# Electronic Supplementary Material (ESI) for Chemical Science.
# 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_JL096_JL_K2N2EtOAc
_database_code_depnum_ccdc_archive 'CCDC 1548897'
_audit_update_record             
;
2017-05-09 deposited with the CCDC.
2017-06-26 downloaded from the CCDC.
;


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

_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 B F3 K N3 O2'
_chemical_formula_sum            'C12 H8 B F3 K N3 O2'
_chemical_formula_weight         333.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
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'
N N 0.0061 0.0033 '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'

_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                   12.9371(9)
_cell_length_b                   7.5514(5)
_cell_length_c                   14.3323(10)
_cell_angle_alpha                90
_cell_angle_beta                 93.205(3)
_cell_angle_gamma                90
_cell_volume                     1397.98(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7338
_cell_measurement_theta_min      2.85
_cell_measurement_theta_max      26.75
_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).
;

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_F_000             672
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    0.423
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.659870
_exptl_absorpt_correction_T_max  0.745430
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17851
_diffrn_reflns_av_R_equivalents  0.0751
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.847
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        26.000
_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             2857
_reflns_number_gt                2516
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          
;
Refined as a 2-component twin.
The crystal was a pseudo-merohedral twin with domains rotated by 179.9 °
around real axis [ -0.001  0.000  1.000]. The BASF parameter was refined to 50%.

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)+(0.0377P)²+2.7374P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2857
_refine_ls_number_parameters     202
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0500
_refine_ls_wR_factor_ref         0.1260
_refine_ls_wR_factor_gt          0.1167
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.49775(7) -0.00779(10) 0.32187(5) 0.01707(18) Uani 1 1 d . . . . .
N1 N 0.5718(2) 0.3472(4) 0.3628(2) 0.0215(7) Uani 1 1 d . . . . .
O1 O 0.3395(2) 0.2091(4) 0.2474(2) 0.0327(7) Uani 1 1 d . . . . .
C1 C 0.6163(3) 0.4178(5) 0.4226(3) 0.0154(7) Uani 1 1 d . . . . .
N2 N 0.6111(2) 0.3499(4) 0.6649(2) 0.0214(7) Uani 1 1 d . . . . .
O2 O 0.1740(2) 0.1167(4) 0.2417(2) 0.0320(7) Uani 1 1 d . . . . .
C2 C 0.6386(3) 0.4229(5) 0.6009(3) 0.0157(7) Uani 1 1 d . . . . .
N3 N 0.6076(2) 0.8580(4) 0.4992(3) 0.0248(7) Uani 1 1 d . . . . .
C3 C 0.6383(2) 0.7168(4) 0.5051(3) 0.0163(7) Uani 1 1 d . . . . .
B4 B 0.6764(3) 0.5150(5) 0.5087(3) 0.0155(7) Uani 1 1 d . . . . .
C12 C 0.8010(3) 0.4898(5) 0.5029(3) 0.0200(8) Uani 1 1 d . . . . .
C13 C 0.8383(3) 0.3177(5) 0.4755(3) 0.0228(8) Uani 1 1 d . . . . .
F13 F 0.77213(17) 0.1870(3) 0.4632(2) 0.0347(6) Uani 1 1 d . . . . .
C14 C 0.9406(3) 0.2854(5) 0.4664(3) 0.0231(8) Uani 1 1 d . . . . .
F14 F 0.96843(18) 0.1241(3) 0.4367(2) 0.0320(6) Uani 1 1 d . . . . .
C15 C 1.0156(3) 0.4153(5) 0.4848(3) 0.0197(8) Uani 1 1 d . . . . .
C21 C 0.2042(3) 0.4013(6) 0.1881(3) 0.0309(10) Uani 1 1 d . . . . .
H00A H 0.1947 0.3889 0.1201 0.046 Uiso 1 1 calc R U . . .
H00B H 0.2516 0.4998 0.2031 0.046 Uiso 1 1 calc R U . . .
H00C H 0.1372 0.4249 0.2143 0.046 Uiso 1 1 calc R U . . .
C22 C 0.2483(3) 0.2357(6) 0.2286(3) 0.0274(9) Uani 1 1 d . . . . .
C23 C 0.2066(3) -0.0505(6) 0.2839(3) 0.0339(10) Uani 1 1 d . . . . .
H00G H 0.2435 -0.0301 0.3453 0.041 Uiso 1 1 calc R U . . .
H00H H 0.2535 -0.1141 0.2431 0.041 Uiso 1 1 calc R U . . .
C24 C 0.1100(3) -0.1564(6) 0.2954(3) 0.0360(11) Uani 1 1 d . . . . .
H00D H 0.0722 -0.1697 0.2347 0.054 Uiso 1 1 calc R U . . .
H00E H 0.0661 -0.0951 0.3387 0.054 Uiso 1 1 calc R U . . .
H00F H 0.1286 -0.2736 0.3205 0.054 Uiso 1 1 calc R U . . .
C11 C 0.8750(3) 0.6122(5) 0.5224(3) 0.0220(8) Uani 1 1 d . . . . .
F11 F 0.84548(16) 0.7725(3) 0.55034(17) 0.0294(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 O1 2.787(3) . ?
K1 N1 2.896(3) . ?
K1 N2 2.953(3) 3_656 ?
K1 N1 2.957(3) 2_645 ?
K1 N2 3.000(3) 4_565 ?
K1 N3 3.017(4) 1_545 ?
K1 N3 3.179(4) 3_666 ?
K1 O1 3.198(3) 2_645 ?
K1 K1 4.3031(7) 2_645 ?
K1 K1 4.3031(7) 2_655 ?
N1 C1 1.138(5) . ?
N1 K1 2.957(3) 2_655 ?
O1 C22 1.212(5) . ?
O1 K1 3.198(3) 2_655 ?
C1 B4 1.600(6) . ?
N2 C2 1.143(5) . ?
N2 K1 2.953(3) 3_656 ?
N2 K1 3.000(3) 4_566 ?
O2 C22 1.336(5) . ?
O2 C23 1.452(5) . ?
C2 B4 1.594(6) . ?
N3 C3 1.139(5) . ?
N3 K1 3.017(4) 1_565 ?
N3 K1 3.179(4) 3_666 ?
C3 B4 1.602(5) . ?
B4 C12 1.630(4) . ?
C12 C11 1.349(5) . ?
C12 C13 1.448(5) . ?
C13 F13 1.312(4) . ?
C13 C14 1.360(5) . ?
C14 F14 1.345(4) . ?
C14 C15 1.394(5) . ?
C15 C15 1.417(7) 3_766 ?
C15 C11 1.440(5) 3_766 ?
C21 C22 1.479(6) . ?
C21 H00A 0.9800 . ?
C21 H00B 0.9800 . ?
C21 H00C 0.9800 . ?
C23 C24 1.500(7) . ?
C23 H00G 0.9900 . ?
C23 H00H 0.9900 . ?
C24 H00D 0.9800 . ?
C24 H00E 0.9800 . ?
C24 H00F 0.9800 . ?
C11 F11 1.337(4) . ?
C11 C15 1.440(5) 3_766 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 K1 N1 76.19(9) . . ?
O1 K1 N2 101.29(10) . 3_656 ?
N1 K1 N2 161.86(9) . 3_656 ?
O1 K1 N1 72.22(9) . 2_645 ?
N1 K1 N1 127.20(9) . 2_645 ?
N2 K1 N1 67.13(9) 3_656 2_645 ?
O1 K1 N2 81.88(9) . 4_565 ?
N1 K1 N2 67.29(9) . 4_565 ?
N2 K1 N2 130.59(8) 3_656 4_565 ?
N1 K1 N2 67.24(9) 2_645 4_565 ?
O1 K1 N3 145.22(9) . 1_545 ?
N1 K1 N3 90.31(9) . 1_545 ?
N2 K1 N3 81.72(9) 3_656 1_545 ?
N1 K1 N3 137.30(9) 2_645 1_545 ?
N2 K1 N3 122.55(9) 4_565 1_545 ?
O1 K1 N3 76.17(9) . 3_666 ?
N1 K1 N3 70.08(9) . 3_666 ?
N2 K1 N3 91.82(9) 3_656 3_666 ?
N1 K1 N3 136.96(9) 2_645 3_666 ?
N2 K1 N3 135.49(9) 4_565 3_666 ?
N3 K1 N3 69.09(10) 1_545 3_666 ?
O1 K1 O1 139.15(4) . 2_645 ?
N1 K1 O1 117.76(8) . 2_645 ?
N2 K1 O1 76.10(8) 3_656 2_645 ?
N1 K1 O1 69.35(8) 2_645 2_645 ?
N2 K1 O1 71.03(8) 4_565 2_645 ?
N3 K1 O1 75.49(8) 1_545 2_645 ?
N3 K1 O1 143.89(8) 3_666 2_645 ?
O1 K1 K1 111.19(7) . 2_645 ?
N1 K1 K1 153.65(7) . 2_645 ?
N2 K1 K1 44.15(6) 3_656 2_645 ?
N1 K1 K1 42.13(7) 2_645 2_645 ?
N2 K1 K1 88.25(7) 4_565 2_645 ?
N3 K1 K1 95.17(7) 1_545 2_645 ?
N3 K1 K1 135.75(6) 3_666 2_645 ?
O1 K1 K1 40.35(5) 2_645 2_645 ?
O1 K1 K1 47.97(7) . 2_655 ?
N1 K1 K1 43.24(7) . 2_655 ?
N2 K1 K1 144.84(7) 3_656 2_655 ?
N1 K1 K1 84.72(7) 2_645 2_655 ?
N2 K1 K1 43.29(6) 4_565 2_655 ?
N3 K1 K1 132.81(7) 1_545 2_655 ?
N3 K1 K1 95.28(6) 3_666 2_655 ?
O1 K1 K1 114.29(6) 2_645 2_655 ?
K1 K1 K1 122.67(3) 2_645 2_655 ?
C1 N1 K1 137.2(3) . . ?
C1 N1 K1 128.1(3) . 2_655 ?
K1 N1 K1 94.63(10) . 2_655 ?
C22 O1 K1 150.2(3) . . ?
C22 O1 K1 118.0(3) . 2_655 ?
K1 O1 K1 91.68(8) . 2_655 ?
N1 C1 B4 178.3(4) . . ?
C2 N2 K1 130.1(3) . 3_656 ?
C2 N2 K1 126.6(3) . 4_566 ?
K1 N2 K1 92.56(9) 3_656 4_566 ?
C22 O2 C23 116.7(3) . . ?
N2 C2 B4 177.0(4) . . ?
C3 N3 K1 121.6(3) . 1_565 ?
C3 N3 K1 115.8(3) . 3_666 ?
K1 N3 K1 110.91(9) 1_565 3_666 ?
N3 C3 B4 176.6(4) . . ?
C2 B4 C1 106.3(3) . . ?
C2 B4 C3 109.5(3) . . ?
C1 B4 C3 106.0(3) . . ?
C2 B4 C12 110.0(3) . . ?
C1 B4 C12 110.2(3) . . ?
C3 B4 C12 114.4(3) . . ?
C11 C12 C13 115.3(3) . . ?
C11 C12 B4 127.0(3) . . ?
C13 C12 B4 117.7(3) . . ?
F13 C13 C14 118.9(3) . . ?
F13 C13 C12 119.1(3) . . ?
C14 C13 C12 121.9(3) . . ?
F14 C14 C13 118.1(3) . . ?
F14 C14 C15 120.1(3) . . ?
C13 C14 C15 121.7(3) . . ?
C14 C15 C15 119.2(4) . 3_766 ?
C14 C15 C11 124.1(3) . 3_766 ?
C15 C15 C11 116.7(4) 3_766 3_766 ?
C22 C21 H00A 109.5 . . ?
C22 C21 H00B 109.5 . . ?
H00A C21 H00B 109.5 . . ?
C22 C21 H00C 109.5 . . ?
H00A C21 H00C 109.5 . . ?
H00B C21 H00C 109.5 . . ?
O1 C22 O2 123.8(4) . . ?
O1 C22 C21 125.2(4) . . ?
O2 C22 C21 111.1(3) . . ?
O2 C23 C24 106.6(3) . . ?
O2 C23 H00G 110.4 . . ?
C24 C23 H00G 110.4 . . ?
O2 C23 H00H 110.4 . . ?
C24 C23 H00H 110.4 . . ?
H00G C23 H00H 108.6 . . ?
C23 C24 H00D 109.5 . . ?
C23 C24 H00E 109.5 . . ?
H00D C24 H00E 109.5 . . ?
C23 C24 H00F 109.5 . . ?
H00D C24 H00F 109.5 . . ?
H00E C24 H00F 109.5 . . ?
F11 C11 C12 118.1(3) . . ?
F11 C11 C15 116.8(3) . 3_766 ?
C12 C11 C15 125.1(3) . 3_766 ?

_refine_diff_density_max         0.920
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.087

####################################################################### 
# 
# 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_JL027_JL_KBP2thf
_database_code_depnum_ccdc_archive 'CCDC 1548896'
_audit_update_record             
;
2017-05-09 deposited with the CCDC.
2017-06-26 downloaded from the CCDC.
;


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

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H16 B2 F8 K2 N6 O2'
_chemical_formula_sum            'C26 H16 B2 F8 K2 N6 O2'
_chemical_formula_weight         696.27

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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 2'
_space_group_name_Hall           'C 2y'

_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'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   28.487(4)
_cell_length_b                   12.3676(16)
_cell_length_c                   8.8225(11)
_cell_angle_alpha                90
_cell_angle_beta                 94.050(5)
_cell_angle_gamma                90
_cell_volume                     3100.6(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7750
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      26.34
_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).
;

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_F_000             1400
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.389
_shelx_estimated_absorpt_T_min   0.926
_shelx_estimated_absorpt_T_max   0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7003
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21628
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.433
_diffrn_reflns_theta_max         26.785
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6608
_reflns_number_gt                5996
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.906
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    0.999

_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. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0269P)²+0.5359P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2562 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(13)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6608
_refine_ls_number_parameters     415
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0301
_refine_ls_wR_factor_ref         0.0611
_refine_ls_wR_factor_gt          0.0588
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_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 0.32138(2) 0.83084(5) 0.99531(7) 0.02035(14) Uani 1 1 d . . . . .
N1 N 0.73101(8) 0.37086(19) 0.8396(3) 0.0216(5) Uani 1 1 d . . . . .
O1 O 0.33523(7) 0.92171(17) 0.7208(2) 0.0255(5) Uani 1 1 d . . . . .
C1 C 0.70104(9) 0.3148(2) 0.7968(3) 0.0167(6) Uani 1 1 d . . . . .
B1 B 0.66215(10) 0.2292(3) 0.7348(4) 0.0153(6) Uani 1 1 d . . . . .
O2 O 0.41513(7) 0.82130(19) 1.0508(3) 0.0403(6) Uani 1 1 d . . . . .
K2 K 0.22979(2) 0.58717(4) 0.20605(6) 0.01681(13) Uani 1 1 d . . . . .
N2 N 0.67680(8) 0.04590(19) 0.9078(3) 0.0203(5) Uani 1 1 d . . . . .
C2 C 0.67083(9) 0.1209(2) 0.8346(3) 0.0147(6) Uani 1 1 d . . . . .
B2 B 0.30967(10) 0.4607(3) 0.7470(4) 0.0164(6) Uani 1 1 d . . . . .
C4 C 0.30377(9) 0.5507(2) 0.8743(3) 0.0180(6) Uani 1 1 d . . . . .
N4 N 0.29995(9) 0.6143(2) 0.9665(3) 0.0261(6) Uani 1 1 d . . . . .
C3 C 0.67173(9) 0.2019(2) 0.5634(3) 0.0166(6) Uani 1 1 d . . . . .
N3 N 0.67832(9) 0.1817(2) 0.4404(3) 0.0255(6) Uani 1 1 d . . . . .
C5 C 0.29625(10) 0.5140(2) 0.5839(4) 0.0210(6) Uani 1 1 d . . . . .
N5 N 0.28594(9) 0.5496(2) 0.4674(3) 0.0329(7) Uani 1 1 d . . . . .
C6 C 0.27114(10) 0.3692(2) 0.7673(3) 0.0170(6) Uani 1 1 d . . . . .
N6 N 0.24168(8) 0.30821(19) 0.7787(3) 0.0216(6) Uani 1 1 d . . . . .
C11 C 0.60793(9) 0.2674(2) 0.7460(3) 0.0157(6) Uani 1 1 d . . . . .
C12 C 0.59319(9) 0.3634(2) 0.8068(3) 0.0155(6) Uani 1 1 d . . . . .
F12 F 0.62480(5) 0.43747(13) 0.86129(19) 0.0221(4) Uani 1 1 d . . . . .
C14 C 0.51038(9) 0.3202(2) 0.7638(3) 0.0179(6) Uani 1 1 d . . . . .
C13 C 0.54619(10) 0.3893(2) 0.8166(3) 0.0178(6) Uani 1 1 d . . . . .
F13 F 0.53545(5) 0.48349(13) 0.88114(19) 0.0252(4) Uani 1 1 d . . . . .
C15 C 0.52440(9) 0.2224(2) 0.7042(3) 0.0185(6) Uani 1 1 d . . . . .
F15 F 0.49183(5) 0.15057(13) 0.6517(2) 0.0250(4) Uani 1 1 d . . . . .
C16 C 0.57151(10) 0.1983(2) 0.6950(3) 0.0173(6) Uani 1 1 d . . . . .
F16 F 0.58226(5) 0.10252(13) 0.63286(18) 0.0235(4) Uani 1 1 d . . . . .
C17 C 0.46023(9) 0.3518(2) 0.7634(3) 0.0182(6) Uani 1 1 d . . . . .
C19 C 0.39848(10) 0.4810(2) 0.6980(3) 0.0210(6) Uani 1 1 d . . . . .
F19 F 0.38758(5) 0.57883(14) 0.6374(2) 0.0308(4) Uani 1 1 d . . . . .
C18 C 0.44480(9) 0.4488(2) 0.6981(3) 0.0212(6) Uani 1 1 d . . . . .
F18 F 0.47540(6) 0.51347(15) 0.6327(2) 0.0318(4) Uani 1 1 d . . . . .
C20 C 0.36385(9) 0.4182(2) 0.7565(3) 0.0157(6) Uani 1 1 d . . . . .
C21 C 0.37971(9) 0.3214(2) 0.8220(3) 0.0160(6) Uani 1 1 d . . . . .
F21 F 0.34945(5) 0.25585(12) 0.88925(18) 0.0203(4) Uani 1 1 d . . . . .
C22 C 0.42619(10) 0.2893(2) 0.8261(3) 0.0163(6) Uani 1 1 d . . . . .
F22 F 0.43852(6) 0.19581(13) 0.89628(19) 0.0225(4) Uani 1 1 d . . . . .
C30 C 0.43839(13) 0.9079(3) 1.1336(4) 0.0404(9) Uani 1 1 d . . . . .
H30A H 0.4171 0.9405 1.2049 0.048 Uiso 1 1 calc R U . . .
H30B H 0.4479 0.9647 1.0628 0.048 Uiso 1 1 calc R U . . .
C31 C 0.48100(13) 0.8608(3) 1.2194(5) 0.0456(10) Uani 1 1 d . . . . .
H31A H 0.4882 0.8988 1.3171 0.055 Uiso 1 1 calc R U . . .
H31B H 0.5089 0.8636 1.1587 0.055 Uiso 1 1 calc R U . . .
C32 C 0.46534(14) 0.7444(3) 1.2446(5) 0.0562(12) Uani 1 1 d . . . . .
H32A H 0.4927 0.6950 1.2579 0.067 Uiso 1 1 calc R U . . .
H32B H 0.4465 0.7387 1.3342 0.067 Uiso 1 1 calc R U . . .
C33 C 0.43587(13) 0.7202(3) 1.0992(5) 0.0462(10) Uani 1 1 d . . . . .
H33A H 0.4558 0.6913 1.0210 0.055 Uiso 1 1 calc R U . . .
H33B H 0.4112 0.6665 1.1177 0.055 Uiso 1 1 calc R U . . .
C40 C 0.38330(10) 0.9529(3) 0.6994(4) 0.0297(7) Uani 1 1 d . . . . .
H40A H 0.4030 0.9470 0.7960 0.036 Uiso 1 1 calc R U . . .
H40B H 0.3846 1.0283 0.6622 0.036 Uiso 1 1 calc R U . . .
C41 C 0.40005(11) 0.8748(3) 0.5822(4) 0.0363(8) Uani 1 1 d . . . . .
H41A H 0.4120 0.8068 0.6301 0.044 Uiso 1 1 calc R U . . .
H41B H 0.4249 0.9074 0.5241 0.044 Uiso 1 1 calc R U . . .
C42 C 0.35529(11) 0.8556(3) 0.4819(4) 0.0388(9) Uani 1 1 d . . . . .
H42A H 0.3499 0.9143 0.4063 0.047 Uiso 1 1 calc R U . . .
H42B H 0.3564 0.7855 0.4281 0.047 Uiso 1 1 calc R U . . .
C43 C 0.31806(11) 0.8552(3) 0.5935(4) 0.0396(9) Uani 1 1 d . . . . .
H43A H 0.2883 0.8851 0.5463 0.047 Uiso 1 1 calc R U . . .
H43B H 0.3122 0.7806 0.6279 0.047 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 2.684(2) . ?
K1 O1 2.724(2) . ?
K1 N4 2.754(3) . ?
K1 N6 2.791(3) 4_557 ?
K1 N2 2.793(2) 2_667 ?
K1 N1 2.874(2) 3_455 ?
K1 C6 3.512(3) 4_557 ?
K1 K2 3.8685(9) 4_556 ?
K1 K2 4.4756(9) 1_556 ?
N1 C1 1.143(3) . ?
N1 K1 2.874(2) 3_545 ?
N1 K2 2.938(2) 2_656 ?
O1 C40 1.448(3) . ?
O1 C43 1.449(4) . ?
O1 K2 2.864(2) 4_556 ?
C1 B1 1.601(4) . ?
B1 C3 1.591(4) . ?
B1 C2 1.612(4) . ?
B1 C11 1.625(4) . ?
O2 C30 1.432(4) . ?
O2 C33 1.435(4) . ?
K2 N5 2.751(3) . ?
K2 N6 2.852(2) 4_556 ?
K2 O1 2.864(2) 4_546 ?
K2 N3 2.867(3) 3_455 ?
K2 N1 2.938(2) 2_656 ?
K2 N2 2.984(2) 3_454 ?
K2 N4 3.029(3) 1_554 ?
K2 F21 3.1445(16) 4_556 ?
K2 C6 3.496(3) 4_556 ?
K2 K1 3.8684(9) 4_546 ?
K2 K1 4.4756(9) 1_554 ?
N2 C2 1.136(3) . ?
N2 K1 2.793(2) 2_647 ?
N2 K2 2.984(2) 3_546 ?
B2 C6 1.595(4) . ?
B2 C4 1.599(4) . ?
B2 C5 1.604(4) . ?
B2 C20 1.627(4) . ?
C4 N4 1.142(4) . ?
N4 K2 3.029(3) 1_556 ?
C3 N3 1.142(4) . ?
N3 K2 2.867(3) 3_545 ?
C5 N5 1.138(4) . ?
C6 N6 1.138(3) . ?
C6 K2 3.496(3) 4_546 ?
C6 K1 3.512(3) 4_547 ?
N6 K1 2.790(3) 4_547 ?
N6 K2 2.853(2) 4_546 ?
C11 C12 1.380(4) . ?
C11 C16 1.395(4) . ?
C12 F12 1.350(3) . ?
C12 C13 1.386(4) . ?
C14 C13 1.387(4) . ?
C14 C15 1.389(4) . ?
C14 C17 1.481(4) . ?
C13 F13 1.341(3) . ?
C15 F15 1.343(3) . ?
C15 C16 1.383(4) . ?
C16 F16 1.349(3) . ?
C17 C22 1.386(4) . ?
C17 C18 1.389(4) . ?
C19 F19 1.349(3) . ?
C19 C18 1.378(4) . ?
C19 C20 1.384(4) . ?
C18 F18 1.342(3) . ?
C20 C21 1.391(4) . ?
C21 F21 1.351(3) . ?
C21 C22 1.380(4) . ?
F21 K2 3.1444(16) 4_546 ?
C22 F22 1.346(3) . ?
C30 C31 1.502(5) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.529(6) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.512(6) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C40 C41 1.517(5) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.519(5) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.497(5) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?

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 O1 88.60(7) . . ?
O2 K1 N4 100.68(7) . . ?
O1 K1 N4 111.35(7) . . ?
O2 K1 N6 123.21(8) . 4_557 ?
O1 K1 N6 144.86(7) . 4_557 ?
N4 K1 N6 79.57(7) . 4_557 ?
O2 K1 N2 89.38(7) . 2_667 ?
O1 K1 N2 83.02(7) . 2_667 ?
N4 K1 N2 162.43(8) . 2_667 ?
N6 K1 N2 82.87(7) 4_557 2_667 ?
O2 K1 N1 160.23(8) . 3_455 ?
O1 K1 N1 71.64(6) . 3_455 ?
N4 K1 N1 86.45(7) . 3_455 ?
N6 K1 N1 76.04(7) 4_557 3_455 ?
N2 K1 N1 88.80(7) 2_667 3_455 ?
O2 K1 C6 132.55(7) . 4_557 ?
O1 K1 C6 129.52(7) . 4_557 ?
N4 K1 C6 90.90(7) . 4_557 ?
N6 K1 C6 16.16(6) 4_557 4_557 ?
N2 K1 C6 71.79(7) 2_667 4_557 ?
N1 K1 C6 64.99(7) 3_455 4_557 ?
O2 K1 K2 117.24(6) . 4_556 ?
O1 K1 K2 47.71(4) . 4_556 ?
N4 K1 K2 132.88(6) . 4_556 ?
N6 K1 K2 99.77(5) 4_557 4_556 ?
N2 K1 K2 50.09(5) 2_667 4_556 ?
N1 K1 K2 48.97(5) 3_455 4_556 ?
C6 K1 K2 83.62(5) 4_557 4_556 ?
O2 K1 K2 119.76(6) . 1_556 ?
O1 K1 K2 140.58(5) . 1_556 ?
N4 K1 K2 41.57(6) . 1_556 ?
N6 K1 K2 38.01(5) 4_557 1_556 ?
N2 K1 K2 120.86(5) 2_667 1_556 ?
N1 K1 K2 77.63(5) 3_455 1_556 ?
C6 K1 K2 50.16(5) 4_557 1_556 ?
K2 K1 K2 122.058(17) 4_556 1_556 ?
C1 N1 K1 132.5(2) . 3_545 ?
C1 N1 K2 142.2(2) . 2_656 ?
K1 N1 K2 83.46(6) 3_545 2_656 ?
C40 O1 C43 108.7(2) . . ?
C40 O1 K1 115.08(17) . . ?
C43 O1 K1 113.1(2) . . ?
C40 O1 K2 118.15(17) . 4_556 ?
C43 O1 K2 113.06(17) . 4_556 ?
K1 O1 K2 87.59(6) . 4_556 ?
N1 C1 B1 175.5(3) . . ?
C3 B1 C1 107.7(2) . . ?
C3 B1 C2 108.2(2) . . ?
C1 B1 C2 106.7(2) . . ?
C3 B1 C11 110.3(2) . . ?
C1 B1 C11 115.1(2) . . ?
C2 B1 C11 108.6(2) . . ?
C30 O2 C33 109.5(3) . . ?
C30 O2 K1 118.61(19) . . ?
C33 O2 K1 118.4(2) . . ?
N5 K2 N6 88.59(8) . 4_556 ?
N5 K2 O1 92.16(7) . 4_546 ?
N6 K2 O1 149.39(7) 4_556 4_546 ?
N5 K2 N3 76.19(8) . 3_455 ?
N6 K2 N3 74.55(7) 4_556 3_455 ?
O1 K2 N3 75.94(7) 4_546 3_455 ?
N5 K2 N1 75.93(8) . 2_656 ?
N6 K2 N1 140.31(7) 4_556 2_656 ?
O1 K2 N1 68.80(6) 4_546 2_656 ?
N3 K2 N1 133.55(7) 3_455 2_656 ?
N5 K2 N2 159.75(8) . 3_454 ?
N6 K2 N2 109.29(7) 4_556 3_454 ?
O1 K2 N2 77.37(6) 4_546 3_454 ?
N3 K2 N2 116.93(7) 3_455 3_454 ?
N1 K2 N2 84.09(7) 2_656 3_454 ?
N5 K2 N4 103.32(8) . 1_554 ?
N6 K2 N4 74.15(7) 4_556 1_554 ?
O1 K2 N4 134.88(7) 4_546 1_554 ?
N3 K2 N4 148.69(7) 3_455 1_554 ?
N1 K2 N4 74.30(7) 2_656 1_554 ?
N2 K2 N4 73.81(7) 3_454 1_554 ?
N5 K2 F21 134.43(7) . 4_556 ?
N6 K2 F21 64.76(6) 4_556 4_556 ?
O1 K2 F21 94.05(5) 4_546 4_556 ?
N3 K2 F21 61.84(6) 3_455 4_556 ?
N1 K2 F21 147.17(6) 2_656 4_556 ?
N2 K2 F21 64.45(5) 3_454 4_556 ?
N4 K2 F21 103.68(6) 1_554 4_556 ?
N5 K2 C6 96.83(8) . 4_556 ?
N6 K2 C6 17.09(6) 4_556 4_556 ?
O1 K2 C6 133.59(7) 4_546 4_556 ?
N3 K2 C6 62.48(7) 3_455 4_556 ?
N1 K2 C6 157.30(7) 2_656 4_556 ?
N2 K2 C6 102.95(6) 3_454 4_556 ?
N4 K2 C6 86.83(7) 1_554 4_556 ?
F21 K2 C6 49.26(5) 4_556 4_556 ?
N5 K2 K1 115.11(6) . 4_546 ?
N6 K2 K1 154.68(5) 4_556 4_546 ?
O1 K2 K1 44.70(4) 4_546 4_546 ?
N3 K2 K1 118.04(5) 3_455 4_546 ?
N1 K2 K1 47.57(5) 2_656 4_546 ?
N2 K2 K1 45.90(5) 3_454 4_546 ?
N4 K2 K1 90.93(5) 1_554 4_546 ?
F21 K2 K1 100.42(3) 4_556 4_546 ?
C6 K2 K1 147.57(5) 4_556 4_546 ?
N5 K2 K1 98.07(6) . 1_554 ?
N6 K2 K1 37.04(5) 4_556 1_554 ?
O1 K2 K1 168.49(5) 4_546 1_554 ?
N3 K2 K1 111.58(5) 3_455 1_554 ?
N1 K2 K1 108.54(5) 2_656 1_554 ?
N2 K2 K1 91.28(5) 3_454 1_554 ?
N4 K2 K1 37.12(5) 1_554 1_554 ?
F21 K2 K1 82.57(3) 4_556 1_554 ?
C6 K2 K1 50.47(5) 4_556 1_554 ?
K1 K2 K1 124.947(17) 4_546 1_554 ?
C2 N2 K1 161.8(2) . 2_647 ?
C2 N2 K2 114.07(19) . 3_546 ?
K1 N2 K2 84.01(6) 2_647 3_546 ?
N2 C2 B1 178.5(3) . . ?
C6 B2 C4 107.9(2) . . ?
C6 B2 C5 105.7(2) . . ?
C4 B2 C5 108.3(2) . . ?
C6 B2 C20 115.0(2) . . ?
C4 B2 C20 109.6(2) . . ?
C5 B2 C20 110.1(2) . . ?
N4 C4 B2 179.1(3) . . ?
C4 N4 K1 134.7(2) . . ?
C4 N4 K2 121.4(2) . 1_556 ?
K1 N4 K2 101.31(8) . 1_556 ?
N3 C3 B1 179.5(3) . . ?
C3 N3 K2 154.3(2) . 3_545 ?
N5 C5 B2 178.2(3) . . ?
C5 N5 K2 157.0(2) . . ?
N6 C6 B2 175.9(3) . . ?
N6 C6 K2 47.44(16) . 4_546 ?
B2 C6 K2 136.35(17) . 4_546 ?
N6 C6 K1 43.03(16) . 4_547 ?
B2 C6 K1 135.59(17) . 4_547 ?
K2 C6 K1 79.38(6) 4_546 4_547 ?
C6 N6 K1 120.8(2) . 4_547 ?
C6 N6 K2 115.47(19) . 4_546 ?
K1 N6 K2 104.95(8) 4_547 4_546 ?
C12 C11 C16 114.4(2) . . ?
C12 C11 B1 126.2(2) . . ?
C16 C11 B1 119.4(2) . . ?
F12 C12 C11 120.6(2) . . ?
F12 C12 C13 116.3(2) . . ?
C11 C12 C13 123.1(2) . . ?
C13 C14 C15 116.1(2) . . ?
C13 C14 C17 121.6(3) . . ?
C15 C14 C17 122.2(2) . . ?
F13 C13 C12 118.6(2) . . ?
F13 C13 C14 119.6(2) . . ?
C12 C13 C14 121.8(2) . . ?
F15 C15 C16 119.2(2) . . ?
F15 C15 C14 119.8(2) . . ?
C16 C15 C14 121.1(2) . . ?
F16 C16 C15 117.5(2) . . ?
F16 C16 C11 119.0(2) . . ?
C15 C16 C11 123.5(2) . . ?
C22 C17 C18 116.0(2) . . ?
C22 C17 C14 123.6(3) . . ?
C18 C17 C14 120.4(3) . . ?
F19 C19 C18 116.9(3) . . ?
F19 C19 C20 120.1(2) . . ?
C18 C19 C20 123.0(3) . . ?
F18 C18 C19 118.6(3) . . ?
F18 C18 C17 119.8(2) . . ?
C19 C18 C17 121.6(3) . . ?
C19 C20 C21 114.8(2) . . ?
C19 C20 B2 119.9(2) . . ?
C21 C20 B2 125.4(2) . . ?
F21 C21 C22 117.1(2) . . ?
F21 C21 C20 120.0(2) . . ?
C22 C21 C20 122.8(2) . . ?
C21 F21 K2 138.53(14) . 4_546 ?
F22 C22 C21 118.5(2) . . ?
F22 C22 C17 119.7(2) . . ?
C21 C22 C17 121.7(2) . . ?
O2 C30 C31 107.2(3) . . ?
O2 C30 H30A 110.3 . . ?
C31 C30 H30A 110.3 . . ?
O2 C30 H30B 110.3 . . ?
C31 C30 H30B 110.3 . . ?
H30A C30 H30B 108.5 . . ?
C30 C31 C32 101.8(3) . . ?
C30 C31 H31A 111.4 . . ?
C32 C31 H31A 111.4 . . ?
C30 C31 H31B 111.4 . . ?
C32 C31 H31B 111.4 . . ?
H31A C31 H31B 109.3 . . ?
C33 C32 C31 102.3(3) . . ?
C33 C32 H32A 111.3 . . ?
C31 C32 H32A 111.3 . . ?
C33 C32 H32B 111.3 . . ?
C31 C32 H32B 111.3 . . ?
H32A C32 H32B 109.2 . . ?
O2 C33 C32 105.8(3) . . ?
O2 C33 H33A 110.6 . . ?
C32 C33 H33A 110.6 . . ?
O2 C33 H33B 110.6 . . ?
C32 C33 H33B 110.6 . . ?
H33A C33 H33B 108.7 . . ?
O1 C40 C41 105.4(3) . . ?
O1 C40 H40A 110.7 . . ?
C41 C40 H40A 110.7 . . ?
O1 C40 H40B 110.7 . . ?
C41 C40 H40B 110.7 . . ?
H40A C40 H40B 108.8 . . ?
C40 C41 C42 101.8(3) . . ?
C40 C41 H41A 111.4 . . ?
C42 C41 H41A 111.4 . . ?
C40 C41 H41B 111.4 . . ?
C42 C41 H41B 111.4 . . ?
H41A C41 H41B 109.3 . . ?
C43 C42 C41 102.8(3) . . ?
C43 C42 H42A 111.2 . . ?
C41 C42 H42A 111.2 . . ?
C43 C42 H42B 111.2 . . ?
C41 C42 H42B 111.2 . . ?
H42A C42 H42B 109.1 . . ?
O1 C43 C42 107.0(3) . . ?
O1 C43 H43A 110.3 . . ?
C42 C43 H43A 110.3 . . ?
O1 C43 H43B 110.3 . . ?
C42 C43 H43B 110.3 . . ?
H43A C43 H43B 108.6 . . ?

_refine_diff_density_max         0.272
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.042

####################################################################### 
# 
# 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_JL086_JL_Et3NH2B4D
_database_code_depnum_ccdc_archive 'CCDC 1548893'
_audit_update_record             
;
2017-05-09 deposited with the CCDC.
2017-06-26 downloaded from the CCDC.
;


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

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H2 B2 F2 N6, 2(C6 H16 N)'
_chemical_formula_sum            'C24 H34 B2 F2 N8'
_chemical_formula_weight         494.21

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'
F F 0.0171 0.0103 '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                   7.2310(18)
_cell_length_b                   10.113(3)
_cell_length_c                   10.502(3)
_cell_angle_alpha                98.148(9)
_cell_angle_beta                 105.678(9)
_cell_angle_gamma                106.755(8)
_cell_volume                     687.6(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2372
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      26.74

_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).
;

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_F_000             262
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    0.083
_shelx_estimated_absorpt_T_min   0.972
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5933
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9798
_diffrn_reflns_av_unetI/netI     0.0725
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.166
_diffrn_reflns_theta_max         26.973
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             2926
_reflns_number_gt                1980
_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. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0668P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2926
_refine_ls_number_parameters     231
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0458
_refine_ls_wR_factor_ref         0.1260
_refine_ls_wR_factor_gt          0.1081
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_restrained_S_all      0.984
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
F1 F -0.18037(16) 0.21732(10) 0.89355(11) 0.0289(3) Uani 1 1 d . . . . .
H1 H -0.291(3) 0.371(2) 1.0425(18) 0.019(5) Uiso 1 1 d . . . . .
N1 N 0.2778(2) 0.13140(17) 0.91980(16) 0.0271(4) Uani 1 1 d . . . . .
C1 C 0.2349(3) 0.22031(18) 0.87689(16) 0.0160(4) Uani 1 1 d . . . . .
B1 B 0.1661(3) 0.34148(19) 0.81570(17) 0.0142(4) Uani 1 1 d . . . . .
C2 C -0.0085(3) 0.26581(17) 0.67124(16) 0.0162(4) Uani 1 1 d . . . . .
N2 N -0.1337(2) 0.21215(16) 0.56770(14) 0.0232(4) Uani 1 1 d . . . . .
N3 N 0.4834(2) 0.52702(15) 0.76446(15) 0.0215(4) Uani 1 1 d . . . . .
C3 C 0.3545(3) 0.44765(17) 0.78706(16) 0.0162(4) Uani 1 1 d . . . . .
C4 C 0.0831(2) 0.42790(16) 0.91521(15) 0.0133(4) Uani 1 1 d . . . . .
C5 C -0.0870(3) 0.36087(16) 0.94684(16) 0.0156(4) Uani 1 1 d . . . . .
C6 C -0.1727(3) 0.42615(18) 1.02732(16) 0.0162(4) Uani 1 1 d . . . . .
C11 C 0.9301(3) 0.77106(19) 0.70150(18) 0.0199(4) Uani 1 1 d . . . . .
H11 H 0.779(3) 0.982(2) 0.7249(19) 0.020(5) Uiso 1 1 d . . . . .
N11 N 0.7166(2) 0.76964(15) 0.68711(13) 0.0152(3) Uani 1 1 d . . . . .
C12 C 0.9331(3) 0.6251(2) 0.6472(2) 0.0240(4) Uani 1 1 d . . . . .
H12 H 0.808(3) 0.919(2) 0.857(2) 0.030(5) Uiso 1 1 d . . . . .
C13 C 0.5759(3) 0.72794(18) 0.54106(16) 0.0182(4) Uani 1 1 d . . . . .
H13 H 0.443(3) 0.818(2) 0.7994(19) 0.023(5) Uiso 1 1 d . . . . .
C14 C 0.6314(3) 0.8356(2) 0.45953(18) 0.0242(4) Uani 1 1 d . . . . .
H14 H 0.523(3) 0.984(2) 0.832(2) 0.034(6) Uiso 1 1 d . . . . .
C15 C 0.7195(3) 0.90742(18) 0.76690(18) 0.0194(4) Uani 1 1 d . . . . .
H15 H 0.418(3) 0.898(2) 0.682(2) 0.031(5) Uiso 1 1 d . . . . .
C16 C 0.5099(3) 0.9012(2) 0.76960(18) 0.0212(4) Uani 1 1 d . . . . .
H17 H 0.992(3) 0.8411(19) 0.6527(18) 0.016(4) Uiso 1 1 d . . . . .
H18 H 0.864(3) 0.559(2) 0.695(2) 0.024(5) Uiso 1 1 d . . . . .
H19 H 1.080(3) 0.634(2) 0.670(2) 0.034(6) Uiso 1 1 d . . . . .
H20 H 0.867(3) 0.593(2) 0.551(2) 0.026(5) Uiso 1 1 d . . . . .
H21 H 0.578(3) 0.635(2) 0.499(2) 0.030(5) Uiso 1 1 d . . . . .
H22 H 0.435(3) 0.7155(19) 0.5456(18) 0.017(5) Uiso 1 1 d . . . . .
H24 H 0.621(3) 0.928(2) 0.499(2) 0.034(6) Uiso 1 1 d . . . . .
H25 H 0.536(3) 0.800(2) 0.370(2) 0.037(6) Uiso 1 1 d . . . . .
H26 H 0.775(4) 0.853(2) 0.455(2) 0.039(6) Uiso 1 1 d . . . . .
H31 H 0.658(3) 0.697(2) 0.7271(19) 0.023(5) Uiso 1 1 d . . . . .
H16 H 1.004(3) 0.805(2) 0.799(2) 0.031(5) Uiso 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
F1 C5 1.3699(19) . ?
N1 C1 1.144(2) . ?
C1 B1 1.601(3) . ?
B1 C2 1.600(2) . ?
B1 C3 1.603(3) . ?
B1 C4 1.612(2) . ?
C2 N2 1.146(2) . ?
N3 C3 1.145(2) . ?
C4 C5 1.374(2) . ?
C4 C6 1.395(2) 2_567 ?
C5 C6 1.376(2) . ?
C6 C4 1.395(2) 2_567 ?
C6 H1 0.95(2) . ?
C11 N11 1.506(2) . ?
C11 C12 1.513(3) . ?
C11 H17 1.003(18) . ?
C11 H16 0.97(2) . ?
N11 C15 1.512(2) . ?
N11 C13 1.514(2) . ?
N11 H31 0.95(2) . ?
C12 H18 0.993(19) . ?
C12 H19 1.00(2) . ?
C12 H20 0.96(2) . ?
C13 C14 1.509(3) . ?
C13 H21 0.98(2) . ?
C13 H22 1.006(19) . ?
C14 H24 1.00(2) . ?
C14 H25 0.95(2) . ?
C14 H26 1.02(2) . ?
C15 C16 1.507(3) . ?
C15 H11 0.981(19) . ?
C15 H12 0.96(2) . ?
C16 H13 0.98(2) . ?
C16 H14 0.95(2) . ?
C16 H15 0.97(2) . ?

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
N1 C1 B1 177.88(18) . . ?
C2 B1 C1 107.54(13) . . ?
C2 B1 C3 106.76(13) . . ?
C1 B1 C3 109.36(14) . . ?
C2 B1 C4 110.41(14) . . ?
C1 B1 C4 112.06(13) . . ?
C3 B1 C4 110.52(14) . . ?
N2 C2 B1 179.69(18) . . ?
N3 C3 B1 176.83(17) . . ?
C5 C4 C6 115.18(15) . 2_567 ?
C5 C4 B1 121.17(14) . . ?
C6 C4 B1 123.63(15) 2_567 . ?
F1 C5 C4 117.56(15) . . ?
F1 C5 C6 117.04(15) . . ?
C4 C5 C6 125.40(16) . . ?
C5 C6 C4 119.42(17) . 2_567 ?
C5 C6 H1 119.0(12) . . ?
C4 C6 H1 121.6(11) 2_567 . ?
N11 C11 C12 111.98(15) . . ?
N11 C11 H17 108.7(10) . . ?
C12 C11 H17 110.7(11) . . ?
N11 C11 H16 104.4(12) . . ?
C12 C11 H16 111.4(12) . . ?
H17 C11 H16 109.4(15) . . ?
C11 N11 C15 111.19(13) . . ?
C11 N11 C13 113.90(14) . . ?
C15 N11 C13 112.90(13) . . ?
C11 N11 H31 107.0(12) . . ?
C15 N11 H31 106.4(12) . . ?
C13 N11 H31 104.8(11) . . ?
C11 C12 H18 107.4(12) . . ?
C11 C12 H19 106.1(13) . . ?
H18 C12 H19 110.9(17) . . ?
C11 C12 H20 111.5(12) . . ?
H18 C12 H20 110.9(16) . . ?
H19 C12 H20 109.8(17) . . ?
C14 C13 N11 114.04(15) . . ?
C14 C13 H21 111.0(12) . . ?
N11 C13 H21 107.0(12) . . ?
C14 C13 H22 109.9(10) . . ?
N11 C13 H22 106.1(10) . . ?
H21 C13 H22 108.6(15) . . ?
C13 C14 H24 111.0(12) . . ?
C13 C14 H25 108.0(13) . . ?
H24 C14 H25 107.7(17) . . ?
C13 C14 H26 112.1(11) . . ?
H24 C14 H26 109.1(17) . . ?
H25 C14 H26 108.8(18) . . ?
C16 C15 N11 112.12(14) . . ?
C16 C15 H11 112.6(11) . . ?
N11 C15 H11 106.3(12) . . ?
C16 C15 H12 109.9(12) . . ?
N11 C15 H12 104.8(12) . . ?
H11 C15 H12 110.9(16) . . ?
C15 C16 H13 111.9(11) . . ?
C15 C16 H14 108.8(12) . . ?
H13 C16 H14 107.9(16) . . ?
C15 C16 H15 113.2(12) . . ?
H13 C16 H15 107.2(16) . . ?
H14 C16 H15 107.6(17) . . ?

