Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2006

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Rita Delgado'
_publ_contact_author_address     
;
Chemistry Division
ITQB
Av. da Republica
Apartado 127
Oeiras
2781-901
PORTUGAL
;

_publ_contact_author_email       DELGADO@ITQB.UNL.PT

_publ_section_title              
;
Bis- and tris-(3-aminopropyl) derivatives of
14-membered tetraazamacrocycles containing pyridine: synthesis, protonation
and complexation studies
;
loop_
_publ_author_name
'Rita Delgado'
'Michael G.B.Drew'
'Vitor Felix'
'Krassimira P.Guerra'

data_compound1
_database_code_depnum_ccdc_archive 'CCDC 600821'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H60 Cl6 Co3 N12'
_chemical_formula_weight         1098.49

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'
Co Co 0.3494 0.9721 '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           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_int_tables_number      15

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

_cell_length_a                   30.071(33)
_cell_length_b                   10.042(12)
_cell_length_c                   16.331(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.39(1)
_cell_angle_gamma                90.00
_cell_volume                     4891(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       parallelopiped
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.20

_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2268
_exptl_absorpt_coefficient_mu    1.377
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  1.00

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Marresearch Image Plate'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4515
_diffrn_reflns_av_R_equivalents  0.0944
_diffrn_reflns_av_sigmaI/netI    0.1170
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         26.03
_reflns_number_total             3116
_reflns_number_gt                1663
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'XDS (Kabsch, 1991)'
_computing_cell_refinement       XDS
_computing_data_reduction        XDS
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    PLATON(Spek,2003)
_computing_publication_material  ?
_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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      
'calc w=1/[\s^2^(Fo^2^)+(0.1524P)^2^+0.0000P] 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         3116
_refine_ls_number_parameters     277
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1728
_refine_ls_R_factor_gt           0.0800
_refine_ls_wR_factor_ref         0.2496
_refine_ls_wR_factor_gt          0.2100
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_restrained_S_all      0.994
_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.34948(4) 0.17328(16) -0.08836(8) 0.0427(5) Uani 1 d . . .
N1 N 0.3798(3) 0.2996(9) 0.0119(5) 0.043(2) Uani 1 d . . .
C2 C 0.3877(3) 0.4339(11) -0.0237(6) 0.049(3) Uani 1 d . . .
H2A H 0.3588 0.4745 -0.0413 0.059 Uiso 1 calc R . .
H2B H 0.4029 0.4890 0.0199 0.059 Uiso 1 calc R . .
C3 C 0.4138(4) 0.4367(13) -0.0937(7) 0.064(3) Uani 1 d . . .
H3A H 0.4423 0.3933 -0.0763 0.077 Uiso 1 calc R . .
H3B H 0.4203 0.5291 -0.1049 0.077 Uiso 1 calc R . .
C4 C 0.3932(4) 0.3721(14) -0.1756(7) 0.057(3) Uani 1 d . . .
H4A H 0.3636 0.4099 -0.1904 0.069 Uiso 1 calc R . .
H4B H 0.4113 0.3983 -0.2180 0.069 Uiso 1 calc R . .
N5 N 0.3889(3) 0.2263(10) -0.1781(5) 0.047(2) Uani 1 d . . .
C6 C 0.3636(4) 0.1927(15) -0.2600(6) 0.069(4) Uani 1 d . . .
H6A H 0.3813 0.2208 -0.3026 0.083 Uiso 1 calc R . .
H6B H 0.3360 0.2438 -0.2670 0.083 Uiso 1 calc R . .
C7 C 0.3519(4) 0.0470(15) -0.2735(6) 0.066(4) Uani 1 d . . .
H7A H 0.3786 -0.0050 -0.2560 0.079 Uiso 1 calc R . .
H7B H 0.3442 0.0327 -0.3324 0.079 Uiso 1 calc R . .
C8 C 0.3136(4) -0.0093(13) -0.2299(6) 0.055(3) Uani 1 d . . .
H8A H 0.2876 0.0480 -0.2419 0.066 Uiso 1 calc R . .
H8B H 0.3055 -0.0965 -0.2526 0.066 Uiso 1 calc R . .
N9 N 0.3247(2) -0.0216(10) -0.1373(5) 0.049(3) Uani 1 d . . .
C10 C 0.3593(3) -0.1268(12) -0.1127(7) 0.052(3) Uani 1 d . . .
H10A H 0.3768 -0.1418 -0.1578 0.063 Uiso 1 calc R . .
H10B H 0.3444 -0.2096 -0.1022 0.063 Uiso 1 calc R . .
C11 C 0.3902(3) -0.0871(13) -0.0366(6) 0.040(3) Uani 1 d . . .
C12 C 0.4165(4) -0.1745(14) 0.0120(7) 0.061(4) Uani 1 d . . .
H12 H 0.4144 -0.2651 0.0002 0.074 Uiso 1 calc R . .
C13 C 0.4457(3) -0.1314(14) 0.0777(7) 0.051(3) Uani 1 d . . .
H13 H 0.4628 -0.1918 0.1115 0.062 Uiso 1 calc R . .
C14 C 0.4491(3) 0.0022(14) 0.0926(6) 0.053(3) Uani 1 d . . .
H14 H 0.4703 0.0343 0.1345 0.063 Uiso 1 calc R . .
C15 C 0.4205(3) 0.0914(12) 0.0442(6) 0.039(3) Uani 1 d . . .
C16 C 0.4224(3) 0.2369(12) 0.0514(7) 0.048(3) Uani 1 d . . .
H16A H 0.4473 0.2702 0.0251 0.058 Uiso 1 calc R . .
H16B H 0.4275 0.2615 0.1093 0.058 Uiso 1 calc R . .
N17 N 0.3918(3) 0.0426(11) -0.0199(4) 0.041(2) Uani 1 d . . .
C51 C 0.4346(3) 0.1662(13) -0.1716(7) 0.063(4) Uani 1 d . . .
H51A H 0.4516 0.2097 -0.2097 0.076 Uiso 1 calc R . .
H51B H 0.4321 0.0730 -0.1846 0.076 Uiso 1 calc R . .
H51C H 0.4494 0.1772 -0.1164 0.076 Uiso 1 calc R . .
C103 C 0.3278(4) 0.3903(13) 0.2042(7) 0.056(3) Uani 1 d . . .
C101 C 0.3464(3) 0.3063(12) 0.0718(6) 0.048(3) Uani 1 d . . .
H10E H 0.3430 0.2182 0.0947 0.058 Uiso 1 calc R . .
H10F H 0.3175 0.3322 0.0425 0.058 Uiso 1 calc R . .
C104 C 0.3592(4) 0.4045(13) 0.1430(7) 0.061(3) Uani 1 d . . .
H10C H 0.3895 0.3865 0.1687 0.073 Uiso 1 calc R . .
H10D H 0.3582 0.4949 0.1219 0.073 Uiso 1 calc R . .
N104 N 0.3040(4) 0.3824(11) 0.2531(6) 0.067(3) Uani 1 d . . .
C501 C 0.2841(3) -0.0477(11) -0.1007(6) 0.044(3) Uani 1 d . . .
H50A H 0.2650 0.0302 -0.1092 0.053 Uiso 1 calc R . .
H50B H 0.2922 -0.0581 -0.0417 0.053 Uiso 1 calc R . .
C502 C 0.2566(3) -0.1684(13) -0.1324(7) 0.068(4) Uani 1 d . . .
H50C H 0.2453 -0.1564 -0.1903 0.081 Uiso 1 calc R . .
H50D H 0.2753 -0.2474 -0.1272 0.081 Uiso 1 calc R . .
C503 C 0.2185(4) -0.1855(13) -0.0839(8) 0.063(4) Uani 1 d . . .
N504 N 0.1901(3) -0.2005(13) -0.0469(7) 0.081(4) Uani 1 d . . .
Co2 Co 0.5000 0.3974(2) 0.2500 0.0454(7) Uani 1 d S . .
Cl1 Cl 0.28574(9) 0.2919(4) -0.12370(17) 0.0635(10) Uani 1 d . . .
Cl2 Cl 0.47060(10) 0.5376(3) 0.14742(17) 0.0648(10) Uani 1 d . . .
Cl3 Cl 0.55166(10) 0.2529(4) 0.20925(19) 0.0697(10) Uani 1 d . . .

