# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_exp_2523
_database_code_depnum_ccdc_archive 'CCDC 1031561'
_audit_update_record             
;
2014-10-29 deposited with the CCDC.
2015-02-17 downloaded from the CCDC.
;


#=================================================================
#DATA 1
#================================================================= 

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H5 B K N3'
_chemical_formula_weight         169.04

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'
N N 0.0061 0.0033 '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'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   9.5267(4)
_cell_length_b                   9.9704(5)
_cell_length_c                   10.1727(5)
_cell_angle_alpha                81.041(4)
_cell_angle_beta                 68.165(4)
_cell_angle_gamma                83.636(4)
_cell_volume                     884.51(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4205
_cell_measurement_theta_min      2.2870
_cell_measurement_theta_max      32.5820

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.7050
_exptl_crystal_size_mid          0.4061
_exptl_crystal_size_min          0.2731
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 0 -1 0.1510 0.0001 0.0001 -0.9995 0.0201 0.0720 0.0114
11 -6 5 0.2103 10.9958 -5.9974 4.9977 -0.7084 0.1820 -0.6474
-8 11 -3 0.2109 -7.9964 10.9951 -2.9980 0.9622 -0.2247 0.3395
12 7 7 0.3373 11.9966 6.9967 6.9981 0.1346 -0.0078 -0.9771
8 -10 3 0.1903 7.9965 -9.9955 2.9981 -0.8929 0.2177 -0.3582
-3 13 0 0.1934 -2.9979 12.9941 0.0011 0.9531 -0.2276 -0.0514
-13 -3 -7 0.2102 -12.9959 -2.9985 -6.9978 0.1600 -0.0657 0.9662
-9 1 6 0.1504 -8.9976 0.9983 5.9964 0.1054 -0.8484 0.4877
4 -3 -11 0.1500 3.9992 -2.9971 -10.9945 -0.0561 0.9953 -0.0740
-7 -6 -13 0.2600 -6.9976 -5.9961 -12.9947 -0.0317 0.6603 0.7075
11 6 11 0.3090 10.9965 5.9966 10.9960 0.0022 -0.3344 -0.9401
-3 4 12 0.1475 -2.9995 3.9966 11.9942 0.0878 -1.0289 -0.0200
-1 10 10 0.2162 -0.9994 9.9943 9.9960 0.5089 -0.8360 -0.2371
-1 -12 4 0.3100 -1.0010 -11.9953 3.9967 -0.8946 -0.2494 0.2426
-2 11 -6 0.1934 -1.9980 10.9958 -5.9960 0.9179 0.2642 -0.0095
-9 6 -10 0.2193 -8.9961 5.9981 -9.9951 0.7742 0.2691 0.5767
13 1 9 0.2840 12.9956 0.9992 8.9966 -0.3388 -0.0643 -0.9516
6 12 -1 0.3129 5.9993 11.9952 -0.9978 0.7469 0.2606 -0.5962
-2 0 12 0.1200 -2.0002 -0.0016 11.9939 -0.2068 -0.9554 -0.0091
4 1 -11 0.1507 3.9996 1.0011 -10.9941 0.2211 0.9673 -0.1488
11 4 -3 0.2690 10.9973 3.9992 -2.9973 0.1457 0.6881 -0.7431
6 -8 10 0.1980 5.9968 -7.9974 9.9947 -0.8604 -0.3915 -0.3477
10 -4 11 0.2251 9.9959 -3.9990 10.9949 -0.6732 -0.3097 -0.6893
-13 -1 -10 0.2204 -12.9956 -0.9990 -9.9961 0.3590 0.1364 0.9630
1 -2 13 0.1504 0.9987 -2.0007 12.9934 -0.4179 -0.8770 -0.1747
-9 -3 -14 0.2105 -8.9967 -2.9974 -13.9940 0.2312 0.6204 0.7905
-2 -13 -6 0.3535 -2.0002 -12.9936 -5.9985 -0.7450 0.4325 0.4392
10 -7 -1 0.1974 9.9964 -6.9962 -0.9994 -0.6393 0.5758 -0.4964
13 -2 3 0.2632 12.9957 -1.9988 2.9993 -0.4258 0.3889 -0.8271
-2 -2 12 0.1393 -2.0004 -2.0007 11.9937 -0.3454 -0.9414 0.0283
4 -11 7 0.2462 3.9974 -10.9958 6.9957 -0.9730 -0.2453 -0.1296
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             344
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_min  0.629
_exptl_absorpt_correction_T_max  0.790
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube Enhanced (Mo)'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
'Gemini E Ultra,Xcalibur,2K*2K EOS CCD detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.2705
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10670
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         32.71
_reflns_number_total             5745
_reflns_number_gt                4749
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro171.36.24, Oxford Diffraction'
_computing_cell_refinement       'CrysAlisPro171.36.24, Oxford Diffraction'
_computing_data_reduction        'CrysAlisPro171.36.24, Oxford Diffraction'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond, v.2.1e (Brandenburg, 2001)'
_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)+(0.0297P)²+0.1637P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5745
_refine_ls_number_parameters     233
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.0793
_refine_ls_wR_factor_gt          0.0727
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.027
_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
B1 B 0.13783(14) 0.14006(12) 0.75205(14) 0.0201(2) Uani 1 1 d . . .
C1 C 0.02957(12) 0.01534(11) 0.80622(12) 0.0213(2) Uani 1 1 d . . .
N1 N -0.04448(12) -0.07552(10) 0.83584(12) 0.0291(2) Uani 1 1 d . . .
C2 C 0.28434(13) 0.09416(11) 0.79412(12) 0.0227(2) Uani 1 1 d . . .
N2 N 0.38933(12) 0.06056(11) 0.82260(12) 0.0311(2) Uani 1 1 d . . .
C3 C 0.05509(13) 0.26660(11) 0.83613(13) 0.0231(2) Uani 1 1 d . . .
N3 N 0.00272(13) 0.36013(11) 0.89330(12) 0.0319(2) Uani 1 1 d . . .
C4 C 0.18321(14) 0.17885(12) 0.58018(13) 0.0262(2) Uani 1 1 d . . .
H4A H 0.0897 0.1952 0.5577 0.031 Uiso 1 1 calc R . .
H4B H 0.2375 0.2640 0.5490 0.031 Uiso 1 1 calc R . .
C5 C 0.28108(14) 0.06882(14) 0.49961(13) 0.0306(3) Uani 1 1 d . . .
H5 H 0.3867 0.0692 0.4798 0.037 Uiso 1 1 calc R . .
C6 C 0.23641(19) -0.02856(16) 0.45322(15) 0.0427(3) Uani 1 1 d . . .
H6A H 0.1320 -0.0336 0.4702 0.051 Uiso 1 1 calc R . .
H6B H 0.3086 -0.0939 0.4027 0.051 Uiso 1 1 calc R . .
B2 B 0.36509(18) 0.56321(16) 0.25482(18) 0.0226(3) Uani 0.896(3) 1 d PD A 1
C7 C 0.30250(18) 0.4499(2) 0.19879(17) 0.0231(4) Uani 0.896(3) 1 d PD A 1
N7 N 0.2625(3) 0.3654(2) 0.1593(2) 0.0304(5) Uani 0.896(3) 1 d PD . 1
C8 C 0.3574(3) 0.7069(2) 0.1623(3) 0.0247(3) Uani 0.896(3) 1 d PD A 1
N8 N 0.3602(2) 0.81162(16) 0.0975(2) 0.0313(4) Uani 0.896(3) 1 d PD . 1
C9 C 0.2559(2) 0.5758(2) 0.4155(2) 0.0309(3) Uani 0.896(3) 1 d PD A 1
N9 N 0.1807(2) 0.58626(19) 0.53137(17) 0.0474(4) Uani 0.896(3) 1 d PD A 1
C10 C 0.54053(16) 0.52164(14) 0.23946(18) 0.0293(3) Uani 0.896(3) 1 d PD A 1
H10A H 0.6038 0.5236 0.1369 0.035 Uiso 0.896(3) 1 calc PR A 1
H10B H 0.5766 0.5906 0.2780 0.035 Uiso 0.896(3) 1 calc PR A 1
C11 C 0.56223(16) 0.38485(15) 0.31468(16) 0.0308(3) Uani 0.896(3) 1 d PD A 1
H11 H 0.5310 0.3765 0.4157 0.037 Uiso 0.896(3) 1 calc PR A 1
C12 C 0.6213(2) 0.27417(18) 0.2528(3) 0.0386(4) Uani 0.896(3) 1 d PD A 1
H12A H 0.6540 0.2780 0.1520 0.046 Uiso 0.896(3) 1 calc PR A 1
H12B H 0.6310 0.1907 0.3091 0.046 Uiso 0.896(3) 1 calc PR A 1
B3 B 0.3367(11) 0.5564(12) 0.2907(12) 0.0226(3) Uani 0.104(3) 1 d PD A 2
C17 C 0.2777(18) 0.4432(19) 0.2300(19) 0.0231(4) Uani 0.104(3) 1 d PD A 2
N17 N 0.244(4) 0.355(2) 0.191(3) 0.0304(5) Uani 0.104(3) 1 d PD . 2
C18 C 0.2116(15) 0.594(2) 0.4365(16) 0.0309(3) Uani 0.104(3) 1 d PD A 2
N18 N 0.1238(18) 0.6247(19) 0.5409(14) 0.0474(4) Uani 0.104(3) 1 d PD A 2
C19 C 0.360(3) 0.6893(19) 0.176(2) 0.0247(3) Uani 0.104(3) 1 d PD A 2
N19 N 0.388(2) 0.7845(17) 0.095(2) 0.0313(4) Uani 0.104(3) 1 d PD . 2
C20 C 0.4929(11) 0.4978(11) 0.3145(12) 0.027(3) Uiso 0.104(3) 1 d PD A 2
H20A H 0.5406 0.5739 0.3306 0.032 Uiso 0.104(3) 1 calc PR A 2
H20B H 0.4675 0.4315 0.4020 0.032 Uiso 0.104(3) 1 calc PR A 2
C21 C 0.6047(11) 0.4310(10) 0.1945(12) 0.031(3) Uiso 0.104(3) 1 d PD A 2
H21 H 0.6502 0.4877 0.1076 0.038 Uiso 0.104(3) 1 calc PR A 2
C22 C 0.6470(16) 0.3010(11) 0.1966(16) 0.029(3) Uiso 0.104(3) 1 d PD A 2
H22A H 0.6048 0.2402 0.2810 0.035 Uiso 0.104(3) 1 calc PR A 2
H22B H 0.7199 0.2679 0.1137 0.035 Uiso 0.104(3) 1 calc PR A 2
K1 K 0.04473(3) 0.64280(2) 0.81043(3) 0.02549(7) Uani 1 1 d . . .
K2 K 0.35694(3) 0.09326(2) 0.12437(3) 0.02387(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
B1 C3 1.5997(17) . ?
B1 C1 1.6005(16) . ?
B1 C2 1.6070(16) . ?
B1 C4 1.6301(17) . ?
C1 N1 1.1436(14) . ?
N1 K1 2.8653(11) 1_545 ?
N1 K2 2.8729(10) 2_556 ?
C2 N2 1.1435(15) . ?
N2 K2 2.8943(11) 2_656 ?
N2 K2 3.0347(12) 1_556 ?
C3 N3 1.1431(15) . ?
N3 K1 2.8412(11) . ?
N3 K1 2.8724(11) 2_567 ?
C4 C5 1.4932(18) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.3152(19) . ?
C5 H5 0.9500 . ?
C6 H6A 0.9500 . ?
C6 H6B 0.9500 . ?
B2 C9 1.593(2) . ?
B2 C8 1.597(2) . ?
B2 C7 1.5999(18) . ?
B2 C10 1.632(2) . ?
C7 N7 1.1430(17) . ?
N7 K2 2.796(3) . ?
N7 K1 2.836(3) 2_566 ?
C8 N8 1.1424(19) . ?
N8 K2 2.8590(19) 1_565 ?
N8 K2 2.9377(19) 2_665 ?
C9 N9 1.144(2) . ?
N9 K1 2.7669(17) . ?
C10 C11 1.489(2) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.321(2) . ?
C11 H11 0.9500 . ?
C12 H12A 0.9500 . ?
C12 H12B 0.9500 . ?
B3 C18 1.587(7) . ?
B3 C19 1.598(8) . ?
B3 C17 1.608(7) . ?
B3 C20 1.627(8) . ?
C17 N17 1.138(8) . ?
N17 K1 2.76(3) 2_566 ?
N17 K2 2.80(3) . ?
C18 N18 1.143(8) . ?
N18 K1 2.589(13) . ?
C19 N19 1.142(8) . ?
N19 K2 2.853(18) 2_665 ?
N19 K2 3.110(19) 1_565 ?
C20 C21 1.483(8) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.312(8) . ?
C21 H21 0.9500 . ?
C22 H22A 0.9500 . ?
C22 H22B 0.9500 . ?
K1 N17 2.76(3) 2_566 ?
K1 N7 2.836(3) 2_566 ?
K1 N1 2.8653(11) 1_565 ?
K1 N3 2.8724(11) 2_567 ?
K2 N19 2.853(18) 2_665 ?
K2 N8 2.8590(19) 1_545 ?
K2 N1 2.8729(10) 2_556 ?
K2 N2 2.8943(11) 2_656 ?
K2 N8 2.9377(19) 2_665 ?
K2 N2 3.0347(12) 1_554 ?
K2 N19 3.110(19) 1_545 ?

