# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_DFClNKFCl
_database_code_depnum_ccdc_archive 'CCDC 1574297'
_audit_update_record             
;
2017-09-13 deposited with the CCDC.
2018-08-13 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H41 Cl2 N7 O9, 7 H2 O'
_chemical_formula_sum            'C32 H55 Cl2 N7 O16'
_chemical_formula_weight         864.73

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0043 0.0021 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0082 0.0043 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0142 0.0079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1778 0.2018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 2'
_space_group_name_Hall           'C 2y'

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

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

_cell_length_a                   26.685(5)
_cell_length_b                   4.809(1)
_cell_length_c                   36.125(7)
_cell_angle_alpha                90
_cell_angle_beta                 107.56(3)
_cell_angle_gamma                90
_cell_volume                     4419.8(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    523
_cell_measurement_theta_min      1.722
_cell_measurement_theta_max      19.299

_exptl_crystal_description       'Thin needles'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_F_000             1832
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.296
_shelx_estimated_absorpt_T_min   0.974
_shelx_estimated_absorpt_T_max   0.997

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3578
_exptl_absorpt_correction_T_max  0.7444
_exptl_absorpt_process_details   'SADABS v2012/1 (Bruker, 2012)'
_exptl_special_details           
;
SADABS was used to perform the Absorption correction.
Parameters refinement is based on 6362 reflections.
Ratio of minimum to maximum apparent transmission: 0.4807
The given Tmin and Tmax were generated using the SHELX SIZE command
;


_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.800

_diffrn_measurement_method       'Rotating crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'Elettra Synchrotron - XRD1 BL'
_diffrn_measurement_device_type  
;
'Huber 4-circles Kappa Goniometer, Pilatus 2M detector'
;

_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6299
_diffrn_reflns_av_unetI/netI     0.1474
_diffrn_reflns_av_R_equivalents  0.1060
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.722
_diffrn_reflns_theta_max         19.299
_diffrn_reflns_theta_full        19.299
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measured_fraction_theta_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_point_group_measured_fraction_full 0.934
_reflns_number_total             2411
_reflns_number_gt                1373
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.636
_reflns_Friedel_fraction_max     0.897
_reflns_Friedel_fraction_full    0.897

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

_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0

_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015)'
_computing_molecular_graphics    'Ortep3 for Windows - Coot'
_computing_publication_material  'enCIFer - publCIF'

