ?
C79 C61 C62 C63 -1.0(4) . . . . ?
C78 C61 C62 C63 178.7(3) . . . . ?
C61 C62 C63 C64 0.4(4) . . . . ?
C62 C63 C64 C65 0.2(4) . . . . ?
C63 C64 C65 C66 179.5(3) . . . . ?
C63 C64 C65 C79 -0.2(4) . . . . ?
C64 C65 C66 C67 -179.3(3) . . . . ?
C79 C65 C66 C67 0.5(4) . . . . ?
C65 C66 C67 C68 0.1(4) . . . . ?
C66 C67 C68 C69 -1.2(4) . . . . ?
C67 C68 C69 C79 1.7(4) . . . . ?
C67 C68 C69 C70 -175.8(3) . . . . ?
C68 C69 C70 C71 3.4(4) . . . . ?
C79 C69 C70 C71 -174.1(2) . . . . ?
C68 C69 C70 C80 -179.6(2) . . . . ?
C79 C69 C70 C80 2.9(4) . . . . ?
C80 C70 C71 C72 0.2(4) . . . . ?
C69 C70 C71 C72 177.2(2) . . . . ?
C70 C71 C72 C73 1.1(4) . . . . ?
C71 C72 C73 C74 -0.8(4) . . . . ?
C72 C73 C74 C75 179.8(3) . . . . ?
C72 C73 C74 C80 -0.8(4) . . . . ?
C73 C74 C75 C76 179.0(3) . . . . ?
C80 C74 C75 C76 -0.3(4) . . . . ?
C74 C75 C76 C77 -1.5(4) . . . . ?
C75 C76 C77 C78 1.0(4) . . . . ?
C76 C77 C78 C80 1.5(4) . . . . ?
C76 C77 C78 C61 -178.3(3) . . . . ?
C62 C61 C78 C77 1.8(4) . . . . ?
C79 C61 C78 C77 -178.5(2) . . . . ?
C62 C61 C78 C80 -177.9(2) . . . . ?
C79 C61 C78 C80 1.7(4) . . . . ?
C62 C61 C79 C69 -179.2(2) . . . . ?
C78 C61 C79 C69 1.1(4) . . . . ?
C62 C61 C79 C65 0.9(4) . . . . ?
C78 C61 C79 C65 -178.8(2) . . . . ?
C68 C69 C79 C61 179.0(2) . . . . ?
C70 C69 C79 C61 -3.4(4) . . . . ?
C68 C69 C79 C65 -1.1(4) . . . . ?
C70 C69 C79 C65 176.5(2) . . . . ?
C66 C65 C79 C61 179.9(2) . . . . ?
C64 C65 C79 C61 -0.3(4) . . . . ?
C66 C65 C79 C69 0.1(4) . . . . ?
C64 C65 C79 C69 179.8(2) . . . . ?
C71 C70 C80 C78 176.9(2) . . . . ?
C69 C70 C80 C78 -0.1(4) . . . . ?
C71 C70 C80 C74 -1.8(4) . . . . ?
C69 C70 C80 C74 -178.9(2) . . . . ?
C77 C78 C80 C70 178.0(2) . . . . ?
C61 C78 C80 C70 -2.2(4) . . . . ?
C77 C78 C80 C74 -3.2(4) . . . . ?
C61 C78 C80 C74 176.5(2) . . . . ?
C75 C74 C80 C70 -178.5(2) . . . . ?
C73 C74 C80 C70 2.1(4) . . . . ?
C75 C74 C80 C78 2.7(4) . . . . ?
C73 C74 C80 C78 -176.7(2) . . . . ?

_refine_diff_density_max         0.841
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.072

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_1027SF_0mS_a
_database_code_depnum_ccdc_archive 'CCDC 1431122'
_audit_update_record             
;
2015-10-13 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H34 Li O8, 1.5 (C20 H12)'
_chemical_formula_sum            'C46 H52 Li O8'
_chemical_formula_weight         739.81

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'
Li Li -0.0003 0.0001 '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'

_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                   8.3174(5)
_cell_length_b                   12.2288(8)
_cell_length_c                   20.1448(13)
_cell_angle_alpha                104.2740(10)
_cell_angle_beta                 99.6340(10)
_cell_angle_gamma                97.9080(10)
_cell_volume                     1923.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1980
_cell_measurement_theta_min      2.356
_cell_measurement_theta_max      27.12

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_F_000             790
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    0.086
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6717
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus tube'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22988
_diffrn_reflns_av_unetI/netI     0.1125
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.067
_diffrn_reflns_theta_max         28.396
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9534
_reflns_number_gt                5153
_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-2014/6 (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)+(0.0536P)²+0.3369P] 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_number_reflns         9534
_refine_ls_number_parameters     498
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1440
_refine_ls_R_factor_gt           0.0635
_refine_ls_wR_factor_ref         0.1438
_refine_ls_wR_factor_gt          0.1123
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_restrained_S_all      0.976
_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
Li1 Li 0.4433(5) 0.5787(3) 0.76413(19) 0.0221(9) Uani 1 1 d . . . . .
