# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry B.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 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_bfdf
#TrackingRef 'bfdf-bff.cif'


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



_audit_update_record             
;

2013-01-05 # Formatted by publCIF

;



_audit_creation_method           SHELXL-97

_chemical_name_systematic        
'(β³-homophenylalanyl)-(α,β-dehydrophenylalanine) monohydrate'

_chemical_name_common            'PEPSEQ A=2 PHE*-PHE*'

_chemical_melting_point          ?

_chemical_formula_moiety         'C19 H20 N2 O3, 1(H2 O1)'

_chemical_formula_sum            'C19 H22 N2 O4'

_chemical_formula_weight         342.39

_exptl_crystal_recrystallization_method 'Mixture of Acetic acid and Acetone'



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'



_symmetry_cell_setting           Monoclinic

_symmetry_space_group_name_H-M   'P 21'

_symmetry_space_group_name_Hall  'P 2yb'

loop_

_symmetry_equiv_pos_as_xyz


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



_cell_length_a                   12.6575(6)

_cell_length_b                   5.6511(3)

_cell_length_c                   12.7702(6)

_cell_angle_alpha                90.00

_cell_angle_beta                 104.861(2)

_cell_angle_gamma                90.00

_cell_volume                     882.88(8)

_cell_formula_units_Z            2

_cell_measurement_temperature    296(2)

_cell_measurement_reflns_used    ?

_cell_measurement_theta_min      ?

_cell_measurement_theta_max      ?



_exptl_crystal_description       'rectangular rod'

_exptl_crystal_colour            colourless

_exptl_crystal_size_max          0.87

_exptl_crystal_size_mid          0.10

_exptl_crystal_size_min          0.07

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.288

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             364

_exptl_absorpt_coefficient_mu    0.091

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.9251

_exptl_absorpt_correction_T_max  0.9937

_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'



_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 Kappa APEX II CCD detector'

_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            11024

_diffrn_reflns_av_R_equivalents  0.0368

_diffrn_reflns_av_sigmaI/netI    0.0464

_diffrn_reflns_limit_h_min       -17

_diffrn_reflns_limit_h_max       17

_diffrn_reflns_limit_k_min       -6

_diffrn_reflns_limit_k_max       7

_diffrn_reflns_limit_l_min       -18

_diffrn_reflns_limit_l_max       17

_diffrn_reflns_theta_min         1.65

_diffrn_reflns_theta_max         30.53

_reflns_number_total             3886

_reflns_number_gt                2666

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       'KAPPA APEX II (BRUKER-AXS)'

_computing_cell_refinement       'SAINTPLUS (BRUKER-AXS)'

_computing_data_reduction        'SAINTPLUS (BRUKER-AXS)'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

_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 > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² are statistically about twice as large as those based on F, and R-

factors based on ALL data will be even larger.

;



_refine_ls_structure_factor_coef Fsqd

_refine_ls_matrix_type           full

_refine_ls_weighting_scheme      calc

_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0430P)²+0.1084P] where P=(Fo²+2Fc²)/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     SHELXL

_refine_ls_extinction_coef       0.006(3)

_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^

_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'

_refine_ls_abs_structure_Flack   -0.1(13)

