# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_2a
_database_code_depnum_ccdc_archive 'CCDC 1455739'
_audit_update_record             
;
2016-06-13 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT026_2a                  
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low .. 27 %
RESPONSE: This low value is due to the overall poor diffraction quality
of the crystal.
;
_vrf_PLAT412_2a                  
;
PROBLEM: Short Intra XH3 .. XHn H34A .. H33D .. 1.63 Ang.
RESPONSE: These are due to the disorder of the ethyl acetate molecule (C33).
;
# end Validation Reply Form 

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H56 N8 O8'
_chemical_formula_weight         728.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   11.231(2)
_cell_length_b                   13.224(3)
_cell_length_c                   13.496(3)
_cell_angle_alpha                86.976(6)
_cell_angle_beta                 88.508(6)
_cell_angle_gamma                85.740(6)
_cell_volume                     1995.6(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    23895
_cell_measurement_theta_min      1.511
_cell_measurement_theta_max      25.000

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_F_000             784
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.286
_exptl_crystal_size_min          0.219
_exptl_absorpt_coefficient_mu    0.087
_shelx_estimated_absorpt_T_min   0.966
_shelx_estimated_absorpt_T_max   0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.971
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Brucker CCD APEX 2'
_diffrn_measurement_method       hemisphere
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29256
_diffrn_reflns_av_unetI/netI     0.2554
_diffrn_reflns_av_R_equivalents  0.1229
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.511
_diffrn_reflns_theta_max         31.444
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.824
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.824
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.824
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             10905
_reflns_number_gt                2918
_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       APEX2
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    sir92
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    diamond3.2
_computing_publication_material  'CIFTAB (Sheldrick 2013)'

_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)+(0.0887P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10905
_refine_ls_number_parameters     514
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.3297
_refine_ls_R_factor_gt           0.0872
_refine_ls_wR_factor_ref         0.2528
_refine_ls_wR_factor_gt          0.1637
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_restrained_S_all      0.941
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
N1 N 0.4975(3) 0.6728(3) 0.7183(3) 0.0565(10) Uani 1 1 d . . . . .
H1N H 0.538(4) 0.661(3) 0.776(3) 0.068 Uiso 1 1 d . U . . .
N2 N 0.4704(3) 0.4379(3) 0.7438(3) 0.0562(10) Uani 1 1 d . . . . .
H2N H 0.538(4) 0.459(3) 0.788(3) 0.084 Uiso 1 1 d . U . . .
N3 N 0.5801(3) 0.2602(3) 0.9007(2) 0.0486(9) Uani 1 1 d . . . . .
H3N H 0.543(3) 0.296(3) 0.949(3) 0.058 Uiso 1 1 d . U . . .
N4 N 0.8551(3) 0.3347(3) 0.9212(3) 0.0543(10) Uani 1 1 d . . . . .
H4N H 0.790(4) 0.370(3) 0.915(3) 0.065 Uiso 1 1 d . U . . .
N5 N 0.9626(3) 0.4893(3) 0.7415(2) 0.0518(10) Uani 1 1 d . . . . .
H5N H 1.024(4) 0.453(3) 0.716(3) 0.078 Uiso 1 1 d . U . . .
N6 N 0.7893(3) 0.7039(3) 0.6718(3) 0.0513(9) Uani 1 1 d . . . . .
H6N H 0.783(3) 0.686(3) 0.606(3) 0.062 Uiso 1 1 d . U . . .
C1 C 0.7294(5) 0.9583(4) 0.5712(4) 0.0921(17) Uani 1 1 d . . . . .
H1A H 0.6896 1.0157 0.6020 0.138 Uiso 1 1 calc R U . . .
H1B H 0.7574 0.9788 0.5059 0.138 Uiso 1 1 calc R U . . .
H1C H 0.7959 0.9321 0.6104 0.138 Uiso 1 1 calc R U . . .
C2 C 0.6427(4) 0.8763(3) 0.5637(3) 0.0656(13) Uani 1 1 d . . . . .
H2A H 0.6792 0.8240 0.5226 0.079 Uiso 1 1 calc R U . . .
H2B H 0.5717 0.9058 0.5307 0.079 Uiso 1 1 calc R U . . .
C3 C 0.6047(4) 0.8260(3) 0.6650(3) 0.0507(11) Uani 1 1 d . . . . .
C4 C 0.5455(4) 0.9059(3) 0.7325(3) 0.0632(13) Uani 1 1 d . . . . .
H4A H 0.5225 0.8722 0.7950 0.076 Uiso 1 1 calc R U . . .
H4B H 0.6039 0.9533 0.7468 0.076 Uiso 1 1 calc R U . . .
C5 C 0.4359(5) 0.9655(4) 0.6897(4) 0.0836(16) Uani 1 1 d . . . . .
H5A H 0.4587 1.0038 0.6307 0.125 Uiso 1 1 calc R U . . .
H5B H 0.4018 1.0110 0.7376 0.125 Uiso 1 1 calc R U . . .
H5C H 0.3781 0.9193 0.6736 0.125 Uiso 1 1 calc R U . . .
C6 C 0.5175(4) 0.7475(3) 0.6470(3) 0.0514(11) Uani 1 1 d . . . . .
C7 C 0.4427(4) 0.7366(4) 0.5724(3) 0.0661(13) Uani 1 1 d . . . . .
H7 H 0.4366 0.7778 0.5145 0.079 Uiso 1 1 calc R U . . .
C8 C 0.3754(4) 0.6529(4) 0.5962(3) 0.0683(14) Uani 1 1 d . . . . .
H8 H 0.3179 0.6284 0.5572 0.082 Uiso 1 1 calc R U . . .
C9 C 0.4101(4) 0.6143(3) 0.6874(3) 0.0596(12) Uani 1 1 d . . . . .
C10 C 0.3751(4) 0.5224(3) 0.7452(3) 0.0631(13) Uani 1 1 d . . . . .
H10A H 0.3030 0.5000 0.7179 0.076 Uiso 1 1 calc R U . . .
H10B H 0.3574 0.5393 0.8133 0.076 Uiso 1 1 calc R U . . .
C11 C 0.5295(4) 0.4234(4) 0.6449(3) 0.0730(14) Uani 1 1 d . . . . .
H11A H 0.4717 0.4060 0.5987 0.109 Uiso 1 1 calc R U . . .
H11B H 0.5917 0.3697 0.6507 0.109 Uiso 1 1 calc R U . . .
H11C H 0.5632 0.4852 0.6216 0.109 Uiso 1 1 calc R U . . .
C12 C 0.4233(4) 0.3385(3) 0.7879(3) 0.0555(12) Uani 1 1 d . . . . .
H12A H 0.3766 0.3522 0.8478 0.067 Uiso 1 1 calc R U . . .
H12B H 0.3714 0.3119 0.7408 0.067 Uiso 1 1 calc R U . . .
C13 C 0.5225(4) 0.2622(3) 0.8113(3) 0.0501(11) Uani 1 1 d . . . . .
C14 C 0.5829(4) 0.1914(3) 0.7559(3) 0.0663(13) Uani 1 1 d . . . . .
H14 H 0.5641 0.1757 0.6920 0.080 Uiso 1 1 calc R U . . .
C15 C 0.6782(4) 0.1461(3) 0.8113(3) 0.0634(13) Uani 1 1 d . . . . .
H15 H 0.7335 0.0951 0.7907 0.076 Uiso 1 1 calc R U . . .
C16 C 0.6758(4) 0.1901(3) 0.9011(3) 0.0468(11) Uani 1 1 d . . . . .
C17 C 0.7639(4) 0.1757(3) 0.9849(3) 0.0477(11) Uani 1 1 d . . . . .
C18 C 0.7079(4) 0.2191(3) 1.0818(3) 0.0539(11) Uani 1 1 d . . . . .
H18A H 0.6846 0.2907 1.0693 0.065 Uiso 1 1 calc R U . . .
H18B H 0.6360 0.1850 1.0990 0.065 Uiso 1 1 calc R U . . .
C19 C 0.7905(4) 0.2073(4) 1.1701(3) 0.0753(15) Uani 1 1 d . . . . .
H19A H 0.8128 0.1366 1.1840 0.113 Uiso 1 1 calc R U . . .
H19B H 0.7499 0.2353 1.2270 0.113 Uiso 1 1 calc R U . . .
H19C H 0.8608 0.2427 1.1547 0.113 Uiso 1 1 calc R U . . .
C20 C 0.8057(4) 0.0618(3) 0.9995(3) 0.0635(13) Uani 1 1 d . . . . .
H20A H 0.8434 0.0391 0.9383 0.076 Uiso 1 1 calc R U . . .
H20B H 0.8655 0.0540 1.0505 0.076 Uiso 1 1 calc R U . . .
C21 C 0.7055(5) -0.0061(4) 1.0288(4) 0.0833(16) Uani 1 1 d . . . . .
H21A H 0.6780 0.0068 1.0952 0.125 Uiso 1 1 calc R U . . .
H21B H 0.7346 -0.0760 1.0257 0.125 Uiso 1 1 calc R U . . .
H21C H 0.6406 0.0082 0.9840 0.125 Uiso 1 1 calc R U . . .
C22 C 0.8696(4) 0.2351(3) 0.9527(3) 0.0467(11) Uani 1 1 d . . . . .
C23 C 0.9899(4) 0.2102(4) 0.9473(3) 0.0601(12) Uani 1 1 d . . . . .
H23 H 1.0275 0.1470 0.9649 0.072 Uiso 1 1 calc R U . . .
C24 C 1.0476(4) 0.2960(4) 0.9106(3) 0.0630(13) Uani 1 1 d . . . . .
H24 H 1.1293 0.2993 0.8998 0.076 Uiso 1 1 calc R U . . .
C25 C 0.9627(4) 0.3727(4) 0.8941(3) 0.0514(11) Uani 1 1 d . . . . .
C26 C 0.9694(4) 0.4786(4) 0.8534(3) 0.0609(12) Uani 1 1 d . . . . .
H26A H 1.0437 0.5037 0.8733 0.073 Uiso 1 1 calc R U . . .
H26B H 0.9044 0.5208 0.8820 0.073 Uiso 1 1 calc R U . . .
C27 C 0.8534(4) 0.4510(3) 0.7019(3) 0.0613(12) Uani 1 1 d . . . . .
H27A H 0.7841 0.4882 0.7284 0.092 Uiso 1 1 calc R U . . .
H27B H 0.8505 0.3802 0.7209 0.092 Uiso 1 1 calc R U . . .
H27C H 0.8548 0.4599 0.6308 0.092 Uiso 1 1 calc R U . . .
C28 C 0.9788(4) 0.5973(3) 0.7037(3) 0.0577(12) Uani 1 1 d . . . . .
H28A H 1.0536 0.6173 0.7280 0.069 Uiso 1 1 calc R U . . .
H28B H 0.9851 0.5988 0.6318 0.069 Uiso 1 1 calc R U . . .
C29 C 0.8825(4) 0.6728(3) 0.7326(3) 0.0511(11) Uani 1 1 d . . . . .
C30 C 0.8651(4) 0.7244(4) 0.8167(3) 0.0665(13) Uani 1 1 d . . . . .
H30 H 0.9143 0.7185 0.8714 0.080 Uiso 1 1 calc R U . . .
C31 C 0.7605(4) 0.7879(3) 0.8068(3) 0.0663(13) Uani 1 1 d . . . . .
H31 H 0.7279 0.8312 0.8542 0.080 Uiso 1 1 calc R U . . .
C32 C 0.7141(4) 0.7758(3) 0.7157(3) 0.0507(11) Uani 1 1 d . . . . .
N7 N 0.1722(4) 0.3889(4) 0.5772(3) 0.0726(12) Uani 1 1 d D U . . .
O1 O 0.2621(4) 0.3670(4) 0.5297(3) 0.1201(15) Uani 1 1 d . . . . .
O2 O 0.0747(8) 0.386(2) 0.5378(8) 0.111(5) Uani 0.63(4) 1 d D U P A 1
O2A O 0.105(4) 0.451(3) 0.5352(13) 0.146(12) Uani 0.37(4) 1 d D U P A 2
O3 O 0.1692(3) 0.3887(3) 0.6698(2) 0.0810(10) Uani 1 1 d . . . . .
N8 N 0.6300(4) 0.5499(3) 0.9431(3) 0.0606(10) Uani 1 1 d . . . . .
O4 O 0.6496(2) 0.4885(2) 0.8754(2) 0.0663(9) Uani 1 1 d . . . . .
O5 O 0.5417(3) 0.6120(3) 0.9367(2) 0.0807(10) Uani 1 1 d . . . . .
O6 O 0.6986(3) 0.5481(3) 1.0126(2) 0.0912(11) Uani 1 1 d . . . . .
C33 C 0.1365(13) 0.1123(13) 0.7128(8) 0.143(7) Uani 0.715(19) 1 d D U P B 1
H33A H 0.1477 0.1223 0.7818 0.215 Uiso 0.715(19) 1 calc R U P B 1
H33B H 0.1941 0.1477 0.6734 0.215 Uiso 0.715(19) 1 calc R U P B 1
H33C H 0.1467 0.0411 0.7013 0.215 Uiso 0.715(19) 1 calc R U P B 1
C33A C 0.041(4) 0.0526(16) 0.7350(17) 0.135(13) Uani 0.285(19) 1 d D U P B 2
H33D H 0.0524 0.0606 0.8044 0.202 Uiso 0.285(19) 1 calc R U P B 2
H33E H 0.1128 0.0203 0.7067 0.202 Uiso 0.285(19) 1 calc R U P B 2
H33F H -0.0242 0.0115 0.7269 0.202 Uiso 0.285(19) 1 calc R U P B 2
C34 C 0.0164(7) 0.1514(6) 0.6853(4) 0.133(3) Uani 1 1 d D U . . .
H34A H -0.0423 0.1169 0.7257 0.160 Uiso 1 1 calc R U . B 1
H34B H 0.0056 0.2234 0.6962 0.160 Uiso 1 1 calc R U . B 1
C35 C -0.0828(7) 0.1839(6) 0.5333(6) 0.111(2) Uani 1 1 d . . . . .
O8 O -0.1609(6) 0.2363(5) 0.5783(5) 0.185(3) Uani 1 1 d . . . . .
O7 O 0.0009(4) 0.1345(3) 0.5827(3) 0.1114(14) Uani 1 1 d . . . . .
C36 C -0.0871(5) 0.1638(5) 0.4293(4) 0.108(2) Uani 1 1 d . . . . .
H36A H -0.1563 0.2000 0.4008 0.162 Uiso 1 1 calc R U . . .
H36B H -0.0915 0.0922 0.4224 0.162 Uiso 1 1 calc R U . . .
H36C H -0.0165 0.1857 0.3956 0.162 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C6 1.368(5) . ?
N1 C9 1.380(5) . ?
N2 C10 1.490(5) . ?
N2 C11 1.490(5) . ?
N2 C12 1.537(5) . ?
N3 C16 1.367(5) . ?
N3 C13 1.382(5) . ?
N4 C22 1.362(5) . ?
N4 C25 1.377(5) . ?
N5 C27 1.484(5) . ?
N5 C26 1.513(5) . ?
N5 C28 1.513(5) . ?
N6 C32 1.372(5) . ?
N6 C29 1.373(5) . ?
C1 C2 1.519(6) . ?
C2 C3 1.553(5) . ?
C3 C6 1.512(6) . ?
C3 C32 1.514(6) . ?
C3 C4 1.535(5) . ?
C4 C5 1.521(6) . ?
C6 C7 1.349(5) . ?
C7 C8 1.405(6) . ?
C8 C9 1.362(6) . ?
C9 C10 1.482(6) . ?
C12 C13 1.476(5) . ?
C13 C14 1.360(5) . ?
C14 C15 1.401(6) . ?
C15 C16 1.371(5) . ?
C16 C17 1.517(5) . ?
C17 C22 1.513(5) . ?
C17 C20 1.549(6) . ?
C17 C18 1.556(5) . ?
C18 C19 1.523(5) . ?
C20 C21 1.523(6) . ?
C22 C23 1.368(5) . ?
C23 C24 1.409(6) . ?
C24 C25 1.353(6) . ?
C25 C26 1.484(6) . ?
C28 C29 1.475(6) . ?
C29 C30 1.358(5) . ?
C30 C31 1.398(6) . ?
C31 C32 1.370(5) . ?
N7 O2A 1.204(12) . ?
N7 O1 1.207(5) . ?
N7 O2 1.233(8) . ?
N7 O3 1.249(5) . ?
N8 O6 1.228(4) . ?
N8 O5 1.242(4) . ?
N8 O4 1.258(4) . ?
C33 C34 1.458(10) . ?
C33A C34 1.448(16) . ?
C34 O7 1.430(6) . ?
C35 O8 1.243(7) . ?
C35 O7 1.285(7) . ?
C35 C36 1.445(8) . ?

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
C6 N1 C9 109.4(4) . . ?
C10 N2 C11 114.5(3) . . ?
C10 N2 C12 110.8(3) . . ?
C11 N2 C12 111.4(3) . . ?
C16 N3 C13 110.3(3) . . ?
C22 N4 C25 111.4(4) . . ?
C27 N5 C26 113.8(3) . . ?
C27 N5 C28 111.5(3) . . ?
C26 N5 C28 111.2(3) . . ?
C32 N6 C29 110.6(4) . . ?
C1 C2 C3 114.4(4) . . ?
C6 C3 C32 109.9(3) . . ?
C6 C3 C4 109.5(4) . . ?
C32 C3 C4 108.7(3) . . ?
C6 C3 C2 108.9(3) . . ?
C32 C3 C2 109.3(3) . . ?
C4 C3 C2 110.5(3) . . ?
C5 C4 C3 114.7(4) . . ?
C7 C6 N1 107.2(4) . . ?
C7 C6 C3 132.6(4) . . ?
N1 C6 C3 120.1(4) . . ?
C6 C7 C8 109.0(4) . . ?
C9 C8 C7 107.0(4) . . ?
C8 C9 N1 107.4(4) . . ?
C8 C9 C10 130.1(5) . . ?
N1 C9 C10 122.3(4) . . ?
C9 C10 N2 112.3(4) . . ?
C13 C12 N2 111.0(3) . . ?
C14 C13 N3 106.5(4) . . ?
C14 C13 C12 132.1(4) . . ?
N3 C13 C12 121.1(4) . . ?
C13 C14 C15 108.5(4) . . ?
C16 C15 C14 108.0(4) . . ?
N3 C16 C15 106.7(4) . . ?
N3 C16 C17 123.3(4) . . ?
C15 C16 C17 129.7(4) . . ?
C22 C17 C16 106.5(3) . . ?
C22 C17 C20 109.3(3) . . ?
C16 C17 C20 109.5(3) . . ?
C22 C17 C18 108.9(3) . . ?
C16 C17 C18 110.7(3) . . ?
C20 C17 C18 111.8(3) . . ?
C19 C18 C17 114.1(3) . . ?
C21 C20 C17 113.9(4) . . ?
N4 C22 C23 105.5(4) . . ?
N4 C22 C17 121.4(4) . . ?
C23 C22 C17 133.1(4) . . ?
C22 C23 C24 108.8(4) . . ?
C25 C24 C23 107.8(4) . . ?
C24 C25 N4 106.5(4) . . ?
C24 C25 C26 132.1(5) . . ?
N4 C25 C26 121.4(4) . . ?
C25 C26 N5 113.6(4) . . ?
C29 C28 N5 115.1(3) . . ?
C30 C29 N6 106.8(4) . . ?
C30 C29 C28 130.7(4) . . ?
N6 C29 C28 122.5(4) . . ?
C29 C30 C31 108.1(4) . . ?
C32 C31 C30 108.6(4) . . ?
C31 C32 N6 105.9(4) . . ?
C31 C32 C3 131.5(4) . . ?
N6 C32 C3 122.6(4) . . ?
O2A N7 O1 113.6(13) . . ?
O1 N7 O2 118.8(7) . . ?
O2A N7 O3 115.9(11) . . ?
O1 N7 O3 122.9(5) . . ?
O2 N7 O3 115.6(6) . . ?
O6 N8 O5 121.6(4) . . ?
O6 N8 O4 119.8(4) . . ?
O5 N8 O4 118.6(4) . . ?
O7 C34 C33A 106.9(12) . . ?
O7 C34 C33 108.6(6) . . ?
O8 C35 O7 119.1(7) . . ?
O8 C35 C36 124.1(8) . . ?
O7 C35 C36 116.2(7) . . ?
C35 O7 C34 121.0(6) . . ?

_refine_diff_density_max         0.419
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.045

_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_2b
_database_code_depnum_ccdc_archive 'CCDC 1455740'
_audit_update_record             
;
2016-06-13 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H48 B2 F8 N6'
_chemical_formula_weight         714.40

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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                   11.3232(9)
_cell_length_b                   12.4132(10)
_cell_length_c                   12.8292(10)
_cell_angle_alpha                90
_cell_angle_beta                 98.879(2)
_cell_angle_gamma                90
_cell_volume                     1781.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    20299
_cell_measurement_theta_min      1.820
_cell_measurement_theta_max      25.000

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_F_000             752
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.343
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.085
_exptl_absorpt_coefficient_mu    0.108
_shelx_estimated_absorpt_T_min   0.964
_shelx_estimated_absorpt_T_max   0.991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.987
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Brucker CCD APEX 2'
_diffrn_measurement_method       hemisphere
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25832
_diffrn_reflns_av_unetI/netI     0.0901
_diffrn_reflns_av_R_equivalents  0.0700
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.820
_diffrn_reflns_theta_max         31.789
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             5614
_reflns_number_gt                2435
_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       APEX2
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    Diamond3.2
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'

