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

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

data_kob40c
_database_code_depnum_ccdc_archive 'CCDC 1061425'
_audit_update_record             
;
2015-04-23 deposited with the CCDC.
2015-06-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H45 N3 Si'
_chemical_formula_sum            'C33 H45 N3 Si'
_chemical_formula_weight         511.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.049(5)
_cell_length_b                   9.540(3)
_cell_length_c                   18.295(8)
_cell_angle_alpha                99.41(3)
_cell_angle_beta                 98.90(3)
_cell_angle_gamma                97.53(3)
_cell_volume                     1519.5(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6212
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      30.83

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             556
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9413
_exptl_absorpt_correction_T_max  0.9792
_exptl_absorpt_process_details   'Sadabs 2008/1 (Bruker 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17741
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.15
_diffrn_reflns_theta_max         26.02
_reflns_number_total             5986
_reflns_number_gt                4879
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP/POV-Ray
_computing_publication_material  Bruker-SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0423P)²+0.6708P] 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         5986
_refine_ls_number_parameters     344
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_ref         0.1000
_refine_ls_wR_factor_gt          0.0918
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si Si 0.74535(5) 0.20957(4) 0.23064(2) 0.01508(11) Uani 1 1 d . . .
N1 N 0.93993(13) 0.18665(12) 0.20471(6) 0.0126(3) Uani 1 1 d . . .
N2 N 0.81589(13) 0.03811(13) 0.25834(6) 0.0126(3) Uani 1 1 d . . .
N3 N 0.62105(14) 0.14173(14) 0.14706(7) 0.0189(3) Uani 1 1 d . . .
C1 C 0.95216(16) 0.07685(15) 0.24164(8) 0.0121(3) Uani 1 1 d . . .
C2 C 1.09062(16) 0.01312(15) 0.25904(8) 0.0128(3) Uani 1 1 d . . .
C3 C 1.19040(16) 0.00823(16) 0.20788(8) 0.0165(3) Uani 1 1 d . . .
H3 H 1.1696 0.0480 0.1638 0.020 Uiso 1 1 calc R . .
C4 C 1.31981(17) -0.05432(17) 0.22104(9) 0.0200(3) Uani 1 1 d . . .
H4 H 1.3870 -0.0575 0.1859 0.024 Uiso 1 1 calc R . .
C5 C 1.35087(17) -0.11208(16) 0.28531(9) 0.0192(3) Uani 1 1 d . . .
H5 H 1.4391 -0.1554 0.2942 0.023 Uiso 1 1 calc R . .
C6 C 1.25307(17) -0.10669(16) 0.33673(9) 0.0184(3) Uani 1 1 d . . .
H6 H 1.2752 -0.1453 0.3811 0.022 Uiso 1 1 calc R . .
C7 C 1.12313(16) -0.04524(16) 0.32366(8) 0.0161(3) Uani 1 1 d . . .
H7 H 1.0561 -0.0429 0.3588 0.019 Uiso 1 1 calc R . .
C8 C 1.06322(16) 0.29403(15) 0.20028(8) 0.0134(3) Uani 1 1 d . . .
C9 C 1.15323(16) 0.37981(15) 0.26606(8) 0.0159(3) Uani 1 1 d . . .
C10 C 1.26398(17) 0.48939(16) 0.25820(9) 0.0199(3) Uani 1 1 d . . .
H10 H 1.3265 0.5476 0.3020 0.024 Uiso 1 1 calc R . .
C11 C 1.28498(18) 0.51545(17) 0.18809(9) 0.0217(3) Uani 1 1 d . . .
H11 H 1.3604 0.5915 0.1840 0.026 Uiso 1 1 calc R . .
C12 C 1.19573(17) 0.43029(16) 0.12395(9) 0.0190(3) Uani 1 1 d . . .
H12 H 1.2110 0.4482 0.0759 0.023 Uiso 1 1 calc R . .
C13 C 1.08396(16) 0.31876(15) 0.12862(8) 0.0153(3) Uani 1 1 d . . .
C14 C 1.13168(18) 0.36244(17) 0.34531(8) 0.0194(3) Uani 1 1 d . . .
H14 H 1.0522 0.2765 0.3406 0.023 Uiso 1 1 calc R . .
C15 C 1.2775(2) 0.3349(2) 0.39173(10) 0.0345(4) Uani 1 1 d . . .
H15A H 1.3120 0.2513 0.3648 0.052 Uiso 1 1 calc R . .
H15B H 1.2577 0.3161 0.4407 0.052 Uiso 1 1 calc R . .
H15C H 1.3560 0.4197 0.3994 0.052 Uiso 1 1 calc R . .
C16 C 1.0751(2) 0.49345(19) 0.38500(10) 0.0330(4) Uani 1 1 d . . .
H16A H 1.1512 0.5794 0.3904 0.049 Uiso 1 1 calc R . .
H16B H 1.0580 0.4784 0.4349 0.049 Uiso 1 1 calc R . .
H16C H 0.9800 0.5066 0.3551 0.049 Uiso 1 1 calc R . .
C17 C 0.98438(17) 0.22856(16) 0.05752(8) 0.0179(3) Uani 1 1 d . . .
H17 H 0.9351 0.1388 0.0712 0.022 Uiso 1 1 calc R . .
C18 C 1.0751(2) 0.1838(2) -0.00386(9) 0.0288(4) Uani 1 1 d . . .
H18A H 1.0074 0.1204 -0.0470 0.043 Uiso 1 1 calc R . .
H18B H 1.1548 0.1326 0.0160 0.043 Uiso 1 1 calc R . .
H18C H 1.1212 0.2696 -0.0200 0.043 Uiso 1 1 calc R . .
C19 C 0.85821(19) 0.30827(19) 0.02747(10) 0.0270(4) Uani 1 1 d . . .
H19A H 0.9034 0.3994 0.0159 0.041 Uiso 1 1 calc R . .
H19B H 0.7949 0.3278 0.0657 0.041 Uiso 1 1 calc R . .
H19C H 0.7957 0.2486 -0.0184 0.041 Uiso 1 1 calc R . .
C20 C 0.77248(15) -0.07362(16) 0.29780(8) 0.0135(3) Uani 1 1 d . . .
C21 C 0.75423(16) -0.21929(16) 0.26289(8) 0.0150(3) Uani 1 1 d . . .
C22 C 0.70646(17) -0.32420(17) 0.30309(9) 0.0199(3) Uani 1 1 d . . .
H22 H 0.6925 -0.4230 0.2802 0.024 Uiso 1 1 calc R . .
C23 C 0.67919(18) -0.28678(18) 0.37557(9) 0.0225(4) Uani 1 1 d . . .
H23 H 0.6469 -0.3594 0.4021 0.027 Uiso 1 1 calc R . .
C24 C 0.69913(17) -0.14330(18) 0.40916(9) 0.0207(3) Uani 1 1 d . . .
H24 H 0.6808 -0.1186 0.4590 0.025 Uiso 1 1 calc R . .
C25 C 0.74536(16) -0.03422(17) 0.37174(8) 0.0165(3) Uani 1 1 d . . .
C26 C 0.78850(17) -0.26739(16) 0.18454(8) 0.0168(3) Uani 1 1 d . . .
H26 H 0.8248 -0.1793 0.1652 0.020 Uiso 1 1 calc R . .
C27 C 0.91487(19) -0.36019(18) 0.18726(9) 0.0242(4) Uani 1 1 d . . .
H27A H 0.9411 -0.3823 0.1371 0.036 Uiso 1 1 calc R . .
H27B H 0.8798 -0.4500 0.2033 0.036 Uiso 1 1 calc R . .
H27C H 1.0044 -0.3075 0.2231 0.036 Uiso 1 1 calc R . .
C28 C 0.64658(18) -0.34869(18) 0.12963(9) 0.0233(4) Uani 1 1 d . . .
H28A H 0.6705 -0.3709 0.0790 0.035 Uiso 1 1 calc R . .
H28B H 0.5665 -0.2888 0.1289 0.035 Uiso 1 1 calc R . .
H28C H 0.6119 -0.4384 0.1458 0.035 Uiso 1 1 calc R . .
C29 C 0.77064(18) 0.12224(17) 0.41238(8) 0.0207(3) Uani 1 1 d . . .
H29 H 0.7956 0.1841 0.3754 0.025 Uiso 1 1 calc R . .
C30 C 0.90485(19) 0.15314(19) 0.47768(9) 0.0260(4) Uani 1 1 d . . .
H30A H 0.9966 0.1325 0.4585 0.039 Uiso 1 1 calc R . .
H30B H 0.8848 0.0922 0.5144 0.039 Uiso 1 1 calc R . .
H30C H 0.9193 0.2546 0.5020 0.039 Uiso 1 1 calc R . .
C31 C 0.6278(2) 0.1635(2) 0.43915(11) 0.0369(5) Uani 1 1 d . . .
H31A H 0.5446 0.1469 0.3959 0.055 Uiso 1 1 calc R . .
H31B H 0.6469 0.2654 0.4631 0.055 Uiso 1 1 calc R . .
H31C H 0.6004 0.1045 0.4756 0.055 Uiso 1 1 calc R . .
C32 C 0.49154(18) 0.21236(19) 0.12576(10) 0.0247(4) Uani 1 1 d . . .
H32A H 0.5045 0.2546 0.0813 0.037 Uiso 1 1 calc R . .
H32B H 0.4847 0.2884 0.1676 0.037 Uiso 1 1 calc R . .
H32C H 0.3984 0.1415 0.1140 0.037 Uiso 1 1 calc R . .
C33 C 0.63402(18) 0.02284(17) 0.08914(9) 0.0222(3) Uani 1 1 d . . .
H33A H 0.5427 -0.0499 0.0799 0.033 Uiso 1 1 calc R . .
H33B H 0.7230 -0.0201 0.1058 0.033 Uiso 1 1 calc R . .
H33C H 0.6451 0.0582 0.0426 0.033 Uiso 1 1 calc R . .


_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
Si N3 1.7249(15) . ?
Si N1 1.9232(16) . ?
Si N2 1.9455(14) . ?
Si C1 2.3947(18) . ?
N1 C1 1.3434(18) . ?
N1 C8 1.4341(19) . ?
N2 C1 1.3359(19) . ?
N2 C20 1.4288(19) . ?
N3 C33 1.450(2) . ?
N3 C32 1.460(2) . ?
C1 C2 1.477(2) . ?
C2 C7 1.395(2) . ?
C2 C3 1.397(2) . ?
C3 C4 1.389(2) . ?
C4 C5 1.384(2) . ?
C5 C6 1.387(2) . ?
C6 C7 1.387(2) . ?
C8 C13 1.405(2) . ?
C8 C9 1.408(2) . ?
C9 C10 1.392(2) . ?
C9 C14 1.525(2) . ?
C10 C11 1.382(2) . ?
C11 C12 1.383(2) . ?
C12 C13 1.392(2) . ?
C13 C17 1.521(2) . ?
C14 C16 1.529(2) . ?
C14 C15 1.532(2) . ?
C17 C18 1.529(2) . ?
C17 C19 1.534(2) . ?
C20 C21 1.408(2) . ?
C20 C25 1.411(2) . ?
C21 C22 1.398(2) . ?
C21 C26 1.523(2) . ?
C22 C23 1.384(2) . ?
C23 C24 1.382(2) . ?
C24 C25 1.391(2) . ?
C25 C29 1.526(2) . ?
C26 C28 1.531(2) . ?
C26 C27 1.535(2) . ?
C29 C31 1.527(2) . ?
C29 C30 1.527(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
N3 Si N1 103.38(7) . . ?
N3 Si N2 102.70(7) . . ?
N1 Si N2 67.41(6) . . ?
N3 Si C1 110.39(6) . . ?
N1 Si C1 34.09(5) . . ?
N2 Si C1 33.89(5) . . ?
C1 N1 C8 125.13(12) . . ?
C1 N1 Si 92.56(9) . . ?
C8 N1 Si 129.52(10) . . ?
C1 N2 C20 127.46(12) . . ?
C1 N2 Si 91.82(9) . . ?
C20 N2 Si 139.22(10) . . ?
C33 N3 C32 112.61(13) . . ?
C33 N3 Si 127.20(10) . . ?
C32 N3 Si 120.03(11) . . ?
N2 C1 N1 106.51(12) . . ?
N2 C1 C2 127.82(13) . . ?
N1 C1 C2 125.67(13) . . ?
N2 C1 Si 54.29(8) . . ?
N1 C1 Si 53.35(7) . . ?
C2 C1 Si 170.81(10) . . ?
C7 C2 C3 119.05(13) . . ?
C7 C2 C1 122.33(13) . . ?
C3 C2 C1 118.60(13) . . ?
C4 C3 C2 120.48(14) . . ?
C5 C4 C3 119.99(14) . . ?
C4 C5 C6 119.94(14) . . ?
C7 C6 C5 120.35(14) . . ?
C6 C7 C2 120.19(14) . . ?
C13 C8 C9 120.96(14) . . ?
C13 C8 N1 118.10(13) . . ?
C9 C8 N1 120.76(13) . . ?
C10 C9 C8 118.16(14) . . ?
C10 C9 C14 118.41(14) . . ?
C8 C9 C14 123.39(13) . . ?
C11 C10 C9 121.48(15) . . ?
C10 C11 C12 119.72(15) . . ?
C11 C12 C13 121.13(15) . . ?
C12 C13 C8 118.54(14) . . ?
C12 C13 C17 120.38(14) . . ?
C8 C13 C17 121.06(13) . . ?
C9 C14 C16 110.77(13) . . ?
C9 C14 C15 111.45(14) . . ?
C16 C14 C15 111.11(15) . . ?
C13 C17 C18 112.52(14) . . ?
C13 C17 C19 110.80(13) . . ?
C18 C17 C19 110.41(14) . . ?
C21 C20 C25 121.05(13) . . ?
C21 C20 N2 120.56(13) . . ?
C25 C20 N2 118.38(13) . . ?
C22 C21 C20 118.21(14) . . ?
C22 C21 C26 118.76(13) . . ?
C20 C21 C26 123.01(13) . . ?
C23 C22 C21 121.22(15) . . ?
C24 C23 C22 119.73(14) . . ?
C23 C24 C25 121.61(15) . . ?
C24 C25 C20 118.16(14) . . ?
C24 C25 C29 119.46(14) . . ?
C20 C25 C29 122.33(13) . . ?
C21 C26 C28 111.58(13) . . ?
C21 C26 C27 111.09(13) . . ?
C28 C26 C27 110.32(13) . . ?
C25 C29 C31 111.67(14) . . ?
C25 C29 C30 111.41(13) . . ?
C31 C29 C30 110.99(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 Si N1 C1 -106.70(9) . . . . ?
N2 Si N1 C1 -8.33(8) . . . . ?
N3 Si N1 C8 111.71(13) . . . . ?
N2 Si N1 C8 -149.91(13) . . . . ?
C1 Si N1 C8 -141.59(16) . . . . ?
N3 Si N2 C1 107.76(10) . . . . ?
N1 Si N2 C1 8.37(8) . . . . ?
N3 Si N2 C20 -86.71(16) . . . . ?
N1 Si N2 C20 173.90(16) . . . . ?
C1 Si N2 C20 165.53(19) . . . . ?
N1 Si N3 C33 34.37(14) . . . . ?
N2 Si N3 C33 -35.08(14) . . . . ?
C1 Si N3 C33 -0.57(15) . . . . ?
N1 Si N3 C32 -140.77(11) . . . . ?
N2 Si N3 C32 149.79(11) . . . . ?
C1 Si N3 C32 -175.70(11) . . . . ?
C20 N2 C1 N1 -179.71(13) . . . . ?
Si N2 C1 N1 -11.57(11) . . . . ?
C20 N2 C1 C2 0.7(2) . . . . ?
Si N2 C1 C2 168.83(13) . . . . ?
C20 N2 C1 Si -168.14(16) . . . . ?
C8 N1 C1 N2 155.84(13) . . . . ?
Si N1 C1 N2 11.72(11) . . . . ?
C8 N1 C1 C2 -24.6(2) . . . . ?
Si N1 C1 C2 -168.68(12) . . . . ?
C8 N1 C1 Si 144.12(15) . . . . ?
N3 Si C1 N2 -82.37(10) . . . . ?
N1 Si C1 N2 -166.13(13) . . . . ?
N3 Si C1 N1 83.76(10) . . . . ?
N2 Si C1 N1 166.13(13) . . . . ?
N3 Si C1 C2 171.0(6) . . . . ?
N1 Si C1 C2 87.3(7) . . . . ?
N2 Si C1 C2 -106.6(7) . . . . ?
N2 C1 C2 C7 -32.4(2) . . . . ?
N1 C1 C2 C7 148.10(14) . . . . ?
Si C1 C2 C7 67.5(7) . . . . ?
N2 C1 C2 C3 146.04(15) . . . . ?
N1 C1 C2 C3 -33.5(2) . . . . ?
Si C1 C2 C3 -114.1(6) . . . . ?
C7 C2 C3 C4 0.2(2) . . . . ?
C1 C2 C3 C4 -178.23(14) . . . . ?
C2 C3 C4 C5 -0.2(2) . . . . ?
C3 C4 C5 C6 -0.4(2) . . . . ?
C4 C5 C6 C7 0.8(2) . . . . ?
C5 C6 C7 C2 -0.7(2) . . . . ?
C3 C2 C7 C6 0.2(2) . . . . ?
C1 C2 C7 C6 178.60(13) . . . . ?
C1 N1 C8 C13 127.32(15) . . . . ?
Si N1 C8 C13 -102.05(14) . . . . ?
C1 N1 C8 C9 -57.59(19) . . . . ?
Si N1 C8 C9 73.04(17) . . . . ?
C13 C8 C9 C10 -0.3(2) . . . . ?
N1 C8 C9 C10 -175.29(13) . . . . ?
C13 C8 C9 C14 177.29(13) . . . . ?
N1 C8 C9 C14 2.3(2) . . . . ?
C8 C9 C10 C11 0.7(2) . . . . ?
C14 C9 C10 C11 -177.01(14) . . . . ?
C9 C10 C11 C12 -0.8(2) . . . . ?
C10 C11 C12 C13 0.4(2) . . . . ?
C11 C12 C13 C8 0.0(2) . . . . ?
C11 C12 C13 C17 178.52(13) . . . . ?
C9 C8 C13 C12 0.0(2) . . . . ?
N1 C8 C13 C12 175.05(12) . . . . ?
C9 C8 C13 C17 -178.52(13) . . . . ?
N1 C8 C13 C17 -3.4(2) . . . . ?
C10 C9 C14 C16 65.15(19) . . . . ?
C8 C9 C14 C16 -112.48(17) . . . . ?
C10 C9 C14 C15 -59.11(18) . . . . ?
C8 C9 C14 C15 123.27(16) . . . . ?
C12 C13 C17 C18 44.87(19) . . . . ?
C8 C13 C17 C18 -136.66(15) . . . . ?
C12 C13 C17 C19 -79.28(17) . . . . ?
C8 C13 C17 C19 99.19(16) . . . . ?
C1 N2 C20 C21 -73.03(19) . . . . ?
Si N2 C20 C21 125.31(14) . . . . ?
C1 N2 C20 C25 108.30(16) . . . . ?
Si N2 C20 C25 -53.4(2) . . . . ?
C25 C20 C21 C22 0.8(2) . . . . ?
N2 C20 C21 C22 -177.79(13) . . . . ?
C25 C20 C21 C26 -177.34(13) . . . . ?
N2 C20 C21 C26 4.0(2) . . . . ?
C20 C21 C22 C23 -0.7(2) . . . . ?
C26 C21 C22 C23 177.57(14) . . . . ?
C21 C22 C23 C24 0.1(2) . . . . ?
C22 C23 C24 C25 0.4(2) . . . . ?
C23 C24 C25 C20 -0.3(2) . . . . ?
C23 C24 C25 C29 -178.00(14) . . . . ?
C21 C20 C25 C24 -0.4(2) . . . . ?
N2 C20 C25 C24 178.28(13) . . . . ?
C21 C20 C25 C29 177.30(13) . . . . ?
N2 C20 C25 C29 -4.0(2) . . . . ?
C22 C21 C26 C28 63.93(18) . . . . ?
C20 C21 C26 C28 -117.90(15) . . . . ?
C22 C21 C26 C27 -59.63(18) . . . . ?
C20 C21 C26 C27 118.54(15) . . . . ?
C24 C25 C29 C31 -58.18(19) . . . . ?
C20 C25 C29 C31 124.17(16) . . . . ?
C24 C25 C29 C30 66.55(18) . . . . ?
C20 C25 C29 C30 -111.10(16) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.043
####################################################################### 
# 
# 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_kob39c
_database_code_depnum_ccdc_archive 'CCDC 1061426'
_audit_update_record             
;
2015-04-23 deposited with the CCDC.
2015-06-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C66 H90 N6 O2 Si2'
_chemical_formula_sum            'C66 H90 N6 O2 Si2'
_chemical_formula_weight         1055.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   26.888(4)
_cell_length_b                   17.559(2)
_cell_length_c                   12.8562(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.712(17)
_cell_angle_gamma                90.00
_cell_volume                     6057.0(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5000
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      29.05

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2288
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  image-plate_Stoe-IPDS
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24116
_diffrn_reflns_av_R_equivalents  0.0759
_diffrn_reflns_av_sigmaI/netI    0.0939
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.56
_diffrn_reflns_theta_max         26.08
_reflns_number_total             5990
_reflns_number_gt                3036
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Stoe-IPDS
_computing_cell_refinement       Stoe-IPDS
_computing_data_reduction        Stoe-IPDS
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP/POV-Ray
_computing_publication_material  Bruker-SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0385P)²+0.0000P] 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         5990
_refine_ls_number_parameters     353
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0380
_refine_ls_wR_factor_ref         0.0869
_refine_ls_wR_factor_gt          0.0748
_refine_ls_goodness_of_fit_ref   0.802
_refine_ls_restrained_S_all      0.802
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si Si 0.045448(19) 0.32743(3) 0.74774(4) 0.02977(13) Uani 1 1 d . . .
O O -0.00291(4) 0.31844(7) 0.66034(9) 0.0334(3) Uani 1 1 d . . .
N1 N 0.09512(6) 0.28864(9) 0.64466(11) 0.0325(4) Uani 1 1 d . . .
N2 N 0.08858(5) 0.25333(8) 0.80312(11) 0.0295(4) Uani 1 1 d . . .
N3 N 0.06855(6) 0.41744(9) 0.76204(12) 0.0360(4) Uani 1 1 d . . .
C1 C 0.11250(7) 0.23994(10) 0.71578(14) 0.0290(4) Uani 1 1 d . . .
C2 C 0.14732(7) 0.17617(11) 0.69926(14) 0.0311(4) Uani 1 1 d . . .
C3 C 0.14197(8) 0.13740(11) 0.60450(15) 0.0373(5) Uani 1 1 d . . .
H3 H 0.1179 0.1531 0.5538 0.045 Uiso 1 1 calc R . .
C4 C 0.17198(8) 0.07605(12) 0.58520(17) 0.0458(5) Uani 1 1 d . . .
H4 H 0.1680 0.0503 0.5220 0.055 Uiso 1 1 calc R . .
C5 C 0.20792(8) 0.05307(12) 0.65986(17) 0.0494(6) Uani 1 1 d . . .
H5 H 0.2283 0.0118 0.6469 0.059 Uiso 1 1 calc R . .
C6 C 0.21383(8) 0.09112(12) 0.75418(17) 0.0459(5) Uani 1 1 d . . .
H6 H 0.2384 0.0756 0.8040 0.055 Uiso 1 1 calc R . .
C7 C 0.18348(7) 0.15184(11) 0.77434(15) 0.0382(5) Uani 1 1 d . . .
H7 H 0.1872 0.1767 0.8383 0.046 Uiso 1 1 calc R . .
C8 C 0.11712(7) 0.30638(10) 0.54837(14) 0.0319(4) Uani 1 1 d . . .
C9 C 0.08776(7) 0.29947(11) 0.45388(14) 0.0358(5) Uani 1 1 d . . .
C10 C 0.10781(8) 0.32479(13) 0.36227(15) 0.0439(5) Uani 1 1 d . . .
H10 H 0.0888 0.3211 0.2994 0.053 Uiso 1 1 calc R . .
C11 C 0.15481(8) 0.35491(13) 0.36295(16) 0.0478(6) Uani 1 1 d . . .
H11 H 0.1673 0.3720 0.3013 0.057 Uiso 1 1 calc R . .
C12 C 0.18350(8) 0.35968(12) 0.45552(16) 0.0431(5) Uani 1 1 d . . .
H12 H 0.2156 0.3793 0.4551 0.052 Uiso 1 1 calc R . .
C13 C 0.16577(7) 0.33584(11) 0.54987(14) 0.0350(5) Uani 1 1 d . . .
C14 C 0.03649(7) 0.26430(13) 0.44687(15) 0.0422(5) Uani 1 1 d . . .
H14 H 0.0293 0.2477 0.5171 0.051 Uiso 1 1 calc R . .
C15 C -0.00376(8) 0.32129(15) 0.41014(16) 0.0543(6) Uani 1 1 d . . .
H15A H 0.0026 0.3393 0.3418 0.081 Uiso 1 1 calc R . .
H15B H -0.0035 0.3635 0.4576 0.081 Uiso 1 1 calc R . .
H15C H -0.0358 0.2969 0.4080 0.081 Uiso 1 1 calc R . .
C16 C 0.03506(9) 0.19365(14) 0.37706(17) 0.0555(6) Uani 1 1 d . . .
H16A H 0.0421 0.2081 0.3075 0.083 Uiso 1 1 calc R . .
H16B H 0.0026 0.1708 0.3762 0.083 Uiso 1 1 calc R . .
H16C H 0.0596 0.1577 0.4037 0.083 Uiso 1 1 calc R . .
C17 C 0.20110(7) 0.34303(11) 0.64721(15) 0.0400(5) Uani 1 1 d . . .
H17 H 0.1830 0.3274 0.7074 0.048 Uiso 1 1 calc R . .
C18 C 0.21944(10) 0.42445(14) 0.66606(19) 0.0619(7) Uani 1 1 d . . .
H18A H 0.2359 0.4419 0.6064 0.093 Uiso 1 1 calc R . .
H18B H 0.2424 0.4257 0.7264 0.093 Uiso 1 1 calc R . .
H18C H 0.1916 0.4570 0.6772 0.093 Uiso 1 1 calc R . .
C19 C 0.24600(7) 0.29052(13) 0.64095(17) 0.0479(6) Uani 1 1 d . . .
H19A H 0.2347 0.2397 0.6253 0.072 Uiso 1 1 calc R . .
H19B H 0.2652 0.2908 0.7066 0.072 Uiso 1 1 calc R . .
H19C H 0.2663 0.3081 0.5871 0.072 Uiso 1 1 calc R . .
C20 C 0.10196(7) 0.22112(11) 0.90548(14) 0.0309(4) Uani 1 1 d . . .
C21 C 0.13345(7) 0.26353(11) 0.97623(14) 0.0343(5) Uani 1 1 d . . .
C22 C 0.14630(8) 0.23160(13) 1.07388(15) 0.0458(5) Uani 1 1 d . . .
H22 H 0.1672 0.2585 1.1212 0.055 Uiso 1 1 calc R . .
C23 C 0.12883(9) 0.16132(14) 1.10189(17) 0.0554(6) Uani 1 1 d . . .
H23 H 0.1376 0.1414 1.1675 0.066 Uiso 1 1 calc R . .
C24 C 0.09834(9) 0.12094(13) 1.03207(17) 0.0511(6) Uani 1 1 d . . .
H24 H 0.0867 0.0734 1.0514 0.061 Uiso 1 1 calc R . .
C25 C 0.08416(7) 0.14935(11) 0.93220(15) 0.0380(5) Uani 1 1 d . . .
C26 C 0.15496(7) 0.34043(11) 0.95157(15) 0.0382(5) Uani 1 1 d . . .
H26 H 0.1393 0.3576 0.8847 0.046 Uiso 1 1 calc R . .
C27 C 0.21144(8) 0.33631(13) 0.94110(17) 0.0507(6) Uani 1 1 d . . .
H27A H 0.2183 0.3018 0.8859 0.076 Uiso 1 1 calc R . .
H27B H 0.2275 0.3185 1.0054 0.076 Uiso 1 1 calc R . .
H27C H 0.2238 0.3860 0.9254 0.076 Uiso 1 1 calc R . .
C28 C 0.14415(9) 0.39979(13) 1.03453(18) 0.0560(6) Uani 1 1 d . . .
H28A H 0.1536 0.4493 1.0113 0.084 Uiso 1 1 calc R . .
H28B H 0.1628 0.3877 1.0985 0.084 Uiso 1 1 calc R . .
H28C H 0.1092 0.3995 1.0458 0.084 Uiso 1 1 calc R . .
C29 C 0.05167(8) 0.10002(11) 0.85919(16) 0.0429(5) Uani 1 1 d . . .
H29 H 0.0467 0.1270 0.7926 0.051 Uiso 1 1 calc R . .
C30 C 0.00050(8) 0.08768(13) 0.90169(18) 0.0534(6) Uani 1 1 d . . .
H30A H -0.0171 0.1352 0.9020 0.080 Uiso 1 1 calc R . .
H30B H 0.0046 0.0682 0.9715 0.080 Uiso 1 1 calc R . .
H30C H -0.0181 0.0519 0.8583 0.080 Uiso 1 1 calc R . .
C31 C 0.07689(10) 0.02367(13) 0.8384(2) 0.0615(7) Uani 1 1 d . . .
H31A H 0.0555 -0.0063 0.7920 0.092 Uiso 1 1 calc R . .
H31B H 0.0832 -0.0032 0.9030 0.092 Uiso 1 1 calc R . .
H31C H 0.1079 0.0327 0.8073 0.092 Uiso 1 1 calc R . .
C32 C 0.08247(9) 0.46460(13) 0.67585(19) 0.0604(7) Uani 1 1 d . . .
H32A H 0.0869 0.4331 0.6161 0.091 Uiso 1 1 calc R . .
H32B H 0.1131 0.4907 0.6952 0.091 Uiso 1 1 calc R . .
H32C H 0.0567 0.5012 0.6592 0.091 Uiso 1 1 calc R . .
C33 C 0.05732(9) 0.46576(13) 0.85013(17) 0.0515(6) Uani 1 1 d . . .
H33A H 0.0865 0.4941 0.8731 0.077 Uiso 1 1 calc R . .
H33B H 0.0471 0.4345 0.9062 0.077 Uiso 1 1 calc R . .
H33C H 0.0310 0.5004 0.8289 0.077 Uiso 1 1 calc R . .