_refine_ls_number_reflns         3886

_refine_ls_number_parameters     235

_refine_ls_number_restraints     1

_refine_ls_R_factor_all          0.0766

_refine_ls_R_factor_gt           0.0431

_refine_ls_wR_factor_ref         0.1027

_refine_ls_wR_factor_gt          0.0898

_refine_ls_goodness_of_fit_ref   0.993

_refine_ls_restrained_S_all      0.993

_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















































N1 N 0.02737(14) -0.0727(3) 0.61754(12) 0.0373(4) Uani 1 1 d . . .
H1A H 0.0672 0.0559 0.6151 0.056 Uiso 1 1 calc R . .
H1B H -0.0368 -0.0600 0.5689 0.056 Uiso 1 1 calc R . .
H1C H 0.0625 -0.1998 0.6028 0.056 Uiso 1 1 calc R . .
C1A C 0.12043(17) -0.1059(4) 0.81257(15) 0.0344(5) Uani 1 1 d . . .
H1A1 H 0.1097 -0.1237 0.8847 0.041 Uiso 1 1 calc R . .
H1A2 H 0.1620 -0.2407 0.7982 0.041 Uiso 1 1 calc R . .
C1B C 0.00912(16) -0.0968(4) 0.72862(15) 0.0345(5) Uani 1 1 d . . .
H1B1 H -0.0303 0.0435 0.7432 0.041 Uiso 1 1 calc R . .
C1' C 0.18229(17) 0.1190(4) 0.80642(15) 0.0329(5) Uani 1 1 d . . .
O1' O 0.15975(14) 0.3054(3) 0.84717(12) 0.0462(4) Uani 1 1 d . . .
C1G C -0.06036(18) -0.3150(4) 0.73478(19) 0.0428(6) Uani 1 1 d . . .
H1G1 H -0.0269 -0.4519 0.7106 0.051 Uiso 1 1 calc R . .
H1G2 H -0.0607 -0.3414 0.8097 0.051 Uiso 1 1 calc R . .
C1D C -0.17684(18) -0.2940(4) 0.66738(18) 0.0371(5) Uani 1 1 d . . .
C1E1 C -0.2201(2) -0.4550(4) 0.58659(19) 0.0454(6) Uani 1 1 d . . .
H1E1 H -0.1770 -0.5786 0.5730 0.054 Uiso 1 1 calc R . .
C1E2 C -0.2430(2) -0.1124(5) 0.6863(2) 0.0529(6) Uani 1 1 d . . .
H1E2 H -0.2151 -0.0036 0.7410 0.064 Uiso 1 1 calc R . .
C1Z1 C -0.3273(2) -0.4338(5) 0.5256(2) 0.0556(7) Uani 1 1 d . . .
H1Z1 H -0.3558 -0.5439 0.4715 0.067 Uiso 1 1 calc R . .
C1Z2 C -0.3497(2) -0.0901(6) 0.6250(2) 0.0620(7) Uani 1 1 d . . .
H1Z2 H -0.3930 0.0335 0.6382 0.074 Uiso 1 1 calc R . .
C1H C -0.3916(2) -0.2524(5) 0.5441(2) 0.0591(8) Uani 1 1 d . . .
H1H H -0.4633 -0.2383 0.5025 0.071 Uiso 1 1 calc R . .
N2 N 0.25627(14) 0.1127(3) 0.74821(13) 0.0325(4) Uani 1 1 d . . .
H2 H 0.2817 -0.0206 0.7332 0.039 Uiso 1 1 calc R . .
C2A C 0.29275(17) 0.3287(4) 0.71117(15) 0.0326(5) Uani 1 1 d . . .
C2' C 0.20391(19) 0.4689(4) 0.63486(16) 0.0352(5) Uani 1 1 d . . .
O2' O 0.11460(12) 0.3669(3) 0.59234(11) 0.0422(4) Uani 1 1 d . . .
C2B C 0.39582(17) 0.4033(4) 0.73691(16) 0.0370(5) Uani 1 1 d . . .
H2B H 0.4065 0.5452 0.7042 0.044 Uiso 1 1 calc R . .
C2G C 0.49617(18) 0.3023(4) 0.80772(17) 0.0390(5) Uani 1 1 d . . .
C2D1 C 0.5009(2) 0.0983(5) 0.8707(2) 0.0535(7) Uani 1 1 d . . .
H2D1 H 0.4375 0.0127 0.8679 0.064 Uiso 1 1 calc R . .
C2D2 C 0.59319(19) 0.4233(5) 0.8145(2) 0.0559(7) Uani 1 1 d . . .
H2D2 H 0.5923 0.5604 0.7740 0.067 Uiso 1 1 calc R . .
C2E1 C 0.5991(2) 0.0233(5) 0.9369(2) 0.0632(8) Uani 1 1 d . . .
H2E1 H 0.6009 -0.1117 0.9789 0.076 Uiso 1 1 calc R . .
C2E2 C 0.6914(2) 0.3433(6) 0.8805(2) 0.0704(9) Uani 1 1 d . . .
H2E2 H 0.7557 0.4254 0.8830 0.084 Uiso 1 1 calc R . .
C2Z C 0.6940(2) 0.1443(6) 0.9418(2) 0.0649(8) Uani 1 1 d . . .
H2Z H 0.7598 0.0913 0.9865 0.078 Uiso 1 1 calc R . .
O2" O 0.22178(13) 0.6820(3) 0.61787(13) 0.0462(4) Uani 1 1 d . . .
O1W O 0.0079(2) 0.3048(6) 0.9704(2) 0.0926(8) Uani 1 1 d . . .
H1W H 0.056(3) 0.303(7) 0.934(3) 0.086(11) Uiso 1 1 d . . .
H2W H 0.008(5) 0.159(11) 0.993(5) 0.17(2) Uiso 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

























