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

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

data_ACN@1-anti
_database_code_depnum_ccdc_archive 'CCDC 1417788'
_audit_update_record             
;
2015-08-09 deposited with the CCDC.
2015-08-26 downloaded from the CCDC.
;
_audit_creation_date             2015-07-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C68 H70 N4 O10, 7.7(C2 H3 N), 0.3(C H2 Cl2), 2(H2 O)'
_chemical_formula_sum            'C83.70 H97.70 Cl0.60 N11.70 O12'
_chemical_formula_weight         1480.90
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C80 H100 O20 Cl2'
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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.6914(4)
_cell_length_b                   13.3995(3)
_cell_length_c                   13.6649(5)
_cell_angle_alpha                105.227(3)
_cell_angle_beta                 99.554(3)
_cell_angle_gamma                102.607(2)
_cell_volume                     1958.27(11)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    7738
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      76.5160
_cell_measurement_theta_min      3.5400
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.698
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.3628
_exptl_crystal_size_mid          0.3119
_exptl_crystal_size_min          0.1031
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14442
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        66.750
_diffrn_reflns_theta_max         76.936
_diffrn_reflns_theta_min         3.450
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -48.00   33.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013   37.0000   60.0000 81

#__ type_ start__ end____ width___ exp.time_
  2 omega  -32.00   29.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013   37.0000 -150.0000 61

#__ type_ start__ end____ width___ exp.time_
  3 omega   34.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.9013 -125.0000  -60.0000 62

#__ type_ start__ end____ width___ exp.time_
  4 omega   40.00  103.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000   30.0000 63

#__ type_ start__ end____ width___ exp.time_
  5 omega   77.00  104.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000   60.0000 27

#__ type_ start__ end____ width___ exp.time_
  6 omega   50.00  123.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -130.0000   16.0000 73

#__ type_ start__ end____ width___ exp.time_
  7 omega   55.00   91.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -120.0000 36

#__ type_ start__ end____ width___ exp.time_
  8 omega   47.00   74.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -180.0000 27

#__ type_ start__ end____ width___ exp.time_
  9 omega   41.00   87.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -150.0000 46

#__ type_ start__ end____ width___ exp.time_
 10 omega   60.00   95.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000 -120.0000 35

#__ type_ start__ end____ width___ exp.time_
 11 omega   91.00  116.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000 -180.0000 25

#__ type_ start__ end____ width___ exp.time_
 12 omega   54.00   84.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  -60.0000 30

#__ type_ start__ end____ width___ exp.time_
 13 omega   47.00   84.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000    0.0000 37

#__ type_ start__ end____ width___ exp.time_
 14 omega   37.00  144.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000   90.0000 107

#__ type_ start__ end____ width___ exp.time_
 15 omega   42.00   91.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  150.0000 49

#__ type_ start__ end____ width___ exp.time_
 16 omega   32.00  160.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -15.0000    0.0000 128

#__ type_ start__ end____ width___ exp.time_
 17 omega   94.00  178.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000 -180.0000 84

#__ type_ start__ end____ width___ exp.time_
 18 omega   40.00   66.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 19 omega   38.00   69.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -60.0000 31

#__ type_ start__ end____ width___ exp.time_
 20 omega  -95.00  -21.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013  125.0000   60.0000 74

#__ type_ start__ end____ width___ exp.time_
 21 omega -117.00  -10.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013  -19.0000 -120.0000 107
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0865811000
_diffrn_orient_matrix_UB_12      -0.0054729000
_diffrn_orient_matrix_UB_13      -0.0736053000
_diffrn_orient_matrix_UB_21      -0.1084485000
_diffrn_orient_matrix_UB_22      -0.0396769000
_diffrn_orient_matrix_UB_23      -0.0950386000
_diffrn_orient_matrix_UB_31      0.0077718000
_diffrn_orient_matrix_UB_32      0.1172906000
_diffrn_orient_matrix_UB_33      0.0038852000
_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         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6943
_reflns_number_total             8014
_reflns_odcompleteness_completeness 99.96
_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 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    ?
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         8014
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0679
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1314P)²+0.6904P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1987
_refine_ls_wR_factor_ref         0.2084
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C39) = Uanis(C40)
3. Others
 Fixed Sof: H12(0.5) H12A(0.5) C13(0.5) H13A(0.5) H13B(0.5) C13B(0.5)
 H13C(0.5) H13D(0.5) H14A(0.5) H14B(0.5) H14C(0.5) H14D(0.5) H14E(0.5)
 H14F(0.5) C40(0.85) H40A(0.85) H40B(0.85) H40C(0.85) C41(0.85) N3(0.85)
 C39(0.15) H39A(0.15) H39B(0.15) Cl1(0.15) Cl3(0.15)
4.a Ternary CH refined with riding coordinates:
 C15(H15), C17(H17)
4.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C13B(H13C,H13D), C16(H16A,H16B), C28(H28A,
 H28B), C29(H29A,H29B), C30(H30A,H30B), C32(H32A,H32B), C34(H34A,H34B),
 C39(H39A,H39B)
4.c Me refined with riding coordinates:
 C14(H14A,H14B,H14C), C14(H14D,H14E,H14F)
4.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C12(H12), C12(H12A), C21(H21), C22(H22),
 C24(H24), C25(H25), N1(H1), N2(H2)
4.e Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C38(H38A,H38B,H38C), C36(H36A,H36B,H36C), C40(H40A,H40B,
 H40C), C9DA(H9DA,H9DB,H9DC)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
C1 C 0.53829(19) 0.62201(13) -0.06496(13) 0.0319(4) Uani 1 1 d . . . . .
C2 C 0.43599(18) 0.61275(13) -0.02073(13) 0.0301(4) Uani 1 1 d . . . . .
C3 C 0.45122(17) 0.63822(12) 0.09012(13) 0.0270(4) Uani 1 1 d . . . . .
C4 C 0.57041(18) 0.66847(13) 0.15091(13) 0.0311(4) Uani 1 1 d . . . . .
H4 H 0.5829 0.6833 0.2229 0.037 Uiso 1 1 calc R . . . .
C5 C 0.66837(19) 0.67674(14) 0.10787(15) 0.0349(4) Uani 1 1 d . . . . .
H5 H 0.7456 0.6960 0.1505 0.042 Uiso 1 1 calc R . . . .
C6 C 0.65273(19) 0.65621(13) -0.00093(15) 0.0338(4) Uani 1 1 d . . . . .
C7 C 0.3164(2) 0.57929(15) -0.08357(14) 0.0368(4) Uani 1 1 d . . . . .
H7 H 0.3043 0.5648 -0.1555 0.044 Uiso 1 1 calc R . . . .
C8 C 0.2193(2) 0.56811(16) -0.04065(15) 0.0401(4) Uani 1 1 d . . . . .
H8 H 0.1417 0.5438 -0.0834 0.048 Uiso 1 1 calc R . . . .
C9 C 0.23613(19) 0.59349(14) 0.06890(15) 0.0343(4) Uani 1 1 d . . . . .
C10 C 0.34875(17) 0.63188(12) 0.13522(13) 0.0284(4) Uani 1 1 d . . . . .
C11 C 0.8679(2) 0.6998(2) 0.0145(2) 0.0595(7) Uani 1 1 d . . . . .
H11A H 0.8805 0.6466 0.0485 0.071 Uiso 1 1 calc R . . . .
H11B H 0.8824 0.7682 0.0679 0.071 Uiso 1 1 calc R . . . .
C12 C 0.9526(3) 0.7099(2) -0.0572(3) 0.0797(11) Uani 1 1 d . . . . .
H12 H 0.9283 0.6689 -0.1273 0.096 Uiso 0.5 1 calc R . P A 1
H12A H 0.9816 0.6533 -0.0886 0.096 Uiso 0.5 1 calc R . P B 2
C13 C 1.0662(5) 0.7809(5) -0.0172(5) 0.0569(12) Uani 0.5 1 d . . P C 1
H13A H 1.1106 0.7712 -0.0714 0.068 Uiso 0.5 1 calc R . P C 1
H13B H 1.1070 0.7606 0.0392 0.068 Uiso 0.5 1 calc R . P C 1
C13B C 0.9833(5) 0.8077(4) -0.0726(4) 0.0550(12) Uani 0.5 1 d . . P C 2
H13C H 0.9104 0.8294 -0.0892 0.066 Uiso 0.5 1 calc R . P C 2
H13D H 1.0187 0.8004 -0.1326 0.066 Uiso 0.5 1 calc R . P C 2
C14 C 1.0753(4) 0.9004(3) 0.0240(3) 0.0832(10) Uani 1 1 d . . . . .
H14A H 1.1586 0.9407 0.0494 0.125 Uiso 0.5 1 calc R . P C 1
H14B H 1.0382 0.9232 -0.0313 0.125 Uiso 0.5 1 calc R . P C 1
H14C H 1.0347 0.9126 0.0798 0.125 Uiso 0.5 1 calc R . P C 1
H14D H 1.0922 0.9663 0.0069 0.125 Uiso 0.5 1 calc R . P C 2
H14E H 1.0404 0.9100 0.0835 0.125 Uiso 0.5 1 calc R . P C 2
H14F H 1.1488 0.8809 0.0400 0.125 Uiso 0.5 1 calc R . P C 2
C15 C 0.35886(17) 0.66851(13) 0.25307(13) 0.0288(4) Uani 1 1 d . . . . .
H15 H 0.4321 0.6585 0.2911 0.035 Uiso 1 1 calc R . . . .
C16 C 0.24580(19) 0.60294(14) 0.27393(15) 0.0356(4) Uani 1 1 d . . . . .
H16A H 0.2433 0.5273 0.2545 0.043 Uiso 1 1 calc R . . . .
H16B H 0.2464 0.6273 0.3475 0.043 Uiso 1 1 calc R . . . .
C17 C 0.13767(19) 0.61898(15) 0.20941(16) 0.0375(4) Uani 1 1 d . . . . .
H17 H 0.0651 0.5800 0.2249 0.045 Uiso 1 1 calc R . . . .
C18 C 0.55828(17) 1.07257(13) 0.39964(12) 0.0270(3) Uani 1 1 d . . . . .
C19 C 0.45350(17) 0.98331(13) 0.35467(12) 0.0270(4) Uani 1 1 d . . . . .
C20 C 0.46257(16) 0.87524(13) 0.33700(12) 0.0260(3) Uani 1 1 d . . . . .
C21 C 0.57748(17) 0.86226(13) 0.37265(13) 0.0278(3) Uani 1 1 d . . . . .
H21 H 0.5852 0.7933 0.3661 0.033 Uiso 1 1 calc R . . . .
C22 C 0.67787(17) 0.94838(14) 0.41652(14) 0.0304(4) Uani 1 1 d . . . . .
H22 H 0.7521 0.9371 0.4394 0.037 Uiso 1 1 calc R . . . .
C23 C 0.66934(17) 1.05442(13) 0.42728(13) 0.0289(4) Uani 1 1 d . . . . .
C24 C 0.33743(18) 0.99826(13) 0.32724(13) 0.0301(4) Uani 1 1 d . . . . .
H24 H 0.3298 1.0675 0.3357 0.036 Uiso 1 1 calc R . . . .
C25 C 0.23662(18) 0.91292(15) 0.28863(14) 0.0323(4) Uani 1 1 d . . . . .
H25 H 0.1609 0.9245 0.2743 0.039 Uiso 1 1 calc R . . . .
C26 C 0.24734(17) 0.80743(14) 0.27058(13) 0.0303(4) Uani 1 1 d . . . . .
C27 C 0.35731(17) 0.78607(13) 0.28876(12) 0.0272(3) Uani 1 1 d . . . . .
C28 C 0.88368(18) 1.12763(15) 0.50000(15) 0.0342(4) Uani 1 1 d . . . . .
H28A H 0.9055 1.0825 0.4420 0.041 Uiso 1 1 calc R . . . .
H28B H 0.8829 1.0934 0.5543 0.041 Uiso 1 1 calc R . . . .
C29 C 0.97265(18) 1.23790(15) 0.54121(15) 0.0352(4) Uani 1 1 d . . . . .
H29A H 0.9799 1.2669 0.4838 0.042 Uiso 1 1 calc R . . . .
H29B H 0.9421 1.2853 0.5906 0.042 Uiso 1 1 calc R . . . .
C30 C 1.0956(2) 1.23587(19) 0.5941(2) 0.0523(6) Uani 1 1 d . . . . .
H30A H 1.1272 1.1897 0.5444 0.063 Uiso 1 1 calc R . . . .
H30B H 1.0885 1.2060 0.6509 0.063 Uiso 1 1 calc R . . . .
C31 C 1.1824(2) 1.3475(2) 0.6364(2) 0.0577(6) Uani 1 1 d . . . . .
H31A H 1.1881 1.3780 0.5805 0.087 Uiso 1 1 calc GR . . . .
H31B H 1.2606 1.3433 0.6670 0.087 Uiso 1 1 calc GR . . . .
H31C H 1.1537 1.3922 0.6885 0.087 Uiso 1 1 calc GR . . . .
C32 C 0.54833(18) 1.18615(13) 0.41673(13) 0.0292(4) Uani 1 1 d . . . . .
H32A H 0.4845 1.1964 0.4522 0.035 Uiso 1 1 calc R . . . .
H32B H 0.6234 1.2370 0.4602 0.035 Uiso 1 1 calc R . . . .
C33 C 0.51669(17) 1.30179(13) 0.30635(13) 0.0285(4) Uani 1 1 d . . . . .
C34 C 0.4767(2) 1.40067(14) 0.18118(14) 0.0360(4) Uani 1 1 d . . . . .
H34A H 0.5457 1.4621 0.2183 0.043 Uiso 1 1 calc R . . . .
H34B H 0.4055 1.4169 0.2012 0.043 Uiso 1 1 calc R . . . .
C37 C 1.1389(3) 1.1832(3) 0.3219(3) 0.0683(8) Uani 1 1 d . . . . .
C38 C 1.2238(3) 1.2877(4) 0.3375(3) 0.0869(11) Uani 1 1 d . . . . .
H38A H 1.2842 1.3067 0.4012 0.130 Uiso 1 1 calc GR . . . .
H38B H 1.1810 1.3416 0.3416 0.130 Uiso 1 1 calc GR . . . .
H38C H 1.2618 1.2830 0.2800 0.130 Uiso 1 1 calc GR . . . .
N1 N 0.52207(16) 1.20519(11) 0.31616(11) 0.0314(3) Uani 1 1 d . . . . .
H1 H 0.5094 1.1522 0.2603 0.038 Uiso 1 1 calc R . . . .
N2 N 0.49475(18) 1.30555(12) 0.20760(12) 0.0366(4) Uani 1 1 d . . . . .
H2 H 0.4912 1.2493 0.1578 0.044 Uiso 1 1 calc R . . . .
N4 N 1.0715(4) 1.1019(3) 0.3104(3) 0.0968(10) Uani 1 1 d . . . . .
O1 O 0.74709(15) 0.66731(12) -0.04819(12) 0.0457(4) Uani 1 1 d . . . . .
O2 O 0.76730(13) 1.14251(10) 0.46633(11) 0.0360(3) Uani 1 1 d . . . . .
O3 O 0.12932(13) 0.57714(12) 0.10096(11) 0.0416(3) Uani 1 1 d . . . . .
O4 O 0.13809(13) 0.72888(10) 0.23196(11) 0.0367(3) Uani 1 1 d . . . . .
O5 O 0.53331(15) 1.38172(10) 0.38316(10) 0.0378(3) Uani 1 1 d . . . . .
C35 C 0.9310(3) 1.4162(2) 0.3592(3) 0.0633(7) Uani 1 1 d . . . . .
C36 C 0.8160(3) 1.3785(2) 0.3814(3) 0.0696(8) Uani 1 1 d . . . . .
H36A H 0.7537 1.3896 0.3335 0.104 Uiso 1 1 calc GR . . . .
H36B H 0.8172 1.4175 0.4515 0.104 Uiso 1 1 calc GR . . . .
H36C H 0.8005 1.3031 0.3739 0.104 Uiso 1 1 calc GR . . . .
N5 N 1.0232(3) 1.4494(3) 0.3471(3) 0.0966(11) Uani 1 1 d . . . . .
C40 C 0.7766(5) 0.9594(3) 0.1722(3) 0.0643(10) Uani 0.85 1 d . . P D 1
H40A H 0.7682 0.9230 0.0997 0.096 Uiso 0.85 1 calc GR . P D 1
H40B H 0.7240 0.9146 0.2002 0.096 Uiso 0.85 1 calc GR . P D 1
H40C H 0.8586 0.9740 0.2096 0.096 Uiso 0.85 1 calc GR . P D 1
C41 C 0.7448(5) 1.0596(5) 0.1829(4) 0.0600(12) Uani 0.85 1 d . . P D 1
N3 N 0.7159(5) 1.1316(5) 0.1877(4) 0.0816(15) Uani 0.85 1 d . . P D 1
C4DA C 0.3992(3) 0.98000(18) 0.06845(17) 0.0547(7) Uani 1 1 d . . . . .
C9DA C 0.3982(3) 0.8697(2) 0.0601(2) 0.0626(7) Uani 1 1 d . . . . .
H9DA H 0.3411 0.8222 -0.0025 0.094 Uiso 1 1 calc GR . . . .
H9DB H 0.3756 0.8529 0.1195 0.094 Uiso 1 1 calc GR . . . .
H9DC H 0.4771 0.8611 0.0578 0.094 Uiso 1 1 calc GR . . . .
N3DA N 0.4006(3) 1.06756(15) 0.07498(16) 0.0613(6) Uani 1 1 d . . . . .
C39 C 0.742(3) 0.980(3) 0.182(2) 0.0643(10) Uani 0.15 1 d . . P E 2
H39A H 0.7162 0.9432 0.1071 0.077 Uiso 0.15 1 calc R . P E 2
H39B H 0.6817 0.9492 0.2147 0.077 Uiso 0.15 1 calc R . P E 2
Cl1 Cl 0.8966(4) 0.9642(4) 0.2376(3) 0.0621(11) Uani 0.15 1 d . . P E 2
Cl3 Cl 0.7563(14) 1.1079(9) 0.2051(11) 0.083(3) Uani 0.15 1 d . . P E 2
O6 O 0.53865(17) 0.60296(12) 0.42640(12) 0.0441(4) Uani 1 1 d . . . . .
H6A H 0.534(3) 0.541(3) 0.409(2) 0.055(8) Uiso 1 1 d . . . . .
H6B H 0.504(2) 0.611(2) 0.483(2) 0.041(6) 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
C1 C2 1.423(3) . ?
C1 C6 1.378(3) . ?
C1 C34 1.509(2) 2_675 ?
C2 C3 1.433(2) . ?
C2 C7 1.421(3) . ?
C3 C4 1.410(3) . ?
C3 C10 1.432(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.368(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.412(3) . ?
C6 O1 1.368(2) . ?
C7 H7 0.9300 . ?
C7 C8 1.360(3) . ?
C8 H8 0.9300 . ?
C8 C9 1.415(3) . ?
C9 C10 1.372(3) . ?
C9 O3 1.383(2) . ?
C10 C15 1.531(2) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.515(3) . ?
C11 O1 1.432(3) . ?
C12 H12 0.9300 . ?
C12 H12A 0.9300 . ?
C12 C13 1.379(6) . ?
C12 C13B 1.361(6) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.525(7) . ?
C13B H13C 0.9700 . ?
C13B H13D 0.9700 . ?
C13B C14 1.589(7) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C14 H14D 0.9600 . ?
C14 H14E 0.9600 . ?
C14 H14F 0.9600 . ?
C15 H15 0.9800 . ?
C15 C16 1.533(2) . ?
C15 C27 1.527(2) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.507(3) . ?
C17 H17 0.9800 . ?
C17 O3 1.418(2) . ?
C17 O4 1.422(2) . ?
C18 C19 1.426(2) . ?
C18 C23 1.382(3) . ?
C18 C32 1.511(2) . ?
C19 C20 1.435(2) . ?
C19 C24 1.418(3) . ?
C20 C21 1.415(3) . ?
C20 C27 1.432(2) . ?
C21 H21 0.9300 . ?
C21 C22 1.371(3) . ?
C22 H22 0.9300 . ?
C22 C23 1.417(2) . ?
C23 O2 1.366(2) . ?
C24 H24 0.9300 . ?
C24 C25 1.365(3) . ?
C25 H25 0.9300 . ?
C25 C26 1.407(3) . ?
C26 C27 1.374(3) . ?
C26 O4 1.384(2) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.510(3) . ?
C28 O2 1.436(2) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.507(3) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.514(3) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 N1 1.458(2) . ?
C33 N1 1.349(2) . ?
C33 N2 1.347(2) . ?
C33 O5 1.240(2) . ?
C34 C1 1.509(2) 2_675 ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 N2 1.460(2) . ?
C37 C38 1.468(6) . ?
C37 N4 1.152(5) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
N1 H1 0.8600 . ?
N2 H2 0.8600 . ?
C35 C36 1.440(4) . ?
C35 N5 1.130(4) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C40 C41 1.448(7) . ?
C41 N3 1.080(8) . ?
C4DA C9DA 1.449(3) . ?
C4DA N3DA 1.149(3) . ?
C9DA H9DA 0.9600 . ?
C9DA H9DB 0.9600 . ?
C9DA H9DC 0.9600 . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 Cl1 1.92(3) . ?
C39 Cl3 1.62(3) . ?
O6 H6A 0.78(3) . ?
O6 H6B 0.92(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
C2 C1 C34 120.74(18) . 2_675 ?
C6 C1 C2 119.88(16) . . ?
C6 C1 C34 119.33(18) . 2_675 ?
C1 C2 C3 120.39(18) . . ?
C7 C2 C1 121.83(16) . . ?
C7 C2 C3 117.78(17) . . ?
C4 C3 C2 116.90(17) . . ?
C4 C3 C10 122.49(15) . . ?
C10 C3 C2 120.61(17) . . ?
C3 C4 H4 118.8 . . ?
C5 C4 C3 122.40(16) . . ?
C5 C4 H4 118.8 . . ?
C4 C5 H5 119.9 . . ?
C4 C5 C6 120.25(19) . . ?
C6 C5 H5 119.9 . . ?
C1 C6 C5 120.05(18) . . ?
O1 C6 C1 116.87(17) . . ?
O1 C6 C5 123.07(19) . . ?
C2 C7 H7 119.4 . . ?
C8 C7 C2 121.30(17) . . ?
C8 C7 H7 119.4 . . ?
C7 C8 H8 120.0 . . ?
C7 C8 C9 120.06(19) . . ?
C9 C8 H8 120.0 . . ?
C10 C9 C8 122.09(19) . . ?
C10 C9 O3 124.39(17) . . ?
O3 C9 C8 113.52(18) . . ?
C3 C10 C15 123.32(16) . . ?
C9 C10 C3 117.96(16) . . ?
C9 C10 C15 118.70(17) . . ?
H11A C11 H11B 108.5 . . ?
C12 C11 H11A 110.2 . . ?
C12 C11 H11B 110.2 . . ?
O1 C11 H11A 110.2 . . ?
O1 C11 H11B 110.2 . . ?
O1 C11 C12 107.5(3) . . ?
C11 C12 H12 120.5 . . ?
C11 C12 H12A 122.3 . . ?
C13 C12 C11 119.1(3) . . ?
C13 C12 H12 120.5 . . ?
C13B C12 C11 115.4(3) . . ?
C13B C12 H12A 122.3 . . ?
C12 C13 H13A 107.9 . . ?
C12 C13 H13B 107.9 . . ?
C12 C13 C14 117.8(4) . . ?
H13A C13 H13B 107.2 . . ?
C14 C13 H13A 107.9 . . ?
C14 C13 H13B 107.9 . . ?
C12 C13B H13C 108.6 . . ?
C12 C13B H13D 108.6 . . ?
C12 C13B C14 114.7(4) . . ?
H13C C13B H13D 107.6 . . ?
C14 C13B H13C 108.6 . . ?
C14 C13B H13D 108.6 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
C13B C14 H14D 109.5 . . ?
C13B C14 H14E 109.5 . . ?
C13B C14 H14F 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
H14D C14 H14E 109.5 . . ?
H14D C14 H14F 109.5 . . ?
H14E C14 H14F 109.5 . . ?
C10 C15 H15 110.9 . . ?
C10 C15 C16 107.83(15) . . ?
C16 C15 H15 110.9 . . ?
C27 C15 C10 109.59(13) . . ?
C27 C15 H15 110.9 . . ?
C27 C15 C16 106.57(14) . . ?
C15 C16 H16A 110.2 . . ?
C15 C16 H16B 110.2 . . ?
H16A C16 H16B 108.5 . . ?
C17 C16 C15 107.57(15) . . ?
C17 C16 H16A 110.2 . . ?
C17 C16 H16B 110.2 . . ?
C16 C17 H17 108.0 . . ?
O3 C17 C16 111.63(17) . . ?
O3 C17 H17 108.0 . . ?
O3 C17 O4 108.08(16) . . ?
O4 C17 C16 112.91(16) . . ?
O4 C17 H17 108.0 . . ?
C19 C18 C32 120.39(16) . . ?
C23 C18 C19 119.45(15) . . ?
C23 C18 C32 120.16(16) . . ?
C18 C19 C20 120.66(17) . . ?
C24 C19 C18 121.36(15) . . ?
C24 C19 C20 117.98(16) . . ?
C21 C20 C19 117.10(15) . . ?
C21 C20 C27 122.66(15) . . ?
C27 C20 C19 120.19(16) . . ?
C20 C21 H21 119.0 . . ?
C22 C21 C20 121.90(15) . . ?
C22 C21 H21 119.0 . . ?
C21 C22 H22 119.8 . . ?
C21 C22 C23 120.46(17) . . ?
C23 C22 H22 119.8 . . ?
C18 C23 C22 120.18(17) . . ?
O2 C23 C18 117.03(15) . . ?
O2 C23 C22 122.79(17) . . ?
C19 C24 H24 119.4 . . ?
C25 C24 C19 121.23(16) . . ?
C25 C24 H24 119.4 . . ?
C24 C25 H25 120.0 . . ?
C24 C25 C26 119.97(18) . . ?
C26 C25 H25 120.0 . . ?
C27 C26 C25 122.20(17) . . ?
C27 C26 O4 123.95(16) . . ?
O4 C26 C25 113.84(17) . . ?
C20 C27 C15 124.53(16) . . ?
C26 C27 C15 117.40(16) . . ?
C26 C27 C20 118.05(15) . . ?
H28A C28 H28B 108.6 . . ?
C29 C28 H28A 110.3 . . ?
C29 C28 H28B 110.3 . . ?
O2 C28 H28A 110.3 . . ?
O2 C28 H28B 110.3 . . ?
O2 C28 C29 106.91(15) . . ?
C28 C29 H29A 109.1 . . ?
C28 C29 H29B 109.1 . . ?
H29A C29 H29B 107.8 . . ?
C30 C29 C28 112.45(17) . . ?
C30 C29 H29A 109.1 . . ?
C30 C29 H29B 109.1 . . ?
C29 C30 H30A 109.3 . . ?
C29 C30 H30B 109.3 . . ?
C29 C30 C31 111.4(2) . . ?
H30A C30 H30B 108.0 . . ?
C31 C30 H30A 109.3 . . ?
C31 C30 H30B 109.3 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C18 C32 H32A 109.8 . . ?
C18 C32 H32B 109.8 . . ?
H32A C32 H32B 108.2 . . ?
N1 C32 C18 109.37(13) . . ?
N1 C32 H32A 109.8 . . ?
N1 C32 H32B 109.8 . . ?
N2 C33 N1 115.27(15) . . ?
O5 C33 N1 122.10(16) . . ?
O5 C33 N2 122.62(15) . . ?
C1 C34 H34A 110.0 2_675 . ?
C1 C34 H34B 110.0 2_675 . ?
H34A C34 H34B 108.4 . . ?
N2 C34 C1 108.38(13) . 2_675 ?
N2 C34 H34A 110.0 . . ?
N2 C34 H34B 110.0 . . ?
N4 C37 C38 179.2(4) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C32 N1 H1 118.4 . . ?
C33 N1 C32 123.26(14) . . ?
C33 N1 H1 118.4 . . ?
C33 N2 C34 123.04(14) . . ?
C33 N2 H2 118.5 . . ?
C34 N2 H2 118.5 . . ?
C6 O1 C11 119.11(18) . . ?
C23 O2 C28 118.81(14) . . ?
C9 O3 C17 116.76(15) . . ?
C26 O4 C17 118.94(16) . . ?
N5 C35 C36 176.3(4) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C41 C40 H40A 109.5 . . ?
C41 C40 H40B 109.5 . . ?
C41 C40 H40C 109.5 . . ?
N3 C41 C40 176.6(6) . . ?
N3DA C4DA C9DA 179.7(3) . . ?
C4DA C9DA H9DA 109.5 . . ?
C4DA C9DA H9DB 109.5 . . ?
C4DA C9DA H9DC 109.5 . . ?
H9DA C9DA H9DB 109.5 . . ?
H9DA C9DA H9DC 109.5 . . ?
H9DB C9DA H9DC 109.5 . . ?
H39A C39 H39B 108.5 . . ?
Cl1 C39 H39A 110.3 . . ?
Cl1 C39 H39B 110.3 . . ?
Cl3 C39 H39A 110.3 . . ?
Cl3 C39 H39B 110.3 . . ?
Cl3 C39 Cl1 107(2) . . ?
H6A O6 H6B 103(3) . . ?

