# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1820791'
_audit_update_record             
;
2018-01-30 deposited with the CCDC.
2018-05-25 downloaded from the CCDC.
;

_audit_creation_date             2018-01-23
_audit_block_code                Wombacher_8851_THF_100_K

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 -1.00 -1.00 0.0350
0.00 1.00 1.00 0.0350
1.00 1.00 0.00 0.0800
-1.00 -1.00 0.00 0.0800
-1.00 2.00 -2.00 0.1000
-1.00 0.00 -1.00 0.0900
1.00 -2.00 2.00 0.0900
1.00 0.00 1.00 0.1000

_diffrn_radiation_monochromator  'MONTEL graded multilayer optic'

_exptl_special_details           
;
 Crystal mounted on a MiTeGen loop using Perfluoropolyether PFO-XR75
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        
;
(5,6:11,12-di-o-phenylenetetracene)-potassium-di(benzo-15-crown-5)
;

_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H40 K O10, C30 H16'
_chemical_formula_sum            'C58 H56 K O10'
_chemical_formula_weight         952.12

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'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.0923(3)
_cell_length_b                   13.0606(3)
_cell_length_c                   16.7307(4)
_cell_angle_alpha                82.9084(10)
_cell_angle_beta                 80.2410(9)
_cell_angle_gamma                76.9312(10)
_cell_volume                     2317.70(10)
_cell_formula_units_Z            2


_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9949
_cell_measurement_theta_min      2.6904
_cell_measurement_theta_max      66.8199

_exptl_crystal_description       prism
_exptl_crystal_colour            dark-green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_F_000             1006
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    1.527
_shelx_estimated_absorpt_T_min   0.716
_shelx_estimated_absorpt_T_max   0.901

_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.77995
_exptl_absorpt_correction_T_max  0.91280
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2012)'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           Cu-K\a
_diffrn_source                   '0.2 x 2mm^2^ focus rotating anode'
_diffrn_measurement_device_type  'Bruker AXS X8 Proteum'
_diffrn_measurement_method       'CCD φ- and ω-scans'
_diffrn_detector_area_resol_mean 66.67
_diffrn_reflns_number            55453
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.690
_diffrn_reflns_theta_max         67.489
_diffrn_reflns_theta_full        67.489
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measured_fraction_theta_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_point_group_measured_fraction_full 0.963
_reflns_number_total             8049
_reflns_number_gt                7238
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX2 (Bruker AXS, 2005-2013)'
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS (G. M. Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL (G. M. Sheldrick, 2018)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 1997-2012)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

 The minimum and maximum estimated transmissions from the multi-scan
 scaling are 0.7721 and 0.9315 (SADABS).

INTENSITY STATISTICS FOR DATASET 

 Resolution  #Data #Theory %Complete Redundancy Mean I Mean I/s Rmerge  Rsigma

 Inf - 3.45     121    121    100.0     4.03      36.9   47.00  0.0232  0.0179
3.45 - 2.28     283    283    100.0     6.99      14.9   60.82  0.0286  0.0143
2.28 - 1.81     417    417    100.0     8.31       9.5   58.28  0.0274  0.0123
1.81 - 1.58     406    406    100.0     7.38       6.2   46.97  0.0252  0.0145
1.58 - 1.44     390    390    100.0     6.81       4.7   39.58  0.0286  0.0169
1.44 - 1.34     399    399    100.0    11.09       2.9   42.17  0.0422  0.0171
1.34 - 1.26     404    404    100.0    11.07       3.5   41.60  0.0394  0.0169
1.26 - 1.19     450    453     99.3    10.52       3.8   40.35  0.0394  0.0169
1.19 - 1.14     398    402     99.0     8.97       4.4   37.36  0.0345  0.0177
1.14 - 1.10     363    369     98.4     8.15       3.9   33.93  0.0317  0.0201
1.10 - 1.06     440    444     99.1     7.94       2.6   29.41  0.0419  0.0238
1.06 - 1.02     469    482     97.3     7.50       2.1   27.10  0.0495  0.0273
1.02 - 0.99     422    431     97.9     7.25       1.7   23.29  0.0568  0.0303
0.99 - 0.97     316    326     96.9     6.92       1.6   23.01  0.0620  0.0313
0.97 - 0.94     491    512     95.9     5.93       1.4   19.31  0.0677  0.0370
0.94 - 0.92     372    389     95.6     3.97       1.4   16.05  0.0627  0.0457
0.92 - 0.90     421    438     96.1     3.94       1.5   16.36  0.0569  0.0416
0.90 - 0.88     418    444     94.1     3.52       1.5   16.25  0.0638  0.0444
0.88 - 0.86     481    512     93.9     3.25       1.2   14.94  0.0729  0.0491
0.86 - 0.85     257    282     91.1     2.89       1.0   12.83  0.0820  0.0556
0.85 - 0.83     331    458     72.3     1.60       0.8    9.34  0.0755  0.0758
#------------------------------------------------------------------------------
0.93 - 0.83    2106   2341     90.0     3.12       1.3   14.53  0.0654  0.0489
 Inf - 0.83    8049   8362     96.3     6.63       3.9   30.58  0.0356  0.0206
#-------------------------------------------------------------------------------

One of the independent 5,6:11,12-di-o-phenylenetetracene anion radicals is
partially rotationally disordered (11.5(7)%). This was manifest as disorder 
of C29 over two positions, C29A and C29B. C29A and C29B were refined with 
isotropic atomic displacement parameters. 


