# Electronic Supplementary Material (ESI) for Chemical Science.
# 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_km47
_database_code_depnum_ccdc_archive 'CCDC 926618'
_audit_update_record             
;
2013-02-26 deposited with the CCDC.
2015-06-18 downloaded from the CCDC.
;
#TrackingRef '18033_web_deposit_cif_file_0_BirgerDittrich_1361906711.km47_.cif'

_audit_creation_method           SHELXL-2012

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H62 N2 Si2'
_chemical_formula_sum            'C40 H62 N2 Si2'
_chemical_formula_weight         627.09

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'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   9.4109(9)
_cell_length_b                   10.1841(10)
_cell_length_c                   11.6538(12)
_cell_angle_alpha                91.036(6)
_cell_angle_beta                 102.694(6)
_cell_angle_gamma                116.006(6)
_cell_volume                     970.92(17)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5183
_cell_measurement_theta_min      3.922
_cell_measurement_theta_max      65.16

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#
_exptl_crystal_description       rectangle
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.019
_exptl_crystal_size_mid          0.014
_exptl_crystal_size_min          0.011
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.0725
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             344.0
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#
_exptl_absorpt_coefficient_mu    1.022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6432
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'SADABS 2012/1 (Sheldrick, 2012)'

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#
_exptl_special_details           
;
Data were collected with a Bruker diffractometer with SMART6000 CCD detector.
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  'INCOATEC multilayer optics'
_diffrn_measurement_device_type  'Bruker SMART 6000'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 5.6020
_diffrn_reflns_number            16983
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.922
_diffrn_reflns_theta_max         66.714
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measured_fraction_theta_full 0.952
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_Laue_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_point_group_measured_fraction_full 0.952
_diffrn_orient_matrix_UB_11      3.3947229e-02
_diffrn_orient_matrix_UB_12      2.6218154e-02
_diffrn_orient_matrix_UB_13      8.8163085e-02
_diffrn_orient_matrix_UB_21      2.4598276e-02
_diffrn_orient_matrix_UB_22      1.0451724e-01
_diffrn_orient_matrix_UB_23      -9.9035846e-03
_diffrn_orient_matrix_UB_31      -1.1480325e-01
_diffrn_orient_matrix_UB_32      -2.3066584e-02
_diffrn_orient_matrix_UB_33      1.8480076e-05


_reflns_number_total             3341
_reflns_number_gt                2685
_reflns_threshold_expression     'I > 2σ(I)'

_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
;

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_data_collection       'Apex2 (Bruker AXS, 2008)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Shelxle (Huebschle et al., 2011)'
_computing_publication_material  'enCIFer 1.3, CCDC, 2008'

_refine_special_details          
;
?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
w=1/[σ²(Fo²)+(0.0578P)²+2.4723P]
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         3341
_refine_ls_number_parameters     276
_refine_ls_number_restraints     130
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0747
_refine_ls_wR_factor_ref         0.2049
_refine_ls_wR_factor_gt          0.1935
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.054
_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
Si1A Si 0.45034(15) 0.87688(12) 0.48103(11) 0.0269(3) Uani 0.75 1 d . U P A 1
Si1B Si 0.4137(5) 0.9696(5) 0.4102(4) 0.0381(9) Uani 0.25 1 d . U P A 2
C1 C 0.4948(4) 0.8502(4) 0.3345(3) 0.0357(8) Uani 1 1 d . U . . .
N2 N 0.3904(3) 0.7374(3) 0.2498(3) 0.0303(7) Uani 1 1 d . U . . .
C3 C 0.4637(4) 0.7021(4) 0.1585(3) 0.0331(8) Uani 1 1 d . U . . .
C4A C 0.6458(9) 0.7975(7) 0.2178(6) 0.0286(13) Uani 0.75 1 d . U P A 1
H41A H 0.7055 0.8427 0.1575 0.034 Uiso 0.75 1 calc R U P A 1
H41B H 0.6936 0.7364 0.2590 0.034 Uiso 0.75 1 calc R U P A 1
C5A C 0.6595(18) 0.9185(15) 0.3078(11) 0.0270(18) Uani 0.75 1 d . U P A 1
C6A C 0.4239(12) 0.5352(9) 0.1460(12) 0.0361(19) Uani 0.75 1 d . U P A 1
H61A H 0.3052 0.4743 0.1203 0.054 Uiso 0.75 1 calc R U P A 1
H61B H 0.4666 0.5109 0.2227 0.054 Uiso 0.75 1 calc R U P A 1
H61C H 0.4748 0.5162 0.0871 0.054 Uiso 0.75 1 calc R U P A 1
C4B C 0.640(4) 0.833(3) 0.188(2) 0.055(5) Uani 0.25 1 d . U P A 2
H42A H 0.7211 0.7950 0.2102 0.066 Uiso 0.25 1 calc R U P A 2
H42B H 0.6580 0.8833 0.1166 0.066 Uiso 0.25 1 calc R U P A 2
C5B C 0.659(6) 0.938(6) 0.286(4) 0.0270(18) Uani 0.25 1 d . U P A 2
C6B C 0.465(4) 0.574(3) 0.165(4) 0.045(6) Uani 0.25 1 d . U P A 2
H62A H 0.5581 0.5773 0.1377 0.068 Uiso 0.25 1 calc R U P A 2
H62B H 0.3634 0.4970 0.1144 0.068 Uiso 0.25 1 calc R U P A 2
H62C H 0.4761 0.5533 0.2472 0.068 Uiso 0.25 1 calc R U P A 2
C7 C 0.3998(5) 0.7338(5) 0.0364(4) 0.0461(10) Uani 1 1 d . U . . .
H7A H 0.4544 0.7137 -0.0193 0.069 Uiso 1 1 calc R U . . .
H7B H 0.4220 0.8374 0.0404 0.069 Uiso 1 1 calc R U . . .
H7C H 0.2817 0.6706 0.0092 0.069 Uiso 1 1 calc R U . . .
C8A C 0.8118(9) 0.9674(7) 0.4111(7) 0.0315(16) Uani 0.75 1 d . U P A 1
H81A H 0.9090 1.0001 0.3800 0.047 Uiso 0.75 1 calc R U P A 1
H81B H 0.8023 0.8845 0.4557 0.047 Uiso 0.75 1 calc R U P A 1
H81C H 0.8217 1.0488 0.4636 0.047 Uiso 0.75 1 calc R U P A 1
C9A C 0.6689(8) 1.0563(7) 0.2459(6) 0.0332(14) Uani 0.75 1 d . U P A 1
H91A H 0.7723 1.1037 0.2229 0.050 Uiso 0.75 1 calc R U P A 1
H91B H 0.6627 1.1263 0.3010 0.050 Uiso 0.75 1 calc R U P A 1
H91C H 0.5775 1.0252 0.1751 0.050 Uiso 0.75 1 calc R U P A 1
C8B C 0.773(4) 0.918(3) 0.390(3) 0.055(6) Uani 0.25 1 d . U P A 2
H82A H 0.7132 0.8243 0.4192 0.082 Uiso 0.25 1 calc R U P A 2
H82B H 0.8133 0.9993 0.4539 0.082 Uiso 0.25 1 calc R U P A 2
H82C H 0.8650 0.9167 0.3651 0.082 Uiso 0.25 1 calc R U P A 2
C9B C 0.718(3) 1.092(3) 0.280(3) 0.054(5) Uani 0.25 1 d . U P A 2
H92A H 0.7945 1.1470 0.3556 0.081 Uiso 0.25 1 calc R U P A 2
H92B H 0.6259 1.1154 0.2637 0.081 Uiso 0.25 1 calc R U P A 2
H92C H 0.7742 1.1184 0.2161 0.081 Uiso 0.25 1 calc R U P A 2
C10 C 0.2185(4) 0.6551(4) 0.2475(3) 0.0300(8) Uani 1 1 d . U . . .
C11 C 0.1069(4) 0.7038(4) 0.1857(3) 0.0346(8) Uani 1 1 d . U . . .
C12 C -0.0580(5) 0.6217(4) 0.1825(4) 0.0392(9) Uani 1 1 d . U . . .
H12 H -0.1352 0.6512 0.1399 0.047 Uiso 1 1 calc R U . . .
C13 C -0.1112(5) 0.4989(4) 0.2399(4) 0.0408(9) Uani 1 1 d . U . . .
H13 H -0.2243 0.4437 0.2357 0.049 Uiso 1 1 calc R U . . .
C14 C -0.0010(5) 0.4561(4) 0.3033(4) 0.0409(9) Uani 1 1 d . U . . .
H14 H -0.0391 0.3723 0.3440 0.049 Uiso 1 1 calc R U . . .
C15 C 0.1656(4) 0.5324(4) 0.3095(3) 0.0351(8) Uani 1 1 d . U . . .
C16 C 0.1599(5) 0.8459(4) 0.1299(4) 0.0459(10) Uani 1 1 d . U . . .
H16 H 0.2785 0.8837 0.1329 0.055 Uiso 1 1 calc R U . B 1
C17 C 0.0676(6) 0.8192(6) 0.0002(5) 0.0617(13) Uani 1 1 d . U . . .
H17A H 0.0726 0.7372 -0.0410 0.092 Uiso 1 1 calc R U . . .
H17B H 0.1175 0.9083 -0.0369 0.092 Uiso 1 1 calc R U . . .
H17C H -0.0468 0.7950 -0.0051 0.092 Uiso 1 1 calc R U . . .
C18A C 0.1432(8) 0.9609(7) 0.2092(6) 0.0408(15) Uani 0.75 1 d . U P C 1
H18A H 0.1844 1.0559 0.1784 0.061 Uiso 0.75 1 calc R U P C 1
H18B H 0.2068 0.9722 0.2907 0.061 Uiso 0.75 1 calc R U P C 1
H18C H 0.0280 0.9266 0.2081 0.061 Uiso 0.75 1 calc R U P C 1
C18B C 0.101(3) 0.961(3) 0.150(2) 0.050(4) Uani 0.25 1 d . U P C 2
H18D H 0.1868 1.0592 0.1482 0.075 Uiso 0.25 1 calc R U P C 2
H18E H 0.0762 0.9558 0.2281 0.075 Uiso 0.25 1 calc R U P C 2
H18F H 0.0023 0.9403 0.0883 0.075 Uiso 0.25 1 calc R U P C 2
C19 C 0.2784(5) 0.4784(5) 0.3857(4) 0.0450(10) Uani 1 1 d . U . . .
H19 H 0.3940 0.5460 0.3858 0.054 Uiso 1 1 calc R U . D 1
C20 C 0.2389(6) 0.3215(5) 0.3395(4) 0.0550(12) Uani 1 1 d . U . . .
H20A H 0.2300 0.3138 0.2541 0.082 Uiso 1 1 calc R U . . .
H20B H 0.1351 0.2518 0.3546 0.082 Uiso 1 1 calc R U . . .
H20C H 0.3262 0.2984 0.3804 0.082 Uiso 1 1 calc R U . . .
C21A C 0.2640(8) 0.4719(6) 0.5137(5) 0.0358(13) Uani 0.75 1 d . U P E 1
H21A H 0.1511 0.4055 0.5145 0.054 Uiso 0.75 1 calc R U P E 1
H21B H 0.2942 0.5708 0.5507 0.054 Uiso 0.75 1 calc R U P E 1
H21C H 0.3374 0.4352 0.5580 0.054 Uiso 0.75 1 calc R U P E 1
C21B C 0.293(3) 0.547(2) 0.5183(18) 0.043(4) Uani 0.25 1 d . U P E 2
H22A H 0.3327 0.6539 0.5217 0.064 Uiso 0.25 1 calc R U P E 2
H22B H 0.3699 0.5263 0.5772 0.064 Uiso 0.25 1 calc R U P E 2
H22C H 0.1855 0.5022 0.5354 0.064 Uiso 0.25 1 calc R U P E 2


