# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Bao-Hui Ye'
_publ_contact_author_email       CESYBH@MAIL.SYSU.EDU.CN

_publ_section_title              
;
Reversible single-crystal-to-single-crystal
transformation driven by adsorption/desorption of water over organic
solvents and thermal stimulation
;
loop_
_publ_author_name
'Bao-Hui Ye'
'Man-Li Cao'
'Jin-Juan Liang'
'Hao-Jun Mo'

# Attachment 'CEC-b817993j.cif'

data_complex_1
_database_code_depnum_ccdc_archive 'CCDC 705313'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H17.20 Co N10 O2.60'
_chemical_formula_weight         570.23

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'
Co Co 0.3494 0.9721 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/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                   7.0901(12)
_cell_length_b                   17.798(3)
_cell_length_c                   11.1041(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 121.728(8)
_cell_angle_gamma                90.00
_cell_volume                     1191.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2324
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      25.99

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             582
_exptl_absorpt_coefficient_mu    0.772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8424
_exptl_absorpt_correction_T_max  0.9131
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_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_%        negligible
_diffrn_reflns_number            5496
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         25.99
_reflns_number_total             2324
_reflns_number_gt                1999
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0577P)²+0.4927P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2324
_refine_ls_number_parameters     195
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0391
_refine_ls_wR_factor_ref         0.1007
_refine_ls_wR_factor_gt          0.0963
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_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 0.5000 0.5000 0.5000 0.01977(15) Uani 1 2 d S . .
O1 O 0.2613(3) 0.43222(8) 0.50104(17) 0.0258(4) Uani 1 1 d . . .
N1 N 0.7220(4) 0.41486(14) 0.0504(3) 0.0482(6) Uani 1 1 d . . .
N2 N 0.3584(3) 0.41089(10) 0.3428(2) 0.0236(4) Uani 1 1 d . . .
N3 N 0.2412(3) 0.30013(11) 0.2073(2) 0.0316(5) Uani 1 1 d . . .
N4 N 0.1226(3) 0.32442(10) 0.3686(2) 0.0281(4) Uani 1 1 d . . .
N5 N -0.2520(3) 0.08178(10) 0.1279(2) 0.0253(4) Uani 1 1 d . . .
C1 C 0.6000(5) 0.35271(18) 0.0211(3) 0.0507(8) Uani 1 1 d . . .
H1A H 0.5973 0.3178 -0.0456 0.054(9) Uiso 1 1 d R . .
C2 C 0.4780(5) 0.33560(15) 0.0813(3) 0.0404(6) Uani 1 1 d . . .
H2A H 0.3924 0.2902 0.0561 0.052(8) Uiso 1 1 d R . .
C3 C 0.4795(4) 0.38425(13) 0.1791(3) 0.0279(5) Uani 1 1 d . . .
C4 C 0.6045(4) 0.44928(14) 0.2098(3) 0.0344(6) Uani 1 1 d . . .
H4A H 0.6095 0.4854 0.2757 0.052(9) Uiso 1 1 d R . .
C5 C 0.7210(4) 0.46112(16) 0.1437(3) 0.0435(7) Uani 1 1 d . . .
H5A H 0.8080 0.5061 0.1665 0.055(10) Uiso 1 1 d R . .
C6 C 0.3520(4) 0.36501(12) 0.2464(2) 0.0255(5) Uani 1 1 d . . .
C7 C 0.2427(4) 0.38878(12) 0.4047(2) 0.0238(5) Uani 1 1 d . . .
C8 C 0.1307(4) 0.28400(12) 0.2713(3) 0.0264(5) Uani 1 1 d . . .
C9 C 0.0034(4) 0.21184(12) 0.2275(3) 0.0280(5) Uani 1 1 d . . .
C10 C 0.0143(4) 0.16518(13) 0.1316(3) 0.0322(6) Uani 1 1 d . . .
H10A H 0.1098 0.1775 0.0974 0.050(8) Uiso 1 1 d R . .
C11 C -0.1143(4) 0.10129(13) 0.0857(3) 0.0314(5) Uani 1 1 d . . .
H11A H -0.1032 0.0688 0.0207 0.051(8) Uiso 1 1 d R . .
C12 C -0.2552(5) 0.12522(15) 0.2251(3) 0.0401(7) Uani 1 1 d . . .
H12A H -0.3483 0.1106 0.2600 0.055(9) Uiso 1 1 d R . .
C13 C -0.1300(5) 0.19022(15) 0.2779(3) 0.0405(7) Uani 1 1 d . . .
H13A H -0.1363 0.2201 0.3476 0.058(9) Uiso 1 1 d R . .
O1W O 0.998(3) 0.5232(9) 0.0289(17) 0.142(6) Uani 0.30 1 d P . .
H1WA H 0.9435 0.4825 0.0372 0.213 Uiso 0.60 1 d PR . .


