# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013

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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
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data_45pycu

_audit_creation_method           SHELXL-97

_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[CuH4(py33233)]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H47 Cl Cu N7 O5, 5(Cl O4), 3(H2 O)'
_chemical_formula_sum            'C21 H53 Cl6 Cu N7 O28'
_chemical_formula_weight         1127.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P c 21 b'
_symmetry_space_group_name_Hall  'P -2bc -2c'

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

_cell_length_a                   8.4130(2)
_cell_length_b                   18.1930(5)
_cell_length_c                   28.4910(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4360.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7370
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      22.722

_exptl_crystal_description       prism
_exptl_crystal_colour            'pale blue'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2332
_exptl_absorpt_coefficient_mu    0.970
_exptl_absorpt_correction_type   none

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 9
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15366
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.82
_diffrn_reflns_theta_max         22.78
_reflns_number_total             5746
_reflns_number_gt                4496
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Mercury
_computing_publication_material  'Microsoft Office 2007'

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

 Due to disorder found in some of the perchlorate oxygens, some restraints
have been applied in order to keep reasonable bond distances and well known
tetraedral geometry of ClO4 anions. Namely Cl-O distances have in perchlorates
1 and 2 have been restrained to be equal using SADI. Additionally, more SADI
restraints have been applied to O-O distances in perchlorate 1.

 O-H distance in water moieties 2 and 4 have been restrained to be 0.82A using
DFIX.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0827P)^2^+5.4760P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5746
_refine_ls_number_parameters     575
_refine_ls_number_restraints     53
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0593
_refine_ls_wR_factor_ref         0.1598
_refine_ls_wR_factor_gt          0.1420
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.45036(11) 0.24647(6) 0.25070(4) 0.0401(3) Uani 1 1 d . . .
N1 N 0.2479(8) 0.2921(4) 0.2591(2) 0.0418(18) Uani 1 1 d . . .
N2 N 0.3559(9) 0.1695(4) 0.2960(2) 0.0427(18) Uani 1 1 d . . .
H2 H 0.4319 0.1577 0.3175 0.06(3) Uiso 1 1 calc R . .
N3 N 0.0701(9) 0.0609(4) 0.1603(3) 0.051(2) Uani 1 1 d . . .
H3C H 0.1220 0.1007 0.1446 0.061 Uiso 1 1 d R . .
H3D H -0.0296 0.0758 0.1723 0.061 Uiso 1 1 d R . .
N4 N 0.1056(10) 0.0315(5) 0.0168(3) 0.068(2) Uani 1 1 d . . .
H4C H 0.0613 -0.0126 0.0052 0.081 Uiso 1 1 d R . .
H4D H 0.1994 0.0233 0.0341 0.081 Uiso 1 1 d R . .
N5 N 0.3514(10) 0.1685(5) -0.0529(3) 0.057(2) Uani 1 1 d . . .
H5C H 0.3863 0.1284 -0.0722 0.068 Uiso 1 1 d R . .
H5D H 0.2792 0.1989 -0.0700 0.068 Uiso 1 1 d R . .
N6 N 0.6306(10) 0.3567(4) 0.0465(3) 0.0489(19) Uani 1 1 d . . .
H6C H 0.7309 0.3781 0.0514 0.059 Uiso 1 1 d R . .
H6D H 0.5515 0.3931 0.0400 0.059 Uiso 1 1 d R . .
N7 N 0.4585(8) 0.3140(4) 0.1935(3) 0.0429(18) Uani 1 1 d . . .
H7 H 0.4253 0.2857 0.1690 0.024(19) Uiso 1 1 calc R . .
C1 C 0.2201(12) 0.2055(6) 0.3216(3) 0.056(3) Uani 1 1 d . . .
H1A H 0.1453 0.1686 0.3289 0.067 Uiso 1 1 d R . .
H1B H 0.2596 0.2282 0.3499 0.067 Uiso 1 1 d R . .
C2 C 0.3086(11) 0.0998(5) 0.2702(3) 0.046(2) Uani 1 1 d . . .
H2A H 0.4008 0.0739 0.2587 0.055 Uiso 1 1 d R . .
H2B H 0.2492 0.0690 0.2906 0.055 Uiso 1 1 d R . .
C3 C 0.2042(11) 0.1143(5) 0.2293(3) 0.045(2) Uani 1 1 d . . .
H3A H 0.1067 0.1379 0.2398 0.055 Uiso 1 1 d R . .
H3B H 0.2588 0.1483 0.2087 0.055 Uiso 1 1 d R . .
C4 C 0.1767(12) 0.0446(5) 0.2022(3) 0.050(2) Uani 1 1 d . . .
H4A H 0.1267 0.0082 0.2222 0.060 Uiso 1 1 calc R . .
