# Electronic Supplementary Material (ESI) for Soft Matter.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_mc268f
_database_code_depnum_ccdc_archive 'CCDC 1535890'
_audit_update_record             
;
2017-03-03 deposited with the CCDC.
2017-05-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H33 N11 O6, 7(H2 O)'
_chemical_formula_sum            'C24 H47 N11 O13'
_chemical_formula_weight         697.72

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   9.11756(10)
_cell_length_b                   21.6446(2)
_cell_length_c                   17.9917(2)
_cell_angle_alpha                90
_cell_angle_beta                 98.1280(10)
_cell_angle_gamma                90
_cell_volume                     3514.92(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    16615
_cell_measurement_theta_min      2.472
_cell_measurement_theta_max      70.963

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_F_000             1488
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.915
_shelx_estimated_absorpt_T_min   0.711
_shelx_estimated_absorpt_T_max   0.956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.59078
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Enhance (Cu) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1274
_diffrn_reflns_number            45118
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.213
_diffrn_reflns_theta_max         70.887
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6749
_reflns_number_gt                5703
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_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    'SIR2014 (Burla et al., 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1002P)²+1.4070P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6749
_refine_ls_number_parameters     432
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0565
_refine_ls_wR_factor_ref         0.1744
_refine_ls_wR_factor_gt          0.1647
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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
N1T N -0.24212(19) 0.49466(7) 0.31118(9) 0.0441(4) Uani 1 1 d . . . . .
C2T C -0.2889(2) 0.46383(9) 0.37017(12) 0.0461(4) Uani 1 1 d . . . . .
O2T O -0.3614(2) 0.41664(8) 0.36129(10) 0.0680(5) Uani 1 1 d . . . . .
N3T N -0.24752(19) 0.49025(7) 0.43880(9) 0.0457(4) Uani 1 1 d . . . . .
H3T H -0.2836 0.4741 0.4760 0.055 Uiso 1 1 calc R U . . .
C4T C -0.1544(2) 0.53997(8) 0.45506(11) 0.0405(4) Uani 1 1 d . . . . .
O4T O -0.11797(18) 0.55649(7) 0.52031(8) 0.0539(4) Uani 1 1 d . . . . .
C5T C -0.1057(2) 0.56960(8) 0.39052(11) 0.0410(4) Uani 1 1 d . . . . .
C6T C -0.1499(2) 0.54500(9) 0.32271(12) 0.0436(4) Uani 1 1 d . . . . .
H6T H -0.1164 0.5630 0.2813 0.052 Uiso 1 1 calc R U . . .
C7T C -0.0087(3) 0.62525(11) 0.40335(14) 0.0575(6) Uani 1 1 d . . . . .
H7T1 H 0.0167 0.6395 0.3562 0.086 Uiso 1 1 calc R U . . .
H7T2 H 0.0800 0.6147 0.4363 0.086 Uiso 1 1 calc R U . . .
H7T3 H -0.0604 0.6573 0.4258 0.086 Uiso 1 1 calc R U . . .
C01 C -0.2783(3) 0.46661(10) 0.23728(12) 0.0515(5) Uani 1 1 d . . . . .
H01A H -0.2609 0.4962 0.1990 0.062 Uiso 1 1 calc R U . . .
H01B H -0.3824 0.4555 0.2290 0.062 Uiso 1 1 calc R U . . .
C0 C -0.1844(2) 0.40925(9) 0.23076(11) 0.0436(4) Uani 1 1 d . . . . .
O0 O -0.05594(16) 0.40677(7) 0.26183(9) 0.0541(4) Uani 1 1 d . . . . .
N1 N -0.25275(18) 0.36408(8) 0.18875(9) 0.0434(4) Uani 1 1 d . . . . .
H1 H -0.3460 0.3678 0.1733 0.052 Uiso 1 1 calc R U . . .
C1A C -0.1771(2) 0.30843(9) 0.16761(10) 0.0428(4) Uani 1 1 d . . . . .
C1B1 C -0.0603(3) 0.32513(12) 0.11760(13) 0.0613(6) Uani 1 1 d . . . . .
H1B1 H -0.1073 0.3451 0.0728 0.092 Uiso 1 1 calc R U . . .
H1B2 H -0.0117 0.2882 0.1043 0.092 Uiso 1 1 calc R U . . .
H1B3 H 0.0115 0.3526 0.1443 0.092 Uiso 1 1 calc R U . . .
C1B2 C -0.2937(3) 0.26494(11) 0.12701(13) 0.0558(5) Uani 1 1 d . . . . .
H1B4 H -0.3663 0.2557 0.1592 0.084 Uiso 1 1 calc R U . . .
H1B5 H -0.2470 0.2274 0.1143 0.084 Uiso 1 1 calc R U . . .
H1B6 H -0.3412 0.2844 0.0820 0.084 Uiso 1 1 calc R U . . .