_refine_diff_density_max         0.325
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.064

####################################################################### 
# 
# 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_JL031_JL_K3Py3thfH2O
_database_code_depnum_ccdc_archive 'CCDC 1548899'
_audit_update_record             
;
2017-05-09 deposited with the CCDC.
2017-06-26 downloaded from the CCDC.
;


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

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H52.17 B6 F4 K6 N20 O8.01'
_chemical_formula_weight         1460.91

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   41.3012(11)
_cell_length_b                   8.4531(2)
_cell_length_c                   46.0735(11)
_cell_angle_alpha                90
_cell_angle_beta                 113.7870(10)
_cell_angle_gamma                90
_cell_volume                     14718.9(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9798
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      26.80
_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).
;

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_F_000             5986
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_exptl_absorpt_coefficient_mu    0.425
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6573
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            44601
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         1.120
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_full        26.000
_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             15069
_reflns_number_gt                11477
_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. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0718P)²+17.1488P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_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         15069
_refine_ls_number_parameters     944
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0457
_refine_ls_wR_factor_ref         0.1377
_refine_ls_wR_factor_gt          0.1250
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.007
_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 0.28895(2) -0.00198(4) 0.19554(2) 0.01193(10) Uani 1 1 d . . . . .
C1 C 0.40226(5) 0.0228(2) 0.37615(5) 0.0106(4) Uani 1 1 d . . . . .
B1 B 0.44118(6) 0.0304(3) 0.37554(5) 0.0137(4) Uani 1 1 d . . . . .
N1 N 0.39986(4) 0.01588(18) 0.40437(4) 0.0106(3) Uani 1 1 d . . . . .
F1 F 0.30572(3) 0.00288(14) 0.37967(3) 0.0174(3) Uani 1 1 d . . . . .
O1 O 0.46716(4) 0.77997(19) 0.27207(4) 0.0314(4) Uani 1 1 d . . . . .
K2 K 0.28897(2) 0.50889(4) -0.05457(2) 0.01187(10) Uani 1 1 d . . . . .
C2 C 0.37165(5) 0.0203(2) 0.34835(4) 0.0107(4) Uani 1 1 d . . . . .
B2 B 0.36580(6) -0.0003(2) 0.43997(5) 0.0106(4) Uani 1 1 d . . . . .
N2 N 0.49003(5) 0.0619(2) 0.43669(4) 0.0252(4) Uani 1 1 d . . . . .
F2 F 0.37559(3) 0.02384(14) 0.32054(3) 0.0162(3) Uani 1 1 d . . . . .
O2 O 0.52919(4) -0.25457(18) 0.47810(4) 0.0292(4) Uani 1 1 d . . . . .
K3 K 0.43870(2) 0.53626(5) 0.30025(2) 0.01710(11) Uani 1 1 d . . . . .
O6 O 0.24844(2) 0.23278(4) 0.37543(2) 0.024(6) Uani 0.089(6) 1 d D . P . .
H201 H 0.23376(2) 0.14905(4) 0.36934(4) 0.029 Uiso 0.089(6) 1 d D U P . .
H200 H 0.27106(2) 0.22249(9) 0.38942(2) 0.029 Uiso 0.089(6) 1 d D U P . .
B3 B 0.30036(6) 0.0158(2) 0.31707(5) 0.0117(4) Uani 1 1 d . . . . .
C3X C 0.33789(5) 0.0141(2) 0.34761(5) 0.0104(4) Uani 1 1 d . . . . .
N3 N 0.44586(5) 0.2834(3) 0.34029(5) 0.0330(5) Uani 1 1 d . . . . .
F3 F 0.30535(3) 0.51082(13) 0.12982(3) 0.0165(3) Uani 1 1 d . . . . .
K4 K 0.24926(2) 0.27861(5) 0.12526(2) 0.01769(11) Uani 1 1 d . . . . .
C41 C 0.33802(5) 0.0082(2) 0.37772(5) 0.0096(4) Uani 1 1 d . . . . .
B4 B 0.44067(6) 0.4833(2) 0.12540(5) 0.0116(4) Uani 1 1 d . . . . .
N4 N 0.45093(6) -0.2397(3) 0.34737(5) 0.0375(5) Uani 1 1 d . . . . .
O3 O 0.35585(5) 0.6136(3) 0.39158(5) 0.0307(5) Uani 0.8 1 d . . P A 3
C3 C 0.36027(10) 0.5838(4) 0.36309(8) 0.0309(7) Uani 0.8 1 d . U P A 3
H3A H 0.3722 0.6739 0.3578 0.037 Uiso 0.8 1 calc R U P A 3
H3B H 0.3371 0.5657 0.3452 0.037 Uiso 0.8 1 calc R U P A 3
C4 C 0.38238(12) 0.4405(5) 0.36965(9) 0.0496(10) Uani 0.8 1 d . U P A 3
H4A H 0.3953 0.4342 0.3556 0.060 Uiso 0.8 1 calc R U P A 3
H4B H 0.3680 0.3437 0.3669 0.060 Uiso 0.8 1 calc R U P A 3
C5 C 0.40763(11) 0.4630(5) 0.40394(10) 0.0499(10) Uani 0.8 1 d . U P A 3
H5A H 0.4301 0.5112 0.4054 0.060 Uiso 0.8 1 calc R U P A 3
H5B H 0.4129 0.3607 0.4154 0.060 Uiso 0.8 1 calc R U P A 3
C6 C 0.38815(10) 0.5728(4) 0.41738(9) 0.0308(8) Uani 0.8 1 d . U P A 3
H6A H 0.3833 0.5190 0.4343 0.037 Uiso 0.8 1 calc R U P A 3
H6B H 0.4024 0.6688 0.4264 0.037 Uiso 0.8 1 calc R U P A 3
O3B O 0.3549(3) 0.4293(16) 0.3893(3) 0.022(3) Uani 0.12 1 d . U P B 4
C3B C 0.3554(3) 0.4770(19) 0.3600(3) 0.028(3) Uani 0.2 1 d . . P B 4
H3B1 H 0.3337 0.5376 0.3476 0.034 Uiso 0.2 1 calc R U P B 4
H3B2 H 0.3560 0.3827 0.3475 0.034 Uiso 0.2 1 calc R U P B 4
C4B C 0.3886(4) 0.479(3) 0.4146(4) 0.052(5) Uani 0.2 1 d . . P B 4
H4AB H 0.3841 0.5538 0.4290 0.063 Uiso 0.2 1 calc R U P B 4
H4BB H 0.4012 0.3857 0.4271 0.063 Uiso 0.2 1 calc R U P B 4
C5B C 0.3868(4) 0.576(2) 0.3659(3) 0.052(5) Uani 0.2 1 d . . P B 4
H5AB H 0.3799 0.6885 0.3613 0.063 Uiso 0.2 1 calc R U P B 4
H5BB H 0.3990 0.5418 0.3524 0.063 Uiso 0.2 1 calc R U P B 4
C6B C 0.4100(3) 0.5547(16) 0.3999(3) 0.034(3) Uani 0.2 1 d . . P B 4
H6AB H 0.4306 0.4874 0.4023 0.040 Uiso 0.2 1 calc R U P B 4
H6BB H 0.4189 0.6583 0.4100 0.040 Uiso 0.2 1 calc R U P B 4
O4 O 0.64435(4) 0.1144(2) 0.36068(4) 0.0311(4) Uani 1 1 d . . . . .
F4 F 0.37500(3) 0.49774(13) 0.07041(3) 0.0160(3) Uani 1 1 d . . . . .
K5 K 0.43873(2) -0.02114(5) 0.04993(2) 0.01618(11) Uani 1 1 d . . . . .
C5X C 0.36792(5) 0.0078(2) 0.40572(5) 0.0105(4) Uani 1 1 d . . . . .
B5 B 0.36549(6) 0.5059(2) 0.19001(5) 0.0102(4) Uani 1 1 d . . . . .
N5 N 0.30260(5) 0.0317(2) 0.25869(4) 0.0216(4) Uani 1 1 d . . . . .
O5 O 0.36764(5) -0.00816(19) 0.02851(5) 0.0377(5) Uani 1 1 d . . . . .
K6 K 0.5000 0.0000 0.5000 0.02118(16) Uani 1 2 d S . P . .
B6 B 0.29993(6) 0.5124(2) 0.06707(5) 0.0122(4) Uani 1 1 d . . . . .
C61 C 0.46992(5) 0.0478(2) 0.41094(5) 0.0173(4) Uani 1 1 d . . . . .
N6 N 0.26521(5) -0.2585(2) 0.31756(4) 0.0208(4) Uani 1 1 d . . . . .
K7 K 0.5000 0.54178(8) 0.2500 0.02018(15) Uani 1 2 d S T P . .
C7X C 0.44451(5) 0.1777(3) 0.35525(5) 0.0197(4) Uani 1 1 d . . . . .
N7 N 0.26492(5) 0.2740(2) 0.32518(5) 0.0302(5) Uani 1 1 d . . . . .
C7 C 0.44154(14) 1.0249(4) 0.27188(11) 0.0840(14) Uani 1 1 d . . . . .
H7A H 0.4311 1.1157 0.2576 0.101 Uiso 1 1 calc R U . . .
H7B H 0.4300 1.0155 0.2869 0.101 Uiso 1 1 calc R U . . .
H9 H 0.2849(11) -0.059(5) 0.1224(10) 0.088(14) Uiso 1 1 d . . . . .
C9 C 0.40337(5) -0.0469(2) 0.46689(4) 0.0133(4) Uani 1 1 d . . . . .
N9 N 0.34569(5) 0.2893(2) 0.45386(5) 0.0271(4) Uani 1 1 d . . . . .
H8 H 0.3103(9) 0.033(3) 0.1385(7) 0.033(8) Uiso 1 1 d . . . . .
C8 C 0.44808(5) -0.1274(3) 0.35972(5) 0.0212(4) Uani 1 1 d . . . . .
N8 N 0.31801(5) -0.2256(2) 0.43884(4) 0.0279(4) Uani 1 1 d . . . . .
H10 H 0.2171(9) -0.061(4) 0.1247(8) 0.054(12) Uiso 1 1 d . . . . .
N10 N 0.42983(5) -0.0821(2) 0.48665(4) 0.0200(4) Uani 1 1 d . . . . .
C10 C 0.35398(5) 0.1673(2) 0.44844(4) 0.0162(4) Uani 1 1 d . . . . .
N12 N 0.43009(5) 0.4383(2) 0.23717(4) 0.0219(4) Uani 1 1 d . . . . .
C12 C 0.30286(5) 0.0270(2) 0.28356(5) 0.0144(4) Uani 1 1 d . . . . .
N13 N 0.34520(5) 0.7987(2) 0.20200(4) 0.0245(4) Uani 1 1 d . . . . .
C13 C 0.27925(5) -0.1438(2) 0.31682(4) 0.0145(4) Uani 1 1 d . . . . .
N14 N 0.31687(5) 0.2860(2) 0.18985(4) 0.0265(4) Uani 1 1 d . . . . .
C14 C 0.27859(5) 0.1649(2) 0.32072(4) 0.0170(4) Uani 1 1 d . . . . .
N15 N 0.48956(5) 0.4686(2) 0.18678(5) 0.0260(4) Uani 1 1 d . . . . .
C15 C 0.36749(5) 0.5040(2) 0.15569(5) 0.0096(4) Uani 1 1 d . . . . .
N16 N 0.45121(5) 0.7416(2) 0.09443(5) 0.0296(4) Uani 1 1 d . . . . .
C16 C 0.33748(5) 0.5065(2) 0.12771(5) 0.0100(4) Uani 1 1 d . . . . .
N17 N 0.44389(5) 0.2168(2) 0.09270(5) 0.0313(5) Uani 1 1 d . . . . .
C17 C 0.33740(5) 0.5051(2) 0.09758(5) 0.0098(4) Uani 1 1 d . . . . .
N18 N 0.30173(5) 0.5169(2) 0.00855(4) 0.0249(4) Uani 1 1 d . . . . .
C18 C 0.37118(5) 0.4996(2) 0.09838(5) 0.0102(4) Uani 1 1 d . . . . .
N19 N 0.26229(5) 0.2469(2) 0.06825(4) 0.0200(4) Uani 1 1 d . . . . .
C19 C 0.40183(5) 0.4950(2) 0.12597(5) 0.0102(4) Uani 1 1 d . . . . .
N20 N 0.26776(5) 0.7833(2) 0.07479(5) 0.0314(5) Uani 1 1 d . . . . .
C20 C 0.40310(5) 0.4656(2) 0.21720(5) 0.0143(4) Uani 1 1 d . . . . .
C21 C 0.35347(5) 0.6756(2) 0.19709(4) 0.0155(4) Uani 1 1 d . . . . .
C35 C 0.34923(6) 0.1399(3) 0.02471(6) 0.0291(5) Uani 1 1 d . . . . .
H02E H 0.3531 0.2062 0.0087 0.035 Uiso 1 1 calc R U . . .
H02F H 0.3579 0.1983 0.0451 0.035 Uiso 1 1 calc R U . . .
C36 C 0.31030(7) 0.1012(3) 0.01397(6) 0.0338(6) Uani 1 1 d . . . . .
H02M H 0.2957 0.1688 -0.0041 0.041 Uiso 1 1 calc R U . . .
H02N H 0.3025 0.1159 0.0315 0.041 Uiso 1 1 calc R U . . .
C37 C 0.30775(6) -0.0714(3) 0.00413(6) 0.0303(5) Uani 1 1 d . . . . .
H02G H 0.2885 -0.1262 0.0078 0.036 Uiso 1 1 calc R U . . .
H02H H 0.3037 -0.0821 -0.0185 0.036 Uiso 1 1 calc R U . . .
C38 C 0.34375(6) -0.1349(3) 0.02578(6) 0.0258(5) Uani 1 1 d . . . . .
H02A H 0.3442 -0.1632 0.0468 0.031 Uiso 1 1 calc R U . . .
H02B H 0.3499 -0.2296 0.0164 0.031 Uiso 1 1 calc R U . . .
C39 C 0.49347(8) 0.8795(3) 0.29516(7) 0.0468(7) Uani 1 1 d . . . . .
H02Z H 0.5163 0.8711 0.2930 0.056 Uiso 1 1 calc R U . . .
H010 H 0.4971 0.8473 0.3169 0.056 Uiso 1 1 calc R U . . .
C40 C 0.47986(12) 1.0443(4) 0.28883(11) 0.0803(13) Uani 1 1 d . . . . .
H098 H 0.4857 1.1032 0.3089 0.096 Uiso 1 1 calc R U . . .
H099 H 0.4899 1.1013 0.2756 0.096 Uiso 1 1 calc R U . . .
C42 C 0.43745(9) 0.8749(4) 0.25328(7) 0.0508(8) Uani 1 1 d . . . . .
H121 H 0.4150 0.8210 0.2502 0.061 Uiso 1 1 calc R U . . .
H122 H 0.4377 0.8971 0.2323 0.061 Uiso 1 1 calc R U . . .
C43 C 0.50315(7) -0.3511(3) 0.45432(6) 0.0379(6) Uani 1 1 d . . . . .
H02S H 0.4991 -0.3126 0.4328 0.045 Uiso 1 1 calc R U . . .
H02T H 0.4804 -0.3473 0.4568 0.045 Uiso 1 1 calc R U . . .
C44 C 0.51733(11) -0.5174(4) 0.45893(10) 0.0609(10) Uani 1 1 d . . . . .
H013 H 0.5060 -0.5826 0.4701 0.073 Uiso 1 1 calc R U . . .
H014 H 0.5130 -0.5674 0.4383 0.073 Uiso 1 1 calc R U . . .
C45 C 0.55544(12) -0.5009(4) 0.47818(10) 0.0684(11) Uani 1 1 d . . . . .
H011 H 0.5687 -0.4844 0.4647 0.082 Uiso 1 1 calc R U . . .
H012 H 0.5650 -0.5950 0.4917 0.082 Uiso 1 1 calc R U . . .
C46 C 0.55712(8) -0.3560(3) 0.49794(7) 0.0492(7) Uani 1 1 d . . . . .
H02W H 0.5536 -0.3854 0.5173 0.059 Uiso 1 1 calc R U . . .
H02X H 0.5803 -0.3028 0.5043 0.059 Uiso 1 1 calc R U . . .
O47 O 0.29055(5) 0.0153(2) 0.13582(4) 0.0225(4) Uani 1 1 d . . . . .
O48 O 0.21026(6) 0.0055(2) 0.11446(4) 0.0273(4) Uani 1 1 d . . . . .
O49 O 0.36737(4) 0.53720(19) 0.27949(5) 0.0350(4) Uani 1 1 d . . . . .
C50 C 0.34440(6) 0.6699(2) 0.27538(5) 0.0229(5) Uani 1 1 d . . . . .
H01A H 0.3513 0.7588 0.2651 0.027 Uiso 1 1 calc R U . . .
H01B H 0.3451 0.7062 0.2961 0.027 Uiso 1 1 calc R U . . .
C51 C 0.30806(6) 0.6105(3) 0.25452(6) 0.0255(5) Uani 1 1 d . . . . .
H02C H 0.3041 0.6134 0.2319 0.031 Uiso 1 1 calc R U . . .
H02D H 0.2894 0.6730 0.2576 0.031 Uiso 1 1 calc R U . . .
C52 C 0.30902(7) 0.4411(3) 0.26611(7) 0.0344(6) Uani 1 1 d . . . . .
H02O H 0.3019 0.4363 0.2842 0.041 Uiso 1 1 calc R U . . .
H02P H 0.2932 0.3719 0.2489 0.041 Uiso 1 1 calc R U . . .
C53 C 0.34732(6) 0.3936(3) 0.27623(6) 0.0282(5) Uani 1 1 d . . . . .
H01C H 0.3558 0.3361 0.2967 0.034 Uiso 1 1 calc R U . . .
H01D H 0.3500 0.3237 0.2601 0.034 Uiso 1 1 calc R U . . .
C22 C 0.33753(5) 0.3776(2) 0.19088(4) 0.0160(4) Uani 1 1 d . . . . .
C24 C 0.27720(5) 0.3591(2) 0.06744(4) 0.0143(4) Uani 1 1 d . . . . .
C23 C 0.27991(5) 0.6693(2) 0.07048(5) 0.0177(4) Uani 1 1 d . . . . .
C26 C 0.46949(6) 0.4747(2) 0.16086(5) 0.0171(4) Uani 1 1 d . . . . .
C25 C 0.30221(6) 0.5160(2) 0.03348(5) 0.0154(4) Uani 1 1 d . . . . .
C27 C 0.44781(5) 0.6335(2) 0.10782(5) 0.0176(4) Uani 1 1 d . . . . .
C28 C 0.44342(5) 0.3283(2) 0.10671(5) 0.0176(4) Uani 1 1 d . . . . .
C29 C 0.61208(7) 0.0734(3) 0.33411(6) 0.0319(5) Uani 1 1 d . . . . .
H02K H 0.6174 0.0218 0.3173 0.038 Uiso 1 1 calc R U . . .
H02L H 0.5978 0.1693 0.3252 0.038 Uiso 1 1 calc R U . . .
C30 C 0.59229(8) -0.0388(4) 0.34661(8) 0.0518(8) Uani 1 1 d . . . . .
H02U H 0.5706 0.0116 0.3465 0.062 Uiso 1 1 calc R U . . .
H02V H 0.5856 -0.1364 0.3336 0.062 Uiso 1 1 calc R U . . .
C31 C 0.61792(8) -0.0754(3) 0.38008(7) 0.0416(7) Uani 1 1 d . . . . .
H02Q H 0.6054 -0.0909 0.3942 0.050 Uiso 1 1 calc R U . . .
H02R H 0.6320 -0.1712 0.3808 0.050 Uiso 1 1 calc R U . . .
C32 C 0.64058(7) 0.0678(3) 0.38908(6) 0.0300(5) Uani 1 1 d . . . . .
H02I H 0.6292 0.1528 0.3964 0.036 Uiso 1 1 calc R U . . .
H02J H 0.6639 0.0435 0.4062 0.036 Uiso 1 1 calc R U . . .
N11 N 0.39950(4) 0.49857(17) 0.15431(4) 0.0104(3) Uani 1 1 d . . . . .
C11 C 0.33808(5) -0.1307(2) 0.43995(4) 0.0170(4) Uani 1 1 d . . . . .
H11 H 0.1902(11) 0.020(4) 0.1132(9) 0.069(13) Uiso 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 N5 2.7461(18) . ?
K1 N14 2.7510(18) . ?
K1 N7 2.7812(19) 4_545 ?
K1 O47 2.7829(17) . ?
K1 N13 2.7867(18) 1_545 ?
K1 N6 2.9179(18) 4 ?
K1 K4 3.8102(6) . ?
C1 N1 1.345(2) . ?
C1 C2 1.390(3) . ?
C1 B1 1.620(3) . ?
B1 C61 1.590(3) . ?
B1 C7X 1.596(3) . ?
B1 C8 1.600(3) . ?
N1 C5X 1.347(2) . ?
F1 C41 1.373(2) . ?
F1 K4 2.8957(12) 4_545 ?
O1 C42 1.429(3) . ?
O1 C39 1.445(3) . ?
O1 K7 2.8356(17) . ?
O1 K3 2.9226(17) . ?
K2 N18 2.7395(19) . ?
K2 N8 2.7491(19) 6 ?
K2 N20 2.7718(19) 7_565 ?
K2 O48 2.7747(18) 7 ?
K2 N9 2.7954(19) 6_565 ?
K2 N19 2.9119(17) 7 ?
K2 K4 3.8546(6) 7 ?
C2 F2 1.355(2) . ?
C2 C3X 1.382(3) . ?
B2 C11 1.589(3) . ?
B2 C9 1.596(3) . ?
B2 C10 1.598(3) . ?
B2 C5X 1.617(3) . ?
N2 C61 1.148(3) . ?
N2 K6 2.8254(18) . ?
N2 K5 2.8401(19) 2_655 ?
O2 C46 1.432(3) . ?
O2 C43 1.440(3) . ?
O2 K6 2.8433(16) . ?
O2 K5 2.9489(16) 2_655 ?
K3 O49 2.7058(17) . ?
K3 N3 2.760(2) . ?
K3 N4 2.769(2) 1_565 ?
K3 N15 2.8343(19) 2_655 ?
K3 N12 2.9027(18) . ?
K3 C26 3.518(2) 2_655 ?
K3 K7 4.0620(4) . ?
O6 H201 0.90000(3) . ?
O6 H200 0.900001(18) . ?
B3 C12 1.591(3) . ?
B3 C14 1.595(3) . ?
B3 C13 1.604(3) . ?
B3 C3X 1.620(3) . ?
C3X C41 1.386(3) . ?
N3 C7X 1.144(3) . ?
F3 C16 1.369(2) . ?
F3 K4 2.9787(12) . ?
K4 O47 2.7255(17) . ?
K4 O48 2.7432(18) . ?
K4 F1 2.8959(12) 4 ?
K4 N19 2.8984(17) . ?
K4 N6 2.9437(17) 4 ?
K4 N8 3.134(2) 4 ?
K4 N14 3.155(2) . ?
K4 C24 3.3723(19) . ?
K4 C13 3.3869(18) 4 ?
K4 K2 3.8544(6) 7 ?
C41 C5X 1.380(3) . ?
B4 C26 1.588(3) . ?
B4 C27 1.596(3) . ?
B4 C28 1.597(3) . ?
B4 C19 1.618(3) . ?
N4 C8 1.137(3) . ?
N4 K3 2.769(2) 1_545 ?
O3 C3 1.419(3) . ?
O3 C6 1.425(4) . ?
C3 C4 1.473(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.513(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.515(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
O3B C3B 1.415(16) . ?
O3B C4B 1.47(2) . ?
C3B C5B 1.474(18) . ?
C3B H3B1 0.9900 . ?
C3B H3B2 0.9900 . ?
C4B C6B 1.46(2) . ?
C4B H4AB 0.9900 . ?
C4B H4BB 0.9900 . ?
C5B C6B 1.482(19) . ?
C5B H5AB 0.9900 . ?
C5B H5BB 0.9900 . ?
C6B H6AB 0.9900 . ?
C6B H6BB 0.9900 . ?
O4 C32 1.434(3) . ?
O4 C29 1.442(3) . ?
F4 C18 1.360(2) . ?
K5 O5 2.6960(18) . ?
K5 N17 2.7628(19) . ?
K5 N16 2.764(2) 1_545 ?
K5 N2 2.8401(19) 2_655 ?
K5 N10 2.9212(17) 6 ?
K5 O2 2.9491(16) 2_655 ?
K5 C61 3.513(2) 2_655 ?
K5 K6 4.0527(4) 2_655 ?
B5 C20 1.590(3) . ?
B5 C21 1.594(3) . ?
B5 C22 1.596(3) . ?
B5 C15 1.617(3) . ?
N5 C12 1.142(3) . ?
O5 C38 1.427(3) . ?
O5 C35 1.438(3) . ?
K6 N10 2.7965(18) . ?
K6 N10 2.7965(18) 5_656 ?
K6 N2 2.8254(18) 5_656 ?
K6 O2 2.8433(16) 5_656 ?
K6 K5 4.0525(4) 2_655 ?
K6 K5 4.0525(4) 6_556 ?
B6 C25 1.588(3) . ?
B6 C24 1.604(3) . ?
B6 C23 1.604(3) . ?
B6 C17 1.618(3) . ?
C61 K5 3.513(2) 2_655 ?
N6 C13 1.137(3) . ?
N6 K1 2.9179(18) 4_545 ?
N6 K4 2.9436(17) 4_545 ?
K7 N15 2.8353(19) 2_655 ?
K7 N15 2.8353(19) . ?
K7 O1 2.8357(17) 2_655 ?
K7 N12 2.8417(19) . ?
K7 N12 2.8418(19) 2_655 ?
K7 K3 4.0621(4) 2_655 ?
N7 C14 1.142(3) . ?
N7 K1 2.7812(19) 4 ?
C7 C40 1.465(6) . ?
C7 C42 1.501(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C9 N10 1.144(3) . ?
N9 C10 1.145(3) . ?
N9 K2 2.7955(19) 6_566 ?
N8 C11 1.139(3) . ?
N8 K2 2.7492(19) 6_556 ?
N8 K4 3.134(2) 4_545 ?
N10 K5 2.9211(17) 6_556 ?
N12 C20 1.147(3) . ?
N13 C21 1.146(3) . ?
N13 K1 2.7868(18) 1_565 ?
C13 K4 3.3869(18) 4_545 ?
N14 C22 1.139(3) . ?
N15 C26 1.148(3) . ?
N15 K3 2.8344(19) 2_655 ?
C15 N11 1.350(2) . ?
C15 C16 1.382(3) . ?
N16 C27 1.142(3) . ?
N16 K5 2.764(2) 1_565 ?
C16 C17 1.387(3) . ?
N17 C28 1.148(3) . ?
C17 C18 1.382(3) . ?
N18 C25 1.141(3) . ?
C18 C19 1.386(3) . ?
N19 C24 1.140(3) . ?
N19 K2 2.9119(17) 7 ?
C19 N11 1.348(2) . ?
N20 C23 1.140(3) . ?
N20 K2 2.7718(19) 7_565 ?
C35 C36 1.515(3) . ?
C35 H02E 0.9900 . ?
C35 H02F 0.9900 . ?
C36 C37 1.519(3) . ?
C36 H02M 0.9900 . ?
C36 H02N 0.9900 . ?
C37 C38 1.516(3) . ?
C37 H02G 0.9900 . ?
C37 H02H 0.9900 . ?
C38 H02A 0.9900 . ?
C38 H02B 0.9900 . ?
C39 C40 1.486(5) . ?
C39 H02Z 0.9900 . ?
C39 H010 0.9900 . ?
C40 H098 0.9900 . ?
C40 H099 0.9900 . ?
C42 H121 0.9900 . ?
C42 H122 0.9900 . ?
C43 C44 1.505(4) . ?
C43 H02S 0.9900 . ?
C43 H02T 0.9900 . ?
C44 C45 1.469(6) . ?
C44 H013 0.9900 . ?
C44 H014 0.9900 . ?
C45 C46 1.510(4) . ?
C45 H011 0.9900 . ?
C45 H012 0.9900 . ?
C46 H02W 0.9900 . ?
C46 H02X 0.9900 . ?
O47 H9 0.84(4) . ?
O47 H8 0.79(3) . ?
O48 K2 2.7747(18) 7 ?
O48 H10 0.72(4) . ?
O48 H11 0.82(4) . ?
O49 C50 1.432(3) . ?
O49 C53 1.443(3) . ?
C50 C51 1.505(3) . ?
C50 H01A 0.9900 . ?
C50 H01B 0.9900 . ?
C51 C52 1.523(3) . ?
C51 H02C 0.9900 . ?
C51 H02D 0.9900 . ?
C52 C53 1.512(3) . ?
C52 H02O 0.9900 . ?
C52 H02P 0.9900 . ?
C53 H01C 0.9900 . ?
C53 H01D 0.9900 . ?
C26 K3 3.518(2) 2_655 ?
C29 C30 1.509(4) . ?
C29 H02K 0.9900 . ?
C29 H02L 0.9900 . ?
C30 C31 1.509(4) . ?
C30 H02U 0.9900 . ?
C30 H02V 0.9900 . ?
C31 C32 1.484(4) . ?
C31 H02Q 0.9900 . ?
C31 H02R 0.9900 . ?
C32 H02I 0.9900 . ?
C32 H02J 0.9900 . ?