H4B H 0.2774 0.0249 0.1914 0.060 Uiso 1 1 calc R . .
C5 C 0.0476(13) -0.0032(7) 0.1284(3) 0.064(3) Uani 1 1 d . . .
H5A H 0.1498 -0.0159 0.1156 0.076 Uiso 1 1 d R . .
H5B H 0.0021 -0.0427 0.1445 0.076 Uiso 1 1 d R . .
C6 C -0.0564(13) 0.0172(8) 0.0866(4) 0.080(4) Uani 1 1 d . . .
H6A H -0.0843 -0.0283 0.0709 0.096 Uiso 1 1 calc R . .
H6B H -0.1543 0.0373 0.0992 0.096 Uiso 1 1 calc R . .
C7 C 0.0002(14) 0.0692(6) 0.0496(4) 0.072(3) Uani 1 1 d . . .
H7A H 0.0529 0.1126 0.0612 0.086 Uiso 1 1 d R . .
H7B H -0.0840 0.0821 0.0293 0.086 Uiso 1 1 d R . .
C8 C 0.1584(13) 0.0788(6) -0.0257(3) 0.059(3) Uani 1 1 d . . .
H8A H 0.2034 0.0471 -0.0496 0.071 Uiso 1 1 calc R . .
H8B H 0.0665 0.1033 -0.0390 0.071 Uiso 1 1 calc R . .
C9 C 0.2776(12) 0.1343(5) -0.0115(3) 0.056(3) Uani 1 1 d . . .
H9A H 0.3542 0.1111 0.0088 0.067 Uiso 1 1 d R . .
H9B H 0.2262 0.1734 0.0048 0.067 Uiso 1 1 d R . .
C10 C 0.4983(12) 0.2117(5) -0.0414(3) 0.052(2) Uani 1 1 d . . .
H10A H 0.5844 0.1805 -0.0305 0.062 Uiso 1 1 d R . .
H10B H 0.5322 0.2375 -0.0687 0.062 Uiso 1 1 d R . .
C11 C 0.4757(11) 0.2707(5) -0.0050(3) 0.052(3) Uani 1 1 d . . .
H11A H 0.4383 0.2478 0.0236 0.063 Uiso 1 1 d R . .
H11B H 0.4093 0.3076 -0.0151 0.063 Uiso 1 1 d R . .
C12 C 0.6350(11) 0.3011(5) 0.0080(3) 0.050(2) Uani 1 1 d . . .
H12A H 0.7033 0.2608 0.0175 0.060 Uiso 1 1 calc R . .
H12B H 0.6821 0.3235 -0.0196 0.060 Uiso 1 1 calc R . .
C13 C 0.5877(11) 0.3261(5) 0.0929(3) 0.050(2) Uani 1 1 d . . .
H13A H 0.6472 0.2812 0.0982 0.060 Uiso 1 1 calc R . .
H13B H 0.4755 0.3140 0.0932 0.060 Uiso 1 1 calc R . .
C14 C 0.6229(11) 0.3803(5) 0.1318(3) 0.046(2) Uani 1 1 d . . .
H14A H 0.5446 0.4179 0.1311 0.056 Uiso 1 1 d R . .
H14B H 0.7257 0.3991 0.1263 0.056 Uiso 1 1 d R . .
C15 C 0.6162(10) 0.3416(5) 0.1794(3) 0.045(2) Uani 1 1 d . . .
H15A H 0.6519 0.3791 0.2016 0.054 Uiso 1 1 d R . .
H15B H 0.6927 0.3032 0.1785 0.054 Uiso 1 1 d R . .
C16 C 0.3361(10) 0.3724(5) 0.1982(3) 0.048(2) Uani 1 1 d . . .
H16A H 0.2879 0.3762 0.1678 0.057 Uiso 1 1 d R . .
H16B H 0.3776 0.4186 0.2078 0.057 Uiso 1 1 d R . .
C17 C 0.2068(11) 0.3476(5) 0.2300(3) 0.043(2) Uani 1 1 d . . .
C18 C 0.0568(10) 0.3786(5) 0.2336(3) 0.048(2) Uani 1 1 d . . .
H18 H 0.0346 0.4220 0.2148 0.057 Uiso 1 1 d R . .
C19 C -0.0418(11) 0.3521(6) 0.2665(3) 0.054(3) Uani 1 1 d . . .
H19 H -0.1407 0.3635 0.2677 0.065 Uiso 1 1 d R . .
C20 C 0.0000(12) 0.2944(6) 0.2957(3) 0.056(3) Uani 1 1 d . . .
H20 H -0.0657 0.2819 0.3207 0.067 Uiso 1 1 d R . .
C21 C 0.1473(11) 0.2655(5) 0.2908(3) 0.046(2) Uani 1 1 d . . .
