# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# 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_macrocycle
_database_code_depnum_ccdc_archive 'CCDC 1416976'
_audit_update_record             
;
2015-08-05 deposited with the CCDC.
2015-09-15 downloaded from the CCDC.
;
_audit_creation_date             2014-06-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C28 H30 N2 O5'
_chemical_formula_sum            'C28 H30 N2 O5'
_chemical_formula_weight         474.54
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C28 H30 N2 O5'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, -y, z'

_cell_length_a                   10.6388(3)
_cell_length_b                   9.0437(3)
_cell_length_c                   24.8594(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2391.83(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3389
_cell_measurement_temperature    99.97(10)
_cell_measurement_theta_max      72.9510
_cell_measurement_theta_min      6.0240
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.736
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.943
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33t (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:01:44)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.1335
_exptl_crystal_size_mid          0.0844
_exptl_crystal_size_min          0.0826
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            5120
_diffrn_reflns_point_group_measured_fraction_full 0.721
_diffrn_reflns_point_group_measured_fraction_max 0.687
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.110
_diffrn_reflns_theta_min         6.051
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2299
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.1368958000
_diffrn_orient_matrix_UB_12      0.0563675000
_diffrn_orient_matrix_UB_13      -0.0010249000
_diffrn_orient_matrix_UB_21      -0.0214819000
_diffrn_orient_matrix_UB_22      -0.0798366000
_diffrn_orient_matrix_UB_23      -0.0540014000
_diffrn_orient_matrix_UB_31      -0.0423392000
_diffrn_orient_matrix_UB_32      -0.1395727000
_diffrn_orient_matrix_UB_33      0.0302801000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.398
_reflns_Friedel_fraction_full    0.437
_reflns_Friedel_fraction_max     0.401
_reflns_number_gt                3207
_reflns_number_total             3287
_reflns_odcompleteness_completeness 98.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33t (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:01:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33t (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:01:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33t (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:01:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.206
_refine_diff_density_min         -0.146
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details 
;
 Flack x determined using 895 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.08(13)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         3287
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0288
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0319P)²+0.4787P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0720
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C3(H3A,H3B), C5(H5A,H5B), C12(H12A,H12B), C15(H15A,H15B),
 C26(H26A,H26B), C22(H22A,H22B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C33(H33), C17(H17), C31(H31), C21(H21), C32(H32),
 C14(H14), C18(H18), C20(H20), C13(H13), C35(H35)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O4 O 0.44075(15) 0.38059(18) 0.08542(7) 0.0259(4) Uani 1 1 d . . . . .
O7 O 0.30174(14) 0.12001(17) 0.07340(6) 0.0228(3) Uani 1 1 d . . . . .
O1 O 0.22896(14) -0.16728(16) 0.12311(7) 0.0237(3) Uani 1 1 d . . . . .
O29 O 0.75860(16) 0.58621(18) 0.37259(8) 0.0311(4) Uani 1 1 d . . . . .
C8 C 0.5535(2) 0.5179(2) 0.15190(10) 0.0222(5) Uani 1 1 d . . . . .
C6 C 0.5526(2) 0.4602(3) 0.09520(10) 0.0247(5) Uani 1 1 d . . . . .
H6A H 0.5588 0.5422 0.0702 0.030 Uiso 1 1 calc R . . . .
H6B H 0.6246 0.3962 0.0896 0.030 Uiso 1 1 calc R . . . .
O25 O 0.45640(15) -0.06091(18) 0.44410(7) 0.0279(4) Uani 1 1 d . . . . .
C3 C 0.4467(2) 0.2957(3) 0.03751(9) 0.0236(5) Uani 1 1 d . . . . .
H3A H 0.5134 0.2229 0.0401 0.028 Uiso 1 1 calc R . . . .
H3B H 0.4640 0.3594 0.0070 0.028 Uiso 1 1 calc R . . . .
C10 C 0.4714(2) 0.4635(2) 0.19077(10) 0.0241(5) Uani 1 1 d . . . . .
H10 H 0.4150 0.3890 0.1818 0.029 Uiso 1 1 calc R . . . .
N27 N 0.5480(2) 0.5900(2) 0.35594(8) 0.0252(4) Uani 1 1 d . . . . .
C19 C 0.27716(19) -0.0428(2) 0.31953(9) 0.0200(4) Uani 1 1 d . . . . .
C11 C 0.6388(2) 0.6270(3) 0.16652(11) 0.0258(5) Uani 1 1 d . . . . .
H11 H 0.6953 0.6633 0.1412 0.031 Uiso 1 1 calc R . . . .
C24 C 0.43165(19) 0.0665(2) 0.43090(9) 0.0205(4) Uani 1 1 d . . . . .
C16 C 0.32149(19) -0.1119(2) 0.21071(10) 0.0215(4) Uani 1 1 d . . . . .
C5 C 0.3224(2) 0.2197(3) 0.03008(9) 0.0243(5) Uani 1 1 d . . . . .
H5A H 0.2555 0.2926 0.0290 0.029 Uiso 1 1 calc R . . . .
H5B H 0.3220 0.1661 -0.0037 0.029 Uiso 1 1 calc R . . . .
N23 N 0.33006(17) 0.1034(2) 0.40168(8) 0.0206(4) Uani 1 1 d . . . . .
C2 C 0.5570(2) 0.6304(2) 0.25711(10) 0.0234(5) Uani 1 1 d . . . . .
C34 C 0.6281(2) 0.4153(2) 0.42024(10) 0.0213(4) Uani 1 1 d . . . . .
C33 C 0.7056(2) 0.4011(3) 0.46505(10) 0.0263(5) Uani 1 1 d . . . . .
H33 H 0.7703 0.4684 0.4708 0.032 Uiso 1 1 calc R . . . .
C17 C 0.3846(2) 0.0029(2) 0.23548(9) 0.0216(4) Uani 1 1 d . . . . .
H17 H 0.4421 0.0583 0.2158 0.026 Uiso 1 1 calc R . . . .
C12 C 0.1543(2) -0.0370(3) 0.11966(9) 0.0239(5) Uani 1 1 d . . . . .
H12A H 0.1694 0.0232 0.1513 0.029 Uiso 1 1 calc R . . . .
H12B H 0.0663 -0.0650 0.1198 0.029 Uiso 1 1 calc R . . . .
C31 C 0.5945(2) 0.1797(3) 0.49093(9) 0.0235(5) Uani 1 1 d . . . . .
H31 H 0.5845 0.1004 0.5144 0.028 Uiso 1 1 calc R . . . .
C21 C 0.2358(2) -0.1944(3) 0.24131(10) 0.0259(5) Uani 1 1 d . . . . .
H21 H 0.1932 -0.2732 0.2256 0.031 Uiso 1 1 calc R . . . .
C15 C 0.3436(2) -0.1491(3) 0.15229(9) 0.0240(5) Uani 1 1 d . . . . .
H15A H 0.3926 -0.0707 0.1358 0.029 Uiso 1 1 calc R . . . .
H15B H 0.3922 -0.2397 0.1500 0.029 Uiso 1 1 calc R . . . .
C26 C 0.5540(2) 0.6986(3) 0.31273(10) 0.0280(5) Uani 1 1 d . . . . .
H26A H 0.6287 0.7588 0.3175 0.034 Uiso 1 1 calc R . . . .