 Highest peak    0.18  at  0.9285  0.9482  0.0184  [  0.68 A from C29A ]
 Deepest hole   -0.26  at  0.3145  0.6415  0.2313  [  0.60 A from K1 ]
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0354P)²+1.3233P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8049
_refine_ls_number_parameters     622
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0319
_refine_ls_wR_factor_ref         0.0788
_refine_ls_wR_factor_gt          0.0754
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_restrained_S_all      0.969
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.40041(13) 0.85387(13) 0.04211(9) 0.0261(3) Uani 1 1 d . . . . .
H1A H 0.476820 0.834193 0.068524 0.031 Uiso 1 1 calc R U . . .
H1B H 0.401165 0.921835 0.008678 0.031 Uiso 1 1 calc R U . . .
C2 C 0.39583(15) 0.77008(13) -0.00987(9) 0.0286(3) Uani 1 1 d . . . . .
H2A H 0.317998 0.789367 -0.034777 0.034 Uiso 1 1 calc R U . . .
H2B H 0.467899 0.763383 -0.054200 0.034 Uiso 1 1 calc R U . . .
C3 C 0.35915(14) 0.59541(13) 0.00220(9) 0.0281(3) Uani 1 1 d . . . . .
H3A H 0.390977 0.524416 0.028363 0.034 Uiso 1 1 calc R U . . .
H3B H 0.395772 0.596757 -0.056061 0.034 Uiso 1 1 calc R U . . .
C4 C 0.21871(14) 0.61368(13) 0.00889(9) 0.0266(3) Uani 1 1 d . . . . .
H4A H 0.184526 0.686589 -0.012787 0.032 Uiso 1 1 calc R U . . .
H4B H 0.195506 0.564031 -0.023063 0.032 Uiso 1 1 calc R U . . .
C5 C 0.03541(13) 0.62189(12) 0.10469(9) 0.0255(3) Uani 1 1 d . . . . .
H5A H 0.003574 0.574915 0.075026 0.031 Uiso 1 1 calc R U . . .
H5B H 0.004579 0.695783 0.083634 0.031 Uiso 1 1 calc R U . . .
C6 C -0.01043(14) 0.60690(12) 0.19460(9) 0.0243(3) Uani 1 1 d . . . . .
H6A H -0.101870 0.611171 0.202527 0.029 Uiso 1 1 calc R U . . .
H6B H 0.029410 0.535297 0.215808 0.029 Uiso 1 1 calc R U . . .
C7 C -0.06927(13) 0.78261(11) 0.23342(9) 0.0231(3) Uani 1 1 d . . . . .
H7A H -0.151290 0.779150 0.266676 0.028 Uiso 1 1 calc R U . . .
H7B H -0.082264 0.801579 0.175905 0.028 Uiso 1 1 calc R U . . .
C8 C -0.01485(13) 0.86410(12) 0.26184(9) 0.0230(3) Uani 1 1 d . . . . .
H8A H -0.072269 0.934064 0.258492 0.028 Uiso 1 1 calc R U . . .
H8B H 0.000735 0.844979 0.318870 0.028 Uiso 1 1 calc R U . . .
C9 C 0.16011(13) 0.94566(11) 0.21032(9) 0.0224(3) Uani 1 1 d . . . . .
C10 C 0.12563(15) 1.02280(12) 0.26416(10) 0.0285(3) Uani 1 1 d . . . . .
H10 H 0.053374 1.024146 0.304007 0.034 Uiso 1 1 calc R U . . .
C11 C 0.19754(16) 1.09872(13) 0.25970(11) 0.0346(4) Uani 1 1 d . . . . .
H11 H 0.174011 1.152136 0.296466 0.042 Uiso 1 1 calc R U . . .
C12 C 0.30221(16) 1.09651(13) 0.20234(11) 0.0351(4) Uani 1 1 d . . . . .
H12 H 0.350853 1.148386 0.199802 0.042 Uiso 1 1 calc R U . . .
C13 C 0.33772(15) 1.01904(12) 0.14789(10) 0.0291(4) Uani 1 1 d . . . . .
H13 H 0.410366 1.017979 0.108415 0.035 Uiso 1 1 calc R U . . .
C14 C 0.26708(13) 0.94377(11) 0.15142(9) 0.0222(3) Uani 1 1 d . . . . .
C15 C 0.14492(13) 0.53519(12) 0.40127(9) 0.0234(3) Uani 1 1 d . . . . .
H15A H 0.064826 0.560639 0.379408 0.028 Uiso 1 1 calc R U . . .
H15B H 0.126621 0.521844 0.461179 0.028 Uiso 1 1 calc R U . . .
C16 C 0.21710(15) 0.43684(12) 0.36438(9) 0.0251(3) Uani 1 1 d . . . . .
H16A H 0.299068 0.414197 0.384168 0.030 Uiso 1 1 calc R U . . .
H16B H 0.170494 0.379402 0.380209 0.030 Uiso 1 1 calc R U . . .
C17 C 0.32868(15) 0.37919(12) 0.23815(10) 0.0284(3) Uani 1 1 d . . . . .
H17A H 0.317705 0.384009 0.180206 0.034 Uiso 1 1 calc R U . . .
H17B H 0.316499 0.308848 0.263234 0.034 Uiso 1 1 calc R U . . .
C18 C 0.46035(15) 0.38834(12) 0.24273(10) 0.0273(3) Uani 1 1 d . . . . .
H18A H 0.471932 0.386639 0.300302 0.033 Uiso 1 1 calc R U . . .
H18B H 0.520886 0.328385 0.218245 0.033 Uiso 1 1 calc R U . . .
C19 C 0.60011(13) 0.50387(12) 0.20904(9) 0.0256(3) Uani 1 1 d . . . . .
H19A H 0.667955 0.446068 0.187901 0.031 Uiso 1 1 calc R U . . .
H19B H 0.604328 0.506514 0.267366 0.031 Uiso 1 1 calc R U . . .
C20 C 0.61569(13) 0.60741(12) 0.16234(9) 0.0252(3) Uani 1 1 d . . . . .
H20A H 0.702958 0.615005 0.160461 0.030 Uiso 1 1 calc R U . . .
H20B H 0.601406 0.606330 0.105648 0.030 Uiso 1 1 calc R U . . .
C21 C 0.57227(13) 0.72655(12) 0.26585(9) 0.0232(3) Uani 1 1 d . . . . .
H21A H 0.641805 0.764014 0.247947 0.028 Uiso 1 1 calc R U . . .
H21B H 0.602527 0.662743 0.301418 0.028 Uiso 1 1 calc R U . . .
C22 C 0.46415(13) 0.79693(11) 0.31180(9) 0.0228(3) Uani 1 1 d . . . . .
H22A H 0.489912 0.820687 0.359057 0.027 Uiso 1 1 calc R U . . .
H22B H 0.431040 0.859751 0.276198 0.027 Uiso 1 1 calc R U . . .
C23 C 0.26887(13) 0.77300(11) 0.39205(8) 0.0208(3) Uani 1 1 d . . . . .
C24 C 0.24361(15) 0.86995(12) 0.42350(9) 0.0270(3) Uani 1 1 d . . . . .
H24 H 0.300350 0.916078 0.408601 0.032 Uiso 1 1 calc R U . . .
C25 C 0.13356(16) 0.89916(13) 0.47748(10) 0.0324(4) Uani 1 1 d . . . . .
H25 H 0.115990 0.965228 0.499905 0.039 Uiso 1 1 calc R U . . .
C26 C 0.05076(15) 0.83342(13) 0.49836(9) 0.0316(4) Uani 1 1 d . . . . .
H26 H -0.024283 0.854819 0.534498 0.038 Uiso 1 1 calc R U . . .
C27 C 0.07549(14) 0.73538(13) 0.46711(9) 0.0257(3) Uani 1 1 d . . . . .
H27 H 0.017894 0.689967 0.481807 0.031 Uiso 1 1 calc R U . . .
C28 C 0.18489(13) 0.70517(11) 0.41450(8) 0.0203(3) Uani 1 1 d . . . . .
C29A C -0.02321(15) 0.95867(14) -0.00952(9) 0.0176(6) Uiso 0.885(7) 1 d . . P .
.
C29B C 0.0472(13) 0.9910(10) -0.0291(8) 0.018(5) Uiso 0.115(7) 1 d . . P . .
C30 C 0.03889(14) 0.89703(11) -0.07341(8) 0.0215(3) Uani 1 1 d . . . . .
C31 C -0.04030(13) 0.82113(12) -0.07032(9) 0.0229(3) Uani 1 1 d . . . . .
C32 C -0.03015(14) 0.73555(12) -0.11513(9) 0.0246(3) Uani 1 1 d . . . . .
H32 H 0.038060 0.720025 -0.157610 0.029 Uiso 1 1 calc R U . . .
C33 C -0.11845(14) 0.67297(12) -0.09838(9) 0.0275(3) Uani 1 1 d . . . . .
