# 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_1a
_database_code_depnum_ccdc_archive 'CCDC 1046050'
_audit_update_record             
;
2015-03-02 deposited with the CCDC.
2015-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H26 N4 O'
_chemical_formula_sum            'C18 H26 N4 O'
_chemical_formula_weight         314.43

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   9.0491(4)
_cell_length_b                   12.7601(5)
_cell_length_c                   16.7496(9)
_cell_angle_alpha                90
_cell_angle_beta                 109.944(4)
_cell_angle_gamma                90
_cell_volume                     1818.04(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      4.46
_cell_measurement_theta_max      70.69

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             680
_exptl_absorpt_coefficient_mu    0.579
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.886
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27'

_exptl_special_details           
;
 'Empirical absorption correction using spherical harmonics,implemented in SCALE3 ABSPACK scaling algorithm.'
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6979
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.46
_diffrn_reflns_theta_max         70.69
_reflns_number_total             3395
_reflns_number_gt                2454
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP III & Olex 2.1'
_computing_publication_material  WinGX

_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 > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0495P)²+0.7050P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0025(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3395
_refine_ls_number_parameters     215
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0592
_refine_ls_wR_factor_ref         0.1735
_refine_ls_wR_factor_gt          0.1609
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_restrained_S_all      1.150
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O -0.1585(2) 0.05999(15) -0.31444(12) 0.0778(6) Uani 1 1 d . . .
N3 N -0.3237(2) -0.17313(16) -0.29433(12) 0.0583(5) Uani 1 1 d . . .
N2 N -0.1647(2) -0.21100(16) -0.36353(12) 0.0566(5) Uani 1 1 d . . .
N1 N -0.3232(2) -0.05663(15) -0.40850(12) 0.0579(5) Uani 1 1 d . . .
N4 N -0.3415(3) 0.11546(16) -0.43954(13) 0.0674(6) Uani 1 1 d . . .
H4 H -0.4197 0.0944 -0.4823 0.081 Uiso 1 1 calc R . .
C9 C -0.3280(5) -0.0527(4) -0.1828(3) 0.1311(17) Uani 1 1 d . . .
H9A H -0.2519 -0.0969 -0.1430 0.197 Uiso 1 1 calc R . .
H9B H -0.3924 -0.0194 -0.1550 0.197 Uiso 1 1 calc R . .
H9C H -0.2747 -0.0002 -0.2038 0.197 Uiso 1 1 calc R . .
C1 C -0.2695(3) -0.13853(19) -0.35587(14) 0.0519(6) Uani 1 1 d . . .
C3 C -0.2497(3) -0.2671(2) -0.26343(17) 0.0705(8) Uani 1 1 d . . .
H3 H -0.2647 -0.3071 -0.2204 0.085 Uiso 1 1 calc R . .
C8 C -0.4305(4) -0.1185(3) -0.25623(18) 0.0761(8) Uani 1 1 d . . .
C10 C -0.5187(5) -0.2017(3) -0.2256(3) 0.1182(14) Uani 1 1 d . . .
H10A H -0.5816 -0.2428 -0.2730 0.177 Uiso 1 1 calc R . .
H10B H -0.5855 -0.1685 -0.1992 0.177 Uiso 1 1 calc R . .
H10C H -0.4448 -0.2463 -0.1851 0.177 Uiso 1 1 calc R . .
C7 C 0.0362(4) -0.3007(3) -0.4073(3) 0.1112(13) Uani 1 1 d . . .
H7A H 0.1032 -0.3017 -0.3488 0.167 Uiso 1 1 calc R . .
H7B H 0.0993 -0.2963 -0.4430 0.167 Uiso 1 1 calc R . .
H7C H -0.0254 -0.3637 -0.4201 0.167 Uiso 1 1 calc R . .
C2 C -0.1539(3) -0.2904(2) -0.30548(17) 0.0684(7) Uani 1 1 d . . .
H2 H -0.0905 -0.3496 -0.2974 0.082 Uiso 1 1 calc R . .
C11 C -0.5511(4) -0.0493(3) -0.3204(2) 0.1091(13) Uani 1 1 d . . .
H11A H -0.4984 0.0082 -0.3362 0.164 Uiso 1 1 calc R . .
H11B H -0.6246 -0.0228 -0.2955 0.164 Uiso 1 1 calc R . .
H11C H -0.6062 -0.0898 -0.3700 0.164 Uiso 1 1 calc R . .
C4 C -0.0731(3) -0.2057(2) -0.42310(19) 0.0723(8) Uani 1 1 d . . .
C12 C -0.2658(3) 0.0386(2) -0.38121(16) 0.0600(6) Uani 1 1 d . . .
C5 C 0.0265(5) -0.1075(3) -0.4037(3) 0.1128(13) Uani 1 1 d . . .
H5A H -0.0404 -0.0470 -0.4186 0.169 Uiso 1 1 calc R . .
H5B H 0.0961 -0.1078 -0.4360 0.169 Uiso 1 1 calc R . .
H5C H 0.0870 -0.1053 -0.3442 0.169 Uiso 1 1 calc R . .
C6 C -0.1875(5) -0.2079(4) -0.5131(2) 0.1253(17) Uani 1 1 d . . .
H6A H -0.2566 -0.2669 -0.5201 0.188 Uiso 1 1 calc R . .
H6B H -0.1305 -0.2138 -0.5518 0.188 Uiso 1 1 calc R . .
H6C H -0.2480 -0.1444 -0.5245 0.188 Uiso 1 1 calc R . .
C13 C -0.3078(3) 0.22241(19) -0.43818(15) 0.0554(6) Uani 1 1 d . . .
C14 C -0.4088(3) 0.2842(2) -0.50091(17) 0.0656(7) Uani 1 1 d . . .
H14 H -0.4948 0.2536 -0.5419 0.079 Uiso 1 1 calc R . .
C18 C -0.1792(3) 0.2698(2) -0.37859(18) 0.0703(7) Uani 1 1 d . . .
H18 H -0.1084 0.2297 -0.3362 0.084 Uiso 1 1 calc R . .
C15 C -0.3843(4) 0.3903(2) -0.5039(2) 0.0833(9) Uani 1 1 d . . .
H15 H -0.4538 0.4306 -0.5466 0.100 Uiso 1 1 calc R . .
C17 C -0.1565(4) 0.3766(2) -0.3822(2) 0.0859(9) Uani 1 1 d . . .
H17 H -0.0705 0.4079 -0.3417 0.103 Uiso 1 1 calc R . .
C16 C -0.2583(4) 0.4369(2) -0.4443(2) 0.0937(11) Uani 1 1 d . . .
H16 H -0.2421 0.5087 -0.4461 0.112 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
O1 C12 1.236(3) . ?
N3 C1 1.358(3) . ?
N3 C3 1.385(3) . ?
N3 C8 1.499(3) . ?
N2 C1 1.362(3) . ?
N2 C2 1.384(3) . ?
N2 C4 1.500(3) . ?
N1 C12 1.339(3) . ?
N1 C1 1.346(3) . ?
N4 C12 1.389(3) . ?
N4 C13 1.397(3) . ?
N4 H4 0.8600 . ?
C9 C8 1.517(5) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C3 C2 1.324(4) . ?
C3 H3 0.9300 . ?
C8 C10 1.519(5) . ?
C8 C11 1.525(4) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C7 C4 1.529(4) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C2 H2 0.9300 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C4 C6 1.510(4) . ?
C4 C5 1.513(4) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C13 C14 1.381(3) . ?
C13 C18 1.387(3) . ?
C14 C15 1.375(4) . ?
C14 H14 0.9300 . ?
C18 C17 1.383(4) . ?
C18 H18 0.9300 . ?
C15 C16 1.368(4) . ?
C15 H15 0.9300 . ?
C17 C16 1.367(4) . ?
C17 H17 0.9300 . ?
C16 H16 0.9300 . ?

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 N3 C3 108.1(2) . . ?
C1 N3 C8 128.6(2) . . ?
C3 N3 C8 122.9(2) . . ?
C1 N2 C2 108.4(2) . . ?
C1 N2 C4 126.3(2) . . ?
C2 N2 C4 125.3(2) . . ?
C12 N1 C1 118.0(2) . . ?
C12 N4 C13 128.8(2) . . ?
C12 N4 H4 115.6 . . ?
C13 N4 H4 115.6 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C1 N3 127.3(2) . . ?
N1 C1 N2 124.9(2) . . ?
N3 C1 N2 107.1(2) . . ?
C2 C3 N3 108.4(2) . . ?
C2 C3 H3 125.8 . . ?
N3 C3 H3 125.8 . . ?
N3 C8 C10 108.0(3) . . ?
N3 C8 C9 107.3(3) . . ?
C10 C8 C9 111.0(3) . . ?
N3 C8 C11 112.3(2) . . ?
C10 C8 C11 108.1(3) . . ?
C9 C8 C11 110.1(3) . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C3 C2 N2 107.9(2) . . ?
C3 C2 H2 126.0 . . ?
N2 C2 H2 126.0 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C4 C6 108.5(2) . . ?
N2 C4 C5 108.6(2) . . ?
C6 C4 C5 112.6(3) . . ?
N2 C4 C7 108.7(3) . . ?
C6 C4 C7 109.9(3) . . ?
C5 C4 C7 108.5(3) . . ?
O1 C12 N1 127.1(2) . . ?
O1 C12 N4 121.8(2) . . ?
N1 C12 N4 111.1(2) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C14 C13 C18 118.3(2) . . ?
C14 C13 N4 117.5(2) . . ?
C18 C13 N4 124.2(2) . . ?
C15 C14 C13 121.1(3) . . ?
C15 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C17 C18 C13 119.9(3) . . ?
C17 C18 H18 120.0 . . ?
C13 C18 H18 120.0 . . ?
C16 C15 C14 120.4(3) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C16 C17 C18 121.1(3) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C15 C16 C17 119.2(3) . . ?
C15 C16 H16 120.4 . . ?
C17 C16 H16 120.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 N1 C1 N3 85.9(3) . . . . ?
C12 N1 C1 N2 -104.3(3) . . . . ?
C3 N3 C1 N1 172.0(2) . . . . ?
C8 N3 C1 N1 -14.4(4) . . . . ?
C3 N3 C1 N2 0.7(3) . . . . ?
C8 N3 C1 N2 174.3(2) . . . . ?
C2 N2 C1 N1 -172.1(2) . . . . ?
C4 N2 C1 N1 9.1(4) . . . . ?
C2 N2 C1 N3 -0.5(3) . . . . ?
C4 N2 C1 N3 -179.3(2) . . . . ?
C1 N3 C3 C2 -0.7(3) . . . . ?
C8 N3 C3 C2 -174.7(2) . . . . ?
C1 N3 C8 C10 152.5(3) . . . . ?
C3 N3 C8 C10 -34.8(4) . . . . ?
C1 N3 C8 C9 -87.7(3) . . . . ?
C3 N3 C8 C9 85.0(4) . . . . ?
C1 N3 C8 C11 33.4(4) . . . . ?
C3 N3 C8 C11 -153.9(3) . . . . ?
N3 C3 C2 N2 0.4(3) . . . . ?
C1 N2 C2 C3 0.0(3) . . . . ?
C4 N2 C2 C3 178.9(2) . . . . ?
C1 N2 C4 C6 -63.3(4) . . . . ?
C2 N2 C4 C6 118.1(3) . . . . ?
C1 N2 C4 C5 59.4(3) . . . . ?
C2 N2 C4 C5 -119.2(3) . . . . ?
C1 N2 C4 C7 177.2(3) . . . . ?
C2 N2 C4 C7 -1.4(4) . . . . ?
C1 N1 C12 O1 5.9(4) . . . . ?
C1 N1 C12 N4 -175.2(2) . . . . ?
C13 N4 C12 O1 4.8(4) . . . . ?
C13 N4 C12 N1 -174.2(3) . . . . ?
C12 N4 C13 C14 -175.2(3) . . . . ?
C12 N4 C13 C18 5.4(4) . . . . ?
C18 C13 C14 C15 -0.9(4) . . . . ?
N4 C13 C14 C15 179.7(3) . . . . ?
C14 C13 C18 C17 1.1(4) . . . . ?
N4 C13 C18 C17 -179.5(3) . . . . ?
C13 C14 C15 C16 0.1(5) . . . . ?
C13 C18 C17 C16 -0.6(5) . . . . ?
C14 C15 C16 C17 0.4(6) . . . . ?
C18 C17 C16 C15 -0.2(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        70.69
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         0.133
_refine_diff_density_min         -0.157
_refine_diff_density_rms         0.033
####################################################################### 
# 
# 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_1d
_database_code_depnum_ccdc_archive 'CCDC 1046051'
_audit_update_record             
;
2015-03-02 deposited with the CCDC.
2015-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            1d
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H26 N4 S, C4 H8 O'
_chemical_formula_sum            'C22 H34 N4 O S'
_chemical_formula_weight         402.59

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234 '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'
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'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

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

_cell_length_a                   30.9905(15)
_cell_length_b                   30.9905(15)
_cell_length_c                   12.3331(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     10257.9(11)
_cell_formula_units_Z            18
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2445
_cell_measurement_theta_min      3.9414
_cell_measurement_theta_max      70.6654

_exptl_crystal_description       chunk
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_F_000             3924
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    0.161
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.89998
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27'

_exptl_special_details           
;
 'Empirical absorption correction using spherical harmonics,implemented in SCALE3 ABSPACK scaling algorithm.'
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8326
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.817
_diffrn_reflns_theta_max         25.806
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             4261
_reflns_number_gt                3388
_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.O1 atom of the tetrahydrofuran molecule is splitted to O1A and O1B with occupancy 0.68(3) and 0.32(3) respectively.DFIX is used to fix the C-C bond length in tetrahydrofuran.
 
 _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       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP III & Olex 2.1'
_computing_publication_material  WinGX

_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)+(0.1148P)²+1.6028P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4261
_refine_ls_number_parameters     259
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0596
_refine_ls_wR_factor_ref         0.1833
_refine_ls_wR_factor_gt          0.1686
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.102
_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
S1 S 0.42976(2) 0.93842(2) 0.54794(4) 0.0304(2) Uani 1 1 d . . . . .
N1 N 0.40163(7) 0.97101(7) 0.72377(15) 0.0291(4) Uani 1 1 d . . . . .
N2 N 0.31495(7) 0.91256(7) 0.67296(14) 0.0280(4) Uani 1 1 d . . . . .
N3 N 0.34898(7) 0.89153(8) 0.80354(15) 0.0310(4) Uani 1 1 d . . . . .
N4 N 0.47944(7) 1.02331(7) 0.65281(15) 0.0315(4) Uani 1 1 d . . . . .
H4 H 0.4998 1.0271 0.6016 0.038 Uiso 1 1 calc R U . . .
C1 C 0.35840(8) 0.92696(9) 0.72766(17) 0.0279(5) Uani 1 1 d . . . . .
C2 C 0.27894(9) 0.86740(9) 0.7151(2) 0.0350(5) Uani 1 1 d . . . . .
H2 H 0.2461 0.8491 0.6916 0.042 Uiso 1 1 calc R U . . .
C3 C 0.29923(10) 0.85450(10) 0.7954(2) 0.0367(6) Uani 1 1 d . . . . .
H3 H 0.2830 0.8260 0.8379 0.044 Uiso 1 1 calc R U . . .
C4 C 0.30352(9) 0.93605(9) 0.57897(17) 0.0293(5) Uani 1 1 d . . . . .
C5 C 0.34258(10) 0.99081(9) 0.56538(19) 0.0345(5) Uani 1 1 d . . . . .
H5A H 0.3480 1.0076 0.6337 0.052 Uiso 1 1 calc R U . . .
H5B H 0.3312 1.0058 0.5131 0.052 Uiso 1 1 calc R U . . .
H5C H 0.3732 0.9935 0.5408 0.052 Uiso 1 1 calc R U . . .
C6 C 0.30009(9) 0.90647(9) 0.47694(18) 0.0346(5) Uani 1 1 d . . . . .
H6A H 0.3313 0.9076 0.4655 0.052 Uiso 1 1 calc R U . . .
H6B H 0.2928 0.9208 0.4156 0.052 Uiso 1 1 calc R U . . .
H6C H 0.2741 0.8725 0.4857 0.052 Uiso 1 1 calc R U . . .
C7 C 0.25274(9) 0.93181(10) 0.6014(2) 0.0372(6) Uani 1 1 d . . . . .
H7A H 0.2269 0.8976 0.5952 0.056 Uiso 1 1 calc R U . . .
H7B H 0.2470 0.9515 0.5496 0.056 Uiso 1 1 calc R U . . .
H7C H 0.2526 0.9436 0.6732 0.056 Uiso 1 1 calc R U . . .
C8 C 0.38435(9) 0.89310(10) 0.88985(19) 0.0359(6) Uani 1 1 d . . . . .
C9 C 0.36021(12) 0.84235(12) 0.9454(2) 0.0493(7) Uani 1 1 d . . . . .
H9A H 0.3297 0.8359 0.9793 0.074 Uiso 1 1 calc R U . . .
H9B H 0.3825 0.8422 0.9994 0.074 Uiso 1 1 calc R U . . .
H9C H 0.3533 0.8170 0.8925 0.074 Uiso 1 1 calc R U . . .
C10 C 0.39269(12) 0.93328(12) 0.9713(2) 0.0470(7) Uani 1 1 d . . . . .
H10A H 0.4082 0.9651 0.9357 0.071 Uiso 1 1 calc R U . . .
H10B H 0.4139 0.9337 1.0286 0.071 Uiso 1 1 calc R U . . .
H10C H 0.3613 0.9264 1.0010 0.071 Uiso 1 1 calc R U . . .
C11 C 0.43356(11) 0.90332(14) 0.8385(2) 0.0519(8) Uani 1 1 d . . . . .
H11A H 0.4268 0.8820 0.7768 0.078 Uiso 1 1 calc R U . . .
H11B H 0.4526 0.8968 0.8907 0.078 Uiso 1 1 calc R U . . .
H11C H 0.4521 0.9375 0.8160 0.078 Uiso 1 1 calc R U . . .
C12 C 0.43513(9) 0.97907(9) 0.64951(17) 0.0290(5) Uani 1 1 d . . . . .
C13 C 0.49721(9) 1.06356(9) 0.72553(18) 0.0311(5) Uani 1 1 d . . . . .
C14 C 0.46864(10) 1.06951(10) 0.80548(19) 0.0365(5) Uani 1 1 d . . . . .
H14 H 0.4353 1.0454 0.8148 0.044 Uiso 1 1 calc R U . . .
C15 C 0.49035(11) 1.11183(10) 0.8712(2) 0.0394(6) Uani 1 1 d . . . . .
H15 H 0.4712 1.1156 0.9244 0.047 Uiso 1 1 calc R U . . .
C16 C 0.53947(10) 1.14815(10) 0.8592(2) 0.0396(6) Uani 1 1 d . . . . .
H16 H 0.5533 1.1763 0.9031 0.047 Uiso 1 1 calc R U . . .
C17 C 0.56834(10) 1.14217(10) 0.7801(2) 0.0408(6) Uani 1 1 d . . . . .
H17 H 0.6017 1.1663 0.7714 0.049 Uiso 1 1 calc R U . . .
C18 C 0.54732(9) 1.10034(9) 0.7149(2) 0.0352(5) Uani 1 1 d . . . . .
H18 H 0.5669 1.0965 0.6629 0.042 Uiso 1 1 calc R U . . .
C21 C 0.5345(3) 1.2260(6) 1.2517(7) 0.278(8) Uani 1 1 d D . . . .
H00A H 0.5493 1.2147 1.3058 0.334 Uiso 1 1 calc R U . . .
H00B H 0.5026 1.2208 1.2771 0.334 Uiso 1 1 calc R U . . .
C22 C 0.5728(5) 1.2848(4) 1.2122(8) 0.214(5) Uani 1 1 d . . . . .
H00C H 0.5886 1.3065 1.2738 0.257 Uiso 1 1 calc R U . A 1
H00D H 0.5553 1.2976 1.1698 0.257 Uiso 1 1 calc R U . A 1
O1A O 0.616(2) 1.2784(14) 1.134(3) 0.58(3) Uiso 0.62(3) 1 d . . P B 1
O1B O 0.5779(6) 1.2751(6) 1.1112(12) 0.134(9) Uiso 0.38(3) 1 d . . P B 2
C20 C 0.5311(3) 1.2032(3) 1.1415(7) 0.144(3) Uani 1 1 d D . . . .
H00E H 0.5284 1.1709 1.1505 0.173 Uiso 1 1 calc R U . . .
H00F H 0.5012 1.1982 1.1050 0.173 Uiso 1 1 calc R U . . .
C19 C 0.5714(3) 1.2325(4) 1.0788(8) 0.176(4) Uani 1 1 d D . . . .
H00G H 0.5603 1.2444 1.0181 0.211 Uiso 1 1 calc R U . B 1
H00H H 0.5839 1.2118 1.0493 0.211 Uiso 1 1 calc R U . B 1


_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
S1 C12 1.724(2) . ?
N1 C12 1.311(3) . ?
N1 C1 1.353(3) . ?
N2 C1 1.366(3) . ?
N2 C2 1.383(3) . ?
N2 C4 1.502(3) . ?
N3 C1 1.359(3) . ?
N3 C3 1.391(3) . ?
N3 C8 1.511(3) . ?
N4 C12 1.373(3) . ?
N4 C13 1.406(3) . ?
N4 H4 0.8600 . ?
C2 C3 1.336(4) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C5 1.523(3) . ?
C4 C6 1.529(3) . ?
C4 C7 1.537(3) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C10 1.518(4) . ?
C8 C9 1.525(4) . ?
C8 C11 1.531(4) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C13 C14 1.398(3) . ?
C13 C18 1.399(3) . ?
C14 C15 1.396(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.376(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.397(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.381(4) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C21 C20 1.511(11) . ?
C21 C22 1.673(15) . ?
C21 H00A 0.9700 . ?
C21 H00B 0.9700 . ?
C22 O1B 1.309(15) . ?
C22 O1A 1.73(5) . ?
C22 H00C 0.9700 . ?
C22 H00D 0.9700 . ?
O1A C19 1.55(5) . ?
O1B C19 1.296(15) . ?
C20 C19 1.360(8) . ?
C20 H00E 0.9700 . ?
C20 H00F 0.9700 . ?
C19 H00G 0.9700 . ?
C19 H00H 0.9700 . ?

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
C12 N1 C1 120.5(2) . . ?
C1 N2 C2 108.04(19) . . ?
C1 N2 C4 130.95(19) . . ?
C2 N2 C4 120.93(19) . . ?
C1 N3 C3 108.57(19) . . ?
C1 N3 C8 126.9(2) . . ?
C3 N3 C8 124.4(2) . . ?
C12 N4 C13 131.1(2) . . ?
C12 N4 H4 114.4 . . ?
C13 N4 H4 114.4 . . ?
N1 C1 N3 123.0(2) . . ?
N1 C1 N2 129.0(2) . . ?
N3 C1 N2 107.3(2) . . ?
C3 C2 N2 108.6(2) . . ?
C3 C2 H2 125.7 . . ?
N2 C2 H2 125.7 . . ?
C2 C3 N3 107.5(2) . . ?
C2 C3 H3 126.3 . . ?
N3 C3 H3 126.3 . . ?
N2 C4 C5 112.10(18) . . ?
N2 C4 C6 107.88(19) . . ?
C5 C4 C6 110.84(19) . . ?
N2 C4 C7 107.41(18) . . ?
C5 C4 C7 108.9(2) . . ?
C6 C4 C7 109.59(19) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 C10 108.4(2) . . ?
N3 C8 C9 108.0(2) . . ?
C10 C8 C9 110.1(2) . . ?
N3 C8 C11 110.30(19) . . ?
C10 C8 C11 111.1(2) . . ?
C9 C8 C11 108.9(2) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N1 C12 N4 118.1(2) . . ?
N1 C12 S1 126.16(18) . . ?
N4 C12 S1 115.73(17) . . ?
C14 C13 C18 118.5(2) . . ?
C14 C13 N4 125.0(2) . . ?
C18 C13 N4 116.5(2) . . ?
C15 C14 C13 119.6(2) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C16 C15 C14 121.5(2) . . ?
C16 C15 H15 119.3 . . ?
C14 C15 H15 119.3 . . ?
C15 C16 C17 119.1(2) . . ?
C15 C16 H16 120.4 . . ?
C17 C16 H16 120.4 . . ?
C18 C17 C16 119.9(2) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
C17 C18 C13 121.4(2) . . ?
C17 C18 H18 119.3 . . ?
C13 C18 H18 119.3 . . ?
C20 C21 C22 95.3(6) . . ?
C20 C21 H00A 112.7 . . ?
C22 C21 H00A 112.7 . . ?
C20 C21 H00B 112.7 . . ?
C22 C21 H00B 112.7 . . ?
H00A C21 H00B 110.2 . . ?
O1B C22 C21 97.5(10) . . ?
C21 C22 O1A 101.8(15) . . ?
C21 C22 H00C 111.4 . . ?
O1A C22 H00C 111.4 . . ?
C21 C22 H00D 111.4 . . ?
O1A C22 H00D 111.4 . . ?
H00C C22 H00D 109.3 . . ?
C19 O1A C22 89(3) . . ?
C22 O1B C19 123.4(12) . . ?
C19 C20 C21 111.9(7) . . ?
C19 C20 H00E 109.2 . . ?
C21 C20 H00E 109.2 . . ?
C19 C20 H00F 109.2 . . ?
C21 C20 H00F 109.2 . . ?
H00E C20 H00F 107.9 . . ?
C20 C19 O1B 97.3(9) . . ?
C20 C19 O1A 117.1(17) . . ?
C20 C19 H00G 108.0 . . ?
O1A C19 H00G 108.0 . . ?
C20 C19 H00H 108.0 . . ?
O1A C19 H00H 108.0 . . ?
H00G C19 H00H 107.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 N1 C1 N3 105.1(3) . . . . ?
C12 N1 C1 N2 -86.2(3) . . . . ?
C3 N3 C1 N1 171.2(2) . . . . ?
C8 N3 C1 N1 -3.8(3) . . . . ?
C3 N3 C1 N2 0.5(3) . . . . ?
C8 N3 C1 N2 -174.5(2) . . . . ?
C2 N2 C1 N1 -171.0(2) . . . . ?
C4 N2 C1 N1 12.2(4) . . . . ?
C2 N2 C1 N3 -1.0(2) . . . . ?
C4 N2 C1 N3 -177.7(2) . . . . ?
C1 N2 C2 C3 1.1(3) . . . . ?
C4 N2 C2 C3 178.3(2) . . . . ?
N2 C2 C3 N3 -0.8(3) . . . . ?
C1 N3 C3 C2 0.2(3) . . . . ?
C8 N3 C3 C2 175.4(2) . . . . ?
C1 N2 C4 C5 -19.2(3) . . . . ?
C2 N2 C4 C5 164.4(2) . . . . ?
C1 N2 C4 C6 103.1(3) . . . . ?
C2 N2 C4 C6 -73.3(3) . . . . ?
C1 N2 C4 C7 -138.9(2) . . . . ?
C2 N2 C4 C7 44.7(3) . . . . ?
C1 N3 C8 C10 68.7(3) . . . . ?
C3 N3 C8 C10 -105.6(3) . . . . ?
C1 N3 C8 C9 -172.1(2) . . . . ?
C3 N3 C8 C9 13.7(3) . . . . ?
C1 N3 C8 C11 -53.2(3) . . . . ?
C3 N3 C8 C11 132.5(3) . . . . ?
C1 N1 C12 N4 -176.5(2) . . . . ?
C1 N1 C12 S1 1.9(3) . . . . ?
C13 N4 C12 N1 1.3(4) . . . . ?
C13 N4 C12 S1 -177.2(2) . . . . ?
C12 N4 C13 C14 -9.7(4) . . . . ?
C12 N4 C13 C18 171.0(2) . . . . ?
C18 C13 C14 C15 0.8(4) . . . . ?
N4 C13 C14 C15 -178.5(2) . . . . ?
C13 C14 C15 C16 0.2(4) . . . . ?
C14 C15 C16 C17 -0.8(4) . . . . ?
C15 C16 C17 C18 0.4(4) . . . . ?
C16 C17 C18 C13 0.5(4) . . . . ?
C14 C13 C18 C17 -1.1(4) . . . . ?
N4 C13 C18 C17 178.2(2) . . . . ?
C20 C21 C22 O1B -2.0(12) . . . . ?
C20 C21 C22 O1A -44(2) . . . . ?
O1B C22 O1A C19 -42.3(17) . . . . ?
C21 C22 O1A C19 46(2) . . . . ?
C21 C22 O1B C19 -24.3(18) . . . . ?
O1A C22 O1B C19 75(2) . . . . ?
C22 C21 C20 C19 24.3(11) . . . . ?
C21 C20 C19 O1B -36.5(13) . . . . ?
C21 C20 C19 O1A 8(3) . . . . ?
C22 O1B C19 C20 40.0(17) . . . . ?
C22 O1B C19 O1A -81(2) . . . . ?
C22 O1A C19 C20 -35(3) . . . . ?
C22 O1A C19 O1B 38.6(16) . . . . ?

