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

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

data_h13msh17
_database_code_depnum_ccdc_archive 'CCDC 1043568'
_audit_update_record             
;
2015-01-14 deposited with the CCDC.
2015-03-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        h13msh17
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H58 B4 K2 N4 O3'
_chemical_formula_sum            'C20 H58 B4 K2 N4 O3'
_chemical_formula_weight         524.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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                   12.5404(3)
_cell_length_b                   17.0035(4)
_cell_length_c                   15.9352(4)
_cell_angle_alpha                90
_cell_angle_beta                 106.6308(12)
_cell_angle_gamma                90
_cell_volume                     3255.74(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    66332
_cell_measurement_theta_min      2.910
_cell_measurement_theta_max      26.022

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_F_000             1152
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    0.316
_shelx_estimated_absorpt_T_min   0.858
_shelx_estimated_absorpt_T_max   0.925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.660
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '337 1.7 degree images with φ and ω scans'
_diffrn_reflns_number            61939
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_av_R_equivalents  0.0977
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.626
_diffrn_reflns_theta_max         26.051
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             6385
_reflns_number_gt                4665
_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       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        
;
 DENZO-SCALEPACK Z. Otwinowski and W. Minor, " 
 Processing of X-ray Diffraction Data Collected in Oscillation Mode ", 
 Methods in Enzymology, Volume 276: Macromolecular Crystallography, 
 part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press.
;
_computing_structure_solution    
; 
 SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , 
 Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. 
 (1999) J. Appl. Cryst. 32, 115-119
;
_computing_structure_refinement  
;
 SHELXL-2013 (Sheldrick, 2013)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. Hübschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_molecular_graphics    
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'

_computing_publication_material  
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0477P)²+1.1465P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6385
_refine_ls_number_parameters     346
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0424
_refine_ls_wR_factor_ref         0.1096
_refine_ls_wR_factor_gt          0.0962
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_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 0.80967(3) 0.27195(2) 0.66205(3) 0.03335(12) Uani 1 1 d . . . . .
K2 K 0.66486(4) 0.19647(3) 0.39680(3) 0.03816(13) Uani 1 1 d . . . . .
B1 B 0.93020(18) 0.21907(13) 0.52266(14) 0.0298(5) Uani 1 1 d . . . . .
H1D H 0.8783(16) 0.2744(11) 0.4911(13) 0.035(5) Uiso 1 1 d . . . . .
H1E H 0.8736(16) 0.1695(11) 0.5291(12) 0.033(5) Uiso 1 1 d . . . . .
B2 B 0.8974(2) 0.16666(15) 0.35940(15) 0.0369(5) Uani 1 1 d . . . . .
H2D H 0.8463(18) 0.2227(13) 0.3348(14) 0.044(6) Uiso 1 1 d . . . . .
H2E H 0.8430(16) 0.1153(12) 0.3714(13) 0.038(5) Uiso 1 1 d . . . . .
H2F H 0.9429(18) 0.1477(12) 0.3113(14) 0.046(6) Uiso 1 1 d . . . . .
B3 B 0.5475(2) 0.27766(15) 0.52526(15) 0.0378(5) Uani 1 1 d . . . . .
H3D H 0.5662(17) 0.2142(13) 0.5485(14) 0.043(6) Uiso 1 1 d . . . . .
H3E H 0.6310(17) 0.3107(12) 0.5312(13) 0.038(5) Uiso 1 1 d . . . . .
B4 B 0.5703(2) 0.31859(18) 0.69222(16) 0.0460(6) Uani 1 1 d . . . . .
H4D H 0.594(2) 0.2537(15) 0.7085(15) 0.057(7) Uiso 1 1 d . . . . .
H4E H 0.6468(19) 0.3557(13) 0.6933(15) 0.052(6) Uiso 1 1 d . . . . .
H4F H 0.5196(19) 0.3426(13) 0.7342(15) 0.053(6) Uiso 1 1 d . . . . .
N1 N 1.00688(13) 0.24115(10) 0.61001(10) 0.0366(4) Uani 1 1 d . . . . .
N2 N 0.98776(12) 0.18657(9) 0.44936(10) 0.0312(4) Uani 1 1 d . . . . .
