Supplementary Material (ESI) for Chemical Communications
This journal is (c) The Royal Society of Chemistry 2001


data_TBDMS-G

_database_code_CSD	168941


_journal_coden_Cambridge      182

_publ_requested_journal       'Chemical Communications'

loop_
_publ_author_name
'Araki, K.'
'Takasawa, Ryoichi'
'Yoshikawa, Isao'


_publ_section_title
;
Design, Fabrication, and Properties of Macroscale 
Supramolecular Fibers consisted of Fully Hydrogen-bonded 
Pseudo-polymer Chains
;



_publ_contact_author_name  'Prof K Araki'

_publ_contact_author_address
;
Institute of Industrial Science, University of Tokyo,
4-6-1 Komaba, Meguro-ku, Tokyo 153-8505, Japan
;

_publ_contact_author_email  'araki@iis.u-tokyo.ac.jp'
_publ_contact_author_fax      '+81-3-5452-6364'

_publ_section_title		
;
Design, Fabrication, and properties of macroscale supramolecular
fibers consisted of fully hydrogen-bonded pseudo-polymer chains.
;


#========================================================

#========================================================

#CHEMICAL DATA

_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
2',3',5'-O-tris(tert-butyldimethylsilyl)-guanosine
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety         'C28 H55 O5 N5 Si3'
_chemical_formula_sum            'C32 H63 O6 N5 Si3'
_chemical_formula_weight          698.14

loop_ 
_atom_type_symbol 
_atom_type_description 
_atom_type_scat_dispersion_real 
_atom_type_scat_dispersion_imag 
_atom_type_scat_source 
'C'  'C'   0.0181   0.0091 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'H'  'H'   0.0000   0.0000 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'O'  'O'   0.0492   0.0322 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'N'  'N'   0.0311   0.0180 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'Si'  'Si'   0.2541   0.3302 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

#CRYSTAL DATA

_symmetry_cell_setting            'Orthorhombic' 
_symmetry_space_group_name_H-M    'P 21 21 21' 

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

_cell_length_a                    11.47600(10) 
_cell_length_b                    18.5090(2) 
_cell_length_c                    19.3310(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      4106.08(7) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     100 
_cell_measurement_reflns_used     46625 
_cell_measurement_theta_min       3.31 
_cell_measurement_theta_max       73.24 

_exptl_crystal_description        'needle' 
_exptl_crystal_colour             'Colourless' 
_exptl_crystal_size_max           0.35 
_exptl_crystal_size_mid           0.21 
_exptl_crystal_size_min           0.17 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.129 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1520 
_exptl_absorpt_coefficient_mu     1.414 
_exptl_absorpt_correction_type    'integration' 
_exptl_absorpt_correction_T_min   0.7432 
_exptl_absorpt_correction_T_max   0.7902 
_exptl_absorpt_process_details    ? 

_exptl_special_details 
; 
? 
; 

#EXPERIMENTAL DATA

_diffrn_ambient_temperature       100 
_diffrn_radiation_wavelength      1.54180 
_diffrn_radiation_type            CuK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'MacScience DIP-Labo' 
_diffrn_measurement_method        'IP' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             46625 
_diffrn_reflns_av_R_equivalents   0.039 
_diffrn_reflns_av_sigmaI/netI     0.0168 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        22 
_diffrn_reflns_limit_l_min        -23 
_diffrn_reflns_limit_l_max        23 
_diffrn_reflns_theta_min          3.31 
_diffrn_reflns_theta_max          73.24 
_reflns_number_total              7920 
_reflns_number_gt                 7804 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        'MacScience Xpress' 
_computing_cell_refinement        'Denzo and Scalepack' 
_computing_data_reduction         'Denzo and Scalepack' 
_computing_structure_solution     'SIR92' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'maXus' 
_computing_publication_material   ? 

#REFINEMENT DATA

_refine_special_details 
; 
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
goodness of fit S are based on F^2^, conventional R-factors R are based 
on F, with F set to zero for negative F^2^. The threshold expression of 
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F^2^ 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/[\s^2^(Fo^2^)+(0.0542P)^2^+3.6840P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.19(2) 
_refine_ls_number_reflns          7920 
_refine_ls_number_parameters      478 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0449 
_refine_ls_R_factor_gt            0.0434 
_refine_ls_wR_factor_ref          0.1202 
_refine_ls_wR_factor_gt           0.1132 
_refine_ls_goodness_of_fit_ref    1.093 
_refine_ls_restrained_S_all       1.093 
_refine_ls_shift/su_max           0.009 
_refine_ls_shift/su_mean          0.001 

_refine_diff_density_max    0.249 
_refine_diff_density_min   -0.377 
_refine_diff_density_rms    0.065 

