Electronic Supplementary Material for CrystEngComm
This journal is (c) The Royal Society of Chemistry 2007

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'M. Hardie'
_publ_contact_author_address     
;
School of Chemistry
University of Leeds
Woodhouse Lane
Leeds
LS2 9JT
UNITED KINGDOM
;

_publ_contact_author_email       M.J.HARDIE@LEEDS.AC.UK

_publ_section_title              
;
Network structures with 2,2'-bipyridine-3,3'diol: a
discrete Co(III) complex that forms a porous 3-D hydrogen bonded
network, and Cu(II) coordination chains.
;
loop_
_publ_author_name
'M. Hardie'
'Maria D. Stephenson'
#######################################################################

#Complex 1

data_1
_database_code_depnum_ccdc_archive 'CCDC 629297'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            
"tris(2,2'-bipyridine-3,3-diol-H)cobalt(iii) hydrate"
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H23 Co N6 O7'
_chemical_formula_weight         638.47

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   P-31c

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

_cell_length_a                   14.2158(4)
_cell_length_b                   14.2158(4)
_cell_length_c                   9.4244(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1649.40(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             656
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8656
_exptl_absorpt_correction_T_max  0.9503
_exptl_absorpt_process_details   SORTAV

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8029
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.95
_diffrn_reflns_theta_max         27.48
_reflns_number_total             1265
_reflns_number_gt                1188
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Nonius)'
_computing_cell_refinement       'DENZO (Nonius)'
_computing_data_reduction        'DENZO (Nonius)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-Seed, (Barbour)'
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The OH hydrogen of the bpydiol-H diol ligand was fully refined, while the H
on the water was constrained to the position that it originally appeared in
the difference map and given a Uiso of 1.5x that of the water O atom.
;

_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^)+(0.1152P)^2^+2.7023P] 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         1265
_refine_ls_number_parameters     70
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0575
_refine_ls_wR_factor_ref         0.2173
_refine_ls_wR_factor_gt          0.2134
_refine_ls_goodness_of_fit_ref   1.257
_refine_ls_restrained_S_all      1.257
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.3333 0.6667 0.2500 0.0181(4) Uani 1 6 d S . .
O1 O 0.6053(2) 0.5266(2) 0.3295(3) 0.0330(6) Uani 1 1 d . . .
N1 N 0.4474(2) 0.66315(19) 0.3571(3) 0.0205(6) Uani 1 1 d . . .
H1 H 0.553(4) 0.447(4) 0.2500 0.08(3) Uiso 1 2 d S . .
O2 O 0.8923(10) 0.785(2) 0.7500 0.097(7) Uiso 0.33 2 d SP . .
H2 H 0.8432 0.8240 0.7512 0.145 Uiso 0.33 1 d P . .
C2 C 0.4773(2) 0.5912(2) 0.3088(3) 0.0206(7) Uani 1 1 d . . .
C3 C 0.5681(3) 0.5900(3) 0.3715(3) 0.0252(7) Uani 1 1 d . . .
C4 C 0.6206(3) 0.6623(3) 0.4848(4) 0.0290(8) Uani 1 1 d . . .
H4 H 0.6813 0.6636 0.5291 0.035 Uiso 1 1 calc R . .
C5 C 0.5857(3) 0.7307(3) 0.5319(4) 0.0286(7) Uani 1 1 d . . .
H5 H 0.6210 0.7780 0.6096 0.034 Uiso 1 1 calc R . .
C6 C 0.4988(2) 0.7306(2) 0.4659(3) 0.0240(7) Uani 1 1 d . . .
H6 H 0.4752 0.7788 0.4979 0.029 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0180(4) 0.0180(4) 0.0184(6) 0.000 0.000 0.0090(2)
O1 0.0364(13) 0.0444(15) 0.0316(13) -0.0081(11) -0.0072(10) 0.0304(12)
N1 0.0208(12) 0.0194(12) 0.0205(12) -0.0010(8) -0.0005(9) 0.0095(10)
C2 0.0209(14) 0.0222(14) 0.0191(14) 0.0002(11) -0.0002(11) 0.0111(12)
C3 0.0259(15) 0.0293(15) 0.0238(14) 0.0004(12) -0.0006(11) 0.0163(13)
C4 0.0283(16) 0.0337(18) 0.0286(16) -0.0029(13) -0.0082(13) 0.0182(14)
C5 0.0300(16) 0.0287(16) 0.0261(15) -0.0050(12) -0.0081(12) 0.0140(13)
C6 0.0248(15) 0.0237(15) 0.0232(14) -0.0032(11) -0.0031(11) 0.0118(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
Co1 N1 1.932(3) 2_665 ?
Co1 N1 1.932(3) 5 ?
Co1 N1 1.932(3) 6_565 ?
Co1 N1 1.932(3) 3_565 ?
Co1 N1 1.932(3) . ?
Co1 N1 1.932(3) 4_665 ?
O1 C3 1.313(4) . ?
O1 H1 1.25(3) . ?
N1 C6 1.343(4) . ?
N1 C2 1.367(4) . ?
O2 H2 1.092(11) . ?
C2 C3 1.427(4) . ?
C2 C2 1.475(6) 4_665 ?
C3 C4 1.410(5) . ?
C4 C5 1.368(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.383(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?

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 Co1 N1 86.73(15) 2_665 5 ?
N1 Co1 N1 82.92(15) 2_665 6_565 ?
N1 Co1 N1 95.20(10) 5 6_565 ?
N1 Co1 N1 95.20(10) 2_665 3_565 ?
N1 Co1 N1 82.92(15) 5 3_565 ?
N1 Co1 N1 177.43(14) 6_565 3_565 ?
N1 Co1 N1 95.20(10) 2_665 . ?
N1 Co1 N1 177.43(14) 5 . ?
N1 Co1 N1 86.73(15) 6_565 . ?
N1 Co1 N1 95.20(10) 3_565 . ?
N1 Co1 N1 177.43(14) 2_665 4_665 ?
N1 Co1 N1 95.20(10) 5 4_665 ?
N1 Co1 N1 95.20(10) 6_565 4_665 ?
N1 Co1 N1 86.73(15) 3_565 4_665 ?
N1 Co1 N1 82.92(15) . 4_665 ?
C3 O1 H1 123(4) . . ?
C6 N1 C2 121.8(3) . . ?
C6 N1 Co1 123.0(2) . . ?
C2 N1 Co1 115.11(19) . . ?
N1 C2 C3 119.5(3) . . ?
N1 C2 C2 113.23(16) . 4_665 ?
C3 C2 C2 127.27(17) . 4_665 ?
O1 C3 C4 118.7(3) . . ?
O1 C3 C2 124.1(3) . . ?
C4 C3 C2 117.2(3) . . ?
C5 C4 C3 121.1(3) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C5 C6 119.7(3) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
N1 C6 C5 120.7(3) . . ?
N1 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.114

#===END

#Compound 1a

data_1a
_database_code_depnum_ccdc_archive 'CCDC 629298'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;

;
_chemical_name_common            tris(2,2'-bipyridine-3,3'-diol-H)cobalt(iii)
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H21 Co N6 O6'
_chemical_formula_weight         620.46

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   P-31c

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

_cell_length_a                   14.311(2)
_cell_length_b                   14.311(2)
_cell_length_c                   9.5165(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1687.8(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             636
_exptl_absorpt_coefficient_mu    0.555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9116
_exptl_absorpt_correction_T_max  0.9364
_exptl_absorpt_process_details   SORTAV

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11083
_diffrn_reflns_av_R_equivalents  0.0948
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.92
_diffrn_reflns_theta_max         27.45
_reflns_number_total             1291
_reflns_number_gt                1207
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Nonius)'
_computing_cell_refinement       'DENZO (Nonius)'
_computing_data_reduction        'DENZO (Nonius)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour)'
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The OH hydrogen of the ligand has been fully refined. There was diffuse
residual electron density which could not be meaningfully modelled as
solvent.
;