_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)+(0.0767P)²+0.4642P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5614
_refine_ls_number_parameters     267
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1914
_refine_ls_R_factor_gt           0.0762
_refine_ls_wR_factor_ref         0.2011
_refine_ls_wR_factor_gt          0.1578
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
F1 F 0.06910(19) 0.94161(18) 0.59355(17) 0.1102(7) Uani 1 1 d D . . A 1
F2 F 0.2606(3) 0.9664(4) 0.6181(5) 0.1208(18) Uani 0.729(8) 1 d D . P A 1
F2A F 0.2293(16) 1.0102(8) 0.6927(14) 0.148(7) Uani 0.271(8) 1 d D . P A 2
F3 F 0.1956(5) 0.8110(3) 0.6646(4) 0.0960(16) Uani 0.729(8) 1 d D . P A 1
F3A F 0.2336(18) 0.8383(18) 0.6466(15) 0.194(10) Uani 0.271(8) 1 d D . P A 2
F4 F 0.1683(4) 0.9537(4) 0.7603(3) 0.1116(18) Uani 0.729(8) 1 d D . P A 1
F4A F 0.1238(16) 0.9045(15) 0.7545(12) 0.292(16) Uani 0.271(8) 1 d D . P A 2
B1 B 0.1746(3) 0.9178(3) 0.6617(3) 0.0623(8) Uani 1 1 d . . . . .
N1 N 0.19618(18) 1.06509(15) 0.34475(15) 0.0442(5) Uani 1 1 d . . . . .
H1N H 0.140(2) 1.0897(17) 0.3744(17) 0.036(6) Uiso 1 1 d . . . . .
N2 N 0.04636(16) 0.85157(16) 0.35392(14) 0.0429(5) Uani 1 1 d . . . . .
H2N H 0.028(2) 0.904(2) 0.401(2) 0.064(8) Uiso 1 1 d . . . . .
N3 N -0.20825(17) 0.80361(16) 0.44637(15) 0.0420(5) Uani 1 1 d . . . . .
H3N H -0.237(2) 0.861(2) 0.4206(18) 0.043(7) Uiso 1 1 d . . . . .
C1 C 0.3690(3) 1.0455(2) 0.2904(2) 0.0688(8) Uani 1 1 d . . . . .
H1 H 0.4475 1.0557 0.2794 0.083 Uiso 1 1 calc R U . . .
C2 C 0.2919(2) 0.9635(2) 0.2459(2) 0.0636(8) Uani 1 1 d . . . . .
H2 H 0.3106 0.9095 0.2008 0.076 Uiso 1 1 calc R U . . .
C3 C 0.1863(2) 0.97660(18) 0.27979(18) 0.0479(6) Uani 1 1 d . . . . .
C4 C 0.0759(2) 0.91070(19) 0.25744(18) 0.0498(6) Uani 1 1 d . . . . .
H4A H 0.0854 0.8584 0.2031 0.060 Uiso 1 1 calc R U . . .
H4B H 0.0095 0.9572 0.2302 0.060 Uiso 1 1 calc R U . . .
C5 C 0.1492(2) 0.7896(2) 0.4095(2) 0.0578(7) Uani 1 1 d . . . . .
H5A H 0.1254 0.7524 0.4686 0.087 Uiso 1 1 calc R U . . .
H5B H 0.2136 0.8380 0.4341 0.087 Uiso 1 1 calc R U . . .
H5C H 0.1751 0.7381 0.3619 0.087 Uiso 1 1 calc R U . . .
C6 C -0.0623(2) 0.7806(2) 0.32161(18) 0.0503(6) Uani 1 1 d . . . . .
H6A H -0.1204 0.8203 0.2728 0.060 Uiso 1 1 calc R U . . .
H6B H -0.0384 0.7180 0.2847 0.060 Uiso 1 1 calc R U . . .
C7 C -0.1201(2) 0.74364(19) 0.41168(18) 0.0441(6) Uani 1 1 d . . . . .
C8 C -0.1079(2) 0.65216(19) 0.46991(19) 0.0504(6) Uani 1 1 d . . . . .
H8 H -0.0546 0.5964 0.4635 0.060 Uiso 1 1 calc R U . . .
C9 C -0.1899(2) 0.65615(18) 0.54186(19) 0.0479(6) Uani 1 1 d . . . . .
H9 H -0.1999 0.6038 0.5916 0.058 Uiso 1 1 calc R U . . .
C10 C -0.25234(19) 0.75037(17) 0.52584(17) 0.0391(5) Uani 1 1 d . . . . .
C11 C -0.35298(19) 0.79810(17) 0.57660(17) 0.0411(5) Uani 1 1 d . . . . .
C12 C -0.4547(2) 0.83921(19) 0.49049(19) 0.0499(6) Uani 1 1 d . . . . .
H12A H -0.5126 0.8784 0.5242 0.060 Uiso 1 1 calc R U . . .
H12B H -0.4213 0.8889 0.4444 0.060 Uiso 1 1 calc R U . . .
C13 C -0.5178(2) 0.7490(2) 0.4248(2) 0.0614(7) Uani 1 1 d . . . . .
H13A H -0.4614 0.7121 0.3874 0.074 Uiso 1 1 calc R U . . .
H13B H -0.5807 0.7788 0.3729 0.074 Uiso 1 1 calc R U . . .
C14 C -0.5712(2) 0.6692(2) 0.4940(2) 0.0668(8) Uani 1 1 d . . . . .
H14A H -0.6105 0.6115 0.4508 0.080 Uiso 1 1 calc R U . . .
H14B H -0.6306 0.7051 0.5288 0.080 Uiso 1 1 calc R U . . .
C15 C -0.4735(2) 0.6230(2) 0.5759(2) 0.0585(7) Uani 1 1 d . . . . .
H15A H -0.4179 0.5823 0.5408 0.070 Uiso 1 1 calc R U . . .
H15B H -0.5086 0.5741 0.6215 0.070 Uiso 1 1 calc R U . . .
C16 C -0.4063(2) 0.71130(19) 0.64223(19) 0.0500(6) Uani 1 1 d . . . . .
H16A H -0.3420 0.6789 0.6909 0.060 Uiso 1 1 calc R U . . .
H16B H -0.4603 0.7458 0.6837 0.060 Uiso 1 1 calc R U . . .
C17 C -0.3087(2) 0.89221(18) 0.64744(19) 0.0463(6) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
F1 B1 1.399(4) . ?
F2 B1 1.340(4) . ?
F2A B1 1.334(9) . ?
F3 B1 1.346(5) . ?
F3A B1 1.224(11) . ?
F4 B1 1.353(4) . ?
F4A B1 1.410(13) . ?
N1 C17 1.369(3) 3_576 ?
N1 C3 1.373(3) . ?
N2 C5 1.484(3) . ?
N2 C6 1.518(3) . ?
N2 C4 1.520(3) . ?
N3 C10 1.372(3) . ?
N3 C7 1.373(3) . ?
C1 C17 1.367(3) 3_576 ?
C1 C2 1.404(4) . ?
C2 C3 1.344(3) . ?
C3 C4 1.484(3) . ?
C6 C7 1.486(3) . ?
C7 C8 1.355(3) . ?
C8 C9 1.408(3) . ?
C9 C10 1.366(3) . ?
C10 C11 1.518(3) . ?
C11 C17 1.517(3) . ?
C11 C16 1.546(3) . ?
C11 C12 1.554(3) . ?
C12 C13 1.513(4) . ?
C13 C14 1.516(4) . ?
C14 C15 1.517(4) . ?
C15 C16 1.518(3) . ?
C17 C1 1.367(3) 3_576 ?
C17 N1 1.369(3) 3_576 ?

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
F3A B1 F2A 120.1(12) . . ?
F2 B1 F3 108.6(4) . . ?
F2 B1 F4 112.9(4) . . ?
F3 B1 F4 109.4(4) . . ?
F2 B1 F1 104.4(3) . . ?
F3 B1 F1 110.8(4) . . ?
F4 B1 F1 110.6(3) . . ?
F3A B1 F4A 110.1(13) . . ?
F2A B1 F4A 94.6(11) . . ?
C17 N1 C3 110.01(19) 3_576 . ?
C5 N2 C6 111.90(19) . . ?
C5 N2 C4 112.77(18) . . ?
C6 N2 C4 109.20(17) . . ?
C10 N3 C7 110.23(19) . . ?
C17 C1 C2 108.2(2) 3_576 . ?
C3 C2 C1 108.0(2) . . ?
C2 C3 N1 107.5(2) . . ?
C2 C3 C4 129.4(2) . . ?
N1 C3 C4 123.1(2) . . ?
C3 C4 N2 113.17(19) . . ?
C7 C6 N2 113.73(18) . . ?
C8 C7 N3 107.0(2) . . ?
C8 C7 C6 131.9(2) . . ?
N3 C7 C6 120.9(2) . . ?
C7 C8 C9 108.1(2) . . ?
C10 C9 C8 108.1(2) . . ?
C9 C10 N3 106.57(19) . . ?
C9 C10 C11 132.5(2) . . ?
N3 C10 C11 120.95(19) . . ?
C17 C11 C10 110.91(18) . . ?
C17 C11 C16 109.34(18) . . ?
C10 C11 C16 110.10(18) . . ?
C17 C11 C12 108.25(18) . . ?
C10 C11 C12 110.27(18) . . ?
C16 C11 C12 107.89(19) . . ?
C13 C12 C11 112.8(2) . . ?
C12 C13 C14 110.7(2) . . ?
C13 C14 C15 109.8(2) . . ?
C14 C15 C16 111.4(2) . . ?
C15 C16 C11 113.7(2) . . ?
C1 C17 N1 106.3(2) 3_576 3_576 ?
C1 C17 C11 129.5(2) 3_576 . ?
N1 C17 C11 124.05(19) 3_576 . ?

_refine_diff_density_max         0.401
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.041

_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_2c
_database_code_depnum_ccdc_archive 'CCDC 1455741'
_audit_update_record             
;
2016-06-13 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;


# start Validation Reply Form
# start Validation Reply Form
_vrf_PLAT353_2c                  
;
PROBLEM: Long N-H (N0.87,N1.01A) N1 - H1N .. 1.12 Ang.
RESPONSE: This hydrogen is involved in a strong hydrogen bond
with the guest chlorine atom and therefore move towards the 
H-bond acceptor.
;
# end Validation Reply Form 

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H52 Cl2 N6 O'
_chemical_formula_weight         619.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   11.4134(14)
_cell_length_b                   11.7294(14)
_cell_length_c                   14.5809(17)
_cell_angle_alpha                101.215(4)
_cell_angle_beta                 109.626(4)
_cell_angle_gamma                96.150(4)
_cell_volume                     1771.8(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    19156
_cell_measurement_theta_min      1.530
_cell_measurement_theta_max      24.171

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_F_000             668
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    0.217
_shelx_estimated_absorpt_T_min   0.899
_shelx_estimated_absorpt_T_max   0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.906
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Brucker CCD APEX 2'
_diffrn_measurement_method       hemisphere
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19156
_diffrn_reflns_av_unetI/netI     0.0794
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.530
_diffrn_reflns_theta_max         24.171
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.895
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.895
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.895
_reflns_number_total             5590
_reflns_number_gt                2891
_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       APEX2
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    sir92
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    Diamond3.2
_computing_publication_material  'CIFTAB (Sheldrick 2013)'

_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)+(0.1571P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5590
_refine_ls_number_parameters     406
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.1341
_refine_ls_R_factor_gt           0.0700
_refine_ls_wR_factor_ref         0.2357
_refine_ls_wR_factor_gt          0.2015
_refine_ls_goodness_of_fit_ref   0.887
_refine_ls_restrained_S_all      0.888
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Cl1 Cl 0.33090(12) 0.52877(11) 0.48077(10) 0.0797(5) Uani 1 1 d . . . . .
Cl2 Cl 0.81757(12) 0.02954(10) 0.53642(10) 0.0758(4) Uani 1 1 d . . . . .
N1 N 0.9805(3) 0.2695(3) 0.5861(3) 0.0531(9) Uani 1 1 d . . . . .
H1N H 0.910(4) 0.186(4) 0.565(3) 0.079(11) Uiso 1 1 d . U . . .
N2 N 1.1303(4) -0.1630(3) 0.6587(3) 0.0584(10) Uani 1 1 d . . . . .
H2N H 1.192(5) -0.108(4) 0.652(3) 0.078(8) Uiso 1 1 d . U . . .
N3 N 1.1207(4) 0.0966(3) 0.7015(3) 0.0558(10) Uani 1 1 d . . . . .
H3N H 1.053(5) 0.043(4) 0.655(4) 0.078(8) Uiso 1 1 d . U . . .
N4 N 0.5666(4) 0.4013(4) 0.7151(3) 0.0574(10) Uani 1 1 d . . . . .
H4N H 0.516(5) 0.444(4) 0.713(4) 0.078(8) Uiso 1 1 d . U . . .
N5 N 0.3080(3) 0.3529(3) 0.2736(3) 0.0565(10) Uani 1 1 d . . . . .
H5N H 0.291(4) 0.412(4) 0.318(4) 0.078(8) Uiso 1 1 d . U . . .
N6 N 0.4513(3) 0.2508(3) 0.4750(3) 0.0571(11) Uani 1 1 d . . . . .
H6N H 0.478(5) 0.315(4) 0.478(4) 0.079(11) Uiso 1 1 d . U . . .
C1 C 1.2821(9) -0.1560(7) 0.9462(6) 0.161(4) Uani 1 1 d . U . . .
H1A H 1.2512 -0.1313 0.9991 0.242 Uiso 1 1 calc R U . . .
H1B H 1.3642 -0.1757 0.9739 0.242 Uiso 1 1 calc R U . . .
H1C H 1.2248 -0.2241 0.8980 0.242 Uiso 1 1 calc R U . . .
C2 C 1.2918(6) -0.0580(5) 0.8960(4) 0.100(2) Uani 1 1 d . U . . .
H2A H 1.3425 -0.0766 0.8554 0.120 Uiso 1 1 calc R U . . .
H2B H 1.3380 0.0133 0.9478 0.120 Uiso 1 1 calc R U . . .
C3 C 0.9607(6) 0.0435(6) 0.8376(5) 0.0985(19) Uani 1 1 d . . . . .
H3A H 0.9824 0.1172 0.8224 0.148 Uiso 1 1 calc R U . . .
H3B H 0.9132 0.0546 0.8808 0.148 Uiso 1 1 calc R U . . .
H3C H 0.9106 -0.0143 0.7764 0.148 Uiso 1 1 calc R U . . .
C4 C 1.0795(7) 0.0014(5) 0.8893(4) 0.0935(18) Uani 1 1 d . . . . .
H4A H 1.0559 -0.0684 0.9102 0.112 Uiso 1 1 calc R U . . .
H4B H 1.1299 0.0621 0.9496 0.112 Uiso 1 1 calc R U . . .
C5 C 1.1649(5) -0.0295(4) 0.8274(4) 0.0689(13) Uani 1 1 d . . . . .
C6 C 1.0955(4) -0.1365(4) 0.7412(3) 0.0585(12) Uani 1 1 d . . . . .
C7 C 1.0035(4) -0.2274(4) 0.7296(4) 0.0614(12) Uani 1 1 d . . . . .
H7 H 0.9630 -0.2339 0.7746 0.074 Uiso 1 1 calc R U . . .
C8 C 0.9793(4) -0.3101(4) 0.6385(4) 0.0598(12) Uani 1 1 d . . . . .
H8 H 0.9205 -0.3805 0.6127 0.072 Uiso 1 1 calc R U . . .
C9 C 0.9431(4) 0.2690(4) 0.4048(3) 0.0537(11) Uani 1 1 d . . . . .
C10 C 0.4291(4) 0.2406(4) 0.5710(3) 0.0652(13) Uani 1 1 d . . . . .
H10A H 0.3637 0.2844 0.5776 0.078 Uiso 1 1 calc R U . . .
H10B H 0.3991 0.1582 0.5661 0.078 Uiso 1 1 calc R U . . .
C11 C 0.5401(5) 0.1754(5) 0.4533(4) 0.0815(16) Uani 1 1 d . . . . .
H11A H 0.5590 0.1922 0.3973 0.122 Uiso 1 1 calc R U . . .
H11B H 0.5018 0.0936 0.4372 0.122 Uiso 1 1 calc R U . . .
H11C H 0.6169 0.1918 0.5112 0.122 Uiso 1 1 calc R U . . .
C12 C 0.3262(4) 0.2218(4) 0.3884(3) 0.0619(12) Uani 1 1 d . . . . .
H12A H 0.2917 0.1384 0.3751 0.074 Uiso 1 1 calc R U . . .
H12B H 0.2681 0.2662 0.4084 0.074 Uiso 1 1 calc R U . . .
C13 C 0.3313(4) 0.2470(4) 0.2949(4) 0.0605(12) Uani 1 1 d . . . . .
C14 C 0.3484(5) 0.1798(5) 0.2139(4) 0.0758(15) Uani 1 1 d . . . . .
H14 H 0.3645 0.1031 0.2069 0.091 Uiso 1 1 calc R U . . .
C15 C 0.3371(5) 0.2482(4) 0.1441(4) 0.0733(14) Uani 1 1 d . . . . .
H15 H 0.3459 0.2248 0.0824 0.088 Uiso 1 1 calc R U . . .
C16 C 0.6886(4) 0.6455(4) 0.8195(3) 0.0607(12) Uani 1 1 d . . . . .
C17 C 0.7259(5) 0.5459(4) 0.8676(3) 0.0687(14) Uani 1 1 d . . . . .
C18 C 0.8773(7) 0.5679(5) 0.9105(5) 0.137(3) Uani 1 1 d . U . . .
H18A H 0.9022 0.5064 0.9448 0.164 Uiso 1 1 calc R U . . .
H18B H 0.9034 0.5552 0.8531 0.164 Uiso 1 1 calc R U . . .
C19 C 0.9494(8) 0.6767(7) 0.9761(7) 0.162(4) Uani 1 1 d . U . . .
H19A H 0.9308 0.7395 0.9432 0.243 Uiso 1 1 calc R U . . .
H19B H 1.0379 0.6739 0.9945 0.243 Uiso 1 1 calc R U . . .
H19C H 0.9287 0.6907 1.0354 0.243 Uiso 1 1 calc R U . . .
C20 C 0.6619(10) 0.5428(6) 0.9467(5) 0.152(4) Uani 1 1 d . U . . .
H20A H 0.6901 0.6190 0.9951 0.182 Uiso 1 1 calc R U . . .
H20B H 0.5712 0.5335 0.9124 0.182 Uiso 1 1 calc R U . . .
C21 C 0.6855(14) 0.4495(9) 1.0030(7) 0.232(6) Uani 1 1 d . U . . .
H21A H 0.7156 0.3883 0.9679 0.348 Uiso 1 1 calc R U . . .
H21B H 0.6083 0.4164 1.0085 0.348 Uiso 1 1 calc R U . . .
H21C H 0.7480 0.4834 1.0690 0.348 Uiso 1 1 calc R U . . .
C22 C 0.6798(4) 0.4275(4) 0.7932(3) 0.0566(11) Uani 1 1 d . . . . .
C23 C 0.7293(5) 0.3263(5) 0.7879(4) 0.0754(14) Uani 1 1 d . . . . .
H23 H 0.8067 0.3171 0.8315 0.090 Uiso 1 1 calc R U . . .
C24 C 0.6449(6) 0.2398(4) 0.7067(4) 0.0821(16) Uani 1 1 d . . . . .
H24 H 0.6555 0.1625 0.6869 0.099 Uiso 1 1 calc R U . . .
C25 C 0.5451(4) 0.2863(4) 0.6613(3) 0.0592(12) Uani 1 1 d . . . . .
C26 C 0.9284(4) 0.3253(4) 0.4988(4) 0.0612(12) Uani 1 1 d . . . . .
H26A H 0.8389 0.3239 0.4853 0.073 Uiso 1 1 calc R U . . .
H26B H 0.9700 0.4076 0.5192 0.073 Uiso 1 1 calc R U . . .
C27 C 0.9744(5) 0.3436(4) 0.6779(4) 0.0787(15) Uani 1 1 d . . . . .
H27A H 0.8897 0.3574 0.6653 0.118 Uiso 1 1 calc R U . . .
H27B H 1.0314 0.4179 0.6971 0.118 Uiso 1 1 calc R U . . .
H27C H 0.9983 0.3038 0.7312 0.118 Uiso 1 1 calc R U . . .
C28 C 1.1106(4) 0.2449(4) 0.5990(3) 0.0568(12) Uani 1 1 d . . . . .
H28A H 1.1058 0.1863 0.5402 0.068 Uiso 1 1 calc R U . . .
H28B H 1.1646 0.3168 0.6030 0.068 Uiso 1 1 calc R U . . .
C29 C 1.1689(4) 0.2017(4) 0.6895(3) 0.0516(11) Uani 1 1 d . . . . .
C30 C 1.2775(5) 0.2499(4) 0.7702(4) 0.0671(13) Uani 1 1 d . . . . .
H30 H 1.3300 0.3216 0.7817 0.081 Uiso 1 1 calc R U . . .
C31 C 1.2956(5) 0.1712(4) 0.8330(4) 0.0704(14) Uani 1 1 d . . . . .
H31 H 1.3629 0.1815 0.8934 0.084 Uiso 1 1 calc R U . . .
C32 C 1.1970(4) 0.0767(4) 0.7900(4) 0.0606(12) Uani 1 1 d . . . . .
O1 O 0.3336(5) 0.5067(4) 0.6808(4) 0.1323(17) Uani 1 1 d . . . . .
H1 H 0.2819 0.4941 0.6234 0.198 Uiso 1 1 calc R U . . .
C33 C 0.3168(7) 0.6067(7) 0.7401(5) 0.114(2) Uani 1 1 d . . . . .
H33A H 0.3294 0.5951 0.8058 0.171 Uiso 1 1 calc R U . . .
H33B H 0.2325 0.6205 0.7100 0.171 Uiso 1 1 calc R U . . .
H33C H 0.3770 0.6738 0.7453 0.171 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C27 1.475(5) . ?
N1 C28 1.499(5) . ?
N1 C26 1.517(5) . ?
N2 C6 1.379(6) . ?
N2 C9 1.382(5) 2_756 ?
N3 C29 1.363(5) . ?
N3 C32 1.372(6) . ?
N4 C22 1.360(6) . ?
N4 C25 1.372(6) . ?
N5 C13 1.370(6) . ?
N5 C16 1.376(6) 2_666 ?
N6 C11 1.486(6) . ?
N6 C12 1.506(6) . ?
N6 C10 1.528(6) . ?
C1 C2 1.491(9) . ?
C2 C5 1.572(7) . ?
C3 C4 1.501(8) . ?
C4 C5 1.560(8) . ?
C5 C32 1.512(7) . ?
C5 C6 1.513(6) . ?
C6 C7 1.356(6) . ?
C7 C8 1.407(6) . ?
C8 C9 1.348(6) 2_756 ?
C9 C8 1.348(6) 2_756 ?
C9 N2 1.382(5) 2_756 ?
C9 C26 1.474(6) . ?
C10 C25 1.475(6) . ?
C12 C13 1.469(6) . ?
C13 C14 1.370(6) . ?
C14 C15 1.397(7) . ?
C15 C16 1.359(6) 2_666 ?
C16 C15 1.359(6) 2_666 ?
C16 N5 1.376(6) 2_666 ?
C16 C17 1.504(6) . ?
C17 C22 1.502(6) . ?
C17 C20 1.562(8) . ?
C17 C18 1.600(8) . ?
C18 C19 1.411(9) . ?
C20 C21 1.486(10) . ?
C22 C23 1.369(6) . ?
C23 C24 1.384(7) . ?
C24 C25 1.341(7) . ?
C28 C29 1.478(6) . ?
C29 C30 1.360(6) . ?
C30 C31 1.405(7) . ?
C31 C32 1.369(6) . ?
O1 C33 1.387(7) . ?

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
C27 N1 C28 113.0(4) . . ?
C27 N1 C26 109.6(3) . . ?
C28 N1 C26 112.2(3) . . ?
C6 N2 C9 109.3(4) . 2_756 ?
C29 N3 C32 109.9(4) . . ?
C22 N4 C25 110.4(4) . . ?
C13 N5 C16 109.9(4) . 2_666 ?
C11 N6 C12 111.1(4) . . ?
C11 N6 C10 112.7(4) . . ?
C12 N6 C10 109.4(4) . . ?
C1 C2 C5 117.6(6) . . ?
C3 C4 C5 116.8(5) . . ?
C32 C5 C6 111.3(4) . . ?
C32 C5 C4 108.6(4) . . ?
C6 C5 C4 109.3(4) . . ?
C32 C5 C2 108.4(4) . . ?
C6 C5 C2 109.1(4) . . ?
C4 C5 C2 110.1(5) . . ?
C7 C6 N2 106.6(4) . . ?
C7 C6 C5 131.5(5) . . ?
N2 C6 C5 121.6(4) . . ?
C6 C7 C8 108.8(4) . . ?
C9 C8 C7 107.6(4) 2_756 . ?
C8 C9 N2 107.6(4) 2_756 2_756 ?
C8 C9 C26 128.6(4) 2_756 . ?
N2 C9 C26 123.7(4) 2_756 . ?
C25 C10 N6 112.1(4) . . ?
C13 C12 N6 115.1(4) . . ?
N5 C13 C14 107.4(4) . . ?
N5 C13 C12 120.0(4) . . ?
C14 C13 C12 132.4(5) . . ?
C13 C14 C15 107.0(4) . . ?
C16 C15 C14 109.3(4) 2_666 . ?
C15 C16 N5 106.4(4) 2_666 2_666 ?
C15 C16 C17 131.7(4) 2_666 . ?
N5 C16 C17 121.4(4) 2_666 . ?
C22 C17 C16 112.3(4) . . ?
C22 C17 C20 107.0(5) . . ?
C16 C17 C20 108.0(4) . . ?
C22 C17 C18 107.2(4) . . ?
C16 C17 C18 106.6(4) . . ?
C20 C17 C18 115.9(6) . . ?
C19 C18 C17 120.9(7) . . ?
C21 C20 C17 117.0(7) . . ?
N4 C22 C23 105.8(4) . . ?
N4 C22 C17 122.2(4) . . ?
C23 C22 C17 131.9(4) . . ?
C22 C23 C24 108.5(5) . . ?
C25 C24 C23 108.5(5) . . ?
C24 C25 N4 106.8(4) . . ?
C24 C25 C10 133.9(5) . . ?
N4 C25 C10 119.3(4) . . ?
C9 C26 N1 115.6(3) . . ?
C29 C28 N1 113.3(3) . . ?
C30 C29 N3 107.9(4) . . ?
C30 C29 C28 129.4(4) . . ?
N3 C29 C28 122.6(4) . . ?
C29 C30 C31 107.3(4) . . ?
C32 C31 C30 108.3(4) . . ?
C31 C32 N3 106.6(4) . . ?
C31 C32 C5 130.7(4) . . ?
N3 C32 C5 122.6(4) . . ?