Cl1 Cl 0.5498(3) 0.37054(14) 0.33438(10) 0.0578(7) Uani 1 1 d D . .
O11 O 0.5771(8) 0.2992(4) 0.3155(3) 0.087(3) Uani 1 1 d D . .
O13 O 0.4201(12) 0.3701(6) 0.3646(4) 0.144(5) Uani 1 1 d D . .
O12 O 0.6871(9) 0.3967(5) 0.3560(4) 0.114(4) Uani 1 1 d D . .
O14 O 0.5156(13) 0.4176(5) 0.2954(3) 0.123(4) Uani 1 1 d D . .
Cl2 Cl 0.0539(3) 0.26171(14) 0.11675(9) 0.0646(7) Uani 1 1 d D . .
O21A O -0.058(2) 0.2088(10) 0.1325(7) 0.127(9) Uiso 0.52(2) 1 d PD A 1
O23A O 0.1934(16) 0.2481(10) 0.1434(5) 0.085(6) Uiso 0.52(2) 1 d PD A 1
O24A O 0.083(2) 0.2518(14) 0.0690(5) 0.124(8) Uiso 0.52(2) 1 d PD A 1
O21B O -0.064(2) 0.2289(13) 0.0885(7) 0.136(10) Uiso 0.48(2) 1 d PD A 2
O23B O 0.100(3) 0.2202(12) 0.1547(6) 0.133(10) Uiso 0.48(2) 1 d PD A 2
O24B O 0.186(2) 0.2770(11) 0.0857(6) 0.114(8) Uiso 0.48(2) 1 d PD A 2
O22 O -0.0032(11) 0.3343(4) 0.1280(3) 0.095(3) Uani 1 1 d D A .
Cl3 Cl 0.4960(3) 0.11500(12) 0.11176(8) 0.0481(6) Uani 1 1 d . . .
O31 O 0.3286(8) 0.1101(5) 0.1000(3) 0.080(2) Uani 1 1 d . . .
O33 O 0.5452(11) 0.0447(4) 0.1265(3) 0.090(3) Uani 1 1 d . . .
O32 O 0.5152(11) 0.1660(4) 0.1495(3) 0.082(2) Uani 1 1 d . . .
O34 O 0.5783(11) 0.1378(5) 0.0706(3) 0.095(3) Uani 1 1 d . . .
Cl4 Cl 0.0001(3) 0.27955(17) 0.43427(9) 0.0642(7) Uani 1 1 d . . .
O41 O -0.1139(10) 0.2492(7) 0.4023(3) 0.108(3) Uani 1 1 d . . .
O42 O 0.0936(13) 0.3305(7) 0.4127(4) 0.134(4) Uani 1 1 d . . .
O43 O 0.094(2) 0.2243(6) 0.4502(7) 0.214(10) Uani 1 1 d . . .
O44 O -0.0779(17) 0.3055(11) 0.4707(5) 0.202(8) Uani 1 1 d . . .
Cl5 Cl 0.7845(3) 0.06918(14) 0.32779(8) 0.0562(6) Uani 1 1 d . . .
O51 O 0.7126(14) 0.0178(4) 0.2977(3) 0.111(3) Uani 1 1 d . . .
O52 O 0.8639(12) 0.1246(6) 0.3020(3) 0.117(4) Uani 1 1 d . . .
O53 O 0.8698(17) 0.0379(6) 0.3627(4) 0.144(5) Uani 1 1 d . . .
O54 O 0.6685(14) 0.1069(9) 0.3487(5) 0.160(5) Uani 1 1 d . . .
Cl6 Cl 0.3273(3) 0.51673(16) 0.06659(12) 0.0771(9) Uani 1 1 d . . .
O61 O 0.4918(12) 0.5186(6) 0.0569(4) 0.121(4) Uani 1 1 d . . .
O62 O 0.2844(16) 0.4494(8) 0.0813(6) 0.203(8) Uani 1 1 d . . .
O63 O 0.2328(16) 0.5461(7) 0.0349(6) 0.177(7) Uani 1 1 d . . .
O64 O 0.322(3) 0.5641(13) 0.1074(7) 0.281(12) Uani 1 1 d . . .
O1 O 0.6562(7) 0.1984(3) 0.2395(2) 0.0493(15) Uani 1 1 d . . .
H1WA H 0.7112 0.2014 0.2632 0.059 Uiso 1 1 calc R . .
H1WB H 0.6134 0.1668 0.2209 0.059 Uiso 1 1 d R . .
O2 O 0.0454(8) 0.4087(4) 0.5369(3) 0.0662(19) Uani 1 1 d D . .
H2WA H 0.0046(11) 0.3829(6) 0.5162(5) 0.079 Uiso 1 1 d RD . .