N1 C1B 1.501(3) . ?
C1A C1' 1.505(3) . ?
C1A C1B 1.537(3) . ?
C1B C1G 1.528(3) . ?
C1' O1' 1.240(3) . ?
C1' N2 1.337(3) . ?
C1G C1D 1.509(3) . ?
C1D C1E1 1.379(3) . ?
C1D C1E2 1.384(3) . ?
C1E1 C1Z1 1.386(3) . ?
C1E2 C1Z2 1.382(4) . ?
C1Z1 C1H 1.367(4) . ?
C1Z2 C1H 1.382(4) . ?
N2 C2A 1.428(3) . ?
C2A C2B 1.330(3) . ?
C2A C2' 1.510(3) . ?
C2' O2" 1.255(3) . ?
C2' O2' 1.261(3) . ?
C2B C2G 1.472(3) . ?
C2G C2D2 1.389(3) . ?
C2G C2D1 1.398(3) . ?
C2D1 C2E1 1.378(3) . ?
C2D2 C2E2 1.387(4) . ?
C2E1 C2Z 1.370(4) . ?
C2E2 C2Z 1.365(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
































C1' C1A C1B 109.37(16) . . ?
N1 C1B C1G 110.61(17) . . ?
N1 C1B C1A 109.06(16) . . ?
C1G C1B C1A 111.96(17) . . ?
O1' C1' N2 121.7(2) . . ?
O1' C1' C1A 121.1(2) . . ?
N2 C1' C1A 117.02(19) . . ?
C1D C1G C1B 113.48(19) . . ?
C1E1 C1D C1E2 118.5(2) . . ?
C1E1 C1D C1G 121.2(2) . . ?
C1E2 C1D C1G 120.3(2) . . ?
C1D C1E1 C1Z1 120.5(2) . . ?
C1Z2 C1E2 C1D 121.1(3) . . ?
C1H C1Z1 C1E1 120.5(2) . . ?
C1E2 C1Z2 C1H 119.7(3) . . ?
C1Z1 C1H C1Z2 119.7(2) . . ?
C1' N2 C2A 119.56(18) . . ?
C2B C2A N2 124.70(18) . . ?
C2B C2A C2' 120.96(19) . . ?
N2 C2A C2' 114.31(17) . . ?
O2" C2' O2' 123.1(2) . . ?
O2" C2' C2A 118.5(2) . . ?
O2' C2' C2A 118.39(19) . . ?
C2A C2B C2G 131.8(2) . . ?
C2D2 C2G C2D1 117.6(2) . . ?
C2D2 C2G C2B 117.2(2) . . ?
C2D1 C2G C2B 125.2(2) . . ?
C2E1 C2D1 C2G 120.4(2) . . ?
C2E2 C2D2 C2G 121.2(3) . . ?
C2Z C2E1 C2D1 121.1(3) . . ?
C2Z C2E2 C2D2 120.2(3) . . ?
C2E2 C2Z C2E1 119.5(3) . . ?