_refine_diff_density_max         0.477
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.067

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_2b
_database_code_depnum_ccdc_archive 'CCDC 1046052'
_audit_update_record             
;
2015-03-02 deposited with the CCDC.
2015-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C128 H148 K4 N16 O8'
_chemical_formula_weight         2195.02

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_H-M_alt        'P -4 21 c'
_space_group_name_Hall           'P -4 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, -y, z'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'-y, x, -z'
'y, -x, -z'

_cell_length_a                   15.1711(6)
_cell_length_b                   15.1711(6)
_cell_length_c                   25.4506(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5857.8(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3163
_cell_measurement_theta_min      3.3893
_cell_measurement_theta_max      70.5283

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_F_000             2336
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_exptl_absorpt_coefficient_mu    1.858
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.61424
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27'

_exptl_special_details           
;
 'Empirical absorption correction using spherical harmonics,implemented in SCALE3 ABSPACK scaling algorithm.'
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12758
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.391
_diffrn_reflns_theta_max         70.661
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4870
_reflns_number_gt                3793
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.811
_reflns_Friedel_fraction_max     0.991
_reflns_Friedel_fraction_full    1.000

_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       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP III & Olex 2.1'
_computing_publication_material  WinGX

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1066P)²+0.4749P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.03(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4870
_refine_ls_number_parameters     377
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0586
_refine_ls_wR_factor_ref         0.1771
_refine_ls_wR_factor_gt          0.1573
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.06836(7) 0.10236(7) 0.06164(4) 0.0581(3) Uani 1 1 d . . . . .
O1 O 0.1011(2) -0.0676(2) 0.04471(12) 0.0592(8) Uani 1 1 d . . . . .
N1 N 0.1594(3) 0.2069(3) -0.01131(16) 0.0571(9) Uani 1 1 d . . . . .
N4 N 0.2346(3) -0.0853(3) 0.08845(18) 0.0664(11) Uani 1 1 d . . . . .
N2 N 0.2872(3) 0.2325(3) -0.06695(18) 0.0643(10) Uani 1 1 d . . . . .
N3 N 0.2765(3) 0.3039(3) 0.0076(2) 0.0707(12) Uani 1 1 d . . . . .
C1 C 0.2323(3) 0.2444(3) -0.0234(2) 0.0595(12) Uani 1 1 d . . . . .
C27 C 0.1770(3) -0.1027(3) 0.05148(18) 0.0554(11) Uani 1 1 d . . . . .
C26 C 0.2100(5) -0.0328(4) 0.1307(2) 0.0767(17) Uani 1 1 d . . . . .
C4 C 0.2393(4) 0.3461(4) 0.0527(2) 0.0664(13) Uani 1 1 d . . . . .
C6 C 0.1457(5) 0.4559(4) 0.0883(3) 0.0840(18) Uani 1 1 d . . . . .
H6 H 0.1050 0.5012 0.0838 0.101 Uiso 1 1 calc R U . . .
C3 C 0.3560(4) 0.3274(4) -0.0165(3) 0.0813(17) Uani 1 1 d . . . . .
H3 H 0.3973 0.3666 -0.0029 0.098 Uiso 1 1 calc R U . . .
C2 C 0.3627(4) 0.2847(4) -0.0619(3) 0.0776(15) Uani 1 1 d . . . . .
H2 H 0.4089 0.2887 -0.0859 0.093 Uiso 1 1 calc R U . . .
C7 C 0.1706(5) 0.4343(5) 0.1381(3) 0.0870(19) Uani 1 1 d . . . . .
C9 C 0.2663(5) 0.3218(5) 0.1029(3) 0.0816(17) Uani 1 1 d . . . . .
C11 C 0.1518(6) 0.4398(5) -0.0095(3) 0.095(2) Uani 1 1 d . . . . .
H11A H 0.1105 0.4877 -0.0078 0.142 Uiso 1 1 calc R U . . .
H11B H 0.1249 0.3905 -0.0269 0.142 Uiso 1 1 calc R U . . .
H11C H 0.2030 0.4581 -0.0288 0.142 Uiso 1 1 calc R U . . .
C8 C 0.2316(5) 0.3680(5) 0.1444(3) 0.090(2) Uani 1 1 d . . . . .
H8 H 0.2500 0.3538 0.1782 0.108 Uiso 1 1 calc R U . . .
C5 C 0.1779(4) 0.4138(4) 0.0443(2) 0.0737(15) Uani 1 1 d . . . . .
C10 C 0.3331(6) 0.2486(7) 0.1092(4) 0.123(3) Uani 1 1 d . . . . .
H10A H 0.3393 0.2345 0.1458 0.184 Uiso 1 1 calc R U . . .
H10B H 0.3889 0.2674 0.0955 0.184 Uiso 1 1 calc R U . . .
H10C H 0.3134 0.1974 0.0904 0.184 Uiso 1 1 calc R U . . .
C12 C 0.1350(7) 0.4809(6) 0.1858(3) 0.127(3) Uani 1 1 d . . . . .
H12A H 0.1385 0.5435 0.1806 0.190 Uiso 1 1 calc R U . . .
H12B H 0.1691 0.4648 0.2161 0.190 Uiso 1 1 calc R U . . .
H12C H 0.0746 0.4643 0.1912 0.190 Uiso 1 1 calc R U . . .
C21 C 0.1323(7) -0.0402(7) 0.1584(3) 0.115(3) Uani 1 1 d . . . . .
H21 H 0.0884 -0.0770 0.1455 0.138 Uiso 1 1 calc R U . . .
C25 C 0.2699(9) 0.0250(6) 0.1505(3) 0.138(4) Uani 1 1 d . . . . .
H25 H 0.3179 0.0349 0.1285 0.166 Uiso 1 1 calc R U . A 1
C22 C 0.1171(12) 0.0053(11) 0.2051(4) 0.175(6) Uani 1 1 d . . . . .
H22 H 0.0676 0.0040 0.2267 0.210 Uiso 1 1 calc R U . B 1
O2 O 0.5000 0.5000 0.0716(8) 0.273(13) Uani 1 2 d S T P . .
C23A C 0.223(5) 0.071(2) 0.2134(18) 0.17(2) Uani 0.55(5) 1 d . . P C 1
H23A H 0.1842 0.0839 0.2406 0.209 Uiso 0.55(5) 1 calc R U P C 1
C24A C 0.273(5) 0.068(2) 0.1931(10) 0.22(3) Uani 0.55(5) 1 d . . P C 1
H24A H 0.3247 0.0961 0.2036 0.267 Uiso 0.55(5) 1 calc R U P C 1
C23B C 0.1666(19) 0.052(2) 0.2263(9) 0.094(9) Uani 0.45(5) 1 d . . P C 2
H23B H 0.1683 0.0585 0.2627 0.113 Uiso 0.45(5) 1 calc R U P C 2
C24B C 0.225(6) 0.101(5) 0.192(3) 0.26(4) Uani 0.45(5) 1 d . . P C 2
H24B H 0.2360 0.1610 0.1924 0.316 Uiso 0.45(5) 1 calc R U P C 2
C31 C 0.4776(12) 0.9227(10) 0.1424(5) 0.182(5) Uani 1 1 d . . . . .
H31A H 0.4151 0.9090 0.1413 0.218 Uiso 1 1 calc R U . . .
H31B H 0.5107 0.8702 0.1334 0.218 Uiso 1 1 calc R U . . .
C30 C 0.5019(13) 0.9537(9) 0.1929(4) 0.212(9) Uani 1 1 d . . . . .
H30A H 0.4620 0.9303 0.2192 0.254 Uiso 1 1 calc R U . . .
H30B H 0.5611 0.9343 0.2013 0.254 Uiso 1 1 calc R U . . .
C29 C 0.5275(15) 0.5603(16) 0.1068(9) 0.292(16) Uani 1 1 d . . . . .
H29A H 0.5044 0.6173 0.0964 0.350 Uiso 1 1 calc R U . . .
H29B H 0.5913 0.5638 0.1048 0.350 Uiso 1 1 calc R U . . .
O3 O 0.5000 1.0000 0.1039(8) 0.327(14) Uani 1 2 d S T P . .
C28 C 0.505(2) 0.5456(12) 0.1576(7) 0.302(16) Uani 1 1 d . . . . .
H28A H 0.4497 0.5748 0.1666 0.362 Uiso 1 1 calc R U . . .
H28B H 0.5505 0.5646 0.1817 0.362 Uiso 1 1 calc R U . . .
C14 C 0.2867(3) 0.0774(4) -0.0937(2) 0.0621(12) Uani 1 1 d . . . . .
C19 C 0.3037(4) 0.0502(4) -0.0380(2) 0.0673(13) Uani 1 1 d . . . . .
H19A H 0.3067 0.1017 -0.0161 0.101 Uiso 1 1 calc R U . . .
H19B H 0.3586 0.0189 -0.0361 0.101 Uiso 1 1 calc R U . . .
H19C H 0.2568 0.0127 -0.0261 0.101 Uiso 1 1 calc R U . . .
C13 C 0.2773(4) 0.1666(4) -0.1070(2) 0.0641(13) Uani 1 1 d . . . . .
C20 C 0.2473(5) 0.2880(5) -0.1721(3) 0.092(2) Uani 1 1 d . . . . .
H20A H 0.2388 0.2938 -0.2093 0.138 Uiso 1 1 calc R U . . .
H20B H 0.2973 0.3226 -0.1615 0.138 Uiso 1 1 calc R U . . .
H20C H 0.1957 0.3085 -0.1540 0.138 Uiso 1 1 calc R U . . .
C18 C 0.2632(4) 0.1929(5) -0.1587(2) 0.0748(16) Uani 1 1 d . . . . .
C16 C 0.2664(5) 0.0388(5) -0.1853(2) 0.0837(18) Uani 1 1 d . . . . .
C17 C 0.2583(5) 0.1276(5) -0.1972(3) 0.0851(19) Uani 1 1 d . . . . .
H17 H 0.2493 0.1443 -0.2320 0.102 Uiso 1 1 calc R U . . .
C15 C 0.2804(4) 0.0156(4) -0.1331(2) 0.0705(14) Uani 1 1 d . . . . .
H15 H 0.2858 -0.0437 -0.1245 0.085 Uiso 1 1 calc R U . . .
C20A C 0.2593(6) -0.0302(6) -0.2283(3) 0.116(3) Uani 1 1 d . . . . .
H20D H 0.2671 -0.0878 -0.2133 0.175 Uiso 1 1 calc R U . . .
H20E H 0.3040 -0.0200 -0.2542 0.175 Uiso 1 1 calc R U . . .
H20F H 0.2022 -0.0266 -0.2445 0.175 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 O1 2.660(4) 2 ?
K1 O1 2.661(3) . ?
K1 O1 2.707(3) 7 ?
K1 N1 2.805(4) . ?
K1 C27 3.137(5) 7 ?
K1 C21 3.418(9) . ?
K1 C26 3.450(6) . ?
K1 C15 3.497(6) 7 ?
K1 C27 3.530(5) . ?
K1 K1 3.735(2) 2 ?
K1 K1 4.1011(18) 8 ?
K1 K1 4.1011(18) 7 ?
O1 C27 1.280(6) . ?
O1 K1 2.660(4) 2 ?
O1 K1 2.707(3) 8 ?
N1 C1 1.281(6) . ?
N1 C27 1.411(6) 7 ?
N4 C27 1.311(6) . ?
N4 C26 1.389(8) . ?
N2 C1 1.397(7) . ?
N2 C2 1.399(7) . ?
N2 C13 1.436(7) . ?
N3 C1 1.374(7) . ?
N3 C3 1.398(7) . ?
N3 C4 1.432(7) . ?
C27 N1 1.411(6) 8 ?
C27 K1 3.137(5) 8 ?
C26 C25 1.361(11) . ?
C26 C21 1.378(11) . ?
C4 C9 1.390(9) . ?
C4 C5 1.403(9) . ?
C6 C7 1.362(10) . ?
C6 C5 1.379(9) . ?
C6 H6 0.9300 . ?
C3 C2 1.331(9) . ?
C3 H3 0.9300 . ?
C2 H2 0.9300 . ?
C7 C8 1.377(10) . ?
C7 C12 1.506(9) . ?
C9 C8 1.373(10) . ?
C9 C10 1.512(11) . ?
C11 C5 1.480(9) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C8 H8 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C21 C22 1.393(13) . ?
C21 H21 0.9300 . ?
C25 C24A 1.27(3) . ?
C25 C24B 1.70(7) . ?
C25 C23A 1.88(7) . ?
C25 H25 0.9300 . ?
C22 C23B 1.17(3) . ?
C22 C23A 1.90(6) . ?
C22 H22 0.9300 . ?
O2 C29 1.35(2) 2_665 ?
O2 C29 1.35(2) . ?
C23A C24A 0.92(9) . ?
C23A H23A 0.9300 . ?
C24A H24A 0.9300 . ?
C23B C24B 1.44(10) . ?
C23B H23B 0.9300 . ?
C24B H24B 0.9300 . ?
C31 C30 1.417(15) . ?
C31 O3 1.566(15) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C30 C30 1.40(3) 2_675 ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C29 C28 1.36(3) . ?
C29 C29 2.01(4) 2_665 ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
O3 C31 1.566(15) 2_675 ?
C28 C28 1.39(3) 2_665 ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C14 C15 1.376(8) . ?
C14 C13 1.402(8) . ?
C14 C19 1.499(8) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C13 C18 1.390(8) . ?
C20 C18 1.503(10) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C18 C17 1.395(9) . ?
C16 C17 1.387(11) . ?
C16 C15 1.391(9) . ?
C16 C20A 1.518(9) . ?
C17 H17 0.9300 . ?
C15 K1 3.497(6) 8 ?
C15 H15 0.9300 . ?
C20A H20D 0.9600 . ?
C20A H20E 0.9600 . ?
C20A H20F 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 K1 O1 87.84(11) 2 . ?
O1 K1 O1 80.35(10) 2 7 ?
O1 K1 O1 80.34(10) . 7 ?
O1 K1 N1 118.74(12) 2 . ?
O1 K1 N1 110.39(12) . . ?
O1 K1 N1 49.02(11) 7 . ?
O1 K1 C27 94.78(12) 2 7 ?
O1 K1 C27 99.80(12) . 7 ?
O1 K1 C27 23.87(11) 7 7 ?
N1 K1 C27 26.73(12) . 7 ?
O1 K1 C21 105.4(2) 2 . ?
O1 K1 C21 56.69(16) . . ?
O1 K1 C21 135.84(16) 7 . ?
N1 K1 C21 134.0(2) . . ?
C27 K1 C21 147.41(18) 7 . ?
O1 K1 C26 124.51(15) 2 . ?
O1 K1 C26 52.43(12) . . ?
O1 K1 C26 120.51(14) 7 . ?
N1 K1 C26 111.47(15) . . ?
C27 K1 C26 125.33(16) 7 . ?
C21 K1 C26 23.14(19) . . ?
O1 K1 C15 83.41(12) 2 7 ?
O1 K1 C15 154.26(13) . 7 ?
O1 K1 C15 121.60(13) 7 7 ?
N1 K1 C15 95.00(13) . 7 ?
C27 K1 C15 105.01(14) 7 7 ?
C21 K1 C15 102.54(17) . 7 ?
C26 K1 C15 114.90(14) . 7 ?
O1 K1 C27 105.35(11) 2 . ?
O1 K1 C27 17.64(11) . . ?
O1 K1 C27 85.56(11) 7 . ?
N1 K1 C27 102.68(12) . . ?
C27 K1 C27 99.98(9) 7 . ?
C21 K1 C27 50.42(15) . . ?
C26 K1 C27 39.00(13) . . ?
C15 K1 C27 152.74(13) 7 . ?
O1 K1 K1 45.43(7) 2 2 ?
O1 K1 K1 45.41(8) . 2 ?
O1 K1 K1 89.53(7) 7 2 ?
N1 K1 K1 138.03(8) . 2 ?
C27 K1 K1 113.10(9) 7 2 ?
C21 K1 K1 68.39(18) . 2 ?
C26 K1 K1 81.47(12) . 2 ?
C15 K1 K1 116.10(11) 7 2 ?
C27 K1 K1 61.74(9) . 2 ?
O1 K1 K1 82.67(7) 2 8 ?
O1 K1 K1 40.59(7) . 8 ?
O1 K1 K1 39.75(8) 7 8 ?
N1 K1 K1 77.80(9) . 8 ?
C27 K1 K1 60.33(9) 7 8 ?
C21 K1 K1 96.67(14) . 8 ?
C26 K1 K1 86.32(11) . 8 ?
C15 K1 K1 158.69(10) 7 8 ?
C27 K1 K1 47.83(8) . 8 ?
K1 K1 K1 62.913(15) 2 8 ?
O1 K1 K1 40.59(7) 2 7 ?
O1 K1 K1 82.66(7) . 7 ?
O1 K1 K1 39.77(7) 7 7 ?
N1 K1 K1 82.86(9) . 7 ?
C27 K1 K1 56.50(9) 7 7 ?
C21 K1 K1 130.62(18) . 7 ?
C26 K1 K1 135.07(11) . 7 ?
C15 K1 K1 105.37(10) 7 7 ?
C27 K1 K1 97.35(8) . 7 ?
K1 K1 K1 62.913(15) 2 7 ?
K1 K1 K1 54.17(3) 8 7 ?
C27 O1 K1 139.9(3) . 2 ?
C27 O1 K1 123.3(3) . . ?
K1 O1 K1 89.16(11) 2 . ?
C27 O1 K1 97.3(3) . 8 ?
K1 O1 K1 99.66(11) 2 8 ?
K1 O1 K1 99.64(11) . 8 ?
C1 N1 C27 119.7(4) . 7 ?
C1 N1 K1 146.7(3) . . ?
C27 N1 K1 89.9(3) 7 . ?
C27 N4 C26 119.5(5) . . ?
C1 N2 C2 110.1(4) . . ?
C1 N2 C13 126.2(4) . . ?
C2 N2 C13 123.0(4) . . ?
C1 N3 C3 109.7(5) . . ?
C1 N3 C4 124.2(5) . . ?
C3 N3 C4 125.3(5) . . ?
N1 C1 N3 125.1(5) . . ?
N1 C1 N2 130.3(5) . . ?
N3 C1 N2 104.5(4) . . ?
O1 C27 N4 127.8(5) . . ?
O1 C27 N1 116.4(4) . 8 ?
N4 C27 N1 115.4(4) . 8 ?
O1 C27 K1 58.9(2) . 8 ?
N4 C27 K1 150.0(4) . 8 ?
N1 C27 K1 63.4(2) 8 8 ?
O1 C27 K1 39.0(2) . . ?
N4 C27 K1 94.7(3) . . ?
N1 C27 K1 137.8(3) 8 . ?
K1 C27 K1 75.67(10) 8 . ?
C25 C26 C21 115.7(8) . . ?
C25 C26 N4 118.5(8) . . ?
C21 C26 N4 125.4(7) . . ?
C25 C26 K1 102.8(5) . . ?
C21 C26 K1 77.1(4) . . ?
N4 C26 K1 96.6(3) . . ?
C9 C4 C5 122.0(6) . . ?
C9 C4 N3 120.1(6) . . ?
C5 C4 N3 117.8(5) . . ?
C7 C6 C5 123.1(7) . . ?
C7 C6 H6 118.5 . . ?
C5 C6 H6 118.5 . . ?
C2 C3 N3 108.8(5) . . ?
C2 C3 H3 125.6 . . ?
N3 C3 H3 125.6 . . ?
C3 C2 N2 107.0(5) . . ?
C3 C2 H2 126.5 . . ?
N2 C2 H2 126.5 . . ?
C6 C7 C8 118.1(6) . . ?
C6 C7 C12 122.5(8) . . ?
C8 C7 C12 119.4(8) . . ?
C8 C9 C4 117.2(7) . . ?
C8 C9 C10 123.4(7) . . ?
C4 C9 C10 119.4(6) . . ?
C5 C11 H11A 109.5 . . ?
C5 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C5 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C8 C7 122.8(7) . . ?
C9 C8 H8 118.6 . . ?
C7 C8 H8 118.6 . . ?
C6 C5 C4 116.8(6) . . ?
C6 C5 C11 122.3(6) . . ?
C4 C5 C11 120.9(6) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C7 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C26 C21 C22 122.6(12) . . ?
C26 C21 K1 79.7(4) . . ?
C22 C21 K1 104.7(8) . . ?
C26 C21 H21 118.7 . . ?
C22 C21 H21 118.7 . . ?
K1 C21 H21 85.5 . . ?
C24A C25 C26 132(3) . . ?
C26 C25 C24B 113(3) . . ?
C24A C25 C23A 25(3) . . ?
C26 C25 C23A 107.4(18) . . ?
C24A C25 H25 113.8 . . ?
C26 C25 H25 113.8 . . ?
C23A C25 H25 138.4 . . ?
C23B C22 C21 126.1(19) . . ?
C21 C22 C23A 102(2) . . ?
C21 C22 H22 128.9 . . ?
C23A C22 H22 128.9 . . ?
C29 O2 C29 97(2) 2_665 . ?
C24A C23A C25 36(4) . . ?
C24A C23A C22 128(5) . . ?
C25 C23A C22 91.9(12) . . ?
C24A C23A H23A 161.8 . . ?
C25 C23A H23A 161.8 . . ?
C22 C23A H23A 70.1 . . ?
C23A C24A C25 118(6) . . ?
C23A C24A H24A 120.9 . . ?
C25 C24A H24A 120.9 . . ?
C22 C23B C24B 115(4) . . ?
C22 C23B H23B 122.5 . . ?
C24B C23B H23B 122.5 . . ?
C23B C24B C25 106(4) . . ?
C23B C24B H24B 126.9 . . ?
C25 C24B H24B 126.9 . . ?
C30 C31 O3 105.2(12) . . ?
C30 C31 H31A 110.7 . . ?
O3 C31 H31A 110.7 . . ?
C30 C31 H31B 110.7 . . ?
O3 C31 H31B 110.7 . . ?
H31A C31 H31B 108.8 . . ?
C30 C30 C31 108.7(11) 2_675 . ?
C30 C30 H30A 109.9 2_675 . ?
C31 C30 H30A 109.9 . . ?
C30 C30 H30B 109.9 2_675 . ?
C31 C30 H30B 109.9 . . ?
H30A C30 H30B 108.3 . . ?
O2 C29 C28 116.2(18) . . ?
O2 C29 C29 41.6(11) . 2_665 ?
C28 C29 C29 75.2(11) . 2_665 ?
O2 C29 H29A 108.2 . . ?
C28 C29 H29A 108.2 . . ?
C29 C29 H29A 131.3 2_665 . ?
O2 C29 H29B 108.2 . . ?
C28 C29 H29B 108.2 . . ?
C29 C29 H29B 117.6 2_665 . ?
H29A C29 H29B 107.4 . . ?
C31 O3 C31 102.5(15) . 2_675 ?
C29 C28 C28 100.9(16) . 2_665 ?
C29 C28 H28A 111.6 . . ?
C28 C28 H28A 111.6 2_665 . ?
C29 C28 H28B 111.6 . . ?
C28 C28 H28B 111.6 2_665 . ?
H28A C28 H28B 109.4 . . ?
C15 C14 C13 118.3(5) . . ?
C15 C14 C19 120.9(5) . . ?
C13 C14 C19 120.7(5) . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C13 C14 121.4(5) . . ?
C18 C13 N2 119.2(5) . . ?
C14 C13 N2 119.3(5) . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C13 C18 C17 118.0(6) . . ?
C13 C18 C20 121.0(6) . . ?
C17 C18 C20 120.9(6) . . ?
C17 C16 C15 117.8(6) . . ?
C17 C16 C20A 120.5(7) . . ?
C15 C16 C20A 121.7(7) . . ?
C16 C17 C18 122.1(6) . . ?
C16 C17 H17 118.9 . . ?
C18 C17 H17 118.9 . . ?
C14 C15 C16 122.4(6) . . ?
C14 C15 K1 85.5(3) . 8 ?
C16 C15 K1 118.1(4) . 8 ?
C14 C15 H15 118.8 . . ?
C16 C15 H15 118.8 . . ?
K1 C15 H15 65.9 8 . ?
C16 C20A H20D 109.5 . . ?
C16 C20A H20E 109.5 . . ?
H20D C20A H20E 109.5 . . ?
C16 C20A H20F 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C27 N1 C1 N3 154.3(5) 7 . . . ?
K1 N1 C1 N3 -56.4(9) . . . . ?
C27 N1 C1 N2 -30.2(8) 7 . . . ?
K1 N1 C1 N2 119.2(6) . . . . ?
C3 N3 C1 N1 176.5(5) . . . . ?
C4 N3 C1 N1 -13.4(9) . . . . ?
C3 N3 C1 N2 0.0(6) . . . . ?
C4 N3 C1 N2 170.1(5) . . . . ?
C2 N2 C1 N1 -176.6(6) . . . . ?
C13 N2 C1 N1 -6.4(9) . . . . ?
C2 N2 C1 N3 -0.4(6) . . . . ?
C13 N2 C1 N3 169.8(5) . . . . ?
K1 O1 C27 N4 -101.2(6) 2 . . . ?
K1 O1 C27 N4 37.7(6) . . . . ?
K1 O1 C27 N4 144.3(5) 8 . . . ?
K1 O1 C27 N1 86.6(5) 2 . . 8 ?
K1 O1 C27 N1 -134.5(3) . . . 8 ?
K1 O1 C27 N1 -27.8(4) 8 . . 8 ?
K1 O1 C27 K1 114.5(4) 2 . . 8 ?
K1 O1 C27 K1 -106.6(3) . . . 8 ?
K1 O1 C27 K1 -138.9(6) 2 . . . ?
K1 O1 C27 K1 106.6(3) 8 . . . ?
C26 N4 C27 O1 10.2(8) . . . . ?
C26 N4 C27 N1 -177.5(5) . . . 8 ?
C26 N4 C27 K1 102.2(7) . . . 8 ?
C26 N4 C27 K1 33.0(5) . . . . ?
C27 N4 C26 C25 -142.4(7) . . . . ?
C27 N4 C26 C21 44.9(9) . . . . ?
C27 N4 C26 K1 -34.0(5) . . . . ?
C1 N3 C4 C9 107.5(7) . . . . ?
C3 N3 C4 C9 -84.0(8) . . . . ?
C1 N3 C4 C5 -74.6(7) . . . . ?
C3 N3 C4 C5 93.9(7) . . . . ?
C1 N3 C3 C2 0.3(8) . . . . ?
C4 N3 C3 C2 -169.6(6) . . . . ?
N3 C3 C2 N2 -0.5(8) . . . . ?
C1 N2 C2 C3 0.5(7) . . . . ?
C13 N2 C2 C3 -170.0(5) . . . . ?
C5 C6 C7 C8 0.8(10) . . . . ?
C5 C6 C7 C12 179.9(7) . . . . ?
C5 C4 C9 C8 -1.1(9) . . . . ?
N3 C4 C9 C8 176.7(6) . . . . ?
C5 C4 C9 C10 -179.7(6) . . . . ?
N3 C4 C9 C10 -2.0(9) . . . . ?
C4 C9 C8 C7 1.7(11) . . . . ?
C10 C9 C8 C7 -179.7(7) . . . . ?
C6 C7 C8 C9 -1.6(11) . . . . ?
C12 C7 C8 C9 179.3(8) . . . . ?
C7 C6 C5 C4 -0.3(10) . . . . ?
C7 C6 C5 C11 -178.4(6) . . . . ?
C9 C4 C5 C6 0.4(8) . . . . ?
N3 C4 C5 C6 -177.4(5) . . . . ?
C9 C4 C5 C11 178.5(6) . . . . ?
N3 C4 C5 C11 0.7(8) . . . . ?
C25 C26 C21 C22 -2.8(13) . . . . ?
N4 C26 C21 C22 170.1(9) . . . . ?
K1 C26 C21 C22 -101.0(10) . . . . ?
C25 C26 C21 K1 98.2(6) . . . . ?
N4 C26 C21 K1 -88.9(6) . . . . ?
C21 C26 C25 C24A 9(4) . . . . ?
N4 C26 C25 C24A -165(4) . . . . ?
K1 C26 C25 C24A 90(4) . . . . ?
C21 C26 C25 C24B -20(4) . . . . ?
N4 C26 C25 C24B 167(3) . . . . ?
K1 C26 C25 C24B 62(3) . . . . ?
C21 C26 C25 C23A 2.9(15) . . . . ?
N4 C26 C25 C23A -170.5(13) . . . . ?
K1 C26 C25 C23A 84.6(13) . . . . ?
C26 C21 C22 C23B -1(3) . . . . ?
K1 C21 C22 C23B -88(2) . . . . ?
C26 C21 C22 C23A 1.0(17) . . . . ?
K1 C21 C22 C23A -86.2(13) . . . . ?
C26 C25 C23A C24A 170(6) . . . . ?
C24B C25 C23A C24A -80(11) . . . . ?
C24A C25 C23A C22 -172(7) . . . . ?
C26 C25 C23A C22 -2.0(17) . . . . ?
C24B C25 C23A C22 107(10) . . . . ?
C22 C23A C24A C25 10(8) . . . . ?
C26 C25 C24A C23A -13(8) . . . . ?
C24B C25 C24A C23A 47(10) . . . . ?
C21 C22 C23B C24B 32(5) . . . . ?
C23A C22 C23B C24B 27(5) . . . . ?
C22 C23B C24B C25 -50(6) . . . . ?
C24A C25 C24B C23B -91(9) . . . . ?
C26 C25 C24B C23B 45(6) . . . . ?
C23A C25 C24B C23B -34(7) . . . . ?
O3 C31 C30 C30 26(2) . . . 2_675 ?
C29 O2 C29 C28 -10.6(18) 2_665 . . . ?
C30 C31 O3 C31 -9.4(10) . . . 2_675 ?
O2 C29 C28 C28 26(4) . . . 2_665 ?
C29 C29 C28 C28 19(3) 2_665 . . 2_665 ?
C15 C14 C13 C18 -0.9(8) . . . . ?
C19 C14 C13 C18 178.7(5) . . . . ?
C15 C14 C13 N2 -177.4(5) . . . . ?
C19 C14 C13 N2 2.1(8) . . . . ?
C1 N2 C13 C18 118.2(6) . . . . ?
C2 N2 C13 C18 -72.9(7) . . . . ?
C1 N2 C13 C14 -65.2(7) . . . . ?
C2 N2 C13 C14 103.8(6) . . . . ?
C14 C13 C18 C17 0.2(9) . . . . ?
N2 C13 C18 C17 176.8(5) . . . . ?
C14 C13 C18 C20 175.9(6) . . . . ?
N2 C13 C18 C20 -7.5(9) . . . . ?
C15 C16 C17 C18 -0.4(11) . . . . ?
C20A C16 C17 C18 179.1(7) . . . . ?
C13 C18 C17 C16 0.4(10) . . . . ?
C20 C18 C17 C16 -175.3(7) . . . . ?
C13 C14 C15 C16 0.9(8) . . . . ?
C19 C14 C15 C16 -178.7(6) . . . . ?
C13 C14 C15 K1 -119.8(5) . . . 8 ?
C19 C14 C15 K1 60.7(5) . . . 8 ?
C17 C16 C15 C14 -0.2(10) . . . . ?
C20A C16 C15 C14 -179.7(6) . . . . ?
C17 C16 C15 K1 103.3(7) . . . 8 ?
C20A C16 C15 K1 -76.2(8) . . . 8 ?

_refine_diff_density_max         0.246
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.049

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_2c
_database_code_depnum_ccdc_archive 'CCDC 1046053'
_audit_update_record             
;
2015-03-02 deposited with the CCDC.
2015-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C80 H118 K4 N10 O2 Si4'
_chemical_formula_sum            'C40 H59 K2 N5 O Si2'
_chemical_formula_weight         760.30

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 '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      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                   28.2189(18)
_cell_length_b                   10.5566(7)
_cell_length_c                   31.0868(17)
_cell_angle_alpha                90
_cell_angle_beta                 108.476(6)
_cell_angle_gamma                90
_cell_volume                     8783.3(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7624
_cell_measurement_theta_min      2.9240
_cell_measurement_theta_max      71.1901

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_F_000             3264
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    2.691
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.63659
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at Zero'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            38290
_diffrn_reflns_av_unetI/netI     0.0708
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.928
_diffrn_reflns_theta_max         69.999
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             16320
_reflns_number_gt                11175
_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       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP III & Olex 2.1'
_computing_publication_material  'MS Word'