N3 N 0.47949(14) 0.27588(10) 0.43038(11) 0.0401(4) Uani 1 1 d . . . . .
N4 N 0.49028(13) 0.31971(10) 0.59456(11) 0.0386(4) Uani 1 1 d . . . . .
O1 O 0.81850(15) 0.11777(9) 0.72136(10) 0.0532(4) Uani 1 1 d . . . . .
O2 O 0.82797(15) 0.42609(8) 0.61690(10) 0.0529(4) Uani 1 1 d . . . . .
O3 O 0.61531(13) 0.04629(9) 0.43399(10) 0.0490(4) Uani 1 1 d . . . . .
C1 C 1.06226(19) 0.31666(14) 0.62739(15) 0.0491(6) Uani 1 1 d . . . . .
H1A H 1.1399 0.3109 0.6272 0.074 Uiso 1 1 calc R U . . .
H1B H 1.0598 0.3359 0.6848 0.074 Uiso 1 1 calc R U . . .
H1C H 1.0245 0.3543 0.5820 0.074 Uiso 1 1 calc R U . . .
C2 C 1.0581(2) 0.18453(15) 0.67663(14) 0.0506(6) Uani 1 1 d . . . . .
H2A H 1.1365 0.1780 0.6789 0.076 Uiso 1 1 calc R U . . .
H2B H 1.0196 0.1339 0.6627 0.076 Uiso 1 1 calc R U . . .
H2C H 1.0529 0.2031 0.7336 0.076 Uiso 1 1 calc R U . . .
C3 C 1.06377(19) 0.24729(16) 0.43279(15) 0.0519(6) Uani 1 1 d . . . . .
H3A H 1.0983 0.2280 0.3888 0.078 Uiso 1 1 calc R U . . .
H3B H 1.1218 0.2587 0.4873 0.078 Uiso 1 1 calc R U . . .
H3C H 1.0216 0.2953 0.4113 0.078 Uiso 1 1 calc R U . . .
C4 C 1.0531(2) 0.11528(15) 0.48149(15) 0.0565(7) Uani 1 1 d . . . . .
H4A H 1.0828 0.0943 0.4355 0.085 Uiso 1 1 calc R U . . .
H4B H 1.0052 0.0758 0.4972 0.085 Uiso 1 1 calc R U . . .
H4C H 1.1147 0.1283 0.5332 0.085 Uiso 1 1 calc R U . . .
C5 C 0.4742(2) 0.34229(16) 0.37235(15) 0.0591(7) Uani 1 1 d . . . . .
H5A H 0.4057 0.3720 0.3673 0.089 Uiso 1 1 calc R U . . .
H5B H 0.4746 0.3233 0.3144 0.089 Uiso 1 1 calc R U . . .
H5C H 0.5387 0.3765 0.3961 0.089 Uiso 1 1 calc R U . . .
C6 C 0.3889(2) 0.22176(17) 0.39640(17) 0.0614(7) Uani 1 1 d . . . . .
H6A H 0.3182 0.2480 0.3931 0.092 Uiso 1 1 calc R U . . .
H6B H 0.3979 0.1760 0.4352 0.092 Uiso 1 1 calc R U . . .
H6C H 0.3889 0.2045 0.3377 0.092 Uiso 1 1 calc R U . . .
C7 C 0.3862(2) 0.27873(19) 0.59297(17) 0.0639(7) Uani 1 1 d . . . . .
H7A H 0.3526 0.3038 0.6347 0.096 Uiso 1 1 calc R U . . .
H7B H 0.4023 0.2235 0.6092 0.096 Uiso 1 1 calc R U . . .
H7C H 0.3343 0.2817 0.5339 0.096 Uiso 1 1 calc R U . . .
C8 C 0.4633(2) 0.40250(15) 0.56847(16) 0.0585(7) Uani 1 1 d . . . . .
H8A H 0.4296 0.4277 0.6101 0.088 Uiso 1 1 calc R U . . .
H8B H 0.4108 0.4042 0.5096 0.088 Uiso 1 1 calc R U . . .
H8C H 0.5316 0.4305 0.5684 0.088 Uiso 1 1 calc R U . . .
