# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
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# Crystallographic Data Centre (CCDC).
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data_pseudorotaxane-3-4-Cu2ClO4
_database_code_depnum_ccdc_archive 'CCDC 1560765'
_audit_update_record             
;
2017-07-06 deposited with the CCDC.
2017-09-12 downloaded from the CCDC.
;
#==============================================================================
# start Validation Reply Form
_vrf_PLAT029_3.4.CuClO42         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.935 Note  
RESPONSE: The crystals were of low quality and diffracted poorly.
Synchrotron radiation was used, but despite this the diffraction was weak. 
The crystal also suffered radiation damage leading to poor completeness.  
Despite this, there is little doubt that the connectivity is correct and that 
the data supports the general conclusions in the manuscript.
;
_vrf_PLAT430_3.4.CuClO42         
;
PROBLEM: Short Inter D...A Contact  O39    ..  O66     ..       2.82 Ang.  
RESPONSE: This is a relatively close contact between a partially occupied water
molecule and one of the carbonyl oxygen atoms of the macrocycle isophthalamide
group, which presumably accepts a hydrogen bond from the partially occupied water
molecule.
;
_vrf_PLAT990_3.4.CuClO42         
;
PROBLEM: Deprecated RES file style based SQUEEZE job ....          ! Note 
RESPONSE: SQUEEZE was implemented within the CRYSTAL suite, which does not use
RES files, hence this alert.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
;The crystals were small and weakly diffracting. Despite the use of synchrotron radiation
the data are still of relatively low quality. Restraints to bond angles and distances were therefore used
where necessary to ensure a physically reasonable model, and when required thermal and vibrational restraints were
applied to maintain sensible anisotropic displacment ellipsoids. Some disorder was identified in the macrocycle
and the non-coordinating perchlorate counteranion. This was modelled using refined partial occupancies over two positions.
In addition some diffuse electron density could be identified in the difference map, presumably arising from the presence
of disordered water and acetonitrile solvent molecules. This was modelled using SQUEEZE, leaving a void from which the 
electron density was removed., SQUEEZE
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.194 0.440 0.166 131 32 ' '
2 0.194 0.940 0.334 131 32 ' '
3 -0.194 0.060 0.666 131 32 ' '
4 0.194 0.560 0.834 131 32 ' '
_platon_squeeze_details          
;
The discrete Fourier transform of the void region were treated as 
contributions to the A and B parts of the calculated structure factors.
;

_cell_length_a                   11.1228(2)
_cell_length_b                   13.2793(2)
_cell_length_c                   33.7959(6)
_cell_angle_alpha                90
_cell_angle_beta                 98.2505(15)
_cell_angle_gamma                90
_cell_volume                     4940.09(15)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c '
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x,-y+1/2,z+1/2
-x,y+1/2,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1250 0.1500 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cu 0.2710 1.2020 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126
1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
I -0.7740 1.7190 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776
4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0070 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'

_cell_formula_units_Z            4

_chemical_formula_sum            'C39.00 H45.90 Cl2.00 Cu1 I1 N6 O16.45'
_chemical_formula_moiety         'C39 H45 Cu N6 O8 I, 2(Cl O4), 0.45(H2 O)'
_chemical_compound_source        synthesised
_chemical_formula_weight         1123.33

_cell_measurement_reflns_used    11408
_cell_measurement_theta_min      2
_cell_measurement_theta_max      24
_cell_measurement_temperature    100

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_min          0.02
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_max          0.05

_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2278.107
_exptl_absorpt_coefficient_mu    1.247

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_T_max  1.00
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_device       'CrystalLogic Kappa (3 circle)'
_diffrn_radiation_monochromator  Synchrotron
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_measurement_method       'profile data from ω-scans'

_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      100
_diffrn_reflns_number            59945
_reflns_number_total             9986
_diffrn_reflns_av_R_equivalents  0.077

_diffrn_reflns_theta_min         1.599
_diffrn_reflns_theta_max         26.330
_diffrn_measured_fraction_theta_max 0.901

_diffrn_reflns_theta_full        25.013
_diffrn_measured_fraction_theta_full 0.935

_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       42
_reflns_limit_h_min              -13
_reflns_limit_h_max              14
_reflns_limit_k_min              0
_reflns_limit_k_max              16
_reflns_limit_l_min              0
_reflns_limit_l_max              42

_oxford_diffrn_Wilson_B_factor   2.84
_oxford_diffrn_Wilson_scale      0.27

_atom_sites_solution_primary     Other
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.00
_refine_diff_density_max         1.33

_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         7709
_refine_ls_number_restraints     863
_refine_ls_number_parameters     754
_oxford_refine_ls_R_factor_ref   0.0681
_refine_ls_wR_factor_ref         0.1288
_refine_ls_goodness_of_fit_ref   0.9746
_refine_ls_shift/su_max          0.0035371
_refine_ls_shift/su_mean         0.0000804

_oxford_reflns_number_all        7709
_refine_ls_R_factor_all          0.0681
_refine_ls_wR_factor_all         0.1288

_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                6311
_refine_ls_R_factor_gt           0.0553
_refine_ls_wR_factor_gt          0.1173

_chemical_absolute_configuration .

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr

_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.209E+04 0.321E+04 0.193E+04 739. 129. 
;

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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 0.3253(5) 0.6494(4) 0.40035(17) 0.0377 1.0000 Uani D U . . . .
C2 C 0.4472(5) 0.6494(4) 0.39583(16) 0.0391 1.0000 Uani D U . . . .
C3 C 0.4803(6) 0.6076(5) 0.36127(18) 0.0518 1.0000 Uani D U . . . .
C4 C 0.3955(6) 0.5637(6) 0.33322(19) 0.0562 1.0000 Uani D U . . . .
C5 C 0.2757(6) 0.5629(5) 0.33789(18) 0.0489 1.0000 Uani D U . . . .
C6 C 0.2392(5) 0.6071(5) 0.37141(17) 0.0422 1.0000 Uani D U . . . .
C7 C 0.1057(5) 0.6108(5) 0.37365(19) 0.0461 1.0000 Uani D U . . . .
O8 O 0.0348(4) 0.5486(4) 0.35596(14) 0.0583 1.0000 Uani . . . . . .
N9 N 0.0697(5) 0.6843(5) 0.39634(18) 0.0544 1.0000 Uani . . . . . .
C10 C -0.0555(6) 0.7005(6) 0.4015(2) 0.0571 1.0000 Uani . . . . . .
C11 C -0.0661(6) 0.7445(5) 0.4416(2) 0.0488 1.0000 Uani . . . . . .
H11 H 0.3013 0.6782 0.4227 0.0452 1.0000 Uiso R . . . . .
O12 O -0.0375(4) 0.6693(3) 0.47065(12) 0.0482 1.0000 Uani D . . . . .
C13 C -0.0576(5) 0.6867(2) 0.50931(11) 0.0449 1.0000 Uani D . . . . .
C14 C -0.0571(5) 0.6078(3) 0.53533(14) 0.0471 1.0000 Uani D . . . . .
C15 C -0.0817(5) 0.6252(3) 0.57360(13) 0.0489 1.0000 Uani D . . . . .
C16 C -0.1041(5) 0.7219(4) 0.58645(10) 0.0510 1.0000 Uani D U . . . .
C17 C -0.1027(6) 0.8008(3) 0.55991(14) 0.0535 1.0000 Uani D . . . . .
C18 C -0.0790(6) 0.7846(3) 0.52161(13) 0.0498 1.0000 Uani D . . . . .
C19 C -0.1354(5) 0.7388(5) 0.62810(13) 0.0630 1.0000 Uani D U . . . .
N20 N -0.0566(4) 0.6867(4) 0.66058(12) 0.0593 1.0000 Uani D U . . . .
C21 C -0.1200(6) 0.6878(6) 0.69595(19) 0.0737 0.454(8) Uani D U P 2 1 .
C22 C -0.0708(7) 0.7737(11) 0.7224(3) 0.0794 0.454(8) Uani D U P 2 1 .
N23 N 0.0611(6) 0.7682(8) 0.7249(5) 0.0722 0.454(8) Uani D U P 2 1 .
C24 C 0.1162(9) 0.8630(8) 0.7402(4) 0.0725 0.454(8) Uani D U P 2 1 .
C25 C 0.2509(8) 0.8515(11) 0.7393(3) 0.0684 0.454(8) Uani D U P 2 1 .
N26 N 0.2690(8) 0.8163(13) 0.6988(2) 0.0575 0.454(8) Uani D U P 2 1 .
C27 C 0.3965(10) 0.7808(13) 0.7015(2) 0.0580 0.454(8) Uani D U P 2 1 .
C28 C 0.4460(12) 0.7717(11) 0.6614(3) 0.0513 0.454(8) Uani D U P 2 1 .
C29 C 0.4843(18) 0.6792(9) 0.6481(3) 0.0521 0.454(8) Uani D U P 2 1 .
C30 C 0.518(2) 0.6691(7) 0.6102(4) 0.0553 0.454(8) Uani D . P 2 1 .
C31 C 0.518(2) 0.7530(5) 0.5860(3) 0.0572 0.454(8) Uani D . P 2 1 .
H31 H 0.5608 0.6090 0.3573 0.0611 1.0000 Uiso R . . . . .
C32 C 0.486(2) 0.8472(7) 0.5995(4) 0.0560 0.454(8) Uani D . P 2 1 .
C33 C 0.4485(17) 0.8552(9) 0.6369(3) 0.0520 0.454(8) Uani D U P 2 1 .
O34 O 0.5551(4) 0.7441(3) 0.54845(11) 0.0468 1.0000 Uani D . . . . .
C35 C 0.5678(6) 0.8251(5) 0.5224(2) 0.0479 1.0000 Uani . . . . . .
C36 C 0.6118(6) 0.7859(5) 0.4854(2) 0.0506 1.0000 Uani . . . . . .
N37 N 0.5192(4) 0.7354(4) 0.45864(15) 0.0416 1.0000 Uani . . . . . .
C38 C 0.5449(5) 0.6952(4) 0.42496(17) 0.0390 1.0000 Uani D U . . . .
O39 O 0.6508(4) 0.6953(4) 0.41771(14) 0.0511 1.0000 Uani . . . . . .
N40 N 0.1832(4) 0.6766(4) 0.62771(15) 0.0372 1.0000 Uani . . . . . .
C41 C 0.1913(5) 0.7327(4) 0.59540(17) 0.0348 1.0000 Uani . . . . . .
H41 H 0.4197 0.5331 0.3110 0.0662 1.0000 Uiso R . . . . .
C42 C 0.2308(5) 0.6944(4) 0.56157(17) 0.0352 1.0000 Uani . . . . . .
C43 C 0.2625(5) 0.5936(4) 0.56168(16) 0.0321 1.0000 Uani . . . . . .
C44 C 0.2543(5) 0.5341(4) 0.59451(17) 0.0343 1.0000 Uani . . . . . .
C45 C 0.2140(5) 0.5793(4) 0.62730(16) 0.0325 1.0000 Uani . . . . . .
I46 I 0.33156(4) 0.53223(3) 0.512539(11) 0.0371 1.0000 Uani . . . . . .
C47 C 0.2087(5) 0.5254(5) 0.66573(18) 0.0406 1.0000 Uani . . . . . .
O48 O 0.1748(4) 0.5669(4) 0.69437(12) 0.0487 1.0000 Uani . . . . . .
O49 O 0.2475(4) 0.4325(3) 0.66537(13) 0.0478 1.0000 Uani . . . . . .
C50 C 0.2434(9) 0.3754(7) 0.7021(2) 0.0788 1.0000 Uani . . . . . .
C51 C 0.1572(6) 0.8404(5) 0.5998(2) 0.0449 1.0000 Uani . . . . . .
H51 H 0.2184 0.5338 0.3186 0.0579 1.0000 Uiso R . . . . .
O52 O 0.1191(4) 0.8716(3) 0.62942(14) 0.0533 1.0000 Uani . . . . . .
O53 O 0.1723(4) 0.8941(3) 0.56834(14) 0.0527 1.0000 Uani . . . . . .
C54 C 0.1408(8) 1.0001(5) 0.5695(3) 0.0704 1.0000 Uani . . . . . .
Cu55 Cu 0.12235(8) 0.73556(7) 0.67658(2) 0.0487 1.0000 Uani . U . . . .
Cl56 Cl 0.24508(15) 0.90327(11) 0.45424(5) 0.0485 1.0000 Uani . . . . . .
O57 O 0.1707(5) 0.8905(4) 0.41562(16) 0.0669 1.0000 Uani . . . . . .
O58 O 0.2602(4) 0.8067(3) 0.47375(13) 0.0452 1.0000 Uani . . . . . .
O59 O 0.1874(7) 0.9710(4) 0.4773(2) 0.1031 1.0000 Uani . . . . . .
O60 O 0.3618(5) 0.9409(4) 0.44810(17) 0.0671 1.0000 Uani . . . . . .
Cl61 Cl 0.4129(9) 0.1227(6) 0.7418(2) 0.1057 0.456(10) Uani D . P 1 1 .
O62 O 0.5225(12) 0.0827(10) 0.7644(4) 0.0958 0.456(10) Uani D . P 1 1 .
O63 O 0.4344(17) 0.1428(13) 0.7020(3) 0.1370 0.456(10) Uani D . P 1 1 .
O64 O 0.3802(15) 0.2136(9) 0.7597(4) 0.1174 0.456(10) Uani D . P 1 1 .
O65 O 0.3131(12) 0.0547(10) 0.7418(4) 0.1114 0.456(10) Uani D . P 1 1 .
H91 H 0.1224 0.7276 0.4062 0.0649 1.0000 Uiso R . . . . .
H101 H -0.0990 0.6370 0.3984 0.0671 1.0000 Uiso R . . . . .
H102 H -0.0914 0.7466 0.3810 0.0669 1.0000 Uiso R . . . . .
H111 H -0.0096 0.8003 0.4471 0.0588 1.0000 Uiso R . . . . .
H112 H -0.1481 0.7681 0.4423 0.0590 1.0000 Uiso R . . . . .
C121 C -0.1133(6) 0.6993(9) 0.69773(18) 0.0846 0.546(8) Uani D U P 2 2 .
C122 C -0.0184(7) 0.6780(7) 0.73320(19) 0.0845 0.546(8) Uani D U P 2 2 .
N123 N 0.0747(9) 0.7558(7) 0.7327(4) 0.0777 0.546(8) Uani D U P 2 2 .
C124 C 0.1816(8) 0.7314(9) 0.7618(2) 0.0756 0.546(8) Uani D U P 2 2 .
C125 C 0.2848(9) 0.7919(9) 0.7495(2) 0.0707 0.546(8) Uani D U P 2 2 .
N126 N 0.2977(11) 0.7651(8) 0.7078(3) 0.0609 0.546(8) Uani D U P 2 2 .
C127 C 0.3807(15) 0.8399(9) 0.6937(3) 0.0714 0.546(8) Uani D U P 2 2 .
C128 C 0.4256(12) 0.8144(8) 0.6543(3) 0.0580 0.546(8) Uani D U P 2 2 .
C129 C 0.4741(14) 0.7198(8) 0.6485(3) 0.0518 0.546(8) Uani D U P 2 2 .
C130 C 0.5220(15) 0.6974(6) 0.6140(3) 0.0468 0.546(8) Uani D U P 2 2 .
C131 C 0.5185(15) 0.7689(5) 0.5845(2) 0.0466 0.546(8) Uani D U P 2 2 .
C132 C 0.4751(18) 0.8656(6) 0.5903(3) 0.0541 0.546(8) Uani D U P 2 2 .
C133 C 0.4282(14) 0.8869(7) 0.6249(3) 0.0584 0.546(8) Uani D U P 2 2 .
H141 H -0.0404 0.5433 0.5273 0.0559 1.0000 Uiso R . . . . .
H151 H -0.0819 0.5710 0.5911 0.0578 1.0000 Uiso R . . . . .
Cl161 Cl 0.4061(8) 0.1004(5) 0.7278(2) 0.1101 0.544(10) Uani D . P 1 2 .
O162 O 0.5040(13) 0.0426(11) 0.7474(4) 0.1252 0.544(10) Uani D . P 1 2 .
O163 O 0.4506(12) 0.1936(7) 0.7133(4) 0.0962 0.544(10) Uani D . P 1 2 .
O164 O 0.3225(13) 0.1214(11) 0.7547(4) 0.1237 0.544(10) Uani D . P 1 2 .
O165 O 0.3456(13) 0.0441(9) 0.6947(3) 0.1331 0.544(10) Uani D . P 1 2 .
H171 H -0.1174 0.8657 0.5685 0.0630 1.0000 Uiso R . . . . .
H181 H -0.0786 0.8386 0.5039 0.0590 1.0000 Uiso R . . . . .
H191 H -0.1286 0.8105 0.6338 0.0759 1.0000 Uiso R . . . . .
H192 H -0.2185 0.7175 0.6285 0.0761 1.0000 Uiso R . . . . .
H211 H -0.2070 0.6948 0.6882 0.0890 0.454(8) Uiso R . P 2 1 .
H212 H -0.1033 0.6255 0.7105 0.0889 0.454(8) Uiso R . P 2 1 .
H221 H -0.0736 0.7477 0.7487 0.1210 0.454(8) Uiso R . P 2 1 .
H222 H -0.1054 0.8367 0.7127 0.1210 0.454(8) Uiso R . P 2 1 .
H231 H 0.0860 0.7205 0.7429 0.1071 0.454(8) Uiso R . P 2 1 .
H241 H 0.0799 0.9244 0.7285 0.1079 0.454(8) Uiso R . P 2 1 .
H242 H 0.1097 0.8449 0.7673 0.1081 0.454(8) Uiso R . P 2 1 .
H251 H 0.2867 0.8059 0.7597 0.1019 0.454(8) Uiso R . P 2 1 .
H252 H 0.2744 0.9203 0.7357 0.1021 0.454(8) Uiso R . P 2 1 .
H261 H 0.2654 0.8751 0.6827 0.0733 0.453(8) Uiso R . P 2 1 .
H271 H 0.4001 0.7145 0.7137 0.0719 0.454(8) Uiso R . P 2 1 .
H272 H 0.4484 0.8263 0.7185 0.0718 0.454(8) Uiso R . P 2 1 .
H291 H 0.4877 0.6234 0.6648 0.0620 0.454(8) Uiso R . P 2 1 .
H301 H 0.5411 0.6069 0.6013 0.0658 0.454(8) Uiso R . P 2 1 .
H321 H 0.4893 0.9040 0.5837 0.0649 0.454(8) Uiso R . P 2 1 .
H331 H 0.4256 0.9180 0.6455 0.0610 0.454(8) Uiso R . P 2 1 .
H351 H 0.6259 0.8730 0.5357 0.0571 1.0000 Uiso R . . . . .
H352 H 0.4897 0.8579 0.5149 0.0569 1.0000 Uiso R . . . . .
H361 H 0.6793 0.7400 0.4930 0.0607 1.0000 Uiso R . . . . .
H362 H 0.6405 0.8427 0.4715 0.0609 1.0000 Uiso R . . . . .
H371 H 0.4450 0.7471 0.4609 0.0488 1.0000 Uiso R . . . . .
H421 H 0.2349 0.7348 0.5395 0.0419 1.0000 Uiso R . . . . .
H441 H 0.2753 0.4663 0.5954 0.0409 1.0000 Uiso R . . . . .
H501 H 0.2907 0.4103 0.7244 0.1149 1.0000 Uiso R . . . . .
H502 H 0.2769 0.3100 0.7003 0.1148 1.0000 Uiso R . . . . .
H503 H 0.1618 0.3700 0.7074 0.1149 1.0000 Uiso R . . . . .
H541 H 0.1586 1.0327 0.5455 0.1041 1.0000 Uiso R . . . . .
H542 H 0.1872 1.0306 0.5924 0.1038 1.0000 Uiso R . . . . .
H543 H 0.0551 1.0068 0.5710 0.1040 1.0000 Uiso R . . . . .
H1211 H -0.1519 0.7621 0.6994 0.1239 0.546(8) Uiso R . P 2 2 .
H1212 H -0.1535 0.6329 0.6950 0.1239 0.546(8) Uiso R . P 2 2 .
H1221 H 0.0045 0.6084 0.7380 0.1221 0.546(8) Uiso R . P 2 2 .
H1222 H -0.0511 0.7163 0.7532 0.1220 0.546(8) Uiso R . P 2 2 .
H1231 H 0.0446 0.8163 0.7352 0.1150 0.546(8) Uiso R . P 2 2 .
H1241 H 0.1515 0.7746 0.7809 0.1120 0.546(8) Uiso R . P 2 2 .
H1242 H 0.1994 0.6622 0.7675 0.1120 0.546(8) Uiso R . P 2 2 .
H1251 H 0.2641 0.8636 0.7506 0.0840 0.546(8) Uiso R . P 2 2 .
H1252 H 0.3577 0.7790 0.7675 0.0840 0.546(8) Uiso R . P 2 2 .
H1261 H 0.3409 0.7033 0.7098 0.0770 0.547(8) Uiso R . P 2 2 .
H1271 H 0.4526 0.8470 0.7143 0.0869 0.546(8) Uiso R . P 2 2 .
H1272 H 0.3382 0.9027 0.6907 0.0871 0.546(8) Uiso R . P 2 2 .
H1291 H 0.4764 0.6712 0.6685 0.0600 0.546(8) Uiso R . P 2 2 .
H1301 H 0.5556 0.6347 0.6106 0.0560 0.546(8) Uiso R . P 2 2 .
H1321 H 0.4769 0.9148 0.5709 0.0649 0.546(8) Uiso R . P 2 2 .
H1331 H 0.3976 0.9508 0.6284 0.0699 0.546(8) Uiso R . P 2 2 .
H201 H -0.0528 0.6182 0.6527 0.0720 0.454(8) Uiso R . P 2 1 .
H202 H -0.0551 0.6169 0.6539 0.0720 0.546(8) Uiso R . P 2 2 .
O66 O 0.2957(11) 0.1481(9) 0.6333(4) 0.0757 0.454(16) Uani . . P 3 1 .
H661 H 0.3448 0.1467 0.6573 0.1003 0.450(16) Uiso R . P 3 1 .
H662 H 0.3250 0.1920 0.6164 0.1003 0.450(16) Uiso R . P 3 1 .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.123(12)

loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . C2 . 1.386(7) yes
C1 . C6 . 1.386(8) yes
C1 . H11 . 0.919 no
C2 . C3 . 1.390(8) yes
C2 . C38 . 1.487(6) yes
C3 . C4 . 1.368(9) yes
C3 . H31 . 0.924 no
C4 . C5 . 1.364(9) yes
C4 . H41 . 0.927 no
C5 . C6 . 1.388(8) yes
C5 . H51 . 0.927 no
C6 . C7 . 1.498(7) yes
C7 . O8 . 1.235(8) yes
C7 . N9 . 1.337(8) yes
N9 . C10 . 1.444(8) yes
N9 . H91 . 0.854 no
C10 . C11 . 1.497(9) yes
C10 . H101 . 0.971 no
C10 . H102 . 0.966 no
C11 . O12 . 1.404(8) yes
C11 . H111 . 0.972 no
C11 . H112 . 0.967 no
O12 . C13 . 1.376(4) yes
C13 . C14 . 1.368(4) yes
C13 . C18 . 1.396(4) yes
C14 . C15 . 1.380(4) yes
C14 . H141 . 0.925 no
C15 . C16 . 1.390(4) yes
C15 . H151 . 0.931 no
C16 . C17 . 1.380(4) yes
C16 . C19 . 1.514(4) yes
C17 . C18 . 1.374(4) yes
C17 . H171 . 0.931 no
C18 . H181 . 0.935 no
C19 . N20 . 1.475(4) yes
C19 . H191 . 0.972 no
C19 . H192 . 0.969 no
N20 . C21 . 1.472(6) yes
N20 . Cu55 . 2.090(5) yes
N20 . H201 . 0.950 no
N20 . Cu55 . 2.090(5) yes
N20 . C121 . 1.493(5) yes
N20 . H202 . 0.955 no
C21 . C22 . 1.502(5) yes
C21 . H211 . 0.971 no
C21 . H212 . 0.967 no
C22 . N23 . 1.459(6) yes
C22 . Cu55 . 2.868(7) yes
C22 . H221 . 0.959 no
C22 . H222 . 0.959 no
N23 . C24 . 1.461(6) yes
N23 . Cu55 . 1.909(17) yes
N23 . H231 . 0.892 no
C24 . C25 . 1.511(5) yes
C24 . Cu55 . 2.743(9) yes
C24 . H241 . 0.969 no
C24 . H242 . 0.960 no
C25 . N26 . 1.487(6) yes
C25 . Cu55 . 2.835(8) yes
C25 . H251 . 0.960 no
C25 . H252 . 0.962 no
N26 . C27 . 1.485(6) yes
N26 . Cu55 . 2.005(11) yes
N26 . H261 . 0.950 no
C27 . C28 . 1.539(6) yes
C27 . H271 . 0.972 no
C27 . H272 . 0.967 no
C28 . C29 . 1.396(5) yes
C28 . C33 . 1.388(5) yes
C29 . C30 . 1.390(5) yes
C29 . H291 . 0.930 no
C30 . C31 . 1.381(5) yes
C30 . H301 . 0.929 no
C31 . C32 . 1.396(5) yes
C31 . O34 . 1.395(6) yes
C32 . C33 . 1.388(5) yes
C32 . H321 . 0.929 no
C33 . H331 . 0.930 no
O34 . C35 . 1.411(8) yes
O34 . C35 . 1.411(8) yes
O34 . C131 . 1.378(5) yes
C35 . C36 . 1.498(9) yes
C35 . H351 . 0.970 no
C35 . H352 . 0.973 no
C36 . N37 . 1.436(8) yes
C36 . H361 . 0.972 no
C36 . H362 . 0.967 no
N37 . C38 . 1.326(7) yes
N37 . H371 . 0.854 no
C38 . O39 . 1.237(7) yes
N40 . C41 . 1.335(7) yes
N40 . C45 . 1.336(7) yes
N40 . Cu55 . 2.030(5) yes
C41 . C42 . 1.380(8) yes
C41 . C51 . 1.493(8) yes
C42 . C43 . 1.383(8) yes
C42 . H421 . 0.926 no
C43 . C44 . 1.376(8) yes
C43 . I46 . 2.093(5) yes
C44 . C45 . 1.390(8) yes
C44 . H441 . 0.929 no
C45 . C47 . 1.491(8) yes
C47 . O48 . 1.220(7) yes
C47 . O49 . 1.308(8) yes
O48 . Cu55 . 2.370(5) yes
O49 . C50 . 1.462(8) yes
C50 . H501 . 0.972 no
C50 . H502 . 0.951 no
C50 . H503 . 0.953 no
C51 . O52 . 1.215(7) yes
C51 . O53 . 1.310(8) yes
O52 . Cu55 . 2.406(5) yes
O53 . C54 . 1.453(8) yes
C54 . H541 . 0.967 no
C54 . H542 . 0.955 no
C54 . H543 . 0.965 no
Cu55 . C121 . 2.855(7) yes
Cu55 . C122 . 2.749(8) yes
Cu55 . N123 . 2.060(15) yes
Cu55 . C124 . 2.862(8) yes
Cu55 . N126 . 2.117(11) yes
Cl56 . O57 . 1.452(5) yes
Cl56 . O58 . 1.441(4) yes
Cl56 . O59 . 1.404(6) yes
Cl56 . O60 . 1.433(5) yes
Cl61 . O62 . 1.444(8) yes
Cl61 . O63 . 1.424(9) yes
Cl61 . O64 . 1.421(9) yes
Cl61 . O65 . 1.431(9) yes
C121 . C122 . 1.506(5) yes
C121 . H1211 . 0.944 no
C121 . H1212 . 0.987 no
C122 . N123 . 1.464(6) yes
C122 . H1221 . 0.967 no
C122 . H1222 . 0.957 no
N123 . C124 . 1.466(6) yes
N123 . H1231 . 0.880 no
C124 . C125 . 1.507(5) yes
C124 . H1241 . 0.959 no
C124 . H1242 . 0.954 no
C125 . N126 . 1.480(6) yes
C125 . H1251 . 0.982 no
C125 . H1252 . 0.956 no
N126 . C127 . 1.481(6) yes
N126 . H1261 . 0.949 no
C127 . C128 . 1.526(6) yes
C127 . H1271 . 0.987 no
C127 . H1272 . 0.957 no
C128 . C129 . 1.393(5) yes
C128 . C133 . 1.386(5) yes
C129 . C130 . 1.382(5) yes
C129 . H1291 . 0.931 no
C130 . C131 . 1.374(5) yes
C130 . H1301 . 0.927 no
C131 . C132 . 1.395(5) yes
C132 . C133 . 1.377(5) yes
C132 . H1321 . 0.928 no
C133 . H1331 . 0.928 no
Cl161 . O162 . 1.416(9) yes
Cl161 . O163 . 1.445(8) yes
Cl161 . O164 . 1.417(8) yes
Cl161 . O165 . 1.431(9) yes
O66 . H661 . 0.910 no
O66 . H662 . 0.909 no

loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 . C1 . C6 . 120.7(5) yes
C2 . C1 . H11 . 119.6 no
C6 . C1 . H11 . 119.7 no
C1 . C2 . C3 . 118.3(6) yes
C1 . C2 . C38 . 124.1(5) yes
C3 . C2 . C38 . 117.6(5) yes
C2 . C3 . C4 . 120.9(6) yes
C2 . C3 . H31 . 119.5 no
C4 . C3 . H31 . 119.6 no
C3 . C4 . C5 . 120.7(6) yes
C3 . C4 . H41 . 119.8 no
C5 . C4 . H41 . 119.5 no
C4 . C5 . C6 . 119.8(6) yes
C4 . C5 . H51 . 120.5 no
C6 . C5 . H51 . 119.7 no
C5 . C6 . C1 . 119.6(5) yes
C5 . C6 . C7 . 117.6(6) yes
C1 . C6 . C7 . 122.8(5) yes
C6 . C7 . O8 . 121.5(6) yes
C6 . C7 . N9 . 115.6(6) yes
O8 . C7 . N9 . 122.9(6) yes
C7 . N9 . C10 . 123.4(6) yes
C7 . N9 . H91 . 118.1 no
C10 . N9 . H91 . 118.1 no
N9 . C10 . C11 . 111.7(6) yes
N9 . C10 . H101 . 109.4 no
C11 . C10 . H101 . 109.6 no
N9 . C10 . H102 . 108.4 no
C11 . C10 . H102 . 108.8 no
H101 . C10 . H102 . 108.9 no
C10 . C11 . O12 . 108.4(6) yes
C10 . C11 . H111 . 109.7 no
O12 . C11 . H111 . 109.5 no
C10 . C11 . H112 . 110.2 no
O12 . C11 . H112 . 109.5 no
H111 . C11 . H112 . 109.5 no
C11 . O12 . C13 . 119.5(4) yes
O12 . C13 . C14 . 119.67(5) yes
O12 . C13 . C18 . 119.81(5) yes
C14 . C13 . C18 . 120.52(5) yes
C13 . C14 . C15 . 119.43(6) yes
C13 . C14 . H141 . 120.2 no
C15 . C14 . H141 . 120.4 no
C14 . C15 . C16 . 121.08(6) yes
C14 . C15 . H151 . 119.0 no
C16 . C15 . H151 . 119.9 no
C15 . C16 . C17 . 118.61(6) yes
C15 . C16 . C19 . 120.2(3) yes
C17 . C16 . C19 . 121.1(3) yes
C16 . C17 . C18 . 121.01(6) yes
C16 . C17 . H171 . 118.7 no
C18 . C17 . H171 . 120.3 no
C13 . C18 . C17 . 119.33(6) yes
C13 . C18 . H181 . 120.5 no
C17 . C18 . H181 . 120.2 no
C16 . C19 . N20 . 115.52(5) yes
C16 . C19 . H191 . 107.9 no
N20 . C19 . H191 . 107.0 no
C16 . C19 . H192 . 108.4 no
N20 . C19 . H192 . 108.6 no
H191 . C19 . H192 . 109.4 no
C19 . N20 . C21 . 107.27(7) yes
C19 . N20 . Cu55 . 119.2(4) yes
C21 . N20 . Cu55 . 109.6(3) yes
C19 . N20 . H201 . 106.6 no
C21 . N20 . H201 . 106.5 no
Cu55 . N20 . H201 . 106.9 no
C19 . N20 . Cu55 . 119.2(4) yes
C19 . N20 . C121 . 107.19(7) yes
Cu55 . N20 . C121 . 104.4(4) yes
C19 . N20 . H202 . 108.0 no
Cu55 . N20 . H202 . 108.4 no
C121 . N20 . H202 . 109.4 no
N20 . C21 . C22 . 108.35(7) yes
N20 . C21 . H211 . 111.0 no
C22 . C21 . H211 . 110.6 no
N20 . C21 . H212 . 108.9 no
C22 . C21 . H212 . 108.7 no
H211 . C21 . H212 . 109.3 no
C21 . C22 . N23 . 105.92(7) yes
C21 . C22 . Cu55 . 77.40(18) yes
N23 . C22 . Cu55 . 36.7(7) yes
C21 . C22 . H221 . 102.8 no
N23 . C22 . H221 . 95.4 no
Cu55 . C22 . H221 . 124.3 no
C21 . C22 . H222 . 111.4 no
N23 . C22 . H222 . 114.5 no
Cu55 . C22 . H222 . 105.4 no
H221 . C22 . H222 . 124.5 no
C22 . N23 . C24 . 110.21(7) yes
C22 . N23 . Cu55 . 116.1(10) yes
C24 . N23 . Cu55 . 108.3(10) yes
C22 . N23 . H231 . 106.7 no
C24 . N23 . H231 . 107.4 no
Cu55 . N23 . H231 . 107.8 no
N23 . C24 . C25 . 105.90(7) yes
N23 . C24 . Cu55 . 41.4(7) yes
C25 . C24 . Cu55 . 77.66(18) yes
N23 . C24 . H241 . 116.9 no
C25 . C24 . H241 . 115.7 no
Cu55 . C24 . H241 . 104.8 no
N23 . C24 . H242 . 92.0 no
C25 . C24 . H242 . 101.8 no
Cu55 . C24 . H242 . 127.4 no
H241 . C24 . H242 . 121.1 no
C24 . C25 . N26 . 108.35(7) yes
C24 . C25 . Cu55 . 70.96(19) yes
N26 . C25 . Cu55 . 42.4(4) yes
C24 . C25 . H251 . 111.0 no
N26 . C25 . H251 . 111.4 no
Cu55 . C25 . H251 . 107.8 no
C24 . C25 . H252 . 101.2 no
N26 . C25 . H252 . 96.3 no
Cu55 . C25 . H252 . 122.6 no
H251 . C25 . H252 . 126.7 no
C25 . N26 . C27 . 107.29(7) yes
C25 . N26 . Cu55 . 107.6(6) yes
C27 . N26 . Cu55 . 124.9(12) yes
C25 . N26 . H261 . 105.5 no
C27 . N26 . H261 . 104.9 no
Cu55 . N26 . H261 . 105.1 no
N26 . C27 . C28 . 115.52(7) yes
N26 . C27 . H271 . 107.1 no
C28 . C27 . H271 . 107.8 no
N26 . C27 . H272 . 108.8 no
C28 . C27 . H272 . 108.3 no
H271 . C27 . H272 . 109.1 no
C27 . C28 . C29 . 121.2(9) yes
C27 . C28 . C33 . 120.2(8) yes
C29 . C28 . C33 . 118.56(6) yes
C28 . C29 . C30 . 121.05(6) yes
C28 . C29 . H291 . 119.5 no
C30 . C29 . H291 . 119.5 no
C29 . C30 . C31 . 119.39(6) yes
C29 . C30 . H301 . 120.5 no
C31 . C30 . H301 . 120.1 no
C30 . C31 . C32 . 120.49(6) yes
C30 . C31 . O34 . 119.71(6) yes
C32 . C31 . O34 . 119.75(6) yes
C31 . C32 . C33 . 119.35(6) yes
C31 . C32 . H321 . 120.5 no
C33 . C32 . H321 . 120.1 no
C32 . C33 . C28 . 121.02(6) yes
C32 . C33 . H331 . 119.0 no
C28 . C33 . H331 . 120.0 no
C31 . O34 . C35 . 125.0(4) yes
C35 . O34 . C131 . 116.0(4) yes
O34 . C35 . C36 . 109.3(5) yes
O34 . C35 . H351 . 109.3 no
C36 . C35 . H351 . 109.8 no
O34 . C35 . H352 . 109.8 no
C36 . C35 . H352 . 108.9 no
H351 . C35 . H352 . 109.8 no
C35 . C36 . N37 . 113.4(5) yes
C35 . C36 . H361 . 109.2 no
N37 . C36 . H361 . 109.3 no
C35 . C36 . H362 . 107.7 no
N37 . C36 . H362 . 108.4 no
H361 . C36 . H362 . 108.8 no
C36 . N37 . C38 . 120.4(5) yes
C36 . N37 . H371 . 118.3 no
C38 . N37 . H371 . 118.8 no
C2 . C38 . N37 . 120.4(5) yes
C2 . C38 . O39 . 119.7(5) yes
N37 . C38 . O39 . 119.9(5) yes
C41 . N40 . C45 . 118.9(5) yes
C41 . N40 . Cu55 . 121.3(4) yes
C45 . N40 . Cu55 . 119.8(4) yes
N40 . C41 . C42 . 122.6(5) yes
N40 . C41 . C51 . 114.0(5) yes
C42 . C41 . C51 . 123.4(6) yes
C41 . C42 . C43 . 117.8(5) yes
C41 . C42 . H421 . 120.8 no
C43 . C42 . H421 . 121.5 no
C42 . C43 . C44 . 120.8(5) yes
C42 . C43 . I46 . 119.8(4) yes
C44 . C43 . I46 . 119.4(4) yes
C43 . C44 . C45 . 117.4(5) yes
C43 . C44 . H441 . 122.5 no
C45 . C44 . H441 . 120.1 no
C44 . C45 . N40 . 122.6(5) yes
C44 . C45 . C47 . 123.0(5) yes
N40 . C45 . C47 . 114.4(5) yes
C45 . C47 . O48 . 122.0(6) yes
C45 . C47 . O49 . 113.0(5) yes
O48 . C47 . O49 . 125.0(6) yes
C47 . O48 . Cu55 . 108.6(4) yes
C47 . O49 . C50 . 115.5(5) yes
O49 . C50 . H501 . 109.4 no
O49 . C50 . H502 . 110.9 no
H501 . C50 . H502 . 108.3 no
O49 . C50 . H503 . 110.3 no
H501 . C50 . H503 . 108.3 no
H502 . C50 . H503 . 109.6 no
C41 . C51 . O52 . 122.1(6) yes
C41 . C51 . O53 . 112.2(5) yes
O52 . C51 . O53 . 125.7(6) yes
C51 . O52 . Cu55 . 108.4(4) yes
C51 . O53 . C54 . 116.4(5) yes
O53 . C54 . H541 . 109.3 no
O53 . C54 . H542 . 109.2 no
H541 . C54 . H542 . 109.7 no
O53 . C54 . H543 . 109.6 no
H541 . C54 . H543 . 108.9 no
H542 . C54 . H543 . 110.0 no
O48 . Cu55 . O52 . 149.02(14) yes
O48 . Cu55 . N20 . 87.86(19) yes
O52 . Cu55 . N20 . 97.96(18) yes
O48 . Cu55 . N40 . 75.11(17) yes
O52 . Cu55 . N40 . 74.09(18) yes
N20 . Cu55 . N40 . 94.93(17) yes
O48 . Cu55 . C24 . 114.7(3) yes
O52 . Cu55 . C24 . 93.2(3) yes
N20 . Cu55 . C24 . 105.3(2) yes
N40 . Cu55 . C24 . 157.5(2) yes
O48 . Cu55 . N26 . 104.7(5) yes
O52 . Cu55 . N26 . 77.3(4) yes
N20 . Cu55 . N26 . 163.0(4) yes
N40 . Cu55 . N26 . 99.3(3) yes
C24 . Cu55 . N26 . 59.2(2) yes
O48 . Cu55 . C25 . 104.2(3) yes
O52 . Cu55 . C25 . 92.6(3) yes
N20 . Cu55 . C25 . 136.2(2) yes
N40 . Cu55 . C25 . 128.8(2) yes
C24 . Cu55 . C25 . 31.38(13) yes
O48 . Cu55 . N23 . 95.9(4) yes
O52 . Cu55 . N23 . 115.1(4) yes
N20 . Cu55 . N23 . 81.3(2) yes
N40 . Cu55 . N23 . 170.4(4) yes
C24 . Cu55 . N23 . 30.4(3) yes
O48 . Cu55 . C22 . 101.9(4) yes
O52 . Cu55 . C22 . 106.5(4) yes
N20 . Cu55 . C22 . 55.59(17) yes
N40 . Cu55 . C22 . 150.5(2) yes
C24 . Cu55 . C22 . 50.47(15) yes
N26 . Cu55 . C25 . 30.0(2) yes
N26 . Cu55 . N23 . 86.0(3) yes
C25 . Cu55 . N23 . 56.0(2) yes
N26 . Cu55 . C22 . 109.6(3) yes
C25 . Cu55 . C22 . 80.65(18) yes
N23 . Cu55 . C22 . 27.2(3) yes
O48 . Cu55 . O52 . 149.02(14) yes
O48 . Cu55 . N20 . 87.86(19) yes
O52 . Cu55 . N20 . 97.96(18) yes
O48 . Cu55 . N40 . 75.11(17) yes
O52 . Cu55 . N40 . 74.09(18) yes
N20 . Cu55 . N40 . 94.93(17) yes
O48 . Cu55 . C121 . 88.8(2) yes
O52 . Cu55 . C121 . 111.4(2) yes
N20 . Cu55 . C121 . 30.43(18) yes
N40 . Cu55 . C121 . 124.3(2) yes
O48 . Cu55 . C122 . 72.8(2) yes
O52 . Cu55 . C122 . 135.6(2) yes
N20 . Cu55 . C122 . 58.48(17) yes
N40 . Cu55 . C122 . 138.5(2) yes
C121 . Cu55 . C122 . 31.10(12) yes
O48 . Cu55 . N123 . 88.6(2) yes
O52 . Cu55 . N123 . 122.1(3) yes
N20 . Cu55 . N123 . 85.3(3) yes
N40 . Cu55 . N123 . 163.7(3) yes
C121 . Cu55 . N123 . 54.86(19) yes
O48 . Cu55 . C124 . 73.4(3) yes
O52 . Cu55 . C124 . 131.4(3) yes
N20 . Cu55 . C124 . 109.13(19) yes
N40 . Cu55 . C124 . 139.1(3) yes
C121 . Cu55 . C124 . 80.32(17) yes
O48 . Cu55 . N126 . 82.7(4) yes
O52 . Cu55 . N126 . 96.7(3) yes
N20 . Cu55 . N126 . 164.1(3) yes
N40 . Cu55 . N126 . 95.0(2) yes
C121 . Cu55 . N126 . 136.0(2) yes
C122 . Cu55 . N123 . 31.5(2) yes
C122 . Cu55 . C124 . 50.65(14) yes
N123 . Cu55 . C124 . 29.3(2) yes
C122 . Cu55 . N126 . 106.3(2) yes
N123 . Cu55 . N126 . 81.8(3) yes
C124 . Cu55 . N126 . 55.9(2) yes
O57 . Cl56 . O58 . 108.8(3) yes
O57 . Cl56 . O59 . 109.1(4) yes
O58 . Cl56 . O59 . 110.4(3) yes
O57 . Cl56 . O60 . 108.8(3) yes
O58 . Cl56 . O60 . 109.2(3) yes
O59 . Cl56 . O60 . 110.6(4) yes
O62 . Cl61 . O63 . 108.9(7) yes
O62 . Cl61 . O64 . 109.6(7) yes
O63 . Cl61 . O64 . 109.4(7) yes
O62 . Cl61 . O65 . 111.3(7) yes
O63 . Cl61 . O65 . 110.9(8) yes
O64 . Cl61 . O65 . 106.8(7) yes
N20 . C121 . Cu55 . 45.1(3) yes
N20 . C121 . C122 . 108.43(7) yes
Cu55 . C121 . C122 . 70.58(14) yes
N20 . C121 . H1211 . 113.6 no
Cu55 . C121 . H1211 . 108.0 no
C122 . C121 . H1211 . 113.0 no
N20 . C121 . H1212 . 93.6 no
Cu55 . C121 . H1212 . 123.3 no
C122 . C121 . H1212 . 99.3 no
H1211 . C121 . H1212 . 126.2 no
C121 . C122 . Cu55 . 78.32(15) yes
C121 . C122 . N123 . 105.96(7) yes
Cu55 . C122 . N123 . 47.3(7) yes
C121 . C122 . H1221 . 116.8 no
Cu55 . C122 . H1221 . 102.7 no
N123 . C122 . H1221 . 120.4 no
C121 . C122 . H1222 . 99.6 no
Cu55 . C122 . H1222 . 130.9 no
N123 . C122 . H1222 . 88.5 no
H1221 . C122 . H1222 . 120.5 no
C122 . N123 . Cu55 . 101.2(8) yes
C122 . N123 . C124 . 110.15(7) yes
Cu55 . N123 . C124 . 107.3(8) yes
C122 . N123 . H1231 . 111.4 no
Cu55 . N123 . H1231 . 111.0 no
C124 . N123 . H1231 . 114.9 no
N123 . C124 . Cu55 . 43.4(6) yes
N123 . C124 . C125 . 105.96(7) yes
Cu55 . C124 . C125 . 77.73(19) yes
N123 . C124 . H1241 . 89.5 no
Cu55 . C124 . H1241 . 127.8 no
C125 . C124 . H1241 . 102.7 no
N123 . C124 . H1242 . 118.2 no
Cu55 . C124 . H1242 . 103.4 no
C125 . C124 . H1242 . 115.1 no
H1241 . C124 . H1242 . 121.6 no
C124 . C125 . N126 . 108.39(7) yes
C124 . C125 . H1251 . 108.4 no
N126 . C125 . H1251 . 108.7 no
C124 . C125 . H1252 . 109.9 no
N126 . C125 . H1252 . 111.8 no
H1251 . C125 . H1252 . 109.5 no
C125 . N126 . Cu55 . 108.1(6) yes
C125 . N126 . C127 . 107.25(7) yes
Cu55 . N126 . C127 . 122.4(11) yes
C125 . N126 . H1261 . 105.1 no
Cu55 . N126 . H1261 . 107.2 no
C127 . N126 . H1261 . 105.6 no
N126 . C127 . C128 . 115.53(7) yes
N126 . C127 . H1271 . 108.4 no
C128 . C127 . H1271 . 107.8 no
N126 . C127 . H1272 . 107.3 no
C128 . C127 . H1272 . 108.7 no
H1271 . C127 . H1272 . 109.1 no
C127 . C128 . C129 . 120.2(7) yes
C127 . C128 . C133 . 121.0(7) yes
C129 . C128 . C133 . 118.57(6) yes
C128 . C129 . C130 . 121.04(6) yes
C128 . C129 . H1291 . 119.7 no
C130 . C129 . H1291 . 119.3 no
C129 . C130 . C131 . 119.38(6) yes
C129 . C130 . H1301 . 120.6 no
C131 . C130 . H1301 . 120.1 no
O34 . C131 . C130 . 119.71(6) yes
O34 . C131 . C132 . 119.77(6) yes
C130 . C131 . C132 . 120.50(5) yes
C131 . C132 . C133 . 119.34(6) yes
C131 . C132 . H1321 . 120.4 no
C133 . C132 . H1321 . 120.3 no
C128 . C133 . C132 . 121.00(6) yes
C128 . C133 . H1331 . 119.8 no
C132 . C133 . H1331 . 119.2 no
O162 . Cl161 . O163 . 110.2(7) yes
O162 . Cl161 . O164 . 109.8(7) yes
O163 . Cl161 . O164 . 109.7(7) yes
O162 . Cl161 . O165 . 109.0(7) yes
O163 . Cl161 . O165 . 109.2(7) yes
O164 . Cl161 . O165 . 109.0(7) yes
H661 . O66 . H662 . 110.5 no

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C1 . H11 . O58 . 161.51 0.919 2.515 3.399(12) yes
C3 . H31 . O49 2_666 162.4 0.924 2.430 3.323(12) yes
C4 . H41 . O62 3_554 163.8 0.927 2.583 3.483(12) yes
N9 . H91 . O57 . 147.5 0.854 2.241 2.996(12) yes
C11 . H112 . O39 1_455 132.53 0.967 2.469 3.203(12) yes
C15 . H151 . O8 2_566 165.17 0.931 2.395 3.303(12) yes
C124 . H231 . C22 . 149.5 1.169 1.916 2.983(12) yes
C124 . H231 . C121 . 176.0 1.169 2.519 3.687(12) yes
C124 . H231 . C122 . 155.2 1.169 1.290 2.402(12) yes
C25 . H252 . O65 1_565 165.8 0.962 1.841 2.784(12) yes
C25 . H252 . O165 1_565 148.8 0.962 2.358 3.220(12) yes
N26 . H261 . O165 1_565 132.9 0.950 2.427 3.151(12) yes
C27 . H271 . O62 4_656 157.1 0.972 2.042 2.962(12) yes
C127 . H272 . O64 4_656 140.9( 1.058 2.453 3.341(12) yes
C29 . H291 . O62 4_656 139.5 0.930 2.472 3.236(12) yes
C35 . H351 . O60 2_676 138.78 0.970 2.531 3.323(12) yes
N37 . H371 . O58 . 168.67 0.854 2.301 3.143(12) yes
C42 . H421 . O58 . 166.84 0.926 2.471 3.379(12) yes
C44 . H441 . O39 2_666 165.10 0.929 2.363 3.270(12) yes
C50 . H502 . O64 . 123.4 0.951 2.517 3.142(12) yes
C50 . H502 . O163 . 149.9 0.951 2.464 3.322(12) yes
C54 . H541 . O59 . 134.0 0.967 2.509 3.256(12) yes
C54 . H542 . O66 1_565 161.2 0.955 2.308 3.226(12) yes
C22 . H1211 . C19 . 122.2 1.113 2.463 3.198(12) yes
C24 . H1231 . C22 . 164.2 1.004 1.413 2.395(12) yes
C24 . H1231 . C121 . 159.1 1.004 2.543 3.499(12) yes
C24 . H1231 . C122 . 148.6 1.004 1.964 2.869(12) yes
C125 . H1252 . O163 4_656 152.7 0.956 2.419 3.298(12) yes
N126 . H1261 . O62 4_656 158.7 0.949 2.292 3.195(12) yes
C127 . H1272 . O165 1_565 147.8 0.957 1.883 2.741(12) yes
C29 . H1291 . C27 . 121.8 0.716 2.106 2.557(12) yes
C29 . H1291 . O62 4_656 159.8 0.716 2.554 3.236(12) yes
C129 . H1291 . O62 4_656 163.5 0.931 2.554 3.457(12) yes
N20 . H201 . O8 2_566 171.16 0.950 2.248 3.190(12) yes
N20 . H202 . O8 2_566 173.52 0.955 2.239 3.190(12) yes
O66 . H661 . O63 . 179.1 0.910 1.687 2.597(12) yes
O66 . H661 . O163 . 162.1 0.910 2.172 3.052(12) yes
O66 . H661 . O165 . 124.3 0.910 1.859 2.488(12) yes
O66 . H662 . O39 2_666 164.9 0.909 1.931 2.819(12) yes

_iucr_refine_instruction_details_constraints 
;
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
EQUIVALENCE PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
EQUIVALENCE PART(2001,OCC) PART(2002,OCC) 
WEIGHT -1 PART(2002,OCC) 
EQUIVALENCE PART(3001,OCC) 
RIDE C(31,U'S) C(131,U'S) 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE N   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) H   ( 102,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) H   ( 192,X'S) 
RIDE N   (  20,X'S) H   ( 201,X'S) H   ( 202,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE N   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) 
RIDE N   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) 
RIDE N   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) H   ( 502,X'S) H   ( 503,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) H   ( 542,X'S) H   ( 543,X'S) 
RIDE C   ( 121,X'S) H   (1211,X'S) H   (1212,X'S) 
RIDE C   ( 122,X'S) H   (1221,X'S) H   (1222,X'S) 
RIDE N   ( 123,X'S) H   (1231,X'S) 
RIDE C   ( 124,X'S) H   (1241,X'S) H   (1242,X'S) 
RIDE C   ( 125,X'S) H   (1251,X'S) H   (1252,X'S) 
RIDE N   ( 126,X'S) H   (1261,X'S) 
RIDE C   ( 127,X'S) H   (1271,X'S) H   (1272,X'S) 
RIDE C   ( 129,X'S) H   (1291,X'S) 
RIDE C   ( 130,X'S) H   (1301,X'S) 
RIDE C   ( 132,X'S) H   (1321,X'S) 
RIDE C   ( 133,X'S) H   (1331,X'S) 
RIDE O   (  66,X'S) H   ( 661,X'S) H   ( 662,X'S) 
END                                                                             
;

_iucr_refine_instruction_details_restraints 
;
#LIST     16                                                                    
NO 
REM TRISAMINE CLEFT 
SAME C(28) C(27) N(26) C(25) C(24) N(23) 
CONT C(22) C(21) N(20) C(19) C(16) AND 
CONT C(16) C(19) N(20) C(21) C(22) N(23) C(24) 
CONT C(25) N(26) C(27) C(28) AND 
CONT C(128) C(127) N(126) C(125) C(124) N(123) 
CONT C(122) C(121) N(20) C(19) C(16) AND 
CONT C(16) C(19) N(20) C(121) C(122) N(123) C(124) 
CONT C(125) N(126) C(127) C(128) 
DISTANCE 1.52, 0.01 = C(21) TO C(22) C(24) TO C(25) 
CONT C(121) TO C(122) C(124) TO C(125) 
DISTANCE 1.46, 0.02 = N(20) TO C(21)  N(20) TO C(121) 
CONT C(22) TO N(23) C(122) TO N(123) 
CONT N(23) TO C(24) N(123) TO C(124) C(25) TO N(26) 
CONT C(125) TO N(126) N(26) TO C(27) N(126) TO C(127) 
DISTANCE 0.0, 0.02 = MEAN N(20) TO C(21)  N(20) TO C(121) 
CONT C(22) TO N(23) C(122) TO N(123) 
CONT N(23) TO C(24) N(123) TO C(124) C(25) TO N(26) 
CONT C(125) TO N(126) N(26) TO C(27) N(126) TO C(127) 
DISTANCE 1.52, 0.02 = C(16) TO C(19) C(27) TO C(28) 
CONT C(127) TO C(128) 
ANGLE 0,1 = MEAN N(20) TO C(21) TO C(22) N(20) TO C(121) TO C(122) 
CONT C(21) TO C(22) TO N(23) C(121) TO C(122) TO N(123) 
CONT N(23) TO C(24) TO C(25) N(123) TO C(124) TO C(125) 
CONT C(24) TO C(25) TO N(26) C(124) TO C(125) TO N(126) 
ANGLE 0, 1 = MEAN C(19) TO N(20) TO C(21) C(19) TO N(20) TO C(121) 
CONT C(22) TO N(23) TO C(24) C(122) TO N(123) TO C(124) 
CONT C(25) TO N(26) TO C(27) C(125) TO N(126) TO C(127) 
SIMU 0.04 C(19) N(20) C(21) C(22) N(23) C(24) C(25) N(26) C(27) AND 
CONT C(19) N(20) C(121) C(122) N(123) C(124) C(125) N(126) C(127) 
DELU 0.01 C(19) N(20) C(21) C(22) N(23) C(24) C(25) N(26) C(27) 
DELU 0.01 C(19) N(20) C(121) C(122) N(123) C(124) C(125) N(126) C(127) 
REM BENZENE RINGS 
SAME O(12) C(13) C(14) C(15) C(16) C(17) C(18) AND 
CONT O(12) C(13) C(18) C(17) C(16) C(15) C(14) AND 
CONT O(34) C(31) C(32) C(33) C(28) C(29) C(30) AND 
CONT O(34) C(31) C(30) C(29) C(28) C(33) C(32) AND 
CONT O(34) C(131) C(132) C(133) C(128) C(129) C(130) AND 
CONT O(34) C(131) C(130) C(129) C(128) C(133) C(132) 
SIMU 0.01 C(28) C(29) C(30) C(31) C(32) C(33) 
SIMU 0.01 C(128) C(129) C(130) C(131) C(132) C(133) 
DELU 0.01 C(28) C(29) C(30) C(31) C(32) C(33) 
DELU 0.01 C(128) C(129) C(130) C(131) C(132) C(133) 
DISTANCE 0.0, 0.02 = MEAN C(1) TO C(2) C(2) TO C(3) 
CONT C(3) TO C(4) C(4) TO C(5) C(5) TO C(6) 
CONT C(6) TO C(1) 
DISTANCE 1.5, 0.01 = C(6) TO C(7) C(2) TO C(38) 
REM PERCHLORATE 
SIMU 0.02 O(62) CL(61) O(63) 
SIMU 0.02 O(62) CL(61) O(64) 
SIMU 0.02 O(62) CL(61) O(65) 
SIMU 0.02 O(63) CL(61) O(64) 
SIMU 0.02 O(63) CL(61) O(65) 
SIMU 0.02 O(64) CL(61) O(65) 
SIMU 0.02 O(162) CL(161) O(163) 
SIMU 0.02 O(162) CL(161) O(164) 
SIMU 0.02 O(162) CL(161) O(165) 
SIMU 0.02 O(163) CL(161) O(164) 
SIMU 0.02 O(163) CL(161) O(165) 
SIMU 0.02 O(164) CL(161) O(165) 
DELU 0.01 O(62) CL(61) O(63) 
DELU 0.01 O(62) CL(61) O(64) 
DELU 0.01 O(62) CL(61) O(65) 
DELU 0.01 O(63) CL(61) O(64) 
DELU 0.01 O(63) CL(61) O(65) 
DELU 0.01 O(64) CL(61) O(65) 
DELU 0.01 O(162) CL(161) O(163) 
DELU 0.01 O(162) CL(161) O(164) 
DELU 0.01 O(162) CL(161) O(165) 
DELU 0.01 O(163) CL(161) O(164) 
DELU 0.01 O(163) CL(161) O(165) 
DELU 0.01 O(164) CL(161) O(165) 
DISTANCE 1.43, 0.01 = CL(61) TO O(62) CL(61) TO O(63) 
CONT CL(61) TO O(64) CL(61) TO O(65) 
ANGLE 109,1 = O(62) TO CL(61) TO O(63) 
CONT O(62) TO CL(61) TO O(64) O(62) TO CL(61) TO O(65) 
CONT O(63) TO CL(61) TO O(64) O(63) TO CL(61) TO O(65) 
CONT O(64) TO CL(61) TO O(65) 
DISTANCE 1.43, 0.01 = CL(161) TO O(162) CL(161) TO O(163) 
CONT CL(161) TO O(164) CL(161) TO O(165) 
ANGLE 109,1 = O(162) TO CL(161) TO O(163) 
CONT O(162) TO CL(161) TO O(164) O(162) TO CL(161) TO O(165) 
CONT O(163) TO CL(161) TO O(164) O(163) TO CL(161) TO O(165) 
CONT O(164) TO CL(161) TO O(165) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = C(1) TO C(2) 
VIBR .0, 0.00200 = C(1) TO C(6) 
VIBR .0, 0.00500 = C(6) TO C(2) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00200 = C(2) TO C(38) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00500 = C(38) TO C(1) 
VIBR .0, 0.00500 = C(38) TO C(3) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00200 = C(4) TO C(5) 
VIBR .0, 0.00500 = C(5) TO C(3) 
VIBR .0, 0.00200 = C(5) TO C(6) 
VIBR .0, 0.00500 = C(6) TO C(4) 
VIBR .0, 0.00200 = C(6) TO C(7) 
VIBR .0, 0.00500 = C(1) TO C(5) 
VIBR .0, 0.00500 = C(7) TO C(5) 
VIBR .0, 0.00500 = C(7) TO C(1) 
VIBR .0, 0.00200 = C(128) TO C(129) 
VIBR .0, 0.00200 = C(128) TO C(133) 
VIBR .0, 0.00500 = C(133) TO C(129) 
VIBR .0, 0.00200 = C(129) TO C(130) 
VIBR .0, 0.00500 = C(130) TO C(128) 
VIBR .0, 0.00200 = C(131) TO C(132) 
VIBR .0, 0.00200 = C(131) TO C(130) 
VIBR .0, 0.00500 = C(130) TO C(132) 
VIBR .0, 0.00200 = C(132) TO C(133) 
VIBR .0, 0.00500 = C(133) TO C(131) 
VIBR .0, 0.00500 = C(132) TO C(128) 
VIBR .0, 0.00200 = C(19) TO N(20) 
VIBR .0, 0.00500 = N(20) TO C(16) 
VIBR .0, 0.00200 = N(20) TO C(21) 
VIBR .0, 0.00200 = N(20) TO CU(55) 
VIBR .0, 0.00500 = C(21) TO C(19) 
VIBR .0, 0.00500 = CU(55) TO C(19) 
VIBR .0, 0.00500 = CU(55) TO C(21) 
VIBR .0, 0.00200 = N(20) TO CU(55) 
VIBR .0, 0.00200 = N(20) TO C(121) 
VIBR .0, 0.00500 = CU(55) TO C(19) 
VIBR .0, 0.00500 = C(121) TO C(19) 
VIBR .0, 0.00500 = C(121) TO CU(55) 
VIBR .0, 0.00200 = C(21) TO C(22) 
VIBR .0, 0.00500 = C(22) TO N(20) 
VIBR .0, 0.00200 = C(22) TO N(23) 
VIBR .0, 0.00500 = N(23) TO C(21) 
VIBR .0, 0.00200 = N(23) TO C(24) 
VIBR .0, 0.00200 = N(23) TO CU(55) 
VIBR .0, 0.00500 = C(24) TO C(22) 
VIBR .0, 0.00500 = CU(55) TO C(22) 
VIBR .0, 0.00500 = CU(55) TO C(24) 
VIBR .0, 0.00200 = C(24) TO C(25) 
VIBR .0, 0.00200 = C(24) TO CU(55) 
VIBR .0, 0.00500 = C(25) TO N(23) 
VIBR .0, 0.00500 = CU(55) TO N(23) 
VIBR .0, 0.00500 = CU(55) TO C(25) 
VIBR .0, 0.00200 = C(25) TO N(26) 
VIBR .0, 0.00200 = C(25) TO CU(55) 
VIBR .0, 0.00500 = N(26) TO C(24) 
VIBR .0, 0.00500 = CU(55) TO C(24) 
VIBR .0, 0.00500 = CU(55) TO N(26) 
VIBR .0, 0.00200 = N(26) TO C(27) 
VIBR .0, 0.00200 = N(26) TO CU(55) 
VIBR .0, 0.00500 = C(27) TO C(25) 
VIBR .0, 0.00500 = CU(55) TO C(25) 
VIBR .0, 0.00500 = CU(55) TO C(27) 
VIBR .0, 0.00200 = C(27) TO C(28) 
VIBR .0, 0.00500 = C(28) TO N(26) 
VIBR .0, 0.00200 = C(28) TO C(29) 
VIBR .0, 0.00200 = C(28) TO C(33) 
VIBR .0, 0.00500 = C(29) TO C(27) 
VIBR .0, 0.00200 = CU(55) TO N(126) 
VIBR .0, 0.00200 = CU(55) TO N(123) 
VIBR .0, 0.00200 = CU(55) TO C(122) 
VIBR .0, 0.00200 = CU(55) TO C(121) 
VIBR .0, 0.00500 = N(123) TO N(126) 
VIBR .0, 0.00500 = C(122) TO N(20) 
VIBR .0, 0.00500 = C(122) TO N(126) 
VIBR .0, 0.00500 = C(122) TO N(123) 
VIBR .0, 0.00500 = C(121) TO N(20) 
VIBR .0, 0.00500 = C(121) TO N(126) 
VIBR .0, 0.00500 = C(121) TO N(123) 
VIBR .0, 0.00500 = C(121) TO C(122) 
VIBR .0, 0.00200 = C(124) TO C(125) 
VIBR .0, 0.00200 = C(124) TO N(123) 
VIBR .0, 0.00500 = N(123) TO C(125) 
VIBR .0, 0.00200 = C(125) TO N(126) 
VIBR .0, 0.00500 = N(126) TO C(124) 
VIBR .0, 0.00200 = N(126) TO C(127) 
VIBR .0, 0.00500 = CU(55) TO C(125) 
VIBR .0, 0.00500 = C(127) TO C(125) 
VIBR .0, 0.00500 = C(127) TO CU(55) 
VIBR .0, 0.00200 = N(123) TO C(122) 
VIBR .0, 0.00500 = CU(55) TO C(124) 
VIBR .0, 0.00500 = C(122) TO C(124) 
VIBR .0, 0.00500 = C(122) TO CU(55) 
VIBR .0, 0.00200 = C(122) TO C(121) 
VIBR .0, 0.00500 = CU(55) TO N(123) 
VIBR .0, 0.00500 = C(121) TO N(123) 
VIBR .0, 0.00500 = C(121) TO CU(55) 
VIBR .0, 0.00500 = C(122) TO N(20) 
VIBR .0, 0.00500 = CU(55) TO N(20) 
VIBR .0, 0.00500 = CU(55) TO C(122) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.04000 = C(1) TO C(6) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(2) TO C(38) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(4) TO C(5) 
U(IJ) .0, 0.04000 = C(5) TO C(6) 
U(IJ) .0, 0.04000 = C(6) TO C(7) 
U(IJ) .0, 0.02000 = C(19) TO N(20) 
U(IJ) .0, 0.02000 = N(20) TO C(21) 
U(IJ) .0, 0.02000 = N(20) TO CU(55) 
U(IJ) .0, 0.02000 = N(20) TO CU(55) 
U(IJ) .0, 0.02000 = N(20) TO C(121) 
U(IJ) .0, 0.02000 = C(21) TO C(22) 
U(IJ) .0, 0.02000 = C(22) TO N(23) 
U(IJ) .0, 0.02000 = N(23) TO C(24) 
U(IJ) .0, 0.02000 = N(23) TO CU(55) 
U(IJ) .0, 0.02000 = C(24) TO C(25) 
U(IJ) .0, 0.02000 = C(24) TO CU(55) 
U(IJ) .0, 0.02000 = C(25) TO N(26) 
U(IJ) .0, 0.02000 = C(25) TO CU(55) 
U(IJ) .0, 0.02000 = N(26) TO C(27) 
U(IJ) .0, 0.02000 = N(26) TO CU(55) 
U(IJ) .0, 0.02000 = C(124) TO C(125) 
U(IJ) .0, 0.02000 = C(124) TO N(123) 
U(IJ) .0, 0.02000 = C(125) TO N(126) 
U(IJ) .0, 0.02000 = N(126) TO C(127) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
-2 0 16 x .
2 2 1 x .
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile, di-isopropyl ether'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_macrocycle-3-Cu-2ClO4
_database_code_depnum_ccdc_archive 'CCDC 1560763'
_audit_update_record             
;
2017-07-06 deposited with the CCDC.
2017-09-12 downloaded from the CCDC.
;
#==============================================================================
# start Validation Reply Form
_vrf_PLAT414_3.CuClO42           
;
PROBLEM: Short Intra D-H..H-X       H201   ..  H212    ..       1.83 Ang.  
RESPONSE: This close contact is between CH and NH hydrogen atoms of the 
macrocycle tris-amine group. The conformaton of the tris-amine group is
presumably restricted as a result of coordination to the copper(II) cation
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
The crystals were small and weakly diffracting and, desite the use of synchrotron radiation,
the data which were obtained were still weak. Upon structure solution it became apparent that there was
some disorder in the macrocycle and in the two perchlorate counteranions. This was modelled accordingly.
Where appropriate, restraints to bond lengths and angles were used to ensure a physically reasonable model,
and thermal and vibrational restraints were applied to maintain sensible anisoptropic displacement ellipsoids.
C-H hydrogen atoms were  visible in the Fourier difference map but were initially positioned geometrically and
refined with restraints on bond lengths and angles, after which the positions were used as the basis for a riding
model. The N-H hydrogen atoms were visible in the Fourier difference map and were refined with 
restraints on bond lengths and angles.
;