_refine_diff_density_max         0.561
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.052

_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_2d
_database_code_depnum_ccdc_archive 'CCDC 1455742'
_audit_update_record             
;
2016-06-13 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_EXPT005_2d                  
;
PROBLEM: _exptl_crystal_description is missing
RESPONSE: ...
;
_vrf_THETM01_2d                  
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The measurement was set up to collect a full set of data. 
The high angle data, however, was dominated by noise [I/sigma(I) < 1.0] 
and consequently omitted. This is based on a weakly diffracting crystal 
in combination with a substantial amount of disorder.
;
_vrf_REFNR01_2d                  
;
PROBLEM: Ratio of reflections to parameters is < 8 for a
RESPONSE: See response above. The use of constraints and restraints affects
this ratio but cannot be avoided in heavily disordered structures.
;
_vrf_PLAT058_2d                  
;
PROBLEM: Maximum Transmission Factor Missing ............ ?
RESPONSE: ...
;
_vrf_PLAT059_2d                  
;
PROBLEM: Minimum Transmission Factor Missing ............ ?
RESPONSE: ...
;
_vrf_PLAT183_2d                  
;
PROBLEM: Missing _cell_measurement_reflns_used value .... Please Do !
RESPONSE: ...
;
_vrf_PLAT184_2d                  
;
PROBLEM: Missing _cell_measurement_theta_min value ...... Please Do !
RESPONSE: ...
;
_vrf_PLAT185_2d                  
;
PROBLEM: Missing _cell_measurement_theta_max value ...... Please Do !
RESPONSE: ...
;
_vrf_PLAT213_2d                  
;
PROBLEM: Atom C25A has ADP max/min Ratio ..... 6.4 prolat
RESPONSE: Atom C25A was refined to a 16% fraction of one carbon atom
of an ethyl substituent. This alert is based on the respective disorder.
;
_vrf_PLAT312_2d                  
;
PROBLEM: Strange C-O-H Geometry (C-O < 1.25 Ang) ..... O5A Check
RESPONSE: This alert is based on the respective disorder of the solvent
methanol appearing in two overlapping positions.
;
_vrf_PLAT088_2d                  
;
PROBLEM: Poor Data / Parameter Ratio .................... 7.66 Note
RESPONSE: See REFNR01_ALERT_3_B
;
# end Validation Reply Form


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C47 H62 N6 O5'
_chemical_formula_weight         791.02

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   12.8015(8)
_cell_length_b                   13.1729(8)
_cell_length_c                   14.8039(8)
_cell_angle_alpha                72.028(3)
_cell_angle_beta                 87.892(3)
_cell_angle_gamma                70.142(3)
_cell_volume                     2227.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_F_000             852
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.077
_shelx_estimated_absorpt_T_min   0.976
_shelx_estimated_absorpt_T_max   0.992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Brucker CCD APEX 2'
_diffrn_measurement_method       hemisphere
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15300
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.450
_diffrn_reflns_theta_max         20.608
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.569
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.569
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.569
_reflns_number_total             4471
_reflns_number_gt                3458
_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       APEX2
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    Diamond3.2
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'

_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)+(0.0528P)²+1.5706P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4471
_refine_ls_number_parameters     592
_refine_ls_number_restraints     94
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0472
_refine_ls_wR_factor_ref         0.1310
_refine_ls_wR_factor_gt          0.1155
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
C1 C 0.2022(4) 0.6613(3) 0.4935(3) 0.1046(16) Uani 1 1 d . . . . .
H1A H 0.1682 0.6423 0.5523 0.157 Uiso 1 1 calc R U . . .
H1B H 0.2016 0.6106 0.4590 0.157 Uiso 1 1 calc R U . . .
H1C H 0.1613 0.7382 0.4560 0.157 Uiso 1 1 calc R U . . .
C2 C 0.3208(3) 0.6501(3) 0.5143(3) 0.0676(10) Uani 1 1 d . . . . .
H2A H 0.3569 0.6597 0.4550 0.081 Uiso 1 1 calc R U . . .
H2B H 0.3596 0.5735 0.5557 0.081 Uiso 1 1 calc R U . . .
C3 C 0.3378(4) 0.6059(4) 0.7340(3) 0.0967(14) Uani 1 1 d . . . . .
H3A H 0.3342 0.5470 0.7103 0.145 Uiso 1 1 calc R U . . .
H3B H 0.2983 0.6038 0.7906 0.145 Uiso 1 1 calc R U . . .
H3C H 0.4142 0.5944 0.7487 0.145 Uiso 1 1 calc R U . . .
C4 C 0.2852(3) 0.7206(3) 0.6591(2) 0.0650(10) Uani 1 1 d . . . . .
H4A H 0.2917 0.7787 0.6834 0.078 Uiso 1 1 calc R U . . .
H4B H 0.2064 0.7341 0.6498 0.078 Uiso 1 1 calc R U . . .
C5 C 0.3346(2) 0.7350(2) 0.5613(2) 0.0464(8) Uani 1 1 d . . . . .
C6 C 0.2740(3) 0.8551(3) 0.4974(2) 0.0422(8) Uani 1 1 d . . . . .
C7 C 0.1721(3) 0.9323(3) 0.5010(2) 0.0501(9) Uani 1 1 d . . . . .
H7 H 0.1234 0.9227 0.5484 0.060 Uiso 1 1 calc R U . . .
C8 C 0.1539(3) 1.0290(3) 0.4205(2) 0.0512(9) Uani 1 1 d . . . . .
H8 H 0.0911 1.0946 0.4056 0.061 Uiso 1 1 calc R U . . .
C9 C 0.2438(3) 1.0098(3) 0.3685(2) 0.0441(8) Uani 1 1 d . . . . .
C10 C 0.2680(3) 1.0843(3) 0.2794(2) 0.0504(9) Uani 1 1 d . . . . .
H10A H 0.1993 1.1453 0.2499 0.060 Uiso 1 1 calc R U . . .
H10B H 0.2949 1.0406 0.2359 0.060 Uiso 1 1 calc R U . . .
C11 C 0.3626(3) 1.2197(3) 0.2026(2) 0.0615(10) Uani 1 1 d . . . . .
H11A H 0.2943 1.2836 0.1858 0.092 Uiso 1 1 calc R U . . .
H11B H 0.3768 1.1849 0.1531 0.092 Uiso 1 1 calc R U . . .
H11C H 0.4228 1.2449 0.2104 0.092 Uiso 1 1 calc R U . . .
C12 C 0.3267(2) 1.1835(3) 0.3745(2) 0.0483(8) Uani 1 1 d . . . . .
H12A H 0.2487 1.2310 0.3659 0.058 Uiso 1 1 calc R U . . .
H12B H 0.3368 1.1209 0.4330 0.058 Uiso 1 1 calc R U . . .
C13 C 1.1915(3) 0.6957(3) 0.1383(2) 0.0571(9) Uani 1 1 d . . . . .
C14 C 1.1469(4) 0.6195(3) 0.1918(3) 0.0803(12) Uani 1 1 d . . . . .
H14 H 1.1811 0.5408 0.2114 0.096 Uiso 1 1 calc R U . . .
C15 C 1.0398(3) 0.6793(3) 0.2127(3) 0.0735(11) Uani 1 1 d . . . . .
H15 H 0.9914 0.6472 0.2490 0.088 Uiso 1 1 calc R U . . .
C16 C 1.0196(3) 0.7920(3) 0.1707(2) 0.0500(8) Uani 1 1 d . . . . .
C17 C 0.9208(3) 0.8909(3) 0.1707(2) 0.0526(9) Uani 1 1 d . . . . .
H17A H 0.8657 0.8641 0.2074 0.063 Uiso 1 1 calc R U . . .
H17B H 0.8885 0.9314 0.1058 0.063 Uiso 1 1 calc R U . . .
C18 C 1.0180(3) 0.9128(3) 0.3017(2) 0.0642(10) Uani 1 1 d . . . . .
H18A H 0.9800 0.8729 0.3488 0.096 Uiso 1 1 calc R U . . .
H18B H 1.0340 0.9677 0.3236 0.096 Uiso 1 1 calc R U . . .
H18C H 1.0864 0.8596 0.2912 0.096 Uiso 1 1 calc R U . . .
C19 C 0.8430(3) 1.0619(3) 0.2253(2) 0.0580(9) Uani 1 1 d . . . . .
H19A H 0.8068 1.0270 0.2786 0.070 Uiso 1 1 calc R U . . .
H19B H 0.8647 1.1180 0.2420 0.070 Uiso 1 1 calc R U . . .
C20 C 0.7619(3) 1.1205(3) 0.1412(2) 0.0574(9) Uani 1 1 d . . . . .
C21 C 0.6605(3) 1.1166(3) 0.1252(3) 0.0771(11) Uani 1 1 d . . . . .
H21 H 0.6243 1.0744 0.1681 0.093 Uiso 1 1 calc R U . . .
C22 C 0.6194(3) 1.1878(3) 0.0319(3) 0.0800(12) Uani 1 1 d . . . . .
H22 H 0.5510 1.2007 0.0025 0.096 Uiso 1 1 calc R U . . .
C23 C 0.6962(3) 1.2340(3) -0.0078(3) 0.0607(10) Uani 1 1 d . . . . .
C24 C 0.6941(3) 1.3206(3) -0.1035(2) 0.0698(11) Uani 1 1 d D U . . .
C25 C 0.6333(7) 1.4433(6) -0.0991(5) 0.099(3) Uani 0.837(10) 1 d D U P A 1
H25A H 0.6315 1.4978 -0.1610 0.119 Uiso 0.837(10) 1 calc R U P A 1
H25B H 0.5570 1.4520 -0.0840 0.119 Uiso 0.837(10) 1 calc R U P A 1
C26 C 0.6901(7) 1.4684(5) -0.0252(4) 0.118(3) Uani 0.837(10) 1 d D U P A 1
H26A H 0.6847 1.4202 0.0370 0.177 Uiso 0.837(10) 1 calc R U P A 1
H26B H 0.6546 1.5466 -0.0285 0.177 Uiso 0.837(10) 1 calc R U P A 1
H26C H 0.7671 1.4545 -0.0372 0.177 Uiso 0.837(10) 1 calc R U P A 1
C25A C 0.685(2) 1.434(2) -0.079(3) 0.071(9) Uani 0.163(10) 1 d D U P A 2
H25C H 0.7511 1.4152 -0.0386 0.085 Uiso 0.163(10) 1 calc R U P A 2
H25D H 0.6892 1.4894 -0.1381 0.085 Uiso 0.163(10) 1 calc R U P A 2
C26A C 0.586(3) 1.492(3) -0.031(2) 0.108(12) Uani 0.163(10) 1 d D U P A 2
H26D H 0.5930 1.5610 -0.0271 0.161 Uiso 0.163(10) 1 calc R U P A 2
H26E H 0.5852 1.4427 0.0315 0.161 Uiso 0.163(10) 1 calc R U P A 2
H26F H 0.5188 1.5098 -0.0682 0.161 Uiso 0.163(10) 1 calc R U P A 2
C27 C 0.6171(3) 1.3146(5) -0.1788(3) 0.1070(16) Uani 1 1 d . . . . .
H27A H 0.5443 1.3240 -0.1542 0.128 Uiso 1 1 calc R U . . .
H27B H 0.6082 1.3793 -0.2354 0.128 Uiso 1 1 calc R U . . .
C28 C 0.6501(4) 1.2146(6) -0.2077(4) 0.142(2) Uani 1 1 d . . . . .
H28A H 0.7171 1.2088 -0.2402 0.213 Uiso 1 1 calc R U . . .
H28B H 0.5921 1.2192 -0.2497 0.213 Uiso 1 1 calc R U . . .
H28C H 0.6633 1.1487 -0.1526 0.213 Uiso 1 1 calc R U . . .
C29 C 0.6064(3) 0.7486(3) 0.6136(2) 0.0434(8) Uani 1 1 d . . . . .
C30 C 0.6423(3) 0.6431(3) 0.6048(2) 0.0540(9) Uani 1 1 d . . . . .
H30 H 0.7157 0.5936 0.6137 0.065 Uiso 1 1 calc R U . . .
C31 C 0.5491(3) 0.6218(3) 0.5799(2) 0.0539(9) Uani 1 1 d . . . . .
H31 H 0.5498 0.5558 0.5687 0.065 Uiso 1 1 calc R U . . .
C32 C 0.4569(2) 0.7145(2) 0.5750(2) 0.0417(8) Uani 1 1 d . . . . .
N1 N 1.1121(2) 0.8011(2) 0.12482(19) 0.0506(8) Uani 1 1 d . . . . .
N2 N 0.9463(2) 0.9718(2) 0.21117(18) 0.0478(7) Uani 1 1 d . . . . .
N3 N 0.7828(3) 1.1931(2) 0.0599(2) 0.0565(8) Uani 1 1 d . . . . .
N4 N 0.3167(2) 0.9030(2) 0.41575(19) 0.0448(7) Uani 1 1 d . . . . .
N5 N 0.3531(2) 1.1356(2) 0.29332(17) 0.0429(7) Uani 1 1 d . . . . .
N6 N 0.4934(2) 0.7921(2) 0.59462(17) 0.0424(7) Uani 1 1 d . . . . .
H1N H 1.120(2) 0.862(3) 0.097(2) 0.042(5) Uiso 1 1 d . U . . .
H2N H 0.987(3) 1.010(3) 0.164(2) 0.065(7) Uiso 1 1 d . U . . .
H3N H 0.842(2) 1.208(2) 0.055(2) 0.042(5) Uiso 1 1 d . U . . .
H4N H 0.383(2) 0.878(2) 0.399(2) 0.042(5) Uiso 1 1 d . U . . .
H5N H 0.419(3) 1.073(3) 0.311(2) 0.065(7) Uiso 1 1 d . U . . .
H6N H 0.450(2) 0.855(2) 0.601(2) 0.042(5) Uiso 1 1 d . U . . .
C33 C 0.6045(3) 0.9238(3) 0.3588(3) 0.0621(10) Uani 1 1 d . . . . .
C34 C 0.6984(2) 0.8134(2) 0.3751(2) 0.0425(8) Uani 1 1 d . . . . .
C35 C 0.6883(3) 0.7294(3) 0.3437(3) 0.0667(10) Uani 1 1 d . . . . .
H35 H 0.6226 0.7419 0.3103 0.080 Uiso 1 1 calc R U . . .
C36 C 0.7732(4) 0.6275(3) 0.3606(3) 0.0901(13) Uani 1 1 d . . . . .
H36 H 0.7647 0.5716 0.3386 0.108 Uiso 1 1 calc R U . . .
C37 C 0.8677(4) 0.6076(3) 0.4081(3) 0.0840(13) Uani 1 1 d . . . . .
H37 H 0.9243 0.5375 0.4192 0.101 Uiso 1 1 calc R U . . .
C38 C 0.8838(3) 0.6876(4) 0.4411(3) 0.0734(11) Uani 1 1 d . . . . .
H38 H 0.9505 0.6728 0.4742 0.088 Uiso 1 1 calc R U . . .
C39 C 0.7969(3) 0.7933(3) 0.4239(2) 0.0573(9) Uani 1 1 d . . . . .
H39 H 0.8059 0.8493 0.4454 0.069 Uiso 1 1 calc R U . . .
O1 O 0.5150(2) 0.9350(2) 0.32237(19) 0.0860(8) Uani 1 1 d . . . . .
O2 O 0.6249(3) 0.9986(2) 0.3833(2) 0.1015(10) Uani 1 1 d . . . . .
C40 C 0.9256(3) 0.8569(4) -0.0718(2) 0.0636(10) Uani 1 1 d . . . . .
C41 C 0.8399(4) 0.8138(4) -0.0185(2) 0.0672(11) Uani 1 1 d . . . . .
C42 C 0.7451(4) 0.8861(4) 0.0027(3) 0.0855(13) Uani 1 1 d . . . . .
H42 H 0.7324 0.9638 -0.0179 0.103 Uiso 1 1 calc R U . . .
C43 C 0.6673(5) 0.8457(7) 0.0543(4) 0.128(2) Uani 1 1 d . . . . .
H43 H 0.6032 0.8956 0.0692 0.154 Uiso 1 1 calc R U . . .
C44 C 0.6856(7) 0.7330(9) 0.0828(5) 0.162(4) Uani 1 1 d . . . . .
H44 H 0.6325 0.7060 0.1161 0.194 Uiso 1 1 calc R U . . .
C45 C 0.7795(7) 0.6586(6) 0.0639(5) 0.153(3) Uani 1 1 d . . . . .
H45 H 0.7915 0.5811 0.0859 0.183 Uiso 1 1 calc R U . . .
C46 C 0.8578(4) 0.6983(4) 0.0117(3) 0.1028(16) Uani 1 1 d . . . . .
H46 H 0.9217 0.6478 -0.0029 0.123 Uiso 1 1 calc R U . . .
O3 O 0.9157(2) 0.9580(2) -0.08440(17) 0.0758(7) Uani 1 1 d . . . . .
O4 O 1.0043(3) 0.7908(3) -0.1009(2) 0.0912(9) Uani 1 1 d . . . . .
C47 C 0.0061(13) 0.6114(12) 0.7551(11) 0.127(4) Uani 0.731(18) 1 d . U P B 1
H47A H -0.0409 0.5886 0.8034 0.191 Uiso 0.731(18) 1 calc R U P B 1
H47B H 0.0815 0.5603 0.7725 0.191 Uiso 0.731(18) 1 calc R U P B 1
H47C H -0.0189 0.6096 0.6954 0.191 Uiso 0.731(18) 1 calc R U P B 1
O5 O 0.0012(9) 0.7170(5) 0.7466(4) 0.128(4) Uani 0.731(18) 1 d . U P B 1
H5 H 0.0135 0.7208 0.7992 0.192 Uiso 0.731(18) 1 calc R U P B 1
O5A O -0.0593(16) 0.667(2) 0.798(2) 0.139(11) Uani 0.269(18) 1 d . U P B 2
H5A H -0.0687 0.6853 0.8463 0.208 Uiso 0.269(18) 1 calc R U P B 2
C47A C 0.034(4) 0.603(4) 0.802(4) 0.196(18) Uani 0.269(18) 1 d . U P B 2
H47D H 0.0552 0.5510 0.8653 0.294 Uiso 0.269(18) 1 calc R U P B 2
H47E H 0.0837 0.6448 0.7843 0.294 Uiso 0.269(18) 1 calc R U P B 2
H47F H 0.0378 0.5603 0.7584 0.294 Uiso 0.269(18) 1 calc R U 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
C1 C2 1.509(5) . ?
C2 C5 1.546(4) . ?
C3 C4 1.515(5) . ?
C4 C5 1.541(4) . ?
C5 C32 1.505(4) . ?
C5 C6 1.516(4) . ?
C6 C7 1.366(4) . ?
C6 N4 1.369(4) . ?
C7 C8 1.406(4) . ?
C8 C9 1.356(4) . ?
C9 N4 1.373(4) . ?
C9 C10 1.476(4) . ?
C10 N5 1.514(4) . ?
C11 N5 1.485(4) . ?
C12 C29 1.481(4) 2_676 ?
C12 N5 1.500(4) . ?
C13 C14 1.352(5) . ?
C13 N1 1.374(4) . ?
C13 C24 1.502(5) 2_775 ?
C14 C15 1.408(5) . ?
C15 C16 1.356(4) . ?
C16 N1 1.366(4) . ?
C16 C17 1.476(4) . ?
C17 N2 1.498(4) . ?
C18 N2 1.485(4) . ?
C19 C20 1.477(5) . ?
C19 N2 1.506(4) . ?
C20 C21 1.349(5) . ?
C20 N3 1.369(4) . ?
C21 C22 1.408(5) . ?
C22 C23 1.352(5) . ?
C23 N3 1.366(4) . ?
C23 C24 1.515(5) . ?
C24 C13 1.502(5) 2_775 ?
C24 C27 1.552(6) . ?
C24 C25 1.558(7) . ?
C24 C25A 1.604(19) . ?
C25 C26 1.510(9) . ?
C25A C26A 1.511(19) . ?
C27 C28 1.433(7) . ?
C29 C30 1.354(4) . ?
C29 N6 1.366(4) . ?
C29 C12 1.481(4) 2_676 ?
C30 C31 1.401(4) . ?
C31 C32 1.365(4) . ?
C32 N6 1.366(4) . ?
C33 O1 1.228(4) . ?
C33 O2 1.254(4) . ?
C33 C34 1.495(5) . ?
C34 C35 1.370(4) . ?
C34 C39 1.380(4) . ?
C35 C36 1.366(5) . ?
C36 C37 1.327(6) . ?
C37 C38 1.366(6) . ?
C38 C39 1.411(5) . ?
C40 O3 1.248(4) . ?
C40 O4 1.250(4) . ?
C40 C41 1.495(5) . ?
C41 C42 1.360(5) . ?
C41 C46 1.384(5) . ?
C42 C43 1.382(6) . ?
C43 C44 1.349(9) . ?
C44 C45 1.351(10) . ?
C45 C46 1.388(8) . ?
C47 O5 1.337(17) . ?
O5A C47A 1.20(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 C2 C5 115.4(3) . . ?
C3 C4 C5 115.9(3) . . ?
C32 C5 C6 110.6(2) . . ?
C32 C5 C4 108.7(2) . . ?
C6 C5 C4 108.1(3) . . ?
C32 C5 C2 108.7(3) . . ?
C6 C5 C2 108.9(2) . . ?
C4 C5 C2 111.8(3) . . ?
C7 C6 N4 106.6(3) . . ?
C7 C6 C5 131.6(3) . . ?
N4 C6 C5 121.6(3) . . ?
C6 C7 C8 108.1(3) . . ?
C9 C8 C7 108.0(3) . . ?
C8 C9 N4 107.0(3) . . ?
C8 C9 C10 130.0(3) . . ?
N4 C9 C10 123.0(3) . . ?
C9 C10 N5 113.7(2) . . ?
C29 C12 N5 115.8(2) 2_676 . ?
C14 C13 N1 106.2(3) . . ?
C14 C13 C24 130.8(3) . 2_775 ?
N1 C13 C24 122.8(3) . 2_775 ?
C13 C14 C15 108.5(3) . . ?
C16 C15 C14 108.0(3) . . ?
C15 C16 N1 106.5(3) . . ?
C15 C16 C17 130.1(3) . . ?
N1 C16 C17 123.4(3) . . ?
C16 C17 N2 113.3(2) . . ?
C20 C19 N2 114.1(3) . . ?
C21 C20 N3 106.8(3) . . ?
C21 C20 C19 131.2(3) . . ?
N3 C20 C19 122.0(3) . . ?
C20 C21 C22 107.9(3) . . ?
C23 C22 C21 108.4(3) . . ?
C22 C23 N3 106.4(3) . . ?
C22 C23 C24 131.3(3) . . ?
N3 C23 C24 122.2(3) . . ?
C13 C24 C23 111.9(3) 2_775 . ?
C13 C24 C27 109.4(3) 2_775 . ?
C23 C24 C27 110.7(3) . . ?
C13 C24 C25 112.7(5) 2_775 . ?
C23 C24 C25 110.1(4) . . ?
C27 C24 C25 101.5(4) . . ?
C13 C24 C25A 94.1(10) 2_775 . ?
C23 C24 C25A 104.4(14) . . ?
C27 C24 C25A 125.2(12) . . ?
C26 C25 C24 111.8(6) . . ?
C26A C25A C24 122(2) . . ?
C28 C27 C24 118.4(4) . . ?
C30 C29 N6 107.4(3) . . ?
C30 C29 C12 128.5(3) . 2_676 ?
N6 C29 C12 123.4(3) . 2_676 ?
C29 C30 C31 107.7(3) . . ?
C32 C31 C30 108.2(3) . . ?
C31 C32 N6 106.6(3) . . ?
C31 C32 C5 131.6(3) . . ?
N6 C32 C5 121.6(3) . . ?
C16 N1 C13 110.8(3) . . ?
C18 N2 C17 112.6(2) . . ?
C18 N2 C19 109.7(2) . . ?
C17 N2 C19 112.8(2) . . ?
C23 N3 C20 110.5(3) . . ?
C6 N4 C9 110.3(3) . . ?
C11 N5 C12 113.5(2) . . ?
C11 N5 C10 110.3(2) . . ?
C12 N5 C10 110.6(2) . . ?
C32 N6 C29 110.1(2) . . ?
O1 C33 O2 125.3(4) . . ?
O1 C33 C34 118.5(4) . . ?
O2 C33 C34 116.2(4) . . ?
C35 C34 C39 118.5(3) . . ?
C35 C34 C33 121.2(3) . . ?
C39 C34 C33 120.3(3) . . ?
C36 C35 C34 121.1(4) . . ?
C37 C36 C35 120.5(4) . . ?
C36 C37 C38 121.6(4) . . ?
C37 C38 C39 118.4(4) . . ?
C34 C39 C38 119.8(3) . . ?
O3 C40 O4 122.8(4) . . ?
O3 C40 C41 118.0(4) . . ?
O4 C40 C41 119.2(4) . . ?
C42 C41 C46 119.2(4) . . ?
C42 C41 C40 121.0(4) . . ?
C46 C41 C40 119.8(5) . . ?
C41 C42 C43 120.9(5) . . ?
C44 C43 C42 119.2(7) . . ?
C43 C44 C45 121.5(7) . . ?
C44 C45 C46 119.8(7) . . ?
C41 C46 C45 119.4(6) . . ?