#ATOM COORDINATES AND THERMAL PARAMETERS

loop_ 
_atom_site_label 
_atom_site_type_symbol 
_atom_site_fract_x 
_atom_site_fract_y 
_atom_site_fract_z 
_atom_site_U_iso_or_equiv 
_atom_site_adp_type 
_atom_site_occupancy 
_atom_site_symmetry_multiplicity 
_atom_site_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_assembly 
_atom_site_disorder_group 
N1 N 0.29408(18) 0.23013(11) 0.96790(11) 0.0223(4) Uani 1 1 d . . . 
H1 H 0.3531 0.2416 0.9982 0.049(10) Uiso 1 1 d R . . 
C2 C 0.3226(2) 0.19866(13) 0.90570(12) 0.0210(5) Uani 1 1 d . . . 
N2 N 0.43602(18) 0.18829(12) 0.89262(11) 0.0243(4) Uani 1 1 d . . . 
H2A H 0.4567 0.1748 0.8497 0.031(8) Uiso 1 1 d R . . 
H2B H 0.4931 0.2043 0.9238 0.060(12) Uiso 1 1 d R . . 
N3 N 0.24513(18) 0.17845(11) 0.85890(11) 0.0232(4) Uani 1 1 d . . . 
C4 C 0.1350(2) 0.19286(13) 0.87943(12) 0.0215(5) Uani 1 1 d . . . 
C5 C 0.0980(2) 0.22611(13) 0.93873(13) 0.0231(5) Uani 1 1 d . . . 
C6 C 0.1806(2) 0.24718(13) 0.98944(13) 0.0222(5) Uani 1 1 d . . . 
O6 O 0.16386(15) 0.27640(10) 1.04567(9) 0.0261(4) Uani 1 1 d . . . 
N7 N -0.02378(18) 0.23156(11) 0.93958(11) 0.0233(4) Uani 1 1 d . . . 
C8 C -0.0569(2) 0.20197(15) 0.88152(12) 0.0242(5) Uani 1 1 d . . . 
H8 H -0.1399 0.1962 0.8658 0.049(10) Uiso 1 1 d R . . 
N9 N 0.03485(18) 0.17777(12) 0.84204(10) 0.0232(4) Uani 1 1 d . . . 
C11 C 0.0255(2) 0.13845(13) 0.77789(13) 0.0238(5) Uani 1 1 d . . . 
H11 H -0.0660 0.1427 0.7605 0.024(7) Uiso 1 1 d R . . 
C12 C 0.1035(2) 0.16552(13) 0.71881(12) 0.0220(5) Uani 1 1 d . . . 
H12 H 0.1801 0.1785 0.7367 0.028(8) Uiso 1 1 d R . . 
O12 O 0.05319(16) 0.22518(10) 0.68437(9) 0.0254(4) Uani 1 1 d . . . 
C13 C 0.1132(2) 0.09721(14) 0.67493(13) 0.0249(5) Uani 1 1 d . . . 
H13 H 0.1829 0.0969 0.6411 0.017(6) Uiso 1 1 d R . . 
O13 O 0.00872(16) 0.08613(10) 0.63792(9) 0.0294(4) Uani 1 1 d . . . 
C14 C 0.1255(3) 0.03938(14) 0.73022(14) 0.0278(5) Uani 1 1 d . . . 
H14 H 0.0863 -0.0119 0.7135 0.023(7) Uiso 1 1 d R . . 
O14 O 0.05932(17) 0.06552(10) 0.78936(9) 0.0274(4) Uani 1 1 d . . . 
C15 C 0.2500(3) 0.02605(15) 0.75214(15) 0.0325(6) Uani 1 1 d . . . 
H15A H 0.2520 -0.0100 0.7929 0.018(7) Uiso 1 1 d R . . 
H15B H 0.2892 0.0689 0.7701 0.044(10) Uiso 1 1 d R . . 
O15 O 0.3135(2) 0.00093(11) 0.69371(11) 0.0392(5) Uani 1 1 d . . . 
Si12 Si 0.12185(7) 0.30433(4) 0.68068(4) 0.02820(16) Uani 1 1 d . . . 