C1 C -0.1042(2) 0.27369(9) 0.23775(11) 0.0401(4) Uani 1 1 d . . . . .
O1 O 0.00358(16) 0.24008(7) 0.23362(9) 0.0520(4) Uani 1 1 d . . . . .
N2 N -0.16359(17) 0.28030(8) 0.30059(9) 0.0435(4) Uani 1 1 d . . . . .
H2 H -0.2392 0.3041 0.3000 0.052 Uiso 1 1 calc R U . . .
C2A C -0.1060(2) 0.24877(11) 0.37098(12) 0.0530(5) Uani 1 1 d . . . . .
C2B1 C -0.1364(3) 0.17968(13) 0.36454(18) 0.0769(8) Uani 1 1 d . . . . .
H2B1 H -0.2413 0.1728 0.3537 0.115 Uiso 1 1 calc R U . . .
H2B2 H -0.0985 0.1599 0.4111 0.115 Uiso 1 1 calc R U . . .
H2B3 H -0.0886 0.1628 0.3248 0.115 Uiso 1 1 calc R U . . .
C2B2 C -0.1828(3) 0.27814(16) 0.43271(14) 0.0734(8) Uani 1 1 d . . . . .
H2B4 H -0.1660 0.3219 0.4336 0.110 Uiso 1 1 calc R U . . .
H2B5 H -0.1432 0.2608 0.4804 0.110 Uiso 1 1 calc R U . . .
H2B6 H -0.2873 0.2701 0.4228 0.110 Uiso 1 1 calc R U . . .
C2 C 0.0618(2) 0.26118(10) 0.39010(12) 0.0511(5) Uani 1 1 d . . . . .
O2 O 0.1437(2) 0.22120(8) 0.42256(12) 0.0780(6) Uani 1 1 d . . . . .
N3 N 0.10875(18) 0.31697(8) 0.37487(10) 0.0459(4) Uani 1 1 d . . . . .
H3 H 0.0437 0.3442 0.3582 0.055 Uiso 1 1 calc R U . . .
C31 C 0.2642(2) 0.33496(10) 0.38469(13) 0.0523(5) Uani 1 1 d . . . . .
H31A H 0.3230 0.3034 0.4134 0.063 Uiso 1 1 calc R U . . .
H31B H 0.2766 0.3733 0.4129 0.063 Uiso 1 1 calc R U . . .
C32 C 0.3191(3) 0.34351(10) 0.30989(15) 0.0574(6) Uani 1 1 d . . . . .
H32A H 0.2657 0.3773 0.2828 0.069 Uiso 1 1 calc R U . . .
H32B H 0.4235 0.3542 0.3182 0.069 Uiso 1 1 calc R U . . .
N4 N 0.2981(2) 0.28760(9) 0.26520(11) 0.0541(5) Uani 1 1 d . . . . .
H4 H 0.2193 0.2846 0.2329 0.065 Uiso 1 1 calc R U . . .
C33 C 0.3918(2) 0.24156(10) 0.27100(13) 0.0492(5) Uani 1 1 d . . . . .
O3 O 0.51780(19) 0.24427(9) 0.30296(15) 0.0910(7) Uani 1 1 d . . . . .
C34 C 0.3265(2) 0.18220(10) 0.23427(14) 0.0548(5) Uani 1 1 d . . . . .
H34A H 0.2522 0.1664 0.2629 0.066 Uiso 1 1 calc R U . . .
H34B H 0.2777 0.1916 0.1841 0.066 Uiso 1 1 calc R U . . .
N1A N 0.6389(2) 0.06444(8) 0.06528(10) 0.0503(4) Uani 1 1 d . . . . .
C35 C 0.5386(2) 0.10948(11) 0.04991(13) 0.0528(5) Uani 1 1 d . . . . .
H35 H 0.5202 0.1218 0.0000 0.063 Uiso 1 1 calc R U . . .
N3A N 0.46198(19) 0.13882(8) 0.09655(11) 0.0506(4) Uani 1 1 d . . . . .
C36 C 0.4960(2) 0.11721(9) 0.16680(12) 0.0435(4) Uani 1 1 d . . . . .
C37 C 0.5959(2) 0.07105(9) 0.19058(12) 0.0433(4) Uani 1 1 d . . . . .
C38 C 0.6723(2) 0.04392(9) 0.13641(12) 0.0443(4) Uani 1 1 d . . . . .
N6A N 0.7748(2) 0.00019(9) 0.15166(11) 0.0560(5) Uani 1 1 d . . . . .
H6A1 H 0.8167 -0.0162 0.1182 0.084 Uiso 1 1 d . U . . .
H6A2 H 0.8033 -0.0131 0.1986 0.084 Uiso 1 1 d . U . . .
N7A N 0.6008(2) 0.06068(8) 0.26692(11) 0.0531(4) Uani 1 1 d . . . . .
C39 C 0.5052(3) 0.10000(11) 0.28723(13) 0.0555(5) Uani 1 1 d . . . . .
H39 H 0.4855 0.1036 0.3364 0.067 Uiso 1 1 calc R U . . .
N9A N 0.43700(19) 0.13516(8) 0.22970(11) 0.0509(4) Uani 1 1 d . . . . .
O1W O -0.5687(2) 0.37569(10) 0.12021(13) 0.0830(6) Uani 1 1 d . . . . .
H1WA H -0.6058 0.3395 0.1074 0.125 Uiso 1 1 d . U . . .
H1WB H -0.6417 0.3970 0.1300 0.125 Uiso 1 1 d . U . . .
O2W O 0.3191(3) 0.23846(10) 0.56377(13) 0.0960(8) Uani 1 1 d . . . . .
H2WA H 0.2652 0.2391 0.5284 0.144 Uiso 1 1 d . U . . .
H2WB H 0.3546 0.2788 0.5655 0.144 Uiso 1 1 d . U . . .
O3W O 0.2121(3) 0.09820(12) 0.38786(18) 0.1166(9) Uani 1 1 d . . . . .
H3WA H 0.1862 0.1380 0.4024 0.175 Uiso 1 1 d . U . . .
H3WB H 0.1317 0.0737 0.3987 0.175 Uiso 1 1 d . U . . .
O4W O 0.7686(3) -0.03745(14) 0.3341(2) 0.1363(12) Uani 1 1 d . . . . .
H4WA H 0.7111 -0.0009 0.3233 0.205 Uiso 1 1 d . U . . .
H4WB H 0.8470 -0.0267 0.3592 0.205 Uiso 1 1 d . U . . .
O5W O 0.0360(6) -0.0005(2) 0.4193(3) 0.205(2) Uani 1 1 d . . . . .
H5WA H 0.1103 -0.0182 0.4426 0.308 Uiso 1 1 d . U . . .
O6W O 0.4681(10) 0.0623(4) 0.4882(4) 0.236(3) Uani 0.8 1 d . . P . .
H6WA H 0.4557 0.0816 0.5272 0.353 Uiso 0.8 1 d . U P . .
H6WB H 0.3931 0.0737 0.4591 0.353 Uiso 0.8 1 d . U P . .
O7W O 0.2714(12) -0.0497(5) 0.5086(6) 0.256(4) Uiso 0.7 1 d . . P . .
O8W O 0.5139(17) 0.1617(6) 0.4575(8) 0.267(6) Uiso 0.5 1 d . . P . .