_diffrn_measured_fraction_theta_max 0.971

_diffrn_reflns_theta_full        30.53

_diffrn_measured_fraction_theta_full 0.971

_refine_diff_density_max         0.178

_refine_diff_density_min         -0.184

_refine_diff_density_rms         0.036
_database_code_depnum_ccdc_archive 'CCDC 918325'
#######################################################################
#
#                 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_bff
#TrackingRef 'bfdf-bff.cif'


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

_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

'(β³-homophenylalanyl)-phenylalanine) hemihydrate'

;



_chemical_name_common            'PEPSEQ A=2 PHE*-PHE*'

_chemical_melting_point          ?

_chemical_formula_moiety         '2(C19 H22 N2 O3), 1(H2 O1)'



# Two Hydrogens from water neither located nor fixed



_chemical_formula_sum            'C38 H46 N4 O7'



_chemical_formula_weight         670.8

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'



_symmetry_cell_setting           Orthorhombic

_symmetry_space_group_name_Hall  'P 2ac 2ab'

_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, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'



_cell_length_a                   5.7860(7)

_cell_length_b                   24.375(3)

_cell_length_c                   25.285(3)

_cell_angle_alpha                90.00

_cell_angle_beta                 90.00

_cell_angle_gamma                90.00

_cell_volume                     3566.0(7)

_cell_formula_units_Z            4

_cell_measurement_temperature    296(2)

_cell_measurement_reflns_used    ?

_cell_measurement_theta_min      ?

_cell_measurement_theta_max      ?



_exptl_crystal_description       'Rectangular rod'

_exptl_crystal_colour            colourless

_exptl_crystal_size_max          0.25

_exptl_crystal_size_mid          0.03

_exptl_crystal_size_min          0.02

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.246

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             1424

_exptl_absorpt_coefficient_mu    0.086

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.9787

_exptl_absorpt_correction_T_max  0.9983

_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'



_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 Kappa APEX II CCD detector'

_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            25027

_diffrn_reflns_av_R_equivalents  0.1922

_diffrn_reflns_av_sigmaI/netI    0.2152

_diffrn_reflns_limit_h_min       -6

_diffrn_reflns_limit_h_max       6

_diffrn_reflns_limit_k_min       -26

_diffrn_reflns_limit_k_max       26

_diffrn_reflns_limit_l_min       -22

_diffrn_reflns_limit_l_max       27

_diffrn_reflns_theta_min         1.61

_diffrn_reflns_theta_max         23.04

_reflns_number_total             5003

_reflns_number_gt                2053

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       'KAPPA APEX II (BRUKER-AXS)'

_computing_cell_refinement       'SAINTPLUS (BRUKER-AXS)'

_computing_data_reduction        'SAINTPLUS (BRUKER-AXS)'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

_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 > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² are statistically about twice as large as those based on F, and R-

factors based on ALL data will be even larger.

;



_refine_ls_structure_factor_coef Fsqd

_refine_ls_matrix_type           full

_refine_ls_weighting_scheme      calc

_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0807P)²+0.0000P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary     direct

_atom_sites_solution_secondary   difmap

_atom_sites_solution_hydrogens   geom

_refine_ls_hydrogen_treatment    mixed

_refine_ls_extinction_method     SHELXL

_refine_ls_extinction_coef       0.0025(11)

_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^

_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'

_refine_ls_abs_structure_Flack   -1(3)

