# Electronic Supplementary Material (ESI) for RSC Advances.
# 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_Complex5
_database_code_depnum_ccdc_archive 'CCDC 944133'
_audit_update_record             
;
2015-02-12 deposited with the CCDC.
2015-05-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C90 H132 N14 O12'
_chemical_formula_weight         1602.10

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           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

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

_cell_length_a                   11.7363(15)
_cell_length_b                   13.918(4)
_cell_length_c                   15.892(2)
_cell_angle_alpha                109.483(4)
_cell_angle_beta                 110.352(3)
_cell_angle_gamma                92.310(4)
_cell_volume                     2258.3(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    2768
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      21.59

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             866
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9922
_exptl_absorpt_correction_T_max  0.9937
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15518
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_UnetI/netI     0.0601
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.47
_diffrn_reflns_theta_max         21.64
_reflns_number_total             5271
_reflns_number_gt                3773
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep 3v.2'
_computing_publication_material  'mercury 3.1'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0780P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    CONSTR
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5271
_refine_ls_number_parameters     530
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0491
_refine_ls_wR_factor_ref         0.1375
_refine_ls_wR_factor_gt          0.1223
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_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
O1 O 0.74754(16) 0.54053(15) 1.08297(14) 0.0366(5) Uani 1 1 d . . .
C2 C 0.6869(3) 0.4680(3) 1.0029(2) 0.0356(7) Uani 1 1 d . . .
O3 O 0.69305(17) 0.37432(16) 0.98426(14) 0.0448(6) Uani 1 1 d . . .
C4 C 0.5989(3) 0.4984(3) 0.9238(2) 0.0662(11) Uani 1 1 d . . .
H4A H 0.6423 0.5147 0.8876 0.099 Uiso 1 1 calc R . .
H4B H 0.5673 0.5580 0.9524 0.099 Uiso 1 1 calc R . .
H4C H 0.5317 0.4419 0.8814 0.099 Uiso 1 1 calc R . .
C5 C -0.0246(2) 0.5015(2) 0.90729(19) 0.0283(7) Uani 1 1 d . . .
C6 C -0.0560(2) 0.5019(2) 0.80666(19) 0.0301(7) Uani 1 1 d . . .
H6A H -0.1278 0.4491 0.7619 0.036 Uiso 1 1 calc R . .
H6B H -0.0770 0.5684 0.8060 0.036 Uiso 1 1 calc R . .
N7 N 0.04645(19) 0.48266(17) 0.77411(16) 0.0328(6) Uani 1 1 d . . .
H7 H 0.1175 0.4801 0.8132 0.039 Uiso 1 1 calc R . .
C8 C 0.0277(3) 0.4692(2) 0.6830(2) 0.0335(7) Uani 1 1 d . . .
O9 O -0.07388(18) 0.47090(17) 0.62467(15) 0.0493(6) Uani 1 1 d . . .
C10 C 0.1350(2) 0.4516(2) 0.6510(2) 0.0307(7) Uani 1 1 d . . .
C11 C 0.1120(3) 0.4270(2) 0.5545(2) 0.0390(8) Uani 1 1 d . . .
H11 H 0.0321 0.4199 0.5109 0.047 Uiso 1 1 calc R . .
C12 C 0.2083(3) 0.4128(2) 0.5227(2) 0.0426(8) Uani 1 1 d . . .
H12 H 0.1907 0.3967 0.4573 0.051 Uiso 1 1 calc R . .
N13 N 0.3248(2) 0.4212(2) 0.58096(19) 0.0453(7) Uani 1 1 d . . .
C14 C 0.3459(3) 0.4463(2) 0.6741(2) 0.0454(8) Uani 1 1 d . . .
H14 H 0.4268 0.4540 0.7164 0.054 Uiso 1 1 calc R . .
C15 C 0.2560(3) 0.4618(2) 0.7125(2) 0.0392(8) Uani 1 1 d . . .
H15 H 0.2763 0.4786 0.7784 0.047 Uiso 1 1 calc R . .
C16 C 0.0000(2) 0.5950(2) 0.9866(2) 0.0274(7) Uani 1 1 d . . .
C17 C 0.0049(3) 0.6969(2) 0.9715(2) 0.0347(7) Uani 1 1 d . . .
H17A H -0.0746 0.6986 0.9257 0.042 Uiso 1 1 calc R . .
H17B H 0.0217 0.7537 1.0323 0.042 Uiso 1 1 calc R . .
N18 N 0.1010(2) 0.71005(17) 0.93522(16) 0.0328(6) Uani 1 1 d . . .
H18 H 0.1727 0.6966 0.9617 0.039 Uiso 1 1 calc R . .
C19 C 0.0796(3) 0.7424(2) 0.8621(2) 0.0326(7) Uani 1 1 d . . .
O20 O -0.01734(19) 0.76991(15) 0.82378(14) 0.0438(5) Uani 1 1 d . . .
C21 C 0.1802(3) 0.7411(2) 0.8233(2) 0.0383(8) Uani 1 1 d . . .
C22 C 0.1473(4) 0.7230(3) 0.7270(3) 0.0604(10) Uani 1 1 d . . .
H22 H 0.0647 0.7128 0.6871 0.072 Uiso 1 1 calc R . .
C23 C 0.2377(5) 0.7201(3) 0.6899(3) 0.0843(14) Uani 1 1 d . . .
H23 H 0.2132 0.7054 0.6239 0.101 Uiso 1 1 calc R . .
N24 N 0.3570(4) 0.7368(3) 0.7423(4) 0.0852(12) Uani 1 1 d . . .
C25 C 0.3886(4) 0.7542(3) 0.8355(4) 0.0775(13) Uani 1 1 d . . .
H25 H 0.4722 0.7653 0.8737 0.093 Uiso 1 1 calc R . .
C26 C 0.3036(3) 0.7567(3) 0.8799(3) 0.0552(10) Uani 1 1 d . . .
H26 H 0.3299 0.7686 0.9454 0.066 Uiso 1 1 calc R . .
C27 C 0.0232(2) 0.5927(2) 1.0786(2) 0.0283(7) Uani 1 1 d . . .
C28 C 0.0393(2) 0.6927(2) 1.1623(2) 0.0310(7) Uani 1 1 d . . .
H28A H 0.0755 0.6824 1.2229 0.037 Uiso 1 1 calc R . .
H28B H 0.0951 0.7465 1.1628 0.037 Uiso 1 1 calc R . .
N29 N -0.07979(19) 0.72543(17) 1.15339(16) 0.0316(6) Uani 1 1 d . . .
H29 H -0.1467 0.6807 1.1181 0.038 Uiso 1 1 calc R . .
C30 C -0.0864(3) 0.8233(2) 1.1990(2) 0.0320(7) Uani 1 1 d . . .
O31 O 0.00669(18) 0.89090(15) 1.24838(15) 0.0456(6) Uani 1 1 d . . .
C32 C -0.2123(2) 0.8505(2) 1.18575(19) 0.0307(7) Uani 1 1 d . . .
C33 C -0.2232(3) 0.9540(2) 1.2160(2) 0.0423(8) Uani 1 1 d . . .
H33 H -0.1534 1.0054 1.2453 0.051 Uiso 1 1 calc R . .
C34 C -0.3384(3) 0.9798(3) 1.2024(3) 0.0538(9) Uani 1 1 d . . .
H34 H -0.3437 1.0498 1.2221 0.065 Uiso 1 1 calc R . .
N35 N -0.4434(2) 0.9114(2) 1.1629(2) 0.0509(7) Uani 1 1 d . . .
C36 C -0.4318(3) 0.8117(3) 1.1352(2) 0.0454(8) Uani 1 1 d . . .
H36 H -0.5030 0.7620 1.1076 0.054 Uiso 1 1 calc R . .
C37 C -0.3203(3) 0.7781(2) 1.1450(2) 0.0389(8) Uani 1 1 d . . .
H37 H -0.3176 0.7076 1.1246 0.047 Uiso 1 1 calc R . .
O38 O 0.6683(2) 0.0870(2) 0.4877(2) 0.0910(9) Uani 1 1 d . . .
C39 C 0.7378(3) 0.1663(3) 0.5075(3) 0.0588(10) Uani 1 1 d . . .
C40 C 0.6947(3) 0.2664(3) 0.5208(3) 0.0656(10) Uani 1 1 d . . .
H40A H 0.6698 0.2778 0.4610 0.098 Uiso 1 1 calc R . .
H40B H 0.7605 0.3212 0.5698 0.098 Uiso 1 1 calc R . .
H40C H 0.6259 0.2655 0.5401 0.098 Uiso 1 1 calc R . .
C41 C 0.8689(3) 0.1633(3) 0.5236(3) 0.0889(14) Uani 1 1 d . . .
H41A H 0.9151 0.1756 0.5904 0.133 Uiso 1 1 calc R . .
H41B H 0.9005 0.2158 0.5067 0.133 Uiso 1 1 calc R . .
H41C H 0.8765 0.0966 0.4841 0.133 Uiso 1 1 calc R . .
N42 N 0.30499(19) 0.09826(17) 0.29070(16) 0.0307(6) Uani 1 1 d . . .
C43 C 0.2316(2) 0.0630(2) 0.18285(19) 0.0329(7) Uani 1 1 d . . .
H43A H 0.1815 -0.0043 0.1614 0.039 Uiso 1 1 calc R . .
H43B H 0.1758 0.1109 0.1715 0.039 Uiso 1 1 calc R . .
C44 C 0.3069(3) 0.0548(2) 0.1215(2) 0.0399(8) Uani 1 1 d . . .
H44A H 0.3686 0.0122 0.1364 0.048 Uiso 1 1 calc R . .
H44B H 0.3494 0.1232 0.1362 0.048 Uiso 1 1 calc R . .
C45 C 0.2239(3) 0.0072(2) 0.0141(2) 0.0463(8) Uani 1 1 d . . .
H45A H 0.2755 -0.0034 -0.0233 0.056 Uiso 1 1 calc R . .
H45B H 0.1801 -0.0601 0.0008 0.056 Uiso 1 1 calc R . .
C46 C 0.1311(3) 0.0715(3) -0.0193(2) 0.0556(9) Uani 1 1 d . . .
H46A H 0.0778 0.0807 0.0159 0.083 Uiso 1 1 calc R . .
H46B H 0.0829 0.0369 -0.0871 0.083 Uiso 1 1 calc R . .
H46C H 0.1735 0.1378 -0.0079 0.083 Uiso 1 1 calc R . .
C47 C 0.3912(2) 0.0249(2) 0.3147(2) 0.0345(7) Uani 1 1 d . . .
H47A H 0.4326 0.0494 0.3845 0.041 Uiso 1 1 calc R . .
H47B H 0.4539 0.0292 0.2888 0.041 Uiso 1 1 calc R . .
C48 C 0.3342(3) -0.0884(2) 0.2785(2) 0.0375(8) Uani 1 1 d . . .
H48A H 0.3042 -0.1180 0.2086 0.045 Uiso 1 1 calc R . .
H48B H 0.2647 -0.0944 0.2973 0.045 Uiso 1 1 calc R . .
C49 C 0.4306(3) -0.1471(2) 0.3214(2) 0.0418(8) Uani 1 1 d . . .
H49A H 0.5050 -0.1313 0.3113 0.050 Uiso 1 1 calc R . .
H49B H 0.4513 -0.1234 0.3905 0.050 Uiso 1 1 calc R . .
C50 C 0.3869(3) -0.2634(2) 0.2772(2) 0.0538(9) Uani 1 1 d . . .
H50A H 0.3154 -0.2798 0.2895 0.081 Uiso 1 1 calc R . .
H50B H 0.4515 -0.2967 0.3054 0.081 Uiso 1 1 calc R . .
H50C H 0.3660 -0.2873 0.2087 0.081 Uiso 1 1 calc R . .
C51 C 0.3858(2) 0.2034(2) 0.3293(2) 0.0330(7) Uani 1 1 d . . .
H51A H 0.4251 0.2252 0.3990 0.040 Uiso 1 1 calc R . .
H51B H 0.4507 0.1951 0.3042 0.040 Uiso 1 1 calc R . .
C52 C 0.3235(2) 0.2902(2) 0.3067(2) 0.0355(7) Uani 1 1 d . . .
H52A H 0.2524 0.2954 0.3246 0.043 Uiso 1 1 calc R . .
H52B H 0.2954 0.2758 0.2379 0.043 Uiso 1 1 calc R . .
C53 C 0.4158(3) 0.3916(2) 0.3631(2) 0.0378(8) Uani 1 1 d . . .
H53A H 0.4409 0.4064 0.4317 0.045 Uiso 1 1 calc R . .
H53B H 0.4886 0.3840 0.3475 0.045 Uiso 1 1 calc R . .
C54 C 0.3626(3) 0.4819(2) 0.3408(2) 0.0445(8) Uani 1 1 d . . .
H54A H 0.3407 0.4689 0.2733 0.067 Uiso 1 1 calc R . .
H54B H 0.4231 0.5441 0.3787 0.067 Uiso 1 1 calc R . .
H54C H 0.2905 0.4898 0.3561 0.067 Uiso 1 1 calc R . .
C55 C 0.2099(2) 0.1032(2) 0.3367(2) 0.0325(7) Uani 1 1 d . . .
H55A H 0.1598 0.1537 0.3221 0.039 Uiso 1 1 calc R . .
H55B H 0.1557 0.0363 0.3061 0.039 Uiso 1 1 calc R . .
C56 C 0.2602(3) 0.1307(2) 0.4452(2) 0.0395(8) Uani 1 1 d . . .
H56A H 0.3104 0.0809 0.4614 0.047 Uiso 1 1 calc R . .
H56B H 0.3120 0.1986 0.4774 0.047 Uiso 1 1 calc R . .
C57 C 0.1550(3) 0.1305(2) 0.4797(2) 0.0411(8) Uani 1 1 d . . .
H57A H 0.1068 0.1820 0.4651 0.049 Uiso 1 1 calc R . .
H57B H 0.1014 0.0633 0.4449 0.049 Uiso 1 1 calc R . .
C58 C 0.2002(3) 0.1533(3) 0.5872(2) 0.0586(10) Uani 1 1 d . . .
H58A H 0.2478 0.1024 0.6020 0.088 Uiso 1 1 calc R . .
H58B H 0.1307 0.1513 0.6056 0.088 Uiso 1 1 calc R . .
H58C H 0.2509 0.2208 0.6221 0.088 Uiso 1 1 calc R . .


