# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_PiCC

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H44 K N4 O11.50'
_chemical_formula_weight         755.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.7592(8)
_cell_length_b                   12.7470(9)
_cell_length_c                   13.3933(9)
_cell_angle_alpha                98.948(4)
_cell_angle_beta                 100.210(4)
_cell_angle_gamma                97.418(3)
_cell_volume                     1926.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    233(2)
_cell_measurement_reflns_used    41860
_cell_measurement_theta_min      1.0
_cell_measurement_theta_max      22.5

_exptl_crystal_description       plate
_exptl_crystal_colour            'light red'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             798
_exptl_absorpt_coefficient_mu    0.202
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      233(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8392
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_sigmaI/netI    0.0726
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.57
_diffrn_reflns_theta_max         21.49
_reflns_number_total             4396
_reflns_number_gt                3127
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  'SHELXTL (Bruker, 1997)'

_refine_special_details          
; 
 The high R-value is caused by a small crystal with low diffraction. Therefore
 data were measured only until 45 degrees in two theta (normal visible
 reflection were only seen until 40 degrees and for refinement only reflection
 down to 43 degrees were used).
 The crystal quality was good and allowed an isotropic refinement of hydrogen
 atoms at nitrogen and oxygen with bond restraints (d(N) = 0.88 angs. and
 d(O) = 0.83 angs.)
 Around the potassium cation all solvent molecules, water and methanole are
 occupational disordered with occupation of 0.5 (C22-O1, C23-O2, O3, O4, O5
 O6 and O7). The disorder is caused by an inversion centre, which bridge two
 potassium cations over the oxygen atoms O1 and O3. The position of O4 and O5
 will be excluded by the position of methanol C23-O1 and O6 and O7 by C22-O1,
 respectively. Because of this disorder hydrogen atoms of solvent could not
 exact localized and were omitted.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0876P)²+1.9892P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4396
_refine_ls_number_parameters     534
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0769
_refine_ls_wR_factor_ref         0.1968
_refine_ls_wR_factor_gt          0.1824
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.109
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
K125 K -0.33619(13) -0.38654(13) 0.55677(11) 0.0750(5) Uani 1 1 d . . .
N21 N -0.5294(4) -0.2229(4) 0.0643(3) 0.0450(12) Uani 1 1 d D . .
H21N H -0.532(3) -0.244(3) 0.123(2) 0.016(11) Uiso 1 1 d D . .
N22 N -0.2425(3) -0.1207(4) 0.2270(3) 0.0389(11) Uani 1 1 d D . .
H22N H -0.301(3) -0.145(4) 0.256(4) 0.052(16) Uiso 1 1 d D . .
N23 N -0.0658(3) 0.1450(4) 0.5286(3) 0.0433(11) Uani 1 1 d . . .
N24 N 0.0983(4) 0.3142(4) 0.6424(4) 0.0492(12) Uani 1 1 d D . .
H24N H 0.083(4) 0.273(4) 0.581(2) 0.053(17) Uiso 1 1 d D . .
O33 O -0.3246(4) -0.2057(4) -0.2959(3) 0.0774(14) Uani 1 1 d D . .
H33O H -0.259(4) -0.176(7) -0.261(6) 0.14(4) Uiso 1 1 d D . .
O82 O 0.1180(3) 0.0548(4) 0.2084(3) 0.0648(12) Uani 1 1 d . . .
O84A O -0.0642(4) 0.2301(4) 0.2943(4) 0.0918(16) Uani 1 1 d . . .
O84B O 0.1097(4) 0.2723(3) 0.4010(3) 0.0672(12) Uani 1 1 d . . .
O102 O -0.7671(4) -0.2326(4) 0.0972(4) 0.0840(15) Uani 1 1 d . . .
O124 O -0.4934(4) -0.3120(4) 0.3958(3) 0.0726(13) Uani 1 1 d . . .
O125 O -0.4368(3) -0.2360(3) 0.2701(3) 0.0595(11) Uani 1 1 d . . .
O191 O 0.2676(4) 0.4184(4) 0.6281(3) 0.0728(13) Uani 1 1 d . . .
