# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
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#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H38 Cl2 Cu2 N6 O11'
_chemical_formula_weight         712.52

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'
O O 0.0106 0.0060 '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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P212121

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

_cell_length_a                   10.456(5)
_cell_length_b                   13.413(5)
_cell_length_c                   21.207(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2974.2(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    36491
_cell_measurement_theta_min      0.96
_cell_measurement_theta_max      26.70

_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1472
_exptl_absorpt_coefficient_mu    1.671
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7998
_exptl_absorpt_correction_T_max  0.8507
_exptl_absorpt_process_details   SADABS

_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 area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            36491
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         0.96
_diffrn_reflns_theta_max         26.70
_reflns_number_total             6164
_reflns_number_gt                5189
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material  'WINGX V1.80.03'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

  the crystal was twinned. Refinement was carried out with 
  twin -1 0 0 0 1 0 0 0 1 and BASF refined to 0.38(1)

  the water molecule O1W had high thermal motion but attempts to refine
  the atom in two positions did not reduce the R value significantly
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0708P)²+0.5771P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(7)
_refine_ls_number_reflns         6164
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0408
_refine_ls_wR_factor_ref         0.1118
_refine_ls_wR_factor_gt          0.1046
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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 -0.11062(4) 0.00264(3) 0.094422(19) 0.04100(13) Uani 1 1 d . . .
Cu2 Cu -0.06877(5) -0.21918(3) 0.18526(2) 0.04806(14) Uani 1 1 d . . .
O11 O 0.0670(3) -0.1240(2) 0.16914(14) 0.0587(7) Uani 1 1 d . . .
N12 N 0.0500(3) -0.0642(2) 0.11993(16) 0.0455(8) Uani 1 1 d . . .
C13 C 0.1500(4) -0.0334(3) 0.0902(2) 0.0483(9) Uani 1 1 d . . .
C14 C 0.1199(5) 0.0258(3) 0.0338(2) 0.0537(11) Uani 1 1 d . . .
C16 C -0.0348(6) 0.1007(5) -0.0325(2) 0.0778(16) Uani 1 1 d . . .
H16A H 0.0084 0.0737 -0.0692 0.093 Uiso 1 1 calc R . .
H16B H -0.0109 0.1702 -0.0284 0.093 Uiso 1 1 calc R . .
C17 C -0.1811(8) 0.0920(7) -0.0411(3) 0.122(3) Uani 1 1 d . . .
H17A H -0.2031 0.1254 -0.0802 0.146 Uiso 1 1 calc R . .
H17B H -0.2012 0.0220 -0.0466 0.146 Uiso 1 1 calc R . .
C18 C -0.2594(7) 0.1283(7) 0.0047(3) 0.118(3) Uani 1 1 d . . .
H18A H -0.3429 0.1401 -0.0139 0.142 Uiso 1 1 calc R . .
H18B H -0.2261 0.1924 0.0181 0.142 Uiso 1 1 calc R . .
N15 N 0.0045(4) 0.0457(3) 0.02388(15) 0.0489(8) Uani 1 1 d . . .
N19 N -0.2768(4) 0.0655(4) 0.0611(2) 0.0738(12) Uani 1 1 d . . .
C20 C -0.3356(8) 0.1340(6) 0.1067(4) 0.123(3) Uani 1 1 d . . .
H20A H -0.2827 0.1920 0.1113 0.185 Uiso 1 1 calc R . .
H20B H -0.3440 0.1011 0.1467 0.185 Uiso 1 1 calc R . .
H20C H -0.4186 0.1535 0.0918 0.185 Uiso 1 1 calc R . .
C21 C -0.3661(6) -0.0189(8) 0.0505(4) 0.120(3) Uani 1 1 d . . .
H21A H -0.4431 0.0054 0.0313 0.180 Uiso 1 1 calc R . .
H21B H -0.3863 -0.0496 0.0902 0.180 Uiso 1 1 calc R . .
H21C H -0.3265 -0.0670 0.0233 0.180 Uiso 1 1 calc R . .
O21 O -0.1981(3) -0.02172(18) 0.17344(12) 0.0464(6) Uani 1 1 d . . .
N22 N -0.2025(3) -0.1152(2) 0.19427(14) 0.0418(7) Uani 1 1 d . . .
C23 C -0.2970(4) -0.1397(3) 0.23025(18) 0.0482(9) Uani 1 1 d . . .
C24 C -0.2993(5) -0.2476(4) 0.24487(19) 0.0554(11) Uani 1 1 d . . .
N25 N -0.2081(4) -0.2998(3) 0.22288(17) 0.0552(9) Uani 1 1 d . . .
C26 C -0.2068(6) -0.4086(4) 0.2310(3) 0.0762(15) Uani 1 1 d . . .
H26A H -0.2918 -0.4348 0.2231 0.091 Uiso 1 1 calc R . .
H26B H -0.1841 -0.4244 0.2742 0.091 Uiso 1 1 calc R . .
C27 C -0.1131(8) -0.4577(4) 0.1870(4) 0.107(2) Uani 1 1 d . . .
H27A H -0.1229 -0.5295 0.1902 0.129 Uiso 1 1 calc R . .
H27B H -0.1336 -0.4387 0.1441 0.129 Uiso 1 1 calc R . .
C28 C 0.0208(8) -0.4317(4) 0.2000(4) 0.099(2) Uani 1 1 d . . .
H28A H 0.0751 -0.4832 0.1822 0.119 Uiso 1 1 calc R . .
H28B H 0.0336 -0.4319 0.2453 0.119 Uiso 1 1 calc R . .
N29 N 0.0641(5) -0.3323(3) 0.1746(2) 0.0700(11) Uani 1 1 d . . .
C30 C 0.0909(10) -0.3361(6) 0.1040(3) 0.124(3) Uani 1 1 d . . .
H30A H 0.1088 -0.2702 0.0889 0.186 Uiso 1 1 calc R . .
H30B H 0.0175 -0.3623 0.0824 0.186 Uiso 1 1 calc R . .
H30C H 0.1634 -0.3784 0.0963 0.186 Uiso 1 1 calc R . .
C31 C 0.1847(6) -0.3088(5) 0.2079(3) 0.0862(18) Uani 1 1 d . . .
H31A H 0.1662 -0.2916 0.2509 0.129 Uiso 1 1 calc R . .
H31B H 0.2261 -0.2536 0.1875 0.129 Uiso 1 1 calc R . .
H31C H 0.2400 -0.3659 0.2069 0.129 Uiso 1 1 calc R . .
C131 C 0.2825(5) -0.0612(5) 0.1100(3) 0.0820(17) Uani 1 1 d . . .
H13A H 0.3042 -0.1250 0.0925 0.123 Uiso 1 1 calc R . .
H13B H 0.2867 -0.0644 0.1551 0.123 Uiso 1 1 calc R . .
H13C H 0.3417 -0.0119 0.0949 0.123 Uiso 1 1 calc R . .
C141 C 0.2293(6) 0.0564(5) -0.0084(3) 0.0825(17) Uani 1 1 d . . .
H14A H 0.2605 0.1206 0.0044 0.124 Uiso 1 1 calc R . .
H14B H 0.2001 0.0598 -0.0513 0.124 Uiso 1 1 calc R . .
H14C H 0.2970 0.0083 -0.0052 0.124 Uiso 1 1 calc R . .
C231 C -0.3982(5) -0.0701(4) 0.2507(3) 0.0767(15) Uani 1 1 d . . .
H23A H -0.4791 -0.0919 0.2344 0.115 Uiso 1 1 calc R . .
H23B H -0.3796 -0.0045 0.2352 0.115 Uiso 1 1 calc R . .
H23C H -0.4016 -0.0687 0.2960 0.115 Uiso 1 1 calc R . .
C241 C -0.4082(6) -0.2879(5) 0.2828(3) 0.0863(17) Uani 1 1 d . . .
H24A H -0.3753 -0.3246 0.3182 0.129 Uiso 1 1 calc R . .
H24B H -0.4590 -0.3313 0.2570 0.129 Uiso 1 1 calc R . .
H24C H -0.4601 -0.2338 0.2977 0.129 Uiso 1 1 calc R . .
O1W O -0.1528(5) -0.1986(6) 0.0705(2) 0.141(3) Uani 1 1 d . . .
H1W1 H -0.0982 -0.2273 0.0383 0.169 Uiso 1 1 calc R . .
H1W2 H -0.2418 -0.2168 0.0646 0.169 Uiso 1 1 calc R . .
Cl4 Cl 0.02917(15) 0.25630(10) 0.13241(6) 0.0724(4) Uani 1 1 d . . .
Cl5 Cl -0.48133(13) -0.31566(10) 0.09131(7) 0.0711(3) Uani 1 1 d . . .
O41 O -0.0446(5) 0.1691(3) 0.1468(2) 0.1042(17) Uani 1 1 d . . .
O42 O 0.1524(5) 0.2213(4) 0.1164(2) 0.1073(15) Uani 1 1 d . . .
O43 O 0.0255(6) 0.3159(3) 0.1868(2) 0.1166(19) Uani 1 1 d . . .
O44 O -0.0280(5) 0.3053(4) 0.0816(2) 0.1183(18) Uani 1 1 d . . .
O51 O -0.3777(7) -0.3202(6) 0.0527(4) 0.176(3) Uani 1 1 d . . .
O52 O -0.5894(6) -0.3238(7) 0.0567(3) 0.167(3) Uani 1 1 d . . .
O53 O -0.4829(5) -0.2314(4) 0.1305(3) 0.1112(16) Uani 1 1 d . . .
O54 O -0.4748(10) -0.3993(4) 0.1278(3) 0.177(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O21 1.937(3) . ?
Cu1 N12 1.978(3) . ?
Cu1 N15 2.005(3) . ?
Cu1 N19 2.057(4) . ?
Cu1 O1W 2.782(7) . ?
Cu1 O41 2.588(4) . ?
Cu2 O11 1.940(3) . ?
Cu2 N25 1.982(4) . ?
Cu2 N22 1.984(3) . ?
Cu2 N29 2.069(4) . ?
Cu2 O1W 2.601(5) . ?
O11 N12 1.329(4) . ?
N12 C13 1.288(5) . ?
C13 C14 1.469(6) . ?
C13 C131 1.494(7) . ?
C14 N15 1.254(6) . ?
C14 C141 1.511(7) . ?
C16 N15 1.464(6) . ?
C16 C17 1.545(10) . ?
C17 C18 1.360(10) . ?
C18 N19 1.474(7) . ?
N19 C20 1.468(9) . ?
N19 C21 1.484(9) . ?
O21 N22 1.330(4) . ?
N22 C23 1.291(5) . ?
C23 C231 1.476(7) . ?
C23 C24 1.480(6) . ?
C24 N25 1.271(6) . ?
C24 C241 1.495(7) . ?
N25 C26 1.470(6) . ?
C26 C27 1.505(9) . ?
C27 C28 1.470(10) . ?
C28 N29 1.507(8) . ?
N29 C31 1.480(8) . ?
N29 C30 1.523(7) . ?
Cl4 O44 1.397(4) . ?
Cl4 O43 1.405(5) . ?
Cl4 O42 1.413(6) . ?
Cl4 O41 1.433(4) . ?
Cl5 O52 1.352(6) . ?
Cl5 O51 1.360(6) . ?
Cl5 O54 1.364(6) . ?
Cl5 O53 1.403(5) . ?

