# Electronic Supplementary Material (ESI) for Polymer Chemistry.
# 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_KN-Si(e-Cl)4
_database_code_depnum_ccdc_archive 'CCDC 1058156'
_audit_update_record             
;
2015-04-07 deposited with the CCDC.
2015-07-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H40 N4 O4 Si'
_chemical_formula_sum            'C24 H40 N4 O4 Si'
_chemical_formula_weight         476.69

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

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

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

_cell_length_a                   18.1083(7)
_cell_length_b                   17.6737(9)
_cell_length_c                   7.6710(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2455.03(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    110
_cell_measurement_reflns_used    2791
_cell_measurement_theta_min      3.5570
_cell_measurement_theta_max      27.6810

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_F_000             1032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    0.133
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.55157
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      110
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         2
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  10
_diffrn_standards_decay_%        0
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10195
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.895
_diffrn_reflns_theta_max         25.495
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_point_group_measured_fraction_full 0.920
_reflns_number_total             4209
_reflns_number_gt                3463
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.709
_reflns_Friedel_fraction_max     0.829
_reflns_Friedel_fraction_full    0.829

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0767P)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_abs_structure_details 
;
 Flack x determined using 1205 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.05(12)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4209
_refine_ls_number_parameters     298
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0562
_refine_ls_wR_factor_ref         0.1384
_refine_ls_wR_factor_gt          0.1307
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_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
C1 C 0.3587(2) 0.1064(3) 0.4355(6) 0.0173(10) Uani 1 1 d . . . . .
C2 C 0.4111(2) 0.0643(3) 0.3177(6) 0.0228(10) Uani 1 1 d . . . . .
H2A H 0.4401 0.1006 0.2521 0.027 Uiso 1 1 calc R U . . .
H2B H 0.3826 0.0347 0.2350 0.027 Uiso 1 1 calc R U . . .
C3 C 0.4638(2) 0.0112(3) 0.4171(6) 0.0224(10) Uani 1 1 d . . . . .
H3A H 0.5086 0.0049 0.3492 0.027 Uiso 1 1 calc R U . . .
H3B H 0.4773 0.0349 0.5266 0.027 Uiso 1 1 calc R U . . .
C4 C 0.4313(2) -0.0663(2) 0.4549(6) 0.0230(11) Uani 1 1 d . . . . .
H4A H 0.4695 -0.0978 0.5059 0.028 Uiso 1 1 calc R U . . .
H4B H 0.4168 -0.0894 0.3454 0.028 Uiso 1 1 calc R U . . .
C5 C 0.3641(2) -0.0658(3) 0.5779(6) 0.0225(10) Uani 1 1 d . . . . .