_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
Si1A C1 1.887(4) . ?
Si1A Si1A 2.254(2) 2_676 ?
Si1B C1 1.978(6) . ?
Si1B Si1B 2.232(9) 2_676 ?
C1 N2 1.342(5) . ?
C1 C5A 1.502(15) . ?
C1 C5B 1.64(5) . ?
N2 C10 1.453(4) . ?
N2 C3 1.504(4) . ?
C3 C6B 1.31(4) . ?
C3 C7 1.517(6) . ?
C3 C4A 1.534(8) . ?
C3 C4B 1.56(3) . ?
C3 C6A 1.568(10) . ?
C4A C5A 1.546(18) . ?
C5A C8A 1.532(15) . ?
C5A C9A 1.567(12) . ?
C4B C5B 1.48(6) . ?
C5B C9B 1.42(5) . ?
C5B C8B 1.51(5) . ?
C10 C15 1.406(5) . ?
C10 C11 1.416(5) . ?
C11 C12 1.395(5) . ?
C11 C16 1.520(5) . ?
C12 C13 1.375(6) . ?
C13 C14 1.372(6) . ?
C14 C15 1.395(5) . ?
C15 C19 1.527(6) . ?
C16 C17 1.521(7) . ?
C16 C18B 1.53(2) . ?
C16 C18A 1.561(8) . ?
C19 C21A 1.527(7) . ?
C19 C20 1.530(6) . ?
C19 C21B 1.64(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Si1A Si1A 103.67(14) . 2_676 ?
C1 Si1B Si1B 98.9(3) . 2_676 ?
N2 C1 C5A 109.0(7) . . ?
N2 C1 C5B 105.9(19) . . ?
N2 C1 Si1A 122.6(3) . . ?
C5A C1 Si1A 126.3(6) . . ?
N2 C1 Si1B 119.7(3) . . ?
C5B C1 Si1B 118(2) . . ?
C1 N2 C10 121.9(3) . . ?
C1 N2 C3 115.5(3) . . ?
C10 N2 C3 122.6(3) . . ?
C6B C3 N2 112.8(19) . . ?
C6B C3 C7 116.9(18) . . ?
N2 C3 C7 112.2(3) . . ?
N2 C3 C4A 99.8(4) . . ?
C7 C3 C4A 116.5(4) . . ?
C6B C3 C4B 112(2) . . ?
N2 C3 C4B 102.9(12) . . ?
C7 C3 C4B 98.2(11) . . ?
N2 C3 C6A 111.5(6) . . ?
C7 C3 C6A 106.9(5) . . ?
C4A C3 C6A 110.0(5) . . ?
C3 C4A C5A 107.5(7) . . ?
C1 C5A C8A 118.4(8) . . ?
C1 C5A C4A 102.4(9) . . ?
C8A C5A C4A 111.2(10) . . ?
C1 C5A C9A 105.4(9) . . ?
C8A C5A C9A 108.6(10) . . ?
C4A C5A C9A 110.5(7) . . ?
C5B C4B C3 109(3) . . ?
C9B C5B C4B 123(3) . . ?
C9B C5B C8B 108(4) . . ?
C4B C5B C8B 104(4) . . ?
C9B C5B C1 119(4) . . ?
C4B C5B C1 104(3) . . ?
C8B C5B C1 95(2) . . ?
C15 C10 C11 120.8(3) . . ?
C15 C10 N2 120.3(3) . . ?
C11 C10 N2 118.9(3) . . ?
C12 C11 C10 118.1(3) . . ?
C12 C11 C16 118.7(4) . . ?
C10 C11 C16 123.1(3) . . ?
C13 C12 C11 121.3(4) . . ?
C14 C13 C12 120.0(4) . . ?
C13 C14 C15 121.7(4) . . ?
C14 C15 C10 118.0(4) . . ?
C14 C15 C19 117.5(3) . . ?
C10 C15 C19 124.5(3) . . ?
C11 C16 C17 111.5(4) . . ?
C11 C16 C18B 122.7(9) . . ?
C17 C16 C18B 88.1(9) . . ?
C11 C16 C18A 107.8(4) . . ?
C17 C16 C18A 114.6(4) . . ?
C15 C19 C21A 113.0(4) . . ?
C15 C19 C20 112.1(3) . . ?
C21A C19 C20 105.0(4) . . ?
C15 C19 C21B 100.6(8) . . ?
C20 C19 C21B 129.6(8) . . ?

_refine_diff_density_max         0.452
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.067


####################################################################### 
# 
# 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_km130
_database_code_depnum_ccdc_archive 'CCDC 927696'
_audit_update_record             
;
2013-03-05 deposited with the CCDC.
2015-06-18 downloaded from the CCDC.
;

_audit_creation_date             '11-Jan-01 T18:16:04-00:00'
_audit_creation_method           'XD routine XDCIF'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H31 N O'
_chemical_formula_sum            'C20 H31 N O'
_chemical_formula_weight         301.46

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 'Invariom modelling (Acta Cryst. A61, 314--320)'
H H 0.0000 0.0000 'Invariom modelling (Acta Cryst. A61, 314--320)'
N N 0.0311 0.0180 'Invariom modelling (Acta Cryst. A61, 314--320)'
O O 0.0492 0.0322 'Invariom modelling (Acta Cryst. A61, 314--320)'

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'


_cell_length_a                   9.269(7)
_cell_length_b                   17.342(10)
_cell_length_c                   11.775(11)
_cell_angle_alpha                90
_cell_angle_beta                 96.71(4)
_cell_angle_gamma                90
_cell_volume                     1880(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8877
_cell_measurement_theta_max      69.50
_cell_measurement_theta_min      4.611

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

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_crystal_description       rectangle
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_F_000             664.0

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#
_exptl_absorpt_coefficient_mu    0.488
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7040
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_process_details   
;
SADABS version 2012/1, multi-scan. (G. M. Sheldrick, 2012)
;

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_measurement_method       'ω and φ scans'
_diffrn_measurement_device_type  'Bruker SMART 6000 Diffractometer'
_diffrn_radiation_wavelength     1.54188
_diffrn_ambient_temperature      100
_diffrn_reflns_number            30611
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.560
_diffrn_reflns_theta_max         68.570
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_orient_matrix_UB_11      9.4941735e-02
_diffrn_orient_matrix_UB_12      -2.6820695e-02
_diffrn_orient_matrix_UB_13      2.6022954e-02
_diffrn_orient_matrix_UB_21      -4.7322001e-02
_diffrn_orient_matrix_UB_22      -5.1585585e-02
_diffrn_orient_matrix_UB_23      -1.9290712e-02
_diffrn_orient_matrix_UB_31      2.8404878e-02
_diffrn_orient_matrix_UB_32      3.7060606e-03
_diffrn_orient_matrix_UB_33      -8.0184594e-02


#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#
_computing_structure_refinement  'XDLSM, Volkov et al, (2006)'
_computing_publication_material  'enCIFer 1.4, CCDC, 2011'
_computing_data_collection       'APEX2 v2009.11-0'
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS, 2012)'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#
_reflns_threshold_expression     F>3(σ)F
_reflns_number_total             3254
_reflns_number_gt                2984
_refine_ls_hydrogen_treatment    refU
_refine_special_details          
;
An invariom refinement was carried out.
Hydrogen atom positions were calculated with shelxl and
their bond distances elongated to idealized values from
geometry optimizations of suitable model compound from
the invariom database.
;
_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
calc w1 = 1/[s²(Fo)]
;
_refine_ls_extinction_method     none
_refine_ls_number_reflns         2984
_refine_ls_number_parameters     230
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.027
_refine_ls_R_factor_gt           0.024
_refine_ls_wR_factor_ref         0.021
_refine_ls_goodness_of_fit_ref   2.192
_refine_ls_shift/su_max          0
_refine_diff_density_max         0.198
_refine_diff_density_min         -0.127
_refine_diff_density_rms         0.024

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#


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
O(1) O 0.36431(7) 0.78414(3) 0.28542(5) 0.027 Uani 1 4
N(2) N 0.45241(7) 0.68121(4) 0.39929(5) 0.015 Uani 1 4
C(1) C 0.44617(9) 0.75726(5) 0.36647(7) 0.018 Uani 1 4
C(3) C 0.55338(9) 0.66521(5) 0.50684(6) 0.016 Uani 1 4
C(4) C 0.64253(9) 0.74155(5) 0.51963(7) 0.019 Uani 1 4
C(5) C 0.55066(9) 0.80474(5) 0.45152(7) 0.017 Uani 1 4
C(6) C 0.64403(10) 0.85881(5) 0.38594(8) 0.028 Uani 1 4
C(7) C 0.45979(10) 0.85309(5) 0.52874(7) 0.025 Uani 1 4
C(8) C 0.46769(9) 0.64905(5) 0.61018(7) 0.02 Uani 1 4
C(9) C 0.65355(9) 0.59555(5) 0.49376(7) 0.023 Uani 1 4
C(10) C 0.36644(9) 0.62165(4) 0.33740(6) 0.014 Uani 1 4
C(11) C 0.42777(9) 0.57936(5) 0.25055(6) 0.016 Uani 1 4
C(12) C 0.34851(10) 0.51656(5) 0.19864(7) 0.021 Uani 1 4
C(13) C 0.21120(10) 0.49688(5) 0.22951(7) 0.022 Uani 1 4
C(14) C 0.14782(9) 0.54273(5) 0.30877(7) 0.019 Uani 1 4
C(15) C 0.22265(9) 0.60603(5) 0.36319(6) 0.015 Uani 1 4
C(16) C 0.57000(9) 0.60374(5) 0.20560(7) 0.019 Uani 1 4
C(17) C 0.67481(10) 0.53559(5) 0.19298(8) 0.028 Uani 1 4
C(18) C 0.53421(10) 0.64622(6) 0.08972(7) 0.028 Uani 1 4
C(19) C 0.14192(9) 0.65882(5) 0.43945(7) 0.017 Uani 1 4
C(20) C 0.02503(9) 0.70483(5) 0.36205(7) 0.023 Uani 1 4
C(21) C 0.07269(10) 0.61488(5) 0.53426(7) 0.025 Uani 1 4
H(4A) H 0.66414 0.75782 0.60975 0.038(3) Uiso 1 4
H(4B) H 0.74644 0.73420 0.48547 0.038(3) Uiso 1 4
H(6A) H 0.70688 0.82460 0.33141 0.053(3) Uiso 1 4
H(6B) H 0.71782 0.89167 0.44677 0.058(4) Uiso 1 4
H(6C) H 0.57337 0.89841 0.33319 0.049(3) Uiso 1 4
H(7A) H 0.38793 0.89186 0.47550 0.045(3) Uiso 1 4
H(7B) H 0.53266 0.88683 0.58907 0.058(4) Uiso 1 4
H(7C) H 0.39499 0.81458 0.57575 0.054(3) Uiso 1 4
H(8A) H 0.39882 0.69848 0.62361 0.039(3) Uiso 1 4
H(8B) H 0.54368 0.63932 0.68686 0.044(3) Uiso 1 4
H(8C) H 0.40011 0.59794 0.59243 0.040(3) Uiso 1 4
H(9A) H 0.58760 0.54382 0.47637 0.051(3) Uiso 1 4
H(9B) H 0.72673 0.58752 0.57246 0.040(3) Uiso 1 4
H(9C) H 0.71706 0.60600 0.42287 0.044(3) Uiso 1 4
H(12) H 0.39408 0.48301 0.13401 0.037(3) Uiso 1 4
H(13) H 0.15456 0.44665 0.19243 0.043(3) Uiso 1 4
H(14) H 0.03942 0.52921 0.32829 0.036(3) Uiso 1 4
H(16) H 0.62526 0.64463 0.26672 0.032(3) Uiso 1 4
H(17A) H 0.62610 0.49626 0.12697 0.054(3) Uiso 1 4
H(17B) H 0.69495 0.50490 0.27420 0.055(3) Uiso 1 4
H(17C) H 0.77729 0.55758 0.16887 0.049(3) Uiso 1 4
H(18A) H 0.63452 0.66747 0.06069 0.053(3) Uiso 1 4
H(18B) H 0.46194 0.69469 0.10049 0.049(3) Uiso 1 4
H(18C) H 0.48105 0.60633 0.02642 0.050(3) Uiso 1 4
H(19) H 0.22032 0.70010 0.48100 0.030(3) Uiso 1 4
H(20A) H 0.07685 0.73665 0.29788 0.048(3) Uiso 1 4
H(20B) H -0.02899 0.74522 0.41425 0.044(3) Uiso 1 4
H(20C) H -0.05491 0.66494 0.31956 0.042(3) Uiso 1 4
H(21A) H -0.00954 0.57497 0.49503 0.047(3) Uiso 1 4
H(21B) H 0.02224 0.65605 0.58756 0.049(3) Uiso 1 4
H(21C) H 0.15680 0.58269 0.58694 0.050(3) Uiso 1 4



#----------------------------------------------------------------------------#
# MULTIPOLE PARAMETERS #
#----------------------------------------------------------------------------#

loop_
_atom_local_axes_atom0
_atom_local_axes_ax1
_atom_local_axes_atom1
_atom_local_axes_atom2
_atom_local_axes_ax2
C(1) Z O(1) N(2) X
C(1) X N(2) C(10) Y
O(1) X C(1) C(5) Y
N(2) Z C(3) C(9) X
DUM1 Z C(4) C(5) Y
C(6) Z C(5) C(1) X
C(5) Z C(6) H(6A) X
C(5) Z C(7) H(7C) X
C(3) Z C(8) H(8C) X
C(3) Z C(9) H(9A) X
N(2) Z C(10) C(15) X
C(12) X C(11) C(10) Y
C(13) X C(12) C(11) Y
DUM2 Z C(13) C(14) X
C(13) X C(14) C(15) Y
C(14) X C(15) C(10) Y
C(11) X C(16) H(16) Y
C(16) Z C(17) H(17B) X
C(16) Z C(18) H(18A) X
C(15) X C(19) H(19) Y
C(19) Z C(20) H(20C) X
C(19) Z C(21) H(21B) X
C(4) Z H(4A) C(5) Y
C(4) Z H(4B) C(5) Y
C(6) Z H(6A) C(5) Y
C(6) Z H(6B) C(5) Y
C(6) Z H(6C) C(5) Y
C(7) Z H(7A) C(5) Y
C(7) Z H(7B) C(5) Y
C(7) Z H(7C) C(5) Y
C(8) Z H(8A) C(3) Y
C(8) Z H(8B) C(3) Y
C(8) Z H(8C) C(3) Y
C(9) Z H(9A) C(3) Y
C(9) Z H(9B) C(3) Y
C(9) Z H(9C) C(3) Y
C(12) Z H(12) C(13) Y
C(13) Z H(13) C(14) Y
C(14) Z H(14) C(13) Y
C(16) Z H(16) C(11) Y
C(17) Z H(17A) C(16) Y
C(17) Z H(17B) C(16) Y
C(17) Z H(17C) C(16) Y
C(18) Z H(18A) C(16) Y
C(18) Z H(18B) C(16) Y
C(18) Z H(18C) C(16) Y
C(19) Z H(19) C(15) Y
C(20) Z H(20A) C(19) Y
C(20) Z H(20B) C(19) Y
C(20) Z H(20C) C(19) Y
C(21) Z H(21A) C(19) Y
C(21) Z H(21B) C(19) Y
C(21) Z H(21C) C(19) Y