_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
N1T C2T 1.372(3) . ?
N1T C6T 1.374(3) . ?
N1T C01 1.456(3) . ?
C2T O2T 1.215(3) . ?
C2T N3T 1.365(3) . ?
N3T C4T 1.376(2) . ?
C4T O4T 1.227(2) . ?
C4T C5T 1.450(3) . ?
C5T C6T 1.340(3) . ?
C5T C7T 1.493(3) . ?
C01 C0 1.522(3) . ?
C0 O0 1.226(2) . ?
C0 N1 1.335(3) . ?
N1 C1A 1.465(2) . ?
C1A C1B2 1.527(3) . ?
C1A C1B1 1.532(3) . ?
C1A C1 1.537(3) . ?
C1 O1 1.233(2) . ?
C1 N2 1.329(3) . ?
N2 C2A 1.469(3) . ?
C2A C2B1 1.522(4) . ?
C2A C2B2 1.532(4) . ?
C2A C2 1.544(3) . ?
C2 O2 1.234(3) . ?
C2 N3 1.323(3) . ?
N3 C31 1.456(3) . ?
C31 C32 1.512(4) . ?
C32 N4 1.451(3) . ?
N4 C33 1.307(3) . ?
C33 O3 1.211(3) . ?
C33 C34 1.527(3) . ?
C34 N9A 1.443(3) . ?
N1A C35 1.338(3) . ?
N1A C38 1.348(3) . ?
C35 N3A 1.327(3) . ?
N3A C36 1.342(3) . ?
C36 N9A 1.376(3) . ?
C36 C37 1.379(3) . ?
C37 N7A 1.386(3) . ?
C37 C38 1.404(3) . ?
C38 N6A 1.331(3) . ?
N7A C39 1.307(3) . ?
C39 N9A 1.362(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
C2T N1T C6T 121.29(17) . . ?
C2T N1T C01 116.64(17) . . ?
C6T N1T C01 121.56(18) . . ?
O2T C2T N3T 123.1(2) . . ?
O2T C2T N1T 122.0(2) . . ?
N3T C2T N1T 114.83(17) . . ?
C2T N3T C4T 127.09(17) . . ?
O4T C4T N3T 120.42(18) . . ?
O4T C4T C5T 124.42(18) . . ?
N3T C4T C5T 115.16(17) . . ?
C6T C5T C4T 117.83(17) . . ?
C6T C5T C7T 123.82(19) . . ?
C4T C5T C7T 118.34(18) . . ?
C5T C6T N1T 123.46(18) . . ?
N1T C01 C0 110.68(16) . . ?
O0 C0 N1 124.45(18) . . ?
O0 C0 C01 120.81(18) . . ?
N1 C0 C01 114.73(17) . . ?
C0 N1 C1A 123.37(16) . . ?
N1 C1A C1B2 108.04(16) . . ?
N1 C1A C1B1 110.53(18) . . ?
C1B2 C1A C1B1 111.07(17) . . ?
N1 C1A C1 110.74(15) . . ?
C1B2 C1A C1 106.39(17) . . ?
C1B1 C1A C1 109.98(17) . . ?
O1 C1 N2 122.60(19) . . ?
O1 C1 C1A 119.68(17) . . ?
N2 C1 C1A 117.71(16) . . ?
C1 N2 C2A 123.02(17) . . ?
N2 C2A C2B1 110.60(19) . . ?
N2 C2A C2B2 106.75(19) . . ?
C2B1 C2A C2B2 111.5(2) . . ?
N2 C2A C2 109.47(17) . . ?
C2B1 C2A C2 110.6(2) . . ?
C2B2 C2A C2 107.84(19) . . ?
O2 C2 N3 123.1(2) . . ?
O2 C2 C2A 119.8(2) . . ?
N3 C2 C2A 116.88(18) . . ?
C2 N3 C31 123.83(18) . . ?
N3 C31 C32 111.33(18) . . ?
N4 C32 C31 110.91(19) . . ?
C33 N4 C32 123.95(19) . . ?
O3 C33 N4 124.5(2) . . ?
O3 C33 C34 122.2(2) . . ?
N4 C33 C34 113.34(18) . . ?
N9A C34 C33 112.66(17) . . ?
C35 N1A C38 119.48(18) . . ?
N3A C35 N1A 128.5(2) . . ?
C35 N3A C36 110.87(18) . . ?
N3A C36 N9A 127.64(19) . . ?
N3A C36 C37 126.84(18) . . ?
N9A C36 C37 105.51(18) . . ?
C36 C37 N7A 110.62(17) . . ?
C36 C37 C38 117.28(19) . . ?
N7A C37 C38 132.10(19) . . ?
N6A C38 N1A 119.18(18) . . ?
N6A C38 C37 123.8(2) . . ?
N1A C38 C37 116.97(18) . . ?
C39 N7A C37 104.02(19) . . ?
N7A C39 N9A 113.7(2) . . ?
C39 N9A C36 106.11(17) . . ?
C39 N9A C34 126.75(19) . . ?
C36 N9A C34 127.1(2) . . ?

