# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 186/1916

data_global

# 1. SUBMISSION DETAILS
_publ_contact_author  'Dr. Malcolm A. Halcrow'
_publ_contact_address
;
   School of Chemistry, 
   University of Leeds,
   Woodhouse Lane,
   Leeds LS2 9JT,
   UK
;
_publ_contact_author_phone       '+44 (0)113 2336506'
_publ_contact_author_fax         '+44 (0)113 2336565'
_publ_contact_author_email       M.A.Halcrow@chem.leeds.ac.uk
_publ_contact_letter
;
This CIF file contains a structure described in a manuscript that we have 
just submitted to Dalton Transactions. 
;

#=======================================================================

# 2. TITLE AND AUTHOR LIST
_publ_requested_journal
   'Dalton Transactions'
_publ_section_title
;
Copper(II) Complexes of Hydroquinone-Containing Schiff Bases. Towards a
Structural Model for Copper Amine Oxidases.
;
loop_
_publ_author_name
   'Peiyi Li'
   'Nayan K. Solanki'
   'Neil Feeder'
   'John E. Davies'
   'Jeremy M. Rawson'
   'Malcolm A. Halcrow'

_publ_author_address
;      
   Department of Chemistry,
   University of Cambridge,
   Lensfield Road,
   Cambridge CB2 1EW,
   UK

AND

   School of Chemistry, 
   University of Leeds,
   Woodhouse Lane,
   Leeds LS2 9JT,
   UK
;

#=================================================================
 
data_mh9601 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
Bis(2-[2-{2',5'-dihydroxybenzaldimino}ethyl]pyridine)dicopper(II) 
ditetrafluoroborate nitromethane solvate 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          
'[C28 H26 N4 O4 Cu2][B F4]2 C H3 N O2'  
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C29 H29 B2 Cu2 F8 N5 O6' 
_chemical_formula_weight          844.27 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
 
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' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cu'  'Cu'   0.3201   1.2651 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'B'  'B'   0.0013   0.0007 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'F'  'F'   0.0171   0.0103 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Triclinic 
_symmetry_space_group_name_H-M    P-1 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    14.605(4) 
_cell_length_b                    12.551(3) 
_cell_length_c                    11.021(3) 
_cell_angle_alpha                 106.74(2) 
_cell_angle_beta                  75.19(3) 
_cell_angle_gamma                 71.34(2) 
_cell_volume                      1692.9(8) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     25 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             'v dark brown'
_exptl_crystal_size_max           0.25 
_exptl_crystal_size_mid           0.20 
_exptl_crystal_size_min           0.15
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.656 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              852 
_exptl_absorpt_coefficient_mu     1.350 
_exptl_absorpt_correction_type    'semi-empirical (2 psi scans)' 
_exptl_absorpt_correction_T_min   0.868 
_exptl_absorpt_correction_T_max   0.976
 
_exptl_special_details 
; 
 There is a pseudo-monoclinic C-centred cell.  The laue symmetry is 
 definitely -1.
; 
 
_diffrn_ambient_temperature       150(2) 
_diffrn_radiation_wavelength      0.71069 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        'Rigaku AFC7R' 
_diffrn_measurement_method        'omega/2theta scans '
_diffrn_standards_number          3 
_diffrn_standards_interval_count  200 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0.7% 
_diffrn_reflns_number             4617 
_diffrn_reflns_av_R_equivalents   0.0504 
_diffrn_reflns_av_sigmaI/netI     0.0908 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        15 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -11 
_diffrn_reflns_limit_l_max        11 
_diffrn_reflns_theta_min          2.69 
_diffrn_reflns_theta_max          22.49 
_reflns_number_total              4407 
_reflns_number_observed           2968 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        'Rigaku control software' 
_computing_cell_refinement        'Rigaku control software' 
_computing_data_reduction         
'TEXSAN (Molecular Structure Corporation, 1995)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Siemens SHELXTL (Sheldrick, 1987)' 
_computing_publication_material   'Siemens SHELXTL (Sheldrick, 1987)' 
 
_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 anion centred on B44 is disordered by rotation about the B44-F45 bond.
 The disordered F atoms were modelled over three orientations:
 F46A-F48A, occupancy 0.5
 F46B-F48B, occupancy 0.3
 F46C-F48C, occupancy 0.2
 All B-F and F...F distances within the disordered anion were restrained to
 1.36(2) and 2.22(2) \%A, respectively. The highest residual peak of 
 1.07 e.\%A^-3^ lies within this disordered region.

 All fully occupied non-H atoms were refined anisotropically.
; 
 