C1 C -0.6161(4) -0.1775(5) 0.0122(4) 0.0461(14) Uani 1 1 d . . .
C2 C -0.5722(4) -0.1368(4) -0.0665(4) 0.0432(14) Uani 1 1 d . . .
C3 C -0.4566(4) -0.1587(4) -0.0608(4) 0.0386(13) Uani 1 1 d . . .
C4 C -0.4330(4) -0.2107(4) 0.0218(4) 0.0388(13) Uani 1 1 d . . .
C5 C -0.3244(4) -0.2524(4) 0.0638(4) 0.0431(14) Uani 1 1 d . . .
H5A H -0.2944 -0.2880 0.0059 0.052 Uiso 1 1 calc . . .
H5B H -0.3451 -0.3069 0.1045 0.052 Uiso 1 1 calc . . .
C6 C -0.2280(4) -0.1674(4) 0.1304(4) 0.0399(13) Uani 1 1 d . . .
C7 C -0.1243(4) -0.1215(4) 0.1112(4) 0.0411(14) Uani 1 1 d . . .
C8 C -0.0735(4) -0.0442(4) 0.2005(4) 0.0412(14) Uani 1 1 d . . .
C9 C -0.1479(4) -0.0447(4) 0.2704(4) 0.0360(13) Uani 1 1 d . . .
C10 C -0.1046(4) 0.0337(4) 0.3636(4) 0.0408(14) Uani 1 1 d . . .
C11 C -0.1409(4) 0.0656(4) 0.4530(4) 0.0414(14) Uani 1 1 d . . .
C12 C -0.2497(4) 0.0331(4) 0.4898(4) 0.0430(14) Uani 1 1 d . . .
C13 C -0.2347(4) 0.0907(5) 0.5874(4) 0.0458(14) Uani 1 1 d . . .
C14 C -0.1204(4) 0.1604(5) 0.6075(4) 0.0462(15) Uani 1 1 d . . .
C15 C -0.0714(5) 0.2378(5) 0.7004(4) 0.0523(16) Uani 1 1 d . . .
H15 H -0.1122 0.2400 0.7548 0.063 Uiso 1 1 calc . . .
C16 C 0.0289(4) 0.3072(4) 0.7145(4) 0.0428(14) Uani 1 1 d . . .
C17 C 0.0864(5) 0.3886(5) 0.8050(4) 0.0493(15) Uani 1 1 d . . .
C18 C 0.1864(5) 0.4383(5) 0.7850(4) 0.0492(15) Uani 1 1 d . . .
C19 C 0.1947(5) 0.3929(5) 0.6785(4) 0.0505(15) Uani 1 1 d . . .
C21 C -0.6373(5) -0.0833(5) -0.1455(4) 0.0634(18) Uani 1 1 d . . .
H21A H -0.6521 -0.1296 -0.2127 0.095 Uiso 1 1 calc R . .
H21B H -0.5907 -0.0154 -0.1477 0.095 Uiso 1 1 calc R . .
H21C H -0.7111 -0.0703 -0.1273 0.095 Uiso 1 1 calc R . .
C31 C -0.3782(5) -0.1325(5) -0.1330(4) 0.0502(15) Uani 1 1 d . . .
H31A H -0.2968 -0.1152 -0.0951 0.060 Uiso 1 1 calc . . .
H31B H -0.3984 -0.0691 -0.1608 0.060 Uiso 1 1 calc . . .
C32 C -0.3897(5) -0.2253(6) -0.2203(5) 0.072(2) Uani 1 1 d . . .
H32A H -0.3652 -0.2868 -0.1915 0.087 Uiso 1 1 calc . . .
H32B H -0.4725 -0.2456 -0.2538 0.087 Uiso 1 1 calc . . .
C71 C -0.0714(5) -0.1492(6) 0.0182(4) 0.0650(18) Uani 1 1 d . . .
H71A H -0.1189 -0.2124 -0.0270 0.097 Uiso 1 1 calc R . .
H71B H 0.0072 -0.1637 0.0400 0.097 Uiso 1 1 calc R . .
H71C H -0.0685 -0.0892 -0.0184 0.097 Uiso 1 1 calc R . .