O1 O 0.3881(2) 0.70013(13) 0.71163(8) 0.0218(4) Uani 1 1 d . . . . .
O2 O 0.6224(2) 0.72135(13) 0.82624(7) 0.0205(4) Uani 1 1 d . . . . .
O3 O 0.52626(19) 0.52428(13) 0.85183(7) 0.0185(4) Uani 1 1 d . . . . .
O4 O 0.3371(2) 0.41718(13) 0.93254(7) 0.0203(4) Uani 1 1 d . . . . .
O5 O 0.0430(2) 0.50277(13) 0.86877(8) 0.0236(4) Uani 1 1 d . . . . .
O6 O 0.1855(2) 0.66925(13) 0.80540(8) 0.0220(4) Uani 1 1 d . . . . .
O7 O 0.5920(2) 0.51406(14) 0.69905(8) 0.0248(4) Uani 1 1 d . . . . .
O8 O 0.2833(2) 0.43260(13) 0.70566(7) 0.0237(4) Uani 1 1 d . . . . .
C1 C 0.5161(3) 0.8006(2) 0.73682(12) 0.0261(6) Uani 1 1 d . . . . .
H1A H 0.4715 0.8671 0.7267 0.031 Uiso 1 1 calc R U . . .
H1B H 0.6083 0.7890 0.7121 0.031 Uiso 1 1 calc R U . . .
C2 C 0.5810(3) 0.8257(2) 0.81474(12) 0.0280(6) Uani 1 1 d . . . . .
H2A H 0.6803 0.8878 0.8305 0.034 Uiso 1 1 calc R U . . .
H2B H 0.4951 0.8498 0.8408 0.034 Uiso 1 1 calc R U . . .
C3 C 0.6482(3) 0.7204(2) 0.89768(11) 0.0224(6) Uani 1 1 d . . . . .
H3A H 0.5524 0.7415 0.9178 0.027 Uiso 1 1 calc R U . . .
H3B H 0.7494 0.7761 0.9252 0.027 Uiso 1 1 calc R U . . .
C4 C 0.6672(3) 0.60109(19) 0.89960(11) 0.0212(5) Uani 1 1 d . . . . .
H4A H 0.7711 0.5837 0.8853 0.025 Uiso 1 1 calc R U . . .
H4B H 0.6711 0.5932 0.9476 0.025 Uiso 1 1 calc R U . . .
C5 C 0.5244(3) 0.40597(19) 0.85067(11) 0.0212(5) Uani 1 1 d . . . . .
H5A H 0.6342 0.3870 0.8451 0.025 Uiso 1 1 calc R U . . .
H5B H 0.4405 0.3563 0.8097 0.025 Uiso 1 1 calc R U . . .
C6 C 0.4851(3) 0.3806(2) 0.91665(11) 0.0208(5) Uani 1 1 d . . . . .
H6A H 0.4729 0.2969 0.9109 0.025 Uiso 1 1 calc R U . . .
H6B H 0.5791 0.4197 0.9564 0.025 Uiso 1 1 calc R U . . .
C7 C 0.1870(3) 0.3474(2) 0.88894(12) 0.0251(6) Uani 1 1 d . . . . .
H7A H 0.1661 0.2735 0.9008 0.030 Uiso 1 1 calc R U . . .
H7B H 0.1959 0.3309 0.8392 0.030 Uiso 1 1 calc R U . . .
C8 C 0.0473(3) 0.4106(2) 0.90036(13) 0.0274(6) Uani 1 1 d . . . . .
H8A H -0.0590 0.3553 0.8815 0.033 Uiso 1 1 calc R U . . .
H8B H 0.0563 0.4415 0.9514 0.033 Uiso 1 1 calc R U . . .
C9 C 0.1596(3) 0.60522(19) 0.90680(11) 0.0211(5) Uani 1 1 d . . . . .
H9A H 0.2742 0.5905 0.9087 0.025 Uiso 1 1 calc R U . . .
