# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_chok1_ply
_database_code_depnum_ccdc_archive 'CCDC 1991245'
loop_
_audit_author_name
_audit_author_address
'Arpan Das'
;Senior Research Fellow
India
;
_audit_update_record             
;
2020-03-18 deposited with the CCDC.	2020-12-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT930_chok1_ply           
;
PROBLEM: FCF-based   Twin Law ( 0 0 1)[ 1 0 4] Est.d BASF       0.30 Check
RESPONSE: Due to the presence of 12 sp3 carbon atoms in 18-crown-6, the molecule is having some disorder with twinning which could not be refined further.
;
# Added during the CSD deposition process: Wednesday 18 March 2020 12:01 PM
# end Validation Reply Form

_audit_creation_date             2020-03-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C25 H31 K O8'
_chemical_formula_sum            'C25 H31 K O8'
_chemical_formula_weight         498.60
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O K'
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      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                   8.3399(4)
_cell_length_b                   27.1397(12)
_cell_length_c                   11.0226(5)
_cell_angle_alpha                90
_cell_angle_beta                 100.071(4)
_cell_angle_gamma                90
_cell_volume                     2456.4(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7126
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      66.2200
_cell_measurement_theta_min      3.2570
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.296
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16231
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        66.366
_diffrn_reflns_theta_max         66.366
_diffrn_reflns_theta_min         3.257
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -12.00 102.00   1.00    4.00    --   26.33  57.00  30.00  114
  2  ω    -50.00  64.00   1.00    4.00    --   26.33 -57.00 -90.00  114
  3  ω    -12.00 102.00   1.00    4.00    --   26.33  57.00 150.00  114
  4  ω     -9.00 104.00   1.00   18.00    --   67.17 -61.00  90.00  113
  5  ω     30.00 144.00   1.00   18.00    --   67.17  61.00 -30.00  114
  6  ω     20.00 147.00   1.00   18.00    --   67.17  45.00  60.00  127
  7  ω     57.00 150.00   1.00   18.00    --   67.17 178.00   0.00   93
  8  ω     82.00 146.00   1.00   18.00    --   67.17 146.00-142.00   64
  9  ω     29.00 145.00   1.00   22.00    --  108.00 -65.00 -30.00  116
 10  ω     65.00 178.00   1.00   22.00    --  108.00  77.00 -30.00  113
 11  ω     19.00 158.00   1.00   22.00    --  108.00 -89.00 -30.00  139
 12  ω    101.00 178.00   1.00   22.00    --  108.00 104.00 120.00   77
 13  ω     69.00 178.00   1.00   22.00    --  108.00  54.00  30.00  109
 14  ω     58.00 178.00   1.00   22.00    --  108.00  43.00-180.00  120
 15  ω     21.00 113.00   1.00   22.00    --  108.00-104.00 -30.00   92
 16  ω     21.00 113.00   1.00   22.00    --  108.00-104.00-120.00   92
 17  ω     71.00 178.00   1.00   22.00    --  108.00  65.00  60.00  107
 18  ω     86.00 178.00   1.00   22.00    --  108.00 138.00-150.00   92
 19  ω    101.00 178.00   1.00   22.00    --  108.00 104.00  60.00   77
 20  ω    101.00 178.00   1.00   22.00    --  108.00 104.00 -90.00   77
 21  ω     36.00 178.00   1.00   22.00    --  108.00  32.00 120.00  142
 22  ω     69.00 140.00   1.00   22.00    --  108.00  54.00  60.00   71
 23  ω     54.00 152.00   1.00   22.00    --  108.00 -47.00  74.81   98
 24  ω     82.00 119.00   1.00   22.00    --  108.00  54.00 -30.00   37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0144809000
_diffrn_orient_matrix_UB_12      -0.0555702000
_diffrn_orient_matrix_UB_13      0.0286592000
_diffrn_orient_matrix_UB_21      -0.0054106000
_diffrn_orient_matrix_UB_22      -0.0109384000
_diffrn_orient_matrix_UB_23      -0.1377811000
_diffrn_orient_matrix_UB_31      0.1869128000
_diffrn_orient_matrix_UB_32      0.0039916000
_diffrn_orient_matrix_UB_33      0.0187554000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3810
_reflns_number_total             4218
_reflns_odcompleteness_completeness 98.02
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.525
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4218
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1199
_refine_ls_R_factor_gt           0.1134
_refine_ls_restrained_S_all      1.046
_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)+(0.1679P)²+11.3134P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3001
_refine_ls_wR_factor_ref         0.3068
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O4-C19
 1.39 with sigma of 0.02
 O5-C17
 1.39 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O5) = Uanis(C17)
Uanis(C19) = Uanis(O4)
4.a Secondary CH2 refined with riding coordinates:
 C00U(H00A,H00B), C00V(H00C,H00D), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,
 H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B),
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12)
;
_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 0.48300(14) 0.57873(4) 0.76611(10) 0.0320(4) Uani 1 1 d . . . . .
O1 O 0.2385(4) 0.60011(14) 0.5856(3) 0.0353(9) Uani 1 1 d . . . . .
O2 O 0.5465(4) 0.63999(15) 0.5949(3) 0.0388(9) Uani 1 1 d . . . . .
O3 O 0.6084(6) 0.65670(16) 0.9338(4) 0.0489(11) Uani 1 1 d . . . . .
O4 O 0.8359(5) 0.6047(2) 0.8210(5) 0.0590(11) Uani 1 1 d D . . . .
O5 O 0.7206(7) 0.5233(3) 0.6715(5) 0.0845(18) Uani 1 1 d D . . . .
O6 O 0.4687(9) 0.4699(2) 0.7386(6) 0.092(2) Uani 1 1 d . . . . .
O7 O 0.2585(6) 0.5140(2) 0.8779(6) 0.0776(19) Uani 1 1 d . . . . .
O8 O 0.3654(6) 0.60169(19) 1.0010(4) 0.0550(12) Uani 1 1 d . . . . .
C00U C 0.2667(10) 0.4609(3) 0.8538(14) 0.104(5) Uani 1 1 d . . . . .
H00A H 0.1617 0.4458 0.8552 0.125 Uiso 1 1 calc R . . . .
H00B H 0.3466 0.4455 0.9168 0.125 Uiso 1 1 calc R . . . .
C00V C 0.2332(10) 0.5240(5) 0.9960(11) 0.105(5) Uani 1 1 d . . . . .
H00C H 0.3250 0.5124 1.0556 0.126 Uiso 1 1 calc R . . . .
H00D H 0.1359 0.5072 1.0113 0.126 Uiso 1 1 calc R . . . .
C1 C 0.1980(6) 0.62939(18) 0.4976(4) 0.0279(10) Uani 1 1 d . . . . .
C2 C 0.0285(6) 0.6302(2) 0.4359(5) 0.0326(11) Uani 1 1 d . . . . .
H2 H -0.0434 0.6074 0.4596 0.039 Uiso 1 1 calc R . . . .
C3 C -0.0282(6) 0.6626(2) 0.3458(5) 0.0316(11) Uani 1 1 d . . . . .
H3 H -0.1382 0.6622 0.3111 0.038 Uiso 1 1 calc R . . . .
C4 C 0.0768(6) 0.69745(19) 0.3026(5) 0.0298(11) Uani 1 1 d . . . . .
C5 C 0.0179(7) 0.7316(2) 0.2104(5) 0.0387(13) Uani 1 1 d . . . . .
H5 H -0.0927 0.7320 0.1778 0.046 Uiso 1 1 calc R . . . .
C6 C 0.1196(8) 0.7644(2) 0.1671(6) 0.0453(14) Uani 1 1 d . . . . .
H6 H 0.0777 0.7875 0.1076 0.054 Uiso 1 1 calc R . . . .
C7 C 0.2845(8) 0.7629(2) 0.2125(5) 0.0413(13) Uani 1 1 d . . . . .
H7 H 0.3535 0.7848 0.1819 0.050 Uiso 1 1 calc R . . . .
C8 C 0.3497(7) 0.72913(18) 0.3038(5) 0.0316(11) Uani 1 1 d . . . . .
C9 C 0.2449(6) 0.69582(17) 0.3528(4) 0.0251(10) Uani 1 1 d . . . . .
C10 C 0.3082(6) 0.66295(17) 0.4508(4) 0.0260(10) Uani 1 1 d . . . . .
C11 C 0.5211(7) 0.7267(2) 0.3497(5) 0.0339(12) Uani 1 1 d . . . . .
H11 H 0.5915 0.7465 0.3145 0.041 Uiso 1 1 calc R . . . .
C12 C 0.5825(6) 0.6964(2) 0.4426(5) 0.0313(11) Uani 1 1 d . . . . .
H12 H 0.6946 0.6958 0.4697 0.038 Uiso 1 1 calc R . . . .
C13 C 0.4796(6) 0.66417(18) 0.5026(5) 0.0290(10) Uani 1 1 d . . . . .
C14 C 0.3133(17) 0.4539(4) 0.7304(16) 0.131(6) Uani 1 1 d . . . . .
H14A H 0.3055 0.4194 0.7073 0.157 Uiso 1 1 calc R . . . .
H14B H 0.2414 0.4727 0.6686 0.157 Uiso 1 1 calc R . . . .
C15 C 0.5384(19) 0.4584(4) 0.6318(10) 0.116(5) Uani 1 1 d . . . . .
H15A H 0.4759 0.4747 0.5606 0.140 Uiso 1 1 calc R . . . .
H15B H 0.5311 0.4232 0.6172 0.140 Uiso 1 1 calc R . . . .
C16 C 0.7120(16) 0.4740(4) 0.6456(9) 0.107(5) Uani 1 1 d . . . . .
H16A H 0.7778 0.4556 0.7118 0.128 Uiso 1 1 calc R . . . .
H16B H 0.7530 0.4675 0.5700 0.128 Uiso 1 1 calc R . . . .
C17 C 0.8866(11) 0.5401(4) 0.6930(7) 0.0845(18) Uani 1 1 d D . . . .
H17A H 0.9364 0.5319 0.6224 0.101 Uiso 1 1 calc R . . . .
H17B H 0.9467 0.5232 0.7643 0.101 Uiso 1 1 calc R . . . .
C18 C 0.8972(9) 0.5931(4) 0.7137(8) 0.081(3) Uani 1 1 d . . . . .
H18A H 1.0098 0.6036 0.7225 0.097 Uiso 1 1 calc R . . . .
H18B H 0.8349 0.6102 0.6438 0.097 Uiso 1 1 calc R . . . .
C19 C 0.8405(8) 0.6565(3) 0.8412(7) 0.0590(11) Uani 1 1 d D . . . .
H19A H 0.7752 0.6730 0.7714 0.071 Uiso 1 1 calc R . . . .
H19B H 0.9516 0.6683 0.8487 0.071 Uiso 1 1 calc R . . . .
C20 C 0.7770(9) 0.6683(3) 0.9543(7) 0.062(2) Uani 1 1 d . . . . .
H20A H 0.8341 0.6491 1.0228 0.074 Uiso 1 1 calc R . . . .
H20B H 0.7929 0.7029 0.9739 0.074 Uiso 1 1 calc R . . . .
C21 C 0.5336(12) 0.6690(2) 1.0376(6) 0.065(2) Uani 1 1 d . . . . .
H21A H 0.5385 0.7043 1.0510 0.079 Uiso 1 1 calc R . . . .
H21B H 0.5917 0.6530 1.1111 0.079 Uiso 1 1 calc R . . . .
C22 C 0.3626(11) 0.6526(3) 1.0140(7) 0.066(2) Uani 1 1 d . . . . .
H22A H 0.3091 0.6616 1.0822 0.080 Uiso 1 1 calc R . . . .
H22B H 0.3042 0.6677 0.9395 0.080 Uiso 1 1 calc R . . . .
C23 C 0.2143(9) 0.5779(4) 1.0083(8) 0.081(3) Uani 1 1 d . . . . .
H23A H 0.1299 0.5899 0.9431 0.097 Uiso 1 1 calc R . . . .
H23B H 0.1822 0.5854 1.0867 0.097 Uiso 1 1 calc R . . . .


_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 O1 2.652(4) . ?
K1 O2 2.637(4) . ?
K1 O3 2.883(4) . ?
K1 O4 2.984(5) . ?
K1 O5 2.829(5) . ?
K1 O6 2.970(5) . ?
K1 O7 2.985(6) . ?
K1 O8 2.991(5) . ?
O1 C1 1.254(6) . ?
O2 C13 1.256(6) . ?
O3 C20 1.420(9) . ?
O3 C21 1.435(9) . ?
O4 C18 1.403(9) . ?
O4 C19 1.425(9) . ?
O5 C16 1.367(13) . ?
O5 C17 1.437(11) . ?
O6 C14 1.354(16) . ?
O6 C15 1.434(15) . ?
O7 C00U 1.470(12) . ?
O7 C00V 1.381(14) . ?
O8 C22 1.390(10) . ?
O8 C23 1.431(10) . ?
C00U H00A 0.9700 . ?
C00U H00B 0.9700 . ?
C00U C14 1.49(2) . ?
C00V H00C 0.9700 . ?
C00V H00D 0.9700 . ?
C00V C23 1.481(16) . ?
C1 C2 1.458(7) . ?
C1 C10 1.451(7) . ?
C2 H2 0.9300 . ?
C2 C3 1.349(8) . ?
C3 H3 0.9300 . ?
C3 C4 1.426(8) . ?
C4 C5 1.398(8) . ?
C4 C9 1.415(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.372(9) . ?
C6 H6 0.9300 . ?
C6 C7 1.379(9) . ?
C7 H7 0.9300 . ?
C7 C8 1.400(8) . ?
C8 C9 1.427(7) . ?
C8 C11 1.433(8) . ?
C9 C10 1.429(7) . ?
C10 C13 1.444(7) . ?
C11 H11 0.9300 . ?
C11 C12 1.343(8) . ?
C12 H12 0.9300 . ?
C12 C13 1.461(7) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.491(19) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.456(15) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.472(11) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.474(13) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?