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
N5 K1 N14 95.41(6) . . ?
N5 K1 N7 103.20(6) . 4_545 ?
N14 K1 N7 151.39(6) . 4_545 ?
N5 K1 O47 164.92(6) . . ?
N14 K1 O47 71.41(5) . . ?
N7 K1 O47 91.78(6) 4_545 . ?
N5 K1 N13 98.26(6) . 1_545 ?
N14 K1 N13 100.46(6) . 1_545 ?
N7 K1 N13 98.16(6) 4_545 1_545 ?
O47 K1 N13 77.65(5) . 1_545 ?
N5 K1 N6 87.64(5) . 4 ?
N14 K1 N6 70.86(5) . 4 ?
N7 K1 N6 88.22(6) 4_545 4 ?
O47 K1 N6 94.60(5) . 4 ?
N13 K1 N6 170.04(5) 1_545 4 ?
N5 K1 K4 132.07(4) . . ?
N14 K1 K4 54.65(4) . . ?
N7 K1 K4 96.99(4) 4_545 . ?
O47 K1 K4 45.61(3) . . ?
N13 K1 K4 121.43(4) 1_545 . ?
N6 K1 K4 49.75(3) 4 . ?
N1 C1 C2 119.72(17) . . ?
N1 C1 B1 118.63(17) . . ?
C2 C1 B1 121.64(17) . . ?
C61 B1 C7X 108.88(17) . . ?
C61 B1 C8 110.35(17) . . ?
C7X B1 C8 108.09(17) . . ?
C61 B1 C1 108.73(16) . . ?
C7X B1 C1 111.19(16) . . ?
C8 B1 C1 109.59(16) . . ?
C1 N1 C5X 120.15(17) . . ?
C41 F1 K4 140.18(10) . 4_545 ?
C42 O1 C39 109.0(2) . . ?
C42 O1 K7 126.85(15) . . ?
C39 O1 K7 110.55(15) . . ?
C42 O1 K3 105.31(16) . . ?
C39 O1 K3 113.65(15) . . ?
K7 O1 K3 89.72(5) . . ?
N18 K2 N8 103.47(6) . 6 ?
N18 K2 N20 96.65(6) . 7_565 ?
N8 K2 N20 149.56(6) 6 7_565 ?
N18 K2 O48 169.21(7) . 7 ?
N8 K2 O48 70.83(6) 6 7 ?
N20 K2 O48 92.33(7) 7_565 7 ?
N18 K2 N9 92.63(6) . 6_565 ?
N8 K2 N9 99.71(6) 6 6_565 ?
N20 K2 N9 101.97(6) 7_565 6_565 ?
O48 K2 N9 79.63(5) 7 6_565 ?
N18 K2 N19 93.43(5) . 7 ?
N8 K2 N19 68.95(5) 6 7 ?
N20 K2 N19 87.45(6) 7_565 7 ?
O48 K2 N19 92.93(5) 7 7 ?
N9 K2 N19 168.14(5) 6_565 7 ?
N18 K2 K4 138.62(4) . 7 ?
N8 K2 K4 53.55(4) 6 7 ?
N20 K2 K4 96.48(4) 7_565 7 ?
O48 K2 K4 45.35(4) 7 7 ?
N9 K2 K4 122.48(4) 6_565 7 ?
N19 K2 K4 48.29(3) 7 7 ?
F2 C2 C3X 118.83(17) . . ?
F2 C2 C1 117.34(17) . . ?
C3X C2 C1 123.83(17) . . ?
C11 B2 C9 107.68(16) . . ?
C11 B2 C10 108.92(16) . . ?
C9 B2 C10 109.02(16) . . ?
C11 B2 C5X 110.59(16) . . ?
C9 B2 C5X 110.52(16) . . ?
C10 B2 C5X 110.05(15) . . ?
C61 N2 K6 142.32(16) . . ?
C61 N2 K5 116.96(15) . 2_655 ?
K6 N2 K5 91.33(5) . 2_655 ?
C46 O2 C43 108.0(2) . . ?
C46 O2 K6 125.05(15) . . ?
C43 O2 K6 113.92(14) . . ?
C46 O2 K5 106.97(16) . 2_655 ?
C43 O2 K5 112.08(14) . 2_655 ?
K6 O2 K5 88.78(4) . 2_655 ?
O49 K3 N3 92.66(6) . . ?
O49 K3 N4 95.94(6) . 1_565 ?
N3 K3 N4 93.96(7) . 1_565 ?
O49 K3 N15 166.31(6) . 2_655 ?
N3 K3 N15 83.21(6) . 2_655 ?
N4 K3 N15 97.36(6) 1_565 2_655 ?
O49 K3 N12 88.32(6) . . ?
N3 K3 N12 112.65(6) . . ?
N4 K3 N12 152.86(6) 1_565 . ?
N15 K3 N12 81.32(5) 2_655 . ?
O49 K3 O1 114.61(5) . . ?
N3 K3 O1 152.73(5) . . ?
N4 K3 O1 83.53(6) 1_565 . ?
N15 K3 O1 70.27(5) 2_655 . ?
N12 K3 O1 70.43(5) . . ?
O49 K3 C26 167.58(5) . 2_655 ?
N3 K3 C26 75.06(5) . 2_655 ?
N4 K3 C26 83.31(6) 1_565 2_655 ?
N15 K3 C26 16.79(5) 2_655 2_655 ?
N12 K3 C26 98.02(5) . 2_655 ?
O1 K3 C26 77.68(5) . 2_655 ?
O49 K3 K7 129.68(4) . . ?
N3 K3 K7 117.80(5) . . ?
N4 K3 K7 118.71(5) 1_565 . ?
N15 K3 K7 44.25(4) 2_655 . ?
N12 K3 K7 44.39(4) . . ?
O1 K3 K7 44.27(3) . . ?
C26 K3 K7 60.04(3) 2_655 . ?
H201 O6 H200 121.436(3) . . ?
C12 B3 C14 108.38(16) . . ?
C12 B3 C13 106.90(16) . . ?
C14 B3 C13 109.71(17) . . ?
C12 B3 C3X 115.46(17) . . ?
C14 B3 C3X 107.35(16) . . ?
C13 B3 C3X 108.98(16) . . ?
C2 C3X C41 112.34(18) . . ?
C2 C3X B3 128.56(17) . . ?
C41 C3X B3 119.09(17) . . ?
C7X N3 K3 171.80(18) . . ?
C16 F3 K4 136.52(10) . . ?
O47 K4 O48 67.95(7) . . ?
O47 K4 F1 164.35(5) . 4 ?
O48 K4 F1 98.76(5) . 4 ?
O47 K4 N19 75.80(5) . . ?
O48 K4 N19 93.89(5) . . ?
F1 K4 N19 114.58(4) 4 . ?
O47 K4 N6 95.25(5) . 4 ?
O48 K4 N6 75.90(5) . 4 ?
F1 K4 N6 72.79(4) 4 4 ?
N19 K4 N6 168.53(6) . 4 ?
O47 K4 F3 96.46(5) . . ?
O48 K4 F3 161.89(5) . . ?
F1 K4 F3 97.88(4) 4 . ?
N19 K4 F3 72.62(4) . . ?
N6 K4 F3 116.11(4) 4 . ?
O47 K4 N8 114.33(5) . 4 ?
O48 K4 N8 65.61(6) . 4 ?
F1 K4 N8 64.19(4) 4 4 ?
N19 K4 N8 64.10(5) . 4 ?
N6 K4 N8 114.79(5) 4 4 ?
F3 K4 N8 116.27(4) . 4 ?
O47 K4 N14 66.15(5) . . ?
O48 K4 N14 114.79(6) . . ?
F1 K4 N14 115.38(4) 4 . ?
N19 K4 N14 116.06(5) . . ?
N6 K4 N14 65.16(5) 4 . ?
F3 K4 N14 63.46(4) . . ?
N8 K4 N14 179.51(6) 4 . ?
O47 K4 C24 85.23(5) . . ?
O48 K4 C24 112.93(5) . . ?
F1 K4 C24 108.26(4) 4 . ?
N19 K4 C24 19.09(5) . . ?
N6 K4 C24 170.46(5) 4 . ?
F3 K4 C24 54.44(4) . . ?
N8 K4 C24 73.36(5) 4 . ?
N14 K4 C24 106.64(5) . . ?
O47 K4 C13 114.13(5) . 4 ?
O48 K4 C13 86.60(5) . 4 ?
F1 K4 C13 54.85(4) 4 4 ?
N19 K4 C13 169.27(5) . 4 ?
N6 K4 C13 19.09(5) 4 4 ?
F3 K4 C13 108.94(4) . 4 ?
N8 K4 C13 106.67(5) 4 4 ?
N14 K4 C13 73.12(5) . 4 ?
C24 K4 C13 157.19(5) . 4 ?
O47 K4 K1 46.86(4) . . ?
O48 K4 K1 69.52(4) . . ?
F1 K4 K1 121.95(3) 4 . ?
N19 K4 K1 122.62(4) . . ?
N6 K4 K1 49.16(3) 4 . ?
F3 K4 K1 107.13(3) . . ?
N8 K4 K1 135.06(4) 4 . ?
N14 K4 K1 45.32(3) . . ?
C24 K4 K1 129.05(4) . . ?
C13 K4 K1 67.55(3) 4 . ?
O47 K4 K2 69.49(4) . 7 ?
O48 K4 K2 46.03(4) . 7 ?
F1 K4 K2 107.79(3) 4 7 ?
N19 K4 K2 48.59(3) . 7 ?
N6 K4 K2 121.81(4) 4 7 ?
F3 K4 K2 121.13(3) . 7 ?
N8 K4 K2 44.87(3) 4 7 ?
N14 K4 K2 135.60(4) . 7 ?
C24 K4 K2 67.29(3) . 7 ?
C13 K4 K2 129.32(4) 4 7 ?
K1 K4 K2 102.403(14) . 7 ?
F1 C41 C5X 117.76(16) . . ?
F1 C41 C3X 117.04(17) . . ?
C5X C41 C3X 125.20(18) . . ?
C26 B4 C27 110.07(17) . . ?
C26 B4 C28 109.29(16) . . ?
C27 B4 C28 108.14(16) . . ?
C26 B4 C19 108.82(16) . . ?
C27 B4 C19 110.30(16) . . ?
C28 B4 C19 110.21(16) . . ?
C8 N4 K3 160.1(2) . 1_545 ?
C3 O3 C6 107.6(2) . . ?
O3 C3 C4 104.9(3) . . ?
O3 C3 H3A 110.8 . . ?
C4 C3 H3A 110.8 . . ?
O3 C3 H3B 110.8 . . ?
C4 C3 H3B 110.8 . . ?
H3A C3 H3B 108.9 . . ?
C3 C4 C5 102.7(3) . . ?
C3 C4 H4A 111.2 . . ?
C5 C4 H4A 111.2 . . ?
C3 C4 H4B 111.2 . . ?
C5 C4 H4B 111.2 . . ?
H4A C4 H4B 109.1 . . ?
C4 C5 C6 104.4(3) . . ?
C4 C5 H5A 110.9 . . ?
C6 C5 H5A 110.9 . . ?
C4 C5 H5B 110.9 . . ?
C6 C5 H5B 110.9 . . ?
H5A C5 H5B 108.9 . . ?
O3 C6 C5 106.2(3) . . ?
O3 C6 H6A 110.5 . . ?
C5 C6 H6A 110.5 . . ?
O3 C6 H6B 110.5 . . ?
C5 C6 H6B 110.5 . . ?
H6A C6 H6B 108.7 . . ?
C3B O3B C4B 107.6(12) . . ?
O3B C3B C5B 109.5(11) . . ?
O3B C3B H3B1 109.8 . . ?
C5B C3B H3B1 109.8 . . ?
O3B C3B H3B2 109.8 . . ?
C5B C3B H3B2 109.8 . . ?
H3B1 C3B H3B2 108.2 . . ?
C6B C4B O3B 108.3(12) . . ?
C6B C4B H4AB 110.0 . . ?
O3B C4B H4AB 110.0 . . ?
C6B C4B H4BB 110.0 . . ?
O3B C4B H4BB 110.0 . . ?
H4AB C4B H4BB 108.4 . . ?
C3B C5B C6B 105.9(11) . . ?
C3B C5B H5AB 110.6 . . ?
C6B C5B H5AB 110.6 . . ?
C3B C5B H5BB 110.6 . . ?
C6B C5B H5BB 110.6 . . ?
H5AB C5B H5BB 108.7 . . ?
C4B C6B C5B 106.6(11) . . ?
C4B C6B H6AB 110.4 . . ?
C5B C6B H6AB 110.4 . . ?
C4B C6B H6BB 110.4 . . ?
C5B C6B H6BB 110.4 . . ?
H6AB C6B H6BB 108.6 . . ?
C32 O4 C29 107.78(18) . . ?
O5 K5 N17 89.48(6) . . ?
O5 K5 N16 98.68(6) . 1_545 ?
N17 K5 N16 93.53(7) . 1_545 ?
O5 K5 N2 161.67(6) . 2_655 ?
N17 K5 N2 83.69(6) . 2_655 ?
N16 K5 N2 98.70(6) 1_545 2_655 ?
O5 K5 N10 86.70(6) . 6 ?
N17 K5 N10 115.90(6) . 6 ?
N16 K5 N10 150.21(6) 1_545 6 ?
N2 K5 N10 81.08(5) 2_655 6 ?
O5 K5 O2 118.83(5) . 2_655 ?
N17 K5 O2 151.67(5) . 2_655 ?
N16 K5 O2 81.77(5) 1_545 2_655 ?
N2 K5 O2 69.59(5) 2_655 2_655 ?
N10 K5 O2 70.17(5) 6 2_655 ?
O5 K5 C61 165.20(5) . 2_655 ?
N17 K5 C61 75.83(5) . 2_655 ?
N16 K5 C61 84.21(5) 1_545 2_655 ?
N2 K5 C61 16.93(5) 2_655 2_655 ?
N10 K5 C61 98.01(5) 6 2_655 ?
O2 K5 C61 75.90(5) 2_655 2_655 ?
O5 K5 K6 128.87(5) . 2_655 ?
N17 K5 K6 119.10(4) . 2_655 ?
N16 K5 K6 118.72(4) 1_545 2_655 ?
N2 K5 K6 44.18(4) 2_655 2_655 ?
N10 K5 K6 43.63(3) 6 2_655 ?
O2 K5 K6 44.54(3) 2_655 2_655 ?
C61 K5 K6 59.78(3) 2_655 2_655 ?
N1 C5X C41 118.73(17) . . ?
N1 C5X B2 119.12(17) . . ?
C41 C5X B2 122.14(17) . . ?
C20 B5 C21 108.51(16) . . ?
C20 B5 C22 108.75(16) . . ?
C21 B5 C22 108.54(16) . . ?
C20 B5 C15 110.45(16) . . ?
C21 B5 C15 110.62(15) . . ?
C22 B5 C15 109.91(16) . . ?
C12 N5 K1 166.91(17) . . ?
C38 O5 C35 109.25(18) . . ?
C38 O5 K5 127.86(13) . . ?
C35 O5 K5 121.63(13) . . ?
N10 K6 N10 180.00(2) . 5_656 ?
N10 K6 N2 83.55(5) . 5_656 ?
N10 K6 N2 96.45(5) 5_656 5_656 ?
N10 K6 N2 96.45(5) . . ?
N10 K6 N2 83.55(5) 5_656 . ?
N2 K6 N2 180.0 5_656 . ?
N10 K6 O2 73.49(5) . 5_656 ?
N10 K6 O2 106.51(5) 5_656 5_656 ?
N2 K6 O2 71.32(5) 5_656 5_656 ?
N2 K6 O2 108.68(5) . 5_656 ?
N10 K6 O2 106.51(5) . . ?
N10 K6 O2 73.49(5) 5_656 . ?
N2 K6 O2 108.68(5) 5_656 . ?
N2 K6 O2 71.32(5) . . ?
O2 K6 O2 180.0 5_656 . ?
N10 K6 K5 133.88(3) . 2_655 ?
N10 K6 K5 46.12(4) 5_656 2_655 ?
N2 K6 K5 135.52(4) 5_656 2_655 ?
N2 K6 K5 44.48(4) . 2_655 ?
O2 K6 K5 133.32(3) 5_656 2_655 ?
O2 K6 K5 46.68(3) . 2_655 ?
N10 K6 K5 46.12(3) . 6_556 ?
N10 K6 K5 133.88(4) 5_656 6_556 ?
N2 K6 K5 44.48(4) 5_656 6_556 ?
N2 K6 K5 135.52(4) . 6_556 ?
O2 K6 K5 46.68(3) 5_656 6_556 ?
O2 K6 K5 133.32(3) . 6_556 ?
K5 K6 K5 180.0 2_655 6_556 ?
C25 B6 C24 106.91(16) . . ?
C25 B6 C23 108.36(16) . . ?
C24 B6 C23 109.87(17) . . ?
C25 B6 C17 115.81(17) . . ?
C24 B6 C17 108.59(16) . . ?
C23 B6 C17 107.24(16) . . ?
N2 C61 B1 178.3(2) . . ?
N2 C61 K5 46.11(12) . 2_655 ?
B1 C61 K5 135.56(12) . 2_655 ?
C13 N6 K1 162.30(16) . 4_545 ?
C13 N6 K4 103.06(14) . 4_545 ?
K1 N6 K4 81.08(4) 4_545 4_545 ?
N15 K7 N15 154.81(9) 2_655 . ?
N15 K7 O1 71.52(5) 2_655 . ?
N15 K7 O1 128.81(6) . . ?
N15 K7 O1 128.81(6) 2_655 2_655 ?
N15 K7 O1 71.52(5) . 2_655 ?
O1 K7 O1 89.52(7) . 2_655 ?
N15 K7 N12 82.37(5) 2_655 . ?
N15 K7 N12 89.91(5) . . ?
O1 K7 N12 72.56(5) . . ?
O1 K7 N12 137.47(5) 2_655 . ?
N15 K7 N12 89.91(5) 2_655 2_655 ?
N15 K7 N12 82.38(5) . 2_655 ?
O1 K7 N12 137.47(5) . 2_655 ?
O1 K7 N12 72.56(5) 2_655 2_655 ?
N12 K7 N12 144.14(8) . 2_655 ?
N15 K7 K3 44.23(4) 2_655 . ?
N15 K7 K3 135.36(4) . . ?
O1 K7 K3 46.01(3) . . ?
O1 K7 K3 135.30(4) 2_655 . ?
N12 K7 K3 45.61(4) . . ?
N12 K7 K3 133.83(4) 2_655 . ?
N15 K7 K3 135.36(4) 2_655 2_655 ?
N15 K7 K3 44.23(4) . 2_655 ?
O1 K7 K3 135.30(4) . 2_655 ?
O1 K7 K3 46.01(3) 2_655 2_655 ?
N12 K7 K3 133.83(4) . 2_655 ?
N12 K7 K3 45.61(4) 2_655 2_655 ?
K3 K7 K3 178.68(2) . 2_655 ?
N3 C7X B1 178.0(2) . . ?
C14 N7 K1 150.80(17) . 4 ?
C40 C7 C42 104.3(3) . . ?
C40 C7 H7A 110.9 . . ?
C42 C7 H7A 110.9 . . ?
C40 C7 H7B 110.9 . . ?
C42 C7 H7B 110.9 . . ?
H7A C7 H7B 108.9 . . ?
N10 C9 B2 178.1(2) . . ?
C10 N9 K2 145.76(17) . 6_566 ?
N4 C8 B1 176.0(2) . . ?
C11 N8 K2 161.77(18) . 6_556 ?
C11 N8 K4 112.74(15) . 4_545 ?
K2 N8 K4 81.58(5) 6_556 4_545 ?
C9 N10 K6 133.08(15) . . ?
C9 N10 K5 114.31(14) . 6_556 ?
K6 N10 K5 90.25(5) . 6_556 ?
N9 C10 B2 178.1(2) . . ?
C20 N12 K7 133.01(15) . . ?
C20 N12 K3 115.64(15) . . ?
K7 N12 K3 90.00(5) . . ?
N5 C12 B3 175.9(2) . . ?
C21 N13 K1 146.09(17) . 1_565 ?
N6 C13 B3 177.7(2) . . ?
N6 C13 K4 57.85(12) . 4_545 ?
B3 C13 K4 121.19(12) . 4_545 ?
C22 N14 K1 158.98(18) . . ?
C22 N14 K4 114.57(15) . . ?
K1 N14 K4 80.03(5) . . ?
N7 C14 B3 175.4(2) . . ?
C26 N15 K3 117.72(15) . 2_655 ?
C26 N15 K7 143.69(16) . . ?
K3 N15 K7 91.52(6) 2_655 . ?
N11 C15 C16 118.93(17) . . ?
N11 C15 B5 118.94(17) . . ?
C16 C15 B5 122.13(17) . . ?
C27 N16 K5 162.59(18) . 1_565 ?
F3 C16 C15 117.67(16) . . ?
F3 C16 C17 117.39(17) . . ?
C15 C16 C17 124.94(18) . . ?
C28 N17 K5 170.24(19) . . ?
C18 C17 C16 112.26(18) . . ?
C18 C17 B6 128.75(17) . . ?
C16 C17 B6 118.98(17) . . ?
C25 N18 K2 170.60(18) . . ?
F4 C18 C17 118.48(17) . . ?
F4 C18 C19 117.17(17) . . ?
C17 C18 C19 124.35(18) . . ?
C24 N19 K4 104.66(14) . . ?
C24 N19 K2 165.07(16) . 7 ?
K4 N19 K2 83.12(4) . 7 ?
N11 C19 C18 119.48(18) . . ?
N11 C19 B4 118.41(17) . . ?
C18 C19 B4 122.10(17) . . ?
C23 N20 K2 148.06(18) . 7_565 ?
N12 C20 B5 178.8(2) . . ?
N13 C21 B5 178.9(2) . . ?
O5 C35 C36 106.95(18) . . ?
O5 C35 H02E 110.3 . . ?
C36 C35 H02E 110.3 . . ?
O5 C35 H02F 110.3 . . ?
C36 C35 H02F 110.3 . . ?
H02E C35 H02F 108.6 . . ?
C35 C36 C37 103.98(19) . . ?
C35 C36 H02M 111.0 . . ?
C37 C36 H02M 111.0 . . ?
C35 C36 H02N 111.0 . . ?
C37 C36 H02N 111.0 . . ?
H02M C36 H02N 109.0 . . ?
C38 C37 C36 102.25(19) . . ?
C38 C37 H02G 111.3 . . ?
C36 C37 H02G 111.3 . . ?
C38 C37 H02H 111.3 . . ?
C36 C37 H02H 111.3 . . ?
H02G C37 H02H 109.2 . . ?
O5 C38 C37 104.59(18) . . ?
O5 C38 H02A 110.8 . . ?
C37 C38 H02A 110.8 . . ?
O5 C38 H02B 110.8 . . ?
C37 C38 H02B 110.8 . . ?
H02A C38 H02B 108.9 . . ?
O1 C39 C40 106.8(3) . . ?
O1 C39 H02Z 110.4 . . ?
C40 C39 H02Z 110.4 . . ?
O1 C39 H010 110.4 . . ?
C40 C39 H010 110.4 . . ?
H02Z C39 H010 108.6 . . ?
C7 C40 C39 104.0(3) . . ?
C7 C40 H098 111.0 . . ?
C39 C40 H098 111.0 . . ?
C7 C40 H099 111.0 . . ?
C39 C40 H099 111.0 . . ?
H098 C40 H099 109.0 . . ?
O1 C42 C7 104.9(3) . . ?
O1 C42 H121 110.8 . . ?
C7 C42 H121 110.8 . . ?
O1 C42 H122 110.8 . . ?
C7 C42 H122 110.8 . . ?
H121 C42 H122 108.8 . . ?
O2 C43 C44 107.1(2) . . ?
O2 C43 H02S 110.3 . . ?
C44 C43 H02S 110.3 . . ?
O2 C43 H02T 110.3 . . ?
C44 C43 H02T 110.3 . . ?
H02S C43 H02T 108.6 . . ?
C45 C44 C43 104.9(3) . . ?
C45 C44 H013 110.8 . . ?
C43 C44 H013 110.8 . . ?
C45 C44 H014 110.8 . . ?
C43 C44 H014 110.8 . . ?
H013 C44 H014 108.8 . . ?
C44 C45 C46 102.6(3) . . ?
C44 C45 H011 111.2 . . ?
C46 C45 H011 111.2 . . ?
C44 C45 H012 111.2 . . ?
C46 C45 H012 111.2 . . ?
H011 C45 H012 109.2 . . ?
O2 C46 C45 105.7(3) . . ?
O2 C46 H02W 110.6 . . ?
C45 C46 H02W 110.6 . . ?
O2 C46 H02X 110.6 . . ?
C45 C46 H02X 110.6 . . ?
H02W C46 H02X 108.7 . . ?
K4 O47 K1 87.52(5) . . ?
K4 O47 H9 121(3) . . ?
K1 O47 H9 125(3) . . ?
K4 O47 H8 114(2) . . ?
K1 O47 H8 107(2) . . ?
H9 O47 H8 102(3) . . ?
K4 O48 K2 88.62(5) . 7 ?
K4 O48 H10 120(3) . . ?
K2 O48 H10 118(3) 7 . ?
K4 O48 H11 113(3) . . ?
K2 O48 H11 111(3) 7 . ?
H10 O48 H11 106(4) . . ?
C50 O49 C53 108.89(17) . . ?
C50 O49 K3 128.17(13) . . ?
C53 O49 K3 122.12(13) . . ?
O49 C50 C51 105.05(17) . . ?
O49 C50 H01A 110.7 . . ?
C51 C50 H01A 110.7 . . ?
O49 C50 H01B 110.7 . . ?
C51 C50 H01B 110.7 . . ?
H01A C50 H01B 108.8 . . ?
C50 C51 C52 102.23(18) . . ?
C50 C51 H02C 111.3 . . ?
C52 C51 H02C 111.3 . . ?
C50 C51 H02D 111.3 . . ?
C52 C51 H02D 111.3 . . ?
H02C C51 H02D 109.2 . . ?
C53 C52 C51 103.54(19) . . ?
C53 C52 H02O 111.1 . . ?
C51 C52 H02O 111.1 . . ?
C53 C52 H02P 111.1 . . ?
C51 C52 H02P 111.1 . . ?
H02O C52 H02P 109.0 . . ?
O49 C53 C52 107.06(18) . . ?
O49 C53 H01C 110.3 . . ?
C52 C53 H01C 110.3 . . ?
O49 C53 H01D 110.3 . . ?
C52 C53 H01D 110.3 . . ?
H01C C53 H01D 108.6 . . ?
N14 C22 B5 176.5(2) . . ?
N19 C24 B6 177.2(2) . . ?
N19 C24 K4 56.25(12) . . ?
B6 C24 K4 124.03(12) . . ?
N20 C23 B6 175.1(2) . . ?
N15 C26 B4 178.1(2) . . ?
N15 C26 K3 45.50(12) . 2_655 ?
B4 C26 K3 136.35(12) . 2_655 ?
N18 C25 B6 175.9(2) . . ?
N16 C27 B4 176.7(2) . . ?
N17 C28 B4 177.2(2) . . ?
O4 C29 C30 106.5(2) . . ?
O4 C29 H02K 110.4 . . ?
C30 C29 H02K 110.4 . . ?
O4 C29 H02L 110.4 . . ?
C30 C29 H02L 110.4 . . ?
H02K C29 H02L 108.6 . . ?
C31 C30 C29 104.7(2) . . ?
C31 C30 H02U 110.8 . . ?
C29 C30 H02U 110.8 . . ?
C31 C30 H02V 110.8 . . ?
C29 C30 H02V 110.8 . . ?
H02U C30 H02V 108.9 . . ?
C32 C31 C30 102.8(2) . . ?
C32 C31 H02Q 111.2 . . ?
C30 C31 H02Q 111.2 . . ?
C32 C31 H02R 111.2 . . ?
C30 C31 H02R 111.2 . . ?
H02Q C31 H02R 109.1 . . ?
O4 C32 C31 104.9(2) . . ?
O4 C32 H02I 110.8 . . ?
C31 C32 H02I 110.8 . . ?
O4 C32 H02J 110.8 . . ?
C31 C32 H02J 110.8 . . ?
H02I C32 H02J 108.8 . . ?
C19 N11 C15 120.03(17) . . ?
N8 C11 B2 177.5(2) . . ?

_refine_diff_density_max         1.075
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.084

####################################################################### 
# 
# 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_JL037_JL_K2Py2acetone
_database_code_depnum_ccdc_archive 'CCDC 1548898'
_audit_update_record             
;
2017-05-09 deposited with the CCDC.
2017-06-26 downloaded from the CCDC.
;


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

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H6 B2 F3 K2 N7 O'
_chemical_formula_sum            'C14 H6 B2 F3 K2 N7 O'
_chemical_formula_weight         445.08

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'
O O 0.0106 0.0060 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

_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, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   25.5118(15)
_cell_length_b                   25.5118(15)
_cell_length_c                   12.1914(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7934.8(11)
_cell_formula_units_Z            16
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6721
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      24.30


_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).
;
_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_F_000             3552
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    0.525
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6928
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31833
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.596
_diffrn_reflns_theta_max         26.030
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3902
_reflns_number_gt                3088
_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. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0106P)²+57.2601P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3902
_refine_ls_number_parameters     322
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0734
_refine_ls_wR_factor_ref         0.1519
_refine_ls_wR_factor_gt          0.1464
_refine_ls_goodness_of_fit_ref   1.272
_refine_ls_restrained_S_all      1.273
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.42165(12) 0.53393(13) 0.4689(3) 0.0213(7) Uani 1 1 d . . . . .
C1 C 0.45891(15) 0.55576(16) 0.5249(3) 0.0257(9) Uani 1 1 d . . . . .
F1 F 0.48277(10) 0.59733(10) 0.4776(2) 0.0397(7) Uani 1 1 d . . . . .
C2 C 0.47441(15) 0.54078(18) 0.6285(3) 0.0279(10) Uani 1 1 d . . . . .
F2 F 0.51162(10) 0.56814(12) 0.6788(2) 0.0496(8) Uani 1 1 d . . . . .
C3 C 0.45121(17) 0.49887(17) 0.6789(3) 0.0290(10) Uani 1 1 d . . . . .
B2 B 0.4642(3) 0.4827(3) 0.8049(6) 0.0282(16) Uani 0.756(4) 1 d . . P A 1
C9 C 0.4297(2) 0.4366(3) 0.8569(5) 0.0339(15) Uani 0.756(4) 1 d . . P A 1
N9 N 0.4049(2) 0.4046(3) 0.8988(4) 0.0475(16) Uani 0.756(4) 1 d . . P A 1
C10 C 0.4538(2) 0.5316(3) 0.8808(5) 0.0376(16) Uani 0.756(4) 1 d . . P A 1
N10 N 0.4426(3) 0.5669(3) 0.9347(5) 0.0569(18) Uani 0.756(4) 1 d . . P A 1
C11 C 0.5241(2) 0.4657(3) 0.8096(5) 0.0436(19) Uani 0.756(4) 1 d . . P A 1
N11 N 0.5669(2) 0.4521(3) 0.8112(5) 0.064(2) Uani 0.756(4) 1 d . . P A 1
B20 B 0.4860(10) 0.4787(12) 0.793(2) 0.0282(16) Uani 0.244(4) 1 d . . P A 2
C20 C 0.5375(7) 0.5095(7) 0.8291(14) 0.029(4) Uani 0.244(4) 1 d . . P A 2
N20 N 0.5757(6) 0.5280(7) 0.8564(12) 0.036(4) Uani 0.244(4) 1 d . . P A 2
C21 C 0.4426(7) 0.4774(10) 0.8870(15) 0.037(5) Uani 0.244(4) 1 d . U P A 2
N21 N 0.4130(8) 0.4749(10) 0.9565(16) 0.065(6) Uani 0.244(4) 1 d . U P A 2
C22 C 0.4997(8) 0.4188(8) 0.7768(14) 0.033(5) Uani 0.244(4) 1 d . . P A 2
N22 N 0.5115(10) 0.3760(9) 0.7672(17) 0.071(7) Uani 0.244(4) 1 d . . P A 2
C4 C 0.41248(16) 0.47558(16) 0.6160(3) 0.0244(9) Uani 1 1 d . . . . .
F4 F 0.38769(11) 0.43249(9) 0.6577(2) 0.0366(6) Uani 1 1 d . . . . .
C5 C 0.39660(14) 0.49256(15) 0.5143(3) 0.0196(8) Uani 1 1 d . . . . .
B1 B 0.34882(18) 0.46694(19) 0.4441(4) 0.0254(10) Uani 1 1 d . . . . .
C6 C 0.36808(17) 0.4185(2) 0.3726(4) 0.0418(13) Uani 1 1 d . . . . .
N6 N 0.38164(17) 0.3840(2) 0.3211(5) 0.0719(18) Uani 1 1 d . . . . .
C7 C 0.32595(16) 0.51023(19) 0.3625(4) 0.0318(10) Uani 1 1 d . . . . .
N7 N 0.30958(16) 0.54220(19) 0.3063(4) 0.0489(12) Uani 1 1 d . . . . .
C8 C 0.30174(16) 0.44724(16) 0.5205(4) 0.0271(9) Uani 1 1 d . . . . .
N8 N 0.26810(14) 0.43362(15) 0.5749(3) 0.0358(9) Uani 1 1 d . . . . .
K1 K 0.15934(4) 0.45492(4) 0.56003(8) 0.0327(3) Uani 1 1 d . . . . .
K2 K 0.37921(5) 0.36032(5) 1.09457(11) 0.0543(4) Uani 1 1 d . . . . .
O1 O 0.4722(2) 0.3183(3) 1.1073(7) 0.138(3) Uani 1 1 d . . . . .
C12 C 0.5190(4) 0.3173(4) 1.1200(13) 0.149(5) Uani 1 1 d . . . . .
C13 C 0.5524(4) 0.3106(5) 1.0066(14) 0.229(9) Uani 1 1 d . . . . .
H13A H 0.5807 0.2852 1.0180 0.343 Uiso 1 1 calc R U . . .
H13B H 0.5674 0.3445 0.9855 0.343 Uiso 1 1 calc R U . . .
H13C H 0.5292 0.2981 0.9481 0.343 Uiso 1 1 calc R U . . .
C14 C 0.5406(7) 0.3144(6) 1.2358(15) 0.286(13) Uani 1 1 d . . . . .
H14A H 0.5790 0.3132 1.2331 0.429 Uiso 1 1 calc R U . . .
H14B H 0.5274 0.2828 1.2720 0.429 Uiso 1 1 calc R U . . .
H14C H 0.5295 0.3454 1.2772 0.429 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
N1 C1 1.296(5) . ?
N1 C5 1.352(5) . ?
N1 K2 2.978(3) 3_554 ?
C1 F1 1.352(5) . ?
C1 C2 1.378(6) . ?
C1 K2 3.386(4) 3_554 ?
F1 K2 2.988(3) 3_554 ?
C2 F2 1.328(5) . ?
C2 C3 1.368(6) . ?
C3 C4 1.385(6) . ?
C3 B2 1.625(8) . ?
C3 B20 1.73(3) . ?
B2 C10 1.577(11) . ?
B2 C11 1.589(9) . ?
B2 C9 1.600(11) . ?
C9 N9 1.152(8) . ?
N9 K2 2.720(5) . ?
N9 K1 3.006(6) 3 ?
C10 N10 1.151(9) . ?
N10 K1 3.067(6) 2_565 ?
C11 N11 1.145(8) . ?
N11 K1 2.834(6) 10_657 ?
N11 K2 3.022(7) 11_667 ?
B20 C22 1.58(4) . ?
B20 C21 1.59(3) . ?
B20 C20 1.59(3) . ?
C20 N20 1.13(2) . ?
N20 K1 3.011(15) 10_657 ?
N20 K2 3.129(17) 9_667 ?
C21 N21 1.14(3) . ?
N21 K1 2.86(2) 2_565 ?
C22 N22 1.14(3) . ?
C22 K2 3.41(2) 11_667 ?
N22 K2 2.87(3) 11_667 ?
C4 F4 1.366(5) . ?
C4 C5 1.374(5) . ?
F4 K1 3.063(3) 3 ?
C5 B1 1.626(6) . ?
B1 C6 1.590(7) . ?
B1 C7 1.597(7) . ?
B1 C8 1.601(6) . ?
C6 N6 1.136(6) . ?
N6 K2 2.828(6) 1_554 ?
C7 N7 1.145(6) . ?
C7 K2 3.450(5) 3_554 ?
N7 K1 2.943(5) 4_454 ?
N7 K2 3.053(4) 3_554 ?
N7 K1 3.106(5) 2_564 ?
C8 N8 1.138(5) . ?
N8 K1 2.833(4) . ?
N8 K1 3.013(4) 3 ?
K1 N11 2.834(6) 10_557 ?
K1 N21 2.86(2) 2_564 ?
K1 N7 2.943(5) 3 ?
K1 N9 3.006(6) 4_454 ?
K1 N20 3.011(15) 10_557 ?
K1 N8 3.013(4) 4_454 ?
K1 F4 3.063(3) 4_454 ?
K1 N10 3.067(6) 2_564 ?
K1 N7 3.106(5) 2_565 ?
K1 K2 4.2667(16) 4_454 ?
K1 K1 4.7576(11) 3 ?
K2 O1 2.608(6) . ?
K2 N6 2.828(6) 1_556 ?
K2 N22 2.87(3) 16_657 ?
K2 N1 2.978(3) 4_455 ?
K2 F1 2.989(3) 4_455 ?
K2 N11 3.022(7) 16_657 ?
K2 N7 3.053(4) 4_455 ?
K2 N20 3.129(17) 9_667 ?
K2 C1 3.386(4) 4_455 ?
K2 C22 3.41(2) 16_657 ?
K2 C7 3.450(5) 4_455 ?
O1 C12 1.204(10) . ?
C12 C14 1.518(19) . ?
C12 C13 1.634(17) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?

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
C1 N1 C5 117.8(3) . . ?
C1 N1 K2 96.8(2) . 3_554 ?
C5 N1 K2 135.7(2) . 3_554 ?
N1 C1 F1 116.3(4) . . ?
N1 C1 C2 125.1(4) . . ?
F1 C1 C2 118.7(4) . . ?
N1 C1 K2 60.9(2) . 3_554 ?
F1 C1 K2 61.6(2) . 3_554 ?
C2 C1 K2 154.0(3) . 3_554 ?
C1 F1 K2 95.0(2) . 3_554 ?
F2 C2 C3 120.8(4) . . ?
F2 C2 C1 118.9(4) . . ?
C3 C2 C1 120.3(4) . . ?
C2 C3 C4 113.3(4) . . ?
C2 C3 B2 122.4(5) . . ?
C4 C3 B2 124.1(5) . . ?
C2 C3 B20 111.9(10) . . ?
C4 C3 B20 133.2(11) . . ?
C10 B2 C11 110.9(6) . . ?
C10 B2 C9 104.9(6) . . ?
C11 B2 C9 108.4(6) . . ?
C10 B2 C3 108.6(5) . . ?
C11 B2 C3 107.5(5) . . ?
C9 B2 C3 116.7(5) . . ?
N9 C9 B2 176.8(7) . . ?
C9 N9 K2 144.7(5) . . ?
C9 N9 K1 108.9(4) . 3 ?
K2 N9 K1 96.21(18) . 3 ?
N10 C10 B2 175.4(7) . . ?
C10 N10 K1 110.6(5) . 2_565 ?
N11 C11 B2 177.8(9) . . ?
C11 N11 K1 142.6(6) . 10_657 ?
C11 N11 K2 123.2(6) . 11_667 ?
K1 N11 K2 93.47(17) 10_657 11_667 ?
C22 B20 C21 103(2) . . ?
C22 B20 C20 109.1(19) . . ?
C21 B20 C20 113(2) . . ?
C22 B20 C3 107.4(18) . . ?
C21 B20 C3 103.2(15) . . ?
C20 B20 C3 120(2) . . ?
N20 C20 B20 175(2) . . ?
C20 N20 K1 116.7(14) . 10_657 ?
C20 N20 K2 138.8(14) . 9_667 ?
K1 N20 K2 103.8(4) 10_657 9_667 ?
N21 C21 B20 177(2) . . ?
C21 N21 K1 136(2) . 2_565 ?
N22 C22 B20 177(2) . . ?
N22 C22 K2 52.6(16) . 11_667 ?
B20 C22 K2 125.8(14) . 11_667 ?
C22 N22 K2 109.0(18) . 11_667 ?
F4 C4 C5 116.9(4) . . ?
F4 C4 C3 118.0(4) . . ?
C5 C4 C3 125.1(4) . . ?
C4 F4 K1 137.6(2) . 3 ?
N1 C5 C4 118.4(4) . . ?
N1 C5 B1 116.9(3) . . ?
C4 C5 B1 124.7(4) . . ?
C6 B1 C7 108.0(4) . . ?
C6 B1 C8 107.9(4) . . ?
C7 B1 C8 107.8(3) . . ?
C6 B1 C5 111.7(4) . . ?
C7 B1 C5 108.9(3) . . ?
C8 B1 C5 112.5(3) . . ?
N6 C6 B1 179.6(7) . . ?
C6 N6 K2 134.3(5) . 1_554 ?
N7 C7 B1 178.2(5) . . ?
N7 C7 K2 60.5(3) . 3_554 ?
B1 C7 K2 118.4(3) . 3_554 ?
C7 N7 K1 128.4(4) . 4_454 ?
C7 N7 K2 100.5(3) . 3_554 ?
K1 N7 K2 107.42(16) 4_454 3_554 ?
C7 N7 K1 120.2(4) . 2_564 ?
K1 N7 K1 103.70(12) 4_454 2_564 ?
K2 N7 K1 87.69(11) 3_554 2_564 ?
N8 C8 B1 179.5(5) . . ?
C8 N8 K1 130.0(3) . . ?
C8 N8 K1 116.4(3) . 3 ?
K1 N8 K1 108.89(12) . 3 ?
N8 K1 N11 140.78(15) . 10_557 ?
N8 K1 N21 141.2(4) . 2_564 ?
N8 K1 N7 76.32(12) . 3 ?
N11 K1 N7 112.44(19) 10_557 3 ?
N21 K1 N7 72.3(5) 2_564 3 ?
N8 K1 N9 80.65(15) . 4_454 ?
N11 K1 N9 75.1(2) 10_557 4_454 ?
N7 K1 N9 150.24(15) 3 4_454 ?
N8 K1 N20 142.3(3) . 10_557 ?
N21 K1 N20 46.0(5) 2_564 10_557 ?
N7 K1 N20 75.0(3) 3 10_557 ?
N8 K1 N8 84.44(11) . 4_454 ?
N11 K1 N8 134.76(15) 10_557 4_454 ?
N21 K1 N8 64.5(4) 2_564 4_454 ?
N7 K1 N8 72.03(11) 3 4_454 ?
N9 K1 N8 124.32(13) 4_454 4_454 ?
N20 K1 N8 109.0(3) 10_557 4_454 ?
N8 K1 F4 72.65(10) . 4_454 ?
N11 K1 F4 118.46(16) 10_557 4_454 ?
N21 K1 F4 109.8(5) 2_564 4_454 ?
N7 K1 F4 127.55(11) 3 4_454 ?
N9 K1 F4 60.48(11) 4_454 4_454 ?
N20 K1 F4 145.1(3) 10_557 4_454 ?
N8 K1 F4 63.86(9) 4_454 4_454 ?
N8 K1 N10 145.82(16) . 2_564 ?
N11 K1 N10 64.25(17) 10_557 2_564 ?
N7 K1 N10 120.89(15) 3 2_564 ?
N9 K1 N10 88.62(18) 4_454 2_564 ?
N8 K1 N10 75.05(14) 4_454 2_564 ?
F4 K1 N10 73.82(14) 4_454 2_564 ?
N8 K1 N7 72.11(11) . 2_565 ?
N11 K1 N7 71.20(14) 10_557 2_565 ?
N21 K1 N7 125.2(4) 2_564 2_565 ?
N7 K1 N7 83.48(12) 3 2_565 ?
N9 K1 N7 71.59(14) 4_454 2_565 ?
N20 K1 N7 80.7(3) 10_557 2_565 ?
N8 K1 N7 149.53(11) 4_454 2_565 ?
F4 K1 N7 123.72(11) 4_454 2_565 ?
N10 K1 N7 134.60(14) 2_564 2_565 ?
N8 K1 K2 97.97(8) . 4_454 ?
N11 K1 K2 44.99(15) 10_557 4_454 ?
N21 K1 K2 119.0(4) 2_564 4_454 ?
N7 K1 K2 126.32(9) 3 4_454 ?
N9 K1 K2 39.33(10) 4_454 4_454 ?
N20 K1 K2 80.1(3) 10_557 4_454 ?
N8 K1 K2 161.60(8) 4_454 4_454 ?
F4 K1 K2 99.30(6) 4_454 4_454 ?
N10 K1 K2 93.73(12) 2_564 4_454 ?
N7 K1 K2 45.64(8) 2_565 4_454 ?
N8 K1 K1 36.81(8) . 3 ?
N11 K1 K1 104.16(13) 10_557 3 ?
N21 K1 K1 154.7(5) 2_564 3 ?
N7 K1 K1 85.76(8) 3 3 ?
N9 K1 K1 64.57(13) 4_454 3 ?
N20 K1 K1 116.8(3) 10_557 3 ?
N8 K1 K1 121.05(8) 4_454 3 ?
F4 K1 K1 93.41(6) 4_454 3 ?
N10 K1 K1 153.10(13) 2_564 3 ?
N7 K1 K1 36.94(8) 2_565 3 ?
K2 K1 K1 64.50(3) 4_454 3 ?
O1 K2 N9 90.2(2) . . ?
O1 K2 N6 90.6(2) . 1_556 ?
N9 K2 N6 139.73(19) . 1_556 ?
O1 K2 N22 73.1(5) . 16_657 ?
N6 K2 N22 130.7(4) 1_556 16_657 ?
O1 K2 N1 126.82(18) . 4_455 ?
N9 K2 N1 139.17(14) . 4_455 ?
N6 K2 N1 65.12(11) 1_556 4_455 ?
N22 K2 N1 87.9(4) 16_657 4_455 ?
O1 K2 F1 83.59(17) . 4_455 ?
N9 K2 F1 150.64(16) . 4_455 ?
N6 K2 F1 69.24(13) 1_556 4_455 ?
N22 K2 F1 63.0(4) 16_657 4_455 ?
N1 K2 F1 44.29(8) 4_455 4_455 ?
O1 K2 N11 120.7(2) . 16_657 ?
N9 K2 N11 76.48(18) . 16_657 ?
N6 K2 N11 135.00(16) 1_556 16_657 ?
N1 K2 N11 70.09(14) 4_455 16_657 ?
F1 K2 N11 82.11(12) 4_455 16_657 ?
O1 K2 N7 161.03(18) . 4_455 ?
N9 K2 N7 76.29(14) . 4_455 ?
N6 K2 N7 91.30(14) 1_556 4_455 ?
N22 K2 N7 118.8(5) 16_657 4_455 ?
N1 K2 N7 70.60(10) 4_455 4_455 ?
F1 K2 N7 114.65(10) 4_455 4_455 ?
N11 K2 N7 69.55(16) 16_657 4_455 ?
O1 K2 N20 91.7(3) . 9_667 ?
N6 K2 N20 67.1(3) 1_556 9_667 ?
N22 K2 N20 155.2(5) 16_657 9_667 ?
N1 K2 N20 116.9(3) 4_455 9_667 ?
F1 K2 N20 136.0(3) 4_455 9_667 ?
N7 K2 N20 71.8(3) 4_455 9_667 ?
O1 K2 C1 104.49(18) . 4_455 ?
N9 K2 C1 156.85(16) . 4_455 ?
N6 K2 C1 59.28(13) 1_556 4_455 ?
N22 K2 C1 79.9(4) 16_657 4_455 ?
N1 K2 C1 22.34(9) 4_455 4_455 ?
F1 K2 C1 23.44(8) 4_455 4_455 ?
N11 K2 C1 80.62(14) 16_657 4_455 ?
N7 K2 C1 92.64(11) 4_455 4_455 ?
N20 K2 C1 123.6(3) 9_667 4_455 ?
O1 K2 C22 90.7(4) . 16_657 ?
N6 K2 C22 127.4(3) 1_556 16_657 ?
N22 K2 C22 18.4(5) 16_657 16_657 ?
N1 K2 C22 72.6(3) 4_455 16_657 ?
F1 K2 C22 58.7(3) 4_455 16_657 ?
N7 K2 C22 103.1(4) 4_455 16_657 ?
N20 K2 C22 165.3(4) 9_667 16_657 ?
C1 K2 C22 69.6(3) 4_455 16_657 ?
O1 K2 C7 172.0(2) . 4_455 ?
N9 K2 C7 94.12(14) . 4_455 ?
N6 K2 C7 81.77(13) 1_556 4_455 ?
N22 K2 C7 113.8(5) 16_657 4_455 ?
N1 K2 C7 51.60(10) 4_455 4_455 ?
F1 K2 C7 95.77(9) 4_455 4_455 ?
N11 K2 C7 66.99(16) 16_657 4_455 ?
N7 K2 C7 19.04(10) 4_455 4_455 ?
N20 K2 C7 83.2(3) 9_667 4_455 ?
C1 K2 C7 73.60(11) 4_455 4_455 ?
C22 K2 C7 95.8(4) 16_657 4_455 ?
C12 O1 K2 156.6(8) . . ?
O1 C12 C14 118.8(14) . . ?
O1 C12 C13 114.3(14) . . ?
C14 C12 C13 126.3(11) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?

_refine_diff_density_max         1.210
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.094

####################################################################### 
# 
# 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_JL092_JL_KB10a
_database_code_depnum_ccdc_archive 'CCDC 1548908'
_audit_update_record             
;
2017-05-09 deposited with the CCDC.
2017-06-26 downloaded from the CCDC.
;


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

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H3 B F4 K N3 O'
_chemical_formula_sum            'C10 H3 B F4 K N3 O'
_chemical_formula_weight         307.06

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'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   10.9629(9)
_cell_length_b                   8.0873(7)
_cell_length_c                   14.1771(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1256.95(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2836
_cell_measurement_theta_min      2.87
_cell_measurement_theta_max      26.55
_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).
;

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_F_000             608
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    0.468
_shelx_estimated_absorpt_T_min   0.861
_shelx_estimated_absorpt_T_max   0.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6454
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10502
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.348
_diffrn_reflns_theta_max         26.791
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1439
_reflns_number_gt                1158
_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. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0431P)²+0.5496P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1439
_refine_ls_number_parameters     104
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_ref         0.0984
_refine_ls_wR_factor_gt          0.0934
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.43567(5) 0.7500 0.99557(4) 0.02316(18) Uani 1 2 d S T P . .
O1 O 0.81117(19) 0.2500 0.44781(16) 0.0641(9) Uani 1 2 d S T P . .
F1 F 0.53672(13) 0.54201(17) 0.64370(11) 0.0507(4) Uani 1 1 d . . . . .
N1 N 0.44621(17) 0.5046(2) 0.86145(14) 0.0386(5) Uani 1 1 d . . . . .
C1 C 0.44088(17) 0.4047(2) 0.80502(14) 0.0260(4) Uani 1 1 d . . . . .
B1 B 0.4303(2) 0.2500 0.7347(2) 0.0196(6) Uani 1 2 d S T P . .
N2 N 0.2030(2) 0.2500 0.65642(18) 0.0384(7) Uani 1 2 d S T P . .
F2 F 0.71085(14) 0.5417(2) 0.51301(11) 0.0639(5) Uani 1 1 d . . . . .
C2 C 0.2972(2) 0.2500 0.69035(19) 0.0247(6) Uani 1 2 d S T P . .
C3 C 0.5325(2) 0.2500 0.65204(19) 0.0240(6) Uani 1 2 d S T P . .
C4 C 0.57908(19) 0.3947(3) 0.61400(15) 0.0327(5) Uani 1 1 d . . . . .
C5 C 0.6696(2) 0.3950(3) 0.54523(17) 0.0414(6) Uani 1 1 d . . . . .
C6 C 0.7167(3) 0.2500 0.5114(2) 0.0423(9) Uani 1 2 d S T P . .
C7 C 0.7751(3) 0.2500 0.3513(2) 0.0412(8) Uani 1 2 d S T P . .
H7A H 0.8469 0.2678 0.3113 0.062 Uiso 0.5 1 calc R U P . .
H7B H 0.7160 0.3388 0.3405 0.062 Uiso 0.5 1 calc R U P . .
H7C H 0.7378 0.1434 0.3356 0.062 Uiso 0.5 1 calc R U P . .


_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 N2 2.740(3) 2_565 ?
K1 N1 2.7508(19) . ?
K1 N1 2.7508(19) 7_575 ?
K1 O1 2.857(2) 2_665 ?
K1 F2 2.9878(16) 6_557 ?
K1 F2 2.9878(16) 4_466 ?
K1 N1 3.166(2) 3_657 ?
K1 N1 3.166(2) 5_667 ?
K1 C1 3.375(2) 3_657 ?
K1 C1 3.375(2) 5_667 ?
K1 K1 4.2845(5) 5_677 ?
K1 K1 4.2845(5) 5_667 ?
O1 C6 1.373(4) . ?
O1 C7 1.425(4) . ?
O1 K1 2.857(2) 2_664 ?
F1 C4 1.346(3) . ?
N1 C1 1.139(3) . ?
N1 K1 3.166(2) 5_667 ?
C1 B1 1.604(3) . ?
C1 K1 3.375(2) 5_667 ?
B1 C2 1.590(4) . ?
B1 C1 1.604(3) 7_565 ?
B1 C3 1.621(4) . ?
N2 C2 1.139(4) . ?
N2 K1 2.740(3) 2_564 ?
F2 C5 1.350(3) . ?
F2 K1 2.9878(16) 6_657 ?
C3 C4 1.386(3) . ?
C3 C4 1.386(3) 7_565 ?
C4 C5 1.391(3) . ?
C5 C6 1.368(3) . ?
C6 C5 1.368(3) 7_565 ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?