H26B H 0.4816 0.7634 0.3153 0.034 Uiso 1 1 calc R . . . .
C32 C 0.6859(2) 0.2862(3) 0.50110(10) 0.0272(5) Uani 1 1 d . . . . .
H32 H 0.7340 0.2803 0.5322 0.033 Uiso 1 1 calc R . . . .
C14 C 0.6404(2) 0.6823(3) 0.21866(10) 0.0268(5) Uani 1 1 d . . . . .
H14 H 0.6982 0.7552 0.2279 0.032 Uiso 1 1 calc R . . . .
C18 C 0.3634(2) 0.0372(2) 0.28958(9) 0.0218(5) Uani 1 1 d . . . . .
H18 H 0.4075 0.1143 0.3056 0.026 Uiso 1 1 calc R . . . .
C22 C 0.2490(2) -0.0083(2) 0.37798(10) 0.0223(4) Uani 1 1 d . . . . .
H22A H 0.1625 0.0248 0.3808 0.027 Uiso 1 1 calc R . . . .
H22B H 0.2568 -0.0987 0.3987 0.027 Uiso 1 1 calc R . . . .
C9 C 0.1804(2) 0.0545(3) 0.07019(10) 0.0246(5) Uani 1 1 d . . . . .
H9A H 0.1757 -0.0078 0.0385 0.030 Uiso 1 1 calc R . . . .
H9B H 0.1173 0.1313 0.0669 0.030 Uiso 1 1 calc R . . . .
C30 C 0.51775(19) 0.1919(2) 0.44541(9) 0.0205(4) Uani 1 1 d . . . . .
C20 C 0.2145(2) -0.1595(3) 0.29452(10) 0.0256(5) Uani 1 1 d . . . . .
H20 H 0.1570 -0.2150 0.3142 0.031 Uiso 1 1 calc R . . . .
C13 C 0.4727(2) 0.5193(3) 0.24278(10) 0.0259(5) Uani 1 1 d . . . . .
H13 H 0.4170 0.4822 0.2682 0.031 Uiso 1 1 calc R . . . .
C35 C 0.5337(2) 0.3111(2) 0.41100(9) 0.0197(4) Uani 1 1 d . . . . .
H35 H 0.4809 0.3217 0.3814 0.024 Uiso 1 1 calc R . . . .
C28 C 0.6512(2) 0.5382(2) 0.38099(10) 0.0231(5) Uani 1 1 d . . . . .
H23 H 0.313(2) 0.193(3) 0.3956(10) 0.015(6) Uiso 1 1 d . . . . .
H27 H 0.474(3) 0.556(3) 0.3671(12) 0.025(7) 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
O4 C6 1.412(3) . ?
O4 C3 1.419(3) . ?
O7 C5 1.422(3) . ?
O7 C9 1.422(3) . ?
O1 C12 1.424(3) . ?
O1 C15 1.429(3) . ?
O29 C28 1.240(3) . ?
C8 C6 1.503(3) . ?
C8 C10 1.392(3) . ?
C8 C11 1.389(3) . ?
O25 C24 1.227(3) . ?
C3 C5 1.502(3) . ?
C10 C13 1.388(3) . ?
N27 C26 1.457(3) . ?
N27 C28 1.347(3) . ?
C19 C18 1.385(3) . ?
C19 C22 1.516(3) . ?
C19 C20 1.395(3) . ?
C11 C14 1.389(4) . ?
C24 N23 1.344(3) . ?
C24 C30 1.502(3) . ?
C16 C17 1.381(3) . ?
C16 C21 1.402(3) . ?
C16 C15 1.509(3) . ?
N23 C22 1.453(3) . ?
C2 C26 1.514(3) . ?
C2 C14 1.386(4) . ?
C2 C13 1.393(3) . ?
C34 C33 1.391(3) . ?
C34 C35 1.396(3) . ?
C34 C28 1.500(3) . ?
C33 C32 1.388(4) . ?
C17 C18 1.399(3) . ?
C12 C9 1.508(3) . ?
C31 C32 1.391(3) . ?
C31 C30 1.400(3) . ?
C21 C20 1.379(3) . ?
C30 C35 1.386(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 O4 C3 112.54(18) . . ?
C5 O7 C9 111.21(17) . . ?
C12 O1 C15 114.32(17) . . ?
C10 C8 C6 121.7(2) . . ?
C11 C8 C6 119.7(2) . . ?
C11 C8 C10 118.6(2) . . ?
O4 C6 C8 110.09(19) . . ?
O4 C3 C5 108.17(19) . . ?
C13 C10 C8 120.8(2) . . ?
C28 N27 C26 122.7(2) . . ?
C18 C19 C22 122.6(2) . . ?
C18 C19 C20 118.2(2) . . ?
C20 C19 C22 119.26(19) . . ?
C8 C11 C14 120.5(2) . . ?
O25 C24 N23 123.4(2) . . ?
O25 C24 C30 120.94(19) . . ?
N23 C24 C30 115.66(19) . . ?
C17 C16 C21 118.3(2) . . ?
C17 C16 C15 121.4(2) . . ?
C21 C16 C15 120.4(2) . . ?
O7 C5 C3 109.43(18) . . ?
C24 N23 C22 121.59(19) . . ?
C14 C2 C26 120.4(2) . . ?
C14 C2 C13 118.7(2) . . ?
C13 C2 C26 120.9(2) . . ?
C33 C34 C35 119.7(2) . . ?
C33 C34 C28 119.5(2) . . ?
C35 C34 C28 120.8(2) . . ?
C32 C33 C34 119.8(2) . . ?
C16 C17 C18 121.2(2) . . ?
O1 C12 C9 113.59(18) . . ?
C32 C31 C30 120.0(2) . . ?
C20 C21 C16 120.4(2) . . ?
O1 C15 C16 112.38(17) . . ?
N27 C26 C2 113.54(19) . . ?
C33 C32 C31 120.4(2) . . ?
C2 C14 C11 120.9(2) . . ?
C19 C18 C17 120.5(2) . . ?
N23 C22 C19 114.50(18) . . ?
O7 C9 C12 110.50(18) . . ?
C31 C30 C24 119.4(2) . . ?
C35 C30 C24 120.9(2) . . ?
C35 C30 C31 119.2(2) . . ?
C21 C20 C19 121.5(2) . . ?
C10 C13 C2 120.4(2) . . ?
C30 C35 C34 120.7(2) . . ?
O29 C28 N27 123.5(2) . . ?
O29 C28 C34 121.4(2) . . ?
N27 C28 C34 115.2(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 C3 C5 O7 -63.3(2) . . . . ?
O1 C12 C9 O7 -69.2(2) . . . . ?
C8 C10 C13 C2 -0.4(3) . . . . ?
C8 C11 C14 C2 -0.2(3) . . . . ?
C6 O4 C3 C5 -178.23(19) . . . . ?
C6 C8 C10 C13 -179.3(2) . . . . ?
C6 C8 C11 C14 179.6(2) . . . . ?
O25 C24 N23 C22 -7.4(3) . . . . ?
O25 C24 C30 C31 -26.7(3) . . . . ?
O25 C24 C30 C35 145.3(2) . . . . ?
C3 O4 C6 C8 -166.45(17) . . . . ?
C10 C8 C6 O4 15.7(3) . . . . ?
C10 C8 C11 C14 -1.1(3) . . . . ?