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 K1 O3 117.73(13) . . ?
O1 K1 O4 134.60(12) . . ?
O1 K1 O5 109.64(14) . . ?
O1 K1 O6 97.41(14) . . ?
O1 K1 O7 89.02(13) . . ?
O1 K1 O8 106.16(12) . . ?
O2 K1 O1 63.23(11) . . ?
O2 K1 O3 84.27(13) . . ?
O2 K1 O4 71.45(12) . . ?
O2 K1 O5 80.24(17) . . ?
O2 K1 O6 124.29(19) . . ?
O2 K1 O7 152.25(13) . . ?
O2 K1 O8 128.71(14) . . ?
O3 K1 O4 57.49(15) . . ?
O3 K1 O6 143.06(14) . . ?
O3 K1 O7 110.51(17) . . ?
O3 K1 O8 55.19(14) . . ?
O4 K1 O7 136.28(13) . . ?
O4 K1 O8 103.69(15) . . ?
O5 K1 O3 115.35(18) . . ?
O5 K1 O4 58.03(19) . . ?
O5 K1 O6 56.7(2) . . ?
O5 K1 O7 111.7(2) . . ?
O5 K1 O8 141.91(14) . . ?
O6 K1 O4 106.02(18) . . ?
O6 K1 O7 56.0(2) . . ?
O6 K1 O8 106.4(2) . . ?
O7 K1 O8 56.00(18) . . ?
C1 O1 K1 141.9(3) . . ?
C13 O2 K1 142.4(3) . . ?
C20 O3 K1 120.2(4) . . ?
C20 O3 C21 112.2(6) . . ?
C21 O3 K1 121.5(4) . . ?
C18 O4 K1 105.6(5) . . ?
C18 O4 C19 110.5(6) . . ?
C19 O4 K1 105.2(3) . . ?
C16 O5 K1 125.7(7) . . ?
C16 O5 C17 111.0(8) . . ?
C17 O5 K1 119.1(5) . . ?
C14 O6 K1 110.2(6) . . ?
C14 O6 C15 113.4(10) . . ?
C15 O6 K1 106.6(6) . . ?
C00U O7 K1 116.7(6) . . ?
C00V O7 K1 119.0(5) . . ?
C00V O7 C00U 112.4(8) . . ?
C22 O8 K1 108.1(4) . . ?
C22 O8 C23 114.3(6) . . ?
C23 O8 K1 112.3(5) . . ?
O7 C00U H00A 110.0 . . ?
O7 C00U H00B 110.0 . . ?
O7 C00U C14 108.5(7) . . ?
H00A C00U H00B 108.4 . . ?
C14 C00U H00A 110.0 . . ?
C14 C00U H00B 110.0 . . ?
O7 C00V H00C 110.0 . . ?
O7 C00V H00D 110.0 . . ?
O7 C00V C23 108.4(6) . . ?
H00C C00V H00D 108.4 . . ?
C23 C00V H00C 110.0 . . ?
C23 C00V H00D 110.0 . . ?
O1 C1 C2 118.6(4) . . ?
O1 C1 C10 124.8(5) . . ?
C10 C1 C2 116.6(4) . . ?
C1 C2 H2 118.7 . . ?
C3 C2 C1 122.7(5) . . ?
C3 C2 H2 118.7 . . ?
C2 C3 H3 119.3 . . ?
C2 C3 C4 121.4(5) . . ?
C4 C3 H3 119.3 . . ?
C5 C4 C3 121.6(5) . . ?
C5 C4 C9 120.2(5) . . ?
C9 C4 C3 118.2(5) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 C4 121.5(5) . . ?
C6 C5 H5 119.2 . . ?
C5 C6 H6 120.2 . . ?
C5 C6 C7 119.6(5) . . ?
C7 C6 H6 120.2 . . ?
C6 C7 H7 119.5 . . ?
C6 C7 C8 121.1(5) . . ?
C8 C7 H7 119.5 . . ?
C7 C8 C9 120.0(5) . . ?
C7 C8 C11 121.5(5) . . ?
C9 C8 C11 118.4(5) . . ?
C4 C9 C8 117.6(4) . . ?
C4 C9 C10 121.7(4) . . ?
C8 C9 C10 120.8(5) . . ?
C9 C10 C1 119.2(4) . . ?
C9 C10 C13 119.6(4) . . ?
C13 C10 C1 121.2(4) . . ?
C8 C11 H11 119.3 . . ?
C12 C11 C8 121.4(5) . . ?
C12 C11 H11 119.3 . . ?
C11 C12 H12 118.8 . . ?
C11 C12 C13 122.4(5) . . ?
C13 C12 H12 118.8 . . ?
O2 C13 C10 125.2(5) . . ?
O2 C13 C12 117.8(5) . . ?
C10 C13 C12 117.0(4) . . ?
O6 C14 C00U 107.4(9) . . ?
O6 C14 H14A 110.2 . . ?
O6 C14 H14B 110.2 . . ?
C00U C14 H14A 110.2 . . ?
C00U C14 H14B 110.2 . . ?
H14A C14 H14B 108.5 . . ?
O6 C15 H15A 109.1 . . ?
O6 C15 H15B 109.1 . . ?
O6 C15 C16 112.4(7) . . ?
H15A C15 H15B 107.9 . . ?
C16 C15 H15A 109.1 . . ?
C16 C15 H15B 109.1 . . ?
O5 C16 C15 108.2(8) . . ?
O5 C16 H16A 110.1 . . ?
O5 C16 H16B 110.1 . . ?
C15 C16 H16A 110.1 . . ?
C15 C16 H16B 110.1 . . ?
H16A C16 H16B 108.4 . . ?
O5 C17 H17A 109.3 . . ?
O5 C17 H17B 109.3 . . ?
O5 C17 C18 111.7(6) . . ?
H17A C17 H17B 107.9 . . ?
C18 C17 H17A 109.3 . . ?
C18 C17 H17B 109.3 . . ?
O4 C18 C17 109.4(7) . . ?
O4 C18 H18A 109.8 . . ?
O4 C18 H18B 109.8 . . ?
C17 C18 H18A 109.8 . . ?
C17 C18 H18B 109.8 . . ?
H18A C18 H18B 108.2 . . ?
O4 C19 H19A 109.7 . . ?
O4 C19 H19B 109.7 . . ?
O4 C19 C20 110.0(6) . . ?
H19A C19 H19B 108.2 . . ?
C20 C19 H19A 109.7 . . ?
C20 C19 H19B 109.7 . . ?
O3 C20 C19 108.1(6) . . ?
O3 C20 H20A 110.1 . . ?
O3 C20 H20B 110.1 . . ?
C19 C20 H20A 110.1 . . ?
C19 C20 H20B 110.1 . . ?
H20A C20 H20B 108.4 . . ?
O3 C21 H21A 109.8 . . ?
O3 C21 H21B 109.8 . . ?
O3 C21 C22 109.3(6) . . ?
H21A C21 H21B 108.3 . . ?
C22 C21 H21A 109.8 . . ?
C22 C21 H21B 109.8 . . ?
O8 C22 C21 106.5(6) . . ?
O8 C22 H22A 110.4 . . ?
O8 C22 H22B 110.4 . . ?
C21 C22 H22A 110.4 . . ?
C21 C22 H22B 110.4 . . ?
H22A C22 H22B 108.6 . . ?
O8 C23 C00V 109.4(6) . . ?
O8 C23 H23A 109.8 . . ?
O8 C23 H23B 109.8 . . ?
C00V C23 H23A 109.8 . . ?
C00V C23 H23B 109.8 . . ?
H23A C23 H23B 108.2 . . ?

_olex2_date_sample_data_collection 2020-01-25
_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 1.579
_oxdiff_exptl_absorpt_empirical_full_min 0.612
####################################################################### 
# 
# 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_jasi_noply
_database_code_depnum_ccdc_archive 'CCDC 2015680'
loop_
_audit_author_name
_audit_author_address
'Arpan Das'
;SRF, Indian Institute of Science Education and Research Kolkata
India
;
_audit_update_record             
;
2020-07-11 deposited with the CCDC.	2020-12-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT340_jasi_noply          
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0128 Ang.
RESPONSE: Due to the poor crystalline quality and because of presence of 12 sp3 carbon atoms in 18-crown-6, the molecule is having some disorders in the crown ether ring. Moreover, The X-ray data quality is poor resulting in low bond precision accuracy.
;
# Added during the CSD deposition process: Saturday 11 July 2020 02:32 PM
# end Validation Reply Form

