# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_A3X2
_database_code_depnum_ccdc_archive 'CCDC 1042072'
_audit_update_record             
;
2015-01-05 deposited with the CCDC.
2015-01-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H54 N8, C H Cl3'
_chemical_formula_sum            'C55 H55 Cl3 N8'
_chemical_formula_weight         934.42

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.6574(14)
_cell_length_b                   14.7322(19)
_cell_length_c                   17.013(2)
_cell_angle_alpha                66.539(4)
_cell_angle_beta                 80.163(4)
_cell_angle_gamma                80.329(4)
_cell_volume                     2399.5(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9827
_cell_measurement_theta_min      3.03
_cell_measurement_theta_max      29.97

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             984
_exptl_absorpt_coefficient_mu    0.238
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            57588
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8428
_reflns_number_gt                6494
_reflns_threshold_expression     >2σ(I)

__computing_data_collection      'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1999)'
_computing_publication_material  WinGX

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1033P)²+3.4425P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8428
_refine_ls_number_parameters     595
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0662
_refine_ls_wR_factor_ref         0.1956
_refine_ls_wR_factor_gt          0.1844
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.2762(3) 0.4719(2) 0.2649(2) 0.0200(7) Uani 1 1 d . . .
H1A H -0.3409 0.4426 0.2517 0.024 Uiso 1 1 calc R . .
H1B H -0.2079 0.4197 0.2874 0.024 Uiso 1 1 calc R . .
C2 C -0.2230(3) 0.5521(2) 0.1827(2) 0.0190(7) Uani 1 1 d . . .
H2A H -0.2060 0.5281 0.1361 0.023 Uiso 1 1 calc R . .
H2B H -0.2851 0.6107 0.1666 0.023 Uiso 1 1 calc R . .
C3 C -0.0930(3) 0.6669(2) 0.18033(19) 0.0164(7) Uani 1 1 d . . .
H3 H -0.1603 0.7161 0.1608 0.020 Uiso 1 1 calc R . .
C4 C 0.0275(3) 0.6940(2) 0.19185(19) 0.0151(6) Uani 1 1 d . . .
C5 C 0.1157(3) 0.6188(2) 0.23911(19) 0.0159(6) Uani 1 1 d . . .
H5 H 0.0947 0.5539 0.2677 0.019 Uiso 1 1 calc R . .
C6 C 0.2342(3) 0.6418(2) 0.2428(2) 0.0182(7) Uani 1 1 d . . .
H6 H 0.2931 0.5920 0.2741 0.022 Uiso 1 1 calc R . .
C7 C 0.2665(3) 0.7380(2) 0.2006(2) 0.0174(7) Uani 1 1 d . . .
H7 H 0.3479 0.7515 0.2023 0.021 Uiso 1 1 calc R . .
C8 C 0.1785(3) 0.8153(2) 0.15529(19) 0.0146(6) Uani 1 1 d . . .
C9 C 0.0586(3) 0.7911(2) 0.15186(19) 0.0153(6) Uani 1 1 d . . .
H9 H -0.0016 0.8411 0.1222 0.018 Uiso 1 1 calc R . .
C10 C 0.2130(3) 0.9188(2) 0.11341(19) 0.0144(6) Uani 1 1 d . . .
C11 C 0.3415(3) 0.9383(2) 0.09539(19) 0.0161(7) Uani 1 1 d . . .
H11 H 0.4060 0.8853 0.1047 0.019 Uiso 1 1 calc R . .
C12 C 0.3738(3) 1.0335(2) 0.06437(19) 0.0160(7) Uani 1 1 d . . .
H12 H 0.4597 1.0440 0.0550 0.019 Uiso 1 1 calc R . .
C13 C 0.2793(3) 1.1152(2) 0.04662(19) 0.0161(7) Uani 1 1 d . . .
C14 C 0.1515(3) 1.0970(2) 0.0597(2) 0.0197(7) Uani 1 1 d . . .
H14 H 0.0874 1.1502 0.0456 0.024 Uiso 1 1 calc R . .
C15 C 0.1192(3) 1.0006(2) 0.0935(2) 0.0195(7) Uani 1 1 d . . .
H15 H 0.0334 0.9900 0.1031 0.023 Uiso 1 1 calc R . .
C16 C 0.3117(3) 1.2177(2) 0.01826(19) 0.0178(7) Uani 1 1 d . . .
H16 H 0.2457 1.2695 0.0100 0.021 Uiso 1 1 calc R . .
C17 C 0.4458(3) 1.3407(2) -0.0162(2) 0.0208(7) Uani 1 1 d . . .
H17A H 0.3669 1.3835 -0.0323 0.025 Uiso 1 1 calc R . .
H17B H 0.5115 1.3614 -0.0648 0.025 Uiso 1 1 calc R . .
C18 C 0.4858(3) 1.3509(2) 0.0608(2) 0.0170(7) Uani 1 1 d . . .
H18A H 0.5553 1.2996 0.0827 0.020 Uiso 1 1 calc R . .
H18B H 0.5178 1.4149 0.0423 0.020 Uiso 1 1 calc R . .
C19 C 0.2963(3) 1.4360(2) 0.1136(2) 0.0173(7) Uani 1 1 d . . .
H19A H 0.2911 1.4685 0.0521 0.021 Uiso 1 1 calc R . .
H19B H 0.3331 1.4797 0.1314 0.021 Uiso 1 1 calc R . .
C20 C 0.1623(3) 1.4209(2) 0.1602(2) 0.0193(7) Uani 1 1 d . . .
H20A H 0.1676 1.3720 0.2185 0.023 Uiso 1 1 calc R . .
H20B H 0.1205 1.4830 0.1639 0.023 Uiso 1 1 calc R . .
C21 C 0.0245(3) 1.3138(2) 0.1594(2) 0.0205(7) Uani 1 1 d . . .
H21 H 0.0336 1.2808 0.2178 0.025 Uiso 1 1 calc R . .
C22 C -0.0620(3) 1.2782(2) 0.1209(2) 0.0180(7) Uani 1 1 d . . .
C23 C -0.0976(3) 1.3360(2) 0.0390(2) 0.0176(7) Uani 1 1 d . . .
H23 H -0.0690 1.3983 0.0083 0.021 Uiso 1 1 calc R . .
C24 C -0.1759(3) 1.3000(2) 0.0040(2) 0.0169(7) Uani 1 1 d . . .
H24 H -0.2000 1.3386 -0.0506 0.020 Uiso 1 1 calc R . .
C25 C -0.2190(3) 1.2078(2) 0.0485(2) 0.0158(6) Uani 1 1 d . . .
H25 H -0.2715 1.1851 0.0234 0.019 Uiso 1 1 calc R . .
C26 C -0.1847(3) 1.1477(2) 0.13112(19) 0.0144(6) Uani 1 1 d . . .
C27 C -0.1060(3) 1.1858(2) 0.1658(2) 0.0164(7) Uani 1 1 d . . .
H27 H -0.0824 1.1478 0.2207 0.020 Uiso 1 1 calc R . .
C28 C -0.2307(3) 1.0487(2) 0.17895(19) 0.0148(6) Uani 1 1 d . . .
C29 C -0.2731(3) 0.9965(2) 0.1369(2) 0.0169(7) Uani 1 1 d . . .
H29 H -0.2688 1.0236 0.0770 0.020 Uiso 1 1 calc R . .
C30 C -0.3206(3) 0.9067(2) 0.18160(19) 0.0157(6) Uani 1 1 d . . .
H30 H -0.3496 0.8747 0.1518 0.019 Uiso 1 1 calc R . .
C31 C -0.3260(3) 0.8627(2) 0.2710(2) 0.0157(6) Uani 1 1 d . . .
C32 C -0.2805(3) 0.9123(2) 0.3134(2) 0.0186(7) Uani 1 1 d . . .
H32 H -0.2802 0.8831 0.3729 0.022 Uiso 1 1 calc R . .
C33 C -0.2362(3) 1.0038(2) 0.2685(2) 0.0182(7) Uani 1 1 d . . .
H33 H -0.2093 1.0364 0.2985 0.022 Uiso 1 1 calc R . .
C34 C -0.3802(3) 0.7681(2) 0.32213(19) 0.0161(7) Uani 1 1 d . . .
H34 H -0.3618 0.7343 0.3788 0.019 Uiso 1 1 calc R . .
C35 C -0.5013(3) 0.6388(2) 0.3532(2) 0.0188(7) Uani 1 1 d . . .
H35A H -0.5939 0.6505 0.3628 0.023 Uiso 1 1 calc R . .
H35B H -0.4681 0.6178 0.4081 0.023 Uiso 1 1 calc R . .
C36 C -0.4638(3) 0.5571(2) 0.3173(2) 0.0191(7) Uani 1 1 d . . .
H36A H -0.5218 0.5062 0.3453 0.023 Uiso 1 1 calc R . .
H36B H -0.4721 0.5850 0.2560 0.023 Uiso 1 1 calc R . .
C37 C -0.3273(3) 0.4344(2) 0.4176(2) 0.0216(7) Uani 1 1 d . . .
H37A H -0.3385 0.3711 0.4161 0.026 Uiso 1 1 calc R . .
H37B H -0.3974 0.4500 0.4564 0.026 Uiso 1 1 calc R . .
C38 C -0.2018(3) 0.4247(2) 0.4522(2) 0.0239(7) Uani 1 1 d . . .
H38A H -0.1890 0.3602 0.4987 0.029 Uiso 1 1 calc R . .
H38B H -0.1315 0.4291 0.4068 0.029 Uiso 1 1 calc R . .
C39 C -0.1292(3) 0.5696(2) 0.4420(2) 0.0215(7) Uani 1 1 d . . .
H39 H -0.0775 0.5650 0.3935 0.026 Uiso 1 1 calc R . .
C40 C -0.1211(3) 0.6538(2) 0.4662(2) 0.0202(7) Uani 1 1 d . . .
C41 C -0.0356(3) 0.7226(2) 0.4176(2) 0.0188(7) Uani 1 1 d . . .
H41 H 0.0135 0.7159 0.3691 0.023 Uiso 1 1 calc R . .
C42 C -0.0217(3) 0.8019(2) 0.4399(2) 0.0190(7) Uani 1 1 d . . .
C43 C -0.0977(3) 0.8103(3) 0.5124(2) 0.0239(8) Uani 1 1 d . . .
