# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1543967'
_audit_update_record             
;
2017-04-13 deposited with the CCDC.
2017-05-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H9 B Cu2 K O14.50'
_chemical_formula_weight         514.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'

loop_
_symmetry_equiv_pos_as_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                   7.8347(4)
_cell_length_b                   13.3996(9)
_cell_length_c                   14.0216(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1472.01(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4699
_cell_measurement_theta_min      4.1680
_cell_measurement_theta_max      27.7580

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.3280
_exptl_crystal_size_mid          0.0689
_exptl_crystal_size_min          0.0637
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1020
_exptl_absorpt_coefficient_mu    3.257
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.986
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14698
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.34
_diffrn_reflns_theta_max         27.99
_reflns_number_total             3474
_reflns_number_gt                3094
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0353P)²+1.7590P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.467(17)
_refine_ls_number_reflns         3474
_refine_ls_number_parameters     242
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_ref         0.0847
_refine_ls_wR_factor_gt          0.0796
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_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
K1 K 0.2728(2) 0.46274(10) 0.07688(10) 0.0536(4) Uani 1 1 d . . .
Cu1 Cu 0.50396(7) 0.33922(4) 0.26898(4) 0.02038(13) Uani 1 1 d . . .
Cu2 Cu -0.01952(6) 0.09172(4) 0.15545(4) 0.01804(12) Uani 1 1 d . . .
B1 B 0.2583(5) 0.2090(3) 0.2057(4) 0.0170(10) Uani 1 1 d . . .
C1 C 0.1917(5) 0.3988(3) 0.3433(3) 0.0204(8) Uani 1 1 d . . .
C2 C 0.1721(5) 0.2856(3) 0.3506(3) 0.0188(8) Uani 1 1 d . . .
H2A H 0.1683 0.2658 0.4178 0.023 Uiso 1 1 calc R . .
C3 C 0.0119(5) 0.2467(3) 0.2990(3) 0.0218(8) Uani 1 1 d . . .
H3A H -0.0749 0.2993 0.2972 0.026 Uiso 1 1 calc R . .
C4 C -0.0632(5) 0.1536(4) 0.3434(4) 0.0277(10) Uani 1 1 d . . .
C5 C 0.6388(5) 0.1999(3) 0.1347(3) 0.0199(9) Uani 1 1 d . . .
C6 C 0.4645(5) 0.2049(3) 0.0858(3) 0.0185(8) Uani 1 1 d . . .
H6A H 0.4759 0.2252 0.0189 0.022 Uiso 1 1 calc R . .
C7 C 0.3775(5) 0.1013(3) 0.0939(3) 0.0174(8) Uani 1 1 d . . .
H7A H 0.4639 0.0484 0.0925 0.021 Uiso 1 1 calc R . .
C8 C 0.2518(5) 0.0872(3) 0.0123(3) 0.0190(8) Uani 1 1 d . . .
O1 O 0.3290(4) 0.4329(2) 0.3117(3) 0.0281(8) Uani 1 1 d . . .
O2 O 0.0666(4) 0.4489(2) 0.3713(3) 0.0284(8) Uani 1 1 d . . .
O3 O -0.1097(6) 0.1568(3) 0.4270(3) 0.0539(12) Uani 1 1 d . . .
O4 O -0.0803(4) 0.0775(2) 0.2892(3) 0.0272(7) Uani 1 1 d . . .
O5 O 0.6597(4) 0.2429(2) 0.2139(2) 0.0267(7) Uani 1 1 d . . .
O6 O 0.7495(3) 0.1506(2) 0.0918(2) 0.0231(7) Uani 1 1 d . . .
O7 O 0.3166(4) 0.0729(3) -0.0674(3) 0.0341(8) Uani 1 1 d . . .
O8 O 0.0918(3) 0.0944(2) 0.0290(2) 0.0225(6) Uani 1 1 d . . .
O9 O 0.3477(3) 0.2685(2) 0.1356(2) 0.0201(7) Uani 1 1 d . . .
O10 O 0.2979(3) 0.1045(2) 0.1847(2) 0.0179(6) Uani 1 1 d . . .
O11 O 0.3114(3) 0.2370(2) 0.3045(2) 0.0194(6) Uani 1 1 d . . .
O12 O 0.0727(3) 0.2275(2) 0.2040(2) 0.0199(7) Uani 1 1 d . . .
O1W O 0.6063(6) 0.4524(3) 0.2024(3) 0.0510(12) Uani 1 1 d . . .
H1WA H 0.6221 0.5034 0.2374 0.061 Uiso 1 1 d R . .
H1WB H 0.6959 0.4378 0.1712 0.061 Uiso 1 1 d R . .
O2W O 0.6229(5) 0.3308(3) 0.4115(3) 0.0466(10) Uani 1 1 d . . .
H2WA H 0.6664 0.2732 0.4192 0.070 Uiso 1 1 d R . .
