# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2001
# CCDC Number: 186/2281
 
 
#====================
data_Clifford #et al. Cu macrocycle
 
_publ_contact_author 
; 
 Dr T. Clifford
    Dept. of Chemistry
    University of Kansas
    Mallot Hall
    Lawrence, Kansas, 66045
    USA

; 
_publ_contact_author_email      tc@eagle.cc.ukans.edu 
_publ_contact_author_fax        1(785)8645396 
_publ_contact_author_phone      1(785)8644818 

_publ_requested_journal         'J Chem Soc Dalton Trans.'


_publ_section_title 
; 
 Preparation of the copper(II) complex of the binucleating hexaaza macrocycle (1,4,7,16,19,22-hexaaza[9.9]paracyclophane (PEA) and its solution chemistry, hydrolytic activity and acid dissociation kinetics.
; 
#====================

data_pea 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          
 '(C24 H38 Cl3 Cu2 N6)+ Cl- 2.9(H2 O) 2.6(C2 H3 N)' 
_chemical_formula_sum 
 'C29.19 H51.60 Cl4 Cu2 N8.60 O2.90' 
_chemical_formula_weight          838.37 
 
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' 
 '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' 
 '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    'I b c a' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'x, -y, -z+1/2' 
 '-x+1/2, y, -z' 
 '-x, -y+1/2, z' 
 'x+1/2, y+1/2, z+1/2' 
 'x+1/2, -y+1/2, -z+1' 
 '-x+1, y+1/2, -z+1/2' 
 '-x+1/2, -y+1, z+1/2' 
 '-x, -y, -z' 
 '-x, y, z-1/2' 
 'x-1/2, -y, z' 
 'x, y-1/2, -z' 
 '-x+1/2, -y+1/2, -z+1/2' 
 '-x+1/2, y+1/2, z' 
 'x, -y+1/2, z+1/2' 
 'x+1/2, y, -z+1/2' 
 
_cell_length_a                    14.971(8) 
_cell_length_b                    42.24(4) 
_cell_length_c                    25.32(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      16012(26) 
_cell_formula_units_Z             16 
_cell_measurement_temperature     120(2) 
_cell_measurement_reflns_used     25 
_cell_measurement_theta_min       9.70 
_cell_measurement_theta_max       12.45 
 