H33 H -0.110262 0.614976 -0.129458 0.033 Uiso 1 1 calc R U . . .
C34 C -0.21922(15) 0.69436(12) -0.03630(9) 0.0271(3) Uani 1 1 d . . . . .
H34 H -0.279632 0.651293 -0.025755 0.033 Uiso 1 1 calc R U . . .
C35 C -0.23192(14) 0.77835(12) 0.01032(9) 0.0248(3) Uani 1 1 d . . . . .
H35 H -0.300369 0.791737 0.052926 0.030 Uiso 1 1 calc R U . . .
C36 C -0.14512(13) 0.84278(12) -0.00506(8) 0.0224(3) Uani 1 1 d . . . . .
C37 C -0.13381(13) 0.93316(11) 0.03480(9) 0.0210(3) Uani 1 1 d . . . . .
C38 C -0.19978(14) 0.99208(11) 0.10078(9) 0.0227(3) Uani 1 1 d . . . . .
C39 C -0.30963(14) 0.96995(11) 0.14987(9) 0.0243(3) Uani 1 1 d . . . . .
H39 H -0.343158 0.913943 0.137506 0.029 Uiso 1 1 calc R U . . .
C40 C -0.36961(15) 1.02598(12) 0.21448(10) 0.0281(3) Uani 1 1 d . . . . .
H40 H -0.442240 1.007697 0.246527 0.034 Uiso 1 1 calc R U . . .
C41 C -0.32346(15) 1.11063(12) 0.23327(10) 0.0275(3) Uani 1 1 d . . . . .
H41 H -0.365363 1.150108 0.277657 0.033 Uiso 1 1 calc R U . . .
C42 C -0.21766(14) 1.13601(12) 0.18728(9) 0.0244(3) Uani 1 1 d . . . . .
H42 H -0.188322 1.193813 0.200589 0.029 Uiso 1 1 calc R U . . .
C43 C -0.15066(14) 1.07982(11) 0.12105(9) 0.0226(3) Uani 1 1 d . . . . .
C44 C 0.52256(13) 0.54558(11) 0.49765(8) 0.0185(3) Uani 1 1 d . . . . .
C45 C 0.45472(13) 0.63465(11) 0.53615(8) 0.0183(3) Uani 1 1 d . . . . .
C46 C 0.53540(13) 0.71152(11) 0.51520(8) 0.0189(3) Uani 1 1 d . . . . .
C47 C 0.52250(14) 0.81475(12) 0.53447(9) 0.0233(3) Uani 1 1 d . . . . .
H47 H 0.448820 0.847691 0.567335 0.028 Uiso 1 1 calc R U . . .
C48 C 0.61746(15) 0.86952(12) 0.50560(10) 0.0286(3) Uani 1 1 d . . . . .
H48 H 0.607929 0.939786 0.519008 0.034 Uiso 1 1 calc R U . . .
C49 C 0.72604(14) 0.82284(12) 0.45743(10) 0.0274(3) Uani 1 1 d . . . . .
H49 H 0.789739 0.861537 0.438195 0.033 Uiso 1 1 calc R U . . .
C50 C 0.74230(13) 0.72004(12) 0.43712(9) 0.0224(3) Uani 1 1 d . . . . .
H50 H 0.817134 0.688690 0.404503 0.027 Uiso 1 1 calc R U . . .
C51 C 0.64871(13) 0.66276(11) 0.46462(8) 0.0191(3) Uani 1 1 d . . . . .
C52 C 0.63908(13) 0.55580(11) 0.45341(8) 0.0185(3) Uani 1 1 d . . . . .
C53 C 0.71271(13) 0.46760(11) 0.41204(8) 0.0185(3) Uani 1 1 d . . . . .
C54 C 0.83081(13) 0.46954(12) 0.36458(8) 0.0210(3) Uani 1 1 d . . . . .
H54 H 0.862377 0.532259 0.359224 0.025 Uiso 1 1 calc R U . . .
C55 C 0.90148(13) 0.38404(12) 0.32598(9) 0.0235(3) Uani 1 1 d . . . . .
H55 H 0.980511 0.388289 0.294879 0.028 Uiso 1 1 calc R U . . .
C56 C 0.85719(14) 0.29078(12) 0.33241(9) 0.0228(3) Uani 1 1 d . . . . .
H56 H 0.906449 0.231444 0.306208 0.027 Uiso 1 1 calc R U . . .
C57 C 0.74211(13) 0.28520(12) 0.37678(8) 0.0212(3) Uani 1 1 d . . . . .
H57 H 0.713160 0.221478 0.380026 0.025 Uiso 1 1 calc R U . . .
C58 C 0.66542(13) 0.37032(11) 0.41763(8) 0.0189(3) Uani 1 1 d . . . . .
K1 K 0.28207(3) 0.66518(2) 0.20706(2) 0.01799(8) Uani 1 1 d . . . . .
O1 O 0.29148(9) 0.86293(8) 0.10203(6) 0.0235(2) Uani 1 1 d . . . . .
O2 O 0.39967(9) 0.67194(8) 0.03910(6) 0.0243(2) Uani 1 1 d . . . . .
O3 O 0.16897(9) 0.59737(8) 0.09251(6) 0.0234(2) Uani 1 1 d . . . . .
O4 O 0.01487(9) 0.68241(8) 0.24100(6) 0.0212(2) Uani 1 1 d . . . . .
O5 O 0.09993(9) 0.86564(8) 0.20845(6) 0.0251(2) Uani 1 1 d . . . . .
O6 O 0.22209(9) 0.61101(8) 0.37999(6) 0.0214(2) Uani 1 1 d . . . . .
O7 O 0.23518(9) 0.45817(8) 0.27777(6) 0.0231(2) Uani 1 1 d . . . . .
O8 O 0.48144(9) 0.48520(8) 0.19973(6) 0.0230(2) Uani 1 1 d . . . . .
O9 O 0.53256(9) 0.69704(8) 0.19656(6) 0.0222(2) Uani 1 1 d . . . . .
O10 O 0.37175(9) 0.73445(8) 0.33830(6) 0.0224(2) 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
C1 O1 1.4258(17) . ?
C1 C2 1.494(2) . ?
C2 O2 1.4296(18) . ?
C3 O2 1.4254(18) . ?
C3 C4 1.509(2) . ?
C4 O3 1.4231(18) . ?
C5 O3 1.4276(17) . ?
C5 C6 1.507(2) . ?
C6 O4 1.4291(17) . ?
C7 O4 1.4305(17) . ?
C7 C8 1.495(2) . ?
C8 O5 1.4286(17) . ?
C9 O5 1.3673(18) . ?
C9 C10 1.381(2) . ?
C9 C14 1.406(2) . ?
C10 C11 1.394(2) . ?
C11 C12 1.372(3) . ?
C12 C13 1.391(2) . ?
C13 C14 1.379(2) . ?
C14 O1 1.3717(18) . ?
C15 O6 1.4260(17) . ?
C15 C16 1.495(2) . ?
C16 O7 1.4299(17) . ?
C17 O7 1.4251(18) . ?
C17 C18 1.507(2) . ?
C18 O8 1.4229(18) . ?
C19 O8 1.4285(17) . ?
C19 C20 1.506(2) . ?
C20 O9 1.4306(18) . ?
C21 O9 1.4307(17) . ?
C21 C22 1.496(2) . ?
C22 O10 1.4311(17) . ?
C23 O10 1.3669(17) . ?
C23 C24 1.383(2) . ?
C23 C28 1.402(2) . ?
C23 K1 3.5233(14) . ?
C24 C25 1.397(2) . ?
C25 C26 1.370(2) . ?
C26 C27 1.395(2) . ?
C27 C28 1.382(2) . ?
C28 O6 1.3714(17) . ?
C28 K1 3.5220(14) . ?
C29A C29B 0.942(12) 2_575 ?
C29A C29B 0.961(13) . ?
C29A C29A 1.387(4) 2_575 ?
C29A C30 1.406(2) . ?
C29A C37 1.408(2) . ?
C29B C29B 1.30(3) 2_575 ?
C29B C37 1.513(13) 2_575 ?
C29B C30 1.538(12) . ?
C29B C38 1.941(14) 2_575 ?
C29B C43 1.953(14) 2_575 ?
C30 C43 1.428(2) 2_575 ?
C30 C31 1.457(2) . ?
C31 C32 1.395(2) . ?
C31 C36 1.456(2) . ?
C32 C33 1.385(2) . ?
C33 C34 1.394(2) . ?
C34 C35 1.391(2) . ?
C35 C36 1.389(2) . ?
C36 C37 1.464(2) . ?
C37 C38 1.424(2) . ?
C38 C39 1.416(2) . ?
C38 C43 1.472(2) . ?
C39 C40 1.370(2) . ?
C40 C41 1.407(2) . ?
C41 C42 1.373(2) . ?
C42 C43 1.412(2) . ?
C44 C44 1.381(3) 2_666 ?
C44 C45 1.400(2) . ?
C44 C52 1.402(2) . ?
C45 C58 1.4337(19) 2_666 ?
C45 C46 1.465(2) . ?
C46 C47 1.395(2) . ?
C46 C51 1.453(2) . ?
C47 C48 1.392(2) . ?
C48 C49 1.390(2) . ?
C49 C50 1.390(2) . ?
C50 C51 1.398(2) . ?
C51 C52 1.462(2) . ?
C52 C53 1.433(2) . ?
C53 C54 1.416(2) . ?
C53 C58 1.467(2) . ?
C54 C55 1.374(2) . ?
C55 C56 1.399(2) . ?
C56 C57 1.376(2) . ?
C57 C58 1.411(2) . ?
K1 O3 2.7871(10) . ?
K1 O8 2.8390(10) . ?
K1 O9 2.8745(10) . ?
K1 O10 2.8753(10) . ?
K1 O4 2.8839(10) . ?
K1 O2 2.8903(10) . ?
K1 O6 2.8930(10) . ?
K1 O5 2.9230(10) . ?
K1 O7 2.9357(10) . ?
K1 O1 2.9509(10) . ?

