# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Sabiah Shahul Hameed'
_publ_contact_author_email       SABIAHS@GMAIL.COM

_publ_section_title              
;
Mononuclear [M(BP)2X]n+ (M = Cu2+, Co2+, Zn2+; X = OH2, Cl-)
Complexes with a New Biphenyl Appended N-bidendate Ligand: Structural,
Spectroscopic, Solution equilibrium and Ligand dynamic studies
;
loop_
_publ_author_name
'Sabiah Shahul Hameed'
'Narasimha. N Murthy'
'Babu Varghese'

#========================END

data_645339
_database_code_depnum_ccdc_archive 'CCDC 645339'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H37 Cl2 Cu N4 O4.50'
_chemical_formula_weight         780.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbca

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'
'-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                   9.342(2)
_cell_length_b                   21.1380(19)
_cell_length_c                   37.486(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7402(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      20
_cell_measurement_theta_max      30

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3232
_exptl_absorpt_coefficient_mu    2.554
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  0.7470
_exptl_absorpt_correction_T_max  0.9981
_exptl_absorpt_process_details   
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968)
Acta. Cryst. A24, 351
Number of psi-scan sets used was 2
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54180
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CAD4 diffractometer'
_diffrn_measurement_method       '\w-2\t scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         2
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  3600
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6723
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         2.36
_diffrn_reflns_theta_max         67.97
_reflns_number_total             6723
_reflns_number_gt                4847
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'cad4 programs'
_computing_cell_refinement       'cad4 programs'
_computing_data_reduction        'XCAD4 (WINGX)'
_computing_structure_solution    'SIR92 (WINGX)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP3 (WINGX)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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.

The perchlorate anion is disordered. This could be resolved as two sets
of near tetrahedral oxygens associaled with different chlorine atoms. For
all atoms of each set common site occupancy was assigned and the occupancies
were refined with sum of the occupancies of the two sets restrained as
one. As the two sets showed nearly equal occupancy(0.5 each), each set
was assigned occupancy of 0.5 during the last refinement job. Anisotropic
refinemnt was applied to perchlorate oxygens. The thermal ellipsoids are
reasonably good.

Water hydrogen were located in difference map and then geometrically
restrained during riding model refinement.The O-H bond distances were
restrained to be 0.90(1)A\%. H5A-H5B distance was restrained as
1.46(1)A\% to maintain tetrahedral bond angle. Free thermal parameter
refinement of water hydrogens showed one large and one small value.
Hence, the two hydrogen's thermal parameters were restrained to be
equal during refinemnt. However, the refined value is found to be
smaller than that of Ueq. of oxygen which is not physically meaningful
except that it minimises the least squares errors.

;

_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^)+(0.0980P)^2^+2.4841P] 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     SHELXL
_refine_ls_extinction_coef       0.00029(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         6723
_refine_ls_number_parameters     522
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0539
_refine_ls_wR_factor_ref         0.1624
_refine_ls_wR_factor_gt          0.1449
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_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
C1 C 0.1595(3) 0.06848(18) 0.68642(9) 0.0629(8) Uani 1 1 d . . .
H1A H 0.1127 0.0983 0.7022 0.076 Uiso 1 1 calc R . .
H1B H 0.0895 0.0549 0.6689 0.076 Uiso 1 1 calc R . .
C2 C 0.2053(3) 0.0120(2) 0.70784(8) 0.0670(9) Uani 1 1 d . . .
C3 C 0.1660(4) -0.0490(2) 0.69788(11) 0.0793(11) Uani 1 1 d . . .
H3 H 0.1158 -0.0551 0.6767 0.095 Uiso 1 1 calc R . .
C4 C 0.1997(5) -0.1005(2) 0.71858(13) 0.0989(14) Uani 1 1 d . . .
H4 H 0.1720 -0.1407 0.7112 0.119 Uiso 1 1 calc R . .
C5 C 0.2729(6) -0.0936(3) 0.74969(16) 0.1111(17) Uani 1 1 d . . .
H5 H 0.2965 -0.1288 0.7634 0.133 Uiso 1 1 calc R . .
C6 C 0.3115(5) -0.0340(3) 0.76069(11) 0.0999(16) Uani 1 1 d . . .
H6 H 0.3607 -0.0293 0.7821 0.120 Uiso 1 1 calc R . .
C7 C 0.2782(4) 0.0208(2) 0.74020(9) 0.0749(10) Uani 1 1 d . . .
C8 C 0.3189(4) 0.0845(2) 0.75156(9) 0.0767(11) Uani 1 1 d . . .
C9 C 0.2928(4) 0.1048(3) 0.78649(10) 0.0973(16) Uani 1 1 d . . .
H9 H 0.2528 0.0772 0.8030 0.117 Uiso 1 1 calc R . .
C10 C 0.3261(5) 0.1655(4) 0.79633(13) 0.117(2) Uani 1 1 d . . .
H10 H 0.3068 0.1783 0.8196 0.140 Uiso 1 1 calc R . .
C11 C 0.3871(6) 0.2080(3) 0.77317(15) 0.1122(18) Uani 1 1 d . . .
H11 H 0.4083 0.2489 0.7805 0.135 Uiso 1 1 calc R . .
C12 C 0.4168(4) 0.1884(2) 0.73800(11) 0.0852(12) Uani 1 1 d . . .
H12 H 0.4598 0.2161 0.7220 0.102 Uiso 1 1 calc R . .
C13 C 0.3818(4) 0.12781(19) 0.72745(9) 0.0675(9) Uani 1 1 d . . .
C14 C 0.4109(3) 0.10544(17) 0.68990(8) 0.0573(8) Uani 1 1 d . . .
H14A H 0.4794 0.1338 0.6788 0.069 Uiso 1 1 calc R . .
H14B H 0.4542 0.0638 0.6909 0.069 Uiso 1 1 calc R . .
C15 C 0.2320(4) 0.16672(16) 0.65795(9) 0.0627(8) Uani 1 1 d . . .
H15A H 0.3144 0.1927 0.6521 0.075 Uiso 1 1 calc R . .
H15B H 0.1844 0.1855 0.6784 0.075 Uiso 1 1 calc R . .
C16 C 0.1307(3) 0.16571(15) 0.62667(9) 0.0567(7) Uani 1 1 d . . .
C17 C 0.0277(4) 0.21124(17) 0.62100(11) 0.0726(10) Uani 1 1 d . . .
H17 H 0.0137 0.2436 0.6375 0.087 Uiso 1 1 calc R . .
C18 C -0.0543(4) 0.2080(2) 0.59042(12) 0.0801(11) Uani 1 1 d . . .
H18 H -0.1234 0.2387 0.5859 0.096 Uiso 1 1 calc R . .
C19 C -0.0334(4) 0.1597(2) 0.56688(11) 0.0768(10) Uani 1 1 d . . .
H19 H -0.0874 0.1571 0.5461 0.092 Uiso 1 1 calc R . .
C20 C 0.0686(4) 0.11484(19) 0.57444(9) 0.0689(9) Uani 1 1 d . . .
H20 H 0.0812 0.0811 0.5588 0.083 Uiso 1 1 calc R . .
C21 C 0.4617(3) 0.04358(13) 0.54513(7) 0.0477(6) Uani 1 1 d . . .
H21A H 0.4454 0.0026 0.5560 0.057 Uiso 1 1 calc R . .
H21B H 0.5585 0.0437 0.5358 0.057 Uiso 1 1 calc R . .
C22 C 0.3593(3) 0.05127(14) 0.51457(8) 0.0501(7) Uani 1 1 d . . .
C23 C 0.2471(4) 0.00869(18) 0.50946(9) 0.0653(9) Uani 1 1 d . . .
H23 H 0.2308 -0.0233 0.5260 0.078 Uiso 1 1 calc R . .
C24 C 0.1594(4) 0.0143(2) 0.47944(11) 0.0832(13) Uani 1 1 d . . .
H24 H 0.0850 -0.0143 0.4761 0.100 Uiso 1 1 calc R . .
C25 C 0.1818(4) 0.0615(2) 0.45482(11) 0.0816(12) Uani 1 1 d . . .
H25 H 0.1207 0.0659 0.4354 0.098 Uiso 1 1 calc R . .
C26 C 0.2942(4) 0.10186(19) 0.45918(9) 0.0692(9) Uani 1 1 d . . .
H26 H 0.3114 0.1327 0.4420 0.083 Uiso 1 1 calc R . .
C27 C 0.3844(3) 0.09801(15) 0.48898(8) 0.0522(7) Uani 1 1 d . . .
C28 C 0.5019(3) 0.14335(14) 0.49374(8) 0.0517(7) Uani 1 1 d . . .
C29 C 0.5940(4) 0.15899(17) 0.46587(9) 0.0698(9) Uani 1 1 d . . .
H29 H 0.5831 0.1397 0.4437 0.084 Uiso 1 1 calc R . .
C30 C 0.7018(5) 0.2032(2) 0.47093(11) 0.0843(12) Uani 1 1 d . . .
H30 H 0.7639 0.2127 0.4523 0.101 Uiso 1 1 calc R . .
C31 C 0.7175(4) 0.23278(19) 0.50286(11) 0.0787(11) Uani 1 1 d . . .
H31 H 0.7891 0.2629 0.5059 0.094 Uiso 1 1 calc R . .
C32 C 0.6274(4) 0.21828(15) 0.53085(9) 0.0618(8) Uani 1 1 d . . .
H32 H 0.6382 0.2390 0.5526 0.074 Uiso 1 1 calc R . .
C33 C 0.5210(3) 0.17306(13) 0.52695(8) 0.0488(6) Uani 1 1 d . . .
C34 C 0.4224(3) 0.15653(13) 0.55747(8) 0.0484(6) Uani 1 1 d . . .
H34A H 0.4319 0.1885 0.5759 0.058 Uiso 1 1 calc R . .
H34B H 0.3244 0.1576 0.5490 0.058 Uiso 1 1 calc R . .
C35 C 0.5885(3) 0.09475(14) 0.59334(8) 0.0508(7) Uani 1 1 d . . .
H35A H 0.5910 0.1316 0.6088 0.061 Uiso 1 1 calc R . .
H35B H 0.6673 0.0979 0.5766 0.061 Uiso 1 1 calc R . .
C36 C 0.6048(3) 0.03598(14) 0.61531(7) 0.0510(7) Uani 1 1 d . . .
C37 C 0.7355(4) 0.00903(16) 0.62294(9) 0.0607(8) Uani 1 1 d . . .
H37 H 0.8197 0.0276 0.6149 0.073 Uiso 1 1 calc R . .
C38 C 0.7394(5) -0.04614(17) 0.64279(9) 0.0736(10) Uani 1 1 d . . .
H38 H 0.8263 -0.0653 0.6482 0.088 Uiso 1 1 calc R . .
C39 C 0.6148(5) -0.07166(18) 0.65418(10) 0.0798(11) Uani 1 1 d . . .
H39 H 0.6160 -0.1087 0.6675 0.096 Uiso 1 1 calc R . .
C40 C 0.4868(5) -0.04333(16) 0.64622(9) 0.0721(10) Uani 1 1 d . . .
H40 H 0.4020 -0.0616 0.6542 0.087 Uiso 1 1 calc R . .
N1 N 0.2801(2) 0.10232(12) 0.66717(6) 0.0522(6) Uani 1 1 d . . .
N2 N 0.1504(3) 0.11856(13) 0.60375(7) 0.0568(6) Uani 1 1 d . . .
N3 N 0.4509(2) 0.09327(10) 0.57353(6) 0.0423(5) Uani 1 1 d . . .
N4 N 0.4819(3) 0.01058(12) 0.62704(7) 0.0575(6) Uani 1 1 d . . .
O5 O 0.2395(12) 0.3269(4) 0.6220(3) 0.154(3) Uani 0.50 1 d PD . .
Cl1 Cl 0.16362(11) -0.02928(4) 0.60124(2) 0.0744(3) Uani 1 1 d . . .
Cl2 Cl 0.6211(6) 0.2883(4) 0.64322(19) 0.0732(12) Uani 0.50 1 d PD A 1
O1 O 0.5229(18) 0.3203(9) 0.6629(5) 0.186(8) Uani 0.50 1 d PD A 1
O2 O 0.607(2) 0.3193(7) 0.6108(3) 0.181(8) Uani 0.50 1 d PD A 1
O3 O 0.568(3) 0.2271(6) 0.6426(6) 0.136(8) Uani 0.50 1 d PD A 1
O4 O 0.7548(9) 0.2915(4) 0.6585(3) 0.153(4) Uani 0.50 1 d PD A 1
Cl2' Cl 0.5765(6) 0.2880(4) 0.63695(19) 0.0801(14) Uani 0.50 1 d PD B 2
O1' O 0.585(2) 0.3221(6) 0.6683(3) 0.157(8) Uani 0.50 1 d PD B 2
O2' O 0.6730(18) 0.3124(6) 0.6122(3) 0.168(8) Uani 0.50 1 d PD B 2
O3' O 0.601(3) 0.2232(6) 0.6389(5) 0.116(6) Uani 0.50 1 d PD B 2
O4' O 0.4404(15) 0.2891(6) 0.6205(5) 0.241(7) Uani 0.50 1 d PD B 2
Cu Cu 0.30495(5) 0.05822(2) 0.615011(12) 0.05609(18) Uani 1 1 d . . .
H5A H 0.261(7) 0.3670(12) 0.6160(12) 0.056(13) Uiso 0.50 1 d PD . .
H5B H 0.232(8) 0.324(2) 0.6458(5) 0.056(13) Uiso 0.50 1 d PD . .

