# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_elu230003_fa
_database_code_depnum_ccdc_archive 'CCDC 2307285'
loop_
_audit_author_name
_audit_author_address
'Paul G. Waddell'
;School of Natural and Environmental Sciences, Newcastle University
United Kingdom
;
_audit_update_record             
;
2023-11-11 deposited with the CCDC.	2024-02-12 downloaded from the CCDC.
;
_audit_creation_date             2023-02-24
_audit_creation_method           
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C96 H66 Li6 O6, 2(C6 H6)'
_chemical_formula_sum            'C108 H78 Li6 O6'
_chemical_formula_weight         1513.34
_chemical_absolute_configuration unk
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C20 H23 Li1 O1 Si1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
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'

_cell_length_a                   19.4816(5)
_cell_length_b                   16.7761(4)
_cell_length_c                   25.2397(6)
_cell_angle_alpha                90
_cell_angle_beta                 96.189(2)
_cell_angle_gamma                90
_cell_volume                     8200.9(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    16644
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      75.8970
_cell_measurement_theta_min      3.4760
_shelx_estimated_absorpt_T_max   0.972
_shelx_estimated_absorpt_T_min   0.946
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.923
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             3168
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 1 0 0.0306
1 -1 0 0.0496
-1 -1 0 0.0436
1 1 0 0.0366
0 0 -1 0.0267
0 0 1 0.0247

_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.0006 1.0006 0.0014 0.0779 0.0890 -0.0286
1.0006 -1.0006 -0.0014 -0.0779 -0.0890 0.0286
-1.0012 -0.9980 0.0037 0.0555 -0.0395 0.1007
1.0012 0.9980 -0.0037 -0.0555 0.0395 -0.1007
-0.0008 0.0004 -0.9997 -0.0271 0.0414 0.0364
0.0008 -0.0004 0.9997 0.0271 -0.0414 -0.0364

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            40731
_diffrn_reflns_point_group_measured_fraction_full 0.853
_diffrn_reflns_point_group_measured_fraction_max 0.772
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.428
_diffrn_reflns_theta_min         3.485
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -79.00 -74.00   0.50    1.00    --  -99.00  70.00   0.00   10
  2  ω    -79.00 -74.00   0.50    1.00    --  -99.00  70.00  90.00   10
  3  ω    -29.00 -24.00   0.50    0.25    --  -49.63  70.00  90.00   10
  4  ω      0.00   5.00   0.50    0.25    --  -49.63  60.00   0.00   10
  5  ω     28.00  33.00   0.50    0.25    --   48.88 -70.00  90.00   10
  6  ω     74.00  79.00   0.50    1.00    --  102.18 -70.00  90.00   10
  7  ω     36.00 120.00   0.50    0.25    --   48.76  72.00   7.00  168
  8  ω    -16.00  30.00   0.50    0.25    --   48.76 -72.00-122.00   92
  9  ω    -95.00 -29.00   0.50    0.25    --  -49.76 -72.00-122.00  132
 10  ω    -87.00 -31.00   0.50    1.00    --  -92.01  72.00   7.00  112
 11  ω   -162.00 -71.00   0.50    1.00    --  -92.01 -72.00-122.00  182
 12  ω     38.00  91.00   0.50    1.00    --  108.00 -72.00-122.00  106
 13  ω    -30.00  26.00   0.50    0.25    --   48.76 -19.00  30.00  112
 14  ω    -19.00   7.00   0.50    0.25    --  -49.76  19.00   0.00   52
 15  ω   -122.00 -77.00   0.50    0.25    --  -49.76-125.00 -30.00   90
 16  ω   -100.00 -73.00   0.50    1.00    --  -92.01 -61.00 -90.00   54
 17  ω    -45.00 -14.00   0.50    1.00    --  -92.01  45.00-180.00   62
 18  ω   -149.00 -67.00   0.50    1.00    --  -92.01 -77.00 120.00  164
 19  ω   -144.00-117.00   0.50    1.00    --  -92.01 -61.00 -90.00   54
 20  ω    -48.00 -16.00   0.50    1.00    --  -92.01  45.00-150.00   64
 21  ω   -108.00 -19.00   0.50    1.00    --  -92.01 125.00   0.00  178
 22  ω    -63.00 -20.00   0.50    1.00    --  -92.01  61.00-150.00   86
 23  ω   -169.00 -72.00   0.50    1.00    --  -92.01 -30.00 -60.00  194
 24  ω     20.00  51.00   0.50    1.00    --   96.11 -45.00 -90.00   62
 25  ω    143.00 169.00   0.50    1.00    --   96.11  61.00 -90.00   52
 26  ω     79.00 108.00   0.50    1.00    --   96.11  61.00 -90.00   58
 27  ω     18.00  43.00   0.50    1.00    --   96.11 -45.00 150.00   50
 28  ω     18.00  50.00   0.50    1.00    --   96.11 -45.00-120.00   64
 29  ω     20.00  46.00   0.50    1.00    --   96.11 -45.00 -30.00   52
 30  ω     18.00  46.00   0.50    1.00    --   96.11 -45.00  60.00   56
 31  ω     44.00  86.00   0.50    1.00    --  108.00 -95.00 150.00   84
 32  ω     43.00  68.00   0.50    1.00    --  108.00 -61.00   0.00   50
 33  ω     94.00 120.00   0.50    1.00    --  108.00  30.00-120.00   52
 34  ω     81.00 106.00   0.50    1.00    --  108.00 -95.00  60.00   50
 35  ω     81.00 106.00   0.50    1.00    --  108.00-125.00  30.00   50
 36  ω     40.00  68.00   0.50    1.00    --  108.00 -61.00  60.00   56
 37  ω    104.00 178.00   0.50    1.00    --  108.00  30.00 -60.00  148
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix-Arc 100'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0665574000
_diffrn_orient_matrix_UB_12      0.0112983000
_diffrn_orient_matrix_UB_13      0.0272083000
_diffrn_orient_matrix_UB_21      -0.0247546000
_diffrn_orient_matrix_UB_22      0.0642777000
_diffrn_orient_matrix_UB_23      -0.0413475000
_diffrn_orient_matrix_UB_31      -0.0362272000
_diffrn_orient_matrix_UB_32      -0.0647123000
_diffrn_orient_matrix_UB_33      -0.0364502000
_diffrn_oxdiff_digest_frames     
;
015429ca097e09fc68f415757de160701b02846a019
;
_diffrn_oxdiff_digest_hkl        
;
01c2956ca57681825ae387a1bac42fff260291
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.654
_reflns_Friedel_fraction_full    0.706
_reflns_Friedel_fraction_max     0.611
_reflns_number_gt                12135
_reflns_number_total             13627
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 
;
 Flack x determined using 4343 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.63(9)
_refine_ls_extinction_coef       0.00013(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1082
_refine_ls_number_reflns         13627
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0466
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0944P)²+1.2194P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1366
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C28(H28), C29(H29),
  C30(H30), C31(H31), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42),
 C44(H44), C45(H45), C46(H46), C47(H47), C53(H53), C54(H54), C55(H55), C56(H56),
  C58(H58), C60(H60), C61(H61), C62(H62), C63(H63), C69(H69), C70(H70),
 C71(H71), C72(H72), C74(H74), C76(H76), C77(H77), C78(H78), C79(H79), C85(H85),
  C86(H86), C87(H87), C88(H88), C90(H90), C92(H92), C93(H93), C94(H94),
 C95(H95), C97(H97), C98(H98), C99(H99), C100(H100), C101(H101), C102(H102),
 C103(H103), C104(H104), C105(H105), C106(H106), C107(H107), C108(H108)
2.b X=CH2 refined with riding coordinates:
 C2(H2A,H2B), C18(H18A,H18B), C34(H34A,H34B), C50(H50A,H50B), C66(H66A,H66B),
 C82(H82A,H82B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
O1 O 0.40515(10) 0.51674(11) 0.54525(8) 0.0288(4) Uani 1 1 d . . . . .
O2 O 0.51678(11) 0.60298(12) 0.46990(8) 0.0310(4) Uani 1 1 d . . . . .
O3 O 0.57452(10) 0.48015(11) 0.56905(8) 0.0304(4) Uani 1 1 d . . . . .
O4 O 0.60173(10) 0.64861(11) 0.56658(8) 0.0303(4) Uani 1 1 d . . . . .
O5 O 0.49132(11) 0.56051(12) 0.64045(8) 0.0306(4) Uani 1 1 d . . . . .
O6 O 0.43293(10) 0.68542(11) 0.53817(8) 0.0301(4) Uani 1 1 d . . . . .
C1 C 0.34258(15) 0.48418(16) 0.53267(11) 0.0279(6) Uani 1 1 d . . . . .
C2 C 0.31583(19) 0.4240(2) 0.55711(14) 0.0409(7) Uani 1 1 d . . . . .
H2A H 0.341583 0.399310 0.586780 0.049 Uiso 1 1 calc R U . . .
H2B H 0.270830 0.405247 0.545021 0.049 Uiso 1 1 calc R U . . .
C3 C 0.30334(15) 0.52389(17) 0.48500(12) 0.0305(6) Uani 1 1 d . . . . .
C4 C 0.24802(16) 0.57636(17) 0.49041(13) 0.0328(6) Uani 1 1 d . . . . .
C5 C 0.22444(17) 0.59386(19) 0.54057(14) 0.0388(7) Uani 1 1 d . . . . .
H5 H 0.246144 0.569398 0.571957 0.047 Uiso 1 1 calc R U . . .
C6 C 0.17101(19) 0.6454(2) 0.54399(17) 0.0476(9) Uani 1 1 d . . . . .
H6 H 0.156473 0.657425 0.577832 0.057 Uiso 1 1 calc R U . . .
C7 C 0.1369(2) 0.6812(2) 0.49757(19) 0.0548(10) Uani 1 1 d . . . . .
H7 H 0.099356 0.716404 0.500538 0.066 Uiso 1 1 calc R U . . .
C8 C 0.1573(2) 0.6659(2) 0.44933(18) 0.0507(9) Uani 1 1 d . . . . .
H8 H 0.133456 0.690081 0.418633 0.061 Uiso 1 1 calc R U . . .
C9 C 0.21395(18) 0.61400(19) 0.44346(14) 0.0393(7) Uani 1 1 d . . . . .
C10 C 0.23578(19) 0.5985(2) 0.39374(14) 0.0431(8) Uani 1 1 d . . . . .
H10 H 0.213370 0.624369 0.363162 0.052 Uiso 1 1 calc R U . . .
C11 C 0.28987(19) 0.5456(2) 0.38775(13) 0.0401(7) Uani 1 1 d . . . . .
C12 C 0.3105(2) 0.5246(2) 0.33621(14) 0.0505(9) Uani 1 1 d . . . . .
H12 H 0.287844 0.548379 0.304941 0.061 Uiso 1 1 calc R U . . .
C13 C 0.3616(2) 0.4716(3) 0.33207(16) 0.0563(10) Uani 1 1 d . . . . .
H13 H 0.373954 0.457780 0.297856 0.068 Uiso 1 1 calc R U . . .
C14 C 0.3972(2) 0.4362(2) 0.37812(14) 0.0478(8) Uani 1 1 d . . . . .
H14 H 0.433561 0.399596 0.374426 0.057 Uiso 1 1 calc R U . . .
C15 C 0.37992(18) 0.4541(2) 0.42734(14) 0.0389(7) Uani 1 1 d . . . . .
H15 H 0.404646 0.430141 0.457750 0.047 Uiso 1 1 calc R U . . .
C16 C 0.32463(16) 0.50876(18) 0.43423(12) 0.0334(6) Uani 1 1 d . . . . .
C17 C 0.53641(15) 0.60772(16) 0.42030(11) 0.0279(6) Uani 1 1 d . . . . .
C18 C 0.49343(17) 0.6173(2) 0.37590(13) 0.0390(7) Uani 1 1 d . . . . .
H18A H 0.445127 0.621272 0.377866 0.047 Uiso 1 1 calc R U . . .
H18B H 0.511129 0.620097 0.342317 0.047 Uiso 1 1 calc R U . . .
C19 C 0.61242(16) 0.60061(17) 0.41964(11) 0.0302(6) Uani 1 1 d . . . . .
C20 C 0.65503(16) 0.66849(19) 0.41969(12) 0.0335(6) Uani 1 1 d . . . . .
C21 C 0.62758(19) 0.7475(2) 0.41573(13) 0.0397(7) Uani 1 1 d . . . . .
H21 H 0.579095 0.755340 0.413978 0.048 Uiso 1 1 calc R U . . .
C22 C 0.6696(2) 0.8110(2) 0.41445(15) 0.0486(9) Uani 1 1 d . . . . .
H22 H 0.650339 0.863094 0.412096 0.058 Uiso 1 1 calc R U . . .
C23 C 0.7419(2) 0.8016(3) 0.41654(17) 0.0556(10) Uani 1 1 d . . . . .
H23 H 0.770599 0.847228 0.415464 0.067 Uiso 1 1 calc R U . . .
C24 C 0.7707(2) 0.7281(2) 0.42005(16) 0.0500(9) Uani 1 1 d . . . . .
H24 H 0.819317 0.722601 0.421108 0.060 Uiso 1 1 calc R U . . .
C25 C 0.72856(18) 0.6590(2) 0.42219(13) 0.0390(7) Uani 1 1 d . . . . .
C26 C 0.75670(18) 0.5823(2) 0.42613(14) 0.0417(7) Uani 1 1 d . . . . .
H26 H 0.805444 0.576253 0.429061 0.050 Uiso 1 1 calc R U . . .
C27 C 0.71587(17) 0.5151(2) 0.42588(12) 0.0366(7) Uani 1 1 d . . . . .
C28 C 0.74404(19) 0.4357(2) 0.42813(14) 0.0426(8) Uani 1 1 d . . . . .
H28 H 0.792592 0.428708 0.429514 0.051 Uiso 1 1 calc R U . . .
C29 C 0.7032(2) 0.3713(2) 0.42831(14) 0.0453(8) Uani 1 1 d . . . . .
H29 H 0.723171 0.319546 0.430213 0.054 Uiso 1 1 calc R U . . .
C30 C 0.6307(2) 0.3799(2) 0.42567(14) 0.0440(8) Uani 1 1 d . . . . .
H30 H 0.602451 0.333845 0.425964 0.053 Uiso 1 1 calc R U . . .
C31 C 0.60102(18) 0.45309(18) 0.42274(13) 0.0371(7) Uani 1 1 d . . . . .
H31 H 0.552175 0.457462 0.420539 0.045 Uiso 1 1 calc R U . . .
C32 C 0.64211(16) 0.52386(18) 0.42292(12) 0.0324(6) Uani 1 1 d . . . . .
C33 C 0.61040(15) 0.41266(16) 0.58019(11) 0.0281(6) Uani 1 1 d . . . . .
C34 C 0.66983(17) 0.3939(2) 0.56286(14) 0.0386(7) Uani 1 1 d . . . . .
H34A H 0.690987 0.429632 0.540369 0.046 Uiso 1 1 calc R U . . .
H34B H 0.691479 0.344578 0.572876 0.046 Uiso 1 1 calc R U . . .
C35 C 0.57457(16) 0.35707(17) 0.61474(12) 0.0307(6) Uani 1 1 d . . . . .
C36 C 0.59635(17) 0.35087(18) 0.66953(13) 0.0347(7) Uani 1 1 d . . . . .
C37 C 0.65325(18) 0.3953(2) 0.69423(13) 0.0383(7) Uani 1 1 d . . . . .
H37 H 0.676864 0.431329 0.673502 0.046 Uiso 1 1 calc R U . . .
C38 C 0.6744(2) 0.3870(2) 0.74715(15) 0.0514(9) Uani 1 1 d . . . . .
H38 H 0.712918 0.416369 0.762985 0.062 Uiso 1 1 calc R U . . .
C39 C 0.6386(3) 0.3342(3) 0.77867(15) 0.0602(11) Uani 1 1 d . . . . .
H39 H 0.653857 0.328312 0.815497 0.072 Uiso 1 1 calc R U . . .
C40 C 0.5842(2) 0.2929(2) 0.75745(15) 0.0536(9) Uani 1 1 d . . . . .
H40 H 0.561045 0.258581 0.779636 0.064 Uiso 1 1 calc R U . . .
C41 C 0.55960(19) 0.2988(2) 0.70221(14) 0.0414(7) Uani 1 1 d . . . . .
C42 C 0.5025(2) 0.2560(2) 0.67840(16) 0.0456(8) Uani 1 1 d . . . . .
H42 H 0.478570 0.221607 0.699995 0.055 Uiso 1 1 calc R U . . .
C43 C 0.47977(18) 0.26199(19) 0.62494(15) 0.0405(7) Uani 1 1 d . . . . .
C44 C 0.4214(2) 0.2185(2) 0.60033(18) 0.0518(9) Uani 1 1 d . . . . .
H44 H 0.397476 0.183200 0.621293 0.062 Uiso 1 1 calc R U . . .
C45 C 0.3998(2) 0.2269(2) 0.54791(19) 0.0566(10) Uani 1 1 d . . . . .
H45 H 0.359972 0.199069 0.532757 0.068 Uiso 1 1 calc R U . . .
C46 C 0.4362(2) 0.2767(2) 0.51559(16) 0.0502(9) Uani 1 1 d . . . . .
H46 H 0.421427 0.280817 0.478579 0.060 Uiso 1 1 calc R U . . .
C47 C 0.49195(18) 0.31875(18) 0.53654(14) 0.0381(7) Uani 1 1 d . . . . .
H47 H 0.515414 0.352105 0.513978 0.046 Uiso 1 1 calc R U . . .
C48 C 0.51623(17) 0.31394(17) 0.59202(13) 0.0339(6) Uani 1 1 d . . . . .
C49 C 0.66200(15) 0.68469(16) 0.58238(12) 0.0295(6) Uani 1 1 d . . . . .
C50 C 0.6874(2) 0.7478(2) 0.56072(15) 0.0455(8) Uani 1 1 d . . . . .
H50A H 0.662367 0.772513 0.530736 0.055 Uiso 1 1 calc R U . . .
H50B H 0.730742 0.768787 0.575038 0.055 Uiso 1 1 calc R U . . .
C51 C 0.70050(16) 0.64498(18) 0.63047(12) 0.0334(6) Uani 1 1 d . . . . .
C52 C 0.75542(17) 0.59276(18) 0.62469(13) 0.0368(7) Uani 1 1 d . . . . .
C53 C 0.77739(18) 0.57406(19) 0.57399(15) 0.0419(8) Uani 1 1 d . . . . .
H53 H 0.754332 0.597718 0.542809 0.050 Uiso 1 1 calc R U . . .
C54 C 0.8310(2) 0.5228(2) 0.56943(19) 0.0525(9) Uani 1 1 d . . . . .
H54 H 0.844277 0.510531 0.535241 0.063 Uiso 1 1 calc R U . . .
C55 C 0.8664(2) 0.4881(2) 0.6153(2) 0.0616(12) Uani 1 1 d . . . . .
H55 H 0.904097 0.453252 0.611760 0.074 Uiso 1 1 calc R U . . .
C56 C 0.8479(2) 0.5036(2) 0.6637(2) 0.0578(11) Uani 1 1 d . . . . .
H56 H 0.872792 0.479399 0.693907 0.069 Uiso 1 1 calc R U . . .
C57 C 0.79153(19) 0.5556(2) 0.67144(16) 0.0453(8) Uani 1 1 d . . . . .
C58 C 0.7701(2) 0.5718(2) 0.72087(15) 0.0505(9) Uani 1 1 d . . . . .
H58 H 0.794247 0.547685 0.751472 0.061 Uiso 1 1 calc R U . . .
C59 C 0.7149(2) 0.6218(2) 0.72761(14) 0.0463(8) Uani 1 1 d . . . . .
C60 C 0.6929(3) 0.6398(3) 0.77868(16) 0.0611(11) Uani 1 1 d . . . . .
H60 H 0.716416 0.615909 0.809590 0.073 Uiso 1 1 calc R U . . .
C61 C 0.6406(3) 0.6891(3) 0.78407(17) 0.0667(12) Uani 1 1 d . . . . .
H61 H 0.627745 0.699781 0.818621 0.080 Uiso 1 1 calc R U . . .
C62 C 0.6034(2) 0.7264(3) 0.73854(16) 0.0552(10) Uani 1 1 d . . . . .
H62 H 0.565988 0.761338 0.742768 0.066 Uiso 1 1 calc R U . . .
C63 C 0.62239(19) 0.7108(2) 0.68887(14) 0.0426(8) Uani 1 1 d . . . . .
H63 H 0.597520 0.735092 0.658664 0.051 Uiso 1 1 calc R U . . .
C64 C 0.67879(17) 0.65888(19) 0.68138(13) 0.0378(7) Uani 1 1 d . . . . .
C65 C 0.47183(15) 0.54824(17) 0.68941(12) 0.0305(6) Uani 1 1 d . . . . .
C66 C 0.51419(19) 0.5316(2) 0.73273(14) 0.0424(7) Uani 1 1 d . . . . .
H66A H 0.562457 0.527544 0.730597 0.051 Uiso 1 1 calc R U . . .
H66B H 0.496271 0.523762 0.765885 0.051 Uiso 1 1 calc R U . . .
C67 C 0.39560(16) 0.55618(19) 0.69053(11) 0.0311(6) Uani 1 1 d . . . . .
C68 C 0.35254(17) 0.48904(19) 0.69484(12) 0.0349(7) Uani 1 1 d . . . . .
C69 C 0.3796(2) 0.4103(2) 0.70131(14) 0.0425(8) Uani 1 1 d . . . . .
H69 H 0.428008 0.401805 0.703036 0.051 Uiso 1 1 calc R U . . .
C70 C 0.3362(2) 0.3466(2) 0.70505(16) 0.0527(9) Uani 1 1 d . . . . .
H70 H 0.354826 0.294343 0.709258 0.063 Uiso 1 1 calc R U . . .
C71 C 0.2636(2) 0.3581(2) 0.70269(16) 0.0537(10) Uani 1 1 d . . . . .
H71 H 0.234226 0.313444 0.705200 0.064 Uiso 1 1 calc R U . . .
C72 C 0.2360(2) 0.4320(2) 0.69691(14) 0.0454(8) Uani 1 1 d . . . . .
H72 H 0.187465 0.438612 0.695907 0.055 Uiso 1 1 calc R U . . .
C73 C 0.27917(18) 0.5004(2) 0.69227(13) 0.0395(7) Uani 1 1 d . . . . .
C74 C 0.25135(18) 0.5763(2) 0.68623(13) 0.0413(7) Uani 1 1 d . . . . .
H74 H 0.202766 0.582714 0.685090 0.050 Uiso 1 1 calc R U . . .
C75 C 0.29245(17) 0.6436(2) 0.68176(13) 0.0374(7) Uani 1 1 d . . . . .
C76 C 0.26439(19) 0.7215(2) 0.67501(15) 0.0448(8) Uani 1 1 d . . . . .
H76 H 0.215928 0.728890 0.674013 0.054 Uiso 1 1 calc R U . . .
C77 C 0.3058(2) 0.7857(2) 0.66995(16) 0.0482(9) Uani 1 1 d . . . . .
H77 H 0.286166 0.837304 0.664825 0.058 Uiso 1 1 calc R U . . .
C78 C 0.37759(19) 0.7757(2) 0.67228(14) 0.0424(7) Uani 1 1 d . . . . .
H78 H 0.405962 0.821125 0.668940 0.051 Uiso 1 1 calc R U . . .
C79 C 0.40763(18) 0.70251(19) 0.67922(13) 0.0371(7) Uani 1 1 d . . . . .
H79 H 0.456432 0.697722 0.681201 0.045 Uiso 1 1 calc R U . . .
C80 C 0.36606(17) 0.63260(19) 0.68356(12) 0.0333(6) Uani 1 1 d . . . . .
C81 C 0.39668(15) 0.75114(16) 0.52265(11) 0.0276(6) Uani 1 1 d . . . . .
C82 C 0.33381(17) 0.7686(2) 0.53466(14) 0.0404(7) Uani 1 1 d . . . . .
H82A H 0.310558 0.733171 0.556029 0.049 Uiso 1 1 calc R U . . .
H82B H 0.312021 0.816614 0.521905 0.049 Uiso 1 1 calc R U . . .
C83 C 0.43474(16) 0.80719(16) 0.48958(12) 0.0319(6) Uani 1 1 d . . . . .
C84 C 0.41909(17) 0.81217(17) 0.43387(13) 0.0340(6) Uani 1 1 d . . . . .
C85 C 0.36550(17) 0.76563(19) 0.40560(13) 0.0386(7) Uani 1 1 d . . . . .
H85 H 0.338917 0.730493 0.424726 0.046 Uiso 1 1 calc R U . . .
C86 C 0.3521(2) 0.7710(2) 0.35172(15) 0.0466(8) Uani 1 1 d . . . . .
H86 H 0.315956 0.740108 0.333770 0.056 Uiso 1 1 calc R U . . .
C87 C 0.3912(2) 0.8220(2) 0.32202(15) 0.0530(9) Uani 1 1 d . . . . .
H87 H 0.381979 0.823627 0.284307 0.064 Uiso 1 1 calc R U . . .
C88 C 0.4419(2) 0.8687(2) 0.34674(15) 0.0493(9) Uani 1 1 d . . . . .
H88 H 0.466738 0.903966 0.326346 0.059 Uiso 1 1 calc R U . . .
C89 C 0.45826(18) 0.86498(19) 0.40365(14) 0.0397(7) Uani 1 1 d . . . . .
C90 C 0.51100(19) 0.9107(2) 0.43005(15) 0.0433(8) Uani 1 1 d . . . . .
H90 H 0.536003 0.946320 0.410055 0.052 Uiso 1 1 calc R U . . .
C91 C 0.52800(18) 0.90554(19) 0.48472(15) 0.0407(7) Uani 1 1 d . . . . .
C92 C 0.5824(2) 0.9520(2) 0.51264(17) 0.0482(9) Uani 1 1 d . . . . .
H92 H 0.606529 0.989370 0.493283 0.058 Uiso 1 1 calc R U . . .
C93 C 0.6003(2) 0.9440(2) 0.56564(18) 0.0551(10) Uani 1 1 d . . . . .
H93 H 0.638424 0.973011 0.582582 0.066 Uiso 1 1 calc R U . . .
C94 C 0.5621(2) 0.8920(2) 0.59603(15) 0.0493(9) Uani 1 1 d . . . . .
H94 H 0.573397 0.888478 0.633515 0.059 Uiso 1 1 calc R U . . .
C95 C 0.50928(18) 0.84737(19) 0.57169(14) 0.0389(7) Uani 1 1 d . . . . .
H95 H 0.484624 0.812542 0.592498 0.047 Uiso 1 1 calc R U . . .
C96 C 0.49034(17) 0.85200(17) 0.51536(13) 0.0352(7) Uani 1 1 d . . . . .
C97 C 0.1130(3) 0.4900(3) 0.31156(19) 0.0726(15) Uani 1 1 d . . . . .
H97 H 0.140335 0.493538 0.345009 0.087 Uiso 1 1 calc R U . . .
C98 C 0.0688(3) 0.5491(3) 0.2956(3) 0.0832(18) Uani 1 1 d . . . . .
H98 H 0.064722 0.594510 0.317559 0.100 Uiso 1 1 calc R U . . .
C99 C 0.0291(3) 0.5428(4) 0.2464(3) 0.0892(19) Uani 1 1 d . . . . .
H99 H -0.002530 0.583750 0.234593 0.107 Uiso 1 1 calc R U . . .
C100 C 0.0359(3) 0.4785(4) 0.2157(2) 0.0758(14) Uani 1 1 d . . . . .
H100 H 0.009393 0.474296 0.181904 0.091 Uiso 1 1 calc R U . . .
C101 C 0.0802(3) 0.4200(3) 0.2327(2) 0.0644(12) Uani 1 1 d . . . . .
H101 H 0.084336 0.374287 0.210995 0.077 Uiso 1 1 calc R U . . .
C102 C 0.1187(2) 0.4256(3) 0.2802(2) 0.0668(12) Uani 1 1 d . . . . .
H102 H 0.149959 0.384074 0.291745 0.080 Uiso 1 1 calc R U . . .
C103 C 0.8824(3) 0.5958(4) 0.3368(3) 0.0886(19) Uani 1 1 d . . . . .
H103 H 0.851831 0.553117 0.326339 0.106 Uiso 1 1 calc R U . . .
C104 C 0.9265(3) 0.5885(3) 0.3796(3) 0.0771(15) Uani 1 1 d . . . . .
H104 H 0.928335 0.540247 0.399322 0.093 Uiso 1 1 calc R U . . .
C105 C 0.9700(3) 0.6501(4) 0.3960(2) 0.0831(16) Uani 1 1 d . . . . .
H105 H 1.000859 0.645212 0.427669 0.100 Uiso 1 1 calc R U . . .
C106 C 0.9687(3) 0.7189(3) 0.3664(3) 0.0852(17) Uani 1 1 d . . . . .
H106 H 0.999072 0.761620 0.377123 0.102 Uiso 1 1 calc R U . . .
C107 C 0.9231(4) 0.7254(3) 0.3215(2) 0.0866(17) Uani 1 1 d . . . . .
H107 H 0.921439 0.772357 0.300289 0.104 Uiso 1 1 calc R U . . .
C108 C 0.8799(3) 0.6624(5) 0.3077(2) 0.096(2) Uani 1 1 d . . . . .
H108 H 0.847619 0.666201 0.276829 0.116 Uiso 1 1 calc R U . . .
Li1 Li 0.4807(3) 0.4734(3) 0.5875(2) 0.0313(10) Uani 1 1 d . . . . .
Li2 Li 0.4290(3) 0.5910(3) 0.4914(2) 0.0323(10) Uani 1 1 d . . . . .
Li3 Li 0.5905(3) 0.5580(3) 0.5176(2) 0.0333(11) Uani 1 1 d . . . . .
Li4 Li 0.5270(3) 0.6911(3) 0.5214(2) 0.0322(10) Uani 1 1 d . . . . .
Li5 Li 0.5794(3) 0.5709(3) 0.6185(2) 0.0320(11) Uani 1 1 d . . . . .
Li6 Li 0.4187(3) 0.6104(3) 0.5920(2) 0.0320(10) 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
O1 C1 1.342(3) . ?
O1 Li1 1.869(5) . ?
O1 Li2 1.937(5) . ?
O1 Li6 1.965(5) . ?
O2 C17 1.350(3) . ?
O2 Li2 1.859(6) . ?
O2 Li3 1.927(6) . ?
O2 Li4 1.964(6) . ?
O3 C33 1.344(3) . ?
O3 Li1 1.936(6) . ?
O3 Li3 1.890(5) . ?
O3 Li5 1.964(6) . ?
O4 C49 1.343(3) . ?
O4 Li3 1.957(6) . ?
O4 Li4 1.890(5) . ?
O4 Li5 1.930(5) . ?
O5 C65 1.347(3) . ?
O5 Li1 1.977(5) . ?
O5 Li5 1.868(6) . ?
O5 Li6 1.956(6) . ?
O6 C81 1.345(3) . ?
O6 Li2 1.971(5) . ?
O6 Li4 1.927(5) . ?
O6 Li6 1.894(5) . ?
C1 C2 1.320(4) . ?
C1 C3 1.509(4) . ?
C1 Li2 2.741(6) . ?
C3 C4 1.410(4) . ?
C3 C16 1.412(4) . ?
C3 Li2 2.684(6) . ?
C4 C5 1.423(5) . ?
C4 C9 1.440(4) . ?
C5 C6 1.363(5) . ?
C6 C7 1.416(6) . ?
C7 C8 1.345(6) . ?
C8 C9 1.426(5) . ?
C9 C10 1.392(5) . ?
C10 C11 1.397(5) . ?
C11 C12 1.446(5) . ?
C11 C16 1.431(4) . ?
C12 C13 1.346(6) . ?
C13 C14 1.418(6) . ?
C14 C15 1.355(5) . ?
C15 C16 1.440(5) . ?
C16 Li2 2.737(6) . ?
C17 C18 1.334(4) . ?
C17 C19 1.487(4) . ?
C17 Li3 2.699(6) . ?
C19 C20 1.409(4) . ?
C19 C32 1.410(4) . ?
C19 Li3 2.653(6) . ?
C20 C21 1.429(5) . ?
C20 C25 1.436(5) . ?
C21 C22 1.346(5) . ?
C22 C23 1.413(6) . ?
C23 C24 1.352(6) . ?
C24 C25 1.425(5) . ?
C25 C26 1.398(5) . ?
C26 C27 1.379(5) . ?
C27 C28 1.440(5) . ?
C27 C32 1.438(4) . ?
C28 C29 1.341(6) . ?
C29 C30 1.415(5) . ?
C30 C31 1.355(5) . ?
C31 C32 1.432(4) . ?
C32 Li3 2.751(6) . ?
C33 C34 1.319(4) . ?
C33 C35 1.500(4) . ?
C33 Li1 2.748(6) . ?
C35 C36 1.406(4) . ?
C35 C48 1.415(4) . ?
C35 Li1 2.711(6) . ?
C36 C37 1.423(5) . ?
C36 C41 1.444(5) . ?
C37 C38 1.362(5) . ?
C38 C39 1.422(6) . ?
C39 C40 1.330(7) . ?
C40 C41 1.428(5) . ?
C41 C42 1.403(5) . ?
C42 C43 1.378(5) . ?
C43 C44 1.434(5) . ?
C43 C48 1.443(5) . ?
C44 C45 1.352(6) . ?
C45 C46 1.412(6) . ?
C46 C47 1.353(5) . ?
C47 C48 1.431(5) . ?
C48 Li1 2.762(6) . ?
C49 C50 1.313(4) . ?
C49 C51 1.511(4) . ?
C49 Li5 2.716(6) . ?
C51 C52 1.403(5) . ?
C51 C64 1.415(5) . ?
C51 Li5 2.654(6) . ?
C52 C53 1.427(5) . ?
C52 C57 1.448(5) . ?
C53 C54 1.367(5) . ?
C54 C55 1.408(7) . ?
C55 C56 1.337(7) . ?
C56 C57 1.431(6) . ?
C57 C58 1.384(6) . ?
C58 C59 1.389(6) . ?
C59 C60 1.434(6) . ?
C59 C64 1.438(5) . ?
C60 C61 1.330(7) . ?
C61 C62 1.435(7) . ?
C62 C63 1.370(5) . ?
C63 C64 1.431(5) . ?
C64 Li5 2.790(6) . ?
C65 C66 1.327(5) . ?
C65 C67 1.494(4) . ?
C65 Li6 2.767(6) . ?
C67 C68 1.416(4) . ?
C67 C80 1.408(4) . ?
C67 Li6 2.731(6) . ?
C68 C69 1.426(5) . ?
C68 C73 1.436(5) . ?
C69 C70 1.371(5) . ?
C70 C71 1.422(6) . ?
C71 C72 1.352(6) . ?
C72 C73 1.435(5) . ?
C73 C74 1.386(5) . ?
C74 C75 1.396(5) . ?
C75 C76 1.420(5) . ?
C75 C80 1.442(4) . ?
C76 C77 1.360(5) . ?
C77 C78 1.403(5) . ?
C78 C79 1.364(5) . ?
C79 C80 1.436(5) . ?
C79 Li6 2.718(6) . ?
C80 Li6 2.654(6) . ?
C81 C82 1.326(4) . ?
C81 C83 1.505(4) . ?
C81 Li4 2.734(6) . ?
C83 C84 1.409(4) . ?
C83 C96 1.418(4) . ?
C83 Li4 2.712(6) . ?
C84 C85 1.431(5) . ?
C84 C89 1.440(5) . ?
C85 C86 1.360(5) . ?
C86 C87 1.413(6) . ?
C87 C88 1.358(6) . ?
C88 C89 1.439(5) . ?
C89 C90 1.393(5) . ?
C90 C91 1.387(5) . ?
C91 C92 1.437(5) . ?
C91 C96 1.437(5) . ?
C92 C93 1.352(6) . ?
C93 C94 1.423(6) . ?
C94 C95 1.364(5) . ?
C95 C96 1.432(5) . ?
C97 C98 1.347(8) . ?
C97 C102 1.350(8) . ?
C98 C99 1.395(10) . ?
C99 C100 1.342(9) . ?
C100 C101 1.347(8) . ?
C101 C102 1.348(7) . ?
C103 C104 1.311(9) . ?
C103 C108 1.334(10) . ?
C104 C105 1.372(8) . ?
C105 C106 1.373(9) . ?
C106 C107 1.367(9) . ?
C107 C108 1.373(10) . ?
Li1 Li2 3.203(7) . ?
Li1 Li3 3.242(7) . ?
Li1 Li5 2.581(7) . ?
Li1 Li6 2.605(7) . ?
Li2 Li3 3.193(7) . ?
Li2 Li4 2.592(7) . ?
Li2 Li6 2.588(7) . ?
Li3 Li4 2.561(7) . ?
Li3 Li5 2.587(7) . ?
Li4 Li5 3.252(7) . ?
Li4 Li6 3.205(7) . ?
Li5 Li6 3.200(7) . ?