C11 C 0.7860(2) 0.09338(14) 0.79557(16) 0.0532(6) Uani 1 1 d . . . . .
H11A H 0.7095 0.1115 0.7907 0.064 Uiso 1 1 calc R U . . .
H11B H 0.8369 0.1157 0.8497 0.064 Uiso 1 1 calc R U . . .
C12 C 0.7912(2) 0.00471(14) 0.79808(16) 0.0586(7) Uani 1 1 d . . . . .
H12A H 0.7204 -0.0177 0.8032 0.070 Uiso 1 1 calc R U . . .
H12B H 0.8528 -0.0136 0.8483 0.070 Uiso 1 1 calc R U . . .
C13 C 0.8110(2) -0.01909(14) 0.71214(16) 0.0563(6) Uani 1 1 d . . . . .
H13A H 0.8882 -0.0379 0.7213 0.068 Uiso 1 1 calc R U . . .
H13B H 0.7587 -0.0610 0.6830 0.068 Uiso 1 1 calc R U . . .
C14 C 0.7904(2) 0.05529(14) 0.65929(15) 0.0548(6) Uani 1 1 d . . . . .
H14A H 0.8375 0.0571 0.6190 0.066 Uiso 1 1 calc R U . . .
H14B H 0.7113 0.0589 0.6244 0.066 Uiso 1 1 calc R U . . .
C15 C 0.8152(2) 0.49081(13) 0.66982(16) 0.0562(6) Uani 1 1 d . . . . .
H15A H 0.8571 0.4815 0.7318 0.067 Uiso 1 1 calc R U . . .
H15B H 0.7358 0.4986 0.6660 0.067 Uiso 1 1 calc R U . . .
C16 C 0.8604(2) 0.56167(13) 0.63488(15) 0.0518(6) Uani 1 1 d . . . . .
H16A H 0.9368 0.5741 0.6713 0.062 Uiso 1 1 calc R U . . .
H16B H 0.8123 0.6081 0.6333 0.062 Uiso 1 1 calc R U . . .
C17 C 0.8602(2) 0.53743(13) 0.54240(15) 0.0495(6) Uani 1 1 d . . . . .
H17A H 0.8160 0.5747 0.4983 0.059 Uiso 1 1 calc R U . . .
H17B H 0.9369 0.5351 0.5372 0.059 Uiso 1 1 calc R U . . .
C18 C 0.8075(2) 0.45731(13) 0.53109(14) 0.0503(6) Uani 1 1 d . . . . .
H18A H 0.7265 0.4613 0.5022 0.060 Uiso 1 1 calc R U . . .
H18B H 0.8412 0.4234 0.4950 0.060 Uiso 1 1 calc R U . . .
C19 C 0.69533(19) -0.01355(14) 0.43599(16) 0.0502(6) Uani 1 1 d . . . . .
H19A H 0.6939 -0.0539 0.4804 0.060 Uiso 1 1 calc R U . . .
H19B H 0.7712 0.0090 0.4497 0.060 Uiso 1 1 calc R U . . .
C20 C 0.6613(2) -0.04808(16) 0.34595(18) 0.0629(7) Uani 1 1 d . . . . .
H20A H 0.6852 -0.1036 0.3468 0.075 Uiso 1 1 calc R U . . .
H20B H 0.6933 -0.0179 0.3058 0.075 Uiso 1 1 calc R U . . .
C21 C 0.5352(2) -0.04159(17) 0.31881(19) 0.0692(8) Uani 1 1 d . . . . .
H21A H 0.5069 -0.0213 0.2583 0.083 Uiso 1 1 calc R U . . .
H21B H 0.5006 -0.0934 0.3223 0.083 Uiso 1 1 calc R U . . .
C22 C 0.5112(2) 0.01489(16) 0.38299(18) 0.0597(7) Uani 1 1 d . . . . .
H22A H 0.4622 0.0577 0.3518 0.072 Uiso 1 1 calc R U . . .
H22B H 0.4733 -0.0125 0.4213 0.072 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 2.7448(15) . ?
K1 O1 2.7781(15) . ?
K1 N1 2.8726(16) . ?
K1 B1 3.154(2) . ?
K1 B2 3.195(2) 4_566 ?
K1 B4 3.270(3) . ?