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
C6T N1T C2T O2T -174.5(2) . . . . ?
C01 N1T C2T O2T -2.6(3) . . . . ?
C6T N1T C2T N3T 5.5(3) . . . . ?
C01 N1T C2T N3T 177.41(17) . . . . ?
O2T C2T N3T C4T 173.4(2) . . . . ?
N1T C2T N3T C4T -6.6(3) . . . . ?
C2T N3T C4T O4T -174.9(2) . . . . ?
C2T N3T C4T C5T 5.2(3) . . . . ?
O4T C4T C5T C6T 177.45(19) . . . . ?
N3T C4T C5T C6T -2.6(3) . . . . ?
O4T C4T C5T C7T -2.1(3) . . . . ?
N3T C4T C5T C7T 177.90(18) . . . . ?
C4T C5T C6T N1T 2.1(3) . . . . ?
C7T C5T C6T N1T -178.38(19) . . . . ?
C2T N1T C6T C5T -3.7(3) . . . . ?
C01 N1T C6T C5T -175.28(18) . . . . ?
C2T N1T C01 C0 -72.2(2) . . . . ?
C6T N1T C01 C0 99.7(2) . . . . ?
N1T C01 C0 O0 -35.1(3) . . . . ?
N1T C01 C0 N1 145.67(19) . . . . ?
O0 C0 N1 C1A -7.1(3) . . . . ?
C01 C0 N1 C1A 172.11(18) . . . . ?
C0 N1 C1A C1B2 174.12(19) . . . . ?
C0 N1 C1A C1B1 -64.2(2) . . . . ?
C0 N1 C1A C1 58.0(2) . . . . ?
N1 C1A C1 O1 -154.58(17) . . . . ?
C1B2 C1A C1 O1 88.2(2) . . . . ?
C1B1 C1A C1 O1 -32.1(2) . . . . ?
N1 C1A C1 N2 27.0(2) . . . . ?
C1B2 C1A C1 N2 -90.2(2) . . . . ?
C1B1 C1A C1 N2 149.47(18) . . . . ?
O1 C1 N2 C2A 0.6(3) . . . . ?
C1A C1 N2 C2A 178.90(18) . . . . ?
C1 N2 C2A C2B1 -69.8(3) . . . . ?
C1 N2 C2A C2B2 168.7(2) . . . . ?
C1 N2 C2A C2 52.3(3) . . . . ?
N2 C2A C2 O2 -147.1(2) . . . . ?
C2B1 C2A C2 O2 -25.0(3) . . . . ?
C2B2 C2A C2 O2 97.2(3) . . . . ?
N2 C2A C2 N3 37.5(3) . . . . ?
C2B1 C2A C2 N3 159.6(2) . . . . ?
C2B2 C2A C2 N3 -78.2(3) . . . . ?
O2 C2 N3 C31 9.0(4) . . . . ?
C2A C2 N3 C31 -175.73(19) . . . . ?
C2 N3 C31 C32 108.9(2) . . . . ?
N3 C31 C32 N4 -57.3(2) . . . . ?
C31 C32 N4 C33 -84.9(3) . . . . ?
C32 N4 C33 O3 -14.6(4) . . . . ?
C32 N4 C33 C34 164.4(2) . . . . ?
O3 C33 C34 N9A -11.0(4) . . . . ?
N4 C33 C34 N9A 170.0(2) . . . . ?
C38 N1A C35 N3A -0.1(4) . . . . ?
N1A C35 N3A C36 -0.5(3) . . . . ?
C35 N3A C36 N9A -178.4(2) . . . . ?
C35 N3A C36 C37 0.0(3) . . . . ?
N3A C36 C37 N7A -179.35(19) . . . . ?
N9A C36 C37 N7A -0.7(2) . . . . ?
N3A C36 C37 C38 0.9(3) . . . . ?
N9A C36 C37 C38 179.59(17) . . . . ?
C35 N1A C38 N6A -178.3(2) . . . . ?
C35 N1A C38 C37 1.1(3) . . . . ?
C36 C37 C38 N6A 178.00(19) . . . . ?
N7A C37 C38 N6A -1.7(4) . . . . ?
C36 C37 C38 N1A -1.4(3) . . . . ?
N7A C37 C38 N1A 178.9(2) . . . . ?
C36 C37 N7A C39 0.2(2) . . . . ?
C38 C37 N7A C39 179.9(2) . . . . ?
C37 N7A C39 N9A 0.4(2) . . . . ?
N7A C39 N9A C36 -0.9(3) . . . . ?
N7A C39 N9A C34 179.8(2) . . . . ?
N3A C36 N9A C39 179.6(2) . . . . ?
C37 C36 N9A C39 0.9(2) . . . . ?
N3A C36 N9A C34 -1.1(3) . . . . ?
C37 C36 N9A C34 -179.77(19) . . . . ?
C33 C34 N9A C39 74.5(3) . . . . ?
C33 C34 N9A C36 -104.7(2) . . . . ?

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
N3 H3 O0 0.86 2.28 3.050(2) 148.4 .
N4 H4 O1 0.86 2.19 2.857(2) 134.0 .
N3T H3T N1A 0.86 2.02 2.884(2) 178.0 4_466
N6A H6A1 O4T 0.84 2.12 2.949(2) 168.8 4_665
N2 H2 O3 0.86 2.57 3.014(3) 112.9 1_455
N1 H1 O1W 0.86 2.13 2.980(2) 172.2 .
N6A H6A2 O4W 0.90 2.56 3.389(4) 155.1 .
O4W H4WA N7A 0.95 1.88 2.791(3) 159.2 .
O2W H2WA O2 0.75 2.10 2.829(3) 165.6 .
O3W H3WA O2 0.94 1.89 2.824(3) 173.7 .
O2W H2WB N3A 0.93 2.07 2.980(3) 164.9 4_566
O1W H1WA O2W 0.87 1.94 2.808(3) 171.3 4_465
O1W H1WB O4W 0.85 2.00 2.821(4) 164.1 2
O3W H3WB O5W 0.95 1.89 2.778(5) 155.3 .
O4W H4WB O5W 0.82 1.98 2.807(6) 179.8 1_655
O5W H5WA O7W 0.84 1.88 2.711(12) 170.4 .
O6W H6WB O3W 0.84 2.01 2.850(8) 178.1 .
O6W H6WA O1W 0.84 1.95 2.789(7) 177.8 4_666