H9B H 0.1430 0.6303 0.9554 0.025 Uiso 1 1 calc R U . . .
C10 C 0.1345(3) 0.6969(2) 0.87077(11) 0.0224(6) Uani 1 1 d . . . . .
H10A H 0.0159 0.7034 0.8627 0.027 Uiso 1 1 calc R U . . .
H10B H 0.2002 0.7718 0.9008 0.027 Uiso 1 1 calc R U . . .
C11 C 0.1633(3) 0.7552(2) 0.76971(12) 0.0241(6) Uani 1 1 d . . . . .
H11A H 0.2282 0.8307 0.7990 0.029 Uiso 1 1 calc R U . . .
H11B H 0.0447 0.7613 0.7600 0.029 Uiso 1 1 calc R U . . .
C12 C 0.2220(3) 0.7210(2) 0.70217(12) 0.0255(6) Uani 1 1 d . . . . .
H12A H 0.1466 0.6506 0.6711 0.031 Uiso 1 1 calc R U . . .
H12B H 0.2153 0.7827 0.6785 0.031 Uiso 1 1 calc R U . . .
C13 C 0.5217(3) 0.3978(2) 0.66153(12) 0.0258(6) Uani 1 1 d . . . . .
H13A H 0.5479 0.3462 0.6911 0.031 Uiso 1 1 calc R U . . .
H13B H 0.5671 0.3749 0.6188 0.031 Uiso 1 1 calc R U . . .
C14 C 0.3393(3) 0.3898(2) 0.64236(11) 0.0275(6) Uani 1 1 d . . . . .
H14A H 0.3127 0.4361 0.6095 0.033 Uiso 1 1 calc R U . . .
H14B H 0.2841 0.3090 0.6194 0.033 Uiso 1 1 calc R U . . .
C15 C 0.7680(3) 0.5313(3) 0.71861(13) 0.0350(7) Uani 1 1 d . . . . .
H15A H 0.7990 0.4821 0.7485 0.052 Uiso 1 1 calc R U . . .
H15B H 0.8119 0.6120 0.7444 0.052 Uiso 1 1 calc R U . . .
H15C H 0.8142 0.5117 0.6765 0.052 Uiso 1 1 calc R U . . .
C16 C 0.1116(3) 0.3940(2) 0.69875(13) 0.0329(7) Uani 1 1 d . . . . .
H16A H 0.0493 0.4151 0.6595 0.049 Uiso 1 1 calc R U . . .
H16B H 0.0776 0.4298 0.7420 0.049 Uiso 1 1 calc R U . . .
H16C H 0.0890 0.3103 0.6899 0.049 Uiso 1 1 calc R U . . .
C17 C 0.5550(3) 0.11499(18) 0.74117(11) 0.0148(5) Uani 1 1 d . . . . .
C18 C 0.7010(3) 0.14165(19) 0.71748(11) 0.0196(5) Uani 1 1 d . . . . .
H18 H 0.8048 0.1596 0.7496 0.023 Uiso 1 1 calc R U . . .
C19 C 0.6978(3) 0.14247(19) 0.64839(11) 0.0214(5) Uani 1 1 d . . . . .
H19 H 0.7990 0.1603 0.6339 0.026 Uiso 1 1 calc R U . . .
C20 C 0.5493(3) 0.11768(19) 0.60069(11) 0.0210(5) Uani 1 1 d . . . . .
H20 H 0.5492 0.1167 0.5534 0.025 Uiso 1 1 calc R U . . .
C21 C 0.3974(3) 0.09372(19) 0.62117(11) 0.0188(5) Uani 1 1 d . . . . .
C22 C 0.2439(3) 0.0728(2) 0.57385(11) 0.0229(6) Uani 1 1 d . . . . .
H22 H 0.2419 0.0735 0.5267 0.028 Uiso 1 1 calc R U . . .
C23 C 0.0969(3) 0.0514(2) 0.59537(11) 0.0243(6) Uani 1 1 d . . . . .
H23 H -0.0055 0.0391 0.5631 0.029 Uiso 1 1 calc R U . . .
C24 C 0.0964(3) 0.04764(19) 0.66364(11) 0.0202(5) Uani 1 1 d . . . . .
H24 H -0.0067 0.0321 0.6771 0.024 Uiso 1 1 calc R U . . .
C25 C 0.2446(3) 0.06617(18) 0.71336(10) 0.0156(5) Uani 1 1 d . . . . .