C11 C8 C6 O4 -165.0(2) . . . . ?
C11 C8 C10 C13 1.4(3) . . . . ?
C24 N23 C22 C19 -96.7(2) . . . . ?
C24 C30 C35 C34 -169.63(19) . . . . ?
C16 C17 C18 C19 -0.7(3) . . . . ?
C16 C21 C20 C19 -0.4(4) . . . . ?
C5 O7 C9 C12 -173.44(18) . . . . ?
N23 C24 C30 C31 155.2(2) . . . . ?
N23 C24 C30 C35 -32.8(3) . . . . ?
C34 C33 C32 C31 4.1(4) . . . . ?
C33 C34 C35 C30 -1.3(3) . . . . ?
C33 C34 C28 O29 31.4(3) . . . . ?
C33 C34 C28 N27 -149.1(2) . . . . ?
C17 C16 C21 C20 0.9(3) . . . . ?
C17 C16 C15 O1 -132.1(2) . . . . ?
C12 O1 C15 C16 63.9(2) . . . . ?
C31 C30 C35 C34 2.4(3) . . . . ?
C21 C16 C17 C18 -0.4(3) . . . . ?
C21 C16 C15 O1 48.1(3) . . . . ?
C15 O1 C12 C9 92.0(2) . . . . ?
C15 C16 C17 C18 179.8(2) . . . . ?
C15 C16 C21 C20 -179.3(2) . . . . ?
C26 N27 C28 O29 5.9(4) . . . . ?
C26 N27 C28 C34 -173.7(2) . . . . ?
C26 C2 C14 C11 -176.0(2) . . . . ?
C26 C2 C13 C10 176.2(2) . . . . ?
C32 C31 C30 C24 171.9(2) . . . . ?
C32 C31 C30 C35 -0.2(3) . . . . ?
C14 C2 C26 N27 -135.4(2) . . . . ?
C14 C2 C13 C10 -0.9(3) . . . . ?
C18 C19 C22 N23 -6.9(3) . . . . ?
C18 C19 C20 C21 -0.7(3) . . . . ?
C22 C19 C18 C17 -178.9(2) . . . . ?
C22 C19 C20 C21 179.4(2) . . . . ?
C9 O7 C5 C3 175.31(18) . . . . ?
C30 C24 N23 C22 170.63(19) . . . . ?
C30 C31 C32 C33 -3.0(3) . . . . ?
C20 C19 C18 C17 1.2(3) . . . . ?
C20 C19 C22 N23 173.02(19) . . . . ?
C13 C2 C26 N27 47.5(3) . . . . ?
C13 C2 C14 C11 1.2(3) . . . . ?
C35 C34 C33 C32 -2.0(3) . . . . ?
C35 C34 C28 O29 -145.6(2) . . . . ?
C35 C34 C28 N27 34.0(3) . . . . ?
C28 N27 C26 C2 93.5(3) . . . . ?
C28 C34 C33 C32 -179.0(2) . . . . ?
C28 C34 C35 C30 175.7(2) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
6 2 2 0.0478 5.9933 2.0005 2.0074 -0.7098 -0.3969 -0.4722
0 0 1 0.0413 -0.0005 -0.0001 0.9986 -0.0010 -0.0539 0.0303
0 0 -1 0.0413 0.0005 0.0001 -0.9986 0.0010 0.0539 -0.0303
0 1 0 0.0422 0.0013 0.9992 -0.0028 0.0562 -0.0797 -0.1396
0 -1 0 0.0422 -0.0013 -0.9992 0.0028 -0.0562 0.0797 0.1396
-4 1 5 0.0212 -3.9957 0.9971 4.9801 0.5981 -0.2627 0.1808

_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Chloroform'
####################################################################### 
# 
# 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_catenane
_database_code_depnum_ccdc_archive 'CCDC 1416977'
_audit_update_record             
;
2015-08-05 deposited with the CCDC.
2015-09-15 downloaded from the CCDC.
;
_audit_creation_date             2014-06-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         
'C H Cl3, C28 H30 N2 O5, C28 H29.56 N2 O5, 0.5(C H2 Cl3)'
_chemical_formula_sum            'C57.50 H61.56 Cl4.50 N4 O10'
_chemical_formula_weight         1128.19
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C56 H60 N4 O10'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   21.3381(9)
_cell_length_b                   10.9654(3)
_cell_length_c                   25.5553(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.186(5)
_cell_angle_gamma                90.00
_cell_volume                     5496.5(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4207
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      72.9940
_cell_measurement_theta_min      4.5600
_exptl_absorpt_coefficient_mu    2.694
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33t (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:01:44)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2364
_exptl_crystal_size_max          0.1408
_exptl_crystal_size_mid          0.0656
_exptl_crystal_size_min          0.0255
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            18597
_diffrn_reflns_theta_full        73.05
_diffrn_reflns_theta_max         73.05
_diffrn_reflns_theta_min         4.45
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2299
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -64.00   30.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   57.0000  -30.0000 94

#__ type_ start__ end____ width___ exp.time_
  2 omega   23.00   97.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1418 -125.0000 -150.0000 74

#__ type_ start__ end____ width___ exp.time_
  3 omega   32.00  136.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      103.5913  -15.0000  -60.0000 104

#__ type_ start__ end____ width___ exp.time_
  4 omega   34.00   98.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      103.5913  -45.0000  120.0000 64

#__ type_ start__ end____ width___ exp.time_
  5 omega   77.00  172.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      103.5913   61.0000  120.0000 95

#__ type_ start__ end____ width___ exp.time_
  6 omega   35.00  130.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      103.5913  -61.0000  -30.0000 95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0567075000
_diffrn_orient_matrix_UB_12      -0.0946024000
_diffrn_orient_matrix_UB_13      0.0283213000
_diffrn_orient_matrix_UB_21      -0.0300882000
_diffrn_orient_matrix_UB_22      -0.0816520000
_diffrn_orient_matrix_UB_23      -0.0531339000
_diffrn_orient_matrix_UB_31      0.0452619000
_diffrn_orient_matrix_UB_32      0.0640724000
_diffrn_orient_matrix_UB_33      -0.0260220000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                7371
_reflns_number_total             10482
_reflns_odcompleteness_completeness 98.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33t (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:01:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33t (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:01:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33t (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:01:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         10482
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0504
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0402P)²+2.6997P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1225
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Rigid bond restraints
 Cl5, C4, Cl6, Cl2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C59A) = Uanis(C59B)
4. Others
 Sof(C61B)=Sof(H61B)=Sof(C1)=Sof(H1A)=Sof(H1B)=1-FVAR(1)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C61A)=Sof(H61A)=Sof(H61C)=FVAR(1)
 Sof(O60B)=1-FVAR(2)
 Sof(O60A)=FVAR(2)
 Sof(C59B)=Sof(H59A)=Sof(H59B)=1-FVAR(3)
 Sof(C59A)=Sof(H59C)=Sof(H59D)=FVAR(3)
 Fixed Sof: Cl2(0.5) Cl5(0.5) C4(0.5) H4A(0.5) H4B(0.5) Cl6(0.5)
5.a Ternary CH refined with riding coordinates:
 C2(H2)
5.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C12(H12A,H12B), C16(H16A,H16B), C19(H19A,H19B), C10(H10A,
 H10B), C33(H33A,H33B), C29(H29A,H29B), C22(H22A,H22B), C64(H64A,H64B),
 C72(H72A,H72B), C74(H74A,H74B), C75(H75A,H75B), C51(H51A,H51B), C59B(H59A,
 H59B), C1(H1A,H1B), C3(H3A,H3B), C61A(H61A,H61C), C59A(H59C,H59D), C4(H4A,H4B)
5.c Aromatic/amide H refined with riding coordinates:
 N34(H34), N30(H30), C17(H17), C42(H42), C24(H24), C20(H20), C38(H38),
 C21(H21), C27(H27), C40(H40), C25(H25), C18(H18), C28(H28), C39(H39), N63(H63),
  N50(H50), C67(H67), C71(H71), C70(H70), C68(H68), C46(H46), C48(H48),
 C44(H44), C57(H57), C45(H45), C54(H54), C55(H55), C58(H58), C61B(H61B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Cl4 Cl 0.34676(4) 0.94941(8) 0.19432(4) 0.0521(2) Uani 1 d . . . .