_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
O1 C2 1.265(3) . ?
C2 O3 1.248(3) . ?
C2 C4 1.522(4) . ?
C5 C27 1.402(4) 2_567 ?
C5 C16 1.410(4) . ?
C5 C6 1.513(4) . ?
C6 N7 1.467(3) . ?
N7 C8 1.333(3) . ?
C8 O9 1.237(3) . ?
C8 C10 1.513(4) . ?
C10 C11 1.376(4) . ?
C10 C15 1.384(4) . ?
C11 C12 1.386(4) . ?
C12 N13 1.332(4) . ?
N13 C14 1.329(4) . ?
C14 C15 1.383(4) . ?
C16 C27 1.403(4) . ?
C16 C17 1.518(4) . ?
C17 N18 1.465(3) . ?
N18 C19 1.331(3) . ?
C19 O20 1.233(3) . ?
C19 C21 1.509(4) . ?
C21 C22 1.371(4) . ?
C21 C26 1.375(4) . ?
C22 C23 1.378(5) . ?
C23 N24 1.320(5) . ?
N24 C25 1.328(5) . ?
C25 C26 1.403(5) . ?
C27 C5 1.402(4) 2_567 ?
C27 C28 1.521(4) . ?
C28 N29 1.462(3) . ?
N29 C30 1.332(3) . ?
C30 O31 1.234(3) . ?
C30 C32 1.501(4) . ?
C32 C33 1.385(4) . ?
C32 C37 1.391(4) . ?
C33 C34 1.376(4) . ?
C34 N35 1.337(4) . ?
N35 C36 1.337(4) . ?
C36 C37 1.383(4) . ?
O38 C39 1.224(4) . ?
C39 C41 1.474(5) . ?
C39 C40 1.476(5) . ?
N42 C47 1.512(3) . ?
N42 C43 1.516(3) . ?
N42 C51 1.518(3) . ?
N42 C55 1.525(3) . ?
C43 C44 1.510(4) . ?
C44 C45 1.529(4) . ?
C45 C46 1.503(4) . ?
C47 C48 1.519(4) . ?
C48 C49 1.523(4) . ?
C49 C50 1.517(4) . ?
C51 C52 1.516(4) . ?
C52 C53 1.525(4) . ?
C53 C54 1.517(4) . ?
C55 C56 1.517(4) . ?
C56 C57 1.516(4) . ?
C57 C58 1.515(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
O3 C2 O1 125.4(3) . . ?
O3 C2 C4 117.9(3) . . ?
O1 C2 C4 116.7(3) . . ?
C27 C5 C16 119.7(2) 2_567 . ?
C27 C5 C6 119.8(2) 2_567 . ?
C16 C5 C6 120.5(2) . . ?
N7 C6 C5 112.2(2) . . ?
C8 N7 C6 118.9(2) . . ?
O9 C8 N7 122.0(3) . . ?
O9 C8 C10 119.7(3) . . ?
N7 C8 C10 118.3(2) . . ?
C11 C10 C15 117.4(3) . . ?
C11 C10 C8 118.0(2) . . ?
C15 C10 C8 124.6(3) . . ?
C10 C11 C12 119.8(3) . . ?
N13 C12 C11 123.4(3) . . ?
C14 N13 C12 116.1(2) . . ?
N13 C14 C15 124.6(3) . . ?
C14 C15 C10 118.7(3) . . ?
C27 C16 C5 119.6(2) . . ?
C27 C16 C17 121.0(2) . . ?
C5 C16 C17 119.3(2) . . ?
N18 C17 C16 110.8(2) . . ?
C19 N18 C17 121.3(2) . . ?
O20 C19 N18 124.0(3) . . ?
O20 C19 C21 119.4(3) . . ?
N18 C19 C21 116.6(3) . . ?
C22 C21 C26 118.3(3) . . ?
C22 C21 C19 118.6(3) . . ?
C26 C21 C19 123.2(3) . . ?
C21 C22 C23 119.5(4) . . ?
N24 C23 C22 123.9(4) . . ?
C23 N24 C25 116.5(3) . . ?
N24 C25 C26 124.0(4) . . ?
C21 C26 C25 117.9(4) . . ?
C5 C27 C16 120.6(2) 2_567 . ?
C5 C27 C28 119.8(2) 2_567 . ?
C16 C27 C28 119.5(2) . . ?
N29 C28 C27 110.4(2) . . ?
C30 N29 C28 121.1(2) . . ?
O31 C30 N29 122.0(3) . . ?
O31 C30 C32 120.2(3) . . ?
N29 C30 C32 117.7(3) . . ?
C33 C32 C37 117.1(3) . . ?
C33 C32 C30 118.8(3) . . ?
C37 C32 C30 124.2(3) . . ?
C34 C33 C32 119.3(3) . . ?
N35 C34 C33 124.6(3) . . ?
C36 N35 C34 115.7(3) . . ?
N35 C36 C37 123.9(3) . . ?
C36 C37 C32 119.4(3) . . ?
O38 C39 C41 119.6(4) . . ?
O38 C39 C40 121.4(3) . . ?
C41 C39 C40 118.9(3) . . ?
C47 N42 C43 111.6(2) . . ?
C47 N42 C51 106.22(19) . . ?
C43 N42 C51 111.2(2) . . ?
C47 N42 C55 111.3(2) . . ?
C43 N42 C55 105.85(19) . . ?
C51 N42 C55 110.8(2) . . ?
C44 C43 N42 115.6(2) . . ?
C43 C44 C45 110.6(2) . . ?
C46 C45 C44 114.3(3) . . ?
N42 C47 C48 117.1(2) . . ?
C47 C48 C49 109.6(2) . . ?
C50 C49 C48 112.8(2) . . ?
C52 C51 N42 117.2(2) . . ?
C51 C52 C53 109.0(2) . . ?
C54 C53 C52 112.4(2) . . ?
C56 C55 N42 116.4(2) . . ?
C57 C56 C55 110.2(2) . . ?
C58 C57 C56 112.3(2) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        21.64
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.045
####################################################################### 
# 
# 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_Complex2
_database_code_depnum_ccdc_archive 'CCDC 944134'
_audit_update_record             
;
2015-02-12 deposited with the CCDC.
2015-05-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C118 H186 Cl2 F6 N10 O16'
_chemical_formula_weight         2185.67

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'
F F 0.0171 0.0103 '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   'P2(1)/n  '

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                   17.066(10)
_cell_length_b                   18.946(10)
_cell_length_c                   20.674(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.450(15)
_cell_angle_gamma                90.00
_cell_volume                     6443(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1443
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      17.47