#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O(1) C(1) 1.2386(10) 1_555 1_555 yes
N(2) C(1) 1.3736(10) 1_555 1_555 yes
N(2) C(10) 1.4482(10) 1_555 1_555 yes
C(4) H(4A) 1.0937 1_555 1_555 yes
C(4) H(4B) 1.0937 1_555 1_555 yes
C(6) H(6A) 1.0914 1_555 1_555 yes
C(6) H(6B) 1.0914 1_555 1_555 yes
C(6) H(6C) 1.0914 1_555 1_555 yes
C(7) H(7A) 1.0914 1_555 1_555 yes
C(7) H(7B) 1.0914 1_555 1_555 yes
C(7) H(7C) 1.0914 1_555 1_555 yes
C(8) H(8A) 1.0914 1_555 1_555 yes
C(8) H(8B) 1.0914 1_555 1_555 yes
C(8) H(8C) 1.0914 1_555 1_555 yes
C(9) H(9A) 1.0914 1_555 1_555 yes
C(9) H(9B) 1.0914 1_555 1_555 yes
C(9) H(9C) 1.0914 1_555 1_555 yes
C(10) C(11) 1.4292(11) 1_555 1_555 yes
C(10) C(15) 1.4270(11) 1_555 1_555 yes
C(11) C(12) 1.4123(11) 1_555 1_555 yes
C(11) C(16) 1.5363(12) 1_555 1_555 yes
C(12) C(13) 1.4059(12) 1_555 1_555 yes
C(12) H(12) 1.0823 1_555 1_555 yes
C(13) C(14) 1.4058(12) 1_555 1_555 yes
C(13) H(13) 1.0822 1_555 1_555 yes
C(14) C(15) 1.4118(11) 1_555 1_555 yes
C(14) H(14) 1.0822 1_555 1_555 yes
C(15) C(19) 1.5367(11) 1_555 1_555 yes
C(16) H(16) 1.0939 1_555 1_555 yes
C(17) H(17A) 1.0914 1_555 1_555 yes
C(17) H(17B) 1.0914 1_555 1_555 yes
C(17) H(17C) 1.0914 1_555 1_555 yes
C(18) H(18A) 1.0914 1_555 1_555 yes
C(18) H(18B) 1.0914 1_555 1_555 yes
C(18) H(18C) 1.0914 1_555 1_555 yes
C(19) H(19) 1.0939 1_555 1_555 yes
C(20) H(20A) 1.0914 1_555 1_555 yes
C(20) H(20B) 1.0914 1_555 1_555 yes
C(20) H(20C) 1.0914 1_555 1_555 yes
C(21) H(21A) 1.0914 1_555 1_555 yes
C(21) H(21B) 1.0914 1_555 1_555 yes
C(21) H(21C) 1.0914 1_555 1_555 yes

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C(1) N(2) C(10) 122.73(6) 1_555 1_555 1_555 yes
O(1) C(1) N(2) 125.44(7) 1_555 1_555 1_555 yes
N(2) C(10) C(11) 118.98(7) 1_555 1_555 1_555 yes
N(2) C(10) C(15) 120.07(7) 1_555 1_555 1_555 yes
C(11) C(10) C(15) 120.95(7) 1_555 1_555 1_555 yes
C(10) C(11) C(12) 118.37(8) 1_555 1_555 1_555 yes
C(10) C(11) C(16) 122.30(7) 1_555 1_555 1_555 yes
C(12) C(11) C(16) 119.15(7) 1_555 1_555 1_555 yes
C(11) C(12) C(13) 121.08(8) 1_555 1_555 1_555 yes
C(12) C(13) C(14) 119.70(8) 1_555 1_555 1_555 yes
C(13) C(14) C(15) 121.33(8) 1_555 1_555 1_555 yes
C(10) C(15) C(14) 118.20(7) 1_555 1_555 1_555 yes
C(10) C(15) C(19) 122.81(7) 1_555 1_555 1_555 yes
C(14) C(15) C(19) 118.79(7) 1_555 1_555 1_555 yes


####################################################################### 
# 
# 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_km102
_database_code_depnum_ccdc_archive 'CCDC 948799'
_audit_update_record             
;
2013-07-04 deposited with the CCDC.
2015-06-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2012

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C92 H140 N4 Si4'
_chemical_formula_weight         1414.43

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0024 0.0013 '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 0.0049 0.0027 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0686 0.0572 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
_cell_length_a                   12.80(3)
_cell_length_b                   13.86(4)
_cell_length_c                   14.36(2)
_cell_angle_alpha                66.45(7)
_cell_angle_beta                 79.90(4)
_cell_angle_gamma                67.84(9)
_cell_volume                     2162(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3093
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      22.6

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#
_computing_data_collection       'XDS (Kabsch, 2010)'
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_publication_material  'enCIFer 1.4, CCDC, 2011'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_molecular_graphics    ?

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_F_000             776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.039
_exptl_crystal_size_mid          0.014
_exptl_crystal_size_min          0.012

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.2980
_exptl_absorpt_correction_T_max  0.4268
_exptl_absorpt_process_details   
;
SADABS version 2012/1, multi-scan. (G. M. Sheldrick, 2008)
;


_exptl_special_details           
;
Synchrotron radiation was used. Phi-scans only.
19.5 keV, SLS-beamline X10SA. Nitrogen-gas stream 
cooling.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.6358
_diffrn_radiation_type           'monochromated X-rays beamline X10SA@SLS'
_diffrn_source                   synchrotron
_diffrn_measurement_method       'φ scans'
_diffrn_measurement_device_type  'Microdiffractometer at the SLS'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24747
_diffrn_reflns_av_unetI/netI     0.0730
_diffrn_reflns_av_R_equivalents  0.0802
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.384
_diffrn_reflns_theta_max         22.720
_diffrn_reflns_theta_full        22.425
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measured_fraction_theta_full 0.917
_diffrn_reflns_Laue_measured_fraction_max 0.897
_diffrn_reflns_Laue_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_point_group_measured_fraction_full 0.917
_reflns_number_total             7289
_reflns_number_gt                5848
_reflns_threshold_expression     'I > 2σ(I)'

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;