_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^)+(0.0857P)^2^+5.9119P] 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          4394 
_refine_ls_number_parameters      483 
_refine_ls_number_restraints      28 
_refine_ls_R_factor_all           0.1087 
_refine_ls_R_factor_gt            0.0666 
_refine_ls_wR_factor_ref          0.1825 
_refine_ls_wR_factor_gt           0.1577 
_refine_ls_goodness_of_fit_ref    1.028 
_refine_ls_restrained_S_all       1.046 
_refine_ls_shift/su_max           0.011 
_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 0.80373(8) 0.22972(9) 1.02126(11) 0.0254(3) Uani 1 1 d . . . 
Cu2 Cu 0.65912(8) 0.15089(9) 0.90982(11) 0.0246(3) Uani 1 1 d . . . 
N3 N 0.7721(5) 0.3241(6) 1.2173(7) 0.0272(17) Uani 1 1 d . . . 
C4 C 0.6853(8) 0.3370(8) 1.3113(10) 0.035(2) Uani 1 1 d . . . 
H4 H 0.6400 0.3087 1.2819 0.041(5) Uiso 1 1 calc R . . 
C5 C 0.6617(9) 0.3907(9) 1.4493(10) 0.047(3) Uani 1 1 d . . . 
H5 H 0.6021 0.3973 1.5130 0.041(5) Uiso 1 1 calc R . . 
C6 C 0.7289(10) 0.4348(10) 1.4910(12) 0.059(3) Uani 1 1 d . . . 
H6 H 0.7149 0.4720 1.5839 0.041(5) Uiso 1 1 calc R . . 
C7 C 0.8167(10) 0.4230(10) 1.3939(11) 0.055(3) Uani 1 1 d . . . 
H7 H 0.8625 0.4517 1.4215 0.041(5) Uiso 1 1 calc R . . 
C8 C 0.8368(7) 0.3694(8) 1.2570(9) 0.032(2) Uani 1 1 d . . . 
C9 C 0.9324(7) 0.3463(8) 1.1477(10) 0.035(2) Uani 1 1 d . . . 
H9A H 0.9725 0.3820 1.1891 0.041(5) Uiso 1 1 calc R . . 
H9B H 0.9127 0.3874 1.0900 0.041(5) Uiso 1 1 calc R . . 
C10 C 1.0010(7) 0.2115(8) 1.0588(10) 0.036(2) Uani 1 1 d . . . 
H10A H 1.0695 0.2016 1.0054 0.041(5) Uiso 1 1 calc R . . 
H10B H 1.0098 0.1670 1.1169 0.041(5) Uiso 1 1 calc R . . 
N11 N 0.9553(5) 0.1586(6) 0.9648(7) 0.0253(17) Uani 1 1 d . . . 
C12 C 1.0187(7) 0.0705(8) 0.8503(9) 0.026(2) Uani 1 1 d . . . 
H12 H 1.0893 0.0459 0.8351 0.041(5) Uiso 1 1 calc R . . 
C13 C 0.9955(6) 0.0036(7) 0.7408(9) 0.024(2) Uani 1 1 d . . . 
C14 C 0.8924(6) 0.0308(7) 0.7427(9) 0.025(2) Uani 1 1 d . . . 
C15 C 0.8825(6) -0.0353(7) 0.6262(9) 0.026(2) Uani 1 1 d . . . 
H15 H 0.8159 -0.0173 0.6248 0.041(5) Uiso 1 1 calc R . . 
C16 C 0.9669(7) -0.1261(8) 0.5131(9) 0.029(2) Uani 1 1 d . . . 
H16 H 0.9574 -0.1694 0.4369 0.041(5) Uiso 1 1 calc R . . 
C17 C 1.0686(7) -0.1536(8) 0.5127(9) 0.033(2) Uani 1 1 d . . . 
C18 C 1.0812(7) -0.0893(8) 0.6249(9) 0.031(2) Uani 1 1 d . . . 
H18 H 1.1483 -0.1075 0.6243 0.041(5) Uiso 1 1 calc R . . 
O19 O 0.8084(4) 0.1188(5) 0.8541(5) 0.0239(13) Uani 1 1 d . . . 
O20 O 1.1556(5) -0.2422(6) 0.3988(7) 0.0439(18) Uani 1 1 d . . . 
H20 H 1.1372 -0.2807 0.3437 0.041(5) Uiso 1 1 calc R . . 
N21 N 0.6799(5) -0.0208(6) 0.8268(7) 0.0263(17) Uani 1 1 d . . . 
C22 C 0.7562(7) -0.1098(8) 0.8359(10) 0.033(2) Uani 1 1 d . . . 
H22 H 0.7982 -0.0876 0.8793 0.041(5) Uiso 1 1 calc R . . 
C23 C 0.7742(8) -0.2291(8) 0.7852(11) 0.043(3) Uani 1 1 d . . . 
H23 H 0.8266 -0.2876 0.7950 0.041(5) Uiso 1 1 calc R . . 
C24 C 0.7134(8) -0.2630(8) 0.7183(11) 0.045(3) Uani 1 1 d . . . 
H24 H 0.7255 -0.3451 0.6805 0.041(5) Uiso 1 1 calc R . . 
C25 C 0.6359(7) -0.1755(8) 0.7083(10) 0.036(2) Uani 1 1 d . . . 
H25 H 0.5941 -0.1973 0.6642 0.041(5) Uiso 1 1 calc R . . 
C26 C 0.6188(7) -0.0531(8) 0.7640(9) 0.028(2) Uani 1 1 d . . . 
C27 C 0.5315(7) 0.0492(8) 0.7627(10) 0.033(2) Uani 1 1 d . . . 
H27A H 0.4913 0.0157 0.7189 0.041(5) Uiso 1 1 calc R . . 
H27B H 0.5606 0.0886 0.7095 0.041(5) Uiso 1 1 calc R . . 
C28 C 0.4590(7) 0.1453(8) 0.9094(10) 0.032(2) Uani 1 1 d . . . 
H28A H 0.3941 0.1974 0.9081 0.041(5) Uiso 1 1 calc R . . 
H28B H 0.4422 0.1036 0.9677 0.041(5) Uiso 1 1 calc R . . 
N29 N 0.5083(5) 0.2222(6) 0.9670(7) 0.0223(16) Uani 1 1 d . . . 
C30 C 0.4462(6) 0.3364(8) 1.0465(9) 0.026(2) Uani 1 1 d . . . 
H30 H 0.3754 0.3608 1.0628 0.041(5) Uiso 1 1 calc R . . 
C31 C 0.4769(6) 0.4299(7) 1.1125(8) 0.0185(18) Uani 1 1 d . . . 
C32 C 0.5793(7) 0.4105(7) 1.1018(8) 0.025(2) Uani 1 1 d . . . 
C33 C 0.5970(7) 0.5102(7) 1.1637(9) 0.027(2) Uani 1 1 d . . . 
H33 H 0.6644 0.4979 1.1587 0.041(5) Uiso 1 1 calc R . . 
C34 C 0.5177(7) 0.6280(8) 1.2328(9) 0.028(2) Uani 1 1 d . . . 
H34 H 0.5311 0.6933 1.2765 0.041(5) Uiso 1 1 calc R . . 
C35 C 0.4164(7) 0.6478(8) 1.2363(8) 0.026(2) Uani 1 1 d . . . 
C36 C 0.3961(6) 0.5502(7) 1.1789(8) 0.0218(19) Uani 1 1 d . . . 
H36 H 0.3287 0.5632 1.1838 0.041(5) Uiso 1 1 calc R . . 
O37 O 0.6582(4) 0.2965(5) 1.0337(6) 0.0255(14) Uani 1 1 d . . . 
O38 O 0.3419(5) 0.7690(5) 1.2961(7) 0.0342(15) Uani 1 1 d . . . 
H38 H 0.2833 0.7712 1.3244 0.041(5) Uiso 1 1 calc R . . 
B39 B 0.6945(10) 0.0485(11) 1.1819(14) 0.043(3) Uani 1 1 d . . . 