H2WB H 0.5472 0.3407 0.4540 0.070 Uiso 1 1 d R . .
O3W O 0.4938(5) 0.6192(3) 0.0596(3) 0.076(3) Uani 0.50 1 d PR . .


_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 O3W 2.730(4) . ?
K1 O9 2.792(3) . ?
K1 O6 2.817(3) 4_455 ?
K1 O4 2.858(4) 3 ?
K1 O3 2.899(4) 3 ?
K1 O8 3.006(3) 4 ?
K1 O1W 3.153(5) . ?
K1 C4 3.238(5) 3 ?
K1 O1 3.346(4) . ?
K1 O2 3.361(4) 2_564 ?
K1 Cu1 3.6434(15) . ?
K1 Cu2 3.7137(15) 4 ?
Cu1 O5 1.936(3) . ?
Cu1 O1 1.952(3) . ?
Cu1 O1W 1.953(4) . ?
Cu1 O11 2.098(3) . ?
Cu1 O2W 2.208(4) . ?
Cu1 O9 2.428(3) . ?
Cu2 O4 1.944(4) . ?
Cu2 O8 1.976(3) . ?
Cu2 O2 1.985(3) 3_545 ?
Cu2 O12 2.073(3) . ?
Cu2 O6 2.167(3) 1_455 ?
Cu2 O10 2.526(3) . ?
Cu2 K1 3.7138(15) 4_455 ?
B1 O9 1.446(6) . ?
B1 O10 1.465(5) . ?
B1 O12 1.475(5) . ?
B1 O11 1.495(6) . ?
C1 O1 1.250(5) . ?
C1 O2 1.251(5) . ?
C1 C2 1.528(6) . ?
C2 O11 1.425(5) . ?
C2 C3 1.540(6) . ?
C3 O12 1.438(5) . ?
C3 C4 1.513(6) . ?
C4 O3 1.229(6) . ?
C4 O4 1.279(6) . ?
C4 K1 3.238(5) 3_545 ?
C5 O6 1.244(5) . ?
C5 O5 1.263(6) . ?
C5 C6 1.530(5) . ?
C6 O9 1.433(5) . ?
C6 C7 1.550(6) . ?
C7 O10 1.419(5) . ?
C7 C8 1.521(6) . ?
C8 O7 1.242(5) . ?
C8 O8 1.279(5) . ?
O2 Cu2 1.985(3) 3 ?
O2 K1 3.361(4) 2_565 ?
O3 K1 2.899(4) 3_545 ?
O4 K1 2.858(4) 3_545 ?
O6 Cu2 2.167(3) 1_655 ?
O6 K1 2.817(3) 4 ?
O8 K1 3.006(3) 4_455 ?

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
O3W K1 O9 127.50(11) . . ?
O3W K1 O6 112.38(11) . 4_455 ?
O9 K1 O6 76.03(10) . 4_455 ?
O3W K1 O4 88.84(10) . 3 ?
O9 K1 O4 114.76(10) . 3 ?
O6 K1 O4 143.88(11) 4_455 3 ?
O3W K1 O3 65.72(12) . 3 ?
O9 K1 O3 159.18(12) . 3 ?
O6 K1 O3 116.07(12) 4_455 3 ?
O4 K1 O3 45.31(10) 3 3 ?
O3W K1 O8 67.95(10) . 4 ?
O9 K1 O8 74.53(9) . 4 ?
O6 K1 O8 60.12(8) 4_455 4 ?
O4 K1 O8 154.22(11) 3 4 ?
O3 K1 O8 125.87(12) 3 4 ?
O3W K1 O1W 63.75(11) . . ?
O9 K1 O1W 67.70(9) . . ?
O6 K1 O1W 119.91(10) 4_455 . ?
O4 K1 O1W 95.41(10) 3 . ?
O3 K1 O1W 114.54(13) 3 . ?
O8 K1 O1W 64.88(10) 4 . ?
O3W K1 C4 75.27(12) . 3 ?
O9 K1 C4 137.81(12) . 3 ?
O6 K1 C4 133.06(12) 4_455 3 ?
O4 K1 C4 23.15(11) 3 3 ?
O3 K1 C4 22.22(11) 3 3 ?
O8 K1 C4 142.50(12) 4 3 ?
O1W K1 C4 105.20(12) . 3 ?
O3W K1 O1 95.49(10) . . ?
O9 K1 O1 64.58(9) . . ?
O6 K1 O1 140.38(9) 4_455 . ?
O4 K1 O1 59.15(9) 3 . ?
O3 K1 O1 100.60(10) 3 . ?
O8 K1 O1 110.25(9) 4 . ?
O1W K1 O1 48.44(9) . . ?
C4 K1 O1 79.72(10) 3 . ?
O3W K1 O2 54.25(10) . 2_564 ?
O9 K1 O2 120.17(9) . 2_564 ?
O6 K1 O2 59.61(9) 4_455 2_564 ?
