# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 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_CHCl3@1(5)4
_database_code_depnum_ccdc_archive 'CCDC 1038850'
_audit_update_record             
;
2014-12-11 deposited with the CCDC.
2015-01-26 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT043_CHCl3@154           
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..
RESPONSE: The structure contains disordered solvent molecules which are
          not fully assigned. The reported molecular formule corresponds
          to the one with whole guest molecules.
;
_vrf_PLAT342_CHCl3@154           
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............
RESPONSE: The low bond precision is caused by the vibration of the whole 
          molecule in the structure which cannot be suppressed by cooling down 
          the temperature, bacause the data were collected 123K.
;
# end Validation Reply Form

_audit_creation_date             2014-12-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
'4(Br), C64 H88 N4 O8, 2(C6 F4 I2), C0.5 Cl1.5, C0.24 H0.24 Cl0.72'
_chemical_formula_sum            'C77 H89 Br4 Cl3 F8 I4 N4 O8'
_chemical_formula_weight         2284.11
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C76 H96 Br4 N4 O8 F8 I4'
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'
Br Br -0.6763 1.2805 '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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 '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      tetragonal
_space_group_IT_number           130
_space_group_name_H-M_alt        'P 4/n c c'
_space_group_name_Hall           '-P 4a 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z+1/2'
'-x, y+1/2, -z+1/2'
'-y, -x, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'y, -x+1/2, z'
'-y+1/2, x, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z-1/2'
'x, -y-1/2, z-1/2'
'y, x, z-1/2'
'-y-1/2, -x-1/2, z-1/2'
'-y, x-1/2, -z'
'y-1/2, -x, -z'

_cell_length_a                   18.4165(3)
_cell_length_b                   18.4165(3)
_cell_length_c                   27.9044(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9464.3(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4011
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      61.8190
_cell_measurement_theta_min      3.9620
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.643
_exptl_absorpt_correction_T_max  0.664
_exptl_absorpt_correction_T_min  0.294
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             4472
_exptl_crystal_size_max          0.1932
_exptl_crystal_size_mid          0.0837
_exptl_crystal_size_min          0.0327
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12644
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        62.500
_diffrn_reflns_theta_max         62.445
_diffrn_reflns_theta_min         3.167
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -2.00   60.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   37.0000 -180.0000 124

#__ type_ start__ end____ width___ exp.time_
  2 omega   14.00   85.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       83.4688  -30.0000    0.0000 142

#__ type_ start__ end____ width___ exp.time_
  3 omega   94.00  137.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       83.4688  125.0000    0.0000 86

#__ type_ start__ end____ width___ exp.time_
  4 omega   72.00  143.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       83.4688   45.0000  150.0000 142
;
_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      0.0025905000
_diffrn_orient_matrix_UB_12      0.0425069000
_diffrn_orient_matrix_UB_13      0.0475234000
_diffrn_orient_matrix_UB_21      -0.0639993000
_diffrn_orient_matrix_UB_22      0.0473255000
_diffrn_orient_matrix_UB_23      -0.0168931000
_diffrn_orient_matrix_UB_31      -0.0538472000
_diffrn_orient_matrix_UB_32      -0.0543224000
_diffrn_orient_matrix_UB_33      0.0224088000
_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                2462
_reflns_number_total             3713
_reflns_odcompleteness_completeness 95.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     62.94
_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 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.206
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.162
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         3713
_refine_ls_number_restraints     67
_refine_ls_R_factor_all          0.1264
_refine_ls_R_factor_gt           0.1053
_refine_ls_restrained_S_all      1.022
_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)+(0.1700P)²+45.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3000
_refine_ls_wR_factor_ref         0.3286
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H11 of C11, H6 of C6, H7 of C7, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H21 of C21, All O(H) groups
2. Restrained distances
 O1-H1
 0.84 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C17 \\sim C18 \\sim C19 \\sim F18 \\sim F19: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C20 \\sim Cl1 \\sim Cl2: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(Cl3) \\sim Ueq, Uanis(Cl4) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.02 and sigma for terminal
atoms of 0.04
4. Others
 Fixed Sof: Br1(0.6) Br1B(0.4) Cl1(0.125) Cl2(0.25) C20(0.125) Cl3(0.09)
 Cl4(0.09) C21(0.06) H21(0.06)
5.a Riding coordinates:
 O2(H2), C21(H21)
5.b Ternary CH refined with riding coordinates:
 C7(H7), C11(H11)
5.c Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C8(H8A,H8B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B), C16(H16A,H16B)
5.d Me refined with riding coordinates:
 C9(H9A,H9B,H9C)
5.e Aromatic/amide H refined with riding coordinates:
 C6(H6)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.1291(2) 0.0221(2) 0.48146(13) 0.1081(10) Uani 0.6 1 d . . . A 1
Br1B Br 0.1525(3) 0.0566(3) 0.4809(2) 0.1090(15) Uani 0.4 1 d . . . B 2
O1 O 0.4731(6) 0.1084(6) 0.5910(4) 0.120(3) Uani 1 1 d D . . . .
H1 H 0.488(11) 0.107(12) 0.562(3) 0.180 Uiso 1 1 d DR . . . .
O2 O 0.2488(7) -0.0155(5) 0.5877(4) 0.126(3) Uani 1 1 d . . . . .
H2 H 0.2050 -0.0056 0.5929 0.188 Uiso 1 1 d R . . . .
N1 N 0.3365(7) 0.0139(6) 0.5048(4) 0.108(3) Uani 1 1 d . . . . .
H1A H 0.2841 0.0163 0.5127 0.130 Uiso 1 1 calc R . . . .
H1B H 0.3514 0.0622 0.4928 0.130 Uiso 1 1 calc R . . . .
C1 C 0.3842(10) 0.1360(9) 0.6500(6) 0.123(5) Uani 1 1 d . . . . .
C2 C 0.4063(10) 0.0963(9) 0.6089(5) 0.115(4) Uani 1 1 d . . . . .
C3 C 0.3587(8) 0.0457(8) 0.5891(5) 0.105(4) Uani 1 1 d . . . . .
C4 C 0.2909(10) 0.0345(9) 0.6080(6) 0.115(4) Uani 1 1 d . . . . .
C5 C 0.2680(9) 0.0743(11) 0.6498(7) 0.133(5) Uani 1 1 d . . . . .
C6 C 0.3163(10) 0.1277(10) 0.6683(5) 0.128(5) Uani 1 1 d . . . . .
H6 H 0.3008 0.1581 0.6938 0.154 Uiso 1 1 calc R . . . .
C7 C 0.1933(10) 0.0649(11) 0.6729(5) 0.140(6) Uani 1 1 d . . . . .
H7 H 0.1775 0.0142 0.6654 0.168 Uiso 1 1 calc R . . . .
C8 C 0.1952(13) 0.0711(15) 0.7296(6) 0.182(9) Uani 1 1 d . . . . .
H8A H 0.2158 0.1188 0.7386 0.218 Uiso 1 1 calc R . . . .
H8B H 0.1448 0.0691 0.7419 0.218 Uiso 1 1 calc R . . . .
C9 C 0.2379(19) 0.0137(16) 0.7528(10) 0.247(15) Uani 1 1 d . . . . .
H9A H 0.2371 0.0207 0.7876 0.370 Uiso 1 1 calc R . . . .
H9B H 0.2881 0.0158 0.7413 0.370 Uiso 1 1 calc R . . . .
H9C H 0.2170 -0.0338 0.7449 0.370 Uiso 1 1 calc R . . . .
C10 C 0.3791(9) -0.0035(8) 0.5500(6) 0.115(4) Uani 1 1 d . . . . .
C11 C 0.3477(7) -0.0411(8) 0.4660(5) 0.107(4) Uani 1 1 d . . . . .
H11 H 0.4008 -0.0513 0.4629 0.128 Uiso 1 1 calc R . . . .
C12 C 0.3110(8) -0.1070(8) 0.4781(6) 0.120(4) Uani 1 1 d . . . . .
H12A H 0.2589 -0.0970 0.4839 0.144 Uiso 1 1 calc R . . . .
H12B H 0.3320 -0.1276 0.5078 0.144 Uiso 1 1 calc R . . . .
C13 C 0.3189(12) -0.1617(11) 0.4371(7) 0.160(7) Uani 1 1 d . . . . .
H13A H 0.2912 -0.2062 0.4449 0.192 Uiso 1 1 calc R . . . .
H13B H 0.3707 -0.1754 0.4337 0.192 Uiso 1 1 calc R . . . .
C14 C 0.2906(12) -0.1298(12) 0.3876(9) 0.165(7) Uani 1 1 d . U . . .
H14A H 0.3004 -0.1653 0.3617 0.199 Uiso 1 1 calc R . . . .
H14B H 0.2374 -0.1225 0.3895 0.199 Uiso 1 1 calc R . . . .
C15 C 0.3250(13) -0.0620(13) 0.3760(7) 0.160(7) Uani 1 1 d . U . . .
H15A H 0.3016 -0.0411 0.3471 0.191 Uiso 1 1 calc R . . . .
H15B H 0.3767 -0.0708 0.3684 0.191 Uiso 1 1 calc R . . . .
C16 C 0.3196(9) -0.0068(9) 0.4178(5) 0.127(5) Uani 1 1 d . . . . .
H16A H 0.2685 0.0086 0.4217 0.153 Uiso 1 1 calc R . . . .
H16B H 0.3488 0.0367 0.4101 0.153 Uiso 1 1 calc R . . . .
I1 I 0.49501(7) -0.10116(6) 0.63303(3) 0.1284(6) Uani 1 1 d . . . . .
F18 F 0.5543(8) 0.0196(8) 0.7050(4) 0.188(4) Uani 1 1 d . . . . .
F19 F 0.3767(9) -0.1609(8) 0.7046(4) 0.210(5) Uani 1 1 d . . . . .
C17 C 0.4637(12) -0.0725(12) 0.7026(6) 0.152(4) Uani 1 1 d . . . . .
C18 C 0.4996(12) -0.0192(12) 0.7265(5) 0.152(5) Uani 1 1 d . . . . .
C19 C 0.4117(13) -0.1095(12) 0.7270(6) 0.165(5) Uani 1 1 d . . . . .
Cl1 Cl 0.2500 0.2500 0.5810(4) 0.124(4) Uani 0.5 4 d S T P C 3
Cl2 Cl 0.3221(6) 0.2174(6) 0.4971(4) 0.096(3) Uani 0.25 1 d . . . C 3
C20 C 0.2500 0.2500 0.5276(17) 0.106(5) Uani 0.5 4 d S T P C 3
Cl3 Cl 0.3231(19) 0.208(2) 0.3567(13) 0.110(10) Uani 0.09 1 d . U . D 1
Cl4 Cl 0.282(2) 0.172(2) 0.3290(16) 0.123(12) Uani 0.09 1 d . U . D 2
C21 C 0.2500 0.2500 0.361(3) 0.073(17) Uani 0.24 4 d S TU P . .
H21 H 0.2500 0.2500 0.3943 0.109 Uiso 0.24 4 d RS T P 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
O1 H1 0.85(2) . ?
O1 C2 1.345(19) . ?
O2 H2 0.8400 . ?
O2 C4 1.330(18) . ?
N1 H1A 0.9900 . ?
N1 H1B 0.9900 . ?
N1 C10 1.521(17) . ?
N1 C11 1.496(18) . ?
C1 C2 1.42(2) . ?
C1 C6 1.36(2) . ?
C1 C7 1.55(2) 8 ?
C2 C3 1.39(2) . ?
C3 C4 1.37(2) . ?
C3 C10 1.47(2) . ?
C4 C5 1.44(2) . ?
C5 C6 1.42(2) . ?
C5 C7 1.53(2) . ?
C6 H6 0.9500 . ?
C7 C1 1.55(2) 7 ?
C7 H7 1.0000 . ?
C7 C8 1.59(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.47(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C11 H11 1.0000 . ?
C11 C12 1.429(18) . ?
C11 C16 1.57(2) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.53(2) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.59(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.44(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.55(2) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
I1 C17 2.093(18) . ?
F18 C18 1.37(2) . ?
F19 C19 1.30(2) . ?
C17 C18 1.36(2) . ?
C17 C19 1.36(2) . ?
C18 C18 1.40(3) 6_546 ?
C19 C19 1.40(4) 6_546 ?
Cl1 C20 1.49(5) . ?
Cl2 Cl2 2.062(14) 8 ?
Cl2 Cl2 2.062(14) 7 ?
Cl2 C20 1.69(3) . ?
C20 Cl2 1.69(3) 2 ?
C20 Cl2 1.69(3) 7 ?
C20 Cl2 1.69(3) 8 ?
Cl3 Cl3 2.20(5) 8 ?
Cl3 Cl3 2.20(5) 7 ?
Cl3 C21 1.56(3) . ?
Cl4 Cl4 2.20(5) 7 ?
Cl4 Cl4 2.20(5) 8 ?
Cl4 C21 1.79(5) . ?
C21 Cl3 1.56(3) 7 ?
C21 Cl3 1.56(3) 8 ?
C21 Cl3 1.56(3) 2 ?
C21 Cl4 1.79(5) 7 ?
C21 Cl4 1.79(5) 8 ?
C21 Cl4 1.79(5) 2 ?
C21 H21 0.9356 . ?