_refine_ls_number_reflns         5003

_refine_ls_number_parameters     428

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.2237

_refine_ls_R_factor_gt           0.0781

_refine_ls_wR_factor_ref         0.2077

_refine_ls_wR_factor_gt          0.1468

_refine_ls_goodness_of_fit_ref   0.972

_refine_ls_restrained_S_all      0.972

_refine_ls_shift/su_max          0.002

_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





























































































N1A N 0.0575(12) 0.5927(3) 0.6493(2) 0.052(2) Uani 1 1 d . . .
H1A1 H 0.1745 0.5758 0.6333 0.077 Uiso 1 1 calc R . .
H1A2 H 0.0713 0.6288 0.6450 0.077 Uiso 1 1 calc R . .
H1A3 H -0.0754 0.5814 0.6353 0.077 Uiso 1 1 calc R . .
C1AA C 0.0583(14) 0.5170(3) 0.7155(3) 0.043(2) Uani 1 1 d . . .
H1A4 H 0.0515 0.5085 0.7530 0.051 Uiso 1 1 calc R . .
H1A5 H -0.0780 0.5017 0.6988 0.051 Uiso 1 1 calc R . .
C1BA C 0.0613(17) 0.5791(3) 0.7079(3) 0.045(2) Uani 1 1 d . . .
H1BA H 0.2076 0.5928 0.7223 0.055 Uiso 1 1 calc R . .
C1'A C 0.2728(17) 0.4915(3) 0.6917(3) 0.044(2) Uani 1 1 d . . .
O1'A O 0.4614(11) 0.4954(3) 0.7134(2) 0.0609(19) Uani 1 1 d . . .
C1GA C -0.1326(16) 0.6096(3) 0.7355(3) 0.055(3) Uani 1 1 d . . .
H1G1 H -0.2784 0.5921 0.7270 0.066 Uiso 1 1 calc R . .
H1G2 H -0.1383 0.6469 0.7223 0.066 Uiso 1 1 calc R . .
C1DA C -0.1042(18) 0.6110(4) 0.7954(3) 0.048(2) Uani 1 1 d . . .
C11A C 0.0785(19) 0.6367(4) 0.8179(4) 0.063(3) Uani 1 1 d . . .
H11A H 0.1902 0.6524 0.7962 0.076 Uiso 1 1 calc R . .
C12A C -0.2703(19) 0.5881(4) 0.8269(5) 0.070(3) Uani 1 1 d . . .
H12A H -0.3965 0.5706 0.8116 0.084 Uiso 1 1 calc R . .
C13A C 0.103(3) 0.6403(5) 0.8716(5) 0.091(4) Uani 1 1 d . . .
H13A H 0.2294 0.6580 0.8868 0.110 Uiso 1 1 calc R . .
C14A C -0.252(3) 0.5909(5) 0.8809(5) 0.094(4) Uani 1 1 d . . .
H14A H -0.3645 0.5756 0.9025 0.113 Uiso 1 1 calc R . .
C1HA C -0.065(3) 0.6166(5) 0.9022(4) 0.093(4) Uani 1 1 d . . .
H1HA H -0.0516 0.6182 0.9388 0.112 Uiso 1 1 calc R . .
N2A N 0.2515(12) 0.4697(3) 0.6426(3) 0.046(2) Uani 1 1 d . . .
H2A H 0.1172 0.4614 0.6304 0.056 Uiso 1 1 calc R . .
C2AA C 0.4571(16) 0.4602(4) 0.6106(3) 0.048(2) Uani 1 1 d . . .
H2AA H 0.5579 0.4346 0.6295 0.057 Uiso 1 1 calc R . .
C2'A C 0.5919(19) 0.5150(4) 0.6022(3) 0.048(2) Uani 1 1 d . . .
O2'A O 0.8022(11) 0.5111(2) 0.5953(2) 0.0614(18) Uani 1 1 d . . .
C2BA C 0.3916(18) 0.4345(4) 0.5573(3) 0.064(3) Uani 1 1 d . . .
H2B1 H 0.2956 0.4606 0.5384 0.076 Uiso 1 1 calc R . .
H2B2 H 0.5324 0.4299 0.5369 0.076 Uiso 1 1 calc R . .
C2GA C 0.267(2) 0.3800(4) 0.5579(4) 0.074(3) Uani 1 1 d . . .
C21A C 0.366(3) 0.3351(7) 0.5778(5) 0.146(6) Uiso 1 1 d . . .
H21A H 0.5147 0.3368 0.5915 0.175 Uiso 1 1 calc R . .
C22A C 0.079(3) 0.3733(6) 0.5281(7) 0.165(7) Uani 1 1 d . . .
H22A H 0.0155 0.4028 0.5098 0.197 Uiso 1 1 calc R . .
C23A C 0.243(4) 0.2846(8) 0.5780(7) 0.171(8) Uiso 1 1 d . . .
H23A H 0.3030 0.2546 0.5959 0.205 Uiso 1 1 calc R . .
C24A C -0.025(3) 0.3202(8) 0.5246(7) 0.168(7) Uiso 1 1 d . . .
H24A H -0.1463 0.3146 0.5010 0.202 Uiso 1 1 calc R . .