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 C1 C2 106.95(12) . . ?
O2 C2 C1 109.30(12) . . ?
O2 C3 C4 113.08(12) . . ?
O3 C4 C3 108.15(12) . . ?
O3 C5 C6 108.57(11) . . ?
O4 C6 C5 113.97(12) . . ?
O4 C7 C8 108.96(11) . . ?
O5 C8 C7 105.46(11) . . ?
O5 C9 C10 125.93(14) . . ?
O5 C9 C14 113.93(13) . . ?
C10 C9 C14 120.13(14) . . ?
C9 C10 C11 119.58(16) . . ?
C12 C11 C10 120.20(16) . . ?
C11 C12 C13 120.62(15) . . ?
C14 C13 C12 119.75(16) . . ?
O1 C14 C13 125.89(14) . . ?
O1 C14 C9 114.39(12) . . ?
C13 C14 C9 119.71(14) . . ?
O6 C15 C16 106.15(11) . . ?
O7 C16 C15 108.56(12) . . ?
O7 C17 C18 113.54(12) . . ?
O8 C18 C17 108.71(12) . . ?
O8 C19 C20 108.43(11) . . ?
O9 C20 C19 113.57(12) . . ?
O9 C21 C22 108.93(11) . . ?
O10 C22 C21 105.65(11) . . ?
O10 C23 C24 125.60(14) . . ?
O10 C23 C28 114.26(12) . . ?
C24 C23 C28 120.14(14) . . ?
O10 C23 K1 51.36(6) . . ?
C24 C23 K1 140.07(10) . . ?
C28 C23 K1 78.47(8) . . ?
C23 C24 C25 119.14(15) . . ?
C26 C25 C24 120.62(15) . . ?
C25 C26 C27 120.69(15) . . ?
C28 C27 C26 119.13(15) . . ?
O6 C28 C27 125.53(14) . . ?
O6 C28 C23 114.20(12) . . ?
C27 C28 C23 120.28(14) . . ?
O6 C28 K1 52.24(6) . . ?
C27 C28 K1 139.13(10) . . ?
C23 C28 K1 78.57(8) . . ?
C29B C29A C29B 86.4(13) 2_575 . ?
C29B C29A C30 165.0(9) 2_575 . ?
C29B C29A C30 78.6(8) . . ?
C29A C29A C30 121.21(19) 2_575 . ?
C29B C29A C37 77.4(9) 2_575 . ?
C29B C29A C37 163.8(9) . . ?
C29A C29A C37 121.12(19) 2_575 . ?
C30 C29A C37 117.67(16) . . ?
C29A C29B C29A 93.6(13) 2_575 . ?
C29A C29B C29B 47.4(9) 2_575 2_575 ?
C29A C29B C29B 46.2(9) . 2_575 ?
C29A C29B C37 65.2(8) 2_575 2_575 ?
C29A C29B C37 158.8(13) . 2_575 ?
C29B C29B C37 112.6(14) 2_575 2_575 ?
C29A C29B C30 157.3(14) 2_575 . ?
C29A C29B C30 63.7(7) . . ?
C29B C29B C30 109.9(14) 2_575 . ?
C37 C29B C30 137.5(10) 2_575 . ?
C29A C29B C38 111.9(11) 2_575 2_575 ?
C29A C29B C38 154.5(12) . 2_575 ?
C29B C29B C38 159.3(15) 2_575 2_575 ?
C37 C29B C38 46.7(4) 2_575 2_575 ?
C30 C29B C38 90.8(7) . 2_575 ?
C29A C29B C43 156.3(13) 2_575 2_575 ?
C29A C29B C43 110.1(10) . 2_575 ?
C29B C29B C43 156.3(15) 2_575 2_575 ?
C37 C29B C43 91.1(7) 2_575 2_575 ?
C30 C29B C43 46.4(4) . 2_575 ?
C29A C30 C43 120.06(14) . 2_575 ?
C29A C30 C31 102.23(13) . . ?
C43 C30 C31 137.71(13) 2_575 . ?
C43 C30 C29B 82.3(5) 2_575 . ?
C31 C30 C29B 140.0(5) . . ?
C32 C31 C36 118.61(14) . . ?
C32 C31 C30 132.17(14) . . ?
C36 C31 C30 109.19(13) . . ?
C33 C32 C31 120.71(14) . . ?
C32 C33 C34 120.56(15) . . ?
C35 C34 C33 120.45(15) . . ?
C36 C35 C34 120.41(14) . . ?
C35 C36 C31 119.26(14) . . ?
C35 C36 C37 131.90(13) . . ?
C31 C36 C37 108.82(13) . . ?
C29A C37 C38 120.10(14) . . ?
C29A C37 C36 102.09(13) . . ?
C38 C37 C36 137.79(13) . . ?
C38 C37 C29B 82.7(5) . 2_575 ?
C36 C37 C29B 139.5(5) . 2_575 ?
C39 C38 C37 123.77(13) . . ?
C39 C38 C43 117.38(14) . . ?
C37 C38 C43 118.84(13) . . ?
C39 C38 C29B 174.3(4) . 2_575 ?
C37 C38 C29B 50.6(4) . 2_575 ?
C43 C38 C29B 68.2(4) . 2_575 ?
C40 C39 C38 122.71(14) . . ?
C39 C40 C41 119.90(15) . . ?
C42 C41 C40 119.82(15) . . ?
C41 C42 C43 122.76(14) . . ?
C42 C43 C30 123.93(13) . 2_575 ?
C42 C43 C38 117.42(14) . . ?
C30 C43 C38 118.66(13) 2_575 . ?
C42 C43 C29B 175.2(4) . 2_575 ?
C30 C43 C29B 51.3(4) 2_575 2_575 ?
C38 C43 C29B 67.4(4) . 2_575 ?
C44 C44 C45 122.37(16) 2_666 . ?
C44 C44 C52 122.39(17) 2_666 . ?
C45 C44 C52 115.24(13) . . ?
C44 C45 C58 118.18(13) . 2_666 ?
C44 C45 C46 104.27(12) . . ?
C58 C45 C46 137.55(13) 2_666 . ?
C47 C46 C51 119.05(13) . . ?
C47 C46 C45 132.94(13) . . ?
C51 C46 C45 108.01(12) . . ?
C48 C47 C46 120.08(14) . . ?
C49 C48 C47 120.91(14) . . ?
C48 C49 C50 120.62(14) . . ?
C49 C50 C51 120.10(14) . . ?
C50 C51 C46 119.23(13) . . ?
C50 C51 C52 132.43(13) . . ?
C46 C51 C52 108.34(12) . . ?
C44 C52 C53 117.96(13) . . ?
C44 C52 C51 104.14(12) . . ?
C53 C52 C51 137.91(13) . . ?
C54 C53 C52 122.86(13) . . ?
C54 C53 C58 117.42(13) . . ?
C52 C53 C58 119.71(12) . . ?
C55 C54 C53 122.43(14) . . ?
C54 C55 C56 120.09(14) . . ?
C57 C56 C55 119.84(14) . . ?
C56 C57 C58 122.62(14) . . ?
C57 C58 C45 123.03(13) . 2_666 ?
C57 C58 C53 117.58(13) . . ?
C45 C58 C53 119.39(13) 2_666 . ?
O3 K1 O8 92.58(3) . . ?
O3 K1 O9 129.88(3) . . ?
O8 K1 O9 61.93(3) . . ?
O3 K1 O10 173.20(3) . . ?
O8 K1 O10 90.85(3) . . ?
O9 K1 O10 56.90(3) . . ?
O3 K1 O4 62.69(3) . . ?
O8 K1 O4 130.88(3) . . ?
O9 K1 O4 164.76(3) . . ?
O10 K1 O4 110.74(3) . . ?
O3 K1 O2 61.49(3) . . ?
O8 K1 O2 75.13(3) . . ?
O9 K1 O2 70.13(3) . . ?
O10 K1 O2 125.15(3) . . ?
O4 K1 O2 118.44(3) . . ?
O3 K1 O6 122.21(3) . . ?
O8 K1 O6 89.26(3) . . ?
O9 K1 O6 101.18(3) . . ?
O10 K1 O6 51.94(3) . . ?
O4 K1 O6 73.21(3) . . ?
O2 K1 O6 164.28(3) . . ?
O3 K1 O5 90.97(3) . . ?
O8 K1 O5 173.08(3) . . ?
O9 K1 O5 111.34(3) . . ?
O10 K1 O5 86.25(3) . . ?
O4 K1 O5 56.02(3) . . ?
O2 K1 O5 101.46(3) . . ?
O6 K1 O5 93.88(3) . . ?
O3 K1 O7 75.28(3) . . ?
O8 K1 O7 60.24(3) . . ?
O9 K1 O7 117.02(3) . . ?
O10 K1 O7 101.45(3) . . ?
O4 K1 O7 72.19(3) . . ?
O2 K1 O7 115.02(3) . . ?
O6 K1 O7 56.28(3) . . ?
O5 K1 O7 126.51(3) . . ?
O3 K1 O1 89.19(3) . . ?
O8 K1 O1 123.13(3) . . ?
O9 K1 O1 74.07(3) . . ?
O10 K1 O1 93.85(3) . . ?
O4 K1 O1 99.65(3) . . ?
O2 K1 O1 56.46(3) . . ?
O6 K1 O1 135.23(3) . . ?
O5 K1 O1 50.96(3) . . ?
O7 K1 O1 164.40(3) . . ?
O3 K1 C28 132.13(3) . . ?
O8 K1 C28 106.83(3) . . ?
O9 K1 C28 97.53(3) . . ?
O10 K1 C28 41.10(3) . . ?
O4 K1 C28 71.85(3) . . ?
O2 K1 C28 165.22(3) . . ?
O6 K1 C28 22.01(3) . . ?
O5 K1 C28 74.91(3) . . ?
O7 K1 C28 77.44(3) . . ?
O1 K1 C28 113.26(3) . . ?
O3 K1 C23 151.72(3) . . ?
O8 K1 C23 107.38(3) . . ?
O9 K1 C23 78.05(3) . . ?
O10 K1 C23 21.80(3) . . ?
O4 K1 C23 89.02(3) . . ?
O2 K1 C23 142.26(3) . . ?
O6 K1 C23 41.11(3) . . ?
O5 K1 C23 71.50(3) . . ?
O7 K1 C23 97.08(3) . . ?
O1 K1 C23 96.02(3) . . ?
C28 K1 C23 22.96(3) . . ?
C14 O1 C1 117.80(11) . . ?
C14 O1 K1 107.88(8) . . ?
C1 O1 K1 112.55(8) . . ?
C3 O2 C2 113.32(11) . . ?
C3 O2 K1 106.56(8) . . ?
C2 O2 K1 120.91(8) . . ?
C4 O3 C5 111.52(11) . . ?
C4 O3 K1 117.81(8) . . ?
C5 O3 K1 115.77(8) . . ?
C6 O4 C7 112.62(11) . . ?
C6 O4 K1 105.31(8) . . ?
C7 O4 K1 121.02(8) . . ?
C9 O5 C8 118.68(11) . . ?
C9 O5 K1 109.14(8) . . ?
C8 O5 K1 115.13(8) . . ?
C28 O6 C15 118.39(11) . . ?
C28 O6 K1 105.75(8) . . ?
C15 O6 K1 114.97(8) . . ?
C17 O7 C16 112.63(11) . . ?
C17 O7 K1 107.95(8) . . ?
C16 O7 K1 118.99(8) . . ?
C18 O8 C19 111.42(11) . . ?
C18 O8 K1 118.78(8) . . ?
C19 O8 K1 115.14(8) . . ?
C20 O9 C21 113.05(11) . . ?
C20 O9 K1 107.34(8) . . ?
C21 O9 K1 119.87(8) . . ?
C23 O10 C22 118.93(11) . . ?
C23 O10 K1 106.84(8) . . ?
C22 O10 K1 113.73(8) . . ?