H2WB H 0.0348(8) 0.4061(4) 0.5648(6) 0.079 Uiso 1 1 d RD . .
O3 O 0.2336(9) 0.0598(5) 0.7021(2) 0.076(2) Uani 1 1 d . . .
H3WA H 0.201(3) 0.0494(11) 0.730(3) 0.091 Uiso 1 1 d R . .
H3WB H 0.321(8) 0.0406(18) 0.6916(9) 0.091 Uiso 1 1 d R . .
O4 O 0.4027(15) -0.0429(5) 0.0428(3) 0.120(4) Uani 1 1 d D . .
H4WA H 0.3974(15) -0.0593(6) 0.0695(6) 0.144 Uiso 1 1 d RD . .
H4WB H 0.494(2) -0.0435(5) 0.0319(4) 0.144 Uiso 1 1 d RD . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0377(5) 0.0402(5) 0.0423(5) -0.0005(5) 0.0004(5) -0.0003(5)
N1 0.033(4) 0.055(5) 0.037(4) -0.011(4) 0.003(3) -0.002(4)
N2 0.048(5) 0.044(4) 0.036(4) 0.000(3) -0.006(4) -0.001(3)
N3 0.061(5) 0.050(5) 0.042(5) -0.009(4) 0.002(4) -0.011(4)
N4 0.062(5) 0.056(5) 0.085(6) -0.022(5) 0.002(5) -0.018(4)
N5 0.066(6) 0.059(5) 0.045(5) 0.003(4) -0.001(4) 0.003(4)
N6 0.048(5) 0.048(5) 0.051(5) 0.002(4) 0.002(4) -0.003(4)
N7 0.030(4) 0.045(4) 0.054(5) -0.008(4) -0.002(3) -0.003(3)
C1 0.048(6) 0.078(7) 0.043(5) 0.000(5) 0.005(5) -0.010(5)
C2 0.055(6) 0.037(5) 0.046(5) 0.009(4) 0.003(4) -0.002(4)
C3 0.057(6) 0.038(5) 0.042(5) 0.003(4) -0.008(4) -0.002(5)
C4 0.072(7) 0.049(6) 0.028(5) 0.002(4) -0.011(4) -0.003(5)
C5 0.086(7) 0.069(6) 0.036(5) -0.020(5) 0.007(5) -0.032(6)
C6 0.076(8) 0.119(11) 0.044(6) -0.017(6) -0.007(5) -0.046(8)
C7 0.066(7) 0.061(7) 0.089(9) -0.019(7) -0.017(6) 0.001(6)
C8 0.077(7) 0.060(6) 0.039(5) 0.000(5) -0.008(5) -0.008(6)
C9 0.059(6) 0.060(7) 0.049(6) -0.009(5) -0.016(5) 0.003(5)
C10 0.054(6) 0.056(6) 0.044(6) -0.002(5) 0.007(4) -0.007(5)
C11 0.047(6) 0.057(7) 0.053(6) -0.003(5) 0.009(4) -0.002(5)
C12 0.048(6) 0.057(6) 0.046(6) -0.002(5) 0.009(4) -0.001(5)
C13 0.049(5) 0.048(6) 0.051(6) 0.005(4) 0.004(5) -0.018(5)
C14 0.037(5) 0.049(5) 0.053(6) -0.003(5) 0.001(4) -0.004(4)
C15 0.032(5) 0.048(5) 0.055(6) 0.005(4) 0.004(4) 0.004(4)
C16 0.043(6) 0.035(5) 0.066(6) -0.005(5) 0.000(5) 0.011(4)
C17 0.046(6) 0.043(5) 0.040(5) -0.003(4) -0.005(4) 0.002(4)
C18 0.033(5) 0.056(6) 0.054(6) -0.004(5) 0.006(4) 0.019(5)
C19 0.041(6) 0.073(7) 0.047(6) -0.024(5) 0.000(5) 0.007(5)
C20 0.044(6) 0.089(8) 0.035(5) -0.018(6) 0.009(4) -0.009(5)
C21 0.048(6) 0.061(7) 0.030(5) -0.006(4) 0.003(4) -0.001(5)
Cl1 0.0485(15) 0.0593(16) 0.0656(16) -0.0216(13) 0.0009(13) -0.0016(12)
O11 0.072(5) 0.068(5) 0.123(7) -0.048(5) -0.029(5) 0.011(4)
O13 0.143(10) 0.123(8) 0.165(10) -0.049(8) 0.097(8) -0.043(7)
O12 0.075(6) 0.101(7) 0.168(10) -0.061(7) -0.036(6) 0.001(5)
O14 0.183(11) 0.091(7) 0.096(7) 0.009(6) -0.017(7) 0.028(7)
Cl2 0.0576(15) 0.0675(19) 0.0686(17) 0.0088(13) -0.0158(12) 0.0081(13)