_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)+(0.0773P)²+1.6102P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7289
_refine_ls_number_parameters     635
_refine_ls_number_restraints     238
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0692
_refine_ls_wR_factor_ref         0.1930
_refine_ls_wR_factor_gt          0.1814
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.023
_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
Si1A Si 0.21533(7) 0.29355(8) 0.32302(7) 0.0389(3) Uani 0.806(2) 1 d . . P A 1
Si2A Si 0.21362(7) 0.26295(8) 0.18053(7) 0.0383(3) Uani 0.806(2) 1 d . . P A 1
Si1C Si 0.2093(4) 0.3741(4) 0.2171(4) 0.0583(14) Uiso 0.194(2) 1 d . . P A 2
Si2C Si 0.2259(4) 0.1941(4) 0.2710(4) 0.0544(13) Uiso 0.194(2) 1 d . . P A 2
C1A C 0.3412(3) 0.3398(3) 0.2981(3) 0.0344(8) Uani 0.806(2) 1 d . U P A 1
N2A N 0.3441(3) 0.4089(3) 0.3414(2) 0.0351(7) Uani 0.806(2) 1 d . U P A 1
C3A C 0.4544(5) 0.4300(4) 0.3282(3) 0.0404(9) Uani 0.806(2) 1 d D U P A 1
C4A C 0.5317(3) 0.3395(3) 0.2871(3) 0.0382(8) Uani 0.806(2) 1 d . . P A 1
H41A H 0.5824 0.3698 0.2322 0.046 Uiso 0.806(2) 1 calc R U P A 1
H41B H 0.5786 0.2749 0.3420 0.046 Uiso 0.806(2) 1 calc R U P A 1
C5A C 0.4564(4) 0.3027(4) 0.2460(3) 0.0340(9) Uani 0.806(2) 1 d D U P A 1
C6A C 0.4438(4) 0.5483(4) 0.2513(4) 0.0502(11) Uani 0.806(2) 1 d D U P A 1
H61A H 0.4213 0.5570 0.1857 0.075 Uiso 0.806(2) 1 calc R U P A 1
H61B H 0.5166 0.5593 0.2428 0.075 Uiso 0.806(2) 1 calc R U P A 1
H61C H 0.3866 0.6038 0.2762 0.075 Uiso 0.806(2) 1 calc R U P A 1
C7A C 0.4948(6) 0.4153(6) 0.4284(4) 0.0493(12) Uani 0.806(2) 1 d D U P A 1
H71A H 0.4383 0.4685 0.4563 0.074 Uiso 0.806(2) 1 calc R U P A 1
H71B H 0.5665 0.4291 0.4165 0.074 Uiso 0.806(2) 1 calc R U P A 1
H71C H 0.5055 0.3387 0.4766 0.074 Uiso 0.806(2) 1 calc R U P A 1
C8A C 0.4432(5) 0.3636(7) 0.1296(6) 0.0409(17) Uani 0.806(2) 1 d D . P A 1
H81A H 0.3836 0.3478 0.1086 0.049 Uiso 0.806(2) 1 calc R U P A 1
H81B H 0.4181 0.4454 0.1131 0.049 Uiso 0.806(2) 1 calc R U P A 1
C9A C 0.5527(5) 0.3286(6) 0.0684(5) 0.0457(14) Uani 0.806(2) 1 d D . P A 1
H91A H 0.5372 0.3649 -0.0051 0.055 Uiso 0.806(2) 1 calc R U P A 1
H91B H 0.6091 0.3545 0.0812 0.055 Uiso 0.806(2) 1 calc R U P A 1
C10A C 0.6006(5) 0.2023(5) 0.0973(4) 0.0528(14) Uani 0.806(2) 1 d D . P A 1
H10A H 0.6743 0.1820 0.0614 0.063 Uiso 0.806(2) 1 calc R U P A 1
H10B H 0.5490 0.1779 0.0753 0.063 Uiso 0.806(2) 1 calc R U P A 1
C11A C 0.6164(4) 0.1412(5) 0.2123(5) 0.0502(14) Uani 0.806(2) 1 d D . P A 1
H11A H 0.6732 0.1600 0.2339 0.060 Uiso 0.806(2) 1 calc R U P A 1
H11B H 0.6440 0.0592 0.2291 0.060 Uiso 0.806(2) 1 calc R U P A 1
C12A C 0.5036(4) 0.1760(4) 0.2691(4) 0.0407(10) Uani 0.806(2) 1 d D . P A 1
H12A H 0.5144 0.1356 0.3432 0.049 Uiso 0.806(2) 1 calc R U P A 1
H12B H 0.4481 0.1540 0.2494 0.049 Uiso 0.806(2) 1 calc R U P A 1
C1B C 0.3360(15) 0.3737(15) 0.2606(13) 0.0352(17) Uani 0.194(2) 1 d . U P A 2
N2B N 0.3404(17) 0.4359(16) 0.3090(12) 0.0366(17) Uani 0.194(2) 1 d . U P A 2
C3B C 0.450(2) 0.4545(16) 0.3033(17) 0.0382(19) Uani 0.194(2) 1 d D U P A 2
C4B C 0.5146(14) 0.4052(18) 0.2278(18) 0.058(5) Uani 0.194(2) 1 d . . P A 2
H42A H 0.5921 0.3579 0.2515 0.069 Uiso 0.194(2) 1 calc R U P A 2
H42B H 0.5199 0.4657 0.1624 0.069 Uiso 0.194(2) 1 calc R U P A 2
C5B C 0.4543(18) 0.3310(16) 0.2113(16) 0.034(2) Uani 0.194(2) 1 d D U P A 2
C6B C 0.4271(19) 0.5786(16) 0.2732(18) 0.048(3) Uani 0.194(2) 1 d D U P A 2
H62A H 0.3734 0.6059 0.3223 0.073 Uiso 0.194(2) 1 calc R U P A 2
H62B H 0.3953 0.6192 0.2054 0.073 Uiso 0.194(2) 1 calc R U P A 2
H62C H 0.4978 0.5908 0.2725 0.073 Uiso 0.194(2) 1 calc R U P A 2
C7B C 0.500(3) 0.397(2) 0.4085(18) 0.049(4) Uani 0.194(2) 1 d D U P A 2
H72A H 0.5707 0.4106 0.4054 0.073 Uiso 0.194(2) 1 calc R U P A 2
H72B H 0.5158 0.3161 0.4314 0.073 Uiso 0.194(2) 1 calc R U P A 2
H72C H 0.4467 0.4266 0.4563 0.073 Uiso 0.194(2) 1 calc R U P A 2
C8B C 0.464(3) 0.345(3) 0.106(3) 0.053(9) Uani 0.194(2) 1 d D . P A 2
H82A H 0.4407 0.4259 0.0637 0.064 Uiso 0.194(2) 1 calc R U P A 2
H82B H 0.4120 0.3143 0.0927 0.064 Uiso 0.194(2) 1 calc R U P A 2
C9B C 0.585(3) 0.286(2) 0.074(3) 0.066(9) Uani 0.194(2) 1 d D . P A 2
H92A H 0.5859 0.2905 0.0035 0.079 Uiso 0.194(2) 1 calc R U P A 2
H92B H 0.6348 0.3252 0.0761 0.079 Uiso 0.194(2) 1 calc R U P A 2
C10B C 0.630(2) 0.163(2) 0.145(2) 0.070(9) Uani 0.194(2) 1 d D . P A 2
H10C H 0.7083 0.1287 0.1226 0.084 Uiso 0.194(2) 1 calc R U P A 2
H10D H 0.5836 0.1231 0.1382 0.084 Uiso 0.194(2) 1 calc R U P A 2
C11B C 0.629(2) 0.149(3) 0.256(2) 0.086(9) Uani 0.194(2) 1 d D . P A 2
H11C H 0.6826 0.1804 0.2653 0.103 Uiso 0.194(2) 1 calc R U P A 2
H11D H 0.6523 0.0684 0.2998 0.103 Uiso 0.194(2) 1 calc R U P A 2
C12B C 0.5083(16) 0.2107(18) 0.2868(16) 0.069(8) Uani 0.194(2) 1 d D . P A 2
H12C H 0.5099 0.2136 0.3543 0.083 Uiso 0.194(2) 1 calc R U P A 2
H12D H 0.4599 0.1668 0.2936 0.083 Uiso 0.194(2) 1 calc R U P A 2
C13A C 0.2474(2) 0.4680(3) 0.3897(2) 0.0450(7) Uani 1 1 d . . . . .
C14A C 0.2336(2) 0.4174(3) 0.4952(2) 0.0477(7) Uani 1 1 d D U . . .
C15A C 0.1456(2) 0.4787(3) 0.5441(2) 0.0555(8) Uani 1 1 d . . . . .
H15A H 0.1347 0.4468 0.6156 0.067 Uiso 1 1 calc R U . . .
C16A C 0.0749(2) 0.5838(3) 0.4911(3) 0.0564(8) Uani 1 1 d . . . . .
H16A H 0.0177 0.6247 0.5264 0.068 Uiso 1 1 calc R U . . .
C17A C 0.0861(2) 0.6302(3) 0.3873(3) 0.0513(7) Uani 1 1 d . . . . .
H17A H 0.0356 0.7026 0.3517 0.062 Uiso 1 1 calc R U . . .
C18A C 0.1704(2) 0.5730(3) 0.3331(2) 0.0457(7) Uani 1 1 d . . . . .
C19A C 0.1686(2) 0.6219(3) 0.2179(2) 0.0548(8) Uani 1 1 d . . . . .
H19A H 0.2372 0.5738 0.1916 0.066 Uiso 1 1 calc R U . . .
C20A C 0.1700(3) 0.7410(3) 0.1715(3) 0.0715(10) Uani 1 1 d . . . . .
H20A H 0.1778 0.7639 0.0974 0.107 Uiso 1 1 calc R U . . .
H20B H 0.2337 0.7447 0.1975 0.107 Uiso 1 1 calc R U . . .
H20C H 0.0993 0.7913 0.1897 0.107 Uiso 1 1 calc R U . . .
C21A C 0.0638(3) 0.6169(3) 0.1832(3) 0.0655(9) Uani 1 1 d . . . . .
H21A H 0.0668 0.6403 0.1090 0.098 Uiso 1 1 calc R U . . .
H21B H -0.0046 0.6671 0.2043 0.098 Uiso 1 1 calc R U . . .
H21C H 0.0628 0.5401 0.2142 0.098 Uiso 1 1 calc R U . . .
C22A C 0.3038(3) 0.3006(3) 0.5611(3) 0.0489(9) Uani 0.806(2) 1 d D U P A 1
H22A H 0.3661 0.2688 0.5176 0.059 Uiso 0.806(2) 1 calc R U P A 1
C23A C 0.3569(3) 0.2981(4) 0.6507(3) 0.0579(11) Uani 0.806(2) 1 d D U P A 1
H23A H 0.4011 0.3483 0.6250 0.087 Uiso 0.806(2) 1 calc R U P A 1
H23B H 0.4062 0.2217 0.6867 0.087 Uiso 0.806(2) 1 calc R U P A 1
H23C H 0.2970 0.3228 0.6975 0.087 Uiso 0.806(2) 1 calc R U P A 1
C24A C 0.2318(3) 0.2245(4) 0.6041(3) 0.0548(9) Uani 0.806(2) 1 d D U P A 1
H24A H 0.1722 0.2523 0.6495 0.082 Uiso 0.806(2) 1 calc R U P A 1
H24B H 0.2796 0.1481 0.6421 0.082 Uiso 0.806(2) 1 calc R U P A 1
H24C H 0.1976 0.2245 0.5481 0.082 Uiso 0.806(2) 1 calc R U P A 1
C22B C 0.3024(17) 0.2912(9) 0.5308(18) 0.075(8) Uiso 0.194(2) 1 d D . P A 2
H22B H 0.3628 0.2786 0.4780 0.090 Uiso 0.194(2) 1 calc R U P A 2
C23B C 0.360(2) 0.258(2) 0.6300(17) 0.078(7) Uiso 0.194(2) 1 d D . P A 2
H23D H 0.3027 0.2646 0.6843 0.117 Uiso 0.194(2) 1 calc R U P A 2
H23E H 0.4022 0.3079 0.6197 0.117 Uiso 0.194(2) 1 calc R U P A 2
H23F H 0.4122 0.1806 0.6492 0.117 Uiso 0.194(2) 1 calc R U P A 2
C24B C 0.2311(19) 0.2171(19) 0.5456(19) 0.082(6) Uiso 0.194(2) 1 d D . P A 2
H24D H 0.2810 0.1393 0.5601 0.124 Uiso 0.194(2) 1 calc R U P A 2
H24E H 0.1902 0.2437 0.4835 0.124 Uiso 0.194(2) 1 calc R U P A 2
H24F H 0.1771 0.2213 0.6026 0.124 Uiso 0.194(2) 1 calc R U P A 2
C1C C 0.0915(2) 0.2141(3) 0.2012(2) 0.0467(7) Uani 1 1 d . . . . .
N2C N 0.09789(17) 0.1169(2) 0.19624(18) 0.0444(6) Uani 1 1 d . . . . .
C3C C -0.0132(2) 0.1051(3) 0.1922(3) 0.0504(7) Uani 1 1 d . . . . .
C4C C -0.0943(7) 0.2294(7) 0.1669(10) 0.047(2) Uani 0.571(18) 1 d . U P B 1
H43A H -0.1104 0.2659 0.0935 0.057 Uiso 0.571(18) 1 calc R U P B 1
H43B H -0.1665 0.2322 0.2060 0.057 Uiso 0.571(18) 1 calc R U P B 1
C4D C -0.0966(10) 0.2015(11) 0.2207(12) 0.048(2) Uani 0.429(18) 1 d . U P B 2
H43A H -0.1191 0.1748 0.2936 0.058 Uiso 0.429(18) 1 calc R U P B 2
H43B H -0.1652 0.2369 0.1798 0.058 Uiso 0.429(18) 1 calc R U P B 2
C5C C -0.0321(2) 0.2889(3) 0.1970(2) 0.0460(7) Uani 1 1 d . . . . .
C6C C -0.0192(3) 0.0831(4) 0.0986(3) 0.0730(11) Uani 1 1 d . . . . .
H63A H -0.0140 0.1471 0.0377 0.109 Uiso 1 1 calc R U . . .
H63B H -0.0909 0.0725 0.0998 0.109 Uiso 1 1 calc R U . . .
H63C H 0.0435 0.0156 0.0975 0.109 Uiso 1 1 calc R U . . .
C7C C -0.0321(3) 0.0112(4) 0.2847(3) 0.0859(13) Uani 1 1 d . . . . .
H73A H -0.1045 0.0047 0.2803 0.129 Uiso 1 1 calc R U . . .
H73B H -0.0329 0.0267 0.3458 0.129 Uiso 1 1 calc R U . . .
H73C H 0.0289 -0.0591 0.2885 0.129 Uiso 1 1 calc R U . . .
C8C C -0.0513(3) 0.3980(3) 0.1055(3) 0.0684(10) Uani 1 1 d . . . . .
H83A H -0.0329 0.3815 0.0424 0.082 Uiso 1 1 calc R U . . .
H83B H -0.0002 0.4356 0.1081 0.082 Uiso 1 1 calc R U . . .
C9C C -0.1751(3) 0.4775(4) 0.1033(3) 0.0822(13) Uani 1 1 d . . . . .