H5A H 0.3457 -0.1171 0.5888 0.027 Uiso 1 1 calc R U . . .
H5B H 0.3802 -0.0495 0.6925 0.027 Uiso 1 1 calc R U . . .
C6 C 0.3012(2) -0.0152(3) 0.5192(6) 0.0200(10) Uani 1 1 d . . . . .
H6A H 0.2922 -0.0244 0.3964 0.024 Uiso 1 1 calc R U . . .
H6B H 0.2570 -0.0298 0.5821 0.024 Uiso 1 1 calc R U . . .
C7 C 0.2381(2) 0.0197(2) 0.9235(6) 0.0184(10) Uani 1 1 d . . . . .
C8 C 0.1958(2) -0.0317(3) 1.0454(6) 0.0212(10) Uani 1 1 d . . . . .
H8A H 0.1647 -0.0011 1.1203 0.025 Uiso 1 1 calc R U . . .
H8B H 0.2306 -0.0586 1.1190 0.025 Uiso 1 1 calc R U . . .
C9 C 0.1476(2) -0.0893(3) 0.9483(6) 0.0249(11) Uani 1 1 d . . . . .
H9A H 0.1742 -0.1067 0.8461 0.030 Uiso 1 1 calc R U . . .
H9B H 0.1398 -0.1327 1.0234 0.030 Uiso 1 1 calc R U . . .
C10 C 0.0726(2) -0.0591(3) 0.8905(7) 0.0257(11) Uani 1 1 d . . . . .
H10A H 0.0454 -0.1002 0.8364 0.031 Uiso 1 1 calc R U . . .
H10B H 0.0453 -0.0438 0.9935 0.031 Uiso 1 1 calc R U . . .
C11 C 0.0743(2) 0.0066(3) 0.7653(6) 0.0228(11) Uani 1 1 d . . . . .
H11A H 0.0240 0.0232 0.7446 0.027 Uiso 1 1 calc R U . . .
H11B H 0.0941 -0.0109 0.6549 0.027 Uiso 1 1 calc R U . . .
C12 C 0.1194(2) 0.0743(3) 0.8257(6) 0.0209(10) Uani 1 1 d . . . . .
H12A H 0.1047 0.1183 0.7585 0.025 Uiso 1 1 calc R U . . .
H12B H 0.1079 0.0844 0.9470 0.025 Uiso 1 1 calc R U . . .
C13 C 0.1573(2) 0.1394(3) 0.4249(6) 0.0180(10) Uani 1 1 d . . . . .
C14 C 0.1069(2) 0.1820(3) 0.3045(6) 0.0213(10) Uani 1 1 d . . . . .
H14A H 0.0816 0.1460 0.2300 0.026 Uiso 1 1 calc R U . . .
H14B H 0.1366 0.2144 0.2303 0.026 Uiso 1 1 calc R U . . .
C15 C 0.0494(2) 0.2305(3) 0.3977(6) 0.0227(11) Uani 1 1 d . . . . .
H15A H 0.0076 0.2377 0.3203 0.027 Uiso 1 1 calc R U . . .
H15B H 0.0318 0.2031 0.4992 0.027 Uiso 1 1 calc R U . . .
C16 C 0.0770(2) 0.3074(3) 0.4560(6) 0.0244(10) Uani 1 1 d . . . . .
H16A H 0.0360 0.3349 0.5069 0.029 Uiso 1 1 calc R U . . .
H16B H 0.0930 0.3353 0.3537 0.029 Uiso 1 1 calc R U . . .
C17 C 0.1402(2) 0.3065(3) 0.5869(6) 0.0230(10) Uani 1 1 d . . . . .
H17A H 0.1553 0.3583 0.6094 0.028 Uiso 1 1 calc R U . . .
H17B H 0.1222 0.2856 0.6958 0.028 Uiso 1 1 calc R U . . .
C18 C 0.2073(2) 0.2617(2) 0.5298(6) 0.0190(10) Uani 1 1 d . . . . .
H18A H 0.2185 0.2747 0.4098 0.023 Uiso 1 1 calc R U . . .
H18B H 0.2491 0.2772 0.6004 0.023 Uiso 1 1 calc R U . . .
C19 C 0.2698(2) 0.2239(2) 0.9275(5) 0.0175(10) Uani 1 1 d . . . . .
C20 C 0.3099(2) 0.2740(3) 1.0549(6) 0.0211(10) Uani 1 1 d . . . . .
H20A H 0.3402 0.2429 1.1305 0.025 Uiso 1 1 calc R U . . .
H20B H 0.2740 0.3000 1.1271 0.025 Uiso 1 1 calc R U . . .
C21 C 0.3594(2) 0.3332(3) 0.9633(7) 0.0253(11) Uani 1 1 d . . . . .
H21A H 0.3349 0.3502 0.8578 0.030 Uiso 1 1 calc R U . . .
H21B H 0.3650 0.3767 1.0393 0.030 Uiso 1 1 calc R U . . .
C22 C 0.4357(2) 0.3032(3) 0.9161(6) 0.0270(11) Uani 1 1 d . . . . .
H22A H 0.4645 0.3444 0.8671 0.032 Uiso 1 1 calc R U . . .
H22B H 0.4602 0.2869 1.0221 0.032 Uiso 1 1 calc R U . . .
C23 C 0.4354(2) 0.2378(3) 0.7872(6) 0.0236(11) Uani 1 1 d . . . . .
H23A H 0.4175 0.2564 0.6760 0.028 Uiso 1 1 calc R U . . .
H23B H 0.4860 0.2212 0.7700 0.028 Uiso 1 1 calc R U . . .