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
C1 C2 C3 C4 -2.2(2) . . . . ?
C1 C2 C3 C10 178.27(14) . . . . ?
C1 C2 C7 C8 178.31(17) . . . . ?
C1 C6 O1 C11 -178.28(18) . . . . ?
C1 C34 N2 C33 176.77(19) 2_675 . . . ?
C2 C1 C6 C5 3.2(3) . . . . ?
C2 C1 C6 O1 -177.55(14) . . . . ?
C2 C3 C4 C5 1.9(2) . . . . ?
C2 C3 C10 C9 4.6(2) . . . . ?
C2 C3 C10 C15 -173.72(14) . . . . ?
C2 C7 C8 C9 2.2(3) . . . . ?
C3 C2 C7 C8 -2.2(3) . . . . ?
C3 C4 C5 C6 0.9(3) . . . . ?
C3 C10 C15 C16 -152.64(16) . . . . ?
C3 C10 C15 C27 91.74(19) . . . . ?
C4 C3 C10 C9 -174.94(16) . . . . ?
C4 C3 C10 C15 6.8(2) . . . . ?
C4 C5 C6 C1 -3.6(3) . . . . ?
C4 C5 C6 O1 177.27(16) . . . . ?
C5 C6 O1 C11 0.9(3) . . . . ?
C6 C1 C2 C3 -0.3(2) . . . . ?
C6 C1 C2 C7 179.09(16) . . . . ?
C7 C2 C3 C4 178.35(15) . . . . ?
C7 C2 C3 C10 -1.2(2) . . . . ?
C7 C8 C9 C10 1.4(3) . . . . ?
C7 C8 C9 O3 -179.38(17) . . . . ?
C8 C9 C10 C3 -4.7(3) . . . . ?
C8 C9 C10 C15 173.64(16) . . . . ?
C8 C9 O3 C17 -168.75(17) . . . . ?
C9 C10 C15 C16 29.1(2) . . . . ?
C9 C10 C15 C27 -86.55(19) . . . . ?
C10 C3 C4 C5 -178.55(15) . . . . ?
C10 C9 O3 C17 10.4(3) . . . . ?
C10 C15 C16 C17 -56.06(19) . . . . ?
C10 C15 C27 C20 -99.53(19) . . . . ?
C10 C15 C27 C26 78.65(19) . . . . ?
C11 C12 C13 C14 -63.9(6) . . . . ?
C11 C12 C13B C14 73.5(5) . . . . ?
C12 C11 O1 C6 -177.6(2) . . . . ?
C15 C16 C17 O3 64.03(19) . . . . ?
C15 C16 C17 O4 -58.0(2) . . . . ?
C16 C15 C27 C20 144.06(16) . . . . ?
C16 C15 C27 C26 -37.77(19) . . . . ?
C16 C17 O3 C9 -40.1(2) . . . . ?
C16 C17 O4 C26 26.5(2) . . . . ?
C18 C19 C20 C21 4.3(2) . . . . ?
C18 C19 C20 C27 -178.03(13) . . . . ?
C18 C19 C24 C25 -176.97(15) . . . . ?
C18 C23 O2 C28 177.47(15) . . . . ?
C18 C32 N1 C33 -175.01(17) . . . . ?
C19 C18 C23 C22 -3.6(2) . . . . ?
C19 C18 C23 O2 177.57(14) . . . . ?
C19 C18 C32 N1 -71.0(2) . . . . ?
C19 C20 C21 C22 -3.9(2) . . . . ?
C19 C20 C27 C15 171.41(14) . . . . ?
C19 C20 C27 C26 -6.8(2) . . . . ?
C19 C24 C25 C26 -3.1(3) . . . . ?
C20 C19 C24 C25 2.3(2) . . . . ?
C20 C21 C22 C23 -0.2(3) . . . . ?
C21 C20 C27 C15 -11.0(2) . . . . ?
C21 C20 C27 C26 170.79(15) . . . . ?
C21 C22 C23 C18 4.1(3) . . . . ?
C21 C22 C23 O2 -177.16(15) . . . . ?
C22 C23 O2 C28 -1.3(2) . . . . ?
C23 C18 C19 C20 -0.6(2) . . . . ?
C23 C18 C19 C24 178.62(15) . . . . ?
C23 C18 C32 N1 108.81(18) . . . . ?
C24 C19 C20 C21 -174.98(14) . . . . ?
C24 C19 C20 C27 2.7(2) . . . . ?
C24 C25 C26 C27 -1.2(3) . . . . ?
C24 C25 C26 O4 179.68(15) . . . . ?
C25 C26 C27 C15 -172.23(15) . . . . ?
C25 C26 C27 C20 6.1(2) . . . . ?
C25 C26 O4 C17 179.22(15) . . . . ?
C27 C15 C16 C17 61.53(18) . . . . ?
C27 C20 C21 C22 178.49(15) . . . . ?
C27 C26 O4 C17 0.1(2) . . . . ?
C28 C29 C30 C31 -179.0(2) . . . . ?
C29 C28 O2 C23 -178.66(15) . . . . ?
C32 C18 C19 C20 179.19(14) . . . . ?
C32 C18 C19 C24 -1.6(2) . . . . ?
C32 C18 C23 C22 176.59(14) . . . . ?
C32 C18 C23 O2 -2.2(2) . . . . ?
C34 C1 C2 C3 -177.72(14) 2_675 . . . ?
C34 C1 C2 C7 1.7(2) 2_675 . . . ?
C34 C1 C6 C5 -179.35(15) 2_675 . . . ?
C34 C1 C6 O1 -0.1(2) 2_675 . . . ?
N1 C33 N2 C34 175.22(19) . . . . ?
N2 C33 N1 C32 178.19(18) . . . . ?
O1 C11 C12 C13 152.2(4) . . . . ?
O1 C11 C12 C13B 87.8(4) . . . . ?
O2 C28 C29 C30 171.41(18) . . . . ?
O3 C9 C10 C3 176.17(15) . . . . ?
O3 C9 C10 C15 -5.5(3) . . . . ?
O3 C17 O4 C26 -97.50(19) . . . . ?
O4 C17 O3 C9 84.7(2) . . . . ?
O4 C26 C27 C15 6.8(2) . . . . ?
O4 C26 C27 C20 -174.90(14) . . . . ?
O5 C33 N1 C32 -0.4(3) . . . . ?
O5 C33 N2 C34 -6.2(3) . . . . ?

_shelx_SHELXL_version_number     2014/7
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
-2 0 -7 0.1322 -2.0000 -0.0000 -7.0000 0.3421 0.8822 -0.0427
2 -1 7 0.1378 2.0000 -1.0000 7.0000 -0.3366 -0.8425 -0.0746
1 -9 3 0.1609 1.0000 -9.0000 3.0000 -0.0850 -0.0365 -1.0362
-1 9 -2 0.1590 -1.0000 9.0000 -2.0000 0.0114 -0.0586 1.0401
-3 6 -7 0.1345 -3.0000 6.0000 -7.0000 0.2227 0.7526 0.6532
7 0 -2 0.0474 7.0000 0.0000 -2.0000 0.7533 -0.5691 0.0466
-7 0 2 0.0558 -7.0000 -0.0000 2.0000 -0.7533 0.5691 -0.0466
8 -1 -2 0.0559 8.0000 -1.0000 -2.0000 0.8453 -0.6378 -0.0629
-1 7 -7 0.1209 -1.0000 7.0000 -7.0000 0.3903 0.4960 0.7861
1 3 6 0.1829 1.0000 3.0000 6.0000 -0.3715 -0.7977 0.3830

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_acn@1-syn
_database_code_depnum_ccdc_archive 'CCDC 1417789'
_audit_update_record             
;
2015-08-09 deposited with the CCDC.
2015-08-26 downloaded from the CCDC.
;
_audit_creation_date             2015-08-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C68 H72 N4 O10, 2.5(C4 H6 N2), C H2 Cl2, 2(H2 O)'
_chemical_formula_sum            'C79 H93 Cl2 N9 O12'
_chemical_formula_weight         1431.52
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C80 H10 O20 N2'
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'

_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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   23.8532(2)
_cell_length_b                   16.58652(16)
_cell_length_c                   19.13712(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7571.45(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10737
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      76.2190
_cell_measurement_theta_min      3.5040
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.313
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3040
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.2921
_exptl_crystal_size_mid          0.2458
_exptl_crystal_size_min          0.1008
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26183
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.861
_diffrn_reflns_theta_min         3.526
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   87.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000   90.0000 91

#__ type_ start__ end____ width___ exp.time_
  2 omega   54.00   97.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000   30.0000 43

#__ type_ start__ end____ width___ exp.time_
  3 omega   52.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   60.0000 39

#__ type_ start__ end____ width___ exp.time_
  4 omega   42.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  -30.0000 57

#__ type_ start__ end____ width___ exp.time_
  5 omega   39.00  139.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000 -150.0000 100

#__ type_ start__ end____ width___ exp.time_
  6 omega   37.00   85.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -90.0000 48

#__ type_ start__ end____ width___ exp.time_
  7 omega  -36.00   32.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013   37.0000 -120.0000 68

#__ type_ start__ end____ width___ exp.time_
  8 omega  -28.00   33.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013   37.0000    0.0000 61