_exptl_crystal_description        prism 
_exptl_crystal_colour             blue 
_exptl_crystal_size_max           0.50 
_exptl_crystal_size_mid           0.40 
_exptl_crystal_size_min           0.35 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.391 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              6978 
_exptl_absorpt_coefficient_mu     1.369 
_exptl_absorpt_correction_type    empirical 
_exptl_absorpt_correction_T_min   0.5476 
_exptl_absorpt_correction_T_max   0.6458 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       493(2) 
_diffrn_radiation_wavelength      0.71069 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        'Rigaku AFC7S' 
_diffrn_measurement_method        '\q-2\q scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  150 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         -8.25 
_diffrn_reflns_number             5676 
_diffrn_reflns_av_R_equivalents   0.0164 
_diffrn_reflns_av_sigmaI/netI     0.0471 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -38 
_diffrn_reflns_limit_k_max        0 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        23 
_diffrn_reflns_theta_min          2.51 
_diffrn_reflns_theta_max          18.96 
_reflns_number_total              3195 
_reflns_number_gt                 2306 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_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  
_refine_ls_weighting_details 
 'calc w=1/[\s^2^(Fo^2^)+(0.1240P)^2^+1000.0000P] 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          3195 
_refine_ls_number_parameters      393 
_refine_ls_number_restraints      70 
_refine_ls_R_factor_all           0.1524 
_refine_ls_R_factor_gt            0.1011 
_refine_ls_wR_factor_ref          0.3101 
_refine_ls_wR_factor_gt           0.2536 
_refine_ls_goodness_of_fit_ref    1.058 
_refine_ls_restrained_S_all       1.046 
_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 0.48008(15) 0.19583(5) 0.10863(9) 0.0485(9) Uani 1 1 d . . . 
Cu2 Cu 0.35445(17) 0.05005(6) 0.21889(15) 0.0885(13) Uani 1 1 d . . . 
Cl1 Cl 0.5968(3) 0.20375(11) 0.16241(18) 0.0479(14) Uani 1 1 d . . . 
Cl2 Cl 0.5000 0.2500 0.0509(3) 0.059(2) Uani 1 2 d S . . 
Cl3 Cl 0.4554(4) 0.04956(13) 0.2858(3) 0.082(2) Uani 1 1 d . . . 
Cl4 Cl 0.2609(6) 0.0001(6) 0.2339(3) 0.051(4) Uani 0.50 1 d P . . 
N1 N 0.3900(10) 0.2188(4) 0.1545(6) 0.059(4) Uani 1 1 d U . . 
H1 H 0.3997 0.2394 0.1461 0.070 Uiso 1 1 calc R . . 
N2 N 0.3750(10) 0.1832(4) 0.0648(7) 0.066(5) Uani 1 1 d U . . 
H2 H 0.3544 0.1644 0.0774 0.079 Uiso 1 1 calc R . . 
N3 N 0.5505(10) 0.1731(4) 0.0522(6) 0.061(4) Uani 1 1 d U . . 
H3 H 0.5765 0.1888 0.0330 0.073 Uiso 1 1 calc R . . 
N4 N 0.4321(11) 0.0260(4) 0.1677(9) 0.089(6) Uani 1 1 d U . . 
H4 H 0.4261 0.0056 0.1787 0.107 Uiso 1 1 calc R . . 
N5 N 0.2744(11) 0.0562(4) 0.1564(10) 0.103(7) Uani 1 1 d U . . 