_refine_special_details          
;
Hydrogen atoms were included at calculated positions with isotropic 
Ufactors=1.2Ueq (Ufactors=1.5Ueq for protonated amino groups). Anisotropic 
thermal motion modeling has been applied only to halogen and backbone oxygen
atoms to avoid overrefinement. Geometric restrains (DFIX, DANG) have 
been used for all residues. Additional thermal restrains (SIMU and ISOR) 
have been used for poorly defined/disordered fragments.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0098P)²+148.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 347 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.27(17)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         2411
_refine_ls_number_parameters     263
_refine_ls_number_restraints     195
_refine_ls_R_factor_all          0.2381
_refine_ls_R_factor_gt           0.1420
_refine_ls_wR_factor_ref         0.3499
_refine_ls_wR_factor_gt          0.2954
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_restrained_S_all      1.151
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N_11 N 0.7917(10) 0.641(5) 0.5567(6) 0.090(11) Uiso 1 1 d D . . . .
H0A_11 H 0.826955 0.619480 0.567476 0.135 Uiso 1 1 calc R U . . .
H0B_11 H 0.776007 0.470983 0.552382 0.135 Uiso 1 1 calc R U . . .
H0C_11 H 0.785208 0.733549 0.533734 0.135 Uiso 1 1 calc R U . . .
CA_11 C 0.7706(7) 0.800(3) 0.5830(5) 0.082(13) Uiso 1 1 d D . . . .
HA_11 H 0.787868 0.986248 0.587092 0.099 Uiso 1 1 calc R U . . .
C_11 C 0.7827(8) 0.653(4) 0.6224(4) 0.074(13) Uiso 1 1 d D . . . .
O_11 O 0.7833(10) 0.397(4) 0.6239(5) 0.092(9) Uani 1 1 d D U . . .
CB_11 C 0.7117(8) 0.842(6) 0.5663(7) 0.104(15) Uiso 1 1 d D . . . .
HB1_11 H 0.694772 0.657626 0.559420 0.125 Uiso 1 1 calc R U . . .
HB2_11 H 0.698349 0.923444 0.586633 0.125 Uiso 1 1 calc R U . . .
CG_11 C 0.6954(8) 1.027(5) 0.5307(6) 0.111(16) Uiso 1 1 d D . . . .
OD1_11 O 0.7291(9) 1.174(5) 0.5229(6) 0.087(8) Uiso 1 1 d D . . . .
OD2_11 O 0.6479(8) 1.025(6) 0.5112(6) 0.146(13) Uiso 1 1 d D . . . .
ClZ_12 Cl 0.9138(6) 0.428(3) 0.8845(2) 0.157(7) Uani 1 1 d D . . . .
N_12 N 0.7877(8) 0.821(5) 0.6518(3) 0.070(8) Uani 1 1 d D U . . .
H0_12 H 0.787213 1.000526 0.647122 0.085 Uiso 1 1 calc R U . . .
CA_12 C 0.7942(6) 0.735(2) 0.6921(4) 0.066(8) Uiso 1 1 d D U . . .
HA_12 H 0.789890 0.528349 0.692586 0.080 Uiso 1 1 calc R U . . .
C_12 C 0.7515(6) 0.871(4) 0.7062(5) 0.060(11) Uiso 1 1 d D . . . .
O_12 O 0.7492(8) 1.127(4) 0.7074(5) 0.061(7) Uani 1 1 d D U . . .
CB_12 C 0.8481(6) 0.809(4) 0.7179(3) 0.067(12) Uiso 1 1 d D . . . .
HB1_12 H 0.851275 1.013816 0.718322 0.081 Uiso 1 1 calc R U . . .
HB2_12 H 0.874057 0.734919 0.705787 0.081 Uiso 1 1 calc R U . . .
CG_12 C 0.8636(5) 0.707(3) 0.7597(3) 0.075(12) Uiso 1 1 d DG . . . .
CD1_12 C 0.8380(6) 0.486(4) 0.7710(3) 0.069(11) Uiso 1 1 d DG . . . .
HD1_12 H 0.809967 0.394188 0.752318 0.083 Uiso 1 1 calc R U . . .
CE1_12 C 0.8533(6) 0.399(3) 0.8094(3) 0.086(13) Uiso 1 1 d DG . . . .
HE1_12 H 0.835741 0.247717 0.817107 0.104 Uiso 1 1 calc R U . . .
CZ_12 C 0.8942(5) 0.533(3) 0.8367(3) 0.071(12) Uiso 1 1 d DG . . . .
CE2_12 C 0.9199(6) 0.755(3) 0.8255(3) 0.094(14) Uiso 1 1 d DG . . . .
HE2_12 H 0.947842 0.846346 0.844141 0.113 Uiso 1 1 calc R U . . .
CD2_12 C 0.9045(6) 0.842(4) 0.7870(4) 0.085(13) Uiso 1 1 d DG . . . .
HD2_12 H 0.922069 0.992820 0.779353 0.102 Uiso 1 1 calc R U . . .
N_13 N 0.7186(7) 0.702(5) 0.7149(5) 0.070(8) Uani 1 1 d D U . . .
H0_13 H 0.719178 0.524944 0.708830 0.084 Uiso 1 1 calc R U . . .
CA_13 C 0.6811(7) 0.794(3) 0.7343(4) 0.070(9) Uiso 1 1 d D U . . .
HA_13 H 0.683765 1.000594 0.737152 0.083 Uiso 1 1 calc R U . . .
C_13 C 0.6943(8) 0.664(4) 0.7748(4) 0.057(11) Uiso 1 1 d D . . . .
O_13 O 0.6959(10) 0.408(4) 0.7780(5) 0.075(8) Uani 1 1 d D U . . .
CB_13 C 0.6250(6) 0.720(5) 0.7107(5) 0.074(12) Uiso 1 1 d D . . . .
HB1_13 H 0.621983 0.515813 0.707517 0.089 Uiso 1 1 calc R U . . .
HB2_13 H 0.600710 0.780014 0.725171 0.089 Uiso 1 1 calc R U . . .
CG_13 C 0.6088(9) 0.857(5) 0.6709(5) 0.14(2) Uiso 1 1 d D . . . .
OD1_13 O 0.6015(11) 1.109(5) 0.6677(6) 0.126(11) Uiso 1 1 d D . . . .
ND2_13 N 0.6037(13) 0.690(6) 0.6408(6) 0.130(14) Uiso 1 1 d D . . . .
HD2A_13 H 0.594766 0.758630 0.617141 0.156 Uiso 1 1 calc R U . . .
HD2B_13 H 0.609345 0.510186 0.644494 0.156 Uiso 1 1 calc R U . . .
N_14 N 0.7082(8) 0.841(4) 0.8037(4) 0.066(8) Uani 1 1 d D U . . .
H0_14 H 0.708534 1.019969 0.798378 0.079 Uiso 1 1 calc R U . . .
CA_14 C 0.7233(7) 0.754(3) 0.8444(5) 0.066(8) Uiso 1 1 d D U . . .
HA_14 H 0.724378 0.546344 0.845244 0.080 Uiso 1 1 calc R U . . .
C_14 C 0.6830(7) 0.853(5) 0.8636(5) 0.082(14) Uiso 1 1 d D . . . .
O_14 O 0.6719(10) 1.102(5) 0.8639(7) 0.108(10) Uani 1 1 d D U . . .
CB_14 C 0.7778(6) 0.863(6) 0.8663(5) 0.079(12) Uiso 1 1 d D . . . .
HB1_14 H 0.776387 1.068856 0.866999 0.095 Uiso 1 1 calc R U . . .
HB2_14 H 0.802451 0.811361 0.851731 0.095 Uiso 1 1 calc R U . . .
CG_14 C 0.7995(10) 0.755(8) 0.9078(6) 0.101(15) Uiso 1 1 d D . . . .
HG1_14 H 0.774224 0.796702 0.922260 0.121 Uiso 1 1 calc R U . . .
HG2_14 H 0.803877 0.551051 0.907357 0.121 Uiso 1 1 calc R U . . .
CD_14 C 0.8521(12) 0.890(9) 0.9282(7) 0.15(2) Uiso 1 1 d D . . . .
HD1_14 H 0.872700 0.908709 0.909663 0.185 Uiso 1 1 calc R U . . .
HD2_14 H 0.846061 1.079228 0.936846 0.185 Uiso 1 1 calc R U . . .
CE_14 C 0.8835(10) 0.722(12) 0.9630(9) 0.22(3) Uiso 1 1 d D . . . .
HE1_14 H 0.891313 0.537049 0.954135 0.268 Uiso 1 1 calc R U . . .
HE2_14 H 0.917326 0.817005 0.975366 0.268 Uiso 1 1 calc R U . . .
NZ_14 N 0.855(2) 0.686(11) 0.9922(10) 0.22(2) Uiso 1 1 d D . . . .
HZ1_14 H 0.875211 0.584034 1.012492 0.323 Uiso 1 1 calc R U . . .
HZ2_14 H 0.848387 0.855176 1.000816 0.323 Uiso 1 1 calc R U . . .
HZ3_14 H 0.824234 0.595230 0.981103 0.323 Uiso 1 1 calc R U . . .
ClZ_15 Cl 0.4820(7) 0.705(4) 0.6995(4) 0.188(8) Uani 1 1 d D . . . .
N_15 N 0.6603(8) 0.660(6) 0.8785(7) 0.104(10) Uani 1 1 d D U . . .
H0_15 H 0.672236 0.488358 0.879919 0.124 Uiso 1 1 calc R U . . .
CA_15 C 0.6160(8) 0.721(3) 0.8926(4) 0.108(11) Uiso 1 1 d D U . . .
HA_15 H 0.606034 0.920765 0.886832 0.129 Uiso 1 1 calc R U . . .
C_15 C 0.6308(10) 0.678(6) 0.9368(4) 0.18(3) Uiso 1 1 d D . . . .
O_15 O 0.6001(15) 0.755(9) 0.9543(7) 0.204(18) Uiso 1 1 d D . . . .
CB_15 C 0.5689(8) 0.542(6) 0.8725(4) 0.127(18) Uiso 1 1 d D . . . .
HB1_15 H 0.540528 0.580521 0.884232 0.152 Uiso 1 1 calc R U . . .
HB2_15 H 0.578984 0.343973 0.877685 0.152 Uiso 1 1 calc R U . . .
CG_15 C 0.5470(6) 0.582(4) 0.8287(4) 0.119(18) Uiso 1 1 d DG . . . .
CD1_15 C 0.5633(8) 0.410(5) 0.8037(4) 0.131(18) Uiso 1 1 d DG . . . .
HD1_15 H 0.588229 0.267235 0.813800 0.158 Uiso 1 1 calc R U . . .
CE1_15 C 0.5433(8) 0.448(4) 0.7637(4) 0.15(2) Uiso 1 1 d DG . . . .
HE1_15 H 0.554476 0.330499 0.746612 0.182 Uiso 1 1 calc R U . . .
CZ_15 C 0.5069(6) 0.657(3) 0.7489(4) 0.135(19) Uiso 1 1 d DG . . . .
CE2_15 C 0.4905(8) 0.829(4) 0.7739(4) 0.133(19) Uiso 1 1 d DG . . . .
HE2_15 H 0.465649 0.972585 0.763799 0.160 Uiso 1 1 calc R U . . .
CD2_15 C 0.5106(9) 0.792(5) 0.8139(4) 0.16(2) Uiso 1 1 d DG . . . .
HD2_15 H 0.499401 0.909326 0.830987 0.196 Uiso 1 1 calc R U . . .
OXT_15 O 0.6724(18) 0.556(9) 0.9539(12) 0.200(18) Uiso 1 1 d . . . . .
O_21 O 1.0146(19) 0.934(13) 0.5504(13) 0.25(2) Uiso 1 1 d . . . . .
OA_22 O 0.898(3) 0.700(15) 0.6089(17) 0.19(3) Uiso 0.65 1 d . . P A 1
OB_22 O 0.895(4) 0.32(3) 0.591(3) 0.17(4) Uiso 0.35 1 d . . P B 2
OA_23 O 1.002(3) 0.04(2) 0.962(2) 0.28(4) Uiso 0.65 1 d . . P C 1
OB_23 O 1.024(6) 0.50(3) 0.962(4) 0.24(6) Uiso 0.35 1 d . . P D 2
O_24 O 0.8979(18) 0.011(10) 0.5227(12) 0.215(19) Uiso 1 1 d . . . . .
O_25 O 1.0706(14) 0.406(8) 0.5561(9) 0.151(13) Uiso 1 1 d . . . . .
O_26 O 0.992(2) 0.675(11) 0.6197(13) 0.23(2) Uiso 1 1 d . . . . .
O_27 O 0.740(2) 0.812(13) 1.0309(14) 0.27(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
N_11 CA_11 1.457(9) . ?
CA_11 CB_11 1.517(9) . ?
CA_11 C_11 1.535(9) . ?
C_11 O_11 1.231(10) . ?
C_11 N_12 1.310(18) . ?
CB_11 CG_11 1.514(9) . ?
CG_11 OD1_11 1.242(10) . ?
CG_11 OD2_11 1.252(9) . ?
ClZ_12 CZ_12 1.721(6) . ?
N_12 CA_12 1.471(9) . ?
CA_12 CB_12 1.501(8) . ?
CA_12 C_12 1.529(9) . ?
C_12 O_12 1.234(10) . ?
C_12 N_13 1.304(19) . ?
CB_12 CG_12 1.522(7) . ?
CG_12 CD1_12 1.3900 . ?
CG_12 CD2_12 1.3900 . ?
CD1_12 CE1_12 1.3900 . ?
CE1_12 CZ_12 1.3900 . ?
CZ_12 CE2_12 1.3900 . ?
CE2_12 CD2_12 1.3900 . ?
N_13 CA_13 1.452(9) . ?
CA_13 CB_13 1.524(9) . ?
CA_13 C_13 1.532(9) . ?
C_13 O_13 1.237(10) . ?
C_13 N_14 1.311(18) . ?
CB_13 CG_13 1.521(9) . ?
CG_13 OD1_13 1.228(10) . ?
CG_13 ND2_13 1.325(10) . ?
N_14 CA_14 1.464(9) . ?
CA_14 CB_14 1.523(9) . ?
CA_14 C_14 1.523(9) . ?
C_14 O_14 1.231(10) . ?
C_14 N_15 1.31(2) . ?
CB_14 CG_14 1.526(11) . ?
CG_14 CD_14 1.521(11) . ?
CD_14 CE_14 1.517(11) . ?
CE_14 NZ_14 1.481(11) . ?
ClZ_15 CZ_15 1.720(7) . ?
N_15 CA_15 1.453(9) . ?
CA_15 CB_15 1.519(9) . ?
CA_15 C_15 1.536(9) . ?
C_15 O_15 1.235(11) . ?
C_15 OXT_15 1.24(5) . ?
CB_15 CG_15 1.525(7) . ?
CG_15 CD1_15 1.3900 . ?
CG_15 CD2_15 1.3900 . ?
CD1_15 CE1_15 1.3900 . ?
CE1_15 CZ_15 1.3900 . ?
CZ_15 CE2_15 1.3900 . ?
CE2_15 CD2_15 1.3900 . ?