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 O1 H1 130(10) . . ?
C4 O2 H2 109.7 . . ?
H1A N1 H1B 107.8 . . ?
C10 N1 H1A 109.1 . . ?
C10 N1 H1B 109.1 . . ?
C11 N1 H1A 109.1 . . ?
C11 N1 H1B 109.1 . . ?
C11 N1 C10 112.7(11) . . ?
C2 C1 C7 120.7(17) . 8 ?
C6 C1 C2 120.6(16) . . ?
C6 C1 C7 118.6(18) . 8 ?
O1 C2 C1 118.4(15) . . ?
O1 C2 C3 122.7(15) . . ?
C3 C2 C1 118.9(16) . . ?
C2 C3 C10 123.1(14) . . ?
C4 C3 C2 121.5(16) . . ?
C4 C3 C10 115.2(14) . . ?
O2 C4 C3 118.1(16) . . ?
O2 C4 C5 121.8(16) . . ?
C3 C4 C5 120.1(16) . . ?
C4 C5 C7 123.1(18) . . ?
C6 C5 C4 117.5(16) . . ?
C6 C5 C7 119.3(19) . . ?
C1 C6 C5 121.2(17) . . ?
C1 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
C1 C7 H7 106.3 7 . ?
C1 C7 C8 112.5(16) 7 . ?
C5 C7 C1 111.8(11) . 7 ?
C5 C7 H7 106.3 . . ?
C5 C7 C8 113.1(16) . . ?
C8 C7 H7 106.3 . . ?
C7 C8 H8A 108.9 . . ?
C7 C8 H8B 108.9 . . ?
H8A C8 H8B 107.7 . . ?
C9 C8 C7 114(2) . . ?
C9 C8 H8A 108.9 . . ?
C9 C8 H8B 108.9 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C3 C10 N1 110.8(12) . . ?
N1 C11 H11 108.9 . . ?
N1 C11 C16 107.5(11) . . ?
C12 C11 N1 109.9(12) . . ?
C12 C11 H11 108.9 . . ?
C12 C11 C16 112.8(13) . . ?
C16 C11 H11 108.9 . . ?
C11 C12 H12A 109.7 . . ?
C11 C12 H12B 109.7 . . ?
C11 C12 C13 109.7(14) . . ?
H12A C12 H12B 108.2 . . ?
C13 C12 H12A 109.7 . . ?
C13 C12 H12B 109.7 . . ?
C12 C13 H13A 109.2 . . ?
C12 C13 H13B 109.2 . . ?
C12 C13 C14 112.0(17) . . ?
H13A C13 H13B 107.9 . . ?
C14 C13 H13A 109.2 . . ?
C14 C13 H13B 109.2 . . ?
C13 C14 H14A 109.2 . . ?
C13 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
C15 C14 C13 111.9(17) . . ?
C15 C14 H14A 109.2 . . ?
C15 C14 H14B 109.2 . . ?
C14 C15 H15A 109.3 . . ?
C14 C15 H15B 109.3 . . ?
C14 C15 C16 111.8(18) . . ?
H15A C15 H15B 107.9 . . ?
C16 C15 H15A 109.3 . . ?
C16 C15 H15B 109.3 . . ?
C11 C16 H16A 109.4 . . ?
C11 C16 H16B 109.4 . . ?
C15 C16 C11 111.1(14) . . ?
C15 C16 H16A 109.4 . . ?
C15 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
C18 C17 I1 120.3(14) . . ?
C18 C17 C19 117.4(18) . . ?
C19 C17 I1 122.1(14) . . ?
F18 C18 C18 117.5(9) . 6_546 ?
C17 C18 F18 121.2(16) . . ?
C17 C18 C18 121.3(11) . 6_546 ?
F19 C19 C17 118.3(17) . . ?
F19 C19 C19 120.3(11) . 6_546 ?
C17 C19 C19 121.1(12) . 6_546 ?
Cl2 Cl2 Cl2 89.998(1) 7 8 ?
C20 Cl2 Cl2 52.4(7) . 7 ?
C20 Cl2 Cl2 52.4(7) . 8 ?
Cl1 C20 Cl2 120.3(15) . 2 ?
Cl1 C20 Cl2 120.3(15) . 8 ?
Cl1 C20 Cl2 120.3(15) . . ?
Cl1 C20 Cl2 120.3(15) . 7 ?
Cl2 C20 Cl2 119(3) 7 8 ?
Cl2 C20 Cl2 75.2(14) 2 8 ?
Cl2 C20 Cl2 75.2(14) 7 . ?
Cl2 C20 Cl2 75.2(14) 8 . ?
Cl2 C20 Cl2 119(3) 2 . ?
Cl2 C20 Cl2 75.2(14) 7 2 ?
Cl3 Cl3 Cl3 90.000(3) 8 7 ?
C21 Cl3 Cl3 45.2(2) . 8 ?
C21 Cl3 Cl3 45.2(2) . 7 ?
Cl4 Cl4 Cl4 89.999(6) 8 7 ?
C21 Cl4 Cl4 52.1(12) . 7 ?
C21 Cl4 Cl4 52.1(12) . 8 ?
Cl3 C21 Cl3 89.7(5) . 8 ?
Cl3 C21 Cl3 172(6) . 2 ?
Cl3 C21 Cl3 89.7(5) 8 2 ?
Cl3 C21 Cl3 89.7(5) 7 2 ?
Cl3 C21 Cl3 172(6) 7 8 ?
Cl3 C21 Cl3 89.7(5) . 7 ?
Cl3 C21 H21 94.2 7 . ?
Cl3 C21 H21 94.2 2 . ?
Cl3 C21 H21 94.2 . . ?
Cl3 C21 H21 94.2 8 . ?
Cl4 C21 Cl4 121(5) 7 8 ?
Cl4 C21 Cl4 76(2) 8 . ?
Cl4 C21 Cl4 121(5) 2 . ?
Cl4 C21 Cl4 76(2) 7 2 ?
Cl4 C21 Cl4 76(2) 8 2 ?
Cl4 C21 Cl4 76(2) 7 . ?
Cl4 C21 H21 119.7 7 . ?
Cl4 C21 H21 119.7 . . ?
Cl4 C21 H21 119.7 8 . ?
Cl4 C21 H21 119.7 2 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2 O1 0.84 1.88 2.702(16) 166.9 7
N1 H1A Br1 0.99 2.99 3.876(12) 150.1 .
N1 H1A Br1B 0.99 2.69 3.541(13) 144.7 .