_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 O1 2.0832(15) . ?
Co1 O1 2.0832(15) 3_666 ?
Co1 N5 2.1449(18) 2 ?
Co1 N5 2.1449(18) 4_666 ?
Co1 N2 2.1744(18) . ?
Co1 N2 2.1744(18) 3_666 ?
O1 C7 1.270(3) . ?
N1 C5 1.326(4) . ?
N1 C1 1.335(4) . ?
N2 C6 1.328(3) . ?
N2 C7 1.375(3) . ?
N3 C6 1.334(3) . ?
N3 C8 1.337(3) . ?
N4 C8 1.324(3) . ?
N4 C7 1.356(3) . ?
N5 C11 1.333(3) . ?
N5 C12 1.337(3) . ?
N5 Co1 2.1449(18) 2_545 ?
C1 C2 1.377(4) . ?
C1 H1A 0.9598 . ?
C2 C3 1.385(3) . ?
C2 H2A 0.9600 . ?
C3 C4 1.387(3) . ?
C3 C6 1.485(3) . ?
C4 C5 1.380(3) . ?
C4 H4A 0.9603 . ?
C5 H5A 0.9601 . ?
C8 C9 1.496(3) . ?
C9 C13 1.383(3) . ?
C9 C10 1.385(3) . ?
C10 C11 1.377(3) . ?
C10 H10A 0.9600 . ?
C11 H11A 0.9599 . ?
C12 C13 1.387(3) . ?
C12 H12A 0.9601 . ?
C13 H13A 0.9600 . ?
O1W O1W 1.06(2) 3_765 ?
O1W H1WA 0.8461 . ?