K1 B3 3.386(2) . ?
K1 K2 4.2915(6) . ?
K1 K2 4.6335(6) 4_566 ?
K1 H1D 3.083(19) . ?
K1 H1E 3.023(19) . ?
K1 H3E 2.67(2) . ?
K1 H4D 3.02(2) . ?
K1 H4E 2.65(2) . ?
K2 O3 2.7328(16) . ?
K2 N3 2.8679(17) . ?
K2 B4 3.144(3) 4_565 ?
K2 B3 3.160(2) . ?
K2 B2 3.180(2) . ?
K2 B1 3.380(2) . ?
K2 K1 4.6335(6) 4_565 ?
K2 H1D 2.979(19) . ?
K2 H1E 2.889(19) . ?
K2 H2D 2.76(2) . ?
K2 H2E 2.753(19) . ?
K2 H3D 3.03(2) . ?
K2 H3E 3.01(2) . ?
B1 N1 1.496(3) . ?
B1 N2 1.635(2) . ?
B1 H1D 1.17(2) . ?
B1 H1E 1.126(19) . ?
B2 N2 1.588(3) . ?
B2 K1 3.195(2) 4_565 ?
B2 H2D 1.15(2) . ?
B2 H2E 1.16(2) . ?
B2 H2F 1.13(2) . ?
B3 N3 1.509(3) . ?
B3 N4 1.643(3) . ?
B3 H3D 1.14(2) . ?
B3 H3E 1.17(2) . ?
B4 N4 1.592(3) . ?
B4 K2 3.144(3) 4_566 ?
B4 H4D 1.15(2) . ?
B4 H4E 1.14(2) . ?
B4 H4F 1.12(2) . ?
N1 C2 1.441(3) . ?
N1 C1 1.448(3) . ?
N2 C4 1.470(3) . ?
N2 C3 1.479(3) . ?
N3 C6 1.442(3) . ?
N3 C5 1.449(3) . ?
N4 C7 1.474(3) . ?
N4 C8 1.479(3) . ?
O1 C11 1.419(3) . ?
O1 C14 1.425(3) . ?
O2 C18 1.420(3) . ?
O2 C15 1.423(3) . ?
O3 C19 1.423(3) . ?
O3 C22 1.430(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C11 C12 1.509(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.515(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.500(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.504(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.530(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.502(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.495(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.520(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.495(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 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 172.76(5) . . ?
O2 K1 N1 87.42(5) . . ?
O1 K1 N1 88.42(5) . . ?
O2 K1 B1 89.70(5) . . ?
O1 K1 B1 89.43(5) . . ?
N1 K1 B1 28.25(5) . . ?
O2 K1 B2 85.12(6) . 4_566 ?
O1 K1 B2 90.26(6) . 4_566 ?
N1 K1 B2 105.14(5) . 4_566 ?
B1 K1 B2 133.37(6) . 4_566 ?
O2 K1 B4 87.48(6) . . ?
O1 K1 B4 97.34(6) . . ?
N1 K1 B4 171.43(6) . . ?
B1 K1 B4 144.85(6) . . ?
B2 K1 B4 81.27(6) 4_566 . ?
O2 K1 B3 86.70(6) . . ?
O1 K1 B3 100.54(6) . . ?
N1 K1 B3 125.23(5) . . ?
B1 K1 B3 97.32(6) . . ?
B2 K1 B3 128.44(6) 4_566 . ?
B4 K1 B3 47.54(6) . . ?
O2 K1 K2 94.07(3) . . ?
O1 K1 K2 90.99(3) . . ?
N1 K1 K2 79.50(3) . . ?
B1 K1 K2 51.25(4) . . ?
B2 K1 K2 175.23(5) 4_566 . ?
B4 K1 K2 94.01(5) . . ?
B3 K1 K2 46.79(4) . . ?
O2 K1 K2 100.51(3) . 4_566 ?
O1 K1 K2 79.71(3) . 4_566 ?
N1 K1 K2 145.38(4) . 4_566 ?
B1 K1 K2 168.28(4) . 4_566 ?
B2 K1 K2 43.26(4) 4_566 4_566 ?
B4 K1 K2 42.68(4) . 4_566 ?