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
N2 K1 N1 126.76(5) 2_565 . ?
N2 K1 N1 126.76(5) 2_565 7_575 ?
N1 K1 N1 92.35(9) . 7_575 ?
N2 K1 O1 137.39(7) 2_565 2_665 ?
N1 K1 O1 78.19(5) . 2_665 ?
N1 K1 O1 78.19(5) 7_575 2_665 ?
N2 K1 F2 64.94(5) 2_565 6_557 ?
N1 K1 F2 66.41(5) . 6_557 ?
N1 K1 F2 114.41(6) 7_575 6_557 ?
O1 K1 F2 142.35(4) 2_665 6_557 ?
N2 K1 F2 64.94(5) 2_565 4_466 ?
N1 K1 F2 114.41(6) . 4_466 ?
N1 K1 F2 66.41(5) 7_575 4_466 ?
O1 K1 F2 142.35(4) 2_665 4_466 ?
F2 K1 F2 68.64(7) 6_557 4_466 ?
N2 K1 N1 72.19(5) 2_565 3_657 ?
N1 K1 N1 153.44(3) . 3_657 ?
N1 K1 N1 87.49(6) 7_575 3_657 ?
O1 K1 N1 75.78(5) 2_665 3_657 ?
F2 K1 N1 136.89(5) 6_557 3_657 ?
F2 K1 N1 89.82(5) 4_466 3_657 ?
N2 K1 N1 72.19(5) 2_565 5_667 ?
N1 K1 N1 87.49(5) . 5_667 ?
N1 K1 N1 153.44(3) 7_575 5_667 ?
O1 K1 N1 75.78(5) 2_665 5_667 ?
F2 K1 N1 89.82(5) 6_557 5_667 ?
F2 K1 N1 136.89(5) 4_466 5_667 ?
N1 K1 N1 81.13(7) 3_657 5_667 ?
N2 K1 C1 61.66(6) 2_565 3_657 ?
N1 K1 C1 146.06(5) . 3_657 ?
N1 K1 C1 107.14(6) 7_575 3_657 ?
O1 K1 C1 78.98(5) 2_665 3_657 ?
F2 K1 C1 125.02(5) 6_557 3_657 ?
F2 K1 C1 98.97(5) 4_466 3_657 ?
N1 K1 C1 19.71(4) 3_657 3_657 ?
N1 K1 C1 62.66(5) 5_667 3_657 ?
N2 K1 C1 61.66(6) 2_565 5_667 ?
N1 K1 C1 107.14(5) . 5_667 ?
N1 K1 C1 146.06(6) 7_575 5_667 ?
O1 K1 C1 78.98(5) 2_665 5_667 ?
F2 K1 C1 98.97(5) 6_557 5_667 ?
F2 K1 C1 125.02(5) 4_466 5_667 ?
N1 K1 C1 62.66(5) 3_657 5_667 ?
N1 K1 C1 19.71(4) 5_667 5_667 ?
C1 K1 C1 43.52(7) 3_657 5_667 ?
N2 K1 K1 99.10(2) 2_565 5_677 ?
N1 K1 K1 133.42(5) . 5_677 ?
N1 K1 K1 47.59(4) 7_575 5_677 ?
O1 K1 K1 71.766(16) 2_665 5_677 ?
F2 K1 K1 143.60(4) 6_557 5_677 ?
F2 K1 K1 74.97(3) 4_466 5_677 ?
N1 K1 K1 39.90(3) 3_657 5_677 ?
N1 K1 K1 117.41(4) 5_667 5_677 ?
C1 K1 K1 59.57(4) 3_657 5_677 ?
C1 K1 K1 101.14(4) 5_667 5_677 ?
N2 K1 K1 99.10(2) 2_565 5_667 ?
N1 K1 K1 47.59(4) . 5_667 ?
N1 K1 K1 133.42(5) 7_575 5_667 ?
O1 K1 K1 71.766(16) 2_665 5_667 ?
F2 K1 K1 74.97(3) 6_557 5_667 ?
F2 K1 K1 143.60(4) 4_466 5_667 ?
N1 K1 K1 117.41(4) 3_657 5_667 ?
N1 K1 K1 39.90(3) 5_667 5_667 ?
C1 K1 K1 101.14(4) 3_657 5_667 ?
C1 K1 K1 59.57(3) 5_667 5_667 ?
K1 K1 K1 141.40(3) 5_677 5_667 ?
C6 O1 C7 114.9(2) . . ?
C6 O1 K1 125.27(18) . 2_664 ?
C7 O1 K1 119.80(17) . 2_664 ?
C1 N1 K1 174.56(17) . . ?
C1 N1 K1 90.54(14) . 5_667 ?
K1 N1 K1 92.51(5) . 5_667 ?
N1 C1 B1 173.7(2) . . ?
N1 C1 K1 69.75(13) . 5_667 ?
B1 C1 K1 105.09(12) . 5_667 ?
C2 B1 C1 108.19(15) . . ?
C2 B1 C1 108.19(15) . 7_565 ?
C1 B1 C1 102.6(2) . 7_565 ?
C2 B1 C3 110.4(2) . . ?
C1 B1 C3 113.55(14) . . ?
C1 B1 C3 113.55(14) 7_565 . ?
C2 N2 K1 148.7(2) . 2_564 ?
C5 F2 K1 141.81(13) . 6_657 ?
N2 C2 B1 178.3(3) . . ?
C4 C3 C4 115.2(3) . 7_565 ?
C4 C3 B1 122.42(13) . . ?
C4 C3 B1 122.42(13) 7_565 . ?
F1 C4 C3 119.88(18) . . ?
F1 C4 C5 117.6(2) . . ?
C3 C4 C5 122.5(2) . . ?
F2 C5 C6 120.5(2) . . ?
F2 C5 C4 118.5(2) . . ?
C6 C5 C4 120.9(2) . . ?
C5 C6 C5 117.9(3) . 7_565 ?
C5 C6 O1 121.01(14) . . ?
C5 C6 O1 121.01(14) 7_565 . ?
O1 C7 H7A 109.5 . . ?
O1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

_refine_diff_density_max         0.495
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.056

####################################################################### 
# 
# 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_JL019_JL_KPy1
_database_code_depnum_ccdc_archive 'CCDC 1548910'
_audit_update_record             
;
2017-05-09 deposited with the CCDC.
2017-06-26 downloaded from the CCDC.
;


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

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 B2 F8 K2 N8'
_chemical_formula_sum            'C16 B2 F8 K2 N8'
_chemical_formula_weight         556.06

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-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                   10.0487(6)
_cell_length_b                   18.9832(12)
_cell_length_c                   22.2949(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4252.9(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9894
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      26.73
_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).
;

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_F_000             2176
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.280
_exptl_absorpt_coefficient_mu    0.539
_shelx_estimated_absorpt_T_min   0.830
_shelx_estimated_absorpt_T_max   0.864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6724
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28164
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.827
_diffrn_reflns_theta_max         26.727
_diffrn_reflns_theta_full        26.000
_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             4508
_reflns_number_gt                3993
_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. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0587P)²+10.7837P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4508
_refine_ls_number_parameters     325
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0575
_refine_ls_wR_factor_ref         0.1509
_refine_ls_wR_factor_gt          0.1470
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_restrained_S_all      1.134
_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 0.07806(7) 0.30053(3) 0.44158(3) 0.02283(18) Uani 1 1 d . . . . .
N1 N 0.3562(3) 0.29644(15) 0.44164(12) 0.0276(6) Uani 1 1 d . . . . .
F1 F 1.3549(2) 0.65928(12) 0.30638(9) 0.0398(5) Uani 1 1 d . . . . .
C1 C 0.4539(3) 0.31196(15) 0.41924(13) 0.0199(6) Uani 1 1 d . . . . .
B1 B 0.5880(3) 0.33948(17) 0.38940(15) 0.0177(6) Uani 1 1 d . . . . .
K2 K 0.67041(6) 0.61378(3) 0.44724(3) 0.02593(19) Uani 1 1 d . . . . .
N2 N 0.8043(3) 0.26505(14) 0.42919(12) 0.0239(6) Uani 1 1 d . . . . .
F2 F 1.3236(2) 0.65603(13) 0.18878(11) 0.0482(6) Uani 1 1 d . . . . .
C2 C 0.7122(3) 0.29555(15) 0.41386(13) 0.0177(6) Uani 1 1 d . . . . .
B2 B 1.1799(3) 0.57865(17) 0.39558(16) 0.0194(7) Uani 1 1 d . . . . .
F3 F 0.9759(2) 0.50764(12) 0.20165(10) 0.0387(5) Uani 1 1 d . . . . .
N3 N 0.6150(4) 0.47516(16) 0.42916(14) 0.0397(8) Uani 1 1 d . . . . .
C3 C 0.6050(3) 0.41876(16) 0.41164(14) 0.0243(7) Uani 1 1 d . . . . .
F4 F 0.9897(2) 0.50337(11) 0.32206(9) 0.0338(5) Uani 1 1 d . . . . .
N4 N 0.9522(3) 0.63835(14) 0.44120(12) 0.0240(6) Uani 1 1 d . . . . .
C4 C 1.0475(3) 0.61406(15) 0.42217(14) 0.0207(6) Uani 1 1 d . . . . .
F5 F 0.77352(19) 0.40912(10) 0.30843(8) 0.0308(4) Uani 1 1 d . . . . .
N5 N 1.1856(3) 0.44435(15) 0.44194(13) 0.0295(6) Uani 1 1 d . . . . .
C5 C 1.1850(3) 0.49997(16) 0.42160(14) 0.0227(6) Uani 1 1 d . . . . .
F6 F 0.7706(2) 0.39999(11) 0.18872(9) 0.0356(5) Uani 1 1 d . . . . .
N6 N 1.3931(3) 0.64957(14) 0.44255(12) 0.0229(6) Uani 1 1 d . . . . .
C6 C 1.3046(3) 0.62027(15) 0.42254(14) 0.0190(6) Uani 1 1 d . . . . .
F7 F 0.4198(2) 0.25168(12) 0.19126(9) 0.0400(5) Uani 1 1 d . . . . .
N7 N 1.1504(3) 0.58197(16) 0.19519(14) 0.0333(7) Uani 1 1 d . . . . .
C7 C 0.5867(3) 0.33383(14) 0.31642(13) 0.0170(6) Uani 1 1 d . . . . .
C8 C 0.6795(3) 0.36952(16) 0.28186(13) 0.0204(6) Uani 1 1 d . . . . .
F8 F 0.4056(2) 0.25337(11) 0.30958(9) 0.0329(5) Uani 1 1 d . . . . .
N8 N 0.5940(3) 0.32618(15) 0.18988(12) 0.0278(6) Uani 1 1 d . . . . .
C9 C 0.6794(3) 0.36452(17) 0.22029(15) 0.0255(7) Uani 1 1 d . . . . .
C10 C 0.4989(3) 0.29300(16) 0.28352(15) 0.0230(6) Uani 1 1 d . . . . .
C11 C 0.5068(3) 0.29127(17) 0.22189(15) 0.0270(7) Uani 1 1 d . . . . .
C12 C 1.1745(3) 0.58022(16) 0.32247(14) 0.0221(6) Uani 1 1 d . . . . .
C13 C 1.2576(3) 0.61891(17) 0.28515(17) 0.0290(7) Uani 1 1 d . . . . .
C14 C 1.2413(4) 0.61777(19) 0.22351(17) 0.0338(8) Uani 1 1 d . . . . .
C15 C 1.0780(3) 0.54239(16) 0.29148(15) 0.0247(7) Uani 1 1 d . . . . .
C16 C 1.0697(3) 0.54447(17) 0.22985(16) 0.0280(7) 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 N1 2.796(3) . ?
K1 N2 2.845(3) 1_455 ?
K1 N4 2.875(3) 5_666 ?
K1 N6 2.880(3) 8_755 ?
K1 N5 2.936(3) 1_455 ?
K1 N8 2.975(3) 6_556 ?
K1 K2 3.8961(10) 5_666 ?
K1 K2 4.3380(10) 8_655 ?
N1 C1 1.140(4) . ?
N1 K2 3.019(3) 5_666 ?
F1 C13 1.329(4) . ?
C1 B1 1.592(4) . ?
C1 K2 3.523(3) 5_666 ?
B1 C3 1.594(4) . ?
B1 C2 1.596(4) . ?
B1 C7 1.631(4) . ?
K2 N3 2.720(3) . ?
K2 N6 2.871(3) 1_455 ?
K2 N4 2.873(3) . ?
K2 N2 2.911(3) 8_765 ?
K2 N1 3.019(3) 5_666 ?
K2 N5 3.069(3) 5_766 ?
K2 N7 3.239(3) 6_556 ?
K2 C1 3.523(3) 5_666 ?
K2 K1 3.8960(10) 5_666 ?
K2 K1 4.3380(10) 8_665 ?
N2 C2 1.144(4) . ?
N2 K1 2.845(3) 1_655 ?
N2 K2 2.911(3) 8_755 ?
F2 C14 1.346(4) . ?
B2 C6 1.598(4) . ?
B2 C5 1.603(4) . ?
B2 C4 1.605(4) . ?
B2 C12 1.631(5) . ?
F3 C16 1.331(4) . ?
N3 C3 1.144(4) . ?
F4 C15 1.342(4) . ?
N4 C4 1.144(4) . ?
N4 K1 2.875(3) 5_666 ?
F5 C8 1.345(3) . ?
N5 C5 1.149(4) . ?
N5 K1 2.936(3) 1_655 ?
N5 K2 3.069(3) 5_766 ?
F6 C9 1.337(4) . ?
N6 C6 1.140(4) . ?
N6 K2 2.871(3) 1_655 ?
N6 K1 2.880(3) 8_765 ?
F7 C11 1.340(4) . ?
N7 C14 1.302(5) . ?
N7 C16 1.327(5) . ?
N7 K2 3.239(3) 6_656 ?
C7 C10 1.385(4) . ?
C7 C8 1.386(4) . ?
C8 C9 1.376(4) . ?
F8 C10 1.335(4) . ?
N8 C11 1.310(5) . ?
N8 C9 1.314(4) . ?
N8 K1 2.975(3) 6_656 ?
C10 C11 1.377(4) . ?
C12 C13 1.389(4) . ?
C12 C15 1.390(4) . ?
C13 C14 1.384(5) . ?
C15 C16 1.377(5) . ?

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
N1 K1 N2 163.70(9) . 1_455 ?
N1 K1 N4 96.70(8) . 5_666 ?
N2 K1 N4 94.67(8) 1_455 5_666 ?
N1 K1 N6 82.63(8) . 8_755 ?
N2 K1 N6 82.10(8) 1_455 8_755 ?
N4 K1 N6 113.91(8) 5_666 8_755 ?
N1 K1 N5 70.00(9) . 1_455 ?
N2 K1 N5 125.18(8) 1_455 1_455 ?
N4 K1 N5 70.20(8) 5_666 1_455 ?
N6 K1 N5 152.62(8) 8_755 1_455 ?
N1 K1 N8 87.21(8) . 6_556 ?
N2 K1 N8 89.72(8) 1_455 6_556 ?
N4 K1 N8 146.60(8) 5_666 6_556 ?
N6 K1 N8 99.49(8) 8_755 6_556 ?
N5 K1 N8 80.26(8) 1_455 6_556 ?
N1 K1 K2 50.42(6) . 5_666 ?
N2 K1 K2 141.98(6) 1_455 5_666 ?
N4 K1 K2 47.31(5) 5_666 5_666 ?
N6 K1 K2 110.20(6) 8_755 5_666 ?
N5 K1 K2 51.05(6) 1_455 5_666 ?
N8 K1 K2 121.57(6) 6_556 5_666 ?
N1 K1 K2 123.55(6) . 8_655 ?
N2 K1 K2 41.66(6) 1_455 8_655 ?
N4 K1 K2 104.03(6) 5_666 8_655 ?
N6 K1 K2 40.95(5) 8_755 8_655 ?
N5 K1 K2 166.31(6) 1_455 8_655 ?
N8 K1 K2 101.14(6) 6_556 8_655 ?
K2 K1 K2 134.117(19) 5_666 8_655 ?
C1 N1 K1 148.6(2) . . ?
C1 N1 K2 106.9(2) . 5_666 ?
K1 N1 K2 84.03(8) . 5_666 ?
N1 C1 B1 175.8(3) . . ?
N1 C1 K2 55.1(2) . 5_666 ?
B1 C1 K2 121.48(18) . 5_666 ?
C1 B1 C3 105.7(2) . . ?
C1 B1 C2 110.3(2) . . ?
C3 B1 C2 107.7(2) . . ?
C1 B1 C7 112.9(2) . . ?
C3 B1 C7 111.9(2) . . ?
C2 B1 C7 108.2(2) . . ?
N3 K2 N6 91.42(10) . 1_455 ?
N3 K2 N4 110.62(10) . . ?
N6 K2 N4 156.46(8) 1_455 . ?
N3 K2 N2 162.15(9) . 8_765 ?
N6 K2 N2 81.15(7) 1_455 8_765 ?
N4 K2 N2 75.37(8) . 8_765 ?
N3 K2 N1 130.52(9) . 5_666 ?
N6 K2 N1 79.05(8) 1_455 5_666 ?
N4 K2 N1 91.96(8) . 5_666 ?
N2 K2 N1 64.16(8) 8_765 5_666 ?
N3 K2 N5 82.42(9) . 5_766 ?
N6 K2 N5 124.91(8) 1_455 5_766 ?
N4 K2 N5 68.36(8) . 5_766 ?
N2 K2 N5 115.15(8) 8_765 5_766 ?
N1 K2 N5 65.43(8) 5_666 5_766 ?
N3 K2 N7 70.22(9) . 6_556 ?
N6 K2 N7 87.02(8) 1_455 6_556 ?
N4 K2 N7 92.62(8) . 6_556 ?
N2 K2 N7 93.08(8) 8_765 6_556 ?
N1 K2 N7 154.73(8) 5_666 6_556 ?
N5 K2 N7 138.74(8) 5_766 6_556 ?
N3 K2 C1 116.09(9) . 5_666 ?
N6 K2 C1 65.91(7) 1_455 5_666 ?
N4 K2 C1 108.91(7) . 5_666 ?
N2 K2 C1 75.69(7) 8_765 5_666 ?
N1 K2 C1 18.03(7) 5_666 5_666 ?
N5 K2 C1 68.33(7) 5_766 5_666 ?
N7 K2 C1 151.78(7) 6_556 5_666 ?
N3 K2 K1 129.14(8) . 5_666 ?
N6 K2 K1 123.65(6) 1_455 5_666 ?
N4 K2 K1 47.36(5) . 5_666 ?
N2 K2 K1 67.63(5) 8_765 5_666 ?
N1 K2 K1 45.55(6) 5_666 5_666 ?
N5 K2 K1 48.08(5) 5_766 5_666 ?
N7 K2 K1 137.90(6) 6_556 5_666 ?
C1 K2 K1 61.66(5) 5_666 5_666 ?
N3 K2 K1 131.95(8) . 8_665 ?
N6 K2 K1 41.12(5) 1_455 8_665 ?
N4 K2 K1 115.67(6) . 8_665 ?
N2 K2 K1 40.53(5) 8_765 8_665 ?
N1 K2 K1 60.75(6) 5_666 8_665 ?
N5 K2 K1 126.07(6) 5_766 8_665 ?
N7 K2 K1 95.05(5) 6_556 8_665 ?
C1 K2 K1 59.57(5) 5_666 8_665 ?
K1 K2 K1 92.904(15) 5_666 8_665 ?
C2 N2 K1 133.8(2) . 1_655 ?
C2 N2 K2 127.7(2) . 8_755 ?
K1 N2 K2 97.81(8) 1_655 8_755 ?
N2 C2 B1 176.9(3) . . ?
C6 B2 C5 107.4(2) . . ?
C6 B2 C4 107.7(2) . . ?
C5 B2 C4 106.4(2) . . ?
C6 B2 C12 113.1(3) . . ?
C5 B2 C12 112.3(2) . . ?
C4 B2 C12 109.5(2) . . ?
C3 N3 K2 166.9(3) . . ?
N3 C3 B1 177.9(4) . . ?
C4 N4 K2 140.9(2) . . ?
C4 N4 K1 126.1(2) . 5_666 ?
K2 N4 K1 85.33(7) . 5_666 ?
N4 C4 B2 179.0(3) . . ?
C5 N5 K1 148.4(3) . 1_655 ?
C5 N5 K2 130.6(2) . 5_766 ?
K1 N5 K2 80.87(7) 1_655 5_766 ?
N5 C5 B2 177.5(3) . . ?
C6 N6 K2 131.0(2) . 1_655 ?
C6 N6 K1 124.1(2) . 8_765 ?
K2 N6 K1 97.93(8) 1_655 8_765 ?
N6 C6 B2 179.0(3) . . ?
C14 N7 C16 115.3(3) . . ?
C14 N7 K2 109.5(2) . 6_656 ?
C16 N7 K2 135.1(2) . 6_656 ?
C10 C7 C8 114.1(3) . . ?
C10 C7 B1 124.8(3) . . ?
C8 C7 B1 121.1(3) . . ?
F5 C8 C9 118.6(3) . . ?
F5 C8 C7 120.1(3) . . ?
C9 C8 C7 121.4(3) . . ?
C11 N8 C9 115.8(3) . . ?
C11 N8 K1 114.7(2) . 6_656 ?
C9 N8 K1 129.3(2) . 6_656 ?
N8 C9 F6 117.1(3) . . ?
N8 C9 C8 123.6(3) . . ?
F6 C9 C8 119.3(3) . . ?
F8 C10 C11 117.5(3) . . ?
F8 C10 C7 122.2(3) . . ?
C11 C10 C7 120.3(3) . . ?
N8 C11 F7 116.3(3) . . ?
N8 C11 C10 124.8(3) . . ?
F7 C11 C10 118.9(3) . . ?
C13 C12 C15 113.2(3) . . ?
C13 C12 B2 126.0(3) . . ?
C15 C12 B2 120.7(3) . . ?
F1 C13 C14 116.7(3) . . ?
F1 C13 C12 122.3(3) . . ?
C14 C13 C12 121.0(3) . . ?
N7 C14 F2 115.7(3) . . ?
N7 C14 C13 124.9(3) . . ?
F2 C14 C13 119.4(3) . . ?
F4 C15 C16 118.8(3) . . ?
F4 C15 C12 119.6(3) . . ?
C16 C15 C12 121.6(3) . . ?
N7 C16 F3 116.1(3) . . ?
N7 C16 C15 124.0(3) . . ?
F3 C16 C15 120.0(3) . . ?

_refine_diff_density_max         1.293
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.085

####################################################################### 
# 
# 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_JL090_JL_KB2a
_database_code_depnum_ccdc_archive 'CCDC 1548900'
_audit_update_record             
;
2017-05-09 deposited with the CCDC.
2017-06-26 downloaded from the CCDC.
;


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

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H8 B2 F2 K2 N6'
_chemical_formula_sum            'C18 H8 B2 F2 K2 N6'
_chemical_formula_weight         446.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
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'

_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                   9.0844(6)
_cell_length_b                   9.8593(6)
_cell_length_c                   12.0751(8)
_cell_angle_alpha                91.429(2)
_cell_angle_beta                 109.254(2)
_cell_angle_gamma                90.945(2)
_cell_volume                     1020.35(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6831
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      26.76
_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).
;

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_F_000             448
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.499
_shelx_estimated_absorpt_T_min   0.894
_shelx_estimated_absorpt_T_max   0.943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7026
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13952
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_av_R_equivalents  0.0311
_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       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.376
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        26.000
_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             4180
_reflns_number_gt                3639
_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. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0253P)²+0.5235P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4180
_refine_ls_number_parameters     303
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0272
_refine_ls_wR_factor_ref         0.0677
_refine_ls_wR_factor_gt          0.0645
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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
N1 N 0.77163(15) 0.45306(14) 0.28268(11) 0.0188(3) Uani 1 1 d . . . . .
C1 C 0.64062(17) 0.42855(15) 0.24286(12) 0.0122(3) Uani 1 1 d . . . . .
B1 B 0.45867(18) 0.38917(16) 0.18392(14) 0.0109(3) Uani 1 1 d . . . . .
F1 F 0.41654(11) 0.61792(9) 0.31746(9) 0.0240(2) Uani 1 1 d . . . . .
K1 K 0.36334(4) 0.85595(3) 0.07365(3) 0.01431(8) Uani 1 1 d . . . . .
F2 F 0.25068(10) 0.90381(10) 0.24427(8) 0.0207(2) Uani 1 1 d . . . . .
K2 K 0.97824(3) 0.40783(3) 0.15536(3) 0.01174(8) Uani 1 1 d . . . . .
N2 N 0.43772(16) 0.13809(13) 0.07571(12) 0.0191(3) Uani 1 1 d . . . . .
C2 C 0.44677(16) 0.24401(15) 0.11888(12) 0.0126(3) Uani 1 1 d . . . . .
B2 B -0.07251(19) 0.86734(17) 0.21634(14) 0.0121(3) Uani 1 1 d . . . . .
C5 C 0.35203(17) 0.50077(15) 0.33998(13) 0.0144(3) Uani 1 1 d . . . . .
C4 C 0.36765(15) 0.38395(14) 0.27882(12) 0.0100(3) Uani 1 1 d . . . . .
C3 C 0.38131(16) 0.49848(14) 0.08709(12) 0.0111(3) Uani 1 1 d . . . . .
N3 N 0.32114(14) 0.57781(13) 0.02079(11) 0.0154(3) Uani 1 1 d . . . . .
C6 C 0.27574(18) 0.50616(17) 0.42137(14) 0.0184(3) Uani 1 1 d . . . . .
H6 H 0.270(2) 0.5900(19) 0.4598(16) 0.023(5) Uiso 1 1 d . . . . .
C7 C 0.21130(18) 0.38687(16) 0.44609(13) 0.0174(3) Uani 1 1 d . . . . .
H7 H 0.155(2) 0.3883(19) 0.5038(17) 0.028(5) Uiso 1 1 d . . . . .
C8 C 0.22316(17) 0.26678(16) 0.38792(13) 0.0154(3) Uani 1 1 d . . . . .
H8 H 0.182(2) 0.1830(19) 0.4051(15) 0.020(4) Uiso 1 1 d . . . . .
C9 C 0.29981(16) 0.26587(15) 0.30507(12) 0.0116(3) Uani 1 1 d . . . . .
H9 H 0.3108(17) 0.1765(16) 0.2662(13) 0.008(4) Uiso 1 1 d . . . . .
C11 C -0.04867(17) 0.75698(15) 0.12422(13) 0.0134(3) Uani 1 1 d . . . . .
N11 N -0.02772(16) 0.67608(13) 0.06183(11) 0.0184(3) Uani 1 1 d . . . . .
C12 C -0.08058(16) 1.01493(15) 0.16160(12) 0.0126(3) Uani 1 1 d . . . . .
N12 N -0.08802(15) 1.12323(13) 0.12784(11) 0.0186(3) Uani 1 1 d . . . . .
C13 C -0.23773(17) 0.83976(15) 0.23266(13) 0.0147(3) Uani 1 1 d . . . . .
N13 N -0.35589(15) 0.82569(15) 0.24643(12) 0.0243(3) Uani 1 1 d . . . . .
C14 C 0.06701(16) 0.86493(14) 0.34029(12) 0.0105(3) Uani 1 1 d . . . . .
C15 C 0.22108(17) 0.88232(14) 0.34739(13) 0.0130(3) Uani 1 1 d . . . . .
C16 C 0.34769(18) 0.88145(16) 0.44892(14) 0.0184(3) Uani 1 1 d . . . . .
H16 H 0.451(2) 0.8913(18) 0.4452(15) 0.020(4) Uiso 1 1 d . . . . .
C17 C 0.31781(19) 0.86523(16) 0.55350(14) 0.0200(3) Uani 1 1 d . . . . .
H17 H 0.400(2) 0.8661(18) 0.6246(16) 0.023(5) Uiso 1 1 d . . . . .
C18 C 0.16605(19) 0.84766(16) 0.55284(14) 0.0189(3) Uani 1 1 d . . . . .
H18 H 0.145(2) 0.8364(19) 0.6265(17) 0.029(5) Uiso 1 1 d . . . . .
C19 C 0.04307(18) 0.84655(15) 0.44753(13) 0.0139(3) Uani 1 1 d . . . . .
H19 H -0.062(2) 0.8355(17) 0.4457(15) 0.019(4) Uiso 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
N1 C1 1.1460(19) . ?
N1 K2 2.8252(13) . ?
C1 B1 1.606(2) . ?
B1 C2 1.600(2) . ?
B1 C3 1.603(2) . ?
B1 C4 1.620(2) . ?
F1 C5 1.3601(16) . ?
K1 F2 2.6217(9) . ?
K1 N13 2.7376(14) 1_655 ?
K1 N3 2.7912(13) . ?
K1 N2 2.8494(14) 1_565 ?
K1 N12 2.8716(13) 2_575 ?
K1 N2 2.9451(13) 2_665 ?
K1 C12 3.4299(14) 2_575 ?
K1 C2 3.4551(14) 2_665 ?
K1 C13 3.5058(15) 1_655 ?
K1 C3 3.5361(15) . ?
K1 K2 4.2136(5) 2_665 ?
K1 K1 4.5088(7) 2_675 ?
F2 C15 1.3783(16) . ?
K2 N12 2.8482(13) 1_645 ?
K2 N3 2.8554(13) 2_665 ?
K2 N11 2.8959(13) 1_655 ?
K2 N11 2.9062(14) 2_665 ?
K2 C9 3.2464(14) 1_655 ?
K2 C8 3.3086(15) 1_655 ?
K2 C4 3.3703(14) 1_655 ?
K2 C7 3.4639(16) 1_655 ?
K2 C11 3.4760(15) 1_655 ?
K2 C5 3.4847(15) 1_655 ?
K2 K1 4.2137(5) 2_665 ?
N2 C2 1.145(2) . ?
N2 K1 2.8494(14) 1_545 ?
N2 K1 2.9451(13) 2_665 ?
C2 K1 3.4551(14) 2_665 ?
B2 C13 1.597(2) . ?
B2 C11 1.604(2) . ?
B2 C12 1.606(2) . ?
B2 C14 1.612(2) . ?
C5 C6 1.377(2) . ?
C5 C4 1.387(2) . ?
C5 K2 3.4847(15) 1_455 ?
C4 C9 1.400(2) . ?
C4 K2 3.3703(14) 1_455 ?
C3 N3 1.1437(19) . ?
N3 K2 2.8554(13) 2_665 ?
C6 C7 1.387(2) . ?
C6 H6 0.948(19) . ?
C7 C8 1.385(2) . ?
C7 K2 3.4638(16) 1_455 ?
C7 H7 0.994(19) . ?
C8 C9 1.395(2) . ?
C8 K2 3.3085(15) 1_455 ?
C8 H8 0.958(18) . ?
C9 K2 3.2464(14) 1_455 ?
C9 H9 1.010(16) . ?
C11 N11 1.144(2) . ?
C11 K2 3.4761(15) 1_455 ?
N11 K2 2.8959(13) 1_455 ?
N11 K2 2.9062(14) 2_665 ?
C12 N12 1.1475(19) . ?
C12 K1 3.4299(14) 2_575 ?
N12 K2 2.8482(13) 1_465 ?
N12 K1 2.8716(13) 2_575 ?
C13 N13 1.146(2) . ?
C13 K1 3.5058(15) 1_455 ?
N13 K1 2.7375(14) 1_455 ?
C14 C15 1.381(2) . ?
C14 C19 1.397(2) . ?
C15 C16 1.377(2) . ?
C16 C17 1.389(2) . ?
C16 H16 0.954(18) . ?
C17 C18 1.384(2) . ?
C17 H17 0.933(19) . ?
C18 C19 1.388(2) . ?
C18 H18 0.977(19) . ?
C19 H19 0.953(17) . ?

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
C1 N1 K2 121.85(11) . . ?
N1 C1 B1 177.62(16) . . ?
C2 B1 C3 108.35(12) . . ?
C2 B1 C1 107.37(12) . . ?
C3 B1 C1 108.25(12) . . ?
C2 B1 C4 110.08(12) . . ?
C3 B1 C4 109.94(11) . . ?
C1 B1 C4 112.72(12) . . ?
F2 K1 N13 86.13(4) . 1_655 ?
F2 K1 N3 106.40(3) . . ?
N13 K1 N3 93.30(4) 1_655 . ?
F2 K1 N2 89.07(3) . 1_565 ?
N13 K1 N2 88.52(4) 1_655 1_565 ?
N3 K1 N2 164.50(4) . 1_565 ?
F2 K1 N12 101.00(4) . 2_575 ?
N13 K1 N12 172.83(4) 1_655 2_575 ?
N3 K1 N12 83.99(4) . 2_575 ?
N2 K1 N12 92.35(4) 1_565 2_575 ?
F2 K1 N2 162.63(4) . 2_665 ?
N13 K1 N2 82.21(4) 1_655 2_665 ?
N3 K1 N2 87.15(4) . 2_665 ?
N2 K1 N2 77.84(4) 1_565 2_665 ?
N12 K1 N2 91.01(4) 2_575 2_665 ?
F2 K1 C12 101.72(3) . 2_575 ?
N13 K1 C12 160.58(4) 1_655 2_575 ?
N3 K1 C12 101.30(4) . 2_575 ?
N2 K1 C12 74.03(4) 1_565 2_575 ?
N12 K1 C12 18.38(4) 2_575 2_575 ?
N2 K1 C12 85.76(4) 2_665 2_575 ?
F2 K1 C2 170.31(3) . 2_665 ?
N13 K1 C2 85.78(4) 1_655 2_665 ?
N3 K1 C2 68.78(4) . 2_665 ?
N2 K1 C2 96.04(4) 1_565 2_665 ?
N12 K1 C2 87.05(4) 2_575 2_665 ?
N2 K1 C2 18.49(4) 2_665 2_665 ?
C12 K1 C2 87.63(3) 2_575 2_665 ?
F2 K1 C13 100.58(3) . 1_655 ?
N13 K1 C13 15.77(4) 1_655 1_655 ?
N3 K1 C13 95.16(4) . 1_655 ?
N2 K1 C13 82.54(4) 1_565 1_655 ?
N12 K1 C13 157.72(4) 2_575 1_655 ?
N2 K1 C13 66.73(4) 2_665 1_655 ?
C12 K1 C13 147.14(4) 2_575 1_655 ?
C2 K1 C13 72.05(4) 2_665 1_655 ?
F2 K1 C3 98.90(3) . . ?
N13 K1 C3 78.73(4) 1_655 . ?
N3 K1 C3 15.88(3) . . ?
N2 K1 C3 164.40(4) 1_565 . ?
N12 K1 C3 99.20(4) 2_575 . ?
N2 K1 C3 91.42(3) 2_665 . ?
C12 K1 C3 116.88(3) 2_575 . ?
C2 K1 C3 74.27(3) 2_665 . ?
C13 K1 C3 82.82(3) 1_655 . ?
F2 K1 K2 102.69(2) . 2_665 ?
N13 K1 K2 135.58(3) 1_655 2_665 ?
N3 K1 K2 42.32(3) . 2_665 ?
N2 K1 K2 134.36(3) 1_565 2_665 ?
N12 K1 K2 42.33(3) 2_575 2_665 ?
N2 K1 K2 94.64(3) 2_665 2_665 ?
C12 K1 K2 60.46(3) 2_575 2_665 ?
C2 K1 K2 79.56(3) 2_665 2_665 ?
C13 K1 K2 135.91(3) 1_655 2_665 ?
C3 K1 K2 56.98(2) . 2_665 ?
F2 K1 K1 127.82(2) . 2_675 ?
N13 K1 K1 83.98(3) 1_655 2_675 ?
N3 K1 K1 125.20(3) . 2_675 ?
N2 K1 K1 39.68(3) 1_565 2_675 ?
N12 K1 K1 92.15(3) 2_575 2_675 ?
N2 K1 K1 38.15(3) 2_665 2_675 ?
C12 K1 K1 77.16(3) 2_575 2_675 ?
C2 K1 K1 56.43(3) 2_665 2_675 ?
C13 K1 K1 70.11(3) 1_655 2_675 ?
C3 K1 K1 128.67(3) . 2_675 ?
K2 K1 K1 119.646(12) 2_665 2_675 ?
C15 F2 K1 157.49(8) . . ?
N1 K2 N12 93.59(4) . 1_645 ?
N1 K2 N3 75.63(4) . 2_665 ?
N12 K2 N3 83.26(4) 1_645 2_665 ?
N1 K2 N11 97.96(4) . 1_655 ?
N12 K2 N11 151.91(4) 1_645 1_655 ?
N3 K2 N11 75.03(4) 2_665 1_655 ?
N1 K2 N11 149.35(4) . 2_665 ?
N12 K2 N11 74.06(4) 1_645 2_665 ?
N3 K2 N11 75.13(4) 2_665 2_665 ?
N11 K2 N11 83.18(4) 1_655 2_665 ?
N1 K2 C9 113.94(4) . 1_655 ?
N12 K2 C9 74.42(4) 1_645 1_655 ?
N3 K2 C9 156.00(4) 2_665 1_655 ?
N11 K2 C9 122.63(4) 1_655 1_655 ?
N11 K2 C9 90.09(4) 2_665 1_655 ?
N1 K2 C8 89.42(4) . 1_655 ?
N12 K2 C8 73.32(4) 1_645 1_655 ?
N3 K2 C8 151.38(4) 2_665 1_655 ?
N11 K2 C8 132.02(4) 1_655 1_655 ?
N11 K2 C8 112.62(4) 2_665 1_655 ?
C9 K2 C8 24.55(4) 1_655 1_655 ?
N1 K2 C4 124.29(4) . 1_655 ?
N12 K2 C4 96.08(4) 1_645 1_655 ?
N3 K2 C4 160.00(4) 2_665 1_655 ?
N11 K2 C4 98.33(4) 1_655 1_655 ?
N11 K2 C4 85.44(4) 2_665 1_655 ?
C9 K2 C4 24.33(3) 1_655 1_655 ?
C8 K2 C4 42.87(3) 1_655 1_655 ?
N1 K2 C7 75.94(4) . 1_655 ?
N12 K2 C7 93.44(4) 1_645 1_655 ?
N3 K2 C7 151.10(4) 2_665 1_655 ?
N11 K2 C7 114.15(4) 1_655 1_655 ?
N11 K2 C7 131.60(4) 2_665 1_655 ?
C9 K2 C7 41.92(4) 1_655 1_655 ?
C8 K2 C7 23.46(4) 1_655 1_655 ?
C4 K2 C7 48.83(3) 1_655 1_655 ?
N1 K2 C11 82.47(4) . 1_655 ?
N12 K2 C11 162.92(4) 1_645 1_655 ?
N3 K2 C11 79.66(4) 2_665 1_655 ?
N11 K2 C11 17.88(3) 1_655 1_655 ?
N11 K2 C11 101.06(4) 2_665 1_655 ?
C9 K2 C11 122.38(4) 1_655 1_655 ?
C8 K2 C11 123.04(4) 1_655 1_655 ?
C4 K2 C11 99.87(3) 1_655 1_655 ?
C7 K2 C11 101.63(4) 1_655 1_655 ?
N1 K2 C5 107.35(4) . 1_655 ?
N12 K2 C5 115.11(4) 1_645 1_655 ?
N3 K2 C5 160.72(4) 2_665 1_655 ?
N11 K2 C5 85.69(4) 1_655 1_655 ?
N11 K2 C5 103.28(4) 2_665 1_655 ?
C9 K2 C5 40.78(4) 1_655 1_655 ?
C8 K2 C5 47.30(4) 1_655 1_655 ?
C4 K2 C5 23.27(3) 1_655 1_655 ?
C7 K2 C5 39.98(3) 1_655 1_655 ?
C11 K2 C5 81.86(3) 1_655 1_655 ?
N1 K2 K1 88.33(3) . 2_665 ?
N12 K2 K1 42.77(3) 1_645 2_665 ?
N3 K2 K1 41.16(3) 2_665 2_665 ?
N11 K2 K1 111.89(3) 1_655 2_665 ?
N11 K2 K1 63.39(3) 2_665 2_665 ?
C9 K2 K1 115.25(3) 1_655 2_665 ?
C8 K2 K1 115.68(3) 1_655 2_665 ?
C4 K2 K1 132.07(3) 1_655 2_665 ?
C7 K2 K1 132.84(3) 1_655 2_665 ?
C11 K2 K1 120.27(3) 1_655 2_665 ?
C5 K2 K1 154.99(3) 1_655 2_665 ?
C2 N2 K1 149.29(11) . 1_545 ?
C2 N2 K1 106.84(10) . 2_665 ?
K1 N2 K1 102.16(4) 1_545 2_665 ?
N2 C2 B1 177.62(15) . . ?
N2 C2 K1 54.67(9) . 2_665 ?
B1 C2 K1 127.31(9) . 2_665 ?
C13 B2 C11 109.17(12) . . ?
C13 B2 C12 106.17(12) . . ?
C11 B2 C12 108.74(12) . . ?
C13 B2 C14 111.11(12) . . ?
C11 B2 C14 111.40(12) . . ?
C12 B2 C14 110.09(12) . . ?
F1 C5 C6 118.00(13) . . ?
F1 C5 C4 117.43(12) . . ?
C6 C5 C4 124.57(14) . . ?
F1 C5 K2 117.44(9) . 1_455 ?
C6 C5 K2 81.34(9) . 1_455 ?
C4 C5 K2 73.73(8) . 1_455 ?
C5 C4 C9 115.41(13) . . ?
C5 C4 B1 120.56(12) . . ?
C9 C4 B1 124.02(13) . . ?
C5 C4 K2 83.00(8) . 1_455 ?
C9 C4 K2 72.87(8) . 1_455 ?
B1 C4 K2 112.91(8) . 1_455 ?
N3 C3 B1 176.69(15) . . ?
N3 C3 K1 41.89(8) . . ?
B1 C3 K1 137.13(9) . . ?
C3 N3 K1 122.23(11) . . ?
C3 N3 K2 134.26(11) . 2_665 ?
K1 N3 K2 96.52(4) . 2_665 ?
C5 C6 C7 118.44(14) . . ?
C5 C6 H6 119.7(11) . . ?
C7 C6 H6 121.9(11) . . ?
C8 C7 C6 119.71(14) . . ?
C8 C7 K2 71.97(9) . 1_455 ?
C6 C7 K2 82.05(9) . 1_455 ?
C8 C7 H7 120.3(11) . . ?
C6 C7 H7 120.0(11) . . ?
K2 C7 H7 115.1(11) 1_455 . ?
C7 C8 C9 120.11(14) . . ?
C7 C8 K2 84.57(9) . 1_455 ?
C9 C8 K2 75.23(8) . 1_455 ?
C7 C8 H8 121.0(11) . . ?
C9 C8 H8 118.9(11) . . ?
K2 C8 H8 111.8(10) 1_455 . ?
C8 C9 C4 121.76(14) . . ?
C8 C9 K2 80.22(9) . 1_455 ?
C4 C9 K2 82.80(8) . 1_455 ?
C8 C9 H9 118.7(9) . . ?
C4 C9 H9 119.5(9) . . ?
K2 C9 H9 110.3(9) 1_455 . ?
N11 C11 B2 177.51(15) . . ?
N11 C11 K2 51.00(9) . 1_455 ?
B2 C11 K2 127.23(9) . 1_455 ?
C11 N11 K2 111.11(10) . 1_455 ?
C11 N11 K2 152.06(11) . 2_665 ?
K2 N11 K2 96.82(4) 1_455 2_665 ?
N12 C12 B2 176.21(15) . . ?
N12 C12 K1 52.10(9) . 2_575 ?
B2 C12 K1 129.14(9) . 2_575 ?
C12 N12 K2 153.33(11) . 1_465 ?
C12 N12 K1 109.52(11) . 2_575 ?
K2 N12 K1 94.90(4) 1_465 2_575 ?
N13 C13 B2 176.97(16) . . ?
N13 C13 K1 40.50(9) . 1_455 ?
B2 C13 K1 139.81(9) . 1_455 ?
C13 N13 K1 123.73(12) . 1_455 ?
C15 C14 C19 115.02(13) . . ?
C15 C14 B2 121.45(12) . . ?
C19 C14 B2 123.52(13) . . ?
C16 C15 F2 117.16(13) . . ?
C16 C15 C14 125.57(14) . . ?
F2 C15 C14 117.27(12) . . ?
C15 C16 C17 117.27(14) . . ?
C15 C16 H16 119.8(11) . . ?
C17 C16 H16 122.9(11) . . ?
C18 C17 C16 120.18(14) . . ?
C18 C17 H17 119.6(11) . . ?
C16 C17 H17 120.2(11) . . ?
C17 C18 C19 120.05(14) . . ?
C17 C18 H18 120.1(11) . . ?
C19 C18 H18 119.9(11) . . ?
C18 C19 C14 121.88(14) . . ?
C18 C19 H19 121.0(11) . . ?
C14 C19 H19 117.1(11) . . ?

_refine_diff_density_max         0.327
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.048

####################################################################### 
# 
# 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_JL084_JL_KB3d
_database_code_depnum_ccdc_archive 'CCDC 1548904'
_audit_update_record             
;
2017-05-09 deposited with the CCDC.
2017-06-26 downloaded from the CCDC.
;


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

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H3 B F2 K N3'
_chemical_formula_sum            'C9 H3 B F2 K N3'
_chemical_formula_weight         241.05

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'
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'

_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                   11.1415(11)
_cell_length_b                   12.3048(12)
_cell_length_c                   7.4382(7)
_cell_angle_alpha                90
_cell_angle_beta                 99.762(3)
_cell_angle_gamma                90
_cell_volume                     1004.97(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2924
_cell_measurement_theta_min      3.31
_cell_measurement_theta_max      26.41

_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).
;

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_F_000             480
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.527
_shelx_estimated_absorpt_T_min   0.797
_shelx_estimated_absorpt_T_max   0.902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6667
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9084
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.855
_diffrn_reflns_theta_max         26.811
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2139
_reflns_number_gt                1779
_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. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0411P)²+0.2526P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2139
_refine_ls_number_parameters     157
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0317
_refine_ls_wR_factor_ref         0.0835
_refine_ls_wR_factor_gt          0.0780
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_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 1.13068(3) 0.65458(3) 0.03236(5) 0.01263(12) Uani 1 1 d . . . . .
B1 B 0.81279(17) 0.57777(15) 0.4672(3) 0.0110(4) Uani 1 1 d . . . . .
H1 H 0.7788(17) 0.7943(15) 0.507(3) 0.012(5) Uiso 1 1 d . . . . .
F1 F 0.61075(10) 0.93488(8) 0.46213(16) 0.0245(3) Uani 1 1 d . . . . .
N1 N 0.90089(13) 0.55910(11) 0.8333(2) 0.0150(3) Uani 1 1 d . . . . .
C1 C 0.86433(14) 0.56572(13) 0.6804(2) 0.0111(4) Uani 1 1 d . . . . .
N2 N 0.98967(13) 0.68020(12) 0.3118(2) 0.0144(3) Uani 1 1 d . . . . .
H2 H 0.411(2) 0.8300(18) 0.356(3) 0.033(6) Uiso 1 1 d . . . . .
F2 F 0.36146(9) 0.63158(10) 0.29077(17) 0.0286(3) Uani 1 1 d . . . . .
C2 C 0.91634(14) 0.63728(13) 0.3766(2) 0.0110(3) Uani 1 1 d . . . . .
N3 N 0.79157(13) 0.37288(12) 0.3180(2) 0.0149(3) Uani 1 1 d . . . . .
H3 H 0.5602(18) 0.5321(17) 0.347(3) 0.022(5) Uiso 1 1 d . . . . .
C3 C 0.79732(14) 0.45844(13) 0.3805(2) 0.0109(4) Uani 1 1 d . . . . .
C4 C 0.68959(14) 0.64961(13) 0.4343(2) 0.0102(3) Uani 1 1 d . . . . .
C5 C 0.70054(15) 0.76165(14) 0.4649(2) 0.0126(4) Uani 1 1 d . . . . .
C6 C 0.59815(16) 0.82584(14) 0.4348(3) 0.0156(4) Uani 1 1 d . . . . .
C8 C 0.47490(15) 0.67463(16) 0.3498(3) 0.0178(4) Uani 1 1 d . . . . .
C7 C 0.48285(16) 0.78540(16) 0.3772(3) 0.0190(4) Uani 1 1 d . . . . .
C9 C 0.57378(15) 0.60547(15) 0.3765(2) 0.0139(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 N2 2.8277(15) . ?
K1 N1 2.8557(15) 3_766 ?
K1 N2 2.9014(15) 4_575 ?
K1 N3 2.9019(16) 3_765 ?
K1 F2 2.9513(12) 1_655 ?
K1 N1 2.9736(15) 1_554 ?
K1 N3 2.9796(15) 2_755 ?
K1 C1 3.4461(17) 3_766 ?
K1 K1 4.3984(5) 4_576 ?
K1 K1 4.3984(5) 4_575 ?
K1 K1 4.7653(8) 3_765 ?
B1 C1 1.600(3) . ?
B1 C3 1.601(2) . ?
B1 C2 1.608(3) . ?
B1 C4 1.616(2) . ?
F1 C6 1.3607(19) . ?
N1 C1 1.144(2) . ?
N1 K1 2.8557(15) 3_766 ?
N1 K1 2.9736(15) 1_556 ?
C1 K1 3.4461(17) 3_766 ?
N2 C2 1.145(2) . ?
N2 K1 2.9015(15) 4_576 ?
F2 C8 1.372(2) . ?
F2 K1 2.9513(11) 1_455 ?
N3 C3 1.148(2) . ?
N3 K1 2.9019(16) 3_765 ?
N3 K1 2.9796(15) 2_745 ?
C4 C9 1.399(2) . ?
C4 C5 1.399(2) . ?
C5 C6 1.374(2) . ?
C5 H1 0.963(18) . ?
C6 C7 1.376(3) . ?
C8 C7 1.379(3) . ?
C8 C9 1.379(2) . ?
C7 H2 0.96(2) . ?
C9 H3 0.94(2) . ?