C24 C 0.3896(2) 0.1701(3) 0.8386(6) 0.0209(10) Uani 1 1 d . . . . .
H24A H 0.4055 0.1270 0.7699 0.025 Uiso 1 1 calc R U . . .
H24B H 0.3994 0.1585 0.9600 0.025 Uiso 1 1 calc R U . . .
N1 N 0.31268(18) 0.0663(2) 0.5439(5) 0.0173(8) Uani 1 1 d . . . . .
N2 N 0.19997(18) 0.0643(2) 0.8087(5) 0.0165(8) Uani 1 1 d . . . . .
N3 N 0.19982(18) 0.1787(2) 0.5422(5) 0.0161(8) Uani 1 1 d . . . . .
N4 N 0.30924(18) 0.1796(2) 0.8159(5) 0.0178(8) Uani 1 1 d . . . . .
O1 O 0.35853(16) 0.17641(17) 0.4420(4) 0.0226(7) Uani 1 1 d . . . . .
O2 O 0.30588(15) 0.01898(18) 0.9216(4) 0.0237(8) Uani 1 1 d . . . . .
O3 O 0.15775(16) 0.06982(17) 0.4283(4) 0.0214(7) Uani 1 1 d . . . . .
O4 O 0.20196(16) 0.22383(17) 0.9198(4) 0.0218(7) Uani 1 1 d . . . . .
Si1 Si 0.25558(5) 0.12226(6) 0.67739(18) 0.0155(3) 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
C1 O1 1.238(5) . ?
C1 N1 1.374(5) . ?
C1 C2 1.507(6) . ?
C2 C3 1.541(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.519(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.540(6) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.517(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N1 1.468(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 O2 1.227(5) . ?
C7 N2 1.368(6) . ?
C7 C8 1.512(6) . ?
C8 C9 1.534(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.525(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.508(7) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.521(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 N2 1.475(5) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 O3 1.229(5) . ?
C13 N3 1.373(6) . ?
C13 C14 1.501(6) . ?
C14 C15 1.527(6) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.517(6) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.523(6) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.516(6) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 N3 1.475(5) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 O4 1.231(5) . ?
C19 N4 1.362(6) . ?
C19 C20 1.505(6) . ?
C20 C21 1.547(6) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.523(6) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.522(7) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.508(6) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 N4 1.475(5) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
N1 Si1 1.759(4) . ?
N2 Si1 1.755(4) . ?
N3 Si1 1.758(4) . ?
N4 Si1 1.760(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
O1 C1 N1 119.3(4) . . ?
O1 C1 C2 121.3(4) . . ?
N1 C1 C2 119.3(4) . . ?
C1 C2 C3 113.2(4) . . ?
C1 C2 H2A 108.9 . . ?
C3 C2 H2A 108.9 . . ?
C1 C2 H2B 108.9 . . ?
C3 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
C4 C3 C2 113.8(4) . . ?
C4 C3 H3A 108.8 . . ?
C2 C3 H3A 108.8 . . ?
C4 C3 H3B 108.8 . . ?
C2 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
C3 C4 C5 114.7(4) . . ?
C3 C4 H4A 108.6 . . ?
C5 C4 H4A 108.6 . . ?
C3 C4 H4B 108.6 . . ?
C5 C4 H4B 108.6 . . ?
H4A C4 H4B 107.6 . . ?
C6 C5 C4 114.5(4) . . ?
C6 C5 H5A 108.6 . . ?
C4 C5 H5A 108.6 . . ?
C6 C5 H5B 108.6 . . ?
C4 C5 H5B 108.6 . . ?
H5A C5 H5B 107.6 . . ?