C21 C 0.1291(4) 0.34536(18) 0.76843(17) 0.0532(10) Uani 1 1 d . . . 
H21A H 0.1757 0.3159 0.7970 0.056(11) Uiso 1 1 d R . . 
H21B H 0.0532 0.3446 0.7913 0.061(13) Uiso 1 1 d R . . 
H21C H 0.1584 0.3936 0.7691 0.092(17) Uiso 1 1 d R . . 
C22 C 0.2721(3) 0.28969(18) 0.64774(19) 0.0435(8) Uani 1 1 d . . . 
H22A H 0.2752 0.2673 0.5994 0.079(15) Uiso 1 1 d R . . 
H22B H 0.3094 0.2597 0.6804 0.018(6) Uiso 1 1 d R . . 
H22C H 0.3082 0.3353 0.6388 0.061(12) Uiso 1 1 d R . . 
C23 C 0.0327(2) 0.36174(15) 0.62024(14) 0.0302(6) Uani 1 1 d . . . 
C24 C -0.0930(3) 0.3667(2) 0.64575(18) 0.0456(8) Uani 1 1 d . . . 
H24A H -0.1417 0.4036 0.6158 0.085(15) Uiso 1 1 d R . . 
H24B H -0.0979 0.3882 0.6949 0.057(11) Uiso 1 1 d R . . 
H24C H -0.1353 0.3170 0.6474 0.063(12) Uiso 1 1 d R . . 
C25 C 0.0868(3) 0.43776(16) 0.61730(18) 0.0435(8) Uani 1 1 d . . . 
H25A H 0.1787 0.4375 0.5983 0.037(9) Uiso 1 1 d R . . 
H25B H 0.0835 0.4620 0.6625 0.043(10) Uiso 1 1 d R . . 
H25C H 0.0388 0.4713 0.5856 0.051(11) Uiso 1 1 d R . . 
C26 C 0.0319(3) 0.32983(17) 0.54700(15) 0.0370(6) Uani 1 1 d . . . 
H26A H -0.0057 0.2803 0.5451 0.039(9) Uiso 1 1 d R . . 
H26B H -0.0149 0.3611 0.5170 0.044(9) Uiso 1 1 d R . . 
H26C H 0.1157 0.3308 0.5225 0.030(8) Uiso 1 1 d R . . 
Si13 Si -0.01244(6) 0.08524(4) 0.55360(3) 0.02485(15) Uani 1 1 d . . . 
C31 C -0.1468(3) 0.13941(16) 0.53849(17) 0.0384(7) Uani 1 1 d . . . 
H31A H -0.1550 0.1464 0.4916 0.11(2) Uiso 1 1 d R . . 
H31B H -0.1419 0.1866 0.5594 0.097(17) Uiso 1 1 d R . . 
H31C H -0.2148 0.1159 0.5548 0.042(9) Uiso 1 1 d R . . 
C32 C 0.1154(3) 0.12529(17) 0.50807(15) 0.0371(7) Uani 1 1 d . . . 
H32A H 0.0935 0.1292 0.4548 0.067(12) Uiso 1 1 d R . . 
H32B H 0.1298 0.1747 0.5256 0.053(11) Uiso 1 1 d R . . 
H32C H 0.1824 0.1050 0.5160 0.084(16) Uiso 1 1 d R . . 
C33 C -0.0367(3) -0.01109(15) 0.52574(14) 0.0320(6) Uani 1 1 d . . . 
C34 C 0.0706(3) -0.05660(17) 0.54002(19) 0.0448(8) Uani 1 1 d . . . 
H34A H 0.0563 -0.1107 0.5276 0.051(10) Uiso 1 1 d R . . 
H34B H 0.0967 -0.0546 0.5892 0.074(14) Uiso 1 1 d R . . 
H34C H 0.1391 -0.0411 0.5144 0.083(16) Uiso 1 1 d R . . 
C35 C -0.0649(4) -0.0144(2) 0.4486(2) 0.0676(13) Uani 1 1 d . . . 
H35A H -0.0016 0.0098 0.4183 0.098(19) Uiso 1 1 d R . . 
H35B H -0.0758 -0.0631 0.4359 0.097(17) Uiso 1 1 d R . . 
H35C H -0.1345 0.0173 0.4362 0.072(13) Uiso 1 1 d R . . 