H43 H -0.0897 0.8621 0.5288 0.029 Uiso 1 1 calc R . .
C44 C -0.1843(3) 0.7436(3) 0.5602(2) 0.0289(8) Uani 1 1 d . . .
H44 H -0.2351 0.7515 0.6077 0.035 Uiso 1 1 calc R . .
C45 C -0.1965(3) 0.6650(3) 0.5385(2) 0.0261(8) Uani 1 1 d . . .
H45 H -0.2544 0.6196 0.5716 0.031 Uiso 1 1 calc R . .
C46 C 0.0731(3) 0.8730(2) 0.39025(19) 0.0179(7) Uani 1 1 d . . .
C47 C 0.1888(3) 0.8438(2) 0.35009(19) 0.0178(7) Uani 1 1 d . . .
H47 H 0.2046 0.7790 0.3518 0.021 Uiso 1 1 calc R . .
C48 C 0.2803(3) 0.9078(2) 0.30809(19) 0.0188(7) Uani 1 1 d . . .
H48 H 0.3561 0.8860 0.2814 0.023 Uiso 1 1 calc R . .
C49 C 0.2606(3) 1.0053(2) 0.30497(19) 0.0187(7) Uani 1 1 d . . .
C50 C 0.1430(3) 1.0366(2) 0.3423(2) 0.0195(7) Uani 1 1 d . . .
H50 H 0.1266 1.1020 0.3389 0.023 Uiso 1 1 calc R . .
C51 C 0.0511(3) 0.9726(2) 0.3839(2) 0.0202(7) Uani 1 1 d . . .
H51 H -0.0264 0.9953 0.4080 0.024 Uiso 1 1 calc R . .
C52 C 0.3643(3) 1.0697(2) 0.2688(2) 0.0193(7) Uani 1 1 d . . .
H52 H 0.4329 1.0534 0.2332 0.023 Uiso 1 1 calc R . .
C53 C 0.4743(3) 1.2015(2) 0.2516(2) 0.0221(7) Uani 1 1 d . . .
H53A H 0.5270 1.1803 0.2082 0.027 Uiso 1 1 calc R . .
H53B H 0.5251 1.1872 0.2982 0.027 Uiso 1 1 calc R . .
C54 C 0.4339(3) 1.3124(2) 0.2124(2) 0.0179(7) Uani 1 1 d . . .
H54A H 0.3701 1.3312 0.2528 0.022 Uiso 1 1 calc R . .
H54B H 0.5075 1.3479 0.2029 0.022 Uiso 1 1 calc R . .
N1 N -0.3329(2) 0.51204(19) 0.33070(16) 0.0165(6) Uani 1 1 d . . .
N2 N -0.1056(2) 0.5776(2) 0.19681(16) 0.0175(6) Uani 1 1 d . . .
N3 N 0.4265(3) 1.2378(2) 0.00472(17) 0.0196(6) Uani 1 1 d . . .
N4 N 0.3812(2) 1.34260(18) 0.13061(16) 0.0140(5) Uani 1 1 d . . .
N5 N 0.0861(2) 1.3872(2) 0.11590(17) 0.0201(6) Uani 1 1 d . . .
N6 N -0.4501(2) 0.73073(19) 0.29298(16) 0.0163(6) Uani 1 1 d . . .
N7 N -0.2028(3) 0.5035(2) 0.48398(18) 0.0240(6) Uani 1 1 d . . .
N8 N 0.3628(3) 1.1464(2) 0.28468(17) 0.0214(6) Uani 1 1 d . . .
Cl1 Cl -0.21892(10) 0.19012(8) 0.38572(7) 0.0455(3) Uani 1 1 d . . .
Cl2 Cl -0.33023(11) 0.00681(7) 0.48412(7) 0.0436(3) Uani 1 1 d . . .
Cl3 Cl -0.47478(11) 0.19291(8) 0.47800(8) 0.0492(3) Uani 1 1 d . . .
C55 C -0.3208(4) 0.1260(3) 0.4770(3) 0.0384(10) Uani 1 1 d . . .
H55 H -0.2841 0.1201 0.5281 0.046 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 N1 1.464(4) . ?
C1 C2 1.521(4) . ?
C2 N2 1.448(4) . ?
C3 N2 1.257(4) . ?
C3 C4 1.473(4) . ?
C4 C9 1.388(4) . ?
C4 C5 1.399(4) . ?
C5 C6 1.379(4) . ?
C6 C7 1.382(4) . ?
C7 C8 1.400(4) . ?
C8 C9 1.400(4) . ?
C8 C10 1.484(4) . ?
C10 C15 1.397(4) . ?
C10 C11 1.403(4) . ?
C11 C12 1.370(4) . ?
C12 C13 1.401(4) . ?
C13 C14 1.397(4) . ?
C13 C16 1.473(4) . ?
C14 C15 1.383(5) . ?
C16 N3 1.268(4) . ?
C17 N3 1.456(4) . ?
C17 C18 1.514(4) . ?
C18 N4 1.465(4) . ?
C19 N4 1.466(4) . ?
C19 C20 1.515(4) . ?
C20 N5 1.454(4) . ?
C21 N5 1.258(4) . ?
C21 C22 1.482(5) . ?
C22 C27 1.386(4) . ?
C22 C23 1.392(5) . ?
C23 C24 1.380(5) . ?
C24 C25 1.379(4) . ?
C25 C26 1.404(4) . ?
C26 C27 1.398(4) . ?
C26 C28 1.480(4) . ?
C28 C33 1.393(4) . ?
C28 C29 1.406(4) . ?
C29 C30 1.370(4) . ?
C30 C31 1.391(4) . ?
C31 C32 1.396(4) . ?
C31 C34 1.471(4) . ?
C32 C33 1.377(4) . ?
C34 N6 1.260(4) . ?
C35 N6 1.461(4) . ?
C35 C36 1.524(5) . ?
C36 N1 1.455(4) . ?
C37 N1 1.470(4) . ?
C37 C38 1.515(5) . ?
C38 N7 1.461(4) . ?
C39 N7 1.260(4) . ?
C39 C40 1.474(5) . ?
C40 C41 1.388(5) . ?
C40 C45 1.402(5) . ?
C41 C42 1.401(5) . ?
C42 C43 1.393(4) . ?
C42 C46 1.480(5) . ?
C43 C44 1.376(5) . ?
C44 C45 1.380(5) . ?
C46 C47 1.393(4) . ?
C46 C51 1.410(4) . ?
C47 C48 1.373(5) . ?
C48 C49 1.398(4) . ?
C49 C50 1.397(5) . ?
C49 C52 1.467(5) . ?
C50 C51 1.375(5) . ?
C52 N8 1.261(4) . ?
C53 N8 1.455(4) . ?
C53 C54 1.515(4) . ?
C54 N4 1.463(4) . ?
Cl1 C55 1.757(4) . ?
Cl2 C55 1.730(4) . ?
Cl3 C55 1.767(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 111.7(3) . . ?
N2 C2 C1 109.4(3) . . ?
N2 C3 C4 120.4(3) . . ?
C9 C4 C5 119.7(3) . . ?
C9 C4 C3 121.2(3) . . ?
C5 C4 C3 118.9(3) . . ?
C6 C5 C4 119.4(3) . . ?
C5 C6 C7 120.8(3) . . ?
C6 C7 C8 121.0(3) . . ?
C7 C8 C9 117.6(3) . . ?
C7 C8 C10 120.3(3) . . ?
C9 C8 C10 122.1(3) . . ?
C4 C9 C8 121.4(3) . . ?
C15 C10 C11 117.5(3) . . ?
C15 C10 C8 121.5(3) . . ?
C11 C10 C8 121.0(3) . . ?
C12 C11 C10 121.4(3) . . ?
C11 C12 C13 120.9(3) . . ?
C14 C13 C12 118.1(3) . . ?
C14 C13 C16 120.1(3) . . ?
C12 C13 C16 121.7(3) . . ?
C15 C14 C13 120.6(3) . . ?
C14 C15 C10 121.3(3) . . ?
N3 C16 C13 122.3(3) . . ?
N3 C17 C18 109.9(3) . . ?
N4 C18 C17 113.1(3) . . ?
N4 C19 C20 113.0(2) . . ?
N5 C20 C19 111.5(3) . . ?
N5 C21 C22 122.3(3) . . ?
C27 C22 C23 119.5(3) . . ?
C27 C22 C21 120.0(3) . . ?
C23 C22 C21 120.5(3) . . ?
C24 C23 C22 119.3(3) . . ?
C25 C24 C23 121.2(3) . . ?
C24 C25 C26 120.8(3) . . ?
C27 C26 C25 117.2(3) . . ?
C27 C26 C28 121.9(3) . . ?
C25 C26 C28 120.9(3) . . ?
C22 C27 C26 122.0(3) . . ?
C33 C28 C29 116.9(3) . . ?
C33 C28 C26 121.2(3) . . ?
C29 C28 C26 121.9(3) . . ?
C30 C29 C28 121.8(3) . . ?
C29 C30 C31 120.8(3) . . ?
C30 C31 C32 118.0(3) . . ?
C30 C31 C34 122.8(3) . . ?
C32 C31 C34 119.2(3) . . ?
C33 C32 C31 121.0(3) . . ?
C32 C33 C28 121.4(3) . . ?
N6 C34 C31 123.3(3) . . ?
N6 C35 C36 110.3(3) . . ?
N1 C36 C35 111.5(3) . . ?
N1 C37 C38 112.3(3) . . ?
N7 C38 C37 110.1(3) . . ?
N7 C39 C40 123.0(3) . . ?
C41 C40 C45 119.2(3) . . ?
C41 C40 C39 119.6(3) . . ?
C45 C40 C39 121.2(3) . . ?
C40 C41 C42 121.5(3) . . ?
C43 C42 C41 117.7(3) . . ?
C43 C42 C46 120.6(3) . . ?
C41 C42 C46 121.6(3) . . ?
C44 C43 C42 121.3(3) . . ?
C43 C44 C45 120.7(3) . . ?
C44 C45 C40 119.6(3) . . ?
C47 C46 C51 117.3(3) . . ?
C47 C46 C42 121.6(3) . . ?
C51 C46 C42 121.1(3) . . ?
C48 C47 C46 121.9(3) . . ?
C47 C48 C49 120.7(3) . . ?
C50 C49 C48 117.9(3) . . ?
C50 C49 C52 121.6(3) . . ?
C48 C49 C52 120.3(3) . . ?
C51 C50 C49 121.3(3) . . ?
C50 C51 C46 120.8(3) . . ?
N8 C52 C49 121.7(3) . . ?
N8 C53 C54 110.8(3) . . ?
N4 C54 C53 112.6(3) . . ?
C36 N1 C1 111.2(2) . . ?
C36 N1 C37 110.9(2) . . ?
C1 N1 C37 110.7(2) . . ?
C3 N2 C2 119.9(3) . . ?
C16 N3 C17 117.1(3) . . ?
C54 N4 C18 109.7(2) . . ?
C54 N4 C19 110.6(2) . . ?
C18 N4 C19 111.7(2) . . ?
C21 N5 C20 118.5(3) . . ?
C34 N6 C35 116.6(3) . . ?
C39 N7 C38 117.2(3) . . ?
C52 N8 C53 118.0(3) . . ?
Cl2 C55 Cl1 111.4(2) . . ?
Cl2 C55 Cl3 111.0(2) . . ?
Cl1 C55 Cl3 111.2(2) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.093
####################################################################### 
# 
# 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_B3X
_database_code_depnum_ccdc_archive 'CCDC 1042073'
_audit_update_record             
;
2015-01-05 deposited with the CCDC.
2015-01-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H42 N4 O6'
_chemical_formula_sum            'C48 H42 N4 O6'
_chemical_formula_weight         770.86