_refine_diff_density_max         0.178
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.043

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: tetrahydrofuran'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1820792'
_audit_update_record             
;
2018-01-30 deposited with the CCDC.
2018-05-25 downloaded from the CCDC.
;

_audit_creation_date             2018-01-23
_audit_block_code                WOM-RUB/K/THF/100/120/20/

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 0.00 0.00 0.1300
1.00 0.00 0.00 0.1060
1.00 3.00 -3.00 0.1620
-1.00 -3.00 3.00 0.1260
3.00 -1.00 -1.00 0.0490
-3.00 1.00 1.00 0.1040
-1.00 1.00 -1.00 0.1680
1.00 -3.00 3.00 0.1170
_diffrn_radiation_source         'Incoatec ImuS/Mo'
_diffrn_radiation_monochromator  'Incoatec Helios mirrors'
_exptl_special_details           
;
 Crystal mounted on a MiTeGen loop using Perfluoropolyether PFO-XR75
;

# start Validation Reply Form
_vrf_PLAT411_2                   
;
PROBLEM: Short Inter H...H Contact H20A     ..H47D      .       1.98 Ang.  
RESPONSE:  H47D belongs to the minor component of the disordered tetrahydrofuran 
solvent molecule.
;
_vrf_PLAT934_2                   
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....          2 Check 
RESPONSE:  Two low-angle weak reflections (0 0 4) and (1 -2 1) at respectively 
3.06 and 6.21 A resolution exhibited calculated Fo2 significantly higher than 
Fc2. The ratios error/esd were respectively 11.67 and 11.18. We have no 
explanation for this other than the low angle reflections were measured with 
a high redundancy resulting in lower estimated standard uncertainties for 
these intensities and higher than expected (Fo2 - Fc2)/SigmaW values. 
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        
;
(5,6:11,12-di-o-phenylenetetracene)-di(potassium-di(benzo-15-crown-5))
;

_chemical_melting_point          ?
_chemical_formula_moiety         '2(C28 H40 K O10), 2(C4 H8 O), C30 H16'
_chemical_formula_sum            'C94 H112 K2 O22'
_chemical_formula_weight         1672.03

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.746(7)
_cell_length_b                   13.528(3)
_cell_length_c                   13.986(4)
_cell_angle_alpha                117.713(4)
_cell_angle_beta                 94.525(6)
_cell_angle_gamma                96.238(5)
_cell_volume                     2099.2(13)
_cell_formula_units_Z            1


_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9981
_cell_measurement_theta_min      2.3474
_cell_measurement_theta_max      34.2134

_exptl_crystal_description       plate
_exptl_crystal_colour            red-black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_F_000             890
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    0.189
_shelx_estimated_absorpt_T_min   0.949
_shelx_estimated_absorpt_T_max   0.972

_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.92526
_exptl_absorpt_correction_T_max  0.97842
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           Mo-K\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker-AXS ImuS Kappa Mach3 APEX-II'
_diffrn_measurement_method       'CCD φ- and ω-scans'
_diffrn_detector_area_resol_mean 66.67
_diffrn_reflns_number            75133
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.625
_diffrn_reflns_theta_max         34.478
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             17651
_reflns_number_gt                13585
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (G. M. Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL (G. M. Sheldrick, 2015)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
_refine_special_details

 The minimum and maximum estimated transmissions from the multi-scan
 scaling are 0.8774 and 1.0000 (SADABS).

INTENSITY STATISTICS FOR DATASET 

 Resolution  #Data #Theory %Complete Redundancy Mean I Mean I/s Rmerge  Rsigma

 Inf - 2.55     265    265    100.0     6.33      42.9   68.18  0.0242  0.0135
2.55 - 1.70     637    637    100.0     6.35      14.5   55.58  0.0229  0.0140
1.70 - 1.35     890    890    100.0     6.33       6.2   46.50  0.0259  0.0158
1.35 - 1.18     884    885     99.9     6.06       5.1   41.31  0.0287  0.0173
1.18 - 1.07     905    905    100.0     5.55       4.3   35.81  0.0328  0.0198
1.07 - 0.99     956    956    100.0     5.18       2.4   26.58  0.0392  0.0257
0.99 - 0.94     766    766    100.0     4.83       1.7   21.33  0.0514  0.0328
0.94 - 0.89     925    925    100.0     4.62       1.6   20.19  0.0508  0.0358
0.89 - 0.85     928    928    100.0     4.38       1.4   17.61  0.0589  0.0408
0.85 - 0.82     817    817    100.0     4.19       1.1   14.10  0.0701  0.0517
0.82 - 0.79     918    918    100.0     4.02       0.9   12.14  0.0806  0.0618
0.79 - 0.76    1112   1112    100.0     3.85       0.7    9.94  0.0903  0.0765
0.76 - 0.74     851    851    100.0     3.73       0.8    9.94  0.0909  0.0755
0.74 - 0.72     931    931    100.0     3.54       0.7    8.91  0.1013  0.0870
0.72 - 0.70    1022   1022    100.0     3.46       0.7    8.33  0.1060  0.0933
0.70 - 0.69     582    583     99.8     3.32       0.6    7.68  0.1163  0.0998
0.69 - 0.67    1208   1212     99.7     3.23       0.6    7.10  0.1234  0.1137
0.67 - 0.66     712    718     99.2     3.11       0.5    5.90  0.1465  0.1381
0.66 - 0.65     670    676     99.1     3.07       0.5    5.68  0.1505  0.1460
0.65 - 0.63    1672   1777     94.1     2.73       0.4    4.49  0.1938  0.1873
#------------------------------------------------------------------------------
0.73 - 0.63    6349   6471     98.1     3.13       0.5    6.55  0.1314  0.1234
 Inf - 0.63   17651  17774     99.3     4.23       2.7   18.59  0.0352  0.0289
#-------------------------------------------------------------------------------

 The solvent tetrahydrofuran is partially disordered (37.9(4)%), so is the
 5,6:11,12-di-o-phenylenetetracene ligand (12.3(3)% based on refinement of
 the atom C29 split over two positions: C29A and C29B were refined with 
 isotropic atomic displacement parameters). The atoms of the minor component 
 of the partially disordered solvent tetrahydrofuran molecule were refined
 with isotropic atomic displacement parameters. 

 H47D belongs to the minor component of the disordered tetrahydrofuran 
 solvent molecule.

 Low-angle reflections were measured with a higher redundancy resulting
 in lower estimated standard uncertainties for these intensities and higher 
 than expected (Iobs-Icalc)/SigmaW values.

 Most Disagreeable Reflections (* if suppressed or used for Rfree).
 Error/esd is calculated as sqrt(wD^2/<wD^2>) where w is given by the weight
 formula, D = Fo2-Fc2 and <> refers to the average over all reflections.

     h   k   l         Fo^2         Fc^2   Error/esd Fc/Fc(max) Resolution(A)

     0   0   4         74.24          3.30      11.67       0.007       3.06
     1  -2   1        362.97        105.99      11.18       0.040       6.21
     2  -2   1         25.24        137.65       8.40       0.046       4.85
     3  -3  12         42.05          0.11       8.09       0.001       1.06