H5 H 0.2925 0.0740 0.1391 0.124 Uiso 1 1 calc R . . 
N6 N 0.2559(11) 0.0741(3) 0.2587(10) 0.090(6) Uani 1 1 d U . . 
H6 H 0.2263 0.0586 0.2764 0.107 Uiso 1 1 calc R . . 
C1 C 0.2992(13) 0.2132(5) 0.1340(10) 0.080(6) Uani 1 1 d U . . 
H1A H 0.2619 0.2316 0.1404 0.096 Uiso 1 1 calc R . . 
H1B H 0.2726 0.1951 0.1515 0.096 Uiso 1 1 calc R . . 
C2 C 0.3069(13) 0.2069(6) 0.0744(11) 0.087(7) Uani 1 1 d U . . 
H2A H 0.2499 0.1996 0.0608 0.104 Uiso 1 1 calc R . . 
H2B H 0.3224 0.2264 0.0562 0.104 Uiso 1 1 calc R . . 
C3 C 0.4047(15) 0.1781(6) 0.0091(10) 0.092(8) Uani 1 1 d U . . 
H3A H 0.4200 0.1981 -0.0076 0.110 Uiso 1 1 calc R . . 
H3B H 0.3582 0.1679 -0.0114 0.110 Uiso 1 1 calc R . . 
C4 C 0.4869(14) 0.1567(5) 0.0137(9) 0.086(8) Uani 1 1 d U . . 
H4A H 0.4701 0.1360 0.0270 0.103 Uiso 1 1 calc R . . 
H4B H 0.5152 0.1541 -0.0205 0.103 Uiso 1 1 calc R . . 
C5 C 0.6260(12) 0.1505(5) 0.0649(8) 0.060(4) Uani 1 1 d U . . 
H5A H 0.6582 0.1460 0.0325 0.071 Uiso 1 1 calc R . . 
H5B H 0.6672 0.1610 0.0887 0.071 Uiso 1 1 calc R . . 
C6 C 0.5995(13) 0.1198(5) 0.0893(8) 0.059(5) Uani 1 1 d U . . 
C7 C 0.6348(14) 0.0917(5) 0.0699(9) 0.073(5) Uani 1 1 d U . . 
H7 H 0.6725 0.0917 0.0407 0.087 Uiso 1 1 calc R . . 
C8 C 0.6123(14) 0.0632(6) 0.0954(10) 0.077(6) Uani 1 1 d U . . 
H8 H 0.6382 0.0446 0.0831 0.093 Uiso 1 1 calc R . . 
C9 C 0.5541(12) 0.0613(5) 0.1376(9) 0.063(5) Uani 1 1 d U . . 
C10 C 0.5193(14) 0.0898(5) 0.1553(10) 0.071(6) Uani 1 1 d U . . 
H10 H 0.4806 0.0899 0.1841 0.085 Uiso 1 1 calc R . . 
C11 C 0.5412(12) 0.1184(5) 0.1311(8) 0.056(5) Uani 1 1 d U . . 
H11 H 0.5157 0.1370 0.1435 0.067 Uiso 1 1 calc R . . 
C12 C 0.5305(13) 0.0299(5) 0.1635(10) 0.077(5) Uani 1 1 d U . . 
H12A H 0.5551 0.0127 0.1428 0.093 Uiso 1 1 calc R . . 
H12B H 0.5568 0.0291 0.1985 0.093 Uiso 1 1 calc R . . 
C13 C 0.3896(15) 0.0256(6) 0.1139(13) 0.114(9) Uani 1 1 d U . . 
H13A H 0.4027 0.0058 0.0962 0.137 Uiso 1 1 calc R . . 
H13B H 0.4128 0.0428 0.0926 0.137 Uiso 1 1 calc R . . 
C14 C 0.2878(15) 0.0293(5) 0.1211(14) 0.119(10) Uani 1 1 d U . . 
H14A H 0.2593 0.0332 0.0873 0.143 Uiso 1 1 calc R . . 
H14B H 0.2625 0.0103 0.1363 0.143 Uiso 1 1 calc R . . 
C15 C 0.1820(14) 0.0615(6) 0.1749(14) 0.116(8) Uani 1 1 d U . . 
H15A H 0.1560 0.0419 0.1877 0.139 Uiso 1 1 calc R . . 
H15B H 0.1451 0.0696 0.1465 0.139 Uiso 1 1 calc R . . 
C16 C 0.1886(17) 0.0855(7) 0.2193(13) 0.124(8) Uani 1 1 d U . . 
H16A H 0.2068 0.1059 0.2053 0.148 Uiso 1 1 calc R . . 
H16B H 0.1309 0.0880 0.2361 0.148 Uiso 1 1 calc R . . 
C17 C 0.2738(16) 0.0982(5) 0.3002(11) 0.095(7) Uani 1 1 d U . . 
H17A H 0.3179 0.0898 0.3245 0.115 Uiso 1 1 calc R . . 
H17B H 0.2193 0.1019 0.3199 0.115 Uiso 1 1 calc R . . 
C18 C 0.3069(14) 0.1293(5) 0.2790(10) 0.071(6) Uani 1 1 d U . . 
C19 C 0.2483(18) 0.1556(5) 0.2762(11) 0.105(10) Uani 1 1 d U . . 