_refine_diff_density_max         0.549
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.049


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol - water'
####################################################################### 
# 
# 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_mc258d
_database_code_depnum_ccdc_archive 'CCDC 1535891'
_audit_update_record             
;
2017-03-03 deposited with the CCDC.
2017-05-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H40 N6 O7, C2 H6 O'
_chemical_formula_sum            'C31 H46 N6 O8'
_chemical_formula_weight         630.74

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   10.7942(5)
_cell_length_b                   18.8139(6)
_cell_length_c                   16.8871(8)
_cell_angle_alpha                90
_cell_angle_beta                 98.486(4)
_cell_angle_gamma                90
_cell_volume                     3391.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8152
_cell_measurement_theta_min      4.560
_cell_measurement_theta_max      72.115

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_F_000             1352
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    0.741
_shelx_estimated_absorpt_T_min   0.708
_shelx_estimated_absorpt_T_max   0.836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.48756
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Enhance (Cu) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1274
_diffrn_reflns_number            27911
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.538
_diffrn_reflns_theta_max         72.983
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6691
_reflns_number_gt                5033
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_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    'SIR2014 (Burla et al., 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 The phenyl ring of the benzyloxycarbonyl group was
 constrained to the idealized geometry.
 The CH3 group of the cocrystallized ethanol molecule
 was refined on two positions (atoms C2E and C2E') with
 population parameters of 0.65 and 0.35, respectively.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0973P)²+1.3063P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6691
_refine_ls_number_parameters     408
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0614
_refine_ls_wR_factor_ref         0.1939
_refine_ls_wR_factor_gt          0.1748
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.003
_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
C01 C 0.62518(19) -0.02504(10) 0.33581(10) 0.0666(7) Uani 1 1 d G . . . .
C02 C 0.5895(2) 0.01670(10) 0.26838(12) 0.0862(9) Uani 1 1 d G . . . .
H02 H 0.5341 0.0543 0.2705 0.103 Uiso 1 1 calc R U . . .
C03 C 0.6367(3) 0.00229(13) 0.19781(11) 0.1007(11) Uani 1 1 d G . . . .
H03 H 0.6128 0.0302 0.1527 0.121 Uiso 1 1 calc R U . . .
C04 C 0.7195(2) -0.05387(15) 0.19467(13) 0.1104(13) Uani 1 1 d G . . . .
H04 H 0.7511 -0.0635 0.1475 0.132 Uiso 1 1 calc R U . . .
C05 C 0.7552(2) -0.09561(12) 0.26210(16) 0.1187(15) Uani 1 1 d G . . . .
H05 H 0.8106 -0.1332 0.2600 0.142 Uiso 1 1 calc R U . . .
C06 C 0.7080(2) -0.08119(10) 0.33267(13) 0.0976(11) Uani 1 1 d G . . . .
H06 H 0.7318 -0.1091 0.3778 0.117 Uiso 1 1 calc R U . . .
C07 C 0.5742(3) -0.01113(14) 0.41309(19) 0.0729(7) Uani 1 1 d . . . . .
H07A H 0.5066 -0.0442 0.4173 0.087 Uiso 1 1 calc R U . . .
H07B H 0.6399 -0.0199 0.4578 0.087 Uiso 1 1 calc R U . . .
OU O 0.52869(16) 0.06014(10) 0.41873(12) 0.0676(5) Uani 1 1 d . . . . .
C0 C 0.6188(2) 0.11051(13) 0.43471(14) 0.0563(5) Uani 1 1 d . . . . .
O0 O 0.72908(17) 0.09678(10) 0.45383(11) 0.0652(4) Uani 1 1 d . . . . .
N1 N 0.57026(19) 0.17582(11) 0.42632(13) 0.0590(5) Uani 1 1 d . . . . .
H1 H 0.4906 0.1812 0.4143 0.071 Uiso 1 1 calc R U . . .
C1A C 0.6518(2) 0.23837(13) 0.43740(14) 0.0562(5) Uani 1 1 d . . . . .
C1B1 C 0.5697(3) 0.30444(15) 0.43302(18) 0.0724(7) Uani 1 1 d . . . . .
H1B1 H 0.5234 0.3087 0.3802 0.109 Uiso 1 1 calc R U . . .
H1B2 H 0.6214 0.3457 0.4449 0.109 Uiso 1 1 calc R U . . .
H1B3 H 0.5124 0.3006 0.4713 0.109 Uiso 1 1 calc R U . . .
C1B2 C 0.7335(3) 0.24061(16) 0.37107(16) 0.0693(7) Uani 1 1 d . . . . .
H1B4 H 0.7878 0.1999 0.3755 0.104 Uiso 1 1 calc R U . . .
H1B5 H 0.7830 0.2832 0.3761 0.104 Uiso 1 1 calc R U . . .
H1B6 H 0.6811 0.2401 0.3199 0.104 Uiso 1 1 calc R U . . .
C1 C 0.7249(2) 0.23489(11) 0.52324(14) 0.0522(5) Uani 1 1 d . . . . .
O1 O 0.67025(16) 0.21947(10) 0.57978(10) 0.0660(5) Uani 1 1 d . . . . .
N2 N 0.84649(18) 0.24980(10) 0.53350(12) 0.0542(5) Uani 1 1 d . . . . .
H2 H 0.8816 0.2583 0.4920 0.065 Uiso 1 1 calc R U . . .
C2A C 0.9239(2) 0.25247(12) 0.61307(14) 0.0567(6) Uani 1 1 d . . . . .
C2B1 C 0.8835(4) 0.31398(14) 0.66301(19) 0.0830(9) Uani 1 1 d . . . . .
H2B1 H 0.8902 0.3580 0.6352 0.125 Uiso 1 1 calc R U . . .
H2B2 H 0.9367 0.3155 0.7138 0.125 Uiso 1 1 calc R U . . .
H2B3 H 0.7983 0.3070 0.6713 0.125 Uiso 1 1 calc R U . . .