O4 K1 O2 124.86(9) 3 2_564 ?
O3 K1 O2 80.37(10) 3 2_564 ?
O8 K1 O2 49.83(8) 4 2_564 ?
O1W K1 O2 100.59(10) . 2_564 ?
C4 K1 O2 101.99(11) 3 2_564 ?
O1 K1 O2 146.81(9) . 2_564 ?
O3W K1 Cu1 95.69(9) . . ?
O9 K1 Cu1 41.77(6) . . ?
O6 K1 Cu1 114.08(7) 4_455 . ?
O4 K1 Cu1 91.20(8) 3 . ?
O3 K1 Cu1 129.85(10) 3 . ?
O8 K1 Cu1 80.57(7) 4 . ?
O1W K1 Cu1 32.39(7) . . ?
C4 K1 Cu1 110.83(10) 3 . ?
O1 K1 Cu1 32.08(5) . . ?
O2 K1 Cu1 127.45(7) 2_564 . ?
O3W K1 Cu2 78.18(8) . 4 ?
O9 K1 Cu2 89.05(7) . 4 ?
O6 K1 Cu2 35.51(6) 4_455 4 ?
O4 K1 Cu2 155.98(8) 3 4 ?
O3 K1 Cu2 110.67(9) 3 4 ?
O8 K1 Cu2 32.05(6) 4 4 ?
O1W K1 Cu2 96.76(8) . 4 ?
C4 K1 Cu2 132.86(10) 3 4 ?
O1 K1 Cu2 141.44(6) . 4 ?
O2 K1 Cu2 32.09(5) 2_564 4 ?
Cu1 K1 Cu2 109.96(4) . 4 ?
O5 Cu1 O1 173.18(15) . . ?
O5 Cu1 O1W 93.89(15) . . ?
O1 Cu1 O1W 86.33(15) . . ?
O5 Cu1 O11 96.48(12) . . ?
O1 Cu1 O11 80.90(11) . . ?
O1W Cu1 O11 156.33(17) . . ?
O5 Cu1 O2W 93.49(14) . . ?
O1 Cu1 O2W 92.94(15) . . ?
O1W Cu1 O2W 107.42(17) . . ?
O11 Cu1 O2W 93.14(14) . . ?
O5 Cu1 O9 75.56(12) . . ?
O1 Cu1 O9 97.66(12) . . ?
O1W Cu1 O9 98.15(15) . . ?
O11 Cu1 O9 64.24(11) . . ?
O2W Cu1 O9 152.87(13) . . ?
O5 Cu1 K1 108.73(10) . . ?
O1 Cu1 K1 65.54(11) . . ?
O1W Cu1 K1 59.87(15) . . ?
O11 Cu1 K1 96.59(9) . . ?
O2W Cu1 K1 154.46(11) . . ?
O9 Cu1 K1 49.99(7) . . ?
O4 Cu2 O8 167.24(12) . . ?
O4 Cu2 O2 92.43(14) . 3_545 ?
O8 Cu2 O2 85.99(14) . 3_545 ?
O4 Cu2 O12 81.65(13) . . ?
O8 Cu2 O12 97.15(12) . . ?
O2 Cu2 O12 166.74(13) 3_545 . ?
O4 Cu2 O6 103.19(12) . 1_455 ?
O8 Cu2 O6 89.56(11) . 1_455 ?
O2 Cu2 O6 96.78(13) 3_545 1_455 ?
O12 Cu2 O6 96.13(11) . 1_455 ?
O4 Cu2 O10 95.24(11) . . ?
O8 Cu2 O10 73.14(10) . . ?
O2 Cu2 O10 106.18(11) 3_545 . ?
O12 Cu2 O10 62.88(10) . . ?
O6 Cu2 O10 149.83(11) 1_455 . ?
O4 Cu2 K1 136.01(9) . 4_455 ?
O8 Cu2 K1 53.84(8) . 4_455 ?
O2 Cu2 K1 64.11(11) 3_545 4_455 ?
O12 Cu2 K1 127.82(9) . 4_455 ?
O6 Cu2 K1 49.03(9) 1_455 4_455 ?
O10 Cu2 K1 125.94(7) . 4_455 ?
O9 B1 O10 106.7(3) . . ?
O9 B1 O12 112.0(4) . . ?
O10 B1 O12 111.5(3) . . ?
O9 B1 O11 110.9(3) . . ?
O10 B1 O11 111.5(4) . . ?
O12 B1 O11 104.3(3) . . ?
O1 C1 O2 126.1(4) . . ?
O1 C1 C2 118.2(4) . . ?
O2 C1 C2 115.7(4) . . ?
O11 C2 C1 110.3(3) . . ?
O11 C2 C3 104.9(3) . . ?
C1 C2 C3 112.7(3) . . ?
O12 C3 C4 111.3(3) . . ?
O12 C3 C2 103.0(3) . . ?
C4 C3 C2 113.8(4) . . ?