F40 F 0.6092(5) 0.0998(6) 1.1498(7) 0.0651(19) Uani 1 1 d . . . 
F41 F 0.6735(6) 0.1008(6) 1.3171(7) 0.078(2) Uani 1 1 d . . . 
F42 F 0.7763(4) 0.0695(5) 1.1079(6) 0.0406(14) Uani 1 1 d . . . 
F43 F 0.7247(4) -0.0761(5) 1.1400(6) 0.0499(16) Uani 1 1 d . . . 
B44 B 0.8701(7) 0.4595(9) 0.8497(11) 0.043(3) Uani 1 1 d D . . 
F45 F 0.8355(7) 0.4843(7) 0.7535(8) 0.105(3) Uani 1 1 d D A . 
F46A F 0.9672(12) 0.451(2) 0.815(2) 0.147(10) Uiso 0.50 1 d PD A 1 
F47A F 0.7986(11) 0.5623(12) 0.9658(12) 0.067(4) Uiso 0.50 1 d PD A 1 
F48A F 0.8624(13) 0.3552(11) 0.8526(16) 0.043(3) Uiso 0.50 1 d PD A 1 
F46B F 0.9443(17) 0.489(2) 0.883(3) 0.076(8) Uiso 0.30 1 d PD A 2 
F47B F 0.7867(16) 0.509(3) 0.9746(17) 0.115(12) Uiso 0.30 1 d PD A 2 
F48B F 0.9100(18) 0.3325(12) 0.803(2) 0.043(6) Uiso 0.30 1 d PD A 2 
F46C F 0.818(2) 0.411(3) 0.923(3) 0.046(8) Uiso 0.20 1 d PD A 3 
F47C F 0.869(3) 0.562(2) 0.937(3) 0.070(10) Uiso 0.20 1 d PD A 3 
F48C F 0.9738(17) 0.373(4) 0.782(3) 0.23(4) Uiso 0.20 1 d PD A 3 
C49 C 0.8028(11) -0.2838(12) 1.2426(13) 0.080(4) Uani 1 1 d . . . 
H49A H 0.7819 -0.2800 1.1676 0.041(5) Uiso 1 1 calc R . . 
H49B H 0.8098 -0.3600 1.2502 0.041(5) Uiso 1 1 calc R . . 
H49C H 0.8687 -0.2785 1.2265 0.041(5) Uiso 1 1 calc R . . 
N50 N 0.7279(12) -0.1867(13) 1.3633(13) 0.090(4) Uani 1 1 d . . . 
O51 O 0.7537(11) -0.1186(12) 1.4337(13) 0.128(5) Uani 1 1 d . . . 
O52 O 0.6345(11) -0.1747(16) 1.3964(15) 0.150(6) Uani 1 1 d . . . 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
Cu1 0.0170(6) 0.0238(6) 0.0298(7) 0.0077(5) -0.0111(5) -0.0030(5) 
Cu2 0.0137(6) 0.0184(6) 0.0341(7) 0.0066(5) -0.0073(5) -0.0029(5) 
N3 0.022(4) 0.022(4) 0.036(5) 0.013(3) -0.014(4) -0.004(3) 
C4 0.039(6) 0.025(5) 0.040(6) 0.015(5) -0.018(5) -0.009(5) 
C5 0.069(8) 0.043(6) 0.030(6) 0.015(5) -0.017(6) -0.026(6) 
C6 0.084(10) 0.053(7) 0.038(7) 0.012(6) -0.026(7) -0.031(7) 
C7 0.064(8) 0.053(7) 0.048(7) 0.011(6) -0.022(6) -0.034(7) 
C8 0.039(6) 0.024(5) 0.036(6) 0.014(4) -0.021(5) -0.012(4) 
C9 0.039(6) 0.024(5) 0.047(6) 0.011(5) -0.026(5) -0.014(5) 
C10 0.024(5) 0.039(6) 0.052(6) 0.018(5) -0.026(5) -0.012(5) 
N11 0.019(4) 0.021(4) 0.031(4) 0.011(4) -0.009(4) -0.001(3) 
C12 0.015(5) 0.028(5) 0.035(6) 0.017(5) -0.011(4) -0.005(4) 
C13 0.014(5) 0.023(5) 0.031(5) 0.009(4) -0.010(4) -0.004(4) 
C14 0.013(5) 0.019(5) 0.031(5) 0.009(4) -0.002(4) 0.001(4) 
C15 0.012(5) 0.027(5) 0.032(5) 0.007(4) -0.009(4) -0.006(4) 
C16 0.028(5) 0.029(5) 0.031(5) 0.012(4) -0.011(5) -0.015(5) 
C17 0.020(5) 0.022(5) 0.037(6) 0.006(4) 0.000(5) 0.001(4) 
C18 0.013(5) 0.030(5) 0.039(6) 0.012(5) -0.004(4) -0.002(4) 
O19 0.015(3) 0.025(3) 0.023(3) 0.007(3) -0.004(3) -0.003(3) 
O20 0.023(4) 0.037(4) 0.044(4) -0.002(3) -0.001(3) -0.004(3) 
N21 0.021(4) 0.020(4) 0.031(4) 0.008(3) -0.007(4) -0.007(3) 
C22 0.022(5) 0.025(5) 0.050(6) 0.014(5) -0.014(5) -0.006(4) 
C23 0.030(6) 0.025(6) 0.063(7) 0.017(5) -0.013(5) -0.003(5) 
C24 0.042(6) 0.014(5) 0.057(7) 0.002(5) -0.002(6) -0.009(5) 
C25 0.026(5) 0.024(5) 0.047(6) 0.003(5) -0.013(5) -0.011(5) 
C26 0.024(5) 0.027(5) 0.029(5) 0.008(4) -0.002(4) -0.014(4) 
C27 0.027(5) 0.026(5) 0.048(6) 0.014(5) -0.017(5) -0.012(4) 
C28 0.017(5) 0.021(5) 0.051(6) 0.009(5) -0.011(5) -0.007(4) 
N29 0.017(4) 0.020(4) 0.030(4) 0.008(3) -0.008(3) -0.010(3) 
C30 0.011(4) 0.032(5) 0.031(5) 0.016(4) -0.004(4) -0.006(4) 
C31 0.009(4) 0.021(5) 0.021(5) 0.008(4) -0.001(4) -0.004(4) 
C32 0.032(5) 0.018(5) 0.026(5) 0.010(4) -0.015(4) -0.009(4) 
C33 0.021(5) 0.023(5) 0.039(5) 0.013(4) -0.011(4) -0.009(4) 
C34 0.036(6) 0.017(5) 0.029(5) 0.004(4) -0.016(4) -0.011(4) 
C35 0.020(5) 0.024(5) 0.022(5) 0.007(4) -0.004(4) -0.001(4) 
C36 0.018(5) 0.022(5) 0.022(5) 0.010(4) -0.002(4) -0.007(4) 
O37 0.013(3) 0.015(3) 0.034(3) 0.002(3) -0.007(3) 0.003(3) 
O38 0.023(3) 0.019(3) 0.047(4) 0.007(3) -0.010(3) -0.002(3) 
B39 0.039(7) 0.040(7) 0.069(9) 0.032(7) -0.036(7) -0.018(6) 
F40 0.031(3) 0.070(4) 0.111(6) 0.056(4) -0.034(4) -0.019(3) 
F41 0.126(7) 0.073(5) 0.050(4) 0.030(4) -0.030(4) -0.058(5) 
F42 0.033(3) 0.038(3) 0.066(4) 0.032(3) -0.023(3) -0.021(3) 
F43 0.044(4) 0.036(3) 0.084(4) 0.033(3) -0.031(3) -0.023(3) 
B44 0.020(6) 0.048(8) 0.068(9) 0.022(7) -0.019(6) -0.022(6) 
F45 0.169(9) 0.098(6) 0.122(7) 0.078(6) -0.092(7) -0.088(7) 
C49 0.084(11) 0.061(9) 0.067(9) 0.022(8) -0.023(8) -0.005(8) 
N50 0.101(11) 0.113(11) 0.075(9) 0.047(9) -0.047(9) -0.051(10) 
O51 0.183(14) 0.126(10) 0.120(10) 0.045(8) -0.109(10) -0.082(10) 
O52 0.116(11) 0.252(18) 0.161(13) 0.126(13) -0.073(10) -0.119(12) 
 