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
N_11 CA_11 CB_11 111.6(7) . . ?
N_11 CA_11 C_11 110.5(7) . . ?
CB_11 CA_11 C_11 109.4(7) . . ?
O_11 C_11 N_12 125.9(16) . . ?
O_11 C_11 CA_11 119.7(11) . . ?
N_12 C_11 CA_11 114.2(15) . . ?
CG_11 CB_11 CA_11 114.4(8) . . ?
OD1_11 CG_11 OD2_11 123.7(10) . . ?
OD1_11 CG_11 CB_11 119.1(9) . . ?
OD2_11 CG_11 CB_11 117.2(10) . . ?
C_11 N_12 CA_12 125.5(16) . . ?
N_12 CA_12 CB_12 110.6(7) . . ?
N_12 CA_12 C_12 109.4(7) . . ?
CB_12 CA_12 C_12 111.2(7) . . ?
O_12 C_12 N_13 124.7(16) . . ?
O_12 C_12 CA_12 119.4(11) . . ?
N_13 C_12 CA_12 115.9(15) . . ?
CA_12 CB_12 CG_12 117.6(7) . . ?
CD1_12 CG_12 CD2_12 120.0 . . ?
CD1_12 CG_12 CB_12 121.6(6) . . ?
CD2_12 CG_12 CB_12 118.4(6) . . ?
CE1_12 CD1_12 CG_12 120.00(6) . . ?
CD1_12 CE1_12 CZ_12 120.00(6) . . ?
CE1_12 CZ_12 CE2_12 120.0 . . ?
CE1_12 CZ_12 ClZ_12 120.7(6) . . ?
CE2_12 CZ_12 ClZ_12 119.3(6) . . ?
CD2_12 CE2_12 CZ_12 120.00(6) . . ?
CE2_12 CD2_12 CG_12 120.00(6) . . ?
C_12 N_13 CA_13 122.6(18) . . ?
N_13 CA_13 CB_13 111.4(7) . . ?
N_13 CA_13 C_13 110.1(7) . . ?
CB_13 CA_13 C_13 110.0(7) . . ?
O_13 C_13 N_14 125.4(16) . . ?
O_13 C_13 CA_13 119.1(11) . . ?
N_14 C_13 CA_13 115.1(15) . . ?
CG_13 CB_13 CA_13 112.3(9) . . ?
OD1_13 CG_13 ND2_13 123.2(11) . . ?
OD1_13 CG_13 CB_13 120.4(10) . . ?
ND2_13 CG_13 CB_13 116.4(10) . . ?
C_13 N_14 CA_14 122.6(16) . . ?
N_14 CA_14 CB_14 110.7(7) . . ?
N_14 CA_14 C_14 110.5(7) . . ?
CB_14 CA_14 C_14 110.5(7) . . ?
O_14 C_14 N_15 122.9(18) . . ?
O_14 C_14 CA_14 120.8(12) . . ?
N_15 C_14 CA_14 116.2(17) . . ?
CA_14 CB_14 CG_14 114.4(10) . . ?
CD_14 CG_14 CB_14 110.6(11) . . ?
CE_14 CD_14 CG_14 111.9(12) . . ?
NZ_14 CE_14 CD_14 112.4(12) . . ?
C_14 N_15 CA_15 122(2) . . ?
N_15 CA_15 CB_15 111.1(7) . . ?
N_15 CA_15 C_15 110.9(7) . . ?
CB_15 CA_15 C_15 109.6(7) . . ?
O_15 C_15 OXT_15 121(3) . . ?
O_15 C_15 CA_15 119.4(13) . . ?
OXT_15 C_15 CA_15 119(2) . . ?
CA_15 CB_15 CG_15 115.2(7) . . ?
CD1_15 CG_15 CD2_15 120.0 . . ?
CD1_15 CG_15 CB_15 120.1(6) . . ?
CD2_15 CG_15 CB_15 119.9(6) . . ?
CE1_15 CD1_15 CG_15 120.0 . . ?
CD1_15 CE1_15 CZ_15 120.0 . . ?
CE2_15 CZ_15 CE1_15 120.0 . . ?
CE2_15 CZ_15 ClZ_15 119.9(6) . . ?
CE1_15 CZ_15 ClZ_15 120.1(6) . . ?
CZ_15 CE2_15 CD2_15 120.0 . . ?
CE2_15 CD2_15 CG_15 120.0 . . ?


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
_geom_hbond_publ_flag
N_11 H0A_11 OA_22^a 0.91 2.06 2.90(7) 153.1 . yes
N_11 H0A_11 OB_22^b 0.91 2.29 3.10(12) 146.8 . yes
N_11 H0B_11 OD1_11 0.91 1.98 2.84(4) 157.1 1_545 yes
N_11 H0C_11 OD1_11 0.91 2.56 3.10(3) 119.0 . yes
N_11 H0C_11 OD1_11 0.91 1.99 2.76(3) 142.4 4_444 yes
CA_11 HA_11 O_11 1.00 2.40 3.20(2) 136.2 1_565 yes
N_12 H0_12 O_11 0.88 2.07 2.94(3) 167.7 1_565 yes
CA_12 HA_12 O_12 1.00 2.35 3.27(2) 151.9 1_545 yes
N_13 H0_13 O_12 0.88 2.08 2.92(3) 158.6 1_545 yes
CA_13 HA_13 O_13 1.00 2.42 3.32(2) 149.6 1_565 yes
CB_13 HB1_13 OD1_13 0.99 2.39 3.30(3) 151.5 1_545 yes
ND2_13 HD2A_13 O_25 0.88 2.22 3.10(4) 176.5 3_455 yes
ND2_13 HD2B_13 OD1_13 0.88 2.14 2.96(2) 155.8 1_545 yes
N_14 H0_14 O_13 0.88 2.00 2.87(3) 168.5 1_565 yes
CD_14 HD1_14 ClZ_12 0.99 2.82 3.42(5) 119.6 . yes
CE_14 HE1_14 ClZ_12 0.99 2.81 3.48(4) 125.6 . yes
NZ_14 HZ1_14 O_15 0.91 1.97 2.84(5) 158.1 4_445 yes
NZ_14 HZ1_14 OB_23^b 0.91 2.59 3.27(15) 132.0 2 yes
NZ_14 HZ2_14 O_15 0.91 2.62 3.36(7) 138.5 4_455 yes
NZ_14 HZ2_14 OXT_15 0.91 2.11 2.89(6) 143.1 4_455 yes
NZ_14 HZ3_14 O_27 0.91 2.12 3.01(7) 164.0 4_445 yes
N_15 H0_15 O_14 0.88 1.95 2.77(3) 155.4 1_545 yes

_refine_diff_density_max         0.519
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.099