H19 H 0.1903 0.1536 0.2889 0.126 Uiso 1 1 calc R . . 
C20 C 0.2754(15) 0.1840(5) 0.2550(10) 0.085(8) Uani 1 1 d U . . 
H20 H 0.2357 0.2009 0.2538 0.102 Uiso 1 1 calc R . . 
C21 C 0.3612(14) 0.1877(5) 0.2353(9) 0.070(6) Uani 1 1 d U . . 
C22 C 0.4192(13) 0.1618(5) 0.2398(8) 0.064(6) Uani 1 1 d U . . 
H22 H 0.4781 0.1640 0.2287 0.077 Uiso 1 1 calc R . . 
C23 C 0.3913(14) 0.1335(5) 0.2601(9) 0.069(6) Uani 1 1 d U . . 
H23 H 0.4311 0.1166 0.2611 0.083 Uiso 1 1 calc R . . 
C24 C 0.3912(15) 0.2193(5) 0.2131(8) 0.069(5) Uani 1 1 d U . . 
H24A H 0.3519 0.2359 0.2258 0.083 Uiso 1 1 calc R . . 
H24B H 0.4512 0.2239 0.2254 0.083 Uiso 1 1 calc R . . 
Cl5 Cl 0.2714(5) 0.11812(15) 0.0864(4) 0.120(3) Uani 1 1 d . . . 
O1 O 0.0799(13) 0.0161(5) 0.0248(7) 0.129(7) Uiso 1 1 d . . . 
H1OA H 0.0960 0.0364 0.0197 0.154 Uiso 1 1 d R . . 
H1OB H 0.1324 0.0068 0.0172 0.154 Uiso 1 1 d R . . 
O2 O 0.1295(14) 0.0811(5) 0.0091(9) 0.141(7) Uiso 1 1 d . . . 
H2OA H 0.1679 0.0912 0.0306 0.170 Uiso 1 1 d R . . 
H2OB H 0.1566 0.0914 -0.0176 0.170 Uiso 1 1 d R . . 
O3 O 0.2500 -0.0126(9) 0.0000 0.197(16) Uiso 1 2 d S . . 
H3OA H 0.2831 -0.0263 0.0188 0.237 Uiso 1 1 d R . . 
N1S N 0.572(3) 0.2145(12) 0.3408(17) 0.238(18) Uiso 1 1 d . . . 
C2S C 0.576(3) 0.1876(11) 0.3589(16) 0.160(14) Uiso 1 1 d . . . 
C3S C 0.575(2) 0.1563(9) 0.3508(14) 0.154(13) Uiso 1 1 d . . . 
H3SA H 0.6139 0.1461 0.3755 0.231 Uiso 1 1 d R . . 
H3SB H 0.5945 0.1519 0.3155 0.231 Uiso 1 1 d R . . 
H3SC H 0.5151 0.1485 0.3554 0.231 Uiso 1 1 d R . . 
N4S N 0.334(4) -0.0508(14) 0.053(2) 0.10(2) Uiso 0.40(2) 1 d P A 1 
C5S C 0.380(7) -0.064(2) 0.061(4) 0.09(3) Uiso 0.40(2) 1 d P A 1 
C6S C 0.465(3) -0.0901(12) 0.0787(19) 0.052(15) Uiso 0.40(2) 1 d P A 1 
H6SD H 0.4400 -0.1097 0.0908 0.078 Uiso 0.40(2) 1 d PR A 1 
H6SE H 0.5000 -0.0808 0.1065 0.078 Uiso 0.40(2) 1 d PR A 1 
H6SF H 0.5028 -0.0941 0.0487 0.078 Uiso 0.40(2) 1 d PR A 1 
N4S' N 0.358(3) -0.1276(10) 0.0859(16) 0.120(15) Uiso 0.60(2) 1 d P A 2 
C5S' C 0.383(3) -0.0996(9) 0.0846(15) 0.069(12) Uiso 0.60(2) 1 d P A 2 
C6S' C 0.413(3) -0.0697(11) 0.0736(19) 0.067(16) Uiso 0.60(2) 1 d P A 2 
H6SA H 0.4121 -0.0572 0.1053 0.100 Uiso 0.60(2) 1 d PR A 2 
H6SB H 0.3743 -0.0601 0.0478 0.100 Uiso 0.60(2) 1 d PR A 2 
H6SC H 0.4725 -0.0707 0.0601 0.100 Uiso 0.60(2) 1 d PR A 2 
O4 O 0.366(3) -0.1679(11) 0.0755(17) 0.108(17) Uiso 0.40(2) 1 d P A 1 
H4OA H 0.3568 -0.1890 0.0777 0.129 Uiso 0.40(2) 1 d PR A 1 
H4OB H 0.4163 -0.1703 0.0568 0.129 Uiso 0.40(2) 1 d PR A 1 
N7S N 0.297(4) -0.2115(13) 0.034(2) 0.17(2) Uiso 0.60(2) 1 d P A 2 
C8S C 0.332(4) -0.2153(13) 0.074(3) 0.118(19) Uiso 0.60(2) 1 d P A 2 
C9S C 0.344(4) -0.2041(14) 0.114(2) 0.14(2) Uiso 0.60(2) 1 d P A 2 
H9SA H 0.3763 -0.2186 0.1358 0.213 Uiso 0.60(2) 1 d PR A 2 
H9SB H 0.2883 -0.1988 0.1298 0.213 Uiso 0.60(2) 1 d PR A 2 
H9SC H 0.3791 -0.1851 0.1090 0.213 Uiso 0.60(2) 1 d PR A 2 
 