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

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'P -3 c 1'
_symmetry_space_group_name_Hall  '-P 3 2"c'

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

_cell_length_a                   13.5006(14)
_cell_length_b                   13.5006(14)
_cell_length_c                   29.691(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     4686.6(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9928
_cell_measurement_theta_min      3.02
_cell_measurement_theta_max      20.59

_exptl_crystal_description       ROD
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1624
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_correction_T_min  0.978
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            87701
_diffrn_reflns_av_R_equivalents  0.1517
_diffrn_reflns_av_sigmaI/netI    0.0600
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2756
_reflns_number_gt                2115
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1999)'
_computing_publication_material  WinGX

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1251P)²+9.3855P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2756
_refine_ls_number_parameters     175
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1766
_refine_ls_R_factor_gt           0.1320
_refine_ls_wR_factor_ref         0.3269
_refine_ls_wR_factor_gt          0.3032
_refine_ls_goodness_of_fit_ref   1.292
_refine_ls_restrained_S_all      1.292
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4996(4) 0.9319(4) 0.16384(17) 0.0286(13) Uani 1 1 d . . .
C2 C 0.5481(5) 0.9674(4) 0.12048(18) 0.0308(13) Uani 1 1 d . . .
H2 H 0.6270 1.0128 0.1177 0.037 Uiso 1 1 calc R . .
C3 C 0.4828(5) 0.9371(4) 0.08302(17) 0.0311(13) Uani 1 1 d . . .
H3 H 0.5186 0.9625 0.0553 0.037 Uiso 1 1 calc R . .
C4 C 0.3617(4) 0.8682(4) 0.08419(16) 0.0255(12) Uani 1 1 d . . .
C5 C 0.3135(5) 0.8349(4) 0.12629(18) 0.0319(13) Uani 1 1 d . . .
H5 H 0.2343 0.7913 0.1285 0.038 Uiso 1 1 calc R . .
C7 C 0.2951(5) 0.8385(4) 0.04207(18) 0.0317(13) Uani 1 1 d . . .
C8 C 0.3425(5) 0.8304(4) 0.00121(18) 0.0326(13) Uani 1 1 d . . .
H8 H 0.4153 0.8391 0.0008 0.039 Uiso 1 1 calc R . .
C6 C 0.3780(5) 0.8636(4) 0.16596(17) 0.0314(13) Uani 1 1 d . . .
C9 C 0.2818(5) 0.8098(4) -0.03861(18) 0.0366(15) Uani 1 1 d . . .
H9 H 0.3141 0.8043 -0.0655 0.044 Uiso 1 1 calc R . .
C10 C 0.1732(5) 0.7970(5) -0.03875(17) 0.0355(14) Uani 1 1 d . . .
C11 C 0.1230(5) 0.7973(5) 0.00159(18) 0.0382(14) Uani 1 1 d . . .
H11 H 0.0482 0.7833 0.0019 0.046 Uiso 1 1 calc R . .
C12 C 0.1827(5) 0.8181(5) 0.04165(18) 0.0361(14) Uani 1 1 d . . .
H12 H 0.1478 0.8187 0.0686 0.043 Uiso 1 1 calc R . .
C13 C 0.1124(5) 0.7840(5) -0.0814(2) 0.0442(16) Uani 1 1 d . . .
H13 H 0.0381 0.7713 -0.0798 0.053 Uiso 1 1 calc R . .
C14 C 0.3212(5) 0.8315(4) 0.20800(18) 0.0340(14) Uani 1 1 d . . .
H14 H 0.2418 0.7877 0.2084 0.041 Uiso 1 1 calc R . .
C15 C 0.3221(5) 0.8401(5) 0.29047(16) 0.0336(14) Uani 1 1 d . . .
H15A H 0.2400 0.7916 0.2874 0.040 Uiso 1 1 calc R . .
H15B H 0.3374 0.9119 0.3038 0.040 Uiso 1 1 calc R . .
C16 C 0.3688(5) 0.7822(5) 0.32069(16) 0.0326(14) Uani 1 1 d . . .
H16A H 0.4517 0.8270 0.3210 0.039 Uiso 1 1 calc R . .
H16B H 0.3419 0.7793 0.3512 0.039 Uiso 1 1 calc R . .
N1 N 0.3760(4) 0.8611(4) 0.24642(13) 0.0302(11) Uani 1 1 d . . .
N2 N 0.3333 0.6667 0.3055(2) 0.0244(17) Uani 1 3 d S . .
O1 O 0.5634(3) 0.9605(3) 0.19990(12) 0.0359(10) Uani 1 1 d . . .
H1 H 0.5227 0.9335 0.2222 0.054 Uiso 1 1 calc R . .
O2 O 0.1516(4) 0.7885(4) -0.11818(14) 0.0534(13) Uani 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 1.306(6) . ?
C1 C2 1.415(7) . ?
C1 C6 1.427(7) . ?
C2 C3 1.349(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.421(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.377(7) . ?
C4 C7 1.474(7) . ?
C5 C6 1.399(7) . ?
C5 H5 0.9300 . ?
C7 C8 1.401(7) . ?
C7 C12 1.401(8) . ?
C8 C9 1.385(8) . ?
C8 H8 0.9300 . ?
C6 C14 1.415(7) . ?
C9 C10 1.388(8) . ?
C9 H9 0.9300 . ?
C10 C11 1.377(8) . ?
C10 C13 1.472(8) . ?
C11 C12 1.385(7) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 O2 1.201(7) . ?
C13 H13 0.9300 . ?
C14 N1 1.309(7) . ?
C14 H14 0.9300 . ?
C15 N1 1.454(6) . ?
C15 C16 1.518(7) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 N2 1.455(6) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
N2 C16 1.455(6) 2_665 ?
N2 C16 1.455(6) 3_565 ?
O1 H1 0.8200 . ?