_audit_creation_date             2020-07-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C26 H34 K N O7, C26 H31 K N O7, 2(C7 H8)'
_chemical_formula_sum            'C66 H81 K2 N2 O14'
_chemical_formula_weight         1204.52
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N O K'
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'
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/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                   14.2195(10)
_cell_length_b                   34.5380(19)
_cell_length_c                   13.8905(9)
_cell_angle_alpha                90
_cell_angle_beta                 113.176(8)
_cell_angle_gamma                90
_cell_volume                     6271.3(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6603
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      66.2200
_cell_measurement_theta_min      2.5930
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.874
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2564
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0885
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            39527
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        66.682
_diffrn_reflns_theta_max         66.682
_diffrn_reflns_theta_min         3.381
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9160
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -12.00 102.00   1.00    4.45    --   26.27  57.00-180.00  114
  2  ω     57.00 121.00   1.00    4.45    --   26.27 178.00 150.00   64
  3  ω    -12.00 102.00   1.00    4.45    --   26.27  57.00 -60.00  114
  4  ω     -9.00 104.00   1.00   15.79    --   67.13 -61.00 -90.00  113
  5  ω     25.00 151.00   1.00   15.79    --   67.13  75.00-131.23  126
  6  ω     -4.00 108.00   1.00   15.79    --   67.13 -94.00 -60.00  112
  7  ω    100.00 153.00   1.00   15.79    --   67.13 111.00-180.00   53
  8  ω    100.00 153.00   1.00   15.79    --   67.13 111.00 -60.00   53
  9  ω    100.00 153.00   1.00   15.79    --   67.13 111.00-120.00   53
 10  ω     29.00 145.00   1.00   25.79    --  108.00 -65.00 120.00  116
 11  ω     23.00 151.00   1.00   25.79    --  108.00 -77.00  60.00  128
 12  ω     28.00 158.00   1.00   25.79    --  108.00 -43.00 120.00  130
 13  ω     21.00 178.00   1.00   25.79    --  108.00 -21.00 -90.00  157
 14  ω     19.00 178.00   1.00   25.79    --  108.00 -11.00 120.00  159
 15  ω    101.00 178.00   1.00   25.79    --  108.00 104.00 120.00   77
 16  ω     58.00 178.00   1.00   25.79    --  108.00  43.00-120.00  120
 17  ω     25.00 145.00   1.00   25.79    --  108.00 -72.00 -32.83  120
 18  ω     58.00  92.00   1.00   25.79    --  108.00-104.00 -90.00   34
 19  ω     62.00 111.00   1.00   25.79    --  108.00-104.00 150.00   49
 20  ω     59.00 109.00   1.00   25.79    --  108.00-104.00-150.00   50
 21  ω    153.00 178.00   1.00   25.79    --  108.00  21.00   0.00   25
 22  ω     37.00 138.00   1.00   25.79    --  108.00  32.00   0.00  101
 23  ω    121.00 156.00   1.00   25.79    --  108.00  32.00-150.00   35
 24  ω     79.00 109.00   1.00   25.79    --  108.00  32.00-150.00   30
 25  ω     61.00 118.00   1.00   25.79    --  108.00  21.00   0.00   57
 26  ω     62.00  88.00   1.00   25.79    --  108.00-104.00 -60.00   26
 27  ω    115.00 157.00   1.00   25.79    --  108.00 138.00  90.00   42
 28  ω     22.00  48.00   1.00   25.79    --  108.00-104.00 150.00   26
 29  ω     56.00  99.00   1.00   25.79    --  108.00-104.00 120.00   43
 30  ω    132.00 159.00   1.00   25.79    --  108.00  65.00 150.00   27
 31  ω     70.00 105.00   1.00   25.79    --  108.00 -43.00 -90.00   35
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0525085000
_diffrn_orient_matrix_UB_12      -0.0380197000
_diffrn_orient_matrix_UB_13      0.0510841000
_diffrn_orient_matrix_UB_21      -0.0711661000
_diffrn_orient_matrix_UB_22      -0.0028338000
_diffrn_orient_matrix_UB_23      0.0596634000
_diffrn_orient_matrix_UB_31      -0.0779285000
_diffrn_orient_matrix_UB_32      -0.0230673000
_diffrn_orient_matrix_UB_33      -0.0915637000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7595
_reflns_number_total             10947
_reflns_odcompleteness_completeness 97.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         10947
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1510
_refine_ls_R_factor_gt           0.1198
_refine_ls_restrained_S_all      1.053
_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)+(0.1682P)²+14.5694P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3097
_refine_ls_wR_factor_ref         0.3471
_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. Uiso/Uaniso restraints and constraints
Uanis(C32) = Uanis(C31) = Uanis(C33) = Uanis(C27) = Uanis(C28) = Uanis(C29) =
Uanis(C30)
Uanis(C49) = Uanis(C50) = Uanis(C51) = Uanis(C48)
Uanis(C1) = Uanis(C12)
3. Others
 Fixed Sof: O14(0.5) O15(0.5)
4.a Ternary CH refined with riding coordinates:
 C16(H16A), C49(H49), C50(H50)
4.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,
 H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B),
 C25(H25A,H25B), C26(H26A,H26B), C47(H47A,H47B), C48(H48A,H48B), C51(H51A,H51B),
  C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,
 H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C35(H35), C36(H36),
 C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C27(H27), C28(H28), C29(H29),
  C30(H30), C33(H33), C60(H60), C61(H61), C62(H62), C65(H65), C66(H66)
4.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C32(H32A,H32B,H32C), C64(H64A,H64B,H64C)
;
_atom_sites_solution_hydrogens   mixed
_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 0.68455(10) 0.28571(4) 0.55882(9) 0.0531(3) Uani 1 1 d . . . . .
O1 O 0.6101(4) 0.21548(15) 0.5438(4) 0.0747(13) Uani 1 1 d . . . . .
O2 O 0.6472(4) 0.27378(14) 0.3495(3) 0.0692(12) Uani 1 1 d . . . . .
O3 O 0.4760(3) 0.28887(12) 0.3969(3) 0.0561(10) Uani 1 1 d . . . . .
O4 O 0.5144(3) 0.30489(12) 0.6101(3) 0.0548(10) Uani 1 1 d . . . . .
O5 O 0.6968(3) 0.33918(12) 0.7320(3) 0.0551(10) Uani 1 1 d . . . . .
O6 O 0.8672(3) 0.33346(13) 0.6794(4) 0.0635(11) Uani 1 1 d . . . . .
O7 O 0.8249(4) 0.31272(15) 0.4719(4) 0.0750(13) Uani 1 1 d . . . . .
N1 N 0.8210(5) 0.21935(18) 0.6275(5) 0.0707(15) Uani 1 1 d . . . . .
C1 C 0.6210(6) 0.1794(2) 0.5380(5) 0.0678(12) Uani 1 1 d . . . . .
C2 C 0.5347(7) 0.1553(3) 0.4975(7) 0.086(2) Uani 1 1 d . . . . .
H2 H 0.4708 0.1669 0.4776 0.104 Uiso 1 1 calc R . . . .
C3 C 0.5370(7) 0.1177(3) 0.4855(8) 0.091(2) Uani 1 1 d . . . . .
H3 H 0.4761 0.1040 0.4556 0.109 Uiso 1 1 calc R . . . .
C4 C 0.6299(6) 0.0983(2) 0.5172(5) 0.0673(17) Uani 1 1 d . . . . .
C5 C 0.6317(8) 0.0562(3) 0.5060(6) 0.093(3) Uani 1 1 d . . . . .
H5 H 0.5718 0.0417 0.4799 0.112 Uiso 1 1 calc R . . . .
C6 C 0.7300(8) 0.0384(2) 0.5372(6) 0.076(2) Uani 1 1 d . . . . .
H6 H 0.7344 0.0117 0.5330 0.092 Uiso 1 1 calc R . . . .
C7 C 0.8145(8) 0.0592(3) 0.5718(6) 0.091(3) Uani 1 1 d . . . . .
H7 H 0.8769 0.0465 0.5904 0.109 Uiso 1 1 calc R . . . .
C8 C 0.8146(7) 0.0977(3) 0.5814(6) 0.081(2) Uani 1 1 d . . . . .
C9 C 0.9110(6) 0.1202(3) 0.6220(8) 0.095(3) Uani 1 1 d . . . . .
H9 H 0.9735 0.1079 0.6382 0.114 Uiso 1 1 calc R . . . .
C10 C 0.9072(7) 0.1586(3) 0.6352(8) 0.092(3) Uani 1 1 d . . . . .
H10 H 0.9697 0.1714 0.6625 0.111 Uiso 1 1 calc R . . . .
C11 C 0.8170(6) 0.1821(2) 0.6117(5) 0.0694(18) Uani 1 1 d . . . . .
C12 C 0.7219(6) 0.1608(2) 0.5676(5) 0.0678(12) Uani 1 1 d . . . . .
C13 C 0.7240(5) 0.1181(2) 0.5540(4) 0.0573(15) Uani 1 1 d . . . . .
C14 C 0.9224(6) 0.2362(3) 0.6798(7) 0.085(2) Uani 1 1 d . . . . .
H14A H 0.9609 0.2325 0.6372 0.127 Uiso 1 1 calc GR . . . .
H14B H 0.9570 0.2238 0.7463 0.127 Uiso 1 1 calc GR . . . .
H14C H 0.9161 0.2634 0.6904 0.127 Uiso 1 1 calc GR . . . .
C15 C 0.7227(7) 0.2836(3) 0.3105(6) 0.084(2) Uani 1 1 d . . . . .
H15A H 0.7087 0.3091 0.2785 0.101 Uiso 1 1 calc R . . . .
H15B H 0.7219 0.2650 0.2579 0.101 Uiso 1 1 calc R . . . .
C16 C 0.8241(8) 0.2834(3) 0.3992(7) 0.095(3) Uani 1 1 d . . . . .
H16A H 0.8806 0.2657 0.4073 0.114 Uiso 1 1 calc R . . . .
H16B H 0.871(8) 0.296(3) 0.365(8) 0.114 Uiso 1 1 d R . . . .
C17 C 0.9233(6) 0.3235(3) 0.5392(8) 0.089(2) Uani 1 1 d . . . . .
H17A H 0.9586 0.3353 0.4995 0.107 Uiso 1 1 calc R . . . .
H17B H 0.9616 0.3008 0.5746 0.107 Uiso 1 1 calc R . . . .
C18 C 0.9165(6) 0.3520(3) 0.6188(7) 0.081(2) Uani 1 1 d . . . . .
H18A H 0.9845 0.3604 0.6646 0.098 Uiso 1 1 calc R . . . .
H18B H 0.8775 0.3745 0.5835 0.098 Uiso 1 1 calc R . . . .
C19 C 0.8626(5) 0.3591(2) 0.7576(5) 0.0660(17) Uani 1 1 d . . . . .
H19A H 0.8330 0.3837 0.7260 0.079 Uiso 1 1 calc R . . . .
H19B H 0.9309 0.3640 0.8095 0.079 Uiso 1 1 calc R . . . .
C20 C 0.7985(5) 0.34121(19) 0.8083(5) 0.0590(15) Uani 1 1 d . . . . .
H20A H 0.8236 0.3155 0.8334 0.071 Uiso 1 1 calc R . . . .
H20B H 0.8010 0.3568 0.8674 0.071 Uiso 1 1 calc R . . . .
C21 C 0.6251(5) 0.3283(2) 0.7768(5) 0.0626(16) Uani 1 1 d . . . . .
H21A H 0.6309 0.3456 0.8339 0.075 Uiso 1 1 calc R . . . .
H21B H 0.6385 0.3021 0.8039 0.075 Uiso 1 1 calc R . . . .
C22 C 0.5205(5) 0.3310(2) 0.6920(5) 0.0638(16) Uani 1 1 d . . . . .
H22A H 0.4696 0.3242 0.7195 0.077 Uiso 1 1 calc R . . . .
H22B H 0.5074 0.3572 0.6652 0.077 Uiso 1 1 calc R . . . .
C23 C 0.4144(5) 0.3055(2) 0.5285(5) 0.0643(17) Uani 1 1 d . . . . .
H23A H 0.3994 0.3312 0.4978 0.077 Uiso 1 1 calc R . . . .
H23B H 0.3638 0.2991 0.5565 0.077 Uiso 1 1 calc R . . . .
C24 C 0.4109(5) 0.2766(2) 0.4469(5) 0.0657(17) Uani 1 1 d . . . . .
H24A H 0.4331 0.2515 0.4793 0.079 Uiso 1 1 calc R . . . .
H24B H 0.3413 0.2741 0.3955 0.079 Uiso 1 1 calc R . . . .
C25 C 0.4746(6) 0.2622(2) 0.3176(5) 0.0704(19) Uani 1 1 d . . . . .
H25A H 0.4061 0.2605 0.2637 0.085 Uiso 1 1 calc R . . . .
H25B H 0.4949 0.2367 0.3478 0.085 Uiso 1 1 calc R . . . .
C26 C 0.5468(6) 0.2761(2) 0.2714(5) 0.073(2) Uani 1 1 d . . . . .
H26A H 0.5410 0.2601 0.2118 0.087 Uiso 1 1 calc R . . . .
H26B H 0.5309 0.3026 0.2475 0.087 Uiso 1 1 calc R . . . .
K2 K 0.25203(9) 0.53140(4) 0.46988(10) 0.0565(4) Uani 1 1 d . . . . .
O8 O 0.2146(4) 0.45957(14) 0.4120(3) 0.0643(11) Uani 1 1 d . . . . .
O9 O 0.2396(3) 0.54179(13) 0.2639(3) 0.0602(11) Uani 1 1 d . . . . .
O10 O 0.0508(3) 0.53812(13) 0.2795(4) 0.0620(11) Uani 1 1 d . . . . .
O11 O 0.0589(3) 0.54620(15) 0.4842(4) 0.0738(13) Uani 1 1 d . . . . .
O12 O 0.2254(4) 0.58878(15) 0.6132(4) 0.0732(13) Uani 1 1 d . . . . .
O13 O 0.4183(4) 0.58364(16) 0.6033(4) 0.0812(15) Uani 1 1 d . . . . .
O14 O 0.4139(6) 0.5677(5) 0.4182(7) 0.083(4) Uani 0.5 1 d . . P . .
O15 O 0.4318(7) 0.5403(2) 0.4116(7) 0.050(2) Uani 0.5 1 d . . P . .
N2 N 0.3126(4) 0.47247(15) 0.6252(4) 0.0565(12) Uani 1 1 d . . . . .
C34 C 0.2081(5) 0.4252(2) 0.4381(5) 0.0582(15) Uani 1 1 d . . . . .
C35 C 0.1618(6) 0.3971(3) 0.3564(6) 0.078(2) Uani 1 1 d . . . . .
H35 H 0.1441 0.4052 0.2876 0.094 Uiso 1 1 calc R . . . .
C36 C 0.1425(6) 0.3605(3) 0.3722(6) 0.083(2) Uani 1 1 d . . . . .
H36 H 0.1104 0.3443 0.3152 0.099 Uiso 1 1 calc R . . . .
C37 C 0.1706(5) 0.3459(2) 0.4758(6) 0.0668(17) Uani 1 1 d . . . . .
C38 C 0.1539(6) 0.3074(2) 0.4950(7) 0.077(2) Uani 1 1 d . . . . .
H38 H 0.1222 0.2911 0.4382 0.093 Uiso 1 1 calc R . . . .
C39 C 0.1820(6) 0.2926(2) 0.5938(8) 0.079(2) Uani 1 1 d . . . . .
H39 H 0.1690 0.2669 0.6046 0.095 Uiso 1 1 calc R . . . .
C40 C 0.2306(6) 0.3173(2) 0.6766(7) 0.077(2) Uani 1 1 d . . . . .
H40 H 0.2518 0.3078 0.7445 0.092 Uiso 1 1 calc R . . . .
C41 C 0.2488(5) 0.3557(2) 0.6625(6) 0.0652(17) Uani 1 1 d . . . . .
C42 C 0.2992(7) 0.3805(2) 0.7486(6) 0.082(2) Uani 1 1 d . . . . .
H42 H 0.3187 0.3708 0.8161 0.098 Uiso 1 1 calc R . . . .
C43 C 0.3199(7) 0.4178(2) 0.7354(5) 0.077(2) Uani 1 1 d . . . . .
H43 H 0.3534 0.4326 0.7952 0.092 Uiso 1 1 calc R . . . .
C44 C 0.2934(5) 0.4364(2) 0.6350(5) 0.0562(14) Uani 1 1 d . . . . .
C45 C 0.2401(4) 0.41085(18) 0.5451(5) 0.0531(14) Uani 1 1 d . . . . .
C46 C 0.2206(4) 0.37189(19) 0.5603(5) 0.0551(14) Uani 1 1 d . . . . .
C47 C 0.3697(5) 0.4943(2) 0.7211(5) 0.0659(17) Uani 1 1 d . . . . .
H47A H 0.4437 0.4923 0.7515 0.079 Uiso 1 1 calc R . . . .
H47B H 0.3377 0.4987 0.7702 0.079 Uiso 1 1 calc R . . . .
C48 C 0.3209(6) 0.5540(3) 0.2386(6) 0.0992(16) Uani 1 1 d . . . . .
H48A H 0.2997 0.5761 0.1917 0.119 Uiso 1 1 calc R . . . .
H48B H 0.3403 0.5333 0.2028 0.119 Uiso 1 1 calc R . . . .
C49 C 0.4081(6) 0.5647(3) 0.3328(6) 0.0992(16) Uani 1 1 d . . . . .
H49 H 0.4667 0.5750 0.3207 0.119 Uiso 1 1 calc R . . . .
C50 C 0.5139(6) 0.5593(3) 0.5073(6) 0.0992(16) Uani 1 1 d . . . . .
H50 H 0.5661 0.5681 0.4827 0.119 Uiso 1 1 calc R . . . .
C51 C 0.4976(6) 0.5930(3) 0.5665(6) 0.0992(16) Uani 1 1 d . . . . .
H51A H 0.5607 0.5989 0.6255 0.119 Uiso 1 1 calc R . . . .
H51B H 0.4778 0.6155 0.5214 0.119 Uiso 1 1 calc R . . . .
C52 C 0.3911(9) 0.6153(2) 0.6556(8) 0.106(3) Uani 1 1 d . . . . .
H52A H 0.3610 0.6362 0.6064 0.127 Uiso 1 1 calc R . . . .
H52B H 0.4518 0.6251 0.7120 0.127 Uiso 1 1 calc R . . . .
C53 C 0.3159(8) 0.6008(3) 0.6987(6) 0.095(3) Uani 1 1 d . . . . .
H53A H 0.3450 0.5793 0.7457 0.114 Uiso 1 1 calc R . . . .
H53B H 0.2997 0.6213 0.7376 0.114 Uiso 1 1 calc R . . . .
C54 C 0.1491(8) 0.5758(3) 0.6483(7) 0.091(3) Uani 1 1 d . . . . .
H54A H 0.1434 0.5939 0.6992 0.109 Uiso 1 1 calc R . . . .
H54B H 0.1680 0.5507 0.6818 0.109 Uiso 1 1 calc R . . . .
C55 C 0.0492(7) 0.5729(3) 0.5570(7) 0.087(3) Uani 1 1 d . . . . .
H55A H -0.0034 0.5642 0.5800 0.104 Uiso 1 1 calc R . . . .
H55B H 0.0295 0.5980 0.5242 0.104 Uiso 1 1 calc R . . . .
C56 C -0.0351(5) 0.5423(3) 0.3946(7) 0.080(2) Uani 1 1 d . . . . .
H56A H -0.0602 0.5676 0.3655 0.096 Uiso 1 1 calc R . . . .
H56B H -0.0863 0.5301 0.4145 0.096 Uiso 1 1 calc R . . . .
C57 C -0.0164(5) 0.5184(2) 0.3165(7) 0.079(2) Uani 1 1 d . . . . .
H57A H 0.0137 0.4939 0.3476 0.095 Uiso 1 1 calc R . . . .
H57B H -0.0807 0.5131 0.2583 0.095 Uiso 1 1 calc R . . . .
C58 C 0.0725(5) 0.5156(2) 0.2041(6) 0.0684(18) Uani 1 1 d . . . . .
H58A H 0.0101 0.5112 0.1427 0.082 Uiso 1 1 calc R . . . .
H58B H 0.1003 0.4906 0.2338 0.082 Uiso 1 1 calc R . . . .
C59 C 0.1476(5) 0.5369(2) 0.1742(5) 0.0630(16) Uani 1 1 d . . . . .
H59A H 0.1611 0.5225 0.1211 0.076 Uiso 1 1 calc R . . . .
H59B H 0.1200 0.5619 0.1454 0.076 Uiso 1 1 calc R . . . .
C27 C 1.0603(9) 0.1881(3) 0.4993(10) 0.1111(13) Uani 1 1 d . . . . .
H27 H 0.9943 0.1863 0.4973 0.133 Uiso 1 1 calc R . . . .
C28 C 1.0759(9) 0.2046(3) 0.4224(10) 0.1111(13) Uani 1 1 d . . . . .
H28 H 1.0193 0.2161 0.3707 0.133 Uiso 1 1 calc R . . . .
C29 C 1.1594(9) 0.2068(3) 0.4101(10) 0.1111(13) Uani 1 1 d . . . . .
H29 H 1.1627 0.2171 0.3496 0.133 Uiso 1 1 calc R . . . .
C30 C 1.2537(9) 0.1918(3) 0.4992(10) 0.1111(13) Uani 1 1 d . . . . .
H30 H 1.3185 0.1927 0.4977 0.133 Uiso 1 1 calc R . . . .
C31 C 1.2350(9) 0.1757(3) 0.5886(10) 0.1111(13) Uani 1 1 d . . . . .
C32 C 1.3195(8) 0.1576(3) 0.6779(9) 0.1111(13) Uani 1 1 d . . . . .
H32A H 1.2985 0.1540 0.7351 0.167 Uiso 1 1 calc GR . . . .
H32B H 1.3785 0.1741 0.6998 0.167 Uiso 1 1 calc GR . . . .
H32C H 1.3361 0.1330 0.6567 0.167 Uiso 1 1 calc GR . . . .
C33 C 1.1388(9) 0.1739(3) 0.5806(10) 0.1111(13) Uani 1 1 d . . . . .
H33 H 1.1257 0.1620 0.6342 0.133 Uiso 1 1 calc R . . . .
C60 C 0.3729(6) 0.4533(2) 0.1918(6) 0.0715(18) Uani 1 1 d . . . . .
H60 H 0.4263 0.4625 0.2511 0.086 Uiso 1 1 calc R . . . .
C61 C 0.3912(6) 0.4429(3) 0.1060(6) 0.078(2) Uani 1 1 d . . . . .
H61 H 0.4566 0.4451 0.1066 0.093 Uiso 1 1 calc R . . . .
C62 C 0.3118(6) 0.4292(2) 0.0182(6) 0.0741(19) Uani 1 1 d . . . . .
H62 H 0.3250 0.4220 -0.0398 0.089 Uiso 1 1 calc R . . . .
C63 C 0.2135(5) 0.42561(19) 0.0136(6) 0.0637(16) Uani 1 1 d . . . . .
C64 C 0.1303(6) 0.4094(2) -0.0798(6) 0.082(2) Uani 1 1 d . . . . .
H64A H 0.1364 0.3817 -0.0794 0.123 Uiso 1 1 calc GR . . . .
H64B H 0.1352 0.4196 -0.1420 0.123 Uiso 1 1 calc GR . . . .
H64C H 0.0653 0.4163 -0.0788 0.123 Uiso 1 1 calc GR . . . .
C65 C 0.1984(5) 0.4368(2) 0.1030(6) 0.0689(17) Uani 1 1 d . . . . .
H65 H 0.1330 0.4350 0.1027 0.083 Uiso 1 1 calc R . . . .
C66 C 0.2764(5) 0.4502(2) 0.1912(6) 0.0715(18) Uani 1 1 d . . . . .
H66 H 0.2642 0.4572 0.2499 0.086 Uiso 1 1 calc R . . . .