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
C3 B1 C1 109.80(9) . . ?
C3 B1 C2 106.60(9) . . ?
C1 B1 C2 107.53(9) . . ?
C3 B1 C4 111.68(9) . . ?
C1 B1 C4 109.32(9) . . ?
C2 B1 C4 111.79(9) . . ?
N1 C1 B1 175.50(12) . . ?
C1 N1 K1 129.15(9) . 1_545 ?
C1 N1 K2 131.80(9) . 2_556 ?
K1 N1 K2 96.86(3) 1_545 2_556 ?
N2 C2 B1 179.12(13) . . ?
C2 N2 K2 164.67(9) . 2_656 ?
C2 N2 K2 115.29(9) . 1_556 ?
K2 N2 K2 73.18(3) 2_656 1_556 ?
N3 C3 B1 176.56(12) . . ?
C3 N3 K1 132.63(10) . . ?
C3 N3 K1 120.85(9) . 2_567 ?
K1 N3 K1 97.25(3) . 2_567 ?
C5 C4 B1 111.96(9) . . ?
C5 C4 H4A 109.2 . . ?
B1 C4 H4A 109.2 . . ?
C5 C4 H4B 109.2 . . ?
B1 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C6 C5 C4 126.83(13) . . ?
C6 C5 H5 116.6 . . ?
C4 C5 H5 116.6 . . ?
C5 C6 H6A 120.0 . . ?
C5 C6 H6B 120.0 . . ?
H6A C6 H6B 120.0 . . ?
C9 B2 C8 107.91(12) . . ?
C9 B2 C7 107.63(11) . . ?
C8 B2 C7 109.71(12) . . ?
C9 B2 C10 112.78(12) . . ?
C8 B2 C10 109.14(13) . . ?
C7 B2 C10 109.62(11) . . ?
N7 C7 B2 177.2(2) . . ?
C7 N7 K2 134.7(2) . . ?
C7 N7 K1 121.5(2) . 2_566 ?
K2 N7 K1 99.32(5) . 2_566 ?
N8 C8 B2 175.5(3) . . ?
C8 N8 K2 140.6(2) . 1_565 ?
C8 N8 K2 120.78(17) . 2_665 ?
K2 N8 K2 75.16(5) 1_565 2_665 ?
N9 C9 B2 178.16(19) . . ?
C9 N9 K1 168.35(16) . . ?
C11 C10 B2 113.69(11) . . ?
C11 C10 H10A 108.8 . . ?
B2 C10 H10A 108.8 . . ?
C11 C10 H10B 108.8 . . ?
B2 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
C12 C11 C10 125.52(16) . . ?
C12 C11 H11 117.2 . . ?
C10 C11 H11 117.2 . . ?
C11 C12 H12A 120.0 . . ?
C11 C12 H12B 120.0 . . ?
H12A C12 H12B 120.0 . . ?
C18 B3 C19 108.0(6) . . ?
C18 B3 C17 110.0(7) . . ?
C19 B3 C17 106.8(7) . . ?
C18 B3 C20 110.4(6) . . ?
C19 B3 C20 112.5(7) . . ?
C17 B3 C20 109.1(6) . . ?
N17 C17 B3 174(2) . . ?
C17 N17 K1 119(2) . 2_566 ?
C17 N17 K2 139(3) . . ?
K1 N17 K2 101.3(4) 2_566 . ?
N18 C18 B3 177.6(19) . . ?
C18 N18 K1 150.1(17) . . ?
N19 C19 B3 174(2) . . ?
C19 N19 K2 139.9(18) . 2_665 ?
C19 N19 K2 133(2) . 1_565 ?
K2 N19 K2 72.6(4) 2_665 1_565 ?
C21 C20 B3 114.6(7) . . ?
C21 C20 H20A 108.6 . . ?
B3 C20 H20A 108.6 . . ?
C21 C20 H20B 108.6 . . ?
B3 C20 H20B 108.6 . . ?
H20A C20 H20B 107.6 . . ?
C22 C21 C20 126.3(10) . . ?
C22 C21 H21 116.8 . . ?
C20 C21 H21 116.8 . . ?
C21 C22 H22A 120.0 . . ?
C21 C22 H22B 120.0 . . ?
H22A C22 H22B 120.0 . . ?
N18 K1 N17 83.4(7) . 2_566 ?
N18 K1 N9 12.6(4) . . ?
N17 K1 N9 93.4(5) 2_566 . ?
N18 K1 N7 89.1(4) . 2_566 ?
N17 K1 N7 6.3(6) 2_566 2_566 ?
N9 K1 N7 98.79(6) . 2_566 ?
N18 K1 N3 94.0(4) . . ?
N17 K1 N3 82.4(5) 2_566 . ?
N9 K1 N3 87.82(5) . . ?
N7 K1 N3 79.49(6) 2_566 . ?
N18 K1 N1 104.6(4) . 1_565 ?
N17 K1 N1 80.7(5) 2_566 1_565 ?
N9 K1 N1 113.84(5) . 1_565 ?
N7 K1 N1 81.60(5) 2_566 1_565 ?
N3 K1 N1 153.19(3) . 1_565 ?
N18 K1 N3 171.6(4) . 2_567 ?
N17 K1 N3 103.7(5) 2_566 2_567 ?
N9 K1 N3 159.07(5) . 2_567 ?
N7 K1 N3 97.80(5) 2_566 2_567 ?
N3 K1 N3 82.75(3) . 2_567 ?
N1 K1 N3 81.17(3) 1_565 2_567 ?
N17 K2 N7 6.5(5) . . ?
N17 K2 N19 87.6(6) . 2_665 ?
N7 K2 N19 81.9(4) . 2_665 ?
N17 K2 N8 159.6(5) . 1_545 ?
N7 K2 N8 162.64(7) . 1_545 ?
N19 K2 N8 110.4(4) 2_665 1_545 ?
N17 K2 N1 79.9(6) . 2_556 ?
N7 K2 N1 82.15(6) . 2_556 ?
N19 K2 N1 135.3(4) 2_665 2_556 ?
N8 K2 N1 80.49(4) 1_545 2_556 ?
N17 K2 N2 127.3(6) . 2_656 ?
N7 K2 N2 128.00(6) . 2_656 ?
N19 K2 N2 77.2(4) 2_665 2_656 ?
N8 K2 N2 68.24(5) 1_545 2_656 ?
N1 K2 N2 142.45(3) 2_556 2_656 ?
N17 K2 N8 93.7(5) . 2_665 ?
N7 K2 N8 88.10(5) . 2_665 ?
N19 K2 N8 6.8(3) 2_665 2_665 ?
N8 K2 N8 104.84(5) 1_545 2_665 ?
N1 K2 N8 139.75(5) 2_556 2_665 ?
N2 K2 N8 71.01(4) 2_656 2_665 ?
N17 K2 N2 111.6(5) . 1_554 ?
N7 K2 N2 106.26(5) . 1_554 ?
N19 K2 N2 65.0(5) 2_665 1_554 ?
N8 K2 N2 70.08(5) 1_545 1_554 ?
N1 K2 N2 80.05(3) 2_556 1_554 ?
N2 K2 N2 106.82(3) 2_656 1_554 ?
N8 K2 N2 65.40(5) 2_665 1_554 ?
N17 K2 N19 163.9(7) . 1_545 ?
N7 K2 N19 167.4(4) . 1_545 ?
N19 K2 N19 107.4(4) 2_665 1_545 ?
N8 K2 N19 4.8(4) 1_545 1_545 ?
N1 K2 N19 85.3(4) 2_556 1_545 ?
N2 K2 N19 63.6(4) 2_656 1_545 ?
N8 K2 N19 101.6(4) 2_665 1_545 ?
N2 K2 N19 71.4(4) 1_554 1_545 ?

_diffrn_measured_fraction_theta_max 0.882
_diffrn_reflns_theta_full        26.40
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.047
####################################################################### 
# 
# 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_KEtBCN3_THF
_database_code_depnum_ccdc_archive 'CCDC 1039991'
_audit_update_record             
;
2014-12-17 deposited with the CCDC.
2015-02-17 downloaded from the CCDC.
;


#=================================================================
#DATA 1
#=================================================================  

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H36 B4 K4 N12 O2'
_chemical_formula_sum            'C28 H36 B4 K4 N12 O2'
_chemical_formula_weight         772.32


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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   7.5693(15)
_cell_length_b                   25.062(5)
_cell_length_c                   22.116(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.30(3)
_cell_angle_gamma                90
_cell_volume                     4183.6(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6551
_cell_measurement_theta_min      2.888
_cell_measurement_theta_max      26.144

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_F_000             1600
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    0.466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_process_details   'SadAbs-2008/1 (Bruker, 2008)'

_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            49858
_diffrn_reflns_av_unetI/netI     0.0960
_diffrn_reflns_av_R_equivalents  0.1903
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.230
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8232
_reflns_number_gt                4947
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Smart-NT v. 5.63'
_computing_cell_refinement       'Saint-NT v. 7.23'
_computing_data_reduction        'Saint-NT v. 7.23'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP in ShelxTL-97'
_computing_publication_material  'XP in ShelxTL-97'