_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 O19 1.933(5) . ? 
Cu1 N11 1.949(7) . ? 
Cu1 O37 1.970(5) . ? 
Cu1 N3 1.987(7) . ? 
Cu1 F42 2.558(5) . ? 
Cu1 Cu2 2.9852(16) . ? 
Cu2 O37 1.935(5) . ? 
Cu2 N29 1.937(7) . ? 
Cu2 N21 1.968(7) . ? 
Cu2 O19 1.976(5) . ? 
Cu2 O38 2.736(7) 2_667 ? 
Cu2 F40 2.869(7) . ? 
N3 C4 1.344(12) . ? 
N3 C8 1.350(11) . ? 
C4 C5 1.370(13) . ? 
C5 C6 1.383(15) . ? 
C6 C7 1.378(15) . ? 
C7 C8 1.370(14) . ? 
C8 C9 1.471(13) . ? 
C9 C10 1.511(12) . ? 
C10 N11 1.483(11) . ? 
N11 C12 1.271(10) . ? 
C12 C13 1.443(12) . ? 
C13 C18 1.396(12) . ? 
C13 C14 1.426(11) . ? 
C14 O19 1.347(10) . ? 
C14 C15 1.384(12) . ? 
C15 C16 1.367(12) . ? 
C16 C17 1.411(12) . ? 
C17 C18 1.360(13) . ? 
C17 O20 1.380(10) . ? 
N21 C26 1.350(11) . ? 
N21 C22 1.351(11) . ? 
C22 C23 1.347(13) . ? 
C23 C24 1.382(14) . ? 
C24 C25 1.356(13) . ? 
C25 C26 1.391(12) . ? 
C26 C27 1.499(12) . ? 
C27 C28 1.542(12) . ? 
C28 N29 1.476(10) . ? 
N29 C30 1.298(10) . ? 
C30 C31 1.455(11) . ? 
C31 C32 1.404(11) . ? 
C31 C36 1.410(11) . ? 
C32 O37 1.350(10) . ? 
C32 C33 1.380(12) . ? 
C33 C34 1.383(12) . ? 
C34 C35 1.408(12) . ? 
C35 C36 1.368(11) . ? 
C35 O38 1.389(10) . ? 
B39 F41 1.348(14) . ? 
B39 F43 1.376(13) . ? 
B39 F40 1.391(12) . ? 
B39 F42 1.410(14) . ? 
B44 F46A 1.332(14) . ? 
B44 F46B 1.348(14) . ? 
B44 F45 1.357(11) . ? 
B44 F48A 1.358(12) . ? 
B44 F47C 1.360(16) . ? 
B44 F46C 1.372(16) . ? 
B44 F47A 1.378(13) . ? 
B44 F48B 1.388(14) . ? 
B44 F48C 1.389(17) . ? 
B44 F47B 1.391(15) . ? 
C49 N50 1.385(16) . ? 
N50 O51 1.204(15) . ? 
N50 O52 1.265(16) . ? 
 