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2360
_exptl_absorpt_coefficient_mu    0.120
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9881
_exptl_absorpt_correction_T_max  0.9929
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26397
_diffrn_reflns_av_R_equivalents  0.1341
_diffrn_reflns_av_UnetI/netI     0.0989
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.38
_diffrn_reflns_theta_max         19.68
_reflns_number_total             5697
_reflns_number_gt                3086
_reflns_threshold_expression     >2sigma(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 3v.2'
_computing_publication_material  'Mercury 3.1'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1590P)²+33.9845P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5697
_refine_ls_number_parameters     675
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1603
_refine_ls_R_factor_gt           0.0949
_refine_ls_wR_factor_ref         0.3064
_refine_ls_wR_factor_gt          0.2479
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_restrained_S_all      0.914
_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
C25A C 0.1687(9) 0.5345(8) 0.0563(7) 0.094(5) Uani 0.92 1 d P . .
H25A H 0.2099 0.5618 0.0876 0.113 Uiso 0.92 1 calc PR . .
H25B H 0.1954 0.5064 0.0292 0.113 Uiso 0.92 1 calc PR . .
C54 C 0.2884(8) 0.3631(8) 0.5151(6) 0.042(3) Uani 0.74 1 d P . .
Cl1 Cl 0.65726(14) 0.53138(14) 0.15195(13) 0.0613(8) Uani 1 1 d . . .
C5 C 0.3186(6) -0.1334(6) 0.5536(5) 0.049(3) Uani 1 1 d . . .
C4 C 0.3386(6) -0.0757(6) 0.5935(5) 0.054(3) Uani 1 1 d . . .
H4 H 0.3015 -0.0388 0.5887 0.064 Uiso 1 1 calc R . .
C6 C 0.3743(6) -0.1883(6) 0.5609(5) 0.057(3) Uani 1 1 d . . .
H6 H 0.3614 -0.2276 0.5331 0.068 Uiso 1 1 calc R . .
C1 C 0.4490(6) -0.1858(7) 0.6090(6) 0.068(3) Uani 1 1 d . . .
H1 H 0.4860 -0.2228 0.6148 0.082 Uiso 1 1 calc R . .
C2 C 0.4650(7) -0.1259(8) 0.6471(6) 0.066(3) Uani 1 1 d . . .
C3 C 0.4134(7) -0.0701(6) 0.6416(5) 0.060(3) Uani 1 1 d . . .
H3 H 0.4272 -0.0303 0.6686 0.072 Uiso 1 1 calc R . .
C7 C 0.2392(6) -0.1429(6) 0.5006(6) 0.051(3) Uani 1 1 d . . .
C9 C -0.0023(7) -0.0279(5) 0.2153(5) 0.058(3) Uani 1 1 d . . .
C11 C -0.1065(10) -0.0592(7) 0.0935(7) 0.094(4) Uani 1 1 d . . .
C10 C -0.1362(7) -0.0515(6) 0.1476(7) 0.079(4) Uani 1 1 d . . .
H10 H -0.1917 -0.0557 0.1433 0.095 Uiso 1 1 calc R . .
C14 C 0.0589(7) -0.0117(5) 0.2801(5) 0.055(3) Uani 1 1 d . . .
C12 C -0.0837(7) -0.0375(6) 0.2085(6) 0.068(3) Uani 1 1 d . . .
H12 H -0.1035 -0.0343 0.2462 0.082 Uiso 1 1 calc R . .
C8 C 0.0263(8) -0.0355(7) 0.1582(6) 0.083(4) Uani 1 1 d . . .
H8 H 0.0814 -0.0301 0.1617 0.099 Uiso 1 1 calc R . .
C13 C -0.0262(11) -0.0507(8) 0.0976(7) 0.106(5) Uani 1 1 d . . .
H13 H -0.0073 -0.0551 0.0595 0.127 Uiso 1 1 calc R . .
O1 O 0.1317(5) -0.0096(4) 0.2836(3) 0.078(2) Uani 1 1 d . . .
N1 N 0.0313(4) 0.0014(4) 0.3339(4) 0.050(2) Uani 1 1 d . . .
H1A H -0.0199 -0.0020 0.3305 0.061 Uiso 1 1 calc R . .
N2 N 0.1601(5) 0.4006(5) 0.1928(4) 0.061(2) Uani 1 1 d . . .
C16 C 0.0879(6) 0.3549(6) 0.1617(6) 0.070(3) Uani 1 1 d . . .
H16A H 0.0466 0.3839 0.1324 0.084 Uiso 1 1 calc R . .
H16B H 0.0656 0.3373 0.1972 0.084 Uiso 1 1 calc R . .
C15 C 0.1057(7) 0.2915(6) 0.1213(6) 0.080(4) Uani 1 1 d . . .
H15A H 0.1433 0.3057 0.0958 0.096 Uiso 1 1 calc R . .
H15B H 0.1310 0.2542 0.1518 0.096 Uiso 1 1 calc R . .
C19 C 0.1338(6) 0.4513(6) 0.2401(5) 0.071(3) Uani 1 1 d . . .
H19A H 0.0873 0.4779 0.2143 0.085 Uiso 1 1 calc R . .
H19B H 0.1157 0.4238 0.2729 0.085 Uiso 1 1 calc R . .
C20 C 0.1973(7) 0.5032(7) 0.2774(6) 0.086(4) Uani 1 1 d . . .
H20A H 0.2121 0.5343 0.2453 0.103 Uiso 1 1 calc R . .
H20B H 0.2456 0.4776 0.3010 0.103 Uiso 1 1 calc R . .
C21 C 0.1669(8) 0.5481(8) 0.3282(6) 0.105(5) Uani 1 1 d . . .
H21A H 0.1191 0.5744 0.3046 0.126 Uiso 1 1 calc R . .
H21B H 0.1515 0.5171 0.3601 0.126 Uiso 1 1 calc R . .
C22 C 0.2312(10) 0.5986(9) 0.3654(8) 0.148(7) Uani 1 1 d . . .
H22A H 0.2793 0.5728 0.3875 0.222 Uiso 1 1 calc R . .
H22B H 0.2116 0.6239 0.3982 0.222 Uiso 1 1 calc R . .
H22C H 0.2438 0.6315 0.3343 0.222 Uiso 1 1 calc R . .
C18 C 0.0281(7) 0.2641(7) 0.0737(6) 0.085(4) Uani 1 1 d . . .
H18A H -0.0147 0.2636 0.0966 0.102 Uiso 1 1 calc R . .
H18B H 0.0115 0.2959 0.0358 0.102 Uiso 1 1 calc R . .
C23 C 0.1881(6) 0.4414(6) 0.1395(5) 0.064(3) Uani 1 1 d . . .
H23A H 0.2336 0.4710 0.1619 0.077 Uiso 1 1 calc R . .
H23B H 0.2080 0.4078 0.1121 0.077 Uiso 1 1 calc R . .
C24 C 0.1264(8) 0.4862(7) 0.0948(7) 0.093(4) Uani 1 1 d . . .
H24A H 0.0981 0.5139 0.1210 0.111 Uiso 1 1 calc R . .
H24B H 0.0868 0.4570 0.0639 0.111 Uiso 1 1 calc R . .
C26 C 0.1133(12) 0.5799(12) 0.0150(10) 0.194(9) Uani 1 1 d . . .
H26A H 0.1097 0.6227 0.0389 0.291 Uiso 1 1 calc R . .
H26B H 0.0609 0.5577 0.0019 0.291 Uiso 1 1 calc R . .
H26C H 0.1310 0.5906 -0.0242 0.291 Uiso 1 1 calc R . .
C27 C 0.2310(6) 0.3566(6) 0.2311(6) 0.079(4) Uani 1 1 d . . .
H27A H 0.2770 0.3877 0.2480 0.095 Uiso 1 1 calc R . .
H27B H 0.2456 0.3241 0.2000 0.095 Uiso 1 1 calc R . .
N3 N 0.7305(4) 0.2140(4) 0.2416(4) 0.055(2) Uani 1 1 d . . .
C41 C 0.7565(6) 0.2211(6) 0.3175(5) 0.056(3) Uani 1 1 d . . .
H41A H 0.7087 0.2169 0.3341 0.067 Uiso 1 1 calc R . .
H41B H 0.7923 0.1820 0.3358 0.067 Uiso 1 1 calc R . .
C39 C 0.8798(6) 0.1829(6) 0.2448(5) 0.069(3) Uani 1 1 d . . .
H39A H 0.8996 0.1964 0.2916 0.083 Uiso 1 1 calc R . .
H39B H 0.8671 0.1329 0.2431 0.083 Uiso 1 1 calc R . .
C40 C 0.8028(6) 0.2247(6) 0.2122(5) 0.068(3) Uani 1 1 d . . .
H40A H 0.8165 0.2744 0.2151 0.081 Uiso 1 1 calc R . .
H40B H 0.7857 0.2124 0.1650 0.081 Uiso 1 1 calc R . .
C42 C 0.7994(6) 0.2890(6) 0.3435(5) 0.066(3) Uani 1 1 d . . .
H42A H 0.7667 0.3287 0.3221 0.080 Uiso 1 1 calc R . .
H42B H 0.8510 0.2910 0.3322 0.080 Uiso 1 1 calc R . .
C32 C 0.5912(6) 0.2656(6) 0.2322(5) 0.066(3) Uani 1 1 d . . .
H32A H 0.5999 0.2894 0.2750 0.079 Uiso 1 1 calc R . .
H32B H 0.5780 0.2167 0.2384 0.079 Uiso 1 1 calc R . .
C31 C 0.6684(6) 0.2683(6) 0.2102(5) 0.063(3) Uani 1 1 d . . .
H31A H 0.6548 0.2626 0.1619 0.076 Uiso 1 1 calc R . .
H31B H 0.6925 0.3147 0.2206 0.076 Uiso 1 1 calc R . .
C34 C 0.4416(6) 0.2940(7) 0.2031(6) 0.093(4) Uani 1 1 d . . .
H34A H 0.4264 0.2452 0.2035 0.140 Uiso 1 1 calc R . .
H34B H 0.3993 0.3195 0.1719 0.140 Uiso 1 1 calc R . .
H34C H 0.4495 0.3136 0.2472 0.140 Uiso 1 1 calc R . .
C43 C 0.8140(7) 0.2946(6) 0.4186(6) 0.075(3) Uani 1 1 d . . .
H43A H 0.7620 0.2948 0.4293 0.090 Uiso 1 1 calc R . .
H43B H 0.8437 0.2532 0.4395 0.090 Uiso 1 1 calc R . .
C35 C 0.6977(6) 0.1404(6) 0.2266(5) 0.061(3) Uani 1 1 d . . .
H35A H 0.6565 0.1328 0.2504 0.074 Uiso 1 1 calc R . .
H35B H 0.7415 0.1074 0.2446 0.074 Uiso 1 1 calc R . .
C36 C 0.6612(9) 0.1229(7) 0.1536(6) 0.109(5) Uani 1 1 d . . .
H36A H 0.7043 0.1148 0.1319 0.131 Uiso 1 1 calc R . .
H36B H 0.6286 0.1622 0.1313 0.131 Uiso 1 1 calc R . .
C33 C 0.5200(6) 0.2998(6) 0.1820(6) 0.076(3) Uani 1 1 d . . .
H33A H 0.5127 0.2774 0.1387 0.091 Uiso 1 1 calc R . .
H33B H 0.5322 0.3492 0.1773 0.091 Uiso 1 1 calc R . .
C44 C 0.8609(7) 0.3598(7) 0.4481(6) 0.096(4) Uani 1 1 d . . .
H44A H 0.9107 0.3619 0.4348 0.144 Uiso 1 1 calc R . .
H44B H 0.8731 0.3580 0.4962 0.144 Uiso 1 1 calc R . .
H44C H 0.8289 0.4010 0.4320 0.144 Uiso 1 1 calc R . .
C45 C 0.9443(6) 0.1959(6) 0.2100(6) 0.078(3) Uani 1 1 d . . .
H45A H 0.9277 0.1741 0.1661 0.093 Uiso 1 1 calc R . .
H45B H 0.9477 0.2463 0.2033 0.093 Uiso 1 1 calc R . .
C46 C 1.0258(7) 0.1701(6) 0.2442(6) 0.086(4) Uani 1 1 d . . .
H46A H 1.0480 0.1980 0.2836 0.129 Uiso 1 1 calc R . .
H46B H 1.0603 0.1737 0.2145 0.129 Uiso 1 1 calc R . .
H46C H 1.0226 0.1217 0.2569 0.129 Uiso 1 1 calc R . .
C47 C 0.0955(5) -0.1137(5) 0.4663(5) 0.054(3) Uani 1 1 d . . .
H47A H 0.0714 -0.1591 0.4709 0.064 Uiso 1 1 calc R . .
H47B H 0.0995 -0.1093 0.4205 0.064 Uiso 1 1 calc R . .
C48 C 0.0869(5) 0.0216(6) 0.3987(5) 0.054(3) Uani 1 1 d . . .
H48A H 0.1026 0.0707 0.3975 0.065 Uiso 1 1 calc R . .
H48B H 0.1357 -0.0071 0.4077 0.065 Uiso 1 1 calc R . .
F1 F 0.5390(4) -0.1231(4) 0.6940(3) 0.092(2) Uani 1 1 d . . .
F2 F -0.1605(5) -0.0741(5) 0.0327(4) 0.129(3) Uani 1 1 d . . .
N4 N 0.1755(4) -0.1088(4) 0.5127(4) 0.052(2) Uani 1 1 d . . .
H4A H 0.1824 -0.0838 0.5485 0.062 Uiso 1 1 calc R . .
C52 C 0.2225(7) 0.2538(6) 0.5047(5) 0.056(3) Uani 1 1 d . . .
H52 H 0.2242 0.2056 0.5135 0.068 Uiso 1 1 calc R . .
C49 C 0.2203(9) 0.3967(7) 0.4823(6) 0.081(4) Uani 1 1 d . . .
H49 H 0.2201 0.4451 0.4749 0.097 Uiso 1 1 calc R . .
C51 C 0.1509(6) 0.2847(6) 0.4708(5) 0.054(3) Uani 1 1 d . . .
C53 C 0.2928(7) 0.2939(8) 0.5261(5) 0.072(3) Uani 1 1 d . . .
H53 H 0.3420 0.2727 0.5477 0.087 Uiso 1 1 calc R . .
C50 C 0.1497(7) 0.3568(7) 0.4598(5) 0.070(3) Uani 1 1 d . . .
H50 H 0.1015 0.3788 0.4371 0.084 Uiso 1 1 calc R . .
F3 F 0.3572(4) 0.4017(4) 0.5368(4) 0.108(2) Uani 1 1 d . . .
C55 C 0.0744(7) 0.2445(7) 0.4418(6) 0.062(3) Uani 1 1 d . . .
O3 O 0.0166(4) 0.2694(4) 0.3973(4) 0.073(2) Uani 1 1 d . . .
N5 N 0.0671(5) 0.1797(5) 0.4656(4) 0.057(2) Uani 1 1 d . . .
H5 H 0.1048 0.1636 0.4986 0.069 Uiso 1 1 calc R . .
C57 C 0.0442(5) 0.0108(6) 0.4530(5) 0.046(3) Uani 1 1 d . . .
C56 C 0.0000(5) 0.0667(5) 0.4697(4) 0.044(3) Uani 1 1 d . . .
C60 C -0.0035(5) 0.1363(5) 0.4362(5) 0.052(3) Uani 1 1 d . . .
H60A H -0.0073 0.1291 0.3890 0.062 Uiso 1 1 calc R . .
H60B H -0.0521 0.1611 0.4393 0.062 Uiso 1 1 calc R . .
C59 C 0.0433(5) -0.0551(6) 0.4817(5) 0.049(3) Uani 1 1 d . . .
O4 O 0.2341(4) -0.1783(4) 0.4506(4) 0.064(2) Uani 1 1 d . . .
O5 O 0.6880(5) 0.3921(4) 0.0752(4) 0.100(3) Uani 1 1 d . . .
O6 O 0.7706(7) 0.4321(5) 0.2521(5) 0.135(4) Uani 1 1 d . . .
C75 C 0.2174(8) 0.3143(7) 0.2897(7) 0.109(5) Uani 1 1 d . . .
H75A H 0.1671 0.2880 0.2746 0.131 Uiso 1 1 calc R . .
H75B H 0.2113 0.3467 0.3244 0.131 Uiso 1 1 calc R . .
C77 C 0.0380(8) 0.1911(8) 0.0486(7) 0.112(5) Uani 1 1 d . . .
H77A H 0.0808 0.1912 0.0264 0.168 Uiso 1 1 calc R . .
H77B H -0.0119 0.1765 0.0175 0.168 Uiso 1 1 calc R . .
H77C H 0.0515 0.1588 0.0857 0.168 Uiso 1 1 calc R . .
Cl2 Cl 0.87451(19) 0.38361(19) 0.1564(2) 0.1139(14) Uani 1 1 d . . .
O10 O 0.0037(5) 0.3794(5) 0.3058(5) 0.122(3) Uani 1 1 d . . .
C76 C 0.2913(9) 0.2592(12) 0.3223(10) 0.192(10) Uani 1 1 d . . .
C100 C 0.6077(15) 0.0563(9) 0.1473(8) 0.199(12) Uani 1 1 d . . .
H10A H 0.6434 0.0159 0.1499 0.238 Uiso 1 1 calc R . .
H10B H 0.5875 0.0547 0.1869 0.238 Uiso 1 1 calc R . .
C101 C 0.5479(13) 0.0463(13) 0.0979(18) 0.265(16) 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
C25A C26 1.39(2) . ?
C25A C24 1.517(16) . ?
C54 C53 1.329(16) . ?
C54 C49 1.340(16) . ?
C54 F3 1.355(12) . ?
C5 C4 1.358(13) . ?
C5 C6 1.390(13) . ?
C5 C7 1.510(14) . ?
C4 C3 1.397(13) . ?
C6 C1 1.394(13) . ?
C1 C2 1.366(15) . ?
C2 C3 1.362(14) . ?
C2 F1 1.373(12) . ?
C7 O4 1.215(11) . ?
C7 N4 1.344(12) . ?
C9 C12 1.370(14) . ?
C9 C8 1.399(14) . ?
C9 C14 1.494(14) . ?
C11 C10 1.352(16) . ?
C11 C13 1.361(17) . ?
C11 F2 1.375(14) . ?
C10 C12 1.364(14) . ?
C14 O1 1.226(11) . ?
C14 N1 1.343(12) . ?
C8 C13 1.363(16) . ?
N1 C48 1.470(11) . ?
N2 C16 1.502(12) . ?
N2 C27 1.508(12) . ?
N2 C19 1.523(12) . ?
N2 C23 1.523(12) . ?
C16 C15 1.539(14) . ?
C15 C18 1.515(15) . ?
C19 C20 1.513(14) . ?
C20 C21 1.544(16) . ?
C21 C22 1.505(18) . ?
C18 C77 1.504(16) . ?
C23 C24 1.472(14) . ?
C27 C75 1.522(15) . ?
N3 C31 1.496(11) . ?
N3 C35 1.504(12) . ?
N3 C41 1.519(11) . ?
N3 C40 1.526(12) . ?
C41 C42 1.507(13) . ?
C39 C45 1.486(13) . ?
C39 C40 1.529(13) . ?
C42 C43 1.511(14) . ?
C32 C31 1.504(13) . ?
C32 C33 1.516(13) . ?
C34 C33 1.518(14) . ?
C43 C44 1.510(15) . ?
C35 C36 1.509(15) . ?
C36 C100 1.54(2) . ?
C45 C46 1.466(14) . ?
C47 N4 1.448(11) . ?
C47 C59 1.509(13) . ?
C48 C57 1.507(12) . ?
C52 C51 1.368(13) . ?
C52 C53 1.388(14) . ?
C49 C50 1.392(15) . ?
C51 C50 1.384(14) . ?
C51 C55 1.492(14) . ?
C55 O3 1.248(12) . ?
C55 N5 1.341(12) . ?
N5 C60 1.451(11) . ?
C57 C59 1.385(13) . ?
C57 C56 1.396(13) . ?
C56 C59 1.414(13) 3_556 ?
C56 C60 1.485(13) . ?
C59 C56 1.414(13) 3_556 ?
C75 C76 1.638(19) . ?
C100 C101 1.25(2) . ?