# start Validation Reply Form

_vrf_PLAT023_DFClNKFCl           
; 
PROBLEM:  Resolution (too) Low [sin(theta)/Lambda < 0.6].. 19.30 Degree
RESPONSE: Crystals diffracted poorly (best ones show reflections at a
          maximum resolution of 1.2 Ang). Radiation damage have been found 
          and limited the maximum dose allowed per data collection.
;
_vrf_THETM01_DFClNKFCl           
; 
PROBLEM:  The value of sine(theta_max)/wavelength is less than 0.4131
RESPONSE: Crystals diffracted poorly (best ones show reflections at a
          maximum resolution of 1.2 Ang). Radiation damage have been found 
          and limited the maximum dose allowed per data collection.
;
_vrf_PLAT340_DFClNKFCl           
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02441 Ang.
RESPONSE: Crystals diffracted poorly (best ones show reflections at a
          maximum resolution of 1.2 Ang) and were prone to radiation damage.
;
_vrf_PLAT201_DFClNKFCl           
; 
PROBLEM:  Isotropic non-H Atoms in Main Residue(s) .......        40
RESPONSE: Crystals diffracted poorly (best ones show reflections at a
          maximum resolution of 1.2 Ang), so few data were available for 
          refinement. Number of model parameters have been kept low to avoid 
          overrefinement. Anisotropic thermal motion modeling have been 
          applied only to halogen and backbone oxygen atoms.
;
_vrf_PLAT430_DFClNKFCl           
;
PROBLEM:  Short Inter D...A Contact
RESPONSE: Water molecules have been located in crystal voids. Most of them are 
          involved in hydrogen bonds with peptide hetero atoms. Crystals 
          diffracted poorly (best ones show reflections at a maximum resolution 
          of 1.2 Ang), therefore hydrogen atoms bound to water molecules could 
          not be unambiguously located and have not been modeled.
;
_vrf_PLAT306_DFClNKFCl           
;
PROBLEM:  Isolated Oxygen Atom (H-atoms Missing ?)
RESPONSE: Water molecules have been located in crystal voids. Most of them are 
          involved in hydrogen bonds with peptide hetero atoms. Crystals 
          diffracted poorly (best ones show reflections at a maximum resolution 
          of 1.2 Ang), therefore hydrogen atoms bound to water molecules could 
          not be unambiguously located and have not been modeled.
;
_vrf_PLAT043_DFClNKFCl           
;
PROBLEM:  Calculated and Reported Mol. Weight Differ by ..      14.11 Check
RESPONSE: Water molecules have been found in crystal voids but their hydrogen 
          atoms could not be unambiguously located and therefore have not been 
          modeled. Contributions of these H atoms have been included in the 
          reported crystal properties.          
;

# end Validation Reply Form


####################################################################### 
# 
# 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_DFINKFI
_database_code_depnum_ccdc_archive 'CCDC 1574298'
_audit_update_record             
;
2017-09-13 deposited with the CCDC.
2018-08-13 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H41 I2 N7 O9, 11.5 (H2 O)'
_chemical_formula_sum            'C32 H64 I2 N7 O20.50'
_chemical_formula_weight         1128.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0059 0.0032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0105 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4630 1.7726 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 2'
_space_group_name_Hall           'C 2y'

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

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

_cell_length_a                   28.206(6)
_cell_length_b                   4.803(1)
_cell_length_c                   35.888(7)
_cell_angle_alpha                90
_cell_angle_beta                 97.44(3)
_cell_angle_gamma                90
_cell_volume                     4820.9(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1440
_cell_measurement_theta_min      1.127
_cell_measurement_theta_max      29.987

_exptl_crystal_description       'Thin plates'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_F_000             2300
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    1.311
_shelx_estimated_absorpt_T_min   0.779
_shelx_estimated_absorpt_T_max   0.962

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6473
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_process_details   'SADABS v2012/1 (Bruker, 2012)'
_exptl_special_details           
;
SADABS was used to perform the Absorption correction.
Parameters refinement is based on 44699 reflections.
Ratio of minimum to maximum apparent transmission: 0.8672
The given Tmin and Tmax were generated using the SHELX SIZE command
;


_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.700

_diffrn_measurement_method       'Rotating crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'Elettra Synchrotron - XRD1 BL'
_diffrn_measurement_device_type  
;
'Huber 4-circles Kappa Goniometer, Pilatus 2M detector'
;

_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            44557
_diffrn_reflns_av_unetI/netI     0.0872
_diffrn_reflns_av_R_equivalents  0.0909
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_theta_min         1.127
_diffrn_reflns_theta_max         29.987
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_point_group_measured_fraction_full 0.962
_reflns_number_total             13701
_reflns_number_gt                10227
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.706
_reflns_Friedel_fraction_max     0.866
_reflns_Friedel_fraction_full    0.924

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


_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0

_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015)'
_computing_molecular_graphics    'Ortep3 for Windows - Coot'
_computing_publication_material  'enCIFer - publCIF'