_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)+(0.1141P)²+3.7744P] 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         16320
_refine_ls_number_parameters     955
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0830
_refine_ls_wR_factor_ref         0.2367
_refine_ls_wR_factor_gt          0.2127
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_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 0.22583(3) 0.73160(11) 0.11739(3) 0.0563(3) Uani 1 1 d . . . . .
K2 K 0.33207(5) 0.87280(12) 0.23556(3) 0.0682(3) Uani 1 1 d . . . . .
K3 K 0.16753(5) 0.41306(12) 0.27509(3) 0.0738(3) Uani 1 1 d . . . . .
K4 K 0.27678(3) 1.25097(12) 0.38397(3) 0.0647(3) Uani 1 1 d . . . . .
Si1 Si 0.32640(4) 0.94741(13) 0.12159(4) 0.0529(3) Uani 1 1 d . . . . .
Si2 Si 0.35678(4) 0.67352(12) 0.14957(4) 0.0496(3) Uani 1 1 d . . . . .
Si3 Si 0.14765(4) 0.17317(11) 0.34944(4) 0.0469(3) Uani 1 1 d . . . . .
Si4 Si 0.17607(4) 0.42541(11) 0.39845(3) 0.0428(2) Uani 1 1 d . . . . .
N1 N 0.14386(10) 0.6268(3) 0.13231(9) 0.0344(6) Uani 1 1 d . . . . .
N2 N 0.05299(10) 0.5903(3) 0.11897(9) 0.0339(6) Uani 1 1 d . . . . .
N3 N 0.08273(10) 0.6096(3) 0.06249(9) 0.0354(6) Uani 1 1 d . . . . .
N4 N 0.20928(11) 0.6622(3) 0.19588(9) 0.0430(7) Uani 1 1 d . . . . .
N5 N 0.32485(11) 0.8075(3) 0.14631(10) 0.0438(7) Uani 1 1 d . . . . .
N6 N 0.17804(11) 0.3110(3) 0.36219(10) 0.0402(7) Uani 1 1 d . . . . .
N7 N 0.35316(11) 1.1240(3) 0.36980(9) 0.0382(7) Uani 1 1 d . . . . .
N8 N 0.41660(11) 1.1229(3) 0.43852(10) 0.0399(7) Uani 1 1 d . . . . .
N9 N 0.44308(11) 1.0885(3) 0.38025(9) 0.0386(7) Uani 1 1 d . . . . .
N10 N 0.29065(11) 1.1695(3) 0.30538(9) 0.0392(7) Uani 1 1 d . . . . .
O1 O 0.14651(10) 0.5264(3) 0.19974(8) 0.0451(6) Uani 1 1 d . . . . .
O2 O 0.34432(10) 1.0008(3) 0.30621(9) 0.0502(7) Uani 1 1 d . . . . .
C1 C 0.09754(12) 0.6077(3) 0.10967(10) 0.0311(7) Uani 1 1 d . . . . .
C2 C 0.01273(13) 0.5874(4) 0.07840(12) 0.0385(8) Uani 1 1 d . . . . .
H2 H -0.0208 0.5779 0.0758 0.046 Uiso 1 1 calc R U . . .
C3 C 0.03134(13) 0.6009(4) 0.04424(12) 0.0384(8) Uani 1 1 d . . . . .
H3 H 0.0130 0.6039 0.0136 0.046 Uiso 1 1 calc R U . . .
C4 C 0.04552(12) 0.5806(4) 0.16279(11) 0.0373(8) Uani 1 1 d . . . . .
C5 C 0.05197(13) 0.6881(4) 0.18969(12) 0.0427(8) Uani 1 1 d . . . . .
C6 C 0.04637(16) 0.6740(5) 0.23231(14) 0.0547(11) Uani 1 1 d . . . . .
H6 H 0.0516 0.7432 0.2518 0.066 Uiso 1 1 calc R U . . .
C7 C 0.03317(17) 0.5589(5) 0.24616(14) 0.0618(12) Uani 1 1 d . . . . .
H7 H 0.0299 0.5514 0.2749 0.074 Uiso 1 1 calc R U . . .
C8 C 0.02477(15) 0.4550(5) 0.21792(13) 0.0516(10) Uani 1 1 d . . . . .
H8 H 0.0150 0.3786 0.2274 0.062 Uiso 1 1 calc R U . . .
C9 C 0.03077(13) 0.4635(4) 0.17493(12) 0.0398(8) Uani 1 1 d . . . . .
C10 C 0.02313(14) 0.3475(4) 0.14429(13) 0.0452(9) Uani 1 1 d . . . . .
H10 H 0.0119 0.3782 0.1129 0.054 Uiso 1 1 calc R U . . .
C11 C -0.0165(2) 0.2584(6) 0.1494(2) 0.095(2) Uani 1 1 d . . . . .
H11A H -0.0259 0.2008 0.1242 0.142 Uiso 1 1 calc R U . . .
H11B H -0.0452 0.3061 0.1501 0.142 Uiso 1 1 calc R U . . .
H11C H -0.0036 0.2114 0.1771 0.142 Uiso 1 1 calc R U . . .
C12 C 0.0720(2) 0.2793(5) 0.1512(2) 0.0768(15) Uani 1 1 d . . . . .
H12A H 0.0830 0.2423 0.1809 0.115 Uiso 1 1 calc R U . . .
H12B H 0.0966 0.3383 0.1482 0.115 Uiso 1 1 calc R U . . .
H12C H 0.0674 0.2138 0.1288 0.115 Uiso 1 1 calc R U . . .
C13 C 0.06391(16) 0.8156(4) 0.17315(15) 0.0530(10) Uani 1 1 d . . . . .
H13 H 0.0898 0.8013 0.1588 0.064 Uiso 1 1 calc R U . . .
C14 C 0.08438(19) 0.9138(5) 0.21069(18) 0.0665(13) Uani 1 1 d . . . . .
H14A H 0.0583 0.9397 0.2224 0.100 Uiso 1 1 calc R U . . .
H14B H 0.0964 0.9861 0.1985 0.100 Uiso 1 1 calc R U . . .
H14C H 0.1113 0.8772 0.2346 0.100 Uiso 1 1 calc R U . . .
C15 C 0.0183(2) 0.8738(5) 0.13670(18) 0.0747(15) Uani 1 1 d . . . . .
H15A H 0.0062 0.8154 0.1120 0.112 Uiso 1 1 calc R U . . .
H15B H 0.0280 0.9514 0.1258 0.112 Uiso 1 1 calc R U . . .
H15C H -0.0077 0.8906 0.1498 0.112 Uiso 1 1 calc R U . . .
C16 C 0.11700(13) 0.6315(4) 0.03800(11) 0.0387(8) Uani 1 1 d . . . . .
C17 C 0.11743(15) 0.7497(4) 0.01836(12) 0.0460(9) Uani 1 1 d . . . . .
C18 C 0.15112(18) 0.7695(5) -0.00541(16) 0.0604(12) Uani 1 1 d . . . . .
H18 H 0.1519 0.8476 -0.0190 0.072 Uiso 1 1 calc R U . . .
C19 C 0.18344(19) 0.6743(6) -0.00898(16) 0.0683(14) Uani 1 1 d . . . . .
H19 H 0.2061 0.6891 -0.0246 0.082 Uiso 1 1 calc R U . . .
C20 C 0.18207(16) 0.5554(5) 0.01086(14) 0.0559(11) Uani 1 1 d . . . . .
H20 H 0.2036 0.4917 0.0079 0.067 Uiso 1 1 calc R U . . .
C21 C 0.14917(14) 0.5318(4) 0.03483(12) 0.0425(8) Uani 1 1 d . . . . .
C22 C 0.08425(16) 0.8581(4) 0.02418(14) 0.0499(10) Uani 1 1 d . . . . .
H22 H 0.0588 0.8213 0.0358 0.060 Uiso 1 1 calc R U . . .
C23 C 0.0566(2) 0.9237(7) -0.02080(19) 0.097(2) Uani 1 1 d . . . . .
H23A H 0.0344 0.9866 -0.0157 0.145 Uiso 1 1 calc R U . . .
H23B H 0.0377 0.8621 -0.0421 0.145 Uiso 1 1 calc R U . . .
H23C H 0.0804 0.9636 -0.0327 0.145 Uiso 1 1 calc R U . . .
C24 C 0.1140(2) 0.9517(5) 0.0593(2) 0.0811(16) Uani 1 1 d . . . . .
H24A H 0.1283 0.9091 0.0877 0.122 Uiso 1 1 calc R U . . .
H24B H 0.0924 1.0183 0.0629 0.122 Uiso 1 1 calc R U . . .
H24C H 0.1403 0.9871 0.0495 0.122 Uiso 1 1 calc R U . . .
C25 C 0.14714(15) 0.4029(4) 0.05634(13) 0.0465(9) Uani 1 1 d . . . . .
H25 H 0.1424 0.4182 0.0858 0.056 Uiso 1 1 calc R U . . .
C26 C 0.10126(17) 0.3292(5) 0.02710(18) 0.0647(12) Uani 1 1 d . . . . .
H26A H 0.0717 0.3791 0.0231 0.097 Uiso 1 1 calc R U . . .
H26B H 0.0985 0.2511 0.0419 0.097 Uiso 1 1 calc R U . . .
H26C H 0.1049 0.3114 -0.0020 0.097 Uiso 1 1 calc R U . . .
C27 C 0.19420(17) 0.3236(5) 0.06481(15) 0.0600(11) Uani 1 1 d . . . . .
H27A H 0.1968 0.2948 0.0364 0.090 Uiso 1 1 calc R U . . .
H27B H 0.1926 0.2519 0.0833 0.090 Uiso 1 1 calc R U . . .
H27C H 0.2229 0.3741 0.0801 0.090 Uiso 1 1 calc R U . . .
C28 C 0.16570(12) 0.6022(4) 0.17929(11) 0.0351(7) Uani 1 1 d . . . . .
C29 C 0.23430(14) 0.6516(4) 0.24248(11) 0.0411(8) Uani 1 1 d . . . . .
C30 C 0.21379(17) 0.6991(5) 0.27468(13) 0.0543(10) Uani 1 1 d . . . . .
H30 H 0.1813 0.7302 0.2652 0.065 Uiso 1 1 calc R U . . .
C31 C 0.24117(19) 0.7006(5) 0.32082(14) 0.0621(12) Uani 1 1 d . . . . .
H31 H 0.2269 0.7326 0.3417 0.075 Uiso 1 1 calc R U . . .
C32 C 0.28923(18) 0.6545(6) 0.33524(14) 0.0696(14) Uani 1 1 d . . . . .
H32 H 0.3083 0.6597 0.3657 0.084 Uiso 1 1 calc R U . . .
C33 C 0.30892(18) 0.6010(7) 0.30462(15) 0.0767(17) Uani 1 1 d . . . . .
H33 H 0.3403 0.5634 0.3145 0.092 Uiso 1 1 calc R U . . .
C34 C 0.28171(16) 0.6031(5) 0.25826(14) 0.0591(12) Uani 1 1 d . . . . .
H34 H 0.2963 0.5706 0.2376 0.071 Uiso 1 1 calc R U . . .
C35 C 0.18810(17) 1.1119(5) 0.17521(15) 0.0612(12) Uani 1 1 d . . . . .
H35 H 0.1649 1.1007 0.1466 0.073 Uiso 1 1 calc R U . . .
C36 C 0.20405(16) 1.0104(5) 0.20330(15) 0.0609(12) Uani 1 1 d . . . . .
H36 H 0.1919 0.9300 0.1936 0.073 Uiso 1 1 calc R U . . .
C37 C 0.23874(14) 1.0265(5) 0.24684(13) 0.0504(10) Uani 1 1 d . . . . .
H37 H 0.2483 0.9567 0.2659 0.060 Uiso 1 1 calc R U . . .
C38 C 0.4036(2) 0.6470(6) 0.2077(2) 0.0817(17) Uani 1 1 d . . . . .
H38A H 0.3873 0.6562 0.2304 0.123 Uiso 1 1 calc R U . . .
H38B H 0.4300 0.7082 0.2130 0.123 Uiso 1 1 calc R U . . .
H38C H 0.4173 0.5632 0.2093 0.123 Uiso 1 1 calc R U . . .
C39 C 0.3147(2) 0.5281(6) 0.1372(2) 0.0775(16) Uani 1 1 d . . . . .
H39A H 0.2933 0.5298 0.1558 0.116 Uiso 1 1 calc R U . . .
H39B H 0.3349 0.4530 0.1437 0.116 Uiso 1 1 calc R U . . .
H39C H 0.2947 0.5282 0.1058 0.116 Uiso 1 1 calc R U . . .
C40 C 0.3946(2) 0.6538(7) 0.1099(2) 0.093(2) Uani 1 1 d . . . . .
H40A H 0.3735 0.6664 0.0793 0.140 Uiso 1 1 calc R U . . .
H40B H 0.4085 0.5700 0.1131 0.140 Uiso 1 1 calc R U . . .
H40C H 0.4212 0.7149 0.1172 0.140 Uiso 1 1 calc R U . . .
C41 C 0.38590(19) 0.9891(6) 0.1111(2) 0.0852(19) Uani 1 1 d . . . . .
H41A H 0.4131 0.9826 0.1389 0.128 Uiso 1 1 calc R U . . .
H41B H 0.3839 1.0743 0.0998 0.128 Uiso 1 1 calc R U . . .
H41C H 0.3914 0.9320 0.0891 0.128 Uiso 1 1 calc R U . . .
C42 C 0.3175(3) 1.0855(5) 0.1581(2) 0.0874(17) Uani 1 1 d . . . . .
H42A H 0.2873 1.0732 0.1655 0.131 Uiso 1 1 calc R U . . .
H42B H 0.3154 1.1633 0.1416 0.131 Uiso 1 1 calc R U . . .
H42C H 0.3454 1.0892 0.1855 0.131 Uiso 1 1 calc R U . . .
C43 C 0.2742(2) 0.9685(7) 0.06677(19) 0.101(2) Uani 1 1 d . . . . .
H43A H 0.2430 0.9475 0.0712 0.151 Uiso 1 1 calc R U . . .
H43B H 0.2796 0.9139 0.0441 0.151 Uiso 1 1 calc R U . . .
H43C H 0.2733 1.0550 0.0570 0.151 Uiso 1 1 calc R U . . .
C44 C 0.39979(13) 1.1090(4) 0.39167(11) 0.0367(8) Uani 1 1 d . . . . .
C45 C 0.46848(14) 1.1185(4) 0.45481(13) 0.0442(9) Uani 1 1 d . . . . .
H45 H 0.4882 1.1290 0.4848 0.053 Uiso 1 1 calc R U . . .
C46 C 0.48495(13) 1.0965(4) 0.41954(13) 0.0460(9) Uani 1 1 d . . . . .
H46 H 0.5182 1.0881 0.4208 0.055 Uiso 1 1 calc R U . . .
C47 C 0.44862(13) 1.0601(4) 0.33673(12) 0.0417(8) Uani 1 1 d . . . . .
C48 C 0.43868(14) 1.1547(4) 0.30357(13) 0.0460(9) Uani 1 1 d . . . . .
C49 C 0.44635(17) 1.1230(6) 0.26276(15) 0.0640(13) Uani 1 1 d . . . . .
H49 H 0.4401 1.1830 0.2397 0.077 Uiso 1 1 calc R U . . .
C50 C 0.46305(18) 1.0045(6) 0.25601(17) 0.0742(16) Uani 1 1 d . . . . .
H50 H 0.4676 0.9854 0.2284 0.089 Uiso 1 1 calc R U . . .
C51 C 0.47304(17) 0.9143(5) 0.28916(17) 0.0664(13) Uani 1 1 d . . . . .
H51 H 0.4851 0.8356 0.2841 0.080 Uiso 1 1 calc R U . . .
C52 C 0.46531(15) 0.9392(5) 0.33071(15) 0.0520(10) Uani 1 1 d . . . . .
C53 C 0.47311(19) 0.8347(5) 0.36543(18) 0.0665(13) Uani 1 1 d . . . . .
H53 H 0.4747 0.8747 0.3943 0.080 Uiso 1 1 calc R U . . .
C54 C 0.4285(3) 0.7485(7) 0.3527(3) 0.097(2) Uani 1 1 d . . . . .
H54A H 0.4262 0.7059 0.3248 0.146 Uiso 1 1 calc R U . . .
H54B H 0.3988 0.7975 0.3489 0.146 Uiso 1 1 calc R U . . .
H54C H 0.4320 0.6871 0.3763 0.146 Uiso 1 1 calc R U . . .
C55 C 0.5216(3) 0.7622(8) 0.3733(3) 0.142(4) Uani 1 1 d . . . . .
H55A H 0.5280 0.7112 0.4001 0.214 Uiso 1 1 calc R U . . .
H55B H 0.5486 0.8210 0.3770 0.214 Uiso 1 1 calc R U . . .
H55C H 0.5189 0.7086 0.3476 0.214 Uiso 1 1 calc R U . . .
C56 C 0.4665(2) 1.3676(6) 0.3369(3) 0.103(2) Uani 1 1 d . . . . .
H56A H 0.4856 1.3266 0.3645 0.154 Uiso 1 1 calc R U . . .
H56B H 0.4547 1.4478 0.3438 0.154 Uiso 1 1 calc R U . . .
H56C H 0.4873 1.3807 0.3181 0.154 Uiso 1 1 calc R U . . .
C57 C 0.42166(17) 1.2836(5) 0.31155(16) 0.0591(12) Uani 1 1 d . . . . .
H57 H 0.3991 1.2764 0.3297 0.071 Uiso 1 1 calc R U . A 1
C58 C 0.398(3) 1.367(6) 0.2707(17) 0.104(12) Uani 0.52(12) 1 d . . P B 1
H58A H 0.3890 1.4470 0.2807 0.156 Uiso 0.52(12) 1 calc R U P B 1
H58B H 0.3681 1.3262 0.2515 0.156 Uiso 0.52(12) 1 calc R U P B 1
H58C H 0.4208 1.3797 0.2542 0.156 Uiso 0.52(12) 1 calc R U P B 1
C58A C 0.3823(14) 1.334(4) 0.2653(10) 0.066(7) Uani 0.48(12) 1 d . . P B 2
H58D H 0.3710 1.4172 0.2701 0.099 Uiso 0.48(12) 1 calc R U P B 2
H58E H 0.3542 1.2776 0.2560 0.099 Uiso 0.48(12) 1 calc R U P B 2
H58F H 0.3980 1.3381 0.2421 0.099 Uiso 0.48(12) 1 calc R U P B 2
C59 C 0.38441(13) 1.1512(4) 0.46453(11) 0.0405(8) Uani 1 1 d . . . . .
C60 C 0.35360(14) 1.0537(4) 0.47204(12) 0.0426(8) Uani 1 1 d . . . . .
C61 C 0.32276(16) 1.0852(5) 0.49737(14) 0.0522(10) Uani 1 1 d . . . . .
H61 H 0.3019 1.0235 0.5029 0.063 Uiso 1 1 calc R U . . .
C62 C 0.32201(19) 1.2065(5) 0.51473(16) 0.0608(12) Uani 1 1 d . . . . .
H62 H 0.3015 1.2250 0.5322 0.073 Uiso 1 1 calc R U . . .
C63 C 0.35216(17) 1.2992(5) 0.50572(15) 0.0558(11) Uani 1 1 d . . . . .
H63 H 0.3511 1.3807 0.5168 0.067 Uiso 1 1 calc R U . . .
C64 C 0.38383(15) 1.2747(4) 0.48083(13) 0.0459(9) Uani 1 1 d . . . . .
C65 C 0.41479(16) 1.3801(4) 0.46934(15) 0.0533(10) Uani 1 1 d . . . . .
H65 H 0.4447 1.3411 0.4654 0.064 Uiso 1 1 calc R U . . .
C66 C 0.4321(3) 1.4811(6) 0.5059(2) 0.0897(19) Uani 1 1 d . . . . .
H66A H 0.4038 1.5282 0.5079 0.135 Uiso 1 1 calc R U . . .
H66B H 0.4550 1.5374 0.4983 0.135 Uiso 1 1 calc R U . . .
H66C H 0.4486 1.4414 0.5345 0.135 Uiso 1 1 calc R U . . .
C67 C 0.3863(2) 1.4433(6) 0.42512(17) 0.0747(15) Uani 1 1 d . . . . .
H67A H 0.3749 1.3802 0.4019 0.112 Uiso 1 1 calc R U . . .
H67B H 0.4079 1.5018 0.4167 0.112 Uiso 1 1 calc R U . . .
H67C H 0.3582 1.4880 0.4287 0.112 Uiso 1 1 calc R U . . .
C68 C 0.35453(15) 0.9206(4) 0.45327(14) 0.0495(9) Uani 1 1 d . . . . .
H68 H 0.3534 0.9297 0.4216 0.059 Uiso 1 1 calc R U . . .
C69 C 0.30990(18) 0.8405(5) 0.45340(17) 0.0640(12) Uani 1 1 d . . . . .
H69A H 0.3100 0.7631 0.4372 0.096 Uiso 1 1 calc R U . . .
H69B H 0.2797 0.8864 0.4390 0.096 Uiso 1 1 calc R U . . .
H69C H 0.3119 0.8214 0.4841 0.096 Uiso 1 1 calc R U . . .
C70 C 0.40225(17) 0.8513(5) 0.47782(17) 0.0651(12) Uani 1 1 d . . . . .
H70A H 0.4036 0.8360 0.5086 0.098 Uiso 1 1 calc R U . . .
H70B H 0.4304 0.9020 0.4775 0.098 Uiso 1 1 calc R U . . .
H70C H 0.4031 0.7720 0.4630 0.098 Uiso 1 1 calc R U . . .
C71 C 0.32914(13) 1.0930(4) 0.32364(11) 0.0379(8) Uani 1 1 d . . . . .
C72 C 0.25908(13) 1.1449(4) 0.26203(12) 0.0417(8) Uani 1 1 d . . . . .
C73 C 0.24148(16) 1.2476(4) 0.23225(13) 0.0532(10) Uani 1 1 d . . . . .
H73 H 0.2535 1.3285 0.2415 0.064 Uiso 1 1 calc R U . . .
C74 C 0.20657(17) 1.2312(5) 0.18935(15) 0.0624(12) Uani 1 1 d . . . . .
H74 H 0.1957 1.3006 0.1703 0.075 Uiso 1 1 calc R U . . .
C76 C 0.10166(19) 0.1297(6) 0.37950(19) 0.0725(15) Uani 1 1 d . . . . .
H76A H 0.1192 0.1145 0.4110 0.109 Uiso 1 1 calc R U . . .
H76B H 0.0839 0.0545 0.3661 0.109 Uiso 1 1 calc R U . . .
H76C H 0.0784 0.1979 0.3767 0.109 Uiso 1 1 calc R U . . .
C77 C 0.1109(3) 0.1651(7) 0.28724(19) 0.108(3) Uani 1 1 d . . . . .
H77A H 0.1322 0.1871 0.2697 0.163 Uiso 1 1 calc R U . . .
H77B H 0.0835 0.2235 0.2807 0.163 Uiso 1 1 calc R U . . .
H77C H 0.0984 0.0807 0.2797 0.163 Uiso 1 1 calc R U . . .
C78 C 0.13210(19) 0.5569(5) 0.37255(17) 0.0704(14) Uani 1 1 d . . . . .
H78A H 0.1398 0.5897 0.3467 0.106 Uiso 1 1 calc R U . . .
H78B H 0.1354 0.6232 0.3945 0.106 Uiso 1 1 calc R U . . .
H78C H 0.0984 0.5256 0.3631 0.106 Uiso 1 1 calc R U . . .
C79 C 0.1594(2) 0.3698(6) 0.44999(16) 0.0797(16) Uani 1 1 d . . . . .
H79A H 0.1245 0.3496 0.4412 0.119 Uiso 1 1 calc R U . . .
H79B H 0.1667 0.4358 0.4724 0.119 Uiso 1 1 calc R U . . .
H79C H 0.1786 0.2958 0.4625 0.119 Uiso 1 1 calc R U . . .
C80 C 0.23843(19) 0.5046(5) 0.42458(19) 0.0619(12) Uani 1 1 d . . . . .
C75 C 0.1902(4) 0.0323(8) 0.3588(5) 0.115(4) Uani 1 1 d . . . . .
H80B H 0.233(2) 0.589(6) 0.4384(19) 0.094(19) Uiso 1 1 d . . . . .
H80A H 0.2648(19) 0.453(5) 0.4459(17) 0.073(15) Uiso 1 1 d . . . . .
H80C H 0.252(2) 0.523(6) 0.402(2) 0.10(2) Uiso 1 1 d . . . . .
H75A H 0.207(2) 0.038(6) 0.391(2) 0.09(3) Uiso 1 1 d . . . . .
H75C H 0.173(3) -0.034(7) 0.351(2) 0.12(3) Uiso 1 1 d . . . . .
H75B H 0.214(3) 0.042(7) 0.346(2) 0.11(3) 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 N4 2.726(3) . ?
K1 N1 2.733(3) . ?
K1 N5 2.769(3) . ?
K1 C28 3.243(3) . ?
K1 C16 3.440(3) . ?
K1 C21 3.492(4) . ?
K1 Si2 3.5623(14) . ?
K1 Si1 3.6092(15) . ?
K1 K2 4.2100(14) . ?
K2 O2 2.508(3) . ?
K2 N5 2.803(3) . ?
K2 C37 3.206(4) . ?
K2 C34 3.356(5) . ?
K2 Si1 3.5832(15) . ?
K2 Si2 3.6385(15) . ?
K3 O1 2.527(3) . ?
K3 N6 2.841(3) . ?
K3 C30 3.291(5) . ?
K3 C73 3.308(5) 1_545 ?
K3 C29 3.482(4) . ?
K3 Si3 3.5906(16) . ?
K3 Si4 3.7678(14) . ?
K3 K4 4.1563(15) 1_545 ?
K4 N7 2.690(3) . ?
K4 N6 2.726(3) 1_565 ?
K4 N10 2.733(3) . ?
K4 C71 3.200(4) . ?
K4 C75 3.271(10) 1_565 ?
K4 C80 3.287(6) 1_565 ?
K4 C59 3.433(4) . ?
K4 Si4 3.5329(14) 1_565 ?
K4 C64 3.534(4) . ?
K4 Si3 3.5533(15) 1_565 ?
K4 K3 4.1564(15) 1_565 ?
Si1 N5 1.672(4) . ?
Si1 C41 1.862(5) . ?
Si1 C43 1.880(5) . ?
Si1 C42 1.912(6) . ?
Si2 N5 1.663(4) . ?
Si2 C40 1.880(5) . ?
Si2 C38 1.893(5) . ?
Si2 C39 1.904(5) . ?
Si3 N6 1.672(3) . ?
Si3 C75 1.875(7) . ?
Si3 C76 1.880(5) . ?
Si3 C77 1.884(6) . ?
Si3 K4 3.5532(15) 1_545 ?
Si4 N6 1.665(3) . ?
Si4 C78 1.866(5) . ?
Si4 C80 1.884(5) . ?
Si4 C79 1.900(5) . ?
Si4 K4 3.5328(14) 1_545 ?
N1 C1 1.289(4) . ?
N1 C28 1.418(4) . ?
N2 C1 1.388(4) . ?
N2 C2 1.405(4) . ?
N2 C4 1.447(4) . ?
N3 C3 1.383(4) . ?
N3 C1 1.392(4) . ?
N3 C16 1.427(4) . ?
N4 C28 1.334(5) . ?
N4 C29 1.400(4) . ?
N6 K4 2.725(3) 1_545 ?
N7 C44 1.285(4) . ?
N7 C71 1.418(4) . ?
N8 C44 1.389(4) . ?
N8 C45 1.390(5) . ?
N8 C59 1.426(5) . ?
N9 C44 1.393(4) . ?
N9 C46 1.407(5) . ?
N9 C47 1.442(5) . ?
N10 C71 1.328(5) . ?
N10 C72 1.384(4) . ?
O1 C28 1.247(4) . ?
O2 C71 1.254(5) . ?
C2 C3 1.333(5) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C5 1.387(5) . ?
C4 C9 1.394(5) . ?
C5 C6 1.391(5) . ?
C5 C13 1.516(6) . ?
C6 C7 1.379(7) . ?
C6 H6 0.9300 . ?
C7 C8 1.378(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.402(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.524(6) . ?
C10 C11 1.507(6) . ?
C10 C12 1.509(7) . ?
C10 H10 0.9800 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.531(6) . ?
C13 C15 1.547(7) . ?
C13 H13 0.9800 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.391(6) . ?
C16 C21 1.414(5) . ?
C17 C18 1.392(6) . ?
C17 C22 1.525(6) . ?
C18 C19 1.386(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.404(7) . ?
C19 H19 0.9300 . ?
C20 C21 1.385(6) . ?
C20 H20 0.9300 . ?
C21 C25 1.525(6) . ?
C22 C24 1.514(7) . ?
C22 C23 1.534(6) . ?
C22 H22 0.9800 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C27 1.520(6) . ?
C25 C26 1.537(6) . ?
C25 H25 0.9800 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C29 C34 1.370(6) . ?
C29 C30 1.399(6) . ?
C30 C31 1.397(5) . ?
C30 H30 0.9300 . ?
C31 C32 1.375(7) . ?
C31 H31 0.9300 . ?
C32 C33 1.367(7) . ?
C32 H32 0.9300 . ?
C33 C34 1.402(6) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 C36 1.365(7) . ?
C35 C74 1.381(7) . ?
C35 H35 0.9300 . ?
C36 C37 1.407(6) . ?
C36 H36 0.9300 . ?
C37 C72 1.394(6) . ?
C37 H37 0.9300 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C45 C46 1.340(5) . ?
C45 H45 0.9300 . ?
C46 H46 0.9300 . ?
C47 C52 1.394(6) . ?
C47 C48 1.398(6) . ?
C48 C49 1.393(6) . ?
C48 C57 1.490(6) . ?
C49 C50 1.377(8) . ?
C49 H49 0.9300 . ?
C50 C51 1.365(8) . ?
C50 H50 0.9300 . ?
C51 C52 1.401(6) . ?
C51 H51 0.9300 . ?
C52 C53 1.510(7) . ?
C53 C54 1.501(8) . ?
C53 C55 1.519(7) . ?
C53 H53 0.9800 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C56 C57 1.542(8) . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C57 C58 1.51(4) . ?
C57 C58A 1.60(3) . ?
C57 H57 0.9800 . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
C58A H58D 0.9600 . ?
C58A H58E 0.9600 . ?
C58A H58F 0.9600 . ?
C59 C64 1.401(6) . ?
C59 C60 1.414(5) . ?
C60 C61 1.386(6) . ?
C60 C68 1.525(6) . ?
C61 C62 1.393(7) . ?
C61 H61 0.9300 . ?
C62 C63 1.382(7) . ?
C62 H62 0.9300 . ?
C63 C64 1.379(6) . ?
C63 H63 0.9300 . ?
C64 C65 1.525(6) . ?
C65 C67 1.510(6) . ?
C65 C66 1.522(7) . ?
C65 H65 0.9800 . ?
C66 H66A 0.9600 . ?
C66 H66B 0.9600 . ?
C66 H66C 0.9600 . ?
C67 H67A 0.9600 . ?
C67 H67B 0.9600 . ?
C67 H67C 0.9600 . ?
C68 C70 1.510(6) . ?
C68 C69 1.517(6) . ?
C68 H68 0.9800 . ?
C69 H69A 0.9600 . ?
C69 H69B 0.9600 . ?
C69 H69C 0.9600 . ?
C70 H70A 0.9600 . ?
C70 H70B 0.9600 . ?
C70 H70C 0.9600 . ?
C72 C73 1.409(6) . ?
C73 C74 1.395(6) . ?
C73 K3 3.308(5) 1_565 ?
C73 H73 0.9300 . ?
C74 H74 0.9300 . ?
C76 H76A 0.9600 . ?
C76 H76B 0.9600 . ?
C76 H76C 0.9600 . ?
C77 H77A 0.9600 . ?
C77 H77B 0.9600 . ?
C77 H77C 0.9600 . ?
C78 H78A 0.9600 . ?
C78 H78B 0.9600 . ?
C78 H78C 0.9600 . ?
C79 H79A 0.9600 . ?
C79 H79B 0.9600 . ?
C79 H79C 0.9600 . ?
C80 K4 3.287(6) 1_545 ?
C80 H80B 1.02(6) . ?
C80 H80A 0.99(5) . ?
C80 H80C 0.90(6) . ?
C75 K4 3.271(10) 1_545 ?
C75 H75A 0.96(5) . ?
C75 H75C 0.85(7) . ?
C75 H75B 0.88(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 K1 N1 49.08(8) . . ?
N4 K1 N5 103.21(9) . . ?
N1 K1 N5 152.05(9) . . ?
N4 K1 C28 23.86(8) . . ?
N1 K1 C28 25.67(8) . . ?
N5 K1 C28 126.38(9) . . ?
N4 K1 C16 101.10(9) . . ?
N1 K1 C16 52.14(8) . . ?
N5 K1 C16 154.35(9) . . ?
C28 K1 C16 77.31(8) . . ?
N4 K1 C21 104.69(10) . . ?
N1 K1 C21 61.30(9) . . ?
N5 K1 C21 137.71(10) . . ?
C28 K1 C21 82.12(9) . . ?
C16 K1 C21 23.52(9) . . ?
N4 K1 Si2 99.16(7) . . ?
N1 K1 Si2 137.83(7) . . ?
N5 K1 Si2 26.91(8) . . ?
C28 K1 Si2 116.88(7) . . ?
C16 K1 Si2 139.41(7) . . ?
C21 K1 Si2 116.64(7) . . ?
N4 K1 Si1 119.53(7) . . ?
N1 K1 Si1 161.34(8) . . ?
N5 K1 Si1 26.43(7) . . ?
C28 K1 Si1 142.91(7) . . ?
C16 K1 Si1 137.12(7) . . ?
C21 K1 Si1 134.80(7) . . ?
Si2 K1 Si1 50.55(3) . . ?
N4 K1 K2 65.83(7) . . ?
N1 K1 K2 113.71(6) . . ?
N5 K1 K2 41.23(7) . . ?
C28 K1 K2 89.61(6) . . ?
C16 K1 K2 164.08(7) . . ?
C21 K1 K2 163.54(8) . . ?
Si2 K1 K2 55.07(3) . . ?
Si1 K1 K2 53.89(3) . . ?
O2 K2 N5 161.11(12) . . ?
O2 K2 C37 61.41(10) . . ?
N5 K2 C37 115.36(10) . . ?
O2 K2 C34 102.88(11) . . ?
N5 K2 C34 95.56(11) . . ?
C37 K2 C34 89.37(12) . . ?
O2 K2 Si1 134.28(9) . . ?
N5 K2 Si1 26.98(7) . . ?
C37 K2 Si1 102.48(8) . . ?
C34 K2 Si1 120.35(8) . . ?
O2 K2 Si2 161.75(8) . . ?
N5 K2 Si2 26.02(7) . . ?
C37 K2 Si2 136.75(8) . . ?
C34 K2 Si2 81.75(9) . . ?
Si1 K2 Si2 50.18(3) . . ?
O2 K2 K1 144.83(7) . . ?
N5 K2 K1 40.62(6) . . ?
C37 K2 K1 83.81(8) . . ?
C34 K2 K1 69.59(7) . . ?
Si1 K2 K1 54.46(3) . . ?
Si2 K2 K1 53.38(3) . . ?
O1 K3 N6 170.28(11) . . ?
O1 K3 C30 62.56(9) . . ?
N6 K3 C30 115.45(10) . . ?
O1 K3 C73 82.51(10) . 1_545 ?
N6 K3 C73 107.15(10) . 1_545 ?
C30 K3 C73 100.45(12) . 1_545 ?
O1 K3 C29 51.53(8) . . ?
N6 K3 C29 130.45(9) . . ?
C30 K3 C29 23.61(10) . . ?
C73 K3 C29 78.23(11) 1_545 . ?
O1 K3 Si3 153.09(8) . . ?
N6 K3 Si3 27.06(7) . . ?
C30 K3 Si3 142.43(8) . . ?
C73 K3 Si3 97.69(9) 1_545 . ?
C29 K3 Si3 155.04(7) . . ?
O1 K3 Si4 147.93(8) . . ?
N6 K3 Si4 24.40(7) . . ?
C30 K3 Si4 94.28(8) . . ?
C73 K3 Si4 125.66(8) 1_545 . ?
C29 K3 Si4 113.91(7) . . ?
Si3 K3 Si4 48.84(3) . . ?
O1 K3 K4 147.69(8) . 1_545 ?
N6 K3 K4 40.65(6) . 1_545 ?
C30 K3 K4 100.84(8) . 1_545 ?
C73 K3 K4 73.18(7) 1_545 1_545 ?
C29 K3 K4 101.80(7) . 1_545 ?
Si3 K3 K4 54.00(3) . 1_545 ?
Si4 K3 K4 52.68(2) . 1_545 ?
N7 K4 N6 152.16(10) . 1_565 ?
N7 K4 N10 49.28(8) . . ?
N6 K4 N10 106.02(9) 1_565 . ?
N7 K4 C71 26.06(9) . . ?
N6 K4 C71 126.96(9) 1_565 . ?
N10 K4 C71 24.26(9) . . ?
N7 K4 C75 100.71(16) . 1_565 ?
N6 K4 C75 58.50(15) 1_565 1_565 ?
N10 K4 C75 82.6(2) . 1_565 ?
C71 K4 C75 86.60(19) . 1_565 ?
N7 K4 C80 147.91(12) . 1_565 ?
N6 K4 C80 58.04(11) 1_565 1_565 ?
N10 K4 C80 139.27(13) . 1_565 ?
C71 K4 C80 156.82(14) . 1_565 ?
C75 K4 C80 110.79(17) 1_565 1_565 ?