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
O1 Co1 O1 180.00(6) . 3_666 ?
O1 Co1 N5 90.64(7) . 2 ?
O1 Co1 N5 89.36(7) 3_666 2 ?
O1 Co1 N5 89.36(7) . 4_666 ?
O1 Co1 N5 90.64(7) 3_666 4_666 ?
N5 Co1 N5 180.0 2 4_666 ?
O1 Co1 N2 63.17(6) . . ?
O1 Co1 N2 116.83(6) 3_666 . ?
N5 Co1 N2 95.25(7) 2 . ?
N5 Co1 N2 84.75(7) 4_666 . ?
O1 Co1 N2 116.83(6) . 3_666 ?
O1 Co1 N2 63.17(6) 3_666 3_666 ?
N5 Co1 N2 84.75(7) 2 3_666 ?
N5 Co1 N2 95.25(7) 4_666 3_666 ?
N2 Co1 N2 180.00(6) . 3_666 ?
C7 O1 Co1 94.15(12) . . ?
C5 N1 C1 115.9(2) . . ?
C6 N2 C7 116.75(18) . . ?
C6 N2 Co1 154.32(15) . . ?
C7 N2 Co1 87.27(13) . . ?
C6 N3 C8 115.00(19) . . ?
C8 N4 C7 114.19(19) . . ?
C11 N5 C12 117.38(19) . . ?
C11 N5 Co1 116.15(15) . 2_545 ?
C12 N5 Co1 124.82(15) . 2_545 ?
N1 C1 C2 123.9(3) . . ?
N1 C1 H1A 118.2 . . ?
C2 C1 H1A 117.9 . . ?
C1 C2 C3 119.6(2) . . ?
C1 C2 H2A 120.5 . . ?
C3 C2 H2A 119.9 . . ?
C2 C3 C4 117.1(2) . . ?
C2 C3 C6 119.7(2) . . ?
C4 C3 C6 123.2(2) . . ?
C5 C4 C3 118.7(2) . . ?
C5 C4 H4A 120.7 . . ?
C3 C4 H4A 120.6 . . ?
N1 C5 C4 124.8(2) . . ?
N1 C5 H5A 117.3 . . ?
C4 C5 H5A 117.9 . . ?
N2 C6 N3 124.0(2) . . ?
N2 C6 C3 119.50(19) . . ?
N3 C6 C3 116.5(2) . . ?
O1 C7 N4 122.3(2) . . ?
O1 C7 N2 114.97(18) . . ?
N4 C7 N2 122.8(2) . . ?
N4 C8 N3 127.3(2) . . ?
N4 C8 C9 117.00(19) . . ?
N3 C8 C9 115.7(2) . . ?
C13 C9 C10 118.1(2) . . ?
C13 C9 C8 122.1(2) . . ?
C10 C9 C8 119.8(2) . . ?
C11 C10 C9 119.1(2) . . ?
C11 C10 H10A 120.7 . . ?
C9 C10 H10A 120.2 . . ?
N5 C11 C10 123.4(2) . . ?
N5 C11 H11A 118.2 . . ?
C10 C11 H11A 118.5 . . ?
N5 C12 C13 123.0(2) . . ?
N5 C12 H12A 118.3 . . ?
C13 C12 H12A 118.7 . . ?
C9 C13 C12 118.9(2) . . ?
C9 C13 H13A 120.3 . . ?
C12 C13 H13A 120.8 . . ?
O1W O1W H1WA 64.0 3_765 . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.062

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

data_complex_1a
_database_code_depnum_ccdc_archive 'CCDC 705314'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H16 Co N10 O2'
_chemical_formula_weight         559.42

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'
Co Co 0.3494 0.9721 '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'

_symmetry_cell_setting           MONOCLINIC
_symmetry_space_group_name_H-M   P21/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                   6.9626(13)
_cell_length_b                   17.913(3)
_cell_length_c                   11.0206(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 121.714(8)
_cell_angle_gamma                90.00
_cell_volume                     1169.3(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2274
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      25.99