_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
Si O 1.6699(13) . ?
Si N3 1.7036(17) . ?
Si O 1.7044(13) 2_556 ?
Si N2 1.8543(16) . ?
Si N1 2.0574(16) . ?
Si C1 2.4239(19) . ?
Si Si 2.4486(11) 2_556 ?
O Si 1.7045(13) 2_556 ?
N1 C1 1.315(2) . ?
N1 C8 1.440(2) . ?
N2 C1 1.350(2) . ?
N2 C20 1.456(2) . ?
N3 C32 1.452(3) . ?
N3 C33 1.462(3) . ?
C1 C2 1.484(3) . ?
C2 C7 1.392(3) . ?
C2 C3 1.395(3) . ?
C3 C4 1.378(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.378(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.385(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.377(3) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C13 1.406(3) . ?
C8 C9 1.410(3) . ?
C9 C10 1.399(3) . ?
C9 C14 1.508(3) . ?
C10 C11 1.369(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.378(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.396(3) . ?
C12 H12 0.9300 . ?
C13 C17 1.527(3) . ?
C14 C15 1.526(3) . ?
C14 C16 1.530(3) . ?
C14 H14 0.9800 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C19 1.525(3) . ?
C17 C18 1.527(3) . ?
C17 H17 0.9800 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C25 1.399(3) . ?
C20 C21 1.414(3) . ?
C21 C22 1.398(3) . ?
C21 C26 1.511(3) . ?
C22 C23 1.377(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.373(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.407(3) . ?
C24 H24 0.9300 . ?
C25 C29 1.513(3) . ?
C26 C28 1.533(3) . ?
C26 C27 1.535(3) . ?
C26 H26 0.9800 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 C30 1.528(3) . ?
C29 C31 1.534(3) . ?
C29 H29 0.9800 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O Si N3 115.02(8) . . ?
O Si O 85.96(6) . 2_556 ?
N3 Si O 105.52(7) . 2_556 ?
O Si N2 129.22(7) . . ?
N3 Si N2 113.26(8) . . ?
O Si N2 95.73(6) 2_556 . ?
O Si N1 92.57(6) . . ?
N3 Si N1 97.43(7) . . ?
O Si N1 155.32(7) 2_556 . ?
N2 Si N1 66.36(6) . . ?
O Si C1 112.41(6) . . ?
N3 Si C1 109.65(7) . . ?
O Si C1 126.78(7) 2_556 . ?
N2 Si C1 33.56(6) . . ?
N1 Si C1 32.86(6) . . ?
O Si Si 44.04(4) . 2_556 ?
N3 Si Si 110.79(5) . 2_556 ?
O Si Si 42.93(4) 2_556 2_556 ?
N2 Si Si 126.25(5) . 2_556 ?
N1 Si Si 134.90(5) . 2_556 ?
C1 Si Si 139.34(5) . 2_556 ?
Si O Si 93.04(6) . 2_556 ?
C1 N1 C8 126.23(15) . . ?
C1 N1 Si 89.07(11) . . ?
C8 N1 Si 143.30(12) . . ?
C1 N2 C20 125.51(15) . . ?
C1 N2 Si 97.04(11) . . ?
C20 N2 Si 137.01(12) . . ?
C32 N3 C33 109.66(17) . . ?
C32 N3 Si 123.85(15) . . ?
C33 N3 Si 121.99(13) . . ?
N1 C1 N2 107.33(15) . . ?
N1 C1 C2 126.17(16) . . ?
N2 C1 C2 126.12(16) . . ?
N1 C1 Si 58.07(9) . . ?
N2 C1 Si 49.40(9) . . ?
C2 C1 Si 170.34(13) . . ?
C7 C2 C3 118.93(17) . . ?
C7 C2 C1 123.45(17) . . ?
C3 C2 C1 117.58(17) . . ?
C4 C3 C2 120.69(19) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C5 C4 C3 119.7(2) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 120.30(19) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C7 C6 C5 120.2(2) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C6 C7 C2 120.18(19) . . ?
C6 C7 H7 119.9 . . ?
C2 C7 H7 119.9 . . ?
C13 C8 C9 120.79(17) . . ?
C13 C8 N1 120.09(16) . . ?
C9 C8 N1 118.92(16) . . ?
C10 C9 C8 118.23(18) . . ?
C10 C9 C14 118.71(17) . . ?
C8 C9 C14 123.04(17) . . ?
C11 C10 C9 121.53(19) . . ?
C11 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
C10 C11 C12 119.59(19) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
C11 C12 C13 121.9(2) . . ?
C11 C12 H12 119.1 . . ?
C13 C12 H12 119.1 . . ?
C12 C13 C8 117.93(18) . . ?
C12 C13 C17 117.26(17) . . ?
C8 C13 C17 124.81(16) . . ?
C9 C14 C15 112.16(18) . . ?
C9 C14 C16 110.82(17) . . ?
C15 C14 C16 111.07(17) . . ?
C9 C14 H14 107.5 . . ?
C15 C14 H14 107.5 . . ?
C16 C14 H14 107.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C19 C17 C18 109.01(18) . . ?
C19 C17 C13 111.07(16) . . ?
C18 C17 C13 112.65(18) . . ?
C19 C17 H17 108.0 . . ?
C18 C17 H17 108.0 . . ?
C13 C17 H17 108.0 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C25 C20 C21 121.11(17) . . ?
C25 C20 N2 120.23(16) . . ?
C21 C20 N2 118.66(16) . . ?
C22 C21 C20 118.00(18) . . ?
C22 C21 C26 118.12(18) . . ?
C20 C21 C26 123.86(17) . . ?
C23 C22 C21 121.7(2) . . ?
C23 C22 H22 119.1 . . ?
C21 C22 H22 119.1 . . ?
C24 C23 C22 119.4(2) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C23 C24 C25 121.9(2) . . ?
C23 C24 H24 119.0 . . ?
C25 C24 H24 119.0 . . ?
C20 C25 C24 117.82(19) . . ?
C20 C25 C29 123.82(17) . . ?
C24 C25 C29 118.34(18) . . ?
C21 C26 C28 111.67(17) . . ?
C21 C26 C27 111.76(17) . . ?
C28 C26 C27 109.05(17) . . ?
C21 C26 H26 108.1 . . ?
C28 C26 H26 108.1 . . ?
C27 C26 H26 108.1 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C25 C29 C30 110.88(17) . . ?
C25 C29 C31 111.37(18) . . ?
C30 C29 C31 110.91(18) . . ?
C25 C29 H29 107.8 . . ?
C30 C29 H29 107.8 . . ?
C31 C29 H29 107.8 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N3 C32 H32A 109.5 . . ?
N3 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N3 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N3 C33 H33A 109.5 . . ?
N3 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N3 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 Si O Si -94.64(8) . . . 2_556 ?
O Si O Si 10.61(9) 2_556 . . 2_556 ?
N2 Si O Si 104.71(8) . . . 2_556 ?
N1 Si O Si 165.93(6) . . . 2_556 ?
C1 Si O Si 138.93(6) . . . 2_556 ?
O Si N1 C1 -129.32(11) . . . . ?
N3 Si N1 C1 115.03(12) . . . . ?
O Si N1 C1 -43.4(2) 2_556 . . . ?
N2 Si N1 C1 2.84(10) . . . . ?
Si Si N1 C1 -115.52(10) 2_556 . . . ?
O Si N1 C8 65.4(2) . . . . ?
N3 Si N1 C8 -50.3(2) . . . . ?
O Si N1 C8 151.30(19) 2_556 . . . ?
N2 Si N1 C8 -162.5(2) . . . . ?
C1 Si N1 C8 -165.3(3) . . . . ?
Si Si N1 C8 79.2(2) 2_556 . . . ?
O Si N2 C1 70.12(13) . . . . ?
N3 Si N2 C1 -90.81(12) . . . . ?
O Si N2 C1 159.57(11) 2_556 . . . ?
N1 Si N2 C1 -2.79(10) . . . . ?
Si Si N2 C1 126.60(10) 2_556 . . . ?
O Si N2 C20 -117.63(17) . . . . ?
N3 Si N2 C20 81.45(18) . . . . ?
O Si N2 C20 -28.17(18) 2_556 . . . ?
N1 Si N2 C20 169.47(19) . . . . ?
C1 Si N2 C20 172.3(2) . . . . ?
Si Si N2 C20 -61.14(19) 2_556 . . . ?
O Si N3 C32 -51.63(18) . . . . ?
O Si N3 C32 -144.42(16) 2_556 . . . ?
N2 Si N3 C32 112.15(17) . . . . ?
N1 Si N3 C32 44.74(17) . . . . ?
C1 Si N3 C32 76.21(18) . . . . ?
Si Si N3 C32 -99.45(16) 2_556 . . . ?
O Si N3 C33 102.10(16) . . . . ?
O Si N3 C33 9.30(17) 2_556 . . . ?
N2 Si N3 C33 -94.12(16) . . . . ?
N1 Si N3 C33 -161.54(16) . . . . ?
C1 Si N3 C33 -130.07(16) . . . . ?
Si Si N3 C33 54.27(17) 2_556 . . . ?
C8 N1 C1 N2 165.42(17) . . . . ?
Si N1 C1 N2 -3.75(13) . . . . ?
C8 N1 C1 C2 -21.3(3) . . . . ?
Si N1 C1 C2 169.51(17) . . . . ?
C8 N1 C1 Si 169.2(2) . . . . ?
C20 N2 C1 N1 -169.33(16) . . . . ?
Si N2 C1 N1 4.19(15) . . . . ?
C20 N2 C1 C2 17.4(3) . . . . ?
Si N2 C1 C2 -169.07(16) . . . . ?
C20 N2 C1 Si -173.5(2) . . . . ?
O Si C1 N1 56.71(12) . . . . ?
N3 Si C1 N1 -72.56(12) . . . . ?
O Si C1 N1 159.01(11) 2_556 . . . ?
N2 Si C1 N1 -175.29(17) . . . . ?
Si Si C1 N1 101.21(12) 2_556 . . . ?
O Si C1 N2 -128.00(11) . . . . ?
N3 Si C1 N2 102.73(12) . . . . ?
O Si C1 N2 -25.70(13) 2_556 . . . ?
N1 Si C1 N2 175.29(17) . . . . ?
Si Si C1 N2 -83.50(13) 2_556 . . . ?
O Si C1 C2 -62.2(8) . . . . ?
N3 Si C1 C2 168.6(8) . . . . ?
O Si C1 C2 40.1(8) 2_556 . . . ?
N2 Si C1 C2 65.8(8) . . . . ?
N1 Si C1 C2 -118.9(8) . . . . ?
Si Si C1 C2 -17.7(8) 2_556 . . . ?
N1 C1 C2 C7 145.77(19) . . . . ?
N2 C1 C2 C7 -42.2(3) . . . . ?
Si C1 C2 C7 -101.2(8) . . . . ?
N1 C1 C2 C3 -36.5(3) . . . . ?
N2 C1 C2 C3 135.49(19) . . . . ?
Si C1 C2 C3 76.4(8) . . . . ?
C7 C2 C3 C4 -0.1(3) . . . . ?
C1 C2 C3 C4 -177.90(18) . . . . ?
C2 C3 C4 C5 -0.5(3) . . . . ?
C3 C4 C5 C6 0.3(3) . . . . ?
C4 C5 C6 C7 0.6(3) . . . . ?
C5 C6 C7 C2 -1.2(3) . . . . ?
C3 C2 C7 C6 1.0(3) . . . . ?
C1 C2 C7 C6 178.62(18) . . . . ?
C1 N1 C8 C13 -59.4(3) . . . . ?
Si N1 C8 C13 102.2(2) . . . . ?
C1 N1 C8 C9 125.6(2) . . . . ?
Si N1 C8 C9 -72.8(3) . . . . ?
C13 C8 C9 C10 -1.9(3) . . . . ?
N1 C8 C9 C10 173.10(17) . . . . ?
C13 C8 C9 C14 176.51(18) . . . . ?
N1 C8 C9 C14 -8.5(3) . . . . ?
C8 C9 C10 C11 0.7(3) . . . . ?
C14 C9 C10 C11 -177.8(2) . . . . ?
C9 C10 C11 C12 0.8(3) . . . . ?
C10 C11 C12 C13 -1.2(3) . . . . ?
C11 C12 C13 C8 0.0(3) . . . . ?
C11 C12 C13 C17 179.34(19) . . . . ?
C9 C8 C13 C12 1.6(3) . . . . ?
N1 C8 C13 C12 -173.34(17) . . . . ?
C9 C8 C13 C17 -177.75(18) . . . . ?
N1 C8 C13 C17 7.3(3) . . . . ?
C10 C9 C14 C15 -64.8(2) . . . . ?
C8 C9 C14 C15 116.8(2) . . . . ?
C10 C9 C14 C16 60.0(2) . . . . ?
C8 C9 C14 C16 -118.4(2) . . . . ?
C12 C13 C17 C19 -65.4(2) . . . . ?
C8 C13 C17 C19 113.9(2) . . . . ?
C12 C13 C17 C18 57.2(2) . . . . ?
C8 C13 C17 C18 -123.5(2) . . . . ?
C1 N2 C20 C25 -85.4(2) . . . . ?
Si N2 C20 C25 104.0(2) . . . . ?
C1 N2 C20 C21 94.1(2) . . . . ?
Si N2 C20 C21 -76.5(2) . . . . ?
C25 C20 C21 C22 0.0(3) . . . . ?
N2 C20 C21 C22 -179.48(16) . . . . ?
C25 C20 C21 C26 178.50(17) . . . . ?
N2 C20 C21 C26 -1.0(3) . . . . ?
C20 C21 C22 C23 -0.5(3) . . . . ?
C26 C21 C22 C23 -179.12(19) . . . . ?
C21 C22 C23 C24 0.6(3) . . . . ?
C22 C23 C24 C25 -0.2(4) . . . . ?
C21 C20 C25 C24 0.4(3) . . . . ?
N2 C20 C25 C24 179.89(18) . . . . ?
C21 C20 C25 C29 -178.09(18) . . . . ?
N2 C20 C25 C29 1.4(3) . . . . ?
C23 C24 C25 C20 -0.3(3) . . . . ?
C23 C24 C25 C29 178.3(2) . . . . ?
C22 C21 C26 C28 -54.2(2) . . . . ?
C20 C21 C26 C28 127.3(2) . . . . ?
C22 C21 C26 C27 68.3(2) . . . . ?
C20 C21 C26 C27 -110.2(2) . . . . ?
C20 C25 C29 C30 -116.6(2) . . . . ?
C24 C25 C29 C30 64.9(2) . . . . ?
C20 C25 C29 C31 119.4(2) . . . . ?
C24 C25 C29 C31 -59.1(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.08
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.037
####################################################################### 
# 
# 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_kob41b
_database_code_depnum_ccdc_archive 'CCDC 1061427'
_audit_update_record             
;
2015-04-23 deposited with the CCDC.
2015-06-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C66 H90 N6 S2 Si2, C7 H8'
_chemical_formula_sum            'C73 H98 N6 S2 Si2'
_chemical_formula_weight         1179.87

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.4605(17)
_cell_length_b                   13.003(2)
_cell_length_c                   13.411(2)
_cell_angle_alpha                111.238(10)
_cell_angle_beta                 91.783(7)
_cell_angle_gamma                96.105(17)
_cell_volume                     1685.9(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6119
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      28.18

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.29
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             638
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9199
_exptl_absorpt_correction_T_max  0.9544
_exptl_absorpt_process_details   'Sadabs 2008/1 (Bruker 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26026
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.63
_diffrn_reflns_theta_max         28.36
_reflns_number_total             8368
_reflns_number_gt                6444
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP & POV-Ray'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0611P)²+0.4343P] 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         8368
_refine_ls_number_parameters     405
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0431
_refine_ls_wR_factor_ref         0.1263
_refine_ls_wR_factor_gt          0.1074
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S S 0.05242(4) 0.38166(3) 0.46693(3) 0.01145(10) Uani 1 1 d . . .
Si Si -0.11694(4) 0.44551(4) 0.43622(4) 0.00940(11) Uani 1 1 d . . .
N1 N -0.15294(13) 0.44208(11) 0.30413(11) 0.0100(3) Uani 1 1 d . . .
N2 N -0.17990(13) 0.25945(11) 0.27594(11) 0.0107(3) Uani 1 1 d . . .
N3 N -0.24604(13) 0.40032(12) 0.48995(11) 0.0125(3) Uani 1 1 d . . .
C1 C -0.18968(15) 0.33252(14) 0.23301(13) 0.0108(3) Uani 1 1 d . . .
C2 C -0.23884(16) 0.31016(14) 0.12070(13) 0.0126(3) Uani 1 1 d . . .
C3 C -0.32164(18) 0.37773(15) 0.09905(14) 0.0179(4) Uani 1 1 d . . .
H3 H -0.3433 0.4407 0.1560 0.021 Uiso 1 1 calc R . .
C4 C -0.37311(19) 0.35432(16) -0.00469(15) 0.0229(4) Uani 1 1 d . . .
H4 H -0.4294 0.4013 -0.0182 0.027 Uiso 1 1 calc R . .
C5 C -0.34256(19) 0.26267(16) -0.08848(14) 0.0204(4) Uani 1 1 d . . .
H5 H -0.3777 0.2465 -0.1595 0.025 Uiso 1 1 calc R . .
C6 C -0.25995(18) 0.19443(15) -0.06788(14) 0.0179(4) Uani 1 1 d . . .
H6 H -0.2386 0.1316 -0.1251 0.021 Uiso 1 1 calc R . .
C7 C -0.20850(16) 0.21758(14) 0.03573(13) 0.0144(3) Uani 1 1 d . . .
H7 H -0.1524 0.1703 0.0490 0.017 Uiso 1 1 calc R . .
C8 C -0.10336(16) 0.53045(13) 0.26747(13) 0.0109(3) Uani 1 1 d . . .
C9 C 0.01427(17) 0.52449(14) 0.21810(13) 0.0140(3) Uani 1 1 d . . .
C10 C 0.06687(18) 0.61686(16) 0.19640(15) 0.0203(4) Uani 1 1 d . . .
H10 H 0.1458 0.6143 0.1629 0.024 Uiso 1 1 calc R . .
C11 C 0.0066(2) 0.71218(16) 0.22254(16) 0.0234(4) Uani 1 1 d . . .
H11 H 0.0464 0.7755 0.2106 0.028 Uiso 1 1 calc R . .
C12 C -0.11174(19) 0.71467(15) 0.26618(15) 0.0194(4) Uani 1 1 d . . .
H12 H -0.1541 0.7792 0.2816 0.023 Uiso 1 1 calc R . .
C13 C -0.17002(17) 0.62404(14) 0.28792(13) 0.0139(3) Uani 1 1 d . . .
C14 C 0.08549(17) 0.42208(15) 0.18352(14) 0.0156(4) Uani 1 1 d . . .
H14 H 0.0364 0.3639 0.2048 0.019 Uiso 1 1 calc R . .
C15 C 0.09089(19) 0.37512(17) 0.06092(15) 0.0227(4) Uani 1 1 d . . .
H15A H 0.0034 0.3611 0.0266 0.034 Uiso 1 1 calc R . .
H15B H 0.1291 0.3054 0.0392 0.034 Uiso 1 1 calc R . .
H15C H 0.1436 0.4290 0.0388 0.034 Uiso 1 1 calc R . .
C16 C 0.22213(18) 0.44744(17) 0.23795(16) 0.0230(4) Uani 1 1 d . . .
H16A H 0.2616 0.3784 0.2190 0.035 Uiso 1 1 calc R . .
H16B H 0.2183 0.4801 0.3159 0.035 Uiso 1 1 calc R . .
H16C H 0.2739 0.5001 0.2137 0.035 Uiso 1 1 calc R . .
C17 C -0.30550(17) 0.62983(14) 0.32703(14) 0.0146(3) Uani 1 1 d . . .
H17 H -0.3374 0.5564 0.3313 0.018 Uiso 1 1 calc R . .
C18 C -0.39882(19) 0.65206(16) 0.24772(15) 0.0219(4) Uani 1 1 d . . .
H18A H -0.3910 0.5998 0.1748 0.033 Uiso 1 1 calc R . .
H18B H -0.3771 0.7284 0.2508 0.033 Uiso 1 1 calc R . .
H18C H -0.4875 0.6421 0.2673 0.033 Uiso 1 1 calc R . .
C19 C -0.31012(18) 0.72050(15) 0.43834(14) 0.0192(4) Uani 1 1 d . . .
H19A H -0.2756 0.7929 0.4367 0.029 Uiso 1 1 calc R . .
H19B H -0.2581 0.7040 0.4914 0.029 Uiso 1 1 calc R . .
H19C H -0.3996 0.7224 0.4579 0.029 Uiso 1 1 calc R . .
C20 C -0.22695(16) 0.14451(14) 0.22648(13) 0.0118(3) Uani 1 1 d . . .
C21 C -0.35988(16) 0.10524(14) 0.20226(13) 0.0135(3) Uani 1 1 d . . .
C22 C -0.39632(18) -0.00967(15) 0.15878(14) 0.0177(4) Uani 1 1 d . . .
H22 H -0.4853 -0.0372 0.1420 0.021 Uiso 1 1 calc R . .
C23 C -0.30735(19) -0.08456(15) 0.13938(15) 0.0211(4) Uani 1 1 d . . .
H23 H -0.3347 -0.1623 0.1087 0.025 Uiso 1 1 calc R . .
C24 C -0.17697(19) -0.04464(15) 0.16545(15) 0.0194(4) Uani 1 1 d . . .
H24 H -0.1155 -0.0959 0.1525 0.023 Uiso 1 1 calc R . .
C25 C -0.13494(17) 0.06902(14) 0.21016(14) 0.0146(3) Uani 1 1 d . . .
C26 C -0.46453(16) 0.18136(15) 0.22067(14) 0.0158(4) Uani 1 1 d . . .
H26 H -0.4223 0.2601 0.2522 0.019 Uiso 1 1 calc R . .
C27 C -0.53909(18) 0.16502(16) 0.11431(15) 0.0198(4) Uani 1 1 d . . .
H27A H -0.4782 0.1733 0.0629 0.030 Uiso 1 1 calc R . .
H27B H -0.5988 0.2209 0.1269 0.030 Uiso 1 1 calc R . .
H27C H -0.5878 0.0904 0.0854 0.030 Uiso 1 1 calc R . .
C28 C -0.55945(18) 0.16267(17) 0.29896(15) 0.0215(4) Uani 1 1 d . . .
H28A H -0.6065 0.0876 0.2673 0.032 Uiso 1 1 calc R . .
H28B H -0.6207 0.2175 0.3136 0.032 Uiso 1 1 calc R . .
H28C H -0.5119 0.1710 0.3661 0.032 Uiso 1 1 calc R . .
C29 C 0.00809(17) 0.11010(15) 0.23999(15) 0.0175(4) Uani 1 1 d . . .
H29 H 0.0178 0.1932 0.2717 0.021 Uiso 1 1 calc R . .
C30 C 0.0863(2) 0.0764(2) 0.14090(17) 0.0318(5) Uani 1 1 d . . .
H30A H 0.0759 -0.0048 0.1063 0.048 Uiso 1 1 calc R . .
H30B H 0.1776 0.1040 0.1627 0.048 Uiso 1 1 calc R . .
H30C H 0.0555 0.1086 0.0903 0.048 Uiso 1 1 calc R . .
C31 C 0.0603(2) 0.06957(18) 0.32489(18) 0.0289(5) Uani 1 1 d . . .
H31A H 0.0532 -0.0118 0.2956 0.043 Uiso 1 1 calc R . .
H31B H 0.0102 0.0939 0.3880 0.043 Uiso 1 1 calc R . .
H31C H 0.1510 0.1006 0.3455 0.043 Uiso 1 1 calc R . .
C32 C -0.25808(18) 0.29600(15) 0.50812(15) 0.0173(4) Uani 1 1 d . . .
H32A H -0.3128 0.2388 0.4493 0.026 Uiso 1 1 calc R . .
H32B H -0.2970 0.3064 0.5761 0.026 Uiso 1 1 calc R . .
H32C H -0.1725 0.2726 0.5112 0.026 Uiso 1 1 calc R . .
C33 C -0.36607(17) 0.44763(15) 0.49427(15) 0.0167(4) Uani 1 1 d . . .
H33A H -0.3485 0.5235 0.4951 0.025 Uiso 1 1 calc R . .
H33B H -0.4071 0.4493 0.5595 0.025 Uiso 1 1 calc R . .
H33C H -0.4238 0.4021 0.4312 0.025 Uiso 1 1 calc R . .
C34 C -0.6707(7) 0.9608(7) 0.4670(7) 0.062(2) Uani 0.50 1 d PU A -1
H34A H -0.6872 0.8856 0.4123 0.092 Uiso 0.50 1 calc PR A -1
H34B H -0.7069 1.0131 0.4401 0.092 Uiso 0.50 1 calc PR A -1
H34C H -0.7111 0.9621 0.5323 0.092 Uiso 0.50 1 calc PR A -1
C38 C -0.2631(3) 1.0516(3) 0.5278(3) 0.0480(16) Uani 0.50 1 d PG A -1
H38 H -0.1723 1.0715 0.5401 0.058 Uiso 0.50 1 calc PR A -1
C37 C -0.3185(3) 0.9959(3) 0.4238(2) 0.0413(13) Uani 0.50 1 d PG A -1
H37 H -0.2655 0.9777 0.3651 0.050 Uiso 0.50 1 calc PR A -1
C36 C -0.4512(3) 0.9669(3) 0.4058(2) 0.0318(11) Uani 0.50 1 d PG A -1
H36 H -0.4891 0.9288 0.3348 0.038 Uiso 0.50 1 calc PR A -1
C35 C -0.5287(2) 0.9935(4) 0.4917(3) 0.0498(15) Uani 0.50 1 d PGU A -1
C40 C -0.4734(4) 1.0492(4) 0.5956(3) 0.0493(15) Uani 0.50 1 d PGU A -1
H40 H -0.5263 1.0674 0.6544 0.059 Uiso 0.50 1 calc PR A -1
C39 C -0.3406(4) 1.0783(3) 0.6137(2) 0.0487(13) Uani 0.50 1 d PGU A -1
H39 H -0.3027 1.1163 0.6847 0.058 Uiso 0.50 1 calc PR A -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S Si 2.1243(7) . ?
S Si 2.1683(7) 2_566 ?
Si N3 1.6990(15) . ?
Si N1 1.7831(14) . ?
Si S 2.1683(7) 2_566 ?
N1 C1 1.401(2) . ?
N1 C8 1.459(2) . ?
N2 C1 1.288(2) . ?
N2 C20 1.422(2) . ?
N3 C33 1.450(2) . ?
N3 C32 1.456(2) . ?
C1 C2 1.490(2) . ?
C2 C3 1.392(2) . ?
C2 C7 1.399(2) . ?
C3 C4 1.389(2) . ?
C4 C5 1.385(3) . ?
C5 C6 1.391(3) . ?
C6 C7 1.388(2) . ?
C8 C9 1.412(2) . ?
C8 C13 1.412(2) . ?
C9 C10 1.397(2) . ?
C9 C14 1.526(2) . ?
C10 C11 1.386(3) . ?
C11 C12 1.384(3) . ?
C12 C13 1.397(2) . ?
C13 C17 1.526(2) . ?
C14 C16 1.531(3) . ?
C14 C15 1.538(2) . ?
C17 C19 1.537(2) . ?
C17 C18 1.545(2) . ?
C20 C25 1.413(2) . ?
C20 C21 1.414(2) . ?
C21 C22 1.397(2) . ?
C21 C26 1.520(2) . ?
C22 C23 1.381(3) . ?
C23 C24 1.393(3) . ?
C24 C25 1.393(2) . ?
C25 C29 1.524(2) . ?
C26 C28 1.532(2) . ?
C26 C27 1.537(2) . ?
C29 C31 1.526(3) . ?
C29 C30 1.533(3) . ?
C34 C35 1.493(7) . ?
C38 C37 1.3900 . ?
C38 C39 1.3900 . ?
C37 C36 1.3900 . ?
C36 C35 1.3900 . ?
C35 C40 1.3900 . ?
C40 C39 1.3900 . ?

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
Si S Si 83.46(3) . 2_566 ?
N3 Si N1 113.39(7) . . ?
N3 Si S 111.70(5) . . ?
N1 Si S 118.51(5) . . ?
N3 Si S 109.04(6) . 2_566 ?
N1 Si S 105.70(5) . 2_566 ?
S Si S 96.54(3) . 2_566 ?
C1 N1 C8 122.18(13) . . ?
C1 N1 Si 110.55(11) . . ?
C8 N1 Si 123.21(11) . . ?
C1 N2 C20 124.96(14) . . ?
C33 N3 C32 113.78(14) . . ?
C33 N3 Si 120.99(11) . . ?
C32 N3 Si 123.32(12) . . ?
N2 C1 N1 113.54(14) . . ?
N2 C1 C2 126.31(15) . . ?
N1 C1 C2 120.12(14) . . ?
C3 C2 C7 118.66(16) . . ?
C3 C2 C1 120.48(15) . . ?
C7 C2 C1 120.77(15) . . ?
C4 C3 C2 120.92(17) . . ?
C5 C4 C3 120.16(17) . . ?
C4 C5 C6 119.48(17) . . ?
C7 C6 C5 120.47(17) . . ?
C6 C7 C2 120.31(16) . . ?
C9 C8 C13 120.92(15) . . ?
C9 C8 N1 119.68(15) . . ?
C13 C8 N1 119.28(14) . . ?
C10 C9 C8 118.01(16) . . ?
C10 C9 C14 117.84(16) . . ?
C8 C9 C14 124.11(15) . . ?
C11 C10 C9 121.59(17) . . ?
C12 C11 C10 119.64(17) . . ?
C11 C12 C13 121.23(17) . . ?
C12 C13 C8 118.38(16) . . ?
C12 C13 C17 117.79(15) . . ?
C8 C13 C17 123.76(15) . . ?
C9 C14 C16 111.98(15) . . ?
C9 C14 C15 110.38(15) . . ?
C16 C14 C15 109.86(15) . . ?
C13 C17 C19 113.09(15) . . ?
C13 C17 C18 110.92(15) . . ?
C19 C17 C18 108.01(14) . . ?
C25 C20 C21 120.51(15) . . ?
C25 C20 N2 116.70(15) . . ?
C21 C20 N2 122.59(15) . . ?
C22 C21 C20 118.01(16) . . ?
C22 C21 C26 118.52(16) . . ?
C20 C21 C26 123.47(15) . . ?
C23 C22 C21 122.19(17) . . ?
C22 C23 C24 119.12(17) . . ?
C23 C24 C25 121.29(17) . . ?
C24 C25 C20 118.82(16) . . ?
C24 C25 C29 120.07(16) . . ?
C20 C25 C29 121.11(15) . . ?
C21 C26 C28 111.96(15) . . ?
C21 C26 C27 110.97(14) . . ?
C28 C26 C27 109.28(14) . . ?
C25 C29 C31 111.17(16) . . ?
C25 C29 C30 111.46(15) . . ?
C31 C29 C30 111.14(16) . . ?
C37 C38 C39 120.0 . . ?
C38 C37 C36 120.0 . . ?
C37 C36 C35 120.0 . . ?
C40 C35 C36 120.0 . . ?
C40 C35 C34 122.6(4) . . ?
C36 C35 C34 117.4(4) . . ?
C39 C40 C35 120.0 . . ?
C40 C39 C38 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Si S Si N3 -113.52(6) 2_566 . . . ?
Si S Si N1 111.86(6) 2_566 . . . ?
Si S Si S 0.0 2_566 . . 2_566 ?
N3 Si N1 C1 -63.61(12) . . . . ?
S Si N1 C1 70.30(11) . . . . ?
S Si N1 C1 177.00(9) 2_566 . . . ?
N3 Si N1 C8 138.69(12) . . . . ?
S Si N1 C8 -87.41(13) . . . . ?
S Si N1 C8 19.29(13) 2_566 . . . ?
N1 Si N3 C33 -53.24(15) . . . . ?
S Si N3 C33 169.71(11) . . . . ?
S Si N3 C33 64.23(14) 2_566 . . . ?
N1 Si N3 C32 110.06(14) . . . . ?
S Si N3 C32 -26.99(15) . . . . ?
S Si N3 C32 -132.47(13) 2_566 . . . ?
C20 N2 C1 N1 171.01(14) . . . . ?
C20 N2 C1 C2 -6.8(3) . . . . ?
C8 N1 C1 N2 152.98(15) . . . . ?
Si N1 C1 N2 -5.00(17) . . . . ?
C8 N1 C1 C2 -29.1(2) . . . . ?
Si N1 C1 C2 172.96(12) . . . . ?
N2 C1 C2 C3 137.38(18) . . . . ?
N1 C1 C2 C3 -40.3(2) . . . . ?
N2 C1 C2 C7 -39.1(3) . . . . ?
N1 C1 C2 C7 143.22(16) . . . . ?
C7 C2 C3 C4 -0.2(3) . . . . ?
C1 C2 C3 C4 -176.75(17) . . . . ?
C2 C3 C4 C5 0.1(3) . . . . ?
C3 C4 C5 C6 -0.1(3) . . . . ?
C4 C5 C6 C7 0.1(3) . . . . ?
C5 C6 C7 C2 -0.2(3) . . . . ?
C3 C2 C7 C6 0.3(3) . . . . ?
C1 C2 C7 C6 176.80(16) . . . . ?
C1 N1 C8 C9 -64.2(2) . . . . ?
Si N1 C8 C9 91.03(17) . . . . ?
C1 N1 C8 C13 119.69(17) . . . . ?
Si N1 C8 C13 -85.12(17) . . . . ?
C13 C8 C9 C10 4.0(2) . . . . ?
N1 C8 C9 C10 -172.05(15) . . . . ?
C13 C8 C9 C14 -173.85(16) . . . . ?
N1 C8 C9 C14 10.1(2) . . . . ?
C8 C9 C10 C11 0.3(3) . . . . ?
C14 C9 C10 C11 178.28(17) . . . . ?
C9 C10 C11 C12 -3.4(3) . . . . ?
C10 C11 C12 C13 2.2(3) . . . . ?
C11 C12 C13 C8 2.0(3) . . . . ?
C11 C12 C13 C17 -174.90(17) . . . . ?
C9 C8 C13 C12 -5.1(2) . . . . ?
N1 C8 C13 C12 170.96(15) . . . . ?
C9 C8 C13 C17 171.54(15) . . . . ?
N1 C8 C13 C17 -12.4(2) . . . . ?
C10 C9 C14 C16 60.7(2) . . . . ?
C8 C9 C14 C16 -121.45(18) . . . . ?
C10 C9 C14 C15 -62.1(2) . . . . ?
C8 C9 C14 C15 115.80(18) . . . . ?
C12 C13 C17 C19 -66.2(2) . . . . ?
C8 C13 C17 C19 117.11(18) . . . . ?
C12 C13 C17 C18 55.3(2) . . . . ?
C8 C13 C17 C18 -121.36(18) . . . . ?
C1 N2 C20 C25 119.58(18) . . . . ?
C1 N2 C20 C21 -65.6(2) . . . . ?
C25 C20 C21 C22 -2.0(2) . . . . ?
N2 C20 C21 C22 -176.70(15) . . . . ?
C25 C20 C21 C26 178.19(15) . . . . ?
N2 C20 C21 C26 3.5(3) . . . . ?
C20 C21 C22 C23 0.1(3) . . . . ?
C26 C21 C22 C23 179.90(17) . . . . ?
C21 C22 C23 C24 1.0(3) . . . . ?
C22 C23 C24 C25 -0.3(3) . . . . ?
C23 C24 C25 C20 -1.6(3) . . . . ?
C23 C24 C25 C29 178.72(17) . . . . ?
C21 C20 C25 C24 2.8(3) . . . . ?
N2 C20 C25 C24 177.76(15) . . . . ?
C21 C20 C25 C29 -177.57(16) . . . . ?
N2 C20 C25 C29 -2.6(2) . . . . ?
C22 C21 C26 C28 60.6(2) . . . . ?
C20 C21 C26 C28 -119.60(18) . . . . ?
C22 C21 C26 C27 -61.8(2) . . . . ?
C20 C21 C26 C27 117.99(18) . . . . ?
C24 C25 C29 C31 -61.3(2) . . . . ?
C20 C25 C29 C31 119.01(19) . . . . ?
C24 C25 C29 C30 63.3(2) . . . . ?
C20 C25 C29 C30 -116.39(19) . . . . ?
C39 C38 C37 C36 0.0 . . . . ?
C38 C37 C36 C35 0.0 . . . . ?
C37 C36 C35 C40 0.0 . . . . ?
C37 C36 C35 C34 179.6(6) . . . . ?
C36 C35 C40 C39 0.0 . . . . ?
C34 C35 C40 C39 -179.6(6) . . . . ?
C35 C40 C39 C38 0.0 . . . . ?
C37 C38 C39 C40 0.0 . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.076
####################################################################### 
# 
# 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_KOB45C_multiscan
_database_code_depnum_ccdc_archive 'CCDC 1061428'
_audit_update_record             
;
2015-04-23 deposited with the CCDC.
2015-06-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H45 N3 Se Si'
_chemical_formula_sum            'C33 H45 N3 Se Si'
_chemical_formula_weight         590.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   20.372(4)
_cell_length_b                   9.872(2)
_cell_length_c                   17.527(4)
_cell_angle_alpha                90
_cell_angle_beta                 113.44(3)
_cell_angle_gamma                90
_cell_volume                     3234.2(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5000
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      29.0

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_F_000             1248
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    1.223
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min  0.7504
_exptl_absorpt_correction_T_max  0.7752

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  image_plate-Stoe-IPDS
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34256
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_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         2.333
_diffrn_reflns_theta_max         26.019
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6362
_reflns_number_gt                4208
_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       'STOE IPDS'
_computing_cell_refinement       'STOE IPDS'
_computing_data_reduction        'STOE IPDS'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP & POV-Ray'
_computing_publication_material  'Bruker SHELXTL'