H93A H -0.1836 0.5492 0.0454 0.099 Uiso 1 1 calc R U . . .
H93B H -0.2255 0.4435 0.0928 0.099 Uiso 1 1 calc R U . . .
C10C C -0.2094(3) 0.4996(3) 0.1987(4) 0.0743(11) Uani 1 1 d . . . . .
H10E H -0.2904 0.5458 0.1964 0.089 Uiso 1 1 calc R U . . .
H10F H -0.1660 0.5429 0.2043 0.089 Uiso 1 1 calc R U . . .
C11C C -0.1904(2) 0.3943(3) 0.2902(3) 0.0611(9) Uani 1 1 d . . . . .
H11E H -0.2413 0.3558 0.2893 0.073 Uiso 1 1 calc R U . . .
H11F H -0.2087 0.4128 0.3522 0.073 Uiso 1 1 calc R U . . .
C12C C -0.0684(2) 0.3161(3) 0.2930(2) 0.0545(8) Uani 1 1 d . . . . .
H12E H -0.0183 0.3515 0.3014 0.065 Uiso 1 1 calc R U . . .
H12F H -0.0597 0.2457 0.3525 0.065 Uiso 1 1 calc R U . . .
C13C C 0.2044(2) 0.0302(2) 0.1934(2) 0.0433(7) Uani 1 1 d . . . . .
C14C C 0.2585(2) 0.0322(2) 0.0983(2) 0.0434(6) Uani 1 1 d . . . . .
C15C C 0.3572(2) -0.0581(3) 0.0971(2) 0.0499(7) Uani 1 1 d . . . . .
H15C H 0.3943 -0.0590 0.0339 0.060 Uiso 1 1 calc R U . . .
C16C C 0.4010(2) -0.1445(3) 0.1848(3) 0.0543(8) Uani 1 1 d . . . . .
H16C H 0.4661 -0.2061 0.1820 0.065 Uiso 1 1 calc R U . . .
C17C C 0.3506(2) -0.1421(3) 0.2771(3) 0.0579(8) Uani 1 1 d . . . . .
H17C H 0.3825 -0.2018 0.3376 0.070 Uiso 1 1 calc R U . . .
C18C C 0.2531(2) -0.0534(3) 0.2839(2) 0.0514(7) Uani 1 1 d D U . . .
C19C C 0.2101(6) -0.0458(5) 0.3878(3) 0.0557(13) Uani 0.806(2) 1 d D U P A 1
H19C H 0.1398 0.0209 0.3793 0.067 Uiso 0.806(2) 1 calc R U P A 1
C20C C 0.1849(5) -0.1513(5) 0.4600(4) 0.0688(13) Uani 0.806(2) 1 d . U P A 1
H20D H 0.1317 -0.1641 0.4286 0.103 Uiso 0.806(2) 1 calc R U P A 1
H20E H 0.1518 -0.1416 0.5239 0.103 Uiso 0.806(2) 1 calc R U P A 1
H20F H 0.2551 -0.2158 0.4736 0.103 Uiso 0.806(2) 1 calc R U P A 1
C21C C 0.3013(5) -0.0333(5) 0.4359(4) 0.0650(13) Uani 0.806(2) 1 d . U P A 1
H21D H 0.3701 -0.0988 0.4448 0.097 Uiso 0.806(2) 1 calc R U P A 1
H21E H 0.2734 -0.0275 0.5022 0.097 Uiso 0.806(2) 1 calc R U P A 1
H21F H 0.3181 0.0344 0.3912 0.097 Uiso 0.806(2) 1 calc R U P A 1
C19D C 0.213(3) -0.085(2) 0.3948(10) 0.068(6) Uani 0.194(2) 1 d D U P A 2
H19D H 0.1412 -0.0224 0.3958 0.082 Uiso 0.194(2) 1 calc R U P A 2
C20D C 0.291(3) -0.084(3) 0.463(2) 0.103(10) Uani 0.194(2) 1 d . U P A 2
H20G H 0.2662 -0.1135 0.5338 0.154 Uiso 0.194(2) 1 calc R U P A 2
H20H H 0.2886 -0.0076 0.4448 0.154 Uiso 0.194(2) 1 calc R U P A 2
H20I H 0.3681 -0.1316 0.4532 0.154 Uiso 0.194(2) 1 calc R U P A 2
C21D C 0.180(3) -0.196(2) 0.449(2) 0.093(9) Uani 0.194(2) 1 d . U P A 2
H21G H 0.2450 -0.2587 0.4845 0.140 Uiso 0.194(2) 1 calc R U P A 2
H21H H 0.1574 -0.2136 0.3971 0.140 Uiso 0.194(2) 1 calc R U P A 2
H21I H 0.1169 -0.1840 0.4974 0.140 Uiso 0.194(2) 1 calc R U P A 2
C22C C 0.2212(3) 0.1282(3) -0.0020(2) 0.0546(7) Uani 1 1 d . . . . .
H22C H 0.1499 0.1850 0.0107 0.066 Uiso 1 1 calc R U . . .
C23C C 0.1989(3) 0.0911(3) -0.0818(3) 0.0741(11) Uani 1 1 d . . . . .
H23G H 0.1660 0.1572 -0.1416 0.111 Uiso 1 1 calc R U . . .
H23H H 0.1464 0.0495 -0.0530 0.111 Uiso 1 1 calc R U . . .
H23I H 0.2702 0.0430 -0.1017 0.111 Uiso 1 1 calc R U . . .
C24C C 0.3112(3) 0.1842(3) -0.0462(3) 0.0740(10) Uani 1 1 d . . . . .
H24G H 0.3800 0.1311 -0.0635 0.111 Uiso 1 1 calc R U . . .
H24H H 0.3280 0.2070 0.0043 0.111 Uiso 1 1 calc R U . . .
H24I H 0.2830 0.2502 -0.1074 0.111 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
Si1A C1A 1.878(5) . ?
Si1A Si2A 2.255(4) . ?
Si2A C1C 1.861(4) . ?
Si1C C1B 1.836(18) . ?
Si1C Si2C 2.232(9) . ?
Si2C C1C 2.016(6) . ?
C1A N2A 1.347(6) . ?
C1A C5A 1.534(6) . ?
N2A C13A 1.440(5) . ?
N2A C3A 1.512(7) . ?
C3A C7A 1.525(6) . ?
C3A C4A 1.533(7) . ?
C3A C6A 1.537(6) . ?
C4A C5A 1.532(6) . ?
C5A C12A 1.538(7) . ?
C5A C8A 1.549(10) . ?
C8A C9A 1.540(6) . ?
C9A C10A 1.520(7) . ?
C10A C11A 1.535(7) . ?
C11A C12A 1.536(6) . ?
C1B N2B 1.33(2) . ?
C1B C5B 1.56(3) . ?
N2B C3B 1.50(3) . ?
N2B C13A 1.58(2) . ?
C3B C4B 1.48(3) . ?
C3B C6B 1.516(11) . ?
C3B C7B 1.525(10) . ?
C4B C5B 1.60(3) . ?
C5B C8B 1.44(4) . ?
C5B C12B 1.543(11) . ?
C8B C9B 1.540(10) . ?
C9B C10B 1.530(11) . ?
C10B C11B 1.535(10) . ?
C11B C12B 1.542(10) . ?
C13A C14A 1.404(5) . ?
C13A C18A 1.416(5) . ?
C14A C15A 1.400(5) . ?
C14A C22A 1.517(5) . ?
C14A C22B 1.542(10) . ?
C15A C16A 1.372(5) . ?
C16A C17A 1.372(5) . ?
C17A C18A 1.397(5) . ?
C18A C19A 1.517(5) . ?
C19A C20A 1.519(6) . ?
C19A C21A 1.544(5) . ?
C22A C24A 1.535(6) . ?
C22A C23A 1.541(6) . ?
C22B C23B 1.541(10) . ?
C22B C24B 1.549(10) . ?
C1C N2C 1.349(5) . ?
C1C C5C 1.527(5) . ?
N2C C13C 1.445(4) . ?
N2C C3C 1.506(4) . ?
C3C C7C 1.503(5) . ?
C3C C6C 1.513(5) . ?
C3C C4D 1.516(13) . ?
C3C C4C 1.568(10) . ?
C4C C5C 1.550(7) . ?
C4D C5C 1.610(10) . ?
C5C C12C 1.521(5) . ?
C5C C8C 1.524(6) . ?
C8C C9C 1.549(6) . ?
C9C C10C 1.479(6) . ?
C10C C11C 1.493(6) . ?
C11C C12C 1.525(5) . ?
C13C C18C 1.400(5) . ?
C13C C14C 1.413(5) . ?
C14C C15C 1.406(5) . ?
C14C C22C 1.518(5) . ?
C15C C16C 1.368(5) . ?
C16C C17C 1.375(5) . ?
C17C C18C 1.405(5) . ?
C18C C19D 1.523(10) . ?
C18C C19C 1.527(5) . ?
C19C C20C 1.531(7) . ?
C19C C21C 1.550(7) . ?
C19D C20D 1.52(4) . ?
C19D C21D 1.60(3) . ?
C22C C23C 1.533(5) . ?
C22C C24C 1.536(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1A Si1A Si2A 101.99(14) . . ?
C1C Si2A Si1A 104.24(12) . . ?
C1B Si1C Si2C 105.1(6) . . ?
C1C Si2C Si1C 97.9(3) . . ?
N2A C1A C5A 107.9(3) . . ?
N2A C1A Si1A 119.3(3) . . ?
C5A C1A Si1A 132.3(3) . . ?
C1A N2A C13A 123.5(3) . . ?
C1A N2A C3A 115.7(4) . . ?
C13A N2A C3A 120.6(4) . . ?
N2A C3A C7A 112.1(5) . . ?
N2A C3A C4A 100.7(4) . . ?
C7A C3A C4A 112.1(4) . . ?
N2A C3A C6A 111.0(4) . . ?
C7A C3A C6A 109.1(5) . . ?
C4A C3A C6A 111.7(4) . . ?
C5A C4A C3A 107.7(4) . . ?
C4A C5A C1A 104.0(3) . . ?
C4A C5A C12A 111.6(4) . . ?
C1A C5A C12A 112.8(4) . . ?
C4A C5A C8A 112.0(4) . . ?
C1A C5A C8A 108.4(4) . . ?
C12A C5A C8A 108.1(4) . . ?
C9A C8A C5A 113.3(6) . . ?
C10A C9A C8A 111.2(6) . . ?
C9A C10A C11A 111.6(5) . . ?
C10A C11A C12A 109.8(4) . . ?
C11A C12A C5A 112.1(4) . . ?
N2B C1B C5B 108.8(15) . . ?
N2B C1B Si1C 127.1(14) . . ?
C5B C1B Si1C 120.9(12) . . ?
C1B N2B C3B 117.5(17) . . ?
C1B N2B C13A 122.8(15) . . ?
C3B N2B C13A 118.3(14) . . ?
C4B C3B N2B 101.0(16) . . ?
C4B C3B C6B 115.7(19) . . ?
N2B C3B C6B 109.1(18) . . ?
C4B C3B C7B 115(2) . . ?
N2B C3B C7B 109(2) . . ?
C6B C3B C7B 107(2) . . ?
C3B C4B C5B 110.3(17) . . ?
C8B C5B C12B 116(2) . . ?
C8B C5B C1B 119.7(18) . . ?
C12B C5B C1B 103.9(15) . . ?
C8B C5B C4B 109(2) . . ?
C12B C5B C4B 106.0(18) . . ?
C1B C5B C4B 99.9(15) . . ?
C5B C8B C9B 112(3) . . ?
C10B C9B C8B 111(3) . . ?
C9B C10B C11B 113(3) . . ?
C10B C11B C12B 108(3) . . ?
C11B C12B C5B 115(2) . . ?
C14A C13A C18A 121.6(3) . . ?
C14A C13A N2A 117.1(3) . . ?
C18A C13A N2A 121.3(3) . . ?
C14A C13A N2B 133.8(6) . . ?
C18A C13A N2B 104.5(7) . . ?
C15A C14A C13A 117.4(3) . . ?
C15A C14A C22A 116.8(3) . . ?
C13A C14A C22A 125.7(3) . . ?
C15A C14A C22B 130.5(10) . . ?
C13A C14A C22B 110.1(10) . . ?
C16A C15A C14A 121.5(3) . . ?
C15A C16A C17A 120.5(3) . . ?
C16A C17A C18A 121.3(3) . . ?
C17A C18A C13A 117.4(3) . . ?
C17A C18A C19A 118.5(3) . . ?
C13A C18A C19A 123.8(3) . . ?
C18A C19A C20A 113.9(3) . . ?
C18A C19A C21A 109.1(3) . . ?
C20A C19A C21A 109.8(3) . . ?
C14A C22A C24A 110.5(3) . . ?
C14A C22A C23A 113.3(4) . . ?
C24A C22A C23A 108.2(4) . . ?
C23B C22B C14A 108.1(15) . . ?
C23B C22B C24B 110.9(18) . . ?
C14A C22B C24B 113.6(15) . . ?
N2C C1C C5C 108.8(2) . . ?
N2C C1C Si2A 124.5(2) . . ?
C5C C1C Si2A 124.8(3) . . ?
N2C C1C Si2C 111.1(3) . . ?
C5C C1C Si2C 133.3(3) . . ?
C1C N2C C13C 122.3(2) . . ?
C1C N2C C3C 115.7(2) . . ?
C13C N2C C3C 122.0(3) . . ?
C7C C3C N2C 110.9(3) . . ?
C7C C3C C6C 108.7(3) . . ?
N2C C3C C6C 111.5(3) . . ?
C7C C3C C4D 97.7(6) . . ?
N2C C3C C4D 102.1(4) . . ?
C6C C3C C4D 124.9(6) . . ?
C7C C3C C4C 121.9(6) . . ?
N2C C3C C4C 100.8(3) . . ?
C6C C3C C4C 102.6(5) . . ?
C5C C4C C3C 106.2(5) . . ?
C3C C4D C5C 105.8(7) . . ?
C12C C5C C8C 108.7(3) . . ?
C12C C5C C1C 110.7(2) . . ?
C8C C5C C1C 110.7(3) . . ?
C12C C5C C4C 120.1(5) . . ?
C8C C5C C4C 101.9(5) . . ?
C1C C5C C4C 104.3(4) . . ?
C12C C5C C4D 98.3(6) . . ?
C8C C5C C4D 125.3(6) . . ?
C1C C5C C4D 102.2(5) . . ?
C5C C8C C9C 111.4(3) . . ?
C10C C9C C8C 111.7(3) . . ?
C9C C10C C11C 112.2(4) . . ?
C10C C11C C12C 111.3(3) . . ?
C5C C12C C11C 112.3(3) . . ?
C18C C13C C14C 120.9(3) . . ?
C18C C13C N2C 120.0(3) . . ?
C14C C13C N2C 119.1(3) . . ?
C15C C14C C13C 117.8(3) . . ?
C15C C14C C22C 117.7(3) . . ?
C13C C14C C22C 124.4(3) . . ?
C16C C15C C14C 121.5(3) . . ?
C15C C16C C17C 119.8(3) . . ?
C16C C17C C18C 121.6(3) . . ?
C13C C18C C17C 117.9(3) . . ?
C13C C18C C19D 133.7(12) . . ?
C17C C18C C19D 107.3(12) . . ?
C13C C18C C19C 122.3(4) . . ?
C17C C18C C19C 119.6(4) . . ?
C18C C19C C20C 111.3(5) . . ?
C18C C19C C21C 109.4(5) . . ?
C20C C19C C21C 108.1(4) . . ?
C20D C19D C18C 113(2) . . ?
C20D C19D C21D 109.1(19) . . ?
C18C C19D C21D 119.2(19) . . ?
C14C C22C C23C 112.9(3) . . ?
C14C C22C C24C 110.4(3) . . ?
C23C C22C C24C 108.1(3) . . ?