Cl1 Cl 0.49094(4) 1.00048(9) 0.23414(4) 0.0595(2) Uani 1 d . . . .
Cl3 Cl 0.43371(5) 0.78891(8) 0.16331(5) 0.0606(2) Uani 1 d . . . .
O11 O 0.90114(9) 0.64478(15) 0.15791(7) 0.0260(4) Uani 1 d . . . .
O36 O 1.14217(10) 1.00670(17) 0.48395(7) 0.0341(4) Uani 1 d . . . .
O14 O 0.75812(9) 0.71258(15) 0.14504(7) 0.0253(4) Uani 1 d . . . .
O8 O 0.67203(9) 0.80031(15) 0.19588(7) 0.0269(4) Uani 1 d . . . .
O32 O 0.85578(9) 1.35232(15) 0.46183(7) 0.0274(4) Uani 1 d . . . .
N34 N 1.03822(11) 0.93298(18) 0.42587(8) 0.0252(4) Uani 1 d . . . .
H34 H 0.9959 0.9508 0.4076 0.030 Uiso 1 calc . . R .
C13 C 0.97376(13) 0.6537(2) 0.18611(10) 0.0259(5) Uani 1 d . . . .
H13A H 0.9904 0.7113 0.1658 0.031 Uiso 1 calc . . R .
H13B H 0.9938 0.5748 0.1849 0.031 Uiso 1 calc . . R .
N30 N 0.83318(11) 1.18623(19) 0.40455(9) 0.0260(5) Uani 1 d . . . .
H30 H 0.8483 1.1350 0.3868 0.031 Uiso 1 calc . . R .
C9 C 1.03795(13) 0.7685(2) 0.36097(10) 0.0252(5) Uani 1 d . . . .
C17 C 1.03876(14) 0.7946(2) 0.26745(10) 0.0262(5) Uani 1 d . . . .
H17 H 1.0537 0.8375 0.2431 0.031 Uiso 1 calc . . R .
C37 C 0.94799(13) 1.2635(2) 0.44423(9) 0.0232(5) Uani 1 d . . . .
C42 C 0.97861(13) 1.1507(2) 0.44630(9) 0.0222(5) Uani 1 d . . . .
H42 H 0.9529 1.0799 0.4415 0.027 Uiso 1 calc . . R .
C15 C 0.99672(13) 0.6938(2) 0.24707(10) 0.0227(5) Uani 1 d . . . .
C41 C 1.04710(13) 1.1423(2) 0.45542(9) 0.0247(5) Uani 1 d . . . .
C24 C 0.66077(14) 1.0124(2) 0.26099(11) 0.0300(6) Uani 1 d . . . .
H24 H 0.6359 1.0314 0.2229 0.036 Uiso 1 calc . . R .
C35 C 1.08058(13) 1.0213(2) 0.45652(9) 0.0249(5) Uani 1 d . . . .
C20 C 1.05888(14) 0.8320(2) 0.32361(10) 0.0264(5) Uani 1 d . . . .
H20 H 1.0866 0.9003 0.3364 0.032 Uiso 1 calc . . R .
C12 C 0.79520(13) 0.7526(2) 0.11234(10) 0.0249(5) Uani 1 d . . . .
H12A H 0.7782 0.8314 0.0955 0.030 Uiso 1 calc . . R .
H12B H 0.7887 0.6951 0.0818 0.030 Uiso 1 calc . . R .
C31 C 0.87533(13) 1.2716(2) 0.43769(10) 0.0232(5) Uani 1 d . . . .
C16 C 0.68588(13) 0.7234(2) 0.11399(11) 0.0274(5) Uani 1 d . . . .
H16A H 0.6702 0.6625 0.0841 0.033 Uiso 1 calc . . R .
H16B H 0.6749 0.8034 0.0966 0.033 Uiso 1 calc . . R .
C38 C 0.98632(14) 1.3696(2) 0.45038(10) 0.0278(6) Uani 1 d . . . .
H38 H 0.9661 1.4455 0.4484 0.033 Uiso 1 calc . . R .
C21 C 0.99644(13) 0.6673(2) 0.34100(10) 0.0262(5) Uani 1 d . . . .
H21 H 0.9822 0.6236 0.3655 0.031 Uiso 1 calc . . R .
C19 C 0.65138(14) 0.7051(2) 0.15449(11) 0.0283(6) Uani 1 d . . . .
H19A H 0.6023 0.7068 0.1339 0.034 Uiso 1 calc . . R .
H19B H 0.6640 0.6265 0.1731 0.034 Uiso 1 calc . . R .
C27 C 0.73185(15) 0.9585(2) 0.37472(12) 0.0330(6) Uani 1 d . . . .
H27 H 0.7552 0.9398 0.4130 0.040 Uiso 1 calc . . R .
C26 C 0.72675(13) 1.0789(2) 0.35681(11) 0.0273(5) Uani 1 d . . . .
C23 C 0.66742(14) 0.8909(2) 0.27846(11) 0.0289(6) Uani 1 d . . . .
C40 C 1.08507(14) 1.2490(2) 0.46271(10) 0.0289(6) Uani 1 d . . . .
H40 H 1.1312 1.2446 0.4698 0.035 Uiso 1 calc . . R .
C25 C 0.69060(14) 1.1049(2) 0.29945(11) 0.0306(6) Uani 1 d . . . .
H25 H 0.6865 1.1853 0.2869 0.037 Uiso 1 calc . . R .
C10 C 0.86991(13) 0.7622(2) 0.14981(10) 0.0236(5) Uani 1 d . . . .
H10A H 0.8920 0.8164 0.1323 0.028 Uiso 1 calc . . R .
H10B H 0.8754 0.7962 0.1864 0.028 Uiso 1 calc . . R .
C33 C 1.06030(15) 0.8090(2) 0.42196(10) 0.0295(6) Uani 1 d . . . .
H33A H 1.0414 0.7542 0.4418 0.035 Uiso 1 calc . . R .
H33B H 1.1096 0.8047 0.4405 0.035 Uiso 1 calc . . R .
C29 C 0.76252(14) 1.1788(2) 0.39803(11) 0.0308(6) Uani 1 d . . . .
H29A H 0.7399 1.2560 0.3841 0.037 Uiso 1 calc . . R .
H29B H 0.7606 1.1622 0.4346 0.037 Uiso 1 calc . . R .
