 
data_2009src0245p21c
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C16 H21 Cl N4 O7 Si'
_chemical_formula_weight          444.91
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 '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'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    P21/c
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    24.2668(9)
_cell_length_b                    6.9038(2)
_cell_length_c                    23.7477(9)
_cell_angle_alpha                 90.00
_cell_angle_beta                  93.232(2)
_cell_angle_gamma                 90.00
_cell_volume                      3972.2(2)
_cell_formula_units_Z             8
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     67214
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        block
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.39
_exptl_crystal_size_mid           0.31
_exptl_crystal_size_min           0.17
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.488
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1856
_exptl_absorpt_coefficient_mu     0.300
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8950
_exptl_absorpt_correction_T_max   0.9522
_exptl_absorpt_process_details    'SADABS 2007/2 (Sheldrick, G.M., 2007)' 
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    'graphite'
_diffrn_measurement_device_type   
'Bruker-Nonius Roper CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   '9.091'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             8357
_diffrn_reflns_av_R_equivalents   0.0000
_diffrn_reflns_av_sigmaI/netI     0.0696
_diffrn_reflns_limit_h_min        0
_diffrn_reflns_limit_h_max        31
_diffrn_reflns_limit_k_min        -8
_diffrn_reflns_limit_k_max        0
_diffrn_reflns_limit_l_min        -30
_diffrn_reflns_limit_l_max        30
_diffrn_reflns_theta_min          3.20
_diffrn_reflns_theta_max          27.48
_reflns_number_total              8357
_reflns_number_gt                 5961
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'  
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

 Non-merohedral twin where components are related by a 180deg rotation
 about the c axis. Data has been refined using hkl 5 with a batch scale
 factor of 0.50273. 

 Due to the twinning, there is partial overlap of some of the reflections
 from each of the twin components. These reflections have been removed as
 they could not be accurately separated therefore the
 diffrn_measured_fraction_theta_full value is lower than usual.
;
 
_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)+(0.0304P)²+14.9808P] 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          8357
_refine_ls_number_parameters      534
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1152
_refine_ls_R_factor_gt            0.0702
_refine_ls_wR_factor_ref          0.1557
_refine_ls_wR_factor_gt           0.1340
_refine_ls_goodness_of_fit_ref    1.085
_refine_ls_restrained_S_all       1.085
_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
C2 C -0.0424(2) 0.4151(8) 0.2323(2) 0.0193(13) Uani 1 1 d . . .
H2 H -0.0193 0.3853 0.2647 0.023 Uiso 1 1 calc R . .
C3 C -0.0974(2) 0.4473(8) 0.2381(2) 0.0199(13) Uani 1 1 d . . .
C4 C -0.1300(2) 0.4938(8) 0.1893(2) 0.0188(13) Uani 1 1 d . . .
H4 H -0.1682 0.5202 0.1919 0.023 Uiso 1 1 calc R . .
C5 C -0.1070(2) 0.5013(8) 0.1378(2) 0.0162(12) Uani 1 1 d . . .
C6 C -0.0502(2) 0.4639(7) 0.1319(2) 0.0123(11) Uani 1 1 d . . .
C7 C 0.0380(2) 0.3807(9) 0.1734(2) 0.0193(13) Uani 1 1 d . . .
H7A H 0.0460 0.2441 0.1836 0.023 Uiso 1 1 calc R . .
H7B H 0.0620 0.4650 0.1980 0.023 Uiso 1 1 calc R . .
C8 C -0.1225(3) 0.4322(10) 0.2941(3) 0.0293(15) Uani 1 1 d . . .
H8A H -0.0931 0.4268 0.3241 0.044 Uiso 1 1 calc R . .
H8B H -0.1449 0.3144 0.2951 0.044 Uiso 1 1 calc R . .
H8C H -0.1458 0.5456 0.2998 0.044 Uiso 1 1 calc R . .
C9 C 0.0712(2) 0.6678(7) 0.0733(2) 0.0184(12) Uani 1 1 d . . .
H9A H 0.0688 0.6720 0.0320 0.028 Uiso 1 1 calc R . .