C26 C 0.2459(3) 0.06023(18) 0.78457(10) 0.0149(5) Uani 1 1 d . . . . .
C27 C 0.0982(3) 0.03290(18) 0.80797(11) 0.0187(5) Uani 1 1 d . . . . .
H27 H -0.0057 0.0186 0.7764 0.022 Uiso 1 1 calc R U . . .
C28 C 0.1019(3) 0.02656(19) 0.87595(11) 0.0194(5) Uani 1 1 d . . . . .
H28 H 0.0006 0.0079 0.8901 0.023 Uiso 1 1 calc R U . . .
C29 C 0.2507(3) 0.04693(18) 0.92348(11) 0.0185(5) Uani 1 1 d . . . . .
H29 H 0.2507 0.0416 0.9697 0.022 Uiso 1 1 calc R U . . .
C30 C 0.4028(3) 0.07569(18) 0.90377(11) 0.0165(5) Uani 1 1 d . . . . .
C31 C 0.5571(3) 0.10027(18) 0.95178(11) 0.0176(5) Uani 1 1 d . . . . .
H31 H 0.5594 0.0975 0.9986 0.021 Uiso 1 1 calc R U . . .
C32 C 0.7039(3) 0.12816(18) 0.93137(11) 0.0187(5) Uani 1 1 d . . . . .
H32 H 0.8059 0.1445 0.9644 0.022 Uiso 1 1 calc R U . . .
C33 C 0.7051(3) 0.13274(18) 0.86321(11) 0.0173(5) Uani 1 1 d . . . . .
H33 H 0.8080 0.1511 0.8503 0.021 Uiso 1 1 calc R U . . .
C34 C 0.5553(3) 0.11045(18) 0.81268(11) 0.0157(5) Uani 1 1 d . . . . .
C35 C 0.3989(3) 0.09150(18) 0.69265(10) 0.0155(5) Uani 1 1 d . . . . .
C36 C 0.4018(3) 0.08188(18) 0.83298(10) 0.0141(5) Uani 1 1 d . . . . .
C37 C 0.6565(3) 0.5769(2) 0.53360(11) 0.0211(6) Uani 1 1 d . . . . .
C38 C 0.8043(3) 0.6533(2) 0.56466(12) 0.0268(6) Uani 1 1 d . . . . .
H38 H 0.9051 0.6248 0.5682 0.032 Uiso 1 1 calc R U . . .
C39 C 0.8100(4) 0.7711(2) 0.59106(12) 0.0329(7) Uani 1 1 d . . . . .
H39 H 0.9138 0.8209 0.6123 0.039 Uiso 1 1 calc R U . . .
C40 C 0.6679(4) 0.8146(2) 0.58652(12) 0.0303(7) Uani 1 1 d . . . . .
H40 H 0.6730 0.8948 0.6047 0.036 Uiso 1 1 calc R U . . .
C41 C 0.5127(3) 0.7416(2) 0.55498(11) 0.0244(6) Uani 1 1 d . . . . .
C42 C 0.3641(3) 0.7856(2) 0.54869(12) 0.0290(6) Uani 1 1 d . . . . .
H42 H 0.3674 0.8654 0.5674 0.035 Uiso 1 1 calc R U . . .
C43 C 0.2157(4) 0.7142(2) 0.51585(13) 0.0308(6) Uani 1 1 d . . . . .
H43 H 0.1169 0.7449 0.5112 0.037 Uiso 1 1 calc R U . . .
C44 C 0.2084(3) 0.5963(2) 0.48911(12) 0.0275(6) Uani 1 1 d . . . . .
H44 H 0.1040 0.5482 0.4665 0.033 Uiso 1 1 calc R U . . .
C45 C 0.3492(3) 0.5477(2) 0.49468(11) 0.0205(5) Uani 1 1 d . . . . .
C46 C 0.5064(3) 0.6212(2) 0.52789(11) 0.0215(6) Uani 1 1 d . . . . .


_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
Li1 O8 2.034(4) . ?
Li1 O7 2.043(4) . ?
Li1 O1 2.082(4) . ?
Li1 O3 2.083(4) . ?
Li1 O2 2.100(4) . ?
O1 C12 1.429(3) . ?
O1 C1 1.433(3) . ?
O2 C3 1.422(2) . ?
O2 C2 1.429(3) . ?
O3 C4 1.434(3) . ?
O3 C5 1.439(3) . ?
O4 C7 1.424(3) . ?
O4 C6 1.425(3) . ?
O5 C8 1.427(3) . ?