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C2 C3 C4 -179.9(12) . . . . ?
O1 C2 C3 C10 6(2) . . . . ?
O2 C4 C5 C6 -178.7(12) . . . . ?
O2 C4 C5 C7 -2(2) . . . . ?
N1 C11 C12 C13 176.8(13) . . . . ?
N1 C11 C16 C15 -176.7(14) . . . . ?
C1 C2 C3 C4 1(2) . . . . ?
C1 C2 C3 C10 -173.2(12) . . . . ?
C1 C7 C8 C9 168(2) 7 . . . ?
C2 C1 C6 C5 6(2) . . . . ?
C2 C3 C4 O2 -179.1(11) . . . . ?
C2 C3 C4 C5 -1.3(19) . . . . ?
C2 C3 C10 N1 -114.0(14) . . . . ?
C3 C4 C5 C6 3.7(19) . . . . ?
C3 C4 C5 C7 179.8(13) . . . . ?
C4 C3 C10 N1 71.3(15) . . . . ?
C4 C5 C6 C1 -6(2) . . . . ?
C4 C5 C7 C1 -88(2) . . . 7 ?
C4 C5 C7 C8 143.9(16) . . . . ?
C5 C7 C8 C9 -64(3) . . . . ?
C6 C1 C2 O1 177.4(13) . . . . ?
C6 C1 C2 C3 -4(2) . . . . ?
C6 C5 C7 C1 88.3(18) . . . 7 ?
C6 C5 C7 C8 -40(2) . . . . ?
C7 C1 C2 O1 2(2) 8 . . . ?
C7 C1 C2 C3 -179.4(12) 8 . . . ?
C7 C1 C6 C5 -177.9(13) 8 . . . ?
C7 C5 C6 C1 177.5(13) . . . . ?
C10 N1 C11 C12 72.5(15) . . . . ?
C10 N1 C11 C16 -164.5(12) . . . . ?
C10 C3 C4 O2 -4.3(17) . . . . ?
C10 C3 C4 C5 173.5(11) . . . . ?
C11 N1 C10 C3 -172.0(12) . . . . ?
C11 C12 C13 C14 -55.8(19) . . . . ?
C12 C11 C16 C15 -55.4(19) . . . . ?
C12 C13 C14 C15 54(2) . . . . ?
C13 C14 C15 C16 -52(3) . . . . ?
C14 C15 C16 C11 52(2) . . . . ?
C16 C11 C12 C13 56.9(17) . . . . ?
I1 C17 C18 F18 4(3) . . . . ?
I1 C17 C18 C18 -178(2) . . . 6_546 ?
I1 C17 C19 F19 -5(3) . . . . ?
I1 C17 C19 C19 -179(3) . . . 6_546 ?
C18 C17 C19 F19 -180(2) . . . . ?
C18 C17 C19 C19 7(5) . . . 6_546 ?
C19 C17 C18 F18 178(2) . . . . ?
C19 C17 C18 C18 -4(5) . . . 6_546 ?
Cl2 Cl2 C20 Cl1 116.8(10) 7 . . . ?
Cl2 Cl2 C20 Cl1 -116.8(10) 8 . . . ?
Cl2 Cl2 C20 Cl2 -126(2) 7 . . 8 ?
Cl2 Cl2 C20 Cl2 -63.2(10) 7 . . 2 ?
Cl2 Cl2 C20 Cl2 126(2) 8 . . 7 ?
Cl2 Cl2 C20 Cl2 63.2(10) 8 . . 2 ?
Cl3 Cl3 C21 Cl3 172(6) 8 . . 7 ?
Cl3 Cl3 C21 Cl3 -172(6) 7 . . 8 ?
Cl3 Cl3 C21 Cl4 -36(4) 7 . . . ?
Cl3 Cl3 C21 Cl4 29(3) 8 . . 8 ?
Cl3 Cl3 C21 Cl4 -130(8) 7 . . 2 ?
Cl3 Cl3 C21 Cl4 138(7) 8 . . 7 ?
Cl3 Cl3 C21 Cl4 -142(4) 7 . . 8 ?
Cl3 Cl3 C21 Cl4 136(4) 8 . . . ?
Cl3 Cl3 C21 Cl4 -33.7(19) 7 . . 7 ?
Cl3 Cl3 C21 Cl4 41(2) 8 . . 2 ?
Cl4 Cl4 C21 Cl3 -54(3) 8 . . . ?
Cl4 Cl4 C21 Cl3 117(7) 8 . . 2 ?
Cl4 Cl4 C21 Cl3 178(4) 7 . . . ?
Cl4 Cl4 C21 Cl3 -129(6) 7 . . 8 ?
Cl4 Cl4 C21 Cl3 -1(3) 8 . . 8 ?
Cl4 Cl4 C21 Cl3 -10(4) 7 . . 2 ?
Cl4 Cl4 C21 Cl3 171(4) 8 . . 7 ?
Cl4 Cl4 C21 Cl3 43(3) 7 . . 7 ?
Cl4 Cl4 C21 Cl4 127(4) 8 . . 7 ?
Cl4 Cl4 C21 Cl4 -63.7(18) 7 . . 2 ?
Cl4 Cl4 C21 Cl4 -127(4) 7 . . 8 ?
Cl4 Cl4 C21 Cl4 63.7(18) 8 . . 2 ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
7 9 0 0.0359 7.0000 9.0000 0.0000 0.4007 -0.0221 -0.8658
-7 -9 0 0.0433 -7.0000 -9.0000 -0.0000 -0.4007 0.0221 0.8658
2 -2 -18 0.0969 2.0000 -2.0000 -18.0000 -0.9353 0.0814 -0.4024
-2 2 18 0.0909 -2.0000 2.0000 18.0000 0.9353 -0.0814 0.4024
10 -6 3 0.0162 10.0000 -6.0000 3.0000 -0.0866 -0.9746 -0.1453
-10 6 -3 0.0166 -10.0000 6.0000 -3.0000 0.0866 0.9746 0.1453
-4 -9 -11 0.0646 -4.0000 -9.0000 -11.0000 -0.9157 0.0159 0.4578

_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_EtOH_C2Cl2@3
_database_code_depnum_ccdc_archive 'CCDC 1038851'
_audit_update_record             
;
2014-12-11 deposited with the CCDC.
2015-01-26 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT911_EtOH_C2Cl2@3        
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L=  0.600
RESPONSE: Due to software error the data was accidentially collected as
tetragonal. Thus 23 % of the reflections are missing but have no impact
on the overall structure 
;
# end Validation Reply Form


_audit_creation_date             2013-11-01
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '4(Br), C2 H4 Cl2, C68 H104 N4 O8, C2 H6 O'
_chemical_formula_sum            'C72 H114 Br4 Cl2 N4 O9'
_chemical_formula_weight         1570.21
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C60 H60 O8 N4 Cl4'
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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y, z+1/2'
3 'x+1/2, -y+1/2, -z'
4 '-x, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x-1/2, y, -z-1/2'
7 '-x-1/2, y-1/2, z'
8 'x, -y-1/2, z-1/2'

_cell_length_a                   23.3371(3)
_cell_length_b                   23.5232(2)
_cell_length_c                   27.0473(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     14848.0(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    22210
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      76.1270
_cell_measurement_theta_min      3.1350
_exptl_absorpt_coefficient_mu    3.753
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.741
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6560
_exptl_crystal_size_max          0.1791
_exptl_crystal_size_mid          0.1233
_exptl_crystal_size_min          0.1089
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            55172
_diffrn_reflns_theta_full        68.00
_diffrn_reflns_theta_max         76.75
_diffrn_reflns_theta_min         3.13
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector_area_resol_mean 10.3953
_diffrn_measured_fraction_theta_full 0.9986
_diffrn_measured_fraction_theta_max 0.9760
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -49.00   20.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676   37.0000   60.0000 69

#__ type_ start__ end____ width___ exp.time_
  2 omega  -47.00   20.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676   37.0000  120.0000 67

#__ type_ start__ end____ width___ exp.time_
  3 omega   53.00   96.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       41.3676 -125.0000   90.0000 43

#__ type_ start__ end____ width___ exp.time_
  4 omega   28.00   63.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       41.3676 -125.0000 -120.0000 35

#__ type_ start__ end____ width___ exp.time_
  5 omega   27.00   55.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       41.3676 -125.0000 -180.0000 28

#__ type_ start__ end____ width___ exp.time_
  6 omega   39.00   73.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   60.0000 34

#__ type_ start__ end____ width___ exp.time_
  7 omega   43.00   79.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000 -120.0000 36

#__ type_ start__ end____ width___ exp.time_
  8 omega   41.00   75.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   90.0000 34

#__ type_ start__ end____ width___ exp.time_
  9 omega   45.00   71.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -30.0000 26

#__ type_ start__ end____ width___ exp.time_
 10 omega  137.00  178.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000   90.0000 41

#__ type_ start__ end____ width___ exp.time_
 11 omega   44.00   84.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  120.0000 40

#__ type_ start__ end____ width___ exp.time_
 12 omega   48.00   88.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  -60.0000 40

#__ type_ start__ end____ width___ exp.time_
 13 omega  108.00  165.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000 -150.0000 57