_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 O1 2.622(5) . ?
K1 O2 2.773(4) . ?
K1 O3 2.935(4) . ?
K1 O4 2.856(4) . ?
K1 O5 2.983(4) . ?
K1 O6 2.975(5) . ?
K1 O7 2.865(5) . ?
K1 N1 2.910(6) . ?
K1 C16 3.510(8) . ?
O1 C1 1.262(9) . ?
O2 C15 1.421(9) . ?
O2 C26 1.416(9) . ?
O3 C24 1.424(8) . ?
O3 C25 1.429(8) . ?
O4 C22 1.427(7) . ?
O4 C23 1.427(7) . ?
O5 C20 1.419(7) . ?
O5 C21 1.438(7) . ?
O6 C18 1.439(8) . ?
O6 C19 1.424(8) . ?
O7 C16 1.427(9) . ?
O7 C17 1.393(10) . ?
N1 C11 1.304(9) . ?
N1 C14 1.457(10) . ?
C1 C2 1.404(11) . ?
C1 C12 1.475(11) . ?
C2 H2 0.9300 . ?
C2 C3 1.310(12) . ?
C3 H3 0.9300 . ?
C3 C4 1.390(12) . ?
C4 C5 1.465(12) . ?
C4 C13 1.406(10) . ?
C5 H5 0.9300 . ?
C5 C6 1.428(13) . ?
C6 H6 0.9300 . ?
C6 C7 1.318(13) . ?
C7 H7 0.9300 . ?
C7 C8 1.334(12) . ?
C8 C9 1.481(13) . ?
C8 C13 1.384(10) . ?
C9 H9 0.9300 . ?
C9 C10 1.341(12) . ?
C10 H10 0.9300 . ?
C10 C11 1.443(10) . ?
C11 C12 1.446(10) . ?
C12 C13 1.490(10) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.483(13) . ?
C16 H16A 0.9800 . ?
C16 H16B 1.05(10) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.511(11) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.487(9) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.493(9) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.497(10) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.488(11) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
K2 O8 2.597(5) . ?
K2 O9 2.819(4) . ?
K2 O10 3.046(4) . ?
K2 O11 2.876(4) . ?
K2 O12 2.937(5) . ?
K2 O13 2.972(5) . ?
K2 O14 2.947(9) . ?
K2 O15 2.986(9) . ?
K2 N2 2.841(5) . ?
K2 C47 3.467(7) . ?
O8 C34 1.254(8) . ?
O9 C48 1.400(8) . ?
O9 C59 1.418(7) . ?
O10 C57 1.423(8) . ?
O10 C58 1.433(9) . ?
O11 C55 1.414(10) . ?
O11 C56 1.430(9) . ?
O12 C53 1.426(10) . ?
O12 C54 1.427(9) . ?
O13 C51 1.445(9) . ?
O13 C52 1.447(11) . ?
O14 O15 0.992(14) . ?
O14 C49 1.161(12) . ?
O14 C50 1.502(11) . ?
O15 C49 1.315(12) . ?
O15 C50 1.530(12) . ?
N2 C44 1.292(8) . ?
N2 C47 1.467(8) . ?
C34 C35 1.441(10) . ?
C34 C45 1.459(9) . ?
C35 H35 0.9300 . ?
C35 C36 1.329(11) . ?
C36 H36 0.9300 . ?
C36 C37 1.425(11) . ?
C37 C38 1.394(10) . ?
C37 C46 1.426(9) . ?
C38 H38 0.9300 . ?
C38 C39 1.368(12) . ?
C39 H39 0.9300 . ?
C39 C40 1.380(12) . ?
C40 H40 0.9300 . ?
C40 C41 1.379(10) . ?
C41 C42 1.415(11) . ?
C41 C46 1.429(9) . ?
C42 H42 0.9300 . ?
C42 C43 1.349(10) . ?
C43 H43 0.9300 . ?
C43 C44 1.446(9) . ?
C44 C45 1.473(9) . ?
C45 C46 1.407(9) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C48 C49 1.452(10) . ?
C49 H49 0.9800 . ?
C50 H50 0.9800 . ?
C50 C51 1.493(15) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C52 C53 1.502(15) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C54 C55 1.490(12) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C56 C57 1.468(12) . ?
C57 H57A 0.9700 . ?
C57 H57B 0.9700 . ?
C58 H58A 0.9700 . ?
C58 H58B 0.9700 . ?
C58 C59 1.484(10) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C27 H27 0.9300 . ?
C27 C28 1.305(15) . ?
C27 C33 1.331(15) . ?
C28 H28 0.9300 . ?
C28 C29 1.267(14) . ?
C29 H29 0.9300 . ?
C29 C30 1.513(16) . ?
C30 H30 0.9300 . ?
C30 C31 1.477(16) . ?
C31 C32 1.484(15) . ?
C31 C33 1.330(15) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33 0.9300 . ?
C60 H60 0.9300 . ?
C60 C61 1.363(11) . ?
C60 C66 1.373(10) . ?
C61 H61 0.9300 . ?
C61 C62 1.379(10) . ?
C62 H62 0.9300 . ?
C62 C63 1.379(10) . ?
C63 C64 1.481(10) . ?
C63 C65 1.395(10) . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C65 H65 0.9300 . ?
C65 C66 1.370(10) . ?
C66 H66 0.9300 . ?