_cell_length_a                   9.04330(10)
_cell_length_b                   23.7126(4)
_cell_length_c                   39.6408(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8500.6(2)

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a '
_symmetry_space_group_name_Hall  '-P 2ac 2ab'

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0070 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cu 0.2710 1.2020 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126
1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1250 0.1500 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'

_cell_formula_units_Z            8

_chemical_formula_sum            'C36.37 H46.56 Cl2.00 Cu1 N8.19 O12.00'
_chemical_formula_moiety         'C30 H37 Cu N5 O4, 2(Cl O4), 3.19(C2 H3 N)'
_chemical_compound_source        synthesised
_chemical_formula_weight         924.86

_cell_measurement_reflns_used    27894
_cell_measurement_theta_min      1
_cell_measurement_theta_max      26
_cell_measurement_temperature    100

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_min          0.02
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_max          0.06

_exptl_crystal_density_diffrn    1.445
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3848.606
_exptl_absorpt_coefficient_mu    0.709

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_T_max  1.00
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_device       'CrystalLogic Kappa (3 circle)'
_diffrn_radiation_monochromator  Synchrotron
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_measurement_method       'profile data from ω-scans'

_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      100
_diffrn_reflns_number            104310
_reflns_number_total             8969
_diffrn_reflns_av_R_equivalents  0.091

_diffrn_reflns_theta_min         1.940
_diffrn_reflns_theta_max         26.436
_diffrn_measured_fraction_theta_max 0.933

_diffrn_reflns_theta_full        25.115
_diffrn_measured_fraction_theta_full 0.963

_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_limit_l_max       50
_reflns_limit_h_min              0
_reflns_limit_h_max              11
_reflns_limit_k_min              0
_reflns_limit_k_max              30
_reflns_limit_l_min              0
_reflns_limit_l_max              50

_oxford_diffrn_Wilson_B_factor   3.36
_oxford_diffrn_Wilson_scale      0.20

_atom_sites_solution_primary     Other
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.46
_refine_diff_density_max         1.47

_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         7312
_refine_ls_number_restraints     1027
_refine_ls_number_parameters     692
_oxford_refine_ls_R_factor_ref   0.0939
_refine_ls_wR_factor_ref         0.2451
_refine_ls_goodness_of_fit_ref   0.9979
_refine_ls_shift/su_max          0.0007581
_refine_ls_shift/su_mean         0.0000439

_oxford_reflns_number_all        7312
_refine_ls_R_factor_all          0.0939
_refine_ls_wR_factor_all         0.2451

_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                6419
_refine_ls_R_factor_gt           0.0872
_refine_ls_wR_factor_gt          0.2401

_chemical_absolute_configuration .

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr

_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.503E+04 0.843E+04 0.539E+04 0.241E+04 581. 
;

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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 0.3948(4) 0.34784(17) 0.29099(11) 0.0338 1.0000 Uani . . . . . .
C2 C 0.4705(4) 0.34476(16) 0.26060(11) 0.0328 1.0000 Uani . . . . . .
C3 C 0.5392(5) 0.29447(17) 0.25147(12) 0.0400 1.0000 Uani . . . . . .
C4 C 0.5269(5) 0.24807(19) 0.27194(13) 0.0456 1.0000 Uani . . . . . .
C5 C 0.4486(5) 0.25076(18) 0.30216(12) 0.0404 1.0000 Uani . . . . . .
C6 C 0.3808(5) 0.30120(19) 0.31147(11) 0.0369 1.0000 Uani D . . . . .
C7 C 0.2928(5) 0.30312(18) 0.34344(10) 0.0386 1.0000 Uani D . . . . .
O8 O 0.3199(4) 0.27183(15) 0.36746(8) 0.0513 1.0000 Uani . . . . . .
N9 N 0.1821(4) 0.34127(16) 0.34380(10) 0.0407 1.0000 Uani D U . . . .
C10 C 0.0861(5) 0.35046(19) 0.37243(11) 0.0442 1.0000 Uani D U . . . .
Cl47 Cl 0.99370(17) 0.58980(6) 0.36506(4) 0.0476 0.773(5) Uani D . P 4 1 .
O48 O 0.8916(4) 0.5870(2) 0.39237(9) 0.0783 1.0000 Uani D U . . . .
O49 O 0.9340(5) 0.62371(15) 0.33879(7) 0.0717 1.0000 Uani D . . . . .
O50 O 1.0392(5) 0.53652(12) 0.35225(11) 0.0766 1.0000 Uani D . . . . .
O51 O 1.1236(4) 0.6137(3) 0.37946(16) 0.0775 0.773(5) Uani D . P 4 1 .
Cl52 Cl 0.1451(3) 0.65974(13) 0.52854(7) 0.0519 0.713(7) Uani D . P 5 1 .
O54 O 0.1107(7) 0.71697(15) 0.52102(14) 0.0530 0.713(7) Uani D . P 5 1 .
N20 N 0.6597(5) 0.60865(19) 0.45222(8) 0.0576 1.0000 Uani D U . . . .
C21 C 0.7443(5) 0.64498(19) 0.47565(8) 0.0649 1.0000 Uani D U . . . .
C22 C 0.8606(4) 0.6755(2) 0.45653(10) 0.0632 1.0000 Uani D U . . . .
N23 N 0.7831(3) 0.70617(16) 0.42976(8) 0.0493 1.0000 Uani D U . . . .
C24 C 0.8800(3) 0.73240(18) 0.40456(9) 0.0512 1.0000 Uani D U . . . .
C25 C 0.7810(4) 0.75045(13) 0.37637(9) 0.0466 1.0000 Uani D U . . . .
N26 N 0.6914(4) 0.70154(11) 0.36503(8) 0.0423 1.0000 Uani D U . . . .
C27 C 0.5710(4) 0.72191(16) 0.34250(10) 0.0474 1.0000 Uani D U . . . .
C28 C 0.5130(3) 0.67691(15) 0.31929(9) 0.0424 1.0000 Uani D U . . . .
C29 C 0.3694(4) 0.6578(2) 0.32195(10) 0.0507 1.0000 Uani D U . . . .
C30 C 0.3168(3) 0.61500(19) 0.30138(11) 0.0470 1.0000 Uani D U . . . .
C31 C 0.4097(3) 0.59030(14) 0.27789(8) 0.0347 1.0000 Uani D U . . . .
C32 C 0.5519(4) 0.61037(16) 0.27406(8) 0.0379 1.0000 Uani D U . . . .
C33 C 0.6027(3) 0.65319(17) 0.29474(10) 0.0427 1.0000 Uani D U . . . .
O34 O 0.3525(2) 0.54602(12) 0.25975(7) 0.0363 1.0000 Uani D . . . . .
C35 C 0.4335(3) 0.52742(16) 0.23056(9) 0.0348 1.0000 Uani D . . . . .
C36 C 0.3522(4) 0.47802(18) 0.21606(10) 0.0367 1.0000 Uani D . . . . .
N37 N 0.3599(4) 0.42856(15) 0.23773(9) 0.0341 1.0000 Uani . . . . . .
C38 C 0.4783(4) 0.39480(18) 0.23754(10) 0.0332 1.0000 Uani . . . . . .
O39 O 0.5862(3) 0.40325(13) 0.21909(8) 0.0400 1.0000 Uani . . . . . .
Cu40 Cu 0.64113(7) 0.65393(3) 0.407292(15) 0.0469 1.0000 Uani . U . . . .
N41 N 0.5480(5) 0.58994(19) 0.38177(10) 0.0497 1.0000 Uani . . . . . .
C42 C 0.4959(7) 0.5542(2) 0.36696(12) 0.0548 1.0000 Uani . . . . . .
C43 C 0.4262(8) 0.5077(3) 0.34877(15) 0.0684 1.0000 Uani . . . . . .
N44 N 0.4362(5) 0.6977(2) 0.42070(11) 0.0557 1.0000 Uani . . . . . .
C45 C 0.3505(6) 0.7276(3) 0.43260(13) 0.0519 1.0000 Uani . . . . . .
C46 C 0.2489(6) 0.7668(3) 0.44744(12) 0.0570 1.0000 Uani . . . . . .
C60 C 0.0504(8) 0.4926(3) 0.51373(19) 0.0774 1.0000 Uani . . . . . .
N61 N 0.1130(14) 0.4861(5) 0.5376(3) 0.0805 0.5000 Uani . . . 3 1 .
C17 C 0.3189(14) 0.5378(6) 0.4428(5) 0.0574 0.65(4) Uani D U P 1 1 .
C18 C 0.2477(11) 0.4932(5) 0.4276(5) 0.0521 0.65(4) Uani D U P 1 1 .
C19 C 0.5384(17) 0.5812(8) 0.4709(2) 0.0863 0.65(4) Uani D U P 1 1 .
C16 C 0.4639(15) 0.5334(6) 0.4534(4) 0.0710 0.65(4) Uani D U P 1 1 .
C13 C 0.3229(13) 0.4431(5) 0.4221(4) 0.0518 0.65(4) Uani D U P 1 1 .
C14 C 0.4663(14) 0.4376(5) 0.4332(5) 0.0568 0.65(4) Uani D U P 1 1 .
C15 C 0.5361(15) 0.4826(6) 0.4485(5) 0.0642 0.65(4) Uani D U P 1 1 .
C58 C 0.2784(12) 0.5877(5) 0.6391(3) 0.0927 0.685(14) Uani D . P 2 1 .
N59 N 0.3020(14) 0.6197(5) 0.6606(3) 0.1315 0.685(14) Uani D . P 2 1 .
O53 O 0.2235(10) 0.6558(3) 0.55956(15) 0.0959 0.713(7) Uani D . P 5 1 .
C57 C 0.2288(10) 0.5486(5) 0.6125(3) 0.0879 0.685(14) Uani D . P 2 1 .
C113 C 0.314(3) 0.4485(7) 0.4218(7) 0.0501 0.35(4) Uani D U P 1 2 .
C118 C 0.249(2) 0.5013(8) 0.4200(7) 0.0484 0.35(4) Uani D U P 1 2 .
C117 C 0.314(2) 0.5466(7) 0.4360(7) 0.0466 0.35(4) Uani D U P 1 2 .
C119 C 0.5213(14) 0.5906(8) 0.4688(2) 0.0496 0.35(4) Uani D U P 1 2 .
C116 C 0.4460(19) 0.5407(7) 0.4534(5) 0.0474 0.35(4) Uani D U P 1 2 .
C115 C 0.508(2) 0.4874(7) 0.4555(6) 0.0466 0.35(4) Uani D U P 1 2 .
H11 H 0.3527 0.3818 0.2975 0.0367 1.0000 Uiso R . . . . .
H31 H 0.5939 0.2926 0.2315 0.0457 1.0000 Uiso R . . . . .
H41 H 0.5715 0.2147 0.2659 0.0499 1.0000 Uiso R . . . . .
H51 H 0.4387 0.2194 0.3156 0.0478 1.0000 Uiso R . . . . .
H211 H 0.6814 0.6697 0.4886 0.0960 1.0000 Uiso R . . . . .
H212 H 0.7998 0.6144 0.4848 0.0962 1.0000 Uiso R . . . . .
H222 H 0.8730 0.7088 0.4696 0.0929 1.0000 Uiso R . . . . .
H221 H 0.9436 0.6528 0.4497 0.0929 1.0000 Uiso R . . . . .
H241 H 0.8915 0.7662 0.4175 0.0771 1.0000 Uiso R . . . . .
H242 H 0.9608 0.7089 0.3975 0.0771 1.0000 Uiso R . . . . .
H252 H 0.7146 0.7800 0.3847 0.0549 1.0000 Uiso R . . . . .
H251 H 0.8376 0.7653 0.3577 0.0549 1.0000 Uiso R . . . . .
H271 H 0.4899 0.7364 0.3559 0.0551 1.0000 Uiso R . . . . .
H272 H 0.6105 0.7519 0.3286 0.0548 1.0000 Uiso R . . . . .
H291 H 0.3076 0.6742 0.3379 0.0560 1.0000 Uiso R . . . . .
H301 H 0.2193 0.6030 0.3033 0.0550 1.0000 Uiso R . . . . .
H321 H 0.6149 0.5953 0.2583 0.0423 1.0000 Uiso R . . . . .
H331 H 0.6982 0.6663 0.2922 0.0467 1.0000 Uiso R . . . . .
H351 H 0.4376 0.5581 0.2144 0.0411 1.0000 Uiso R . . . . .
H352 H 0.5316 0.5156 0.2364 0.0411 1.0000 Uiso R . . . . .
H361 H 0.2500 0.4885 0.2136 0.0438 1.0000 Uiso R . . . . .
H362 H 0.3916 0.4688 0.1942 0.0440 1.0000 Uiso R . . . . .
H432 H 0.4650 0.5054 0.3264 0.0971 1.0000 Uiso R . . . . .
H431 H 0.3208 0.5143 0.3475 0.0972 1.0000 Uiso R . . . . .
H433 H 0.4428 0.4720 0.3595 0.0970 1.0000 Uiso R . . . . .
H462 H 0.1894 0.7477 0.4638 0.0839 1.0000 Uiso R . . . . .
H461 H 0.3031 0.7969 0.4582 0.0838 1.0000 Uiso R . . . . .
H463 H 0.1877 0.7825 0.4303 0.0838 1.0000 Uiso R . . . . .
H171 H 0.2718 0.5723 0.4450 0.0690 0.65(4) Uiso R . P 1 1 .
H181 H 0.1547 0.4988 0.4183 0.0630 0.65(4) Uiso R . P 1 1 .
H191 H 0.5854 0.5662 0.4910 0.0850 0.65(4) Uiso R . P 1 1 .
H192 H 0.4626 0.6083 0.4771 0.0850 0.65(4) Uiso R . P 1 1 .
H141 H 0.5099 0.4020 0.4330 0.0669 0.65(4) Uiso R . P 1 1 .
H151 H 0.6315 0.4785 0.4566 0.0700 0.65(4) Uiso R . P 1 1 .
H572 H 0.3135 0.5300 0.6031 0.1471 0.685(14) Uiso R . P 2 1 .
H571 H 0.1651 0.5208 0.6228 0.1470 0.685(14) Uiso R . P 2 1 .
H573 H 0.1764 0.5678 0.5947 0.1470 0.685(14) Uiso R . P 2 1 .
H1181 H 0.1522 0.5046 0.4124 0.0560 0.35(4) Uiso R . P 1 2 .
H1171 H 0.2652 0.5810 0.4375 0.0519 0.35(4) Uiso R . P 1 2 .
H1192 H 0.5408 0.5817 0.4924 0.0620 0.35(4) Uiso R . P 1 2 .
H1191 H 0.4544 0.6226 0.4673 0.0619 0.35(4) Uiso R . P 1 2 .
H1151 H 0.5998 0.4836 0.4654 0.0640 0.35(4) Uiso R . P 1 2 .
H371 H 0.2998 0.4259 0.2540 0.0399 1.0000 Uiso R . . . . .
H231 H 0.7301 0.7332 0.4390 0.0742 1.0000 Uiso R . . . . .
H261 H 0.7501 0.6805 0.3523 0.0640 1.0000 Uiso R . . . . .
H91 H 0.1580 0.3565 0.3251 0.0459 1.0000 Uiso R . . . . .
O112 O 0.2685(15) 0.4048(8) 0.4010(7) 0.0470 0.35(4) Uani D U P 1 2 .
O12 O 0.2599(11) 0.3965(5) 0.4075(4) 0.0472 0.65(4) Uani D U P 1 1 .
C111 C 0.1221(19) 0.4079(6) 0.3869(9) 0.0441 0.35(4) Uani D U P 1 2 .
C11 C 0.1173(11) 0.4031(4) 0.3925(5) 0.0465 0.65(4) Uani D U P 1 1 .
H1111 H 0.0402 0.4193 0.4010 0.0690 0.35(4) Uiso R . P 1 2 .
H1112 H 0.1382 0.4363 0.3695 0.0688 0.35(4) Uiso R . P 1 2 .
H111 H 0.0537 0.4071 0.4119 0.0449 0.65(4) Uiso R . P 1 1 .
H112 H 0.1065 0.4358 0.3778 0.0449 0.65(4) Uiso R . P 1 1 .
C114 C 0.441(3) 0.4413(7) 0.4405(6) 0.0507 0.35(4) Uani D U P 1 2 .
H1141 H 0.4929 0.4077 0.4380 0.0600 0.35(4) Uiso R . P 1 2 .
H201 H 0.7295 0.5802 0.4466 0.0686 0.65(4) Uiso R . P 1 1 .
H202 H 0.7167 0.5754 0.4479 0.0686 0.35(4) Uiso R . P 1 2 .
H101 H 0.0953 0.3196 0.3875 0.0528 0.65(4) Uiso R . P 1 1 .
H102 H -0.0133 0.3531 0.3648 0.0528 0.65(4) Uiso R . P 1 1 .
H103 H 0.1024 0.3218 0.3886 0.0528 0.35(4) Uiso R . P 1 2 .
H104 H -0.0140 0.3497 0.3652 0.0528 0.35(4) Uiso R . P 1 2 .
Cl147 Cl 0.9174(5) 0.57326(14) 0.35795(8) 0.0793 0.227(5) Uani D . P 4 2 .
O151 O 0.7914(12) 0.5419(6) 0.3474(4) 0.1069 0.227(5) Uani D . P 4 2 .
H601 H 0.0104 0.5025 0.5351 0.0941 0.5000 Uiso R . . 3 2 .
H602 H 0.1404 0.5124 0.5102 0.0941 0.5000 Uiso R . . 3 2 .
H603 H 0.0688 0.4532 0.5131 0.0941 0.5000 Uiso R . . 3 2 .
O155 O 0.3478(12) 0.6810(6) 0.5262(4) 0.0795 0.287(7) Uani D . P 5 2 .
O154 O 0.1005(18) 0.7058(7) 0.5354(5) 0.0900 0.287(7) Uani D . P 5 2 .
O153 O 0.190(2) 0.6176(7) 0.5536(4) 0.1033 0.287(7) Uani D . P 5 2 .
O55 O 0.0109(5) 0.6301(3) 0.53470(19) 0.0843 0.713(7) Uani D . P 5 1 .
O56 O 0.2139(11) 0.6319(5) 0.5009(2) 0.1058 0.713(7) Uani D . P 5 1 .
O156 O 0.1586(16) 0.6377(8) 0.4964(4) 0.0712 0.287(7) Uani D . P 5 2 .
Cl152 Cl 0.1998(9) 0.6604(4) 0.5282(2) 0.0702 0.287(7) Uani D . P 5 2 .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.63(4)

loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . C2 . 1.388(6) yes
C1 . C6 . 1.378(6) yes
C1 . H11 . 0.927 no
C2 . C3 . 1.392(6) yes
C2 . C38 . 1.499(6) yes
C3 . C4 . 1.372(7) yes
C3 . H31 . 0.934 no
C4 . C5 . 1.393(7) yes
C4 . H41 . 0.919 no
C5 . C6 . 1.394(6) yes
C5 . H51 . 0.920 no
C6 . C7 . 1.497(6) yes
C7 . O8 . 1.232(5) yes
C7 . N9 . 1.349(6) yes
N9 . C10 . 1.445(6) yes
N9 . H91 . 0.853 no
C10 . C11 . 1.505(7) yes
C10 . H101 . 0.950 no
C10 . H102 . 0.950 no
C10 . C111 . 1.514(8) yes
C10 . H103 . 0.946 no
C10 . H104 . 0.950 no
Cl47 . O48 . 1.4243(9) yes
Cl47 . O49 . 1.4222(9) yes
Cl47 . O50 . 1.4225(9) yes
Cl47 . O51 . 1.4236(10) yes
O48 . Cu40 . 2.829(4) yes
O48 . Cu40 . 2.829(4) yes
O48 . Cl147 . 1.4221(10) yes
O49 . Cl147 . 1.4250(10) yes
O50 . Cl147 . 1.4227(10) yes
Cl52 . O54 . 1.4237(10) yes
Cl52 . O53 . 1.4229(10) yes
Cl52 . O55 . 1.4233(10) yes
Cl52 . O56 . 1.4229(10) yes
N20 . C21 . 1.480(4) yes
N20 . Cu40 . 2.086(4) yes
N20 . C19 . 1.474(6) yes
N20 . H201 . 0.950 no
N20 . C21 . 1.480(4) yes
N20 . Cu40 . 2.086(4) yes
N20 . C119 . 1.478(6) yes
N20 . H202 . 0.957 no
C21 . C22 . 1.485(4) yes
C21 . Cu40 . 2.873(3) yes
C21 . H211 . 0.964 no
C21 . H212 . 0.953 no
C22 . N23 . 1.465(4) yes
C22 . Cu40 . 2.830(3) yes
C22 . H222 . 0.952 no
C22 . H221 . 0.962 no
N23 . C24 . 1.467(4) yes
N23 . Cu40 . 1.994(4) yes
N23 . H231 . 0.880 no
C24 . C25 . 1.495(3) yes
C24 . Cu40 . 2.853(3) yes
C24 . H241 . 0.957 no
C24 . H242 . 0.959 no
C25 . N26 . 1.485(4) yes
C25 . H252 . 0.980 no
C25 . H251 . 0.968 no
N26 . C27 . 1.489(4) yes
N26 . Cu40 . 2.071(3) yes
N26 . H261 . 0.887 no
C27 . C28 . 1.503(4) yes
C27 . H271 . 0.969 no
C27 . H272 . 0.967 no
C28 . C29 . 1.380(4) yes
C28 . C33 . 1.386(4) yes
C29 . C30 . 1.386(4) yes
C29 . H291 . 0.928 no
C30 . C31 . 1.384(4) yes
C30 . H301 . 0.930 no
C31 . C32 . 1.379(4) yes
C31 . O34 . 1.374(3) yes
C32 . C33 . 1.384(4) yes
C32 . H321 . 0.919 no
C33 . H331 . 0.924 no
O34 . C35 . 1.438(4) yes
C35 . C36 . 1.498(5) yes
C35 . H351 . 0.970 no
C35 . H352 . 0.959 no
C36 . N37 . 1.456(5) yes
C36 . H361 . 0.962 no
C36 . H362 . 0.960 no
N37 . C38 . 1.337(5) yes
N37 . H371 . 0.845 no
C38 . O39 . 1.236(5) yes
Cu40 . N41 . 2.009(4) yes
Cu40 . N44 . 2.190(5) yes
N41 . C42 . 1.133(7) yes
C42 . C43 . 1.461(8) yes
C43 . H432 . 0.956 no
C43 . H431 . 0.967 no
C43 . H433 . 0.960 no
N44 . C45 . 1.152(7) yes
C45 . C46 . 1.433(8) yes
C46 . H462 . 0.957 no
C46 . H461 . 0.965 no
C46 . H463 . 0.952 no
C60 . C60 2_566 1.462(13) yes
C60 . N61 . 1.114(13) yes
C60 . H601 . 0.950 no
C60 . H602 . 0.950 no
C60 . H603 . 0.950 no
C17 . C18 . 1.378(5) yes
C17 . C16 . 1.380(5) yes
C17 . H171 . 0.927 no
C18 . C13 . 1.386(5) yes
C18 . H181 . 0.928 no
C19 . C16 . 1.489(5) yes
C19 . H191 . 0.973 no
C19 . H192 . 0.972 no
C16 . C15 . 1.383(5) yes
C13 . C14 . 1.376(5) yes
C13 . O12 . 1.371(6) yes
C14 . C15 . 1.381(5) yes
C14 . H141 . 0.930 no
C15 . H151 . 0.927 no
C58 . N59 . 1.158(13) yes
C58 . C57 . 1.475(13) yes
C57 . H572 . 0.959 no
C57 . H571 . 0.967 no
C57 . H573 . 0.963 no
C113 . C118 . 1.385(5) yes
C113 . O112 . 1.385(8) yes
C113 . C114 . 1.379(5) yes
C118 . C117 . 1.383(5) yes
C118 . H1181 . 0.927 no
C117 . C116 . 1.382(5) yes
C117 . H1171 . 0.929 no
C119 . C116 . 1.496(6) yes
C119 . H1192 . 0.974 no
C119 . H1191 . 0.973 no
C116 . C115 . 1.383(5) yes
C115 . H1151 . 0.925 no
C115 . C114 . 1.385(5) yes
O112 . C111 . 1.439(9) yes
O12 . C11 . 1.428(7) yes
C111 . H1111 . 0.965 no
C111 . H1112 . 0.974 no
C11 . H111 . 0.966 no
C11 . H112 . 0.974 no
C114 . H1141 . 0.931 no
Cl147 . O151 . 1.4233(10) yes
O155 . Cl152 . 1.426(9) yes
O154 . Cl152 . 1.430(9) yes
O153 . Cl152 . 1.433(9) yes
O156 . Cl152 . 1.423(9) yes

loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 . C1 . C6 . 121.0(4) yes
C2 . C1 . H11 . 119.4 no
C6 . C1 . H11 . 119.6 no
C1 . C2 . C3 . 119.4(4) yes
C1 . C2 . C38 . 120.7(4) yes
C3 . C2 . C38 . 119.9(4) yes
C2 . C3 . C4 . 119.8(4) yes
C2 . C3 . H31 . 119.9 no
C4 . C3 . H31 . 120.3 no
C3 . C4 . C5 . 120.9(4) yes
C3 . C4 . H41 . 120.1 no
C5 . C4 . H41 . 119.1 no
C4 . C5 . C6 . 119.4(4) yes
C4 . C5 . H51 . 120.7 no
C6 . C5 . H51 . 119.9 no
C5 . C6 . C1 . 119.5(4) yes
C5 . C6 . C7 . 118.9(4) yes
C1 . C6 . C7 . 121.6(4) yes
C6 . C7 . O8 . 122.0(4) yes
C6 . C7 . N9 . 115.1(4) yes
O8 . C7 . N9 . 122.9(4) yes
C7 . N9 . C10 . 123.7(4) yes
C7 . N9 . H91 . 117.7 no
C10 . N9 . H91 . 117.7 no
N9 . C10 . C11 . 115.2(8) yes
N9 . C10 . H101 . 109.0 no
C11 . C10 . H101 . 106.9 no
N9 . C10 . H102 . 109.2 no
C11 . C10 . H102 . 106.9 no
H101 . C10 . H102 . 109.5 no
N9 . C10 . C111 . 107.7(14) yes
N9 . C10 . H103 . 109.2 no
C111 . C10 . H103 . 110.9 no
N9 . C10 . H104 . 109.4 no
C111 . C10 . H104 . 109.7 no
H103 . C10 . H104 . 109.8 no
O48 . Cl47 . O49 . 109.7(3) yes
O48 . Cl47 . O50 . 114.7(3) yes
O49 . Cl47 . O50 . 110.5(3) yes
O48 . Cl47 . O51 . 104.4(3) yes
O49 . Cl47 . O51 . 112.4(3) yes
O50 . Cl47 . O51 . 105.0(3) yes
Cl47 . O48 . Cu40 . 130.7(3) yes
Cu40 . O48 . Cl147 . 117.4(3) yes
O54 . Cl52 . O53 . 110.6(4) yes
O54 . Cl52 . O55 . 108.7(5) yes
O53 . Cl52 . O55 . 104.2(5) yes
O54 . Cl52 . O56 . 112.2(6) yes
O53 . Cl52 . O56 . 114.6(7) yes
O55 . Cl52 . O56 . 106.0(6) yes
C21 . N20 . Cu40 . 106.1(3) yes
C21 . N20 . C19 . 109.07(7) yes
Cu40 . N20 . C19 . 126.6(8) yes
C21 . N20 . H201 . 102.5 no
Cu40 . N20 . H201 . 102.7 no
C19 . N20 . H201 . 107.3 no
C21 . N20 . Cu40 . 106.1(3) yes
C21 . N20 . C119 . 109.09(7) yes
Cu40 . N20 . C119 . 117.4(8) yes
C21 . N20 . H202 . 108.2 no
Cu40 . N20 . H202 . 108.4 no
C119 . N20 . H202 . 107.3 no
N20 . C21 . C22 . 109.24(5) yes
N20 . C21 . Cu40 . 44.23(18) yes
C22 . C21 . Cu40 . 73.30(8) yes
N20 . C21 . H211 . 112.6 no
C22 . C21 . H211 . 113.1 no
Cu40 . C21 . H211 . 105.4 no
N20 . C21 . H212 . 93.9 no
C22 . C21 . H212 . 101.0 no
Cu40 . C21 . H212 . 125.8 no
H211 . C21 . H212 . 124.8 no
C21 . C22 . N23 . 105.81(5) yes
C21 . C22 . Cu40 . 76.53(8) yes
N23 . C22 . Cu40 . 41.82(17) yes
C21 . C22 . H222 . 102.1 no
N23 . C22 . H222 . 92.2 no
Cu40 . C22 . H222 . 127.5 no
C21 . C22 . H221 . 115.0 no
N23 . C22 . H221 . 116.7 no
Cu40 . C22 . H221 . 104.7 no
H222 . C22 . H221 . 121.7 no
C22 . N23 . C24 . 114.68(5) yes
C22 . N23 . Cu40 . 108.8(3) yes
C24 . N23 . Cu40 . 110.1(2) yes
C22 . N23 . H231 . 108.6 no
C24 . N23 . H231 . 107.6 no
Cu40 . N23 . H231 . 106.7 no
N23 . C24 . C25 . 105.80(5) yes
N23 . C24 . Cu40 . 41.01(16) yes
C25 . C24 . Cu40 . 76.20(8) yes
N23 . C24 . H241 . 93.1 no
C25 . C24 . H241 . 103.1 no
Cu40 . C24 . H241 . 127.4 no
N23 . C24 . H242 . 114.0 no
C25 . C24 . H242 . 113.8 no
Cu40 . C24 . H242 . 102.1 no
H241 . C24 . H242 . 124.0 no
C24 . C25 . N26 . 109.25(5) yes
C24 . C25 . H252 . 108.7 no
N26 . C25 . H252 . 109.1 no
C24 . C25 . H251 . 111.1 no
N26 . C25 . H251 . 110.0 no
H252 . C25 . H251 . 108.7 no
C25 . N26 . C27 . 109.10(5) yes
C25 . N26 . Cu40 . 107.5(2) yes
C27 . N26 . Cu40 . 120.1(2) yes
C25 . N26 . H261 . 106.6 no
C27 . N26 . H261 . 106.2 no
Cu40 . N26 . H261 . 106.5 no
N26 . C27 . C28 . 113.1(3) yes
N26 . C27 . H271 . 109.8 no
C28 . C27 . H271 . 108.9 no
N26 . C27 . H272 . 108.0 no
C28 . C27 . H272 . 107.7 no
H271 . C27 . H272 . 109.4 no
C27 . C28 . C29 . 120.98(5) yes
C27 . C28 . C33 . 120.91(5) yes
C29 . C28 . C33 . 118.11(5) yes
C28 . C29 . C30 . 121.23(6) yes
C28 . C29 . H291 . 118.7 no
C30 . C29 . H291 . 120.1 no
C29 . C30 . C31 . 119.83(6) yes
C29 . C30 . H301 . 120.1 no
C31 . C30 . H301 . 120.1 no
C30 . C31 . C32 . 119.59(6) yes
C30 . C31 . O34 . 116.58(16) yes
C32 . C31 . O34 . 123.84(16) yes
C31 . C32 . C33 . 119.84(6) yes
C31 . C32 . H321 . 121.3 no
C33 . C32 . H321 . 118.9 no
C28 . C33 . C32 . 121.31(6) yes
C28 . C33 . H331 . 119.2 no
C32 . C33 . H331 . 119.5 no
C31 . O34 . C35 . 117.64(9) yes
O34 . C35 . C36 . 107.37(9) yes
O34 . C35 . H351 . 108.7 no
C36 . C35 . H351 . 110.6 no
O34 . C35 . H352 . 111.5 no
C36 . C35 . H352 . 108.5 no
H351 . C35 . H352 . 110.1 no
C35 . C36 . N37 . 112.3(3) yes
C35 . C36 . H361 . 108.0 no
N37 . C36 . H361 . 108.4 no
C35 . C36 . H362 . 109.9 no
N37 . C36 . H362 . 109.3 no
H361 . C36 . H362 . 108.8 no
C36 . N37 . C38 . 121.2(3) yes
C36 . N37 . H371 . 118.5 no
C38 . N37 . H371 . 118.4 no
C2 . C38 . N37 . 115.6(4) yes
C2 . C38 . O39 . 121.8(4) yes
N37 . C38 . O39 . 122.6(4) yes
N20 . Cu40 . N26 . 162.47(14) yes
N20 . Cu40 . N23 . 83.49(13) yes
N26 . Cu40 . N23 . 83.19(12) yes
N20 . Cu40 . O48 . 79.93(15) yes
N26 . Cu40 . O48 . 87.77(12) yes
N23 . Cu40 . O48 . 85.79(14) yes
N20 . Cu40 . C22 . 56.49(11) yes
N26 . Cu40 . C22 . 107.79(11) yes
N23 . Cu40 . C22 . 29.34(11) yes
O48 . Cu40 . C22 . 71.57(14) yes
N20 . Cu40 . C24 . 107.88(12) yes
N26 . Cu40 . C24 . 56.47(10) yes
N23 . Cu40 . C24 . 28.88(10) yes
O48 . Cu40 . C24 . 75.63(12) yes
C22 . Cu40 . C24 . 51.49(8) yes
N20 . Cu40 . C21 . 29.65(11) yes
N26 . Cu40 . C21 . 137.05(11) yes
N23 . Cu40 . C21 . 54.25(10) yes
O48 . Cu40 . C21 . 84.02(13) yes
C22 . Cu40 . C21 . 30.17(8) yes
N20 . Cu40 . N41 . 94.30(15) yes
N26 . Cu40 . N41 . 95.52(14) yes
N23 . Cu40 . N41 . 164.62(16) yes
O48 . Cu40 . N41 . 78.84(16) yes
C22 . Cu40 . N41 . 141.05(16) yes
N20 . Cu40 . N44 . 96.01(18) yes
N26 . Cu40 . N44 . 97.11(16) yes
N23 . Cu40 . N44 . 98.17(15) yes
O48 . Cu40 . N44 . 174.02(15) yes
C22 . Cu40 . N44 . 109.92(15) yes
C24 . Cu40 . C21 . 80.69(10) yes
C24 . Cu40 . N41 . 142.27(15) yes
C21 . Cu40 . N41 . 123.73(15) yes
C24 . Cu40 . N44 . 109.95(15) yes
C21 . Cu40 . N44 . 94.63(15) yes
N41 . Cu40 . N44 . 97.20(17) yes
Cu40 . N41 . C42 . 179.0(4) yes
N41 . C42 . C43 . 178.3(6) yes
C42 . C43 . H432 . 110.0 no
C42 . C43 . H431 . 109.3 no
H432 . C43 . H431 . 108.9 no
C42 . C43 . H433 . 112.3 no
H432 . C43 . H433 . 107.8 no
H431 . C43 . H433 . 108.6 no
Cu40 . N44 . C45 . 163.9(4) yes
N44 . C45 . C46 . 177.4(6) yes
C45 . C46 . H462 . 109.4 no
C45 . C46 . H461 . 109.6 no
H462 . C46 . H461 . 109.6 no
C45 . C46 . H463 . 109.5 no
H462 . C46 . H463 . 110.0 no
H461 . C46 . H463 . 108.8 no
C60 2_566 C60 . N61 . 169.3(13) yes
H601 . C60 . H602 . 109.5 no
H601 . C60 . H603 . 109.5 no
H602 . C60 . H603 . 109.5 no
C18 . C17 . C16 . 121.28(6) yes
C18 . C17 . H171 . 120.2 no
C16 . C17 . H171 . 118.4 no
C17 . C18 . C13 . 119.82(6) yes
C17 . C18 . H181 . 119.2 no
C13 . C18 . H181 . 120.3 no
N20 . C19 . C16 . 116.0(6) yes
N20 . C19 . H191 . 104.4 no
C16 . C19 . H191 . 107.6 no
N20 . C19 . H192 . 111.1 no
C16 . C19 . H192 . 107.6 no
H191 . C19 . H192 . 109.9 no
C19 . C16 . C17 . 120.91(6) yes
C19 . C16 . C15 . 120.91(6) yes
C17 . C16 . C15 . 118.12(6) yes
C18 . C13 . C14 . 119.58(6) yes
C18 . C13 . O12 . 123.5(4) yes
C14 . C13 . O12 . 116.8(4) yes
C13 . C14 . C15 . 119.84(6) yes
C13 . C14 . H141 . 118.9 no
C15 . C14 . H141 . 120.7 no
C16 . C15 . C14 . 121.30(6) yes
C16 . C15 . H151 . 119.0 no
C14 . C15 . H151 . 119.7 no
N59 . C58 . C57 . 172.9(13) yes
C58 . C57 . H572 . 108.9 no
C58 . C57 . H571 . 107.8 no
H572 . C57 . H571 . 109.0 no
C58 . C57 . H573 . 112.2 no
H572 . C57 . H573 . 109.0 no
H571 . C57 . H573 . 109.8 no
C118 . C113 . O112 . 121.4(7) yes
C118 . C113 . C114 . 119.56(7) yes
O112 . C113 . C114 . 118.2(6) yes
C113 . C118 . C117 . 119.82(7) yes
C113 . C118 . H1181 . 119.4 no
C117 . C118 . H1181 . 119.2 no
C118 . C117 . C116 . 121.27(7) yes
C118 . C117 . H1171 . 120.2 no
C116 . C117 . H1171 . 118.1 no
N20 . C119 . C116 . 115.7(9) yes
N20 . C119 . H1192 . 109.6 no
C116 . C119 . H1192 . 107.6 no
N20 . C119 . H1191 . 105.8 no
C116 . C119 . H1191 . 108.0 no
H1192 . C119 . H1191 . 110.0 no
C119 . C116 . C117 . 120.94(6) yes
C119 . C116 . C115 . 120.93(6) yes
C117 . C116 . C115 . 118.11(6) yes
C116 . C115 . H1151 . 118.6 no
C116 . C115 . C114 . 121.28(7) yes
H1151 . C115 . C114 . 119.9 no
C113 . O112 . C111 . 117.61(10) yes
C13 . O12 . C11 . 117.62(10) yes
C10 . C111 . O112 . 107.40(10) yes
C10 . C111 . H1111 . 107.8 no
O112 . C111 . H1111 . 119.8 no
C10 . C111 . H1112 . 112.6 no
O112 . C111 . H1112 . 100.0 no
H1111 . C111 . H1112 . 109.2 no
C10 . C11 . O12 . 107.38(10) yes
C10 . C11 . H111 . 113.0 no
O12 . C11 . H111 . 102.5 no
C10 . C11 . H112 . 109.0 no
O12 . C11 . H112 . 115.2 no
H111 . C11 . H112 . 109.7 no
C115 . C114 . C113 . 119.82(7) yes
C115 . C114 . H1141 . 120.1 no
C113 . C114 . H1141 . 118.1 no
O49 . Cl147 . O50 . 110.3(3) yes
O49 . Cl147 . O48 . 109.7(3) yes
O50 . Cl147 . O48 . 114.8(3) yes
O49 . Cl147 . O151 . 111.5(7) yes
O50 . Cl147 . O151 . 104.6(7) yes
O48 . Cl147 . O151 . 105.7(7) yes
O153 . Cl152 . O154 . 110.8(8) yes
O153 . Cl152 . O155 . 109.8(7) yes
O154 . Cl152 . O155 . 110.1(8) yes
O153 . Cl152 . O156 . 109.9(8) yes
O154 . Cl152 . O156 . 107.2(7) yes
O155 . Cl152 . O156 . 108.9(7) yes

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C24 . H241 . O53 7_566 136.9 0.957 2.560 3.324(13) yes
C24 . H241 . O155 7_566 148.4 0.957 2.591 3.442(13) yes
C32 . H321 . O34 6_555 153.10 0.919 2.549 3.394(13) yes
C46 . H462 . O54 . 156.67 0.957 2.487 3.387(13) yes
C46 . H461 . O55 7_566 156.49 0.965 2.570 3.477(13) yes
C46 . H463 . O8 8_555 133.30 0.952 2.505 3.233(13) yes
C19 . H192 . O56 . 151.3 0.972 2.502 3.387(13) yes
C119 . H192 . O56 . 157.4 0.752 2.502 3.210(13) yes
C15 . H151 . N61 2_666 150.2 0.927 2.468 3.305(13) yes
C115 . H151 . N61 2_666 149.2 1.140 2.468 3.497(13) yes
C57 . H572 . C14 2_666 134.2 0.959 2.575 3.316(13) yes
C57 . H572 . C15 2_666 144.6 0.959 2.475 3.304(13) yes
C57 . H571 . O50 2_666 168.4 0.967 2.497 3.450(13) yes
C57 . H571 . O151 2_666 131.4 0.967 1.938 2.677(13) yes
C57 . H573 . O53 . 134.8 0.963 2.547 3.297(13) yes
C57 . H573 . O153 . 146.8 0.963 2.016 2.871(13) yes
C119 . H1191 . N44 . 128.7 0.973 2.570 3.268(13) yes
C119 . H1191 . O56 . 124.2 0.973 2.560 3.210(13) yes
N37 . H371 . O39 6_455 157.41 0.845 2.272 3.069(13) yes
N23 . H231 . O54 7_566 159.51 0.880 2.252 3.092(13) yes
N23 . H231 . O154 7_566 175.7 0.880 2.120 2.998(13) yes
N26 . H261 . O49 . 159.04 0.887 2.206 3.050(13) yes
N9 . H91 . O39 6_455 173.37 0.853 2.172 3.021(13) yes
C111 . H111 . O55 2_566 153.5 1.166 2.367 3.451(13) yes
C11 . H111 . O55 2_566 145.4 0.966 2.367 3.210(13) yes
N20 . H201 . N61 2_666 150.1 0.950 2.212 3.072(13) yes
N20 . H202 . N61 2_666 151.4 0.957 2.197 3.072(13) yes

_iucr_refine_instruction_details_constraints 
;
#
# Punched on 10/06/17 at 18:35:02
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
EQUIVALENCE PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
EQUIVALENCE PART(2001,OCC) 
EQUIVALENCE PART(4001,OCC) PART(4002,OCC) 
WEIGHT -1 PART (4002,OCC) 
EQUIVALENCE PART(5001,OCC) PART(5002,OCC) 
WEIGHT -1 PART (5002,OCC) 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE N   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) H   ( 102,X'S) H   ( 103,X'S) H   ( 104,X'S) 
RIDE N   (  20,X'S) H   ( 201,X'S) H   ( 202,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) 
RIDE C   (  22,X'S) H   ( 222,X'S) H   ( 221,X'S) 
RIDE N   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 252,X'S) H   ( 251,X'S) 
RIDE N   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) 
RIDE N   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  43,X'S) H   ( 432,X'S) H   ( 431,X'S) H   ( 433,X'S) 
RIDE C   (  46,X'S) H   ( 462,X'S) H   ( 461,X'S) H   ( 463,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) H   ( 602,X'S) H   ( 603,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) H   ( 192,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  57,X'S) H   ( 572,X'S) H   ( 571,X'S) H   ( 573,X'S) 
RIDE C   ( 118,X'S) H   (1181,X'S) 
RIDE C   ( 117,X'S) H   (1171,X'S) 
RIDE C   ( 119,X'S) H   (1192,X'S) H   (1191,X'S) 
RIDE C   ( 115,X'S) H   (1151,X'S) 
RIDE C   ( 111,X'S) H   (1111,X'S) H   (1112,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) 
RIDE C   ( 114,X'S) H   (1141,X'S) 
RIDE C(14,U'S) C(114,U'S) 
END                                                                             
;

_iucr_refine_instruction_details_restraints 
;
#
# Punched on 10/06/17 at 18:35:02
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
SIMU 0.02 C(6) C(7) N(9) C(10) C(11) O(12) C(13) 
SIMU 0.02 C(6) C(7) N(9) C(10) C(111) O(112) C(113) 
DELU 0.01 C(6) C(7) N(9) C(10) C(11) O(12) C(13) 
DELU 0.01 C(6) C(7) N(9) C(10) C(111) O(112) C(113) 
SIMU 0.02 C(13) C(14) C(15) C(16) C(17) C(18) 
SIMU 0.02 C(113) C(114) C(115) C(116) C(117) C(118) 
DELU 0.01 C(13) C(14) C(15) C(16) C(17) C(18) 
DELU 0.01 C(113) C(114) C(115) C(116) C(117) C(118) 
SAME C(10) C(11) O(12) C(13) AND 
CONT C(10) C(111) O(112) C(113) AND 
CONT C(36) C(35) O(34) C(31) 
ANGLE 120,1 = C(18) TO C(13) TO O(12) 
CONT C(118) TO C(113) TO O(112) 
CONT C(14) TO C(13) TO O(12) 
CONT C(114) TO C(113) TO O(112) 
DISTANCE 1.44, 0.02 = C(57) TO C(58) 
DISTANCE 1.14, 0.02 = C(58) TO N(59) 
SAME C(19) C(16) C(15) C(14) C(13) C(18) C(17) AND 
CONT C(19) C(16) C(17) C(18) C(13) C(14) C(15) AND 
CONT C(119) C(116) C(115) C(114) C(113) C(118) C(117) AND 
CONT C(119) C(116) C(117) C(118) C(113) C(114) C(115) AND 
CONT C(27) C(28) C(29) C(30) C(31) C(32) C(33) AND 
CONT C(27) C(28) C(33) C(32) C(31) C(30) C(29) 
SAME C(19) N(20) C(21) C(22) N(23) C(24) C(25) N(26) C(27) AND 
CONT C(27) N(26) C(25) C(24) N(23) C(22) C(21) N(20) C(19) AND 
CONT C(119) N(20) C(21) C(22) N(23) C(24) C(25) N(26) C(27) AND 
CONT C(27) N(26) C(25) C(24) N(23) C(22) C(21) N(20) C(119) 
DISTANCE 0, 0.001 = MEAN CL(52) TO O(53) CL(52) TO O(54) 
CONT CL(52) TO O(55) CL(52) TO O(56) CL(47) TO O(48) 
CONT CL(47) TO O(49) CL(47) TO O(50) CL(47) TO O(51) 
CONT CL(147) TO O(48) CL(147) TO O(49) CL(147) TO O(50) 
CONT CL(147) TO O(151) 
DISTANCE 1.44, 0.01 = CL(52) TO O(53) CL(52) TO O(54) 
CONT CL(52) TO O(55) CL(52) TO O(56) CL(152) TO O(153) 
CONT CL(152) TO O(154) CL(152) TO O(155) CL(152) TO O(156) 
CONT CL(47) TO O(48) CL(47) TO O(49) CL(47) TO O(50) 
CONT CL(47) TO O(51) CL(147) TO O(48) CL(147) TO O(49) 
CONT CL(147) TO O(50) CL(147) TO O(151) 
ANGLE 109.5,1 = O(153) TO CL(152) TO O(154) 
CONT O(153) TO CL(152) TO O(155) O(153) TO CL(152) TO O(156) 
CONT O(154) TO CL(152) TO O(155) O(154) TO CL(152) TO O(156) 
CONT O(155) TO CL(152) TO O(156) 
ANGLE 109.5, 1 = O(151) TO CL(147) TO O(48) 
CONT O(151) TO CL(147) TO O(49) 
CONT O(151) TO CL(147) TO O(50) 
SIMU 0.04 C(57) C(58) N(59) 
DELU 0.01 C(57) C(58) N(59) 
SIMU 0.02 O(53) CL(52) O(54) 
SIMU 0.02 O(53) CL(52) O(55) 
SIMU 0.02 O(53) CL(52) O(56) 
SIMU 0.02 O(54) CL(52) O(55) 
SIMU 0.02 O(54) CL(52) O(56) 
SIMU 0.02 O(55) CL(52) O(56) 
DELU 0.01 O(53) CL(52) O(54) 
DELU 0.01 O(53) CL(52) O(55) 
DELU 0.01 O(53) CL(52) O(56) 
DELU 0.01 O(54) CL(52) O(55) 
DELU 0.01 O(54) CL(52) O(56) 
DELU 0.01 O(55) CL(52) O(56) 
SIMU 0.02 O(153) CL(152) O(154) 
SIMU 0.02 O(153) CL(152) O(155) 
SIMU 0.02 O(153) CL(152) O(156) 
SIMU 0.02 O(154) CL(152) O(155) 
SIMU 0.02 O(154) CL(152) O(156) 
SIMU 0.02 O(155) CL(152) O(156) 
DELU 0.01 O(153) CL(152) O(154) 
DELU 0.01 O(153) CL(152) O(155) 
DELU 0.01 O(153) CL(152) O(156) 
DELU 0.01 O(154) CL(152) O(155) 
DELU 0.01 O(154) CL(152) O(156) 
DELU 0.01 O(155) CL(152) O(156) 
SIMU 0.02 O(48) CL(147) O(49) 
SIMU 0.02 O(48) CL(147) O(50) 
SIMU 0.02 O(48) CL(147) O(151) 
SIMU 0.02 O(49) CL(147) O(50) 
SIMU 0.02 O(49) CL(147) O(151) 
SIMU 0.02 O(50) CL(147) O(151) 
DELU 0.01 O(48) CL(147) O(49) 
DELU 0.01 O(48) CL(147) O(50) 
DELU 0.01 O(48) CL(147) O(151) 
DELU 0.01 O(49) CL(147) O(50) 
DELU 0.01 O(49) CL(147) O(151) 
DELU 0.01 O(50) CL(147) O(151) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = N(9) TO C(10) 
VIBR .0, 0.00200 = C(10) TO C(11) 
VIBR .0, 0.00500 = C(11) TO N(9) 
VIBR .0, 0.00200 = C(10) TO C(111) 
VIBR .0, 0.00500 = C(111) TO N(9) 
VIBR .0, 0.00200 = N(20) TO C(21) 
VIBR .0, 0.00200 = N(20) TO CU(40) 
VIBR .0, 0.00200 = N(20) TO C(19) 
VIBR .0, 0.00500 = CU(40) TO C(21) 
VIBR .0, 0.00500 = C(19) TO C(21) 
VIBR .0, 0.00500 = C(19) TO CU(40) 
VIBR .0, 0.00200 = N(20) TO C(21) 
VIBR .0, 0.00200 = N(20) TO CU(40) 
VIBR .0, 0.00200 = N(20) TO C(119) 
VIBR .0, 0.00500 = CU(40) TO C(21) 
VIBR .0, 0.00500 = C(119) TO C(21) 
VIBR .0, 0.00500 = C(119) TO CU(40) 
VIBR .0, 0.00200 = C(21) TO C(22) 
VIBR .0, 0.00200 = C(21) TO CU(40) 
VIBR .0, 0.00500 = C(22) TO N(20) 
VIBR .0, 0.00500 = CU(40) TO N(20) 
VIBR .0, 0.00500 = CU(40) TO C(22) 
VIBR .0, 0.00200 = C(22) TO N(23) 
VIBR .0, 0.00200 = C(22) TO CU(40) 
VIBR .0, 0.00500 = N(23) TO C(21) 
VIBR .0, 0.00500 = CU(40) TO C(21) 
VIBR .0, 0.00500 = CU(40) TO N(23) 
VIBR .0, 0.00200 = N(23) TO C(24) 
VIBR .0, 0.00200 = N(23) TO CU(40) 
VIBR .0, 0.00500 = C(24) TO C(22) 
VIBR .0, 0.00500 = CU(40) TO C(22) 
VIBR .0, 0.00500 = CU(40) TO C(24) 
VIBR .0, 0.00200 = C(24) TO C(25) 
VIBR .0, 0.00200 = C(24) TO CU(40) 
VIBR .0, 0.00500 = C(25) TO N(23) 
VIBR .0, 0.00500 = CU(40) TO N(23) 
VIBR .0, 0.00500 = CU(40) TO C(25) 
VIBR .0, 0.00200 = C(25) TO N(26) 
VIBR .0, 0.00500 = N(26) TO C(24) 
VIBR .0, 0.00200 = N(26) TO C(27) 
VIBR .0, 0.00200 = N(26) TO CU(40) 
VIBR .0, 0.00500 = C(27) TO C(25) 
VIBR .0, 0.00500 = CU(40) TO C(25) 
VIBR .0, 0.00500 = CU(40) TO C(27) 
VIBR .0, 0.00500 = N(26) TO N(20) 
VIBR .0, 0.00500 = N(23) TO N(20) 
VIBR .0, 0.00500 = N(23) TO N(26) 
VIBR .0, 0.00500 = C(22) TO N(20) 
VIBR .0, 0.00500 = C(22) TO N(26) 
VIBR .0, 0.00500 = C(22) TO N(23) 
VIBR .0, 0.00500 = C(24) TO N(20) 
VIBR .0, 0.00500 = C(24) TO N(26) 
VIBR .0, 0.00500 = C(24) TO N(23) 
VIBR .0, 0.00500 = C(24) TO O(48) 
VIBR .0, 0.00500 = C(24) TO C(22) 
VIBR .0, 0.00500 = C(21) TO N(20) 
VIBR .0, 0.00500 = C(21) TO N(26) 
VIBR .0, 0.00500 = C(21) TO N(23) 
VIBR .0, 0.00500 = C(21) TO O(48) 
VIBR .0, 0.00500 = C(21) TO C(22) 
VIBR .0, 0.00500 = C(21) TO C(24) 
VIBR .0, 0.00200 = C(17) TO C(18) 
VIBR .0, 0.00200 = C(17) TO C(16) 
VIBR .0, 0.00500 = C(16) TO C(18) 
VIBR .0, 0.00200 = C(18) TO C(13) 
VIBR .0, 0.00500 = C(13) TO C(17) 
VIBR .0, 0.00200 = C(19) TO C(16) 
VIBR .0, 0.00500 = C(16) TO N(20) 
VIBR .0, 0.00200 = C(16) TO C(15) 
VIBR .0, 0.00500 = C(17) TO C(19) 
VIBR .0, 0.00500 = C(15) TO C(19) 
VIBR .0, 0.00500 = C(15) TO C(17) 
VIBR .0, 0.00200 = C(13) TO C(14) 
VIBR .0, 0.00200 = C(13) TO O(12) 
VIBR .0, 0.00500 = C(14) TO C(18) 
VIBR .0, 0.00500 = O(12) TO C(18) 
VIBR .0, 0.00500 = O(12) TO C(14) 
VIBR .0, 0.00200 = C(14) TO C(15) 
VIBR .0, 0.00500 = C(15) TO C(13) 
VIBR .0, 0.00500 = C(14) TO C(16) 
VIBR .0, 0.00200 = C(113) TO C(118) 
VIBR .0, 0.00200 = C(113) TO O(112) 
VIBR .0, 0.00200 = C(113) TO C(114) 
VIBR .0, 0.00500 = O(112) TO C(118) 
VIBR .0, 0.00500 = C(114) TO C(118) 
VIBR .0, 0.00500 = C(114) TO O(112) 
VIBR .0, 0.00200 = C(118) TO C(117) 
VIBR .0, 0.00500 = C(117) TO C(113) 
VIBR .0, 0.00200 = C(117) TO C(116) 
VIBR .0, 0.00500 = C(116) TO C(118) 
VIBR .0, 0.00200 = C(119) TO C(116) 
VIBR .0, 0.00500 = C(116) TO N(20) 
VIBR .0, 0.00200 = C(116) TO C(115) 
VIBR .0, 0.00500 = C(117) TO C(119) 
VIBR .0, 0.00500 = C(115) TO C(119) 
VIBR .0, 0.00500 = C(115) TO C(117) 
VIBR .0, 0.00200 = C(115) TO C(114) 
VIBR .0, 0.00500 = C(114) TO C(116) 
VIBR .0, 0.00200 = O(112) TO C(111) 
VIBR .0, 0.00500 = C(111) TO C(113) 
VIBR .0, 0.00200 = O(12) TO C(11) 
VIBR .0, 0.00500 = C(11) TO C(13) 
VIBR .0, 0.00500 = O(112) TO C(10) 
VIBR .0, 0.00500 = O(12) TO C(10) 
VIBR .0, 0.00500 = C(115) TO C(113) 
VIBR .0, 0.00200 = C(27) TO C(28) 
VIBR .0, 0.00500 = C(28) TO N(26) 
VIBR .0, 0.00200 = C(28) TO C(29) 
VIBR .0, 0.00200 = C(28) TO C(33) 
VIBR .0, 0.00500 = C(29) TO C(27) 
VIBR .0, 0.00500 = C(33) TO C(27) 
VIBR .0, 0.00500 = C(33) TO C(29) 
VIBR .0, 0.00200 = C(29) TO C(30) 
VIBR .0, 0.00500 = C(30) TO C(28) 
VIBR .0, 0.00200 = C(30) TO C(31) 
VIBR .0, 0.00500 = C(31) TO C(29) 
VIBR .0, 0.00200 = C(31) TO C(32) 
VIBR .0, 0.00500 = C(32) TO C(30) 
VIBR .0, 0.00200 = C(32) TO C(33) 
VIBR .0, 0.00500 = C(33) TO C(31) 
VIBR .0, 0.00500 = C(28) TO C(32) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = N(9) TO C(10) 
U(IJ) .0, 0.04000 = C(10) TO C(11) 
U(IJ) .0, 0.04000 = C(10) TO C(111) 
U(IJ) .0, 0.04000 = N(20) TO C(21) 
U(IJ) .0, 0.04000 = N(20) TO CU(40) 
U(IJ) .0, 0.04000 = N(20) TO C(19) 
U(IJ) .0, 0.04000 = N(20) TO C(21) 
U(IJ) .0, 0.04000 = N(20) TO CU(40) 
U(IJ) .0, 0.04000 = N(20) TO C(119) 
U(IJ) .0, 0.04000 = C(21) TO C(22) 
U(IJ) .0, 0.04000 = C(21) TO CU(40) 
U(IJ) .0, 0.04000 = C(22) TO N(23) 
U(IJ) .0, 0.04000 = C(22) TO CU(40) 
U(IJ) .0, 0.04000 = N(23) TO C(24) 
U(IJ) .0, 0.04000 = N(23) TO CU(40) 
U(IJ) .0, 0.04000 = C(24) TO C(25) 
U(IJ) .0, 0.04000 = C(24) TO CU(40) 
U(IJ) .0, 0.04000 = C(25) TO N(26) 
U(IJ) .0, 0.04000 = N(26) TO C(27) 
U(IJ) .0, 0.04000 = N(26) TO CU(40) 
U(IJ) .0, 0.04000 = C(17) TO C(18) 
U(IJ) .0, 0.04000 = C(17) TO C(16) 
U(IJ) .0, 0.04000 = C(18) TO C(13) 
U(IJ) .0, 0.04000 = C(19) TO C(16) 
U(IJ) .0, 0.04000 = C(16) TO C(15) 
U(IJ) .0, 0.04000 = C(13) TO C(14) 
U(IJ) .0, 0.04000 = C(13) TO O(12) 
U(IJ) .0, 0.04000 = C(14) TO C(15) 
U(IJ) .0, 0.04000 = C(113) TO C(118) 
U(IJ) .0, 0.04000 = C(113) TO O(112) 
U(IJ) .0, 0.04000 = C(113) TO C(114) 
U(IJ) .0, 0.04000 = C(118) TO C(117) 
U(IJ) .0, 0.04000 = C(117) TO C(116) 
U(IJ) .0, 0.04000 = C(119) TO C(116) 
U(IJ) .0, 0.04000 = C(116) TO C(115) 
U(IJ) .0, 0.04000 = C(115) TO C(114) 
U(IJ) .0, 0.04000 = O(112) TO C(111) 
U(IJ) .0, 0.04000 = O(12) TO C(11) 
U(IJ) .0, 0.04000 = C(28) TO C(29) 
U(IJ) .0, 0.04000 = C(28) TO C(33) 
U(IJ) .0, 0.04000 = C(29) TO C(30) 
U(IJ) .0, 0.04000 = C(30) TO C(31) 
U(IJ) .0, 0.04000 = C(31) TO C(32) 
U(IJ) .0, 0.04000 = C(32) TO C(33) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
1 0 8 x .
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile, di-isopropyl ether'
####################################################################### 
# 
# 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_pseudorotaxane-3-bipyridine-Cu-2ClO4
_database_code_depnum_ccdc_archive 'CCDC 1560764'
_audit_update_record             
;
2017-07-06 deposited with the CCDC.
2017-09-12 downloaded from the CCDC.
;
#============================================================================== 

# start Validation Reply Form
_vrf_PLAT990_3.2,2-bipyridine.CuClO42 
;
PROBLEM: Deprecated RES file style based SQUEEZE job ....          ! Note 
RESPONSE: SQUEEZE was implemented within the CRYSTAL suite, which does not use
RES files, hence this alert.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;

_refine_special_details          
;The crystals were weakly diffracting and, despite several attempts, this is the best data that could be obtained.
For the solvent molecules, counteranions and macrocycle tris-amine cleft, restraints on bond lengths and angles were used where appropriate
to ensure a physically reasonable model and thermal and vibrational restraints were used to maintain sensible displacement
ellipsoids. Large, prolate ellipsoidswere observed for one of the perchlorate counteranions, suggesting the presence of disorder. This was
modelled using refined partial occpancies over two postions. The difference map also indicated the presence of diffuse electron density,
believed to originate from diffuse, disordered solvent molecules. This was modelled using SQUEEZE, leaving a void from which the electron density
was removed. Hydrogen atoms were generally visible in the Fourier difference map and were initially positioned geometrically before
being refined with restraints on bond lengths and angles, after which the positions were used as the basis
for a riding model., SQUEEZE
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.500 197 15 ' '
2 0.500 0.000 0.500 145 13 ' '
_platon_squeeze_details          
;
The discrete Fourier transform of the void region were treated as 
contributions to the A and B parts of the calculated structure factors.
;

_cell_length_a                   14.48680(10)
_cell_length_b                   16.0097(2)
_cell_length_c                   21.0577(2)
_cell_angle_alpha                89.3012(5)
_cell_angle_beta                 89.6569(5)
_cell_angle_gamma                83.8028(5)
_cell_volume                     4854.94(8)

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

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126
1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'

_cell_formula_units_Z            2

_chemical_formula_sum            'C86 H99 Cl4 Cu2 N17 O24'
_chemical_formula_moiety         '2(C40 H45 Cu N7 O4), 4(Cl O4), 3(C2 H3 N)'
_chemical_compound_source        synthesised
_chemical_formula_weight         2023.73

_cell_measurement_reflns_used    101751
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       plate
_exptl_crystal_colour            'pale blue'
_exptl_crystal_size_min          0.04
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_max          0.18

_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2104
_exptl_absorpt_coefficient_mu    0.628

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_T_max  1.00
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            197575
_reflns_number_total             22025
_diffrn_reflns_av_R_equivalents  0.078

_diffrn_reflns_theta_min         5.100
_diffrn_reflns_theta_max         27.461
_diffrn_measured_fraction_theta_max 0.991

_diffrn_reflns_theta_full        26.912
_diffrn_measured_fraction_theta_full 0.993

_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       27
_reflns_limit_h_min              -18
_reflns_limit_h_max              18
_reflns_limit_k_min              -20
_reflns_limit_k_max              20
_reflns_limit_l_min              0
_reflns_limit_l_max              27

_oxford_diffrn_Wilson_B_factor   3.19
_oxford_diffrn_Wilson_scale      28.06

_atom_sites_solution_primary     Other
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.81
_refine_diff_density_max         1.84

_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         15286
_refine_ls_number_restraints     551
_refine_ls_number_parameters     1238
_oxford_refine_ls_R_factor_ref   0.0908
_refine_ls_wR_factor_ref         0.1901
_refine_ls_goodness_of_fit_ref   0.9502
_refine_ls_shift/su_max          0.0004864
_refine_ls_shift/su_mean         0.0000208

_oxford_reflns_number_all        15286
_refine_ls_R_factor_all          0.0908
_refine_ls_wR_factor_all         0.1901

_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                11584
_refine_ls_R_factor_gt           0.0695
_refine_ls_wR_factor_gt          0.1722

_chemical_absolute_configuration .