_refine_diff_density_max         0.455
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.032

_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_2e
_database_code_depnum_ccdc_archive 'CCDC 1455743'
_audit_update_record             
;
2016-06-13 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H48 Cl2 N6 O8'
_chemical_formula_weight         715.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   10.826(5)
_cell_length_b                   10.886(5)
_cell_length_c                   15.397(7)
_cell_angle_alpha                86.377(13)
_cell_angle_beta                 81.065(14)
_cell_angle_gamma                81.984(12)
_cell_volume                     1773.4(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    20498
_cell_measurement_theta_min      1.340
_cell_measurement_theta_max      24.663

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_F_000             760
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.219
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    0.240
_shelx_estimated_absorpt_T_min   0.949
_shelx_estimated_absorpt_T_max   0.958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.949
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Brucker CCD APEX 2'
_diffrn_measurement_method       hemisphere
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20498
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.340
_diffrn_reflns_theta_max         24.663
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.956
_reflns_number_total             5963
_reflns_number_gt                3985
_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       APEX2
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    Diamond3.2
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'

_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)+(0.0518P)²+0.5637P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5963
_refine_ls_number_parameters     537
_refine_ls_number_restraints     120
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0476
_refine_ls_wR_factor_ref         0.1262
_refine_ls_wR_factor_gt          0.1071
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.023
_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
C1 C -0.2246(3) 0.1208(3) -0.1801(2) 0.0689(9) Uani 1 1 d . . . . .
H1A H -0.2314 0.1927 -0.2194 0.103 Uiso 1 1 calc R U . . .
H1B H -0.2293 0.0482 -0.2111 0.103 Uiso 1 1 calc R U . . .
H1C H -0.1453 0.1126 -0.1583 0.103 Uiso 1 1 calc R U . . .
C2 C -0.3310(3) 0.1350(3) -0.10393(19) 0.0549(8) Uani 1 1 d . . . . .
H2A H -0.3301 0.0570 -0.0698 0.066 Uiso 1 1 calc R U . . .
H2B H -0.4101 0.1501 -0.1274 0.066 Uiso 1 1 calc R U . . .
C3 C -0.4811(3) 0.1498(3) 0.0848(2) 0.0813(11) Uani 1 1 d . . . . .
H3A H -0.4996 0.0837 0.0526 0.122 Uiso 1 1 calc R U . . .
H3B H -0.5520 0.1746 0.1287 0.122 Uiso 1 1 calc R U . . .
H3C H -0.4084 0.1219 0.1128 0.122 Uiso 1 1 calc R U . . .
C4 C -0.4550(3) 0.2594(3) 0.0222(2) 0.0577(8) Uani 1 1 d . . . . .
H4A H -0.4559 0.3313 0.0566 0.069 Uiso 1 1 calc R U . . .
H4B H -0.5230 0.2776 -0.0128 0.069 Uiso 1 1 calc R U . . .
C5 C -0.3282(2) 0.2404(2) -0.04074(17) 0.0412(6) Uani 1 1 d . . . . .
C6 C -0.2242(2) 0.2050(2) 0.01462(16) 0.0387(6) Uani 1 1 d . . . . .
C7 C -0.1603(2) 0.0926(2) 0.03518(17) 0.0440(6) Uani 1 1 d . . . . .
H7 H -0.1636 0.0179 0.0099 0.053 Uiso 1 1 calc R U . . .
C8 C -0.0885(2) 0.1091(2) 0.10141(17) 0.0460(7) Uani 1 1 d . . . . .
H8 H -0.0362 0.0474 0.1276 0.055 Uiso 1 1 calc R U . . .
C9 C -0.1095(2) 0.2321(2) 0.12049(16) 0.0383(6) Uani 1 1 d . . . . .
C10 C -0.0601(2) 0.3016(2) 0.18398(16) 0.0434(6) Uani 1 1 d . . . . .
H10A H -0.0497 0.2486 0.2361 0.052 Uiso 1 1 calc R U . . .
H10B H -0.1216 0.3725 0.2016 0.052 Uiso 1 1 calc R U . . .
C12 C 0.1680(3) 0.2435(3) 0.1277(2) 0.0658(9) Uani 1 1 d . . . . .
H12A H 0.1808 0.1952 0.1807 0.099 Uiso 1 1 calc R U . . .
H12B H 0.2442 0.2767 0.1034 0.099 Uiso 1 1 calc R U . . .
H12C H 0.1458 0.1917 0.0859 0.099 Uiso 1 1 calc R U . . .
C13 C 0.0982(3) 0.4342(2) 0.21165(17) 0.0458(7) Uani 1 1 d . . . . .
H13A H 0.0261 0.4964 0.2274 0.055 Uiso 1 1 calc R U . . .
H13B H 0.1158 0.3873 0.2650 0.055 Uiso 1 1 calc R U . . .
C14 C 0.2082(3) 0.4970(2) 0.17484(16) 0.0425(6) Uani 1 1 d . . . . .
C15 C 0.3324(3) 0.4701(3) 0.18326(19) 0.0526(7) Uani 1 1 d . . . . .
H15 H 0.3681 0.4041 0.2165 0.063 Uiso 1 1 calc R U . . .
C16 C 0.3970(3) 0.5599(3) 0.13282(19) 0.0512(7) Uani 1 1 d . . . . .
H16 H 0.4833 0.5636 0.1267 0.061 Uiso 1 1 calc R U . . .
C17 C 0.3115(2) 0.6405(2) 0.09441(17) 0.0395(6) Uani 1 1 d . . . . .
C18 C 0.0635(3) 0.6627(3) 0.3655(2) 0.0710(9) Uani 1 1 d . . . . .
H18A H 0.1450 0.6476 0.3303 0.107 Uiso 1 1 calc R U . . .
H18B H 0.0023 0.6974 0.3288 0.107 Uiso 1 1 calc R U . . .
H18C H 0.0404 0.5859 0.3931 0.107 Uiso 1 1 calc R U . . .
C19 C 0.0681(3) 0.7534(3) 0.43601(19) 0.0579(8) Uani 1 1 d . . . . .
H19A H -0.0119 0.7605 0.4750 0.069 Uiso 1 1 calc R U . . .
H19B H 0.0769 0.8345 0.4076 0.069 Uiso 1 1 calc R U . . .
C20 C 0.2515(4) 0.5489(3) 0.6052(2) 0.0858(11) Uani 1 1 d . . . . .
H20A H 0.3355 0.5360 0.5734 0.129 Uiso 1 1 calc R U . . .
H20B H 0.2308 0.4724 0.6346 0.129 Uiso 1 1 calc R U . . .
H20C H 0.2466 0.6107 0.6478 0.129 Uiso 1 1 calc R U . . .
C21 C 0.1597(3) 0.5922(3) 0.5419(2) 0.0648(9) Uani 1 1 d . . . . .
H21A H 0.0749 0.5976 0.5743 0.078 Uiso 1 1 calc R U . . .
H21B H 0.1671 0.5294 0.4987 0.078 Uiso 1 1 calc R U . . .
C22 C 0.1757(2) 0.7182(2) 0.49249(17) 0.0412(6) Uani 1 1 d . . . . .
C23 C 0.3003(2) 0.7104(2) 0.43230(16) 0.0393(6) Uani 1 1 d . . . . .
C24 C 0.3764(3) 0.6115(2) 0.39363(19) 0.0514(7) Uani 1 1 d . . . . .
H24 H 0.3664 0.5283 0.4052 0.062 Uiso 1 1 calc R U . . .
C25 C 0.4718(3) 0.6574(3) 0.33368(19) 0.0517(7) Uani 1 1 d . . . . .
H25 H 0.5355 0.6099 0.2980 0.062 Uiso 1 1 calc R U . . .
C26 C 0.4552(2) 0.7836(2) 0.33658(16) 0.0421(6) Uani 1 1 d . . . . .
C27 C 0.5302(2) 0.8765(2) 0.28918(16) 0.0435(6) Uani 1 1 d . . . . .
H27A H 0.4736 0.9492 0.2741 0.052 Uiso 1 1 calc R U . . .
H27B H 0.5754 0.8425 0.2347 0.052 Uiso 1 1 calc R U . . .
C28 C 0.7161(3) 0.8090(3) 0.3655(2) 0.0545(7) Uani 1 1 d . . . . .
H28A H 0.7636 0.7746 0.3126 0.082 Uiso 1 1 calc R U . . .
H28B H 0.6718 0.7467 0.3986 0.082 Uiso 1 1 calc R U . . .
H28C H 0.7724 0.8367 0.4002 0.082 Uiso 1 1 calc R U . . .
C29 C 0.6896(2) 1.0188(2) 0.29224(16) 0.0449(7) Uani 1 1 d . . . . .
H29A H 0.7365 0.9876 0.2374 0.054 Uiso 1 1 calc R U . . .
H29B H 0.6264 1.0860 0.2779 0.054 Uiso 1 1 calc R U . . .
C30 C 0.7770(2) 1.0680(2) 0.34206(16) 0.0394(6) Uani 1 1 d . . . . .
C31 C 0.9036(2) 1.0386(2) 0.33975(17) 0.0441(6) Uani 1 1 d . . . . .
H31 H 0.9560 0.9814 0.3037 0.053 Uiso 1 1 calc R U . . .
C32 C 0.9417(2) 1.1099(2) 0.40171(17) 0.0429(6) Uani 1 1 d . . . . .
H32 H 1.0235 1.1080 0.4137 0.051 Uiso 1 1 calc R U . . .
C33 C 0.8369(2) 1.1827(2) 0.44123(16) 0.0374(6) Uani 1 1 d . . . . .
N1 N -0.1921(2) 0.2895(2) 0.06687(14) 0.0409(5) Uani 1 1 d . . . . .
N2 N 0.0647(2) 0.3469(2) 0.14812(15) 0.0402(5) Uani 1 1 d . . . . .
N3 N 0.1961(2) 0.6011(2) 0.12065(14) 0.0408(5) Uani 1 1 d . . . . .
N4 N 0.3504(2) 0.8146(2) 0.39728(14) 0.0397(5) Uani 1 1 d . . . . .
N5 N 0.62411(19) 0.91572(19) 0.34226(14) 0.0378(5) Uani 1 1 d . . . . .
N6 N 0.7369(2) 1.1555(2) 0.40393(14) 0.0399(5) Uani 1 1 d . . . . .
H1N H -0.218(2) 0.365(3) 0.0654(17) 0.046(8) Uiso 1 1 d . . . . .
H2N H 0.054(2) 0.390(2) 0.1002(17) 0.047(8) Uiso 1 1 d . . . . .
H3N H 0.129(2) 0.640(2) 0.1063(15) 0.038(8) Uiso 1 1 d . . . . .
H4N H 0.321(2) 0.882(2) 0.4075(15) 0.026(7) Uiso 1 1 d . . . . .
H5N H 0.582(2) 0.949(2) 0.3924(18) 0.052(8) Uiso 1 1 d . . . . .
H6N H 0.662(2) 1.189(2) 0.4166(15) 0.037(7) Uiso 1 1 d . . . . .
Cl1 Cl 0.64711(8) 0.81782(8) 0.60656(5) 0.0648(2) Uani 1 1 d . . . . .
O1 O 0.7531(10) 0.7368(11) 0.5702(10) 0.111(4) Uani 0.591(8) 1 d D U P A 1
O2 O 0.6676(12) 0.8544(12) 0.6860(6) 0.169(6) Uani 0.591(8) 1 d D U P A 1
O3 O 0.5444(5) 0.7445(6) 0.6220(8) 0.176(4) Uani 0.591(8) 1 d D U P A 1
O4 O 0.6065(8) 0.9196(5) 0.5545(4) 0.092(3) Uani 0.591(8) 1 d D U P A 1
O1A O 0.7079(13) 0.7125(12) 0.5731(14) 0.088(4) Uani 0.409(8) 1 d D U P A 2
O2A O 0.7399(6) 0.9108(6) 0.5817(7) 0.119(4) Uani 0.409(8) 1 d D U P A 2
O3A O 0.6053(15) 0.8170(14) 0.6916(6) 0.143(9) Uani 0.409(8) 1 d D U P A 2
O4A O 0.5505(7) 0.8746(11) 0.5579(7) 0.087(3) Uani 0.409(8) 1 d D U P A 2
Cl2 Cl -0.17996(8) 0.65316(8) 0.11065(5) 0.0626(2) Uani 1 1 d . . . . .
O5 O -0.2605(13) 0.7503(11) 0.0824(11) 0.126(5) Uani 0.545(11) 1 d D U P B 1
O6 O -0.0955(8) 0.7080(12) 0.1553(11) 0.197(6) Uani 0.545(11) 1 d D U P B 1
O7 O -0.2450(10) 0.5828(10) 0.1701(8) 0.165(6) Uani 0.545(11) 1 d D U P B 1
O8 O -0.1055(12) 0.5810(10) 0.0487(7) 0.123(5) Uani 0.545(11) 1 d D U P B 1
O5A O -0.2340(15) 0.7709(11) 0.0956(11) 0.112(5) Uani 0.455(11) 1 d D U P B 2
O6A O -0.1674(12) 0.6223(10) 0.1972(4) 0.110(5) Uani 0.455(11) 1 d D U P B 2
O7A O -0.2653(7) 0.5745(7) 0.0832(11) 0.141(5) Uani 0.455(11) 1 d D U P B 2
O8A O -0.0676(9) 0.6181(15) 0.0548(10) 0.114(6) Uani 0.455(11) 1 d D U 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
C1 C2 1.510(4) . ?
C2 C5 1.557(4) . ?
C3 C4 1.515(4) . ?
C4 C5 1.550(4) . ?
C5 C6 1.509(3) . ?
C5 C17 1.509(3) 2_565 ?
C6 C7 1.363(3) . ?
C6 N1 1.372(3) . ?
C7 C8 1.409(4) . ?
C8 C9 1.369(3) . ?
C9 N1 1.371(3) . ?
C9 C10 1.478(3) . ?
C10 N2 1.514(3) . ?
C12 N2 1.483(3) . ?
C13 C14 1.475(3) . ?
C13 N2 1.521(3) . ?
C14 C15 1.360(4) . ?
C14 N3 1.368(3) . ?
C15 C16 1.405(4) . ?
C16 C17 1.362(3) . ?
C17 N3 1.370(3) . ?
C17 C5 1.509(3) 2_565 ?
C18 C19 1.523(4) . ?
C19 C22 1.552(4) . ?
C20 C21 1.507(5) . ?
C21 C22 1.545(4) . ?
C22 C23 1.508(3) . ?
C22 C33 1.509(3) 2_676 ?
C23 N4 1.369(3) . ?
C23 C24 1.369(3) . ?
C24 C25 1.399(4) . ?
C25 C26 1.364(4) . ?
C26 N4 1.371(3) . ?
C26 C27 1.472(3) . ?
C27 N5 1.519(3) . ?
C28 N5 1.485(3) . ?
C29 C30 1.479(3) . ?
C29 N5 1.516(3) . ?
C30 C31 1.360(3) . ?
C30 N6 1.369(3) . ?
C31 C32 1.410(3) . ?
C32 C33 1.372(3) . ?
C33 N6 1.376(3) . ?
C33 C22 1.509(3) 2_676 ?
Cl1 O3A 1.317(9) . ?
Cl1 O1A 1.331(12) . ?
Cl1 O2 1.369(8) . ?
Cl1 O4 1.387(6) . ?
Cl1 O1 1.410(10) . ?
Cl1 O4A 1.429(9) . ?
Cl1 O3 1.439(5) . ?
Cl1 O2A 1.515(7) . ?
Cl2 O7 1.334(6) . ?
Cl2 O5A 1.354(12) . ?
Cl2 O8 1.363(9) . ?
Cl2 O5 1.367(10) . ?
Cl2 O6A 1.376(6) . ?
Cl2 O8A 1.397(11) . ?
Cl2 O6 1.437(6) . ?
Cl2 O7A 1.468(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 C2 C5 115.8(2) . . ?
C3 C4 C5 114.9(3) . . ?
C6 C5 C17 111.6(2) . 2_565 ?
C6 C5 C4 107.9(2) . . ?
C17 C5 C4 108.8(2) 2_565 . ?
C6 C5 C2 110.2(2) . . ?
C17 C5 C2 109.0(2) 2_565 . ?
C4 C5 C2 109.3(2) . . ?
C7 C6 N1 106.8(2) . . ?
C7 C6 C5 131.6(2) . . ?
N1 C6 C5 120.9(2) . . ?
C6 C7 C8 108.1(2) . . ?
C9 C8 C7 107.9(2) . . ?
C8 C9 N1 106.7(2) . . ?
C8 C9 C10 131.5(2) . . ?
N1 C9 C10 121.8(2) . . ?
C9 C10 N2 113.7(2) . . ?
C14 C13 N2 113.0(2) . . ?
C15 C14 N3 107.2(2) . . ?
C15 C14 C13 131.5(3) . . ?
N3 C14 C13 121.3(2) . . ?
C14 C15 C16 107.8(2) . . ?
C17 C16 C15 108.2(2) . . ?
C16 C17 N3 106.8(2) . . ?
C16 C17 C5 130.0(2) . 2_565 ?
N3 C17 C5 122.9(2) . 2_565 ?
C18 C19 C22 115.3(2) . . ?
C20 C21 C22 116.0(3) . . ?
C23 C22 C33 112.0(2) . 2_676 ?
C23 C22 C21 110.6(2) . . ?
C33 C22 C21 109.0(2) 2_676 . ?
C23 C22 C19 108.5(2) . . ?
C33 C22 C19 107.4(2) 2_676 . ?
C21 C22 C19 109.3(2) . . ?
N4 C23 C24 106.4(2) . . ?
N4 C23 C22 121.8(2) . . ?
C24 C23 C22 131.4(2) . . ?
C23 C24 C25 108.1(2) . . ?
C26 C25 C24 108.3(2) . . ?
C25 C26 N4 106.5(2) . . ?
C25 C26 C27 130.7(2) . . ?
N4 C26 C27 122.8(2) . . ?
C26 C27 N5 113.0(2) . . ?
C30 C29 N5 113.2(2) . . ?
C31 C30 N6 107.2(2) . . ?
C31 C30 C29 130.2(2) . . ?
N6 C30 C29 122.6(2) . . ?
C30 C31 C32 108.0(2) . . ?
C33 C32 C31 108.1(2) . . ?
C32 C33 N6 106.3(2) . . ?
C32 C33 C22 130.5(2) . 2_676 ?
N6 C33 C22 123.1(2) . 2_676 ?
C9 N1 C6 110.5(2) . . ?
C12 N2 C10 112.5(2) . . ?
C12 N2 C13 111.2(2) . . ?
C10 N2 C13 110.16(19) . . ?
C14 N3 C17 110.1(2) . . ?
C23 N4 C26 110.6(2) . . ?
C28 N5 C29 111.6(2) . . ?
C28 N5 C27 111.8(2) . . ?
C29 N5 C27 109.73(19) . . ?
C30 N6 C33 110.5(2) . . ?
O3A Cl1 O1A 117.7(10) . . ?
O2 Cl1 O4 110.8(6) . . ?
O2 Cl1 O1 109.0(8) . . ?
O4 Cl1 O1 117.4(7) . . ?
O3A Cl1 O4A 110.5(8) . . ?
O1A Cl1 O4A 113.1(10) . . ?
O2 Cl1 O3 108.3(6) . . ?
O4 Cl1 O3 105.4(4) . . ?
O1 Cl1 O3 105.5(5) . . ?
O3A Cl1 O2A 111.0(8) . . ?
O1A Cl1 O2A 104.2(7) . . ?
O4A Cl1 O2A 98.5(5) . . ?
O7 Cl2 O8 110.2(7) . . ?
O7 Cl2 O5 109.2(8) . . ?
O8 Cl2 O5 118.0(8) . . ?
O5A Cl2 O6A 114.8(8) . . ?
O5A Cl2 O8A 114.5(9) . . ?
O6A Cl2 O8A 111.2(7) . . ?
O7 Cl2 O6 107.3(8) . . ?
O8 Cl2 O6 106.0(6) . . ?
O5 Cl2 O6 105.6(7) . . ?
O5A Cl2 O7A 104.7(8) . . ?
O6A Cl2 O7A 108.4(7) . . ?
O8A Cl2 O7A 102.1(6) . . ?

_refine_diff_density_max         0.296
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.039

_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_2f
_database_code_depnum_ccdc_archive 'CCDC 1455744'
_audit_update_record             
;
2016-06-13 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_THETM01_2f                  
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: The investigated crystal was diffracting comparably weakly.
In addition some substantial disorder is present. The measurement was 
set up to collect a full set of data. 
The high angle data, however, was dominated by noise [I/sigma(I) < 1.0] 
and consequently omitted. Even using Cu radiation could not circumvent 
this problem.
;
_vrf_PLAT412_2f                  
;
PROBLEM: Short Intra XH3 .. XHn H16A .. H17D .. 1.34 Ang.
RESPONSE: These alerts are generated because of the disorder in the structure. 
Short contacts between disordered fragments (in fact belonging to distinct 
molecules)are to be expected.
;
_vrf_PLAT019_2f                  
;
PROBLEM: _diffrn_measured_fraction_theta_full/*_max < 1.0 0.973 Report
RESPONSE: See above response to THETM01_ALERT_3_B
;
_vrf_PLAT090_2f                  
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........ 5.10 Note
RESPONSE: See above response to THETM01_ALERT_3_B
;
_vrf_PLAT353_2f                  
;
PROBLEM: Long N-H (N0.87,N1.01A) N2 - H2N .. 1.08 Ang.
RESPONSE: The respective Hydrogen is involved in strong hydrogen bonding
with the chromate as acceptor and slightly moved towards it.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H46 Cr N6 O4'
_chemical_formula_weight         630.75

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'
Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_H-M_alt        'C m c 21'
_space_group_name_Hall           'C 2c -2'

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

_cell_length_a                   17.1257(9)
_cell_length_b                   16.2367(9)
_cell_length_c                   11.2669(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3132.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    33664
_cell_measurement_theta_min      3.751
_cell_measurement_theta_max      59.969