B3 K1 K2 89.07(4) . 4_566 ?
K2 K1 K2 132.585(14) . 4_566 ?
O2 K1 H1D 71.9(4) . . ?
O1 K1 H1D 108.6(4) . . ?
N1 K1 H1D 42.8(4) . . ?
B1 K1 H1D 21.6(4) . . ?
B2 K1 H1D 139.5(4) 4_566 . ?
B4 K1 H1D 128.8(4) . . ?
B3 K1 H1D 84.0(4) . . ?
K2 K1 H1D 44.0(4) . . ?
K2 K1 H1D 170.0(4) 4_566 . ?
O2 K1 H1E 107.9(4) . . ?
O1 K1 H1E 72.6(4) . . ?
N1 K1 H1E 43.1(4) . . ?
B1 K1 H1E 20.9(4) . . ?
B2 K1 H1E 142.4(4) 4_566 . ?
B4 K1 H1E 133.0(4) . . ?
B3 K1 H1E 88.2(4) . . ?
K2 K1 H1E 42.2(4) . . ?
K2 K1 H1E 151.2(4) 4_566 . ?
H1D K1 H1E 36.1(5) . . ?
O2 K1 H3E 71.0(4) . . ?
O1 K1 H3E 116.2(4) . . ?
N1 K1 H3E 114.8(4) . . ?
B1 K1 H3E 89.1(4) . . ?
B2 K1 H3E 131.6(4) 4_566 . ?
B4 K1 H3E 56.9(4) . . ?
B3 K1 H3E 17.6(4) . . ?
K2 K1 H3E 44.0(4) . . ?
K2 K1 H3E 99.6(4) 4_566 . ?
H1D K1 H3E 72.0(6) . . ?
H1E K1 H3E 85.8(5) . . ?
O2 K1 H4D 108.1(5) . . ?
O1 K1 H4D 76.8(5) . . ?
N1 K1 H4D 163.4(5) . . ?
B1 K1 H4D 141.9(5) . . ?
B2 K1 H4D 82.7(4) 4_566 . ?
B4 K1 H4D 20.6(5) . . ?
B3 K1 H4D 52.2(4) . . ?
K2 K1 H4D 93.1(4) . . ?
K2 K1 H4D 39.5(4) 4_566 . ?
H1D K1 H4D 135.6(6) . . ?
H1E K1 H4D 123.3(6) . . ?
H3E K1 H4D 66.8(6) . . ?
O2 K1 H4E 70.3(5) . . ?
O1 K1 H4E 113.6(5) . . ?
N1 K1 H4E 157.7(5) . . ?
B1 K1 H4E 146.7(5) . . ?
B2 K1 H4E 72.9(5) 4_566 . ?
B4 K1 H4E 18.8(5) . . ?
B3 K1 H4E 56.5(5) . . ?
K2 K1 H4E 102.4(5) . . ?
K2 K1 H4E 44.4(5) 4_566 . ?
H1D K1 H4E 125.7(6) . . ?
H1E K1 H4E 144.5(6) . . ?
H3E K1 H4E 59.6(6) . . ?
H4D K1 H4E 38.4(7) . . ?
O3 K2 N3 98.79(5) . . ?
O3 K2 B4 96.15(6) . 4_565 ?
N3 K2 B4 98.43(6) . 4_565 ?
O3 K2 B3 95.22(6) . . ?
N3 K2 B3 28.47(5) . . ?
B4 K2 B3 126.87(7) 4_565 . ?
O3 K2 B2 99.75(6) . . ?
N3 K2 B2 161.05(6) . . ?
B4 K2 B2 83.49(7) 4_565 . ?
B3 K2 B2 144.40(6) . . ?
O3 K2 B1 102.94(5) . . ?
N3 K2 B1 123.28(5) . . ?
B4 K2 B1 129.76(6) 4_565 . ?
B3 K2 B1 97.34(6) . . ?
B2 K2 B1 47.88(5) . . ?
O3 K2 K1 97.14(4) . . ?
N3 K2 K1 79.20(4) . . ?
B4 K2 K1 166.71(5) 4_565 . ?
B3 K2 K1 51.36(4) . . ?
B2 K2 K1 94.59(4) . . ?