N7 K4 C59 52.92(9) . . ?
N6 K4 C59 148.32(9) 1_565 . ?
N10 K4 C59 102.20(9) . . ?
C71 K4 C59 78.56(9) . . ?
C75 K4 C59 112.3(2) 1_565 . ?
C80 K4 C59 107.01(12) 1_565 . ?
N7 K4 Si4 177.58(8) . 1_565 ?
N6 K4 Si4 27.13(7) 1_565 1_565 ?
N10 K4 Si4 128.82(7) . 1_565 ?
C71 K4 Si4 152.36(7) . 1_565 ?
C75 K4 Si4 80.11(14) 1_565 1_565 ?
C80 K4 Si4 31.82(9) 1_565 1_565 ?
C59 K4 Si4 128.93(7) . 1_565 ?
N7 K4 C64 70.25(9) . . ?
N6 K4 C64 136.52(10) 1_565 . ?
N10 K4 C64 117.27(9) . . ?
C71 K4 C64 96.18(9) . . ?
C75 K4 C64 128.7(2) 1_565 . ?
C80 K4 C64 84.92(12) 1_565 . ?
C59 K4 C64 23.14(10) . . ?
Si4 K4 C64 111.06(7) 1_565 . ?
N7 K4 Si3 129.31(8) . 1_565 ?
N6 K4 Si3 26.99(7) 1_565 1_565 ?
N10 K4 Si3 94.64(7) . 1_565 ?
C71 K4 Si3 108.80(7) . 1_565 ?
C75 K4 Si3 31.56(13) 1_565 1_565 ?
C80 K4 Si3 82.73(9) 1_565 1_565 ?
C59 K4 Si3 137.30(8) . 1_565 ?
Si4 K4 Si3 50.92(3) 1_565 1_565 ?
C64 K4 Si3 142.34(8) . 1_565 ?
N7 K4 K3 119.85(7) . 1_565 ?
N6 K4 K3 42.77(7) 1_565 1_565 ?
N10 K4 K3 71.40(7) . 1_565 ?
C71 K4 K3 95.64(7) . 1_565 ?
C75 K4 K3 77.9(2) 1_565 1_565 ?
C80 K4 K3 74.21(10) 1_565 1_565 ?
C59 K4 K3 167.65(7) . 1_565 ?
Si4 K4 K3 58.01(3) 1_565 1_565 ?
C64 K4 K3 151.37(8) . 1_565 ?
Si3 K4 K3 54.84(3) 1_565 1_565 ?
N5 Si1 C41 116.5(2) . . ?
N5 Si1 C43 113.2(2) . . ?
C41 Si1 C43 107.7(3) . . ?
N5 Si1 C42 111.9(2) . . ?
C41 Si1 C42 102.6(3) . . ?
C43 Si1 C42 103.6(3) . . ?
N5 Si1 K2 49.52(11) . . ?
C41 Si1 K2 117.72(18) . . ?
C43 Si1 K2 134.4(2) . . ?
C42 Si1 K2 63.50(18) . . ?
N5 Si1 K1 47.49(11) . . ?
C41 Si1 K1 152.3(2) . . ?
C43 Si1 K1 70.17(19) . . ?
C42 Si1 K1 104.7(2) . . ?
K2 Si1 K1 71.65(3) . . ?
N5 Si2 C40 117.6(3) . . ?
N5 Si2 C38 112.6(2) . . ?
C40 Si2 C38 103.9(3) . . ?
N5 Si2 C39 112.5(2) . . ?
C40 Si2 C39 103.0(3) . . ?
C38 Si2 C39 106.0(3) . . ?
N5 Si2 K1 48.89(11) . . ?
C40 Si2 K1 126.1(2) . . ?
C38 Si2 K1 130.0(2) . . ?
C39 Si2 K1 63.70(19) . . ?
N5 Si2 K2 47.67(11) . . ?
C40 Si2 K2 145.7(2) . . ?
C38 Si2 K2 67.8(2) . . ?
C39 Si2 K2 111.23(18) . . ?
K1 Si2 K2 71.55(3) . . ?
N6 Si3 C75 113.5(4) . . ?
N6 Si3 C76 118.5(2) . . ?
C75 Si3 C76 103.7(3) . . ?
N6 Si3 C77 110.9(2) . . ?
C75 Si3 C77 103.9(5) . . ?
C76 Si3 C77 104.9(3) . . ?
N6 Si3 K4 47.73(11) . 1_545 ?
C75 Si3 K4 65.9(3) . 1_545 ?
C76 Si3 K4 135.19(18) . 1_545 ?
C77 Si3 K4 119.9(2) . 1_545 ?
N6 Si3 K3 50.62(10) . . ?
C75 Si3 K3 115.9(3) . . ?
C76 Si3 K3 139.9(2) . . ?
C77 Si3 K3 61.2(2) . . ?
K4 Si3 K3 71.15(4) 1_545 . ?
N6 Si4 C78 114.07(19) . . ?
N6 Si4 C80 112.8(2) . . ?
C78 Si4 C80 105.0(3) . . ?
N6 Si4 C79 114.6(2) . . ?
C78 Si4 C79 106.6(3) . . ?
C80 Si4 C79 102.7(3) . . ?
N6 Si4 K4 48.30(10) . 1_545 ?
C78 Si4 K4 141.68(19) . 1_545 ?
C80 Si4 K4 66.87(17) . 1_545 ?
C79 Si4 K4 111.7(2) . 1_545 ?
N6 Si4 K3 44.83(11) . . ?
C78 Si4 K3 76.54(17) . . ?
C80 Si4 K3 101.77(18) . . ?
C79 Si4 K3 153.43(18) . . ?
K4 Si4 K3 69.32(3) 1_545 . ?
C1 N1 C28 124.6(3) . . ?
C1 N1 K1 137.5(2) . . ?
C28 N1 K1 97.72(19) . . ?
C1 N2 C2 110.1(3) . . ?
C1 N2 C4 128.1(3) . . ?
C2 N2 C4 121.7(3) . . ?
C3 N3 C1 110.9(3) . . ?
C3 N3 C16 126.3(3) . . ?
C1 N3 C16 122.5(3) . . ?
C28 N4 C29 117.6(3) . . ?
C28 N4 K1 100.4(2) . . ?
C29 N4 K1 140.7(2) . . ?
Si2 N5 Si1 133.4(2) . . ?
Si2 N5 K1 104.20(16) . . ?
Si1 N5 K1 106.09(15) . . ?
Si2 N5 K2 106.31(14) . . ?
Si1 N5 K2 103.50(16) . . ?
K1 N5 K2 98.16(10) . . ?
Si4 N6 Si3 131.85(19) . . ?
Si4 N6 K4 104.56(13) . 1_545 ?
Si3 N6 K4 105.28(15) . 1_545 ?
Si4 N6 K3 110.77(16) . . ?
Si3 N6 K3 102.32(13) . . ?
K4 N6 K3 96.58(10) 1_545 . ?
C44 N7 C71 126.0(3) . . ?
C44 N7 K4 135.6(2) . . ?
C71 N7 K4 97.5(2) . . ?
C44 N8 C45 110.4(3) . . ?
C44 N8 C59 123.3(3) . . ?
C45 N8 C59 126.0(3) . . ?
C44 N9 C46 109.4(3) . . ?
C44 N9 C47 129.5(3) . . ?
C46 N9 C47 121.1(3) . . ?
C71 N10 C72 119.3(3) . . ?
C71 N10 K4 98.0(2) . . ?
C72 N10 K4 134.3(2) . . ?
C28 O1 K3 139.8(2) . . ?
C71 O2 K2 145.7(2) . . ?
N1 C1 N2 137.4(3) . . ?
N1 C1 N3 119.1(3) . . ?
N2 C1 N3 103.4(3) . . ?
C3 C2 N2 107.6(3) . . ?
C3 C2 H2 126.2 . . ?
N2 C2 H2 126.2 . . ?
C2 C3 N3 107.9(3) . . ?
C2 C3 H3 126.1 . . ?
N3 C3 H3 126.1 . . ?
C5 C4 C9 123.8(3) . . ?
C5 C4 N2 118.7(3) . . ?
C9 C4 N2 117.6(3) . . ?
C4 C5 C6 117.0(4) . . ?
C4 C5 C13 121.5(3) . . ?
C6 C5 C13 121.5(4) . . ?
C7 C6 C5 121.0(4) . . ?
C7 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C8 C7 C6 120.8(4) . . ?
C8 C7 H7 119.6 . . ?
C6 C7 H7 119.6 . . ?
C7 C8 C9 120.5(4) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 H8 119.8 . . ?
C4 C9 C8 116.9(4) . . ?
C4 C9 C10 122.6(3) . . ?
C8 C9 C10 120.5(4) . . ?
C11 C10 C12 111.2(5) . . ?
C11 C10 C9 113.5(4) . . ?
C12 C10 C9 110.6(3) . . ?
C11 C10 H10 107.1 . . ?
C12 C10 H10 107.1 . . ?
C9 C10 H10 107.1 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 C13 C14 114.4(4) . . ?
C5 C13 C15 112.2(4) . . ?
C14 C13 C15 108.4(4) . . ?
C5 C13 H13 107.2 . . ?
C14 C13 H13 107.2 . . ?
C15 C13 H13 107.2 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C21 122.8(3) . . ?
C17 C16 N3 118.8(3) . . ?
C21 C16 N3 118.4(3) . . ?
C17 C16 K1 84.8(2) . . ?
C21 C16 K1 80.3(2) . . ?
N3 C16 K1 105.60(19) . . ?
C16 C17 C18 118.0(4) . . ?
C16 C17 C22 122.0(3) . . ?
C18 C17 C22 119.9(4) . . ?
C19 C18 C17 120.7(4) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C18 C19 C20 120.2(4) . . ?
C18 C19 H19 119.9 . . ?
C20 C19 H19 119.9 . . ?
C21 C20 C19 120.9(4) . . ?
C21 C20 H20 119.5 . . ?
C19 C20 H20 119.5 . . ?
C20 C21 C16 117.3(4) . . ?
C20 C21 C25 121.4(4) . . ?
C16 C21 C25 121.3(3) . . ?
C20 C21 K1 85.5(3) . . ?
C16 C21 K1 76.2(2) . . ?
C25 C21 K1 108.5(2) . . ?
C24 C22 C17 110.7(4) . . ?
C24 C22 C23 111.6(5) . . ?
C17 C22 C23 112.7(4) . . ?
C24 C22 H22 107.2 . . ?
C17 C22 H22 107.2 . . ?
C23 C22 H22 107.2 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C27 C25 C21 114.5(4) . . ?
C27 C25 C26 110.4(4) . . ?
C21 C25 C26 109.5(3) . . ?
C27 C25 H25 107.3 . . ?
C21 C25 H25 107.3 . . ?
C26 C25 H25 107.3 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O1 C28 N4 127.2(3) . . ?
O1 C28 N1 121.7(3) . . ?
N4 C28 N1 110.9(3) . . ?
O1 C28 K1 165.0(3) . . ?
N4 C28 K1 55.77(18) . . ?
N1 C28 K1 56.61(16) . . ?
C34 C29 C30 117.2(3) . . ?
C34 C29 N4 121.0(4) . . ?
C30 C29 N4 121.6(4) . . ?
C34 C29 K3 100.5(3) . . ?
C30 C29 K3 70.5(2) . . ?
N4 C29 K3 102.6(2) . . ?
C31 C30 C29 121.3(4) . . ?
C31 C30 K3 95.6(3) . . ?
C29 C30 K3 85.9(3) . . ?
C31 C30 H30 119.4 . . ?
C29 C30 H30 119.4 . . ?
K3 C30 H30 88.5 . . ?
C32 C31 C30 119.9(4) . . ?
C32 C31 H31 120.1 . . ?
C30 C31 H31 120.1 . . ?
C33 C32 C31 119.7(4) . . ?
C33 C32 H32 120.2 . . ?
C31 C32 H32 120.2 . . ?
C32 C33 C34 119.9(5) . . ?
C32 C33 H33 120.1 . . ?
C34 C33 H33 120.1 . . ?
C29 C34 C33 121.9(4) . . ?
C29 C34 K2 92.2(3) . . ?
C33 C34 K2 95.7(4) . . ?
C29 C34 H34 119.0 . . ?
C33 C34 H34 119.0 . . ?
K2 C34 H34 81.9 . . ?
C36 C35 C74 119.8(4) . . ?
C36 C35 H35 120.1 . . ?
C74 C35 H35 120.1 . . ?
C35 C36 C37 120.6(5) . . ?
C35 C36 H36 119.7 . . ?
C37 C36 H36 119.7 . . ?
C72 C37 C36 121.3(4) . . ?
C72 C37 K2 103.1(2) . . ?
C36 C37 K2 100.3(3) . . ?
C72 C37 H37 119.3 . . ?
C36 C37 H37 119.3 . . ?
K2 C37 H37 65.5 . . ?
Si2 C38 H38A 109.5 . . ?
Si2 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
Si2 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
Si2 C39 H39A 109.5 . . ?
Si2 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
Si2 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
Si2 C40 H40A 109.5 . . ?
Si2 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
Si2 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
Si1 C41 H41A 109.5 . . ?
Si1 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
Si1 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
Si1 C42 H42A 109.5 . . ?
Si1 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
Si1 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
Si1 C43 H43A 109.5 . . ?
Si1 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
Si1 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N7 C44 N8 119.6(3) . . ?
N7 C44 N9 135.9(3) . . ?
N8 C44 N9 104.4(3) . . ?
C46 C45 N8 107.8(3) . . ?
C46 C45 H45 126.1 . . ?
N8 C45 H45 126.1 . . ?
C45 C46 N9 107.9(3) . . ?
C45 C46 H46 126.1 . . ?
N9 C46 H46 126.1 . . ?
C52 C47 C48 123.5(4) . . ?
C52 C47 N9 117.3(4) . . ?
C48 C47 N9 119.2(4) . . ?
C49 C48 C47 116.6(4) . . ?
C49 C48 C57 121.4(4) . . ?
C47 C48 C57 122.0(4) . . ?
C50 C49 C48 121.1(5) . . ?
C50 C49 H49 119.5 . . ?
C48 C49 H49 119.5 . . ?
C51 C50 C49 121.2(4) . . ?
C51 C50 H50 119.4 . . ?
C49 C50 H50 119.4 . . ?
C50 C51 C52 120.7(5) . . ?
C50 C51 H51 119.7 . . ?
C52 C51 H51 119.7 . . ?
C47 C52 C51 117.0(4) . . ?
C47 C52 C53 123.5(4) . . ?
C51 C52 C53 119.5(4) . . ?
C54 C53 C52 109.6(4) . . ?
C54 C53 C55 112.0(6) . . ?
C52 C53 C55 113.7(5) . . ?
C54 C53 H53 107.1 . . ?
C52 C53 H53 107.1 . . ?
C55 C53 H53 107.1 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C57 C56 H56A 109.5 . . ?
C57 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C57 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C48 C57 C58 118(2) . . ?
C48 C57 C56 110.7(4) . . ?
C58 C57 C56 100(4) . . ?
C48 C57 C58A 108.9(14) . . ?
C56 C57 C58A 119.3(18) . . ?
C48 C57 H57 109.2 . . ?
C58 C57 H57 109.2 . . ?
C56 C57 H57 109.2 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C57 C58A H58D 109.5 . . ?
C57 C58A H58E 109.5 . . ?
H58D C58A H58E 109.5 . . ?
C57 C58A H58F 109.5 . . ?
H58D C58A H58F 109.5 . . ?
H58E C58A H58F 109.5 . . ?
C64 C59 C60 122.7(4) . . ?
C64 C59 N8 118.8(3) . . ?
C60 C59 N8 118.5(4) . . ?
C64 C59 K4 82.5(2) . . ?
C60 C59 K4 84.0(2) . . ?
N8 C59 K4 103.05(19) . . ?
C61 C60 C59 116.6(4) . . ?
C61 C60 C68 121.9(4) . . ?
C59 C60 C68 121.4(3) . . ?
C60 C61 C62 122.0(4) . . ?
C60 C61 H61 119.0 . . ?
C62 C61 H61 119.0 . . ?
C63 C62 C61 119.1(4) . . ?
C63 C62 H62 120.4 . . ?
C61 C62 H62 120.4 . . ?
C64 C63 C62 122.1(4) . . ?
C64 C63 H63 119.0 . . ?
C62 C63 H63 119.0 . . ?
C63 C64 C59 117.5(4) . . ?
C63 C64 C65 121.0(4) . . ?
C59 C64 C65 121.4(4) . . ?
C63 C64 K4 87.7(3) . . ?
C59 C64 K4 74.4(2) . . ?
C65 C64 K4 104.5(2) . . ?
C67 C65 C66 108.9(5) . . ?
C67 C65 C64 110.9(4) . . ?
C66 C65 C64 114.1(4) . . ?
C67 C65 H65 107.6 . . ?
C66 C65 H65 107.6 . . ?
C64 C65 H65 107.6 . . ?
C65 C66 H66A 109.5 . . ?
C65 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C65 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C65 C67 H67A 109.5 . . ?
C65 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C65 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C70 C68 C69 109.7(4) . . ?
C70 C68 C60 111.9(4) . . ?
C69 C68 C60 113.4(4) . . ?
C70 C68 H68 107.2 . . ?
C69 C68 H68 107.2 . . ?
C60 C68 H68 107.2 . . ?
C68 C69 H69A 109.5 . . ?
C68 C69 H69B 109.5 . . ?
H69A C69 H69B 109.5 . . ?
C68 C69 H69C 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C68 C70 H70A 109.5 . . ?
C68 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C68 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
O2 C71 N10 129.3(3) . . ?
O2 C71 N7 119.8(3) . . ?
N10 C71 N7 110.9(3) . . ?
O2 C71 K4 160.5(3) . . ?
N10 C71 K4 57.76(18) . . ?
N7 C71 K4 56.47(17) . . ?
N10 C72 C37 124.5(4) . . ?
N10 C72 C73 118.7(4) . . ?
C37 C72 C73 116.5(3) . . ?
C74 C73 C72 121.9(4) . . ?
C74 C73 K3 96.1(3) . 1_565 ?
C72 C73 K3 106.1(3) . 1_565 ?
C74 C73 H73 119.1 . . ?
C72 C73 H73 119.1 . . ?
K3 C73 H73 66.8 1_565 . ?
C35 C74 C73 119.9(5) . . ?
C35 C74 H74 120.1 . . ?
C73 C74 H74 120.1 . . ?
Si3 C76 H76A 109.5 . . ?
Si3 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
Si3 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
Si3 C77 H77A 109.5 . . ?
Si3 C77 H77B 109.5 . . ?
H77A C77 H77B 109.5 . . ?
Si3 C77 H77C 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
Si4 C78 H78A 109.5 . . ?
Si4 C78 H78B 109.5 . . ?
H78A C78 H78B 109.5 . . ?
Si4 C78 H78C 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
Si4 C79 H79A 109.5 . . ?
Si4 C79 H79B 109.5 . . ?
H79A C79 H79B 109.5 . . ?
Si4 C79 H79C 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
Si4 C80 K4 81.31(18) . 1_545 ?
Si4 C80 H80B 109(3) . . ?
K4 C80 H80B 170(3) 1_545 . ?
Si4 C80 H80A 116(3) . . ?
K4 C80 H80A 62(3) 1_545 . ?
H80B C80 H80A 113(4) . . ?
Si4 C80 H80C 109(4) . . ?
K4 C80 H80C 67(4) 1_545 . ?
H80B C80 H80C 107(5) . . ?
H80A C80 H80C 103(5) . . ?
Si3 C75 K4 82.5(3) . 1_545 ?
Si3 C75 H75A 101(4) . . ?
K4 C75 H75A 68(4) 1_545 . ?
Si3 C75 H75C 109(5) . . ?
K4 C75 H75C 167(5) 1_545 . ?
H75A C75 H75C 114(7) . . ?
Si3 C75 H75B 112(5) . . ?
K4 C75 H75B 54(5) 1_545 . ?
H75A C75 H75B 105(6) . . ?
H75C C75 H75B 115(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C40 Si2 N5 Si1 -14.0(4) . . . . ?
C38 Si2 N5 Si1 106.8(3) . . . . ?
C39 Si2 N5 Si1 -133.5(3) . . . . ?
K1 Si2 N5 Si1 -129.2(3) . . . . ?
K2 Si2 N5 Si1 127.7(3) . . . . ?
C40 Si2 N5 K1 115.2(3) . . . . ?
C38 Si2 N5 K1 -124.0(2) . . . . ?
C39 Si2 N5 K1 -4.3(3) . . . . ?
K2 Si2 N5 K1 -103.09(15) . . . . ?
C40 Si2 N5 K2 -141.7(3) . . . . ?
C38 Si2 N5 K2 -20.9(3) . . . . ?
C39 Si2 N5 K2 98.8(2) . . . . ?
K1 Si2 N5 K2 103.09(15) . . . . ?
C41 Si1 N5 Si2 -23.7(4) . . . . ?
C43 Si1 N5 Si2 102.0(4) . . . . ?
C42 Si1 N5 Si2 -141.3(3) . . . . ?
K2 Si1 N5 Si2 -128.6(3) . . . . ?
K1 Si1 N5 Si2 128.6(3) . . . . ?
C41 Si1 N5 K1 -152.3(2) . . . . ?
C43 Si1 N5 K1 -26.6(3) . . . . ?
C42 Si1 N5 K1 90.1(2) . . . . ?
K2 Si1 N5 K1 102.77(15) . . . . ?
C41 Si1 N5 K2 105.0(3) . . . . ?
C43 Si1 N5 K2 -129.3(3) . . . . ?
C42 Si1 N5 K2 -12.7(3) . . . . ?
K1 Si1 N5 K2 -102.77(15) . . . . ?
C78 Si4 N6 Si3 -94.4(3) . . . . ?
C80 Si4 N6 Si3 146.0(3) . . . . ?
C79 Si4 N6 Si3 28.9(4) . . . . ?
K4 Si4 N6 Si3 126.7(3) 1_545 . . . ?
K3 Si4 N6 Si3 -130.2(3) . . . . ?
C78 Si4 N6 K4 138.8(2) . . . 1_545 ?
C80 Si4 N6 K4 19.2(3) . . . 1_545 ?
C79 Si4 N6 K4 -97.9(2) . . . 1_545 ?
K3 Si4 N6 K4 103.01(16) . . . 1_545 ?
C78 Si4 N6 K3 35.8(3) . . . . ?
C80 Si4 N6 K3 -83.8(2) . . . . ?
C79 Si4 N6 K3 159.1(2) . . . . ?
K4 Si4 N6 K3 -103.01(16) 1_545 . . . ?
C75 Si3 N6 Si4 -121.9(5) . . . . ?
C76 Si3 N6 Si4 0.2(4) . . . . ?
C77 Si3 N6 Si4 121.6(4) . . . . ?
K4 Si3 N6 Si4 -126.5(3) 1_545 . . . ?
K3 Si3 N6 Si4 133.1(3) . . . . ?
C75 Si3 N6 K4 4.6(5) . . . 1_545 ?
C76 Si3 N6 K4 126.7(2) . . . 1_545 ?
C77 Si3 N6 K4 -112.0(3) . . . 1_545 ?
K3 Si3 N6 K4 -100.45(14) . . . 1_545 ?
C75 Si3 N6 K3 105.0(5) . . . . ?
C76 Si3 N6 K3 -132.9(2) . . . . ?
C77 Si3 N6 K3 -11.5(3) . . . . ?
K4 Si3 N6 K3 100.45(14) 1_545 . . . ?
C28 N1 C1 N2 18.1(7) . . . . ?
K1 N1 C1 N2 -155.8(3) . . . . ?
C28 N1 C1 N3 -166.5(3) . . . . ?
K1 N1 C1 N3 19.6(5) . . . . ?
C2 N2 C1 N1 173.4(4) . . . . ?
C4 N2 C1 N1 -4.2(7) . . . . ?
C2 N2 C1 N3 -2.4(4) . . . . ?
C4 N2 C1 N3 179.9(3) . . . . ?
C3 N3 C1 N1 -173.6(3) . . . . ?
C16 N3 C1 N1 0.3(5) . . . . ?
C3 N3 C1 N2 3.2(4) . . . . ?
C16 N3 C1 N2 177.1(3) . . . . ?
C1 N2 C2 C3 0.9(4) . . . . ?
C4 N2 C2 C3 178.7(3) . . . . ?
N2 C2 C3 N3 1.2(4) . . . . ?
C1 N3 C3 C2 -2.8(4) . . . . ?
C16 N3 C3 C2 -176.4(4) . . . . ?
C1 N2 C4 C5 70.3(5) . . . . ?
C2 N2 C4 C5 -107.2(4) . . . . ?
C1 N2 C4 C9 -111.5(4) . . . . ?
C2 N2 C4 C9 71.0(4) . . . . ?
C9 C4 C5 C6 4.4(6) . . . . ?
N2 C4 C5 C6 -177.6(3) . . . . ?
C9 C4 C5 C13 -174.9(4) . . . . ?
N2 C4 C5 C13 3.2(5) . . . . ?
C4 C5 C6 C7 -2.4(6) . . . . ?
C13 C5 C6 C7 176.9(4) . . . . ?
C5 C6 C7 C8 -0.5(7) . . . . ?
C6 C7 C8 C9 1.7(7) . . . . ?
C5 C4 C9 C8 -3.3(5) . . . . ?
N2 C4 C9 C8 178.6(3) . . . . ?
C5 C4 C9 C10 178.9(3) . . . . ?
N2 C4 C9 C10 0.8(5) . . . . ?
C7 C8 C9 C4 0.2(6) . . . . ?
C7 C8 C9 C10 178.0(4) . . . . ?
C4 C9 C10 C11 -149.0(5) . . . . ?
C8 C9 C10 C11 33.3(6) . . . . ?
C4 C9 C10 C12 85.2(5) . . . . ?
C8 C9 C10 C12 -92.5(5) . . . . ?
C4 C5 C13 C14 -163.3(4) . . . . ?
C6 C5 C13 C14 17.5(6) . . . . ?
C4 C5 C13 C15 72.8(5) . . . . ?
C6 C5 C13 C15 -106.4(5) . . . . ?
C3 N3 C16 C17 69.2(5) . . . . ?
C1 N3 C16 C17 -103.8(4) . . . . ?
C3 N3 C16 C21 -110.9(4) . . . . ?
C1 N3 C16 C21 76.1(4) . . . . ?
C3 N3 C16 K1 161.8(3) . . . . ?
C1 N3 C16 K1 -11.1(4) . . . . ?
C21 C16 C17 C18 0.1(6) . . . . ?
N3 C16 C17 C18 180.0(4) . . . . ?
K1 C16 C17 C18 75.0(4) . . . . ?
C21 C16 C17 C22 -176.9(3) . . . . ?
N3 C16 C17 C22 3.0(5) . . . . ?
K1 C16 C17 C22 -101.9(3) . . . . ?
C16 C17 C18 C19 -0.5(7) . . . . ?
C22 C17 C18 C19 176.5(4) . . . . ?
C17 C18 C19 C20 1.0(8) . . . . ?
C18 C19 C20 C21 -1.0(7) . . . . ?
C19 C20 C21 C16 0.6(6) . . . . ?
C19 C20 C21 C25 179.7(4) . . . . ?
C19 C20 C21 K1 -71.3(4) . . . . ?
C17 C16 C21 C20 -0.1(5) . . . . ?
N3 C16 C21 C20 180.0(3) . . . . ?
K1 C16 C21 C20 -77.4(3) . . . . ?
C17 C16 C21 C25 -179.2(3) . . . . ?
N3 C16 C21 C25 0.9(5) . . . . ?
K1 C16 C21 C25 103.5(3) . . . . ?
C17 C16 C21 K1 77.3(3) . . . . ?
N3 C16 C21 K1 -102.6(3) . . . . ?
C16 C17 C22 C24 101.8(5) . . . . ?
C18 C17 C22 C24 -75.1(5) . . . . ?
C16 C17 C22 C23 -132.5(5) . . . . ?
C18 C17 C22 C23 50.6(6) . . . . ?
C20 C21 C25 C27 21.7(5) . . . . ?
C16 C21 C25 C27 -159.3(3) . . . . ?
K1 C21 C25 C27 -74.5(3) . . . . ?
C20 C21 C25 C26 -103.0(4) . . . . ?
C16 C21 C25 C26 76.0(4) . . . . ?
K1 C21 C25 C26 160.8(3) . . . . ?
K3 O1 C28 N4 -6.4(7) . . . . ?
K3 O1 C28 N1 168.3(2) . . . . ?
K3 O1 C28 K1 89.4(9) . . . . ?
C29 N4 C28 O1 -7.7(6) . . . . ?
K1 N4 C28 O1 161.9(3) . . . . ?
C29 N4 C28 N1 177.2(3) . . . . ?
K1 N4 C28 N1 -13.3(3) . . . . ?
C29 N4 C28 K1 -169.5(4) . . . . ?
C1 N1 C28 O1 21.8(6) . . . . ?
K1 N1 C28 O1 -162.3(3) . . . . ?
C1 N1 C28 N4 -162.7(3) . . . . ?
K1 N1 C28 N4 13.2(3) . . . . ?
C1 N1 C28 K1 -175.9(4) . . . . ?
C28 N4 C29 C34 121.6(5) . . . . ?
K1 N4 C29 C34 -42.0(7) . . . . ?
C28 N4 C29 C30 -63.6(5) . . . . ?
K1 N4 C29 C30 132.8(4) . . . . ?
C28 N4 C29 K3 11.0(4) . . . . ?
K1 N4 C29 K3 -152.6(3) . . . . ?
C34 C29 C30 C31 2.0(7) . . . . ?
N4 C29 C30 C31 -172.9(4) . . . . ?
K3 C29 C30 C31 94.1(5) . . . . ?
C34 C29 C30 K3 -92.1(4) . . . . ?
N4 C29 C30 K3 93.0(4) . . . . ?
C29 C30 C31 C32 -0.1(8) . . . . ?
K3 C30 C31 C32 88.5(5) . . . . ?
C30 C31 C32 C33 -3.6(9) . . . . ?
C31 C32 C33 C34 5.4(10) . . . . ?
C30 C29 C34 C33 -0.2(8) . . . . ?
N4 C29 C34 C33 174.7(5) . . . . ?
K3 C29 C34 C33 -73.6(6) . . . . ?
C30 C29 C34 K2 -98.3(4) . . . . ?
N4 C29 C34 K2 76.7(4) . . . . ?
K3 C29 C34 K2 -171.62(10) . . . . ?
C32 C33 C34 C29 -3.5(9) . . . . ?
C32 C33 C34 K2 92.6(6) . . . . ?
C74 C35 C36 C37 0.8(7) . . . . ?
C35 C36 C37 C72 -2.2(7) . . . . ?
C35 C36 C37 K2 -114.5(4) . . . . ?
C71 N7 C44 N8 -168.9(3) . . . . ?
K4 N7 C44 N8 25.1(6) . . . . ?
C71 N7 C44 N9 16.7(7) . . . . ?
K4 N7 C44 N9 -149.4(4) . . . . ?
C45 N8 C44 N7 -172.6(4) . . . . ?
C59 N8 C44 N7 1.2(6) . . . . ?
C45 N8 C44 N9 3.4(4) . . . . ?
C59 N8 C44 N9 177.2(3) . . . . ?
C46 N9 C44 N7 172.1(5) . . . . ?
C47 N9 C44 N7 -9.2(7) . . . . ?
C46 N9 C44 N8 -2.9(4) . . . . ?
C47 N9 C44 N8 175.8(4) . . . . ?
C44 N8 C45 C46 -2.7(5) . . . . ?
C59 N8 C45 C46 -176.3(4) . . . . ?
N8 C45 C46 N9 0.8(5) . . . . ?
C44 N9 C46 C45 1.4(5) . . . . ?
C47 N9 C46 C45 -177.4(4) . . . . ?
C44 N9 C47 C52 -111.0(4) . . . . ?
C46 N9 C47 C52 67.5(5) . . . . ?
C44 N9 C47 C48 70.9(5) . . . . ?
C46 N9 C47 C48 -110.6(4) . . . . ?
C52 C47 C48 C49 -0.1(6) . . . . ?
N9 C47 C48 C49 177.8(3) . . . . ?
C52 C47 C48 C57 -179.0(4) . . . . ?
N9 C47 C48 C57 -1.1(6) . . . . ?
C47 C48 C49 C50 -0.2(7) . . . . ?
C57 C48 C49 C50 178.7(5) . . . . ?
C48 C49 C50 C51 -0.5(8) . . . . ?
C49 C50 C51 C52 1.6(8) . . . . ?
C48 C47 C52 C51 1.1(6) . . . . ?
N9 C47 C52 C51 -176.9(4) . . . . ?
C48 C47 C52 C53 -176.2(4) . . . . ?
N9 C47 C52 C53 5.8(6) . . . . ?
C50 C51 C52 C47 -1.8(7) . . . . ?
C50 C51 C52 C53 175.6(5) . . . . ?
C47 C52 C53 C54 98.4(6) . . . . ?
C51 C52 C53 C54 -78.9(6) . . . . ?
C47 C52 C53 C55 -135.4(6) . . . . ?
C51 C52 C53 C55 47.3(7) . . . . ?
C49 C48 C57 C58 19(4) . . . . ?
C47 C48 C57 C58 -163(4) . . . . ?
C49 C48 C57 C56 -95.6(5) . . . . ?
C47 C48 C57 C56 83.2(5) . . . . ?
C49 C48 C57 C58A 37.4(17) . . . . ?
C47 C48 C57 C58A -143.7(16) . . . . ?
C44 N8 C59 C64 -103.7(4) . . . . ?
C45 N8 C59 C64 69.1(5) . . . . ?
C44 N8 C59 C60 75.1(5) . . . . ?
C45 N8 C59 C60 -112.1(4) . . . . ?
C44 N8 C59 K4 -15.1(4) . . . . ?
C45 N8 C59 K4 157.7(3) . . . . ?
C64 C59 C60 C61 -1.1(5) . . . . ?
N8 C59 C60 C61 -179.8(3) . . . . ?
K4 C59 C60 C61 -78.2(3) . . . . ?
C64 C59 C60 C68 179.1(3) . . . . ?
N8 C59 C60 C68 0.4(5) . . . . ?
K4 C59 C60 C68 102.0(3) . . . . ?
C59 C60 C61 C62 -0.1(6) . . . . ?
C68 C60 C61 C62 179.7(4) . . . . ?
C60 C61 C62 C63 1.3(7) . . . . ?
C61 C62 C63 C64 -1.4(7) . . . . ?
C62 C63 C64 C59 0.3(7) . . . . ?
C62 C63 C64 C65 176.9(4) . . . . ?
C62 C63 C64 K4 71.3(4) . . . . ?
C60 C59 C64 C63 1.0(6) . . . . ?
N8 C59 C64 C63 179.7(3) . . . . ?
K4 C59 C64 C63 78.9(4) . . . . ?
C60 C59 C64 C65 -175.6(4) . . . . ?
N8 C59 C64 C65 3.1(5) . . . . ?
K4 C59 C64 C65 -97.7(3) . . . . ?
C60 C59 C64 K4 -77.9(3) . . . . ?
N8 C59 C64 K4 100.8(3) . . . . ?
C63 C64 C65 C67 -89.4(5) . . . . ?
C59 C64 C65 C67 87.1(5) . . . . ?
K4 C64 C65 C67 6.8(4) . . . . ?
C63 C64 C65 C66 33.9(6) . . . . ?
C59 C64 C65 C66 -149.5(4) . . . . ?
K4 C64 C65 C66 130.1(4) . . . . ?
C61 C60 C68 C70 -108.6(5) . . . . ?
C59 C60 C68 C70 71.1(5) . . . . ?
C61 C60 C68 C69 16.1(5) . . . . ?
C59 C60 C68 C69 -164.1(4) . . . . ?
K2 O2 C71 N10 2.9(8) . . . . ?
K2 O2 C71 N7 -179.8(3) . . . . ?
K2 O2 C71 K4 107.0(7) . . . . ?
C72 N10 C71 O2 4.9(6) . . . . ?
K4 N10 C71 O2 157.5(4) . . . . ?
C72 N10 C71 N7 -172.7(3) . . . . ?
K4 N10 C71 N7 -20.1(3) . . . . ?
C72 N10 C71 K4 -152.6(4) . . . . ?
C44 N7 C71 O2 32.4(6) . . . . ?
K4 N7 C71 O2 -157.4(3) . . . . ?
C44 N7 C71 N10 -149.8(4) . . . . ?
K4 N7 C71 N10 20.4(3) . . . . ?
C44 N7 C71 K4 -170.2(4) . . . . ?
C71 N10 C72 C37 47.6(5) . . . . ?
K4 N10 C72 C37 -92.8(5) . . . . ?
C71 N10 C72 C73 -139.7(4) . . . . ?
K4 N10 C72 C73 79.8(5) . . . . ?
C36 C37 C72 N10 175.4(4) . . . . ?
K2 C37 C72 N10 -73.7(4) . . . . ?
C36 C37 C72 C73 2.5(6) . . . . ?
K2 C37 C72 C73 113.5(3) . . . . ?
N10 C72 C73 C74 -174.9(4) . . . . ?
C37 C72 C73 C74 -1.7(6) . . . . ?
N10 C72 C73 K3 -66.9(4) . . . 1_565 ?
C37 C72 C73 K3 106.3(3) . . . 1_565 ?
C36 C35 C74 C73 0.1(7) . . . . ?
C72 C73 C74 C35 0.4(7) . . . . ?
K3 C73 C74 C35 -112.9(4) 1_565 . . . ?
N6 Si4 C80 K4 -15.5(2) . . . 1_545 ?
C78 Si4 C80 K4 -140.26(19) . . . 1_545 ?
C79 Si4 C80 K4 108.4(2) . . . 1_545 ?
K3 Si4 C80 K4 -61.23(11) . . . 1_545 ?
N6 Si3 C75 K4 -3.7(4) . . . 1_545 ?
C76 Si3 C75 K4 -133.7(2) . . . 1_545 ?
C77 Si3 C75 K4 116.8(3) . . . 1_545 ?
K3 Si3 C75 K4 52.4(4) . . . 1_545 ?

