# Electronic Supplementary Material (ESI) for Soft Matter.
# 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_mc237f
_database_code_depnum_ccdc_archive 'CCDC 1057628'
_audit_update_record             
;
2015-04-02 deposited with the CCDC.
2015-10-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 Boc-L-Cys(Me)-L-Leu-OMe
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H30 N2 O5 S'
_chemical_formula_weight         362.48
_chemical_absolute_configuration syn

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'
N N 0.0311 0.0180 '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'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   'P 65'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'x-y, x, z+5/6'
'y, -x+y, z+1/6'

_cell_length_a                   11.4458(2)
_cell_length_b                   11.4458(2)
_cell_length_c                   27.7551(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3148.95(10)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5829
_cell_measurement_theta_min      4.4330
_cell_measurement_theta_max      51.2950

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1176
_exptl_absorpt_coefficient_mu    1.580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.81551
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 Data collection was performed up to theta 51.25 deg as the
 extremely thin crystal did not diffract significantly
 beyond 1.0 Ang resolution.
 The choice of space group P65 (rather than its enantiomorph
 P61) is based on the known configuration of the chiral amino
 acids L-Cys and L-Leu used in the synthesis.
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1274
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18290
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         4.46
_diffrn_reflns_theta_max         51.25
_reflns_number_total             2281
_reflns_number_gt                2056
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 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)+(0.0689P)²+0.3892P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_number_reflns         2281
_refine_ls_number_parameters     217
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_ref         0.1083
_refine_ls_wR_factor_gt          0.1040
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C01 C -0.2364(4) -0.4365(4) 0.32817(15) 0.0707(12) Uani 1 1 d . . .
C02 C -0.3379(6) -0.4891(6) 0.2873(2) 0.1128(19) Uani 1 1 d U . .
H02A H -0.2984 -0.4347 0.2592 0.169 Uiso 1 1 calc R . .
H02B H -0.4166 -0.4850 0.2965 0.169 Uiso 1 1 calc R . .
H02C H -0.3629 -0.5809 0.2805 0.169 Uiso 1 1 calc R . .
C03 C -0.2939(8) -0.5237(5) 0.3713(2) 0.155(3) Uani 1 1 d U . .
H03A H -0.3089 -0.6123 0.3643 0.233 Uiso 1 1 calc R . .
H03B H -0.3780 -0.5294 0.3796 0.233 Uiso 1 1 calc R . .
H03C H -0.2320 -0.4857 0.3977 0.233 Uiso 1 1 calc R . .
C04 C -0.1108(6) -0.4274(6) 0.3127(3) 0.158(3) Uani 1 1 d U . .
H04A H -0.0412 -0.3753 0.3357 0.236 Uiso 1 1 calc R . .
H04B H -0.0857 -0.3844 0.2818 0.236 Uiso 1 1 calc R . .
H04C H -0.1225 -0.5163 0.3105 0.236 Uiso 1 1 calc R . .
OU O -0.2127(3) -0.3048(3) 0.34450(9) 0.0827(9) Uani 1 1 d . . .
C0 C -0.1707(4) -0.2000(4) 0.31499(15) 0.0589(10) Uani 1 1 d . . .
O0 O -0.1470(3) -0.2011(3) 0.27266(10) 0.0836(9) Uani 1 1 d . . .
N1 N -0.1582(3) -0.0913(3) 0.33776(10) 0.0626(9) Uani 1 1 d . . .
H1 H -0.1710 -0.0952 0.3684 0.075 Uiso 1 1 calc R . .
C1A C -0.1240(3) 0.0318(3) 0.31273(12) 0.0505(9) Uani 1 1 d . . .
H1A H -0.1511 0.0096 0.2790 0.061 Uiso 1 1 calc R . .