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
Co1 0.0426(8) 0.0467(13) 0.0388(8) 0.0019(7) 0.0049(6) 0.0050(7)
N1 0.047(5) 0.028(7) 0.053(5) 0.009(4) 0.007(4) 0.005(4)
C2 0.060(7) 0.027(9) 0.060(7) -0.007(6) 0.009(5) 0.006(6)
C3 0.083(8) 0.043(10) 0.069(8) -0.007(7) 0.022(7) -0.001(7)
C4 0.065(8) 0.055(12) 0.057(7) 0.020(6) 0.032(6) 0.000(6)
N5 0.052(5) 0.032(8) 0.056(6) 0.009(4) 0.008(4) 0.011(4)
C6 0.071(8) 0.111(14) 0.026(6) 0.004(6) 0.006(5) 0.001(8)
C7 0.065(8) 0.103(13) 0.030(6) -0.010(7) 0.003(5) -0.008(7)
C8 0.068(7) 0.054(10) 0.043(6) 0.004(6) 0.006(5) 0.002(6)
N9 0.036(5) 0.067(8) 0.046(5) -0.001(5) 0.013(4) -0.013(4)
C10 0.039(6) 0.053(10) 0.063(7) -0.001(6) 0.000(5) 0.006(6)
C11 0.039(6) 0.031(10) 0.050(6) -0.003(6) 0.012(4) 0.002(5)
C12 0.058(7) 0.065(11) 0.060(7) 0.013(7) 0.006(6) -0.002(7)
C13 0.045(6) 0.034(10) 0.069(8) 0.010(6) -0.014(5) 0.011(6)
C14 0.052(6) 0.050(11) 0.052(7) 0.014(6) -0.010(5) 0.003(6)
C15 0.043(6) 0.039(10) 0.037(6) -0.008(5) 0.010(4) 0.006(5)
C16 0.044(6) 0.034(10) 0.063(7) 0.003(6) -0.011(5) -0.003(6)
N17 0.043(5) 0.039(8) 0.039(5) 0.004(4) 0.000(4) -0.003(4)
C51 0.050(7) 0.078(12) 0.060(7) 0.004(7) 0.005(5) -0.005(6)
C103 0.068(8) 0.051(10) 0.048(7) -0.005(6) 0.000(6) 0.001(6)
C101 0.043(6) 0.060(9) 0.042(6) -0.004(5) 0.011(4) 0.006(6)
C104 0.065(8) 0.056(10) 0.064(8) -0.001(7) 0.013(6) -0.003(7)
N104 0.084(7) 0.059(9) 0.059(7) -0.019(6) 0.008(6) -0.018(6)
C501 0.048(6) 0.034(9) 0.049(6) -0.008(5) 0.004(5) -0.002(5)
C502 0.041(6) 0.092(13) 0.070(8) -0.029(7) 0.006(5) -0.013(7)
C503 0.077(9) 0.045(10) 0.066(8) -0.008(6) -0.001(7) -0.018(7)
N504 0.056(7) 0.110(12) 0.081(8) 0.019(7) 0.024(6) -0.011(6)
Co2 0.0451(11) 0.0434(18) 0.0475(12) 0.000 0.0047(8) 0.000
Cl1 0.0536(17) 0.072(3) 0.0625(18) 0.0050(15) 0.0005(13) 0.0147(15)
Cl2 0.0672(19) 0.057(3) 0.0667(18) 0.0159(16) -0.0041(14) -0.0035(16)
Cl3 0.0675(19) 0.073(3) 0.073(2) -0.0031(17) 0.0249(15) 0.0166(17)