_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     
'w=1/[σ²(Fo²)+(0.0027P)²+7.3800P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8232
_refine_ls_number_parameters     455
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0626
_refine_ls_wR_factor_ref         0.1591
_refine_ls_wR_factor_gt          0.1446
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_restrained_S_all      0.917
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 1.01391(9) 0.32919(3) 0.55578(3) 0.02707(18) Uani 1 1 d . . . . .
K2 K 0.97584(9) 0.16945(3) 0.46498(3) 0.02889(19) Uani 1 1 d . . . . .
K3 K 1.47576(10) 0.07935(3) 0.46188(4) 0.0320(2) Uani 1 1 d . . . . .
K4 K 0.51477(9) 0.42050(3) 0.55124(3) 0.02705(18) Uani 1 1 d . . . . .
B1 B 0.4737(5) 0.27406(13) 0.40749(16) 0.0219(8) Uani 1 1 d . . . . .
C1 C 0.2787(4) 0.27059(12) 0.43118(14) 0.0246(7) Uani 1 1 d . . . . .
N1 N 0.1379(4) 0.26847(11) 0.44644(13) 0.0321(7) Uani 1 1 d . . . . .
C2 C 0.5936(4) 0.30965(12) 0.45386(14) 0.0237(7) Uani 1 1 d . . . . .
N2 N 0.6806(4) 0.33550(11) 0.48601(13) 0.0309(7) Uani 1 1 d . . . . .
C3 C 0.5550(4) 0.21494(13) 0.40899(14) 0.0249(7) Uani 1 1 d . . . . .
N3 N 0.6155(4) 0.17320(11) 0.40927(13) 0.0338(7) Uani 1 1 d . . . . .
C4 C 0.4676(4) 0.29810(13) 0.33923(14) 0.0261(7) Uani 1 1 d . . . . .
H4A H 0.5874 0.3003 0.3266 0.031 Uiso 1 1 calc R U . . .
H4B H 0.4014 0.2739 0.3118 0.031 Uiso 1 1 calc R U . . .
C5 C 0.3823(5) 0.35335(14) 0.33440(16) 0.0368(9) Uani 1 1 d . . . . .
H5A H 0.3849 0.3663 0.2936 0.055 Uiso 1 1 calc R U . . .
H5B H 0.4466 0.3774 0.3617 0.055 Uiso 1 1 calc R U . . .
H5C H 0.2616 0.3510 0.3448 0.055 Uiso 1 1 calc R U . . .
B2 B 1.9753(5) -0.02215(14) 0.39622(16) 0.0243(8) Uani 1 1 d . . . . .
C6 C 1.7809(5) -0.01973(12) 0.42003(14) 0.0258(7) Uani 1 1 d . . . . .
N4 N 1.6411(4) -0.01851(11) 0.43594(13) 0.0340(7) Uani 1 1 d . . . . .
C7 C 2.0964(4) -0.05846(12) 0.44217(14) 0.0255(7) Uani 1 1 d . . . . .
N5 N 2.1868(4) -0.08438(12) 0.47380(13) 0.0348(7) Uani 1 1 d . . . . .
C8 C 2.0559(4) 0.03719(13) 0.40046(14) 0.0263(7) Uani 1 1 d . . . . .
N6 N 2.1162(4) 0.07906(11) 0.40320(13) 0.0353(7) Uani 1 1 d . . . . .
C9 C 1.9724(4) -0.04544(13) 0.32820(14) 0.0287(8) Uani 1 1 d . . . . .
H9A H 1.9072 -0.0210 0.3008 0.034 Uiso 1 1 calc R U . . .
H9B H 2.0929 -0.0475 0.3162 0.034 Uiso 1 1 calc R U . . .
C10 C 1.8876(5) -0.10069(14) 0.32218(16) 0.0357(8) Uani 1 1 d . . . . .
H10A H 1.8964 -0.1138 0.2817 0.054 Uiso 1 1 calc R U . . .
H10B H 1.7651 -0.0983 0.3304 0.054 Uiso 1 1 calc R U . . .
H10C H 1.9480 -0.1246 0.3506 0.054 Uiso 1 1 calc R U . . .
B3 B 0.5226(5) 0.21929(14) 0.60696(16) 0.0236(8) Uani 1 1 d . . . . .
C11 C 0.4423(4) 0.27835(13) 0.60417(14) 0.0262(7) Uani 1 1 d . . . . .
N7 N 0.3831(4) 0.32020(11) 0.60188(13) 0.0344(7) Uani 1 1 d . . . . .
C12 C 0.4007(4) 0.18355(12) 0.56094(14) 0.0243(7) Uani 1 1 d . . . . .
N8 N 0.3108(4) 0.15767(11) 0.52942(13) 0.0335(7) Uani 1 1 d . . . . .
C13 C 0.7175(4) 0.22182(12) 0.58253(14) 0.0250(7) Uani 1 1 d . . . . .
N9 N 0.8570(4) 0.22350(11) 0.56662(14) 0.0339(7) Uani 1 1 d . . . . .
C14 C 0.5291(4) 0.19417(13) 0.67404(14) 0.0276(7) Uani 1 1 d . . . . .
H14A H 0.5954 0.2179 0.7019 0.033 Uiso 1 1 calc R U . . .
H14B H 0.4093 0.1918 0.6867 0.033 Uiso 1 1 calc R U . . .
C15 C 0.6137(5) 0.13887(14) 0.67811(16) 0.0377(9) Uani 1 1 d . . . . .
H15A H 0.5492 0.1152 0.6504 0.057 Uiso 1 1 calc R U . . .
H15B H 0.6107 0.1255 0.7187 0.057 Uiso 1 1 calc R U . . .
H15C H 0.7344 0.1412 0.6678 0.057 Uiso 1 1 calc R U . . .
B4 B 0.0263(5) 0.53237(14) 0.59602(16) 0.0238(8) Uani 1 1 d . . . . .
C16 C 0.2200(5) 0.52846(12) 0.57165(14) 0.0251(7) Uani 1 1 d . . . . .
N10 N 0.3600(4) 0.52618(11) 0.55581(13) 0.0336(7) Uani 1 1 d . . . . .
C17 C -0.0560(4) 0.47338(13) 0.59612(14) 0.0248(7) Uani 1 1 d . . . . .
N11 N -0.1174(4) 0.43164(11) 0.59686(13) 0.0344(7) Uani 1 1 d . . . . .
C18 C -0.0958(4) 0.56721(12) 0.54842(14) 0.0241(7) Uani 1 1 d . . . . .
N12 N -0.1834(4) 0.59270(11) 0.51591(13) 0.0313(7) Uani 1 1 d . . . . .
C19 C 0.0320(4) 0.55925(12) 0.66242(14) 0.0272(7) Uani 1 1 d . . . . .
H19A H -0.0879 0.5618 0.6749 0.033 Uiso 1 1 calc R U . . .
H19B H 0.0988 0.5363 0.6911 0.033 Uiso 1 1 calc R U . . .
C20 C 0.1152(5) 0.61453(14) 0.66466(16) 0.0363(9) Uani 1 1 d . . . . .
H20A H 0.2356 0.6121 0.6541 0.054 Uiso 1 1 calc R U . . .
H20B H 0.1128 0.6288 0.7049 0.054 Uiso 1 1 calc R U . . .
H20C H 0.0496 0.6375 0.6364 0.054 Uiso 1 1 calc R U . . .
O1 O 0.4806(5) 0.43875(14) 0.67427(15) 0.0855(12) Uani 1 1 d . . . . .
C21 C 0.3625(9) 0.4145(2) 0.7127(3) 0.102(2) Uani 1 1 d . . . . .
H21A H 0.3722 0.3760 0.7102 0.122 Uiso 1 1 calc R U . . .
H21B H 0.2416 0.4245 0.6999 0.122 Uiso 1 1 calc R U . . .
C22 C 0.4067(14) 0.4322(4) 0.7759(4) 0.178(4) Uani 1 1 d . . . . .
H22A H 0.3001 0.4390 0.7964 0.214 Uiso 1 1 calc R U . . .
H22B H 0.4772 0.4056 0.7985 0.214 Uiso 1 1 calc R U . . .
C23 C 0.5019(11) 0.4785(4) 0.7702(4) 0.167(4) Uani 1 1 d . U . . .
H23A H 0.6038 0.4789 0.7995 0.200 Uiso 1 1 calc R U . . .
H23B H 0.4286 0.5092 0.7775 0.200 Uiso 1 1 calc R U . . .
C24 C 0.5607(9) 0.4805(2) 0.7079(3) 0.099(2) Uani 1 1 d . . . . .
H24A H 0.5274 0.5144 0.6891 0.119 Uiso 1 1 calc R U . . .
H24B H 0.6886 0.4771 0.7090 0.119 Uiso 1 1 calc R U . . .
O2 O 0.9833(5) 0.31420(13) 0.67925(13) 0.0687(9) Uani 1 1 d . . . . .
C25 C 1.0632(9) 0.2734(2) 0.7150(2) 0.0886(19) Uani 1 1 d . . . . .
H25A H 1.1909 0.2776 0.7173 0.106 Uiso 1 1 calc R U . . .
H25B H 1.0340 0.2390 0.6968 0.106 Uiso 1 1 calc R U . . .
C26 C 0.9999(11) 0.2759(4) 0.7760(4) 0.162(4) Uani 1 1 d . U . . .
H26A H 0.9318 0.2443 0.7842 0.194 Uiso 1 1 calc R U . . .
H26B H 1.0988 0.2786 0.8064 0.194 Uiso 1 1 calc R U . . .
C27 C 0.8942(12) 0.3212(3) 0.7767(3) 0.145(3) Uani 1 1 d . . . . .
H27A H 0.9530 0.3484 0.8020 0.173 Uiso 1 1 calc R U . . .
H27B H 0.7824 0.3126 0.7931 0.173 Uiso 1 1 calc R U . . .
C28 C 0.8625(8) 0.3409(2) 0.7143(2) 0.0872(18) Uani 1 1 d . . . . .
H28A H 0.7417 0.3333 0.6989 0.105 Uiso 1 1 calc R U . . .
H28B H 0.8813 0.3791 0.7129 0.105 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K1 O2 2.783(3) . ?
K1 N2 2.861(3) . ?
K1 N12 2.880(3) 3_666 ?
K1 N7 2.911(3) 1_655 ?
K1 N9 2.920(3) . ?
K1 N11 2.923(3) 1_655 ?
K1 N1 3.063(3) 1_655 ?
K1 K4 4.4119(13) . ?
K1 K4 4.4358(13) 1_655 ?
K1 K2 4.4782(12) . ?
K2 N1 2.812(3) 1_655 ?
K2 N9 2.828(3) . ?
K2 N8 2.829(3) 1_655 ?
K2 N5 2.854(3) 3_856 ?
K2 N6 2.889(3) 1_455 ?
K2 N3 2.909(3) . ?
K2 C3 3.520(3) . ?
K2 C7 3.525(3) 3_856 ?
K2 C1 3.535(3) 1_655 ?
K2 K3 4.4037(13) 1_455 ?
K2 K3 4.4115(13) . ?
K3 N8 2.815(3) 1_655 ?
K3 N5 2.832(3) 3_956 ?
K3 N4 2.832(3) . ?
K3 N3 2.862(3) 1_655 ?
K3 N4 2.918(3) 3_856 ?
K3 N6 2.926(3) 1_455 ?
K3 C12 3.483(3) 1_655 ?
K3 C8 3.523(3) 1_455 ?
K3 K3 4.3249(16) 3_856 ?
K3 K2 4.4037(13) 1_655 ?
K4 O1 2.790(3) . ?
K4 N12 2.837(3) 3_566 ?
K4 N10 2.901(3) . ?
K4 N11 2.903(3) 1_655 ?
K4 N2 2.910(3) . ?
K4 N10 2.937(3) 3_666 ?
K4 N7 2.955(3) . ?
K4 K1 4.4358(13) 1_455 ?
K4 K4 4.5818(15) 3_666 ?
B1 C2 1.591(5) . ?
B1 C3 1.604(5) . ?
B1 C1 1.606(5) . ?
B1 C4 1.623(4) . ?
C1 N1 1.143(4) . ?
C1 K2 3.535(3) 1_455 ?
N1 K2 2.812(3) 1_455 ?
N1 K1 3.063(3) 1_455 ?
C2 N2 1.135(4) . ?
C3 N3 1.142(4) . ?
N3 K3 2.862(3) 1_455 ?
C4 C5 1.528(4) . ?
B2 C7 1.600(5) . ?
B2 C6 1.601(5) . ?
B2 C8 1.607(5) . ?
B2 C9 1.612(5) . ?
C6 N4 1.140(4) . ?
N4 K3 2.918(3) 3_856 ?
C7 N5 1.144(4) . ?
C7 K2 3.524(3) 3_856 ?
N5 K3 2.832(3) 3_956 ?
N5 K2 2.854(3) 3_856 ?
C8 N6 1.144(4) . ?
C8 K3 3.523(3) 1_655 ?
N6 K2 2.889(3) 1_655 ?
N6 K3 2.926(3) 1_655 ?
C9 C10 1.528(4) . ?
B3 C12 1.597(5) . ?
B3 C11 1.600(5) . ?
B3 C14 1.609(5) . ?
B3 C13 1.610(5) . ?
C11 N7 1.140(4) . ?
N7 K1 2.911(3) 1_455 ?
C12 N8 1.140(4) . ?
C12 K3 3.482(3) 1_455 ?
N8 K3 2.815(3) 1_455 ?
N8 K2 2.829(3) 1_455 ?
C13 N9 1.138(4) . ?
C14 C15 1.527(4) . ?
B4 C16 1.603(5) . ?
B4 C17 1.604(5) . ?
B4 C18 1.606(5) . ?
B4 C19 1.613(5) . ?
C16 N10 1.143(4) . ?
N10 K4 2.937(3) 3_666 ?
C17 N11 1.145(4) . ?
N11 K4 2.903(3) 1_455 ?
N11 K1 2.923(3) 1_455 ?
C18 N12 1.137(4) . ?
N12 K4 2.837(3) 3_566 ?
N12 K1 2.880(3) 3_666 ?
C19 C20 1.521(4) . ?
O1 C24 1.396(6) . ?
O1 C21 1.416(6) . ?
C21 C22 1.481(10) . ?
C22 C23 1.375(11) . ?
C23 C24 1.481(10) . ?
O2 C25 1.400(5) . ?
O2 C28 1.411(6) . ?
C25 C26 1.468(10) . ?
C26 C27 1.389(10) . ?
C27 C28 1.469(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 K1 N2 113.69(10) . . ?
O2 K1 N12 134.83(10) . 3_666 ?
N2 K1 N12 94.39(9) . 3_666 ?
O2 K1 N7 78.12(10) . 1_655 ?
N2 K1 N7 167.89(9) . 1_655 ?
N12 K1 N7 77.87(8) 3_666 1_655 ?
O2 K1 N9 74.50(10) . . ?
N2 K1 N9 75.34(8) . . ?
N12 K1 N9 149.59(9) 3_666 . ?
N7 K1 N9 106.66(9) 1_655 . ?