#__ type_ start__ end____ width___ exp.time_
  9 omega  -49.00   33.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013   37.0000  120.0000 82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0540203000
_diffrn_orient_matrix_UB_12      0.0437204000
_diffrn_orient_matrix_UB_13      -0.0226463000
_diffrn_orient_matrix_UB_21      -0.0322841000
_diffrn_orient_matrix_UB_22      0.0412142000
_diffrn_orient_matrix_UB_23      -0.0598714000
_diffrn_orient_matrix_UB_31      -0.0145858000
_diffrn_orient_matrix_UB_32      0.0708068000
_diffrn_orient_matrix_UB_33      0.0488084000
_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         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6922
_reflns_number_total             8120
_reflns_odcompleteness_completeness 99.77
_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 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    ?
_refine_diff_density_max         1.163
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         8120
_refine_ls_number_restraints     62
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0682
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1189P)²+4.8315P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1940
_refine_ls_wR_factor_ref         0.2042
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N6-C44
 1.15 with sigma of 0.01
 C44-C43
 1.45 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C45B) \\sim Ueq, Uanis(C46B) \\sim Ueq, Uanis(N7B) \\sim Ueq, Uanis(C45)
\\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C36) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N6) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C43) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: H12A(0.5) H12B(0.5) H31A(0.5) H31B(0.5) C33(0.5) H33A(0.5)
 H33B(0.5) C33B(0.5) H33C(0.5) H33D(0.5) C34(0.5) H34A(0.5) H34B(0.5) C34B(0.5)
 H34C(0.5) H34D(0.5) C35(0.5) H35A(0.5) H35B(0.5) C35B(0.5) H35C(0.5) H35D(0.5)
 C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5) C36B(0.5) H36D(0.5) H36E(0.5) H36F(0.5)
 O3(0.5) O3B(0.5) O5(0.5) O5B(0.5) H43A(0.5) H43B(0.5) H43C(0.5) H47A(0.5)
 H47B(0.5) Cl2(0.25) Cl2B(0.25) C45B(0.23) H45A(0.23) H45B(0.23) H45C(0.23)
 C46B(0.23) N7B(0.23) H41A(0.5) H41B(0.5) H41C(0.5) C37(0.5) C38(0.5) H38A(0.5)
 H38B(0.5) H38C(0.5) N3(0.5) C45(0.27) H45D(0.27) H45E(0.27) H45F(0.27)
 C46(0.27) N7(0.27) C39(0.5) C40(0.5) H40A(0.5) H40B(0.5) H40C(0.5) N4(0.5)
 Fixed X: N7B(0.95516)
 Fixed Y: C45B(0.25) C46B(0.25) N7B(0.25)
 Fixed Z: N7B(0.22208)
5.a Riding coordinates:
 C43(H43A,H43B,H43C)
5.b Ternary CH refined with riding coordinates:
 C11(H11), C13(H13), C30(H30), C32(H32)
5.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C18(H18A,
 H18B), C20(H20A,H20B), C31(H31A,H31B), C33(H33A,H33B), C33B(H33C,H33D),
 C34(H34A,H34B), C34B(H34C,H34D), C35(H35A,H35B), C35B(H35C,H35D), C47(H47A,
 H47B)
5.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C24(H24), C25(H25), C26(H26), C27(H27),
 N1(H1), N2(H2)
5.e Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C36(H36A,H36B,H36C), C36B(H36D,H36E,H36F), C45B(H45A,
 H45B,H45C), C41(H41A,H41B,H41C), C38(H38A,H38B,H38C), C45(H45D,H45E,H45F),
 C40(H40A,H40B,H40C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
C1 C 0.81670(8) 0.47883(11) 0.23289(9) 0.0273(4) Uani 1 1 d . . . . .
C2 C 0.76495(8) 0.43694(11) 0.24138(9) 0.0263(4) Uani 1 1 d . . . . .
C3 C 0.75117(7) 0.37040(10) 0.19712(9) 0.0235(3) Uani 1 1 d . . . . .
C4 C 0.78909(7) 0.35221(10) 0.14213(9) 0.0251(4) Uani 1 1 d . . . . .
H4 H 0.7799 0.3118 0.1104 0.030 Uiso 1 1 calc R . . . .
C5 C 0.83874(8) 0.39249(11) 0.13452(10) 0.0279(4) Uani 1 1 d . . . . .
H5 H 0.8631 0.3783 0.0987 0.034 Uiso 1 1 calc R . . . .
C6 C 0.85318(8) 0.45544(11) 0.18066(10) 0.0277(4) Uani 1 1 d . . . . .
C6CA C 0.84083(9) 0.45756(14) 0.63672(11) 0.0373(5) Uani 1 1 d . . . . .
C7 C 0.72576(9) 0.46024(11) 0.29342(10) 0.0317(4) Uani 1 1 d . . . . .
H7 H 0.7340 0.5031 0.3230 0.038 Uiso 1 1 calc R . . . .
C8 C 0.67616(9) 0.42030(12) 0.30044(11) 0.0346(4) Uani 1 1 d . . . . .
H8 H 0.6503 0.4373 0.3337 0.041 Uiso 1 1 calc R . . . .
C9 C 0.66371(8) 0.35358(12) 0.25781(10) 0.0292(4) Uani 1 1 d . . . . .
C10 C 0.70044(7) 0.32595(10) 0.20776(9) 0.0245(4) Uani 1 1 d . . . . .
C11 C 0.68453(10) 0.2500 0.16723(13) 0.0248(5) Uani 1 2 d S T P . .
H11 H 0.7023 0.2500 0.1211 0.030 Uiso 1 2 calc RS T P . .
C12 C 0.62063(11) 0.2500 0.15998(15) 0.0340(6) Uani 1 2 d S T P . .
H12A H 0.6084 0.2975 0.1346 0.041 Uiso 0.5 1 calc R . . . .
H12B H 0.6084 0.2025 0.1346 0.041 Uiso 0.5 1 calc R . . . .
C13 C 0.59624(11) 0.2500 0.23279(16) 0.0338(6) Uani 1 2 d S T P . .
H13 H 0.5553 0.2500 0.2286 0.041 Uiso 1 2 calc RS T P . .
C14 C 0.94439(8) 0.47062(13) 0.12904(11) 0.0346(4) Uani 1 1 d . . . . .
H14A H 0.9297 0.4651 0.0820 0.042 Uiso 1 1 calc R . . . .
H14B H 0.9583 0.4186 0.1443 0.042 Uiso 1 1 calc R . . . .
C15 C 0.99122(9) 0.53301(13) 0.13065(12) 0.0373(5) Uani 1 1 d . . . . .
H15A H 0.9782 0.5822 0.1086 0.045 Uiso 1 1 calc R . . . .
H15B H 1.0003 0.5455 0.1789 0.045 Uiso 1 1 calc R . . . .
C16 C 1.04347(9) 0.50431(14) 0.09391(12) 0.0394(5) Uani 1 1 d . . . . .
H16A H 1.0341 0.4887 0.0465 0.047 Uiso 1 1 calc R . . . .
H16B H 1.0581 0.4572 0.1178 0.047 Uiso 1 1 calc R . . . .
C17 C 1.08827(10) 0.56959(14) 0.09218(13) 0.0439(5) Uani 1 1 d . . . . .
H17A H 1.0746 0.6151 0.0663 0.066 Uiso 1 1 calc GR . . . .
H17B H 1.1214 0.5489 0.0701 0.066 Uiso 1 1 calc GR . . . .
H17C H 1.0970 0.5859 0.1391 0.066 Uiso 1 1 calc GR . . . .
C18 C 0.83135(9) 0.54781(12) 0.28093(10) 0.0324(4) Uani 1 1 d . . . . .
H18A H 0.8640 0.5759 0.2630 0.039 Uiso 1 1 calc R . . . .
H18B H 0.8004 0.5857 0.2825 0.039 Uiso 1 1 calc R . . . .
C19 C 0.82630(8) 0.55679(11) 0.40968(9) 0.0271(4) Uani 1 1 d . . . . .
C20 C 0.81673(8) 0.54913(12) 0.53783(9) 0.0298(4) Uani 1 1 d . . . . .
H20A H 0.7838 0.5827 0.5315 0.036 Uiso 1 1 calc R . . . .
H20B H 0.8461 0.5820 0.5583 0.036 Uiso 1 1 calc R . . . .
C21 C 0.80307(8) 0.48023(12) 0.58576(9) 0.0283(4) Uani 1 1 d . . . . .
C22 C 0.75186(8) 0.43703(11) 0.57855(9) 0.0247(4) Uani 1 1 d . . . . .
C23 C 0.73943(7) 0.37053(10) 0.62352(9) 0.0234(3) Uani 1 1 d . . . . .
C24 C 0.77859(8) 0.35316(11) 0.67713(9) 0.0267(4) Uani 1 1 d . . . . .
H24 H 0.7705 0.3124 0.7089 0.032 Uiso 1 1 calc R . . . .
C25 C 0.82785(8) 0.39463(13) 0.68349(11) 0.0346(4) Uani 1 1 d . . . . .
H25 H 0.8529 0.3813 0.7189 0.041 Uiso 1 1 calc R . . . .
C26 C 0.71158(8) 0.45844(11) 0.52698(9) 0.0281(4) Uani 1 1 d . . . . .
H26 H 0.7192 0.5003 0.4961 0.034 Uiso 1 1 calc R . . . .
C27 C 0.66205(8) 0.41840(12) 0.52226(10) 0.0298(4) Uani 1 1 d . . . . .
H27 H 0.6355 0.4345 0.4895 0.036 Uiso 1 1 calc R . . . .
C28 C 0.65051(8) 0.35297(11) 0.56633(10) 0.0271(4) Uani 1 1 d . . . . .
C29 C 0.68842(7) 0.32578(10) 0.61513(9) 0.0235(3) Uani 1 1 d . . . . .
C30 C 0.67364(10) 0.2500 0.65624(13) 0.0242(5) Uani 1 2 d S T P . .
H30 H 0.6928 0.2500 0.7016 0.029 Uiso 1 2 calc RS T P . .
C31 C 0.60988(11) 0.2500 0.66642(14) 0.0310(6) Uani 1 2 d S T P . .
H31A H 0.5984 0.2025 0.6923 0.037 Uiso 0.5 1 calc R . . . .
H31B H 0.5984 0.2975 0.6923 0.037 Uiso 0.5 1 calc R . . . .
C32 C 0.58344(11) 0.2500 0.59498(15) 0.0307(6) Uani 1 2 d S T P . .
H32 H 0.5426 0.2500 0.6010 0.037 Uiso 1 2 calc RS T P . .
C33 C 0.9304(6) 0.4830(7) 0.6905(8) 0.0349(19) Uani 0.5 1 d . . . A 1
H33A H 0.9409 0.4284 0.6780 0.042 Uiso 0.5 1 calc R . . A 1
H33B H 0.9183 0.4832 0.7389 0.042 Uiso 0.5 1 calc R . . A 1
C33B C 0.9371(7) 0.4622(8) 0.6784(8) 0.046(3) Uani 0.5 1 d . . . B 2
H33C H 0.9407 0.4039 0.6799 0.055 Uiso 0.5 1 calc R . . B 2
H33D H 0.9274 0.4813 0.7247 0.055 Uiso 0.5 1 calc R . . B 2
C34 C 0.97946(19) 0.5386(3) 0.6813(3) 0.0373(9) Uani 0.5 1 d . . . A 1
H34A H 1.0102 0.5197 0.7101 0.045 Uiso 0.5 1 calc R . . A 1
H34B H 0.9691 0.5919 0.6977 0.045 Uiso 0.5 1 calc R . . A 1
C34B C 0.9919(2) 0.5006(5) 0.6538(4) 0.0557(14) Uani 0.5 1 d . . . B 2
H34C H 1.0208 0.4888 0.6878 0.067 Uiso 0.5 1 calc R . . B 2
H34D H 1.0028 0.4755 0.6101 0.067 Uiso 0.5 1 calc R . . B 2
C35 C 0.9999(2) 0.5452(4) 0.6049(3) 0.0562(15) Uani 0.5 1 d . . . A 1
H35A H 0.9711 0.5726 0.5781 0.067 Uiso 0.5 1 calc R . . A 1
H35B H 1.0330 0.5790 0.6042 0.067 Uiso 0.5 1 calc R . . A 1
C35B C 0.9896(2) 0.5868(4) 0.6435(4) 0.0636(16) Uani 0.5 1 d . . . B 2
H35C H 0.9783 0.6119 0.6871 0.076 Uiso 0.5 1 calc R . . B 2
H35D H 0.9608 0.5986 0.6092 0.076 Uiso 0.5 1 calc R . . B 2
C36 C 1.0132(3) 0.4699(7) 0.5695(5) 0.103(3) Uani 0.5 1 d . U . A 1
H36A H 1.0293 0.4814 0.5247 0.155 Uiso 0.5 1 calc GR . . A 1
H36B H 0.9796 0.4388 0.5635 0.155 Uiso 0.5 1 calc GR . . A 1
H36C H 1.0396 0.4398 0.5971 0.155 Uiso 0.5 1 calc GR . . A 1
C36B C 1.0446(2) 0.6253(4) 0.6193(4) 0.0701(18) Uani 0.5 1 d . . . B 2
H36D H 1.0570 0.5997 0.5770 0.105 Uiso 0.5 1 calc GR . . B 2
H36E H 1.0726 0.6187 0.6548 0.105 Uiso 0.5 1 calc GR . . B 2
H36F H 1.0388 0.6818 0.6108 0.105 Uiso 0.5 1 calc GR . . B 2
N1 N 0.84312(8) 0.51832(10) 0.35141(8) 0.0331(4) Uani 1 1 d . . . . .
H1 H 0.8617 0.4742 0.3559 0.040 Uiso 1 1 calc R . . . .
N2 N 0.83525(7) 0.51800(10) 0.47031(8) 0.0303(4) Uani 1 1 d . . . . .
H2 H 0.8527 0.4727 0.4693 0.036 Uiso 1 1 calc R . . . .
O1 O 0.61209(6) 0.31946(9) 0.27130(8) 0.0366(3) Uani 1 1 d . . . . .
O2 O 0.90195(6) 0.49878(9) 0.17510(8) 0.0376(3) Uani 1 1 d . . . . .
O3 O 0.7937(2) 0.6176(4) 0.4064(3) 0.0310(11) Uani 0.5 1 d . . . C 1
O3B O 0.8149(3) 0.6290(4) 0.4087(4) 0.0393(13) Uani 0.5 1 d . . . C 2
O4 O 0.59817(6) 0.31911(8) 0.55562(8) 0.0332(3) Uani 1 1 d . . . . .
O5 O 0.8866(2) 0.5101(3) 0.6468(3) 0.0280(9) Uani 0.5 1 d . . . A 1
O5B O 0.8950(2) 0.4856(3) 0.6286(3) 0.0431(12) Uani 0.5 1 d . . . B 2
C43 C 0.6620(2) 0.7500 0.3943(3) 0.0812(15) Uani 1 2 d DS TU P . .
H43A H 0.6920 0.7878 0.3881 0.122 Uiso 0.5 1 d R . . D -1
H43B H 0.6772 0.6970 0.4013 0.122 Uiso 0.5 1 d R . . D -1
H43C H 0.6401 0.7651 0.4343 0.122 Uiso 0.5 1 d R . . D -1
C44 C 0.6266(3) 0.7500 0.3324(3) 0.0719(13) Uani 1 2 d DS TU P . .
N6 N 0.5992(3) 0.7500 0.2891(3) 0.1045(18) Uani 1 2 d DS TU P . .
C47 C 0.9245(3) 0.7500 0.4013(5) 0.121(3) Uani 1 2 d S T P . .
H47A H 0.9009 0.7972 0.3967 0.145 Uiso 0.5 1 calc R . . E 1
H47B H 0.9009 0.7028 0.3967 0.145 Uiso 0.5 1 calc R . . E 1
Cl1 Cl 0.97627(8) 0.7500 0.33083(9) 0.1122(6) Uani 1 2 d S T P F .
Cl2 Cl 0.9553(3) 0.7500 0.4851(3) 0.137(4) Uani 0.5 2 d S T P F 1
Cl2B Cl 0.9593(4) 0.7013(6) 0.4684(4) 0.118(3) Uani 0.25 1 d . . . F -1
C45B C 0.8575(7) 0.2500 0.2850(10) 0.026(5) Uani 0.23 1 d S TU P G -1
H45A H 0.8611 0.2715 0.3314 0.039 Uiso 0.23 1 calc GR . . G -1
H45B H 0.8435 0.1958 0.2875 0.039 Uiso 0.23 1 calc GR . . G -1
H45C H 0.8319 0.2827 0.2586 0.039 Uiso 0.23 1 calc GR . . G -1
C46B C 0.9140(8) 0.2500 0.2498(10) 0.040(5) Uani 0.23 1 d S TU P G -1
N7B N 0.9552 0.2500 0.2221 0.068(5) Uani 0.23 1 d S TU P G -1
C41 C 0.53842(15) 0.2500 0.40771(17) 0.0468(8) Uani 1 2 d S T P . .
H41A H 0.5673 0.2267 0.4361 0.070 Uiso 0.5 1 calc GR . . H -1
H41B H 0.5484 0.3044 0.3959 0.070 Uiso 0.5 1 calc GR . . H -1
H41C H 0.5342 0.2189 0.3657 0.070 Uiso 0.5 1 calc GR . . H -1
C42 C 0.48624(16) 0.2500 0.44583(19) 0.0502(8) Uani 1 2 d S T P . .
N5 N 0.44538(19) 0.2500 0.4757(2) 0.0877(14) Uani 1 2 d S T P . .
C37 C 0.7711(2) 0.3027(3) 0.4208(2) 0.0401(10) Uani 0.5 1 d . . . I -1
C38 C 0.7253(3) 0.2459(13) 0.4184(3) 0.066(2) Uani 0.5 1 d . . . I -1
H38A H 0.7081 0.2476 0.3730 0.099 Uiso 0.5 1 calc GR . . I -1
H38B H 0.6980 0.2598 0.4533 0.099 Uiso 0.5 1 calc GR . . I -1
H38C H 0.7392 0.1926 0.4272 0.099 Uiso 0.5 1 calc GR . . I -1
N3 N 0.80700(19) 0.3465(2) 0.4229(2) 0.0469(9) Uani 0.5 1 d . . . I -1
C45 C 0.8638(8) 0.2290(19) 0.2871(12) 0.040(4) Uani 0.27 1 d . U . J -2
H45D H 0.8446 0.2751 0.2687 0.060 Uiso 0.27 1 calc GR . . J -2
H45E H 0.8699 0.2360 0.3363 0.060 Uiso 0.27 1 calc GR . . J -2
H45F H 0.8416 0.1815 0.2794 0.060 Uiso 0.27 1 calc GR . . J -2
C46 C 0.9147(6) 0.2207(10) 0.2538(7) 0.029(3) Uani 0.27 1 d . U . J -2
N7 N 0.9572(3) 0.2108(7) 0.2295(5) 0.049(3) Uani 0.27 1 d . U . J -2
C39 C 0.88224(19) 0.2963(3) 0.5024(3) 0.0438(10) Uani 0.5 1 d . . . K -2
C40 C 0.8845(2) 0.2348(4) 0.5569(3) 0.052(2) Uani 0.5 1 d . . . K -2
H40A H 0.9017 0.1869 0.5386 0.078 Uiso 0.5 1 calc GR . . K -2
H40B H 0.8472 0.2226 0.5724 0.078 Uiso 0.5 1 calc GR . . K -2
H40C H 0.9062 0.2544 0.5956 0.078 Uiso 0.5 1 calc GR . . K -2
N4 N 0.88015(19) 0.3434(3) 0.4592(3) 0.0537(10) Uani 0.5 1 d . . . K -2
O6 O 0.77497(15) 0.7500 0.50042(12) 0.0599(8) Uani 1 2 d S T P . .
H6 H 0.7855(14) 0.7079(19) 0.4725(17) 0.065(9) Uiso 1 1 d . . . . .
O7 O 0.78489(12) 0.7500 0.31665(11) 0.0476(6) Uani 1 2 d S T P . .
H7A H 0.7911(11) 0.7098(17) 0.3453(15) 0.047(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
C1 C2 1.426(3) . ?
C1 C6 1.381(3) . ?
C1 C18 1.509(3) . ?
C2 C3 1.430(2) . ?
C2 C7 1.419(3) . ?
C3 C4 1.420(2) . ?
C3 C10 1.431(2) . ?
C4 H4 0.9300 . ?
C4 C5 1.367(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.410(3) . ?