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr

_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 31.0 47.2 22.9 5.72 
;


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 0.3087(3) 0.2750(3) 0.6550(2) 0.0354 1.0000 Uani . . . . . .
C2 C 0.3412(3) 0.3410(3) 0.6872(2) 0.0349 1.0000 Uani . . . . . .
C3 C 0.3886(3) 0.3984(3) 0.6537(2) 0.0413 1.0000 Uani . . . . . .
C4 C 0.4031(4) 0.3901(3) 0.5888(2) 0.0479 1.0000 Uani . . . . . .
C5 C 0.3708(3) 0.3248(3) 0.5573(2) 0.0448 1.0000 Uani . . . . . .
C6 C 0.3241(3) 0.2655(3) 0.5902(2) 0.0366 1.0000 Uani . . . . . .
C7 C 0.2913(3) 0.1948(4) 0.5530(2) 0.0425 1.0000 Uani . . . . . .
O8 O 0.2750(3) 0.2041(3) 0.49630(16) 0.0638 1.0000 Uani . . . . . .
N9 N 0.2821(3) 0.1232(3) 0.58433(19) 0.0456 1.0000 Uani . . . . . .
C10 C 0.2554(4) 0.0480(4) 0.5546(3) 0.0514 1.0000 Uani . . . . . .
C11 C 0.1567(4) 0.0321(3) 0.5712(3) 0.0488 1.0000 Uani . . . . . .
O12 O 0.0957(2) 0.0969(2) 0.54142(16) 0.0461 1.0000 Uani . . . . . .
C13 C 0.0026(3) 0.0960(3) 0.5521(2) 0.0396 1.0000 Uani . . . . . .
C14 C -0.0537(4) 0.1589(3) 0.5216(2) 0.0472 1.0000 Uani . . . . . .
C15 C -0.1484(4) 0.1659(3) 0.5312(2) 0.0466 1.0000 Uani . . . . . .
C16 C -0.1887(3) 0.1110(3) 0.5716(2) 0.0409 1.0000 Uani . . . . . .
C17 C -0.1311(4) 0.0477(3) 0.6009(2) 0.0422 1.0000 Uani . . . . . .
C18 C -0.0357(4) 0.0386(3) 0.5911(2) 0.0426 1.0000 Uani . . . . . .
C19 C -0.2912(4) 0.1218(3) 0.5843(2) 0.0473 1.0000 Uani . . . . . .
N20 N -0.3196(3) 0.2001(3) 0.6209(2) 0.0417 1.0000 Uani . . . . . .
C21 C -0.4222(4) 0.2135(3) 0.6289(3) 0.0479 1.0000 Uani . . . . . .
C22 C -0.4511(3) 0.1548(3) 0.6810(3) 0.0460 1.0000 Uani . . . . . .
N23 N -0.3867(3) 0.1540(3) 0.7364(2) 0.0443 1.0000 Uani . . . . . .
C24 C -0.4272(4) 0.2008(4) 0.7922(3) 0.0565 1.0000 Uani . . . . . .
C25 C -0.4167(4) 0.2936(4) 0.7819(3) 0.0548 1.0000 Uani . . . . . .
N26 N -0.3178(3) 0.3039(3) 0.7754(2) 0.0475 1.0000 Uani . . . . . .
C27 C -0.2745(4) 0.3133(4) 0.8384(3) 0.0578 1.0000 Uani . . . . . .
C28 C -0.1718(4) 0.3177(3) 0.8369(2) 0.0452 1.0000 Uani . . . . . .
C29 C -0.1133(4) 0.2634(3) 0.8740(2) 0.0417 1.0000 Uani . . . . . .
C30 C -0.0187(3) 0.2658(3) 0.8749(2) 0.0377 1.0000 Uani . . . . . .
C31 C 0.0207(3) 0.3239(3) 0.8374(2) 0.0387 1.0000 Uani . . . . . .
C32 C -0.0371(4) 0.3797(3) 0.8004(2) 0.0478 1.0000 Uani . . . . . .
C33 C -0.1309(4) 0.3764(3) 0.8002(3) 0.0502 1.0000 Uani . . . . . .
O34 O 0.1131(2) 0.3327(2) 0.83358(15) 0.0427 1.0000 Uani . . . . . .
C35 C 0.1754(4) 0.2753(3) 0.8703(2) 0.0420 1.0000 Uani . . . . . .
C36 C 0.2715(4) 0.2969(3) 0.8581(2) 0.0414 1.0000 Uani . . . . . .
N37 N 0.2955(3) 0.2929(3) 0.79035(18) 0.0425 1.0000 Uani . . . . . .
C38 C 0.3269(3) 0.3542(3) 0.7578(2) 0.0359 1.0000 Uani . . . . . .
O39 O 0.3451(4) 0.4198(3) 0.78247(18) 0.0698 1.0000 Uani . . . . . .
N40 N -0.1474(3) 0.2429(3) 0.6858(2) 0.0504 1.0000 Uani . . . . . .
C41 C -0.1398(5) 0.3088(4) 0.6452(3) 0.0642 1.0000 Uani . . . . . .
C42 C -0.0555(5) 0.3344(5) 0.6264(4) 0.0757 1.0000 Uani . . . . . .
C43 C 0.0231(6) 0.2888(5) 0.6478(4) 0.0794 1.0000 Uani . . . . . .
C44 C 0.0191(4) 0.2223(4) 0.6885(3) 0.0671 1.0000 Uani . . . . . .
C45 C -0.0693(4) 0.2011(4) 0.7083(3) 0.0516 1.0000 Uani . . . . . .
C46 C -0.0842(4) 0.1376(3) 0.7560(3) 0.0542 1.0000 Uani . . . . . .
C47 C -0.0118(5) 0.0953(4) 0.7915(3) 0.0656 1.0000 Uani . . . . . .
C48 C -0.0339(5) 0.0450(4) 0.8407(4) 0.0712 1.0000 Uani . . . . . .
C49 C -0.1229(6) 0.0308(4) 0.8538(3) 0.0756 1.0000 Uani . . . . . .
C50 C -0.1943(5) 0.0725(4) 0.8137(3) 0.0611 1.0000 Uani . . . . . .
N51 N -0.1745(3) 0.1230(3) 0.7674(2) 0.0501 1.0000 Uani . . . . . .
Cu52 Cu -0.26714(4) 0.20051(4) 0.71218(3) 0.0392 1.0000 Uani . . . . . .
Cl53 Cl 0.30163(9) 0.06070(8) 0.76540(6) 0.0477 1.0000 Uani D U . . . .
O54 O 0.3434(4) 0.0279(3) 0.7081(2) 0.0851 1.0000 Uani D U . . . .
O55 O 0.3678(3) 0.0993(3) 0.8012(2) 0.0667 1.0000 Uani D U . . . .
O56 O 0.2258(3) 0.1240(3) 0.7496(2) 0.0642 1.0000 Uani D U . . . .
O57 O 0.2672(4) -0.0050(2) 0.80223(19) 0.0698 1.0000 Uani D U . . . .
Cl58 Cl 0.74656(9) 0.60166(8) 0.74074(6) 0.0486 1.0000 Uani D U . . . .
O59 O 0.8056(3) 0.5522(2) 0.6976(2) 0.0650 1.0000 Uani D U . . . .
O60 O 0.6751(3) 0.6527(3) 0.7067(2) 0.0720 1.0000 Uani D U . . . .
O61 O 0.7053(3) 0.5496(3) 0.7858(2) 0.0827 1.0000 Uani D U . . . .
O62 O 0.8011(3) 0.6565(3) 0.7743(2) 0.0685 1.0000 Uani D U . . . .
Cl63 Cl 0.66068(10) 0.16865(8) 0.99503(7) 0.0531 1.0000 Uani D U . . . .
O64 O 0.5938(4) 0.1335(4) 0.9598(3) 0.1072 1.0000 Uani D U . . . .
O65 O 0.6539(4) 0.2575(3) 0.9855(3) 0.0799 1.0000 Uani D U . . . .
O66 O 0.7527(4) 0.1351(3) 0.9788(3) 0.1064 1.0000 Uani D U . . . .
O67 O 0.6456(3) 0.1535(3) 1.0609(2) 0.0798 1.0000 Uani D U . . . .
C73 C 0.6226(9) 0.5421(4) 0.5858(4) 0.1222 1.0000 Uani D U . . . .
C74 C 0.6312(5) 0.4697(4) 0.6264(3) 0.0742 1.0000 Uani D U . . . .
N75 N 0.6411(5) 0.4118(4) 0.6575(4) 0.1087 1.0000 Uani D U . . . .
C76 C 0.4612(5) 0.3661(5) 0.9501(4) 0.0847 1.0000 Uani D U . . . .
C77 C 0.5287(4) 0.4236(4) 0.9413(3) 0.0582 1.0000 Uani D U . . . .
N78 N 0.5825(4) 0.4698(3) 0.9342(3) 0.0748 1.0000 Uani D U . . . .
C79 C 0.2706(4) 1.0598(4) 0.9556(3) 0.0681 1.0000 Uani D U . . . .
C80 C 0.1728(5) 1.0738(4) 0.9694(3) 0.0691 1.0000 Uani D U . . . .
N81 N 0.0955(5) 1.0860(6) 0.9800(4) 0.1142 1.0000 Uani D U . . . .
C101 C 0.6817(3) 0.8229(3) 0.8422(2) 0.0368 1.0000 Uani . . . . . .
C102 C 0.6395(3) 0.8909(3) 0.8067(2) 0.0355 1.0000 Uani . . . . . .
C103 C 0.5711(3) 0.9461(3) 0.8347(3) 0.0440 1.0000 Uani . . . . . .
C104 C 0.5426(4) 0.9321(4) 0.8967(3) 0.0545 1.0000 Uani . . . . . .
C105 C 0.5838(4) 0.8640(4) 0.9310(2) 0.0479 1.0000 Uani . . . . . .
C106 C 0.6533(3) 0.8086(3) 0.9047(2) 0.0402 1.0000 Uani . . . . . .
C107 C 0.6950(4) 0.7366(3) 0.9449(2) 0.0446 1.0000 Uani . . . . . .
O108 O 0.6938(3) 0.7417(3) 1.00333(17) 0.0646 1.0000 Uani . . . . . .
N109 N 0.7310(3) 0.6678(3) 0.91523(19) 0.0460 1.0000 Uani . . . . . .
C110 C 0.7649(4) 0.5890(4) 0.9475(3) 0.0530 1.0000 Uani . . . . . .
C111 C 0.8625(4) 0.5577(3) 0.9284(2) 0.0449 1.0000 Uani . . . . . .
O112 O 0.9238(2) 0.6096(2) 0.95741(15) 0.0428 1.0000 Uani . . . . . .
C113 C 1.0163(3) 0.5930(3) 0.9446(2) 0.0380 1.0000 Uani . U . . . .
C114 C 1.0558(4) 0.5323(3) 0.9031(2) 0.0406 1.0000 Uani . . . . . .
C115 C 1.1500(4) 0.5265(3) 0.8912(2) 0.0401 1.0000 Uani . U . . . .
C116 C 1.2072(4) 0.5775(3) 0.9202(2) 0.0395 1.0000 Uani . U . . . .
C117 C 1.1677(4) 0.6351(3) 0.9643(2) 0.0428 1.0000 Uani . U . . . .
C118 C 1.0738(4) 0.6432(3) 0.9759(2) 0.0413 1.0000 Uani . U . . . .
C119 C 1.3097(4) 0.5712(3) 0.9051(3) 0.0481 1.0000 Uani . U . . . .
N120 N 1.3386(3) 0.6530(3) 0.8816(2) 0.0555 1.0000 Uani . U . . . .
C121 C 1.4439(4) 0.6449(5) 0.8670(4) 0.0887 1.0000 Uani . U . . . .
C122 C 1.4541(5) 0.6038(5) 0.8002(5) 0.0891 1.0000 Uani . U . . . .
N123 N 1.4052(4) 0.6643(4) 0.7548(4) 0.0926 1.0000 Uani . U . . . .
C124 C 1.4490(4) 0.7409(5) 0.7292(3) 0.0710 1.0000 Uani . U . . . .
C125 C 1.4056(4) 0.8202(5) 0.7566(4) 0.0751 1.0000 Uani . U . . . .
N126 N 1.3030(3) 0.8191(3) 0.7524(2) 0.0519 1.0000 Uani . U . . . .
C127 C 1.2684(4) 0.8304(4) 0.6859(3) 0.0508 1.0000 Uani . U . . . .
C128 C 1.1640(3) 0.8338(3) 0.6834(2) 0.0426 1.0000 Uani . U . . . .
C129 C 1.1073(4) 0.8925(3) 0.7192(2) 0.0428 1.0000 Uani . U . . . .
C130 C 1.0124(3) 0.8959(3) 0.7163(2) 0.0422 1.0000 Uani . . . . . .
C131 C 0.9705(3) 0.8420(3) 0.6783(2) 0.0360 1.0000 Uani . . . . . .
C132 C 1.0244(3) 0.7823(3) 0.6421(2) 0.0381 1.0000 Uani . . . . . .
C133 C 1.1210(4) 0.7797(3) 0.6455(2) 0.0420 1.0000 Uani . U . . . .
O134 O 0.8756(2) 0.8535(2) 0.67823(15) 0.0418 1.0000 Uani . . . . . .
C135 C 0.8270(3) 0.8040(3) 0.6367(2) 0.0396 1.0000 Uani . . . . . .
C136 C 0.7258(3) 0.8382(3) 0.6408(2) 0.0402 1.0000 Uani . . . . . .
N137 N 0.6913(3) 0.8368(2) 0.70574(17) 0.0359 1.0000 Uani . . . . . .
C138 C 0.6677(3) 0.9057(3) 0.7398(2) 0.0353 1.0000 Uani . . . . . .
O139 O 0.6670(3) 0.9780(2) 0.71782(16) 0.0492 1.0000 Uani . . . . . .
N140 N 1.1598(3) 0.7513(2) 0.83376(19) 0.0404 1.0000 Uani . . . . . .
C141 C 1.1493(4) 0.8117(3) 0.8768(3) 0.0490 1.0000 Uani . . . . . .
C142 C 1.0619(4) 0.8408(3) 0.9021(3) 0.0539 1.0000 Uani . . . . . .
C143 C 0.9858(4) 0.8042(4) 0.8803(3) 0.0551 1.0000 Uani . . . . . .
C144 C 0.9958(4) 0.7435(3) 0.8357(3) 0.0481 1.0000 Uani . . . . . .
C145 C 1.0844(3) 0.7165(3) 0.8134(2) 0.0415 1.0000 Uani . . . . . .
C146 C 1.1027(4) 0.6487(3) 0.7658(2) 0.0451 1.0000 Uani . . . . . .
C147 C 1.0321(4) 0.6079(4) 0.7377(3) 0.0555 1.0000 Uani . . . . . .
C148 C 1.0564(6) 0.5469(4) 0.6935(3) 0.0694 1.0000 Uani . . . . . .
C149 C 1.1468(6) 0.5267(4) 0.6779(3) 0.0730 1.0000 Uani . . . . . .
C150 C 1.2128(5) 0.5684(4) 0.7067(3) 0.0645 1.0000 Uani . . . . . .
N151 N 1.1923(3) 0.6295(3) 0.7508(2) 0.0476 1.0000 Uani . . . . . .
Cu152 Cu 1.28068(4) 0.70326(4) 0.79576(3) 0.0477 1.0000 Uani . U . . . .
O570 O 0.3227(14) 0.6325(15) 0.5984(9) 0.1238 0.395(15) Uani D U P 1 2 .
O70 O 0.3759(10) 0.6278(9) 0.6112(4) 0.1099 0.605(15) Uani D U P 1 1 .
O72 O 0.3456(11) 0.7350(6) 0.5349(8) 0.1410 0.605(15) Uani D U P 1 1 .
O572 O 0.4056(18) 0.7264(12) 0.5450(12) 0.1460 0.395(15) Uani D U P 1 2 .
O569 O 0.2922(15) 0.6579(12) 0.4892(9) 0.1394 0.395(15) Uani D U P 1 2 .
O69 O 0.2643(7) 0.6193(11) 0.5357(8) 0.1545 0.605(15) Uani D U P 1 1 .
H11 H 0.2753 0.2367 0.6772 0.0399 1.0000 Uiso R . . . . .
H31 H 0.4110 0.4425 0.6744 0.0455 1.0000 Uiso R . . . . .
H41 H 0.4337 0.4294 0.5661 0.0548 1.0000 Uiso R . . . . .
H51 H 0.3813 0.3182 0.5140 0.0520 1.0000 Uiso R . . . . .
H101 H 0.2956 -0.0002 0.5686 0.0597 1.0000 Uiso R . . . . .
H102 H 0.2610 0.0543 0.5088 0.0597 1.0000 Uiso R . . . . .
H112 H 0.1487 0.0351 0.6173 0.0568 1.0000 Uiso R . . . . .
H111 H 0.1439 -0.0228 0.5567 0.0572 1.0000 Uiso R . . . . .
H141 H -0.0276 0.1970 0.4953 0.0541 1.0000 Uiso R . . . . .
H151 H -0.1868 0.2080 0.5099 0.0550 1.0000 Uiso R . . . . .
H171 H -0.1571 0.0103 0.6287 0.0489 1.0000 Uiso R . . . . .
H181 H 0.0025 -0.0061 0.6102 0.0491 1.0000 Uiso R . . . . .
H192 H -0.3101 0.0742 0.6080 0.0549 1.0000 Uiso R . . . . .
H191 H -0.3238 0.1266 0.5444 0.0547 1.0000 Uiso R . . . . .
H212 H -0.4378 0.2709 0.6418 0.0548 1.0000 Uiso R . . . . .
H211 H -0.4534 0.2031 0.5890 0.0548 1.0000 Uiso R . . . . .
H221 H -0.5151 0.1719 0.6941 0.0558 1.0000 Uiso R . . . . .
H222 H -0.4467 0.0980 0.6645 0.0557 1.0000 Uiso R . . . . .
H241 H -0.4028 0.1797 0.8322 0.0821 1.0000 Uiso R . . . . .
H242 H -0.4907 0.1985 0.7800 0.0823 1.0000 Uiso R . . . . .
H251 H -0.4431 0.3248 0.8182 0.0661 1.0000 Uiso R . . . . .
H252 H -0.4494 0.3136 0.7433 0.0660 1.0000 Uiso R . . . . .
H271 H -0.3029 0.3655 0.8561 0.0679 1.0000 Uiso R . . . . .
H272 H -0.2882 0.2656 0.8643 0.0680 1.0000 Uiso R . . . . .
H291 H -0.1380 0.2247 0.9004 0.0469 1.0000 Uiso R . . . . .
H301 H 0.0179 0.2280 0.9003 0.0438 1.0000 Uiso R . . . . .
H321 H -0.0104 0.4187 0.7752 0.0548 1.0000 Uiso R . . . . .
H331 H -0.1685 0.4151 0.7762 0.0580 1.0000 Uiso R . . . . .
H352 H 0.1613 0.2809 0.9153 0.0492 1.0000 Uiso R . . . . .
H351 H 0.1721 0.2177 0.8565 0.0490 1.0000 Uiso R . . . . .
H362 H 0.2756 0.3537 0.8726 0.0479 1.0000 Uiso R . . . . .
H361 H 0.3149 0.2583 0.8815 0.0481 1.0000 Uiso R . . . . .
H411 H -0.1942 0.3387 0.6300 0.0769 1.0000 Uiso R . . . . .
H421 H -0.0534 0.3810 0.6004 0.0899 1.0000 Uiso R . . . . .
H431 H 0.0813 0.3038 0.6347 0.0959 1.0000 Uiso R . . . . .
H441 H 0.0726 0.1912 0.7022 0.0782 1.0000 Uiso R . . . . .
H471 H 0.0498 0.1022 0.7821 0.0792 1.0000 Uiso R . . . . .
H481 H 0.0132 0.0198 0.8659 0.0922 1.0000 Uiso R . . . . .
H491 H -0.1378 -0.0034 0.8871 0.0861 1.0000 Uiso R . . . . .
H501 H -0.2567 0.0637 0.8213 0.0726 1.0000 Uiso R . . . . .
H793 H 0.2779 1.0344 0.9151 0.0989 1.0000 Uiso R . . . . .
H791 H 0.2957 1.1127 0.9559 0.0991 1.0000 Uiso R . . . . .
H792 H 0.2997 1.0237 0.9875 0.0989 1.0000 Uiso R . . . . .
H1011 H 0.7295 0.7866 0.8245 0.0410 1.0000 Uiso R . . . . .
H1031 H 0.5438 0.9921 0.8118 0.0512 1.0000 Uiso R . . . . .
H1041 H 0.4961 0.9689 0.9149 0.0627 1.0000 Uiso R . . . . .
H1051 H 0.5647 0.8561 0.9728 0.0572 1.0000 Uiso R . . . . .
H1101 H 0.7635 0.5988 0.9931 0.0611 1.0000 Uiso R . . . . .
H1102 H 0.7234 0.5469 0.9371 0.0609 1.0000 Uiso R . . . . .
H1111 H 0.8772 0.5011 0.9430 0.0519 1.0000 Uiso R . . . . .
H1112 H 0.8690 0.5595 0.8830 0.0518 1.0000 Uiso R . . . . .
H1141 H 1.0201 0.4959 0.8837 0.0449 1.0000 Uiso R . . . . .
H1151 H 1.1751 0.4863 0.8626 0.0482 1.0000 Uiso R . . . . .
H1171 H 1.2051 0.6684 0.9874 0.0477 1.0000 Uiso R . . . . .
H1181 H 1.0482 0.6835 1.0041 0.0489 1.0000 Uiso R . . . . .
H1191 H 1.3449 0.5544 0.9433 0.0590 1.0000 Uiso R . . . . .
H1192 H 1.3242 0.5301 0.8716 0.0592 1.0000 Uiso R . . . . .
H1212 H 1.4552 0.5971 0.8952 0.1341 1.0000 Uiso R . . . . .
H1211 H 1.4743 0.6960 0.8666 0.1333 1.0000 Uiso R . . . . .
H1221 H 1.5193 0.5901 0.7879 0.1113 1.0000 Uiso R . . . . .
H1222 H 1.4243 0.5510 0.8011 0.1115 1.0000 Uiso R . . . . .
H1241 H 1.5147 0.7341 0.7370 0.0901 1.0000 Uiso R . . . . .
H1242 H 1.4385 0.7425 0.6834 0.0899 1.0000 Uiso R . . . . .
H1251 H 1.4235 0.8194 0.8012 0.0868 1.0000 Uiso R . . . . .
H1252 H 1.4245 0.8686 0.7335 0.0871 1.0000 Uiso R . . . . .
H1271 H 1.2885 0.8816 0.6685 0.0600 1.0000 Uiso R . . . . .
H1272 H 1.2956 0.7825 0.6626 0.0599 1.0000 Uiso R . . . . .
H1291 H 1.1343 0.9295 0.7453 0.0490 1.0000 Uiso R . . . . .
H1301 H 0.9766 0.9348 0.7408 0.0492 1.0000 Uiso R . . . . .
H1321 H 0.9974 0.7449 0.6164 0.0436 1.0000 Uiso R . . . . .
H1331 H 1.1573 0.7393 0.6216 0.0470 1.0000 Uiso R . . . . .
H1351 H 0.8495 0.8090 0.5939 0.0470 1.0000 Uiso R . . . . .
H1352 H 0.8335 0.7461 0.6502 0.0470 1.0000 Uiso R . . . . .
H1361 H 0.7210 0.8951 0.6255 0.0477 1.0000 Uiso R . . . . .
H1362 H 0.6904 0.8042 0.6144 0.0480 1.0000 Uiso R . . . . .
H1411 H 1.2018 0.8352 0.8905 0.0561 1.0000 Uiso R . . . . .
H1421 H 1.0576 0.8808 0.9333 0.0620 1.0000 Uiso R . . . . .
H1431 H 0.9273 0.8215 0.8966 0.0619 1.0000 Uiso R . . . . .
H1441 H 0.9442 0.7203 0.8208 0.0549 1.0000 Uiso R . . . . .
H1471 H 0.9706 0.6215 0.7488 0.0642 1.0000 Uiso R . . . . .
H1481 H 1.0104 0.5193 0.6740 0.0828 1.0000 Uiso R . . . . .
H1491 H 1.1646 0.4852 0.6479 0.0871 1.0000 Uiso R . . . . .
H1501 H 1.2743 0.5555 0.6959 0.0739 1.0000 Uiso R . . . . .
H1091 H 0.7207 0.6651 0.8754 0.0529 1.0000 Uiso R . . . . .
H91 H 0.3060 0.1176 0.6211 0.0531 1.0000 Uiso R . . . . .
H1371 H 0.6583 0.7969 0.7132 0.0423 1.0000 Uiso R . . . . .
H371 H 0.2641 0.2598 0.7687 0.0524 1.0000 Uiso R . . . . .
H201 H -0.3025 0.2432 0.5991 0.0591 1.0000 Uiso R . . . . .
H231 H -0.3725 0.1007 0.7483 0.0640 1.0000 Uiso R . . . . .
H261 H -0.3137 0.3509 0.7541 0.0688 1.0000 Uiso R . . . . .
H1261 H 1.2747 0.8615 0.7766 0.0784 1.0000 Uiso R . . . . .
H1231 H 1.3937 0.6350 0.7197 0.1305 1.0000 Uiso R . . . . .
H1201 H 1.3258 0.6914 0.9124 0.0874 1.0000 Uiso R . . . . .
H731 H 0.5604 0.5689 0.5890 0.1811 1.0000 Uiso R . . . . .
H732 H 0.6652 0.5805 0.5991 0.1809 1.0000 Uiso R . . . . .
H733 H 0.6360 0.5245 0.5429 0.1811 1.0000 Uiso R . . . . .
H761 H 0.4719 0.3369 0.9895 0.1282 1.0000 Uiso R . . . . .
H762 H 0.4004 0.3968 0.9505 0.1282 1.0000 Uiso R . . . . .
H763 H 0.4663 0.3269 0.9162 0.1282 1.0000 Uiso R . . . . .
Cl68 Cl 0.3536(6) 0.6476(6) 0.5463(4) 0.0848 0.605(15) Uani D U P 1 1 .
O71 O 0.4247(9) 0.6082(9) 0.5081(6) 0.0982 0.605(15) Uani D U P 1 1 .
O571 O 0.4281(17) 0.5844(12) 0.5230(10) 0.0990 0.395(15) Uani D U P 1 2 .
Cl568 Cl 0.3613(9) 0.6522(9) 0.5382(6) 0.0848 0.395(15) Uani D U P 1 2 .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.20436(14)

loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . C2 . 1.388(7) yes
C1 . C6 . 1.388(6) yes
C1 . H11 . 0.940 no
C2 . C3 . 1.388(7) yes
C2 . C38 . 1.514(6) yes
C3 . C4 . 1.386(7) yes
C3 . H31 . 0.924 no
C4 . C5 . 1.370(8) yes
C4 . H41 . 0.934 no
C5 . C6 . 1.399(7) yes
C5 . H51 . 0.930 no
C6 . C7 . 1.503(7) yes
C7 . O8 . 1.222(6) yes
C7 . N9 . 1.335(7) yes
N9 . C10 . 1.454(7) yes
N9 . H91 . 0.849 no
C10 . C11 . 1.517(8) yes
C10 . H101 . 0.959 no
C10 . H102 . 0.974 no
C11 . O12 . 1.431(6) yes
C11 . H112 . 0.978 no
C11 . H111 . 0.971 no
O12 . C13 . 1.369(6) yes
C13 . C14 . 1.379(7) yes
C13 . C18 . 1.384(7) yes
C14 . C15 . 1.379(7) yes
C14 . H141 . 0.928 no
C15 . C16 . 1.388(7) yes
C15 . H151 . 0.937 no
C16 . C17 . 1.383(7) yes
C16 . C19 . 1.499(7) yes
C17 . C18 . 1.388(7) yes
C17 . H171 . 0.939 no
C18 . H181 . 0.943 no
C19 . N20 . 1.497(6) yes
C19 . H192 . 0.969 no
C19 . H191 . 0.965 no
N20 . C21 . 1.488(6) yes
N20 . Cu52 . 2.071(4) yes
N20 . H201 . 0.882 no
C21 . C22 . 1.523(8) yes
C21 . H212 . 0.965 no
C21 . H211 . 0.980 no
C22 . N23 . 1.497(6) yes
C22 . H221 . 0.976 no
C22 . H222 . 0.974 no
N23 . C24 . 1.484(7) yes
N23 . Cu52 . 2.019(4) yes
N23 . H231 . 0.889 no
C24 . C25 . 1.522(8) yes
C24 . Cu52 . 2.858(5) yes
C24 . H241 . 0.960 no
C24 . H242 . 0.961 no
C25 . N26 . 1.466(7) yes
C25 . H251 . 0.973 no
C25 . H252 . 0.975 no
N26 . C27 . 1.486(7) yes
N26 . Cu52 . 2.198(4) yes
N26 . H261 . 0.877 no
C27 . C28 . 1.497(8) yes
C27 . H271 . 0.968 no
C27 . H272 . 0.971 no
C28 . C29 . 1.385(7) yes
C28 . C33 . 1.390(8) yes
C29 . C30 . 1.375(7) yes
C29 . H291 . 0.926 no
C30 . C31 . 1.381(7) yes
C30 . H301 . 0.928 no
C31 . C32 . 1.391(7) yes
C31 . O34 . 1.361(6) yes
C32 . C33 . 1.366(8) yes
C32 . H321 . 0.929 no
C33 . H331 . 0.926 no
O34 . C35 . 1.439(6) yes
C35 . C36 . 1.490(7) yes
C35 . H352 . 0.970 no
C35 . H351 . 0.977 no
C36 . N37 . 1.467(6) yes
C36 . H362 . 0.971 no
C36 . H361 . 0.965 no
N37 . C38 . 1.310(6) yes
N37 . H371 . 0.869 no
C38 . O39 . 1.233(6) yes
N40 . C41 . 1.362(8) yes
N40 . C45 . 1.337(7) yes
N40 . Cu52 . 2.003(5) yes
C41 . C42 . 1.384(9) yes
C41 . H411 . 0.933 no
C42 . C43 . 1.361(11) yes
C42 . H421 . 0.923 no
C43 . C44 . 1.364(10) yes
C43 . H431 . 0.939 no
C44 . C45 . 1.420(8) yes
C44 . H441 . 0.921 no
C45 . C46 . 1.452(9) yes
C46 . C47 . 1.399(8) yes
C46 . N51 . 1.374(7) yes
C47 . C48 . 1.362(10) yes
C47 . H471 . 0.932 no
C48 . C49 . 1.359(11) yes
C48 . H481 . 0.921 no
C49 . C50 . 1.441(9) yes
C49 . H491 . 0.924 no
C50 . N51 . 1.309(8) yes
C50 . H501 . 0.943 no
N51 . Cu52 . 2.078(4) yes
Cl53 . O54 . 1.427(4) yes
Cl53 . O55 . 1.420(4) yes
Cl53 . O56 . 1.449(4) yes
Cl53 . O57 . 1.430(4) yes
Cl58 . O59 . 1.430(4) yes
Cl58 . O60 . 1.436(4) yes
Cl58 . O61 . 1.427(4) yes
Cl58 . O62 . 1.438(4) yes
Cl63 . O64 . 1.394(5) yes
Cl63 . O65 . 1.427(4) yes
Cl63 . O66 . 1.424(4) yes
Cl63 . O67 . 1.425(4) yes
C73 . C74 . 1.427(7) yes
C73 . H731 . 0.957 no
C73 . H732 . 0.962 no
C73 . H733 . 0.962 no
C74 . N75 . 1.125(6) yes
C76 . C77 . 1.422(7) yes
C76 . H761 . 0.952 no
C76 . H762 . 0.961 no
C76 . H763 . 0.954 no
C77 . N78 . 1.139(6) yes
C79 . C80 . 1.440(7) yes
C79 . H793 . 0.951 no
C79 . H791 . 0.956 no
C79 . H792 . 0.950 no
C80 . N81 . 1.137(7) yes
C101 . C102 . 1.399(7) yes
C101 . C106 . 1.400(6) yes
C101 . H1011 . 0.934 no
C102 . C103 . 1.388(7) yes
C102 . C138 . 1.488(6) yes
C103 . C104 . 1.389(8) yes
C103 . H1031 . 0.928 no
C104 . C105 . 1.382(8) yes
C104 . H1041 . 0.930 no
C105 . C106 . 1.386(7) yes
C105 . H1051 . 0.932 no
C106 . C107 . 1.498(7) yes
C107 . O108 . 1.233(6) yes
C107 . N109 . 1.329(7) yes
N109 . C110 . 1.464(7) yes
N109 . H1091 . 0.854 no
C110 . C111 . 1.503(8) yes
C110 . H1101 . 0.975 no
C110 . H1102 . 0.977 no
C111 . O112 . 1.425(6) yes
C111 . H1111 . 0.956 no
C111 . H1112 . 0.959 no
O112 . C113 . 1.363(6) yes
C113 . C114 . 1.390(7) yes
C113 . C118 . 1.392(7) yes
C114 . C115 . 1.380(7) yes
C114 . H1141 . 0.921 no
C115 . C116 . 1.375(7) yes
C115 . H1151 . 0.929 no
C116 . C117 . 1.394(7) yes
C116 . C119 . 1.510(7) yes
C117 . C118 . 1.372(7) yes
C117 . H1171 . 0.942 no
C118 . H1181 . 0.929 no
C119 . N120 . 1.495(7) yes
C119 . H1191 . 0.974 no
C119 . H1192 . 0.977 no
N120 . C121 . 1.546(8) yes
N120 . Cu152 . 2.110(5) yes
N120 . H1201 . 0.904 no
C121 . C122 . 1.559(12) yes
C121 . Cu152 . 2.872(7) yes
C121 . H1212 . 0.964 no
C121 . H1211 . 0.970 no
C122 . N123 . 1.480(10) yes
C122 . H1221 . 0.980 no
C122 . H1222 . 0.989 no
N123 . C124 . 1.531(9) yes
N123 . Cu152 . 2.035(5) yes
N123 . H1231 . 0.907 no
C124 . C125 . 1.477(10) yes
C124 . H1241 . 0.961 no
C124 . H1242 . 0.975 no
C125 . N126 . 1.491(7) yes
C125 . H1251 . 0.976 no
C125 . H1252 . 0.972 no
N126 . C127 . 1.491(7) yes
N126 . Cu152 . 2.112(5) yes
N126 . H1261 . 0.914 no
C127 . C128 . 1.509(7) yes
C127 . H1271 . 0.967 no
C127 . H1272 . 0.961 no
C128 . C129 . 1.403(7) yes
C128 . C133 . 1.383(7) yes
C129 . C130 . 1.372(7) yes
C129 . H1291 . 0.931 no
C130 . C131 . 1.375(7) yes
C130 . H1301 . 0.927 no
C131 . C132 . 1.398(7) yes
C131 . O134 . 1.368(6) yes
C132 . C133 . 1.397(7) yes
C132 . H1321 . 0.929 no
C133 . H1331 . 0.939 no
O134 . C135 . 1.424(6) yes
C135 . C136 . 1.511(7) yes
C135 . H1351 . 0.963 no
C135 . H1352 . 0.962 no
C136 . N137 . 1.453(6) yes
C136 . H1361 . 0.958 no
C136 . H1362 . 0.970 no
N137 . C138 . 1.335(6) yes
N137 . H1371 . 0.851 no
C138 . O139 . 1.240(6) yes
N140 . C141 . 1.329(7) yes
N140 . C145 . 1.353(7) yes
N140 . Cu152 . 2.002(4) yes
C141 . C142 . 1.404(7) yes
C141 . H1411 . 0.934 no
C142 . C143 . 1.387(8) yes
C142 . H1421 . 0.922 no
C143 . C144 . 1.355(8) yes
C143 . H1431 . 0.929 no
C144 . C145 . 1.391(7) yes
C144 . H1441 . 0.927 no
C145 . C146 . 1.488(8) yes
C146 . C147 . 1.409(8) yes
C146 . N151 . 1.337(7) yes
C147 . C148 . 1.373(9) yes
C147 . H1471 . 0.923 no
C148 . C149 . 1.355(10) yes
C148 . H1481 . 0.938 no
C149 . C150 . 1.372(10) yes
C149 . H1491 . 0.936 no
C150 . N151 . 1.364(7) yes
C150 . H1501 . 0.921 no
N151 . Cu152 . 2.074(5) yes
O570 . Cl568 . 1.429(9) yes
O70 . Cl68 . 1.431(8) yes
O72 . Cl68 . 1.408(8) yes
O572 . Cl568 . 1.421(9) yes
O569 . Cl568 . 1.437(9) yes
O69 . Cl68 . 1.435(8) yes
Cl68 . O71 . 1.404(7) yes
O571 . Cl568 . 1.412(9) yes

loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 . C1 . C6 . 120.8(4) yes
C2 . C1 . H11 . 119.6 no
C6 . C1 . H11 . 119.6 no
C1 . C2 . C3 . 119.1(4) yes
C1 . C2 . C38 . 123.0(4) yes
C3 . C2 . C38 . 117.8(4) yes
C2 . C3 . C4 . 120.5(5) yes
C2 . C3 . H31 . 120.3 no
C4 . C3 . H31 . 119.2 no
C3 . C4 . C5 . 120.1(5) yes
C3 . C4 . H41 . 120.5 no
C5 . C4 . H41 . 119.4 no
C4 . C5 . C6 . 120.5(4) yes
C4 . C5 . H51 . 120.6 no
C6 . C5 . H51 . 118.8 no
C5 . C6 . C1 . 119.0(5) yes
C5 . C6 . C7 . 117.9(4) yes
C1 . C6 . C7 . 123.1(4) yes
C6 . C7 . O8 . 120.1(5) yes
C6 . C7 . N9 . 117.2(4) yes
O8 . C7 . N9 . 122.7(5) yes
C7 . N9 . C10 . 123.9(4) yes
C7 . N9 . H91 . 117.0 no
C10 . N9 . H91 . 117.2 no
N9 . C10 . C11 . 112.3(4) yes
N9 . C10 . H101 . 110.0 no
C11 . C10 . H101 . 107.4 no
N9 . C10 . H102 . 108.6 no
C11 . C10 . H102 . 109.2 no
H101 . C10 . H102 . 109.3 no
C10 . C11 . O12 . 107.5(4) yes
C10 . C11 . H112 . 108.8 no
O12 . C11 . H112 . 109.4 no
C10 . C11 . H111 . 110.8 no
O12 . C11 . H111 . 110.6 no
H112 . C11 . H111 . 109.7 no
C11 . O12 . C13 . 117.2(4) yes
O12 . C13 . C14 . 115.1(4) yes
O12 . C13 . C18 . 124.5(5) yes
C14 . C13 . C18 . 120.4(5) yes
C13 . C14 . C15 . 119.9(5) yes
C13 . C14 . H141 . 120.0 no
C15 . C14 . H141 . 120.1 no
C14 . C15 . C16 . 121.1(5) yes
C14 . C15 . H151 . 120.0 no
C16 . C15 . H151 . 118.9 no
C15 . C16 . C17 . 117.9(5) yes
C15 . C16 . C19 . 120.7(5) yes
C17 . C16 . C19 . 121.4(5) yes
C16 . C17 . C18 . 122.0(5) yes
C16 . C17 . H171 . 119.0 no
C18 . C17 . H171 . 119.0 no
C17 . C18 . C13 . 118.6(5) yes
C17 . C18 . H181 . 121.1 no
C13 . C18 . H181 . 120.3 no
C16 . C19 . N20 . 111.5(4) yes
C16 . C19 . H192 . 110.9 no
N20 . C19 . H192 . 108.6 no
C16 . C19 . H191 . 109.1 no
N20 . C19 . H191 . 107.7 no
H192 . C19 . H191 . 109.0 no
C19 . N20 . C21 . 110.9(4) yes
C19 . N20 . Cu52 . 115.0(3) yes
C21 . N20 . Cu52 . 105.1(3) yes
C19 . N20 . H201 . 108.3 no
C21 . N20 . H201 . 107.6 no
Cu52 . N20 . H201 . 109.8 no
N20 . C21 . C22 . 108.9(4) yes
N20 . C21 . H212 . 107.3 no
C22 . C21 . H212 . 109.1 no
N20 . C21 . H211 . 110.8 no
C22 . C21 . H211 . 110.2 no
H212 . C21 . H211 . 110.5 no
C21 . C22 . N23 . 110.6(4) yes
C21 . C22 . H221 . 110.0 no
N23 . C22 . H221 . 110.8 no
C21 . C22 . H222 . 108.6 no
N23 . C22 . H222 . 107.6 no
H221 . C22 . H222 . 109.2 no
C22 . N23 . C24 . 113.9(4) yes
C22 . N23 . Cu52 . 111.4(3) yes
C24 . N23 . Cu52 . 108.4(3) yes
C22 . N23 . H231 . 107.5 no
C24 . N23 . H231 . 107.9 no
Cu52 . N23 . H231 . 107.6 no
N23 . C24 . C25 . 108.3(4) yes
N23 . C24 . Cu52 . 42.1(2) yes
C25 . C24 . Cu52 . 76.0(3) yes
N23 . C24 . H241 . 114.1 no
C25 . C24 . H241 . 112.7 no
Cu52 . C24 . H241 . 104.1 no
N23 . C24 . H242 . 95.3 no
C25 . C24 . H242 . 101.5 no
Cu52 . C24 . H242 . 128.4 no
H241 . C24 . H242 . 122.9 no
C24 . C25 . N26 . 108.9(4) yes
C24 . C25 . H251 . 108.9 no
N26 . C25 . H251 . 110.2 no
C24 . C25 . H252 . 109.4 no
N26 . C25 . H252 . 109.7 no
H251 . C25 . H252 . 109.7 no
C25 . N26 . C27 . 111.2(4) yes
C25 . N26 . Cu52 . 102.6(3) yes
C27 . N26 . Cu52 . 121.0(3) yes
C25 . N26 . H261 . 107.2 no
C27 . N26 . H261 . 107.0 no
Cu52 . N26 . H261 . 107.0 no
N26 . C27 . C28 . 115.0(5) yes
N26 . C27 . H271 . 107.2 no
C28 . C27 . H271 . 107.3 no
N26 . C27 . H272 . 107.0 no
C28 . C27 . H272 . 109.5 no
H271 . C27 . H272 . 111.0 no
C27 . C28 . C29 . 120.5(5) yes
C27 . C28 . C33 . 122.5(5) yes
C29 . C28 . C33 . 116.9(5) yes
C28 . C29 . C30 . 122.6(5) yes
C28 . C29 . H291 . 119.6 no
C30 . C29 . H291 . 117.8 no
C29 . C30 . C31 . 119.6(5) yes
C29 . C30 . H301 . 119.6 no
C31 . C30 . H301 . 120.8 no
C30 . C31 . C32 . 118.7(5) yes
C30 . C31 . O34 . 125.5(4) yes
C32 . C31 . O34 . 115.8(4) yes
C31 . C32 . C33 . 120.9(5) yes
C31 . C32 . H321 . 118.6 no
C33 . C32 . H321 . 120.5 no
C28 . C33 . C32 . 121.3(5) yes
C28 . C33 . H331 . 119.0 no
C32 . C33 . H331 . 119.7 no
C31 . O34 . C35 . 117.5(4) yes
O34 . C35 . C36 . 107.6(4) yes
O34 . C35 . H352 . 110.6 no
C36 . C35 . H352 . 109.4 no
O34 . C35 . H351 . 110.3 no
C36 . C35 . H351 . 108.0 no
H352 . C35 . H351 . 110.9 no
C35 . C36 . N37 . 111.9(4) yes
C35 . C36 . H362 . 108.5 no
N37 . C36 . H362 . 108.6 no
C35 . C36 . H361 . 109.3 no
N37 . C36 . H361 . 109.1 no
H362 . C36 . H361 . 109.4 no
C36 . N37 . C38 . 124.4(4) yes
C36 . N37 . H371 . 114.1 no
C38 . N37 . H371 . 115.5 no
C2 . C38 . N37 . 116.9(4) yes
C2 . C38 . O39 . 120.4(4) yes
N37 . C38 . O39 . 122.7(4) yes
C41 . N40 . C45 . 118.1(5) yes
C41 . N40 . Cu52 . 125.0(4) yes
C45 . N40 . Cu52 . 116.9(4) yes
N40 . C41 . C42 . 123.3(7) yes
N40 . C41 . H411 . 118.2 no
C42 . C41 . H411 . 118.5 no
C41 . C42 . C43 . 117.6(7) yes
C41 . C42 . H421 . 120.6 no
C43 . C42 . H421 . 121.8 no
C42 . C43 . C44 . 121.2(7) yes
C42 . C43 . H431 . 119.4 no
C44 . C43 . H431 . 119.4 no
C43 . C44 . C45 . 118.6(6) yes
C43 . C44 . H441 . 120.8 no
C45 . C44 . H441 . 120.6 no
C44 . C45 . N40 . 121.1(6) yes
C44 . C45 . C46 . 124.6(5) yes
N40 . C45 . C46 . 114.2(5) yes
C45 . C46 . C47 . 122.8(6) yes
C45 . C46 . N51 . 116.7(4) yes
C47 . C46 . N51 . 120.4(6) yes
C46 . C47 . C48 . 118.4(7) yes
C46 . C47 . H471 . 120.7 no
C48 . C47 . H471 . 120.9 no
C47 . C48 . C49 . 122.2(6) yes
C47 . C48 . H481 . 118.8 no
C49 . C48 . H481 . 119.0 no
C48 . C49 . C50 . 117.1(7) yes
C48 . C49 . H491 . 122.2 no
C50 . C49 . H491 . 120.7 no
C49 . C50 . N51 . 121.5(7) yes
C49 . C50 . H501 . 119.3 no
N51 . C50 . H501 . 119.2 no
C46 . N51 . C50 . 120.3(5) yes
C46 . N51 . Cu52 . 111.8(4) yes
C50 . N51 . Cu52 . 127.5(4) yes
N26 . Cu52 . N51 . 104.53(16) yes
N26 . Cu52 . N20 . 118.67(16) yes
N51 . Cu52 . N20 . 136.78(16) yes
N26 . Cu52 . N23 . 84.22(17) yes
N51 . Cu52 . N23 . 99.69(18) yes
N20 . Cu52 . N23 . 84.01(17) yes
N26 . Cu52 . N40 . 98.03(17) yes
N51 . Cu52 . N40 . 79.9(2) yes
N20 . Cu52 . N40 . 94.75(17) yes
N23 . Cu52 . N40 . 177.75(17) yes
N26 . Cu52 . C24 . 55.66(17) yes
N51 . Cu52 . C24 . 98.47(19) yes
N20 . Cu52 . C24 . 104.24(17) yes
N23 . Cu52 . C24 . 29.53(17) yes
N40 . Cu52 . C24 . 152.68(17) yes
O54 . Cl53 . O55 . 109.8(3) yes
O54 . Cl53 . O56 . 109.0(3) yes
O55 . Cl53 . O56 . 108.3(3) yes
O54 . Cl53 . O57 . 110.3(3) yes
O55 . Cl53 . O57 . 109.8(3) yes
O56 . Cl53 . O57 . 109.6(3) yes
O59 . Cl58 . O60 . 110.5(3) yes
O59 . Cl58 . O61 . 111.0(3) yes
O60 . Cl58 . O61 . 109.6(3) yes
O59 . Cl58 . O62 . 108.9(3) yes
O60 . Cl58 . O62 . 108.2(3) yes
O61 . Cl58 . O62 . 108.6(3) yes
O64 . Cl63 . O65 . 110.9(4) yes
O64 . Cl63 . O66 . 112.5(4) yes
O65 . Cl63 . O66 . 107.8(3) yes
O64 . Cl63 . O67 . 109.4(3) yes
O65 . Cl63 . O67 . 107.4(3) yes
O66 . Cl63 . O67 . 108.8(4) yes
C74 . C73 . H731 . 108.6 no
C74 . C73 . H732 . 109.6 no
H731 . C73 . H732 . 109.3 no
C74 . C73 . H733 . 108.6 no
H731 . C73 . H733 . 110.2 no
H732 . C73 . H733 . 110.4 no
C73 . C74 . N75 . 177.5(10) yes
C77 . C76 . H761 . 109.5 no
C77 . C76 . H762 . 109.1 no
H761 . C76 . H762 . 109.5 no
C77 . C76 . H763 . 109.0 no
H761 . C76 . H763 . 109.6 no
H762 . C76 . H763 . 110.1 no
C76 . C77 . N78 . 179.8(7) yes
C80 . C79 . H793 . 107.8 no
C80 . C79 . H791 . 108.7 no
H793 . C79 . H791 . 111.2 no
C80 . C79 . H792 . 108.6 no
H793 . C79 . H792 . 110.5 no
H791 . C79 . H792 . 109.9 no
C79 . C80 . N81 . 178.9(8) yes
C102 . C101 . C106 . 120.6(4) yes
C102 . C101 . H1011 . 120.3 no
C106 . C101 . H1011 . 119.1 no
C101 . C102 . C103 . 119.5(4) yes
C101 . C102 . C138 . 121.1(4) yes
C103 . C102 . C138 . 119.4(4) yes
C102 . C103 . C104 . 120.1(5) yes
C102 . C103 . H1031 . 119.9 no
C104 . C103 . H1031 . 120.0 no
C103 . C104 . C105 . 119.9(5) yes
C103 . C104 . H1041 . 119.6 no
C105 . C104 . H1041 . 120.5 no
C104 . C105 . C106 . 121.3(5) yes
C104 . C105 . H1051 . 118.9 no
C106 . C105 . H1051 . 119.8 no
C101 . C106 . C105 . 118.6(5) yes
C101 . C106 . C107 . 123.2(4) yes
C105 . C106 . C107 . 118.2(4) yes
C106 . C107 . O108 . 120.3(5) yes
C106 . C107 . N109 . 117.4(4) yes
O108 . C107 . N109 . 122.3(5) yes
C107 . N109 . C110 . 124.1(4) yes
C107 . N109 . H1091 . 117.2 no
C110 . N109 . H1091 . 116.6 no
N109 . C110 . C111 . 112.4(4) yes
N109 . C110 . H1101 . 108.2 no
C111 . C110 . H1101 . 108.6 no
N109 . C110 . H1102 . 108.2 no
C111 . C110 . H1102 . 109.5 no
H1101 . C110 . H1102 . 109.9 no
C110 . C111 . O112 . 108.1(4) yes
C110 . C111 . H1111 . 109.8 no
O112 . C111 . H1111 . 109.1 no
C110 . C111 . H1112 . 110.3 no
O112 . C111 . H1112 . 110.5 no
H1111 . C111 . H1112 . 109.0 no
C111 . O112 . C113 . 117.5(4) yes
O112 . C113 . C114 . 125.6(4) yes
O112 . C113 . C118 . 115.5(4) yes
C114 . C113 . C118 . 118.9(5) yes
C113 . C114 . C115 . 119.3(5) yes
C113 . C114 . H1141 . 121.0 no
C115 . C114 . H1141 . 119.7 no
C114 . C115 . C116 . 122.3(5) yes
C114 . C115 . H1151 . 118.1 no
C116 . C115 . H1151 . 119.5 no
C115 . C116 . C117 . 117.9(5) yes
C115 . C116 . C119 . 121.3(5) yes
C117 . C116 . C119 . 120.9(5) yes
C116 . C117 . C118 . 120.8(5) yes
C116 . C117 . H1171 . 120.5 no
C118 . C117 . H1171 . 118.7 no
C113 . C118 . C117 . 120.7(5) yes
C113 . C118 . H1181 . 119.6 no
C117 . C118 . H1181 . 119.6 no
C116 . C119 . N120 . 112.0(4) yes
C116 . C119 . H1191 . 109.3 no
N120 . C119 . H1191 . 108.5 no
C116 . C119 . H1192 . 109.4 no
N120 . C119 . H1192 . 107.3 no
H1191 . C119 . H1192 . 110.3 no
C119 . N120 . C121 . 110.8(5) yes
C119 . N120 . Cu152 . 118.0(3) yes
C121 . N120 . Cu152 . 102.4(4) yes
C119 . N120 . H1201 . 107.9 no
C121 . N120 . H1201 . 109.0 no
Cu152 . N120 . H1201 . 108.5 no
N120 . C121 . C122 . 105.0(5) yes
N120 . C121 . Cu152 . 45.9(3) yes
C122 . C121 . Cu152 . 72.6(4) yes
N120 . C121 . H1212 . 91.7 no
C122 . C121 . H1212 . 102.5 no
Cu152 . C121 . H1212 . 129.7 no
N120 . C121 . H1211 . 117.5 no
C122 . C121 . H1211 . 109.3 no
Cu152 . C121 . H1211 . 99.3 no
H1212 . C121 . H1211 . 127.8 no
C121 . C122 . N123 . 106.7(6) yes
C121 . C122 . H1221 . 112.1 no
N123 . C122 . H1221 . 111.1 no
C121 . C122 . H1222 . 109.0 no
N123 . C122 . H1222 . 109.9 no
H1221 . C122 . H1222 . 108.0 no
C122 . N123 . C124 . 122.1(6) yes
C122 . N123 . Cu152 . 106.0(4) yes
C124 . N123 . Cu152 . 109.2(4) yes
C122 . N123 . H1231 . 106.9 no
C124 . N123 . H1231 . 104.5 no
Cu152 . N123 . H1231 . 107.4 no
N123 . C124 . C125 . 112.2(5) yes
N123 . C124 . H1241 . 109.8 no
C125 . C124 . H1241 . 110.6 no
N123 . C124 . H1242 . 106.2 no
C125 . C124 . H1242 . 108.7 no
H1241 . C124 . H1242 . 109.2 no
C124 . C125 . N126 . 107.2(5) yes
C124 . C125 . H1251 . 106.6 no
N126 . C125 . H1251 . 109.1 no
C124 . C125 . H1252 . 111.1 no
N126 . C125 . H1252 . 110.2 no
H1251 . C125 . H1252 . 112.5 no
C125 . N126 . C127 . 112.5(5) yes
C125 . N126 . Cu152 . 103.3(4) yes
C127 . N126 . Cu152 . 114.9(3) yes
C125 . N126 . H1261 . 108.8 no
C127 . N126 . H1261 . 108.7 no
Cu152 . N126 . H1261 . 108.4 no
N126 . C127 . C128 . 111.4(4) yes
N126 . C127 . H1271 . 108.6 no
C128 . C127 . H1271 . 110.3 no
N126 . C127 . H1272 . 106.6 no
C128 . C127 . H1272 . 109.3 no
H1271 . C127 . H1272 . 110.6 no
C127 . C128 . C129 . 121.0(5) yes
C127 . C128 . C133 . 121.2(5) yes
C129 . C128 . C133 . 117.8(5) yes
C128 . C129 . C130 . 120.7(5) yes
C128 . C129 . H1291 . 119.8 no
C130 . C129 . H1291 . 119.5 no
C129 . C130 . C131 . 120.9(5) yes
C129 . C130 . H1301 . 118.9 no
C131 . C130 . H1301 . 120.1 no
C130 . C131 . C132 . 120.2(4) yes
C130 . C131 . O134 . 115.1(4) yes
C132 . C131 . O134 . 124.7(4) yes
C131 . C132 . C133 . 118.2(5) yes
C131 . C132 . H1321 . 121.5 no
C133 . C132 . H1321 . 120.3 no
C132 . C133 . C128 . 122.2(5) yes
C132 . C133 . H1331 . 118.2 no
C128 . C133 . H1331 . 119.5 no
C131 . O134 . C135 . 118.5(4) yes
O134 . C135 . C136 . 106.4(4) yes
O134 . C135 . H1351 . 110.1 no
C136 . C135 . H1351 . 110.2 no
O134 . C135 . H1352 . 110.9 no
C136 . C135 . H1352 . 108.9 no
H1351 . C135 . H1352 . 110.3 no
C135 . C136 . N137 . 111.6(4) yes
C135 . C136 . H1361 . 107.1 no
N137 . C136 . H1361 . 109.3 no
C135 . C136 . H1362 . 108.4 no
N137 . C136 . H1362 . 109.7 no
H1361 . C136 . H1362 . 110.7 no
C136 . N137 . C138 . 123.9(4) yes
C136 . N137 . H1371 . 113.2 no
C138 . N137 . H1371 . 114.3 no
C102 . C138 . N137 . 115.7(4) yes
C102 . C138 . O139 . 121.1(4) yes
N137 . C138 . O139 . 123.3(4) yes
C141 . N140 . C145 . 119.5(4) yes
C141 . N140 . Cu152 . 125.6(4) yes
C145 . N140 . Cu152 . 115.0(3) yes
N140 . C141 . C142 . 122.0(5) yes
N140 . C141 . H1411 . 118.7 no
C142 . C141 . H1411 . 119.3 no
C141 . C142 . C143 . 117.4(5) yes
C141 . C142 . H1421 . 119.6 no
C143 . C142 . H1421 . 122.9 no
C142 . C143 . C144 . 120.9(5) yes
C142 . C143 . H1431 . 119.3 no
C144 . C143 . H1431 . 119.8 no
C143 . C144 . C145 . 118.8(5) yes
C143 . C144 . H1441 . 120.1 no
C145 . C144 . H1441 . 121.0 no
C144 . C145 . N140 . 121.4(5) yes
C144 . C145 . C146 . 122.8(5) yes
N140 . C145 . C146 . 115.8(4) yes
C145 . C146 . C147 . 123.4(5) yes
C145 . C146 . N151 . 114.8(5) yes
C147 . C146 . N151 . 121.9(5) yes
C146 . C147 . C148 . 118.7(6) yes
C146 . C147 . H1471 . 120.9 no
C148 . C147 . H1471 . 120.4 no
C147 . C148 . C149 . 120.1(7) yes
C147 . C148 . H1481 . 120.1 no
C149 . C148 . H1481 . 119.8 no
C148 . C149 . C150 . 118.7(6) yes
C148 . C149 . H1491 . 121.2 no
C150 . C149 . H1491 . 120.1 no
C149 . C150 . N151 . 123.4(6) yes
C149 . C150 . H1501 . 119.2 no
N151 . C150 . H1501 . 117.4 no
C150 . N151 . C146 . 117.1(5) yes
C150 . N151 . Cu152 . 129.0(4) yes
C146 . N151 . Cu152 . 113.8(4) yes
N126 . Cu152 . N120 . 127.00(18) yes
N126 . Cu152 . N151 . 117.77(17) yes
N120 . Cu152 . N151 . 115.24(17) yes
N126 . Cu152 . N123 . 82.9(2) yes
N120 . Cu152 . N123 . 86.6(2) yes
N151 . Cu152 . N123 . 102.1(3) yes
N126 . Cu152 . N140 . 92.35(17) yes
N120 . Cu152 . N140 . 95.82(18) yes
N151 . Cu152 . N140 . 80.61(17) yes
N123 . Cu152 . N140 . 175.2(2) yes
N126 . Cu152 . C121 . 107.9(2) yes
N120 . Cu152 . C121 . 31.7(2) yes
N151 . Cu152 . C121 . 126.6(2) yes
N123 . Cu152 . C121 . 56.6(3) yes
N140 . Cu152 . C121 . 124.9(2) yes
O69 . Cl68 . O70 . 106.0(8) yes
O69 . Cl68 . O72 . 107.9(10) yes
O70 . Cl68 . O72 . 111.3(9) yes
O69 . Cl68 . O71 . 114.0(9) yes
O70 . Cl68 . O71 . 108.1(8) yes
O72 . Cl68 . O71 . 109.5(9) yes
O569 . Cl568 . O570 . 111.4(11) yes
O569 . Cl568 . O572 . 113.8(13) yes
O570 . Cl568 . O572 . 107.9(13) yes
O569 . Cl568 . O571 . 107.3(13) yes
O570 . Cl568 . O571 . 106.7(12) yes
O572 . Cl568 . O571 . 109.6(13) yes

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C1 . H11 . O56 . 165.33 0.940 2.509 3.426(8) yes
C4 . H41 . O71 2_666 124.5 0.934 2.593 3.216(8) yes
C15 . H151 . O72 2_566 150.6 0.937 2.563 3.410(8) yes
C15 . H151 . O569 2_566 150.6 0.937 2.497 3.346(8) yes
C44 . H441 . O56 . 171.47 0.921 2.562 3.476(8) yes
C79 . H793 . O57 1_565 166.27 0.951 2.476 3.407(8) yes
C79 . H791 . O108 2_677 153.45 0.956 2.513 3.395(8) yes
C101 . H1011 . O62 . 156.21 0.934 2.471 3.346(8) yes
C110 . H1102 . N78 . 160.94 0.977 2.499 3.437(8) yes
C117 . H1171 . O65 2_767 158.24 0.942 2.542 3.434(8) yes
C119 . H1192 . O39 1_655 174.32 0.977 2.587 3.560(8) yes
C122 . H1222 . O39 1_655 170.0 0.989 2.536 3.514(8) yes
C129 . H1291 . O57 1_665 157.02 0.931 2.595 3.471(8) yes
C141 . H1411 . O67 2_767 160.07 0.934 2.465 3.358(8) yes
C147 . H1471 . O62 . 177.47 0.923 2.516 3.438(8) yes
N109 . H1091 . O62 . 141.23 0.854 2.419 3.131(8) yes
N9 . H91 . O54 . 146.83 0.849 2.343 3.089(8) yes
N137 . H1371 . O60 . 137.19 0.851 2.301 2.982(8) yes
N37 . H371 . O56 . 148.98 0.869 2.341 3.118(8) yes
N20 . H201 . O569 2_566 159.1 0.882 2.442 3.281(8) yes
N23 . H231 . O139 1_445 145.73 0.889 2.093 2.871(8) yes
N26 . H261 . N75 1_455 139.16 0.877 2.313 3.032(8) yes
N126 . H1261 . O57 1_665 146.87 0.914 2.201 3.009(8) yes
N123 . H1231 . O70 1_655 150.4 0.907 2.307 3.128(8) yes
N120 . H1201 . O65 2_767 152.04 0.904 2.340 3.167(8) yes
C73 . H731 . O571 . 136.1 0.957 2.363 3.124(8) yes
C73 . H732 . O60 . 128.8 0.962 2.569 3.259(8) yes
C73 . H733 . O571 2_666 131.3 0.962 2.500 3.217(8) yes