O5 C9 1.429(3) . ?
O6 C10 1.427(3) . ?
O6 C11 1.427(3) . ?
O7 C15 1.422(3) . ?
O7 C13 1.424(3) . ?
O8 C16 1.413(3) . ?
O8 C14 1.433(3) . ?
C1 C2 1.511(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.498(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.514(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.500(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.498(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.504(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.484(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.404(3) . ?
C17 C35 1.434(3) . ?
C17 C34 1.455(3) . ?
C18 C19 1.390(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.378(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.408(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.409(3) . ?
C21 C35 1.445(3) . ?
C22 C23 1.378(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.388(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.404(3) . ?
C24 H24 0.9500 . ?
C25 C35 1.432(3) . ?
C25 C26 1.452(3) . ?
C26 C27 1.414(3) . ?
C26 C36 1.434(3) . ?
C27 C28 1.386(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.383(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.413(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.417(3) . ?
C30 C36 1.445(3) . ?
C31 C32 1.378(3) . ?
C31 H31 0.9500 . ?
C32 C33 1.390(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.417(3) . ?
C33 H33 0.9500 . ?
C34 C36 1.429(3) . ?
C37 C38 1.383(3) . ?
C37 C46 1.425(3) . ?
C37 C45 1.481(3) 2_666 ?
C38 C39 1.398(3) . ?
C38 H38 0.9500 . ?
C39 C40 1.361(4) . ?
C39 H39 0.9500 . ?
C40 C41 1.413(3) . ?
C40 H40 0.9500 . ?
C41 C42 1.413(4) . ?
C41 C46 1.429(3) . ?
C42 C43 1.367(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.398(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.385(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.432(3) . ?
C45 C37 1.481(3) 2_666 ?

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
O8 Li1 O7 81.49(15) . . ?
O8 Li1 O1 103.63(18) . . ?
O7 Li1 O1 93.59(17) . . ?
O8 Li1 O3 98.78(18) . . ?
O7 Li1 O3 101.29(19) . . ?
O1 Li1 O3 154.7(2) . . ?
O8 Li1 O2 175.4(2) . . ?
O7 Li1 O2 95.85(18) . . ?
O1 Li1 O2 80.20(15) . . ?
O3 Li1 O2 78.02(14) . . ?
C12 O1 C1 115.49(18) . . ?
C12 O1 Li1 117.85(18) . . ?
C1 O1 Li1 110.01(17) . . ?
C3 O2 C2 113.91(17) . . ?
C3 O2 Li1 110.20(17) . . ?
C2 O2 Li1 111.10(17) . . ?
C4 O3 C5 113.06(17) . . ?
C4 O3 Li1 113.53(17) . . ?
C5 O3 Li1 124.12(16) . . ?
C7 O4 C6 114.94(17) . . ?
C8 O5 C9 114.25(17) . . ?
C10 O6 C11 111.15(17) . . ?
C15 O7 C13 111.73(19) . . ?
C15 O7 Li1 124.23(17) . . ?
C13 O7 Li1 109.91(17) . . ?
C16 O8 C14 112.46(17) . . ?
C16 O8 Li1 133.01(18) . . ?
C14 O8 Li1 108.60(18) . . ?
O1 C1 C2 110.91(19) . . ?
O1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.0 . . ?
O2 C2 C1 106.22(18) . . ?
O2 C2 H2A 110.5 . . ?
C1 C2 H2A 110.5 . . ?
O2 C2 H2B 110.5 . . ?
C1 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
O2 C3 C4 107.17(17) . . ?
O2 C3 H3A 110.3 . . ?
C4 C3 H3A 110.3 . . ?
O2 C3 H3B 110.3 . . ?
C4 C3 H3B 110.3 . . ?
H3A C3 H3B 108.5 . . ?
O3 C4 C3 107.02(18) . . ?
O3 C4 H4A 110.3 . . ?
C3 C4 H4A 110.3 . . ?
O3 C4 H4B 110.3 . . ?
C3 C4 H4B 110.3 . . ?
H4A C4 H4B 108.6 . . ?
O3 C5 C6 112.46(17) . . ?
O3 C5 H5A 109.1 . . ?
C6 C5 H5A 109.1 . . ?
O3 C5 H5B 109.1 . . ?
C6 C5 H5B 109.1 . . ?
H5A C5 H5B 107.8 . . ?
O4 C6 C5 112.49(19) . . ?
O4 C6 H6A 109.1 . . ?
C5 C6 H6A 109.1 . . ?
O4 C6 H6B 109.1 . . ?