_refine_special_details          
;
Hydrogen atoms were included at calculated positions with isotropic 
Ufactors=1.2Ueq (Ufactors=1.5Ueq for protonated amino groups). Anisotropic 
thermal motion modeling has been applied to all atoms with occupancy greater
than 50%. Minor thermal restrains (SIMU) have been used for peptide linkage 
between residues 12 and 13 to prevent oxygen atom to become NPD.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0808P)²+29.6631P] 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 x determined using 3208 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.009(13)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         13701
_refine_ls_number_parameters     561
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0714
_refine_ls_wR_factor_ref         0.1904
_refine_ls_wR_factor_gt          0.1751
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
IZ_11 I 0.91208(3) 0.47150(18) 0.87622(2) 0.0472(2) Uani 1 1 d . . . . .
N_11 N 0.7922(3) 0.7201(13) 0.55005(17) 0.0221(13) Uani 1 1 d . . . . .
H0A_11 H 0.783461 0.807695 0.527726 0.033 Uiso 1 1 calc R U . . .
H0B_11 H 0.777767 0.550358 0.549702 0.033 Uiso 1 1 calc R U . . .
H0C_11 H 0.824470 0.697790 0.553736 0.033 Uiso 1 1 calc R U . . .
CA_11 C 0.7771(3) 0.8910(14) 0.5811(2) 0.0202(14) Uani 1 1 d . . . . .
HA_11 H 0.794036 1.074277 0.582504 0.024 Uiso 1 1 calc R U . . .
C_11 C 0.7899(3) 0.7311(13) 0.61808(19) 0.0177(13) Uani 1 1 d . . . . .
O_11 O 0.7887(2) 0.4754(13) 0.61862(14) 0.0296(13) Uani 1 1 d . . . . .
CB_11 C 0.7227(3) 0.9378(18) 0.5754(2) 0.0271(16) Uani 1 1 d . . . . .
HB1_11 H 0.706477 0.755222 0.571657 0.033 Uiso 1 1 calc R U . . .
HB2_11 H 0.713116 1.021688 0.598539 0.033 Uiso 1 1 calc R U . . .
CG_11 C 0.7056(3) 1.1265(18) 0.5420(2) 0.0263(15) Uani 1 1 d . . . . .
OD1_11 O 0.7351(2) 1.2677(12) 0.52761(15) 0.0270(12) Uani 1 1 d . . . . .
OD2_11 O 0.6616(3) 1.120(3) 0.5306(3) 0.063(3) Uani 1 1 d . . . . .
N_12 N 0.7998(2) 0.8963(12) 0.64794(15) 0.0171(11) Uani 1 1 d . . . . .
H0_12 H 0.802597 1.076411 0.644320 0.021 Uiso 1 1 calc R U . . .
CA_12 C 0.8061(3) 0.7910(15) 0.68612(18) 0.0166(13) Uani 1 1 d . . . . .
HA_12 H 0.802306 0.583933 0.685736 0.020 Uiso 1 1 calc R U . . .
C_12 C 0.7665(2) 0.9224(13) 0.70558(18) 0.0134(12) Uani 1 1 d . U . . .
O_12 O 0.76498(19) 1.1814(10) 0.70822(14) 0.0186(9) Uani 1 1 d . U . . .
CB_12 C 0.8558(3) 0.8670(17) 0.7058(2) 0.0205(14) Uani 1 1 d . . . . .
HB1_12 H 0.879900 0.783746 0.691420 0.025 Uiso 1 1 calc R U . . .
HB2_12 H 0.859436 1.071738 0.704746 0.025 Uiso 1 1 calc R U . . .
CG_12 C 0.8668(3) 0.7753(16) 0.7465(2) 0.0187(13) Uani 1 1 d . . . . .
CD1_12 C 0.8429(3) 0.5593(16) 0.7621(2) 0.0236(16) Uani 1 1 d . . . . .
HD1_12 H 0.818308 0.461502 0.746929 0.028 Uiso 1 1 calc R U . . .
CD2_12 C 0.9041(3) 0.9051(16) 0.7695(2) 0.0252(16) Uani 1 1 d . . . . .
HD2_12 H 0.920815 1.053199 0.759475 0.030 Uiso 1 1 calc R U . . .
CE1_12 C 0.8546(3) 0.486(2) 0.7994(2) 0.0278(15) Uani 1 1 d . . . . .
HE1_12 H 0.836722 0.345286 0.810075 0.033 Uiso 1 1 calc R U . . .
CE2_12 C 0.9175(3) 0.8261(19) 0.8062(2) 0.0276(16) Uani 1 1 d . . . . .
HE2_12 H 0.943629 0.913700 0.821081 0.033 Uiso 1 1 calc R U . . .
CZ_12 C 0.8918(3) 0.615(2) 0.8211(2) 0.0264(16) Uani 1 1 d . . . . .
N_13 N 0.7349(2) 0.7512(12) 0.71812(16) 0.0170(11) Uani 1 1 d . . . . .
H0_13 H 0.736920 0.571949 0.713504 0.020 Uiso 1 1 calc R U . . .
CA_13 C 0.6971(3) 0.8479(15) 0.73920(19) 0.0177(13) Uani 1 1 d . . . . .
HA_13 H 0.697605 1.055800 0.740740 0.021 Uiso 1 1 calc R U . . .
C_13 C 0.7071(3) 0.7230(13) 0.7788(2) 0.0164(13) Uani 1 1 d . . . . .
O_13 O 0.7083(2) 0.4706(12) 0.78291(14) 0.0274(12) Uani 1 1 d . . . . .
CB_13 C 0.6483(3) 0.7496(16) 0.7205(2) 0.0219(14) Uani 1 1 d . . . . .
HB1_13 H 0.647983 0.543679 0.719258 0.026 Uiso 1 1 calc R U . . .
HB2_13 H 0.623357 0.809032 0.735808 0.026 Uiso 1 1 calc R U . . .
CG_13 C 0.6373(3) 0.8663(15) 0.6816(2) 0.0228(15) Uani 1 1 d . . . . .
OD1_13 O 0.6302(3) 1.1181(13) 0.6767(2) 0.0381(16) Uani 1 1 d . . . . .
ND2_13 N 0.6355(3) 0.6890(15) 0.65279(19) 0.0285(14) Uani 1 1 d . . . . .
HD2A_13 H 0.629071 0.750635 0.629593 0.034 Uiso 1 1 calc R U . . .
HD2B_13 H 0.640658 0.510385 0.657010 0.034 Uiso 1 1 calc R U . . .
N_14 N 0.7154(3) 0.9072(12) 0.80678(17) 0.0205(13) Uani 1 1 d . . . . .
H0_14 H 0.714919 1.085918 0.801347 0.025 Uiso 1 1 calc R U . . .
CA_14 C 0.7250(3) 0.8221(16) 0.84607(19) 0.0218(15) Uani 1 1 d . . . . .
HA_14 H 0.724841 0.614194 0.847506 0.026 Uiso 1 1 calc R U . . .
C_14 C 0.6840(3) 0.9384(17) 0.8661(2) 0.0276(17) Uani 1 1 d . . . . .
O_14 O 0.6805(3) 1.1903(13) 0.8707(2) 0.0432(19) Uani 1 1 d . . . . .
CB_14 C 0.7728(3) 0.9299(18) 0.8649(2) 0.0309(18) Uani 1 1 d . . . . .
HB1_14 H 0.771289 1.134395 0.868042 0.037 Uiso 1 1 calc R U . . .
HB2_14 H 0.798172 0.887364 0.849154 0.037 Uiso 1 1 calc R U . . .
CG_14 C 0.7846(4) 0.788(3) 0.9042(3) 0.045(2) Uani 1 1 d . . . . .
HG1_14 H 0.755706 0.790743 0.917148 0.054 Uiso 1 1 calc R U . . .
HG2_14 H 0.793049 0.590350 0.900472 0.054 Uiso 1 1 calc R U . . .
CD_14 C 0.8257(5) 0.928(2) 0.9293(3) 0.046(3) Uani 1 1 d . . . . .
HD1_14 H 0.852441 0.963605 0.914599 0.055 Uiso 1 1 calc R U . . .
HD2_14 H 0.814779 1.108932 0.938223 0.055 Uiso 1 1 calc R U . . .
CE_14 C 0.8431(5) 0.746(3) 0.9628(3) 0.053(3) Uani 1 1 d . . . . .
HE1_14 H 0.815194 0.681805 0.974691 0.064 Uiso 1 1 calc R U . . .
HE2_14 H 0.859002 0.578787 0.954003 0.064 Uiso 1 1 calc R U . . .
NZ_14 N 0.8764(4) 0.891(2) 0.9909(3) 0.055(3) Uani 1 1 d . . . . .
HZ1_14 H 0.888655 0.768209 1.008945 0.083 Uiso 1 1 calc R U . . .
HZ2_14 H 0.860760 1.029277 1.001501 0.083 Uiso 1 1 calc R U . . .
HZ3_14 H 0.900630 0.964813 0.979584 0.083 Uiso 1 1 calc R U . . .
IZ_15 I 0.50863(3) 0.65136(18) 0.70468(2) 0.0489(2) Uani 1 1 d . . . . .
N_15 N 0.6543(3) 0.7553(14) 0.8779(2) 0.0287(16) Uani 1 1 d . . . . .
H0_15 H 0.659977 0.576433 0.875511 0.034 Uiso 1 1 calc R U . . .
CA_15 C 0.6123(3) 0.843(2) 0.8949(3) 0.0318(18) Uani 1 1 d . . . . .
HA_15 H 0.603052 1.030981 0.884442 0.038 Uiso 1 1 calc R U . . .
C_15 C 0.6216(4) 0.875(2) 0.9375(3) 0.043(2) Uani 1 1 d . . . . .
O_15 O 0.5911(3) 1.013(3) 0.9521(3) 0.079(4) Uani 1 1 d . . . . .
CB_15 C 0.5708(4) 0.649(2) 0.8825(3) 0.0349(18) Uani 1 1 d . . . . .
HB1_15 H 0.579921 0.457572 0.890932 0.042 Uiso 1 1 calc R U . . .
HB2_15 H 0.543137 0.705275 0.895052 0.042 Uiso 1 1 calc R U . . .
CG_15 C 0.5557(3) 0.644(2) 0.8405(3) 0.0344(19) Uani 1 1 d . . . . .
CD1_15 C 0.5769(4) 0.467(2) 0.8170(3) 0.0346(19) Uani 1 1 d . . . . .
HD1_15 H 0.601246 0.342913 0.827525 0.042 Uiso 1 1 calc R U . . .
CD2_15 C 0.5218(3) 0.834(2) 0.8235(3) 0.035(2) Uani 1 1 d . . . . .
HD2_15 H 0.507456 0.961596 0.838869 0.042 Uiso 1 1 calc R U . . .
CE1_15 C 0.5635(4) 0.467(2) 0.7785(3) 0.0367(19) Uani 1 1 d . . . . .
HE1_15 H 0.578220 0.341275 0.763068 0.044 Uiso 1 1 calc R U . . .
CE2_15 C 0.5088(3) 0.840(2) 0.7858(3) 0.038(2) Uani 1 1 d . . . . .
HE2_15 H 0.486293 0.973952 0.775231 0.045 Uiso 1 1 calc R U . . .
CZ_15 C 0.5283(3) 0.650(2) 0.7624(3) 0.0335(18) Uani 1 1 d . . . . .
OXT_15 O 0.6581(4) 0.765(2) 0.9556(2) 0.064(3) Uani 1 1 d . . . . .
O_21 O 0.4971(3) 0.679(2) 0.6123(3) 0.059(2) Uani 1 1 d . . . . .
O_22 O 0.5478(3) 1.1807(19) 0.6213(2) 0.0498(19) Uani 1 1 d . . . . .
O_23 O 0.8859(3) 0.661(3) 0.5815(3) 0.064(2) Uani 1 1 d . . . . .
O_24 O 0.6019(3) 0.876(2) 0.5745(2) 0.052(2) Uani 1 1 d . . . . .
O_25 O 0.8991(4) 1.151(3) 0.6238(3) 0.087(4) Uani 1 1 d . . . . .
O_26 O 0.9499(4) 0.080(3) 0.9520(3) 0.077(3) Uani 1 1 d . . . . .
O_27 O 1.000000 0.682(6) 0.500000 0.116(7) Uani 1 2 d S T P . .
O_28 O 0.9982(5) 0.567(2) 0.9612(3) 0.073(3) Uani 1 1 d . . . . .
O_29 O 0.8649(6) 0.098(4) 0.5137(4) 0.115(5) Uani 1 1 d . . . . .
O_30 O 0.9498(5) 0.330(4) 0.5423(4) 0.119(6) Uani 1 1 d . . . . .
O_31 O 0.7156(8) 1.307(5) 0.9531(7) 0.158(8) Uani 1 1 d . . . . .
OA_32 O 0.5845(12) 0.487(6) 0.5175(7) 0.150(12) Uani 0.7 1 d . . P A 1
OB_32 O 0.5521(13) 0.397(7) 0.5433(9) 0.064(8) Uiso 0.3 1 d . . P B 2