O22 0.118(7) 0.063(5) 0.105(7) 0.006(5) 0.003(6) 0.048(5)
Cl3 0.0570(14) 0.0408(13) 0.0466(13) -0.0011(11) -0.0018(11) 0.0006(11)
O31 0.057(5) 0.106(6) 0.078(5) -0.001(5) -0.002(4) -0.003(4)
O33 0.115(7) 0.051(4) 0.105(7) -0.003(4) -0.049(5) 0.004(4)
O32 0.121(7) 0.061(5) 0.063(5) -0.021(4) -0.023(5) 0.010(4)
O34 0.097(6) 0.128(8) 0.061(5) 0.024(5) 0.003(4) -0.029(6)
Cl4 0.0582(15) 0.0819(18) 0.0525(15) 0.0032(14) -0.0012(13) -0.0112(14)
O41 0.098(6) 0.156(8) 0.069(5) 0.027(6) -0.013(4) -0.060(7)
O42 0.126(8) 0.162(10) 0.113(8) 0.046(7) 0.002(7) -0.072(8)
O43 0.196(15) 0.090(9) 0.36(2) 0.010(10) -0.171(18) -0.012(8)
O44 0.168(12) 0.32(2) 0.116(10) -0.110(12) 0.073(9) -0.117(14)
Cl5 0.0695(16) 0.0560(14) 0.0432(13) 0.0057(12) -0.0044(12) -0.0101(13)
O51 0.201(10) 0.072(6) 0.060(5) 0.008(4) -0.032(6) -0.051(6)
O52 0.128(8) 0.148(9) 0.075(6) 0.030(6) -0.015(5) -0.068(7)
O53 0.205(12) 0.111(7) 0.116(8) 0.032(6) -0.092(9) 0.003(8)
O54 0.106(8) 0.229(14) 0.144(10) -0.075(11) -0.029(7) 0.038(10)
Cl6 0.0500(16) 0.075(2) 0.106(2) 0.0397(18) -0.0108(15) -0.0017(13)
O61 0.075(6) 0.125(9) 0.164(10) 0.056(8) 0.001(6) 0.010(5)
O62 0.146(11) 0.168(11) 0.294(18) 0.160(13) -0.129(12) -0.082(9)
O63 0.154(11) 0.149(10) 0.228(15) 0.079(10) -0.118(11) -0.004(9)
O64 0.40(4) 0.28(2) 0.168(15) -0.094(16) 0.006(18) 0.09(2)
O1 0.048(4) 0.046(4) 0.054(4) -0.001(3) 0.000(3) 0.008(3)
O2 0.062(5) 0.063(4) 0.074(5) 0.015(4) 0.016(4) -0.001(3)
O3 0.072(5) 0.103(6) 0.052(4) -0.012(4) 0.009(4) 0.017(4)
O4 0.174(10) 0.091(6) 0.095(7) -0.021(5) -0.053(7) 0.050(7)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 1.909(7) . ?
Cu1 O1 1.966(6) . ?
Cu1 N7 2.043(8) . ?
Cu1 N2 2.063(7) . ?
Cu1 O11 2.338(7) . ?
N1 C21 1.329(11) . ?
N1 C17 1.353(11) . ?
N2 C1 1.505(12) . ?
N2 C2 1.519(11) . ?
N2 H2 0.9100 . ?
N3 C5 1.493(12) . ?
N3 C4 1.521(11) . ?
N3 H3C 0.9566 . ?
N3 H3D 0.9449 . ?
N4 C7 1.459(14) . ?
N4 C8 1.550(13) . ?
N4 H4C 0.9451 . ?
N4 H4D 0.9427 . ?
N5 C9 1.469(12) . ?
N5 C10 1.502(12) . ?
N5 H5C 0.9597 . ?
N5 H5D 0.9555 . ?
N6 C13 1.478(12) . ?
N6 C12 1.492(12) . ?
N6 H6C 0.9403 . ?
N6 H6D 0.9568 . ?
N7 C15 1.474(11) . ?
N7 C16 1.486(11) . ?
N7 H7 0.9100 . ?
C1 C21 1.528(13) . ?
C1 H1A 0.9436 . ?
C1 H1B 0.9654 . ?
C2 C3 1.483(12) . ?
C2 H2A 0.9650 . ?
C2 H2B 0.9494 . ?
C3 C4 1.503(13) . ?
C3 H3A 0.9727 . ?
C3 H3B 0.9678 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.523(15) . ?
C5 H5A 0.9618 . ?
C5 H5B 0.9338 . ?
C6 C7 1.494(16) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9642 . ?
C7 H7B 0.9435 . ?
C8 C9 1.479(13) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9644 . ?