N1 C6 C5 115.8(4) . . ?
N1 C6 H6A 108.3 . . ?
C5 C6 H6A 108.3 . . ?
N1 C6 H6B 108.3 . . ?
C5 C6 H6B 108.3 . . ?
H6A C6 H6B 107.4 . . ?
O2 C7 N2 120.2(4) . . ?
O2 C7 C8 120.5(4) . . ?
N2 C7 C8 119.2(4) . . ?
C7 C8 C9 112.7(4) . . ?
C7 C8 H8A 109.0 . . ?
C9 C8 H8A 109.0 . . ?
C7 C8 H8B 109.0 . . ?
C9 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C10 C9 C8 114.6(4) . . ?
C10 C9 H9A 108.6 . . ?
C8 C9 H9A 108.6 . . ?
C10 C9 H9B 108.6 . . ?
C8 C9 H9B 108.6 . . ?
H9A C9 H9B 107.6 . . ?
C11 C10 C9 115.9(4) . . ?
C11 C10 H10A 108.3 . . ?
C9 C10 H10A 108.3 . . ?
C11 C10 H10B 108.3 . . ?
C9 C10 H10B 108.3 . . ?
H10A C10 H10B 107.4 . . ?
C10 C11 C12 115.0(4) . . ?
C10 C11 H11A 108.5 . . ?
C12 C11 H11A 108.5 . . ?
C10 C11 H11B 108.5 . . ?
C12 C11 H11B 108.5 . . ?
H11A C11 H11B 107.5 . . ?
N2 C12 C11 114.3(4) . . ?
N2 C12 H12A 108.7 . . ?
C11 C12 H12A 108.7 . . ?
N2 C12 H12B 108.7 . . ?
C11 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
O3 C13 N3 119.3(4) . . ?
O3 C13 C14 121.3(4) . . ?
N3 C13 C14 119.3(4) . . ?
C13 C14 C15 114.1(4) . . ?
C13 C14 H14A 108.7 . . ?
C15 C14 H14A 108.7 . . ?
C13 C14 H14B 108.7 . . ?
C15 C14 H14B 108.7 . . ?
H14A C14 H14B 107.6 . . ?
C16 C15 C14 114.6(4) . . ?
C16 C15 H15A 108.6 . . ?
C14 C15 H15A 108.6 . . ?
C16 C15 H15B 108.6 . . ?
C14 C15 H15B 108.6 . . ?
H15A C15 H15B 107.6 . . ?
C15 C16 C17 115.7(4) . . ?
C15 C16 H16A 108.4 . . ?
C17 C16 H16A 108.4 . . ?
C15 C16 H16B 108.4 . . ?
C17 C16 H16B 108.4 . . ?
H16A C16 H16B 107.4 . . ?
C18 C17 C16 114.6(4) . . ?
C18 C17 H17A 108.6 . . ?
C16 C17 H17A 108.6 . . ?
C18 C17 H17B 108.6 . . ?
C16 C17 H17B 108.6 . . ?
H17A C17 H17B 107.6 . . ?
N3 C18 C17 115.3(3) . . ?
N3 C18 H18A 108.4 . . ?
C17 C18 H18A 108.4 . . ?
N3 C18 H18B 108.4 . . ?
C17 C18 H18B 108.4 . . ?
H18A C18 H18B 107.5 . . ?
O4 C19 N4 119.5(4) . . ?
O4 C19 C20 120.8(4) . . ?
N4 C19 C20 119.6(4) . . ?
C19 C20 C21 112.5(4) . . ?
C19 C20 H20A 109.1 . . ?
C21 C20 H20A 109.1 . . ?
C19 C20 H20B 109.1 . . ?
C21 C20 H20B 109.1 . . ?
H20A C20 H20B 107.8 . . ?
C22 C21 C20 113.5(4) . . ?
C22 C21 H21A 108.9 . . ?
C20 C21 H21A 108.9 . . ?
C22 C21 H21B 108.9 . . ?
C20 C21 H21B 108.9 . . ?
H21A C21 H21B 107.7 . . ?
C23 C22 C21 114.6(4) . . ?
C23 C22 H22A 108.6 . . ?
C21 C22 H22A 108.6 . . ?
C23 C22 H22B 108.6 . . ?
C21 C22 H22B 108.6 . . ?
H22A C22 H22B 107.6 . . ?
C24 C23 C22 115.8(4) . . ?
C24 C23 H23A 108.3 . . ?
C22 C23 H23A 108.3 . . ?
C24 C23 H23B 108.3 . . ?
C22 C23 H23B 108.3 . . ?
H23A C23 H23B 107.4 . . ?
N4 C24 C23 114.9(4) . . ?
N4 C24 H24A 108.5 . . ?
C23 C24 H24A 108.5 . . ?
N4 C24 H24B 108.5 . . ?
C23 C24 H24B 108.5 . . ?
H24A C24 H24B 107.5 . . ?
C1 N1 C6 120.9(4) . . ?
C1 N1 Si1 114.8(3) . . ?
C6 N1 Si1 122.9(3) . . ?
C7 N2 C12 120.7(4) . . ?
C7 N2 Si1 114.6(3) . . ?
C12 N2 Si1 123.3(3) . . ?
C13 N3 C18 120.9(4) . . ?
C13 N3 Si1 114.9(3) . . ?
C18 N3 Si1 123.3(3) . . ?
C19 N4 C24 120.5(4) . . ?
C19 N4 Si1 114.9(3) . . ?
C24 N4 Si1 123.4(3) . . ?
N2 Si1 N3 109.92(16) . . ?
N2 Si1 N1 110.08(18) . . ?
N3 Si1 N1 108.24(19) . . ?
N2 Si1 N4 107.84(19) . . ?
N3 Si1 N4 110.28(17) . . ?
N1 Si1 N4 110.49(16) . . ?