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 K1 O2 82.78(16) . . ?
O1 K1 O3 73.67(14) . . ?
O1 K1 O4 83.07(14) . . ?
O1 K1 O5 122.05(14) . . ?
O1 K1 O6 142.53(15) . . ?
O1 K1 O7 126.45(16) . . ?
O1 K1 N1 59.59(17) . . ?
O1 K1 C16 103.9(2) . . ?
O2 K1 O3 58.90(14) . . ?
O2 K1 O4 117.69(14) . . ?
O2 K1 O5 149.75(13) . . ?
O2 K1 O6 115.91(15) . . ?
O2 K1 O7 58.96(16) . . ?
O2 K1 N1 93.13(16) . . ?
O2 K1 C16 42.0(2) . . ?
O3 K1 O5 108.40(12) . . ?
O3 K1 O6 143.70(13) . . ?
O3 K1 C16 99.72(19) . . ?
O4 K1 O3 58.86(12) . . ?
O4 K1 O5 56.06(12) . . ?
O4 K1 O6 111.64(13) . . ?
O4 K1 O7 145.96(14) . . ?
O4 K1 N1 128.44(15) . . ?
O4 K1 C16 155.19(19) . . ?
O5 K1 C16 130.93(19) . . ?
O6 K1 O5 56.07(12) . . ?
O6 K1 C16 77.44(19) . . ?
O7 K1 O3 109.06(14) . . ?
O7 K1 O5 107.98(14) . . ?
O7 K1 O6 57.16(14) . . ?
O7 K1 N1 84.81(16) . . ?
O7 K1 C16 23.14(19) . . ?
N1 K1 O3 128.51(16) . . ?
N1 K1 O5 113.78(15) . . ?
N1 K1 O6 86.00(16) . . ?
N1 K1 C16 73.7(2) . . ?
C1 O1 K1 149.6(5) . . ?
C15 O2 K1 120.2(4) . . ?
C26 O2 K1 121.0(4) . . ?
C26 O2 C15 112.3(6) . . ?
C24 O3 K1 105.7(3) . . ?
C24 O3 C25 111.7(5) . . ?
C25 O3 K1 105.6(4) . . ?
C22 O4 K1 123.6(4) . . ?
C22 O4 C23 110.7(5) . . ?
C23 O4 K1 118.8(3) . . ?
C20 O5 K1 110.6(3) . . ?
C20 O5 C21 112.2(5) . . ?
C21 O5 K1 111.2(3) . . ?
C18 O6 K1 115.8(4) . . ?
C19 O6 K1 118.8(4) . . ?
C19 O6 C18 110.4(5) . . ?
C16 O7 K1 104.7(5) . . ?
C17 O7 K1 119.1(4) . . ?
C17 O7 C16 113.0(6) . . ?
C11 N1 K1 138.0(5) . . ?
C11 N1 C14 116.6(7) . . ?
C14 N1 K1 104.5(5) . . ?
O1 C1 C2 120.1(8) . . ?
O1 C1 C12 122.9(7) . . ?
C2 C1 C12 117.0(7) . . ?
C1 C2 H2 117.4 . . ?
C3 C2 C1 125.2(9) . . ?
C3 C2 H2 117.4 . . ?
C2 C3 H3 119.8 . . ?
C2 C3 C4 120.4(9) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 C5 120.0(8) . . ?
C3 C4 C13 122.0(7) . . ?
C13 C4 C5 117.8(7) . . ?
C4 C5 H5 121.6 . . ?
C6 C5 C4 116.7(8) . . ?
C6 C5 H5 121.6 . . ?
C5 C6 H6 119.3 . . ?
C7 C6 C5 121.3(8) . . ?
C7 C6 H6 119.3 . . ?
C6 C7 H7 118.5 . . ?
C6 C7 C8 122.9(10) . . ?
C8 C7 H7 118.5 . . ?
C7 C8 C9 121.7(8) . . ?
C7 C8 C13 121.0(9) . . ?
C13 C8 C9 117.3(8) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 C8 119.4(8) . . ?
C10 C9 H9 120.3 . . ?
C9 C10 H10 116.4 . . ?
C9 C10 C11 127.1(9) . . ?
C11 C10 H10 116.4 . . ?
N1 C11 C10 122.8(8) . . ?
N1 C11 C12 123.0(7) . . ?
C10 C11 C12 114.2(8) . . ?
C1 C12 C13 117.5(6) . . ?
C11 C12 C1 122.8(7) . . ?
C11 C12 C13 119.6(7) . . ?
C4 C13 C12 117.6(6) . . ?
C8 C13 C4 120.2(7) . . ?
C8 C13 C12 122.2(7) . . ?
N1 C14 H14A 109.5 . . ?
N1 C14 H14B 109.5 . . ?
N1 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O2 C15 H15A 110.0 . . ?
O2 C15 H15B 110.0 . . ?
O2 C15 C16 108.4(6) . . ?
H15A C15 H15B 108.4 . . ?
C16 C15 H15A 110.0 . . ?
C16 C15 H15B 110.0 . . ?
K1 C16 H16A 125.7 . . ?
K1 C16 H16B 153(5) . . ?
O7 C16 K1 52.1(4) . . ?
O7 C16 C15 108.6(7) . . ?
O7 C16 H16A 125.7 . . ?
O7 C16 H16B 101(5) . . ?
C15 C16 K1 85.3(5) . . ?
C15 C16 H16A 125.7 . . ?
C15 C16 H16B 102(6) . . ?
H16A C16 H16B 71.0 . . ?
O7 C17 H17A 109.8 . . ?
O7 C17 H17B 109.8 . . ?
O7 C17 C18 109.2(6) . . ?
H17A C17 H17B 108.3 . . ?
C18 C17 H17A 109.8 . . ?
C18 C17 H17B 109.8 . . ?
O6 C18 C17 108.9(6) . . ?
O6 C18 H18A 109.9 . . ?
O6 C18 H18B 109.9 . . ?
C17 C18 H18A 109.9 . . ?
C17 C18 H18B 109.9 . . ?
H18A C18 H18B 108.3 . . ?
O6 C19 H19A 109.9 . . ?
O6 C19 H19B 109.9 . . ?
O6 C19 C20 108.8(5) . . ?
H19A C19 H19B 108.3 . . ?
C20 C19 H19A 109.9 . . ?
C20 C19 H19B 109.9 . . ?
O5 C20 C19 107.5(5) . . ?
O5 C20 H20A 110.2 . . ?
O5 C20 H20B 110.2 . . ?
C19 C20 H20A 110.2 . . ?
C19 C20 H20B 110.2 . . ?
H20A C20 H20B 108.5 . . ?
O5 C21 H21A 110.2 . . ?
O5 C21 H21B 110.2 . . ?
O5 C21 C22 107.4(5) . . ?
H21A C21 H21B 108.5 . . ?
C22 C21 H21A 110.2 . . ?
C22 C21 H21B 110.2 . . ?
O4 C22 C21 108.6(5) . . ?
O4 C22 H22A 110.0 . . ?
O4 C22 H22B 110.0 . . ?
C21 C22 H22A 110.0 . . ?
C21 C22 H22B 110.0 . . ?
H22A C22 H22B 108.3 . . ?
O4 C23 H23A 110.0 . . ?
O4 C23 H23B 110.0 . . ?
O4 C23 C24 108.5(5) . . ?
H23A C23 H23B 108.4 . . ?
C24 C23 H23A 110.0 . . ?
C24 C23 H23B 110.0 . . ?
O3 C24 C23 109.6(5) . . ?
O3 C24 H24A 109.8 . . ?
O3 C24 H24B 109.8 . . ?
C23 C24 H24A 109.8 . . ?
C23 C24 H24B 109.8 . . ?
H24A C24 H24B 108.2 . . ?
O3 C25 H25A 109.9 . . ?
O3 C25 H25B 109.9 . . ?
O3 C25 C26 108.9(6) . . ?
H25A C25 H25B 108.3 . . ?
C26 C25 H25A 109.9 . . ?
C26 C25 H25B 109.9 . . ?
O2 C26 C25 108.0(5) . . ?
O2 C26 H26A 110.1 . . ?
O2 C26 H26B 110.1 . . ?
C25 C26 H26A 110.1 . . ?
C25 C26 H26B 110.1 . . ?
H26A C26 H26B 108.4 . . ?
O8 K2 O9 83.35(14) . . ?
O8 K2 O10 78.23(13) . . ?
O8 K2 O11 96.09(16) . . ?
O8 K2 O12 142.08(15) . . ?
O8 K2 O13 142.06(16) . . ?
O8 K2 O14 114.5(3) . . ?
O8 K2 O15 96.18(18) . . ?
O8 K2 N2 60.97(15) . . ?
O8 K2 C47 85.26(15) . . ?
O9 K2 O10 56.43(12) . . ?
O9 K2 O11 111.55(14) . . ?
O9 K2 O12 128.95(14) . . ?
O9 K2 O13 105.81(14) . . ?
O9 K2 O14 56.06(19) . . ?
O9 K2 O15 55.26(19) . . ?
O9 K2 N2 137.79(15) . . ?
O9 K2 C47 151.78(16) . . ?
O10 K2 C47 144.89(15) . . ?
O11 K2 O10 56.64(14) . . ?
O11 K2 O12 56.78(16) . . ?
O11 K2 O13 113.33(18) . . ?
O11 K2 O14 143.1(3) . . ?
O11 K2 O15 160.58(19) . . ?
O11 K2 C47 95.26(16) . . ?
O12 K2 O10 102.09(14) . . ?
O12 K2 O13 56.68(16) . . ?
O12 K2 O14 101.5(3) . . ?
O12 K2 O15 117.81(19) . . ?
O12 K2 C47 72.97(15) . . ?
O13 K2 O10 137.75(14) . . ?
O13 K2 O15 63.3(2) . . ?
O13 K2 C47 69.29(15) . . ?
O14 K2 O10 108.2(2) . . ?
O14 K2 O13 52.2(2) . . ?
O14 K2 O15 19.2(3) . . ?
O14 K2 C47 106.8(2) . . ?
O15 K2 O10 111.64(19) . . ?
O15 K2 C47 100.7(2) . . ?
N2 K2 O10 127.89(14) . . ?
N2 K2 O11 95.01(15) . . ?
N2 K2 O12 92.89(14) . . ?
N2 K2 O13 91.85(15) . . ?
N2 K2 O14 117.2(3) . . ?
N2 K2 O15 104.09(19) . . ?
N2 K2 C47 24.40(15) . . ?
C34 O8 K2 147.5(4) . . ?
C48 O9 K2 124.4(4) . . ?
C48 O9 C59 112.5(5) . . ?
C59 O9 K2 123.0(4) . . ?
C57 O10 K2 100.7(4) . . ?
C57 O10 C58 111.8(6) . . ?
C58 O10 K2 101.2(3) . . ?
C55 O11 K2 122.0(5) . . ?
C55 O11 C56 111.3(6) . . ?
C56 O11 K2 120.9(4) . . ?
C53 O12 K2 116.5(5) . . ?
C53 O12 C54 111.4(7) . . ?
C54 O12 K2 109.7(5) . . ?
C51 O13 K2 117.0(5) . . ?
C51 O13 C52 114.2(7) . . ?
C52 O13 K2 117.9(5) . . ?
O15 O14 K2 82.6(9) . . ?
O15 O14 C49 74.8(11) . . ?
O15 O14 C50 72.5(9) . . ?
C49 O14 K2 117.6(7) . . ?
C49 O14 C50 119.3(9) . . ?
C50 O14 K2 107.1(6) . . ?
O14 O15 K2 78.2(8) . . ?
O14 O15 C49 58.4(8) . . ?
O14 O15 C50 69.3(8) . . ?
C49 O15 K2 109.0(6) . . ?
C49 O15 C50 107.9(7) . . ?
C50 O15 K2 104.5(5) . . ?
C44 N2 K2 139.1(4) . . ?
C44 N2 C47 117.6(5) . . ?
C47 N2 K2 102.4(4) . . ?
O8 C34 C35 118.2(6) . . ?
O8 C34 C45 126.0(6) . . ?
C35 C34 C45 115.8(6) . . ?
C34 C35 H35 117.6 . . ?
C36 C35 C34 124.8(7) . . ?
C36 C35 H35 117.6 . . ?
C35 C36 H36 119.7 . . ?
C35 C36 C37 120.6(7) . . ?
C37 C36 H36 119.7 . . ?
C36 C37 C46 117.4(6) . . ?
C38 C37 C36 122.0(7) . . ?
C38 C37 C46 120.6(7) . . ?
C37 C38 H38 118.5 . . ?
C39 C38 C37 123.0(8) . . ?
C39 C38 H38 118.5 . . ?
C38 C39 H39 121.4 . . ?
C38 C39 C40 117.2(8) . . ?
C40 C39 H39 121.4 . . ?
C39 C40 H40 118.8 . . ?
C41 C40 C39 122.5(8) . . ?
C41 C40 H40 118.8 . . ?
C40 C41 C42 121.6(7) . . ?
C40 C41 C46 121.5(7) . . ?
C42 C41 C46 116.9(6) . . ?
C41 C42 H42 119.0 . . ?
C43 C42 C41 121.9(7) . . ?
C43 C42 H42 119.0 . . ?
C42 C43 H43 117.7 . . ?
C42 C43 C44 124.6(7) . . ?
C44 C43 H43 117.7 . . ?
N2 C44 C43 123.0(6) . . ?
N2 C44 C45 123.2(6) . . ?
C43 C44 C45 113.7(6) . . ?
C34 C45 C44 120.6(6) . . ?
C46 C45 C34 118.6(6) . . ?
C46 C45 C44 120.8(6) . . ?
C37 C46 C41 115.3(6) . . ?
C45 C46 C37 122.8(6) . . ?
C45 C46 C41 121.9(6) . . ?
K2 C47 H47A 118.4 . . ?
K2 C47 H47B 118.4 . . ?
N2 C47 K2 53.2(3) . . ?
N2 C47 H47A 118.4 . . ?
N2 C47 H47B 118.4 . . ?
H47A C47 H47B 115.7 . . ?
O9 C48 H48A 109.6 . . ?
O9 C48 H48B 109.6 . . ?
O9 C48 C49 110.3(6) . . ?
H48A C48 H48B 108.1 . . ?
C49 C48 H48A 109.6 . . ?
C49 C48 H48B 109.6 . . ?
O14 C49 O15 46.7(8) . . ?
O14 C49 C48 129.5(8) . . ?
O14 C49 H49 114.8 . . ?
O15 C49 C48 115.8(8) . . ?
O15 C49 H49 114.8 . . ?
C48 C49 H49 114.8 . . ?
O14 C50 O15 38.2(6) . . ?
O14 C50 H50 104.7 . . ?
O15 C50 H50 104.7 . . ?
C51 C50 O14 90.1(9) . . ?
C51 C50 O15 125.5(8) . . ?
C51 C50 H50 104.7 . . ?
O13 C51 C50 109.5(7) . . ?
O13 C51 H51A 109.8 . . ?
O13 C51 H51B 109.8 . . ?
C50 C51 H51A 109.8 . . ?
C50 C51 H51B 109.8 . . ?
H51A C51 H51B 108.2 . . ?
O13 C52 H52A 109.9 . . ?
O13 C52 H52B 109.9 . . ?
O13 C52 C53 108.8(7) . . ?
H52A C52 H52B 108.3 . . ?
C53 C52 H52A 109.9 . . ?
C53 C52 H52B 109.9 . . ?
O12 C53 C52 108.4(7) . . ?
O12 C53 H53A 110.0 . . ?
O12 C53 H53B 110.0 . . ?
C52 C53 H53A 110.0 . . ?
C52 C53 H53B 110.0 . . ?
H53A C53 H53B 108.4 . . ?
O12 C54 H54A 109.8 . . ?
O12 C54 H54B 109.8 . . ?
O12 C54 C55 109.2(6) . . ?
H54A C54 H54B 108.3 . . ?
C55 C54 H54A 109.8 . . ?
C55 C54 H54B 109.8 . . ?
O11 C55 C54 108.9(6) . . ?
O11 C55 H55A 109.9 . . ?
O11 C55 H55B 109.9 . . ?
C54 C55 H55A 109.9 . . ?
C54 C55 H55B 109.9 . . ?
H55A C55 H55B 108.3 . . ?
O11 C56 H56A 110.0 . . ?
O11 C56 H56B 110.0 . . ?
O11 C56 C57 108.5(6) . . ?
H56A C56 H56B 108.4 . . ?
C57 C56 H56A 110.0 . . ?
C57 C56 H56B 110.0 . . ?
O10 C57 C56 109.9(6) . . ?
O10 C57 H57A 109.7 . . ?
O10 C57 H57B 109.7 . . ?
C56 C57 H57A 109.7 . . ?
C56 C57 H57B 109.7 . . ?
H57A C57 H57B 108.2 . . ?
O10 C58 H58A 109.9 . . ?
O10 C58 H58B 109.9 . . ?
O10 C58 C59 108.7(5) . . ?
H58A C58 H58B 108.3 . . ?
C59 C58 H58A 109.9 . . ?
C59 C58 H58B 109.9 . . ?
O9 C59 C58 109.3(5) . . ?
O9 C59 H59A 109.8 . . ?
O9 C59 H59B 109.8 . . ?
C58 C59 H59A 109.8 . . ?
C58 C59 H59B 109.8 . . ?
H59A C59 H59B 108.3 . . ?
C28 C27 H27 120.0 . . ?
C28 C27 C33 120.0(12) . . ?
C33 C27 H27 120.0 . . ?
C27 C28 H28 116.3 . . ?
C29 C28 C27 127.4(14) . . ?
C29 C28 H28 116.3 . . ?
C28 C29 H29 121.8 . . ?
C28 C29 C30 116.5(12) . . ?
C30 C29 H29 121.8 . . ?
C29 C30 H30 122.5 . . ?
C31 C30 C29 114.9(10) . . ?
C31 C30 H30 122.5 . . ?
C30 C31 C32 120.5(10) . . ?
C33 C31 C30 117.9(12) . . ?
C33 C31 C32 121.1(12) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C27 C33 H33 118.5 . . ?
C31 C33 C27 123.0(13) . . ?
C31 C33 H33 118.5 . . ?
C61 C60 H60 119.7 . . ?
C61 C60 C66 120.5(7) . . ?
C66 C60 H60 119.7 . . ?
C60 C61 H61 120.3 . . ?
C60 C61 C62 119.5(7) . . ?
C62 C61 H61 120.3 . . ?
C61 C62 H62 118.9 . . ?
C63 C62 C61 122.2(7) . . ?
C63 C62 H62 118.9 . . ?
C62 C63 C64 121.3(7) . . ?
C62 C63 C65 116.3(7) . . ?
C65 C63 C64 122.4(7) . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C63 C65 H65 118.8 . . ?
C66 C65 C63 122.3(7) . . ?
C66 C65 H65 118.8 . . ?
C60 C66 H66 120.4 . . ?
C65 C66 C60 119.2(7) . . ?
C65 C66 H66 120.4 . . ?