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
N2 K1 N1 74.25(4) . 3_766 ?
N2 K1 N2 91.28(4) . 4_575 ?
N1 K1 N2 139.11(4) 3_766 4_575 ?
N2 K1 N3 163.90(4) . 3_765 ?
N1 K1 N3 106.28(4) 3_766 3_765 ?
N2 K1 N3 77.84(4) 4_575 3_765 ?
N2 K1 F2 93.62(4) . 1_655 ?
N1 K1 F2 80.17(4) 3_766 1_655 ?
N2 K1 F2 139.80(4) 4_575 1_655 ?
N3 K1 F2 102.35(4) 3_765 1_655 ?
N2 K1 N1 82.61(4) . 1_554 ?
N1 K1 N1 70.35(5) 3_766 1_554 ?
N2 K1 N1 69.96(4) 4_575 1_554 ?
N3 K1 N1 82.51(4) 3_765 1_554 ?
F2 K1 N1 150.22(4) 1_655 1_554 ?
N2 K1 N3 77.73(4) . 2_755 ?
N1 K1 N3 138.12(5) 3_766 2_755 ?
N2 K1 N3 71.02(4) 4_575 2_755 ?
N3 K1 N3 109.17(4) 3_765 2_755 ?
F2 K1 N3 71.16(4) 1_655 2_755 ?
N1 K1 N3 135.52(4) 1_554 2_755 ?
N2 K1 C1 65.45(4) . 3_766 ?
N1 K1 C1 17.97(4) 3_766 3_766 ?
N2 K1 C1 148.42(4) 4_575 3_766 ?
N3 K1 C1 119.30(4) 3_765 3_766 ?
F2 K1 C1 66.43(4) 1_655 3_766 ?
N1 K1 C1 85.41(4) 1_554 3_766 ?
N3 K1 C1 120.29(4) 2_755 3_766 ?
N2 K1 K1 40.47(3) . 4_576 ?
N1 K1 K1 100.25(3) 3_766 4_576 ?
N2 K1 K1 91.51(3) 4_575 4_576 ?
N3 K1 K1 149.80(3) 3_765 4_576 ?
F2 K1 K1 68.00(2) 1_655 4_576 ?
N1 K1 K1 120.57(3) 1_554 4_576 ?
N3 K1 K1 40.93(3) 2_755 4_576 ?
C1 K1 K1 84.15(3) 3_766 4_576 ?
N2 K1 K1 129.92(3) . 4_575 ?
N1 K1 K1 143.62(3) 3_766 4_575 ?
N2 K1 K1 39.24(3) 4_575 4_575 ?
N3 K1 K1 42.27(3) 3_765 4_575 ?
F2 K1 K1 118.49(2) 1_655 4_575 ?
N1 K1 K1 85.03(3) 1_554 4_575 ?
N3 K1 K1 78.05(3) 2_755 4_575 ?
C1 K1 K1 160.37(3) 3_766 4_575 ?
K1 K1 K1 115.463(17) 4_576 4_575 ?
N2 K1 K1 75.94(3) . 3_765 ?
N1 K1 K1 35.99(3) 3_766 3_765 ?
N2 K1 K1 103.84(3) 4_575 3_765 ?
N3 K1 K1 94.97(3) 3_765 3_765 ?
F2 K1 K1 116.06(3) 1_655 3_765 ?
N1 K1 K1 34.36(3) 1_554 3_765 ?
N3 K1 K1 153.05(3) 2_755 3_765 ?
C1 K1 K1 51.69(3) 3_766 3_765 ?
K1 K1 K1 115.088(10) 4_576 3_765 ?
K1 K1 K1 115.367(10) 4_575 3_765 ?
C1 B1 C3 108.07(14) . . ?
C1 B1 C2 107.18(13) . . ?
C3 B1 C2 106.54(14) . . ?
C1 B1 C4 110.72(14) . . ?
C3 B1 C4 114.21(14) . . ?
C2 B1 C4 109.81(14) . . ?
C1 N1 K1 111.66(12) . 3_766 ?
C1 N1 K1 126.75(12) . 1_556 ?
K1 N1 K1 109.65(5) 3_766 1_556 ?
N1 C1 B1 178.74(17) . . ?
N1 C1 K1 50.37(10) . 3_766 ?
B1 C1 K1 130.77(10) . 3_766 ?
C2 N2 K1 141.49(13) . . ?
C2 N2 K1 116.22(13) . 4_576 ?
K1 N2 K1 100.29(5) . 4_576 ?
C8 F2 K1 145.58(11) . 1_455 ?
N2 C2 B1 179.59(17) . . ?
C3 N3 K1 117.75(12) . 3_765 ?
C3 N3 K1 133.05(13) . 2_745 ?
K1 N3 K1 96.80(4) 3_765 2_745 ?
N3 C3 B1 177.01(16) . . ?
C9 C4 C5 118.88(15) . . ?
C9 C4 B1 123.35(15) . . ?
C5 C4 B1 117.77(15) . . ?
C6 C5 C4 119.51(16) . . ?
C6 C5 H1 119.6(11) . . ?
C4 C5 H1 120.9(11) . . ?
F1 C6 C5 118.72(16) . . ?
F1 C6 C7 118.04(15) . . ?
C5 C6 C7 123.24(17) . . ?
F2 C8 C7 117.48(16) . . ?
F2 C8 C9 118.54(16) . . ?
C7 C8 C9 123.97(17) . . ?
C6 C7 C8 115.88(16) . . ?
C6 C7 H2 123.7(13) . . ?
C8 C7 H2 120.4(13) . . ?
C8 C9 C4 118.51(17) . . ?
C8 C9 H3 117.9(12) . . ?
C4 C9 H3 123.5(12) . . ?

_refine_diff_density_max         0.374
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.064

####################################################################### 
# 
# 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_JL098_JL_KB11a
_database_code_depnum_ccdc_archive 'CCDC 1548909'
_audit_update_record             
;
2017-05-09 deposited with the CCDC.
2017-06-26 downloaded from the CCDC.
;


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

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 B2 F8 K2 N8'
_chemical_formula_sum            'C20 B2 F8 K2 N8'
_chemical_formula_weight         604.10

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'

_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                   9.8453(7)
_cell_length_b                   10.0627(7)
_cell_length_c                   13.4136(10)
_cell_angle_alpha                87.223(3)
_cell_angle_beta                 87.467(3)
_cell_angle_gamma                66.895(2)
_cell_volume                     1220.40(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3382
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      26.41
_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).
;

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.477
_shelx_estimated_absorpt_T_min   0.961
_shelx_estimated_absorpt_T_max   0.991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7004
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16011
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.202
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        26.000
_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             5004
_reflns_number_gt                3659
_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. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0251P)²+0.6674P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5004
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.0802
_refine_ls_wR_factor_gt          0.0721
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.74746(6) 0.60553(5) 0.06739(4) 0.01441(13) Uani 1 1 d . . . . .
N1 N 0.4711(2) 0.6022(2) 0.10686(16) 0.0255(5) Uani 1 1 d . . . . .
C1 C 0.3646(3) 0.6125(3) 0.14943(18) 0.0164(5) Uani 1 1 d . . . . .
B1 B 0.2127(3) 0.6427(3) 0.2093(2) 0.0156(6) Uani 1 1 d . . . . .
K2 K 0.11214(6) 0.20098(6) 0.15683(4) 0.01573(13) Uani 1 1 d . . . . .
N2 N 0.0722(2) 0.9386(2) 0.19712(16) 0.0231(5) Uani 1 1 d . . . . .
C2 C 0.1261(3) 0.8150(3) 0.20334(17) 0.0173(5) Uani 1 1 d . . . . .
B2 B 0.3141(3) -0.1231(3) 0.85154(19) 0.0114(5) Uani 1 1 d . . . . .
N3 N 0.0532(2) 0.5099(2) 0.12256(15) 0.0181(5) Uani 1 1 d . . . . .
C3 C 0.1186(3) 0.5683(2) 0.15625(17) 0.0139(5) Uani 1 1 d . . . . .
C11 C 0.2328(3) 0.5822(2) 0.32540(17) 0.0139(5) Uani 1 1 d . . . . .
C12 C 0.3633(3) 0.4832(3) 0.36588(17) 0.0154(5) Uani 1 1 d . . . . .
F12 F 0.48771(15) 0.42846(15) 0.30959(10) 0.0223(3) Uani 1 1 d . . . . .
C13 C 0.3726(3) 0.4382(2) 0.46489(18) 0.0170(5) Uani 1 1 d . . . . .
F13 F 0.50421(15) 0.34618(15) 0.49939(10) 0.0234(3) Uani 1 1 d . . . . .
C14 C 0.2514(3) 0.4885(3) 0.52981(17) 0.0184(5) Uani 1 1 d . . . . .
C15 C 0.1198(3) 0.5849(3) 0.49040(18) 0.0196(6) Uani 1 1 d . . . . .
F15 F -0.00167(16) 0.63654(15) 0.54989(11) 0.0275(4) Uani 1 1 d . . . . .
C16 C 0.1124(3) 0.6280(2) 0.39170(18) 0.0181(5) Uani 1 1 d . . . . .
F16 F -0.02089(15) 0.72085(15) 0.35823(10) 0.0239(3) Uani 1 1 d . . . . .
C17 C 0.2586(3) 0.4457(3) 0.63404(19) 0.0225(6) Uani 1 1 d . . . . .
N17 N 0.2604(3) 0.4143(3) 0.71712(16) 0.0303(6) Uani 1 1 d . . . . .
C21 C 0.4875(3) -0.1974(2) 0.87119(16) 0.0136(5) Uani 1 1 d . . . . .
N21 N 0.6124(2) -0.2456(2) 0.88295(15) 0.0197(5) Uani 1 1 d . . . . .
C22 C 0.2480(3) 0.0221(3) 0.91424(17) 0.0146(5) Uani 1 1 d . . . . .
N22 N 0.2043(2) 0.1259(2) 0.95796(15) 0.0194(5) Uani 1 1 d . . . . .
C23 C 0.2366(3) -0.2283(2) 0.89300(17) 0.0146(5) Uani 1 1 d . . . . .
N23 N 0.1808(2) -0.3028(2) 0.92286(15) 0.0192(5) Uani 1 1 d . . . . .
C31 C 0.2905(2) -0.0795(2) 0.73338(16) 0.0123(5) Uani 1 1 d . . . . .
C32 C 0.3529(3) 0.0129(2) 0.69069(17) 0.0144(5) Uani 1 1 d . . . . .
F32 F 0.42907(15) 0.06363(15) 0.74872(10) 0.0219(3) Uani 1 1 d . . . . .
C33 C 0.3408(3) 0.0554(2) 0.59167(18) 0.0164(5) Uani 1 1 d . . . . .
F33 F 0.40542(16) 0.14317(15) 0.55494(10) 0.0231(3) Uani 1 1 d . . . . .
C34 C 0.2620(3) 0.0094(3) 0.52838(17) 0.0163(5) Uani 1 1 d . . . . .
C35 C 0.1987(3) -0.0828(2) 0.56890(17) 0.0165(5) Uani 1 1 d . . . . .
C36 C 0.2142(3) -0.1259(2) 0.66801(17) 0.0144(5) Uani 1 1 d . . . . .
F36 F 0.15056(15) -0.21836(14) 0.69925(10) 0.0203(3) Uani 1 1 d . . . . .
C37 C 0.2484(3) 0.0557(3) 0.42588(18) 0.0187(5) Uani 1 1 d . . . . .
N37 N 0.2361(3) 0.0978(3) 0.34435(17) 0.0342(6) Uani 1 1 d . . . . .
F37 F 0.12342(16) -0.13162(15) 0.50935(10) 0.0250(3) 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 N1 2.762(2) . ?
K1 N23 2.842(2) 2_656 ?
K1 N17 2.887(2) 2_666 ?
K1 N3 2.897(2) 1_655 ?
K1 N21 2.915(2) 1_564 ?
K1 N22 2.924(2) 2_666 ?
K1 N3 3.122(2) 2_665 ?
K1 C3 3.485(2) 2_665 ?
K1 K2 3.9906(7) 2_665 ?
K1 K2 4.3975(8) 1_655 ?
K1 K1 4.8781(11) 2_765 ?
N1 C1 1.142(3) . ?
C1 B1 1.592(4) . ?
B1 C2 1.604(4) . ?
B1 C3 1.607(4) . ?
B1 C11 1.636(4) . ?
K2 N37 2.814(2) . ?
K2 N22 2.820(2) 1_554 ?
K2 N2 2.842(2) 1_545 ?
K2 N23 2.891(2) 2_556 ?
K2 N21 2.940(2) 2_656 ?
K2 N3 2.947(2) . ?
K2 F36 3.1118(15) 2_556 ?
K2 C23 3.429(2) 2_556 ?
K2 K1 3.9906(7) 2_665 ?
K2 K1 4.3975(8) 1_455 ?
N2 C2 1.145(3) . ?
N2 K2 2.841(2) 1_565 ?
B2 C23 1.598(3) . ?
B2 C21 1.601(4) . ?
B2 C22 1.609(3) . ?
B2 C31 1.626(3) . ?
N3 C3 1.145(3) . ?
N3 K1 2.897(2) 1_455 ?
N3 K1 3.122(2) 2_665 ?
C3 K1 3.485(2) 2_665 ?
C11 C16 1.388(3) . ?
C11 C12 1.393(3) . ?
C12 F12 1.343(3) . ?
C12 C13 1.377(3) . ?
C13 F13 1.349(3) . ?
C13 C14 1.384(3) . ?
C14 C15 1.387(4) . ?
C14 C17 1.439(3) . ?
C15 F15 1.343(3) . ?
C15 C16 1.369(3) . ?
C16 F16 1.358(3) . ?
C17 N17 1.142(3) . ?
N17 K1 2.887(2) 2_666 ?
C21 N21 1.146(3) . ?
N21 K1 2.915(2) 1_546 ?
N21 K2 2.940(2) 2_656 ?
C22 N22 1.142(3) . ?
N22 K2 2.820(2) 1_556 ?
N22 K1 2.924(2) 2_666 ?
C23 N23 1.139(3) . ?
C23 K2 3.429(2) 2_556 ?
N23 K1 2.842(2) 2_656 ?
N23 K2 2.891(2) 2_556 ?
C31 C36 1.388(3) . ?
C31 C32 1.392(3) . ?
C32 F32 1.348(2) . ?
C32 C33 1.371(3) . ?
C33 F33 1.342(3) . ?
C33 C34 1.384(3) . ?
C34 C35 1.385(3) . ?
C34 C37 1.425(3) . ?
C35 F37 1.344(2) . ?
C35 C36 1.374(3) . ?
C36 F36 1.352(2) . ?
F36 K2 3.1117(15) 2_556 ?
C37 N37 1.148(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 K1 N23 79.61(6) . 2_656 ?
N1 K1 N17 78.41(7) . 2_666 ?
N23 K1 N17 85.59(6) 2_656 2_666 ?
N1 K1 N3 148.54(6) . 1_655 ?
N23 K1 N3 81.53(6) 2_656 1_655 ?
N17 K1 N3 75.23(6) 2_666 1_655 ?
N1 K1 N21 82.98(6) . 1_564 ?
N23 K1 N21 115.22(6) 2_656 1_564 ?
N17 K1 N21 149.01(7) 2_666 1_564 ?
N3 K1 N21 128.05(6) 1_655 1_564 ?
N1 K1 N22 122.44(7) . 2_666 ?
N23 K1 N22 157.95(6) 2_656 2_666 ?
N17 K1 N22 98.41(6) 2_666 2_666 ?
N3 K1 N22 78.60(6) 1_655 2_666 ?
N21 K1 N22 71.20(6) 1_564 2_666 ?
N1 K1 N3 126.33(6) . 2_665 ?
N23 K1 N3 75.48(6) 2_656 2_665 ?
N17 K1 N3 143.87(6) 2_666 2_665 ?
N3 K1 N3 71.77(6) 1_655 2_665 ?
N21 K1 N3 66.68(6) 1_564 2_665 ?
N22 K1 N3 89.22(6) 2_666 2_665 ?
N1 K1 C3 107.64(6) . 2_665 ?
N23 K1 C3 65.22(6) 2_656 2_665 ?
N17 K1 C3 147.75(6) 2_666 2_665 ?
N3 K1 C3 86.65(6) 1_655 2_665 ?
N21 K1 C3 62.06(6) 1_564 2_665 ?
N22 K1 C3 103.94(6) 2_666 2_665 ?
N3 K1 C3 18.94(5) 2_665 2_665 ?
N1 K1 K2 129.88(5) . 2_665 ?
N23 K1 K2 122.49(4) 2_656 2_665 ?
N17 K1 K2 140.32(5) 2_666 2_665 ?
N3 K1 K2 81.56(4) 1_655 2_665 ?
N21 K1 K2 47.30(4) 1_564 2_665 ?
N22 K1 K2 44.94(4) 2_666 2_665 ?
N3 K1 K2 47.02(4) 2_665 2_665 ?
C3 K1 K2 59.24(4) 2_665 2_665 ?
N1 K1 K2 113.62(5) . 1_655 ?
N23 K1 K2 40.33(4) 2_656 1_655 ?
N17 K1 K2 72.97(5) 2_666 1_655 ?
N3 K1 K2 41.62(4) 1_655 1_655 ?
N21 K1 K2 137.76(4) 1_564 1_655 ?
N22 K1 K2 120.17(4) 2_666 1_655 ?
N3 K1 K2 72.70(4) 2_665 1_655 ?
C3 K1 K2 75.76(4) 2_665 1_655 ?
K2 K1 K2 109.070(15) 2_665 1_655 ?
N1 K1 K1 152.33(5) . 2_765 ?
N23 K1 K1 75.65(4) 2_656 2_765 ?
N17 K1 K1 111.44(5) 2_666 2_765 ?
N3 K1 K1 37.44(4) 1_655 2_765 ?
N21 K1 K1 96.47(4) 1_564 2_765 ?
N22 K1 K1 82.75(4) 2_666 2_765 ?
N3 K1 K1 34.33(4) 2_665 2_765 ?
C3 K1 K1 50.20(4) 2_665 2_765 ?
K2 K1 K1 58.431(13) 2_665 2_765 ?
K2 K1 K1 50.639(12) 1_655 2_765 ?
C1 N1 K1 160.00(19) . . ?
N1 C1 B1 174.6(3) . . ?
C1 B1 C2 104.96(19) . . ?
C1 B1 C3 110.38(19) . . ?
C2 B1 C3 109.5(2) . . ?
C1 B1 C11 113.8(2) . . ?
C2 B1 C11 110.9(2) . . ?
C3 B1 C11 107.21(19) . . ?
N37 K2 N22 134.37(7) . 1_554 ?
N37 K2 N2 74.38(7) . 1_545 ?
N22 K2 N2 91.70(6) 1_554 1_545 ?
N37 K2 N23 135.53(7) . 2_556 ?
N22 K2 N23 83.78(6) 1_554 2_556 ?
N2 K2 N23 84.44(6) 1_545 2_556 ?
N37 K2 N21 83.30(6) . 2_656 ?
N22 K2 N21 72.30(6) 1_554 2_656 ?
N2 K2 N21 129.07(6) 1_545 2_656 ?
N23 K2 N21 138.02(6) 2_556 2_656 ?
N37 K2 N3 111.62(6) . . ?
N22 K2 N3 94.87(6) 1_554 . ?
N2 K2 N3 162.20(6) 1_545 . ?
N23 K2 N3 79.87(6) 2_556 . ?
N21 K2 N3 68.73(6) 2_656 . ?
N37 K2 F36 74.12(6) . 2_556 ?
N22 K2 F36 137.89(5) 1_554 2_556 ?
N2 K2 F36 63.73(5) 1_545 2_556 ?
N23 K2 F36 61.44(5) 2_556 2_556 ?
N21 K2 F36 149.77(5) 2_656 2_556 ?
N3 K2 F36 100.99(5) . 2_556 ?
N37 K2 C23 121.05(6) . 2_556 ?
N22 K2 C23 90.34(6) 1_554 2_556 ?
N2 K2 C23 67.04(6) 1_545 2_556 ?
N23 K2 C23 18.36(5) 2_556 2_556 ?
N21 K2 C23 155.37(6) 2_656 2_556 ?
N3 K2 C23 96.35(6) . 2_556 ?
F36 K2 C23 49.51(5) 2_556 2_556 ?
N37 K2 K1 129.55(5) . 2_665 ?
N22 K2 K1 47.08(4) 1_554 2_665 ?
N2 K2 K1 138.72(5) 1_545 2_665 ?
N23 K2 K1 91.78(4) 2_556 2_665 ?
N21 K2 K1 46.78(4) 2_656 2_665 ?
N3 K2 K1 50.81(4) . 2_665 ?
F36 K2 K1 146.07(3) 2_556 2_665 ?
C23 K2 K1 108.59(4) 2_556 2_665 ?
N37 K2 K1 131.02(5) . 1_455 ?
N22 K2 K1 93.36(4) 1_554 1_455 ?
N2 K2 K1 122.41(5) 1_545 1_455 ?
N23 K2 K1 39.51(4) 2_556 1_455 ?
N21 K2 K1 106.90(4) 2_656 1_455 ?
N3 K2 K1 40.76(4) . 1_455 ?
F36 K2 K1 75.16(3) 2_556 1_455 ?
C23 K2 K1 55.61(4) 2_556 1_455 ?
K1 K2 K1 70.929(15) 2_665 1_455 ?
C2 N2 K2 147.01(19) . 1_565 ?
N2 C2 B1 175.9(3) . . ?
C23 B2 C21 109.43(19) . . ?
C23 B2 C22 108.07(19) . . ?
C21 B2 C22 107.34(18) . . ?
C23 B2 C31 114.13(19) . . ?
C21 B2 C31 108.83(19) . . ?
C22 B2 C31 108.83(18) . . ?
C3 N3 K1 132.46(17) . 1_455 ?
C3 N3 K2 124.81(17) . . ?
K1 N3 K2 97.62(6) 1_455 . ?
C3 N3 K1 98.74(16) . 2_665 ?
K1 N3 K1 108.22(6) 1_455 2_665 ?
K2 N3 K1 82.17(5) . 2_665 ?
N3 C3 B1 176.4(2) . . ?
N3 C3 K1 62.31(14) . 2_665 ?
B1 C3 K1 119.08(14) . 2_665 ?
C16 C11 C12 114.8(2) . . ?
C16 C11 B1 119.6(2) . . ?
C12 C11 B1 125.5(2) . . ?
F12 C12 C13 116.6(2) . . ?
F12 C12 C11 121.0(2) . . ?
C13 C12 C11 122.4(2) . . ?
F13 C13 C12 118.9(2) . . ?
F13 C13 C14 119.6(2) . . ?
C12 C13 C14 121.5(2) . . ?
C13 C14 C15 117.0(2) . . ?
C13 C14 C17 122.7(2) . . ?
C15 C14 C17 120.3(2) . . ?
F15 C15 C16 119.7(2) . . ?
F15 C15 C14 119.5(2) . . ?
C16 C15 C14 120.8(2) . . ?
F16 C16 C15 117.3(2) . . ?
F16 C16 C11 119.1(2) . . ?
C15 C16 C11 123.5(2) . . ?
N17 C17 C14 178.1(3) . . ?
C17 N17 K1 168.7(2) . 2_666 ?
N21 C21 B2 177.0(2) . . ?
C21 N21 K1 123.62(17) . 1_546 ?
C21 N21 K2 144.33(18) . 2_656 ?
K1 N21 K2 85.92(6) 1_546 2_656 ?
N22 C22 B2 178.2(2) . . ?
C22 N22 K2 136.26(17) . 1_556 ?
C22 N22 K1 132.03(18) . 2_666 ?
K2 N22 K1 87.99(6) 1_556 2_666 ?
N23 C23 B2 179.6(3) . . ?
N23 C23 K2 53.06(14) . 2_556 ?
B2 C23 K2 126.80(14) . 2_556 ?
C23 N23 K1 136.33(18) . 2_656 ?
C23 N23 K2 108.58(17) . 2_556 ?
K1 N23 K2 100.17(6) 2_656 2_556 ?
C36 C31 C32 114.9(2) . . ?
C36 C31 B2 126.8(2) . . ?
C32 C31 B2 118.28(19) . . ?
F32 C32 C33 118.0(2) . . ?
F32 C32 C31 119.0(2) . . ?
C33 C32 C31 123.0(2) . . ?
F33 C33 C32 120.0(2) . . ?
F33 C33 C34 119.0(2) . . ?
C32 C33 C34 121.0(2) . . ?
C33 C34 C35 117.2(2) . . ?
C33 C34 C37 120.5(2) . . ?
C35 C34 C37 122.3(2) . . ?
F37 C35 C36 120.2(2) . . ?
F37 C35 C34 118.9(2) . . ?
C36 C35 C34 120.9(2) . . ?
F36 C36 C35 115.99(19) . . ?
F36 C36 C31 121.0(2) . . ?
C35 C36 C31 123.0(2) . . ?
C36 F36 K2 135.13(12) . 2_556 ?
N37 C37 C34 177.6(3) . . ?
C37 N37 K2 161.0(2) . . ?

_refine_diff_density_max         0.355
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.065

####################################################################### 
# 
# 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_JL087_JL_Me3NHB4c
_database_code_depnum_ccdc_archive 'CCDC 1548895'
_audit_update_record             
;
2017-05-09 deposited with the CCDC.
2017-06-26 downloaded from the CCDC.
;


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

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H2 B F3 N3, C3 H10 N'
_chemical_formula_sum            'C12 H13 B F3 N4'
_chemical_formula_weight         281.07

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           46
_space_group_name_H-M_alt        'I m a 2'
_space_group_name_Hall           'I 2 -2a'

_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'
'x+1/2, -y, z'
'-x+1/2, y, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1, -y+1/2, z+1/2'
'-x+1, y+1/2, z+1/2'

_cell_length_a                   7.7462(5)
_cell_length_b                   16.7938(10)
_cell_length_c                   10.8073(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1405.90(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2100
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      26.60

_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).
;
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_F_000             580
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.110
_shelx_estimated_absorpt_T_min   0.964
_shelx_estimated_absorpt_T_max   0.991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6984
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4838
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.241
_diffrn_reflns_theta_max         26.756
_diffrn_reflns_theta_full        26.000
_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 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             1597
_reflns_number_gt                1477
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.877
_reflns_Friedel_fraction_max     0.976
_reflns_Friedel_fraction_full    0.982

_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. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0340P)²+0.4125P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 647 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.3(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1597
_refine_ls_number_parameters     140
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0287
_refine_ls_wR_factor_ref         0.0686
_refine_ls_wR_factor_gt          0.0659
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
F1 F 0.7500 0.27739(9) 0.60970(15) 0.0233(4) Uani 1 2 d S T P . .
H1 H 0.7500 0.3230(18) 0.833(3) 0.015(7) Uiso 1 2 d S . P . .
N1 N 0.4711(2) 0.30312(11) 0.35092(16) 0.0240(4) Uani 1 1 d . . . . .
C1 C 0.5852(3) 0.34229(11) 0.37917(17) 0.0167(4) Uani 1 1 d . . . . .
B1 B 0.7500 0.39431(19) 0.4173(3) 0.0167(7) Uani 1 2 d S T P . .
F2 F 0.7500 0.45773(12) 0.94208(18) 0.0372(5) Uani 1 2 d S T P . .
H2 H 0.7500 0.535(2) 0.558(4) 0.023(9) Uiso 1 2 d S . P . .
N2 N 0.7500 0.52955(16) 0.2755(3) 0.0277(6) Uani 1 2 d S T P . .
C2 C 0.7500 0.47326(17) 0.3347(3) 0.0191(6) Uani 1 2 d S T P . .
F3 F 0.7500 0.58012(11) 0.78185(19) 0.0493(6) Uani 1 2 d S T P . .
H3 H 0.7500 0.6577(19) 0.201(4) 0.023(9) Uiso 1 2 d S . P . .
C3 C 0.7500 0.41468(17) 0.5636(3) 0.0176(6) Uani 1 2 d S T P . .
C4 C 0.7500 0.35417(16) 0.6510(3) 0.0182(6) Uani 1 2 d S T P . .
H4 H 0.646(3) 0.7802(12) 0.163(2) 0.021(6) Uiso 1 1 d . . . . .
C5 C 0.7500 0.36510(18) 0.7775(3) 0.0218(6) Uani 1 2 d S T P . .
H5 H 0.7500 0.7811(19) 0.034(4) 0.029(10) Uiso 1 2 d S . P . .
C6 C 0.7500 0.44246(19) 0.8193(3) 0.0261(7) Uani 1 2 d S T P . .
H6 H 0.588(3) 0.6594(13) -0.030(2) 0.030(7) Uiso 1 1 d . . . . .
C8 C 0.7500 0.49198(18) 0.6112(3) 0.0241(6) Uani 1 2 d S T P . .
H8 H 0.593(3) 0.5854(14) 0.063(2) 0.029(6) Uiso 1 1 d . . . . .
C7 C 0.7500 0.50499(18) 0.7365(3) 0.0294(8) Uani 1 2 d S T P . .
H7 H 0.494(3) 0.6637(14) 0.103(2) 0.028(6) Uiso 1 1 d . . . . .
C9 C 0.5910(3) 0.64275(13) 0.0585(2) 0.0222(5) Uani 1 1 d . . . . .
N9 N 0.7500 0.67477(13) 0.1190(2) 0.0168(5) Uani 1 2 d S T P . .
C10 C 0.7500 0.76363(17) 0.1191(3) 0.0225(6) Uani 1 2 d S T P . .


_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
F1 C4 1.364(3) . ?
N1 C1 1.143(3) . ?
C1 B1 1.601(3) . ?
B1 C2 1.598(4) . ?
B1 C1 1.601(3) 4_655 ?
B1 C3 1.618(4) . ?
F2 C6 1.351(4) . ?
N2 C2 1.141(4) . ?
F3 C7 1.353(4) . ?
C3 C4 1.387(4) . ?
C3 C8 1.396(4) . ?
C4 C5 1.379(4) . ?
C5 C6 1.376(4) . ?
C5 H1 0.92(3) . ?
C6 C7 1.380(4) . ?
C8 C7 1.372(5) . ?
C8 H2 0.93(4) . ?
C9 N9 1.494(2) . ?
C9 H6 1.00(3) . ?
C9 H8 0.97(2) . ?
C9 H7 0.96(3) . ?
N9 C10 1.492(4) . ?
N9 C9 1.494(2) 4_655 ?
N9 H3 0.93(4) . ?
C10 H4 0.98(2) . ?
C10 H5 0.96(4) . ?

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
N1 C1 B1 177.7(2) . . ?
C2 B1 C1 108.00(16) . 4_655 ?
C2 B1 C1 108.00(16) . . ?
C1 B1 C1 105.8(2) 4_655 . ?
C2 B1 C3 111.7(2) . . ?
C1 B1 C3 111.52(15) 4_655 . ?
C1 B1 C3 111.52(15) . . ?
N2 C2 B1 179.9(3) . . ?
C4 C3 C8 115.5(3) . . ?
C4 C3 B1 120.7(2) . . ?
C8 C3 B1 123.8(3) . . ?
F1 C4 C5 116.7(3) . . ?
F1 C4 C3 118.0(2) . . ?
C5 C4 C3 125.2(3) . . ?
C6 C5 C4 116.9(3) . . ?
C6 C5 H1 121(2) . . ?
C4 C5 H1 122(2) . . ?
F2 C6 C5 120.1(3) . . ?
F2 C6 C7 119.5(3) . . ?
C5 C6 C7 120.4(3) . . ?
C7 C8 C3 120.8(3) . . ?
C7 C8 H2 119(2) . . ?
C3 C8 H2 120(2) . . ?
F3 C7 C8 120.4(3) . . ?
F3 C7 C6 118.4(3) . . ?
C8 C7 C6 121.3(3) . . ?
N9 C9 H6 109.6(14) . . ?
N9 C9 H8 108.8(16) . . ?
H6 C9 H8 109(2) . . ?
N9 C9 H7 107.1(15) . . ?
H6 C9 H7 111(2) . . ?
H8 C9 H7 111(2) . . ?
C10 N9 C9 111.11(15) . 4_655 ?
C10 N9 C9 111.11(15) . . ?
C9 N9 C9 111.0(2) 4_655 . ?
C10 N9 H3 108(2) . . ?
C9 N9 H3 107.8(10) 4_655 . ?
C9 N9 H3 107.8(10) . . ?
N9 C10 H4 106.6(12) . . ?
N9 C10 H5 108(2) . . ?
H4 C10 H5 112.1(16) . . ?

_refine_diff_density_max         0.179
_refine_diff_density_min         -0.136
_refine_diff_density_rms         0.032

####################################################################### 
# 
# 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_JL083_JL_KB4a
_database_code_depnum_ccdc_archive 'CCDC 1548905'
_audit_update_record             
;
2017-05-09 deposited with the CCDC.
2017-06-26 downloaded from the CCDC.
;


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


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H2 B F3 K N3'
_chemical_formula_sum            'C9 H2 B F3 K N3'
_chemical_formula_weight         259.05

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'
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'

_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                   7.4212(4)
_cell_length_b                   21.5366(12)
_cell_length_c                   7.4276(4)
_cell_angle_alpha                90
_cell_angle_beta                 118.496(2)
_cell_angle_gamma                90
_cell_volume                     1043.31(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8430
_cell_measurement_theta_min      3.19
_cell_measurement_theta_max      26.79


_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).
;

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_F_000             512
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.527
_shelx_estimated_absorpt_T_min   0.916
_shelx_estimated_absorpt_T_max   0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7180
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14316
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.891
_diffrn_reflns_theta_max         26.798
_diffrn_reflns_theta_full        26.000
_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             2236
_reflns_number_gt                2035
_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. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0239P)²+0.6323P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2236
_refine_ls_number_parameters     162
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0272
_refine_ls_wR_factor_ref         0.0657
_refine_ls_wR_factor_gt          0.0638
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_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
N1 N 0.86967(19) 0.56023(6) 0.55710(19) 0.0189(3) Uani 1 1 d . . . . .
H1 H 0.515(3) 0.8563(9) 0.381(3) 0.027(5) Uiso 1 1 d . . . . .
K1 K 0.17342(5) 0.47348(2) -0.16612(5) 0.01674(9) Uani 1 1 d . . . . .
F1 F 0.54629(14) 0.66548(4) 0.18236(13) 0.0228(2) Uani 1 1 d . . . . .
B1 B 0.5019(2) 0.60816(7) 0.4977(2) 0.0140(3) Uani 1 1 d . . . . .
C1 C 0.7167(2) 0.58016(6) 0.5322(2) 0.0145(3) Uani 1 1 d . . . . .
N2 N 0.20103(19) 0.55195(6) 0.15371(19) 0.0179(3) Uani 1 1 d . . . . .
H2 H 0.548(2) 0.7825(7) 0.148(2) 0.011(4) Uiso 1 1 d . . . . .
F2 F 0.45690(15) 0.70912(4) 0.75575(14) 0.0235(2) Uani 1 1 d . . . . .
C2 C 0.3264(2) 0.57556(6) 0.2960(2) 0.0141(3) Uani 1 1 d . . . . .
N3 N 0.45072(19) 0.56261(6) 0.81442(19) 0.0192(3) Uani 1 1 d . . . . .
F3 F 0.46090(15) 0.82973(4) 0.68815(16) 0.0295(2) Uani 1 1 d . . . . .
C3 C 0.4709(2) 0.58423(6) 0.6849(2) 0.0142(3) Uani 1 1 d . . . . .
C4 C 0.4995(2) 0.68244(6) 0.4688(2) 0.0132(3) Uani 1 1 d . . . . .
C5 C 0.5246(2) 0.70698(7) 0.3087(2) 0.0165(3) Uani 1 1 d . . . . .
C6 C 0.5307(2) 0.76904(7) 0.2701(2) 0.0208(3) Uani 1 1 d . . . . .
C7 C 0.5096(2) 0.81126(7) 0.4000(2) 0.0214(3) Uani 1 1 d . . . . .
C9 C 0.4789(2) 0.72658(7) 0.5933(2) 0.0158(3) Uani 1 1 d . . . . .
C8 C 0.4830(2) 0.78946(7) 0.5590(2) 0.0188(3) 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
N1 C1 1.1433(19) . ?
N1 K1 2.8595(13) 3_665 ?
N1 K1 2.8943(13) 1_656 ?
K1 N2 2.8420(13) . ?
K1 N1 2.8595(13) 3_665 ?
K1 N3 2.8679(13) 1_554 ?
K1 N3 2.8732(13) 3_666 ?
K1 N2 2.8766(13) 3_565 ?
K1 N1 2.8943(13) 1_454 ?
K1 F3 3.2325(10) 2_545 ?
K1 C1 3.3924(14) 3_665 ?
K1 C3 3.5048(14) 3_666 ?
K1 C2 3.5200(14) 3_565 ?
K1 K1 4.4132(6) 3_665 ?
K1 K1 4.4813(6) 3_565 ?
F1 C5 1.3599(17) . ?
B1 C3 1.600(2) . ?
B1 C2 1.604(2) . ?
B1 C1 1.606(2) . ?
B1 C4 1.613(2) . ?
C1 K1 3.3924(14) 3_665 ?
N2 C2 1.1414(19) . ?
N2 K1 2.8766(13) 3_565 ?
F2 C9 1.3459(16) . ?
C2 K1 3.5199(14) 3_565 ?
N3 C3 1.1408(19) . ?
N3 K1 2.8679(13) 1_556 ?
N3 K1 2.8733(13) 3_666 ?
F3 C8 1.3601(17) . ?
F3 K1 3.2324(10) 2 ?
C3 K1 3.5048(14) 3_666 ?
C4 C9 1.384(2) . ?
C4 C5 1.393(2) . ?
C5 C6 1.372(2) . ?
C6 C7 1.388(2) . ?
C6 H2 1.020(16) . ?
C7 C8 1.369(2) . ?
C7 H1 0.984(19) . ?
C9 C8 1.381(2) . ?

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
C1 N1 K1 108.04(10) . 3_665 ?
C1 N1 K1 137.23(11) . 1_656 ?
K1 N1 K1 103.26(4) 3_665 1_656 ?
N2 K1 N1 158.19(4) . 3_665 ?
N2 K1 N3 82.92(4) . 1_554 ?
N1 K1 N3 81.61(4) 3_665 1_554 ?
N2 K1 N3 75.48(4) . 3_666 ?
N1 K1 N3 116.38(4) 3_665 3_666 ?
N3 K1 N3 79.53(4) 1_554 3_666 ?
N2 K1 N2 76.81(4) . 3_565 ?
N1 K1 N2 110.03(4) 3_665 3_565 ?
N3 K1 N2 148.91(4) 1_554 3_565 ?
N3 K1 N2 116.94(4) 3_666 3_565 ?
N2 K1 N1 86.04(4) . 1_454 ?
N1 K1 N1 76.75(4) 3_665 1_454 ?
N3 K1 N1 82.33(4) 1_554 1_454 ?
N3 K1 N1 155.46(4) 3_666 1_454 ?
N2 K1 N1 73.06(4) 3_565 1_454 ?
N2 K1 F3 120.62(3) . 2_545 ?
N1 K1 F3 79.81(3) 3_665 2_545 ?
N3 K1 F3 148.20(3) 1_554 2_545 ?
N3 K1 F3 85.93(3) 3_666 2_545 ?
N2 K1 F3 62.62(3) 3_565 2_545 ?
N1 K1 F3 117.74(3) 1_454 2_545 ?
N2 K1 C1 157.43(4) . 3_665 ?
N1 K1 C1 18.69(3) 3_665 3_665 ?
N3 K1 C1 74.62(4) 1_554 3_665 ?
N3 K1 C1 97.83(4) 3_666 3_665 ?
N2 K1 C1 124.49(4) 3_565 3_665 ?
N1 K1 C1 93.10(4) 1_454 3_665 ?
F3 K1 C1 79.61(3) 2_545 3_665 ?
N2 K1 C3 68.87(3) . 3_666 ?
N1 K1 C3 127.63(4) 3_665 3_666 ?
N3 K1 C3 94.55(3) 1_554 3_666 ?
N3 K1 C3 17.22(3) 3_666 3_666 ?
N2 K1 C3 99.73(3) 3_565 3_666 ?
N1 K1 C3 154.91(3) 1_454 3_666 ?
F3 K1 C3 77.06(3) 2_545 3_666 ?
C1 K1 C3 110.15(3) 3_665 3_666 ?
N2 K1 C2 93.08(4) . 3_565 ?
N1 K1 C2 93.03(4) 3_665 3_565 ?
N3 K1 C2 151.01(3) 1_554 3_565 ?
N3 K1 C2 127.37(4) 3_666 3_565 ?
N2 K1 C2 17.04(3) 3_565 3_565 ?
N1 K1 C2 68.73(3) 1_454 3_565 ?
F3 K1 C2 55.92(3) 2_545 3_565 ?
C1 K1 C2 107.64(3) 3_665 3_565 ?
C3 K1 C2 110.83(3) 3_666 3_565 ?
N2 K1 K1 75.92(3) . 3_665 ?
N1 K1 K1 101.21(3) 3_665 3_665 ?
N3 K1 K1 39.81(3) 1_554 3_665 ?
N3 K1 K1 39.72(3) 3_666 3_665 ?
N2 K1 K1 148.37(3) 3_565 3_665 ?
N1 K1 K1 120.36(3) 1_454 3_665 ?
F3 K1 K1 120.41(2) 2_545 3_665 ?
C1 K1 K1 85.21(3) 3_665 3_665 ?
C3 K1 K1 55.23(2) 3_666 3_665 ?
C2 K1 K1 164.49(3) 3_565 3_665 ?
N2 K1 K1 38.68(3) . 3_565 ?
N1 K1 K1 143.97(3) 3_665 3_565 ?
N3 K1 K1 118.14(3) 1_554 3_565 ?
N3 K1 K1 97.57(3) 3_666 3_565 ?
N2 K1 K1 38.13(3) 3_565 3_565 ?
N1 K1 K1 76.66(3) 1_454 3_565 ?
F3 K1 K1 91.59(2) 2_545 3_565 ?
C1 K1 K1 161.64(3) 3_665 3_565 ?
C3 K1 K1 83.10(3) 3_666 3_565 ?
C2 K1 K1 54.57(2) 3_565 3_565 ?
K1 K1 K1 113.095(13) 3_665 3_565 ?
C3 B1 C2 106.34(11) . . ?
C3 B1 C1 106.48(11) . . ?
C2 B1 C1 106.66(11) . . ?
C3 B1 C4 115.96(12) . . ?
C2 B1 C4 110.95(11) . . ?
C1 B1 C4 109.94(11) . . ?
N1 C1 B1 179.89(17) . . ?
N1 C1 K1 53.27(8) . 3_665 ?
B1 C1 K1 126.84(9) . 3_665 ?
C2 N2 K1 137.79(11) . . ?
C2 N2 K1 115.36(10) . 3_565 ?
K1 N2 K1 103.19(4) . 3_565 ?
N2 C2 B1 179.28(16) . . ?
N2 C2 K1 47.60(9) . 3_565 ?
B1 C2 K1 131.87(9) . 3_565 ?
C3 N3 K1 134.55(11) . 1_556 ?
C3 N3 K1 114.58(10) . 3_666 ?
K1 N3 K1 100.47(4) 1_556 3_666 ?
C8 F3 K1 135.49(9) . 2 ?
N3 C3 B1 174.70(14) . . ?
N3 C3 K1 48.20(8) . 3_666 ?
B1 C3 K1 130.55(9) . 3_666 ?
C9 C4 C5 114.34(13) . . ?
C9 C4 B1 126.17(13) . . ?
C5 C4 B1 119.47(13) . . ?
F1 C5 C6 118.01(13) . . ?
F1 C5 C4 116.62(13) . . ?
C6 C5 C4 125.37(14) . . ?
C5 C6 C7 117.86(14) . . ?
C5 C6 H2 119.6(9) . . ?
C7 C6 H2 122.6(9) . . ?
C8 C7 C6 119.01(14) . . ?
C8 C7 H1 119.6(11) . . ?
C6 C7 H1 121.3(11) . . ?
F2 C9 C8 117.54(13) . . ?
F2 C9 C4 120.40(13) . . ?
C8 C9 C4 122.06(14) . . ?
F3 C8 C7 120.33(13) . . ?
F3 C8 C9 118.31(14) . . ?
C7 C8 C9 121.36(14) . . ?