C36 C -0.1377(4) -0.0429(2) 0.5664(3) 0.0727(14) Uani 1 1 d . . . 
H36A H -0.1280 -0.0404 0.6235 0.16(3) Uiso 1 1 d R . . 
H36B H -0.1495 -0.0890 0.5559 0.068(13) Uiso 1 1 d R . . 
H36C H -0.2175 -0.0150 0.5589 0.093(17) Uiso 1 1 d R . . 
Si15 Si 0.39120(7) -0.07296(4) 0.68632(4) 0.03036(17) Uani 1 1 d . . . 
C51 C 0.4881(4) -0.0855(2) 0.76277(19) 0.0538(9) Uani 1 1 d . . . 
H51A H 0.5333 -0.1320 0.7588 0.070(13) Uiso 1 1 d R . . 
H51B H 0.5413 -0.0409 0.7675 0.080(15) Uiso 1 1 d R . . 
H51C H 0.4341 -0.0883 0.8069 0.058(11) Uiso 1 1 d R . . 
C52 C 0.2937(3) -0.15318(17) 0.67895(17) 0.0403(7) Uani 1 1 d . . . 
H52A H 0.2535 -0.1646 0.7232 0.051(10) Uiso 1 1 d R . . 
H52B H 0.3453 -0.1991 0.6673 0.074(14) Uiso 1 1 d R . . 
H52C H 0.2413 -0.1487 0.6410 0.062(12) Uiso 1 1 d R . . 
C53 C 0.4777(3) -0.05620(15) 0.60558(16) 0.0340(6) Uani 1 1 d . . . 
C54 C 0.5612(3) -0.11918(17) 0.59058(19) 0.0419(7) Uani 1 1 d . . . 
H54A H 0.5178 -0.1660 0.5863 0.044(9) Uiso 1 1 d R . . 
H54B H 0.6108 -0.1106 0.5418 0.049(10) Uiso 1 1 d R . . 
H54C H 0.6146 -0.1240 0.6355 0.031(8) Uiso 1 1 d R . . 
C55 C 0.3943(3) -0.04903(18) 0.54357(17) 0.0426(7) Uani 1 1 d . . . 
H55A H 0.3438 -0.0925 0.5295 0.041(9) Uiso 1 1 d R . . 
H55B H 0.4424 -0.0396 0.4999 0.018(7) Uiso 1 1 d R . . 
H55C H 0.3428 -0.0038 0.5512 0.054(11) Uiso 1 1 d R . . 
C56 C 0.5475(3) 0.01421(17) 0.6124(2) 0.0482(8) Uani 1 1 d . . . 
H56A H 0.4966 0.0560 0.6229 0.049(10) Uiso 1 1 d R . . 
H56B H 0.5860 0.0284 0.5618 0.067(13) Uiso 1 1 d R . . 
H56C H 0.6014 0.0130 0.6508 0.059(12) Uiso 1 1 d R . . 
C90 C 0.5913(3) 0.2308(2) 0.64043(16) 0.0424(8) Uani 1 1 d . . . 
H90A H 0.6124 0.2031 0.6070 0.072(14) Uiso 1 1 d R . . 
H90B H 0.5115 0.2605 0.6319 0.076(14) Uiso 1 1 d R . . 
H90C H 0.6616 0.2643 0.6379 0.14(3) Uiso 1 1 d R . . 
C91 C 0.5876(2) 0.18957(17) 0.70676(14) 0.0334(6) Uani 1 1 d . . . 
O91 O 0.49917(19) 0.18646(14) 0.74140(11) 0.0447(5) Uani 1 1 d . . . 
C92 C 0.6987(3) 0.15238(16) 0.72952(15) 0.0323(6) Uani 1 1 d . . . 
H92A H 0.7559 0.1905 0.7342 0.050(10) Uiso 1 1 d R . . 
H92B H 0.7205 0.1208 0.6898 0.049(10) Uiso 1 1 d R . . 
C93 C 0.6879(3) 0.10911(17) 0.79572(15) 0.0371(7) Uani 1 1 d . . . 
H93A H 0.6756 0.1413 0.8359 0.057(12) Uiso 1 1 d R . . 
H93B H 0.7679 0.0788 0.8071 0.060(12) Uiso 1 1 d R . . 
H93C H 0.6245 0.0729 0.7860 0.045(9) Uiso 1 1 d R . . 