_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
Co1 N17 2.056(9) . ?
Co1 N5 2.068(9) . ?
Co1 N1 2.176(9) . ?
Co1 N9 2.207(10) . ?
Co1 Cl1 2.268(4) . ?
N1 C101 1.490(12) . ?
N1 C16 1.499(12) . ?
N1 C2 1.501(14) . ?
C2 C3 1.468(14) . ?
C3 C4 1.542(15) . ?
C4 N5 1.471(15) . ?
N5 C6 1.489(13) . ?
N5 C51 1.493(13) . ?
C6 C7 1.515(18) . ?
C7 C8 1.538(15) . ?
C8 N9 1.511(12) . ?
N9 C501 1.452(12) . ?
N9 C10 1.500(14) . ?
C10 C11 1.507(14) . ?
C11 N17 1.331(14) . ?
C11 C12 1.365(15) . ?
C12 C13 1.367(15) . ?
C13 C14 1.365(16) . ?
C14 C15 1.411(14) . ?
C15 N17 1.359(12) . ?
C15 C16 1.466(15) . ?
C103 N104 1.139(14) . ?
C103 C104 1.470(16) . ?
C101 C104 1.536(15) . ?
C501 C502 1.520(15) . ?
C502 C503 1.484(16) . ?
C503 N504 1.118(14) . ?
Co2 Cl2 2.278(4) 6_656 ?
Co2 Cl2 2.278(4) . ?
Co2 Cl3 2.287(4) 6_656 ?
Co2 Cl3 2.287(4) . ?

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
N17 Co1 N5 100.3(3) . . ?
N17 Co1 N1 78.0(4) . . ?
N5 Co1 N1 99.3(3) . . ?
N17 Co1 N9 77.7(4) . . ?
N5 Co1 N9 99.7(4) . . ?
N1 Co1 N9 151.4(3) . . ?
N17 Co1 Cl1 156.6(2) . . ?
N5 Co1 Cl1 103.1(3) . . ?
N1 Co1 Cl1 98.2(2) . . ?
N9 Co1 Cl1 98.0(2) . . ?
C101 N1 C16 110.4(8) . . ?
C101 N1 C2 111.6(8) . . ?
C16 N1 C2 112.0(8) . . ?
C101 N1 Co1 105.6(6) . . ?
C16 N1 Co1 109.3(6) . . ?
C2 N1 Co1 107.7(6) . . ?
C3 C2 N1 116.6(9) . . ?
C2 C3 C4 118.1(10) . . ?
N5 C4 C3 117.9(9) . . ?
C4 N5 C6 106.5(9) . . ?
C4 N5 C51 108.8(9) . . ?
C6 N5 C51 109.3(9) . . ?
C4 N5 Co1 107.1(6) . . ?
C6 N5 Co1 107.8(7) . . ?
C51 N5 Co1 116.9(7) . . ?
N5 C6 C7 115.6(10) . . ?
C6 C7 C8 117.4(11) . . ?
N9 C8 C7 114.2(8) . . ?
C501 N9 C10 110.7(9) . . ?
C501 N9 C8 109.6(7) . . ?
C10 N9 C8 112.5(8) . . ?
C501 N9 Co1 105.9(6) . . ?
C10 N9 Co1 109.7(6) . . ?
C8 N9 Co1 108.1(7) . . ?
N9 C10 C11 111.5(10) . . ?
N17 C11 C12 120.5(10) . . ?
N17 C11 C10 115.5(9) . . ?
C12 C11 C10 124.0(12) . . ?
C11 C12 C13 121.2(13) . . ?
C14 C13 C12 118.6(10) . . ?
C13 C14 C15 119.8(10) . . ?
N17 C15 C14 118.9(11) . . ?
N17 C15 C16 115.8(9) . . ?
C14 C15 C16 125.0(10) . . ?
C15 C16 N1 111.2(8) . . ?
C11 N17 C15 120.9(9) . . ?
C11 N17 Co1 120.6(6) . . ?
C15 N17 Co1 118.5(8) . . ?
N104 C103 C104 177.9(12) . . ?
N1 C101 C104 113.6(9) . . ?
C103 C104 C101 109.3(9) . . ?
N9 C501 C502 117.0(9) . . ?
C503 C502 C501 109.5(9) . . ?
N504 C503 C502 178.8(15) . . ?
Cl2 Co2 Cl2 103.7(2) 6_656 . ?
Cl2 Co2 Cl3 113.09(13) 6_656 6_656 ?
Cl2 Co2 Cl3 113.11(13) . 6_656 ?
Cl2 Co2 Cl3 113.11(13) 6_656 . ?
Cl2 Co2 Cl3 113.09(13) . . ?
Cl3 Co2 Cl3 101.2(2) 6_656 . ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        26.03
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.136

_publ_section_references         
;

Sheldrick, G.M. (1997) SHELXL97 program for crystallography refinement.
University of Gottingen, Germany.

Spek, A.L., (1994) PLATON program, Utrecht University, The Netherlands
;

#===END

data_compound2
_database_code_depnum_ccdc_archive 'CCDC 600822'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H50 Cl4 Cu N7 O17.50'
_chemical_formula_weight         910.04

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           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_int_tables_number      14

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

_cell_length_a                   12.613(14)
_cell_length_b                   24.302(27)
_cell_length_c                   13.488(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.390(10)
_cell_angle_gamma                90.00
_cell_volume                     4100(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       parallelopiped
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1896
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_T_max  1.00

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Marresearch Image Plate'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21692
_diffrn_reflns_av_R_equivalents  0.1028
_diffrn_reflns_av_sigmaI/netI    0.2398
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.74
_diffrn_reflns_theta_max         25.89
_reflns_number_total             7147
_reflns_number_gt                3296
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'XDS (Kabsch, 1991)'
_computing_cell_refinement       XDS
_computing_data_reduction        XDS
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    PLATON(Spek,2003)
_computing_publication_material  ?