_olex2_date_sample_data_collection 2020-01-20
_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 1.819
_oxdiff_exptl_absorpt_empirical_full_min 0.438
####################################################################### 
# 
# 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_jasi_3ktollt
_database_code_depnum_ccdc_archive 'CCDC 1991246'
loop_
_audit_author_name
_audit_author_address
'Arpan Das'
;Senior Research Fellow
India
;
_audit_update_record             
;
2020-03-18 deposited with the CCDC.	2020-12-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT987_jasi_3ktollt        
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check
RESPONSE: Flack test results are as follows. From the CIF: _refine_ls_abs_structure_Flack 0.450.   From the CIF: _refine_ls_abs_structure_Flack_su 0.002
;
# Added during the CSD deposition process: Wednesday 18 March 2020 12:07 PM
# end Validation Reply Form

_audit_creation_date             2020-03-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C37 H53 K2 O14, 2(C7 H8)'
_chemical_formula_sum            'C51 H69 K2 O14'
_chemical_formula_weight         984.26
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O K'
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           19
_space_group_name_H-M_alt        'P 21 21 21'
_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'

_cell_length_a                   14.23700(10)
_cell_length_b                   18.7126(2)
_cell_length_c                   19.1013(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5088.80(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    22202
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      66.1460
_cell_measurement_theta_min      3.2850
_shelx_estimated_absorpt_T_max   0.812
_shelx_estimated_absorpt_T_min   0.612
_exptl_absorpt_coefficient_mu    2.176
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34892
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        66.146
_diffrn_reflns_theta_max         66.146
_diffrn_reflns_theta_min         3.306
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -58.00   70.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       26.3311  -77.0000 -180.0000 128

#__ type_ start__ end____ width___ exp.time_
  2 omega  -12.00  102.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       26.3311   57.0000 -180.0000 114

#__ type_ start__ end____ width___ exp.time_
  3 omega  100.00  153.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656  111.0000 -180.0000 53

#__ type_ start__ end____ width___ exp.time_
  4 omega  -17.00  144.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656  -30.0000 -180.0000 161

#__ type_ start__ end____ width___ exp.time_
  5 omega   57.00  150.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656  178.0000  -30.0000 93

#__ type_ start__ end____ width___ exp.time_
  6 omega   95.00  147.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656  126.0000   69.0000 52

#__ type_ start__ end____ width___ exp.time_
  7 omega   69.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   54.0000  150.0000 109

#__ type_ start__ end____ width___ exp.time_
  8 omega  101.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000   90.0000 77

#__ type_ start__ end____ width___ exp.time_
  9 omega  101.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000  -30.0000 77

#__ type_ start__ end____ width___ exp.time_
 10 omega   71.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   65.0000 -150.0000 107

#__ type_ start__ end____ width___ exp.time_
 11 omega   86.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  138.0000 -150.0000 92

#__ type_ start__ end____ width___ exp.time_
 12 omega   21.00  113.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -104.0000    0.0000 92

#__ type_ start__ end____ width___ exp.time_
 13 omega   21.00  113.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -104.0000 -150.0000 92

#__ type_ start__ end____ width___ exp.time_
 14 omega   21.00  113.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -104.0000  120.0000 92

#__ type_ start__ end____ width___ exp.time_
 15 omega  101.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000   30.0000 77

#__ type_ start__ end____ width___ exp.time_
 16 omega   71.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   65.0000  -90.0000 107

#__ type_ start__ end____ width___ exp.time_
 17 omega  101.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  104.0000 -180.0000 77

#__ type_ start__ end____ width___ exp.time_
 18 omega   69.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   68.0000   77.1316 109

#__ type_ start__ end____ width___ exp.time_
 19 omega   70.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   56.0000 -113.2181 108

#__ type_ start__ end____ width___ exp.time_
 20 omega  -12.00  102.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       26.3311   57.0000  -60.0000 114

#__ type_ start__ end____ width___ exp.time_
 21 omega  -50.00   64.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       26.3311  -57.0000   30.0000 114

#__ type_ start__ end____ width___ exp.time_
 22 omega   57.00  121.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       26.3311  178.0000   90.0000 64

#__ type_ start__ end____ width___ exp.time_
 23 omega  -12.00  102.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       26.3311   57.0000   60.0000 114

#__ type_ start__ end____ width___ exp.time_
 24 omega   20.00  147.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   45.0000 -120.0000 127

#__ type_ start__ end____ width___ exp.time_
 25 omega   20.00  135.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   45.0000   60.0000 115