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_F_000             1344
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    3.378
_shelx_estimated_absorpt_T_min   0.729
_shelx_estimated_absorpt_T_max   0.967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7287
_exptl_absorpt_correction_T_max  0.9670
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'MWPC area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            33664
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_av_R_equivalents  0.0845
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.751
_diffrn_reflns_theta_max         59.969
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             2405
_reflns_number_gt                1980
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.888
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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       APEX2
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    Diamond3.2
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0717P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.023(13)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2405
_refine_ls_number_parameters     252
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0449
_refine_ls_wR_factor_ref         0.1114
_refine_ls_wR_factor_gt          0.1091
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Cr1 Cr 0.0000 0.17154(7) 0.82686(11) 0.0268(4) Uani 1 2 d S T P . .
O1 O 0.0000 0.2031(3) 0.6849(5) 0.0313(13) Uani 1 2 d S T P A .
O2A O 0.0245(7) 0.2488(5) 0.9050(7) 0.057(5) Uani 0.5 1 d . . P A .
O3A O 0.0885(6) 0.1419(8) 0.8606(12) 0.045(3) Uani 0.5 1 d . U P A 1
O3B O 0.0623(7) 0.0985(6) 0.8399(12) 0.056(3) Uani 0.5 1 d . U P A 2
N1 N 0.0000 0.0576(4) 0.5527(6) 0.0287(15) Uani 1 2 d DS T P . .
H1N H 0.0000 0.108(4) 0.610(6) 0.034 Uiso 1 2 d DS U P . .
N2 N -0.1757(3) 0.1011(3) 0.6506(4) 0.0300(11) Uani 1 1 d D . . . .
H2N H -0.149(3) 0.115(4) 0.735(4) 0.036 Uiso 1 1 d D U . . .
N3 N -0.1733(3) 0.2908(3) 0.7316(4) 0.0363(13) Uani 1 1 d D . . . .
H3N H -0.141(3) 0.244(3) 0.773(6) 0.044 Uiso 1 1 d D U . . .
N4 N 0.0000 0.3694(4) 0.6968(6) 0.0330(17) Uani 1 2 d DS T P . .
H4N H 0.0000 0.304(3) 0.694(8) 0.040 Uiso 1 2 d DS U P . .
C1 C 0.0000 0.0880(5) 0.4304(8) 0.039(2) Uani 1 2 d S T P . .
H1A H 0.0458 0.1206 0.4160 0.059 Uiso 0.5 1 d R U P . .
H1B H 0.0000 0.0412 0.3782 0.059 Uiso 1 2 d R U P . .
C2 C -0.0720(3) 0.0058(4) 0.5801(7) 0.0358(14) Uani 1 1 d . . . . .
H2A H -0.0679 -0.0146 0.6598 0.043 Uiso 1 1 d R U . . .
H2B H -0.0717 -0.0411 0.5282 0.043 Uiso 1 1 d R U . . .
C3 C -0.1451(4) 0.0511(3) 0.5624(5) 0.0300(13) Uani 1 1 d . . . . .
C5 C -0.2436(3) 0.1379(4) 0.6091(6) 0.0312(14) Uani 1 1 d . . . . .
C6 C -0.2878(3) 0.1995(4) 0.6834(6) 0.0380(15) Uani 1 1 d . . . . .
C7 C -0.2452(4) 0.2810(3) 0.6791(5) 0.0347(15) Uani 1 1 d . . . . .
C8 C -0.1469(4) 0.3695(4) 0.7118(6) 0.0398(16) Uani 1 1 d . . . . .
C9 C -0.0713(3) 0.3999(4) 0.7624(6) 0.0410(16) Uani 1 1 d . . . . .
H9A H -0.0715 0.4590 0.7587 0.049 Uiso 1 1 d R U . . .
H9B H -0.0676 0.3848 0.8446 0.049 Uiso 1 1 d R U . . .
C10 C 0.0000 0.3930(6) 0.5701(8) 0.049(3) Uani 1 2 d S T P . .
H10A H 0.0457 0.3697 0.5342 0.074 Uiso 0.5 1 d R U P . .
H10C H 0.0000 0.4515 0.5585 0.074 Uiso 1 2 d R U P . .
C11 C -0.2633(4) 0.3548(4) 0.6264(6) 0.0411(17) Uani 1 1 d . . . . .
H11A H -0.3093 0.3662 0.5824 0.049 Uiso 1 1 calc R U . . .
C12 C -0.2027(4) 0.4100(4) 0.6485(6) 0.0463(18) Uani 1 1 d . . . . .
H12A H -0.2007 0.4659 0.6237 0.056 Uiso 1 1 calc R U . . .
C13 C -0.1941(4) 0.0555(4) 0.4661(6) 0.0390(16) Uani 1 1 d . . . . .
H13A H -0.1877 0.0271 0.3931 0.047 Uiso 1 1 calc R U . . .
C14 C -0.2555(4) 0.1097(4) 0.4946(6) 0.0387(16) Uani 1 1 d . . . . .
H14A H -0.2977 0.1244 0.4441 0.046 Uiso 1 1 calc R U . . .
C15 C -0.3696(4) 0.2106(5) 0.6262(7) 0.054(2) Uani 1 1 d . . . . .
H15A H -0.3635 0.2332 0.5481 0.065 Uiso 1 1 d R U . B -1
H15B H -0.3980 0.2500 0.6728 0.065 Uiso 1 1 d R U . B -1
C16 C -0.2942(4) 0.1693(4) 0.8136(7) 0.0499(18) Uani 1 1 d . . . . .
H16A H -0.3185 0.2125 0.8585 0.060 Uiso 1 1 d R U . C -1
H16B H -0.2422 0.1628 0.8440 0.060 Uiso 1 1 d R U . C -1
C17 C -0.3335(6) 0.0998(6) 0.8397(13) 0.044(4) Uani 0.546(16) 1 d . U P D -1
H17A H -0.3249 0.0855 0.9232 0.066 Uiso 0.546(16) 1 calc R U P D -1
H17B H -0.3148 0.0549 0.7891 0.066 Uiso 0.546(16) 1 calc R U P D -1
H17C H -0.3894 0.1085 0.8259 0.066 Uiso 0.546(16) 1 calc R U P D -1
C17' C -0.3545(7) 0.2171(8) 0.8801(12) 0.032(4) Uani 0.454(16) 1 d . U P D -2
H17D H -0.3535 0.2012 0.9639 0.048 Uiso 0.454(16) 1 calc R U P D -2
H17E H -0.4063 0.2054 0.8469 0.048 Uiso 0.454(16) 1 calc R U P D -2
H17F H -0.3435 0.2761 0.8729 0.048 Uiso 0.454(16) 1 calc R U P D -2
C18 C -0.4205(7) 0.2776(8) 0.7179(13) 0.042(4) Uani 0.465(14) 1 d . . P E -1
H18D H -0.3853 0.3211 0.7456 0.062 Uiso 0.465(14) 1 calc R U P E -1
H18E H -0.4410 0.2472 0.7863 0.062 Uiso 0.465(14) 1 calc R U P E -1
H18F H -0.4639 0.3022 0.6737 0.062 Uiso 0.465(14) 1 calc R U P E -1
C18' C -0.4237(7) 0.1261(7) 0.6194(13) 0.045(4) Uani 0.535(14) 1 d . . P E -2
H18A H -0.3921 0.0805 0.5888 0.068 Uiso 0.535(14) 1 calc R U P E -2
H18B H -0.4682 0.1356 0.5663 0.068 Uiso 0.535(14) 1 calc R U P E -2
H18C H -0.4429 0.1124 0.6989 0.068 Uiso 0.535(14) 1 calc R U P E -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
Cr1 O2A 1.589(8) . ?
Cr1 O2A 1.589(8) 3 ?
Cr1 O3B 1.601(10) 3 ?
Cr1 O3B 1.601(9) . ?
Cr1 O3A 1.634(10) 3 ?
Cr1 O3A 1.634(10) . ?
Cr1 O1 1.680(5) . ?
O2A O2A 0.84(2) 3 ?
N1 C1 1.464(10) . ?
N1 C2 1.525(6) 3 ?
N1 C2 1.525(6) . ?
N1 H1N 1.05(4) . ?
N2 C3 1.385(7) . ?
N2 C5 1.390(7) . ?
N2 H2N 1.07(4) . ?
N3 C8 1.374(8) . ?
N3 C7 1.376(8) . ?
N3 H3N 1.05(4) . ?
N4 C10 1.479(11) . ?
N4 C9 1.511(7) 3 ?
N4 C9 1.511(7) . ?
N4 H4N 1.06(4) . ?
C1 H1A 0.9598 . ?
C1 H1B 0.9600 . ?
C2 C3 1.466(8) . ?
C2 H2A 0.9601 . ?
C2 H2B 0.9601 . ?
C3 C13 1.374(9) . ?
C5 C14 1.384(9) . ?
C5 C6 1.506(9) . ?
C6 C7 1.511(9) . ?
C6 C16 1.551(9) . ?
C6 C15 1.553(9) . ?
C7 C11 1.373(9) . ?
C8 C12 1.361(9) . ?
C8 C9 1.498(9) . ?
C9 H9A 0.9601 . ?
C9 H9B 0.9602 . ?
C10 H10A 0.9587 . ?
C10 H10C 0.9586 . ?
C11 C12 1.393(10) . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9500 . ?
C13 C14 1.408(9) . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?
C15 C18' 1.657(14) . ?
C15 C18 1.735(14) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9601 . ?
C16 C17 1.346(12) . ?
C16 C17' 1.494(14) . ?
C16 H16A 0.9599 . ?
C16 H16B 0.9600 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C17' H17D 0.9800 . ?
C17' H17E 0.9800 . ?
C17' H17F 0.9800 . ?
C18 H15B 0.7790 . ?
C18 H18D 0.9800 . ?
C18 H18E 0.9800 . ?
C18 H18F 0.9800 . ?
C18' H18A 0.9800 . ?
C18' H18B 0.9800 . ?
C18' H18C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2A Cr1 O2A 30.6(8) . 3 ?
O2A Cr1 O3B 135.2(7) . 3 ?
O2A Cr1 O3B 111.0(7) 3 3 ?
O2A Cr1 O3B 111.0(7) . . ?
O2A Cr1 O3B 135.2(7) 3 . ?
O3B Cr1 O3B 83.5(9) 3 . ?
O2A Cr1 O3A 110.4(6) . 3 ?
O2A Cr1 O3A 81.9(6) 3 3 ?
O2A Cr1 O3A 81.9(6) . . ?
O2A Cr1 O3A 110.4(6) 3 . ?
O3A Cr1 O3A 135.9(9) 3 . ?
O2A Cr1 O1 106.7(3) . . ?
O2A Cr1 O1 106.7(3) 3 . ?
O3B Cr1 O1 108.3(5) 3 . ?
O3B Cr1 O1 108.3(5) . . ?
O3A Cr1 O1 108.2(5) 3 . ?
O3A Cr1 O1 108.2(5) . . ?
O2A O2A Cr1 74.7(4) 3 . ?
C1 N1 C2 112.1(4) . 3 ?
C1 N1 C2 112.1(4) . . ?
C2 N1 C2 108.0(6) 3 . ?
C1 N1 H1N 109(5) . . ?
C2 N1 H1N 108(2) 3 . ?
C2 N1 H1N 108(2) . . ?
C3 N2 C5 109.1(5) . . ?
C3 N2 H2N 127(3) . . ?
C5 N2 H2N 124(3) . . ?
C8 N3 C7 109.4(5) . . ?
C8 N3 H3N 125(3) . . ?
C7 N3 H3N 125(3) . . ?
C10 N4 C9 112.7(4) . 3 ?
C10 N4 C9 112.7(4) . . ?
C9 N4 C9 107.9(6) 3 . ?
C10 N4 H4N 103(5) . . ?
C9 N4 H4N 110(2) 3 . ?
C9 N4 H4N 110(2) . . ?
N1 C1 H1A 110.2 . . ?
N1 C1 H1B 108.1 . . ?
H1A C1 H1B 109.5 . . ?
C3 C2 N1 112.7(5) . . ?
C3 C2 H2A 111.3 . . ?
N1 C2 H2A 108.6 . . ?
C3 C2 H2B 108.7 . . ?
N1 C2 H2B 108.0 . . ?
H2A C2 H2B 107.2 . . ?
C13 C3 N2 107.8(5) . . ?
C13 C3 C2 130.9(6) . . ?
N2 C3 C2 121.3(6) . . ?
C14 C5 N2 107.1(6) . . ?
C14 C5 C6 131.5(6) . . ?
N2 C5 C6 121.3(5) . . ?
C5 C6 C7 108.7(5) . . ?
C5 C6 C16 110.6(5) . . ?
C7 C6 C16 109.9(6) . . ?
C5 C6 C15 107.5(6) . . ?
C7 C6 C15 108.7(5) . . ?
C16 C6 C15 111.4(5) . . ?
C11 C7 N3 106.6(6) . . ?
C11 C7 C6 132.0(6) . . ?
N3 C7 C6 121.4(5) . . ?
C12 C8 N3 107.7(6) . . ?
C12 C8 C9 130.3(6) . . ?
N3 C8 C9 121.9(6) . . ?
C8 C9 N4 113.9(5) . . ?
C8 C9 H9A 108.0 . . ?
N4 C9 H9A 108.1 . . ?
C8 C9 H9B 109.9 . . ?
N4 C9 H9B 109.5 . . ?
H9A C9 H9B 107.2 . . ?
N4 C10 H10A 107.8 . . ?
N4 C10 H10C 112.9 . . ?
H10A C10 H10C 109.4 . . ?
C7 C11 C12 108.5(6) . . ?
C7 C11 H11A 125.8 . . ?
C12 C11 H11A 125.8 . . ?
C8 C12 C11 107.8(6) . . ?
C8 C12 H12A 126.1 . . ?
C11 C12 H12A 126.1 . . ?
C3 C13 C14 108.0(5) . . ?
C3 C13 H13A 126.0 . . ?
C14 C13 H13A 126.0 . . ?
C5 C14 C13 108.0(6) . . ?
C5 C14 H14A 126.0 . . ?
C13 C14 H14A 126.0 . . ?
C6 C15 C18' 115.3(7) . . ?
C6 C15 C18 106.2(7) . . ?
C6 C15 H15A 109.0 . . ?
C18 C15 H15A 111.2 . . ?
C6 C15 H15B 107.9 . . ?
C18 C15 H15B 3.6 . . ?
H15A C15 H15B 107.6 . . ?
C17 C16 C6 120.5(9) . . ?
C17' C16 C6 111.0(7) . . ?
C17 C16 H16A 106.3 . . ?
C6 C16 H16A 107.3 . . ?
C17 C16 H16B 107.1 . . ?
C6 C16 H16B 107.8 . . ?
H16A C16 H16B 107.2 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C17' H17D 109.5 . . ?
C16 C17' H17E 109.5 . . ?
H17D C17' H17E 109.5 . . ?
C16 C17' H17F 109.5 . . ?
H17D C17' H17F 109.5 . . ?
H17E C17' H17F 109.5 . . ?
C15 C18 H15B 4.5 . . ?
C15 C18 H18D 109.5 . . ?
H15B C18 H18D 108.6 . . ?
C15 C18 H18E 109.5 . . ?
H15B C18 H18E 113.7 . . ?
H18D C18 H18E 109.5 . . ?
C15 C18 H18F 109.5 . . ?
H15B C18 H18F 106.1 . . ?
H18D C18 H18F 109.5 . . ?
H18E C18 H18F 109.5 . . ?
C15 C18' H18A 109.5 . . ?
C15 C18' H18B 109.5 . . ?
H18A C18' H18B 109.5 . . ?
C15 C18' H18C 109.5 . . ?
H18A C18' H18C 109.5 . . ?
H18B C18' H18C 109.5 . . ?

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
O3B Cr1 O2A O2A -45.3(7) 3 . . 3 ?
O3B Cr1 O2A O2A -147.6(5) . . . 3 ?
O3A Cr1 O2A O2A -22.6(5) 3 . . 3 ?
O3A Cr1 O2A O2A -158.7(4) . . . 3 ?
O1 Cr1 O2A O2A 94.70(16) . . . 3 ?
C1 N1 C2 C3 -58.9(7) . . . . ?
C2 N1 C2 C3 177.2(4) 3 . . . ?
C5 N2 C3 C13 -0.7(6) . . . . ?
C5 N2 C3 C2 178.4(5) . . . . ?
N1 C2 C3 C13 94.3(8) . . . . ?
N1 C2 C3 N2 -84.6(7) . . . . ?
C3 N2 C5 C14 0.5(6) . . . . ?
C3 N2 C5 C6 -176.7(5) . . . . ?
C14 C5 C6 C7 -99.6(8) . . . . ?
N2 C5 C6 C7 76.9(7) . . . . ?
C14 C5 C6 C16 139.7(7) . . . . ?
N2 C5 C6 C16 -43.8(7) . . . . ?
C14 C5 C6 C15 17.9(9) . . . . ?
N2 C5 C6 C15 -165.6(5) . . . . ?
C8 N3 C7 C11 -0.1(7) . . . . ?
C8 N3 C7 C6 178.3(5) . . . . ?
C5 C6 C7 C11 109.7(7) . . . . ?
C16 C6 C7 C11 -129.2(7) . . . . ?
C15 C6 C7 C11 -7.0(9) . . . . ?
C5 C6 C7 N3 -68.2(7) . . . . ?
C16 C6 C7 N3 52.9(7) . . . . ?
C15 C6 C7 N3 175.1(6) . . . . ?
C7 N3 C8 C12 1.0(7) . . . . ?
C7 N3 C8 C9 177.5(5) . . . . ?
C12 C8 C9 N4 -107.3(8) . . . . ?
N3 C8 C9 N4 77.0(8) . . . . ?
C10 N4 C9 C8 58.7(7) . . . . ?
C9 N4 C9 C8 -176.2(4) 3 . . . ?
N3 C7 C11 C12 -0.9(7) . . . . ?
C6 C7 C11 C12 -179.0(7) . . . . ?
N3 C8 C12 C11 -1.5(7) . . . . ?
C9 C8 C12 C11 -177.6(7) . . . . ?
C7 C11 C12 C8 1.5(7) . . . . ?
N2 C3 C13 C14 0.6(6) . . . . ?
C2 C3 C13 C14 -178.5(6) . . . . ?
N2 C5 C14 C13 -0.2(7) . . . . ?
C6 C5 C14 C13 176.7(6) . . . . ?
C3 C13 C14 C5 -0.2(7) . . . . ?
C5 C6 C15 C18' 60.7(8) . . . . ?
C7 C6 C15 C18' 178.2(7) . . . . ?
C16 C6 C15 C18' -60.6(9) . . . . ?
C5 C6 C15 C18 177.0(6) . . . . ?
C7 C6 C15 C18 -65.5(8) . . . . ?
C16 C6 C15 C18 55.8(8) . . . . ?
C5 C6 C16 C17 -63.4(9) . . . . ?
C7 C6 C16 C17 176.6(7) . . . . ?
C15 C6 C16 C17 56.0(9) . . . . ?
C5 C6 C16 C17' -165.0(7) . . . . ?
C7 C6 C16 C17' 75.0(8) . . . . ?
C15 C6 C16 C17' -45.6(9) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1N O1 1.05(4) 1.75(5) 2.793(8) 170(7) .
N3 H3N O2A 1.05(4) 2.49(6) 3.283(11) 132(4) 3
N4 H4N O1 1.06(4) 1.65(4) 2.702(8) 178(8) .
N4 H4N O2A 1.06(4) 2.58(8) 3.084(11) 109(5) .
N4 H4N O2A 1.06(4) 2.58(8) 3.084(11) 109(5) 3
N2 H2N O3A 1.07(4) 1.81(4) 2.876(14) 169(5) 3
N2 H2N O3B 1.07(4) 1.92(5) 2.885(13) 147(5) 3
N3 H3N O3A 1.05(4) 2.12(5) 3.174(13) 173(5) 3

_refine_diff_density_max         0.212
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.055

_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_2g
_database_code_depnum_ccdc_archive 'CCDC 1455745'
_audit_update_record             
;
2016-06-13 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_CHEMW03_2g                  
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: This is due to the use of SQUEEZE/PLATON and including
the diffuse and not refined solvent (nine water molecules)in the 
formula. 
;
_vrf_THETM01_2g                  
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: A full set of data was collected. However, data dominated 
by noise was omitted. Subtantial disorder in the structure is 
responsible, involving the whole dichromate ion and nine water molecules, 
with the latter not having been refined at all but "squeezed out".
;
_vrf_PLAT019_2g                  
;
PROBLEM: _diffrn_measured_fraction_theta_full/*_max < 1.0 0.833 Report
RESPONSE: see response to THETM01_ALERT_3_B
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32H48N6, Cr2O7, 9 H2O'
_chemical_formula_sum            'C32 H66 Cr2 N6 O16'
_chemical_formula_weight         894.90

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'
Cr Cr -0.1635 2.4439 '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                   8.815(3)
_cell_length_b                   17.954(6)
_cell_length_c                   26.463(9)
_cell_angle_alpha                90
_cell_angle_beta                 96.493(11)
_cell_angle_gamma                90
_cell_volume                     4162(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    27489
_cell_measurement_theta_min      2.980
_cell_measurement_theta_max      59.983

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_F_000             1904
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    4.943
_shelx_estimated_absorpt_T_min   0.638
_shelx_estimated_absorpt_T_max   0.952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6378
_exptl_absorpt_correction_T_max  0.9522
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'MWPC area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27489
_diffrn_reflns_av_unetI/netI     0.1610
_diffrn_reflns_av_R_equivalents  0.1608
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.980
_diffrn_reflns_theta_max         59.983
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measured_fraction_theta_full 0.785
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_Laue_measured_fraction_full 0.785
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_point_group_measured_fraction_full 0.785
_reflns_number_total             5821
_reflns_number_gt                2916
_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       APEX2
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    Diamond3.2
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'


_refine_special_details          
;
 ?
;

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.035 0.500 0.000 487 179 ' '
2 0.016 1.000 0.500 487 180 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The SQUEEZE/PLATON procedure yielded total void volume and electron 
count of 920.0Å³ and 360 e, respectively. It was concluded that
9 molecules water are present per formula which could not be refined.
The fraction of solvent has been treated as a diffuse contribution 
to the overall scattering without specific atom positions.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0611P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5821
_refine_ls_number_parameters     476
_refine_ls_number_restraints     234
_refine_ls_R_factor_all          0.1435
_refine_ls_R_factor_gt           0.0760
_refine_ls_wR_factor_ref         0.1791
_refine_ls_wR_factor_gt          0.1535
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_restrained_S_all      0.909
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Cr1 Cr -0.07416(14) 0.29607(11) 0.23412(6) 0.0386(6) Uani 0.858(7) 1 d D U P A
1
Cr2 Cr 0.06292(16) 0.45402(10) 0.23667(6) 0.0409(6) Uani 0.858(7) 1 d D U P A 1
O1 O -0.2310(5) 0.2599(4) 0.2491(2) 0.0542(16) Uani 0.858(7) 1 d D U P A 1
O2 O -0.0558(6) 0.2798(3) 0.1758(2) 0.0520(15) Uani 0.858(7) 1 d D U P A 1
O3 O 0.0686(8) 0.2624(5) 0.2697(3) 0.046(2) Uani 0.858(7) 1 d D U P A 1
O4 O -0.0951(5) 0.3917(3) 0.2400(2) 0.0501(15) Uani 0.858(7) 1 d D U P A 1
O5 O 0.1594(7) 0.4280(3) 0.1922(2) 0.0648(18) Uani 0.858(7) 1 d D U P A 1
O6 O -0.0067(7) 0.5336(3) 0.2237(3) 0.0692(19) Uani 0.858(7) 1 d D U P A 1
O7 O 0.1696(6) 0.4553(3) 0.2908(2) 0.0663(19) Uani 0.858(7) 1 d D U P A 1
Cr1' Cr -0.055(2) 0.3252(14) 0.2456(8) 0.123(8) Uiso 0.142(7) 1 d D U P A 2
Cr2' Cr 0.101(3) 0.4782(15) 0.2414(10) 0.165(10) Uiso 0.142(7) 1 d D U P A 2
O1' O -0.224(4) 0.298(3) 0.2560(18) 0.093(17) Uiso 0.142(7) 1 d D U P A 2
O2' O -0.037(5) 0.320(3) 0.1860(10) 0.093(16) Uiso 0.142(7) 1 d D U P A 2
O3' O 0.069(6) 0.272(3) 0.277(2) 0.07(2) Uiso 0.142(7) 1 d D U P A 2
O4' O -0.044(4) 0.4176(16) 0.2607(15) 0.109(12) Uiso 0.142(7) 1 d D U P A 2
O5' O 0.229(5) 0.430(3) 0.219(2) 0.15(2) Uiso 0.142(7) 1 d D U P A 2
O6' O 0.022(6) 0.528(2) 0.1959(15) 0.13(2) Uiso 0.142(7) 1 d D U P A 2
O7' O 0.166(5) 0.529(3) 0.2897(14) 0.135(18) Uiso 0.142(7) 1 d D U P A 2
N1 N 0.2392(6) 0.3356(3) 0.3673(2) 0.0410(13) Uani 1 1 d D . . . .
H1N H 0.193(6) 0.366(3) 0.3447(19) 0.049 Uiso 1 1 d D U . . .
N2 N 0.3902(5) 0.2687(3) 0.27268(19) 0.0413(13) Uani 1 1 d . . . . .
H2 H 0.2771 0.2652 0.2731 0.050 Uiso 1 1 calc R U . . .
N3 N 0.2439(5) 0.2103(3) 0.1666(2) 0.0408(13) Uani 1 1 d D . . . .
H3N H 0.159(5) 0.233(3) 0.172(2) 0.049 Uiso 1 1 d D U . . .
N4 N 0.0530(6) 0.0519(3) 0.1939(2) 0.0445(14) Uani 1 1 d D . . . .
H4N H 0.146(4) 0.037(3) 0.204(2) 0.053 Uiso 1 1 d D U . . .
N5 N -0.0283(6) 0.0513(3) 0.3151(2) 0.0478(14) Uani 1 1 d D . . . .
H5N H -0.042(7) 0.027(3) 0.3428(17) 0.057 Uiso 1 1 d D U . . .
N6 N -0.0595(5) 0.2180(3) 0.36591(19) 0.0406(13) Uani 1 1 d D . . . .
H6N H -0.017(6) 0.233(3) 0.3392(17) 0.049 Uiso 1 1 d D U . . .
C1 C 0.0330(6) 0.3208(3) 0.4257(2) 0.0331(15) Uani 1 1 d . . . . .
C2 C 0.1917(7) 0.3111(3) 0.4114(2) 0.0415(16) Uani 1 1 d . . . . .
C3 C 0.3127(7) 0.2692(4) 0.4349(3) 0.0490(18) Uani 1 1 d . . . . .
H3A H 0.3136 0.2439 0.4664 0.059 Uiso 1 1 calc R U . . .
C4 C 0.4335(7) 0.2701(4) 0.4043(3) 0.0502(18) Uani 1 1 d . . . . .
H4A H 0.5304 0.2470 0.4118 0.060 Uiso 1 1 calc R U . . .
C5 C 0.3852(6) 0.3103(3) 0.3623(2) 0.0358(15) Uani 1 1 d . . . . .
C6 C 0.4478(7) 0.3268(4) 0.3138(2) 0.0469(18) Uani 1 1 d . . . . .
H6A H 0.5608 0.3257 0.3193 0.056 Uiso 1 1 calc R U . . .
H6B H 0.4158 0.3773 0.3020 0.056 Uiso 1 1 calc R U . . .
C7 C 0.4152(7) 0.2950(4) 0.2205(2) 0.0486(18) Uani 1 1 d . . . . .
H7A H 0.3469 0.3378 0.2111 0.058 Uiso 1 1 calc R U . . .
H7B H 0.5218 0.3126 0.2210 0.058 Uiso 1 1 calc R U . . .
C8 C 0.3865(7) 0.2371(3) 0.1825(2) 0.0432(16) Uani 1 1 d . . . . .
C9 C 0.4890(7) 0.1911(4) 0.1609(3) 0.0526(19) Uani 1 1 d . . . . .
H9A H 0.5968 0.1969 0.1646 0.063 Uiso 1 1 calc R U . . .
C10 C 0.4076(7) 0.1351(4) 0.1329(3) 0.0494(18) Uani 1 1 d . . . . .
H10A H 0.4481 0.0954 0.1149 0.059 Uiso 1 1 calc R U . . .
C11 C 0.2572(7) 0.1495(4) 0.1371(2) 0.0452(17) Uani 1 1 d . . . . .
C12 C 0.1196(7) 0.1094(4) 0.1112(2) 0.0467(17) Uani 1 1 d . . . . .
C13 C 0.0048(7) 0.0895(4) 0.1509(3) 0.0422(16) Uani 1 1 d . . . . .
C14 C -0.1486(6) 0.1019(3) 0.1494(2) 0.0419(16) Uani 1 1 d . . . . .
H14A H -0.2113 0.1280 0.1237 0.050 Uiso 1 1 calc R U . . .
C15 C -0.1967(8) 0.0684(4) 0.1935(3) 0.0499(18) Uani 1 1 d . . . . .
H15A H -0.2978 0.0671 0.2027 0.060 Uiso 1 1 calc R U . . .
C16 C -0.0678(7) 0.0379(4) 0.2205(3) 0.0451(17) Uani 1 1 d . . . . .
C17 C -0.0553(7) 0.0007(4) 0.2701(3) 0.0470(17) Uani 1 1 d . . . . .
H17A H 0.0295 -0.0356 0.2716 0.056 Uiso 1 1 calc R U . . .
H17B H -0.1505 -0.0276 0.2726 0.056 Uiso 1 1 calc R U . . .
C18 C -0.1586(7) 0.1072(4) 0.3179(3) 0.0516(19) Uani 1 1 d . . . . .
H18A H -0.1655 0.1399 0.2876 0.062 Uiso 1 1 calc R U . . .
H18B H -0.2562 0.0797 0.3172 0.062 Uiso 1 1 calc R U . . .
C19 C -0.1369(7) 0.1534(4) 0.3640(3) 0.0420(16) Uani 1 1 d . . . . .
C20 C -0.1857(8) 0.1422(4) 0.4107(3) 0.058(2) Uani 1 1 d . . . . .
H20A H -0.2428 0.1009 0.4206 0.069 Uiso 1 1 calc R U . . .
C21 C -0.1348(7) 0.2038(4) 0.4415(2) 0.0456(17) Uani 1 1 d . . . . .
H21A H -0.1523 0.2119 0.4759 0.055 Uiso 1 1 calc R U . . .
C22 C -0.0558(6) 0.2495(3) 0.4125(2) 0.0363(15) Uani 1 1 d . . . . .
C23 C -0.0441(7) 0.3869(3) 0.3929(3) 0.0456(17) Uani 1 1 d . . . . .
H23A H 0.0212 0.4317 0.3984 0.055 Uiso 1 1 calc R U . . .
H23B H -0.0499 0.3735 0.3565 0.055 Uiso 1 1 calc R U . . .
C24 C -0.2007(7) 0.4054(4) 0.4055(3) 0.057(2) Uani 1 1 d . . . . .
H24A H -0.2423 0.4467 0.3840 0.086 Uiso 1 1 calc R U . . .
H24B H -0.1956 0.4200 0.4414 0.086 Uiso 1 1 calc R U . . .
H24C H -0.2668 0.3617 0.3995 0.086 Uiso 1 1 calc R U . . .
C25 C 0.0384(7) 0.3371(4) 0.4824(2) 0.0474(17) Uani 1 1 d . . . . .
H25A H 0.0902 0.2950 0.5013 0.057 Uiso 1 1 calc R U . . .
H25B H -0.0677 0.3389 0.4912 0.057 Uiso 1 1 calc R U . . .
C26 C 0.1201(7) 0.4103(4) 0.5011(3) 0.0539(19) Uani 1 1 d . . . . .
H26A H 0.1172 0.4154 0.5379 0.081 Uiso 1 1 calc R U . . .
H26B H 0.0682 0.4528 0.4836 0.081 Uiso 1 1 calc R U . . .
H26C H 0.2266 0.4088 0.4938 0.081 Uiso 1 1 calc R U . . .
C27 C 0.4522(7) 0.1928(4) 0.2849(3) 0.0547(19) Uani 1 1 d . . . . .
H27A H 0.4320 0.1789 0.3193 0.082 Uiso 1 1 calc R U . . .
H27B H 0.5625 0.1926 0.2830 0.082 Uiso 1 1 calc R U . . .
H27C H 0.4028 0.1569 0.2604 0.082 Uiso 1 1 calc R U . . .
C28 C 0.0360(7) 0.1610(5) 0.0724(3) 0.067(2) Uani 1 1 d . . . . .
H28A H -0.0533 0.1343 0.0549 0.080 Uiso 1 1 calc R U . . .
H28B H -0.0029 0.2041 0.0904 0.080 Uiso 1 1 calc R U . . .
C29 C 0.1318(8) 0.1897(6) 0.0328(3) 0.087(3) Uani 1 1 d . . . . .
H29A H 0.0699 0.2226 0.0092 0.130 Uiso 1 1 calc R U . . .
H29B H 0.1686 0.1477 0.0140 0.130 Uiso 1 1 calc R U . . .
H29C H 0.2191 0.2175 0.0495 0.130 Uiso 1 1 calc R U . . .
C30 C 0.1665(8) 0.0323(4) 0.0881(3) 0.0558(19) Uani 1 1 d . . . . .
H30A H 0.2274 0.0426 0.0597 0.067 Uiso 1 1 calc R U . . .
H30B H 0.2331 0.0052 0.1146 0.067 Uiso 1 1 calc R U . . .
C31 C 0.0364(9) -0.0174(4) 0.0691(3) 0.070(2) Uani 1 1 d . . . . .
H31A H 0.0761 -0.0634 0.0557 0.105 Uiso 1 1 calc R U . . .
H31B H -0.0290 0.0081 0.0420 0.105 Uiso 1 1 calc R U . . .
H31C H -0.0233 -0.0294 0.0971 0.105 Uiso 1 1 calc R U . . .
C32 C 0.1244(8) 0.0874(4) 0.3177(3) 0.064(2) Uani 1 1 d . . . . .
H32A H 0.1390 0.1201 0.3475 0.097 Uiso 1 1 calc R U . . .
H32B H 0.1307 0.1169 0.2868 0.097 Uiso 1 1 calc R U . . .
H32C H 0.2039 0.0490 0.3204 0.097 Uiso 1 1 calc R U . . .