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
O1 C1 C2 C3 119.3(4) . . . . ?
N1 C1 C2 C3 -57.5(5) . . . . ?
C1 C2 C3 C4 85.1(5) . . . . ?
C2 C3 C4 C5 -64.4(5) . . . . ?
C3 C4 C5 C6 55.2(5) . . . . ?
C4 C5 C6 N1 -75.3(5) . . . . ?
O2 C7 C8 C9 -117.0(5) . . . . ?
N2 C7 C8 C9 59.7(5) . . . . ?
C7 C8 C9 C10 -83.2(5) . . . . ?
C8 C9 C10 C11 61.1(6) . . . . ?
C9 C10 C11 C12 -54.2(6) . . . . ?
C10 C11 C12 N2 76.8(5) . . . . ?
O3 C13 C14 C15 116.2(5) . . . . ?
N3 C13 C14 C15 -59.2(5) . . . . ?
C13 C14 C15 C16 83.0(5) . . . . ?
C14 C15 C16 C17 -61.6(5) . . . . ?
C15 C16 C17 C18 55.0(5) . . . . ?
C16 C17 C18 N3 -76.3(5) . . . . ?
O4 C19 C20 C21 -117.1(4) . . . . ?
N4 C19 C20 C21 61.0(5) . . . . ?
C19 C20 C21 C22 -85.0(5) . . . . ?
C20 C21 C22 C23 62.4(6) . . . . ?
C21 C22 C23 C24 -55.3(6) . . . . ?
C22 C23 C24 N4 76.6(5) . . . . ?
O1 C1 N1 C6 168.9(4) . . . . ?
C2 C1 N1 C6 -14.2(6) . . . . ?
O1 C1 N1 Si1 2.0(5) . . . . ?
C2 C1 N1 Si1 178.9(3) . . . . ?
C5 C6 N1 C1 75.4(5) . . . . ?
C5 C6 N1 Si1 -118.8(4) . . . . ?
O2 C7 N2 C12 -171.1(4) . . . . ?
C8 C7 N2 C12 12.2(6) . . . . ?
O2 C7 N2 Si1 -4.3(5) . . . . ?
C8 C7 N2 Si1 179.0(3) . . . . ?
C11 C12 N2 C7 -75.6(5) . . . . ?
C11 C12 N2 Si1 118.8(4) . . . . ?
O3 C13 N3 C18 173.1(4) . . . . ?
C14 C13 N3 C18 -11.5(5) . . . . ?
O3 C13 N3 Si1 3.9(5) . . . . ?
C14 C13 N3 Si1 179.3(3) . . . . ?
C17 C18 N3 C13 73.9(5) . . . . ?
C17 C18 N3 Si1 -117.8(4) . . . . ?
O4 C19 N4 C24 -171.2(4) . . . . ?
C20 C19 N4 C24 10.7(6) . . . . ?
O4 C19 N4 Si1 -3.2(5) . . . . ?
C20 C19 N4 Si1 178.7(3) . . . . ?
C23 C24 N4 C19 -73.8(5) . . . . ?
C23 C24 N4 Si1 119.2(4) . . . . ?
C7 N2 Si1 N3 -177.9(3) . . . . ?
C12 N2 Si1 N3 -11.5(4) . . . . ?
C7 N2 Si1 N1 63.0(4) . . . . ?
C12 N2 Si1 N1 -130.7(3) . . . . ?
C7 N2 Si1 N4 -57.7(3) . . . . ?
C12 N2 Si1 N4 108.7(4) . . . . ?
C13 N3 Si1 N2 -63.1(3) . . . . ?
C18 N3 Si1 N2 127.9(3) . . . . ?
C13 N3 Si1 N1 57.1(3) . . . . ?
C18 N3 Si1 N1 -111.8(3) . . . . ?
C13 N3 Si1 N4 178.1(3) . . . . ?
C18 N3 Si1 N4 9.2(4) . . . . ?
C1 N1 Si1 N2 -180.0(3) . . . . ?
C6 N1 Si1 N2 13.4(4) . . . . ?
C1 N1 Si1 N3 59.9(3) . . . . ?
C6 N1 Si1 N3 -106.7(3) . . . . ?
C1 N1 Si1 N4 -61.0(4) . . . . ?
C6 N1 Si1 N4 132.4(3) . . . . ?
C19 N4 Si1 N2 -58.2(3) . . . . ?
C24 N4 Si1 N2 109.4(4) . . . . ?
C19 N4 Si1 N3 61.8(4) . . . . ?
C24 N4 Si1 N3 -130.6(3) . . . . ?
C19 N4 Si1 N1 -178.6(3) . . . . ?
C24 N4 Si1 N1 -11.0(4) . . . . ?