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
C1 O1 Li1 128.0(2) . . ?
C1 O1 Li2 112.1(2) . . ?
C1 O1 Li6 121.8(2) . . ?
Li1 O1 Li2 114.6(2) . . ?
Li1 O1 Li6 85.6(2) . . ?
Li2 O1 Li6 83.1(2) . . ?
C17 O2 Li2 129.7(2) . . ?
C17 O2 Li3 109.6(2) . . ?
C17 O2 Li4 123.4(2) . . ?
Li2 O2 Li3 115.0(2) . . ?
Li2 O2 Li4 85.3(2) . . ?
Li3 O2 Li4 82.3(2) . . ?
C33 O3 Li1 112.5(2) . . ?
C33 O3 Li3 127.2(2) . . ?
C33 O3 Li5 122.1(2) . . ?
Li1 O3 Li5 82.9(2) . . ?
Li3 O3 Li1 115.8(2) . . ?
Li3 O3 Li5 84.3(2) . . ?
C49 O4 Li3 124.9(2) . . ?
C49 O4 Li4 127.0(2) . . ?
C49 O4 Li5 110.9(2) . . ?
Li4 O4 Li3 83.4(2) . . ?
Li4 O4 Li5 116.7(2) . . ?
Li5 O4 Li3 83.4(2) . . ?
C65 O5 Li1 119.2(2) . . ?
C65 O5 Li5 130.2(2) . . ?
C65 O5 Li6 112.5(2) . . ?
Li5 O5 Li1 84.3(2) . . ?
Li5 O5 Li6 113.6(2) . . ?
Li6 O5 Li1 83.0(2) . . ?
C81 O6 Li2 119.9(2) . . ?
C81 O6 Li4 112.2(2) . . ?
C81 O6 Li6 129.9(2) . . ?
Li4 O6 Li2 83.4(2) . . ?
Li6 O6 Li2 84.0(2) . . ?
Li6 O6 Li4 114.0(2) . . ?
O1 C1 C3 112.2(2) . . ?
O1 C1 Li2 40.90(16) . . ?
C2 C1 O1 126.5(3) . . ?
C2 C1 C3 121.3(3) . . ?
C2 C1 Li2 165.4(3) . . ?
C3 C1 Li2 71.80(19) . . ?
C1 C3 Li2 75.93(19) . . ?
C4 C3 C1 121.7(3) . . ?
C4 C3 C16 120.2(3) . . ?
C4 C3 Li2 115.7(2) . . ?
C16 C3 C1 118.1(3) . . ?
C16 C3 Li2 77.0(2) . . ?
C3 C4 C5 122.6(3) . . ?
C3 C4 C9 118.9(3) . . ?
C5 C4 C9 118.5(3) . . ?
C6 C5 C4 120.6(3) . . ?
C5 C6 C7 120.6(4) . . ?
C8 C7 C6 120.7(4) . . ?
C7 C8 C9 121.2(4) . . ?
C8 C9 C4 118.4(3) . . ?
C10 C9 C4 120.1(3) . . ?
C10 C9 C8 121.5(3) . . ?
C9 C10 C11 121.6(3) . . ?
C10 C11 C12 122.6(3) . . ?
C10 C11 C16 118.8(3) . . ?
C16 C11 C12 118.6(3) . . ?
C13 C12 C11 120.7(3) . . ?
C12 C13 C14 120.9(3) . . ?
C15 C14 C13 120.7(4) . . ?
C14 C15 C16 121.0(3) . . ?
C3 C16 C11 120.5(3) . . ?
C3 C16 C15 121.4(3) . . ?
C3 C16 Li2 72.8(2) . . ?
C11 C16 C15 118.1(3) . . ?
C11 C16 Li2 118.3(2) . . ?
C15 C16 Li2 82.1(2) . . ?
O2 C17 C19 112.8(2) . . ?
O2 C17 Li3 42.25(17) . . ?
C18 C17 O2 124.8(3) . . ?
C18 C17 C19 122.4(3) . . ?
C18 C17 Li3 161.8(3) . . ?
C19 C17 Li3 72.16(19) . . ?
C17 C19 Li3 75.58(19) . . ?
C20 C19 C17 121.5(3) . . ?
C20 C19 C32 120.0(3) . . ?
C20 C19 Li3 111.8(2) . . ?
C32 C19 C17 118.4(3) . . ?
C32 C19 Li3 78.8(2) . . ?
C19 C20 C21 122.3(3) . . ?
C19 C20 C25 119.7(3) . . ?
C21 C20 C25 118.0(3) . . ?
C22 C21 C20 120.8(3) . . ?
C21 C22 C23 121.1(4) . . ?
C24 C23 C22 120.6(3) . . ?
C23 C24 C25 120.5(4) . . ?
C24 C25 C20 118.9(3) . . ?
C26 C25 C20 119.1(3) . . ?
C26 C25 C24 121.9(3) . . ?
C27 C26 C25 122.0(3) . . ?
C26 C27 C28 122.6(3) . . ?
C26 C27 C32 119.3(3) . . ?
C32 C27 C28 118.1(3) . . ?
C29 C28 C27 121.5(3) . . ?
C28 C29 C30 120.4(3) . . ?
C31 C30 C29 120.9(3) . . ?
C30 C31 C32 121.0(3) . . ?
C19 C32 C27 119.8(3) . . ?
C19 C32 C31 122.1(3) . . ?
C19 C32 Li3 71.05(19) . . ?
C27 C32 Li3 115.6(2) . . ?
C31 C32 C27 118.1(3) . . ?
C31 C32 Li3 85.3(2) . . ?
O3 C33 C35 112.4(2) . . ?
O3 C33 Li1 40.61(16) . . ?
C34 C33 O3 125.9(3) . . ?
C34 C33 C35 121.6(3) . . ?
C34 C33 Li1 163.1(3) . . ?
C35 C33 Li1 72.71(19) . . ?
C33 C35 Li1 75.41(19) . . ?
C36 C35 C33 120.5(3) . . ?
C36 C35 C48 120.3(3) . . ?
C36 C35 Li1 115.3(2) . . ?
C48 C35 C33 119.1(3) . . ?
C48 C35 Li1 77.0(2) . . ?
C35 C36 C37 122.0(3) . . ?
C35 C36 C41 119.4(3) . . ?
C37 C36 C41 118.6(3) . . ?
C38 C37 C36 121.0(3) . . ?
C37 C38 C39 119.9(4) . . ?
C40 C39 C38 121.1(4) . . ?
C39 C40 C41 121.8(4) . . ?
C40 C41 C36 117.7(3) . . ?
C42 C41 C36 118.9(3) . . ?
C42 C41 C40 123.4(3) . . ?
C43 C42 C41 122.6(3) . . ?
C42 C43 C44 122.9(3) . . ?
C42 C43 C48 118.8(3) . . ?
C44 C43 C48 118.3(3) . . ?
C45 C44 C43 121.3(3) . . ?
C44 C45 C46 120.3(4) . . ?
C47 C46 C45 121.0(4) . . ?
C46 C47 C48 121.3(3) . . ?
C35 C48 C43 119.9(3) . . ?
C35 C48 C47 122.3(3) . . ?
C35 C48 Li1 73.04(19) . . ?
C43 C48 Li1 118.2(2) . . ?
C47 C48 C43 117.8(3) . . ?
C47 C48 Li1 81.4(2) . . ?
O4 C49 C51 112.5(2) . . ?
O4 C49 Li5 41.60(17) . . ?
C50 C49 O4 126.6(3) . . ?
C50 C49 C51 120.9(3) . . ?
C50 C49 Li5 165.9(3) . . ?
C51 C49 Li5 71.43(19) . . ?
C49 C51 Li5 75.9(2) . . ?
C52 C51 C49 120.7(3) . . ?
C52 C51 C64 120.2(3) . . ?
C52 C51 Li5 112.0(2) . . ?
C64 C51 C49 119.1(3) . . ?
C64 C51 Li5 80.3(2) . . ?
C51 C52 C53 122.4(3) . . ?
C51 C52 C57 119.5(3) . . ?
C53 C52 C57 118.0(3) . . ?
C54 C53 C52 121.3(4) . . ?
C53 C54 C55 120.2(4) . . ?
C56 C55 C54 120.9(4) . . ?
C55 C56 C57 122.0(4) . . ?
C56 C57 C52 117.6(4) . . ?
C58 C57 C52 118.9(3) . . ?
C58 C57 C56 123.5(4) . . ?
C57 C58 C59 122.8(3) . . ?
C58 C59 C60 123.2(4) . . ?
C58 C59 C64 118.7(3) . . ?
C60 C59 C64 118.1(4) . . ?
C61 C60 C59 122.0(4) . . ?
C60 C61 C62 121.0(4) . . ?
C63 C62 C61 119.1(4) . . ?
C62 C63 C64 121.6(4) . . ?
C51 C64 C59 119.9(3) . . ?
C51 C64 C63 122.0(3) . . ?
C51 C64 Li5 69.7(2) . . ?
C59 C64 Li5 118.8(2) . . ?
C63 C64 C59 118.2(3) . . ?
C63 C64 Li5 84.3(2) . . ?
O5 C65 C67 112.5(2) . . ?
O5 C65 Li6 40.77(16) . . ?
C66 C65 O5 125.2(3) . . ?
C66 C65 C67 122.3(3) . . ?
C66 C65 Li6 162.1(3) . . ?
C67 C65 Li6 72.90(19) . . ?
C65 C67 Li6 75.57(19) . . ?
C68 C67 C65 121.9(3) . . ?
C68 C67 Li6 119.5(2) . . ?
C80 C67 C65 118.2(3) . . ?
C80 C67 C68 119.8(3) . . ?
C80 C67 Li6 71.85(19) . . ?
C67 C68 C69 122.1(3) . . ?
C67 C68 C73 119.1(3) . . ?
C69 C68 C73 118.8(3) . . ?
C70 C69 C68 120.5(4) . . ?
C69 C70 C71 120.5(4) . . ?
C72 C71 C70 120.8(3) . . ?
C71 C72 C73 120.8(4) . . ?
C72 C73 C68 118.7(3) . . ?
C74 C73 C68 120.1(3) . . ?
C74 C73 C72 121.2(3) . . ?
C73 C74 C75 122.1(3) . . ?
C74 C75 C76 122.5(3) . . ?
C74 C75 C80 118.1(3) . . ?
C76 C75 C80 119.4(3) . . ?
C77 C76 C75 121.0(3) . . ?
C76 C77 C78 120.0(3) . . ?
C79 C78 C77 121.6(3) . . ?
C78 C79 C80 120.5(3) . . ?
C78 C79 Li6 118.6(3) . . ?
C80 C79 Li6 72.05(19) . . ?
C67 C80 C75 120.8(3) . . ?
C67 C80 C79 121.8(3) . . ?
C67 C80 Li6 77.9(2) . . ?
C75 C80 Li6 117.8(2) . . ?
C79 C80 C75 117.4(3) . . ?
C79 C80 Li6 77.0(2) . . ?
O6 C81 C83 113.5(2) . . ?
O6 C81 Li4 40.74(16) . . ?
C82 C81 O6 125.7(3) . . ?
C82 C81 C83 120.7(3) . . ?
C82 C81 Li4 165.0(3) . . ?
C83 C81 Li4 73.15(19) . . ?
C81 C83 Li4 74.78(19) . . ?
C84 C83 C81 121.6(3) . . ?
C84 C83 C96 119.9(3) . . ?
C84 C83 Li4 113.8(2) . . ?
C96 C83 C81 118.3(3) . . ?
C96 C83 Li4 78.2(2) . . ?
C83 C84 C85 122.2(3) . . ?
C83 C84 C89 119.7(3) . . ?
C85 C84 C89 118.1(3) . . ?
C86 C85 C84 120.9(3) . . ?
C85 C86 C87 121.0(4) . . ?
C88 C87 C86 120.8(3) . . ?
C87 C88 C89 120.3(3) . . ?
C88 C89 C84 118.9(3) . . ?
C90 C89 C84 119.4(3) . . ?
C90 C89 C88 121.7(3) . . ?
C91 C90 C89 121.8(3) . . ?
C90 C91 C92 122.6(3) . . ?
C90 C91 C96 119.6(3) . . ?
C96 C91 C92 117.9(3) . . ?
C93 C92 C91 122.0(3) . . ?
C92 C93 C94 120.0(3) . . ?
C95 C94 C93 120.4(4) . . ?
C94 C95 C96 121.2(3) . . ?
C83 C96 C91 119.6(3) . . ?
C83 C96 C95 122.0(3) . . ?
C95 C96 C91 118.4(3) . . ?
C98 C97 C102 120.3(5) . . ?
C97 C98 C99 119.0(5) . . ?
C100 C99 C98 119.8(5) . . ?
C99 C100 C101 120.1(5) . . ?
C100 C101 C102 120.6(5) . . ?
C101 C102 C97 120.3(5) . . ?
C104 C103 C108 120.8(6) . . ?
C103 C104 C105 120.5(6) . . ?
C104 C105 C106 119.5(6) . . ?
C107 C106 C105 119.4(5) . . ?
C106 C107 C108 118.2(6) . . ?
C103 C108 C107 121.4(6) . . ?
O1 Li1 O3 123.1(3) . . ?
O1 Li1 O5 96.7(2) . . ?
O1 Li1 C33 141.2(3) . . ?
O1 Li1 C35 153.2(3) . . ?
O1 Li1 C48 125.4(3) . . ?
O1 Li1 Li2 33.37(14) . . ?
O1 Li1 Li3 92.6(2) . . ?
O1 Li1 Li5 116.2(2) . . ?
O1 Li1 Li6 48.76(17) . . ?
O3 Li1 O5 95.0(2) . . ?
O3 Li1 C33 26.87(11) . . ?
O3 Li1 C35 58.37(15) . . ?
O3 Li1 C48 80.12(19) . . ?
O3 Li1 Li2 90.6(2) . . ?
O3 Li1 Li3 31.67(13) . . ?
O3 Li1 Li5 49.04(17) . . ?
O3 Li1 Li6 114.4(2) . . ?
O5 Li1 C33 106.8(2) . . ?
O5 Li1 C35 110.0(2) . . ?
O5 Li1 C48 132.9(2) . . ?
O5 Li1 Li2 93.3(2) . . ?
O5 Li1 Li3 91.0(2) . . ?
O5 Li1 Li5 46.06(17) . . ?
O5 Li1 Li6 48.17(17) . . ?
C33 Li1 C48 54.27(13) . . ?
C33 Li1 Li2 113.22(19) . . ?
C33 Li1 Li3 57.37(14) . . ?
C35 Li1 C33 31.88(10) . . ?
C35 Li1 C48 29.96(11) . . ?
C35 Li1 Li2 141.6(2) . . ?
C35 Li1 Li3 89.25(18) . . ?
C48 Li1 Li2 133.2(2) . . ?
C48 Li1 Li3 105.65(19) . . ?
Li2 Li1 Li3 59.39(16) . . ?
Li5 Li1 C33 66.14(17) . . ?
Li5 Li1 C35 85.4(2) . . ?
Li5 Li1 C48 115.2(2) . . ?
Li5 Li1 Li2 90.1(2) . . ?
Li5 Li1 Li3 51.24(17) . . ?
Li5 Li1 Li6 76.2(2) . . ?
Li6 Li1 C33 139.8(2) . . ?
Li6 Li1 C35 158.0(3) . . ?
Li6 Li1 C48 165.4(2) . . ?
Li6 Li1 Li2 51.68(17) . . ?
Li6 Li1 Li3 88.52(19) . . ?
O1 Li2 O6 95.4(2) . . ?
O1 Li2 C1 26.98(11) . . ?
O1 Li2 C3 59.05(16) . . ?
O1 Li2 C16 79.88(19) . . ?
O1 Li2 Li1 32.05(14) . . ?
O1 Li2 Li3 92.8(2) . . ?
O1 Li2 Li4 115.9(3) . . ?
O1 Li2 Li6 48.90(17) . . ?
O2 Li2 O1 124.9(3) . . ?
O2 Li2 O6 96.4(2) . . ?
O2 Li2 C1 143.5(3) . . ?
O2 Li2 C3 152.8(3) . . ?
O2 Li2 C16 123.7(3) . . ?
O2 Li2 Li1 93.6(2) . . ?
O2 Li2 Li3 33.16(15) . . ?
O2 Li2 Li4 49.04(17) . . ?
O2 Li2 Li6 116.4(3) . . ?
O6 Li2 C1 106.5(2) . . ?
O6 Li2 C3 110.4(2) . . ?
O6 Li2 C16 134.4(3) . . ?
O6 Li2 Li1 93.0(2) . . ?
O6 Li2 Li3 92.4(2) . . ?
O6 Li2 Li4 47.58(17) . . ?
O6 Li2 Li6 46.71(17) . . ?
C1 Li2 Li1 57.69(14) . . ?
C1 Li2 Li3 116.1(2) . . ?
C3 Li2 C1 32.28(11) . . ?
C3 Li2 C16 30.17(11) . . ?
C3 Li2 Li1 89.85(18) . . ?
C3 Li2 Li3 144.3(2) . . ?
C16 Li2 C1 54.44(13) . . ?
C16 Li2 Li1 104.09(19) . . ?
C16 Li2 Li3 132.9(2) . . ?
Li3 Li2 Li1 60.90(16) . . ?
Li4 Li2 C1 140.9(2) . . ?
Li4 Li2 C3 158.0(3) . . ?
Li4 Li2 C16 164.2(2) . . ?
Li4 Li2 Li1 91.0(2) . . ?
Li4 Li2 Li3 51.27(17) . . ?
Li6 Li2 C1 66.00(18) . . ?
Li6 Li2 C3 86.8(2) . . ?
Li6 Li2 C16 116.6(2) . . ?
Li6 Li2 Li1 52.15(16) . . ?
Li6 Li2 Li3 89.9(2) . . ?
Li6 Li2 Li4 76.4(2) . . ?
O2 Li3 O4 96.6(2) . . ?
O2 Li3 C17 28.12(11) . . ?
O2 Li3 C19 59.70(16) . . ?
O2 Li3 C32 81.72(19) . . ?
O2 Li3 Li1 91.2(2) . . ?
O2 Li3 Li2 31.85(14) . . ?
O2 Li3 Li4 49.47(17) . . ?
O2 Li3 Li5 116.5(3) . . ?
O3 Li3 O2 122.2(3) . . ?
O3 Li3 O4 96.8(2) . . ?
O3 Li3 C17 139.6(3) . . ?
O3 Li3 C19 151.8(3) . . ?
O3 Li3 C32 123.8(2) . . ?
O3 Li3 Li1 32.53(14) . . ?
O3 Li3 Li2 91.7(2) . . ?
O3 Li3 Li4 117.4(3) . . ?
O3 Li3 Li5 49.07(17) . . ?
O4 Li3 C17 109.9(2) . . ?
O4 Li3 C19 111.2(2) . . ?
O4 Li3 C32 133.2(3) . . ?
O4 Li3 Li1 91.8(2) . . ?
O4 Li3 Li2 92.1(2) . . ?
O4 Li3 Li4 47.16(17) . . ?
O4 Li3 Li5 47.83(17) . . ?
C17 Li3 C32 54.34(13) . . ?
C17 Li3 Li1 114.5(2) . . ?
C17 Li3 Li2 58.54(15) . . ?
C19 Li3 C17 32.26(11) . . ?
C19 Li3 C32 30.19(11) . . ?
C19 Li3 Li1 143.8(2) . . ?
C19 Li3 Li2 90.79(18) . . ?
C32 Li3 Li1 134.9(2) . . ?
C32 Li3 Li2 107.5(2) . . ?
Li2 Li3 Li1 59.71(16) . . ?
Li4 Li3 C17 67.72(18) . . ?
Li4 Li3 C19 85.8(2) . . ?
Li4 Li3 C32 115.9(2) . . ?
Li4 Li3 Li1 90.7(2) . . ?
Li4 Li3 Li2 52.15(17) . . ?
Li4 Li3 Li5 78.3(2) . . ?
Li5 Li3 C17 143.5(2) . . ?
Li5 Li3 C19 159.0(3) . . ?
Li5 Li3 C32 161.7(3) . . ?
Li5 Li3 Li1 51.07(17) . . ?
Li5 Li3 Li2 90.2(2) . . ?
O2 Li4 C81 104.9(2) . . ?
O2 Li4 C83 109.2(2) . . ?
O2 Li4 Li2 45.63(17) . . ?
O2 Li4 Li3 48.21(17) . . ?
O2 Li4 Li5 91.9(2) . . ?
O2 Li4 Li6 91.4(2) . . ?
O4 Li4 O2 97.6(2) . . ?
O4 Li4 O6 122.5(3) . . ?
O4 Li4 C81 142.0(3) . . ?
O4 Li4 C83 153.2(3) . . ?
O4 Li4 Li2 115.3(2) . . ?
O4 Li4 Li3 49.39(17) . . ?
O4 Li4 Li5 32.03(14) . . ?
O4 Li4 Li6 90.9(2) . . ?
O6 Li4 O2 94.4(2) . . ?
O6 Li4 C81 27.09(11) . . ?
O6 Li4 C83 59.02(15) . . ?
O6 Li4 Li2 49.06(17) . . ?
O6 Li4 Li3 116.1(3) . . ?
O6 Li4 Li5 91.9(2) . . ?
O6 Li4 Li6 32.68(14) . . ?
C81 Li4 Li5 115.9(2) . . ?
C81 Li4 Li6 58.78(14) . . ?
C83 Li4 C81 32.08(10) . . ?
C83 Li4 Li5 144.4(2) . . ?
C83 Li4 Li6 90.76(18) . . ?
Li2 Li4 C81 65.60(17) . . ?
Li2 Li4 C83 86.29(19) . . ?
Li2 Li4 Li5 88.85(19) . . ?
Li2 Li4 Li6 51.73(17) . . ?
Li3 Li4 C81 140.8(2) . . ?
Li3 Li4 C83 157.4(3) . . ?
Li3 Li4 Li2 76.6(2) . . ?
Li3 Li4 Li5 51.19(17) . . ?
Li3 Li4 Li6 90.1(2) . . ?
Li6 Li4 Li5 59.41(16) . . ?
O3 Li5 C49 108.8(2) . . ?
O3 Li5 C51 114.6(2) . . ?
O3 Li5 C64 139.0(3) . . ?
O3 Li5 Li1 48.11(17) . . ?
O3 Li5 Li3 46.64(17) . . ?
O3 Li5 Li4 90.7(2) . . ?
O3 Li5 Li6 92.8(2) . . ?
O4 Li5 O3 95.3(2) . . ?
O4 Li5 C49 27.51(11) . . ?
O4 Li5 C51 59.93(16) . . ?
O4 Li5 C64 80.55(19) . . ?
O4 Li5 Li1 115.9(3) . . ?
O4 Li5 Li3 48.72(17) . . ?
O4 Li5 Li4 31.30(14) . . ?
O4 Li5 Li6 90.3(2) . . ?
O5 Li5 O3 97.6(2) . . ?
O5 Li5 O4 123.1(3) . . ?
O5 Li5 C49 139.6(3) . . ?
O5 Li5 C51 147.5(3) . . ?
O5 Li5 C64 118.9(2) . . ?
O5 Li5 Li1 49.65(18) . . ?
O5 Li5 Li3 117.5(3) . . ?
O5 Li5 Li4 93.3(2) . . ?
O5 Li5 Li6 34.07(15) . . ?
C49 Li5 C64 54.51(13) . . ?
C49 Li5 Li4 57.38(14) . . ?
C49 Li5 Li6 112.73(19) . . ?
C51 Li5 C49 32.66(11) . . ?
C51 Li5 C64 29.99(11) . . ?
C51 Li5 Li4 89.94(18) . . ?
C51 Li5 Li6 139.9(2) . . ?
C64 Li5 Li4 104.08(19) . . ?
C64 Li5 Li6 127.8(2) . . ?
Li1 Li5 C49 142.4(2) . . ?
Li1 Li5 C51 162.7(3) . . ?
Li1 Li5 C64 163.0(2) . . ?
Li1 Li5 Li3 77.7(2) . . ?
Li1 Li5 Li4 90.1(2) . . ?
Li1 Li5 Li6 52.24(17) . . ?
Li3 Li5 C49 67.27(18) . . ?
Li3 Li5 C51 89.1(2) . . ?
Li3 Li5 C64 118.5(2) . . ?
Li3 Li5 Li4 50.47(17) . . ?
Li3 Li5 Li6 89.7(2) . . ?
Li6 Li5 Li4 59.56(15) . . ?
O1 Li6 C65 104.2(2) . . ?
O1 Li6 C67 104.8(2) . . ?
O1 Li6 C79 157.5(3) . . ?
O1 Li6 C80 126.6(2) . . ?
O1 Li6 Li1 45.69(16) . . ?
O1 Li6 Li2 48.00(17) . . ?
O1 Li6 Li4 93.3(2) . . ?
O1 Li6 Li5 91.4(2) . . ?
O5 Li6 O1 94.3(2) . . ?
O5 Li6 C65 26.73(11) . . ?
O5 Li6 C67 57.79(15) . . ?
O5 Li6 C79 81.5(2) . . ?
O5 Li6 C80 80.6(2) . . ?
O5 Li6 Li1 48.87(17) . . ?
O5 Li6 Li2 115.6(2) . . ?
O5 Li6 Li4 93.1(2) . . ?
O5 Li6 Li5 32.34(14) . . ?
O6 Li6 O1 97.0(2) . . ?
O6 Li6 O5 125.5(3) . . ?
O6 Li6 C65 144.9(3) . . ?
O6 Li6 C67 157.7(3) . . ?
O6 Li6 C79 103.5(2) . . ?
O6 Li6 C80 129.1(2) . . ?
O6 Li6 Li1 116.8(3) . . ?
O6 Li6 Li2 49.25(17) . . ?
O6 Li6 Li4 33.31(14) . . ?
O6 Li6 Li5 94.1(2) . . ?
C65 Li6 Li4 116.6(2) . . ?
C65 Li6 Li5 58.16(15) . . ?
C67 Li6 C65 31.53(11) . . ?
C67 Li6 Li4 146.1(2) . . ?
C67 Li6 Li5 89.67(18) . . ?
C79 Li6 C65 63.18(15) . . ?
C79 Li6 C67 54.27(13) . . ?
C79 Li6 Li4 108.9(2) . . ?
C79 Li6 Li5 96.28(19) . . ?
C80 Li6 C65 54.66(14) . . ?
C80 Li6 C67 30.28(11) . . ?
C80 Li6 C79 30.98(11) . . ?
C80 Li6 Li4 139.8(2) . . ?
C80 Li6 Li5 107.9(2) . . ?
Li1 Li6 C65 64.89(17) . . ?
Li1 Li6 C67 82.47(19) . . ?
Li1 Li6 C79 127.9(2) . . ?
Li1 Li6 C80 112.8(2) . . ?
Li1 Li6 Li4 90.7(2) . . ?
Li1 Li6 Li5 51.57(17) . . ?
Li2 Li6 C65 139.7(2) . . ?
Li2 Li6 C67 152.8(2) . . ?
Li2 Li6 C79 152.5(2) . . ?
Li2 Li6 C80 161.8(3) . . ?
Li2 Li6 Li1 76.2(2) . . ?
Li2 Li6 Li4 51.84(17) . . ?
Li2 Li6 Li5 90.1(2) . . ?
Li5 Li6 Li4 61.03(15) . . ?