C81 C 0.0313(4) 0.0330(5) 0.2446(4) 0.0442(14) Uani 1 1 d . . .
C82 C 0.0163(4) 0.0880(5) 0.3510(4) 0.0412(14) Uani 1 1 d . . .
H82 H 0.0780 0.0731 0.4050 0.049 Uiso 1 1 calc . . .
C83 C 0.0277(5) 0.2065(5) 0.3546(5) 0.0531(16) Uani 1 1 d . . .
C85 C -0.0609(9) 0.3429(8) 0.2836(10) 0.160(5) Uani 1 1 d . . .
H85A H -0.1328 0.3509 0.2392 0.240 Uiso 1 1 calc . . .
H85B H 0.0053 0.3654 0.2535 0.240 Uiso 1 1 calc . . .
H85C H -0.0531 0.3872 0.3510 0.240 Uiso 1 1 calc . . .
C101 C -0.7315(5) -0.1858(6) 0.0335(5) 0.0622(17) Uani 1 1 d . . .
H101 H -0.7851 -0.1518 -0.0055 0.075 Uiso 1 1 calc . . .
C121 C -0.3522(4) -0.0469(5) 0.4309(4) 0.0467(15) Uani 1 1 d . . .
H12A H -0.3632 -0.0409 0.3579 0.056 Uiso 1 1 calc . . .
H12B H -0.4225 -0.0297 0.4555 0.056 Uiso 1 1 calc . . .
C122 C -0.3392(5) -0.1608(5) 0.4408(4) 0.0532(16) Uani 1 1 d . . .
H12C H -0.3458 -0.1710 0.5107 0.064 Uiso 1 1 calc . . .
H12D H -0.2611 -0.1730 0.4310 0.064 Uiso 1 1 calc . . .
C123 C -0.4305(5) -0.2433(5) 0.3632(5) 0.0536(16) Uani 1 1 d . . .
C131 C -0.3161(5) 0.0883(6) 0.6610(4) 0.0631(18) Uani 1 1 d . . .
H13A H -0.3485 0.1547 0.6678 0.095 Uiso 1 1 calc R . .
H13B H -0.2737 0.0807 0.7279 0.095 Uiso 1 1 calc R . .
H13C H -0.3792 0.0278 0.6353 0.095 Uiso 1 1 calc R . .
C171 C 0.0391(6) 0.4095(6) 0.9011(5) 0.076(2) Uani 1 1 d . . .
H17A H 0.1034 0.4282 0.9604 0.114 Uiso 1 1 calc R . .
H17B H -0.0117 0.3454 0.9069 0.114 Uiso 1 1 calc R . .
H17C H -0.0052 0.4685 0.8984 0.114 Uiso 1 1 calc R . .
C181 C 0.2741(6) 0.5225(5) 0.8544(5) 0.0683(18) Uani 1 1 d . . .
H18A H 0.2538 0.5537 0.9158 0.082 Uiso 1 1 calc . . .
C182 C 0.3753(8) 0.5580(7) 0.8399(6) 0.105(3) Uani 1 1 d . . .
H18B H 0.3998 0.5294 0.7796 0.126 Uiso 1 1 calc . . .
H18C H 0.4254 0.6126 0.8894 0.126 Uiso 1 1 calc . . .
O1 O -0.5999(11) -0.3844(10) 0.5407(11) 0.100(4) Uani 0.50 1 d P . 1
C22 C -0.698(4) -0.345(2) 0.520(3) 0.166(14) Uani 0.50 1 d P . 1
O3 O -0.4957(15) -0.5237(13) 0.3746(14) 0.192(8) Uani 0.50 1 d P . 1
O4 O -0.2004(6) -0.4784(8) 0.7591(9) 0.103(4) Uani 0.50 1 d P . 1
O5 O -0.3645(10) -0.5167(6) 0.8861(6) 0.081(3) Uani 0.50 1 d P A 1
O2 O -0.3590(9) -0.5082(8) 0.7118(8) 0.099(3) Uani 0.50 1 d P . 2
C23 C -0.2973(11) -0.5543(17) 0.8018(10) 0.106(6) Uani 0.50 1 d P . 2
O6 O -0.6787(18) -0.2976(19) 0.5860(17) 0.172(10) Uani 0.50 1 d P B 2
O7 O -0.8493(14) -0.4361(12) 0.4591(13) 0.175(7) Uani 0.50 1 d P . 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K125 O3 2.539(12) 2_446 ?