_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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      
'calc w=1/[\s^2^(Fo^2^)+(0.0829P)^2^+0.0000P] 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         7147
_refine_ls_number_parameters     511
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1804
_refine_ls_R_factor_gt           0.0951
_refine_ls_wR_factor_ref         0.2057
_refine_ls_wR_factor_gt          0.1826
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_restrained_S_all      0.948
_refine_ls_shift/su_max          0.064
_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.28952(8) 0.19541(4) 0.32220(7) 0.0347(3) Uani 1 d . . .
N1 N 0.2161(5) 0.1847(2) 0.4516(4) 0.0266(15) Uani 1 d . . .
C2 C 0.1033(7) 0.1638(3) 0.4399(6) 0.046(2) Uani 1 d . . .
H2A H 0.0548 0.1932 0.4156 0.055 Uiso 1 calc R . .
H2B H 0.0853 0.1520 0.5043 0.055 Uiso 1 calc R . .
C3 C 0.0901(6) 0.1161(3) 0.3672(6) 0.042(2) Uani 1 d . . .
H3A H 0.1399 0.0876 0.3932 0.051 Uiso 1 calc R . .
H3B H 0.0187 0.1014 0.3678 0.051 Uiso 1 calc R . .
C4 C 0.1055(6) 0.1258(3) 0.2611(5) 0.032(2) Uani 1 d . . .
H4A H 0.0677 0.1592 0.2388 0.038 Uiso 1 calc R . .
H4B H 0.0721 0.0957 0.2213 0.038 Uiso 1 calc R . .
N5 N 0.2208(5) 0.1310(2) 0.2388(5) 0.0327(17) Uani 1 d . . .
C6 C 0.2143(7) 0.1490(3) 0.1354(6) 0.044(2) Uani 1 d . . .
H6A H 0.1737 0.1830 0.1289 0.052 Uiso 1 calc R . .
H6B H 0.1735 0.1217 0.0940 0.052 Uiso 1 calc R . .
C7 C 0.3211(8) 0.1589(4) 0.0916(7) 0.057(3) Uani 1 d . . .
H7A H 0.3685 0.1280 0.1098 0.069 Uiso 1 calc R . .
H7B H 0.3062 0.1596 0.0192 0.069 Uiso 1 calc R . .
C8 C 0.3781(7) 0.2112(3) 0.1263(5) 0.036(2) Uani 1 d . . .
H8A H 0.4403 0.2158 0.0917 0.043 Uiso 1 calc R . .
H8B H 0.3309 0.2423 0.1095 0.043 Uiso 1 calc R . .
N9 N 0.4121(5) 0.2107(2) 0.2354(4) 0.0258(15) Uani 1 d . . .
C10 C 0.4556(6) 0.2674(3) 0.2654(6) 0.034(2) Uani 1 d . . .
H10J H 0.5325 0.2673 0.2651 0.041 Uiso 1 calc R . .
H10L H 0.4255 0.2939 0.2158 0.041 Uiso 1 calc R . .
C11 C 0.4326(6) 0.2851(3) 0.3630(6) 0.0240(18) Uani 1 d . . .
C12 C 0.4763(7) 0.3291(3) 0.4193(7) 0.042(2) Uani 1 d . . .
H12 H 0.5322 0.3495 0.3991 0.050 Uiso 1 calc R . .
C13 C 0.4356(7) 0.3416(4) 0.5045(7) 0.048(2) Uani 1 d . . .
H13 H 0.4663 0.3712 0.5414 0.058 Uiso 1 calc R . .
C14 C 0.3554(8) 0.3155(3) 0.5410(7) 0.053(3) Uani 1 d . . .
H14 H 0.3322 0.3248 0.6015 0.064 Uiso 1 calc R . .
C15 C 0.3105(8) 0.2737(3) 0.4807(7) 0.051(3) Uani 1 d . . .
C16 C 0.2153(6) 0.2400(3) 0.4970(6) 0.0329(19) Uani 1 d . . .
H16A H 0.2131 0.2361 0.5683 0.039 Uiso 1 calc R . .
H16B H 0.1510 0.2592 0.4688 0.039 Uiso 1 calc R . .
N17 N 0.3496(5) 0.2579(2) 0.3953(5) 0.0330(16) Uani 1 d . . .
C51 C 0.2818(6) 0.0797(3) 0.2624(5) 0.0297(19) Uani 1 d . . .
H51A H 0.2775 0.0704 0.3317 0.036 Uiso 1 calc R . .
H51B H 0.3564 0.0870 0.2565 0.036 Uiso 1 calc R . .
C52 C 0.2476(6) 0.0302(3) 0.1993(6) 0.036(2) Uani 1 d . . .
H52A H 0.1752 0.0207 0.2099 0.043 Uiso 1 calc R . .
H52B H 0.2460 0.0403 0.1296 0.043 Uiso 1 calc R . .
C53 C 0.3156(7) -0.0200(3) 0.2182(7) 0.050(2) Uani 1 d . . .
H53A H 0.3844 -0.0139 0.1952 0.060 Uiso 1 calc R . .
H53B H 0.3276 -0.0277 0.2893 0.060 Uiso 1 calc R . .
N54 N 0.2625(5) -0.0665(2) 0.1654(5) 0.0424(18) Uani 1 d . . .
H54A H 0.2182 -0.0544 0.1132 0.051 Uiso 1 calc R . .
H54B H 0.2256 -0.0850 0.2064 0.051 Uiso 1 calc R . .