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 C1 C2 121.4(5) . . ?
O1 C1 C6 122.1(5) . . ?
C2 C1 C6 116.6(5) . . ?
C3 C2 C1 121.7(5) . . ?
C3 C2 H2 119.1 . . ?
C1 C2 H2 119.1 . . ?
C2 C3 C4 122.8(5) . . ?
C2 C3 H3 118.6 . . ?
C4 C3 H3 118.6 . . ?
C5 C4 C3 115.9(5) . . ?
C5 C4 C7 123.9(5) . . ?
C3 C4 C7 120.2(5) . . ?
C4 C5 C6 123.2(5) . . ?
C4 C5 H5 118.4 . . ?
C6 C5 H5 118.4 . . ?
C8 C7 C12 118.0(5) . . ?
C8 C7 C4 121.1(5) . . ?
C12 C7 C4 120.9(5) . . ?
C9 C8 C7 120.5(5) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C5 C6 C14 119.4(5) . . ?
C5 C6 C1 119.8(5) . . ?
C14 C6 C1 120.6(5) . . ?
C8 C9 C10 120.6(5) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 H9 119.7 . . ?
C11 C10 C9 119.2(5) . . ?
C11 C10 C13 120.2(6) . . ?
C9 C10 C13 120.6(5) . . ?
C10 C11 C12 120.7(6) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C11 C12 C7 120.7(5) . . ?
C11 C12 H12 119.6 . . ?
C7 C12 H12 119.6 . . ?
O2 C13 C10 124.8(6) . . ?
O2 C13 H13 117.6 . . ?
C10 C13 H13 117.6 . . ?
N1 C14 C6 122.6(5) . . ?
N1 C14 H14 118.7 . . ?
C6 C14 H14 118.7 . . ?
N1 C15 C16 109.7(4) . . ?
N1 C15 H15A 109.7 . . ?
C16 C15 H15A 109.7 . . ?
N1 C15 H15B 109.7 . . ?
C16 C15 H15B 109.7 . . ?
H15A C15 H15B 108.2 . . ?
N2 C16 C15 111.7(4) . . ?
N2 C16 H16A 109.3 . . ?
C15 C16 H16A 109.3 . . ?
N2 C16 H16B 109.3 . . ?
C15 C16 H16B 109.3 . . ?
H16A C16 H16B 107.9 . . ?
C14 N1 C15 125.0(5) . . ?
C16 N2 C16 110.9(3) . 2_665 ?
C16 N2 C16 110.9(3) . 3_565 ?
C16 N2 C16 110.9(3) 2_665 3_565 ?
C1 O1 H1 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
O1 C1 C2 C3 179.3(5) . . . . ?
C6 C1 C2 C3 -0.7(7) . . . . ?
C1 C2 C3 C4 0.1(8) . . . . ?
C2 C3 C4 C5 1.1(7) . . . . ?
C2 C3 C4 C7 179.7(5) . . . . ?
C3 C4 C5 C6 -1.6(7) . . . . ?
C7 C4 C5 C6 179.8(5) . . . . ?
C5 C4 C7 C8 -152.9(5) . . . . ?
C3 C4 C7 C8 28.5(7) . . . . ?
C5 C4 C7 C12 27.5(8) . . . . ?
C3 C4 C7 C12 -151.0(5) . . . . ?
C12 C7 C8 C9 3.8(7) . . . . ?
C4 C7 C8 C9 -175.8(5) . . . . ?
C4 C5 C6 C14 176.4(5) . . . . ?
C4 C5 C6 C1 1.0(8) . . . . ?
O1 C1 C6 C5 -179.7(5) . . . . ?
C2 C1 C6 C5 0.2(7) . . . . ?
O1 C1 C6 C14 4.9(8) . . . . ?
C2 C1 C6 C14 -175.1(5) . . . . ?
C7 C8 C9 C10 0.2(8) . . . . ?
C8 C9 C10 C11 -4.5(8) . . . . ?
C8 C9 C10 C13 175.2(5) . . . . ?
C9 C10 C11 C12 4.6(8) . . . . ?
C13 C10 C11 C12 -175.1(5) . . . . ?
C10 C11 C12 C7 -0.6(8) . . . . ?
C8 C7 C12 C11 -3.6(8) . . . . ?
C4 C7 C12 C11 176.0(5) . . . . ?
C11 C10 C13 O2 176.1(6) . . . . ?
C9 C10 C13 O2 -3.6(9) . . . . ?
C5 C6 C14 N1 -176.1(5) . . . . ?
C1 C6 C14 N1 -0.7(8) . . . . ?
N1 C15 C16 N2 -67.9(6) . . . . ?
C6 C14 N1 C15 173.8(5) . . . . ?
C16 C15 N1 C14 128.7(5) . . . . ?
C15 C16 N2 C16 -81.2(7) . . . 2_665 ?
C15 C16 N2 C16 155.2(5) . . . 3_565 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.076
# 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 0.000 0.000 -0.001 1127 217 ' '
_platon_squeeze_details          
;
;

####################################################################### 
# 
# 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_B3X2
_database_code_depnum_ccdc_archive 'CCDC 1042074'
_audit_update_record             
;
2015-01-05 deposited with the CCDC.
2015-01-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H54 N8 O3, 2(C H Cl3)'
_chemical_formula_sum            'C56 H56 Cl6 N8 O3'
_chemical_formula_weight         1101.79

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   17.6515(12)
_cell_length_b                   27.3690(18)
_cell_length_c                   11.1516(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.653(2)
_cell_angle_gamma                90.00
_cell_volume                     5256.5(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9883
_cell_measurement_theta_min      3.06
_cell_measurement_theta_max      23.27

_exptl_crystal_description       Rod
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2296
_exptl_absorpt_coefficient_mu    0.381
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_correction_T_min  0.846
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            134692
_diffrn_reflns_av_R_equivalents  0.1069
_diffrn_reflns_av_sigmaI/netI    0.0507
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.98
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9243
_reflns_number_gt                6459
_reflns_threshold_expression     >2σ(I)

__computing_data_collection      'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1999)'
_computing_publication_material  WinGX