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             570
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8404
_exptl_absorpt_correction_T_max  0.8982
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_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_%        negligible
_diffrn_reflns_number            4798
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.27
_diffrn_reflns_theta_max         25.99
_reflns_number_total             2274
_reflns_number_gt                1967
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0709P)²+0.4484P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2274
_refine_ls_number_parameters     186
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0437
_refine_ls_wR_factor_ref         0.1158
_refine_ls_wR_factor_gt          0.1098
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_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 0.5000 0.5000 0.5000 0.01785(17) Uani 1 2 d S . .
O1 O 0.2579(3) 0.43204(9) 0.49867(19) 0.0238(4) Uani 1 1 d . . .
N1 N 0.7286(5) 0.41411(15) 0.0445(3) 0.0435(6) Uani 1 1 d . . .
N2 N 0.3601(3) 0.41106(11) 0.3408(2) 0.0215(5) Uani 1 1 d . . .
N3 N 0.2468(4) 0.29984(12) 0.2076(2) 0.0292(5) Uani 1 1 d . . .
N4 N 0.1237(4) 0.32437(11) 0.3685(2) 0.0257(5) Uani 1 1 d . . .
N5 N -0.2464(4) 0.08077(11) 0.1310(2) 0.0233(5) Uani 1 1 d . . .
C1 C 0.6083(6) 0.35215(19) 0.0176(3) 0.0450(8) Uani 1 1 d . . .
H1A H 0.6068 0.3183 -0.0468 0.057(10) Uiso 1 1 d R . .
C2 C 0.4857(5) 0.33494(16) 0.0793(3) 0.0364(7) Uani 1 1 d . . .
H2A H 0.4031 0.2908 0.0556 0.059(11) Uiso 1 1 d R . .
C3 C 0.4861(4) 0.38396(14) 0.1771(3) 0.0255(6) Uani 1 1 d . . .
C4 C 0.6111(5) 0.44903(15) 0.2060(3) 0.0307(6) Uani 1 1 d . . .
H4A H 0.6161 0.4840 0.2699 0.045(9) Uiso 1 1 d R . .
C5 C 0.7282(5) 0.46082(18) 0.1380(3) 0.0404(7) Uani 1 1 d . . .
H5A H 0.8123 0.5045 0.1591 0.049(11) Uiso 1 1 d R . .
C6 C 0.3572(4) 0.36469(14) 0.2454(2) 0.0229(5) Uani 1 1 d . . .
C7 C 0.2426(4) 0.38883(13) 0.4030(3) 0.0209(5) Uani 1 1 d . . .
C8 C 0.1347(4) 0.28363(13) 0.2718(3) 0.0241(5) Uani 1 1 d . . .
C9 C 0.0074(4) 0.21143(14) 0.2290(3) 0.0253(6) Uani 1 1 d . . .
C10 C 0.0181(5) 0.16571(14) 0.1316(3) 0.0305(6) Uani 1 1 d . . .
H10A H 0.1105 0.1781 0.0971 0.043(9) Uiso 1 1 d R . .
C11 C -0.1100(5) 0.10143(14) 0.0864(3) 0.0283(6) Uani 1 1 d . . .
H11A H -0.1006 0.0710 0.0214 0.038(8) Uiso 1 1 d R . .
C12 C -0.2468(5) 0.12319(16) 0.2311(3) 0.0369(7) Uani 1 1 d . . .
H12A H -0.3347 0.1083 0.2675 0.029(7) Uiso 1 1 d R . .
C13 C -0.1221(5) 0.18812(16) 0.2823(3) 0.0383(7) Uani 1 1 d . . .
H13A H -0.1257 0.2159 0.3525 0.059(11) Uiso 1 1 d R . .