_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1291
_refine_ls_number_parameters     68
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1372
_refine_ls_R_factor_gt           0.1321
_refine_ls_wR_factor_ref         0.4634
_refine_ls_wR_factor_gt          0.4540
_refine_ls_goodness_of_fit_ref   2.358
_refine_ls_restrained_S_all      2.358
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.6667 0.3333 0.2500 0.0260(9) Uani 1 6 d S . .
N1 N 0.7834(4) 0.4463(3) 0.3555(5) 0.0288(12) Uani 1 1 d . . .
C6 C 0.7671(4) 0.4963(4) 0.4648(6) 0.0344(13) Uani 1 1 d . . .
H6 H 0.6956 0.4730 0.4953 0.041 Uiso 1 1 calc R . .
C2 C 0.8844(4) 0.4757(4) 0.3074(5) 0.0298(13) Uani 1 1 d . . .
C5 C 0.8536(5) 0.5816(5) 0.5339(6) 0.0413(15) Uani 1 1 d . . .
H5 H 0.8417 0.6152 0.6126 0.050 Uiso 1 1 calc R . .
O1 O 1.0759(3) 0.6043(3) 0.3277(5) 0.0438(13) Uani 1 1 d . . .
C4 C 0.9565(5) 0.6162(5) 0.4858(7) 0.0383(15) Uani 1 1 d . . .
H4 H 1.0157 0.6757 0.5304 0.046 Uiso 1 1 calc R . .
C3 C 0.9761(4) 0.5652(4) 0.3714(6) 0.0349(13) Uani 1 1 d . . .
H1 H 1.08(2) 0.540(12) 0.2500 0.14(7) Uiso 1 2 d S . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0220(10) 0.0220(10) 0.0340(12) 0.000 0.000 0.0110(5)
N1 0.027(2) 0.023(2) 0.036(2) -0.0006(16) 0.0010(16) 0.0123(18)
C6 0.033(3) 0.031(3) 0.042(3) -0.004(2) 0.002(2) 0.017(2)
C2 0.025(2) 0.028(2) 0.034(2) 0.0001(18) 0.0008(17) 0.012(2)
C5 0.040(3) 0.040(3) 0.045(3) -0.008(2) -0.002(2) 0.020(2)
O1 0.027(2) 0.041(2) 0.050(2) -0.0083(18) 0.0013(16) 0.0065(16)
C4 0.033(3) 0.035(3) 0.043(3) -0.010(2) -0.004(2) 0.014(2)
C3 0.030(3) 0.033(3) 0.036(2) -0.006(2) -0.0022(19) 0.011(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
Co1 N1 1.927(5) 6 ?
Co1 N1 1.927(5) 3_665 ?
Co1 N1 1.927(5) . ?
Co1 N1 1.927(5) 4_665 ?
Co1 N1 1.927(5) 5_655 ?
Co1 N1 1.927(5) 2_655 ?
N1 C6 1.346(7) . ?
N1 C2 1.367(6) . ?
C6 C5 1.394(8) . ?
C2 C3 1.432(7) . ?
C2 C2 1.453(9) 6 ?
C5 C4 1.376(8) . ?
O1 C3 1.314(7) . ?
C4 C3 1.415(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
N1 Co1 N1 86.8(2) 6 3_665 ?
N1 Co1 N1 82.7(3) 6 . ?
N1 Co1 N1 95.33(19) 3_665 . ?
N1 Co1 N1 95.33(19) 6 4_665 ?
N1 Co1 N1 82.7(3) 3_665 4_665 ?
N1 Co1 N1 177.2(2) . 4_665 ?
N1 Co1 N1 95.33(19) 6 5_655 ?
N1 Co1 N1 177.2(2) 3_665 5_655 ?
N1 Co1 N1 86.8(2) . 5_655 ?
N1 Co1 N1 95.33(19) 4_665 5_655 ?
N1 Co1 N1 177.2(2) 6 2_655 ?
N1 Co1 N1 95.33(19) 3_665 2_655 ?
N1 Co1 N1 95.33(19) . 2_655 ?
N1 Co1 N1 86.8(3) 4_665 2_655 ?
N1 Co1 N1 82.7(3) 5_655 2_655 ?
C6 N1 C2 122.2(4) . . ?
C6 N1 Co1 122.7(4) . . ?
C2 N1 Co1 115.0(3) . . ?
N1 C6 C5 121.0(5) . . ?
N1 C2 C3 119.2(4) . . ?
N1 C2 C2 113.4(3) . 6 ?
C3 C2 C2 127.4(3) . 6 ?
C4 C5 C6 118.7(5) . . ?
C5 C4 C3 121.5(5) . . ?
O1 C3 C4 118.5(5) . . ?
O1 C3 C2 124.1(5) . . ?
C4 C3 C2 117.4(5) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.953
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.206

#===END

#Compound 1b
data_1b
_database_code_depnum_ccdc_archive 'CCDC 629299'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            
"tris(2,2'-bipyridine-3,3-diol-H)cobalt(iii) hydrate"
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H23 Co N6 O7'
_chemical_formula_weight         638.47

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   P-31c

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

_cell_length_a                   14.1281(3)
_cell_length_b                   14.1281(3)
_cell_length_c                   9.4484(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1633.26(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    30(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             656
_exptl_absorpt_coefficient_mu    0.577
_exptl_absorpt_correction_type   multiscan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
Data collected to only 98% completion due to icing problems
;

_diffrn_ambient_temperature      30(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7876
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0496
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.72
_diffrn_reflns_theta_max         30.12
_reflns_number_total             1577
_reflns_number_gt                1201
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker-Nonius)'
_computing_cell_refinement       'SAINT (Bruker)'
_computing_data_reduction        'SAINT (Bruker)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour)'
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1375P)^2^+0.2202P] 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    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1577
_refine_ls_number_parameters     68
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0628
_refine_ls_wR_factor_ref         0.2086
_refine_ls_wR_factor_gt          0.1927
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.6667 0.3333 0.2500 0.0139(3) Uani 1 6 d S . .
O1 O 0.52650(18) 0.60992(18) 0.3270(2) 0.0231(5) Uani 1 1 d . . .
H1 H 0.4588 0.5412 0.2500 0.035 Uiso 1 2 d S . .
N1 N 0.66342(18) 0.44883(19) 0.3568(2) 0.0153(5) Uani 1 1 d . . .
O2 O 0.7957(7) 0.8979(4) 0.7500 0.0243(18) Uiso 0.33 2 d SP . .
H5 H 0.8279 0.9712 0.7182 0.036 Uiso 0.33 1 d P . .
C2 C 0.7317(2) 0.5008(2) 0.4655(2) 0.0177(5) Uani 1 1 d . . .
H2 H 0.7797 0.4764 0.4975 0.021 Uiso 1 1 calc R . .
C3 C 0.7332(2) 0.5903(2) 0.5321(3) 0.0198(6) Uani 1 1 d . . .
H3 H 0.7810 0.6257 0.6095 0.024 Uiso 1 1 calc R . .
C4 C 0.6640(3) 0.6261(2) 0.4834(3) 0.0213(6) Uani 1 1 d . . .
H4 H 0.6662 0.6880 0.5260 0.026 Uiso 1 1 calc R . .
C5 C 0.5899(2) 0.5718(2) 0.3705(3) 0.0186(6) Uani 1 1 d . . .
C6 C 0.5906(2) 0.4795(2) 0.3080(2) 0.0157(5) 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
Co1 0.0173(4) 0.0173(4) 0.0072(4) 0.000 0.000 0.00864(18)
O1 0.0359(12) 0.0312(12) 0.0132(9) -0.0032(7) -0.0044(8) 0.0251(10)
N1 0.0179(11) 0.0192(11) 0.0093(9) 0.0005(7) 0.0002(7) 0.0096(9)
C2 0.0210(13) 0.0222(13) 0.0107(10) -0.0013(9) -0.0011(9) 0.0115(11)
C3 0.0258(14) 0.0235(13) 0.0102(10) -0.0028(9) -0.0016(9) 0.0123(11)
C4 0.0296(15) 0.0251(14) 0.0128(11) -0.0028(9) -0.0024(10) 0.0164(12)
C5 0.0276(14) 0.0236(13) 0.0095(10) 0.0005(9) 0.0008(9) 0.0163(12)
C6 0.0204(12) 0.0205(13) 0.0085(9) 0.0001(8) -0.0003(9) 0.0119(11)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N1 1.938(2) 6 ?
Co1 N1 1.938(2) 3_665 ?
Co1 N1 1.938(2) 5_655 ?
Co1 N1 1.938(2) 2_655 ?
Co1 N1 1.938(2) 4_665 ?
Co1 N1 1.938(2) . ?
O1 C5 1.322(3) . ?
N1 C2 1.348(3) . ?
N1 C6 1.380(3) . ?
C2 C3 1.403(4) . ?
C3 C4 1.386(4) . ?
C4 C5 1.421(4) . ?
C5 C6 1.435(4) . ?
C6 C6 1.477(5) 4_665 ?