_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
IZ_11 CZ_12 2.102(7) . ?
N_11 CA_11 1.491(9) . ?
N_11 H0A_11 0.9100 . ?
N_11 H0B_11 0.9100 . ?
N_11 H0C_11 0.9100 . ?
CA_11 C_11 1.535(10) . ?
CA_11 CB_11 1.538(12) . ?
CA_11 HA_11 1.0000 . ?
C_11 O_11 1.229(9) . ?
C_11 N_12 1.334(9) . ?
CB_11 CG_11 1.532(11) . ?
CB_11 HB1_11 0.9900 . ?
CB_11 HB2_11 0.9900 . ?
CG_11 OD1_11 1.235(10) . ?
CG_11 OD2_11 1.257(11) . ?
N_12 CA_12 1.450(8) . ?
N_12 H0_12 0.8800 . ?
CA_12 C_12 1.528(9) . ?
CA_12 CB_12 1.529(11) . ?
CA_12 HA_12 1.0000 . ?
C_12 O_12 1.249(9) . ?
C_12 N_13 1.333(8) . ?
CB_12 CG_12 1.521(10) . ?
CB_12 HB1_12 0.9900 . ?
CB_12 HB2_12 0.9900 . ?
CG_12 CD1_12 1.394(11) . ?
CG_12 CD2_12 1.396(11) . ?
CD1_12 CE1_12 1.382(10) . ?
CD1_12 HD1_12 0.9500 . ?
CD2_12 CE2_12 1.376(12) . ?
CD2_12 HD2_12 0.9500 . ?
CE1_12 CZ_12 1.373(12) . ?
CE1_12 HE1_12 0.9500 . ?
CE2_12 CZ_12 1.393(13) . ?
CE2_12 HE2_12 0.9500 . ?
N_13 CA_13 1.461(9) . ?
N_13 H0_13 0.8800 . ?
CA_13 CB_13 1.525(11) . ?
CA_13 C_13 1.534(10) . ?
CA_13 HA_13 1.0000 . ?
C_13 O_13 1.221(9) . ?
C_13 N_14 1.337(9) . ?
CB_13 CG_13 1.500(11) . ?
CB_13 HB1_13 0.9900 . ?
CB_13 HB2_13 0.9900 . ?
CG_13 OD1_13 1.234(9) . ?
CG_13 ND2_13 1.335(11) . ?
ND2_13 HD2A_13 0.8800 . ?
ND2_13 HD2B_13 0.8800 . ?
N_14 CA_14 1.459(9) . ?
N_14 H0_14 0.8800 . ?
CA_14 CB_14 1.518(12) . ?
CA_14 C_14 1.544(11) . ?
CA_14 HA_14 1.0000 . ?
C_14 O_14 1.227(11) . ?
C_14 N_15 1.321(11) . ?
CB_14 CG_14 1.562(13) . ?
CB_14 HB1_14 0.9900 . ?
CB_14 HB2_14 0.9900 . ?
CG_14 CD_14 1.529(16) . ?
CG_14 HG1_14 0.9900 . ?
CG_14 HG2_14 0.9900 . ?
CD_14 CE_14 1.516(15) . ?
CD_14 HD1_14 0.9900 . ?
CD_14 HD2_14 0.9900 . ?
CE_14 NZ_14 1.463(16) . ?
CE_14 HE1_14 0.9900 . ?
CE_14 HE2_14 0.9900 . ?
NZ_14 HZ1_14 0.9100 . ?
NZ_14 HZ2_14 0.9100 . ?
NZ_14 HZ3_14 0.9100 . ?
IZ_15 CZ_15 2.075(10) . ?
N_15 CA_15 1.463(11) . ?
N_15 H0_15 0.8800 . ?
CA_15 CB_15 1.518(14) . ?
CA_15 C_15 1.522(15) . ?
CA_15 HA_15 1.0000 . ?
C_15 O_15 1.255(14) . ?
C_15 OXT_15 1.260(15) . ?
CB_15 CG_15 1.510(14) . ?
CB_15 HB1_15 0.9900 . ?
CB_15 HB2_15 0.9900 . ?
CG_15 CD1_15 1.388(13) . ?
CG_15 CD2_15 1.402(15) . ?
CD1_15 CE1_15 1.382(13) . ?
CD1_15 HD1_15 0.9500 . ?
CD2_15 CE2_15 1.354(16) . ?
CD2_15 HD2_15 0.9500 . ?
CE1_15 CZ_15 1.396(15) . ?
CE1_15 HE1_15 0.9500 . ?
CE2_15 CZ_15 1.398(14) . ?
CE2_15 HE2_15 0.9500 . ?