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
C1 0.0434(16) 0.093(2) 0.0528(17) 0.0056(16) 0.0046(13) 0.0001(16)
C2 0.0440(16) 0.105(3) 0.0521(17) 0.0147(18) 0.0060(14) -0.0003(18)
C3 0.066(2) 0.099(3) 0.072(2) 0.017(2) 0.0052(19) -0.018(2)
C4 0.097(3) 0.102(3) 0.097(3) 0.032(3) 0.001(3) -0.019(3)
C5 0.104(4) 0.115(4) 0.115(4) 0.048(3) 0.001(3) -0.013(3)
C6 0.075(3) 0.160(5) 0.065(2) 0.039(3) -0.005(2) 0.001(3)
C7 0.053(2) 0.120(3) 0.0523(18) 0.012(2) 0.0011(15) -0.002(2)
C8 0.0497(18) 0.131(3) 0.0499(17) 0.002(2) -0.0031(16) 0.015(2)
C9 0.064(2) 0.177(5) 0.051(2) -0.015(3) -0.0032(17) 0.019(3)
C10 0.076(3) 0.208(7) 0.066(3) -0.040(4) -0.008(2) 0.041(4)
C11 0.089(3) 0.144(5) 0.104(4) -0.051(3) -0.029(3) 0.032(3)
C12 0.077(3) 0.103(3) 0.076(2) -0.025(2) -0.017(2) 0.014(2)
C13 0.0455(17) 0.102(3) 0.0556(18) -0.0107(18) -0.0062(15) 0.0133(17)
C14 0.0436(16) 0.078(2) 0.0505(16) -0.0044(15) 0.0010(13) 0.0005(15)
C15 0.0574(19) 0.071(2) 0.0599(18) -0.0082(16) -0.0011(15) 0.0061(16)
C16 0.0445(16) 0.0645(19) 0.0612(18) 0.0077(15) 0.0044(14) 0.0033(14)
C17 0.068(2) 0.068(2) 0.082(2) 0.0049(18) 0.0017(19) 0.0122(18)
C18 0.060(2) 0.082(3) 0.099(3) 0.023(2) -0.011(2) 0.0116(19)
C19 0.0516(19) 0.106(3) 0.072(2) 0.015(2) -0.0069(17) 0.004(2)
C20 0.0502(18) 0.096(3) 0.0604(19) -0.0009(18) -0.0042(15) 0.0029(18)
C21 0.0521(16) 0.0420(14) 0.0492(15) -0.0051(11) 0.0053(13) 0.0022(12)
C22 0.0442(14) 0.0579(17) 0.0482(15) -0.0148(13) 0.0058(12) -0.0002(13)
C23 0.0549(17) 0.079(2) 0.0617(19) -0.0243(16) 0.0173(16) -0.0174(17)
C24 0.0456(18) 0.131(4) 0.073(2) -0.049(3) 0.0057(17) -0.020(2)
C25 0.061(2) 0.120(3) 0.064(2) -0.032(2) -0.0101(18) 0.006(2)
C26 0.066(2) 0.085(2) 0.0560(18) -0.0126(17) -0.0148(16) 0.0138(18)
C27 0.0495(16) 0.0605(17) 0.0467(15) -0.0090(13) -0.0008(13) 0.0049(14)
C28 0.0507(16) 0.0552(16) 0.0493(16) 0.0072(13) -0.0034(13) 0.0019(13)
C29 0.079(2) 0.076(2) 0.0540(18) 0.0131(16) 0.0041(17) -0.0006(19)
C30 0.087(3) 0.089(3) 0.077(3) 0.028(2) 0.016(2) -0.020(2)
C31 0.077(3) 0.077(3) 0.082(3) 0.020(2) -0.007(2) -0.028(2)
C32 0.062(2) 0.0574(18) 0.0655(19) 0.0115(15) -0.0101(16) -0.0100(15)
C33 0.0450(15) 0.0477(15) 0.0539(15) 0.0059(12) -0.0060(13) 0.0034(12)
C34 0.0484(15) 0.0466(15) 0.0503(15) -0.0031(12) -0.0033(13) 0.0025(12)
C35 0.0443(15) 0.0554(16) 0.0528(16) -0.0017(13) -0.0076(13) 0.0027(13)
C36 0.0555(17) 0.0541(16) 0.0435(15) -0.0065(12) -0.0040(13) 0.0075(14)
C37 0.0556(18) 0.068(2) 0.0582(17) -0.0105(15) -0.0110(15) 0.0131(16)
C38 0.080(3) 0.072(2) 0.069(2) -0.0077(18) -0.017(2) 0.029(2)
C39 0.107(3) 0.062(2) 0.070(2) 0.0126(18) -0.002(2) 0.022(2)
C40 0.083(3) 0.065(2) 0.069(2) 0.0121(17) 0.0069(19) 0.0123(19)
N1 0.0414(13) 0.0674(15) 0.0476(13) 0.0002(11) 0.0009(10) 0.0010(11)
N2 0.0433(13) 0.0738(17) 0.0533(14) 0.0004(13) 0.0006(11) 0.0055(12)
N3 0.0413(12) 0.0426(11) 0.0430(12) -0.0029(9) -0.0013(9) 0.0004(9)
N4 0.0620(16) 0.0579(14) 0.0526(13) 0.0043(12) 0.0066(13) 0.0107(13)
O5 0.147(8) 0.115(6) 0.201(9) 0.033(6) -0.051(8) -0.046(6)
Cl1 0.0801(6) 0.0775(6) 0.0655(5) 0.0032(4) -0.0040(4) -0.0227(5)
Cl2 0.082(3) 0.0592(17) 0.079(2) 0.0006(15) 0.0018(19) 0.010(2)
O1 0.154(11) 0.213(15) 0.191(14) -0.071(11) 0.054(10) 0.077(11)
O2 0.28(2) 0.163(10) 0.098(7) 0.082(8) -0.027(9) -0.026(11)
O3 0.166(13) 0.067(8) 0.175(14) 0.003(8) 0.020(9) -0.056(8)
O4 0.108(6) 0.099(5) 0.252(12) 0.019(6) -0.051(7) -0.024(5)
Cl2' 0.099(4) 0.0567(17) 0.084(3) -0.0041(18) 0.013(2) -0.003(3)
O1' 0.270(19) 0.108(8) 0.093(6) -0.047(6) 0.076(9) -0.087(10)
O2' 0.241(15) 0.125(8) 0.138(10) -0.056(7) 0.133(11) -0.080(9)
O3' 0.173(14) 0.075(8) 0.101(7) -0.018(6) -0.026(8) 0.011(7)
O4' 0.209(15) 0.182(11) 0.33(2) 0.036(12) -0.115(14) -0.033(10)
Cu 0.0479(3) 0.0650(3) 0.0553(3) 0.0008(2) 0.0027(2) 0.0064(2)

_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
C1 C2 1.501(5) . ?
C1 N1 1.517(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.392(6) . ?
C2 C7 1.404(5) . ?
C3 C4 1.373(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.360(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.374(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.423(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.464(6) . ?
C8 C9 1.399(5) . ?
C8 C13 1.414(5) . ?
C9 C10 1.370(8) . ?
C9 H9 0.9300 . ?
C10 C11 1.373(8) . ?
C10 H10 0.9300 . ?
C11 C12 1.410(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.379(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.510(4) . ?
C14 N1 1.492(4) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 N1 1.475(4) . ?
C15 C16 1.507(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 N2 1.328(4) . ?
C16 C17 1.377(5) . ?
C17 C18 1.380(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.364(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.374(5) . ?
C19 H19 0.9300 . ?
C20 N2 1.341(4) . ?
C20 H20 0.9300 . ?
C21 N3 1.499(3) . ?
C21 C22 1.501(4) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.394(4) . ?
C22 C27 1.397(4) . ?
C23 C24 1.397(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.376(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.362(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.402(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.468(4) . ?
C28 C29 1.393(4) . ?
C28 C33 1.406(4) . ?
C29 C30 1.388(5) . ?
C29 H29 0.9300 . ?
C30 C31 1.358(6) . ?
C30 H30 0.9300 . ?
C31 C32 1.379(5) . ?
C31 H31 0.9300 . ?
C32 C33 1.387(4) . ?
C32 H32 0.9300 . ?
C33 C34 1.509(4) . ?
C34 N3 1.490(3) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 N3 1.485(3) . ?
C35 C36 1.498(4) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 N4 1.341(4) . ?
C36 C37 1.378(4) . ?
C37 C38 1.384(5) . ?
C37 H37 0.9300 . ?
C38 C39 1.352(6) . ?
C38 H38 0.9300 . ?
C39 C40 1.370(6) . ?
C39 H39 0.9300 . ?
C40 N4 1.348(4) . ?
C40 H40 0.9300 . ?
N1 Cu 2.178(2) . ?
N2 Cu 1.972(3) . ?
N3 Cu 2.197(2) . ?
N4 Cu 1.988(3) . ?
O5 H5A 0.898(10) . ?
O5 H5B 0.896(10) . ?
Cl1 Cu 2.3304(10) . ?
Cl2 O1 1.357(11) . ?
Cl2 O4 1.376(9) . ?
Cl2 O3 1.385(10) . ?
Cl2 O2 1.386(9) . ?
Cl2' O1' 1.381(10) . ?
Cl2' O3' 1.391(12) . ?
Cl2' O2' 1.393(10) . ?
Cl2' O4' 1.413(11) . ?