loop_ 
_atom_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
N1 0.0229(10) 0.0240(10) 0.0201(10) -0.0027(8) -0.0021(8) -0.0004(8) 
C2 0.0249(12) 0.0196(11) 0.0184(11) 0.0003(9) -0.0013(9) 0.0008(10) 
N2 0.0209(10) 0.0300(11) 0.0220(10) -0.0037(9) 0.0014(8) 0.0012(9) 
N3 0.0220(10) 0.0271(11) 0.0205(10) -0.0027(8) -0.0001(8) 0.0021(8) 
C4 0.0213(11) 0.0221(11) 0.0209(11) -0.0012(9) -0.0001(9) -0.0014(10) 
C5 0.0230(12) 0.0234(11) 0.0230(12) 0.0005(9) -0.0006(10) -0.0012(10) 
C6 0.0241(12) 0.0213(11) 0.0213(12) 0.0007(10) 0.0001(10) 0.0018(10) 
O6 0.0292(9) 0.0320(9) 0.0170(8) -0.0054(7) 0.0003(7) -0.0004(7) 
N7 0.0226(10) 0.0290(10) 0.0184(10) -0.0033(8) 0.0003(8) 0.0013(8) 
C8 0.0231(11) 0.0319(13) 0.0175(11) -0.0022(10) 0.0005(9) 0.0012(10) 
N9 0.0209(10) 0.0287(11) 0.0198(10) -0.0031(8) -0.0006(8) -0.0016(8) 
C11 0.0259(12) 0.0234(12) 0.0220(12) -0.0017(10) -0.0008(10) -0.0017(10) 
C12 0.0271(12) 0.0251(12) 0.0139(11) -0.0002(9) -0.0013(10) 0.0006(10) 
O12 0.0278(9) 0.0268(9) 0.0216(8) 0.0015(7) -0.0018(7) 0.0004(7) 
C13 0.0254(12) 0.0283(12) 0.0210(12) -0.0033(10) 0.0019(10) -0.0038(10) 
O13 0.0290(9) 0.0377(10) 0.0214(8) -0.0062(7) -0.0003(7) -0.0039(8) 
C14 0.0365(14) 0.0219(12) 0.0249(12) -0.0045(10) 0.0016(11) 0.0013(11) 
O14 0.0386(10) 0.0234(9) 0.0202(8) 0.0000(7) 0.0036(8) -0.0020(8) 
C15 0.0427(16) 0.0264(14) 0.0285(14) -0.0038(11) 0.0015(12) 0.0049(12) 
O15 0.0517(13) 0.0359(11) 0.0301(11) 0.0016(9) 0.0067(10) 0.0180(10) 
Si12 0.0350(4) 0.0253(3) 0.0243(3) 0.0014(3) -0.0027(3) -0.0021(3) 
C21 0.097(3) 0.0336(17) 0.0289(15) -0.0002(12) -0.0166(18) -0.0132(19) 
C22 0.0325(15) 0.0405(18) 0.058(2) 0.0183(15) -0.0029(14) -0.0039(13) 
C23 0.0325(14) 0.0272(13) 0.0309(14) 0.0037(11) 0.0014(11) 0.0047(11) 
C24 0.0403(17) 0.051(2) 0.0454(18) 0.0031(15) 0.0066(15) 0.0137(15) 
C25 0.058(2) 0.0272(15) 0.0455(18) 0.0050(13) -0.0005(15) 0.0030(14) 
C26 0.0468(17) 0.0382(15) 0.0260(13) 0.0051(12) -0.0042(13) 0.0013(13) 
Si13 0.0298(3) 0.0259(3) 0.0189(3) -0.0020(2) -0.0007(3) 0.0016(3) 
C31 0.0442(17) 0.0333(15) 0.0378(16) 0.0017(13) -0.0004(13) 0.0080(13) 
C32 0.0445(18) 0.0415(16) 0.0251(13) 0.0043(12) 0.0031(13) 0.0008(14) 
C33 0.0391(15) 0.0301(14) 0.0270(13) -0.0083(11) -0.0055(12) 0.0040(12) 
C34 0.0508(19) 0.0355(17) 0.0481(19) -0.0134(14) -0.0129(16) 0.0115(14) 
C35 0.110(4) 0.048(2) 0.045(2) -0.0241(17) -0.035(2) 0.024(2) 
C36 0.060(2) 0.0383(19) 0.119(4) -0.020(2) 0.029(3) -0.0156(18) 
Si15 0.0366(4) 0.0250(3) 0.0295(4) -0.0023(3) -0.0032(3) 0.0062(3) 
C51 0.070(2) 0.0458(19) 0.0452(19) 0.0021(15) -0.0145(18) 0.0021(19) 
C52 0.0432(17) 0.0404(17) 0.0374(16) 0.0014(13) 0.0037(14) -0.0033(14) 
C53 0.0303(14) 0.0292(14) 0.0424(16) -0.0047(11) 0.0026(13) 0.0003(11) 
C54 0.0365(16) 0.0349(16) 0.054(2) -0.0066(14) 0.0052(15) 0.0027(13) 
C55 0.0460(17) 0.0452(17) 0.0367(16) 0.0040(13) 0.0068(15) -0.0030(14) 
C56 0.0419(18) 0.0320(16) 0.071(2) -0.0081(16) 0.0039(17) -0.0028(14) 
C90 0.0416(17) 0.057(2) 0.0289(15) 0.0040(14) 0.0033(13) 0.0127(15) 
C91 0.0313(14) 0.0412(16) 0.0277(13) -0.0077(12) 0.0016(11) 0.0013(12) 
O91 0.0321(11) 0.0682(15) 0.0338(11) 0.0038(10) 0.0069(9) 0.0064(11) 
C92 0.0308(14) 0.0361(15) 0.0300(14) 0.0017(12) 0.0018(11) -0.0004(12) 
C93 0.0399(16) 0.0404(16) 0.0310(15) 0.0046(12) 0.0006(12) -0.0051(13) 