 Highest peak    0.89  at  0.2676  0.7504  0.0385  [  0.60 A from K1 ]
 Deepest hole   -0.43  at  0.2587  0.5855  0.4407  [  0.51 A from C42 ]
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0908P)²+0.9054P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         17651
_refine_ls_number_parameters     552
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0564
_refine_ls_wR_factor_ref         0.1706
_refine_ls_wR_factor_gt          0.1547
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.97033(11) 0.41105(11) 0.21931(11) 0.0252(2) Uani 1 1 d . . . . .
H1A H 0.914371 0.409151 0.263938 0.030 Uiso 1 1 calc R U . . .
H1B H 1.034194 0.464471 0.268572 0.030 Uiso 1 1 calc R U . . .
C2 C 0.99761(10) 0.29457(11) 0.15390(12) 0.0261(2) Uani 1 1 d . . . . .
H2A H 1.053633 0.297466 0.109681 0.031 Uiso 1 1 calc R U . . .
H2B H 1.025406 0.267085 0.203729 0.031 Uiso 1 1 calc R U . . .
C3 C 0.92867(10) 0.11736(10) -0.00169(12) 0.0256(2) Uani 1 1 d . . . . .
H3A H 0.869998 0.054332 -0.019965 0.031 Uiso 1 1 calc R U . . .
H3B H 0.994656 0.099135 0.024257 0.031 Uiso 1 1 calc R U . . .
C4 C 0.94357(11) 0.12690(12) -0.10282(12) 0.0276(2) Uani 1 1 d . . . . .
H4A H 1.000311 0.191494 -0.084941 0.033 Uiso 1 1 calc R U . . .
H4B H 0.965495 0.057011 -0.157974 0.033 Uiso 1 1 calc R U . . .
C5 C 0.85628(12) 0.15589(14) -0.24043(13) 0.0323(3) Uani 1 1 d . . . . .
H5A H 0.867243 0.083305 -0.301351 0.039 Uiso 1 1 calc R U . . .
H5B H 0.918913 0.213889 -0.225259 0.039 Uiso 1 1 calc R U . . .
C6 C 0.75638(12) 0.19105(13) -0.27174(12) 0.0302(3) Uani 1 1 d . . . . .
H6A H 0.760658 0.192019 -0.341675 0.036 Uiso 1 1 calc R U . . .
H6B H 0.694043 0.134227 -0.283248 0.036 Uiso 1 1 calc R U . . .
C7 C 0.80511(12) 0.39127(13) -0.19318(12) 0.0300(3) Uani 1 1 d . . . . .
H7A H 0.779276 0.397985 -0.258209 0.036 Uiso 1 1 calc R U . . .
H7B H 0.879991 0.378215 -0.196413 0.036 Uiso 1 1 calc R U . . .
C8 C 0.79835(11) 0.49710(12) -0.09123(12) 0.0276(3) Uani 1 1 d . . . . .
H8A H 0.838697 0.563840 -0.091342 0.033 Uiso 1 1 calc R U . . .
H8B H 0.723116 0.507952 -0.085157 0.033 Uiso 1 1 calc R U . . .
C9 C 0.85434(10) 0.57110(10) 0.10056(11) 0.0230(2) Uani 1 1 d . . . . .
C10 C 0.82064(11) 0.67429(11) 0.12993(12) 0.0262(2) Uani 1 1 d . . . . .
H10 H 0.787828 0.689109 0.075587 0.031 Uiso 1 1 calc R U . . .
C11 C 0.83526(12) 0.75627(11) 0.23988(13) 0.0302(3) Uani 1 1 d . . . . .
H11 H 0.812313 0.827003 0.260278 0.036 Uiso 1 1 calc R U . . .
C12 C 0.88299(12) 0.73484(12) 0.31910(13) 0.0303(3) Uani 1 1 d . . . . .
H12 H 0.892743 0.791054 0.393654 0.036 Uiso 1 1 calc R U . . .
C13 C 0.91698(11) 0.63110(11) 0.29032(11) 0.0260(2) Uani 1 1 d . . . . .
H13 H 0.949565 0.616653 0.345019 0.031 Uiso 1 1 calc R U . . .
C14 C 0.90281(10) 0.54949(10) 0.18148(11) 0.0225(2) Uani 1 1 d . . . . .
C15 C 0.71527(12) 0.26155(13) 0.26236(12) 0.0291(3) Uani 1 1 d . . . . .
H15A H 0.793707 0.278501 0.267675 0.035 Uiso 1 1 calc R U . . .
H15B H 0.698991 0.229154 0.311091 0.035 Uiso 1 1 calc R U . . .
C16 C 0.66688(13) 0.36694(13) 0.29327(12) 0.0314(3) Uani 1 1 d . . . . .
H16A H 0.588193 0.348509 0.284103 0.038 Uiso 1 1 calc R U . . .
H16B H 0.692916 0.422671 0.370667 0.038 Uiso 1 1 calc R U . . .
C17 C 0.63661(13) 0.49872(12) 0.23171(13) 0.0304(3) Uani 1 1 d . . . . .
H17A H 0.679128 0.552319 0.214200 0.036 Uiso 1 1 calc R U . . .
H17B H 0.621646 0.541553 0.307489 0.036 Uiso 1 1 calc R U . . .
C18 C 0.53277(12) 0.44869(12) 0.15471(13) 0.0293(3) Uani 1 1 d . . . . .
H18A H 0.491574 0.391410 0.168515 0.035 Uiso 1 1 calc R U . . .
H18B H 0.489503 0.508779 0.166304 0.035 Uiso 1 1 calc R U . . .
C19 C 0.46149(10) 0.34324(12) -0.03205(13) 0.0282(3) Uani 1 1 d . . . . .
H19A H 0.419458 0.400649 -0.032001 0.034 Uiso 1 1 calc R U . . .
H19B H 0.416948 0.292414 -0.012741 0.034 Uiso 1 1 calc R U . . .
C20 C 0.49225(11) 0.27596(13) -0.14349(13) 0.0288(3) Uani 1 1 d . . . . .
H20A H 0.426973 0.244187 -0.198322 0.035 Uiso 1 1 calc R U . . .
H20B H 0.538709 0.327515 -0.160479 0.035 Uiso 1 1 calc R U . . .
C21 C 0.47685(11) 0.08654(12) -0.17234(12) 0.0269(2) Uani 1 1 d . . . . .
H21A H 0.436984 0.049240 -0.247297 0.032 Uiso 1 1 calc R U . . .
H21B H 0.424857 0.106387 -0.119970 0.032 Uiso 1 1 calc R U . . .
C22 C 0.54455(11) 0.00846(11) -0.15804(12) 0.0271(2) Uani 1 1 d . . . . .
H22A H 0.500557 -0.065097 -0.177715 0.033 Uiso 1 1 calc R U . . .
H22B H 0.601735 -0.005219 -0.204515 0.033 Uiso 1 1 calc R U . . .
C23 C 0.65339(10) 0.01313(11) -0.00724(12) 0.0246(2) Uani 1 1 d . . . . .
C24 C 0.67683(12) -0.09491(12) -0.06734(15) 0.0315(3) Uani 1 1 d . . . . .
H24 H 0.646258 -0.140429 -0.141775 0.038 Uiso 1 1 calc R U . . .
C25 C 0.74640(12) -0.13624(13) -0.01669(17) 0.0371(4) Uani 1 1 d . . . . .
H25 H 0.762962 -0.210138 -0.057069 0.045 Uiso 1 1 calc R U . . .
C26 C 0.79049(12) -0.07022(14) 0.09086(17) 0.0366(4) Uani 1 1 d . . . . .
H26 H 0.837241 -0.099176 0.124184 0.044 Uiso 1 1 calc R U . . .
C27 C 0.76768(11) 0.03922(13) 0.15233(14) 0.0306(3) Uani 1 1 d . . . . .
H27 H 0.798958 0.084609 0.226565 0.037 Uiso 1 1 calc R U . . .
C28 C 0.69849(10) 0.08016(11) 0.10278(12) 0.0248(2) Uani 1 1 d . . . . .
C29A C -0.01281(12) 0.44355(12) 0.48652(12) 0.0236(3) Uiso 0.877(3) 1 d . . P .
.
C29B C 0.0491(8) 0.4911(9) 0.4814(9) 0.0236(3) Uiso 0.123(3) 1 d . . P . .
C30 C -0.11019(11) 0.40080(12) 0.50690(11) 0.0269(2) Uani 1 1 d . . . . .
C31 C -0.10205(12) 0.28348(13) 0.46931(11) 0.0282(3) Uani 1 1 d . . . . .
C32 C -0.16948(13) 0.19420(14) 0.46875(12) 0.0328(3) Uani 1 1 d . . . . .
H32 H -0.235845 0.206832 0.495103 0.039 Uiso 1 1 calc R U . . .
C33 C -0.14086(15) 0.08748(14) 0.43027(14) 0.0370(3) Uani 1 1 d . . . . .
H33 H -0.187032 0.028501 0.432075 0.044 Uiso 1 1 calc R U . . .
C34 C -0.04444(14) 0.06610(14) 0.38879(14) 0.0374(3) Uani 1 1 d . . . . .
H34 H -0.025880 -0.007309 0.362511 0.045 Uiso 1 1 calc R U . . .
C35 C 0.02414(13) 0.15128(14) 0.38581(13) 0.0336(3) Uani 1 1 d . . . . .
H35 H 0.088492 0.135085 0.356021 0.040 Uiso 1 1 calc R U . . .
C36 C -0.00036(12) 0.26126(13) 0.42631(12) 0.0293(3) Uani 1 1 d . . . . .
C37 C 0.05669(12) 0.36554(12) 0.43827(11) 0.0285(3) Uani 1 1 d . . . . .
C38 C 0.15824(12) 0.40458(12) 0.41699(11) 0.0290(3) Uani 1 1 d . . . . .
C39 C 0.23325(14) 0.33329(14) 0.37088(15) 0.0379(3) Uani 1 1 d . . . . .
H39 H 0.215917 0.255305 0.350468 0.045 Uiso 1 1 calc R U . . .
C40 C 0.33178(16) 0.37260(16) 0.35405(17) 0.0448(4) Uani 1 1 d . . . . .
H40 H 0.380629 0.321993 0.323252 0.054 Uiso 1 1 calc R U . . .
C41 C 0.35862(15) 0.48622(16) 0.38242(15) 0.0403(4) Uani 1 1 d . . . . .
H41 H 0.426226 0.513765 0.372066 0.048 Uiso 1 1 calc R U . . .
C42 C 0.28589(13) 0.55939(14) 0.42608(12) 0.0329(3) Uani 1 1 d . . . . .
H42 H 0.304761 0.636500 0.443864 0.040 Uiso 1 1 calc R U . . .
C43 C 0.18555(12) 0.52345(12) 0.44483(11) 0.0284(3) Uani 1 1 d . . . . .
K1 K 0.73187(2) 0.28465(2) 0.00760(2) 0.01998(6) Uani 1 1 d . . . . .
O1 O 0.93262(8) 0.44506(8) 0.14167(8) 0.02442(18) Uani 1 1 d . . . . .
O2 O 0.90447(7) 0.21930(7) 0.08409(8) 0.02285(17) Uani 1 1 d . . . . .
O3 O 0.84582(8) 0.14345(9) -0.14561(9) 0.02735(19) Uani 1 1 d . . . . .
O4 O 0.74047(8) 0.29978(9) -0.19122(8) 0.02613(18) Uani 1 1 d . . . . .
O5 O 0.84358(8) 0.48278(8) -0.00318(8) 0.02672(19) Uani 1 1 d . . . . .
O6 O 0.66829(8) 0.18422(8) 0.15191(8) 0.02548(18) Uani 1 1 d . . . . .
O7 O 0.69683(8) 0.41328(8) 0.22429(8) 0.02658(19) Uani 1 1 d . . . . .
O8 O 0.55574(8) 0.39748(8) 0.04572(9) 0.02620(19) Uani 1 1 d . . . . .
O9 O 0.54650(8) 0.18585(8) -0.15299(9) 0.02554(18) Uani 1 1 d . . . . .
O10 O 0.58886(8) 0.06531(8) -0.04538(8) 0.02521(18) Uani 1 1 d . . . . .
C44A C 0.3401(3) 0.1022(3) 0.4543(3) 0.0458(7) Uani 0.621(4) 1 d . . P A 1
H44A H 0.297035 0.053911 0.477541 0.055 Uiso 0.621(4) 1 calc R U P A 1
H44B H 0.294389 0.109980 0.398391 0.055 Uiso 0.621(4) 1 calc R U P A 1
C45A C 0.3821(4) 0.2179(3) 0.5516(3) 0.0559(10) Uani 0.621(4) 1 d . . P A 1
H45A H 0.341830 0.232828 0.613389 0.067 Uiso 0.621(4) 1 calc R U P A 1
H45B H 0.379956 0.279159 0.531938 0.067 Uiso 0.621(4) 1 calc R U P A 1
C46A C 0.5029(2) 0.2034(3) 0.5791(2) 0.0445(7) Uani 0.621(4) 1 d . . P A 1
H46A H 0.551747 0.276782 0.612837 0.053 Uiso 0.621(4) 1 calc R U P A 1
H46B H 0.507458 0.169552 0.628414 0.053 Uiso 0.621(4) 1 calc R U P A 1
C47A C 0.5267(3) 0.1270(3) 0.4715(3) 0.0508(9) Uani 0.621(4) 1 d . . P A 1
H47A H 0.553154 0.170312 0.434950 0.061 Uiso 0.621(4) 1 calc R U P A 1
H47B H 0.582093 0.083469 0.477655 0.061 Uiso 0.621(4) 1 calc R U P A 1
O11A O 0.43010(18) 0.05276(19) 0.41081(18) 0.0477(7) Uani 0.621(4) 1 d . . P A
1
C44B C 0.4923(15) 0.1833(16) 0.4487(15) 0.146(6) Uiso 0.379(4) 1 d . . P A 2
H44C H 0.541264 0.128204 0.438052 0.176 Uiso 0.379(4) 1 calc R U P A 2
H44D H 0.515760 0.231152 0.415629 0.176 Uiso 0.379(4) 1 calc R U P A 2
C45B C 0.3817(12) 0.1295(13) 0.4097(12) 0.123(4) Uiso 0.379(4) 1 d . . P A 2
H45C H 0.352601 0.145887 0.351841 0.147 Uiso 0.379(4) 1 calc R U P A 2
H45D H 0.376879 0.046409 0.378033 0.147 Uiso 0.379(4) 1 calc R U P A 2
C46B C 0.3204(18) 0.171(2) 0.4985(18) 0.174(7) Uiso 0.379(4) 1 d . . P A 2
H46C H 0.312793 0.250867 0.523083 0.208 Uiso 0.379(4) 1 calc R U P A 2
H46D H 0.248809 0.124263 0.478486 0.208 Uiso 0.379(4) 1 calc R U P A 2
C47B C 0.3838(14) 0.1595(14) 0.5779(14) 0.140(5) Uiso 0.379(4) 1 d . . P A 2
H47C H 0.448427 0.130162 0.562215 0.168 Uiso 0.379(4) 1 calc R U P A 2
H47D H 0.362291 0.181114 0.647422 0.168 Uiso 0.379(4) 1 calc R U P A 2
O11B O 0.4801(19) 0.245(2) 0.554(2) 0.270(10) Uiso 0.379(4) 1 d . . P A 2