_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
Cr1 O2 1.598(6) . ?
Cr1 O3 1.602(5) . ?
Cr1 O1 1.616(5) . ?
Cr1 O4 1.736(6) . ?
Cr2 O6 1.578(5) . ?
Cr2 O5 1.597(6) . ?
Cr2 O7 1.623(6) . ?
Cr2 O4 1.797(5) . ?
Cr1' O3' 1.600(17) . ?
Cr1' O2' 1.606(18) . ?
Cr1' O1' 1.621(18) . ?
Cr1' O4' 1.707(18) . ?
Cr2' O6' 1.591(18) . ?
Cr2' O5' 1.592(18) . ?
Cr2' O7' 1.617(18) . ?
Cr2' O4' 1.799(18) . ?
N1 C2 1.357(8) . ?
N1 C5 1.385(7) . ?
N1 H1N 0.88(3) . ?
N2 C27 1.491(8) . ?
N2 C7 1.499(8) . ?
N2 C6 1.551(7) . ?
N2 H2 1.0000 . ?
N3 C11 1.354(8) . ?
N3 C8 1.367(7) . ?
N3 H3N 0.88(3) . ?
N4 C13 1.349(8) . ?
N4 C16 1.365(8) . ?
N4 H4N 0.88(3) . ?
N5 C32 1.489(8) . ?
N5 C17 1.496(8) . ?
N5 C18 1.532(8) . ?
N5 H5N 0.87(3) . ?
N6 C19 1.344(8) . ?
N6 C22 1.354(7) . ?
N6 H6N 0.88(3) . ?
C1 C2 1.500(8) . ?
C1 C22 1.521(8) . ?
C1 C25 1.523(8) . ?
C1 C23 1.577(8) . ?
C2 C3 1.393(8) . ?
C3 C4 1.407(8) . ?
C3 H3A 0.9500 . ?
C4 C5 1.354(8) . ?
C4 H4A 0.9500 . ?
C5 C6 1.483(8) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.449(9) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.394(8) . ?
C9 C10 1.398(9) . ?
C9 H9A 0.9500 . ?
C10 C11 1.368(8) . ?
C10 H10A 0.9500 . ?
C11 C12 1.508(8) . ?
C12 C28 1.512(9) . ?
C12 C13 1.580(9) . ?
C12 C30 1.586(9) . ?
C13 C14 1.367(8) . ?
C14 C15 1.418(9) . ?
C14 H14A 0.9500 . ?
C15 C16 1.385(9) . ?
C15 H15A 0.9500 . ?
C16 C17 1.465(9) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.470(9) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.368(9) . ?
C20 C21 1.417(9) . ?
C20 H20A 0.9500 . ?
C21 C22 1.366(8) . ?
C21 H21A 0.9500 . ?
C23 C24 1.494(8) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.552(9) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.508(9) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.495(9) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cr1 O3 109.9(4) . . ?
O2 Cr1 O1 110.2(3) . . ?
O3 Cr1 O1 110.0(3) . . ?
O2 Cr1 O4 107.0(3) . . ?
O3 Cr1 O4 113.8(4) . . ?
O1 Cr1 O4 105.8(3) . . ?
O6 Cr2 O5 109.3(3) . . ?
O6 Cr2 O7 110.6(4) . . ?
O5 Cr2 O7 110.5(3) . . ?
O6 Cr2 O4 106.9(3) . . ?
O5 Cr2 O4 109.6(3) . . ?
O7 Cr2 O4 109.9(3) . . ?
Cr1 O4 Cr2 121.4(3) . . ?
O3' Cr1' O2' 109(2) . . ?
O3' Cr1' O1' 109(2) . . ?
O2' Cr1' O1' 110.0(19) . . ?
O3' Cr1' O4' 116(2) . . ?
O2' Cr1' O4' 106.3(18) . . ?
O1' Cr1' O4' 106.4(18) . . ?
O6' Cr2' O5' 107(2) . . ?
O6' Cr2' O7' 112(2) . . ?
O5' Cr2' O7' 114(2) . . ?
O6' Cr2' O4' 106.7(19) . . ?
O5' Cr2' O4' 109.5(19) . . ?
O7' Cr2' O4' 108.2(19) . . ?
Cr1' O4' Cr2' 123.0(18) . . ?
C2 N1 C5 110.9(5) . . ?
C2 N1 H1N 129(4) . . ?
C5 N1 H1N 120(4) . . ?
C27 N2 C7 113.6(5) . . ?
C27 N2 C6 112.3(5) . . ?
C7 N2 C6 111.4(5) . . ?
C27 N2 H2 106.3 . . ?
C7 N2 H2 106.3 . . ?
C6 N2 H2 106.3 . . ?
C11 N3 C8 109.0(5) . . ?
C11 N3 H3N 127(4) . . ?
C8 N3 H3N 123(4) . . ?
C13 N4 C16 109.7(5) . . ?
C13 N4 H4N 128(4) . . ?
C16 N4 H4N 123(4) . . ?
C32 N5 C17 111.2(5) . . ?
C32 N5 C18 113.0(5) . . ?
C17 N5 C18 112.5(5) . . ?
C32 N5 H5N 113(4) . . ?
C17 N5 H5N 110(4) . . ?
C18 N5 H5N 97(4) . . ?
C19 N6 C22 110.7(5) . . ?
C19 N6 H6N 119(4) . . ?
C22 N6 H6N 130(4) . . ?
C2 C1 C22 108.3(5) . . ?
C2 C1 C25 110.1(5) . . ?
C22 C1 C25 110.2(5) . . ?
C2 C1 C23 107.7(5) . . ?
C22 C1 C23 109.2(4) . . ?
C25 C1 C23 111.1(5) . . ?
N1 C2 C3 105.2(6) . . ?
N1 C2 C1 124.5(5) . . ?
C3 C2 C1 129.8(6) . . ?
C2 C3 C4 109.2(6) . . ?
C2 C3 H3A 125.4 . . ?
C4 C3 H3A 125.4 . . ?
C5 C4 C3 106.8(6) . . ?
C5 C4 H4A 126.6 . . ?
C3 C4 H4A 126.6 . . ?
C4 C5 N1 107.8(6) . . ?
C4 C5 C6 134.7(6) . . ?
N1 C5 C6 117.3(6) . . ?
C5 C6 N2 110.4(5) . . ?
C5 C6 H6A 109.6 . . ?
N2 C6 H6A 109.6 . . ?
C5 C6 H6B 109.6 . . ?
N2 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?
C8 C7 N2 112.4(6) . . ?
C8 C7 H7A 109.1 . . ?
N2 C7 H7A 109.1 . . ?
C8 C7 H7B 109.1 . . ?
N2 C7 H7B 109.1 . . ?
H7A C7 H7B 107.9 . . ?
N3 C8 C9 106.3(6) . . ?
N3 C8 C7 123.3(6) . . ?
C9 C8 C7 129.8(6) . . ?
C8 C9 C10 109.0(6) . . ?
C8 C9 H9A 125.5 . . ?
C10 C9 H9A 125.5 . . ?
C11 C10 C9 105.4(6) . . ?
C11 C10 H10A 127.3 . . ?
C9 C10 H10A 127.3 . . ?
N3 C11 C10 110.3(5) . . ?
N3 C11 C12 122.0(6) . . ?
C10 C11 C12 127.6(6) . . ?
C11 C12 C28 108.7(6) . . ?
C11 C12 C13 110.3(5) . . ?
C28 C12 C13 106.9(5) . . ?
C11 C12 C30 111.2(5) . . ?
C28 C12 C30 113.7(6) . . ?
C13 C12 C30 105.8(5) . . ?
N4 C13 C14 108.8(6) . . ?
N4 C13 C12 120.7(5) . . ?
C14 C13 C12 130.5(6) . . ?
C13 C14 C15 107.1(6) . . ?
C13 C14 H14A 126.4 . . ?
C15 C14 H14A 126.4 . . ?
C16 C15 C14 106.7(6) . . ?
C16 C15 H15A 126.6 . . ?
C14 C15 H15A 126.6 . . ?
N4 C16 C15 107.7(6) . . ?
N4 C16 C17 124.2(6) . . ?
C15 C16 C17 128.1(6) . . ?
C16 C17 N5 115.2(5) . . ?
C16 C17 H17A 108.5 . . ?
N5 C17 H17A 108.5 . . ?
C16 C17 H17B 108.5 . . ?
N5 C17 H17B 108.5 . . ?
H17A C17 H17B 107.5 . . ?
C19 C18 N5 112.4(5) . . ?
C19 C18 H18A 109.1 . . ?
N5 C18 H18A 109.1 . . ?
C19 C18 H18B 109.1 . . ?
N5 C18 H18B 109.1 . . ?
H18A C18 H18B 107.8 . . ?
N6 C19 C20 107.7(6) . . ?
N6 C19 C18 122.4(6) . . ?
C20 C19 C18 130.0(6) . . ?
C19 C20 C21 107.1(6) . . ?
C19 C20 H20A 126.5 . . ?
C21 C20 H20A 126.5 . . ?
C22 C21 C20 107.1(6) . . ?
C22 C21 H21A 126.5 . . ?
C20 C21 H21A 126.5 . . ?
N6 C22 C21 107.4(5) . . ?
N6 C22 C1 121.3(5) . . ?
C21 C22 C1 131.1(6) . . ?
C24 C23 C1 113.3(5) . . ?
C24 C23 H23A 108.9 . . ?
C1 C23 H23A 108.9 . . ?
C24 C23 H23B 108.9 . . ?
C1 C23 H23B 108.9 . . ?
H23A C23 H23B 107.7 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C1 C25 C26 116.1(5) . . ?
C1 C25 H25A 108.3 . . ?
C26 C25 H25A 108.3 . . ?
C1 C25 H25B 108.3 . . ?
C26 C25 H25B 108.3 . . ?
H25A C25 H25B 107.4 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N2 C27 H27A 109.5 . . ?
N2 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N2 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C12 114.4(6) . . ?
C29 C28 H28A 108.7 . . ?
C12 C28 H28A 108.7 . . ?
C29 C28 H28B 108.7 . . ?
C12 C28 H28B 108.7 . . ?
H28A C28 H28B 107.6 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 C12 115.3(6) . . ?
C31 C30 H30A 108.5 . . ?
C12 C30 H30A 108.5 . . ?
C31 C30 H30B 108.5 . . ?
C12 C30 H30B 108.5 . . ?
H30A C30 H30B 107.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N5 C32 H32A 109.5 . . ?
N5 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N5 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?

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
O2 Cr1 O4 Cr2 -72.2(4) . . . . ?
O3 Cr1 O4 Cr2 49.4(5) . . . . ?
O1 Cr1 O4 Cr2 170.3(4) . . . . ?
O6 Cr2 O4 Cr1 160.0(4) . . . . ?
O5 Cr2 O4 Cr1 41.7(5) . . . . ?
O7 Cr2 O4 Cr1 -80.0(4) . . . . ?
O3' Cr1' O4' Cr2' 75(4) . . . . ?
O2' Cr1' O4' Cr2' -47(3) . . . . ?
O1' Cr1' O4' Cr2' -164(3) . . . . ?
O6' Cr2' O4' Cr1' 104(3) . . . . ?
O5' Cr2' O4' Cr1' -11(4) . . . . ?
O7' Cr2' O4' Cr1' -135(3) . . . . ?
C5 N1 C2 C3 0.2(7) . . . . ?
C5 N1 C2 C1 -172.5(5) . . . . ?
C22 C1 C2 N1 97.2(7) . . . . ?
C25 C1 C2 N1 -142.1(6) . . . . ?
C23 C1 C2 N1 -20.8(8) . . . . ?
C22 C1 C2 C3 -73.6(8) . . . . ?
C25 C1 C2 C3 47.0(8) . . . . ?
C23 C1 C2 C3 168.4(6) . . . . ?
N1 C2 C3 C4 0.9(7) . . . . ?
C1 C2 C3 C4 173.1(6) . . . . ?
C2 C3 C4 C5 -1.6(8) . . . . ?
C3 C4 C5 N1 1.7(7) . . . . ?
C3 C4 C5 C6 -173.1(6) . . . . ?
C2 N1 C5 C4 -1.2(7) . . . . ?
C2 N1 C5 C6 174.6(5) . . . . ?
C4 C5 C6 N2 91.7(8) . . . . ?
N1 C5 C6 N2 -82.6(6) . . . . ?
C27 N2 C6 C5 -67.0(6) . . . . ?
C7 N2 C6 C5 164.4(5) . . . . ?
C27 N2 C7 C8 42.3(7) . . . . ?
C6 N2 C7 C8 170.2(5) . . . . ?
C11 N3 C8 C9 1.0(7) . . . . ?
C11 N3 C8 C7 -170.6(6) . . . . ?
N2 C7 C8 N3 70.1(8) . . . . ?
N2 C7 C8 C9 -99.4(8) . . . . ?
N3 C8 C9 C10 -1.6(8) . . . . ?
C7 C8 C9 C10 169.3(7) . . . . ?
C8 C9 C10 C11 1.5(8) . . . . ?
C8 N3 C11 C10 -0.1(8) . . . . ?
C8 N3 C11 C12 -176.5(6) . . . . ?
C9 C10 C11 N3 -0.9(8) . . . . ?
C9 C10 C11 C12 175.2(7) . . . . ?
N3 C11 C12 C28 64.9(8) . . . . ?
C10 C11 C12 C28 -110.9(8) . . . . ?
N3 C11 C12 C13 -52.1(8) . . . . ?
C10 C11 C12 C13 132.2(7) . . . . ?
N3 C11 C12 C30 -169.2(6) . . . . ?
C10 C11 C12 C30 15.1(10) . . . . ?
C16 N4 C13 C14 1.2(7) . . . . ?
C16 N4 C13 C12 -176.7(5) . . . . ?
C11 C12 C13 N4 -53.3(8) . . . . ?
C28 C12 C13 N4 -171.4(6) . . . . ?
C30 C12 C13 N4 67.1(7) . . . . ?
C11 C12 C13 C14 129.3(7) . . . . ?
C28 C12 C13 C14 11.3(9) . . . . ?
C30 C12 C13 C14 -110.3(7) . . . . ?
N4 C13 C14 C15 -1.4(7) . . . . ?
C12 C13 C14 C15 176.2(6) . . . . ?
C13 C14 C15 C16 1.1(7) . . . . ?
C13 N4 C16 C15 -0.5(7) . . . . ?
C13 N4 C16 C17 -177.4(6) . . . . ?
C14 C15 C16 N4 -0.4(7) . . . . ?
C14 C15 C16 C17 176.4(6) . . . . ?
N4 C16 C17 N5 89.8(7) . . . . ?
C15 C16 C17 N5 -86.5(8) . . . . ?
C32 N5 C17 C16 -66.6(7) . . . . ?
C18 N5 C17 C16 61.4(7) . . . . ?
C32 N5 C18 C19 -56.9(7) . . . . ?
C17 N5 C18 C19 176.1(6) . . . . ?
C22 N6 C19 C20 0.1(7) . . . . ?
C22 N6 C19 C18 -179.9(5) . . . . ?
N5 C18 C19 N6 88.7(7) . . . . ?
N5 C18 C19 C20 -91.3(8) . . . . ?
N6 C19 C20 C21 0.4(7) . . . . ?
C18 C19 C20 C21 -179.7(6) . . . . ?
C19 C20 C21 C22 -0.7(7) . . . . ?
C19 N6 C22 C21 -0.5(7) . . . . ?
C19 N6 C22 C1 176.3(5) . . . . ?
C20 C21 C22 N6 0.8(7) . . . . ?
C20 C21 C22 C1 -175.7(6) . . . . ?
C2 C1 C22 N6 -50.6(7) . . . . ?
C25 C1 C22 N6 -171.2(5) . . . . ?
C23 C1 C22 N6 66.5(7) . . . . ?
C2 C1 C22 C21 125.4(7) . . . . ?
C25 C1 C22 C21 4.8(8) . . . . ?
C23 C1 C22 C21 -117.5(7) . . . . ?
C2 C1 C23 C24 -176.8(5) . . . . ?
C22 C1 C23 C24 65.7(7) . . . . ?
C25 C1 C23 C24 -56.1(7) . . . . ?
C2 C1 C25 C26 62.9(7) . . . . ?
C22 C1 C25 C26 -177.6(5) . . . . ?
C23 C1 C25 C26 -56.4(7) . . . . ?
C11 C12 C28 C29 57.4(8) . . . . ?
C13 C12 C28 C29 176.5(6) . . . . ?
C30 C12 C28 C29 -67.0(8) . . . . ?
C11 C12 C30 C31 170.4(6) . . . . ?
C28 C12 C30 C31 -66.4(8) . . . . ?
C13 C12 C30 C31 50.7(8) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1N O7 0.88(3) 2.14(4) 2.968(8) 158(5) .
N3 H3N O2 0.88(3) 2.08(3) 2.957(7) 171(6) .
N3 H3N O2' 0.88(3) 2.38(6) 3.25(4) 168(6) .
N4 H4N O7 0.88(3) 2.18(4) 2.988(8) 152(6) 2_545
N4 H4N O7' 0.88(3) 1.65(5) 2.50(4) 162(6) 2_545
N6 H6N O3 0.88(3) 2.13(3) 3.007(10) 174(6) .

