# Electronic Supplementary Material (ESI) for Nanoscale
# This journal is © The Royal Society of Chemistry 2013


#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material 
#  of the CCDC or of third parties, and may not be copied or further 
#  disseminated in any form, whether machine-readable or not,  
#  except for the purpose of generating routine backup copies 
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and 
#  data retrieval see:
#                         www.ccdc.cam.ac.uk 
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively. 
#
####################################################################### 

data_tilac1_0m
_database_code_depnum_ccdc_archive 'CCDC 915222'
#TrackingRef 'tilac1_0m.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H26 N2 O12 Ti'
_chemical_formula_weight         402.22
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   P3
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
_cell_length_a                   15.3040(15)
_cell_length_b                   15.3040(15)
_cell_length_c                   6.6658(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1352.0(3)
_cell_formula_units_Z            3
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5298
_cell_measurement_theta_min      2.66
_cell_measurement_theta_max      23.82
_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             636
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.8518
_exptl_absorpt_correction_T_max  0.9585
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      296(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  'Bruker SMART Apex-II CCD'
_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            9275
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         2.66
_diffrn_reflns_theta_max         23.82
_reflns_number_total             2772
_reflns_number_gt                2640
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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^)+(0.0286P)^2^+0.0000P] 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   -0.03(10)
_refine_ls_number_reflns         2772
_refine_ls_number_parameters     262
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0219
_refine_ls_wR_factor_ref         0.0516
_refine_ls_wR_factor_gt          0.0509
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_restrained_S_all      5.959
_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
Ti1 Ti 0.3333 0.6667 0.8779(5) 0.0258(10) Uani 1 3 d S . .
Ti2 Ti 0.0000 1.0000 -0.1171(5) 0.0257(10) Uani 1 3 d S . .
Ti3 Ti 0.6667 0.3333 0.6998(5) 0.0241(9) Uani 1 3 d S . .
O2 O -0.1002(7) 0.8939(7) 0.0805(14) 0.032(2) Uani 1 1 d . . .
O1 O 0.4235(7) 0.7756(7) 0.6798(15) 0.038(2) Uani 1 1 d . . .
O3 O 0.6385(7) 0.2152(6) 0.8348(13) 0.033(2) Uani 1 1 d . . .
O8 O -0.2027(8) 0.7286(7) 0.1248(15) 0.042(2) Uani 1 1 d . . .
C1 C 0.5464(10) 0.1341(11) 0.540(2) 0.033(3) Uani 1 1 d . . .
O7 O 0.5006(9) 0.0651(8) 0.4234(16) 0.060(3) Uani 1 1 d . . .
C8 C 0.5411(10) 0.8162(10) 0.941(2) 0.032(3) Uani 1 1 d . . .
H8A H 0.5552 0.8738 1.0270 0.039 Uiso 1 1 calc R . .
C2 C 0.5774(10) 0.1188(9) 0.749(2) 0.032(3) Uani 1 1 d . . .
H2A H 0.6179 0.0859 0.7345 0.039 Uiso 1 1 calc R . .
O9 O 0.5772(9) 0.9043(9) 0.6300(17) 0.059(3) Uani 1 1 d . . .
C7 C 0.5153(10) 0.8357(10) 0.735(2) 0.033(3) Uani 1 1 d . . .
C9 C 0.6328(11) 0.8039(14) 0.939(3) 0.053(4) Uani 1 1 d . . .
H9A H 0.6475 0.7923 1.0733 0.079 Uiso 1 1 calc R . .
H9B H 0.6894 0.8640 0.8868 0.079 Uiso 1 1 calc R . .
H9C H 0.6200 0.7475 0.8560 0.079 Uiso 1 1 calc R . .
C4 C -0.1459(9) 0.8021(10) 0.021(2) 0.028(3) Uani 1 1 d . . .
O6 O 0.5732(7) 0.2266(7) 0.5006(13) 0.035(2) Uani 1 1 d . . .
O5 O -0.0418(7) 0.8810(6) -0.2594(13) 0.032(2) Uani 1 1 d . . .
O4 O 0.4552(6) 0.7288(7) 1.0186(13) 0.034(2) Uani 1 1 d . . .
O10 O 0.0444(10) 0.8594(9) -0.6084(18) 0.049(3) Uani 1 1 d D . .
O11 O -0.3125(10) 0.7507(10) 0.4484(19) 0.057(3) Uani 1 1 d D . .
O12 O 0.6735(10) 1.0125(9) 0.2872(18) 0.051(3) Uani 1 1 d D . .