C2NA C 0.046(3) 0.2800(6) 0.5532(7) 0.160(7) Uani 1 1 d . . .
H2NA H -0.0416 0.2482 0.5562 0.193 Uiso 1 1 calc R . .
O2"A O 0.4730(11) 0.5587(3) 0.5998(2) 0.0587(19) Uani 1 1 d . . .
N1B N 0.8790(12) 0.3494(3) 1.0480(2) 0.0424(19) Uani 1 1 d . . .
H1B1 H 0.9146 0.3798 1.0659 0.064 Uiso 1 1 calc R . .
H1B2 H 1.0023 0.3380 1.0302 0.064 Uiso 1 1 calc R . .
H1B3 H 0.8346 0.3235 1.0706 0.064 Uiso 1 1 calc R . .
C1AB C 0.6223(14) 0.3084(3) 0.9821(3) 0.046(2) Uani 1 1 d . . .
H1A6 H 0.7471 0.2988 0.9583 0.055 Uiso 1 1 calc R . .
H1A7 H 0.6115 0.2796 1.0085 0.055 Uiso 1 1 calc R . .
C1BB C 0.6854(15) 0.3615(3) 1.0100(3) 0.043(2) Uani 1 1 d . . .
H1BB H 0.5510 0.3746 1.0299 0.052 Uiso 1 1 calc R . .
C1'B C 0.4015(17) 0.3096(3) 0.9513(4) 0.041(2) Uani 1 1 d . . .
O1'B O 0.2142(11) 0.3232(2) 0.9731(2) 0.0552(17) Uani 1 1 d . . .
C1GB C 0.7655(15) 0.4067(3) 0.9730(3) 0.048(2) Uani 1 1 d . . .
H1G3 H 0.8334 0.4356 0.9943 0.058 Uiso 1 1 calc R . .
H1G4 H 0.8876 0.3918 0.9509 0.058 Uiso 1 1 calc R . .
C1DB C 0.5869(17) 0.4326(3) 0.9370(4) 0.044(2) Uani 1 1 d . . .
C11B C 0.4005(18) 0.4602(4) 0.9585(3) 0.055(3) Uani 1 1 d . . .
H11B H 0.3845 0.4615 0.9950 0.066 Uiso 1 1 calc R . .
C12B C 0.6006(19) 0.4309(4) 0.8834(4) 0.065(3) Uani 1 1 d . . .
H12B H 0.7233 0.4122 0.8679 0.078 Uiso 1 1 calc R . .
C13B C 0.2384(19) 0.4855(4) 0.9274(4) 0.068(3) Uani 1 1 d . . .
H13B H 0.1143 0.5037 0.9429 0.082 Uiso 1 1 calc R . .
C14B C 0.442(2) 0.4555(4) 0.8515(4) 0.067(3) Uani 1 1 d . . .
H14B H 0.4569 0.4529 0.8149 0.081 Uiso 1 1 calc R . .
C1HB C 0.260(2) 0.4840(4) 0.8724(5) 0.073(3) Uani 1 1 d . . .
H1HB H 0.1547 0.5018 0.8507 0.088 Uiso 1 1 calc R . .
N2B N 0.4101(12) 0.2963(3) 0.9009(3) 0.0439(19) Uani 1 1 d . . .
H2B H 0.5395 0.2851 0.8880 0.053 Uiso 1 1 calc R . .
C2AB C 0.2073(14) 0.2995(3) 0.8651(3) 0.040(2) Uani 1 1 d . . .
H2AB H 0.1155 0.3317 0.8749 0.049 Uiso 1 1 calc R . .
C2'B C 0.0533(17) 0.2485(4) 0.8694(3) 0.045(2) Uani 1 1 d . . .
O2'B O 0.1453(11) 0.2026(2) 0.8707(2) 0.0530(18) Uani 1 1 d . . .
C2BB C 0.2961(16) 0.3074(3) 0.8081(3) 0.050(2) Uani 1 1 d . . .
H2B3 H 0.4028 0.3381 0.8072 0.060 Uiso 1 1 calc R . .
H2B4 H 0.3796 0.2748 0.7972 0.060 Uiso 1 1 calc R . .
C2GB C 0.1029(18) 0.3178(5) 0.7705(4) 0.056(3) Uani 1 1 d . . .
C21B C -0.0065(19) 0.3679(5) 0.7694(4) 0.070(3) Uani 1 1 d . . .
H21B H 0.0428 0.3964 0.7911 0.084 Uiso 1 1 calc R . .
C22B C 0.020(2) 0.2780(5) 0.7389(5) 0.102(5) Uani 1 1 d . . .
H22B H 0.0922 0.2439 0.7392 0.123 Uiso 1 1 calc R . .
C23B C -0.196(2) 0.3753(5) 0.7344(5) 0.087(4) Uani 1 1 d . . .
H23B H -0.2700 0.4092 0.7326 0.105 Uiso 1 1 calc R . .
C24B C -0.167(3) 0.2855(6) 0.7060(6) 0.144(7) Uani 1 1 d . . .
H24B H -0.2211 0.2567 0.6854 0.173 Uiso 1 1 calc R . .
C2NB C -0.269(3) 0.3341(7) 0.7041(5) 0.134(7) Uani 1 1 d . . .
H2NB H -0.3928 0.3396 0.6813 0.160 Uiso 1 1 calc R . .
O2"B O -0.1611(12) 0.2577(3) 0.8675(2) 0.077(2) Uani 1 1 d . . .
O1W O 0.5928(14) 0.1748(3) 0.8254(3) 0.115(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


















