H54C H 0.3112 -0.0886 0.1441 0.051 Uiso 1 calc R . .
C91 C 0.5068(7) 0.1741(3) 0.2552(6) 0.042(2) Uani 1 d . . .
H91A H 0.5635 0.1899 0.2220 0.050 Uiso 1 calc R . .
H91B H 0.4882 0.1390 0.2234 0.050 Uiso 1 calc R . .
C92 C 0.5516(6) 0.1629(3) 0.3609(5) 0.0298(19) Uani 1 d . . .
H92A H 0.4960 0.1480 0.3966 0.036 Uiso 1 calc R . .
H92B H 0.5767 0.1970 0.3932 0.036 Uiso 1 calc R . .
C93 C 0.6449(7) 0.1217(3) 0.3658(6) 0.039(2) Uani 1 d . . .
H93A H 0.6176 0.0865 0.3396 0.046 Uiso 1 calc R . .
H93B H 0.6960 0.1348 0.3233 0.046 Uiso 1 calc R . .
N94 N 0.6969(6) 0.1139(3) 0.4611(6) 0.062(2) Uani 1 d . . .
H94A H 0.6761 0.1314 0.5106 0.074 Uiso 1 calc R . .
H94B H 0.7501 0.0916 0.4711 0.074 Uiso 1 calc R . .
C101 C 0.2895(7) 0.1468(3) 0.5171(6) 0.039(2) Uani 1 d . . .
H10A H 0.3610 0.1623 0.5250 0.047 Uiso 1 calc R . .
H10B H 0.2923 0.1117 0.4833 0.047 Uiso 1 calc R . .
C102 C 0.2566(10) 0.1367(4) 0.6210(8) 0.081(3) Uani 1 d . . .
H10C H 0.2545 0.1712 0.6567 0.097 Uiso 1 calc R . .
H10D H 0.1859 0.1203 0.6149 0.097 Uiso 1 calc R . .
C103 C 0.3366(9) 0.0987(4) 0.6771(7) 0.068(3) Uani 1 d . . .
H10E H 0.3243 0.0615 0.6519 0.081 Uiso 1 calc R . .
H10F H 0.4080 0.1096 0.6656 0.081 Uiso 1 calc R . .
N104 N 0.3300(11) 0.0993(5) 0.7806(9) 0.151(5) Uani 1 d . . .
H10G H 0.3139 0.1331 0.7992 0.181 Uiso 1 calc R . .
H10H H 0.3926 0.0892 0.8137 0.181 Uiso 1 calc R . .
H10I H 0.2795 0.0760 0.7943 0.181 Uiso 1 calc R . .
Cl1 Cl 0.5000 0.0000 0.5000 0.0562(10) Uani 1 d SD . .
O11 O 0.5100(11) 0.0092(5) 0.3981(4) 0.077(4) Uani 0.50 d PD . .
O12 O 0.6128(4) -0.0002(5) 0.5207(10) 0.079(4) Uani 0.50 d PD . .
O13 O 0.4643(10) 0.0537(3) 0.4728(10) 0.196(13) Uani 0.50 d PD . .
O14 O 0.5341(9) 0.0475(3) 0.5560(7) 0.111(6) Uani 0.50 d PD . .
Cl2 Cl 0.3105(3) 0.25002(13) 0.8452(2) 0.0679(8) Uani 1 d . . .
O21 O 0.4015(7) 0.2176(3) 0.8583(6) 0.103(3) Uani 1 d . . .
O22 O 0.3039(8) 0.2810(4) 0.9262(7) 0.133(4) Uani 1 d . . .
O23 O 0.2726(12) 0.2688(6) 0.7611(10) 0.208(6) Uani 1 d . . .
O24 O 0.2331(11) 0.2150(6) 0.8464(10) 0.180(5) Uani 1 d . . .
Cl3 Cl 0.4414(3) 0.42535(13) 0.1402(3) 0.0686(8) Uani 1 d . . .
O31 O 0.4418(11) 0.4168(5) 0.2346(10) 0.188(5) Uani 1 d . . .
O32 O 0.4265(8) 0.3776(4) 0.0807(7) 0.127(3) Uani 1 d . . .
O33 O 0.5176(10) 0.4546(5) 0.1050(9) 0.179(5) Uani 1 d . . .
O34 O 0.3578(15) 0.4565(6) 0.1180(11) 0.225(6) Uani 1 d . . .
Cl4 Cl 0.1224(2) 0.30704(11) 0.2011(2) 0.0621(7) Uani 1 d . . .
O41 O 0.1434(5) 0.2551(2) 0.2491(5) 0.0678(19) Uani 1 d . . .
O42 O 0.2148(9) 0.3289(4) 0.1799(8) 0.135(3) Uani 1 d . . .
O43 O 0.0949(7) 0.3380(3) 0.2763(7) 0.111(3) Uani 1 d . . .
O44 O 0.0433(9) 0.3022(4) 0.1259(8) 0.150(4) Uani 1 d . . .
Cl5 Cl 0.0428(7) 0.0052(3) 0.9609(6) 0.100(2) Uani 0.50 d P . .
O51 O -0.0655(9) 0.0293(4) 0.9597(9) 0.146(4) Uani 1 d . . .
O52 O 0.1183(14) 0.0512(6) 0.9402(14) 0.122(7) Uani 0.50 d P . .
O53 O 0.0360(18) -0.0270(9) 0.8784(18) 0.166(9) Uani 0.50 d P . .
C201 C 0.6569(7) 0.0553(3) 1.1084(6) 0.042(2) Uani 1 d . . .
H20A H 0.7088 0.0802 1.1418 0.050 Uiso 1 calc R . .
H20B H 0.6928 0.0264 1.0775 0.050 Uiso 1 calc R . .
H20C H 0.6151 0.0397 1.1561 0.050 Uiso 1 calc R . .
O202 O 0.5939(7) 0.0821(3) 1.0398(6) 0.108(3) Uani 1 d . . .
H202 H 0.5331 0.0827 1.0551 0.129 Uiso 1 calc R . .
O401 O 0.8217(9) 0.0329(4) 0.3728(8) 0.047(3) Uiso 0.50 d P . .