#__ type_ start__ end____ width___ exp.time_
 14 omega   31.00  163.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -15.0000 -150.0000 132
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0068254000
_diffrn_orient_matrix_UB_12      -0.0531740000
_diffrn_orient_matrix_UB_13      -0.0327604000
_diffrn_orient_matrix_UB_21      0.0131785000
_diffrn_orient_matrix_UB_22      0.0359757000
_diffrn_orient_matrix_UB_23      -0.0462174000
_diffrn_orient_matrix_UB_31      0.0642903000
_diffrn_orient_matrix_UB_32      -0.0130167000
_diffrn_orient_matrix_UB_33      0.0060655000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                9727
_reflns_number_total             12047
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         2.038
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     864
_refine_ls_number_reflns         12047
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0778
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1400P)²+21.2397P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2208
_refine_ls_wR_factor_ref         0.2411
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C71-C72
 1.5 with sigma of 0.02
 C71-Cl1A = C72-Cl2A = C71-Cl1B = C72-Cl2B
 1.7 with sigma of 0.02
 H4-H5
 2.1 with sigma of 0.02
 C71-Cl1A \\sim C71-Cl1B \\sim C72-Cl2A \\sim C72-Cl2B
 with sigma of 0.01
 C16-C17A \\sim C16-C17B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C17A) \\sim Ueq, Uanis(C17B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C16) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(Cl2A) \\sim Ueq, Uanis(Cl1B) \\sim Ueq, Uanis(Cl2B) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
4. Others
 Sof(Cl1B)=1-FVAR(1)
 Sof(Cl1A)=FVAR(1)
 Sof(Cl2B)=Sof(H72C)=Sof(H72D)=1-FVAR(2)
 Sof(Cl2A)=Sof(H72A)=Sof(H72B)=FVAR(2)
 Sof(H16C)=Sof(H16D)=Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(3)
 Sof(H16A)=Sof(H16B)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(3)
5.a Riding coordinates:
 O8(H8)
5.b Ternary CH refined with riding coordinates:
 C8(H8A), C14(H14), C25(H25), C31(H31), C42(H42), C48(H48), C59(H59), C65(H65)
5.c Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C72(H72A,H72B), C72(H72C,H72D), N1(H1A,H1B), N2(H2A,H2B),
 N3(H3A,H3B), N4(H4A,H4B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,
 H11B), C12(H12A,H12B), C13(H13A,H13B), C15(H15A,H15B), C16(H16A,H16B),
 C16(H16C,H16D), C24(H24A,H24B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B),
  C29(H29A,H29B), C30(H30A,H30B), C32(H32A,H32B), C33(H33A,H33B), C41(H41A,
 H41B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B),
 C47(H47A,H47B), C49(H49A,H49B), C50(H50A,H50B), C58(H58A,H58B), C60(H60A,H60B),
  C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C66(H66A,
 H66B), C67(H67A,H67B), C70(H70A,H70B)
5.d Aromatic/amide H refined with riding coordinates:
 C4(H4C), C23(H23), C40(H40), C57(H57)
5.e Idealised Me refined as rotating group:
 C17A(H17A,H17B,H17C), C17B(H17D,H17E,H17F), C34(H34A,H34B,H34C), C51(H51A,
 H51B,H51C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C)
5.f Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O3(H3), O4(H4), O5(H5), O6(H6), O7(H7), O9(H9)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br -0.02864(4) 0.26684(3) 0.66340(3) 0.0611(2) Uani 1 1 d . . .
Br2 Br 0.16498(3) 0.05522(3) 0.67805(2) 0.0541(2) Uani 1 1 d . . .
Br3 Br 0.31142(3) 0.24310(2) 0.66177(2) 0.0509(2) Uani 1 1 d . . .
Br4 Br 0.13297(4) 0.40404(4) 0.66753(2) 0.0640(3) Uani 1 1 d . . .
Cl1A Cl 0.1318(3) 0.2384(2) 0.4964(2) 0.145(3) Uani 0.711(11) 1 d PD A 1
Cl1B Cl 0.0953(5) 0.2669(5) 0.5260(5) 0.111(4) Uani 0.289(11) 1 d PDU A 2
Cl2A Cl 0.2498(5) 0.1774(5) 0.5257(3) 0.169(4) Uani 0.522(10) 1 d PDU A 1
Cl2B Cl 0.1908(4) 0.1546(4) 0.5282(3) 0.145(4) Uani 0.478(10) 1 d PDU A 2
C71 C 0.1650(6) 0.2605(8) 0.5493(6) 0.204(9) Uani 1 1 d DU . .
H71A H 0.1903 0.2933 0.5423 0.245 Uiso 1 1 calc R A 1
H71B H 0.1363 0.2720 0.5743 0.245 Uiso 1 1 calc R A 1
C72 C 0.2005(6) 0.2093(6) 0.5680(5) 0.147(6) Uani 1 1 d DU A .
H72A H 0.1734 0.1796 0.5791 0.176 Uiso 0.522(10) 1 calc PR A 1
H72B H 0.2223 0.2219 0.5974 0.176 Uiso 0.522(10) 1 calc PR A 1
H72C H 0.1877 0.1983 0.6016 0.176 Uiso 0.478(10) 1 calc PR A 2
H72D H 0.2416 0.2196 0.5697 0.176 Uiso 0.478(10) 1 calc PR A 2
O1 O 0.08819(19) 0.48019(15) 0.78340(15) 0.0475(10) Uani 1 1 d . . .
H1 H 0.1230 0.4759 0.7766 0.071 Uiso 1 1 calc R . .
O2 O -0.06205(18) 0.34802(16) 0.78186(18) 0.0526(10) Uani 1 1 d . . .
H2 H -0.0672 0.3128 0.7846 0.079 Uiso 1 1 calc R . .
O3 O -0.05274(18) 0.23365(15) 0.77245(17) 0.0495(10) Uani 1 1 d . . .
H3 H -0.0441 0.2394 0.7427 0.074 Uiso 1 1 calc R . .
O4 O 0.07014(18) 0.07344(14) 0.77743(15) 0.0438(9) Uani 1 1 d . . .
H4 H 0.1050 0.0673 0.7828 0.066 Uiso 1 1 calc RD . .
O5 O 0.18435(18) 0.04907(13) 0.79210(14) 0.0433(9) Uani 1 1 d . . .
H5 H 0.1880 0.0458 0.7613 0.065 Uiso 1 1 calc RD . .
O6 O 0.34367(17) 0.17502(14) 0.78516(14) 0.0418(9) Uani 1 1 d . . .
H6 H 0.3491 0.2103 0.7845 0.063 Uiso 1 1 calc R . .
O7 O 0.33296(17) 0.29020(13) 0.76976(13) 0.0390(8) Uani 1 1 d . . .
H7 H 0.3267 0.2854 0.7395 0.058 Uiso 1 1 calc R . .
O8 O 0.19802(19) 0.44463(14) 0.76407(14) 0.0469(10) Uani 1 1 d . . .
H8 H 0.1831 0.4332 0.7376 0.070 Uiso 1 1 d R . .
N1 N -0.0078(2) 0.40931(18) 0.69502(17) 0.0458(11) Uani 1 1 d . . .
H1A H -0.0174 0.3720 0.7008 0.055 Uiso 1 1 calc R . .
H1B H 0.0302 0.4103 0.6860 0.055 Uiso 1 1 calc R . .