B1 K2 K1 46.71(4) . . ?
O3 K2 K1 116.70(3) . 4_565 ?
N3 K2 K1 128.46(4) . 4_565 ?
B4 K2 K1 44.84(5) 4_565 4_565 ?
B3 K2 K1 146.63(5) . 4_565 ?
B2 K2 K1 43.51(4) . 4_565 ?
B1 K2 K1 85.36(4) . 4_565 ?
K1 K2 K1 127.398(13) . 4_565 ?
O3 K2 H1D 122.2(4) . . ?
N3 K2 H1D 110.8(4) . . ?
B4 K2 H1D 125.2(4) 4_565 . ?
B3 K2 H1D 89.8(4) . . ?
B2 K2 H1D 54.9(4) . . ?
B1 K2 H1D 20.0(4) . . ?
K1 K2 H1D 45.9(4) . . ?
K1 K2 H1D 81.5(4) 4_565 . ?
O3 K2 H1E 84.7(4) . . ?
N3 K2 H1E 123.5(4) . . ?
B4 K2 H1E 137.5(4) 4_565 . ?
B3 K2 H1E 95.1(4) . . ?
B2 K2 H1E 54.8(4) . . ?
B1 K2 H1E 18.7(4) . . ?
K1 K2 H1E 44.7(4) . . ?
K1 K2 H1E 97.2(4) 4_565 . ?
H1D K2 H1E 37.6(5) . . ?
O3 K2 H2D 119.3(4) . . ?
N3 K2 H2D 141.7(5) . . ?
B4 K2 H2D 75.4(4) 4_565 . ?
B3 K2 H2D 138.1(4) . . ?
B2 K2 H2D 20.9(4) . . ?
B1 K2 H2D 54.7(4) . . ?
K1 K2 H2D 98.3(4) . . ?
K1 K2 H2D 30.7(4) 4_565 . ?
H1D K2 H2D 52.8(6) . . ?
H1E K2 H2D 67.7(6) . . ?
O3 K2 H2E 78.9(4) . . ?
N3 K2 H2E 177.1(4) . . ?
B4 K2 H2E 83.6(4) 4_565 . ?
B3 K2 H2E 149.6(4) . . ?
B2 K2 H2E 21.0(4) . . ?
B1 K2 H2E 56.1(4) . . ?
K1 K2 H2E 99.3(4) . . ?
K1 K2 H2E 54.4(4) 4_565 . ?
H1D K2 H2E 69.3(6) . . ?
H1E K2 H2E 54.8(6) . . ?
H2D K2 H2E 40.8(6) . . ?
O3 K2 H3D 75.5(4) . . ?
N3 K2 H3D 42.8(4) . . ?
B4 K2 H3D 135.8(4) 4_565 . ?
B3 K2 H3D 21.1(4) . . ?
B2 K2 H3D 140.5(4) . . ?
B1 K2 H3D 94.2(4) . . ?
K1 K2 H3D 48.6(4) . . ?
K1 K2 H3D 167.6(4) 4_565 . ?
H1D K2 H3D 93.8(5) . . ?
H1E K2 H3D 85.7(5) . . ?
H2D K2 H3D 146.6(6) . . ?
H2E K2 H3D 134.5(6) . . ?
O3 K2 H3E 111.2(4) . . ?
N3 K2 H3E 43.7(4) . . ?
B4 K2 H3E 134.6(4) 4_565 . ?
B3 K2 H3E 21.6(4) . . ?
B2 K2 H3E 124.0(4) . . ?
B1 K2 H3E 79.6(4) . . ?
K1 K2 H3E 38.0(4) . . ?
K1 K2 H3E 131.9(4) 4_565 . ?
H1D K2 H3E 69.1(5) . . ?
H1E K2 H3E 82.3(5) . . ?
H2D K2 H3E 116.6(6) . . ?
H2E K2 H3E 135.6(6) . . ?
H3D K2 H3E 36.4(5) . . ?
N1 B1 N2 116.87(16) . . ?
N1 B1 K1 65.36(9) . . ?
N2 B1 K1 176.33(13) . . ?
N1 B1 K2 147.39(12) . . ?
N2 B1 K2 95.66(10) . . ?