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
O21 Cu1 N12 95.04(12) . . ?
O21 Cu1 N15 167.83(13) . . ?
N12 Cu1 N15 79.92(15) . . ?
O21 Cu1 N19 88.15(15) . . ?
N12 Cu1 N19 175.27(18) . . ?
N15 Cu1 N19 97.62(16) . . ?
O21 Cu1 O1W 85.35(12) . . ?
N12 Cu1 O1W 75.22(15) . . ?
N15 Cu1 O1W 103.83(14) . . ?
N19 Cu1 O1W 101.62(19) . . ?
O21 Cu1 O41 84.27(12) . . ?
N12 Cu1 O41 92.69(16) . . ?
N15 Cu1 O41 84.91(14) . . ?
N19 Cu1 O41 91.1(2) . . ?
O1W Cu1 O41 163.29(16) . . ?
O11 Cu2 N25 165.47(14) . . ?
O11 Cu2 N22 94.03(13) . . ?
N25 Cu2 N22 80.00(15) . . ?
O11 Cu2 N29 88.38(16) . . ?
N25 Cu2 N29 97.92(17) . . ?
N22 Cu2 N29 177.30(17) . . ?
O11 Cu2 O1W 90.73(16) . . ?
N25 Cu2 O1W 100.72(16) . . ?
N22 Cu2 O1W 77.15(17) . . ?
N29 Cu2 O1W 101.6(2) . . ?
C24 Cu2 O1W 98.56(14) . . ?
N12 O11 Cu2 116.0(2) . . ?
C13 N12 O11 117.9(3) . . ?
C13 N12 Cu1 114.2(3) . . ?
O11 N12 Cu1 127.0(3) . . ?
N12 C13 C14 113.4(4) . . ?
N12 C13 C131 122.4(4) . . ?
C14 C13 C131 124.1(4) . . ?
N15 C14 C13 117.3(4) . . ?
N15 C14 C141 124.8(5) . . ?
C13 C14 C141 117.9(4) . . ?
N15 C16 C17 109.7(5) . . ?
C18 C17 C16 119.0(7) . . ?
C17 C18 N19 116.7(7) . . ?
C14 N15 C16 121.0(4) . . ?
C14 N15 Cu1 113.0(3) . . ?
C16 N15 Cu1 125.9(3) . . ?
C20 N19 C18 103.2(6) . . ?
C20 N19 C21 108.2(6) . . ?
C18 N19 C21 113.0(6) . . ?
C20 N19 Cu1 112.6(4) . . ?
C18 N19 Cu1 114.1(4) . . ?
C21 N19 Cu1 105.7(4) . . ?
N22 O21 Cu1 117.6(2) . . ?
C23 N22 O21 117.5(3) . . ?
C23 N22 Cu2 114.7(3) . . ?
O21 N22 Cu2 127.3(2) . . ?
N22 C23 C231 124.2(4) . . ?
N22 C23 C24 112.6(4) . . ?
C231 C23 C24 123.0(4) . . ?
N25 C24 C23 116.7(4) . . ?
N25 C24 C241 124.7(5) . . ?
C23 C24 C241 118.6(5) . . ?
C24 N25 C26 120.7(4) . . ?
C24 N25 Cu2 113.5(3) . . ?
C26 N25 Cu2 125.6(4) . . ?
N25 C26 C27 111.6(5) . . ?
C28 C27 C26 113.6(6) . . ?
C27 C28 N29 115.5(6) . . ?
C31 N29 C28 105.9(5) . . ?
C31 N29 C30 108.6(6) . . ?
C28 N29 C30 112.1(5) . . ?
C31 N29 Cu2 111.3(3) . . ?
C28 N29 Cu2 114.1(4) . . ?
C30 N29 Cu2 104.8(4) . . ?
Cu1 O1W Cu2 83.05(14) . . ?
O44 Cl4 O43 110.8(3) . . ?
O44 Cl4 O42 111.2(3) . . ?
O43 Cl4 O42 114.3(3) . . ?
O44 Cl4 O41 108.5(3) . . ?
O43 Cl4 O41 105.9(3) . . ?
O42 Cl4 O41 105.7(3) . . ?
O52 Cl5 O51 109.6(5) . . ?
O52 Cl5 O54 106.5(6) . . ?
O51 Cl5 O54 105.4(6) . . ?
O52 Cl5 O53 112.1(4) . . ?
O51 Cl5 O53 113.7(4) . . ?
O54 Cl5 O53 109.0(4) . . ?
Cl4 O41 Cu1 139.1(3) . . ?