_refine_diff_density_max         0.412
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.064

_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_2h
_database_code_depnum_ccdc_archive 'CCDC 1455746'
_audit_update_record             
;
2016-06-13 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_CHEMW03_2h                  
;
PROBLEM: WARNING: The ratio of given/expected molecular weight as
RESPONSE: This is due to the use of SQUEEZE/PLATON and including
the diffuse and not refined solvent (two methanol molecules)in the 
formula.
;
# end Validation Reply Form 

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H56 F6 N6 O2 Si'
_chemical_formula_weight         722.93

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   12.93(2)
_cell_length_b                   10.616(16)
_cell_length_c                   27.70(4)
_cell_angle_alpha                90
_cell_angle_beta                 99.20(3)
_cell_angle_gamma                90
_cell_volume                     3753(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    13255
_cell_measurement_theta_min      1.489
_cell_measurement_theta_max      24.995

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_F_000             1544
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.049
_exptl_absorpt_coefficient_mu    0.131
_shelx_estimated_absorpt_T_min   0.982
_shelx_estimated_absorpt_T_max   0.994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.982
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Brucker CCD APEX 2'
_diffrn_measurement_method       hemisphere
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14408
_diffrn_reflns_av_unetI/netI     0.1671
_diffrn_reflns_av_R_equivalents  0.1183
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.489
_diffrn_reflns_theta_max         27.345
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3904
_reflns_number_gt                1619
_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       APEX2
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    Diamond3.2
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'

_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)+(0.0511P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3904
_refine_ls_number_parameters     235
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.1744
_refine_ls_R_factor_gt           0.0689
_refine_ls_wR_factor_ref         0.1690
_refine_ls_wR_factor_gt          0.1391
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_restrained_S_all      0.876
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.423 0.223 0.127 81 21 ' '
2 0.577 0.223 0.373 81 21 ' '
3 -0.077 0.277 0.627 81 21 ' '
4 0.077 0.277 0.873 81 21 ' '
5 0.923 0.723 0.127 81 21 ' '
6 0.077 0.723 0.373 81 21 ' '
7 0.423 0.777 0.627 81 21 ' '
8 0.577 0.777 0.873 81 21 ' '
_platon_squeeze_details          
;
The SQUEEZE/PLATON procedure yielded total void volume and electron 
count of 648Å³ and 168 e, respectively. These numbers suggest 
roughly 2 molecules of solvent methanol per formula or 8 molecules 
per unit cell. 
The fraction of solvent has been treated as a diffuse contribution 
to the overall scattering without specific atom positions.
;

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
F1 F 0.5000 0.5825(2) 0.7500 0.0493(8) Uani 1 2 d S T P A .
F2 F 0.5000 0.2675(2) 0.7500 0.0529(9) Uani 1 2 d S T P A .
F3 F 0.3988(3) 0.4246(3) 0.70580(16) 0.070(2) Uani 0.865(13) 1 d D U P A 1
F3A F 0.3731(10) 0.4147(17) 0.7499(15) 0.077(13) Uani 0.135(13) 1 d D U P A 2
F4 F 0.4201(3) 0.4255(3) 0.79075(17) 0.070(2) Uani 0.865(13) 1 d D U P A 1
F4A F 0.521(3) 0.4242(19) 0.8110(4) 0.076(13) Uani 0.135(13) 1 d D U P A 2
Si1 Si 0.5000 0.42860(13) 0.7500 0.0359(4) Uani 1 2 d DS T P . .
N1 N 0.6006(2) 0.2257(3) 0.64464(12) 0.0445(9) Uani 1 1 d . . . . .
H1N H 0.577(3) 0.287(3) 0.6599(14) 0.053 Uiso 1 1 d . U . . .
N2 N 0.6969(2) 0.1567(3) 0.75519(11) 0.0394(8) Uani 1 1 d . . . . .
H2N H 0.636(3) 0.209(3) 0.7513(13) 0.059 Uiso 1 1 d . U . . .
N3 N 0.6541(2) 0.2239(3) 0.86071(12) 0.0444(9) Uani 1 1 d . . . . .
H3N H 0.625(3) 0.284(4) 0.8454(14) 0.053 Uiso 1 1 d . U . . .
C1 C 0.5554(3) 0.1762(4) 0.60077(13) 0.0466(10) Uani 1 1 d . . . . .
C2 C 0.6139(3) 0.0750(4) 0.59295(16) 0.0675(13) Uani 1 1 d . . . . .
H2 H 0.6027 0.0234 0.5655 0.081 Uiso 1 1 calc R U . . .
C3 C 0.6940(3) 0.0607(4) 0.63297(16) 0.0663(13) Uani 1 1 d . . . . .
H3 H 0.7445 -0.0025 0.6370 0.080 Uiso 1 1 calc R U . . .
C4 C 0.6848(3) 0.1548(4) 0.66464(14) 0.0463(10) Uani 1 1 d . . . . .
C5 C 0.7484(3) 0.1842(4) 0.71184(13) 0.0460(10) Uani 1 1 d . . . . .
H5A H 0.7665 0.2729 0.7123 0.055 Uiso 1 1 calc R U . . .
H5B H 0.8131 0.1366 0.7148 0.055 Uiso 1 1 calc R U . . .
C6 C 0.6588(3) 0.0268(4) 0.75496(15) 0.0593(12) Uani 1 1 d . . . . .
H6A H 0.6104 0.0118 0.7255 0.089 Uiso 1 1 calc R U . . .
H6B H 0.6243 0.0136 0.7827 0.089 Uiso 1 1 calc R U . . .
H6C H 0.7169 -0.0302 0.7565 0.089 Uiso 1 1 calc R U . . .
C7 C 0.7723(3) 0.1872(4) 0.80050(14) 0.0501(11) Uani 1 1 d . . . . .
H7A H 0.8365 0.1402 0.8001 0.060 Uiso 1 1 calc R U . . .
H7B H 0.7894 0.2762 0.8002 0.060 Uiso 1 1 calc R U . . .
C8 C 0.7316(3) 0.1581(4) 0.84598(15) 0.0480(10) Uani 1 1 d . . . . .
C9 C 0.7626(3) 0.0698(4) 0.87996(17) 0.0664(13) Uani 1 1 d . . . . .
H9 H 0.8161 0.0116 0.8794 0.080 Uiso 1 1 calc R U . . .
C10 C 0.6996(3) 0.0817(4) 0.91625(16) 0.0652(13) Uani 1 1 d . . . . .
H10 H 0.7030 0.0312 0.9439 0.078 Uiso 1 1 calc R U . . .
C11 C 0.3673(3) 0.1790(4) 0.59568(14) 0.0461(10) Uani 1 1 d . . . . .
C12 C 0.4561(3) 0.2287(4) 0.57326(14) 0.0498(11) Uani 1 1 d . . . . .
C13 C 0.4578(3) 0.3736(4) 0.57394(15) 0.0570(11) Uani 1 1 d . . . . .
H13A H 0.4658 0.4016 0.6077 0.068 Uiso 1 1 calc R U . . .
H13B H 0.5188 0.4021 0.5607 0.068 Uiso 1 1 calc R U . . .
C14 C 0.3618(3) 0.4356(4) 0.54566(16) 0.0775(14) Uani 1 1 d . . . . .
H14A H 0.3595 0.4203 0.5113 0.116 Uiso 1 1 calc R U . . .
H14B H 0.3648 0.5247 0.5517 0.116 Uiso 1 1 calc R U . . .
H14C H 0.3002 0.4014 0.5559 0.116 Uiso 1 1 calc R U . . .
C15 C 0.4431(3) 0.1818(5) 0.52017(14) 0.0676(13) Uani 1 1 d . . . . .
H15A H 0.4472 0.0905 0.5205 0.081 Uiso 1 1 calc R U . . .
H15B H 0.3736 0.2047 0.5039 0.081 Uiso 1 1 calc R U . . .
C16 C 0.5223(4) 0.2318(5) 0.49036(18) 0.0949(17) Uani 1 1 d . . . . .
H16A H 0.5106 0.3202 0.4845 0.142 Uiso 1 1 calc R U . . .
H16B H 0.5149 0.1880 0.4597 0.142 Uiso 1 1 calc R U . . .
H16C H 0.5918 0.2190 0.5079 0.142 Uiso 1 1 calc R U . . .


_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
F1 Si1 1.634(4) . ?
F2 Si1 1.711(4) . ?
F3 Si1 1.643(3) . ?
F3A Si1 1.647(12) . ?
F4 Si1 1.647(3) . ?
F4A Si1 1.669(12) . ?
Si1 F3 1.643(3) 2_656 ?
Si1 F3A 1.647(12) 2_656 ?
Si1 F4 1.647(3) 2_656 ?
Si1 F4A 1.669(12) 2_656 ?
N1 C4 1.365(5) . ?
N1 C1 1.367(5) . ?
N2 C6 1.464(5) . ?
N2 C5 1.492(5) . ?
N2 C7 1.496(5) . ?
N3 C8 1.338(5) . ?
N3 C11 1.367(5) 2_656 ?
C1 C2 1.351(5) . ?
C1 C12 1.492(5) . ?
C2 C3 1.399(6) . ?
C3 C4 1.348(5) . ?
C4 C5 1.463(5) . ?
C7 C8 1.474(5) . ?
C8 C9 1.343(5) . ?
C9 C10 1.397(6) . ?
C10 C11 1.354(5) 2_656 ?
C11 C10 1.354(5) 2_656 ?
C11 N3 1.367(5) 2_656 ?
C11 C12 1.487(5) . ?
C12 C15 1.536(5) . ?
C12 C13 1.539(6) . ?
C13 C14 1.509(5) . ?
C15 C16 1.511(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F1 Si1 F3 91.47(11) . 2_656 ?
F1 Si1 F3 91.47(11) . . ?
F3 Si1 F3 177.1(2) 2_656 . ?
F1 Si1 F3A 95.1(6) . 2_656 ?
F1 Si1 F3A 95.1(6) . . ?
F3A Si1 F3A 169.7(13) 2_656 . ?
F1 Si1 F4 91.14(11) . . ?
F3 Si1 F4 90.0(2) 2_656 . ?
F3 Si1 F4 89.9(2) . . ?
F1 Si1 F4 91.14(11) . 2_656 ?
F3 Si1 F4 89.9(2) 2_656 2_656 ?
F3 Si1 F4 90.0(2) . 2_656 ?
F4 Si1 F4 177.7(2) . 2_656 ?
F1 Si1 F4A 91.6(7) . . ?
F3A Si1 F4A 89.8(14) 2_656 . ?
F3A Si1 F4A 89.9(14) . . ?
F1 Si1 F4A 91.6(7) . 2_656 ?
F3A Si1 F4A 89.9(14) 2_656 2_656 ?
F3A Si1 F4A 89.8(14) . 2_656 ?
F4A Si1 F4A 176.8(14) . 2_656 ?
F1 Si1 F2 180.0 . . ?
F3 Si1 F2 88.53(11) 2_656 . ?
F3 Si1 F2 88.53(11) . . ?
F3A Si1 F2 84.9(6) 2_656 . ?
F3A Si1 F2 84.9(6) . . ?
F4 Si1 F2 88.86(11) . . ?
F4 Si1 F2 88.86(11) 2_656 . ?
F4A Si1 F2 88.4(7) . . ?
F4A Si1 F2 88.4(7) 2_656 . ?
C4 N1 C1 110.4(3) . . ?
C6 N2 C5 112.0(3) . . ?
C6 N2 C7 112.4(3) . . ?
C5 N2 C7 108.6(3) . . ?
C8 N3 C11 110.8(3) . 2_656 ?
C2 C1 N1 106.1(4) . . ?
C2 C1 C12 132.3(4) . . ?
N1 C1 C12 121.4(3) . . ?
C1 C2 C3 108.8(4) . . ?
C4 C3 C2 107.7(4) . . ?
C3 C4 N1 107.0(4) . . ?
C3 C4 C5 130.2(4) . . ?
N1 C4 C5 122.9(4) . . ?
C4 C5 N2 114.7(3) . . ?
C8 C7 N2 113.4(3) . . ?
N3 C8 C9 107.7(4) . . ?
N3 C8 C7 122.6(4) . . ?
C9 C8 C7 129.7(4) . . ?
C8 C9 C10 107.4(4) . . ?
C11 C10 C9 108.4(4) 2_656 . ?
C10 C11 N3 105.7(4) 2_656 2_656 ?
C10 C11 C12 132.4(4) 2_656 . ?
N3 C11 C12 121.6(3) 2_656 . ?
C11 C12 C1 108.2(3) . . ?
C11 C12 C15 108.1(3) . . ?
C1 C12 C15 108.8(3) . . ?
C11 C12 C13 111.1(3) . . ?
C1 C12 C13 110.9(3) . . ?
C15 C12 C13 109.6(3) . . ?
C14 C13 C12 114.9(3) . . ?
C16 C15 C12 115.4(4) . . ?

_refine_diff_density_max         0.227
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.050

_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_2i
_database_code_depnum_ccdc_archive 'CCDC 1455747'
_audit_update_record             
;
2016-06-13 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_THETM01_2i                  
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: A full set of data was collected. However, data dominated 
by noise was omitted. Subtantial disorder in the structure is a
significant contributor to this problem, involving the whole 
thiosulfate ion and all eight carbon of four ethyl substituents.
;
_vrf_PLAT089_2i                  
;
PROBLEM: Poor Data / Parameter Ratio (Zmax < 18) ........ 4.98 Note
RESPONSE: See response to THETM01_ALERT_3_B above.
;
_vrf_PLAT340_2i                  
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.02005 Ang.
RESPONSE: This alert is generated because there is a large amount 
of disorder in the structure involving 8 C atoms.
;
_vrf_PLAT410_2i                  
;
PROBLEM: Short Intra H...H Contact H21A .. H23A .. 1.82 Ang.
RESPONSE: This alert is generated because there is a large amount 
of disorder in the structure involving 8 C atoms C23 being one of them.
;
_vrf_PLAT411_2i                  
;
PROBLEM: Short Inter H...H Contact H14A .. H28B .. 1.84 Ang.
RESPONSE: This alert is generated because there is a large amount 
of disorder in the structure involving 8 C atoms C28 being one of them.
;
_vrf_PLAT414_2i                  
;
PROBLEM: Short Intra D-H..H-X H1N .. H25A .. 1.82 Ang.
RESPONSE: This alert is generated because there is a large amount 
of disorder in the structure involving 8 C atoms C25 being one of them.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H48 N6 O3 S2'
_chemical_formula_weight         628.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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'

_cell_length_a                   11.660(9)
_cell_length_b                   11.998(9)
_cell_length_c                   11.826(9)
_cell_angle_alpha                90
_cell_angle_beta                 92.19(2)
_cell_angle_gamma                90
_cell_volume                     1653(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    23895
_cell_measurement_theta_min      1.511
_cell_measurement_theta_max      25.000

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_F_000             676
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    1.790
_shelx_estimated_absorpt_T_min   0.616
_shelx_estimated_absorpt_T_max   0.982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.971
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Brucker CCD APEX 2'
_diffrn_measurement_method       hemisphere
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12097
_diffrn_reflns_av_unetI/netI     0.1787
_diffrn_reflns_av_R_equivalents  0.1222
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.740
_diffrn_reflns_theta_max         59.999
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.823
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.823
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_point_group_measured_fraction_full 0.770
_reflns_number_total             4602
_reflns_number_gt                2310
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.779
_reflns_Friedel_fraction_max     0.871
_reflns_Friedel_fraction_full    0.711

_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       APEX2
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    Diamond3.2
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'


_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)+(0.0683P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0080(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 720 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.09(4)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         4602
_refine_ls_number_parameters     519
_refine_ls_number_restraints     288
_refine_ls_R_factor_all          0.1264
_refine_ls_R_factor_gt           0.0695
_refine_ls_wR_factor_ref         0.1602
_refine_ls_wR_factor_gt          0.1437
_refine_ls_goodness_of_fit_ref   0.834
_refine_ls_restrained_S_all      0.812
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
S1 S 0.1551(4) 0.8886(4) 0.1406(5) 0.0387(13) Uani 0.832(8) 1 d D U P A 1
S2 S 0.1738(4) 1.0054(3) 0.2589(4) 0.0595(15) Uani 0.832(8) 1 d D U P A 1
O1 O 0.0331(6) 0.8776(7) 0.1053(7) 0.045(2) Uani 0.832(8) 1 d D U P A 1
O2 O 0.2250(8) 0.9194(6) 0.0427(8) 0.059(3) Uani 0.832(8) 1 d D U P A 1
O3 O 0.1934(12) 0.7785(8) 0.1883(14) 0.038(4) Uani 0.832(8) 1 d D U P A 1
S1' S 0.139(3) 0.888(3) 0.162(3) 0.094(13) Uani 0.168(8) 1 d D U P A 2
S2' S 0.255(2) 1.0094(19) 0.177(3) 0.092(10) Uani 0.168(8) 1 d D U P A 2
O1' O 0.038(4) 0.912(4) 0.229(4) 0.084(14) Uani 0.168(8) 1 d D U P A 2
O2' O 0.110(3) 0.877(4) 0.038(3) 0.049(12) Uiso 0.168(8) 1 d D U P A 2
O3' O 0.189(7) 0.781(4) 0.208(7) 0.06(3) Uiso 0.168(8) 1 d D U P A 2
N1 N 0.1154(9) 0.8238(9) 0.4598(9) 0.061(3) Uani 1 1 d D . . . .
H1N H 0.103(10) 0.862(9) 0.394(7) 0.074 Uiso 1 1 d D U . . .
N2 N 0.3601(9) 0.7865(8) 0.3636(10) 0.066(3) Uani 1 1 d D . . . .
H2N H 0.303(9) 0.797(10) 0.296(7) 0.079 Uiso 1 1 d D U . . .
N3 N 0.4600(8) 0.8113(8) 0.1069(11) 0.063(3) Uani 1 1 d D . . . .
H3N H 0.396(7) 0.861(8) 0.116(9) 0.075 Uiso 1 1 d D U . . .
N4 N 0.2709(8) 0.7199(8) -0.0824(9) 0.057(3) Uani 1 1 d D . . . .
H4N H 0.265(10) 0.788(6) -0.066(10) 0.068 Uiso 1 1 d D U . . .
N5 N 0.0527(8) 0.6274(9) 0.0570(10) 0.063(3) Uani 1 1 d D . . . .
H5N H 0.096(9) 0.680(8) 0.106(9) 0.076 Uiso 1 1 d D U . . .
N6 N -0.0845(8) 0.7235(8) 0.2689(9) 0.052(3) Uani 1 1 d D . . . .
H6N H -0.047(8) 0.785(7) 0.245(9) 0.062 Uiso 1 1 d D U . . .
C1 C -0.0963(12) 0.7808(12) 0.4782(12) 0.075(4) Uani 1 1 d . . . . .
C2 C 0.0280(13) 0.7720(10) 0.5192(11) 0.063(4) Uani 1 1 d . . . . .
C3 C 0.0799(13) 0.7167(11) 0.6129(10) 0.065(4) Uani 1 1 d . . . . .
H3A H 0.0421 0.6762 0.6673 0.078 Uiso 1 1 calc R U . . .
C4 C 0.2011(14) 0.7338(10) 0.6094(12) 0.080(5) Uani 1 1 d . . . . .
H4A H 0.2563 0.7061 0.6609 0.095 Uiso 1 1 calc R U . . .
C5 C 0.2215(14) 0.7992(10) 0.5154(12) 0.068(4) Uani 1 1 d . . . . .
C6 C 0.3282(12) 0.8433(11) 0.4712(11) 0.069(4) Uani 1 1 d . . . . .
H6A H 0.3899 0.8336 0.5277 0.083 Uiso 1 1 calc R U . . .
H6B H 0.3193 0.9226 0.4571 0.083 Uiso 1 1 calc R U . . .
C7 C 0.4620(11) 0.8454(11) 0.3178(13) 0.076(4) Uani 1 1 d . . . . .
H7A H 0.5222 0.8472 0.3767 0.091 Uiso 1 1 calc R U . . .
H7B H 0.4402 0.9220 0.3016 0.091 Uiso 1 1 calc R U . . .
C8 C 0.5110(10) 0.7964(10) 0.2130(14) 0.070(4) Uani 1 1 d . . . . .
C9 C 0.6051(11) 0.7301(10) 0.1999(15) 0.082(5) Uani 1 1 d . . . . .
H9A H 0.6558 0.7062 0.2575 0.098 Uiso 1 1 calc R U . . .
C10 C 0.6121(10) 0.7043(10) 0.0836(13) 0.066(4) Uani 1 1 d . . . . .
H10A H 0.6674 0.6601 0.0510 0.079 Uiso 1 1 calc R U . . .
C11 C 0.5202(10) 0.7578(10) 0.0269(13) 0.061(4) Uani 1 1 d . . . . .
C12 C 0.4850(12) 0.7607(13) -0.0954(13) 0.083(5) Uani 1 1 d . . . . .
C13 C 0.3764(11) 0.6843(13) -0.1123(11) 0.069(4) Uani 1 1 d . . . . .
C14 C 0.3706(14) 0.5744(14) -0.1521(11) 0.080(5) Uani 1 1 d . . . . .
H14A H 0.4296 0.5316 -0.1802 0.097 Uiso 1 1 calc R U . . .
C15 C 0.2501(14) 0.5420(13) -0.1394(12) 0.090(5) Uani 1 1 d . . . . .
H15A H 0.2186 0.4723 -0.1550 0.108 Uiso 1 1 calc R U . . .
C16 C 0.1922(12) 0.6334(11) -0.1003(10) 0.065(4) Uani 1 1 d . . . . .
C17 C 0.0712(11) 0.6453(11) -0.0698(11) 0.066(4) Uani 1 1 d . . . . .
H17A H 0.0250 0.5918 -0.1129 0.079 Uiso 1 1 calc R U . . .
H17B H 0.0446 0.7193 -0.0910 0.079 Uiso 1 1 calc R U . . .
C18 C -0.0763(9) 0.6401(11) 0.0791(12) 0.064(4) Uani 1 1 d . . . . .
H18A H -0.1027 0.7115 0.0497 0.077 Uiso 1 1 calc R U . . .
H18B H -0.1185 0.5822 0.0382 0.077 Uiso 1 1 calc R U . . .
C19 C -0.1014(10) 0.6331(11) 0.1999(13) 0.059(4) Uani 1 1 d . . . . .
C20 C -0.1417(11) 0.5506(12) 0.2619(18) 0.087(5) Uani 1 1 d . . . . .
H20A H -0.1621 0.4803 0.2347 0.104 Uiso 1 1 calc R U . . .
C21 C -0.1490(11) 0.5858(12) 0.3759(16) 0.078(5) Uani 1 1 d . . . . .
H21A H -0.1731 0.5446 0.4372 0.093 Uiso 1 1 calc R U . . .
C22 C -0.1125(10) 0.6947(12) 0.3751(13) 0.066(4) Uani 1 1 d . . . . .
C23 C -0.191(2) 0.713(3) 0.557(3) 0.047(8) Uani 0.453(18) 1 d . U P B 1
H23A H -0.1669 0.6359 0.5604 0.056 Uiso 0.453(18) 1 calc R U P B 1
H23B H -0.1819 0.7425 0.6331 0.056 Uiso 0.453(18) 1 calc R U P B 1
C24 C -0.3149(18) 0.712(2) 0.529(2) 0.059(9) Uani 0.453(18) 1 d . U P B 1
H24A H -0.3533 0.6683 0.5843 0.089 Uiso 0.453(18) 1 calc R U P B 1
H24B H -0.3285 0.6803 0.4555 0.089 Uiso 0.453(18) 1 calc R U P B 1
H24C H -0.3439 0.7870 0.5299 0.089 Uiso 0.453(18) 1 calc R U P B 1
C23' C -0.152(2) 0.759(3) 0.589(2) 0.067(9) Uani 0.547(18) 1 d . U P B 2
H23C H -0.1214 0.6891 0.6183 0.081 Uiso 0.547(18) 1 calc R U P B 2
H23D H -0.2331 0.7470 0.5721 0.081 Uiso 0.547(18) 1 calc R U P B 2
C24' C -0.1436(17) 0.843(2) 0.686(2) 0.077(9) Uani 0.547(18) 1 d . U P B 2
H24D H -0.1881 0.8168 0.7477 0.116 Uiso 0.547(18) 1 calc R U P B 2
H24E H -0.1725 0.9137 0.6607 0.116 Uiso 0.547(18) 1 calc R U P B 2
H24F H -0.0648 0.8506 0.7118 0.116 Uiso 0.547(18) 1 calc R U P B 2
C25 C -0.101(3) 0.909(6) 0.440(5) 0.069(14) Uani 0.50(2) 1 d . U P B 1
H25A H -0.0247 0.9393 0.4289 0.083 Uiso 0.50(2) 1 calc R U P B 1
H25B H -0.1484 0.9203 0.3719 0.083 Uiso 0.50(2) 1 calc R U P B 1
C26 C -0.151(2) 0.9560(19) 0.536(2) 0.062(8) Uani 0.50(2) 1 d . U P B 1
H26A H -0.1841 1.0271 0.5170 0.093 Uiso 0.50(2) 1 calc R U P B 1
H26B H -0.0935 0.9653 0.5957 0.093 Uiso 0.50(2) 1 calc R U P B 1
H26C H -0.2101 0.9070 0.5616 0.093 Uiso 0.50(2) 1 calc R U P B 1
C25' C -0.145(3) 0.894(5) 0.439(4) 0.050(11) Uani 0.50(2) 1 d . U P B 2
H25C H -0.1136 0.9452 0.4950 0.060 Uiso 0.50(2) 1 calc R U P B 2
H25D H -0.1044 0.9088 0.3708 0.060 Uiso 0.50(2) 1 calc R U P B 2
C26' C -0.2346(19) 0.9287(19) 0.419(2) 0.056(8) Uani 0.50(2) 1 d . U P B 2
H26D H -0.2291 1.0070 0.4032 0.084 Uiso 0.50(2) 1 calc R U P B 2
H26E H -0.2822 0.9173 0.4821 0.084 Uiso 0.50(2) 1 calc R U P B 2
H26F H -0.2678 0.8913 0.3535 0.084 Uiso 0.50(2) 1 calc R U P B 2
C27 C 0.3773(11) 0.6659(9) 0.3758(12) 0.076(4) Uani 1 1 d . . . . .
H27A H 0.3098 0.6328 0.4055 0.114 Uiso 1 1 calc R U . . .
H27B H 0.4419 0.6521 0.4267 0.114 Uiso 1 1 calc R U . . .
H27C H 0.3916 0.6339 0.3033 0.114 Uiso 1 1 calc R U . . .
C28 C 0.571(2) 0.681(3) -0.184(3) 0.047(8) Uani 0.476(19) 1 d . U P C 1
H28A H 0.6499 0.7059 -0.1729 0.056 Uiso 0.476(19) 1 calc R U P C 1
H28B H 0.5683 0.6040 -0.1590 0.056 Uiso 0.476(19) 1 calc R U P C 1
C29 C 0.5415(19) 0.683(2) -0.3115(19) 0.059(9) Uani 0.476(19) 1 d . U P C 1
H29A H 0.5950 0.6372 -0.3502 0.089 Uiso 0.476(19) 1 calc R U P C 1
H29B H 0.5457 0.7581 -0.3388 0.089 Uiso 0.476(19) 1 calc R U P C 1
H29C H 0.4652 0.6547 -0.3252 0.089 Uiso 0.476(19) 1 calc R U P C 1
C28' C 0.597(2) 0.734(2) -0.149(2) 0.055(8) Uani 0.524(19) 1 d . U P C 2
H28C H 0.5783 0.7241 -0.2289 0.066 Uiso 0.524(19) 1 calc R U P C 2
H28D H 0.6190 0.6608 -0.1204 0.066 Uiso 0.524(19) 1 calc R U P C 2
C29' C 0.711(2) 0.805(2) -0.143(2) 0.084(10) Uani 0.524(19) 1 d . U P C 2
H29D H 0.7687 0.7667 -0.1840 0.126 Uiso 0.524(19) 1 calc R U P C 2
H29E H 0.7361 0.8140 -0.0659 0.126 Uiso 0.524(19) 1 calc R U P C 2
H29F H 0.6961 0.8763 -0.1771 0.126 Uiso 0.524(19) 1 calc R U P C 2
C30 C 0.453(3) 0.858(3) -0.151(4) 0.057(10) Uani 0.53(3) 1 d . U P C 1
H30A H 0.3896 0.8918 -0.1126 0.068 Uiso 0.53(3) 1 calc R U P C 1
H30B H 0.4254 0.8395 -0.2276 0.068 Uiso 0.53(3) 1 calc R U P C 1
C31 C 0.550(2) 0.9401(18) -0.157(2) 0.060(8) Uani 0.53(3) 1 d . U P C 1
H31A H 0.5239 1.0058 -0.1962 0.091 Uiso 0.53(3) 1 calc R U P C 1
H31B H 0.6121 0.9072 -0.1957 0.091 Uiso 0.53(3) 1 calc R U P C 1
H31C H 0.5758 0.9599 -0.0812 0.091 Uiso 0.53(3) 1 calc R U P C 1
C30' C 0.456(4) 0.900(3) -0.115(4) 0.058(11) Uani 0.47(3) 1 d . U P C 2
H30C H 0.3878 0.9212 -0.0761 0.070 Uiso 0.47(3) 1 calc R U P C 2
H30D H 0.5200 0.9449 -0.0846 0.070 Uiso 0.47(3) 1 calc R U P C 2
C31' C 0.440(2) 0.920(2) -0.241(2) 0.062(9) Uani 0.47(3) 1 d . U P C 2
H31D H 0.4262 0.9974 -0.2547 0.093 Uiso 0.47(3) 1 calc R U P C 2
H31E H 0.3748 0.8772 -0.2689 0.093 Uiso 0.47(3) 1 calc R U P C 2
H31F H 0.5071 0.8963 -0.2782 0.093 Uiso 0.47(3) 1 calc R U P C 2
C32 C 0.1026(10) 0.5193(10) 0.0998(11) 0.066(4) Uani 1 1 d . . . . .
H32A H 0.0889 0.5117 0.1789 0.099 Uiso 1 1 calc R U . . .
H32B H 0.1838 0.5185 0.0887 0.099 Uiso 1 1 calc R U . . .
H32C H 0.0671 0.4585 0.0590 0.099 Uiso 1 1 calc R U . . .