_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)+(0.0746P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6362
_refine_ls_number_parameters     353
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0462
_refine_ls_wR_factor_ref         0.1182
_refine_ls_wR_factor_gt          0.1102
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_restrained_S_all      0.910
_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
Se Se 0.18761(2) 0.84293(4) 0.47384(2) 0.04373(13) Uani 1 1 d . . . . .
Si Si 0.19993(4) 1.04949(9) 0.51082(4) 0.0276(2) Uani 1 1 d . . . . .
N1 N 0.19028(11) 1.0887(3) 0.60928(13) 0.0248(5) Uani 1 1 d . . . . .
N2 N 0.28744(11) 1.1142(2) 0.58894(12) 0.0225(5) Uani 1 1 d . . . . .
N3 N 0.16341(13) 1.1674(3) 0.43653(14) 0.0375(7) Uani 1 1 d . . . . .
C1 C 0.25990(13) 1.1224(3) 0.64724(15) 0.0224(6) Uani 1 1 d . . . . .
C2 C 0.29799(14) 1.1613(3) 0.73511(15) 0.0257(6) Uani 1 1 d . . . . .
C3 C 0.26382(16) 1.2437(4) 0.77218(17) 0.0378(8) Uani 1 1 d . . . . .
H3 H 0.2160 1.2725 0.7413 0.045 Uiso 1 1 calc R U . . .
C4 C 0.29958(18) 1.2844(4) 0.85471(19) 0.0485(10) Uani 1 1 d . . . . .
H4 H 0.2768 1.3424 0.8799 0.058 Uiso 1 1 calc R U . . .
C5 C 0.36897(17) 1.2391(4) 0.89959(18) 0.0490(10) Uani 1 1 d . . . . .
H5 H 0.3934 1.2654 0.9560 0.059 Uiso 1 1 calc R U . . .
C6 C 0.40267(16) 1.1566(4) 0.86320(17) 0.0407(8) Uani 1 1 d . . . . .
H6 H 0.4500 1.1263 0.8949 0.049 Uiso 1 1 calc R U . . .
C7 C 0.36825(15) 1.1170(3) 0.78044(16) 0.0325(7) Uani 1 1 d . . . . .
H7 H 0.3919 1.0610 0.7552 0.039 Uiso 1 1 calc R U . . .
C8 C 0.14458(13) 1.0535(3) 0.65179(15) 0.0245(6) Uani 1 1 d . . . . .
C9 C 0.16085(15) 0.9423(3) 0.70635(17) 0.0302(7) Uani 1 1 d . . . . .
C10 C 0.11734(16) 0.9202(4) 0.75042(18) 0.0392(8) Uani 1 1 d . . . . .
H10 H 0.1286 0.8480 0.7894 0.047 Uiso 1 1 calc R U . . .
C11 C 0.05903(17) 1.0003(4) 0.73842(19) 0.0415(8) Uani 1 1 d . . . . .
H11 H 0.0309 0.9840 0.7696 0.050 Uiso 1 1 calc R U . . .
C12 C 0.04084(15) 1.1054(4) 0.68087(19) 0.0369(8) Uani 1 1 d . . . . .
H12 H -0.0009 1.1577 0.6711 0.044 Uiso 1 1 calc R U . . .
C13 C 0.08373(14) 1.1346(3) 0.63710(16) 0.0288(7) Uani 1 1 d . . . . .
C14 C 0.22025(16) 0.8418(4) 0.7170(2) 0.0408(8) Uani 1 1 d . . . . .
H14 H 0.2469 0.8739 0.6833 0.049 Uiso 1 1 calc R U . . .
C15 C 0.27354(18) 0.8295(5) 0.8082(2) 0.0616(12) Uani 1 1 d . . . . .
H15A H 0.3133 0.7705 0.8115 0.092 Uiso 1 1 calc R U . . .
H15B H 0.2493 0.7906 0.8414 0.092 Uiso 1 1 calc R U . . .
H15C H 0.2920 0.9194 0.8297 0.092 Uiso 1 1 calc R U . . .
C16 C 0.1877(2) 0.7030(4) 0.6839(3) 0.0613(11) Uani 1 1 d . . . . .
H16A H 0.1541 0.7117 0.6257 0.092 Uiso 1 1 calc R U . . .
H16B H 0.1623 0.6688 0.7171 0.092 Uiso 1 1 calc R U . . .
H16C H 0.2259 0.6396 0.6876 0.092 Uiso 1 1 calc R U . . .
C17 C 0.06361(15) 1.2494(3) 0.57492(17) 0.0338(7) Uani 1 1 d . . . . .
H17 H 0.1078 1.2781 0.5675 0.041 Uiso 1 1 calc R U . . .
C18 C 0.0345(3) 1.3728(4) 0.6040(2) 0.0689(13) Uani 1 1 d . . . . .
H18A H 0.0331 1.4507 0.5688 0.103 Uiso 1 1 calc R U . . .
H18B H 0.0656 1.3933 0.6619 0.103 Uiso 1 1 calc R U . . .
H18C H -0.0140 1.3533 0.5999 0.103 Uiso 1 1 calc R U . . .
C19 C 0.00918(18) 1.2007(4) 0.49042(19) 0.0473(9) Uani 1 1 d . . . . .
H19A H -0.0012 1.2743 0.4498 0.071 Uiso 1 1 calc R U . . .
H19B H -0.0350 1.1733 0.4958 0.071 Uiso 1 1 calc R U . . .
H19C H 0.0290 1.1232 0.4716 0.071 Uiso 1 1 calc R U . . .
C20 C 0.35863(13) 1.1556(3) 0.59933(14) 0.0214(5) Uani 1 1 d . . . . .
C21 C 0.38049(14) 1.2915(3) 0.61625(15) 0.0235(6) Uani 1 1 d . . . . .
C22 C 0.45059(15) 1.3237(3) 0.62650(17) 0.0307(7) Uani 1 1 d . . . . .
H22 H 0.4663 1.4149 0.6377 0.037 Uiso 1 1 calc R U . . .
C23 C 0.49744(14) 1.2271(3) 0.62082(16) 0.0309(7) Uani 1 1 d . . . . .
H23 H 0.5447 1.2516 0.6285 0.037 Uiso 1 1 calc R U . . .
C24 C 0.47497(14) 1.0954(3) 0.60401(16) 0.0279(6) Uani 1 1 d . . . . .
H24 H 0.5072 1.0294 0.5995 0.034 Uiso 1 1 calc R U . . .
C25 C 0.40581(13) 1.0553(3) 0.59329(15) 0.0220(6) Uani 1 1 d . . . . .
C26 C 0.33393(16) 1.4065(3) 0.62328(18) 0.0329(7) Uani 1 1 d . . . . .
H26 H 0.2870 1.3673 0.6180 0.040 Uiso 1 1 calc R U . . .
C27 C 0.36781(18) 1.4767(4) 0.7084(2) 0.0419(8) Uani 1 1 d . . . . .
H27A H 0.4134 1.5181 0.7145 0.063 Uiso 1 1 calc R U . . .
H27B H 0.3763 1.4098 0.7527 0.063 Uiso 1 1 calc R U . . .
H27C H 0.3354 1.5471 0.7124 0.063 Uiso 1 1 calc R U . . .
C28 C 0.31946(19) 1.5072(4) 0.5522(2) 0.0460(9) Uani 1 1 d . . . . .
H28A H 0.2971 1.4599 0.4989 0.069 Uiso 1 1 calc R U . . .
H28B H 0.3647 1.5478 0.5564 0.069 Uiso 1 1 calc R U . . .
H28C H 0.2873 1.5785 0.5557 0.069 Uiso 1 1 calc R U . . .
C29 C 0.38612(15) 0.9076(3) 0.57879(16) 0.0283(6) Uani 1 1 d . . . . .
H29 H 0.3346 0.8985 0.5694 0.034 Uiso 1 1 calc R U . . .
C30 C 0.4303(2) 0.8245(4) 0.6559(2) 0.0497(10) Uani 1 1 d . . . . .
H30A H 0.4163 0.7290 0.6461 0.075 Uiso 1 1 calc R U . . .
H30B H 0.4217 0.8578 0.7038 0.075 Uiso 1 1 calc R U . . .
H30C H 0.4812 0.8334 0.6672 0.075 Uiso 1 1 calc R U . . .
C31 C 0.3948(2) 0.8538(4) 0.5020(2) 0.0478(9) Uani 1 1 d . . . . .
H31A H 0.3700 0.9140 0.4547 0.072 Uiso 1 1 calc R U . . .
H31B H 0.3743 0.7627 0.4892 0.072 Uiso 1 1 calc R U . . .
H31C H 0.4458 0.8502 0.5125 0.072 Uiso 1 1 calc R U . . .
C32 C 0.16475(18) 1.3099(4) 0.4489(2) 0.0477(10) Uani 1 1 d . . . . .
H32A H 0.1856 1.3543 0.4137 0.072 Uiso 1 1 calc R U . . .
H32B H 0.1938 1.3307 0.5074 0.072 Uiso 1 1 calc R U . . .
H32C H 0.1159 1.3430 0.4341 0.072 Uiso 1 1 calc R U . . .
C33 C 0.11857(18) 1.1327(5) 0.34992(19) 0.0548(11) Uani 1 1 d . . . . .
H33A H 0.1375 1.1773 0.3129 0.082 Uiso 1 1 calc R U . . .
H33B H 0.0695 1.1634 0.3364 0.082 Uiso 1 1 calc R U . . .
H33C H 0.1189 1.0344 0.3426 0.082 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Se Si 2.1241(10) . ?
Si N3 1.683(3) . ?
Si N1 1.854(2) . ?
Si N2 1.876(2) . ?
Si C1 2.324(3) . ?
N1 C1 1.347(3) . ?
N1 C8 1.447(3) . ?
N2 C1 1.349(3) . ?
N2 C20 1.447(3) . ?
N3 C32 1.422(5) . ?
N3 C33 1.467(4) . ?
C1 C2 1.474(3) . ?
C2 C3 1.389(4) . ?
C2 C7 1.403(4) . ?
C3 C4 1.395(4) . ?
C4 C5 1.390(5) . ?
C5 C6 1.375(5) . ?
C6 C7 1.393(4) . ?
C8 C9 1.406(4) . ?
C8 C13 1.411(4) . ?
C9 C10 1.405(4) . ?
C9 C14 1.518(4) . ?
C10 C11 1.372(5) . ?
C11 C12 1.390(5) . ?
C12 C13 1.403(4) . ?
C13 C17 1.511(4) . ?
C14 C16 1.532(6) . ?
C14 C15 1.538(4) . ?
C17 C18 1.528(5) . ?
C17 C19 1.532(4) . ?
C20 C21 1.408(4) . ?
C20 C25 1.413(4) . ?
C21 C22 1.403(4) . ?
C21 C26 1.515(4) . ?
C22 C23 1.380(4) . ?
C23 C24 1.371(4) . ?
C24 C25 1.402(4) . ?
C25 C29 1.506(4) . ?
C26 C28 1.529(4) . ?
C26 C27 1.538(4) . ?
C29 C31 1.522(4) . ?
C29 C30 1.531(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
N3 Si N1 113.44(13) . . ?
N3 Si N2 109.16(13) . . ?
N1 Si N2 70.81(10) . . ?
N3 Si Se 117.75(10) . . ?
N1 Si Se 116.17(9) . . ?
N2 Si Se 120.83(8) . . ?
N3 Si C1 118.12(13) . . ?
N1 Si C1 35.40(9) . . ?
N2 Si C1 35.49(9) . . ?
Se Si C1 124.12(8) . . ?
C1 N1 C8 124.9(2) . . ?
C1 N1 Si 91.75(17) . . ?
C8 N1 Si 139.23(18) . . ?
C1 N2 C20 125.9(2) . . ?
C1 N2 Si 90.71(16) . . ?
C20 N2 Si 143.32(17) . . ?
C32 N3 C33 110.8(3) . . ?
C32 N3 Si 126.2(2) . . ?
C33 N3 Si 122.7(3) . . ?
N1 C1 N2 106.5(2) . . ?
N1 C1 C2 126.4(2) . . ?
N2 C1 C2 127.0(2) . . ?
N1 C1 Si 52.86(13) . . ?
N2 C1 Si 53.81(12) . . ?
C2 C1 Si 177.1(2) . . ?
C3 C2 C7 120.4(2) . . ?
C3 C2 C1 119.2(2) . . ?
C7 C2 C1 120.3(3) . . ?
C2 C3 C4 120.1(3) . . ?
C5 C4 C3 119.2(3) . . ?
C6 C5 C4 120.7(3) . . ?
C5 C6 C7 120.8(3) . . ?
C6 C7 C2 118.7(3) . . ?
C9 C8 C13 121.3(3) . . ?
C9 C8 N1 120.8(2) . . ?
C13 C8 N1 117.9(2) . . ?
C10 C9 C8 117.7(3) . . ?
C10 C9 C14 118.5(3) . . ?
C8 C9 C14 123.7(3) . . ?
C11 C10 C9 121.5(3) . . ?
C10 C11 C12 120.4(3) . . ?
C11 C12 C13 120.4(3) . . ?
C12 C13 C8 118.5(3) . . ?
C12 C13 C17 120.0(3) . . ?
C8 C13 C17 121.6(3) . . ?
C9 C14 C16 109.5(3) . . ?
C9 C14 C15 112.2(3) . . ?
C16 C14 C15 110.1(3) . . ?
C13 C17 C18 112.8(3) . . ?
C13 C17 C19 110.2(3) . . ?
C18 C17 C19 110.2(3) . . ?
C21 C20 C25 121.1(2) . . ?
C21 C20 N2 120.8(2) . . ?
C25 C20 N2 118.1(2) . . ?
C22 C21 C20 117.6(3) . . ?
C22 C21 C26 117.3(3) . . ?
C20 C21 C26 125.1(2) . . ?
C23 C22 C21 122.1(3) . . ?
C24 C23 C22 119.3(3) . . ?
C23 C24 C25 121.9(3) . . ?
C24 C25 C20 118.0(3) . . ?
C24 C25 C29 118.8(3) . . ?
C20 C25 C29 123.2(2) . . ?
C21 C26 C28 110.2(3) . . ?
C21 C26 C27 111.3(2) . . ?
C28 C26 C27 111.4(3) . . ?
C25 C29 C31 111.7(3) . . ?
C25 C29 C30 110.3(2) . . ?
C31 C29 C30 111.1(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 Si N1 C1 -106.07(19) . . . . ?
N2 Si N1 C1 -2.90(17) . . . . ?
Se Si N1 C1 112.80(16) . . . . ?
N3 Si N1 C8 98.3(3) . . . . ?
N2 Si N1 C8 -158.6(3) . . . . ?
Se Si N1 C8 -42.9(3) . . . . ?
C1 Si N1 C8 -155.7(4) . . . . ?
N3 Si N2 C1 111.85(19) . . . . ?
N1 Si N2 C1 2.89(16) . . . . ?
Se Si N2 C1 -106.75(16) . . . . ?
N3 Si N2 C20 -63.9(4) . . . . ?
N1 Si N2 C20 -172.9(4) . . . . ?
Se Si N2 C20 77.5(3) . . . . ?
C1 Si N2 C20 -175.7(4) . . . . ?
N1 Si N3 C32 38.4(3) . . . . ?
N2 Si N3 C32 -38.4(3) . . . . ?
Se Si N3 C32 178.8(2) . . . . ?
C1 Si N3 C32 -0.8(3) . . . . ?
N1 Si N3 C33 -134.8(2) . . . . ?
N2 Si N3 C33 148.4(2) . . . . ?
Se Si N3 C33 5.7(3) . . . . ?
C1 Si N3 C33 -173.9(2) . . . . ?
C8 N1 C1 N2 164.8(3) . . . . ?
Si N1 C1 N2 4.0(2) . . . . ?
C8 N1 C1 C2 -15.6(5) . . . . ?
Si N1 C1 C2 -176.5(3) . . . . ?
C8 N1 C1 Si 160.9(3) . . . . ?
C20 N2 C1 N1 172.9(3) . . . . ?
Si N2 C1 N1 -3.9(2) . . . . ?
C20 N2 C1 C2 -6.6(5) . . . . ?
Si N2 C1 C2 176.5(3) . . . . ?
C20 N2 C1 Si 176.9(3) . . . . ?
N1 C1 C2 C3 -39.7(5) . . . . ?
N2 C1 C2 C3 139.7(3) . . . . ?
N1 C1 C2 C7 141.0(3) . . . . ?
N2 C1 C2 C7 -39.5(5) . . . . ?
C7 C2 C3 C4 0.8(5) . . . . ?
C1 C2 C3 C4 -178.5(3) . . . . ?
C2 C3 C4 C5 -1.4(6) . . . . ?
C3 C4 C5 C6 0.8(6) . . . . ?
C4 C5 C6 C7 0.3(6) . . . . ?
C5 C6 C7 C2 -0.9(5) . . . . ?
C3 C2 C7 C6 0.4(5) . . . . ?
C1 C2 C7 C6 179.6(3) . . . . ?
C1 N1 C8 C9 -60.0(4) . . . . ?
Si N1 C8 C9 89.9(3) . . . . ?
C1 N1 C8 C13 119.6(3) . . . . ?
Si N1 C8 C13 -90.5(4) . . . . ?
C13 C8 C9 C10 -4.4(4) . . . . ?
N1 C8 C9 C10 175.2(3) . . . . ?
C13 C8 C9 C14 172.6(3) . . . . ?
N1 C8 C9 C14 -7.8(4) . . . . ?
C8 C9 C10 C11 2.7(5) . . . . ?
C14 C9 C10 C11 -174.5(3) . . . . ?
C9 C10 C11 C12 0.9(5) . . . . ?
C10 C11 C12 C13 -2.9(5) . . . . ?
C11 C12 C13 C8 1.2(4) . . . . ?
C11 C12 C13 C17 -179.8(3) . . . . ?
C9 C8 C13 C12 2.5(4) . . . . ?
N1 C8 C13 C12 -177.1(2) . . . . ?
C9 C8 C13 C17 -176.5(3) . . . . ?
N1 C8 C13 C17 3.9(4) . . . . ?
C10 C9 C14 C16 64.1(4) . . . . ?
C8 C9 C14 C16 -112.9(3) . . . . ?
C10 C9 C14 C15 -58.5(4) . . . . ?
C8 C9 C14 C15 124.5(3) . . . . ?
C12 C13 C17 C18 39.1(4) . . . . ?
C8 C13 C17 C18 -141.9(3) . . . . ?
C12 C13 C17 C19 -84.5(3) . . . . ?
C8 C13 C17 C19 94.5(3) . . . . ?
C1 N2 C20 C21 -62.2(4) . . . . ?
Si N2 C20 C21 112.5(3) . . . . ?
C1 N2 C20 C25 116.8(3) . . . . ?
Si N2 C20 C25 -68.4(4) . . . . ?
C25 C20 C21 C22 0.3(4) . . . . ?
N2 C20 C21 C22 179.3(2) . . . . ?
C25 C20 C21 C26 179.5(2) . . . . ?
N2 C20 C21 C26 -1.5(4) . . . . ?
C20 C21 C22 C23 -0.3(4) . . . . ?
C26 C21 C22 C23 -179.6(3) . . . . ?
C21 C22 C23 C24 0.5(4) . . . . ?
C22 C23 C24 C25 -0.7(4) . . . . ?
C23 C24 C25 C20 0.7(4) . . . . ?
C23 C24 C25 C29 -177.3(2) . . . . ?
C21 C20 C25 C24 -0.5(4) . . . . ?
N2 C20 C25 C24 -179.5(2) . . . . ?
C21 C20 C25 C29 177.4(2) . . . . ?
N2 C20 C25 C29 -1.6(3) . . . . ?
C22 C21 C26 C28 65.6(3) . . . . ?
C20 C21 C26 C28 -113.6(3) . . . . ?
C22 C21 C26 C27 -58.4(4) . . . . ?
C20 C21 C26 C27 122.4(3) . . . . ?
C24 C25 C29 C31 -58.5(3) . . . . ?
C20 C25 C29 C31 123.6(3) . . . . ?
C24 C25 C29 C30 65.5(3) . . . . ?
C20 C25 C29 C30 -112.4(3) . . . . ?

_refine_diff_density_max         0.664
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.067

_shelxl_version_number           2013-4

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

data_KOB48B
_database_code_depnum_ccdc_archive 'CCDC 1061429'
_audit_update_record             
;
2015-04-23 deposited with the CCDC.
2015-06-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H45 N3 Si Te'
_chemical_formula_sum            'C33 H45 N3 Si Te'
_chemical_formula_weight         639.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   20.332(11)
_cell_length_b                   9.991(4)
_cell_length_c                   17.444(6)
_cell_angle_alpha                90
_cell_angle_beta                 113.408(18)
_cell_angle_gamma                90
_cell_volume                     3252(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9850
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      28.50

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_F_000             1320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.511
_exptl_crystal_size_mid          0.317
_exptl_crystal_size_min          0.186
_exptl_absorpt_coefficient_mu    0.976
_shelx_estimated_absorpt_T_min   0.635
_shelx_estimated_absorpt_T_max   0.839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5595
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'Sadabs 2008/1 (Bruker 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34122
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_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         1.091
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6399
_reflns_number_gt                5510
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP & POV-Ray'
_computing_publication_material  'Bruker SHELXTL'


_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6399
_refine_ls_number_parameters     353
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0289
_refine_ls_wR_factor_ref         0.1043
_refine_ls_wR_factor_gt          0.0904
_refine_ls_goodness_of_fit_ref   0.825
_refine_ls_restrained_S_all      0.825
_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
Te Te 0.31749(2) 0.15732(2) 0.04223(2) 0.02442(9) Uani 1 1 d . . . . .
Si Si 0.30035(3) -0.06521(6) -0.00636(4) 0.01404(14) Uani 1 1 d . . . . .
N1 N 0.21129(9) -0.12337(19) -0.08610(11) 0.0116(4) Uani 1 1 d . . . . .
N2 N 0.30819(9) -0.09790(19) -0.10678(11) 0.0129(4) Uani 1 1 d . . . . .
N3 N 0.33687(11) -0.1885(2) 0.06483(12) 0.0201(4) Uani 1 1 d . . . . .
C1 C 0.23824(11) -0.1286(2) -0.14460(14) 0.0126(4) Uani 1 1 d . . . . .
C2 C 0.20008(12) -0.1659(2) -0.23320(14) 0.0137(5) Uani 1 1 d . . . . .
C3 C 0.12920(12) -0.1257(2) -0.27866(14) 0.0164(5) Uani 1 1 d . . . . .
H3 H 0.1051 -0.0722 -0.2529 0.020 Uiso 1 1 calc R U . . .
C4 C 0.09436(14) -0.1644(2) -0.36128(16) 0.0226(6) Uani 1 1 d . . . . .
H4 H 0.0467 -0.1351 -0.3927 0.027 Uiso 1 1 calc R U . . .
C5 C 0.12858(13) -0.2456(3) -0.39844(15) 0.0261(6) Uani 1 1 d . . . . .
H5 H 0.1041 -0.2730 -0.4549 0.031 Uiso 1 1 calc R U . . .
C6 C 0.19879(14) -0.2868(3) -0.35302(16) 0.0281(6) Uani 1 1 d . . . . .
H6 H 0.2224 -0.3422 -0.3785 0.034 Uiso 1 1 calc R U . . .
C7 C 0.23426(12) -0.2472(3) -0.27076(14) 0.0205(5) Uani 1 1 d . . . . .
H7 H 0.2821 -0.2757 -0.2398 0.025 Uiso 1 1 calc R U . . .
C8 C 0.13945(12) -0.1595(2) -0.09735(13) 0.0112(4) Uani 1 1 d . . . . .
C9 C 0.09330(11) -0.0584(2) -0.09204(12) 0.0113(4) Uani 1 1 d . . . . .
C10 C 0.02364(11) -0.0923(2) -0.10362(13) 0.0145(4) Uani 1 1 d . . . . .
H10 H -0.0077 -0.0246 -0.0998 0.017 Uiso 1 1 calc R U . . .
C11 C -0.00098(11) -0.2233(2) -0.12069(14) 0.0160(5) Uani 1 1 d . . . . .
H11 H -0.0487 -0.2452 -0.1285 0.019 Uiso 1 1 calc R U . . .
C12 C 0.04502(13) -0.3208(2) -0.12614(14) 0.0156(5) Uani 1 1 d . . . . .
H12 H 0.0281 -0.4102 -0.1380 0.019 Uiso 1 1 calc R U . . .
C13 C 0.11564(11) -0.2929(2) -0.11480(13) 0.0128(4) Uani 1 1 d . . . . .
C14 C 0.11539(12) 0.0886(2) -0.07777(14) 0.0151(4) Uani 1 1 d . . . . .
H14 H 0.1674 0.0948 -0.0669 0.018 Uiso 1 1 calc R U . . .
C15 C 0.07336(15) 0.1705(2) -0.15581(16) 0.0224(5) Uani 1 1 d . . . . .
H15A H 0.0824 0.1353 -0.2031 0.034 Uiso 1 1 calc R U . . .
H15B H 0.0886 0.2642 -0.1462 0.034 Uiso 1 1 calc R U . . .
H15C H 0.0220 0.1645 -0.1682 0.034 Uiso 1 1 calc R U . . .
C16 C 0.10507(15) 0.1450(2) -0.00174(16) 0.0224(5) Uani 1 1 d . . . . .
H16A H 0.1238 0.2366 0.0090 0.034 Uiso 1 1 calc R U . . .
H16B H 0.1308 0.0890 0.0471 0.034 Uiso 1 1 calc R U . . .
H16C H 0.0539 0.1457 -0.0127 0.034 Uiso 1 1 calc R U . . .
C17 C 0.16109(12) -0.4082(2) -0.12190(14) 0.0178(5) Uani 1 1 d . . . . .
H17 H 0.2086 -0.3716 -0.1161 0.021 Uiso 1 1 calc R U . . .
C18 C 0.12692(13) -0.4775(2) -0.20727(15) 0.0232(5) Uani 1 1 d . . . . .
H18A H 0.1209 -0.4125 -0.2516 0.035 Uiso 1 1 calc R U . . .
H18B H 0.0800 -0.5136 -0.2145 0.035 Uiso 1 1 calc R U . . .
H18C H 0.1580 -0.5506 -0.2102 0.035 Uiso 1 1 calc R U . . .
C19 C 0.17390(13) -0.5086(2) -0.05016(14) 0.0246(6) Uani 1 1 d . . . . .
H19A H 0.1279 -0.5459 -0.0547 0.037 Uiso 1 1 calc R U . . .
H19B H 0.1969 -0.4626 0.0036 0.037 Uiso 1 1 calc R U . . .
H19C H 0.2050 -0.5811 -0.0538 0.037 Uiso 1 1 calc R U . . .
C20 C 0.35384(11) -0.0575(2) -0.14857(13) 0.0133(4) Uani 1 1 d . . . . .
C21 C 0.41551(12) -0.1347(2) -0.13428(14) 0.0153(5) Uani 1 1 d . . . . .
C22 C 0.45855(12) -0.0990(3) -0.17638(14) 0.0197(5) Uani 1 1 d . . . . .
H22 H 0.5010 -0.1485 -0.1669 0.024 Uiso 1 1 calc R U . . .
C23 C 0.44045(12) 0.0074(3) -0.23184(14) 0.0218(5) Uani 1 1 d . . . . .
H23 H 0.4693 0.0279 -0.2618 0.026 Uiso 1 1 calc R U . . .
C24 C 0.38090(12) 0.0832(3) -0.24357(15) 0.0217(5) Uani 1 1 d . . . . .
H24 H 0.3693 0.1564 -0.2814 0.026 Uiso 1 1 calc R U . . .
C25 C 0.33673(11) 0.0551(2) -0.20102(13) 0.0172(5) Uani 1 1 d . . . . .
C26 C 0.43620(12) -0.2516(2) -0.07350(14) 0.0187(5) Uani 1 1 d . . . . .
H26 H 0.3919 -0.2835 -0.0675 0.022 Uiso 1 1 calc R U . . .
C27 C 0.46742(17) -0.3699(3) -0.10410(18) 0.0337(7) Uani 1 1 d . . . . .
H27A H 0.4344 -0.3949 -0.1607 0.051 Uiso 1 1 calc R U . . .
H27B H 0.4741 -0.4463 -0.0665 0.051 Uiso 1 1 calc R U . . .
H27C H 0.5137 -0.3441 -0.1047 0.051 Uiso 1 1 calc R U . . .
C28 C 0.48909(13) -0.2042(3) 0.01254(15) 0.0244(5) Uani 1 1 d . . . . .
H28A H 0.5340 -0.1763 0.0089 0.037 Uiso 1 1 calc R U . . .
H28B H 0.4987 -0.2776 0.0528 0.037 Uiso 1 1 calc R U . . .
H28C H 0.4684 -0.1284 0.0309 0.037 Uiso 1 1 calc R U . . .
C29 C 0.27548(14) 0.1510(2) -0.21217(18) 0.0247(6) Uani 1 1 d . . . . .
H29 H 0.2497 0.1181 -0.1776 0.030 Uiso 1 1 calc R U . . .
C30 C 0.22167(15) 0.1597(3) -0.3034(2) 0.0385(8) Uani 1 1 d . . . . .
H30A H 0.2452 0.1988 -0.3375 0.058 Uiso 1 1 calc R U . . .
H30B H 0.1811 0.2161 -0.3069 0.058 Uiso 1 1 calc R U . . .
H30C H 0.2043 0.0697 -0.3240 0.058 Uiso 1 1 calc R U . . .
C31 C 0.30585(15) 0.2912(3) -0.1807(2) 0.0361(7) Uani 1 1 d . . . . .
H31A H 0.3295 0.3267 -0.2156 0.054 Uiso 1 1 calc R U . . .
H31B H 0.3407 0.2850 -0.1227 0.054 Uiso 1 1 calc R U . . .
H31C H 0.2667 0.3511 -0.1838 0.054 Uiso 1 1 calc R U . . .
C32 C 0.33446(16) -0.3307(3) 0.04683(17) 0.0271(6) Uani 1 1 d . . . . .
H32A H 0.3062 -0.3456 -0.0128 0.041 Uiso 1 1 calc R U . . .
H32B H 0.3123 -0.3784 0.0796 0.041 Uiso 1 1 calc R U . . .
H32C H 0.3833 -0.3641 0.0616 0.041 Uiso 1 1 calc R U . . .
C33 C 0.38159(15) -0.1619(3) 0.15274(16) 0.0294(7) Uani 1 1 d . . . . .
H33A H 0.4311 -0.1888 0.1649 0.044 Uiso 1 1 calc R U . . .
H33B H 0.3634 -0.2130 0.1882 0.044 Uiso 1 1 calc R U . . .
H33C H 0.3802 -0.0661 0.1641 0.044 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
Te Si 2.3555(11) . ?
Si N3 1.697(2) . ?
Si N2 1.8500(19) . ?
Si N1 1.884(2) . ?
Si C1 2.322(2) . ?
N1 C1 1.337(3) . ?
N1 C8 1.440(3) . ?
N2 C1 1.344(3) . ?
N2 C20 1.447(3) . ?
N3 C32 1.451(3) . ?
N3 C33 1.463(3) . ?
C1 C2 1.475(3) . ?
C2 C7 1.391(3) . ?
C2 C3 1.400(3) . ?
C3 C4 1.384(3) . ?
C4 C5 1.386(4) . ?
C5 C6 1.392(4) . ?
C6 C7 1.383(3) . ?
C8 C9 1.407(3) . ?
C8 C13 1.410(3) . ?
C9 C10 1.391(3) . ?
C9 C14 1.526(3) . ?
C10 C11 1.391(3) . ?
C11 C12 1.380(3) . ?
C12 C13 1.398(3) . ?
C13 C17 1.512(3) . ?
C14 C15 1.526(3) . ?
C14 C16 1.531(3) . ?
C17 C18 1.535(3) . ?
C17 C19 1.543(3) . ?
C20 C25 1.404(3) . ?
C20 C21 1.408(3) . ?
C21 C22 1.394(3) . ?
C21 C26 1.520(3) . ?
C22 C23 1.385(4) . ?
C23 C24 1.373(3) . ?
C24 C25 1.402(3) . ?
C25 C29 1.521(3) . ?
C26 C28 1.533(3) . ?
C26 C27 1.534(3) . ?
C29 C30 1.534(4) . ?
C29 C31 1.542(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
N3 Si N2 112.80(10) . . ?
N3 Si N1 109.22(10) . . ?
N2 Si N1 70.46(8) . . ?
N3 Si C1 117.48(10) . . ?
N2 Si C1 35.35(8) . . ?
N1 Si C1 35.17(8) . . ?
N3 Si Te 117.57(8) . . ?
N2 Si Te 116.83(7) . . ?
N1 Si Te 121.21(6) . . ?
C1 Si Te 124.94(6) . . ?
C1 N1 C8 125.94(18) . . ?
C1 N1 Si 90.60(14) . . ?
C8 N1 Si 143.42(14) . . ?
C1 N2 C20 125.58(18) . . ?
C1 N2 Si 91.87(14) . . ?
C20 N2 Si 137.88(15) . . ?
C32 N3 C33 111.0(2) . . ?
C32 N3 Si 125.80(17) . . ?
C33 N3 Si 122.95(19) . . ?
N1 C1 N2 106.91(19) . . ?
N1 C1 C2 127.2(2) . . ?
N2 C1 C2 125.8(2) . . ?
N1 C1 Si 54.23(11) . . ?
N2 C1 Si 52.78(11) . . ?
C2 C1 Si 178.24(17) . . ?
C7 C2 C3 119.7(2) . . ?
C7 C2 C1 119.2(2) . . ?
C3 C2 C1 121.1(2) . . ?
C4 C3 C2 119.7(2) . . ?
C3 C4 C5 120.4(2) . . ?
C4 C5 C6 119.9(2) . . ?
C7 C6 C5 120.0(2) . . ?
C6 C7 C2 120.3(2) . . ?
C9 C8 C13 120.8(2) . . ?
C9 C8 N1 118.56(18) . . ?
C13 C8 N1 120.60(19) . . ?
C10 C9 C8 118.9(2) . . ?
C10 C9 C14 118.32(19) . . ?
C8 C9 C14 122.74(19) . . ?
C11 C10 C9 121.3(2) . . ?
C12 C11 C10 118.9(2) . . ?
C11 C12 C13 122.4(2) . . ?
C12 C13 C8 117.7(2) . . ?
C12 C13 C17 117.6(2) . . ?
C8 C13 C17 124.7(2) . . ?
C15 C14 C9 110.24(18) . . ?
C15 C14 C16 110.8(2) . . ?
C9 C14 C16 111.30(18) . . ?
C13 C17 C18 111.53(18) . . ?
C13 C17 C19 109.90(19) . . ?
C18 C17 C19 111.0(2) . . ?
C25 C20 C21 121.8(2) . . ?
C25 C20 N2 120.62(19) . . ?
C21 C20 N2 117.56(19) . . ?
C22 C21 C20 117.9(2) . . ?
C22 C21 C26 120.4(2) . . ?
C20 C21 C26 121.7(2) . . ?
C23 C22 C21 121.1(2) . . ?
C24 C23 C22 120.1(2) . . ?
C23 C24 C25 121.5(2) . . ?
C24 C25 C20 117.4(2) . . ?
C24 C25 C29 118.0(2) . . ?
C20 C25 C29 124.5(2) . . ?
C21 C26 C28 109.7(2) . . ?
C21 C26 C27 112.8(2) . . ?
C28 C26 C27 110.6(2) . . ?
C25 C29 C30 112.2(2) . . ?
C25 C29 C31 109.6(2) . . ?
C30 C29 C31 109.7(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 Si N1 C1 -110.71(14) . . . . ?
N2 Si N1 C1 -2.55(13) . . . . ?
Te Si N1 C1 107.63(12) . . . . ?
N3 Si N1 C8 66.9(3) . . . . ?
N2 Si N1 C8 175.0(3) . . . . ?
C1 Si N1 C8 177.6(3) . . . . ?
Te Si N1 C8 -74.8(3) . . . . ?
N3 Si N2 C1 105.81(15) . . . . ?
N1 Si N2 C1 2.53(13) . . . . ?
Te Si N2 C1 -113.36(12) . . . . ?
N3 Si N2 C20 -99.5(2) . . . . ?
N1 Si N2 C20 157.2(2) . . . . ?
C1 Si N2 C20 154.7(3) . . . . ?
Te Si N2 C20 41.3(2) . . . . ?
N2 Si N3 C32 -37.1(2) . . . . ?
N1 Si N3 C32 39.1(2) . . . . ?
C1 Si N3 C32 1.7(2) . . . . ?
Te Si N3 C32 -177.63(19) . . . . ?
N2 Si N3 C33 136.61(19) . . . . ?
N1 Si N3 C33 -147.14(19) . . . . ?
C1 Si N3 C33 175.48(18) . . . . ?
Te Si N3 C33 -3.9(2) . . . . ?
C8 N1 C1 N2 -174.75(19) . . . . ?
Si N1 C1 N2 3.45(17) . . . . ?
C8 N1 C1 C2 3.0(3) . . . . ?
Si N1 C1 C2 -178.8(2) . . . . ?
C8 N1 C1 Si -178.2(2) . . . . ?
C20 N2 C1 N1 -162.9(2) . . . . ?
Si N2 C1 N1 -3.52(17) . . . . ?
C20 N2 C1 C2 19.3(3) . . . . ?
Si N2 C1 C2 178.66(19) . . . . ?
C20 N2 C1 Si -159.4(2) . . . . ?
N1 C1 C2 C7 -138.4(2) . . . . ?
N2 C1 C2 C7 39.0(3) . . . . ?
N1 C1 C2 C3 38.7(3) . . . . ?
N2 C1 C2 C3 -143.9(2) . . . . ?
C7 C2 C3 C4 -1.7(3) . . . . ?
C1 C2 C3 C4 -178.8(2) . . . . ?
C2 C3 C4 C5 1.8(4) . . . . ?
C3 C4 C5 C6 -1.1(4) . . . . ?
C4 C5 C6 C7 0.2(4) . . . . ?
C5 C6 C7 C2 -0.2(4) . . . . ?
C3 C2 C7 C6 0.9(4) . . . . ?
C1 C2 C7 C6 178.0(2) . . . . ?
C1 N1 C8 C9 -113.5(2) . . . . ?
Si N1 C8 C9 69.5(3) . . . . ?
C1 N1 C8 C13 65.3(3) . . . . ?
Si N1 C8 C13 -111.6(3) . . . . ?
C13 C8 C9 C10 0.5(3) . . . . ?
N1 C8 C9 C10 179.40(18) . . . . ?
C13 C8 C9 C14 -176.76(19) . . . . ?
N1 C8 C9 C14 2.1(3) . . . . ?
C8 C9 C10 C11 -0.4(3) . . . . ?
C14 C9 C10 C11 177.04(19) . . . . ?
C9 C10 C11 C12 0.0(3) . . . . ?
C10 C11 C12 C13 0.3(3) . . . . ?
C11 C12 C13 C8 -0.1(3) . . . . ?
C11 C12 C13 C17 179.7(2) . . . . ?
C9 C8 C13 C12 -0.3(3) . . . . ?
N1 C8 C13 C12 -179.15(19) . . . . ?
C9 C8 C13 C17 179.88(19) . . . . ?
N1 C8 C13 C17 1.0(3) . . . . ?
C10 C9 C14 C15 -65.7(3) . . . . ?
C8 C9 C14 C15 111.6(2) . . . . ?
C10 C9 C14 C16 57.6(3) . . . . ?
C8 C9 C14 C16 -125.0(2) . . . . ?
C12 C13 C17 C18 57.7(3) . . . . ?
C8 C13 C17 C18 -122.5(2) . . . . ?
C12 C13 C17 C19 -65.9(2) . . . . ?
C8 C13 C17 C19 113.9(2) . . . . ?
C1 N2 C20 C25 57.7(3) . . . . ?
Si N2 C20 C25 -90.6(3) . . . . ?
C1 N2 C20 C21 -122.5(2) . . . . ?
Si N2 C20 C21 89.2(3) . . . . ?
C25 C20 C21 C22 -2.2(3) . . . . ?
N2 C20 C21 C22 177.99(19) . . . . ?
C25 C20 C21 C26 176.3(2) . . . . ?
N2 C20 C21 C26 -3.4(3) . . . . ?
C20 C21 C22 C23 -1.3(3) . . . . ?
C26 C21 C22 C23 -179.9(2) . . . . ?
C21 C22 C23 C24 2.7(4) . . . . ?
C22 C23 C24 C25 -0.6(4) . . . . ?
C23 C24 C25 C20 -2.8(3) . . . . ?
C23 C24 C25 C29 175.0(2) . . . . ?
C21 C20 C25 C24 4.2(3) . . . . ?
N2 C20 C25 C24 -176.0(2) . . . . ?
C21 C20 C25 C29 -173.4(2) . . . . ?
N2 C20 C25 C29 6.4(3) . . . . ?
C22 C21 C26 C28 84.5(3) . . . . ?
C20 C21 C26 C28 -94.0(3) . . . . ?
C22 C21 C26 C27 -39.3(3) . . . . ?
C20 C21 C26 C27 142.2(2) . . . . ?
C24 C25 C29 C30 61.0(3) . . . . ?
C20 C25 C29 C30 -121.4(2) . . . . ?
C24 C25 C29 C31 -61.1(3) . . . . ?
C20 C25 C29 C31 116.4(3) . . . . ?