C18 C 0.97583(13) 0.6302(2) 0.28438(10) 0.0249(5) Uani 1 d . . . .
H18 H 0.9479 0.5623 0.2715 0.030 Uiso 1 calc . . R .
C28 C 0.70214(14) 0.8654(2) 0.33557(12) 0.0333(6) Uani 1 d . . . .
H28 H 0.7058 0.7851 0.3481 0.040 Uiso 1 calc . . R .
C39 C 1.05428(14) 1.3618(2) 0.45945(11) 0.0299(6) Uani 1 d . . . .
H39 H 1.0797 1.4326 0.4634 0.036 Uiso 1 calc . . R .
C22 C 0.63968(15) 0.7903(2) 0.23532(12) 0.0329(6) Uani 1 d . . . .
H22A H 0.6494 0.7114 0.2540 0.040 Uiso 1 calc . . R .
H22B H 0.5907 0.7985 0.2155 0.040 Uiso 1 calc . . R .
C2 C 0.41901(15) 0.9412(3) 0.17818(13) 0.0409(7) Uani 1 d . . . .
H2 H 0.4107 0.9904 0.1441 0.049 Uiso 1 calc . . R .
O65 O 0.89170(9) 0.97251(16) 0.34332(7) 0.0287(4) Uani 1 d . . . .
O73 O 0.66065(9) 1.00846(16) -0.04263(7) 0.0283(4) Uani 1 d . . . .
N63 N 0.81661(11) 0.93277(18) 0.25348(8) 0.0231(4) Uani 1 d . . . .
H63 H 0.7896 0.8808 0.2302 0.028 Uiso 1 calc . . R .
O76 O 0.59515(11) 0.81347(18) -0.11514(8) 0.0410(5) Uani 1 d . . . .
C66 C 0.79358(13) 1.0612(2) 0.16903(10) 0.0221(5) Uani 1 d . . . .
N50 N 0.78104(13) 0.46889(19) 0.20667(11) 0.0369(6) Uani 1 d . . . .
H50 H 0.7854 0.5403 0.1946 0.044 Uiso 1 calc . . R .
C67 C 0.72344(13) 1.0584(2) 0.13810(10) 0.0253(5) Uani 1 d . . . .
H67 H 0.6946 1.0477 0.1572 0.030 Uiso 1 calc . . R .
C64 C 0.82317(14) 1.0547(2) 0.23331(10) 0.0255(5) Uani 1 d . . . .
H64A H 0.8710 1.0772 0.2478 0.031 Uiso 1 calc . . R .
H64B H 0.7998 1.1128 0.2479 0.031 Uiso 1 calc . . R .
C62 C 0.85222(13) 0.9008(2) 0.30782(10) 0.0229(5) Uani 1 d . . . .
C47 C 0.84241(13) 0.7730(2) 0.32374(10) 0.0255(5) Uani 1 d . . . .
C69 C 0.73802(13) 1.0869(2) 0.04979(10) 0.0228(5) Uani 1 d . . . .
C71 C 0.83556(13) 1.0740(2) 0.13940(10) 0.0244(5) Uani 1 d . . . .
H71 H 0.8826 1.0740 0.1592 0.029 Uiso 1 calc . . R .
C43 C 0.81083(14) 0.5621(2) 0.30006(12) 0.0304(6) Uani 1 d . . . .
C70 C 0.80785(13) 1.0869(2) 0.08024(10) 0.0231(5) Uani 1 d . . . .
H70 H 0.8367 1.0955 0.0611 0.028 Uiso 1 calc . . R .
O52 O 0.78235(15) 0.35379(19) 0.27924(11) 0.0617(7) Uani 1 d . . . .
C68 C 0.69574(13) 1.0714(2) 0.07950(10) 0.0257(5) Uani 1 d . . . .
H68 H 0.6487 1.0697 0.0597 0.031 Uiso 1 calc . . R .
C46 C 0.85668(14) 0.7481(3) 0.38077(11) 0.0334(6) Uani 1 d . . . .
H46 H 0.8732 0.8093 0.4080 0.040 Uiso 1 calc . . R .
C72 C 0.70685(14) 1.1047(2) -0.01399(10) 0.0293(6) Uani 1 d . . . .
H72A H 0.6827 1.1818 -0.0227 0.035 Uiso 1 calc . . R .
H72B H 0.7429 1.1084 -0.0280 0.035 Uiso 1 calc . . R .
C48 C 0.81973(13) 0.6802(2) 0.28373(11) 0.0251(5) Uani 1 d . . . .
H48 H 0.8104 0.6968 0.2457 0.030 Uiso 1 calc . . R .
C49 C 0.79045(15) 0.4534(2) 0.26098(13) 0.0364(7) Uani 1 d . . . .
C44 C 0.82320(15) 0.5401(3) 0.35683(13) 0.0388(7) Uani 1 d . . . .
H44 H 0.8159 0.4624 0.3680 0.047 Uiso 1 calc . . R .
C74 C 0.69565(15) 0.8986(2) -0.04499(11) 0.0338(6) Uani 1 d . . . .
H74A H 0.7329 0.8841 -0.0086 0.041 Uiso 1 calc A . R .
H74B H 0.7144 0.9058 -0.0738 0.041 Uiso 1 calc . . R .
C75 C 0.64596(17) 0.7950(3) -0.05919(12) 0.0418(7) Uani 1 d . . . .
H75A H 0.6695 0.7184 -0.0576 0.050 Uiso 1 calc . . R .
H75B H 0.6248 0.7915 -0.0319 0.050 Uiso 1 calc . . R .
C53 C 0.71343(17) 0.3973(2) 0.10856(14) 0.0403(7) Uani 1 d . . . .
C57 C 0.5978(2) 0.4133(4) 0.03985(15) 0.0636(11) Uani 1 d . . . .
H57 H 0.5513 0.4079 0.0313 0.076 Uiso 1 calc . . R .
C45 C 0.84602(16) 0.6315(3) 0.39667(12) 0.0402(7) Uani 1 d . . . .
H45 H 0.8544 0.6151 0.4345 0.048 Uiso 1 calc . . R .
C51 C 0.76326(17) 0.3651(3) 0.16751(15) 0.0473(8) Uani 1 d . . . .
H51A H 0.7438 0.3012 0.1827 0.057 Uiso 1 calc . . R .
H51B H 0.8045 0.3331 0.1652 0.057 Uiso 1 calc . . R .
C54 C 0.7358(2) 0.4303(3) 0.06682(17) 0.0499(9) Uani 1 d . . . .
H54 H 0.7823 0.4365 0.0755 0.060 Uiso 1 calc . . R .
O60B O 0.5416(11) 0.617(2) -0.0626(4) 0.040(4) Uani 0.48(5) d A 2 . .
C55 C 0.6897(2) 0.4541(3) 0.01212(17) 0.0592(11) Uani 1 d . . . .
H55 H 0.7056 0.4772 -0.0155 0.071 Uiso 1 calc . . R .
C58 C 0.64401(18) 0.3902(3) 0.09465(14) 0.0494(8) Uani 1 d . . . .
H58 H 0.6282 0.3697 0.1226 0.059 Uiso 1 calc . . R .
C56 C 0.6202(2) 0.4443(3) -0.00240(15) 0.0642(12) Uani 1 d . . . .