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
O1W H1W2 O51 0.97 2.00 2.887(9) 150.6 .
O1W H1W1 O52 0.97 2.13 2.795(8) 124.4 3_545

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        26.70
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.070
_database_code_depnum_ccdc_archive 'CCDC 973637'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H38 B2 Cu2 F8 N6 O3'
_chemical_formula_weight         687.24

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P212121

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

_cell_length_a                   10.4206(3)
_cell_length_b                   13.2830(3)
_cell_length_c                   21.0965(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2920.11(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    50961
_cell_measurement_theta_min      1.81
_cell_measurement_theta_max      30.98

_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1408
_exptl_absorpt_coefficient_mu    1.538
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8134
_exptl_absorpt_correction_T_max  0.8614
_exptl_absorpt_process_details   sadabs

_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_standards_number         n/a
_diffrn_measurement_device       'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_decay_%        n/a
_diffrn_reflns_number            50961
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.81
_diffrn_reflns_theta_max         30.98
_reflns_number_total             9258
_reflns_number_gt                6316
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material  'WINGX V1.80.03'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0830P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.016(16)
_refine_ls_number_reflns         9258
_refine_ls_number_parameters     360
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0486
_refine_ls_wR_factor_ref         0.1417
_refine_ls_wR_factor_gt          0.1262
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_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 -0.10875(3) 0.00056(3) 0.093074(17) 0.03986(11) Uani 1 1 d . . .
Cu2 Cu -0.06788(4) -0.22227(3) 0.18504(2) 0.04821(12) Uani 1 1 d . . .
O11 O 0.0677(3) -0.1253(2) 0.16999(13) 0.0571(6) Uani 1 1 d . . .
N12 N 0.0521(3) -0.0671(2) 0.11973(14) 0.0446(6) Uani 1 1 d . . .
C13 C 0.1529(3) -0.0372(3) 0.0899(2) 0.0522(8) Uani 1 1 d . . .
C14 C 0.1242(4) 0.0230(3) 0.0326(2) 0.0539(9) Uani 1 1 d . . .
C16 C -0.0301(5) 0.0980(4) -0.0353(2) 0.0781(14) Uani 1 1 d . . .
H16A H 0.0078 0.0656 -0.0719 0.094 Uiso 1 1 calc R . .
H16B H 0.0010 0.1668 -0.0335 0.094 Uiso 1 1 calc R . .
C17 C -0.1738(8) 0.0979(9) -0.0413(3) 0.155(5) Uani 1 1 d . . .
H17A H -0.1933 0.1361 -0.0793 0.186 Uiso 1 1 calc R . .
H17B H -0.1981 0.0288 -0.0502 0.186 Uiso 1 1 calc R . .
C18 C -0.2544(6) 0.1304(8) 0.0029(3) 0.136(4) Uani 1 1 d . . .
H18A H -0.3377 0.1389 -0.0169 0.163 Uiso 1 1 calc R . .
H18B H -0.2258 0.1967 0.0160 0.163 Uiso 1 1 calc R . .
N15 N 0.0072(3) 0.0440(2) 0.02270(15) 0.0488(7) Uani 1 1 d . . .
N19 N -0.2731(3) 0.0692(4) 0.0610(2) 0.0750(12) Uani 1 1 d . . .
C20 C -0.3215(7) 0.1405(6) 0.1070(4) 0.127(3) Uani 1 1 d . . .
H20A H -0.2539 0.1856 0.1193 0.190 Uiso 1 1 calc R . .
H20B H -0.3521 0.1049 0.1437 0.190 Uiso 1 1 calc R . .
H20C H -0.3906 0.1783 0.0887 0.190 Uiso 1 1 calc R . .
C21 C -0.3676(6) -0.0101(8) 0.0517(4) 0.133(3) Uani 1 1 d . . .
H21A H -0.4425 0.0175 0.0318 0.199 Uiso 1 1 calc R . .
H21B H -0.3907 -0.0383 0.0920 0.199 Uiso 1 1 calc R . .
H21C H -0.3319 -0.0618 0.0252 0.199 Uiso 1 1 calc R . .
O21 O -0.1973(2) -0.02357(16) 0.17228(11) 0.0459(5) Uani 1 1 d . . .
N22 N -0.2028(3) -0.1172(2) 0.19277(14) 0.0413(6) Uani 1 1 d . . .
C23 C -0.2972(4) -0.1430(3) 0.22895(17) 0.0494(8) Uani 1 1 d . . .
C24 C -0.2999(4) -0.2516(3) 0.24397(18) 0.0545(9) Uani 1 1 d . . .
N25 N -0.2080(4) -0.3042(2) 0.22214(17) 0.0575(8) Uani 1 1 d . . .
C26 C -0.2089(6) -0.4135(4) 0.2307(3) 0.0836(15) Uani 1 1 d . . .
H26A H -0.2938 -0.4393 0.2213 0.100 Uiso 1 1 calc R . .
H26B H -0.1892 -0.4294 0.2745 0.100 Uiso 1 1 calc R . .
C27 C -0.1122(7) -0.4636(4) 0.1880(4) 0.105(2) Uani 1 1 d . . .
H27A H -0.1209 -0.5361 0.1920 0.126 Uiso 1 1 calc R . .
H27B H -0.1311 -0.4459 0.1444 0.126 Uiso 1 1 calc R . .
C28 C 0.0233(8) -0.4349(4) 0.2025(4) 0.106(2) Uani 1 1 d . . .
H28A H 0.0795 -0.4869 0.1860 0.127 Uiso 1 1 calc R . .
H28B H 0.0339 -0.4335 0.2481 0.127 Uiso 1 1 calc R . .
N29 N 0.0662(5) -0.3349(3) 0.17613(18) 0.0697(10) Uani 1 1 d . . .
C30 C 0.0994(10) -0.3375(6) 0.1070(3) 0.131(3) Uani 1 1 d . . .
H30A H 0.1057 -0.2700 0.0911 0.196 Uiso 1 1 calc R . .
H30B H 0.0337 -0.3730 0.0842 0.196 Uiso 1 1 calc R . .
H30C H 0.1801 -0.3713 0.1014 0.196 Uiso 1 1 calc R . .
C31 C 0.1834(5) -0.3116(4) 0.2120(3) 0.0896(17) Uani 1 1 d . . .
H31A H 0.1623 -0.3019 0.2558 0.134 Uiso 1 1 calc R . .
H31B H 0.2216 -0.2513 0.1954 0.134 Uiso 1 1 calc R . .
H31C H 0.2430 -0.3664 0.2081 0.134 Uiso 1 1 calc R . .
C131 C 0.2855(4) -0.0641(4) 0.1108(3) 0.0782(14) Uani 1 1 d . . .
H13A H 0.3136 -0.1233 0.0887 0.117 Uiso 1 1 calc R . .
H13B H 0.2855 -0.0770 0.1556 0.117 Uiso 1 1 calc R . .
H13C H 0.3427 -0.0093 0.1017 0.117 Uiso 1 1 calc R . .
C141 C 0.2329(5) 0.0496(5) -0.0110(3) 0.0829(15) Uani 1 1 d . . .
H14A H 0.2730 0.1105 0.0034 0.124 Uiso 1 1 calc R . .
H14B H 0.2005 0.0591 -0.0531 0.124 Uiso 1 1 calc R . .
H14C H 0.2948 -0.0040 -0.0110 0.124 Uiso 1 1 calc R . .
C231 C -0.3994(5) -0.0725(4) 0.2489(3) 0.0762(14) Uani 1 1 d . . .
H23A H -0.4814 -0.0983 0.2361 0.114 Uiso 1 1 calc R . .
H23B H -0.3853 -0.0080 0.2295 0.114 Uiso 1 1 calc R . .
H23C H -0.3977 -0.0653 0.2942 0.114 Uiso 1 1 calc R . .
C241 C -0.4109(5) -0.2926(4) 0.2810(3) 0.0862(15) Uani 1 1 d . . .
H24A H -0.3850 -0.3527 0.3027 0.129 Uiso 1 1 calc R . .
H24B H -0.4802 -0.3080 0.2526 0.129 Uiso 1 1 calc R . .
H24C H -0.4388 -0.2433 0.3113 0.129 Uiso 1 1 calc R . .
O1W O -0.1537(5) -0.1997(6) 0.0675(2) 0.163(3) Uani 1 1 d . . .
H1W1 H -0.2432 -0.2172 0.0614 0.196 Uiso 1 1 calc R . .
H1W2 H -0.0993 -0.2286 0.0349 0.196 Uiso 1 1 calc R . .
B4 B 0.0404(7) 0.2542(5) 0.1316(3) 0.0746(15) Uani 1 1 d . . .
B5 B -0.4809(5) -0.3111(5) 0.0916(4) 0.0769(15) Uani 1 1 d . . .
F41 F -0.0317(4) 0.1675(3) 0.1445(2) 0.1144(14) Uani 1 1 d . . .
F42 F 0.1591(4) 0.2189(4) 0.1170(2) 0.1261(14) Uani 1 1 d . . .
F44 F 0.0323(6) 0.3099(3) 0.1851(2) 0.144(2) Uani 1 1 d . . .
F43 F -0.0148(4) 0.3014(4) 0.0824(2) 0.1331(18) Uani 1 1 d . . .
F51 F -0.3718(5) -0.3208(6) 0.0582(4) 0.201(3) Uani 1 1 d . . .
F52 F -0.5820(5) -0.3203(5) 0.0555(3) 0.166(2) Uani 1 1 d . . .
F53 F -0.4818(5) -0.2320(3) 0.1305(2) 0.1277(16) Uani 1 1 d . . .
F54 F -0.4775(9) -0.3965(4) 0.1274(3) 0.199(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O21 1.935(2) . ?
Cu1 N12 1.984(3) . ?
Cu1 N15 1.999(3) . ?
Cu1 N19 2.054(4) . ?
Cu1 F41 2.595(4) . ?
Cu1 O1W 2.755(7) . ?
Cu2 O11 1.938(3) . ?
Cu2 N25 1.982(4) . ?
Cu2 N22 1.988(3) . ?
Cu2 N29 2.056(4) . ?
Cu2 O1W 2.653(6) . ?
O11 N12 1.322(4) . ?
N12 C13 1.288(5) . ?
C13 C14 1.480(6) . ?
C13 C131 1.494(6) . ?
C14 N15 1.268(5) . ?
C14 C141 1.501(6) . ?
C16 N15 1.471(5) . ?
C16 C17 1.502(10) . ?
C17 C18 1.327(11) . ?
C18 N19 1.484(7) . ?
N19 C20 1.448(9) . ?
N19 C21 1.455(9) . ?
O21 N22 1.318(4) . ?
N22 C23 1.291(5) . ?
C23 C24 1.478(6) . ?
C23 C231 1.479(6) . ?
C24 N25 1.272(6) . ?
C24 C241 1.498(6) . ?
N25 C26 1.462(5) . ?
C26 C27 1.506(9) . ?
C27 C28 1.494(10) . ?
C28 N29 1.507(8) . ?
N29 C31 1.469(8) . ?
N29 C30 1.499(8) . ?
B4 F43 1.343(7) . ?
B4 F44 1.353(8) . ?
B4 F42 1.357(8) . ?
B4 F41 1.402(7) . ?
B5 F52 1.306(8) . ?
B5 F53 1.333(8) . ?
B5 F51 1.343(8) . ?
B5 F54 1.364(8) . ?