_refine_diff_density_max         0.786
_refine_diff_density_min         -1.058
_refine_diff_density_rms         0.099

_shelxl_version_number           2013-4

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

data_KOB43C
_database_code_depnum_ccdc_archive 'CCDC 1061430'
_audit_update_record             
;
2015-04-23 deposited with the CCDC.
2015-06-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H54 N4 Si2'
_chemical_formula_sum            'C36 H54 N4 Si2'
_chemical_formula_weight         599.01

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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                   17.885(10)
_cell_length_b                   10.954(7)
_cell_length_c                   36.93(2)
_cell_angle_alpha                90
_cell_angle_beta                 91.253(10)
_cell_angle_gamma                90
_cell_volume                     7234(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9880
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      25.40

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_F_000             2608
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.560
_exptl_crystal_size_mid          0.357
_exptl_crystal_size_min          0.314
_exptl_absorpt_coefficient_mu    0.127
_shelx_estimated_absorpt_T_min   0.932
_shelx_estimated_absorpt_T_max   0.961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6523
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'Sadabs 2008/1 (Bruker 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            83339
_diffrn_reflns_av_unetI/netI     0.0663
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         1.276
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             14140
_reflns_number_gt                9325
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP & POV-Ray'
_computing_publication_material  'Bruker SHELXTL'


_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)+(0.0469P)²+6.1688P] 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       0.00075(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         14140
_refine_ls_number_parameters     784
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1002
_refine_ls_R_factor_gt           0.0558
_refine_ls_wR_factor_ref         0.1404
_refine_ls_wR_factor_gt          0.1238
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_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
Si1 Si 0.87986(4) 0.14003(7) 0.13713(2) 0.01451(17) Uani 1 1 d . . . . .
Si2 Si 0.95030(4) -0.10332(7) 0.16581(2) 0.01973(18) Uani 1 1 d . . . . .
N1 N 0.83598(11) 0.18328(19) 0.09297(5) 0.0133(5) Uani 1 1 d . . . . .
N2 N 0.77747(11) 0.15780(19) 0.14238(5) 0.0131(5) Uani 1 1 d . . . . .
N3 N 0.92375(12) 0.2625(2) 0.15538(5) 0.0197(5) Uani 1 1 d . . . . .
N4 N 0.91762(11) 0.0087(2) 0.13935(5) 0.0192(5) Uani 1 1 d . . . . .
C1 C 0.76767(13) 0.1844(2) 0.10710(6) 0.0133(5) Uani 1 1 d . . . . .
C2 C 0.69641(13) 0.2155(2) 0.08857(6) 0.0145(5) Uani 1 1 d . . . . .
C3 C 0.68165(13) 0.1823(2) 0.05256(6) 0.0164(6) Uani 1 1 d . . . . .
H3 H 0.7183 0.1397 0.0393 0.020 Uiso 1 1 calc R U . . .
C4 C 0.61347(14) 0.2117(2) 0.03630(7) 0.0195(6) Uani 1 1 d . . . . .
H4 H 0.6032 0.1880 0.0119 0.023 Uiso 1 1 calc R U . . .
C5 C 0.56027(14) 0.2752(3) 0.05522(7) 0.0231(6) Uani 1 1 d . . . . .
H5 H 0.5138 0.2955 0.0438 0.028 Uiso 1 1 calc R U . . .
C6 C 0.57461(15) 0.3094(3) 0.09091(7) 0.0241(6) Uani 1 1 d . . . . .
H6 H 0.5383 0.3539 0.1039 0.029 Uiso 1 1 calc R U . . .
C7 C 0.64202(14) 0.2786(2) 0.10749(7) 0.0191(6) Uani 1 1 d . . . . .
H7 H 0.6514 0.3006 0.1321 0.023 Uiso 1 1 calc R U . . .
C8 C 0.85448(13) 0.1960(2) 0.05528(6) 0.0141(5) Uani 1 1 d . . . . .
C9 C 0.86856(13) 0.0885(2) 0.03591(6) 0.0149(6) Uani 1 1 d . . . . .
C10 C 0.88474(13) 0.1000(3) -0.00072(7) 0.0192(6) Uani 1 1 d . . . . .
H10 H 0.8941 0.0288 -0.0146 0.023 Uiso 1 1 calc R U . . .
C11 C 0.88742(14) 0.2136(3) -0.01723(7) 0.0235(6) Uani 1 1 d . . . . .
H11 H 0.8982 0.2197 -0.0422 0.028 Uiso 1 1 calc R U . . .
C12 C 0.87449(14) 0.3175(3) 0.00264(7) 0.0215(6) Uani 1 1 d . . . . .
H12 H 0.8770 0.3949 -0.0089 0.026 Uiso 1 1 calc R U . . .
C13 C 0.85770(13) 0.3119(2) 0.03934(7) 0.0167(6) Uani 1 1 d . . . . .
C14 C 0.86618(13) -0.0384(2) 0.05257(6) 0.0159(6) Uani 1 1 d . . . . .
H14 H 0.8564 -0.0293 0.0790 0.019 Uiso 1 1 calc R U . . .
C15 C 0.80322(14) -0.1161(3) 0.03572(7) 0.0224(6) Uani 1 1 d . . . . .
H15A H 0.8112 -0.1251 0.0097 0.034 Uiso 1 1 calc R U . . .
H15B H 0.7550 -0.0760 0.0395 0.034 Uiso 1 1 calc R U . . .
H15C H 0.8032 -0.1968 0.0472 0.034 Uiso 1 1 calc R U . . .
C16 C 0.94148(14) -0.1030(3) 0.04874(7) 0.0224(6) Uani 1 1 d . . . . .
H16A H 0.9527 -0.1114 0.0230 0.034 Uiso 1 1 calc R U . . .
H16B H 0.9391 -0.1840 0.0599 0.034 Uiso 1 1 calc R U . . .
H16C H 0.9808 -0.0548 0.0609 0.034 Uiso 1 1 calc R U . . .
C17 C 0.84486(16) 0.4294(2) 0.06005(7) 0.0239(6) Uani 1 1 d . . . . .
H17 H 0.8337 0.4068 0.0856 0.029 Uiso 1 1 calc R U . . .
C18 C 0.77780(17) 0.5013(3) 0.04490(8) 0.0327(7) Uani 1 1 d . . . . .
H18A H 0.7875 0.5261 0.0199 0.049 Uiso 1 1 calc R U . . .
H18B H 0.7700 0.5740 0.0598 0.049 Uiso 1 1 calc R U . . .
H18C H 0.7330 0.4498 0.0452 0.049 Uiso 1 1 calc R U . . .
C19 C 0.91565(18) 0.5078(3) 0.06088(8) 0.0375(8) Uani 1 1 d . . . . .
H19A H 0.9287 0.5298 0.0361 0.056 Uiso 1 1 calc R U . . .
H19B H 0.9569 0.4616 0.0722 0.056 Uiso 1 1 calc R U . . .
H19C H 0.9067 0.5822 0.0749 0.056 Uiso 1 1 calc R U . . .
C20 C 0.72148(13) 0.1097(2) 0.16602(6) 0.0148(5) Uani 1 1 d . . . . .
C21 C 0.71582(14) 0.1607(2) 0.20080(6) 0.0186(6) Uani 1 1 d . . . . .
C22 C 0.66040(15) 0.1163(3) 0.22321(7) 0.0236(6) Uani 1 1 d . . . . .
H22 H 0.6548 0.1510 0.2466 0.028 Uiso 1 1 calc R U . . .
C23 C 0.61346(15) 0.0230(3) 0.21219(7) 0.0232(6) Uani 1 1 d . . . . .
H23 H 0.5750 -0.0045 0.2275 0.028 Uiso 1 1 calc R U . . .
C24 C 0.62273(14) -0.0302(3) 0.17862(7) 0.0207(6) Uani 1 1 d . . . . .
H24 H 0.5913 -0.0963 0.1715 0.025 Uiso 1 1 calc R U . . .
C25 C 0.67675(13) 0.0103(2) 0.15495(6) 0.0156(6) Uani 1 1 d . . . . .
C26 C 0.76802(15) 0.2616(3) 0.21393(7) 0.0232(6) Uani 1 1 d . . . . .
H26 H 0.8123 0.2620 0.1979 0.028 Uiso 1 1 calc R U . . .
C27 C 0.72967(17) 0.3865(3) 0.21035(8) 0.0326(7) Uani 1 1 d . . . . .
H27A H 0.7156 0.4011 0.1849 0.049 Uiso 1 1 calc R U . . .
H27B H 0.7642 0.4505 0.2187 0.049 Uiso 1 1 calc R U . . .
H27C H 0.6848 0.3876 0.2251 0.049 Uiso 1 1 calc R U . . .
C28 C 0.79659(18) 0.2398(3) 0.25259(7) 0.0355(8) Uani 1 1 d . . . . .
H28A H 0.8178 0.1575 0.2545 0.053 Uiso 1 1 calc R U . . .
H28B H 0.7551 0.2478 0.2693 0.053 Uiso 1 1 calc R U . . .
H28C H 0.8353 0.3001 0.2588 0.053 Uiso 1 1 calc R U . . .
C29 C 0.68833(14) -0.0616(2) 0.12033(7) 0.0180(6) Uani 1 1 d . . . . .
H29 H 0.7236 -0.0141 0.1051 0.022 Uiso 1 1 calc R U . . .
C30 C 0.61568(15) -0.0784(3) 0.09827(7) 0.0285(7) Uani 1 1 d . . . . .
H30A H 0.5919 0.0012 0.0943 0.043 Uiso 1 1 calc R U . . .
H30B H 0.5818 -0.1317 0.1115 0.043 Uiso 1 1 calc R U . . .
H30C H 0.6268 -0.1155 0.0748 0.043 Uiso 1 1 calc R U . . .
C31 C 0.72566(15) -0.1840(3) 0.12951(8) 0.0271(7) Uani 1 1 d . . . . .
H31A H 0.7362 -0.2279 0.1071 0.041 Uiso 1 1 calc R U . . .
H31B H 0.6921 -0.2330 0.1443 0.041 Uiso 1 1 calc R U . . .
H31C H 0.7725 -0.1694 0.1431 0.041 Uiso 1 1 calc R U . . .
C32 C 0.89724(16) 0.3883(3) 0.15512(7) 0.0266(7) Uani 1 1 d . . . . .
H32A H 0.9313 0.4391 0.1412 0.040 Uiso 1 1 calc R U . . .
H32B H 0.8955 0.4189 0.1800 0.040 Uiso 1 1 calc R U . . .
H32C H 0.8470 0.3917 0.1440 0.040 Uiso 1 1 calc R U . . .
C33 C 0.99305(15) 0.2500(3) 0.17679(7) 0.0271(7) Uani 1 1 d . . . . .
H33A H 1.0099 0.1650 0.1761 0.041 Uiso 1 1 calc R U . . .
H33B H 0.9841 0.2737 0.2019 0.041 Uiso 1 1 calc R U . . .
H33C H 1.0315 0.3030 0.1667 0.041 Uiso 1 1 calc R U . . .
C34 C 0.93723(17) -0.2571(3) 0.14436(9) 0.0376(8) Uani 1 1 d . . . . .
H34A H 0.8840 -0.2705 0.1389 0.056 Uiso 1 1 calc R U . . .
H34B H 0.9555 -0.3205 0.1611 0.056 Uiso 1 1 calc R U . . .
H34C H 0.9653 -0.2608 0.1219 0.056 Uiso 1 1 calc R U . . .
C35 C 0.90214(19) -0.1079(3) 0.21020(8) 0.0447(9) Uani 1 1 d . . . . .
H35A H 0.8485 -0.1212 0.2060 0.067 Uiso 1 1 calc R U . . .
H35B H 0.9099 -0.0302 0.2229 0.067 Uiso 1 1 calc R U . . .
H35C H 0.9228 -0.1746 0.2250 0.067 Uiso 1 1 calc R U . . .
C36 C 1.05266(16) -0.0906(3) 0.17585(9) 0.0406(8) Uani 1 1 d . . . . .
H36A H 1.0798 -0.0879 0.1531 0.061 Uiso 1 1 calc R U . . .
H36B H 1.0693 -0.1615 0.1901 0.061 Uiso 1 1 calc R U . . .
H36C H 1.0627 -0.0158 0.1897 0.061 Uiso 1 1 calc R U . . .
Si3 Si 0.62392(4) 0.63055(7) -0.14840(2) 0.01487(17) Uani 1 1 d . . . . .
Si4 Si 0.53773(4) 0.39014(7) -0.17161(2) 0.02190(19) Uani 1 1 d . . . . .
N5 N 0.66476(11) 0.67197(19) -0.10288(5) 0.0135(5) Uani 1 1 d . . . . .
N6 N 0.72495(11) 0.66203(19) -0.15235(5) 0.0141(5) Uani 1 1 d . . . . .
N7 N 0.57327(12) 0.7504(2) -0.16444(6) 0.0204(5) Uani 1 1 d . . . . .
N8 N 0.59568(12) 0.4941(2) -0.15394(6) 0.0213(5) Uani 1 1 d . . . . .
C37 C 0.73282(13) 0.6840(2) -0.11655(6) 0.0130(5) Uani 1 1 d . . . . .
C38 C 0.80213(13) 0.7185(2) -0.09721(6) 0.0147(6) Uani 1 1 d . . . . .
C39 C 0.81804(14) 0.6784(2) -0.06202(6) 0.0175(6) Uani 1 1 d . . . . .
H39 H 0.7835 0.6272 -0.0500 0.021 Uiso 1 1 calc R U . . .
C40 C 0.88384(14) 0.7129(3) -0.04456(7) 0.0205(6) Uani 1 1 d . . . . .
H40 H 0.8948 0.6841 -0.0208 0.025 Uiso 1 1 calc R U . . .
C41 C 0.93406(14) 0.7893(3) -0.06161(7) 0.0223(6) Uani 1 1 d . . . . .
H41 H 0.9791 0.8131 -0.0495 0.027 Uiso 1 1 calc R U . . .
C42 C 0.91815(14) 0.8306(3) -0.09630(7) 0.0244(7) Uani 1 1 d . . . . .
H42 H 0.9521 0.8838 -0.1079 0.029 Uiso 1 1 calc R U . . .
C43 C 0.85310(14) 0.7950(2) -0.11424(7) 0.0192(6) Uani 1 1 d . . . . .
H43 H 0.8430 0.8226 -0.1382 0.023 Uiso 1 1 calc R U . . .
C44 C 0.64524(13) 0.6866(2) -0.06533(6) 0.0137(5) Uani 1 1 d . . . . .
C45 C 0.62855(13) 0.5796(2) -0.04594(6) 0.0153(6) Uani 1 1 d . . . . .
C46 C 0.61305(13) 0.5933(2) -0.00904(6) 0.0177(6) Uani 1 1 d . . . . .
H46 H 0.6017 0.5230 0.0049 0.021 Uiso 1 1 calc R U . . .
C47 C 0.61396(14) 0.7059(3) 0.00750(7) 0.0205(6) Uani 1 1 d . . . . .
H47 H 0.6044 0.7124 0.0326 0.025 Uiso 1 1 calc R U . . .
C48 C 0.62872(14) 0.8095(3) -0.01236(7) 0.0210(6) Uani 1 1 d . . . . .
H48 H 0.6280 0.8870 -0.0008 0.025 Uiso 1 1 calc R U . . .
C49 C 0.64477(13) 0.8024(2) -0.04937(7) 0.0176(6) Uani 1 1 d . . . . .
C50 C 0.62744(14) 0.4537(2) -0.06260(7) 0.0179(6) Uani 1 1 d . . . . .
H50 H 0.6339 0.4630 -0.0893 0.021 Uiso 1 1 calc R U . . .
C51 C 0.69178(15) 0.3751(3) -0.04780(7) 0.0249(7) Uani 1 1 d . . . . .
H51A H 0.6894 0.2941 -0.0590 0.037 Uiso 1 1 calc R U . . .
H51B H 0.6877 0.3669 -0.0215 0.037 Uiso 1 1 calc R U . . .
H51C H 0.7395 0.4138 -0.0534 0.037 Uiso 1 1 calc R U . . .
C52 C 0.55268(15) 0.3893(3) -0.05668(7) 0.0247(6) Uani 1 1 d . . . . .
H52A H 0.5118 0.4402 -0.0663 0.037 Uiso 1 1 calc R U . . .
H52B H 0.5460 0.3759 -0.0307 0.037 Uiso 1 1 calc R U . . .
H52C H 0.5524 0.3105 -0.0693 0.037 Uiso 1 1 calc R U . . .
C53 C 0.65796(14) 0.9198(2) -0.07002(7) 0.0202(6) Uani 1 1 d . . . . .
H53 H 0.6699 0.8970 -0.0955 0.024 Uiso 1 1 calc R U . . .
C54 C 0.72401(16) 0.9935(3) -0.05482(7) 0.0276(7) Uani 1 1 d . . . . .
H54A H 0.7688 0.9420 -0.0539 0.041 Uiso 1 1 calc R U . . .
H54B H 0.7128 1.0218 -0.0304 0.041 Uiso 1 1 calc R U . . .
H54C H 0.7328 1.0641 -0.0705 0.041 Uiso 1 1 calc R U . . .
C55 C 0.58719(17) 0.9973(3) -0.07151(8) 0.0343(8) Uani 1 1 d . . . . .
H55A H 0.5956 1.0697 -0.0865 0.051 Uiso 1 1 calc R U . . .
H55B H 0.5745 1.0227 -0.0470 0.051 Uiso 1 1 calc R U . . .
H55C H 0.5459 0.9494 -0.0821 0.051 Uiso 1 1 calc R U . . .
C56 C 0.78391(13) 0.6189(2) -0.17531(6) 0.0141(5) Uani 1 1 d . . . . .
C57 C 0.79389(14) 0.6793(2) -0.20844(6) 0.0178(6) Uani 1 1 d . . . . .
C58 C 0.85062(14) 0.6379(3) -0.23076(7) 0.0207(6) Uani 1 1 d . . . . .
H58 H 0.8589 0.6780 -0.2531 0.025 Uiso 1 1 calc R U . . .
C59 C 0.89473(14) 0.5398(3) -0.22085(7) 0.0215(6) Uani 1 1 d . . . . .
H59 H 0.9338 0.5142 -0.2361 0.026 Uiso 1 1 calc R U . . .
C60 C 0.88240(14) 0.4784(3) -0.18881(7) 0.0190(6) Uani 1 1 d . . . . .
H60 H 0.9125 0.4098 -0.1825 0.023 Uiso 1 1 calc R U . . .
C61 C 0.82597(13) 0.5161(2) -0.16543(6) 0.0166(6) Uani 1 1 d . . . . .
C62 C 0.74217(14) 0.7809(2) -0.22080(7) 0.0197(6) Uani 1 1 d . . . . .
H62 H 0.7197 0.8168 -0.1987 0.024 Uiso 1 1 calc R U . . .
C63 C 0.78004(17) 0.8845(3) -0.24103(9) 0.0374(8) Uani 1 1 d . . . . .
H63A H 0.7979 0.8541 -0.2642 0.056 Uiso 1 1 calc R U . . .
H63B H 0.8224 0.9152 -0.2265 0.056 Uiso 1 1 calc R U . . .
H63C H 0.7441 0.9506 -0.2454 0.056 Uiso 1 1 calc R U . . .
C64 C 0.67773(16) 0.7273(3) -0.24413(8) 0.0337(7) Uani 1 1 d . . . . .
H64A H 0.6395 0.7901 -0.2484 0.051 Uiso 1 1 calc R U . . .
H64B H 0.6556 0.6580 -0.2315 0.051 Uiso 1 1 calc R U . . .
H64C H 0.6971 0.6996 -0.2674 0.051 Uiso 1 1 calc R U . . .
C65 C 0.81247(14) 0.4397(2) -0.13192(7) 0.0207(6) Uani 1 1 d . . . . .
H65 H 0.7745 0.4832 -0.1172 0.025 Uiso 1 1 calc R U . . .
C66 C 0.88337(16) 0.4262(3) -0.10837(7) 0.0343(8) Uani 1 1 d . . . . .
H66A H 0.9193 0.3741 -0.1208 0.051 Uiso 1 1 calc R U . . .
H66B H 0.8707 0.3889 -0.0852 0.051 Uiso 1 1 calc R U . . .
H66C H 0.9056 0.5068 -0.1041 0.051 Uiso 1 1 calc R U . . .
C67 C 0.77978(17) 0.3160(3) -0.14257(8) 0.0336(8) Uani 1 1 d . . . . .
H67A H 0.7322 0.3279 -0.1557 0.050 Uiso 1 1 calc R U . . .
H67B H 0.7713 0.2676 -0.1207 0.050 Uiso 1 1 calc R U . . .
H67C H 0.8148 0.2728 -0.1581 0.050 Uiso 1 1 calc R U . . .
C68 C 0.59433(16) 0.8780(3) -0.16386(7) 0.0254(7) Uani 1 1 d . . . . .
H68A H 0.5961 0.9089 -0.1887 0.038 Uiso 1 1 calc R U . . .
H68B H 0.6437 0.8868 -0.1521 0.038 Uiso 1 1 calc R U . . .
H68C H 0.5575 0.9246 -0.1503 0.038 Uiso 1 1 calc R U . . .
C69 C 0.50167(15) 0.7324(3) -0.18362(8) 0.0290(7) Uani 1 1 d . . . . .
H69A H 0.5061 0.7584 -0.2089 0.043 Uiso 1 1 calc R U . . .
H69B H 0.4630 0.7809 -0.1720 0.043 Uiso 1 1 calc R U . . .
H69C H 0.4880 0.6458 -0.1829 0.043 Uiso 1 1 calc R U . . .
C70 C 0.57324(17) 0.2320(3) -0.16260(9) 0.0385(8) Uani 1 1 d . . . . .
H70A H 0.5371 0.1724 -0.1722 0.058 Uiso 1 1 calc R U . . .
H70B H 0.5799 0.2200 -0.1364 0.058 Uiso 1 1 calc R U . . .
H70C H 0.6213 0.2209 -0.1744 0.058 Uiso 1 1 calc R U . . .
C71 C 0.52199(18) 0.4033(3) -0.22177(8) 0.0456(9) Uani 1 1 d . . . . .
H71A H 0.5700 0.3973 -0.2339 0.068 Uiso 1 1 calc R U . . .
H71B H 0.4988 0.4823 -0.2274 0.068 Uiso 1 1 calc R U . . .
H71C H 0.4889 0.3374 -0.2302 0.068 Uiso 1 1 calc R U . . .
C72 C 0.44149(16) 0.3983(3) -0.15237(9) 0.0359(8) Uani 1 1 d . . . . .
H72A H 0.4220 0.4815 -0.1551 0.054 Uiso 1 1 calc R U . . .
H72B H 0.4439 0.3766 -0.1266 0.054 Uiso 1 1 calc R U . . .
H72C H 0.4084 0.3412 -0.1654 0.054 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
Si1 N4 1.590(2) . ?
Si1 N3 1.688(2) . ?
Si1 N1 1.856(2) . ?
Si1 N2 1.856(2) . ?
Si1 C1 2.323(3) . ?
Si2 N4 1.667(2) . ?
Si2 C36 1.865(3) . ?
Si2 C35 1.869(3) . ?
Si2 C34 1.874(3) . ?
N1 C1 1.339(3) . ?
N1 C8 1.445(3) . ?
N2 C1 1.343(3) . ?
N2 C20 1.442(3) . ?
N3 C32 1.457(4) . ?
N3 C33 1.462(3) . ?
C1 C2 1.473(3) . ?
C2 C7 1.393(3) . ?
C2 C3 1.398(3) . ?
C3 C4 1.385(3) . ?
C4 C5 1.381(4) . ?
C5 C6 1.389(4) . ?
C6 C7 1.382(4) . ?
C8 C13 1.402(4) . ?
C8 C9 1.403(4) . ?
C9 C10 1.395(3) . ?
C9 C14 1.521(4) . ?
C10 C11 1.387(4) . ?
C11 C12 1.376(4) . ?
C12 C13 1.396(4) . ?
C13 C17 1.517(4) . ?
C14 C16 1.530(3) . ?
C14 C15 1.532(3) . ?
C17 C19 1.530(4) . ?
C17 C18 1.531(4) . ?
C20 C21 1.406(3) . ?
C20 C25 1.407(4) . ?
C21 C22 1.393(4) . ?
C21 C26 1.519(4) . ?
C22 C23 1.378(4) . ?
C23 C24 1.383(4) . ?
C24 C25 1.390(3) . ?
C25 C29 1.519(4) . ?
C26 C28 1.524(4) . ?
C26 C27 1.535(4) . ?
C29 C30 1.530(4) . ?
C29 C31 1.533(4) . ?
Si3 N8 1.590(2) . ?
Si3 N7 1.695(2) . ?
Si3 N6 1.848(2) . ?
Si3 N5 1.874(2) . ?
Si3 C37 2.328(3) . ?
Si4 N8 1.664(2) . ?
Si4 C70 1.872(3) . ?
Si4 C71 1.873(3) . ?
Si4 C72 1.879(3) . ?
N5 C37 1.335(3) . ?
N5 C44 1.446(3) . ?
N6 C37 1.348(3) . ?
N6 C56 1.447(3) . ?
N7 C68 1.448(4) . ?
N7 C69 1.463(3) . ?
C37 C38 1.466(3) . ?
C38 C39 1.395(3) . ?
C38 C43 1.398(3) . ?
C39 C40 1.382(4) . ?
C40 C41 1.389(4) . ?
C41 C42 1.382(4) . ?
C42 C43 1.382(4) . ?
C44 C49 1.399(4) . ?
C44 C45 1.409(4) . ?
C45 C46 1.405(3) . ?
C45 C50 1.510(4) . ?
C46 C47 1.377(4) . ?
C47 C48 1.380(4) . ?
C48 C49 1.405(4) . ?
C49 C53 1.516(4) . ?
C50 C51 1.529(4) . ?
C50 C52 1.532(4) . ?
C53 C55 1.524(4) . ?
C53 C54 1.527(4) . ?
C56 C61 1.398(4) . ?
C56 C57 1.406(3) . ?
C57 C58 1.397(3) . ?
C57 C62 1.511(4) . ?
C58 C59 1.378(4) . ?
C59 C60 1.383(4) . ?
C60 C61 1.404(3) . ?
C61 C65 1.518(4) . ?
C62 C63 1.526(4) . ?
C62 C64 1.540(4) . ?
C65 C67 1.524(4) . ?
C65 C66 1.529(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
N4 Si1 N3 120.35(12) . . ?
N4 Si1 N1 116.56(10) . . ?
N3 Si1 N1 109.39(11) . . ?
N4 Si1 N2 120.56(11) . . ?
N3 Si1 N2 109.04(11) . . ?
N1 Si1 N2 70.47(9) . . ?
N4 Si1 C1 125.13(10) . . ?
N3 Si1 C1 114.42(11) . . ?
N1 Si1 C1 35.18(8) . . ?
N2 Si1 C1 35.30(8) . . ?
N4 Si2 C36 113.06(13) . . ?
N4 Si2 C35 111.80(14) . . ?
C36 Si2 C35 107.27(16) . . ?
N4 Si2 C34 112.05(13) . . ?
C36 Si2 C34 105.30(14) . . ?
C35 Si2 C34 106.92(16) . . ?
C1 N1 C8 127.2(2) . . ?
C1 N1 Si1 91.83(15) . . ?
C8 N1 Si1 140.35(16) . . ?
C1 N2 C20 126.1(2) . . ?
C1 N2 Si1 91.70(14) . . ?
C20 N2 Si1 136.44(16) . . ?
C32 N3 C33 111.3(2) . . ?
C32 N3 Si1 126.93(18) . . ?
C33 N3 Si1 121.53(19) . . ?
Si1 N4 Si2 147.06(14) . . ?
N1 C1 N2 106.0(2) . . ?
N1 C1 C2 127.5(2) . . ?
N2 C1 C2 126.5(2) . . ?
N1 C1 Si1 52.99(12) . . ?
N2 C1 Si1 53.00(12) . . ?
C2 C1 Si1 178.57(19) . . ?
C7 C2 C3 119.1(2) . . ?
C7 C2 C1 119.2(2) . . ?
C3 C2 C1 121.7(2) . . ?
C4 C3 C2 119.9(2) . . ?
C5 C4 C3 120.5(2) . . ?
C4 C5 C6 120.1(2) . . ?
C7 C6 C5 119.7(2) . . ?
C6 C7 C2 120.7(2) . . ?
C13 C8 C9 122.5(2) . . ?
C13 C8 N1 120.3(2) . . ?
C9 C8 N1 117.2(2) . . ?
C10 C9 C8 117.5(2) . . ?
C10 C9 C14 118.9(2) . . ?
C8 C9 C14 123.6(2) . . ?
C11 C10 C9 121.2(2) . . ?
C12 C11 C10 120.0(2) . . ?
C11 C12 C13 121.6(3) . . ?
C12 C13 C8 117.4(2) . . ?
C12 C13 C17 119.4(2) . . ?
C8 C13 C17 123.3(2) . . ?
C9 C14 C16 110.6(2) . . ?
C9 C14 C15 111.7(2) . . ?
C16 C14 C15 110.3(2) . . ?
C13 C17 C19 110.6(2) . . ?
C13 C17 C18 112.2(2) . . ?
C19 C17 C18 111.1(2) . . ?
C21 C20 C25 121.4(2) . . ?
C21 C20 N2 118.2(2) . . ?
C25 C20 N2 120.3(2) . . ?
C22 C21 C20 118.1(2) . . ?
C22 C21 C26 120.3(2) . . ?
C20 C21 C26 121.6(2) . . ?
C23 C22 C21 121.4(2) . . ?
C22 C23 C24 119.5(2) . . ?
C23 C24 C25 121.9(3) . . ?
C24 C25 C20 117.6(2) . . ?
C24 C25 C29 118.2(2) . . ?
C20 C25 C29 124.0(2) . . ?
C21 C26 C28 112.1(2) . . ?
C21 C26 C27 110.5(2) . . ?
C28 C26 C27 111.1(2) . . ?
C25 C29 C30 112.4(2) . . ?
C25 C29 C31 109.5(2) . . ?
C30 C29 C31 111.9(2) . . ?
N8 Si3 N7 121.17(12) . . ?
N8 Si3 N6 118.27(11) . . ?
N7 Si3 N6 110.11(11) . . ?
N8 Si3 N5 117.37(11) . . ?
N7 Si3 N5 108.73(11) . . ?
N6 Si3 N5 70.31(9) . . ?
N8 Si3 C37 124.17(10) . . ?
N7 Si3 C37 114.62(11) . . ?
N6 Si3 C37 35.36(8) . . ?
N5 Si3 C37 34.96(8) . . ?
N8 Si4 C70 110.95(13) . . ?
N8 Si4 C71 114.45(14) . . ?
C70 Si4 C71 106.88(16) . . ?
N8 Si4 C72 112.78(13) . . ?
C70 Si4 C72 106.68(14) . . ?
C71 Si4 C72 104.55(15) . . ?
C37 N5 C44 126.4(2) . . ?
C37 N5 Si3 91.46(15) . . ?
C44 N5 Si3 142.14(16) . . ?
C37 N6 C56 124.8(2) . . ?
C37 N6 Si3 92.14(14) . . ?
C56 N6 Si3 135.36(17) . . ?
C68 N7 C69 111.2(2) . . ?
C68 N7 Si3 127.29(18) . . ?
C69 N7 Si3 121.36(19) . . ?
Si3 N8 Si4 152.59(15) . . ?
N5 C37 N6 106.1(2) . . ?
N5 C37 C38 127.6(2) . . ?
N6 C37 C38 126.4(2) . . ?
N5 C37 Si3 53.57(12) . . ?
N6 C37 Si3 52.50(12) . . ?
C38 C37 Si3 178.80(18) . . ?
C39 C38 C43 119.1(2) . . ?
C39 C38 C37 121.7(2) . . ?
C43 C38 C37 119.2(2) . . ?
C40 C39 C38 120.2(2) . . ?
C39 C40 C41 120.4(2) . . ?
C42 C41 C40 119.7(2) . . ?
C43 C42 C41 120.4(2) . . ?
C42 C43 C38 120.3(2) . . ?
C49 C44 C45 122.5(2) . . ?
C49 C44 N5 120.5(2) . . ?
C45 C44 N5 116.9(2) . . ?
C46 C45 C44 116.9(2) . . ?
C46 C45 C50 119.5(2) . . ?
C44 C45 C50 123.6(2) . . ?
C47 C46 C45 121.7(2) . . ?
C46 C47 C48 120.1(2) . . ?
C47 C48 C49 121.2(3) . . ?
C44 C49 C48 117.6(2) . . ?
C44 C49 C53 123.7(2) . . ?
C48 C49 C53 118.7(2) . . ?
C45 C50 C51 111.4(2) . . ?
C45 C50 C52 111.5(2) . . ?
C51 C50 C52 110.0(2) . . ?
C49 C53 C55 110.6(2) . . ?
C49 C53 C54 113.0(2) . . ?
C55 C53 C54 110.7(2) . . ?
C61 C56 C57 121.9(2) . . ?
C61 C56 N6 120.3(2) . . ?
C57 C56 N6 117.7(2) . . ?
C58 C57 C56 117.9(2) . . ?
C58 C57 C62 120.6(2) . . ?
C56 C57 C62 121.4(2) . . ?
C59 C58 C57 121.0(2) . . ?
C58 C59 C60 120.4(2) . . ?
C59 C60 C61 120.9(3) . . ?
C56 C61 C60 117.8(2) . . ?
C56 C61 C65 124.2(2) . . ?
C60 C61 C65 117.9(2) . . ?
C57 C62 C63 114.9(2) . . ?
C57 C62 C64 109.5(2) . . ?
C63 C62 C64 110.1(2) . . ?
C61 C65 C67 110.3(2) . . ?
C61 C65 C66 111.9(2) . . ?
C67 C65 C66 111.7(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 Si1 N1 C1 114.05(16) . . . . ?
N3 Si1 N1 C1 -105.16(16) . . . . ?
N2 Si1 N1 C1 -1.15(14) . . . . ?
N4 Si1 N1 C8 -56.7(3) . . . . ?
N3 Si1 N1 C8 84.1(3) . . . . ?
N2 Si1 N1 C8 -171.9(3) . . . . ?
C1 Si1 N1 C8 -170.7(3) . . . . ?
N4 Si1 N2 C1 -108.83(16) . . . . ?
N3 Si1 N2 C1 105.64(16) . . . . ?
N1 Si1 N2 C1 1.14(14) . . . . ?
N4 Si1 N2 C20 43.6(3) . . . . ?
N3 Si1 N2 C20 -102.0(3) . . . . ?
N1 Si1 N2 C20 153.5(3) . . . . ?
C1 Si1 N2 C20 152.4(3) . . . . ?
N4 Si1 N3 C32 179.0(2) . . . . ?
N1 Si1 N3 C32 40.0(2) . . . . ?
N2 Si1 N3 C32 -35.4(2) . . . . ?
C1 Si1 N3 C32 2.3(2) . . . . ?
N4 Si1 N3 C33 -6.5(2) . . . . ?
N1 Si1 N3 C33 -145.53(19) . . . . ?
N2 Si1 N3 C33 139.15(19) . . . . ?
C1 Si1 N3 C33 176.82(18) . . . . ?
N3 Si1 N4 Si2 61.1(3) . . . . ?
N1 Si1 N4 Si2 -162.6(2) . . . . ?
N2 Si1 N4 Si2 -80.6(3) . . . . ?
C1 Si1 N4 Si2 -122.6(2) . . . . ?
C36 Si2 N4 Si1 -93.2(3) . . . . ?
C35 Si2 N4 Si1 28.0(3) . . . . ?
C34 Si2 N4 Si1 148.0(3) . . . . ?
C8 N1 C1 N2 174.1(2) . . . . ?
Si1 N1 C1 N2 1.55(19) . . . . ?
C8 N1 C1 C2 -9.1(4) . . . . ?
Si1 N1 C1 C2 178.3(2) . . . . ?
C8 N1 C1 Si1 172.6(3) . . . . ?
C20 N2 C1 N1 -158.3(2) . . . . ?
Si1 N2 C1 N1 -1.55(19) . . . . ?
C20 N2 C1 C2 24.9(4) . . . . ?
Si1 N2 C1 C2 -178.3(2) . . . . ?
C20 N2 C1 Si1 -156.7(3) . . . . ?
N1 C1 C2 C7 -143.4(3) . . . . ?
N2 C1 C2 C7 32.7(4) . . . . ?
N1 C1 C2 C3 37.2(4) . . . . ?
N2 C1 C2 C3 -146.7(3) . . . . ?
C7 C2 C3 C4 -0.3(4) . . . . ?
C1 C2 C3 C4 179.1(2) . . . . ?
C2 C3 C4 C5 0.9(4) . . . . ?
C3 C4 C5 C6 -0.4(4) . . . . ?
C4 C5 C6 C7 -0.7(4) . . . . ?
C5 C6 C7 C2 1.3(4) . . . . ?
C3 C2 C7 C6 -0.8(4) . . . . ?
C1 C2 C7 C6 179.8(2) . . . . ?
C1 N1 C8 C13 81.3(3) . . . . ?
Si1 N1 C8 C13 -110.4(3) . . . . ?
C1 N1 C8 C9 -98.5(3) . . . . ?
Si1 N1 C8 C9 69.8(3) . . . . ?
C13 C8 C9 C10 -1.3(4) . . . . ?
N1 C8 C9 C10 178.5(2) . . . . ?
C13 C8 C9 C14 179.4(2) . . . . ?
N1 C8 C9 C14 -0.7(3) . . . . ?
C8 C9 C10 C11 0.6(4) . . . . ?
C14 C9 C10 C11 179.9(2) . . . . ?
C9 C10 C11 C12 0.4(4) . . . . ?
C10 C11 C12 C13 -0.7(4) . . . . ?
C11 C12 C13 C8 0.0(4) . . . . ?
C11 C12 C13 C17 179.3(2) . . . . ?
C9 C8 C13 C12 1.1(4) . . . . ?
N1 C8 C13 C12 -178.8(2) . . . . ?
C9 C8 C13 C17 -178.2(2) . . . . ?
N1 C8 C13 C17 1.9(4) . . . . ?
C10 C9 C14 C16 59.2(3) . . . . ?
C8 C9 C14 C16 -121.5(3) . . . . ?
C10 C9 C14 C15 -64.0(3) . . . . ?
C8 C9 C14 C15 115.2(3) . . . . ?
C12 C13 C17 C19 -62.8(3) . . . . ?
C8 C13 C17 C19 116.5(3) . . . . ?
C12 C13 C17 C18 61.9(3) . . . . ?
C8 C13 C17 C18 -118.8(3) . . . . ?
C1 N2 C20 C21 -135.9(3) . . . . ?
Si1 N2 C20 C21 79.1(3) . . . . ?
C1 N2 C20 C25 47.4(4) . . . . ?
Si1 N2 C20 C25 -97.6(3) . . . . ?
C25 C20 C21 C22 -5.0(4) . . . . ?
N2 C20 C21 C22 178.3(2) . . . . ?
C25 C20 C21 C26 175.2(2) . . . . ?
N2 C20 C21 C26 -1.5(4) . . . . ?
C20 C21 C22 C23 1.6(4) . . . . ?
C26 C21 C22 C23 -178.6(2) . . . . ?
C21 C22 C23 C24 1.9(4) . . . . ?
C22 C23 C24 C25 -2.1(4) . . . . ?
C23 C24 C25 C20 -1.1(4) . . . . ?
C23 C24 C25 C29 173.8(2) . . . . ?
C21 C20 C25 C24 4.7(4) . . . . ?
N2 C20 C25 C24 -178.7(2) . . . . ?
C21 C20 C25 C29 -169.9(2) . . . . ?
N2 C20 C25 C29 6.7(4) . . . . ?
C22 C21 C26 C28 44.3(3) . . . . ?
C20 C21 C26 C28 -135.9(3) . . . . ?
C22 C21 C26 C27 -80.3(3) . . . . ?
C20 C21 C26 C27 99.5(3) . . . . ?
C24 C25 C29 C30 54.1(3) . . . . ?
C20 C25 C29 C30 -131.3(3) . . . . ?
C24 C25 C29 C31 -71.0(3) . . . . ?
C20 C25 C29 C31 103.6(3) . . . . ?
N8 Si3 N5 C37 111.31(16) . . . . ?
N7 Si3 N5 C37 -106.43(16) . . . . ?
N6 Si3 N5 C37 -1.10(14) . . . . ?
N8 Si3 N5 C44 -66.5(3) . . . . ?
N7 Si3 N5 C44 75.8(3) . . . . ?
N6 Si3 N5 C44 -178.9(3) . . . . ?
C37 Si3 N5 C44 -177.8(4) . . . . ?
N8 Si3 N6 C37 -110.14(16) . . . . ?
N7 Si3 N6 C37 104.51(16) . . . . ?
N5 Si3 N6 C37 1.09(14) . . . . ?
N8 Si3 N6 C56 38.2(3) . . . . ?
N7 Si3 N6 C56 -107.1(2) . . . . ?
N5 Si3 N6 C56 149.5(3) . . . . ?
C37 Si3 N6 C56 148.4(3) . . . . ?
N8 Si3 N7 C68 -175.0(2) . . . . ?
N6 Si3 N7 C68 -30.8(2) . . . . ?
N5 Si3 N7 C68 44.5(2) . . . . ?
C37 Si3 N7 C68 7.3(2) . . . . ?
N8 Si3 N7 C69 0.6(2) . . . . ?
N6 Si3 N7 C69 144.75(19) . . . . ?
N5 Si3 N7 C69 -140.01(19) . . . . ?
C37 Si3 N7 C69 -177.21(18) . . . . ?
N7 Si3 N8 Si4 8.1(4) . . . . ?
N6 Si3 N8 Si4 -133.3(3) . . . . ?
N5 Si3 N8 Si4 145.5(3) . . . . ?
C37 Si3 N8 Si4 -174.4(3) . . . . ?
C70 Si4 N8 Si3 170.5(3) . . . . ?
C71 Si4 N8 Si3 49.5(4) . . . . ?
C72 Si4 N8 Si3 -69.9(4) . . . . ?
C44 N5 C37 N6 179.8(2) . . . . ?
Si3 N5 C37 N6 1.48(19) . . . . ?
C44 N5 C37 C38 -2.2(4) . . . . ?
Si3 N5 C37 C38 179.5(2) . . . . ?
C44 N5 C37 Si3 178.3(3) . . . . ?
C56 N6 C37 N5 -154.8(2) . . . . ?
Si3 N6 C37 N5 -1.50(19) . . . . ?
C56 N6 C37 C38 27.1(4) . . . . ?
Si3 N6 C37 C38 -179.5(2) . . . . ?
C56 N6 C37 Si3 -153.3(3) . . . . ?
N5 C37 C38 C39 37.5(4) . . . . ?
N6 C37 C38 C39 -144.9(3) . . . . ?
N5 C37 C38 C43 -141.5(3) . . . . ?
N6 C37 C38 C43 36.2(4) . . . . ?
C43 C38 C39 C40 -0.8(4) . . . . ?
C37 C38 C39 C40 -179.8(2) . . . . ?
C38 C39 C40 C41 1.1(4) . . . . ?
C39 C40 C41 C42 -0.3(4) . . . . ?
C40 C41 C42 C43 -0.9(4) . . . . ?
C41 C42 C43 C38 1.1(4) . . . . ?
C39 C38 C43 C42 -0.3(4) . . . . ?
C37 C38 C43 C42 178.8(2) . . . . ?
C37 N5 C44 C49 71.7(3) . . . . ?
Si3 N5 C44 C49 -111.1(3) . . . . ?
C37 N5 C44 C45 -107.1(3) . . . . ?
Si3 N5 C44 C45 70.1(3) . . . . ?
C49 C44 C45 C46 -1.7(4) . . . . ?
N5 C44 C45 C46 177.1(2) . . . . ?
C49 C44 C45 C50 179.0(2) . . . . ?
N5 C44 C45 C50 -2.2(3) . . . . ?
C44 C45 C46 C47 0.1(4) . . . . ?
C50 C45 C46 C47 179.5(2) . . . . ?
C45 C46 C47 C48 1.5(4) . . . . ?
C46 C47 C48 C49 -1.5(4) . . . . ?
C45 C44 C49 C48 1.6(4) . . . . ?
N5 C44 C49 C48 -177.1(2) . . . . ?
C45 C44 C49 C53 -176.2(2) . . . . ?
N5 C44 C49 C53 5.1(4) . . . . ?
C47 C48 C49 C44 0.0(4) . . . . ?
C47 C48 C49 C53 178.0(2) . . . . ?
C46 C45 C50 C51 -68.0(3) . . . . ?
C44 C45 C50 C51 111.3(3) . . . . ?
C46 C45 C50 C52 55.3(3) . . . . ?
C44 C45 C50 C52 -125.4(2) . . . . ?
C44 C49 C53 C55 113.2(3) . . . . ?
C48 C49 C53 C55 -64.6(3) . . . . ?
C44 C49 C53 C54 -122.0(3) . . . . ?
C48 C49 C53 C54 60.2(3) . . . . ?
C37 N6 C56 C61 51.2(3) . . . . ?
Si3 N6 C56 C61 -89.2(3) . . . . ?
C37 N6 C56 C57 -132.5(3) . . . . ?
Si3 N6 C56 C57 87.1(3) . . . . ?
C61 C56 C57 C58 -3.7(4) . . . . ?
N6 C56 C57 C58 -179.9(2) . . . . ?
C61 C56 C57 C62 172.7(2) . . . . ?
N6 C56 C57 C62 -3.5(4) . . . . ?
C56 C57 C58 C59 0.9(4) . . . . ?
C62 C57 C58 C59 -175.5(2) . . . . ?
C57 C58 C59 C60 1.5(4) . . . . ?
C58 C59 C60 C61 -1.3(4) . . . . ?
C57 C56 C61 C60 3.8(4) . . . . ?
N6 C56 C61 C60 179.9(2) . . . . ?
C57 C56 C61 C65 -173.6(2) . . . . ?
N6 C56 C61 C65 2.6(4) . . . . ?
C59 C60 C61 C56 -1.3(4) . . . . ?
C59 C60 C61 C65 176.3(2) . . . . ?
C58 C57 C62 C63 -40.1(3) . . . . ?
C56 C57 C62 C63 143.6(3) . . . . ?
C58 C57 C62 C64 84.4(3) . . . . ?
C56 C57 C62 C64 -91.9(3) . . . . ?
C56 C61 C65 C67 109.0(3) . . . . ?
C60 C61 C65 C67 -68.4(3) . . . . ?
C56 C61 C65 C66 -126.0(3) . . . . ?
C60 C61 C65 C66 56.6(3) . . . . ?