#MOLECULAR GEOMETRY

_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 C2 1.375(3) . ? 
N1 C6 1.403(3) . ? 
N1 H1 0.9202 . ? 
C2 N3 1.322(3) . ? 
C2 N2 1.340(3) . ? 
N2 H2A 0.8981 . ? 
N2 H2B 0.9386 . ? 
N3 C4 1.351(3) . ? 
C4 C5 1.368(3) . ? 
C4 N9 1.386(3) . ? 
C5 N7 1.401(3) . ? 
C5 C6 1.418(4) . ? 
C6 O6 1.229(3) . ? 
N7 C8 1.305(3) . ? 
C8 N9 1.375(3) . ? 
C8 H8 1.0054 . ? 
N9 C11 1.442(3) . ? 
C11 O14 1.422(3) . ? 
C11 C12 1.535(3) . ? 
C11 H11 1.1055 . ? 
C12 O12 1.413(3) . ? 
C12 C13 1.527(3) . ? 
C12 H12 0.9749 . ? 
O12 Si12 1.6649(19) . ? 
C13 O13 1.411(3) . ? 
C13 C14 1.519(4) . ? 
C13 H13 1.0328 . ? 
O13 Si13 1.6481(19) . ? 
C14 O14 1.455(3) . ? 
C14 C15 1.510(4) . ? 
C14 H14 1.0992 . ? 
C15 O15 1.422(3) . ? 
C15 H15A 1.0339 . ? 
C15 H15B 0.9752 . ? 
O15 Si15 1.639(2) . ? 
Si12 C22 1.857(3) . ? 
Si12 C21 1.860(3) . ? 
Si12 C23 1.882(3) . ? 
C21 H21A 0.9433 . ? 
C21 H21B 0.9772 . ? 
C21 H21C 0.9535 . ? 
C22 H22A 1.0222 . ? 
C22 H22B 0.9440 . ? 
C22 H22C 0.9558 . ? 
C23 C24 1.527(4) . ? 
C23 C26 1.534(4) . ? 
C23 C25 1.539(4) . ? 
C24 H24A 1.0560 . ? 
C24 H24B 1.0307 . ? 
C24 H24C 1.0406 . ? 
C25 H25A 1.1168 . ? 
C25 H25B 0.9826 . ? 
C25 H25C 1.0312 . ? 
C26 H26A 1.0134 . ? 
C26 H26B 0.9800 . ? 
C26 H26C 1.0722 . ? 
Si13 C31 1.862(3) . ? 
Si13 C32 1.864(3) . ? 
Si13 C33 1.883(3) . ? 
C31 H31A 0.9207 . ? 
C31 H31B 0.9642 . ? 
C31 H31C 0.9473 . ? 
C32 H32A 1.0630 . ? 
C32 H32B 0.9888 . ? 
C32 H32C 0.8693 . ? 
C33 C34 1.517(4) . ? 
C33 C36 1.519(5) . ? 
C33 C35 1.528(4) . ? 
C34 H34A 1.0426 . ? 
C34 H34B 0.9978 . ? 
C34 H34C 0.9722 . ? 
C35 H35A 1.0351 . ? 
C35 H35B 0.9425 . ? 
C35 H35C 1.0196 . ? 
C36 H36A 1.1104 . ? 
C36 H36B 0.8875 . ? 
C36 H36C 1.0613 . ? 
Si15 C51 1.864(4) . ? 
Si15 C52 1.865(3) . ? 
Si15 C53 1.875(3) . ? 
C51 H51A 1.0079 . ? 
C51 H51B 1.0307 . ? 
C51 H51C 1.0552 . ? 
C52 H52A 0.9953 . ? 
C52 H52B 1.0596 . ? 
C52 H52C 0.9515 . ? 
C53 C56 1.535(4) . ? 
C53 C54 1.537(4) . ? 
C53 C55 1.539(4) . ? 
C54 H54A 1.0027 . ? 
C54 H54B 1.1132 . ? 
C54 H54C 1.0662 . ? 
C55 H55A 1.0288 . ? 
C55 H55B 1.0240 . ? 
C55 H55C 1.0348 . ? 
C56 H56A 0.9904 . ? 
C56 H56B 1.1050 . ? 
C56 H56C 0.9665 . ? 
C90 C91 1.493(4) . ? 
C90 H90A 0.8593 . ? 
C90 H90B 1.0807 . ? 
C90 H90C 1.0187 . ? 
C91 O91 1.217(3) . ? 
C91 C92 1.515(4) . ? 
C92 C93 1.515(4) . ? 
C92 H92A 0.9677 . ? 
C92 H92B 0.9968 . ? 
C93 H93A 0.9895 . ? 
C93 H93B 1.0982 . ? 
C93 H93C 1.0067 . ? 