N2 N 0.0313(2) 0.13170(18) 0.68571(17) 0.0449(11) Uani 1 1 d . . .
H2A H 0.0620 0.1089 0.6934 0.054 Uiso 1 1 calc R . .
H2B H 0.0445 0.1685 0.6841 0.054 Uiso 1 1 calc R . .
N3 N 0.2931(2) 0.10481(17) 0.69990(15) 0.0397(10) Uani 1 1 d . . .
H3A H 0.3044 0.1422 0.7014 0.048 Uiso 1 1 calc R . .
H3B H 0.2556 0.1039 0.6893 0.048 Uiso 1 1 calc R . .
N4 N 0.2716(2) 0.37498(18) 0.67283(16) 0.0428(11) Uani 1 1 d . . .
H4A H 0.2323 0.3780 0.6743 0.051 Uiso 1 1 calc R . .
H4B H 0.2804 0.3373 0.6678 0.051 Uiso 1 1 calc R . .
C1 C 0.0141(3) 0.4119(2) 0.78412(19) 0.0407(12) Uani 1 1 d . . .
C2 C -0.0105(2) 0.3626(2) 0.80314(19) 0.0391(12) Uani 1 1 d . . .
C3 C 0.0154(2) 0.33113(18) 0.84058(17) 0.0355(11) Uani 1 1 d . . .
C4 C 0.0685(2) 0.35042(18) 0.85708(16) 0.0348(11) Uani 1 1 d . . .
H4C H 0.0877 0.3290 0.8818 0.042 Uiso 1 1 calc R . .
C5 C 0.0952(2) 0.39935(18) 0.83938(16) 0.0322(11) Uani 1 1 d . . .
C6 C 0.0665(2) 0.43008(18) 0.80245(17) 0.0374(11) Uani 1 1 d . . .
C7 C -0.0153(3) 0.4425(2) 0.7419(2) 0.0483(14) Uani 1 1 d . . .
H7A H -0.0567 0.4467 0.7493 0.058 Uiso 1 1 calc R . .
H7B H 0.0013 0.4810 0.7379 0.058 Uiso 1 1 calc R . .
C8 C -0.0438(3) 0.4317(2) 0.6527(2) 0.0497(15) Uani 1 1 d . . .
H8A H -0.0408 0.4741 0.6522 0.060 Uiso 1 1 calc R . .
C9 C -0.0185(4) 0.4083(3) 0.6043(2) 0.0626(18) Uani 1 1 d . . .
H9A H -0.0149 0.3664 0.6067 0.075 Uiso 1 1 calc R . .
H9B H 0.0203 0.4243 0.5992 0.075 Uiso 1 1 calc R . .
C10 C -0.0570(4) 0.4238(4) 0.5602(3) 0.081(3) Uani 1 1 d . . .
H10A H -0.0544 0.4652 0.5541 0.097 Uiso 1 1 calc R . .
H10B H -0.0428 0.4041 0.5303 0.097 Uiso 1 1 calc R . .
C11 C -0.1186(4) 0.4081(4) 0.5685(3) 0.080(2) Uani 1 1 d . . .
H11A H -0.1220 0.3661 0.5698 0.096 Uiso 1 1 calc R . .
H11B H -0.1418 0.4217 0.5402 0.096 Uiso 1 1 calc R . .
C12 C -0.1423(3) 0.4337(3) 0.6166(3) 0.0603(17) Uani 1 1 d . . .
H12A H -0.1427 0.4756 0.6142 0.072 Uiso 1 1 calc R . .
H12B H -0.1822 0.4205 0.6219 0.072 Uiso 1 1 calc R . .
C13 C -0.1054(3) 0.4156(2) 0.6600(2) 0.0486(14) Uani 1 1 d . . .
H13A H -0.1199 0.4338 0.6905 0.058 Uiso 1 1 calc R . .
H13B H -0.1083 0.3739 0.6643 0.058 Uiso 1 1 calc R . .
C14 C -0.0127(3) 0.2787(2) 0.8627(2) 0.0433(13) Uani 1 1 d . . .
H14 H -0.0542 0.2802 0.8534 0.052 Uiso 1 1 calc R . .
C15 C -0.0104(3) 0.2795(2) 0.9197(2) 0.0552(17) Uani 1 1 d . B .
H15A H 0.0301 0.2762 0.9304 0.066 Uiso 1 1 calc R . .
H15B H -0.0253 0.3164 0.9317 0.066 Uiso 1 1 calc R . .
C16 C -0.0451(5) 0.2314(3) 0.9429(3) 0.087(3) Uani 1 1 d DU . .
H16A H -0.0864 0.2384 0.9371 0.104 Uiso 0.77(4) 1 calc PR B 1
H16B H -0.0348 0.1951 0.9267 0.104 Uiso 0.77(4) 1 calc PR B 1
H16C H -0.0774 0.2237 0.9201 0.104 Uiso 0.23(4) 1 calc PR B 2
H16D H -0.0203 0.1973 0.9423 0.104 Uiso 0.23(4) 1 calc PR B 2
C17A C -0.0343(11) 0.2268(6) 0.9973(4) 0.107(7) Uani 0.77(4) 1 d PDU B 1
H17A H 0.0039 0.2108 1.0030 0.161 Uiso 0.77(4) 1 calc PR B 1
H17B H -0.0632 0.2019 1.0123 0.161 Uiso 0.77(4) 1 calc PR B 1
H17C H -0.0367 0.2646 1.0124 0.161 Uiso 0.77(4) 1 calc PR B 1
C17B C -0.0695(16) 0.2349(13) 0.9927(8) 0.049(9) Uani 0.23(4) 1 d PDU B 2
H17D H -0.0809 0.2742 0.9996 0.073 Uiso 0.23(4) 1 calc PR B 2
H17E H -0.0408 0.2228 1.0170 0.073 Uiso 0.23(4) 1 calc PR B 2
H17F H -0.1031 0.2101 0.9949 0.073 Uiso 0.23(4) 1 calc PR B 2
C18 C 0.0116(2) 0.22416(19) 0.84030(19) 0.0379(12) Uani 1 1 d . . .
C19 C -0.0094(2) 0.20334(19) 0.7952(2) 0.0401(12) Uani 1 1 d . . .
C20 C 0.0119(3) 0.1532(2) 0.7742(2) 0.0420(12) Uani 1 1 d . . .
C21 C 0.0545(2) 0.12395(17) 0.79900(18) 0.0372(11) Uani 1 1 d . . .
C22 C 0.0790(2) 0.14382(18) 0.84329(17) 0.0362(11) Uani 1 1 d . . .
C23 C 0.0561(2) 0.19407(18) 0.86249(17) 0.0375(12) Uani 1 1 d . . .
H23 H 0.0718 0.2085 0.8924 0.045 Uiso 1 1 calc R . .
C24 C -0.0111(3) 0.1279(2) 0.7267(2) 0.0430(12) Uani 1 1 d . . .
H24A H -0.0211 0.0875 0.7324 0.052 Uiso 1 1 calc R . .
H24B H -0.0465 0.1483 0.7170 0.052 Uiso 1 1 calc R . .
C25 C 0.0097(3) 0.1151(2) 0.6356(2) 0.0525(15) Uani 1 1 d . . .
H25 H -0.0288 0.1330 0.6311 0.063 Uiso 1 1 calc R . .
C26 C 0.0487(3) 0.1374(3) 0.5953(2) 0.0611(17) Uani 1 1 d . . .
H26A H 0.0873 0.1206 0.5994 0.073 Uiso 1 1 calc R . .
H26B H 0.0523 0.1791 0.5986 0.073 Uiso 1 1 calc R . .
C27 C 0.0263(4) 0.1233(3) 0.5436(2) 0.072(2) Uani 1 1 d . . .
H27A H 0.0543 0.1363 0.5185 0.087 Uiso 1 1 calc R . .
H27B H -0.0102 0.1436 0.5378 0.087 Uiso 1 1 calc R . .
C28 C 0.0170(4) 0.0590(3) 0.5387(3) 0.070(2) Uani 1 1 d . . .
H28A H 0.0545 0.0395 0.5396 0.084 Uiso 1 1 calc R . .
H28B H -0.0010 0.0508 0.5063 0.084 Uiso 1 1 calc R . .
C29 C -0.0215(4) 0.0355(3) 0.5803(3) 0.0659(19) Uani 1 1 d . . .
H29A H -0.0240 -0.0064 0.5772 0.079 Uiso 1 1 calc R . .
H29B H -0.0606 0.0512 0.5767 0.079 Uiso 1 1 calc R . .
C30 C 0.0021(3) 0.0509(2) 0.6320(2) 0.0525(15) Uani 1 1 d . . .
H30A H -0.0249 0.0377 0.6578 0.063 Uiso 1 1 calc R . .
H30B H 0.0394 0.0318 0.6373 0.063 Uiso 1 1 calc R . .
C31 C 0.1278(3) 0.11241(18) 0.86736(17) 0.0398(12) Uani 1 1 d . . .
H31 H 0.1226 0.0713 0.8592 0.048 Uiso 1 1 calc R . .
C32 C 0.1303(3) 0.1166(2) 0.92396(18) 0.0502(15) Uani 1 1 d . . .
H32A H 0.1660 0.0983 0.9356 0.060 Uiso 1 1 calc R . .
H32B H 0.1320 0.1573 0.9334 0.060 Uiso 1 1 calc R . .
C33 C 0.0808(3) 0.0898(3) 0.9495(3) 0.0632(18) Uani 1 1 d . . .
H33A H 0.0717 0.0531 0.9334 0.076 Uiso 1 1 calc R . .
H33B H 0.0468 0.1148 0.9466 0.076 Uiso 1 1 calc R . .
C34 C 0.0943(5) 0.0796(6) 1.0047(3) 0.117(4) Uani 1 1 d . . .
H34A H 0.1358 0.0764 1.0092 0.175 Uiso 1 1 calc R . .