_refine_diff_density_max         0.382
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.049

####################################################################### 
# 
# 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_JL094_JL_KB2b
_database_code_depnum_ccdc_archive 'CCDC 1548901'
_audit_update_record             
;
2017-05-09 deposited with the CCDC.
2017-06-26 downloaded from the CCDC.
;


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

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H4 B F K N3'
_chemical_formula_sum            'C9 H4 B F K N3'
_chemical_formula_weight         223.06

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'
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'

_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                   11.3175(10)
_cell_length_b                   12.5441(11)
_cell_length_c                   7.3312(6)
_cell_angle_alpha                90
_cell_angle_beta                 100.954(4)
_cell_angle_gamma                90
_cell_volume                     1021.83(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3915
_cell_measurement_theta_min      3.25
_cell_measurement_theta_max      26.24

_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).
;

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_F_000             448
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.498
_shelx_estimated_absorpt_T_min   0.929
_shelx_estimated_absorpt_T_max   0.990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6859
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13906
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_av_R_equivalents  0.0495
_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       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.833
_diffrn_reflns_theta_max         26.791
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2185
_reflns_number_gt                1792
_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. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0375P)²+0.5529P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2185
_refine_ls_number_parameters     152
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0369
_refine_ls_wR_factor_ref         0.0876
_refine_ls_wR_factor_gt          0.0820
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K -0.11498(4) 0.34471(3) 0.96954(6) 0.01727(13) Uani 1 1 d . . . . .
N1 N 0.02033(15) 0.31972(13) 0.6898(2) 0.0196(4) Uani 1 1 d . . . . .
C1 C 0.09095(17) 0.36525(15) 0.6278(3) 0.0155(4) Uani 1 1 d . . . . .
B1 B 0.19081(19) 0.42784(17) 0.5418(3) 0.0153(4) Uani 1 1 d . . . . .
F1 F 0.63771(11) 0.40613(12) 0.7545(2) 0.0471(4) Uani 1 1 d . . . . .
C3 C 0.19655(16) 0.54669(15) 0.6247(3) 0.0160(4) Uani 1 1 d . . . . .
N3 N 0.19712(15) 0.63109(13) 0.6844(2) 0.0206(4) Uani 1 1 d . . . . .
C2 C 0.14371(16) 0.43661(14) 0.3217(3) 0.0154(4) Uani 1 1 d . . . . .
N2 N 0.11012(15) 0.44224(12) 0.1642(2) 0.0204(4) Uani 1 1 d . . . . .
C4 C 0.31761(18) 0.36540(16) 0.5894(3) 0.0183(4) Uani 1 1 d . . . . .
C5 C 0.31800(19) 0.25478(17) 0.5671(3) 0.0230(5) Uani 1 1 d . . . . .
H5 H 0.238(2) 0.2166(19) 0.523(3) 0.030(6) Uiso 1 1 d . . . . .
C9 C 0.42714(19) 0.41643(18) 0.6511(3) 0.0239(5) Uani 1 1 d . . . . .
H9 H 0.434(2) 0.494(2) 0.668(3) 0.035(7) Uiso 1 1 d . . . . .
C8 C 0.53072(19) 0.35515(19) 0.6892(3) 0.0298(5) Uani 1 1 d . . . . .
C7 C 0.5311(2) 0.24731(19) 0.6688(3) 0.0306(5) Uani 1 1 d . . . . .
H7 H 0.608(2) 0.211(2) 0.700(4) 0.041(7) Uiso 1 1 d . . . . .
C6 C 0.4232(2) 0.19666(19) 0.6066(3) 0.0294(5) Uani 1 1 d . . . . .
H6 H 0.421(2) 0.118(2) 0.589(3) 0.029(6) Uiso 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 N1 2.8005(18) . ?
K1 N2 2.8508(17) 3_566 ?
K1 N1 2.8753(17) 4_566 ?
K1 N3 2.8788(18) 3_567 ?
K1 N2 2.9398(18) 1_556 ?
K1 N3 2.9868(18) 2_546 ?
K1 F1 3.0392(14) 1_455 ?
K1 C2 3.4532(19) 3_566 ?
K1 K1 4.3684(5) 4_565 ?
K1 K1 4.3684(5) 4_566 ?
K1 K1 4.6593(9) 3_567 ?
N1 C1 1.144(3) . ?
N1 K1 2.8753(17) 4_565 ?
C1 B1 1.601(3) . ?
B1 C2 1.604(3) . ?
B1 C3 1.607(3) . ?
B1 C4 1.614(3) . ?
F1 C8 1.373(2) . ?
F1 K1 3.0392(14) 1_655 ?
C3 N3 1.145(2) . ?
N3 K1 2.8787(18) 3_567 ?
N3 K1 2.9867(17) 2_556 ?
C2 N2 1.147(2) . ?
C2 K1 3.4532(19) 3_566 ?
N2 K1 2.8508(17) 3_566 ?
N2 K1 2.9397(17) 1_554 ?
C4 C9 1.392(3) . ?
C4 C5 1.397(3) . ?
C5 C6 1.379(3) . ?
C5 H5 1.02(2) . ?
C9 C8 1.385(3) . ?
C9 H9 0.98(3) . ?
C8 C7 1.361(3) . ?
C7 C6 1.375(3) . ?
C7 H7 0.97(3) . ?
C6 H6 0.99(2) . ?

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
N1 K1 N2 78.70(5) . 3_566 ?
N1 K1 N1 91.37(5) . 4_566 ?
N2 K1 N1 145.35(5) 3_566 4_566 ?
N1 K1 N3 165.97(5) . 3_567 ?
N2 K1 N3 103.58(5) 3_566 3_567 ?
N1 K1 N3 78.90(5) 4_566 3_567 ?
N1 K1 N2 81.84(5) . 1_556 ?
N2 K1 N2 72.86(5) 3_566 1_556 ?
N1 K1 N2 72.90(5) 4_566 1_556 ?
N3 K1 N2 85.61(5) 3_567 1_556 ?
N1 K1 N3 78.29(5) . 2_546 ?
N2 K1 N3 137.39(5) 3_566 2_546 ?
N1 K1 N3 70.30(5) 4_566 2_546 ?
N3 K1 N3 107.35(5) 3_567 2_546 ?
N2 K1 N3 137.36(5) 1_556 2_546 ?
N1 K1 F1 103.08(5) . 1_455 ?
N2 K1 F1 70.12(5) 3_566 1_455 ?
N1 K1 F1 144.38(5) 4_566 1_455 ?
N3 K1 F1 90.61(5) 3_567 1_455 ?
N2 K1 F1 140.72(4) 1_556 1_455 ?
N3 K1 F1 80.88(4) 2_546 1_455 ?
N1 K1 C2 68.69(5) . 3_566 ?
N2 K1 C2 17.89(4) 3_566 3_566 ?
N1 K1 C2 153.46(5) 4_566 3_566 ?
N3 K1 C2 116.92(5) 3_567 3_566 ?
N2 K1 C2 86.60(5) 1_556 3_566 ?
N3 K1 C2 119.54(5) 2_546 3_566 ?
F1 K1 C2 60.57(4) 1_455 3_566 ?
N1 K1 K1 40.31(3) . 4_565 ?
N2 K1 K1 102.60(4) 3_566 4_565 ?
N1 K1 K1 89.78(4) 4_566 4_565 ?
N3 K1 K1 148.02(4) 3_567 4_565 ?
N2 K1 K1 119.71(3) 1_556 4_565 ?
N3 K1 K1 40.92(4) 2_546 4_565 ?
F1 K1 K1 81.34(3) 1_455 4_565 ?
C2 K1 K1 85.89(3) 3_566 4_565 ?
N1 K1 K1 129.85(4) . 4_566 ?
N2 K1 K1 143.29(4) 3_566 4_566 ?
N1 K1 K1 39.06(4) 4_566 4_566 ?
N3 K1 K1 42.82(3) 3_567 4_566 ?
N2 K1 K1 87.55(3) 1_556 4_566 ?
N3 K1 K1 77.26(4) 2_546 4_566 ?
F1 K1 K1 115.24(3) 1_455 4_566 ?
C2 K1 K1 159.37(3) 3_566 4_566 ?
K1 K1 K1 114.094(18) 4_565 4_566 ?
N1 K1 K1 77.91(4) . 3_567 ?
N2 K1 K1 37.08(3) 3_566 3_567 ?
N1 K1 K1 108.53(4) 4_566 3_567 ?
N3 K1 K1 95.47(4) 3_567 3_567 ?
N2 K1 K1 35.78(3) 1_556 3_567 ?
N3 K1 K1 156.13(4) 2_546 3_567 ?
F1 K1 K1 106.28(3) 1_455 3_567 ?
C2 K1 K1 51.71(3) 3_566 3_567 ?
K1 K1 K1 116.499(12) 4_565 3_567 ?
K1 K1 K1 117.611(12) 4_566 3_567 ?
C1 N1 K1 139.04(14) . . ?
C1 N1 K1 118.22(14) . 4_565 ?
K1 N1 K1 100.64(5) . 4_565 ?
N1 C1 B1 179.3(2) . . ?
C1 B1 C2 107.80(16) . . ?
C1 B1 C3 106.66(16) . . ?
C2 B1 C3 107.38(15) . . ?
C1 B1 C4 110.00(16) . . ?
C2 B1 C4 111.28(16) . . ?
C3 B1 C4 113.46(16) . . ?
C8 F1 K1 136.65(13) . 1_655 ?
N3 C3 B1 177.9(2) . . ?
C3 N3 K1 117.08(15) . 3_567 ?
C3 N3 K1 134.91(15) . 2_556 ?
K1 N3 K1 96.26(5) 3_567 2_556 ?
N2 C2 B1 179.6(2) . . ?
N2 C2 K1 49.80(11) . 3_566 ?
B1 C2 K1 130.59(11) . 3_566 ?
C2 N2 K1 112.31(13) . 3_566 ?
C2 N2 K1 123.64(14) . 1_554 ?
K1 N2 K1 107.14(5) 3_566 1_554 ?
C9 C4 C5 118.18(18) . . ?
C9 C4 B1 123.19(18) . . ?
C5 C4 B1 118.63(17) . . ?
C6 C5 C4 121.5(2) . . ?
C6 C5 H5 119.8(13) . . ?
C4 C5 H5 118.7(13) . . ?
C8 C9 C4 118.5(2) . . ?
C8 C9 H9 118.9(14) . . ?
C4 C9 H9 122.6(14) . . ?
C7 C8 F1 118.7(2) . . ?
C7 C8 C9 123.4(2) . . ?
F1 C8 C9 117.9(2) . . ?
C8 C7 C6 118.3(2) . . ?
C8 C7 H7 117.5(16) . . ?
C6 C7 H7 124.2(16) . . ?
C7 C6 C5 120.2(2) . . ?
C7 C6 H6 119.9(13) . . ?
C5 C6 H6 119.9(13) . . ?

_refine_diff_density_max         0.329
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.061

####################################################################### 
# 
# 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_JL022_JL_Et4N2B4c
_database_code_depnum_ccdc_archive 'CCDC 1548894'
_audit_update_record             
;
2017-05-09 deposited with the CCDC.
2017-06-26 downloaded from the CCDC.
;


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


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 B2 F4 N6, 2(C8 H20 N)'
_chemical_formula_sum            'C28 H40 B2 F4 N8'
_chemical_formula_weight         586.30

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'
F F 0.0171 0.0103 '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                   9.2925(5)
_cell_length_b                   13.9870(7)
_cell_length_c                   19.7322(10)
_cell_angle_alpha                103.804(2)
_cell_angle_beta                 92.966(2)
_cell_angle_gamma                107.242(2)
_cell_volume                     2357.8(2)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8531
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      24.44
_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).
;

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_F_000             930
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.092
_shelx_estimated_absorpt_T_min   0.983
_shelx_estimated_absorpt_T_max   0.989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6786
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31095
_diffrn_reflns_av_unetI/netI     0.0753
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.072
_diffrn_reflns_theta_max         26.886
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10150
_reflns_number_gt                6261
_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. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0775P)²+1.1324P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10150
_refine_ls_number_parameters     771
_refine_ls_number_restraints     131
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0624
_refine_ls_wR_factor_ref         0.1745
_refine_ls_wR_factor_gt          0.1478
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
B1 B 0.3261(3) 0.3143(2) 0.02789(14) 0.0180(6) Uani 1 1 d . . . . .
C1 C 0.1825(3) 0.23004(19) 0.04356(12) 0.0189(5) Uani 1 1 d . . . . .
N1 N 0.0770(3) 0.17176(17) 0.05482(11) 0.0275(5) Uani 1 1 d . . . . .
C2 C 0.4581(3) 0.26269(19) 0.01351(12) 0.0207(5) Uani 1 1 d . . . . .
N2 N 0.5534(3) 0.22719(18) 0.00657(12) 0.0305(5) Uani 1 1 d . . . . .
C3 C 0.2709(3) 0.33916(19) -0.04162(13) 0.0208(5) Uani 1 1 d . . . . .
N3 N 0.2230(3) 0.35202(18) -0.09148(12) 0.0329(6) Uani 1 1 d . . . . .
B2 B 0.5682(3) 0.6792(2) 0.29086(16) 0.0242(7) Uani 1 1 d . . . . .
C4 C 0.6660(3) 0.6565(2) 0.34987(14) 0.0275(6) Uani 1 1 d . . . . .
N4 N 0.7452(3) 0.6459(2) 0.39068(14) 0.0483(7) Uani 1 1 d . . . . .
C5 C 0.4344(3) 0.7174(2) 0.32030(15) 0.0379(8) Uani 1 1 d . . . . .
N5 N 0.3350(3) 0.7445(2) 0.33879(15) 0.0554(8) Uani 1 1 d . . . . .
C6 C 0.6856(3) 0.7739(2) 0.26994(15) 0.0317(7) Uani 1 1 d . . . . .
N6 N 0.7764(3) 0.8408(2) 0.25745(14) 0.0499(7) Uani 1 1 d . . . . .
C11 C 0.3852(3) 0.41278(18) 0.09633(12) 0.0164(5) Uani 1 1 d . . . . .
C12 C 0.3988(3) 0.51442(19) 0.09847(12) 0.0192(5) Uani 1 1 d . . . . .
F12 F 0.35982(18) 0.53951(11) 0.03978(7) 0.0308(4) Uani 1 1 d . . . . .
C13 C 0.4512(3) 0.59375(18) 0.15929(13) 0.0203(5) Uani 1 1 d . . . . .
F13 F 0.45538(18) 0.68991(11) 0.15516(8) 0.0321(4) Uani 1 1 d . . . . .
C14 C 0.4981(3) 0.58049(18) 0.22256(12) 0.0179(5) Uani 1 1 d . . . . .
C15 C 0.4815(3) 0.47825(19) 0.22094(12) 0.0176(5) Uani 1 1 d . . . . .
F15 F 0.52139(16) 0.45379(11) 0.27974(7) 0.0262(4) Uani 1 1 d . . . . .
C16 C 0.4282(3) 0.39868(17) 0.16039(12) 0.0156(5) Uani 1 1 d . . . . .
F16 F 0.41900(16) 0.30187(10) 0.16420(7) 0.0220(3) Uani 1 1 d . . . . .
B3 B 0.4008(3) 0.2935(2) 0.38711(15) 0.0227(6) Uani 1 1 d . . . . .
C21 C 0.5273(3) 0.2638(2) 0.34269(14) 0.0240(6) Uani 1 1 d . . . . .
N21 N 0.6079(3) 0.23390(19) 0.30798(13) 0.0348(6) Uani 1 1 d . . . . .
C22 C 0.2667(3) 0.2829(2) 0.32864(14) 0.0264(6) Uani 1 1 d . . . . .
N22 N 0.1723(3) 0.26996(19) 0.28476(13) 0.0360(6) Uani 1 1 d . . . . .
C23 C 0.3419(3) 0.2051(2) 0.42661(14) 0.0248(6) Uani 1 1 d . . . . .
N23 N 0.3038(3) 0.14110(19) 0.45487(13) 0.0350(6) Uani 1 1 d . . . . .
C24 C 0.4559(3) 0.40488(19) 0.44490(13) 0.0225(6) Uani 1 1 d . . . . .
C25 C 0.3533(3) 0.4445(2) 0.47876(16) 0.0215(7) Uani 0.870(3) 1 d . . P A 1
F25 F 0.20390(18) 0.39114(13) 0.45950(9) 0.0299(5) Uani 0.870(3) 1 d . . P A 1
C26 C 0.3927(3) 0.5348(2) 0.53145(16) 0.0233(7) Uani 0.870(3) 1 d . . P A 1
F26 F 0.27888(18) 0.56462(13) 0.56061(9) 0.0322(5) Uani 0.870(3) 1 d . . P A 1
C27 C 0.412(2) 0.4883(19) 0.4409(11) 0.033(6) Uani 0.130(3) 1 d . . P A 2
F27 F 0.3267(14) 0.4905(9) 0.3825(6) 0.036(4) Uani 0.130(3) 1 d . . P A 2
C28 C 0.470(2) 0.5843(16) 0.4929(11) 0.026(5) Uani 0.130(3) 1 d . . P A 2
F28 F 0.4345(15) 0.6663(9) 0.4802(6) 0.038(4) Uani 0.130(3) 1 d . . P A 2
N30 N 0.9271(2) 0.43920(16) 0.19703(11) 0.0248(5) Uani 1 1 d . . . . .
C31 C 0.8728(3) 0.5334(2) 0.20976(15) 0.0308(6) Uani 1 1 d . . . . .
H31A H 0.8028 0.5260 0.1679 0.037 Uiso 1 1 calc R U . . .
H31B H 0.8138 0.5338 0.2501 0.037 Uiso 1 1 calc R U . . .
C32 C 0.9968(4) 0.6371(2) 0.22453(17) 0.0413(8) Uani 1 1 d . . . . .
H32A H 1.0607 0.6364 0.1865 0.062 Uiso 1 1 calc R U . . .
H32B H 1.0592 0.6499 0.2693 0.062 Uiso 1 1 calc R U . . .
H32C H 0.9507 0.6923 0.2273 0.062 Uiso 1 1 calc R U . . .
C33 C 1.0300(3) 0.4463(2) 0.26243(16) 0.0367(7) Uani 1 1 d . . . . .
H33A H 1.0709 0.3873 0.2520 0.044 Uiso 1 1 calc R U . . .
H33B H 1.1172 0.5110 0.2721 0.044 Uiso 1 1 calc R U . . .
C34 C 0.9542(4) 0.4452(3) 0.32740(16) 0.0451(8) Uani 1 1 d . . . . .
H34A H 0.9098 0.5017 0.3374 0.068 Uiso 1 1 calc R U . . .
H34B H 1.0294 0.4547 0.3672 0.068 Uiso 1 1 calc R U . . .
H34C H 0.8739 0.3785 0.3202 0.068 Uiso 1 1 calc R U . . .
C35 C 0.7864(3) 0.3457(2) 0.18291(15) 0.0312(7) Uani 1 1 d . . . . .
H35A H 0.7204 0.3455 0.1418 0.037 Uiso 1 1 calc R U . . .
H35B H 0.7298 0.3525 0.2240 0.037 Uiso 1 1 calc R U . . .
C36 C 0.8168(3) 0.2421(2) 0.16868(16) 0.0364(7) Uani 1 1 d . . . . .
H36A H 0.8724 0.2342 0.1279 0.055 Uiso 1 1 calc R U . . .
H36B H 0.7200 0.1855 0.1590 0.055 Uiso 1 1 calc R U . . .
H36C H 0.8777 0.2399 0.2100 0.055 Uiso 1 1 calc R U . . .
C37 C 1.0208(3) 0.4340(2) 0.13803(16) 0.0386(7) Uani 1 1 d . . . . .
H37A H 1.0589 0.3741 0.1343 0.046 Uiso 1 1 calc R U . . .
H37B H 1.1101 0.4977 0.1496 0.046 Uiso 1 1 calc R U . . .
C38 C 0.9366(4) 0.4231(3) 0.06625(17) 0.0493(9) Uani 1 1 d . . . . .
H38A H 1.0068 0.4228 0.0309 0.074 Uiso 1 1 calc R U . . .
H38B H 0.8974 0.4815 0.0693 0.074 Uiso 1 1 calc R U . . .
H38C H 0.8518 0.3578 0.0527 0.074 Uiso 1 1 calc R U . . .
N40 N 0.8336(2) 0.14260(16) 0.46045(11) 0.0223(5) Uani 0.821(4) 1 d . . P B -3
C41 C 0.8815(4) 0.1713(3) 0.39460(16) 0.0275(8) Uani 0.821(4) 1 d . . P B -3
H41A H 0.7961 0.1845 0.3705 0.033 Uiso 0.821(4) 1 calc R U P B -3
H41B H 0.9675 0.2370 0.4081 0.033 Uiso 0.821(4) 1 calc R U P B -3
C42 C 0.9283(4) 0.0922(3) 0.34360(18) 0.0343(9) Uani 0.821(4) 1 d . . P B -3
H42A H 0.8426 0.0276 0.3279 0.051 Uiso 0.821(4) 1 calc R U P B -3
H42B H 1.0138 0.0788 0.3665 0.051 Uiso 0.821(4) 1 calc R U P B -3
H42C H 0.9593 0.1181 0.3029 0.051 Uiso 0.821(4) 1 calc R U P B -3
C43 C 0.7600(4) 0.2186(3) 0.49974(17) 0.0285(8) Uani 0.821(4) 1 d . . P B -3
H43A H 0.6752 0.2193 0.4676 0.034 Uiso 0.821(4) 1 calc R U P B -3
H43B H 0.7160 0.1932 0.5392 0.034 Uiso 0.821(4) 1 calc R U P B -3
C44 C 0.8641(7) 0.3278(5) 0.5286(3) 0.0428(13) Uani 0.821(4) 1 d . . P B -3
H44A H 0.9092 0.3540 0.4901 0.064 Uiso 0.821(4) 1 calc R U P B -3
H44B H 0.9449 0.3291 0.5631 0.064 Uiso 0.821(4) 1 calc R U P B -3
H44C H 0.8063 0.3719 0.5515 0.064 Uiso 0.821(4) 1 calc R U P B -3
C45 C 0.9725(4) 0.1462(2) 0.50609(15) 0.0212(7) Uani 0.821(4) 1 d . . P B -3
H45A H 1.0152 0.0936 0.4799 0.025 Uiso 0.821(4) 1 calc R U P B -3
H45B H 1.0497 0.2151 0.5129 0.025 Uiso 0.821(4) 1 calc R U P B -3
C46 C 0.9495(4) 0.1282(3) 0.57694(17) 0.0310(9) Uani 0.821(4) 1 d . . P B -3
H46A H 0.8900 0.0554 0.5714 0.047 Uiso 0.821(4) 1 calc R U P B -3
H46B H 0.8949 0.1734 0.6015 0.047 Uiso 0.821(4) 1 calc R U P B -3
H46C H 1.0485 0.1439 0.6044 0.047 Uiso 0.821(4) 1 calc R U P B -3
C47 C 0.7222(4) 0.0342(2) 0.44486(17) 0.0245(8) Uani 0.821(4) 1 d . . P B -3
H47A H 0.6932 0.0198 0.4899 0.029 Uiso 0.821(4) 1 calc R U P B -3
H47B H 0.7737 -0.0159 0.4231 0.029 Uiso 0.821(4) 1 calc R U P B -3
C48 C 0.5791(4) 0.0160(3) 0.3965(2) 0.0320(9) Uani 0.821(4) 1 d . . P B -3
H48A H 0.6064 0.0310 0.3520 0.048 Uiso 0.821(4) 1 calc R U P B -3
H48B H 0.5232 0.0617 0.4190 0.048 Uiso 0.821(4) 1 calc R U P B -3
H48C H 0.5150 -0.0566 0.3873 0.048 Uiso 0.821(4) 1 calc R U P B -3
N50 N 0.8336(2) 0.14260(16) 0.46045(11) 0.0223(5) Uani 0.179(4) 1 d D . P B -4
C50 C 0.885(2) 0.0959(18) 0.3916(5) 0.064(6) Uani 0.179(4) 1 d D U P B -4
H50A H 0.9972 0.1272 0.3968 0.077 Uiso 0.179(4) 1 calc R U P B -4
H50B H 0.8644 0.0210 0.3877 0.077 Uiso 0.179(4) 1 calc R U P B -4
C51 C 0.822(3) 0.1046(18) 0.3219(8) 0.062(6) Uani 0.179(4) 1 d D U P B -4
H51A H 0.8586 0.0628 0.2835 0.094 Uiso 0.179(4) 1 calc R U P B -4
H51B H 0.8569 0.1774 0.3206 0.094 Uiso 0.179(4) 1 calc R U P B -4
H51C H 0.7111 0.0791 0.3165 0.094 Uiso 0.179(4) 1 calc R U P B -4
C52 C 0.878(2) 0.2590(5) 0.4703(9) 0.054(5) Uani 0.179(4) 1 d D U P B -4
H52A H 0.9778 0.2819 0.4535 0.065 Uiso 0.179(4) 1 calc R U P B -4
H52B H 0.8031 0.2726 0.4395 0.065 Uiso 0.179(4) 1 calc R U P B -4
C53 C 0.888(6) 0.326(4) 0.5441(13) 0.094(11) Uani 0.179(4) 1 d D U P B -4
H53A H 0.9882 0.3794 0.5570 0.141 Uiso 0.179(4) 1 calc R U P B -4
H53B H 0.8752 0.2823 0.5771 0.141 Uiso 0.179(4) 1 calc R U P B -4
H53C H 0.8087 0.3587 0.5461 0.141 Uiso 0.179(4) 1 calc R U P B -4
C54 C 0.6614(6) 0.1040(9) 0.4461(7) 0.027(4) Uani 0.179(4) 1 d D U P B -4
H54A H 0.6199 0.1303 0.4893 0.032 Uiso 0.179(4) 1 calc R U P B -4
H54B H 0.6286 0.1328 0.4090 0.032 Uiso 0.179(4) 1 calc R U P B -4
C55 C 0.596(3) -0.0129(10) 0.4230(12) 0.051(6) Uani 0.179(4) 1 d D U P B -4
H55A H 0.4875 -0.0340 0.4280 0.077 Uiso 0.179(4) 1 calc R U P B -4
H55B H 0.6490 -0.0428 0.4523 0.077 Uiso 0.179(4) 1 calc R U P B -4
H55C H 0.6088 -0.0380 0.3736 0.077 Uiso 0.179(4) 1 calc R U P B -4
C56 C 0.895(2) 0.1115(14) 0.5213(7) 0.129(11) Uani 0.179(4) 1 d D U P B -4
H56A H 0.8335 0.0391 0.5182 0.155 Uiso 0.179(4) 1 calc R U P B -4
H56B H 1.0000 0.1114 0.5147 0.155 Uiso 0.179(4) 1 calc R U P B -4
C57 C 0.899(5) 0.176(3) 0.5947(11) 0.131(11) Uani 0.179(4) 1 d D U P B -4
H57A H 0.7961 0.1749 0.6033 0.196 Uiso 0.179(4) 1 calc R U P B -4
H57B H 0.9632 0.2477 0.5997 0.196 Uiso 0.179(4) 1 calc R U P B -4
H57C H 0.9418 0.1476 0.6288 0.196 Uiso 0.179(4) 1 calc R U P B -4
N60 N 0.2449(2) -0.04308(15) 0.15139(10) 0.0211(5) Uani 0.868(3) 1 d . . P C -5
C60 C 0.2979(3) 0.0350(2) 0.10993(17) 0.0264(7) Uani 0.868(3) 1 d . . P C -5
H60A H 0.4037 0.0785 0.1296 0.032 Uiso 0.868(3) 1 calc R U P C -5
H60B H 0.2341 0.0812 0.1163 0.032 Uiso 0.868(3) 1 calc R U P C -5
C61 C 0.2927(9) -0.0112(7) 0.0316(4) 0.0323(16) Uani 0.868(3) 1 d . . P C -5
H61A H 0.1870 -0.0483 0.0105 0.048 Uiso 0.868(3) 1 calc R U P C -5
H61B H 0.3515 -0.0597 0.0245 0.048 Uiso 0.868(3) 1 calc R U P C -5
H61C H 0.3363 0.0445 0.0093 0.048 Uiso 0.868(3) 1 calc R U P C -5
C62 C 0.0819(3) -0.1101(2) 0.12571(15) 0.0238(7) Uani 0.868(3) 1 d . . P C -5
H62A H 0.0755 -0.1491 0.0761 0.029 Uiso 0.868(3) 1 calc R U P C -5
H62B H 0.0534 -0.1616 0.1536 0.029 Uiso 0.868(3) 1 calc R U P C -5
C63 C -0.0328(4) -0.0525(3) 0.1301(2) 0.0288(9) Uani 0.868(3) 1 d . . P C -5
H63A H -0.0087 -0.0033 0.1011 0.043 Uiso 0.868(3) 1 calc R U P C -5
H63B H -0.0294 -0.0146 0.1792 0.043 Uiso 0.868(3) 1 calc R U P C -5
H63C H -0.1349 -0.1021 0.1129 0.043 Uiso 0.868(3) 1 calc R U P C -5
C64 C 0.2614(4) 0.0179(2) 0.22730(15) 0.0305(8) Uani 0.868(3) 1 d . . P C -5
H64A H 0.3697 0.0594 0.2426 0.037 Uiso 0.868(3) 1 calc R U P C -5
H64B H 0.2029 0.0672 0.2299 0.037 Uiso 0.868(3) 1 calc R U P C -5
C65 C 0.2096(5) -0.0455(4) 0.2783(2) 0.0401(11) Uani 0.868(3) 1 d . . P C -5
H65A H 0.0997 -0.0808 0.2672 0.060 Uiso 0.868(3) 1 calc R U P C -5
H65B H 0.2328 0.0002 0.3263 0.060 Uiso 0.868(3) 1 calc R U P C -5
H65C H 0.2625 -0.0973 0.2746 0.060 Uiso 0.868(3) 1 calc R U P C -5
C66 C 0.3397(3) -0.1162(2) 0.14391(16) 0.0245(7) Uani 0.868(3) 1 d . . P C -5
H66A H 0.3058 -0.1633 0.1744 0.029 Uiso 0.868(3) 1 calc R U P C -5
H66B H 0.3188 -0.1596 0.0946 0.029 Uiso 0.868(3) 1 calc R U P C -5
C67 C 0.5085(6) -0.0642(4) 0.1623(3) 0.0344(12) Uani 0.868(3) 1 d . . P C -5
H67A H 0.5591 -0.1170 0.1597 0.052 Uiso 0.868(3) 1 calc R U P C -5
H67B H 0.5307 -0.0182 0.2102 0.052 Uiso 0.868(3) 1 calc R U P C -5
H67C H 0.5457 -0.0234 0.1291 0.052 Uiso 0.868(3) 1 calc R U P C -5
N70 N 0.2449(2) -0.04308(15) 0.15139(10) 0.0211(5) Uani 0.132(3) 1 d . . P C -6
C70 C 0.223(2) -0.0972(14) 0.0710(9) 0.017(4) Uani 0.132(3) 1 d . U P C -6
H70A H 0.2855 -0.1441 0.0632 0.021 Uiso 0.132(3) 1 calc R U P C -6
H70B H 0.1153 -0.1408 0.0567 0.021 Uiso 0.132(3) 1 calc R U P C -6
C71 C 0.264(5) -0.025(4) 0.024(3) 0.017(9) Uani 0.132(3) 1 d . U P C -6
H71A H 0.2624 -0.0662 -0.0244 0.025 Uiso 0.132(3) 1 calc R U P C -6
H71B H 0.3654 0.0246 0.0409 0.025 Uiso 0.132(3) 1 calc R U P C -6
H71C H 0.1895 0.0119 0.0236 0.025 Uiso 0.132(3) 1 calc R U P C -6
C72 C 0.156(2) 0.0365(15) 0.1633(10) 0.023(5) Uani 0.132(3) 1 d . U P C -6
H72A H 0.1766 0.0750 0.2137 0.028 Uiso 0.132(3) 1 calc R U P C -6
H72B H 0.1954 0.0873 0.1359 0.028 Uiso 0.132(3) 1 calc R U P C -6
C73 C -0.015(3) -0.0098(19) 0.1429(14) 0.023(7) Uani 0.132(3) 1 d . U P C -6
H73A H -0.0372 -0.0470 0.0928 0.034 Uiso 0.132(3) 1 calc R U P C -6
H73B H -0.0607 0.0458 0.1518 0.034 Uiso 0.132(3) 1 calc R U P C -6
H73C H -0.0562 -0.0583 0.1709 0.034 Uiso 0.132(3) 1 calc R U P C -6
C74 C 0.190(2) -0.1245(14) 0.1869(9) 0.020(4) Uani 0.132(3) 1 d . U P C -6
H74A H 0.2535 -0.1709 0.1780 0.025 Uiso 0.132(3) 1 calc R U P C -6
H74B H 0.0849 -0.1664 0.1653 0.025 Uiso 0.132(3) 1 calc R U P C -6
C75 C 0.191(4) -0.086(2) 0.2688(17) 0.030(8) Uani 0.132(3) 1 d . U P C -6
H75A H 0.2964 -0.0536 0.2918 0.045 Uiso 0.132(3) 1 calc R U P C -6
H75B H 0.1421 -0.1459 0.2868 0.045 Uiso 0.132(3) 1 calc R U P C -6
H75C H 0.1358 -0.0360 0.2788 0.045 Uiso 0.132(3) 1 calc R U P C -6
C76 C 0.406(2) 0.0274(16) 0.1773(11) 0.031(5) Uani 0.132(3) 1 d . U P C -6
H76A H 0.4110 0.0657 0.2270 0.037 Uiso 0.132(3) 1 calc R U P C -6
H76B H 0.4316 0.0790 0.1495 0.037 Uiso 0.132(3) 1 calc R U P C -6
C77 C 0.525(5) -0.030(2) 0.172(2) 0.030(9) Uani 0.132(3) 1 d . U P C -6
H77A H 0.5156 -0.0724 0.1239 0.046 Uiso 0.132(3) 1 calc R U P C -6
H77B H 0.5084 -0.0746 0.2044 0.046 Uiso 0.132(3) 1 calc R U P C -6
H77C H 0.6272 0.0211 0.1853 0.046 Uiso 0.132(3) 1 calc R U P C -6


_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 1.589(4) . ?
B1 C1 1.597(4) . ?
B1 C2 1.603(4) . ?
B1 C11 1.615(3) . ?
C1 N1 1.145(3) . ?
C2 N2 1.136(3) . ?
C3 N3 1.134(3) . ?
B2 C5 1.578(4) . ?
B2 C4 1.587(4) . ?
B2 C6 1.602(4) . ?
B2 C14 1.623(4) . ?
C4 N4 1.128(3) . ?
C5 N5 1.143(4) . ?
C6 N6 1.145(4) . ?
C11 C12 1.380(3) . ?
C11 C16 1.382(3) . ?
C12 F12 1.350(3) . ?
C12 C13 1.376(3) . ?
C13 F13 1.356(3) . ?
C13 C14 1.373(3) . ?
C14 C15 1.384(3) . ?
C15 F15 1.350(3) . ?
C15 C16 1.374(3) . ?
C16 F16 1.352(3) . ?
B3 C23 1.593(4) . ?
B3 C21 1.595(4) . ?
B3 C22 1.602(4) . ?
B3 C24 1.615(4) . ?
C21 N21 1.143(3) . ?
C22 N22 1.142(3) . ?
C23 N23 1.144(3) . ?
C24 C28 1.33(2) 2_666 ?
C24 C27 1.37(2) . ?
C24 C25 1.365(4) . ?
C24 C26 1.396(4) 2_666 ?
C25 F25 1.351(3) . ?
C25 C26 1.368(4) . ?
C26 F26 1.354(3) . ?
C26 C24 1.396(4) 2_666 ?
C27 F27 1.37(2) . ?
C27 C28 1.42(3) . ?
C28 C24 1.33(2) 2_666 ?
C28 F28 1.36(2) . ?
N30 C37 1.490(3) . ?
N30 C35 1.507(3) . ?
N30 C31 1.518(3) . ?
N30 C33 1.531(3) . ?
C31 C32 1.513(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.495(4) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.522(4) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.534(4) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
N40 C41 1.500(4) . ?
N40 C47 1.509(4) . ?
N40 C43 1.514(4) . ?
N40 C45 1.516(3) . ?
C41 C42 1.492(5) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.499(7) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.494(4) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C48 1.515(4) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
N50 C56 1.511(5) . ?
N50 C52 1.517(5) . ?
N50 C54 1.517(5) . ?
N50 C50 1.528(5) . ?
C50 C51 1.512(5) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 C53 1.512(5) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 C55 1.510(5) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 C57 1.504(5) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
N60 C60 1.502(4) . ?
N60 C62 1.511(3) . ?
N60 C64 1.511(3) . ?
N60 C66 1.523(3) . ?
C60 C61 1.519(9) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 C63 1.510(5) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 C65 1.501(6) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 C67 1.503(6) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
N70 C74 1.457(18) . ?
N70 C76 1.51(2) . ?
N70 C72 1.556(19) . ?
N70 C70 1.559(17) . ?
C70 C71 1.51(6) . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C72 C73 1.51(3) . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C74 C75 1.58(4) . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C76 C77 1.54(4) . ?
C76 H76A 0.9900 . ?
C76 H76B 0.9900 . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?

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 105.8(2) . . ?
C3 B1 C2 109.7(2) . . ?
C1 B1 C2 108.1(2) . . ?
C3 B1 C11 115.1(2) . . ?
C1 B1 C11 109.0(2) . . ?
C2 B1 C11 108.90(19) . . ?
N1 C1 B1 177.8(3) . . ?
N2 C2 B1 176.8(3) . . ?
N3 C3 B1 175.6(3) . . ?
C5 B2 C4 112.1(2) . . ?
C5 B2 C6 107.6(2) . . ?
C4 B2 C6 103.9(2) . . ?
C5 B2 C14 108.7(2) . . ?
C4 B2 C14 113.5(2) . . ?
C6 B2 C14 110.9(2) . . ?
N4 C4 B2 174.6(3) . . ?
N5 C5 B2 177.1(3) . . ?
N6 C6 B2 175.8(3) . . ?
C12 C11 C16 113.9(2) . . ?
C12 C11 B1 126.3(2) . . ?
C16 C11 B1 119.8(2) . . ?
F12 C12 C13 117.3(2) . . ?
F12 C12 C11 120.4(2) . . ?
C13 C12 C11 122.4(2) . . ?
F13 C13 C14 119.3(2) . . ?
F13 C13 C12 116.9(2) . . ?
C14 C13 C12 123.8(2) . . ?
C13 C14 C15 113.9(2) . . ?
C13 C14 B2 120.9(2) . . ?
C15 C14 B2 125.2(2) . . ?
F15 C15 C16 117.4(2) . . ?
F15 C15 C14 120.2(2) . . ?
C16 C15 C14 122.4(2) . . ?
F16 C16 C15 117.7(2) . . ?
F16 C16 C11 118.8(2) . . ?
C15 C16 C11 123.5(2) . . ?
C23 B3 C21 106.1(2) . . ?
C23 B3 C22 108.5(2) . . ?
C21 B3 C22 104.2(2) . . ?
C23 B3 C24 108.5(2) . . ?
C21 B3 C24 116.1(2) . . ?
C22 B3 C24 113.0(2) . . ?
N21 C21 B3 173.6(3) . . ?
N22 C22 B3 175.9(3) . . ?
N23 C23 B3 177.9(3) . . ?
C28 C24 C27 113.8(12) 2_666 . ?
C25 C24 C26 114.0(2) . 2_666 ?
C28 C24 B3 120.1(8) 2_666 . ?
C27 C24 B3 125.2(9) . . ?
C25 C24 B3 120.9(2) . . ?
C26 C24 B3 124.9(2) 2_666 . ?
F25 C25 C24 118.2(2) . . ?
F25 C25 C26 117.9(3) . . ?
C24 C25 C26 123.9(3) . . ?
F26 C26 C25 117.6(3) . . ?
F26 C26 C24 120.4(3) . 2_666 ?
C25 C26 C24 122.0(3) . 2_666 ?
C24 C27 F27 123.0(16) . . ?
C24 C27 C28 121.2(16) . . ?
F27 C27 C28 115.2(19) . . ?
C24 C28 F28 119.2(16) 2_666 . ?
C24 C28 C27 123.5(16) 2_666 . ?
F28 C28 C27 116.9(17) . . ?
C37 N30 C35 112.0(2) . . ?
C37 N30 C31 112.1(2) . . ?
C35 N30 C31 106.28(19) . . ?
C37 N30 C33 106.1(2) . . ?
C35 N30 C33 110.8(2) . . ?
C31 N30 C33 109.5(2) . . ?
C32 C31 N30 115.4(2) . . ?
C32 C31 H31A 108.4 . . ?
N30 C31 H31A 108.4 . . ?
C32 C31 H31B 108.4 . . ?
N30 C31 H31B 108.4 . . ?
H31A C31 H31B 107.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 N30 114.9(2) . . ?
C34 C33 H33A 108.5 . . ?
N30 C33 H33A 108.5 . . ?
C34 C33 H33B 108.5 . . ?
N30 C33 H33B 108.5 . . ?
H33A C33 H33B 107.5 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N30 C35 C36 114.5(2) . . ?
N30 C35 H35A 108.6 . . ?
C36 C35 H35A 108.6 . . ?
N30 C35 H35B 108.6 . . ?
C36 C35 H35B 108.6 . . ?
H35A C35 H35B 107.6 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N30 C37 C38 114.6(2) . . ?
N30 C37 H37A 108.6 . . ?
C38 C37 H37A 108.6 . . ?
N30 C37 H37B 108.6 . . ?
C38 C37 H37B 108.6 . . ?
H37A C37 H37B 107.6 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C41 N40 C47 112.0(2) . . ?
C41 N40 C43 109.4(2) . . ?
C47 N40 C43 108.8(2) . . ?
C41 N40 C45 109.0(2) . . ?
C47 N40 C45 107.7(2) . . ?
C43 N40 C45 110.0(2) . . ?
C42 C41 N40 115.3(3) . . ?
C42 C41 H41A 108.4 . . ?
N40 C41 H41A 108.4 . . ?
C42 C41 H41B 108.4 . . ?
N40 C41 H41B 108.4 . . ?
H41A C41 H41B 107.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 N40 115.1(3) . . ?
C44 C43 H43A 108.5 . . ?
N40 C43 H43A 108.5 . . ?
C44 C43 H43B 108.5 . . ?
N40 C43 H43B 108.5 . . ?
H43A C43 H43B 107.5 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 N40 116.9(3) . . ?
C46 C45 H45A 108.1 . . ?
N40 C45 H45A 108.1 . . ?
C46 C45 H45B 108.1 . . ?
N40 C45 H45B 108.1 . . ?
H45A C45 H45B 107.3 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N40 C47 C48 114.4(3) . . ?
N40 C47 H47A 108.7 . . ?
C48 C47 H47A 108.7 . . ?
N40 C47 H47B 108.7 . . ?
C48 C47 H47B 108.7 . . ?
H47A C47 H47B 107.6 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C56 N50 C52 114.2(7) . . ?
C56 N50 C54 113.2(7) . . ?
C52 N50 C54 105.0(9) . . ?
C56 N50 C50 111.4(7) . . ?
C52 N50 C50 107.6(12) . . ?
C54 N50 C50 104.8(10) . . ?
C51 C50 N50 121.2(13) . . ?
C51 C50 H50A 107.0 . . ?
N50 C50 H50A 107.0 . . ?
C51 C50 H50B 107.0 . . ?
N50 C50 H50B 107.0 . . ?
H50A C50 H50B 106.8 . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C53 C52 N50 117(2) . . ?
C53 C52 H52A 108.1 . . ?
N50 C52 H52A 108.1 . . ?
C53 C52 H52B 108.1 . . ?
N50 C52 H52B 108.1 . . ?
H52A C52 H52B 107.3 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C55 C54 N50 113.0(12) . . ?
C55 C54 H54A 109.0 . . ?
N50 C54 H54A 109.0 . . ?
C55 C54 H54B 109.0 . . ?
N50 C54 H54B 109.0 . . ?
H54A C54 H54B 107.8 . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C57 C56 N50 118.0(18) . . ?
C57 C56 H56A 107.8 . . ?
N50 C56 H56A 107.8 . . ?
C57 C56 H56B 107.8 . . ?
N50 C56 H56B 107.8 . . ?
H56A C56 H56B 107.2 . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C60 N60 C62 111.5(2) . . ?
C60 N60 C64 106.6(2) . . ?
C62 N60 C64 110.7(2) . . ?
C60 N60 C66 111.0(2) . . ?
C62 N60 C66 106.7(2) . . ?
C64 N60 C66 110.5(2) . . ?
N60 C60 C61 114.8(4) . . ?
N60 C60 H60A 108.6 . . ?
C61 C60 H60A 108.6 . . ?
N60 C60 H60B 108.6 . . ?
C61 C60 H60B 108.6 . . ?
H60A C60 H60B 107.5 . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C60 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C63 C62 N60 115.3(3) . . ?
C63 C62 H62A 108.4 . . ?
N60 C62 H62A 108.4 . . ?
C63 C62 H62B 108.4 . . ?
N60 C62 H62B 108.4 . . ?
H62A C62 H62B 107.5 . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C65 C64 N60 115.6(3) . . ?
C65 C64 H64A 108.4 . . ?
N60 C64 H64A 108.4 . . ?
C65 C64 H64B 108.4 . . ?
N60 C64 H64B 108.4 . . ?
H64A C64 H64B 107.4 . . ?
C64 C65 H65A 109.5 . . ?
C64 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C64 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C67 C66 N60 115.3(3) . . ?
C67 C66 H66A 108.4 . . ?
N60 C66 H66A 108.4 . . ?
C67 C66 H66B 108.4 . . ?
N60 C66 H66B 108.4 . . ?
H66A C66 H66B 107.5 . . ?
C66 C67 H67A 109.5 . . ?
C66 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C66 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C74 N70 C76 115.3(11) . . ?
C74 N70 C72 112.9(10) . . ?
C76 N70 C72 101.3(11) . . ?
C74 N70 C70 107.1(10) . . ?
C76 N70 C70 111.8(11) . . ?
C72 N70 C70 108.4(10) . . ?
C71 C70 N70 116(2) . . ?
C71 C70 H70A 108.3 . . ?
N70 C70 H70A 108.3 . . ?
C71 C70 H70B 108.3 . . ?
N70 C70 H70B 108.3 . . ?
H70A C70 H70B 107.4 . . ?
C70 C71 H71A 109.5 . . ?
C70 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
C70 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C73 C72 N70 115.3(16) . . ?
C73 C72 H72A 108.5 . . ?
N70 C72 H72A 108.5 . . ?
C73 C72 H72B 108.5 . . ?
N70 C72 H72B 108.5 . . ?
H72A C72 H72B 107.5 . . ?
C72 C73 H73A 109.5 . . ?
C72 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C72 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
N70 C74 C75 115.8(16) . . ?
N70 C74 H74A 108.3 . . ?
C75 C74 H74A 108.3 . . ?
N70 C74 H74B 108.3 . . ?
C75 C74 H74B 108.3 . . ?
H74A C74 H74B 107.4 . . ?
C74 C75 H75A 109.5 . . ?
C74 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
C74 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
N70 C76 C77 114.1(19) . . ?
N70 C76 H76A 108.7 . . ?
C77 C76 H76A 108.7 . . ?
N70 C76 H76B 108.7 . . ?
C77 C76 H76B 108.7 . . ?
H76A C76 H76B 107.6 . . ?
C76 C77 H77A 109.5 . . ?
C76 C77 H77B 109.5 . . ?
H77A C77 H77B 109.5 . . ?
C76 C77 H77C 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?