_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
S1 O1 1.473(9) . ?
S1 O2 1.488(10) . ?
S1 O3 1.498(8) . ?
S1 S2 1.987(6) . ?
S1' O1' 1.47(3) . ?
S1' O2' 1.50(3) . ?
S1' O3' 1.50(3) . ?
S1' S2' 2.00(3) . ?
N1 C2 1.405(17) . ?
N1 C5 1.409(15) . ?
N1 H1N 0.91(6) . ?
N2 C27 1.468(14) . ?
N2 C7 1.501(16) . ?
N2 C6 1.502(15) . ?
N2 H2N 1.03(6) . ?
N3 C11 1.360(16) . ?
N3 C8 1.379(16) . ?
N3 H3N 0.96(6) . ?
N4 C13 1.362(15) . ?
N4 C16 1.396(16) . ?
N4 H4N 0.84(6) . ?
N5 C32 1.502(15) . ?
N5 C17 1.539(16) . ?
N5 C18 1.544(14) . ?
N5 H5N 0.98(6) . ?
N6 C22 1.354(16) . ?
N6 C19 1.367(15) . ?
N6 H6N 0.91(6) . ?
C1 C23' 1.51(3) . ?
C1 C2 1.515(19) . ?
C1 C25' 1.53(6) . ?
C1 C22 1.60(2) . ?
C1 C25 1.61(7) . ?
C1 C23 1.68(3) . ?
C2 C3 1.408(16) . ?
C3 C4 1.430(19) . ?
C3 H3A 0.9300 . ?
C4 C5 1.390(18) . ?
C4 H4A 0.9300 . ?
C5 C6 1.466(18) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.505(18) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.368(17) . ?
C9 C10 1.415(17) . ?
C9 H9A 0.9300 . ?
C10 C11 1.399(16) . ?
C10 H10A 0.9300 . ?
C11 C12 1.489(18) . ?
C12 C30 1.38(5) . ?
C12 C28' 1.51(3) . ?
C12 C13 1.57(2) . ?
C12 C30' 1.72(4) . ?
C12 C28 1.76(3) . ?
C13 C14 1.401(19) . ?
C14 C15 1.47(2) . ?
C14 H14A 0.9300 . ?
C15 C16 1.376(17) . ?
C15 H15A 0.9300 . ?
C16 C17 1.476(17) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.473(17) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.328(18) . ?
C20 C21 1.42(2) . ?
C20 H20A 0.9300 . ?
C21 C22 1.375(18) . ?
C21 H21A 0.9300 . ?
C23 C24 1.47(3) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C23' C24' 1.53(3) . ?
C23' H23C 0.9700 . ?
C23' H23D 0.9700 . ?
C24' H24D 0.9600 . ?
C24' H24E 0.9600 . ?
C24' H24F 0.9600 . ?
C25 C26 1.42(6) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C25' C26' 1.14(4) . ?
C25' H25C 0.9700 . ?
C25' H25D 0.9700 . ?
C26' H26D 0.9600 . ?
C26' H26E 0.9600 . ?
C26' H26F 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 C29 1.53(3) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C28' C29' 1.57(3) . ?
C28' H28C 0.9700 . ?
C28' H28D 0.9700 . ?
C29' H29D 0.9600 . ?
C29' H29E 0.9600 . ?
C29' H29F 0.9600 . ?
C30 C31 1.51(5) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C30' C31' 1.51(5) . ?
C30' H30C 0.9700 . ?
C30' H30D 0.9700 . ?
C31' H31D 0.9600 . ?
C31' H31E 0.9600 . ?
C31' H31F 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?

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
O1 S1 O2 110.8(6) . . ?
O1 S1 O3 107.4(7) . . ?
O2 S1 O3 110.4(8) . . ?
O1 S1 S2 109.9(5) . . ?
O2 S1 S2 108.9(5) . . ?
O3 S1 S2 109.5(7) . . ?
O1' S1' O2' 113(3) . . ?
O1' S1' O3' 107(3) . . ?
O2' S1' O3' 111(3) . . ?
O1' S1' S2' 111(3) . . ?
O2' S1' S2' 106(2) . . ?
O3' S1' S2' 110(3) . . ?
C2 N1 C5 108.3(12) . . ?
C2 N1 H1N 123(8) . . ?
C5 N1 H1N 128(8) . . ?
C27 N2 C7 113.1(11) . . ?
C27 N2 C6 113.6(11) . . ?
C7 N2 C6 108.5(10) . . ?
C27 N2 H2N 106(7) . . ?
C7 N2 H2N 99(7) . . ?
C6 N2 H2N 116(7) . . ?
C11 N3 C8 110.8(11) . . ?
C11 N3 H3N 142(7) . . ?
C8 N3 H3N 107(7) . . ?
C13 N4 C16 108.8(11) . . ?
C13 N4 H4N 117(9) . . ?
C16 N4 H4N 134(9) . . ?
C32 N5 C17 112.5(10) . . ?
C32 N5 C18 113.3(10) . . ?
C17 N5 C18 108.9(10) . . ?
C32 N5 H5N 100(7) . . ?
C17 N5 H5N 113(7) . . ?
C18 N5 H5N 109(7) . . ?
C22 N6 C19 108.5(11) . . ?
C22 N6 H6N 129(7) . . ?
C19 N6 H6N 121(7) . . ?
C23' C1 C2 98.5(16) . . ?
C23' C1 C25' 104(2) . . ?
C2 C1 C25' 120(2) . . ?
C23' C1 C22 120.6(17) . . ?
C2 C1 C22 106.3(10) . . ?
C25' C1 C22 108(2) . . ?
C2 C1 C25 100.2(18) . . ?
C22 C1 C25 114(2) . . ?
C2 C1 C23 115.6(14) . . ?
C22 C1 C23 92.8(16) . . ?
C25 C1 C23 127(2) . . ?
N1 C2 C3 107.7(12) . . ?
N1 C2 C1 120.8(11) . . ?
C3 C2 C1 131.5(14) . . ?
C2 C3 C4 107.8(12) . . ?
C2 C3 H3A 126.1 . . ?
C4 C3 H3A 126.1 . . ?
C5 C4 C3 107.7(12) . . ?
C5 C4 H4A 126.2 . . ?
C3 C4 H4A 126.2 . . ?
C4 C5 N1 108.5(14) . . ?
C4 C5 C6 131.5(12) . . ?
N1 C5 C6 120.0(13) . . ?
C5 C6 N2 112.3(11) . . ?
C5 C6 H6A 109.1 . . ?
N2 C6 H6A 109.1 . . ?
C5 C6 H6B 109.1 . . ?
N2 C6 H6B 109.1 . . ?
H6A C6 H6B 107.9 . . ?
N2 C7 C8 116.3(11) . . ?
N2 C7 H7A 108.2 . . ?
C8 C7 H7A 108.2 . . ?
N2 C7 H7B 108.2 . . ?
C8 C7 H7B 108.2 . . ?
H7A C7 H7B 107.4 . . ?
C9 C8 N3 107.0(14) . . ?
C9 C8 C7 130.7(14) . . ?
N3 C8 C7 122.2(12) . . ?
C8 C9 C10 108.3(13) . . ?
C8 C9 H9A 125.9 . . ?
C10 C9 H9A 125.9 . . ?
C11 C10 C9 107.1(12) . . ?
C11 C10 H10A 126.5 . . ?
C9 C10 H10A 126.5 . . ?
N3 C11 C10 106.8(13) . . ?
N3 C11 C12 122.3(11) . . ?
C10 C11 C12 130.9(14) . . ?
C30 C12 C11 122.9(19) . . ?
C11 C12 C28' 101.0(15) . . ?
C30 C12 C13 103.1(19) . . ?
C11 C12 C13 107.5(10) . . ?
C28' C12 C13 122.0(16) . . ?
C11 C12 C30' 101.3(17) . . ?
C28' C12 C30' 109(2) . . ?
C13 C12 C30' 114(2) . . ?
C30 C12 C28 108.9(19) . . ?
C11 C12 C28 115.1(14) . . ?
C13 C12 C28 94.7(14) . . ?
N4 C13 C14 110.5(14) . . ?
N4 C13 C12 121.1(13) . . ?
C14 C13 C12 128.4(13) . . ?
C13 C14 C15 104.4(12) . . ?
C13 C14 H14A 127.8 . . ?
C15 C14 H14A 127.8 . . ?
C16 C15 C14 107.9(14) . . ?
C16 C15 H15A 126.1 . . ?
C14 C15 H15A 126.1 . . ?
C15 C16 N4 108.4(13) . . ?
C15 C16 C17 130.1(15) . . ?
N4 C16 C17 121.3(11) . . ?
C16 C17 N5 113.2(10) . . ?
C16 C17 H17A 108.9 . . ?
N5 C17 H17A 108.9 . . ?
C16 C17 H17B 108.9 . . ?
N5 C17 H17B 108.9 . . ?
H17A C17 H17B 107.7 . . ?
C19 C18 N5 112.9(10) . . ?
C19 C18 H18A 109.0 . . ?
N5 C18 H18A 109.0 . . ?
C19 C18 H18B 109.0 . . ?
N5 C18 H18B 109.0 . . ?
H18A C18 H18B 107.8 . . ?
C20 C19 N6 108.0(14) . . ?
C20 C19 C18 131.8(15) . . ?
N6 C19 C18 120.2(12) . . ?
C19 C20 C21 109.7(14) . . ?
C19 C20 H20A 125.1 . . ?
C21 C20 H20A 125.1 . . ?
C22 C21 C20 104.3(14) . . ?
C22 C21 H21A 127.9 . . ?
C20 C21 H21A 127.9 . . ?
N6 C22 C21 109.5(15) . . ?
N6 C22 C1 121.1(12) . . ?
C21 C22 C1 129.4(15) . . ?
C24 C23 C1 123(2) . . ?
C24 C23 H23A 106.6 . . ?
C1 C23 H23A 106.6 . . ?
C24 C23 H23B 106.6 . . ?
C1 C23 H23B 106.6 . . ?
H23A C23 H23B 106.6 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C1 C23' C24' 122(2) . . ?
C1 C23' H23C 106.9 . . ?
C24' C23' H23C 106.9 . . ?
C1 C23' H23D 106.9 . . ?
C24' C23' H23D 106.9 . . ?
H23C C23' H23D 106.7 . . ?
C23' C24' H24D 109.5 . . ?
C23' C24' H24E 109.5 . . ?
H24D C24' H24E 109.5 . . ?
C23' C24' H24F 109.5 . . ?
H24D C24' H24F 109.5 . . ?
H24E C24' H24F 109.5 . . ?
C26 C25 C1 99(4) . . ?
C26 C25 H25A 111.9 . . ?
C1 C25 H25A 111.9 . . ?
C26 C25 H25B 111.9 . . ?
C1 C25 H25B 111.9 . . ?
H25A C25 H25B 109.6 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C26' C25' C1 136(5) . . ?
C26' C25' H25C 103.2 . . ?
C1 C25' H25C 103.2 . . ?
C26' C25' H25D 103.2 . . ?
C1 C25' H25D 103.2 . . ?
H25C C25' H25D 105.2 . . ?
C25' C26' H26D 109.5 . . ?
C25' C26' H26E 109.5 . . ?
H26D C26' H26E 109.5 . . ?
C25' C26' H26F 109.5 . . ?
H26D C26' H26F 109.5 . . ?
H26E C26' H26F 109.5 . . ?
N2 C27 H27A 109.5 . . ?
N2 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N2 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C12 117.6(19) . . ?
C29 C28 H28A 107.9 . . ?
C12 C28 H28A 107.9 . . ?
C29 C28 H28B 107.9 . . ?
C12 C28 H28B 107.9 . . ?
H28A C28 H28B 107.2 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C12 C28' C29' 128(2) . . ?
C12 C28' H28C 105.4 . . ?
C29' C28' H28C 105.4 . . ?
C12 C28' H28D 105.4 . . ?
C29' C28' H28D 105.4 . . ?
H28C C28' H28D 106.0 . . ?
C28' C29' H29D 109.5 . . ?
C28' C29' H29E 109.5 . . ?
H29D C29' H29E 109.5 . . ?
C28' C29' H29F 109.5 . . ?
H29D C29' H29F 109.5 . . ?
H29E C29' H29F 109.5 . . ?
C12 C30 C31 112(3) . . ?
C12 C30 H30A 109.1 . . ?
C31 C30 H30A 109.1 . . ?
C12 C30 H30B 109.1 . . ?
C31 C30 H30B 109.1 . . ?
H30A C30 H30B 107.9 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C31' C30' C12 107(3) . . ?
C31' C30' H30C 110.3 . . ?
C12 C30' H30C 110.3 . . ?
C31' C30' H30D 110.3 . . ?
C12 C30' H30D 110.3 . . ?
H30C C30' H30D 108.5 . . ?
C30' C31' H31D 109.5 . . ?
C30' C31' H31E 109.5 . . ?
H31D C31' H31E 109.5 . . ?
C30' C31' H31F 109.5 . . ?
H31D C31' H31F 109.5 . . ?
H31E C31' H31F 109.5 . . ?
N5 C32 H32A 109.5 . . ?
N5 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N5 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?

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
C5 N1 C2 C3 0.9(13) . . . . ?
C5 N1 C2 C1 -178.5(11) . . . . ?
C23' C1 C2 N1 -156.8(16) . . . . ?
C25' C1 C2 N1 -45(3) . . . . ?
C22 C1 C2 N1 77.8(14) . . . . ?
C25 C1 C2 N1 -41(3) . . . . ?
C23 C1 C2 N1 179.2(17) . . . . ?
C23' C1 C2 C3 24(2) . . . . ?
C25' C1 C2 C3 136(2) . . . . ?
C22 C1 C2 C3 -101.5(15) . . . . ?
C25 C1 C2 C3 140(2) . . . . ?
C23 C1 C2 C3 0(2) . . . . ?
N1 C2 C3 C4 -0.8(14) . . . . ?
C1 C2 C3 C4 178.5(13) . . . . ?
C2 C3 C4 C5 0.4(15) . . . . ?
C3 C4 C5 N1 0.1(14) . . . . ?
C3 C4 C5 C6 179.3(13) . . . . ?
C2 N1 C5 C4 -0.6(13) . . . . ?
C2 N1 C5 C6 -179.9(11) . . . . ?
C4 C5 C6 N2 109.0(15) . . . . ?
N1 C5 C6 N2 -71.9(15) . . . . ?
C27 N2 C6 C5 -59.7(14) . . . . ?
C7 N2 C6 C5 173.6(10) . . . . ?
C27 N2 C7 C8 49.6(15) . . . . ?
C6 N2 C7 C8 176.7(11) . . . . ?
C11 N3 C8 C9 -1.0(13) . . . . ?
C11 N3 C8 C7 -179.4(11) . . . . ?
N2 C7 C8 C9 -100.8(15) . . . . ?
N2 C7 C8 N3 77.2(15) . . . . ?
N3 C8 C9 C10 0.2(14) . . . . ?
C7 C8 C9 C10 178.4(12) . . . . ?
C8 C9 C10 C11 0.6(14) . . . . ?
C8 N3 C11 C10 1.3(13) . . . . ?
C8 N3 C11 C12 -179.5(12) . . . . ?
C9 C10 C11 N3 -1.1(13) . . . . ?
C9 C10 C11 C12 179.7(13) . . . . ?
N3 C11 C12 C30 46(3) . . . . ?
C10 C11 C12 C30 -135(2) . . . . ?
N3 C11 C12 C28' 157.9(14) . . . . ?
C10 C11 C12 C28' -23(2) . . . . ?
N3 C11 C12 C13 -73.3(15) . . . . ?
C10 C11 C12 C13 105.7(15) . . . . ?
N3 C11 C12 C30' 46(2) . . . . ?
C10 C11 C12 C30' -135(2) . . . . ?
N3 C11 C12 C28 -177.3(13) . . . . ?
C10 C11 C12 C28 2(2) . . . . ?
C16 N4 C13 C14 0.8(15) . . . . ?
C16 N4 C13 C12 -176.5(11) . . . . ?
C30 C12 C13 N4 -54(2) . . . . ?
C11 C12 C13 N4 77.1(15) . . . . ?
C28' C12 C13 N4 -167.2(17) . . . . ?
C30' C12 C13 N4 -34(2) . . . . ?
C28 C12 C13 N4 -164.8(14) . . . . ?
C30 C12 C13 C14 129.2(19) . . . . ?
C11 C12 C13 C14 -99.7(16) . . . . ?
C28' C12 C13 C14 16(2) . . . . ?
C30' C12 C13 C14 149(2) . . . . ?
C28 C12 C13 C14 18.5(18) . . . . ?
N4 C13 C14 C15 -2.4(15) . . . . ?
C12 C13 C14 C15 174.6(12) . . . . ?
C13 C14 C15 C16 3.2(15) . . . . ?
C14 C15 C16 N4 -2.9(15) . . . . ?
C14 C15 C16 C17 -177.8(13) . . . . ?
C13 N4 C16 C15 1.4(15) . . . . ?
C13 N4 C16 C17 176.8(11) . . . . ?
C15 C16 C17 N5 94.2(16) . . . . ?
N4 C16 C17 N5 -80.2(15) . . . . ?
C32 N5 C17 C16 -52.7(14) . . . . ?
C18 N5 C17 C16 -179.2(10) . . . . ?
C32 N5 C18 C19 58.5(13) . . . . ?
C17 N5 C18 C19 -175.5(10) . . . . ?
C22 N6 C19 C20 1.4(14) . . . . ?
C22 N6 C19 C18 -179.2(10) . . . . ?
N5 C18 C19 C20 -100.7(15) . . . . ?
N5 C18 C19 N6 80.1(13) . . . . ?
N6 C19 C20 C21 -1.6(15) . . . . ?
C18 C19 C20 C21 179.1(12) . . . . ?
C19 C20 C21 C22 1.2(15) . . . . ?
C19 N6 C22 C21 -0.6(13) . . . . ?
C19 N6 C22 C1 177.0(10) . . . . ?
C20 C21 C22 N6 -0.3(14) . . . . ?
C20 C21 C22 C1 -177.7(12) . . . . ?
C23' C1 C22 N6 165.8(17) . . . . ?
C2 C1 C22 N6 -83.6(13) . . . . ?
C25' C1 C22 N6 46(2) . . . . ?
C25 C1 C22 N6 26(2) . . . . ?
C23 C1 C22 N6 158.7(14) . . . . ?
C23' C1 C22 C21 -17(2) . . . . ?
C2 C1 C22 C21 93.6(15) . . . . ?
C25' C1 C22 C21 -136.6(19) . . . . ?
C25 C1 C22 C21 -157.1(19) . . . . ?
C23 C1 C22 C21 -24.1(18) . . . . ?
C23' C1 C23 C24 123(6) . . . . ?
C2 C1 C23 C24 -180(3) . . . . ?
C25' C1 C23 C24 40(4) . . . . ?
C22 C1 C23 C24 -70(3) . . . . ?
C25 C1 C23 C24 53(5) . . . . ?
C2 C1 C23' C24' 69(3) . . . . ?
C25' C1 C23' C24' -55(3) . . . . ?
C22 C1 C23' C24' -176.5(18) . . . . ?
C25 C1 C23' C24' -36(3) . . . . ?
C23 C1 C23' C24' -162(6) . . . . ?
C23' C1 C25 C26 4(3) . . . . ?
C2 C1 C25 C26 -100(2) . . . . ?
C25' C1 C25 C26 71(10) . . . . ?
C22 C1 C25 C26 147(2) . . . . ?
C23 C1 C25 C26 34(4) . . . . ?
C23' C1 C25' C26' -59(6) . . . . ?
C2 C1 C25' C26' -168(5) . . . . ?
C22 C1 C25' C26' 71(6) . . . . ?
C25 C1 C25' C26' -179(16) . . . . ?
C23 C1 C25' C26' -30(7) . . . . ?
C30 C12 C28 C29 -36(3) . . . . ?
C11 C12 C28 C29 -178.3(18) . . . . ?
C28' C12 C28 C29 -115(4) . . . . ?
C13 C12 C28 C29 70(2) . . . . ?
C30' C12 C28 C29 -53(3) . . . . ?
C30 C12 C28' C29' 64(3) . . . . ?
C11 C12 C28' C29' -64(3) . . . . ?
C13 C12 C28' C29' 177(2) . . . . ?
C30' C12 C28' C29' 42(3) . . . . ?
C28 C12 C28' C29' 172(6) . . . . ?
C11 C12 C30 C31 65(3) . . . . ?
C28' C12 C30 C31 -47(3) . . . . ?
C13 C12 C30 C31 -174(2) . . . . ?
C30' C12 C30 C31 64(7) . . . . ?
C28 C12 C30 C31 -74(3) . . . . ?
C30 C12 C30' C31' -11(6) . . . . ?
C11 C12 C30' C31' 170(3) . . . . ?
C28' C12 C30' C31' 64(3) . . . . ?
C13 C12 C30' C31' -75(3) . . . . ?
C28 C12 C30' C31' 39(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1N S2 0.91(6) 2.51(8) 3.314(13) 147(10) .
N2 H2N O3 1.03(6) 1.78(7) 2.788(16) 165(10) .
N2 H2N S1 1.03(6) 2.70(7) 3.700(11) 163(9) .
N2 H2N S2 1.03(6) 2.94(10) 3.597(10) 122(8) .
N3 H3N O2 0.96(6) 2.26(8) 3.099(14) 145(9) .
N3 H3N S1 0.96(6) 2.86(8) 3.710(11) 148(9) .
N4 H4N O2 0.84(6) 2.10(8) 2.875(14) 154(11) .
N4 H4N S1 0.84(6) 3.05(10) 3.625(12) 128(10) .
N5 H5N O3 0.98(6) 1.89(7) 2.862(16) 174(11) .
N5 H5N O1 0.98(6) 2.48(11) 3.066(14) 118(8) .
N5 H5N S1 0.98(6) 2.63(8) 3.482(11) 146(9) .
N6 H6N O1 0.91(6) 2.22(8) 3.041(13) 149(9) .

_refine_diff_density_max         0.224
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.055

_shelxl_version_number           2013-3