_refine_diff_density_max         0.735
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.078

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_3a
_database_code_depnum_ccdc_archive 'CCDC 1046054'
_audit_update_record             
;
2015-03-02 deposited with the CCDC.
2015-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C66 H98 Li2 N8 O4, 2(C18 H26 N4 O)'
_chemical_formula_sum            'C102 H150 Li2 N16 O6'
_chemical_formula_weight         1710.26

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 '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      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 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, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   16.8744(6)
_cell_length_b                   14.2505(6)
_cell_length_c                   23.1944(13)
_cell_angle_alpha                90
_cell_angle_beta                 114.678(4)
_cell_angle_gamma                90
_cell_volume                     5068.1(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6473
_cell_measurement_theta_min      3.0979
_cell_measurement_theta_max      70.8318

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_F_000             1856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_absorpt_coefficient_mu    0.547
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.74586
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27'

_exptl_special_details           
;
 'Empirical absorption correction using spherical harmonics,implemented in SCALE3 ABSPACK scaling algorithm.'
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22833
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.101
_diffrn_reflns_theta_max         70.994
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             9435
_reflns_number_gt                6652
_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       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP III & Olex 2.1'
_computing_publication_material  WinGX

_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)+(0.0071P)²+21.8065P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9435
_refine_ls_number_parameters     587
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_gt           0.0826
_refine_ls_wR_factor_ref         0.2410
_refine_ls_wR_factor_gt          0.2408
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_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
Li1 Li 0.5806(5) 0.7453(7) 0.2643(4) 0.039(2) Uani 1 1 d . . . . .
N1 N 0.8736(3) 0.7385(3) 0.3996(2) 0.0370(10) Uani 1 1 d . . . . .
N2 N 0.8631(3) 0.5861(3) 0.38540(19) 0.0352(10) Uani 1 1 d . . . . .
N3 N 0.8323(3) 0.6779(3) 0.29175(19) 0.0333(9) Uani 1 1 d . . . . .
N4 N 0.7314(3) 0.7045(3) 0.1893(2) 0.0394(11) Uani 1 1 d . . . . .
H8 H 0.6779 0.7186 0.1658 0.047 Uiso 1 1 d R U . . .
N5 N 0.2201(3) 0.7525(3) 0.89444(19) 0.0333(9) Uani 1 1 d . . . . .
N6 N 0.2133(3) 0.9050(3) 0.9037(2) 0.0347(10) Uani 1 1 d . . . . .
N7 N 0.0826(3) 0.8308(3) 0.82937(19) 0.0349(10) Uani 1 1 d . . . . .
N8 N -0.0624(3) 0.8260(3) 0.8072(2) 0.0374(10) Uani 1 1 d . . . . .
H4 H -0.0687 0.8328 0.7687 0.045 Uiso 1 1 d R U . . .
O1 O 0.6892(2) 0.7159(3) 0.26946(17) 0.0417(9) Uani 1 1 d . . . . .
O2 O 0.5194(2) 0.7541(3) 0.31492(16) 0.0377(8) Uani 1 1 d . . . . .
O3 O 0.0384(2) 0.7972(3) 0.90885(16) 0.0422(9) Uani 1 1 d . . . . .
C1 C 0.8515(3) 0.6699(4) 0.3546(2) 0.0327(11) Uani 1 1 d . . . . .
C2 C 0.8982(4) 0.6963(4) 0.4584(2) 0.0449(14) Uani 1 1 d . . . . .
H50 H 0.9158 0.7271 0.4972 0.054 Uiso 1 1 calc R U . . .
C3 C 0.8922(4) 0.6038(4) 0.4495(3) 0.0480(15) Uani 1 1 d . . . . .
H48 H 0.9053 0.5587 0.4811 0.058 Uiso 1 1 calc R U . . .
C4 C 0.8561(4) 0.4900(4) 0.3571(3) 0.0424(13) Uani 1 1 d . . . . .
C5 C 0.7720(4) 0.4803(4) 0.2967(3) 0.0485(15) Uani 1 1 d . . . . .
H30A H 0.7768 0.5161 0.2632 0.073 Uiso 1 1 calc R U . . .
H30B H 0.7238 0.5033 0.3043 0.073 Uiso 1 1 calc R U . . .
H30C H 0.7625 0.4155 0.2845 0.073 Uiso 1 1 calc R U . . .
C6 C 0.9357(4) 0.4750(5) 0.3429(3) 0.0625(19) Uani 1 1 d . . . . .
H58A H 0.9878 0.4836 0.3811 0.094 Uiso 1 1 calc R U . . .
H58B H 0.9347 0.5195 0.3116 0.094 Uiso 1 1 calc R U . . .
H58C H 0.9346 0.4125 0.3272 0.094 Uiso 1 1 calc R U . . .
C7 C 0.8538(6) 0.4187(5) 0.4053(3) 0.074(2) Uani 1 1 d . . . . .
H63A H 0.8081 0.4347 0.4178 0.111 Uiso 1 1 calc R U . . .
H63B H 0.9088 0.4191 0.4418 0.111 Uiso 1 1 calc R U . . .
H63C H 0.8432 0.3573 0.3866 0.111 Uiso 1 1 calc R U . . .
C8 C 0.8657(4) 0.8437(4) 0.3920(3) 0.0425(13) Uani 1 1 d . . . . .
C9 C 0.8692(5) 0.8764(5) 0.3306(3) 0.0632(19) Uani 1 1 d . . . . .
H37A H 0.9190 0.8491 0.3270 0.095 Uiso 1 1 calc R U . . .
H37B H 0.8738 0.9435 0.3309 0.095 Uiso 1 1 calc R U . . .
H37C H 0.8170 0.8571 0.2952 0.095 Uiso 1 1 calc R U . . .
C10 C 0.7802(4) 0.8722(5) 0.3946(4) 0.072(2) Uani 1 1 d . . . . .
H54A H 0.7745 0.9393 0.3918 0.107 Uiso 1 1 calc R U . . .
H54B H 0.7801 0.8513 0.4339 0.107 Uiso 1 1 calc R U . . .
H54C H 0.7323 0.8440 0.3598 0.107 Uiso 1 1 calc R U . . .
C11 C 0.9428(4) 0.8868(4) 0.4479(3) 0.0500(15) Uani 1 1 d . . . . .
H9A H 0.9964 0.8610 0.4496 0.075 Uiso 1 1 calc R U . . .
H9B H 0.9377 0.8729 0.4867 0.075 Uiso 1 1 calc R U . . .
H9C H 0.9428 0.9536 0.4425 0.075 Uiso 1 1 calc R U . . .
C12 C 0.7518(3) 0.6999(4) 0.2540(2) 0.0350(11) Uani 1 1 d . . . . .
C13 C 0.7834(3) 0.6899(4) 0.1557(2) 0.0354(11) Uani 1 1 d . . . . .
C14 C 0.7413(3) 0.6713(4) 0.0912(2) 0.0391(12) Uani 1 1 d . . . . .
H21 H 0.6809 0.6648 0.0725 0.047 Uiso 1 1 calc R U . . .
C15 C 0.7874(4) 0.6622(4) 0.0544(3) 0.0454(14) Uani 1 1 d . . . . .
H7 H 0.7577 0.6502 0.0112 0.055 Uiso 1 1 calc R U . . .
C16 C 0.8769(4) 0.6708(4) 0.0810(3) 0.0467(14) Uani 1 1 d . . . . .
H38 H 0.9080 0.6654 0.0562 0.056 Uiso 1 1 calc R U . . .
C17 C 0.9193(4) 0.6877(5) 0.1453(3) 0.0492(15) Uani 1 1 d . . . . .
H46 H 0.9798 0.6925 0.1640 0.059 Uiso 1 1 calc R U . . .
C18 C 0.8738(4) 0.6978(4) 0.1826(3) 0.0446(14) Uani 1 1 d . . . . .
H40 H 0.9037 0.7099 0.2257 0.054 Uiso 1 1 calc R U . . .
C19 C 0.5083(3) 0.7549(4) 0.3688(2) 0.0353(12) Uani 1 1 d . . . . .
C20 C 0.5149(3) 0.6701(4) 0.4032(2) 0.0375(12) Uani 1 1 d . . . . .
C21 C 0.4987(3) 0.6733(4) 0.4580(2) 0.0395(12) Uani 1 1 d . . . . .
H12 H 0.5026 0.6180 0.4803 0.047 Uiso 1 1 calc R U . . .
C22 C 0.4773(3) 0.7551(4) 0.4801(2) 0.0392(13) Uani 1 1 d . . . . .
C23 C 0.4722(3) 0.8366(4) 0.4467(3) 0.0411(13) Uani 1 1 d . . . . .
H22 H 0.4583 0.8921 0.4614 0.049 Uiso 1 1 calc R U . . .
C24 C 0.4868(3) 0.8398(4) 0.3918(2) 0.0371(12) Uani 1 1 d . . . . .
C25 C 0.5392(4) 0.5764(4) 0.3823(3) 0.0451(14) Uani 1 1 d . . . . .
C26 C 0.6279(4) 0.5836(5) 0.3783(3) 0.0616(19) Uani 1 1 d . . . . .
H39A H 0.6429 0.5237 0.3667 0.092 Uiso 1 1 calc R U . . .
H39B H 0.6719 0.6022 0.4188 0.092 Uiso 1 1 calc R U . . .
H39C H 0.6241 0.6294 0.3469 0.092 Uiso 1 1 calc R U . . .
C27 C 0.5474(5) 0.4962(5) 0.4284(3) 0.068(2) Uani 1 1 d . . . . .
H41A H 0.5620 0.4392 0.4129 0.102 Uiso 1 1 calc R U . . .
H41B H 0.4930 0.4882 0.4317 0.102 Uiso 1 1 calc R U . . .
H41C H 0.5924 0.5108 0.4694 0.102 Uiso 1 1 calc R U . . .
C28 C 0.4603(4) 0.7557(5) 0.5396(3) 0.0501(15) Uani 1 1 d . . . . .
H11A H 0.5144 0.7480 0.5763 0.075 Uiso 1 1 calc R U . . .
H11B H 0.4215 0.7052 0.5376 0.075 Uiso 1 1 calc R U . . .
H11C H 0.4341 0.8144 0.5424 0.075 Uiso 1 1 calc R U . . .
C29 C 0.4812(4) 0.9343(4) 0.3583(3) 0.0443(14) Uani 1 1 d . . . . .
C30 C 0.5721(4) 0.9600(5) 0.3625(3) 0.0563(17) Uani 1 1 d . . . . .
H34A H 0.5945 0.9086 0.3470 0.084 Uiso 1 1 calc R U . . .
H34B H 0.6107 0.9724 0.4059 0.084 Uiso 1 1 calc R U . . .
H34C H 0.5677 1.0148 0.3373 0.084 Uiso 1 1 calc R U . . .
C31 C 0.4145(4) 0.9315(4) 0.2884(3) 0.0487(14) Uani 1 1 d . . . . .
H35A H 0.3612 0.9037 0.2857 0.073 Uiso 1 1 calc R U . . .
H35B H 0.4375 0.8948 0.2642 0.073 Uiso 1 1 calc R U . . .
H35C H 0.4032 0.9942 0.2718 0.073 Uiso 1 1 calc R U . . .
C32 C 0.4519(5) 1.0149(5) 0.3889(3) 0.065(2) Uani 1 1 d . . . . .
H3A H 0.4911 1.0197 0.4330 0.098 Uiso 1 1 calc R U . . .
H3B H 0.3940 1.0026 0.3852 0.098 Uiso 1 1 calc R U . . .
H3C H 0.4522 1.0727 0.3678 0.098 Uiso 1 1 calc R U . . .
C33 C 0.1660(3) 0.8283(4) 0.8738(2) 0.0315(11) Uani 1 1 d . . . . .
C34 C 0.2956(3) 0.8762(4) 0.9443(3) 0.0414(13) Uani 1 1 d . . . . .
H26 H 0.3405 0.9147 0.9708 0.050 Uiso 1 1 calc R U . . .
C35 C 0.2997(3) 0.7839(4) 0.9389(3) 0.0409(13) Uani 1 1 d . . . . .
H14 H 0.3480 0.7466 0.9613 0.049 Uiso 1 1 calc R U . . .
C36 C 0.2010(3) 0.6502(4) 0.8792(2) 0.0376(12) Uani 1 1 d . . . . .
C37 C 0.1253(4) 0.6348(4) 0.8143(3) 0.0522(15) Uani 1 1 d . . . . .
H2A H 0.1378 0.6658 0.7823 0.078 Uiso 1 1 calc R U . . .
H2B H 0.0728 0.6603 0.8146 0.078 Uiso 1 1 calc R U . . .
H2C H 0.1179 0.5689 0.8053 0.078 Uiso 1 1 calc R U . . .
C38 C 0.2827(4) 0.6049(5) 0.8782(3) 0.0598(18) Uani 1 1 d . . . . .
H32A H 0.3290 0.6063 0.9201 0.090 Uiso 1 1 calc R U . . .
H32B H 0.3001 0.6391 0.8497 0.090 Uiso 1 1 calc R U . . .
H32C H 0.2702 0.5411 0.8641 0.090 Uiso 1 1 calc R U . . .
C39 C 0.1787(5) 0.6079(4) 0.9306(3) 0.0574(17) Uani 1 1 d . . . . .
H55A H 0.1268 0.6369 0.9296 0.086 Uiso 1 1 calc R U . . .
H55B H 0.2260 0.6182 0.9713 0.086 Uiso 1 1 calc R U . . .
H55C H 0.1690 0.5417 0.9234 0.086 Uiso 1 1 calc R U . . .
C40 C 0.1829(4) 1.0055(4) 0.8909(3) 0.0419(13) Uani 1 1 d . . . . .
C41 C 0.0999(4) 1.0197(5) 0.9006(4) 0.068(2) Uani 1 1 d . . . . .
H19A H 0.1079 0.9949 0.9412 0.102 Uiso 1 1 calc R U . . .
H19B H 0.0524 0.9877 0.8677 0.102 Uiso 1 1 calc R U . . .
H19C H 0.0870 1.0855 0.8991 0.102 Uiso 1 1 calc R U . . .
C42 C 0.1691(5) 1.0301(5) 0.8236(3) 0.0637(19) Uani 1 1 d . . . . .
H51A H 0.1229 0.9922 0.7941 0.096 Uiso 1 1 calc R U . . .
H51B H 0.2219 1.0183 0.8185 0.096 Uiso 1 1 calc R U . . .
H51C H 0.1538 1.0952 0.8157 0.096 Uiso 1 1 calc R U . . .
C43 C 0.2528(4) 1.0685(5) 0.9380(3) 0.0634(18) Uani 1 1 d . . . . .
H31A H 0.3052 1.0637 0.9315 0.095 Uiso 1 1 calc R U . . .
H31B H 0.2645 1.0493 0.9805 0.095 Uiso 1 1 calc R U . . .
H31C H 0.2328 1.1324 0.9318 0.095 Uiso 1 1 calc R U . . .
C44 C 0.0221(3) 0.8164(4) 0.8526(2) 0.0351(11) Uani 1 1 d . . . . .
C45 C -0.1392(3) 0.8259(4) 0.8169(2) 0.0353(11) Uani 1 1 d . . . . .
C46 C -0.1400(4) 0.8371(4) 0.8765(3) 0.0438(13) Uani 1 1 d . . . . .
H43 H -0.0881 0.8448 0.9124 0.053 Uiso 1 1 calc R U . . .
C47 C -0.2196(4) 0.8368(5) 0.8815(3) 0.0546(16) Uani 1 1 d . . . . .
H49 H -0.2201 0.8446 0.9212 0.066 Uiso 1 1 calc R U . . .
C48 C -0.2979(4) 0.8252(5) 0.8289(4) 0.0608(18) Uani 1 1 d . . . . .
H25 H -0.3503 0.8238 0.8331 0.073 Uiso 1 1 calc R U . . .
C49 C -0.2965(4) 0.8157(5) 0.7702(3) 0.0571(17) Uani 1 1 d . . . . .
H53 H -0.3486 0.8086 0.7343 0.068 Uiso 1 1 calc R U . . .
C50 C -0.2180(3) 0.8167(4) 0.7641(3) 0.0463(14) Uani 1 1 d . . . . .
H61 H -0.2183 0.8112 0.7241 0.056 Uiso 1 1 calc R U . . .
C57 C 0.4671(4) 0.5458(5) 0.3176(3) 0.0593(17) Uani 1 1 d . . . . .
H57A H 0.4823 0.4863 0.3055 0.089 Uiso 1 1 calc R U . . .
H57B H 0.4616 0.5919 0.2860 0.089 Uiso 1 1 calc R U . . .
H57C H 0.4126 0.5401 0.3212 0.089 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
Li1 O1 1.835(9) . ?
Li1 O2 1.863(9) . ?
Li1 O2 1.911(8) 2_655 ?
Li1 Li1 2.516(16) 2_655 ?
N1 C1 1.363(6) . ?
N1 C2 1.386(7) . ?
N1 C8 1.509(7) . ?
N2 C1 1.362(7) . ?
N2 C3 1.380(7) . ?
N2 C4 1.503(7) . ?
N3 C12 1.310(6) . ?
N3 C1 1.360(6) . ?
N4 C12 1.394(6) . ?
N4 C13 1.413(6) . ?
N4 H8 0.8599 . ?
N5 C33 1.366(6) . ?
N5 C35 1.383(7) . ?
N5 C36 1.503(7) . ?
N6 C33 1.361(6) . ?
N6 C34 1.375(7) . ?
N6 C40 1.507(7) . ?
N7 C33 1.354(6) . ?
N7 C44 1.355(6) . ?
N8 C44 1.380(6) . ?
N8 C45 1.405(6) . ?
N8 H4 0.8600 . ?
O1 C12 1.270(6) . ?
O2 C19 1.339(6) . ?
O2 Li1 1.911(8) 2_655 ?
O3 C44 1.246(6) . ?
C2 C3 1.332(8) . ?
C2 H50 0.9300 . ?
C3 H48 0.9300 . ?
C4 C7 1.522(8) . ?
C4 C6 1.525(8) . ?
C4 C5 1.528(8) . ?
C5 H30A 0.9600 . ?
C5 H30B 0.9600 . ?
C5 H30C 0.9600 . ?
C6 H58A 0.9600 . ?
C6 H58B 0.9600 . ?
C6 H58C 0.9600 . ?
C7 H63A 0.9600 . ?
C7 H63B 0.9600 . ?
C7 H63C 0.9600 . ?
C8 C9 1.522(8) . ?
C8 C10 1.525(8) . ?
C8 C11 1.531(8) . ?
C9 H37A 0.9600 . ?
C9 H37B 0.9600 . ?
C9 H37C 0.9600 . ?
C10 H54A 0.9600 . ?
C10 H54B 0.9600 . ?
C10 H54C 0.9600 . ?
C11 H9A 0.9600 . ?
C11 H9B 0.9600 . ?
C11 H9C 0.9600 . ?
C13 C14 1.387(7) . ?
C13 C18 1.390(7) . ?
C14 C15 1.381(7) . ?
C14 H21 0.9300 . ?
C15 C16 1.378(8) . ?
C15 H7 0.9300 . ?
C16 C17 1.380(8) . ?
C16 H38 0.9300 . ?
C17 C18 1.383(7) . ?
C17 H46 0.9300 . ?
C18 H40 0.9300 . ?
C19 C20 1.427(8) . ?
C19 C24 1.428(8) . ?
C20 C21 1.409(7) . ?
C20 C25 1.533(8) . ?
C21 C22 1.381(8) . ?
C21 H12 0.9300 . ?
C22 C23 1.378(8) . ?
C22 C28 1.522(7) . ?
C23 C24 1.396(7) . ?
C23 H22 0.9300 . ?
C24 C29 1.538(8) . ?
C25 C27 1.531(8) . ?
C25 C26 1.541(8) . ?
C25 C57 1.549(8) . ?
C26 H39A 0.9600 . ?
C26 H39B 0.9600 . ?
C26 H39C 0.9600 . ?
C27 H41A 0.9600 . ?
C27 H41B 0.9600 . ?
C27 H41C 0.9600 . ?
C28 H11A 0.9600 . ?
C28 H11B 0.9600 . ?
C28 H11C 0.9600 . ?
C29 C32 1.537(8) . ?
C29 C30 1.539(8) . ?
C29 C31 1.540(8) . ?
C30 H34A 0.9600 . ?
C30 H34B 0.9600 . ?
C30 H34C 0.9600 . ?
C31 H35A 0.9600 . ?
C31 H35B 0.9600 . ?
C31 H35C 0.9600 . ?
C32 H3A 0.9600 . ?
C32 H3B 0.9600 . ?
C32 H3C 0.9600 . ?
C34 C35 1.325(8) . ?
C34 H26 0.9300 . ?
C35 H14 0.9300 . ?
C36 C39 1.517(7) . ?
C36 C37 1.530(8) . ?
C36 C38 1.531(7) . ?
C37 H2A 0.9600 . ?
C37 H2B 0.9600 . ?
C37 H2C 0.9600 . ?
C38 H32A 0.9600 . ?
C38 H32B 0.9600 . ?
C38 H32C 0.9600 . ?
C39 H55A 0.9600 . ?
C39 H55B 0.9600 . ?
C39 H55C 0.9600 . ?
C40 C42 1.520(8) . ?
C40 C43 1.522(8) . ?
C40 C41 1.523(8) . ?
C41 H19A 0.9600 . ?
C41 H19B 0.9600 . ?
C41 H19C 0.9600 . ?
C42 H51A 0.9600 . ?
C42 H51B 0.9600 . ?
C42 H51C 0.9600 . ?
C43 H31A 0.9600 . ?
C43 H31B 0.9600 . ?
C43 H31C 0.9600 . ?
C45 C50 1.387(8) . ?
C45 C46 1.397(7) . ?
C46 C47 1.397(8) . ?
C46 H43 0.9300 . ?
C47 C48 1.384(9) . ?
C47 H49 0.9300 . ?
C48 C49 1.379(9) . ?
C48 H25 0.9300 . ?
C49 C50 1.390(8) . ?
C49 H53 0.9300 . ?
C50 H61 0.9300 . ?
C57 H57A 0.9600 . ?
C57 H57B 0.9600 . ?
C57 H57C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Li1 O2 140.9(5) . . ?
O1 Li1 O2 122.3(5) . 2_655 ?
O2 Li1 O2 95.9(4) . 2_655 ?
O1 Li1 Li1 163.2(5) . 2_655 ?
O2 Li1 Li1 49.0(3) . 2_655 ?
O2 Li1 Li1 47.4(3) 2_655 2_655 ?
C1 N1 C2 108.5(4) . . ?
C1 N1 C8 129.8(4) . . ?
C2 N1 C8 121.4(4) . . ?
C1 N2 C3 108.3(4) . . ?
C1 N2 C4 127.0(4) . . ?
C3 N2 C4 124.4(5) . . ?
C12 N3 C1 117.0(4) . . ?
C12 N4 C13 131.0(4) . . ?
C12 N4 H8 114.5 . . ?
C13 N4 H8 114.5 . . ?
C33 N5 C35 107.7(4) . . ?
C33 N5 C36 129.7(4) . . ?
C35 N5 C36 122.4(4) . . ?
C33 N6 C34 108.6(4) . . ?
C33 N6 C40 125.6(4) . . ?
C34 N6 C40 125.6(5) . . ?
C33 N7 C44 114.2(4) . . ?
C44 N8 C45 127.2(4) . . ?
C44 N8 H4 116.4 . . ?
C45 N8 H4 116.4 . . ?
C12 O1 Li1 161.6(4) . . ?
C19 O2 Li1 156.8(4) . . ?
C19 O2 Li1 119.2(4) . 2_655 ?
Li1 O2 Li1 83.6(4) . 2_655 ?
N3 C1 N2 123.6(5) . . ?
N3 C1 N1 128.8(5) . . ?
N2 C1 N1 107.0(4) . . ?
C3 C2 N1 107.7(5) . . ?
C3 C2 H50 126.2 . . ?
N1 C2 H50 126.2 . . ?
C2 C3 N2 108.6(5) . . ?
C2 C3 H48 125.7 . . ?
N2 C3 H48 125.7 . . ?
N2 C4 C7 108.0(5) . . ?
N2 C4 C6 107.8(5) . . ?
C7 C4 C6 111.0(6) . . ?
N2 C4 C5 110.9(4) . . ?
C7 C4 C5 108.4(5) . . ?
C6 C4 C5 110.7(5) . . ?
C4 C5 H30A 109.5 . . ?
C4 C5 H30B 109.5 . . ?
H30A C5 H30B 109.5 . . ?
C4 C5 H30C 109.5 . . ?
H30A C5 H30C 109.5 . . ?
H30B C5 H30C 109.5 . . ?
C4 C6 H58A 109.5 . . ?
C4 C6 H58B 109.5 . . ?
H58A C6 H58B 109.5 . . ?
C4 C6 H58C 109.5 . . ?
H58A C6 H58C 109.5 . . ?
H58B C6 H58C 109.5 . . ?
C4 C7 H63A 109.5 . . ?
C4 C7 H63B 109.5 . . ?
H63A C7 H63B 109.5 . . ?
C4 C7 H63C 109.5 . . ?
H63A C7 H63C 109.5 . . ?
H63B C7 H63C 109.5 . . ?
N1 C8 C9 112.2(5) . . ?
N1 C8 C10 107.4(5) . . ?
C9 C8 C10 111.2(6) . . ?
N1 C8 C11 107.3(5) . . ?
C9 C8 C11 108.6(5) . . ?
C10 C8 C11 110.0(5) . . ?
C8 C9 H37A 109.5 . . ?
C8 C9 H37B 109.5 . . ?
H37A C9 H37B 109.5 . . ?
C8 C9 H37C 109.5 . . ?
H37A C9 H37C 109.5 . . ?
H37B C9 H37C 109.5 . . ?
C8 C10 H54A 109.5 . . ?
C8 C10 H54B 109.5 . . ?
H54A C10 H54B 109.5 . . ?
C8 C10 H54C 109.5 . . ?
H54A C10 H54C 109.5 . . ?
H54B C10 H54C 109.5 . . ?
C8 C11 H9A 109.5 . . ?
C8 C11 H9B 109.5 . . ?
H9A C11 H9B 109.5 . . ?
C8 C11 H9C 109.5 . . ?
H9A C11 H9C 109.5 . . ?
H9B C11 H9C 109.5 . . ?
O1 C12 N3 127.3(5) . . ?
O1 C12 N4 115.8(5) . . ?
N3 C12 N4 116.9(4) . . ?
C14 C13 C18 118.2(5) . . ?
C14 C13 N4 117.8(5) . . ?
C18 C13 N4 124.0(5) . . ?
C15 C14 C13 121.1(5) . . ?
C15 C14 H21 119.4 . . ?
C13 C14 H21 119.4 . . ?
C16 C15 C14 120.6(5) . . ?
C16 C15 H7 119.7 . . ?
C14 C15 H7 119.7 . . ?
C15 C16 C17 118.5(5) . . ?
C15 C16 H38 120.8 . . ?
C17 C16 H38 120.8 . . ?
C16 C17 C18 121.4(6) . . ?
C16 C17 H46 119.3 . . ?
C18 C17 H46 119.3 . . ?
C17 C18 C13 120.1(5) . . ?
C17 C18 H40 119.9 . . ?
C13 C18 H40 119.9 . . ?
O2 C19 C20 120.4(5) . . ?
O2 C19 C24 120.8(5) . . ?
C20 C19 C24 118.8(4) . . ?
C21 C20 C19 118.5(5) . . ?
C21 C20 C25 119.5(5) . . ?
C19 C20 C25 122.0(4) . . ?
C22 C21 C20 122.8(5) . . ?
C22 C21 H12 118.6 . . ?
C20 C21 H12 118.6 . . ?
C23 C22 C21 117.8(5) . . ?
C23 C22 C28 120.9(5) . . ?
C21 C22 C28 121.3(5) . . ?
C22 C23 C24 123.2(5) . . ?
C22 C23 H22 118.4 . . ?
C24 C23 H22 118.4 . . ?
C23 C24 C19 118.8(5) . . ?
C23 C24 C29 119.5(5) . . ?
C19 C24 C29 121.7(4) . . ?
C27 C25 C20 112.8(5) . . ?
C27 C25 C26 106.6(5) . . ?
C20 C25 C26 110.8(5) . . ?
C27 C25 C57 105.7(6) . . ?
C20 C25 C57 110.2(5) . . ?
C26 C25 C57 110.5(5) . . ?
C25 C26 H39A 109.5 . . ?
C25 C26 H39B 109.5 . . ?
H39A C26 H39B 109.5 . . ?
C25 C26 H39C 109.5 . . ?
H39A C26 H39C 109.5 . . ?
H39B C26 H39C 109.5 . . ?
C25 C27 H41A 109.5 . . ?
C25 C27 H41B 109.5 . . ?
H41A C27 H41B 109.5 . . ?
C25 C27 H41C 109.5 . . ?
H41A C27 H41C 109.5 . . ?
H41B C27 H41C 109.5 . . ?
C22 C28 H11A 109.5 . . ?
C22 C28 H11B 109.5 . . ?
H11A C28 H11B 109.5 . . ?
C22 C28 H11C 109.5 . . ?
H11A C28 H11C 109.5 . . ?
H11B C28 H11C 109.5 . . ?
C32 C29 C24 112.6(5) . . ?
C32 C29 C30 107.3(5) . . ?
C24 C29 C30 109.0(5) . . ?
C32 C29 C31 105.7(5) . . ?
C24 C29 C31 111.9(5) . . ?
C30 C29 C31 110.1(5) . . ?
C29 C30 H34A 109.5 . . ?
C29 C30 H34B 109.5 . . ?
H34A C30 H34B 109.5 . . ?
C29 C30 H34C 109.5 . . ?
H34A C30 H34C 109.5 . . ?
H34B C30 H34C 109.5 . . ?
C29 C31 H35A 109.5 . . ?
C29 C31 H35B 109.5 . . ?
H35A C31 H35B 109.5 . . ?
C29 C31 H35C 109.5 . . ?
H35A C31 H35C 109.5 . . ?
H35B C31 H35C 109.5 . . ?
C29 C32 H3A 109.5 . . ?
C29 C32 H3B 109.5 . . ?
H3A C32 H3B 109.5 . . ?
C29 C32 H3C 109.5 . . ?
H3A C32 H3C 109.5 . . ?
H3B C32 H3C 109.5 . . ?
N7 C33 N6 124.7(5) . . ?
N7 C33 N5 128.2(5) . . ?
N6 C33 N5 107.0(4) . . ?
C35 C34 N6 108.0(5) . . ?
C35 C34 H26 126.0 . . ?
N6 C34 H26 126.0 . . ?
C34 C35 N5 108.6(5) . . ?
C34 C35 H14 125.7 . . ?
N5 C35 H14 125.7 . . ?
N5 C36 C39 107.5(4) . . ?
N5 C36 C37 112.2(4) . . ?
C39 C36 C37 109.7(5) . . ?
N5 C36 C38 107.9(5) . . ?
C39 C36 C38 111.5(5) . . ?
C37 C36 C38 108.1(5) . . ?
C36 C37 H2A 109.5 . . ?
C36 C37 H2B 109.5 . . ?
H2A C37 H2B 109.5 . . ?
C36 C37 H2C 109.5 . . ?
H2A C37 H2C 109.5 . . ?
H2B C37 H2C 109.5 . . ?
C36 C38 H32A 109.5 . . ?
C36 C38 H32B 109.5 . . ?
H32A C38 H32B 109.5 . . ?
C36 C38 H32C 109.5 . . ?
H32A C38 H32C 109.5 . . ?
H32B C38 H32C 109.5 . . ?
C36 C39 H55A 109.5 . . ?
C36 C39 H55B 109.5 . . ?
H55A C39 H55B 109.5 . . ?
C36 C39 H55C 109.5 . . ?
H55A C39 H55C 109.5 . . ?
H55B C39 H55C 109.5 . . ?
N6 C40 C42 108.4(5) . . ?
N6 C40 C43 108.7(5) . . ?
C42 C40 C43 110.0(5) . . ?
N6 C40 C41 110.9(5) . . ?
C42 C40 C41 111.4(6) . . ?
C43 C40 C41 107.5(5) . . ?
C40 C41 H19A 109.5 . . ?
C40 C41 H19B 109.5 . . ?
H19A C41 H19B 109.5 . . ?
C40 C41 H19C 109.5 . . ?
H19A C41 H19C 109.5 . . ?
H19B C41 H19C 109.5 . . ?
C40 C42 H51A 109.5 . . ?
C40 C42 H51B 109.5 . . ?
H51A C42 H51B 109.5 . . ?
C40 C42 H51C 109.5 . . ?
H51A C42 H51C 109.5 . . ?
H51B C42 H51C 109.5 . . ?
C40 C43 H31A 109.5 . . ?
C40 C43 H31B 109.5 . . ?
H31A C43 H31B 109.5 . . ?
C40 C43 H31C 109.5 . . ?
H31A C43 H31C 109.5 . . ?
H31B C43 H31C 109.5 . . ?
O3 C44 N7 125.2(5) . . ?
O3 C44 N8 121.9(5) . . ?
N7 C44 N8 113.0(4) . . ?
C50 C45 C46 118.8(5) . . ?
C50 C45 N8 117.9(5) . . ?
C46 C45 N8 123.3(5) . . ?
C47 C46 C45 119.3(6) . . ?
C47 C46 H43 120.3 . . ?
C45 C46 H43 120.3 . . ?
C48 C47 C46 121.5(6) . . ?
C48 C47 H49 119.2 . . ?
C46 C47 H49 119.2 . . ?
C49 C48 C47 118.7(6) . . ?
C49 C48 H25 120.6 . . ?
C47 C48 H25 120.6 . . ?
C48 C49 C50 120.6(6) . . ?
C48 C49 H53 119.7 . . ?
C50 C49 H53 119.7 . . ?
C45 C50 C49 121.0(6) . . ?
C45 C50 H61 119.5 . . ?
C49 C50 H61 119.5 . . ?
C25 C57 H57A 109.5 . . ?
C25 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C25 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Li1 O1 C12 176.5(11) . . . . ?
O2 Li1 O1 C12 11(2) 2_655 . . . ?
Li1 Li1 O1 C12 58(3) 2_655 . . . ?
O1 Li1 O2 C19 9(2) . . . . ?
O2 Li1 O2 C19 176.5(9) 2_655 . . . ?
Li1 Li1 O2 C19 169.0(15) 2_655 . . . ?
O1 Li1 O2 Li1 -160.3(7) . . . 2_655 ?
O2 Li1 O2 Li1 7.5(7) 2_655 . . 2_655 ?
C12 N3 C1 N2 105.0(6) . . . . ?
C12 N3 C1 N1 -84.4(7) . . . . ?
C3 N2 C1 N3 172.7(5) . . . . ?
C4 N2 C1 N3 -1.0(8) . . . . ?
C3 N2 C1 N1 0.2(6) . . . . ?
C4 N2 C1 N1 -173.4(5) . . . . ?
C2 N1 C1 N3 -172.5(5) . . . . ?
C8 N1 C1 N3 14.1(9) . . . . ?
C2 N1 C1 N2 -0.6(6) . . . . ?
C8 N1 C1 N2 -174.0(5) . . . . ?
C1 N1 C2 C3 0.7(7) . . . . ?
C8 N1 C2 C3 174.8(5) . . . . ?
N1 C2 C3 N2 -0.5(7) . . . . ?
C1 N2 C3 C2 0.2(7) . . . . ?
C4 N2 C3 C2 174.0(5) . . . . ?
C1 N2 C4 C7 -167.3(6) . . . . ?
C3 N2 C4 C7 20.0(8) . . . . ?
C1 N2 C4 C6 72.6(7) . . . . ?
C3 N2 C4 C6 -100.0(6) . . . . ?
C1 N2 C4 C5 -48.7(7) . . . . ?
C3 N2 C4 C5 138.6(5) . . . . ?
C1 N1 C8 C9 -27.1(8) . . . . ?
C2 N1 C8 C9 160.2(5) . . . . ?
C1 N1 C8 C10 95.5(7) . . . . ?
C2 N1 C8 C10 -77.2(7) . . . . ?
C1 N1 C8 C11 -146.3(5) . . . . ?
C2 N1 C8 C11 41.0(7) . . . . ?
Li1 O1 C12 N3 178.8(13) . . . . ?
Li1 O1 C12 N4 -2.6(18) . . . . ?
C1 N3 C12 O1 1.0(8) . . . . ?
C1 N3 C12 N4 -177.6(5) . . . . ?
C13 N4 C12 O1 -179.2(5) . . . . ?
C13 N4 C12 N3 -0.5(9) . . . . ?
C12 N4 C13 C14 160.9(5) . . . . ?
C12 N4 C13 C18 -22.5(9) . . . . ?
C18 C13 C14 C15 -1.0(8) . . . . ?
N4 C13 C14 C15 175.8(5) . . . . ?
C13 C14 C15 C16 0.5(9) . . . . ?
C14 C15 C16 C17 0.6(9) . . . . ?
C15 C16 C17 C18 -1.2(10) . . . . ?
C16 C17 C18 C13 0.7(10) . . . . ?
C14 C13 C18 C17 0.4(9) . . . . ?
N4 C13 C18 C17 -176.2(5) . . . . ?
Li1 O2 C19 C20 -72.3(14) . . . . ?
Li1 O2 C19 C20 95.2(6) 2_655 . . . ?
Li1 O2 C19 C24 109.8(12) . . . . ?
Li1 O2 C19 C24 -82.7(6) 2_655 . . . ?
O2 C19 C20 C21 -177.0(4) . . . . ?
C24 C19 C20 C21 1.0(7) . . . . ?
O2 C19 C20 C25 3.1(7) . . . . ?
C24 C19 C20 C25 -178.9(5) . . . . ?
C19 C20 C21 C22 -0.5(8) . . . . ?
C25 C20 C21 C22 179.4(5) . . . . ?
C20 C21 C22 C23 -0.2(8) . . . . ?
C20 C21 C22 C28 -180.0(5) . . . . ?
C21 C22 C23 C24 0.5(8) . . . . ?
C28 C22 C23 C24 -179.7(5) . . . . ?
C22 C23 C24 C19 -0.1(8) . . . . ?
C22 C23 C24 C29 -178.9(5) . . . . ?
O2 C19 C24 C23 177.3(5) . . . . ?
C20 C19 C24 C23 -0.7(7) . . . . ?
O2 C19 C24 C29 -3.9(7) . . . . ?
C20 C19 C24 C29 178.1(5) . . . . ?
C21 C20 C25 C27 -3.1(8) . . . . ?
C19 C20 C25 C27 176.8(5) . . . . ?
C21 C20 C25 C26 -122.5(5) . . . . ?
C19 C20 C25 C26 57.4(7) . . . . ?
C21 C20 C25 C57 114.9(6) . . . . ?
C19 C20 C25 C57 -65.3(7) . . . . ?
C23 C24 C29 C32 -4.6(7) . . . . ?
C19 C24 C29 C32 176.6(5) . . . . ?
C23 C24 C29 C30 114.4(5) . . . . ?
C19 C24 C29 C30 -64.4(6) . . . . ?
C23 C24 C29 C31 -123.5(5) . . . . ?
C19 C24 C29 C31 57.6(7) . . . . ?
C44 N7 C33 N6 -95.0(6) . . . . ?
C44 N7 C33 N5 89.4(6) . . . . ?
C34 N6 C33 N7 -178.4(5) . . . . ?
C40 N6 C33 N7 -2.6(8) . . . . ?
C34 N6 C33 N5 -1.9(5) . . . . ?
C40 N6 C33 N5 173.8(4) . . . . ?
C35 N5 C33 N7 178.4(5) . . . . ?
C36 N5 C33 N7 -6.8(8) . . . . ?
C35 N5 C33 N6 2.2(5) . . . . ?
C36 N5 C33 N6 177.0(5) . . . . ?
C33 N6 C34 C35 1.0(6) . . . . ?
C40 N6 C34 C35 -174.8(5) . . . . ?
N6 C34 C35 N5 0.4(6) . . . . ?
C33 N5 C35 C34 -1.6(6) . . . . ?
C36 N5 C35 C34 -176.9(5) . . . . ?
C33 N5 C36 C39 -93.8(6) . . . . ?
C35 N5 C36 C39 80.4(6) . . . . ?
C33 N5 C36 C37 26.9(7) . . . . ?
C35 N5 C36 C37 -158.9(5) . . . . ?
C33 N5 C36 C38 145.9(5) . . . . ?
C35 N5 C36 C38 -39.9(7) . . . . ?
C33 N6 C40 C42 -64.9(7) . . . . ?
C34 N6 C40 C42 110.1(6) . . . . ?
C33 N6 C40 C43 175.6(5) . . . . ?
C34 N6 C40 C43 -9.4(7) . . . . ?
C33 N6 C40 C41 57.7(7) . . . . ?
C34 N6 C40 C41 -127.3(6) . . . . ?
C33 N7 C44 O3 -3.8(8) . . . . ?
C33 N7 C44 N8 175.6(5) . . . . ?
C45 N8 C44 O3 7.0(9) . . . . ?
C45 N8 C44 N7 -172.4(5) . . . . ?
C44 N8 C45 C50 -166.8(5) . . . . ?
C44 N8 C45 C46 15.1(9) . . . . ?
C50 C45 C46 C47 1.4(9) . . . . ?
N8 C45 C46 C47 179.5(5) . . . . ?
C45 C46 C47 C48 0.3(10) . . . . ?
C46 C47 C48 C49 -1.4(10) . . . . ?
C47 C48 C49 C50 0.8(11) . . . . ?
C46 C45 C50 C49 -2.0(9) . . . . ?
N8 C45 C50 C49 179.8(6) . . . . ?
C48 C49 C50 C45 0.9(10) . . . . ?