C6 O2 1.372(2) . ?
C6CA C21 1.380(3) . ?
C6CA C25 1.409(3) . ?
C6CA O5 1.410(6) . ?
C6CA O5B 1.381(6) . ?
C7 H7 0.9300 . ?
C7 C8 1.363(3) . ?
C8 H8 0.9300 . ?
C8 C9 1.407(3) . ?
C9 C10 1.377(2) . ?
C9 O1 1.379(2) . ?
C10 C11 1.527(2) . ?
C11 C10 1.527(2) 8_565 ?
C11 H11 0.9800 . ?
C11 C12 1.531(3) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C13 1.510(4) . ?
C13 H13 0.9800 . ?
C13 O1 1.419(2) . ?
C13 O1 1.419(2) 8_565 ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.523(3) . ?
C14 O2 1.421(2) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.508(3) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.522(3) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 N1 1.462(2) . ?
C19 N1 1.346(2) . ?
C19 N2 1.344(2) . ?
C19 O3 1.275(7) . ?
C19 O3B 1.229(7) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.501(2) . ?
C20 N2 1.460(2) . ?
C21 C22 1.423(3) . ?
C22 C23 1.430(2) . ?
C22 C26 1.422(2) . ?
C23 C24 1.417(2) . ?
C23 C29 1.434(2) . ?
C24 H24 0.9300 . ?
C24 C25 1.367(3) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C26 C27 1.358(3) . ?
C27 H27 0.9300 . ?
C27 C28 1.402(3) . ?
C28 C29 1.376(3) . ?
C28 O4 1.384(2) . ?
C29 C30 1.524(2) . ?
C30 C29 1.524(2) 8_565 ?
C30 H30 0.9800 . ?
C30 C31 1.533(3) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.506(4) . ?
C32 H32 0.9800 . ?
C32 O4 1.416(2) . ?
C32 O4 1.416(2) 8_565 ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C34 1.501(16) . ?
C33 O5 1.413(17) . ?
C33B H33C 0.9700 . ?
C33B H33D 0.9700 . ?
C33B C34B 1.527(17) . ?
C33B O5B 1.439(18) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C35 1.544(8) . ?
C34B H34C 0.9700 . ?
C34B H34D 0.9700 . ?
C34B C35B 1.445(10) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C35 C36 1.455(13) . ?
C35B H35C 0.9700 . ?
C35B H35D 0.9700 . ?
C35B C36B 1.533(8) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C36B H36D 0.9600 . ?
C36B H36E 0.9600 . ?
C36B H36F 0.9600 . ?
N1 H1 0.8600 . ?
N2 H2 0.8600 . ?
C43 H43A 0.9601 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C43 C44 1.453(7) . ?
C44 N6 1.056(6) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C47 Cl1 1.828(8) . ?
C47 Cl2 1.764(10) . ?
C47 Cl2B 1.730(10) . ?
Cl2 Cl2B 0.874(8) . ?
C45B H45A 0.9600 . ?
C45B H45B 0.9600 . ?
C45B H45C 0.9600 . ?
C45B C46B 1.51(3) . ?
C46B N7B 1.116(19) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C41 C42 1.443(5) . ?
C42 N5 1.130(5) . ?
C37 C38 1.444(12) . ?
C37 N3 1.124(7) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C45 H45D 0.9600 . ?
C45 H45E 0.9600 . ?
C45 H45F 0.9600 . ?
C45 C46 1.38(2) . ?
C46 N7 1.128(16) . ?
C39 C40 1.459(8) . ?
C39 N4 1.139(7) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
O6 H6 0.91(3) . ?
O7 H7A 0.88(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
C2 C1 C18 120.03(16) . . ?
C6 C1 C2 119.42(17) . . ?
C6 C1 C18 120.55(17) . . ?
C1 C2 C3 120.51(16) . . ?
C7 C2 C1 121.16(17) . . ?
C7 C2 C3 118.33(17) . . ?
C2 C3 C10 120.51(16) . . ?
C4 C3 C2 117.17(16) . . ?
C4 C3 C10 122.31(16) . . ?
C3 C4 H4 119.1 . . ?
C5 C4 C3 121.79(16) . . ?
C5 C4 H4 119.1 . . ?
C4 C5 H5 119.8 . . ?
C4 C5 C6 120.43(16) . . ?
C6 C5 H5 119.8 . . ?
C1 C6 C5 120.49(17) . . ?
O2 C6 C1 116.32(16) . . ?
O2 C6 C5 123.13(16) . . ?
C21 C6CA C25 120.48(18) . . ?
C21 C6CA O5 115.7(3) . . ?
C21 C6CA O5B 116.1(3) . . ?
C25 C6CA O5 122.7(3) . . ?
O5B C6CA C25 121.7(3) . . ?
C2 C7 H7 119.7 . . ?
C8 C7 C2 120.57(18) . . ?
C8 C7 H7 119.7 . . ?
C7 C8 H8 119.7 . . ?
C7 C8 C9 120.58(17) . . ?
C9 C8 H8 119.7 . . ?
C10 C9 C8 122.07(18) . . ?
C10 C9 O1 124.18(18) . . ?
O1 C9 C8 113.75(16) . . ?
C3 C10 C11 124.24(16) . . ?
C9 C10 C3 117.75(17) . . ?
C9 C10 C11 118.02(17) . . ?
C10 C11 C10 111.1(2) . 8_565 ?
C10 C11 H11 110.5 8_565 . ?
C10 C11 H11 110.5 . . ?
C10 C11 C12 107.07(13) . . ?
C10 C11 C12 107.07(13) 8_565 . ?
C12 C11 H11 110.5 . . ?
C11 C12 H12A 110.2 . . ?
C11 C12 H12B 110.2 . . ?
H12A C12 H12B 108.5 . . ?
C13 C12 C11 107.5(2) . . ?
C13 C12 H12A 110.2 . . ?
C13 C12 H12B 110.2 . . ?
C12 C13 H13 108.0 . . ?
O1 C13 C12 112.12(14) 8_565 . ?
O1 C13 C12 112.12(14) . . ?
O1 C13 H13 108.0 8_565 . ?
O1 C13 H13 108.0 . . ?
O1 C13 O1 108.6(2) 8_565 . ?
H14A C14 H14B 108.6 . . ?
C15 C14 H14A 110.4 . . ?
C15 C14 H14B 110.4 . . ?
O2 C14 H14A 110.4 . . ?
O2 C14 H14B 110.4 . . ?
O2 C14 C15 106.66(16) . . ?
C14 C15 H15A 109.1 . . ?
C14 C15 H15B 109.1 . . ?
H15A C15 H15B 107.8 . . ?
C16 C15 C14 112.48(17) . . ?
C16 C15 H15A 109.1 . . ?
C16 C15 H15B 109.1 . . ?
C15 C16 H16A 109.3 . . ?
C15 C16 H16B 109.3 . . ?
C15 C16 C17 111.47(19) . . ?
H16A C16 H16B 108.0 . . ?
C17 C16 H16A 109.3 . . ?
C17 C16 H16B 109.3 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C1 C18 H18A 109.5 . . ?
C1 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
N1 C18 C1 110.66(16) . . ?
N1 C18 H18A 109.5 . . ?
N1 C18 H18B 109.5 . . ?
N2 C19 N1 116.17(17) . . ?
O3 C19 N1 121.0(3) . . ?
O3 C19 N2 121.2(3) . . ?
O3B C19 N1 121.0(4) . . ?
O3B C19 N2 121.0(4) . . ?
H20A C20 H20B 108.2 . . ?
C21 C20 H20A 109.7 . . ?
C21 C20 H20B 109.7 . . ?
N2 C20 H20A 109.7 . . ?
N2 C20 H20B 109.7 . . ?
N2 C20 C21 109.70(16) . . ?
C6CA C21 C20 119.83(17) . . ?
C6CA C21 C22 119.46(17) . . ?
C22 C21 C20 120.70(16) . . ?
C21 C22 C23 120.54(16) . . ?
C26 C22 C21 121.43(16) . . ?
C26 C22 C23 118.03(16) . . ?
C22 C23 C29 120.51(16) . . ?
C24 C23 C22 117.10(16) . . ?
C24 C23 C29 122.36(16) . . ?
C23 C24 H24 119.0 . . ?
C25 C24 C23 121.93(17) . . ?
C25 C24 H24 119.0 . . ?
C6CA C25 H25 119.8 . . ?
C24 C25 C6CA 120.33(17) . . ?
C24 C25 H25 119.8 . . ?
C22 C26 H26 119.6 . . ?
C27 C26 C22 120.78(17) . . ?
C27 C26 H26 119.6 . . ?
C26 C27 H27 119.7 . . ?
C26 C27 C28 120.61(17) . . ?
C28 C27 H27 119.7 . . ?
C29 C28 C27 122.22(17) . . ?
C29 C28 O4 124.08(17) . . ?
O4 C28 C27 113.70(16) . . ?
C23 C29 C30 124.41(16) . . ?
C28 C29 C23 117.64(16) . . ?
C28 C29 C30 117.95(17) . . ?
C29 C30 C29 111.1(2) . 8_565 ?
C29 C30 H30 110.4 . . ?
C29 C30 H30 110.4 8_565 . ?
C29 C30 C31 107.16(14) . . ?
C29 C30 C31 107.16(14) 8_565 . ?
C31 C30 H30 110.4 . . ?
C30 C31 H31A 110.2 . . ?
C30 C31 H31B 110.2 . . ?
H31A C31 H31B 108.5 . . ?
C32 C31 C30 107.5(2) . . ?
C32 C31 H31A 110.2 . . ?
C32 C31 H31B 110.2 . . ?
C31 C32 H32 108.0 . . ?
O4 C32 C31 112.28(14) . . ?
O4 C32 C31 112.29(14) 8_565 . ?
O4 C32 H32 108.0 . . ?
O4 C32 H32 108.0 8_565 . ?
O4 C32 O4 108.1(2) 8_565 . ?
H33A C33 H33B 108.4 . . ?
C34 C33 H33A 110.1 . . ?
C34 C33 H33B 110.1 . . ?
O5 C33 H33A 110.1 . . ?
O5 C33 H33B 110.1 . . ?
O5 C33 C34 108.1(10) . . ?
H33C C33B H33D 108.7 . . ?
C34B C33B H33C 110.5 . . ?
C34B C33B H33D 110.5 . . ?
O5B C33B H33C 110.5 . . ?
O5B C33B H33D 110.5 . . ?
O5B C33B C34B 106.3(10) . . ?
C33 C34 H34A 108.8 . . ?
C33 C34 H34B 108.8 . . ?
C33 C34 C35 113.6(7) . . ?
H34A C34 H34B 107.7 . . ?
C35 C34 H34A 108.8 . . ?
C35 C34 H34B 108.8 . . ?
C33B C34B H34C 108.5 . . ?
C33B C34B H34D 108.5 . . ?
H34C C34B H34D 107.5 . . ?
C35B C34B C33B 115.0(7) . . ?
C35B C34B H34C 108.5 . . ?
C35B C34B H34D 108.5 . . ?
C34 C35 H35A 108.1 . . ?
C34 C35 H35B 108.1 . . ?
H35A C35 H35B 107.3 . . ?
C36 C35 C34 116.7(6) . . ?
C36 C35 H35A 108.1 . . ?
C36 C35 H35B 108.1 . . ?
C34B C35B H35C 108.5 . . ?
C34B C35B H35D 108.5 . . ?
C34B C35B C36B 114.9(5) . . ?
H35C C35B H35D 107.5 . . ?
C36B C35B H35C 108.5 . . ?
C36B C35B H35D 108.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35B C36B H36D 109.5 . . ?
C35B C36B H36E 109.5 . . ?
C35B C36B H36F 109.5 . . ?
H36D C36B H36E 109.5 . . ?
H36D C36B H36F 109.5 . . ?
H36E C36B H36F 109.5 . . ?
C18 N1 H1 118.4 . . ?
C19 N1 C18 123.26(17) . . ?
C19 N1 H1 118.4 . . ?
C19 N2 C20 123.15(16) . . ?
C19 N2 H2 118.4 . . ?
C20 N2 H2 118.4 . . ?
C9 O1 C13 118.28(16) . . ?
C6 O2 C14 118.69(15) . . ?
C28 O4 C32 118.25(16) . . ?
C6CA O5 C33 117.2(7) . . ?
C6CA O5B C33B 119.2(7) . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C44 C43 H43A 109.4 . . ?
C44 C43 H43B 109.5 . . ?
C44 C43 H43C 109.5 . . ?
N6 C44 C43 177.2(7) . . ?
H47A C47 H47B 107.8 . . ?
Cl1 C47 H47A 109.0 . . ?
Cl1 C47 H47B 109.0 . . ?
Cl2 C47 H47A 109.0 . . ?
Cl2 C47 H47B 109.0 . . ?
Cl2 C47 Cl1 113.0(4) . . ?
Cl2B C47 H47A 136.4 . . ?
Cl2B C47 H47B 88.3 . . ?
Cl2B C47 Cl1 103.0(4) . . ?
Cl2B C47 Cl2 29.0(3) . . ?
Cl2B Cl2 C47 73.4(8) . . ?
Cl2 Cl2B C47 77.7(8) . . ?
H45A C45B H45B 109.5 . . ?
H45A C45B H45C 109.5 . . ?
H45B C45B H45C 109.5 . . ?
C46B C45B H45A 109.5 . . ?
C46B C45B H45B 109.5 . . ?
C46B C45B H45C 109.5 . . ?
N7B C46B C45B 178.1(18) . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C42 C41 H41A 109.5 . . ?
C42 C41 H41B 109.5 . . ?
C42 C41 H41C 109.5 . . ?
N5 C42 C41 180.0(5) . . ?
N3 C37 C38 179.5(9) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
H45D C45 H45E 109.5 . . ?
H45D C45 H45F 109.5 . . ?
H45E C45 H45F 109.5 . . ?
C46 C45 H45D 109.5 . . ?
C46 C45 H45E 109.5 . . ?
C46 C45 H45F 109.5 . . ?
N7 C46 C45 176.1(18) . . ?
N4 C39 C40 178.8(6) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -4.3(3) . . . . ?
C1 C2 C3 C10 177.03(16) . . . . ?
C1 C2 C7 C8 179.22(18) . . . . ?
C1 C6 O2 C14 171.30(17) . . . . ?
C1 C18 N1 C19 -140.28(19) . . . . ?
C2 C1 C6 C5 2.1(3) . . . . ?
C2 C1 C6 O2 179.47(16) . . . . ?
C2 C1 C18 N1 69.9(2) . . . . ?
C2 C3 C4 C5 4.6(3) . . . . ?
C2 C3 C10 C9 5.3(3) . . . . ?
C2 C3 C10 C11 -174.70(17) . . . . ?
C2 C7 C8 C9 2.1(3) . . . . ?
C3 C2 C7 C8 -0.4(3) . . . . ?
C3 C4 C5 C6 -1.6(3) . . . . ?
C3 C10 C11 C10 96.3(2) . . . 8_565 ?
C3 C10 C11 C12 -147.13(18) . . . . ?
C4 C3 C10 C9 -173.30(17) . . . . ?
C4 C3 C10 C11 6.7(3) . . . . ?
C4 C5 C6 C1 -1.9(3) . . . . ?
C4 C5 C6 O2 -179.05(18) . . . . ?
C5 C6 O2 C14 -11.4(3) . . . . ?
C6 C1 C2 C3 1.1(3) . . . . ?
C6 C1 C2 C7 -178.58(17) . . . . ?
C6 C1 C18 N1 -109.8(2) . . . . ?
C6CA C21 C22 C23 -0.1(3) . . . . ?
C6CA C21 C22 C26 179.73(19) . . . . ?
C7 C2 C3 C4 175.34(16) . . . . ?
C7 C2 C3 C10 -3.3(3) . . . . ?
C7 C8 C9 C10 0.0(3) . . . . ?
C7 C8 C9 O1 179.79(18) . . . . ?
C8 C9 C10 C3 -3.6(3) . . . . ?
C8 C9 C10 C11 176.35(18) . . . . ?
C8 C9 O1 C13 -177.87(18) . . . . ?
C9 C10 C11 C10 -83.7(2) . . . 8_565 ?
C9 C10 C11 C12 32.9(2) . . . . ?
C10 C3 C4 C5 -176.74(17) . . . . ?
C10 C9 O1 C13 1.9(3) . . . . ?
C10 C11 C12 C13 59.64(13) 8_565 . . . ?
C10 C11 C12 C13 -59.64(13) . . . . ?
C11 C12 C13 O1 -61.21(16) . . . 8_565 ?
C11 C12 C13 O1 61.21(16) . . . . ?
C12 C13 O1 C9 -31.6(3) . . . . ?
C14 C15 C16 C17 176.36(19) . . . . ?
C15 C14 O2 C6 176.63(17) . . . . ?
C18 C1 C2 C3 -178.67(16) . . . . ?
C18 C1 C2 C7 1.7(3) . . . . ?
C18 C1 C6 C5 -178.16(17) . . . . ?
C18 C1 C6 O2 -0.8(3) . . . . ?
C20 C21 C22 C23 178.90(16) . . . . ?
C20 C21 C22 C26 -1.3(3) . . . . ?
C21 C6CA C25 C24 2.6(4) . . . . ?
C21 C6CA O5 C33 -170.4(6) . . . . ?
C21 C6CA O5B C33B -177.9(6) . . . . ?
C21 C20 N2 C19 148.65(18) . . . . ?
C21 C22 C23 C24 3.4(3) . . . . ?
C21 C22 C23 C29 -178.48(16) . . . . ?
C21 C22 C26 C27 -177.74(17) . . . . ?
C22 C23 C24 C25 -3.8(3) . . . . ?
C22 C23 C29 C28 -4.9(2) . . . . ?
C22 C23 C29 C30 174.69(16) . . . . ?
C22 C26 C27 C28 -2.6(3) . . . . ?
C23 C22 C26 C27 2.1(3) . . . . ?
C23 C24 C25 C6CA 0.9(3) . . . . ?
C23 C29 C30 C29 -96.3(2) . . . 8_565 ?
C23 C29 C30 C31 146.92(18) . . . . ?
C24 C23 C29 C28 173.12(17) . . . . ?
C24 C23 C29 C30 -7.3(3) . . . . ?
C25 C6CA C21 C20 178.0(2) . . . . ?
C25 C6CA C21 C22 -3.0(3) . . . . ?
C25 C6CA O5 C33 21.4(7) . . . . ?
C25 C6CA O5B C33B -12.8(8) . . . . ?
C26 C22 C23 C24 -176.42(16) . . . . ?
C26 C22 C23 C29 1.7(2) . . . . ?
C26 C27 C28 C29 -0.9(3) . . . . ?
C26 C27 C28 O4 179.37(17) . . . . ?
C27 C28 C29 C23 4.5(3) . . . . ?
C27 C28 C29 C30 -175.07(17) . . . . ?
C27 C28 O4 C32 176.81(17) . . . . ?
C28 C29 C30 C29 83.3(2) . . . 8_565 ?
C28 C29 C30 C31 -33.5(2) . . . . ?
C29 C23 C24 C25 178.08(18) . . . . ?
C29 C28 O4 C32 -2.9(3) . . . . ?
C29 C30 C31 C32 -59.66(13) 8_565 . . . ?
C29 C30 C31 C32 59.66(13) . . . . ?
C30 C31 C32 O4 -61.04(16) . . . . ?
C30 C31 C32 O4 61.04(16) . . . 8_565 ?
C31 C32 O4 C28 31.9(2) . . . . ?
C33 C34 C35 C36 -53.9(8) . . . . ?
C33B C34B C35B C36B 179.6(8) . . . . ?
C34 C33 O5 C6CA 167.5(5) . . . . ?
C34B C33B O5B C6CA 178.3(6) . . . . ?
N1 C19 N2 C20 -176.45(17) . . . . ?
N2 C19 N1 C18 173.36(18) . . . . ?
N2 C20 C21 C6CA 101.6(2) . . . . ?
N2 C20 C21 C22 -77.4(2) . . . . ?
O1 C9 C10 C3 176.56(17) . . . . ?
O1 C9 C10 C11 -3.5(3) . . . . ?
O1 C13 O1 C9 92.9(2) 8_565 . . . ?
O2 C14 C15 C16 170.06(18) . . . . ?
O3 C19 N1 C18 7.5(4) . . . . ?
O3 C19 N2 C20 -10.6(4) . . . . ?
O3B C19 N1 C18 -21.7(4) . . . . ?
O3B C19 N2 C20 18.6(4) . . . . ?
O4 C28 C29 C23 -175.73(16) . . . . ?
O4 C28 C29 C30 4.7(3) . . . . ?
O4 C32 O4 C28 -92.5(2) 8_565 . . . ?
O5 C6CA C21 C20 9.6(3) . . . . ?
O5 C6CA C21 C22 -171.4(2) . . . . ?
O5 C6CA C25 C24 170.2(3) . . . . ?
O5 C33 C34 C35 -57.0(8) . . . . ?
O5B C6CA C21 C20 -16.7(4) . . . . ?
O5B C6CA C21 C22 162.3(3) . . . . ?
O5B C6CA C25 C24 -161.8(3) . . . . ?
O5B C33B C34B C35B 54.7(10) . . . . ?
Cl1 C47 Cl2 Cl2B -74.7(9) . . . . ?
Cl1 C47 Cl2B Cl2 114.3(9) . . . . ?