H9B H 0.1091 0.6963 0.0872 0.028 Uiso 1 1 calc R . .
H9C H 0.0461 0.7643 0.0880 0.028 Uiso 1 1 calc R . .
C22 C 0.1177(2) 0.0522(8) -0.0108(2) 0.0190(12) Uani 1 1 d . . .
H22 H 0.0894 0.0111 -0.0374 0.023 Uiso 1 1 calc R . .
C23 C 0.1715(2) 0.0042(8) -0.0195(2) 0.0183(12) Uani 1 1 d . . .
C24 C 0.2112(2) 0.0644(8) 0.0216(2) 0.0189(12) Uani 1 1 d . . .
H24 H 0.2489 0.0346 0.0171 0.023 Uiso 1 1 calc R . .
C25 C 0.1972(2) 0.1654(8) 0.0684(2) 0.0170(12) Uani 1 1 d . . .
C26 C 0.1417(2) 0.2224(7) 0.0748(2) 0.0157(11) Uani 1 1 d . . .
C27 C 0.0467(2) 0.2261(8) 0.0424(2) 0.0165(12) Uani 1 1 d . . .
H27A H 0.0235 0.1184 0.0550 0.020 Uiso 1 1 calc R . .
H27B H 0.0301 0.2770 0.0063 0.020 Uiso 1 1 calc R . .
C28 C 0.1871(2) -0.1028(9) -0.0716(3) 0.0293(15) Uani 1 1 d . . .
H28A H 0.1538 -0.1288 -0.0957 0.044 Uiso 1 1 calc R . .
H28B H 0.2049 -0.2256 -0.0606 0.044 Uiso 1 1 calc R . .
H28C H 0.2127 -0.0237 -0.0923 0.044 Uiso 1 1 calc R . .
N1 N -0.02038(18) 0.4250(6) 0.18118(19) 0.0163(11) Uani 1 1 d . . .
N5 N -0.14278(18) 0.5526(7) 0.0891(2) 0.0166(11) Uani 1 1 d . . .
N21 N 0.10388(17) 0.1572(6) 0.0349(2) 0.0153(10) Uani 1 1 d . . .
N25 N 0.24003(18) 0.2215(7) 0.1104(2) 0.0181(10) Uani 1 1 d . . .
O5A O -0.18813(15) 0.6241(6) 0.09713(17) 0.0273(10) Uani 1 1 d . . .
O5B O -0.12641(16) 0.5217(6) 0.04192(17) 0.0232(9) Uani 1 1 d . . .
O6 O -0.02438(14) 0.4653(5) 0.08689(15) 0.0150(8) Uani 1 1 d . . .
O25A O 0.22727(16) 0.2504(7) 0.15869(17) 0.0280(10) Uani 1 1 d . . .
O25B O 0.28736(14) 0.2341(6) 0.09524(17) 0.0259(9) Uani 1 1 d . . .
O26 O 0.12424(14) 0.3328(5) 0.11275(16) 0.0181(9) Uani 1 1 d . . .
Si1 Si 0.05155(6) 0.4238(2) 0.09727(6) 0.0150(4) Uani 1 1 d . . .
Cl1 Cl 0.04514(6) 0.4575(2) 0.35784(6) 0.0247(4) Uani 1 1 d . . .
C32 C 0.3847(2) 0.9530(8) 0.4751(2) 0.0168(12) Uani 1 1 d . . .
H32 H 0.4133 0.9879 0.4513 0.020 Uiso 1 1 calc R . .
C33 C 0.3315(2) 1.0140(8) 0.4615(2) 0.0173(12) Uani 1 1 d . . .
C34 C 0.2919(2) 0.9657(8) 0.5001(2) 0.0173(12) Uani 1 1 d . . .
H34 H 0.2552 1.0115 0.4937 0.021 Uiso 1 1 calc R . .
C35 C 0.3048(2) 0.8552(7) 0.5463(2) 0.0145(11) Uani 1 1 d . . .
C36 C 0.3589(2) 0.7838(8) 0.5571(2) 0.0159(12) Uani 1 1 d . . .