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
C2 C1 N1 114.7(3) . . ?
C2 C1 H1A 108.6 . . ?
N1 C1 H1A 108.6 . . ?
C2 C1 H1B 108.6 . . ?
N1 C1 H1B 108.6 . . ?
H1A C1 H1B 107.6 . . ?
C3 C2 C7 118.8(4) . . ?
C3 C2 C1 121.2(3) . . ?
C7 C2 C1 119.7(4) . . ?
C4 C3 C2 121.5(4) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C5 C4 C3 121.0(5) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C5 C6 119.2(5) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C5 C6 C7 121.7(4) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 H6 119.1 . . ?
C2 C7 C6 117.7(4) . . ?
C2 C7 C8 119.9(4) . . ?
C6 C7 C8 122.3(4) . . ?
C9 C8 C13 118.2(5) . . ?
C9 C8 C7 120.6(4) . . ?
C13 C8 C7 121.2(3) . . ?
C10 C9 C8 119.9(5) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C9 C10 C11 122.4(5) . . ?
C9 C10 H10 118.8 . . ?
C11 C10 H10 118.8 . . ?
C10 C11 C12 118.7(5) . . ?
C10 C11 H11 120.6 . . ?
C12 C11 H11 120.6 . . ?
C13 C12 C11 119.7(5) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C12 C13 C8 121.0(4) . . ?
C12 C13 C14 121.0(4) . . ?
C8 C13 C14 117.9(3) . . ?
N1 C14 C13 113.5(2) . . ?
N1 C14 H14A 108.9 . . ?
C13 C14 H14A 108.9 . . ?
N1 C14 H14B 108.9 . . ?
C13 C14 H14B 108.9 . . ?
H14A C14 H14B 107.7 . . ?
N1 C15 C16 111.1(3) . . ?
N1 C15 H15A 109.4 . . ?
C16 C15 H15A 109.4 . . ?
N1 C15 H15B 109.4 . . ?
C16 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
N2 C16 C17 121.4(3) . . ?
N2 C16 C15 115.3(3) . . ?
C17 C16 C15 123.3(3) . . ?
C16 C17 C18 118.8(4) . . ?
C16 C17 H17 120.6 . . ?
C18 C17 H17 120.6 . . ?
C19 C18 C17 119.7(4) . . ?
C19 C18 H18 120.2 . . ?
C17 C18 H18 120.2 . . ?
C18 C19 C20 118.9(4) . . ?
C18 C19 H19 120.6 . . ?
C20 C19 H19 120.6 . . ?
N2 C20 C19 121.6(4) . . ?
N2 C20 H20 119.2 . . ?
C19 C20 H20 119.2 . . ?
N3 C21 C22 115.0(2) . . ?
N3 C21 H21A 108.5 . . ?
C22 C21 H21A 108.5 . . ?
N3 C21 H21B 108.5 . . ?
C22 C21 H21B 108.5 . . ?
H21A C21 H21B 107.5 . . ?
C23 C22 C27 119.2(3) . . ?
C23 C22 C21 120.9(3) . . ?
C27 C22 C21 119.6(3) . . ?
C22 C23 C24 119.8(4) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
C25 C24 C23 120.8(3) . . ?
C25 C24 H24 119.6 . . ?
C23 C24 H24 119.6 . . ?
C26 C25 C24 119.4(4) . . ?
C26 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
C25 C26 C27 121.5(4) . . ?
C25 C26 H26 119.3 . . ?
C27 C26 H26 119.3 . . ?
C22 C27 C26 119.2(3) . . ?
C22 C27 C28 120.2(3) . . ?
C26 C27 C28 120.6(3) . . ?
C29 C28 C33 118.7(3) . . ?
C29 C28 C27 121.7(3) . . ?
C33 C28 C27 119.6(3) . . ?
C30 C29 C28 120.4(3) . . ?
C30 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
C31 C30 C29 120.6(4) . . ?
C31 C30 H30 119.7 . . ?
C29 C30 H30 119.7 . . ?
C30 C31 C32 120.2(3) . . ?
C30 C31 H31 119.9 . . ?
C32 C31 H31 119.9 . . ?
C31 C32 C33 120.7(3) . . ?
C31 C32 H32 119.7 . . ?
C33 C32 H32 119.7 . . ?
C32 C33 C28 119.5(3) . . ?
C32 C33 C34 121.1(3) . . ?
C28 C33 C34 119.4(3) . . ?
N3 C34 C33 113.9(2) . . ?
N3 C34 H34A 108.8 . . ?
C33 C34 H34A 108.8 . . ?
N3 C34 H34B 108.8 . . ?
C33 C34 H34B 108.8 . . ?
H34A C34 H34B 107.7 . . ?
N3 C35 C36 110.2(2) . . ?
N3 C35 H35A 109.6 . . ?
C36 C35 H35A 109.6 . . ?
N3 C35 H35B 109.6 . . ?
C36 C35 H35B 109.6 . . ?
H35A C35 H35B 108.1 . . ?
N4 C36 C37 121.7(3) . . ?
N4 C36 C35 115.2(3) . . ?
C37 C36 C35 123.2(3) . . ?
C36 C37 C38 118.9(4) . . ?
C36 C37 H37 120.5 . . ?
C38 C37 H37 120.5 . . ?
C39 C38 C37 118.9(4) . . ?
C39 C38 H38 120.5 . . ?
C37 C38 H38 120.5 . . ?
C38 C39 C40 120.5(3) . . ?
C38 C39 H39 119.7 . . ?
C40 C39 H39 119.7 . . ?
N4 C40 C39 121.0(4) . . ?
N4 C40 H40 119.5 . . ?
C39 C40 H40 119.5 . . ?
C15 N1 C14 110.0(2) . . ?
C15 N1 C1 108.7(2) . . ?
C14 N1 C1 110.9(2) . . ?
C15 N1 Cu 102.54(18) . . ?
C14 N1 Cu 116.38(17) . . ?
C1 N1 Cu 107.72(19) . . ?
C16 N2 C20 119.7(3) . . ?
C16 N2 Cu 116.6(2) . . ?
C20 N2 Cu 123.7(2) . . ?
C35 N3 C34 109.7(2) . . ?
C35 N3 C21 108.2(2) . . ?
C34 N3 C21 110.7(2) . . ?
C35 N3 Cu 100.97(16) . . ?
C34 N3 Cu 118.55(17) . . ?
C21 N3 Cu 107.95(16) . . ?
C36 N4 C40 119.0(3) . . ?
C36 N4 Cu 115.76(19) . . ?
C40 N4 Cu 125.3(3) . . ?
H5A O5 H5B 108.8(17) . . ?
O1 Cl2 O4 111.3(10) . . ?
O1 Cl2 O3 103.5(15) . . ?
O4 Cl2 O3 112.1(11) . . ?
O1 Cl2 O2 100.2(13) . . ?
O4 Cl2 O2 115.2(11) . . ?
O3 Cl2 O2 113.2(13) . . ?
O1' Cl2' O3' 117.4(11) . . ?
O1' Cl2' O2' 109.6(9) . . ?
O3' Cl2' O2' 107.1(13) . . ?
O1' Cl2' O4' 114.7(11) . . ?
O3' Cl2' O4' 100.7(11) . . ?
O2' Cl2' O4' 106.6(11) . . ?
N2 Cu N4 170.11(12) . . ?
N2 Cu N1 80.63(10) . . ?
N4 Cu N1 95.85(10) . . ?
N2 Cu N3 94.87(10) . . ?
N4 Cu N3 79.35(10) . . ?
N1 Cu N3 123.86(9) . . ?
N2 Cu Cl1 92.93(9) . . ?
N4 Cu Cl1 96.86(9) . . ?
N1 Cu Cl1 118.55(7) . . ?
N3 Cu Cl1 117.55(6) . . ?