_iucr_refine_instruction_details_constraints 
;
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
EQUIVALENCE PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
RIDE CL(68, U'S) CL(568, U'S) 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE N   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) H   ( 102,X'S) 
RIDE C   (  11,X'S) H   ( 112,X'S) H   ( 111,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 192,X'S) H   ( 191,X'S) 
RIDE N   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 212,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE N   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) 
RIDE N   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  35,X'S) H   ( 352,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 362,X'S) H   ( 361,X'S) 
RIDE N   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) H   ( 732,X'S) H   ( 733,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) H   ( 762,X'S) H   ( 763,X'S) 
RIDE C   (  79,X'S) H   ( 793,X'S) H   ( 791,X'S) H   ( 792,X'S) 
RIDE C   ( 101,X'S) H   (1011,X'S) 
RIDE C   ( 103,X'S) H   (1031,X'S) 
RIDE C   ( 104,X'S) H   (1041,X'S) 
RIDE C   ( 105,X'S) H   (1051,X'S) 
RIDE N   ( 109,X'S) H   (1091,X'S) 
RIDE C   ( 110,X'S) H   (1101,X'S) H   (1102,X'S) 
RIDE C   ( 111,X'S) H   (1111,X'S) H   (1112,X'S) 
RIDE C   ( 114,X'S) H   (1141,X'S) 
RIDE C   ( 115,X'S) H   (1151,X'S) 
RIDE C   ( 117,X'S) H   (1171,X'S) 
RIDE C   ( 118,X'S) H   (1181,X'S) 
RIDE C   ( 119,X'S) H   (1191,X'S) H   (1192,X'S) 
RIDE N   ( 120,X'S) H   (1201,X'S) 
RIDE C   ( 121,X'S) H   (1212,X'S) H   (1211,X'S) 
RIDE C   ( 122,X'S) H   (1221,X'S) H   (1222,X'S) 
RIDE N   ( 123,X'S) H   (1231,X'S) 
RIDE C   ( 124,X'S) H   (1241,X'S) H   (1242,X'S) 
RIDE C   ( 125,X'S) H   (1251,X'S) H   (1252,X'S) 
RIDE N   ( 126,X'S) H   (1261,X'S) 
RIDE C   ( 127,X'S) H   (1271,X'S) H   (1272,X'S) 
RIDE C   ( 129,X'S) H   (1291,X'S) 
RIDE C   ( 130,X'S) H   (1301,X'S) 
RIDE C   ( 132,X'S) H   (1321,X'S) 
RIDE C   ( 133,X'S) H   (1331,X'S) 
RIDE C   ( 135,X'S) H   (1351,X'S) H   (1352,X'S) 
RIDE C   ( 136,X'S) H   (1361,X'S) H   (1362,X'S) 
RIDE N   ( 137,X'S) H   (1371,X'S) 
RIDE C   ( 141,X'S) H   (1411,X'S) 
RIDE C   ( 142,X'S) H   (1421,X'S) 
RIDE C   ( 143,X'S) H   (1431,X'S) 
RIDE C   ( 144,X'S) H   (1441,X'S) 
RIDE C   ( 147,X'S) H   (1471,X'S) 
RIDE C   ( 148,X'S) H   (1481,X'S) 
RIDE C   ( 149,X'S) H   (1491,X'S) 
RIDE C   ( 150,X'S) H   (1501,X'S) 
END                                                                             
;

_iucr_refine_instruction_details_restraints 
;
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM PERCHLORATES 
DISTANCE 0, 0.01 = MEAN CL(68) TO O(69) CL(68) TO O(70) 
CONT CL(68) TO O(71) CL(68) TO O(72) CL(58) TO O(59) 
CONT CL(568) TO O(572) CL(568) TO O(570) 
CONT CL(568) TO O(569) CL(568) TO O(571) 
CONT CL(58) TO O(60) CL(58) TO O(61) CL(58) TO O(62) 
CONT CL(53) TO O(54) CL(53) TO O(55) CL(53) TO O(56) 
CONT CL(53) TO O(57) CL(63) TO O(64) CL(63) TO O(65) 
CONT CL(63) TO O(66) CL(63) TO O(67) 
ANGLE 109,2 = O(69) TO CL(68) TO O(70) 
CONT O(69) TO CL(68) TO O(70) O(69) TO CL(68) TO O(71) 
CONT O(69) TO CL(68) TO O(72) O(70) TO CL(68) TO O(71) 
CONT O(70) TO CL(68) TO O(72) O(71) TO CL(68) TO O(72) 
CONT O(569) TO CL(568) TO O(570) 
CONT O(569) TO CL(568) TO O(570) O(569) TO CL(568) TO O(571) 
CONT O(569) TO CL(568) TO O(572) O(570) TO CL(568) TO O(571) 
CONT O(570) TO CL(568) TO O(572) O(571) TO CL(568) TO O(572) 
SIMU 0.04 O(69) CL(68) O(70) 
SIMU 0.04 O(69) CL(68) O(71) 
SIMU 0.04 O(69) CL(68) O(72) 
SIMU 0.04 O(70) CL(68) O(71) 
SIMU 0.04 O(70) CL(68) O(72) 
SIMU 0.04 O(71) CL(68) O(72) 
DELU 0.01 O(69) CL(68) O(70) 
DELU 0.01 O(69) CL(68) O(71) 
DELU 0.01 O(69) CL(68) O(72) 
DELU 0.01 O(70) CL(68) O(71) 
DELU 0.01 O(70) CL(68) O(72) 
DELU 0.01 O(71) CL(68) O(72) 
SIMU 0.04 O(569) CL(568) O(570) 
SIMU 0.04 O(569) CL(568) O(571) 
SIMU 0.04 O(569) CL(568) O(572) 
SIMU 0.04 O(570) CL(568) O(571) 
SIMU 0.04 O(570) CL(568) O(572) 
SIMU 0.04 O(571) CL(568) O(572) 
DELU 0.01 O(569) CL(568) O(570) 
DELU 0.01 O(569) CL(568) O(571) 
DELU 0.01 O(569) CL(568) O(572) 
DELU 0.01 O(570) CL(568) O(571) 
DELU 0.01 O(570) CL(568) O(572) 
DELU 0.01 O(571) CL(568) O(572) 
REM ACETONITRILES 
DISTANCE 1.44, 0.01 = C(76) TO C(77) C(73) TO C(74) 
CONT C(79) TO C(80) 
DISTANCE 1.14, 0.01 = C(74) TO N(75) 
CONT C(77) TO N(78) C(80) TO N(81) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = CL(53) TO O(54) 
VIBR .0, 0.00200 = CL(53) TO O(55) 
VIBR .0, 0.00200 = CL(53) TO O(56) 
VIBR .0, 0.00200 = CL(53) TO O(57) 
VIBR .0, 0.00500 = O(55) TO O(54) 
VIBR .0, 0.00500 = O(56) TO O(54) 
VIBR .0, 0.00500 = O(56) TO O(55) 
VIBR .0, 0.00500 = O(57) TO O(54) 
VIBR .0, 0.00500 = O(57) TO O(55) 
VIBR .0, 0.00500 = O(57) TO O(56) 
VIBR .0, 0.00200 = CL(58) TO O(59) 
VIBR .0, 0.00200 = CL(58) TO O(60) 
VIBR .0, 0.00200 = CL(58) TO O(61) 
VIBR .0, 0.00200 = CL(58) TO O(62) 
VIBR .0, 0.00500 = O(60) TO O(59) 
VIBR .0, 0.00500 = O(61) TO O(59) 
VIBR .0, 0.00500 = O(61) TO O(60) 
VIBR .0, 0.00500 = O(62) TO O(59) 
VIBR .0, 0.00500 = O(62) TO O(60) 
VIBR .0, 0.00500 = O(62) TO O(61) 
VIBR .0, 0.00200 = CL(63) TO O(64) 
VIBR .0, 0.00200 = CL(63) TO O(65) 
VIBR .0, 0.00200 = CL(63) TO O(66) 
VIBR .0, 0.00200 = CL(63) TO O(67) 
VIBR .0, 0.00500 = O(65) TO O(64) 
VIBR .0, 0.00500 = O(66) TO O(64) 
VIBR .0, 0.00500 = O(66) TO O(65) 
VIBR .0, 0.00500 = O(67) TO O(64) 
VIBR .0, 0.00500 = O(67) TO O(65) 
VIBR .0, 0.00500 = O(67) TO O(66) 
VIBR .0, 0.00200 = CL(68) TO O(71) 
VIBR .0, 0.00200 = CL(68) TO O(70) 
VIBR .0, 0.00200 = CL(68) TO O(72) 
VIBR .0, 0.00200 = CL(68) TO O(69) 
VIBR .0, 0.00500 = O(70) TO O(71) 
VIBR .0, 0.00500 = O(72) TO O(71) 
VIBR .0, 0.00500 = O(72) TO O(70) 
VIBR .0, 0.00500 = O(69) TO O(71) 
VIBR .0, 0.00500 = O(69) TO O(70) 
VIBR .0, 0.00500 = O(69) TO O(72) 
VIBR .0, 0.00200 = CL(568) TO O(570) 
VIBR .0, 0.00200 = CL(568) TO O(571) 
VIBR .0, 0.00200 = CL(568) TO O(572) 
VIBR .0, 0.00200 = CL(568) TO O(569) 
VIBR .0, 0.00500 = O(572) TO O(570) 
VIBR .0, 0.00500 = O(571) TO O(570) 
VIBR .0, 0.00500 = O(569) TO O(570) 
VIBR .0, 0.00500 = O(569) TO O(571) 
VIBR .0, 0.00500 = O(569) TO O(572) 
VIBR .0, 0.00500 = O(571) TO O(572) 
VIBR .0, 0.00200 = C(73) TO C(74) 
VIBR .0, 0.00200 = C(74) TO N(75) 
VIBR .0, 0.00500 = N(75) TO C(73) 
VIBR .0, 0.00200 = C(76) TO C(77) 
VIBR .0, 0.00200 = C(77) TO N(78) 
VIBR .0, 0.00500 = N(78) TO C(76) 
VIBR .0, 0.00200 = C(79) TO C(80) 
VIBR .0, 0.00200 = C(80) TO N(81) 
VIBR .0, 0.00500 = N(81) TO C(79) 
VIBR .0, 0.00200 = C(116) TO C(119) 
VIBR .0, 0.00500 = C(117) TO C(115) 
VIBR .0, 0.00500 = C(119) TO C(115) 
VIBR .0, 0.00500 = C(119) TO C(117) 
VIBR .0, 0.00200 = C(117) TO C(118) 
VIBR .0, 0.00500 = C(118) TO C(116) 
VIBR .0, 0.00500 = C(113) TO C(117) 
VIBR .0, 0.00200 = C(119) TO N(120) 
VIBR .0, 0.00500 = N(120) TO C(116) 
VIBR .0, 0.00200 = N(120) TO C(121) 
VIBR .0, 0.00200 = N(120) TO CU(152) 
VIBR .0, 0.00500 = C(121) TO C(119) 
VIBR .0, 0.00500 = CU(152) TO C(119) 
VIBR .0, 0.00500 = CU(152) TO C(121) 
VIBR .0, 0.00200 = C(121) TO C(122) 
VIBR .0, 0.00500 = C(122) TO N(120) 
VIBR .0, 0.00200 = C(122) TO N(123) 
VIBR .0, 0.00200 = C(122) TO CU(152) 
VIBR .0, 0.00500 = N(123) TO C(121) 
VIBR .0, 0.00500 = CU(152) TO C(121) 
VIBR .0, 0.00500 = CU(152) TO N(123) 
VIBR .0, 0.00200 = N(123) TO C(124) 
VIBR .0, 0.00200 = N(123) TO CU(152) 
VIBR .0, 0.00500 = C(124) TO C(122) 
VIBR .0, 0.00500 = CU(152) TO C(122) 
VIBR .0, 0.00500 = CU(152) TO C(124) 
VIBR .0, 0.00200 = C(124) TO C(125) 
VIBR .0, 0.00500 = C(125) TO N(123) 
VIBR .0, 0.00200 = C(125) TO N(126) 
VIBR .0, 0.00200 = C(125) TO CU(152) 
VIBR .0, 0.00500 = N(126) TO C(124) 
VIBR .0, 0.00500 = CU(152) TO C(124) 
VIBR .0, 0.00500 = CU(152) TO N(126) 
VIBR .0, 0.00200 = N(126) TO C(127) 
VIBR .0, 0.00200 = N(126) TO CU(152) 
VIBR .0, 0.00500 = C(127) TO C(125) 
VIBR .0, 0.00500 = CU(152) TO C(125) 
VIBR .0, 0.00500 = CU(152) TO C(127) 
VIBR .0, 0.00200 = C(127) TO C(128) 
VIBR .0, 0.00500 = C(128) TO N(126) 
VIBR .0, 0.00200 = C(128) TO C(129) 
VIBR .0, 0.00200 = C(128) TO C(133) 
VIBR .0, 0.00500 = C(129) TO C(127) 
VIBR .0, 0.00500 = C(133) TO C(127) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.08000 = CL(53) TO O(54) 
U(IJ) .0, 0.08000 = CL(53) TO O(55) 
U(IJ) .0, 0.08000 = CL(53) TO O(56) 
U(IJ) .0, 0.08000 = CL(53) TO O(57) 
U(IJ) .0, 0.08000 = CL(58) TO O(59) 
U(IJ) .0, 0.08000 = CL(58) TO O(60) 
U(IJ) .0, 0.08000 = CL(58) TO O(61) 
U(IJ) .0, 0.08000 = CL(58) TO O(62) 
U(IJ) .0, 0.08000 = CL(63) TO O(64) 
U(IJ) .0, 0.08000 = CL(63) TO O(65) 
U(IJ) .0, 0.08000 = CL(63) TO O(66) 
U(IJ) .0, 0.08000 = CL(63) TO O(67) 
U(IJ) .0, 0.08000 = CL(68) TO O(71) 
U(IJ) .0, 0.08000 = CL(68) TO O(70) 
U(IJ) .0, 0.08000 = CL(68) TO O(72) 
U(IJ) .0, 0.08000 = CL(68) TO O(69) 
U(IJ) .0, 0.08000 = CL(568) TO O(570) 
U(IJ) .0, 0.08000 = CL(568) TO O(571) 
U(IJ) .0, 0.08000 = CL(568) TO O(572) 
U(IJ) .0, 0.08000 = CL(568) TO O(569) 
U(IJ) .0, 0.08000 = C(73) TO C(74) 
U(IJ) .0, 0.08000 = C(74) TO N(75) 
U(IJ) .0, 0.08000 = C(76) TO C(77) 
U(IJ) .0, 0.08000 = C(77) TO N(78) 
U(IJ) .0, 0.08000 = C(79) TO C(80) 
U(IJ) .0, 0.08000 = C(80) TO N(81) 
U(IJ) .0, 0.04000 = C(119) TO N(120) 
U(IJ) .0, 0.04000 = N(120) TO C(121) 
U(IJ) .0, 0.04000 = N(120) TO CU(152) 
U(IJ) .0, 0.04000 = C(121) TO C(122) 
U(IJ) .0, 0.04000 = C(122) TO N(123) 
U(IJ) .0, 0.04000 = C(122) TO CU(152) 
U(IJ) .0, 0.04000 = N(123) TO C(124) 
U(IJ) .0, 0.04000 = N(123) TO CU(152) 
U(IJ) .0, 0.04000 = C(124) TO C(125) 
U(IJ) .0, 0.04000 = C(125) TO N(126) 
U(IJ) .0, 0.04000 = C(125) TO CU(152) 
U(IJ) .0, 0.04000 = N(126) TO C(127) 
U(IJ) .0, 0.04000 = N(126) TO CU(152) 
U(IJ) .0, 0.04000 = C(127) TO C(128) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
-2 3 2 x .
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile, di-isopropyl ether'
####################################################################### 
# 
# 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_pseudorotaxane-3-9-Cu2ClO4
_database_code_depnum_ccdc_archive 'CCDC 1560766'
_audit_update_record             
;
2017-07-06 deposited with the CCDC.
2017-09-12 downloaded from the CCDC.
;
#==============================================================================
# start Validation Reply Form
_vrf_PLAT029_3.9.CuClO42         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.930 Note  
RESPONSE: The crystals were of low quality and diffracted poorly.
Synchrotron radiation was used, but despite this the diffraction was weak. The
crystal also suffered radiation damage leading to poor completeness.  Despite 
this, there is little doubt that the connectivity is correct and that the data 
supports the general conclusions in the manuscript.
;
_vrf_PLAT414_3.9.CuClO42         
;
PROBLEM: Short Intra D-H..H-X       H231   ..  H241    ..       1.89 Ang.  
RESPONSE: This close contact is between CH and NH hydrogen atoms of the 
macrocycle tris-amine group. The conformaton of the tris-amine group is
presumably constricted as a result of coordination to the copper(II) cation.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;

_refine_special_details          
; 
Some disorder was identified in one of the side-arms of the 4-iodopyridine threading component, and
in one of the perchlorate counteranions. For these parts of the strucutre, restraints to bond lengths
and angles, as well as thermal and vibrational restraints were used to ensure a physically reasonable
model and maintain sensible anisotropic displacement ellipsoids. In addition, the disorder in the
side-arm was modelled using refined partial occupancies over two positions. C-H hydrogen atoms were 
visible in the Fourier difference map and were initially initially positioned geometrically, before being
refined with restraints on bond lengths and angles, after which the positions were used as the basis for a 
riding model. The N-H hydrogen atoms were visible in the Fourier difference map and were refined with 
restraints on bond lengths and angles.
;

_cell_length_a                   11.8265(3)
_cell_length_b                   12.4818(3)
_cell_length_c                   19.5954(5)
_cell_angle_alpha                72.764(2)
_cell_angle_beta                 89.197(2)
_cell_angle_gamma                68.746(2)
_cell_volume                     2560.57(12)

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
I -0.7740 1.7190 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776
4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cu 0.2710 1.2020 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126
1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0070 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1250 0.1500 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'

_cell_formula_units_Z            2

_chemical_formula_sum            'C45 H59 Cl2 Cu1 I1 N8 O18'
_chemical_formula_moiety         'C45 H59  Cu1 I1 N8 O10, 2(Cl O4)'
_chemical_compound_source        synthesised
_chemical_formula_weight         1261.36

_cell_measurement_reflns_used    17507
_cell_measurement_theta_min      2
_cell_measurement_theta_max      27
_cell_measurement_temperature    100

_exptl_crystal_description       block
_exptl_crystal_colour            'pale blue'
_exptl_crystal_size_min          0.02
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_max          0.05

_exptl_crystal_density_diffrn    1.636
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1290
_exptl_absorpt_coefficient_mu    1.216

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_T_max  1.000
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_device       'CrystalLogic Kappa (3 circle)'
_diffrn_radiation_monochromator  Synchrotron
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_measurement_method       'profile data from ω-scans'

_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      100
_diffrn_reflns_number            36137
_reflns_number_total             11094
_diffrn_reflns_av_R_equivalents  0.047

_diffrn_reflns_theta_min         1.770
_diffrn_reflns_theta_max         27.263
_diffrn_measured_fraction_theta_max 0.879

_diffrn_reflns_theta_full        25.082
_diffrn_measured_fraction_theta_full 0.930

_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_reflns_limit_h_min              -15
_reflns_limit_h_max              15
_reflns_limit_k_min              -14
_reflns_limit_k_max              16
_reflns_limit_l_min              0
_reflns_limit_l_max              25

_oxford_diffrn_Wilson_B_factor   2.75
_oxford_diffrn_Wilson_scale      0.11

_atom_sites_solution_primary     Other
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.06
_refine_diff_density_max         1.49

_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         9329
_refine_ls_number_restraints     202
_refine_ls_number_parameters     695
_oxford_refine_ls_R_factor_ref   0.0449
_refine_ls_wR_factor_ref         0.1080
_refine_ls_goodness_of_fit_ref   0.9513
_refine_ls_shift/su_max          0.0018934
_refine_ls_shift/su_mean         0.0000377

_oxford_reflns_number_all        9329
_refine_ls_R_factor_all          0.0449
_refine_ls_wR_factor_all         0.1080

_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                8502
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_gt          0.1041

_chemical_absolute_configuration .

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr

_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.198E+04 0.330E+04 0.205E+04 875. 205. 
;

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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 0.7871(3) 1.0474(3) 0.44471(16) 0.0291 1.0000 Uani . . . . . .
C2 C 0.7726(3) 1.1665(3) 0.40876(16) 0.0299 1.0000 Uani . . . . . .
C3 C 0.8135(3) 1.2309(3) 0.44281(17) 0.0325 1.0000 Uani . . . . . .
C4 C 0.8685(3) 1.1779(3) 0.51232(18) 0.0357 1.0000 Uani . . . . . .
C5 C 0.8811(3) 1.0596(3) 0.54912(16) 0.0329 1.0000 Uani . . . . . .
C6 C 0.8411(3) 0.9939(3) 0.51589(16) 0.0309 1.0000 Uani . . . . . .
C7 C 0.8628(3) 0.8656(3) 0.55939(16) 0.0332 1.0000 Uani . . . . . .
O8 O 0.8918(3) 0.8305(3) 0.62475(12) 0.0477 1.0000 Uani . . . . . .
N9 N 0.8527(3) 0.7920(2) 0.52474(14) 0.0350 1.0000 Uani . . . . . .
C10 C 0.8807(4) 0.6646(3) 0.56243(19) 0.0444 1.0000 Uani . . . . . .
C11 C 0.8168(3) 0.6123(3) 0.52315(18) 0.0371 1.0000 Uani . . . . . .
O12 O 0.6890(2) 0.6748(2) 0.52068(12) 0.0369 1.0000 Uani . . . . . .
C13 C 0.6137(3) 0.6509(3) 0.47961(16) 0.0318 1.0000 Uani . . . . . .
C14 C 0.6506(3) 0.5530(3) 0.45296(15) 0.0315 1.0000 Uani . . . . . .
C15 C 0.5660(3) 0.5360(3) 0.41337(15) 0.0308 1.0000 Uani . . . . . .
C16 C 0.4449(3) 0.6155(3) 0.39826(15) 0.0321 1.0000 Uani . . . . . .
C17 C 0.4097(3) 0.7118(3) 0.42586(16) 0.0348 1.0000 Uani . . . . . .
C18 C 0.4917(3) 0.7291(3) 0.46695(17) 0.0352 1.0000 Uani . . . . . .
C19 C 0.3507(3) 0.5951(3) 0.35759(16) 0.0356 1.0000 Uani . . . . . .
N20 N 0.3930(2) 0.5576(2) 0.29386(14) 0.0306 1.0000 Uani . . . . . .
C21 C 0.3178(3) 0.4973(3) 0.27251(19) 0.0417 1.0000 Uani . . . . . .
C22 C 0.3641(4) 0.4666(3) 0.2057(2) 0.0442 1.0000 Uani . . . . . .
N23 N 0.3569(3) 0.5808(3) 0.15193(15) 0.0379 1.0000 Uani . . . . . .
C24 C 0.4308(4) 0.5688(4) 0.0918(2) 0.0481 1.0000 Uani . . . . . .
C25 C 0.4157(4) 0.6962(4) 0.04931(19) 0.0449 1.0000 Uani . . . . . .
N26 N 0.4545(3) 0.7504(3) 0.09808(13) 0.0338 1.0000 Uani . . . . . .
C27 C 0.4203(3) 0.8814(3) 0.06311(16) 0.0365 1.0000 Uani . . . . . .
C28 C 0.4918(3) 0.9373(3) 0.09437(15) 0.0310 1.0000 Uani . . . . . .
C29 C 0.4318(3) 1.0482(3) 0.10574(15) 0.0334 1.0000 Uani . . . . . .
C30 C 0.4944(3) 1.1062(3) 0.13078(15) 0.0319 1.0000 Uani . . . . . .
C31 C 0.6207(3) 1.0523(3) 0.14600(15) 0.0301 1.0000 Uani . . . . . .
C32 C 0.6823(3) 0.9404(3) 0.13529(15) 0.0303 1.0000 Uani . . . . . .
C33 C 0.6187(3) 0.8852(3) 0.10904(15) 0.0313 1.0000 Uani . . . . . .
O34 O 0.6909(2) 1.10131(19) 0.17095(11) 0.0326 1.0000 Uani . . . . . .
C35 C 0.6313(3) 1.2205(3) 0.17585(17) 0.0356 1.0000 Uani . . . . . .
C36 C 0.7249(3) 1.2536(3) 0.20653(17) 0.0358 1.0000 Uani . . . . . .
N37 N 0.7653(2) 1.1868(2) 0.28238(14) 0.0343 1.0000 Uani . . . . . .
C38 C 0.7119(3) 1.2333(3) 0.33341(16) 0.0306 1.0000 Uani . . . . . .
O39 O 0.6222(2) 1.3269(2) 0.31996(12) 0.0438 1.0000 Uani . . . . . .
N40 N 0.4219(2) 0.8054(2) 0.24363(12) 0.0246 1.0000 Uani . . . . . .
C41 C 0.3210(3) 0.8967(3) 0.24748(15) 0.0263 1.0000 Uani . . . . . .
C42 C 0.3245(3) 0.9798(3) 0.28101(15) 0.0278 1.0000 Uani . . . . . .
C43 C 0.4364(3) 0.9694(3) 0.30758(15) 0.0286 1.0000 Uani . . . . . .
C44 C 0.5418(3) 0.8770(3) 0.30192(15) 0.0289 1.0000 Uani . . . . . .
C45 C 0.5302(3) 0.7952(3) 0.27060(14) 0.0260 1.0000 Uani . . . . . .
I46 I 0.44775(2) 1.09221(2) 0.358189(13) 0.0415 1.0000 Uani . . . . . .
C47 C 0.6345(3) 0.6847(3) 0.26512(14) 0.0272 1.0000 Uani . . . . . .
O48 O 0.61394(19) 0.61346(19) 0.23952(11) 0.0314 1.0000 Uani . . . . . .
N49 N 0.7454(2) 0.6680(2) 0.29084(13) 0.0299 1.0000 Uani . . . . . .
C50 C 0.8500(3) 0.5581(3) 0.29547(18) 0.0355 1.0000 Uani . . . . . .
C51 C 0.8991(3) 0.5593(3) 0.2246(2) 0.0420 1.0000 Uani . . . . . .
O52 O 1.0035(2) 0.4517(2) 0.23653(14) 0.0463 1.0000 Uani . . . . . .
C53 C 1.0372(4) 0.4230(3) 0.1727(2) 0.0526 1.0000 Uani . . . . . .
C54 C 1.1236(4) 0.2941(4) 0.1930(2) 0.0509 1.0000 Uani . . . . . .
O55 O 1.0662(2) 0.2139(2) 0.23145(13) 0.0425 1.0000 Uani . . . . . .
C56 C 0.2074(3) 0.9013(3) 0.20991(14) 0.0266 1.0000 Uani . U . . . .
O57 O 0.2134(2) 0.8154(2) 0.18886(13) 0.0354 1.0000 Uani . . . . . .
N58 N 0.1078(2) 0.9994(2) 0.20017(12) 0.0283 1.0000 Uani D U . . . .
C59 C -0.0022(2) 1.0164(3) 0.15904(15) 0.0342 1.0000 Uani D U . . . .
C60 C 0.0106(5) 1.0544(5) 0.0785(3) 0.0406 0.303(7) Uani D U P 1 1 .
O61 O 0.0254(5) 1.1671(4) 0.0607(2) 0.0523 0.303(7) Uani D U P 1 1 .
C62 C 0.0792(3) 1.1947(4) -0.0036(2) 0.0823 1.0000 Uani D U . . . .
O64 O -0.1235(3) 1.3192(3) -0.06222(16) 0.0627 1.0000 Uani D U . . . .
Cu65 Cu 0.40502(3) 0.68155(3) 0.199228(18) 0.0266 1.0000 Uani . . . . . .
Cl66 Cl 0.75013(9) 0.55824(9) 0.01506(5) 0.0501 1.0000 Uani D . . . . .
O67 O 0.6831(4) 0.6187(3) -0.05327(16) 0.0702 1.0000 Uani D . . . . .
O68 O 0.8744(4) 0.5146(7) 0.0078(3) 0.1396 1.0000 Uani D . . . . .
O69 O 0.7270(6) 0.4502(4) 0.0475(2) 0.1180 1.0000 Uani D . . . . .
O70 O 0.7206(4) 0.6284(4) 0.0608(2) 0.0904 1.0000 Uani D . . . . .
Cl71 Cl 0.93933(7) 0.80549(7) 0.33413(4) 0.0319 1.0000 Uani D . . . . .
O72 O 0.9329(3) 0.7913(3) 0.26467(13) 0.0466 1.0000 Uani D . . . . .
O73 O 0.9646(2) 0.9115(2) 0.32972(12) 0.0391 1.0000 Uani D . . . . .
O74 O 0.8229(2) 0.8190(2) 0.36278(12) 0.0384 1.0000 Uani D . . . . .
O75 O 1.0312(2) 0.7001(2) 0.38204(15) 0.0484 1.0000 Uani D . . . . .
C160 C -0.0301(3) 1.1220(3) 0.0911(2) 0.0444 0.697(7) Uani D U P 1 2 .
O161 O 0.0689(3) 1.0920(3) 0.04897(17) 0.0613 0.697(7) Uani D U P 1 2 .
C63 C -0.0069(4) 1.2411(4) -0.06830(16) 0.0815 1.0000 Uani D U . . . .
H11 H 0.7610 1.0039 0.4216 0.0345 1.0000 Uiso R . . . . .
H31 H 0.8032 1.3100 0.4183 0.0390 1.0000 Uiso R . . . . .
H41 H 0.8973 1.2222 0.5336 0.0430 1.0000 Uiso R . . . . .
H51 H 0.9160 1.0243 0.5959 0.0394 1.0000 Uiso R . . . . .
H102 H 0.9674 0.6193 0.5678 0.0533 1.0000 Uiso R . . . . .
H101 H 0.8538 0.6569 0.6106 0.0527 1.0000 Uiso R . . . . .
H111 H 0.8368 0.5280 0.5492 0.0442 1.0000 Uiso R . . . . .
H112 H 0.8398 0.6205 0.4748 0.0436 1.0000 Uiso R . . . . .
H141 H 0.7306 0.4997 0.4618 0.0375 1.0000 Uiso R . . . . .
H151 H 0.5907 0.4719 0.3961 0.0366 1.0000 Uiso R . . . . .
H171 H 0.3276 0.7660 0.4172 0.0422 1.0000 Uiso R . . . . .
H181 H 0.4659 0.7921 0.4858 0.0418 1.0000 Uiso R . . . . .
H192 H 0.2785 0.6677 0.3414 0.0426 1.0000 Uiso R . . . . .
H191 H 0.3273 0.5332 0.3897 0.0430 1.0000 Uiso R . . . . .
H212 H 0.2320 0.5425 0.2669 0.0616 1.0000 Uiso R . . . . .
H211 H 0.3545 0.4231 0.3096 0.0624 1.0000 Uiso R . . . . .
H221 H 0.4447 0.4053 0.2155 0.0657 1.0000 Uiso R . . . . .
H222 H 0.2977 0.4590 0.1828 0.0661 1.0000 Uiso R . . . . .
H242 H 0.5143 0.5133 0.1049 0.0712 1.0000 Uiso R . . . . .
H241 H 0.3744 0.5531 0.0669 0.0721 1.0000 Uiso R . . . . .
H251 H 0.4647 0.6950 0.0088 0.0546 1.0000 Uiso R . . . . .
H252 H 0.3299 0.7416 0.0327 0.0532 1.0000 Uiso R . . . . .
H271 H 0.4354 0.8928 0.0130 0.0443 1.0000 Uiso R . . . . .
H272 H 0.3344 0.9218 0.0661 0.0441 1.0000 Uiso R . . . . .
H291 H 0.3478 1.0846 0.0964 0.0395 1.0000 Uiso R . . . . .
H301 H 0.4534 1.1800 0.1365 0.0386 1.0000 Uiso R . . . . .
H321 H 0.7656 0.9027 0.1462 0.0367 1.0000 Uiso R . . . . .
H331 H 0.6607 0.8121 0.1011 0.0377 1.0000 Uiso R . . . . .
H351 H 0.5983 1.2765 0.1285 0.0428 1.0000 Uiso R . . . . .
H352 H 0.5668 1.2221 0.2066 0.0423 1.0000 Uiso R . . . . .
H361 H 0.6892 1.3384 0.2016 0.0430 1.0000 Uiso R . . . . .
H362 H 0.7949 1.2379 0.1798 0.0434 1.0000 Uiso R . . . . .
H421 H 0.2534 1.0404 0.2845 0.0333 1.0000 Uiso R . . . . .
H441 H 0.6180 0.8692 0.3186 0.0346 1.0000 Uiso R . . . . .
H501 H 0.9140 0.5517 0.3289 0.0430 1.0000 Uiso R . . . . .
H502 H 0.8275 0.4897 0.3119 0.0429 1.0000 Uiso R . . . . .
H511 H 0.9248 0.6271 0.2061 0.0513 1.0000 Uiso R . . . . .
H512 H 0.8389 0.5618 0.1900 0.0504 1.0000 Uiso R . . . . .
H532 H 1.0739 0.4751 0.1423 0.0643 1.0000 Uiso R . . . . .
H531 H 0.9648 0.4272 0.1469 0.0641 1.0000 Uiso R . . . . .
H542 H 1.1960 0.2825 0.2230 0.0608 1.0000 Uiso R . . . . .
H541 H 1.1479 0.2731 0.1499 0.0611 1.0000 Uiso R . . . . .
H601 H -0.0625 1.0637 0.0519 0.0481 0.303(7) Uiso R . P 1 1 .
H602 H 0.0806 0.9940 0.0673 0.0480 0.303(7) Uiso R . P 1 1 .
H1601 H -0.0388 1.1957 0.1023 0.0540 0.697(7) Uiso R . P 1 2 .
H1602 H -0.1060 1.1341 0.0656 0.0541 0.697(7) Uiso R . P 1 2 .
H631 H 0.0276 1.2821 -0.1075 0.0986 1.0000 Uiso R . . . . .
H632 H -0.0147 1.1707 -0.0752 0.0990 1.0000 Uiso R . . . . .
H91 H 0.8377 0.8174 0.4795 0.0421 1.0000 Uiso R . . . . .
H201 H 0.4671 0.5029 0.3071 0.0455 1.0000 Uiso R . . . . .
H231 H 0.2796 0.6214 0.1331 0.0569 1.0000 Uiso R . . . . .
H261 H 0.5363 0.7184 0.1038 0.0504 1.0000 Uiso R . . . . .
H371 H 0.8288 1.1212 0.2949 0.0408 1.0000 Uiso R . . . . .
H551 H 1.0625 0.2204 0.2713 0.0641 1.0000 Uiso R . . . . .
H491 H 0.7562 0.7209 0.3068 0.0360 1.0000 Uiso R . . . . .
H641 H -0.1233 1.3627 -0.0373 0.0943 1.0000 Uiso R . . . . .
H591 H -0.0697 1.0776 0.1692 0.0419 0.303(7) Uiso R . P 1 1 .
H592 H -0.0156 0.9426 0.1723 0.0419 0.303(7) Uiso R . P 1 1 .
H593 H -0.0687 1.0314 0.1872 0.0419 0.697(7) Uiso R . P 1 2 .
H594 H 0.0095 0.9452 0.1467 0.0419 0.697(7) Uiso R . P 1 2 .
H581 H 0.1080 1.0597 0.2204 0.0339 1.0000 Uiso R . . . . .
H621 H 0.1111 1.2543 -0.0032 0.0987 0.303(7) Uiso R . P 1 1 .
H622 H 0.1438 1.1232 -0.0052 0.0987 0.303(7) Uiso R . P 1 1 .
H623 H 0.0644 1.2575 0.0176 0.0987 0.697(7) Uiso R . P 1 2 .
H624 H 0.1600 1.1722 -0.0171 0.0987 0.697(7) Uiso R . P 1 2 .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          3.25(2)

loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . C2 . 1.390(4) yes
C1 . C6 . 1.401(4) yes
C1 . H11 . 0.930 no
C2 . C3 . 1.391(4) yes
C2 . C38 . 1.502(4) yes
C3 . C4 . 1.376(5) yes
C3 . H31 . 0.924 no
C4 . C5 . 1.392(5) yes
C4 . H41 . 0.934 no
C5 . C6 . 1.388(5) yes
C5 . H51 . 0.919 no
C6 . C7 . 1.501(5) yes
C7 . O8 . 1.233(4) yes
C7 . N9 . 1.331(4) yes
N9 . C10 . 1.453(4) yes
N9 . H91 . 0.845 no
C10 . C11 . 1.503(5) yes
C10 . H102 . 0.965 no
C10 . H101 . 0.980 no
C11 . O12 . 1.421(4) yes
C11 . H111 . 0.964 no
C11 . H112 . 0.967 no
O12 . C13 . 1.372(4) yes
C13 . C14 . 1.394(5) yes
C13 . C18 . 1.393(4) yes
C14 . C15 . 1.387(5) yes
C14 . H141 . 0.920 no
C15 . C16 . 1.390(4) yes
C15 . H151 . 0.909 no
C16 . C17 . 1.388(5) yes
C16 . C19 . 1.514(5) yes
C17 . C18 . 1.383(5) yes
C17 . H171 . 0.943 no
C18 . H181 . 0.918 no
C19 . N20 . 1.479(4) yes
C19 . H192 . 0.963 no
C19 . H191 . 0.965 no
N20 . C21 . 1.489(4) yes
N20 . Cu65 . 2.075(2) yes
N20 . H201 . 0.877 no
C21 . C22 . 1.512(5) yes
C21 . Cu65 . 2.853(3) yes
C21 . H212 . 0.954 no
C21 . H211 . 0.945 no
C22 . N23 . 1.475(4) yes
C22 . Cu65 . 2.861(4) yes
C22 . H221 . 0.959 no
C22 . H222 . 0.956 no
N23 . C24 . 1.468(5) yes
N23 . Cu65 . 1.997(3) yes
N23 . H231 . 0.890 no
C24 . C25 . 1.505(6) yes
C24 . Cu65 . 2.817(4) yes
C24 . H242 . 0.963 no
C24 . H241 . 0.939 no
C25 . N26 . 1.484(4) yes
C25 . H251 . 0.976 no
C25 . H252 . 0.970 no
N26 . C27 . 1.474(4) yes
N26 . Cu65 . 2.081(3) yes
N26 . H261 . 0.897 no
C27 . C28 . 1.508(5) yes
C27 . H271 . 0.973 no
C27 . H272 . 0.966 no
C28 . C29 . 1.390(5) yes
C28 . C33 . 1.397(4) yes
C29 . C30 . 1.387(5) yes
C29 . H291 . 0.925 no
C30 . C31 . 1.392(4) yes
C30 . H301 . 0.913 no
C31 . C32 . 1.399(4) yes
C31 . O34 . 1.364(4) yes
C32 . C33 . 1.379(5) yes
C32 . H321 . 0.921 no
C33 . H331 . 0.926 no
O34 . C35 . 1.428(4) yes
C35 . C36 . 1.502(5) yes
C35 . H351 . 0.964 no
C35 . H352 . 0.964 no
C36 . N37 . 1.459(4) yes
C36 . H361 . 0.961 no
C36 . H362 . 0.964 no
N37 . C38 . 1.340(4) yes
N37 . H371 . 0.857 no
C38 . O39 . 1.219(4) yes
N40 . C41 . 1.339(4) yes
N40 . C45 . 1.340(4) yes
N40 . Cu65 . 2.052(3) yes
C41 . C42 . 1.395(4) yes
C41 . C56 . 1.515(4) yes
C42 . C43 . 1.377(4) yes
C42 . H421 . 0.923 no
C43 . C44 . 1.387(4) yes
C43 . I46 . 2.098(3) yes
C44 . C45 . 1.384(4) yes
C44 . H441 . 0.925 no
C45 . C47 . 1.512(4) yes
C47 . O48 . 1.235(4) yes
C47 . N49 . 1.332(4) yes
O48 . Cu65 . 2.363(2) yes
N49 . C50 . 1.456(4) yes
N49 . H491 . 0.857 no
C50 . C51 . 1.497(5) yes
C50 . H501 . 0.974 no
C50 . H502 . 0.951 no
C51 . O52 . 1.414(4) yes
C51 . H511 . 0.970 no
C51 . H512 . 0.976 no
O52 . C53 . 1.415(4) yes
C53 . C54 . 1.494(5) yes
C53 . H532 . 0.966 no
C53 . H531 . 0.977 no
C54 . O55 . 1.436(5) yes
C54 . H542 . 0.987 no
C54 . H541 . 0.966 no
O55 . H551 . 0.807 no
C56 . O57 . 1.238(4) yes
C56 . N58 . 1.321(4) yes
O57 . Cu65 . 2.244(2) yes
N58 . C59 . 1.455(3) yes
N58 . H581 . 0.950 no
C59 . C60 . 1.531(5) yes
C59 . H591 . 0.950 no
C59 . H592 . 0.950 no
C59 . C160 . 1.508(4) yes
C59 . H593 . 0.949 no
C59 . H594 . 0.951 no
C60 . O61 . 1.420(6) yes
C60 . H601 . 0.967 no
C60 . H602 . 0.970 no
O61 . C62 . 1.411(5) yes
C62 . C63 . 1.468(4) yes
C62 . H621 . 0.950 no
C62 . H622 . 0.950 no
C62 . O161 . 1.430(4) yes
C62 . C63 . 1.468(4) yes
C62 . H623 . 0.953 no
C62 . H624 . 0.950 no
O64 . C63 . 1.399(4) yes
O64 . H641 . 0.830 no
Cl66 . O67 . 1.410(3) yes
Cl66 . O68 . 1.392(4) yes
Cl66 . O69 . 1.433(4) yes
Cl66 . O70 . 1.388(3) yes
Cl71 . O72 . 1.430(2) yes
Cl71 . O73 . 1.438(2) yes
Cl71 . O74 . 1.452(2) yes
Cl71 . O75 . 1.433(2) yes
C160 . O161 . 1.425(4) yes
C160 . H1601 . 0.977 no
C160 . H1602 . 0.974 no
C63 . H631 . 0.964 no
C63 . H632 . 0.963 no

loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 . C1 . C6 . 119.4(3) yes
C2 . C1 . H11 . 120.1 no
C6 . C1 . H11 . 120.5 no
C1 . C2 . C3 . 120.2(3) yes
C1 . C2 . C38 . 123.4(3) yes
C3 . C2 . C38 . 116.4(3) yes
C2 . C3 . C4 . 120.6(3) yes
C2 . C3 . H31 . 119.3 no
C4 . C3 . H31 . 120.1 no
C3 . C4 . C5 . 119.5(3) yes
C3 . C4 . H41 . 119.0 no
C5 . C4 . H41 . 121.4 no
C4 . C5 . C6 . 120.6(3) yes
C4 . C5 . H51 . 120.0 no
C6 . C5 . H51 . 119.4 no
C1 . C6 . C5 . 119.6(3) yes
C1 . C6 . C7 . 123.9(3) yes
C5 . C6 . C7 . 116.4(3) yes
C6 . C7 . O8 . 120.2(3) yes
C6 . C7 . N9 . 117.8(3) yes
O8 . C7 . N9 . 122.0(3) yes
C7 . N9 . C10 . 120.9(3) yes
C7 . N9 . H91 . 119.7 no
C10 . N9 . H91 . 119.0 no
N9 . C10 . C11 . 111.1(3) yes
N9 . C10 . H102 . 110.7 no
C11 . C10 . H102 . 109.3 no
N9 . C10 . H101 . 108.5 no
C11 . C10 . H101 . 109.4 no
H102 . C10 . H101 . 107.9 no
C10 . C11 . O12 . 108.1(3) yes
C10 . C11 . H111 . 109.4 no
O12 . C11 . H111 . 108.6 no
C10 . C11 . H112 . 111.4 no
O12 . C11 . H112 . 109.8 no
H111 . C11 . H112 . 109.6 no
C11 . O12 . C13 . 117.5(3) yes
O12 . C13 . C14 . 124.4(3) yes
O12 . C13 . C18 . 116.2(3) yes
C14 . C13 . C18 . 119.3(3) yes
C13 . C14 . C15 . 119.6(3) yes
C13 . C14 . H141 . 120.2 no
C15 . C14 . H141 . 120.2 no
C14 . C15 . C16 . 121.7(3) yes
C14 . C15 . H151 . 119.1 no
C16 . C15 . H151 . 119.2 no
C15 . C16 . C17 . 117.8(3) yes
C15 . C16 . C19 . 122.1(3) yes
C17 . C16 . C19 . 119.9(3) yes
C16 . C17 . C18 . 121.6(3) yes
C16 . C17 . H171 . 119.5 no
C18 . C17 . H171 . 119.0 no
C13 . C18 . C17 . 119.9(3) yes
C13 . C18 . H181 . 120.0 no
C17 . C18 . H181 . 120.1 no
C16 . C19 . N20 . 114.2(2) yes
C16 . C19 . H192 . 110.5 no
N20 . C19 . H192 . 107.3 no
C16 . C19 . H191 . 108.7 no
N20 . C19 . H191 . 108.3 no
H192 . C19 . H191 . 107.6 no
C19 . N20 . C21 . 111.1(3) yes
C19 . N20 . Cu65 . 121.2(2) yes
C21 . N20 . Cu65 . 105.18(19) yes
C19 . N20 . H201 . 106.3 no
C21 . N20 . H201 . 106.7 no
Cu65 . N20 . H201 . 105.5 no
N20 . C21 . C22 . 107.4(3) yes
N20 . C21 . Cu65 . 44.58(13) yes
C22 . C21 . Cu65 . 74.98(18) yes
N20 . C21 . H212 . 114.1 no
C22 . C21 . H212 . 113.0 no
Cu65 . C21 . H212 . 101.1 no
N20 . C21 . H211 . 95.1 no
C22 . C21 . H211 . 103.3 no
Cu65 . C21 . H211 . 132.4 no
H212 . C21 . H211 . 121.7 no
C21 . C22 . N23 . 106.7(3) yes
C21 . C22 . Cu65 . 74.34(19) yes
N23 . C22 . Cu65 . 40.96(15) yes
C21 . C22 . H221 . 111.9 no
N23 . C22 . H221 . 112.9 no
Cu65 . C22 . H221 . 103.5 no
C21 . C22 . H222 . 105.3 no
N23 . C22 . H222 . 95.9 no
Cu65 . C22 . H222 . 128.6 no
H221 . C22 . H222 . 122.2 no
C22 . N23 . C24 . 116.0(3) yes
C22 . N23 . Cu65 . 110.1(2) yes
C24 . N23 . Cu65 . 107.7(2) yes
C22 . N23 . H231 . 107.8 no
C24 . N23 . H231 . 106.9 no
Cu65 . N23 . H231 . 108.0 no
N23 . C24 . C25 . 105.1(3) yes
N23 . C24 . Cu65 . 42.49(15) yes
C25 . C24 . Cu65 . 77.52(19) yes
N23 . C24 . H242 . 115.5 no
C25 . C24 . H242 . 114.3 no
Cu65 . C24 . H242 . 99.6 no
N23 . C24 . H241 . 93.7 no
C25 . C24 . H241 . 103.6 no
Cu65 . C24 . H241 . 131.7 no
H242 . C24 . H241 . 121.7 no
C24 . C25 . N26 . 108.1(3) yes
C24 . C25 . H251 . 109.6 no
N26 . C25 . H251 . 111.2 no
C24 . C25 . H252 . 108.0 no
N26 . C25 . H252 . 108.9 no
H251 . C25 . H252 . 110.9 no
C25 . N26 . C27 . 110.2(3) yes
C25 . N26 . Cu65 . 107.3(2) yes
C27 . N26 . Cu65 . 121.9(2) yes
C25 . N26 . H261 . 106.3 no
C27 . N26 . H261 . 105.9 no
Cu65 . N26 . H261 . 104.1 no
N26 . C27 . C28 . 114.5(3) yes
N26 . C27 . H271 . 106.9 no
C28 . C27 . H271 . 107.8 no
N26 . C27 . H272 . 108.6 no
C28 . C27 . H272 . 109.2 no
H271 . C27 . H272 . 109.8 no
C27 . C28 . C29 . 119.7(3) yes
C27 . C28 . C33 . 122.4(3) yes
C29 . C28 . C33 . 117.7(3) yes
C28 . C29 . C30 . 121.8(3) yes
C28 . C29 . H291 . 119.4 no
C30 . C29 . H291 . 118.8 no
C29 . C30 . C31 . 119.7(3) yes
C29 . C30 . H301 . 120.4 no
C31 . C30 . H301 . 119.9 no
C30 . C31 . C32 . 119.2(3) yes
C30 . C31 . O34 . 124.4(3) yes
C32 . C31 . O34 . 116.4(3) yes
C31 . C32 . C33 . 120.3(3) yes
C31 . C32 . H321 . 120.2 no
C33 . C32 . H321 . 119.5 no
C28 . C33 . C32 . 121.2(3) yes
C28 . C33 . H331 . 119.2 no
C32 . C33 . H331 . 119.6 no
C31 . O34 . C35 . 117.3(2) yes
O34 . C35 . C36 . 107.8(3) yes
O34 . C35 . H351 . 109.4 no
C36 . C35 . H351 . 109.6 no
O34 . C35 . H352 . 109.9 no
C36 . C35 . H352 . 110.1 no
H351 . C35 . H352 . 110.0 no
C35 . C36 . N37 . 113.5(3) yes
C35 . C36 . H361 . 108.0 no
N37 . C36 . H361 . 108.1 no
C35 . C36 . H362 . 108.8 no
N37 . C36 . H362 . 108.5 no
H361 . C36 . H362 . 109.9 no
C36 . N37 . C38 . 120.5(3) yes
C36 . N37 . H371 . 120.4 no
C38 . N37 . H371 . 118.7 no
C2 . C38 . N37 . 116.1(3) yes
C2 . C38 . O39 . 121.2(3) yes
N37 . C38 . O39 . 122.7(3) yes
C41 . N40 . C45 . 119.4(3) yes
C41 . N40 . Cu65 . 118.7(2) yes
C45 . N40 . Cu65 . 121.9(2) yes
N40 . C41 . C42 . 121.9(3) yes
N40 . C41 . C56 . 113.1(3) yes
C42 . C41 . C56 . 125.0(3) yes
C41 . C42 . C43 . 118.1(3) yes
C41 . C42 . H421 . 120.3 no
C43 . C42 . H421 . 121.5 no
C42 . C43 . C44 . 120.3(3) yes
C42 . C43 . I46 . 119.9(2) yes
C44 . C43 . I46 . 119.8(2) yes
C43 . C44 . C45 . 118.1(3) yes
C43 . C44 . H441 . 121.7 no
C45 . C44 . H441 . 120.2 no
C44 . C45 . N40 . 122.1(3) yes
C44 . C45 . C47 . 124.6(3) yes
N40 . C45 . C47 . 113.2(3) yes
C45 . C47 . O48 . 119.8(3) yes
C45 . C47 . N49 . 116.9(3) yes
O48 . C47 . N49 . 123.3(3) yes
C47 . O48 . Cu65 . 111.40(18) yes
C47 . N49 . C50 . 121.3(3) yes
C47 . N49 . H491 . 120.4 no
C50 . N49 . H491 . 118.2 no
N49 . C50 . C51 . 112.5(3) yes
N49 . C50 . H501 . 108.0 no
C51 . C50 . H501 . 108.3 no
N49 . C50 . H502 . 109.9 no
C51 . C50 . H502 . 107.8 no
H501 . C50 . H502 . 110.4 no
C50 . C51 . O52 . 107.2(3) yes
C50 . C51 . H511 . 110.6 no
O52 . C51 . H511 . 107.8 no
C50 . C51 . H512 . 111.0 no
O52 . C51 . H512 . 109.5 no
H511 . C51 . H512 . 110.5 no
C51 . O52 . C53 . 112.9(3) yes
O52 . C53 . C54 . 108.1(3) yes
O52 . C53 . H532 . 113.0 no
C54 . C53 . H532 . 110.2 no
O52 . C53 . H531 . 108.4 no
C54 . C53 . H531 . 106.2 no
H532 . C53 . H531 . 110.7 no
C53 . C54 . O55 . 111.1(3) yes
C53 . C54 . H542 . 110.1 no
O55 . C54 . H542 . 109.5 no
C53 . C54 . H541 . 109.2 no
O55 . C54 . H541 . 107.0 no
H542 . C54 . H541 . 110.0 no
C54 . O55 . H551 . 105.6 no
C41 . C56 . O57 . 118.9(3) yes
C41 . C56 . N58 . 117.3(3) yes
O57 . C56 . N58 . 123.8(3) yes
C56 . O57 . Cu65 . 112.65(19) yes
C56 . N58 . C59 . 121.1(3) yes
C56 . N58 . H581 . 119.5 no
C59 . N58 . H581 . 119.4 no
N58 . C59 . C60 . 110.47(10) yes
N58 . C59 . H591 . 109.2 no
C60 . C59 . H591 . 109.2 no
N58 . C59 . H592 . 109.3 no
C60 . C59 . H592 . 109.1 no
H591 . C59 . H592 . 109.5 no
N58 . C59 . C160 . 110.38(9) yes
N58 . C59 . H593 . 109.3 no
C160 . C59 . H593 . 109.3 no
N58 . C59 . H594 . 109.2 no
C160 . C59 . H594 . 109.1 no
H593 . C59 . H594 . 109.5 no
C59 . C60 . O61 . 107.05(10) yes
C59 . C60 . H601 . 109.5 no
O61 . C60 . H601 . 109.8 no
C59 . C60 . H602 . 110.4 no
O61 . C60 . H602 . 110.5 no
H601 . C60 . H602 . 109.5 no
C60 . O61 . C62 . 113.92(10) yes
O61 . C62 . C63 . 113.22(10) yes
O61 . C62 . H621 . 108.4 no
C63 . C62 . H621 . 108.5 no
O61 . C62 . H622 . 108.5 no
C63 . C62 . H622 . 108.7 no
H621 . C62 . H622 . 109.5 no
O161 . C62 . C63 . 113.29(10) yes
O161 . C62 . H623 . 108.5 no
C63 . C62 . H623 . 108.5 no
O161 . C62 . H624 . 108.6 no
C63 . C62 . H624 . 108.7 no
H623 . C62 . H624 . 109.2 no
C63 . O64 . H641 . 113.5 no
O48 . Cu65 . O57 . 149.63(8) yes
O48 . Cu65 . N26 . 85.61(9) yes
O57 . Cu65 . N26 . 99.99(10) yes
O48 . Cu65 . N20 . 86.25(9) yes
O57 . Cu65 . N20 . 96.20(9) yes
N26 . Cu65 . N20 . 160.11(11) yes
O48 . Cu65 . N40 . 73.66(8) yes
O57 . Cu65 . N40 . 76.01(9) yes
N26 . Cu65 . N40 . 97.73(10) yes
N20 . Cu65 . N40 . 97.34(10) yes
O48 . Cu65 . N23 . 116.67(10) yes
O57 . Cu65 . N23 . 93.68(10) yes
N26 . Cu65 . N23 . 83.23(11) yes
N20 . Cu65 . N23 . 84.28(11) yes
N40 . Cu65 . N23 . 169.66(11) yes
O48 . Cu65 . C24 . 98.08(10) yes
O57 . Cu65 . C24 . 110.03(11) yes
N26 . Cu65 . C24 . 56.87(11) yes
N20 . Cu65 . C24 . 106.55(11) yes
N40 . Cu65 . C24 . 154.25(10) yes
O48 . Cu65 . C21 . 107.84(9) yes
O57 . Cu65 . C21 . 87.53(10) yes
N26 . Cu65 . C21 . 138.97(11) yes
N20 . Cu65 . C21 . 30.24(10) yes
N40 . Cu65 . C21 . 123.13(10) yes
O48 . Cu65 . C22 . 104.82(9) yes
O57 . Cu65 . C22 . 101.49(10) yes
N26 . Cu65 . C22 . 109.00(11) yes
N20 . Cu65 . C22 . 55.99(11) yes
N40 . Cu65 . C22 . 153.11(10) yes
N23 . Cu65 . C24 . 29.77(12) yes
N23 . Cu65 . C21 . 55.93(11) yes
C24 . Cu65 . C21 . 82.54(12) yes
N23 . Cu65 . C22 . 28.95(11) yes
C24 . Cu65 . C22 . 52.14(11) yes
C21 . Cu65 . C22 . 30.68(11) yes
O67 . Cl66 . O68 . 110.0(3) yes
O67 . Cl66 . O69 . 109.2(2) yes
O68 . Cl66 . O69 . 103.2(4) yes
O67 . Cl66 . O70 . 112.9(2) yes
O68 . Cl66 . O70 . 112.6(3) yes
O69 . Cl66 . O70 . 108.5(3) yes
O72 . Cl71 . O73 . 110.79(15) yes
O72 . Cl71 . O74 . 109.05(15) yes
O73 . Cl71 . O74 . 108.43(15) yes
O72 . Cl71 . O75 . 110.03(17) yes
O73 . Cl71 . O75 . 110.30(15) yes
O74 . Cl71 . O75 . 108.19(16) yes
C59 . C160 . O161 . 107.09(9) yes
C59 . C160 . H1601 . 110.7 no
O161 . C160 . H1601 . 110.4 no
C59 . C160 . H1602 . 109.0 no
O161 . C160 . H1602 . 110.5 no
H1601 . C160 . H1602 . 109.1 no
C62 . O161 . C160 . 113.87(10) yes
C62 . C63 . O64 . 114.31(7) yes
C62 . C63 . H631 . 107.8 no
O64 . C63 . H631 . 109.7 no
C62 . C63 . H632 . 105.2 no
O64 . C63 . H632 . 107.6 no
H631 . C63 . H632 . 112.2 no

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C4 . H41 . O75 2_776 165.07 0.934 2.444 3.356(5) yes
C5 . H51 . O73 2_776 130.89 0.919 2.516 3.194(5) yes
C15 . H151 . O39 1_545 165.72 0.909 2.596 3.484(5) yes
C24 . H241 . O67 2_665 142.50 0.939 2.556 3.350(5) yes
C24 . H241 . O69 2_665 153.31 0.939 2.575 3.440(5) yes
C30 . H301 . O67 2_675 133.65 0.913 2.507 3.205(5) yes
C33 . H331 . O70 . 164.53 0.926 2.502 3.404(5) yes
C42 . H421 . O55 1_465 151.90 0.923 2.435 3.278(5) yes
C44 . H441 . O74 . 171.67 0.925 2.376 3.294(5) yes
N9 . H91 . O74 . 161.05 0.845 2.290 3.102(5) yes
N20 . H201 . O39 1_545 157.18 0.877 2.240 3.067(5) yes
N23 . H231 . O64 2_575 158.56 0.890 2.087 2.933(5) yes
N26 . H261 . O70 . 149.71 0.897 2.336 3.144(5) yes
N37 . H371 . O73 . 163.64 0.857 2.412 3.244(5) yes
O55 . H551 . O8 2_766 155.94 0.807 1.965 2.722(5) yes
N49 . H491 . O74 . 166.08 0.857 2.201 3.040(5) yes
O64 . H641 . O68 1_465 167.43 0.830 2.311 3.126(5) yes
O64 . H641 . O69 1_465 132.98 0.830 2.586 3.210(5) yes
C59 . H592 . O72 1_455 147.89 0.950 2.448 3.292(5) yes
N58 . H581 . O55 1_465 159.09 0.950 1.885 2.793(5) yes

_iucr_refine_instruction_details_constraints 
;
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
EQUIVALENCE PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE N   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 102,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 192,X'S) H   ( 191,X'S) 
RIDE N   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 212,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE N   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 242,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) 
RIDE N   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) 
RIDE N   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE N   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) H   ( 502,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) H   ( 512,X'S) 
RIDE C   (  53,X'S) H   ( 532,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 542,X'S) H   ( 541,X'S) 
RIDE O   (  55,X'S) H   ( 551,X'S) 
RIDE N   (  58,X'S) H   ( 581,X'S) 
RIDE C   (  59,X'S) H   ( 591,X'S) H   ( 592,X'S) H   ( 593,X'S) H   ( 594,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) H   ( 602,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) H   ( 622,X'S) H   ( 623,X'S) H   ( 624,X'S) 
RIDE O   (  64,X'S) H   ( 641,X'S) 
RIDE C   ( 160,X'S) H   (1601,X'S) H   (1602,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) H   ( 632,X'S) 
END                                                                             
;

_iucr_refine_instruction_details_restraints 
;
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
SAME N(58) C(59) C(60) O(61) C(62) C(63) O(64) AND 
CONT N(58) C(59) C(160) O(161) C(62) C(63) O(64) 
DISTANCE 1.52, 0.01 = C(59) TO C(60) C(62) TO C(63) 
DISTANCE 1.42, 0.01 = C(60) TO O(61) O(61) TO C(62) 
CONT C(63) TO O(64) 
DISTANCE 1.52, 0.01 = C(59) TO C(160) 
DISTANCE 1.42, 0.01 = C(160) TO O(161) O(161) TO C(62) 
SIMU 0.02 N(58) C(59) C(60) O(61) C(62) C(63) O(64) 
DELU 0.01 N(58) C(59) C(60) O(61) C(62) C(63) O(64) 
SIMU 0.02 N(58) C(59) C(160) O(161) C(62) C(63) O(64) 
DELU 0.01 N(58) C(59) C(160) O(161) C(62) C(63) O(64) 
REM PERCHLORATE 
DISTANCE 0, 0.01 = MEAN CL(66) TO O(67) CL(66) TO O(68) 
CONT CL(66) TO O(69) CL(66) TO O(70) 
CONT CL(71) TO O(72) CL(71) TO O(73) CL(71) TO O(74) 
CONT CL(71) TO O(75) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.02000 = N(58) TO C(59) 
U(IJ) .0, 0.02000 = C(59) TO C(60) 
U(IJ) .0, 0.02000 = C(59) TO C(160) 
U(IJ) .0, 0.02000 = C(60) TO O(61) 
U(IJ) .0, 0.02000 = O(61) TO C(62) 
U(IJ) .0, 0.02000 = C(62) TO C(63) 
U(IJ) .0, 0.02000 = C(62) TO O(161) 
U(IJ) .0, 0.02000 = C(62) TO C(63) 
U(IJ) .0, 0.04000 = O(64) TO C(63) 
U(IJ) .0, 0.02000 = C(160) TO O(161) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = N(58) TO C(59) 
VIBR .0, 0.00500 = C(59) TO C(56) 
VIBR .0, 0.00200 = C(59) TO C(60) 
VIBR .0, 0.00500 = C(60) TO N(58) 
VIBR .0, 0.00200 = C(59) TO C(160) 
VIBR .0, 0.00500 = C(160) TO N(58) 
VIBR .0, 0.00200 = C(60) TO O(61) 
VIBR .0, 0.00500 = O(61) TO C(59) 
VIBR .0, 0.00200 = O(61) TO C(62) 
VIBR .0, 0.00500 = C(62) TO C(60) 
VIBR .0, 0.00200 = C(62) TO C(63) 
VIBR .0, 0.00500 = C(63) TO O(61) 
VIBR .0, 0.00200 = C(62) TO O(161) 
VIBR .0, 0.00200 = C(62) TO C(63) 
VIBR .0, 0.00500 = C(63) TO O(161) 
VIBR .0, 0.00200 = O(64) TO C(63) 
VIBR .0, 0.00200 = C(160) TO O(161) 
VIBR .0, 0.00500 = O(161) TO C(59) 
VIBR .0, 0.00500 = C(160) TO C(62) 
VIBR .0, 0.00500 = O(64) TO C(62) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
0 -1 4 x .
-10 -10 1 x .
3 11 2 x .
1 -3 1 x .

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile, di-isopropyl ether'