O2 K1 N11 76.01(9) . 1_655 ?
N2 K1 N11 79.19(8) . 1_655 ?
N12 K1 N11 75.51(9) 3_666 1_655 ?
N7 K1 N11 107.39(9) 1_655 1_655 ?
N9 K1 N11 128.43(9) . 1_655 ?
O2 K1 N1 139.50(9) . 1_655 ?
N2 K1 N1 84.93(8) . 1_655 ?
N12 K1 N1 74.20(8) 3_666 1_655 ?
N7 K1 N1 83.99(8) 1_655 1_655 ?
N9 K1 N1 76.39(8) . 1_655 ?
N11 K1 N1 144.42(8) 1_655 1_655 ?
O2 K1 K4 87.61(7) . . ?
N2 K1 K4 40.54(6) . . ?
N12 K1 K4 92.92(6) 3_666 . ?
N7 K1 K4 147.79(6) 1_655 . ?
N9 K1 K4 96.86(6) . . ?
N11 K1 K4 40.60(6) 1_655 . ?
N1 K1 K4 123.52(6) 1_655 . ?
O2 K1 K4 103.05(8) . 1_655 ?
N2 K1 K4 132.83(6) . 1_655 ?
N12 K1 K4 38.77(6) 3_666 1_655 ?
N7 K1 K4 41.24(6) 1_655 1_655 ?
N9 K1 K4 145.42(6) . 1_655 ?
N11 K1 K4 82.24(6) 1_655 1_655 ?
N1 K1 K4 85.73(6) 1_655 1_655 ?
K4 K1 K4 117.63(2) . 1_655 ?
O2 K1 K2 108.18(7) . . ?
N2 K1 K2 77.48(6) . . ?
N12 K1 K2 112.16(6) 3_666 . ?
N7 K1 K2 96.65(6) 1_655 . ?
N9 K1 K2 38.10(6) . . ?
N11 K1 K2 155.90(6) 1_655 . ?
N1 K1 K2 38.30(5) 1_655 . ?
K4 K1 K2 115.29(3) . . ?
K4 K1 K2 118.52(3) 1_655 . ?
N1 K2 N9 82.03(8) 1_655 . ?
N1 K2 N8 77.37(9) 1_655 1_655 ?
N9 K2 N8 88.62(9) . 1_655 ?
N1 K2 N5 159.55(9) 1_655 3_856 ?
N9 K2 N5 78.85(9) . 3_856 ?
N8 K2 N5 94.89(9) 1_655 3_856 ?
N1 K2 N6 116.31(9) 1_655 1_455 ?
N9 K2 N6 154.37(9) . 1_455 ?
N8 K2 N6 78.99(9) 1_655 1_455 ?
N5 K2 N6 79.96(9) 3_856 1_455 ?
N1 K2 N3 108.37(9) 1_655 . ?
N9 K2 N3 88.70(9) . . ?
N8 K2 N3 173.25(9) 1_655 . ?
N5 K2 N3 78.52(8) 3_856 . ?
N6 K2 N3 101.03(9) 1_455 . ?
N1 K2 C3 93.21(8) 1_655 . ?
N9 K2 C3 77.95(8) . . ?
N8 K2 C3 164.63(8) 1_655 . ?
N5 K2 C3 89.86(8) 3_856 . ?
N6 K2 C3 116.29(8) 1_455 . ?
N3 K2 C3 17.34(7) . . ?
N1 K2 C7 150.46(9) 1_655 3_856 ?
N9 K2 C7 80.93(8) . 3_856 ?
N8 K2 C7 78.26(8) 1_655 3_856 ?
N5 K2 C7 16.79(8) 3_856 3_856 ?
N6 K2 C7 74.65(8) 1_455 3_856 ?
N3 K2 C7 95.20(8) . 3_856 ?
C3 K2 C7 106.54(8) . 3_856 ?
N1 K2 C1 16.15(7) 1_655 1_655 ?
N9 K2 C1 94.27(8) . 1_655 ?
N8 K2 C1 67.08(8) 1_655 1_655 ?
N5 K2 C1 161.03(8) 3_856 1_655 ?
N6 K2 C1 101.24(8) 1_455 1_655 ?
N3 K2 C1 119.32(8) . 1_655 ?
C3 K2 C1 106.11(8) . 1_655 ?
C7 K2 C1 145.14(8) 3_856 1_655 ?
N1 K2 K3 146.52(6) 1_655 1_455 ?
N9 K2 K3 86.20(7) . 1_455 ?
N8 K2 K3 133.71(6) 1_655 1_455 ?
N5 K2 K3 39.05(6) 3_856 1_455 ?
N6 K2 K3 86.37(6) 1_455 1_455 ?
N3 K2 K3 39.86(6) . 1_455 ?
C3 K2 K3 53.59(5) . 1_455 ?
C7 K2 K3 55.50(6) 3_856 1_455 ?
C1 K2 K3 159.18(6) 1_655 1_455 ?
N1 K2 K3 93.75(6) 1_655 . ?
N9 K2 K3 125.57(7) . . ?
N8 K2 K3 38.47(6) 1_655 . ?
N5 K2 K3 91.49(7) 3_856 . ?
N6 K2 K3 40.97(6) 1_455 . ?
N3 K2 K3 142.00(6) . . ?
C3 K2 K3 156.21(6) . . ?
C7 K2 K3 77.05(6) 3_856 . ?
C1 K2 K3 78.06(6) 1_655 . ?
K3 K2 K3 118.33(2) 1_455 . ?
N1 K2 K1 42.47(6) 1_655 . ?
N9 K2 K1 39.57(6) . . ?
N8 K2 K1 80.93(6) 1_655 . ?
N5 K2 K1 118.08(7) 3_856 . ?
N6 K2 K1 154.09(6) 1_455 . ?
N3 K2 K1 100.83(6) . . ?
C3 K2 K1 83.94(6) . . ?
C7 K2 K1 116.86(5) 3_856 . ?
C1 K2 K1 55.45(5) 1_655 . ?
K3 K2 K1 119.45(3) 1_455 . ?
K3 K2 K1 115.98(3) . . ?
N8 K3 N5 97.00(9) 1_655 3_956 ?
N8 K3 N4 158.73(9) 1_655 . ?
N5 K3 N4 75.20(9) 3_956 . ?
N8 K3 N3 80.50(9) 1_655 1_655 ?
N5 K3 N3 79.66(9) 3_956 1_655 ?
N4 K3 N3 116.55(9) . 1_655 ?
N8 K3 N4 77.36(8) 1_655 3_856 ?
N5 K3 N4 87.06(9) 3_956 3_856 ?
N4 K3 N4 82.45(9) . 3_856 ?
N3 K3 N4 152.52(8) 1_655 3_856 ?
N8 K3 N6 78.59(8) 1_655 1_455 ?
N5 K3 N6 175.47(9) 3_956 1_455 ?
N4 K3 N6 108.57(9) . 1_455 ?
N3 K3 N6 100.47(9) 1_655 1_455 ?
N4 K3 N6 90.93(9) 3_856 1_455 ?
N8 K3 C12 16.96(8) 1_655 1_655 ?
N5 K3 C12 80.45(8) 3_956 1_655 ?
N4 K3 C12 150.73(8) . 1_655 ?
N3 K3 C12 73.88(8) 1_655 1_655 ?
N4 K3 C12 80.29(8) 3_856 1_655 ?
N6 K3 C12 95.21(8) 1_455 1_655 ?
N8 K3 C8 89.45(8) 1_655 1_455 ?
N5 K3 C8 163.85(8) 3_956 1_455 ?
N4 K3 C8 93.54(8) . 1_455 ?
N3 K3 C8 116.11(8) 1_655 1_455 ?
N4 K3 C8 79.91(8) 3_856 1_455 ?
N6 K3 C8 17.48(7) 1_455 1_455 ?
C12 K3 C8 106.41(8) 1_655 1_455 ?
N8 K3 K3 117.55(7) 1_655 3_856 ?
N5 K3 K3 78.35(6) 3_956 3_856 ?
N4 K3 K3 41.98(6) . 3_856 ?
N3 K3 K3 153.02(7) 1_655 3_856 ?
N4 K3 K3 40.47(6) 3_856 3_856 ?
N6 K3 K3 102.68(6) 1_455 3_856 ?
C12 K3 K3 117.22(6) 1_655 3_856 ?
C8 K3 K3 85.54(6) 1_455 3_856 ?
N8 K3 K2 92.82(7) 1_655 1_655 ?
N5 K3 K2 39.42(6) 3_956 1_655 ?
N4 K3 K2 93.14(7) . 1_655 ?
N3 K3 K2 40.65(6) 1_655 1_655 ?
N4 K3 K2 124.47(7) 3_856 1_655 ?
N6 K3 K2 141.08(6) 1_455 1_655 ?
C12 K3 K2 77.66(6) 1_655 1_655 ?
C8 K3 K2 155.40(6) 1_455 1_655 ?
K3 K3 K2 114.69(3) 3_856 1_655 ?
N8 K3 K2 38.70(6) 1_655 . ?
N5 K3 K2 135.39(7) 3_956 . ?
N4 K3 K2 147.05(7) . . ?
N3 K3 K2 85.95(6) 1_655 . ?
N4 K3 K2 86.86(7) 3_856 . ?
N6 K3 K2 40.34(6) 1_455 . ?
C12 K3 K2 54.96(6) 1_655 . ?
C8 K3 K2 53.81(6) 1_455 . ?
K3 K3 K2 120.83(3) 3_856 . ?
K2 K3 K2 118.33(2) 1_655 . ?
O1 K4 N12 112.75(11) . 3_566 ?
O1 K4 N10 75.47(10) . . ?
N12 K4 N10 77.36(9) 3_566 . ?
O1 K4 N11 78.57(11) . 1_655 ?
N12 K4 N11 168.67(9) 3_566 1_655 ?
N10 K4 N11 106.22(9) . 1_655 ?
O1 K4 N2 132.72(10) . . ?
N12 K4 N2 93.01(9) 3_566 . ?
N10 K4 N2 151.17(8) . . ?
N11 K4 N2 78.73(8) 1_655 . ?
O1 K4 N10 140.41(9) . 3_666 ?
N12 K4 N10 87.54(9) 3_566 3_666 ?
N10 K4 N10 76.60(9) . 3_666 ?
N11 K4 N10 82.96(9) 1_655 3_666 ?
N2 K4 N10 75.88(8) . 3_666 ?
O1 K4 N7 73.22(9) . . ?
N12 K4 N7 77.83(8) 3_566 . ?
N10 K4 N7 127.94(9) . . ?
N11 K4 N7 106.98(8) 1_655 . ?
N2 K4 N7 74.67(8) . . ?
N10 K4 N7 146.19(8) 3_666 . ?
O1 K4 K1 101.81(10) . . ?
N12 K4 K1 132.34(6) 3_566 . ?
N10 K4 K1 145.10(6) . . ?
N11 K4 K1 40.94(6) 1_655 . ?
N2 K4 K1 39.73(6) . . ?
N10 K4 K1 85.80(6) 3_666 . ?
N7 K4 K1 82.12(6) . . ?
O1 K4 K1 85.45(8) . 1_455 ?
N12 K4 K1 39.47(6) 3_566 1_455 ?
N10 K4 K1 97.02(6) . 1_455 ?
N11 K4 K1 147.23(6) 1_655 1_455 ?
N2 K4 K1 91.99(6) . 1_455 ?
N10 K4 K1 125.51(7) 3_666 1_455 ?
N7 K4 K1 40.49(6) . 1_455 ?
K1 K4 K1 117.63(2) . 1_455 ?
O1 K4 K4 109.58(8) . 3_666 ?
N12 K4 K4 80.44(6) 3_566 3_666 ?
N10 K4 K4 38.58(6) . 3_666 ?
N11 K4 K4 95.64(6) 1_655 3_666 ?
N2 K4 K4 113.47(6) . 3_666 ?
N10 K4 K4 38.02(5) 3_666 3_666 ?
N7 K4 K4 157.21(6) . 3_666 ?
K1 K4 K4 118.19(3) . 3_666 ?
K1 K4 K4 116.73(3) 1_455 3_666 ?
C2 B1 C3 107.8(3) . . ?
C2 B1 C1 108.3(3) . . ?
C3 B1 C1 107.7(3) . . ?
C2 B1 C4 111.5(3) . . ?
C3 B1 C4 110.3(3) . . ?
C1 B1 C4 111.2(3) . . ?
N1 C1 B1 178.1(3) . . ?
N1 C1 K2 43.15(18) . 1_455 ?
B1 C1 K2 137.28(19) . 1_455 ?
C1 N1 K2 120.7(2) . 1_455 ?
C1 N1 K1 123.9(2) . 1_455 ?
K2 N1 K1 99.24(9) 1_455 1_455 ?
N2 C2 B1 178.6(3) . . ?
C2 N2 K1 138.8(2) . . ?
C2 N2 K4 118.5(2) . . ?
K1 N2 K4 99.72(9) . . ?
N3 C3 B1 178.5(4) . . ?
N3 C3 K2 49.4(2) . . ?
B1 C3 K2 130.0(2) . . ?
C3 N3 K3 126.5(2) . 1_455 ?
C3 N3 K2 113.3(2) . . ?
K3 N3 K2 99.48(9) 1_455 . ?
C5 C4 B1 112.6(3) . . ?
C7 B2 C6 108.0(3) . . ?
C7 B2 C8 107.0(3) . . ?
C6 B2 C8 107.4(3) . . ?
C7 B2 C9 110.7(3) . . ?
C6 B2 C9 111.8(3) . . ?
C8 B2 C9 111.6(3) . . ?
N4 C6 B2 178.6(4) . . ?
C6 N4 K3 121.3(2) . . ?
C6 N4 K3 124.6(3) . 3_856 ?
K3 N4 K3 97.55(9) . 3_856 ?
N5 C7 B2 178.0(4) . . ?
N5 C7 K2 46.1(2) . 3_856 ?
B2 C7 K2 135.4(2) . 3_856 ?
C7 N5 K3 139.3(3) . 3_956 ?
C7 N5 K2 117.1(2) . 3_856 ?
K3 N5 K2 101.53(9) 3_956 3_856 ?
N6 C8 B2 178.7(4) . . ?
N6 C8 K3 50.2(2) . 1_655 ?
B2 C8 K3 128.9(2) . 1_655 ?
C8 N6 K2 125.8(2) . 1_655 ?
C8 N6 K3 112.3(3) . 1_655 ?
K2 N6 K3 98.69(9) 1_655 1_655 ?
C10 C9 B2 112.7(3) . . ?
C12 B3 C11 107.1(3) . . ?
C12 B3 C14 110.1(3) . . ?
C11 B3 C14 112.5(3) . . ?
C12 B3 C13 108.0(3) . . ?
C11 B3 C13 107.8(3) . . ?
C14 B3 C13 111.1(3) . . ?
N7 C11 B3 179.1(4) . . ?
C11 N7 K1 116.8(3) . 1_455 ?
C11 N7 K4 131.0(3) . . ?
K1 N7 K4 98.26(9) 1_455 . ?
N8 C12 B3 178.0(3) . . ?
N8 C12 K3 46.1(2) . 1_455 ?
B3 C12 K3 135.1(2) . 1_455 ?
C12 N8 K3 116.9(2) . 1_455 ?
C12 N8 K2 136.1(2) . 1_455 ?
K3 N8 K2 102.82(9) 1_455 1_455 ?
N9 C13 B3 178.4(3) . . ?
C13 N9 K2 125.8(3) . . ?
C13 N9 K1 116.8(2) . . ?
K2 N9 K1 102.34(9) . . ?
C15 C14 B3 113.2(3) . . ?
C16 B4 C17 108.0(3) . . ?
C16 B4 C18 108.0(3) . . ?
C17 B4 C18 107.3(3) . . ?
C16 B4 C19 111.6(3) . . ?
C17 B4 C19 111.6(3) . . ?
C18 B4 C19 110.2(3) . . ?
N10 C16 B4 178.1(4) . . ?
C16 N10 K4 116.3(2) . . ?
C16 N10 K4 126.0(3) . 3_666 ?
K4 N10 K4 103.40(9) . 3_666 ?
N11 C17 B4 178.6(3) . . ?
C17 N11 K4 117.5(2) . 1_455 ?
C17 N11 K1 130.6(3) . 1_455 ?
K4 N11 K1 98.46(9) 1_455 1_455 ?
N12 C18 B4 178.2(3) . . ?
C18 N12 K4 135.7(3) . 3_566 ?
C18 N12 K1 117.9(2) . 3_666 ?
K4 N12 K1 101.76(9) 3_566 3_666 ?
C20 C19 B4 113.1(3) . . ?
C24 O1 C21 105.7(4) . . ?
C24 O1 K4 125.0(3) . . ?
C21 O1 K4 128.6(3) . . ?
O1 C21 C22 109.2(5) . . ?
C23 C22 C21 104.4(7) . . ?
C22 C23 C24 108.1(6) . . ?
O1 C24 C23 108.7(6) . . ?
C25 O2 C28 107.9(4) . . ?
C25 O2 K1 126.0(3) . . ?
C28 O2 K1 125.4(3) . . ?
O2 C25 C26 109.4(5) . . ?
C27 C26 C25 105.7(6) . . ?
C26 C27 C28 108.6(6) . . ?
O2 C28 C27 106.8(5) . . ?