_refine_diff_density_max         0.516
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.063

_shelxl_version_number           2013-4

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

data_KOB47c
_database_code_depnum_ccdc_archive 'CCDC 1061431'
_audit_update_record             
;
2015-04-23 deposited with the CCDC.
2015-06-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H52 N4 S Si'
_chemical_formula_sum            'C40 H52 N4 S Si'
_chemical_formula_weight         649.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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                   9.866(3)
_cell_length_b                   12.248(4)
_cell_length_c                   16.690(6)
_cell_angle_alpha                92.69(3)
_cell_angle_beta                 98.34(2)
_cell_angle_gamma                108.06(3)
_cell_volume                     1888.0(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6968
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      28.18

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_F_000             700
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.522
_exptl_crystal_size_mid          0.341
_exptl_crystal_size_min          0.339
_exptl_absorpt_coefficient_mu    0.150
_shelx_estimated_absorpt_T_min   0.926
_shelx_estimated_absorpt_T_max   0.951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6858
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'Sadabs 2008/1 (Bruker 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22773
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.703
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7434
_reflns_number_gt                5754
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP & POV-Ray'
_computing_publication_material  'Bruker SHELXTL'


_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)+(0.0795P)²+0.2039P] 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         7434
_refine_ls_number_parameters     449
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0412
_refine_ls_wR_factor_ref         0.1233
_refine_ls_wR_factor_gt          0.1109
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_restrained_S_all      0.954
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.17125(14) 0.73573(11) 0.25178(8) 0.0145(3) Uani 1 1 d . . . . .
N2 N 0.23796(14) 0.93180(11) 0.26391(8) 0.0145(3) Uani 1 1 d . . . . .
C1 C 0.16521(16) 0.83733(13) 0.21914(10) 0.0140(3) Uani 1 1 d . . . . .
C2 C 0.07551(19) 0.82983(14) 0.13754(10) 0.0192(4) Uani 1 1 d . . . . .
C3 C -0.0703(2) 0.76279(15) 0.12188(11) 0.0260(4) Uani 1 1 d . . . . .
H3 H -0.1123 0.7185 0.1625 0.031 Uiso 1 1 calc R U . . .
C4 C -0.1538(2) 0.76073(18) 0.04720(13) 0.0387(5) Uani 1 1 d . . . . .
H4 H -0.2534 0.7163 0.0372 0.046 Uiso 1 1 calc R U . . .
C5 C -0.0931(3) 0.82260(18) -0.01241(12) 0.0409(6) Uani 1 1 d . . . . .
H5 H -0.1507 0.8207 -0.0636 0.049 Uiso 1 1 calc R U . . .
C6 C 0.0519(3) 0.88775(17) 0.00198(12) 0.0395(6) Uani 1 1 d . . . . .
H6 H 0.0941 0.9291 -0.0398 0.047 Uiso 1 1 calc R U . . .
C7 C 0.1359(2) 0.89282(15) 0.07727(11) 0.0274(4) Uani 1 1 d . . . . .
H7 H 0.2347 0.9394 0.0875 0.033 Uiso 1 1 calc R U . . .
C8 C 0.12574(17) 0.62880(13) 0.19888(9) 0.0148(3) Uani 1 1 d . . . . .
C9 C -0.00083(18) 0.53983(14) 0.20775(10) 0.0195(4) Uani 1 1 d . . . . .
C10 C -0.04373(19) 0.43964(14) 0.15433(11) 0.0245(4) Uani 1 1 d . . . . .
H10 H -0.1285 0.3789 0.1596 0.029 Uiso 1 1 calc R U . . .
C11 C 0.0334(2) 0.42643(15) 0.09417(11) 0.0263(4) Uani 1 1 d . . . . .
H11 H 0.0009 0.3581 0.0578 0.032 Uiso 1 1 calc R U . . .
C12 C 0.15834(19) 0.51337(15) 0.08723(11) 0.0241(4) Uani 1 1 d . . . . .
H12 H 0.2118 0.5035 0.0461 0.029 Uiso 1 1 calc R U . . .
C13 C 0.20806(17) 0.61524(14) 0.13900(10) 0.0171(4) Uani 1 1 d . . . . .
C14 C -0.0925(2) 0.54631(16) 0.27272(12) 0.0313(5) Uani 1 1 d . . . . .
H14 H -0.0537 0.6254 0.3023 0.038 Uiso 1 1 calc R U . . .
C15 C -0.2526(2) 0.52310(19) 0.23709(16) 0.0448(6) Uani 1 1 d . . . . .
H15A H -0.2604 0.5768 0.1963 0.067 Uiso 1 1 calc R U . . .
H15B H -0.3050 0.5341 0.2807 0.067 Uiso 1 1 calc R U . . .
H15C H -0.2944 0.4436 0.2115 0.067 Uiso 1 1 calc R U . . .
C16 C -0.0831(2) 0.4586(2) 0.33405(14) 0.0476(6) Uani 1 1 d . . . . .
H16A H -0.1275 0.3802 0.3068 0.071 Uiso 1 1 calc R U . . .
H16B H -0.1345 0.4688 0.3784 0.071 Uiso 1 1 calc R U . . .
H16C H 0.0186 0.4706 0.3562 0.071 Uiso 1 1 calc R U . . .
C17 C 0.34997(18) 0.70559(15) 0.12915(11) 0.0223(4) Uani 1 1 d . . . . .
H17 H 0.3601 0.7782 0.1629 0.027 Uiso 1 1 calc R U . . .
C18 C 0.3551(2) 0.73324(18) 0.04067(12) 0.0330(5) Uani 1 1 d . . . . .
H18A H 0.3586 0.6659 0.0079 0.049 Uiso 1 1 calc R U . . .
H18B H 0.4414 0.7990 0.0387 0.049 Uiso 1 1 calc R U . . .
H18C H 0.2685 0.7525 0.0189 0.049 Uiso 1 1 calc R U . . .
C19 C 0.4792(2) 0.66509(18) 0.16003(12) 0.0322(5) Uani 1 1 d . . . . .
H19A H 0.4700 0.5928 0.1285 0.048 Uiso 1 1 calc R U . . .
H19B H 0.4807 0.6525 0.2177 0.048 Uiso 1 1 calc R U . . .
H19C H 0.5692 0.7242 0.1536 0.048 Uiso 1 1 calc R U . . .
C20 C 0.22784(17) 1.04199(13) 0.24574(9) 0.0142(3) Uani 1 1 d . . . . .
C21 C 0.35103(17) 1.12494(14) 0.22657(9) 0.0163(3) Uani 1 1 d . . . . .
C22 C 0.34703(19) 1.23609(14) 0.21556(10) 0.0205(4) Uani 1 1 d . . . . .
H22 H 0.4296 1.2920 0.2023 0.025 Uiso 1 1 calc R U . . .
C23 C 0.22605(19) 1.26692(15) 0.22343(10) 0.0228(4) Uani 1 1 d . . . . .
H23 H 0.2251 1.3430 0.2156 0.027 Uiso 1 1 calc R U . . .
C24 C 0.10637(19) 1.18528(15) 0.24281(10) 0.0221(4) Uani 1 1 d . . . . .
H24 H 0.0229 1.2063 0.2480 0.027 Uiso 1 1 calc R U . . .
C25 C 0.10430(18) 1.07271(14) 0.25504(10) 0.0189(4) Uani 1 1 d . . . . .
C26 C 0.48962(17) 1.09756(14) 0.22067(10) 0.0194(4) Uani 1 1 d . . . . .
H26 H 0.4680 1.0123 0.2213 0.023 Uiso 1 1 calc R U . . .
C27 C 0.5458(2) 1.13214(17) 0.14152(12) 0.0324(5) Uani 1 1 d . . . . .
H27A H 0.4681 1.0984 0.0951 0.049 Uiso 1 1 calc R U . . .
H27B H 0.6270 1.1037 0.1366 0.049 Uiso 1 1 calc R U . . .
H27C H 0.5782 1.2164 0.1423 0.049 Uiso 1 1 calc R U . . .
C28 C 0.60344(19) 1.15656(16) 0.29535(12) 0.0278(4) Uani 1 1 d . . . . .
H28A H 0.6924 1.1381 0.2920 0.042 Uiso 1 1 calc R U . . .
H28B H 0.5669 1.1290 0.3448 0.042 Uiso 1 1 calc R U . . .
H28C H 0.6239 1.2403 0.2971 0.042 Uiso 1 1 calc R U . . .
C29 C -0.02995(18) 0.99042(15) 0.28085(11) 0.0227(4) Uani 1 1 d . . . . .
H29 H -0.0155 0.9136 0.2858 0.027 Uiso 1 1 calc R U . . .
C30 C -0.16559(19) 0.97466(17) 0.21749(12) 0.0314(5) Uani 1 1 d . . . . .
H30A H -0.1535 0.9421 0.1653 0.047 Uiso 1 1 calc R U . . .
H30B H -0.1799 1.0496 0.2109 0.047 Uiso 1 1 calc R U . . .
H30C H -0.2500 0.9222 0.2358 0.047 Uiso 1 1 calc R U . . .
C31 C -0.0508(2) 1.03556(18) 0.36395(12) 0.0325(5) Uani 1 1 d . . . . .
H31A H -0.0685 1.1096 0.3596 0.049 Uiso 1 1 calc R U . . .
H31B H 0.0365 1.0460 0.4039 0.049 Uiso 1 1 calc R U . . .
H31C H -0.1336 0.9798 0.3814 0.049 Uiso 1 1 calc R U . . .
C34 C 0.58931(19) 0.79975(14) 0.41930(11) 0.0230(4) Uani 1 1 d D . . . .
C35 C 0.57426(19) 0.79625(15) 0.50054(11) 0.0247(4) Uani 1 1 d . . . . .
H35 H 0.5032 0.8233 0.5197 0.030 Uiso 1 1 calc R U . . .
C36 C 0.6622(2) 0.75350(15) 0.55413(11) 0.0283(4) Uani 1 1 d . . . . .
H36 H 0.6498 0.7499 0.6094 0.034 Uiso 1 1 calc R U . . .
C37 C 0.7679(2) 0.71615(16) 0.52714(12) 0.0332(5) Uani 1 1 d . . . . .
H37 H 0.8286 0.6875 0.5639 0.040 Uiso 1 1 calc R U . . .
C38 C 0.7850(3) 0.72052(19) 0.44631(13) 0.0409(5) Uani 1 1 d . . . . .
H38 H 0.8582 0.6958 0.4277 0.049 Uiso 1 1 calc R U . . .
C39 C 0.6950(2) 0.76111(17) 0.39251(12) 0.0344(5) Uani 1 1 d . . . . .
H39 H 0.7057 0.7625 0.3369 0.041 Uiso 1 1 calc R U . . .
S1 S 0.48373(14) 0.86593(11) 0.35255(8) 0.0221(2) Uani 0.823(3) 1 d D . P A 1
C32 C 0.3268(4) 0.5528(4) 0.3552(3) 0.0310(8) Uani 0.823(3) 1 d D . P A 1
H32A H 0.3454 0.5727 0.3007 0.046 Uiso 0.823(3) 1 calc R U P A 1
H32B H 0.2620 0.4731 0.3515 0.046 Uiso 0.823(3) 1 calc R U P A 1
H32C H 0.4183 0.5602 0.3904 0.046 Uiso 0.823(3) 1 calc R U P A 1
C33 C 0.2324(3) 0.6044(2) 0.47113(13) 0.0299(6) Uani 0.823(3) 1 d D . P A 1
H33A H 0.1681 0.5249 0.4692 0.045 Uiso 0.823(3) 1 calc R U P A 1
H33B H 0.1867 0.6576 0.4924 0.045 Uiso 0.823(3) 1 calc R U P A 1
H33C H 0.3242 0.6136 0.5067 0.045 Uiso 0.823(3) 1 calc R U P A 1
N3 N 0.2595(2) 0.63028(17) 0.38892(13) 0.0201(4) Uani 0.823(3) 1 d D . P A 1
Si Si 0.26372(14) 0.75875(10) 0.35275(8) 0.0152(2) Uani 0.823(3) 1 d D . P A 1
N4 N 0.1672(2) 0.81412(16) 0.41349(11) 0.0252(5) Uani 0.823(3) 1 d D . P A 1
C40 C 0.2181(4) 0.9082(3) 0.4567(2) 0.0411(9) Uani 0.823(3) 1 d D . P A 1
H40A H 0.3156 0.9544 0.4577 0.049 Uiso 0.823(3) 1 calc R U P A 1
H40B H 0.1594 0.9337 0.4886 0.049 Uiso 0.823(3) 1 calc R U P A 1
S1B S 0.4988(8) 0.8488(6) 0.3400(4) 0.0221(2) Uani 0.177(3) 1 d D . P A 2
C32B C 0.1512(12) 0.7150(8) 0.4844(7) 0.0310(8) Uani 0.177(3) 1 d D . P A 2
H32D H 0.2182 0.7150 0.5339 0.046 Uiso 0.177(3) 1 calc R U P A 2
H32E H 0.1085 0.6363 0.4576 0.046 Uiso 0.177(3) 1 calc R U P A 2
H32F H 0.0744 0.7434 0.4987 0.046 Uiso 0.177(3) 1 calc R U P A 2
C33B C 0.2669(18) 0.9122(12) 0.4620(12) 0.0299(6) Uani 0.177(3) 1 d D . P A 2
H33D H 0.1777 0.9306 0.4649 0.045 Uiso 0.177(3) 1 calc R U P A 2
H33E H 0.3230 0.9628 0.4264 0.045 Uiso 0.177(3) 1 calc R U P A 2
H33F H 0.3242 0.9238 0.5167 0.045 Uiso 0.177(3) 1 calc R U P A 2
N3B N 0.2301(11) 0.7906(7) 0.4290(5) 0.0201(4) Uani 0.177(3) 1 d D . P A 2
SiB Si 0.2851(8) 0.7416(6) 0.3488(5) 0.0152(2) Uani 0.177(3) 1 d D . P A 2
N4B N 0.2724(13) 0.6011(10) 0.3623(7) 0.0252(5) Uani 0.177(3) 1 d D . P A 2
C40B C 0.358(3) 0.549(2) 0.3542(18) 0.0411(9) Uani 0.177(3) 1 d D . P A 2
H40C H 0.4476 0.5878 0.3380 0.049 Uiso 0.177(3) 1 calc R U P A 2
H40D H 0.3345 0.4704 0.3641 0.049 Uiso 0.177(3) 1 calc R U P A 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
N1 C1 1.396(2) . ?
N1 C8 1.452(2) . ?
N1 Si 1.761(2) . ?
N1 SiB 1.817(8) . ?
N2 C1 1.289(2) . ?
N2 C20 1.427(2) . ?
C1 C2 1.495(2) . ?
C2 C7 1.387(2) . ?
C2 C3 1.397(3) . ?
C3 C4 1.385(3) . ?
C4 C5 1.373(3) . ?
C5 C6 1.384(3) . ?
C6 C7 1.389(3) . ?
C8 C13 1.410(2) . ?
C8 C9 1.412(2) . ?
C9 C10 1.395(2) . ?
C9 C14 1.524(3) . ?
C10 C11 1.377(3) . ?
C11 C12 1.381(3) . ?
C12 C13 1.393(2) . ?
C13 C17 1.528(2) . ?
C14 C16 1.532(3) . ?
C14 C15 1.537(3) . ?
C17 C18 1.535(3) . ?
C17 C19 1.537(3) . ?
C20 C25 1.409(2) . ?
C20 C21 1.410(2) . ?
C21 C22 1.394(2) . ?
C21 C26 1.521(2) . ?
C22 C23 1.380(2) . ?
C23 C24 1.381(3) . ?
C24 C25 1.398(2) . ?
C25 C29 1.528(2) . ?
C26 C28 1.531(3) . ?
C26 C27 1.533(2) . ?
C29 C31 1.534(3) . ?
C29 C30 1.535(2) . ?
C34 C35 1.386(3) . ?
C34 C39 1.390(3) . ?
C34 S1B 1.725(7) . ?
C34 S1 1.804(2) . ?
C35 C36 1.389(3) . ?
C36 C37 1.382(3) . ?
C37 C38 1.385(3) . ?
C38 C39 1.388(3) . ?
S1 Si 2.1610(19) . ?
C32 N3 1.452(4) . ?
C33 N3 1.466(3) . ?
N3 Si 1.702(2) . ?
Si N4 1.735(2) . ?
N4 C40 1.249(4) . ?
S1B SiB 2.141(10) . ?
C32B N3B 1.470(10) . ?
C33B N3B 1.478(13) . ?
N3B SiB 1.668(9) . ?
SiB N4B 1.713(12) . ?
N4B C40B 1.219(16) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C8 119.49(13) . . ?
C1 N1 Si 113.31(11) . . ?
C8 N1 Si 126.34(11) . . ?
C1 N1 SiB 120.4(2) . . ?
C8 N1 SiB 117.3(2) . . ?
C1 N2 C20 123.32(13) . . ?
N2 C1 N1 115.82(14) . . ?
N2 C1 C2 125.05(14) . . ?
N1 C1 C2 119.12(13) . . ?
C7 C2 C3 119.33(17) . . ?
C7 C2 C1 119.92(16) . . ?
C3 C2 C1 120.72(16) . . ?
C4 C3 C2 120.10(19) . . ?
C5 C4 C3 120.3(2) . . ?
C4 C5 C6 120.07(19) . . ?
C5 C6 C7 120.2(2) . . ?
C2 C7 C6 119.98(19) . . ?
C13 C8 C9 120.79(14) . . ?
C13 C8 N1 119.63(14) . . ?
C9 C8 N1 119.58(14) . . ?
C10 C9 C8 118.05(16) . . ?
C10 C9 C14 118.06(15) . . ?
C8 C9 C14 123.89(15) . . ?
C11 C10 C9 121.80(16) . . ?
C10 C11 C12 119.43(16) . . ?
C11 C12 C13 121.74(17) . . ?
C12 C13 C8 118.14(15) . . ?
C12 C13 C17 118.52(15) . . ?
C8 C13 C17 123.33(14) . . ?
C9 C14 C16 110.25(17) . . ?
C9 C14 C15 112.79(17) . . ?
C16 C14 C15 108.35(16) . . ?
C13 C17 C18 112.68(15) . . ?
C13 C17 C19 110.55(15) . . ?
C18 C17 C19 108.91(15) . . ?
C25 C20 C21 119.96(14) . . ?
C25 C20 N2 121.42(14) . . ?
C21 C20 N2 118.27(14) . . ?
C22 C21 C20 119.00(15) . . ?
C22 C21 C26 119.21(14) . . ?
C20 C21 C26 121.76(14) . . ?
C23 C22 C21 121.64(16) . . ?
C22 C23 C24 118.91(15) . . ?
C23 C24 C25 122.04(16) . . ?
C24 C25 C20 118.44(15) . . ?
C24 C25 C29 118.24(15) . . ?
C20 C25 C29 123.28(15) . . ?
C21 C26 C28 109.39(14) . . ?
C21 C26 C27 112.05(14) . . ?
C28 C26 C27 111.36(15) . . ?
C25 C29 C31 110.19(14) . . ?
C25 C29 C30 111.21(15) . . ?
C31 C29 C30 109.95(15) . . ?
C35 C34 C39 118.98(17) . . ?
C35 C34 S1B 130.9(3) . . ?
C39 C34 S1B 110.1(2) . . ?
C35 C34 S1 119.73(14) . . ?
C39 C34 S1 121.05(15) . . ?
C34 C35 C36 120.52(18) . . ?
C37 C36 C35 120.11(18) . . ?
C36 C37 C38 119.84(18) . . ?
C37 C38 C39 119.93(19) . . ?
C38 C39 C34 120.59(19) . . ?
C34 S1 Si 103.28(9) . . ?
C32 N3 C33 111.1(3) . . ?
C32 N3 Si 123.4(2) . . ?
C33 N3 Si 122.61(17) . . ?
N3 Si N4 104.23(11) . . ?
N3 Si N1 110.12(11) . . ?
N4 Si N1 108.19(10) . . ?
N3 Si S1 110.86(9) . . ?
N4 Si S1 115.78(10) . . ?
N1 Si S1 107.58(9) . . ?
C40 N4 Si 124.2(2) . . ?
C34 S1B SiB 97.1(4) . . ?
C32B N3B C33B 109.2(10) . . ?
C32B N3B SiB 123.4(7) . . ?
C33B N3B SiB 127.0(9) . . ?
N3B SiB N4B 106.0(6) . . ?
N3B SiB N1 114.6(5) . . ?
N4B SiB N1 105.4(5) . . ?
N3B SiB S1B 110.0(5) . . ?
N4B SiB S1B 113.8(5) . . ?
N1 SiB S1B 107.2(4) . . ?
C40B N4B SiB 130.1(18) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C20 N2 C1 N1 -170.75(13) . . . . ?
C20 N2 C1 C2 8.2(2) . . . . ?
C8 N1 C1 N2 -163.99(13) . . . . ?
Si N1 C1 N2 6.07(17) . . . . ?
SiB N1 C1 N2 -3.6(3) . . . . ?
C8 N1 C1 C2 17.0(2) . . . . ?
Si N1 C1 C2 -172.96(12) . . . . ?
SiB N1 C1 C2 177.4(3) . . . . ?
N2 C1 C2 C7 53.0(2) . . . . ?
N1 C1 C2 C7 -128.05(16) . . . . ?
N2 C1 C2 C3 -124.92(18) . . . . ?
N1 C1 C2 C3 54.0(2) . . . . ?
C7 C2 C3 C4 -0.8(2) . . . . ?
C1 C2 C3 C4 177.10(15) . . . . ?
C2 C3 C4 C5 1.3(3) . . . . ?
C3 C4 C5 C6 -0.2(3) . . . . ?
C4 C5 C6 C7 -1.4(3) . . . . ?
C3 C2 C7 C6 -0.7(2) . . . . ?
C1 C2 C7 C6 -178.70(15) . . . . ?
C5 C6 C7 C2 1.9(3) . . . . ?
C1 N1 C8 C13 67.84(19) . . . . ?
Si N1 C8 C13 -100.81(16) . . . . ?
SiB N1 C8 C13 -93.1(3) . . . . ?
C1 N1 C8 C9 -111.85(16) . . . . ?
Si N1 C8 C9 79.49(18) . . . . ?
SiB N1 C8 C9 87.2(3) . . . . ?
C13 C8 C9 C10 -1.6(2) . . . . ?
N1 C8 C9 C10 178.13(14) . . . . ?
C13 C8 C9 C14 177.82(16) . . . . ?
N1 C8 C9 C14 -2.5(2) . . . . ?
C8 C9 C10 C11 -0.2(2) . . . . ?
C14 C9 C10 C11 -179.62(16) . . . . ?
C9 C10 C11 C12 1.4(3) . . . . ?
C10 C11 C12 C13 -0.8(3) . . . . ?
C11 C12 C13 C8 -1.0(2) . . . . ?
C11 C12 C13 C17 177.99(15) . . . . ?
C9 C8 C13 C12 2.1(2) . . . . ?
N1 C8 C13 C12 -177.57(14) . . . . ?
C9 C8 C13 C17 -176.77(14) . . . . ?
N1 C8 C13 C17 3.5(2) . . . . ?
C10 C9 C14 C16 66.8(2) . . . . ?
C8 C9 C14 C16 -112.61(19) . . . . ?
C10 C9 C14 C15 -54.5(2) . . . . ?
C8 C9 C14 C15 126.13(18) . . . . ?
C12 C13 C17 C18 49.7(2) . . . . ?
C8 C13 C17 C18 -131.44(17) . . . . ?
C12 C13 C17 C19 -72.4(2) . . . . ?
C8 C13 C17 C19 106.44(18) . . . . ?
C1 N2 C20 C25 72.2(2) . . . . ?
C1 N2 C20 C21 -114.62(17) . . . . ?
C25 C20 C21 C22 -1.2(2) . . . . ?
N2 C20 C21 C22 -174.52(14) . . . . ?
C25 C20 C21 C26 176.48(14) . . . . ?
N2 C20 C21 C26 3.2(2) . . . . ?
C20 C21 C22 C23 0.4(2) . . . . ?
C26 C21 C22 C23 -177.40(15) . . . . ?
C21 C22 C23 C24 0.1(2) . . . . ?
C22 C23 C24 C25 0.3(3) . . . . ?
C23 C24 C25 C20 -1.1(2) . . . . ?
C23 C24 C25 C29 176.70(15) . . . . ?
C21 C20 C25 C24 1.6(2) . . . . ?
N2 C20 C25 C24 174.66(14) . . . . ?
C21 C20 C25 C29 -176.12(15) . . . . ?
N2 C20 C25 C29 -3.1(2) . . . . ?
C22 C21 C26 C28 71.60(19) . . . . ?
C20 C21 C26 C28 -106.12(17) . . . . ?
C22 C21 C26 C27 -52.4(2) . . . . ?
C20 C21 C26 C27 129.89(17) . . . . ?
C24 C25 C29 C31 -62.6(2) . . . . ?
C20 C25 C29 C31 115.08(18) . . . . ?
C24 C25 C29 C30 59.5(2) . . . . ?
C20 C25 C29 C30 -122.73(17) . . . . ?
C39 C34 C35 C36 -0.8(3) . . . . ?
S1B C34 C35 C36 -179.1(4) . . . . ?
S1 C34 C35 C36 -175.16(14) . . . . ?
C34 C35 C36 C37 1.3(3) . . . . ?
C35 C36 C37 C38 -0.6(3) . . . . ?
C36 C37 C38 C39 -0.7(3) . . . . ?
C37 C38 C39 C34 1.3(3) . . . . ?
C35 C34 C39 C38 -0.5(3) . . . . ?
S1B C34 C39 C38 178.1(3) . . . . ?
S1 C34 C39 C38 173.79(17) . . . . ?
C35 C34 S1 Si -63.10(15) . . . . ?
C39 C34 S1 Si 122.62(15) . . . . ?
S1B C34 S1 Si 102.0(14) . . . . ?
C32 N3 Si N4 179.5(3) . . . . ?
C33 N3 Si N4 -21.6(2) . . . . ?
C32 N3 Si N1 63.6(3) . . . . ?
C33 N3 Si N1 -137.43(17) . . . . ?
C32 N3 Si S1 -55.3(3) . . . . ?
C33 N3 Si S1 103.63(18) . . . . ?
C1 N1 Si N3 177.54(12) . . . . ?
C8 N1 Si N3 -13.21(17) . . . . ?
SiB N1 Si N3 -51.1(14) . . . . ?
C1 N1 Si N4 64.22(14) . . . . ?
C8 N1 Si N4 -126.53(14) . . . . ?
SiB N1 Si N4 -164.4(15) . . . . ?
C1 N1 Si S1 -61.54(12) . . . . ?
C8 N1 Si S1 107.71(13) . . . . ?
SiB N1 Si S1 69.9(14) . . . . ?
N3 Si N4 C40 120.5(3) . . . . ?
N1 Si N4 C40 -122.3(3) . . . . ?
S1 Si N4 C40 -1.5(3) . . . . ?
C35 C34 S1B SiB -56.7(4) . . . . ?
C39 C34 S1B SiB 124.8(3) . . . . ?
S1 C34 S1B SiB -73.9(14) . . . . ?
C32B N3B SiB N4B -14.8(12) . . . . ?
C33B N3B SiB N4B 156.7(12) . . . . ?
C32B N3B SiB N1 100.9(10) . . . . ?
C33B N3B SiB N1 -87.6(13) . . . . ?
C32B N3B SiB S1B -138.2(9) . . . . ?
C33B N3B SiB S1B 33.3(13) . . . . ?
C1 N1 SiB N3B 68.6(5) . . . . ?
C8 N1 SiB N3B -130.6(4) . . . . ?
Si N1 SiB N3B 15.6(11) . . . . ?
C1 N1 SiB N4B -175.3(5) . . . . ?
C8 N1 SiB N4B -14.5(6) . . . . ?
Si N1 SiB N4B 131.7(17) . . . . ?
C1 N1 SiB S1B -53.8(3) . . . . ?
C8 N1 SiB S1B 107.0(3) . . . . ?
Si N1 SiB S1B -106.8(15) . . . . ?
N3B SiB N4B C40B -135(2) . . . . ?
N1 SiB N4B C40B 103(2) . . . . ?
S1B SiB N4B C40B -14(2) . . . . ?