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 0.0457(16) 0.0556(16) 0.0442(15) -0.0187(13) -0.0026(13) -0.0031(12) 
Cu2 0.0423(17) 0.0448(17) 0.178(4) -0.0122(19) 0.0025(19) 0.0000(13) 
Cl1 0.058(3) 0.048(3) 0.037(3) -0.011(2) -0.013(3) -0.005(2) 
Cl2 0.055(4) 0.093(5) 0.029(4) 0.000 0.000 -0.011(4) 
Cl3 0.054(4) 0.053(3) 0.138(6) -0.019(4) 0.019(4) -0.005(3) 
Cl4 0.054(5) 0.040(4) 0.058(12) 0.014(14) -0.003(5) 0.000(6) 
N1 0.061(8) 0.045(9) 0.070(8) -0.026(8) 0.026(8) -0.019(9) 
N2 0.052(10) 0.049(10) 0.096(12) -0.033(10) -0.021(9) 0.000(7) 
N3 0.049(9) 0.084(10) 0.049(11) -0.035(8) -0.006(7) 0.006(7) 
N4 0.052(8) 0.045(10) 0.170(18) -0.027(12) -0.007(10) -0.001(8) 
N5 0.039(8) 0.071(12) 0.20(2) -0.015(12) -0.024(11) 0.005(9) 
N6 0.051(11) 0.023(8) 0.194(19) 0.008(9) 0.036(11) 0.000(8) 
C1 0.049(9) 0.063(14) 0.127(12) -0.020(13) 0.020(10) 0.002(11) 
C2 0.040(12) 0.087(16) 0.133(13) -0.056(16) -0.013(10) 0.006(9) 
C3 0.075(13) 0.105(17) 0.095(13) -0.068(16) -0.041(11) 0.033(12) 
C4 0.072(13) 0.095(16) 0.091(18) -0.060(13) -0.038(9) 0.028(11) 
C5 0.048(10) 0.087(8) 0.044(13) -0.028(9) -0.004(8) 0.005(8) 
C6 0.044(12) 0.076(7) 0.057(13) -0.041(7) -0.004(8) 0.001(8) 
C7 0.058(14) 0.084(8) 0.075(15) -0.049(9) -0.001(10) 0.008(11) 
C8 0.047(13) 0.080(8) 0.106(18) -0.040(11) -0.003(10) 0.019(12) 
C9 0.033(11) 0.060(6) 0.097(15) -0.043(9) -0.015(8) 0.003(8) 
C10 0.060(14) 0.053(7) 0.100(17) -0.029(9) 0.011(10) 0.004(10) 
C11 0.048(12) 0.063(7) 0.056(13) -0.027(9) -0.004(8) 0.008(10) 
C12 0.053(8) 0.049(7) 0.130(16) -0.048(10) -0.002(10) 0.002(10) 
C13 0.066(10) 0.085(17) 0.19(2) -0.046(19) -0.033(13) 0.014(13) 
C14 0.064(9) 0.048(13) 0.24(3) -0.018(15) -0.036(13) 0.012(12) 
C15 0.044(10) 0.068(15) 0.24(2) 0.010(15) -0.004(14) -0.003(12) 
C16 0.058(17) 0.085(19) 0.23(3) 0.003(14) 0.015(12) 0.018(13) 
C17 0.083(16) 0.037(8) 0.17(2) 0.008(9) 0.063(13) -0.007(9) 
C18 0.069(11) 0.038(6) 0.106(19) 0.001(8) 0.043(13) -0.011(6) 
C19 0.091(14) 0.061(11) 0.16(3) 0.041(15) 0.073(18) 0.012(9) 
C20 0.085(12) 0.063(10) 0.106(19) 0.032(13) 0.064(15) 0.014(9) 
C21 0.064(10) 0.057(8) 0.088(14) -0.008(10) 0.030(12) -0.014(6) 
C22 0.048(10) 0.070(10) 0.075(16) 0.008(12) 0.021(11) -0.015(7) 
C23 0.067(10) 0.060(9) 0.082(17) -0.002(11) 0.038(12) -0.013(8) 
C24 0.085(13) 0.053(8) 0.069(8) -0.019(10) 0.051(9) -0.013(9) 
Cl5 0.093(5) 0.066(4) 0.202(9) -0.029(5) -0.006(5) -0.012(4) 
 