N1 N 0.3687(10) 0.8568(10) 0.3535(18) 0.044(3) Uani 1 1 d D . .
H1A H 0.341(2) 0.816(3) 0.201(10) 0.09(7) Uiso 1 1 d RD . .
H1B H 0.3722(11) 0.818(3) 0.429(5) 0.07(6) Uiso 1 1 d RD . .
H1C H 0.319(3) 0.8736(14) 0.392(3) 0.08(7) Uiso 1 1 d RD . .
H1D H 0.440(5) 0.936(5) 0.340(2) 0.10(7) Uiso 1 1 d RD . .
N2 N 0.4623(10) 0.2496(10) 0.1826(19) 0.036(3) Uani 1 1 d D . .
C3 C 0.4865(12) 0.0525(12) 0.877(2) 0.051(4) Uani 1 1 d . . .
H3A H 0.5084 0.0440 1.0064 0.076 Uiso 1 1 calc R . .
H3B H 0.4476 -0.0121 0.8134 0.076 Uiso 1 1 calc R . .
H3C H 0.4457 0.0836 0.8912 0.076 Uiso 1 1 calc R . .
C6 C -0.1132(15) 0.7014(11) -0.238(3) 0.060(5) Uani 1 1 d . . .
H6A H -0.1023 0.6979 -0.3787 0.090 Uiso 1 1 calc R . .
H6B H -0.1725 0.6406 -0.1965 0.090 Uiso 1 1 calc R . .
H6C H -0.0559 0.7089 -0.1641 0.090 Uiso 1 1 calc R . .
C5 C -0.1269(10) 0.7902(10) -0.198(2) 0.034(3) Uani 1 1 d . . .
H5A H -0.1852 0.7813 -0.2754 0.041 Uiso 1 1 calc R . .
H2AA H 0.499(10) 0.283(10) 0.065(18) 0.04(4) Uiso 1 1 d D . .
H2BA H 0.429(12) 0.286(12) 0.22(3) 0.07(6) Uiso 1 1 d D . .
H11A H -0.280(16) 0.815(9) 0.46(3) 0.09(8) Uiso 1 1 d D . .
H2CA H 0.501(12) 0.247(14) 0.29(2) 0.07(6) Uiso 1 1 d D . .
H2DA H 0.407(11) 0.185(9) 0.14(3) 0.07(6) Uiso 1 1 d D . .
H10A H 0.050(15) 0.897(13) -0.70(3) 0.08(7) Uiso 1 1 d D . .
H12A H 0.724(11) 1.002(14) 0.31(3) 0.07(6) Uiso 1 1 d D . .
H10B H 0.019(13) 0.874(13) -0.51(2) 0.06(6) Uiso 1 1 d D . .
H11B H -0.282(14) 0.737(16) 0.35(2) 0.08(7) Uiso 1 1 d D . .
H12B H 0.633(14) 0.980(14) 0.38(2) 0.07(7) Uiso 1 1 d D . .
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
Ti1 0.0274(14) 0.0274(14) 0.023(2) 0.000 0.000 0.0137(7)
Ti2 0.0265(14) 0.0265(14) 0.024(2) 0.000 0.000 0.0133(7)
Ti3 0.0252(13) 0.0252(13) 0.022(2) 0.000 0.000 0.0126(7)
O2 0.034(5) 0.029(5) 0.030(5) 0.000(4) 0.006(4) 0.014(4)
O1 0.037(6) 0.038(6) 0.031(5) 0.011(5) -0.002(4) 0.012(5)
O3 0.041(6) 0.029(5) 0.028(5) 0.000(4) -0.008(4) 0.017(4)
O8 0.044(6) 0.032(6) 0.045(6) 0.007(5) 0.015(5) 0.016(5)
C1 0.027(7) 0.030(8) 0.036(8) -0.002(6) -0.004(6) 0.010(6)
O7 0.073(8) 0.039(6) 0.051(7) -0.013(6) -0.022(6) 0.015(6)
C8 0.026(7) 0.029(7) 0.034(8) 0.001(6) -0.002(6) 0.009(6)
C2 0.034(8) 0.023(7) 0.039(8) -0.001(6) -0.003(6) 0.014(6)
O9 0.048(7) 0.050(7) 0.062(7) 0.028(6) 0.009(6) 0.011(6)
C7 0.033(8) 0.026(7) 0.041(8) 0.005(6) 0.003(7) 0.014(7)
C9 0.032(9) 0.063(11) 0.062(11) 0.019(9) 0.002(7) 0.023(8)