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 
O19 Cu1 N11 93.7(3) . . ? 
O19 Cu1 O37 76.3(2) . . ? 
N11 Cu1 O37 166.7(3) . . ? 
O19 Cu1 N3 163.3(3) . . ? 
N11 Cu1 N3 95.8(3) . . ? 
O37 Cu1 N3 96.1(3) . . ? 
O19 Cu1 F42 82.2(2) . . ? 
N11 Cu1 F42 95.8(2) . . ? 
O37 Cu1 F42 91.5(2) . . ? 
N3 Cu1 F42 83.2(2) . . ? 
O37 Cu2 N29 93.4(3) . . ? 
O37 Cu2 N21 159.5(3) . . ? 
N29 Cu2 N21 95.7(3) . . ? 
O37 Cu2 O19 76.1(2) . . ? 
N29 Cu2 O19 165.9(3) . . ? 
N21 Cu2 O19 97.3(3) . . ? 
O37 Cu2 O38 95.1(2) . 2_667 ? 
N29 Cu2 O38 85.0(2) . 2_667 ? 
N21 Cu2 O38 104.0(2) . 2_667 ? 
O19 Cu2 O38 86.7(2) . 2_667 ? 
O37 Cu2 F40 83.6(2) . . ? 
N29 Cu2 F40 82.0(2) . . ? 
N21 Cu2 F40 79.5(2) . . ? 
O19 Cu2 F40 105.6(2) . . ? 
O38 Cu2 F40 166.82(17) 2_667 . ? 
C4 N3 C8 120.3(8) . . ? 
C4 N3 Cu1 117.6(6) . . ? 
C8 N3 Cu1 122.1(6) . . ? 
N3 C4 C5 122.0(10) . . ? 
C4 C5 C6 118.1(11) . . ? 
C7 C6 C5 119.5(10) . . ? 
C8 C7 C6 120.4(11) . . ? 
N3 C8 C7 119.7(9) . . ? 
N3 C8 C9 116.7(8) . . ? 
C7 C8 C9 123.4(9) . . ? 
C8 C9 C10 113.7(8) . . ? 
N11 C10 C9 111.7(7) . . ? 
C12 N11 C10 117.2(7) . . ? 
C12 N11 Cu1 124.1(6) . . ? 
C10 N11 Cu1 118.6(5) . . ? 
N11 C12 C13 128.5(8) . . ? 
C18 C13 C14 119.5(8) . . ? 
C18 C13 C12 116.4(7) . . ? 
C14 C13 C12 124.0(7) . . ? 
O19 C14 C15 121.8(7) . . ? 
O19 C14 C13 120.6(7) . . ? 
C15 C14 C13 117.7(7) . . ? 
C16 C15 C14 122.4(8) . . ? 
C15 C16 C17 119.6(8) . . ? 
C18 C17 O20 119.4(8) . . ? 
C18 C17 C16 119.5(8) . . ? 
O20 C17 C16 121.0(8) . . ? 
C17 C18 C13 121.3(8) . . ? 
C14 O19 Cu1 128.9(5) . . ? 
C14 O19 Cu2 130.6(5) . . ? 
Cu1 O19 Cu2 99.6(2) . . ? 
C26 N21 C22 118.4(7) . . ? 
C26 N21 Cu2 122.5(6) . . ? 
C22 N21 Cu2 119.1(6) . . ? 
C23 C22 N21 123.1(9) . . ? 
C22 C23 C24 118.8(9) . . ? 
C25 C24 C23 119.4(9) . . ? 
C24 C25 C26 120.0(9) . . ? 
N21 C26 C25 120.4(8) . . ? 
N21 C26 C27 116.7(7) . . ? 
C25 C26 C27 122.9(8) . . ? 
C26 C27 C28 111.1(8) . . ? 
N29 C28 C27 111.5(7) . . ? 
C30 N29 C28 116.2(7) . . ? 
C30 N29 Cu2 124.9(6) . . ? 
C28 N29 Cu2 118.8(5) . . ? 
N29 C30 C31 126.1(7) . . ? 
C32 C31 C36 119.9(7) . . ? 
C32 C31 C30 125.3(7) . . ? 
C36 C31 C30 114.5(7) . . ? 
O37 C32 C33 120.9(8) . . ? 
O37 C32 C31 120.6(7) . . ? 
C33 C32 C31 118.5(8) . . ? 
C32 C33 C34 122.0(8) . . ? 
C33 C34 C35 119.2(8) . . ? 
C36 C35 O38 123.2(8) . . ? 
C36 C35 C34 119.9(8) . . ? 
O38 C35 C34 116.9(7) . . ? 
C35 C36 C31 120.4(8) . . ? 
C32 O37 Cu2 128.1(5) . . ? 
C32 O37 Cu1 132.2(5) . . ? 
Cu2 O37 Cu1 99.7(2) . . ? 
F41 B39 F43 110.2(9) . . ? 
F41 B39 F40 112.0(10) . . ? 
F43 B39 F40 109.7(9) . . ? 
F41 B39 F42 109.2(9) . . ? 
F43 B39 F42 109.1(9) . . ? 
F40 B39 F42 106.6(9) . . ? 
B39 F40 Cu2 114.7(7) . . ? 
B39 F42 Cu1 139.9(6) . . ? 
F46A B44 F45 106.5(12) . . ? 
F46B B44 F45 124.4(12) . . ? 
F46A B44 F48A 114.5(12) . . ? 
F45 B44 F48A 107.7(8) . . ? 
F45 B44 F47C 109.8(12) . . ?  
F45 B44 F46C 115.6(11) . . ? 
F47C B44 F46C 109.9(14) . . ? 
F46A B44 F47A 113.7(13) . . ? 
F45 B44 F47A 100.6(9) . . ? 
F48A B44 F47A 112.5(10) . . ? 
F46B B44 F48B 105.1(12) . . ? 
F45 B44 F48B 104.4(9) . . ? 
F45 B44 F48C 107.3(15) . . ?  
F47C B44 F48C 107.2(15) . . ? 
F46C B44 F48C 106.7(15) . . ? 
F46B B44 F47B 104.3(13) . . ? 
F45 B44 F47B 110.3(12) . . ? 
F48B B44 F47B 107.3(13) . . ? 
O51 N50 O52 122.4(16) . . ? 
O51 N50 C49 119.4(16) . . ? 
O52 N50 C49 118.1(15) . . ? 
 