_refine_diff_density_max         0.485
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.051

_shelxl_version_number           2012-9


####################################################################### 
# 
# 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_km102_23
_database_code_depnum_ccdc_archive 'CCDC 983863'
_audit_update_record             
;
2014-01-28 deposited with the CCDC.
2015-06-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H70 N2 Si2'
_chemical_formula_sum            'C46 H70 N2 Si2'
_chemical_formula_weight         707.22

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0006 0.0007 '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 0.0018 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0382 0.0313 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
_cell_length_a                   12.79(2)
_cell_length_b                   13.783(9)
_cell_length_c                   14.433(19)
_cell_angle_alpha                66.35(6)
_cell_angle_beta                 79.58(10)
_cell_angle_gamma                67.48(7)
_cell_volume                     2152(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    23(2)
_cell_measurement_reflns_used    9196
_cell_measurement_theta_min      1.034
_cell_measurement_theta_max      16.923

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#
_computing_data_collection       'XDS (Kabsch, 2013)'
_computing_cell_refinement       'XDS (Kabsch, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_publication_material  'enCIFer 1.4, CCDC, 2011'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
_exptl_crystal_description       bloc
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.091
_exptl_crystal_F_000             776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.065
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.017

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
_exptl_absorpt_coefficient_mu    0.059
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6688
_exptl_absorpt_correction_T_max  0.7441
_exptl_absorpt_process_details   
;
SADABS version 2013/1, multi-scan. (G. M. Sheldrick, 2008)
;

_exptl_special_details           
;
The data were measured at the PETRA beamline P11
with an Cryosystems of America low temperature device
at a temperature of 23 K and hard X-rays of 0.4769 Angstroem.
;

_diffrn_ambient_temperature      23(2)
_diffrn_radiation_wavelength     0.4769
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'Piezodiffractometer at P11 beamline (DESY)'
_diffrn_measurement_method       'φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            45604
_diffrn_reflns_av_unetI/netI     0.0833
_diffrn_reflns_av_R_equivalents  0.1179
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.034
_diffrn_reflns_theta_max         16.923
_diffrn_reflns_theta_full        16.627
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measured_fraction_theta_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_point_group_measured_fraction_full 0.971
_reflns_number_total             7928
_reflns_number_gt                4507
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;