_refine_diff_density_max         0.368
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.058

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_4a
_database_code_depnum_ccdc_archive 'CCDC 1046055'
_audit_update_record             
;
2015-03-02 deposited with the CCDC.
2015-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H69 Ca K N6 O Si4'
_chemical_formula_weight         805.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 '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      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                   13.3821(4)
_cell_length_b                   18.2812(3)
_cell_length_c                   18.9510(5)
_cell_angle_alpha                90
_cell_angle_beta                 103.948(2)
_cell_angle_gamma                90
_cell_volume                     4499.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6792
_cell_measurement_theta_min      3.4021
_cell_measurement_theta_max      70.6772

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_F_000             1744
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_exptl_absorpt_coefficient_mu    3.315
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.62213
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27'

_exptl_special_details           
;
 'Empirical absorption correction using spherical harmonics,implemented in SCALE3 ABSPACK scaling algorithm.'
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17614
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.403
_diffrn_reflns_theta_max         70.776
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8468
_reflns_number_gt                6548
_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       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP III & Olex 2.1'
_computing_publication_material  WinGX

_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)+(0.0493P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8468
_refine_ls_number_parameters     389
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0418
_refine_ls_wR_factor_ref         0.1128
_refine_ls_wR_factor_gt          0.1041
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_restrained_S_all      0.997
_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
Ca1 Ca 0.66808(3) 0.19711(2) 0.23478(3) 0.03170(12) Uani 1 1 d . . . . .
K1 K 0.52134(4) 0.02138(3) 0.25569(3) 0.03811(13) Uani 1 1 d . . . . .
Si1 Si 0.77891(5) 0.32193(4) 0.36227(4) 0.04227(18) Uani 1 1 d . . . . .
Si2 Si 0.88439(5) 0.29976(4) 0.24046(4) 0.03762(17) Uani 1 1 d . . . . .
Si3 Si 0.66098(5) 0.05828(3) 0.11378(4) 0.03552(16) Uani 1 1 d . . . . .
Si4 Si 0.79856(5) 0.03746(3) 0.26514(3) 0.03041(14) Uani 1 1 d . . . . .
O1 O 0.50510(11) 0.16427(8) 0.25131(8) 0.0326(4) Uani 1 1 d . . . . .
N1 N 0.35655(13) 0.23380(10) 0.21401(10) 0.0293(4) Uani 1 1 d . . . . .
N2 N 0.30668(15) 0.17184(10) 0.31460(10) 0.0340(4) Uani 1 1 d . . . . .
N3 N 0.23369(13) 0.13737(10) 0.20328(10) 0.0322(4) Uani 1 1 d . . . . .
N4 N 0.51929(13) 0.27056(10) 0.19614(10) 0.0302(4) Uani 1 1 d . . . . .
N5 N 0.70079(13) 0.07679(10) 0.20319(10) 0.0281(4) Uani 1 1 d . . . . .
N6 N 0.79638(14) 0.27872(10) 0.28806(11) 0.0342(4) Uani 1 1 d . . . . .
C1 C 0.30565(16) 0.18399(12) 0.24328(12) 0.0290(5) Uani 1 1 d . . . . .
C2 C 0.19297(19) 0.09505(14) 0.25075(15) 0.0424(6) Uani 1 1 d . . . . .
H2 H 0.1433 0.0587 0.2376 0.051 Uiso 1 1 calc R U . . .
C3 C 0.2373(2) 0.11557(14) 0.31767(15) 0.0440(6) Uani 1 1 d . . . . .
H3 H 0.2246 0.0958 0.3599 0.053 Uiso 1 1 calc R U . . .
C4 C 0.3655(2) 0.21025(13) 0.38237(13) 0.0399(6) Uani 1 1 d . . . . .
C5 C 0.4063(3) 0.28353(15) 0.36426(15) 0.0619(9) Uani 1 1 d . . . . .
H5A H 0.3498 0.3137 0.3398 0.093 Uiso 1 1 calc R U . . .
H5B H 0.4525 0.2761 0.3333 0.093 Uiso 1 1 calc R U . . .
H5C H 0.4423 0.3072 0.4083 0.093 Uiso 1 1 calc R U . . .
C6 C 0.2917(2) 0.2236(2) 0.43123(16) 0.0705(10) Uani 1 1 d . . . . .
H6A H 0.2364 0.2547 0.4065 0.106 Uiso 1 1 calc R U . . .
H6B H 0.3281 0.2468 0.4754 0.106 Uiso 1 1 calc R U . . .
H6C H 0.2641 0.1778 0.4424 0.106 Uiso 1 1 calc R U . . .
C7 C 0.4526(2) 0.16117(15) 0.42107(14) 0.0483(7) Uani 1 1 d . . . . .
H7A H 0.4250 0.1153 0.4324 0.072 Uiso 1 1 calc R U . . .
H7B H 0.4893 0.1843 0.4652 0.072 Uiso 1 1 calc R U . . .
H7C H 0.4987 0.1527 0.3902 0.072 Uiso 1 1 calc R U . . .
C8 C 0.19928(18) 0.13629(14) 0.12179(13) 0.0379(5) Uani 1 1 d . . . . .
C9 C 0.1192(2) 0.07597(15) 0.09859(16) 0.0544(7) Uani 1 1 d . . . . .
H9A H 0.0611 0.0855 0.1186 0.082 Uiso 1 1 calc R U . . .
H9B H 0.1491 0.0297 0.1160 0.082 Uiso 1 1 calc R U . . .
H9C H 0.0972 0.0748 0.0465 0.082 Uiso 1 1 calc R U . . .
C10 C 0.1497(2) 0.21027(14) 0.09632(15) 0.0507(7) Uani 1 1 d . . . . .
H10A H 0.0925 0.2184 0.1176 0.076 Uiso 1 1 calc R U . . .
H10B H 0.1261 0.2102 0.0443 0.076 Uiso 1 1 calc R U . . .
H10C H 0.1996 0.2485 0.1111 0.076 Uiso 1 1 calc R U . . .
C11 C 0.2909(2) 0.12069(15) 0.08949(14) 0.0475(6) Uani 1 1 d . . . . .
H11A H 0.3201 0.0741 0.1065 0.071 Uiso 1 1 calc R U . . .
H11B H 0.3419 0.1582 0.1042 0.071 Uiso 1 1 calc R U . . .
H11C H 0.2685 0.1199 0.0374 0.071 Uiso 1 1 calc R U . . .
C12 C 0.45740(16) 0.22278(12) 0.22041(12) 0.0291(5) Uani 1 1 d . . . . .
C15 C 0.7155(3) 0.25920(18) 0.41662(17) 0.0693(9) Uani 1 1 d . . . . .
H15A H 0.6527 0.2405 0.3861 0.104 Uiso 1 1 calc R U . . .
H15B H 0.7003 0.2857 0.4565 0.104 Uiso 1 1 calc R U . . .
H15C H 0.7609 0.2193 0.4350 0.104 Uiso 1 1 calc R U . . .
C16 C 0.6883(2) 0.40219(15) 0.33974(16) 0.0532(7) Uani 1 1 d . . . . .
H16A H 0.7158 0.4372 0.3117 0.080 Uiso 1 1 calc R U . . .
H16B H 0.6806 0.4246 0.3839 0.080 Uiso 1 1 calc R U . . .
H16C H 0.6224 0.3856 0.3121 0.080 Uiso 1 1 calc R U . . .
C17 C 0.9005(2) 0.35546(18) 0.42603(17) 0.0709(10) Uani 1 1 d . . . . .
H17A H 0.9359 0.3879 0.4005 0.106 Uiso 1 1 calc R U . . .
H17B H 0.9440 0.3145 0.4443 0.106 Uiso 1 1 calc R U . . .
H17C H 0.8836 0.3811 0.4659 0.106 Uiso 1 1 calc R U . . .
C18 C 0.8904(2) 0.40019(14) 0.22045(18) 0.0584(8) Uani 1 1 d . . . . .
H18A H 0.9082 0.4270 0.2653 0.088 Uiso 1 1 calc R U . . .
H18B H 0.8245 0.4163 0.1923 0.088 Uiso 1 1 calc R U . . .
H18C H 0.9416 0.4085 0.1935 0.088 Uiso 1 1 calc R U . . .
C19 C 1.02084(19) 0.27301(16) 0.28589(18) 0.0573(8) Uani 1 1 d . . . . .
H19A H 1.0232 0.2219 0.2978 0.086 Uiso 1 1 calc R U . . .
H19B H 1.0442 0.3011 0.3296 0.086 Uiso 1 1 calc R U . . .
H19C H 1.0645 0.2824 0.2535 0.086 Uiso 1 1 calc R U . . .
C20 C 0.8492(2) 0.25265(15) 0.14925(14) 0.0484(7) Uani 1 1 d . . . . .
H20A H 0.8446 0.2009 0.1563 0.073 Uiso 1 1 calc R U . . .
H20B H 0.9010 0.2624 0.1232 0.073 Uiso 1 1 calc R U . . .
H20C H 0.7840 0.2707 0.1218 0.073 Uiso 1 1 calc R U . . .
C21 C 0.7667(3) 0.03277(18) 0.06851(16) 0.0659(9) Uani 1 1 d . . . . .
H21A H 0.8029 -0.0092 0.0923 0.099 Uiso 1 1 calc R U . . .
H21B H 0.8137 0.0730 0.0718 0.099 Uiso 1 1 calc R U . . .
H21C H 0.7374 0.0215 0.0183 0.099 Uiso 1 1 calc R U . . .
C22 C 0.5926(2) 0.14036(13) 0.06481(13) 0.0444(6) Uani 1 1 d . . . . .
H22A H 0.5379 0.1545 0.0867 0.067 Uiso 1 1 calc R U . . .
H22B H 0.5646 0.1283 0.0146 0.067 Uiso 1 1 calc R U . . .
H22C H 0.6405 0.1801 0.0682 0.067 Uiso 1 1 calc R U . . .
C23 C 0.5651(2) -0.01885(15) 0.09579(15) 0.0612(9) Uani 1 1 d . . . . .
H23A H 0.5095 -0.0081 0.1181 0.092 Uiso 1 1 calc R U . . .
H23B H 0.5982 -0.0634 0.1158 0.092 Uiso 1 1 calc R U . . .
H23C H 0.5385 -0.0245 0.0443 0.092 Uiso 1 1 calc R U . . .
C24 C 0.7930(2) 0.07511(14) 0.35668(13) 0.0452(6) Uani 1 1 d . . . . .
H24A H 0.7267 0.0648 0.3656 0.068 Uiso 1 1 calc R U . . .
H24B H 0.8036 0.1271 0.3573 0.068 Uiso 1 1 calc R U . . .
H24C H 0.8457 0.0527 0.3938 0.068 Uiso 1 1 calc R U . . .
C25 C 0.93023(18) 0.06020(14) 0.25351(16) 0.0469(7) Uani 1 1 d . . . . .
H25A H 0.9374 0.0421 0.2074 0.070 Uiso 1 1 calc R U . . .
H25B H 0.9812 0.0379 0.2919 0.070 Uiso 1 1 calc R U . . .
H25C H 0.9395 0.1123 0.2553 0.070 Uiso 1 1 calc R U . . .
C26 C 0.79372(19) -0.06570(12) 0.26720(14) 0.0410(6) Uani 1 1 d . . . . .
H26A H 0.7967 -0.0847 0.2205 0.061 Uiso 1 1 calc R U . . .
H26B H 0.7308 -0.0811 0.2785 0.061 Uiso 1 1 calc R U . . .
H26C H 0.8512 -0.0838 0.3036 0.061 Uiso 1 1 calc R U . . .
C31 C 0.48731(16) 0.33526(12) 0.15900(11) 0.0289(5) Uani 1 1 d . . . . .
C32 C 0.56697(18) 0.38003(12) 0.14534(13) 0.0349(5) Uani 1 1 d . . . . .
H32 H 0.6350 0.3654 0.1628 0.042 Uiso 1 1 calc R U . . .
C33 C 0.5467(2) 0.44452(13) 0.10695(13) 0.0408(6) Uani 1 1 d . . . . .
H33 H 0.6011 0.4722 0.0989 0.049 Uiso 1 1 calc R U . . .
C34 C 0.4469(2) 0.46889(13) 0.08020(13) 0.0382(6) Uani 1 1 d . . . . .
H34 H 0.4335 0.5124 0.0543 0.046 Uiso 1 1 calc R U . . .
C35 C 0.36760(19) 0.42645(13) 0.09323(12) 0.0359(5) Uani 1 1 d . . . . .
H35 H 0.2999 0.4417 0.0753 0.043 Uiso 1 1 calc R U . . .
C36 C 0.38658(17) 0.36146(12) 0.13245(12) 0.0325(5) Uani 1 1 d . . . . .
H36 H 0.3315 0.3349 0.1412 0.039 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
Ca1 N6 2.3146(19) . ?
Ca1 N5 2.3482(18) . ?
Ca1 O1 2.3548(15) . ?
Ca1 N4 2.3666(18) . ?
Ca1 C12 2.806(2) . ?
Ca1 Si4 3.3784(7) . ?
Ca1 Si1 3.3936(8) . ?
Ca1 Si3 3.4063(8) . ?
Ca1 Si2 3.4295(8) . ?
Ca1 K1 3.8352(7) . ?
K1 O1 2.6208(16) . ?
K1 N5 2.9891(18) . ?
K1 C34 3.184(2) 2_645 ?
K1 C33 3.274(2) 2_645 ?
K1 C35 3.371(2) 2_645 ?
K1 Si4 3.6824(8) . ?
K1 Si3 3.6881(9) . ?
Si1 N6 1.6778(19) . ?
Si1 C15 1.876(3) . ?
Si1 C17 1.880(3) . ?
Si1 C16 1.886(3) . ?
Si2 N6 1.6914(19) . ?
Si2 C18 1.880(3) . ?
Si2 C19 1.886(3) . ?
Si2 C20 1.887(3) . ?
Si3 N5 1.6834(18) . ?
Si3 C22 1.881(2) . ?
Si3 C21 1.882(3) . ?
Si3 C23 1.882(3) . ?
Si4 N5 1.6932(18) . ?
Si4 C25 1.874(2) . ?
Si4 C24 1.885(3) . ?
Si4 C26 1.888(2) . ?
O1 C12 1.309(3) . ?
N1 C1 1.335(3) . ?
N1 C12 1.341(3) . ?
N2 C1 1.366(3) . ?
N2 C3 1.396(3) . ?
N2 C4 1.508(3) . ?
N3 C1 1.370(3) . ?
N3 C2 1.393(3) . ?
N3 C8 1.501(3) . ?
N4 C12 1.358(3) . ?
N4 C31 1.390(3) . ?
C2 C3 1.319(4) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C7 1.513(3) . ?
C4 C5 1.517(4) . ?
C4 C6 1.528(4) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C11 1.524(3) . ?
C8 C9 1.526(3) . ?
C8 C10 1.532(3) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C31 C36 1.405(3) . ?
C31 C32 1.416(3) . ?
C32 C33 1.378(3) . ?
C32 H32 0.9300 . ?
C33 C34 1.383(3) . ?
C33 K1 3.274(2) 2_655 ?
C33 H33 0.9300 . ?
C34 C35 1.384(3) . ?
C34 K1 3.184(2) 2_655 ?
C34 H34 0.9300 . ?
C35 C36 1.392(3) . ?
C35 K1 3.371(2) 2_655 ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?