_refine_diff_density_max         1.259
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.107

####################################################################### 
# 
# 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_KC6F5BCN3
_database_code_depnum_ccdc_archive 'CCDC 1039992'
_audit_update_record             
;
2014-12-17 deposited with the CCDC.
2015-02-17 downloaded from the CCDC.
;


#=================================================================
#DATA 1
#=================================================================  

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 B F5 K N3'
_chemical_formula_sum            'C9 B F5 K N3'
_chemical_formula_weight         295.03

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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                   11.894(2)
_cell_length_b                   12.782(3)
_cell_length_c                   7.5458(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.98(3)
_cell_angle_gamma                90.00
_cell_volume                     1113.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    2000
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      25.00

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             576
_exptl_absorpt_coefficient_mu    0.530
_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      123(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  'Stoe IPDS'
_diffrn_measurement_method       φ-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9150
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.38
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1955
_reflns_number_gt                1755
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'EXPOSE (Stoe & Cie, 1996)'
_computing_cell_refinement       'CELL (Stoe & Cie, 1996)'
_computing_data_reduction        'INTEGRATE (Stoe & Cie, 1996)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond3.1 (Crystal Impact GbR, 2006)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0536P)²+0.4900P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    .
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1955
_refine_ls_number_parameters     172
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0326
_refine_ls_wR_factor_ref         0.0826
_refine_ls_wR_factor_gt          0.0815
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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 0.57411(3) 0.83946(3) 0.02369(5) 0.02253(14) Uani 1 1 d . . .
B1 B 1.29907(16) 0.94697(15) 0.4232(3) 0.0200(4) Uani 1 1 d . . .
C1 C 1.16442(14) 0.91134(12) 0.3524(2) 0.0188(3) Uani 1 1 d . . .
C2 C 1.11633(15) 0.90225(13) 0.1667(2) 0.0221(4) Uani 1 1 d . . .
F2 F 1.18364(9) 0.92055(9) 0.04912(13) 0.0310(3) Uani 1 1 d . . .
C3 C 1.00143(15) 0.87757(13) 0.0920(2) 0.0239(4) Uani 1 1 d . . .
F3 F 0.95997(10) 0.87024(9) -0.08977(14) 0.0341(3) Uani 1 1 d . . .
C4 C 0.92906(15) 0.86243(14) 0.2068(3) 0.0264(4) Uani 1 1 d . . .
F4 F 0.81629(9) 0.84138(9) 0.13800(18) 0.0379(3) Uani 1 1 d . . .
C5 C 0.97232(15) 0.86957(14) 0.3919(3) 0.0247(4) Uani 1 1 d . . .
F5 F 0.90118(10) 0.85470(9) 0.50418(16) 0.0360(3) Uani 1 1 d . . .
C6 C 1.08844(15) 0.89252(13) 0.4622(2) 0.0222(4) Uani 1 1 d . . .
F6 F 1.12490(9) 0.89800(9) 0.64520(14) 0.0325(3) Uani 1 1 d . . .
C7 C 1.34746(15) 0.95296(13) 0.6399(2) 0.0224(4) Uani 1 1 d . . .
N7 N 1.38899(14) 0.96168(12) 0.7930(2) 0.0295(4) Uani 1 1 d . . .
C8 C 1.31836(14) 1.06162(13) 0.3481(2) 0.0210(4) Uani 1 1 d . . .
N8 N 1.33530(14) 1.14309(12) 0.2983(2) 0.0270(3) Uani 1 1 d . . .
C9 C 1.38233(14) 0.86916(14) 0.3471(2) 0.0219(4) Uani 1 1 d . . .
N9 N 1.44238(14) 0.81536(13) 0.2915(2) 0.0298(4) 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 F4 2.8004(14) . ?
K1 N9 2.8487(17) 4_475 ?
K1 N9 2.8570(17) 1_455 ?
K1 N7 2.8761(17) 3_776 ?
K1 N8 2.8951(17) 3_775 ?
K1 N7 2.9096(17) 1_454 ?
K1 N8 2.9267(17) 2_745 ?
K1 K1 4.4119(8) 4_575 ?
K1 K1 4.4119(8) 4_576 ?
K1 K1 4.4467(11) 3_675 ?
B1 C7 1.599(2) . ?
B1 C9 1.605(2) . ?
B1 C8 1.607(2) . ?
B1 C1 1.626(2) . ?
C1 C2 1.384(2) . ?
C1 C6 1.387(2) . ?
C2 F2 1.3513(19) . ?
C2 C3 1.383(3) . ?
C3 F3 1.344(2) . ?
C3 C4 1.375(3) . ?
C4 F4 1.343(2) . ?
C4 C5 1.369(3) . ?
C5 F5 1.348(2) . ?
C5 C6 1.386(3) . ?
C6 F6 1.345(2) . ?
C7 N7 1.147(2) . ?
N7 K1 2.8761(17) 3_776 ?
N7 K1 2.9096(17) 1_656 ?
C8 N8 1.141(2) . ?
N8 K1 2.8951(17) 3_775 ?
N8 K1 2.9267(17) 2_755 ?
C9 N9 1.142(2) . ?
N9 K1 2.8487(17) 4_676 ?
N9 K1 2.8570(17) 1_655 ?