_shelx_SHELXL_version_number     2014/7
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
1 8 -9 0.1093 1.0025 7.9964 -9.0067 0.6077 0.8364 0.1120
-1 -7 9 0.1108 -1.0024 -6.9964 9.0065 -0.5640 -0.7952 -0.0412
-4 8 8 0.1266 -3.9996 8.0021 8.0023 -0.0474 -0.0202 1.0155
3 -8 -7 0.1130 2.9998 -8.0019 -7.0019 -0.0292 -0.0074 -0.9521
4 -6 -10 0.1221 4.0003 -6.0029 -10.0039 0.1802 0.2224 -0.9717
-15 0 2 0.0559 -14.9930 -0.0021 1.9977 -0.8553 0.3643 0.3160
15 0 -2 0.0449 14.9930 0.0021 -1.9977 0.8553 -0.3643 -0.3160
13 5 4 0.1053 12.9927 5.0039 4.0044 0.8300 -0.4530 0.3602
-12 -6 -4 0.1175 -11.9933 -6.0037 -4.0040 -0.8197 0.3795 -0.4456
13 -3 5 0.0804 12.9919 -2.9954 5.0066 0.4575 -0.8426 -0.1572

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_4@1-anti
_database_code_depnum_ccdc_archive 'CCDC 1417790'
_audit_update_record             
;
2015-08-09 deposited with the CCDC.
2015-08-26 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT026_4@1-anti            
;
PROBLEM: Ratio Observed / Unique Reflections too Low ....         27 %     
RESPONSE: Since the crystal could easily lose crystallinity, the reflections are very weak, particularly at high resolution.
;
_vrf_PLAT340_4@1-anti            
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0168 Ang.  
RESPONSE: The structure involve disorder and the reflections are too weak.
;
_vrf_PLAT910_4@1-anti            
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...         11 Report
RESPONSE: The missing reflections at low resolution might be shielded by the beamstop.
;
# end Validation Reply Form


_audit_creation_date             2015-07-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C68 H72 N4 O10, C4 H8 O2, 2(C H Cl3)'
_chemical_formula_sum            'C74 H82 Cl6 N4 O12'
_chemical_formula_weight         1432.13
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C50 H50 O6 N4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.992(4)
_cell_length_b                   12.642(5)
_cell_length_c                   13.390(4)
_cell_angle_alpha                78.03(3)
_cell_angle_beta                 69.89(3)
_cell_angle_gamma                65.52(3)
_cell_volume                     1729.7(11)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    569
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      20.2030
_cell_measurement_theta_min      3.6360
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.314
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.993
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.1123
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.0616
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1157
_diffrn_reflns_av_unetI/netI     0.3715
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9961
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.248
_diffrn_reflns_theta_max         25.248
_diffrn_reflns_theta_min         3.222
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0053
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -42.00   56.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7586   37.0000    0.0000 98

#__ type_ start__ end____ width___ exp.time_
  2 omega  -83.00    9.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7586  -37.0000 -180.0000 92

#__ type_ start__ end____ width___ exp.time_
  3 omega  -19.00   25.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7586  -99.0000  120.0000 44

#__ type_ start__ end____ width___ exp.time_
  4 omega  -11.00   86.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       17.9305   77.0000   90.0000 97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0059419000
_diffrn_orient_matrix_UB_12      -0.0520846000
_diffrn_orient_matrix_UB_13      -0.0170566000
_diffrn_orient_matrix_UB_21      0.0673291000
_diffrn_orient_matrix_UB_22      -0.0211828000
_diffrn_orient_matrix_UB_23      -0.0098873000
_diffrn_orient_matrix_UB_31      -0.0065177000
_diffrn_orient_matrix_UB_32      -0.0257177000
_diffrn_orient_matrix_UB_33      0.0530273000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1655
_reflns_number_total             6199
_reflns_odcompleteness_completeness 96.38
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    ?
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         6199
_refine_ls_number_restraints     330
_refine_ls_R_factor_all          0.3169
_refine_ls_R_factor_gt           0.1110
_refine_ls_restrained_S_all      0.963
_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)+(0.0999P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2243
_refine_ls_wR_factor_ref         0.3446
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
3. Others
 Sof(H11C)=Sof(H11D)=Sof(C12B)=Sof(H12C)=Sof(H12D)=Sof(C13B)=Sof(H13C)=
 Sof(H13D)=Sof(C14B)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(1)
 Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C13)=Sof(H13A)=Sof(H13B)=
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(1)
 Fixed Sof: C28(0.5) H28A(0.5) H28B(0.5) C28B(0.5) H28C(0.5) H28D(0.5)
 C29(0.5) H29A(0.5) H29B(0.5) C29B(0.5) H29C(0.5) H29D(0.5) C30(0.5) H30A(0.5)
 H30B(0.5) C30B(0.5) H30C(0.5) H30D(0.5) H31D(0.5) H31E(0.5) H31F(0.5)
 H31A(0.5) H31B(0.5) H31C(0.5) O4(0.5) O4B(0.5)
4.a Ternary CH refined with riding coordinates:
 C15(H15), C17(H17), C37(H37)
4.b Secondary CH2 refined with riding coordinates:
 C11(H11C,H11D), C11(H11A,H11B), C12(H12A,H12B), C12B(H12C,H12D), C13(H13A,
 H13B), C13B(H13C,H13D), C16(H16A,H16B), C28(H28A,H28B), C28B(H28C,H28D),
 C29(H29A,H29B), C29B(H29C,H29D), C30(H30A,H30B), C30B(H30C,H30D), C32(H32A,
 H32B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B)
4.c Me refined with riding coordinates:
 C31(H31D,H31E,H31F), C31(H31A,H31B,H31C)
4.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C20(H20), C21(H21), C26(H26), C27(H27),
 N1(H1), N2(H2)
4.e Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C14B(H14D,H14E,H14F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
C1 C 1.1547(10) 0.4830(9) 0.1070(7) 0.033(3) Uani 1 1 d . . . . .
C2 C 1.0224(10) 0.5189(10) 0.1267(7) 0.041(3) Uani 1 1 d . . . . .
C3 C 0.9433(10) 0.6398(9) 0.1353(7) 0.032(3) Uani 1 1 d . . . . .
C4 C 1.0036(11) 0.7187(10) 0.1216(8) 0.044(3) Uani 1 1 d . . . . .
H4 H 0.9524 0.7993 0.1273 0.053 Uiso 1 1 calc R . . . .
C5 C 1.1330(11) 0.6834(9) 0.1005(8) 0.043(3) Uani 1 1 d . . . . .
H5 H 1.1723 0.7385 0.0875 0.052 Uiso 1 1 calc R . . . .
C6 C 1.2082(10) 0.5607(11) 0.0984(8) 0.044(3) Uani 1 1 d . . . . .
C7 C 0.9617(10) 0.4395(10) 0.1373(7) 0.040(3) Uani 1 1 d . . . . .
H7 H 1.0121 0.3585 0.1343 0.048 Uiso 1 1 calc R . . . .
C8 C 0.8356(11) 0.4759(10) 0.1513(8) 0.046(3) Uani 1 1 d . . . . .
H8 H 0.7986 0.4220 0.1528 0.055 Uiso 1 1 calc R . . . .
C9 C 0.7578(10) 0.5953(10) 0.1640(7) 0.037(3) Uani 1 1 d . . . . .
C10 C 0.8074(10) 0.6774(9) 0.1566(7) 0.030(3) Uani 1 1 d . . . . .
C11 C 1.3896(10) 0.5689(10) 0.1317(8) 0.047(3) Uani 1 1 d . . . . .
H11C H 1.3228 0.6384 0.1683 0.056 Uiso 0.468(19) 1 calc R . P A 2
H11D H 1.4645 0.5881 0.0861 0.056 Uiso 0.468(19) 1 calc R . P A 2
H11A H 1.3540 0.6551 0.1222 0.056 Uiso 0.532(19) 1 calc R . P A 1
H11B H 1.4836 0.5431 0.1000 0.056 Uiso 0.532(19) 1 calc R . P A 1
C12 C 1.361(2) 0.532(2) 0.2574(15) 0.045(7) Uani 0.532(19) 1 d . . P A 1
H12A H 1.3993 0.5671 0.2897 0.054 Uiso 0.532(19) 1 calc R . P A 1
H12B H 1.2677 0.5603 0.2921 0.054 Uiso 0.532(19) 1 calc R . P A 1
C12B C 1.428(3) 0.464(3) 0.211(3) 0.070(10) Uani 0.468(19) 1 d . . P A 2
H12C H 1.3546 0.4383 0.2467 0.084 Uiso 0.468(19) 1 calc R . P A 2
H12D H 1.4480 0.4871 0.2672 0.084 Uiso 0.468(19) 1 calc R . P A 2
C13 C 1.420(2) 0.396(2) 0.2750(19) 0.059(8) Uani 0.532(19) 1 d . . P A 1
H13A H 1.3910 0.3740 0.3521 0.071 Uiso 0.532(19) 1 calc R . P A 1
H13B H 1.3859 0.3628 0.2372 0.071 Uiso 0.532(19) 1 calc R . P A 1
C13B C 1.547(3) 0.360(3) 0.154(2) 0.069(10) Uani 0.468(19) 1 d . . P A 2
H13C H 1.5242 0.3356 0.1001 0.083 Uiso 0.468(19) 1 calc R . P A 2
H13D H 1.6173 0.3883 0.1147 0.083 Uiso 0.468(19) 1 calc R . P A 2
C14 C 1.563(2) 0.343(2) 0.238(2) 0.052(8) Uani 0.532(19) 1 d . . P A 1
H14A H 1.5916 0.2595 0.2597 0.078 Uiso 0.532(19) 1 calc GR . P A 1
H14B H 1.5986 0.3803 0.2702 0.078 Uiso 0.532(19) 1 calc GR . P A 1
H14C H 1.5929 0.3548 0.1602 0.078 Uiso 0.532(19) 1 calc GR . P A 1
C14B C 1.593(3) 0.262(3) 0.221(2) 0.083(13) Uani 0.468(19) 1 d . . P A 2
H14D H 1.6025 0.2867 0.2809 0.125 Uiso 0.468(19) 1 calc GR . P A 2
H14E H 1.6761 0.2089 0.1807 0.125 Uiso 0.468(19) 1 calc GR . P A 2
H14F H 1.5321 0.2225 0.2470 0.125 Uiso 0.468(19) 1 calc GR . P A 2
C15 C 0.7148(10) 0.8039(9) 0.1731(8) 0.043(3) Uani 1 1 d . . . . .
H15 H 0.7552 0.8588 0.1263 0.052 Uiso 1 1 calc R . . . .
C16 C 0.5924(10) 0.8209(10) 0.1467(8) 0.045(3) Uani 1 1 d . . . . .
H16A H 0.5266 0.8992 0.1645 0.054 Uiso 1 1 calc R . . . .
H16B H 0.6120 0.8140 0.0696 0.054 Uiso 1 1 calc R . . . .
C17 C 0.5457(10) 0.7310(9) 0.2096(7) 0.037(3) Uani 1 1 d . . . . .
H17 H 0.4620 0.7469 0.1980 0.044 Uiso 1 1 calc R . . . .
C18 C 0.7216(10) 0.9588(9) 0.4923(8) 0.038(3) Uani 1 1 d . . . . .
C19 C 0.7995(12) 1.0138(11) 0.4284(9) 0.050(3) Uani 1 1 d . . . . .
C20 C 0.8310(11) 1.0145(10) 0.3136(8) 0.052(3) Uani 1 1 d . . . . .
H20 H 0.8799 1.0584 0.2686 0.063 Uiso 1 1 calc R . . . .
C21 C 0.7927(11) 0.9549(10) 0.2702(9) 0.049(3) Uani 1 1 d . . . . .
H21 H 0.8178 0.9551 0.1947 0.059 Uiso 1 1 calc R . . . .
C22 C 0.7160(10) 0.8915(9) 0.3323(8) 0.036(3) Uani 1 1 d . . . . .
C23 C 0.6758(9) 0.8970(9) 0.4477(8) 0.032(3) Uani 1 1 d . . . . .
C24 C 0.6719(10) 0.8294(9) 0.2920(8) 0.035(3) Uani 1 1 d . . . . .
C25 C 0.5841(10) 0.7841(9) 0.3565(8) 0.032(3) Uani 1 1 d . . . . .
C26 C 0.5416(10) 0.7908(9) 0.4686(8) 0.043(3) Uani 1 1 d . . . . .
H26 H 0.4809 0.7581 0.5129 0.052 Uiso 1 1 calc R . . . .
C27 C 0.5891(9) 0.8442(9) 0.5104(8) 0.033(3) Uani 1 1 d . . . . .
H27 H 0.5632 0.8465 0.5857 0.039 Uiso 1 1 calc R . . . .
C28 C 0.944(2) 1.120(2) 0.4300(19) 0.043(7) Uani 0.5 1 d . . P B 1
H28A H 1.0128 1.0807 0.3678 0.051 Uiso 0.5 1 calc R . P B 1
H28B H 0.9857 1.1270 0.4795 0.051 Uiso 0.5 1 calc R . P B 1
C28B C 0.888(3) 1.166(2) 0.3988(18) 0.037(7) Uani 0.5 1 d . . P C 2
H28C H 0.8391 1.2207 0.3504 0.045 Uiso 0.5 1 calc R . P C 2
H28D H 0.9742 1.1197 0.3550 0.045 Uiso 0.5 1 calc R . P C 2
C29 C 0.866(2) 1.241(2) 0.3927(19) 0.052(7) Uani 0.5 1 d . . P B 1
H29A H 0.8169 1.2348 0.3490 0.062 Uiso 0.5 1 calc R . P B 1
H29B H 0.9230 1.2814 0.3479 0.062 Uiso 0.5 1 calc R . P B 1
C29B C 0.899(2) 1.2321(19) 0.4726(17) 0.041(6) Uani 0.5 1 d . . P C 2
H29C H 0.9459 1.2829 0.4302 0.050 Uiso 0.5 1 calc R . P C 2
H29D H 0.9500 1.1761 0.5189 0.050 Uiso 0.5 1 calc R . P C 2
C30 C 0.774(3) 1.309(2) 0.489(2) 0.049(8) Uani 0.5 1 d . . P B 1
H30A H 0.7295 1.2598 0.5390 0.059 Uiso 0.5 1 calc R . P B 1
H30B H 0.8248 1.3236 0.5251 0.059 Uiso 0.5 1 calc R . P B 1
C30B C 0.766(2) 1.310(2) 0.5453(19) 0.048(7) Uani 0.5 1 d . . P C 2
H30C H 0.7793 1.3464 0.5963 0.057 Uiso 0.5 1 calc R . P C 2
H30D H 0.7163 1.2606 0.5866 0.057 Uiso 0.5 1 calc R . P C 2
C31 C 0.6816(12) 1.4158(11) 0.4663(10) 0.083(5) Uani 1 1 d . . . . .
H31D H 0.5988 1.4641 0.5113 0.124 Uiso 0.5 1 calc R . P B 2
H31E H 0.7305 1.4647 0.4262 0.124 Uiso 0.5 1 calc R . P B 2
H31F H 0.6676 1.3790 0.4165 0.124 Uiso 0.5 1 calc R . P B 2
H31A H 0.6274 1.4530 0.5329 0.124 Uiso 0.5 1 calc R . P B 1
H31B H 0.7241 1.4666 0.4183 0.124 Uiso 0.5 1 calc R . P B 1
H31C H 0.6285 1.4026 0.4322 0.124 Uiso 0.5 1 calc R . P B 1
C32 C 0.6848(10) 0.9606(9) 0.6115(7) 0.040(3) Uani 1 1 d . . . . .
H32A H 0.7057 1.0209 0.6295 0.048 Uiso 1 1 calc R . . . .
H32B H 0.5917 0.9791 0.6425 0.048 Uiso 1 1 calc R . . . .
C33 C 0.7217(10) 0.8130(10) 0.7610(9) 0.042(3) Uani 1 1 d . . . . .
C34 C 0.7613(10) 0.6478(9) 0.8943(7) 0.041(3) Uani 1 1 d . . . . .
H34A H 0.6696 0.6588 0.9220 0.049 Uiso 1 1 calc R . . . .
H34B H 0.7805 0.6853 0.9410 0.049 Uiso 1 1 calc R . . . .
N1 N 0.7561(8) 0.8457(7) 0.6545(6) 0.050(3) Uani 1 1 d . . . . .
H1 H 0.8222 0.7967 0.6111 0.060 Uiso 1 1 calc R . . . .
N2 N 0.7897(8) 0.6997(7) 0.7848(6) 0.041(3) Uani 1 1 d . . . . .
H2 H 0.8512 0.6571 0.7340 0.050 Uiso 1 1 calc R . . . .
O1 O 1.3408(7) 0.5252(7) 0.0705(6) 0.062(2) Uani 1 1 d . . . . .
O2 O 0.6292(7) 0.6178(6) 0.1780(5) 0.054(2) Uani 1 1 d . . . . .
O3 O 0.5244(7) 0.7283(6) 0.3221(5) 0.051(2) Uani 1 1 d . . . . .
O4 O 0.8675(18) 1.0478(16) 0.4842(13) 0.048(6) Uani 0.5 1 d . . P B 1
O4B O 0.8236(17) 1.0914(17) 0.4620(14) 0.049(6) Uani 0.5 1 d . . P C 2
O5 O 0.6391(7) 0.8804(6) 0.8279(5) 0.052(2) Uani 1 1 d . . . . .
C35 C 0.9688(12) 0.5288(11) 0.4086(9) 0.073(4) Uani 1 1 d . . . . .
H35A H 1.0152 0.5815 0.3717 0.088 Uiso 1 1 calc R . . . .
H35B H 0.9240 0.5242 0.3608 0.088 Uiso 1 1 calc R . . . .
C36 C 1.1211(13) 0.4232(12) 0.4999(10) 0.083(5) Uani 1 1 d . . . . .
H36A H 1.1802 0.3451 0.5188 0.099 Uiso 1 1 calc R . . . .
H36B H 1.1720 0.4726 0.4648 0.099 Uiso 1 1 calc R . . . .
O6 O 1.0624(7) 0.4126(7) 0.4258(6) 0.067(3) Uani 1 1 d . . . . .
C37 C 0.7585(10) 1.0176(10) 0.8858(8) 0.049(3) Uani 1 1 d . . . . .
H37 H 0.7100 0.9785 0.8695 0.059 Uiso 1 1 calc R . . . .
Cl1 Cl 0.6611(3) 1.0979(3) 0.9951(2) 0.0645(11) Uani 1 1 d . . . . .
Cl2 Cl 0.8035(3) 1.1078(3) 0.7720(2) 0.0603(11) Uani 1 1 d . . . . .
Cl3 Cl 0.8976(3) 0.9093(3) 0.9131(2) 0.0879(15) 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
C1 C2 1.400(13) . ?
C1 C6 1.346(14) . ?
C1 C34 1.539(12) 2_766 ?
C2 C3 1.430(13) . ?
C2 C7 1.426(14) . ?
C3 C4 1.407(14) . ?
C3 C10 1.435(13) . ?
C4 H4 0.9500 . ?
C4 C5 1.366(13) . ?
C5 H5 0.9500 . ?
C5 C6 1.436(14) . ?
C6 O1 1.392(12) . ?
C7 H7 0.9500 . ?
C7 C8 1.341(13) . ?
C8 H8 0.9500 . ?
C8 C9 1.417(13) . ?
C9 C10 1.367(14) . ?
C9 O2 1.399(12) . ?
C10 C15 1.532(13) . ?
C11 H11C 0.9900 . ?
C11 H11D 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.61(2) . ?
C11 C12B 1.53(3) . ?
C11 O1 1.451(11) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.56(3) . ?
C12B H12C 0.9900 . ?
C12B H12D 0.9900 . ?
C12B C13B 1.58(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.50(3) . ?
C13B H13C 0.9900 . ?
C13B H13D 0.9900 . ?
C13B C14B 1.39(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C14B H14D 0.9800 . ?
C14B H14E 0.9800 . ?
C14B H14F 0.9800 . ?
C15 H15 1.0000 . ?
C15 C16 1.546(12) . ?
C15 C24 1.554(13) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.457(14) . ?
C17 H17 1.0000 . ?
C17 O2 1.414(11) . ?
C17 O3 1.434(10) . ?
C18 C19 1.354(15) . ?
C18 C23 1.430(14) . ?
C18 C32 1.504(12) . ?
C19 C20 1.449(14) . ?
C19 O4 1.50(2) . ?
C19 O4B 1.32(2) . ?
C20 H20 0.9500 . ?
C20 C21 1.330(14) . ?
C21 H21 0.9500 . ?
C21 C22 1.411(15) . ?
C22 C23 1.459(13) . ?
C22 C24 1.380(14) . ?
C23 C27 1.405(13) . ?
C24 C25 1.361(14) . ?
C25 C26 1.418(13) . ?
C25 O3 1.414(12) . ?
C26 H26 0.9500 . ?
C26 C27 1.337(13) . ?
C27 H27 0.9500 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.51(3) . ?
C28 O4 1.47(3) . ?
C28B H28C 0.9900 . ?
C28B H28D 0.9900 . ?
C28B C29B 1.49(3) . ?
C28B O4B 1.43(3) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.52(3) . ?
C29B H29C 0.9900 . ?
C29B H29D 0.9900 . ?
C29B C30B 1.58(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.40(3) . ?
C30B H30C 0.9900 . ?
C30B H30D 0.9900 . ?
C30B C31 1.72(2) . ?
C31 H31D 0.9800 . ?
C31 H31E 0.9800 . ?
C31 H31F 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 N1 1.461(11) . ?
C33 N1 1.366(12) . ?
C33 N2 1.357(12) . ?
C33 O5 1.232(11) . ?
C34 C1 1.539(12) 2_766 ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 N2 1.463(11) . ?
N1 H1 0.8800 . ?
N2 H2 0.8800 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.375(15) 2_766 ?
C35 O6 1.463(12) . ?
C36 C35 1.375(15) 2_766 ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 O6 1.453(12) . ?
C37 H37 1.0000 . ?
C37 Cl1 1.730(11) . ?
C37 Cl2 1.772(11) . ?
C37 Cl3 1.763(10) . ?