_refine_diff_density_max         0.746
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.059

####################################################################### 
# 
# 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_JL076_JL_KB3a
_database_code_depnum_ccdc_archive 'CCDC 1548902'
_audit_update_record             
;
2017-05-09 deposited with the CCDC.
2017-06-26 downloaded from the CCDC.
;


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


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H3 B F2 K N3'
_chemical_formula_sum            'C9 H3 B F2 K N3'
_chemical_formula_weight         241.05

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'
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'

_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                   7.2218(4)
_cell_length_b                   7.3375(4)
_cell_length_c                   11.5902(7)
_cell_angle_alpha                100.165(2)
_cell_angle_beta                 95.640(2)
_cell_angle_gamma                116.645(2)
_cell_volume                     529.22(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5850
_cell_measurement_theta_min      3.21
_cell_measurement_theta_max      26.80

_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).
;
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_F_000             240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.500
_shelx_estimated_absorpt_T_min   0.844
_shelx_estimated_absorpt_T_max   0.929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7072
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7270
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.822
_diffrn_reflns_theta_max         26.798
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2258
_reflns_number_gt                2100
_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. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0490P)²+0.6556P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2258
_refine_ls_number_parameters     145
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0389
_refine_ls_wR_factor_ref         0.1059
_refine_ls_wR_factor_gt          0.1042
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_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 -0.16517(6) 0.17798(6) 1.01353(4) 0.01873(14) Uani 1 1 d . . . . .
N1 N 0.8056(3) 0.4354(3) 0.86461(16) 0.0220(4) Uani 1 1 d . . . . .
C1 C 0.6467(3) 0.4219(3) 0.82577(17) 0.0167(4) Uani 1 1 d . . . . .
F1 F -0.0936(2) 0.2289(3) 0.41145(15) 0.0457(4) Uani 1 1 d . . . . .
B1 B 0.4242(3) 0.4086(3) 0.77899(19) 0.0149(4) Uani 1 1 d . . . . .
F2 F 0.0453(2) 0.3679(2) 0.65099(12) 0.0283(3) Uani 1 1 d . . . . .
N2 N 0.1422(3) 0.1443(3) 0.89303(16) 0.0202(4) Uani 1 1 d . . . . .
C2 C 0.2583(3) 0.2563(3) 0.84613(17) 0.0162(4) Uani 1 1 d . . . . .
C3 C 0.4536(3) 0.6407(3) 0.82773(17) 0.0165(4) Uani 1 1 d . . . . .
N3 N 0.4804(3) 0.8079(3) 0.86458(16) 0.0215(4) Uani 1 1 d . . . . .
C11 C 0.3477(3) 0.3252(3) 0.63620(17) 0.0163(4) Uani 1 1 d . . . . .
C12 C 0.1611(3) 0.3119(3) 0.58213(19) 0.0209(4) Uani 1 1 d . . . . .
C13 C 0.0887(4) 0.2414(4) 0.4595(2) 0.0292(5) Uani 1 1 d . . . . .
C14 C 0.2005(4) 0.1803(3) 0.3872(2) 0.0320(6) Uani 1 1 d . . . . .
H14 H 0.1503 0.1316 0.3030 0.038 Uiso 1 1 calc R U . . .
C15 C 0.3866(4) 0.1903(3) 0.4382(2) 0.0288(5) Uani 1 1 d . . . . .
H15 H 0.4647 0.1475 0.3889 0.035 Uiso 1 1 calc R U . . .
C16 C 0.4604(4) 0.2625(3) 0.56103(19) 0.0217(4) Uani 1 1 d . . . . .
H16 H 0.5895 0.2696 0.5948 0.026 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 N2 2.8140(18) . ?
K1 N3 2.8248(18) 2_567 ?
K1 N2 2.8309(18) 2_557 ?
K1 N1 2.8334(19) 1_455 ?
K1 N1 2.8358(19) 2_667 ?
K1 N3 2.8545(19) 1_445 ?
K1 C3 3.445(2) 2_567 ?
K1 K1 4.2496(8) 2_557 ?
K1 K1 4.2885(8) 2_457 ?
K1 K1 4.3219(9) 2_567 ?
N1 C1 1.145(3) . ?
N1 K1 2.8334(19) 1_655 ?
N1 K1 2.8359(18) 2_667 ?
C1 B1 1.598(3) . ?
F1 C13 1.335(3) . ?
B1 C3 1.605(3) . ?
B1 C11 1.606(3) . ?
B1 C2 1.606(3) . ?
F2 C12 1.352(3) . ?
N2 C2 1.142(3) . ?
N2 K1 2.8309(18) 2_557 ?
C3 N3 1.145(3) . ?
C3 K1 3.445(2) 2_567 ?
N3 K1 2.8247(18) 2_567 ?
N3 K1 2.8545(18) 1_665 ?
C11 C12 1.383(3) . ?
C11 C16 1.402(3) . ?
C12 C13 1.383(3) . ?
C13 C14 1.372(4) . ?
C14 C15 1.379(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.387(3) . ?
C15 H15 0.9500 . ?
C16 H16 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
N2 K1 N3 177.29(5) . 2_567 ?
N2 K1 N2 82.33(5) . 2_557 ?
N3 K1 N2 95.20(5) 2_567 2_557 ?
N2 K1 N1 87.78(5) . 1_455 ?
N3 K1 N1 94.45(5) 2_567 1_455 ?
N2 K1 N1 165.53(5) 2_557 1_455 ?
N2 K1 N1 80.16(5) . 2_667 ?
N3 K1 N1 101.70(5) 2_567 2_667 ?
N2 K1 N1 107.82(5) 2_557 2_667 ?
N1 K1 N1 80.66(6) 1_455 2_667 ?
N2 K1 N3 96.44(5) . 1_445 ?
N3 K1 N3 81.93(6) 2_567 1_445 ?
N2 K1 N3 77.76(5) 2_557 1_445 ?
N1 K1 N3 92.97(5) 1_455 1_445 ?
N1 K1 N3 172.85(5) 2_667 1_445 ?
N2 K1 C3 164.82(5) . 2_567 ?
N3 K1 C3 17.75(5) 2_567 2_567 ?
N2 K1 C3 108.54(5) 2_557 2_567 ?
N1 K1 C3 83.27(5) 1_455 2_567 ?
N1 K1 C3 86.30(5) 2_667 2_567 ?
N3 K1 C3 96.24(5) 1_445 2_567 ?
N2 K1 K1 41.32(4) . 2_557 ?
N3 K1 K1 136.20(4) 2_567 2_557 ?
N2 K1 K1 41.02(4) 2_557 2_557 ?
N1 K1 K1 128.27(4) 1_455 2_557 ?
N1 K1 K1 95.20(4) 2_667 2_557 ?
N3 K1 K1 86.16(4) 1_445 2_557 ?
C3 K1 K1 148.32(4) 2_567 2_557 ?
N2 K1 K1 137.10(4) . 2_457 ?
N3 K1 K1 41.23(4) 2_567 2_457 ?
N2 K1 K1 85.33(4) 2_557 2_457 ?
N1 K1 K1 94.91(4) 1_455 2_457 ?
N1 K1 K1 142.56(4) 2_667 2_457 ?
N3 K1 K1 40.70(4) 1_445 2_457 ?
C3 K1 K1 56.29(3) 2_567 2_457 ?
K1 K1 K1 115.521(19) 2_557 2_457 ?
N2 K1 K1 82.09(4) . 2_567 ?
N3 K1 K1 100.60(4) 2_567 2_567 ?
N2 K1 K1 146.68(4) 2_557 2_567 ?
N1 K1 K1 40.35(4) 1_455 2_567 ?
N1 K1 K1 40.31(4) 2_667 2_567 ?
N3 K1 K1 133.24(4) 1_445 2_567 ?
C3 K1 K1 83.15(4) 2_567 2_567 ?
K1 K1 K1 117.745(19) 2_557 2_567 ?
K1 K1 K1 125.25(2) 2_457 2_567 ?
C1 N1 K1 121.81(15) . 1_655 ?
C1 N1 K1 123.64(15) . 2_667 ?
K1 N1 K1 99.34(6) 1_655 2_667 ?
N1 C1 B1 176.8(2) . . ?
C1 B1 C3 105.75(15) . . ?
C1 B1 C11 112.96(16) . . ?
C3 B1 C11 112.61(16) . . ?
C1 B1 C2 106.27(16) . . ?
C3 B1 C2 107.36(16) . . ?
C11 B1 C2 111.44(16) . . ?
C2 N2 K1 130.95(15) . . ?
C2 N2 K1 128.89(15) . 2_557 ?
K1 N2 K1 97.67(5) . 2_557 ?
N2 C2 B1 178.2(2) . . ?
N3 C3 B1 177.9(2) . . ?
N3 C3 K1 48.76(12) . 2_567 ?
B1 C3 K1 132.25(12) . 2_567 ?
C3 N3 K1 113.49(14) . 2_567 ?
C3 N3 K1 132.31(15) . 1_665 ?
K1 N3 K1 98.07(5) 2_567 1_665 ?
C12 C11 C16 116.95(19) . . ?
C12 C11 B1 119.62(18) . . ?
C16 C11 B1 123.43(18) . . ?
F2 C12 C13 119.0(2) . . ?
F2 C12 C11 119.19(18) . . ?
C13 C12 C11 121.8(2) . . ?
F1 C13 C14 119.7(2) . . ?
F1 C13 C12 119.7(2) . . ?
C14 C13 C12 120.6(2) . . ?
C13 C14 C15 119.1(2) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
C14 C15 C16 120.4(2) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C15 C16 C11 121.1(2) . . ?
C15 C16 H16 119.4 . . ?
C11 C16 H16 119.4 . . ?

_refine_diff_density_max         1.575
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.069

####################################################################### 
# 
# 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_JL088_JL_KB3c
_database_code_depnum_ccdc_archive 'CCDC 1548903'
_audit_update_record             
;
2017-05-09 deposited with the CCDC.
2017-06-26 downloaded from the CCDC.
;


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

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H3 B F2 K N3'
_chemical_formula_sum            'C9 H3 B F2 K N3'
_chemical_formula_weight         241.05

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'
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'

_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                   7.3664(11)
_cell_length_b                   21.174(3)
_cell_length_c                   7.3900(11)
_cell_angle_alpha                90
_cell_angle_beta                 117.188(4)
_cell_angle_gamma                90
_cell_volume                     1025.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2367
_cell_measurement_theta_min      3.24
_cell_measurement_theta_max      26.35
_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).
;

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_F_000             480
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.516
_shelx_estimated_absorpt_T_min   0.882
_shelx_estimated_absorpt_T_max   0.960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6401
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8062
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.924
_diffrn_reflns_theta_max         26.802
_diffrn_reflns_theta_full        26.000
_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             2198
_reflns_number_gt                1765
_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. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0310P)²+0.3899P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2198
_refine_ls_number_parameters     157
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0336
_refine_ls_wR_factor_ref         0.0784
_refine_ls_wR_factor_gt          0.0733
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_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 0.82696(6) 0.47361(2) 1.16770(6) 0.01767(12) Uani 1 1 d . . . . .
H1 H 0.545(3) 0.7109(9) 0.281(3) 0.014(5) Uiso 1 1 d . . . . .
F1 F 0.46410(18) 0.67251(5) 0.82076(16) 0.0227(3) Uani 1 1 d . . . . .
N1 N 0.5460(3) 0.56872(8) 0.1718(2) 0.0206(4) Uani 1 1 d . . . . .
C1 C 0.5273(3) 0.58676(8) 0.3083(3) 0.0160(4) Uani 1 1 d . . . . .
B1 B 0.4979(3) 0.60931(10) 0.4999(3) 0.0151(4) Uani 1 1 d . . . . .
N2 N 0.1253(3) 0.56354(7) 0.4442(2) 0.0192(4) Uani 1 1 d . . . . .
H2 H 0.496(3) 0.8629(9) 0.592(3) 0.013(5) Uiso 1 1 d . . . . .
F2 F 0.54475(18) 0.83106(5) 0.28570(18) 0.0265(3) Uani 1 1 d . . . . .
C2 C 0.2799(3) 0.58253(8) 0.4675(3) 0.0155(4) Uani 1 1 d . . . . .
N3 N 0.7896(2) 0.54844(7) 0.8343(2) 0.0183(4) Uani 1 1 d . . . . .
H3 H 0.470(3) 0.7921(9) 0.832(3) 0.021(5) Uiso 1 1 d . . . . .
C3 C 0.6681(3) 0.57438(8) 0.6955(3) 0.0151(4) Uani 1 1 d . . . . .
C4 C 0.5065(3) 0.68499(8) 0.5253(3) 0.0147(4) Uani 1 1 d . . . . .
C5 C 0.5285(3) 0.72679(9) 0.3904(3) 0.0164(4) Uani 1 1 d . . . . .
C6 C 0.5243(3) 0.79081(9) 0.4207(3) 0.0187(4) Uani 1 1 d . . . . .
C9 C 0.4844(3) 0.71216(9) 0.6855(3) 0.0166(4) Uani 1 1 d . . . . .
C8 C 0.4798(3) 0.77627(9) 0.7155(3) 0.0204(4) Uani 1 1 d . . . . .
C7 C 0.5000(3) 0.81675(9) 0.5787(3) 0.0201(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 N3 2.8348(17) . ?
K1 N2 2.8367(17) 3_667 ?
K1 N3 2.8699(18) 3_767 ?
K1 N1 2.8892(17) 3_666 ?
K1 N1 2.8974(18) 1_556 ?
K1 N2 2.9202(17) 1_656 ?
K1 F2 3.1345(13) 2_646 ?
K1 C2 3.352(2) 3_667 ?
K1 C1 3.5258(19) 3_666 ?
K1 C3 3.529(2) 3_767 ?
K1 K1 4.4347(10) 3_767 ?
K1 K1 4.4368(10) 3_667 ?
F1 C9 1.365(2) . ?
N1 C1 1.145(2) . ?
N1 K1 2.8892(17) 3_666 ?
N1 K1 2.8975(18) 1_554 ?
C1 B1 1.600(3) . ?
C1 K1 3.5257(19) 3_666 ?
B1 C3 1.598(3) . ?
B1 C4 1.611(3) . ?
B1 C2 1.615(3) . ?
N2 C2 1.144(3) . ?
N2 K1 2.8367(17) 3_667 ?
N2 K1 2.9202(17) 1_454 ?
F2 C6 1.372(2) . ?
F2 K1 3.1345(13) 2_656 ?
C2 K1 3.3524(19) 3_667 ?
N3 C3 1.147(2) . ?
N3 K1 2.8699(18) 3_767 ?
C3 K1 3.529(2) 3_767 ?
C4 C9 1.392(3) . ?
C4 C5 1.396(3) . ?
C5 C6 1.377(3) . ?
C5 H1 0.94(2) . ?
C6 C7 1.374(3) . ?
C9 C8 1.378(3) . ?
C8 C7 1.385(3) . ?
C8 H3 0.96(2) . ?
C7 H2 0.984(19) . ?

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
N3 K1 N2 162.11(5) . 3_667 ?
N3 K1 N3 77.96(5) . 3_767 ?
N2 K1 N3 107.01(5) 3_667 3_767 ?
N3 K1 N1 75.08(5) . 3_666 ?
N2 K1 N1 114.91(5) 3_667 3_666 ?
N3 K1 N1 119.53(5) 3_767 3_666 ?
N3 K1 N1 80.46(5) . 1_556 ?
N2 K1 N1 86.64(5) 3_667 1_556 ?
N3 K1 N1 145.33(5) 3_767 1_556 ?
N1 K1 N1 79.88(5) 3_666 1_556 ?
N3 K1 N2 89.25(5) . 1_656 ?
N2 K1 N2 76.55(5) 3_667 1_656 ?
N3 K1 N2 71.45(5) 3_767 1_656 ?
N1 K1 N2 157.36(5) 3_666 1_656 ?
N1 K1 N2 81.51(5) 1_556 1_656 ?
N3 K1 F2 122.58(4) . 2_646 ?
N2 K1 F2 74.34(4) 3_667 2_646 ?
N3 K1 F2 66.16(4) 3_767 2_646 ?
N1 K1 F2 85.18(4) 3_666 2_646 ?
N1 K1 F2 148.11(4) 1_556 2_646 ?
N2 K1 F2 117.28(4) 1_656 2_646 ?
N3 K1 C2 158.71(5) . 3_667 ?
N2 K1 C2 19.06(5) 3_667 3_667 ?
N3 K1 C2 122.67(5) 3_767 3_667 ?
N1 K1 C2 96.23(5) 3_666 3_667 ?
N1 K1 C2 78.87(5) 1_556 3_667 ?
N2 K1 C2 92.68(5) 1_656 3_667 ?
F2 K1 C2 74.93(4) 2_646 3_667 ?
N3 K1 C1 66.54(5) . 3_666 ?
N2 K1 C1 126.98(5) 3_667 3_666 ?
N3 K1 C1 102.56(5) 3_767 3_666 ?
N1 K1 C1 17.15(4) 3_666 3_666 ?
N1 K1 C1 93.20(5) 1_556 3_666 ?
N2 K1 C1 155.77(5) 1_656 3_666 ?
F2 K1 C1 78.99(4) 2_646 3_666 ?
C2 K1 C1 109.57(5) 3_667 3_666 ?
N3 K1 C3 94.64(5) . 3_767 ?
N2 K1 C3 90.18(5) 3_667 3_767 ?
N3 K1 C3 16.96(4) 3_767 3_767 ?
N1 K1 C3 128.25(5) 3_666 3_767 ?
N1 K1 C3 149.48(5) 1_556 3_767 ?
N2 K1 C3 68.26(5) 1_656 3_767 ?
F2 K1 C3 57.71(4) 2_646 3_767 ?
C2 K1 C3 105.76(5) 3_667 3_767 ?
C1 K1 C3 112.59(4) 3_666 3_767 ?
N3 K1 K1 39.27(3) . 3_767 ?
N2 K1 K1 142.91(4) 3_667 3_767 ?
N3 K1 K1 38.69(3) 3_767 3_767 ?
N1 K1 K1 98.88(4) 3_666 3_767 ?
N1 K1 K1 115.23(4) 1_556 3_767 ?
N2 K1 K1 77.62(4) 1_656 3_767 ?
F2 K1 K1 94.74(3) 2_646 3_767 ?
C2 K1 K1 160.90(4) 3_667 3_767 ?
C1 K1 K1 83.47(4) 3_666 3_767 ?
C3 K1 K1 55.44(3) 3_767 3_767 ?
N3 K1 K1 73.99(4) . 3_667 ?
N2 K1 K1 103.65(4) 3_667 3_667 ?
N3 K1 K1 149.10(4) 3_767 3_667 ?
N1 K1 K1 40.01(3) 3_666 3_667 ?
N1 K1 K1 39.87(3) 1_556 3_667 ?
N2 K1 K1 120.30(4) 1_656 3_667 ?
F2 K1 K1 119.99(3) 2_646 3_667 ?
C2 K1 K1 86.83(4) 3_667 3_667 ?
C1 K1 K1 54.14(3) 3_666 3_667 ?
C3 K1 K1 164.95(3) 3_767 3_667 ?
K1 K1 K1 112.27(2) 3_767 3_667 ?
C1 N1 K1 114.78(14) . 3_666 ?
C1 N1 K1 127.97(14) . 1_554 ?
K1 N1 K1 100.12(5) 3_666 1_554 ?
N1 C1 B1 177.76(19) . . ?
N1 C1 K1 48.07(11) . 3_666 ?
B1 C1 K1 130.79(12) . 3_666 ?
C3 B1 C1 107.17(15) . . ?
C3 B1 C4 112.46(15) . . ?
C1 B1 C4 112.70(16) . . ?
C3 B1 C2 106.70(15) . . ?
C1 B1 C2 106.98(15) . . ?
C4 B1 C2 110.49(16) . . ?
C2 N2 K1 106.86(13) . 3_667 ?
C2 N2 K1 135.54(15) . 1_454 ?
K1 N2 K1 103.45(5) 3_667 1_454 ?
C6 F2 K1 130.25(11) . 2_656 ?
N2 C2 B1 179.9(2) . . ?
N2 C2 K1 54.07(11) . 3_667 ?
B1 C2 K1 126.06(11) . 3_667 ?
C3 N3 K1 140.44(15) . . ?
C3 N3 K1 116.16(14) . 3_767 ?
K1 N3 K1 102.04(5) . 3_767 ?
N3 C3 B1 178.93(19) . . ?
N3 C3 K1 46.88(11) . 3_767 ?
B1 C3 K1 132.91(12) . 3_767 ?
C9 C4 C5 116.25(17) . . ?
C9 C4 B1 119.78(16) . . ?
C5 C4 B1 123.94(17) . . ?
C6 C5 C4 119.31(18) . . ?
C6 C5 H1 121.1(12) . . ?
C4 C5 H1 119.6(12) . . ?
F2 C6 C7 118.03(17) . . ?
F2 C6 C5 118.38(17) . . ?
C7 C6 C5 123.58(18) . . ?
F1 C9 C8 117.99(17) . . ?
F1 C9 C4 117.61(16) . . ?
C8 C9 C4 124.40(18) . . ?
C9 C8 C7 118.27(19) . . ?
C9 C8 H3 120.4(12) . . ?
C7 C8 H3 121.2(12) . . ?
C6 C7 C8 118.19(18) . . ?
C6 C7 H2 120.0(11) . . ?
C8 C7 H2 121.8(11) . . ?

_refine_diff_density_max         0.315
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.061

####################################################################### 
# 
# 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_JL089_JL_KB4b
_database_code_depnum_ccdc_archive 'CCDC 1548906'
_audit_update_record             
;
2017-05-09 deposited with the CCDC.
2017-06-26 downloaded from the CCDC.
;


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

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H2 B F3 K N3'
_chemical_formula_sum            'C9 H2 B F3 K N3'
_chemical_formula_weight         259.05

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'
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'

_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                   7.1368(4)
_cell_length_b                   21.0081(11)
_cell_length_c                   6.8083(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.830(2)
_cell_angle_gamma                90
_cell_volume                     1020.67(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5414
_cell_measurement_theta_min      2.85
_cell_measurement_theta_max      26.80
_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).
;

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_F_000             512
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.539
_shelx_estimated_absorpt_T_min   0.938
_shelx_estimated_absorpt_T_max   0.958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7039
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13961
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         1.939
_diffrn_reflns_theta_max         26.815
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2183
_reflns_number_gt                1886
_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. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0214P)²+0.7337P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2183
_refine_ls_number_parameters     162
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0284
_refine_ls_wR_factor_ref         0.0647
_refine_ls_wR_factor_gt          0.0616
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_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 0.21040(5) 0.68741(2) 0.19830(5) 0.01279(10) Uani 1 1 d . . . . .
N1 N -0.0024(2) 0.29788(7) 0.1616(2) 0.0188(3) Uani 1 1 d . . . . .
F1 F 0.14691(14) 0.34361(4) 0.66121(14) 0.0187(2) Uani 1 1 d . . . . .
C1 C 0.1342(2) 0.32182(7) 0.2104(2) 0.0131(3) Uani 1 1 d . . . . .
B1 B 0.3207(2) 0.35737(8) 0.2859(3) 0.0119(3) Uani 1 1 d . . . . .
F2 F 0.05936(14) 0.43583(5) 0.90850(14) 0.0229(2) Uani 1 1 d . . . . .
N2 N 0.54726(19) 0.27368(6) 0.4879(2) 0.0159(3) Uani 1 1 d . . . . .
C2 C 0.4494(2) 0.30727(7) 0.4032(2) 0.0125(3) Uani 1 1 d . . . . .
C3 C 0.4392(2) 0.38103(7) 0.1023(2) 0.0131(3) Uani 1 1 d . . . . .
F3 F 0.27725(14) 0.58892(4) 0.46262(14) 0.0189(2) Uani 1 1 d . . . . .
N3 N 0.5307(2) 0.39838(7) -0.0236(2) 0.0202(3) Uani 1 1 d . . . . .
C4 C 0.2675(2) 0.41625(7) 0.4278(2) 0.0105(3) Uani 1 1 d . . . . .
H4 H 0.351(2) 0.4930(7) 0.252(2) 0.002(4) Uiso 1 1 d . . . . .
C5 C 0.1866(2) 0.40449(7) 0.6079(2) 0.0130(3) Uani 1 1 d . . . . .
H5 H 0.144(3) 0.5476(10) 0.780(3) 0.025(5) Uiso 1 1 d . . . . .
C6 C 0.1407(2) 0.45212(8) 0.7375(2) 0.0150(3) Uani 1 1 d . . . . .
C7 C 0.1728(2) 0.51508(8) 0.6933(2) 0.0136(3) Uani 1 1 d . . . . .
C9 C 0.2982(2) 0.48030(7) 0.3802(2) 0.0121(3) Uani 1 1 d . . . . .
C8 C 0.2493(2) 0.52679(7) 0.5126(2) 0.0130(3) 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 F3 2.7790(10) . ?
K1 F1 2.8130(10) 3_566 ?
K1 N2 2.8188(14) 2_655 ?
K1 N2 2.8492(14) 3_666 ?
K1 N3 2.8532(15) 3_665 ?
K1 N1 2.8628(14) 3_565 ?
K1 N1 2.9222(15) 2 ?
K1 F2 3.3012(11) 3_566 ?
K1 K1 4.3015(4) 4_576 ?
K1 K1 4.3015(4) 4_575 ?
N1 C1 1.142(2) . ?
N1 K1 2.8628(14) 3_565 ?
N1 K1 2.9222(15) 2_545 ?
F1 C5 1.3604(17) . ?
F1 K1 2.8130(10) 3_566 ?
C1 B1 1.605(2) . ?
B1 C3 1.599(2) . ?
B1 C2 1.602(2) . ?
B1 C4 1.618(2) . ?
F2 C6 1.3522(18) . ?
F2 K1 3.3013(11) 3_566 ?
N2 C2 1.143(2) . ?
N2 K1 2.8187(14) 2_645 ?
N2 K1 2.8493(14) 3_666 ?
C3 N3 1.145(2) . ?
F3 C8 1.3641(17) . ?
N3 K1 2.8532(15) 3_665 ?
C4 C5 1.385(2) . ?
C4 C9 1.402(2) . ?
C5 C6 1.377(2) . ?
C6 C7 1.377(2) . ?
C7 C8 1.376(2) . ?
C7 H5 0.93(2) . ?
C9 C8 1.377(2) . ?
C9 H4 0.990(16) . ?

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
F3 K1 F1 75.84(3) . 3_566 ?
F3 K1 N2 132.00(4) . 2_655 ?
F1 K1 N2 150.11(4) 3_566 2_655 ?
F3 K1 N2 68.36(3) . 3_666 ?
F1 K1 N2 110.78(4) 3_566 3_666 ?
N2 K1 N2 77.47(3) 2_655 3_666 ?
F3 K1 N3 72.15(4) . 3_665 ?
F1 K1 N3 126.24(4) 3_566 3_665 ?
N2 K1 N3 79.25(4) 2_655 3_665 ?
N2 K1 N3 95.98(4) 3_666 3_665 ?
F3 K1 N1 135.77(4) . 3_565 ?
F1 K1 N1 81.65(4) 3_566 3_565 ?
N2 K1 N1 81.93(4) 2_655 3_565 ?
N2 K1 N1 155.84(4) 3_666 3_565 ?
N3 K1 N1 92.41(4) 3_665 3_565 ?
F3 K1 N1 117.59(4) . 2 ?
F1 K1 N1 66.78(4) 3_566 2 ?
N2 K1 N1 87.36(4) 2_655 2 ?
N2 K1 N1 80.39(4) 3_666 2 ?
N3 K1 N1 166.60(4) 3_665 2 ?
N1 K1 N1 86.23(4) 3_565 2 ?
F3 K1 F2 69.68(3) . 3_566 ?
F1 K1 F2 50.55(3) 3_566 3_566 ?
N2 K1 F2 139.90(3) 2_655 3_566 ?
N2 K1 F2 137.38(3) 3_666 3_566 ?
N3 K1 F2 77.99(4) 3_665 3_566 ?
N1 K1 F2 66.59(3) 3_565 3_566 ?
N1 K1 F2 113.42(4) 2 3_566 ?
F3 K1 K1 86.83(2) . 4_576 ?
F1 K1 K1 82.07(2) 3_566 4_576 ?
N2 K1 K1 88.27(3) 2_655 4_576 ?
N2 K1 K1 40.37(3) 3_666 4_576 ?
N3 K1 K1 136.35(3) 3_665 4_576 ?
N1 K1 K1 127.26(3) 3_565 4_576 ?
N1 K1 K1 41.44(3) 2 4_576 ?
F2 K1 K1 130.321(18) 3_566 4_576 ?
F3 K1 K1 164.95(2) . 4_575 ?
F1 K1 K1 114.90(2) 3_566 4_575 ?
N2 K1 K1 40.90(3) 2_655 4_575 ?
N2 K1 K1 114.28(3) 3_666 4_575 ?
N3 K1 K1 92.80(3) 3_665 4_575 ?
N1 K1 K1 42.50(3) 3_565 4_575 ?
N1 K1 K1 77.22(3) 2 4_575 ?
F2 K1 K1 108.169(18) 3_566 4_575 ?
K1 K1 K1 104.631(14) 4_576 4_575 ?
C1 N1 K1 129.16(12) . 3_565 ?
C1 N1 K1 133.63(12) . 2_545 ?
K1 N1 K1 96.07(4) 3_565 2_545 ?
C5 F1 K1 120.12(8) . 3_566 ?
N1 C1 B1 177.39(17) . . ?
C3 B1 C2 106.75(13) . . ?
C3 B1 C1 109.88(13) . . ?
C2 B1 C1 108.72(13) . . ?
C3 B1 C4 111.13(13) . . ?
C2 B1 C4 110.02(12) . . ?
C1 B1 C4 110.26(13) . . ?
C6 F2 K1 105.37(9) . 3_566 ?
C2 N2 K1 123.01(11) . 2_645 ?
C2 N2 K1 124.12(11) . 3_666 ?
K1 N2 K1 98.74(4) 2_645 3_666 ?
N2 C2 B1 176.85(16) . . ?
N3 C3 B1 176.92(16) . . ?
C8 F3 K1 148.17(9) . . ?
C3 N3 K1 119.42(12) . 3_665 ?
C5 C4 C9 116.40(14) . . ?
C5 C4 B1 119.77(13) . . ?
C9 C4 B1 123.83(14) . . ?
F1 C5 C6 117.38(14) . . ?
F1 C5 C4 119.67(14) . . ?
C6 C5 C4 122.95(15) . . ?
F2 C6 C7 120.42(14) . . ?
F2 C6 C5 118.49(14) . . ?
C7 C6 C5 121.08(15) . . ?
C8 C7 C6 115.92(15) . . ?
C8 C7 H5 122.2(12) . . ?
C6 C7 H5 121.9(12) . . ?
C8 C9 C4 119.16(14) . . ?
C8 C9 H4 119.1(9) . . ?
C4 C9 H4 121.7(9) . . ?
F3 C8 C7 117.10(14) . . ?
F3 C8 C9 118.42(14) . . ?
C7 C8 C9 124.48(15) . . ?

_refine_diff_density_max         0.399
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.053

####################################################################### 
# 
# 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_JL021_JL_KB7thf
_database_code_depnum_ccdc_archive 'CCDC 1548907'
_audit_update_record             
;
2017-05-09 deposited with the CCDC.
2017-06-26 downloaded from the CCDC.
;


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


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H32 B4 F28 K4 N12 O4'
_chemical_formula_sum            'C56 H32 B4 F28 K4 N12 O4'
_chemical_formula_weight         1668.57

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'
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'

_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                   12.5972(7)
_cell_length_b                   32.4417(17)
_cell_length_c                   16.9137(9)
_cell_angle_alpha                90
_cell_angle_beta                 92.820(3)
_cell_angle_gamma                90
_cell_volume                     6903.8(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5499
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      20.40
_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).
;