C9 H9B 0.9533 . ?
C10 C11 1.503(13) . ?
C10 H10A 0.9711 . ?
C10 H10B 0.9541 . ?
C11 C12 1.497(13) . ?
C11 H11A 0.9672 . ?
C11 H11B 0.9201 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.514(13) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.530(13) . ?
C14 H14A 0.9490 . ?
C14 H14B 0.9432 . ?
C15 H15A 0.9767 . ?
C15 H15B 0.9501 . ?
C16 C17 1.485(13) . ?
C16 H16A 0.9580 . ?
C16 H16B 0.9495 . ?
C17 C18 1.386(12) . ?
C18 C19 1.341(13) . ?
C18 H18 0.9716 . ?
C19 C20 1.385(15) . ?
C19 H19 0.8587 . ?
C20 C21 1.353(13) . ?
C20 H20 0.9295 . ?
Cl1 O13 1.390(8) . ?
Cl1 O12 1.393(7) . ?
Cl1 O11 1.423(7) . ?
Cl1 O14 1.431(8) . ?
Cl2 O23B 1.376(14) . ?
Cl2 O24A 1.394(13) . ?
Cl2 O21B 1.409(14) . ?
Cl2 O21A 1.417(13) . ?
Cl2 O23A 1.419(11) . ?
Cl2 O22 1.441(7) . ?
Cl2 O24B 1.449(13) . ?
Cl3 O33 1.408(8) . ?
Cl3 O34 1.425(9) . ?
Cl3 O32 1.429(7) . ?
Cl3 O31 1.450(7) . ?
Cl4 O44 1.315(12) . ?
Cl4 O43 1.357(12) . ?
Cl4 O42 1.362(10) . ?
Cl4 O41 1.433(9) . ?
Cl5 O54 1.334(12) . ?
Cl5 O53 1.351(9) . ?
Cl5 O51 1.406(8) . ?
Cl5 O52 1.416(9) . ?
Cl6 O63 1.316(10) . ?
Cl6 O62 1.344(11) . ?
Cl6 O61 1.412(10) . ?
Cl6 O64 1.448(17) . ?
O1 H1WA 0.8200 . ?
O1 H1WB 0.8609 . ?
O2 H2WA 0.8271 . ?
O2 H2WB 0.8014 . ?
O3 H3WA 0.86(8) . ?
O3 H3WB 0.8655 . ?
O4 H4WA 0.8194 . ?
O4 H4WB 0.8283 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 O1 177.8(3) . . ?
N1 Cu1 N7 82.5(3) . . ?
O1 Cu1 N7 96.3(3) . . ?
N1 Cu1 N2 82.7(3) . . ?
O1 Cu1 N2 98.0(3) . . ?
N7 Cu1 N2 157.0(3) . . ?
N1 Cu1 O11 97.4(3) . . ?
O1 Cu1 O11 84.8(3) . . ?
N7 Cu1 O11 111.6(3) . . ?
N2 Cu1 O11 87.7(3) . . ?
C21 N1 C17 121.7(7) . . ?
C21 N1 Cu1 119.7(6) . . ?
C17 N1 Cu1 118.4(6) . . ?
C1 N2 C2 113.5(7) . . ?
C1 N2 Cu1 107.5(5) . . ?
C2 N2 Cu1 111.4(5) . . ?
C1 N2 H2 108.1 . . ?
C2 N2 H2 108.1 . . ?
Cu1 N2 H2 108.1 . . ?
C5 N3 C4 113.6(8) . . ?
C5 N3 H3C 111.3 . . ?
C4 N3 H3C 104.3 . . ?
C5 N3 H3D 109.3 . . ?
C4 N3 H3D 107.2 . . ?
H3C N3 H3D 111.1 . . ?
C7 N4 C8 114.5(9) . . ?
C7 N4 H4C 112.5 . . ?
C8 N4 H4C 108.1 . . ?
C7 N4 H4D 104.4 . . ?
C8 N4 H4D 104.9 . . ?
H4C N4 H4D 112.3 . . ?
C9 N5 C10 113.2(7) . . ?
C9 N5 H5C 105.6 . . ?
C10 N5 H5C 105.7 . . ?
C9 N5 H5D 112.7 . . ?
C10 N5 H5D 109.4 . . ?
H5C N5 H5D 109.9 . . ?
C13 N6 C12 114.1(7) . . ?
C13 N6 H6C 104.0 . . ?
C12 N6 H6C 111.6 . . ?
C13 N6 H6D 105.2 . . ?
C12 N6 H6D 110.2 . . ?
H6C N6 H6D 111.4 . . ?
C15 N7 C16 113.9(7) . . ?
C15 N7 Cu1 116.8(5) . . ?
C16 N7 Cu1 109.6(5) . . ?