C1B C -0.1969(4) 0.1006(4) 0.33340(15) 0.0689(11) Uani 1 1 d . . .
H1B1 H -0.1524 0.1928 0.3218 0.083 Uiso 1 1 calc R . .
H1B2 H -0.1869 0.1041 0.3682 0.083 Uiso 1 1 calc R . .
S1 S -0.37020(13) 0.02454(17) 0.31976(5) 0.1052(5) Uani 1 1 d . . .
C1D C -0.3624(7) 0.0725(9) 0.2583(2) 0.147(3) Uani 1 1 d U . .
H1D1 H -0.2817 0.1574 0.2530 0.221 Uiso 1 1 calc R . .
H1D2 H -0.4397 0.0811 0.2508 0.221 Uiso 1 1 calc R . .
H1D3 H -0.3618 0.0050 0.2380 0.221 Uiso 1 1 calc R . .
C1 C 0.0267(3) 0.1337(3) 0.31403(13) 0.0475(8) Uani 1 1 d . . .
O1 O 0.0909(2) 0.1671(3) 0.35217(9) 0.0611(7) Uani 1 1 d . . .
N2 N 0.0803(3) 0.1898(3) 0.27201(10) 0.0510(7) Uani 1 1 d . . .
H2 H 0.0326 0.1587 0.2463 0.061 Uiso 1 1 calc R . .
C2A C 0.2171(3) 0.3020(3) 0.26815(12) 0.0480(9) Uani 1 1 d . . .
H2A H 0.2784 0.2775 0.2839 0.058 Uiso 1 1 calc R . .
C2B C 0.2544(4) 0.3296(4) 0.21484(12) 0.0552(9) Uani 1 1 d . . .
H2B1 H 0.3354 0.4171 0.2118 0.066 Uiso 1 1 calc R . .
H2B2 H 0.1824 0.3338 0.1979 0.066 Uiso 1 1 calc R . .
C2G C 0.2785(4) 0.2241(4) 0.19068(13) 0.0593(10) Uani 1 1 d . . .
H2G H 0.2070 0.1345 0.2007 0.071 Uiso 1 1 calc R . .
C2D1 C 0.2729(4) 0.2344(5) 0.13574(14) 0.0841(14) Uani 1 1 d . . .
H2D1 H 0.3338 0.3254 0.1258 0.126 Uiso 1 1 calc R . .
H2D2 H 0.1828 0.2094 0.1261 0.126 Uiso 1 1 calc R . .
H2D3 H 0.2985 0.1748 0.1209 0.126 Uiso 1 1 calc R . .
C2D2 C 0.4130(4) 0.2407(5) 0.20591(18) 0.0805(13) Uani 1 1 d . . .
H2D4 H 0.4269 0.1742 0.1900 0.121 Uiso 1 1 calc R . .
H2D5 H 0.4135 0.2294 0.2402 0.121 Uiso 1 1 calc R . .
H2D6 H 0.4840 0.3292 0.1972 0.121 Uiso 1 1 calc R . .
C2 C 0.2305(5) 0.4273(4) 0.29242(15) 0.0653(11) Uani 1 1 d . . .
O2 O 0.1435(4) 0.4506(3) 0.30063(12) 0.0879(9) Uani 1 1 d . . .
OT O 0.3591(3) 0.5091(3) 0.30290(14) 0.1100(13) Uani 1 1 d . . .
CT C 0.3942(7) 0.6378(6) 0.3238(3) 0.142(2) Uani 1 1 d U . .
HT1 H 0.4099 0.7014 0.2986 0.214 Uiso 1 1 calc R . .
HT2 H 0.4745 0.6695 0.3428 0.214 Uiso 1 1 calc R . .
HT3 H 0.3216 0.6282 0.3439 0.214 Uiso 1 1 calc 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
C01 0.080(3) 0.046(2) 0.066(3) -0.004(2) -0.013(2) 0.016(2)
C02 0.103(4) 0.104(4) 0.124(4) -0.045(3) -0.054(3) 0.047(3)
C03 0.271(9) 0.063(3) 0.078(4) 0.006(3) -0.001(5) 0.045(4)
C04 0.092(4) 0.109(4) 0.284(10) 0.040(5) 0.010(5) 0.059(4)
OU 0.125(3) 0.0543(17) 0.0394(15) 0.0008(13) 0.0023(15) 0.0227(16)
C0 0.061(2) 0.067(3) 0.045(3) 0.007(2) -0.0011(19) 0.029(2)
O0 0.139(3) 0.091(2) 0.0354(18) 0.0087(13) 0.0220(16) 0.069(2)
N1 0.089(2) 0.058(2) 0.0284(15) 0.0024(15) 0.0129(15) 0.0277(17)
C1A 0.058(2) 0.059(2) 0.035(2) 0.0032(17) -0.0005(17) 0.0294(19)
C1B 0.073(3) 0.086(3) 0.057(2) 0.005(2) 0.010(2) 0.046(2)
S1 0.0610(7) 0.1417(13) 0.1089(10) 0.0094(8) 0.0137(7) 0.0478(7)
C1D 0.137(5) 0.260(8) 0.092(4) 0.005(5) -0.017(4) 0.134(6)
C1 0.052(2) 0.058(2) 0.034(2) 0.0038(19) 0.002(2) 0.0293(18)
O1 0.0665(16) 0.0827(18) 0.0330(15) 0.0019(13) -0.0091(13) 0.0366(14)
N2 0.0556(19) 0.0590(18) 0.0291(17) -0.0032(14) -0.0030(14) 0.0218(16)
C2A 0.047(2) 0.050(2) 0.044(2) -0.0037(16) -0.0020(16) 0.0219(18)
C2B 0.053(2) 0.055(2) 0.050(2) 0.0043(18) 0.0107(17) 0.0213(18)
C2G 0.052(2) 0.055(2) 0.056(2) 0.0006(19) 0.0131(18) 0.0157(18)
C2D1 0.085(3) 0.103(3) 0.052(3) -0.009(2) 0.015(2) 0.038(3)
C2D2 0.072(3) 0.084(3) 0.092(3) -0.016(2) -0.001(2) 0.044(2)
C2 0.070(3) 0.065(3) 0.061(3) -0.002(2) 0.002(2) 0.034(3)
O2 0.089(2) 0.091(2) 0.104(3) -0.0051(17) 0.0099(18) 0.0602(19)
OT 0.073(2) 0.089(2) 0.148(3) -0.061(2) -0.013(2) 0.0252(18)
CT 0.138(5) 0.094(4) 0.184(6) -0.082(4) -0.030(4) 0.049(4)