O3 C4 O4 124.4(5) . . ?
O3 C4 C3 118.6(4) . . ?
O4 C4 C3 117.0(4) . . ?
O3 C4 K1 63.1(3) . 3_545 ?
O4 C4 K1 61.5(2) . 3_545 ?
C3 C4 K1 172.0(3) . 3_545 ?
O6 C5 O5 125.2(4) . . ?
O6 C5 C6 115.4(4) . . ?
O5 C5 C6 119.4(4) . . ?
O9 C6 C5 112.2(3) . . ?
O9 C6 C7 102.5(3) . . ?
C5 C6 C7 108.7(3) . . ?
O10 C7 C8 113.2(3) . . ?
O10 C7 C6 103.4(3) . . ?
C8 C7 C6 109.9(3) . . ?
O7 C8 O8 125.2(4) . . ?
O7 C8 C7 115.5(3) . . ?
O8 C8 C7 119.2(4) . . ?
C1 O1 Cu1 118.6(3) . . ?
C1 O1 K1 106.2(3) . . ?
Cu1 O1 K1 82.37(12) . . ?
C1 O2 Cu2 127.1(3) . 3 ?
C1 O2 K1 99.5(3) . 2_565 ?
Cu2 O2 K1 83.80(11) 3 2_565 ?
C4 O3 K1 94.6(3) . 3_545 ?
C4 O4 Cu2 118.0(3) . . ?
C4 O4 K1 95.4(3) . 3_545 ?
Cu2 O4 K1 144.68(15) . 3_545 ?
C5 O5 Cu1 125.0(3) . . ?
C5 O6 Cu2 125.2(3) . 1_655 ?
C5 O6 K1 137.5(3) . 4 ?
Cu2 O6 K1 95.46(11) 1_655 4 ?
C8 O8 Cu2 126.5(3) . . ?
C8 O8 K1 134.9(3) . 4_455 ?
Cu2 O8 K1 94.10(10) . 4_455 ?
C6 O9 B1 108.2(3) . . ?
C6 O9 Cu1 106.6(2) . . ?
B1 O9 Cu1 86.3(2) . . ?
C6 O9 K1 123.0(2) . . ?
B1 O9 K1 127.7(2) . . ?
Cu1 O9 K1 88.24(9) . . ?
C7 O10 B1 107.6(3) . . ?
C7 O10 Cu2 106.6(2) . . ?
B1 O10 Cu2 83.6(2) . . ?
C2 O11 B1 108.8(3) . . ?
C2 O11 Cu1 111.1(2) . . ?
B1 O11 Cu1 98.3(2) . . ?
C3 O12 B1 110.0(3) . . ?
C3 O12 Cu2 110.2(2) . . ?
B1 O12 Cu2 101.6(2) . . ?
Cu1 O1W K1 87.74(15) . . ?

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
O1W H1WA O10 0.85 1.85 2.687(5) 168.1 3_655
O1W H1WB O7 0.85 1.74 2.532(5) 153.8 4
O2W H2WB O3 0.85 2.07 2.911(6) 168.2 4_556

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.99
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.221
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.103
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1543966'
_audit_update_record             
;
2017-04-13 deposited with the CCDC.
2017-05-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H5 B3 K2 O11'
_chemical_formula_weight         339.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.9959(4)
_cell_length_b                   13.2785(3)
_cell_length_c                   7.9060(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.567(4)
_cell_angle_gamma                90.00
_cell_volume                     1100.51(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3107
_cell_measurement_theta_min      4.2138
_cell_measurement_theta_max      67.1035

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.050
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             680
_exptl_absorpt_coefficient_mu    0.918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.80503
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6603
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         25.15
_reflns_number_total             1972
_reflns_number_gt                1734
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0485P)²+0.5377P] 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         1972
_refine_ls_number_parameters     181
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0337
_refine_ls_wR_factor_ref         0.0923
_refine_ls_wR_factor_gt          0.0876
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_restrained_S_all      1.140
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.45301(5) 0.63822(4) 1.07356(7) 0.02759(17) Uani 1 1 d . . .
K2 K 0.00859(5) 0.61417(4) -0.26881(7) 0.02763(17) Uani 1 1 d . . .
C1 C 0.1260(2) 0.61548(18) 0.1610(3) 0.0218(5) Uani 1 1 d . . .
C2 C 0.1800(2) 0.65583(17) 0.3477(3) 0.0201(5) Uani 1 1 d . . .
H2A H 0.2248 0.7192 0.3443 0.024 Uiso 1 1 calc R . .
C3 C 0.2753(2) 0.57805(17) 0.4583(3) 0.0206(5) Uani 1 1 d . . .
H3A H 0.3490 0.5737 0.4133 0.025 Uiso 1 1 calc R . .
C4 C 0.3203(2) 0.61016(18) 0.6511(3) 0.0203(5) Uani 1 1 d . . .