_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
C1 O1 1.4327(15) . ?
C1 C2 1.5064(19) . ?
C2 O2 1.4244(16) . ?
C3 O2 1.4311(16) . ?
C3 C4 1.503(2) . ?
C3 K1 3.5272(16) . ?
C4 O3 1.4240(18) . ?
C5 O3 1.4268(19) . ?
C5 C6 1.509(2) . ?
C6 O4 1.4259(19) . ?
C7 O4 1.4229(17) . ?
C7 C8 1.496(2) . ?
C8 O5 1.4215(16) . ?
C9 O5 1.3683(17) . ?
C9 C10 1.3880(18) . ?
C9 C14 1.4089(17) . ?
C10 C11 1.398(2) . ?
C11 C12 1.383(2) . ?
C12 C13 1.398(2) . ?
C13 C14 1.3853(19) . ?
C14 O1 1.3669(15) . ?
C15 O6 1.4332(18) . ?
C15 C16 1.503(2) . ?
C16 O7 1.4276(18) . ?
C17 O7 1.4247(17) . ?
C17 C18 1.507(2) . ?
C18 O8 1.4218(19) . ?
C19 O8 1.4228(18) . ?
C19 C20 1.505(2) . ?
C20 O9 1.4244(17) . ?
C20 K1 3.5326(19) . ?
C21 O9 1.4250(17) . ?
C21 C22 1.506(2) . ?
C22 O10 1.4253(17) . ?
C23 O10 1.3662(15) . ?
C23 C24 1.3870(19) . ?
C23 C28 1.404(2) . ?
C24 C25 1.406(2) . ?
C25 C26 1.373(3) . ?
C26 C27 1.402(2) . ?
C27 C28 1.3897(18) . ?
C28 O6 1.3645(16) . ?
C29A C29B 0.974(11) 2_566 ?
C29A C29B 0.992(11) . ?
C29A C29A 1.385(3) 2_566 ?
C29A C37 1.410(2) . ?
C29A C30 1.418(2) . ?
C29B C29B 1.39(2) 2_566 ?
C29B C30 1.510(11) 2_566 ?
C29B C37 1.534(11) . ?
C29B C43 1.913(11) . ?
C29B C38 1.921(11) . ?
C30 C31 1.440(2) . ?
C30 C43 1.450(2) 2_566 ?
C31 C32 1.401(2) . ?
C31 C36 1.474(2) . ?
C32 C33 1.389(2) . ?
C33 C34 1.402(3) . ?
C34 C35 1.387(2) . ?
C35 C36 1.406(2) . ?
C36 C37 1.444(2) . ?
C37 C38 1.449(2) . ?
C38 C39 1.407(2) . ?
C38 C43 1.460(2) . ?
C39 C40 1.391(3) . ?
C40 C41 1.391(3) . ?
C41 C42 1.392(3) . ?
C42 C43 1.406(2) . ?
K1 O3 2.7635(12) . ?
K1 O2 2.7743(13) . ?
K1 O8 2.7982(14) . ?
K1 O7 2.8089(12) . ?
K1 O9 2.8456(14) . ?
K1 O4 2.8911(12) . ?
K1 O5 2.9689(12) . ?
K1 O1 3.0039(14) . ?
K1 O6 3.0243(11) . ?
K1 O10 3.0401(12) . ?
C44A O11A 1.426(4) . ?
C44A C45A 1.520(5) . ?
C45A C46A 1.613(6) . ?
C46A C47A 1.456(5) . ?
C47A O11A 1.421(4) . ?
C44B O11B 1.35(2) . ?
C44B C45B 1.45(2) . ?
C45B C46B 1.44(2) . ?
C46B C47B 1.40(2) . ?
C47B O11B 1.75(3) . ?