_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
C01 C04 1.453(7) . ?
C01 C03 1.484(7) . ?
C01 OU 1.464(5) . ?
C01 C02 1.515(6) . ?
OU C0 1.329(5) . ?
C0 O0 1.208(4) . ?
C0 N1 1.337(5) . ?
N1 C1A 1.439(5) . ?
C1A C1B 1.517(5) . ?
C1A C1 1.524(5) . ?
C1B S1 1.763(4) . ?
S1 C1D 1.780(6) . ?
C1 O1 1.236(4) . ?
C1 N2 1.325(4) . ?
N2 C2A 1.450(4) . ?
C2A C2B 1.529(5) . ?
C2A C2 1.521(5) . ?
C2B C2G 1.523(5) . ?
C2G C2D1 1.533(6) . ?
C2G C2D2 1.514(5) . ?
C2 O2 1.176(5) . ?
C2 OT 1.323(5) . ?
OT CT 1.440(6) . ?

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
C04 C01 C03 112.1(5) . . ?
C04 C01 OU 110.5(4) . . ?
C03 C01 OU 103.5(4) . . ?
C04 C01 C02 110.0(5) . . ?
C03 C01 C02 110.0(4) . . ?
OU C01 C02 110.5(4) . . ?
C0 OU C01 122.4(3) . . ?
O0 C0 OU 124.9(4) . . ?
O0 C0 N1 123.3(4) . . ?
OU C0 N1 111.8(4) . . ?
C0 N1 C1A 122.2(3) . . ?
N1 C1A C1B 112.0(3) . . ?
N1 C1A C1 112.8(3) . . ?
C1B C1A C1 107.4(3) . . ?
C1A C1B S1 115.9(3) . . ?
C1B S1 C1D 100.5(3) . . ?
O1 C1 N2 123.0(3) . . ?
O1 C1 C1A 121.9(3) . . ?
N2 C1 C1A 115.0(3) . . ?
C1 N2 C2A 121.9(3) . . ?
N2 C2A C2B 108.7(3) . . ?
N2 C2A C2 111.0(3) . . ?
C2B C2A C2 110.3(3) . . ?
C2A C2B C2G 113.9(3) . . ?
C2D1 C2G C2D2 110.3(3) . . ?
C2D1 C2G C2B 110.2(3) . . ?
C2D2 C2G C2B 110.7(3) . . ?
O2 C2 OT 124.4(4) . . ?
O2 C2 C2A 127.0(4) . . ?
OT C2 C2A 108.5(4) . . ?
C2 OT CT 117.1(4) . . ?