B1 B -0.0451(3) 0.63758(19) 0.2788(4) 0.0219(5) Uani 1 1 d . . .
B2 B -0.2228(3) 0.54893(19) 0.3619(4) 0.0208(5) Uani 1 1 d . . .
B3 B -0.2556(3) 0.7144(2) 0.2205(4) 0.0232(5) Uani 1 1 d . . .
O1 O 0.18916(18) 0.59652(15) 0.0617(2) 0.0299(4) Uani 1 1 d . . .
O2 O 0.00321(16) 0.60275(13) 0.1225(2) 0.0246(4) Uani 1 1 d . . .
O3 O 0.07466(16) 0.67464(13) 0.4086(2) 0.0236(4) Uani 1 1 d . . .
O4 O 0.22275(16) 0.48147(12) 0.4573(2) 0.0226(4) Uani 1 1 d . . .
O5 O 0.29391(17) 0.54108(13) 0.7511(2) 0.0246(4) Uani 1 1 d . . .
O6 O 0.37283(17) 0.68995(13) 0.7061(2) 0.0272(4) Uani 1 1 d . . .
O7 O -0.34384(18) 0.78735(14) 0.1411(3) 0.0323(4) Uani 1 1 d D . .
H7A H -0.3507 0.8276 0.2163 0.048 Uiso 1 1 calc RD . .
O8 O -0.29950(16) 0.63931(12) 0.3055(2) 0.0233(4) Uani 1 1 d . . .
O9 O -0.09882(16) 0.55680(12) 0.3465(2) 0.0251(4) Uani 1 1 d . . .
O10 O -0.13518(17) 0.71966(12) 0.2111(2) 0.0256(4) Uani 1 1 d . . .
O1W O 0.3830(2) 0.43734(17) 1.1179(3) 0.0470(6) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K1 O6 2.7641(18) 4_576 ?
K1 O8 2.7850(19) 1_656 ?
K1 O1W 2.827(2) . ?
K1 O6 2.8533(19) . ?
K1 O1W 2.863(2) 3_667 ?
K1 O7 2.911(2) 1_656 ?
K1 O5 2.9211(17) . ?
K1 O1 2.927(2) 1_556 ?
K1 B3 3.223(3) 1_656 ?
K1 C4 3.238(2) . ?
K1 K1 4.0768(11) 3_667 ?
K1 K2 4.8296(8) 1_556 ?
K2 O9 2.6237(17) 3_565 ?
K2 O10 2.6910(17) 4_575 ?
K2 O1 2.7738(19) . ?
K2 O4 2.8314(18) 3_565 ?
K2 O3 2.9660(18) 1_554 ?
K2 O9 3.0093(19) 1_554 ?
K2 O2 3.1154(18) . ?
K2 O3 3.1215(18) 4_575 ?
K2 O2 3.1214(19) 3_565 ?
K2 O5 3.2421(19) 1_554 ?
K2 C1 3.251(2) . ?
K2 B2 3.356(3) 1_554 ?
C1 O1 1.221(3) . ?
C1 O2 1.302(3) . ?
C1 C2 1.513(3) . ?
C2 O3 1.405(3) . ?
C2 C3 1.542(3) . ?
C2 H2A 0.9800 . ?
C3 O4 1.406(3) . ?
C3 C4 1.515(3) . ?
C3 H3A 0.9800 . ?
C4 O6 1.222(3) . ?
C4 O5 1.299(3) . ?
B1 O9 1.406(3) . ?
B1 O10 1.462(3) . ?
B1 O3 1.487(3) . ?
B1 O2 1.556(3) . ?
B1 K2 3.371(3) 3_565 ?
B1 K2 3.390(3) 4_576 ?
B1 K2 3.459(3) 1_556 ?
B2 O9 1.408(3) . ?
B2 O8 1.457(3) . ?
B2 O4 1.485(3) 3_566 ?
B2 O5 1.554(3) 3_566 ?
B2 K2 3.356(3) 1_556 ?
B2 K2 3.438(3) 3_565 ?
B3 O10 1.350(3) . ?
B3 O8 1.369(3) . ?
B3 O7 1.381(3) . ?
B3 K1 3.223(3) 1_454 ?
O1 K1 2.927(2) 1_554 ?
O2 K2 3.1213(19) 3_565 ?
O3 K2 2.9661(18) 1_556 ?
O3 K2 3.1215(18) 4_576 ?
O4 B2 1.485(3) 3_566 ?
O4 K2 2.8314(18) 3_565 ?
O5 B2 1.554(3) 3_566 ?
O5 K2 3.2422(19) 1_556 ?
O6 K1 2.7640(18) 4_575 ?
O7 K1 2.911(2) 1_454 ?
O7 H7A 0.8200 . ?
O8 K1 2.7850(19) 1_454 ?
O9 K2 2.6237(17) 3_565 ?
O9 K2 3.0093(19) 1_556 ?
O10 K2 2.6911(17) 4_576 ?