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 
C2 N1 C6 125.1(2) . . ? 
C2 N1 H1 118.7 . . ? 
C6 N1 H1 116.2 . . ? 
N3 C2 N2 118.9(2) . . ? 
N3 C2 N1 123.9(2) . . ? 
N2 C2 N1 117.2(2) . . ? 
C2 N2 H2A 118.1 . . ? 
C2 N2 H2B 120.8 . . ? 
H2A N2 H2B 119.8 . . ? 
C2 N3 C4 111.8(2) . . ? 
N3 C4 C5 128.7(2) . . ? 
N3 C4 N9 125.6(2) . . ? 
C5 C4 N9 105.7(2) . . ? 
C4 C5 N7 110.6(2) . . ? 
C4 C5 C6 119.7(2) . . ? 
N7 C5 C6 129.7(2) . . ? 
O6 C6 N1 120.4(2) . . ? 
O6 C6 C5 128.9(2) . . ? 
N1 C6 C5 110.7(2) . . ? 
C8 N7 C5 104.5(2) . . ? 
N7 C8 N9 113.0(2) . . ? 
N7 C8 H8 125.5 . . ? 
N9 C8 H8 121.5 . . ? 
C8 N9 C4 106.2(2) . . ? 
C8 N9 C11 125.8(2) . . ? 
C4 N9 C11 127.7(2) . . ? 
O14 C11 N9 108.95(19) . . ? 
O14 C11 C12 105.5(2) . . ? 
N9 C11 C12 115.6(2) . . ? 
O14 C11 H11 112.0 . . ? 
N9 C11 H11 107.2 . . ? 
C12 C11 H11 107.7 . . ? 
O12 C12 C13 114.53(19) . . ? 
O12 C12 C11 111.5(2) . . ? 
C13 C12 C11 100.68(19) . . ? 
O12 C12 H12 110.1 . . ? 
C13 C12 H12 109.6 . . ? 
C11 C12 H12 110.0 . . ? 
C12 O12 Si12 120.96(16) . . ? 
O13 C13 C14 109.5(2) . . ? 
O13 C13 C12 109.9(2) . . ? 
C14 C13 C12 101.50(19) . . ? 
O13 C13 H13 109.7 . . ? 
C14 C13 H13 111.7 . . ? 
C12 C13 H13 114.3 . . ? 
C13 O13 Si13 128.90(16) . . ? 
O14 C14 C15 109.1(2) . . ? 
O14 C14 C13 105.7(2) . . ? 
C15 C14 C13 113.6(2) . . ? 
O14 C14 H14 107.7 . . ? 
C15 C14 H14 109.2 . . ? 
C13 C14 H14 111.3 . . ? 
C11 O14 C14 109.62(19) . . ? 
O15 C15 C14 108.4(2) . . ? 
O15 C15 H15A 112.5 . . ? 
C14 C15 H15A 109.9 . . ? 
O15 C15 H15B 108.2 . . ? 
C14 C15 H15B 113.8 . . ? 
H15A C15 H15B 104.0 . . ? 
C15 O15 Si15 128.38(18) . . ? 
O12 Si12 C22 109.00(13) . . ? 
O12 Si12 C21 109.96(13) . . ? 
C22 Si12 C21 109.3(2) . . ? 
O12 Si12 C23 105.44(11) . . ? 
C22 Si12 C23 111.96(14) . . ? 
C21 Si12 C23 111.10(15) . . ? 
Si12 C21 H21A 108.9 . . ? 
Si12 C21 H21B 111.5 . . ? 
H21A C21 H21B 103.4 . . ? 
Si12 C21 H21C 114.3 . . ? 
H21A C21 H21C 109.5 . . ? 
H21B C21 H21C 108.8 . . ? 
Si12 C22 H22A 113.9 . . ? 
Si12 C22 H22B 106.1 . . ? 
H22A C22 H22B 110.9 . . ? 
Si12 C22 H22C 109.6 . . ? 
H22A C22 H22C 100.3 . . ? 
H22B C22 H22C 116.3 . . ? 
C24 C23 C26 108.4(3) . . ? 
C24 C23 C25 109.7(3) . . ? 
C26 C23 C25 108.7(2) . . ? 
C24 C23 Si12 110.3(2) . . ? 
C26 C23 Si12 111.04(19) . . ? 
C25 C23 Si12 108.7(2) . . ? 
C23 C24 H24A 111.2 . . ? 
C23 C24 H24B 111.9 . . ? 
H24A C24 H24B 103.1 . . ? 
C23 C24 H24C 113.4 . . ? 
H24A C24 H24C 109.9 . . ? 
H24B C24 H24C 106.8 . . ? 
C23 C25 H25A 112.8 . . ? 
C23 C25 H25B 111.6 . . ? 
H25A C25 H25B 109.3 . . ? 
C23 C25 H25C 110.9 . . ? 
H25A C25 H25C 108.2 . . ? 
H25B C25 H25C 103.5 . . ? 
C23 C26 H26A 112.6 . . ? 
C23 C26 H26B 108.8 . . ? 
H26A C26 H26B 106.2 . . ? 
C23 C26 H26C 113.3 . . ? 
H26A C26 H26C 112.4 . . ? 
H26B C26 H26C 102.7 . . ? 
O13 Si13 C31 105.77(13) . . ? 
O13 Si13 C32 110.31(12) . . ? 