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
C04 C01 OU C0 65.1(6) . . . . ?
C03 C01 OU C0 -174.6(4) . . . . ?
C02 C01 OU C0 -56.9(5) . . . . ?
C01 OU C0 O0 -0.7(6) . . . . ?
C01 OU C0 N1 179.0(3) . . . . y
O0 C0 N1 C1A 4.5(6) . . . . ?
OU C0 N1 C1A -175.2(3) . . . . y
C0 N1 C1A C1B 143.5(3) . . . . ?
C0 N1 C1A C1 -95.2(4) . . . . y
N1 C1A C1B S1 -73.8(4) . . . . y
C1 C1A C1B S1 161.7(3) . . . . ?
C1A C1B S1 C1D -74.4(4) . . . . y
N1 C1A C1 O1 -51.5(4) . . . . ?
C1B C1A C1 O1 72.4(4) . . . . ?
N1 C1A C1 N2 132.9(3) . . . . y
C1B C1A C1 N2 -103.2(3) . . . . ?
O1 C1 N2 C2A -4.4(5) . . . . ?
C1A C1 N2 C2A 171.1(3) . . . . y
C1 N2 C2A C2B 172.1(3) . . . . ?
C1 N2 C2A C2 -66.3(4) . . . . y
N2 C2A C2B C2G -72.8(4) . . . . y
C2 C2A C2B C2G 165.3(3) . . . . ?
C2A C2B C2G C2D1 163.0(3) . . . . y
C2A C2B C2G C2D2 -74.7(4) . . . . y
N2 C2A C2 O2 -22.0(6) . . . . ?
C2B C2A C2 O2 98.6(5) . . . . ?
N2 C2A C2 OT 158.5(3) . . . . y
C2B C2A C2 OT -80.9(4) . . . . ?
O2 C2 OT CT -3.0(7) . . . . ?
C2A C2 OT CT 176.6(5) . . . . y

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O0 0.86 2.09 2.929(4) 164.1 6
N2 H2 O1 0.86 2.01 2.868(4) 178.5 5_554

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        51.25
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.145
_refine_diff_density_rms         0.028

#===END===

# start Validation Reply Form
_vrf_THETM01_mc237f              
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Owing to its small size (lowest dimension 0.01 mm) and 
quality, the crystal did not significantly diffract beyond 1.0 
resolution. Attempts to grow larger single crystals failed. Indeed,
this peptide shows a remarkable tendency to give (twinned) hollow 
rods rather than single crystals.
;
_vrf_PLAT089_mc237f              
;
PROBLEM: Poor Data / Parameter Ratio (Zmax < 18) ........ 5.41 Note
RESPONSE: The low number of reflections in this ratio is related 
to the limited resolution at which data could be collected 
(see above). It has to be noted that the number of reflections used 
in this test is the number obtained by Laue group averaging. 
Since Friedel opposites were not combined, the actual data/parameter
ratio in our L.S. refinement is 2281/217, that is 10.51. In any 
case, we understand that many crystallographic parameters suffer
from the far from optimal crystal size and quality. We are 
confident, however, that the basic conformational features of the 
molecule and its packing mode, as discussed in this work, are 
unambiguously established.
 
;
_vrf_PLAT242_mc237f              
;
PROBLEM: Low Ueq as Compared to Neighbors for ..... C01 Check
RESPONSE: C01 is the quaternary carbon atom of a t-butyl group,
the low Ueq of which as compared to the methyl neighbors is a 
common observation. 
;
####################################################################### 
# 
# 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_mc238f
_database_code_depnum_ccdc_archive 'CCDC 1057629'
_audit_update_record             
;
2015-04-02 deposited with the CCDC.
2015-10-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 Boc-L-Leu-L-Cys(Me)-OMe
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H30 N2 O5 S'
_chemical_formula_weight         362.48
_chemical_absolute_configuration syn

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'
N N 0.0311 0.0180 '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'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   5.08911(7)
_cell_length_b                   12.09583(13)
_cell_length_c                   32.4406(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1996.95(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7556
_cell_measurement_theta_min      3.6730
_cell_measurement_theta_max      69.5280