_shelx_SHELXL_version_number     2019/1
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.286
_oxdiff_exptl_absorpt_empirical_full_min 0.658
####################################################################### 
# 
# 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_elu230006_fa
_database_code_depnum_ccdc_archive 'CCDC 2307289'
loop_
_audit_author_name
_audit_author_address
'Paul G. Waddell'
;School of Natural and Environmental Sciences, Newcastle University
United Kingdom
;
_audit_update_record             
;
2023-11-11 deposited with the CCDC.	2024-02-12 downloaded from the CCDC.
;
_audit_creation_date             2023-03-03
_audit_creation_method           
;
Olex2 1.5-ac5-023
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C28 H41 Li N4 O), C7 H8'
_chemical_formula_sum            'C63 H90 Li2 N8 O2'
_chemical_formula_weight         1005.30
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C32 H53 Li1 N4 O1 Si1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   12.4692(2)
_cell_length_b                   17.6687(4)
_cell_length_c                   13.5637(2)
_cell_angle_alpha                90
_cell_angle_beta                 95.153(2)
_cell_angle_gamma                90
_cell_volume                     2976.20(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      77.6440
_cell_measurement_theta_min      4.1110
_shelx_estimated_absorpt_T_max   0.945
_shelx_estimated_absorpt_T_min   0.894
_exptl_absorpt_coefficient_mu    0.519
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1092
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.0565
0 1 0 0.0505
0 0 -1 0.1048
0 0 1 0.0758
-1 0 1 0.0811
1 0 -1 0.0821
1 -1 0 0.0793
-1 1 0 0.0943
-1 -1 -1 0.1186
0 -1 -1 0.0932
0 1 1 0.0682
1 0 0 0.0990
-1 0 0 0.1220
1 1 1 0.0856
-1 0 -1 0.1243
1 0 1 0.0953
1 1 -1 0.0827
-1 -1 1 0.0817
-1 2 1 0.0670
1 -2 -1 0.0800
0 -2 1 0.0752

_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0000 -1.0000 0.0000 -0.0061 -0.0861 0.0124
-0.0000 1.0000 -0.0000 0.0061 0.0861 -0.0124
-0.0000 0.0000 -1.0000 -0.1000 0.0147 0.0528
0.0000 -0.0000 1.0000 0.1000 -0.0147 -0.0528
-1.0000 0.0000 1.0000 0.1492 -0.0018 0.0602
1.0000 -0.0000 -1.0000 -0.1492 0.0018 -0.0602
1.0000 -1.0000 0.0000 -0.0552 -0.0990 -0.1006
-1.0000 1.0000 -0.0000 0.0552 0.0990 0.1006
-1.0000 -1.0000 -1.0000 -0.0570 -0.0586 0.1783
-0.0000 -1.0000 -1.0000 -0.1061 -0.0715 0.0652
0.0000 1.0000 1.0000 0.1061 0.0715 -0.0652
1.0000 -0.0000 0.0000 -0.0491 -0.0129 -0.1130
-1.0000 0.0000 -0.0000 0.0491 0.0129 0.1130
1.0000 1.0000 1.0000 0.0570 0.0586 -0.1783
-1.0000 0.0000 -1.0000 -0.0509 0.0276 0.1659
1.0000 -0.0000 1.0000 0.0509 -0.0276 -0.1659
1.0000 1.0000 -1.0000 -0.1431 0.0879 -0.0726
-1.0000 -1.0000 1.0000 0.1431 -0.0879 0.0726
-1.0000 2.0000 1.0000 0.1613 0.1705 0.0354
1.0000 -2.0000 -1.0000 -0.1613 -0.1705 -0.0354
0.0000 -2.0000 1.0000 0.0878 -0.1870 -0.0280

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23333
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.316
_diffrn_reflns_theta_min         4.119
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -51.00 -17.00   0.50    1.17    --  -92.01  45.00-120.00   68
  2  ω    -25.00  29.00   0.50    1.17    --  -49.76  19.00-120.00  108
  3  ω    -27.00  29.00   0.50    1.17    --  -49.76  19.00 -60.00  112
  4  ω    -27.00  29.00   0.50    1.17    --  -49.76  19.00   0.00  112
  5  ω    -45.00 -17.00   0.50    1.17    --  -92.01  45.00 -90.00   56
  6  ω    -46.00 -21.00   0.50    1.17    --  -92.01  45.00 -30.00   50
  7  ω    -51.00 -20.00   0.50    1.17    --  -92.01  45.00   0.00   62
  8  ω   -109.00 -46.00   0.50    1.17    --  -92.01 117.00 129.00  126
  9  ω    -77.00 -52.00   0.50    1.17    --  -49.76 117.00 129.00   50
 10  ω   -145.00-120.00   0.50    1.17    --  -92.01-117.00  42.00   50
 11  ω    -89.00 -61.00   0.50    1.17    --  -49.76-162.00-107.00   56
 12  ω   -137.00 -51.00   0.50    1.17    --  -92.01-162.00-107.00  172
 13  ω     41.00 129.00   0.50    1.17    --  108.00-162.00-107.00  176
 14  ω     29.00 110.00   0.50    1.17    --   96.11-125.00 -60.00  162
 15  ω     46.00  98.00   0.50    1.17    --   48.76-117.00  42.00  104
 16  ω     49.00  74.00   0.50    1.17    --  108.00-117.00  42.00   50
 17  ω     59.00 106.00   0.50    1.17    --  108.00 -95.00  30.00   94
 18  ω     35.00  67.00   0.50    1.17    --  108.00 -61.00  30.00   64
 19  ω     45.00  70.00   0.50    1.17    --  108.00 -61.00  90.00   50
 20  ω     26.00  51.00   0.50    1.17    --   96.11 -45.00 120.00   50
 21  ω     25.00  51.00   0.50    1.17    --   96.11 -45.00 -60.00   52
 22  ω     18.00  51.00   0.50    1.17    --   96.11 -45.00-120.00   66
 23  ω     22.00  48.00   0.50    1.17    --   96.11 -45.00-180.00   52
 24  ω     36.00  61.00   0.50    1.17    --  108.00 -61.00-150.00   50
 25  ω     21.00  49.00   0.50    1.17    --   96.11 -45.00 -90.00   56
 26  ω     99.00 124.00   0.50    1.17    --   96.11 117.00 129.00   50
 27  ω     74.00  99.00   0.50    1.17    --   48.76 125.00 -30.00   50
 28  ω     54.00  83.00   0.50    1.17    --   48.76 162.00 -80.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix-Arc 100'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0491381000
_diffrn_orient_matrix_UB_12      0.0060871000
_diffrn_orient_matrix_UB_13      0.1000204000
_diffrn_orient_matrix_UB_21      -0.0128987000
_diffrn_orient_matrix_UB_22      0.0861471000
_diffrn_orient_matrix_UB_23      -0.0146945000
_diffrn_orient_matrix_UB_31      -0.1130346000
_diffrn_orient_matrix_UB_32      -0.0124049000
_diffrn_orient_matrix_UB_33      -0.0528268000
_diffrn_oxdiff_digest_frames     
;
0191e215742374f4b43aca3b51fc1248b102206fc18
;
_diffrn_oxdiff_digest_hkl        
;
01725a1c67b32592baed3b878ff070787b748e
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4825
_reflns_number_total             5969
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.139
_refine_diff_density_rms         0.031
_refine_ls_extinction_coef       0.00110(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         5969
_refine_ls_number_restraints     408
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0402
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0507P)²+0.4827P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1107
_refine_special_details          
;
The asymmetric unit contains a half a molecule of toluene 
modelled as disordered over a centre of symmetry. 
Accordingly, the solvent molecule was modelled in a 
negative part with an occupancy constrained to be a half. 
The atomic displacement parameters of all partially-
occupied non-hydrogen atoms were restrained using the 
SIMU card.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C29(0.5) C30(0.5) H30(0.5) C31(0.5) H31(0.5) C32(0.5) H32(0.5)
 C33(0.5) H33(0.5) C34(0.5) H34(0.5) C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
5.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C24(H24), C25(H25),
 C26(H26), C27(H27), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34)
5.c X=CH2 refined with riding coordinates:
 C14(H14A,H14B)
5.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C35(H35A,H35B,H35C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
O1 O 0.21640(7) 0.70767(5) 0.64755(6) 0.0466(2) Uani 1 1 d . . . . .
N1 N 0.05046(8) 0.58746(6) 0.85155(7) 0.0445(3) Uani 1 1 d . . . . .
N2 N 0.16339(8) 0.53320(6) 0.68643(7) 0.0415(2) Uani 1 1 d . . . . .
N3 N 0.23498(8) 0.68438(6) 0.87637(7) 0.0413(2) Uani 1 1 d . . . . .
N4 N -0.02150(8) 0.69633(6) 0.70166(7) 0.0430(2) Uani 1 1 d . . . . .
C1 C 0.07822(13) 0.50737(8) 0.84121(10) 0.0561(4) Uani 1 1 d . . . . .
H1A H 0.022605 0.475741 0.868822 0.067 Uiso 1 1 calc R U . . .
H1B H 0.147871 0.497128 0.879871 0.067 Uiso 1 1 calc R U . . .
C2 C 0.08652(12) 0.48547(8) 0.73386(10) 0.0513(3) Uani 1 1 d . . . . .
H2A H 0.109393 0.431936 0.730776 0.062 Uiso 1 1 calc R U . . .
H2B H 0.014653 0.490012 0.696886 0.062 Uiso 1 1 calc R U . . .
C3 C 0.08848(11) 0.61769(9) 0.94936(9) 0.0524(3) Uani 1 1 d . . . . .
H3A H 0.074212 0.580166 1.000787 0.063 Uiso 1 1 calc R U . . .
H3B H 0.047707 0.664256 0.961958 0.063 Uiso 1 1 calc R U . . .
C4 C 0.20725(11) 0.63567(9) 0.95714(9) 0.0500(3) Uani 1 1 d . . . . .
H4A H 0.227665 0.661125 1.021102 0.060 Uiso 1 1 calc R U . . .
H4B H 0.248718 0.587947 0.955907 0.060 Uiso 1 1 calc R U . . .
C5 C -0.06457(11) 0.60232(9) 0.82666(10) 0.0560(4) Uani 1 1 d . . . . .
H5A H -0.103503 0.595740 0.886556 0.067 Uiso 1 1 calc R U . . .
H5B H -0.093786 0.565241 0.776510 0.067 Uiso 1 1 calc R U . . .
C6 C -0.08334(10) 0.68170(9) 0.78667(10) 0.0539(4) Uani 1 1 d . . . . .
H6A H -0.160981 0.688666 0.766423 0.065 Uiso 1 1 calc R U . . .
H6B H -0.062282 0.718763 0.839644 0.065 Uiso 1 1 calc R U . . .
C7 C 0.27400(11) 0.51579(9) 0.72360(11) 0.0557(4) Uani 1 1 d . . . . .
H7A H 0.282879 0.523489 0.795423 0.084 Uiso 1 1 calc R U . . .
H7B H 0.323390 0.549203 0.691889 0.084 Uiso 1 1 calc R U . . .
H7C H 0.290066 0.462977 0.708472 0.084 Uiso 1 1 calc R U . . .
C8 C 0.15238(12) 0.52154(8) 0.57927(9) 0.0517(3) Uani 1 1 d . . . . .
H8A H 0.166670 0.468357 0.564674 0.078 Uiso 1 1 calc R U . . .
H8B H 0.204038 0.553784 0.548608 0.078 Uiso 1 1 calc R U . . .
H8C H 0.079061 0.534679 0.552699 0.078 Uiso 1 1 calc R U . . .
C9 C 0.35104(11) 0.68546(10) 0.86898(11) 0.0620(4) Uani 1 1 d . . . . .
H9A H 0.387202 0.708138 0.928988 0.093 Uiso 1 1 calc R U . . .
H9B H 0.366809 0.715380 0.811187 0.093 Uiso 1 1 calc R U . . .
H9C H 0.377031 0.633577 0.861811 0.093 Uiso 1 1 calc R U . . .
C10 C 0.19864(12) 0.76181(8) 0.88914(11) 0.0556(4) Uani 1 1 d . . . . .
H10A H 0.120542 0.762147 0.893036 0.083 Uiso 1 1 calc R U . . .
H10B H 0.216334 0.792550 0.832683 0.083 Uiso 1 1 calc R U . . .
H10C H 0.234592 0.782848 0.950301 0.083 Uiso 1 1 calc R U . . .
C11 C -0.01773(13) 0.77719(9) 0.67968(11) 0.0592(4) Uani 1 1 d . . . . .
H11A H -0.090724 0.795614 0.660314 0.089 Uiso 1 1 calc R U . . .
H11B H 0.027667 0.785620 0.625356 0.089 Uiso 1 1 calc R U . . .
H11C H 0.012394 0.804582 0.738616 0.089 Uiso 1 1 calc R U . . .
C12 C -0.06757(12) 0.65690(9) 0.61305(10) 0.0569(4) Uani 1 1 d . . . . .
H12A H -0.070930 0.602517 0.626613 0.085 Uiso 1 1 calc R U . . .
H12B H -0.022354 0.665669 0.558684 0.085 Uiso 1 1 calc R U . . .
H12C H -0.140321 0.676091 0.594447 0.085 Uiso 1 1 calc R U . . .
C13 C 0.28130(9) 0.74390(7) 0.59635(8) 0.0350(2) Uani 1 1 d . . . . .
C14 C 0.30965(13) 0.81676(8) 0.60644(11) 0.0582(4) Uani 1 1 d . . . . .
H14A H 0.280825 0.847036 0.655571 0.070 Uiso 1 1 calc R U . . .
H14B H 0.358602 0.838193 0.564458 0.070 Uiso 1 1 calc R U . . .
C15 C 0.32700(9) 0.69640(6) 0.51710(8) 0.0321(2) Uani 1 1 d . . . . .
C16 C 0.26225(9) 0.67952(6) 0.42974(8) 0.0339(2) Uani 1 1 d . . . . .
C17 C 0.15703(10) 0.71033(7) 0.40988(9) 0.0425(3) Uani 1 1 d . . . . .
H17 H 0.129379 0.743282 0.456817 0.051 Uiso 1 1 calc R U . . .
C18 C 0.09549(11) 0.69343(9) 0.32497(10) 0.0542(3) Uani 1 1 d . . . . .
H18 H 0.025050 0.713999 0.313793 0.065 Uiso 1 1 calc R U . . .
C19 C 0.13512(13) 0.64565(9) 0.25323(10) 0.0585(4) Uani 1 1 d . . . . .
H19 H 0.092097 0.635463 0.193303 0.070 Uiso 1 1 calc R U . . .
C20 C 0.23371(12) 0.61440(8) 0.26931(9) 0.0523(3) Uani 1 1 d . . . . .
H20 H 0.258857 0.581826 0.220639 0.063 Uiso 1 1 calc R U . . .
C21 C 0.30121(10) 0.62917(7) 0.35787(8) 0.0394(3) Uani 1 1 d . . . . .
C22 C 0.40231(10) 0.59680(7) 0.37687(9) 0.0440(3) Uani 1 1 d . . . . .
H22 H 0.427435 0.562791 0.329811 0.053 Uiso 1 1 calc R U . . .
C23 C 0.46791(10) 0.61262(7) 0.46261(9) 0.0400(3) Uani 1 1 d . . . . .
C24 C 0.57075(11) 0.57808(8) 0.48405(12) 0.0521(3) Uani 1 1 d . . . . .
H24 H 0.596142 0.543416 0.437925 0.062 Uiso 1 1 calc R U . . .
C25 C 0.63274(11) 0.59348(9) 0.56822(13) 0.0585(4) Uani 1 1 d . . . . .
H25 H 0.700668 0.569372 0.580952 0.070 Uiso 1 1 calc R U . . .
C26 C 0.59721(11) 0.64527(9) 0.63754(11) 0.0573(4) Uani 1 1 d . . . . .
H26 H 0.641956 0.656597 0.696097 0.069 Uiso 1 1 calc R U . . .
C27 C 0.49936(10) 0.67899(8) 0.62093(9) 0.0466(3) Uani 1 1 d . . . . .
H27 H 0.476471 0.713393 0.668627 0.056 Uiso 1 1 calc R U . . .
C28 C 0.43025(9) 0.66402(7) 0.53374(8) 0.0355(2) Uani 1 1 d . . . . .
Li1 Li 0.14389(15) 0.65210(11) 0.73369(13) 0.0346(4) Uani 1 1 d . . . . .
C29 C 0.0505(3) 0.9786(2) 0.4568(3) 0.0578(8) Uani 0.5 1 d . U P A -1
C30 C 0.0511(6) 0.9513(5) 0.5505(5) 0.069(2) Uani 0.5 1 d . U P A -1
H30 H 0.097989 0.911319 0.573092 0.083 Uiso 0.5 1 calc R U P A -1
C31 C -0.0207(6) 0.9845(5) 0.6137(4) 0.108(2) Uani 0.5 1 d . U P A -1
H31 H -0.019997 0.967376 0.680143 0.130 Uiso 0.5 1 calc R U P A -1
C32 C -0.0911(5) 1.0407(4) 0.5810(6) 0.107(2) Uani 0.5 1 d . U P A -1
H32 H -0.140299 1.061749 0.623004 0.128 Uiso 0.5 1 calc R U P A -1
C33 C -0.0880(5) 1.0650(4) 0.4870(6) 0.0960(18) Uani 0.5 1 d . U P A -1
H33 H -0.134503 1.104867 0.463482 0.115 Uiso 0.5 1 calc R U P A -1
C34 C -0.0188(6) 1.0335(4) 0.4236(6) 0.0681(18) Uani 0.5 1 d . U P A -1
H34 H -0.020343 1.050474 0.357021 0.082 Uiso 0.5 1 calc R U P A -1
C35 C 0.1274(6) 0.9445(4) 0.3889(5) 0.1051(18) Uani 0.5 1 d . U P A -1
H35A H 0.101131 0.954487 0.319876 0.158 Uiso 0.5 1 calc R U P A -1
H35B H 0.132048 0.889688 0.399852 0.158 Uiso 0.5 1 calc R U P A -1
H35C H 0.198891 0.967104 0.403041 0.158 Uiso 0.5 1 calc R U P A -1


_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
O1 C13 1.2836(13) . ?
O1 Li1 1.827(2) . ?
N1 C1 1.4665(18) . ?
N1 C3 1.4688(16) . ?
N1 C5 1.4674(17) . ?
N1 Li1 2.356(2) . ?
N2 C2 1.4679(16) . ?
N2 C7 1.4581(17) . ?
N2 C8 1.4623(16) . ?
N2 Li1 2.216(2) . ?
N3 C4 1.4590(17) . ?
N3 C9 1.4597(17) . ?
N3 C10 1.4565(18) . ?
N3 Li1 2.228(2) . ?
N4 C6 1.4664(16) . ?
N4 C11 1.4612(18) . ?
N4 C12 1.4614(17) . ?
N4 Li1 2.212(2) . ?
C1 C2 1.5191(19) . ?
C3 C4 1.509(2) . ?
C5 C6 1.514(2) . ?
C13 C14 1.3389(18) . ?
C13 C15 1.5148(14) . ?
C15 C16 1.4046(15) . ?
C15 C28 1.4084(16) . ?
C16 C17 1.4236(17) . ?
C16 C21 1.4362(15) . ?
C17 C18 1.3586(18) . ?
C18 C19 1.411(2) . ?
C19 C20 1.347(2) . ?
C20 C21 1.4276(18) . ?
C21 C22 1.3872(18) . ?
C22 C23 1.3887(18) . ?
C23 C24 1.4263(18) . ?
C23 C28 1.4345(16) . ?
C24 C25 1.348(2) . ?
C25 C26 1.412(2) . ?
C26 C27 1.3584(19) . ?
C27 C28 1.4241(17) . ?
C29 C30 1.360(7) . ?
C29 C34 1.349(7) . ?
C29 C35 1.513(6) . ?
C30 C31 1.420(8) . ?
C31 C32 1.373(10) . ?
C32 C33 1.349(10) . ?
C33 C34 1.388(8) . ?

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
C13 O1 Li1 170.54(10) . . ?
C1 N1 C3 112.17(11) . . ?
C1 N1 C5 112.64(12) . . ?
C1 N1 Li1 105.52(9) . . ?
C3 N1 Li1 107.30(9) . . ?
C5 N1 C3 111.86(10) . . ?
C5 N1 Li1 106.85(9) . . ?
C2 N2 Li1 108.96(9) . . ?
C7 N2 C2 111.22(11) . . ?
C7 N2 C8 108.38(10) . . ?
C7 N2 Li1 103.00(9) . . ?
C8 N2 C2 110.37(10) . . ?
C8 N2 Li1 114.72(9) . . ?
C4 N3 C9 111.26(11) . . ?
C4 N3 Li1 111.37(9) . . ?
C9 N3 Li1 112.01(9) . . ?
C10 N3 C4 111.57(10) . . ?
C10 N3 C9 108.47(12) . . ?
C10 N3 Li1 101.77(9) . . ?
C6 N4 Li1 109.28(9) . . ?
C11 N4 C6 111.20(11) . . ?
C11 N4 C12 108.40(11) . . ?
C11 N4 Li1 109.82(10) . . ?
C12 N4 C6 111.53(11) . . ?
C12 N4 Li1 106.49(9) . . ?
N1 C1 C2 111.98(11) . . ?
N2 C2 C1 112.16(11) . . ?
N1 C3 C4 112.01(10) . . ?
N3 C4 C3 111.65(10) . . ?
N1 C5 C6 111.38(11) . . ?
N4 C6 C5 111.69(11) . . ?
O1 C13 C14 126.71(11) . . ?
O1 C13 C15 113.78(10) . . ?
C14 C13 C15 119.51(10) . . ?
C16 C15 C13 119.46(10) . . ?
C16 C15 C28 119.80(10) . . ?
C28 C15 C13 120.53(10) . . ?
C15 C16 C17 121.91(10) . . ?
C15 C16 C21 120.01(11) . . ?
C17 C16 C21 118.08(11) . . ?
C18 C17 C16 121.14(12) . . ?
C17 C18 C19 120.67(13) . . ?
C20 C19 C18 120.31(13) . . ?
C19 C20 C21 121.44(12) . . ?
C20 C21 C16 118.33(12) . . ?
C22 C21 C16 119.11(11) . . ?
C22 C21 C20 122.56(11) . . ?
C21 C22 C23 121.98(11) . . ?
C22 C23 C24 122.40(12) . . ?
C22 C23 C28 119.14(11) . . ?
C24 C23 C28 118.45(12) . . ?
C25 C24 C23 121.54(13) . . ?
C24 C25 C26 120.31(13) . . ?
C27 C26 C25 120.32(14) . . ?
C26 C27 C28 121.59(13) . . ?
C15 C28 C23 119.94(11) . . ?
C15 C28 C27 122.27(11) . . ?
C27 C28 C23 117.77(11) . . ?
O1 Li1 N1 176.24(11) . . ?
O1 Li1 N2 104.54(9) . . ?
O1 Li1 N3 100.08(9) . . ?
O1 Li1 N4 101.00(9) . . ?
N2 Li1 N1 79.08(7) . . ?
N2 Li1 N3 115.67(9) . . ?
N3 Li1 N1 77.25(7) . . ?
N4 Li1 N1 78.19(7) . . ?
N4 Li1 N2 113.75(9) . . ?
N4 Li1 N3 118.27(9) . . ?
C30 C29 C35 118.5(6) . . ?
C34 C29 C30 121.1(4) . . ?
C34 C29 C35 120.4(5) . . ?
C29 C30 C31 117.9(7) . . ?
C32 C31 C30 121.6(7) . . ?
C33 C32 C31 117.6(6) . . ?
C32 C33 C34 122.1(8) . . ?
C29 C34 C33 119.8(7) . . ?