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 0.0342(6) 0.0329(5) 0.0364(6) 0.0003(5) 0.0024(4) -0.0013(5)
N1 0.027(4) 0.031(4) 0.022(3) 0.005(3) 0.006(3) -0.002(3)
C2 0.040(6) 0.046(5) 0.053(6) 0.003(5) 0.009(5) -0.001(4)
C3 0.026(5) 0.042(5) 0.061(6) 0.004(5) 0.012(4) -0.007(4)
C4 0.026(5) 0.032(4) 0.035(5) -0.006(4) -0.008(4) -0.003(4)
N5 0.039(5) 0.025(3) 0.031(4) 0.001(3) -0.006(3) -0.003(3)
C6 0.051(6) 0.037(5) 0.039(5) -0.009(4) -0.007(5) 0.001(4)
C7 0.060(7) 0.060(6) 0.050(6) 0.006(5) 0.000(5) 0.006(5)
C8 0.046(6) 0.028(4) 0.032(5) 0.009(4) 0.004(4) 0.008(4)
N9 0.032(4) 0.021(3) 0.023(3) -0.002(3) 0.001(3) 0.002(3)
C10 0.026(5) 0.034(4) 0.042(5) 0.008(4) 0.007(4) 0.000(4)
C11 0.016(4) 0.020(4) 0.035(5) 0.004(4) -0.002(4) -0.002(3)
C12 0.038(6) 0.034(5) 0.053(6) 0.010(4) 0.001(5) -0.012(4)
C13 0.045(7) 0.047(5) 0.049(6) 0.007(5) -0.006(5) -0.002(5)
C14 0.063(7) 0.037(5) 0.058(6) -0.008(5) 0.000(5) -0.004(5)
C15 0.054(7) 0.041(5) 0.056(6) 0.008(5) 0.001(5) 0.015(5)
C16 0.037(5) 0.025(4) 0.039(5) 0.001(4) 0.013(4) 0.003(4)
N17 0.039(4) 0.028(4) 0.029(4) -0.006(3) -0.009(3) -0.001(3)
C51 0.028(5) 0.043(5) 0.018(4) 0.004(4) 0.004(4) -0.009(4)
C52 0.036(5) 0.035(4) 0.037(5) -0.004(4) 0.006(4) 0.000(4)
C53 0.050(6) 0.048(5) 0.052(6) -0.017(5) 0.005(5) -0.003(5)
N54 0.053(5) 0.032(4) 0.042(4) 0.006(3) 0.009(4) 0.001(3)
C91 0.034(5) 0.054(5) 0.039(5) -0.007(4) 0.009(4) 0.001(4)
C92 0.019(5) 0.030(4) 0.040(5) 0.000(4) 0.004(4) 0.001(3)
C93 0.040(6) 0.033(4) 0.043(5) 0.002(4) 0.005(4) -0.004(4)
N94 0.053(6) 0.065(6) 0.066(6) 0.009(4) -0.001(5) 0.014(4)
C101 0.040(6) 0.030(4) 0.047(5) -0.003(4) 0.010(5) -0.005(4)
C102 0.106(10) 0.065(7) 0.072(8) 0.014(6) 0.009(7) 0.004(7)
C103 0.084(9) 0.081(7) 0.040(6) -0.002(6) 0.016(6) -0.009(6)
N104 0.182(14) 0.131(10) 0.143(12) 0.037(9) 0.038(10) 0.038(9)
Cl1 0.061(3) 0.055(2) 0.053(2) -0.0048(19) 0.007(2) -0.0088(18)
O11 0.075(11) 0.058(9) 0.095(12) 0.002(8) -0.003(9) -0.015(8)
O12 0.064(11) 0.087(11) 0.080(11) -0.005(8) -0.013(9) 0.007(8)
O13 0.23(3) 0.098(15) 0.29(3) 0.13(2) 0.16(2) 0.115(18)
O14 0.104(15) 0.108(14) 0.127(17) 0.031(13) 0.037(13) 0.029(12)
Cl2 0.068(2) 0.0745(19) 0.061(2) -0.0005(16) 0.0066(16) 0.0093(17)
O21 0.084(6) 0.110(6) 0.114(7) -0.003(5) 0.014(5) 0.018(5)
O22 0.165(10) 0.123(7) 0.103(7) -0.012(6) -0.010(7) 0.038(7)
O23 0.256(16) 0.240(14) 0.140(11) 0.022(11) 0.068(11) 0.075(12)
O24 0.146(11) 0.216(13) 0.178(12) 0.015(10) 0.019(9) -0.009(10)
Cl3 0.069(2) 0.0645(18) 0.074(2) -0.0024(17) 0.0153(18) 0.0017(16)
O31 0.222(15) 0.199(12) 0.138(11) 0.008(9) 0.004(10) -0.007(10)
O32 0.115(8) 0.126(7) 0.141(8) 0.007(7) 0.019(6) 0.009(6)
O33 0.149(11) 0.191(11) 0.199(13) 0.006(10) 0.031(10) -0.041(10)
O34 0.231(17) 0.234(15) 0.208(16) -0.059(12) 0.022(13) -0.007(14)
Cl4 0.0554(19) 0.0527(16) 0.079(2) 0.0080(16) 0.0101(16) 0.0024(15)
O41 0.061(5) 0.060(4) 0.079(5) 0.001(4) -0.005(4) 0.002(4)
O42 0.133(9) 0.113(7) 0.161(9) 0.024(6) 0.031(7) 0.003(7)
O43 0.102(7) 0.101(6) 0.133(8) -0.004(6) 0.028(6) -0.015(5)
O44 0.135(9) 0.149(9) 0.156(10) 0.020(8) -0.015(8) 0.017(7)
Cl5 0.113(7) 0.081(5) 0.097(6) -0.006(4) -0.024(4) 0.009(5)
O51 0.150(11) 0.124(8) 0.157(10) -0.006(8) -0.009(8) 0.005(7)
O52 0.123(15) 0.065(10) 0.158(17) -0.017(11) -0.064(13) 0.001(10)
O53 0.16(2) 0.18(2) 0.15(2) -0.033(17) -0.023(16) -0.026(17)
C201 0.067(7) 0.024(4) 0.033(5) 0.002(4) -0.004(5) 0.015(4)
O202 0.080(6) 0.144(8) 0.106(7) -0.007(6) 0.040(5) 0.016(6)