C15 N7 H7 105.1 . . ?
C16 N7 H7 105.1 . . ?
Cu1 N7 H7 105.1 . . ?
N2 C1 C21 109.7(7) . . ?
N2 C1 H1A 107.7 . . ?
C21 C1 H1A 111.6 . . ?
N2 C1 H1B 109.3 . . ?
C21 C1 H1B 108.2 . . ?
H1A C1 H1B 110.4 . . ?
C3 C2 N2 112.8(7) . . ?
C3 C2 H2A 107.2 . . ?
N2 C2 H2A 111.2 . . ?
C3 C2 H2B 105.9 . . ?
N2 C2 H2B 109.6 . . ?
H2A C2 H2B 109.9 . . ?
C2 C3 C4 110.2(8) . . ?
C2 C3 H3A 109.6 . . ?
C4 C3 H3A 113.6 . . ?
C2 C3 H3B 107.9 . . ?
C4 C3 H3B 107.5 . . ?
H3A C3 H3B 107.8 . . ?
C3 C4 N3 109.2(7) . . ?
C3 C4 H4A 109.8 . . ?
N3 C4 H4A 109.8 . . ?
C3 C4 H4B 109.8 . . ?
N3 C4 H4B 109.8 . . ?
H4A C4 H4B 108.3 . . ?
N3 C5 C6 111.1(10) . . ?
N3 C5 H5A 107.7 . . ?
C6 C5 H5A 106.1 . . ?
N3 C5 H5B 110.6 . . ?
C6 C5 H5B 109.7 . . ?
H5A C5 H5B 111.6 . . ?
C7 C6 C5 121.5(9) . . ?
C7 C6 H6A 107.0 . . ?
C5 C6 H6A 107.0 . . ?
C7 C6 H6B 107.0 . . ?
C5 C6 H6B 107.0 . . ?
H6A C6 H6B 106.7 . . ?
N4 C7 C6 110.4(10) . . ?
N4 C7 H7A 108.9 . . ?
C6 C7 H7A 115.1 . . ?
N4 C7 H7B 100.4 . . ?
C6 C7 H7B 110.5 . . ?
H7A C7 H7B 110.5 . . ?
C9 C8 N4 111.1(8) . . ?
C9 C8 H8A 109.4 . . ?
N4 C8 H8A 109.4 . . ?
C9 C8 H8B 109.4 . . ?
N4 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
N5 C9 C8 110.9(8) . . ?
N5 C9 H9A 112.7 . . ?
C8 C9 H9A 108.5 . . ?
N5 C9 H9B 105.4 . . ?
C8 C9 H9B 109.6 . . ?
H9A C9 H9B 109.7 . . ?
N5 C10 C11 114.8(8) . . ?
N5 C10 H10A 112.2 . . ?
C11 C10 H10A 107.0 . . ?
N5 C10 H10B 109.0 . . ?
C11 C10 H10B 104.5 . . ?
H10A C10 H10B 109.0 . . ?
C12 C11 C10 108.7(7) . . ?
C12 C11 H11A 104.0 . . ?
C10 C11 H11A 108.4 . . ?
C12 C11 H11B 110.5 . . ?
C10 C11 H11B 112.6 . . ?
H11A C11 H11B 112.3 . . ?
N6 C12 C11 114.2(7) . . ?
N6 C12 H12A 108.7 . . ?
C11 C12 H12A 108.7 . . ?
N6 C12 H12B 108.7 . . ?
C11 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
N6 C13 C14 111.3(7) . . ?
N6 C13 H13A 109.4 . . ?
C14 C13 H13A 109.4 . . ?
N6 C13 H13B 109.4 . . ?
C14 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
C13 C14 C15 110.0(8) . . ?
C13 C14 H14A 108.5 . . ?
C15 C14 H14A 109.0 . . ?
C13 C14 H14B 107.1 . . ?
C15 C14 H14B 110.3 . . ?
H14A C14 H14B 111.9 . . ?
N7 C15 C14 115.5(7) . . ?
N7 C15 H15A 109.9 . . ?
C14 C15 H15A 103.9 . . ?
N7 C15 H15B 111.5 . . ?
C14 C15 H15B 106.7 . . ?
H15A C15 H15B 108.9 . . ?
C17 C16 N7 110.2(7) . . ?
C17 C16 H16A 105.2 . . ?
N7 C16 H16A 105.3 . . ?
C17 C16 H16B 111.2 . . ?
N7 C16 H16B 113.9 . . ?
H16A C16 H16B 110.5 . . ?
N1 C17 C18 119.4(8) . . ?
N1 C17 C16 114.4(8) . . ?
C18 C17 C16 126.0(8) . . ?
C19 C18 C17 117.9(9) . . ?
C19 C18 H18 123.9 . . ?