_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 N2 1.997(15) . ? 
Cu1 N3 2.018(15) . ? 
Cu1 N1 2.026(14) . ? 
Cu1 Cl1 2.241(5) . ? 
Cu1 Cl2 2.731(5) . ? 
Cu2 N5 2.00(2) . ? 
Cu2 N4 2.014(19) . ? 
Cu2 N6 2.056(17) . ? 
Cu2 Cl3 2.270(8) . ? 
Cu2 Cl4 2.56(2) . ? 
Cl2 Cu1 2.731(5) 4_655 ? 
Cl4 Cl4 0.816(16) 2 ? 
N1 C1 1.47(3) . ? 
N1 C24 1.49(2) . ? 
N2 C2 1.45(2) . ? 
N2 C3 1.50(3) . ? 
N3 C5 1.52(2) . ? 
N3 C4 1.53(2) . ? 
N4 C12 1.49(2) . ? 
N4 C13 1.50(3) . ? 
N5 C14 1.46(3) . ? 
N5 C15 1.48(3) . ? 
N6 C17 1.49(3) . ? 
N6 C16 1.50(3) . ? 
C1 C2 1.54(3) . ? 
C3 C4 1.53(3) . ? 
C5 C6 1.49(3) . ? 
C6 C11 1.37(3) . ? 
C6 C7 1.39(3) . ? 
C7 C8 1.40(3) . ? 
C8 C9 1.38(3) . ? 
C9 C10 1.39(3) . ? 
C9 C12 1.52(3) . ? 
C10 C11 1.39(3) . ? 
C13 C14 1.54(3) . ? 
C15 C16 1.52(4) . ? 
C17 C18 1.50(3) . ? 
C18 C23 1.36(3) . ? 
C18 C19 1.42(3) . ? 
C19 C20 1.37(3) . ? 
C20 C21 1.39(3) . ? 
C21 C22 1.40(3) . ? 
C21 C24 1.51(3) . ? 
C22 C23 1.37(3) . ? 
N1S C2S 1.23(5) . ? 
C2S C3S 1.34(5) . ? 
N4S C5S 0.92(9) . ? 
C5S C6S 1.74(12) . ? 
N4S' C5S' 1.24(5) . ? 
C5S' C6S' 1.37(5) . ? 
N7S C8S 1.16(7) . ? 
C8S C9S 1.12(6) . ? 
 