_refine_diff_density_max         0.341
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.045

_shelxl_version_number           2013-4

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

data_KOB46B
_database_code_depnum_ccdc_archive 'CCDC 1061432'
_audit_update_record             
;
2015-04-23 deposited with the CCDC.
2015-06-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H45 Fe N3 O4 Si'
_chemical_formula_sum            'C37 H45 Fe N3 O4 Si'
_chemical_formula_weight         679.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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                   10.2963(19)
_cell_length_b                   10.5302(19)
_cell_length_c                   16.804(3)
_cell_angle_alpha                93.254(17)
_cell_angle_beta                 93.943(17)
_cell_angle_gamma                104.57(2)
_cell_volume                     1753.9(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6610
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      27.81

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_F_000             720
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.595
_exptl_crystal_size_mid          0.472
_exptl_crystal_size_min          0.345
_exptl_absorpt_coefficient_mu    0.507
_shelx_estimated_absorpt_T_min   0.753
_shelx_estimated_absorpt_T_max   0.845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6842
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'Sadabs 2008/1 (Bruker 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23098
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.218
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6894
_reflns_number_gt                5805
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP & POV-Ray'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0336P)²+1.0409P] 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         6894
_refine_ls_number_parameters     425
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0338
_refine_ls_wR_factor_ref         0.0892
_refine_ls_wR_factor_gt          0.0781
_refine_ls_goodness_of_fit_ref   1.054
_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
Fe Fe 0.35858(3) -0.11999(3) 0.23095(2) 0.01290(8) Uani 1 1 d . . . . .
Si Si 0.32642(5) 0.06312(5) 0.29426(3) 0.01012(12) Uani 1 1 d . . . . .
O1 O 0.10815(15) -0.17663(15) 0.12547(9) 0.0258(3) Uani 1 1 d . . . . .
O2 O 0.34689(16) -0.23101(14) 0.38742(9) 0.0261(3) Uani 1 1 d . . . . .
O3 O 0.43599(16) -0.34092(14) 0.14982(9) 0.0256(3) Uani 1 1 d . . . . .
O4 O 0.60741(15) 0.06478(14) 0.19311(9) 0.0251(3) Uani 1 1 d . . . . .
N1 N 0.33094(15) 0.20043(14) 0.22734(9) 0.0094(3) Uani 1 1 d . . . . .
N2 N 0.16848(15) 0.11817(14) 0.29778(9) 0.0098(3) Uani 1 1 d . . . . .
N3 N 0.41500(15) 0.11111(15) 0.38538(9) 0.0135(3) Uani 1 1 d . . . . .
C1 C 0.20545(18) 0.20316(17) 0.24071(11) 0.0099(4) Uani 1 1 d . . . . .
C2 C 0.12080(18) 0.27578(18) 0.19854(11) 0.0112(4) Uani 1 1 d . . . . .
C3 C 0.1778(2) 0.40065(19) 0.17399(12) 0.0157(4) Uani 1 1 d . . . . .
H3 H 0.2716 0.4395 0.1849 0.019 Uiso 1 1 calc R U . . .
C4 C 0.0970(2) 0.4676(2) 0.13370(12) 0.0198(4) Uani 1 1 d . . . . .
H4 H 0.1353 0.5529 0.1174 0.024 Uiso 1 1 calc R U . . .
C5 C -0.0403(2) 0.4101(2) 0.11709(12) 0.0202(4) Uani 1 1 d . . . . .
H5 H -0.0951 0.4563 0.0892 0.024 Uiso 1 1 calc R U . . .
C6 C -0.0976(2) 0.2858(2) 0.14090(12) 0.0167(4) Uani 1 1 d . . . . .
H6 H -0.1912 0.2468 0.1291 0.020 Uiso 1 1 calc R U . . .
C7 C -0.01738(19) 0.21871(19) 0.18222(11) 0.0135(4) Uani 1 1 d . . . . .
H7 H -0.0564 0.1341 0.1993 0.016 Uiso 1 1 calc R U . . .
C8 C 0.41265(18) 0.26530(18) 0.16804(11) 0.0110(4) Uani 1 1 d . . . . .
C9 C 0.37819(19) 0.23213(19) 0.08591(11) 0.0147(4) Uani 1 1 d . . . . .
C10 C 0.4625(2) 0.3024(2) 0.03312(12) 0.0194(4) Uani 1 1 d . . . . .
H10 H 0.4410 0.2827 -0.0228 0.023 Uiso 1 1 calc R U . . .
C11 C 0.5767(2) 0.4002(2) 0.06036(12) 0.0206(5) Uani 1 1 d . . . . .
H11 H 0.6321 0.4472 0.0232 0.025 Uiso 1 1 calc R U . . .
C12 C 0.61039(19) 0.42960(19) 0.14174(12) 0.0171(4) Uani 1 1 d . . . . .
H12 H 0.6892 0.4965 0.1600 0.021 Uiso 1 1 calc R U . . .
C13 C 0.52995(18) 0.36220(18) 0.19723(11) 0.0131(4) Uani 1 1 d . . . . .
C14 C 0.2563(2) 0.1232(2) 0.05137(12) 0.0181(4) Uani 1 1 d . . . . .
H14 H 0.2073 0.0834 0.0969 0.022 Uiso 1 1 calc R U . . .
C15 C 0.1582(2) 0.1758(2) -0.00274(13) 0.0269(5) Uani 1 1 d . . . . .
H15A H 0.2044 0.2154 -0.0478 0.040 Uiso 1 1 calc R U . . .
H15B H 0.1267 0.2423 0.0281 0.040 Uiso 1 1 calc R U . . .
H15C H 0.0811 0.1031 -0.0230 0.040 Uiso 1 1 calc R U . . .
C16 C 0.3016(2) 0.0145(2) 0.00423(13) 0.0269(5) Uani 1 1 d . . . . .
H16A H 0.2227 -0.0577 -0.0141 0.040 Uiso 1 1 calc R U . . .
H16B H 0.3641 -0.0186 0.0389 0.040 Uiso 1 1 calc R U . . .
H16C H 0.3467 0.0507 -0.0421 0.040 Uiso 1 1 calc R U . . .
C17 C 0.56854(19) 0.39478(19) 0.28653(11) 0.0151(4) Uani 1 1 d . . . . .
H17 H 0.5165 0.3198 0.3148 0.018 Uiso 1 1 calc R U . . .
C18 C 0.5289(2) 0.5192(2) 0.31674(13) 0.0244(5) Uani 1 1 d . . . . .
H18A H 0.5762 0.5942 0.2889 0.037 Uiso 1 1 calc R U . . .
H18B H 0.5538 0.5365 0.3744 0.037 Uiso 1 1 calc R U . . .
H18C H 0.4314 0.5060 0.3062 0.037 Uiso 1 1 calc R U . . .
C19 C 0.7184(2) 0.4075(2) 0.30828(13) 0.0227(5) Uani 1 1 d . . . . .
H19A H 0.7420 0.3285 0.2869 0.034 Uiso 1 1 calc R U . . .
H19B H 0.7367 0.4170 0.3666 0.034 Uiso 1 1 calc R U . . .
H19C H 0.7722 0.4850 0.2853 0.034 Uiso 1 1 calc R U . . .
C20 C 0.05905(18) 0.11320(18) 0.34815(11) 0.0110(4) Uani 1 1 d . . . . .
C21 C 0.05325(18) 0.22522(18) 0.39801(11) 0.0120(4) Uani 1 1 d . . . . .
C22 C -0.04594(19) 0.2085(2) 0.45175(11) 0.0158(4) Uani 1 1 d . . . . .
H22 H -0.0522 0.2823 0.4851 0.019 Uiso 1 1 calc R U . . .
C23 C -0.13548(19) 0.0879(2) 0.45791(12) 0.0176(4) Uani 1 1 d . . . . .
H23 H -0.1985 0.0780 0.4973 0.021 Uiso 1 1 calc R U . . .
C24 C -0.13234(19) -0.0184(2) 0.40613(12) 0.0161(4) Uani 1 1 d . . . . .
H24 H -0.1958 -0.1005 0.4092 0.019 Uiso 1 1 calc R U . . .
C25 C -0.03796(18) -0.00708(18) 0.34968(11) 0.0126(4) Uani 1 1 d . . . . .
C26 C 0.14558(19) 0.36319(18) 0.39539(11) 0.0138(4) Uani 1 1 d . . . . .
H26 H 0.2200 0.3568 0.3614 0.017 Uiso 1 1 calc R U . . .
C27 C 0.0686(2) 0.45553(19) 0.35779(13) 0.0190(4) Uani 1 1 d . . . . .
H27A H 0.1319 0.5398 0.3504 0.028 Uiso 1 1 calc R U . . .
H27B H 0.0012 0.4704 0.3932 0.028 Uiso 1 1 calc R U . . .
H27C H 0.0235 0.4153 0.3058 0.028 Uiso 1 1 calc R U . . .
C28 C 0.2091(2) 0.4269(2) 0.47867(12) 0.0200(4) Uani 1 1 d . . . . .
H28A H 0.2774 0.5085 0.4725 0.030 Uiso 1 1 calc R U . . .
H28B H 0.2511 0.3659 0.5062 0.030 Uiso 1 1 calc R U . . .
H28C H 0.1389 0.4467 0.5101 0.030 Uiso 1 1 calc R U . . .
C29 C -0.04561(19) -0.12308(18) 0.28939(12) 0.0151(4) Uani 1 1 d . . . . .
H29 H 0.0245 -0.0935 0.2513 0.018 Uiso 1 1 calc R U . . .
C30 C -0.1827(2) -0.1640(2) 0.24056(13) 0.0237(5) Uani 1 1 d . . . . .
H30A H -0.1985 -0.0887 0.2133 0.036 Uiso 1 1 calc R U . . .
H30B H -0.2537 -0.1933 0.2764 0.036 Uiso 1 1 calc R U . . .
H30C H -0.1836 -0.2360 0.2008 0.036 Uiso 1 1 calc R U . . .
C31 C -0.0153(2) -0.2404(2) 0.32883(13) 0.0223(5) Uani 1 1 d . . . . .
H31A H -0.0140 -0.3095 0.2875 0.033 Uiso 1 1 calc R U . . .
H31B H -0.0851 -0.2745 0.3646 0.033 Uiso 1 1 calc R U . . .
H31C H 0.0726 -0.2127 0.3597 0.033 Uiso 1 1 calc R U . . .
C32 C 0.55034(19) 0.0924(2) 0.40309(12) 0.0163(4) Uani 1 1 d . . . . .
H32A H 0.5650 0.0248 0.3647 0.024 Uiso 1 1 calc R U . . .
H32B H 0.5584 0.0643 0.4574 0.024 Uiso 1 1 calc R U . . .
H32C H 0.6178 0.1754 0.3990 0.024 Uiso 1 1 calc R U . . .
C33 C 0.3855(2) 0.2030(2) 0.44595(12) 0.0166(4) Uani 1 1 d . . . . .
H33A H 0.4387 0.2924 0.4392 0.025 Uiso 1 1 calc R U . . .
H33B H 0.4087 0.1782 0.4994 0.025 Uiso 1 1 calc R U . . .
H33C H 0.2894 0.2000 0.4398 0.025 Uiso 1 1 calc R U . . .
C34 C 0.2058(2) -0.14959(19) 0.16778(12) 0.0179(4) Uani 1 1 d . . . . .
C35 C 0.3499(2) -0.18676(19) 0.32599(13) 0.0179(4) Uani 1 1 d . . . . .
C36 C 0.4055(2) -0.2555(2) 0.18221(12) 0.0169(4) Uani 1 1 d . . . . .
C37 C 0.5076(2) -0.00640(19) 0.20732(12) 0.0178(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe C37 1.777(2) . ?
Fe C35 1.780(2) . ?
Fe C34 1.785(2) . ?
Fe C36 1.791(2) . ?
Fe Si 2.2574(7) . ?
Si N3 1.7087(17) . ?
Si N2 1.8622(16) . ?
Si N1 1.8750(16) . ?
Si C1 2.3360(19) . ?
O1 C34 1.154(2) . ?
O2 C35 1.156(2) . ?
O3 C36 1.146(2) . ?
O4 C37 1.158(2) . ?
N1 C1 1.334(2) . ?
N1 C8 1.439(2) . ?
N2 C1 1.357(2) . ?
N2 C20 1.447(2) . ?
N3 C33 1.464(2) . ?
N3 C32 1.469(2) . ?
C1 C2 1.469(3) . ?
C2 C3 1.396(3) . ?
C2 C7 1.399(3) . ?
C3 C4 1.386(3) . ?
C4 C5 1.392(3) . ?
C5 C6 1.387(3) . ?
C6 C7 1.391(3) . ?
C8 C9 1.403(3) . ?
C8 C13 1.408(3) . ?
C9 C10 1.395(3) . ?
C9 C14 1.525(3) . ?
C10 C11 1.384(3) . ?
C11 C12 1.385(3) . ?
C12 C13 1.395(3) . ?
C13 C17 1.523(3) . ?
C14 C15 1.538(3) . ?
C14 C16 1.540(3) . ?
C17 C19 1.531(3) . ?
C17 C18 1.537(3) . ?
C20 C25 1.405(3) . ?
C20 C21 1.424(3) . ?
C21 C22 1.394(3) . ?
C21 C26 1.528(3) . ?
C22 C23 1.383(3) . ?
C23 C24 1.386(3) . ?
C24 C25 1.393(3) . ?
C25 C29 1.525(3) . ?
C26 C27 1.537(3) . ?
C26 C28 1.543(3) . ?
C29 C31 1.523(3) . ?
C29 C30 1.532(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C37 Fe C35 120.60(9) . . ?
C37 Fe C34 121.10(9) . . ?
C35 Fe C34 117.52(9) . . ?
C37 Fe C36 92.00(9) . . ?
C35 Fe C36 94.62(9) . . ?
C34 Fe C36 92.28(9) . . ?
C37 Fe Si 81.68(7) . . ?
C35 Fe Si 86.16(7) . . ?
C34 Fe Si 93.50(7) . . ?
C36 Fe Si 173.03(7) . . ?
N3 Si N2 106.63(8) . . ?
N3 Si N1 114.22(8) . . ?
N2 Si N1 70.12(7) . . ?
N3 Si Fe 115.67(6) . . ?
N2 Si Fe 128.82(5) . . ?
N1 Si Fe 113.40(5) . . ?
N3 Si C1 117.83(7) . . ?
N2 Si C1 35.50(6) . . ?
N1 Si C1 34.79(6) . . ?
Fe Si C1 126.08(5) . . ?
C1 N1 C8 128.09(15) . . ?
C1 N1 Si 91.87(11) . . ?
C8 N1 Si 138.69(12) . . ?
C1 N2 C20 126.59(15) . . ?
C1 N2 Si 91.67(11) . . ?
C20 N2 Si 140.05(12) . . ?
C33 N3 C32 110.75(15) . . ?
C33 N3 Si 125.20(13) . . ?
C32 N3 Si 122.22(13) . . ?
N1 C1 N2 105.85(15) . . ?
N1 C1 C2 127.25(16) . . ?
N2 C1 C2 126.78(16) . . ?
N1 C1 Si 53.34(9) . . ?
N2 C1 Si 52.83(9) . . ?
C2 C1 Si 171.90(13) . . ?
C3 C2 C7 119.95(17) . . ?
C3 C2 C1 120.34(17) . . ?
C7 C2 C1 119.71(17) . . ?
C4 C3 C2 119.74(18) . . ?
C3 C4 C5 120.13(19) . . ?
C6 C5 C4 120.51(18) . . ?
C5 C6 C7 119.67(18) . . ?
C6 C7 C2 120.00(18) . . ?
C9 C8 C13 122.06(17) . . ?
C9 C8 N1 121.75(16) . . ?
C13 C8 N1 116.18(16) . . ?
C10 C9 C8 117.42(18) . . ?
C10 C9 C14 118.48(18) . . ?
C8 C9 C14 124.10(17) . . ?
C11 C10 C9 121.55(19) . . ?
C10 C11 C12 120.10(18) . . ?
C11 C12 C13 120.80(19) . . ?
C12 C13 C8 118.03(18) . . ?
C12 C13 C17 120.30(17) . . ?
C8 C13 C17 121.66(16) . . ?
C9 C14 C15 112.14(17) . . ?
C9 C14 C16 110.49(17) . . ?
C15 C14 C16 109.73(17) . . ?
C13 C17 C19 112.00(16) . . ?
C13 C17 C18 111.56(16) . . ?
C19 C17 C18 110.87(16) . . ?
C25 C20 C21 120.63(17) . . ?
C25 C20 N2 118.25(16) . . ?
C21 C20 N2 121.04(16) . . ?
C22 C21 C20 117.66(17) . . ?
C22 C21 C26 117.62(17) . . ?
C20 C21 C26 124.71(17) . . ?
C23 C22 C21 121.99(18) . . ?
C22 C23 C24 119.39(18) . . ?
C23 C24 C25 121.27(18) . . ?
C24 C25 C20 118.77(18) . . ?
C24 C25 C29 119.45(17) . . ?
C20 C25 C29 121.75(17) . . ?
C21 C26 C27 110.89(15) . . ?
C21 C26 C28 113.26(16) . . ?
C27 C26 C28 107.80(16) . . ?
C31 C29 C25 112.39(16) . . ?
C31 C29 C30 110.48(16) . . ?
C25 C29 C30 111.12(16) . . ?
O1 C34 Fe 175.55(18) . . ?
O2 C35 Fe 178.41(18) . . ?
O3 C36 Fe 178.76(18) . . ?
O4 C37 Fe 177.54(18) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 Si N1 C1 -104.46(12) . . . . ?
N2 Si N1 C1 -4.62(10) . . . . ?
Fe Si N1 C1 120.12(10) . . . . ?
N3 Si N1 C8 89.07(19) . . . . ?
N2 Si N1 C8 -171.1(2) . . . . ?
Fe Si N1 C8 -46.34(19) . . . . ?
C1 Si N1 C8 -166.5(2) . . . . ?
N3 Si N2 C1 114.85(11) . . . . ?
N1 Si N2 C1 4.54(10) . . . . ?
Fe Si N2 C1 -100.01(11) . . . . ?
N3 Si N2 C20 -49.6(2) . . . . ?
N1 Si N2 C20 -160.0(2) . . . . ?
Fe Si N2 C20 95.51(19) . . . . ?
C1 Si N2 C20 -164.5(2) . . . . ?
N2 Si N3 C33 -12.60(17) . . . . ?
N1 Si N3 C33 62.64(17) . . . . ?
Fe Si N3 C33 -162.99(13) . . . . ?
C1 Si N3 C33 23.98(18) . . . . ?
N2 Si N3 C32 -175.76(14) . . . . ?
N1 Si N3 C32 -100.52(15) . . . . ?
Fe Si N3 C32 33.85(16) . . . . ?
C1 Si N3 C32 -139.19(14) . . . . ?
C8 N1 C1 N2 174.88(16) . . . . ?
Si N1 C1 N2 6.20(14) . . . . ?
C8 N1 C1 C2 -1.2(3) . . . . ?
Si N1 C1 C2 -169.89(16) . . . . ?
C8 N1 C1 Si 168.7(2) . . . . ?
C20 N2 C1 N1 161.41(16) . . . . ?
Si N2 C1 N1 -6.24(14) . . . . ?
C20 N2 C1 C2 -22.5(3) . . . . ?
Si N2 C1 C2 169.87(16) . . . . ?
C20 N2 C1 Si 167.7(2) . . . . ?
N1 C1 C2 C3 -37.1(3) . . . . ?
N2 C1 C2 C3 147.64(19) . . . . ?
N1 C1 C2 C7 142.26(19) . . . . ?
N2 C1 C2 C7 -33.0(3) . . . . ?
C7 C2 C3 C4 0.2(3) . . . . ?
C1 C2 C3 C4 179.47(18) . . . . ?
C2 C3 C4 C5 -0.6(3) . . . . ?
C3 C4 C5 C6 0.3(3) . . . . ?
C4 C5 C6 C7 0.5(3) . . . . ?
C5 C6 C7 C2 -0.9(3) . . . . ?
C3 C2 C7 C6 0.6(3) . . . . ?
C1 C2 C7 C6 -178.71(17) . . . . ?
C1 N1 C8 C9 -65.2(3) . . . . ?
Si N1 C8 C9 97.5(2) . . . . ?
C1 N1 C8 C13 115.7(2) . . . . ?
Si N1 C8 C13 -81.6(2) . . . . ?
C13 C8 C9 C10 -2.2(3) . . . . ?
N1 C8 C9 C10 178.79(17) . . . . ?
C13 C8 C9 C14 176.73(18) . . . . ?
N1 C8 C9 C14 -2.2(3) . . . . ?
C8 C9 C10 C11 0.7(3) . . . . ?
C14 C9 C10 C11 -178.30(18) . . . . ?
C9 C10 C11 C12 0.5(3) . . . . ?
C10 C11 C12 C13 -0.4(3) . . . . ?
C11 C12 C13 C8 -1.1(3) . . . . ?
C11 C12 C13 C17 179.58(18) . . . . ?
C9 C8 C13 C12 2.4(3) . . . . ?
N1 C8 C13 C12 -178.55(16) . . . . ?
C9 C8 C13 C17 -178.24(17) . . . . ?
N1 C8 C13 C17 0.8(3) . . . . ?
C10 C9 C14 C15 -60.8(2) . . . . ?
C8 C9 C14 C15 120.2(2) . . . . ?
C10 C9 C14 C16 61.9(2) . . . . ?
C8 C9 C14 C16 -117.0(2) . . . . ?
C12 C13 C17 C19 -45.3(2) . . . . ?
C8 C13 C17 C19 135.38(19) . . . . ?
C12 C13 C17 C18 79.6(2) . . . . ?
C8 C13 C17 C18 -99.7(2) . . . . ?
C1 N2 C20 C25 125.93(19) . . . . ?
Si N2 C20 C25 -73.5(2) . . . . ?
C1 N2 C20 C21 -57.2(2) . . . . ?
Si N2 C20 C21 103.3(2) . . . . ?
C25 C20 C21 C22 4.3(3) . . . . ?
N2 C20 C21 C22 -172.50(16) . . . . ?
C25 C20 C21 C26 -174.10(17) . . . . ?
N2 C20 C21 C26 9.1(3) . . . . ?
C20 C21 C22 C23 0.7(3) . . . . ?
C26 C21 C22 C23 179.19(17) . . . . ?
C21 C22 C23 C24 -3.9(3) . . . . ?
C22 C23 C24 C25 2.1(3) . . . . ?
C23 C24 C25 C20 2.8(3) . . . . ?
C23 C24 C25 C29 -174.90(17) . . . . ?
C21 C20 C25 C24 -6.0(3) . . . . ?
N2 C20 C25 C24 170.86(16) . . . . ?
C21 C20 C25 C29 171.66(17) . . . . ?
N2 C20 C25 C29 -11.5(3) . . . . ?
C22 C21 C26 C27 -70.7(2) . . . . ?
C20 C21 C26 C27 107.7(2) . . . . ?
C22 C21 C26 C28 50.6(2) . . . . ?
C20 C21 C26 C28 -131.00(19) . . . . ?
C24 C25 C29 C31 -66.8(2) . . . . ?
C20 C25 C29 C31 115.5(2) . . . . ?
C24 C25 C29 C30 57.5(2) . . . . ?
C20 C25 C29 C30 -120.09(19) . . . . ?

_refine_diff_density_max         0.347
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.061

_shelxl_version_number           2013-4

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

data_KOB52D
_database_code_depnum_ccdc_archive 'CCDC 1061433'
_audit_update_record             
;
2015-04-23 deposited with the CCDC.
2015-06-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H59 Li N2 O2'
_chemical_formula_sum            'C39 H59 Li N2 O2'
_chemical_formula_weight         594.82

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   15.646(6)
_cell_length_b                   13.477(6)
_cell_length_c                   35.262(14)
_cell_angle_alpha                90
_cell_angle_beta                 101.163(12)
_cell_angle_gamma                90
_cell_volume                     7295(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7912
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      24.74