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
N1 C1 C2 C3 -111.8(4) . . . . ?
N1 C1 C2 C7 73.9(4) . . . . ?
C7 C2 C3 C4 -1.4(6) . . . . ?
C1 C2 C3 C4 -175.8(4) . . . . ?
C2 C3 C4 C5 0.0(7) . . . . ?
C3 C4 C5 C6 1.0(8) . . . . ?
C4 C5 C6 C7 -0.6(8) . . . . ?
C3 C2 C7 C6 1.7(5) . . . . ?
C1 C2 C7 C6 176.1(3) . . . . ?
C3 C2 C7 C8 -179.1(3) . . . . ?
C1 C2 C7 C8 -4.7(5) . . . . ?
C5 C6 C7 C2 -0.7(6) . . . . ?
C5 C6 C7 C8 -179.9(4) . . . . ?
C2 C7 C8 C9 133.2(4) . . . . ?
C6 C7 C8 C9 -47.7(5) . . . . ?
C2 C7 C8 C13 -45.0(5) . . . . ?
C6 C7 C8 C13 134.1(4) . . . . ?
C13 C8 C9 C10 0.9(6) . . . . ?
C7 C8 C9 C10 -177.3(4) . . . . ?
C8 C9 C10 C11 -0.9(7) . . . . ?
C9 C10 C11 C12 -0.2(7) . . . . ?
C10 C11 C12 C13 1.3(7) . . . . ?
C11 C12 C13 C8 -1.3(6) . . . . ?
C11 C12 C13 C14 179.5(3) . . . . ?
C9 C8 C13 C12 0.2(5) . . . . ?
C7 C8 C13 C12 178.4(3) . . . . ?
C9 C8 C13 C14 179.4(3) . . . . ?
C7 C8 C13 C14 -2.3(5) . . . . ?
C12 C13 C14 N1 -104.3(4) . . . . ?
C8 C13 C14 N1 76.4(4) . . . . ?
N1 C15 C16 N2 -29.1(4) . . . . ?
N1 C15 C16 C17 153.2(3) . . . . ?
N2 C16 C17 C18 -1.3(5) . . . . ?
C15 C16 C17 C18 176.3(3) . . . . ?
C16 C17 C18 C19 1.0(6) . . . . ?
C17 C18 C19 C20 0.5(6) . . . . ?
C18 C19 C20 N2 -1.9(6) . . . . ?
N3 C21 C22 C23 -111.3(3) . . . . ?
N3 C21 C22 C27 74.9(3) . . . . ?
C27 C22 C23 C24 -1.6(5) . . . . ?
C21 C22 C23 C24 -175.5(3) . . . . ?
C22 C23 C24 C25 -0.3(5) . . . . ?
C23 C24 C25 C26 2.4(6) . . . . ?
C24 C25 C26 C27 -2.6(5) . . . . ?
C23 C22 C27 C26 1.4(4) . . . . ?
C21 C22 C27 C26 175.4(3) . . . . ?
C23 C22 C27 C28 -179.9(3) . . . . ?
C21 C22 C27 C28 -6.0(4) . . . . ?
C25 C26 C27 C22 0.7(5) . . . . ?
C25 C26 C27 C28 -177.9(3) . . . . ?
C22 C27 C28 C29 135.2(3) . . . . ?
C26 C27 C28 C29 -46.2(4) . . . . ?
C22 C27 C28 C33 -46.2(4) . . . . ?
C26 C27 C28 C33 132.4(3) . . . . ?
C33 C28 C29 C30 -0.3(5) . . . . ?
C27 C28 C29 C30 178.3(3) . . . . ?
C28 C29 C30 C31 -1.2(6) . . . . ?
C29 C30 C31 C32 1.0(6) . . . . ?
C30 C31 C32 C33 0.7(6) . . . . ?
C31 C32 C33 C28 -2.2(5) . . . . ?
C31 C32 C33 C34 179.6(3) . . . . ?
C29 C28 C33 C32 1.9(4) . . . . ?
C27 C28 C33 C32 -176.7(3) . . . . ?
C29 C28 C33 C34 -179.8(3) . . . . ?
C27 C28 C33 C34 1.6(4) . . . . ?
C32 C33 C34 N3 -107.7(3) . . . . ?
C28 C33 C34 N3 74.0(3) . . . . ?
N3 C35 C36 N4 -30.5(3) . . . . ?
N3 C35 C36 C37 149.0(3) . . . . ?
N4 C36 C37 C38 0.9(5) . . . . ?
C35 C36 C37 C38 -178.5(3) . . . . ?
C36 C37 C38 C39 -0.3(5) . . . . ?
C37 C38 C39 C40 -0.1(6) . . . . ?
C38 C39 C40 N4 -0.3(6) . . . . ?
C16 C15 N1 C14 162.6(3) . . . . ?
C16 C15 N1 C1 -75.7(3) . . . . ?
C16 C15 N1 Cu 38.2(3) . . . . ?
C13 C14 N1 C15 72.3(3) . . . . ?
C13 C14 N1 C1 -48.1(4) . . . . ?
C13 C14 N1 Cu -171.7(2) . . . . ?
C2 C1 N1 C15 -160.8(3) . . . . ?
C2 C1 N1 C14 -39.6(4) . . . . ?
C2 C1 N1 Cu 88.8(3) . . . . ?
C17 C16 N2 C20 -0.1(5) . . . . ?
C15 C16 N2 C20 -177.8(3) . . . . ?
C17 C16 N2 Cu 178.6(3) . . . . ?
C15 C16 N2 Cu 0.9(4) . . . . ?
C19 C20 N2 C16 1.7(5) . . . . ?
C19 C20 N2 Cu -176.9(3) . . . . ?
C36 C35 N3 C34 169.1(2) . . . . ?
C36 C35 N3 C21 -70.0(3) . . . . ?
C36 C35 N3 Cu 43.2(2) . . . . ?
C33 C34 N3 C35 70.3(3) . . . . ?
C33 C34 N3 C21 -49.1(3) . . . . ?
C33 C34 N3 Cu -174.57(18) . . . . ?
C22 C21 N3 C35 -158.2(2) . . . . ?
C22 C21 N3 C34 -37.9(3) . . . . ?
C22 C21 N3 Cu 93.4(2) . . . . ?
C37 C36 N4 C40 -1.2(4) . . . . ?
C35 C36 N4 C40 178.3(3) . . . . ?
C37 C36 N4 Cu 177.5(2) . . . . ?
C35 C36 N4 Cu -2.9(3) . . . . ?
C39 C40 N4 C36 0.9(5) . . . . ?
C39 C40 N4 Cu -177.8(3) . . . . ?
C16 N2 Cu N4 -52.7(7) . . . . ?
C20 N2 Cu N4 125.9(6) . . . . ?
C16 N2 Cu N1 17.1(2) . . . . ?
C20 N2 Cu N1 -164.3(3) . . . . ?
C16 N2 Cu N3 -106.5(2) . . . . ?
C20 N2 Cu N3 72.2(3) . . . . ?
C16 N2 Cu Cl1 135.5(2) . . . . ?
C20 N2 Cu Cl1 -45.8(3) . . . . ?
C36 N4 Cu N2 -32.4(7) . . . . ?
C40 N4 Cu N2 146.3(6) . . . . ?
C36 N4 Cu N1 -100.9(2) . . . . ?
C40 N4 Cu N1 77.8(3) . . . . ?
C36 N4 Cu N3 22.5(2) . . . . ?
C40 N4 Cu N3 -158.8(3) . . . . ?
C36 N4 Cu Cl1 139.3(2) . . . . ?
C40 N4 Cu Cl1 -42.0(3) . . . . ?
C15 N1 Cu N2 -29.90(19) . . . . ?
C14 N1 Cu N2 -150.1(2) . . . . ?
C1 N1 Cu N2 84.7(2) . . . . ?
C15 N1 Cu N4 140.77(19) . . . . ?
C14 N1 Cu N4 20.6(2) . . . . ?
C1 N1 Cu N4 -104.6(2) . . . . ?
C15 N1 Cu N3 59.7(2) . . . . ?
C14 N1 Cu N3 -60.5(2) . . . . ?
C1 N1 Cu N3 174.27(17) . . . . ?
C15 N1 Cu Cl1 -118.14(18) . . . . ?
C14 N1 Cu Cl1 121.7(2) . . . . ?
C1 N1 Cu Cl1 -3.6(2) . . . . ?
C35 N3 Cu N2 136.63(17) . . . . ?
C34 N3 Cu N2 16.8(2) . . . . ?
C21 N3 Cu N2 -110.01(18) . . . . ?
C35 N3 Cu N4 -35.27(17) . . . . ?
C34 N3 Cu N4 -155.1(2) . . . . ?
C21 N3 Cu N4 78.09(18) . . . . ?
C35 N3 Cu N1 54.65(19) . . . . ?
C34 N3 Cu N1 -65.2(2) . . . . ?
C21 N3 Cu N1 168.02(16) . . . . ?
C35 N3 Cu Cl1 -127.50(14) . . . . ?
C34 N3 Cu Cl1 112.70(17) . . . . ?
C21 N3 Cu Cl1 -14.14(18) . . . . ?

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
O5 H5A Cl1 0.898(10) 2.369(15) 3.266(8) 176(6) 7_665

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        67.97
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.070
_vrf_PLAT242_3chloro             
;
PROBLEM: Check Low Ueq as Compared to Neighbors for Cl2
RESPONSE: The chlorine atoms must be at the libration center
and hence not affeted by libration motion while the clorine
atoms suffer from thermal libration as they are not at center.
;
# end Validation Reply Form

#========================END


# Attachment 'B910519K_revised.cif'

data_645340
_database_code_depnum_ccdc_archive 'CCDC 645340'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H38 Cl2 N4 O9 Zn'
_chemical_formula_weight         855.01

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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                   22.156(5)
_cell_length_b                   9.8328(17)
_cell_length_c                   20.202(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.408(13)
_cell_angle_gamma                90.00
_cell_volume                     3975.4(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      10
_cell_measurement_theta_max      15

_exptl_crystal_description       needle
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1768
_exptl_absorpt_coefficient_mu    0.812
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_process_details   
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was 3
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;
_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  'cad4 diffractometer'
_diffrn_measurement_method       '\w-2\t scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         2
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  3600
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6164
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.04
_diffrn_reflns_theta_max         24.98
_reflns_number_total             3496
_reflns_number_gt                2409
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'cad4 programs'
_computing_cell_refinement       'cad4 programs'
_computing_data_reduction        'xcad4 (wingx)'
_computing_structure_solution    'sir92 (wingx)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ortep3 (wingx)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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.
The perchlorate anion is disordered. This could be resolved as two sets
of near tetrahedral oxygens associaled with same chlorine. For all atoms of
each set common site occupancy was assigned and the occupancies were refined
with sum of the occupancies of the two sets restrained as one. As the two
sets showed nearly equal occupancy(0.5 each), each set was assigned
occupancy of 0.5 during the last refinement job. The anisotropic thermal
ellipsoisds of perchlorate oxygens show large eccentricities. The disorder
resolved as two sets may be thought only as an approximation to true
situation in the lattice. The true disorder fixing may need several
sets which is practically not feasible. The anisotropic refinement was
preferred for perchlorate oxygens because it cleanses a fairly good amount
of unaccounted electron density (around the perchlorate)in the difference
map( it may not be truely representing the correct thermal motion).