N1A C1BA 1.517(9) . ?
C1AA C1'A 1.513(11) . ?
C1AA C1BA 1.527(10) . ?
C1BA C1GA 1.516(11) . ?
C1'A O1'A 1.226(9) . ?
C1'A N2A 1.355(10) . ?
C1GA C1DA 1.524(11) . ?
C1DA C11A 1.354(12) . ?
C1DA C12A 1.366(12) . ?
C11A C13A 1.369(13) . ?
C12A C14A 1.371(14) . ?
C13A C1HA 1.372(17) . ?
C14A C1HA 1.359(17) . ?
N2A C2AA 1.457(10) . ?
C2AA C2BA 1.535(10) . ?
C2AA C2'A 1.561(12) . ?
C2'A O2'A 1.233(11) . ?
C2'A O2"A 1.269(10) . ?
C2BA C2GA 1.512(13) . ?
C2GA C22A 1.333(15) . ?
C2GA C21A 1.336(16) . ?
C21A C23A 1.42(2) . ?
C22A C24A 1.43(2) . ?
C23A C2NA 1.30(2) . ?
C24A C2NA 1.286(18) . ?
N1B C1BB 1.506(10) . ?
C1AB C1'B 1.497(11) . ?
C1AB C1BB 1.518(10) . ?
C1BB C1GB 1.517(10) . ?
C1'B O1'B 1.261(10) . ?
C1'B N2B 1.317(9) . ?
C1GB C1DB 1.515(12) . ?
C1DB C12B 1.358(10) . ?
C1DB C11B 1.381(12) . ?
C11B C13B 1.370(12) . ?
C12B C14B 1.363(13) . ?
C13B C1HB 1.397(12) . ?
C14B C1HB 1.364(13) . ?
N2B C2AB 1.483(9) . ?
C2AB C2'B 1.534(11) . ?
C2AB C2BB 1.542(11) . ?
C2'B O2'B 1.240(10) . ?
C2'B O2"B 1.262(10) . ?
C2BB C2GB 1.489(12) . ?
C2GB C22B 1.345(13) . ?
C2GB C21B 1.377(12) . ?
C21B C23B 1.421(14) . ?
C22B C24B 1.375(17) . ?
C23B C2NB 1.331(14) . ?
C24B C2NB 1.325(17) . ?