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 
O20 H20 F45  0.82 2.32 2.961(10) 135.3 2_756 
O20 H20 F48A  0.82 2.09 2.847(14) 152.9 2_756 
O20 H20 F48B  0.82 1.94 2.739(18) 163.3 2_756 
O38 H38 O20  0.82 1.92 2.731(9) 171.6 1_466 
 
_diffrn_measured_fraction_theta_max    0.995 
_diffrn_reflns_theta_full              22.49 
_diffrn_measured_fraction_theta_full   0.995 
_refine_diff_density_max    1.066 
_refine_diff_density_min   -0.772 
_refine_diff_density_rms    0.113 


#=END

 
data_mh9803a/PL2 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
[N-(2-{pyrid-2-ylmethylamino}ethyl)-2,5-dihydroxybenzaldimino]copper(II) 
perchlorate
; 
_chemical_name_common             ? 
_chemical_formula_moiety          
'[C15 H16 N3 O2 Cu] Cl O4' 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C15 H16 Cl Cu N3 O6' 
_chemical_formula_weight          433.30 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
 
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    P2(1)/c
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
 
_cell_length_a                    7.683(1) 
_cell_length_b                    11.404(1) 
_cell_length_c                    19.242(1) 
_cell_angle_alpha                 90.000 
_cell_angle_beta                  99.56(1) 
_cell_angle_gamma                 90.000 
_cell_volume                      1662.5(3) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     180(2) 
_cell_measurement_reflns_used     25 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             red 
_exptl_crystal_size_max           0.45 
_exptl_crystal_size_mid           0.32 
_exptl_crystal_size_min           0.30 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.731 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              884 
_exptl_absorpt_coefficient_mu     1.514 
_exptl_absorpt_correction_type    none 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
 
_exptl_special_details 
; 
 Crystal lost before psi scans could be done.  
; 
 
_diffrn_ambient_temperature       180
_diffrn_radiation_wavelength      0.71069 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        'Stoe STADI4 '
_diffrn_measurement_method        ? 
_diffrn_standards_number          3
_diffrn_standards_interval_count  200 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             11232 
_diffrn_reflns_av_R_equivalents   0.0764 
_diffrn_reflns_av_sigmaI/netI     0.0484 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -22 
_diffrn_reflns_limit_l_max        22 
_diffrn_reflns_theta_min          3.54 
_diffrn_reflns_theta_max          24.92 
_reflns_number_total              2891 
_reflns_number_observed           2216 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        'Siemens XSCANS' 
_computing_cell_refinement        'Siemens XSCANS' 
_computing_data_reduction         'Siemens SHELXTL' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Siemens SHELXTL' 
_computing_publication_material   'Siemens SHELXTL' 

_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 pyCH~2~NHC~2~H~4 portion of the ligand, and the anion O atoms, are 
 both disordered over two orientations:
 C3A-C10A and O23-O26, occupany 0.7
 C3B-C10B and O27-O30, occupancy 0.3.