C37 C 0.45362(19) 0.7703(8) 0.5351(2) 0.0161(12) Uani 1 1 d . . .
H37A H 0.4777 0.8756 0.5505 0.019 Uiso 1 1 calc R . .
H37B H 0.4697 0.7185 0.5008 0.019 Uiso 1 1 calc R . .
C38 C 0.3172(2) 1.1216(8) 0.4079(2) 0.0215(13) Uani 1 1 d . . .
H38A H 0.3508 1.1448 0.3879 0.032 Uiso 1 1 calc R . .
H38B H 0.3002 1.2458 0.4168 0.032 Uiso 1 1 calc R . .
H38C H 0.2912 1.0446 0.3841 0.032 Uiso 1 1 calc R . .
C39 C 0.4275(2) 0.3270(8) 0.5636(2) 0.0206(13) Uani 1 1 d . . .
H39A H 0.4271 0.3250 0.5223 0.031 Uiso 1 1 calc R . .
H39B H 0.3906 0.2961 0.5757 0.031 Uiso 1 1 calc R . .
H39C H 0.4540 0.2308 0.5790 0.031 Uiso 1 1 calc R . .
C42 C 0.5412(2) 0.5765(8) 0.7356(2) 0.0160(12) Uani 1 1 d . . .
H42 H 0.5178 0.6075 0.7651 0.019 Uiso 1 1 calc R . .
C43 C 0.5967(2) 0.5434(9) 0.7489(2) 0.0207(13) Uani 1 1 d . . .
C44 C 0.6279(2) 0.4945(8) 0.7041(3) 0.0182(12) Uani 1 1 d . . .
H44 H 0.6659 0.4651 0.7113 0.022 Uiso 1 1 calc R . .
C45 C 0.6062(2) 0.4868(8) 0.6499(2) 0.0148(12) Uani 1 1 d . . .
C46 C 0.5497(2) 0.5257(7) 0.6365(2) 0.0138(12) Uani 1 1 d . . .
C47 C 0.4609(2) 0.6114(8) 0.6675(2) 0.0177(12) Uani 1 1 d . . .
H47A H 0.4530 0.7477 0.6772 0.021 Uiso 1 1 calc R . .
H47B H 0.4367 0.5263 0.6889 0.021 Uiso 1 1 calc R . .
C48 C 0.6205(3) 0.5572(10) 0.8080(3) 0.0306(15) Uani 1 1 d . . .
H48A H 0.6456 0.6685 0.8115 0.046 Uiso 1 1 calc R . .
H48B H 0.6410 0.4383 0.8178 0.046 Uiso 1 1 calc R . .
H48C H 0.5907 0.5738 0.8337 0.046 Uiso 1 1 calc R . .
N31 N 0.39719(17) 0.8452(6) 0.52136(18) 0.0128(9) Uani 1 1 d . . .
N35 N 0.26134(18) 0.8127(6) 0.5849(2) 0.0195(11) Uani 1 1 d . . .
N41 N 0.51940(17) 0.5659(6) 0.68204(17) 0.0119(10) Uani 1 1 d . . .
N45 N 0.64188(18) 0.4330(6) 0.6049(2) 0.0174(10) Uani 1 1 d . . .
O35A O 0.21434(15) 0.8713(6) 0.57101(17) 0.0267(9) Uani 1 1 d . . .
O35B O 0.27264(16) 0.7209(7) 0.62754(18) 0.0340(11) Uani 1 1 d . . .
O36 O 0.37567(14) 0.6659(5) 0.59623(16) 0.0183(9) Uani 1 1 d . . .
O45A O 0.62753(16) 0.4689(6) 0.55560(17) 0.0220(10) Uani 1 1 d . . .
O45B O 0.68664(15) 0.3578(6) 0.61934(18) 0.0276(10) Uani 1 1 d . . .
O46 O 0.52416(14) 0.5264(5) 0.58827(15) 0.0147(8) Uani 1 1 d . . .
Si2 Si 0.44808(6) 0.5709(2) 0.58954(6) 0.0134(3) Uani 1 1 d . . .