Coordinating water oxygen stays on the two-fold axis. Water hydrogen
were located in difference map and then geometrically restrained
during riding model refinement. The isotropic thermal parameter
was refined.
;

_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^)+(0.0652P)^2^+14.5152P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3496
_refine_ls_number_parameters     291
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0613
_refine_ls_wR_factor_ref         0.1737
_refine_ls_wR_factor_gt          0.1454
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.089
_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
C1 C 0.4895(3) 0.0433(6) 0.3935(3) 0.0686(14) Uani 1 1 d . . .
H1A H 0.5202 0.1169 0.3981 0.082 Uiso 1 1 calc R . .
H1B H 0.5051 -0.0010 0.4409 0.082 Uiso 1 1 calc R . .
C2 C 0.4214(3) 0.1024(7) 0.3744(4) 0.0799(18) Uani 1 1 d . . .
C3 C 0.4095(3) 0.2381(7) 0.3559(5) 0.106(3) Uani 1 1 d . . .
H3 H 0.4431 0.2917 0.3536 0.128 Uiso 1 1 calc R . .
C4 C 0.3474(4) 0.2953(9) 0.3408(6) 0.138(4) Uani 1 1 d . . .
H4 H 0.3398 0.3872 0.3291 0.166 Uiso 1 1 calc R . .
C5 C 0.2973(4) 0.2154(11) 0.3432(7) 0.149(4) Uani 1 1 d . . .
H5 H 0.2552 0.2524 0.3311 0.179 Uiso 1 1 calc R . .
C6 C 0.3091(4) 0.0833(10) 0.3629(5) 0.123(3) Uani 1 1 d . . .
H6 H 0.2752 0.0314 0.3659 0.147 Uiso 1 1 calc R . .
C7 C 0.3708(3) 0.0227(7) 0.3791(4) 0.084(2) Uani 1 1 d . . .
C8 C 0.3847(3) -0.1197(8) 0.4033(3) 0.0805(19) Uani 1 1 d . . .
C9 C 0.3663(4) -0.1724(11) 0.4573(4) 0.110(3) Uani 1 1 d . . .
H9 H 0.3429 -0.1180 0.4759 0.132 Uiso 1 1 calc R . .
C10 C 0.3825(4) -0.3020(13) 0.4820(4) 0.121(4) Uani 1 1 d . . .
H10 H 0.3699 -0.3351 0.5174 0.145 Uiso 1 1 calc R . .
C11 C 0.4171(4) -0.3847(10) 0.4558(4) 0.110(3) Uani 1 1 d . . .
H11 H 0.4290 -0.4722 0.4743 0.132 Uiso 1 1 calc R . .
C12 C 0.4345(3) -0.3376(7) 0.4018(4) 0.0875(19) Uani 1 1 d . . .
H12 H 0.4569 -0.3942 0.3828 0.105 Uiso 1 1 calc R . .
C13 C 0.4184(3) -0.2063(6) 0.3760(3) 0.0679(15) Uani 1 1 d . . .
C14 C 0.4334(3) -0.1526(5) 0.3144(3) 0.0612(13) Uani 1 1 d . . .
H14A H 0.4419 -0.2291 0.2892 0.073 Uiso 1 1 calc R . .
H14B H 0.3942 -0.1057 0.2794 0.073 Uiso 1 1 calc R . .
C15 C 0.5551(3) -0.1351(6) 0.3736(3) 0.0668(14) Uani 1 1 d . . .
H15A H 0.5514 -0.2177 0.3458 0.080 Uiso 1 1 calc R . .
H15B H 0.5624 -0.1610 0.4227 0.080 Uiso 1 1 calc R . .
C16 C 0.6142(2) -0.0547(6) 0.3774(3) 0.0609(13) Uani 1 1 d . . .
C17 C 0.6786(3) -0.0807(7) 0.4294(3) 0.0823(18) Uani 1 1 d . . .
H17 H 0.6864 -0.1453 0.4659 0.099 Uiso 1 1 calc R . .
C18 C 0.7308(3) -0.0090(8) 0.4263(4) 0.092(2) Uani 1 1 d . . .
H18 H 0.7746 -0.0264 0.4599 0.110 Uiso 1 1 calc R . .
C19 C 0.7177(3) 0.0878(7) 0.3732(4) 0.093(2) Uani 1 1 d . . .
H19 H 0.7524 0.1373 0.3705 0.112 Uiso 1 1 calc R . .
C20 C 0.6531(3) 0.1107(6) 0.3244(4) 0.0804(17) Uani 1 1 d . . .
H20 H 0.6442 0.1772 0.2887 0.096 Uiso 1 1 calc R . .
N1 N 0.49179(18) -0.0577(4) 0.3387(2) 0.0550(10) Uani 1 1 d . . .
N2 N 0.60190(19) 0.0397(5) 0.3264(2) 0.0617(11) Uani 1 1 d . . .
O1 O 0.5000 0.2534(6) 0.2500 0.099(2) Uani 1 2 d S . .
H1 H 0.4649 0.2812 0.2174 0.15(4) Uiso 1 1 calc R . .
Zn Zn 0.5000 0.04887(8) 0.2500 0.0557(3) Uani 1 2 d S . .
Cl1 Cl 0.62177(9) 0.51496(18) 0.34950(12) 0.0993(6) Uani 1 1 d D . .
O2 O 0.6722(7) 0.4160(12) 0.3687(8) 0.202(10) Uani 0.50 1 d PD A 1
O3 O 0.6059(9) 0.5716(15) 0.2862(5) 0.35(2) Uani 0.50 1 d PD A 1
O4 O 0.6417(6) 0.5988(9) 0.4102(5) 0.174(9) Uani 0.50 1 d PD A 1
O5 O 0.5678(6) 0.4376(16) 0.3498(6) 0.157(6) Uani 0.50 1 d PD A 1
O2' O 0.6089(9) 0.4073(14) 0.3032(11) 0.37(2) Uani 0.50 1 d PD A 2
O3' O 0.6375(6) 0.6281(10) 0.3187(7) 0.127(4) Uani 0.50 1 d PD A 2
O4' O 0.6798(5) 0.486(2) 0.4124(7) 0.39(3) Uani 0.50 1 d PD A 2
O5' O 0.5708(8) 0.5462(14) 0.3658(13) 0.39(3) Uani 0.50 1 d PD 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
C1 0.059(3) 0.080(4) 0.071(3) -0.029(3) 0.031(3) -0.016(3)
C2 0.067(4) 0.079(4) 0.098(5) -0.047(4) 0.039(3) -0.012(3)
C3 0.085(4) 0.090(5) 0.154(7) -0.057(5) 0.062(5) -0.009(4)
C4 0.111(6) 0.092(6) 0.220(10) -0.058(6) 0.078(7) 0.012(5)
C5 0.080(5) 0.127(8) 0.245(12) -0.078(8) 0.073(7) 0.007(5)
C6 0.079(5) 0.130(7) 0.179(9) -0.066(7) 0.075(5) -0.018(5)
C7 0.065(4) 0.099(5) 0.101(5) -0.047(4) 0.046(3) -0.018(3)
C8 0.059(3) 0.116(5) 0.070(4) -0.034(4) 0.031(3) -0.032(4)
C9 0.086(5) 0.172(9) 0.087(5) -0.054(6) 0.051(4) -0.067(6)
C10 0.104(6) 0.186(10) 0.071(5) -0.017(6) 0.035(4) -0.081(7)
C11 0.092(5) 0.136(7) 0.084(5) 0.022(5) 0.019(4) -0.046(5)
C12 0.079(4) 0.092(5) 0.087(4) 0.008(4) 0.031(4) -0.018(4)
C13 0.059(3) 0.083(4) 0.061(3) -0.014(3) 0.024(3) -0.020(3)
C14 0.064(3) 0.060(3) 0.060(3) -0.013(3) 0.027(2) -0.011(3)
C15 0.065(3) 0.071(4) 0.064(3) 0.009(3) 0.026(3) 0.011(3)
C16 0.052(3) 0.064(3) 0.060(3) -0.015(3) 0.018(2) 0.009(3)
C17 0.068(4) 0.084(4) 0.077(4) -0.008(3) 0.014(3) 0.018(3)
C18 0.046(3) 0.106(5) 0.098(5) -0.021(4) 0.007(3) 0.004(3)
C19 0.052(3) 0.090(5) 0.121(6) -0.017(4) 0.022(4) -0.011(3)
C20 0.055(3) 0.077(4) 0.096(4) -0.005(3) 0.020(3) -0.013(3)
N1 0.050(2) 0.056(2) 0.058(2) -0.013(2) 0.0228(19) -0.0031(19)
N2 0.046(2) 0.062(3) 0.071(3) -0.003(2) 0.019(2) -0.001(2)
O1 0.071(4) 0.056(3) 0.151(6) 0.000 0.030(5) 0.000
Zn 0.0432(4) 0.0519(5) 0.0674(6) 0.000 0.0194(4) 0.000
Cl1 0.0831(11) 0.0752(11) 0.1251(16) 0.0043(11) 0.0309(11) -0.0084(9)
O2 0.37(3) 0.086(9) 0.188(17) 0.060(10) 0.156(19) 0.123(14)
O3 0.61(5) 0.162(18) 0.087(10) 0.052(12) -0.036(18) -0.12(2)
O4 0.136(11) 0.061(6) 0.168(12) -0.020(7) -0.084(10) 0.007(6)
O5 0.131(10) 0.231(17) 0.100(8) -0.032(10) 0.040(7) -0.092(12)
O2' 0.157(17) 0.182(19) 0.71(6) -0.27(3) 0.11(3) -0.030(14)
O3' 0.152(11) 0.098(9) 0.145(12) 0.037(8) 0.078(10) 0.010(8)
O4' 0.083(10) 0.85(7) 0.151(16) 0.22(3) -0.018(10) -0.10(2)
O5' 0.37(3) 0.094(11) 0.95(8) -0.03(2) 0.53(5) 0.003(16)