_refine_special_details          
;
ISOR restraints were used for the two Si atoms of the alternative
site which only have 6% occupancy.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0752P)²+0.3950P] 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       0.039(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7928
_refine_ls_number_parameters     493
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1285
_refine_ls_R_factor_gt           0.0641
_refine_ls_wR_factor_ref         0.1721
_refine_ls_wR_factor_gt          0.1418
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.034
_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
Si1A Si 0.21255(8) 0.29049(8) 0.32632(7) 0.0358(3) Uani 0.932(2) 1 d . . P A 1
Si2A Si 0.20942(8) 0.26205(8) 0.18374(7) 0.0358(3) Uani 0.932(2) 1 d . . P A 1
Si1B Si 0.207(2) 0.3737(19) 0.2203(18) 0.091(7) Uani 0.068(2) 1 d . U P A 2
Si2B Si 0.2219(18) 0.1928(18) 0.2747(16) 0.081(7) Uani 0.068(2) 1 d . U P A 2
C1 C 0.3376(3) 0.3384(2) 0.2986(2) 0.0353(7) Uani 1 1 d . . . . .
N2 N 0.3423(2) 0.4074(2) 0.34162(19) 0.0350(6) Uani 1 1 d . . . . .
C3 C 0.4521(3) 0.4284(3) 0.3281(2) 0.0409(8) Uani 1 1 d . . . . .
C4 C 0.5295(3) 0.3381(3) 0.2859(3) 0.0422(8) Uani 1 1 d . . . . .
H4A H 0.5766 0.2722 0.3400 0.051 Uiso 1 1 calc R U . . .
H4B H 0.5802 0.3688 0.2313 0.051 Uiso 1 1 calc R U . . .
C5 C 0.4532(3) 0.3025(3) 0.2442(2) 0.0365(7) Uani 1 1 d . . . . .
C6 C 0.4405(3) 0.5477(3) 0.2565(3) 0.0494(9) Uani 1 1 d . . . . .
H6A H 0.4132 0.5615 0.1916 0.074 Uiso 1 1 calc R U . . .
H6B H 0.5144 0.5573 0.2458 0.074 Uiso 1 1 calc R U . . .
H6C H 0.3865 0.6015 0.2859 0.074 Uiso 1 1 calc R U . . .
C7 C 0.4943(3) 0.4094(3) 0.4285(3) 0.0492(9) Uani 1 1 d . . . . .
H7A H 0.4381 0.4615 0.4585 0.074 Uiso 1 1 calc R U . . .
H7B H 0.5661 0.4231 0.4166 0.074 Uiso 1 1 calc R U . . .
H7C H 0.5056 0.3315 0.4747 0.074 Uiso 1 1 calc R U . . .
C8 C 0.4381(3) 0.3653(3) 0.1294(2) 0.0408(8) Uani 1 1 d . . . . .
H8A H 0.3788 0.3491 0.1087 0.049 Uiso 1 1 calc R U . . .
H8B H 0.4118 0.4475 0.1140 0.049 Uiso 1 1 calc R U . . .
C9 C 0.5469(3) 0.3320(3) 0.0678(3) 0.0507(9) Uani 1 1 d . . . . .
H9A H 0.5311 0.3705 -0.0052 0.061 Uiso 1 1 calc R U . . .
H9B H 0.6034 0.3570 0.0817 0.061 Uiso 1 1 calc R U . . .
C10 C 0.5954(3) 0.2051(3) 0.0937(3) 0.0556(10) Uani 1 1 d . . . . .
H10A H 0.6686 0.1855 0.0563 0.067 Uiso 1 1 calc R U . . .
H10B H 0.5429 0.1813 0.0723 0.067 Uiso 1 1 calc R U . . .
C11 C 0.6135(3) 0.1423(3) 0.2072(3) 0.0499(9) Uani 1 1 d . . . . .
H11A H 0.6707 0.1613 0.2277 0.060 Uiso 1 1 calc R U . . .
H11B H 0.6424 0.0599 0.2226 0.060 Uiso 1 1 calc R U . . .
C12 C 0.5022(3) 0.1743(3) 0.2671(2) 0.0429(8) Uani 1 1 d . . . . .
H12A H 0.5158 0.1335 0.3404 0.052 Uiso 1 1 calc R U . . .
H12B H 0.4466 0.1511 0.2494 0.052 Uiso 1 1 calc R U . . .
C13 C 0.2454(3) 0.4649(3) 0.3939(2) 0.0366(7) Uani 1 1 d . . . . .
C14 C 0.2322(3) 0.4147(3) 0.4993(2) 0.0397(8) Uani 1 1 d . . . . .
C15 C 0.1448(3) 0.4775(3) 0.5475(3) 0.0456(8) Uani 1 1 d . . . . .
H15A H 0.1339 0.4459 0.6188 0.055 Uiso 1 1 calc R U . . .
C16 C 0.0737(3) 0.5843(3) 0.4945(3) 0.0453(9) Uani 1 1 d . . . . .
H16A H 0.0171 0.6268 0.5295 0.054 Uiso 1 1 calc R U . . .
C17 C 0.0852(3) 0.6291(3) 0.3910(3) 0.0437(8) Uani 1 1 d . . . . .
H17A H 0.0347 0.7020 0.3550 0.052 Uiso 1 1 calc R U . . .
C18 C 0.1688(3) 0.5703(3) 0.3374(2) 0.0378(7) Uani 1 1 d . . . . .
C19 C 0.1667(3) 0.6180(3) 0.2226(2) 0.0434(8) Uani 1 1 d . . . . .
H19A H 0.2355 0.5692 0.1964 0.052 Uiso 1 1 calc R U . . .
C20 C 0.1672(3) 0.7395(3) 0.1754(3) 0.0574(10) Uani 1 1 d . . . . .
H20A H 0.1776 0.7614 0.1018 0.086 Uiso 1 1 calc R U . . .
H20B H 0.2293 0.7441 0.2026 0.086 Uiso 1 1 calc R U . . .
H20C H 0.0950 0.7906 0.1917 0.086 Uiso 1 1 calc R U . . .
C21 C 0.0616(3) 0.6136(3) 0.1891(3) 0.0513(9) Uani 1 1 d . . . . .
H21A H 0.0619 0.6415 0.1151 0.077 Uiso 1 1 calc R U . . .
H21B H -0.0069 0.6610 0.2141 0.077 Uiso 1 1 calc R U . . .
H21C H 0.0629 0.5356 0.2169 0.077 Uiso 1 1 calc R U . . .
C22 C 0.3027(3) 0.2953(3) 0.5623(2) 0.0467(8) Uani 1 1 d . . . . .
H22A H 0.3645 0.2644 0.5176 0.056 Uiso 1 1 calc R U . . .
C23 C 0.3572(3) 0.2906(3) 0.6513(3) 0.0587(10) Uani 1 1 d . . . . .
H23A H 0.3982 0.3439 0.6263 0.088 Uiso 1 1 calc R U . . .
H23B H 0.4100 0.2141 0.6837 0.088 Uiso 1 1 calc R U . . .
H23C H 0.2980 0.3108 0.7007 0.088 Uiso 1 1 calc R U . . .
C24 C 0.2305(3) 0.2189(3) 0.6047(3) 0.0567(10) Uani 1 1 d . . . . .
H24A H 0.1717 0.2457 0.6514 0.085 Uiso 1 1 calc R U . . .
H24B H 0.2788 0.1413 0.6409 0.085 Uiso 1 1 calc R U . . .
H24C H 0.1949 0.2209 0.5489 0.085 Uiso 1 1 calc R U . . .
C1C C 0.0867(3) 0.2161(3) 0.2017(2) 0.0390(8) Uani 1 1 d . . . . .
N2C N 0.0936(2) 0.1172(2) 0.1979(2) 0.0384(6) Uani 1 1 d . . . . .
C3C C -0.0175(3) 0.1050(3) 0.1945(3) 0.0448(8) Uani 1 1 d . . . . .
C4C C -0.0978(11) 0.2327(12) 0.1666(15) 0.045(3) Uani 0.43(2) 1 d . U P B 1
H43A H -0.1112 0.2687 0.0931 0.054 Uiso 0.43(2) 1 calc R U P B 1
H43B H -0.1716 0.2376 0.2036 0.054 Uiso 0.43(2) 1 calc R U P B 1
C4D C -0.1048(7) 0.2055(9) 0.2192(11) 0.040(2) Uani 0.57(2) 1 d . U P B 2
H43C H -0.1313 0.1811 0.2909 0.048 Uiso 0.57(2) 1 calc R U P B 2
H43D H -0.1710 0.2415 0.1755 0.048 Uiso 0.57(2) 1 calc R U P B 2
C5C C -0.0380(3) 0.2908(3) 0.1970(2) 0.0403(8) Uani 1 1 d . . . . .
C6C C -0.0257(3) 0.0877(4) 0.0988(3) 0.0681(12) Uani 1 1 d . . . . .
H6D H -0.0167 0.1516 0.0394 0.102 Uiso 1 1 calc R U . . .
H6E H -0.0999 0.0825 0.0981 0.102 Uiso 1 1 calc R U . . .
H6F H 0.0340 0.0178 0.0971 0.102 Uiso 1 1 calc R U . . .
C7C C -0.0339(3) 0.0053(4) 0.2845(3) 0.0736(12) Uani 1 1 d . . . . .
H7D H -0.1062 -0.0012 0.2796 0.110 Uiso 1 1 calc R U . . .
H7E H -0.0343 0.0170 0.3473 0.110 Uiso 1 1 calc R U . . .
H7F H 0.0281 -0.0640 0.2848 0.110 Uiso 1 1 calc R U . . .
C8C C -0.0587(3) 0.3972(3) 0.1027(3) 0.0667(11) Uani 1 1 d . . . . .
H8C H -0.0391 0.3761 0.0422 0.080 Uiso 1 1 calc R U . . .
H8D H -0.0084 0.4371 0.1019 0.080 Uiso 1 1 calc R U . . .
C9C C -0.1825(3) 0.4774(4) 0.0973(3) 0.0807(14) Uani 1 1 d . . . . .
H9C H -0.1910 0.5472 0.0367 0.097 Uiso 1 1 calc R U . . .
H9D H -0.2326 0.4409 0.0909 0.097 Uiso 1 1 calc R U . . .
C10C C -0.2171(3) 0.5071(3) 0.1910(4) 0.0761(14) Uani 1 1 d . . . . .
H10C H -0.1734 0.5521 0.1926 0.091 Uiso 1 1 calc R U . . .
H10D H -0.2984 0.5538 0.1885 0.091 Uiso 1 1 calc R U . . .
C11C C -0.1969(3) 0.4040(3) 0.2843(3) 0.0570(10) Uani 1 1 d . . . . .
H11C H -0.2466 0.3632 0.2860 0.068 Uiso 1 1 calc R U . . .
H11D H -0.2166 0.4261 0.3443 0.068 Uiso 1 1 calc R U . . .
C12C C -0.0737(3) 0.3260(3) 0.2891(3) 0.0528(9) Uani 1 1 d . . . . .
H12C H -0.0637 0.2578 0.3514 0.063 Uiso 1 1 calc R U . . .
H12D H -0.0244 0.3650 0.2923 0.063 Uiso 1 1 calc R U . . .
C13C C 0.2013(3) 0.0286(2) 0.1963(2) 0.0374(7) Uani 1 1 d . . . . .
C14C C 0.2554(3) 0.0300(2) 0.1015(2) 0.0377(8) Uani 1 1 d . . . . .
C15C C 0.3541(3) -0.0622(3) 0.1022(3) 0.0438(8) Uani 1 1 d . . . . .
H15C H 0.3918 -0.0647 0.0397 0.053 Uiso 1 1 calc R U . . .
C16C C 0.3977(3) -0.1484(3) 0.1901(3) 0.0454(8) Uani 1 1 d . . . . .
H16C H 0.4631 -0.2109 0.1880 0.054 Uiso 1 1 calc R U . . .
C17C C 0.3466(3) -0.1443(3) 0.2817(3) 0.0486(9) Uani 1 1 d . . . . .
H17C H 0.3786 -0.2038 0.3423 0.058 Uiso 1 1 calc R U . . .
C18C C 0.2490(3) -0.0551(3) 0.2877(3) 0.0432(8) Uani 1 1 d . . . . .
C19C C 0.2051(3) -0.0501(3) 0.3910(3) 0.0544(9) Uani 1 1 d . . . . .
H19C H 0.1345 0.0173 0.3823 0.065 Uiso 1 1 calc R U . . .
C20C C 0.1770(4) -0.1565(3) 0.4618(3) 0.0758(13) Uani 1 1 d . . . . .
H20D H 0.1253 -0.1684 0.4283 0.114 Uiso 1 1 calc R U . . .
H20E H 0.1410 -0.1463 0.5248 0.114 Uiso 1 1 calc R U . . .
H20F H 0.2470 -0.2223 0.4771 0.114 Uiso 1 1 calc R U . . .
C21C C 0.2934(4) -0.0375(3) 0.4414(3) 0.0678(12) Uani 1 1 d . . . . .
H21D H 0.3621 -0.1045 0.4529 0.102 Uiso 1 1 calc R U . . .
H21E H 0.2623 -0.0296 0.5062 0.102 Uiso 1 1 calc R U . . .
H21F H 0.3120 0.0296 0.3970 0.102 Uiso 1 1 calc R U . . .
C22C C 0.2196(3) 0.1252(3) 0.0015(2) 0.0442(8) Uani 1 1 d . . . . .
H22C H 0.1486 0.1838 0.0133 0.053 Uiso 1 1 calc R U . . .
C23C C 0.1967(3) 0.0867(3) -0.0772(3) 0.0601(10) Uani 1 1 d . . . . .
H23D H 0.1662 0.1527 -0.1380 0.090 Uiso 1 1 calc R U . . .
H23E H 0.1418 0.0476 -0.0485 0.090 Uiso 1 1 calc R U . . .
H23F H 0.2675 0.0354 -0.0951 0.090 Uiso 1 1 calc R U . . .
C24C C 0.3117(3) 0.1793(3) -0.0427(3) 0.0582(10) Uani 1 1 d . . . . .
H24D H 0.3805 0.1242 -0.0587 0.087 Uiso 1 1 calc R U . . .
H24E H 0.3283 0.2028 0.0070 0.087 Uiso 1 1 calc R U . . .
H24F H 0.2848 0.2452 -0.1044 0.087 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
Si1A C1 1.876(4) . ?
Si1A Si2A 2.254(3) . ?
Si2A C1C 1.849(4) . ?
Si1B C1 1.99(2) . ?
Si1B Si2B 2.23(3) . ?
Si2B C1C 2.04(2) . ?
C1 N2 1.352(3) . ?
C1 C5 1.542(5) . ?
N2 C13 1.457(4) . ?
N2 C3 1.503(4) . ?
C3 C6 1.517(5) . ?
C3 C7 1.526(5) . ?
C3 C4 1.532(4) . ?
C4 C5 1.540(4) . ?
C5 C8 1.539(5) . ?
C5 C12 1.543(4) . ?
C8 C9 1.526(5) . ?
C9 C10 1.520(5) . ?
C10 C11 1.527(5) . ?
C11 C12 1.532(5) . ?
C13 C14 1.405(5) . ?
C13 C18 1.409(5) . ?
C14 C15 1.395(5) . ?
C14 C22 1.519(5) . ?
C15 C16 1.379(5) . ?
C16 C17 1.373(5) . ?
C17 C18 1.392(4) . ?
C18 C19 1.519(5) . ?
C19 C20 1.536(4) . ?
C19 C21 1.537(5) . ?
C22 C24 1.536(5) . ?
C22 C23 1.537(5) . ?
C1C N2C 1.355(4) . ?
C1C C5C 1.528(5) . ?
N2C C13C 1.453(4) . ?
N2C C3C 1.505(4) . ?
C3C C7C 1.520(5) . ?
C3C C6C 1.521(5) . ?
C3C C4D 1.535(10) . ?
C3C C4C 1.584(13) . ?
C4C C5C 1.513(13) . ?
C4D C5C 1.608(9) . ?
C5C C8C 1.518(5) . ?
C5C C12C 1.529(5) . ?
C8C C9C 1.539(6) . ?
C9C C10C 1.510(6) . ?
C10C C11C 1.486(6) . ?
C11C C12C 1.525(5) . ?
C13C C18C 1.405(5) . ?
C13C C14C 1.413(5) . ?
C14C C15C 1.406(5) . ?
C14C C22C 1.508(5) . ?
C15C C16C 1.368(5) . ?
C16C C17C 1.377(5) . ?
C17C C18C 1.396(5) . ?
C18C C19C 1.514(5) . ?
C19C C21C 1.544(5) . ?
C19C C20C 1.547(5) . ?
C22C C24C 1.538(5) . ?
C22C C23C 1.543(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Si1A Si2A 101.22(13) . . ?
C1C Si2A Si1A 105.14(13) . . ?
C1 Si1B Si2B 92.7(11) . . ?
C1C Si2B Si1B 97.3(10) . . ?
N2 C1 C5 106.9(3) . . ?
N2 C1 Si1A 119.8(2) . . ?
C5 C1 Si1A 132.7(2) . . ?
N2 C1 Si1B 122.7(7) . . ?
C5 C1 Si1B 113.8(7) . . ?
C1 N2 C13 122.9(3) . . ?
C1 N2 C3 116.6(2) . . ?
C13 N2 C3 120.4(2) . . ?
N2 C3 C6 111.4(3) . . ?
N2 C3 C7 111.9(3) . . ?
C6 C3 C7 108.3(3) . . ?
N2 C3 C4 100.7(2) . . ?
C6 C3 C4 113.4(3) . . ?
C7 C3 C4 111.0(3) . . ?
C3 C4 C5 107.5(3) . . ?
C8 C5 C4 112.5(3) . . ?
C8 C5 C1 108.5(3) . . ?
C4 C5 C1 103.9(2) . . ?
C8 C5 C12 108.9(3) . . ?
C4 C5 C12 110.5(3) . . ?
C1 C5 C12 112.5(2) . . ?
C9 C8 C5 112.9(3) . . ?
C10 C9 C8 111.3(3) . . ?
C9 C10 C11 111.0(3) . . ?
C10 C11 C12 110.5(3) . . ?
C11 C12 C5 111.3(3) . . ?
C14 C13 C18 121.9(3) . . ?
C14 C13 N2 119.1(3) . . ?
C18 C13 N2 119.0(3) . . ?
C15 C14 C13 117.2(3) . . ?
C15 C14 C22 118.5(3) . . ?
C13 C14 C22 124.2(3) . . ?
C16 C15 C14 121.8(3) . . ?
C17 C16 C15 119.8(3) . . ?
C16 C17 C18 121.7(3) . . ?
C17 C18 C13 117.4(3) . . ?
C17 C18 C19 118.7(3) . . ?
C13 C18 C19 123.7(3) . . ?
C18 C19 C20 113.3(3) . . ?
C18 C19 C21 109.4(3) . . ?
C20 C19 C21 109.4(3) . . ?
C14 C22 C24 111.0(3) . . ?
C14 C22 C23 112.5(3) . . ?
C24 C22 C23 108.3(3) . . ?
N2C C1C C5C 108.1(3) . . ?
N2C C1C Si2A 124.0(2) . . ?
C5C C1C Si2A 126.3(2) . . ?
N2C C1C Si2B 110.1(6) . . ?
C5C C1C Si2B 133.9(6) . . ?
C1C N2C C13C 122.2(3) . . ?
C1C N2C C3C 115.7(3) . . ?
C13C N2C C3C 122.0(2) . . ?
N2C C3C C7C 111.4(3) . . ?
N2C C3C C6C 111.7(3) . . ?
C7C C3C C6C 107.8(3) . . ?
N2C C3C C4D 103.1(4) . . ?
C7C C3C C4D 101.9(6) . . ?
C6C C3C C4D 120.6(6) . . ?
N2C C3C C4C 99.6(5) . . ?
C7C C3C C4C 126.0(8) . . ?
C6C C3C C4C 99.7(7) . . ?
C5C C4C C3C 106.8(8) . . ?
C3C C4D C5C 104.5(5) . . ?
C4C C5C C8C 98.4(8) . . ?
C4C C5C C1C 104.8(5) . . ?
C8C C5C C1C 110.7(3) . . ?
C4C C5C C12C 123.7(8) . . ?
C8C C5C C12C 107.9(3) . . ?
C1C C5C C12C 110.6(3) . . ?
C8C C5C C4D 121.3(6) . . ?
C1C C5C C4D 104.0(4) . . ?
C12C C5C C4D 101.9(5) . . ?
C5C C8C C9C 112.4(3) . . ?
C10C C9C C8C 110.6(4) . . ?
C11C C10C C9C 111.3(3) . . ?
C10C C11C C12C 111.5(3) . . ?
C11C C12C C5C 111.6(3) . . ?
C18C C13C C14C 121.9(3) . . ?
C18C C13C N2C 119.8(3) . . ?
C14C C13C N2C 118.3(3) . . ?
C15C C14C C13C 116.8(3) . . ?
C15C C14C C22C 117.9(3) . . ?
C13C C14C C22C 125.3(3) . . ?
C16C C15C C14C 122.0(3) . . ?
C15C C16C C17C 119.8(3) . . ?
C16C C17C C18C 121.7(3) . . ?
C17C C18C C13C 117.4(3) . . ?
C17C C18C C19C 118.6(3) . . ?
C13C C18C C19C 123.9(3) . . ?
C18C C19C C21C 110.2(3) . . ?
C18C C19C C20C 112.1(3) . . ?
C21C C19C C20C 108.9(3) . . ?
C14C C22C C24C 110.1(3) . . ?
C14C C22C C23C 112.8(3) . . ?
C24C C22C C23C 108.5(3) . . ?