 The following restraints were applied:
 N2-C3A, N2-C7A, N2-C3B, N2-C7B = 1.34(2)\%A
 C3A-C4A, C4A-C5A, C5A-C6A, C6A-C7A, C3B-C4B, C4B-C5B, C5B-C6B, C6B-C7B = 
 1.37(2)\%A
 C3A...C7A, C3B...C7B = 2.32(1)\%A
 C3A...C5A, C4A...C6A, C5A...C7A, C3B...C5B, C4B...C6B, C5B...C7B = 2.37(1)\%A
 C7A-C8A, C10A-C11, C7B-C8B, C10B-C11 = 1.51(2)\%A
 C8A-N9A, N9A-C10A, C8B-N9B, N9B-C10B = 1.50(2)\%A

 All Cl-O bonds and O...O distances within the anion restrained to be the same 
 to
 within an esd of 0.03\%A.

 All non-H atoms with occupancy >0.5 were refined anisotropically.
; 
  
_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^)+(0.0342P)^2^+5.0480P] 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          2891 
_refine_ls_number_parameters      288 
_refine_ls_number_restraints      128 
_refine_ls_R_factor_all           0.0871 
_refine_ls_R_factor_gt            0.0635 
_refine_ls_wR_factor_ref          0.1452 
_refine_ls_wR_factor_gt           0.1344 
_refine_ls_goodness_of_fit_ref    1.129 
_refine_ls_restrained_S_all       1.185 
_refine_ls_shift/su_max           0.028 
_refine_ls_shift/su_mean          0.002 
 
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 0.21832(11) 0.04337(7) 0.53728(4) 0.0512(3) Uani 1 1 d . . . 
N2 N 0.1703(6) -0.1050(5) 0.5827(2) 0.0469(12) Uani 1 1 d D A . 
C3A C 0.194(7) -0.2131(12) 0.5584(14) 0.055(14) Uani 0.70 1 d PD A 1 
H3A H 0.2388 -0.2207 0.5167 0.066 Uiso 0.70 1 calc PR A 1 
C4A C 0.154(6) -0.3135(13) 0.5924(15) 0.064(12) Uani 0.70 1 d PD A 1 
H4A H 0.1663 -0.3871 0.5729 0.077 Uiso 0.70 1 calc PR A 1 
C5A C 0.096(4) -0.3020(12) 0.6564(13) 0.096(11) Uani 0.70 1 d PD A 1 
H5A H 0.0712 -0.3683 0.6812 0.115 Uiso 0.70 1 calc PR A 1 
C6A C 0.075(4) -0.1935(15) 0.6828(10) 0.076(9) Uani 0.70 1 d PD A 1 
H6A H 0.0351 -0.1851 0.7257 0.091 Uiso 0.70 1 calc PR A 1 
C7A C 0.112(4) -0.0954(10) 0.6454(10) 0.059(9) Uani 0.70 1 d PD A 1 
C8A C 0.102(2) 0.0290(10) 0.6720(8) 0.053(7) Uani 0.70 1 d PD A 1 
H8A1 H -0.0037 0.0386 0.6929 0.064 Uiso 0.70 1 calc PR A 1 
H8A2 H 0.2035 0.0451 0.7079 0.064 Uiso 0.70 1 calc PR A 1 
N9A N 0.0982(10) 0.1114(6) 0.6133(4) 0.0533(19) Uani 0.70 1 d PD A 1 
H9A H -0.0157 0.1291 0.5951 0.064 Uiso 0.70 1 calc PR A 1 
C10A C 0.1968(14) 0.2188(9) 0.6309(5) 0.065(3) Uani 0.70 1 d PD A 1 
H10A H 0.3124 0.1998 0.6570 0.078 Uiso 0.70 1 calc PR A 1 
H10B H 0.1359 0.2667 0.6609 0.078 Uiso 0.70 1 calc PR A 1 
C3B C 0.184(16) -0.211(2) 0.557(3) 0.04(3) Uiso 0.30 1 d PD A 2 
H3B H 0.2074 -0.2199 0.5110 0.054 Uiso 0.30 1 calc PR A 2 
C4B C 0.165(15) -0.308(3) 0.597(3) 0.07(3) Uiso 0.30 1 d PD A 2 
H4B H 0.1881 -0.3829 0.5810 0.084 Uiso 0.30 1 calc PR A 2 
C5B C 0.109(8) -0.2930(18) 0.661(3) 0.062(15) Uiso 0.30 1 d PD A 2 
H5B H 0.0836 -0.3575 0.6870 0.074 Uiso 0.30 1 calc PR A 2 
C6B C 0.092(9) -0.182(2) 0.685(2) 0.065(18) Uiso 0.30 1 d PD A 2 
H6B H 0.0602 -0.1702 0.7295 0.078 Uiso 0.30 1 calc PR A 2 
C7B C 0.122(9) -0.0866(14) 0.645(2) 0.043(16) Uiso 0.30 1 d PD A 2 
C8B C 0.091(6) 0.0392(17) 0.666(3) 0.08(2) Uiso 0.30 1 d PD A 2 
H8B1 H -0.0300 0.0619 0.6481 0.091 Uiso 0.30 1 calc PR A 2 
H8B2 H 0.1108 0.0462 0.7168 0.091 Uiso 0.30 1 calc PR A 2 
N9B N 0.215(2) 0.1173(11) 0.6356(8) 0.039(4) Uiso 0.30 1 d PD A 2 
H9B H 0.3236 0.1243 0.6628 0.046 Uiso 0.30 1 calc PR A 2 
C10B C 0.123(3) 0.2335(17) 0.6157(13) 0.053(8) Uiso 0.30 1 d PD A 2 
H10C H 0.0006 0.2204 0.5951 0.064 Uiso 0.30 1 calc PR A 2 
H10D H 0.1269 0.2828 0.6570 0.064 Uiso 0.30 1 calc PR A 2 
C11 C 0.2187(10) 0.2893(6) 0.5642(3) 0.0623(18) Uani 1 1 d D . . 
H11A H 0.1103 0.3304 0.5457 0.075 Uiso 1 1 calc R A 1 
H11B H 0.3131 0.3463 0.5750 0.075 Uiso 1 1 calc R A 1 
N12 N 0.2616(6) 0.2021(4) 0.5127(3) 0.0480(12) Uani 1 1 d . A . 
C13 C 0.3191(8) 0.2348(6) 0.4569(3) 0.0501(15) Uani 1 1 d . . . 
H13 H 0.3381 0.3146 0.4514 0.060 Uiso 1 1 calc R A . 
C14 C 0.3566(7) 0.1571(5) 0.4020(3) 0.0431(13) Uani 1 1 d . A . 
C15 C 0.3339(7) 0.0325(6) 0.4039(3) 0.0438(13) Uani 1 1 d . . . 
C16 C 0.3732(7) -0.0301(6) 0.3464(3) 0.0477(14) Uani 1 1 d . A . 
H16 H 0.3613 -0.1112 0.3461 0.057 Uiso 1 1 calc R . . 
C17 C 0.4287(7) 0.0233(7) 0.2898(3) 0.0550(17) Uani 1 1 d . . . 
H17 H 0.4515 -0.0219 0.2520 0.066 Uiso 1 1 calc R A . 
C18 C 0.4512(8) 0.1438(7) 0.2886(3) 0.0566(17) Uani 1 1 d . A . 
C19 C 0.4145(8) 0.2091(6) 0.3435(3) 0.0537(16) Uani 1 1 d . . . 
H19 H 0.4280 0.2901 0.3424 0.064 Uiso 1 1 calc R A . 
O20 O 0.2737(5) -0.0238(3) 0.45502(19) 0.0460(9) Uani 1 1 d . A . 
O21 O 0.5077(7) 0.2002(5) 0.2327(3) 0.0799(16) Uani 1 1 d . . . 
H21 H 0.5444 0.1516 0.2072 0.120 Uiso 1 1 calc R A . 
Cl22 Cl 0.2450(3) -0.42470(15) 0.38962(10) 0.0718(6) Uani 1 1 d D . . 
O23 O 0.3834(16) -0.4764(12) 0.3611(7) 0.110(5) Uani 0.70 1 d PD B 3 
O24 O 0.264(2) -0.3031(6) 0.3974(7) 0.117(6) Uani 0.70 1 d PD B 3 
O25 O 0.0791(11) -0.4466(8) 0.3381(5) 0.103(3) Uani 0.70 1 d PD B 3 
O26 O 0.2084(13) -0.4791(7) 0.4501(4) 0.093(3) Uani 0.70 1 d PD B 3 
O27 O 0.339(3) -0.445(2) 0.4591(7) 0.114(8) Uiso 0.30 1 d PD B 4 
O28 O 0.236(4) -0.3007(12) 0.3785(15) 0.090(10) Uiso 0.30 1 d PD B 4 
O29 O 0.077(2) -0.472(2) 0.3819(13) 0.121(9) Uiso 0.30 1 d PD B 4 
O30 O 0.343(3) -0.476(3) 0.3406(12) 0.087(10) Uiso 0.30 1 d PD B 4 
 