_shelx_SHELXL_version_number     2019/1
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.338
_oxdiff_exptl_absorpt_empirical_full_min 0.705
####################################################################### 
# 
# 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_elu230001_fa
_database_code_depnum_ccdc_archive 'CCDC 2307287'
loop_
_audit_author_name
_audit_author_address
'Paul G. Waddell'
;School of Natural and Environmental Sciences, Newcastle University
United Kingdom
;
_audit_update_record             
;
2023-11-11 deposited with the CCDC.	2024-02-12 downloaded from the CCDC.
;
_audit_creation_date             2023-02-21
_audit_creation_method           
;
Olex2 1.5-ac5-023
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.167(C108 H78 Na6 O6), 0.667(C6 H6)'
_chemical_formula_sum            'C22 H17 Na O'
_chemical_formula_weight         320.35
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C20 H23 Na1 O1 '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.3035(3)
_cell_length_b                   13.3928(3)
_cell_length_c                   17.4184(4)
_cell_angle_alpha                81.860(2)
_cell_angle_beta                 85.940(2)
_cell_angle_gamma                63.004(2)
_cell_volume                     2531.60(11)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    18519
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      77.8470
_cell_measurement_theta_min      2.5490
_shelx_estimated_absorpt_T_max   0.976
_shelx_estimated_absorpt_T_min   0.835
_exptl_absorpt_coefficient_mu    0.814
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.888
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0229
0 0 -1 0.0079
0 -1 0 0.0533
0 1 0 0.0533
-1 0 0 0.0952
1 0 0 0.0952
1 1 0 0.1064
-1 -1 0 0.1064
1 -1 0 0.0689

_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0000 -0.0002 0.9996 -0.0649 0.0589 0.0171
0.0000 0.0002 -0.9996 0.0649 -0.0589 -0.0171
0.0000 -0.9990 0.0000 0.0729 0.1072 -0.0087
-0.0000 0.9990 -0.0000 -0.0729 -0.1072 0.0087
-0.9995 0.0008 -0.0002 -0.0171 -0.0546 0.1283
0.9995 -0.0008 0.0002 0.0171 0.0546 -0.1283
0.9995 0.9981 0.0002 -0.0558 -0.0526 -0.1196
-0.9995 -0.9981 -0.0002 0.0558 0.0526 0.1196
0.9995 -0.9998 0.0002 0.0900 0.1619 -0.1370

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29892
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.717
_diffrn_reflns_theta_min         2.563
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -25.00  29.00   0.50    0.81    --  -49.76  19.00 150.00  108
  2  ω    -27.00  29.00   0.50    0.81    --  -49.76  19.00 -90.00  112
  3  ω    -27.00  29.00   0.50    0.81    --  -49.76  19.00-150.00  112
  4  ω     75.00 111.00   0.50    0.81    --   48.76 125.00-120.00   72
  5  ω     90.00 138.00   0.50    0.81    --  108.00 125.00-150.00   96
  6  ω    100.00 125.00   0.50    0.81    --   96.11 112.00   4.00   50
  7  ω     91.00 116.00   0.50    0.81    --  108.00 112.00   4.00   50
  8  ω    118.00 155.00   0.50    0.81    --   96.11  77.00 -30.00   74
  9  ω    139.00 164.00   0.50    0.81    --  108.00  45.00  30.00   50
 10  ω    111.00 137.00   0.50    0.81    --  108.00  45.00  30.00   52
 11  ω     75.00 100.00   0.50    0.81    --   96.11  77.00 -30.00   50
 12  ω    -28.00  16.00   0.50    0.81    --   48.76 -19.00 -30.00   88
 13  ω     18.00  45.00   0.50    0.81    --   96.11 -45.00 120.00   54
 14  ω     35.00  71.00   0.50    0.81    --  108.00 -61.00 120.00   72
 15  ω     40.00  71.00   0.50    0.81    --  108.00 -61.00  60.00   62
 16  ω     52.00  77.00   0.50    0.81    --   96.11 -77.00  30.00   50
 17  ω     24.00  54.00   0.50    0.81    --   96.11-125.00 -30.00   60
 18  ω     36.00  91.00   0.50    0.81    --  108.00-125.00   0.00  110
 19  ω     42.00  67.00   0.50    0.81    --   96.11-112.00 -88.00   50
 20  ω     39.00  64.00   0.50    0.81    --  108.00-125.00-120.00   50
 21  ω     56.00  82.00   0.50    0.81    --  108.00-112.00 -88.00   52
 22  ω     81.00 106.00   0.50    0.81    --  108.00-125.00-120.00   50
 23  ω     15.00  41.00   0.50    0.81    --   48.76-112.00 -88.00   52
 24  ω   -107.00 -48.00   0.50    0.81    --  -99.00 106.00-113.15  118
 25  ω   -107.00 -71.00   0.50    0.81    --  -99.00 107.00 -27.80   72
 26  ω   -125.00 -71.00   0.50    0.81    --  -99.00 143.00  31.67  108
 27  ω    -99.00 -69.00   0.50    0.81    --  -92.01 112.00   4.00   60
 28  ω    -88.00  -4.00   0.50    0.81    --  -49.76 112.00   4.00  168
 29  ω    -49.00 -17.00   0.50    0.81    --  -92.01  45.00 -90.00   64
 30  ω    -51.00 -24.00   0.50    0.81    --  -92.01  45.00-150.00   54
 31  ω   -105.00 -23.00   0.50    0.81    --  -92.01  77.00-150.00  164
 32  ω    -46.00 -20.00   0.50    0.81    --  -92.01  45.00-180.00   52
 33  ω    -51.00 -14.00   0.50    0.81    --  -92.01  45.00 -60.00   74
 34  ω    -48.00 -19.00   0.50    0.81    --  -92.01  45.00 -30.00   58
 35  ω    -71.00 -17.00   0.50    0.81    --  -92.01  61.00  30.00  108
 36  ω    -44.00 -16.00   0.50    0.81    --  -92.01  45.00 120.00   56
 37  ω   -168.00 -76.00   0.50    0.81    --  -92.01 -45.00 -30.00  184
 38  ω   -163.00 -82.00   0.50    0.81    --  -92.01-112.00 -88.00  162
 39  ω   -119.00 -81.00   0.50    0.81    --  -49.76-125.00-180.00   76
 40  ω   -111.00 -78.00   0.50    0.81    --  -49.76-125.00  60.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix-Arc 100'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0170236000
_diffrn_orient_matrix_UB_12      -0.0729664000
_diffrn_orient_matrix_UB_13      -0.0649703000
_diffrn_orient_matrix_UB_21      0.0545539000
_diffrn_orient_matrix_UB_22      -0.1073413000
_diffrn_orient_matrix_UB_23      0.0588916000
_diffrn_orient_matrix_UB_31      -0.1283848000
_diffrn_orient_matrix_UB_32      0.0087261000
_diffrn_orient_matrix_UB_33      0.0171326000
_diffrn_oxdiff_digest_frames     
;
01403703c5b295ae20c7373a2d2caee80603220e0ed
;
_diffrn_oxdiff_digest_hkl        
;
01a5ac70335aa3f39fa9aa94e3dd943353adbf
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8312
_reflns_number_total             10031
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.00068(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         10031
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0424
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0558P)²+0.8656P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1204
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C28(H28), C29(H29),
  C30(H30), C31(H31), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42),
 C44(H44), C45(H45), C46(H46), C47(H47), C49(H49), C50(H50), C51(H51), C52(H52),
  C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59),
 C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66)
2.b X=CH2 refined with riding coordinates:
 C2(H2A,H2B), C18(H18A,H18B), C34(H34A,H34B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.35586(5) 0.65448(5) 0.60356(4) 0.03401(15) Uani 1 1 d . . . . .
Na2 Na 0.61763(5) 0.47252(5) 0.64678(4) 0.03210(15) Uani 1 1 d . . . . .
Na3 Na 0.55053(5) 0.59605(5) 0.46336(3) 0.02786(14) Uani 1 1 d . . . . .
O1 O 0.35656(9) 0.59675(8) 0.48138(6) 0.0264(2) Uani 1 1 d . . . . .
O2 O 0.43576(9) 0.47004(9) 0.65836(6) 0.0297(2) Uani 1 1 d . . . . .
O3 O 0.54101(10) 0.64979(8) 0.58703(6) 0.0314(2) Uani 1 1 d . . . . .
C1 C 0.24954(13) 0.67713(11) 0.45426(9) 0.0259(3) Uani 1 1 d . . . . .
C2 C 0.16838(14) 0.66097(13) 0.41671(10) 0.0344(3) Uani 1 1 d . . . . .
H2A H 0.185334 0.587021 0.407522 0.041 Uiso 1 1 calc R U . . .
H2B H 0.093962 0.723471 0.399308 0.041 Uiso 1 1 calc R U . . .
C3 C 0.22088(13) 0.79436(11) 0.47064(9) 0.0278(3) Uani 1 1 d . . . . .
C4 C 0.27192(13) 0.85807(12) 0.42466(10) 0.0307(3) Uani 1 1 d . . . . .
C5 C 0.34562(15) 0.81988(13) 0.35813(11) 0.0379(4) Uani 1 1 d . . . . .
H5 H 0.363162 0.747913 0.344344 0.045 Uiso 1 1 calc R U . . .
C6 C 0.39152(17) 0.88443(15) 0.31383(13) 0.0484(5) Uani 1 1 d . . . . .
H6 H 0.440900 0.856708 0.269897 0.058 Uiso 1 1 calc R U . . .
C7 C 0.36651(18) 0.99247(15) 0.33247(13) 0.0496(5) Uani 1 1 d . . . . .
H7 H 0.398466 1.036984 0.300856 0.059 Uiso 1 1 calc R U . . .
C8 C 0.29714(16) 1.03218(14) 0.39528(12) 0.0421(4) Uani 1 1 d . . . . .
H8 H 0.280949 1.104656 0.407360 0.051 Uiso 1 1 calc R U . . .
C9 C 0.24790(14) 0.96737(12) 0.44367(10) 0.0336(3) Uani 1 1 d . . . . .
C10 C 0.17507(14) 1.00827(12) 0.50771(10) 0.0340(4) Uani 1 1 d . . . . .
H10 H 0.160411 1.080007 0.520473 0.041 Uiso 1 1 calc R U . . .
C11 C 0.12316(13) 0.94743(12) 0.55354(9) 0.0311(3) Uani 1 1 d . . . . .
C12 C 0.04437(15) 0.99131(13) 0.61742(10) 0.0368(4) Uani 1 1 d . . . . .
H12 H 0.027301 1.064090 0.629330 0.044 Uiso 1 1 calc R U . . .
C13 C -0.00652(16) 0.93170(14) 0.66135(10) 0.0402(4) Uani 1 1 d . . . . .
H13 H -0.058831 0.962839 0.703471 0.048 Uiso 1 1 calc R U . . .
C14 C 0.01811(16) 0.82252(14) 0.64462(10) 0.0392(4) Uani 1 1 d . . . . .
H14 H -0.016422 0.780384 0.676477 0.047 Uiso 1 1 calc R U . . .
C15 C 0.09055(14) 0.77780(12) 0.58352(9) 0.0331(3) Uani 1 1 d . . . . .
H15 H 0.104818 0.705195 0.572848 0.040 Uiso 1 1 calc R U . . .
C16 C 0.14592(13) 0.83810(12) 0.53481(9) 0.0292(3) Uani 1 1 d . . . . .
C17 C 0.35407(14) 0.47941(12) 0.71444(9) 0.0284(3) Uani 1 1 d . . . . .
C18 C 0.29629(17) 0.56857(14) 0.75442(10) 0.0404(4) Uani 1 1 d . . . . .
H18A H 0.312908 0.631836 0.743270 0.048 Uiso 1 1 calc R U . . .
H18B H 0.238892 0.568244 0.793793 0.048 Uiso 1 1 calc R U . . .
C19 C 0.32596(13) 0.38007(12) 0.73184(9) 0.0275(3) Uani 1 1 d . . . . .
C20 C 0.36363(14) 0.30764(13) 0.80187(9) 0.0302(3) Uani 1 1 d . . . . .
C21 C 0.42314(15) 0.32718(14) 0.86147(10) 0.0366(4) Uani 1 1 d . . . . .
H21 H 0.438357 0.391391 0.854056 0.044 Uiso 1 1 calc R U . . .
C22 C 0.45840(19) 0.25584(17) 0.92851(11) 0.0489(5) Uani 1 1 d . . . . .
H22 H 0.497901 0.270821 0.967151 0.059 Uiso 1 1 calc R U . . .
C23 C 0.4371(2) 0.15951(18) 0.94155(12) 0.0569(5) Uani 1 1 d . . . . .
H23 H 0.460658 0.111192 0.989165 0.068 Uiso 1 1 calc R U . . .
C24 C 0.3830(2) 0.13608(17) 0.88623(11) 0.0510(5) Uani 1 1 d . . . . .
H24 H 0.370342 0.070479 0.895262 0.061 Uiso 1 1 calc R U . . .
C25 C 0.34467(16) 0.20814(14) 0.81456(10) 0.0362(4) Uani 1 1 d . . . . .
C26 C 0.29159(17) 0.18326(15) 0.75685(10) 0.0400(4) Uani 1 1 d . . . . .
H26 H 0.282351 0.115854 0.764683 0.048 Uiso 1 1 calc R U . . .
C27 C 0.25177(15) 0.25488(14) 0.68800(9) 0.0347(3) Uani 1 1 d . . . . .
C28 C 0.19348(18) 0.23175(17) 0.62942(10) 0.0437(4) Uani 1 1 d . . . . .
H28 H 0.184541 0.164197 0.636702 0.052 Uiso 1 1 calc R U . . .
C29 C 0.15078(17) 0.30432(16) 0.56376(10) 0.0422(4) Uani 1 1 d . . . . .
H29 H 0.112357 0.287333 0.525582 0.051 Uiso 1 1 calc R U . . .
C30 C 0.16330(15) 0.40564(15) 0.55189(9) 0.0355(3) Uani 1 1 d . . . . .
H30 H 0.131828 0.456852 0.506161 0.043 Uiso 1 1 calc R U . . .
C31 C 0.22011(13) 0.43002(13) 0.60557(9) 0.0307(3) Uani 1 1 d . . . . .
H31 H 0.228428 0.497856 0.596312 0.037 Uiso 1 1 calc R U . . .
C32 C 0.26745(13) 0.35590(13) 0.67545(9) 0.0285(3) Uani 1 1 d . . . . .
C33 C 0.54299(13) 0.74549(12) 0.59726(9) 0.0271(3) Uani 1 1 d . . . . .
C34 C 0.52412(17) 0.83141(14) 0.54208(10) 0.0391(4) Uani 1 1 d . . . . .
H34A H 0.507641 0.827037 0.490525 0.047 Uiso 1 1 calc R U . . .
H34B H 0.527153 0.896998 0.554327 0.047 Uiso 1 1 calc R U . . .
C35 C 0.57102(13) 0.75066(11) 0.67896(9) 0.0268(3) Uani 1 1 d . . . . .
C36 C 0.69331(13) 0.69760(12) 0.70364(9) 0.0281(3) Uani 1 1 d . . . . .
C37 C 0.79161(15) 0.64335(13) 0.65198(10) 0.0353(3) Uani 1 1 d . . . . .
H37 H 0.774562 0.643853 0.599540 0.042 Uiso 1 1 calc R U . . .
C38 C 0.90968(16) 0.59073(15) 0.67645(12) 0.0438(4) Uani 1 1 d . . . . .
H38 H 0.973637 0.555050 0.640988 0.053 Uiso 1 1 calc R U . . .
C39 C 0.93760(16) 0.58887(15) 0.75414(12) 0.0452(4) Uani 1 1 d . . . . .
H39 H 1.020126 0.551441 0.770568 0.054 Uiso 1 1 calc R U . . .
C40 C 0.84745(15) 0.64015(14) 0.80548(11) 0.0395(4) Uani 1 1 d . . . . .
H40 H 0.867647 0.638718 0.857396 0.047 Uiso 1 1 calc R U . . .
C41 C 0.72227(14) 0.69637(12) 0.78230(9) 0.0321(3) Uani 1 1 d . . . . .
C42 C 0.62763(15) 0.74853(13) 0.83389(9) 0.0342(3) Uani 1 1 d . . . . .
H42 H 0.646419 0.748808 0.885809 0.041 Uiso 1 1 calc R U . . .
C43 C 0.50587(14) 0.80037(12) 0.81096(9) 0.0310(3) Uani 1 1 d . . . . .
C44 C 0.40800(16) 0.84928(14) 0.86442(10) 0.0390(4) Uani 1 1 d . . . . .
H44 H 0.426239 0.849261 0.916521 0.047 Uiso 1 1 calc R U . . .
C45 C 0.28983(16) 0.89568(15) 0.84252(11) 0.0422(4) Uani 1 1 d . . . . .
H45 H 0.226502 0.925979 0.879501 0.051 Uiso 1 1 calc R U . . .
C46 C 0.26043(15) 0.89915(14) 0.76486(10) 0.0389(4) Uani 1 1 d . . . . .
H46 H 0.177403 0.932457 0.749793 0.047 Uiso 1 1 calc R U . . .
C47 C 0.35063(14) 0.85495(13) 0.71144(10) 0.0324(3) Uani 1 1 d . . . . .
H47 H 0.329274 0.859348 0.659283 0.039 Uiso 1 1 calc R U . . .
C48 C 0.47644(13) 0.80221(12) 0.73218(9) 0.0276(3) Uani 1 1 d . . . . .
C49 C 0.7259(2) 0.3397(2) 0.80578(13) 0.0594(5) Uani 1 1 d . . . . .
H49 H 0.641141 0.388656 0.809031 0.071 Uiso 1 1 calc R U . . .
C50 C 0.7674(2) 0.2243(2) 0.81648(14) 0.0639(6) Uani 1 1 d . . . . .
H50 H 0.710976 0.193662 0.827141 0.077 Uiso 1 1 calc R U . . .
C51 C 0.8904(2) 0.15315(19) 0.81176(15) 0.0668(6) Uani 1 1 d . . . . .
H51 H 0.919004 0.073624 0.819952 0.080 Uiso 1 1 calc R U . . .
C52 C 0.9717(2) 0.19795(19) 0.79512(14) 0.0606(5) Uani 1 1 d . . . . .
H52 H 1.056333 0.149093 0.790623 0.073 Uiso 1 1 calc R U . . .
C53 C 0.93109(19) 0.31278(17) 0.78500(13) 0.0535(5) Uani 1 1 d . . . . .
H53 H 0.987599 0.343273 0.774352 0.064 Uiso 1 1 calc R U . . .
C54 C 0.8083(2) 0.38369(17) 0.79031(13) 0.0553(5) Uani 1 1 d . . . . .
H54 H 0.780175 0.463167 0.783307 0.066 Uiso 1 1 calc R U . . .
C55 C 0.9815(4) 0.8274(2) 0.86768(16) 0.0853(9) Uani 1 1 d . . . . .
H55 H 1.042158 0.781206 0.834142 0.102 Uiso 1 1 calc R U . . .
C56 C 0.8617(3) 0.8752(2) 0.84883(17) 0.0824(9) Uani 1 1 d . . . . .
H56 H 0.840018 0.861005 0.801709 0.099 Uiso 1 1 calc R U . . .
C57 C 0.7729(3) 0.9415(3) 0.89375(18) 0.0954(10) Uani 1 1 d . . . . .
H57 H 0.690130 0.974183 0.878307 0.114 Uiso 1 1 calc R U . . .
C58 C 0.8025(4) 0.9614(4) 0.96154(19) 0.1045(12) Uani 1 1 d . . . . .
H58 H 0.739148 1.008359 0.993338 0.125 Uiso 1 1 calc R U . . .
C59 C 0.9201(4) 0.9162(3) 0.98556(17) 0.0941(10) Uani 1 1 d . . . . .
H59 H 0.937968 0.931041 1.033674 0.113 Uiso 1 1 calc R U . . .
C60 C 1.0150(4) 0.8476(3) 0.9388(2) 0.0959(10) Uani 1 1 d . . . . .
H60 H 1.097881 0.815885 0.953773 0.115 Uiso 1 1 calc R U . . .
C61 C 0.3913(3) 0.5620(3) 0.96408(19) 0.0879(9) Uani 1 1 d . . . . .
H61 H 0.314828 0.605450 0.939116 0.105 Uiso 1 1 calc R U . . .
C62 C 0.4945(4) 0.5561(3) 0.92826(15) 0.0841(9) Uani 1 1 d . . . . .
H62 H 0.490897 0.595333 0.877860 0.101 Uiso 1 1 calc R U . . .
C63 C 0.6027(3) 0.4945(4) 0.96407(19) 0.0988(11) Uani 1 1 d . . . . .
H63 H 0.675259 0.490534 0.938780 0.119 Uiso 1 1 calc R U . . .
C64 C 1.0654(3) 0.4112(2) 0.95984(17) 0.0866(9) Uani 1 1 d . . . . .
H64 H 1.111139 0.349003 0.931672 0.104 Uiso 1 1 calc R U . . .
C65 C 1.1130(3) 0.4801(3) 0.97325(17) 0.0849(9) Uani 1 1 d . . . . .
H65 H 1.192421 0.466205 0.954526 0.102 Uiso 1 1 calc R U . . .
C66 C 1.0480(3) 0.5692(3) 1.01335(19) 0.0852(8) Uani 1 1 d . . . . .
H66 H 1.081761 0.617586 1.022640 0.102 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 Na2 3.0946(8) . ?
Na1 Na3 3.2131(8) . ?
Na1 O1 2.3632(11) . ?
Na1 O2 2.2890(12) . ?
Na1 O3 2.2491(12) . ?
Na1 C1 2.9094(16) . ?
Na1 C3 2.8496(16) . ?
Na1 C15 2.9340(16) . ?
Na1 C16 2.8268(15) . ?
Na1 C17 2.8260(16) . ?
Na1 C18 2.8987(19) . ?
Na1 C33 3.0450(15) . ?
Na2 Na3 3.3560(8) . ?
Na2 Na3 3.4046(8) 2_666 ?
Na2 O1 2.4825(11) 2_666 ?
Na2 O2 2.2474(12) . ?
Na2 O3 2.2396(12) . ?
Na2 C1 2.7209(15) 2_666 ?
Na2 C2 2.6880(17) 2_666 ?
Na2 C49 3.096(2) . ?
Na3 Na3 3.3976(11) 2_666 ?
Na3 O1 2.3809(11) . ?
Na3 O1 2.3818(11) 2_666 ?
Na3 O2 2.3776(11) 2_666 ?
Na3 O3 2.3450(11) . ?
Na3 C31 2.8760(16) 2_666 ?
O1 C1 1.3315(17) . ?
O2 C17 1.3271(18) . ?
O3 C33 1.3299(17) . ?
C1 C2 1.342(2) . ?
C1 C3 1.5103(19) . ?
C3 C4 1.409(2) . ?
C3 C16 1.411(2) . ?
C4 C5 1.423(2) . ?
C4 C9 1.439(2) . ?
C5 C6 1.362(2) . ?
C6 C7 1.417(2) . ?
C7 C8 1.352(3) . ?
C8 C9 1.424(2) . ?
C9 C10 1.390(2) . ?
C10 C11 1.387(2) . ?
C11 C12 1.428(2) . ?
C11 C16 1.442(2) . ?
C12 C13 1.352(3) . ?
C13 C14 1.422(2) . ?
C14 C15 1.359(2) . ?
C15 C16 1.435(2) . ?
C17 C18 1.346(2) . ?
C17 C19 1.507(2) . ?
C19 C20 1.407(2) . ?
C19 C32 1.410(2) . ?
C20 C21 1.429(2) . ?
C20 C25 1.439(2) . ?
C21 C22 1.358(2) . ?
C22 C23 1.415(3) . ?
C23 C24 1.355(3) . ?
C24 C25 1.429(2) . ?
C25 C26 1.391(2) . ?
C26 C27 1.389(2) . ?
C27 C28 1.430(2) . ?
C27 C32 1.436(2) . ?
C28 C29 1.355(3) . ?
C29 C30 1.419(2) . ?
C30 C31 1.362(2) . ?
C31 C32 1.428(2) . ?
C33 C34 1.333(2) . ?
C33 C35 1.506(2) . ?
C35 C36 1.410(2) . ?
C35 C48 1.410(2) . ?
C36 C37 1.426(2) . ?
C36 C41 1.436(2) . ?
C37 C38 1.364(2) . ?
C38 C39 1.414(3) . ?
C39 C40 1.358(3) . ?
C40 C41 1.432(2) . ?
C41 C42 1.394(2) . ?
C42 C43 1.396(2) . ?
C43 C44 1.430(2) . ?
C43 C48 1.438(2) . ?
C44 C45 1.355(3) . ?
C45 C46 1.414(3) . ?
C46 C47 1.364(2) . ?
C47 C48 1.428(2) . ?
C49 C50 1.378(3) . ?
C49 C54 1.381(3) . ?
C50 C51 1.379(4) . ?
C51 C52 1.378(3) . ?
C52 C53 1.373(3) . ?
C53 C54 1.377(3) . ?
C55 C56 1.357(4) . ?
C55 C60 1.430(5) . ?
C56 C57 1.337(4) . ?
C57 C58 1.355(4) . ?
C58 C59 1.362(5) . ?
C59 C60 1.405(4) . ?
C61 C62 1.348(4) . ?
C61 C63 1.355(5) 2_667 ?
C62 C63 1.348(5) . ?
C64 C65 1.350(5) . ?
C64 C66 1.358(4) 2_767 ?
C65 C66 1.357(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
Na2 Na1 Na3 64.255(19) . . ?
O1 Na1 Na2 95.20(3) . . ?
O1 Na1 Na3 47.60(3) . . ?
O1 Na1 C1 26.78(4) . . ?
O1 Na1 C3 53.64(4) . . ?
O1 Na1 C15 84.85(4) . . ?
O1 Na1 C16 78.60(4) . . ?
O1 Na1 C17 105.63(4) . . ?
O1 Na1 C18 128.72(5) . . ?
O1 Na1 C33 107.76(4) . . ?
O2 Na1 Na2 46.43(3) . . ?
O2 Na1 Na3 92.64(3) . . ?
O2 Na1 O1 89.74(4) . . ?
O2 Na1 C1 109.60(4) . . ?
O2 Na1 C3 139.81(5) . . ?
O2 Na1 C15 117.72(5) . . ?
O2 Na1 C16 144.53(5) . . ?
O2 Na1 C17 27.60(4) . . ?
O2 Na1 C18 52.96(4) . . ?
O2 Na1 C33 111.36(4) . . ?
O3 Na1 Na2 46.29(3) . . ?
O3 Na1 Na3 46.86(3) . . ?
O3 Na1 O1 94.44(4) . . ?
O3 Na1 O2 92.63(4) . . ?
O3 Na1 C1 110.40(4) . . ?
O3 Na1 C3 104.87(5) . . ?
O3 Na1 C15 149.61(5) . . ?
O3 Na1 C16 121.35(5) . . ?
O3 Na1 C17 113.09(5) . . ?
O3 Na1 C18 118.00(5) . . ?
O3 Na1 C33 23.49(4) . . ?
C1 Na1 Na2 121.86(4) . . ?
C1 Na1 Na3 66.39(3) . . ?
C1 Na1 C15 60.07(4) . . ?
C1 Na1 C33 114.19(4) . . ?
C3 Na1 Na2 139.44(4) . . ?
C3 Na1 Na3 75.19(4) . . ?
C3 Na1 C1 30.38(4) . . ?
C3 Na1 C15 51.15(5) . . ?
C3 Na1 C18 135.51(5) . . ?
C3 Na1 C33 96.88(4) . . ?
C15 Na1 Na2 164.10(4) . . ?
C15 Na1 Na3 124.43(4) . . ?
C15 Na1 C33 129.32(5) . . ?
C16 Na1 Na2 166.23(4) . . ?
C16 Na1 Na3 103.17(4) . . ?
C16 Na1 C1 52.09(4) . . ?
C16 Na1 C3 28.79(4) . . ?
C16 Na1 C15 28.77(5) . . ?
C16 Na1 C18 110.43(5) . . ?
C16 Na1 C33 104.10(5) . . ?
C17 Na1 Na2 68.42(3) . . ?
C17 Na1 Na3 120.05(4) . . ?
C17 Na1 C1 115.53(4) . . ?
C17 Na1 C3 138.39(5) . . ?
C17 Na1 C15 96.20(5) . . ?
C17 Na1 C16 124.97(5) . . ?
C17 Na1 C18 27.15(4) . . ?
C17 Na1 C33 124.70(5) . . ?
C18 Na1 Na2 83.08(4) . . ?
C18 Na1 Na3 144.51(4) . . ?
C18 Na1 C1 128.18(5) . . ?
C18 Na1 C15 84.52(5) . . ?
C18 Na1 C33 117.54(5) . . ?
C33 Na1 Na2 65.80(3) . . ?
C33 Na1 Na3 62.55(3) . . ?
Na1 Na2 Na3 59.586(19) . . ?
Na1 Na2 Na3 62.239(18) . 2_666 ?
Na1 Na2 C49 130.28(5) . . ?
Na3 Na2 Na3 60.335(19) . 2_666 ?
O1 Na2 Na1 90.56(3) 2_666 . ?
O1 Na2 Na3 45.14(3) 2_666 . ?
O1 Na2 Na3 44.36(3) 2_666 2_666 ?
O1 Na2 C1 29.19(4) 2_666 2_666 ?
O1 Na2 C2 54.59(4) 2_666 2_666 ?
O1 Na2 C49 129.37(5) 2_666 . ?
O2 Na2 Na1 47.55(3) . . ?
O2 Na2 Na3 89.72(3) . . ?
O2 Na2 Na3 44.10(3) . 2_666 ?
O2 Na2 O1 88.46(4) . 2_666 ?
O2 Na2 C1 105.96(4) . 2_666 ?
O2 Na2 C2 132.90(5) . 2_666 ?
O2 Na2 C49 98.76(5) . . ?
O3 Na2 Na1 46.54(3) . . ?
O3 Na2 Na3 44.18(3) . . ?
O3 Na2 Na3 92.25(3) . 2_666 ?
O3 Na2 O1 89.25(4) . 2_666 ?
O3 Na2 O2 94.02(4) . . ?
O3 Na2 C1 110.64(5) . 2_666 ?
O3 Na2 C2 111.45(5) . 2_666 ?
O3 Na2 C49 139.28(6) . . ?
C1 Na2 Na1 119.64(4) 2_666 . ?
C1 Na2 Na3 69.73(3) 2_666 . ?
C1 Na2 Na3 65.47(3) 2_666 2_666 ?
C1 Na2 C49 102.69(6) 2_666 . ?
C2 Na2 Na1 142.02(4) 2_666 . ?
C2 Na2 Na3 94.19(4) 2_666 2_666 ?
C2 Na2 Na3 83.20(4) 2_666 . ?
C2 Na2 C1 28.72(4) 2_666 2_666 ?
C2 Na2 C49 87.19(6) 2_666 . ?
C49 Na2 Na3 123.28(5) . 2_666 ?
C49 Na2 Na3 170.05(5) . . ?
Na1 Na3 Na1 117.90(2) . 2_666 ?
Na1 Na3 Na2 54.365(16) 2_666 2_666 ?
Na1 Na3 Na2 56.159(17) . . ?
Na1 Na3 Na2 93.92(2) . 2_666 ?
Na1 Na3 Na3 61.21(2) . 2_666 ?
Na1 Na3 Na3 56.693(19) 2_666 2_666 ?
Na2 Na3 Na1 92.01(2) . 2_666 ?
Na2 Na3 Na2 119.666(19) . 2_666 ?
Na2 Na3 Na3 60.541(19) . 2_666 ?
Na3 Na3 Na2 59.124(19) 2_666 2_666 ?
O1 Na3 Na1 47.14(3) . . ?
O1 Na3 Na1 85.96(3) . 2_666 ?
O1 Na3 Na1 44.54(3) 2_666 2_666 ?
O1 Na3 Na1 89.60(3) 2_666 . ?
O1 Na3 Na2 87.26(3) 2_666 2_666 ?
O1 Na3 Na2 46.81(3) . 2_666 ?
O1 Na3 Na2 88.41(3) . . ?
O1 Na3 Na2 47.63(3) 2_666 . ?
O1 Na3 Na3 44.50(3) . 2_666 ?
O1 Na3 Na3 44.48(3) 2_666 2_666 ?
O1 Na3 O1 88.98(4) . 2_666 ?
O1 Na3 C31 90.25(4) 2_666 2_666 ?
O1 Na3 C31 161.04(5) . 2_666 ?
O2 Na3 Na1 135.03(3) 2_666 . ?
O2 Na3 Na1 42.75(3) 2_666 2_666 ?
O2 Na3 Na2 41.14(3) 2_666 2_666 ?
O2 Na3 Na2 134.76(3) 2_666 . ?
O2 Na3 Na3 86.61(3) 2_666 2_666 ?
O2 Na3 O1 87.94(4) 2_666 . ?
O2 Na3 O1 87.22(4) 2_666 2_666 ?
O2 Na3 C31 73.10(4) 2_666 2_666 ?
O3 Na3 Na1 44.41(3) . . ?
O3 Na3 Na1 133.74(3) . 2_666 ?
O3 Na3 Na2 41.73(3) . . ?
O3 Na3 Na2 138.23(3) . 2_666 ?
O3 Na3 Na3 90.58(3) . 2_666 ?
O3 Na3 O1 91.54(4) . . ?
O3 Na3 O1 89.29(4) . 2_666 ?
O3 Na3 O2 176.48(4) . 2_666 ?
O3 Na3 C31 107.39(4) . 2_666 ?
C31 Na3 Na1 151.81(4) 2_666 . ?
C31 Na3 Na1 80.27(3) 2_666 2_666 ?
C31 Na3 Na2 114.24(4) 2_666 2_666 ?
C31 Na3 Na2 104.93(4) 2_666 . ?
C31 Na3 Na3 131.75(4) 2_666 2_666 ?
Na1 O1 Na2 173.62(5) . 2_666 ?
Na1 O1 Na3 85.26(4) . . ?
Na1 O1 Na3 90.48(4) . 2_666 ?
Na3 O1 Na2 87.22(4) 2_666 2_666 ?
Na3 O1 Na2 88.83(4) . 2_666 ?
Na3 O1 Na3 91.02(4) . 2_666 ?
C1 O1 Na1 100.13(8) . . ?
C1 O1 Na2 85.38(8) . 2_666 ?
C1 O1 Na3 140.48(9) . 2_666 ?
C1 O1 Na3 127.51(9) . . ?
Na1 O2 Na3 92.42(4) . 2_666 ?
Na2 O2 Na1 86.02(4) . . ?
Na2 O2 Na3 94.76(4) . 2_666 ?
C17 O2 Na1 99.34(8) . . ?
C17 O2 Na2 136.39(9) . . ?
C17 O2 Na3 127.84(9) . 2_666 ?
Na1 O3 Na3 88.73(4) . . ?
Na2 O3 Na1 87.17(4) . . ?
Na2 O3 Na3 94.08(4) . . ?
C33 O3 Na1 114.13(9) . . ?
C33 O3 Na2 136.76(9) . . ?
C33 O3 Na3 122.04(9) . . ?
Na2 C1 Na1 118.45(5) 2_666 . ?
O1 C1 Na1 53.09(7) . . ?
O1 C1 Na2 65.43(7) . 2_666 ?
O1 C1 C2 125.65(13) . . ?
O1 C1 C3 114.46(12) . . ?
C2 C1 Na1 145.79(11) . . ?
C2 C1 Na2 74.28(9) . 2_666 ?
C2 C1 C3 119.88(13) . . ?
C3 C1 Na1 72.62(8) . . ?
C3 C1 Na2 139.72(10) . 2_666 ?
C1 C2 Na2 77.00(9) . 2_666 ?
C1 C3 Na1 77.00(8) . . ?
C4 C3 Na1 116.63(10) . . ?
C4 C3 C1 120.80(13) . . ?
C4 C3 C16 120.00(13) . . ?
C16 C3 Na1 74.71(8) . . ?
C16 C3 C1 119.15(13) . . ?
C3 C4 C5 122.65(13) . . ?
C3 C4 C9 119.76(14) . . ?
C5 C4 C9 117.58(14) . . ?
C6 C5 C4 121.31(15) . . ?
C5 C6 C7 120.80(18) . . ?
C8 C7 C6 119.98(17) . . ?
C7 C8 C9 121.24(15) . . ?
C8 C9 C4 119.09(15) . . ?
C10 C9 C4 119.32(14) . . ?
C10 C9 C8 121.58(14) . . ?
C11 C10 C9 121.96(14) . . ?
C10 C11 C12 122.00(14) . . ?
C10 C11 C16 119.25(14) . . ?
C12 C11 C16 118.72(15) . . ?
C13 C12 C11 121.54(15) . . ?
C12 C13 C14 120.11(16) . . ?
C15 C14 C13 120.68(16) . . ?
C14 C15 Na1 119.55(11) . . ?
C14 C15 C16 121.30(15) . . ?
C16 C15 Na1 71.46(8) . . ?
C3 C16 Na1 76.50(8) . . ?
C3 C16 C11 119.70(14) . . ?
C3 C16 C15 122.69(13) . . ?
C11 C16 Na1 115.17(9) . . ?
C15 C16 Na1 79.76(8) . . ?
C15 C16 C11 117.61(14) . . ?
O2 C17 Na1 53.06(7) . . ?
O2 C17 C18 125.53(14) . . ?
O2 C17 C19 114.84(12) . . ?
C18 C17 Na1 79.43(10) . . ?
C18 C17 C19 119.62(14) . . ?
C19 C17 Na1 147.27(10) . . ?
C17 C18 Na1 73.42(10) . . ?
C20 C19 C17 120.66(13) . . ?
C20 C19 C32 119.72(13) . . ?
C32 C19 C17 119.52(13) . . ?
C19 C20 C21 122.64(14) . . ?
C19 C20 C25 119.70(14) . . ?
C21 C20 C25 117.65(14) . . ?
C22 C21 C20 121.34(16) . . ?
C21 C22 C23 120.85(17) . . ?
C24 C23 C22 120.09(17) . . ?
C23 C24 C25 121.25(17) . . ?
C24 C25 C20 118.79(15) . . ?
C26 C25 C20 119.67(15) . . ?
C26 C25 C24 121.54(15) . . ?
C27 C26 C25 121.39(15) . . ?
C26 C27 C28 121.72(15) . . ?
C26 C27 C32 119.43(15) . . ?
C28 C27 C32 118.84(15) . . ?
C29 C28 C27 121.27(16) . . ?
C28 C29 C30 120.16(16) . . ?
C31 C30 C29 120.48(16) . . ?
C30 C31 Na3 105.83(10) . 2_666 ?
C30 C31 C32 121.50(15) . . ?
C32 C31 Na3 97.45(9) . 2_666 ?
C19 C32 C27 120.01(14) . . ?
C19 C32 C31 122.26(14) . . ?
C31 C32 C27 117.72(14) . . ?
O3 C33 Na1 42.38(7) . . ?
O3 C33 C34 125.34(14) . . ?
O3 C33 C35 114.13(12) . . ?
C34 C33 Na1 114.90(11) . . ?
C34 C33 C35 120.52(13) . . ?
C35 C33 Na1 108.56(9) . . ?
C36 C35 C33 119.35(13) . . ?
C36 C35 C48 119.66(13) . . ?
C48 C35 C33 120.90(13) . . ?
C35 C36 C37 121.48(14) . . ?
C35 C36 C41 120.53(14) . . ?
C37 C36 C41 117.99(14) . . ?
C38 C37 C36 121.24(16) . . ?
C37 C38 C39 120.54(17) . . ?
C40 C39 C38 120.54(16) . . ?
C39 C40 C41 120.79(16) . . ?
C40 C41 C36 118.89(15) . . ?
C42 C41 C36 118.98(14) . . ?
C42 C41 C40 122.12(15) . . ?
C41 C42 C43 121.45(14) . . ?
C42 C43 C44 121.80(14) . . ?
C42 C43 C48 119.77(14) . . ?
C44 C43 C48 118.40(14) . . ?
C45 C44 C43 121.55(16) . . ?
C44 C45 C46 120.26(16) . . ?
C47 C46 C45 120.37(15) . . ?
C46 C47 C48 121.47(15) . . ?
C35 C48 C43 119.60(13) . . ?
C35 C48 C47 122.47(14) . . ?
C47 C48 C43 117.91(14) . . ?
C50 C49 Na2 118.92(16) . . ?
C50 C49 C54 119.6(2) . . ?
C54 C49 Na2 84.17(14) . . ?
C49 C50 C51 120.2(2) . . ?
C52 C51 C50 119.7(2) . . ?
C53 C52 C51 120.3(2) . . ?
C52 C53 C54 119.9(2) . . ?
C53 C54 C49 120.2(2) . . ?
C56 C55 C60 119.0(3) . . ?
C57 C56 C55 122.8(3) . . ?
C56 C57 C58 119.2(4) . . ?
C57 C58 C59 122.1(3) . . ?
C58 C59 C60 119.6(3) . . ?
C59 C60 C55 117.2(3) . . ?
C62 C61 C63 119.6(3) . 2_667 ?
C61 C62 C63 119.9(3) . . ?
C62 C63 C61 120.5(3) . 2_667 ?
C65 C64 C66 119.9(3) . 2_767 ?
C64 C65 C66 120.3(3) . . ?
C65 C66 C64 119.7(3) . 2_767 ?