#__ type_ start__ end____ width___ exp.time_
 26 omega   20.00  147.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       67.1656   45.0000  -30.0000 127
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0920513000
_diffrn_orient_matrix_UB_12      -0.0430501000
_diffrn_orient_matrix_UB_13      0.0046459000
_diffrn_orient_matrix_UB_21      0.0564800000
_diffrn_orient_matrix_UB_22      0.0701727000
_diffrn_orient_matrix_UB_23      0.0026218000
_diffrn_orient_matrix_UB_31      -0.0070802000
_diffrn_orient_matrix_UB_32      0.0001585000
_diffrn_orient_matrix_UB_33      0.0804616000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.791
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                8624
_reflns_number_total             8827
_reflns_odcompleteness_completeness 98.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 
;
 Flack x determined using 3669 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.450(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         8827
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0407
_refine_ls_restrained_S_all      1.028
_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)+(0.0565P)²+4.4367P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1077
_refine_special_details          ?
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5
 0.5
2. 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
3.a Ternary CH refined with riding coordinates:
 C30(H30), C37(H37)
3.b Secondary CH2 refined with riding coordinates:
 C14(H14a,H14b), C15(H15a,H15b), C16(H16a,H16b), C17(H17a,H17b), C18(H18a,
 H18b), C19(H19a,H19b), C20(H20a,H20b), C21(H21a,H21b), C22(H22a,H22b),
 C23(H23a,H23b), C24(H24a,H24b), C25(H25a,H25b), C26(H26a,H26b), C27(H27a,H27b),
  C28(H28a,H28b), C29(H29a,H29b), C31(H31a,H31b), C32(H32a,H32b), C33(H33a,
 H33b), C34(H34a,H34b), C35(H35a,H35b), C36(H36a,H36b)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C38(H38),
 C39(H39), C40(H40), C41(H41), C43(H43), C47(H47), C48(H48), C49(H49), C50(H50),
  C51(H51)
3.d Idealised Me refined as rotating group:
 C44(H44a,H44b,H44c), C45(H45a,H45b,H45c)
;
_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 0.74556(5) 0.61502(3) 0.55607(3) 0.01995(16) Uani 1 1 d . . . . .
K2 K 0.75848(5) 0.44600(4) 0.68003(3) 0.02098(16) Uani 1 1 d . . . . .
O1 O 0.85165(17) 0.50085(12) 0.56952(13) 0.0210(5) Uani 1 1 d . . . . .
O2 O 0.65866(17) 0.49137(13) 0.56882(13) 0.0210(5) Uani 1 1 d . . . . .
O3 O 0.93229(18) 0.37497(15) 0.68871(14) 0.0286(6) Uani 1 1 d . . . . .
O4 O 0.77588(18) 0.28553(13) 0.68630(13) 0.0260(5) Uani 1 1 d . . . . .
O5 O 0.60242(18) 0.35615(14) 0.68587(14) 0.0271(6) Uani 1 1 d . . . . .
O6 O 0.5744(2) 0.48383(14) 0.75639(14) 0.0278(6) Uani 1 1 d . . . . .
O7 O 0.7417(2) 0.56608(13) 0.77282(12) 0.0300(6) Uani 1 1 d . . . . .
O8 O 0.9249(2) 0.50497(14) 0.75753(15) 0.0288(6) Uani 1 1 d . . . . .
O9 O 0.91659(18) 0.65030(14) 0.46771(14) 0.0256(6) Uani 1 1 d . . . . .
O10 O 0.74053(18) 0.60604(13) 0.41173(11) 0.0243(5) Uani 1 1 d . . . . .
O11 O 0.56534(17) 0.63410(13) 0.47570(14) 0.0241(5) Uani 1 1 d . . . . .
O12 O 0.57682(18) 0.67229(14) 0.61662(14) 0.0263(6) Uani 1 1 d . . . . .
O13 O 0.73756(19) 0.75206(13) 0.65297(12) 0.0273(5) Uani 1 1 d . . . . .
O14 O 0.90918(18) 0.69588(14) 0.60642(15) 0.0276(6) Uani 1 1 d . . . . .
C1 C 0.8500(2) 0.44242(19) 0.53328(18) 0.0197(7) Uani 1 1 d . . . . .
C2 C 0.9354(3) 0.4110(2) 0.51183(19) 0.0235(7) Uani 1 1 d . . . . .
H2 H 0.9916 0.4341 0.5222 0.028 Uiso 1 1 calc R . . . .
C3 C 0.9382(3) 0.3462(2) 0.47548(19) 0.0258(8) Uani 1 1 d . . . . .
H3 H 0.9962 0.3271 0.4633 0.031 Uiso 1 1 calc R . . . .
C4 C 0.8586(3) 0.3100(2) 0.45715(19) 0.0247(8) Uani 1 1 d . . . . .
C5 C 0.8643(3) 0.2415(2) 0.4179(2) 0.0379(10) Uani 1 1 d . . . . .
H5 H 0.9222 0.2227 0.4051 0.045 Uiso 1 1 calc R . . . .
C6 C 0.7806(4) 0.2058(2) 0.4003(2) 0.0415(11) Uani 1 1 d . . . . .
H6 H 0.7844 0.1616 0.3783 0.050 Uiso 1 1 calc R . . . .
C7 C 0.6923(3) 0.2343(2) 0.4149(2) 0.0331(9) Uani 1 1 d . . . . .
H7 H 0.6383 0.2114 0.3991 0.040 Uiso 1 1 calc R . . . .
C8 C 0.6853(3) 0.3018(2) 0.45581(18) 0.0242(8) Uani 1 1 d . . . . .
C9 C 0.7688(2) 0.33916(18) 0.47530(16) 0.0203(7) Uani 1 1 d . . . . .
C10 C 0.7633(2) 0.40552(17) 0.51374(16) 0.0189(7) Uani 1 1 d . . . . .
C11 C 0.5997(3) 0.3300(2) 0.4736(2) 0.0261(8) Uani 1 1 d . . . . .
H11 H 0.5455 0.3056 0.4609 0.031 Uiso 1 1 calc R . . . .
C12 C 0.5913(3) 0.39415(19) 0.51023(19) 0.0231(7) Uani 1 1 d . . . . .
H12 H 0.5316 0.4115 0.5204 0.028 Uiso 1 1 calc R . . . .
C13 C 0.6704(2) 0.43366(18) 0.53239(18) 0.0198(7) Uani 1 1 d . . . . .
C14 C 0.9959(3) 0.4902(2) 0.7072(2) 0.0330(9) Uani 1 1 d . . . . .
H14A H 1.0527 0.5165 0.7183 0.040 Uiso 1 1 calc R . . . .
H14B H 0.9750 0.5045 0.6609 0.040 Uiso 1 1 calc R . . . .
C15 C 1.0149(3) 0.4114(2) 0.7087(2) 0.0328(9) Uani 1 1 d . . . . .
H15A H 1.0656 0.3998 0.6767 0.039 Uiso 1 1 calc R . . . .
H15B H 1.0334 0.3969 0.7555 0.039 Uiso 1 1 calc R . . . .
C16 C 0.9411(3) 0.2997(2) 0.6898(2) 0.0319(9) Uani 1 1 d . . . . .
H16A H 0.9415 0.2828 0.7378 0.038 Uiso 1 1 calc R . . . .
H16B H 0.9998 0.2857 0.6680 0.038 Uiso 1 1 calc R . . . .
C17 C 0.8608(3) 0.2675(2) 0.6513(2) 0.0301(8) Uani 1 1 d . . . . .
H17A H 0.8593 0.2854 0.6037 0.036 Uiso 1 1 calc R . . . .
H17B H 0.8679 0.2159 0.6496 0.036 Uiso 1 1 calc R . . . .
C18 C 0.6965(3) 0.2584(2) 0.6499(2) 0.0282(8) Uani 1 1 d . . . . .
H18A H 0.6999 0.2067 0.6476 0.034 Uiso 1 1 calc R . . . .
H18B H 0.6956 0.2769 0.6025 0.034 Uiso 1 1 calc R . . . .
C19 C 0.6093(3) 0.2805(2) 0.6876(2) 0.0285(8) Uani 1 1 d . . . . .
H19A H 0.5547 0.2594 0.6653 0.034 Uiso 1 1 calc R . . . .
H19B H 0.6116 0.2641 0.7358 0.034 Uiso 1 1 calc R . . . .
C20 C 0.5115(3) 0.3817(2) 0.7024(2) 0.0316(9) Uani 1 1 d . . . . .
H20A H 0.4929 0.3649 0.7484 0.038 Uiso 1 1 calc R . . . .
H20B H 0.4664 0.3642 0.6684 0.038 Uiso 1 1 calc R . . . .
C21 C 0.5137(3) 0.4617(2) 0.7013(2) 0.0282(8) Uani 1 1 d . . . . .
H21A H 0.5371 0.4787 0.6566 0.034 Uiso 1 1 calc R . . . .
H21B H 0.4511 0.4808 0.7084 0.034 Uiso 1 1 calc R . . . .
C22 C 0.5753(3) 0.5590(2) 0.7665(2) 0.0314(9) Uani 1 1 d . . . . .
H22A H 0.5174 0.5742 0.7887 0.038 Uiso 1 1 calc R . . . .
H22B H 0.5806 0.5831 0.7217 0.038 Uiso 1 1 calc R . . . .
C23 C 0.6572(3) 0.5777(2) 0.8118(2) 0.0321(9) Uani 1 1 d . . . . .
H23A H 0.6532 0.6273 0.8261 0.038 Uiso 1 1 calc R . . . .
H23B H 0.6571 0.5481 0.8535 0.038 Uiso 1 1 calc R . . . .
C24 C 0.8224(3) 0.5889(2) 0.8106(2) 0.0332(9) Uani 1 1 d . . . . .
H24A H 0.8293 0.5609 0.8530 0.040 Uiso 1 1 calc R . . . .
H24B H 0.8159 0.6388 0.8236 0.040 Uiso 1 1 calc R . . . .
C25 C 0.9073(3) 0.5794(2) 0.7646(2) 0.0346(9) Uani 1 1 d . . . . .
H25A H 0.8959 0.6004 0.7189 0.041 Uiso 1 1 calc R . . . .
H25B H 0.9612 0.6028 0.7854 0.041 Uiso 1 1 calc R . . . .
C26 C 0.5775(3) 0.5866(2) 0.4184(2) 0.0254(8) Uani 1 1 d . . . . .
H26A H 0.5201 0.5840 0.3913 0.030 Uiso 1 1 calc R . . . .
H26B H 0.5921 0.5391 0.4356 0.030 Uiso 1 1 calc R . . . .
C27 C 0.6559(3) 0.6132(2) 0.37350(19) 0.0253(8) Uani 1 1 d . . . . .
H27A H 0.6592 0.5855 0.3306 0.030 Uiso 1 1 calc R . . . .
H27B H 0.6455 0.6628 0.3613 0.030 Uiso 1 1 calc R . . . .
C28 C 0.8218(3) 0.6190(2) 0.37010(19) 0.0267(8) Uani 1 1 d . . . . .
H28A H 0.8245 0.6689 0.3567 0.032 Uiso 1 1 calc R . . . .
H28B H 0.8196 0.5902 0.3279 0.032 Uiso 1 1 calc R . . . .
C29 C 0.9061(3) 0.5996(2) 0.4128(2) 0.0276(8) Uani 1 1 d . . . . .
H29A H 0.8984 0.5521 0.4323 0.033 Uiso 1 1 calc R . . . .
H29B H 0.9617 0.5997 0.3835 0.033 Uiso 1 1 calc R . . . .
C30 C 0.9864(2) 0.6291(2) 0.5169(2) 0.0264(8) Uani 1 1 d . . . . .
H30 H 1.0301 0.5890 0.5113 0.032 Uiso 1 1 calc R . . . .
C31 C 0.9957(3) 0.6885(2) 0.5693(2) 0.0294(8) Uani 1 1 d . . . . .
H31A H 1.0461 0.6779 0.6018 0.035 Uiso 1 1 calc R . . . .
H31B H 1.0106 0.7329 0.5454 0.035 Uiso 1 1 calc R . . . .
C32 C 0.9017(3) 0.7648(2) 0.6368(2) 0.0328(9) Uani 1 1 d . . . . .
H32A H 0.8891 0.8001 0.6009 0.039 Uiso 1 1 calc R . . . .
H32B H 0.9601 0.7773 0.6599 0.039 Uiso 1 1 calc R . . . .
C33 C 0.8236(3) 0.7635(2) 0.6886(2) 0.0327(9) Uani 1 1 d . . . . .
H33A H 0.8339 0.7256 0.7224 0.039 Uiso 1 1 calc R . . . .
H33B H 0.8213 0.8086 0.7137 0.039 Uiso 1 1 calc R . . . .
C34 C 0.6634(3) 0.7393(2) 0.7010(2) 0.0344(10) Uani 1 1 d . . . . .
H34A H 0.6592 0.7785 0.7341 0.041 Uiso 1 1 calc R . . . .
H34B H 0.6755 0.6957 0.7270 0.041 Uiso 1 1 calc R . . . .
C35 C 0.5729(3) 0.7325(2) 0.6614(2) 0.0360(10) Uani 1 1 d . . . . .
H35A H 0.5211 0.7273 0.6940 0.043 Uiso 1 1 calc R . . . .
H35B H 0.5622 0.7754 0.6339 0.043 Uiso 1 1 calc R . . . .
C36 C 0.4886(3) 0.6609(2) 0.5830(2) 0.0296(8) Uani 1 1 d . . . . .
H36A H 0.4661 0.7053 0.5628 0.036 Uiso 1 1 calc R . . . .
H36B H 0.4427 0.6443 0.6168 0.036 Uiso 1 1 calc R . . . .
C37 C 0.5016(2) 0.6058(2) 0.5264(2) 0.0267(8) Uani 1 1 d . . . . .
H37 H 0.4649 0.5618 0.5213 0.032 Uiso 1 1 calc R . . . .
C38 C 0.7236(5) 1.0902(3) 0.5507(3) 0.0580(15) Uani 1 1 d . . . . .
H38 H 0.6910 1.1232 0.5236 0.070 Uiso 1 1 calc R . . . .
C39 C 0.8216(5) 1.0941(3) 0.5537(3) 0.0598(15) Uani 1 1 d . . . . .
H39 H 0.8541 1.1292 0.5292 0.072 Uiso 1 1 calc R . . . .
C40 C 0.8682(4) 1.0451(3) 0.5933(3) 0.0498(12) Uani 1 1 d . . . . .
H40 H 0.9333 1.0470 0.5964 0.060 Uiso 1 1 calc R . . . .
C41 C 0.8190(3) 0.9919(2) 0.6294(2) 0.0368(10) Uani 1 1 d . . . . .
H41 H 0.8521 0.9589 0.6561 0.044 Uiso 1 1 calc R . . . .
C42 C 0.7225(3) 0.9876(2) 0.6262(2) 0.0388(10) Uani 1 1 d . . . . .
C43 C 0.6752(4) 1.0401(3) 0.5859(2) 0.0464(12) Uani 1 1 d . . . . .
H43 H 0.6099 1.0399 0.5837 0.056 Uiso 1 1 calc R . . . .
C44 C 0.6703(4) 0.9310(3) 0.6606(3) 0.0490(12) Uani 1 1 d . . . . .
H44A H 0.6692 0.8894 0.6311 0.073 Uiso 1 1 calc GR . . . .
H44B H 0.6072 0.9467 0.6693 0.073 Uiso 1 1 calc GR . . . .
H44C H 0.7000 0.9193 0.7043 0.073 Uiso 1 1 calc GR . . . .
C45 C 0.2386(3) 0.7117(2) 0.5298(2) 0.0364(9) Uani 1 1 d . . . . .
H45A H 0.2980 0.7360 0.5291 0.055 Uiso 1 1 calc GR . . . .
H45B H 0.1898 0.7448 0.5420 0.055 Uiso 1 1 calc GR . . . .
H45C H 0.2261 0.6920 0.4843 0.055 Uiso 1 1 calc GR . . . .
C46 C 0.2417(3) 0.6528(2) 0.58258(19) 0.0289(8) Uani 1 1 d . . . . .
C47 C 0.2467(3) 0.5821(2) 0.5616(2) 0.0322(8) Uani 1 1 d . . . . .
H47 H 0.2470 0.5709 0.5142 0.039 Uiso 1 1 calc R . . . .
C48 C 0.2513(4) 0.5278(2) 0.6112(2) 0.0455(10) Uani 1 1 d . . . . .
H48 H 0.2555 0.4805 0.5966 0.055 Uiso 1 1 calc R . . . .
C49 C 0.2498(4) 0.5433(3) 0.6815(2) 0.0482(11) Uani 1 1 d . . . . .
H49 H 0.2530 0.5068 0.7144 0.058 Uiso 1 1 calc R . . . .
C50 C 0.2435(3) 0.6134(3) 0.7026(2) 0.0420(10) Uani 1 1 d . . . . .
H50 H 0.2418 0.6241 0.7502 0.050 Uiso 1 1 calc R . . . .
C51 C 0.2398(3) 0.6678(2) 0.6542(2) 0.0344(9) Uani 1 1 d . . . . .
H51 H 0.2360 0.7150 0.6693 0.041 Uiso 1 1 calc R . . . .


_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 3.9552(9) . ?
K1 O1 2.629(2) . ?
K1 O2 2.635(2) . ?
K1 O9 3.035(3) . ?
K1 O10 2.763(2) . ?
K1 O11 3.011(3) . ?
K1 O12 2.874(3) . ?
K1 O13 3.165(2) . ?
K1 O14 2.940(3) . ?
K1 C30 3.520(4) . ?
K1 C37 3.524(4) . ?
K2 O1 2.696(3) . ?
K2 O2 2.693(3) . ?
K2 O3 2.814(3) . ?
K2 O4 3.015(3) . ?
K2 O5 2.788(3) . ?
K2 O6 3.082(3) . ?
K2 O7 2.872(2) . ?
K2 O8 3.004(3) . ?
K2 C1 3.092(3) . ?
K2 C10 3.266(3) . ?
K2 C13 3.095(4) . ?
K2 C14 3.518(4) . ?
O1 C1 1.294(4) . ?
O2 C13 1.296(4) . ?
O3 C15 1.411(5) . ?
O3 C16 1.414(5) . ?
O4 C17 1.422(5) . ?
O4 C18 1.420(5) . ?
O5 C19 1.419(5) . ?
O5 C20 1.416(5) . ?
O6 C21 1.424(5) . ?
O6 C22 1.419(5) . ?
O7 C23 1.432(5) . ?
O7 C24 1.422(5) . ?
O8 C14 1.422(5) . ?
O8 C25 1.421(5) . ?
O9 C29 1.422(5) . ?
O9 C30 1.425(4) . ?
O10 C27 1.415(4) . ?
O10 C28 1.424(4) . ?
O11 C26 1.420(5) . ?
O11 C37 1.429(4) . ?
O12 C35 1.416(5) . ?
O12 C36 1.427(5) . ?
O13 C33 1.418(5) . ?
O13 C34 1.419(5) . ?
O14 C31 1.428(5) . ?
O14 C32 1.418(5) . ?
C1 C2 1.411(5) . ?
C1 C10 1.463(5) . ?
C2 C3 1.398(5) . ?
C3 C4 1.366(6) . ?
C4 C5 1.486(5) . ?
C4 C9 1.433(5) . ?
C5 C6 1.407(7) . ?
C6 C7 1.394(7) . ?
C7 C8 1.489(5) . ?
C8 C9 1.429(5) . ?
C8 C11 1.370(6) . ?
C9 C10 1.445(4) . ?
C10 C13 1.467(5) . ?
C11 C12 1.394(5) . ?
C12 C13 1.412(5) . ?
C14 C15 1.500(6) . ?
C16 C17 1.487(6) . ?
C18 C19 1.494(6) . ?
C20 C21 1.497(6) . ?
C22 C23 1.494(6) . ?
C24 C25 1.504(6) . ?
C26 C27 1.493(5) . ?
C28 C29 1.496(5) . ?
C30 C31 1.501(6) . ?
C32 C33 1.489(6) . ?
C34 C35 1.500(6) . ?
C36 C37 1.505(5) . ?
C38 C39 1.398(9) . ?
C38 C43 1.343(8) . ?
C39 C40 1.362(8) . ?
C40 C41 1.398(7) . ?
C41 C42 1.378(7) . ?
C42 C43 1.420(7) . ?
C42 C44 1.451(7) . ?
C45 C46 1.495(5) . ?
C46 C47 1.383(5) . ?
C46 C51 1.397(5) . ?
C47 C48 1.391(6) . ?
C48 C49 1.374(7) . ?
C49 C50 1.375(7) . ?
C50 C51 1.378(6) . ?