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 
N2 Cu1 N3 83.8(6) . . ? 
N2 Cu1 N1 85.5(7) . . ? 
N3 Cu1 N1 168.7(6) . . ? 
N2 Cu1 Cl1 172.6(5) . . ? 
N3 Cu1 Cl1 95.3(4) . . ? 
N1 Cu1 Cl1 95.7(5) . . ? 
N2 Cu1 Cl2 90.7(5) . . ? 
N3 Cu1 Cl2 87.9(5) . . ? 
N1 Cu1 Cl2 88.8(5) . . ? 
Cl1 Cu1 Cl2 96.59(16) . . ? 
N5 Cu2 N4 84.4(8) . . ? 
N5 Cu2 N6 83.9(9) . . ? 
N4 Cu2 N6 168.0(9) . . ? 
N5 Cu2 Cl3 171.7(6) . . ? 
N4 Cu2 Cl3 95.2(6) . . ? 
N6 Cu2 Cl3 96.7(7) . . ? 
N5 Cu2 Cl4 84.1(6) . . ? 
N4 Cu2 Cl4 89.8(6) . . ? 
N6 Cu2 Cl4 86.7(6) . . ? 
Cl3 Cu2 Cl4 104.2(3) . . ? 
Cu1 Cl2 Cu1 115.3(3) 4_655 . ? 
Cl4 Cl4 Cu2 99(3) 2 . ? 
C1 N1 C24 111.4(16) . . ? 
C1 N1 Cu1 109.6(12) . . ? 
C24 N1 Cu1 124.8(14) . . ? 
C2 N2 C3 117.7(19) . . ? 
C2 N2 Cu1 106.1(12) . . ? 
C3 N2 Cu1 109.2(13) . . ? 
C5 N3 C4 108.3(14) . . ? 
C5 N3 Cu1 122.7(12) . . ? 
C4 N3 Cu1 109.9(11) . . ? 
C12 N4 C13 111(2) . . ? 
C12 N4 Cu2 124.2(14) . . ? 
C13 N4 Cu2 110.1(13) . . ? 
C14 N5 C15 116.2(19) . . ? 
C14 N5 Cu2 107.5(15) . . ? 
C15 N5 Cu2 109(2) . . ? 
C17 N6 C16 111.8(17) . . ? 
C17 N6 Cu2 123.7(14) . . ? 
C16 N6 Cu2 108.4(17) . . ? 
N1 C1 C2 107.7(17) . . ? 
N2 C2 C1 110(2) . . ? 
N2 C3 C4 104.5(19) . . ? 
N3 C4 C3 106.4(15) . . ? 
C6 C5 N3 116.0(16) . . ? 
C11 C6 C7 118(2) . . ? 
C11 C6 C5 121.8(18) . . ? 
C7 C6 C5 119.8(19) . . ? 
C6 C7 C8 119(2) . . ? 
C9 C8 C7 124(2) . . ? 
C8 C9 C10 116(2) . . ? 
C8 C9 C12 122.2(19) . . ? 
C10 C9 C12 122(2) . . ? 
C9 C10 C11 121(2) . . ? 
C6 C11 C10 121.9(19) . . ? 
N4 C12 C9 111.0(17) . . ? 
N4 C13 C14 108(2) . . ? 
N5 C14 C13 106.7(19) . . ? 
N5 C15 C16 106(2) . . ? 
N6 C16 C15 109(2) . . ? 
N6 C17 C18 114(2) . . ? 
C23 C18 C19 117.1(19) . . ? 
C23 C18 C17 123(2) . . ? 
C19 C18 C17 119.9(19) . . ? 
C20 C19 C18 121(2) . . ? 
C19 C20 C21 121(2) . . ? 
C20 C21 C22 117.1(19) . . ? 
C20 C21 C24 121(2) . . ? 
C22 C21 C24 122.3(18) . . ? 
C23 C22 C21 121.6(19) . . ? 
C18 C23 C22 122(2) . . ? 
N1 C24 C21 110.8(17) . . ? 
N1S C2S C3S 149(5) . . ? 
N4S C5S C6S 177(10) . . ? 
N4S' C5S' C6S' 170(5) . . ? 
C9S C8S N7S 143(8) . . ? 
 