C31 Si13 C32 111.30(14) . . ? 
O13 Si13 C33 108.31(11) . . ? 
C31 Si13 C33 110.02(14) . . ? 
C32 Si13 C33 110.96(14) . . ? 
Si13 C31 H31A 108.4 . . ? 
Si13 C31 H31B 111.9 . . ? 
H31A C31 H31B 106.9 . . ? 
Si13 C31 H31C 112.5 . . ? 
H31A C31 H31C 107.9 . . ? 
H31B C31 H31C 108.9 . . ? 
Si13 C32 H32A 107.4 . . ? 
Si13 C32 H32B 109.7 . . ? 
H32A C32 H32B 108.0 . . ? 
Si13 C32 H32C 116.2 . . ? 
H32A C32 H32C 114.1 . . ? 
H32B C32 H32C 101.1 . . ? 
C34 C33 C36 108.1(3) . . ? 
C34 C33 C35 109.1(3) . . ? 
C36 C33 C35 109.1(4) . . ? 
C34 C33 Si13 110.7(2) . . ? 
C36 C33 Si13 109.4(2) . . ? 
C35 C33 Si13 110.4(2) . . ? 
C33 C34 H34A 111.3 . . ? 
C33 C34 H34B 113.4 . . ? 
H34A C34 H34B 107.6 . . ? 
C33 C34 H34C 113.6 . . ? 
H34A C34 H34C 107.1 . . ? 
H34B C34 H34C 103.4 . . ? 
C33 C35 H35A 112.7 . . ? 
C33 C35 H35B 108.7 . . ? 
H35A C35 H35B 111.1 . . ? 
C33 C35 H35C 111.9 . . ? 
H35A C35 H35C 99.7 . . ? 
H35B C35 H35C 112.6 . . ? 
C33 C36 H36A 114.9 . . ? 
C33 C36 H36B 111.8 . . ? 
H36A C36 H36B 106.4 . . ? 
C33 C36 H36C 113.5 . . ? 
H36A C36 H36C 101.7 . . ? 
H36B C36 H36C 107.8 . . ? 
O15 Si15 C51 111.05(15) . . ? 
O15 Si15 C52 110.15(14) . . ? 
C51 Si15 C52 108.63(16) . . ? 
O15 Si15 C53 102.86(12) . . ? 
C51 Si15 C53 111.40(17) . . ? 
C52 Si15 C53 112.68(14) . . ? 
Si15 C51 H51A 110.6 . . ? 
Si15 C51 H51B 108.9 . . ? 
H51A C51 H51B 112.7 . . ? 
Si15 C51 H51C 107.2 . . ? 
H51A C51 H51C 108.8 . . ? 
H51B C51 H51C 108.4 . . ? 
Si15 C52 H52A 112.4 . . ? 
Si15 C52 H52B 108.6 . . ? 
H52A C52 H52B 105.7 . . ? 
Si15 C52 H52C 111.6 . . ? 
H52A C52 H52C 112.8 . . ? 
H52B C52 H52C 105.1 . . ? 
C56 C53 C54 109.6(3) . . ? 
C56 C53 C55 108.6(3) . . ? 
C54 C53 C55 107.8(3) . . ? 
C56 C53 Si15 110.2(2) . . ? 
C54 C53 Si15 111.2(2) . . ? 
C55 C53 Si15 109.5(2) . . ? 
C53 C54 H54A 111.2 . . ? 
C53 C54 H54B 111.7 . . ? 
H54A C54 H54B 107.9 . . ? 
C53 C54 H54C 105.5 . . ? 
H54A C54 H54C 106.3 . . ? 
H54B C54 H54C 114.1 . . ? 
C53 C55 H55A 119.3 . . ? 
C53 C55 H55B 108.8 . . ? 
H55A C55 H55B 102.6 . . ? 
C53 C55 H55C 108.3 . . ? 
H55A C55 H55C 110.4 . . ? 
H55B C55 H55C 106.7 . . ? 
C53 C56 H56A 111.9 . . ? 
C53 C56 H56B 109.5 . . ? 
H56A C56 H56B 103.4 . . ? 
C53 C56 H56C 112.4 . . ? 
H56A C56 H56C 103.8 . . ? 
H56B C56 H56C 115.4 . . ? 
C91 C90 H90A 110.4 . . ? 
C91 C90 H90B 111.5 . . ? 
H90A C90 H90B 115.3 . . ? 
C91 C90 H90C 112.0 . . ? 
H90A C90 H90C 96.0 . . ? 
H90B C90 H90C 110.7 . . ? 
O91 C91 C90 121.4(3) . . ? 
O91 C91 C92 121.4(3) . . ? 
C90 C91 C92 117.2(2) . . ? 
C93 C92 C91 114.6(2) . . ? 
C93 C92 H92A 111.2 . . ? 
C91 C92 H92A 105.5 . . ? 
C93 C92 H92B 111.1 . . ? 
C91 C92 H92B 104.7 . . ? 
H92A C92 H92B 109.2 . . ? 
C92 C93 H93A 110.9 . . ? 
C92 C93 H93B 111.8 . . ? 
H93A C93 H93B 105.6 . . ? 
C92 C93 H93C 104.7 . . ? 
H93A C93 H93C 116.4 . . ? 
H93B C93 H93C 107.6 . . ?