K125 O191 2.725(4) 2_556 ?
K125 O33 2.763(5) 1_556 ?
K125 O84B 2.783(4) 2_556 ?
K125 O2 2.808(10) . ?
K125 O124 2.941(5) . ?
K125 O1 2.949(12) 2_446 ?
K125 O3 2.955(17) . ?
K125 O1 3.074(13) . ?
K125 O4 3.347(8) . ?
K125 O7 3.347(16) 2_446 ?
K125 C122 3.477(6) . ?
N21 C4 1.358(6) . ?
N21 C1 1.374(7) . ?
N21 H21N 0.878(19) . ?
N22 C9 1.353(6) . ?
N22 C6 1.387(6) . ?
N22 H22N 0.89(2) . ?
N23 C14 1.333(6) . ?
N23 C11 1.401(6) . ?
N24 C19 1.374(7) . ?
N24 C16 1.377(6) . ?
N24 H24N 0.88(2) . ?
O33 C32 1.406(7) . ?
O33 K125 2.763(5) 1_554 ?
O33 H33O 0.84(2) . ?
O82 C81 1.223(6) . ?
O84A C83 1.327(7) . ?
O84A C85 1.463(10) . ?
O84B C83 1.198(7) . ?
O84B K125 2.783(4) 2_556 ?
O102 C101 1.215(7) . ?
O124 C123 1.252(6) . ?
O125 C123 1.255(6) . ?
O191 C19 1.224(6) . ?
O191 K125 2.725(4) 2_556 ?
C1 C2 1.392(7) . ?
C1 C101 1.430(8) . ?
C2 C3 1.414(7) . ?
C2 C21 1.498(8) . ?
C3 C4 1.382(7) . ?
C3 C31 1.494(7) . ?
C4 C5 1.498(7) . ?
C5 C6 1.509(7) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 C7 1.367(7) . ?
C7 C8 1.409(7) . ?
C7 C71 1.502(7) . ?
C8 C9 1.390(7) . ?
C8 C81 1.443(7) . ?
C9 C10 1.439(7) . ?
C10 C11 1.362(7) . ?
C10 C82 1.548(7) . ?
C11 C12 1.484(7) . ?
C12 C13 1.366(7) . ?
C12 C121 1.486(7) . ?
C13 C14 1.469(7) . ?
C13 C131 1.493(7) . ?
C14 C15 1.439(8) . ?
C15 C16 1.345(7) . ?
C15 H15 0.9400 . ?
C16 C17 1.463(7) . ?
C17 C18 1.352(7) . ?
C17 C171 1.491(8) . ?
C18 C181 1.464(8) . ?
C18 C19 1.478(8) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C31 C32 1.502(8) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C71 H71A 0.9700 . ?
C71 H71B 0.9700 . ?
C71 H71C 0.9700 . ?
C81 C82 1.537(7) . ?
C82 C83 1.491(8) . ?
C82 H82 0.9900 . ?
C85 H85A 0.9700 . ?
C85 H85B 0.9700 . ?
C85 H85C 0.9700 . ?
C101 H101 0.9400 . ?
C121 C122 1.503(8) . ?
C121 H12A 0.9800 . ?
C121 H12B 0.9800 . ?
C122 C123 1.520(8) . ?
C122 H12C 0.9800 . ?
C122 H12D 0.9800 . ?
C131 H13A 0.9700 . ?
C131 H13B 0.9700 . ?
C131 H13C 0.9700 . ?
C171 H17A 0.9700 . ?
C171 H17B 0.9700 . ?
C171 H17C 0.9700 . ?
C181 C182 1.276(9) . ?
C181 H18A 0.9400 . ?
C182 H18B 0.9400 . ?
C182 H18C 0.9400 . ?
O1 C22 1.32(5) . ?
O1 K125 2.949(12) 2_446 ?
C22 K125 3.51(4) 2_446 ?