Cl2 Cl 0.45772(6) 0.9638(2) 0.35419(6) 0.0232(4) Uani 1 1 d . . .
C91 C 0.1910(3) 0.4854(13) 0.2807(3) 0.052(2) Uani 1 1 d . . .
H91A H 0.1953 0.6129 0.2986 0.078 Uiso 1 1 calc R . .
H91B H 0.2112 0.4828 0.2462 0.078 Uiso 1 1 calc R . .
H91C H 0.2057 0.3855 0.3068 0.078 Uiso 1 1 calc R . .
O91 O 0.1371(2) 0.4512(11) 0.2680(2) 0.0635(17) Uani 1 1 d . . .
H91 H 0.1186 0.4849 0.2952 0.095 Uiso 1 1 calc R . .
C92 C 0.3122(3) 0.9917(12) 0.2585(3) 0.053(2) Uani 1 1 d . . .
H92A H 0.2971 0.8927 0.2828 0.080 Uiso 1 1 calc R . .
H92B H 0.2930 0.9861 0.2211 0.080 Uiso 1 1 calc R . .
H92C H 0.3069 1.1201 0.2750 0.080 Uiso 1 1 calc R . .
O92 O 0.3663(2) 0.9594(12) 0.2538(2) 0.075(2) Uani 1 1 d . . .
H92 H 0.3829 0.9686 0.2857 0.113 Uiso 1 1 calc R . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C2 N1 1.356(7) . ?
C2 C3 1.366(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.402(8) . ?
C3 C8 1.498(8) . ?
C4 C5 1.374(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.417(7) . ?
C5 N5 1.451(7) . ?
C6 O6 1.269(6) . ?
C6 N1 1.367(7) . ?
C7 N1 1.471(6) . ?
C7 Si1 1.880(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 Si1 1.849(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C22 N21 1.362(7) . ?
C22 C23 1.375(7) . ?
C22 H22 0.9500 . ?
C23 C24 1.396(8) . ?
C23 C28 1.506(8) . ?
C24 C25 1.370(8) . ?
C24 H24 0.9500 . ?
C25 C26 1.420(7) . ?
C25 N25 1.452(7) . ?
C26 O26 1.271(6) . ?
C26 N21 1.358(7) . ?
C27 N21 1.487(6) . ?
C27 Si1 1.887(6) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
N5 O5B 1.229(6) . ?
N5 O5A 1.231(6) . ?
N25 O25A 1.222(6) . ?
N25 O25B 1.226(5) . ?
O6 Si1 1.867(4) . ?
O26 Si1 1.889(4) . ?
C32 N31 1.348(6) . ?
C32 C33 1.379(7) . ?
C32 H32 0.9500 . ?
C33 C34 1.406(8) . ?
C33 C38 1.496(7) . ?
C34 C35 1.360(8) . ?
C34 H34 0.9500 . ?
C35 C36 1.411(7) . ?
C35 N35 1.465(7) . ?
C36 O36 1.284(6) . ?
C36 N31 1.361(7) . ?
C37 N31 1.483(6) . ?
C37 Si2 1.898(6) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 Si2 1.852(6) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C42 N41 1.353(6) . ?
C42 C43 1.385(8) . ?
C42 H42 0.9500 . ?
C43 C44 1.381(8) . ?
C43 C48 1.492(8) . ?
C44 C45 1.364(8) . ?
C44 H44 0.9500 . ?
C45 C46 1.415(7) . ?
C45 N45 1.461(7) . ?
C46 O46 1.272(6) . ?
C46 N41 1.370(6) . ?
C47 N41 1.476(6) . ?
C47 Si2 1.882(6) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
N35 O35B 1.214(6) . ?
N35 O35A 1.237(5) . ?
N45 O45A 1.228(6) . ?
N45 O45B 1.235(6) . ?
O36 Si2 1.891(4) . ?
O46 Si2 1.873(4) . ?
C91 O91 1.347(9) . ?
C91 H91A 0.9800 . ?
C91 H91B 0.9800 . ?
C91 H91C 0.9800 . ?
O91 H91 0.8400 . ?