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
C26 C25A C24 110.8(13) . . ?
C53 C54 C49 123.8(11) . . ?
C53 C54 F3 118.1(13) . . ?
C49 C54 F3 118.0(13) . . ?
C4 C5 C6 118.9(10) . . ?
C4 C5 C7 124.6(10) . . ?
C6 C5 C7 116.4(10) . . ?
C5 C4 C3 121.8(10) . . ?
C5 C6 C1 121.3(10) . . ?
C2 C1 C6 116.4(10) . . ?
C3 C2 C1 124.9(10) . . ?
C3 C2 F1 118.7(12) . . ?
C1 C2 F1 116.4(12) . . ?
C2 C3 C4 116.6(10) . . ?
O4 C7 N4 123.0(9) . . ?
O4 C7 C5 122.0(10) . . ?
N4 C7 C5 114.9(10) . . ?
C12 C9 C8 118.2(10) . . ?
C12 C9 C14 124.4(10) . . ?
C8 C9 C14 117.3(11) . . ?
C10 C11 C13 122.0(12) . . ?
C10 C11 F2 118.1(14) . . ?
C13 C11 F2 119.9(14) . . ?
C11 C10 C12 119.0(12) . . ?
O1 C14 N1 121.2(10) . . ?
O1 C14 C9 121.0(10) . . ?
N1 C14 C9 117.8(10) . . ?
C10 C12 C9 121.3(11) . . ?
C13 C8 C9 120.4(12) . . ?
C11 C13 C8 119.1(12) . . ?
C14 N1 C48 121.3(8) . . ?
C16 N2 C27 111.0(8) . . ?
C16 N2 C19 106.9(8) . . ?
C27 N2 C19 110.1(8) . . ?
C16 N2 C23 111.3(8) . . ?
C27 N2 C23 107.3(8) . . ?
C19 N2 C23 110.3(8) . . ?
N2 C16 C15 115.1(8) . . ?
C18 C15 C16 110.8(10) . . ?
C20 C19 N2 116.4(9) . . ?
C19 C20 C21 112.3(10) . . ?
C22 C21 C20 111.5(12) . . ?
C77 C18 C15 112.3(11) . . ?
C24 C23 N2 115.8(8) . . ?
C23 C24 C25A 108.5(10) . . ?
N2 C27 C75 116.0(9) . . ?
C31 N3 C35 111.5(7) . . ?
C31 N3 C41 111.5(8) . . ?
C35 N3 C41 106.5(7) . . ?
C31 N3 C40 106.9(7) . . ?
C35 N3 C40 109.7(8) . . ?
C41 N3 C40 110.8(7) . . ?
C42 C41 N3 115.1(8) . . ?
C45 C39 C40 111.2(9) . . ?
N3 C40 C39 116.6(8) . . ?
C41 C42 C43 111.0(9) . . ?
C31 C32 C33 112.7(9) . . ?
N3 C31 C32 115.0(8) . . ?
C44 C43 C42 113.3(10) . . ?
N3 C35 C36 116.2(9) . . ?
C35 C36 C100 110.0(11) . . ?
C32 C33 C34 112.4(9) . . ?
C46 C45 C39 116.2(9) . . ?
N4 C47 C59 108.6(8) . . ?
N1 C48 C57 108.6(7) . . ?
C7 N4 C47 120.8(8) . . ?
C51 C52 C53 120.5(10) . . ?
C54 C49 C50 117.9(11) . . ?
C52 C51 C50 118.6(10) . . ?
C52 C51 C55 123.7(11) . . ?
C50 C51 C55 117.7(11) . . ?
C54 C53 C52 118.7(11) . . ?
C51 C50 C49 120.5(11) . . ?
O3 C55 N5 119.0(10) . . ?
O3 C55 C51 122.6(11) . . ?
N5 C55 C51 118.4(11) . . ?
C55 N5 C60 120.8(8) . . ?
C59 C57 C56 120.7(9) . . ?
C59 C57 C48 120.4(10) . . ?
C56 C57 C48 118.8(10) . . ?
C57 C56 C59 118.5(9) . 3_556 ?
C57 C56 C60 121.1(9) . . ?
C59 C56 C60 120.3(10) 3_556 . ?
N5 C60 C56 112.5(8) . . ?
C57 C59 C56 120.8(9) . 3_556 ?
C57 C59 C47 119.9(10) . . ?
C56 C59 C47 119.1(10) 3_556 . ?
C27 C75 C76 113.5(12) . . ?
C101 C100 C36 121.9(18) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        19.68
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.072
####################################################################### 
# 
# 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_Complex3
_database_code_depnum_ccdc_archive 'CCDC 944137'
_audit_update_record             
;
2015-02-12 deposited with the CCDC.
2015-05-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C90 H120 N14 O26'
_chemical_formula_weight         1814.00

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   'C2/c  '

loop_
_symmetry_equiv_pos_as_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                   38.647(4)
_cell_length_b                   10.5794(11)
_cell_length_c                   23.724(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.545(3)
_cell_angle_gamma                90.00
_cell_volume                     9615.9(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    1773
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      18.91

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3864
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9890
_exptl_absorpt_correction_T_max  0.9926
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19921
_diffrn_reflns_av_R_equivalents  0.0903
_diffrn_reflns_av_UnetI/netI     0.0704
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.06
_diffrn_reflns_theta_max         19.74
_reflns_number_total             4282
_reflns_number_gt                2783
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep 3v.2'
_computing_publication_material  'mercury 3.1'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.5000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4282
_refine_ls_number_parameters     590
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0524
_refine_ls_wR_factor_ref         0.1712
_refine_ls_wR_factor_gt          0.1449
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_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
C2 C 0.03853(16) 0.1066(6) 0.8853(2) 0.0392(15) Uani 1 1 d . . .
C4 C 0.01882(15) 0.0261(6) 0.8388(2) 0.0604(19) Uani 1 1 d . . .
H4A H -0.0054 0.0490 0.8341 0.091 Uiso 1 1 calc R . .
H4B H 0.0212 -0.0614 0.8492 0.091 Uiso 1 1 calc R . .
H4C H 0.0282 0.0399 0.8038 0.091 Uiso 1 1 calc R . .
C6 C 0.02887(13) -0.0739(6) 1.0204(2) 0.0343(15) Uani 1 1 d . . .
C7 C 0.06109(13) -0.1526(5) 1.0403(2) 0.0417(16) Uani 1 1 d . . .
H7A H 0.0711 -0.1262 1.0782 0.050 Uiso 1 1 calc R . .
H7B H 0.0548 -0.2412 1.0418 0.050 Uiso 1 1 calc R . .
C9 C 0.12057(15) -0.1360(5) 1.0198(3) 0.0333(15) Uani 1 1 d . . .
C11 C 0.14483(14) -0.0939(5) 0.9791(2) 0.0294(14) Uani 1 1 d . . .
C12 C 0.17746(15) -0.0502(5) 1.0013(2) 0.0360(15) Uani 1 1 d . . .
H12 H 0.1837 -0.0495 1.0405 0.043 Uiso 1 1 calc R . .
C13 C 0.20087(14) -0.0079(5) 0.9669(3) 0.0372(15) Uani 1 1 d . . .
H13 H 0.2230 0.0197 0.9822 0.045 Uiso 1 1 calc R . .
C14 C 0.19075(15) -0.0075(5) 0.9094(2) 0.0330(14) Uani 1 1 d . . .
C15 C 0.15891(15) -0.0529(5) 0.8849(2) 0.0380(15) Uani 1 1 d . . .
H15 H 0.1531 -0.0551 0.8456 0.046 Uiso 1 1 calc R . .
C16 C 0.13599(14) -0.0948(5) 0.9204(3) 0.0359(15) Uani 1 1 d . . .
H16 H 0.1141 -0.1243 0.9049 0.043 Uiso 1 1 calc R . .
C21 C 0.02867(14) 0.0556(6) 1.0326(2) 0.0326(14) Uani 1 1 d . . .
C22 C 0.06059(13) 0.1162(6) 1.0656(2) 0.0444(16) Uani 1 1 d . . .
H22A H 0.0537 0.1908 1.0851 0.053 Uiso 1 1 calc R . .
H22B H 0.0713 0.0574 1.0941 0.053 Uiso 1 1 calc R . .
C24 C 0.11609(15) 0.2036(5) 1.0492(3) 0.0329(14) Uani 1 1 d . . .
C26 C 0.14094(13) 0.2411(5) 1.0089(2) 0.0285(13) Uani 1 1 d . . .
C27 C 0.17460(15) 0.2778(5) 1.0320(2) 0.0372(15) Uani 1 1 d . . .
H27 H 0.1810 0.2743 1.0712 0.045 Uiso 1 1 calc R . .
C28 C 0.19861(14) 0.3192(5) 0.9977(2) 0.0340(15) Uani 1 1 d . . .
H28 H 0.2210 0.3425 1.0134 0.041 Uiso 1 1 calc R . .
C29 C 0.18848(14) 0.3251(5) 0.9398(2) 0.0305(14) Uani 1 1 d . . .
C30 C 0.15612(15) 0.2872(5) 0.9152(2) 0.0330(14) Uani 1 1 d . . .
H30 H 0.1504 0.2888 0.8759 0.040 Uiso 1 1 calc R . .
C31 C 0.13216(14) 0.2466(5) 0.9495(2) 0.0327(14) Uani 1 1 d . . .
H31 H 0.1099 0.2226 0.9332 0.039 Uiso 1 1 calc R . .
C35 C -0.00042(15) 0.1286(5) 1.0128(2) 0.0331(14) Uani 1 1 d . . .
C36 C -0.00048(14) 0.2685(5) 1.0284(3) 0.0482(16) Uani 1 1 d . . .
H36A H -0.0239 0.3024 1.0194 0.058 Uiso 1 1 calc R . .
H36B H 0.0066 0.2785 1.0689 0.058 Uiso 1 1 calc R . .
C38 C 0.04252(14) 0.4344(5) 1.0202(3) 0.0366(15) Uani 1 1 d . . .
C40 C 0.06919(15) 0.4859(5) 0.9862(2) 0.0325(14) Uani 1 1 d . . .
C41 C 0.06454(15) 0.4919(5) 0.9275(3) 0.0412(15) Uani 1 1 d . . .
H41 H 0.0435 0.4655 0.9072 0.049 Uiso 1 1 calc R . .
C42 C 0.09083(16) 0.5367(5) 0.8986(2) 0.0446(16) Uani 1 1 d . . .
H42 H 0.0877 0.5418 0.8592 0.054 Uiso 1 1 calc R . .
C43 C 0.12214(15) 0.5740(5) 0.9302(3) 0.0391(15) Uani 1 1 d . . .
C44 C 0.12689(15) 0.5706(5) 0.9886(2) 0.0364(15) Uani 1 1 d . . .
H44 H 0.1478 0.5972 1.0090 0.044 Uiso 1 1 calc R . .
C45 C 0.10038(16) 0.5274(5) 1.0163(2) 0.0350(15) Uani 1 1 d . . .
H45 H 0.1033 0.5257 1.0558 0.042 Uiso 1 1 calc R . .
C50 C 0.16649(13) 0.4140(5) 0.6436(2) 0.0317(14) Uani 1 1 d . . .
H50A H 0.1692 0.4882 0.6205 0.038 Uiso 1 1 calc R . .
H50B H 0.1488 0.3609 0.6225 0.038 Uiso 1 1 calc R . .
C51 C 0.20070(13) 0.3423(5) 0.6507(2) 0.0404(15) Uani 1 1 d . . .
H51A H 0.1979 0.2630 0.6701 0.049 Uiso 1 1 calc R . .
H51B H 0.2184 0.3915 0.6737 0.049 Uiso 1 1 calc R . .
C52 C 0.21224(13) 0.3162(5) 0.5931(2) 0.0396(15) Uani 1 1 d . . .
H52A H 0.2168 0.3960 0.5754 0.048 Uiso 1 1 calc R . .
H52B H 0.1934 0.2746 0.5691 0.048 Uiso 1 1 calc R . .
C53 C 0.24483(14) 0.2340(5) 0.5963(2) 0.0512(17) Uani 1 1 d . . .
H53A H 0.2637 0.2744 0.6201 0.077 Uiso 1 1 calc R . .
H53B H 0.2511 0.2227 0.5588 0.077 Uiso 1 1 calc R . .
H53C H 0.2402 0.1531 0.6121 0.077 Uiso 1 1 calc R . .
C54 C 0.14748(14) 0.3445(5) 0.7358(2) 0.0413(16) Uani 1 1 d . . .
H54A H 0.1701 0.3086 0.7497 0.050 Uiso 1 1 calc R . .
H54B H 0.1375 0.3762 0.7685 0.050 Uiso 1 1 calc R . .
C55 C 0.12443(15) 0.2401(5) 0.7094(2) 0.0450(16) Uani 1 1 d . . .
H55A H 0.1336 0.2086 0.6759 0.054 Uiso 1 1 calc R . .
H55B H 0.1012 0.2729 0.6976 0.054 Uiso 1 1 calc R . .
C56 C 0.12250(18) 0.1328(6) 0.7512(3) 0.074(2) Uani 1 1 d . . .
H56A H 0.1460 0.1044 0.7647 0.089 Uiso 1 1 calc R . .
H56B H 0.1123 0.1643 0.7837 0.089 Uiso 1 1 calc R . .
C57 C 0.1013(2) 0.0212(7) 0.7263(3) 0.097(3) Uani 1 1 d . . .
H57A H 0.0777 0.0474 0.7146 0.146 Uiso 1 1 calc R . .
H57B H 0.1016 -0.0440 0.7545 0.146 Uiso 1 1 calc R . .
H57C H 0.1112 -0.0106 0.6941 0.146 Uiso 1 1 calc R . .
C58 C 0.11849(13) 0.5230(5) 0.6796(2) 0.0352(15) Uani 1 1 d . . .
H58A H 0.1223 0.5881 0.6523 0.042 Uiso 1 1 calc R . .
H58B H 0.1023 0.4621 0.6602 0.042 Uiso 1 1 calc R . .
C59 C 0.10123(13) 0.5835(5) 0.7267(2) 0.0409(15) Uani 1 1 d . . .
H59A H 0.0949 0.5183 0.7521 0.049 Uiso 1 1 calc R . .
H59B H 0.1177 0.6398 0.7484 0.049 Uiso 1 1 calc R . .
C60 C 0.06914(14) 0.6570(6) 0.7036(2) 0.0479(16) Uani 1 1 d . . .
H60A H 0.0533 0.6018 0.6799 0.057 Uiso 1 1 calc R . .
H60B H 0.0758 0.7251 0.6798 0.057 Uiso 1 1 calc R . .
C61 C 0.05029(16) 0.7121(6) 0.7497(3) 0.069(2) Uani 1 1 d . . .
H61A H 0.0416 0.6448 0.7712 0.104 Uiso 1 1 calc R . .
H61B H 0.0311 0.7630 0.7329 0.104 Uiso 1 1 calc R . .
H61C H 0.0661 0.7634 0.7746 0.104 Uiso 1 1 calc R . .
C62 C 0.17952(13) 0.5439(5) 0.7315(2) 0.0376(15) Uani 1 1 d . . .
H62A H 0.1703 0.5689 0.7660 0.045 Uiso 1 1 calc R . .
H62B H 0.2009 0.4968 0.7427 0.045 Uiso 1 1 calc R . .
C63 C 0.18839(14) 0.6615(5) 0.7005(2) 0.0404(16) Uani 1 1 d . . .
H63A H 0.2015 0.6379 0.6699 0.048 Uiso 1 1 calc R . .
H63B H 0.1670 0.7018 0.6836 0.048 Uiso 1 1 calc R . .
C64 C 0.20947(16) 0.7545(6) 0.7390(2) 0.0591(19) Uani 1 1 d . . .
H64A H 0.2315 0.7158 0.7544 0.071 Uiso 1 1 calc R . .
H64B H 0.1969 0.7749 0.7707 0.071 Uiso 1 1 calc R . .
C65 C 0.21673(18) 0.8757(6) 0.7081(3) 0.079(2) Uani 1 1 d . . .
H65A H 0.2302 0.8565 0.6779 0.118 Uiso 1 1 calc R . .
H65B H 0.2295 0.9332 0.7343 0.118 Uiso 1 1 calc R . .
H65C H 0.1950 0.9139 0.6925 0.118 Uiso 1 1 calc R . .
N8 N 0.08628(11) -0.1349(4) 1.00082(17) 0.0327(12) Uani 1 1 d . . .
H8 H 0.0793 -0.1236 0.9653 0.039 Uiso 1 1 calc R . .
N17 N 0.21522(15) 0.0434(5) 0.8728(2) 0.0480(14) Uani 1 1 d . . .
N23 N 0.08595(11) 0.1517(4) 1.02752(18) 0.0334(12) Uani 1 1 d . . .
H23 H 0.0814 0.1391 0.9915 0.040 Uiso 1 1 calc R . .
N32 N 0.21363(14) 0.3721(4) 0.9031(2) 0.0453(13) Uani 1 1 d . . .
N37 N 0.02333(11) 0.3375(4) 0.99694(19) 0.0379(12) Uani 1 1 d . . .
H37 H 0.0251 0.3156 0.9625 0.046 Uiso 1 1 calc R . .
N46 N 0.15109(16) 0.6161(5) 0.9007(3) 0.0522(14) Uani 1 1 d . . .
N49 N 0.15313(10) 0.4561(4) 0.69753(16) 0.0337(12) Uani 1 1 d . . .
O1 O 0.06352(9) 0.0564(3) 0.91641(15) 0.0403(10) Uani 1 1 d . . .
O3 O 0.02909(10) 0.2192(4) 0.88861(16) 0.0566(12) Uani 1 1 d . . .
O5 O 0.03018(11) 0.3421(4) 0.65858(18) 0.0804(15) Uani 1 1 d . . .
O10 O 0.13207(9) -0.1694(3) 1.06843(17) 0.0399(10) Uani 1 1 d . . .
O19 O 0.20770(11) 0.0337(4) 0.8214(2) 0.0724(14) Uani 1 1 d . . .
O20 O 0.24169(11) 0.0963(4) 0.89458(18) 0.0568(12) Uani 1 1 d . . .
O25 O 0.12387(9) 0.2231(4) 1.10050(18) 0.0448(11) Uani 1 1 d . . .
O33 O 0.24336(11) 0.3987(4) 0.92553(16) 0.0523(11) Uani 1 1 d . . .
O34 O 0.20406(10) 0.3823(4) 0.85256(19) 0.0647(14) Uani 1 1 d . . .
O39 O 0.04001(9) 0.4751(3) 1.06852(18) 0.0476(11) Uani 1 1 d . . .
O47 O 0.14495(12) 0.6392(5) 0.8497(2) 0.0776(15) Uani 1 1 d . . .
O48 O 0.18007(12) 0.6283(4) 0.9286(2) 0.0614(13) Uani 1 1 d . . .
O5A O 0.05796(17) 0.3463(6) 0.7862(3) 0.080(2) Uiso 0.78 1 d P . .
O5B O 0.0404(6) 0.385(2) 0.7702(9) 0.071(6) Uiso 0.22 1 d P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C2 O3 1.251(6) . ?
C2 O1 1.254(6) . ?
C2 C4 1.516(7) . ?
C6 C35 1.391(7) 5_557 ?
C6 C21 1.401(7) . ?
C6 C7 1.521(7) . ?
C7 N8 1.450(6) . ?
C9 O10 1.232(6) . ?
C9 N8 1.343(6) . ?
C9 C11 1.499(7) . ?
C11 C12 1.381(7) . ?
C11 C16 1.390(7) . ?
C12 C13 1.371(7) . ?
C13 C14 1.368(7) . ?
C14 C15 1.377(7) . ?
C14 N17 1.469(7) . ?
C15 C16 1.374(7) . ?
C21 C35 1.394(7) . ?
C21 C22 1.515(7) . ?
C22 N23 1.467(6) . ?
C24 O25 1.232(6) . ?
C24 N23 1.329(6) . ?
C24 C26 1.495(7) . ?
C26 C27 1.399(7) . ?
C26 C31 1.406(7) . ?
C27 C28 1.383(7) . ?
C28 C29 1.380(7) . ?
C29 C30 1.369(7) . ?
C29 N32 1.474(7) . ?
C30 C31 1.380(7) . ?
C35 C6 1.391(7) 5_557 ?
C35 C36 1.525(7) . ?
C36 N37 1.454(6) . ?
C38 O39 1.241(6) . ?
C38 N37 1.340(6) . ?
C38 C40 1.492(7) . ?
C40 C41 1.384(7) . ?
C40 C45 1.388(7) . ?
C41 C42 1.381(7) . ?
C42 C43 1.394(7) . ?
C43 C44 1.374(7) . ?
C43 N46 1.464(7) . ?
C44 C45 1.365(7) . ?
C50 N49 1.509(6) . ?
C50 C51 1.514(6) . ?
C51 C52 1.517(7) . ?
C52 C53 1.524(7) . ?
C54 C55 1.503(7) . ?
C54 N49 1.523(6) . ?
C55 C56 1.515(7) . ?
C56 C57 1.511(8) . ?
C58 C59 1.516(7) . ?
C58 N49 1.524(6) . ?
C59 C60 1.505(7) . ?
C60 C61 1.509(7) . ?
C62 C63 1.508(7) . ?
C62 N49 1.528(6) . ?
C63 C64 1.508(7) . ?
C64 C65 1.522(8) . ?
N17 O20 1.220(5) . ?
N17 O19 1.221(5) . ?
N32 O34 1.213(5) . ?
N32 O33 1.234(5) . ?
N46 O47 1.227(6) . ?
N46 O48 1.230(6) . ?
O5A O5B 0.84(2) . ?