K1 B1 K2 82.04(5) . . ?
N1 B1 H1D 109.2(10) . . ?
N2 B1 H1D 105.6(9) . . ?
K1 B1 H1D 75.8(9) . . ?
K2 B1 H1D 60.3(9) . . ?
N1 B1 H1E 110.9(10) . . ?
N2 B1 H1E 103.3(10) . . ?
K1 B1 H1E 73.0(10) . . ?
K2 B1 H1E 55.2(10) . . ?
H1D B1 H1E 110.7(14) . . ?
N2 B2 K2 104.61(11) . . ?
N2 B2 K1 140.75(14) . 4_565 ?
K2 B2 K1 93.23(6) . 4_565 ?
N2 B2 H2D 108.3(11) . . ?
K2 B2 H2D 58.8(10) . . ?
K1 B2 H2D 52.7(10) 4_565 . ?
N2 B2 H2E 108.3(10) . . ?
K2 B2 H2E 58.2(10) . . ?
K1 B2 H2E 110.9(10) 4_565 . ?
H2D B2 H2E 112.5(14) . . ?
N2 B2 H2F 107.8(11) . . ?
K2 B2 H2F 147.6(11) . . ?
K1 B2 H2F 61.5(11) 4_565 . ?
H2D B2 H2F 110.3(15) . . ?
H2E B2 H2F 109.5(15) . . ?
N3 B3 N4 116.85(17) . . ?
N3 B3 K2 64.96(10) . . ?
N4 B3 K2 178.17(14) . . ?
N3 B3 K1 144.18(13) . . ?
N4 B3 K1 96.33(12) . . ?
K2 B3 K1 81.85(5) . . ?
N3 B3 H3D 108.1(11) . . ?
N4 B3 H3D 106.3(10) . . ?
K2 B3 H3D 73.0(10) . . ?
K1 B3 H3D 72.1(11) . . ?
N3 B3 H3E 109.1(10) . . ?
N4 B3 H3E 106.9(10) . . ?
K2 B3 H3E 71.9(10) . . ?
K1 B3 H3E 43.9(10) . . ?
H3D B3 H3E 109.4(14) . . ?
N4 B4 K2 163.62(15) . 4_566 ?
N4 B4 K1 101.98(12) . . ?
K2 B4 K1 92.47(7) 4_566 . ?
N4 B4 H4D 106.3(12) . . ?
K2 B4 H4D 72.1(12) 4_566 . ?
K1 B4 H4D 67.4(12) . . ?
N4 B4 H4E 107.4(11) . . ?
K2 B4 H4E 87.9(11) 4_566 . ?
K1 B4 H4E 48.4(11) . . ?
H4D B4 H4E 111.6(16) . . ?
N4 B4 H4F 105.8(12) . . ?
K2 B4 H4F 61.5(12) 4_566 . ?
K1 B4 H4F 151.1(12) . . ?
H4D B4 H4F 111.4(16) . . ?
H4E B4 H4F 113.9(16) . . ?
C2 N1 C1 111.31(18) . . ?
C2 N1 B1 123.38(17) . . ?
C1 N1 B1 123.08(17) . . ?
C2 N1 K1 98.51(12) . . ?
C1 N1 K1 100.87(12) . . ?
B1 N1 K1 86.39(10) . . ?
C4 N2 C3 108.32(18) . . ?
C4 N2 B2 108.72(17) . . ?
C3 N2 B2 108.49(16) . . ?
C4 N2 B1 110.22(15) . . ?
C3 N2 B1 109.29(15) . . ?
B2 N2 B1 111.73(14) . . ?
C6 N3 C5 111.7(2) . . ?
C6 N3 B3 123.23(19) . . ?
C5 N3 B3 122.23(19) . . ?
C6 N3 K2 102.90(13) . . ?
C5 N3 K2 98.02(13) . . ?
B3 N3 K2 86.58(11) . . ?
C7 N4 C8 108.34(19) . . ?
C7 N4 B4 108.58(18) . . ?
C8 N4 B4 108.40(18) . . ?
C7 N4 B3 109.76(18) . . ?
C8 N4 B3 109.51(16) . . ?
B4 N4 B3 112.16(15) . . ?