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             784
_exptl_absorpt_coefficient_mu    1.661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.63618
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1274
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14108
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0150
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         2.72
_diffrn_reflns_theta_max         69.34
_reflns_number_total             3652
_reflns_number_gt                3513
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 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.
 The Leu side chain shows positional disorder. It was refined on two sets
 of positions (atoms C1G, C1D1, C1D2 for the first set, while C1G', C1D3,
 C1D4 for the second set) with refined population parameters of 0.658(8)
 and 0.342(8), respectively. Restraints were applied to the bond distances
 and bond angles involving atoms of the disordered parts, as well to their
 anisotropic displacement parameters. 
;

_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)+(0.0732P)²+0.2664P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_number_reflns         3652
_refine_ls_number_parameters     245
_refine_ls_number_restraints     50
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0391
_refine_ls_wR_factor_ref         0.1091
_refine_ls_wR_factor_gt          0.1077
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.038
_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
C01 C 0.6033(4) 0.5277(2) 0.50212(6) 0.0574(5) Uani 1 1 d . . .
C02 C 0.4281(5) 0.6283(2) 0.50182(7) 0.0667(6) Uani 1 1 d . . .
H02A H 0.5330 0.6933 0.4977 0.100 Uiso 1 1 calc R . .
H02B H 0.3372 0.6336 0.5277 0.100 Uiso 1 1 calc R . .
H02C H 0.3026 0.6219 0.4799 0.100 Uiso 1 1 calc R . .
C03 C 0.4515(6) 0.4203(2) 0.50093(9) 0.0805(8) Uani 1 1 d . . .
H03A H 0.3392 0.4195 0.4772 0.121 Uiso 1 1 calc R . .
H03B H 0.3468 0.4137 0.5254 0.121 Uiso 1 1 calc R . .
H03C H 0.5723 0.3594 0.4994 0.121 Uiso 1 1 calc R . .
C04 C 0.7838(6) 0.5333(4) 0.53927(7) 0.0938(11) Uani 1 1 d . . .
H04A H 0.8952 0.4693 0.5397 0.141 Uiso 1 1 calc R . .
H04B H 0.6803 0.5355 0.5640 0.141 Uiso 1 1 calc R . .
H04C H 0.8900 0.5988 0.5376 0.141 Uiso 1 1 calc R . .
OU O 0.7885(3) 0.53129(15) 0.46700(4) 0.0577(4) Uani 1 1 d . . .
C0 C 0.6965(4) 0.53390(15) 0.42809(5) 0.0416(4) Uani 1 1 d . . .
O0 O 0.4673(3) 0.53685(16) 0.41876(4) 0.0596(4) Uani 1 1 d . . .