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
N6 Ca1 N5 123.42(7) . . ?
N6 Ca1 O1 136.03(6) . . ?
N5 Ca1 O1 91.76(6) . . ?
N6 Ca1 N4 104.45(7) . . ?
N5 Ca1 N4 130.33(6) . . ?
O1 Ca1 N4 56.54(6) . . ?
N6 Ca1 C12 123.84(7) . . ?
N5 Ca1 C12 112.12(6) . . ?
O1 Ca1 C12 27.67(6) . . ?
N4 Ca1 C12 28.87(6) . . ?
N6 Ca1 Si4 100.60(5) . . ?
N5 Ca1 Si4 27.60(4) . . ?
O1 Ca1 Si4 102.38(4) . . ?
N4 Ca1 Si4 154.77(5) . . ?
C12 Ca1 Si4 128.83(5) . . ?
N6 Ca1 Si1 26.50(5) . . ?
N5 Ca1 Si1 137.31(5) . . ?
O1 Ca1 Si1 109.67(4) . . ?
N4 Ca1 Si1 91.69(5) . . ?
C12 Ca1 Si1 102.30(5) . . ?
Si4 Ca1 Si1 109.90(2) . . ?
N6 Ca1 Si3 132.17(5) . . ?
N5 Ca1 Si3 26.77(4) . . ?
O1 Ca1 Si3 91.33(4) . . ?
N4 Ca1 Si3 109.24(5) . . ?
C12 Ca1 Si3 101.24(5) . . ?
Si4 Ca1 Si3 53.160(17) . . ?
Si1 Ca1 Si3 156.46(2) . . ?
N6 Ca1 Si2 26.09(5) . . ?
N5 Ca1 Si2 108.23(5) . . ?
O1 Ca1 Si2 159.58(4) . . ?
N4 Ca1 Si2 109.88(5) . . ?
C12 Ca1 Si2 137.07(5) . . ?
Si4 Ca1 Si2 93.999(18) . . ?
Si1 Ca1 Si2 52.340(19) . . ?
Si3 Ca1 Si2 108.38(2) . . ?
N6 Ca1 K1 147.06(5) . . ?
N5 Ca1 K1 51.19(4) . . ?
O1 Ca1 K1 42.18(4) . . ?
N4 Ca1 K1 95.37(4) . . ?
C12 Ca1 K1 67.83(5) . . ?
Si4 Ca1 K1 61.003(15) . . ?
Si1 Ca1 K1 129.52(2) . . ?
Si3 Ca1 K1 60.893(16) . . ?
Si2 Ca1 K1 154.744(19) . . ?
O1 K1 N5 73.67(5) . . ?
O1 K1 C34 108.78(6) . 2_645 ?
N5 K1 C34 119.91(6) . 2_645 ?
O1 K1 C33 114.59(6) . 2_645 ?
N5 K1 C33 144.06(6) . 2_645 ?
C34 K1 C33 24.67(6) 2_645 2_645 ?
O1 K1 C35 123.79(5) . 2_645 ?
N5 K1 C35 103.42(6) . 2_645 ?
C34 K1 C35 24.16(6) 2_645 2_645 ?
C33 K1 C35 41.76(6) 2_645 2_645 ?
O1 K1 Si4 89.82(4) . . ?
N5 K1 Si4 26.92(3) . . ?
C34 K1 Si4 94.64(5) 2_645 . ?
C33 K1 Si4 117.74(5) 2_645 . ?
C35 K1 Si4 76.53(4) 2_645 . ?
O1 K1 Si3 81.22(4) . . ?
N5 K1 Si3 26.67(4) . . ?
C34 K1 Si3 142.72(5) 2_645 . ?
C33 K1 Si3 160.91(5) 2_645 . ?
C35 K1 Si3 121.08(5) 2_645 . ?
Si4 K1 Si3 48.648(16) . . ?
O1 K1 Ca1 37.11(3) . . ?
N5 K1 Ca1 37.75(3) . . ?
C34 K1 Ca1 113.72(5) 2_645 . ?
C33 K1 Ca1 133.55(5) 2_645 . ?
C35 K1 Ca1 112.77(4) 2_645 . ?
Si4 K1 Ca1 53.364(13) . . ?
Si3 K1 Ca1 53.800(14) . . ?
N6 Si1 C15 110.21(12) . . ?
N6 Si1 C17 114.74(12) . . ?
C15 Si1 C17 106.40(16) . . ?
N6 Si1 C16 112.86(12) . . ?
C15 Si1 C16 104.40(14) . . ?
C17 Si1 C16 107.53(13) . . ?
N6 Si1 Ca1 37.99(6) . . ?
C15 Si1 Ca1 78.58(10) . . ?
C17 Si1 Ca1 147.01(10) . . ?
C16 Si1 Ca1 102.43(9) . . ?
N6 Si2 C18 113.50(11) . . ?
N6 Si2 C19 114.81(13) . . ?
C18 Si2 C19 105.15(13) . . ?
N6 Si2 C20 109.43(11) . . ?
C18 Si2 C20 105.92(14) . . ?
C19 Si2 C20 107.48(13) . . ?
N6 Si2 Ca1 37.00(6) . . ?
C18 Si2 Ca1 127.21(9) . . ?
C19 Si2 Ca1 126.12(10) . . ?
C20 Si2 Ca1 72.48(8) . . ?
N5 Si3 C22 109.54(10) . . ?
N5 Si3 C21 114.73(12) . . ?
C22 Si3 C21 107.60(13) . . ?
N5 Si3 C23 111.68(11) . . ?
C22 Si3 C23 106.20(12) . . ?
C21 Si3 C23 106.66(15) . . ?
N5 Si3 Ca1 38.92(6) . . ?
C22 Si3 Ca1 70.69(8) . . ?
C21 Si3 Ca1 126.13(11) . . ?
C23 Si3 Ca1 125.97(11) . . ?
N5 Si3 K1 52.84(6) . . ?
C22 Si3 K1 103.53(9) . . ?
C21 Si3 K1 148.86(11) . . ?
C23 Si3 K1 63.36(10) . . ?
Ca1 Si3 K1 65.307(16) . . ?
N5 Si4 C25 114.55(11) . . ?
N5 Si4 C24 106.72(10) . . ?
C25 Si4 C24 105.92(12) . . ?
N5 Si4 C26 114.46(10) . . ?
C25 Si4 C26 105.19(11) . . ?
C24 Si4 C26 109.67(12) . . ?
N5 Si4 Ca1 39.98(6) . . ?
C25 Si4 Ca1 104.49(8) . . ?
C24 Si4 Ca1 73.00(8) . . ?
C26 Si4 Ca1 147.96(8) . . ?
N5 Si4 K1 53.07(6) . . ?
C25 Si4 K1 167.56(9) . . ?
C24 Si4 K1 79.09(8) . . ?
C26 Si4 K1 83.23(8) . . ?
Ca1 Si4 K1 65.634(15) . . ?
C12 O1 Ca1 95.71(12) . . ?
C12 O1 K1 148.89(14) . . ?
Ca1 O1 K1 100.71(5) . . ?
C1 N1 C12 117.59(19) . . ?
C1 N2 C3 108.2(2) . . ?
C1 N2 C4 130.2(2) . . ?
C3 N2 C4 121.5(2) . . ?
C1 N3 C2 108.7(2) . . ?
C1 N3 C8 125.29(18) . . ?
C2 N3 C8 125.9(2) . . ?
C12 N4 C31 125.47(18) . . ?
C12 N4 Ca1 93.83(13) . . ?
C31 N4 Ca1 140.60(14) . . ?
Si3 N5 Si4 128.08(11) . . ?
Si3 N5 Ca1 114.31(9) . . ?
Si4 N5 Ca1 112.42(9) . . ?
Si3 N5 K1 100.50(8) . . ?
Si4 N5 K1 100.01(8) . . ?
Ca1 N5 K1 91.06(5) . . ?
Si1 N6 Si2 126.55(12) . . ?
Si1 N6 Ca1 115.51(10) . . ?
Si2 N6 Ca1 116.91(10) . . ?
N1 C1 N2 129.6(2) . . ?
N1 C1 N3 123.7(2) . . ?
N2 C1 N3 106.52(19) . . ?
C3 C2 N3 107.9(2) . . ?
C3 C2 H2 126.0 . . ?
N3 C2 H2 126.0 . . ?
C2 C3 N2 108.6(2) . . ?
C2 C3 H3 125.7 . . ?
N2 C3 H3 125.7 . . ?
N2 C4 C7 108.6(2) . . ?
N2 C4 C5 111.2(2) . . ?
C7 C4 C5 110.9(2) . . ?
N2 C4 C6 108.1(2) . . ?
C7 C4 C6 109.6(2) . . ?
C5 C4 C6 108.4(2) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 C11 109.80(19) . . ?
N3 C8 C9 109.0(2) . . ?
C11 C8 C9 109.0(2) . . ?
N3 C8 C10 108.3(2) . . ?
C11 C8 C10 111.6(2) . . ?
C9 C8 C10 109.1(2) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O1 C12 N1 122.3(2) . . ?
O1 C12 N4 113.92(18) . . ?
N1 C12 N4 123.8(2) . . ?
O1 C12 Ca1 56.62(10) . . ?
N1 C12 Ca1 178.93(17) . . ?
N4 C12 Ca1 57.30(11) . . ?
Si1 C15 H15A 109.5 . . ?
Si1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si1 C16 H16A 109.5 . . ?
Si1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si1 C17 H17A 109.5 . . ?
Si1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si2 C18 H18A 109.5 . . ?
Si2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si2 C19 H19A 109.5 . . ?
Si2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si2 C20 H20A 109.5 . . ?
Si2 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Si2 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si3 C21 H21A 109.5 . . ?
Si3 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si3 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si3 C22 H22A 109.5 . . ?
Si3 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si3 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si3 C23 H23A 109.5 . . ?
Si3 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si3 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si4 C24 H24A 109.5 . . ?
Si4 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si4 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si4 C25 H25A 109.5 . . ?
Si4 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
Si4 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si4 C26 H26A 109.5 . . ?
Si4 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si4 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N4 C31 C36 128.6(2) . . ?
N4 C31 C32 115.52(19) . . ?
C36 C31 C32 115.9(2) . . ?
C33 C32 C31 122.0(2) . . ?
C33 C32 H32 119.0 . . ?
C31 C32 H32 119.0 . . ?
C32 C33 C34 121.3(2) . . ?
C32 C33 K1 90.26(15) . 2_655 ?
C34 C33 K1 73.99(14) . 2_655 ?
C32 C33 H33 119.4 . . ?
C34 C33 H33 119.4 . . ?
K1 C33 H33 106.1 2_655 . ?
C33 C34 C35 117.9(2) . . ?
C33 C34 K1 81.33(14) . 2_655 ?
C35 C34 K1 85.54(14) . 2_655 ?
C33 C34 H34 121.0 . . ?
C35 C34 H34 121.0 . . ?
K1 C34 H34 102.8 2_655 . ?
C34 C35 C36 121.6(2) . . ?
C34 C35 K1 70.30(13) . 2_655 ?
C36 C35 K1 89.98(14) . 2_655 ?
C34 C35 H35 119.2 . . ?
C36 C35 H35 119.2 . . ?
K1 C35 H35 110.2 2_655 . ?
C35 C36 C31 121.2(2) . . ?
C35 C36 H36 119.4 . . ?
C31 C36 H36 119.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C22 Si3 N5 Si4 -155.86(14) . . . . ?
C21 Si3 N5 Si4 -34.7(2) . . . . ?
C23 Si3 N5 Si4 86.77(17) . . . . ?
Ca1 Si3 N5 Si4 -152.32(19) . . . . ?
K1 Si3 N5 Si4 111.70(15) . . . . ?
C22 Si3 N5 Ca1 -3.55(13) . . . . ?
C21 Si3 N5 Ca1 117.57(13) . . . . ?
C23 Si3 N5 Ca1 -120.92(13) . . . . ?
K1 Si3 N5 Ca1 -95.99(9) . . . . ?
C22 Si3 N5 K1 92.44(10) . . . . ?
C21 Si3 N5 K1 -146.44(12) . . . . ?
C23 Si3 N5 K1 -24.93(13) . . . . ?
Ca1 Si3 N5 K1 95.99(9) . . . . ?
C25 Si4 N5 Si3 69.43(17) . . . . ?
C24 Si4 N5 Si3 -173.69(14) . . . . ?
C26 Si4 N5 Si3 -52.18(17) . . . . ?
Ca1 Si4 N5 Si3 152.74(19) . . . . ?
K1 Si4 N5 Si3 -111.92(15) . . . . ?
C25 Si4 N5 Ca1 -83.31(13) . . . . ?
C24 Si4 N5 Ca1 33.57(13) . . . . ?
C26 Si4 N5 Ca1 155.08(10) . . . . ?
K1 Si4 N5 Ca1 95.34(9) . . . . ?
C25 Si4 N5 K1 -178.65(10) . . . . ?
C24 Si4 N5 K1 -61.77(11) . . . . ?
C26 Si4 N5 K1 59.74(11) . . . . ?
Ca1 Si4 N5 K1 -95.34(9) . . . . ?
C15 Si1 N6 Si2 -156.57(16) . . . . ?
C17 Si1 N6 Si2 -36.5(2) . . . . ?
C16 Si1 N6 Si2 87.15(17) . . . . ?
Ca1 Si1 N6 Si2 167.9(2) . . . . ?
C15 Si1 N6 Ca1 35.50(16) . . . . ?
C17 Si1 N6 Ca1 155.56(14) . . . . ?
C16 Si1 N6 Ca1 -80.78(14) . . . . ?
C18 Si2 N6 Si1 -46.54(19) . . . . ?
C19 Si2 N6 Si1 74.46(18) . . . . ?
C20 Si2 N6 Si1 -164.61(14) . . . . ?
Ca1 Si2 N6 Si1 -167.8(2) . . . . ?
C18 Si2 N6 Ca1 121.25(14) . . . . ?
C19 Si2 N6 Ca1 -117.75(13) . . . . ?
C20 Si2 N6 Ca1 3.17(15) . . . . ?
C12 N1 C1 N2 74.8(3) . . . . ?
C12 N1 C1 N3 -110.4(2) . . . . ?
C3 N2 C1 N1 177.5(2) . . . . ?
C4 N2 C1 N1 -0.3(4) . . . . ?
C3 N2 C1 N3 2.1(2) . . . . ?
C4 N2 C1 N3 -175.8(2) . . . . ?
C2 N3 C1 N1 -177.6(2) . . . . ?
C8 N3 C1 N1 -1.7(3) . . . . ?
C2 N3 C1 N2 -1.8(2) . . . . ?
C8 N3 C1 N2 174.07(19) . . . . ?
C1 N3 C2 C3 0.8(3) . . . . ?
C8 N3 C2 C3 -175.0(2) . . . . ?
N3 C2 C3 N2 0.5(3) . . . . ?
C1 N2 C3 C2 -1.7(3) . . . . ?
C4 N2 C3 C2 176.4(2) . . . . ?
C1 N2 C4 C7 -105.4(3) . . . . ?
C3 N2 C4 C7 77.0(3) . . . . ?
C1 N2 C4 C5 16.8(3) . . . . ?
C3 N2 C4 C5 -160.8(2) . . . . ?
C1 N2 C4 C6 135.7(3) . . . . ?
C3 N2 C4 C6 -41.9(3) . . . . ?
C1 N3 C8 C11 60.1(3) . . . . ?
C2 N3 C8 C11 -124.8(2) . . . . ?
C1 N3 C8 C9 179.4(2) . . . . ?
C2 N3 C8 C9 -5.4(3) . . . . ?
C1 N3 C8 C10 -62.0(3) . . . . ?
C2 N3 C8 C10 113.2(2) . . . . ?
Ca1 O1 C12 N1 179.85(19) . . . . ?
K1 O1 C12 N1 58.0(4) . . . . ?
Ca1 O1 C12 N4 -0.40(19) . . . . ?
K1 O1 C12 N4 -122.2(2) . . . . ?
K1 O1 C12 Ca1 -121.8(3) . . . . ?
C1 N1 C12 O1 2.8(3) . . . . ?
C1 N1 C12 N4 -176.9(2) . . . . ?
C31 N4 C12 O1 177.37(19) . . . . ?
Ca1 N4 C12 O1 0.40(19) . . . . ?
C31 N4 C12 N1 -2.9(3) . . . . ?
Ca1 N4 C12 N1 -179.86(19) . . . . ?
C31 N4 C12 Ca1 177.0(2) . . . . ?
C12 N4 C31 C36 -7.0(4) . . . . ?
Ca1 N4 C31 C36 168.25(17) . . . . ?
C12 N4 C31 C32 174.0(2) . . . . ?
Ca1 N4 C31 C32 -10.8(3) . . . . ?
N4 C31 C32 C33 177.8(2) . . . . ?
C36 C31 C32 C33 -1.4(3) . . . . ?
C31 C32 C33 C34 0.4(4) . . . . ?
C31 C32 C33 K1 71.8(2) . . . 2_655 ?
C32 C33 C34 C35 0.1(4) . . . . ?
K1 C33 C34 C35 -80.2(2) 2_655 . . . ?
C32 C33 C34 K1 80.3(2) . . . 2_655 ?
C33 C34 C35 C36 0.5(4) . . . . ?
K1 C34 C35 C36 -77.2(2) 2_655 . . . ?
C33 C34 C35 K1 77.7(2) . . . 2_655 ?
C34 C35 C36 C31 -1.6(4) . . . . ?
K1 C35 C36 C31 -68.2(2) 2_655 . . . ?
N4 C31 C36 C35 -177.1(2) . . . . ?
C32 C31 C36 C35 2.0(3) . . . . ?

_refine_diff_density_max         0.295
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.063

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_5a
_database_code_depnum_ccdc_archive 'CCDC 1046056'
_audit_update_record             
;
2015-03-02 deposited with the CCDC.
2015-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
' 	C92 H160 Ca3 K4 N18 O10 Si8, 2(C6 H18 N Si2), 2(C7 H8), 2(Ca)'
_chemical_formula_sum            'C118 H212 Ca5 K4 N20 O10 Si12'
_chemical_formula_weight         2764.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   13.5505(8)
_cell_length_b                   14.8203(10)
_cell_length_c                   20.0745(14)
_cell_angle_alpha                95.918(6)
_cell_angle_beta                 96.395(5)
_cell_angle_gamma                101.199(5)
_cell_volume                     3897.7(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8294
_cell_measurement_theta_min      3.0635
_cell_measurement_theta_max      70.7611

_exptl_crystal_description       chunk
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1484
_exptl_absorpt_coefficient_mu    3.771
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.66635
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27'

_exptl_special_details           
;
 'Empirical absorption correction using spherical harmonics,implemented in SCALE3 ABSPACK scaling algorithm.'
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29900
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_av_sigmaI/netI    0.0998
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         70.84
_reflns_number_total             14690
_reflns_number_gt                10347
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP III & Olex 2.1'
_computing_publication_material  WinGX