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
O3 C2 O1 125.0(5) . . ?
O3 C2 C4 117.2(6) . . ?
O1 C2 C4 117.7(6) . . ?
C35 C6 C21 119.9(5) 5_557 . ?
C35 C6 C7 120.2(5) 5_557 . ?
C21 C6 C7 119.8(5) . . ?
N8 C7 C6 108.7(4) . . ?
O10 C9 N8 122.4(5) . . ?
O10 C9 C11 120.6(5) . . ?
N8 C9 C11 117.0(5) . . ?
C12 C11 C16 118.4(5) . . ?
C12 C11 C9 118.1(5) . . ?
C16 C11 C9 123.4(5) . . ?
C13 C12 C11 121.6(5) . . ?
C14 C13 C12 118.0(5) . . ?
C13 C14 C15 122.9(5) . . ?
C13 C14 N17 118.0(6) . . ?
C15 C14 N17 119.1(6) . . ?
C16 C15 C14 117.8(5) . . ?
C15 C16 C11 121.2(5) . . ?
C35 C21 C6 119.9(5) . . ?
C35 C21 C22 120.4(5) . . ?
C6 C21 C22 119.7(5) . . ?
N23 C22 C21 110.7(4) . . ?
O25 C24 N23 122.7(5) . . ?
O25 C24 C26 119.6(5) . . ?
N23 C24 C26 117.8(5) . . ?
C27 C26 C31 118.1(5) . . ?
C27 C26 C24 117.7(5) . . ?
C31 C26 C24 124.1(5) . . ?
C28 C27 C26 121.3(5) . . ?
C29 C28 C27 118.4(5) . . ?
C30 C29 C28 122.4(5) . . ?
C30 C29 N32 118.9(5) . . ?
C28 C29 N32 118.7(5) . . ?
C29 C30 C31 119.0(5) . . ?
C30 C31 C26 120.8(5) . . ?
C6 C35 C21 120.1(5) 5_557 . ?
C6 C35 C36 121.0(5) 5_557 . ?
C21 C35 C36 118.9(5) . . ?
N37 C36 C35 110.0(4) . . ?
O39 C38 N37 122.6(5) . . ?
O39 C38 C40 121.0(5) . . ?
N37 C38 C40 116.2(5) . . ?
C41 C40 C45 119.5(5) . . ?
C41 C40 C38 123.6(6) . . ?
C45 C40 C38 117.0(5) . . ?
C42 C41 C40 120.5(5) . . ?
C41 C42 C43 118.3(5) . . ?
C44 C43 C42 121.7(5) . . ?
C44 C43 N46 118.7(6) . . ?
C42 C43 N46 119.5(6) . . ?
C45 C44 C43 118.9(5) . . ?
C44 C45 C40 121.0(5) . . ?
N49 C50 C51 116.4(4) . . ?
C50 C51 C52 110.3(4) . . ?
C51 C52 C53 113.4(4) . . ?
C55 C54 N49 116.4(4) . . ?
C54 C55 C56 110.8(5) . . ?
C57 C56 C55 113.6(5) . . ?
C59 C58 N49 116.5(4) . . ?
C60 C59 C58 111.8(4) . . ?
C59 C60 C61 112.9(5) . . ?
C63 C62 N49 115.0(4) . . ?
C64 C63 C62 112.4(5) . . ?
C63 C64 C65 112.1(5) . . ?
C9 N8 C7 119.9(4) . . ?
O20 N17 O19 122.6(5) . . ?
O20 N17 C14 119.1(5) . . ?
O19 N17 C14 118.3(6) . . ?
C24 N23 C22 119.3(4) . . ?
O34 N32 O33 123.5(5) . . ?
O34 N32 C29 118.4(5) . . ?
O33 N32 C29 118.1(5) . . ?
C38 N37 C36 121.8(5) . . ?
O47 N46 O48 123.6(5) . . ?
O47 N46 C43 118.1(6) . . ?
O48 N46 C43 118.3(5) . . ?
C50 N49 C54 111.6(4) . . ?
C50 N49 C58 106.6(4) . . ?
C54 N49 C58 109.7(4) . . ?
C50 N49 C62 110.4(4) . . ?
C54 N49 C62 107.1(4) . . ?
C58 N49 C62 111.5(4) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        19.74
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.047
####################################################################### 
# 
# 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_Complex4
_database_code_depnum_ccdc_archive 'CCDC 996872'
_audit_update_record             
;
2015-02-12 deposited with the CCDC.
2015-05-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C96 H120 F18 N8 O14'
_chemical_formula_weight         1952.00

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'
F F 0.0171 0.0103 '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   '

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

_cell_length_a                   11.425(4)
_cell_length_b                   14.397(5)
_cell_length_c                   16.570(6)
_cell_angle_alpha                80.640(10)
_cell_angle_beta                 71.645(10)
_cell_angle_gamma                89.007(10)
_cell_volume                     2550.8(17)
_cell_formula_units_Z            1
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    946
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      13.44

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1026
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.9936
_exptl_absorpt_correction_T_max  0.9979
_exptl_absorpt_process_details   multi-scan