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 0.0659(5) 0.0502(5) 0.0418(4) 0.0001(4) 0.0217(3) 0.0109(4) 
N2 0.041(3) 0.062(3) 0.039(3) 0.002(2) 0.009(2) -0.003(2) 
C3A 0.043(15) 0.075(19) 0.048(13) 0.001(5) 0.008(6) -0.018(6) 
C4A 0.073(15) 0.066(15) 0.050(10) 0.009(5) 0.000(7) -0.029(9) 
C5A 0.106(15) 0.122(17) 0.056(9) 0.024(8) 0.002(7) -0.069(12) 
C6A 0.062(10) 0.131(19) 0.039(7) 0.005(7) 0.018(6) -0.044(10) 
C7A 0.031(7) 0.103(16) 0.044(8) 0.003(6) 0.010(4) -0.008(6) 
C8A 0.040(7) 0.093(13) 0.031(6) 0.003(5) 0.020(4) 0.010(6) 
N9A 0.051(5) 0.063(5) 0.047(4) -0.007(4) 0.010(4) 0.010(4) 
C10A 0.034(6) 0.107(10) 0.053(6) -0.042(6) 0.005(5) -0.014(6) 
C11 0.078(5) 0.047(4) 0.060(4) -0.019(3) 0.006(4) 0.005(3) 
N12 0.047(3) 0.048(3) 0.048(3) -0.010(2) 0.005(2) 0.000(2) 
C13 0.049(4) 0.043(3) 0.057(4) 0.002(3) 0.008(3) -0.004(3) 
C14 0.034(3) 0.051(4) 0.045(3) 0.003(3) 0.009(2) -0.001(3) 
C15 0.040(3) 0.054(4) 0.039(3) 0.002(3) 0.010(2) 0.006(3) 
C16 0.047(3) 0.049(4) 0.051(3) -0.003(3) 0.017(3) 0.000(3) 
C17 0.040(3) 0.086(5) 0.043(3) -0.002(3) 0.017(3) 0.002(3) 
C18 0.049(4) 0.078(5) 0.045(3) 0.014(3) 0.016(3) -0.006(3) 
C19 0.046(3) 0.057(4) 0.059(4) 0.012(3) 0.008(3) -0.005(3) 
O20 0.053(2) 0.046(2) 0.042(2) -0.0041(19) 0.0194(18) -0.004(2) 
O21 0.084(4) 0.102(4) 0.060(3) 0.025(3) 0.030(3) -0.006(3) 
Cl22 0.1129(16) 0.0500(10) 0.0622(10) -0.0024(8) 0.0425(11) -0.0087(10) 
O23 0.127(10) 0.095(8) 0.127(10) -0.026(8) 0.083(9) -0.007(7) 
O24 0.212(15) 0.047(5) 0.115(10) -0.033(5) 0.094(9) -0.055(6) 
O25 0.140(8) 0.078(6) 0.085(6) -0.010(5) 0.003(5) -0.019(5) 
O26 0.147(8) 0.079(6) 0.069(5) 0.012(4) 0.059(5) 0.008(6) 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Cu1 O20 1.870(4) . ? 
Cu1 N12 1.915(5) . ? 
Cu1 N2 1.967(5) . ? 
Cu1 N9A 2.010(7) . ? 
Cu1 N9B 2.075(16) . ? 
N2 C3B 1.320(19) . ? 
N2 C7B 1.326(18) . ? 
N2 C3A 1.341(13) . ? 
N2 C7A 1.361(11) . ? 
C3A C4A 1.378(13) . ? 
C4A C5A 1.385(12) . ? 
C5A C6A 1.357(14) . ? 
C6A C7A 1.386(13) . ? 
C7A C8A 1.515(12) . ? 
C8A N9A 1.465(14) . ? 
N9A C10A 1.450(10) . ? 
C10A C11 1.547(10) . ? 
C3B C4B 1.37(2) . ? 
C4B C5B 1.383(18) . ? 
C5B C6B 1.368(18) . ? 
C6B C7B 1.38(2) . ? 
C7B C8B 1.52(2) . ? 
C8B N9B 1.49(2) . ? 
N9B C10B 1.521(17) . ? 
C10B C11 1.472(17) . ? 
C11 N12 1.480(7) . ? 
N12 C13 1.282(7) . ? 
C13 C14 1.446(8) . ? 
C14 C19 1.408(8) . ? 
C14 C15 1.432(8) . ? 
C15 O20 1.320(6) . ? 
C15 C16 1.392(8) . ? 
C16 C17 1.376(8) . ? 
C17 C18 1.386(10) . ? 
C18 C19 1.360(9) . ? 
C18 O21 1.383(7) . ? 
Cl22 O29 1.384(12) . ? 
Cl22 O26 1.388(6) . ? 
Cl22 O24 1.399(7) . ? 
Cl22 O23 1.405(7) . ? 
Cl22 O30 1.424(12) . ? 
Cl22 O27 1.428(12) . ? 
Cl22 O28 1.430(12) . ? 
Cl22 O25 1.500(8) . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O20 Cu1 N12 96.02(18) . . ? 
O20 Cu1 N2 96.29(18) . . ? 
N12 Cu1 N2 167.5(2) . . ? 
O20 Cu1 N9A 166.0(3) . . ? 
N12 Cu1 N9A 86.2(2) . . ? 
N2 Cu1 N9A 82.3(2) . . ? 
O20 Cu1 N9B 167.6(5) . . ? 
N12 Cu1 N9B 82.5(3) . . ? 
N2 Cu1 N9B 85.0(3) . . ? 
N9A Cu1 N9B 26.3(4) . . ? 
C3B N2 C7B 122.6(17) . . ? 
C3B N2 C3A 3(8) . . ? 
C7B N2 C3A 122.2(11) . . ? 
C3B N2 C7A 118.0(17) . . ? 
C7B N2 C7A 5(2) . . ? 
C3A N2 C7A 117.8(9) . . ? 
C3B N2 Cu1 125.9(15) . . ? 
C7B N2 Cu1 111.5(7) . . ? 
C3A N2 Cu1 126.2(7) . . ? 
C7A N2 Cu1 116.1(6) . . ? 
N2 C3A C4A 123.1(9) . . ? 
C3A C4A C5A 118.2(10) . . ? 
C6A C5A C4A 119.7(8) . . ? 
C5A C6A C7A 119.6(9) . . ? 
N2 C7A C6A 121.5(8) . . ? 
N2 C7A C8A 114.6(8) . . ? 
C6A C7A C8A 123.7(10) . . ? 
N9A C8A C7A 109.7(11) . . ? 
C10A N9A C8A 114.8(9) . . ? 
C10A N9A Cu1 102.2(5) . . ? 
C8A N9A Cu1 111.2(6) . . ? 
N9A C10A C11 111.7(7) . . ? 
N2 C3B C4B 120.3(18) . . ? 
C3B C4B C5B 118.5(17) . . ? 
C6B C5B C4B 119.1(12) . . ? 
C5B C6B C7B 120.0(17) . . ? 
N2 C7B C6B 119.0(14) . . ? 
N2 C7B C8B 118(2) . . ? 
C6B C7B C8B 122.9(19) . . ? 
N9B C8B C7B 108.7(18) . . ? 
C8B N9B C10B 108.4(14) . . ? 
C8B N9B Cu1 102.6(19) . . ? 
C10B N9B Cu1 101.5(12) . . ? 
C11 C10B N9B 106.4(13) . . ? 
C10B C11 N12 110.6(10) . . ? 
C10B C11 C10A 23.4(8) . . ? 
N12 C11 C10A 105.9(6) . . ? 
C13 N12 C11 120.8(5) . . ? 
C13 N12 Cu1 125.4(4) . . ? 
C11 N12 Cu1 113.7(4) . . ? 
N12 C13 C14 124.9(6) . . ? 
C19 C14 C15 119.7(5) . . ? 
C19 C14 C13 117.0(6) . . ? 
C15 C14 C13 123.3(5) . . ? 
O20 C15 C16 119.5(6) . . ? 
O20 C15 C14 124.1(5) . . ? 
C16 C15 C14 116.3(5) . . ? 
C17 C16 C15 122.7(6) . . ? 
C16 C17 C18 120.5(6) . . ? 
C19 C18 O21 118.8(7) . . ? 
C19 C18 C17 119.2(6) . . ? 
O21 C18 C17 122.0(6) . . ? 
C18 C19 C14 121.6(6) . . ? 
C15 O20 Cu1 126.0(4) . . ? 
O26 Cl22 O24 112.7(6) . . ? 
O26 Cl22 O23 114.3(7) . . ? 
O24 Cl22 O23 112.6(6) . . ? 
O29 Cl22 O30 110.6(11) . . ? 
O29 Cl22 O27 110.6(10) . . ? 
O30 Cl22 O27 108.2(10) . . ? 
O29 Cl22 O28 110.5(11) . . ? 
O30 Cl22 O28 108.9(11) . . ? 
O27 Cl22 O28 107.9(10) . . ? 
O26 Cl22 O25 102.2(5) . . ? 
O24 Cl22 O25 107.4(7) . . ? 
O23 Cl22 O25 106.6(7) . . ? 

 
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 
N9A H9A O20  0.91 2.38 3.106(9) 136.6 3_556 
N9A H9A O24  0.91 2.77 3.520(16) 139.9 3_556 
N9B H9B O21  0.91 2.68 3.388(18) 135.2 4_566 
O21 H21 O23  0.82 2.10 2.918(14) 175.3 2_655 
O21 H21 O28  0.82 2.61 3.14(3) 124.1 2_655 
O21 H21 O30  0.82 1.99 2.81(3) 170.8 2_655 
 
_diffrn_measured_fraction_theta_max    0.996 
_diffrn_reflns_theta_full              24.92 
_diffrn_measured_fraction_theta_full   0.996 
_refine_diff_density_max    0.544 
_refine_diff_density_min   -0.901 
_refine_diff_density_rms    0.078