_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 O1 2.0728(17) . ?
Co1 O1 2.0728(17) 3_666 ?
Co1 N5 2.148(2) 4_666 ?
Co1 N5 2.148(2) 2 ?
Co1 N2 2.1834(19) . ?
Co1 N2 2.1834(19) 3_666 ?
O1 C7 1.266(3) . ?
N1 C1 1.326(4) . ?
N1 C5 1.328(4) . ?
N2 C6 1.332(3) . ?
N2 C7 1.374(3) . ?
N3 C8 1.331(3) . ?
N3 C6 1.333(3) . ?
N4 C8 1.326(3) . ?
N4 C7 1.354(3) . ?
N5 C11 1.331(3) . ?
N5 C12 1.341(3) . ?
N5 Co1 2.148(2) 2_545 ?
C1 C2 1.377(4) . ?
C2 C3 1.390(4) . ?
C3 C4 1.388(4) . ?
C3 C6 1.484(3) . ?
C4 C5 1.383(4) . ?
C8 C9 1.497(3) . ?
C9 C13 1.375(4) . ?
C9 C10 1.383(3) . ?
C10 C11 1.379(3) . ?
C12 C13 1.382(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
O1 Co1 O1 180.00(7) . 3_666 ?
O1 Co1 N5 89.27(8) . 4_666 ?
O1 Co1 N5 90.73(8) 3_666 4_666 ?
O1 Co1 N5 90.73(8) . 2 ?
O1 Co1 N5 89.27(8) 3_666 2 ?
N5 Co1 N5 180.000(1) 4_666 2 ?
O1 Co1 N2 63.14(7) . . ?
O1 Co1 N2 116.86(7) 3_666 . ?
N5 Co1 N2 84.87(8) 4_666 . ?
N5 Co1 N2 95.13(8) 2 . ?
O1 Co1 N2 116.86(7) . 3_666 ?
O1 Co1 N2 63.14(7) 3_666 3_666 ?
N5 Co1 N2 95.13(8) 4_666 3_666 ?
N5 Co1 N2 84.87(8) 2 3_666 ?
N2 Co1 N2 180.00(7) . 3_666 ?
C7 O1 Co1 94.43(14) . . ?
C1 N1 C5 116.2(3) . . ?
C6 N2 C7 116.6(2) . . ?
C6 N2 Co1 154.78(17) . . ?
C7 N2 Co1 86.67(14) . . ?
C8 N3 C6 115.3(2) . . ?
C8 N4 C7 114.2(2) . . ?
C11 N5 C12 117.2(2) . . ?
C11 N5 Co1 115.66(16) . 2_545 ?
C12 N5 Co1 125.31(18) . 2_545 ?
N1 C1 C2 124.0(3) . . ?
C1 C2 C3 119.5(3) . . ?
C4 C3 C2 117.0(2) . . ?
C4 C3 C6 123.6(2) . . ?
C2 C3 C6 119.4(2) . . ?
C5 C4 C3 118.8(3) . . ?
N1 C5 C4 124.5(3) . . ?
N2 C6 N3 123.9(2) . . ?
N2 C6 C3 119.5(2) . . ?
N3 C6 C3 116.6(2) . . ?
O1 C7 N4 121.8(2) . . ?
O1 C7 N2 115.2(2) . . ?
N4 C7 N2 122.9(2) . . ?
N4 C8 N3 127.2(2) . . ?
N4 C8 C9 117.0(2) . . ?
N3 C8 C9 115.9(2) . . ?
C13 C9 C10 117.9(2) . . ?
C13 C9 C8 122.7(2) . . ?
C10 C9 C8 119.4(2) . . ?
C11 C10 C9 119.1(2) . . ?
N5 C11 C10 123.4(2) . . ?
N5 C12 C13 122.7(3) . . ?
C9 C13 C12 119.6(2) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.074

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

data_complex_1'
_database_code_depnum_ccdc_archive 'CCDC 705315'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H17.20 Co N10 O2.60'
_chemical_formula_weight         570.23

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'
Co Co 0.3494 0.9721 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/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                   7.063(6)
_cell_length_b                   17.792(14)
_cell_length_c                   11.089(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 121.31(4)
_cell_angle_gamma                90.00
_cell_volume                     1190.6(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2309
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      26.00