O1W K1 2.863(2) 3_667 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 K1 O8 96.10(5) 4_576 1_656 ?
O6 K1 O1W 126.99(6) 4_576 . ?
O8 K1 O1W 99.90(6) 1_656 . ?
O6 K1 O6 98.71(4) 4_576 . ?
O8 K1 O6 127.54(5) 1_656 . ?
O1W K1 O6 109.96(6) . . ?
O6 K1 O1W 144.45(6) 4_576 3_667 ?
O8 K1 O1W 72.76(6) 1_656 3_667 ?
O1W K1 O1W 88.49(7) . 3_667 ?
O6 K1 O1W 66.21(6) . 3_667 ?
O6 K1 O7 71.58(5) 4_576 1_656 ?
O8 K1 O7 48.13(5) 1_656 1_656 ?
O1W K1 O7 147.31(6) . 1_656 ?
O6 K1 O7 90.41(5) . 1_656 ?
O1W K1 O7 76.37(6) 3_667 1_656 ?
O6 K1 O5 121.33(6) 4_576 . ?
O8 K1 O5 141.79(5) 1_656 . ?
O1W K1 O5 65.03(6) . . ?
O6 K1 O5 45.41(5) . . ?
O1W K1 O5 71.98(6) 3_667 . ?
O7 K1 O5 133.20(6) 1_656 . ?
O6 K1 O1 75.03(6) 4_576 1_556 ?
O8 K1 O1 141.64(5) 1_656 1_556 ?
O1W K1 O1 61.38(6) . 1_556 ?
O6 K1 O1 90.82(5) . 1_556 ?
O1W K1 O1 133.88(7) 3_667 1_556 ?
O7 K1 O1 146.38(6) 1_656 1_556 ?
O5 K1 O1 64.02(5) . 1_556 ?
O6 K1 B3 90.03(6) 4_576 1_656 ?
O8 K1 B3 24.99(6) 1_656 1_656 ?
O1W K1 B3 121.97(7) . 1_656 ?
O6 K1 B3 105.04(6) . 1_656 ?
O1W K1 B3 65.43(7) 3_667 1_656 ?
O7 K1 B3 25.37(6) 1_656 1_656 ?
O5 K1 B3 136.17(6) . 1_656 ?
O1 K1 B3 159.82(6) 1_556 1_656 ?
O6 K1 C4 112.96(6) 4_576 . ?
O8 K1 C4 136.60(6) 1_656 . ?
O1W K1 C4 87.96(7) . . ?
O6 K1 C4 22.01(6) . . ?
O1W K1 C4 64.80(7) 3_667 . ?
O7 K1 C4 110.46(6) 1_656 . ?
O5 K1 C4 23.64(6) . . ?
O1 K1 C4 79.12(6) 1_556 . ?
B3 K1 C4 119.84(7) 1_656 . ?
O6 K1 K1 171.41(5) 4_576 3_667 ?
O8 K1 K1 84.90(4) 1_656 3_667 ?
O1W K1 K1 44.60(5) . 3_667 ?
O6 K1 K1 87.32(4) . 3_667 ?
O1W K1 K1 43.89(5) 3_667 3_667 ?
O7 K1 K1 114.72(4) 1_656 3_667 ?
O5 K1 K1 59.34(4) . 3_667 ?
O1 K1 K1 98.90(4) 1_556 3_667 ?
B3 K1 K1 94.32(5) 1_656 3_667 ?
C4 K1 K1 71.11(4) . 3_667 ?
O6 K1 K2 83.25(4) 4_576 1_556 ?
O8 K1 K2 172.62(4) 1_656 1_556 ?
O1W K1 K2 74.91(5) . 1_556 ?
O6 K1 K2 59.73(4) . 1_556 ?
O1W K1 K2 111.89(5) 3_667 1_556 ?
O7 K1 K2 137.59(4) 1_656 1_556 ?
O5 K1 K2 40.84(4) . 1_556 ?
O1 K1 K2 31.14(4) 1_556 1_556 ?
B3 K1 K2 161.86(5) 1_656 1_556 ?
C4 K1 K2 49.41(4) . 1_556 ?
K1 K1 K2 94.662(19) 3_667 1_556 ?
O9 K2 O10 162.29(6) 3_565 4_575 ?
O9 K2 O1 86.20(6) 3_565 . ?
O10 K2 O1 111.44(6) 4_575 . ?
O9 K2 O4 80.31(5) 3_565 3_565 ?
O10 K2 O4 85.31(5) 4_575 3_565 ?
O1 K2 O4 137.05(6) . 3_565 ?
O9 K2 O3 79.91(5) 3_565 1_554 ?
O10 K2 O3 91.11(5) 4_575 1_554 ?
O1 K2 O3 122.79(5) . 1_554 ?
O4 K2 O3 94.76(5) 3_565 1_554 ?
O9 K2 O9 66.74(6) 3_565 1_554 ?