_refine_diff_density_max         0.683
_refine_diff_density_min         -0.262
_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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1058182'
_audit_update_record             
;
2015-04-07 deposited with the CCDC.
2015-07-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H40 N4 O4 Si'
_chemical_formula_sum            'C24 H40 N4 O4 Si'
_chemical_formula_weight         476.69

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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_H-M_alt        'I -4 2 d'
_space_group_name_Hall           'I -4 2bw'

_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'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'x+1/2, -y, -z+3/4'
'-y+1/2, -x, z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1, y+1/2, -z+5/4'
'x+1, -y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'y+1, x+1/2, z+5/4'

_cell_length_a                   13.9688(3)
_cell_length_b                   13.9688(3)
_cell_length_c                   13.3347(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2601.97(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    110
_cell_measurement_reflns_used    2460
_cell_measurement_theta_min      3.0491
_cell_measurement_theta_max      28.5752

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_F_000             1032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_exptl_absorpt_coefficient_mu    0.126
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.88537
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      110
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3191
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.602
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        25.000
_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 0.958
_diffrn_reflns_point_group_measured_fraction_full 0.958
_reflns_number_total             1107
_reflns_number_gt                1060
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.700
_reflns_Friedel_fraction_max     0.914
_reflns_Friedel_fraction_full    0.914