_shelx_SHELXL_version_number     2019/1
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.344
_oxdiff_exptl_absorpt_empirical_full_min 0.686
####################################################################### 
# 
# 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_elu230005_fa
_database_code_depnum_ccdc_archive 'CCDC 2307290'
loop_
_audit_author_name
_audit_author_address
'Paul G. Waddell'
;School of Natural and Environmental Sciences, Newcastle University
United Kingdom
;
_audit_update_record             
;
2023-11-11 deposited with the CCDC.	2024-02-12 downloaded from the CCDC.
;
_audit_creation_date             2023-03-03
_audit_creation_method           
;
Olex2 1.5-ac5-023
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H41 N4 Na O'
_chemical_formula_sum            'C28 H41 N4 Na O'
_chemical_formula_weight         472.64
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C32 H53 N4 Na1 O1 Si1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   11.3331(5)
_cell_length_b                   12.8913(5)
_cell_length_c                   19.8712(9)
_cell_angle_alpha                90
_cell_angle_beta                 103.504(4)
_cell_angle_gamma                90
_cell_volume                     2822.9(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7799
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      69.2080
_cell_measurement_theta_min      3.9900
_shelx_estimated_absorpt_T_max   0.925
_shelx_estimated_absorpt_T_min   0.868
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1024
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
6 5 -6 0.0653
-6 5 6 0.0693
-7 -1 8 0.0710
-5 -6 6 0.0686
2 -8 -2 0.0971
7 -1 -8 0.0643
-1 8 2 0.1182
-5 5 -3 0.0695
-6 0 -5 0.0626
-4 -6 -5 0.0676
3 -8 0 0.0956
6 1 5 0.0588
-1 -4 11 0.0705
1 4 -11 0.0705
-2 1 13 0.0741
2 -1 -13 0.0521

_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
5.6890 4.5564 -6.3827 -0.4413 0.8130 0.3798
-5.5545 4.7315 6.4582 0.3401 -0.6196 0.7074
-6.6807 -1.2947 7.5952 0.4781 -0.8778 0.0304
-5.0256 -5.6319 5.5987 0.4058 -0.7487 -0.5242
1.5882 -8.1307 -2.0138 -0.0302 0.0486 -0.9984
6.7191 -0.8328 -7.6916 -0.4598 0.8423 -0.2813
-0.6839 8.2564 2.0675 0.0515 0.0781 0.9956
-5.2770 4.7123 -2.9801 -0.4001 -0.6588 0.6371
-5.8664 -0.3942 -5.1208 -0.5210 -0.8528 0.0356
-3.6759 -5.8080 -4.9933 -0.4017 -0.6533 -0.6418
3.0916 -7.5378 0.2129 0.1698 0.2838 -0.9437
5.7708 1.0233 5.2413 0.5211 0.8525 0.0409
-1.0468 -3.8267 11.4367 0.9279 -0.1221 -0.3523
1.0468 3.8267 -11.4367 -0.9279 0.1221 0.3523
-1.8421 1.3663 12.7245 0.9518 -0.1231 0.2810
1.8421 -1.3663 -12.7245 -0.9518 0.1231 -0.2810

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19536
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.782
_diffrn_reflns_theta_min         4.012
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -22.00   3.00   0.50    5.34    --   49.01 -14.00-144.00   50
  2  ω    -22.00   3.00   0.50    5.34    --  -49.76  14.00  26.00   50
  3  ω   -126.00 -70.00   0.50    5.34    --  -49.76 -14.00-144.00  112
  4  ω   -169.00-141.00   0.50    5.34    --  -92.01 -14.00-144.00   56
  5  ω   -136.00 -38.00   0.50    5.34    --  -92.01 -14.00-144.00  196
  6  ω     29.00  55.00   0.50    5.34    --   96.11  14.00  26.00   52
  7  ω     90.00 138.00   0.50    5.34    --  108.00  14.00  26.00   96
  8  ω     12.00 125.00   0.50    5.34    --   49.01  14.00  26.00  226
  9  ω    -42.00  29.00   0.50    5.34    --  -49.76  38.00 150.00  142
 10  ω    -79.00 -34.00   0.50    5.34    --  -92.01  77.00-180.00   90
 11  ω    -49.00 -14.00   0.50    5.34    --  -92.01  45.00-120.00   70
 12  ω    -50.00 -19.00   0.50    5.34    --  -92.01  45.00 120.00   62
 13  ω   -105.00 -29.00   0.50    5.34    --  -92.01  77.00 120.00  152
 14  ω    -50.00 -22.00   0.50    5.34    --  -92.01  45.00-180.00   56
 15  ω     22.00  47.00   0.50    5.34    --   96.11 -45.00 -90.00   50
 16  ω     69.00 106.00   0.50    5.34    --   96.11  14.00  26.00   74
 17  ω     18.00  51.00   0.50    5.34    --   96.11 -45.00 -30.00   66
 18  ω     36.00  66.00   0.50    5.34    --  108.00 -61.00 120.00   60
 19  ω     34.00  70.00   0.50    5.34    --  108.00 -61.00-150.00   72
 20  ω     53.00 106.00   0.50    5.34    --  108.00 -95.00  90.00  106
 21  ω     35.00  70.00   0.50    5.34    --  108.00 -61.00   0.00   70
 22  ω     44.00  69.00   0.50    5.34    --  108.00 -61.00 -90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix-Arc 100'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0206016000
_diffrn_orient_matrix_UB_12      -0.0118471000
_diffrn_orient_matrix_UB_13      0.0790528000
_diffrn_orient_matrix_UB_21      0.1370060000
_diffrn_orient_matrix_UB_22      0.0187721000
_diffrn_orient_matrix_UB_23      0.0081409000
_diffrn_orient_matrix_UB_31      -0.0197392000
_diffrn_orient_matrix_UB_32      0.1172905000
_diffrn_orient_matrix_UB_33      0.0066317000
_diffrn_oxdiff_digest_frames     
;
01701dc5f645ba54f2386bda7195f117da019585dc0
;
_diffrn_oxdiff_digest_hkl        
;
016fdee114c92103df6dc80e734e9e2ae1c4d6
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4539
_reflns_number_total             5608
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         5608
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0650
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0853P)²+1.4341P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1740
_refine_ls_wR_factor_ref         0.1829
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C24(H24), C25(H25),
 C26(H26), C27(H27)
2.c X=CH2 refined with riding coordinates:
 C14(H14A,H14B)
2.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.60202(7) 0.40753(7) 0.33425(4) 0.0468(2) Uani 1 1 d . . . . .
O1 O 0.40927(15) 0.41935(18) 0.31415(12) 0.0801(6) Uani 1 1 d . . . . .
N1 N 0.83365(16) 0.40208(15) 0.37580(10) 0.0500(5) Uani 1 1 d . . . . .
N2 N 0.67108(17) 0.57280(17) 0.39606(10) 0.0546(5) Uani 1 1 d . . . . .
N3 N 0.6848(2) 0.3833(2) 0.22956(11) 0.0647(6) Uani 1 1 d . . . . .
N4 N 0.65546(19) 0.25370(17) 0.40969(12) 0.0641(6) Uani 1 1 d . . . . .
C1 C 0.8765(2) 0.50790(19) 0.39984(13) 0.0542(6) Uani 1 1 d . . . . .
H1A H 0.884404 0.549532 0.359263 0.065 Uiso 1 1 calc R U . . .
H1B H 0.958158 0.502181 0.431127 0.065 Uiso 1 1 calc R U . . .
C2 C 0.7954(2) 0.5643(2) 0.43678(12) 0.0564(6) Uani 1 1 d . . . . .
H2A H 0.795424 0.527505 0.480517 0.068 Uiso 1 1 calc R U . . .
H2B H 0.828316 0.634762 0.448766 0.068 Uiso 1 1 calc R U . . .
C3 C 0.8811(2) 0.3704(2) 0.31663(15) 0.0599(6) Uani 1 1 d . . . . .
H3A H 0.879691 0.293694 0.313750 0.072 Uiso 1 1 calc R U . . .
H3B H 0.966780 0.392843 0.324553 0.072 Uiso 1 1 calc R U . . .
C4 C 0.8122(2) 0.4135(2) 0.24921(14) 0.0630(7) Uani 1 1 d . . . . .
H4A H 0.817002 0.490116 0.251537 0.076 Uiso 1 1 calc R U . . .
H4B H 0.852185 0.390650 0.212446 0.076 Uiso 1 1 calc R U . . .
C5 C 0.8637(2) 0.3293(2) 0.43415(16) 0.0701(8) Uani 1 1 d . . . . .
H5A H 0.852481 0.364397 0.476534 0.084 Uiso 1 1 calc R U . . .
H5B H 0.950163 0.309280 0.441866 0.084 Uiso 1 1 calc R U . . .
C6 C 0.7852(2) 0.2315(2) 0.42182(17) 0.0681(7) Uani 1 1 d . . . . .
H6A H 0.800816 0.193992 0.381300 0.082 Uiso 1 1 calc R U . . .
H6B H 0.809168 0.185434 0.462587 0.082 Uiso 1 1 calc R U . . .
C7 C 0.5877(3) 0.6063(3) 0.43824(16) 0.0745(8) Uani 1 1 d . . . . .
H7A H 0.608253 0.677092 0.454928 0.112 Uiso 1 1 calc R U . . .
H7B H 0.594843 0.559488 0.477833 0.112 Uiso 1 1 calc R U . . .
H7C H 0.504203 0.604807 0.410130 0.112 Uiso 1 1 calc R U . . .
C8 C 0.6608(3) 0.6477(2) 0.33886(15) 0.0672(7) Uani 1 1 d . . . . .
H8A H 0.716748 0.628027 0.310146 0.101 Uiso 1 1 calc R U . . .
H8B H 0.681473 0.717306 0.357875 0.101 Uiso 1 1 calc R U . . .
H8C H 0.577489 0.647677 0.310557 0.101 Uiso 1 1 calc R U . . .
C9 C 0.6194(4) 0.4480(4) 0.17370(18) 0.1195(16) Uani 1 1 d . . . . .
H9A H 0.534610 0.425350 0.160102 0.179 Uiso 1 1 calc R U . . .
H9B H 0.656587 0.442129 0.134017 0.179 Uiso 1 1 calc R U . . .
H9C H 0.622689 0.520382 0.189129 0.179 Uiso 1 1 calc R U . . .
C10 C 0.6768(3) 0.2742(3) 0.2076(2) 0.1005(12) Uani 1 1 d . . . . .
H10A H 0.719313 0.230543 0.246041 0.151 Uiso 1 1 calc R U . . .
H10B H 0.714392 0.265908 0.168236 0.151 Uiso 1 1 calc R U . . .
H10C H 0.591383 0.253359 0.193880 0.151 Uiso 1 1 calc R U . . .
C11 C 0.5841(3) 0.1638(3) 0.3825(2) 0.0921(11) Uani 1 1 d . . . . .
H11A H 0.497635 0.181444 0.372939 0.138 Uiso 1 1 calc R U . . .
H11B H 0.601105 0.107493 0.416581 0.138 Uiso 1 1 calc R U . . .
H11C H 0.604997 0.141357 0.339649 0.138 Uiso 1 1 calc R U . . .
C12 C 0.6212(4) 0.2904(4) 0.4726(2) 0.1121(14) Uani 1 1 d . . . . .
H12A H 0.642104 0.237351 0.508788 0.168 Uiso 1 1 calc R U . . .
H12B H 0.533679 0.303535 0.462300 0.168 Uiso 1 1 calc R U . . .
H12C H 0.665093 0.354587 0.488635 0.168 Uiso 1 1 calc R U . . .
C13 C 0.30071(18) 0.42877(18) 0.32166(13) 0.0497(5) Uani 1 1 d . . . . .
C14 C 0.2555(2) 0.5042(2) 0.35488(16) 0.0674(7) Uani 1 1 d . . . . .
H14A H 0.306336 0.559219 0.376352 0.081 Uiso 1 1 calc R U . . .
H14B H 0.172552 0.502587 0.356912 0.081 Uiso 1 1 calc R U . . .
C15 C 0.21256(17) 0.34459(17) 0.28780(12) 0.0450(5) Uani 1 1 d . . . . .
C16 C 0.18253(19) 0.26268(17) 0.32723(13) 0.0487(5) Uani 1 1 d . . . . .
C17 C 0.2388(2) 0.2506(2) 0.39881(13) 0.0578(6) Uani 1 1 d . . . . .
H17 H 0.298074 0.299488 0.420751 0.069 Uiso 1 1 calc R U . . .
C18 C 0.2095(3) 0.1706(2) 0.43634(16) 0.0735(8) Uani 1 1 d . . . . .
H18 H 0.249192 0.163557 0.483815 0.088 Uiso 1 1 calc R U . . .
C19 C 0.1197(3) 0.0976(2) 0.40495(17) 0.0806(9) Uani 1 1 d . . . . .
H19 H 0.099415 0.042142 0.431677 0.097 Uiso 1 1 calc R U . . .
C20 C 0.0630(3) 0.1061(2) 0.33747(16) 0.0709(8) Uani 1 1 d . . . . .
H20 H 0.002246 0.057122 0.317560 0.085 Uiso 1 1 calc R U . . .
C21 C 0.0925(2) 0.18748(18) 0.29534(13) 0.0530(6) Uani 1 1 d . . . . .
C22 C 0.0361(2) 0.19709(19) 0.22555(14) 0.0570(7) Uani 1 1 d . . . . .
H22 H -0.025964 0.149521 0.205154 0.068 Uiso 1 1 calc R U . . .
C23 C 0.06882(19) 0.27483(19) 0.18509(13) 0.0525(6) Uani 1 1 d . . . . .
C24 C 0.0151(2) 0.2834(2) 0.11280(14) 0.0637(7) Uani 1 1 d . . . . .
H24 H -0.047812 0.236836 0.091869 0.076 Uiso 1 1 calc R U . . .
C25 C 0.0523(3) 0.3566(2) 0.07365(15) 0.0689(8) Uani 1 1 d . . . . .
H25 H 0.016288 0.360329 0.025481 0.083 Uiso 1 1 calc R U . . .
C26 C 0.1451(3) 0.4284(2) 0.10417(15) 0.0637(7) Uani 1 1 d . . . . .
H26 H 0.171551 0.478818 0.076067 0.076 Uiso 1 1 calc R U . . .
C27 C 0.1957(2) 0.42520(18) 0.17296(13) 0.0537(6) Uani 1 1 d . . . . .
H27 H 0.256046 0.474634 0.192709 0.064 Uiso 1 1 calc R U . . .
C28 C 0.16006(18) 0.34886(17) 0.21634(12) 0.0467(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
Na1 O1 2.1324(18) . ?
Na1 N1 2.5623(19) . ?
Na1 N2 2.492(2) . ?
Na1 N3 2.493(2) . ?
Na1 N4 2.474(2) . ?
Na1 C12 3.100(4) . ?
O1 C13 1.279(3) . ?
N1 C1 1.489(3) . ?
N1 C3 1.461(3) . ?
N1 C5 1.468(3) . ?
N2 C2 1.456(3) . ?
N2 C7 1.467(3) . ?
N2 C8 1.476(4) . ?
N3 C4 1.458(3) . ?
N3 C9 1.447(4) . ?
N3 C10 1.470(4) . ?
N4 C6 1.462(3) . ?
N4 C11 1.444(4) . ?
N4 C12 1.471(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.491(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.492(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.529(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.343(3) . ?
C13 C15 1.521(3) . ?
C14 H14A 0.9500 . ?
C14 H14B 0.9500 . ?
C15 C16 1.403(3) . ?
C15 C28 1.407(3) . ?
C16 C17 1.425(4) . ?
C16 C21 1.442(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.358(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.419(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.350(5) . ?
C20 H20 0.9500 . ?
C20 C21 1.429(4) . ?
C21 C22 1.390(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.388(4) . ?
C23 C24 1.428(4) . ?
C23 C28 1.437(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.352(4) . ?
C25 H25 0.9500 . ?
C25 C26 1.426(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.354(4) . ?
C27 H27 0.9500 . ?
C27 C28 1.427(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
O1 Na1 N1 171.87(8) . . ?
O1 Na1 N2 102.79(8) . . ?
O1 Na1 N3 114.91(8) . . ?
O1 Na1 N4 105.42(9) . . ?
O1 Na1 C12 93.31(11) . . ?
N1 Na1 C12 81.16(10) . . ?
N2 Na1 N1 71.61(7) . . ?
N2 Na1 N3 112.46(8) . . ?
N2 Na1 C12 91.76(9) . . ?
N3 Na1 N1 73.06(7) . . ?
N3 Na1 C12 135.80(11) . . ?
N4 Na1 N1 72.27(7) . . ?
N4 Na1 N2 112.48(8) . . ?
N4 Na1 N3 108.58(8) . . ?
N4 Na1 C12 27.81(10) . . ?
C13 O1 Na1 162.94(19) . . ?
C1 N1 Na1 108.12(13) . . ?
C3 N1 Na1 106.88(13) . . ?
C3 N1 C1 111.16(18) . . ?
C3 N1 C5 113.3(2) . . ?
C5 N1 Na1 107.65(14) . . ?
C5 N1 C1 109.51(19) . . ?
C2 N2 Na1 111.17(15) . . ?
C2 N2 C7 112.0(2) . . ?
C2 N2 C8 111.67(19) . . ?
C7 N2 Na1 111.30(15) . . ?
C7 N2 C8 107.6(2) . . ?
C8 N2 Na1 102.77(15) . . ?
C4 N3 Na1 106.58(15) . . ?
C4 N3 C10 108.8(2) . . ?
C9 N3 Na1 110.1(2) . . ?
C9 N3 C4 110.5(3) . . ?
C9 N3 C10 109.8(3) . . ?
C10 N3 Na1 111.0(2) . . ?
C6 N4 Na1 110.56(15) . . ?
C6 N4 C12 112.2(3) . . ?
C11 N4 Na1 112.4(2) . . ?
C11 N4 C6 111.0(2) . . ?
C11 N4 C12 109.8(3) . . ?
C12 N4 Na1 100.5(2) . . ?
N1 C1 H1A 108.7 . . ?
N1 C1 H1B 108.7 . . ?
N1 C1 C2 114.34(18) . . ?
H1A C1 H1B 107.6 . . ?
C2 C1 H1A 108.7 . . ?
C2 C1 H1B 108.7 . . ?
N2 C2 C1 112.99(19) . . ?
N2 C2 H2A 109.0 . . ?
N2 C2 H2B 109.0 . . ?
C1 C2 H2A 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
N1 C3 H3A 108.8 . . ?
N1 C3 H3B 108.8 . . ?
N1 C3 C4 113.88(19) . . ?
H3A C3 H3B 107.7 . . ?
C4 C3 H3A 108.8 . . ?
C4 C3 H3B 108.8 . . ?
N3 C4 C3 114.8(2) . . ?
N3 C4 H4A 108.6 . . ?
N3 C4 H4B 108.6 . . ?
C3 C4 H4A 108.6 . . ?
C3 C4 H4B 108.6 . . ?
H4A C4 H4B 107.5 . . ?
N1 C5 H5A 109.1 . . ?
N1 C5 H5B 109.1 . . ?
N1 C5 C6 112.4(2) . . ?
H5A C5 H5B 107.9 . . ?
C6 C5 H5A 109.1 . . ?
C6 C5 H5B 109.1 . . ?
N4 C6 C5 113.0(2) . . ?
N4 C6 H6A 109.0 . . ?
N4 C6 H6B 109.0 . . ?
C5 C6 H6A 109.0 . . ?
C5 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 H11A 109.5 . . ?
N4 C11 H11B 109.5 . . ?
N4 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Na1 C12 H12A 161.0 . . ?
Na1 C12 H12B 82.7 . . ?
Na1 C12 H12C 78.6 . . ?
N4 C12 Na1 51.72(17) . . ?
N4 C12 H12A 109.5 . . ?
N4 C12 H12B 109.5 . . ?
N4 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O1 C13 C14 127.9(2) . . ?
O1 C13 C15 115.5(2) . . ?
C14 C13 C15 116.58(19) . . ?
C13 C14 H14A 120.0 . . ?
C13 C14 H14B 120.0 . . ?
H14A C14 H14B 120.0 . . ?
C16 C15 C13 120.6(2) . . ?
C16 C15 C28 119.50(19) . . ?
C28 C15 C13 119.9(2) . . ?
C15 C16 C17 122.0(2) . . ?
C15 C16 C21 120.0(2) . . ?
C17 C16 C21 118.1(2) . . ?
C16 C17 H17 119.3 . . ?
C18 C17 C16 121.4(2) . . ?
C18 C17 H17 119.3 . . ?
C17 C18 H18 119.9 . . ?
C17 C18 C19 120.3(3) . . ?
C19 C18 H18 119.9 . . ?
C18 C19 H19 119.7 . . ?
C20 C19 C18 120.6(3) . . ?
C20 C19 H19 119.7 . . ?
C19 C20 H20 119.3 . . ?
C19 C20 C21 121.3(2) . . ?
C21 C20 H20 119.3 . . ?
C20 C21 C16 118.3(2) . . ?
C22 C21 C16 119.4(2) . . ?
C22 C21 C20 122.3(2) . . ?
C21 C22 H22 119.4 . . ?
C23 C22 C21 121.3(2) . . ?
C23 C22 H22 119.4 . . ?
C22 C23 C24 122.0(2) . . ?
C22 C23 C28 119.4(2) . . ?
C24 C23 C28 118.6(2) . . ?
C23 C24 H24 119.5 . . ?
C25 C24 C23 121.1(3) . . ?
C25 C24 H24 119.5 . . ?
C24 C25 H25 119.8 . . ?
C24 C25 C26 120.4(3) . . ?
C26 C25 H25 119.8 . . ?
C25 C26 H26 119.8 . . ?
C27 C26 C25 120.4(3) . . ?
C27 C26 H26 119.8 . . ?
C26 C27 H27 119.4 . . ?
C26 C27 C28 121.2(2) . . ?
C28 C27 H27 119.4 . . ?
C15 C28 C23 120.1(2) . . ?
C15 C28 C27 121.6(2) . . ?
C27 C28 C23 118.3(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
Na1 O1 C13 C14 54.2(8) . . . . ?
Na1 O1 C13 C15 -126.7(6) . . . . ?
Na1 N1 C1 C2 37.7(2) . . . . ?
Na1 N1 C3 C4 37.0(2) . . . . ?
Na1 N1 C5 C6 41.6(3) . . . . ?
Na1 N2 C2 C1 41.7(2) . . . . ?
Na1 N3 C4 C3 46.2(2) . . . . ?
Na1 N4 C6 C5 41.1(3) . . . . ?
O1 C13 C15 C16 100.3(3) . . . . ?
O1 C13 C15 C28 -79.9(3) . . . . ?
N1 C1 C2 N2 -55.9(3) . . . . ?
N1 C3 C4 N3 -60.6(3) . . . . ?
N1 C5 C6 N4 -58.6(4) . . . . ?
C1 N1 C3 C4 -80.8(2) . . . . ?
C1 N1 C5 C6 159.0(2) . . . . ?
C3 N1 C1 C2 154.7(2) . . . . ?
C3 N1 C5 C6 -76.3(3) . . . . ?
C5 N1 C1 C2 -79.3(3) . . . . ?
C5 N1 C3 C4 155.4(2) . . . . ?
C6 N4 C12 Na1 117.5(2) . . . . ?
C7 N2 C2 C1 166.8(2) . . . . ?
C8 N2 C2 C1 -72.5(3) . . . . ?
C9 N3 C4 C3 165.7(3) . . . . ?
C10 N3 C4 C3 -73.6(3) . . . . ?
C11 N4 C6 C5 166.5(3) . . . . ?
C11 N4 C12 Na1 -118.6(3) . . . . ?
C12 N4 C6 C5 -70.2(3) . . . . ?
C13 C15 C16 C17 -4.5(3) . . . . ?
C13 C15 C16 C21 175.70(19) . . . . ?
C13 C15 C28 C23 -174.56(18) . . . . ?
C13 C15 C28 C27 5.9(3) . . . . ?
C14 C13 C15 C16 -80.5(3) . . . . ?
C14 C13 C15 C28 99.3(3) . . . . ?
C15 C16 C17 C18 -179.6(2) . . . . ?
C15 C16 C21 C20 -179.0(2) . . . . ?
C15 C16 C21 C22 -0.1(3) . . . . ?
C16 C15 C28 C23 5.2(3) . . . . ?
C16 C15 C28 C27 -174.34(19) . . . . ?
C16 C17 C18 C19 -1.0(4) . . . . ?
C16 C21 C22 C23 3.1(3) . . . . ?
C17 C16 C21 C20 1.1(3) . . . . ?
C17 C16 C21 C22 -179.9(2) . . . . ?
C17 C18 C19 C20 0.4(5) . . . . ?
C18 C19 C20 C21 1.0(5) . . . . ?
C19 C20 C21 C16 -1.8(4) . . . . ?
C19 C20 C21 C22 179.3(3) . . . . ?
C20 C21 C22 C23 -178.0(2) . . . . ?
C21 C16 C17 C18 0.2(4) . . . . ?
C21 C22 C23 C24 177.6(2) . . . . ?
C21 C22 C23 C28 -2.0(3) . . . . ?
C22 C23 C24 C25 -176.8(2) . . . . ?
C22 C23 C28 C15 -2.2(3) . . . . ?
C22 C23 C28 C27 177.31(19) . . . . ?
C23 C24 C25 C26 -1.1(4) . . . . ?
C24 C23 C28 C15 178.23(19) . . . . ?
C24 C23 C28 C27 -2.2(3) . . . . ?
C24 C25 C26 C27 -1.1(4) . . . . ?
C25 C26 C27 C28 1.5(4) . . . . ?
C26 C27 C28 C15 179.7(2) . . . . ?
C26 C27 C28 C23 0.2(3) . . . . ?
C28 C15 C16 C17 175.8(2) . . . . ?
C28 C15 C16 C21 -4.0(3) . . . . ?
C28 C23 C24 C25 2.7(3) . . . . ?