_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 N17 1.913(6) . ?
Cu1 N5 2.054(6) . ?
Cu1 N9 2.090(6) . ?
Cu1 N1 2.095(6) . ?
N1 C16 1.476(8) . ?
N1 C2 1.501(9) . ?
N1 C101 1.508(9) . ?
C2 C3 1.513(10) . ?
C3 C4 1.488(10) . ?
C4 N5 1.527(9) . ?
N5 C6 1.453(9) . ?
N5 C51 1.479(9) . ?
C6 C7 1.558(11) . ?
C7 C8 1.506(10) . ?
C8 N9 1.479(9) . ?
N9 C91 1.485(9) . ?
N9 C10 1.519(8) . ?
C10 C11 1.450(10) . ?
C11 N17 1.357(9) . ?
C11 C12 1.384(10) . ?
C12 C13 1.353(11) . ?
C13 C14 1.340(12) . ?
C14 C15 1.377(11) . ?
C15 N17 1.366(10) . ?
C15 C16 1.493(11) . ?
C51 C52 1.504(9) . ?
C52 C53 1.493(10) . ?
C53 N54 1.453(9) . ?
C91 C92 1.490(10) . ?
C92 C93 1.540(10) . ?
C93 N94 1.380(9) . ?
C101 C102 1.533(12) . ?
C102 C103 1.498(13) . ?
C103 N104 1.409(13) . ?
Cl1 O13 1.414(5) 3_656 ?
Cl1 O13 1.414(5) . ?
Cl1 O12 1.415(5) 3_656 ?
Cl1 O12 1.415(5) . ?
Cl1 O11 1.415(5) . ?
Cl1 O11 1.415(5) 3_656 ?
Cl1 O14 1.415(5) 3_656 ?
Cl1 O14 1.415(5) . ?
O11 O13 1.633(6) . ?
O11 O14 1.636(6) 3_656 ?
O12 O13 1.633(6) 3_656 ?
O12 O14 1.636(6) . ?
O13 O14 1.343(11) . ?
O13 O12 1.633(6) 3_656 ?
O14 O11 1.636(6) 3_656 ?
Cl2 O23 1.258(14) . ?
Cl2 O24 1.296(14) . ?
Cl2 O22 1.337(9) . ?
Cl2 O21 1.386(8) . ?
Cl3 O31 1.289(13) . ?
Cl3 O34 1.302(18) . ?
Cl3 O33 1.331(12) . ?
Cl3 O32 1.410(10) . ?
Cl4 O44 1.333(10) . ?
Cl4 O43 1.343(9) . ?
Cl4 O42 1.345(10) . ?
Cl4 O41 1.428(6) . ?
Cl5 O53 1.35(2) . ?
Cl5 O51 1.362(11) 3_557 ?
Cl5 O51 1.484(12) . ?
Cl5 O52 1.517(18) . ?
Cl5 Cl5 1.623(18) 3_557 ?
O51 Cl5 1.362(11) 3_557 ?
C201 O202 1.312(9) . ?