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11098
_diffrn_reflns_av_R_equivalents  0.0815
_diffrn_reflns_av_UnetI/netI     0.1113
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.31
_diffrn_reflns_theta_max         19.71
_reflns_number_total             4503
_reflns_number_gt                2205
_reflns_threshold_expression     >2sigma(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    'mercury 3.1'
_computing_publication_material  'ortep 3v.2'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1856P)²+8.0843P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4503
_refine_ls_number_parameters     616
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1678
_refine_ls_R_factor_gt           0.0856
_refine_ls_wR_factor_ref         0.3084
_refine_ls_wR_factor_gt          0.2260
_refine_ls_goodness_of_fit_ref   0.855
_refine_ls_restrained_S_all      0.855
_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
F12A F 0.4281(18) 0.4830(14) 0.7227(13) 0.144(6) Uiso 0.50 1 d P A 2
F14A F 0.2796(17) 0.3974(14) 0.7378(13) 0.146(6) Uiso 0.50 1 d P A 2
F13B F 0.3355(18) 0.5021(12) 0.6332(11) 0.134(5) Uiso 0.51 1 d P A 2
C58B C 0.260(5) 0.515(4) 0.744(3) 0.073(13) Uiso 0.38 1 d P A 2
F5B F 0.2215(13) 0.5534(11) 1.0220(9) 0.110(4) Uiso 0.54 1 d P B 2
F4B F 0.3552(11) 0.5974(10) 1.0835(8) 0.107(4) Uiso 0.57 1 d P B 2
F6A F 0.2286(12) 0.6924(9) 1.0522(8) 0.095(4) Uiso 0.57 1 d P B 2
F8B F 0.0483(16) 0.6111(11) 0.2698(11) 0.117(5) Uiso 0.54 1 d P C 2
F7B F 0.1473(13) 0.4862(11) 0.2721(9) 0.114(4) Uiso 0.52 1 d P C 2
F12B F 0.3595(18) 0.4291(13) 0.7686(11) 0.133(6) Uiso 0.50 1 d P A 1
F13A F 0.4117(15) 0.5225(10) 0.6510(10) 0.105(5) Uiso 0.49 1 d P A 1
F14B F 0.2511(17) 0.4333(14) 0.6812(13) 0.142(6) Uiso 0.50 1 d P A 1
C58A C 0.323(2) 0.4834(13) 0.7106(13) 0.054(5) Uiso 0.62 1 d P A 1
F8A F -0.0457(16) 0.5916(12) 0.3453(11) 0.122(5) Uiso 0.46 1 d P C 1
F7A F 0.117(2) 0.5761(18) 0.2469(15) 0.167(8) Uiso 0.48 1 d P C 1
F5A F 0.2903(16) 0.5375(13) 1.0563(11) 0.119(5) Uiso 0.46 1 d P B 1
F4A F 0.303(2) 0.6685(18) 1.0806(15) 0.152(8) Uiso 0.43 1 d P B 1
F6B F 0.181(2) 0.6528(16) 1.0237(13) 0.135(7) Uiso 0.43 1 d P B 1
C11 C 0.4133(9) 0.9753(6) 0.5806(6) 0.047(2) Uani 1 1 d . . .
C22 C 0.4973(10) 0.7711(7) 0.8184(7) 0.053(3) Uani 1 1 d . . .
C15 C 0.1852(10) 0.7073(7) 0.7882(7) 0.051(3) Uani 1 1 d . . .
C9 C 0.2544(8) 0.9323(7) 0.5128(6) 0.053(3) Uani 1 1 d . . .
H9A H 0.1983 0.9303 0.5708 0.063 Uiso 1 1 calc R . .
H9B H 0.2210 0.9735 0.4736 0.063 Uiso 1 1 calc R . .
C27 C 0.4109(10) 0.7440(8) 0.8999(7) 0.060(3) Uani 1 1 d . . .
H27 H 0.3659 0.7889 0.9302 0.072 Uiso 1 1 calc R . .
C12 C 0.5322(9) 1.0025(6) 0.5744(6) 0.044(2) Uani 1 1 d . . .
C30 C 0.1692(9) 0.0355(7) 0.2513(6) 0.063(3) Uani 1 1 d . . .
H30A H 0.1627 -0.0167 0.2978 0.075 Uiso 1 1 calc R . .
H30B H 0.2501 0.0657 0.2368 0.075 Uiso 1 1 calc R . .
C8 C 0.3803(8) 0.9712(6) 0.5069(7) 0.049(2) Uani 1 1 d . . .
C10 C 0.3154(9) 0.9493(6) 0.6692(6) 0.054(3) Uani 1 1 d . . .
H10A H 0.3426 0.9730 0.7121 0.065 Uiso 1 1 calc R . .
H10B H 0.2391 0.9793 0.6680 0.065 Uiso 1 1 calc R . .
C14 C 0.2063(9) 0.8134(7) 0.7678(7) 0.050(3) Uani 1 1 d . . .
C13 C 0.5674(9) 0.9968(7) 0.6559(6) 0.056(3) Uani 1 1 d . . .
H13A H 0.6510 1.0219 0.6417 0.067 Uiso 1 1 calc R . .
H13B H 0.5124 1.0340 0.6947 0.067 Uiso 1 1 calc R . .
C34 C 0.1551(9) 0.0723(8) 0.1015(6) 0.068(3) Uani 1 1 d . . .
H34A H 0.1602 0.0440 0.0513 0.081 Uiso 1 1 calc R . .
H34B H 0.0747 0.0997 0.1195 0.081 Uiso 1 1 calc R . .
C16 C 0.2595(10) 0.6479(8) 0.7437(7) 0.063(3) Uani 1 1 d . A .
H16 H 0.3304 0.6688 0.6983 0.075 Uiso 1 1 calc R . .
C38 C 0.2804(9) -0.0573(7) 0.1397(6) 0.067(3) Uani 1 1 d . . .
H38A H 0.2818 -0.0751 0.0854 0.080 Uiso 1 1 calc R . .
H38B H 0.3501 -0.0138 0.1275 0.080 Uiso 1 1 calc R . .
C26 C 0.3937(11) 0.6499(10) 0.9346(7) 0.072(3) Uani 1 1 d . B .
C1 C 0.2068(10) 0.7036(8) 0.4384(6) 0.064(3) Uani 1 1 d . . .
C23 C 0.5625(11) 0.7021(10) 0.7772(7) 0.081(3) Uani 1 1 d . . .
H23 H 0.6201 0.7191 0.7228 0.097 Uiso 1 1 calc R . .
C21 C 0.5138(9) 0.8737(8) 0.7833(8) 0.056(3) Uani 1 1 d . . .
C6 C 0.1366(10) 0.6718(8) 0.3935(7) 0.071(3) Uani 1 1 d . . .
H6 H 0.0831 0.7120 0.3739 0.086 Uiso 1 1 calc R . .
C35 C 0.2524(11) 0.1503(8) 0.0753(7) 0.089(4) Uani 1 1 d . . .
H35A H 0.2486 0.1792 0.1250 0.107 Uiso 1 1 calc R . .
H35B H 0.3332 0.1241 0.0554 0.107 Uiso 1 1 calc R . .
C5 C 0.1460(12) 0.5799(11) 0.3777(8) 0.090(4) Uani 1 1 d . C .
C2 C 0.2815(11) 0.6421(9) 0.4703(7) 0.085(4) Uani 1 1 d . . .
H2 H 0.3259 0.6620 0.5031 0.102 Uiso 1 1 calc R . .
C42 C 0.0482(9) -0.0699(7) 0.2011(7) 0.073(3) Uani 1 1 d . . .
H42A H 0.0523 -0.1166 0.2493 0.087 Uiso 1 1 calc R . .
H42B H -0.0234 -0.0329 0.2220 0.087 Uiso 1 1 calc R . .
C40 C 0.4279(11) -0.1797(9) 0.1618(8) 0.095(4) Uani 1 1 d . . .
H40A H 0.4365 -0.1983 0.1066 0.114 Uiso 1 1 calc R . .
H40B H 0.4878 -0.1288 0.1520 0.114 Uiso 1 1 calc R . .
C7 C 0.1927(10) 0.8047(8) 0.4497(6) 0.058(3) Uani 1 1 d . . .
C25 C 0.4577(13) 0.5824(8) 0.8925(10) 0.085(4) Uani 1 1 d . . .
H25 H 0.4425 0.5190 0.9168 0.102 Uiso 1 1 calc R . .
C39 C 0.2997(10) -0.1439(8) 0.1972(7) 0.078(3) Uani 1 1 d . . .
H39A H 0.2390 -0.1925 0.2022 0.094 Uiso 1 1 calc R . .
H39B H 0.2881 -0.1294 0.2543 0.094 Uiso 1 1 calc R . .
C24 C 0.5452(13) 0.6088(10) 0.8138(10) 0.099(4) Uani 1 1 d . . .
H24 H 0.5926 0.5637 0.7853 0.119 Uiso 1 1 calc R . .
C32 C 0.0967(10) 0.1463(9) 0.3557(7) 0.083(3) Uani 1 1 d . . .
H32A H 0.0570 0.1055 0.4100 0.100 Uiso 1 1 calc R . .
H32B H 0.1846 0.1482 0.3472 0.100 Uiso 1 1 calc R . .
C3 C 0.2903(13) 0.5514(9) 0.4534(9) 0.106(4) Uani 1 1 d . . .
H3 H 0.3442 0.5112 0.4726 0.127 Uiso 1 1 calc R . .
C43 C 0.0277(11) -0.1201(9) 0.1352(8) 0.093(4) Uani 1 1 d . . .
H43A H 0.1046 -0.1466 0.1051 0.112 Uiso 1 1 calc R . .
H43B H 0.0039 -0.0751 0.0933 0.112 Uiso 1 1 calc R . .
C44 C -0.0721(14) -0.1994(9) 0.1733(11) 0.118(5) Uani 1 1 d . . .
H44A H -0.0768 -0.2322 0.1277 0.142 Uiso 1 1 calc R . .
H44B H -0.0484 -0.2443 0.2153 0.142 Uiso 1 1 calc R . .
C28 C 0.2971(17) 0.6249(10) 1.0198(11) 0.115(5) Uani 1 1 d . . .
C4 C 0.2217(15) 0.5193(10) 0.4093(10) 0.113(5) Uani 1 1 d . . .
H4 H 0.2259 0.4570 0.4005 0.136 Uiso 1 1 calc R . .
C31 C 0.0748(11) 0.1046(9) 0.2845(7) 0.090(4) Uani 1 1 d . . .
H31A H -0.0062 0.0734 0.3054 0.108 Uiso 1 1 calc R . .
H31B H 0.0756 0.1548 0.2376 0.108 Uiso 1 1 calc R . .
C33 C 0.0505(12) 0.2416(9) 0.3612(8) 0.110(4) Uani 1 1 d . . .
H33A H 0.0947 0.2838 0.3098 0.164 Uiso 1 1 calc R . .
H33B H 0.0625 0.2625 0.4103 0.164 Uiso 1 1 calc R . .
H33C H -0.0359 0.2410 0.3673 0.164 Uiso 1 1 calc R . .
C36 C 0.2358(12) 0.2242(9) 0.0052(8) 0.102(4) Uani 1 1 d . . .
H36A H 0.1489 0.2377 0.0188 0.122 Uiso 1 1 calc R . .
H36B H 0.2601 0.1991 -0.0484 0.122 Uiso 1 1 calc R . .
C37 C 0.3082(16) 0.3147(10) -0.0083(10) 0.144(6) Uani 1 1 d . . .
H37A H 0.3941 0.3019 -0.0199 0.217 Uiso 1 1 calc R . .
H37B H 0.2796 0.3432 0.0426 0.217 Uiso 1 1 calc R . .
H37C H 0.2971 0.3569 -0.0564 0.217 Uiso 1 1 calc R . .
C45 C -0.1923(17) -0.1656(11) 0.2143(11) 0.150(6) Uani 1 1 d . . .
H45A H -0.1906 -0.1393 0.2637 0.226 Uiso 1 1 calc R . .
H45B H -0.2522 -0.2169 0.2324 0.226 Uiso 1 1 calc R . .
H45C H -0.2140 -0.1180 0.1743 0.226 Uiso 1 1 calc R . .
C41 C 0.4564(13) -0.2611(11) 0.2196(9) 0.137(6) Uani 1 1 d . . .
H41A H 0.4415 -0.2451 0.2759 0.205 Uiso 1 1 calc R . .
H41B H 0.5415 -0.2760 0.1966 0.205 Uiso 1 1 calc R . .
H41C H 0.4048 -0.3146 0.2235 0.205 Uiso 1 1 calc R . .
N2 N 0.2924(7) 0.8482(5) 0.6937(5) 0.051(2) Uani 1 1 d . . .
H2A H 0.3341 0.8108 0.6606 0.061 Uiso 1 1 calc R . .
N4 N 0.1628(7) -0.0048(5) 0.1731(5) 0.056(2) Uani 1 1 d . . .
N1 N 0.2642(7) 0.8371(5) 0.4905(5) 0.060(2) Uani 1 1 d . . .
H1 H 0.3179 0.8007 0.5042 0.072 Uiso 1 1 calc R . .
N3 N 0.5588(7) 0.8984(5) 0.6978(5) 0.054(2) Uani 1 1 d . . .
H3A H 0.5835 0.8553 0.6665 0.065 Uiso 1 1 calc R . .
O2 O 0.1455(6) 0.8645(5) 0.8178(4) 0.0621(19) Uani 1 1 d . . .
O3 O 0.4836(6) 0.9333(5) 0.8314(4) 0.066(2) Uani 1 1 d . . .
O1 O 0.1209(6) 0.8557(5) 0.4231(4) 0.066(2) Uani 1 1 d . . .
F9 F 0.0003(12) 0.4763(9) 0.3665(8) 0.219(6) Uani 1 1 d . C .
O5 O 0.4475(7) 0.7542(4) 0.5677(4) 0.0644(19) Uani 1 1 d . . .
O4 O 0.6378(6) 0.7873(5) 0.5654(4) 0.073(2) Uani 1 1 d . . .
C46 C 0.5611(13) 0.7580(7) 0.5331(7) 0.061(3) Uani 1 1 d . . .
C47 C 0.6122(11) 0.7285(10) 0.4470(8) 0.118(5) Uani 1 1 d . . .
H47A H 0.5619 0.6774 0.4436 0.177 Uiso 1 1 calc R . .
H47B H 0.6949 0.7083 0.4392 0.177 Uiso 1 1 calc R . .
H47C H 0.6125 0.7807 0.4027 0.177 Uiso 1 1 calc R . .
O6 O 0.8621(8) 0.8726(6) 0.4257(5) 0.097(3) Uani 1 1 d . . .
O7 O 0.2374(16) 0.9558(8) 0.9320(6) 0.114(4) Uani 1 1 d . . .
C54A C 0.0519(15) 0.5783(13) 0.8753(10) 0.132(6) Uani 1 1 d . . .
H54A H -0.0194 0.5564 0.9201 0.158 Uiso 1 1 calc R . .
C55A C 0.0807(12) 0.6741(10) 0.8550(8) 0.099(4) Uani 1 1 d . . .
H55A H 0.0298 0.7157 0.8863 0.118 Uiso 1 1 calc R . .
C53A C 0.1218(17) 0.5178(11) 0.8335(12) 0.121(6) Uani 1 1 d . A .
H53A H 0.1025 0.4535 0.8469 0.145 Uiso 1 1 calc R . .
C52A C 0.2252(17) 0.5548(12) 0.7688(11) 0.095(7) Uani 1 1 d . . .
C48B C 0.0638(17) 0.5454(14) 0.3284(12) 0.128(5) Uiso 1 1 d . . .
H51A H 0.934(10) 0.880(7) 0.439(6) 0.09(4) Uiso 1 1 d . . .
H52 H 0.309(15) 0.948(11) 0.905(11) 0.16(9) Uiso 1 1 d . . .
H53 H 0.192(14) 0.939(11) 0.902(10) 0.16(8) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
F12A C58B 1.90(6) . ?
F14A C58B 1.73(6) . ?
F13B C58B 1.80(5) . ?
C58B C52A 0.79(5) . ?
F5B C28 1.343(18) . ?
F4B C28 1.417(18) . ?
F6A C28 1.312(17) . ?
F8B C48B 1.29(2) . ?
F7B C48B 1.47(2) . ?
F12B C58A 1.31(2) . ?
F13A C58A 1.24(2) . ?
F14B C58A 1.35(2) . ?
C58A C52A 1.68(2) . ?
F8A C48B 1.38(2) . ?
F7A C48B 1.30(2) . ?
F5A C28 1.30(2) . ?
F4A C28 1.29(2) . ?
F6B C28 1.36(2) . ?
C11 C12 1.388(12) . ?
C11 C8 1.396(12) . ?
C11 C10 1.533(12) . ?
C22 C23 1.372(13) . ?
C22 C27 1.398(13) . ?
C22 C21 1.488(13) . ?
C15 C16 1.334(13) . ?
C15 C55A 1.377(14) . ?
C15 C14 1.515(13) . ?
C9 N1 1.469(11) . ?
C9 C8 1.522(12) . ?
C27 C26 1.375(14) . ?
C12 C8 1.400(12) 2_676 ?
C12 C13 1.514(11) . ?
C30 C31 1.490(12) . ?
C30 N4 1.526(11) . ?
C8 C12 1.400(12) 2_676 ?
C10 N2 1.451(10) . ?
C14 O2 1.238(10) . ?
C14 N2 1.334(11) . ?
C13 N3 1.463(11) . ?
C34 C35 1.506(13) . ?
C34 N4 1.510(12) . ?
C16 C52A 1.363(17) . ?
C38 C39 1.499(13) . ?
C38 N4 1.522(11) . ?
C26 C25 1.357(14) . ?
C26 C28 1.486(18) . ?
C1 C2 1.377(14) . ?
C1 C6 1.380(13) . ?
C1 C7 1.497(14) . ?
C23 C24 1.371(15) . ?
C21 O3 1.237(11) . ?
C21 N3 1.336(11) . ?
C6 C5 1.386(15) . ?
C35 C36 1.499(14) . ?
C5 C4 1.376(16) . ?
C5 C48B 1.559(19) . ?
C2 C3 1.375(15) . ?
C42 C43 1.481(13) . ?
C42 N4 1.526(12) . ?
C40 C41 1.488(15) . ?
C40 C39 1.512(14) . ?
C7 O1 1.228(11) . ?
C7 N1 1.344(11) . ?
C25 C24 1.370(15) . ?
C32 C33 1.468(14) . ?
C32 C31 1.495(13) . ?
C3 C4 1.358(16) . ?
C43 C44 1.537(16) . ?
C44 C45 1.443(18) . ?
C36 C37 1.503(17) . ?
F9 C48B 1.203(18) . ?
O5 C46 1.241(12) . ?
O4 C46 1.271(11) . ?
C46 C47 1.489(14) . ?
C54A C53A 1.303(18) . ?
C54A C55A 1.386(17) . ?
C53A C52A 1.367(18) . ?