_shelx_SHELXL_version_number     2019/1
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.394
_oxdiff_exptl_absorpt_empirical_full_min 0.443
####################################################################### 
# 
# 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_elu230015_fa
_database_code_depnum_ccdc_archive 'CCDC 2307288'
loop_
_audit_author_name
_audit_author_address
'Paul G. Waddell'
;School of Natural and Environmental Sciences, Newcastle University
United Kingdom
;
_audit_update_record             
;
2023-11-11 deposited with the CCDC.	2024-02-12 downloaded from the CCDC.
;
_audit_creation_date             2023-09-18
_audit_creation_method           
;
Olex2 1.5-ac5-023
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C164.898 H125.796 K8 O8'
_chemical_formula_sum            'C164.90 H125.79 K8 O8'
_chemical_formula_weight         2548.01
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C20 H23 K1 O1 Si1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_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'
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                   20.2465(4)
_cell_length_b                   24.7118(4)
_cell_length_c                   28.6260(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     14322.4(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    29126
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      71.9860
_cell_measurement_theta_min      3.1740
_shelx_estimated_absorpt_T_max   0.904
_shelx_estimated_absorpt_T_min   0.683
_exptl_absorpt_coefficient_mu    2.584
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.702
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             5325
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.0291
0 -1 0 0.0071
1 0 -2 0.0580
-1 0 2 0.0580
-1 0 -2 0.0628
1 0 2 0.0368

_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0000 1.0000 -0.0000 -0.0340 0.0518 0.0064
-0.0000 -1.0000 0.0000 0.0340 -0.0518 -0.0064
1.0000 -0.0000 -2.0000 0.1009 0.0587 0.0612
-1.0000 0.0000 2.0000 -0.1009 -0.0587 -0.0612
-1.0000 0.0000 -2.0000 0.0761 0.0609 -0.0888
1.0000 -0.0000 2.0000 -0.0761 -0.0609 0.0888

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            72419
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.159
_diffrn_reflns_theta_min         3.088
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     52.00 116.00   0.50    9.29    --   46.35 158.00-128.00  128
  2  ω   -109.00 -17.00   0.50    9.29    --  -92.45 119.00  76.00  184
  3  ω   -168.00 -75.00   0.50    9.29    --  -92.45-122.00 -97.00  186
  4  ω     39.00 178.00   0.50    9.29    --  108.07  12.00 -98.00  278
  5  ω    -35.00  24.00   0.50    9.29    --   46.35 -12.00  89.00  118
  6  ω     74.00 106.00   0.50    9.29    --   46.35 125.00 -60.00   64
  7  ω    -41.00  33.00   0.50    9.29    --  -47.35  38.00  30.00  148
  8  ω     -6.00  34.00   0.50    9.29    --  -47.35  12.00 -98.00   80
  9  ω    -48.00 -11.00   0.50    9.29    --  -92.45  45.00-150.00   74
 10  ω    -49.00 -15.00   0.50    9.29    --  -92.45  45.00 -60.00   68
 11  ω     26.00  51.00   0.50    9.29    --   97.10 -45.00  60.00   50
 12  ω     77.00 105.00   0.50    9.29    --  108.07 -95.00 -30.00   56
 13  ω     48.00  73.00   0.50    9.29    --  108.07 -95.00 -30.00   50
 14  ω     35.00  82.00   0.50    9.29    --  108.07 -95.00 -90.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix-Arc 100'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0124300000
_diffrn_orient_matrix_UB_12      -0.0340404000
_diffrn_orient_matrix_UB_13      -0.0442493000
_diffrn_orient_matrix_UB_21      -0.0011095000
_diffrn_orient_matrix_UB_22      0.0518432000
_diffrn_orient_matrix_UB_23      -0.0299086000
_diffrn_orient_matrix_UB_31      0.0749961000
_diffrn_orient_matrix_UB_32      0.0063928000
_diffrn_orient_matrix_UB_33      0.0069171000
_diffrn_oxdiff_digest_frames     
;
01b55740b005ecaa278382756d96a3b7ef01578166c
;
_diffrn_oxdiff_digest_hkl        
;
015014877ae46d8502db67d10d72ed63c80149
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11956
_reflns_number_total             14282
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         14282
_refine_ls_number_restraints     1246
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0555
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0930P)²+7.5317P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1630
_refine_ls_wR_factor_ref         0.1697
_refine_special_details          
;
It appears that there are both benzene and toluene 
molecules occupying the same positions throughout the 
crystal manifesting as disorder. One such site has been 
modelled as substitutionally disordered. The occupancy of 
the methyl group of the toluene was allowed to refine 
independently of the atomic displacement parameters and 
fixed before anisotropy was introduced into the model. The 
asymmetric unit also contains a solvent-accessible void in 
which there appear to be multiple orientations of both 
toluene and benzene. An unambiguous model for these 
solvent molecules in this site could not be achieved and 
hence the associated electron density was treated using 
the Olex2 solvent mask routine.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: H77(0.55098) C83(0.44902) H83A(0.44902) H83B(0.44902) H83C(0.44902)
4.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C28(H28), C29(H29),
  C30(H30), C31(H31), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42),
 C44(H44), C45(H45), C46(H46), C47(H47), C53(H53), C54(H54), C55(H55), C56(H56),
  C58(H58), C60(H60), C61(H61), C62(H62), C63(H63), C65(H65), C66(H66),
 C67(H67), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72), C73(H73), C74(H74),
  C75(H75), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80), C81(H81), C82(H82)
4.b X=CH2 refined with riding coordinates:
 C2(H2A,H2B), C18(H18A,H18B), C34(H34A,H34B), C50(H50A,H50B)
4.c Idealised Me refined as rotating group:
 C83(H83A,H83B,H83C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.55565(3) 0.55600(2) 0.42632(2) 0.04971(14) Uani 1 1 d . . . . .
K2 K 0.39247(3) 0.55797(2) 0.35770(2) 0.06225(17) Uani 1 1 d . . . . .
K3 K 0.52926(3) 0.64984(2) 0.31460(2) 0.06345(18) Uani 1 1 d . . . . .
K4 K 0.44036(3) 0.68116(2) 0.43304(2) 0.05140(14) Uani 1 1 d . . . . .
O1 O 0.51355(11) 0.54651(7) 0.34006(7) 0.0655(5) Uani 1 1 d . . . . .
O2 O 0.42385(8) 0.57405(7) 0.44265(6) 0.0499(4) Uani 1 1 d . . . . .
O3 O 0.56232(9) 0.65943(7) 0.40268(7) 0.0565(4) Uani 1 1 d . . . . .
O4 O 0.40917(10) 0.66247(8) 0.34810(7) 0.0611(5) Uani 1 1 d . . . . .
C1 C 0.53429(13) 0.51072(9) 0.31027(8) 0.0502(5) Uani 1 1 d . . . . .
C2 C 0.51315(17) 0.50514(13) 0.26631(10) 0.0690(8) Uani 1 1 d . . . . .
H2A H 0.480038 0.528648 0.254429 0.083 Uiso 1 1 calc R U . . .
H2B H 0.531236 0.477670 0.246937 0.083 Uiso 1 1 calc R U . . .
C3 C 0.58801(14) 0.47363(9) 0.32869(7) 0.0490(5) Uani 1 1 d . . . . .
C4 C 0.57328(14) 0.42090(10) 0.34318(8) 0.0518(6) Uani 1 1 d . . . . .
C5 C 0.50828(16) 0.40032(10) 0.34191(9) 0.0605(7) Uani 1 1 d . . . . .
H5 H 0.473532 0.422794 0.330911 0.073 Uiso 1 1 calc R U . . .
C6 C 0.49407(18) 0.34853(12) 0.35621(11) 0.0700(8) Uani 1 1 d . . . . .
H6 H 0.450054 0.335263 0.355192 0.084 Uiso 1 1 calc R U . . .
C7 C 0.54673(19) 0.31490(11) 0.37266(10) 0.0691(8) Uani 1 1 d . . . . .
H7 H 0.537322 0.278927 0.382297 0.083 Uiso 1 1 calc R U . . .
C8 C 0.60866(18) 0.33298(11) 0.37475(10) 0.0643(7) Uani 1 1 d . . . . .
H8 H 0.642357 0.309560 0.385905 0.077 Uiso 1 1 calc R U . . .
C9 C 0.62567(16) 0.38641(10) 0.36074(8) 0.0575(6) Uani 1 1 d . . . . .
C10 C 0.68898(16) 0.40652(12) 0.36338(9) 0.0600(6) Uani 1 1 d . . . . .
H10 H 0.723260 0.383392 0.374089 0.072 Uiso 1 1 calc R U . . .
C11 C 0.70444(15) 0.45856(11) 0.35116(9) 0.0592(6) Uani 1 1 d . . . . .
C12 C 0.77006(16) 0.48051(15) 0.35579(11) 0.0723(8) Uani 1 1 d . . . . .
H12 H 0.804405 0.458226 0.367671 0.087 Uiso 1 1 calc R U . . .
C13 C 0.78393(18) 0.53269(15) 0.34344(12) 0.0770(9) Uani 1 1 d . . . . .
H13 H 0.827538 0.546398 0.346635 0.092 Uiso 1 1 calc R U . . .
C14 C 0.73315(17) 0.56612(13) 0.32591(11) 0.0699(8) Uani 1 1 d . . . . .
H14 H 0.742839 0.602562 0.317853 0.084 Uiso 1 1 calc R U . . .
C15 C 0.67108(15) 0.54729(11) 0.32039(9) 0.0592(6) Uani 1 1 d . . . . .
H15 H 0.638341 0.570535 0.307646 0.071 Uiso 1 1 calc R U . . .
C16 C 0.65320(14) 0.49321(10) 0.33320(8) 0.0525(6) Uani 1 1 d . . . . .
C17 C 0.40573(11) 0.56873(9) 0.48631(8) 0.0422(5) Uani 1 1 d . . . . .
C18 C 0.44259(13) 0.58182(12) 0.52380(10) 0.0587(7) Uani 1 1 d . . . . .
H18A H 0.485686 0.596251 0.519677 0.070 Uiso 1 1 calc R U . . .
H18B H 0.425499 0.576611 0.554383 0.070 Uiso 1 1 calc R U . . .
C19 C 0.33769(11) 0.54534(9) 0.49430(7) 0.0396(4) Uani 1 1 d . . . . .
C20 C 0.28503(11) 0.57761(9) 0.51052(7) 0.0423(5) Uani 1 1 d . . . . .
C21 C 0.29210(13) 0.63415(10) 0.52045(8) 0.0473(5) Uani 1 1 d . . . . .
H21 H 0.333663 0.651098 0.515616 0.057 Uiso 1 1 calc R U . . .
C22 C 0.24043(14) 0.66414(11) 0.53669(9) 0.0557(6) Uani 1 1 d . . . . .
H22 H 0.246599 0.701551 0.542964 0.067 Uiso 1 1 calc R U . . .
C23 C 0.17800(14) 0.64046(12) 0.54432(10) 0.0607(7) Uani 1 1 d . . . . .
H23 H 0.142653 0.661708 0.556152 0.073 Uiso 1 1 calc R U . . .
C24 C 0.16852(14) 0.58736(12) 0.53475(10) 0.0589(6) Uani 1 1 d . . . . .
H24 H 0.126148 0.571866 0.539670 0.071 Uiso 1 1 calc R U . . .
C25 C 0.22105(12) 0.55395(10) 0.51735(8) 0.0487(5) Uani 1 1 d . . . . .
C26 C 0.21131(12) 0.49945(11) 0.50735(9) 0.0520(6) Uani 1 1 d . . . . .
H26 H 0.168789 0.484052 0.511861 0.062 Uiso 1 1 calc R U . . .
C27 C 0.26239(12) 0.46696(10) 0.49089(8) 0.0456(5) Uani 1 1 d . . . . .
C28 C 0.25272(14) 0.41098(10) 0.48002(9) 0.0529(6) Uani 1 1 d . . . . .
H28 H 0.210004 0.395578 0.483464 0.064 Uiso 1 1 calc R U . . .
C29 C 0.30301(14) 0.37959(10) 0.46497(9) 0.0542(6) Uani 1 1 d . . . . .
H29 H 0.295556 0.342433 0.458265 0.065 Uiso 1 1 calc R U . . .
C30 C 0.36713(13) 0.40212(9) 0.45914(8) 0.0487(5) Uani 1 1 d . . . . .
H30 H 0.402487 0.379789 0.448931 0.058 Uiso 1 1 calc R U . . .
C31 C 0.37821(12) 0.45548(9) 0.46810(7) 0.0418(5) Uani 1 1 d . . . . .
H31 H 0.421191 0.469924 0.463451 0.050 Uiso 1 1 calc R U . . .
C32 C 0.32673(11) 0.49022(9) 0.48431(7) 0.0398(4) Uani 1 1 d . . . . .
C33 C 0.59910(12) 0.69727(9) 0.42123(9) 0.0473(5) Uani 1 1 d . . . . .
C34 C 0.59683(15) 0.71396(12) 0.46590(9) 0.0610(7) Uani 1 1 d . . . . .
H34A H 0.566480 0.697870 0.487059 0.073 Uiso 1 1 calc R U . . .
H34B H 0.625579 0.741850 0.476314 0.073 Uiso 1 1 calc R U . . .
C35 C 0.64701(12) 0.72411(9) 0.38786(8) 0.0472(5) Uani 1 1 d . . . . .
C36 C 0.71230(12) 0.70552(10) 0.38487(8) 0.0481(5) Uani 1 1 d . . . . .
C37 C 0.73700(13) 0.66294(11) 0.41372(9) 0.0526(6) Uani 1 1 d . . . . .
H37 H 0.708473 0.646626 0.435984 0.063 Uiso 1 1 calc R U . . .
C38 C 0.80011(14) 0.64524(12) 0.41010(10) 0.0611(7) Uani 1 1 d . . . . .
H38 H 0.815456 0.617367 0.430209 0.073 Uiso 1 1 calc R U . . .
C39 C 0.84350(15) 0.66806(13) 0.37646(10) 0.0652(7) Uani 1 1 d . . . . .
H39 H 0.887356 0.654765 0.373694 0.078 Uiso 1 1 calc R U . . .
C40 C 0.82274(14) 0.70864(12) 0.34832(10) 0.0620(7) Uani 1 1 d . . . . .
H40 H 0.852267 0.723549 0.325971 0.074 Uiso 1 1 calc R U . . .
C41 C 0.75739(13) 0.72927(11) 0.35171(9) 0.0548(6) Uani 1 1 d . . . . .
C42 C 0.73593(15) 0.77283(12) 0.32416(10) 0.0630(7) Uani 1 1 d . . . . .
H42 H 0.766013 0.789340 0.303055 0.076 Uiso 1 1 calc R U . . .
C43 C 0.67218(15) 0.79221(11) 0.32702(10) 0.0614(7) Uani 1 1 d . . . . .
C44 C 0.64926(19) 0.83627(14) 0.29901(12) 0.0804(9) Uani 1 1 d . . . . .
H44 H 0.679417 0.854136 0.278797 0.097 Uiso 1 1 calc R U . . .
C45 C 0.5862(2) 0.85307(15) 0.30053(13) 0.0886(11) Uani 1 1 d . . . . .
H45 H 0.572378 0.882540 0.281584 0.106 Uiso 1 1 calc R U . . .
C46 C 0.53984(18) 0.82687(14) 0.33043(12) 0.0767(9) Uani 1 1 d . . . . .
H46 H 0.495051 0.838320 0.330768 0.092 Uiso 1 1 calc R U . . .
C47 C 0.55963(15) 0.78549(11) 0.35847(10) 0.0615(7) Uani 1 1 d . . . . .
H47 H 0.528252 0.768828 0.378520 0.074 Uiso 1 1 calc R U . . .
C48 C 0.62583(14) 0.76648(10) 0.35865(9) 0.0522(6) Uani 1 1 d . . . . .
C49 C 0.36509(13) 0.66995(10) 0.31516(8) 0.0498(5) Uani 1 1 d . . . . .
C50 C 0.35963(16) 0.64155(11) 0.27523(9) 0.0607(7) Uani 1 1 d . . . . .
H50A H 0.389596 0.612911 0.268823 0.073 Uiso 1 1 calc R U . . .
H50B H 0.325813 0.650138 0.253454 0.073 Uiso 1 1 calc R U . . .
C51 C 0.31776(12) 0.71593(9) 0.32414(8) 0.0449(5) Uani 1 1 d . . . . .
C52 C 0.26425(12) 0.70903(9) 0.35534(8) 0.0461(5) Uani 1 1 d . . . . .
C53 C 0.25300(14) 0.65935(10) 0.37974(9) 0.0531(6) Uani 1 1 d . . . . .
H53 H 0.281779 0.629575 0.374624 0.064 Uiso 1 1 calc R U . . .
C54 C 0.20189(14) 0.65407(11) 0.41007(10) 0.0590(6) Uani 1 1 d . . . . .
H54 H 0.195829 0.620839 0.426189 0.071 Uiso 1 1 calc R U . . .
C55 C 0.15782(14) 0.69700(12) 0.41799(10) 0.0612(7) Uani 1 1 d . . . . .
H55 H 0.122279 0.692647 0.439328 0.073 Uiso 1 1 calc R U . . .
C56 C 0.16596(14) 0.74467(12) 0.39520(10) 0.0597(6) Uani 1 1 d . . . . .
H56 H 0.135409 0.773200 0.400492 0.072 Uiso 1 1 calc R U . . .
C57 C 0.21942(12) 0.75293(10) 0.36345(9) 0.0499(5) Uani 1 1 d . . . . .
C58 C 0.22955(14) 0.80208(10) 0.34060(10) 0.0552(6) Uani 1 1 d . . . . .
H58 H 0.199112 0.830801 0.345437 0.066 Uiso 1 1 calc R U . . .
C59 C 0.28309(13) 0.81017(10) 0.31091(9) 0.0501(5) Uani 1 1 d . . . . .
C60 C 0.29535(15) 0.86104(10) 0.28882(9) 0.0576(6) Uani 1 1 d . . . . .
H60 H 0.265629 0.890183 0.293987 0.069 Uiso 1 1 calc R U . . .
C61 C 0.34830(15) 0.86872(11) 0.26069(9) 0.0586(6) Uani 1 1 d . . . . .
H61 H 0.355205 0.902899 0.246309 0.070 Uiso 1 1 calc R U . . .
C62 C 0.39352(14) 0.82583(11) 0.25263(9) 0.0558(6) Uani 1 1 d . . . . .
H62 H 0.430963 0.831562 0.233255 0.067 Uiso 1 1 calc R U . . .
C63 C 0.38338(13) 0.77636(10) 0.27264(8) 0.0509(5) Uani 1 1 d . . . . .
H63 H 0.413808 0.747954 0.266562 0.061 Uiso 1 1 calc R U . . .
C64 C 0.32821(12) 0.76622(9) 0.30245(8) 0.0462(5) Uani 1 1 d . . . . .
C65 C 0.32960(18) 0.44433(13) 0.34401(12) 0.0729(8) Uani 1 1 d . . . . .
H65 H 0.354939 0.419933 0.362355 0.087 Uiso 1 1 calc R U . . .
C66 C 0.27703(19) 0.47029(17) 0.36306(12) 0.0843(10) Uani 1 1 d . . . . .
H66 H 0.265948 0.464434 0.394906 0.101 Uiso 1 1 calc R U . . .
C67 C 0.2388(2) 0.50595(19) 0.33568(16) 0.1013(12) Uani 1 1 d . . . . .
H67 H 0.202027 0.524488 0.348697 0.122 Uiso 1 1 calc R U . . .
C68 C 0.2560(3) 0.51311(16) 0.29007(14) 0.0984(12) Uani 1 1 d . . . . .
H68 H 0.230526 0.536475 0.270834 0.118 Uiso 1 1 calc R U . . .
C69 C 0.3090(2) 0.48725(16) 0.27194(13) 0.0913(11) Uani 1 1 d . . . . .
H69 H 0.320403 0.492927 0.240130 0.110 Uiso 1 1 calc R U . . .
C70 C 0.3460(2) 0.45340(16) 0.29838(12) 0.0840(10) Uani 1 1 d . . . . .
H70 H 0.383375 0.435928 0.285177 0.101 Uiso 1 1 calc R U . . .
C71 C 0.6393(2) 0.65225(17) 0.22138(13) 0.0843(9) Uani 1 1 d . . . . .
H71 H 0.681624 0.637171 0.227380 0.101 Uiso 1 1 calc R U . . .
C72 C 0.6285(3) 0.70512(19) 0.23017(14) 0.1014(12) Uani 1 1 d . . . . .
H72 H 0.662502 0.727631 0.242184 0.122 Uiso 1 1 calc R U . . .
C73 C 0.5650(3) 0.72583(18) 0.22093(15) 0.1087(14) Uani 1 1 d . . . . .
H73 H 0.555375 0.762785 0.227027 0.130 Uiso 1 1 calc R U . . .
C74 C 0.5171(2) 0.6923(2) 0.20303(15) 0.1102(14) Uani 1 1 d . . . . .
H74 H 0.474319 0.706245 0.196682 0.132 Uiso 1 1 calc R U . . .
C75 C 0.5305(2) 0.6394(2) 0.19437(14) 0.1039(12) Uani 1 1 d . . . . .
H75 H 0.497924 0.616066 0.181600 0.125 Uiso 1 1 calc R U . . .
C76 C 0.5917(2) 0.62103(17) 0.20449(14) 0.0892(10) Uani 1 1 d . . . . .
H76 H 0.601093 0.583857 0.199237 0.107 Uiso 1 1 calc R U . . .
C77 C 0.4563(2) 0.8202(2) 0.47131(19) 0.1102(14) Uani 1 1 d . . . . .
H77 H 0.498234 0.837386 0.470966 0.132 Uiso 0.551 1 calc R U P A 2
C78 C 0.4146(2) 0.82416(15) 0.43277(15) 0.0934(11) Uani 1 1 d . . . . .
H78 H 0.428530 0.843819 0.406005 0.112 Uiso 1 1 calc R U . . .
C79 C 0.35479(19) 0.80044(13) 0.43305(12) 0.0743(8) Uani 1 1 d . . . . .
H79 H 0.326709 0.803132 0.406558 0.089 Uiso 1 1 calc R U . . .
C80 C 0.33478(17) 0.77256(12) 0.47152(11) 0.0677(7) Uani 1 1 d . . . . .
H80 H 0.292441 0.755990 0.471817 0.081 Uiso 1 1 calc R U . . .
C81 C 0.37529(18) 0.76807(12) 0.51014(11) 0.0704(8) Uani 1 1 d . . . . .
H81 H 0.360373 0.748800 0.536845 0.084 Uiso 1 1 calc R U . . .
C82 C 0.4362(2) 0.79095(18) 0.51027(14) 0.0953(11) Uani 1 1 d . . . . .
H82 H 0.464595 0.787057 0.536484 0.114 Uiso 1 1 calc R U . . .
C83 C 0.5111(6) 0.8555(5) 0.4738(5) 0.141(4) Uani 0.449 1 d . . P B 1
H83A H 0.501006 0.889009 0.456843 0.212 Uiso 0.449 1 calc R U P B 1
H83B H 0.549680 0.838085 0.459610 0.212 Uiso 0.449 1 calc R U P B 1
H83C H 0.520579 0.864012 0.506522 0.212 Uiso 0.449 1 calc R U P B 1