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
F4 K1 N9 124.58(5) . 4_475 ?
F4 K1 N9 118.83(5) . 1_455 ?
N9 K1 N9 92.64(5) 4_475 1_455 ?
F4 K1 N7 79.51(4) . 3_776 ?
N9 K1 N7 155.10(5) 4_475 3_776 ?
N9 K1 N7 78.54(5) 1_455 3_776 ?
F4 K1 N8 72.19(5) . 3_775 ?
N9 K1 N8 78.35(5) 4_475 3_775 ?
N9 K1 N8 168.78(5) 1_455 3_775 ?
N7 K1 N8 106.92(5) 3_776 3_775 ?
F4 K1 N7 138.85(4) . 1_454 ?
N9 K1 N7 77.33(5) 4_475 1_454 ?
N9 K1 N7 90.91(5) 1_455 1_454 ?
N7 K1 N7 79.55(5) 3_776 1_454 ?
N8 K1 N7 80.67(5) 3_775 1_454 ?
F4 K1 N8 68.21(4) . 2_745 ?
N9 K1 N8 76.90(5) 4_475 2_745 ?
N9 K1 N8 77.70(4) 1_455 2_745 ?
N7 K1 N8 122.74(5) 3_776 2_745 ?
N8 K1 N8 106.30(4) 3_775 2_745 ?
N7 K1 N8 151.22(5) 1_454 2_745 ?
F4 K1 K1 93.18(4) . 4_575 ?
N9 K1 K1 39.42(3) 4_475 4_575 ?
N9 K1 K1 131.47(4) 1_455 4_575 ?
N7 K1 K1 146.90(3) 3_776 4_575 ?
N8 K1 K1 40.99(3) 3_775 4_575 ?
N7 K1 K1 85.59(4) 1_454 4_575 ?
N8 K1 K1 82.63(4) 2_745 4_575 ?
F4 K1 K1 87.34(4) . 4_576 ?
N9 K1 K1 93.00(4) 4_475 4_576 ?
N9 K1 K1 39.28(3) 1_455 4_576 ?
N7 K1 K1 94.50(4) 3_776 4_576 ?
N8 K1 K1 146.58(3) 3_775 4_576 ?
N7 K1 K1 129.31(4) 1_454 4_576 ?
N8 K1 K1 40.46(3) 2_745 4_576 ?
K1 K1 K1 117.55(2) 4_575 4_576 ?
F4 K1 K1 112.03(3) . 3_675 ?
N9 K1 K1 116.31(4) 4_475 3_675 ?
N9 K1 K1 83.22(3) 1_455 3_675 ?
N7 K1 K1 40.05(3) 3_776 3_675 ?
N8 K1 K1 94.71(3) 3_775 3_675 ?
N7 K1 K1 39.50(3) 1_454 3_675 ?
N8 K1 K1 157.41(3) 2_745 3_675 ?
K1 K1 K1 119.443(18) 4_575 3_675 ?
K1 K1 K1 117.727(17) 4_576 3_675 ?
C7 B1 C9 107.16(14) . . ?
C7 B1 C8 105.66(14) . . ?
C9 B1 C8 106.61(13) . . ?
C7 B1 C1 115.61(14) . . ?
C9 B1 C1 110.66(14) . . ?
C8 B1 C1 110.65(13) . . ?
C2 C1 C6 114.89(15) . . ?
C2 C1 B1 119.30(15) . . ?
C6 C1 B1 125.75(15) . . ?
F2 C2 C3 117.12(15) . . ?
F2 C2 C1 118.98(15) . . ?
C3 C2 C1 123.88(16) . . ?
F3 C3 C4 120.15(16) . . ?
F3 C3 C2 120.96(16) . . ?
C4 C3 C2 118.88(16) . . ?
F4 C4 C5 120.11(17) . . ?
F4 C4 C3 120.22(17) . . ?
C5 C4 C3 119.67(16) . . ?
C4 F4 K1 167.84(11) . . ?
F5 C5 C4 119.56(16) . . ?
F5 C5 C6 120.52(17) . . ?
C4 C5 C6 119.92(17) . . ?
F6 C6 C5 116.64(16) . . ?
F6 C6 C1 120.62(15) . . ?
C5 C6 C1 122.73(16) . . ?
N7 C7 B1 174.81(18) . . ?
C7 N7 K1 123.29(13) . 3_776 ?
C7 N7 K1 129.04(13) . 1_656 ?
K1 N7 K1 100.45(5) 3_776 1_656 ?
N8 C8 B1 177.94(18) . . ?
C8 N8 K1 118.53(13) . 3_775 ?
C8 N8 K1 134.92(13) . 2_755 ?
K1 N8 K1 98.55(5) 3_775 2_755 ?
N9 C9 B1 178.71(18) . . ?
C9 N9 K1 119.48(13) . 4_676 ?
C9 N9 K1 133.91(14) . 1_655 ?
K1 N9 K1 101.29(5) 4_676 1_655 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.132







####################################################################### 
# 
# 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_KC3H5BCN3
_database_code_depnum_ccdc_archive 'CCDC 1039993'
_audit_update_record             
;
2014-12-17 deposited with the CCDC.
2015-02-17 downloaded from the CCDC.
;


#=================================================================
#DATA 1
#=================================================================  

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H5 B K N3'
_chemical_formula_sum            'C6 H5 B K N3'
_chemical_formula_weight         169.04

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'
N N 0.0061 0.0033 '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'

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

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

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

_cell_length_a                   9.5044(12)
_cell_length_b                   9.9760(13)
_cell_length_c                   10.1345(13)
_cell_angle_alpha                81.033(3)
_cell_angle_beta                 68.217(3)
_cell_angle_gamma                83.514(3)
_cell_volume                     879.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    17435
_cell_measurement_theta_min      2.527
_cell_measurement_theta_max      26.7275

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_F_000             344
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_absorpt_coefficient_mu    0.540
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.6565
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'Sadabs 2012/1 (Bruker 2008)'

_exptl_special_details           
;
 The crystal was immersed in a film of perfluoropolyether oil, mounted
on a polyimide microloop (MicroMounts of MiTeGen) and transferred to
stream of cold nitrogen (Oxford Cryostream 700).
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16314
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.312
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3455
_reflns_number_gt                3213
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX2 ver. 2010.3 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. 7.68A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.68A (Bruker AXS)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'XP ver. 5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0324P)²+0.5055P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3455
_refine_ls_number_parameters     199
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0273
_refine_ls_wR_factor_ref         0.0713
_refine_ls_wR_factor_gt          0.0703
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.35623(3) 0.09257(3) 0.12428(3) 0.01773(9) Uani 1 1 d . . . . .
K2 K 0.04511(3) 0.64293(3) 0.81063(3) 0.01919(9) Uani 1 1 d . . . . .
B1 B 0.13821(18) 0.14017(15) 0.75140(16) 0.0157(3) Uani 1 1 d . . . . .
C1 C 0.28538(16) 0.09466(13) 0.79287(14) 0.0172(3) Uani 1 1 d . . . . .
N1 N 0.39068(14) 0.06129(13) 0.82159(14) 0.0239(3) Uani 1 1 d . . . . .
C2 C 0.05477(16) 0.26713(14) 0.83530(15) 0.0182(3) Uani 1 1 d . . . . .
N2 N 0.00235(16) 0.36077(12) 0.89262(14) 0.0249(3) Uani 1 1 d . . . . .
C3 C 0.02995(15) 0.01515(13) 0.80600(14) 0.0159(3) Uani 1 1 d . . . . .
N3 N -0.04419(14) -0.07569(12) 0.83636(13) 0.0218(3) Uani 1 1 d . . . . .
C4 C 0.18257(17) 0.17885(14) 0.57854(15) 0.0211(3) Uani 1 1 d . . . . .
H4A H 0.0885 0.1948 0.5564 0.025 Uiso 1 1 calc R U . . .
H4B H 0.2366 0.2640 0.5468 0.025 Uiso 1 1 calc R U . . .
C5 C 0.28110(18) 0.06806(16) 0.49807(15) 0.0249(3) Uani 1 1 d . . . . .
H5 H 0.3870 0.0684 0.4776 0.030 Uiso 1 1 calc R U . . .
C6 C 0.2355(2) -0.02982(18) 0.45280(17) 0.0340(4) Uani 1 1 d . . . . .
H6A H 0.1306 -0.0346 0.4705 0.041 Uiso 1 1 calc R U . . .
H6B H 0.3074 -0.0956 0.4024 0.041 Uiso 1 1 calc R U . . .
B2 B 0.3639(2) 0.56215(16) 0.25595(18) 0.0208(3) Uani 1 1 d . . . . .
C7 C 0.30145(16) 0.44881(14) 0.19933(16) 0.0200(3) Uani 1 1 d . . . . .
N4 N 0.26157(15) 0.36394(13) 0.16034(15) 0.0260(3) Uani 1 1 d . . . . .
C8 C 0.2529(2) 0.57669(16) 0.41608(17) 0.0278(3) Uani 1 1 d . . . . .
N5 N 0.1767(2) 0.58815(17) 0.53128(16) 0.0433(4) Uani 1 1 d . . . . .
C9 C 0.35831(17) 0.70502(14) 0.16171(15) 0.0204(3) Uani 1 1 d . . . . .
N6 N 0.36264(16) 0.80950(13) 0.09530(14) 0.0264(3) Uani 1 1 d . . . . .
C10 C 0.54071(18) 0.52018(16) 0.24046(18) 0.0287(3) Uani 1 1 d . . . . .
H10A H 0.6040 0.5218 0.1376 0.034 Uiso 1 1 calc R U . . .
H10B H 0.5769 0.5891 0.2790 0.034 Uiso 1 1 calc R U . . .
C11 C 0.56203(19) 0.38404(17) 0.31601(18) 0.0296(3) Uani 1 1 d . . . . .
H11 H 0.5304 0.3753 0.4174 0.036 Uiso 1 1 calc R U . . .
C12 C 0.6220(2) 0.27358(18) 0.2524(2) 0.0354(4) Uani 1 1 d . . . . .
H12A H 0.6550 0.2784 0.1512 0.043 Uiso 1 1 calc R U . . .
H12B H 0.6320 0.1897 0.3081 0.043 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K1 N4 2.7903(13) . ?
K1 N3 2.8629(13) 2_556 ?
K1 N6 2.8760(13) 1_545 ?
K1 N1 2.8856(13) 2_656 ?
K1 N6 2.9232(14) 2_665 ?
K1 N1 3.0240(13) 1_554 ?
K1 C6 3.1790(17) . ?
K1 K1 3.5251(6) 2_655 ?
K1 K2 4.2835(6) 2_566 ?
K2 N5 2.7528(16) . ?
K2 N4 2.8266(14) 2_566 ?
K2 N2 2.8386(13) . ?
K2 N3 2.8624(13) 1_565 ?
K2 N2 2.8655(13) 2_567 ?
K2 C12 3.1686(18) 2_666 ?
K2 C11 3.4620(17) 2_666 ?
K2 K2 4.2777(7) 2_567 ?
K2 K1 4.2835(6) 2_566 ?
B1 C2 1.601(2) . ?
B1 C3 1.6040(19) . ?
B1 C1 1.604(2) . ?
B1 C4 1.635(2) . ?
C1 N1 1.1436(19) . ?
N1 K1 2.8856(13) 2_656 ?
N1 K1 3.0240(13) 1_556 ?
C2 N2 1.1434(19) . ?
N2 K2 2.8656(13) 2_567 ?
C3 N3 1.1441(18) . ?
N3 K2 2.8623(13) 1_545 ?
N3 K1 2.8629(13) 2_556 ?
C4 C5 1.498(2) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.317(2) . ?
C5 H5 0.9500 . ?
C6 H6A 0.9500 . ?
C6 H6B 0.9500 . ?
B2 C8 1.592(2) . ?
B2 C9 1.595(2) . ?
B2 C7 1.602(2) . ?
B2 C10 1.640(2) . ?
C7 N4 1.1423(19) . ?
N4 K2 2.8265(14) 2_566 ?
C8 N5 1.138(2) . ?
C9 N6 1.145(2) . ?
N6 K1 2.8760(13) 1_565 ?
N6 K1 2.9232(14) 2_665 ?
C10 C11 1.483(2) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.327(2) . ?
C11 K2 3.4620(17) 2_666 ?
C11 H11 0.9500 . ?
C12 K2 3.1686(18) 2_666 ?
C12 H12A 0.9500 . ?
C12 H12B 0.9500 . ?