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 Co1 N1 86.39(13) 6 3_665 ?
N1 Co1 N1 95.37(9) 6 5_655 ?
N1 Co1 N1 82.91(13) 3_665 5_655 ?
N1 Co1 N1 82.91(13) 6 2_655 ?
N1 Co1 N1 95.37(9) 3_665 2_655 ?
N1 Co1 N1 177.65(13) 5_655 2_655 ?
N1 Co1 N1 95.37(9) 6 4_665 ?
N1 Co1 N1 177.65(13) 3_665 4_665 ?
N1 Co1 N1 95.37(8) 5_655 4_665 ?
N1 Co1 N1 86.39(13) 2_655 4_665 ?
N1 Co1 N1 177.65(13) 6 . ?
N1 Co1 N1 95.37(9) 3_665 . ?
N1 Co1 N1 86.39(13) 5_655 . ?
N1 Co1 N1 95.37(9) 2_655 . ?
N1 Co1 N1 82.91(13) 4_665 . ?
C2 N1 C6 121.8(2) . . ?
C2 N1 Co1 122.89(18) . . ?
C6 N1 Co1 115.18(16) . . ?
N1 C2 C3 121.1(2) . . ?
C4 C3 C2 119.0(2) . . ?
C3 C4 C5 121.1(3) . . ?
O1 C5 C4 118.7(2) . . ?
O1 C5 C6 123.8(2) . . ?
C4 C5 C6 117.5(2) . . ?
N1 C6 C5 119.5(2) . . ?
N1 C6 C6 113.12(14) . 4_665 ?
C5 C6 C6 127.43(15) . 4_665 ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        30.12
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         1.602
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.127

#===END

#Complex 2

data_2
_database_code_depnum_ccdc_archive 'CCDC 629300'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            
;tris(2,2'-bipyridine-3,3-diol-H)cobalt(iii) 1,2-
dibromobenzene clathrate
;
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H25 Br2 Co N6 O6'
_chemical_formula_weight         856.37

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   P-31c

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

_cell_length_a                   14.2706(5)
_cell_length_b                   14.2706(5)
_cell_length_c                   9.4516(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1666.94(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             856
_exptl_absorpt_coefficient_mu    2.970
_exptl_absorpt_correction_type   multiscan
_exptl_absorpt_correction_T_min  0.5123
_exptl_absorpt_correction_T_max  0.7759
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25702
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.71
_diffrn_reflns_theta_max         27.20
_reflns_number_total             1245
_reflns_number_gt                977
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2 (Bruker-Nonius)'
_computing_cell_refinement       'SAINT (Bruker)'
_computing_data_reduction        'SAINT (Bruker)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour)'
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The three largest residual electron density peaks that occur after refinement
of the [Co(bpydiol-H)3] moiety were assigned as partly occupied Br atoms.
The Uiso values for these positions were initially set at 0.08 and their
occupancies allowed to refine. This gave an overall Br occupancy of
approximately
two per [Co(bpydiol-H)3] molecule, as would be expected for the proposed
formula.
The Br occupancies were then set at levels to give exactly two Br per
[Co(bpydiol-H)3], and their displacement parameters were refined
anisotropically.
Further residual electron density peaks were assigned as disordered carbon
atoms and
refined isotropically. Hydrogen atoms were not included for the
1,2-dibromobenzene
due to its extreme disorder.
;

_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^)+(0.0585P)^2^+3.9865P] 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         1245
_refine_ls_number_parameters     95
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0495
_refine_ls_wR_factor_ref         0.1378
_refine_ls_wR_factor_gt          0.1250
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.3333 0.6667 0.2500 0.0152(3) Uani 1 6 d S . .
N1 N 0.44762(19) 0.66337(19) 0.3572(2) 0.0164(5) Uani 1 1 d . . .
O1 O 0.60634(19) 0.5273(2) 0.3286(2) 0.0305(6) Uani 1 1 d . . .
C4 C 0.6218(3) 0.6628(3) 0.4840(3) 0.0260(7) Uani 1 1 d . . .
H4 H 0.6825 0.6644 0.5277 0.031 Uiso 1 1 calc R . .
C6 C 0.4992(2) 0.7309(2) 0.4655(3) 0.0211(6) Uani 1 1 d . . .
H6 H 0.4758 0.7790 0.4972 0.025 Uiso 1 1 calc R . .
C3 C 0.5691(2) 0.5905(2) 0.3710(3) 0.0211(6) Uani 1 1 d . . .
C5 C 0.5864(3) 0.7311(3) 0.5317(3) 0.0254(7) Uani 1 1 d . . .
H5 H 0.6214 0.7781 0.6093 0.030 Uiso 1 1 calc R . .
C2 C 0.4779(2) 0.5916(2) 0.3088(3) 0.0176(6) Uani 1 1 d . . .
Br2 Br 0.8362(3) 0.8237(4) 0.7691(6) 0.0863(13) Uani 0.18 1 d P . .
Br3 Br 0.9032(5) 0.8063(9) 0.7500 0.103(6) Uani 0.14 2 d SP . .
C7 C 0.9699(7) 0.9397(15) 0.7500 0.225(11) Uiso 1 2 d S . .
Br1 Br 0.9226(18) 0.8207(8) 0.6690(14) 0.097(5) Uani 0.09 1 d P . .
C8 C 0.844(3) 0.9222(13) 0.7500 0.305(15) Uiso 1 2 d S . .
H(1) H 0.543(3) 0.457(3) 0.2500 0.08(2) Uiso 1 2 d S . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0139(3) 0.0139(3) 0.0177(5) 0.000 0.000 0.00696(16)
N1 0.0153(11) 0.0147(11) 0.0188(11) -0.0001(10) 0.0011(9) 0.0072(10)
O1 0.0314(13) 0.0424(14) 0.0312(13) -0.0101(11) -0.0092(10) 0.0287(12)
C4 0.0236(16) 0.0320(17) 0.0266(16) -0.0021(14) -0.0075(13) 0.0172(14)
C6 0.0200(14) 0.0187(14) 0.0243(16) -0.0022(12) -0.0027(12) 0.0095(12)
C3 0.0191(14) 0.0248(15) 0.0223(14) 0.0000(12) -0.0001(12) 0.0130(13)
C5 0.0242(16) 0.0240(16) 0.0247(16) -0.0058(13) -0.0069(13) 0.0096(13)
C2 0.0169(14) 0.0160(13) 0.0197(14) 0.0009(12) 0.0008(11) 0.0081(11)
Br2 0.0416(17) 0.078(2) 0.112(4) 0.014(2) -0.001(2) 0.0092(16)
Br3 0.132(13) 0.030(4) 0.113(13) 0.000 -0.009(14) 0.0152(19)
Br1 0.125(12) 0.031(4) 0.113(11) -0.038(6) -0.050(10) 0.023(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
Co1 N1 1.940(2) 5 ?
Co1 N1 1.940(2) 2_665 ?
Co1 N1 1.940(2) 6_565 ?
Co1 N1 1.940(2) 3_565 ?
Co1 N1 1.940(2) 4_665 ?
Co1 N1 1.940(2) . ?
N1 C6 1.345(4) . ?
N1 C2 1.374(4) . ?
O1 C3 1.317(4) . ?
C4 C5 1.379(4) . ?
C4 C3 1.413(4) . ?
C6 C5 1.392(4) . ?
C3 C2 1.435(4) . ?
C2 C2 1.489(6) 4_665 ?
Br2 Br1 1.08(2) 5_656 ?
Br2 Br3 1.115(6) . ?
Br2 C8 1.363(6) . ?
Br2 Br1 1.57(2) . ?
Br2 C7 1.804(15) . ?
Br2 Br2 2.189(10) 5_656 ?
Br2 Br2 2.719(10) 6_566 ?
Br3 Br1 0.805(16) 5_656 ?
Br3 Br1 0.805(16) . ?
Br3 Br2 1.115(6) 5_656 ?
Br3 C7 1.65(2) . ?
Br3 C8 2.196(13) 2_765 ?
Br3 C8 2.196(13) . ?
C7 C7 1.29(3) 2_765 ?
C7 C7 1.29(3) 3_675 ?
C7 Br1 1.667(18) . ?
C7 Br1 1.667(19) 5_656 ?
C7 C8 1.68(3) 2_765 ?
C7 C8 1.68(3) . ?
C7 Br2 1.804(15) 5_656 ?
Br1 Br2 1.08(2) 5_656 ?
Br1 Br1 1.57(3) 5_656 ?
Br1 C8 2.09(2) 2_765 ?
Br1 C8 2.36(2) . ?
C8 Br2 1.363(6) 6_566 ?
C8 C7 1.68(3) 3_675 ?
C8 Br1 2.09(2) 5_656 ?
C8 Br1 2.09(2) 3_675 ?
C8 Br3 2.196(13) 3_675 ?
C8 Br1 2.36(2) 6_566 ?