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
O21 Cu1 N12 94.76(11) . . ?
O21 Cu1 N15 167.69(12) . . ?
N12 Cu1 N15 80.24(13) . . ?
O21 Cu1 N19 87.73(13) . . ?
N12 Cu1 N19 177.24(16) . . ?
N15 Cu1 N19 97.55(14) . . ?
O21 Cu1 F41 85.87(11) . . ?
N12 Cu1 F41 90.43(14) . . ?
N15 Cu1 F41 82.94(12) . . ?
N19 Cu1 F41 90.95(18) . . ?
O21 Cu1 O1W 85.89(12) . . ?
N12 Cu1 O1W 76.20(16) . . ?
N15 Cu1 O1W 103.63(13) . . ?
N19 Cu1 O1W 102.83(19) . . ?
F41 Cu1 O1W 163.63(18) . . ?
O11 Cu2 N25 165.16(13) . . ?
O11 Cu2 N22 93.60(11) . . ?
N25 Cu2 N22 80.34(13) . . ?
O11 Cu2 N29 88.46(14) . . ?
N25 Cu2 N29 97.87(16) . . ?
N22 Cu2 N29 177.76(15) . . ?
O11 Cu2 O1W 91.01(14) . . ?
N25 Cu2 O1W 100.54(15) . . ?
N22 Cu2 O1W 76.06(18) . . ?
N29 Cu2 O1W 103.05(19) . . ?
N12 O11 Cu2 115.5(2) . . ?
C13 N12 O11 118.2(3) . . ?
C13 N12 Cu1 114.3(2) . . ?
O11 N12 Cu1 126.6(2) . . ?
N12 C13 C14 113.7(3) . . ?
N12 C13 C131 122.4(4) . . ?
C14 C13 C131 123.9(4) . . ?
N15 C14 C13 116.6(3) . . ?
N15 C14 C141 125.0(4) . . ?
C13 C14 C141 118.3(4) . . ?
N15 C14 Cu1 41.73(19) . . ?
C13 C14 Cu1 75.04(19) . . ?
C141 C14 Cu1 166.6(4) . . ?
N15 C16 C17 109.5(4) . . ?
C18 C17 C16 124.8(8) . . ?
C17 C18 N19 119.0(7) . . ?
C14 N15 C16 119.9(4) . . ?
C14 N15 Cu1 113.3(3) . . ?
C16 N15 Cu1 126.7(3) . . ?
C20 N19 C21 109.1(6) . . ?
C20 N19 C18 104.0(6) . . ?
C21 N19 C18 112.0(6) . . ?
C20 N19 Cu1 111.1(4) . . ?
C21 N19 Cu1 106.7(4) . . ?
C18 N19 Cu1 113.9(3) . . ?
N22 O21 Cu1 117.41(19) . . ?
C23 N22 O21 118.5(3) . . ?
C23 N22 Cu2 113.7(2) . . ?
O21 N22 Cu2 127.2(2) . . ?
N22 C23 C24 113.6(4) . . ?
N22 C23 C231 123.3(4) . . ?
C24 C23 C231 123.0(4) . . ?
N25 C24 C23 116.4(3) . . ?
N25 C24 C241 124.8(4) . . ?
C23 C24 C241 118.7(4) . . ?
C24 N25 C26 119.7(4) . . ?
C24 N25 Cu2 113.3(3) . . ?
C26 N25 Cu2 126.7(4) . . ?
N25 C26 C27 111.2(5) . . ?
C28 C27 C26 113.4(6) . . ?
C27 C28 N29 115.5(5) . . ?
C31 N29 C30 108.3(6) . . ?
C31 N29 C28 104.0(4) . . ?
C30 N29 C28 114.0(5) . . ?
C31 N29 Cu2 111.4(3) . . ?
C30 N29 Cu2 105.2(4) . . ?
C28 N29 Cu2 113.9(4) . . ?
Cu2 O1W Cu1 82.44(13) . . ?
F43 B4 F44 111.2(6) . . ?
F43 B4 F42 112.2(5) . . ?
F44 B4 F42 115.8(6) . . ?
F43 B4 F41 107.7(5) . . ?
F44 B4 F41 104.7(5) . . ?
F42 B4 F41 104.5(5) . . ?
F52 B5 F53 115.3(6) . . ?
F52 B5 F51 111.6(7) . . ?
F53 B5 F51 113.8(6) . . ?
F52 B5 F54 105.5(7) . . ?
F53 B5 F54 108.4(6) . . ?
F51 B5 F54 100.8(7) . . ?
B4 F41 Cu1 141.8(3) . . ?

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
O1W H1W1 F51 0.97 1.92 2.791(7) 147.9 .
O1W H1W2 F52 0.97 2.02 2.712(7) 126.4 3_545

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        30.98
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.078
_database_code_depnum_ccdc_archive 'CCDC 973638'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H115 Cl9 Cu6 N18 O44'
_chemical_formula_weight         2420.93

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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   13.7881(15)
_cell_length_b                   13.8192(14)
_cell_length_c                   15.706(3)
_cell_angle_alpha                92.716(13)
_cell_angle_beta                 96.802(13)
_cell_angle_gamma                119.851(11)
_cell_volume                     2557.6(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    18227
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      30.00

_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1244
_exptl_absorpt_coefficient_mu    1.551
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_absorpt_correction_T_min  0.844
_exptl_absorpt_correction_T_max  1.000
_exptl_special_details           
;
 ?
;


_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_standards_number         n/a
_diffrn_measurement_device       'Oxford Diffaction X-Calibur System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_decay_%        n/a
_diffrn_reflns_number            18227
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.2797
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.63
_diffrn_reflns_theta_max         30.00
_reflns_number_total             14301
_reflns_number_gt                4005
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material  'SHELXL-97, PLATON'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