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
N4 K1 N3 82.15(4) . 2_556 ?
N4 K1 N6 163.14(4) . 1_545 ?
N3 K1 N6 81.01(4) 2_556 1_545 ?
N4 K1 N1 127.85(4) . 2_656 ?
N3 K1 N1 142.40(4) 2_556 2_656 ?
N6 K1 N1 67.91(4) 1_545 2_656 ?
N4 K1 N6 87.42(4) . 2_665 ?
N3 K1 N6 139.79(4) 2_556 2_665 ?
N6 K1 N6 105.13(3) 1_545 2_665 ?
N1 K1 N6 71.46(4) 2_656 2_665 ?
N4 K1 N1 106.33(4) . 1_554 ?
N3 K1 N1 80.41(4) 2_556 1_554 ?
N6 K1 N1 70.14(4) 1_545 1_554 ?
N1 K1 N1 106.80(3) 2_656 1_554 ?
N6 K1 N1 65.49(4) 2_665 1_554 ?
N4 K1 C6 97.87(4) . . ?
N3 K1 C6 81.33(4) 2_556 . ?
N6 K1 C6 80.25(4) 1_545 . ?
N1 K1 C6 73.25(4) 2_656 . ?
N6 K1 C6 138.73(4) 2_665 . ?
N1 K1 C6 147.19(4) 1_554 . ?
N4 K1 K1 138.03(3) . 2_655 ?
N3 K1 K1 120.38(3) 2_556 2_655 ?
N6 K1 K1 53.18(3) 1_545 2_655 ?
N1 K1 K1 55.21(3) 2_656 2_655 ?
N6 K1 K1 51.96(3) 2_665 2_655 ?
N1 K1 K1 51.59(3) 1_554 2_655 ?
C6 K1 K1 119.01(4) . 2_655 ?
N4 K1 K2 40.62(3) . 2_566 ?
N3 K1 K2 41.56(2) 2_556 2_566 ?
N6 K1 K2 122.52(3) 1_545 2_566 ?
N1 K1 K2 159.87(3) 2_656 2_566 ?
N6 K1 K2 117.17(3) 2_665 2_566 ?
N1 K1 K2 93.25(3) 1_554 2_566 ?
C6 K1 K2 90.90(4) . 2_566 ?
K1 K1 K2 144.813(14) 2_655 2_566 ?
N5 K2 N4 97.88(5) . 2_566 ?
N5 K2 N2 87.88(4) . . ?
N4 K2 N2 79.44(4) 2_566 . ?
N5 K2 N3 113.43(4) . 1_565 ?
N4 K2 N3 81.53(4) 2_566 1_565 ?
N2 K2 N3 153.17(4) . 1_565 ?
N5 K2 N2 159.85(5) . 2_567 ?
N4 K2 N2 97.94(4) 2_566 2_567 ?
N2 K2 N2 82.84(4) . 2_567 ?
N3 K2 N2 81.26(4) 1_565 2_567 ?
N5 K2 C12 81.43(5) . 2_666 ?
N4 K2 C12 165.83(4) 2_566 2_666 ?
N2 K2 C12 114.61(4) . 2_666 ?
N3 K2 C12 85.76(4) 1_565 2_666 ?
N2 K2 C12 86.23(5) 2_567 2_666 ?
N5 K2 C11 65.90(5) . 2_666 ?
N4 K2 C11 163.56(4) 2_566 2_666 ?
N2 K2 C11 96.59(4) . 2_666 ?
N3 K2 C11 106.75(4) 1_565 2_666 ?
N2 K2 C11 97.37(4) 2_567 2_666 ?
C12 K2 C11 22.54(4) 2_666 2_666 ?
N5 K2 K2 127.18(4) . 2_567 ?
N4 K2 K2 88.33(3) 2_566 2_567 ?
N2 K2 K2 41.66(3) . 2_567 ?
N3 K2 K2 119.36(3) 1_565 2_567 ?
N2 K2 K2 41.18(3) 2_567 2_567 ?
C12 K2 K2 103.43(4) 2_666 2_567 ?
C11 K2 K2 99.33(3) 2_666 2_567 ?
N5 K2 K1 111.80(4) . 2_566 ?
N4 K2 K1 39.99(3) 2_566 2_566 ?
N2 K2 K1 116.69(3) . 2_566 ?
N3 K2 K1 41.57(3) 1_565 2_566 ?
N2 K2 K1 88.35(3) 2_567 2_566 ?
C12 K2 K1 127.20(3) 2_666 2_566 ?
C11 K2 K1 146.70(3) 2_666 2_566 ?
K2 K2 K1 106.182(12) 2_567 2_566 ?
C2 B1 C3 109.85(11) . . ?
C2 B1 C1 106.88(11) . . ?
C3 B1 C1 107.62(11) . . ?
C2 B1 C4 111.41(11) . . ?
C3 B1 C4 109.13(11) . . ?
C1 B1 C4 111.87(12) . . ?
N1 C1 B1 179.35(14) . . ?
C1 N1 K1 164.48(11) . 2_656 ?
C1 N1 K1 115.11(10) . 1_556 ?
K1 N1 K1 73.20(3) 2_656 1_556 ?
N2 C2 B1 176.42(15) . . ?
C2 N2 K2 132.77(11) . . ?
C2 N2 K2 120.70(10) . 2_567 ?
K2 N2 K2 97.16(4) . 2_567 ?
N3 C3 B1 175.76(14) . . ?
C3 N3 K2 129.19(10) . 1_545 ?
C3 N3 K1 131.60(10) . 2_556 ?
K2 N3 K1 96.86(4) 1_545 2_556 ?
C5 C4 B1 111.60(11) . . ?
C5 C4 H4A 109.3 . . ?
B1 C4 H4A 109.3 . . ?
C5 C4 H4B 109.3 . . ?
B1 C4 H4B 109.3 . . ?
H4A C4 H4B 108.0 . . ?
C6 C5 C4 126.47(15) . . ?
C6 C5 H5 116.8 . . ?
C4 C5 H5 116.8 . . ?
C5 C6 K1 95.63(11) . . ?
C5 C6 H6A 120.0 . . ?
K1 C6 H6A 101.0 . . ?
C5 C6 H6B 120.0 . . ?
K1 C6 H6B 73.2 . . ?
H6A C6 H6B 120.0 . . ?
C8 B2 C9 107.83(12) . . ?
C8 B2 C7 107.72(12) . . ?
C9 B2 C7 109.64(12) . . ?
C8 B2 C10 113.62(13) . . ?
C9 B2 C10 108.44(12) . . ?
C7 B2 C10 109.53(12) . . ?
N4 C7 B2 176.97(15) . . ?
C7 N4 K1 135.15(11) . . ?
C7 N4 K2 121.35(11) . 2_566 ?
K1 N4 K2 99.39(4) . 2_566 ?
N5 C8 B2 178.17(18) . . ?
C8 N5 K2 167.54(14) . . ?
N6 C9 B2 175.55(15) . . ?
C9 N6 K1 139.93(11) . 1_565 ?
C9 N6 K1 122.11(12) . 2_665 ?
K1 N6 K1 74.87(3) 1_565 2_665 ?
C11 C10 B2 113.51(13) . . ?
C11 C10 H10A 108.9 . . ?
B2 C10 H10A 108.9 . . ?
C11 C10 H10B 108.9 . . ?
B2 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
C12 C11 C10 124.82(16) . . ?
C12 C11 K2 66.21(10) . 2_666 ?
C10 C11 K2 98.56(10) . 2_666 ?
C12 C11 H11 117.6 . . ?
C10 C11 H11 117.6 . . ?
K2 C11 H11 105.9 2_666 . ?
C11 C12 K2 91.25(11) . 2_666 ?
C11 C12 H12A 120.0 . . ?
K2 C12 H12A 84.0 2_666 . ?
C11 C12 H12B 120.0 . . ?
K2 C12 H12B 94.8 2_666 . ?
H12A C12 H12B 120.0 . . ?

_refine_diff_density_max         0.685
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.044


####################################################################### 
# 
# 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_KBHCN3
_database_code_depnum_ccdc_archive 'CCDC 1039994'
_audit_update_record             
;
2014-12-17 deposited with the CCDC.
2015-02-17 downloaded from the CCDC.
;


#=================================================================
#DATA 1
#=================================================================  

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H8 B2 K2 N6 O'
_chemical_formula_sum            'C9 H8 B2 K2 N6 O'
_chemical_formula_weight         316.03

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   9.8586(5)
_cell_length_b                   13.1307(6)
_cell_length_c                   12.1811(6)
_cell_angle_alpha                90
_cell_angle_beta                 93.991(2)
_cell_angle_gamma                90
_cell_volume                     1573.02(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9950
_cell_measurement_theta_min      2.284
_cell_measurement_theta_max      26.871

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_F_000             640
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    0.603
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.6612
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'Sadabs 2012/1 (Bruker 2012)'

_exptl_special_details           
;
 The crystal was immersed in a film of perfluoropolyether oil, mounted
on a polyimide microloop (MicroMounts of MiTeGen) and transferred to
stream of cold nitrogen (Oxford Cryostream 700). 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'rotation anode'
_diffrn_radiation_monochromator  helios
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21007
_diffrn_reflns_av_unetI/netI     0.0110
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.284
_diffrn_reflns_theta_max         26.498
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3268
_reflns_number_gt                2992
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'APEX2 ver. 2010.3 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. 7.68A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.68A (Bruker AXS)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'XP ver. 5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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     
'w=1/[σ²(Fo²)+(0.0262P)²+0.4838P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3268
_refine_ls_number_parameters     250
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0201
_refine_ls_wR_factor_ref         0.0549
_refine_ls_wR_factor_gt          0.0536
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.75376(2) 0.23324(2) 0.50961(2) 0.01875(7) Uani 1 1 d . . . . .
K2 K 0.52917(2) 0.25493(2) 0.26399(2) 0.01769(7) Uani 1 1 d . . . . .
B1 B 1.24760(12) 0.42900(10) 0.49392(10) 0.0217(3) Uani 1 1 d . . . . .
H4 H 1.2304(14) 0.4596(10) 0.4094(11) 0.035(4) Uiso 1 1 d . . . . .
C1 C 1.11270(11) 0.37191(8) 0.52409(9) 0.0228(2) Uani 1 1 d . . . . .
N1 N 1.01382(10) 0.33319(8) 0.54421(8) 0.0309(2) Uani 1 1 d . . . . .
C2 C 1.37381(11) 0.35333(8) 0.49585(9) 0.0231(2) Uani 1 1 d . . . . .
N2 N 1.46674(11) 0.30152(8) 0.49345(9) 0.0307(2) Uani 1 1 d . . . . .
C3 C 1.27841(10) 0.52005(8) 0.57781(9) 0.0209(2) Uani 1 1 d . . . . .
N3 N 1.30062(10) 0.58818(7) 0.63455(9) 0.0272(2) Uani 1 1 d . . . . .
B2A B 0.05229(17) 0.12169(13) 0.34694(14) 0.0172(4) Uani 0.672(4) 1 d . . P A 1
H2A H 0.0653(18) 0.1512(14) 0.4304(15) 0.025(5) Uiso 0.672(4) 1 d . . P A 1
C4A C -0.0942(3) 0.1552(3) 0.2973(2) 0.0177(6) Uani 0.672(4) 1 d D U P A 1
N4A N -0.2001(3) 0.1835(5) 0.2651(7) 0.0213(10) Uani 0.672(4) 1 d D U P A 1
C5A C 0.1668(3) 0.1684(3) 0.2766(3) 0.0176(7) Uani 0.672(4) 1 d D U P A 1
N5A N 0.2494(4) 0.2032(4) 0.2269(6) 0.0297(12) Uani 0.672(4) 1 d D U P A 1
C6A C 0.0678(5) 0.0012(4) 0.3548(3) 0.0166(6) Uani 0.672(4) 1 d . U P A 1
N6A N 0.08749(10) -0.08303(7) 0.37041(8) 0.0271(2) Uani 0.672(4) 1 d . . P A 1
B2B B 0.0428(3) 0.0803(3) 0.2421(3) 0.0160(9) Uani 0.328(4) 1 d . . P A 2
H2B H 0.030(4) 0.050(3) 0.157(3) 0.020(9) Uiso 0.328(4) 1 d . . P A 2
C4B C -0.0951(6) 0.1386(5) 0.2651(5) 0.0151(9) Uani 0.328(4) 1 d D U P A 2
N4B N -0.1935(6) 0.1803(9) 0.2843(15) 0.0188(15) Uani 0.328(4) 1 d D U P A 2
C5B C 0.1660(7) 0.1564(6) 0.2472(6) 0.0152(11) Uani 0.328(4) 1 d D U P A 2
N5B N 0.2582(7) 0.2095(8) 0.2500(13) 0.025(2) Uani 0.328(4) 1 d D U P A 2
C6B C 0.0716(11) -0.0111(8) 0.3237(6) 0.0156(10) Uani 0.328(4) 1 d . U P A 2
N6B N 0.08749(10) -0.08303(7) 0.37041(8) 0.0271(2) Uani 0.328(4) 1 d . . P A 2
O1 O 0.58224(8) 0.08498(6) 0.40370(7) 0.02607(18) Uani 1 1 d . . . . .
C7 C 0.58611(11) -0.00362(8) 0.37491(9) 0.0209(2) Uani 1 1 d . . . . .
C8 C 0.69613(13) -0.07342(9) 0.41737(11) 0.0312(3) Uani 1 1 d . . . . .
H8A H 0.7694 -0.0344 0.4523 0.047 Uiso 1 1 calc R U . . .
H8B H 0.7289 -0.1116 0.3574 0.047 Uiso 1 1 calc R U . . .
H8C H 0.6613 -0.1194 0.4699 0.047 Uiso 1 1 calc R U . . .
C9 C 0.48026(13) -0.04670(11) 0.29450(12) 0.0410(3) Uani 1 1 d . . . . .
H9A H 0.4070 0.0011 0.2829 0.061 Uiso 1 1 calc R U . . .
H9B H 0.4462 -0.1091 0.3229 0.061 Uiso 1 1 calc R U . . .
H9C H 0.5195 -0.0598 0.2259 0.061 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K1 N5A 2.778(7) 4_666 ?
K1 O1 2.8302(8) . ?
K1 N6B 2.8561(10) 3_656 ?
K1 N6A 2.8561(10) 3_656 ?
K1 N1 2.8849(10) . ?
K1 N4B 2.913(17) 1_655 ?
K1 N3 2.9562(10) 3_766 ?
K1 N2 2.9617(11) 1_455 ?
K1 N5B 3.021(15) 4_666 ?
K1 N4A 3.113(8) 1_655 ?
K1 C4A 3.245(3) 1_655 ?
K1 C5B 3.402(8) 4_666 ?
K2 N5B 2.731(6) . ?
K2 N4A 2.828(3) 1_655 ?
K2 O1 2.8330(8) . ?
K2 N5A 2.846(4) . ?
K2 N6B 2.8753(10) 2 ?
K2 N6A 2.8753(10) 2 ?
K2 N3 2.8807(10) 3_766 ?
K2 N4B 2.899(5) 1_655 ?
K2 N1 2.9108(10) 4_565 ?
K2 N2 2.9673(10) 1_455 ?
K2 C6B 3.379(9) 2 ?
K2 C1 3.5109(11) 4_565 ?
B1 C3 1.5883(16) . ?
B1 C2 1.5912(17) . ?
B1 C1 1.5918(15) . ?
B1 H4 1.107(14) . ?
C1 N1 1.1411(15) . ?
C1 K2 3.5109(11) 4_666 ?
N1 K2 2.9108(10) 4_666 ?
C2 N2 1.1432(15) . ?
N2 K1 2.9617(11) 1_655 ?
N2 K2 2.9673(10) 1_655 ?
C3 N3 1.1423(15) . ?
C3 K1 3.4178(11) 3_766 ?
N3 K2 2.8807(10) 3_766 ?
N3 K1 2.9561(10) 3_766 ?
B2A C5A 1.587(4) . ?
B2A C4A 1.588(3) . ?
B2A C6A 1.592(5) . ?
B2A H2A 1.087(18) . ?
C4A N4A 1.152(4) . ?
C4A K1 3.245(3) 1_455 ?
N4A K2 2.828(3) 1_455 ?
N4A K1 3.113(8) 1_455 ?
C5A N5A 1.144(4) . ?
N5A K1 2.778(7) 4_565 ?
C6A N6A 1.136(5) . ?
N6A K1 2.8561(10) 3_656 ?
N6A K2 2.8752(10) 2_545 ?
B2B C6B 1.571(11) . ?
B2B C5B 1.571(7) . ?
B2B C4B 1.601(6) . ?
B2B H2B 1.11(4) . ?
C4B N4B 1.152(4) . ?
N4B K2 2.899(5) 1_455 ?
N4B K1 2.913(17) 1_455 ?
C5B N5B 1.144(4) . ?
C5B K1 3.402(8) 4_565 ?
N5B K1 3.021(15) 4_565 ?
C6B K2 3.379(9) 2_545 ?
O1 C7 1.2165(13) . ?
C7 C8 1.4852(16) . ?
C7 C9 1.4920(16) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?