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 Co1 N1 86.57(14) 5 2_665 ?
N1 Co1 N1 95.23(9) 5 6_565 ?
N1 Co1 N1 83.00(14) 2_665 6_565 ?
N1 Co1 N1 83.00(14) 5 3_565 ?
N1 Co1 N1 95.23(9) 2_665 3_565 ?
N1 Co1 N1 177.59(14) 6_565 3_565 ?
N1 Co1 N1 95.23(9) 5 4_665 ?
N1 Co1 N1 177.59(14) 2_665 4_665 ?
N1 Co1 N1 95.23(9) 6_565 4_665 ?
N1 Co1 N1 86.57(14) 3_565 4_665 ?
N1 Co1 N1 177.59(14) 5 . ?
N1 Co1 N1 95.23(9) 2_665 . ?
N1 Co1 N1 86.57(14) 6_565 . ?
N1 Co1 N1 95.23(9) 3_565 . ?
N1 Co1 N1 83.00(14) 4_665 . ?
C6 N1 C2 121.6(2) . . ?
C6 N1 Co1 123.1(2) . . ?
C2 N1 Co1 115.18(19) . . ?
C5 C4 C3 120.9(3) . . ?
N1 C6 C5 120.9(3) . . ?
O1 C3 C4 118.7(3) . . ?
O1 C3 C2 124.1(3) . . ?
C4 C3 C2 117.2(3) . . ?
C4 C5 C6 119.6(3) . . ?
N1 C2 C3 119.8(3) . . ?
N1 C2 C2 113.09(16) . 4_665 ?
C3 C2 C2 127.14(17) . 4_665 ?
Br1 Br2 Br3 43.0(11) 5_656 . ?
Br1 Br2 C8 117.6(14) 5_656 . ?
Br3 Br2 C8 124.5(15) . . ?
Br1 Br2 Br1 69.9(12) 5_656 . ?
Br3 Br2 Br1 29.0(7) . . ?
C8 Br2 Br1 106.5(11) . . ?
Br1 Br2 C7 65.1(6) 5_656 . ?
Br3 Br2 C7 63.7(7) . . ?
C8 Br2 C7 62.2(15) . . ?
Br1 Br2 C7 58.7(5) . . ?
Br1 Br2 Br2 42.4(10) 5_656 5_656 ?
Br3 Br2 Br2 11.1(6) . 5_656 ?
C8 Br2 Br2 113.7(14) . 5_656 ?
Br1 Br2 Br2 27.5(6) . 5_656 ?
C7 Br2 Br2 52.6(4) . 5_656 ?
Br1 Br2 Br2 121.2(8) 5_656 6_566 ?
Br3 Br2 Br2 128.5(6) . 6_566 ?
C8 Br2 Br2 4.3(14) . 6_566 ?
Br1 Br2 Br2 109.6(5) . 6_566 ?
C7 Br2 Br2 66.5(4) . 6_566 ?
Br2 Br2 Br2 117.83(15) 5_656 6_566 ?
Br1 Br3 Br1 155(3) 5_656 . ?
Br1 Br3 Br2 108.8(17) 5_656 5_656 ?
Br1 Br3 Br2 66.0(16) . 5_656 ?
Br1 Br3 Br2 66.0(16) 5_656 . ?
Br1 Br3 Br2 108.8(17) . . ?
Br2 Br3 Br2 157.9(12) 5_656 . ?
Br1 Br3 C7 77.3(13) 5_656 . ?
Br1 Br3 C7 77.3(13) . . ?
Br2 Br3 C7 78.9(6) 5_656 . ?
Br2 Br3 C7 78.9(6) . . ?
Br1 Br3 C8 91.3(16) 5_656 2_765 ?
Br1 Br3 C8 72.0(15) . 2_765 ?
Br2 Br3 C8 30.8(9) 5_656 2_765 ?
Br2 Br3 C8 127.5(12) . 2_765 ?
C7 Br3 C8 49.3(9) . 2_765 ?
Br1 Br3 C8 72.0(15) 5_656 . ?
Br1 Br3 C8 91.3(16) . . ?
Br2 Br3 C8 127.5(12) 5_656 . ?
Br2 Br3 C8 30.8(9) . . ?
C7 Br3 C8 49.3(9) . . ?
C8 Br3 C8 98.6(17) 2_765 . ?
C7 C7 C7 60.000(5) 2_765 3_675 ?
C7 C7 Br3 150.000(2) 2_765 . ?
C7 C7 Br3 150.000(8) 3_675 . ?
C7 C7 Br1 135.3(8) 2_765 . ?
C7 C7 Br1 144.7(7) 3_675 . ?
Br3 C7 Br1 28.1(6) . . ?
C7 C7 Br1 144.7(7) 2_765 5_656 ?
C7 C7 Br1 135.3(8) 3_675 5_656 ?
Br3 C7 Br1 28.1(6) . 5_656 ?
Br1 C7 Br1 56.2(12) . 5_656 ?
C7 C7 C8 67.4(7) 2_765 2_765 ?
C7 C7 C8 127.4(7) 3_675 2_765 ?
Br3 C7 C8 82.6(7) . 2_765 ?
Br1 C7 C8 77.4(10) . 2_765 ?
Br1 C7 C8 89.5(11) 5_656 2_765 ?
C7 C7 C8 127.4(7) 2_765 . ?
C7 C7 C8 67.4(7) 3_675 . ?
Br3 C7 C8 82.6(7) . . ?