N1 N 0.8954(3) 0.53506(13) 0.40126(4) 0.0408(3) Uani 1 1 d . . .
H1 H 1.0538 0.5331 0.4104 0.049 Uiso 1 1 calc R . .
C1A C 0.8522(4) 0.53951(13) 0.35672(5) 0.0387(4) Uani 1 1 d D A .
H1A H 0.6630 0.5433 0.3512 0.046 Uiso 1 1 calc R . .
C1B C 0.9876(4) 0.63851(14) 0.33653(6) 0.0490(5) Uani 1 1 d D . .
H1B1 H 1.0168 0.6217 0.3077 0.059 Uiso 0.658(8) 1 calc PR A 1
H1B2 H 1.1582 0.6486 0.3493 0.059 Uiso 0.658(8) 1 calc PR A 1
H1B3 H 0.9333 0.6408 0.3079 0.059 Uiso 0.342(8) 1 calc PR A 2
H1B4 H 1.1753 0.6246 0.3368 0.059 Uiso 0.342(8) 1 calc PR A 2
C1G C 0.8347(10) 0.7474(3) 0.33954(11) 0.0610(13) Uani 0.658(8) 1 d PDU A 1
H1G H 0.6572 0.7352 0.3288 0.073 Uiso 0.658(8) 1 calc PR A 1
C1D1 C 0.8120(19) 0.7872(3) 0.38350(13) 0.114(3) Uani 0.658(8) 1 d PDU A 1
H1D1 H 0.9784 0.7788 0.3971 0.171 Uiso 0.658(8) 1 calc PR A 1
H1D2 H 0.6814 0.7444 0.3977 0.171 Uiso 0.658(8) 1 calc PR A 1
H1D3 H 0.7619 0.8637 0.3837 0.171 Uiso 0.658(8) 1 calc PR A 1
C1D2 C 0.9685(16) 0.8336(4) 0.31293(16) 0.094(2) Uani 0.658(8) 1 d PDU A 1
H1D4 H 0.9071 0.9058 0.3205 0.142 Uiso 0.658(8) 1 calc PR A 1
H1D5 H 0.9281 0.8199 0.2845 0.142 Uiso 0.658(8) 1 calc PR A 1
H1D6 H 1.1552 0.8296 0.3169 0.142 Uiso 0.658(8) 1 calc PR A 1
C1G' C 0.9410(14) 0.7543(3) 0.3551(3) 0.060(2) Uani 0.342(8) 1 d PDU A 2
H1G' H 1.0013 0.7534 0.3838 0.072 Uiso 0.342(8) 1 calc PR A 2
C1D3 C 0.6510(14) 0.7824(6) 0.3549(5) 0.110(5) Uani 0.342(8) 1 d PDU A 2
H1DA H 0.6296 0.8611 0.3532 0.166 Uiso 0.342(8) 1 calc PR A 2
H1DB H 0.5710 0.7558 0.3798 0.166 Uiso 0.342(8) 1 calc PR A 2
H1DC H 0.5685 0.7481 0.3316 0.166 Uiso 0.342(8) 1 calc PR A 2
C1D4 C 1.096(2) 0.8427(6) 0.3321(5) 0.107(5) Uani 0.342(8) 1 d PDU A 2
H1DD H 1.1305 0.8179 0.3045 0.160 Uiso 0.342(8) 1 calc PR A 2
H1DE H 1.2592 0.8559 0.3460 0.160 Uiso 0.342(8) 1 calc PR A 2
H1DF H 0.9956 0.9098 0.3312 0.160 Uiso 0.342(8) 1 calc PR A 2
C1 C 0.9624(4) 0.43221(14) 0.33851(5) 0.0378(4) Uani 1 1 d . . .
O1 O 1.1986(3) 0.41487(11) 0.33757(5) 0.0524(3) Uani 1 1 d . A .
N2 N 0.7859(3) 0.35853(12) 0.32489(4) 0.0405(3) Uani 1 1 d . A .
H2 H 0.6219 0.3757 0.3241 0.049 Uiso 1 1 calc R . .
C2A C 0.8708(4) 0.24965(15) 0.31139(6) 0.0441(4) Uani 1 1 d . . .
H2A H 1.0312 0.2592 0.2951 0.053 Uiso 1 1 calc R A .
C2B C 0.9372(4) 0.17428(16) 0.34792(7) 0.0549(5) Uani 1 1 d . A .
H2B1 H 1.0565 0.2137 0.3660 0.066 Uiso 1 1 calc R . .
H2B2 H 1.0301 0.1101 0.3375 0.066 Uiso 1 1 calc R . .
S2 S 0.66171(14) 0.12690(4) 0.378106(17) 0.06518(19) Uani 1 1 d . . .