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0517P)²+5.6050P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9243
_refine_ls_number_parameters     658
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0552
_refine_ls_wR_factor_ref         0.1279
_refine_ls_wR_factor_gt          0.1146
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.14038(18) 0.56002(11) 0.3409(3) 0.0255(7) Uani 1 1 d . . .
H1A H 0.1704 0.5302 0.3603 0.031 Uiso 1 1 calc R . .
H1B H 0.1020 0.5609 0.3911 0.031 Uiso 1 1 calc R . .
C2 C 0.19393(18) 0.60372(12) 0.3719(3) 0.0279(7) Uani 1 1 d . . .
H2A H 0.1679 0.6328 0.3334 0.033 Uiso 1 1 calc R . .
H2B H 0.2061 0.6088 0.4602 0.033 Uiso 1 1 calc R . .
C3 C 0.28103(18) 0.62662(11) 0.2530(3) 0.0249(7) Uani 1 1 d . . .
H3 H 0.2457 0.6516 0.2257 0.030 Uiso 1 1 calc R . .
C4 C 0.35205(18) 0.62459(11) 0.2055(3) 0.0255(7) Uani 1 1 d . . .
C5 C 0.37139(18) 0.66449(11) 0.1400(3) 0.0250(7) Uani 1 1 d . . .
H5 H 0.3372 0.6907 0.1222 0.030 Uiso 1 1 calc R . .
C6 C 0.44032(18) 0.66572(11) 0.1011(3) 0.0260(7) Uani 1 1 d . . .
H6 H 0.4520 0.6929 0.0583 0.031 Uiso 1 1 calc R . .
C7 C 0.49313(18) 0.62682(11) 0.1249(3) 0.0246(7) Uani 1 1 d . . .
C8 C 0.47164(19) 0.58616(11) 0.1870(3) 0.0286(8) Uani 1 1 d . . .
H8 H 0.5044 0.5592 0.2012 0.034 Uiso 1 1 calc R . .
C9 C 0.40341(19) 0.58531(11) 0.2271(3) 0.0282(8) Uani 1 1 d . . .
H9 H 0.3913 0.5581 0.2693 0.034 Uiso 1 1 calc R . .
C10 C 0.56908(18) 0.62981(11) 0.0897(3) 0.0255(7) Uani 1 1 d . . .
C11 C 0.57996(18) 0.65737(11) -0.0095(3) 0.0254(7) Uani 1 1 d . . .
H11 H 0.5379 0.6745 -0.0555 0.030 Uiso 1 1 calc R . .
C12 C 0.65159(18) 0.66048(11) -0.0434(3) 0.0265(7) Uani 1 1 d . . .
C13 C 0.71605(18) 0.63546(12) 0.0278(3) 0.0300(8) Uani 1 1 d . . .
C14 C 0.7059(2) 0.60779(12) 0.1269(3) 0.0336(8) Uani 1 1 d . . .
H14 H 0.7479 0.5910 0.1739 0.040 Uiso 1 1 calc R . .
C15 C 0.63404(19) 0.60485(12) 0.1570(3) 0.0299(8) Uani 1 1 d . . .
H15 H 0.6287 0.5858 0.2237 0.036 Uiso 1 1 calc R . .
C16 C 0.65924(18) 0.68903(11) -0.1500(3) 0.0272(7) Uani 1 1 d . . .
H16 H 0.6153 0.7036 -0.1981 0.033 Uiso 1 1 calc R . .
C17 C 0.73000(19) 0.72565(12) -0.2825(3) 0.0322(8) Uani 1 1 d . . .
H17A H 0.7636 0.7532 -0.2537 0.039 Uiso 1 1 calc R . .
H17B H 0.6790 0.7382 -0.3204 0.039 Uiso 1 1 calc R . .
C18 C 0.76229(18) 0.69720(12) -0.3766(3) 0.0330(8) Uani 1 1 d . . .
H18A H 0.7823 0.7198 -0.4291 0.040 Uiso 1 1 calc R . .
H18B H 0.8050 0.6769 -0.3348 0.040 Uiso 1 1 calc R . .
C19 C 0.65459(19) 0.69521(12) -0.5511(3) 0.0314(8) Uani 1 1 d . . .
H19A H 0.6770 0.6935 -0.6231 0.038 Uiso 1 1 calc R . .
H19B H 0.6556 0.7291 -0.5255 0.038 Uiso 1 1 calc R . .
C20 C 0.57145(18) 0.67827(12) -0.5858(3) 0.0303(8) Uani 1 1 d . . .
H20A H 0.5463 0.6927 -0.6638 0.036 Uiso 1 1 calc R . .
H20B H 0.5701 0.6430 -0.5953 0.036 Uiso 1 1 calc R . .
C21 C 0.47676(18) 0.66362(11) -0.4738(3) 0.0254(7) Uani 1 1 d . . .
H21 H 0.4688 0.6348 -0.5191 0.031 Uiso 1 1 calc R . .
C22 C 0.42792(17) 0.67314(11) -0.3865(3) 0.0228(7) Uani 1 1 d . . .
C23 C 0.36342(17) 0.64391(11) -0.3867(3) 0.0250(7) Uani 1 1 d . . .
H23 H 0.3530 0.6177 -0.4408 0.030 Uiso 1 1 calc R . .
C24 C 0.31489(17) 0.65306(11) -0.3083(3) 0.0231(7) Uani 1 1 d . . .
H24 H 0.2717 0.6332 -0.3117 0.028 Uiso 1 1 calc R . .
C25 C 0.32888(17) 0.69133(10) -0.2240(3) 0.0211(7) Uani 1 1 d . . .
C26 C 0.39478(17) 0.71992(11) -0.2218(3) 0.0230(7) Uani 1 1 d . . .
H26 H 0.4066 0.7452 -0.1650 0.028 Uiso 1 1 calc R . .
C27 C 0.44245(18) 0.71135(11) -0.3019(3) 0.0248(7) Uani 1 1 d . . .
H27 H 0.4852 0.7314 -0.2996 0.030 Uiso 1 1 calc R . .
C28 C 0.27450(16) 0.70204(10) -0.1439(3) 0.0203(7) Uani 1 1 d . . .
C29 C 0.22407(17) 0.66699(11) -0.1152(3) 0.0216(7) Uani 1 1 d . . .
H29 H 0.2262 0.6355 -0.1455 0.026 Uiso 1 1 calc R . .
C30 C 0.17087(16) 0.67693(11) -0.0436(3) 0.0223(7) Uani 1 1 d . . .
C31 C 0.16796(17) 0.72428(11) 0.0047(3) 0.0236(7) Uani 1 1 d . . .
C32 C 0.11598(17) 0.63943(11) -0.0221(3) 0.0252(7) Uani 1 1 d . . .
H32 H 0.1179 0.6085 -0.0559 0.030 Uiso 1 1 calc R . .
C33 C 0.01185(17) 0.60958(11) 0.0575(3) 0.0272(7) Uani 1 1 d . . .
H33A H 0.0146 0.5830 0.0012 0.033 Uiso 1 1 calc R . .
H33B H -0.0407 0.6223 0.0388 0.033 Uiso 1 1 calc R . .
C34 C 0.21879(18) 0.75954(11) -0.0208(3) 0.0260(7) Uani 1 1 d . . .
H34 H 0.2181 0.7908 0.0116 0.031 Uiso 1 1 calc R . .
C35 C 0.03157(17) 0.59080(11) 0.1884(3) 0.0250(7) Uani 1 1 d . . .
H35A H 0.0407 0.6183 0.2446 0.030 Uiso 1 1 calc R . .
H35B H -0.0122 0.5725 0.2045 0.030 Uiso 1 1 calc R . .
C36 C 0.27008(17) 0.74870(11) -0.0935(3) 0.0230(7) Uani 1 1 d . . .
H36 H 0.3031 0.7731 -0.1098 0.028 Uiso 1 1 calc R . .
C37 C 0.08054(17) 0.50927(11) 0.1711(3) 0.0222(7) Uani 1 1 d . . .
H37A H 0.0376 0.5099 0.0999 0.027 Uiso 1 1 calc R . .
H37B H 0.0636 0.4918 0.2362 0.027 Uiso 1 1 calc R . .
C38 C 0.14804(18) 0.48231(11) 0.1387(3) 0.0235(7) Uani 1 1 d . . .
H38A H 0.1947 0.4889 0.2008 0.028 Uiso 1 1 calc R . .
H38B H 0.1381 0.4474 0.1384 0.028 Uiso 1 1 calc R . .
C39 C 0.22849(18) 0.50685(10) 0.0068(3) 0.0220(7) Uani 1 1 d . . .
H39 H 0.2687 0.5083 0.0763 0.026 Uiso 1 1 calc R . .
C40 C 0.24512(16) 0.51608(10) -0.1138(3) 0.0180(6) Uani 1 1 d . . .
C41 C 0.18506(16) 0.51399(10) -0.2196(3) 0.0201(7) Uani 1 1 d . . .
C42 C 0.20289(17) 0.51845(11) -0.3344(3) 0.0229(7) Uani 1 1 d . . .
H42 H 0.1634 0.5174 -0.4049 0.027 Uiso 1 1 calc R . .
C43 C 0.27862(17) 0.52433(11) -0.3440(3) 0.0223(7) Uani 1 1 d . . .
H43 H 0.2894 0.5267 -0.4218 0.027 Uiso 1 1 calc R . .
C44 C 0.34028(16) 0.52689(10) -0.2405(3) 0.0171(6) Uani 1 1 d . . .
C45 C 0.32100(16) 0.52280(10) -0.1265(3) 0.0197(7) Uani 1 1 d . . .
H45 H 0.3604 0.5246 -0.0560 0.024 Uiso 1 1 calc R . .
C46 C 0.42160(16) 0.53427(10) -0.2529(3) 0.0178(6) Uani 1 1 d . . .
C47 C 0.44158(17) 0.53007(11) -0.3674(3) 0.0225(7) Uani 1 1 d . . .
H47 H 0.4041 0.5201 -0.4352 0.027 Uiso 1 1 calc R . .
C48 C 0.51529(16) 0.54034(11) -0.3817(3) 0.0221(7) Uani 1 1 d . . .
H48 H 0.5261 0.5385 -0.4595 0.026 Uiso 1 1 calc R . .
C49 C 0.57415(16) 0.55346(10) -0.2818(3) 0.0203(7) Uani 1 1 d . . .
C50 C 0.55581(17) 0.55528(10) -0.1666(3) 0.0219(7) Uani 1 1 d . . .
H50 H 0.5944 0.5627 -0.0978 0.026 Uiso 1 1 calc R . .
C51 C 0.48090(16) 0.54614(10) -0.1530(3) 0.0208(7) Uani 1 1 d . . .
H51 H 0.4701 0.5480 -0.0752 0.025 Uiso 1 1 calc R . .
C52 C 0.65150(17) 0.56735(10) -0.2987(3) 0.0216(7) Uani 1 1 d . . .
H52 H 0.6863 0.5813 -0.2328 0.026 Uiso 1 1 calc R . .
C53 C 0.74741(17) 0.58142(11) -0.4076(3) 0.0252(7) Uani 1 1 d . . .
H53A H 0.7788 0.5563 -0.4342 0.030 Uiso 1 1 calc R . .
H53B H 0.7748 0.5931 -0.3276 0.030 Uiso 1 1 calc R . .