C4 0.024(7) 0.028(8) 0.035(8) 0.001(6) 0.002(6) 0.014(6)
O6 0.037(5) 0.031(5) 0.031(5) -0.001(4) -0.012(4) 0.012(4)
O5 0.035(5) 0.028(5) 0.031(5) 0.000(4) 0.007(4) 0.014(4)
O4 0.029(5) 0.039(5) 0.029(5) 0.007(4) -0.002(4) 0.013(4)
O10 0.067(8) 0.051(7) 0.038(7) 0.013(6) 0.014(6) 0.035(6)
O11 0.057(8) 0.063(9) 0.048(7) -0.004(6) 0.001(6) 0.028(7)
O12 0.059(8) 0.052(7) 0.045(7) 0.009(6) 0.004(6) 0.029(6)
N1 0.060(8) 0.039(7) 0.038(7) -0.002(6) -0.013(6) 0.028(7)
N2 0.033(7) 0.043(8) 0.029(7) 0.004(6) -0.001(6) 0.017(6)
C3 0.053(10) 0.040(9) 0.048(9) 0.003(7) 0.008(8) 0.014(8)
C6 0.078(12) 0.032(9) 0.062(11) 0.002(8) 0.036(10) 0.021(9)
C5 0.032(8) 0.030(7) 0.034(7) -0.001(6) 0.001(6) 0.011(6)
_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
Ti1 O4 1.868(9) 2_665 ?
Ti1 O4 1.868(9) . ?
Ti1 O4 1.868(9) 3_565 ?
Ti1 O1 2.032(10) 2_665 ?
Ti1 O1 2.032(10) . ?
Ti1 O1 2.032(10) 3_565 ?
Ti2 O5 1.860(9) . ?
Ti2 O5 1.860(9) 3_465 ?
Ti2 O5 1.860(9) 2_675 ?
Ti2 O2 2.057(9) 3_465 ?
Ti2 O2 2.057(9) 2_675 ?
Ti2 O2 2.057(9) . ?
Ti3 O3 1.866(8) . ?
Ti3 O3 1.866(8) 2_655 ?
Ti3 O3 1.866(8) 3_665 ?
Ti3 O6 2.035(9) 2_655 ?
Ti3 O6 2.035(9) . ?
Ti3 O6 2.035(9) 3_665 ?
O2 C4 1.280(16) . ?
O1 C7 1.289(17) . ?
O3 C2 1.414(15) . ?
O8 C4 1.234(16) . ?
C1 O7 1.215(17) . ?
C1 O6 1.289(17) . ?
C1 C2 1.523(19) . ?
C8 O4 1.424(16) . ?
C8 C7 1.50(2) . ?
C8 C9 1.51(2) . ?
C8 H8A 0.9800 . ?
C2 C3 1.51(2) . ?
C2 H2A 0.9800 . ?
O9 C7 1.223(16) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C4 C5 1.514(19) . ?
O5 C5 1.410(16) . ?
O10 H10A 0.79(13) . ?
O10 H10B 0.84(10) . ?
O11 H11A 0.86(11) . ?
O11 H11B 0.87(11) . ?
O12 H12A 0.88(11) . ?
O12 H12B 0.86(11) . ?
N1 H1A 1.1538 . ?
N1 H1B 0.8053 . ?
N1 H1C 0.9461 . ?
N1 H1D 1.1613 . ?
N2 H2AA 0.95(9) . ?
N2 H2BA 0.96(10) . ?
N2 H2CA 0.96(10) . ?
N2 H2DA 0.97(10) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C6 C5 1.50(2) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C5 H5A 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
O4 Ti1 O4 97.0(4) 2_665 . ?
O4 Ti1 O4 97.0(4) 2_665 3_565 ?
O4 Ti1 O4 97.0(4) . 3_565 ?
O4 Ti1 O1 79.2(4) 2_665 2_665 ?
O4 Ti1 O1 159.8(4) . 2_665 ?
O4 Ti1 O1 103.2(4) 3_565 2_665 ?
O4 Ti1 O1 103.2(4) 2_665 . ?
O4 Ti1 O1 79.2(4) . . ?
O4 Ti1 O1 159.8(4) 3_565 . ?
O1 Ti1 O1 82.3(4) 2_665 . ?
O4 Ti1 O1 159.8(4) 2_665 3_565 ?
O4 Ti1 O1 103.2(4) . 3_565 ?
O4 Ti1 O1 79.2(4) 3_565 3_565 ?
O1 Ti1 O1 82.3(4) 2_665 3_565 ?
O1 Ti1 O1 82.3(4) . 3_565 ?