C5 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
O4 C7 C8 108.53(19) . . ?
O4 C7 H7A 110.0 . . ?
C8 C7 H7A 110.0 . . ?
O4 C7 H7B 110.0 . . ?
C8 C7 H7B 110.0 . . ?
H7A C7 H7B 108.4 . . ?
O5 C8 C7 114.4(2) . . ?
O5 C8 H8A 108.6 . . ?
C7 C8 H8A 108.6 . . ?
O5 C8 H8B 108.6 . . ?
C7 C8 H8B 108.6 . . ?
H8A C8 H8B 107.6 . . ?
O5 C9 C10 108.79(18) . . ?
O5 C9 H9A 109.9 . . ?
C10 C9 H9A 109.9 . . ?
O5 C9 H9B 109.9 . . ?
C10 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
O6 C10 C9 109.75(18) . . ?
O6 C10 H10A 109.7 . . ?
C9 C10 H10A 109.7 . . ?
O6 C10 H10B 109.7 . . ?
C9 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
O6 C11 C12 107.95(19) . . ?
O6 C11 H11A 110.1 . . ?
C12 C11 H11A 110.1 . . ?
O6 C11 H11B 110.1 . . ?
C12 C11 H11B 110.1 . . ?
H11A C11 H11B 108.4 . . ?
O1 C12 C11 113.34(19) . . ?
O1 C12 H12A 108.9 . . ?
C11 C12 H12A 108.9 . . ?
O1 C12 H12B 108.9 . . ?
C11 C12 H12B 108.9 . . ?
H12A C12 H12B 107.7 . . ?
O7 C13 C14 107.35(19) . . ?
O7 C13 H13A 110.2 . . ?
C14 C13 H13A 110.2 . . ?
O7 C13 H13B 110.2 . . ?
C14 C13 H13B 110.2 . . ?
H13A C13 H13B 108.5 . . ?
O8 C14 C13 107.52(18) . . ?
O8 C14 H14A 110.2 . . ?
C13 C14 H14A 110.2 . . ?
O8 C14 H14B 110.2 . . ?
C13 C14 H14B 110.2 . . ?
H14A C14 H14B 108.5 . . ?
O7 C15 H15A 109.5 . . ?
O7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O8 C16 H16A 109.5 . . ?
O8 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O8 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C35 118.40(19) . . ?
C18 C17 C34 122.9(2) . . ?
C35 C17 C34 118.7(2) . . ?
C19 C18 C17 121.8(2) . . ?
C19 C18 H18 119.1 . . ?
C17 C18 H18 119.1 . . ?
C20 C19 C18 120.6(2) . . ?
C20 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
C19 C20 C21 120.8(2) . . ?
C19 C20 H20 119.6 . . ?
C21 C20 H20 119.6 . . ?
C20 C21 C22 121.7(2) . . ?
C20 C21 C35 119.2(2) . . ?
C22 C21 C35 119.2(2) . . ?
C23 C22 C21 120.6(2) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C22 C23 C24 120.9(2) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 H23 119.6 . . ?
C23 C24 C25 121.6(2) . . ?
C23 C24 H24 119.2 . . ?
C25 C24 H24 119.2 . . ?
C24 C25 C35 118.5(2) . . ?
C24 C25 C26 122.1(2) . . ?
C35 C25 C26 119.4(2) . . ?
C27 C26 C36 118.53(19) . . ?
C27 C26 C25 122.3(2) . . ?
C36 C26 C25 119.2(2) . . ?
C28 C27 C26 121.5(2) . . ?
C28 C27 H27 119.3 . . ?
C26 C27 H27 119.3 . . ?
C29 C28 C27 121.0(2) . . ?
C29 C28 H28 119.5 . . ?
C27 C28 H28 119.5 . . ?
C28 C29 C30 120.5(2) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C29 C30 C31 121.9(2) . . ?
C29 C30 C36 119.4(2) . . ?
C31 C30 C36 118.7(2) . . ?
C32 C31 C30 120.8(2) . . ?
C32 C31 H31 119.6 . . ?
C30 C31 H31 119.6 . . ?
C31 C32 C33 121.1(2) . . ?
C31 C32 H32 119.5 . . ?
C33 C32 H32 119.5 . . ?
C32 C33 C34 121.1(2) . . ?
C32 C33 H33 119.5 . . ?
C34 C33 H33 119.5 . . ?
C33 C34 C36 118.61(19) . . ?
C33 C34 C17 121.6(2) . . ?