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
C52A C58B F14A 149(5) . . ?
C52A C58B F13B 137(4) . . ?
F14A C58B F13B 71(3) . . ?
C52A C58B F12A 128(4) . . ?
F14A C58B F12A 68(2) . . ?
F13B C58B F12A 67(2) . . ?
F13A C58A F12B 111.3(19) . . ?
F13A C58A F14B 111.3(18) . . ?
F12B C58A F14B 110.0(17) . . ?
F13A C58A C52A 116.2(16) . . ?
F12B C58A C52A 103.0(16) . . ?
F14B C58A C52A 104.5(16) . . ?
C12 C11 C8 121.1(8) . . ?
C12 C11 C10 120.2(9) . . ?
C8 C11 C10 118.7(9) . . ?
C23 C22 C27 118.1(10) . . ?
C23 C22 C21 124.7(11) . . ?
C27 C22 C21 117.2(11) . . ?
C16 C15 C55A 120.5(10) . . ?
C16 C15 C14 123.5(10) . . ?
C55A C15 C14 116.0(11) . . ?
N1 C9 C8 110.6(7) . . ?
C26 C27 C22 118.9(10) . . ?
C11 C12 C8 119.6(8) . 2_676 ?
C11 C12 C13 119.3(9) . . ?
C8 C12 C13 121.0(9) 2_676 . ?
C31 C30 N4 117.1(8) . . ?
C11 C8 C12 119.3(8) . 2_676 ?
C11 C8 C9 121.7(9) . . ?
C12 C8 C9 118.9(9) 2_676 . ?
N2 C10 C11 111.9(7) . . ?
O2 C14 N2 122.2(9) . . ?
O2 C14 C15 120.9(10) . . ?
N2 C14 C15 116.9(10) . . ?
N3 C13 C12 109.3(7) . . ?
C35 C34 N4 115.7(8) . . ?
C15 C16 C52A 116.0(12) . . ?
C39 C38 N4 117.1(8) . . ?
C25 C26 C27 122.3(11) . . ?
C25 C26 C28 121.2(13) . . ?
C27 C26 C28 116.5(13) . . ?
C2 C1 C6 119.4(10) . . ?
C2 C1 C7 124.9(11) . . ?
C6 C1 C7 115.7(11) . . ?
C24 C23 C22 122.0(11) . . ?
O3 C21 N3 121.5(9) . . ?
O3 C21 C22 121.2(10) . . ?
N3 C21 C22 117.2(11) . . ?
C1 C6 C5 119.8(11) . . ?
C36 C35 C34 111.8(10) . . ?
C4 C5 C6 120.2(11) . . ?
C4 C5 C48B 120.9(14) . . ?
C6 C5 C48B 118.8(14) . . ?
C3 C2 C1 119.9(11) . . ?
C43 C42 N4 117.0(9) . . ?
C41 C40 C39 113.6(10) . . ?
O1 C7 N1 121.5(10) . . ?
O1 C7 C1 122.5(10) . . ?
N1 C7 C1 116.0(10) . . ?
C26 C25 C24 119.0(11) . . ?
C38 C39 C40 111.0(9) . . ?
C25 C24 C23 119.7(12) . . ?
C33 C32 C31 113.8(10) . . ?
C4 C3 C2 121.2(12) . . ?
C42 C43 C44 113.1(10) . . ?
C45 C44 C43 112.9(12) . . ?
F4A C28 F5A 101.9(17) . . ?
F4A C28 F6A 51.0(12) . . ?
F5A C28 F6A 125.9(17) . . ?
F4A C28 F5B 130.2(19) . . ?
F5A C28 F5B 49.6(10) . . ?
F6A C28 F5B 108.0(16) . . ?
F4A C28 F6B 94.5(18) . . ?
F5A C28 F6B 108.6(18) . . ?
F6A C28 F6B 46.2(10) . . ?
F5B C28 F6B 67.2(14) . . ?
F4A C28 F4B 51.2(13) . . ?
F5A C28 F4B 60.1(10) . . ?
F6A C28 F4B 100.4(13) . . ?
F5B C28 F4B 108.1(13) . . ?
F6B C28 F4B 133.1(17) . . ?
F4A C28 C26 117.0(17) . . ?
F5A C28 C26 116.1(14) . . ?
F6A C28 C26 118.0(13) . . ?
F5B C28 C26 112.5(13) . . ?
F6B C28 C26 116.0(14) . . ?
F4B C28 C26 108.8(13) . . ?
C3 C4 C5 119.4(12) . . ?
C30 C31 C32 112.6(9) . . ?
C35 C36 C37 114.2(12) . . ?
C14 N2 C10 119.8(8) . . ?
C34 N4 C38 108.1(7) . . ?
C34 N4 C30 111.4(7) . . ?
C38 N4 C30 108.1(7) . . ?
C34 N4 C42 109.2(7) . . ?
C38 N4 C42 111.8(7) . . ?
C30 N4 C42 108.3(7) . . ?
C7 N1 C9 122.6(8) . . ?
C21 N3 C13 121.8(8) . . ?
O5 C46 O4 124.3(10) . . ?
O5 C46 C47 118.5(10) . . ?
O4 C46 C47 117.2(11) . . ?
C53A C54A C55A 121.9(14) . . ?
C15 C55A C54A 119.5(12) . . ?
C54A C53A C52A 115.8(15) . . ?
C58B C52A C16 123(4) . . ?
C58B C52A C53A 111(4) . . ?
C16 C52A C53A 126.1(15) . . ?
C58B C52A C58A 10(3) . . ?
C16 C52A C58A 113.8(15) . . ?
C53A C52A C58A 120.1(16) . . ?
F9 C48B F8B 129.7(18) . . ?
F9 C48B F7A 133(2) . . ?
F8B C48B F7A 42.3(13) . . ?
F9 C48B F8A 84.9(15) . . ?
F8B C48B F8A 61.1(12) . . ?
F7A C48B F8A 102.5(19) . . ?
F9 C48B F7B 89.2(15) . . ?
F8B C48B F7B 99.1(15) . . ?
F7A C48B F7B 58.7(14) . . ?
F8A C48B F7B 145.8(16) . . ?
F9 C48B C5 114.0(16) . . ?
F8B C48B C5 112.2(16) . . ?
F7A C48B C5 107.0(18) . . ?
F8A C48B C5 110.2(15) . . ?
F7B C48B C5 103.0(13) . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        19.71
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.055
####################################################################### 
# 
# 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_Complex1
_database_code_depnum_ccdc_archive 'CCDC 996873'
_audit_update_record             
;
2015-02-12 deposited with the CCDC.
2015-05-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C86 H118 Cl2 N14 O20'
_chemical_formula_weight         1738.84

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   P2(1)/c

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                   11.195(2)
_cell_length_b                   15.809(3)
_cell_length_c                   25.390(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.337(5)
_cell_angle_gamma                90.00
_cell_volume                     4480.7(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2731
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      16.69