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             582
_exptl_absorpt_coefficient_mu    0.773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8127
_exptl_absorpt_correction_T_max  0.8608
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_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_%        negligible
_diffrn_reflns_number            3677
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         26.00
_reflns_number_total             2309
_reflns_number_gt                1815
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0694P)²+0.5484P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2309
_refine_ls_number_parameters     195
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.1148
_refine_ls_wR_factor_gt          0.1106
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_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 0.5000 0.5000 0.5000 0.02382(19) Uani 1 2 d S . .
O1 O 0.2606(3) 0.43231(10) 0.50047(18) 0.0299(4) Uani 1 1 d . . .
N1 N 0.7236(5) 0.41628(18) 0.0518(3) 0.0572(8) Uani 1 1 d . . .
N2 N 0.3597(3) 0.41117(12) 0.3431(2) 0.0293(5) Uani 1 1 d . . .
N3 N 0.2410(4) 0.30063(14) 0.2077(2) 0.0382(6) Uani 1 1 d . . .
N4 N 0.1221(4) 0.32444(13) 0.3687(2) 0.0328(5) Uani 1 1 d . . .
N5 N -0.2546(3) 0.08246(13) 0.1257(2) 0.0301(5) Uani 1 1 d . . .
C1 C 0.6011(6) 0.3541(2) 0.0219(4) 0.0570(9) Uani 1 1 d . . .
H1A H 0.5984 0.3192 -0.0448 0.061(10) Uiso 1 1 d R . .
C2 C 0.4787(5) 0.33677(19) 0.0811(3) 0.0459(8) Uani 1 1 d . . .
H2A H 0.3932 0.2913 0.0559 0.056(10) Uiso 1 1 d R . .
C3 C 0.4803(4) 0.38526(16) 0.1795(3) 0.0348(6) Uani 1 1 d . . .
C4 C 0.6069(5) 0.45023(18) 0.2120(3) 0.0411(7) Uani 1 1 d . . .
H4A H 0.6120 0.4863 0.2779 0.055(10) Uiso 1 1 d R . .
C5 C 0.7235(5) 0.4622(2) 0.1453(3) 0.0500(8) Uani 1 1 d . . .
H5A H 0.8105 0.5072 0.1682 0.055(10) Uiso 1 1 d R . .
C6 C 0.3529(4) 0.36515(16) 0.2469(3) 0.0305(6) Uani 1 1 d . . .
C7 C 0.2425(4) 0.38856(15) 0.4046(2) 0.0291(6) Uani 1 1 d . . .
C8 C 0.1301(4) 0.28438(15) 0.2715(3) 0.0316(6) Uani 1 1 d . . .
C9 C 0.0029(4) 0.21262(16) 0.2273(3) 0.0326(6) Uani 1 1 d . . .
C10 C 0.0130(4) 0.16631(16) 0.1308(3) 0.0377(7) Uani 1 1 d . . .
H10A H 0.1084 0.1787 0.0966 0.060(10) Uiso 1 1 d R . .
C11 C -0.1159(4) 0.10261(16) 0.0844(3) 0.0365(7) Uani 1 1 d . . .
H11A H -0.1048 0.0701 0.0194 0.037(7) Uiso 1 1 d R . .
C12 C -0.2575(5) 0.12564(17) 0.2233(3) 0.0448(8) Uani 1 1 d . . .
H12A H -0.3505 0.1110 0.2582 0.055(9) Uiso 1 1 d R . .
C13 C -0.1316(5) 0.19020(19) 0.2765(3) 0.0472(8) Uani 1 1 d . . .
H13A H -0.1378 0.2201 0.3463 0.065(10) Uiso 1 1 d R . .
O1W O 1.017(3) 0.5192(11) 0.0379(18) 0.155(7) Uani 0.30 1 d P . .
H1WA H 0.9608 0.4770 0.0466 0.232 Uiso 0.60 1 d PR . .


_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 O1 2.078(2) . ?
Co1 O1 2.078(2) 3_666 ?
Co1 N5 2.142(2) 4_666 ?
Co1 N5 2.142(2) 2 ?
Co1 N2 2.171(2) . ?
Co1 N2 2.171(2) 3_666 ?
O1 C7 1.269(3) . ?
N1 C5 1.320(4) . ?
N1 C1 1.335(5) . ?
N2 C6 1.325(3) . ?
N2 C7 1.378(3) . ?
N3 C6 1.332(4) . ?
N3 C8 1.333(3) . ?
N4 C8 1.317(3) . ?
N4 C7 1.353(3) . ?
N5 C11 1.329(3) . ?
N5 C12 1.336(3) . ?
N5 Co1 2.142(2) 2_545 ?
C1 C2 1.365(4) . ?
C1 H1A 0.9591 . ?
C2 C3 1.387(4) . ?
C2 H2A 0.9598 . ?
C3 C4 1.390(4) . ?
C3 C6 1.482(4) . ?
C4 C5 1.379(4) . ?
C4 H4A 0.9597 . ?
C5 H5A 0.9597 . ?
C8 C9 1.490(4) . ?
C9 C13 1.378(4) . ?
C9 C10 1.381(4) . ?
C10 C11 1.375(4) . ?
C10 H10A 0.9555 . ?
C11 H11A 0.9585 . ?
C12 C13 1.383(4) . ?
C12 H12A 0.9557 . ?
C13 H13A 0.9587 . ?
O1W O1W 1.01(2) 3_765 ?
O1W H1WA 0.8776 . ?