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
CA_11 N_11 H0A_11 109.5 . . ?
CA_11 N_11 H0B_11 109.5 . . ?
H0A_11 N_11 H0B_11 109.5 . . ?
CA_11 N_11 H0C_11 109.5 . . ?
H0A_11 N_11 H0C_11 109.5 . . ?
H0B_11 N_11 H0C_11 109.5 . . ?
N_11 CA_11 C_11 108.2(6) . . ?
N_11 CA_11 CB_11 111.0(6) . . ?
C_11 CA_11 CB_11 107.9(6) . . ?
N_11 CA_11 HA_11 109.9 . . ?
C_11 CA_11 HA_11 109.9 . . ?
CB_11 CA_11 HA_11 109.9 . . ?
O_11 C_11 N_12 125.8(7) . . ?
O_11 C_11 CA_11 120.7(6) . . ?
N_12 C_11 CA_11 113.4(6) . . ?
CG_11 CB_11 CA_11 113.4(6) . . ?
CG_11 CB_11 HB1_11 108.9 . . ?
CA_11 CB_11 HB1_11 108.9 . . ?
CG_11 CB_11 HB2_11 108.9 . . ?
CA_11 CB_11 HB2_11 108.9 . . ?
HB1_11 CB_11 HB2_11 107.7 . . ?
OD1_11 CG_11 OD2_11 124.6(8) . . ?
OD1_11 CG_11 CB_11 119.5(8) . . ?
OD2_11 CG_11 CB_11 116.0(8) . . ?
C_11 N_12 CA_12 122.6(6) . . ?
C_11 N_12 H0_12 118.7 . . ?
CA_12 N_12 H0_12 118.7 . . ?
N_12 CA_12 C_12 106.3(6) . . ?
N_12 CA_12 CB_12 110.2(6) . . ?
C_12 CA_12 CB_12 111.8(6) . . ?
N_12 CA_12 HA_12 109.5 . . ?
C_12 CA_12 HA_12 109.5 . . ?
CB_12 CA_12 HA_12 109.5 . . ?
O_12 C_12 N_13 123.9(6) . . ?
O_12 C_12 CA_12 118.7(6) . . ?
N_13 C_12 CA_12 117.4(6) . . ?
CG_12 CB_12 CA_12 115.9(6) . . ?
CG_12 CB_12 HB1_12 108.3 . . ?
CA_12 CB_12 HB1_12 108.3 . . ?
CG_12 CB_12 HB2_12 108.3 . . ?
CA_12 CB_12 HB2_12 108.3 . . ?
HB1_12 CB_12 HB2_12 107.4 . . ?
CD1_12 CG_12 CD2_12 117.5(7) . . ?
CD1_12 CG_12 CB_12 123.5(7) . . ?
CD2_12 CG_12 CB_12 119.0(7) . . ?
CE1_12 CD1_12 CG_12 120.9(8) . . ?
CE1_12 CD1_12 HD1_12 119.6 . . ?
CG_12 CD1_12 HD1_12 119.6 . . ?
CE2_12 CD2_12 CG_12 122.3(7) . . ?
CE2_12 CD2_12 HD2_12 118.8 . . ?
CG_12 CD2_12 HD2_12 118.8 . . ?
CZ_12 CE1_12 CD1_12 120.1(8) . . ?
CZ_12 CE1_12 HE1_12 120.0 . . ?
CD1_12 CE1_12 HE1_12 120.0 . . ?
CD2_12 CE2_12 CZ_12 118.4(8) . . ?
CD2_12 CE2_12 HE2_12 120.8 . . ?
CZ_12 CE2_12 HE2_12 120.8 . . ?
CE1_12 CZ_12 CE2_12 120.7(7) . . ?
CE1_12 CZ_12 IZ_11 118.7(6) . . ?
CE2_12 CZ_12 IZ_11 120.5(6) . . ?
C_12 N_13 CA_13 122.9(6) . . ?
C_12 N_13 H0_13 118.5 . . ?
CA_13 N_13 H0_13 118.5 . . ?
N_13 CA_13 CB_13 110.5(6) . . ?
N_13 CA_13 C_13 107.2(6) . . ?
CB_13 CA_13 C_13 109.5(6) . . ?
N_13 CA_13 HA_13 109.9 . . ?
CB_13 CA_13 HA_13 109.9 . . ?
C_13 CA_13 HA_13 109.9 . . ?
O_13 C_13 N_14 124.5(7) . . ?
O_13 C_13 CA_13 120.0(6) . . ?
N_14 C_13 CA_13 115.5(6) . . ?
CG_13 CB_13 CA_13 111.2(6) . . ?
CG_13 CB_13 HB1_13 109.4 . . ?
CA_13 CB_13 HB1_13 109.4 . . ?
CG_13 CB_13 HB2_13 109.4 . . ?
CA_13 CB_13 HB2_13 109.4 . . ?
HB1_13 CB_13 HB2_13 108.0 . . ?
OD1_13 CG_13 ND2_13 121.8(8) . . ?
OD1_13 CG_13 CB_13 120.5(8) . . ?
ND2_13 CG_13 CB_13 117.7(7) . . ?
CG_13 ND2_13 HD2A_13 120.0 . . ?
CG_13 ND2_13 HD2B_13 120.0 . . ?
HD2A_13 ND2_13 HD2B_13 120.0 . . ?
C_13 N_14 CA_14 122.2(6) . . ?
C_13 N_14 H0_14 118.9 . . ?
CA_14 N_14 H0_14 118.9 . . ?
N_14 CA_14 CB_14 112.3(7) . . ?
N_14 CA_14 C_14 107.0(6) . . ?
CB_14 CA_14 C_14 110.1(6) . . ?
N_14 CA_14 HA_14 109.1 . . ?
CB_14 CA_14 HA_14 109.1 . . ?
C_14 CA_14 HA_14 109.1 . . ?
O_14 C_14 N_15 123.3(8) . . ?
O_14 C_14 CA_14 119.8(8) . . ?
N_15 C_14 CA_14 116.9(7) . . ?
CA_14 CB_14 CG_14 109.1(8) . . ?
CA_14 CB_14 HB1_14 109.9 . . ?
CG_14 CB_14 HB1_14 109.9 . . ?
CA_14 CB_14 HB2_14 109.9 . . ?
CG_14 CB_14 HB2_14 109.9 . . ?
HB1_14 CB_14 HB2_14 108.3 . . ?
CD_14 CG_14 CB_14 113.3(9) . . ?
CD_14 CG_14 HG1_14 108.9 . . ?
CB_14 CG_14 HG1_14 108.9 . . ?
CD_14 CG_14 HG2_14 108.9 . . ?
CB_14 CG_14 HG2_14 108.9 . . ?
HG1_14 CG_14 HG2_14 107.7 . . ?
CE_14 CD_14 CG_14 110.8(10) . . ?
CE_14 CD_14 HD1_14 109.5 . . ?
CG_14 CD_14 HD1_14 109.5 . . ?
CE_14 CD_14 HD2_14 109.5 . . ?
CG_14 CD_14 HD2_14 109.5 . . ?
HD1_14 CD_14 HD2_14 108.1 . . ?
NZ_14 CE_14 CD_14 112.5(10) . . ?
NZ_14 CE_14 HE1_14 109.1 . . ?
CD_14 CE_14 HE1_14 109.1 . . ?
NZ_14 CE_14 HE2_14 109.1 . . ?
CD_14 CE_14 HE2_14 109.1 . . ?
HE1_14 CE_14 HE2_14 107.8 . . ?
CE_14 NZ_14 HZ1_14 109.5 . . ?
CE_14 NZ_14 HZ2_14 109.5 . . ?
HZ1_14 NZ_14 HZ2_14 109.5 . . ?
CE_14 NZ_14 HZ3_14 109.5 . . ?
HZ1_14 NZ_14 HZ3_14 109.5 . . ?
HZ2_14 NZ_14 HZ3_14 109.5 . . ?
C_14 N_15 CA_15 121.5(7) . . ?
C_14 N_15 H0_15 119.2 . . ?
CA_15 N_15 H0_15 119.2 . . ?
N_15 CA_15 CB_15 109.6(7) . . ?
N_15 CA_15 C_15 113.8(9) . . ?
CB_15 CA_15 C_15 112.5(8) . . ?
N_15 CA_15 HA_15 106.8 . . ?
CB_15 CA_15 HA_15 106.8 . . ?
C_15 CA_15 HA_15 106.8 . . ?
O_15 C_15 OXT_15 124.2(11) . . ?
O_15 C_15 CA_15 115.8(11) . . ?
OXT_15 C_15 CA_15 119.9(9) . . ?
CG_15 CB_15 CA_15 114.2(8) . . ?
CG_15 CB_15 HB1_15 108.7 . . ?
CA_15 CB_15 HB1_15 108.7 . . ?
CG_15 CB_15 HB2_15 108.7 . . ?
CA_15 CB_15 HB2_15 108.7 . . ?
HB1_15 CB_15 HB2_15 107.6 . . ?
CD1_15 CG_15 CD2_15 117.1(9) . . ?
CD1_15 CG_15 CB_15 121.8(9) . . ?
CD2_15 CG_15 CB_15 120.9(9) . . ?
CE1_15 CD1_15 CG_15 121.7(9) . . ?
CE1_15 CD1_15 HD1_15 119.2 . . ?
CG_15 CD1_15 HD1_15 119.2 . . ?
CE2_15 CD2_15 CG_15 122.0(9) . . ?
CE2_15 CD2_15 HD2_15 119.0 . . ?
CG_15 CD2_15 HD2_15 119.0 . . ?
CD1_15 CE1_15 CZ_15 120.0(9) . . ?
CD1_15 CE1_15 HE1_15 120.0 . . ?
CZ_15 CE1_15 HE1_15 120.0 . . ?
CD2_15 CE2_15 CZ_15 120.7(10) . . ?
CD2_15 CE2_15 HE2_15 119.7 . . ?
CZ_15 CE2_15 HE2_15 119.7 . . ?
CE1_15 CZ_15 CE2_15 118.4(9) . . ?
CE1_15 CZ_15 IZ_15 119.9(7) . . ?
CE2_15 CZ_15 IZ_15 121.6(8) . . ?