Br1 C7 C8 89.5(11) . . ?
Br1 C7 C8 77.4(10) 5_656 . ?
C8 C7 C8 165.2(15) 2_765 . ?
C7 C7 Br2 112.9(4) 2_765 5_656 ?
C7 C7 Br2 171.0(4) 3_675 5_656 ?
Br3 C7 Br2 37.4(4) . 5_656 ?
Br1 C7 Br2 35.9(8) . 5_656 ?
Br1 C7 Br2 53.7(9) 5_656 5_656 ?
C8 C7 Br2 45.9(5) 2_765 5_656 ?
C8 C7 Br2 119.4(11) . 5_656 ?
C7 C7 Br2 171.0(4) 2_765 . ?
C7 C7 Br2 112.9(4) 3_675 . ?
Br3 C7 Br2 37.4(4) . . ?
Br1 C7 Br2 53.7(9) . . ?
Br1 C7 Br2 35.9(8) 5_656 . ?
C8 C7 Br2 119.4(11) 2_765 . ?
C8 C7 Br2 45.9(5) . . ?
Br2 C7 Br2 74.7(8) 5_656 . ?
Br3 Br1 Br2 71.0(13) . 5_656 ?
Br3 Br1 Br1 12.7(13) . 5_656 ?
Br2 Br1 Br1 70.0(13) 5_656 5_656 ?
Br3 Br1 Br2 42.2(12) . . ?
Br2 Br1 Br2 110.0(11) 5_656 . ?
Br1 Br1 Br2 40.1(12) 5_656 . ?
Br3 Br1 C7 74.6(13) . . ?
Br2 Br1 C7 79.0(6) 5_656 . ?
Br1 Br1 C7 61.9(6) 5_656 . ?
Br2 Br1 C7 67.6(6) . . ?
Br3 Br1 C8 86.5(14) . 2_765 ?
Br2 Br1 C8 35.3(9) 5_656 2_765 ?
Br1 Br1 C8 78.6(12) 5_656 2_765 ?
Br2 Br1 C8 109.5(8) . 2_765 ?
C7 Br1 C8 51.6(10) . 2_765 ?
Br3 Br1 C8 68.8(15) . . ?
Br2 Br1 C8 117.5(9) 5_656 . ?
Br1 Br1 C8 60.6(13) 5_656 . ?
Br2 Br1 C8 33.7(6) . . ?
C7 Br1 C8 45.5(9) . . ?
C8 Br1 C8 96.8(16) 2_765 . ?
Br2 C8 Br2 171(3) . 6_566 ?
Br2 C8 C7 116.6(19) . 3_675 ?
Br2 C8 C7 71.9(12) 6_566 3_675 ?
Br2 C8 C7 71.9(12) . . ?
Br2 C8 C7 116.6(19) 6_566 . ?
C7 C8 C7 45.2(15) 3_675 . ?
Br2 C8 Br1 27.1(6) . 5_656 ?
Br2 C8 Br1 159.5(17) 6_566 5_656 ?
C7 C8 Br1 92.5(14) 3_675 5_656 ?
C7 C8 Br1 51.0(9) . 5_656 ?
Br2 C8 Br1 159.5(17) . 3_675 ?
Br2 C8 Br1 27.1(6) 6_566 3_675 ?
C7 C8 Br1 51.0(9) 3_675 3_675 ?
C7 C8 Br1 92.5(14) . 3_675 ?
Br1 C8 Br1 143(2) 5_656 3_675 ?
Br2 C8 Br3 163(2) . 3_675 ?
Br2 C8 Br3 24.7(6) 6_566 3_675 ?
C7 C8 Br3 48.1(8) 3_675 3_675 ?
C7 C8 Br3 93.3(14) . 3_675 ?
Br1 C8 Br3 136.1(15) 5_656 3_675 ?
Br1 C8 Br3 21.5(5) 3_675 3_675 ?
Br2 C8 Br3 24.7(6) . . ?
Br2 C8 Br3 163(2) 6_566 . ?
C7 C8 Br3 93.3(14) 3_675 . ?
C7 C8 Br3 48.1(8) . . ?
Br1 C8 Br3 21.5(5) 5_656 . ?
Br1 C8 Br3 136.1(15) 3_675 . ?
Br3 C8 Br3 141.4(17) 3_675 . ?
Br2 C8 Br1 146.0(13) . 6_566 ?
Br2 C8 Br1 39.8(6) 6_566 6_566 ?
C7 C8 Br1 45.1(8) 3_675 6_566 ?
C7 C8 Br1 87.0(13) . 6_566 ?
Br1 C8 Br1 119.8(13) 5_656 6_566 ?
Br1 C8 Br1 40.8(8) 3_675 6_566 ?
Br3 C8 Br1 20.0(4) 3_675 6_566 ?
Br3 C8 Br1 131.9(15) . 6_566 ?
Br2 C8 Br1 39.8(6) . . ?
Br2 C8 Br1 146.0(13) 6_566 . ?
C7 C8 Br1 87.0(13) 3_675 . ?
C7 C8 Br1 45.1(8) . . ?
Br1 C8 Br1 40.8(8) 5_656 . ?
Br1 C8 Br1 119.8(13) 3_675 . ?
Br3 C8 Br1 131.9(15) 3_675 . ?
Br3 C8 Br1 20.0(4) . . ?
Br1 C8 Br1 131.5(17) 6_566 . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.20
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.088