C59B C 0.5707(4) 0.4707(5) -0.06122(18) 0.100(3) Uani 0.953(12) d A 2 . .
H59A H 0.5329 0.4137 -0.0721 0.120 Uiso 0.953(12) calc A 2 R .
H59B H 0.5927 0.4624 -0.0878 0.120 Uiso 0.953(12) calc A 2 R .
C61B C 0.5107(4) 0.6716(9) -0.1173(3) 0.033(2) Uani 0.439(11) d A 2 . .
H61B H 0.4638 0.6825 -0.1356 0.040 Uiso 0.439(11) calc A 2 R .
Cl2 Cl 0.54625(8) 0.98882(16) 0.11045(6) 0.0465(4) Uani 0.50 d B -1 . U
C1 C 0.5603(4) 0.7111(6) -0.1437(3) 0.0271(19) Uani 0.439(11) d A 2 . .
H1A H 0.5923 0.6458 -0.1406 0.033 Uiso 0.439(11) calc A 2 R .
H1B H 0.5356 0.7298 -0.1837 0.033 Uiso 0.439(11) calc A 2 R .
C3 C 0.5292(4) 0.7441(7) -0.1281(3) 0.055(3) Uani 0.561(11) d A 1 . .
H3A H 0.5096 0.7716 -0.1017 0.066 Uiso 0.561(11) calc A 1 R .
H3B H 0.4977 0.7666 -0.1661 0.066 Uiso 0.561(11) calc A 1 R .
C61A C 0.5334(5) 0.6122(9) -0.1253(3) 0.057(2) Uani 0.561(11) d A 1 . .
H61A H 0.4881 0.5773 -0.1431 0.068 Uiso 0.561(11) calc A 1 R .
H61C H 0.5606 0.5830 -0.1454 0.068 Uiso 0.561(11) calc A 1 R .
O60A O 0.5639(12) 0.576(2) -0.0668(3) 0.046(5) Uani 0.52(5) d A 1 . .
C59A C 0.525(8) 0.454(10) -0.065(4) 0.100(3) Uani 0.047(12) d A 1 . .
H59C H 0.5161 0.3984 -0.0970 0.120 Uiso 0.047(12) calc A 1 R .
H59D H 0.4878 0.4606 -0.0530 0.120 Uiso 0.047(12) calc A 1 R .
Cl5 Cl 0.50606(13) 0.8966(3) 0.00075(11) 0.0651(7) Uani 0.50 d . -1 . U
C4 C 0.4861(3) 0.9782(6) 0.0402(3) 0.0442(14) Uani 0.50 d . . . U
H4A H 0.4438 0.9477 0.0410 0.053 Uiso 0.50 calc B -1 R .
H4B H 0.4773 1.0596 0.0241 0.053 Uiso 0.50 calc B -1 R .
Cl6 Cl 0.4953(2) 0.8398(3) 0.01187(13) 0.1027(13) Uani 0.50 d B -2 . U


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl4 C2 1.748(3) . ?
Cl1 C2 1.759(3) . ?
Cl3 C2 1.768(3) . ?
O11 C13 1.432(3) . ?
O11 C10 1.427(3) . ?
O36 C35 1.232(3) . ?
O14 C12 1.427(3) . ?
O14 C16 1.434(3) . ?
O8 C19 1.427(3) . ?
O8 C22 1.432(3) . ?
O32 C31 1.241(3) . ?
N34 C35 1.345(3) . ?
N34 C33 1.455(3) . ?
C13 C15 1.503(3) . ?
N30 C31 1.343(3) . ?
N30 C29 1.453(3) . ?
C9 C20 1.390(4) . ?
C9 C21 1.386(4) . ?
C9 C33 1.506(3) . ?
C17 C15 1.389(4) . ?
C17 C20 1.388(3) . ?
C37 C42 1.390(3) . ?
C37 C31 1.495(4) . ?
C37 C38 1.395(4) . ?
C42 C41 1.389(4) . ?
C15 C18 1.389(3) . ?
C41 C35 1.502(3) . ?
C41 C40 1.393(4) . ?
C24 C23 1.394(4) . ?
C24 C25 1.382(4) . ?
C12 C10 1.506(4) . ?
C16 C19 1.501(4) . ?
C38 C39 1.378(4) . ?
C21 C18 1.397(3) . ?
C27 C26 1.387(4) . ?
C27 C28 1.395(4) . ?
C26 C25 1.391(4) . ?
C26 C29 1.503(4) . ?
C23 C28 1.381(4) . ?
C23 C22 1.507(4) . ?
C40 C39 1.388(4) . ?
O65 C62 1.245(3) . ?
O73 C72 1.433(3) . ?
O73 C74 1.431(3) . ?
N63 C64 1.460(3) . ?
N63 C62 1.341(3) . ?
O76 C75 1.429(3) . ?
O76 C1 1.385(6) . ?
O76 C3 1.517(8) . ?
C66 C67 1.391(4) . ?
C66 C64 1.512(3) . ?
C66 C71 1.389(3) . ?
N50 C49 1.332(4) . ?
N50 C51 1.464(4) . ?
C67 C68 1.384(3) . ?
C62 C47 1.496(3) . ?
C47 C46 1.393(3) . ?
C47 C48 1.388(4) . ?
C69 C70 1.383(4) . ?
C69 C68 1.400(3) . ?
C69 C72 1.511(3) . ?
C71 C70 1.397(3) . ?
C43 C48 1.396(4) . ?
C43 C49 1.505(4) . ?
C43 C44 1.390(4) . ?
O52 C49 1.227(3) . ?
C46 C45 1.388(4) . ?
C44 C45 1.374(4) . ?
C74 C75 1.498(4) . ?
C53 C51 1.505(5) . ?
C53 C54 1.377(4) . ?
C53 C58 1.383(5) . ?
C57 C58 1.382(5) . ?
C57 C56 1.385(5) . ?
C54 C55 1.381(6) . ?
O60B C59B 1.71(3) . ?
O60B C61B 1.423(12) . ?
C55 C56 1.384(6) . ?
C56 C59B 1.486(6) . ?
C56 C59A 2.03(14) . ?
C61B C1 1.525(13) . ?
Cl2 C4 1.752(6) . ?
C3 C61A 1.449(13) . ?
C61A O60A 1.432(10) . ?
O60A C59A 1.58(11) . ?
Cl5 C4 1.529(7) . ?
Cl5 C4 1.774(7) 3_675 ?
C4 Cl5 1.774(7) 3_675 ?
C4 Cl6 1.725(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C10 O11 C13 111.27(18) . . ?
C12 O14 C16 111.93(18) . . ?
C19 O8 C22 111.83(19) . . ?
C35 N34 C33 123.4(2) . . ?
O11 C13 C15 112.8(2) . . ?
C31 N30 C29 121.2(2) . . ?
C20 C9 C33 120.4(2) . . ?
C21 C9 C20 118.7(2) . . ?
C21 C9 C33 120.9(2) . . ?
C20 C17 C15 120.9(2) . . ?
C42 C37 C31 120.6(2) . . ?
C42 C37 C38 119.4(2) . . ?
C38 C37 C31 119.9(2) . . ?
C41 C42 C37 120.9(2) . . ?
C17 C15 C13 121.4(2) . . ?
C17 C15 C18 118.5(2) . . ?
C18 C15 C13 120.2(2) . . ?