C36 C34 C17 119.80(19) . . ?
C25 C35 C17 121.61(19) . . ?
C25 C35 C21 119.2(2) . . ?
C17 C35 C21 119.2(2) . . ?
C34 C36 C26 121.25(19) . . ?
C34 C36 C30 119.6(2) . . ?
C26 C36 C30 119.1(2) . . ?
C38 C37 C46 118.3(2) . . ?
C38 C37 C45 122.0(2) . 2_666 ?
C46 C37 C45 119.7(2) . 2_666 ?
C37 C38 C39 122.1(3) . . ?
C37 C38 H38 118.9 . . ?
C39 C38 H38 118.9 . . ?
C40 C39 C38 120.4(2) . . ?
C40 C39 H39 119.8 . . ?
C38 C39 H39 119.8 . . ?
C39 C40 C41 120.5(2) . . ?
C39 C40 H40 119.8 . . ?
C41 C40 H40 119.8 . . ?
C40 C41 C42 121.3(2) . . ?
C40 C41 C46 119.3(2) . . ?
C42 C41 C46 119.5(2) . . ?
C43 C42 C41 120.5(2) . . ?
C43 C42 H42 119.8 . . ?
C41 C42 H42 119.8 . . ?
C42 C43 C44 120.5(3) . . ?
C42 C43 H43 119.8 . . ?
C44 C43 H43 119.8 . . ?
C45 C44 C43 121.8(2) . . ?
C45 C44 H44 119.1 . . ?
C43 C44 H44 119.1 . . ?
C44 C45 C46 118.7(2) . . ?
C44 C45 C37 122.4(2) . 2_666 ?
C46 C45 C37 118.9(2) . 2_666 ?
C37 C46 C41 119.5(2) . . ?
C37 C46 C45 121.4(2) . . ?
C41 C46 C45 119.1(2) . . ?

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
C12 O1 C1 C2 99.5(2) . . . . ?
Li1 O1 C1 C2 -37.0(3) . . . . ?
C3 O2 C2 C1 -165.84(19) . . . . ?
Li1 O2 C2 C1 -40.7(3) . . . . ?
O1 C1 C2 O2 51.6(3) . . . . ?
C2 O2 C3 C4 172.47(19) . . . . ?
Li1 O2 C3 C4 46.8(2) . . . . ?
C5 O3 C4 C3 -177.37(17) . . . . ?
Li1 O3 C4 C3 34.4(2) . . . . ?
O2 C3 C4 O3 -52.7(2) . . . . ?
C4 O3 C5 C6 71.7(2) . . . . ?
Li1 O3 C5 C6 -143.9(2) . . . . ?
C7 O4 C6 C5 74.2(2) . . . . ?
O3 C5 C6 O4 52.4(3) . . . . ?
C6 O4 C7 C8 -166.87(19) . . . . ?
C9 O5 C8 C7 -78.4(2) . . . . ?
O4 C7 C8 O5 74.7(2) . . . . ?
C8 O5 C9 C10 -176.30(18) . . . . ?
C11 O6 C10 C9 -179.94(19) . . . . ?
O5 C9 C10 O6 -69.3(2) . . . . ?
C10 O6 C11 C12 179.15(19) . . . . ?
C1 O1 C12 C11 -76.8(2) . . . . ?
Li1 O1 C12 C11 56.1(3) . . . . ?
O6 C11 C12 O1 -54.4(3) . . . . ?
C15 O7 C13 C14 -178.74(19) . . . . ?
Li1 O7 C13 C14 39.2(2) . . . . ?
C16 O8 C14 C13 -159.4(2) . . . . ?
Li1 O8 C14 C13 44.0(2) . . . . ?
O7 C13 C14 O8 -55.3(2) . . . . ?
C35 C17 C18 C19 -1.9(3) . . . . ?
C34 C17 C18 C19 178.3(2) . . . . ?
C17 C18 C19 C20 0.5(3) . . . . ?
C18 C19 C20 C21 1.5(3) . . . . ?
C19 C20 C21 C22 177.3(2) . . . . ?
C19 C20 C21 C35 -2.1(3) . . . . ?
C20 C21 C22 C23 -178.9(2) . . . . ?
C35 C21 C22 C23 0.5(3) . . . . ?
C21 C22 C23 C24 -1.3(4) . . . . ?
C22 C23 C24 C25 0.5(4) . . . . ?
C23 C24 C25 C35 1.1(3) . . . . ?
C23 C24 C25 C26 -178.8(2) . . . . ?