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0344P)²+0.6068P] 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_abs_structure_details 
;
 Flack x determined using 427 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.35(9)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1107
_refine_ls_number_parameters     75
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0263
_refine_ls_wR_factor_ref         0.0650
_refine_ls_wR_factor_gt          0.0639
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_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 1.5000 1.0000 1.2500 0.0204(3) Uani 1 4 d S T P . .
O1 O 1.46927(9) 1.09118(10) 1.18015(9) 0.0243(4) Uani 1 1 d . . . . .
N2 N 1.55231(12) 1.11749(12) 1.11965(13) 0.0264(4) Uani 1 1 d . . . . .
C6 C 1.42856(15) 1.18268(14) 1.00361(15) 0.0263(5) Uani 1 1 d . . . . .
H6A H 1.4138 1.2498 1.0143 0.032 Uiso 1 1 calc R U . . .
H6B H 1.3829 1.1449 1.0415 0.032 Uiso 1 1 calc R U . . .
C2 C 1.60943(15) 1.19822(16) 0.97722(15) 0.0312(5) Uani 1 1 d . . . . .
H2A H 1.6689 1.1707 1.0014 0.037 Uiso 1 1 calc R U . . .
H2B H 1.6139 1.2672 0.9839 0.037 Uiso 1 1 calc R U . . .
C1 C 1.52785(14) 1.16211(14) 1.04030(15) 0.0245(5) Uani 1 1 d . . . . .
C4 C 1.4985(2) 1.20564(19) 0.83059(15) 0.0419(6) Uani 1 1 d . . . . .
H4A H 1.4909 1.1889 0.7604 0.050 Uiso 1 1 calc R U . . .
H4B H 1.4939 1.2747 0.8365 0.050 Uiso 1 1 calc R U . . .
C3 C 1.59637(17) 1.17266(17) 0.86718(17) 0.0388(6) Uani 1 1 d . . . . .
H3A H 1.6021 1.1039 0.8587 0.047 Uiso 1 1 calc R U . . .
H3B H 1.6461 1.2031 0.8276 0.047 Uiso 1 1 calc R U . . .
C5 C 1.41922(18) 1.15893(19) 0.89183(18) 0.0401(6) Uani 1 1 d . . . . .
H5A H 1.4219 1.0901 0.8829 0.048 Uiso 1 1 calc R U . . .
H5B H 1.3576 1.1810 0.8676 0.048 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 O1 1.6353(13) . ?
Si1 O1 1.6353(13) 11_577 ?
Si1 O1 1.6353(13) 2_875 ?
Si1 O1 1.6353(13) 12_747 ?
O1 N2 1.460(2) . ?
N2 C1 1.275(3) . ?
C6 C1 1.498(3) . ?
C6 C5 1.533(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C2 C1 1.504(3) . ?
C2 C3 1.521(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C4 C3 1.523(3) . ?
C4 C5 1.523(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Si1 O1 108.93(4) . 11_577 ?
O1 Si1 O1 110.56(9) . 2_875 ?
O1 Si1 O1 108.93(4) 11_577 2_875 ?
O1 Si1 O1 108.93(4) . 12_747 ?
O1 Si1 O1 110.56(9) 11_577 12_747 ?
O1 Si1 O1 108.93(4) 2_875 12_747 ?
N2 O1 Si1 107.59(10) . . ?
C1 N2 O1 111.64(15) . . ?
C1 C6 C5 110.78(18) . . ?
C1 C6 H6A 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C1 C6 H6B 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
C1 C2 C3 111.71(18) . . ?
C1 C2 H2A 109.3 . . ?
C3 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
C3 C2 H2B 109.3 . . ?
H2A C2 H2B 107.9 . . ?
N2 C1 C6 127.80(18) . . ?
N2 C1 C2 115.16(17) . . ?
C6 C1 C2 117.04(16) . . ?
C3 C4 C5 110.58(19) . . ?
C3 C4 H4A 109.5 . . ?
C5 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C5 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
C2 C3 C4 110.23(18) . . ?
C2 C3 H3A 109.6 . . ?
C4 C3 H3A 109.6 . . ?
C2 C3 H3B 109.6 . . ?
C4 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
C4 C5 C6 111.52(19) . . ?
C4 C5 H5A 109.3 . . ?
C6 C5 H5A 109.3 . . ?
C4 C5 H5B 109.3 . . ?
C6 C5 H5B 109.3 . . ?
H5A C5 H5B 108.0 . . ?