C2B2 C 1.0588(3) 0.2622(2) 0.5998(2) 0.0908(11) Uani 1 1 d . . . . .
H2B4 H 1.0817 0.2245 0.5665 0.136 Uiso 1 1 calc R U . . .
H2B5 H 1.1126 0.2613 0.6504 0.136 Uiso 1 1 calc R U . . .
H2B6 H 1.0675 0.3070 0.5740 0.136 Uiso 1 1 calc R U . . .
C2 C 0.9187(2) 0.18155(11) 0.65897(13) 0.0490(5) Uani 1 1 d . . . . .
O2 O 0.94083(17) 0.18132(9) 0.73175(10) 0.0613(4) Uani 1 1 d . . . . .
N3 N 0.9013(2) 0.12301(10) 0.61480(12) 0.0572(5) Uani 1 1 d . . . . .
H3 H 0.8887 0.1272 0.5635 0.069 Uiso 1 1 calc R U . . .
C31 C 0.9025(2) 0.05187(11) 0.64934(14) 0.0542(5) Uani 1 1 d . . . . .
H31 H 0.9533 0.0527 0.7025 0.065 Uiso 1 1 calc R U . . .
C32 C 0.9622(3) 0.00148(14) 0.59632(19) 0.0706(7) Uani 1 1 d . . . . .
H32A H 1.0471 0.0169 0.5934 0.085 Uiso 1 1 calc R U . . .
H32B H 0.9156 0.0027 0.5426 0.085 Uiso 1 1 calc R U . . .
C33 C 0.9648(3) -0.07467(14) 0.6281(2) 0.0763(8) Uani 1 1 d . . . . .
H33A H 0.9986 -0.1060 0.5910 0.092 Uiso 1 1 calc R U . . .
H33B H 1.0194 -0.0770 0.6791 0.092 Uiso 1 1 calc R U . . .
C34 C 0.8355(3) -0.09979(12) 0.63883(15) 0.0620(6) Uani 1 1 d . . . . .
H34 H 0.7840 -0.1016 0.5859 0.074 Uiso 1 1 calc R U . . .
C35 C 0.7741(3) -0.04922(13) 0.69051(17) 0.0640(6) Uani 1 1 d . . . . .
H35A H 0.8196 -0.0499 0.7445 0.077 Uiso 1 1 calc R U . . .
H35B H 0.6890 -0.0648 0.6928 0.077 Uiso 1 1 calc R U . . .
C36 C 0.7718(2) 0.02667(13) 0.65775(16) 0.0598(6) Uani 1 1 d . . . . .
H36A H 0.7194 0.0283 0.6059 0.072 Uiso 1 1 calc R U . . .
H36B H 0.7357 0.0582 0.6936 0.072 Uiso 1 1 calc R U . . .
N4 N 0.8426(2) -0.17149(10) 0.67231(14) 0.0696(6) Uani 1 1 d . . . . .
H4 H 0.8863 -0.1776 0.7187 0.084 Uiso 1 1 calc R U . . .
C37 C 0.7867(2) -0.22744(12) 0.63636(16) 0.0573(6) Uani 1 1 d . . . . .
O4 O 0.7161(2) -0.22605(10) 0.57285(14) 0.0797(6) Uani 1 1 d . . . . .
C38 C 0.8130(3) -0.29589(12) 0.68458(16) 0.0622(6) Uani 1 1 d . . . . .
H38A H 0.8928 -0.2916 0.7191 0.075 Uiso 1 1 calc R U . . .
H38B H 0.7487 -0.3024 0.7184 0.075 Uiso 1 1 calc R U . . .
N1T N 0.81590(19) -0.35823(9) 0.63346(12) 0.0558(5) Uani 1 1 d . . . . .
C39 C 0.9168(2) -0.36443(12) 0.59225(15) 0.0554(5) Uani 1 1 d . . . . .
O2T O 0.99495(18) -0.31819(9) 0.59237(12) 0.0695(5) Uani 1 1 d . . . . .
N3T N 0.92107(19) -0.42739(10) 0.55164(13) 0.0578(5) Uani 1 1 d . . . . .
H3T H 0.9829 -0.4328 0.5254 0.069 Uiso 1 1 calc R U . . .
C40 C 0.8375(2) -0.48261(12) 0.54830(14) 0.0547(5) Uani 1 1 d . . . . .
O4T O 0.85626(18) -0.53801(9) 0.51321(12) 0.0712(5) Uani 1 1 d . . . . .
C41 C 0.7296(2) -0.47054(11) 0.58843(14) 0.0520(5) Uani 1 1 d . . . . .
C42 C 0.7256(2) -0.40954(11) 0.62914(14) 0.0524(5) Uani 1 1 d . . . . .
H42 H 0.6575 -0.4017 0.6559 0.063 Uiso 1 1 calc R U . . .
C43 C 0.6304(3) -0.52656(14) 0.58293(18) 0.0663(6) Uani 1 1 d . . . . .
H43A H 0.5629 -0.5104 0.6095 0.099 Uiso 1 1 calc R U . . .
H43B H 0.6652 -0.5693 0.6081 0.099 Uiso 1 1 calc R U . . .
H43C H 0.5995 -0.5360 0.5277 0.099 Uiso 1 1 calc R U . . .
O1E O 0.5242(3) 0.30041(17) 0.66799(16) 0.1122(9) Uani 1 1 d . . . . .
H1OE H 0.5587 0.2718 0.6418 0.168 Uiso 1 1 calc R U . . .
C1E C 0.3955(4) 0.2982(3) 0.6435(4) 0.1312(17) Uani 1 1 d . . . . .
H1E1 H 0.3534 0.2894 0.6895 0.157 Uiso 0.65 1 calc R U P A 1
H1E2 H 0.3756 0.2592 0.6061 0.157 Uiso 0.65 1 calc R U P A 1
H1E3 H 0.3590 0.2584 0.6684 0.157 Uiso 0.35 1 calc R U P B 2
H1E4 H 0.3773 0.2927 0.5858 0.157 Uiso 0.35 1 calc R U P B 2
C2E C 0.3505(6) 0.3638(4) 0.6059(6) 0.113(2) Uani 0.65 1 d . . P C 1
H2E1 H 0.3988 0.4027 0.6309 0.169 Uiso 0.65 1 calc R U P C 1
H2E2 H 0.2640 0.3702 0.6115 0.169 Uiso 0.65 1 calc R U P C 1
H2E3 H 0.3586 0.3622 0.5500 0.169 Uiso 0.65 1 calc R U P C 1
C2E' C 0.3445(13) 0.3642(9) 0.6677(12) 0.126(5) Uani 0.35 1 d . . P C 2
H2E4 H 0.3561 0.3670 0.7251 0.189 Uiso 0.35 1 calc R U P C 2
H2E5 H 0.2567 0.3664 0.6474 0.189 Uiso 0.35 1 calc R U P C 2
H2E6 H 0.3868 0.4033 0.6467 0.189 Uiso 0.35 1 calc R U P C 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
C01 C02 1.3900 . ?
C01 C06 1.3900 . ?
C01 C07 1.512(3) . ?
C02 C03 1.3900 . ?
C03 C04 1.3900 . ?
C04 C05 1.3900 . ?
C05 C06 1.3900 . ?
C07 OU 1.436(3) . ?
OU C0 1.357(3) . ?
C0 O0 1.214(3) . ?
C0 N1 1.335(3) . ?
N1 C1A 1.465(3) . ?
C1A C1B1 1.522(4) . ?
C1A C1B2 1.525(4) . ?
C1A C1 1.546(3) . ?
C1 O1 1.229(3) . ?
C1 N2 1.328(3) . ?
N2 C2A 1.475(3) . ?
C2A C2B2 1.518(4) . ?
C2A C2B1 1.532(4) . ?
C2A C2 1.548(3) . ?
C2 O2 1.217(3) . ?
C2 N3 1.328(3) . ?
N3 C31 1.459(3) . ?
C31 C32 1.512(3) . ?
C31 C36 1.515(3) . ?
C32 C33 1.529(4) . ?
C33 C34 1.509(4) . ?
C34 N4 1.460(3) . ?
C34 C35 1.509(4) . ?
C35 C36 1.530(3) . ?
N4 C37 1.316(3) . ?
C37 O4 1.221(3) . ?
C37 C38 1.528(3) . ?
C38 N1T 1.459(3) . ?
N1T C42 1.366(3) . ?
N1T C39 1.381(3) . ?
C39 O2T 1.212(3) . ?
C39 N3T 1.373(3) . ?
N3T C40 1.371(3) . ?
C40 O4T 1.230(3) . ?
C40 C41 1.449(3) . ?
C41 C42 1.342(3) . ?
C41 C43 1.495(3) . ?
O1E C1E 1.391(5) . ?
C1E C2E 1.440(8) . ?
C1E C2E' 1.443(15) . ?