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
O1 Co1 O1 180.00(8) . 3_666 ?
O1 Co1 N5 89.18(10) . 4_666 ?
O1 Co1 N5 90.82(10) 3_666 4_666 ?
O1 Co1 N5 90.82(10) . 2 ?
O1 Co1 N5 89.18(10) 3_666 2 ?
N5 Co1 N5 180.0 4_666 2 ?
O1 Co1 N2 63.07(8) . . ?
O1 Co1 N2 116.93(8) 3_666 . ?
N5 Co1 N2 84.32(10) 4_666 . ?
N5 Co1 N2 95.68(10) 2 . ?
O1 Co1 N2 116.93(8) . 3_666 ?
O1 Co1 N2 63.07(8) 3_666 3_666 ?
N5 Co1 N2 95.68(10) 4_666 3_666 ?
N5 Co1 N2 84.32(10) 2 3_666 ?
N2 Co1 N2 180.000(1) . 3_666 ?
C7 O1 Co1 94.65(15) . . ?
C5 N1 C1 116.3(3) . . ?
C6 N2 C7 116.0(2) . . ?
C6 N2 Co1 154.81(18) . . ?
C7 N2 Co1 87.56(15) . . ?
C6 N3 C8 115.2(2) . . ?
C8 N4 C7 114.2(2) . . ?
C11 N5 C12 116.6(2) . . ?
C11 N5 Co1 116.91(17) . 2_545 ?
C12 N5 Co1 125.00(18) . 2_545 ?
N1 C1 C2 124.0(3) . . ?
N1 C1 H1A 118.6 . . ?
C2 C1 H1A 117.4 . . ?
C1 C2 C3 119.3(3) . . ?
C1 C2 H2A 120.8 . . ?
C3 C2 H2A 119.9 . . ?
C2 C3 C4 117.5(3) . . ?
C2 C3 C6 119.2(3) . . ?
C4 C3 C6 123.2(2) . . ?
C5 C4 C3 118.2(3) . . ?
C5 C4 H4A 120.6 . . ?
C3 C4 H4A 121.2 . . ?
N1 C5 C4 124.7(3) . . ?
N1 C5 H5A 117.5 . . ?
C4 C5 H5A 117.8 . . ?
N2 C6 N3 124.2(2) . . ?
N2 C6 C3 118.6(2) . . ?
N3 C6 C3 117.1(2) . . ?
O1 C7 N4 122.5(2) . . ?
O1 C7 N2 114.2(2) . . ?
N4 C7 N2 123.2(2) . . ?
N4 C8 N3 127.2(2) . . ?
N4 C8 C9 117.3(2) . . ?
N3 C8 C9 115.5(2) . . ?
C13 C9 C10 117.2(3) . . ?
C13 C9 C8 122.6(2) . . ?
C10 C9 C8 120.1(2) . . ?
C11 C10 C9 119.4(2) . . ?
C11 C10 H10A 120.5 . . ?
C9 C10 H10A 120.1 . . ?
N5 C11 C10 123.8(2) . . ?
N5 C11 H11A 117.3 . . ?
C10 C11 H11A 118.8 . . ?
N5 C12 C13 123.1(2) . . ?
N5 C12 H12A 118.3 . . ?
C13 C12 H12A 118.6 . . ?
C9 C13 C12 119.6(3) . . ?
C9 C13 H13A 119.3 . . ?
C12 C13 H13A 121.0 . . ?
O1W O1W H1WA 65.5 3_765 . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.061