#===END

#Complex 3

data_3
_database_code_depnum_ccdc_archive 'CCDC 629301'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            
"(2,2'-bipyridine-3,3'-diol -H)chlorocopper(ii)"
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H7 Cl Cu N2 O2'
_chemical_formula_weight         286.17

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           Tetragonal
_symmetry_space_group_name_H-M   I4(1)/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   13.1259(3)
_cell_length_b                   13.1259(3)
_cell_length_c                   22.2808(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3838.74(16)
_cell_formula_units_Z            16
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.981
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2288
_exptl_absorpt_coefficient_mu    2.535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6872
_exptl_absorpt_correction_T_max  0.8040
_exptl_absorpt_process_details   SORTAV

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12365
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.59
_diffrn_reflns_theta_max         27.49
_reflns_number_total             2195
_reflns_number_gt                1855
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Nonius)'
_computing_cell_refinement       'DENZO (Nonius)'
_computing_data_reduction        'DENZO (Nonius)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour)'
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+8.2642P] 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         2195
_refine_ls_number_parameters     169
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0364
_refine_ls_wR_factor_ref         0.0949
_refine_ls_wR_factor_gt          0.0887
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.13268(3) 0.71075(3) 0.085357(15) 0.02404(14) Uani 1 1 d . . .
Cl1 Cl 0.08542(6) 0.85263(6) 0.03803(3) 0.02987(19) Uani 1 1 d . . .
O1 O 0.13156(18) 0.65190(18) 0.31945(9) 0.0335(5) Uani 1 1 d . . .
H1 H 0.1300 0.5916 0.3068 0.040 Uiso 1 1 calc R . .
N1 N 0.12057(18) 0.75965(18) 0.16917(11) 0.0237(5) Uani 1 1 d . . .
O1A O 0.08790(17) 0.48363(16) 0.27701(9) 0.0298(5) Uani 1 1 d . . .
N1A N 0.13256(18) 0.57888(18) 0.12680(10) 0.0223(5) Uani 1 1 d . . .
C2 C 0.1205(2) 0.6856(2) 0.21230(13) 0.0224(6) Uani 1 1 d . . .
C2A C 0.1194(2) 0.5804(2) 0.18741(12) 0.0211(5) Uani 1 1 d . . .
C3 C 0.1251(2) 0.7160(2) 0.27324(13) 0.0249(6) Uani 1 1 d . . .
C3A C 0.1059(2) 0.4868(2) 0.21855(13) 0.0240(6) Uani 1 1 d . . .
C4 C 0.1267(2) 0.8192(2) 0.28677(14) 0.0283(6) Uani 1 1 d . . .
H4 H 0.128(3) 0.835(3) 0.3218(16) 0.028(9) Uiso 1 1 d . . .
C4A C 0.1121(2) 0.3964(2) 0.18526(14) 0.0267(6) Uani 1 1 d . . .
H4A H 0.104(3) 0.343(3) 0.2045(16) 0.030(9) Uiso 1 1 d . . .
C5 C 0.1271(2) 0.8910(2) 0.24209(14) 0.0286(6) Uani 1 1 d . . .
H5 H 0.130(3) 0.959(3) 0.2503(16) 0.031(9) Uiso 1 1 d . . .
C5A C 0.1258(2) 0.3986(2) 0.12424(14) 0.0284(6) Uani 1 1 d . . .
H5A H 0.132(3) 0.340(3) 0.1038(18) 0.042(10) Uiso 1 1 d . . .
C6 C 0.1244(2) 0.8584(2) 0.18302(14) 0.0262(6) Uani 1 1 d . . .
H6 H 0.121(3) 0.906(3) 0.1499(17) 0.033(9) Uiso 1 1 d . . .
C6A C 0.1347(2) 0.4914(2) 0.09593(14) 0.0280(6) Uani 1 1 d . . .
H6A H 0.147(3) 0.497(3) 0.0544(17) 0.031(9) Uiso 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 0.0313(2) 0.0239(2) 0.0169(2) 0.00173(13) 0.00449(13) 0.00195(13)
Cl1 0.0363(4) 0.0278(4) 0.0256(4) 0.0053(3) -0.0018(3) 0.0004(3)
O1 0.0475(14) 0.0355(12) 0.0176(10) 0.0005(9) -0.0008(9) -0.0043(10)
N1 0.0253(12) 0.0246(12) 0.0212(12) 0.0014(9) 0.0023(9) 0.0001(9)
O1A 0.0395(12) 0.0328(11) 0.0170(9) 0.0057(8) -0.0013(9) -0.0042(9)
N1A 0.0254(12) 0.0253(12) 0.0163(11) 0.0007(9) 0.0021(9) 0.0009(9)
C2 0.0208(13) 0.0272(14) 0.0190(13) -0.0007(11) 0.0018(10) 0.0005(10)
C2A 0.0206(13) 0.0263(14) 0.0163(12) 0.0018(10) 0.0009(10) -0.0005(10)
C3 0.0216(13) 0.0342(15) 0.0188(14) -0.0015(12) 0.0013(10) -0.0029(11)
C3A 0.0231(13) 0.0278(14) 0.0211(13) 0.0038(11) -0.0031(11) 0.0008(10)
C4 0.0246(14) 0.0390(17) 0.0213(15) -0.0086(13) 0.0026(12) -0.0021(12)
C4A 0.0275(15) 0.0242(15) 0.0284(15) 0.0058(12) 0.0002(12) 0.0012(11)
C5 0.0260(14) 0.0286(16) 0.0313(16) -0.0072(13) 0.0015(12) -0.0009(11)
C5A 0.0325(16) 0.0232(14) 0.0295(15) -0.0025(12) 0.0018(12) 0.0012(12)
C6 0.0251(14) 0.0269(15) 0.0267(15) -0.0001(12) 0.0019(12) -0.0006(11)
C6A 0.0323(15) 0.0300(15) 0.0216(14) -0.0006(12) 0.0030(12) 0.0012(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 N1A 1.962(2) . ?
Cu1 O1A 1.963(2) 8_454 ?
Cu1 N1 1.981(2) . ?
Cu1 Cl1 2.2282(8) . ?
O1 C3 1.332(4) . ?
N1 C6 1.333(4) . ?
N1 C2 1.366(4) . ?
O1A C3A 1.324(3) . ?
O1A Cu1 1.963(2) 2 ?
N1A C6A 1.339(4) . ?
N1A C2A 1.362(3) . ?
C2 C3 1.416(4) . ?
C2 C2A 1.488(4) . ?
C2A C3A 1.422(4) . ?
C3 C4 1.389(4) . ?
C3A C4A 1.402(4) . ?
C4 C5 1.370(5) . ?
C4A C5A 1.372(4) . ?
C5 C6 1.384(4) . ?
C5A C6A 1.377(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1A Cu1 O1A 91.45(9) . 8_454 ?
N1A Cu1 N1 80.91(10) . . ?
O1A Cu1 N1 141.62(10) 8_454 . ?
N1A Cu1 Cl1 163.73(7) . . ?
O1A Cu1 Cl1 98.42(7) 8_454 . ?
N1 Cu1 Cl1 98.80(7) . . ?
C6 N1 C2 121.9(3) . . ?
C6 N1 Cu1 122.0(2) . . ?
C2 N1 Cu1 115.64(19) . . ?
C3A O1A Cu1 136.96(19) . 2 ?
C6A N1A C2A 121.7(2) . . ?
C6A N1A Cu1 120.98(19) . . ?
C2A N1A Cu1 116.97(18) . . ?
N1 C2 C3 118.3(3) . . ?
N1 C2 C2A 113.4(2) . . ?
C3 C2 C2A 128.2(3) . . ?
N1A C2A C3A 119.1(2) . . ?
N1A C2A C2 112.5(2) . . ?
C3A C2A C2 128.4(2) . . ?
O1 C3 C4 116.6(3) . . ?
O1 C3 C2 124.5(3) . . ?
C4 C3 C2 118.9(3) . . ?
O1A C3A C4A 120.2(3) . . ?
O1A C3A C2A 122.0(3) . . ?
C4A C3A C2A 117.8(3) . . ?
C5 C4 C3 120.9(3) . . ?
C5A C4A C3A 121.0(3) . . ?
C4 C5 C6 118.6(3) . . ?
C4A C5A C6A 118.9(3) . . ?
N1 C6 C5 121.4(3) . . ?
N1A C6A C5A 121.4(3) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.096

#===END

#Complex 4

data_4
_database_code_depnum_ccdc_archive 'CCDC 629302'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            (2,2'-bipyridine-3,3'-diol-H)bromocopper(ii)
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H7 Br Cu N2 O2'
_chemical_formula_weight         330.63

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I4(1)/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   13.2775(1)
_cell_length_b                   13.2775(1)
_cell_length_c                   22.4184(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3952.18(7)
_cell_formula_units_Z            16
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            Black
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2576
_exptl_absorpt_coefficient_mu    6.236
_exptl_absorpt_correction_type   multiscan
_exptl_absorpt_correction_T_min  0.4978
_exptl_absorpt_correction_T_max  0.7060
_exptl_absorpt_process_details   SORTAV