C54 C 0.73513(18) 0.62316(11) -0.4987(3) 0.0267(7) Uani 1 1 d . . .
H54A H 0.7844 0.6317 -0.5181 0.032 Uiso 1 1 calc R . .
H54B H 0.7004 0.6126 -0.5741 0.032 Uiso 1 1 calc R . .
C55 C -0.01243(18) 0.40560(12) 0.3663(3) 0.0298(8) Uani 1 1 d . . .
H55 H -0.0421 0.4315 0.3160 0.036 Uiso 1 1 calc R . .
C56 C 0.0384(2) 0.22247(14) 0.1310(4) 0.0474(10) Uani 1 1 d . . .
H56 H 0.0034 0.2061 0.0624 0.057 Uiso 1 1 calc R . .
N1 N 0.10071(14) 0.55927(9) 0.2109(2) 0.0217(6) Uani 1 1 d . . .
N2 N 0.26537(15) 0.59605(9) 0.3296(2) 0.0269(6) Uani 1 1 d . . .
N3 N 0.72451(15) 0.69467(9) -0.1794(2) 0.0299(6) Uani 1 1 d . . .
N4 N 0.70261(14) 0.66634(9) -0.4522(2) 0.0244(6) Uani 1 1 d . . .
N5 N 0.52916(15) 0.69222(10) -0.4914(2) 0.0280(6) Uani 1 1 d . . .
N6 N 0.06588(14) 0.64807(9) 0.0413(2) 0.0254(6) Uani 1 1 d . . .
N7 N 0.16035(14) 0.49686(9) 0.0191(2) 0.0203(6) Uani 1 1 d . . .
N8 N 0.67291(14) 0.56122(9) -0.3984(2) 0.0231(6) Uani 1 1 d . . .
O1 O 0.78618(12) 0.63724(8) -0.0014(2) 0.0384(6) Uani 1 1 d . . .
H1 H 0.7838 0.6549 -0.0615 0.058 Uiso 1 1 calc R . .
O2 O 0.11701(12) 0.73657(8) 0.07331(19) 0.0314(5) Uani 1 1 d . . .
H2 H 0.0906 0.7127 0.0817 0.047 Uiso 1 1 calc R . .
O3 O 0.10993(11) 0.50734(8) -0.21314(18) 0.0261(5) Uani 1 1 d . . .
H3A H 0.1071 0.5053 -0.1409 0.039 Uiso 1 1 calc R . .
Cl1 Cl 0.04813(5) 0.37766(3) 0.28064(8) 0.0387(2) Uani 1 1 d . . .
Cl2 Cl -0.07839(5) 0.36238(3) 0.40098(8) 0.0395(2) Uani 1 1 d . . .
Cl3 Cl 0.04306(6) 0.43226(4) 0.50053(9) 0.0514(3) Uani 1 1 d . . .
Cl4 Cl 0.10414(7) 0.17890(4) 0.20942(18) 0.1022(6) Uani 1 1 d . . .
Cl5 Cl 0.08765(5) 0.26918(4) 0.07086(9) 0.0556(3) Uani 1 1 d . . .
Cl6 Cl -0.01666(6) 0.24589(4) 0.22841(9) 0.0527(3) Uani 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 N1 1.465(4) . ?
C1 C2 1.517(4) . ?
C2 N2 1.455(4) . ?
C3 N2 1.268(4) . ?
C3 C4 1.465(4) . ?
C4 C9 1.393(4) . ?
C4 C5 1.397(4) . ?
C5 C6 1.378(4) . ?
C6 C7 1.402(4) . ?
C7 C8 1.406(4) . ?
C7 C10 1.479(4) . ?
C8 C9 1.374(4) . ?
C10 C11 1.387(4) . ?
C10 C15 1.403(4) . ?
C11 C12 1.399(4) . ?
C12 C13 1.413(4) . ?
C12 C16 1.454(5) . ?
C13 O1 1.348(4) . ?
C13 C14 1.383(5) . ?
C14 C15 1.384(5) . ?
C16 N3 1.274(4) . ?
C17 N3 1.449(4) . ?
C17 C18 1.515(5) . ?
C18 N4 1.464(4) . ?
C19 N4 1.466(4) . ?
C19 C20 1.506(4) . ?
C20 N5 1.468(4) . ?
C21 N5 1.259(4) . ?
C21 C22 1.458(4) . ?
C22 C23 1.391(4) . ?
C22 C27 1.394(4) . ?
C23 C24 1.374(4) . ?
C24 C25 1.393(4) . ?
C25 C26 1.398(4) . ?
C25 C28 1.476(4) . ?
C26 C27 1.375(4) . ?
C28 C29 1.393(4) . ?
C28 C36 1.405(4) . ?
C29 C30 1.386(4) . ?
C30 C31 1.409(4) . ?
C30 C32 1.467(4) . ?
C31 O2 1.345(4) . ?
C31 C34 1.389(4) . ?
C32 N6 1.270(4) . ?
C33 N6 1.458(4) . ?
C33 C35 1.514(4) . ?
C34 C36 1.373(4) . ?
C35 N1 1.471(4) . ?
C37 N1 1.459(4) . ?
C37 C38 1.511(4) . ?
C38 N7 1.453(4) . ?
C39 N7 1.270(4) . ?
C39 C40 1.461(4) . ?
C40 C45 1.389(4) . ?
C40 C41 1.404(4) . ?
C41 O3 1.356(3) . ?
C41 C42 1.388(4) . ?
C42 C43 1.374(4) . ?
C43 C44 1.404(4) . ?
C44 C45 1.391(4) . ?
C44 C46 1.486(4) . ?
C46 C51 1.390(4) . ?
C46 C47 1.402(4) . ?
C47 C48 1.374(4) . ?
C48 C49 1.394(4) . ?
C49 C50 1.393(4) . ?
C49 C52 1.469(4) . ?
C50 C51 1.386(4) . ?
C52 N8 1.262(4) . ?
C53 N8 1.451(4) . ?
C53 C54 1.513(4) . ?
C54 N4 1.458(4) . ?
C55 Cl1 1.757(3) . ?
C55 Cl3 1.758(3) . ?
C55 Cl2 1.761(3) . ?
C56 Cl6 1.731(4) . ?
C56 Cl4 1.758(4) . ?
C56 Cl5 1.759(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 112.1(2) . . ?
N2 C2 C1 110.7(3) . . ?
N2 C3 C4 123.3(3) . . ?
C9 C4 C5 118.0(3) . . ?
C9 C4 C3 122.9(3) . . ?
C5 C4 C3 119.1(3) . . ?
C6 C5 C4 121.1(3) . . ?
C5 C6 C7 121.2(3) . . ?
C6 C7 C8 117.0(3) . . ?
C6 C7 C10 120.8(3) . . ?
C8 C7 C10 122.2(3) . . ?
C9 C8 C7 121.6(3) . . ?
C8 C9 C4 121.0(3) . . ?
C11 C10 C15 116.9(3) . . ?
C11 C10 C7 122.3(3) . . ?
C15 C10 C7 120.9(3) . . ?
C10 C11 C12 122.6(3) . . ?
C11 C12 C13 118.9(3) . . ?
C11 C12 C16 120.3(3) . . ?
C13 C12 C16 120.8(3) . . ?
O1 C13 C14 119.9(3) . . ?
O1 C13 C12 121.0(3) . . ?
C14 C13 C12 119.0(3) . . ?
C13 C14 C15 120.7(3) . . ?
C14 C15 C10 121.8(3) . . ?
N3 C16 C12 121.8(3) . . ?
N3 C17 C18 110.5(3) . . ?
N4 C18 C17 111.3(3) . . ?
N4 C19 C20 113.4(3) . . ?
N5 C20 C19 110.8(3) . . ?
N5 C21 C22 123.7(3) . . ?
C23 C22 C27 117.5(3) . . ?
C23 C22 C21 120.0(3) . . ?
C27 C22 C21 122.5(3) . . ?
C24 C23 C22 121.2(3) . . ?
C23 C24 C25 121.6(3) . . ?
C24 C25 C26 117.2(3) . . ?
C24 C25 C28 121.0(3) . . ?
C26 C25 C28 121.8(3) . . ?
C27 C26 C25 121.2(3) . . ?
C26 C27 C22 121.3(3) . . ?
C29 C28 C36 116.1(3) . . ?
C29 C28 C25 122.4(3) . . ?
C36 C28 C25 121.5(3) . . ?
C30 C29 C28 123.0(3) . . ?
C29 C30 C31 119.1(3) . . ?
C29 C30 C32 120.8(3) . . ?
C31 C30 C32 120.0(3) . . ?
O2 C31 C34 119.0(3) . . ?
O2 C31 C30 122.2(3) . . ?
C34 C31 C30 118.8(3) . . ?
N6 C32 C30 121.8(3) . . ?
N6 C33 C35 110.2(2) . . ?
C36 C34 C31 120.7(3) . . ?
N1 C35 C33 111.8(2) . . ?
C34 C36 C28 122.3(3) . . ?
N1 C37 C38 112.2(2) . . ?
N7 C38 C37 111.7(2) . . ?
N7 C39 C40 121.5(3) . . ?
C45 C40 C41 119.2(3) . . ?
C45 C40 C39 120.6(3) . . ?
C41 C40 C39 120.0(3) . . ?
O3 C41 C42 118.9(3) . . ?
O3 C41 C40 121.8(3) . . ?
C42 C41 C40 119.3(3) . . ?
C43 C42 C41 120.2(3) . . ?
C42 C43 C44 122.3(3) . . ?
C45 C44 C43 116.5(3) . . ?
C45 C44 C46 122.1(3) . . ?
C43 C44 C46 121.4(3) . . ?
C40 C45 C44 122.5(3) . . ?
C51 C46 C47 117.0(3) . . ?
C51 C46 C44 122.0(3) . . ?
C47 C46 C44 121.0(3) . . ?
C48 C47 C46 121.5(3) . . ?
C47 C48 C49 121.3(3) . . ?
C50 C49 C48 117.6(3) . . ?
C50 C49 C52 121.3(3) . . ?
C48 C49 C52 121.0(3) . . ?
C51 C50 C49 121.0(3) . . ?
C50 C51 C46 121.6(3) . . ?
N8 C52 C49 123.0(3) . . ?
N8 C53 C54 109.6(2) . . ?
N4 C54 C53 112.5(2) . . ?
Cl1 C55 Cl3 110.59(17) . . ?
Cl1 C55 Cl2 109.70(18) . . ?
Cl3 C55 Cl2 111.33(17) . . ?
Cl6 C56 Cl4 109.8(2) . . ?
Cl6 C56 Cl5 111.2(2) . . ?
Cl4 C56 Cl5 110.80(19) . . ?
C37 N1 C1 110.2(2) . . ?
C37 N1 C35 111.1(2) . . ?
C1 N1 C35 111.1(2) . . ?
C3 N2 C2 117.1(3) . . ?
C16 N3 C17 119.8(3) . . ?
C54 N4 C18 112.5(2) . . ?
C54 N4 C19 112.2(2) . . ?
C18 N4 C19 110.3(2) . . ?
C21 N5 C20 117.1(3) . . ?
C32 N6 C33 119.2(3) . . ?
C39 N7 C38 119.6(3) . . ?
C52 N8 C53 117.5(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.095
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.064
####################################################################### 
# 
# 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_C3X
_database_code_depnum_ccdc_archive 'CCDC 1042075'
_audit_update_record             
;
2015-01-05 deposited with the CCDC.
2015-01-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H36 N4 O6'
_chemical_formula_sum            'C33 H36 N4 O6'
_chemical_formula_weight         584.66