_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
C1 N1 1.503(6) . ?
C1 C2 1.503(8) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.380(10) . ?
C2 C7 1.404(8) . ?
C3 C4 1.394(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.378(12) . ?
C4 H4 0.9300 . ?
C5 C6 1.351(13) . ?
C5 H5 0.9300 . ?
C6 C7 1.397(10) . ?
C6 H6 0.9300 . ?
C7 C8 1.471(10) . ?
C8 C13 1.394(8) . ?
C8 C9 1.415(10) . ?
C9 C10 1.360(12) . ?
C9 H9 0.9300 . ?
C10 C11 1.370(12) . ?
C10 H10 0.9300 . ?
C11 C12 1.384(10) . ?
C11 H11 0.9300 . ?
C12 C13 1.380(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.514(7) . ?
C14 N1 1.497(6) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 N1 1.482(6) . ?
C15 C16 1.502(7) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 N2 1.326(7) . ?
C16 C17 1.385(7) . ?
C17 C18 1.380(9) . ?
C17 H17 0.9300 . ?
C18 C19 1.368(10) . ?
C18 H18 0.9300 . ?
C19 C20 1.364(8) . ?
C19 H19 0.9300 . ?
C20 N2 1.347(7) . ?
C20 H20 0.9300 . ?
N1 Zn 2.151(4) . ?
N2 Zn 2.121(4) . ?
O1 Zn 2.012(6) . ?
O1 H1 0.8200 . ?
Zn N2 2.121(4) 2_655 ?
Zn N1 2.151(4) 2_655 ?
Cl1 O3 1.296(7) . ?
Cl1 O5' 1.341(7) . ?
Cl1 O2' 1.359(8) . ?
Cl1 O4 1.383(7) . ?
Cl1 O3' 1.390(7) . ?
Cl1 O4' 1.394(8) . ?
Cl1 O2 1.405(7) . ?
Cl1 O5 1.419(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 114.4(4) . . ?
N1 C1 H1A 108.7 . . ?
C2 C1 H1A 108.7 . . ?
N1 C1 H1B 108.7 . . ?
C2 C1 H1B 108.7 . . ?
H1A C1 H1B 107.6 . . ?
C3 C2 C7 119.4(6) . . ?
C3 C2 C1 119.9(6) . . ?
C7 C2 C1 120.6(6) . . ?
C2 C3 C4 120.4(7) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C5 C4 C3 119.7(8) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C6 C5 C4 120.2(8) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C7 121.7(8) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C6 C7 C2 118.5(7) . . ?
C6 C7 C8 121.9(7) . . ?
C2 C7 C8 119.6(6) . . ?
C13 C8 C9 117.5(8) . . ?
C13 C8 C7 121.4(6) . . ?
C9 C8 C7 121.1(7) . . ?
C10 C9 C8 120.6(8) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C11 121.1(8) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C10 C11 C12 119.8(9) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C13 C12 C11 119.8(8) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C12 C13 C8 121.2(6) . . ?
C12 C13 C14 121.6(6) . . ?
C8 C13 C14 117.2(6) . . ?
N1 C14 C13 114.2(4) . . ?
N1 C14 H14A 108.7 . . ?
C13 C14 H14A 108.7 . . ?
N1 C14 H14B 108.7 . . ?
C13 C14 H14B 108.7 . . ?
H14A C14 H14B 107.6 . . ?
N1 C15 C16 112.4(4) . . ?
N1 C15 H15A 109.1 . . ?
C16 C15 H15A 109.1 . . ?
N1 C15 H15B 109.1 . . ?
C16 C15 H15B 109.1 . . ?
H15A C15 H15B 107.9 . . ?
N2 C16 C17 121.3(5) . . ?
N2 C16 C15 116.4(4) . . ?
C17 C16 C15 122.2(6) . . ?
C18 C17 C16 118.8(6) . . ?
C18 C17 H17 120.6 . . ?
C16 C17 H17 120.6 . . ?
C19 C18 C17 119.4(6) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C20 C19 C18 119.0(6) . . ?
C20 C19 H19 120.5 . . ?
C18 C19 H19 120.5 . . ?
N2 C20 C19 121.9(6) . . ?
N2 C20 H20 119.0 . . ?
C19 C20 H20 119.0 . . ?
C15 N1 C14 110.2(4) . . ?
C15 N1 C1 108.3(4) . . ?
C14 N1 C1 110.9(4) . . ?
C15 N1 Zn 104.1(3) . . ?
C14 N1 Zn 113.6(3) . . ?
C1 N1 Zn 109.5(3) . . ?
C16 N2 C20 119.4(5) . . ?
C16 N2 Zn 113.3(3) . . ?
C20 N2 Zn 127.1(4) . . ?
Zn O1 H1 109.5 . . ?
O1 Zn N2 92.43(12) . . ?
O1 Zn N2 92.43(12) . 2_655 ?
N2 Zn N2 175.1(2) . 2_655 ?
O1 Zn N1 119.16(10) . 2_655 ?
N2 Zn N1 98.16(15) . 2_655 ?
N2 Zn N1 79.45(16) 2_655 2_655 ?
O1 Zn N1 119.16(10) . . ?
N2 Zn N1 79.45(16) . . ?
N2 Zn N1 98.16(15) 2_655 . ?
N1 Zn N1 121.7(2) 2_655 . ?
O3 Cl1 O5' 104.0(12) . . ?
O3 Cl1 O2' 76.6(10) . . ?
O5' Cl1 O2' 113.4(7) . . ?
O3 Cl1 O4 117.8(7) . . ?
O5' Cl1 O4 68.1(9) . . ?
O2' Cl1 O4 165.2(10) . . ?
O3 Cl1 O3' 39.6(7) . . ?
O5' Cl1 O3' 109.0(6) . . ?
O2' Cl1 O3' 109.5(8) . . ?
O4 Cl1 O3' 82.8(7) . . ?
O3 Cl1 O4' 137.7(10) . . ?
O5' Cl1 O4' 111.5(8) . . ?
O2' Cl1 O4' 108.0(8) . . ?
O4 Cl1 O4' 59.6(10) . . ?
O3' Cl1 O4' 105.1(7) . . ?
O3 Cl1 O2 114.6(8) . . ?
O5' Cl1 O2 138.2(9) . . ?
O2' Cl1 O2 63.7(9) . . ?
O4 Cl1 O2 104.8(6) . . ?
O3' Cl1 O2 110.8(8) . . ?
O4' Cl1 O2 45.2(10) . . ?
O3 Cl1 O5 111.2(7) . . ?
O5' Cl1 O5 47.3(7) . . ?
O2' Cl1 O5 70.0(8) . . ?
O4 Cl1 O5 105.3(6) . . ?
O3' Cl1 O5 143.5(8) . . ?
O4' Cl1 O5 109.7(8) . . ?
O2 Cl1 O5 101.5(6) . . ?

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
N1 C1 C2 C3 -112.1(7) . . . . ?
N1 C1 C2 C7 71.6(7) . . . . ?
C7 C2 C3 C4 -1.2(11) . . . . ?
C1 C2 C3 C4 -177.6(7) . . . . ?
C2 C3 C4 C5 -1.0(14) . . . . ?
C3 C4 C5 C6 2.6(16) . . . . ?
C4 C5 C6 C7 -2.1(16) . . . . ?
C5 C6 C7 C2 -0.1(13) . . . . ?
C5 C6 C7 C8 177.7(8) . . . . ?
C3 C2 C7 C6 1.7(10) . . . . ?
C1 C2 C7 C6 178.1(6) . . . . ?
C3 C2 C7 C8 -176.2(6) . . . . ?
C1 C2 C7 C8 0.2(9) . . . . ?
C6 C7 C8 C13 137.1(7) . . . . ?
C2 C7 C8 C13 -45.1(8) . . . . ?
C6 C7 C8 C9 -45.2(9) . . . . ?
C2 C7 C8 C9 132.6(6) . . . . ?
C13 C8 C9 C10 1.3(9) . . . . ?
C7 C8 C9 C10 -176.4(6) . . . . ?
C8 C9 C10 C11 0.2(11) . . . . ?
C9 C10 C11 C12 -1.8(11) . . . . ?
C10 C11 C12 C13 1.8(10) . . . . ?
C11 C12 C13 C8 -0.2(9) . . . . ?
C11 C12 C13 C14 -177.0(5) . . . . ?
C9 C8 C13 C12 -1.3(8) . . . . ?
C7 C8 C13 C12 176.5(5) . . . . ?
C9 C8 C13 C14 175.6(5) . . . . ?
C7 C8 C13 C14 -6.7(8) . . . . ?
C12 C13 C14 N1 -104.8(6) . . . . ?
C8 C13 C14 N1 78.4(6) . . . . ?
N1 C15 C16 N2 -27.5(6) . . . . ?
N1 C15 C16 C17 155.0(5) . . . . ?
N2 C16 C17 C18 -1.9(9) . . . . ?
C15 C16 C17 C18 175.4(5) . . . . ?
C16 C17 C18 C19 1.6(10) . . . . ?
C17 C18 C19 C20 -0.3(11) . . . . ?
C18 C19 C20 N2 -0.7(11) . . . . ?
C16 C15 N1 C14 161.9(4) . . . . ?
C16 C15 N1 C1 -76.7(5) . . . . ?
C16 C15 N1 Zn 39.7(5) . . . . ?
C13 C14 N1 C15 75.6(5) . . . . ?
C13 C14 N1 C1 -44.3(6) . . . . ?
C13 C14 N1 Zn -168.1(4) . . . . ?
C2 C1 N1 C15 -164.2(5) . . . . ?
C2 C1 N1 C14 -43.2(7) . . . . ?
C2 C1 N1 Zn 82.9(5) . . . . ?
C17 C16 N2 C20 0.9(8) . . . . ?
C15 C16 N2 C20 -176.5(5) . . . . ?
C17 C16 N2 Zn 176.2(4) . . . . ?
C15 C16 N2 Zn -1.3(6) . . . . ?
C19 C20 N2 C16 0.4(9) . . . . ?
C19 C20 N2 Zn -174.2(5) . . . . ?
C16 N2 Zn O1 138.1(3) . . . . ?
C20 N2 Zn O1 -47.0(5) . . . . ?
C16 N2 Zn N2 -41.9(3) . . . 2_655 ?
C20 N2 Zn N2 133.0(5) . . . 2_655 ?
C16 N2 Zn N1 -101.9(4) . . . 2_655 ?
C20 N2 Zn N1 72.9(5) . . . 2_655 ?
C16 N2 Zn N1 18.9(4) . . . . ?
C20 N2 Zn N1 -166.2(5) . . . . ?
C15 N1 Zn O1 -117.8(3) . . . . ?
C14 N1 Zn O1 122.4(3) . . . . ?
C1 N1 Zn O1 -2.1(3) . . . . ?
C15 N1 Zn N2 -30.9(3) . . . . ?
C14 N1 Zn N2 -150.7(3) . . . . ?
C1 N1 Zn N2 84.7(3) . . . . ?
C15 N1 Zn N2 144.8(3) . . . 2_655 ?
C14 N1 Zn N2 25.0(3) . . . 2_655 ?
C1 N1 Zn N2 -99.5(3) . . . 2_655 ?
C15 N1 Zn N1 62.2(3) . . . 2_655 ?
C14 N1 Zn N1 -57.6(3) . . . 2_655 ?
C1 N1 Zn N1 177.9(3) . . . 2_655 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O5 0.82 1.97 2.646(12) 139.0 2_655
O1 H1 O2' 0.82 1.95 2.654(15) 143.4 2_655

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        24.98
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.060

#========================END

data_645341
_database_code_depnum_ccdc_archive 'CCDC 645341'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H38 Cl2 Cu N4 O9'
_chemical_formula_weight         853.18

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           monoclinic
_symmetry_space_group_name_H-M   C2/c

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                   22.153(12)
_cell_length_b                   9.755(2)
_cell_length_c                   22.365(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 124.36(3)
_cell_angle_gamma                90.00
_cell_volume                     3990(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      10
_cell_measurement_theta_max      15

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1764
_exptl_absorpt_coefficient_mu    0.741
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  0.9381
_exptl_absorpt_correction_T_max  0.9991
_exptl_absorpt_process_details   
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was 3
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;
_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  'CAD4 diffractometer'
_diffrn_measurement_method       '\w-2\t scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         2
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  3600
_diffrn_standards_decay_%        0
_diffrn_reflns_number            3580
_diffrn_reflns_av_R_equivalents  0.0148
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3485
_reflns_number_gt                2214
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'cad4 programs'
_computing_cell_refinement       'cad4 programs'
_computing_data_reduction        'xcad4 (wingx)'
_computing_structure_solution    'SIR92 (WINGX)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP3 (WINGX)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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.
The perchlorate anion is disordered. This could be resolved as two sets
of near tetrahedral oxygens associaled with same chlorine. For all atoms of
each set common site occupancy was assigned and the occupancies were refined
with sum of the occupancies of the two sets restrained as one. As the two
sets showed nearly equal occupancy(0.5 each), each set was assigned
occupancy of 0.5 during the last refinement job. The anisotropic thermal
ellipsoisds of perchlorate oxygens show some what large eccentricities.
The disorder resolved as two sets may be thought only as an approximation
to true situation in the lattice. The true disorder fixing may need several
sets which is practically not feasible. The anisotropic refinement was
preferred for perchlorate oxygens because it cleanses a fairly good amount
of unaccounted electron density (around the perchlorate).