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
N_11 CA_11 C_11 O_11 -32.7(11) . . . . ?
CB_11 CA_11 C_11 O_11 87.4(9) . . . . ?
N_11 CA_11 C_11 N_12 149.9(7) . . . . ?
CB_11 CA_11 C_11 N_12 -90.0(8) . . . . ?
N_11 CA_11 CB_11 CG_11 -68.7(8) . . . . ?
C_11 CA_11 CB_11 CG_11 173.0(6) . . . . ?
CA_11 CB_11 CG_11 OD1_11 -14.7(11) . . . . ?
CA_11 CB_11 CG_11 OD2_11 163.9(9) . . . . ?
O_11 C_11 N_12 CA_12 -6.2(13) . . . . ?
CA_11 C_11 N_12 CA_12 171.0(7) . . . . ?
C_11 N_12 CA_12 C_12 -117.4(8) . . . . ?
C_11 N_12 CA_12 CB_12 121.3(8) . . . . ?
N_12 CA_12 C_12 O_12 -60.8(8) . . . . ?
CB_12 CA_12 C_12 O_12 59.5(8) . . . . ?
N_12 CA_12 C_12 N_13 118.0(7) . . . . ?
CB_12 CA_12 C_12 N_13 -121.7(7) . . . . ?
N_12 CA_12 CB_12 CG_12 178.5(6) . . . . ?
C_12 CA_12 CB_12 CG_12 60.6(8) . . . . ?
CA_12 CB_12 CG_12 CD1_12 22.0(11) . . . . ?
CA_12 CB_12 CG_12 CD2_12 -160.6(7) . . . . ?
CD2_12 CG_12 CD1_12 CE1_12 2.7(12) . . . . ?
CB_12 CG_12 CD1_12 CE1_12 -179.9(8) . . . . ?
CD1_12 CG_12 CD2_12 CE2_12 0.2(12) . . . . ?
CB_12 CG_12 CD2_12 CE2_12 -177.4(8) . . . . ?
CG_12 CD1_12 CE1_12 CZ_12 -3.7(14) . . . . ?
CG_12 CD2_12 CE2_12 CZ_12 -2.0(13) . . . . ?
CD1_12 CE1_12 CZ_12 CE2_12 1.8(14) . . . . ?
CD1_12 CE1_12 CZ_12 IZ_11 -174.6(7) . . . . ?
CD2_12 CE2_12 CZ_12 CE1_12 1.0(13) . . . . ?
CD2_12 CE2_12 CZ_12 IZ_11 177.3(6) . . . . ?
O_12 C_12 N_13 CA_13 -5.2(11) . . . . ?
CA_12 C_12 N_13 CA_13 176.2(6) . . . . ?
C_12 N_13 CA_13 CB_13 125.4(7) . . . . ?
C_12 N_13 CA_13 C_13 -115.3(7) . . . . ?
N_13 CA_13 C_13 O_13 -60.3(9) . . . . ?
CB_13 CA_13 C_13 O_13 59.6(9) . . . . ?
N_13 CA_13 C_13 N_14 118.0(7) . . . . ?
CB_13 CA_13 C_13 N_14 -122.0(7) . . . . ?
N_13 CA_13 CB_13 CG_13 -61.8(8) . . . . ?
C_13 CA_13 CB_13 CG_13 -179.7(6) . . . . ?
CA_13 CB_13 CG_13 OD1_13 -67.7(11) . . . . ?
CA_13 CB_13 CG_13 ND2_13 112.2(8) . . . . ?
O_13 C_13 N_14 CA_14 -2.3(13) . . . . ?
CA_13 C_13 N_14 CA_14 179.4(7) . . . . ?
C_13 N_14 CA_14 CB_14 122.1(8) . . . . ?
C_13 N_14 CA_14 C_14 -117.0(8) . . . . ?
N_14 CA_14 C_14 O_14 -68.8(10) . . . . ?
CB_14 CA_14 C_14 O_14 53.4(11) . . . . ?
N_14 CA_14 C_14 N_15 111.8(8) . . . . ?
CB_14 CA_14 C_14 N_15 -125.9(8) . . . . ?
N_14 CA_14 CB_14 CG_14 -169.9(7) . . . . ?
C_14 CA_14 CB_14 CG_14 71.0(9) . . . . ?
CA_14 CB_14 CG_14 CD_14 -166.7(9) . . . . ?
CB_14 CG_14 CD_14 CE_14 -166.9(10) . . . . ?
CG_14 CD_14 CE_14 NZ_14 -170.0(11) . . . . ?
O_14 C_14 N_15 CA_15 5.0(15) . . . . ?
CA_14 C_14 N_15 CA_15 -175.7(8) . . . . ?
C_14 N_15 CA_15 CB_15 142.3(9) . . . . ?
C_14 N_15 CA_15 C_15 -90.7(11) . . . . ?
N_15 CA_15 C_15 O_15 162.9(11) . . . . ?
CB_15 CA_15 C_15 O_15 -71.7(13) . . . . ?
N_15 CA_15 C_15 OXT_15 -17.0(15) . . . . ?
CB_15 CA_15 C_15 OXT_15 108.4(13) . . . . ?
N_15 CA_15 CB_15 CG_15 -60.9(11) . . . . ?
C_15 CA_15 CB_15 CG_15 171.4(8) . . . . ?
CA_15 CB_15 CG_15 CD1_15 87.3(11) . . . . ?
CA_15 CB_15 CG_15 CD2_15 -88.2(10) . . . . ?
CD2_15 CG_15 CD1_15 CE1_15 -3.3(14) . . . . ?
CB_15 CG_15 CD1_15 CE1_15 -178.9(9) . . . . ?
CD1_15 CG_15 CD2_15 CE2_15 2.1(14) . . . . ?
CB_15 CG_15 CD2_15 CE2_15 177.7(9) . . . . ?
CG_15 CD1_15 CE1_15 CZ_15 1.0(15) . . . . ?
CG_15 CD2_15 CE2_15 CZ_15 1.5(14) . . . . ?
CD1_15 CE1_15 CZ_15 CE2_15 2.7(14) . . . . ?
CD1_15 CE1_15 CZ_15 IZ_15 179.5(7) . . . . ?
CD2_15 CE2_15 CZ_15 CE1_15 -3.9(14) . . . . ?
CD2_15 CE2_15 CZ_15 IZ_15 179.4(7) . . . . ?

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
_geom_hbond_publ_flag
N_11 H0A_11 OD1_11 0.91 2.60 3.134(9) 118.5 . yes
N_11 H0A_11 OD1_11 0.91 2.00 2.803(8) 146.8 4_646 yes
N_11 H0B_11 OD1_11 0.91 1.92 2.762(9) 153.5 1_545 yes
N_11 H0C_11 O_23 0.91 1.89 2.751(12) 156.7 . yes
CA_11 HA_11 O_11 1.00 2.34 3.111(9) 133.5 1_565 yes
N_12 H0_12 O_11 0.88 2.14 2.976(8) 158.2 1_565 yes
CA_12 HA_12 O_12 1.00 2.39 3.284(9) 148.2 1_545 yes
N_13 H0_13 O_12 0.88 2.05 2.901(8) 161.1 1_545 yes
CA_13 HA_13 O_13 1.00 2.50 3.373(9) 146.1 1_565 yes
CB_13 HB1_13 OD1_13 0.99 2.56 3.423(10) 145.5 1_545 yes
ND2_13 HD2A_13 O_24 0.88 2.11 2.986(10) 170.4 . yes
ND2_13 HD2B_13 OD1_13 0.88 2.05 2.883(9) 158.2 1_545 yes
N_14 H0_14 O_13 0.88 1.96 2.837(8) 172.2 1_565 yes
CA_14 HA_14 O_14 1.00 2.58 3.443(10) 144.1 1_545 yes
CD_14 HD1_14 IZ_11 0.99 3.30 3.946(13) 124.2 . yes
NZ_14 HZ1_14 O_15 0.91 1.89 2.798(14) 175.2 4_647 yes
NZ_14 HZ2_14 OXT_15 0.91 2.04 2.892(15) 155.9 4_657 yes
NZ_14 HZ3_14 O_26 0.91 1.89 2.793(16) 172.8 1_565 yes
N_15 H0_15 O_14 0.88 1.96 2.833(9) 173.2 1_545 yes

_refine_diff_density_max         2.306
_refine_diff_density_min         -1.903
_refine_diff_density_rms         0.158


# start Validation Reply Form

_vrf_PLAT430_DFINKFI             
;
PROBLEM:  Short Inter D...A Contact
RESPONSE: Water molecules have been located in crystal voids. Most of them are 
          involved in hydrogen bonds with peptide hetero atoms. Hydrogen atoms
          bound to water molecules could not be unambiguously located and 
          have not been modeled.
;
_vrf_PLAT306_DFINKFI             
;
PROBLEM:  Isolated Oxygen Atom (H-atoms Missing ?)
RESPONSE: Water molecules have been located in crystal voids. Most of them are 
          involved in hydrogen bonds with peptide hetero atoms. Hydrogen atoms
          bound to water molecules could not be unambiguously located and 
          have not been modeled.
;
_vrf_PLAT043_DFINKFI             
;
PROBLEM:  Calculated and Reported Mol. Weight Differ by ..      46.36 Check
RESPONSE: Water molecules have been found in crystal voids but their hydrogen 
          atoms could not be unambiguously located and therefore have not been 
          modeled. Contributions of these H atoms have been included in the 
          reported crystal properties.          
;

# end Validation Reply Form