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
C02 C01 C06 120.0 . . ?
C02 C01 C07 121.16(17) . . ?
C06 C01 C07 118.84(17) . . ?
C01 C02 C03 120.0 . . ?
C04 C03 C02 120.0 . . ?
C03 C04 C05 120.0 . . ?
C04 C05 C06 120.0 . . ?
C05 C06 C01 120.0 . . ?
OU C07 C01 113.0(2) . . ?
C0 OU C07 115.0(2) . . ?
O0 C0 N1 125.3(2) . . ?
O0 C0 OU 123.4(2) . . ?
N1 C0 OU 111.3(2) . . ?
C0 N1 C1A 120.4(2) . . ?
N1 C1A C1B1 108.3(2) . . ?
N1 C1A C1B2 109.3(2) . . ?
C1B1 C1A C1B2 109.7(2) . . ?
N1 C1A C1 107.44(18) . . ?
C1B1 C1A C1 107.0(2) . . ?
C1B2 C1A C1 114.8(2) . . ?
O1 C1 N2 121.8(2) . . ?
O1 C1 C1A 120.1(2) . . ?
N2 C1 C1A 118.1(2) . . ?
C1 N2 C2A 122.8(2) . . ?
N2 C2A C2B2 107.2(2) . . ?
N2 C2A C2B1 111.0(2) . . ?
C2B2 C2A C2B1 110.3(3) . . ?
N2 C2A C2 111.68(18) . . ?
C2B2 C2A C2 106.5(2) . . ?
C2B1 C2A C2 109.9(2) . . ?
O2 C2 N3 123.7(2) . . ?
O2 C2 C2A 119.5(2) . . ?
N3 C2 C2A 116.50(19) . . ?
C2 N3 C31 122.96(19) . . ?
N3 C31 C32 108.5(2) . . ?
N3 C31 C36 111.8(2) . . ?
C32 C31 C36 110.1(2) . . ?
C31 C32 C33 111.5(2) . . ?
C34 C33 C32 111.5(2) . . ?
N4 C34 C35 111.2(2) . . ?
N4 C34 C33 109.8(2) . . ?
C35 C34 C33 111.4(2) . . ?
C34 C35 C36 111.4(2) . . ?
C31 C36 C35 111.1(2) . . ?
C37 N4 C34 124.5(2) . . ?
O4 C37 N4 124.9(2) . . ?
O4 C37 C38 121.9(2) . . ?
N4 C37 C38 113.1(2) . . ?
N1T C38 C37 112.4(2) . . ?
C42 N1T C39 121.53(19) . . ?
C42 N1T C38 121.45(19) . . ?
C39 N1T C38 117.0(2) . . ?
O2T C39 N3T 123.1(2) . . ?
O2T C39 N1T 122.6(2) . . ?
N3T C39 N1T 114.31(19) . . ?
C40 N3T C39 127.14(19) . . ?
O4T C40 N3T 120.5(2) . . ?
O4T C40 C41 124.0(2) . . ?
N3T C40 C41 115.5(2) . . ?
C42 C41 C40 117.6(2) . . ?
C42 C41 C43 123.9(2) . . ?
C40 C41 C43 118.5(2) . . ?
C41 C42 N1T 123.7(2) . . ?
O1E C1E C2E 111.2(4) . . ?
O1E C1E C2E' 107.2(7) . . ?