O3 K125 2.539(12) 2_446 ?
O2 C23 1.531(16) . ?
O7 K125 3.347(16) 2_446 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 K125 O191 133.6(4) 2_446 2_556 ?
O3 K125 O33 88.3(4) 2_446 1_556 ?
O191 K125 O33 133.22(14) 2_556 1_556 ?
O3 K125 O84B 147.9(5) 2_446 2_556 ?
O191 K125 O84B 76.06(12) 2_556 2_556 ?
O33 K125 O84B 71.63(13) 1_556 2_556 ?
O3 K125 O2 43.9(6) 2_446 . ?
O191 K125 O2 135.5(3) 2_556 . ?
O33 K125 O2 87.3(2) 1_556 . ?
O84B K125 O2 108.7(2) 2_556 . ?
O3 K125 O124 93.2(5) 2_446 . ?
O191 K125 O124 68.07(13) 2_556 . ?
O33 K125 O124 94.25(15) 1_556 . ?
O84B K125 O124 112.49(12) 2_556 . ?
O2 K125 O124 137.1(2) . . ?
O3 K125 O1 69.5(4) 2_446 2_446 ?
O191 K125 O1 70.1(3) 2_556 2_446 ?
O33 K125 O1 156.6(3) 1_556 2_446 ?
O84B K125 O1 124.1(3) 2_556 2_446 ?
O2 K125 O1 71.6(3) . 2_446 ?
O124 K125 O1 94.5(3) . 2_446 ?
O3 K125 O3 74.5(5) 2_446 . ?
O191 K125 O3 60.0(3) 2_556 . ?
O33 K125 O3 141.5(4) 1_556 . ?
O84B K125 O3 136.1(3) 2_556 . ?
O2 K125 O3 102.1(4) . . ?
O124 K125 O3 53.8(4) . . ?
O1 K125 O3 40.7(5) 2_446 . ?
O3 K125 O1 41.6(6) 2_446 . ?
O191 K125 O1 114.5(3) 2_556 . ?
O33 K125 O1 81.2(3) 1_556 . ?
O84B K125 O1 148.7(3) 2_556 . ?
O2 K125 O1 84.7(4) . . ?
O124 K125 O1 53.4(3) . . ?
O1 K125 O1 86.7(4) 2_446 . ?
O3 K125 O1 62.9(4) . . ?
O3 K125 O4 76.7(5) 2_446 . ?
O191 K125 O4 121.1(2) 2_556 . ?
O33 K125 O4 82.7(2) 1_556 . ?
O84B K125 O4 76.11(15) 2_556 . ?
O2 K125 O4 33.1(2) . . ?
O124 K125 O4 169.56(18) . . ?
O1 K125 O4 84.8(4) 2_446 . ?
O3 K125 O4 124.5(4) . . ?
O1 K125 O4 116.2(3) . . ?
O3 K125 O7 105.8(6) 2_446 2_446 ?
O191 K125 O7 66.4(3) 2_556 2_446 ?
O33 K125 O7 129.9(3) 1_556 2_446 ?
O84B K125 O7 71.9(3) 2_556 2_446 ?
O2 K125 O7 73.3(4) . 2_446 ?
O124 K125 O7 131.3(3) . 2_446 ?
O1 K125 O7 54.3(4) 2_446 2_446 ?
O3 K125 O7 88.4(5) . 2_446 ?
O1 K125 O7 139.3(4) . 2_446 ?
O4 K125 O7 55.9(4) . 2_446 ?
O3 K125 C122 125.6(5) 2_446 . ?
O191 K125 C122 67.92(14) 2_556 . ?
O33 K125 C122 70.25(14) 1_556 . ?
O84B K125 C122 71.51(13) 2_556 . ?
O2 K125 C122 156.5(3) . . ?
O124 K125 C122 42.71(12) . . ?
O1 K125 C122 128.7(3) 2_446 . ?
O3 K125 C122 91.9(4) . . ?
O1 K125 C122 85.0(3) . . ?
O4 K125 C122 142.83(18) . . ?
O7 K125 C122 126.5(3) 2_446 . ?
C4 N21 C1 109.7(4) . . ?