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
O1 Si1 O1 N2 58.71(8) 11_577 . . . ?
O1 Si1 O1 N2 -60.95(9) 2_875 . . . ?
O1 Si1 O1 N2 179.38(11) 12_747 . . . ?
Si1 O1 N2 C1 156.50(14) . . . . ?
O1 N2 C1 C6 -4.0(3) . . . . ?
O1 N2 C1 C2 175.75(16) . . . . ?
C5 C6 C1 N2 -133.3(2) . . . . ?
C5 C6 C1 C2 47.0(2) . . . . ?
C3 C2 C1 N2 131.8(2) . . . . ?
C3 C2 C1 C6 -48.4(2) . . . . ?
C1 C2 C3 C4 52.8(2) . . . . ?
C5 C4 C3 C2 -59.1(3) . . . . ?
C3 C4 C5 C6 58.8(3) . . . . ?
C1 C6 C5 C4 -51.1(3) . . . . ?

_refine_diff_density_max         0.131
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.026


# start Validation Reply Form
_vrf_STRVA01_shelx               
;
PROBLEM: Flack test results are ambiguous.
RESPONSE: With a value of:
_refine_ls_abs_structure_Flack    0.35(9)
not only the absolute structure seems to be wrongly
determined. 
A level G alert claimes further:
ADDSYM Detects (Pseudo) Centre of Symmetry .....         88 %Fit.

Indeed, PLATON (ADDSYM) suggests the centrosymmetric space group
I4(1)/amd (No 141), although ADDSYM-EXT does not claim the
used space group to be wrong.

All trials to solve/refine the structure in No 141 gave non-reliable
results. Thereby, the possibilities of statistical and/or dynamical 
disorder, the presence of a racemic and/or inversion twin has been
taken into account.

Of all measured reflections a unit cell search revealed 96.5 % of
all reflections to belong to the tI lattice - which should indicate that
the crystals was not twinned. After data integration the following
value for the E statistic were observed -
<[E*E-1]>           exp      0.741
         ideal acentric      0.736
         ideal centric       0.968

which indicate the space group to be non-centrosymmetric.

By solving the structure with:

                           Superflip
                    Version: 04/17/13 12:45
Palatinus, L. & Chapuis, G.(2007): J. Appl. Cryst. 40, 786-790
              http://superspace.epfl.ch/superflip

the following output was observed:

Symmetry operations compatible with the lattice and centering:
                      Symmetry operation             agreement factor
       d(1,-1,0):        3/4+x2       3/4+x1       1/4+x3    0.081    
        2(1,0,0):            x1          -x2          -x3    0.093    
       -4(0,0,1):           -x2           x1          -x3    0.094    
       -4(0,0,1):            x2          -x1          -x3    0.098    
        2(0,1,0):           -x1           x2          -x3    0.120    
        d(1,1,0):        1/4-x2       3/4-x1       1/4+x3    0.123    
        2(0,0,1):           -x1          -x2           x3    0.132    

        m(0,1,0):            x1          -x2           x3   54.454    
        .
        .
        .

The threshold set automatically for acceptance of symmtry operations
is 25 % (agreement factor), which indicates that no further 
symmetry operation other than the used ones is applicable.

It was tried further to integrate the data and to solve/refine in 
oI and/or mI space groups, which might emulate a tI lattice.
Even in such case no reliable solution/refinement was obtained.


It is thus supposed that the lattice/space group used is correct.

;

# end Validation Reply Form

_shelxl_version_number           2013-4