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 C1 C2 106.23(11) . . ?
O2 C2 C1 109.40(10) . . ?
O2 C3 C4 112.38(10) . . ?
O2 C3 K1 47.71(6) . . ?
C4 C3 K1 81.11(7) . . ?
O3 C4 C3 109.22(11) . . ?
O3 C5 C6 109.16(12) . . ?
O4 C6 C5 112.84(12) . . ?
O4 C7 C8 107.78(11) . . ?
O5 C8 C7 106.09(11) . . ?
O5 C9 C10 125.94(12) . . ?
O5 C9 C14 114.09(11) . . ?
C10 C9 C14 119.96(12) . . ?
C9 C10 C11 119.64(12) . . ?
C12 C11 C10 120.26(13) . . ?
C11 C12 C13 120.50(14) . . ?
C14 C13 C12 119.54(13) . . ?
O1 C14 C13 125.82(11) . . ?
O1 C14 C9 114.08(11) . . ?
C13 C14 C9 120.10(12) . . ?
O6 C15 C16 105.83(11) . . ?
O7 C16 C15 108.40(12) . . ?
O7 C17 C18 111.55(11) . . ?
O8 C18 C17 108.61(12) . . ?
O8 C19 C20 109.03(11) . . ?
O9 C20 C19 113.57(11) . . ?
O9 C20 K1 50.43(6) . . ?
C19 C20 K1 83.34(8) . . ?
O9 C21 C22 107.56(11) . . ?
O10 C22 C21 105.38(11) . . ?
O10 C23 C24 125.91(14) . . ?
O10 C23 C28 113.76(11) . . ?
C24 C23 C28 120.33(13) . . ?
C23 C24 C25 119.17(16) . . ?
C26 C25 C24 120.26(14) . . ?
C25 C26 C27 121.09(13) . . ?
C28 C27 C26 118.83(16) . . ?
O6 C28 C27 125.62(14) . . ?
O6 C28 C23 114.07(11) . . ?
C27 C28 C23 120.31(13) . . ?
C29B C29A C29B 90.4(9) 2_566 . ?
C29B C29A C29A 45.7(6) 2_566 2_566 ?
C29B C29A C37 167.6(7) 2_566 . ?
C29B C29A C37 77.2(6) . . ?
C29A C29A C37 121.88(18) 2_566 . ?
C29B C29A C30 75.8(6) 2_566 . ?
C29B C29A C30 166.1(6) . . ?
C29A C29A C30 121.50(17) 2_566 . ?
C37 C29A C30 116.62(13) . . ?
C29A C29B C29A 89.6(9) 2_566 . ?
C29A C29B C29B 45.3(6) 2_566 2_566 ?
C29A C29B C30 65.5(6) 2_566 2_566 ?
C29A C29B C30 155.1(10) . 2_566 ?
C29B C29B C30 110.8(11) 2_566 2_566 ?
C29A C29B C37 153.3(10) 2_566 . ?
C29A C29B C37 63.7(6) . . ?
C29B C29B C37 108.0(11) 2_566 . ?
C30 C29B C37 141.1(8) 2_566 . ?
C29A C29B C43 113.9(8) 2_566 . ?
C29A C29B C43 156.5(9) . . ?
C29B C29B C43 159.2(12) 2_566 . ?
C30 C29B C43 48.4(3) 2_566 . ?
C37 C29B C43 92.8(5) . . ?
C29A C29B C38 158.6(9) 2_566 . ?
C29A C29B C38 111.7(8) . . ?
C29B C29B C38 156.0(12) 2_566 . ?
C30 C29B C38 93.1(5) 2_566 . ?
C37 C29B C38 48.0(3) . . ?
C29A C30 C31 102.64(13) . . ?
C29A C30 C43 119.23(13) . 2_566 ?
C31 C30 C43 138.13(13) . 2_566 ?
C31 C30 C29B 141.3(4) . 2_566 ?
C43 C30 C29B 80.5(4) 2_566 2_566 ?
C32 C31 C30 132.41(14) . . ?
C32 C31 C36 118.44(14) . . ?
C30 C31 C36 109.14(13) . . ?
C33 C32 C31 121.05(16) . . ?
C32 C33 C34 120.54(16) . . ?
C35 C34 C33 120.54(16) . . ?
C34 C35 C36 120.87(15) . . ?
C35 C36 C37 132.87(14) . . ?
C35 C36 C31 118.54(14) . . ?
C37 C36 C31 108.58(13) . . ?
C29A C37 C36 103.00(13) . . ?
C29A C37 C38 119.19(13) . . ?
C36 C37 C38 137.79(13) . . ?
C36 C37 C29B 142.1(4) . . ?
C38 C37 C29B 80.1(4) . . ?
C39 C38 C37 123.11(14) . . ?
C39 C38 C43 117.68(14) . . ?
C37 C38 C43 119.21(13) . . ?
C39 C38 C29B 174.9(3) . . ?
C37 C38 C29B 51.9(3) . . ?
C43 C38 C29B 67.3(3) . . ?
C40 C39 C38 122.52(16) . . ?
C39 C40 C41 119.81(17) . . ?
C40 C41 C42 119.66(16) . . ?
C41 C42 C43 122.47(15) . . ?
C42 C43 C30 123.14(14) . 2_566 ?
C42 C43 C38 117.85(14) . . ?
C30 C43 C38 118.98(13) 2_566 . ?
C42 C43 C29B 173.9(3) . . ?
C30 C43 C29B 51.1(3) 2_566 . ?
C38 C43 C29B 67.9(3) . . ?
O3 K1 O2 62.78(4) . . ?
O3 K1 O8 146.81(3) . . ?
O2 K1 O8 150.27(3) . . ?
O3 K1 O7 151.63(3) . . ?
O2 K1 O7 88.86(3) . . ?
O8 K1 O7 61.54(3) . . ?
O3 K1 O9 88.65(4) . . ?
O2 K1 O9 139.41(3) . . ?
O8 K1 O9 61.83(4) . . ?
O7 K1 O9 116.04(4) . . ?
O3 K1 O4 61.70(3) . . ?
O2 K1 O4 117.67(3) . . ?
O8 K1 O4 89.71(3) . . ?
O7 K1 O4 140.80(3) . . ?
O9 K1 O4 62.74(3) . . ?
O3 K1 O5 90.43(4) . . ?
O2 K1 O5 99.73(4) . . ?
O8 K1 O5 85.95(4) . . ?
O7 K1 O5 93.92(3) . . ?
O9 K1 O5 109.23(3) . . ?
O4 K1 O5 55.56(3) . . ?
O3 K1 O1 91.47(4) . . ?
O2 K1 O1 56.55(3) . . ?
O8 K1 O1 110.70(4) . . ?
O7 K1 O1 70.50(4) . . ?
O9 K1 O1 159.25(3) . . ?
O4 K1 O1 99.27(3) . . ?
O5 K1 O1 50.02(3) . . ?
O3 K1 O6 109.50(3) . . ?
O2 K1 O6 68.69(4) . . ?
O8 K1 O6 90.54(3) . . ?
O7 K1 O6 56.01(3) . . ?
O9 K1 O6 98.02(3) . . ?
O4 K1 O6 157.70(3) . . ?
O5 K1 O6 146.66(3) . . ?
O1 K1 O6 101.48(3) . . ?
O3 K1 O10 84.12(4) . . ?
O2 K1 O10 91.30(4) . . ?
O8 K1 O10 90.31(4) . . ?
O7 K1 O10 98.10(3) . . ?
O9 K1 O10 55.59(3) . . ?
O4 K1 O10 108.79(3) . . ?
O5 K1 O10 163.85(3) . . ?
O1 K1 O10 145.02(3) . . ?
O6 K1 O10 48.91(3) . . ?
O3 K1 C3 42.46(4) . . ?
O2 K1 C3 22.43(3) . . ?
O8 K1 C3 166.50(3) . . ?
O7 K1 C3 109.73(3) . . ?
O9 K1 C3 118.90(4) . . ?
O4 K1 C3 102.57(3) . . ?
O5 K1 C3 105.55(4) . . ?
O1 K1 C3 73.21(4) . . ?
O6 K1 C3 75.97(4) . . ?
O10 K1 C3 80.51(4) . . ?
O3 K1 C20 105.25(4) . . ?
O2 K1 C20 162.11(3) . . ?
O8 K1 C20 42.30(4) . . ?
O7 K1 C20 102.47(4) . . ?
O9 K1 C20 22.70(3) . . ?
O4 K1 C20 60.79(4) . . ?
O5 K1 C20 93.34(4) . . ?
O1 K1 C20 140.31(3) . . ?
O6 K1 C20 106.12(4) . . ?
O10 K1 C20 73.59(4) . . ?
C3 K1 C20 141.00(4) . . ?
C14 O1 C1 117.48(10) . . ?
C14 O1 K1 103.87(7) . . ?
C1 O1 K1 107.55(7) . . ?
C2 O2 C3 112.58(10) . . ?
C2 O2 K1 124.74(7) . . ?
C3 O2 K1 109.85(7) . . ?
C4 O3 C5 111.53(11) . . ?
C4 O3 K1 115.58(8) . . ?
C5 O3 K1 118.46(8) . . ?
C7 O4 C6 113.68(11) . . ?
C7 O4 K1 121.85(8) . . ?
C6 O4 K1 105.84(8) . . ?
C9 O5 C8 118.54(10) . . ?
C9 O5 K1 105.24(7) . . ?
C8 O5 K1 113.79(8) . . ?
C28 O6 C15 118.22(10) . . ?
C28 O6 K1 103.00(8) . . ?
C15 O6 K1 108.70(8) . . ?
C17 O7 C16 112.02(11) . . ?
C17 O7 K1 109.62(8) . . ?
C16 O7 K1 124.54(8) . . ?
C18 O8 C19 112.00(11) . . ?
C18 O8 K1 116.47(8) . . ?
C19 O8 K1 117.35(8) . . ?
C20 O9 C21 113.58(11) . . ?
C20 O9 K1 106.87(8) . . ?
C21 O9 K1 123.67(8) . . ?
C23 O10 C22 118.77(11) . . ?
C23 O10 K1 103.13(8) . . ?
C22 O10 K1 109.49(8) . . ?
O11A C44A C45A 107.4(3) . . ?
C44A C45A C46A 100.7(3) . . ?
C47A C46A C45A 102.1(3) . . ?
O11A C47A C46A 106.8(3) . . ?
C47A O11A C44A 110.8(2) . . ?
O11B C44B C45B 96.1(17) . . ?
C46B C45B C44B 109.8(16) . . ?
C47B C46B C45B 101.1(18) . . ?
C46B C47B O11B 82.0(15) . . ?
C44B O11B C47B 105.2(18) . . ?

_refine_diff_density_max         0.886
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.075


#===END
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: tetrahydrofuran'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