 distance constraints proved necessary for the atoms affected by high thermal
 motion and were applied to the NHMe2 groups based on N19, N29 and N39
 and in addition to the perchlorate groups based on cl10, cl11 and cl8 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0773P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14301
_refine_ls_number_parameters     570
_refine_ls_number_restraints     62
_refine_ls_R_factor_all          0.2169
_refine_ls_R_factor_gt           0.0932
_refine_ls_wR_factor_ref         0.2580
_refine_ls_wR_factor_gt          0.2182
_refine_ls_goodness_of_fit_ref   0.821
_refine_ls_restrained_S_all      0.836
_refine_ls_shift/su_max          0.000
_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 0.52417(8) 0.14903(8) 0.60985(7) 0.0436(3) Uani 1 1 d . . .
Cu2 Cu 0.67476(8) 0.03209(8) 0.60044(7) 0.0435(3) Uani 1 1 d . . .
Cu3 Cu 0.40653(8) -0.11935(8) 0.60399(7) 0.0457(3) Uani 1 1 d . . .
O11 O 0.3023(4) -0.0615(4) 0.5994(3) 0.0353(12) Uani 1 1 d . . .
N12 N 0.3587(5) 0.0497(5) 0.6050(4) 0.0427(17) Uani 1 1 d . . .
C13 C 0.3048(6) 0.1058(7) 0.6160(6) 0.048(2) Uani 1 1 d . . .
C14 C 0.3806(7) 0.2286(7) 0.6224(5) 0.045(2) Uani 1 1 d . . .
C131 C 0.1712(7) 0.0448(6) 0.6103(6) 0.057(3) Uani 1 1 d . . .
H13A H 0.1492 0.0019 0.6580 0.085 Uiso 1 1 calc R . .
H13B H 0.1351 -0.0045 0.5570 0.085 Uiso 1 1 calc R . .
H13C H 0.1485 0.1001 0.6124 0.085 Uiso 1 1 calc R . .
C141 C 0.3251(7) 0.3012(7) 0.6374(6) 0.056(2) Uani 1 1 d . . .
H14A H 0.3772 0.3674 0.6767 0.083 Uiso 1 1 calc R . .
H14B H 0.2572 0.2582 0.6614 0.083 Uiso 1 1 calc R . .
H14C H 0.3066 0.3227 0.5833 0.083 Uiso 1 1 calc R . .
N15 N 0.4863(6) 0.2696(5) 0.6270(5) 0.0468(18) Uani 1 1 d . . .
C16 C 0.5743(7) 0.3905(6) 0.6437(6) 0.045(2) Uani 1 1 d . . .
H16A H 0.6341 0.4032 0.6109 0.054 Uiso 1 1 calc R . .
H16B H 0.5408 0.4336 0.6219 0.054 Uiso 1 1 calc R . .
C17 C 0.6227(12) 0.4318(13) 0.7294(8) 0.118(6) Uani 1 1 d D . .
H17A H 0.5670 0.4385 0.7576 0.142 Uiso 1 1 calc R . .
H17B H 0.6857 0.5075 0.7303 0.142 Uiso 1 1 calc R . .
C18 C 0.6628(16) 0.3757(13) 0.7815(9) 0.190(10) Uani 1 1 d D . .
H18A H 0.7368 0.3925 0.7697 0.228 Uiso 1 1 calc R . .
H18B H 0.6115 0.2952 0.7688 0.228 Uiso 1 1 calc R . .
N19 N 0.6709(4) 0.4111(12) 0.8706(9) 0.199(7) Uani 1 1 d DU . .
H19 H 0.7386 0.4246 0.8821 0.239 Uiso 1 1 d D . .
C21 C 0.7051(11) 0.5239(10) 0.9074(8) 0.132(5) Uani 1 1 d DU . .
H21A H 0.7857 0.5712 0.9118 0.159 Uiso 1 1 calc R . .
H21B H 0.6844 0.5217 0.9638 0.159 Uiso 1 1 calc R . .
H21C H 0.6678 0.5535 0.8709 0.159 Uiso 1 1 calc R . .
C20 C 0.6361(12) 0.3205(10) 0.9271(8) 0.121(5) Uani 1 1 d DU . .
H20A H 0.6054 0.2494 0.8924 0.146 Uiso 1 1 calc R . .
H20B H 0.5795 0.3193 0.9579 0.146 Uiso 1 1 calc R . .
H20C H 0.7007 0.3340 0.9675 0.146 Uiso 1 1 calc R . .
O21 O 0.6128(4) -0.1301(4) 0.5919(4) 0.0504(15) Uani 1 1 d . . .
N22 N 0.5042(6) -0.1840(6) 0.5975(5) 0.0517(19) Uani 1 1 d . . .
C23 C 0.4517(6) -0.2963(6) 0.5974(5) 0.043(2) Uani 1 1 d . . .
C24 C 0.3285(7) -0.3462(7) 0.6045(6) 0.052(2) Uani 1 1 d . . .
N25 N 0.2946(5) -0.2731(5) 0.6140(4) 0.0432(17) Uani 1 1 d . . .
C231 C 0.5094(8) -0.3602(8) 0.5933(6) 0.063(3) Uani 1 1 d . . .
H23A H 0.4793 -0.4104 0.5403 0.094 Uiso 1 1 calc R . .
H23B H 0.4978 -0.4029 0.6414 0.094 Uiso 1 1 calc R . .
H23C H 0.5890 -0.3095 0.5954 0.094 Uiso 1 1 calc R . .
C241 C 0.2629(7) -0.4734(6) 0.6066(6) 0.058(3) Uani 1 1 d . . .
H24A H 0.2354 -0.4893 0.6606 0.087 Uiso 1 1 calc R . .
H24B H 0.3122 -0.5028 0.6006 0.087 Uiso 1 1 calc R . .
H24C H 0.2000 -0.5080 0.5599 0.087 Uiso 1 1 calc R . .
C26 C 0.1729(7) -0.3115(7) 0.6204(6) 0.059(3) Uani 1 1 d . . .
H26A H 0.1240 -0.3849 0.5872 0.070 Uiso 1 1 calc R . .
H26B H 0.1528 -0.2594 0.5961 0.070 Uiso 1 1 calc R . .
C27 C 0.1546(8) -0.3181(8) 0.7139(7) 0.069(3) Uani 1 1 d . . .
H27A H 0.0767 -0.3397 0.7175 0.082 Uiso 1 1 calc R . .
H27B H 0.1693 -0.3741 0.7374 0.082 Uiso 1 1 calc R . .
C28 C 0.2314(11) -0.2084(12) 0.7630(8) 0.110(5) Uani 1 1 d D . .
H28A H 0.2173 -0.1525 0.7386 0.132 Uiso 1 1 calc R . .
H28B H 0.3091 -0.1874 0.7594 0.132 Uiso 1 1 calc R . .
N29 N 0.2152(11) -0.2107(11) 0.8560(8) 0.130(4) Uani 1 1 d D . .
H29 H 0.2011 -0.2810 0.8641 0.156 Uiso 1 1 calc R . .
C30 C 0.1089(12) -0.2212(13) 0.8664(7) 0.217(10) Uani 1 1 d D . .
H30A H 0.1078 -0.2072 0.9266 0.260 Uiso 1 1 calc R . .