C42 C41 C35 121.5(2) . . ?
C42 C41 C40 119.0(2) . . ?
C40 C41 C35 119.5(2) . . ?
C25 C24 C23 120.9(3) . . ?
O36 C35 N34 124.0(2) . . ?
O36 C35 C41 121.2(2) . . ?
N34 C35 C41 114.8(2) . . ?
C17 C20 C9 120.6(2) . . ?
O14 C12 C10 109.96(19) . . ?
O32 C31 N30 122.5(2) . . ?
O32 C31 C37 121.6(2) . . ?
N30 C31 C37 115.9(2) . . ?
O14 C16 C19 108.6(2) . . ?
C39 C38 C37 119.9(2) . . ?
C9 C21 C18 120.6(2) . . ?
O8 C19 C16 108.8(2) . . ?
C26 C27 C28 120.3(2) . . ?
C27 C26 C25 118.8(2) . . ?
C27 C26 C29 120.7(2) . . ?
C25 C26 C29 120.4(2) . . ?
C24 C23 C22 120.3(2) . . ?
C28 C23 C24 118.5(2) . . ?
C28 C23 C22 121.2(2) . . ?
C39 C40 C41 120.2(3) . . ?
C24 C25 C26 120.5(2) . . ?
O11 C10 C12 110.26(19) . . ?
N34 C33 C9 111.5(2) . . ?
N30 C29 C26 109.8(2) . . ?
C15 C18 C21 120.6(2) . . ?
C23 C28 C27 120.9(3) . . ?
C38 C39 C40 120.5(2) . . ?
O8 C22 C23 107.4(2) . . ?
Cl4 C2 Cl1 110.95(18) . . ?
Cl4 C2 Cl3 110.29(17) . . ?
Cl1 C2 Cl3 110.60(17) . . ?
C74 O73 C72 112.1(2) . . ?
C62 N63 C64 120.8(2) . . ?
C75 O76 C3 114.9(3) . . ?
C1 O76 C75 116.8(3) . . ?
C1 O76 C3 38.7(3) . . ?
C67 C66 C64 120.8(2) . . ?
C71 C66 C67 118.2(2) . . ?
C71 C66 C64 120.9(2) . . ?
C49 N50 C51 120.3(2) . . ?
C68 C67 C66 121.2(2) . . ?
N63 C64 C66 111.67(19) . . ?
O65 C62 N63 122.3(2) . . ?
O65 C62 C47 121.4(2) . . ?
N63 C62 C47 116.3(2) . . ?
C46 C47 C62 118.1(2) . . ?
C48 C47 C62 122.1(2) . . ?
C48 C47 C46 119.8(2) . . ?
C70 C69 C68 118.5(2) . . ?
C70 C69 C72 121.8(2) . . ?
C68 C69 C72 119.8(2) . . ?
C66 C71 C70 120.7(2) . . ?
C48 C43 C49 125.0(2) . . ?
C44 C43 C48 118.7(3) . . ?
C44 C43 C49 116.2(2) . . ?
C69 C70 C71 120.8(2) . . ?
C67 C68 C69 120.5(2) . . ?
C45 C46 C47 119.5(3) . . ?
O73 C72 C69 112.2(2) . . ?
C47 C48 C43 120.6(2) . . ?
N50 C49 C43 118.4(2) . . ?
O52 C49 N50 121.6(3) . . ?
O52 C49 C43 120.0(3) . . ?
C45 C44 C43 120.9(3) . . ?
O73 C74 C75 108.5(2) . . ?
O76 C75 C74 108.7(2) . . ?
C54 C53 C51 120.9(3) . . ?
C54 C53 C58 118.6(3) . . ?
C58 C53 C51 120.5(3) . . ?
C58 C57 C56 120.4(4) . . ?
C44 C45 C46 120.4(3) . . ?
N50 C51 C53 113.1(2) . . ?
C53 C54 C55 120.5(3) . . ?
C61B O60B C59B 116.0(15) . . ?
C54 C55 C56 121.2(3) . . ?
C57 C58 C53 121.0(3) . . ?
C57 C56 C59B 120.7(5) . . ?
C57 C56 C59A 95(4) . . ?
C55 C56 C57 118.2(4) . . ?
C55 C56 C59B 121.1(4) . . ?
C55 C56 C59A 147(4) . . ?
C59B C56 C59A 26(4) . . ?
C56 C59B O60B 108.0(4) . . ?
O60B C61B C1 114.9(11) . . ?
O76 C1 C61B 108.6(7) . . ?
C61A C3 O76 117.2(9) . . ?
O60A C61A C3 108.9(13) . . ?
C61A O60A C59A 104(4) . . ?
O60A C59A C56 72(5) . . ?
C4 Cl5 C4 93.0(4) . 3_675 ?
Cl2 C4 Cl5 110.6(3) . 3_675 ?
Cl5 C4 Cl2 115.6(4) . . ?
Cl5 C4 Cl5 87.0(4) . 3_675 ?
Cl5 C4 Cl6 25.99(18) . . ?
Cl6 C4 Cl2 109.3(4) . . ?
Cl6 C4 Cl5 112.3(4) . 3_675 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O11 C13 C15 C17 -125.1(3) . . . . ?
O11 C13 C15 C18 54.8(3) . . . . ?
O14 C12 C10 O11 80.5(2) . . . . ?
O14 C16 C19 O8 63.3(3) . . . . ?
C13 O11 C10 C12 171.27(19) . . . . ?
C13 C15 C18 C21 -179.5(2) . . . . ?
C9 C21 C18 C15 0.2(4) . . . . ?
C17 C15 C18 C21 0.3(4) . . . . ?
C37 C42 C41 C35 -178.7(2) . . . . ?
C37 C42 C41 C40 0.2(3) . . . . ?
C37 C38 C39 C40 -0.2(4) . . . . ?
C42 C37 C31 O32 144.1(2) . . . . ?
C42 C37 C31 N30 -35.6(3) . . . . ?
C42 C37 C38 C39 -1.2(3) . . . . ?
C42 C41 C35 O36 -152.9(2) . . . . ?
C42 C41 C35 N34 26.9(3) . . . . ?
C42 C41 C40 C39 -1.6(3) . . . . ?
C15 C17 C20 C9 0.7(4) . . . . ?
C41 C40 C39 C38 1.6(4) . . . . ?
C24 C23 C28 C27 -2.1(4) . . . . ?
C24 C23 C22 O8 58.3(3) . . . . ?
C35 N34 C33 C9 -128.1(3) . . . . ?
C35 C41 C40 C39 177.3(2) . . . . ?
C20 C9 C21 C18 -0.3(4) . . . . ?
C20 C9 C33 N34 59.5(3) . . . . ?
C20 C17 C15 C13 179.0(2) . . . . ?
C20 C17 C15 C18 -0.8(4) . . . . ?
C12 O14 C16 C19 -168.30(19) . . . . ?
C31 N30 C29 C26 177.6(2) . . . . ?
C31 C37 C42 C41 -176.5(2) . . . . ?
C31 C37 C38 C39 176.5(2) . . . . ?
C16 O14 C12 C10 169.32(19) . . . . ?
C38 C37 C42 C41 1.2(3) . . . . ?
C38 C37 C31 O32 -33.6(3) . . . . ?
C38 C37 C31 N30 146.8(2) . . . . ?