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
N17 Cu1 N5 177.1(2) . . ?
N17 Cu1 N9 82.8(3) . . ?
N5 Cu1 N9 96.8(2) . . ?
N17 Cu1 N1 81.8(3) . . ?
N5 Cu1 N1 99.3(2) . . ?
N9 Cu1 N1 158.0(2) . . ?
C16 N1 C2 107.2(6) . . ?
C16 N1 C101 110.5(6) . . ?
C2 N1 C101 110.9(5) . . ?
C16 N1 Cu1 105.1(4) . . ?
C2 N1 Cu1 118.0(5) . . ?
C101 N1 Cu1 105.1(4) . . ?
N1 C2 C3 110.6(7) . . ?
C4 C3 C2 119.0(7) . . ?
C3 C4 N5 116.6(6) . . ?
C6 N5 C51 115.1(6) . . ?
C6 N5 C4 106.0(6) . . ?
C51 N5 C4 111.7(5) . . ?
C6 N5 Cu1 105.3(4) . . ?
C51 N5 Cu1 110.7(4) . . ?
C4 N5 Cu1 107.5(4) . . ?
N5 C6 C7 117.7(7) . . ?
C8 C7 C6 114.4(7) . . ?
N9 C8 C7 111.6(6) . . ?
C8 N9 C91 108.0(5) . . ?
C8 N9 C10 107.8(5) . . ?
C91 N9 C10 103.9(6) . . ?
C8 N9 Cu1 114.7(5) . . ?
C91 N9 Cu1 115.4(4) . . ?
C10 N9 Cu1 106.3(4) . . ?
C11 C10 N9 113.8(6) . . ?
N17 C11 C12 118.1(7) . . ?
N17 C11 C10 113.6(6) . . ?
C12 C11 C10 128.0(7) . . ?
C13 C12 C11 118.1(8) . . ?
C14 C13 C12 126.3(9) . . ?
C13 C14 C15 113.9(9) . . ?
N17 C15 C14 122.7(9) . . ?
N17 C15 C16 110.7(8) . . ?
C14 C15 C16 126.6(9) . . ?
N1 C16 C15 112.9(6) . . ?
C11 N17 C15 120.7(7) . . ?
C11 N17 Cu1 119.5(5) . . ?
C15 N17 Cu1 119.7(6) . . ?
N5 C51 C52 116.7(6) . . ?
C53 C52 C51 116.1(7) . . ?
N54 C53 C52 109.5(7) . . ?
N9 C91 C92 118.7(6) . . ?
C91 C92 C93 110.7(6) . . ?
N94 C93 C92 113.4(7) . . ?
N1 C101 C102 114.6(7) . . ?
C103 C102 C101 108.5(9) . . ?
N104 C103 C102 111.8(10) . . ?
O13 Cl1 O13 180.000(2) 3_656 . ?
O13 Cl1 O12 109.47(8) 3_656 3_656 ?
O13 Cl1 O12 70.53(8) . 3_656 ?
O13 Cl1 O12 70.53(8) 3_656 . ?
O13 Cl1 O12 109.47(8) . . ?
O12 Cl1 O12 180.0 3_656 . ?
O13 Cl1 O11 109.46(8) 3_656 . ?
O13 Cl1 O11 70.54(8) . . ?
O12 Cl1 O11 91.2(8) 3_656 . ?
O12 Cl1 O11 88.8(8) . . ?
O13 Cl1 O11 70.54(8) 3_656 3_656 ?
O13 Cl1 O11 109.46(8) . 3_656 ?
O12 Cl1 O11 88.8(8) 3_656 3_656 ?
O12 Cl1 O11 91.2(8) . 3_656 ?
O11 Cl1 O11 180.000(2) . 3_656 ?
O13 Cl1 O14 56.7(4) 3_656 3_656 ?
O13 Cl1 O14 123.3(4) . 3_656 ?
O12 Cl1 O14 70.65(9) 3_656 3_656 ?
O12 Cl1 O14 109.35(9) . 3_656 ?
O11 Cl1 O14 70.64(10) . 3_656 ?
O11 Cl1 O14 109.36(10) 3_656 3_656 ?
O13 Cl1 O14 123.3(4) 3_656 . ?
O13 Cl1 O14 56.7(4) . . ?
O12 Cl1 O14 109.35(9) 3_656 . ?
O12 Cl1 O14 70.65(9) . . ?
O11 Cl1 O14 109.36(10) . . ?
O11 Cl1 O14 70.64(10) 3_656 . ?
O14 Cl1 O14 180.000(1) 3_656 . ?
Cl1 O11 O13 54.71(7) . . ?
Cl1 O11 O14 54.70(5) . 3_656 ?
O13 O11 O14 99.2(3) . 3_656 ?
Cl1 O12 O13 54.71(7) . 3_656 ?
Cl1 O12 O14 54.70(7) . . ?
O13 O12 O14 99.2(3) 3_656 . ?
O14 O13 Cl1 61.7(2) . . ?
O14 O13 O12 101.3(4) . 3_656 ?
Cl1 O13 O12 54.75(8) . 3_656 ?
O14 O13 O11 101.3(4) . . ?
Cl1 O13 O11 54.75(8) . . ?
O12 O13 O11 76.4(6) 3_656 . ?
O13 O14 Cl1 61.6(2) . . ?
O13 O14 O11 101.2(4) . 3_656 ?
Cl1 O14 O11 54.66(9) . 3_656 ?
O13 O14 O12 101.2(4) . . ?
Cl1 O14 O12 54.65(9) . . ?
O11 O14 O12 76.3(6) 3_656 . ?
O23 Cl2 O24 92.8(9) . . ?
O23 Cl2 O22 118.5(7) . . ?
O24 Cl2 O22 103.5(8) . . ?
O23 Cl2 O21 122.2(8) . . ?
O24 Cl2 O21 103.7(7) . . ?
O22 Cl2 O21 110.7(6) . . ?
O31 Cl3 O34 102.7(9) . . ?
O31 Cl3 O33 121.8(8) . . ?
O34 Cl3 O33 102.1(9) . . ?
O31 Cl3 O32 114.3(7) . . ?
O34 Cl3 O32 107.6(8) . . ?
O33 Cl3 O32 106.6(7) . . ?
O44 Cl4 O43 112.5(7) . . ?
O44 Cl4 O42 117.2(7) . . ?
O43 Cl4 O42 104.7(6) . . ?
O44 Cl4 O41 110.2(5) . . ?
O43 Cl4 O41 101.7(5) . . ?
O42 Cl4 O41 109.3(5) . . ?
O53 Cl5 O51 105.9(12) . 3_557 ?
O53 Cl5 O51 105.0(12) . . ?
O51 Cl5 O51 110.6(9) 3_557 . ?
O53 Cl5 O52 104.4(14) . . ?
O51 Cl5 O52 121.7(10) 3_557 . ?
O51 Cl5 O52 107.9(10) . . ?
O53 Cl5 Cl5 117.8(13) . 3_557 ?
O51 Cl5 Cl5 58.9(7) 3_557 3_557 ?
O51 Cl5 Cl5 51.8(6) . 3_557 ?
O52 Cl5 Cl5 136.2(10) . 3_557 ?
Cl5 O51 Cl5 69.4(9) 3_557 . ?

_diffrn_measured_fraction_theta_max 0.895
_diffrn_reflns_theta_full        25.89
_diffrn_measured_fraction_theta_full 0.895
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.093

_publ_section_references         
;

Sheldrick, G.M. (1997) SHELXL97 program for crystallography refinement.
University of Gottingen, Germany.

Spek, A.L., (1994) PLATON program, Utrecht University, The Netherlands
;

#===END