H34B H 0.0758 0.0444 1.0156 0.175 Uiso 1 1 calc R . .
H34C H 0.0798 0.1116 1.0243 0.175 Uiso 1 1 calc R . .
C35 C 0.1846(2) 0.13062(19) 0.84446(17) 0.0361(11) Uani 1 1 d . . .
C36 C 0.2113(2) 0.09835(17) 0.80771(17) 0.0365(11) Uani 1 1 d . . .
C37 C 0.2646(2) 0.11412(18) 0.78832(17) 0.0358(11) Uani 1 1 d . . .
C38 C 0.2911(2) 0.16393(18) 0.80502(17) 0.0370(12) Uani 1 1 d . . .
C39 C 0.2649(2) 0.19771(17) 0.84150(17) 0.0341(11) Uani 1 1 d . . .
C40 C 0.2123(2) 0.18039(18) 0.85961(16) 0.0348(11) Uani 1 1 d . . .
H40 H 0.1939 0.2036 0.8836 0.042 Uiso 1 1 calc R . .
C41 C 0.2966(3) 0.07925(18) 0.7505(2) 0.0411(12) Uani 1 1 d . . .
H41A H 0.3373 0.0763 0.7604 0.049 Uiso 1 1 calc R . .
H41B H 0.2804 0.0403 0.7496 0.049 Uiso 1 1 calc R . .
C42 C 0.3304(3) 0.0735(2) 0.66294(19) 0.0444(14) Uani 1 1 d . . .
H42 H 0.3271 0.0318 0.6696 0.053 Uiso 1 1 calc R . .
C43 C 0.3088(3) 0.0848(3) 0.6112(2) 0.0599(17) Uani 1 1 d . . .
H43A H 0.3110 0.1260 0.6039 0.072 Uiso 1 1 calc R . .
H43B H 0.2683 0.0728 0.6084 0.072 Uiso 1 1 calc R . .
C44 C 0.3456(4) 0.0517(3) 0.5743(3) 0.071(2) Uani 1 1 d . . .
H44A H 0.3413 0.0105 0.5805 0.085 Uiso 1 1 calc R . .
H44B H 0.3319 0.0596 0.5403 0.085 Uiso 1 1 calc R . .
C45 C 0.4081(4) 0.0679(3) 0.5784(3) 0.069(2) Uani 1 1 d . . .
H45A H 0.4130 0.1082 0.5689 0.083 Uiso 1 1 calc R . .
H45B H 0.4309 0.0444 0.5553 0.083 Uiso 1 1 calc R . .
C46 C 0.4299(4) 0.0591(3) 0.6310(3) 0.069(2) Uani 1 1 d . . .
H46A H 0.4698 0.0731 0.6334 0.083 Uiso 1 1 calc R . .
H46B H 0.4299 0.0180 0.6388 0.083 Uiso 1 1 calc R . .
C47 C 0.3925(3) 0.0907(3) 0.6689(2) 0.0554(16) Uani 1 1 d . . .
H47A H 0.4056 0.0815 0.7028 0.067 Uiso 1 1 calc R . .
H47B H 0.3963 0.1322 0.6640 0.067 Uiso 1 1 calc R . .
C48 C 0.2937(2) 0.25142(19) 0.86146(17) 0.0334(10) Uani 1 1 d . . .
H48 H 0.3350 0.2495 0.8518 0.040 Uiso 1 1 calc R . .
C49 C 0.2914(3) 0.2536(2) 0.91815(18) 0.0454(14) Uani 1 1 d . . .
H49A H 0.2511 0.2588 0.9287 0.054 Uiso 1 1 calc R . .
H49B H 0.3135 0.2870 0.9297 0.054 Uiso 1 1 calc R . .
C50 C 0.3159(4) 0.1994(5) 0.9432(3) 0.085(3) Uani 1 1 d . . .
H50A H 0.3229 0.2082 0.9784 0.102 Uiso 1 1 calc R . .
H50B H 0.2859 0.1696 0.9420 0.102 Uiso 1 1 calc R . .
C51 C 0.3690(5) 0.1754(5) 0.9223(4) 0.109(4) Uani 1 1 d . . .
H51A H 0.3602 0.1551 0.8916 0.164 Uiso 1 1 calc R . .
H51B H 0.3860 0.1489 0.9462 0.164 Uiso 1 1 calc R . .
H51C H 0.3962 0.2061 0.9154 0.164 Uiso 1 1 calc R . .
C52 C 0.2686(2) 0.30387(17) 0.83708(15) 0.0304(10) Uani 1 1 d . . .
C53 C 0.2884(2) 0.32085(17) 0.79041(16) 0.0326(10) Uani 1 1 d . . .
C54 C 0.2673(2) 0.36878(18) 0.76661(17) 0.0368(11) Uani 1 1 d . . .
C55 C 0.2217(2) 0.39868(17) 0.78905(17) 0.0352(11) Uani 1 1 d . . .
C56 C 0.2009(2) 0.38371(17) 0.83581(16) 0.0317(10) Uani 1 1 d . . .
C57 C 0.2256(2) 0.33662(17) 0.85842(15) 0.0325(10) Uani 1 1 d . . .
H57 H 0.2124 0.3262 0.8904 0.039 Uiso 1 1 calc R . .
C58 C 0.2961(2) 0.39335(18) 0.72110(17) 0.0370(11) Uani 1 1 d . . .
H58A H 0.2939 0.4353 0.7230 0.044 Uiso 1 1 calc R . .
H58B H 0.3371 0.3827 0.7218 0.044 Uiso 1 1 calc R . .
C59 C 0.2931(3) 0.4090(2) 0.62944(19) 0.0488(15) Uani 1 1 d . . .
H59 H 0.2816 0.4496 0.6341 0.059 Uiso 1 1 calc R . .
C60 C 0.2645(4) 0.3866(3) 0.5830(2) 0.0648(19) Uani 1 1 d . . .
H60A H 0.2223 0.3893 0.5865 0.078 Uiso 1 1 calc R . .
H60B H 0.2747 0.3462 0.5782 0.078 Uiso 1 1 calc R . .
C61 C 0.2840(4) 0.4213(4) 0.5383(3) 0.082(3) Uani 1 1 d . . .
H61A H 0.2710 0.4612 0.5419 0.099 Uiso 1 1 calc R . .
H61B H 0.2666 0.4056 0.5079 0.099 Uiso 1 1 calc R . .
C62 C 0.3502(5) 0.4196(4) 0.5340(3) 0.088(3) Uani 1 1 d . . .
H62A H 0.3624 0.3801 0.5269 0.106 Uiso 1 1 calc R . .
H62B H 0.3623 0.4436 0.5058 0.106 Uiso 1 1 calc R . .
C63 C 0.3797(4) 0.4399(3) 0.5801(3) 0.071(2) Uani 1 1 d . . .
H63A H 0.3717 0.4809 0.5850 0.085 Uiso 1 1 calc R . .
H63B H 0.4216 0.4350 0.5765 0.085 Uiso 1 1 calc R . .
C64 C 0.3584(3) 0.4061(3) 0.6255(2) 0.0582(18) Uani 1 1 d . . .
H64A H 0.3706 0.3659 0.6225 0.070 Uiso 1 1 calc R . .
H64B H 0.3758 0.4220 0.6559 0.070 Uiso 1 1 calc R . .
C65 C 0.1532(2) 0.41850(17) 0.85888(17) 0.0358(11) Uani 1 1 d . . .
H65 H 0.1587 0.4584 0.8471 0.043 Uiso 1 1 calc R . .
C66 C 0.1542(3) 0.4208(2) 0.91549(19) 0.0430(13) Uani 1 1 d . . .
H66A H 0.1204 0.4425 0.9270 0.052 Uiso 1 1 calc R . .
H66B H 0.1506 0.3816 0.9284 0.052 Uiso 1 1 calc R . .
C67 C 0.2082(3) 0.4479(3) 0.9374(2) 0.0552(16) Uani 1 1 d . . .
H67A H 0.2030 0.4522 0.9735 0.066 Uiso 1 1 calc R . .
H67B H 0.2410 0.4220 0.9320 0.066 Uiso 1 1 calc R . .
C68 C 0.2225(4) 0.5059(3) 0.9152(3) 0.074(2) Uani 1 1 d . . .
H68A H 0.2343 0.5011 0.8807 0.112 Uiso 1 1 calc R . .
H68B H 0.2538 0.5233 0.9340 0.112 Uiso 1 1 calc R . .
H68C H 0.1886 0.5304 0.9167 0.112 Uiso 1 1 calc R . .
O9 O 0.1053(3) 0.2278(2) 0.6776(2) 0.0713(14) Uani 1 1 d . . .
H9 H 0.0843 0.2568 0.6771 0.107 Uiso 1 1 calc R . .
C69 C 0.1336(3) 0.2669(3) 0.7570(3) 0.0625(18) Uani 1 1 d . . .
H69A H 0.1152 0.3032 0.7490 0.094 Uiso 1 1 calc R . .
H69B H 0.1673 0.2738 0.7778 0.094 Uiso 1 1 calc R . .
H69C H 0.1065 0.2426 0.7747 0.094 Uiso 1 1 calc R . .
C70 C 0.1522(4) 0.2375(4) 0.7093(4) 0.079(3) Uani 1 1 d . . .
H70A H 0.1809 0.2614 0.6921 0.095 Uiso 1 1 calc R . .
H70B H 0.1706 0.2007 0.7174 0.095 Uiso 1 1 calc R . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1A C71 1.708(9) . ?
Cl1B C71 1.749(9) . ?
Cl2A C72 1.788(9) . ?
Cl2B C72 1.693(9) . ?
C71 C72 1.547(17) . ?
O1 C6 1.383(6) . ?
O2 C2 1.376(7) . ?