_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 K2 3.8438(8) . ?
K1 K3 3.9860(7) . ?
K1 K4 3.8795(8) . ?
K1 O1 2.6227(19) . ?
K1 O2 2.7455(18) . ?
K1 O3 2.6472(18) . ?
K1 C1 3.532(2) . ?
K1 C3 3.519(2) . ?
K1 C17 3.502(2) . ?
K1 C31 3.318(2) 5_666 ?
K2 K3 3.7878(9) . ?
K2 O1 2.519(2) . ?
K2 O2 2.5445(18) . ?
K2 O4 2.619(2) . ?
K2 C1 3.384(3) . ?
K2 C49 3.074(2) . ?
K2 C50 3.207(3) . ?
K2 C65 3.108(3) . ?
K2 C66 3.191(4) . ?
K2 C67 3.425(5) . ?
K2 C69 3.455(4) . ?
K2 C70 3.232(3) . ?
K3 O1 2.674(2) . ?
K3 O3 2.619(2) . ?
K3 O4 2.632(2) . ?
K3 C1 3.441(2) . ?
K3 C49 3.361(3) . ?
K3 C71 3.477(4) . ?
K3 C72 3.427(4) . ?
K3 C73 3.353(4) . ?
K3 C74 3.371(4) . ?
K3 C75 3.451(4) . ?
K3 C76 3.470(4) . ?
K4 O2 2.6821(17) . ?
K4 O3 2.6723(19) . ?
K4 O4 2.5543(19) . ?
K4 C17 3.246(2) . ?
K4 C33 3.256(3) . ?
K4 C34 3.403(3) . ?
K4 C79 3.419(3) . ?
K4 C80 3.299(3) . ?
K4 C81 3.350(3) . ?
K4 C82 3.501(4) . ?
O1 C1 1.298(3) . ?
O2 C17 1.309(3) . ?
O3 C33 1.308(3) . ?
O4 C49 1.311(3) . ?
C1 C2 1.336(4) . ?
C1 C3 1.517(4) . ?
C2 H2A 0.9500 . ?
C2 H2B 0.9500 . ?
C3 C4 1.400(3) . ?
C3 C16 1.412(4) . ?
C4 C5 1.411(4) . ?
C4 C9 1.451(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.374(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.431(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.333(5) . ?
C8 H8 0.9500 . ?
C8 C9 1.422(4) . ?
C9 C10 1.377(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.369(4) . ?
C11 C12 1.441(5) . ?
C11 C16 1.440(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.366(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.411(5) . ?
C14 H14 0.9500 . ?
C14 C15 1.349(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.432(4) . ?
C17 C18 1.347(3) . ?
C17 C19 1.511(3) . ?
C18 H18A 0.9500 . ?
C18 H18B 0.9500 . ?
C19 C20 1.410(3) . ?
C19 C32 1.409(3) . ?
C20 C21 1.433(3) . ?
C20 C25 1.434(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.364(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.410(4) . ?
C23 H23 0.9500 . ?
C23 C24 1.354(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.436(4) . ?
C25 C26 1.391(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.392(3) . ?
C27 C28 1.431(3) . ?
C27 C32 1.436(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.351(4) . ?
C29 H29 0.9500 . ?
C29 C30 1.422(4) . ?
C30 H30 0.9500 . ?
C30 C31 1.362(3) . ?
C31 H31 0.9500 . ?
C31 C32 1.428(3) . ?
C33 C34 1.344(4) . ?
C33 C35 1.514(3) . ?
C34 H34A 0.9500 . ?
C34 H34B 0.9500 . ?
C35 C36 1.402(4) . ?
C35 C48 1.407(4) . ?
C36 C37 1.428(4) . ?
C36 C41 1.442(3) . ?
C37 H37 0.9500 . ?
C37 C38 1.354(4) . ?
C38 H38 0.9500 . ?
C38 C39 1.420(4) . ?
C39 H39 0.9500 . ?
C39 C40 1.353(4) . ?
C40 H40 0.9500 . ?
C40 C41 1.421(4) . ?
C41 C42 1.403(4) . ?
C42 H42 0.9500 . ?
C42 C43 1.379(4) . ?
C43 C44 1.430(4) . ?
C43 C48 1.451(4) . ?
C44 H44 0.9500 . ?
C44 C45 1.344(5) . ?
C45 H45 0.9500 . ?
C45 C46 1.425(5) . ?
C46 H46 0.9500 . ?
C46 C47 1.360(4) . ?
C47 H47 0.9500 . ?
C47 C48 1.420(4) . ?
C49 C50 1.346(4) . ?
C49 C51 1.508(3) . ?
C50 H50A 0.9500 . ?
C50 H50B 0.9500 . ?
C51 C52 1.414(3) . ?
C51 C64 1.405(3) . ?
C52 C53 1.431(3) . ?
C52 C57 1.433(3) . ?
C53 H53 0.9500 . ?
C53 C54 1.357(4) . ?
C54 H54 0.9500 . ?
C54 C55 1.405(4) . ?
C55 H55 0.9500 . ?
C55 C56 1.357(4) . ?
C56 H56 0.9500 . ?
C56 C57 1.428(4) . ?
C57 C58 1.395(3) . ?
C58 H58 0.9500 . ?
C58 C59 1.392(4) . ?
C59 C60 1.429(3) . ?
C59 C64 1.440(3) . ?
C60 H60 0.9500 . ?
C60 C61 1.354(4) . ?
C61 H61 0.9500 . ?
C61 C62 1.419(4) . ?
C62 H62 0.9500 . ?
C62 C63 1.366(4) . ?
C63 H63 0.9500 . ?
C63 C64 1.428(3) . ?
C65 H65 0.9500 . ?
C65 C66 1.357(5) . ?
C65 C70 1.366(5) . ?
C66 H66 0.9500 . ?
C66 C67 1.411(6) . ?
C67 H67 0.9500 . ?
C67 C68 1.363(6) . ?
C68 H68 0.9500 . ?
C68 C69 1.352(6) . ?
C69 H69 0.9500 . ?
C69 C70 1.355(5) . ?
C70 H70 0.9500 . ?
C71 H71 0.9500 . ?
C71 C72 1.348(6) . ?
C71 C76 1.326(6) . ?
C72 H72 0.9500 . ?
C72 C73 1.408(7) . ?
C73 H73 0.9500 . ?
C73 C74 1.375(7) . ?
C74 H74 0.9500 . ?
C74 C75 1.358(7) . ?
C75 H75 0.9500 . ?
C75 C76 1.350(6) . ?
C76 H76 0.9500 . ?
C77 H77 0.9500 . ?
C77 C78 1.392(7) . ?
C77 C82 1.390(6) . ?
C77 C83 1.414(11) . ?
C78 H78 0.9500 . ?
C78 C79 1.345(6) . ?
C79 H79 0.9500 . ?
C79 C80 1.361(5) . ?
C80 H80 0.9500 . ?
C80 C81 1.381(5) . ?
C81 H81 0.9500 . ?
C81 C82 1.357(5) . ?
C82 H82 0.9500 . ?
C83 H83A 0.9800 . ?
C83 H83B 0.9800 . ?
C83 H83C 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
K2 K1 K3 57.829(16) . . ?
K2 K1 K4 59.878(14) . . ?
K4 K1 K3 59.695(14) . . ?
O1 K1 K2 40.60(5) . . ?
O1 K1 K3 41.68(4) . . ?
O1 K1 K4 85.55(4) . . ?
O1 K1 O2 81.89(6) . . ?
O1 K1 O3 82.08(6) . . ?
O1 K1 C1 17.52(6) . . ?
O1 K1 C3 42.36(6) . . ?
O1 K1 C17 100.84(6) . . ?
O1 K1 C31 168.85(6) . 5_666 ?
O2 K1 K2 41.37(4) . . ?
O2 K1 K3 84.95(4) . . ?
O2 K1 K4 43.73(4) . . ?
O2 K1 C1 95.32(6) . . ?
O2 K1 C3 114.21(6) . . ?
O2 K1 C17 19.85(5) . . ?
O2 K1 C31 104.54(6) . 5_666 ?
O3 K1 K2 84.32(4) . . ?
O3 K1 K3 40.55(4) . . ?
O3 K1 K4 43.43(4) . . ?
O3 K1 O2 86.35(5) . . ?
O3 K1 C1 94.11(6) . . ?
O3 K1 C3 110.24(6) . . ?
O3 K1 C17 94.76(5) . . ?
O3 K1 C31 107.15(6) . 5_666 ?
C1 K1 K2 54.42(5) . . ?
C1 K1 K3 54.08(4) . . ?
C1 K1 K4 103.04(4) . . ?
C3 K1 K2 76.20(5) . . ?
C3 K1 K3 74.00(4) . . ?
C3 K1 K4 127.78(4) . . ?
C3 K1 C1 24.85(6) . . ?
C17 K1 K2 60.29(4) . . ?
C17 K1 K3 103.01(4) . . ?
C17 K1 K4 51.87(4) . . ?
C17 K1 C1 112.56(6) . . ?
C17 K1 C3 127.08(6) . . ?
C31 K1 K2 144.43(4) 5_666 . ?
C31 K1 K3 146.58(4) 5_666 . ?
C31 K1 K4 105.42(4) 5_666 . ?
C31 K1 C1 151.53(6) 5_666 . ?
C31 K1 C3 126.78(6) 5_666 . ?
C31 K1 C17 84.88(6) 5_666 . ?
O1 K2 K3 44.80(5) . . ?
O1 K2 O2 88.06(6) . . ?
O1 K2 O4 87.94(6) . . ?
O1 K2 C1 19.09(6) . . ?
O1 K2 C49 101.37(7) . . ?
O1 K2 C50 97.27(7) . . ?
O1 K2 C65 105.77(9) . . ?
O1 K2 C66 130.26(9) . . ?
O1 K2 C67 143.62(9) . . ?
O1 K2 C69 106.08(9) . . ?
O1 K2 C70 95.06(9) . . ?
O2 K2 K3 92.01(4) . . ?
O2 K2 O4 85.07(6) . . ?
O2 K2 C1 103.03(6) . . ?
O2 K2 C49 106.44(6) . . ?
O2 K2 C50 130.90(6) . . ?
O2 K2 C65 111.34(7) . . ?
O2 K2 C66 104.07(7) . . ?
O2 K2 C67 117.47(9) . . ?
O2 K2 C69 151.66(8) . . ?
O2 K2 C70 134.40(8) . . ?
O4 K2 K3 43.98(4) . . ?
O4 K2 C1 100.86(6) . . ?
O4 K2 C49 25.04(6) . . ?
O4 K2 C50 46.71(7) . . ?
O4 K2 C65 158.52(8) . . ?
O4 K2 C66 140.28(9) . . ?
O4 K2 C67 117.90(9) . . ?
O4 K2 C69 119.16(8) . . ?
O4 K2 C70 140.42(8) . . ?
C1 K2 K3 57.02(4) . . ?
C1 K2 C67 124.58(9) . . ?
C1 K2 C69 87.46(9) . . ?
C49 K2 K3 57.53(5) . . ?
C49 K2 C1 107.74(7) . . ?
C49 K2 C50 24.63(6) . . ?
C49 K2 C65 133.60(8) . . ?
C49 K2 C66 119.88(9) . . ?
C49 K2 C67 95.80(10) . . ?
C49 K2 C69 94.91(8) . . ?
C49 K2 C70 117.33(9) . . ?
C50 K2 K3 61.69(6) . . ?
C50 K2 C1 95.90(7) . . ?
C50 K2 C67 85.29(10) . . ?
C50 K2 C69 72.61(8) . . ?
C50 K2 C70 93.89(9) . . ?
C65 K2 K3 143.12(8) . . ?
C65 K2 C1 89.15(9) . . ?
C65 K2 C50 113.84(8) . . ?
C65 K2 C66 24.84(10) . . ?
C65 K2 C67 42.75(10) . . ?
C65 K2 C69 41.67(9) . . ?
C65 K2 C70 24.79(9) . . ?
C66 K2 K3 163.39(7) . . ?
C66 K2 C1 113.99(9) . . ?
C66 K2 C50 108.72(9) . . ?
C66 K2 C67 24.29(10) . . ?
C66 K2 C69 48.11(9) . . ?
C66 K2 C70 43.03(10) . . ?
C67 K2 K3 146.02(8) . . ?
C67 K2 C69 40.09(11) . . ?
C69 K2 K3 115.43(7) . . ?
C70 K2 K3 121.40(8) . . ?
C70 K2 C1 76.14(9) . . ?
C70 K2 C67 48.60(11) . . ?
C70 K2 C69 23.06(9) . . ?
O1 K3 K2 41.58(5) . . ?
O1 K3 C1 19.88(6) . . ?
O1 K3 C49 91.27(6) . . ?
O1 K3 C71 107.56(8) . . ?
O1 K3 C72 129.98(10) . . ?
O1 K3 C73 141.11(9) . . ?
O1 K3 C74 123.15(12) . . ?
O1 K3 C75 101.61(10) . . ?
O1 K3 C76 95.45(8) . . ?
O3 K3 K2 85.85(4) . . ?
O3 K3 O1 81.63(6) . . ?
O3 K3 O4 82.80(6) . . ?
O3 K3 C1 96.75(6) . . ?
O3 K3 C49 103.58(6) . . ?
O3 K3 C71 124.99(9) . . ?
O3 K3 C72 119.54(10) . . ?
O3 K3 C73 131.60(12) . . ?
O3 K3 C74 154.48(13) . . ?
O3 K3 C75 164.73(10) . . ?
O3 K3 C76 143.12(9) . . ?
O4 K3 K2 43.70(4) . . ?
O4 K3 O1 84.50(6) . . ?
O4 K3 C1 99.15(6) . . ?
O4 K3 C49 21.12(6) . . ?
O4 K3 C71 150.39(8) . . ?
O4 K3 C72 138.68(10) . . ?
O4 K3 C73 115.11(10) . . ?
O4 K3 C74 103.93(9) . . ?
O4 K3 C75 112.27(9) . . ?
O4 K3 C76 133.77(9) . . ?
C1 K3 K2 55.57(5) . . ?
C1 K3 C71 88.31(8) . . ?
C1 K3 C75 83.64(10) . . ?
C1 K3 C76 75.61(8) . . ?
C49 K3 K2 50.50(4) . . ?
C49 K3 C1 100.20(6) . . ?
C49 K3 C71 129.41(8) . . ?
C49 K3 C72 121.61(10) . . ?
C49 K3 C74 83.47(9) . . ?
C49 K3 C75 91.33(9) . . ?
C49 K3 C76 113.26(9) . . ?
C71 K3 K2 136.79(8) . . ?
C72 K3 K2 153.80(8) . . ?
C72 K3 C1 110.82(9) . . ?
C72 K3 C71 22.51(10) . . ?
C72 K3 C75 47.31(12) . . ?
C72 K3 C76 39.42(10) . . ?
C73 K3 K2 138.95(12) . . ?
C73 K3 C1 121.62(9) . . ?
C73 K3 C49 97.73(11) . . ?
C73 K3 C71 40.37(10) . . ?
C73 K3 C72 23.94(12) . . ?
C73 K3 C74 23.59(12) . . ?
C73 K3 C75 40.77(13) . . ?
C73 K3 C76 46.35(10) . . ?
C74 K3 K2 116.23(11) . . ?
C74 K3 C1 106.20(12) . . ?
C74 K3 C71 46.70(10) . . ?
C74 K3 C72 41.44(12) . . ?
C74 K3 C75 22.92(12) . . ?
C74 K3 C76 39.62(11) . . ?
C75 K3 K2 106.59(9) . . ?
C75 K3 C71 39.75(11) . . ?
C75 K3 C76 22.50(10) . . ?
C76 K3 K2 116.06(8) . . ?
C76 K3 C71 22.01(9) . . ?
K2 K4 K1 59.602(14) . . ?
O2 K4 K1 45.03(4) . . ?
O2 K4 K2 41.12(4) . . ?
O2 K4 C17 23.10(5) . . ?
O2 K4 C33 104.74(6) . . ?
O2 K4 C34 108.83(6) . . ?
O2 K4 C79 141.96(8) . . ?
O2 K4 C80 124.10(7) . . ?
O2 K4 C81 121.08(7) . . ?
O2 K4 C82 134.19(9) . . ?
O3 K4 K1 42.92(4) . . ?
O3 K4 K2 83.79(4) . . ?
O3 K4 O2 87.14(5) . . ?
O3 K4 C17 100.39(6) . . ?
O3 K4 C33 22.89(6) . . ?
O3 K4 C34 43.74(6) . . ?
O3 K4 C79 129.91(8) . . ?
O3 K4 C80 147.66(7) . . ?
O3 K4 C81 134.96(8) . . ?
O3 K4 C82 112.54(8) . . ?
O4 K4 K1 87.56(4) . . ?
O4 K4 K2 42.48(5) . . ?
O4 K4 O2 83.59(6) . . ?
O4 K4 O3 83.25(6) . . ?
O4 K4 C17 103.83(6) . . ?
O4 K4 C33 99.64(7) . . ?
O4 K4 C34 122.44(7) . . ?
O4 K4 C79 91.75(7) . . ?
O4 K4 C80 106.34(7) . . ?
O4 K4 C81 130.23(7) . . ?
O4 K4 C82 137.34(9) . . ?
C17 K4 K1 58.06(4) . . ?
C17 K4 K2 62.13(4) . . ?
C17 K4 C33 111.51(6) . . ?
C17 K4 C34 105.97(6) . . ?
C17 K4 C79 128.93(7) . . ?
C17 K4 C80 106.81(7) . . ?
C17 K4 C81 98.88(7) . . ?
C17 K4 C82 111.19(9) . . ?
C33 K4 K1 59.90(4) . . ?
C33 K4 K2 106.67(5) . . ?
C33 K4 C34 23.16(6) . . ?
C33 K4 C79 113.25(8) . . ?
C33 K4 C80 126.19(8) . . ?
C33 K4 C81 112.22(8) . . ?
C33 K4 C82 89.68(9) . . ?
C34 K4 K1 69.11(5) . . ?
C34 K4 K2 125.24(5) . . ?
C34 K4 C79 105.45(8) . . ?
C34 K4 C82 70.31(9) . . ?
C79 K4 K1 172.82(7) . . ?
C79 K4 K2 123.60(7) . . ?
C79 K4 C82 47.13(10) . . ?
C80 K4 K1 162.21(6) . . ?
C80 K4 K2 124.37(6) . . ?
C80 K4 C34 110.35(8) . . ?
C80 K4 C79 23.28(8) . . ?
C80 K4 C81 23.96(8) . . ?
C80 K4 C82 40.80(9) . . ?
C81 K4 K1 141.31(6) . . ?
C81 K4 K2 140.90(7) . . ?
C81 K4 C34 91.79(8) . . ?
C81 K4 C79 41.22(8) . . ?
C81 K4 C82 22.71(9) . . ?
C82 K4 K1 131.57(8) . . ?
C82 K4 K2 163.60(8) . . ?
K1 O1 K3 97.61(6) . . ?
K2 O1 K1 96.74(7) . . ?
K2 O1 K3 93.62(6) . . ?
C1 O1 K1 125.04(16) . . ?
C1 O1 K2 121.53(18) . . ?
C1 O1 K3 115.66(16) . . ?
K2 O2 K1 93.13(5) . . ?
K2 O2 K4 95.00(6) . . ?
K4 O2 K1 91.24(5) . . ?
C17 O2 K1 114.75(14) . . ?
C17 O2 K2 145.76(15) . . ?
C17 O2 K4 103.41(13) . . ?
K1 O3 K4 93.65(5) . . ?
K3 O3 K1 98.38(6) . . ?
K3 O3 K4 95.46(6) . . ?
C33 O3 K1 127.99(16) . . ?
C33 O3 K3 126.94(15) . . ?
C33 O3 K4 104.49(15) . . ?
K2 O4 K3 92.32(6) . . ?
K4 O4 K2 96.33(7) . . ?
K4 O4 K3 98.03(7) . . ?
C49 O4 K2 97.27(15) . . ?
C49 O4 K3 112.55(16) . . ?
C49 O4 K4 145.82(16) . . ?
K2 C1 K1 67.49(5) . . ?
K2 C1 K3 67.41(5) . . ?
K3 C1 K1 69.71(5) . . ?
O1 C1 K1 37.45(12) . . ?
O1 C1 K2 39.38(14) . . ?
O1 C1 K3 44.46(12) . . ?
O1 C1 C2 125.8(3) . . ?
O1 C1 C3 114.5(2) . . ?
C2 C1 K1 163.3(2) . . ?
C2 C1 K2 98.1(2) . . ?
C2 C1 K3 97.33(18) . . ?
C2 C1 C3 119.6(2) . . ?
C3 C1 K1 77.10(12) . . ?
C3 C1 K2 132.64(15) . . ?
C3 C1 K3 127.76(16) . . ?
C1 C2 H2A 120.0 . . ?
C1 C2 H2B 120.0 . . ?
H2A C2 H2B 120.0 . . ?
C1 C3 K1 78.05(12) . . ?
C4 C3 K1 105.28(14) . . ?
C4 C3 C1 120.9(2) . . ?
C4 C3 C16 119.4(2) . . ?
C16 C3 K1 84.44(13) . . ?
C16 C3 C1 119.7(2) . . ?
C3 C4 C5 121.8(2) . . ?
C3 C4 C9 119.6(3) . . ?
C5 C4 C9 118.6(2) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 C4 121.5(3) . . ?
C6 C5 H5 119.2 . . ?
C5 C6 H6 120.6 . . ?
C5 C6 C7 118.9(3) . . ?
C7 C6 H6 120.6 . . ?
C6 C7 H7 119.3 . . ?
C8 C7 C6 121.4(3) . . ?
C8 C7 H7 119.3 . . ?
C7 C8 H8 119.1 . . ?
C7 C8 C9 121.8(3) . . ?
C9 C8 H8 119.1 . . ?
C8 C9 C4 117.8(3) . . ?
C10 C9 C4 119.2(2) . . ?
C10 C9 C8 123.0(3) . . ?
C9 C10 H10 118.7 . . ?
C11 C10 C9 122.5(3) . . ?
C11 C10 H10 118.7 . . ?
C10 C11 C12 122.7(3) . . ?
C10 C11 C16 119.0(3) . . ?
C16 C11 C12 118.2(3) . . ?
C11 C12 H12 119.3 . . ?
C13 C12 C11 121.4(3) . . ?
C13 C12 H12 119.3 . . ?
C12 C13 H13 120.2 . . ?
C12 C13 C14 119.7(3) . . ?
C14 C13 H13 120.2 . . ?
C13 C14 H14 119.4 . . ?
C15 C14 C13 121.2(3) . . ?
C15 C14 H14 119.4 . . ?
C14 C15 H15 119.1 . . ?
C14 C15 C16 121.8(3) . . ?
C16 C15 H15 119.1 . . ?
C3 C16 C11 120.2(2) . . ?
C3 C16 C15 122.2(2) . . ?
C15 C16 C11 117.6(3) . . ?
K4 C17 K1 70.07(5) . . ?
O2 C17 K1 45.40(11) . . ?
O2 C17 K4 53.49(11) . . ?
O2 C17 C18 125.6(2) . . ?
O2 C17 C19 115.99(19) . . ?
C18 C17 K1 86.11(16) . . ?
C18 C17 K4 92.82(17) . . ?
C18 C17 C19 118.4(2) . . ?
C19 C17 K1 146.10(13) . . ?
C19 C17 K4 126.53(14) . . ?
C17 C18 H18A 120.0 . . ?
C17 C18 H18B 120.0 . . ?
H18A C18 H18B 120.0 . . ?
C20 C19 C17 121.5(2) . . ?
C32 C19 C17 118.85(19) . . ?
C32 C19 C20 119.6(2) . . ?
C19 C20 C21 122.8(2) . . ?
C19 C20 C25 119.8(2) . . ?
C21 C20 C25 117.4(2) . . ?
C20 C21 H21 119.3 . . ?
C22 C21 C20 121.4(2) . . ?
C22 C21 H21 119.3 . . ?
C21 C22 H22 119.5 . . ?
C21 C22 C23 121.0(3) . . ?
C23 C22 H22 119.5 . . ?
C22 C23 H23 120.1 . . ?
C24 C23 C22 119.9(2) . . ?
C24 C23 H23 120.1 . . ?
C23 C24 H24 119.2 . . ?
C23 C24 C25 121.5(3) . . ?
C25 C24 H24 119.2 . . ?
C20 C25 C24 118.8(2) . . ?
C26 C25 C20 119.7(2) . . ?
C26 C25 C24 121.5(2) . . ?
C25 C26 H26 119.2 . . ?
C25 C26 C27 121.5(2) . . ?
C27 C26 H26 119.2 . . ?
C26 C27 C28 122.0(2) . . ?
C26 C27 C32 119.2(2) . . ?
C28 C27 C32 118.8(2) . . ?
C27 C28 H28 119.3 . . ?
C29 C28 C27 121.4(2) . . ?
C29 C28 H28 119.3 . . ?
C28 C29 H29 120.0 . . ?
C28 C29 C30 120.0(2) . . ?
C30 C29 H29 120.0 . . ?
C29 C30 H30 119.8 . . ?
C31 C30 C29 120.5(2) . . ?
C31 C30 H30 119.8 . . ?
K1 C31 H31 77.9 5_666 . ?
C30 C31 K1 98.92(15) . 5_666 ?
C30 C31 H31 119.2 . . ?
C30 C31 C32 121.5(2) . . ?
C32 C31 K1 92.87(12) . 5_666 ?
C32 C31 H31 119.2 . . ?
C19 C32 C27 120.2(2) . . ?
C19 C32 C31 122.1(2) . . ?
C31 C32 C27 117.6(2) . . ?
O3 C33 K4 52.62(12) . . ?
O3 C33 C34 125.9(2) . . ?
O3 C33 C35 114.9(2) . . ?
C34 C33 K4 84.56(17) . . ?
C34 C33 C35 119.2(2) . . ?
C35 C33 K4 138.70(16) . . ?
K4 C34 H34A 58.3 . . ?
K4 C34 H34B 146.1 . . ?
C33 C34 K4 72.28(16) . . ?
C33 C34 H34A 120.0 . . ?
C33 C34 H34B 120.0 . . ?
H34A C34 H34B 120.0 . . ?
C36 C35 C33 119.9(2) . . ?
C36 C35 C48 119.7(2) . . ?
C48 C35 C33 120.4(2) . . ?
C35 C36 C37 122.4(2) . . ?
C35 C36 C41 120.2(2) . . ?
C37 C36 C41 117.3(2) . . ?