Coordinating water oxygen stays on the two-fold axis. water hydrogen
were located in difference map and then geometrically restrained
during riding model refinement.Thermal parameter was allowed to
refine.
;

_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^)+(0.0791P)^2^+7.0101P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3485
_refine_ls_number_parameters     291
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.1049
_refine_ls_R_factor_gt           0.0624
_refine_ls_wR_factor_ref         0.1750
_refine_ls_wR_factor_gt          0.1514
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.068
_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
C15 C 0.4294(3) 0.3872(5) 0.1275(3) 0.0720(13) Uani 1 1 d . . .
H15A H 0.3890 0.4121 0.0790 0.086 Uiso 1 1 calc R . .
H15B H 0.4519 0.4710 0.1544 0.086 Uiso 1 1 calc R . .
C16 C 0.4839(3) 0.3071(5) 0.1233(3) 0.0659(13) Uani 1 1 d . . .
C17 C 0.4972(3) 0.3288(6) 0.0706(3) 0.0852(17) Uani 1 1 d . . .
H17 H 0.4703 0.3927 0.0339 0.102 Uiso 1 1 calc R . .
C18 C 0.5517(4) 0.2527(7) 0.0738(4) 0.098(2) Uani 1 1 d . . .
H18 H 0.5618 0.2654 0.0390 0.118 Uiso 1 1 calc R . .
C19 C 0.5911(4) 0.1580(7) 0.1285(4) 0.0971(19) Uani 1 1 d . . .
H19 H 0.6281 0.1065 0.1315 0.116 Uiso 1 1 calc R . .
C20 C 0.5741(3) 0.1423(6) 0.1779(3) 0.0855(16) Uani 1 1 d . . .
H20 H 0.5995 0.0771 0.2142 0.103 Uiso 1 1 calc R . .
C1 C 0.3466(3) 0.2029(5) 0.1094(3) 0.0744(14) Uani 1 1 d . . .
H1A H 0.3167 0.2465 0.0623 0.089 Uiso 1 1 calc R . .
H1B H 0.3732 0.1289 0.1052 0.089 Uiso 1 1 calc R . .
C2 C 0.2975(3) 0.1432(6) 0.1284(3) 0.0871(17) Uani 1 1 d . . .
C3 C 0.3045(4) 0.0056(7) 0.1482(5) 0.124(3) Uani 1 1 d . . .
H3 H 0.3401 -0.0484 0.1502 0.149 Uiso 1 1 calc R . .
C4 C 0.2577(5) -0.0511(9) 0.1651(6) 0.161(4) Uani 1 1 d . . .
H4 H 0.2627 -0.1427 0.1787 0.193 Uiso 1 1 calc R . .
C5 C 0.2052(6) 0.0271(11) 0.1617(6) 0.171(5) Uani 1 1 d . . .
H5 H 0.1754 -0.0106 0.1745 0.205 Uiso 1 1 calc R . .
C6 C 0.1955(4) 0.1627(10) 0.1393(5) 0.136(3) Uani 1 1 d . . .
H6 H 0.1578 0.2140 0.1349 0.163 Uiso 1 1 calc R . .
C7 C 0.2420(3) 0.2221(7) 0.1235(4) 0.0928(19) Uani 1 1 d . . .
C8 C 0.2313(3) 0.3667(7) 0.0988(3) 0.0884(18) Uani 1 1 d . . .
C9 C 0.1615(4) 0.4192(11) 0.0456(4) 0.120(3) Uani 1 1 d . . .
H9 H 0.1204 0.3641 0.0276 0.144 Uiso 1 1 calc R . .
C10 C 0.1534(6) 0.5512(14) 0.0199(4) 0.144(4) Uani 1 1 d . . .
H10 H 0.1073 0.5841 -0.0160 0.172 Uiso 1 1 calc R . .
C11 C 0.2135(6) 0.6331(11) 0.0477(4) 0.132(3) Uani 1 1 d . . .
H11 H 0.2079 0.7218 0.0301 0.158 Uiso 1 1 calc R . .
C12 C 0.2823(4) 0.5872(7) 0.1014(4) 0.0962(18) Uani 1 1 d . . .
H12 H 0.3224 0.6453 0.1200 0.115 Uiso 1 1 calc R . .
C13 C 0.2920(3) 0.4535(6) 0.1278(3) 0.0718(14) Uani 1 1 d . . .
C14 C 0.3657(3) 0.4005(5) 0.1878(3) 0.0652(12) Uani 1 1 d . . .
H14A H 0.3978 0.4780 0.2127 0.078 Uiso 1 1 calc R . .
H14B H 0.3604 0.3519 0.2224 0.078 Uiso 1 1 calc R . .
N1 N 0.4012(2) 0.3070(4) 0.1634(2) 0.0599(10) Uani 1 1 d . . .
N2 N 0.5228(2) 0.2162(4) 0.1765(2) 0.0685(11) Uani 1 1 d . . .
O1 O 0.5000 -0.0044(5) 0.2500 0.121(3) Uani 1 2 d S . .
H1 H 0.5024 -0.0325 0.2168 0.20(4) Uiso 1 1 calc R . .
Cl1 Cl 0.51719(12) -0.26484(17) 0.14426(11) 0.1046(6) Uani 1 1 d D . .
Cu Cu 0.5000 0.21043(9) 0.2500 0.0666(3) Uani 1 2 d S . .
O2 O 0.5234(8) -0.1378(10) 0.1226(8) 0.217(12) Uani 0.50 1 d PD A 1
O3 O 0.4623(8) -0.2752(18) 0.1529(11) 0.279(16) Uani 0.50 1 d PD A 1
O4 O 0.5848(7) -0.283(2) 0.2126(6) 0.297(16) Uani 0.50 1 d PD A 1
O5 O 0.5151(11) -0.3638(16) 0.1002(11) 0.296(16) Uani 0.50 1 d PD A 1
O2' O 0.5538(7) -0.1848(13) 0.1245(9) 0.231(12) Uani 0.50 1 d PD A 2
O3' O 0.4699(6) -0.1751(16) 0.1487(6) 0.160(6) Uani 0.50 1 d PD A 2
O4' O 0.5518(7) -0.3527(11) 0.1950(6) 0.230(13) Uani 0.50 1 d PD A 2
O5' O 0.4628(7) -0.3375(10) 0.0774(4) 0.160(7) Uani 0.50 1 d PD 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
C15 0.077(3) 0.073(3) 0.075(3) 0.005(3) 0.048(3) -0.007(3)
C16 0.080(3) 0.062(3) 0.071(3) -0.019(3) 0.052(3) -0.026(3)
C17 0.118(5) 0.083(4) 0.084(4) -0.012(3) 0.074(4) -0.025(3)
C18 0.140(6) 0.099(5) 0.113(5) -0.033(4) 0.107(5) -0.036(4)
C19 0.129(5) 0.093(4) 0.123(5) -0.015(4) 0.104(5) -0.007(4)
C20 0.110(4) 0.079(4) 0.108(4) -0.004(3) 0.086(4) 0.005(3)
C1 0.073(3) 0.080(3) 0.083(3) -0.032(3) 0.052(3) -0.017(3)
C2 0.084(4) 0.088(4) 0.114(5) -0.047(4) 0.071(4) -0.032(3)
C3 0.148(6) 0.082(4) 0.199(8) -0.065(5) 0.131(6) -0.051(4)
C4 0.210(9) 0.099(5) 0.264(11) -0.069(6) 0.188(9) -0.083(6)
C5 0.195(10) 0.140(8) 0.288(13) -0.089(9) 0.202(10) -0.085(7)
C6 0.123(6) 0.136(7) 0.204(9) -0.076(7) 0.126(6) -0.053(5)
C7 0.080(4) 0.111(5) 0.111(5) -0.057(4) 0.068(4) -0.039(4)
C8 0.074(4) 0.123(5) 0.082(4) -0.045(4) 0.052(3) -0.009(4)
C9 0.072(5) 0.198(9) 0.079(5) -0.057(5) 0.037(4) 0.011(5)
C10 0.121(7) 0.227(12) 0.073(5) -0.003(6) 0.048(5) 0.082(8)
C11 0.152(7) 0.174(9) 0.093(6) 0.037(6) 0.083(6) 0.084(8)
C12 0.112(5) 0.099(5) 0.101(5) 0.008(4) 0.074(4) 0.023(4)
C13 0.074(4) 0.083(4) 0.066(3) -0.013(3) 0.045(3) 0.004(3)
C14 0.073(3) 0.059(3) 0.070(3) -0.014(2) 0.044(3) -0.005(2)
N1 0.070(2) 0.058(2) 0.066(2) -0.0133(19) 0.047(2) -0.0129(19)
N2 0.087(3) 0.067(2) 0.081(3) -0.007(2) 0.066(3) -0.005(2)
O1 0.202(8) 0.063(3) 0.193(7) 0.000 0.169(7) 0.000
Cl1 0.1473(17) 0.0788(11) 0.1314(16) 0.0074(10) 0.1050(15) 0.0120(11)
Cu 0.0822(6) 0.0664(6) 0.0804(6) 0.000 0.0635(5) 0.000
O2 0.124(11) 0.050(6) 0.31(2) 0.055(9) 0.020(12) -0.008(7)
O3 0.27(2) 0.217(19) 0.53(4) -0.19(2) 0.34(3) -0.114(18)
O4 0.171(16) 0.56(5) 0.169(15) 0.18(2) 0.102(14) 0.10(2)
O5 0.41(4) 0.170(16) 0.52(4) -0.13(2) 0.40(4) -0.04(2)
O2' 0.213(18) 0.115(12) 0.46(3) 0.122(15) 0.25(2) 0.068(11)
O3' 0.142(11) 0.200(16) 0.099(8) -0.043(8) 0.044(7) 0.039(11)
O4' 0.194(17) 0.111(9) 0.166(13) 0.098(9) -0.030(12) -0.026(10)
O5' 0.33(2) 0.070(6) 0.111(8) -0.007(6) 0.140(11) -0.014(9)

_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
C15 C16 1.484(7) . ?
C15 N1 1.488(6) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 N2 1.337(6) . ?
C16 C17 1.384(7) . ?
C17 C18 1.383(8) . ?
C17 H17 0.9300 . ?
C18 C19 1.381(9) . ?
C18 H18 0.9300 . ?
C19 C20 1.362(7) . ?
C19 H19 0.9300 . ?
C20 N2 1.332(6) . ?
C20 H20 0.9300 . ?
C1 C2 1.492(7) . ?
C1 N1 1.519(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.394(9) . ?
C2 C7 1.400(8) . ?
C3 C4 1.401(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.358(12) . ?
C4 H4 0.9300 . ?
C5 C6 1.387(13) . ?
C5 H5 0.9300 . ?
C6 C7 1.391(9) . ?
C6 H6 0.9300 . ?
C7 C8 1.485(9) . ?
C8 C13 1.399(8) . ?
C8 C9 1.412(9) . ?
C9 C10 1.380(13) . ?
C9 H9 0.9300 . ?
C10 C11 1.364(12) . ?
C10 H10 0.9300 . ?
C11 C12 1.378(10) . ?
C11 H11 0.9300 . ?
C12 C13 1.398(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.504(7) . ?
C14 N1 1.494(5) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
N1 Cu 2.155(4) . ?
N2 Cu 1.975(4) . ?
O1 Cu 2.096(5) . ?
O1 H1 0.8200 . ?
Cl1 O4' 1.275(6) . ?
Cl1 O3 1.338(7) . ?
Cl1 O5 1.362(8) . ?
Cl1 O2 1.365(7) . ?
Cl1 O2' 1.367(7) . ?
Cl1 O3' 1.410(7) . ?
Cl1 O4 1.425(8) . ?
Cl1 O5' 1.468(7) . ?
Cu N2 1.975(4) 2_655 ?
Cu N1 2.155(4) 2_655 ?