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_F_000             2608
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          .35
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .25
_exptl_absorpt_coefficient_mu    0.065
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5944
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'Sababs 2008/1 (Bruker 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            63534
_diffrn_reflns_av_unetI/netI     0.0969
_diffrn_reflns_av_R_equivalents  0.0863
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_theta_min         1.594
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             14347
_reflns_number_gt                7487
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP & POV-Ray'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0670P)²+1.5766P] 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         14347
_refine_ls_number_parameters     859
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.1459
_refine_ls_R_factor_gt           0.0641
_refine_ls_wR_factor_ref         0.1676
_refine_ls_wR_factor_gt          0.1361
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Li1 Li 0.1174(3) 0.3597(3) 0.37990(13) 0.0260(11) Uani 1 1 d . . . . .
O1 O 0.05127(11) 0.29491(13) 0.41484(5) 0.0274(5) Uani 1 1 d . . . . .
O2 O 0.15333(12) 0.25295(13) 0.34704(5) 0.0323(5) Uani 1 1 d . . . . .
N1 N 0.05387(12) 0.48453(15) 0.35859(6) 0.0162(5) Uani 1 1 d . . . . .
N2 N 0.19518(12) 0.48281(15) 0.38728(6) 0.0160(5) Uani 1 1 d . . . . .
C1 C 0.12576(15) 0.53687(18) 0.37163(7) 0.0161(6) Uani 1 1 d . . . . .
C2 C 0.12813(15) 0.64791(18) 0.36874(7) 0.0165(6) Uani 1 1 d . . . . .
C3 C 0.07955(16) 0.69706(19) 0.33702(7) 0.0208(6) Uani 1 1 d . . . . .
H3 H 0.0466 0.6595 0.3165 0.025 Uiso 1 1 calc R U . . .
C4 C 0.07837(16) 0.7998(2) 0.33487(8) 0.0246(6) Uani 1 1 d . . . . .
H4 H 0.0442 0.8320 0.3131 0.029 Uiso 1 1 calc R U . . .
C5 C 0.12712(16) 0.8560(2) 0.36448(8) 0.0256(7) Uani 1 1 d . . . . .
H5 H 0.1267 0.9264 0.3630 0.031 Uiso 1 1 calc R U . . .
C6 C 0.17611(16) 0.80855(19) 0.39603(8) 0.0234(6) Uani 1 1 d . . . . .
H6 H 0.2095 0.8464 0.4164 0.028 Uiso 1 1 calc R U . . .
C7 C 0.17680(15) 0.70611(18) 0.39812(7) 0.0192(6) Uani 1 1 d . . . . .
H7 H 0.2110 0.6745 0.4200 0.023 Uiso 1 1 calc R U . . .
C8 C -0.02984(15) 0.52525(18) 0.34821(7) 0.0177(6) Uani 1 1 d . . . . .
C9 C -0.06855(15) 0.58661(19) 0.37267(7) 0.0193(6) Uani 1 1 d . . . . .
C10 C -0.15051(16) 0.6270(2) 0.35852(8) 0.0257(6) Uani 1 1 d . . . . .
H10 H -0.1756 0.6707 0.3745 0.031 Uiso 1 1 calc R U . . .
C11 C -0.19594(17) 0.6053(2) 0.32199(8) 0.0299(7) Uani 1 1 d . . . . .
H11 H -0.2504 0.6361 0.3124 0.036 Uiso 1 1 calc R U . . .
C12 C -0.16152(16) 0.5383(2) 0.29954(8) 0.0288(7) Uani 1 1 d . . . . .
H12 H -0.1944 0.5202 0.2750 0.035 Uiso 1 1 calc R U . . .
C13 C -0.07994(16) 0.4967(2) 0.31200(7) 0.0214(6) Uani 1 1 d . . . . .
C14 C -0.02654(16) 0.60647(19) 0.41442(7) 0.0198(6) Uani 1 1 d . . . . .
H14 H 0.0344 0.5802 0.4187 0.024 Uiso 1 1 calc R U . . .
C15 C -0.02172(17) 0.7170(2) 0.42426(8) 0.0307(7) Uani 1 1 d . . . . .
H15A H -0.0807 0.7429 0.4230 0.046 Uiso 1 1 calc R U . . .
H15B H 0.0062 0.7525 0.4057 0.046 Uiso 1 1 calc R U . . .
H15C H 0.0125 0.7263 0.4504 0.046 Uiso 1 1 calc R U . . .
C16 C -0.07506(17) 0.5515(2) 0.44192(7) 0.0264(7) Uani 1 1 d . . . . .
H16A H -0.0448 0.5618 0.4687 0.040 Uiso 1 1 calc R U . . .
H16B H -0.0768 0.4804 0.4360 0.040 Uiso 1 1 calc R U . . .
H16C H -0.1347 0.5770 0.4387 0.040 Uiso 1 1 calc R U . . .
C17 C -0.04313(16) 0.4223(2) 0.28709(7) 0.0250(6) Uani 1 1 d . . . . .
H17 H -0.0014 0.3791 0.3049 0.030 Uiso 1 1 calc R U . . .
C18 C 0.00909(18) 0.4746(2) 0.26031(8) 0.0364(8) Uani 1 1 d . . . . .
H18A H 0.0557 0.5142 0.2758 0.055 Uiso 1 1 calc R U . . .
H18B H -0.0297 0.5183 0.2425 0.055 Uiso 1 1 calc R U . . .
H18C H 0.0346 0.4250 0.2455 0.055 Uiso 1 1 calc R U . . .
C19 C -0.11265(18) 0.3540(2) 0.26405(8) 0.0424(9) Uani 1 1 d . . . . .
H19A H -0.1481 0.3256 0.2814 0.064 Uiso 1 1 calc R U . . .
H19B H -0.0843 0.3004 0.2523 0.064 Uiso 1 1 calc R U . . .
H19C H -0.1500 0.3923 0.2437 0.064 Uiso 1 1 calc R U . . .
C20 C 0.28013(15) 0.52169(18) 0.39761(7) 0.0164(6) Uani 1 1 d . . . . .
C21 C 0.32533(15) 0.56664(18) 0.37120(7) 0.0184(6) Uani 1 1 d . . . . .
C22 C 0.40883(16) 0.60402(19) 0.38488(7) 0.0219(6) Uani 1 1 d . . . . .
H22 H 0.4387 0.6366 0.3674 0.026 Uiso 1 1 calc R U . . .
C23 C 0.44907(16) 0.59477(19) 0.42313(8) 0.0238(6) Uani 1 1 d . . . . .
H23 H 0.5054 0.6221 0.4319 0.029 Uiso 1 1 calc R U . . .
C24 C 0.40692(16) 0.54549(19) 0.44856(8) 0.0232(6) Uani 1 1 d . . . . .
H24 H 0.4355 0.5373 0.4747 0.028 Uiso 1 1 calc R U . . .
C25 C 0.32331(15) 0.50762(18) 0.43655(7) 0.0181(6) Uani 1 1 d . . . . .
C26 C 0.28822(16) 0.57411(19) 0.32820(7) 0.0206(6) Uani 1 1 d . . . . .
H26 H 0.2264 0.5507 0.3237 0.025 Uiso 1 1 calc R U . . .
C27 C 0.28838(17) 0.6806(2) 0.31291(8) 0.0299(7) Uani 1 1 d . . . . .
H27A H 0.2582 0.7242 0.3283 0.045 Uiso 1 1 calc R U . . .
H27B H 0.2584 0.6824 0.2858 0.045 Uiso 1 1 calc R U . . .
H27C H 0.3486 0.7032 0.3149 0.045 Uiso 1 1 calc R U . . .
C28 C 0.33894(17) 0.5055(2) 0.30540(8) 0.0307(7) Uani 1 1 d . . . . .
H28A H 0.3998 0.5273 0.3092 0.046 Uiso 1 1 calc R U . . .
H28B H 0.3127 0.5085 0.2778 0.046 Uiso 1 1 calc R U . . .
H28C H 0.3366 0.4372 0.3146 0.046 Uiso 1 1 calc R U . . .
C29 C 0.27703(16) 0.4557(2) 0.46507(7) 0.0220(6) Uani 1 1 d . . . . .
H29 H 0.2387 0.4037 0.4503 0.026 Uiso 1 1 calc R U . . .
C30 C 0.21764(17) 0.5271(2) 0.48165(8) 0.0300(7) Uani 1 1 d . . . . .
H30A H 0.1894 0.4917 0.5001 0.045 Uiso 1 1 calc R U . . .
H30B H 0.1731 0.5534 0.4606 0.045 Uiso 1 1 calc R U . . .
H30C H 0.2524 0.5820 0.4948 0.045 Uiso 1 1 calc R U . . .
C31 C 0.33715(18) 0.4033(2) 0.49817(8) 0.0348(7) Uani 1 1 d . . . . .
H31A H 0.3706 0.4528 0.5153 0.052 Uiso 1 1 calc R U . . .
H31B H 0.3772 0.3599 0.4877 0.052 Uiso 1 1 calc R U . . .
H31C H 0.3023 0.3635 0.5128 0.052 Uiso 1 1 calc R U . . .
C32 C -0.02040(17) 0.2321(2) 0.39780(9) 0.0342(7) Uani 1 1 d . . . . .
H32A H -0.0266 0.1782 0.4161 0.041 Uiso 1 1 calc R U . . .
H32B H -0.0072 0.2013 0.3741 0.041 Uiso 1 1 calc R U . . .
C33 C -0.10468(18) 0.2870(2) 0.38774(9) 0.0385(8) Uani 1 1 d . . . . .
H33A H -0.1190 0.3161 0.4112 0.058 Uiso 1 1 calc R U . . .
H33B H -0.1510 0.2411 0.3762 0.058 Uiso 1 1 calc R U . . .
H33C H -0.0994 0.3399 0.3693 0.058 Uiso 1 1 calc R U . . .
C34 C 0.05715(19) 0.3133(2) 0.45545(8) 0.0345(7) Uani 1 1 d . . . . .
H34A H -0.0022 0.3151 0.4613 0.041 Uiso 1 1 calc R U . . .
H34B H 0.0844 0.3789 0.4620 0.041 Uiso 1 1 calc R U . . .
C35 C 0.1100(2) 0.2346(2) 0.48002(9) 0.0454(9) Uani 1 1 d . . . . .
H35A H 0.1153 0.2516 0.5074 0.068 Uiso 1 1 calc R U . . .
H35B H 0.1682 0.2310 0.4736 0.068 Uiso 1 1 calc R U . . .
H35C H 0.0809 0.1702 0.4750 0.068 Uiso 1 1 calc R U . . .
C36 C 0.1857(2) 0.1533(2) 0.35467(9) 0.0458(9) Uani 1 1 d . . . . .
H36A H 0.2429 0.1467 0.3469 0.055 Uiso 1 1 calc R U . . .
H36B H 0.1449 0.1057 0.3392 0.055 Uiso 1 1 calc R U . . .
C37 C 0.1950(2) 0.1294(2) 0.39669(9) 0.0487(9) Uani 1 1 d . . . . .
H37A H 0.2340 0.1777 0.4120 0.073 Uiso 1 1 calc R U . . .
H37B H 0.2194 0.0626 0.4016 0.073 Uiso 1 1 calc R U . . .
H37C H 0.1377 0.1322 0.4040 0.073 Uiso 1 1 calc R U . . .
C38 C 0.17086(19) 0.2901(2) 0.31107(8) 0.0372(8) Uani 1 1 d . . . . .
H38A H 0.2344 0.2876 0.3119 0.045 Uiso 1 1 calc R U . . .
H38B H 0.1526 0.3604 0.3082 0.045 Uiso 1 1 calc R U . . .
C39 C 0.1250(2) 0.2327(3) 0.27604(9) 0.0530(9) Uani 1 1 d . . . . .
H39A H 0.1478 0.1649 0.2771 0.079 Uiso 1 1 calc R U . . .
H39B H 0.1352 0.2654 0.2525 0.079 Uiso 1 1 calc R U . . .
H39C H 0.0623 0.2309 0.2759 0.079 Uiso 1 1 calc R U . . .
Li2 Li 0.6222(3) 0.2111(3) 0.38475(13) 0.0253(11) Uani 1 1 d D . . . .
O3 O 0.65827(12) 0.31901(14) 0.35283(6) 0.0330(5) Uani 1 1 d . . . . .
N4 N 0.56077(12) 0.08818(15) 0.36112(6) 0.0177(5) Uani 1 1 d . . . . .
N3 N 0.70275(12) 0.08671(15) 0.38970(6) 0.0177(5) Uani 1 1 d . . . . .
C40 C 0.63214(15) 0.03412(18) 0.37383(7) 0.0167(6) Uani 1 1 d . . . . .
C41 C 0.63261(15) -0.07766(19) 0.37105(7) 0.0196(6) Uani 1 1 d . . . . .
C42 C 0.58538(16) -0.1262(2) 0.33899(8) 0.0244(6) Uani 1 1 d . . . . .
H42 H 0.5543 -0.0885 0.3180 0.029 Uiso 1 1 calc R U . . .
C43 C 0.58283(17) -0.2290(2) 0.33712(8) 0.0297(7) Uani 1 1 d . . . . .
H43 H 0.5504 -0.2612 0.3150 0.036 Uiso 1 1 calc R U . . .
C44 C 0.62749(17) -0.2842(2) 0.36751(9) 0.0315(7) Uani 1 1 d . . . . .
H44 H 0.6250 -0.3546 0.3665 0.038 Uiso 1 1 calc R U . . .
C45 C 0.67563(17) -0.2375(2) 0.39934(8) 0.0296(7) Uani 1 1 d . . . . .
H45 H 0.7074 -0.2758 0.4200 0.036 Uiso 1 1 calc R U . . .
C46 C 0.67787(15) -0.13481(19) 0.40129(8) 0.0224(6) Uani 1 1 d . . . . .
H46 H 0.7106 -0.1031 0.4235 0.027 Uiso 1 1 calc R U . . .
C47 C 0.47697(15) 0.04631(19) 0.35055(7) 0.0200(6) Uani 1 1 d . . . . .
C48 C 0.42797(16) 0.0736(2) 0.31363(7) 0.0232(6) Uani 1 1 d . . . . .
C49 C 0.34702(16) 0.0298(2) 0.30085(8) 0.0312(7) Uani 1 1 d . . . . .
H49 H 0.3147 0.0459 0.2760 0.037 Uiso 1 1 calc R U . . .
C50 C 0.31296(17) -0.0365(2) 0.32374(9) 0.0347(8) Uani 1 1 d . . . . .
H50 H 0.2591 -0.0686 0.3141 0.042 Uiso 1 1 calc R U . . .
C51 C 0.35723(17) -0.0560(2) 0.36061(8) 0.0284(7) Uani 1 1 d . . . . .
H51 H 0.3319 -0.0992 0.3766 0.034 Uiso 1 1 calc R U . . .
C52 C 0.43859(15) -0.01376(19) 0.37512(8) 0.0217(6) Uani 1 1 d . . . . .
C53 C 0.46469(16) 0.1475(2) 0.28860(7) 0.0267(7) Uani 1 1 d . . . . .
H53 H 0.5077 0.1894 0.3063 0.032 Uiso 1 1 calc R U . . .
C54 C 0.51435(19) 0.0956(2) 0.26107(8) 0.0411(8) Uani 1 1 d . . . . .
H54A H 0.5616 0.0558 0.2760 0.062 Uiso 1 1 calc R U . . .
H54B H 0.5389 0.1454 0.2460 0.062 Uiso 1 1 calc R U . . .
H54C H 0.4745 0.0523 0.2436 0.062 Uiso 1 1 calc R U . . .
C55 C 0.39540(19) 0.2179(3) 0.26657(9) 0.0461(9) Uani 1 1 d . . . . .
H55A H 0.3628 0.2481 0.2847 0.069 Uiso 1 1 calc R U . . .
H55B H 0.3553 0.1804 0.2469 0.069 Uiso 1 1 calc R U . . .
H55C H 0.4238 0.2699 0.2541 0.069 Uiso 1 1 calc R U . . .
C56 C 0.47917(16) -0.0307(2) 0.41728(8) 0.0244(6) Uani 1 1 d . . . . .
H56 H 0.5407 -0.0064 0.4216 0.029 Uiso 1 1 calc R U . . .
C57 C 0.48090(18) -0.1397(2) 0.42917(9) 0.0385(8) Uani 1 1 d . . . . .
H57A H 0.5154 -0.1471 0.4554 0.058 Uiso 1 1 calc R U . . .
H57B H 0.5072 -0.1793 0.4111 0.058 Uiso 1 1 calc R U . . .
H57C H 0.4213 -0.1627 0.4287 0.058 Uiso 1 1 calc R U . . .
C58 C 0.42996(18) 0.0310(2) 0.44296(8) 0.0345(7) Uani 1 1 d . . . . .
H58A H 0.4571 0.0214 0.4702 0.052 Uiso 1 1 calc R U . . .
H58B H 0.3690 0.0094 0.4388 0.052 Uiso 1 1 calc R U . . .
H58C H 0.4324 0.1014 0.4363 0.052 Uiso 1 1 calc R U . . .
C59 C 0.78705(15) 0.04432(18) 0.39910(7) 0.0172(6) Uani 1 1 d . . . . .
C60 C 0.83065(16) 0.04905(19) 0.43809(7) 0.0210(6) Uani 1 1 d . . . . .
C61 C 0.91489(16) 0.0105(2) 0.44836(8) 0.0266(7) Uani 1 1 d . . . . .
H61 H 0.9437 0.0122 0.4747 0.032 Uiso 1 1 calc R U . . .
C62 C 0.95709(16) -0.0300(2) 0.42114(8) 0.0273(7) Uani 1 1 d . . . . .
H62 H 1.0142 -0.0564 0.4286 0.033 Uiso 1 1 calc R U . . .
C63 C 0.91539(16) -0.03179(19) 0.38307(8) 0.0255(6) Uani 1 1 d . . . . .
H63 H 0.9450 -0.0588 0.3643 0.031 Uiso 1 1 calc R U . . .
C64 C 0.83098(15) 0.00488(18) 0.37103(7) 0.0195(6) Uani 1 1 d . . . . .
C65 C 0.78734(17) 0.0927(2) 0.46908(7) 0.0275(7) Uani 1 1 d . . . . .
H65 H 0.7282 0.1163 0.4563 0.033 Uiso 1 1 calc R U . . .
C66 C 0.7756(2) 0.0172(3) 0.50003(9) 0.0541(10) Uani 1 1 d . . . . .
H66A H 0.8328 -0.0022 0.5148 0.081 Uiso 1 1 calc R U . . .
H66B H 0.7454 -0.0415 0.4876 0.081 Uiso 1 1 calc R U . . .
H66C H 0.7411 0.0470 0.5175 0.081 Uiso 1 1 calc R U . . .
C67 C 0.83788(19) 0.1821(2) 0.48842(9) 0.0393(8) Uani 1 1 d . . . . .
H67A H 0.8074 0.2100 0.5078 0.059 Uiso 1 1 calc R U . . .
H67B H 0.8422 0.2325 0.4689 0.059 Uiso 1 1 calc R U . . .
H67C H 0.8965 0.1611 0.5010 0.059 Uiso 1 1 calc R U . . .
C68 C 0.79187(17) 0.0026(2) 0.32803(7) 0.0247(6) Uani 1 1 d . . . . .
H68 H 0.7304 0.0268 0.3246 0.030 Uiso 1 1 calc R U . . .
C69 C 0.78996(18) -0.1026(2) 0.31146(8) 0.0335(7) Uani 1 1 d . . . . .
H69A H 0.8497 -0.1266 0.3132 0.050 Uiso 1 1 calc R U . . .
H69B H 0.7602 -0.1018 0.2843 0.050 Uiso 1 1 calc R U . . .
H69C H 0.7587 -0.1466 0.3262 0.050 Uiso 1 1 calc R U . . .
C70 C 0.84153(18) 0.0727(2) 0.30560(8) 0.0336(7) Uani 1 1 d . . . . .
H70A H 0.8415 0.1399 0.3162 0.050 Uiso 1 1 calc R U . . .
H70B H 0.8131 0.0734 0.2783 0.050 Uiso 1 1 calc R U . . .
H70C H 0.9017 0.0496 0.3080 0.050 Uiso 1 1 calc R U . . .
C71 C 0.67831(18) 0.2848(2) 0.31703(8) 0.0364(8) Uani 1 1 d . . . . .
H71A H 0.6625 0.2138 0.3138 0.044 Uiso 1 1 calc R U . . .
H71B H 0.7420 0.2901 0.3185 0.044 Uiso 1 1 calc R U . . .
C72 C 0.6322(2) 0.3412(2) 0.28184(9) 0.0490(9) Uani 1 1 d . . . . .
H72A H 0.5697 0.3445 0.2821 0.074 Uiso 1 1 calc R U . . .
H72B H 0.6411 0.3071 0.2584 0.074 Uiso 1 1 calc R U . . .
H72C H 0.6559 0.4086 0.2823 0.074 Uiso 1 1 calc R U . . .
C73 C 0.6898(2) 0.4186(2) 0.36176(10) 0.0492(9) Uani 1 1 d . . . . .
H73A H 0.6516 0.4664 0.3451 0.059 Uiso 1 1 calc R U . . .
H73B H 0.7493 0.4251 0.3563 0.059 Uiso 1 1 calc R U . . .
C74 C 0.6911(2) 0.4421(2) 0.40294(10) 0.0532(10) Uani 1 1 d . . . . .
H74A H 0.7276 0.3936 0.4194 0.080 Uiso 1 1 calc R U . . .
H74B H 0.6317 0.4393 0.4079 0.080 Uiso 1 1 calc R U . . .
H74C H 0.7150 0.5088 0.4087 0.080 Uiso 1 1 calc R U . . .
O4 O 0.5384(3) 0.2774(5) 0.41318(12) 0.0253(10) Uani 0.658(6) 1 d D . P A 1
C75 C 0.4693(3) 0.3272(5) 0.38782(19) 0.0302(15) Uani 0.658(6) 1 d D U P A 1
H75A H 0.4818 0.3264 0.3614 0.036 Uiso 0.658(6) 1 calc R U P A 1
H75B H 0.4682 0.3974 0.3960 0.036 Uiso 0.658(6) 1 calc R U P A 1
C76 C 0.3797(3) 0.2824(4) 0.38665(16) 0.0356(14) Uani 0.658(6) 1 d D U P A 1
H76A H 0.3809 0.2118 0.3801 0.053 Uiso 0.658(6) 1 calc R U P A 1
H76B H 0.3369 0.3167 0.3670 0.053 Uiso 0.658(6) 1 calc R U P A 1
H76C H 0.3636 0.2900 0.4120 0.053 Uiso 0.658(6) 1 calc R U P A 1
C77 C 0.5366(3) 0.3001(3) 0.45364(11) 0.0329(14) Uani 0.658(6) 1 d D U P A 1
H77A H 0.4793 0.2816 0.4595 0.040 Uiso 0.658(6) 1 calc R U P A 1
H77B H 0.5452 0.3722 0.4583 0.040 Uiso 0.658(6) 1 calc R U P A 1
C78 C 0.6069(5) 0.2440(6) 0.47931(19) 0.0314(17) Uani 0.658(6) 1 d D U P A 1
H78A H 0.6061 0.2599 0.5064 0.047 Uiso 0.658(6) 1 calc R U P A 1
H78B H 0.6635 0.2625 0.4734 0.047 Uiso 0.658(6) 1 calc R U P A 1
H78C H 0.5975 0.1727 0.4751 0.047 Uiso 0.658(6) 1 calc R U P A 1
O4B O 0.5601(7) 0.2690(12) 0.4233(2) 0.0253(10) Uani 0.342(6) 1 d D . P A 2
C75B C 0.4764(5) 0.3122(8) 0.4160(3) 0.038(3) Uani 0.342(6) 1 d D U P A 2
H75C H 0.4815 0.3841 0.4218 0.045 Uiso 0.342(6) 1 calc R U P A 2
H75D H 0.4408 0.2819 0.4333 0.045 Uiso 0.342(6) 1 calc R U P A 2
C76B C 0.4322(10) 0.2979(11) 0.3750(3) 0.052(5) Uani 0.342(6) 1 d D U P A 2
H76D H 0.4690 0.3242 0.3579 0.078 Uiso 0.342(6) 1 calc R U P A 2
H76E H 0.3763 0.3330 0.3703 0.078 Uiso 0.342(6) 1 calc R U P A 2
H76F H 0.4220 0.2269 0.3699 0.078 Uiso 0.342(6) 1 calc R U P A 2
C77B C 0.6127(6) 0.2893(7) 0.4599(2) 0.029(3) Uani 0.342(6) 1 d D U P A 2
H77C H 0.6064 0.3603 0.4661 0.035 Uiso 0.342(6) 1 calc R U P A 2
H77D H 0.6744 0.2777 0.4585 0.035 Uiso 0.342(6) 1 calc R U P A 2
C78B C 0.5904(12) 0.2277(16) 0.4918(4) 0.054(5) Uani 0.342(6) 1 d D U P A 2
H78D H 0.5302 0.2413 0.4943 0.081 Uiso 0.342(6) 1 calc R U P A 2
H78E H 0.6299 0.2442 0.5161 0.081 Uiso 0.342(6) 1 calc R U P A 2
H78F H 0.5964 0.1573 0.4859 0.081 Uiso 0.342(6) 1 calc R U P A 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
Li1 O1 1.961(5) . ?
Li1 O2 1.995(5) . ?
Li1 N1 2.023(5) . ?
Li1 N2 2.044(5) . ?
Li1 C1 2.412(5) . ?
O1 C34 1.438(3) . ?
O1 C32 1.440(3) . ?
O2 C38 1.438(3) . ?
O2 C36 1.442(3) . ?
N1 C1 1.332(3) . ?
N1 C8 1.402(3) . ?
N2 C1 1.335(3) . ?
N2 C20 1.410(3) . ?
C1 C2 1.501(3) . ?
C2 C3 1.392(3) . ?
C2 C7 1.401(3) . ?
C3 C4 1.387(4) . ?
C4 C5 1.392(4) . ?
C5 C6 1.380(4) . ?
C6 C7 1.383(4) . ?
C8 C9 1.413(3) . ?
C8 C13 1.416(3) . ?
C9 C10 1.394(3) . ?
C9 C14 1.515(3) . ?
C10 C11 1.377(4) . ?
C11 C12 1.377(4) . ?
C12 C13 1.385(3) . ?
C13 C17 1.519(4) . ?
C14 C15 1.527(4) . ?
C14 C16 1.533(3) . ?
C17 C19 1.532(4) . ?
C17 C18 1.535(4) . ?
C20 C21 1.410(3) . ?
C20 C25 1.421(3) . ?
C21 C22 1.396(3) . ?
C21 C26 1.519(3) . ?
C22 C23 1.379(3) . ?
C23 C24 1.382(4) . ?
C24 C25 1.392(3) . ?
C25 C29 1.519(3) . ?
C26 C27 1.533(4) . ?
C26 C28 1.542(3) . ?
C29 C31 1.523(3) . ?
C29 C30 1.530(3) . ?
C32 C33 1.494(4) . ?
C34 C35 1.511(4) . ?
C36 C37 1.496(4) . ?
C38 C39 1.515(4) . ?
Li2 O4B 1.976(8) . ?
Li2 O3 1.987(5) . ?
Li2 O4 2.007(5) . ?
Li2 N4 2.013(5) . ?
Li2 N3 2.084(5) . ?
Li2 C40 2.426(5) . ?
O3 C71 1.434(3) . ?
O3 C73 1.443(3) . ?
N4 C40 1.336(3) . ?
N4 C47 1.410(3) . ?
N3 C40 1.340(3) . ?
N3 C59 1.417(3) . ?
C40 C41 1.510(4) . ?
C41 C42 1.389(3) . ?
C41 C46 1.393(3) . ?
C42 C43 1.387(4) . ?
C43 C44 1.379(4) . ?
C44 C45 1.377(4) . ?
C45 C46 1.386(4) . ?
C47 C52 1.403(3) . ?
C47 C48 1.425(3) . ?
C48 C49 1.390(3) . ?
C48 C53 1.516(4) . ?
C49 C50 1.379(4) . ?
C50 C51 1.375(4) . ?
C51 C52 1.398(3) . ?
C52 C56 1.517(4) . ?
C53 C54 1.526(4) . ?
C53 C55 1.533(4) . ?
C56 C57 1.527(4) . ?
C56 C58 1.541(4) . ?
C59 C60 1.413(3) . ?
C59 C64 1.414(3) . ?
C60 C61 1.398(3) . ?
C60 C65 1.512(4) . ?
C61 C62 1.379(4) . ?
C62 C63 1.374(4) . ?
C63 C64 1.397(3) . ?
C64 C68 1.521(3) . ?
C65 C67 1.527(4) . ?
C65 C66 1.529(4) . ?
C68 C69 1.532(4) . ?
C68 C70 1.536(4) . ?
C71 C72 1.514(4) . ?
C73 C74 1.482(4) . ?
O4 C75 1.430(6) . ?
O4 C77 1.465(5) . ?
C75 C76 1.519(7) . ?
C77 C78 1.489(8) . ?
O4B C75B 1.411(8) . ?
O4B C77B 1.417(11) . ?
C75B C76B 1.489(12) . ?
C77B C78B 1.493(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Li1 O2 106.6(2) . . ?
O1 Li1 N1 108.8(2) . . ?
O2 Li1 N1 123.9(2) . . ?
O1 Li1 N2 130.9(2) . . ?
O2 Li1 N2 115.6(2) . . ?
N1 Li1 N2 67.05(16) . . ?
O1 Li1 C1 124.4(2) . . ?
O2 Li1 C1 128.0(2) . . ?
N1 Li1 C1 33.52(10) . . ?
N2 Li1 C1 33.61(10) . . ?
C34 O1 C32 114.3(2) . . ?
C34 O1 Li1 127.5(2) . . ?
C32 O1 Li1 117.6(2) . . ?
C38 O2 C36 111.6(2) . . ?
C38 O2 Li1 112.6(2) . . ?
C36 O2 Li1 133.7(2) . . ?
C1 N1 C8 124.5(2) . . ?
C1 N1 Li1 89.47(19) . . ?
C8 N1 Li1 142.1(2) . . ?
C1 N2 C20 123.7(2) . . ?
C1 N2 Li1 88.49(19) . . ?
C20 N2 Li1 147.5(2) . . ?
N1 C1 N2 114.8(2) . . ?
N1 C1 C2 122.3(2) . . ?
N2 C1 C2 122.9(2) . . ?
N1 C1 Li1 57.02(16) . . ?
N2 C1 Li1 57.90(16) . . ?
C2 C1 Li1 176.2(2) . . ?
C3 C2 C7 117.5(2) . . ?
C3 C2 C1 120.8(2) . . ?
C7 C2 C1 121.7(2) . . ?
C4 C3 C2 121.2(2) . . ?
C3 C4 C5 120.2(2) . . ?
C6 C5 C4 119.4(3) . . ?
C5 C6 C7 120.2(3) . . ?
C6 C7 C2 121.5(2) . . ?
N1 C8 C9 124.0(2) . . ?
N1 C8 C13 117.1(2) . . ?
C9 C8 C13 118.8(2) . . ?
C10 C9 C8 118.9(2) . . ?
C10 C9 C14 118.3(2) . . ?
C8 C9 C14 122.7(2) . . ?
C11 C10 C9 121.6(3) . . ?
C10 C11 C12 119.3(3) . . ?
C11 C12 C13 121.4(3) . . ?
C12 C13 C8 119.4(2) . . ?
C12 C13 C17 120.9(2) . . ?
C8 C13 C17 119.7(2) . . ?
C9 C14 C15 112.7(2) . . ?
C9 C14 C16 110.7(2) . . ?
C15 C14 C16 109.7(2) . . ?
C13 C17 C19 113.2(2) . . ?
C13 C17 C18 111.0(2) . . ?
C19 C17 C18 111.0(2) . . ?
N2 C20 C21 123.9(2) . . ?
N2 C20 C25 116.6(2) . . ?
C21 C20 C25 119.3(2) . . ?
C22 C21 C20 118.8(2) . . ?
C22 C21 C26 118.2(2) . . ?
C20 C21 C26 123.0(2) . . ?
C23 C22 C21 121.7(2) . . ?
C22 C23 C24 119.5(2) . . ?
C23 C24 C25 121.2(2) . . ?
C24 C25 C20 119.2(2) . . ?
C24 C25 C29 120.5(2) . . ?
C20 C25 C29 120.2(2) . . ?
C21 C26 C27 112.8(2) . . ?
C21 C26 C28 110.2(2) . . ?
C27 C26 C28 110.0(2) . . ?
C25 C29 C31 114.7(2) . . ?
C25 C29 C30 111.5(2) . . ?
C31 C29 C30 109.2(2) . . ?
O1 C32 C33 112.8(2) . . ?
O1 C34 C35 111.9(2) . . ?
O2 C36 C37 110.4(2) . . ?
O2 C38 C39 113.6(2) . . ?
O4B Li2 O3 109.4(5) . . ?
O3 Li2 O4 104.0(3) . . ?
O4B Li2 N4 110.5(6) . . ?
O3 Li2 N4 122.2(2) . . ?
O4 Li2 N4 105.5(3) . . ?
O4B Li2 N3 129.0(4) . . ?
O3 Li2 N3 113.7(2) . . ?
O4 Li2 N3 139.4(3) . . ?
N4 Li2 N3 66.75(16) . . ?
O4B Li2 C40 123.5(6) . . ?
O3 Li2 C40 126.6(2) . . ?
O4 Li2 C40 125.8(3) . . ?
N4 Li2 C40 33.42(10) . . ?
N3 Li2 C40 33.50(10) . . ?
C71 O3 C73 111.5(2) . . ?
C71 O3 Li2 113.5(2) . . ?
C73 O3 Li2 132.8(2) . . ?
C40 N4 C47 123.0(2) . . ?
C40 N4 Li2 90.52(19) . . ?
C47 N4 Li2 141.6(2) . . ?
C40 N3 C59 122.6(2) . . ?
C40 N3 Li2 87.37(19) . . ?
C59 N3 Li2 149.8(2) . . ?
N4 C40 N3 114.8(2) . . ?
N4 C40 C41 122.5(2) . . ?
N3 C40 C41 122.7(2) . . ?
N4 C40 Li2 56.07(16) . . ?
N3 C40 Li2 59.13(16) . . ?
C41 C40 Li2 173.0(2) . . ?
C42 C41 C46 118.3(2) . . ?
C42 C41 C40 121.0(2) . . ?
C46 C41 C40 120.7(2) . . ?
C43 C42 C41 121.0(3) . . ?
C44 C43 C42 119.8(3) . . ?
C45 C44 C43 120.1(3) . . ?
C44 C45 C46 120.1(3) . . ?
C45 C46 C41 120.7(3) . . ?
C52 C47 N4 123.7(2) . . ?
C52 C47 C48 119.6(2) . . ?
N4 C47 C48 116.5(2) . . ?
C49 C48 C47 118.8(3) . . ?
C49 C48 C53 120.9(2) . . ?
C47 C48 C53 120.2(2) . . ?
C50 C49 C48 121.1(3) . . ?
C51 C50 C49 119.8(3) . . ?
C50 C51 C52 121.7(3) . . ?
C51 C52 C47 118.5(2) . . ?
C51 C52 C56 118.4(2) . . ?
C47 C52 C56 123.0(2) . . ?
C48 C53 C54 111.4(2) . . ?
C48 C53 C55 113.0(2) . . ?
C54 C53 C55 111.0(2) . . ?
C52 C56 C57 113.3(2) . . ?
C52 C56 C58 109.4(2) . . ?
C57 C56 C58 110.0(2) . . ?
C60 C59 C64 119.3(2) . . ?
C60 C59 N3 117.5(2) . . ?
C64 C59 N3 123.0(2) . . ?
C61 C60 C59 119.3(2) . . ?
C61 C60 C65 119.3(2) . . ?
C59 C60 C65 121.4(2) . . ?
C62 C61 C60 121.4(3) . . ?
C63 C62 C61 119.1(2) . . ?
C62 C63 C64 122.2(3) . . ?
C63 C64 C59 118.6(2) . . ?
C63 C64 C68 118.0(2) . . ?
C59 C64 C68 123.3(2) . . ?
C60 C65 C67 111.3(2) . . ?
C60 C65 C66 112.9(2) . . ?
C67 C65 C66 109.2(2) . . ?
C64 C68 C69 111.9(2) . . ?
C64 C68 C70 110.8(2) . . ?
C69 C68 C70 110.3(2) . . ?
O3 C71 C72 114.2(2) . . ?
O3 C73 C74 110.6(3) . . ?
C75 O4 C77 110.8(4) . . ?
C75 O4 Li2 112.6(4) . . ?
C77 O4 Li2 135.8(3) . . ?
O4 C75 C76 114.4(6) . . ?
O4 C77 C78 109.5(4) . . ?
C75B O4B C77B 116.1(8) . . ?
C75B O4B Li2 126.9(7) . . ?
C77B O4B Li2 115.3(6) . . ?
O4B C75B C76B 111.3(9) . . ?
O4B C77B C78B 113.6(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C8 N1 C1 N2 166.8(2) . . . . ?
Li1 N1 C1 N2 4.6(2) . . . . ?
C8 N1 C1 C2 -13.4(4) . . . . ?
Li1 N1 C1 C2 -175.6(2) . . . . ?
C8 N1 C1 Li1 162.2(3) . . . . ?
C20 N2 C1 N1 170.4(2) . . . . ?
Li1 N2 C1 N1 -4.6(2) . . . . ?
C20 N2 C1 C2 -9.4(4) . . . . ?
Li1 N2 C1 C2 175.6(2) . . . . ?
C20 N2 C1 Li1 175.0(3) . . . . ?
N1 C1 C2 C3 -35.3(3) . . . . ?
N2 C1 C2 C3 144.5(2) . . . . ?
N1 C1 C2 C7 142.8(2) . . . . ?
N2 C1 C2 C7 -37.4(3) . . . . ?
C7 C2 C3 C4 -0.9(4) . . . . ?
C1 C2 C3 C4 177.2(2) . . . . ?
C2 C3 C4 C5 0.8(4) . . . . ?
C3 C4 C5 C6 -0.4(4) . . . . ?
C4 C5 C6 C7 0.1(4) . . . . ?
C5 C6 C7 C2 -0.3(4) . . . . ?
C3 C2 C7 C6 0.7(4) . . . . ?
C1 C2 C7 C6 -177.4(2) . . . . ?
C1 N1 C8 C9 -53.7(3) . . . . ?
Li1 N1 C8 C9 96.4(4) . . . . ?
C1 N1 C8 C13 130.9(3) . . . . ?
Li1 N1 C8 C13 -79.0(4) . . . . ?
N1 C8 C9 C10 176.8(2) . . . . ?
C13 C8 C9 C10 -7.9(4) . . . . ?
N1 C8 C9 C14 -6.3(4) . . . . ?
C13 C8 C9 C14 169.0(2) . . . . ?
C8 C9 C10 C11 2.8(4) . . . . ?
C14 C9 C10 C11 -174.3(2) . . . . ?
C9 C10 C11 C12 3.1(4) . . . . ?
C10 C11 C12 C13 -3.8(4) . . . . ?
C11 C12 C13 C8 -1.5(4) . . . . ?
C11 C12 C13 C17 179.5(2) . . . . ?
N1 C8 C13 C12 -177.0(2) . . . . ?
C9 C8 C13 C12 7.4(4) . . . . ?
N1 C8 C13 C17 2.0(3) . . . . ?
C9 C8 C13 C17 -173.6(2) . . . . ?
C10 C9 C14 C15 -53.6(3) . . . . ?
C8 C9 C14 C15 129.4(2) . . . . ?
C10 C9 C14 C16 69.6(3) . . . . ?
C8 C9 C14 C16 -107.4(3) . . . . ?
C12 C13 C17 C19 -35.4(4) . . . . ?
C8 C13 C17 C19 145.6(2) . . . . ?
C12 C13 C17 C18 90.1(3) . . . . ?
C8 C13 C17 C18 -88.9(3) . . . . ?
C1 N2 C20 C21 -60.1(3) . . . . ?
Li1 N2 C20 C21 110.6(4) . . . . ?
C1 N2 C20 C25 124.4(3) . . . . ?
Li1 N2 C20 C25 -65.0(4) . . . . ?
N2 C20 C21 C22 179.0(2) . . . . ?
C25 C20 C21 C22 -5.6(4) . . . . ?
N2 C20 C21 C26 -2.6(4) . . . . ?
C25 C20 C21 C26 172.8(2) . . . . ?
C20 C21 C22 C23 2.4(4) . . . . ?
C26 C21 C22 C23 -176.1(2) . . . . ?
C21 C22 C23 C24 1.4(4) . . . . ?
C22 C23 C24 C25 -2.0(4) . . . . ?
C23 C24 C25 C20 -1.2(4) . . . . ?
C23 C24 C25 C29 -178.6(2) . . . . ?
N2 C20 C25 C24 -179.2(2) . . . . ?
C21 C20 C25 C24 5.0(4) . . . . ?
N2 C20 C25 C29 -1.8(3) . . . . ?
C21 C20 C25 C29 -177.6(2) . . . . ?
C22 C21 C26 C27 -55.2(3) . . . . ?
C20 C21 C26 C27 126.4(3) . . . . ?
C22 C21 C26 C28 68.1(3) . . . . ?
C20 C21 C26 C28 -110.3(3) . . . . ?
C24 C25 C29 C31 -29.7(3) . . . . ?
C20 C25 C29 C31 153.0(2) . . . . ?
C24 C25 C29 C30 95.1(3) . . . . ?
C20 C25 C29 C30 -82.2(3) . . . . ?
C34 O1 C32 C33 81.4(3) . . . . ?
Li1 O1 C32 C33 -90.0(3) . . . . ?
C32 O1 C34 C35 87.9(3) . . . . ?
Li1 O1 C34 C35 -101.7(3) . . . . ?
C38 O2 C36 C37 160.5(2) . . . . ?
Li1 O2 C36 C37 -1.6(4) . . . . ?
C36 O2 C38 C39 63.8(3) . . . . ?
Li1 O2 C38 C39 -130.1(3) . . . . ?
C47 N4 C40 N3 -167.3(2) . . . . ?
Li2 N4 C40 N3 -7.2(2) . . . . ?
C47 N4 C40 C41 11.8(4) . . . . ?
Li2 N4 C40 C41 171.9(2) . . . . ?
C47 N4 C40 Li2 -160.1(3) . . . . ?
C59 N3 C40 N4 -169.7(2) . . . . ?
Li2 N3 C40 N4 7.0(2) . . . . ?
C59 N3 C40 C41 11.2(4) . . . . ?
Li2 N3 C40 C41 -172.1(2) . . . . ?
C59 N3 C40 Li2 -176.7(3) . . . . ?
N4 C40 C41 C42 37.9(4) . . . . ?
N3 C40 C41 C42 -143.0(2) . . . . ?
N4 C40 C41 C46 -139.6(2) . . . . ?
N3 C40 C41 C46 39.4(4) . . . . ?
C46 C41 C42 C43 0.3(4) . . . . ?
C40 C41 C42 C43 -177.3(2) . . . . ?
C41 C42 C43 C44 0.2(4) . . . . ?
C42 C43 C44 C45 -1.1(4) . . . . ?
C43 C44 C45 C46 1.4(4) . . . . ?
C44 C45 C46 C41 -0.8(4) . . . . ?
C42 C41 C46 C45 0.0(4) . . . . ?
C40 C41 C46 C45 177.6(2) . . . . ?
C40 N4 C47 C52 55.6(3) . . . . ?
Li2 N4 C47 C52 -91.2(4) . . . . ?
C40 N4 C47 C48 -128.8(3) . . . . ?
Li2 N4 C47 C48 84.4(4) . . . . ?
C52 C47 C48 C49 -8.0(4) . . . . ?
N4 C47 C48 C49 176.3(2) . . . . ?
C52 C47 C48 C53 173.2(2) . . . . ?
N4 C47 C48 C53 -2.6(3) . . . . ?
C47 C48 C49 C50 2.0(4) . . . . ?
C53 C48 C49 C50 -179.2(3) . . . . ?
C48 C49 C50 C51 3.5(4) . . . . ?
C49 C50 C51 C52 -3.1(4) . . . . ?
C50 C51 C52 C47 -2.9(4) . . . . ?
C50 C51 C52 C56 174.0(2) . . . . ?
N4 C47 C52 C51 -176.2(2) . . . . ?
C48 C47 C52 C51 8.4(4) . . . . ?
N4 C47 C52 C56 7.1(4) . . . . ?
C48 C47 C52 C56 -168.4(2) . . . . ?
C49 C48 C53 C54 -86.8(3) . . . . ?
C47 C48 C53 C54 92.1(3) . . . . ?
C49 C48 C53 C55 39.0(4) . . . . ?
C47 C48 C53 C55 -142.1(3) . . . . ?
C51 C52 C56 C57 50.5(3) . . . . ?
C47 C52 C56 C57 -132.7(3) . . . . ?
C51 C52 C56 C58 -72.7(3) . . . . ?
C47 C52 C56 C58 104.1(3) . . . . ?
C40 N3 C59 C60 -121.0(3) . . . . ?
Li2 N3 C59 C60 65.6(5) . . . . ?
C40 N3 C59 C64 63.8(3) . . . . ?
Li2 N3 C59 C64 -109.6(4) . . . . ?
C64 C59 C60 C61 -2.9(4) . . . . ?
N3 C59 C60 C61 -178.3(2) . . . . ?
C64 C59 C60 C65 178.6(2) . . . . ?
N3 C59 C60 C65 3.2(4) . . . . ?
C59 C60 C61 C62 1.5(4) . . . . ?
C65 C60 C61 C62 -180.0(2) . . . . ?
C60 C61 C62 C63 0.4(4) . . . . ?
C61 C62 C63 C64 -0.9(4) . . . . ?
C62 C63 C64 C59 -0.5(4) . . . . ?
C62 C63 C64 C68 178.0(2) . . . . ?
C60 C59 C64 C63 2.4(4) . . . . ?
N3 C59 C64 C63 177.5(2) . . . . ?
C60 C59 C64 C68 -176.0(2) . . . . ?
N3 C59 C64 C68 -0.9(4) . . . . ?
C61 C60 C65 C67 62.0(3) . . . . ?
C59 C60 C65 C67 -119.5(3) . . . . ?
C61 C60 C65 C66 -61.3(3) . . . . ?
C59 C60 C65 C66 117.2(3) . . . . ?
C63 C64 C68 C69 57.6(3) . . . . ?
C59 C64 C68 C69 -124.1(3) . . . . ?
C63 C64 C68 C70 -66.0(3) . . . . ?
C59 C64 C68 C70 112.4(3) . . . . ?
C73 O3 C71 C72 -65.7(3) . . . . ?
Li2 O3 C71 C72 129.0(3) . . . . ?
C71 O3 C73 C74 -164.1(2) . . . . ?
Li2 O3 C73 C74 -2.5(4) . . . . ?
C77 O4 C75 C76 -74.4(7) . . . . ?
Li2 O4 C75 C76 113.8(6) . . . . ?
C75 O4 C77 C78 177.7(6) . . . . ?
Li2 O4 C77 C78 -13.2(10) . . . . ?
C77B O4B C75B C76B 172.0(13) . . . . ?
Li2 O4B C75B C76B 8(2) . . . . ?
C75B O4B C77B C78B 79.2(18) . . . . ?
Li2 O4B C77B C78B -114.6(14) . . . . ?

_refine_diff_density_max         0.229
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.050

_shelxl_version_number           2013-4

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

data_kob33d3abs
_database_code_depnum_ccdc_archive 'CCDC 1061434'
_audit_update_record             
;
2015-04-23 deposited with the CCDC.
2015-06-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H39 Cl3 N2 Si'
_chemical_formula_sum            'C31 H39 Cl3 N2 Si'
_chemical_formula_weight         574.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'P 31 2 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'-x, -x+y, -z+1/3'
'x-y, -y, -z+2/3'

_cell_length_a                   14.761(2)
_cell_length_b                   14.761(2)
_cell_length_c                   24.465(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     4616.5(12)
_cell_formula_units_Z            6
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4998
_cell_measurement_theta_min      4.65
_cell_measurement_theta_max      24.9

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .5
_exptl_crystal_size_min          .5
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1824
_exptl_absorpt_coefficient_mu    0.359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min  0.8537
_exptl_absorpt_correction_T_max  0.9009

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  image_plate_Stoe-IPDS
_diffrn_measurement_method       omega_scan
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            51169
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.50
_diffrn_reflns_theta_max         29.22
_reflns_number_total             8352
_reflns_number_gt                6585
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Stoe-IPDS
_computing_cell_refinement       Stoe-IPDS
_computing_data_reduction        Stoe-IPDS
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Ortep/Povray
_computing_publication_material  Bruker-SHELXTL