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_F_000             3328
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.388
_shelx_estimated_absorpt_T_min   0.899
_shelx_estimated_absorpt_T_max   0.955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6438
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            89364
_diffrn_reflns_av_unetI/netI     0.1150
_diffrn_reflns_av_R_equivalents  0.1395
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.255
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        26.000
_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             14119
_reflns_number_gt                7469
_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. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0401P)²+4.4553P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14119
_refine_ls_number_parameters     1047
_refine_ls_number_restraints     218
_refine_ls_R_factor_all          0.1433
_refine_ls_R_factor_gt           0.0552
_refine_ls_wR_factor_ref         0.1311
_refine_ls_wR_factor_gt          0.0998
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.004
_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
O1A O -0.4861(2) 0.16994(8) 0.23061(15) 0.0333(7) Uani 0.478(11) 1 d D . P A -1
C61 C -0.5681(3) 0.16812(12) 0.1684(2) 0.0337(9) Uani 0.478(11) 1 d D U P A -1
H61A H -0.5603 0.1916 0.1317 0.040 Uiso 0.478(11) 1 calc R U P A -1
H61B H -0.6387 0.1703 0.1914 0.040 Uiso 0.478(11) 1 calc R U P A -1
C62 C -0.5607(10) 0.1279(3) 0.1236(6) 0.0370(14) Uani 0.478(11) 1 d D U P A -1
H62A H -0.5188 0.1310 0.0759 0.044 Uiso 0.478(11) 1 calc R U P A -1
H62B H -0.6318 0.1167 0.1082 0.044 Uiso 0.478(11) 1 calc R U P A -1
C63 C -0.5032(10) 0.1016(3) 0.1866(6) 0.0407(14) Uani 0.478(11) 1 d D U P A -1
H63A H -0.5535 0.0900 0.2239 0.049 Uiso 0.478(11) 1 calc R U P A -1
H63B H -0.4638 0.0788 0.1625 0.049 Uiso 0.478(11) 1 calc R U P A -1
C64 C -0.4278(15) 0.1321(4) 0.2278(13) 0.0410(16) Uani 0.478(11) 1 d D U P A -1
H64A H -0.4066 0.1225 0.2818 0.049 Uiso 0.478(11) 1 calc R U P A -1
H64B H -0.3630 0.1357 0.1976 0.049 Uiso 0.478(11) 1 calc R U P A -1
O1B O -0.4861(2) 0.16994(8) 0.23061(15) 0.0333(7) Uani 0.522(11) 1 d D . P A -2
C71 C -0.5681(3) 0.16812(12) 0.1684(2) 0.0337(9) Uani 0.522(11) 1 d D U P A -2
H71A H -0.5506 0.1860 0.1235 0.040 Uiso 0.522(11) 1 calc R U P A -2
H71B H -0.6375 0.1767 0.1880 0.040 Uiso 0.522(11) 1 calc R U P A -2
C72 C -0.5702(8) 0.1233(2) 0.1443(7) 0.0382(14) Uani 0.522(11) 1 d D U P A -2
H72A H -0.5928 0.1203 0.0877 0.046 Uiso 0.522(11) 1 calc R U P A -2
H72B H -0.6194 0.1074 0.1765 0.046 Uiso 0.522(11) 1 calc R U P A -2
C73 C -0.4564(8) 0.1086(3) 0.1594(6) 0.0396(14) Uani 0.522(11) 1 d D U P A -2
H73A H -0.4527 0.0785 0.1681 0.047 Uiso 0.522(11) 1 calc R U P A -2
H73B H -0.4111 0.1163 0.1155 0.047 Uiso 0.522(11) 1 calc R U P A -2
C74 C -0.4265(15) 0.1324(4) 0.2345(11) 0.0415(16) Uani 0.522(11) 1 d D U P A -2
H74A H -0.4443 0.1163 0.2817 0.050 Uiso 0.522(11) 1 calc R U P A -2
H74B H -0.3493 0.1384 0.2378 0.050 Uiso 0.522(11) 1 calc R U P A -2
O2 O -0.5289(3) 0.12764(10) 0.42398(19) 0.0511(9) Uani 1 1 d . . . . .
C67 C -0.4702(5) 0.07307(17) 0.5050(3) 0.0688(18) Uani 1 1 d . . . . .
H67A H -0.4126 0.0595 0.4769 0.083 Uiso 1 1 calc R U . . .
H67B H -0.4646 0.0652 0.5616 0.083 Uiso 1 1 calc R U . . .
O3A O 0.8595(17) 0.3830(8) 0.2458(17) 0.035(3) Uani 0.165(5) 1 d D U P B -3
C50 C 0.759(2) 0.4019(10) 0.2252(15) 0.046(2) Uani 0.165(5) 1 d D U P B -3
H50A H 0.7446 0.4246 0.2622 0.055 Uiso 0.165(5) 1 calc R U P B -3
H50B H 0.7008 0.3814 0.2271 0.055 Uiso 0.165(5) 1 calc R U P B -3
C51 C 0.767(2) 0.4183(10) 0.1415(15) 0.0449(15) Uani 0.165(5) 1 d D U P B -3
H51A H 0.7465 0.4477 0.1375 0.054 Uiso 0.165(5) 1 calc R U P B -3
H51B H 0.7239 0.4020 0.1024 0.054 Uiso 0.165(5) 1 calc R U P B -3
C52 C 0.886(2) 0.4122(12) 0.1324(16) 0.0437(18) Uani 0.165(5) 1 d D U P B -3
H52A H 0.8995 0.3860 0.1048 0.052 Uiso 0.165(5) 1 calc R U P B -3
H52B H 0.9156 0.4352 0.1021 0.052 Uiso 0.165(5) 1 calc R U P B -3
C53 C 0.934(2) 0.4113(9) 0.2166(15) 0.045(2) Uani 0.165(5) 1 d D U P B -3
H53A H 1.0075 0.4005 0.2196 0.054 Uiso 0.165(5) 1 calc R U P B -3
H53B H 0.9315 0.4385 0.2429 0.054 Uiso 0.165(5) 1 calc R U P B -3
O3B O 0.8937(3) 0.39145(13) 0.2300(3) 0.0348(11) Uani 0.835(5) 1 d D U P B -4
C55 C 0.8081(5) 0.41583(18) 0.2563(4) 0.0492(14) Uani 0.835(5) 1 d D U P B -4
H55A H 0.8310 0.4318 0.3040 0.059 Uiso 0.835(5) 1 calc R U P B -4
H55B H 0.7475 0.3981 0.2693 0.059 Uiso 0.835(5) 1 calc R U P B -4
C56 C 0.7768(4) 0.44436(17) 0.1889(3) 0.0464(13) Uani 0.835(5) 1 d D U P B -4
H56A H 0.8126 0.4714 0.1953 0.056 Uiso 0.835(5) 1 calc R U P B -4
H56B H 0.6989 0.4487 0.1849 0.056 Uiso 0.835(5) 1 calc R U P B -4
C57 C 0.8141(5) 0.42167(18) 0.1174(3) 0.0452(13) Uani 0.835(5) 1 d D U P B -4
H57A H 0.7617 0.4008 0.0982 0.054 Uiso 0.835(5) 1 calc R U P B -4
H57B H 0.8285 0.4409 0.0737 0.054 Uiso 0.835(5) 1 calc R U P B -4
C58 C 0.9147(5) 0.40189(19) 0.1508(3) 0.0404(13) Uani 0.835(5) 1 d D U P B -4
H58A H 0.9318 0.3769 0.1202 0.048 Uiso 0.835(5) 1 calc R U P B -4
H58B H 0.9751 0.4213 0.1495 0.048 Uiso 0.835(5) 1 calc R U P B -4
K1 K -0.56877(6) 0.20339(3) 0.36797(5) 0.0233(2) Uani 1 1 d . . . . .
N1 N -0.3506(3) 0.21016(10) 0.3933(2) 0.0319(9) Uani 1 1 d . . . . .
C1 C 0.5262(3) 0.40866(12) 0.4075(2) 0.0254(9) Uani 1 1 d . . . . .
B1 B 0.5890(3) 0.33114(13) 0.4336(2) 0.0198(10) Uani 1 1 d . . . . .
F1 F -0.2400(2) 0.12451(8) 0.3891(2) 0.0703(10) Uani 1 1 d . . . . .
B2 B 0.3144(3) 0.19060(14) 0.6690(2) 0.0200(10) Uani 1 1 d . . . . .
N2 N -0.1838(3) 0.20246(11) 0.6288(2) 0.0335(9) Uani 1 1 d . . . . .
F2 F -0.1352(2) 0.05771(9) 0.3641(2) 0.0793(10) Uani 1 1 d . . . . .
K2 K 0.67599(6) 0.26497(3) 0.72357(5) 0.0239(2) Uani 1 1 d . . . . .
C3 C 0.9610(3) 0.29603(12) 0.7374(2) 0.0217(9) Uani 1 1 d . . . . .
N3 N -0.0458(3) 0.26865(10) 0.42593(18) 0.0266(8) Uani 1 1 d . . . . .
B3 B 1.0571(4) 0.32429(13) 0.7127(2) 0.0211(10) Uani 1 1 d . . . . .
K3 K 1.17748(6) 0.27031(2) 0.42339(5) 0.02010(19) Uani 1 1 d . . . . .
F3 F 0.0316(2) 0.01664(9) 0.37641(19) 0.0708(9) Uani 1 1 d . . . . .
B4 B -0.1557(3) 0.20084(14) 0.4689(2) 0.0210(10) Uani 1 1 d . . . . .
N4 N 0.3171(2) 0.21269(10) 0.51290(18) 0.0264(8) Uani 1 1 d . . . . .
K4 K 0.93101(6) 0.31226(2) 0.27713(5) 0.0213(2) Uani 1 1 d . . . . .
O4 O 1.08686(19) 0.34848(7) 0.38232(14) 0.0230(6) Uani 1 1 d . . . . .
F4 F 0.1203(3) 0.03161(10) 0.48228(18) 0.1013(14) Uani 1 1 d . . . . .
C4 C 0.6309(3) 0.31060(12) 0.5143(2) 0.0223(9) Uani 1 1 d . . . . .
F5 F 0.1694(2) 0.05228(9) 0.37179(19) 0.0678(9) Uani 1 1 d . . . . .
N5 N 0.1380(3) 0.21614(10) 0.74373(19) 0.0259(8) Uani 1 1 d . . . . .
C5 C 0.3119(3) 0.20372(11) 0.5778(2) 0.0195(8) Uani 1 1 d . . . . .
F6 F 0.1739(2) 0.11789(8) 0.48003(15) 0.0505(7) Uani 1 1 d . . . . .
N6 N 0.4698(3) 0.23660(10) 0.74333(19) 0.0285(8) Uani 1 1 d . . . . .
C6 C -0.2688(3) 0.20495(11) 0.4251(2) 0.0222(9) Uani 1 1 d . . . . .
F7 F 0.06601(18) 0.18609(7) 0.50509(15) 0.0436(7) Uani 1 1 d . . . . .
N7 N 0.7178(2) 0.30578(10) 0.31801(19) 0.0246(8) Uani 1 1 d . . . . .
C7 C -0.1723(3) 0.20222(12) 0.5626(2) 0.0225(9) Uani 1 1 d . . . . .
C8 C -0.0905(3) 0.24064(12) 0.4454(2) 0.0208(9) Uani 1 1 d . . . . .
N8 N 0.3871(3) 0.30095(10) 0.40948(19) 0.0301(8) Uani 1 1 d . . . . .
C9 C -0.0926(3) 0.15905(12) 0.4485(2) 0.0220(9) Uani 1 1 d . . . . .
N9 N 0.6570(3) 0.29550(11) 0.5728(2) 0.0365(9) Uani 1 1 d . . . . .
F11 F 0.14781(18) 0.13116(7) 0.64117(14) 0.0374(6) Uani 1 1 d . . . . .
N11 N 0.8927(3) 0.27619(10) 0.7573(2) 0.0302(8) Uani 1 1 d . . . . .
C11 C -0.0819(4) 0.08868(13) 0.4004(3) 0.0420(12) Uani 1 1 d . . . . .
F12 F 0.16452(19) 0.05015(7) 0.64672(15) 0.0469(7) Uani 1 1 d . . . . .
N12 N 1.2121(3) 0.31103(10) 0.82881(19) 0.0298(8) Uani 1 1 d . . . . .
C12 C 0.0230(4) 0.08493(13) 0.4230(2) 0.0327(11) Uani 1 1 d . . . . .
F13 F 0.3200(2) -0.00704(8) 0.61315(17) 0.0646(9) Uani 1 1 d . . . . .
C13 C 0.0704(3) 0.11914(14) 0.4574(2) 0.0326(11) Uani 1 1 d . . . . .
C15 C 0.0854(4) 0.04600(15) 0.4151(3) 0.0462(13) Uani 1 1 d . . . . .
F15 F 0.4505(3) -0.00664(8) 0.6974(2) 0.0776(10) Uani 1 1 d . . . . .
C14 C 0.0140(3) 0.15446(12) 0.4695(2) 0.0248(9) Uani 1 1 d . . . . .
F14 F 0.2929(3) -0.00929(8) 0.73590(17) 0.0678(9) Uani 1 1 d . . . . .
F16 F 0.5269(2) 0.06373(7) 0.72433(16) 0.0508(7) Uani 1 1 d . . . . .
C16 C 0.2082(3) 0.20577(11) 0.7096(2) 0.0207(9) Uani 1 1 d . . . . .
F17 F 0.51077(18) 0.14315(7) 0.71585(16) 0.0449(7) Uani 1 1 d . . . . .
C17 C 0.4072(3) 0.21631(12) 0.7120(2) 0.0202(9) Uani 1 1 d . . . . .
C18 C 0.3279(3) 0.14141(11) 0.6777(2) 0.0204(9) Uani 1 1 d . . . . .
C19 C 0.4216(3) 0.12136(12) 0.6983(2) 0.0287(10) Uani 1 1 d . . . . .
C20 C 0.4307(3) 0.07920(13) 0.7020(2) 0.0324(10) Uani 1 1 d . . . . .
C21 C 0.3467(4) 0.05366(12) 0.6844(2) 0.0301(10) Uani 1 1 d . . . . .
F21 F 0.42950(17) 0.39563(7) 0.38120(14) 0.0386(6) Uani 1 1 d . . . . .
C22 C 0.2518(3) 0.07300(13) 0.6637(2) 0.0298(10) Uani 1 1 d . . . . .
F22 F 0.4665(2) 0.47489(7) 0.37585(15) 0.0488(7) Uani 1 1 d . . . . .
C23 C 0.2438(3) 0.11490(12) 0.6614(2) 0.0249(9) Uani 1 1 d . . . . .
F23 F 0.5877(3) 0.53360(8) 0.45709(18) 0.0708(10) Uani 1 1 d . . . . .
C24 C 0.3525(4) 0.00778(14) 0.6833(3) 0.0433(12) Uani 1 1 d . . . . .
F24 F 0.6447(2) 0.52341(7) 0.34163(16) 0.0491(7) Uani 1 1 d . . . . .
C28 C 0.5448(3) 0.45014(13) 0.4041(2) 0.0311(10) Uani 1 1 d . . . . .
C27 C 0.6011(3) 0.38079(11) 0.4347(2) 0.0206(9) Uani 1 1 d . . . . .
F27 F 0.77831(17) 0.37349(7) 0.48410(14) 0.0353(6) Uani 1 1 d . . . . .
C26 C 0.4698(3) 0.31482(12) 0.4179(2) 0.0214(9) Uani 1 1 d . . . . .
F26 F 0.81762(19) 0.45223(7) 0.47608(15) 0.0450(7) Uani 1 1 d . . . . .
C25 C 0.6610(3) 0.31495(11) 0.3655(2) 0.0187(8) Uani 1 1 d . . . . .
F25 F 0.7546(2) 0.52471(8) 0.44315(16) 0.0595(8) Uani 1 1 d . . . . .
C29 C 0.6418(4) 0.46680(12) 0.4270(2) 0.0309(10) Uani 1 1 d . . . . .
C10 C -0.1367(3) 0.12455(13) 0.4127(3) 0.0356(11) Uani 1 1 d . . . . .
N10 N 1.1397(3) 0.29666(10) 0.5759(2) 0.0349(9) Uani 1 1 d . . . . .
C30 C 0.7189(3) 0.43954(13) 0.4544(2) 0.0296(10) Uani 1 1 d . . . . .
C31 C 0.6977(3) 0.39814(12) 0.4583(2) 0.0247(9) Uani 1 1 d . . . . .
F31 F 0.84130(18) 0.35368(7) 0.66374(15) 0.0430(7) Uani 1 1 d . . . . .
C32 C 0.6584(4) 0.51242(14) 0.4177(3) 0.0448(13) Uani 1 1 d . . . . .
F32 F 0.7829(2) 0.42905(7) 0.63897(16) 0.0489(7) Uani 1 1 d . . . . .
C33 C 1.1042(3) 0.30737(12) 0.6333(2) 0.0241(9) Uani 1 1 d . . . . .
F33 F 0.8297(3) 0.50476(8) 0.62747(18) 0.0656(9) Uani 1 1 d . . . . .
C34 C 1.1475(3) 0.31842(12) 0.7810(2) 0.0223(9) Uani 1 1 d . . . . .
F34 F 0.9884(3) 0.51295(8) 0.59408(18) 0.0734(10) Uani 1 1 d . . . . .
C35 C 1.0192(3) 0.37161(11) 0.6995(2) 0.0200(9) Uani 1 1 d . . . . .
F35 F 0.9500(3) 0.52227(8) 0.71421(18) 0.0765(10) Uani 1 1 d . . . . .
C36 C 0.9166(3) 0.38280(12) 0.6753(2) 0.0278(10) Uani 1 1 d . . . . .
F36 F 1.1328(2) 0.47384(7) 0.70062(16) 0.0511(7) Uani 1 1 d . . . . .
C37 C 0.8853(3) 0.42253(13) 0.6611(2) 0.0325(11) Uani 1 1 d . . . . .
F37 F 1.19178(19) 0.39689(7) 0.72596(15) 0.0423(7) Uani 1 1 d . . . . .
C38 C 0.9562(4) 0.45449(12) 0.6686(2) 0.0323(11) Uani 1 1 d . . . . .
C39 C 1.0591(4) 0.44405(12) 0.6920(2) 0.0333(11) Uani 1 1 d . . . . .
C40 C 1.0886(3) 0.40432(12) 0.7062(2) 0.0266(10) Uani 1 1 d . . . . .
C41 C 0.9308(5) 0.49851(15) 0.6520(3) 0.0508(14) Uani 1 1 d . . . . .
C80 C 1.0239(3) 0.37008(12) 0.4377(2) 0.0301(10) Uani 1 1 d . . . . .
H80A H 0.9871 0.3503 0.4715 0.036 Uiso 1 1 calc R U . . .
H80B H 0.9699 0.3875 0.4093 0.036 Uiso 1 1 calc R U . . .
C81 C 1.1009(3) 0.39655(12) 0.4874(2) 0.0318(11) Uani 1 1 d . . . . .
H81A H 1.1131 0.3849 0.5412 0.038 Uiso 1 1 calc R U . . .
H81B H 1.0738 0.4251 0.4920 0.038 Uiso 1 1 calc R U . . .
C82 C 1.2025(3) 0.39571(13) 0.4422(2) 0.0348(11) Uani 1 1 d . . . . .
H82A H 1.2305 0.4239 0.4351 0.042 Uiso 1 1 calc R U . . .
H82B H 1.2578 0.3788 0.4704 0.042 Uiso 1 1 calc R U . . .
C83 C 1.1691(3) 0.37665(12) 0.3636(2) 0.0266(10) Uani 1 1 d . . . . .
H83A H 1.1420 0.3979 0.3258 0.032 Uiso 1 1 calc R U . . .
H83B H 1.2292 0.3620 0.3406 0.032 Uiso 1 1 calc R U . . .
C65 C -0.5903(5) 0.09245(16) 0.4008(3) 0.0708(17) Uani 1 1 d . . . . .
H65A H -0.5641 0.0803 0.3517 0.085 Uiso 1 1 calc R U . . .
H65B H -0.6660 0.1000 0.3914 0.085 Uiso 1 1 calc R U . . .
C66 C -0.5772(5) 0.06268(17) 0.4680(4) 0.0779(19) Uani 1 1 d . . . . .
H66A H -0.5793 0.0339 0.4487 0.094 Uiso 1 1 calc R U . . .
H66B H -0.6335 0.0665 0.5062 0.094 Uiso 1 1 calc R U . . .
C68 C -0.4671(5) 0.11905(17) 0.4950(3) 0.0680(17) Uani 1 1 d . . . . .
H68A H -0.4977 0.1330 0.5408 0.082 Uiso 1 1 calc R U . . .
H68B H -0.3930 0.1287 0.4905 0.082 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
O1A C64 1.433(8) . ?
O1A C61 1.439(4) . ?
O1A K1 2.811(3) . ?
C61 C62 1.514(8) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 C63 1.522(9) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 C64 1.517(10) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
O1B C74 1.429(8) . ?
O1B C71 1.439(4) . ?
O1B K1 2.811(3) . ?
C71 C72 1.511(8) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 C73 1.519(8) . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C73 C74 1.518(9) . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
O2 C65 1.423(6) . ?
O2 C68 1.427(6) . ?
O2 K1 2.673(3) . ?
C67 C66 1.497(7) . ?
C67 C68 1.502(7) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
O3A C53 1.420(10) . ?
O3A C50 1.436(10) . ?
O3A K4 2.51(2) . ?
C50 C51 1.520(10) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.523(10) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 C53 1.521(10) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 K4 3.37(3) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
O3B C58 1.419(6) . ?
O3B C55 1.425(6) . ?
O3B K4 2.724(4) . ?
C55 C56 1.505(6) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 C57 1.511(6) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 C58 1.505(6) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
K1 N1 2.770(4) . ?
K1 N12 2.846(3) 4_365 ?
K1 N4 2.918(3) 1_455 ?
K1 N6 2.928(3) 4_465 ?
K1 N8 3.295(3) 1_455 ?
K1 K3 4.0131(11) 1_355 ?
K1 K2 4.1553(12) 4_465 ?
N1 C6 1.150(5) . ?
N1 K2 3.017(3) 4_465 ?
C1 F21 1.345(4) . ?
C1 C28 1.368(5) . ?
C1 C27 1.370(5) . ?
B1 C4 1.586(6) . ?
B1 C25 1.591(6) . ?
B1 C26 1.601(6) . ?
B1 C27 1.618(6) . ?
F1 C10 1.342(5) . ?
B2 C17 1.583(6) . ?
B2 C5 1.599(6) . ?
B2 C16 1.610(6) . ?
B2 C18 1.611(6) . ?
N2 C7 1.136(4) . ?
N2 K4 2.874(3) 4_466 ?
N2 K2 3.175(4) 1_455 ?
F2 C11 1.340(5) . ?
K2 N9 2.735(4) . ?
K2 N11 2.785(3) . ?
K2 N6 2.791(3) . ?
K2 N7 2.831(3) 4_566 ?
K2 N1 3.017(3) 4_666 ?
K2 N2 3.175(4) 1_655 ?
K2 K4 4.1390(12) 4_566 ?
K2 K1 4.1552(12) 4_666 ?
C3 N11 1.138(5) . ?
C3 B3 1.590(6) . ?
N3 C8 1.127(4) . ?
N3 K3 2.816(3) 1_455 ?
N3 K4 2.889(3) 1_455 ?
B3 C33 1.592(6) . ?
B3 C34 1.593(6) . ?
B3 C35 1.620(5) . ?
K3 N10 2.780(4) . ?
K3 N3 2.816(3) 1_655 ?
K3 N8 2.841(4) 1_655 ?
K3 O4 2.853(3) . ?
K3 N4 2.936(3) 1_655 ?
K3 N5 3.086(3) 4_665 ?
K3 N12 3.128(3) 4_565 ?
K3 F7 3.397(3) 1_655 ?
K3 K1 4.0131(11) 1_755 ?
K3 K4 4.1056(11) . ?
F3 C15 1.323(5) . ?
B4 C6 1.580(6) . ?
B4 C8 1.591(6) . ?
B4 C7 1.609(6) . ?
B4 C9 1.617(6) . ?
N4 C5 1.140(4) . ?
N4 K1 2.918(3) 1_655 ?
N4 K3 2.936(3) 1_455 ?
K4 N7 2.814(3) . ?
K4 O4 2.838(3) . ?
K4 N5 2.848(3) 4_665 ?
K4 N2 2.874(3) 4_665 ?
K4 N3 2.889(3) 1_655 ?
K4 N11 2.926(3) 4_565 ?
K4 C80 3.457(4) . ?
K4 K2 4.1391(12) 4_565 ?
O4 C83 1.428(4) . ?
O4 C80 1.439(4) . ?
F4 C15 1.286(5) . ?
C4 N9 1.138(5) . ?
F5 C15 1.332(5) . ?
N5 C16 1.132(4) . ?
N5 K4 2.848(3) 4_466 ?
N5 K3 3.086(3) 4_466 ?
F6 C13 1.342(4) . ?
N6 C17 1.139(4) . ?
N6 K1 2.928(3) 4_666 ?
F7 C14 1.344(4) . ?
F7 K3 3.397(3) 1_455 ?
N7 C25 1.140(4) . ?
N7 K2 2.831(3) 4_565 ?
N8 C26 1.138(5) . ?
N8 K3 2.841(4) 1_455 ?
N8 K1 3.295(3) 1_655 ?
C9 C10 1.377(5) . ?
C9 C14 1.380(5) . ?
F11 C23 1.348(4) . ?
N11 K4 2.926(3) 4_566 ?
C11 C12 1.363(6) . ?
C11 C10 1.374(6) . ?
F12 C22 1.345(4) . ?
N12 C34 1.144(4) . ?
N12 K1 2.846(3) 4_766 ?
N12 K3 3.128(3) 4_566 ?
C12 C13 1.375(6) . ?
C12 C15 1.497(6) . ?
F13 C24 1.326(5) . ?
C13 C14 1.369(5) . ?
F15 C24 1.330(5) . ?
F14 C24 1.315(5) . ?
F16 C20 1.348(4) . ?
F17 C19 1.348(4) . ?
C18 C19 1.378(5) . ?
C18 C23 1.381(5) . ?
C19 C20 1.374(5) . ?
C20 C21 1.365(6) . ?
C21 C22 1.381(6) . ?
C21 C24 1.490(6) . ?
C22 C23 1.363(5) . ?
F22 C28 1.342(4) . ?
F23 C32 1.329(5) . ?
F24 C32 1.339(5) . ?
C28 C29 1.375(6) . ?
C27 C31 1.381(5) . ?
F27 C31 1.348(4) . ?
F26 C30 1.344(4) . ?
F25 C32 1.327(5) . ?
C29 C30 1.377(6) . ?
C29 C32 1.504(6) . ?
N10 C33 1.143(5) . ?
C30 C31 1.372(5) . ?
F31 C36 1.346(4) . ?
F32 C37 1.343(5) . ?
F33 C41 1.335(6) . ?
F34 C41 1.333(5) . ?
C35 C40 1.377(5) . ?
C35 C36 1.384(5) . ?
F35 C41 1.317(5) . ?
C36 C37 1.366(5) . ?
F36 C39 1.343(4) . ?
C37 C38 1.370(6) . ?
F37 C40 1.347(4) . ?
C38 C39 1.378(6) . ?
C38 C41 1.487(6) . ?
C39 C40 1.360(5) . ?
C80 C81 1.519(5) . ?
C80 H80A 0.9900 . ?
C80 H80B 0.9900 . ?
C81 C82 1.523(5) . ?
C81 H81A 0.9900 . ?
C81 H81B 0.9900 . ?
C82 C83 1.507(5) . ?
C82 H82A 0.9900 . ?
C82 H82B 0.9900 . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
C65 C66 1.494(7) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?

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
C64 O1A C61 106.9(6) . . ?
C64 O1A K1 124.8(10) . . ?
C61 O1A K1 109.7(2) . . ?
O1A C61 C62 110.0(5) . . ?
O1A C61 H61A 109.7 . . ?
C62 C61 H61A 109.7 . . ?
O1A C61 H61B 109.7 . . ?
C62 C61 H61B 109.7 . . ?
H61A C61 H61B 108.2 . . ?
C61 C62 C63 99.9(7) . . ?
C61 C62 H62A 111.8 . . ?
C63 C62 H62A 111.8 . . ?
C61 C62 H62B 111.8 . . ?
C63 C62 H62B 111.8 . . ?
H62A C62 H62B 109.5 . . ?
C64 C63 C62 102.7(10) . . ?
C64 C63 H63A 111.2 . . ?
C62 C63 H63A 111.2 . . ?
C64 C63 H63B 111.2 . . ?
C62 C63 H63B 111.2 . . ?
H63A C63 H63B 109.1 . . ?
O1A C64 C63 105.3(9) . . ?
O1A C64 H64A 110.7 . . ?
C63 C64 H64A 110.7 . . ?
O1A C64 H64B 110.7 . . ?
C63 C64 H64B 110.7 . . ?
H64A C64 H64B 108.8 . . ?
C74 O1B C71 110.8(5) . . ?
C74 O1B K1 120.4(8) . . ?
C71 O1B K1 109.7(2) . . ?
O1B C71 C72 103.8(5) . . ?
O1B C71 H71A 111.0 . . ?
C72 C71 H71A 111.0 . . ?
O1B C71 H71B 111.0 . . ?
C72 C71 H71B 111.0 . . ?
H71A C71 H71B 109.0 . . ?
C71 C72 C73 104.6(7) . . ?
C71 C72 H72A 110.8 . . ?
C73 C72 H72A 110.8 . . ?
C71 C72 H72B 110.8 . . ?
C73 C72 H72B 110.8 . . ?
H72A C72 H72B 108.9 . . ?
C74 C73 C72 100.1(9) . . ?
C74 C73 H73A 111.8 . . ?
C72 C73 H73A 111.8 . . ?
C74 C73 H73B 111.8 . . ?
C72 C73 H73B 111.8 . . ?
H73A C73 H73B 109.5 . . ?
O1B C74 C73 106.6(8) . . ?
O1B C74 H74A 110.4 . . ?
C73 C74 H74A 110.4 . . ?
O1B C74 H74B 110.4 . . ?
C73 C74 H74B 110.4 . . ?
H74A C74 H74B 108.6 . . ?
C65 O2 C68 110.0(4) . . ?
C65 O2 K1 123.4(3) . . ?
C68 O2 K1 124.3(3) . . ?
C66 C67 C68 101.8(4) . . ?
C66 C67 H67A 111.4 . . ?
C68 C67 H67A 111.4 . . ?
C66 C67 H67B 111.4 . . ?
C68 C67 H67B 111.4 . . ?
H67A C67 H67B 109.3 . . ?
C53 O3A C50 103(2) . . ?
C53 O3A K4 115.4(19) . . ?
C50 O3A K4 138.1(18) . . ?
O3A C50 C51 106(2) . . ?
O3A C50 H50A 110.5 . . ?
C51 C50 H50A 110.5 . . ?
O3A C50 H50B 110.5 . . ?
C51 C50 H50B 110.5 . . ?
H50A C50 H50B 108.7 . . ?
C50 C51 C52 99(2) . . ?
C50 C51 H51A 111.9 . . ?
C52 C51 H51A 111.9 . . ?
C50 C51 H51B 111.9 . . ?
C52 C51 H51B 111.9 . . ?
H51A C51 H51B 109.6 . . ?
C53 C52 C51 105(2) . . ?
C53 C52 H52A 110.8 . . ?
C51 C52 H52A 110.8 . . ?
C53 C52 H52B 110.8 . . ?
C51 C52 H52B 110.8 . . ?
H52A C52 H52B 108.8 . . ?
O3A C53 C52 96(2) . . ?
O3A C53 K4 42.3(14) . . ?
C52 C53 K4 107.0(19) . . ?
O3A C53 H53A 112.6 . . ?
C52 C53 H53A 112.6 . . ?
K4 C53 H53A 70.8 . . ?
O3A C53 H53B 112.6 . . ?
C52 C53 H53B 112.6 . . ?
K4 C53 H53B 135.4 . . ?
H53A C53 H53B 110.1 . . ?
C58 O3B C55 109.9(4) . . ?
C58 O3B K4 117.6(3) . . ?
C55 O3B K4 123.7(3) . . ?
O3B C55 C56 106.3(4) . . ?
O3B C55 H55A 110.5 . . ?
C56 C55 H55A 110.5 . . ?
O3B C55 H55B 110.5 . . ?
C56 C55 H55B 110.5 . . ?
H55A C55 H55B 108.7 . . ?
C55 C56 C57 103.1(4) . . ?
C55 C56 H56A 111.2 . . ?
C57 C56 H56A 111.2 . . ?
C55 C56 H56B 111.2 . . ?
C57 C56 H56B 111.2 . . ?
H56A C56 H56B 109.1 . . ?
C58 C57 C56 101.3(4) . . ?
C58 C57 H57A 111.5 . . ?
C56 C57 H57A 111.5 . . ?
C58 C57 H57B 111.5 . . ?
C56 C57 H57B 111.5 . . ?
H57A C57 H57B 109.3 . . ?
O3B C58 C57 105.3(4) . . ?
O3B C58 H58A 110.7 . . ?
C57 C58 H58A 110.7 . . ?
O3B C58 H58B 110.7 . . ?
C57 C58 H58B 110.7 . . ?
H58A C58 H58B 108.8 . . ?
O2 K1 N1 81.39(10) . . ?
O2 K1 O1B 82.36(9) . . ?
N1 K1 O1B 75.71(9) . . ?
O2 K1 O1A 82.36(9) . . ?
N1 K1 O1A 75.71(9) . . ?
O2 K1 N12 95.42(10) . 4_365 ?
N1 K1 N12 173.22(10) . 4_365 ?
O1B K1 N12 97.99(9) . 4_365 ?
O1A K1 N12 97.99(9) . 4_365 ?
O2 K1 N4 83.62(10) . 1_455 ?
N1 K1 N4 112.83(10) . 1_455 ?
O1B K1 N4 162.24(9) . 1_455 ?
O1A K1 N4 162.24(9) . 1_455 ?
N12 K1 N4 72.55(9) 4_365 1_455 ?
O2 K1 N6 146.28(10) . 4_465 ?
N1 K1 N6 81.96(10) . 4_465 ?
O1B K1 N6 65.17(8) . 4_465 ?
O1A K1 N6 65.17(8) . 4_465 ?
N12 K1 N6 97.78(9) 4_365 4_465 ?
N4 K1 N6 129.97(10) 1_455 4_465 ?
O2 K1 N8 146.98(10) . 1_455 ?
N1 K1 N8 93.88(10) . 1_455 ?
O1B K1 N8 128.35(8) . 1_455 ?
O1A K1 N8 128.35(8) . 1_455 ?
N12 K1 N8 92.03(9) 4_365 1_455 ?
N4 K1 N8 68.06(9) 1_455 1_455 ?
N6 K1 N8 63.29(8) 4_465 1_455 ?
O2 K1 K3 123.54(7) . 1_355 ?
N1 K1 K3 135.79(8) . 1_355 ?
O1B K1 K3 137.22(6) . 1_355 ?
O1A K1 K3 137.22(6) . 1_355 ?
N12 K1 K3 50.85(7) 4_365 1_355 ?
N4 K1 K3 46.90(6) 1_455 1_355 ?
N6 K1 K3 88.33(7) 4_465 1_355 ?
N8 K1 K3 44.42(6) 1_455 1_355 ?
O2 K1 K2 107.68(7) . 4_465 ?
N1 K1 K2 46.53(7) . 4_465 ?
O1B K1 K2 45.05(6) . 4_465 ?
O1A K1 K2 45.05(6) . 4_465 ?
N12 K1 K2 130.03(7) 4_365 4_465 ?
N4 K1 K2 151.50(7) 1_455 4_465 ?
N6 K1 K2 42.11(7) 4_465 4_465 ?
N8 K1 K2 91.49(6) 1_455 4_465 ?
K3 K1 K2 128.78(3) 1_355 4_465 ?
C6 N1 K1 156.8(3) . . ?
C6 N1 K2 110.2(3) . 4_465 ?
K1 N1 K2 91.69(10) . 4_465 ?
F21 C1 C28 116.7(4) . . ?
F21 C1 C27 120.1(3) . . ?
C28 C1 C27 123.2(4) . . ?
C4 B1 C25 107.9(3) . . ?
C4 B1 C26 105.9(3) . . ?
C25 B1 C26 109.5(3) . . ?
C4 B1 C27 112.4(3) . . ?
C25 B1 C27 106.2(3) . . ?
C26 B1 C27 114.7(3) . . ?
C17 B2 C5 106.4(3) . . ?
C17 B2 C16 104.7(3) . . ?
C5 B2 C16 110.7(3) . . ?
C17 B2 C18 114.1(3) . . ?
C5 B2 C18 110.4(3) . . ?
C16 B2 C18 110.5(3) . . ?
C7 N2 K4 140.9(3) . 4_466 ?
C7 N2 K2 127.1(3) . 1_455 ?
K4 N2 K2 86.22(9) 4_466 1_455 ?
N9 K2 N11 100.57(10) . . ?
N9 K2 N6 101.05(10) . . ?
N11 K2 N6 157.99(10) . . ?
N9 K2 N7 145.60(10) . 4_566 ?
N11 K2 N7 80.64(9) . 4_566 ?
N6 K2 N7 79.24(9) . 4_566 ?
N9 K2 N1 141.42(10) . 4_666 ?
N11 K2 N1 85.62(10) . 4_666 ?
N6 K2 N1 80.03(10) . 4_666 ?
N7 K2 N1 72.90(9) 4_566 4_666 ?
N9 K2 N2 77.65(10) . 1_655 ?
N11 K2 N2 67.84(10) . 1_655 ?
N6 K2 N2 113.20(10) . 1_655 ?
N7 K2 N2 71.00(9) 4_566 1_655 ?
N1 K2 N2 137.88(9) 4_666 1_655 ?
N9 K2 K4 117.05(8) . 4_566 ?
N11 K2 K4 44.92(7) . 4_566 ?
N6 K2 K4 119.41(7) . 4_566 ?
N7 K2 K4 42.69(7) 4_566 4_566 ?
N1 K2 K4 94.29(7) 4_666 4_566 ?
N2 K2 K4 43.85(6) 1_655 4_566 ?
N9 K2 K1 115.15(8) . 4_666 ?
N11 K2 K1 126.55(8) . 4_666 ?
N6 K2 K1 44.70(7) . 4_666 ?
N7 K2 K1 89.50(7) 4_566 4_666 ?
N1 K2 K1 41.79(7) 4_666 4_666 ?
N2 K2 K1 154.40(7) 1_655 4_666 ?
K4 K2 K1 127.68(3) 4_566 4_666 ?
N11 C3 B3 178.0(4) . . ?
C8 N3 K3 122.3(3) . 1_455 ?
C8 N3 K4 128.3(3) . 1_455 ?
K3 N3 K4 92.04(10) 1_455 1_455 ?
C3 B3 C33 110.0(3) . . ?
C3 B3 C34 105.5(3) . . ?
C33 B3 C34 106.7(3) . . ?
C3 B3 C35 111.1(3) . . ?
C33 B3 C35 109.3(3) . . ?
C34 B3 C35 114.1(3) . . ?
N10 K3 N3 77.00(10) . 1_655 ?
N10 K3 N8 99.87(10) . 1_655 ?
N3 K3 N8 160.20(10) 1_655 1_655 ?
N10 K3 O4 82.41(9) . . ?
N3 K3 O4 68.45(9) 1_655 . ?
N8 K3 O4 91.79(9) 1_655 . ?
N10 K3 N4 80.96(9) . 1_655 ?
N3 K3 N4 123.60(10) 1_655 1_655 ?
N8 K3 N4 74.34(9) 1_655 1_655 ?
O4 K3 N4 156.07(8) . 1_655 ?
N10 K3 N5 147.45(9) . 4_665 ?
N3 K3 N5 84.54(9) 1_655 4_665 ?
N8 K3 N5 88.52(9) 1_655 4_665 ?
O4 K3 N5 65.82(8) . 4_665 ?
N4 K3 N5 131.45(9) 1_655 4_665 ?
N10 K3 N12 140.21(10) . 4_565 ?
N3 K3 N12 98.98(9) 1_655 4_565 ?
N8 K3 N12 95.70(9) 1_655 4_565 ?
O4 K3 N12 133.60(8) . 4_565 ?
N4 K3 N12 68.37(9) 1_655 4_565 ?
N5 K3 N12 68.67(8) 4_665 4_565 ?
N10 K3 F7 77.11(8) . 1_655 ?
N3 K3 F7 62.94(8) 1_655 1_655 ?
N8 K3 F7 136.01(8) 1_655 1_655 ?
O4 K3 F7 130.21(7) . 1_655 ?
N4 K3 F7 61.77(7) 1_655 1_655 ?
N5 K3 F7 117.72(8) 4_665 1_655 ?
N12 K3 F7 66.44(7) 4_565 1_655 ?
N10 K3 K1 123.89(8) . 1_755 ?
N3 K3 K1 143.22(7) 1_655 1_755 ?
N8 K3 K1 54.26(7) 1_655 1_755 ?
O4 K3 K1 137.55(6) . 1_755 ?
N4 K3 K1 46.54(6) 1_655 1_755 ?
N5 K3 K1 86.49(6) 4_665 1_755 ?
N12 K3 K1 44.87(6) 4_565 1_755 ?
F7 K3 K1 90.56(4) 1_655 1_755 ?
N10 K3 K4 107.35(7) . . ?
N3 K3 K4 44.69(7) 1_655 . ?
N8 K3 K4 120.82(7) 1_655 . ?
O4 K3 K4 43.69(5) . . ?
N4 K3 K4 159.70(7) 1_655 . ?
N5 K3 K4 43.86(6) 4_665 . ?
N12 K3 K4 95.27(6) 4_565 . ?
F7 K3 K4 101.32(4) 1_655 . ?
K1 K3 K4 128.76(3) 1_755 . ?
C6 B4 C8 106.2(3) . . ?
C6 B4 C7 107.6(3) . . ?
C8 B4 C7 108.5(3) . . ?
C6 B4 C9 114.3(3) . . ?
C8 B4 C9 111.2(3) . . ?
C7 B4 C9 108.8(3) . . ?
C5 N4 K1 146.7(3) . 1_655 ?
C5 N4 K3 126.7(3) . 1_455 ?
K1 N4 K3 86.56(9) 1_655 1_455 ?
O3A K4 N7 77.5(5) . . ?
O3B K4 N7 89.38(11) . . ?
O3A K4 O4 89.1(6) . . ?
O3B K4 O4 84.10(11) . . ?
N7 K4 O4 121.07(9) . . ?
O3A K4 N5 125.2(5) . 4_665 ?
O3B K4 N5 113.19(11) . 4_665 ?
N7 K4 N5 156.74(10) . 4_665 ?
O4 K4 N5 69.30(8) . 4_665 ?
O3A K4 N2 78.9(7) . 4_665 ?
O3B K4 N2 80.16(12) . 4_665 ?
N7 K4 N2 75.91(10) . 4_665 ?
O4 K4 N2 156.78(9) . 4_665 ?
N5 K4 N2 101.51(10) 4_665 4_665 ?
O3A K4 N3 130.6(7) . 1_655 ?
O3B K4 N3 136.49(12) . 1_655 ?
N7 K4 N3 78.83(9) . 1_655 ?
O4 K4 N3 67.64(8) . 1_655 ?
N5 K4 N3 87.71(9) 4_665 1_655 ?
N2 K4 N3 134.75(10) 4_665 1_655 ?
O3A K4 N11 144.7(6) . 4_565 ?
O3B K4 N11 150.01(12) . 4_565 ?
N7 K4 N11 78.51(9) . 4_565 ?
O4 K4 N11 125.66(9) . 4_565 ?
N5 K4 N11 78.90(9) 4_665 4_565 ?
N2 K4 N11 70.35(10) 4_665 4_565 ?
N3 K4 N11 68.21(9) 1_655 4_565 ?
O3A K4 C53 22.3(5) . . ?
N7 K4 C53 99.8(5) . . ?
O4 K4 C53 77.2(4) . . ?
N5 K4 C53 102.9(5) 4_665 . ?
N2 K4 C53 84.6(4) 4_665 . ?
N3 K4 C53 136.8(5) 1_655 . ?
N11 K4 C53 154.6(5) 4_565 . ?
O3A K4 C80 76.9(7) . . ?
O3B K4 C80 76.40(13) . . ?
N7 K4 C80 97.92(9) . . ?
O4 K4 C80 23.94(8) . . ?
N5 K4 C80 93.08(9) 4_665 . ?
N2 K4 C80 155.84(10) 4_665 . ?
N3 K4 C80 64.26(10) 1_655 . ?
N11 K4 C80 132.06(10) 4_565 . ?
C53 K4 C80 73.3(5) . . ?
O3A K4 K3 133.0(6) . . ?
O3B K4 K3 127.12(10) . . ?
N7 K4 K3 122.00(7) . . ?
O4 K4 K3 43.97(5) . . ?
N5 K4 K3 48.68(7) 4_665 . ?
N2 K4 K3 143.54(8) 4_665 . ?
N3 K4 K3 43.27(7) 1_655 . ?
N11 K4 K3 81.94(7) 4_565 . ?
C53 K4 K3 118.6(4) . . ?
C80 K4 K3 59.33(7) . . ?
O3A K4 K2 103.9(5) . 4_565 ?
O3B K4 K2 112.70(10) . 4_565 ?
N7 K4 K2 43.00(7) . 4_565 ?
O4 K4 K2 153.28(6) . 4_565 ?
N5 K4 K2 117.97(7) 4_665 4_565 ?
N2 K4 K2 49.93(7) 4_665 4_565 ?
N3 K4 K2 86.47(7) 1_655 4_565 ?
N11 K4 K2 42.22(7) 4_565 4_565 ?
C53 K4 K2 122.0(4) . 4_565 ?
C80 K4 K2 136.85(7) . 4_565 ?
K3 K4 K2 119.15(3) . 4_565 ?
C83 O4 C80 105.1(3) . . ?
C83 O4 K4 127.8(2) . . ?
C80 O4 K4 102.9(2) . . ?
C83 O4 K3 109.7(2) . . ?
C80 O4 K3 120.1(2) . . ?
K4 O4 K3 92.34(7) . . ?
N9 C4 B1 177.3(4) . . ?
C16 N5 K4 138.7(3) . 4_466 ?
C16 N5 K3 116.9(3) . 4_466 ?
K4 N5 K3 87.46(9) 4_466 4_466 ?
N4 C5 B2 175.5(4) . . ?
C17 N6 K2 139.7(3) . . ?
C17 N6 K1 125.8(3) . 4_666 ?
K2 N6 K1 93.18(10) . 4_666 ?
N1 C6 B4 176.4(4) . . ?
C14 F7 K3 129.4(2) . 1_455 ?
C25 N7 K4 142.4(3) . . ?
C25 N7 K2 120.2(3) . 4_565 ?
K4 N7 K2 94.31(10) . 4_565 ?
N2 C7 B4 178.8(4) . . ?
N3 C8 B4 177.4(4) . . ?
C26 N8 K3 167.7(3) . 1_455 ?
C26 N8 K1 104.1(3) . 1_655 ?
K3 N8 K1 81.32(9) 1_455 1_655 ?
C10 C9 C14 113.1(4) . . ?
C10 C9 B4 125.7(4) . . ?
C14 C9 B4 121.2(3) . . ?
C4 N9 K2 167.2(3) . . ?
C3 N11 K2 139.5(3) . . ?
C3 N11 K4 117.7(3) . 4_566 ?
K2 N11 K4 92.85(10) . 4_566 ?
F2 C11 C12 121.2(4) . . ?
F2 C11 C10 117.4(4) . . ?
C12 C11 C10 121.4(4) . . ?
C34 N12 K1 147.9(3) . 4_766 ?
C34 N12 K3 115.2(3) . 4_566 ?
K1 N12 K3 84.28(9) 4_766 4_566 ?
C11 C12 C13 116.2(4) . . ?
C11 C12 C15 123.8(4) . . ?
C13 C12 C15 120.0(4) . . ?
F6 C13 C14 119.1(4) . . ?
F6 C13 C12 119.5(4) . . ?
C14 C13 C12 121.4(4) . . ?
F4 C15 F3 108.7(4) . . ?
F4 C15 F5 107.2(5) . . ?
F3 C15 F5 103.9(4) . . ?
F4 C15 C12 112.7(4) . . ?
F3 C15 C12 113.2(4) . . ?
F5 C15 C12 110.8(4) . . ?
F7 C14 C13 117.5(4) . . ?
F7 C14 C9 118.7(3) . . ?
C13 C14 C9 123.8(4) . . ?
N5 C16 B2 174.6(4) . . ?
N6 C17 B2 176.0(4) . . ?
C19 C18 C23 113.3(4) . . ?
C19 C18 B2 125.2(3) . . ?
C23 C18 B2 121.5(3) . . ?
F17 C19 C20 116.5(4) . . ?
F17 C19 C18 120.2(3) . . ?
C20 C19 C18 123.4(4) . . ?
F16 C20 C21 120.7(4) . . ?
F16 C20 C19 117.1(4) . . ?
C21 C20 C19 122.2(4) . . ?
C20 C21 C22 115.6(4) . . ?
C20 C21 C24 124.8(4) . . ?
C22 C21 C24 119.5(4) . . ?
F12 C22 C23 119.0(4) . . ?
F12 C22 C21 119.5(4) . . ?
C23 C22 C21 121.5(4) . . ?
F11 C23 C22 117.4(4) . . ?
F11 C23 C18 118.5(3) . . ?
C22 C23 C18 124.1(4) . . ?
F14 C24 F13 106.9(4) . . ?
F14 C24 F15 106.6(4) . . ?
F13 C24 F15 106.0(4) . . ?
F14 C24 C21 112.4(4) . . ?
F13 C24 C21 111.1(4) . . ?
F15 C24 C21 113.3(4) . . ?
F22 C28 C1 118.7(4) . . ?
F22 C28 C29 119.6(4) . . ?
C1 C28 C29 121.8(4) . . ?
C1 C27 C31 114.2(4) . . ?
C1 C27 B1 126.2(3) . . ?
C31 C27 B1 119.4(3) . . ?
N8 C26 B1 175.5(4) . . ?
N7 C25 B1 174.8(4) . . ?
C28 C29 C30 116.4(4) . . ?
C28 C29 C32 118.9(4) . . ?
C30 C29 C32 124.6(4) . . ?
F1 C10 C11 116.2(4) . . ?
F1 C10 C9 119.8(4) . . ?
C11 C10 C9 124.1(4) . . ?
C33 N10 K3 166.8(3) . . ?
F26 C30 C31 117.8(4) . . ?
F26 C30 C29 121.5(4) . . ?
C31 C30 C29 120.6(4) . . ?
F27 C31 C30 116.8(4) . . ?
F27 C31 C27 119.4(3) . . ?
C30 C31 C27 123.8(4) . . ?
F25 C32 F23 107.8(4) . . ?
F25 C32 F24 107.7(4) . . ?
F23 C32 F24 106.6(4) . . ?
F25 C32 C29 113.0(4) . . ?
F23 C32 C29 110.9(4) . . ?
F24 C32 C29 110.5(4) . . ?
N10 C33 B3 177.4(4) . . ?
N12 C34 B3 174.7(4) . . ?
C40 C35 C36 113.7(4) . . ?
C40 C35 B3 122.5(3) . . ?
C36 C35 B3 123.6(3) . . ?
F31 C36 C37 116.2(4) . . ?
F31 C36 C35 120.0(3) . . ?
C37 C36 C35 123.8(4) . . ?
F32 C37 C36 117.6(4) . . ?
F32 C37 C38 121.3(4) . . ?
C36 C37 C38 121.1(4) . . ?
C37 C38 C39 116.1(4) . . ?
C37 C38 C41 125.2(4) . . ?
C39 C38 C41 118.7(4) . . ?
F36 C39 C40 118.7(4) . . ?
F36 C39 C38 119.3(4) . . ?
C40 C39 C38 121.9(4) . . ?
F37 C40 C39 117.8(4) . . ?
F37 C40 C35 118.9(3) . . ?
C39 C40 C35 123.3(4) . . ?
F35 C41 F34 107.3(4) . . ?
F35 C41 F33 107.1(4) . . ?
F34 C41 F33 105.3(4) . . ?
F35 C41 C38 112.5(4) . . ?
F34 C41 C38 110.9(4) . . ?
F33 C41 C38 113.4(4) . . ?
O4 C80 C81 106.2(3) . . ?
O4 C80 K4 53.18(16) . . ?
C81 C80 K4 157.6(3) . . ?
O4 C80 H80A 110.5 . . ?
C81 C80 H80A 110.5 . . ?
K4 C80 H80A 87.3 . . ?
O4 C80 H80B 110.5 . . ?
C81 C80 H80B 110.5 . . ?
K4 C80 H80B 74.4 . . ?
H80A C80 H80B 108.7 . . ?
C80 C81 C82 104.0(3) . . ?
C80 C81 H81A 111.0 . . ?
C82 C81 H81A 111.0 . . ?
C80 C81 H81B 111.0 . . ?
C82 C81 H81B 111.0 . . ?
H81A C81 H81B 109.0 . . ?
C83 C82 C81 104.2(3) . . ?
C83 C82 H82A 110.9 . . ?
C81 C82 H82A 110.9 . . ?
C83 C82 H82B 110.9 . . ?
C81 C82 H82B 110.9 . . ?
H82A C82 H82B 108.9 . . ?
O4 C83 C82 104.0(3) . . ?
O4 C83 H83A 111.0 . . ?
C82 C83 H83A 111.0 . . ?
O4 C83 H83B 111.0 . . ?
C82 C83 H83B 111.0 . . ?
H83A C83 H83B 109.0 . . ?
O2 C65 C66 105.8(5) . . ?
O2 C65 H65A 110.6 . . ?
C66 C65 H65A 110.6 . . ?
O2 C65 H65B 110.6 . . ?
C66 C65 H65B 110.6 . . ?
H65A C65 H65B 108.7 . . ?
C65 C66 C67 103.6(5) . . ?
C65 C66 H66A 111.0 . . ?
C67 C66 H66A 111.0 . . ?
C65 C66 H66B 111.0 . . ?
C67 C66 H66B 111.0 . . ?
H66A C66 H66B 109.0 . . ?
O2 C68 C67 105.8(5) . . ?
O2 C68 H68A 110.6 . . ?
C67 C68 H68A 110.6 . . ?
O2 C68 H68B 110.6 . . ?
C67 C68 H68B 110.6 . . ?
H68A C68 H68B 108.7 . . ?

_refine_diff_density_max         0.544
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.082