C21 C9 C20 C17 -0.2(4) . . . . ?
C21 C9 C33 N34 -120.7(3) . . . . ?
C19 O8 C22 C23 177.4(2) . . . . ?
C27 C26 C25 C24 -0.5(4) . . . . ?
C27 C26 C29 N30 82.9(3) . . . . ?
C26 C27 C28 C23 0.2(4) . . . . ?
C23 C24 C25 C26 -1.4(4) . . . . ?
C40 C41 C35 O36 28.2(3) . . . . ?
C40 C41 C35 N34 -152.0(2) . . . . ?
C25 C24 C23 C28 2.7(4) . . . . ?
C25 C24 C23 C22 -174.9(2) . . . . ?
C25 C26 C29 N30 -94.1(3) . . . . ?
C10 O11 C13 C15 68.7(3) . . . . ?
C33 N34 C35 O36 0.6(4) . . . . ?
C33 N34 C35 C41 -179.2(2) . . . . ?
C33 C9 C20 C17 179.6(2) . . . . ?
C33 C9 C21 C18 179.9(2) . . . . ?
C29 N30 C31 O32 -4.1(4) . . . . ?
C29 N30 C31 C37 175.5(2) . . . . ?
C29 C26 C25 C24 176.5(2) . . . . ?
C28 C27 C26 C25 1.1(4) . . . . ?
C28 C27 C26 C29 -175.9(2) . . . . ?
C28 C23 C22 O8 -119.2(3) . . . . ?
C22 O8 C19 C16 178.6(2) . . . . ?
C22 C23 C28 C27 175.4(3) . . . . ?
O65 C62 C47 C46 23.6(4) . . . . ?
O65 C62 C47 C48 -156.5(2) . . . . ?
O73 C74 C75 O76 64.8(3) . . . . ?
N63 C62 C47 C46 -156.8(2) . . . . ?
N63 C62 C47 C48 23.1(4) . . . . ?
O76 C3 C61A O60A 73.6(16) . . . . ?
C66 C67 C68 C69 0.4(4) . . . . ?
C66 C71 C70 C69 -0.1(4) . . . . ?
C67 C66 C64 N63 72.5(3) . . . . ?
C67 C66 C71 C70 1.6(3) . . . . ?
C64 N63 C62 O65 0.4(4) . . . . ?
C64 N63 C62 C47 -179.1(2) . . . . ?
C64 C66 C67 C68 176.2(2) . . . . ?
C64 C66 C71 C70 -176.3(2) . . . . ?
C62 N63 C64 C66 165.3(2) . . . . ?
C62 C47 C46 C45 177.9(3) . . . . ?
C62 C47 C48 C43 -179.7(2) . . . . ?
C47 C46 C45 C44 1.7(4) . . . . ?
C71 C66 C67 C68 -1.7(4) . . . . ?
C71 C66 C64 N63 -109.6(3) . . . . ?
C43 C44 C45 C46 0.5(5) . . . . ?
C70 C69 C68 C67 1.1(4) . . . . ?
C70 C69 C72 O73 125.8(2) . . . . ?
C68 C69 C70 C71 -1.2(3) . . . . ?
C68 C69 C72 O73 -55.0(3) . . . . ?
C46 C47 C48 C43 0.2(4) . . . . ?
C72 O73 C74 C75 163.4(2) . . . . ?
C72 C69 C70 C71 178.0(2) . . . . ?
C72 C69 C68 C67 -178.2(2) . . . . ?
C48 C47 C46 C45 -2.0(4) . . . . ?
C48 C43 C49 N50 1.2(4) . . . . ?
C48 C43 C49 O52 -178.2(3) . . . . ?
C48 C43 C44 C45 -2.2(4) . . . . ?
C49 N50 C51 C53 142.8(3) . . . . ?
C49 C43 C48 C47 -176.3(2) . . . . ?
C49 C43 C44 C45 176.1(3) . . . . ?
C44 C43 C48 C47 1.8(4) . . . . ?
C44 C43 C49 N50 -177.0(3) . . . . ?
C44 C43 C49 O52 3.6(4) . . . . ?
C74 O73 C72 C69 -75.1(3) . . . . ?
C75 O76 C1 C61B 73.4(7) . . . . ?
C75 O76 C3 C61A -61.0(9) . . . . ?
C53 C54 C55 C56 -0.7(5) . . . . ?
C57 C56 C59B O60B 79.8(8) . . . . ?
C57 C56 C59A O60A 129(4) . . . . ?
C51 N50 C49 C43 178.1(3) . . . . ?
C51 N50 C49 O52 -2.5(5) . . . . ?
C51 C53 C54 C55 176.9(3) . . . . ?
C51 C53 C58 C57 -176.5(3) . . . . ?
C54 C53 C51 N50 93.5(3) . . . . ?
C54 C53 C58 C57 1.3(5) . . . . ?
C54 C55 C56 C57 1.8(5) . . . . ?
C54 C55 C56 C59B 179.7(4) . . . . ?
C54 C55 C56 C59A -177(6) . . . . ?
O60B C61B C1 O76 -72.7(14) . . . . ?
C55 C56 C59B O60B -98.0(8) . . . . ?
C55 C56 C59A O60A -52(9) . . . . ?
C58 C53 C51 N50 -88.8(4) . . . . ?
C58 C53 C54 C55 -0.8(4) . . . . ?
C58 C57 C56 C55 -1.4(6) . . . . ?
C58 C57 C56 C59B -179.3(4) . . . . ?
C58 C57 C56 C59A 178(3) . . . . ?
C56 C57 C58 C53 -0.1(6) . . . . ?
C59B O60B C61B C1 -74.5(10) . . . . ?
C59B C56 C59A O60A -45(5) . . . . ?
C61B O60B C59B C56 161.4(10) . . . . ?
C1 O76 C75 C74 157.2(4) . . . . ?
C1 O76 C3 C61A 41.5(8) . . . . ?
C3 O76 C75 C74 -159.6(5) . . . . ?
C3 O76 C1 C61B -23.6(6) . . . . ?
C3 C61A O60A C59A 145(7) . . . . ?
C61A O60A C59A C56 151(3) . . . . ?
C59A C56 C59B O60B 87(8) . . . . ?
C4 Cl5 C4 Cl2 -111.4(5) 3_675 . . . ?
C4 Cl5 C4 Cl5 0.0 3_675 . . 3_675 ?
C4 Cl5 C4 Cl6 167.2(5) 3_675 . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
7 5 -10 0.0616 6.7876 5.3759 -9.8344 -0.4022 -0.1206 0.9076
-12 4 6 0.0101 -11.8736 3.6599 5.8578 -0.8537 -0.2528 -0.4554
11 -4 -5 0.0118 11.4818 -3.9780 -5.2833 0.8778 0.2601 0.4023
10 2 -15 0.0636 10.1587 1.6357 -14.5353 0.0097 0.3331 0.9428
0 4 13 0.0236 -0.1891 3.9729 12.7468 -0.0256 -0.9960 -0.0857
-10 -5 4 0.0412 -9.9543 -4.9371 3.8516 0.0117 0.4980 -0.8671
-1 -4 -12 0.0308 -0.6603 -4.2370 -11.9284 0.0256 0.9996 0.0090
12 3 -3 0.0366 12.0077 2.9952 -3.0303 0.3118 -0.4448 0.8143

_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Chloroform'