C24 C25 C26 C27 1.5(3) . . . . ?
C35 C25 C26 C27 -178.4(2) . . . . ?
C24 C25 C26 C36 -179.0(2) . . . . ?
C35 C25 C26 C36 1.1(3) . . . . ?
C36 C26 C27 C28 -0.1(3) . . . . ?
C25 C26 C27 C28 179.4(2) . . . . ?
C26 C27 C28 C29 0.0(3) . . . . ?
C27 C28 C29 C30 0.5(3) . . . . ?
C28 C29 C30 C31 178.2(2) . . . . ?
C28 C29 C30 C36 -1.0(3) . . . . ?
C29 C30 C31 C32 -180.0(2) . . . . ?
C36 C30 C31 C32 -0.8(3) . . . . ?
C30 C31 C32 C33 -0.2(3) . . . . ?
C31 C32 C33 C34 0.9(3) . . . . ?
C32 C33 C34 C36 -0.6(3) . . . . ?
C32 C33 C34 C17 180.0(2) . . . . ?
C18 C17 C34 C33 -0.2(3) . . . . ?
C35 C17 C34 C33 180.0(2) . . . . ?
C18 C17 C34 C36 -179.5(2) . . . . ?
C35 C17 C34 C36 0.6(3) . . . . ?
C24 C25 C35 C17 178.0(2) . . . . ?
C26 C25 C35 C17 -2.1(3) . . . . ?
C24 C25 C35 C21 -1.9(3) . . . . ?
C26 C25 C35 C21 178.0(2) . . . . ?
C18 C17 C35 C25 -178.6(2) . . . . ?
C34 C17 C35 C25 1.3(3) . . . . ?
C18 C17 C35 C21 1.3(3) . . . . ?
C34 C17 C35 C21 -178.88(19) . . . . ?
C20 C21 C35 C25 -179.5(2) . . . . ?
C22 C21 C35 C25 1.1(3) . . . . ?
C20 C21 C35 C17 0.7(3) . . . . ?
C22 C21 C35 C17 -178.8(2) . . . . ?
C33 C34 C36 C26 179.0(2) . . . . ?
C17 C34 C36 C26 -1.6(3) . . . . ?
C33 C34 C36 C30 -0.4(3) . . . . ?
C17 C34 C36 C30 179.02(19) . . . . ?
C27 C26 C36 C34 -179.7(2) . . . . ?
C25 C26 C36 C34 0.8(3) . . . . ?
C27 C26 C36 C30 -0.3(3) . . . . ?
C25 C26 C36 C30 -179.87(19) . . . . ?
C29 C30 C36 C34 -179.7(2) . . . . ?
C31 C30 C36 C34 1.1(3) . . . . ?
C29 C30 C36 C26 0.9(3) . . . . ?
C31 C30 C36 C26 -178.30(19) . . . . ?
C46 C37 C38 C39 0.8(3) . . . . ?
C45 C37 C38 C39 179.7(2) 2_666 . . . ?
C37 C38 C39 C40 -0.3(4) . . . . ?
C38 C39 C40 C41 -0.1(4) . . . . ?
C39 C40 C41 C42 -178.9(2) . . . . ?
C39 C40 C41 C46 0.1(3) . . . . ?
C40 C41 C42 C43 177.7(2) . . . . ?
C46 C41 C42 C43 -1.2(3) . . . . ?
C41 C42 C43 C44 1.1(4) . . . . ?
C42 C43 C44 C45 0.0(4) . . . . ?
C43 C44 C45 C46 -1.0(3) . . . . ?
C43 C44 C45 C37 -179.8(2) . . . 2_666 ?
C38 C37 C46 C41 -0.8(3) . . . . ?
C45 C37 C46 C41 -179.73(19) 2_666 . . . ?
C38 C37 C46 C45 178.3(2) . . . . ?
C45 C37 C46 C45 -0.6(3) 2_666 . . . ?
C40 C41 C46 C37 0.4(3) . . . . ?
C42 C41 C46 C37 179.4(2) . . . . ?
C40 C41 C46 C45 -178.7(2) . . . . ?
C42 C41 C46 C45 0.2(3) . . . . ?
C44 C45 C46 C37 -178.3(2) . . . . ?
C37 C45 C46 C37 0.6(3) 2_666 . . . ?
C44 C45 C46 C41 0.9(3) . . . . ?
C37 C45 C46 C41 179.73(19) 2_666 . . . ?

_refine_diff_density_max         0.333
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.056

_shelxl_version_number           2014/6