O3 C19 1.383(7) . ?
O4 C21 1.373(5) . ?
O5 C36 1.384(6) . ?
O6 C38 1.365(7) . ?
O7 C53 1.383(6) . ?
O8 C55 1.390(6) . ?
N1 C7 1.500(7) . ?
N1 C8 1.514(7) . ?
N2 C24 1.489(7) . ?
N2 C25 1.497(7) . ?
N3 C41 1.497(7) . ?
N3 C42 1.516(6) . ?
N4 C58 1.489(7) . ?
N4 C59 1.506(6) . ?
C1 C2 1.395(7) . ?
C1 C6 1.385(8) . ?
C1 C7 1.515(7) . ?
C2 C3 1.392(8) . ?
C3 C4 1.395(8) . ?
C3 C14 1.519(7) . ?
C4 C5 1.393(6) . ?
C5 C6 1.403(7) . ?
C5 C65 1.522(8) . ?
C8 C9 1.537(9) . ?
C8 C13 1.500(10) . ?
C9 C10 1.539(10) . ?
C10 C11 1.500(13) . ?
C11 C12 1.539(12) . ?
C12 C13 1.515(9) . ?
C14 C15 1.541(8) . ?
C14 C18 1.529(6) . ?
C15 C16 1.526(8) . ?
C16 C17A 1.499(16) . ?
C16 C17B 1.47(2) . ?
C18 C19 1.403(8) . ?
C18 C23 1.393(8) . ?
C19 C20 1.399(7) . ?
C20 C21 1.384(8) . ?
C20 C24 1.513(7) . ?
C21 C22 1.407(7) . ?
C22 C23 1.397(7) . ?
C22 C31 1.506(8) . ?
C25 C26 1.515(10) . ?
C25 C30 1.524(8) . ?
C26 C27 1.526(9) . ?
C27 C28 1.535(9) . ?
C28 C29 1.542(11) . ?
C29 C30 1.545(8) . ?
C31 C32 1.535(7) . ?
C31 C35 1.524(8) . ?
C32 C33 1.486(9) . ?
C33 C34 1.544(11) . ?
C35 C36 1.397(7) . ?
C35 C40 1.398(7) . ?
C36 C37 1.400(8) . ?
C37 C38 1.400(7) . ?
C37 C41 1.510(7) . ?
C38 C39 1.406(7) . ?
C39 C40 1.384(8) . ?
C39 C48 1.529(6) . ?
C42 C43 1.511(9) . ?
C42 C47 1.513(9) . ?
C43 C44 1.529(9) . ?
C44 C45 1.512(11) . ?
C45 C46 1.524(12) . ?
C46 C47 1.537(9) . ?
C48 C49 1.535(6) . ?
C48 C52 1.516(6) . ?
C49 C50 1.551(9) . ?
C50 C51 1.475(13) . ?
C52 C53 1.402(6) . ?
C52 C57 1.390(7) . ?
C53 C54 1.389(6) . ?
C54 C55 1.411(7) . ?
C54 C58 1.517(6) . ?
C55 C56 1.400(6) . ?
C56 C57 1.391(6) . ?
C56 C65 1.515(7) . ?
C59 C60 1.516(9) . ?
C59 C64 1.530(11) . ?
C60 C61 1.529(9) . ?
C61 C62 1.550(14) . ?
C62 C63 1.503(12) . ?
C63 C64 1.545(8) . ?
C65 C66 1.532(7) . ?
C66 C67 1.532(8) . ?
C67 C68 1.527(10) . ?
O9 C70 1.409(10) . ?
C69 C70 1.527(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1A C71 Cl1B 45.8(5) . . ?
C72 C71 Cl1A 106.3(10) . . ?
C72 C71 Cl1B 133.0(14) . . ?
Cl2B C72 Cl2A 50.2(5) . . ?
C71 C72 Cl2A 117.5(11) . . ?
C71 C72 Cl2B 108.2(10) . . ?
C7 N1 C8 113.2(4) . . ?
C24 N2 C25 115.7(5) . . ?
C41 N3 C42 112.1(4) . . ?
C58 N4 C59 113.6(4) . . ?
C2 C1 C7 119.1(5) . . ?
C6 C1 C2 119.3(5) . . ?
C6 C1 C7 121.6(5) . . ?
O2 C2 C1 114.4(5) . . ?
O2 C2 C3 123.5(5) . . ?
C3 C2 C1 122.1(5) . . ?
C2 C3 C4 116.5(4) . . ?
C2 C3 C14 122.0(5) . . ?
C4 C3 C14 121.5(5) . . ?
C5 C4 C3 123.8(5) . . ?
C4 C5 C6 117.2(5) . . ?
C4 C5 C65 121.5(4) . . ?
C6 C5 C65 121.3(4) . . ?
O1 C6 C1 116.9(5) . . ?
O1 C6 C5 122.0(5) . . ?
C1 C6 C5 121.1(4) . . ?
N1 C7 C1 109.7(4) . . ?
N1 C8 C9 107.8(5) . . ?
C13 C8 N1 110.2(5) . . ?
C13 C8 C9 112.9(5) . . ?
C8 C9 C10 110.5(7) . . ?
C11 C10 C9 112.7(6) . . ?
C10 C11 C12 112.0(7) . . ?
C13 C12 C11 109.9(6) . . ?
C8 C13 C12 111.9(5) . . ?
C3 C14 C15 111.6(4) . . ?
C3 C14 C18 111.3(4) . . ?
C18 C14 C15 113.2(5) . . ?
C16 C15 C14 112.5(6) . . ?
C17A C16 C15 111.6(9) . . ?
C17B C16 C15 122.9(14) . . ?
C17B C16 C17A 33.4(12) . . ?
C19 C18 C14 120.6(5) . . ?
C23 C18 C14 122.2(5) . . ?
C23 C18 C19 117.2(4) . . ?
O3 C19 C18 117.5(4) . . ?
O3 C19 C20 120.9(5) . . ?
C20 C19 C18 121.6(5) . . ?
C19 C20 C24 123.4(5) . . ?
C21 C20 C19 118.5(5) . . ?
C21 C20 C24 118.1(4) . . ?
O4 C21 C20 114.5(4) . . ?
O4 C21 C22 122.8(5) . . ?
C20 C21 C22 122.7(4) . . ?
C21 C22 C31 120.8(4) . . ?
C23 C22 C21 116.2(5) . . ?
C23 C22 C31 122.9(5) . . ?
C18 C23 C22 123.7(5) . . ?
N2 C24 C20 111.9(4) . . ?
N2 C25 C26 111.0(5) . . ?
N2 C25 C30 110.9(5) . . ?
C26 C25 C30 111.4(5) . . ?
C25 C26 C27 112.3(6) . . ?
C26 C27 C28 110.0(6) . . ?
C27 C28 C29 111.9(6) . . ?
C28 C29 C30 111.7(6) . . ?
C25 C30 C29 109.4(5) . . ?
C22 C31 C32 115.3(5) . . ?
C22 C31 C35 110.1(4) . . ?
C35 C31 C32 110.8(5) . . ?
C33 C32 C31 114.0(6) . . ?
C32 C33 C34 111.0(8) . . ?
C36 C35 C31 121.6(4) . . ?
C36 C35 C40 117.3(5) . . ?
C40 C35 C31 121.2(4) . . ?
O5 C36 C35 118.1(5) . . ?
O5 C36 C37 120.7(4) . . ?
C35 C36 C37 121.2(4) . . ?
C36 C37 C41 123.4(4) . . ?
C38 C37 C36 119.6(4) . . ?
C38 C37 C41 117.1(5) . . ?
O6 C38 C37 115.5(4) . . ?
O6 C38 C39 123.9(5) . . ?
C37 C38 C39 120.5(5) . . ?
C38 C39 C48 121.6(5) . . ?
C40 C39 C38 117.9(4) . . ?
C40 C39 C48 120.5(4) . . ?
C39 C40 C35 123.5(5) . . ?
N3 C41 C37 112.0(4) . . ?
C43 C42 N3 109.6(5) . . ?
C43 C42 C47 111.8(5) . . ?
C47 C42 N3 110.5(4) . . ?
C42 C43 C44 109.2(7) . . ?
C45 C44 C43 111.4(5) . . ?
C44 C45 C46 110.9(6) . . ?
C45 C46 C47 111.5(7) . . ?
C42 C47 C46 110.2(5) . . ?
C39 C48 C49 111.4(4) . . ?
C52 C48 C39 110.5(4) . . ?
C52 C48 C49 113.2(4) . . ?
C48 C49 C50 113.3(5) . . ?
C51 C50 C49 117.2(7) . . ?
C53 C52 C48 119.8(4) . . ?
C57 C52 C48 123.3(4) . . ?
C57 C52 C53 117.0(4) . . ?
O7 C53 C52 117.5(4) . . ?
O7 C53 C54 120.2(4) . . ?
C54 C53 C52 122.1(5) . . ?
C53 C54 C55 118.2(4) . . ?
C53 C54 C58 121.9(5) . . ?
C55 C54 C58 119.5(4) . . ?
O8 C55 C54 118.6(4) . . ?
O8 C55 C56 119.8(4) . . ?
C56 C55 C54 121.7(4) . . ?
C55 C56 C65 119.4(4) . . ?
C57 C56 C55 116.9(5) . . ?
C57 C56 C65 123.6(4) . . ?
C52 C57 C56 124.0(4) . . ?
N4 C58 C54 115.5(4) . . ?
N4 C59 C60 108.3(5) . . ?
N4 C59 C64 111.3(5) . . ?
C60 C59 C64 111.4(5) . . ?
C59 C60 C61 109.8(6) . . ?
C60 C61 C62 110.0(7) . . ?
C63 C62 C61 112.7(7) . . ?
C62 C63 C64 110.4(6) . . ?
C59 C64 C63 110.7(6) . . ?
C5 C65 C66 111.7(4) . . ?
C56 C65 C5 110.5(4) . . ?
C56 C65 C66 114.8(5) . . ?
C67 C66 C65 114.4(5) . . ?
C68 C67 C66 113.6(6) . . ?
O9 C70 C69 111.4(7) . . ?