_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 > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+13.1870P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14690
_refine_ls_number_parameters     792
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0533
_refine_ls_wR_factor_ref         0.1758
_refine_ls_wR_factor_gt          0.1649
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.214
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.0000 1.0000 1.0000 0.0241(3) Uani 1 2 d S . .
Ca2 Ca 0.11510(8) 0.88702(7) 0.90435(5) 0.0256(2) Uani 1 1 d . . .
Ca3 Ca 0.41613(9) 0.59446(8) 0.47678(6) 0.0416(3) Uani 1 1 d . . .
Si1 Si 0.26037(11) 1.08041(10) 1.02980(7) 0.0284(3) Uani 1 1 d . . .
Si2 Si -0.14186(11) 0.93032(10) 0.84566(7) 0.0298(3) Uani 1 1 d . . .
Si3 Si 0.35242(13) 0.83628(11) 0.48320(8) 0.0405(4) Uani 1 1 d . . .
Si4 Si 0.17996(12) 0.67109(11) 0.44410(8) 0.0385(4) Uani 1 1 d . . .
Si5 Si 0.35086(12) 0.42243(11) 0.58803(8) 0.0361(3) Uani 1 1 d . . .
Si6 Si 0.31471(12) 0.33779(11) 0.43820(8) 0.0368(4) Uani 1 1 d . . .
K1 K 0.09725(9) 1.10014(7) 0.86118(6) 0.0341(3) Uani 1 1 d . . .
K2 K 0.25199(10) 0.74810(8) 0.62749(6) 0.0413(3) Uani 1 1 d . . .
O1 O 0.1661(2) 1.0276(2) 0.97494(16) 0.0273(7) Uani 1 1 d . . .
O2 O -0.0284(2) 0.9454(2) 0.88449(16) 0.0272(7) Uani 1 1 d . . .
O3 O 0.0302(3) 0.8501(2) 1.01305(17) 0.0312(8) Uani 1 1 d . . .
O4 O 0.1907(3) 0.9707(2) 0.82098(16) 0.0286(8) Uani 1 1 d . . .
O5 O 0.2262(3) 1.1035(3) 1.10420(18) 0.0437(10) Uani 1 1 d . . .
N1 N 0.3524(3) 1.0414(3) 0.7253(2) 0.0344(10) Uani 1 1 d . . .
N2 N 0.2105(3) 1.0362(3) 0.6604(2) 0.0317(10) Uani 1 1 d . . .
N3 N 0.2177(3) 0.9028(3) 0.7170(2) 0.0270(9) Uani 1 1 d . . .
N4 N 0.2264(3) 0.6434(3) 0.9569(2) 0.0309(10) Uani 1 1 d . . .
N5 N 0.0692(3) 0.5962(3) 0.9083(2) 0.0285(9) Uani 1 1 d . . .
N6 N 0.1211(3) 0.7565(3) 0.9627(2) 0.0278(9) Uani 1 1 d . . .
N7 N 0.1502(3) 0.8154(3) 0.7998(2) 0.0293(10) Uani 1 1 d . . .
N8 N 0.2820(3) 0.7342(3) 0.4947(2) 0.0337(10) Uani 1 1 d . . .
N9 N 0.3722(3) 0.4079(3) 0.5078(2) 0.0357(11) Uani 1 1 d . . .
N10 N -0.0447(3) 1.2893(3) 0.9448(2) 0.0330(10) Uani 1 1 d . . .
C1 C 0.0245(4) 1.2854(3) 0.8991(3) 0.0322(12) Uani 1 1 d . . .
C2 C 0.1290(4) 1.2995(4) 0.9191(3) 0.0372(13) Uani 1 1 d . . .
H2 H 0.1532 1.3045 0.9649 0.045 Uiso 1 1 calc R . .
C3 C 0.1976(5) 1.3062(4) 0.8727(3) 0.0425(14) Uani 1 1 d . . .
H3 H 0.2668 1.3161 0.8877 0.051 Uiso 1 1 calc R . .
C4 C 0.1642(5) 1.2981(4) 0.8040(3) 0.0495(16) Uani 1 1 d . . .
H4 H 0.2102 1.3021 0.7728 0.059 Uiso 1 1 calc R . .
C5 C 0.0606(5) 1.2839(4) 0.7828(3) 0.0476(16) Uani 1 1 d . . .
H5 H 0.0371 1.2785 0.7370 0.057 Uiso 1 1 calc R . .
C6 C -0.0085(5) 1.2778(4) 0.8294(3) 0.0378(13) Uani 1 1 d . . .
H6 H -0.0775 1.2686 0.8141 0.045 Uiso 1 1 calc R . .
C7 C -0.1653(4) 1.0414(4) 0.8173(3) 0.0454(15) Uani 1 1 d . . .
H7A H -0.1541 1.0882 0.8557 0.068 Uiso 1 1 calc R . .
H7B H -0.2341 1.0323 0.7960 0.068 Uiso 1 1 calc R . .
H7C H -0.1197 1.0608 0.7858 0.068 Uiso 1 1 calc R . .
C8 C -0.1685(4) 0.8408(4) 0.7700(3) 0.0392(13) Uani 1 1 d . . .
H8A H -0.1197 0.8569 0.7397 0.059 Uiso 1 1 calc R . .
H8B H -0.2355 0.8379 0.7474 0.059 Uiso 1 1 calc R . .
H8C H -0.1640 0.7815 0.7839 0.059 Uiso 1 1 calc R . .
C9 C 0.3600(4) 1.0107(4) 1.0405(3) 0.0473(15) Uani 1 1 d . . .
H9A H 0.3319 0.9532 1.0559 0.071 Uiso 1 1 calc R . .
H9B H 0.4154 1.0447 1.0731 0.071 Uiso 1 1 calc R . .
H9C H 0.3841 0.9983 0.9980 0.071 Uiso 1 1 calc R . .
C10 C 0.3232(4) 1.1948(4) 1.0076(3) 0.0441(14) Uani 1 1 d . . .
H10A H 0.3418 1.1867 0.9629 0.066 Uiso 1 1 calc R . .
H10B H 0.3830 1.2201 1.0394 0.066 Uiso 1 1 calc R . .
H10C H 0.2772 1.2365 1.0091 0.066 Uiso 1 1 calc R . .
C11 C 0.0607(4) 0.7721(3) 1.0126(3) 0.0307(11) Uani 1 1 d . . .
C12 C 0.1861(4) 0.8969(3) 0.7788(2) 0.0279(11) Uani 1 1 d . . .
C13 C 0.1356(4) 0.6700(3) 0.9459(2) 0.0273(11) Uani 1 1 d . . .
C14 C 0.1197(4) 0.5243(4) 0.8977(3) 0.0340(12) Uani 1 1 d . . .
H14 H 0.0914 0.4658 0.8743 0.041 Uiso 1 1 calc R . .
C15 C 0.2159(4) 0.5532(4) 0.9267(3) 0.0341(12) Uani 1 1 d . . .
H15 H 0.2666 0.5190 0.9265 0.041 Uiso 1 1 calc R . .
C16 C -0.0424(4) 0.5834(4) 0.8844(3) 0.0306(11) Uani 1 1 d . . .
C17 C -0.0743(4) 0.6750(4) 0.8756(3) 0.0369(13) Uani 1 1 d . . .
H17A H -0.0697 0.7103 0.9191 0.055 Uiso 1 1 calc R . .
H17B H -0.1430 0.6629 0.8535 0.055 Uiso 1 1 calc R . .
H17C H -0.0302 0.7094 0.8486 0.055 Uiso 1 1 calc R . .
C18 C -0.0659(4) 0.5243(4) 0.8148(3) 0.0394(13) Uani 1 1 d . . .
H18A H -0.0240 0.5536 0.7843 0.059 Uiso 1 1 calc R . .
H18B H -0.1361 0.5187 0.7975 0.059 Uiso 1 1 calc R . .
H18C H -0.0524 0.4638 0.8191 0.059 Uiso 1 1 calc R . .
C19 C -0.1005(4) 0.5322(4) 0.9352(3) 0.0389(13) Uani 1 1 d . . .
H19A H -0.0861 0.4713 0.9350 0.058 Uiso 1 1 calc R . .
H19B H -0.1721 0.5273 0.9229 0.058 Uiso 1 1 calc R . .
H19C H -0.0798 0.5660 0.9796 0.058 Uiso 1 1 calc R . .
C20 C 0.3231(4) 0.7019(4) 0.9952(3) 0.0369(13) Uani 1 1 d . . .
C21 C 0.3609(4) 0.7803(4) 0.9546(3) 0.0451(15) Uani 1 1 d . . .
H21A H 0.3742 0.7545 0.9114 0.068 Uiso 1 1 calc R . .
H21B H 0.4222 0.8189 0.9787 0.068 Uiso 1 1 calc R . .
H21C H 0.3101 0.8167 0.9480 0.068 Uiso 1 1 calc R . .
C22 C 0.3030(5) 0.7385(4) 1.0656(3) 0.0460(15) Uani 1 1 d . . .
H22A H 0.2557 0.7788 1.0612 0.069 Uiso 1 1 calc R . .
H22B H 0.3655 0.7723 1.0914 0.069 Uiso 1 1 calc R . .
H22C H 0.2751 0.6874 1.0882 0.069 Uiso 1 1 calc R . .
C23 C 0.4023(5) 0.6418(4) 1.0028(3) 0.0502(16) Uani 1 1 d . . .
H23A H 0.3770 0.5901 1.0258 0.075 Uiso 1 1 calc R . .
H23B H 0.4638 0.6780 1.0285 0.075 Uiso 1 1 calc R . .
H23C H 0.4160 0.6193 0.9589 0.075 Uiso 1 1 calc R . .
C24 C 0.2576(4) 0.9884(3) 0.7042(2) 0.0279(11) Uani 1 1 d . . .
C25 C 0.2758(5) 1.1197(4) 0.6562(3) 0.0438(14) Uani 1 1 d . . .
H25 H 0.2617 1.1652 0.6303 0.053 Uiso 1 1 calc R . .
C26 C 0.3619(5) 1.1228(4) 0.6959(3) 0.0443(15) Uani 1 1 d . . .
H26 H 0.4186 1.1711 0.7027 0.053 Uiso 1 1 calc R . .
C27 C 0.1026(4) 1.0081(4) 0.6272(3) 0.0347(12) Uani 1 1 d . . .
C28 C 0.0822(5) 1.0780(4) 0.5788(3) 0.0491(16) Uani 1 1 d . . .
H28A H 0.0926 1.1386 0.6038 0.074 Uiso 1 1 calc R . .
H28B H 0.0134 1.0601 0.5568 0.074 Uiso 1 1 calc R . .
H28C H 0.1278 1.0789 0.5454 0.074 Uiso 1 1 calc R . .
C29 C 0.0851(4) 0.9122(4) 0.5871(3) 0.0404(14) Uani 1 1 d . . .
H29A H 0.1330 0.9122 0.5553 0.061 Uiso 1 1 calc R . .
H29B H 0.0174 0.8964 0.5633 0.061 Uiso 1 1 calc R . .
H29C H 0.0939 0.8675 0.6174 0.061 Uiso 1 1 calc R . .
C30 C 0.0325(4) 1.0102(4) 0.6818(3) 0.0441(14) Uani 1 1 d . . .
H30A H 0.0462 0.9679 0.7131 0.066 Uiso 1 1 calc R . .
H30B H -0.0370 0.9922 0.6612 0.066 Uiso 1 1 calc R . .
H30C H 0.0443 1.0718 0.7055 0.066 Uiso 1 1 calc R . .
C31 C 0.4356(4) 1.0253(4) 0.7761(3) 0.0414(14) Uani 1 1 d . . .
C32 C 0.4291(5) 0.9223(5) 0.7810(3) 0.0551(18) Uani 1 1 d . . .
H32A H 0.3692 0.8980 0.8001 0.083 Uiso 1 1 calc R . .
H32B H 0.4880 0.9143 0.8092 0.083 Uiso 1 1 calc R . .
H32C H 0.4261 0.8898 0.7366 0.083 Uiso 1 1 calc R . .
C33 C 0.4260(5) 1.0772(5) 0.8445(3) 0.0510(16) Uani 1 1 d . . .
H33A H 0.4313 1.1420 0.8405 0.076 Uiso 1 1 calc R . .
H33B H 0.4792 1.0697 0.8779 0.076 Uiso 1 1 calc R . .
H33C H 0.3613 1.0525 0.8579 0.076 Uiso 1 1 calc R . .
C34 C 0.5378(5) 1.0642(6) 0.7532(4) 0.066(2) Uani 1 1 d . . .
H34A H 0.5392 1.0365 0.7080 0.099 Uiso 1 1 calc R . .
H34B H 0.5917 1.0502 0.7830 0.099 Uiso 1 1 calc R . .
H34C H 0.5466 1.1302 0.7542 0.099 Uiso 1 1 calc R . .
C35 C 0.1318(4) 0.7332(3) 0.7549(2) 0.0279(11) Uani 1 1 d . . .
C36 C 0.1854(4) 0.6639(4) 0.7673(3) 0.0330(12) Uani 1 1 d . . .
H36 H 0.2360 0.6743 0.8042 0.040 Uiso 1 1 calc R . .
C37 C 0.1650(4) 0.5791(4) 0.7255(3) 0.0378(13) Uani 1 1 d . . .
H37 H 0.2017 0.5339 0.7345 0.045 Uiso 1 1 calc R . .
C38 C 0.0895(5) 0.5631(4) 0.6704(3) 0.0401(14) Uani 1 1 d . . .
H38 H 0.0760 0.5073 0.6419 0.048 Uiso 1 1 calc R . .
C39 C 0.0345(4) 0.6306(4) 0.6580(3) 0.0387(13) Uani 1 1 d . . .
H39 H -0.0163 0.6197 0.6213 0.046 Uiso 1 1 calc R . .
C40 C 0.0545(4) 0.7141(4) 0.6998(3) 0.0345(12) Uani 1 1 d . . .
H40 H 0.0160 0.7582 0.6912 0.041 Uiso 1 1 calc R . .
C41 C 0.4126(5) 0.9048(4) 0.5672(3) 0.0534(17) Uani 1 1 d . . .
H41A H 0.3613 0.9258 0.5903 0.080 Uiso 1 1 calc R . .
H41B H 0.4623 0.9573 0.5600 0.080 Uiso 1 1 calc R . .
H41C H 0.4449 0.8661 0.5942 0.080 Uiso 1 1 calc R . .
C42 C 0.4594(5) 0.8230(4) 0.4325(3) 0.0549(18) Uani 1 1 d . . .
H42A H 0.5023 0.7878 0.4549 0.082 Uiso 1 1 calc R . .
H42B H 0.4984 0.8831 0.4285 0.082 Uiso 1 1 calc R . .
H42C H 0.4317 0.7912 0.3883 0.082 Uiso 1 1 calc R . .
C43 C 0.2848(6) 0.9174(5) 0.4378(4) 0.068(2) Uani 1 1 d . . .
H43A H 0.2570 0.8885 0.3928 0.102 Uiso 1 1 calc R . .
H43B H 0.3321 0.9740 0.4355 0.102 Uiso 1 1 calc R . .
H43C H 0.2310 0.9309 0.4619 0.102 Uiso 1 1 calc R . .
C44 C 0.3716(5) 0.5497(4) 0.6224(3) 0.0452(15) Uani 1 1 d . . .
H44A H 0.4390 0.5804 0.6173 0.068 Uiso 1 1 calc R . .
H44B H 0.3632 0.5554 0.6694 0.068 Uiso 1 1 calc R . .
H44C H 0.3230 0.5776 0.5979 0.068 Uiso 1 1 calc R . .
C45 C 0.2203(5) 0.3706(4) 0.6063(3) 0.0489(16) Uani 1 1 d . . .
H45A H 0.1709 0.3953 0.5798 0.073 Uiso 1 1 calc R . .
H45B H 0.2161 0.3855 0.6534 0.073 Uiso 1 1 calc R . .
H45C H 0.2073 0.3044 0.5949 0.073 Uiso 1 1 calc R . .
C46 C 0.4383(5) 0.3754(5) 0.6489(3) 0.0540(17) Uani 1 1 d . . .
H46A H 0.4381 0.3121 0.6327 0.081 Uiso 1 1 calc R . .
H46B H 0.4154 0.3784 0.6925 0.081 Uiso 1 1 calc R . .
H46C H 0.5060 0.4118 0.6526 0.081 Uiso 1 1 calc R . .
C47 C 0.1379(5) 0.5571(4) 0.4773(3) 0.0488(16) Uani 1 1 d . . .
H47A H 0.1902 0.5219 0.4756 0.073 Uiso 1 1 calc R . .
H47B H 0.0768 0.5228 0.4501 0.073 Uiso 1 1 calc R . .
H47C H 0.1253 0.5688 0.5232 0.073 Uiso 1 1 calc R . .
C48 C 0.0655(5) 0.7261(5) 0.4377(4) 0.074(2) Uani 1 1 d . . .
H48A H 0.0437 0.7342 0.4814 0.111 Uiso 1 1 calc R . .
H48B H 0.0116 0.6867 0.4066 0.111 Uiso 1 1 calc R . .
H48C H 0.0830 0.7853 0.4219 0.111 Uiso 1 1 calc R . .
C49 C 0.2005(6) 0.6430(5) 0.3533(3) 0.063(2) Uani 1 1 d . . .
H49A H 0.2156 0.6994 0.3333 0.094 Uiso 1 1 calc R . .
H49B H 0.1401 0.6037 0.3285 0.094 Uiso 1 1 calc R . .
H49C H 0.2561 0.6118 0.3519 0.094 Uiso 1 1 calc R . .
C50 C 0.2967(5) 0.4036(4) 0.3635(3) 0.0525(17) Uani 1 1 d . . .
H50A H 0.2535 0.4463 0.3729 0.079 Uiso 1 1 calc R . .
H50B H 0.2661 0.3607 0.3241 0.079 Uiso 1 1 calc R . .
H50C H 0.3614 0.4373 0.3556 0.079 Uiso 1 1 calc R . .
C51 C 0.3884(5) 0.2486(4) 0.4088(3) 0.0534(17) Uani 1 1 d . . .
H51A H 0.4562 0.2791 0.4044 0.080 Uiso 1 1 calc R . .
H51B H 0.3556 0.2159 0.3658 0.080 Uiso 1 1 calc R . .
H51C H 0.3909 0.2055 0.4412 0.080 Uiso 1 1 calc R . .
C52 C 0.1848(5) 0.2662(5) 0.4424(3) 0.0597(19) Uani 1 1 d . . .
H52A H 0.1905 0.2212 0.4729 0.090 Uiso 1 1 calc R . .
H52B H 0.1558 0.2351 0.3982 0.090 Uiso 1 1 calc R . .
H52C H 0.1419 0.3060 0.4582 0.090 Uiso 1 1 calc R . .
C53 C 0.4425(6) 0.5663(7) 0.8181(4) 0.075(2) Uani 1 1 d . . .
H53 H 0.3876 0.5956 0.8163 0.090 Uiso 1 1 calc R . .
C54 C 0.4300(9) 0.4758(8) 0.8312(5) 0.100(3) Uani 1 1 d . . .
H54 H 0.3658 0.4454 0.8381 0.120 Uiso 1 1 calc R . .
C55 C 0.5074(13) 0.4278(9) 0.8347(5) 0.126(5) Uani 1 1 d . . .
H55 H 0.4972 0.3668 0.8441 0.151 Uiso 1 1 calc R . .
C56 C 0.6028(11) 0.4764(13) 0.8232(7) 0.157(6) Uani 1 1 d . . .
H56 H 0.6575 0.4469 0.8234 0.189 Uiso 1 1 calc R . .
C57 C 0.6147(8) 0.5680(10) 0.8116(6) 0.124(5) Uani 1 1 d . . .
H57 H 0.6787 0.6003 0.8061 0.149 Uiso 1 1 calc R . .
C58 C 0.5346(7) 0.6126(7) 0.8079(4) 0.085(3) Uani 1 1 d . . .
C59 C 0.5496(9) 0.7089(7) 0.7929(5) 0.128(4) Uani 1 1 d . . .
H59A H 0.4896 0.7324 0.7990 0.193 Uiso 1 1 calc R . .
H59B H 0.5628 0.7109 0.7470 0.193 Uiso 1 1 calc R . .
H59C H 0.6063 0.7462 0.8229 0.193 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
Ca1 O1 2.329(3) . ?
Ca1 O1 2.329(3) 2_577 ?
Ca1 O2 2.339(3) . ?
Ca1 O2 2.339(3) 2_577 ?
Ca1 O3 2.370(3) 2_577 ?
Ca1 O3 2.370(3) . ?
Ca1 Ca2 3.1530(10) . ?
Ca1 Ca2 3.1530(10) 2_577 ?
Ca1 Si2 3.4064(14) . ?
Ca1 Si2 3.4064(14) 2_577 ?
Ca1 Si1 3.4606(14) . ?
Ca1 Si1 3.4606(14) 2_577 ?
Ca2 O2 2.290(3) . ?
Ca2 O1 2.332(3) . ?
Ca2 N6 2.372(4) . ?
Ca2 O4 2.389(3) . ?
Ca2 N7 2.390(4) . ?
Ca2 O3 2.635(4) . ?
Ca2 C12 2.804(5) . ?
Ca2 C11 2.965(5) . ?
Ca2 K1 3.4059(15) . ?
Ca3 N9 2.858(5) 2_666 ?
Ca3 N9 2.861(5) . ?
Ca3 N8 3.030(5) . ?
Ca3 Si5 3.589(2) 2_666 ?
Ca3 Si5 3.607(2) . ?
Ca3 Si4 3.614(2) . ?
Ca3 Ca3 4.051(2) 2_666 ?
Ca3 K2 4.6186(17) . ?
Si1 O1 1.606(3) . ?
Si1 O5 1.634(4) . ?
Si1 C9 1.859(6) . ?
Si1 C10 1.865(6) . ?
Si1 K1 3.9010(18) . ?
Si2 O2 1.608(3) . ?
Si2 O5 1.646(4) 2_577 ?
Si2 C8 1.864(5) . ?
Si2 C7 1.868(6) . ?
Si2 K1 3.6573(19) . ?
Si3 N8 1.677(5) . ?
Si3 C41 1.887(6) . ?
Si3 C42 1.890(6) . ?
Si3 C43 1.893(7) . ?
Si3 K2 3.594(2) . ?
Si4 N8 1.675(5) . ?
Si4 C48 1.885(7) . ?
Si4 C47 1.888(6) . ?
Si4 C49 1.891(6) . ?
Si4 K2 3.703(2) . ?
Si5 N9 1.668(5) . ?
Si5 C45 1.878(6) . ?
Si5 C46 1.887(6) . ?
Si5 C44 1.896(6) . ?
Si5 Ca3 3.589(2) 2_666 ?
Si6 N9 1.667(5) . ?
Si6 C52 1.886(6) . ?
Si6 C50 1.890(6) . ?
Si6 C51 1.892(6) . ?
K1 O4 2.606(3) . ?
K1 O2 2.694(4) . ?
K1 O1 2.768(3) . ?
K1 C2 2.992(5) . ?
K1 C3 3.066(6) . ?
K1 C1 3.143(5) . ?
K1 C4 3.262(6) . ?
K1 O3 3.314(4) 2_577 ?
K1 C6 3.317(6) . ?
K1 C5 3.372(6) . ?
K2 N8 2.734(4) . ?
K2 N3 2.907(4) . ?
K2 C40 3.165(6) . ?
K2 C35 3.186(5) . ?
K2 C39 3.274(6) . ?
K2 C36 3.331(5) . ?
K2 C38 3.416(6) . ?
K2 C37 3.452(6) . ?
O3 C11 1.301(6) . ?
O3 K1 3.314(4) 2_577 ?
O4 C12 1.299(6) . ?
O5 Si2 1.646(4) 2_577 ?
N1 C24 1.366(6) . ?
N1 C26 1.387(7) . ?
N1 C31 1.505(7) . ?
N2 C24 1.365(6) . ?
N2 C25 1.390(7) . ?
N2 C27 1.498(7) . ?
N3 C24 1.342(6) . ?
N3 C12 1.362(6) . ?
N4 C13 1.366(6) . ?
N4 C15 1.383(6) . ?
N4 C20 1.502(7) . ?
N5 C13 1.368(6) . ?
N5 C14 1.385(6) . ?
N5 C16 1.504(6) . ?
N6 C13 1.349(6) . ?
N6 C11 1.390(6) . ?
N7 C12 1.341(6) . ?
N7 C35 1.402(6) . ?
N9 Ca3 2.858(5) 2_666 ?
N10 C11 1.316(6) 2_577 ?
N10 C1 1.387(7) . ?
C1 C2 1.397(8) . ?
C1 C6 1.408(7) . ?
C2 C3 1.386(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.388(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.389(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.391(8) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N10 1.316(6) 2_577 ?
C14 C15 1.335(7) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.523(7) . ?
C16 C19 1.531(7) . ?
C16 C18 1.536(7) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C23 1.528(8) . ?
C20 C21 1.529(8) . ?
C20 C22 1.533(8) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C25 C26 1.327(8) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 C29 1.522(7) . ?
C27 C30 1.531(8) . ?
C27 C28 1.534(7) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C32 1.526(8) . ?
C31 C34 1.533(8) . ?
C31 C33 1.534(8) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 C36 1.396(7) . ?
C35 C40 1.401(7) . ?
C36 C37 1.398(7) . ?
C36 H36 0.9300 . ?
C37 C38 1.387(8) . ?
C37 H37 0.9300 . ?
C38 C39 1.385(8) . ?
C38 H38 0.9300 . ?
C39 C40 1.383(7) . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C53 C58 1.350(11) . ?
C53 C54 1.375(13) . ?
C53 H53 0.9300 . ?
C54 C55 1.376(15) . ?
C54 H54 0.9300 . ?
C55 C56 1.408(17) . ?
C55 H55 0.9300 . ?
C56 C57 1.383(18) . ?
C56 H56 0.9300 . ?
C57 C58 1.376(14) . ?
C57 H57 0.9300 . ?
C58 C59 1.469(13) . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ca1 O1 180.000(1) . 2_577 ?
O1 Ca1 O2 79.75(11) . . ?
O1 Ca1 O2 100.25(11) 2_577 . ?
O1 Ca1 O2 100.25(11) . 2_577 ?
O1 Ca1 O2 79.75(11) 2_577 2_577 ?
O2 Ca1 O2 180.000(1) . 2_577 ?
O1 Ca1 O3 96.78(12) . 2_577 ?
O1 Ca1 O3 83.22(12) 2_577 2_577 ?
O2 Ca1 O3 95.56(11) . 2_577 ?
O2 Ca1 O3 84.44(11) 2_577 2_577 ?
O1 Ca1 O3 83.22(12) . . ?
O1 Ca1 O3 96.78(12) 2_577 . ?
O2 Ca1 O3 84.44(11) . . ?
O2 Ca1 O3 95.56(11) 2_577 . ?
O3 Ca1 O3 180.000(1) 2_577 . ?
O1 Ca1 Ca2 47.47(8) . . ?
O1 Ca1 Ca2 132.53(8) 2_577 . ?
O2 Ca1 Ca2 46.41(8) . . ?
O2 Ca1 Ca2 133.59(8) 2_577 . ?
O3 Ca1 Ca2 125.20(9) 2_577 . ?
O3 Ca1 Ca2 54.80(9) . . ?
O1 Ca1 Ca2 132.53(8) . 2_577 ?
O1 Ca1 Ca2 47.47(8) 2_577 2_577 ?
O2 Ca1 Ca2 133.59(8) . 2_577 ?
O2 Ca1 Ca2 46.41(8) 2_577 2_577 ?
O3 Ca1 Ca2 54.80(9) 2_577 2_577 ?
O3 Ca1 Ca2 125.20(9) . 2_577 ?
Ca2 Ca1 Ca2 180.0 . 2_577 ?
O1 Ca1 Si2 103.41(8) . . ?
O1 Ca1 Si2 76.59(8) 2_577 . ?
O2 Ca1 Si2 24.60(8) . . ?
O2 Ca1 Si2 155.40(8) 2_577 . ?
O3 Ca1 Si2 86.19(9) 2_577 . ?
O3 Ca1 Si2 93.81(9) . . ?
Ca2 Ca1 Si2 69.53(3) . . ?
Ca2 Ca1 Si2 110.47(3) 2_577 . ?
O1 Ca1 Si2 76.59(8) . 2_577 ?
O1 Ca1 Si2 103.41(8) 2_577 2_577 ?
O2 Ca1 Si2 155.40(8) . 2_577 ?
O2 Ca1 Si2 24.60(8) 2_577 2_577 ?
O3 Ca1 Si2 93.81(9) 2_577 2_577 ?
O3 Ca1 Si2 86.19(9) . 2_577 ?
Ca2 Ca1 Si2 110.47(3) . 2_577 ?
Ca2 Ca1 Si2 69.53(3) 2_577 2_577 ?
Si2 Ca1 Si2 180.000(1) . 2_577 ?
O1 Ca1 Si1 23.14(8) . . ?
O1 Ca1 Si1 156.86(8) 2_577 . ?
O2 Ca1 Si1 102.80(9) . . ?
O2 Ca1 Si1 77.20(9) 2_577 . ?
O3 Ca1 Si1 92.49(9) 2_577 . ?
O3 Ca1 Si1 87.51(9) . . ?
Ca2 Ca1 Si1 67.73(3) . . ?
Ca2 Ca1 Si1 112.27(3) 2_577 . ?
Si2 Ca1 Si1 125.97(3) . . ?
Si2 Ca1 Si1 54.03(3) 2_577 . ?
O1 Ca1 Si1 156.86(8) . 2_577 ?
O1 Ca1 Si1 23.14(8) 2_577 2_577 ?
O2 Ca1 Si1 77.20(9) . 2_577 ?
O2 Ca1 Si1 102.80(8) 2_577 2_577 ?
O3 Ca1 Si1 87.51(9) 2_577 2_577 ?
O3 Ca1 Si1 92.49(9) . 2_577 ?
Ca2 Ca1 Si1 112.27(3) . 2_577 ?
Ca2 Ca1 Si1 67.73(3) 2_577 2_577 ?
Si2 Ca1 Si1 54.03(3) . 2_577 ?
Si2 Ca1 Si1 125.97(3) 2_577 2_577 ?
Si1 Ca1 Si1 180.0 . 2_577 ?
O2 Ca2 O1 80.71(12) . . ?
O2 Ca2 N6 123.15(14) . . ?
O1 Ca2 N6 112.95(13) . . ?
O2 Ca2 O4 90.77(12) . . ?
O1 Ca2 O4 85.02(12) . . ?
N6 Ca2 O4 142.79(14) . . ?
O2 Ca2 N7 108.94(14) . . ?
O1 Ca2 N7 139.10(14) . . ?
N6 Ca2 N7 95.12(14) . . ?
O4 Ca2 N7 55.99(12) . . ?
O2 Ca2 O3 79.64(11) . . ?
O1 Ca2 O3 77.57(11) . . ?
N6 Ca2 O3 53.38(12) . . ?
O4 Ca2 O3 161.23(11) . . ?
N7 Ca2 O3 142.48(13) . . ?
O2 Ca2 C12 100.04(13) . . ?
O1 Ca2 C12 111.99(14) . . ?
N6 Ca2 C12 120.97(14) . . ?
O4 Ca2 C12 27.51(12) . . ?
N7 Ca2 C12 28.51(14) . . ?
O3 Ca2 C12 170.33(13) . . ?
O2 Ca2 C11 100.63(14) . . ?
O1 Ca2 C11 95.97(13) . . ?
N6 Ca2 C11 27.41(14) . . ?
O4 Ca2 C11 168.58(14) . . ?
N7 Ca2 C11 119.72(14) . . ?
O3 Ca2 C11 26.01(12) . . ?
C12 Ca2 C11 147.47(15) . . ?
O2 Ca2 Ca1 47.73(8) . . ?
O1 Ca2 Ca1 47.38(8) . . ?
N6 Ca2 Ca1 100.47(10) . . ?
O4 Ca2 Ca1 114.81(8) . . ?
N7 Ca2 Ca1 156.60(11) . . ?
O3 Ca2 Ca1 47.31(7) . . ?
C12 Ca2 Ca1 138.30(11) . . ?
C11 Ca2 Ca1 73.28(10) . . ?
O2 Ca2 K1 52.08(9) . . ?
O1 Ca2 K1 53.83(9) . . ?
N6 Ca2 K1 164.87(10) . . ?
O4 Ca2 K1 49.74(8) . . ?
N7 Ca2 K1 99.98(10) . . ?
O3 Ca2 K1 112.75(8) . . ?
C12 Ca2 K1 73.64(11) . . ?
C11 Ca2 K1 138.66(11) . . ?
Ca1 Ca2 K1 65.45(3) . . ?
N9 Ca3 N9 89.79(13) 2_666 . ?
N9 Ca3 N8 138.23(13) 2_666 . ?
N9 Ca3 N8 125.54(13) . . ?
N9 Ca3 Si5 27.08(9) 2_666 2_666 ?
N9 Ca3 Si5 95.54(10) . 2_666 ?
N8 Ca3 Si5 138.85(9) . 2_666 ?
N9 Ca3 Si5 95.20(10) 2_666 . ?
N9 Ca3 Si5 26.86(9) . . ?
N8 Ca3 Si5 107.63(9) . . ?
Si5 Ca3 Si5 111.47(4) 2_666 . ?
N9 Ca3 Si4 161.52(10) 2_666 . ?
N9 Ca3 Si4 108.68(10) . . ?
N8 Ca3 Si4 27.45(9) . . ?
Si5 Ca3 Si4 143.95(5) 2_666 . ?
Si5 Ca3 Si4 101.61(5) . . ?
N9 Ca3 Ca3 44.93(9) 2_666 2_666 ?
N9 Ca3 Ca3 44.87(9) . 2_666 ?
N8 Ca3 Ca3 159.50(10) . 2_666 ?
Si5 Ca3 Ca3 55.95(4) 2_666 2_666 ?
Si5 Ca3 Ca3 55.52(4) . 2_666 ?
Si4 Ca3 Ca3 153.54(6) . 2_666 ?
N9 Ca3 K2 125.98(10) 2_666 . ?
N9 Ca3 K2 102.90(9) . . ?
N8 Ca3 K2 34.60(8) . . ?
Si5 Ca3 K2 147.87(4) 2_666 . ?
Si5 Ca3 K2 78.47(4) . . ?
Si4 Ca3 K2 51.72(3) . . ?
Ca3 Ca3 K2 124.90(5) 2_666 . ?
O1 Si1 O5 112.20(19) . . ?
O1 Si1 C9 111.8(2) . . ?
O5 Si1 C9 107.2(3) . . ?
O1 Si1 C10 113.2(2) . . ?
O5 Si1 C10 105.1(3) . . ?
C9 Si1 C10 106.9(3) . . ?
O1 Si1 Ca1 34.75(12) . . ?
O5 Si1 Ca1 77.56(14) . . ?
C9 Si1 Ca1 127.5(2) . . ?
C10 Si1 Ca1 122.5(2) . . ?
O1 Si1 K1 36.03(13) . . ?
O5 Si1 K1 123.22(16) . . ?
C9 Si1 K1 126.7(2) . . ?
C10 Si1 K1 77.15(19) . . ?
Ca1 Si1 K1 57.32(3) . . ?
O2 Si2 O5 110.86(19) . 2_577 ?
O2 Si2 C8 113.4(2) . . ?
O5 Si2 C8 106.6(2) 2_577 . ?
O2 Si2 C7 110.1(2) . . ?
O5 Si2 C7 107.7(3) 2_577 . ?
C8 Si2 C7 107.9(3) . . ?
O2 Si2 Ca1 37.27(12) . . ?
O5 Si2 Ca1 79.19(13) 2_577 . ?
C8 Si2 Ca1 144.5(2) . . ?
C7 Si2 Ca1 103.23(19) . . ?
O2 Si2 K1 42.26(12) . . ?
O5 Si2 K1 136.22(14) 2_577 . ?
C8 Si2 K1 115.85(19) . . ?
C7 Si2 K1 69.72(19) . . ?
Ca1 Si2 K1 60.25(3) . . ?
N8 Si3 C41 110.3(3) . . ?
N8 Si3 C42 112.8(3) . . ?
C41 Si3 C42 106.8(3) . . ?
N8 Si3 C43 117.1(3) . . ?
C41 Si3 C43 105.2(3) . . ?
C42 Si3 C43 103.9(3) . . ?
N8 Si3 K2 46.78(15) . . ?
C41 Si3 K2 65.22(19) . . ?
C42 Si3 K2 138.0(2) . . ?
C43 Si3 K2 118.1(2) . . ?
N8 Si4 C48 114.8(3) . . ?
N8 Si4 C47 109.6(3) . . ?
C48 Si4 C47 105.8(3) . . ?
N8 Si4 C49 114.8(3) . . ?
C48 Si4 C49 104.1(4) . . ?
C47 Si4 C49 107.2(3) . . ?
N8 Si4 Ca3 56.49(16) . . ?
C48 Si4 Ca3 171.2(2) . . ?
C47 Si4 Ca3 77.7(2) . . ?
C49 Si4 Ca3 82.2(2) . . ?
N8 Si4 K2 43.22(15) . . ?
C48 Si4 K2 94.2(3) . . ?
C47 Si4 K2 80.59(19) . . ?
C49 Si4 K2 156.9(2) . . ?
Ca3 Si4 K2 78.28(4) . . ?
N9 Si5 C45 116.8(3) . . ?
N9 Si5 C46 114.5(3) . . ?
C45 Si5 C46 104.0(3) . . ?
N9 Si5 C44 111.8(2) . . ?
C45 Si5 C44 104.6(3) . . ?
C46 Si5 C44 103.8(3) . . ?
N9 Si5 Ca3 51.26(16) . 2_666 ?
C45 Si5 Ca3 152.2(2) . 2_666 ?
C46 Si5 Ca3 68.4(2) . 2_666 ?
C44 Si5 Ca3 103.23(19) . 2_666 ?
N9 Si5 Ca3 50.80(16) . . ?
C45 Si5 Ca3 127.1(2) . . ?
C46 Si5 Ca3 128.5(2) . . ?
C44 Si5 Ca3 61.07(18) . . ?
Ca3 Si5 Ca3 68.53(4) 2_666 . ?
N9 Si6 C52 117.0(3) . . ?
N9 Si6 C50 112.0(3) . . ?
C52 Si6 C50 104.8(3) . . ?
N9 Si6 C51 113.8(3) . . ?
C52 Si6 C51 103.5(3) . . ?
C50 Si6 C51 104.5(3) . . ?
O4 K1 O2 77.86(11) . . ?
O4 K1 O1 72.76(10) . . ?
O2 K1 O1 66.43(10) . . ?
O4 K1 C2 143.64(14) . . ?
O2 K1 C2 132.66(13) . . ?
O1 K1 C2 99.47(13) . . ?
O4 K1 C3 121.52(14) . . ?
O2 K1 C3 159.06(14) . . ?
O1 K1 C3 109.42(15) . . ?
C2 K1 C3 26.42(15) . . ?
O4 K1 C1 167.37(13) . . ?
O2 K1 C1 114.77(13) . . ?
O1 K1 C1 111.77(12) . . ?
C2 K1 C1 26.17(14) . . ?
C3 K1 C1 46.09(15) . . ?
O4 K1 C4 115.62(14) . . ?
O2 K1 C4 157.39(15) . . ?
O1 K1 C4 133.38(15) . . ?
C2 K1 C4 45.08(15) . . ?
C3 K1 C4 25.09(16) . . ?
C1 K1 C4 52.40(15) . . ?
O4 K1 O3 137.97(10) . 2_577 ?
O2 K1 O3 70.10(9) . 2_577 ?
O1 K1 O3 69.90(9) . 2_577 ?
C2 K1 O3 62.71(12) . 2_577 ?
C3 K1 O3 89.09(13) . 2_577 ?
C1 K1 O3 52.35(11) . 2_577 ?
C4 K1 O3 103.94(13) . 2_577 ?
O4 K1 C6 149.92(12) . . ?
O2 K1 C6 116.51(13) . . ?
O1 K1 C6 136.52(12) . . ?
C2 K1 C6 44.18(15) . . ?
C3 K1 C6 51.20(16) . . ?
C1 K1 C6 24.99(13) . . ?
C4 K1 C6 43.13(15) . . ?
O3 K1 C6 71.26(11) 2_577 . ?
O4 K1 C5 127.49(13) . . ?
O2 K1 C5 133.30(15) . . ?
O1 K1 C5 150.27(13) . . ?
C2 K1 C5 50.98(15) . . ?
C3 K1 C5 43.21(17) . . ?
C1 K1 C5 43.75(13) . . ?
C4 K1 C5 24.10(15) . . ?
O3 K1 C5 94.49(12) 2_577 . ?
C6 K1 C5 23.99(14) . . ?
O4 K1 Ca2 44.39(8) . . ?
O2 K1 Ca2 42.10(7) . . ?
O1 K1 Ca2 42.85(7) . . ?
C2 K1 Ca2 142.20(12) . . ?
C3 K1 Ca2 147.03(13) . . ?
C1 K1 Ca2 146.31(10) . . ?
C4 K1 Ca2 158.20(12) . . ?
O3 K1 Ca2 94.04(7) 2_577 . ?
C6 K1 Ca2 158.45(11) . . ?
C5 K1 Ca2 166.82(11) . . ?
O4 K1 Ca1 97.95(8) . . ?
O2 K1 Ca1 41.19(7) . . ?
O1 K1 Ca1 40.93(7) . . ?
C2 K1 Ca1 97.91(11) . . ?
C3 K1 Ca1 121.80(12) . . ?
C1 K1 Ca1 92.51(10) . . ?
C4 K1 Ca1 142.61(11) . . ?
O3 K1 Ca1 40.20(6) 2_577 . ?
C6 K1 Ca1 110.07(10) . . ?
C5 K1 Ca1 133.97(11) . . ?
Ca2 K1 Ca1 53.84(2) . . ?
N8 K2 N3 130.87(13) . . ?
N8 K2 C40 132.89(14) . . ?
N3 K2 C40 62.81(13) . . ?
N8 K2 C35 158.23(14) . . ?
N3 K2 C35 53.97(12) . . ?
C40 K2 C35 25.49(13) . . ?
N8 K2 C39 115.28(14) . . ?
N3 K2 C39 87.39(13) . . ?
C40 K2 C39 24.73(13) . . ?
C35 K2 C39 44.03(13) . . ?
N8 K2 C36 154.31(14) . . ?
N3 K2 C36 73.30(12) . . ?
C40 K2 C36 43.13(14) . . ?
C35 K2 C36 24.61(12) . . ?
C39 K2 C36 49.40(14) . . ?
N8 K2 C38 114.86(14) . . ?
N3 K2 C38 102.75(13) . . ?
C40 K2 C38 42.67(13) . . ?
C35 K2 C38 50.25(13) . . ?
C39 K2 C38 23.77(13) . . ?
C36 K2 C38 41.74(13) . . ?
N8 K2 C37 130.61(13) . . ?
N3 K2 C37 95.85(12) . . ?
C40 K2 C37 49.41(14) . . ?
C35 K2 C37 42.87(12) . . ?
C39 K2 C37 41.64(14) . . ?
C36 K2 C37 23.70(12) . . ?
C38 K2 C37 23.29(13) . . ?
N8 K2 Si3 26.55(9) . . ?
N3 K2 Si3 108.47(9) . . ?
C40 K2 Si3 143.32(11) . . ?
C35 K2 Si3 160.10(10) . . ?
C39 K2 Si3 136.25(11) . . ?
C36 K2 Si3 173.52(11) . . ?
C38 K2 Si3 141.18(10) . . ?
C37 K2 Si3 155.67(10) . . ?
N8 K2 Si4 24.81(10) . . ?
N3 K2 Si4 133.15(9) . . ?
C40 K2 Si4 108.95(11) . . ?
C35 K2 Si4 133.71(11) . . ?
C39 K2 Si4 90.51(10) . . ?
C36 K2 Si4 134.67(10) . . ?
C38 K2 Si4 92.95(10) . . ?
C37 K2 Si4 112.82(10) . . ?
Si3 K2 Si4 48.65(4) . . ?
N8 K2 Ca3 39.01(10) . . ?
N3 K2 Ca3 156.91(9) . . ?
C40 K2 Ca3 140.27(10) . . ?
C35 K2 Ca3 145.56(10) . . ?
C39 K2 Ca3 115.62(10) . . ?
C36 K2 Ca3 122.40(10) . . ?
C38 K2 Ca3 99.69(10) . . ?
C37 K2 Ca3 102.74(9) . . ?
Si3 K2 Ca3 54.00(3) . . ?
Si4 K2 Ca3 50.01(3) . . ?
Si1 O1 Ca1 122.11(17) . . ?
Si1 O1 Ca2 138.7(2) . . ?
Ca1 O1 Ca2 85.15(11) . . ?
Si1 O1 K1 124.03(17) . . ?
Ca1 O1 K1 87.91(11) . . ?
Ca2 O1 K1 83.32(10) . . ?
Si2 O2 Ca2 147.47(19) . . ?
Si2 O2 Ca1 118.13(18) . . ?
Ca2 O2 Ca1 85.86(11) . . ?
Si2 O2 K1 114.08(17) . . ?
Ca2 O2 K1 85.82(11) . . ?
Ca1 O2 K1 89.49(11) . . ?
C11 O3 Ca1 168.6(3) . . ?
C11 O3 Ca2 91.3(3) . . ?
Ca1 O3 Ca2 77.89(10) . . ?
C11 O3 K1 115.5(3) . 2_577 ?
Ca1 O3 K1 75.31(9) . 2_577 ?
Ca2 O3 K1 153.19(13) . 2_577 ?
C12 O4 Ca2 94.4(3) . . ?
C12 O4 K1 145.9(3) . . ?
Ca2 O4 K1 85.87(11) . . ?
Si1 O5 Si2 144.0(2) . 2_577 ?
C24 N1 C26 108.9(4) . . ?
C24 N1 C31 129.5(4) . . ?
C26 N1 C31 121.4(5) . . ?
C24 N2 C25 108.9(4) . . ?
C24 N2 C27 125.7(4) . . ?
C25 N2 C27 125.1(4) . . ?
C24 N3 C12 115.9(4) . . ?
C24 N3 K2 117.0(3) . . ?
C12 N3 K2 125.2(3) . . ?
C13 N4 C15 109.1(4) . . ?
C13 N4 C20 126.1(4) . . ?
C15 N4 C20 124.9(4) . . ?
C13 N5 C14 108.5(4) . . ?
C13 N5 C16 130.3(4) . . ?
C14 N5 C16 121.1(4) . . ?
C13 N6 C11 119.4(4) . . ?
C13 N6 Ca2 134.8(3) . . ?
C11 N6 Ca2 100.8(3) . . ?
C12 N7 C35 120.1(4) . . ?
C12 N7 Ca2 93.2(3) . . ?
C35 N7 Ca2 145.3(3) . . ?
Si4 N8 Si3 127.6(3) . . ?
Si4 N8 K2 112.0(2) . . ?
Si3 N8 K2 106.7(2) . . ?
Si4 N8 Ca3 96.06(18) . . ?
Si3 N8 Ca3 105.7(2) . . ?
K2 N8 Ca3 106.39(15) . . ?
Si6 N9 Si5 135.3(3) . . ?
Si6 N9 Ca3 109.1(2) . 2_666 ?
Si5 N9 Ca3 101.7(2) . 2_666 ?
Si6 N9 Ca3 109.1(2) . . ?
Si5 N9 Ca3 102.3(2) . . ?
Ca3 N9 Ca3 90.21(13) 2_666 . ?
C11 N10 C1 122.0(5) 2_577 . ?
N10 C1 C2 122.8(5) . . ?
N10 C1 C6 119.8(5) . . ?
C2 C1 C6 117.0(5) . . ?
N10 C1 K1 120.4(3) . . ?
C2 C1 K1 70.9(3) . . ?
C6 C1 K1 84.4(3) . . ?
C3 C2 C1 121.8(5) . . ?
C3 C2 K1 79.7(3) . . ?
C1 C2 K1 83.0(3) . . ?
C3 C2 H2 119.1 . . ?
C1 C2 H2 119.1 . . ?
K1 C2 H2 108.0 . . ?
C2 C3 C4 120.7(6) . . ?
C2 C3 K1 73.8(3) . . ?
C4 C3 K1 85.4(4) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
K1 C3 H3 111.2 . . ?
C3 C4 C5 118.6(6) . . ?
C3 C4 K1 69.5(3) . . ?
C5 C4 K1 82.4(4) . . ?
C3 C4 H4 120.7 . . ?
C5 C4 H4 120.7 . . ?
K1 C4 H4 118.2 . . ?
C4 C5 C6 120.9(6) . . ?
C4 C5 K1 73.5(3) . . ?
C6 C5 K1 75.8(3) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
K1 C5 H5 122.5 . . ?
C5 C6 C1 121.0(6) . . ?
C5 C6 K1 80.2(4) . . ?
C1 C6 K1 70.6(3) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
K1 C6 H6 120.7 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si1 C9 H9A 109.5 . . ?
Si1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si1 C10 H10A 109.5 . . ?
Si1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O3 C11 N10 127.4(5) . 2_577 ?
O3 C11 N6 114.4(4) . . ?
N10 C11 N6 118.2(5) 2_577 . ?
O3 C11 Ca2 62.7(3) . . ?
N10 C11 Ca2 169.9(4) 2_577 . ?
N6 C11 Ca2 51.8(2) . . ?
O4 C12 N7 116.4(4) . . ?
O4 C12 N3 121.4(4) . . ?
N7 C12 N3 122.3(4) . . ?
O4 C12 Ca2 58.1(2) . . ?
N7 C12 Ca2 58.3(2) . . ?
N3 C12 Ca2 178.0(4) . . ?
N6 C13 N4 124.8(5) . . ?
N6 C13 N5 128.3(5) . . ?
N4 C13 N5 106.5(4) . . ?
C15 C14 N5 108.4(5) . . ?
C15 C14 H14 125.8 . . ?
N5 C14 H14 125.8 . . ?
C14 C15 N4 107.6(5) . . ?
C14 C15 H15 126.2 . . ?
N4 C15 H15 126.2 . . ?
N5 C16 C17 112.4(4) . . ?
N5 C16 C19 107.8(4) . . ?
C17 C16 C19 111.3(4) . . ?
N5 C16 C18 108.3(4) . . ?
C17 C16 C18 107.1(4) . . ?
C19 C16 C18 109.8(4) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N4 C20 C23 108.8(5) . . ?
N4 C20 C21 108.4(4) . . ?
C23 C20 C21 109.2(5) . . ?
N4 C20 C22 109.2(4) . . ?
C23 C20 C22 109.0(5) . . ?
C21 C20 C22 112.1(5) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N3 C24 N2 124.3(5) . . ?
N3 C24 N1 129.3(5) . . ?
N2 C24 N1 106.2(4) . . ?
C26 C25 N2 107.9(5) . . ?
C26 C25 H25 126.0 . . ?
N2 C25 H25 126.0 . . ?
C25 C26 N1 108.0(5) . . ?
C25 C26 H26 126.0 . . ?
N1 C26 H26 126.0 . . ?
N2 C27 C29 109.8(4) . . ?
N2 C27 C30 108.7(4) . . ?
C29 C27 C30 111.6(5) . . ?
N2 C27 C28 108.9(4) . . ?
C29 C27 C28 109.0(5) . . ?
C30 C27 C28 108.9(5) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N1 C31 C32 111.9(5) . . ?
N1 C31 C34 108.2(5) . . ?
C32 C31 C34 108.0(5) . . ?
N1 C31 C33 107.4(5) . . ?
C32 C31 C33 110.8(5) . . ?
C34 C31 C33 110.6(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 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 C40 117.6(5) . . ?
C36 C35 N7 120.2(5) . . ?
C40 C35 N7 122.0(5) . . ?
C36 C35 K2 83.5(3) . . ?
C40 C35 K2 76.4(3) . . ?
N7 C35 K2 114.0(3) . . ?
C35 C36 C37 121.6(5) . . ?
C35 C36 K2 71.9(3) . . ?
C37 C36 K2 83.0(3) . . ?
C35 C36 H36 119.2 . . ?
C37 C36 H36 119.2 . . ?
K2 C36 H36 116.3 . . ?
C38 C37 C36 119.5(5) . . ?
C38 C37 K2 76.9(3) . . ?
C36 C37 K2 73.3(3) . . ?
C38 C37 H37 120.3 . . ?
C36 C37 H37 120.3 . . ?
K2 C37 H37 120.6 . . ?
C39 C38 C37 119.7(5) . . ?
C39 C38 K2 72.4(3) . . ?
C37 C38 K2 79.8(3) . . ?
C39 C38 H38 120.2 . . ?
C37 C38 H38 120.2 . . ?
K2 C38 H38 118.6 . . ?
C40 C39 C38 120.7(5) . . ?
C40 C39 K2 73.2(3) . . ?
C38 C39 K2 83.9(4) . . ?
C40 C39 H39 119.7 . . ?
C38 C39 H39 119.7 . . ?
K2 C39 H39 113.6 . . ?
C39 C40 C35 121.0(5) . . ?
C39 C40 K2 82.1(3) . . ?
C35 C40 K2 78.1(3) . . ?
C39 C40 H40 119.5 . . ?
C35 C40 H40 119.5 . . ?
K2 C40 H40 110.5 . . ?
Si3 C41 H41A 109.5 . . ?
Si3 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
Si3 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
Si3 C42 H42A 109.5 . . ?
Si3 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
Si3 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
Si3 C43 H43A 109.5 . . ?
Si3 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
Si3 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
Si5 C44 H44A 109.5 . . ?
Si5 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
Si5 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
Si5 C45 H45A 109.5 . . ?
Si5 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
Si5 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
Si5 C46 H46A 109.5 . . ?
Si5 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
Si5 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
Si4 C47 H47A 109.5 . . ?
Si4 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
Si4 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
Si4 C48 H48A 109.5 . . ?
Si4 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
Si4 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
Si4 C49 H49A 109.5 . . ?
Si4 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
Si4 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
Si6 C50 H50A 109.5 . . ?
Si6 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
Si6 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
Si6 C51 H51A 109.5 . . ?
Si6 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
Si6 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
Si6 C52 H52A 109.5 . . ?
Si6 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
Si6 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C58 C53 C54 119.9(10) . . ?
C58 C53 H53 120.1 . . ?
C54 C53 H53 120.1 . . ?
C53 C54 C55 123.4(11) . . ?
C53 C54 H54 118.3 . . ?
C55 C54 H54 118.3 . . ?
C54 C55 C56 116.2(13) . . ?
C54 C55 H55 121.9 . . ?
C56 C55 H55 121.9 . . ?
C57 C56 C55 119.7(14) . . ?
C57 C56 H56 120.2 . . ?
C55 C56 H56 120.2 . . ?
C58 C57 C56 121.8(11) . . ?
C58 C57 H57 119.1 . . ?
C56 C57 H57 119.1 . . ?
C53 C58 C57 118.9(10) . . ?
C53 C58 C59 120.9(11) . . ?
C57 C58 C59 120.1(10) . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        70.84
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.068