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20539
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.78
_diffrn_reflns_theta_max         27.45
_reflns_number_total             2260
_reflns_number_gt                2150
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Nonius)'
_computing_cell_refinement       'DENZO (Nonius)'
_computing_data_reduction        'DENZO (Nonius)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour)'
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+142.6358P] 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    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2260
_refine_ls_number_parameters     146
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0539
_refine_ls_wR_factor_ref         0.1413
_refine_ls_wR_factor_gt          0.1403
_refine_ls_goodness_of_fit_ref   1.287
_refine_ls_restrained_S_all      1.287
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.08623(6) 0.64135(6) 0.03853(3) 0.0207(2) Uani 1 1 d . . .
Cu1 Cu 0.13671(7) 0.79076(7) 0.08857(4) 0.0164(2) Uani 1 1 d . . .
O1 O 0.1344(5) 0.8507(5) 0.3209(2) 0.0276(13) Uani 1 1 d . . .
H1 H 0.1198 0.9092 0.3094 0.041 Uiso 1 1 calc R . .
N1 N 0.1212(4) 0.7430(4) 0.1720(3) 0.0154(12) Uani 1 1 d . . .
O1A O 0.0885(4) 1.0145(4) 0.2790(2) 0.0219(11) Uani 1 1 d . . .
N1A N 0.1371(4) 0.9221(4) 0.1296(2) 0.0145(11) Uani 1 1 d . . .
C2 C 0.1220(5) 0.8166(5) 0.2146(3) 0.0141(13) Uani 1 1 d . . .
C2A C 0.1212(5) 0.9200(5) 0.1903(3) 0.0136(13) Uani 1 1 d . . .
C3 C 0.1274(5) 0.7872(6) 0.2751(3) 0.0191(14) Uani 1 1 d . . .
C3A C 0.1064(5) 1.0121(5) 0.2210(3) 0.0145(13) Uani 1 1 d . . .
C4 C 0.1267(6) 0.6849(6) 0.2896(3) 0.0233(16) Uani 1 1 d . . .
H4 H 0.1263 0.6648 0.3302 0.028 Uiso 1 1 calc R . .
C4A C 0.1114(5) 1.1026(5) 0.1877(3) 0.0182(14) Uani 1 1 d . . .
H4A H 0.1036 1.1655 0.2074 0.022 Uiso 1 1 calc R . .
C5 C 0.1267(5) 0.6135(6) 0.2455(4) 0.0209(15) Uani 1 1 d . . .
H5 H 0.1280 0.5438 0.2551 0.025 Uiso 1 1 calc R . .
C5A C 0.1276(6) 1.1000(6) 0.1270(4) 0.0216(15) Uani 1 1 d . . .
H5A H 0.1308 1.1606 0.1046 0.026 Uiso 1 1 calc R . .
C6 C 0.1247(5) 0.6453(5) 0.1860(3) 0.0176(14) Uani 1 1 d . . .
H6 H 0.1259 0.5965 0.1550 0.021 Uiso 1 1 calc R . .
C6A C 0.1392(6) 1.0073(5) 0.0990(3) 0.0194(15) Uani 1 1 d . . .
H6A H 0.1487 1.0051 0.0570 0.023 Uiso 1 1 calc R . .

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
Br1 0.0245(4) 0.0194(4) 0.0182(4) -0.0046(3) -0.0020(3) 0.0004(3)
Cu1 0.0239(5) 0.0150(4) 0.0103(4) -0.0012(3) 0.0044(3) -0.0018(3)
O1 0.042(4) 0.032(3) 0.009(2) 0.000(2) -0.001(2) 0.004(3)
N1 0.018(3) 0.013(3) 0.015(3) 0.002(2) 0.001(2) 0.001(2)
O1A 0.033(3) 0.024(3) 0.009(2) -0.007(2) -0.002(2) -0.003(2)
N1A 0.018(3) 0.019(3) 0.007(3) 0.002(2) 0.002(2) -0.002(2)
C2 0.015(3) 0.016(3) 0.011(3) 0.000(2) 0.004(2) 0.001(2)
C2A 0.015(3) 0.019(3) 0.007(3) -0.002(2) 0.003(2) -0.001(2)
C3 0.015(3) 0.029(4) 0.014(3) 0.003(3) 0.004(3) 0.004(3)
C3A 0.012(3) 0.019(3) 0.012(3) -0.005(3) -0.001(2) -0.002(2)
C4 0.021(4) 0.033(4) 0.017(4) 0.010(3) 0.000(3) 0.006(3)
C4A 0.017(3) 0.015(3) 0.022(4) -0.003(3) -0.002(3) 0.002(3)
C5 0.016(3) 0.018(3) 0.029(4) 0.009(3) 0.004(3) 0.003(3)
C5A 0.023(4) 0.019(4) 0.022(4) 0.003(3) 0.003(3) 0.000(3)
C6 0.017(3) 0.014(3) 0.022(4) -0.002(3) 0.001(3) -0.003(3)
C6A 0.024(4) 0.018(3) 0.016(3) 0.005(3) 0.003(3) 0.001(3)

_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
Br1 Cu1 2.3756(11) . ?
Cu1 N1A 1.972(6) . ?
Cu1 O1A 1.977(5) 6_554 ?
Cu1 N1 1.985(6) . ?
O1 C3 1.332(9) . ?
N1 C6 1.336(9) . ?
N1 C2 1.367(9) . ?
O1A C3A 1.322(8) . ?
O1A Cu1 1.977(5) 4_465 ?
N1A C6A 1.323(9) . ?
N1A C2A 1.378(8) . ?
C2 C3 1.412(9) . ?
C2 C2A 1.477(9) . ?
C2A C3A 1.417(9) . ?
C3 C4 1.396(11) . ?
C3A C4A 1.415(10) . ?
C4 C5 1.370(12) . ?
C4A C5A 1.379(10) . ?
C5 C6 1.400(10) . ?
C5A C6A 1.390(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
N1A Cu1 O1A 91.7(2) . 6_554 ?
N1A Cu1 N1 81.0(2) . . ?
O1A Cu1 N1 143.9(2) 6_554 . ?
N1A Cu1 Br1 163.69(18) . . ?
O1A Cu1 Br1 97.80(16) 6_554 . ?
N1 Cu1 Br1 98.55(17) . . ?
C6 N1 C2 121.9(6) . . ?
C6 N1 Cu1 121.9(5) . . ?
C2 N1 Cu1 115.4(5) . . ?
C3A O1A Cu1 137.6(5) . 4_465 ?
C6A N1A C2A 122.2(6) . . ?
C6A N1A Cu1 121.0(5) . . ?
C2A N1A Cu1 116.2(5) . . ?
N1 C2 C3 118.3(6) . . ?
N1 C2 C2A 113.9(6) . . ?
C3 C2 C2A 127.7(6) . . ?
N1A C2A C3A 118.9(6) . . ?
N1A C2A C2 112.5(6) . . ?
C3A C2A C2 128.6(6) . . ?
O1 C3 C4 115.9(7) . . ?
O1 C3 C2 124.6(7) . . ?
C4 C3 C2 119.5(7) . . ?
O1A C3A C4A 120.4(6) . . ?
O1A C3A C2A 121.5(6) . . ?
C4A C3A C2A 118.1(6) . . ?
C5 C4 C3 120.4(7) . . ?
C5A C4A C3A 120.4(7) . . ?
C4 C5 C6 118.6(7) . . ?
C4A C5A C6A 119.1(7) . . ?
N1 C6 C5 121.2(7) . . ?
N1A C6A C5A 121.3(7) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.184

#===END

#Complex 5

data_5
_database_code_depnum_ccdc_archive 'CCDC 629303'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            (2,2'-bipyridine-3,3'-diol-H)nitrocopper(ii)
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H7 Cu N3 O5'
_chemical_formula_weight         312.73

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   9.1960(2)
_cell_length_b                   10.6603(3)
_cell_length_c                   11.4383(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.196(1)
_cell_angle_gamma                90.00
_cell_volume                     1091.71(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             628
_exptl_absorpt_coefficient_mu    2.023
_exptl_absorpt_correction_type   multiscan
_exptl_absorpt_correction_T_min  0.7249
_exptl_absorpt_correction_T_max  0.9235
_exptl_absorpt_process_details   SORTAV