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
C2 C1 C34 119.7(11) . 2_766 ?
C6 C1 C2 120.8(10) . . ?
C6 C1 C34 119.3(10) . 2_766 ?
C1 C2 C3 119.7(12) . . ?
C1 C2 C7 122.6(10) . . ?
C7 C2 C3 117.7(10) . . ?
C2 C3 C10 120.1(11) . . ?
C4 C3 C2 117.8(10) . . ?
C4 C3 C10 122.1(10) . . ?
C3 C4 H4 118.9 . . ?
C5 C4 C3 122.3(11) . . ?
C5 C4 H4 118.9 . . ?
C4 C5 H5 120.9 . . ?
C4 C5 C6 118.2(11) . . ?
C6 C5 H5 120.9 . . ?
C1 C6 C5 121.0(10) . . ?
C1 C6 O1 120.1(10) . . ?
O1 C6 C5 118.1(12) . . ?
C2 C7 H7 119.1 . . ?
C8 C7 C2 121.9(11) . . ?
C8 C7 H7 119.1 . . ?
C7 C8 H8 120.2 . . ?
C7 C8 C9 119.6(12) . . ?
C9 C8 H8 120.2 . . ?
C10 C9 C8 122.4(11) . . ?
C10 C9 O2 125.5(10) . . ?
O2 C9 C8 112.0(11) . . ?
C3 C10 C15 123.7(11) . . ?
C9 C10 C3 118.1(10) . . ?
C9 C10 C15 118.2(10) . . ?
H11C C11 H11D 109.4 . . ?
H11A C11 H11B 107.2 . . ?
C12 C11 H11A 107.9 . . ?
C12 C11 H11B 107.9 . . ?
C12B C11 H11C 111.5 . . ?
C12B C11 H11D 111.5 . . ?
O1 C11 H11C 111.5 . . ?
O1 C11 H11D 111.5 . . ?
O1 C11 H11A 107.9 . . ?
O1 C11 H11B 107.9 . . ?
O1 C11 C12 117.8(12) . . ?
O1 C11 C12B 101.2(14) . . ?
C11 C12 H12A 109.8 . . ?
C11 C12 H12B 109.8 . . ?
H12A C12 H12B 108.3 . . ?
C13 C12 C11 109.2(17) . . ?
C13 C12 H12A 109.8 . . ?
C13 C12 H12B 109.8 . . ?
C11 C12B H12C 109.5 . . ?
C11 C12B H12D 109.5 . . ?
C11 C12B C13B 111(2) . . ?
H12C C12B H12D 108.1 . . ?
C13B C12B H12C 109.5 . . ?
C13B C12B H12D 109.5 . . ?
C12 C13 H13A 108.5 . . ?
C12 C13 H13B 108.5 . . ?
H13A C13 H13B 107.5 . . ?
C14 C13 C12 115(2) . . ?
C14 C13 H13A 108.5 . . ?
C14 C13 H13B 108.5 . . ?
C12B C13B H13C 108.5 . . ?
C12B C13B H13D 108.5 . . ?
H13C C13B H13D 107.5 . . ?
C14B C13B C12B 115(3) . . ?
C14B C13B H13C 108.5 . . ?
C14B C13B H13D 108.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13B C14B H14D 109.5 . . ?
C13B C14B H14E 109.5 . . ?
C13B C14B H14F 109.5 . . ?
H14D C14B H14E 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
C10 C15 H15 110.5 . . ?
C10 C15 C16 108.2(9) . . ?
C10 C15 C24 110.8(7) . . ?
C16 C15 H15 110.5 . . ?
C16 C15 C24 106.3(8) . . ?
C24 C15 H15 110.5 . . ?
C15 C16 H16A 110.2 . . ?
C15 C16 H16B 110.2 . . ?
H16A C16 H16B 108.5 . . ?
C17 C16 C15 107.7(8) . . ?
C17 C16 H16A 110.2 . . ?
C17 C16 H16B 110.2 . . ?
C16 C17 H17 107.6 . . ?
O2 C17 C16 112.6(9) . . ?
O2 C17 H17 107.6 . . ?
O2 C17 O3 107.1(7) . . ?
O3 C17 C16 114.1(9) . . ?
O3 C17 H17 107.6 . . ?
C19 C18 C23 120.5(10) . . ?
C19 C18 C32 119.8(11) . . ?
C23 C18 C32 119.6(11) . . ?
C18 C19 C20 119.2(12) . . ?
C18 C19 O4 114.8(12) . . ?
C20 C19 O4 124.7(13) . . ?
O4B C19 C18 123.1(13) . . ?
O4B C19 C20 115.5(14) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 C19 121.3(12) . . ?
C21 C20 H20 119.4 . . ?
C20 C21 H21 118.9 . . ?
C20 C21 C22 122.2(11) . . ?
C22 C21 H21 118.9 . . ?
C21 C22 C23 117.0(11) . . ?
C24 C22 C21 125.0(10) . . ?
C24 C22 C23 117.9(11) . . ?
C18 C23 C22 119.4(11) . . ?
C27 C23 C18 122.5(10) . . ?
C27 C23 C22 118.0(10) . . ?
C22 C24 C15 125.1(11) . . ?
C25 C24 C15 113.8(10) . . ?
C25 C24 C22 121.1(10) . . ?
C24 C25 C26 121.5(11) . . ?
C24 C25 O3 125.6(10) . . ?
O3 C25 C26 112.9(10) . . ?
C25 C26 H26 120.8 . . ?
C27 C26 C25 118.4(11) . . ?
C27 C26 H26 120.8 . . ?
C23 C27 H27 118.6 . . ?
C26 C27 C23 122.7(10) . . ?
C26 C27 H27 118.6 . . ?
H28A C28 H28B 107.8 . . ?
C29 C28 H28A 109.0 . . ?
C29 C28 H28B 109.0 . . ?
O4 C28 H28A 109.0 . . ?
O4 C28 H28B 109.0 . . ?
O4 C28 C29 113(2) . . ?
H28C C28B H28D 108.5 . . ?
C29B C28B H28C 110.2 . . ?
C29B C28B H28D 110.2 . . ?
O4B C28B H28C 110.2 . . ?
O4B C28B H28D 110.2 . . ?
O4B C28B C29B 108(2) . . ?
C28 C29 H29A 109.8 . . ?
C28 C29 H29B 109.8 . . ?
C28 C29 C30 109.6(19) . . ?
H29A C29 H29B 108.2 . . ?
C30 C29 H29A 109.8 . . ?
C30 C29 H29B 109.8 . . ?
C28B C29B H29C 108.8 . . ?
C28B C29B H29D 108.8 . . ?
C28B C29B C30B 114(2) . . ?
H29C C29B H29D 107.7 . . ?
C30B C29B H29C 108.8 . . ?
C30B C29B H29D 108.8 . . ?
C29 C30 H30A 108.4 . . ?
C29 C30 H30B 108.4 . . ?
H30A C30 H30B 107.4 . . ?
C31 C30 C29 115.7(19) . . ?
C31 C30 H30A 108.4 . . ?
C31 C30 H30B 108.4 . . ?
C29B C30B H30C 109.8 . . ?
C29B C30B H30D 109.8 . . ?
C29B C30B C31 109.3(16) . . ?
H30C C30B H30D 108.3 . . ?
C31 C30B H30C 109.8 . . ?
C31 C30B H30D 109.8 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
C30B C31 H31D 109.5 . . ?
C30B C31 H31E 109.5 . . ?
C30B C31 H31F 109.5 . . ?
H31D C31 H31E 109.5 . . ?
H31D C31 H31F 109.5 . . ?
H31E C31 H31F 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C18 C32 H32A 110.1 . . ?
C18 C32 H32B 110.1 . . ?
H32A C32 H32B 108.4 . . ?
N1 C32 C18 108.2(7) . . ?
N1 C32 H32A 110.1 . . ?
N1 C32 H32B 110.1 . . ?
N2 C33 N1 112.8(9) . . ?
O5 C33 N1 123.2(10) . . ?
O5 C33 N2 124.0(10) . . ?
C1 C34 H34A 110.2 2_766 . ?
C1 C34 H34B 110.2 2_766 . ?
H34A C34 H34B 108.5 . . ?
N2 C34 C1 107.7(8) . 2_766 ?
N2 C34 H34A 110.2 . . ?
N2 C34 H34B 110.2 . . ?
C32 N1 H1 119.5 . . ?
C33 N1 C32 121.0(8) . . ?
C33 N1 H1 119.5 . . ?
C33 N2 C34 120.4(8) . . ?
C33 N2 H2 119.8 . . ?
C34 N2 H2 119.8 . . ?
C6 O1 C11 116.0(8) . . ?
C9 O2 C17 113.5(9) . . ?
C25 O3 C17 117.9(9) . . ?
C28 O4 C19 122.3(15) . . ?
C19 O4B C28B 127.5(18) . . ?
H35A C35 H35B 107.6 . . ?
C36 C35 H35A 108.6 2_766 . ?
C36 C35 H35B 108.6 2_766 . ?
C36 C35 O6 114.6(9) 2_766 . ?
O6 C35 H35A 108.6 . . ?
O6 C35 H35B 108.6 . . ?
C35 C36 H36A 109.3 2_766 . ?
C35 C36 H36B 109.3 2_766 . ?
C35 C36 O6 111.8(12) 2_766 . ?
H36A C36 H36B 107.9 . . ?
O6 C36 H36A 109.3 . . ?
O6 C36 H36B 109.3 . . ?
C36 O6 C35 106.3(9) . . ?
Cl1 C37 H37 108.5 . . ?
Cl1 C37 Cl2 111.4(6) . . ?
Cl1 C37 Cl3 110.9(5) . . ?
Cl2 C37 H37 108.5 . . ?
Cl3 C37 H37 108.5 . . ?
Cl3 C37 Cl2 109.1(6) . . ?

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
C1 C2 C3 C4 1.0(13) . . . . ?
C1 C2 C3 C10 -179.3(8) . . . . ?
C1 C2 C7 C8 -176.9(9) . . . . ?
C1 C6 O1 C11 -135.9(10) . . . . ?
C1 C34 N2 C33 174.8(10) 2_766 . . . ?
C2 C1 C6 C5 -5.1(15) . . . . ?
C2 C1 C6 O1 -174.9(8) . . . . ?
C2 C3 C4 C5 0.2(14) . . . . ?
C2 C3 C10 C9 -2.5(13) . . . . ?
C2 C3 C10 C15 176.6(8) . . . . ?
C2 C7 C8 C9 -4.8(14) . . . . ?
C3 C2 C7 C8 2.2(13) . . . . ?
C3 C4 C5 C6 -3.6(15) . . . . ?
C3 C10 C15 C16 156.4(8) . . . . ?
C3 C10 C15 C24 -87.4(12) . . . . ?
C4 C3 C10 C9 177.1(9) . . . . ?
C4 C3 C10 C15 -3.8(14) . . . . ?
C4 C5 C6 C1 6.2(15) . . . . ?
C4 C5 C6 O1 176.1(9) . . . . ?
C5 C6 O1 C11 54.1(13) . . . . ?
C6 C1 C2 C3 1.5(14) . . . . ?
C6 C1 C2 C7 -179.4(9) . . . . ?
C7 C2 C3 C4 -178.1(8) . . . . ?
C7 C2 C3 C10 1.6(13) . . . . ?
C7 C8 C9 C10 3.7(14) . . . . ?
C7 C8 C9 O2 -179.9(8) . . . . ?
C8 C9 C10 C3 -0.1(14) . . . . ?
C8 C9 C10 C15 -179.2(8) . . . . ?
C8 C9 O2 C17 169.4(8) . . . . ?
C9 C10 C15 C16 -24.5(11) . . . . ?
C9 C10 C15 C24 91.7(11) . . . . ?
C10 C3 C4 C5 -179.5(9) . . . . ?
C10 C9 O2 C17 -14.4(13) . . . . ?
C10 C15 C16 C17 53.3(10) . . . . ?
C10 C15 C24 C22 104.1(11) . . . . ?
C10 C15 C24 C25 -75.8(11) . . . . ?
C11 C12 C13 C14 67(2) . . . . ?
C11 C12B C13B C14B 177(3) . . . . ?
C12 C11 O1 C6 62.6(15) . . . . ?
C12B C11 O1 C6 99.4(18) . . . . ?
C15 C16 C17 O2 -67.2(10) . . . . ?
C15 C16 C17 O3 55.1(11) . . . . ?
C15 C24 C25 C26 174.9(8) . . . . ?
C15 C24 C25 O3 -6.1(13) . . . . ?
C16 C15 C24 C22 -138.5(10) . . . . ?
C16 C15 C24 C25 41.6(10) . . . . ?
C16 C17 O2 C9 46.3(10) . . . . ?
C16 C17 O3 C25 -18.6(12) . . . . ?
C18 C19 C20 C21 -5.1(17) . . . . ?
C18 C19 O4 C28 -172.8(15) . . . . ?
C18 C19 O4B C28B -170.0(19) . . . . ?
C18 C23 C27 C26 176.9(9) . . . . ?
C18 C32 N1 C33 -165.0(10) . . . . ?
C19 C18 C23 C22 1.3(14) . . . . ?
C19 C18 C23 C27 -176.3(9) . . . . ?
C19 C18 C32 N1 -105.7(11) . . . . ?
C19 C20 C21 C22 2.3(17) . . . . ?
C20 C19 O4 C28 20(2) . . . . ?
C20 C19 O4B C28B -7(3) . . . . ?
C20 C21 C22 C23 2.1(15) . . . . ?
C20 C21 C22 C24 179.1(10) . . . . ?
C21 C22 C23 C18 -3.9(13) . . . . ?
C21 C22 C23 C27 173.8(8) . . . . ?
C21 C22 C24 C15 9.3(15) . . . . ?
C21 C22 C24 C25 -170.8(9) . . . . ?
C22 C23 C27 C26 -0.8(14) . . . . ?
C22 C24 C25 C26 -5.0(14) . . . . ?
C22 C24 C25 O3 174.0(8) . . . . ?
C23 C18 C19 C20 3.1(15) . . . . ?
C23 C18 C19 O4 -164.7(11) . . . . ?
C23 C18 C19 O4B 165.6(12) . . . . ?
C23 C18 C32 N1 73.2(11) . . . . ?
C23 C22 C24 C15 -173.7(8) . . . . ?
C23 C22 C24 C25 6.2(13) . . . . ?
C24 C15 C16 C17 -65.8(10) . . . . ?
C24 C22 C23 C18 178.8(8) . . . . ?
C24 C22 C23 C27 -3.4(12) . . . . ?
C24 C25 C26 C27 0.6(14) . . . . ?
C24 C25 O3 C17 -7.7(13) . . . . ?
C25 C26 C27 C23 2.2(14) . . . . ?
C26 C25 O3 C17 171.3(7) . . . . ?
C28 C29 C30 C31 -171(2) . . . . ?
C28B C29B C30B C31 -64(3) . . . . ?
C29 C28 O4 C19 63(3) . . . . ?
C29B C28B O4B C19 -176.5(17) . . . . ?
C32 C18 C19 C20 -178.1(9) . . . . ?
C32 C18 C19 O4 14.1(16) . . . . ?
C32 C18 C19 O4B -15.6(18) . . . . ?
C32 C18 C23 C22 -177.5(8) . . . . ?
C32 C18 C23 C27 4.8(14) . . . . ?
C34 C1 C2 C3 175.7(8) 2_766 . . . ?
C34 C1 C2 C7 -5.2(13) 2_766 . . . ?
C34 C1 C6 C5 -179.3(8) 2_766 . . . ?
C34 C1 C6 O1 10.9(14) 2_766 . . . ?
N1 C33 N2 C34 -176.8(9) . . . . ?
N2 C33 N1 C32 173.3(9) . . . . ?
O1 C11 C12 C13 59.6(19) . . . . ?
O1 C11 C12B C13B 70(2) . . . . ?
O2 C9 C10 C3 -175.9(8) . . . . ?
O2 C9 C10 C15 5.0(14) . . . . ?
O2 C17 O3 C25 106.8(10) . . . . ?
O3 C17 O2 C9 -80.0(10) . . . . ?
O3 C25 C26 C27 -178.5(8) . . . . ?
O4 C19 C20 C21 161.4(13) . . . . ?
O4 C28 C29 C30 68(3) . . . . ?
O4B C19 C20 C21 -168.9(13) . . . . ?
O4B C28B C29B C30B -60(3) . . . . ?
O5 C33 N1 C32 -7.6(17) . . . . ?
O5 C33 N2 C34 4.2(17) . . . . ?
C35 C36 O6 C35 54.2(16) 2_766 . . . ?
C36 C35 O6 C36 -55.9(18) 2_766 . . . ?