C11 O1 C14 106.71(17) . . ?
C11 O1 K1 124.50(13) . . ?
C14 O1 K1 119.30(12) . . ?
C18 O2 C15 105.16(16) . . ?
C18 O2 K1 127.14(12) . . ?
C15 O2 K1 123.45(12) . . ?
C19 O3 C22 105.64(17) . . ?
C19 O3 K2 118.06(13) . . ?
C22 O3 K2 116.94(15) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C5 H5A 109.5 . . ?
N3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N4 C8 H8A 109.5 . . ?
N4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O1 C11 C12 107.08(19) . . ?
O1 C11 H11A 110.3 . . ?
C12 C11 H11A 110.3 . . ?
O1 C11 H11B 110.3 . . ?
C12 C11 H11B 110.3 . . ?
H11A C11 H11B 108.6 . . ?
C11 C12 C13 105.07(18) . . ?
C11 C12 H12A 110.7 . . ?
C13 C12 H12A 110.7 . . ?
C11 C12 H12B 110.7 . . ?
C13 C12 H12B 110.7 . . ?
H12A C12 H12B 108.8 . . ?
C14 C13 C12 103.6(2) . . ?
C14 C13 H13A 111.0 . . ?
C12 C13 H13A 111.0 . . ?
C14 C13 H13B 111.0 . . ?
C12 C13 H13B 111.0 . . ?
H13A C13 H13B 109.0 . . ?
O1 C14 C13 105.67(18) . . ?
O1 C14 H14A 110.6 . . ?
C13 C14 H14A 110.6 . . ?
O1 C14 H14B 110.6 . . ?
C13 C14 H14B 110.6 . . ?
H14A C14 H14B 108.7 . . ?
O2 C15 C16 106.38(18) . . ?
O2 C15 H15A 110.5 . . ?
C16 C15 H15A 110.5 . . ?
O2 C15 H15B 110.5 . . ?
C16 C15 H15B 110.5 . . ?
H15A C15 H15B 108.6 . . ?
C15 C16 C17 104.11(18) . . ?
C15 C16 H16A 110.9 . . ?
C17 C16 H16A 110.9 . . ?
C15 C16 H16B 110.9 . . ?
C17 C16 H16B 110.9 . . ?
H16A C16 H16B 109.0 . . ?
C18 C17 C16 103.86(18) . . ?
C18 C17 H17A 111.0 . . ?
C16 C17 H17A 111.0 . . ?
C18 C17 H17B 111.0 . . ?
C16 C17 H17B 111.0 . . ?
H17A C17 H17B 109.0 . . ?
O2 C18 C17 105.75(18) . . ?
O2 C18 H18A 110.6 . . ?
C17 C18 H18A 110.6 . . ?
O2 C18 H18B 110.6 . . ?
C17 C18 H18B 110.6 . . ?
H18A C18 H18B 108.7 . . ?
O3 C19 C20 104.70(19) . . ?
O3 C19 H19A 110.8 . . ?
C20 C19 H19A 110.8 . . ?
O3 C19 H19B 110.8 . . ?
C20 C19 H19B 110.8 . . ?
H19A C19 H19B 108.9 . . ?
C19 C20 C21 103.4(2) . . ?
C19 C20 H20A 111.1 . . ?
C21 C20 H20A 111.1 . . ?
C19 C20 H20B 111.1 . . ?
C21 C20 H20B 111.1 . . ?
H20A C20 H20B 109.0 . . ?
C22 C21 C20 104.4(2) . . ?
C22 C21 H21A 110.9 . . ?
C20 C21 H21A 110.9 . . ?
C22 C21 H21B 110.9 . . ?
C20 C21 H21B 110.9 . . ?
H21A C21 H21B 108.9 . . ?
O3 C22 C21 107.37(19) . . ?
O3 C22 H22A 110.2 . . ?
C21 C22 H22A 110.2 . . ?
O3 C22 H22B 110.2 . . ?
C21 C22 H22B 110.2 . . ?
H22A C22 H22B 108.5 . . ?

_refine_diff_density_max         0.215
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.043

_shelxl_version_number           2013-4


_chemical_properties_physical    'Air-sensitive, Oxygen-sensitive'