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
C16 C15 N1 111.2(4) . . ?
C16 C15 H15A 109.4 . . ?
N1 C15 H15A 109.4 . . ?
C16 C15 H15B 109.4 . . ?
N1 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
N2 C16 C17 121.3(5) . . ?
N2 C16 C15 115.6(4) . . ?
C17 C16 C15 123.0(5) . . ?
C18 C17 C16 118.2(6) . . ?
C18 C17 H17 120.9 . . ?
C16 C17 H17 120.9 . . ?
C19 C18 C17 120.1(5) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C20 C19 C18 117.8(6) . . ?
C20 C19 H19 121.1 . . ?
C18 C19 H19 121.1 . . ?
N2 C20 C19 123.0(6) . . ?
N2 C20 H20 118.5 . . ?
C19 C20 H20 118.5 . . ?
C2 C1 N1 114.6(4) . . ?
C2 C1 H1A 108.6 . . ?
N1 C1 H1A 108.6 . . ?
C2 C1 H1B 108.6 . . ?
N1 C1 H1B 108.6 . . ?
H1A C1 H1B 107.6 . . ?
C3 C2 C7 119.3(6) . . ?
C3 C2 C1 119.8(5) . . ?
C7 C2 C1 120.8(6) . . ?
C2 C3 C4 120.0(7) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 120.2(8) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 120.6(8) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C7 120.2(8) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C6 C7 C2 119.6(7) . . ?
C6 C7 C8 120.4(6) . . ?
C2 C7 C8 120.0(5) . . ?
C13 C8 C9 118.7(7) . . ?
C13 C8 C7 119.6(5) . . ?
C9 C8 C7 121.8(7) . . ?
C10 C9 C8 120.8(8) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C11 C10 C9 119.5(9) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C10 C11 C12 121.5(10) . . ?
C10 C11 H11 119.3 . . ?
C12 C11 H11 119.3 . . ?
C11 C12 C13 120.1(7) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C12 C13 C8 119.4(6) . . ?
C12 C13 C14 121.9(5) . . ?
C8 C13 C14 118.7(5) . . ?
N1 C14 C13 114.5(4) . . ?
N1 C14 H14A 108.6 . . ?
C13 C14 H14A 108.6 . . ?
N1 C14 H14B 108.6 . . ?
C13 C14 H14B 108.6 . . ?
H14A C14 H14B 107.6 . . ?
C15 N1 C14 110.2(4) . . ?
C15 N1 C1 108.1(4) . . ?
C14 N1 C1 110.6(3) . . ?
C15 N1 Cu 101.1(3) . . ?
C14 N1 Cu 114.6(3) . . ?
C1 N1 Cu 111.8(3) . . ?
C20 N2 C16 119.5(4) . . ?
C20 N2 Cu 125.6(4) . . ?
C16 N2 Cu 114.8(3) . . ?
Cu O1 H1 109.5 . . ?
O4' Cl1 O3 87.7(11) . . ?
O4' Cl1 O5 85.7(12) . . ?
O3 Cl1 O5 112.9(7) . . ?
O4' Cl1 O2 142.7(8) . . ?
O3 Cl1 O2 113.6(7) . . ?
O5 Cl1 O2 110.9(8) . . ?
O4' Cl1 O2' 120.2(7) . . ?
O3 Cl1 O2' 147.5(8) . . ?
O5 Cl1 O2' 87.4(10) . . ?
O2 Cl1 O2' 33.9(7) . . ?
O4' Cl1 O3' 116.9(8) . . ?
O3 Cl1 O3' 42.8(8) . . ?
O5 Cl1 O3' 140.1(10) . . ?
O2 Cl1 O3' 71.8(8) . . ?
O2' Cl1 O3' 105.5(6) . . ?
O4' Cl1 O4 38.8(9) . . ?
O3 Cl1 O4 109.0(8) . . ?
O5 Cl1 O4 105.8(7) . . ?
O2 Cl1 O4 103.9(7) . . ?
O2' Cl1 O4 87.9(10) . . ?
O3' Cl1 O4 112.1(10) . . ?
O4' Cl1 O5' 108.5(6) . . ?
O3 Cl1 O5' 79.7(9) . . ?
O5 Cl1 O5' 41.2(9) . . ?
O2 Cl1 O5' 105.4(8) . . ?
O2' Cl1 O5' 104.0(7) . . ?
O3' Cl1 O5' 99.0(6) . . ?
O4 Cl1 O5' 142.5(10) . . ?
N2 Cu N2 176.7(2) 2_655 . ?
N2 Cu O1 91.63(12) 2_655 . ?
N2 Cu O1 91.63(12) . . ?
N2 Cu N1 81.18(16) 2_655 2_655 ?
N2 Cu N1 97.37(16) . 2_655 ?
O1 Cu N1 115.93(9) . 2_655 ?
N2 Cu N1 97.37(16) 2_655 . ?
N2 Cu N1 81.18(16) . . ?
O1 Cu N1 115.93(9) . . ?
N1 Cu N1 128.14(19) 2_655 . ?

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
N1 C15 C16 N2 -29.9(6) . . . . ?
N1 C15 C16 C17 153.5(4) . . . . ?
N2 C16 C17 C18 0.6(8) . . . . ?
C15 C16 C17 C18 177.0(5) . . . . ?
C16 C17 C18 C19 0.1(9) . . . . ?
C17 C18 C19 C20 0.4(9) . . . . ?
C18 C19 C20 N2 -1.6(10) . . . . ?
N1 C1 C2 C3 -111.5(6) . . . . ?
N1 C1 C2 C7 71.4(7) . . . . ?
C7 C2 C3 C4 -2.0(11) . . . . ?
C1 C2 C3 C4 -179.1(7) . . . . ?
C2 C3 C4 C5 0.5(14) . . . . ?
C3 C4 C5 C6 2.1(16) . . . . ?
C4 C5 C6 C7 -3.2(15) . . . . ?
C5 C6 C7 C2 1.7(12) . . . . ?
C5 C6 C7 C8 179.4(8) . . . . ?
C3 C2 C7 C6 0.8(10) . . . . ?
C1 C2 C7 C6 178.0(6) . . . . ?
C3 C2 C7 C8 -176.9(6) . . . . ?
C1 C2 C7 C8 0.3(8) . . . . ?
C6 C7 C8 C13 136.0(6) . . . . ?
C2 C7 C8 C13 -46.3(8) . . . . ?
C6 C7 C8 C9 -45.2(8) . . . . ?
C2 C7 C8 C9 132.5(6) . . . . ?
C13 C8 C9 C10 3.1(9) . . . . ?
C7 C8 C9 C10 -175.6(6) . . . . ?
C8 C9 C10 C11 -1.7(11) . . . . ?
C9 C10 C11 C12 -0.4(12) . . . . ?
C10 C11 C12 C13 1.0(10) . . . . ?
C11 C12 C13 C8 0.6(8) . . . . ?
C11 C12 C13 C14 -178.1(5) . . . . ?
C9 C8 C13 C12 -2.5(7) . . . . ?
C7 C8 C13 C12 176.2(5) . . . . ?
C9 C8 C13 C14 176.2(4) . . . . ?
C7 C8 C13 C14 -5.0(7) . . . . ?
C12 C13 C14 N1 -103.7(5) . . . . ?
C8 C13 C14 N1 77.6(5) . . . . ?
C16 C15 N1 C14 162.3(4) . . . . ?
C16 C15 N1 C1 -76.8(5) . . . . ?
C16 C15 N1 Cu 40.8(4) . . . . ?
C13 C14 N1 C15 74.4(5) . . . . ?
C13 C14 N1 C1 -45.1(5) . . . . ?
C13 C14 N1 Cu -172.5(3) . . . . ?
C2 C1 N1 C15 -162.8(5) . . . . ?
C2 C1 N1 C14 -42.1(6) . . . . ?
C2 C1 N1 Cu 86.8(5) . . . . ?
C19 C20 N2 C16 2.4(8) . . . . ?
C19 C20 N2 Cu -175.0(5) . . . . ?
C17 C16 N2 C20 -1.8(7) . . . . ?
C15 C16 N2 C20 -178.4(4) . . . . ?
C17 C16 N2 Cu 175.8(4) . . . . ?
C15 C16 N2 Cu -0.8(5) . . . . ?
C20 N2 Cu N2 133.3(4) . . . 2_655 ?
C16 N2 Cu N2 -44.1(3) . . . 2_655 ?
C20 N2 Cu O1 -46.7(4) . . . . ?
C16 N2 Cu O1 135.9(3) . . . . ?
C20 N2 Cu N1 69.7(4) . . . 2_655 ?
C16 N2 Cu N1 -107.7(3) . . . 2_655 ?
C20 N2 Cu N1 -162.7(4) . . . . ?
C16 N2 Cu N1 19.9(3) . . . . ?
C15 N1 Cu N2 144.6(3) . . . 2_655 ?
C14 N1 Cu N2 26.2(3) . . . 2_655 ?
C1 N1 Cu N2 -100.6(3) . . . 2_655 ?
C15 N1 Cu N2 -32.5(3) . . . . ?
C14 N1 Cu N2 -150.9(3) . . . . ?
C1 N1 Cu N2 82.3(3) . . . . ?
C15 N1 Cu O1 -120.0(2) . . . . ?
C14 N1 Cu O1 121.6(3) . . . . ?
C1 N1 Cu O1 -5.2(3) . . . . ?
C15 N1 Cu N1 60.0(2) . . . 2_655 ?
C14 N1 Cu N1 -58.4(3) . . . 2_655 ?
C1 N1 Cu N1 174.8(3) . . . 2_655 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O3' 0.82 1.88 2.578(10) 142.1 .

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.055