O5 Ti2 O5 96.3(4) . 3_465 ?
O5 Ti2 O5 96.3(4) . 2_675 ?
O5 Ti2 O5 96.3(4) 3_465 2_675 ?
O5 Ti2 O2 159.1(4) . 3_465 ?
O5 Ti2 O2 78.3(3) 3_465 3_465 ?
O5 Ti2 O2 104.3(4) 2_675 3_465 ?
O5 Ti2 O2 104.3(4) . 2_675 ?
O5 Ti2 O2 159.1(4) 3_465 2_675 ?
O5 Ti2 O2 78.3(4) 2_675 2_675 ?
O2 Ti2 O2 83.4(4) 3_465 2_675 ?
O5 Ti2 O2 78.3(3) . . ?
O5 Ti2 O2 104.3(4) 3_465 . ?
O5 Ti2 O2 159.1(4) 2_675 . ?
O2 Ti2 O2 83.4(4) 3_465 . ?
O2 Ti2 O2 83.4(4) 2_675 . ?
O3 Ti3 O3 98.7(4) . 2_655 ?
O3 Ti3 O3 98.7(4) . 3_665 ?
O3 Ti3 O3 98.7(4) 2_655 3_665 ?
O3 Ti3 O6 101.3(4) . 2_655 ?
O3 Ti3 O6 78.9(4) 2_655 2_655 ?
O3 Ti3 O6 159.9(4) 3_665 2_655 ?
O3 Ti3 O6 78.9(4) . . ?
O3 Ti3 O6 159.9(4) 2_655 . ?
O3 Ti3 O6 101.3(4) 3_665 . ?
O6 Ti3 O6 82.0(4) 2_655 . ?
O3 Ti3 O6 159.9(4) . 3_665 ?
O3 Ti3 O6 101.3(4) 2_655 3_665 ?
O3 Ti3 O6 78.9(4) 3_665 3_665 ?
O6 Ti3 O6 82.0(4) 2_655 3_665 ?
O6 Ti3 O6 82.0(4) . 3_665 ?
C4 O2 Ti2 116.8(8) . . ?
C7 O1 Ti1 116.8(9) . . ?
C2 O3 Ti3 121.8(8) . . ?
O7 C1 O6 123.5(13) . . ?
O7 C1 C2 122.7(13) . . ?
O6 C1 C2 113.8(11) . . ?
O4 C8 C7 107.9(10) . . ?
O4 C8 C9 111.5(11) . . ?
C7 C8 C9 111.8(12) . . ?
O4 C8 H8A 108.5 . . ?
C7 C8 H8A 108.5 . . ?
C9 C8 H8A 108.5 . . ?
O3 C2 C3 112.2(11) . . ?
O3 C2 C1 107.7(10) . . ?
C3 C2 C1 111.4(12) . . ?
O3 C2 H2A 108.5 . . ?
C3 C2 H2A 108.5 . . ?
C1 C2 H2A 108.5 . . ?
O9 C7 O1 123.3(13) . . ?
O9 C7 C8 121.8(13) . . ?
O1 C7 C8 114.9(11) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O8 C4 O2 125.1(12) . . ?
O8 C4 C5 121.4(12) . . ?
O2 C4 C5 113.5(11) . . ?
C1 O6 Ti3 117.2(8) . . ?
C5 O5 Ti2 120.8(8) . . ?
C8 O4 Ti1 121.0(8) . . ?
H10A O10 H10B 106(10) . . ?
H11A O11 H11B 105(10) . . ?
H12A O12 H12B 104(10) . . ?
H1A N1 H1B 107.1 . . ?
H1A N1 H1C 104.3 . . ?
H1B N1 H1C 113.4 . . ?
H1A N1 H1D 113.1 . . ?
H1B N1 H1D 116.5 . . ?
H1C N1 H1D 101.8 . . ?
H2AA N2 H2BA 104(10) . . ?
H2AA N2 H2CA 117(10) . . ?
H2BA N2 H2CA 110(10) . . ?
H2AA N2 H2DA 107(10) . . ?
H2BA N2 H2DA 102(10) . . ?
H2CA N2 H2DA 115(10) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O5 C5 C6 111.2(11) . . ?
O5 C5 C4 107.5(11) . . ?
C6 C5 C4 113.8(12) . . ?
O5 C5 H5A 108.1 . . ?
C6 C5 H5A 108.1 . . ?
C4 C5 H5A 108.1 . . ?
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        23.82
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.120
_refine_diff_density_min         -0.127
_refine_diff_density_rms         0.029