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

loop_
_symmetry_equiv_pos_as_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                   7.2035(9)
_cell_length_b                   18.776(2)
_cell_length_c                   21.734(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.764(4)
_cell_angle_gamma                90.00
_cell_volume                     2938.1(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9894
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      24.87

_exptl_crystal_description       Block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1240
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_correction_T_min  0.973
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            69381
_diffrn_reflns_av_R_equivalents  0.1367
_diffrn_reflns_av_sigmaI/netI    0.0706
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5167
_reflns_number_gt                3320
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1999)'
_computing_publication_material  WinGX

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1071P)²+14.2932P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5167
_refine_ls_number_parameters     388
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1494
_refine_ls_R_factor_gt           0.0981
_refine_ls_wR_factor_ref         0.2848
_refine_ls_wR_factor_gt          0.2662
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4428(7) 0.5598(3) 0.8799(3) 0.0207(12) Uani 1 1 d . . .
H1A H 0.3229 0.5805 0.8884 0.025 Uiso 1 1 calc R . .
H1B H 0.4354 0.5090 0.8877 0.025 Uiso 1 1 calc R . .
C2 C 0.4846(8) 0.5718(3) 0.8130(3) 0.0242(13) Uani 1 1 d . . .
H2A H 0.6122 0.5585 0.8056 0.029 Uiso 1 1 calc R . .
H2B H 0.4037 0.5423 0.7871 0.029 Uiso 1 1 calc R . .
C3 C 0.4820(7) 0.6755(3) 0.7438(2) 0.0205(12) Uani 1 1 d . . .
H3 H 0.5288 0.6466 0.7133 0.025 Uiso 1 1 calc R . .
C4 C 0.4433(7) 0.7478(3) 0.7296(2) 0.0176(12) Uani 1 1 d . . .
C5 C 0.4743(7) 0.7732(3) 0.6706(2) 0.0194(12) Uani 1 1 d . . .
H5 H 0.5193 0.7422 0.6412 0.023 Uiso 1 1 calc R . .
C6 C 0.4400(7) 0.8431(3) 0.6546(2) 0.0205(12) Uani 1 1 d . . .
C7 C 0.3724(8) 0.8897(3) 0.7001(2) 0.0237(13) Uani 1 1 d . . .
H7 H 0.3530 0.9372 0.6899 0.028 Uiso 1 1 calc R . .
C8 C 0.3345(8) 0.8678(3) 0.7582(3) 0.0232(13) Uani 1 1 d . . .
C9 C 0.3700(8) 0.7941(3) 0.7753(3) 0.0243(13) Uani 1 1 d . . .
C10 C 0.2499(9) 0.9159(3) 0.8037(3) 0.0298(14) Uani 1 1 d . . .
H10A H 0.2344 0.8907 0.8416 0.045 Uiso 1 1 calc R . .
H10B H 0.1310 0.9318 0.7880 0.045 Uiso 1 1 calc R . .
H10C H 0.3294 0.9563 0.8109 0.045 Uiso 1 1 calc R . .
C11 C 0.4718(8) 0.8689(3) 0.5926(2) 0.0252(13) Uani 1 1 d . . .
H11 H 0.5241 0.8371 0.5653 0.030 Uiso 1 1 calc R . .
C12 C 0.7557(7) 0.5480(3) 0.9270(3) 0.0218(12) Uani 1 1 d . . .
H12A H 0.7562 0.5139 0.8935 0.026 Uiso 1 1 calc R . .
H12B H 0.7566 0.5217 0.9654 0.026 Uiso 1 1 calc R . .
C13 C 0.9276(8) 0.5936(3) 0.9250(2) 0.0217(12) Uani 1 1 d . . .
H13A H 0.9122 0.6357 0.9502 0.026 Uiso 1 1 calc R . .
H13B H 1.0338 0.5672 0.9413 0.026 Uiso 1 1 calc R . .
C14 C 0.9266(7) 0.6782(3) 0.8426(2) 0.0182(12) Uani 1 1 d . . .
H14 H 0.8893 0.7125 0.8706 0.022 Uiso 1 1 calc R . .
C15 C 0.9461(7) 0.6978(3) 0.7786(2) 0.0204(12) Uani 1 1 d . . .
C16 C 1.0042(7) 0.6466(3) 0.7351(3) 0.0221(13) Uani 1 1 d . . .
C17 C 1.0278(7) 0.6664(3) 0.6733(2) 0.0223(13) Uani 1 1 d . . .
C18 C 0.9948(7) 0.7365(3) 0.6568(3) 0.0225(13) Uani 1 1 d . . .
H18 H 1.0124 0.7503 0.6163 0.027 Uiso 1 1 calc R . .
C19 C 0.9358(7) 0.7878(3) 0.6991(3) 0.0254(13) Uani 1 1 d . . .
C20 C 0.9125(8) 0.7682(3) 0.7597(3) 0.0234(13) Uani 1 1 d . . .
H20 H 0.8745 0.8018 0.7880 0.028 Uiso 1 1 calc R . .
C21 C 1.0985(8) 0.6127(3) 0.6287(3) 0.0297(14) Uani 1 1 d . . .
H21A H 1.1124 0.5674 0.6489 0.045 Uiso 1 1 calc R . .
H21B H 1.2166 0.6280 0.6142 0.045 Uiso 1 1 calc R . .
H21C H 1.0119 0.6083 0.5944 0.045 Uiso 1 1 calc R . .
C22 C 0.9019(9) 0.8615(3) 0.6807(3) 0.0316(15) Uani 1 1 d . . .
H22 H 0.8645 0.8934 0.7107 0.038 Uiso 1 1 calc R . .
C23 C 0.5098(8) 0.6063(3) 0.9823(2) 0.0237(13) Uani 1 1 d . . .
H23A H 0.6082 0.6016 1.0135 0.028 Uiso 1 1 calc R . .
H23B H 0.4154 0.5711 0.9909 0.028 Uiso 1 1 calc R . .
C24 C 0.4253(8) 0.6803(3) 0.9866(3) 0.0255(13) Uani 1 1 d . . .
H24A H 0.3377 0.6878 0.9524 0.031 Uiso 1 1 calc R . .
H24B H 0.3589 0.6847 1.0246 0.031 Uiso 1 1 calc R . .
C25 C 0.5711(8) 0.7863(3) 0.9454(3) 0.0237(13) Uani 1 1 d . . .
H25 H 0.4691 0.7911 0.9184 0.028 Uiso 1 1 calc R . .
C26 C 0.7175(8) 0.8356(3) 0.9420(3) 0.0222(13) Uani 1 1 d . . .
C27 C 0.8758(8) 0.8315(3) 0.9829(3) 0.0256(13) Uani 1 1 d . . .
C28 C 1.0169(9) 0.8859(3) 0.9776(3) 0.0278(14) Uani 1 1 d . . .
C29 C 0.9943(9) 0.9378(3) 0.9350(3) 0.0303(14) Uani 1 1 d . . .
H29 H 1.0843 0.9732 0.9333 0.036 Uiso 1 1 calc R . .
C30 C 0.8378(8) 0.9411(3) 0.8921(3) 0.0269(14) Uani 1 1 d . . .
C31 C 0.7019(8) 0.8896(3) 0.8969(3) 0.0278(14) Uani 1 1 d . . .
H31 H 0.5989 0.8906 0.8700 0.033 Uiso 1 1 calc R . .
C32 C 1.1835(9) 0.8813(4) 1.0211(3) 0.0436(17) Uani 1 1 d . . .
H32A H 1.1720 0.8403 1.0471 0.065 Uiso 1 1 calc R . .
H32B H 1.1903 0.9235 1.0460 0.065 Uiso 1 1 calc R . .
H32C H 1.2942 0.8772 0.9979 0.065 Uiso 1 1 calc R . .
C33 C 0.8188(9) 0.9950(3) 0.8452(3) 0.0347(15) Uani 1 1 d . . .
H33 H 0.7145 0.9927 0.8190 0.042 Uiso 1 1 calc R . .
N1 N 0.5856(6) 0.5915(2) 0.9218(2) 0.0189(10) Uani 1 1 d . . .
N2 N 0.4551(6) 0.6480(2) 0.7976(2) 0.0206(10) Uani 1 1 d . . .
N3 N 0.9598(6) 0.6145(2) 0.8616(2) 0.0196(10) Uani 1 1 d . . .
N4 N 0.5733(7) 0.7342(2) 0.9851(2) 0.0253(11) Uani 1 1 d . . .
O1 O 0.3358(5) 0.7722(2) 0.82945(17) 0.0279(10) Uani 1 1 d . . .