_shelx_SHELXL_version_number     2014/7
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
16 10 3 0.0469 16.0000 10.0000 3.0000 -0.4769 0.8358 -0.2024
-16 -10 -3 0.0251 -16.0000 -10.0000 -3.0000 0.4769 -0.8358 0.2024
-3 -7 15 0.0251 -3.0000 -7.0000 15.0000 0.0909 -0.2020 0.9950
1 6 -15 0.0661 1.0000 6.0000 -15.0000 -0.0507 0.0885 -0.9562
-2 15 0 0.0406 -2.0000 15.0000 -0.0000 -0.7932 -0.4524 -0.3727
2 -15 0 0.0210 2.0000 -15.0000 0.0000 0.7932 0.4524 0.3727
12 -5 1 0.0214 12.0000 -5.0000 1.0000 0.3147 0.9040 0.1034
0 -5 16 0.0246 -0.0000 -5.0000 16.0000 -0.0125 -0.0523 0.9770
-11 -14 -13 0.0374 -11.0000 -14.0000 -13.0000 0.8856 -0.3155 -0.2576
7 5 19 0.0377 7.0000 5.0000 19.0000 -0.5429 0.1775 0.8333

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_4@1-syn
_database_code_depnum_ccdc_archive 'CCDC 1417791'
_audit_update_record             
;
2015-08-09 deposited with the CCDC.
2015-08-26 downloaded from the CCDC.
;
_audit_creation_date             2015-08-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '1.4(C H2 Cl2), 2.6(C4 H8 O2), C68 H72 N4 O10'
_chemical_formula_sum            'C79.80 H95.60 Cl2.80 N4 O15.20'
_chemical_formula_weight         1453.26
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C40 H40 O8 N4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/n 1'
_space_group_name_Hall           '-P 2yac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'

_cell_length_a                   12.4884(7)
_cell_length_b                   17.1551(9)
_cell_length_c                   17.3844(8)
_cell_angle_alpha                90
_cell_angle_beta                 96.545(4)
_cell_angle_gamma                90
_cell_volume                     3700.2(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6236
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.6420
_cell_measurement_theta_min      3.5660
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.186
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.974
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1543
_exptl_crystal_size_max          0.5527
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.031
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0887
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            42494
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_min         2.887
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0053
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -37.00   48.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7586   57.0000 -150.0000 85

#__ type_ start__ end____ width___ exp.time_
  2 omega  -47.00   53.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7586   77.0000  -60.0000 100

#__ type_ start__ end____ width___ exp.time_
  3 omega   -3.00   87.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       17.9305   57.0000 -150.0000 90

#__ type_ start__ end____ width___ exp.time_
  4 omega    7.00   80.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       17.9305 -133.0000   49.2284 73

#__ type_ start__ end____ width___ exp.time_
  5 omega  -50.00   39.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       17.9305  -57.0000   90.0000 89

#__ type_ start__ end____ width___ exp.time_
  6 omega    2.00   87.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       17.9305   57.0000   90.0000 85

#__ type_ start__ end____ width___ exp.time_
  7 omega   26.00   76.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       17.9305   37.0000  -90.0000 50

#__ type_ start__ end____ width___ exp.time_
  8 omega  -12.00   75.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       17.9305   77.0000  -30.0000 87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0404208000
_diffrn_orient_matrix_UB_12      0.0034064000
_diffrn_orient_matrix_UB_13      0.0253512000
_diffrn_orient_matrix_UB_21      -0.0073489000
_diffrn_orient_matrix_UB_22      -0.0410226000
_diffrn_orient_matrix_UB_23      -0.0011091000
_diffrn_orient_matrix_UB_31      0.0397342000
_diffrn_orient_matrix_UB_32      -0.0040148000
_diffrn_orient_matrix_UB_33      0.0322849000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4270
_reflns_number_total             6696
_reflns_odcompleteness_completeness 99.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    ?
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         6696
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_gt           0.0763
_refine_ls_restrained_S_all      1.084
_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)+(0.1042P)²+2.1619P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1857
_refine_ls_wR_factor_ref         0.2193
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C42-C38
 1.52 with sigma of 0.01
 H28A_$1-H32A
 2.2 with sigma of 0.01
 C44-Cl3 \\sim C44-Cl4
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C39) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C33B) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl3) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(Cl4) \\sim Ueq, Uanis(O10)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C44) = Uanis(C38)
4. Others
 Sof(Cl2)=1-FVAR(1)
 Sof(H40C)=Sof(H40D)=0.5*(1-FVAR(2))
 Sof(H40A)=Sof(H40B)=0.5*FVAR(2)
 Sof(Cl1)=FVAR(1)
 Fixed Sof: H31A(0.75) H31B(0.75) H31C(0.25) H31D(0.25) C32(0.75) H32A(0.75)
 H32B(0.75) C33(0.75) H33A(0.75) H33B(0.75) H33C(0.75) O11(0.8) O10(0.8)
 C36(0.8) H36A(0.8) H36B(0.8) C38(0.8) H38A(0.8) H38B(0.8) C32B(0.25)
 H32C(0.25) H32D(0.25) C33B(0.25) H33D(0.25) H33E(0.25) H33F(0.25) Cl4(0.2)
 C39(0.8) H39A(0.8) H39B(0.8) C42(0.8) H42A(0.8) H42B(0.8) Cl3(0.2) C44(0.2)
 H44A(0.2) H44B(0.2)
5.a Ternary CH refined with riding coordinates:
 C43(H43), C24(H24)
5.b Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C40(H40C,H40D), C34(H34A,H34B), C35(H35A,H35B), C11(H11A,
 H11B), C13(H13A,H13B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B),
 C28(H28A,H28B), C30(H30A,H30B), C31(H31A,H31B), C31(H31C,H31D), C32(H32A,H32B),
  C36(H36A,H36B), C38(H38A,H38B), C32B(H32C,H32D), C39(H39A,H39B), C42(H42A,
 H42B), C44(H44A,H44B)
5.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C3(H3A), C4(H4), C0AA(H0AA), C1AA(H1AA), C16(H16), C17(H17),
 C20(H20), C21(H21)
5.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C33(H33A,H33B,H33C), C33B(H33D,H33E,H33F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Cl1 Cl 0.6352(5) 0.3434(2) 0.2699(8) 0.116(2) Uani 0.61(2) 1 d . . . A 1
Cl2 Cl 0.6322(6) 0.3333(5) 0.2241(11) 0.096(4) Uani 0.39(2) 1 d . . . A 2
C40 C 0.7500 0.2854(3) 0.2500 0.0553(15) Uani 1 2 d S T P . .
H40A H 0.7717 0.2514 0.2951 0.066 Uiso 0.307(11) 1 calc R . . A 1
H40B H 0.7283 0.2514 0.2049 0.066 Uiso 0.307(11) 1 calc R . . A 1
H40C H 0.7379 0.2509 0.2938 0.066 Uiso 0.193(11) 1 calc R . . A 2
H40D H 0.7621 0.2509 0.2062 0.066 Uiso 0.193(11) 1 calc R . . A 2
O6 O 0.7435(2) 0.24936(15) 0.66833(13) 0.0491(7) Uani 1 1 d . . . . .
C34 C 0.7754(3) 0.1815(2) 0.7129(2) 0.0527(10) Uani 1 1 d . . . . .
H34A H 0.8549 0.1805 0.7247 0.063 Uiso 1 1 calc R . . . .
H34B H 0.7531 0.1341 0.6827 0.063 Uiso 1 1 calc R . . . .
C35 C 0.7741(4) 0.3172(2) 0.7126(2) 0.0556(11) Uani 1 1 d . . . . .
H35A H 0.7499 0.3642 0.6824 0.067 Uiso 1 1 calc R . . . .
H35B H 0.8536 0.3193 0.7232 0.067 Uiso 1 1 calc R . . . .
O1 O 0.61003(18) -0.09610(13) 0.73645(12) 0.0388(6) Uani 1 1 d . . . . .
O2 O 0.92876(19) -0.10289(13) 0.63710(12) 0.0380(6) Uani 1 1 d . . . . .
O3 O 0.75091(18) 0.18335(15) 0.39883(11) 0.0420(6) Uani 1 1 d . . . . .
O4 O 0.35476(18) 0.21987(15) 0.45433(13) 0.0433(6) Uani 1 1 d . . . . .
O5 O 1.0683(2) 0.33443(14) 0.59476(14) 0.0455(6) Uani 1 1 d . . . . .
C43 C 0.4175(3) -0.0194(2) 0.75551(17) 0.0345(8) Uani 1 1 d . . . . .
H43 H 0.3413 -0.0008 0.7462 0.041 Uiso 1 1 calc R . . . .
N2 N 0.6448(2) 0.20463(16) 0.49468(14) 0.0346(7) Uani 1 1 d . . . . .
H2 H 0.6363 0.2292 0.5380 0.042 Uiso 1 1 calc R . . . .
N3 N 0.8181(2) 0.24996(16) 0.50727(14) 0.0327(6) Uani 1 1 d . . . . .
H3 H 0.8007 0.2789 0.5458 0.039 Uiso 1 1 calc R . . . .
C1 C 0.4779(2) 0.00057(19) 0.68696(17) 0.0313(7) Uani 1 1 d . . . . .
C2 C 0.5743(3) -0.03784(19) 0.68535(17) 0.0331(8) Uani 1 1 d . . . . .
C3 C 0.6454(3) -0.0185(2) 0.62996(17) 0.0343(8) Uani 1 1 d . . . . .
H3A H 0.7123 -0.0448 0.6301 0.041 Uiso 1 1 calc R . . . .
C4 C 0.6165(3) 0.03783(19) 0.57689(17) 0.0328(8) Uani 1 1 d . . . . .
H4 H 0.6661 0.0525 0.5419 0.039 Uiso 1 1 calc R . . . .
C5 C 0.5146(3) 0.0758(2) 0.57165(17) 0.0326(8) Uani 1 1 d . . . . .
C6 C 0.4425(3) 0.05336(19) 0.62640(16) 0.0310(7) Uani 1 1 d . . . . .
C0AA C 0.3369(3) 0.08370(19) 0.61499(17) 0.0327(8) Uani 1 1 d . . . . .
H0AA H 0.2859 0.0663 0.6478 0.039 Uiso 1 1 calc R . . . .
C1AA C 0.3050(3) 0.1369(2) 0.55888(17) 0.0341(8) Uani 1 1 d . . . . .
H1AA H 0.2331 0.1560 0.5530 0.041 Uiso 1 1 calc R . . . .
C9 C 0.3798(3) 0.1636(2) 0.50927(17) 0.0343(8) Uani 1 1 d . . . . .
C10 C 0.4821(2) 0.13228(19) 0.51393(17) 0.0318(7) Uani 1 1 d . . . . .
C11 C 0.5581(3) 0.1568(2) 0.45682(17) 0.0348(8) Uani 1 1 d . . . . .
H11A H 0.5889 0.1099 0.4344 0.042 Uiso 1 1 calc R . . . .
H11B H 0.5180 0.1867 0.4141 0.042 Uiso 1 1 calc R . . . .
C12 C 0.7397(3) 0.21128(19) 0.46271(17) 0.0316(7) Uani 1 1 d . . . . .
C13 C 0.9322(2) 0.2450(2) 0.49308(18) 0.0355(8) Uani 1 1 d . . . . .
H13A H 0.9598 0.2977 0.4828 0.043 Uiso 1 1 calc R . . . .
H13B H 0.9389 0.2120 0.4472 0.043 Uiso 1 1 calc R . . . .
C14 C 0.9973(2) 0.2102(2) 0.56382(17) 0.0316(8) Uani 1 1 d . . . . .
C15 C 1.0614(3) 0.2571(2) 0.61400(18) 0.0345(8) Uani 1 1 d . . . . .
C16 C 1.1148(3) 0.2261(2) 0.68295(18) 0.0370(8) Uani 1 1 d . . . . .
H16 H 1.1581 0.2590 0.7177 0.044 Uiso 1 1 calc R . . . .
C17 C 1.1046(3) 0.1492(2) 0.70007(18) 0.0351(8) Uani 1 1 d . . . . .
H17 H 1.1424 0.1295 0.7465 0.042 Uiso 1 1 calc R . . . .
C18 C 1.0400(2) 0.0976(2) 0.65131(16) 0.0308(7) Uani 1 1 d . . . . .
C19 C 0.9848(2) 0.1300(2) 0.58200(16) 0.0304(7) Uani 1 1 d . . . . .
C20 C 0.9151(2) 0.0797(2) 0.53364(17) 0.0311(8) Uani 1 1 d . . . . .
H20 H 0.8790 0.0992 0.4865 0.037 Uiso 1 1 calc R . . . .
C21 C 0.8998(3) 0.0045(2) 0.55402(17) 0.0324(8) Uani 1 1 d . . . . .
H21 H 0.8521 -0.0277 0.5215 0.039 Uiso 1 1 calc R . . . .
C22 C 0.9539(3) -0.0263(2) 0.62275(17) 0.0324(8) Uani 1 1 d . . . . .
C23 C 1.0254(2) 0.0173(2) 0.67077(17) 0.0320(8) Uani 1 1 d . . . . .
C24 C 0.5375(3) -0.1288(2) 0.78650(18) 0.0399(8) Uani 1 1 d . . . . .
H24 H 0.5444 -0.1869 0.7853 0.048 Uiso 1 1 calc R . . . .
C25 C 0.4209(3) -0.1079(2) 0.76367(19) 0.0395(9) Uani 1 1 d . . . . .
H25A H 0.3760 -0.1251 0.8039 0.047 Uiso 1 1 calc R . . . .
H25B H 0.3937 -0.1331 0.7140 0.047 Uiso 1 1 calc R . . . .
C26 C 0.2475(3) 0.2501(2) 0.4444(2) 0.0478(9) Uani 1 1 d . . . . .
H26A H 0.2294 0.2737 0.4933 0.057 Uiso 1 1 calc R . . . .
H26B H 0.1953 0.2078 0.4293 0.057 Uiso 1 1 calc R . . . .
C27 C 0.2431(3) 0.3116(3) 0.3807(2) 0.0603(12) Uani 1 1 d . . . . .
H27A H 0.2954 0.3536 0.3967 0.072 Uiso 1 1 calc R . . . .
H27B H 0.2640 0.2876 0.3328 0.072 Uiso 1 1 calc R . . . .
C28 C 0.1322(4) 0.3458(3) 0.3648(3) 0.0743(14) Uani 1 1 d . . . . .
H28A H 0.1058 0.3601 0.4144 0.089 Uiso 1 1 calc DR . . . .
H28B H 0.0828 0.3060 0.3394 0.089 Uiso 1 1 calc R . . . .
C29 C 0.1301(5) 0.4174(3) 0.3133(4) 0.0959(18) Uani 1 1 d . . . . .
H29A H 0.1611 0.4045 0.2656 0.144 Uiso 1 1 calc GR . . . .
H29B H 0.1724 0.4591 0.3407 0.144 Uiso 1 1 calc GR . . . .
H29C H 0.0554 0.4348 0.3005 0.144 Uiso 1 1 calc GR . . . .
C30 C 1.1369(4) 0.3836(2) 0.6444(2) 0.0688(13) Uani 1 1 d . . . . .
H30A H 1.2118 0.3639 0.6487 0.083 Uiso 1 1 calc R . . . .
H30B H 1.1130 0.3844 0.6967 0.083 Uiso 1 1 calc R . . . .
C31 C 1.1315(5) 0.4637(3) 0.6106(3) 0.0871(17) Uani 1 1 d . . . . .
H31A H 1.0548 0.4791 0.6015 0.105 Uiso 0.75 1 calc R . . B 1
H31B H 1.1673 0.4998 0.6499 0.105 Uiso 0.75 1 calc R . . B 1
H31C H 1.0754 0.4948 0.6323 0.105 Uiso 0.25 1 calc R . . C 2
H31D H 1.1139 0.4612 0.5537 0.105 Uiso 0.25 1 calc R . . C 2
C32 C 1.1768(5) 0.4749(3) 0.5424(3) 0.0638(16) Uani 0.75 1 d . . . D 1
H32A H 1.1367 0.4422 0.5020 0.077 Uiso 0.75 1 calc DR . . D 1
H32B H 1.2517 0.4551 0.5502 0.077 Uiso 0.75 1 calc R . . D 1
C33 C 1.1800(6) 0.5565(3) 0.5115(4) 0.0749(18) Uani 0.75 1 d . . . D 1
H33A H 1.2083 0.5557 0.4612 0.112 Uiso 0.75 1 calc GR . . D 1
H33B H 1.2267 0.5887 0.5477 0.112 Uiso 0.75 1 calc GR . . D 1
H33C H 1.1070 0.5783 0.5053 0.112 Uiso 0.75 1 calc GR . . D 1
O11 O 0.4068(3) 0.3871(2) 0.6574(2) 0.0772(12) Uani 0.8 1 d . . . E 1
O10 O 0.5702(5) 0.4497(4) 0.5748(3) 0.089(2) Uani 0.8 1 d . U . E 1
C36 C 0.4669(6) 0.4541(3) 0.6838(4) 0.0783(18) Uani 0.8 1 d . . . E 1
H36A H 0.5305 0.4379 0.7194 0.094 Uiso 0.8 1 calc R . . E 1
H36B H 0.4217 0.4881 0.7129 0.094 Uiso 0.8 1 calc R . . E 1
C38 C 0.5045(9) 0.3828(5) 0.5475(4) 0.083(3) Uani 0.8 1 d D U . E 1
H38A H 0.5461 0.3490 0.5156 0.100 Uiso 0.8 1 calc R . . E 1
H38B H 0.4396 0.4011 0.5145 0.100 Uiso 0.8 1 calc R . . E 1
C32B C 1.2529(19) 0.5042(10) 0.6335(11) 0.076(6) Uani 0.25 1 d . . . D 2
H32C H 1.2655 0.5135 0.6900 0.091 Uiso 0.25 1 calc R . . D 2
H32D H 1.3097 0.4686 0.6190 0.091 Uiso 0.25 1 calc R . . D 2
C33B C 1.257(2) 0.5812(13) 0.5901(13) 0.101(7) Uani 0.25 1 d . U . D 2
H33D H 1.2711 0.5709 0.5366 0.151 Uiso 0.25 1 calc GR . . D 2
H33E H 1.3153 0.6136 0.6157 0.151 Uiso 0.25 1 calc GR . . D 2
H33F H 1.1884 0.6085 0.5900 0.151 Uiso 0.25 1 calc GR . . D 2
Cl4 Cl 0.4632(9) 0.3175(6) 0.6377(5) 0.064(2) Uani 0.2 1 d D U . F 2
C39 C 0.5033(7) 0.4989(4) 0.6179(4) 0.0819(19) Uani 0.8 1 d . U . E 1
H39A H 0.4399 0.5172 0.5833 0.098 Uiso 0.8 1 calc R . . E 1
H39B H 0.5450 0.5451 0.6379 0.098 Uiso 0.8 1 calc R . . E 1
C42 C 0.4709(9) 0.3367(6) 0.6136(5) 0.066(3) Uani 0.8 1 d D U . E 1
H42A H 0.4279 0.2909 0.5940 0.079 Uiso 0.8 1 calc R . . E 1
H42B H 0.5352 0.3179 0.6471 0.079 Uiso 0.8 1 calc R . . E 1
Cl3 Cl 0.5779(11) 0.4613(7) 0.6157(8) 0.110(3) Uani 0.2 1 d D U . F 2
C44 C 0.512(4) 0.3815(19) 0.576(2) 0.083(3) Uani 0.2 1 d D . . F 2
H44A H 0.4504 0.3999 0.5389 0.100 Uiso 0.2 1 calc R . . F 2
H44B H 0.5613 0.3530 0.5451 0.100 Uiso 0.2 1 calc R . . F 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C40 1.810(5) . ?
Cl2 C40 1.700(7) . ?
C40 Cl1 1.810(5) 2_655 ?
C40 Cl2 1.700(7) 2_655 ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 H40C 0.9900 . ?
C40 H40D 0.9900 . ?
O6 C34 1.430(5) . ?
O6 C35 1.423(4) . ?
C34 C34 1.500(7) 2_656 ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C35 1.495(7) 2_656 ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
O1 C2 1.377(4) . ?
O1 C24 1.439(4) . ?
O2 C22 1.381(4) . ?
O2 C24 1.418(4) 2_656 ?
O3 C12 1.232(4) . ?
O4 C9 1.369(4) . ?
O4 C26 1.428(4) . ?
O5 C15 1.373(4) . ?
O5 C30 1.421(5) . ?
C43 H43 1.0000 . ?
C43 C1 1.520(4) . ?
C43 C23 1.530(4) 2_656 ?
C43 C25 1.525(5) . ?
N2 H2 0.8800 . ?
N2 C11 1.455(4) . ?
N2 C12 1.370(4) . ?
N3 H3 0.8800 . ?
N3 C12 1.351(4) . ?
N3 C13 1.476(4) . ?
C1 C2 1.376(4) . ?
C1 C6 1.420(4) . ?
C2 C3 1.421(4) . ?
C3 H3A 0.9500 . ?
C3 C4 1.356(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.423(4) . ?
C5 C6 1.436(4) . ?
C5 C10 1.420(5) . ?
C6 C0AA 1.411(4) . ?
C0AA H0AA 0.9500 . ?
C0AA C1AA 1.362(5) . ?
C1AA H1AA 0.9500 . ?
C1AA C9 1.418(4) . ?
C9 C10 1.380(4) . ?
C10 C11 1.510(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.518(4) . ?
C14 C15 1.376(5) . ?
C14 C19 1.423(5) . ?
C15 C16 1.408(5) . ?
C16 H16 0.9500 . ?
C16 C17 1.361(5) . ?
C17 H17 0.9500 . ?
C17 C18 1.414(5) . ?
C18 C19 1.431(4) . ?
C18 C23 1.434(5) . ?
C19 C20 1.429(5) . ?
C20 H20 0.9500 . ?
C20 C21 1.358(5) . ?
C21 H21 0.9500 . ?
C21 C22 1.407(4) . ?
C22 C23 1.372(5) . ?
C23 C43 1.530(4) 2_656 ?
C24 O2 1.418(4) 2_656 ?
C24 H24 1.0000 . ?
C24 C25 1.509(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.525(5) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.501(6) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.518(7) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.494(6) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 H31C 0.9900 . ?
C31 H31D 0.9900 . ?
C31 C32 1.383(7) . ?
C31 C32B 1.67(2) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.501(8) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
O11 C36 1.419(7) . ?
O11 C42 1.453(11) . ?
O10 C38 1.458(9) . ?
O10 C39 1.454(9) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C39 1.492(9) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C42 1.494(7) . ?
C32B H32C 0.9900 . ?
C32B H32D 0.9900 . ?
C32B C33B 1.53(3) . ?
C33B H33D 0.9800 . ?
C33B H33E 0.9800 . ?
C33B H33F 0.9800 . ?
Cl4 C44 1.70(2) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
Cl3 C44 1.71(2) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?