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
N2 Cu1 Cl2 Cu1 131.7(5) . . . 4_655 ? 
N3 Cu1 Cl2 Cu1 -144.5(4) . . . 4_655 ? 
N1 Cu1 Cl2 Cu1 46.2(5) . . . 4_655 ? 
Cl1 Cu1 Cl2 Cu1 -49.40(13) . . . 4_655 ? 
N5 Cu2 Cl4 Cl4 -145(2) . . . 2 ? 
N4 Cu2 Cl4 Cl4 130(2) . . . 2 ? 
N6 Cu2 Cl4 Cl4 -61(2) . . . 2 ? 
Cl3 Cu2 Cl4 Cl4 35(2) . . . 2 ? 
N2 Cu1 N1 C1 2.4(14) . . . . ? 
N3 Cu1 N1 C1 21(4) . . . . ? 
Cl1 Cu1 N1 C1 -170.2(13) . . . . ? 
Cl2 Cu1 N1 C1 93.3(14) . . . . ? 
N2 Cu1 N1 C24 138.6(15) . . . . ? 
N3 Cu1 N1 C24 157(3) . . . . ? 
Cl1 Cu1 N1 C24 -34.1(14) . . . . ? 
Cl2 Cu1 N1 C24 -130.6(14) . . . . ? 
N3 Cu1 N2 C2 -152.1(17) . . . . ? 
N1 Cu1 N2 C2 24.4(16) . . . . ? 
Cl1 Cu1 N2 C2 124(4) . . . . ? 
Cl2 Cu1 N2 C2 -64.3(16) . . . . ? 
N3 Cu1 N2 C3 -24.3(14) . . . . ? 
N1 Cu1 N2 C3 152.2(14) . . . . ? 
Cl1 Cu1 N2 C3 -108(4) . . . . ? 
Cl2 Cu1 N2 C3 63.5(13) . . . . ? 
N2 Cu1 N3 C5 -135.3(16) . . . . ? 
N1 Cu1 N3 C5 -154(3) . . . . ? 
Cl1 Cu1 N3 C5 37.3(15) . . . . ? 
Cl2 Cu1 N3 C5 133.8(14) . . . . ? 
N2 Cu1 N3 C4 -6.3(14) . . . . ? 
N1 Cu1 N3 C4 -25(4) . . . . ? 
Cl1 Cu1 N3 C4 166.3(14) . . . . ? 
Cl2 Cu1 N3 C4 -97.3(14) . . . . ? 
N5 Cu2 N4 C12 134(2) . . . . ? 
N6 Cu2 N4 C12 146(3) . . . . ? 
Cl3 Cu2 N4 C12 -37.2(19) . . . . ? 
Cl4 Cu2 N4 C12 -141.5(19) . . . . ? 
N5 Cu2 N4 C13 -0.5(16) . . . . ? 
N6 Cu2 N4 C13 11(4) . . . . ? 
Cl3 Cu2 N4 C13 -172.2(15) . . . . ? 
Cl4 Cu2 N4 C13 83.6(15) . . . . ? 
N4 Cu2 N5 C14 28.2(16) . . . . ? 
N6 Cu2 N5 C14 -149.4(17) . . . . ? 
Cl3 Cu2 N5 C14 116(4) . . . . ? 
Cl4 Cu2 N5 C14 -62.1(16) . . . . ? 
N4 Cu2 N5 C15 155.1(15) . . . . ? 
N6 Cu2 N5 C15 -22.5(14) . . . . ? 
Cl3 Cu2 N5 C15 -117(4) . . . . ? 
Cl4 Cu2 N5 C15 64.8(14) . . . . ? 
N5 Cu2 N6 C17 -140.3(18) . . . . ? 
N4 Cu2 N6 C17 -152(3) . . . . ? 
Cl3 Cu2 N6 C17 31.4(17) . . . . ? 
Cl4 Cu2 N6 C17 135.3(17) . . . . ? 
N5 Cu2 N6 C16 -6.5(15) . . . . ? 
N4 Cu2 N6 C16 -18(4) . . . . ? 
Cl3 Cu2 N6 C16 165.1(13) . . . . ? 
Cl4 Cu2 N6 C16 -90.9(14) . . . . ? 
C24 N1 C1 C2 -169.7(17) . . . . ? 
Cu1 N1 C1 C2 -27(2) . . . . ? 
C3 N2 C2 C1 -168.9(18) . . . . ? 
Cu1 N2 C2 C1 -46(2) . . . . ? 
N1 C1 C2 N2 50(2) . . . . ? 
C2 N2 C3 C4 169.8(18) . . . . ? 
Cu1 N2 C3 C4 49(2) . . . . ? 
C5 N3 C4 C3 171.0(19) . . . . ? 
Cu1 N3 C4 C3 35(2) . . . . ? 
N2 C3 C4 N3 -53(2) . . . . ? 
C4 N3 C5 C6 -59(2) . . . . ? 
Cu1 N3 C5 C6 70(2) . . . . ? 
N3 C5 C6 C11 -48(3) . . . . ? 
N3 C5 C6 C7 132.9(19) . . . . ? 
C11 C6 C7 C8 -3(3) . . . . ? 
C5 C6 C7 C8 176.6(19) . . . . ? 
C6 C7 C8 C9 3(3) . . . . ? 
C7 C8 C9 C10 -2(3) . . . . ? 
C7 C8 C9 C12 179(2) . . . . ? 
C8 C9 C10 C11 1(3) . . . . ? 
C12 C9 C10 C11 -179.8(19) . . . . ? 
C7 C6 C11 C10 2(3) . . . . ? 
C5 C6 C11 C10 -177.2(19) . . . . ? 
C9 C10 C11 C6 -1(3) . . . . ? 
C13 N4 C12 C9 62(2) . . . . ? 
Cu2 N4 C12 C9 -73(3) . . . . ? 
C8 C9 C12 N4 -129(2) . . . . ? 
C10 C9 C12 N4 52(3) . . . . ? 
C12 N4 C13 C14 -167.0(17) . . . . ? 
Cu2 N4 C13 C14 -26(2) . . . . ? 
C15 N5 C14 C13 -172(2) . . . . ? 
Cu2 N5 C14 C13 -49(3) . . . . ? 
N4 C13 C14 N5 49(3) . . . . ? 
C14 N5 C15 C16 168(2) . . . . ? 
Cu2 N5 C15 C16 46(2) . . . . ? 
C17 N6 C16 C15 173(2) . . . . ? 
Cu2 N6 C16 C15 34(2) . . . . ? 
N5 C15 C16 N6 -52(3) . . . . ? 
C16 N6 C17 C18 -58(3) . . . . ? 
Cu2 N6 C17 C18 74(2) . . . . ? 
N6 C17 C18 C23 -74(3) . . . . ? 
N6 C17 C18 C19 104(3) . . . . ? 
C23 C18 C19 C20 0(4) . . . . ? 
C17 C18 C19 C20 -177(3) . . . . ? 
C18 C19 C20 C21 0(5) . . . . ? 
C19 C20 C21 C22 -2(4) . . . . ? 
C19 C20 C21 C24 -179(3) . . . . ? 
C20 C21 C22 C23 3(4) . . . . ? 
C24 C21 C22 C23 180(2) . . . . ? 
C19 C18 C23 C22 1(4) . . . . ? 
C17 C18 C23 C22 178(2) . . . . ? 
C21 C22 C23 C18 -3(4) . . . . ? 
C1 N1 C24 C21 62(2) . . . . ? 
Cu1 N1 C24 C21 -74(2) . . . . ? 
C20 C21 C24 N1 -102(2) . . . . ? 
C22 C21 C24 N1 82(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 
N1 H1 Cl1  0.91 2.44 3.285(16) 155.3 4_655 
N1 H1 Cl2  0.91 2.87 3.365(17) 115.4 . 
N2 H2 Cl5  0.91 2.33 3.203(18) 161.5 . 
N3 H3 Cl2  0.91 2.86 3.334(17) 113.7 . 
N4 H4 Cl3  0.91 2.54 3.42(2) 164.1 2 
N5 H5 Cl5  0.91 2.31 3.16(2) 154.2 . 
N6 H6 Cl4  0.91 2.74 3.19(3) 111.4 . 
O1 H1OA O2  0.90 1.97 2.87(3) 179.1 . 
O1 H1OB O3  0.90 1.99 2.89(3) 178.3 . 
O2 H2OA Cl5  0.90 2.39 3.28(2) 178.9 . 
O2 H2OB Cl5  0.90 2.34 3.24(2) 179.3 3 
O3 H3OA N4S  0.90 1.54 2.44(7) 176.0 . 
 
_diffrn_measured_fraction_theta_max    0.993 
_diffrn_reflns_theta_full              18.96 
_diffrn_measured_fraction_theta_full   0.993 
_refine_diff_density_max    0.954 
_refine_diff_density_min   -1.705 
_refine_diff_density_rms    0.151 
 
#===END