O10 K2 O9 95.94(5) 4_575 1_554 ?
O1 K2 O9 151.85(5) . 1_554 ?
O4 K2 O9 48.57(5) 3_565 1_554 ?
O3 K2 O9 47.37(5) 1_554 1_554 ?
O9 K2 O2 108.20(5) 3_565 . ?
O10 K2 O2 84.93(5) 4_575 . ?
O1 K2 O2 44.21(5) . . ?
O4 K2 O2 102.57(5) 3_565 . ?
O3 K2 O2 161.81(5) 1_554 . ?
O9 K2 O2 150.67(5) 1_554 . ?
O9 K2 O3 146.04(5) 3_565 4_575 ?
O10 K2 O3 48.91(5) 4_575 4_575 ?
O1 K2 O3 69.47(5) . 4_575 ?
O4 K2 O3 133.61(5) 3_565 4_575 ?
O3 K2 O3 93.38(4) 1_554 4_575 ?
O9 K2 O3 130.43(5) 1_554 4_575 ?
O2 K2 O3 70.69(5) . 4_575 ?
O9 K2 O2 49.41(5) 3_565 3_565 ?
O10 K2 O2 133.56(5) 4_575 3_565 ?
O1 K2 O2 70.78(5) . 3_565 ?
O4 K2 O2 69.51(5) 3_565 3_565 ?
O3 K2 O2 128.10(5) 1_554 3_565 ?
O9 K2 O2 95.37(5) 1_554 3_565 ?
O2 K2 O2 64.64(5) . 3_565 ?
O3 K2 O2 133.84(5) 4_575 3_565 ?
O9 K2 O5 47.44(5) 3_565 1_554 ?
O10 K2 O5 142.27(5) 4_575 1_554 ?
O1 K2 O5 61.45(5) . 1_554 ?
O4 K2 O5 126.42(5) 3_565 1_554 ?
O3 K2 O5 68.78(4) 1_554 1_554 ?
O9 K2 O5 92.99(5) 1_554 1_554 ?
O2 K2 O5 104.21(5) . 1_554 ?
O3 K2 O5 99.01(4) 4_575 1_554 ?
O2 K2 O5 81.59(4) 3_565 1_554 ?
O9 K2 C1 100.99(6) 3_565 . ?
O10 K2 C1 95.63(6) 4_575 . ?
O1 K2 C1 21.58(6) . . ?
O4 K2 C1 124.25(6) 3_565 . ?
O3 K2 C1 140.77(6) 1_554 . ?
O9 K2 C1 165.64(5) 1_554 . ?
O2 K2 C1 23.48(5) . . ?
O3 K2 C1 63.92(5) 4_575 . ?
O2 K2 C1 70.44(5) 3_565 . ?
O5 K2 C1 82.99(5) 1_554 . ?
O9 K2 B2 79.27(6) 3_565 1_554 ?
O10 K2 B2 83.27(6) 4_575 1_554 ?
O1 K2 B2 159.54(6) . 1_554 ?
O4 K2 B2 26.05(6) 3_565 1_554 ?
O3 K2 B2 68.89(6) 1_554 1_554 ?
O9 K2 B2 24.80(6) 1_554 1_554 ?
O2 K2 B2 127.93(6) . 1_554 ?
O3 K2 B2 129.44(6) 4_575 1_554 ?
O2 K2 B2 88.79(6) 3_565 1_554 ?
O5 K2 B2 115.67(6) 1_554 1_554 ?
C1 K2 B2 150.27(7) . 1_554 ?
O1 C1 O2 125.0(2) . . ?
O1 C1 C2 124.6(2) . . ?
O2 C1 C2 110.4(2) . . ?
O1 C1 K2 56.66(13) . . ?
O2 C1 K2 72.42(13) . . ?
C2 C1 K2 159.52(16) . . ?
O3 C2 C1 105.97(19) . . ?
O3 C2 C3 114.48(19) . . ?
C1 C2 C3 108.42(19) . . ?
O3 C2 H2A 109.3 . . ?
C1 C2 H2A 109.3 . . ?
C3 C2 H2A 109.3 . . ?
O4 C3 C4 105.72(18) . . ?
O4 C3 C2 113.58(19) . . ?
C4 C3 C2 109.98(19) . . ?
O4 C3 H3A 109.1 . . ?
C4 C3 H3A 109.1 . . ?
C2 C3 H3A 109.1 . . ?
O6 C4 O5 124.3(2) . . ?
O6 C4 C3 125.3(2) . . ?
O5 C4 C3 110.39(19) . . ?
O6 C4 K1 61.02(13) . . ?
O5 C4 K1 64.39(12) . . ?
C3 C4 K1 168.24(15) . . ?
O9 B1 O10 113.1(2) . . ?
O9 B1 O3 112.1(2) . . ?
O10 B1 O3 111.5(2) . . ?
O9 B1 O2 111.05(19) . . ?