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
N5A K1 O1 126.34(11) 4_666 . ?
O1 K1 N6B 92.69(3) . 3_656 ?
N5A K1 N6A 76.35(10) 4_666 3_656 ?
O1 K1 N6A 92.69(3) . 3_656 ?
N5A K1 N1 78.27(10) 4_666 . ?
O1 K1 N1 151.19(3) . . ?
N6B K1 N1 77.86(3) 3_656 . ?
N6A K1 N1 77.86(3) 3_656 . ?
O1 K1 N4B 63.0(2) . 1_655 ?
N6B K1 N4B 100.9(2) 3_656 1_655 ?
N1 K1 N4B 91.78(19) . 1_655 ?
N5A K1 N3 108.28(12) 4_666 3_766 ?
O1 K1 N3 101.36(3) . 3_766 ?
N6B K1 N3 157.23(3) 3_656 3_766 ?
N6A K1 N3 157.23(3) 3_656 3_766 ?
N1 K1 N3 81.29(3) . 3_766 ?
N4B K1 N3 70.5(2) 1_655 3_766 ?
N5A K1 N2 83.95(8) 4_666 1_455 ?
O1 K1 N2 68.91(3) . 1_455 ?
N6B K1 N2 136.89(3) 3_656 1_455 ?
N6A K1 N2 136.89(3) 3_656 1_455 ?
N1 K1 N2 135.01(3) . 1_455 ?
N4B K1 N2 104.01(14) 1_655 1_455 ?
N3 K1 N2 65.64(3) 3_766 1_455 ?
O1 K1 N5B 125.5(2) . 4_666 ?
N6B K1 N5B 72.86(16) 3_656 4_666 ?
N1 K1 N5B 78.02(17) . 4_666 ?
N4B K1 N5B 168.9(2) 1_655 4_666 ?
N3 K1 N5B 111.6(2) 3_766 4_666 ?
N2 K1 N5B 86.47(13) 1_455 4_666 ?
N5A K1 N4A 170.88(15) 4_666 1_655 ?
O1 K1 N4A 62.73(11) . 1_655 ?
N6A K1 N4A 103.49(9) 3_656 1_655 ?
N1 K1 N4A 92.74(9) . 1_655 ?
N3 K1 N4A 68.33(11) 3_766 1_655 ?
N2 K1 N4A 101.67(6) 1_455 1_655 ?
N5A K1 C4A 153.23(9) 4_666 1_655 ?
O1 K1 C4A 73.38(6) . 1_655 ?
N6A K1 C4A 85.57(6) 3_656 1_655 ?
N1 K1 C4A 78.75(6) . 1_655 ?
N3 K1 C4A 81.47(6) 3_766 1_655 ?
N2 K1 C4A 122.34(5) 1_455 1_655 ?
N4A K1 C4A 20.74(6) 1_655 1_655 ?
O1 K1 C5B 120.11(13) . 4_666 ?
N6B K1 C5B 91.24(11) 3_656 4_666 ?
N1 K1 C5B 87.59(13) . 4_666 ?
N4B K1 C5B 167.4(3) 1_655 4_666 ?
N3 K1 C5B 96.96(11) 3_766 4_666 ?
N2 K1 C5B 68.24(11) 1_455 4_666 ?
N5B K1 C5B 19.37(13) 4_666 4_666 ?
N5B K2 O1 90.2(2) . . ?
N4A K2 O1 66.48(15) 1_655 . ?
N4A K2 N5A 145.63(18) 1_655 . ?
O1 K2 N5A 92.52(12) . . ?
N5B K2 N6B 77.0(2) . 2 ?
O1 K2 N6B 167.09(3) . 2 ?
N4A K2 N6A 126.03(16) 1_655 2 ?
O1 K2 N6A 167.09(3) . 2 ?
N5A K2 N6A 75.00(12) . 2 ?
N5B K2 N3 136.1(3) . 3_766 ?
N4A K2 N3 73.37(14) 1_655 3_766 ?
O1 K2 N3 103.17(3) . 3_766 ?
N5A K2 N3 140.17(13) . 3_766 ?
N6B K2 N3 85.01(3) 2 3_766 ?
N6A K2 N3 85.01(3) 2 3_766 ?
N5B K2 N4B 147.6(3) . 1_655 ?
O1 K2 N4B 63.2(3) . 1_655 ?
N6B K2 N4B 129.5(3) 2 1_655 ?
N3 K2 N4B 71.8(3) 3_766 1_655 ?
N5B K2 N1 82.4(3) . 4_565 ?
N4A K2 N1 82.03(16) 1_655 4_565 ?
O1 K2 N1 103.59(3) . 4_565 ?
N5A K2 N1 76.78(15) . 4_565 ?
N6B K2 N1 77.14(3) 2 4_565 ?
N6A K2 N1 77.14(3) 2 4_565 ?
N3 K2 N1 132.09(3) 3_766 4_565 ?
N4B K2 N1 86.1(3) 1_655 4_565 ?
N5B K2 N2 80.6(3) . 1_455 ?
N4A K2 N2 108.74(17) 1_655 1_455 ?
O1 K2 N2 68.79(3) . 1_455 ?
N5A K2 N2 86.37(15) . 1_455 ?
N6B K2 N2 106.43(3) 2 1_455 ?
N6A K2 N2 106.43(3) 2 1_455 ?
N3 K2 N2 66.50(3) 3_766 1_455 ?
N4B K2 N2 104.2(3) 1_655 1_455 ?
N1 K2 N2 161.33(3) 4_565 1_455 ?
N5B K2 C6B 85.1(3) . 2 ?
O1 K2 C6B 160.72(13) . 2 ?
N6B K2 C6B 18.23(16) 2 2 ?
N3 K2 C6B 68.59(18) 3_766 2 ?
N4B K2 C6B 126.1(3) 1_655 2 ?
N1 K2 C6B 94.33(14) 4_565 2 ?
N2 K2 C6B 91.98(13) 1_455 2 ?
N5B K2 C1 97.4(3) . 4_565 ?
N4A K2 C1 64.58(16) 1_655 4_565 ?
O1 K2 C1 94.71(2) . 4_565 ?
N5A K2 C1 92.03(15) . 4_565 ?
N6B K2 C1 89.13(3) 2 4_565 ?
N6A K2 C1 89.13(3) 2 4_565 ?
N3 K2 C1 122.21(3) 3_766 4_565 ?
N4B K2 C1 68.7(3) 1_655 4_565 ?
N1 K2 C1 17.46(3) 4_565 4_565 ?
N2 K2 C1 163.30(3) 1_455 4_565 ?
C6B K2 C1 104.43(13) 2 4_565 ?
C3 B1 C2 110.26(9) . . ?
C3 B1 C1 109.35(9) . . ?
C2 B1 C1 111.56(9) . . ?
C3 B1 H4 109.6(7) . . ?
C2 B1 H4 108.0(7) . . ?
C1 B1 H4 108.0(7) . . ?
N1 C1 B1 178.00(12) . . ?
N1 C1 K2 49.95(7) . 4_666 ?
B1 C1 K2 131.59(7) . 4_666 ?
C1 N1 K1 159.25(9) . . ?
C1 N1 K2 112.59(8) . 4_666 ?
K1 N1 K2 86.69(3) . 4_666 ?
N2 C2 B1 176.87(11) . . ?
C2 N2 K1 160.42(9) . 1_655 ?
C2 N2 K2 111.47(9) . 1_655 ?
K1 N2 K2 74.95(2) 1_655 1_655 ?
N3 C3 B1 177.20(11) . . ?
N3 C3 K1 57.05(7) . 3_766 ?
B1 C3 K1 120.23(7) . 3_766 ?
C3 N3 K2 154.30(8) . 3_766 ?
C3 N3 K1 104.03(8) . 3_766 ?
K2 N3 K1 76.34(2) 3_766 3_766 ?
C5A B2A C4A 110.4(2) . . ?
C5A B2A C6A 110.3(2) . . ?
C4A B2A C6A 112.3(2) . . ?
C5A B2A H2A 109.0(10) . . ?
C4A B2A H2A 107.6(10) . . ?
C6A B2A H2A 107.1(10) . . ?
N4A C4A B2A 176.5(4) . . ?
N4A C4A K1 73.2(4) . 1_455 ?
B2A C4A K1 104.01(14) . 1_455 ?
C4A N4A K2 160.5(6) . 1_455 ?
C4A N4A K1 86.1(5) . 1_455 ?
K2 N4A K1 74.61(14) 1_455 1_455 ?
N5A C5A B2A 179.1(5) . . ?
C5A N5A K1 133.1(4) . 4_565 ?
C5A N5A K2 136.8(5) . . ?
K1 N5A K2 90.05(14) 4_565 . ?
N6A C6A B2A 172.7(4) . . ?
C6A N6A K1 147.0(2) . 3_656 ?
C6A N6A K2 124.6(2) . 2_545 ?
K1 N6A K2 87.91(3) 3_656 2_545 ?
C6B B2B C5B 110.8(5) . . ?
C6B B2B C4B 111.9(5) . . ?
C5B B2B C4B 110.7(4) . . ?
C6B B2B H2B 108.8(19) . . ?
C5B B2B H2B 107.5(19) . . ?
C4B B2B H2B 107.1(19) . . ?
N4B C4B B2B 178.4(10) . . ?
C4B N4B K2 161.1(12) . 1_455 ?
C4B N4B K1 120.8(10) . 1_455 ?
K2 N4B K1 76.7(3) 1_455 1_455 ?
N5B C5B B2B 178.0(9) . . ?
N5B C5B K1 61.2(8) . 4_565 ?
B2B C5B K1 118.6(4) . 4_565 ?
C5B N5B K2 155.0(8) . . ?
C5B N5B K1 99.5(9) . 4_565 ?
K2 N5B K1 87.4(3) . 4_565 ?
B2B C6B K2 117.3(4) . 2_545 ?
C7 O1 K1 139.42(7) . . ?
C7 O1 K2 126.04(7) . . ?
K1 O1 K2 79.14(2) . . ?
O1 C7 C8 121.78(10) . . ?
O1 C7 C9 121.15(11) . . ?
C8 C7 C9 117.07(10) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?

_refine_diff_density_max         0.240
_refine_diff_density_min         -0.171
_refine_diff_density_rms         0.036