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10694
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_sigmaI/netI    0.0439
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.64
_diffrn_reflns_theta_max         27.48
_reflns_number_total             2489
_reflns_number_gt                2255
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Nonius)'
_computing_cell_refinement       'DENZO (Nonius)'
_computing_data_reduction        'DENZO (Nonius)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour)'
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+0.6961P] 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    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2489
_refine_ls_number_parameters     172
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0342
_refine_ls_wR_factor_ref         0.0973
_refine_ls_wR_factor_gt          0.0944
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.12743(3) 0.82493(2) 0.72366(2) 0.01794(12) Uani 1 1 d . . .
O1 O -0.25383(16) 0.98879(14) 0.34639(13) 0.0217(3) Uani 1 1 d . . .
H1 H -0.1994 0.9401 0.3174 0.026 Uiso 1 1 calc R . .
N1 N -0.0642(2) 0.90873(17) 0.65255(16) 0.0205(4) Uani 1 1 d . . .
O2 O 0.15258(17) 0.90367(15) 0.88434(13) 0.0231(3) Uani 1 1 d . . .
N2 N 0.0958(2) 0.82466(17) 0.94869(18) 0.0252(4) Uani 1 1 d . . .
C2 C -0.1114(2) 0.8948(2) 0.53139(18) 0.0185(4) Uani 1 1 d . . .
O3 O 0.0308(2) 0.73142(17) 0.89630(15) 0.0324(4) Uani 1 1 d . . .
C3 C -0.2207(2) 0.9774(2) 0.46747(19) 0.0198(4) Uani 1 1 d . . .
O4 O 0.1097(3) 0.8447(2) 1.05562(17) 0.0475(5) Uani 1 1 d . . .
C4 C -0.2934(2) 1.0583(2) 0.5318(2) 0.0244(5) Uani 1 1 d . . .
H4 H -0.3742 1.1087 0.4906 0.029 Uiso 1 1 calc R . .
C5 C -0.2476(3) 1.0649(2) 0.6548(2) 0.0276(5) Uani 1 1 d . . .
H5 H -0.2969 1.1190 0.6993 0.033 Uiso 1 1 calc R . .
C6 C -0.1290(2) 0.9915(2) 0.71268(19) 0.0246(5) Uani 1 1 d . . .
H6 H -0.0926 0.9999 0.7970 0.030 Uiso 1 1 calc R . .
O1A O -0.19455(16) 0.77705(14) 0.28455(12) 0.0207(3) Uani 1 1 d . . .
N1A N 0.08851(19) 0.74757(17) 0.56273(15) 0.0193(4) Uani 1 1 d . . .
C2A C -0.0329(2) 0.7930(2) 0.48190(18) 0.0178(4) Uani 1 1 d . . .
C3A C -0.0747(2) 0.7389(2) 0.36631(18) 0.0197(4) Uani 1 1 d . . .
C4A C 0.0140(3) 0.6415(2) 0.33795(19) 0.0246(5) Uani 1 1 d . . .
H4A H -0.0101 0.6052 0.2601 0.029 Uiso 1 1 calc R . .
C5A C 0.1349(3) 0.5983(2) 0.4214(2) 0.0267(5) Uani 1 1 d . . .
H5A H 0.1936 0.5312 0.4025 0.032 Uiso 1 1 calc R . .
C6A C 0.1703(3) 0.6541(2) 0.5341(2) 0.0228(4) Uani 1 1 d . . .
H6A H 0.2547 0.6250 0.5921 0.027 Uiso 1 1 calc R . .

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 0.01738(18) 0.02023(19) 0.01373(17) -0.00066(8) -0.00158(11) 0.00119(9)
O1 0.0221(7) 0.0221(8) 0.0186(7) 0.0014(6) -0.0003(6) 0.0045(6)
N1 0.0199(8) 0.0230(9) 0.0174(8) -0.0002(7) 0.0019(7) 0.0002(7)
O2 0.0258(8) 0.0236(8) 0.0188(7) -0.0009(6) 0.0028(6) -0.0026(6)
N2 0.0251(10) 0.0306(11) 0.0194(9) -0.0011(7) 0.0041(8) 0.0010(8)
C2 0.0163(9) 0.0211(10) 0.0161(9) -0.0009(7) -0.0003(7) -0.0003(8)
O3 0.0327(9) 0.0323(10) 0.0321(9) -0.0011(7) 0.0072(7) -0.0112(8)
C3 0.0173(9) 0.0210(11) 0.0193(10) 0.0008(8) 0.0004(8) -0.0023(8)
O4 0.0717(15) 0.0527(13) 0.0213(9) -0.0050(8) 0.0174(10) -0.0067(11)
C4 0.0206(10) 0.0248(11) 0.0266(11) 0.0012(9) 0.0027(9) 0.0049(8)
C5 0.0264(11) 0.0301(12) 0.0272(11) -0.0021(9) 0.0078(9) 0.0066(9)
C6 0.0250(11) 0.0304(12) 0.0178(10) -0.0020(8) 0.0036(8) 0.0036(9)
O1A 0.0191(7) 0.0227(8) 0.0160(7) -0.0001(6) -0.0047(5) -0.0009(6)
N1A 0.0182(8) 0.0213(9) 0.0158(8) 0.0003(6) -0.0013(6) 0.0024(7)
C2A 0.0161(9) 0.0190(10) 0.0166(9) 0.0001(8) 0.0001(7) -0.0008(8)
C3A 0.0185(9) 0.0203(10) 0.0174(9) 0.0006(8) -0.0023(8) -0.0010(8)
C4A 0.0259(11) 0.0266(11) 0.0189(10) -0.0052(9) 0.0001(9) 0.0026(9)
C5A 0.0258(11) 0.0261(12) 0.0259(11) -0.0071(9) 0.0011(9) 0.0056(9)
C6A 0.0213(10) 0.0244(11) 0.0195(10) -0.0007(8) -0.0021(8) 0.0059(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
Cu1 O1A 1.9561(15) 4_676 ?
Cu1 N1A 1.9738(17) . ?
Cu1 N1 1.9774(18) . ?
Cu1 O2 1.9854(15) . ?
O1 C3 1.354(2) . ?
N1 C6 1.339(3) . ?
N1 C2 1.363(3) . ?
O2 N2 1.303(3) . ?
N2 O4 1.219(3) . ?
N2 O3 1.241(3) . ?
C2 C3 1.410(3) . ?
C2 C2A 1.485(3) . ?
C3 C4 1.399(3) . ?
C4 C5 1.374(3) . ?
C5 C6 1.383(3) . ?
O1A C3A 1.336(2) . ?
O1A Cu1 1.9561(15) 4_575 ?
N1A C6A 1.334(3) . ?
N1A C2A 1.365(3) . ?
C2A C3A 1.413(3) . ?
C3A C4A 1.403(3) . ?
C4A C5A 1.369(3) . ?
C5A C6A 1.390(3) . ?

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
O1A Cu1 N1A 93.36(7) 4_676 . ?
O1A Cu1 N1 172.88(7) 4_676 . ?
N1A Cu1 N1 81.39(7) . . ?
O1A Cu1 O2 89.67(6) 4_676 . ?
N1A Cu1 O2 176.34(7) . . ?
N1 Cu1 O2 95.41(7) . . ?
C6 N1 C2 121.23(18) . . ?
C6 N1 Cu1 123.06(14) . . ?
C2 N1 Cu1 114.59(14) . . ?
N2 O2 Cu1 105.81(12) . . ?
O4 N2 O3 123.6(2) . . ?
O4 N2 O2 119.3(2) . . ?
O3 N2 O2 117.10(18) . . ?
N1 C2 C3 118.89(19) . . ?
N1 C2 C2A 113.44(17) . . ?
C3 C2 C2A 127.63(18) . . ?
O1 C3 C4 117.42(19) . . ?
O1 C3 C2 123.61(19) . . ?
C4 C3 C2 118.84(19) . . ?
C5 C4 C3 119.9(2) . . ?
C4 C5 C6 119.0(2) . . ?
N1 C6 C5 121.4(2) . . ?
C3A O1A Cu1 124.73(13) . 4_575 ?
C6A N1A C2A 121.24(18) . . ?
C6A N1A Cu1 123.27(14) . . ?
C2A N1A Cu1 115.44(14) . . ?
N1A C2A C3A 119.67(19) . . ?
N1A C2A C2 113.22(17) . . ?
C3A C2A C2 127.06(18) . . ?
O1A C3A C4A 119.58(18) . . ?
O1A C3A C2A 122.40(19) . . ?
C4A C3A C2A 118.02(18) . . ?
C5A C4A C3A 120.7(2) . . ?
C4A C5A C6A 118.9(2) . . ?
N1A C6A C5A 121.4(2) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.091