_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0907P)²+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(6)
_refine_ls_number_reflns         8352
_refine_ls_number_parameters     355
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1328
_refine_ls_wR_factor_gt          0.1232
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si Si 0.53113(5) 0.52579(5) 0.75935(2) 0.03585(15) Uani 1 1 d D . .
N1 N 0.66533(13) 0.59999(13) 0.71725(6) 0.0292(3) Uani 1 1 d . A .
N2 N 0.61435(13) 0.65642(14) 0.78500(7) 0.0303(3) Uani 1 1 d . A .
C1 C 0.69427(16) 0.68101(16) 0.74959(7) 0.0298(4) Uani 1 1 d . A .
C2 C 0.79468(17) 0.78016(17) 0.74927(8) 0.0334(4) Uani 1 1 d . . .
C3 C 0.88668(18) 0.7791(2) 0.73774(10) 0.0430(5) Uani 1 1 d . A .
H3 H 0.8843 0.7150 0.7298 0.052 Uiso 1 1 calc R . .
C4 C 0.9815(2) 0.8718(2) 0.73785(13) 0.0557(7) Uani 1 1 d . . .
H4 H 1.0443 0.8714 0.7299 0.067 Uiso 1 1 calc R A .
C5 C 0.9847(2) 0.9646(2) 0.74953(13) 0.0621(8) Uani 1 1 d . A .
H5 H 1.0500 1.0280 0.7495 0.074 Uiso 1 1 calc R . .
C6 C 0.8948(2) 0.9669(2) 0.76128(13) 0.0558(7) Uani 1 1 d . . .
H6 H 0.8979 1.0313 0.7693 0.067 Uiso 1 1 calc R A .
C7 C 0.7997(2) 0.87436(18) 0.76130(10) 0.0433(5) Uani 1 1 d . A .
H7 H 0.7373 0.8755 0.7696 0.052 Uiso 1 1 calc R . .
C8 C 0.71316(15) 0.60349(16) 0.66519(8) 0.0296(4) Uani 1 1 d . . .
C9 C 0.70669(16) 0.66360(17) 0.62229(8) 0.0335(4) Uani 1 1 d . A .
C10 C 0.75699(19) 0.66769(19) 0.57323(9) 0.0407(5) Uani 1 1 d . . .
H10 H 0.7538 0.7081 0.5439 0.049 Uiso 1 1 calc R A .
C11 C 0.8112(2) 0.6149(2) 0.56616(9) 0.0426(5) Uani 1 1 d . A .
H11 H 0.8455 0.6196 0.5325 0.051 Uiso 1 1 calc R . .
C12 C 0.81508(18) 0.55525(19) 0.60846(10) 0.0404(5) Uani 1 1 d . . .
H12 H 0.8520 0.5185 0.6033 0.048 Uiso 1 1 calc R A .
C13 C 0.76648(17) 0.54720(18) 0.65855(9) 0.0343(4) Uani 1 1 d . A .
C14 C 0.64561(19) 0.72107(19) 0.62571(9) 0.0395(5) Uani 1 1 d . . .
H14 H 0.6146 0.7101 0.6631 0.047 Uiso 1 1 calc R A .
C15 C 0.7158(3) 0.8392(2) 0.61657(13) 0.0576(7) Uani 1 1 d . A .
H15A H 0.7735 0.8672 0.6429 0.086 Uiso 1 1 calc R . .
H15B H 0.6746 0.8740 0.6216 0.086 Uiso 1 1 calc R . .
H15C H 0.7442 0.8519 0.5794 0.086 Uiso 1 1 calc R . .
C16 C 0.5557(2) 0.6758(3) 0.58395(11) 0.0554(7) Uani 1 1 d . A .
H16A H 0.5845 0.6871 0.5469 0.083 Uiso 1 1 calc R . .
H16B H 0.5144 0.7107 0.5879 0.083 Uiso 1 1 calc R . .
H16C H 0.5107 0.6006 0.5904 0.083 Uiso 1 1 calc R . .
C17 C 0.7698(2) 0.4765(2) 0.70263(10) 0.0422(5) Uani 1 1 d . . .
H17 H 0.7479 0.4938 0.7380 0.051 Uiso 1 1 calc R A .
C18 C 0.8787(3) 0.4899(3) 0.71031(12) 0.0598(7) Uani 1 1 d . A .
H18A H 0.8772 0.4460 0.7407 0.090 Uiso 1 1 calc R . .
H18B H 0.9290 0.5633 0.7183 0.090 Uiso 1 1 calc R . .
H18C H 0.8996 0.4689 0.6768 0.090 Uiso 1 1 calc R . .
C19 C 0.6916(3) 0.3618(2) 0.68859(12) 0.0545(6) Uani 1 1 d . A .
H19A H 0.7135 0.3425 0.6548 0.082 Uiso 1 1 calc R . .
H19B H 0.6219 0.3532 0.6835 0.082 Uiso 1 1 calc R . .
H19C H 0.6896 0.3167 0.7185 0.082 Uiso 1 1 calc R . .
C20 C 0.61903(16) 0.71298(15) 0.83406(7) 0.0295(4) Uani 1 1 d . . .
C21 C 0.56235(17) 0.76595(17) 0.83584(9) 0.0347(4) Uani 1 1 d . A .
C22 C 0.5693(2) 0.82154(19) 0.88347(10) 0.0416(5) Uani 1 1 d . . .
H22 H 0.5314 0.8578 0.8857 0.050 Uiso 1 1 calc R A .
C23 C 0.6299(2) 0.8251(2) 0.92727(10) 0.0456(5) Uani 1 1 d . A .
H23 H 0.6338 0.8637 0.9591 0.055 Uiso 1 1 calc R . .
C24 C 0.6849(2) 0.77205(19) 0.92449(9) 0.0396(5) Uani 1 1 d . . .
H24 H 0.7261 0.7744 0.9549 0.048 Uiso 1 1 calc R A .
C25 C 0.68153(16) 0.71497(17) 0.87803(8) 0.0331(4) Uani 1 1 d . A .
C26 C 0.4926(2) 0.7634(2) 0.78936(10) 0.0436(5) Uani 1 1 d . . .
H26 H 0.4950 0.7181 0.7597 0.052 Uiso 1 1 calc R A .
C27 C 0.5293(3) 0.8712(3) 0.76562(17) 0.0804(11) Uani 1 1 d . A .
H27A H 0.5327 0.9185 0.7947 0.121 Uiso 1 1 calc R . .
H27B H 0.4801 0.8666 0.7374 0.121 Uiso 1 1 calc R . .
H27C H 0.5989 0.8982 0.7494 0.121 Uiso 1 1 calc R . .
C28 C 0.3792(2) 0.7155(3) 0.80847(13) 0.0627(8) Uani 1 1 d . A .
H28A H 0.3744 0.7606 0.8364 0.094 Uiso 1 1 calc R . .
H28B H 0.3558 0.6461 0.8239 0.094 Uiso 1 1 calc R . .
H28C H 0.3347 0.7093 0.7773 0.094 Uiso 1 1 calc R . .
C29 C 0.74306(18) 0.65770(18) 0.87793(9) 0.0369(4) Uani 1 1 d . . .
H29 H 0.7386 0.6288 0.8404 0.044 Uiso 1 1 calc R A .
C30 C 0.8591(2) 0.7312(2) 0.89127(13) 0.0521(6) Uani 1 1 d . A .
H30A H 0.8888 0.7895 0.8652 0.078 Uiso 1 1 calc R . .
H30B H 0.8970 0.6925 0.8886 0.078 Uiso 1 1 calc R . .
H30C H 0.8657 0.7585 0.9284 0.078 Uiso 1 1 calc R . .
C31 C 0.6941(3) 0.5659(2) 0.91804(11) 0.0528(6) Uani 1 1 d . A .
H31A H 0.7326 0.5278 0.9166 0.079 Uiso 1 1 calc R . .
H31B H 0.6209 0.5188 0.9080 0.079 Uiso 1 1 calc R . .
H31C H 0.6975 0.5924 0.9551 0.079 Uiso 1 1 calc R . .
Cl1 Cl 0.44316(5) 0.48720(7) 0.68926(3) 0.0562(2) Uani 0.900(2) 1 d P A 1
Cl2 Cl 0.55801(6) 0.41042(5) 0.78802(3) 0.05153(19) Uani 0.900(2) 1 d P A 1
Cl3 Cl 0.40579(5) 0.49051(6) 0.81398(3) 0.04951(18) Uani 0.900(2) 1 d P A 1
Cl1B Cl 0.4159(9) 0.5514(10) 0.7220(5) 0.090(3) Uiso 0.100(2) 1 d PD A 2
Cl2B Cl 0.4912(12) 0.4037(10) 0.6993(5) 0.111(4) Uiso 0.100(2) 1 d PD A 2
Cl3B Cl 0.5020(18) 0.4335(16) 0.8292(7) 0.151(7) Uiso 0.100(2) 1 d PD A 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
Si N2 1.8034(19) . ?
Si N1 2.0037(17) . ?
Si Cl1 2.0523(9) . ?
Si Cl2 2.0554(10) . ?
Si Cl3B 2.092(11) . ?
Si Cl1B 2.125(10) . ?
Si Cl3 2.1254(9) . ?
Si Cl2B 2.167(11) . ?
Si C1 2.364(2) . ?
N1 C1 1.315(3) . ?
N1 C8 1.445(2) . ?
N2 C1 1.358(3) . ?
N2 C20 1.444(2) . ?
C1 C2 1.473(3) . ?
C2 C7 1.387(3) . ?
C2 C3 1.394(3) . ?
C3 C4 1.384(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.377(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.374(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.386(4) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.408(3) . ?
C8 C13 1.411(3) . ?
C9 C10 1.397(3) . ?
C9 C14 1.518(3) . ?
C10 C11 1.379(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.378(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.395(3) . ?
C12 H12 0.9500 . ?
C13 C17 1.518(3) . ?
C14 C15 1.536(4) . ?
C14 C16 1.538(4) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.529(4) . ?
C17 C19 1.537(4) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.403(3) . ?
C20 C25 1.408(3) . ?
C21 C22 1.399(3) . ?
C21 C26 1.521(3) . ?
C22 C23 1.379(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.384(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.401(3) . ?
C24 H24 0.9500 . ?
C25 C29 1.519(3) . ?
C26 C27 1.517(4) . ?
C26 C28 1.529(4) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C31 1.530(3) . ?
C29 C30 1.537(4) . ?
C29 H29 1.0000 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Si N1 68.64(7) . . ?
N2 Si Cl1 125.85(7) . . ?
N1 Si Cl1 92.15(6) . . ?
N2 Si Cl2 117.17(7) . . ?
N1 Si Cl2 94.63(6) . . ?
Cl1 Si Cl2 114.37(5) . . ?
N2 Si Cl3B 102.7(6) . . ?
N1 Si Cl3B 126.9(6) . . ?
Cl1 Si Cl3B 127.3(7) . . ?
Cl2 Si Cl3B 40.9(6) . . ?
N2 Si Cl1B 97.9(3) . . ?
N1 Si Cl1B 110.0(3) . . ?
Cl1 Si Cl1B 40.4(3) . . ?
Cl2 Si Cl1B 142.9(4) . . ?
Cl3B Si Cl1B 123.0(7) . . ?
N2 Si Cl3 95.01(6) . . ?
N1 Si Cl3 163.49(6) . . ?
Cl1 Si Cl3 96.03(4) . . ?
Cl2 Si Cl3 95.01(4) . . ?
Cl3B Si Cl3 57.1(6) . . ?
Cl1B Si Cl3 68.8(3) . . ?
N2 Si Cl2B 151.9(4) . . ?
N1 Si Cl2B 83.6(4) . . ?
Cl1 Si Cl2B 48.0(4) . . ?
Cl2 Si Cl2B 68.1(4) . . ?
Cl3B Si Cl2B 97.5(7) . . ?
Cl1B Si Cl2B 87.0(5) . . ?
Cl3 Si Cl2B 112.4(4) . . ?
N2 Si C1 34.88(7) . . ?
N1 Si C1 33.77(7) . . ?
Cl1 Si C1 112.40(6) . . ?
Cl2 Si C1 108.21(6) . . ?
Cl3B Si C1 119.5(6) . . ?
Cl1B Si C1 107.6(3) . . ?
Cl3 Si C1 129.88(6) . . ?
Cl2B Si C1 117.3(4) . . ?
C1 N1 C8 124.58(17) . . ?
C1 N1 Si 88.31(12) . . ?
C8 N1 Si 143.58(13) . . ?
C1 N2 C20 126.26(17) . . ?
C1 N2 Si 95.74(13) . . ?
C20 N2 Si 135.86(14) . . ?
N1 C1 N2 107.28(18) . . ?
N1 C1 C2 127.48(19) . . ?
N2 C1 C2 125.23(19) . . ?
N1 C1 Si 57.91(11) . . ?
N2 C1 Si 49.38(10) . . ?
C2 C1 Si 174.21(15) . . ?
C7 C2 C3 119.4(2) . . ?
C7 C2 C1 121.2(2) . . ?
C3 C2 C1 119.5(2) . . ?
C4 C3 C2 119.9(2) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C5 C4 C3 119.9(3) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C6 C5 C4 121.0(3) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C5 C6 C7 119.4(3) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 H6 120.3 . . ?
C6 C7 C2 120.5(3) . . ?
C6 C7 H7 119.7 . . ?
C2 C7 H7 119.7 . . ?
C9 C8 C13 121.27(18) . . ?
C9 C8 N1 119.58(17) . . ?
C13 C8 N1 119.15(18) . . ?
C10 C9 C8 117.7(2) . . ?
C10 C9 C14 118.3(2) . . ?
C8 C9 C14 123.89(18) . . ?
C11 C10 C9 122.0(2) . . ?
C11 C10 H10 119.0 . . ?
C9 C10 H10 119.0 . . ?
C12 C11 C10 119.2(2) . . ?
C12 C11 H11 120.4 . . ?
C10 C11 H11 120.4 . . ?
C11 C12 C13 122.0(2) . . ?
C11 C12 H12 119.0 . . ?
C13 C12 H12 119.0 . . ?
C12 C13 C8 117.8(2) . . ?
C12 C13 C17 119.4(2) . . ?
C8 C13 C17 122.84(19) . . ?
C9 C14 C15 112.0(2) . . ?
C9 C14 C16 110.2(2) . . ?
C15 C14 C16 110.0(2) . . ?
C9 C14 H14 108.2 . . ?
C15 C14 H14 108.2 . . ?
C16 C14 H14 108.2 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 C17 C18 113.1(2) . . ?
C13 C17 C19 109.5(2) . . ?
C18 C17 C19 109.4(2) . . ?
C13 C17 H17 108.3 . . ?
C18 C17 H17 108.3 . . ?
C19 C17 H17 108.3 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C25 122.13(18) . . ?
C21 C20 N2 118.61(18) . . ?
C25 C20 N2 119.25(18) . . ?
C22 C21 C20 117.6(2) . . ?
C22 C21 C26 119.2(2) . . ?
C20 C21 C26 123.20(19) . . ?
C23 C22 C21 121.7(2) . . ?
C23 C22 H22 119.1 . . ?
C21 C22 H22 119.1 . . ?
C22 C23 C24 119.5(2) . . ?
C22 C23 H23 120.2 . . ?
C24 C23 H23 120.2 . . ?
C23 C24 C25 121.7(2) . . ?
C23 C24 H24 119.1 . . ?
C25 C24 H24 119.1 . . ?
C24 C25 C20 117.28(19) . . ?
C24 C25 C29 118.99(19) . . ?
C20 C25 C29 123.71(18) . . ?
C27 C26 C21 112.2(3) . . ?
C27 C26 C28 109.6(3) . . ?
C21 C26 C28 110.7(2) . . ?
C27 C26 H26 108.0 . . ?
C21 C26 H26 108.0 . . ?
C28 C26 H26 108.0 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C25 C29 C31 110.0(2) . . ?
C25 C29 C30 111.87(19) . . ?
C31 C29 C30 110.8(2) . . ?
C25 C29 H29 108.0 . . ?
C31 C29 H29 108.0 . . ?
C30 C29 H29 108.0 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Si N1 C1 1.12(11) . . . . ?
Cl1 Si N1 C1 129.05(11) . . . . ?
Cl2 Si N1 C1 -116.29(11) . . . . ?
Cl3B Si N1 C1 -89.0(8) . . . . ?
Cl1B Si N1 C1 92.0(4) . . . . ?
Cl3 Si N1 C1 9.3(3) . . . . ?
Cl2B Si N1 C1 176.4(4) . . . . ?
N2 Si N1 C8 -155.3(2) . . . . ?
Cl1 Si N1 C8 -27.4(2) . . . . ?
Cl2 Si N1 C8 87.3(2) . . . . ?
Cl3B Si N1 C8 114.6(8) . . . . ?
Cl1B Si N1 C8 -64.4(4) . . . . ?
Cl3 Si N1 C8 -147.1(2) . . . . ?
Cl2B Si N1 C8 20.0(5) . . . . ?
C1 Si N1 C8 -156.4(3) . . . . ?
N1 Si N2 C1 -1.09(11) . . . . ?
Cl1 Si N2 C1 -77.62(13) . . . . ?
Cl2 Si N2 C1 82.98(12) . . . . ?
Cl3B Si N2 C1 123.9(7) . . . . ?
Cl1B Si N2 C1 -109.5(4) . . . . ?
Cl3 Si N2 C1 -178.77(11) . . . . ?
Cl2B Si N2 C1 -11.1(9) . . . . ?
N1 Si N2 C20 -164.3(2) . . . . ?
Cl1 Si N2 C20 119.21(18) . . . . ?
Cl2 Si N2 C20 -80.2(2) . . . . ?
Cl3B Si N2 C20 -39.3(7) . . . . ?
Cl1B Si N2 C20 87.3(4) . . . . ?
Cl3 Si N2 C20 18.1(2) . . . . ?
Cl2B Si N2 C20 -174.3(9) . . . . ?
C1 Si N2 C20 -163.2(3) . . . . ?
C8 N1 C1 N2 161.78(18) . . . . ?
Si N1 C1 N2 -1.45(14) . . . . ?
C8 N1 C1 C2 -19.3(3) . . . . ?
Si N1 C1 C2 177.5(2) . . . . ?
C8 N1 C1 Si 163.2(2) . . . . ?
C20 N2 C1 N1 167.14(18) . . . . ?
Si N2 C1 N1 1.62(16) . . . . ?
C20 N2 C1 C2 -11.8(3) . . . . ?
Si N2 C1 C2 -177.32(18) . . . . ?
C20 N2 C1 Si 165.5(2) . . . . ?
N2 Si C1 N1 -178.17(18) . . . . ?
Cl1 Si C1 N1 -57.08(12) . . . . ?
Cl2 Si C1 N1 70.18(12) . . . . ?
Cl3B Si C1 N1 113.4(7) . . . . ?
Cl1B Si C1 N1 -99.9(4) . . . . ?
Cl3 Si C1 N1 -176.57(11) . . . . ?
Cl2B Si C1 N1 -4.0(5) . . . . ?
N1 Si C1 N2 178.17(18) . . . . ?
Cl1 Si C1 N2 121.10(12) . . . . ?
Cl2 Si C1 N2 -111.64(12) . . . . ?
Cl3B Si C1 N2 -68.4(7) . . . . ?
Cl1B Si C1 N2 78.3(4) . . . . ?
Cl3 Si C1 N2 1.60(14) . . . . ?
Cl2B Si C1 N2 174.1(5) . . . . ?
N2 Si C1 C2 22.3(15) . . . . ?
N1 Si C1 C2 -159.5(16) . . . . ?
Cl1 Si C1 C2 143.4(15) . . . . ?
Cl2 Si C1 C2 -89.4(16) . . . . ?
Cl3B Si C1 C2 -46.1(18) . . . . ?
Cl1B Si C1 C2 100.6(16) . . . . ?
Cl3 Si C1 C2 23.9(16) . . . . ?
Cl2B Si C1 C2 -163.6(16) . . . . ?
N1 C1 C2 C7 144.9(2) . . . . ?
N2 C1 C2 C7 -36.4(3) . . . . ?
Si C1 C2 C7 -57.1(16) . . . . ?
N1 C1 C2 C3 -36.4(3) . . . . ?
N2 C1 C2 C3 142.3(2) . . . . ?
Si C1 C2 C3 121.7(15) . . . . ?
C7 C2 C3 C4 -0.7(4) . . . . ?
C1 C2 C3 C4 -179.4(2) . . . . ?
C2 C3 C4 C5 0.2(5) . . . . ?
C3 C4 C5 C6 0.1(5) . . . . ?
C4 C5 C6 C7 -0.1(5) . . . . ?
C5 C6 C7 C2 -0.4(5) . . . . ?
C3 C2 C7 C6 0.7(4) . . . . ?
C1 C2 C7 C6 179.5(2) . . . . ?
C1 N1 C8 C9 -64.2(3) . . . . ?
Si N1 C8 C9 86.7(3) . . . . ?
C1 N1 C8 C13 115.1(2) . . . . ?
Si N1 C8 C13 -93.9(3) . . . . ?
C13 C8 C9 C10 -1.5(3) . . . . ?
N1 C8 C9 C10 177.88(19) . . . . ?
C13 C8 C9 C14 176.5(2) . . . . ?
N1 C8 C9 C14 -4.1(3) . . . . ?
C8 C9 C10 C11 0.2(3) . . . . ?
C14 C9 C10 C11 -177.9(2) . . . . ?
C9 C10 C11 C12 0.8(4) . . . . ?
C10 C11 C12 C13 -0.6(4) . . . . ?
C11 C12 C13 C8 -0.6(3) . . . . ?
C11 C12 C13 C17 177.4(2) . . . . ?
C9 C8 C13 C12 1.7(3) . . . . ?
N1 C8 C13 C12 -177.69(19) . . . . ?
C9 C8 C13 C17 -176.3(2) . . . . ?
N1 C8 C13 C17 4.3(3) . . . . ?
C10 C9 C14 C15 -61.1(3) . . . . ?
C8 C9 C14 C15 120.9(2) . . . . ?
C10 C9 C14 C16 61.7(3) . . . . ?
C8 C9 C14 C16 -116.2(2) . . . . ?
C12 C13 C17 C18 45.9(3) . . . . ?
C8 C13 C17 C18 -136.1(2) . . . . ?
C12 C13 C17 C19 -76.3(3) . . . . ?
C8 C13 C17 C19 101.7(3) . . . . ?
C1 N2 C20 C21 112.2(2) . . . . ?
Si N2 C20 C21 -88.7(2) . . . . ?
C1 N2 C20 C25 -66.6(3) . . . . ?
Si N2 C20 C25 92.5(2) . . . . ?
C25 C20 C21 C22 -0.3(3) . . . . ?
N2 C20 C21 C22 -179.0(2) . . . . ?
C25 C20 C21 C26 -178.8(2) . . . . ?
N2 C20 C21 C26 2.4(3) . . . . ?
C20 C21 C22 C23 0.3(4) . . . . ?
C26 C21 C22 C23 178.9(2) . . . . ?
C21 C22 C23 C24 -0.4(4) . . . . ?
C22 C23 C24 C25 0.5(4) . . . . ?
C23 C24 C25 C20 -0.4(3) . . . . ?
C23 C24 C25 C29 -179.4(2) . . . . ?
C21 C20 C25 C24 0.3(3) . . . . ?
N2 C20 C25 C24 179.10(19) . . . . ?
C21 C20 C25 C29 179.3(2) . . . . ?
N2 C20 C25 C29 -1.9(3) . . . . ?
C22 C21 C26 C27 63.3(3) . . . . ?
C20 C21 C26 C27 -118.2(3) . . . . ?
C22 C21 C26 C28 -59.6(3) . . . . ?
C20 C21 C26 C28 119.0(3) . . . . ?
C24 C25 C29 C31 69.0(3) . . . . ?
C20 C25 C29 C31 -110.0(2) . . . . ?
C24 C25 C29 C30 -54.7(3) . . . . ?
C20 C25 C29 C30 126.4(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        29.22
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.056
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_kob37d_twin5
_database_code_depnum_ccdc_archive 'CCDC 1061435'
_audit_update_record             
;
2015-04-23 deposited with the CCDC.
2015-06-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H45 Cl2 N3 Si'
_chemical_formula_sum            'C33 H45 Cl2 N3 Si'
_chemical_formula_weight         582.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   P31

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'

_cell_length_a                   15.1910(19)
_cell_length_b                   15.1910(19)
_cell_length_c                   12.3499(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2468.1(6)
_cell_formula_units_Z            3
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5000
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      26.55

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936
_exptl_absorpt_coefficient_mu    0.259
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  image_plate_Stoe-IPDS
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6471
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0481
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.10
_diffrn_reflns_theta_max         26.01
_reflns_number_total             6471
_reflns_number_gt                5209
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Stoe-IPDS
_computing_cell_refinement       Stoe-IPDS
_computing_data_reduction        Stoe-IPDS
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP/POV-Ray
_computing_publication_material  Bruker-SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0807P)²+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(8)
_refine_ls_number_reflns         6471
_refine_ls_number_parameters     363
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0470
_refine_ls_wR_factor_ref         0.1178
_refine_ls_wR_factor_gt          0.1102
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_restrained_S_all      0.971
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.43653(8) 0.19712(8) 0.51590(8) 0.0568(2) Uani 1 1 d . . .
Cl2 Cl 0.20622(9) 0.07713(8) 0.44885(11) 0.0684(3) Uani 1 1 d . . .
Si Si 0.30158(8) 0.18969(8) 0.56278(10) 0.0530(3) Uani 1 1 d . . .
N1 N 0.3852(2) 0.3354(2) 0.6481(2) 0.0342(6) Uani 1 1 d . . .
N2 N 0.2819(2) 0.2867(2) 0.51104(19) 0.0340(6) Uani 1 1 d . . .
N3 N 0.2548(3) 0.1304(3) 0.6815(3) 0.0672(10) Uani 1 1 d . . .
C1 C 0.3429(2) 0.3666(2) 0.5788(2) 0.0344(6) Uani 1 1 d . . .
C2 C 0.3535(3) 0.4679(3) 0.5708(3) 0.0424(8) Uani 1 1 d . . .
C3 C 0.4460(3) 0.5537(3) 0.5974(3) 0.0547(9) Uani 1 1 d . . .
H3 H 0.5024 0.5465 0.6178 0.066 Uiso 1 1 calc R . .
C4 C 0.4557(4) 0.6491(4) 0.5940(5) 0.0862(17) Uani 1 1 d . . .
H4 H 0.5188 0.7073 0.6118 0.103 Uiso 1 1 calc R . .
C5 C 0.3751(5) 0.6599(4) 0.5653(6) 0.102(2) Uani 1 1 d . . .
H5 H 0.3816 0.7255 0.5657 0.123 Uiso 1 1 calc R . .
C6 C 0.2849(5) 0.5773(4) 0.5359(6) 0.103(2) Uani 1 1 d . . .
H6 H 0.2297 0.5858 0.5136 0.124 Uiso 1 1 calc R . .
C7 C 0.2736(4) 0.4817(3) 0.5385(4) 0.0659(12) Uani 1 1 d . . .
H7 H 0.2106 0.4245 0.5180 0.079 Uiso 1 1 calc R . .
C8 C 0.4291(3) 0.3849(2) 0.7479(3) 0.0367(7) Uani 1 1 d . . .
C9 C 0.3676(3) 0.3937(3) 0.8277(3) 0.0449(8) Uani 1 1 d . . .
C10 C 0.4144(3) 0.4419(3) 0.9248(3) 0.0511(9) Uani 1 1 d . . .
H10 H 0.3748 0.4493 0.9798 0.061 Uiso 1 1 calc R . .
C11 C 0.5156(3) 0.4787(3) 0.9425(3) 0.0522(10) Uani 1 1 d . . .
H11 H 0.5453 0.5121 1.0088 0.063 Uiso 1 1 calc R . .
C12 C 0.5744(3) 0.4681(3) 0.8663(3) 0.0440(8) Uani 1 1 d . . .
H12 H 0.6442 0.4925 0.8809 0.053 Uiso 1 1 calc R . .
C13 C 0.5328(2) 0.4215(3) 0.7662(2) 0.0360(7) Uani 1 1 d . . .
C14 C 0.2533(3) 0.3502(3) 0.8163(3) 0.0596(11) Uani 1 1 d . . .
H14 H 0.2332 0.3182 0.7430 0.072 Uiso 1 1 calc R . .
C15 C 0.2226(4) 0.4307(5) 0.8230(5) 0.0901(19) Uani 1 1 d . . .
H15A H 0.2593 0.4828 0.7679 0.135 Uiso 1 1 calc R . .
H15B H 0.2393 0.4621 0.8950 0.135 Uiso 1 1 calc R . .
H15C H 0.1492 0.3994 0.8106 0.135 Uiso 1 1 calc R . .
C16 C 0.1968(4) 0.2661(5) 0.9001(4) 0.093(2) Uani 1 1 d . . .
H16A H 0.1236 0.2320 0.8858 0.140 Uiso 1 1 calc R . .
H16B H 0.2106 0.2958 0.9729 0.140 Uiso 1 1 calc R . .
H16C H 0.2200 0.2165 0.8953 0.140 Uiso 1 1 calc R . .
C17 C 0.6021(3) 0.4115(3) 0.6828(3) 0.0408(8) Uani 1 1 d . . .
H17 H 0.5619 0.3817 0.6151 0.049 Uiso 1 1 calc R . .
C18 C 0.6942(3) 0.5148(3) 0.6544(3) 0.0546(9) Uani 1 1 d . . .
H18A H 0.7322 0.5065 0.5950 0.082 Uiso 1 1 calc R . .
H18B H 0.7384 0.5423 0.7180 0.082 Uiso 1 1 calc R . .
H18C H 0.6710 0.5618 0.6321 0.082 Uiso 1 1 calc R . .
C19 C 0.6380(3) 0.3417(3) 0.7226(3) 0.0546(9) Uani 1 1 d . . .
H19A H 0.5792 0.2744 0.7369 0.082 Uiso 1 1 calc R . .
H19B H 0.6770 0.3691 0.7895 0.082 Uiso 1 1 calc R . .
H19C H 0.6812 0.3359 0.6675 0.082 Uiso 1 1 calc R . .
C20 C 0.2387(2) 0.2947(2) 0.4096(2) 0.0338(7) Uani 1 1 d . . .
C21 C 0.3042(3) 0.3404(3) 0.3198(2) 0.0369(7) Uani 1 1 d . . .
C22 C 0.2586(3) 0.3397(3) 0.2217(3) 0.0522(9) Uani 1 1 d . . .
H22 H 0.3004 0.3697 0.1599 0.063 Uiso 1 1 calc R . .
C23 C 0.1558(3) 0.2972(4) 0.2114(3) 0.0598(11) Uani 1 1 d . . .
H23 H 0.1269 0.2967 0.1430 0.072 Uiso 1 1 calc R . .
C24 C 0.0934(3) 0.2546(3) 0.3012(3) 0.0509(9) Uani 1 1 d . . .
H24 H 0.0222 0.2271 0.2940 0.061 Uiso 1 1 calc R . .
C25 C 0.1333(3) 0.2516(3) 0.4004(3) 0.0404(7) Uani 1 1 d . . .
C26 C 0.4184(3) 0.3870(3) 0.3244(3) 0.0433(8) Uani 1 1 d . . .
H26 H 0.4368 0.3792 0.4002 0.052 Uiso 1 1 calc R . .
C27 C 0.4722(3) 0.5004(4) 0.2989(4) 0.0647(11) Uani 1 1 d . . .
H27A H 0.5459 0.5279 0.2990 0.097 Uiso 1 1 calc R . .
H27B H 0.4546 0.5355 0.3540 0.097 Uiso 1 1 calc R . .
H27C H 0.4508 0.5108 0.2275 0.097 Uiso 1 1 calc R . .
C28 C 0.4543(4) 0.3317(4) 0.2500(3) 0.0600(11) Uani 1 1 d . . .
H28A H 0.4352 0.3360 0.1752 0.090 Uiso 1 1 calc R . .
H28B H 0.4224 0.2602 0.2717 0.090 Uiso 1 1 calc R . .
H28C H 0.5283 0.3632 0.2551 0.090 Uiso 1 1 calc R . .
C29 C 0.0596(3) 0.2065(3) 0.4953(3) 0.0453(8) Uani 1 1 d . . .
H29 H 0.0999 0.2096 0.5607 0.054 Uiso 1 1 calc R . .
C30 C 0.0072(4) 0.2679(4) 0.5195(5) 0.0750(14) Uani 1 1 d . . .
H30A H -0.0308 0.2683 0.4555 0.113 Uiso 1 1 calc R . .
H30B H 0.0585 0.3379 0.5380 0.113 Uiso 1 1 calc R . .
H30C H -0.0397 0.2371 0.5805 0.113 Uiso 1 1 calc R . .
C31 C -0.0200(3) 0.0958(4) 0.4766(4) 0.0690(12) Uani 1 1 d . . .
H31A H -0.0609 0.0905 0.4130 0.104 Uiso 1 1 calc R . .
H31B H -0.0641 0.0694 0.5403 0.104 Uiso 1 1 calc R . .
H31C H 0.0138 0.0560 0.4645 0.104 Uiso 1 1 calc R . .
C32 C 0.3273(4) 0.1334(4) 0.7629(4) 0.0845(18) Uani 1 1 d . . .
H32A H 0.3936 0.1567 0.7287 0.127 Uiso 1 1 calc R . .
H32B H 0.3021 0.0651 0.7928 0.127 Uiso 1 1 calc R . .
H32C H 0.3345 0.1802 0.8213 0.127 Uiso 1 1 calc R . .
C33 C 0.1494(3) 0.0594(3) 0.6983(4) 0.0639(11) Uani 1 1 d . . .
H33A H 0.1102 0.0605 0.6359 0.096 Uiso 1 1 calc R . .
H33B H 0.1260 0.0779 0.7639 0.096 Uiso 1 1 calc R . .
H33C H 0.1398 -0.0090 0.7068 0.096 Uiso 1 1 calc R . .


_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
Cl1 Si 2.0783(15) . ?
Cl2 Si 2.1272(17) . ?
Si N3 1.681(3) . ?
Si N2 1.763(3) . ?
Si N1 2.193(3) . ?
N1 C1 1.294(4) . ?
N1 C8 1.424(4) . ?
N2 C1 1.382(4) . ?
N2 C20 1.447(4) . ?
N3 C33 1.429(5) . ?
N3 C32 1.476(6) . ?
C1 C2 1.467(5) . ?
C2 C7 1.389(5) . ?
C2 C3 1.397(5) . ?
C3 C4 1.382(7) . ?
C4 C5 1.362(8) . ?
C5 C6 1.366(8) . ?
C6 C7 1.375(6) . ?
C8 C13 1.402(5) . ?
C8 C9 1.410(5) . ?
C9 C10 1.401(5) . ?
C9 C14 1.524(5) . ?
C10 C11 1.364(6) . ?
C11 C12 1.361(6) . ?
C12 C13 1.409(5) . ?
C13 C17 1.534(5) . ?
C14 C15 1.514(8) . ?
C14 C16 1.531(7) . ?
C17 C19 1.497(5) . ?
C17 C18 1.533(5) . ?
C20 C25 1.399(5) . ?
C20 C21 1.418(5) . ?
C21 C22 1.392(5) . ?
C21 C26 1.512(5) . ?
C22 C23 1.366(6) . ?
C23 C24 1.391(6) . ?
C24 C25 1.377(5) . ?
C25 C29 1.526(5) . ?
C26 C28 1.518(6) . ?
C26 C27 1.525(6) . ?
C29 C31 1.519(6) . ?
C29 C30 1.529(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Si N2 124.11(18) . . ?
N3 Si Cl1 114.42(15) . . ?
N2 Si Cl1 115.36(11) . . ?
N3 Si Cl2 102.17(15) . . ?
N2 Si Cl2 95.75(10) . . ?
Cl1 Si Cl2 96.67(7) . . ?
N3 Si N1 89.88(17) . . ?
N2 Si N1 65.51(11) . . ?
Cl1 Si N1 91.22(9) . . ?
Cl2 Si N1 161.24(9) . . ?
C1 N1 C8 124.4(3) . . ?
C1 N1 Si 84.82(18) . . ?
C8 N1 Si 146.2(2) . . ?
C1 N2 C20 125.7(3) . . ?
C1 N2 Si 101.3(2) . . ?
C20 N2 Si 131.1(2) . . ?
C33 N3 C32 117.4(4) . . ?
C33 N3 Si 123.0(3) . . ?
C32 N3 Si 118.0(3) . . ?
N1 C1 N2 108.4(3) . . ?
N1 C1 C2 127.9(3) . . ?
N2 C1 C2 123.7(3) . . ?
C7 C2 C3 118.3(4) . . ?
C7 C2 C1 122.1(3) . . ?
C3 C2 C1 119.6(3) . . ?
C4 C3 C2 120.1(4) . . ?
C5 C4 C3 120.3(5) . . ?
C4 C5 C6 120.5(5) . . ?
C5 C6 C7 120.2(5) . . ?
C6 C7 C2 120.6(4) . . ?
C13 C8 C9 121.1(3) . . ?
C13 C8 N1 119.1(3) . . ?
C9 C8 N1 119.9(3) . . ?
C10 C9 C8 117.5(3) . . ?
C10 C9 C14 118.5(3) . . ?
C8 C9 C14 124.0(3) . . ?
C11 C10 C9 121.6(3) . . ?
C12 C11 C10 120.8(3) . . ?
C11 C12 C13 120.7(3) . . ?
C8 C13 C12 118.3(3) . . ?
C8 C13 C17 122.9(3) . . ?
C12 C13 C17 118.8(3) . . ?
C15 C14 C9 112.9(4) . . ?
C15 C14 C16 111.5(4) . . ?
C9 C14 C16 109.9(4) . . ?
C19 C17 C18 109.3(3) . . ?
C19 C17 C13 111.2(3) . . ?
C18 C17 C13 111.9(3) . . ?
C25 C20 C21 121.6(3) . . ?
C25 C20 N2 119.5(3) . . ?
C21 C20 N2 118.8(3) . . ?
C22 C21 C20 116.9(3) . . ?
C22 C21 C26 119.1(3) . . ?
C20 C21 C26 124.0(3) . . ?
C23 C22 C21 122.1(4) . . ?
C22 C23 C24 119.9(3) . . ?
C25 C24 C23 121.1(4) . . ?
C24 C25 C20 118.4(3) . . ?
C24 C25 C29 117.5(3) . . ?
C20 C25 C29 124.0(3) . . ?
C21 C26 C28 111.3(3) . . ?
C21 C26 C27 111.2(3) . . ?
C28 C26 C27 111.3(3) . . ?
C31 C29 C25 112.3(3) . . ?
C31 C29 C30 109.7(4) . . ?
C25 C29 C30 111.4(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 Si N1 C1 -128.4(2) . . . . ?
N2 Si N1 C1 -0.26(19) . . . . ?
Cl1 Si N1 C1 117.19(18) . . . . ?
Cl2 Si N1 C1 2.1(4) . . . . ?
N3 Si N1 C8 23.8(4) . . . . ?
N2 Si N1 C8 151.9(4) . . . . ?
Cl1 Si N1 C8 -90.6(4) . . . . ?
Cl2 Si N1 C8 154.3(3) . . . . ?
N3 Si N2 C1 72.1(3) . . . . ?
Cl1 Si N2 C1 -78.8(2) . . . . ?
Cl2 Si N2 C1 -178.98(18) . . . . ?
N1 Si N2 C1 0.25(18) . . . . ?
N3 Si N2 C20 -123.4(3) . . . . ?
Cl1 Si N2 C20 85.7(3) . . . . ?
Cl2 Si N2 C20 -14.5(3) . . . . ?
N1 Si N2 C20 164.8(3) . . . . ?
N2 Si N3 C33 71.9(4) . . . . ?
Cl1 Si N3 C33 -137.0(4) . . . . ?
Cl2 Si N3 C33 -33.8(4) . . . . ?
N1 Si N3 C33 131.8(4) . . . . ?
N2 Si N3 C32 -122.7(4) . . . . ?
Cl1 Si N3 C32 28.5(4) . . . . ?
Cl2 Si N3 C32 131.7(4) . . . . ?
N1 Si N3 C32 -62.8(4) . . . . ?
C8 N1 C1 N2 -161.3(3) . . . . ?
Si N1 C1 N2 0.3(2) . . . . ?
C8 N1 C1 C2 17.7(5) . . . . ?
Si N1 C1 C2 179.3(3) . . . . ?
C20 N2 C1 N1 -166.1(3) . . . . ?
Si N2 C1 N1 -0.4(3) . . . . ?
C20 N2 C1 C2 14.9(5) . . . . ?
Si N2 C1 C2 -179.5(3) . . . . ?
N1 C1 C2 C7 -145.4(4) . . . . ?
N2 C1 C2 C7 33.5(5) . . . . ?
N1 C1 C2 C3 33.9(6) . . . . ?
N2 C1 C2 C3 -147.2(4) . . . . ?
C7 C2 C3 C4 1.7(7) . . . . ?
C1 C2 C3 C4 -177.6(4) . . . . ?
C2 C3 C4 C5 0.3(9) . . . . ?
C3 C4 C5 C6 -2.2(12) . . . . ?
C4 C5 C6 C7 2.1(13) . . . . ?
C5 C6 C7 C2 0.0(11) . . . . ?
C3 C2 C7 C6 -1.9(8) . . . . ?
C1 C2 C7 C6 177.4(6) . . . . ?
C1 N1 C8 C13 -119.2(4) . . . . ?
Si N1 C8 C13 95.1(4) . . . . ?
C1 N1 C8 C9 62.7(5) . . . . ?
Si N1 C8 C9 -83.0(5) . . . . ?
C13 C8 C9 C10 1.1(5) . . . . ?
N1 C8 C9 C10 179.2(3) . . . . ?
C13 C8 C9 C14 -176.2(4) . . . . ?
N1 C8 C9 C14 1.9(6) . . . . ?
C8 C9 C10 C11 -0.4(6) . . . . ?
C14 C9 C10 C11 177.1(4) . . . . ?
C9 C10 C11 C12 -1.0(7) . . . . ?
C10 C11 C12 C13 1.8(6) . . . . ?
C9 C8 C13 C12 -0.4(5) . . . . ?
N1 C8 C13 C12 -178.6(3) . . . . ?
C9 C8 C13 C17 178.6(3) . . . . ?
N1 C8 C13 C17 0.5(5) . . . . ?
C11 C12 C13 C8 -1.0(5) . . . . ?
C11 C12 C13 C17 179.9(3) . . . . ?
C10 C9 C14 C15 62.5(6) . . . . ?
C8 C9 C14 C15 -120.2(4) . . . . ?
C10 C9 C14 C16 -62.7(5) . . . . ?
C8 C9 C14 C16 114.6(4) . . . . ?
C8 C13 C17 C19 -113.4(4) . . . . ?
C12 C13 C17 C19 65.7(4) . . . . ?
C8 C13 C17 C18 124.1(4) . . . . ?
C12 C13 C17 C18 -56.9(4) . . . . ?
C1 N2 C20 C25 -113.4(4) . . . . ?
Si N2 C20 C25 85.4(4) . . . . ?
C1 N2 C20 C21 70.7(4) . . . . ?
Si N2 C20 C21 -90.5(4) . . . . ?
C25 C20 C21 C22 -0.6(5) . . . . ?
N2 C20 C21 C22 175.2(3) . . . . ?
C25 C20 C21 C26 -179.2(3) . . . . ?
N2 C20 C21 C26 -3.4(5) . . . . ?
C20 C21 C22 C23 0.1(6) . . . . ?
C26 C21 C22 C23 178.7(4) . . . . ?
C21 C22 C23 C24 1.2(7) . . . . ?
C22 C23 C24 C25 -2.0(7) . . . . ?
C23 C24 C25 C20 1.5(6) . . . . ?
C23 C24 C25 C29 178.2(4) . . . . ?
C21 C20 C25 C24 -0.1(5) . . . . ?
N2 C20 C25 C24 -176.0(3) . . . . ?
C21 C20 C25 C29 -176.6(3) . . . . ?
N2 C20 C25 C29 7.6(5) . . . . ?
C22 C21 C26 C28 -61.1(5) . . . . ?
C20 C21 C26 C28 117.5(4) . . . . ?
C22 C21 C26 C27 63.6(5) . . . . ?
C20 C21 C26 C27 -117.8(4) . . . . ?
C24 C25 C29 C31 61.3(5) . . . . ?
C20 C25 C29 C31 -122.2(4) . . . . ?
C24 C25 C29 C30 -62.1(5) . . . . ?
C20 C25 C29 C30 114.4(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.01
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.057