_exptl_crystal_description       Plate
_exptl_crystal_colour            Block
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1852
_exptl_absorpt_coefficient_mu    0.149
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9852
_exptl_absorpt_correction_T_max  0.9911
_exptl_absorpt_process_details   Sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20946
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_av_UnetI/netI     0.0406
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         17.08
_reflns_number_total             2639
_reflns_number_gt                2048
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep 3v.2'
_computing_publication_material  'Mercury 3.1'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0895P)²+9.0711P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2639
_refine_ls_number_parameters     554
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0570
_refine_ls_wR_factor_ref         0.1660
_refine_ls_wR_factor_gt          0.1485
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_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 0.9754(11) 0.5805(5) -0.0214(5) 0.031(2) Uani 1 1 d . . .
Cl1 Cl 0.18996(16) 0.67113(12) 0.07105(7) 0.0542(7) Uani 1 1 d . . .
C2 C 0.9455(6) 0.6664(5) -0.0457(3) 0.038(2) Uani 1 1 d . . .
H2A H 0.9815 0.6710 -0.0792 0.046 Uiso 1 1 calc R . .
H2B H 0.8594 0.6712 -0.0526 0.046 Uiso 1 1 calc R . .
O2 O 0.319(2) 0.9062(17) 0.2771(8) 0.465(14) Uani 1 1 d . . .
N3 N 0.9886(5) 0.7352(5) -0.0112(2) 0.0419(17) Uani 1 1 d . . .
H3 H 1.0559 0.7288 0.0070 0.050 Uiso 1 1 calc R . .
C4 C 0.9290(10) 0.8081(7) -0.0064(4) 0.048(2) Uani 1 1 d . . .
O5 O 0.8312(6) 0.8220(3) -0.0297(2) 0.0687(19) Uani 1 1 d . . .
C6 C 0.9924(11) 0.8713(6) 0.0294(4) 0.039(2) Uani 1 1 d . . .
C7 C 1.1109(12) 0.8911(6) 0.0240(3) 0.051(2) Uani 1 1 d . . .
H7 H 1.1543 0.8606 0.0007 0.062 Uiso 1 1 calc R . .
C8 C 1.1665(8) 0.9572(8) 0.0536(5) 0.061(3) Uani 1 1 d . . .
H8 H 1.2462 0.9705 0.0496 0.073 Uiso 1 1 calc R . .
C9 C 1.1033(14) 1.0023(5) 0.0885(4) 0.058(3) Uani 1 1 d . . .
H9 H 1.1408 1.0456 0.1083 0.069 Uiso 1 1 calc R . .
C10 C 0.9857(13) 0.9838(7) 0.0943(3) 0.055(2) Uani 1 1 d . . .
H10 H 0.9425 1.0139 0.1179 0.065 Uiso 1 1 calc R . .
C11 C 0.9330(10) 0.9197(7) 0.0643(5) 0.046(2) Uani 1 1 d . . .
N12 N 0.8083(9) 0.9008(7) 0.0720(3) 0.066(2) Uani 1 1 d . . .
O13 O 0.7378(6) 0.9603(5) 0.0697(3) 0.099(3) Uani 1 1 d . . .
O14 O 0.7789(6) 0.8280(5) 0.0815(3) 0.082(2) Uani 1 1 d . . .
C15 C 0.9147(6) 0.5503(8) 0.0207(5) 0.032(2) Uani 1 1 d . . .
C16 C 0.8347(6) 0.6103(5) 0.0481(3) 0.040(2) Uani 1 1 d . . .
H16A H 0.8122 0.6575 0.0250 0.047 Uiso 1 1 calc R . .
H16B H 0.7623 0.5813 0.0566 0.047 Uiso 1 1 calc R . .
N17 N 0.8984(5) 0.6412(4) 0.0961(3) 0.0438(18) Uani 1 1 d . . .
H17 H 0.9746 0.6484 0.0964 0.053 Uiso 1 1 calc R . .
C18 C 0.8434(11) 0.6590(5) 0.1403(4) 0.047(2) Uani 1 1 d . . .
O19 O 0.7363(6) 0.6548(4) 0.1435(2) 0.073(2) Uani 1 1 d . . .
C20 C 0.9285(9) 0.6923(9) 0.1836(5) 0.058(3) Uani 1 1 d . . .
C21 C 0.9959(10) 0.7644(9) 0.1792(4) 0.063(3) Uani 1 1 d . . .
H21 H 0.9957 0.7915 0.1467 0.076 Uiso 1 1 calc R . .
C22 C 1.0645(9) 0.7977(7) 0.2225(7) 0.081(3) Uani 1 1 d . . .
H22 H 1.1084 0.8470 0.2187 0.097 Uiso 1 1 calc R . .
C23 C 1.0673(10) 0.7572(12) 0.2711(6) 0.084(4) Uani 1 1 d . . .
H23 H 1.1140 0.7792 0.2997 0.101 Uiso 1 1 calc R . .
C24 C 1.0028(14) 0.6864(11) 0.2771(5) 0.086(3) Uani 1 1 d . . .
H24 H 1.0035 0.6593 0.3096 0.103 Uiso 1 1 calc R . .
C25 C 0.9358(10) 0.6554(8) 0.2335(7) 0.067(3) Uani 1 1 d . . .
N26 N 0.8759(9) 0.5730(8) 0.2427(4) 0.085(3) Uani 1 1 d . . .
O27 O 0.8449(8) 0.5555(5) 0.2861(4) 0.123(3) Uani 1 1 d . . .
O28 O 0.8599(6) 0.5248(5) 0.2059(3) 0.099(2) Uani 1 1 d . . .
C29 C 0.9384(9) 0.4708(9) 0.0421(3) 0.035(2) Uani 1 1 d . . .
C30 C 0.8610(7) 0.4357(5) 0.0827(3) 0.047(2) Uani 1 1 d . . .
H30A H 0.9107 0.4110 0.1117 0.057 Uiso 1 1 calc R . .
H30B H 0.8133 0.4804 0.0967 0.057 Uiso 1 1 calc R . .
N31 N 0.7829(6) 0.3711(5) 0.0573(3) 0.0421(18) Uani 1 1 d . . .
H31 H 0.7750 0.3686 0.0234 0.051 Uiso 1 1 calc R . .
C32 C 0.7236(8) 0.3161(6) 0.0855(5) 0.040(2) Uani 1 1 d . . .
O33 O 0.7261(4) 0.3176(3) 0.1342(3) 0.0507(16) Uani 1 1 d . . .
C34 C 0.6448(8) 0.2542(8) 0.0542(4) 0.038(2) Uani 1 1 d . . .
C35 C 0.5630(11) 0.2790(6) 0.0134(4) 0.052(2) Uani 1 1 d . . .
H35 H 0.5650 0.3343 0.0009 0.063 Uiso 1 1 calc R . .
C36 C 0.4792(9) 0.2239(9) -0.0091(4) 0.063(3) Uani 1 1 d . . .
H36 H 0.4247 0.2418 -0.0363 0.076 Uiso 1 1 calc R . .
C37 C 0.4767(9) 0.1411(8) 0.0092(5) 0.065(3) Uani 1 1 d . . .
H37 H 0.4200 0.1035 -0.0057 0.078 Uiso 1 1 calc R . .
C38 C 0.5566(12) 0.1149(6) 0.0487(5) 0.055(2) Uani 1 1 d . . .
H38 H 0.5555 0.0593 0.0606 0.066 Uiso 1 1 calc R . .
C39 C 0.6387(9) 0.1710(9) 0.0708(4) 0.040(2) Uani 1 1 d . . .
N40 N 0.7311(9) 0.1398(5) 0.1107(3) 0.049(2) Uani 1 1 d . . .
O41 O 0.8350(6) 0.1601(3) 0.1069(2) 0.0550(17) Uani 1 1 d . . .
O42 O 0.6977(6) 0.0933(4) 0.1451(3) 0.071(2) Uani 1 1 d . . .
N43 N 0.4299(6) 0.6395(4) 0.2032(3) 0.0444(17) Uani 1 1 d . . .
C44 C 0.4571(8) 0.6022(6) 0.1503(4) 0.068(3) Uani 1 1 d . . .
H44A H 0.3844 0.6050 0.1271 0.081 Uiso 1 1 calc R . .
H44B H 0.5156 0.6385 0.1353 0.081 Uiso 1 1 calc R . .
C45 C 0.5018(8) 0.5158(6) 0.1492(4) 0.087(3) Uani 1 1 d . . .
H45A H 0.4496 0.4785 0.1672 0.105 Uiso 1 1 calc R . .
H45B H 0.5814 0.5128 0.1671 0.105 Uiso 1 1 calc R . .
C46 C 0.5061(8) 0.4872(6) 0.0900(4) 0.098(3) Uani 1 1 d . . .
H46A H 0.5488 0.5303 0.0717 0.117 Uiso 1 1 calc R . .
H46B H 0.5533 0.4358 0.0896 0.117 Uiso 1 1 calc R . .
C47 C 0.3896(8) 0.4712(6) 0.0587(4) 0.100(4) Uani 1 1 d . . .
H47A H 0.3451 0.4291 0.0762 0.150 Uiso 1 1 calc R . .
H47B H 0.4049 0.4515 0.0240 0.150 Uiso 1 1 calc R . .
H47C H 0.3442 0.5227 0.0557 0.150 Uiso 1 1 calc R . .
C48 C 0.3445(7) 0.5817(6) 0.2307(3) 0.060(3) Uani 1 1 d . . .
H48A H 0.3891 0.5314 0.2419 0.072 Uiso 1 1 calc R . .
H48B H 0.3238 0.6105 0.2625 0.072 Uiso 1 1 calc R . .
C49 C 0.2313(8) 0.5534(6) 0.2023(4) 0.084(3) Uani 1 1 d . . .
H49A H 0.2481 0.5300 0.1683 0.101 Uiso 1 1 calc R . .
H49B H 0.1784 0.6016 0.1960 0.101 Uiso 1 1 calc R . .
C50 C 0.1686(9) 0.4862(7) 0.2343(4) 0.101(4) Uani 1 1 d . . .
H50A H 0.1503 0.5117 0.2674 0.121 Uiso 1 1 calc R . .
H50B H 0.0927 0.4727 0.2151 0.121 Uiso 1 1 calc R . .
C51 C 0.2288(11) 0.4096(9) 0.2460(6) 0.174(6) Uani 1 1 d . . .
H51A H 0.2313 0.3767 0.2143 0.261 Uiso 1 1 calc R . .
H51B H 0.1872 0.3785 0.2714 0.261 Uiso 1 1 calc R . .
H51C H 0.3090 0.4213 0.2602 0.261 Uiso 1 1 calc R . .
C52 C 0.3673(7) 0.7239(6) 0.1921(3) 0.062(3) Uani 1 1 d . . .
H52A H 0.2963 0.7139 0.1687 0.074 Uiso 1 1 calc R . .
H52B H 0.3410 0.7455 0.2251 0.074 Uiso 1 1 calc R . .
C53 C 0.4405(8) 0.7906(7) 0.1682(4) 0.083(3) Uani 1 1 d . . .
H53A H 0.4595 0.7726 0.1333 0.100 Uiso 1 1 calc R . .
H53B H 0.5152 0.7978 0.1897 0.100 Uiso 1 1 calc R . .
C54 C 0.3730(10) 0.8760(7) 0.1640(5) 0.114(4) Uani 1 1 d . . .
H54A H 0.2985 0.8683 0.1424 0.137 Uiso 1 1 calc R . .
H54B H 0.3532 0.8931 0.1989 0.137 Uiso 1 1 calc R . .
C55 C 0.4412(9) 0.9430(7) 0.1412(5) 0.121(4) Uani 1 1 d . . .
H55A H 0.5136 0.9528 0.1632 0.182 Uiso 1 1 calc R . .
H55B H 0.3943 0.9939 0.1390 0.182 Uiso 1 1 calc R . .
H55C H 0.4609 0.9267 0.1065 0.182 Uiso 1 1 calc R . .
C56 C 0.5435(6) 0.6504(5) 0.2382(3) 0.050(2) Uani 1 1 d . . .
H56A H 0.6029 0.6767 0.2176 0.060 Uiso 1 1 calc R . .
H56B H 0.5734 0.5948 0.2485 0.060 Uiso 1 1 calc R . .
C57 C 0.5331(7) 0.7023(6) 0.2876(3) 0.064(3) Uani 1 1 d . . .
H57A H 0.5098 0.7596 0.2779 0.077 Uiso 1 1 calc R . .
H57B H 0.4712 0.6784 0.3078 0.077 Uiso 1 1 calc R . .
C58 C 0.6489(8) 0.7042(6) 0.3210(4) 0.082(3) Uani 1 1 d . . .
H58A H 0.7120 0.7239 0.2999 0.099 Uiso 1 1 calc R . .
H58B H 0.6692 0.6473 0.3329 0.099 Uiso 1 1 calc R . .
C59 C 0.6426(8) 0.7608(7) 0.3681(4) 0.104(4) Uani 1 1 d . . .
H59A H 0.6315 0.8182 0.3566 0.156 Uiso 1 1 calc R . .
H59B H 0.7158 0.7563 0.3902 0.156 Uiso 1 1 calc R . .
H59C H 0.5766 0.7440 0.3877 0.156 Uiso 1 1 calc R . .


_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 C15 1.394(10) . ?
C1 C29 1.394(11) 3_765 ?
C1 C2 1.517(9) . ?
C2 N3 1.456(8) . ?
N3 C4 1.343(9) . ?
C4 O5 1.223(9) . ?
C4 C6 1.493(11) . ?
C6 C11 1.380(10) . ?
C6 C7 1.380(10) . ?
C7 C8 1.404(10) . ?
C8 C9 1.373(11) . ?
C9 C10 1.367(11) . ?
C10 C11 1.373(10) . ?
C11 N12 1.455(11) . ?
N12 O14 1.226(9) . ?
N12 O13 1.226(8) . ?
C15 C29 1.387(10) . ?
C15 C16 1.511(9) . ?
C16 N17 1.448(8) . ?
N17 C18 1.350(10) . ?
C18 O19 1.209(10) . ?
C18 C20 1.496(13) . ?
C20 C21 1.376(11) . ?
C20 C25 1.392(13) . ?
C21 C22 1.394(12) . ?
C22 C23 1.388(13) . ?
C23 C24 1.347(13) . ?
C24 C25 1.378(14) . ?
C25 N26 1.491(13) . ?
N26 O28 1.208(9) . ?
N26 O27 1.211(10) . ?
C29 C1 1.394(11) 3_765 ?
C29 C30 1.502(9) . ?
C30 N31 1.462(9) . ?
N31 C32 1.334(10) . ?
C32 O33 1.237(9) . ?
C32 C34 1.504(11) . ?
C34 C39 1.385(10) . ?
C34 C35 1.387(10) . ?
C35 C36 1.372(10) . ?
C36 C37 1.390(11) . ?
C37 C38 1.357(11) . ?
C38 C39 1.366(10) . ?
C39 N40 1.475(11) . ?
N40 O41 1.218(8) . ?
N40 O42 1.223(8) . ?
N43 C56 1.505(9) . ?
N43 C44 1.518(10) . ?
N43 C52 1.523(9) . ?
N43 C48 1.529(9) . ?
C44 C45 1.455(11) . ?
C45 C46 1.573(12) . ?
C46 C47 1.496(11) . ?
C48 C49 1.479(10) . ?
C49 C50 1.539(12) . ?
C50 C51 1.407(13) . ?
C52 C53 1.493(11) . ?
C53 C54 1.547(12) . ?
C54 C55 1.450(12) . ?
C56 C57 1.511(10) . ?
C57 C58 1.495(10) . ?
C58 C59 1.499(11) . ?

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
C15 C1 C29 118.7(8) . 3_765 ?
C15 C1 C2 120.9(13) . . ?
C29 C1 C2 120.4(13) 3_765 . ?
N3 C2 C1 111.8(6) . . ?
C4 N3 C2 123.5(7) . . ?
O5 C4 N3 122.9(8) . . ?
O5 C4 C6 122.7(9) . . ?
N3 C4 C6 114.4(9) . . ?
C11 C6 C7 116.8(8) . . ?
C11 C6 C4 122.2(11) . . ?
C7 C6 C4 120.6(11) . . ?
C6 C7 C8 120.4(8) . . ?
C9 C8 C7 120.2(8) . . ?
C10 C9 C8 120.3(8) . . ?
C9 C10 C11 118.4(8) . . ?
C10 C11 C6 123.9(9) . . ?
C10 C11 N12 117.0(13) . . ?
C6 C11 N12 119.0(11) . . ?
O14 N12 O13 123.3(10) . . ?
O14 N12 C11 119.5(8) . . ?
O13 N12 C11 117.2(10) . . ?
C29 C15 C1 121.5(7) . . ?
C29 C15 C16 119.3(13) . . ?
C1 C15 C16 118.6(13) . . ?
N17 C16 C15 109.2(6) . . ?
C18 N17 C16 122.9(7) . . ?
O19 C18 N17 124.2(9) . . ?
O19 C18 C20 123.2(10) . . ?
N17 C18 C20 112.4(10) . . ?
C21 C20 C25 115.2(10) . . ?
C21 C20 C18 123.7(12) . . ?
C25 C20 C18 120.9(13) . . ?
C20 C21 C22 121.5(10) . . ?
C23 C22 C21 119.9(11) . . ?
C24 C23 C22 120.5(11) . . ?
C23 C24 C25 118.0(12) . . ?
C24 C25 C20 124.9(12) . . ?
C24 C25 N26 114.2(16) . . ?
C20 C25 N26 120.8(13) . . ?
O28 N26 O27 121.5(13) . . ?
O28 N26 C25 118.2(11) . . ?
O27 N26 C25 120.3(12) . . ?
C15 C29 C1 119.8(8) . 3_765 ?
C15 C29 C30 120.1(13) . . ?
C1 C29 C30 119.6(12) 3_765 . ?
N31 C30 C29 108.1(7) . . ?
C32 N31 C30 121.6(7) . . ?
O33 C32 N31 123.3(8) . . ?
O33 C32 C34 120.6(10) . . ?
N31 C32 C34 116.0(10) . . ?
C39 C34 C35 116.9(8) . . ?
C39 C34 C32 119.9(11) . . ?
C35 C34 C32 122.5(11) . . ?
C36 C35 C34 121.5(8) . . ?
C35 C36 C37 119.3(8) . . ?
C38 C37 C36 120.4(8) . . ?
C37 C38 C39 119.4(8) . . ?
C38 C39 C34 122.6(9) . . ?
C38 C39 N40 118.7(12) . . ?
C34 C39 N40 118.5(11) . . ?
O41 N40 O42 124.0(9) . . ?
O41 N40 C39 118.9(8) . . ?
O42 N40 C39 117.1(9) . . ?
C56 N43 C44 110.4(6) . . ?
C56 N43 C52 111.4(6) . . ?
C44 N43 C52 107.3(6) . . ?
C56 N43 C48 109.2(6) . . ?
C44 N43 C48 110.3(6) . . ?
C52 N43 C48 108.2(6) . . ?
C45 C44 N43 118.4(8) . . ?
C44 C45 C46 108.9(8) . . ?
C47 C46 C45 117.9(8) . . ?
C49 C48 N43 120.0(7) . . ?
C48 C49 C50 111.1(8) . . ?
C51 C50 C49 118.4(9) . . ?
C53 C52 N43 115.8(7) . . ?
C52 C53 C54 111.4(8) . . ?
C55 C54 C53 113.4(9) . . ?
N43 C56 C57 115.9(6) . . ?
C58 C57 C56 111.4(7) . . ?
C57 C58 C59 112.0(8) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        17.08
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.049