C36 C37 H37 119.2 . . ?
C38 C37 C36 121.6(3) . . ?
C38 C37 H37 119.2 . . ?
C37 C38 H38 119.8 . . ?
C37 C38 C39 120.5(3) . . ?
C39 C38 H38 119.8 . . ?
C38 C39 H39 119.8 . . ?
C40 C39 C38 120.4(3) . . ?
C40 C39 H39 119.8 . . ?
C39 C40 H40 119.5 . . ?
C39 C40 C41 121.0(3) . . ?
C41 C40 H40 119.5 . . ?
C40 C41 C36 119.2(3) . . ?
C42 C41 C36 119.1(3) . . ?
C42 C41 C40 121.7(2) . . ?
C41 C42 H42 119.2 . . ?
C43 C42 C41 121.5(2) . . ?
C43 C42 H42 119.2 . . ?
C42 C43 C44 122.3(3) . . ?
C42 C43 C48 119.3(3) . . ?
C44 C43 C48 118.3(3) . . ?
C43 C44 H44 119.1 . . ?
C45 C44 C43 121.7(3) . . ?
C45 C44 H44 119.1 . . ?
C44 C45 H45 119.8 . . ?
C44 C45 C46 120.3(3) . . ?
C46 C45 H45 119.8 . . ?
C45 C46 H46 119.9 . . ?
C47 C46 C45 120.1(3) . . ?
C47 C46 H46 119.9 . . ?
C46 C47 H47 119.0 . . ?
C46 C47 C48 121.9(3) . . ?
C48 C47 H47 119.0 . . ?
C35 C48 C43 120.0(3) . . ?
C35 C48 C47 122.4(2) . . ?
C47 C48 C43 117.6(2) . . ?
K2 C49 K3 71.97(5) . . ?
O4 C49 K2 57.70(12) . . ?
O4 C49 K3 46.33(12) . . ?
O4 C49 C50 126.4(2) . . ?
O4 C49 C51 114.6(2) . . ?
C50 C49 K2 83.22(16) . . ?
C50 C49 K3 90.00(18) . . ?
C50 C49 C51 119.0(2) . . ?
C51 C49 K2 136.49(16) . . ?
C51 C49 K3 137.77(17) . . ?
K2 C50 H50A 62.0 . . ?
K2 C50 H50B 140.9 . . ?
C49 C50 K2 72.15(15) . . ?
C49 C50 H50A 120.0 . . ?
C49 C50 H50B 120.0 . . ?
H50A C50 H50B 120.0 . . ?
C52 C51 C49 120.2(2) . . ?
C64 C51 C49 119.7(2) . . ?
C64 C51 C52 120.1(2) . . ?
C51 C52 C53 122.3(2) . . ?
C51 C52 C57 119.7(2) . . ?
C53 C52 C57 118.0(2) . . ?
C52 C53 H53 119.5 . . ?
C54 C53 C52 121.1(2) . . ?
C54 C53 H53 119.5 . . ?
C53 C54 H54 119.5 . . ?
C53 C54 C55 121.0(2) . . ?
C55 C54 H54 119.5 . . ?
C54 C55 H55 120.0 . . ?
C56 C55 C54 120.1(3) . . ?
C56 C55 H55 120.0 . . ?
C55 C56 H56 119.3 . . ?
C55 C56 C57 121.5(3) . . ?
C57 C56 H56 119.3 . . ?
C56 C57 C52 118.4(2) . . ?
C58 C57 C52 119.3(2) . . ?
C58 C57 C56 122.3(2) . . ?
C57 C58 H58 119.1 . . ?
C59 C58 C57 121.7(2) . . ?
C59 C58 H58 119.1 . . ?
C58 C59 C60 122.1(2) . . ?
C58 C59 C64 119.2(2) . . ?
C60 C59 C64 118.6(2) . . ?
C59 C60 H60 119.2 . . ?
C61 C60 C59 121.6(2) . . ?
C61 C60 H60 119.2 . . ?
C60 C61 H61 119.9 . . ?
C60 C61 C62 120.2(2) . . ?
C62 C61 H61 119.9 . . ?
C61 C62 H62 119.9 . . ?
C63 C62 C61 120.2(2) . . ?
C63 C62 H62 119.9 . . ?
C62 C63 H63 119.2 . . ?
C62 C63 C64 121.7(2) . . ?
C64 C63 H63 119.2 . . ?
C51 C64 C59 119.8(2) . . ?
C51 C64 C63 122.5(2) . . ?
C63 C64 C59 117.7(2) . . ?
K2 C65 H65 106.4 . . ?
C66 C65 K2 81.0(2) . . ?
C66 C65 H65 120.1 . . ?
C66 C65 C70 119.8(3) . . ?
C70 C65 K2 82.7(2) . . ?
C70 C65 H65 120.1 . . ?
K2 C66 H66 108.8 . . ?
C65 C66 K2 74.2(2) . . ?
C65 C66 H66 119.9 . . ?
C65 C66 C67 120.2(4) . . ?
C67 C66 K2 87.2(3) . . ?
C67 C66 H66 119.9 . . ?
K2 C67 H67 117.3 . . ?
C66 C67 K2 68.5(2) . . ?
C66 C67 H67 120.9 . . ?
C68 C67 K2 84.0(3) . . ?
C68 C67 C66 118.2(4) . . ?
C68 C67 H67 120.9 . . ?
C67 C68 H68 119.7 . . ?
C69 C68 C67 120.6(4) . . ?
C69 C68 H68 119.7 . . ?
K2 C69 H69 119.1 . . ?
C68 C69 K2 82.9(2) . . ?
C68 C69 H69 119.5 . . ?
C68 C69 C70 121.1(4) . . ?
C70 C69 K2 69.2(2) . . ?
C70 C69 H69 119.5 . . ?
K2 C70 H70 109.9 . . ?
C65 C70 K2 72.50(18) . . ?
C65 C70 H70 120.0 . . ?
C69 C70 K2 87.8(2) . . ?
C69 C70 C65 120.1(4) . . ?
C69 C70 H70 120.0 . . ?
K3 C71 H71 115.6 . . ?
C72 C71 K3 76.7(2) . . ?
C72 C71 H71 119.5 . . ?
C76 C71 K3 78.7(2) . . ?
C76 C71 H71 119.5 . . ?
C76 C71 C72 120.9(4) . . ?
K3 C72 H72 113.8 . . ?
C71 C72 K3 80.8(2) . . ?
C71 C72 H72 121.1 . . ?
C71 C72 C73 117.8(5) . . ?
C73 C72 K3 75.1(2) . . ?
C73 C72 H72 121.1 . . ?
K3 C73 H73 110.3 . . ?
C72 C73 K3 81.0(2) . . ?
C72 C73 H73 120.2 . . ?
C74 C73 K3 78.9(2) . . ?
C74 C73 C72 119.7(4) . . ?
C74 C73 H73 120.2 . . ?
K3 C74 H74 111.1 . . ?
C73 C74 K3 77.5(2) . . ?
C73 C74 H74 119.8 . . ?
C75 C74 K3 81.9(3) . . ?
C75 C74 C73 120.5(5) . . ?
C75 C74 H74 119.8 . . ?
K3 C75 H75 115.1 . . ?
C74 C75 K3 75.2(3) . . ?
C74 C75 H75 121.0 . . ?
C76 C75 K3 79.5(2) . . ?
C76 C75 C74 117.9(5) . . ?
C76 C75 H75 121.0 . . ?
K3 C76 H76 114.5 . . ?
C71 C76 K3 79.3(2) . . ?
C71 C76 C75 123.3(4) . . ?
C71 C76 H76 118.4 . . ?
C75 C76 K3 78.0(2) . . ?
C75 C76 H76 118.4 . . ?
C78 C77 H77 120.1 . . ?
C78 C77 C83 118.1(8) . . ?
C82 C77 H77 120.1 . . ?
C82 C77 C78 119.7(4) . . ?
C82 C77 C83 120.7(8) . . ?
C77 C78 H78 119.7 . . ?
C79 C78 C77 120.7(4) . . ?
C79 C78 H78 119.7 . . ?
K4 C79 H79 111.3 . . ?
C78 C79 K4 85.4(2) . . ?
C78 C79 H79 120.2 . . ?
C78 C79 C80 119.6(4) . . ?
C80 C79 K4 73.41(17) . . ?
C80 C79 H79 120.2 . . ?
K4 C80 H80 107.0 . . ?
C79 C80 K4 83.31(18) . . ?
C79 C80 H80 119.6 . . ?
C79 C80 C81 120.8(3) . . ?
C81 C80 K4 80.07(17) . . ?
C81 C80 H80 119.6 . . ?
K4 C81 H81 109.5 . . ?
C80 C81 K4 75.97(16) . . ?
C80 C81 H81 119.7 . . ?
C82 C81 K4 84.9(2) . . ?
C82 C81 C80 120.6(3) . . ?
C82 C81 H81 119.7 . . ?
K4 C82 H82 113.9 . . ?
C77 C82 K4 83.6(3) . . ?
C77 C82 H82 120.7 . . ?
C81 C82 K4 72.37(19) . . ?
C81 C82 C77 118.7(4) . . ?
C81 C82 H82 120.7 . . ?
C77 C83 H83A 109.5 . . ?
C77 C83 H83B 109.5 . . ?
C77 C83 H83C 109.5 . . ?
H83A C83 H83B 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 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
K1 O1 C1 K2 126.8(3) . . . . ?
K1 O1 C1 K3 -121.1(2) . . . . ?
K1 O1 C1 C2 179.6(2) . . . . ?
K1 O1 C1 C3 -1.4(3) . . . . ?
K1 O2 C17 K4 97.72(11) . . . . ?
K1 O2 C17 C18 34.7(3) . . . . ?
K1 O2 C17 C19 -144.69(15) . . . . ?
K1 O3 C33 K4 -106.58(17) . . . . ?
K1 O3 C33 C34 -61.0(3) . . . . ?
K1 O3 C33 C35 120.00(19) . . . . ?
K1 C1 C3 C4 100.80(19) . . . . ?
K1 C1 C3 C16 -76.43(19) . . . . ?
K1 C3 C4 C5 84.2(2) . . . . ?
K1 C3 C4 C9 -94.8(2) . . . . ?
K1 C3 C16 C11 106.4(2) . . . . ?
K1 C3 C16 C15 -73.6(2) . . . . ?
K1 C17 C19 C20 -155.83(19) . . . . ?
K1 C17 C19 C32 22.9(4) . . . . ?
K1 C31 C32 C19 76.85(19) 5_666 . . . ?
K1 C31 C32 C27 -102.34(17) 5_666 . . . ?
K2 O1 C1 K1 -126.8(3) . . . . ?
K2 O1 C1 K3 112.15(18) . . . . ?
K2 O1 C1 C2 52.9(4) . . . . ?
K2 O1 C1 C3 -128.13(19) . . . . ?
K2 O2 C17 K1 141.6(3) . . . . ?
K2 O2 C17 K4 -120.6(3) . . . . ?
K2 O2 C17 C18 176.4(2) . . . . ?
K2 O2 C17 C19 -3.0(4) . . . . ?
K2 O4 C49 K3 -95.58(11) . . . . ?
K2 O4 C49 C50 -50.3(3) . . . . ?
K2 O4 C49 C51 130.87(18) . . . . ?
K2 C1 C3 K1 -41.87(17) . . . . ?
K2 C1 C3 C4 58.9(3) . . . . ?
K2 C1 C3 C16 -118.3(2) . . . . ?
K2 C49 C51 C52 -10.1(4) . . . . ?
K2 C49 C51 C64 167.92(18) . . . . ?
K2 C65 C66 C67 77.1(3) . . . . ?
K2 C65 C70 C69 -76.7(3) . . . . ?
K2 C66 C67 C68 70.2(4) . . . . ?
K2 C67 C68 C69 60.7(4) . . . . ?
K2 C69 C70 C65 68.3(3) . . . . ?
K3 O1 C1 K1 121.1(2) . . . . ?
K3 O1 C1 K2 -112.15(18) . . . . ?
K3 O1 C1 C2 -59.3(4) . . . . ?
K3 O1 C1 C3 119.72(19) . . . . ?
K3 O3 C33 K4 108.49(18) . . . . ?
K3 O3 C33 C34 154.1(2) . . . . ?
K3 O3 C33 C35 -24.9(3) . . . . ?
K3 O4 C49 K2 95.58(11) . . . . ?
K3 O4 C49 C50 45.3(3) . . . . ?
K3 O4 C49 C51 -133.55(17) . . . . ?
K3 C1 C3 K1 51.15(14) . . . . ?
K3 C1 C3 C4 151.95(17) . . . . ?
K3 C1 C3 C16 -25.3(3) . . . . ?
K3 C49 C50 K2 71.83(5) . . . . ?
K3 C49 C51 C52 -129.6(2) . . . . ?
K3 C49 C51 C64 48.5(3) . . . . ?
K3 C71 C72 C73 -67.7(3) . . . . ?
K3 C71 C76 C75 67.8(4) . . . . ?
K3 C72 C73 C74 -71.7(3) . . . . ?
K3 C73 C74 C75 -72.6(4) . . . . ?
K3 C74 C75 C76 -69.3(4) . . . . ?
K3 C75 C76 C71 -68.5(4) . . . . ?
K4 O2 C17 K1 -97.72(11) . . . . ?
K4 O2 C17 C18 -63.0(3) . . . . ?
K4 O2 C17 C19 117.59(16) . . . . ?
K4 O3 C33 C34 45.6(3) . . . . ?
K4 O3 C33 C35 -133.43(18) . . . . ?
K4 O4 C49 K2 -112.7(3) . . . . ?
K4 O4 C49 K3 151.7(4) . . . . ?
K4 O4 C49 C50 -162.9(2) . . . . ?
K4 O4 C49 C51 18.2(4) . . . . ?
K4 C17 C19 C20 -45.8(3) . . . . ?
K4 C17 C19 C32 132.85(16) . . . . ?
K4 C33 C35 C36 -155.88(18) . . . . ?
K4 C33 C35 C48 22.0(4) . . . . ?
K4 C79 C80 C81 74.2(3) . . . . ?
K4 C80 C81 C82 75.3(3) . . . . ?
K4 C81 C82 C77 72.1(4) . . . . ?
O1 C1 C3 K1 0.9(2) . . . . ?
O1 C1 C3 C4 101.7(3) . . . . ?
O1 C1 C3 C16 -75.6(3) . . . . ?
O2 C17 C19 C20 -108.3(2) . . . . ?
O2 C17 C19 C32 70.4(3) . . . . ?
O3 C33 C34 K4 -34.7(2) . . . . ?
O3 C33 C35 C36 -94.9(3) . . . . ?
O3 C33 C35 C48 83.0(3) . . . . ?
O4 C49 C50 K2 40.9(2) . . . . ?
O4 C49 C51 C52 -78.3(3) . . . . ?
O4 C49 C51 C64 99.7(3) . . . . ?
C1 C3 C4 C5 -0.9(3) . . . . ?
C1 C3 C4 C9 -179.9(2) . . . . ?
C1 C3 C16 C11 179.3(2) . . . . ?
C1 C3 C16 C15 -0.8(3) . . . . ?
C2 C1 C3 K1 179.9(3) . . . . ?
C2 C1 C3 C4 -79.3(3) . . . . ?
C2 C1 C3 C16 103.5(3) . . . . ?
C3 C4 C5 C6 -179.9(2) . . . . ?
C3 C4 C9 C8 -179.5(2) . . . . ?
C3 C4 C9 C10 0.8(3) . . . . ?
C4 C3 C16 C11 2.0(3) . . . . ?
C4 C3 C16 C15 -178.0(2) . . . . ?
C4 C5 C6 C7 -0.1(4) . . . . ?
C4 C9 C10 C11 1.7(4) . . . . ?
C5 C4 C9 C8 1.5(3) . . . . ?
C5 C4 C9 C10 -178.2(2) . . . . ?
C5 C6 C7 C8 0.6(4) . . . . ?
C6 C7 C8 C9 -0.1(4) . . . . ?
C7 C8 C9 C4 -1.0(4) . . . . ?
C7 C8 C9 C10 178.7(3) . . . . ?
C8 C9 C10 C11 -177.9(2) . . . . ?
C9 C4 C5 C6 -1.0(4) . . . . ?
C9 C10 C11 C12 177.2(3) . . . . ?
C9 C10 C11 C16 -2.4(4) . . . . ?
C10 C11 C12 C13 -179.8(3) . . . . ?
C10 C11 C16 C3 0.5(3) . . . . ?
C10 C11 C16 C15 -179.5(2) . . . . ?
C11 C12 C13 C14 0.2(5) . . . . ?
C12 C11 C16 C3 -179.1(2) . . . . ?
C12 C11 C16 C15 0.9(3) . . . . ?
C12 C13 C14 C15 -1.0(5) . . . . ?
C13 C14 C15 C16 1.8(4) . . . . ?
C14 C15 C16 C3 178.3(2) . . . . ?
C14 C15 C16 C11 -1.7(4) . . . . ?
C16 C3 C4 C5 176.4(2) . . . . ?
C16 C3 C4 C9 -2.6(3) . . . . ?
C16 C11 C12 C13 -0.2(4) . . . . ?
C17 C19 C20 C21 0.0(3) . . . . ?
C17 C19 C20 C25 179.6(2) . . . . ?
C17 C19 C32 C27 -179.11(19) . . . . ?
C17 C19 C32 C31 1.7(3) . . . . ?
C18 C17 C19 C20 72.3(3) . . . . ?
C18 C17 C19 C32 -109.0(2) . . . . ?
C19 C20 C21 C22 -179.1(2) . . . . ?
C19 C20 C25 C24 178.8(2) . . . . ?
C19 C20 C25 C26 -0.8(3) . . . . ?
C20 C19 C32 C27 -0.4(3) . . . . ?
C20 C19 C32 C31 -179.57(19) . . . . ?
C20 C21 C22 C23 0.0(4) . . . . ?
C20 C25 C26 C27 0.2(4) . . . . ?
C21 C20 C25 C24 -1.6(3) . . . . ?
C21 C20 C25 C26 178.8(2) . . . . ?
C21 C22 C23 C24 -1.1(4) . . . . ?
C22 C23 C24 C25 0.7(4) . . . . ?
C23 C24 C25 C20 0.7(4) . . . . ?
C23 C24 C25 C26 -179.8(3) . . . . ?
C24 C25 C26 C27 -179.4(2) . . . . ?
C25 C20 C21 C22 1.3(3) . . . . ?
C25 C26 C27 C28 -179.3(2) . . . . ?
C25 C26 C27 C32 0.3(4) . . . . ?
C26 C27 C28 C29 -178.6(2) . . . . ?
C26 C27 C32 C19 -0.2(3) . . . . ?
C26 C27 C32 C31 179.0(2) . . . . ?
C27 C28 C29 C30 -0.7(4) . . . . ?
C28 C27 C32 C19 179.4(2) . . . . ?
C28 C27 C32 C31 -1.4(3) . . . . ?
C28 C29 C30 C31 -0.8(4) . . . . ?
C29 C30 C31 K1 100.1(2) . . . 5_666 ?
C29 C30 C31 C32 1.1(4) . . . . ?
C30 C31 C32 C19 179.1(2) . . . . ?
C30 C31 C32 C27 0.0(3) . . . . ?
C32 C19 C20 C21 -178.7(2) . . . . ?
C32 C19 C20 C25 0.9(3) . . . . ?
C32 C27 C28 C29 1.7(4) . . . . ?
C33 C35 C36 C37 -2.5(3) . . . . ?
C33 C35 C36 C41 177.2(2) . . . . ?
C33 C35 C48 C43 179.6(2) . . . . ?
C33 C35 C48 C47 -0.8(4) . . . . ?
C34 C33 C35 C36 86.0(3) . . . . ?
C34 C33 C35 C48 -96.1(3) . . . . ?
C35 C33 C34 K4 144.2(2) . . . . ?
C35 C36 C37 C38 179.5(2) . . . . ?
C35 C36 C41 C40 -178.1(2) . . . . ?
C35 C36 C41 C42 3.0(3) . . . . ?
C36 C35 C48 C43 -2.6(4) . . . . ?
C36 C35 C48 C47 177.1(2) . . . . ?
C36 C37 C38 C39 -1.3(4) . . . . ?
C36 C41 C42 C43 -2.1(4) . . . . ?
C37 C36 C41 C40 1.7(3) . . . . ?
C37 C36 C41 C42 -177.2(2) . . . . ?
C37 C38 C39 C40 1.5(4) . . . . ?
C38 C39 C40 C41 0.0(4) . . . . ?
C39 C40 C41 C36 -1.6(4) . . . . ?
C39 C40 C41 C42 177.3(3) . . . . ?
C40 C41 C42 C43 179.0(3) . . . . ?
C41 C36 C37 C38 -0.3(3) . . . . ?
C41 C42 C43 C44 -179.5(3) . . . . ?
C41 C42 C43 C48 -1.0(4) . . . . ?
C42 C43 C44 C45 176.8(4) . . . . ?
C42 C43 C48 C35 3.4(4) . . . . ?
C42 C43 C48 C47 -176.2(3) . . . . ?
C43 C44 C45 C46 -0.2(6) . . . . ?
C44 C43 C48 C35 -178.0(3) . . . . ?
C44 C43 C48 C47 2.3(4) . . . . ?
C44 C45 C46 C47 1.6(6) . . . . ?
C45 C46 C47 C48 -0.9(5) . . . . ?
C46 C47 C48 C35 179.3(3) . . . . ?
C46 C47 C48 C43 -1.0(4) . . . . ?
C48 C35 C36 C37 179.6(2) . . . . ?
C48 C35 C36 C41 -0.6(3) . . . . ?
C48 C43 C44 C45 -1.8(5) . . . . ?
C49 C51 C52 C53 0.6(4) . . . . ?
C49 C51 C52 C57 -179.7(2) . . . . ?
C49 C51 C64 C59 179.9(2) . . . . ?
C49 C51 C64 C63 -1.5(3) . . . . ?
C50 C49 C51 C52 102.7(3) . . . . ?
C50 C49 C51 C64 -79.2(3) . . . . ?
C51 C49 C50 K2 -140.3(2) . . . . ?
C51 C52 C53 C54 178.9(2) . . . . ?
C51 C52 C57 C56 -179.9(2) . . . . ?
C51 C52 C57 C58 -0.4(4) . . . . ?
C52 C51 C64 C59 -2.0(3) . . . . ?
C52 C51 C64 C63 176.6(2) . . . . ?
C52 C53 C54 C55 0.9(4) . . . . ?
C52 C57 C58 C59 -1.6(4) . . . . ?
C53 C52 C57 C56 -0.2(4) . . . . ?
C53 C52 C57 C58 179.2(2) . . . . ?
C53 C54 C55 C56 0.0(5) . . . . ?
C54 C55 C56 C57 -1.0(5) . . . . ?
C55 C56 C57 C52 1.1(4) . . . . ?
C55 C56 C57 C58 -178.3(3) . . . . ?
C56 C57 C58 C59 177.9(3) . . . . ?
C57 C52 C53 C54 -0.7(4) . . . . ?
C57 C58 C59 C60 -177.4(3) . . . . ?
C57 C58 C59 C64 1.8(4) . . . . ?
C58 C59 C60 C61 178.7(3) . . . . ?
C58 C59 C64 C51 0.0(4) . . . . ?
C58 C59 C64 C63 -178.6(2) . . . . ?
C59 C60 C61 C62 -0.3(4) . . . . ?
C60 C59 C64 C51 179.3(2) . . . . ?
C60 C59 C64 C63 0.7(4) . . . . ?
C60 C61 C62 C63 1.0(4) . . . . ?
C61 C62 C63 C64 -0.8(4) . . . . ?
C62 C63 C64 C51 -178.6(2) . . . . ?
C62 C63 C64 C59 0.0(4) . . . . ?
C64 C51 C52 C53 -177.4(2) . . . . ?
C64 C51 C52 C57 2.2(3) . . . . ?
C64 C59 C60 C61 -0.5(4) . . . . ?
C65 C66 C67 K2 -69.9(3) . . . . ?
C65 C66 C67 C68 0.3(6) . . . . ?
C66 C65 C70 K2 75.2(3) . . . . ?
C66 C65 C70 C69 -1.5(5) . . . . ?
C66 C67 C68 C69 -1.0(7) . . . . ?
C67 C68 C69 K2 -60.0(4) . . . . ?
C67 C68 C69 C70 0.5(7) . . . . ?
C68 C69 C70 K2 -67.4(4) . . . . ?
C68 C69 C70 C65 0.8(6) . . . . ?
C70 C65 C66 K2 -76.2(3) . . . . ?
C70 C65 C66 C67 0.9(5) . . . . ?
C71 C72 C73 K3 70.9(3) . . . . ?
C71 C72 C73 C74 -0.8(6) . . . . ?
C72 C71 C76 K3 -66.8(3) . . . . ?
C72 C71 C76 C75 1.0(6) . . . . ?
C72 C73 C74 K3 72.8(3) . . . . ?
C72 C73 C74 C75 0.2(6) . . . . ?
C73 C74 C75 K3 70.2(4) . . . . ?
C73 C74 C75 C76 0.9(6) . . . . ?
C74 C75 C76 K3 66.9(4) . . . . ?
C74 C75 C76 C71 -1.5(6) . . . . ?
C76 C71 C72 K3 67.9(3) . . . . ?
C76 C71 C72 C73 0.2(6) . . . . ?
C77 C78 C79 K4 -67.6(4) . . . . ?
C77 C78 C79 C80 0.4(6) . . . . ?
C78 C77 C82 K4 64.2(4) . . . . ?
C78 C77 C82 C81 -1.7(7) . . . . ?
C78 C79 C80 K4 -74.6(3) . . . . ?
C78 C79 C80 C81 -0.4(5) . . . . ?
C79 C80 C81 K4 -76.0(3) . . . . ?
C79 C80 C81 C82 -0.7(5) . . . . ?
C80 C81 C82 K4 -70.4(3) . . . . ?
C80 C81 C82 C77 1.7(6) . . . . ?
C82 C77 C78 C79 0.7(7) . . . . ?
C83 C77 C78 C79 -165.6(7) . . . . ?
C83 C77 C82 K4 -129.9(8) . . . . ?
C83 C77 C82 C81 164.2(8) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 408.5 94.6 '2 Benzene/Toluene'
2 0.000 0.500 0.500 408.5 94.6 '2 Benzene/Toluene'
3 0.500 0.500 0.000 408.5 94.6 '2 Benzene/Toluene'
4 0.500 1.000 0.500 408.5 94.6 '2 Benzene/Toluene'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_SHELXL_version_number     2019/1
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.272
_oxdiff_exptl_absorpt_empirical_full_min 0.710