C92 O92 1.343(9) . ?
C92 H92A 0.9800 . ?
C92 H92B 0.9800 . ?
C92 H92C 0.9800 . ?
O92 H92 0.8400 . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
N1 C2 C3 121.2(5) . . ?
N1 C2 H2 119.4 . . ?
C3 C2 H2 119.4 . . ?
C2 C3 C4 117.6(5) . . ?
C2 C3 C8 121.7(6) . . ?
C4 C3 C8 120.7(5) . . ?
C5 C4 C3 120.3(5) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 121.9(5) . . ?
C4 C5 N5 117.6(5) . . ?
C6 C5 N5 120.5(5) . . ?
O6 C6 N1 117.4(5) . . ?
O6 C6 C5 127.6(5) . . ?
N1 C6 C5 114.9(5) . . ?
N1 C7 Si1 108.0(4) . . ?
N1 C7 H7A 110.1 . . ?
Si1 C7 H7A 110.1 . . ?
N1 C7 H7B 110.1 . . ?
Si1 C7 H7B 110.1 . . ?
H7A C7 H7B 108.4 . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si1 C9 H9A 109.5 . . ?
Si1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N21 C22 C23 121.8(5) . . ?
N21 C22 H22 119.1 . . ?
C23 C22 H22 119.1 . . ?
C22 C23 C24 116.6(5) . . ?
C22 C23 C28 121.7(5) . . ?
C24 C23 C28 121.7(5) . . ?
C25 C24 C23 121.7(5) . . ?
C25 C24 H24 119.2 . . ?
C23 C24 H24 119.2 . . ?
C24 C25 C26 120.6(5) . . ?
C24 C25 N25 119.4(5) . . ?
C26 C25 N25 119.9(5) . . ?
O26 C26 N21 117.1(5) . . ?
O26 C26 C25 126.7(5) . . ?
N21 C26 C25 116.1(5) . . ?
N21 C27 Si1 107.0(3) . . ?
N21 C27 H27A 110.3 . . ?
Si1 C27 H27A 110.3 . . ?
N21 C27 H27B 110.3 . . ?
Si1 C27 H27B 110.3 . . ?
H27A C27 H27B 108.6 . . ?
C23 C28 H28A 109.5 . . ?
C23 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C23 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C2 N1 C6 124.1(5) . . ?
C2 N1 C7 122.2(5) . . ?
C6 N1 C7 113.6(4) . . ?
O5B N5 O5A 123.3(5) . . ?
O5B N5 C5 118.3(4) . . ?
O5A N5 C5 118.4(5) . . ?
C26 N21 C22 123.1(5) . . ?
C26 N21 C27 114.1(4) . . ?
C22 N21 C27 122.6(4) . . ?
O25A N25 O25B 123.7(5) . . ?
O25A N25 C25 118.6(4) . . ?
O25B N25 C25 117.7(5) . . ?
C6 O6 Si1 114.7(4) . . ?
C26 O26 Si1 113.9(3) . . ?
C9 Si1 O6 95.1(2) . . ?
C9 Si1 C7 120.2(3) . . ?
O6 Si1 C7 85.8(2) . . ?
C9 Si1 C27 116.9(3) . . ?
O6 Si1 C27 89.86(19) . . ?
C7 Si1 C27 122.9(3) . . ?
C9 Si1 O26 96.2(2) . . ?
O6 Si1 O26 168.66(19) . . ?
C7 Si1 O26 88.4(2) . . ?
C27 Si1 O26 85.1(2) . . ?
N31 C32 C33 121.6(5) . . ?
N31 C32 H32 119.2 . . ?
C33 C32 H32 119.2 . . ?
C32 C33 C34 116.1(5) . . ?
C32 C33 C38 121.4(5) . . ?
C34 C33 C38 122.5(5) . . ?
C35 C34 C33 121.7(5) . . ?
C35 C34 H34 119.1 . . ?
C33 C34 H34 119.1 . . ?
C34 C35 C36 120.8(5) . . ?
C34 C35 N35 118.4(5) . . ?
C36 C35 N35 120.8(5) . . ?