C4 N21 H21N 125(3) . . ?
C1 N21 H21N 124(3) . . ?
C9 N22 C6 108.3(4) . . ?
C9 N22 H22N 128(3) . . ?
C6 N22 H22N 123(3) . . ?
C14 N23 C11 106.0(4) . . ?
C19 N24 C16 111.6(5) . . ?
C19 N24 H24N 125(3) . . ?
C16 N24 H24N 124(3) . . ?
C32 O33 K125 112.8(4) . 1_554 ?
C32 O33 H33O 103(6) . . ?
K125 O33 H33O 118(7) 1_554 . ?
C83 O84A C85 116.7(6) . . ?
C83 O84B K125 156.9(4) . 2_556 ?
C123 O124 K125 106.1(3) . . ?
C19 O191 K125 147.0(4) . 2_556 ?
N21 C1 C2 107.1(4) . . ?
N21 C1 C101 122.5(5) . . ?
C2 C1 C101 130.0(5) . . ?
C1 C2 C3 107.8(5) . . ?
C1 C2 C21 126.1(5) . . ?
C3 C2 C21 126.0(5) . . ?
C4 C3 C2 106.6(4) . . ?
C4 C3 C31 127.6(5) . . ?
C2 C3 C31 125.8(5) . . ?
N21 C4 C3 108.8(4) . . ?
N21 C4 C5 121.2(4) . . ?
C3 C4 C5 130.0(4) . . ?
C4 C5 C6 114.5(4) . . ?
C4 C5 H5A 108.6 . . ?
C6 C5 H5A 108.6 . . ?
C4 C5 H5B 108.6 . . ?
C6 C5 H5B 108.6 . . ?
H5A C5 H5B 107.6 . . ?
C7 C6 N22 110.2(4) . . ?
C7 C6 C5 130.9(5) . . ?
N22 C6 C5 118.8(4) . . ?
C6 C7 C8 105.0(4) . . ?
C6 C7 C71 128.5(5) . . ?
C8 C7 C71 126.5(4) . . ?
C9 C8 C7 109.2(4) . . ?
C9 C8 C81 109.7(4) . . ?
C7 C8 C81 141.1(4) . . ?
N22 C9 C8 107.3(4) . . ?
N22 C9 C10 139.2(4) . . ?
C8 C9 C10 113.4(4) . . ?
C11 C10 C9 137.0(5) . . ?
C11 C10 C82 118.2(5) . . ?
C9 C10 C82 104.8(4) . . ?
C10 C11 N23 117.9(4) . . ?
C10 C11 C12 132.6(5) . . ?
N23 C11 C12 109.6(4) . . ?
C13 C12 C11 105.8(4) . . ?
C13 C12 C121 128.1(5) . . ?
C11 C12 C121 126.0(5) . . ?
C12 C13 C14 106.3(4) . . ?
C12 C13 C131 128.7(5) . . ?
C14 C13 C131 125.0(5) . . ?
N23 C14 C15 122.8(4) . . ?
N23 C14 C13 112.2(5) . . ?
C15 C14 C13 124.9(5) . . ?
C16 C15 C14 124.3(5) . . ?
C16 C15 H15 117.8 . . ?
C14 C15 H15 117.8 . . ?
C15 C16 N24 124.8(5) . . ?
C15 C16 C17 128.9(5) . . ?
N24 C16 C17 106.2(4) . . ?
C18 C17 C16 108.2(5) . . ?
C18 C17 C171 127.8(5) . . ?
C16 C17 C171 123.9(5) . . ?
C17 C18 C181 127.5(5) . . ?
C17 C18 C19 108.3(5) . . ?
C181 C18 C19 124.1(5) . . ?
O191 C19 N24 124.6(5) . . ?
O191 C19 C18 129.8(5) . . ?
N24 C19 C18 105.5(5) . . ?
C2 C21 H21A 109.5 . . ?
C2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C3 C31 C32 111.1(4) . . ?
C3 C31 H31A 109.4 . . ?
C32 C31 H31A 109.4 . . ?
C3 C31 H31B 109.4 . . ?
C32 C31 H31B 109.4 . . ?