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
Cl1A C71 C72 Cl2A 53.9(16) . . . . ?
Cl1A C71 C72 Cl2B 0.0(15) . . . . ?
Cl1B C71 C72 Cl2A 97.9(19) . . . . ?
Cl1B C71 C72 Cl2B 44(2) . . . . ?
O2 C2 C3 C4 177.9(4) . . . . ?
O2 C2 C3 C14 -2.6(7) . . . . ?
O3 C19 C20 C21 -178.7(5) . . . . ?
O3 C19 C20 C24 -1.3(8) . . . . ?
O4 C21 C22 C23 -175.9(4) . . . . ?
O4 C21 C22 C31 5.2(7) . . . . ?
O5 C36 C37 C38 -179.5(4) . . . . ?
O5 C36 C37 C41 -0.9(7) . . . . ?
O6 C38 C39 C40 -177.8(4) . . . . ?
O6 C38 C39 C48 1.2(7) . . . . ?
O7 C53 C54 C55 180.0(4) . . . . ?
O7 C53 C54 C58 -7.4(7) . . . . ?
O8 C55 C56 C57 178.8(4) . . . . ?
O8 C55 C56 C65 -0.9(7) . . . . ?
N1 C8 C9 C10 173.6(6) . . . . ?
N1 C8 C13 C12 -176.0(5) . . . . ?
N2 C25 C26 C27 -177.5(5) . . . . ?
N2 C25 C30 C29 178.8(6) . . . . ?
N3 C42 C43 C44 -178.3(5) . . . . ?
N3 C42 C47 C46 -179.6(6) . . . . ?
N4 C59 C60 C61 178.4(6) . . . . ?
N4 C59 C64 C63 178.6(5) . . . . ?
C1 C2 C3 C4 -2.2(7) . . . . ?
C1 C2 C3 C14 177.4(4) . . . . ?
C2 C1 C6 O1 -178.1(4) . . . . ?
C2 C1 C6 C5 0.6(7) . . . . ?
C2 C1 C7 N1 -73.3(7) . . . . ?
C2 C3 C4 C5 2.1(7) . . . . ?
C2 C3 C14 C15 -133.3(5) . . . . ?
C2 C3 C14 C18 99.1(6) . . . . ?
C3 C4 C5 C6 -0.7(7) . . . . ?
C3 C4 C5 C65 179.8(4) . . . . ?
C3 C14 C15 C16 172.5(6) . . . . ?
C3 C14 C18 C19 -83.2(6) . . . . ?
C3 C14 C18 C23 94.8(6) . . . . ?
C4 C3 C14 C15 46.3(7) . . . . ?
C4 C3 C14 C18 -81.3(6) . . . . ?
C4 C5 C6 O1 177.9(4) . . . . ?
C4 C5 C6 C1 -0.7(7) . . . . ?
C4 C5 C65 C56 78.4(5) . . . . ?
C4 C5 C65 C66 -50.7(6) . . . . ?
C5 C65 C66 C67 -171.5(4) . . . . ?
C6 C1 C2 O2 -179.1(4) . . . . ?
C6 C1 C2 C3 0.9(7) . . . . ?
C6 C1 C7 N1 103.2(6) . . . . ?
C6 C5 C65 C56 -101.0(5) . . . . ?
C6 C5 C65 C66 129.8(5) . . . . ?
C7 N1 C8 C9 161.7(5) . . . . ?
C7 N1 C8 C13 -74.7(6) . . . . ?
C7 C1 C2 O2 -2.6(7) . . . . ?
C7 C1 C2 C3 177.4(5) . . . . ?
C7 C1 C6 O1 5.5(7) . . . . ?
C7 C1 C6 C5 -175.8(5) . . . . ?
C8 N1 C7 C1 170.7(5) . . . . ?
C8 C9 C10 C11 -51.2(10) . . . . ?
C9 C8 C13 C12 -55.4(7) . . . . ?
C9 C10 C11 C12 54.4(10) . . . . ?
C10 C11 C12 C13 -56.0(8) . . . . ?
C11 C12 C13 C8 56.2(7) . . . . ?
C13 C8 C9 C10 51.6(7) . . . . ?
C14 C3 C4 C5 -177.5(4) . . . . ?
C14 C15 C16 C17A 170.3(11) . . . . ?
C14 C15 C16 C17B -154.1(18) . . . . ?
C14 C18 C19 O3 -0.6(7) . . . . ?
C14 C18 C19 C20 -179.4(5) . . . . ?
C14 C18 C23 C22 179.4(4) . . . . ?
C15 C14 C18 C19 150.1(5) . . . . ?
C15 C14 C18 C23 -31.9(7) . . . . ?
C18 C14 C15 C16 -61.0(8) . . . . ?
C18 C19 C20 C21 0.0(8) . . . . ?
C18 C19 C20 C24 177.4(5) . . . . ?
C19 C18 C23 C22 -2.5(7) . . . . ?
C19 C20 C21 O4 176.0(4) . . . . ?
C19 C20 C21 C22 -2.8(8) . . . . ?
C19 C20 C24 N2 111.3(6) . . . . ?
C20 C21 C22 C23 2.7(7) . . . . ?
C20 C21 C22 C31 -176.2(5) . . . . ?
C21 C20 C24 N2 -71.3(6) . . . . ?
C21 C22 C23 C18 0.0(7) . . . . ?
C21 C22 C31 C32 -149.2(5) . . . . ?
C21 C22 C31 C35 84.6(5) . . . . ?
C22 C31 C32 C33 64.7(6) . . . . ?
C22 C31 C35 C36 -98.3(5) . . . . ?
C22 C31 C35 C40 81.9(5) . . . . ?
C23 C18 C19 O3 -178.7(4) . . . . ?
C23 C18 C19 C20 2.5(7) . . . . ?
C23 C22 C31 C32 32.0(6) . . . . ?
C23 C22 C31 C35 -94.3(5) . . . . ?
C24 N2 C25 C26 162.3(5) . . . . ?
C24 N2 C25 C30 -73.3(7) . . . . ?
C24 C20 C21 O4 -1.6(7) . . . . ?
C24 C20 C21 C22 179.7(5) . . . . ?
C25 N2 C24 C20 -171.9(4) . . . . ?
C25 C26 C27 C28 -55.4(9) . . . . ?
C26 C25 C30 C29 -57.0(8) . . . . ?
C26 C27 C28 C29 53.5(10) . . . . ?
C27 C28 C29 C30 -54.7(9) . . . . ?
C28 C29 C30 C25 55.4(8) . . . . ?
C30 C25 C26 C27 58.3(8) . . . . ?
C31 C22 C23 C18 178.9(4) . . . . ?
C31 C32 C33 C34 163.1(7) . . . . ?
C31 C35 C36 O5 0.5(7) . . . . ?
C31 C35 C36 C37 -177.3(4) . . . . ?
C31 C35 C40 C39 177.3(4) . . . . ?
C32 C31 C35 C36 132.9(5) . . . . ?
C32 C31 C35 C40 -46.9(6) . . . . ?
C35 C31 C32 C33 -169.4(5) . . . . ?
C35 C36 C37 C38 -1.8(7) . . . . ?
C35 C36 C37 C41 176.8(4) . . . . ?
C36 C35 C40 C39 -2.5(7) . . . . ?
C36 C37 C38 O6 178.1(4) . . . . ?
C36 C37 C38 C39 0.9(7) . . . . ?
C36 C37 C41 N3 104.5(5) . . . . ?
C37 C38 C39 C40 -0.8(7) . . . . ?
C37 C38 C39 C48 178.3(4) . . . . ?
C38 C37 C41 N3 -76.9(6) . . . . ?
C38 C39 C40 C35 1.6(7) . . . . ?
C38 C39 C48 C49 -133.2(5) . . . . ?
C38 C39 C48 C52 100.0(5) . . . . ?
C39 C48 C49 C50 53.5(8) . . . . ?
C39 C48 C52 C53 -82.1(6) . . . . ?
C39 C48 C52 C57 97.0(5) . . . . ?
C40 C35 C36 O5 -179.7(4) . . . . ?
C40 C35 C36 C37 2.5(7) . . . . ?
C40 C39 C48 C49 45.8(6) . . . . ?
C40 C39 C48 C52 -81.0(5) . . . . ?
C41 N3 C42 C43 158.1(5) . . . . ?
C41 N3 C42 C47 -78.4(6) . . . . ?
C41 C37 C38 O6 -0.5(6) . . . . ?
C41 C37 C38 C39 -177.8(4) . . . . ?
C42 N3 C41 C37 173.8(4) . . . . ?
C42 C43 C44 C45 -58.0(8) . . . . ?
C43 C42 C47 C46 -57.3(8) . . . . ?
C43 C44 C45 C46 56.3(9) . . . . ?
C44 C45 C46 C47 -54.2(8) . . . . ?
C45 C46 C47 C42 54.3(8) . . . . ?
C47 C42 C43 C44 58.8(7) . . . . ?
C48 C39 C40 C35 -177.4(4) . . . . ?
C48 C49 C50 C51 42.3(12) . . . . ?
C48 C52 C53 O7 -3.7(6) . . . . ?
C48 C52 C53 C54 -179.5(4) . . . . ?
C48 C52 C57 C56 -177.7(4) . . . . ?
C49 C48 C52 C53 152.1(5) . . . . ?
C49 C48 C52 C57 -28.7(7) . . . . ?
C52 C48 C49 C50 178.8(6) . . . . ?
C52 C53 C54 C55 -4.4(7) . . . . ?
C52 C53 C54 C58 168.2(4) . . . . ?
C53 C52 C57 C56 1.4(7) . . . . ?
C53 C54 C55 O8 -176.2(4) . . . . ?
C53 C54 C55 C56 4.9(7) . . . . ?
C53 C54 C58 N4 96.0(6) . . . . ?
C54 C55 C56 C57 -2.3(7) . . . . ?
C54 C55 C56 C65 178.0(4) . . . . ?
C55 C54 C58 N4 -91.5(5) . . . . ?
C55 C56 C57 C52 -0.9(7) . . . . ?
C55 C56 C65 C5 82.9(5) . . . . ?
C55 C56 C65 C66 -149.7(4) . . . . ?
C56 C65 C66 C67 61.6(6) . . . . ?
C57 C52 C53 O7 177.1(4) . . . . ?
C57 C52 C53 C54 1.3(7) . . . . ?
C57 C56 C65 C5 -96.8(5) . . . . ?
C57 C56 C65 C66 30.6(6) . . . . ?
C58 N4 C59 C60 -179.3(5) . . . . ?
C58 N4 C59 C64 57.9(6) . . . . ?
C58 C54 C55 O8 11.0(7) . . . . ?
C58 C54 C55 C56 -167.9(5) . . . . ?
C59 N4 C58 C54 168.2(4) . . . . ?
C59 C60 C61 C62 56.9(9) . . . . ?
C60 C59 C64 C63 57.6(7) . . . . ?
C60 C61 C62 C63 -56.2(10) . . . . ?
C61 C62 C63 C64 54.6(10) . . . . ?
C62 C63 C64 C59 -54.7(9) . . . . ?
C64 C59 C60 C61 -58.9(8) . . . . ?
C65 C5 C6 O1 -2.6(7) . . . . ?
C65 C5 C6 C1 178.8(4) . . . . ?
C65 C56 C57 C52 178.8(4) . . . . ?
C65 C66 C67 C68 51.2(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 -15 1 0.0453 0.5001 -15.4999 0.9998 0.7880 -0.5972 0.2400
15 3 1 0.0863 15.0001 2.9999 1.0001 -0.2947 0.2594 0.9314
-15 -3 -1 0.0773 -15.0001 -2.9999 -1.0001 0.2947 -0.2594 -0.9314
0 -3 17 0.0281 -0.4999 -2.5001 16.9999 -0.4206 -0.8822 0.1035
1 3 -17 0.0757 1.4999 2.5001 -16.9999 0.4137 0.8954 -0.0392
12 -1 -10 0.0863 12.5000 -1.5000 -9.9999 0.3220 0.5729 0.7625
-2 12 -11 0.0710 -2.0002 12.0000 -10.9998 -0.2641 0.9137 -0.3515
-8 10 -9 0.0858 -8.0002 10.0001 -8.9998 -0.1823 0.6703 -0.6991
9 9 -9 0.0799 8.9999 9.0000 -8.9998 -0.2452 0.8583 0.4069
10 -4 12 0.0676 10.0002 -4.0001 11.9999 -0.2487 -0.5667 0.7678
0 -13 -8 0.0614 0.5000 -13.4999 -8.0002 0.9765 -0.1093 0.1593
8 -12 -5 0.0735 8.0001 -11.9999 -5.0001 0.7473 -0.0952 0.6402
12 4 -10 0.0745 12.0000 4.0000 -9.9999 0.0330 0.7642 0.6588
5 8 -14 0.0695 5.4999 7.5000 -13.9998 0.0223 0.9893 0.1710
-3 9 -14 0.0743 -2.5002 8.5001 -13.9998 0.0237 0.9199 -0.3563
-2 13 -8 0.0586 -1.5001 13.5000 -7.9998 -0.4455 0.8356 -0.3207
0 15 -3 0.0736 -0.0001 14.9999 -2.9998 -0.6993 0.6783 -0.2135
-1 8 15 0.0757 -1.4999 8.4998 15.0001 -0.9331 -0.4072 -0.1161
4 7 15 0.0692 3.5001 7.4998 15.0001 -0.9141 -0.3773 0.2184
13 2 10 0.0777 12.5001 2.4999 10.0000 -0.5459 -0.2075 0.8318
-2 15 1 0.0638 -1.5001 15.4999 1.0002 -0.8467 0.4916 -0.2921
14 5 3 0.0827 13.5001 5.4999 3.0001 -0.4829 0.2371 0.8145