C17 C18 H18 117.7 . . ?
C18 C19 C20 122.4(9) . . ?
C18 C19 H19 122.8 . . ?
C20 C19 H19 113.8 . . ?
C21 C20 C19 117.7(9) . . ?
C21 C20 H20 121.9 . . ?
C19 C20 H20 119.7 . . ?
N1 C21 C20 120.8(9) . . ?
N1 C21 C1 113.2(8) . . ?
C20 C21 C1 125.8(8) . . ?
O13 Cl1 O12 112.3(6) . . ?
O13 Cl1 O11 110.8(5) . . ?
O12 Cl1 O11 110.2(4) . . ?
O13 Cl1 O14 109.1(7) . . ?
O12 Cl1 O14 107.8(6) . . ?
O11 Cl1 O14 106.5(5) . . ?
Cl1 O11 Cu1 126.8(4) . . ?
O23B Cl2 O21B 114.6(11) . . ?
O24A Cl2 O21A 109.8(10) . . ?
O24A Cl2 O23A 110.6(9) . . ?
O21A Cl2 O23A 105.1(9) . . ?
O23B Cl2 O22 115.0(11) . . ?
O24A Cl2 O22 113.3(11) . . ?
O21B Cl2 O22 106.3(12) . . ?
O21A Cl2 O22 109.3(10) . . ?
O23A Cl2 O22 108.4(9) . . ?
O23B Cl2 O24B 111.5(10) . . ?
O21B Cl2 O24B 105.9(9) . . ?
O22 Cl2 O24B 102.5(9) . . ?
O33 Cl3 O34 111.5(6) . . ?
O33 Cl3 O32 109.4(5) . . ?
O34 Cl3 O32 112.1(6) . . ?
O33 Cl3 O31 107.4(5) . . ?
O34 Cl3 O31 107.4(5) . . ?
O32 Cl3 O31 108.8(5) . . ?
O44 Cl4 O43 107.1(13) . . ?
O44 Cl4 O42 113.5(10) . . ?
O43 Cl4 O42 108.5(10) . . ?
O44 Cl4 O41 107.8(7) . . ?
O43 Cl4 O41 108.5(7) . . ?
O42 Cl4 O41 111.3(6) . . ?
O54 Cl5 O53 106.1(9) . . ?
O54 Cl5 O51 107.5(7) . . ?
O53 Cl5 O51 113.4(6) . . ?
O54 Cl5 O52 102.1(10) . . ?
O53 Cl5 O52 115.6(7) . . ?
O51 Cl5 O52 111.1(5) . . ?
O63 Cl6 O62 114.9(8) . . ?
O63 Cl6 O61 116.6(9) . . ?
O62 Cl6 O61 110.3(8) . . ?
O63 Cl6 O64 107.0(12) . . ?
O62 Cl6 O64 106.5(13) . . ?
O61 Cl6 O64 99.8(13) . . ?
Cu1 O1 H1WA 109.5 . . ?
Cu1 O1 H1WB 91.6 . . ?
H1WA O1 H1WB 142.0 . . ?
H2WA O2 H2WB 128.7 . . ?
H3WA O3 H3WB 119.9 . . ?
H4WA O4 H4WB 113.2 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1WA O52 0.82 2.20 2.831(12) 134.4 .
O1 H1WB O32 0.86 2.20 2.887(10) 137.0 .
O2 H2WB O22 0.80 2.24 2.950(11) 147.7 3
O2 H2WA O44 0.83 2.04 2.856(14) 170.7 .
O3 H3WA O51 0.86 2.13 2.865(11) 141.5 3_655
O3 H3WB O33 0.87 2.17 2.859(10) 136.1 3_655
O4 H4WB O61 0.83 2.77 3.178(17) 112.0 2_645
O4 H4WA O13 0.82 2.28 3.081(14) 164.8 4_545
N2 H2 O54 0.91 2.37 3.234(14) 159.2 .
N3 H3D O3 0.94 1.94 2.819(11) 154.5 3_554
N3 H3C O31 0.96 2.16 2.913(11) 134.7 .
N4 H4D O4 0.94 2.11 2.937(14) 146.3 .
N4 H4C O2 0.95 1.87 2.755(11) 154.5 4_545
N5 H5D O41 0.96 1.84 2.789(11) 170.4 3_554
N5 H5C O54 0.96 2.33 3.025(14) 128.4 3_654
N5 H5C O61 0.96 2.29 3.031(14) 133.6 2_645
N6 H6D O61 0.96 2.39 3.183(13) 140.4 .
N6 H6D O4 0.96 2.66 3.145(12) 111.9 2_655
N7 H7 O32 0.91 2.37 3.008(10) 126.9 .

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        22.78
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.088
_database_code_depnum_ccdc_archive 'CCDC 934155'