C2D C 0.5960(7) 0.2426(2) 0.41117(8) 0.0825(9) Uani 1 1 d . A .
H2D1 H 0.7582 0.2701 0.4222 0.124 Uiso 1 1 calc R . .
H2D2 H 0.4834 0.2196 0.4333 0.124 Uiso 1 1 calc R . .
H2D3 H 0.5111 0.2999 0.3956 0.124 Uiso 1 1 calc R . .
C2 C 0.6644(4) 0.19929(15) 0.28365(5) 0.0428(4) Uani 1 1 d . A .
O2 O 0.4763(3) 0.24663(13) 0.27068(5) 0.0612(4) Uani 1 1 d . . .
OT O 0.7234(3) 0.09483(11) 0.27508(5) 0.0610(4) Uani 1 1 d . . .
CT C 0.5322(6) 0.0353(2) 0.25075(8) 0.0737(7) Uani 1 1 d . A .
HT1 H 0.3699 0.0304 0.2657 0.111 Uiso 1 1 calc R . .
HT2 H 0.5965 -0.0377 0.2451 0.111 Uiso 1 1 calc R . .
HT3 H 0.5031 0.0737 0.2253 0.111 Uiso 1 1 calc 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
C01 0.0425(11) 0.0819(14) 0.0479(10) 0.0043(10) 0.0098(9) 0.0029(11)
C02 0.0588(14) 0.0758(14) 0.0655(13) -0.0137(11) 0.0079(12) 0.0002(12)
C03 0.0874(19) 0.0702(15) 0.0838(17) 0.0102(12) 0.0346(16) 0.0024(14)
C04 0.0626(16) 0.174(3) 0.0448(11) 0.0146(16) 0.0082(11) 0.021(2)
OU 0.0342(7) 0.0960(11) 0.0427(6) 0.0063(7) 0.0029(6) 0.0051(8)
C0 0.0319(9) 0.0467(9) 0.0462(8) -0.0008(7) -0.0013(7) 0.0020(8)
O0 0.0300(7) 0.0939(11) 0.0549(8) -0.0086(8) -0.0021(6) 0.0014(7)
N1 0.0285(8) 0.0532(8) 0.0406(7) -0.0018(6) -0.0026(6) 0.0011(7)
C1A 0.0360(9) 0.0393(8) 0.0407(8) -0.0028(6) -0.0027(7) 0.0024(7)
C1B 0.0592(13) 0.0385(9) 0.0495(9) 0.0007(7) 0.0049(9) 0.0014(8)
C1G 0.074(4) 0.0428(16) 0.067(2) -0.0012(15) -0.011(2) 0.007(2)
C1D1 0.214(9) 0.048(2) 0.081(3) -0.0125(19) 0.026(4) 0.019(3)
C1D2 0.148(6) 0.049(2) 0.086(3) 0.018(2) -0.001(3) 0.011(3)
C1G' 0.055(5) 0.038(3) 0.088(7) 0.007(4) 0.000(4) 0.015(3)
C1D3 0.074(6) 0.054(4) 0.203(15) 0.000(6) 0.039(8) 0.013(4)
C1D4 0.094(8) 0.052(4) 0.174(13) 0.034(7) 0.015(8) 0.001(5)
C1 0.0341(10) 0.0389(8) 0.0404(8) -0.0018(6) 0.0015(7) 0.0008(6)
O1 0.0325(7) 0.0504(7) 0.0744(9) -0.0162(6) -0.0003(6) 0.0021(6)
N2 0.0320(8) 0.0372(7) 0.0522(8) -0.0034(6) -0.0014(6) 0.0031(6)
C2A 0.0357(10) 0.0394(8) 0.0573(10) -0.0056(7) 0.0015(8) 0.0012(8)
C2B 0.0492(12) 0.0430(9) 0.0726(13) -0.0052(9) -0.0169(10) 0.0110(9)
S2 0.0859(4) 0.0464(3) 0.0633(3) 0.0066(2) -0.0050(3) -0.0020(3)
C2D 0.122(3) 0.0608(13) 0.0648(14) 0.0026(11) 0.0083(16) 0.0141(17)
C2 0.0406(10) 0.0418(8) 0.0460(9) -0.0043(7) 0.0052(8) -0.0009(8)
O2 0.0533(9) 0.0598(8) 0.0704(9) -0.0157(7) -0.0134(7) 0.0081(7)
OT 0.0692(10) 0.0419(7) 0.0720(9) -0.0153(6) -0.0109(8) 0.0028(7)
CT 0.0893(18) 0.0568(12) 0.0750(14) -0.0210(11) -0.0080(14) -0.0135(14)