H1 H 0.3619 0.7298 0.8323 0.042 Uiso 1 1 calc R . .
O2 O 0.4365(6) 0.9278(2) 0.57347(18) 0.0348(11) Uani 1 1 d . . .
O3 O 1.0373(5) 0.57961(19) 0.75174(17) 0.0243(9) Uani 1 1 d . . .
H3O H 1.0184 0.5749 0.7885 0.036 Uiso 1 1 calc R . .
O4 O 0.9192(7) 0.8838(3) 0.6290(2) 0.0470(13) Uani 1 1 d . . .
O5 O 0.8947(6) 0.7823(2) 1.02283(18) 0.0298(10) Uani 1 1 d . . .
H5A H 0.8047 0.7556 1.0205 0.045 Uiso 1 1 calc R . .
O6 O 0.9273(7) 1.0433(2) 0.8371(2) 0.0478(13) Uani 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 N1 1.478(7) . ?
C1 C2 1.510(8) . ?
C2 N2 1.484(7) . ?
C3 N2 1.298(7) . ?
C3 C4 1.417(7) . ?
C4 C5 1.393(7) . ?
C4 C9 1.433(8) . ?
C5 C6 1.379(8) . ?
C6 C7 1.417(8) . ?
C6 C11 1.457(8) . ?
C7 C8 1.362(8) . ?
C8 C9 1.454(8) . ?
C8 C10 1.484(8) . ?
C9 O1 1.277(7) . ?
C11 O2 1.205(7) . ?
C12 N1 1.474(7) . ?
C12 C13 1.507(8) . ?
C13 N3 1.457(7) . ?
C14 N3 1.285(7) . ?
C14 C15 1.451(7) . ?
C15 C20 1.403(8) . ?
C15 C16 1.419(8) . ?
C16 O3 1.328(6) . ?
C16 C17 1.411(8) . ?
C17 C18 1.383(8) . ?
C17 C21 1.498(8) . ?
C18 C19 1.406(8) . ?
C19 C20 1.381(8) . ?
C19 C22 1.460(8) . ?
C22 O4 1.210(7) . ?
C23 N1 1.465(7) . ?
C23 C24 1.521(8) . ?
C24 N4 1.470(7) . ?
C25 N4 1.305(7) . ?
C25 C26 1.406(8) . ?
C26 C31 1.414(8) . ?
C26 C27 1.426(8) . ?
C27 O5 1.272(7) . ?
C27 C28 1.447(8) . ?
C28 C29 1.351(8) . ?
C28 C32 1.506(9) . ?
C29 C30 1.442(9) . ?
C30 C31 1.382(8) . ?
C30 C33 1.440(8) . ?
C33 O6 1.213(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
N1 C1 C2 112.3(4) . . ?
N2 C2 C1 109.2(4) . . ?
N2 C3 C4 122.9(5) . . ?
C5 C4 C3 119.5(5) . . ?
C5 C4 C9 120.2(5) . . ?
C3 C4 C9 120.2(5) . . ?
C6 C5 C4 121.7(5) . . ?
C5 C6 C7 118.3(5) . . ?
C5 C6 C11 121.1(5) . . ?
C7 C6 C11 120.5(5) . . ?
C8 C7 C6 122.9(5) . . ?
C7 C8 C9 119.0(5) . . ?
C7 C8 C10 122.2(5) . . ?
C9 C8 C10 118.8(5) . . ?
O1 C9 C4 121.9(5) . . ?
O1 C9 C8 120.3(5) . . ?
C4 C9 C8 117.8(5) . . ?
O2 C11 C6 125.9(6) . . ?
N1 C12 C13 111.4(4) . . ?
N3 C13 C12 109.6(4) . . ?
N3 C14 C15 121.4(5) . . ?
C20 C15 C16 119.7(5) . . ?
C20 C15 C14 120.0(5) . . ?
C16 C15 C14 120.4(5) . . ?
O3 C16 C17 118.9(5) . . ?
O3 C16 C15 121.0(5) . . ?
C17 C16 C15 120.1(5) . . ?
C18 C17 C16 118.2(5) . . ?
C18 C17 C21 122.2(5) . . ?
C16 C17 C21 119.5(5) . . ?
C17 C18 C19 122.3(5) . . ?
C20 C19 C18 119.3(5) . . ?
C20 C19 C22 119.3(6) . . ?
C18 C19 C22 121.4(5) . . ?
C19 C20 C15 120.3(5) . . ?
O4 C22 C19 124.2(6) . . ?
N1 C23 C24 112.9(4) . . ?
N4 C24 C23 109.6(5) . . ?
N4 C25 C26 122.3(5) . . ?
C25 C26 C31 117.7(5) . . ?
C25 C26 C27 121.3(5) . . ?
C31 C26 C27 121.0(5) . . ?
O5 C27 C26 122.0(5) . . ?
O5 C27 C28 120.4(5) . . ?
C26 C27 C28 117.6(5) . . ?
C29 C28 C27 119.6(6) . . ?
C29 C28 C32 123.2(6) . . ?
C27 C28 C32 117.3(5) . . ?
C28 C29 C30 123.3(6) . . ?
C31 C30 C33 119.5(6) . . ?
C31 C30 C29 117.6(5) . . ?
C33 C30 C29 122.9(6) . . ?
C30 C31 C26 120.8(6) . . ?
O6 C33 C30 125.5(6) . . ?
C23 N1 C12 111.6(4) . . ?
C23 N1 C1 111.0(4) . . ?
C12 N1 C1 112.7(4) . . ?
C3 N2 C2 124.2(5) . . ?
C14 N3 C13 121.4(5) . . ?
C25 N4 C24 122.5(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
N1 C1 C2 N2 -71.2(6) . . . . ?
N2 C3 C4 C5 -179.4(5) . . . . ?
N2 C3 C4 C9 -0.4(8) . . . . ?
C3 C4 C5 C6 -179.6(5) . . . . ?
C9 C4 C5 C6 1.4(8) . . . . ?
C4 C5 C6 C7 0.3(8) . . . . ?
C4 C5 C6 C11 -179.6(5) . . . . ?
C5 C6 C7 C8 -2.1(8) . . . . ?
C11 C6 C7 C8 177.8(5) . . . . ?
C6 C7 C8 C9 1.9(8) . . . . ?
C6 C7 C8 C10 -175.1(5) . . . . ?
C5 C4 C9 O1 178.4(5) . . . . ?
C3 C4 C9 O1 -0.6(8) . . . . ?
C5 C4 C9 C8 -1.5(8) . . . . ?
C3 C4 C9 C8 179.5(5) . . . . ?
C7 C8 C9 O1 180.0(5) . . . . ?
C10 C8 C9 O1 -2.9(8) . . . . ?
C7 C8 C9 C4 -0.1(8) . . . . ?
C10 C8 C9 C4 177.0(5) . . . . ?
C5 C6 C11 O2 175.7(6) . . . . ?
C7 C6 C11 O2 -4.2(9) . . . . ?
N1 C12 C13 N3 -77.6(6) . . . . ?
N3 C14 C15 C20 -178.6(5) . . . . ?
N3 C14 C15 C16 -0.5(8) . . . . ?
C20 C15 C16 O3 179.9(5) . . . . ?
C14 C15 C16 O3 1.7(8) . . . . ?
C20 C15 C16 C17 -0.1(8) . . . . ?
C14 C15 C16 C17 -178.3(5) . . . . ?
O3 C16 C17 C18 -179.3(5) . . . . ?
C15 C16 C17 C18 0.7(8) . . . . ?
O3 C16 C17 C21 -3.1(8) . . . . ?
C15 C16 C17 C21 176.9(5) . . . . ?
C16 C17 C18 C19 -1.2(8) . . . . ?
C21 C17 C18 C19 -177.3(5) . . . . ?
C17 C18 C19 C20 1.1(8) . . . . ?
C17 C18 C19 C22 -180.0(5) . . . . ?
C18 C19 C20 C15 -0.5(8) . . . . ?
C22 C19 C20 C15 -179.4(5) . . . . ?
C16 C15 C20 C19 0.0(8) . . . . ?
C14 C15 C20 C19 178.2(5) . . . . ?
C20 C19 C22 O4 179.7(6) . . . . ?
C18 C19 C22 O4 0.8(9) . . . . ?
N1 C23 C24 N4 -69.1(6) . . . . ?
N4 C25 C26 C31 179.3(5) . . . . ?
N4 C25 C26 C27 -1.0(8) . . . . ?
C25 C26 C27 O5 2.1(8) . . . . ?
C31 C26 C27 O5 -178.2(5) . . . . ?
C25 C26 C27 C28 -177.9(5) . . . . ?
C31 C26 C27 C28 1.8(8) . . . . ?
O5 C27 C28 C29 -179.8(5) . . . . ?
C26 C27 C28 C29 0.1(8) . . . . ?
O5 C27 C28 C32 -0.1(8) . . . . ?
C26 C27 C28 C32 179.8(5) . . . . ?
C27 C28 C29 C30 -2.2(9) . . . . ?
C32 C28 C29 C30 178.1(6) . . . . ?
C28 C29 C30 C31 2.4(9) . . . . ?
C28 C29 C30 C33 -177.4(6) . . . . ?
C33 C30 C31 C26 179.4(5) . . . . ?
C29 C30 C31 C26 -0.4(8) . . . . ?
C25 C26 C31 C30 178.1(5) . . . . ?
C27 C26 C31 C30 -1.6(8) . . . . ?
C31 C30 C33 O6 179.0(6) . . . . ?
C29 C30 C33 O6 -1.2(10) . . . . ?
C24 C23 N1 C12 143.8(5) . . . . ?
C24 C23 N1 C1 -89.6(5) . . . . ?
C13 C12 N1 C23 -97.5(5) . . . . ?
C13 C12 N1 C1 136.8(5) . . . . ?
C2 C1 N1 C23 156.1(4) . . . . ?
C2 C1 N1 C12 -77.8(5) . . . . ?
C4 C3 N2 C2 176.6(5) . . . . ?
C1 C2 N2 C3 178.9(5) . . . . ?
C15 C14 N3 C13 -175.6(5) . . . . ?
C12 C13 N3 C14 105.8(6) . . . . ?
C26 C25 N4 C24 -176.7(5) . . . . ?
C23 C24 N4 C25 125.6(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.096