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 K1 K2 42.69(5) . . ?
O1 K1 O2 63.07(7) . . ?
O1 K1 O9 76.71(7) . . ?
O1 K1 O10 93.61(8) . . ?
O1 K1 O11 129.47(7) . . ?
O1 K1 O12 138.08(8) . . ?
O1 K1 O13 128.46(7) . . ?
O1 K1 O14 86.04(8) . . ?
O1 K1 C30 61.44(8) . . ?
O1 K1 C37 122.85(9) . . ?
O2 K1 K2 42.64(6) . . ?
O2 K1 O9 128.24(7) . . ?
O2 K1 O10 91.53(8) . . ?
O2 K1 O11 75.59(7) . . ?
O2 K1 O12 84.13(8) . . ?
O2 K1 O13 129.83(7) . . ?
O2 K1 O14 142.54(8) . . ?
O2 K1 C30 122.88(9) . . ?
O2 K1 C37 60.61(8) . . ?
O9 K1 K2 118.00(5) . . ?
O9 K1 O13 100.25(7) . . ?
O9 K1 C30 23.65(8) . . ?
O9 K1 C37 135.39(8) . . ?
O10 K1 K2 123.36(5) . . ?
O10 K1 O9 58.61(7) . . ?
O10 K1 O11 58.43(7) . . ?
O10 K1 O12 113.75(8) . . ?
O10 K1 O13 129.20(7) . . ?
O10 K1 O14 112.23(8) . . ?
O10 K1 C30 79.50(9) . . ?
O10 K1 C37 79.11(8) . . ?
O11 K1 K2 116.08(5) . . ?
O11 K1 O9 111.98(7) . . ?
O11 K1 O13 99.88(7) . . ?
O11 K1 C30 135.48(9) . . ?
O11 K1 C37 23.63(8) . . ?
O12 K1 K2 95.52(6) . . ?
O12 K1 O9 144.43(7) . . ?
O12 K1 O11 56.54(7) . . ?
O12 K1 O13 55.41(7) . . ?
O12 K1 O14 109.81(8) . . ?
O12 K1 C30 150.70(9) . . ?
O12 K1 C37 42.17(8) . . ?
O13 K1 K2 107.43(5) . . ?
O13 K1 C30 95.66(8) . . ?
O13 K1 C37 95.63(8) . . ?
O14 K1 K2 100.30(6) . . ?
O14 K1 O9 55.55(7) . . ?
O14 K1 O11 141.36(7) . . ?
O14 K1 O13 54.55(7) . . ?
O14 K1 C30 42.17(8) . . ?
O14 K1 C37 149.20(9) . . ?
C30 K1 K2 98.15(7) . . ?
C30 K1 C37 158.42(9) . . ?
C37 K1 K2 95.92(7) . . ?
O1 K2 O3 78.07(8) . . ?
O1 K2 O4 111.70(7) . . ?
O1 K2 O5 130.76(8) . . ?
O1 K2 O6 134.55(8) . . ?
O1 K2 O7 103.07(7) . . ?
O1 K2 O8 81.83(8) . . ?
O1 K2 C1 24.64(8) . . ?
O1 K2 C10 46.88(8) . . ?
O1 K2 C13 60.94(8) . . ?
O1 K2 C14 63.46(9) . . ?
O2 K2 O1 61.45(7) . . ?
O2 K2 O3 131.26(8) . . ?
O2 K2 O4 112.87(7) . . ?
O2 K2 O5 78.53(8) . . ?
O2 K2 O6 81.50(7) . . ?
O2 K2 O7 101.32(8) . . ?
O2 K2 O8 133.56(8) . . ?
O2 K2 C1 60.93(8) . . ?
O2 K2 C10 46.93(8) . . ?
O2 K2 C13 24.63(8) . . ?
O2 K2 C14 123.30(9) . . ?
O3 K2 O4 56.98(7) . . ?
O3 K2 O6 145.94(8) . . ?
O3 K2 O7 113.97(8) . . ?
O3 K2 O8 56.68(8) . . ?
O3 K2 C1 70.88(9) . . ?
O3 K2 C10 85.94(8) . . ?
O3 K2 C13 112.01(9) . . ?
O3 K2 C14 42.05(9) . . ?
O4 K2 O6 106.25(7) . . ?
O4 K2 C1 88.84(8) . . ?
O4 K2 C10 78.81(7) . . ?
O4 K2 C13 89.72(8) . . ?
O4 K2 C14 98.59(9) . . ?
O5 K2 O3 114.43(8) . . ?
O5 K2 O4 57.55(7) . . ?
O5 K2 O6 56.08(8) . . ?
O5 K2 O7 112.39(8) . . ?
O5 K2 O8 146.12(8) . . ?
O5 K2 C1 111.05(9) . . ?
O5 K2 C10 85.18(8) . . ?
O5 K2 C13 70.65(9) . . ?
O5 K2 C14 154.33(9) . . ?
O6 K2 C1 142.42(9) . . ?
O6 K2 C10 122.11(8) . . ?
O6 K2 C13 95.97(9) . . ?
O6 K2 C14 133.89(9) . . ?
O7 K2 O4 139.59(7) . . ?
O7 K2 O6 57.15(8) . . ?
O7 K2 O8 58.26(8) . . ?
O7 K2 C1 127.69(9) . . ?
O7 K2 C10 141.57(8) . . ?
O7 K2 C13 125.96(9) . . ?
O7 K2 C14 78.75(10) . . ?
O8 K2 O4 106.34(7) . . ?
O8 K2 O6 110.69(7) . . ?
O8 K2 C1 97.02(9) . . ?
O8 K2 C10 123.21(9) . . ?
O8 K2 C13 142.75(9) . . ?
O8 K2 C14 23.53(9) . . ?
C1 K2 C10 26.42(9) . . ?
C1 K2 C13 48.93(9) . . ?
C1 K2 C14 74.55(10) . . ?
C10 K2 C14 100.23(9) . . ?
C13 K2 C10 26.50(9) . . ?
C13 K2 C14 122.75(10) . . ?
K1 O1 K2 95.92(8) . . ?
C1 O1 K1 128.6(2) . . ?
C1 O1 K2 95.07(19) . . ?
K1 O2 K2 95.85(8) . . ?
C13 O2 K1 128.4(2) . . ?
C13 O2 K2 95.32(19) . . ?
C15 O3 K2 121.4(2) . . ?
C15 O3 C16 113.8(3) . . ?
C16 O3 K2 123.3(2) . . ?
C17 O4 K2 106.7(2) . . ?
C18 O4 K2 105.7(2) . . ?
C18 O4 C17 111.2(3) . . ?
C19 O5 K2 123.2(2) . . ?
C20 O5 K2 122.3(2) . . ?
C20 O5 C19 113.2(3) . . ?
C21 O6 K2 95.7(2) . . ?
C22 O6 K2 106.5(2) . . ?
C22 O6 C21 113.2(3) . . ?
C23 O7 K2 120.6(2) . . ?
C24 O7 K2 118.8(2) . . ?
C24 O7 C23 111.7(3) . . ?
C14 O8 K2 99.0(2) . . ?
C25 O8 K2 105.5(2) . . ?
C25 O8 C14 112.3(3) . . ?
C29 O9 K1 100.44(19) . . ?
C29 O9 C30 112.0(3) . . ?
C30 O9 K1 97.62(19) . . ?
C27 O10 K1 122.1(2) . . ?
C27 O10 C28 112.8(2) . . ?
C28 O10 K1 121.7(2) . . ?
C26 O11 K1 102.37(19) . . ?
C26 O11 C37 111.6(3) . . ?
C37 O11 K1 98.7(2) . . ?
C35 O12 K1 125.0(2) . . ?
C35 O12 C36 110.8(3) . . ?
C36 O12 K1 119.9(2) . . ?
C33 O13 K1 111.9(2) . . ?
C33 O13 C34 111.0(3) . . ?
C34 O13 K1 105.6(2) . . ?
C31 O14 K1 118.1(2) . . ?
C32 O14 K1 122.9(2) . . ?
C32 O14 C31 110.8(3) . . ?
O1 C1 K2 60.29(17) . . ?
O1 C1 C2 119.4(3) . . ?
O1 C1 C10 123.4(3) . . ?
C2 C1 K2 129.4(2) . . ?
C2 C1 C10 117.2(3) . . ?
C10 C1 K2 83.44(19) . . ?
C3 C2 C1 122.0(3) . . ?
C4 C3 C2 122.4(3) . . ?
C3 C4 C5 120.8(4) . . ?
C3 C4 C9 119.2(3) . . ?
C9 C4 C5 120.0(4) . . ?
C6 C5 C4 118.9(4) . . ?
C7 C6 C5 122.3(4) . . ?
C6 C7 C8 119.4(4) . . ?
C9 C8 C7 119.7(3) . . ?
C11 C8 C7 121.2(4) . . ?
C11 C8 C9 119.1(3) . . ?
C4 C9 C10 120.0(3) . . ?
C8 C9 C4 119.5(3) . . ?
C8 C9 C10 120.5(3) . . ?
C1 C10 K2 70.13(18) . . ?
C1 C10 C13 122.0(3) . . ?
C9 C10 K2 134.0(2) . . ?
C9 C10 C1 119.3(3) . . ?
C9 C10 C13 118.7(3) . . ?
C13 C10 K2 70.23(18) . . ?
C8 C11 C12 122.2(3) . . ?
C11 C12 C13 122.2(3) . . ?
O2 C13 K2 60.05(17) . . ?
O2 C13 C10 123.1(3) . . ?
O2 C13 C12 119.6(3) . . ?
C10 C13 K2 83.27(19) . . ?
C12 C13 K2 129.4(2) . . ?
C12 C13 C10 117.3(3) . . ?
O8 C14 K2 57.51(18) . . ?
O8 C14 C15 107.8(3) . . ?
C15 C14 K2 86.8(2) . . ?
O3 C15 C14 108.6(3) . . ?
O3 C16 C17 109.2(3) . . ?
O4 C17 C16 108.9(3) . . ?
O4 C18 C19 109.1(3) . . ?
O5 C19 C18 108.8(3) . . ?
O5 C20 C21 108.4(3) . . ?
O6 C21 K2 60.58(17) . . ?
O6 C21 C20 107.1(3) . . ?
C20 C21 K2 86.5(2) . . ?
O6 C22 C23 108.5(3) . . ?
O7 C23 C22 108.6(3) . . ?
O7 C24 C25 108.5(3) . . ?
O8 C25 C24 108.3(3) . . ?
O11 C26 C27 109.0(3) . . ?
O10 C27 C26 107.9(3) . . ?
O10 C28 C29 107.8(3) . . ?
O9 C29 C28 109.0(3) . . ?
O9 C30 K1 58.73(16) . . ?
O9 C30 C31 107.1(3) . . ?
C31 C30 K1 90.0(2) . . ?
O14 C31 C30 109.1(3) . . ?
O14 C32 C33 108.3(3) . . ?
O13 C33 C32 109.2(3) . . ?
O13 C34 C35 109.1(3) . . ?
O12 C35 C34 109.7(3) . . ?
O12 C36 C37 108.5(3) . . ?
O11 C37 K1 57.63(16) . . ?
O11 C37 C36 108.2(3) . . ?
C36 C37 K1 88.4(2) . . ?
C43 C38 C39 121.9(6) . . ?
C40 C39 C38 118.2(6) . . ?
C39 C40 C41 120.6(5) . . ?
C42 C41 C40 121.3(5) . . ?
C41 C42 C43 117.1(5) . . ?
C41 C42 C44 122.3(5) . . ?
C43 C42 C44 120.6(5) . . ?
C38 C43 C42 120.7(5) . . ?
C47 C46 C45 120.7(3) . . ?
C47 C46 C51 118.5(4) . . ?
C51 C46 C45 120.8(4) . . ?
C46 C47 C48 120.3(4) . . ?
C49 C48 C47 120.6(4) . . ?
C48 C49 C50 119.3(4) . . ?
C49 C50 C51 120.7(4) . . ?
C50 C51 C46 120.5(4) . . ?

_olex2_date_sample_data_collection 2019-12-08
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.5
2 0.5