_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
C01 OU 1.479(2) . ?
C01 C03 1.513(4) . ?
C01 C02 1.508(3) . ?
C01 C04 1.517(3) . ?
OU C0 1.346(2) . ?
C0 O0 1.206(2) . ?
C0 N1 1.335(2) . ?
N1 C1A 1.462(2) . ?
C1A C1B 1.529(2) . ?
C1A C1 1.533(2) . ?
C1B C1G 1.533(3) . ?
C1B C1G' 1.544(4) . ?
C1G C1D2 1.515(4) . ?
C1G C1D1 1.509(4) . ?
C1G' C1D3 1.514(5) . ?
C1G' C1D4 1.525(5) . ?
C1 O1 1.220(2) . ?
C1 N2 1.341(2) . ?
N2 C2A 1.454(2) . ?
C2A C2 1.511(3) . ?
C2A C2B 1.533(3) . ?
C2B S2 1.804(3) . ?
S2 C2D 1.795(3) . ?
C2 O2 1.192(2) . ?
C2 OT 1.328(2) . ?
OT CT 1.445(3) . ?

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
OU C01 C03 109.30(19) . . ?
OU C01 C02 110.39(18) . . ?
C03 C01 C02 113.02(19) . . ?
OU C01 C04 102.99(17) . . ?
C03 C01 C04 111.6(2) . . ?
C02 C01 C04 109.1(2) . . ?
C0 OU C01 120.07(15) . . ?
O0 C0 N1 124.72(17) . . ?
O0 C0 OU 124.91(17) . . ?
N1 C0 OU 110.36(15) . . ?
C0 N1 C1A 122.04(15) . . ?
N1 C1A C1B 112.59(14) . . ?
N1 C1A C1 107.14(13) . . ?
C1B C1A C1 109.46(14) . . ?
C1A C1B C1G 114.6(2) . . ?
C1A C1B C1G' 118.3(3) . . ?
C1D2 C1G C1D1 110.7(4) . . ?
C1D2 C1G C1B 109.1(3) . . ?
C1D1 C1G C1B 111.9(3) . . ?
C1D3 C1G' C1D4 110.1(6) . . ?
C1D3 C1G' C1B 110.6(5) . . ?
C1D4 C1G' C1B 111.4(5) . . ?
O1 C1 N2 122.53(16) . . ?
O1 C1 C1A 121.05(16) . . ?
N2 C1 C1A 116.40(15) . . ?
C1 N2 C2A 120.15(15) . . ?
N2 C2A C2 109.74(15) . . ?
N2 C2A C2B 111.81(15) . . ?
C2 C2A C2B 111.96(15) . . ?
C2A C2B S2 115.94(15) . . ?
C2D S2 C2B 102.81(13) . . ?
O2 C2 OT 124.37(18) . . ?
O2 C2 C2A 125.08(17) . . ?
OT C2 C2A 110.54(16) . . ?
C2 OT CT 115.85(19) . . ?

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
C03 C01 OU C0 64.9(3) . . . . ?
C02 C01 OU C0 -60.0(3) . . . . ?
C04 C01 OU C0 -176.4(2) . . . . ?
C01 OU C0 O0 2.3(3) . . . . ?
C01 OU C0 N1 -179.00(18) . . . . y
O0 C0 N1 C1A -0.4(3) . . . . ?
OU C0 N1 C1A -179.10(15) . . . . y
C0 N1 C1A C1B 122.93(19) . . . . ?
C0 N1 C1A C1 -116.68(18) . . . . y
N1 C1A C1B C1G -82.1(3) . . . . y
C1 C1A C1B C1G 158.8(2) . . . . ?
N1 C1A C1B C1G' -51.0(4) . . . . y
C1 C1A C1B C1G' -170.0(4) . . . . ?
C1A C1B C1G C1D2 -171.3(3) . . . . y
C1A C1B C1G C1D1 65.9(5) . . . . y
C1A C1B C1G' C1D3 -58.7(9) . . . . y
C1A C1B C1G' C1D4 178.5(6) . . . . y
N1 C1A C1 O1 -69.9(2) . . . . ?
C1B C1A C1 O1 52.5(2) . . . . ?
N1 C1A C1 N2 108.45(17) . . . . y
C1B C1A C1 N2 -129.19(17) . . . . ?
O1 C1 N2 C2A 5.1(3) . . . . ?
C1A C1 N2 C2A -173.14(15) . . . . y
C1 N2 C2A C2 -159.11(15) . . . . y
C1 N2 C2A C2B 76.0(2) . . . . ?
N2 C2A C2B S2 71.18(19) . . . . y
C2 C2A C2B S2 -52.4(2) . . . . ?
C2A C2B S2 C2D -80.84(18) . . . . y
N2 C2A C2 O2 8.6(3) . . . . ?
C2B C2A C2 O2 133.3(2) . . . . ?
N2 C2A C2 OT -172.42(16) . . . . y
C2B C2A C2 OT -47.7(2) . . . . ?
O2 C2 OT CT -4.6(3) . . . . ?
C2A C2 OT CT 176.39(19) . . . . y

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O0 0.86 2.12 2.965(2) 166.7 1_655
N2 H2 O1 0.86 2.25 3.093(2) 167.1 1_455

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        69.34
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.037

#===END===

# start Validation Reply Form
_vrf_PLAT242_mc238f              
;
PROBLEM: Low Ueq as Compared to Neighbors for ..... C01 Check
RESPONSE: C01 is the quaternary carbon atom of a t-butyl group,
the low Ueq of which as compared to the methyl neighbors is a 
common observation. 
;
# end Validation Reply Form
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol'