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
Cl1 C40 Cl1 113.3(4) 2_655 . ?
Cl1 C40 H40A 108.9 2_655 . ?
Cl1 C40 H40A 108.9 . . ?
Cl1 C40 H40B 108.9 2_655 . ?
Cl1 C40 H40B 108.9 . . ?
Cl2 C40 Cl2 122.2(6) 2_655 . ?
Cl2 C40 H40C 106.8 . . ?
Cl2 C40 H40C 106.8 2_655 . ?
Cl2 C40 H40D 106.8 2_655 . ?
Cl2 C40 H40D 106.8 . . ?
H40A C40 H40B 107.7 . . ?
H40C C40 H40D 106.6 . . ?
C35 O6 C34 109.4(3) . . ?
O6 C34 C34 110.3(3) . 2_656 ?
O6 C34 H34A 109.6 . . ?
O6 C34 H34B 109.6 . . ?
C34 C34 H34A 109.6 2_656 . ?
C34 C34 H34B 109.6 2_656 . ?
H34A C34 H34B 108.1 . . ?
O6 C35 C35 111.1(3) . 2_656 ?
O6 C35 H35A 109.4 . . ?
O6 C35 H35B 109.4 . . ?
C35 C35 H35A 109.4 2_656 . ?
C35 C35 H35B 109.4 2_656 . ?
H35A C35 H35B 108.0 . . ?
C2 O1 C24 119.5(3) . . ?
C22 O2 C24 114.7(3) . 2_656 ?
C9 O4 C26 118.5(3) . . ?
C15 O5 C30 118.4(3) . . ?
C1 C43 H43 110.4 . . ?
C1 C43 C23 109.8(2) . 2_656 ?
C1 C43 C25 106.7(3) . . ?
C23 C43 H43 110.4 2_656 . ?
C25 C43 H43 110.4 . . ?
C25 C43 C23 109.1(3) . 2_656 ?
C11 N2 H2 120.1 . . ?
C12 N2 H2 120.1 . . ?
C12 N2 C11 119.8(3) . . ?
C12 N3 H3 119.1 . . ?
C12 N3 C13 121.7(3) . . ?
C13 N3 H3 119.1 . . ?
C2 C1 C43 114.9(3) . . ?
C2 C1 C6 119.3(3) . . ?
C6 C1 C43 125.8(3) . . ?
O1 C2 C3 115.1(3) . . ?
C1 C2 O1 123.7(3) . . ?
C1 C2 C3 121.2(3) . . ?
C2 C3 H3A 120.4 . . ?
C4 C3 C2 119.3(3) . . ?
C4 C3 H3A 120.4 . . ?
C3 C4 H4 118.8 . . ?
C3 C4 C5 122.4(3) . . ?
C5 C4 H4 118.8 . . ?
C4 C5 C6 117.3(3) . . ?
C10 C5 C4 122.6(3) . . ?
C10 C5 C6 120.1(3) . . ?
C1 C6 C5 119.8(3) . . ?
C0AA C6 C1 123.1(3) . . ?
C0AA C6 C5 117.1(3) . . ?
C6 C0AA H0AA 118.6 . . ?
C1AA C0AA C6 122.7(3) . . ?
C1AA C0AA H0AA 118.6 . . ?
C0AA C1AA H1AA 120.2 . . ?
C0AA C1AA C9 119.5(3) . . ?
C9 C1AA H1AA 120.2 . . ?
O4 C9 C1AA 122.6(3) . . ?
O4 C9 C10 116.9(3) . . ?
C10 C9 C1AA 120.6(3) . . ?
C5 C10 C11 120.2(3) . . ?
C9 C10 C5 119.7(3) . . ?
C9 C10 C11 120.0(3) . . ?
N2 C11 C10 110.6(2) . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 108.1 . . ?
O3 C12 N2 121.7(3) . . ?
O3 C12 N3 124.0(3) . . ?
N3 C12 N2 114.3(3) . . ?
N3 C13 H13A 109.9 . . ?
N3 C13 H13B 109.9 . . ?
N3 C13 C14 109.0(2) . . ?
H13A C13 H13B 108.3 . . ?
C14 C13 H13A 109.9 . . ?
C14 C13 H13B 109.9 . . ?
C15 C14 C13 120.2(3) . . ?
C15 C14 C19 119.7(3) . . ?
C19 C14 C13 119.9(3) . . ?
O5 C15 C14 117.4(3) . . ?
O5 C15 C16 122.4(3) . . ?
C14 C15 C16 120.2(3) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 C15 120.4(3) . . ?
C17 C16 H16 119.8 . . ?
C16 C17 H17 118.8 . . ?
C16 C17 C18 122.5(3) . . ?
C18 C17 H17 118.8 . . ?
C17 C18 C19 116.7(3) . . ?
C17 C18 C23 122.6(3) . . ?
C19 C18 C23 120.7(3) . . ?
C14 C19 C18 120.6(3) . . ?
C14 C19 C20 121.8(3) . . ?
C20 C19 C18 117.6(3) . . ?
C19 C20 H20 119.5 . . ?
C21 C20 C19 121.0(3) . . ?
C21 C20 H20 119.5 . . ?
C20 C21 H21 119.7 . . ?
C20 C21 C22 120.6(3) . . ?
C22 C21 H21 119.7 . . ?
O2 C22 C21 114.4(3) . . ?
C23 C22 O2 123.7(3) . . ?
C23 C22 C21 121.9(3) . . ?
C18 C23 C43 122.3(3) . 2_656 ?
C22 C23 C43 119.6(3) . 2_656 ?
C22 C23 C18 118.1(3) . . ?
O1 C24 H24 108.3 . . ?
O1 C24 C25 113.8(3) . . ?
O2 C24 O1 107.7(3) 2_656 . ?
O2 C24 H24 108.3 2_656 . ?
O2 C24 C25 110.3(3) 2_656 . ?
C25 C24 H24 108.3 . . ?
C43 C25 H25A 110.5 . . ?
C43 C25 H25B 110.5 . . ?
C24 C25 C43 106.1(3) . . ?
C24 C25 H25A 110.5 . . ?
C24 C25 H25B 110.5 . . ?
H25A C25 H25B 108.7 . . ?
O4 C26 H26A 110.3 . . ?
O4 C26 H26B 110.3 . . ?
O4 C26 C27 107.1(3) . . ?
H26A C26 H26B 108.5 . . ?
C27 C26 H26A 110.3 . . ?
C27 C26 H26B 110.3 . . ?
C26 C27 H27A 109.4 . . ?
C26 C27 H27B 109.4 . . ?
H27A C27 H27B 108.0 . . ?
C28 C27 C26 111.1(4) . . ?
C28 C27 H27A 109.4 . . ?
C28 C27 H27B 109.4 . . ?
C27 C28 H28A 109.1 . . ?
C27 C28 H28B 109.1 . . ?
C27 C28 C29 112.3(4) . . ?
H28A C28 H28B 107.9 . . ?
C29 C28 H28A 109.1 . . ?
C29 C28 H28B 109.1 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O5 C30 H30A 110.1 . . ?
O5 C30 H30B 110.1 . . ?
O5 C30 C31 108.1(4) . . ?
H30A C30 H30B 108.4 . . ?
C31 C30 H30A 110.1 . . ?
C31 C30 H30B 110.1 . . ?
C30 C31 H31A 107.9 . . ?
C30 C31 H31B 107.9 . . ?
C30 C31 H31C 110.3 . . ?
C30 C31 H31D 110.3 . . ?
C30 C31 C32B 106.9(7) . . ?
H31A C31 H31B 107.2 . . ?
H31C C31 H31D 108.6 . . ?
C32 C31 C30 117.4(5) . . ?
C32 C31 H31A 107.9 . . ?
C32 C31 H31B 107.9 . . ?
C32B C31 H31C 110.3 . . ?
C32B C31 H31D 110.3 . . ?
C31 C32 H32A 107.8 . . ?
C31 C32 H32B 107.8 . . ?
C31 C32 C33 117.8(5) . . ?
H32A C32 H32B 107.2 . . ?
C33 C32 H32A 107.8 . . ?
C33 C32 H32B 107.8 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C36 O11 C42 110.4(6) . . ?
C39 O10 C38 106.9(7) . . ?
O11 C36 H36A 109.3 . . ?
O11 C36 H36B 109.3 . . ?
O11 C36 C39 111.5(5) . . ?
H36A C36 H36B 108.0 . . ?
C39 C36 H36A 109.3 . . ?
C39 C36 H36B 109.3 . . ?
O10 C38 H38A 109.4 . . ?
O10 C38 H38B 109.4 . . ?
O10 C38 C42 111.3(6) . . ?
H38A C38 H38B 108.0 . . ?
C42 C38 H38A 109.4 . . ?
C42 C38 H38B 109.4 . . ?
C31 C32B H32C 109.9 . . ?
C31 C32B H32D 109.9 . . ?
H32C C32B H32D 108.3 . . ?
C33B C32B C31 108.9(17) . . ?
C33B C32B H32C 109.9 . . ?
C33B C32B H32D 109.9 . . ?
C32B C33B H33D 109.5 . . ?
C32B C33B H33E 109.5 . . ?
C32B C33B H33F 109.5 . . ?
H33D C33B H33E 109.5 . . ?
H33D C33B H33F 109.5 . . ?
H33E C33B H33F 109.5 . . ?
O10 C39 C36 109.9(6) . . ?
O10 C39 H39A 109.7 . . ?
O10 C39 H39B 109.7 . . ?
C36 C39 H39A 109.7 . . ?
C36 C39 H39B 109.7 . . ?
H39A C39 H39B 108.2 . . ?
O11 C42 C38 107.9(7) . . ?
O11 C42 H42A 110.1 . . ?
O11 C42 H42B 110.1 . . ?
C38 C42 H42A 110.1 . . ?
C38 C42 H42B 110.1 . . ?
H42A C42 H42B 108.4 . . ?
Cl4 C44 Cl3 117(2) . . ?
Cl4 C44 H44A 108.1 . . ?
Cl4 C44 H44B 108.1 . . ?
Cl3 C44 H44A 108.1 . . ?
Cl3 C44 H44B 108.1 . . ?
H44A C44 H44B 107.3 . . ?

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
C34 O6 C35 C35 -57.2(5) . . . 2_656 ?
C35 O6 C34 C34 58.3(5) . . . 2_656 ?
O1 C2 C3 C4 179.5(3) . . . . ?
O1 C24 C25 C43 -51.8(3) . . . . ?
O2 C22 C23 C43 0.5(4) . . . 2_656 ?
O2 C22 C23 C18 -176.7(3) . . . . ?
O2 C24 C25 C43 69.3(3) 2_656 . . . ?
O4 C9 C10 C5 177.6(3) . . . . ?
O4 C9 C10 C11 -3.7(4) . . . . ?
O4 C26 C27 C28 178.8(3) . . . . ?
O5 C15 C16 C17 179.2(3) . . . . ?
O5 C30 C31 C32 -68.9(6) . . . . ?
O5 C30 C31 C32B -147.5(8) . . . . ?
C43 C1 C2 O1 6.6(4) . . . . ?
C43 C1 C2 C3 -172.6(3) . . . . ?
C43 C1 C6 C5 170.5(3) . . . . ?
C43 C1 C6 C0AA -11.8(5) . . . . ?
N3 C13 C14 C15 -104.2(3) . . . . ?
N3 C13 C14 C19 70.3(4) . . . . ?
C1 C43 C25 C24 66.3(3) . . . . ?
C1 C2 C3 C4 -1.2(5) . . . . ?
C1 C6 C0AA C1AA 177.0(3) . . . . ?
C2 O1 C24 O2 -108.8(3) . . . 2_656 ?
C2 O1 C24 C25 13.8(4) . . . . ?
C2 C1 C6 C5 -10.2(4) . . . . ?
C2 C1 C6 C0AA 167.4(3) . . . . ?
C2 C3 C4 C5 -3.5(5) . . . . ?
C3 C4 C5 C6 1.3(5) . . . . ?
C3 C4 C5 C10 -177.0(3) . . . . ?
C4 C5 C6 C1 5.6(4) . . . . ?
C4 C5 C6 C0AA -172.2(3) . . . . ?
C4 C5 C10 C9 176.2(3) . . . . ?
C4 C5 C10 C11 -2.5(5) . . . . ?
C5 C6 C0AA C1AA -5.2(5) . . . . ?
C5 C10 C11 N2 -72.0(4) . . . . ?
C6 C1 C2 O1 -172.7(3) . . . . ?
C6 C1 C2 C3 8.1(5) . . . . ?
C6 C5 C10 C9 -2.0(5) . . . . ?
C6 C5 C10 C11 179.3(3) . . . . ?
C6 C0AA C1AA C9 0.0(5) . . . . ?
C0AA C1AA C9 O4 -176.6(3) . . . . ?
C0AA C1AA C9 C10 4.4(5) . . . . ?
C1AA C9 C10 C5 -3.4(5) . . . . ?
C1AA C9 C10 C11 175.4(3) . . . . ?
C9 O4 C26 C27 179.5(3) . . . . ?
C9 C10 C11 N2 109.3(3) . . . . ?
C10 C5 C6 C1 -176.0(3) . . . . ?
C10 C5 C6 C0AA 6.2(4) . . . . ?
C11 N2 C12 O3 6.5(5) . . . . ?
C11 N2 C12 N3 -173.0(3) . . . . ?
C12 N2 C11 C10 158.1(3) . . . . ?
C12 N3 C13 C14 -118.7(3) . . . . ?
C13 N3 C12 O3 -16.1(5) . . . . ?
C13 N3 C12 N2 163.4(3) . . . . ?
C13 C14 C15 O5 -3.7(4) . . . . ?
C13 C14 C15 C16 174.7(3) . . . . ?
C13 C14 C19 C18 -175.7(3) . . . . ?
C13 C14 C19 C20 2.4(4) . . . . ?
C14 C15 C16 C17 0.9(5) . . . . ?
C14 C19 C20 C21 -176.4(3) . . . . ?
C15 O5 C30 C31 179.2(4) . . . . ?
C15 C14 C19 C18 -1.1(4) . . . . ?
C15 C14 C19 C20 177.0(3) . . . . ?
C15 C16 C17 C18 -1.1(5) . . . . ?
C16 C17 C18 C19 0.1(4) . . . . ?
C16 C17 C18 C23 -177.2(3) . . . . ?
C17 C18 C19 C14 1.0(4) . . . . ?
C17 C18 C19 C20 -177.2(3) . . . . ?
C17 C18 C23 C43 -2.5(4) . . . 2_656 ?
C17 C18 C23 C22 174.6(3) . . . . ?
C18 C19 C20 C21 1.7(4) . . . . ?
C19 C14 C15 O5 -178.2(3) . . . . ?
C19 C14 C15 C16 0.1(4) . . . . ?
C19 C18 C23 C43 -179.7(3) . . . 2_656 ?
C19 C18 C23 C22 -2.6(4) . . . . ?
C19 C20 C21 C22 -1.2(4) . . . . ?
C20 C21 C22 O2 178.5(3) . . . . ?
C20 C21 C22 C23 -1.4(4) . . . . ?
C21 C22 C23 C43 -179.6(3) . . . 2_656 ?
C21 C22 C23 C18 3.3(4) . . . . ?
C23 C43 C1 C2 72.7(4) 2_656 . . . ?
C23 C43 C1 C6 -108.0(3) 2_656 . . . ?
C23 C43 C25 C24 -52.2(3) 2_656 . . . ?
C23 C18 C19 C14 178.4(3) . . . . ?
C23 C18 C19 C20 0.2(4) . . . . ?
C24 O1 C2 C1 10.8(4) . . . . ?
C24 O1 C2 C3 -170.0(3) . . . . ?
C24 O2 C22 C21 -166.1(3) 2_656 . . . ?
C24 O2 C22 C23 13.9(4) 2_656 . . . ?
C25 C43 C1 C2 -45.4(4) . . . . ?
C25 C43 C1 C6 133.9(3) . . . . ?
C26 O4 C9 C1AA -3.0(5) . . . . ?
C26 O4 C9 C10 176.0(3) . . . . ?
C26 C27 C28 C29 169.0(4) . . . . ?
C30 O5 C15 C14 -177.9(3) . . . . ?
C30 O5 C15 C16 3.7(5) . . . . ?
C30 C31 C32 C33 -175.1(5) . . . . ?
C30 C31 C32B C33B 171.4(13) . . . . ?
O11 C36 C39 O10 -59.3(8) . . . . ?
O10 C38 C42 O11 61.1(10) . . . . ?
C36 O11 C42 C38 -58.0(8) . . . . ?
C38 O10 C39 C36 58.9(8) . . . . ?
C39 O10 C38 C42 -61.7(10) . . . . ?
C42 O11 C36 C39 58.4(7) . . . . ?

_shelx_SHELXL_version_number     2014/7
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
-13 5 17 0.0554 -13.0000 5.0000 17.0000 0.9735 -0.1284 0.0122
15 -5 -14 0.0596 15.0000 -5.0000 -14.0000 -0.9783 0.1104 0.1641
-10 2 -18 0.2674 -10.0000 2.0000 -18.0000 -0.0453 0.0114 -0.9865
-3 2 24 0.1737 -3.0000 2.0000 24.0000 0.7365 -0.0866 0.6476
4 -23 -6 0.0109 4.0000 -23.0000 -6.0000 -0.3921 0.9208 0.0576
-4 23 6 0.0201 -4.0000 23.0000 6.0000 0.3921 -0.9208 -0.0576
11 16 -11 0.0672 11.0000 16.0000 -11.0000 -0.6690 -0.7250 0.0177
-11 -16 12 0.0575 -11.0000 -16.0000 12.0000 0.6943 0.7239 0.0146

_olex2_submission_special_instructions 'No special instructions were received'