H30B H 0.0486 -0.2959 0.8439 0.260 Uiso 1 1 calc R . .
H30C H 0.0987 -0.1677 0.8356 0.260 Uiso 1 1 calc R . .
C31 C 0.3112(12) -0.1446(13) 0.9208(7) 0.199(10) Uani 1 1 d RD . .
H31A H 0.3295 -0.0677 0.9244 0.239 Uiso 1 1 calc R . .
H31B H 0.3744 -0.1497 0.9064 0.239 Uiso 1 1 calc R . .
H31C H 0.2947 -0.1718 0.9755 0.239 Uiso 1 1 calc R . .
O31 O 0.6815(4) 0.2481(4) 0.5993(4) 0.0541(16) Uani 1 1 d . . .
N32 N 0.7441(6) 0.1968(6) 0.6059(5) 0.056(2) Uani 1 1 d . . .
C33 C 0.8573(6) 0.2545(6) 0.6114(5) 0.041(2) Uani 1 1 d . . .
C34 C 0.9055(6) 0.1829(7) 0.6282(5) 0.043(2) Uani 1 1 d . . .
N35 N 0.8359(6) 0.0744(6) 0.6205(4) 0.0465(17) Uani 1 1 d . . .
C331 C 0.9221(8) 0.3811(7) 0.6218(7) 0.077(3) Uani 1 1 d . . .
H33A H 0.9706 0.4091 0.6770 0.116 Uiso 1 1 calc R . .
H33B H 0.8698 0.4080 0.6183 0.116 Uiso 1 1 calc R . .
H33C H 0.9672 0.4068 0.5767 0.116 Uiso 1 1 calc R . .
C341 C 1.0277(7) 0.2381(8) 0.6459(7) 0.073(3) Uani 1 1 d . . .
H34A H 1.0545 0.2756 0.7040 0.110 Uiso 1 1 calc R . .
H34B H 1.0593 0.2922 0.6062 0.110 Uiso 1 1 calc R . .
H34C H 1.0504 0.1832 0.6392 0.110 Uiso 1 1 calc R . .
C36 C 0.8784(8) -0.0042(8) 0.6274(7) 0.064(3) Uani 1 1 d . . .
H36A H 0.8227 -0.0758 0.5941 0.077 Uiso 1 1 calc R . .
H36B H 0.9474 0.0250 0.6024 0.077 Uiso 1 1 calc R . .
C37 C 0.9021(8) -0.0225(8) 0.7167(7) 0.068(3) Uani 1 1 d . . .
H37A H 0.9530 0.0497 0.7510 0.082 Uiso 1 1 calc R . .
H37B H 0.9405 -0.0653 0.7179 0.082 Uiso 1 1 calc R . .
C38 C 0.7947(9) -0.0853(9) 0.7580(8) 0.085(4) Uani 1 1 d D . .
H38A H 0.7479 -0.0522 0.7443 0.101 Uiso 1 1 calc R . .
H38B H 0.7523 -0.1627 0.7312 0.101 Uiso 1 1 calc R . .
N39 N 0.8123(8) -0.0853(8) 0.8513(6) 0.087(3) Uani 1 1 d D . .
H39 H 0.8374 -0.0124 0.8709 0.105 Uiso 1 1 calc R . .
C40 C 0.9082(19) -0.100(2) 0.8916(12) 0.276(16) Uani 1 1 d D . .
H40A H 0.8891 -0.1766 0.8778 0.331 Uiso 1 1 calc R . .
H40B H 0.9206 -0.0824 0.9532 0.331 Uiso 1 1 calc R . .
H40C H 0.9759 -0.0508 0.8696 0.331 Uiso 1 1 calc R . .
C41 C 0.6983(11) -0.1438(14) 0.8755(10) 0.152(7) Uani 1 1 d D . .
H41A H 0.6751 -0.2212 0.8794 0.183 Uiso 1 1 calc R . .
H41B H 0.6456 -0.1392 0.8325 0.183 Uiso 1 1 calc R . .
H41C H 0.7000 -0.1089 0.9305 0.183 Uiso 1 1 calc R . .
O1 O 0.5282(4) 0.0156(4) 0.5802(3) 0.0412(13) Uani 1 1 d . . .
H1W H 0.5000 0.0000 0.5000 0.049 Uiso 1 2 d S . .
Cl6 Cl 0.7396(4) 0.8503(4) 0.1399(3) 0.1175(17) Uani 0.75 1 d P . .
O61 O 0.8146(12) 0.9321(12) 0.0932(9) 0.140(5) Uiso 0.75 1 d P . .
O62 O 0.8075(10) 0.8098(10) 0.1841(8) 0.120(4) Uiso 0.75 1 d P . .
O63 O 0.6883(12) 0.8962(12) 0.1950(10) 0.154(5) Uiso 0.75 1 d P . .
O64 O 0.6375(14) 0.7391(14) 0.0801(11) 0.176(6) Uiso 0.75 1 d P . .
Cl7 Cl 0.5813(3) 0.0505(2) 0.7979(2) 0.0866(9) Uani 1 1 d . . .
O71 O 0.5559(8) 0.1290(7) 0.7646(5) 0.106(3) Uani 1 1 d . . .
O72 O 0.6894(7) 0.0724(7) 0.7659(6) 0.119(3) Uani 1 1 d . . .
O73 O 0.4972(6) -0.0604(6) 0.7626(5) 0.084(2) Uani 1 1 d . . .
O74 O 0.5924(7) 0.0623(7) 0.8917(5) 0.102(3) Uani 1 1 d . . .
Cl8 Cl 0.4065(3) 0.5773(3) 0.8498(2) 0.0742(10) Uiso 0.75 1 d PD . .
O81 O 0.4697(8) 0.5830(9) 0.7786(6) 0.105(4) Uiso 0.75 1 d PD . .
O82 O 0.4611(9) 0.5704(9) 0.9234(6) 0.120(4) Uiso 0.75 1 d PD . .
O83 O 0.2911(9) 0.4873(10) 0.8250(8) 0.154(5) Uiso 0.75 1 d PD . .
O84 O 0.3970(13) 0.6786(11) 0.8496(11) 0.208(7) Uiso 0.75 1 d PD . .
Cl9 Cl 0.8725(2) 0.6923(2) 0.6077(2) 0.0680(7) Uani 1 1 d . . .
O91 O 0.9141(8) 0.6257(8) 0.5711(7) 0.152(4) Uani 1 1 d . . .
O92 O 0.7569(9) 0.6457(10) 0.5746(8) 0.163(4) Uani 1 1 d . . .
O93 O 0.9212(11) 0.7914(9) 0.5739(9) 0.189(6) Uani 1 1 d . . .
O94 O 0.8986(13) 0.7183(12) 0.6972(8) 0.203(6) Uani 1 1 d . . .
Cl10 Cl 0.9593(4) 0.4340(4) 0.8701(3) 0.0717(15) Uani 0.50 1 d PD . .
O102 O 1.0830(11) 0.5019(17) 0.8734(14) 0.182(10) Uiso 0.50 1 d PD . .
O103 O 0.9087(19) 0.3256(13) 0.8229(13) 0.172(10) Uiso 0.50 1 d PD . .
O104 O 0.9100(16) 0.5006(15) 0.8367(13) 0.159(8) Uiso 0.50 1 d PD . .
O101 O 0.942(2) 0.419(2) 0.9604(10) 0.242(14) Uiso 0.50 1 d PD . .
Cl11 Cl 0.9738(5) 0.2579(6) 0.9044(4) 0.103(2) Uani 0.50 1 d PD . .
O111 O 1.1039(10) 0.2987(13) 0.9096(11) 0.115(6) Uiso 0.50 1 d PD . .
O112 O 0.9152(9) 0.1434(9) 0.9131(8) 0.064(3) Uiso 0.50 1 d PD . .
O113 O 0.944(2) 0.290(3) 0.8233(16) 0.34(3) Uiso 0.50 1 d PD . .
O114 O 0.971(2) 0.330(2) 0.9744(19) 0.37(3) Uiso 0.50 1 d PD . .