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
C06 C01 C02 C03 0.0 . . . . ?
C07 C01 C02 C03 -179.3(2) . . . . ?
C01 C02 C03 C04 0.0 . . . . ?
C02 C03 C04 C05 0.0 . . . . ?
C03 C04 C05 C06 0.0 . . . . ?
C04 C05 C06 C01 0.0 . . . . ?
C02 C01 C06 C05 0.0 . . . . ?
C07 C01 C06 C05 179.3(2) . . . . ?
C02 C01 C07 OU -21.8(3) . . . . ?
C06 C01 C07 OU 158.87(18) . . . . ?
C01 C07 OU C0 -75.1(3) . . . . ?
C07 OU C0 O0 -9.8(3) . . . . ?
C07 OU C0 N1 170.0(2) . . . . ?
O0 C0 N1 C1A 2.4(4) . . . . ?
OU C0 N1 C1A -177.4(2) . . . . ?
C0 N1 C1A C1B1 -174.0(2) . . . . ?
C0 N1 C1A C1B2 66.5(3) . . . . ?
C0 N1 C1A C1 -58.6(3) . . . . ?
N1 C1A C1 O1 -44.5(3) . . . . ?
C1B1 C1A C1 O1 71.7(3) . . . . ?
C1B2 C1A C1 O1 -166.2(2) . . . . ?
N1 C1A C1 N2 136.3(2) . . . . ?
C1B1 C1A C1 N2 -107.5(2) . . . . ?
C1B2 C1A C1 N2 14.6(3) . . . . ?
O1 C1 N2 C2A -3.0(3) . . . . ?
C1A C1 N2 C2A 176.1(2) . . . . ?
C1 N2 C2A C2B2 173.4(2) . . . . ?
C1 N2 C2A C2B1 -66.0(3) . . . . ?
C1 N2 C2A C2 57.0(3) . . . . ?
N2 C2A C2 O2 -156.0(2) . . . . ?
C2B2 C2A C2 O2 87.3(3) . . . . ?
C2B1 C2A C2 O2 -32.3(3) . . . . ?
N2 C2A C2 N3 30.1(3) . . . . ?
C2B2 C2A C2 N3 -86.6(3) . . . . ?
C2B1 C2A C2 N3 153.8(2) . . . . ?
O2 C2 N3 C31 2.2(4) . . . . ?
C2A C2 N3 C31 175.8(2) . . . . ?
C2 N3 C31 C32 -143.8(2) . . . . ?
C2 N3 C31 C36 94.5(3) . . . . ?
N3 C31 C32 C33 -179.0(2) . . . . ?
C36 C31 C32 C33 -56.4(3) . . . . ?
C31 C32 C33 C34 55.4(3) . . . . ?
C32 C33 C34 N4 -177.7(2) . . . . ?
C32 C33 C34 C35 -54.1(3) . . . . ?
N4 C34 C35 C36 177.4(2) . . . . ?
C33 C34 C35 C36 54.6(3) . . . . ?
N3 C31 C36 C35 177.5(2) . . . . ?
C32 C31 C36 C35 56.7(3) . . . . ?
C34 C35 C36 C31 -56.2(3) . . . . ?
C35 C34 N4 C37 117.6(3) . . . . ?
C33 C34 N4 C37 -118.7(3) . . . . ?
C34 N4 C37 O4 -4.6(5) . . . . ?
C34 N4 C37 C38 178.7(2) . . . . ?
O4 C37 C38 N1T 35.6(4) . . . . ?
N4 C37 C38 N1T -147.6(2) . . . . ?
C37 C38 N1T C42 -111.9(3) . . . . ?
C37 C38 N1T C39 70.7(3) . . . . ?
C42 N1T C39 O2T 176.6(2) . . . . ?
C38 N1T C39 O2T -6.0(4) . . . . ?
C42 N1T C39 N3T -3.7(3) . . . . ?
C38 N1T C39 N3T 173.8(2) . . . . ?
O2T C39 N3T C40 179.7(3) . . . . ?
N1T C39 N3T C40 0.0(4) . . . . ?
C39 N3T C40 O4T -175.8(2) . . . . ?
C39 N3T C40 C41 4.0(4) . . . . ?
O4T C40 C41 C42 175.4(2) . . . . ?
N3T C40 C41 C42 -4.4(3) . . . . ?
O4T C40 C41 C43 -4.0(4) . . . . ?
N3T C40 C41 C43 176.2(2) . . . . ?
C40 C41 C42 N1T 1.2(4) . . . . ?
C43 C41 C42 N1T -179.4(2) . . . . ?
C39 N1T C42 C41 3.1(4) . . . . ?
C38 N1T C42 C41 -174.2(2) . . . . ?

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
N3 H3 O0 0.86 2.41 3.098(3) 137.9 .
N1 H1 O4 0.86 2.42 3.234(3) 157.1 3_656
C1B2 H1B5 O2T 0.96 2.47 3.251(3) 138.8 3_756
N2 H2 O2T 0.86 2.37 3.190(3) 158.6 3_756
N3T H3T O4T 0.86 2.02 2.860(3) 165.6 3_746
O1E H1OE O1 0.82 1.97 2.778(3) 167.3 .
N4 H4 O1E 0.86 2.05 2.911(3) 173.8 2_646

_refine_diff_density_max         0.612
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.043


#===END===

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: ethanol'