_refine_diff_density_max         0.314
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.058

_shelxl_version_number           2013-4


# start Validation Reply Form
_vrf_PLAT410_km102_23            
;
PROBLEM: Short Intra H...H Contact  H8C    ..  H43A    ..       1.87 Ang.  
RESPONSE: Due to disorder the abovementioned atoms are closer than
the PLATON checkcif validation threshold.
;
# end Validation Reply Form




####################################################################### 
# 
# 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_km343
_database_code_depnum_ccdc_archive 'CCDC 1060365'
_audit_update_record             
;
2015-04-18 deposited with the CCDC.
2015-06-18 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        'carbene stabilized silicondislenide'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H31 N Se2 Si, (C4 H8 O)'
_chemical_formula_sum            'C24 H39 N O Se2 Si'
_chemical_formula_weight         543.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.7943 1.1372 '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'

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

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

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

_cell_length_a                   14.6952(6)
_cell_length_b                   10.0800(4)
_cell_length_c                   17.7472(7)
_cell_angle_alpha                90
_cell_angle_beta                 109.567(2)
_cell_angle_gamma                90
_cell_volume                     2477.03(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_F_000             1120
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_colour            orange
_exptl_absorpt_coefficient_mu    4.300
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3765
_exptl_absorpt_correction_T_max  0.4684
_exptl_absorpt_process_details   
;
SADABS version 2015/1, multi-scan. (G. M. Sheldrick, 2015)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Incoatec Microfocus source with mirror optics'
_diffrn_measurement_device_type  'Bruker Photon 100'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22159
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.394
_diffrn_reflns_theta_max         70.093
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.979
_reflns_number_total             4611
_reflns_number_gt                3674
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0464P)²+3.1905P] 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         4611
_refine_ls_number_parameters     301
_refine_ls_number_restraints     264
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0393
_refine_ls_wR_factor_ref         0.1002
_refine_ls_wR_factor_gt          0.0922
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.009
_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
Se1 Se 0.37973(3) 0.48848(4) -0.01157(2) 0.02407(11) Uani 1 1 d . U . . .
Se2 Se 0.55832(3) 0.34421(4) 0.18273(2) 0.02800(12) Uani 1 1 d . U . . .
Si1 Si 0.52444(7) 0.49314(9) 0.09065(5) 0.0205(2) Uani 1 1 d . U . . .
N1 N 0.4761(2) 0.7026(3) 0.18381(17) 0.0236(6) Uani 1 1 d . U . . .
C1 C 0.5414(3) 0.6471(3) 0.1588(2) 0.0220(7) Uani 1 1 d . U . . .
C2 C 0.6409(3) 0.7048(4) 0.2038(2) 0.0297(8) Uani 1 1 d . U . . .
C4 C 0.5198(3) 0.7836(4) 0.2612(2) 0.0333(9) Uani 1 1 d . U . . .
C5 C 0.6672(3) 0.7999(4) 0.1478(3) 0.0398(10) Uani 1 1 d . U . . .
H5A H 0.6705 0.7512 0.1010 0.060 Uiso 1 1 calc R U . . .
H5B H 0.7301 0.8404 0.1759 0.060 Uiso 1 1 calc R U . . .
H5C H 0.6180 0.8695 0.1305 0.060 Uiso 1 1 calc R U . . .
C6 C 0.7233(3) 0.6047(5) 0.2332(3) 0.0511(13) Uani 1 1 d . U . . .
H6A H 0.7310 0.5579 0.1873 0.077 Uiso 1 1 calc R U . . .
H6B H 0.7084 0.5406 0.2689 0.077 Uiso 1 1 calc R U . . .
H6C H 0.7833 0.6514 0.2622 0.077 Uiso 1 1 calc R U . . .
C9 C 0.3717(3) 0.7004(4) 0.1418(2) 0.0232(7) Uani 1 1 d . U . . .
C10 C 0.3120(3) 0.6048(4) 0.1593(2) 0.0270(8) Uani 1 1 d . U . . .
C11 C 0.2128(3) 0.6123(4) 0.1170(3) 0.0335(9) Uani 1 1 d . U . . .
H11 H 0.1707 0.5499 0.1284 0.040 Uiso 1 1 calc R U . . .
C12 C 0.1743(3) 0.7074(4) 0.0594(3) 0.0347(9) Uani 1 1 d . U . . .
H12 H 0.1069 0.7096 0.0310 0.042 Uiso 1 1 calc R U . . .
C13 C 0.2351(3) 0.7997(4) 0.0433(2) 0.0286(8) Uani 1 1 d . U . . .
H13 H 0.2083 0.8655 0.0038 0.034 Uiso 1 1 calc R U . . .
C14 C 0.3338(3) 0.7990(4) 0.0833(2) 0.0236(7) Uani 1 1 d . U . . .
C15 C 0.3462(3) 0.4914(4) 0.2191(2) 0.0318(8) Uani 1 1 d . U . . .
H15 H 0.4183 0.4938 0.2419 0.038 Uiso 1 1 calc R U . . .
C16 C 0.3053(4) 0.5055(5) 0.2873(3) 0.0420(10) Uani 1 1 d . U . . .
H16A H 0.2346 0.5040 0.2655 0.063 Uiso 1 1 calc R U . . .
H16B H 0.3269 0.5897 0.3151 0.063 Uiso 1 1 calc R U . . .
H16C H 0.3283 0.4318 0.3249 0.063 Uiso 1 1 calc R U . . .
C17 C 0.3153(3) 0.3573(4) 0.1783(3) 0.0386(10) Uani 1 1 d . U . . .
H17A H 0.2446 0.3512 0.1590 0.058 Uiso 1 1 calc R U . . .
H17B H 0.3423 0.2859 0.2168 0.058 Uiso 1 1 calc R U . . .
H17C H 0.3390 0.3488 0.1332 0.058 Uiso 1 1 calc R U . . .
C18 C 0.3940(3) 0.9024(4) 0.0588(2) 0.0288(8) Uani 1 1 d . U . . .
H18 H 0.4614 0.8982 0.0976 0.035 Uiso 1 1 calc R U . . .
C19 C 0.3557(3) 1.0440(4) 0.0603(3) 0.0360(9) Uani 1 1 d . U . . .
H19A H 0.4026 1.1081 0.0537 0.054 Uiso 1 1 calc R U . . .
H19B H 0.3460 1.0596 0.1116 0.054 Uiso 1 1 calc R U . . .
H19C H 0.2942 1.0546 0.0167 0.054 Uiso 1 1 calc R U . . .
C20 C 0.3975(4) 0.8706(4) -0.0242(3) 0.0420(11) Uani 1 1 d . U . . .
H20A H 0.3316 0.8679 -0.0627 0.063 Uiso 1 1 calc R U . . .
H20B H 0.4285 0.7842 -0.0231 0.063 Uiso 1 1 calc R U . . .
H20C H 0.4346 0.9392 -0.0402 0.063 Uiso 1 1 calc R U . . .
C3A C 0.6294(5) 0.7559(9) 0.2805(4) 0.0296(16) Uani 0.604(9) 1 d . U P A 1
H3A H 0.6672 0.8382 0.2982 0.036 Uiso 0.604(9) 1 calc R U P A 1
H3B H 0.6521 0.6888 0.3235 0.036 Uiso 0.604(9) 1 calc R U P A 1
C7A C 0.4989(6) 0.9398(7) 0.2434(4) 0.0367(19) Uani 0.604(9) 1 d . U P A 1
H7AA H 0.5339 0.9713 0.2085 0.055 Uiso 0.604(9) 1 calc R U P A 1
H7AB H 0.5207 0.9891 0.2939 0.055 Uiso 0.604(9) 1 calc R U P A 1
H7AC H 0.4295 0.9538 0.2170 0.055 Uiso 0.604(9) 1 calc R U P A 1
C8A C 0.4805(6) 0.7470(8) 0.3227(4) 0.0389(19) Uani 0.604(9) 1 d . U P A 1
H8A1 H 0.4894 0.6516 0.3332 0.058 Uiso 0.604(9) 1 calc R U P A 1
H8A2 H 0.4115 0.7683 0.3050 0.058 Uiso 0.604(9) 1 calc R U P A 1
H8A3 H 0.5141 0.7963 0.3718 0.058 Uiso 0.604(9) 1 calc R U P A 1
C3B C 0.6124(9) 0.8125(13) 0.2581(8) 0.034(3) Uani 0.396(9) 1 d . U P A 2
H3B1 H 0.6603 0.8113 0.3128 0.041 Uiso 0.396(9) 1 calc R U P A 2
H3B2 H 0.6125 0.9022 0.2354 0.041 Uiso 0.396(9) 1 calc R U P A 2
C7B C 0.4520(9) 0.8843(11) 0.2705(7) 0.041(3) Uani 0.396(9) 1 d . U P A 2
H7BA H 0.4342 0.9442 0.2244 0.061 Uiso 0.396(9) 1 calc R U P A 2
H7BB H 0.4828 0.9352 0.3195 0.061 Uiso 0.396(9) 1 calc R U P A 2
H7BC H 0.3940 0.8405 0.2739 0.061 Uiso 0.396(9) 1 calc R U P A 2
C8B C 0.5327(10) 0.6734(12) 0.3327(6) 0.041(3) Uani 0.396(9) 1 d . U P A 2
H8B1 H 0.5712 0.5986 0.3250 0.062 Uiso 0.396(9) 1 calc R U P A 2
H8B2 H 0.4690 0.6416 0.3309 0.062 Uiso 0.396(9) 1 calc R U P A 2
H8B3 H 0.5656 0.7147 0.3848 0.062 Uiso 0.396(9) 1 calc R U P A 2
O5T_1 O 0.5720(3) 0.1949(5) 0.5170(2) 0.0723(12) Uani 1 1 d . U . . .
C1T_1 C 0.5871(6) 0.3267(8) 0.5003(4) 0.095(2) Uani 1 1 d . U . . .
H1TA_1 H 0.6518 0.3552 0.5355 0.114 Uiso 1 1 calc R U . . .
H1TB_1 H 0.5385 0.3835 0.5119 0.114 Uiso 1 1 calc R U . . .
C2T_1 C 0.5801(5) 0.3442(6) 0.4173(4) 0.0673(15) Uani 1 1 d . U . . .
H2TA_1 H 0.6404 0.3826 0.4135 0.081 Uiso 1 1 calc R U . . .
H2TB_1 H 0.5255 0.4033 0.3891 0.081 Uiso 1 1 calc R U . . .
C3T_1 C 0.5640(7) 0.2090(7) 0.3831(4) 0.086(2) Uani 1 1 d . U . . .
H3TA_1 H 0.6078 0.1904 0.3524 0.103 Uiso 1 1 calc R U . . .
H3TB_1 H 0.4964 0.1978 0.3474 0.103 Uiso 1 1 calc R U . . .
C4T_1 C 0.5858(5) 0.1194(7) 0.4547(4) 0.0747(19) Uani 1 1 d . U . . .
H4TA_1 H 0.5420 0.0418 0.4422 0.090 Uiso 1 1 calc R U . . .
H4TB_1 H 0.6533 0.0871 0.4705 0.090 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
Se1 Si1 2.2874(10) . ?
Se1 Si1 2.3045(10) 3_665 ?
Se2 Si1 2.1510(10) . ?
Si1 C1 1.931(4) . ?
Si1 Se1 2.3046(10) 3_665 ?
N1 C1 1.311(5) . ?
N1 C9 1.464(5) . ?
N1 C4 1.540(4) . ?
C1 C2 1.528(5) . ?
C2 C3A 1.516(8) . ?
C2 C5 1.521(6) . ?
C2 C6 1.527(6) . ?
C2 C3B 1.599(12) . ?
C4 C3B 1.410(13) . ?
C4 C8A 1.444(8) . ?
C4 C7B 1.469(12) . ?
C4 C3A 1.555(9) . ?
C4 C7A 1.615(8) . ?
C4 C8B 1.650(12) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C9 C10 1.407(5) . ?
C9 C14 1.410(5) . ?
C10 C11 1.401(6) . ?
C10 C15 1.525(5) . ?
C11 C12 1.377(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.384(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.386(5) . ?
C13 H13 0.9500 . ?
C14 C18 1.522(5) . ?
C15 C16 1.527(5) . ?
C15 C17 1.528(6) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C20 1.525(5) . ?
C18 C19 1.538(5) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C3A H3A 0.9900 . ?
C3A H3B 0.9900 . ?
C7A H7AA 0.9800 . ?
C7A H7AB 0.9800 . ?
C7A H7AC 0.9800 . ?
C8A H8A1 0.9800 . ?
C8A H8A2 0.9800 . ?
C8A H8A3 0.9800 . ?
C3B H3B1 0.9900 . ?
C3B H3B2 0.9900 . ?
C7B H7BA 0.9800 . ?
C7B H7BB 0.9800 . ?
C7B H7BC 0.9800 . ?
C8B H8B1 0.9800 . ?
C8B H8B2 0.9800 . ?
C8B H8B3 0.9800 . ?
O5T_1 C1T_1 1.395(8) . ?
O5T_1 C4T_1 1.411(7) . ?
C1T_1 C2T_1 1.453(8) . ?
C1T_1 H1TA_1 0.9900 . ?
C1T_1 H1TB_1 0.9900 . ?
C2T_1 C3T_1 1.478(9) . ?
C2T_1 H2TA_1 0.9900 . ?
C2T_1 H2TB_1 0.9900 . ?
C3T_1 C4T_1 1.503(8) . ?
C3T_1 H3TA_1 0.9900 . ?
C3T_1 H3TB_1 0.9900 . ?
C4T_1 H4TA_1 0.9900 . ?
C4T_1 H4TB_1 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Si1 Se1 Si1 83.45(4) . 3_665 ?
C1 Si1 Se2 97.86(11) . . ?
C1 Si1 Se1 113.81(11) . . ?
Se2 Si1 Se1 120.35(4) . . ?
C1 Si1 Se1 109.85(11) . 3_665 ?
Se2 Si1 Se1 119.05(4) . 3_665 ?
Se1 Si1 Se1 96.55(4) . 3_665 ?
C1 N1 C9 125.6(3) . . ?
C1 N1 C4 113.2(3) . . ?
C9 N1 C4 121.0(3) . . ?
N1 C1 C2 110.0(3) . . ?
N1 C1 Si1 126.9(3) . . ?
C2 C1 Si1 122.3(3) . . ?
C3A C2 C5 120.1(5) . . ?
C3A C2 C6 103.4(5) . . ?
C5 C2 C6 107.1(4) . . ?
C3A C2 C1 102.9(4) . . ?
C5 C2 C1 107.8(3) . . ?
C6 C2 C1 116.0(3) . . ?
C5 C2 C3B 98.1(6) . . ?
C6 C2 C3B 125.5(6) . . ?
C1 C2 C3B 100.1(5) . . ?
C3B C4 C7B 124.1(8) . . ?
C3B C4 N1 101.3(5) . . ?
C8A C4 N1 112.7(4) . . ?
C7B C4 N1 111.7(5) . . ?
C8A C4 C3A 115.7(5) . . ?
N1 C4 C3A 101.1(4) . . ?
C8A C4 C7A 107.4(5) . . ?
N1 C4 C7A 110.3(4) . . ?
C3A C4 C7A 109.5(5) . . ?
C3B C4 C8B 107.8(8) . . ?
C7B C4 C8B 106.6(7) . . ?
N1 C4 C8B 103.6(5) . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C10 C9 C14 121.6(3) . . ?
C10 C9 N1 121.5(3) . . ?
C14 C9 N1 116.9(3) . . ?
C11 C10 C9 117.3(4) . . ?
C11 C10 C15 117.0(4) . . ?
C9 C10 C15 125.7(4) . . ?
C12 C11 C10 122.0(4) . . ?
C12 C11 H11 119.0 . . ?
C10 C11 H11 119.0 . . ?
C11 C12 C13 119.3(4) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
C12 C13 C14 121.9(4) . . ?
C12 C13 H13 119.1 . . ?
C14 C13 H13 119.1 . . ?
C13 C14 C9 117.9(4) . . ?
C13 C14 C18 117.3(3) . . ?
C9 C14 C18 124.7(3) . . ?
C10 C15 C16 110.8(3) . . ?
C10 C15 C17 110.9(3) . . ?
C16 C15 C17 108.9(4) . . ?
C10 C15 H15 108.7 . . ?
C16 C15 H15 108.7 . . ?
C17 C15 H15 108.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 C20 110.0(3) . . ?
C14 C18 C19 112.3(3) . . ?
C20 C18 C19 110.1(3) . . ?
C14 C18 H18 108.1 . . ?
C20 C18 H18 108.1 . . ?
C19 C18 H18 108.1 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
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 . . ?
C2 C3A C4 106.4(5) . . ?
C2 C3A H3A 110.5 . . ?
C4 C3A H3A 110.5 . . ?
C2 C3A H3B 110.5 . . ?
C4 C3A H3B 110.5 . . ?
H3A C3A H3B 108.6 . . ?
C4 C7A H7AA 109.5 . . ?
C4 C7A H7AB 109.5 . . ?
H7AA C7A H7AB 109.5 . . ?
C4 C7A H7AC 109.5 . . ?
H7AA C7A H7AC 109.5 . . ?
H7AB C7A H7AC 109.5 . . ?
C4 C8A H8A1 109.5 . . ?
C4 C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
C4 C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
C4 C3B C2 109.5(8) . . ?
C4 C3B H3B1 109.8 . . ?
C2 C3B H3B1 109.8 . . ?
C4 C3B H3B2 109.8 . . ?
C2 C3B H3B2 109.8 . . ?
H3B1 C3B H3B2 108.2 . . ?
C4 C7B H7BA 109.5 . . ?
C4 C7B H7BB 109.5 . . ?
H7BA C7B H7BB 109.5 . . ?
C4 C7B H7BC 109.5 . . ?
H7BA C7B H7BC 109.5 . . ?
H7BB C7B H7BC 109.5 . . ?
C4 C8B H8B1 109.5 . . ?
C4 C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C4 C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C1T_1 O5T_1 C4T_1 105.8(5) . . ?
O5T_1 C1T_1 C2T_1 111.7(6) . . ?
O5T_1 C1T_1 H1TA_1 109.3 . . ?
C2T_1 C1T_1 H1TA_1 109.3 . . ?
O5T_1 C1T_1 H1TB_1 109.3 . . ?
C2T_1 C1T_1 H1TB_1 109.3 . . ?
H1TA_1 C1T_1 H1TB_1 108.0 . . ?
C1T_1 C2T_1 C3T_1 104.5(6) . . ?
C1T_1 C2T_1 H2TA_1 110.8 . . ?
C3T_1 C2T_1 H2TA_1 110.8 . . ?
C1T_1 C2T_1 H2TB_1 110.8 . . ?
C3T_1 C2T_1 H2TB_1 110.8 . . ?
H2TA_1 C2T_1 H2TB_1 108.9 . . ?
C2T_1 C3T_1 C4T_1 104.4(6) . . ?
C2T_1 C3T_1 H3TA_1 110.9 . . ?
C4T_1 C3T_1 H3TA_1 110.9 . . ?
C2T_1 C3T_1 H3TB_1 110.9 . . ?
C4T_1 C3T_1 H3TB_1 110.9 . . ?
H3TA_1 C3T_1 H3TB_1 108.9 . . ?
O5T_1 C4T_1 C3T_1 107.0(5) . . ?
O5T_1 C4T_1 H4TA_1 110.3 . . ?
C3T_1 C4T_1 H4TA_1 110.3 . . ?
O5T_1 C4T_1 H4TB_1 110.3 . . ?
C3T_1 C4T_1 H4TB_1 110.3 . . ?
H4TA_1 C4T_1 H4TB_1 108.6 . . ?

_refine_diff_density_max         1.006
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.089

_shelxl_version_number           2014/6




_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