H31A C31 H31B 108.0 . . ?
O33 C32 C31 115.2(5) . . ?
O33 C32 H32A 108.5 . . ?
C31 C32 H32A 108.5 . . ?
O33 C32 H32B 108.5 . . ?
C31 C32 H32B 108.5 . . ?
H32A C32 H32B 107.5 . . ?
C7 C71 H71A 109.5 . . ?
C7 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
C7 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
O82 C81 C8 129.3(5) . . ?
O82 C81 C82 123.7(5) . . ?
C8 C81 C82 107.0(4) . . ?
C83 C82 C81 109.3(4) . . ?
C83 C82 C10 114.7(5) . . ?
C81 C82 C10 105.1(4) . . ?
C83 C82 H82 109.2 . . ?
C81 C82 H82 109.2 . . ?
C10 C82 H82 109.2 . . ?
O84B C83 O84A 123.5(6) . . ?
O84B C83 C82 125.9(6) . . ?
O84A C83 C82 110.5(5) . . ?
O84A C85 H85A 109.5 . . ?
O84A C85 H85B 109.5 . . ?
H85A C85 H85B 109.5 . . ?
O84A C85 H85C 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
O102 C101 C1 126.4(6) . . ?
O102 C101 H101 116.8 . . ?
C1 C101 H101 116.8 . . ?
C12 C121 C122 113.2(4) . . ?
C12 C121 H12A 108.9 . . ?
C122 C121 H12A 108.9 . . ?
C12 C121 H12B 108.9 . . ?
C122 C121 H12B 108.9 . . ?
H12A C121 H12B 107.8 . . ?
C121 C122 C123 112.8(5) . . ?
C121 C122 K125 157.2(4) . . ?
C123 C122 K125 78.3(3) . . ?
C121 C122 H12C 109.0 . . ?
C123 C122 H12C 109.0 . . ?
K125 C122 H12C 48.4 . . ?
C121 C122 H12D 109.0 . . ?
C123 C122 H12D 109.0 . . ?
K125 C122 H12D 84.2 . . ?
H12C C122 H12D 107.8 . . ?
O124 C123 O125 125.1(5) . . ?
O124 C123 C122 118.8(5) . . ?
O125 C123 C122 116.1(5) . . ?
O124 C123 K125 53.8(3) . . ?
O125 C123 K125 145.7(4) . . ?
C122 C123 K125 76.5(3) . . ?
C13 C131 H13A 109.5 . . ?
C13 C131 H13B 109.5 . . ?
H13A C131 H13B 109.5 . . ?
C13 C131 H13C 109.5 . . ?
H13A C131 H13C 109.5 . . ?
H13B C131 H13C 109.5 . . ?
C17 C171 H17A 109.5 . . ?
C17 C171 H17B 109.5 . . ?
H17A C171 H17B 109.5 . . ?
C17 C171 H17C 109.5 . . ?
H17A C171 H17C 109.5 . . ?
H17B C171 H17C 109.5 . . ?
C182 C181 C18 126.6(6) . . ?
C182 C181 H18A 116.7 . . ?
C18 C181 H18A 116.7 . . ?
C181 C182 H18B 120.0 . . ?
C181 C182 H18C 120.0 . . ?
H18B C182 H18C 120.0 . . ?
C22 O1 K125 104.0(16) . 2_446 ?
C22 O1 K125 155.1(15) . . ?
K125 O1 K125 93.3(4) 2_446 . ?
O1 C22 K125 54.7(14) . 2_446 ?
K125 O3 K125 105.5(5) 2_446 . ?
C23 O2 K125 147.3(8) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N21 H21N O125 0.878(19) 2.06(3) 2.818(6) 144(3) .
N22 H22N O125 0.89(2) 1.90(3) 2.753(5) 158(5) .
N24 H24N N23 0.88(2) 2.16(4) 2.750(6) 124(4) .
N24 H24N O84B 0.88(2) 2.49(4) 3.224(6) 142(4) .
O33 H33O O82 0.84(2) 2.05(4) 2.839(6) 156(9) 2

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        21.49
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.059

#============================================================================


_database_code_depnum_ccdc_archive 'CCDC 981318'