loop_

_geom_angle_atom_site_label_1

_geom_angle_atom_site_label_2

_geom_angle_atom_site_label_3

_geom_angle

_geom_angle_site_symmetry_1

_geom_angle_site_symmetry_3

_geom_angle_publ_flag
































































C1'A C1AA C1BA 110.3(7) . . ?
N1A C1BA C1GA 109.4(7) . . ?
N1A C1BA C1AA 109.9(6) . . ?
C1GA C1BA C1AA 114.7(8) . . ?
O1'A C1'A N2A 121.5(8) . . ?
O1'A C1'A C1AA 121.3(8) . . ?
N2A C1'A C1AA 116.8(8) . . ?
C1BA C1GA C1DA 112.9(7) . . ?
C11A C1DA C12A 119.6(9) . . ?
C11A C1DA C1GA 120.8(9) . . ?
C12A C1DA C1GA 119.6(10) . . ?
C1DA C11A C13A 121.9(11) . . ?
C1DA C12A C14A 120.3(11) . . ?
C11A C13A C1HA 117.2(13) . . ?
C1HA C14A C12A 118.7(12) . . ?
C14A C1HA C13A 122.3(12) . . ?
C1'A N2A C2AA 119.8(7) . . ?
N2A C2AA C2BA 110.6(8) . . ?
N2A C2AA C2'A 110.4(7) . . ?
C2BA C2AA C2'A 110.7(7) . . ?
O2'A C2'A O2"A 126.4(10) . . ?
O2'A C2'A C2AA 116.5(10) . . ?
O2"A C2'A C2AA 116.9(9) . . ?
C2GA C2BA C2AA 117.9(8) . . ?
C22A C2GA C21A 117.5(13) . . ?
C22A C2GA C2BA 119.6(11) . . ?
C21A C2GA C2BA 121.2(12) . . ?
C2GA C21A C23A 119.7(17) . . ?
C2GA C22A C24A 119.3(14) . . ?
C2NA C23A C21A 120.7(19) . . ?
C2NA C24A C22A 121.4(17) . . ?
C24A C2NA C23A 118.9(18) . . ?
C1'B C1AB C1BB 115.5(7) . . ?
N1B C1BB C1GB 108.0(7) . . ?
N1B C1BB C1AB 108.0(6) . . ?
C1GB C1BB C1AB 114.0(7) . . ?
O1'B C1'B N2B 121.4(8) . . ?
O1'B C1'B C1AB 120.7(8) . . ?
N2B C1'B C1AB 117.9(9) . . ?
C1DB C1GB C1BB 117.7(7) . . ?
C12B C1DB C11B 116.9(9) . . ?
C12B C1DB C1GB 123.1(9) . . ?
C11B C1DB C1GB 120.0(8) . . ?
C13B C11B C1DB 121.9(9) . . ?
C1DB C12B C14B 122.6(10) . . ?
C11B C13B C1HB 119.7(10) . . ?
C12B C14B C1HB 120.8(10) . . ?
C14B C1HB C13B 118.1(10) . . ?
C1'B N2B C2AB 123.2(7) . . ?
N2B C2AB C2'B 111.9(7) . . ?
N2B C2AB C2BB 108.2(7) . . ?
C2'B C2AB C2BB 111.1(6) . . ?
O2'B C2'B O2"B 125.8(9) . . ?
O2'B C2'B C2AB 119.0(9) . . ?
O2"B C2'B C2AB 115.1(9) . . ?
C2GB C2BB C2AB 111.6(8) . . ?
C22B C2GB C21B 117.6(10) . . ?
C22B C2GB C2BB 121.7(10) . . ?
C21B C2GB C2BB 120.6(10) . . ?
C2GB C21B C23B 118.8(10) . . ?
C2GB C22B C24B 122.9(12) . . ?
C2NB C23B C21B 120.4(12) . . ?
C2NB C24B C22B 119.5(13) . . ?
C24B C2NB C23B 120.8(13) . . ?



_diffrn_measured_fraction_theta_max 1.000

_diffrn_reflns_theta_full        23.04

_diffrn_measured_fraction_theta_full 1.000

_refine_diff_density_max         0.388

_refine_diff_density_min         -0.231

_refine_diff_density_rms         0.052

#===END





_database_code_depnum_ccdc_archive 'CCDC 918326'