O36 C36 N31 116.7(5) . . ?
O36 C36 C35 127.3(5) . . ?
N31 C36 C35 116.0(5) . . ?
N31 C37 Si2 107.6(3) . . ?
N31 C37 H37A 110.2 . . ?
Si2 C37 H37A 110.2 . . ?
N31 C37 H37B 110.2 . . ?
Si2 C37 H37B 110.2 . . ?
H37A C37 H37B 108.5 . . ?
C33 C38 H38A 109.5 . . ?
C33 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C33 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
Si2 C39 H39A 109.5 . . ?
Si2 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
Si2 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N41 C42 C43 121.9(5) . . ?
N41 C42 H42 119.1 . . ?
C43 C42 H42 119.1 . . ?
C44 C43 C42 115.7(5) . . ?
C44 C43 C48 122.7(5) . . ?
C42 C43 C48 121.5(5) . . ?
C45 C44 C43 122.4(5) . . ?
C45 C44 H44 118.8 . . ?
C43 C44 H44 118.8 . . ?
C44 C45 C46 121.5(5) . . ?
C44 C45 N45 119.1(5) . . ?
C46 C45 N45 119.4(5) . . ?
O46 C46 N41 117.0(5) . . ?
O46 C46 C45 128.3(5) . . ?
N41 C46 C45 114.7(5) . . ?
N41 C47 Si2 107.5(3) . . ?
N41 C47 H47A 110.2 . . ?
Si2 C47 H47A 110.2 . . ?
N41 C47 H47B 110.2 . . ?
Si2 C47 H47B 110.2 . . ?
H47A C47 H47B 108.5 . . ?
C43 C48 H48A 109.5 . . ?
C43 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C43 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C32 N31 C36 123.4(5) . . ?
C32 N31 C37 122.3(4) . . ?
C36 N31 C37 114.1(4) . . ?
O35B N35 O35A 123.7(5) . . ?
O35B N35 C35 119.3(4) . . ?
O35A N35 C35 117.1(5) . . ?
C42 N41 C46 123.7(5) . . ?
C42 N41 C47 121.9(4) . . ?
C46 N41 C47 114.3(4) . . ?
O45A N45 O45B 123.2(5) . . ?
O45A N45 C45 119.9(5) . . ?
O45B N45 C45 116.9(5) . . ?
C36 O36 Si2 114.7(3) . . ?
C46 O46 Si2 114.6(3) . . ?
C39 Si2 O46 95.3(2) . . ?
C39 Si2 C47 119.3(3) . . ?
O46 Si2 C47 86.1(2) . . ?
C39 Si2 O36 96.3(2) . . ?
O46 Si2 O36 168.39(18) . . ?
C47 Si2 O36 88.2(2) . . ?
C39 Si2 C37 117.5(3) . . ?
O46 Si2 C37 90.01(19) . . ?
C47 Si2 C37 123.2(3) . . ?
O36 Si2 C37 84.7(2) . . ?
O91 C91 H91A 109.5 . . ?
O91 C91 H91B 109.5 . . ?
H91A C91 H91B 109.5 . . ?
O91 C91 H91C 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
C91 O91 H91 109.5 . . ?
O92 C92 H92A 109.5 . . ?
O92 C92 H92B 109.5 . . ?
H92A C92 H92B 109.5 . . ?
O92 C92 H92C 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
C92 O92 H92 109.5 . . ?

loop_
 _geom_hbond_atom_site_label_D
 _geom_hbond_atom_site_label_H
 _geom_hbond_atom_site_label_A
 _geom_hbond_distance_DH
 _geom_hbond_distance_HA
 _geom_hbond_distance_DA
 _geom_hbond_angle_DHA
 _geom_hbond_site_symmetry_A
O91 H91 Cl1  0.84 2.39 3.173(6) 154.9 .
O92 H92 Cl2  0.84 2.37 3.164(6) 158.1 .
 
_diffrn_measured_fraction_theta_max    0.912
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.912
_refine_diff_density_max    0.673
_refine_diff_density_min   -0.657
_refine_diff_density_rms    0.118