_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 O1 1.909(5) . ?
Cu1 O31 1.938(5) . ?
Cu1 N12 1.982(6) . ?
Cu1 N15 1.994(7) . ?
Cu2 O1 1.902(5) . ?
Cu2 O21 1.952(5) . ?
Cu2 N32 1.974(7) . ?
Cu2 N35 1.975(7) . ?
Cu3 O1 1.879(5) . ?
Cu3 N25 1.936(6) . ?
Cu3 O11 1.958(5) . ?
Cu3 N22 1.960(7) . ?
O11 N12 1.324(7) . ?
N12 C13 1.332(10) . ?
C13 C14 1.475(10) . ?
C13 C131 1.587(10) . ?
C14 N15 1.265(9) . ?
C14 C141 1.560(11) . ?
N15 C16 1.483(9) . ?
C16 C17 1.386(14) . ?
C17 C18 1.398(15) . ?
C18 N19 1.432(13) . ?
N19 C21 1.450(13) . ?
N19 C20 1.482(13) . ?
O21 N22 1.317(8) . ?
N22 C23 1.346(9) . ?
C23 C231 1.458(11) . ?
C23 C24 1.504(11) . ?
C24 N25 1.315(10) . ?
C24 C241 1.530(11) . ?
N25 C26 1.505(10) . ?
C26 C27 1.519(12) . ?
C27 C28 1.453(15) . ?
C28 N29 1.503(12) . ?
N29 C31 1.419(12) . ?
N29 C30 1.429(12) . ?
O31 N32 1.362(8) . ?
N32 C33 1.342(9) . ?
C33 C34 1.458(11) . ?
C33 C331 1.506(11) . ?
C34 N35 1.307(9) . ?
C34 C341 1.445(11) . ?
N35 C36 1.471(11) . ?
C36 C37 1.465(13) . ?
C37 C38 1.539(13) . ?
C38 N39 1.457(11) . ?
N39 C41 1.475(12) . ?
N39 C40 1.508(14) . ?
Cl6 O61 1.408(14) . ?
Cl6 O62 1.441(13) . ?
Cl6 O63 1.480(15) . ?
Cl6 O64 1.619(16) . ?
Cl7 O71 1.401(8) . ?
Cl7 O73 1.414(7) . ?
Cl7 O74 1.456(8) . ?
Cl7 O72 1.519(9) . ?
Cl8 O82 1.338(9) . ?
Cl8 O83 1.438(10) . ?
Cl8 O84 1.469(11) . ?
Cl8 O81 1.480(9) . ?
Cl9 O93 1.359(11) . ?
Cl9 O94 1.392(12) . ?
Cl9 O92 1.405(11) . ?
Cl9 O91 1.434(9) . ?
Cl10 O103 1.419(13) . ?
Cl10 O101 1.472(13) . ?
Cl10 O104 1.473(13) . ?
Cl10 O102 1.474(13) . ?
Cl10 O113 1.99(3) . ?
O103 O113 0.84(4) . ?
O103 Cl11 2.00(2) . ?
O101 O114 1.48(4) . ?
Cl11 O112 1.396(11) . ?
Cl11 O113 1.449(14) . ?
Cl11 O114 1.462(15) . ?
Cl11 O111 1.580(12) . ?