O10 B1 O2 106.66(19) . . ?
O3 B1 O2 101.71(19) . . ?
O9 B1 K2 47.09(11) . 3_565 ?
O10 B1 K2 143.45(17) . 3_565 ?
O3 B1 K2 104.92(14) . 3_565 ?
O2 B1 K2 67.35(11) . 3_565 ?
O9 B1 K2 153.04(17) . 4_576 ?
O10 B1 K2 49.88(11) . 4_576 ?
O3 B1 K2 66.88(12) . 4_576 ?
O2 B1 K2 95.06(13) . 4_576 ?
K2 B1 K2 159.37(9) 3_565 4_576 ?
O9 B1 K2 59.86(12) . 1_556 ?
O10 B1 K2 109.33(15) . 1_556 ?
O3 B1 K2 58.50(11) . 1_556 ?
O2 B1 K2 143.36(15) . 1_556 ?
K2 B1 K2 87.18(6) 3_565 1_556 ?
K2 B1 K2 102.78(7) 4_576 1_556 ?
O9 B2 O8 113.5(2) . . ?
O9 B2 O4 112.6(2) . 3_566 ?
O8 B2 O4 110.5(2) . 3_566 ?
O9 B2 O5 109.9(2) . 3_566 ?
O8 B2 O5 108.23(19) . 3_566 ?
O4 B2 O5 101.39(18) 3_566 3_566 ?
O9 B2 K2 63.68(12) . 1_556 ?
O8 B2 K2 105.69(14) . 1_556 ?
O4 B2 K2 56.84(11) 3_566 1_556 ?
O5 B2 K2 144.70(15) 3_566 1_556 ?
O9 B2 K2 44.37(11) . 3_565 ?
O8 B2 K2 145.48(16) . 3_565 ?
O4 B2 K2 103.51(14) 3_566 3_565 ?
O5 B2 K2 69.59(12) 3_566 3_565 ?
K2 B2 K2 87.74(7) 1_556 3_565 ?
O10 B3 O8 124.2(2) . . ?
O10 B3 O7 120.3(2) . . ?
O8 B3 O7 115.5(2) . . ?
O10 B3 K1 151.77(18) . 1_454 ?
O8 B3 K1 59.28(13) . 1_454 ?
O7 B3 K1 64.59(14) . 1_454 ?
C1 O1 K2 101.76(15) . . ?
C1 O1 K1 133.72(17) . 1_554 ?
K2 O1 K1 115.77(6) . 1_554 ?
C1 O2 B1 110.71(18) . . ?
C1 O2 K2 84.10(13) . . ?
B1 O2 K2 152.61(14) . . ?
C1 O2 K2 100.90(14) . 3_565 ?
B1 O2 K2 85.26(12) . 3_565 ?
K2 O2 K2 115.36(5) . 3_565 ?
C2 O3 B1 110.79(18) . . ?
C2 O3 K2 133.47(14) . 1_556 ?
B1 O3 K2 96.19(13) . 1_556 ?
C2 O3 K2 96.32(12) . 4_576 ?
B1 O3 K2 87.13(12) . 4_576 ?
K2 O3 K2 123.05(6) 1_556 4_576 ?
C3 O4 B2 111.23(17) . 3_566 ?
C3 O4 K2 135.62(14) . 3_565 ?
B2 O4 K2 97.11(13) 3_566 3_565 ?
C4 O5 B2 111.07(18) . 3_566 ?
C4 O5 K1 91.97(13) . . ?
B2 O5 K1 154.95(13) 3_566 . ?
C4 O5 K2 98.59(14) . 1_556 ?
B2 O5 K2 83.71(12) 3_566 1_556 ?
K1 O5 K2 103.06(5) . 1_556 ?
C4 O6 K1 138.70(16) . 4_575 ?
C4 O6 K1 96.97(14) . . ?
K1 O6 K1 123.29(6) 4_575 . ?
B3 O7 K1 90.05(15) . 1_454 ?
B3 O7 H7A 109.5 . . ?
K1 O7 H7A 110.1 1_454 . ?
B3 O8 B2 119.5(2) . . ?
B3 O8 K1 95.73(15) . 1_454 ?
B2 O8 K1 123.89(14) . 1_454 ?
B2 O9 B1 128.19(19) . . ?
B2 O9 K2 113.59(14) . 3_565 ?
B1 O9 K2 109.80(14) . 3_565 ?
B2 O9 K2 91.52(14) . 1_556 ?
B1 O9 K2 96.30(14) . 1_556 ?
K2 O9 K2 113.26(6) 3_565 1_556 ?
B3 O10 B1 120.57(19) . . ?
B3 O10 K2 127.43(15) . 4_576 ?
B1 O10 K2 105.58(14) . 4_576 ?
K1 O1W K1 91.51(7) . 3_667 ?

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
O7 H7A O1W 0.82 2.06 2.877(3) 173.4 2_556

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.15
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.071