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
O1 Cu1 O31 93.7(2) . . ?
O1 Cu1 N12 86.6(2) . . ?
O31 Cu1 N12 172.7(3) . . ?
O1 Cu1 N15 167.8(2) . . ?
O31 Cu1 N15 96.3(3) . . ?
N12 Cu1 N15 82.6(3) . . ?
O1 Cu2 O21 92.7(2) . . ?
O1 Cu2 N32 89.8(3) . . ?
O21 Cu2 N32 176.9(3) . . ?
O1 Cu2 N35 171.1(2) . . ?
O21 Cu2 N35 96.2(3) . . ?
N32 Cu2 N35 81.3(3) . . ?
O1 Cu3 N25 167.7(3) . . ?
O1 Cu3 O11 94.0(2) . . ?
N25 Cu3 O11 96.0(2) . . ?
O1 Cu3 N22 86.9(3) . . ?
N25 Cu3 N22 82.5(3) . . ?
O11 Cu3 N22 174.6(3) . . ?
N12 O11 Cu3 110.7(4) . . ?
O11 N12 C13 119.6(6) . . ?
O11 N12 Cu1 126.8(5) . . ?
C13 N12 Cu1 113.3(5) . . ?
N12 C13 C14 112.4(7) . . ?
N12 C13 C131 122.6(7) . . ?
C14 C13 C131 124.5(7) . . ?
N15 C14 C13 119.9(7) . . ?
N15 C14 C141 123.4(7) . . ?
C13 C14 C141 116.0(7) . . ?
C14 N15 C16 126.3(7) . . ?
C14 N15 Cu1 111.2(5) . . ?
C16 N15 Cu1 122.4(5) . . ?
C17 C16 N15 115.6(9) . . ?
C16 C17 C18 121.2(14) . . ?
C17 C18 N19 109.4(13) . . ?
C18 N19 C21 126.0(12) . . ?
C18 N19 C20 114.8(12) . . ?
C21 N19 C20 119.2(12) . . ?
N22 O21 Cu2 111.4(5) . . ?
O21 N22 C23 117.8(7) . . ?
O21 N22 Cu3 127.2(5) . . ?
C23 N22 Cu3 115.0(6) . . ?
N22 C23 C231 123.5(8) . . ?
N22 C23 C24 111.9(7) . . ?
C231 C23 C24 124.6(7) . . ?
N25 C24 C23 115.2(7) . . ?
N25 C24 C241 129.3(8) . . ?
C23 C24 C241 115.3(8) . . ?
C24 N25 C26 120.9(7) . . ?
C24 N25 Cu3 115.0(6) . . ?
C26 N25 Cu3 123.7(5) . . ?
N25 C26 C27 110.8(7) . . ?
C28 C27 C26 108.6(8) . . ?
C27 C28 N29 110.3(11) . . ?
C31 N29 C30 119.4(10) . . ?
C31 N29 C28 118.6(11) . . ?
C30 N29 C28 111.9(10) . . ?
N32 O31 Cu1 113.2(5) . . ?
C33 N32 O31 122.1(7) . . ?
C33 N32 Cu2 115.2(6) . . ?
O31 N32 Cu2 122.6(5) . . ?
N32 C33 C34 111.4(7) . . ?
N32 C33 C331 120.9(8) . . ?
C34 C33 C331 125.9(7) . . ?
N35 C34 C341 125.3(8) . . ?
N35 C34 C33 117.9(7) . . ?
C341 C34 C33 116.6(7) . . ?
C34 N35 C36 121.2(7) . . ?
C34 N35 Cu2 113.1(6) . . ?
C36 N35 Cu2 125.7(6) . . ?
C37 C36 N35 112.9(8) . . ?
C36 C37 C38 113.2(8) . . ?
N39 C38 C37 116.3(9) . . ?
C38 N39 C41 106.0(10) . . ?
C38 N39 C40 118.3(11) . . ?
C41 N39 C40 123.1(12) . . ?
Cu3 O1 Cu2 117.2(3) . . ?
Cu3 O1 Cu1 116.1(3) . . ?
Cu2 O1 Cu1 115.0(2) . . ?
O61 Cl6 O62 103.5(8) . . ?
O61 Cl6 O63 111.7(9) . . ?
O62 Cl6 O63 116.3(9) . . ?
O61 Cl6 O64 114.1(9) . . ?
O62 Cl6 O64 103.4(9) . . ?
O63 Cl6 O64 107.8(9) . . ?
O71 Cl7 O73 111.1(5) . . ?
O71 Cl7 O74 110.1(5) . . ?
O73 Cl7 O74 110.2(5) . . ?
O71 Cl7 O72 105.7(6) . . ?
O73 Cl7 O72 106.3(5) . . ?
O74 Cl7 O72 113.4(5) . . ?
O82 Cl8 O83 115.2(7) . . ?
O82 Cl8 O84 114.8(8) . . ?
O83 Cl8 O84 103.3(8) . . ?
O82 Cl8 O81 109.5(6) . . ?
O83 Cl8 O81 108.8(7) . . ?
O84 Cl8 O81 104.6(7) . . ?
O93 Cl9 O94 106.8(8) . . ?
O93 Cl9 O92 102.6(8) . . ?
O94 Cl9 O92 114.0(8) . . ?
O93 Cl9 O91 106.6(8) . . ?
O94 Cl9 O91 115.9(7) . . ?
O92 Cl9 O91 109.8(6) . . ?
O103 Cl10 O101 107.5(11) . . ?
O103 Cl10 O104 112.8(11) . . ?
O101 Cl10 O104 109.2(12) . . ?
O103 Cl10 O102 113.9(12) . . ?
O101 Cl10 O102 105.5(11) . . ?
O104 Cl10 O102 107.6(10) . . ?
O112 Cl11 O113 116.5(13) . . ?
O112 Cl11 O114 114.1(13) . . ?
O113 Cl11 O114 107.8(13) . . ?
O112 Cl11 O111 108.7(8) . . ?
O113 Cl11 O111 104.4(12) . . ?
O114 Cl11 O111 104.1(12) . . ?


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
N19 H19 O104 0.8503(10) 2.28(2) 3.02(2) 145.1(11) .
N29 H29 O102 0.91 2.63 3.49(2) 158.5 1_445
N39 H39 O112 0.91 1.90 2.804(15) 170.1 .
O1 H1W O1 1.249(5) 1.249(5) 2.498(10) 180.000(2) 2_656

_diffrn_measured_fraction_theta_max 0.958
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.958
_refine_diff_density_max         1.169
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.129
_database_code_depnum_ccdc_archive 'CCDC 973639'