#===END

data_complex_2
_database_code_depnum_ccdc_archive 'CCDC 705316'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H17.20 N10 Ni O2.60'
_chemical_formula_weight         569.99

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/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                   7.1011(18)
_cell_length_b                   17.440(4)
_cell_length_c                   11.2157(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 120.736(11)
_cell_angle_gamma                90.00
_cell_volume                     1193.9(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2317
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      26.00

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             584
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8346
_exptl_absorpt_correction_T_max  0.8663
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_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_%        negligible
_diffrn_reflns_number            4837
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.34
_diffrn_reflns_theta_max         26.00
_reflns_number_total             2317
_reflns_number_gt                1947
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0676P)²+0.8510P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2317
_refine_ls_number_parameters     187
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0410
_refine_ls_wR_factor_ref         0.1118
_refine_ls_wR_factor_gt          0.1064
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_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
Ni1 Ni 0.5000 0.5000 0.5000 0.02138(17) Uani 1 2 d S . .
O1 O 0.2627(3) 0.43282(10) 0.50448(19) 0.0277(4) Uani 1 1 d . . .
N1 N 0.7245(5) 0.41899(18) 0.0552(3) 0.0565(8) Uani 1 1 d . . .
N2 N 0.3603(4) 0.41288(12) 0.3460(2) 0.0284(5) Uani 1 1 d . . .
N3 N 0.2391(4) 0.30196(13) 0.2094(3) 0.0377(6) Uani 1 1 d . . .
N4 N 0.1198(4) 0.32471(12) 0.3699(2) 0.0320(5) Uani 1 1 d . . .
N5 N -0.2633(4) 0.08198(12) 0.1200(2) 0.0273(5) Uani 1 1 d . . .
C1 C 0.5985(7) 0.3564(2) 0.0237(4) 0.0583(10) Uani 1 1 d . . .
H1A H 0.5941 0.3225 -0.0419 0.070 Uiso 1 1 d R . .
C2 C 0.4763(6) 0.33886(18) 0.0832(4) 0.0483(8) Uani 1 1 d . . .
H2A H 0.3924 0.2944 0.0579 0.058 Uiso 1 1 d R . .
C3 C 0.4795(5) 0.38731(16) 0.1821(3) 0.0336(6) Uani 1 1 d . . .
C4 C 0.6067(5) 0.45260(17) 0.2147(3) 0.0398(7) Uani 1 1 d . . .
H4A H 0.6139 0.4875 0.2797 0.048 Uiso 1 1 d R . .
C5 C 0.7253(5) 0.4652(2) 0.1496(4) 0.0503(8) Uani 1 1 d . . .
H5A H 0.8099 0.5093 0.1726 0.060 Uiso 1 1 d R . .
C6 C 0.3521(4) 0.36719(15) 0.2491(3) 0.0297(6) Uani 1 1 d . . .
C7 C 0.2429(4) 0.38954(14) 0.4076(3) 0.0274(6) Uani 1 1 d . . .
C8 C 0.1274(5) 0.28496(15) 0.2721(3) 0.0308(6) Uani 1 1 d . . .
C9 C -0.0022(5) 0.21223(15) 0.2257(3) 0.0310(6) Uani 1 1 d . . .
C10 C 0.0054(5) 0.16689(16) 0.1275(3) 0.0361(7) Uani 1 1 d . . .
H10A H 0.0988 0.1792 0.0949 0.043 Uiso 1 1 d R . .
C11 C -0.1254(5) 0.10323(16) 0.0786(3) 0.0353(7) Uani 1 1 d . . .
H11A H -0.1176 0.0728 0.0130 0.042 Uiso 1 1 d R . .
C12 C -0.2648(5) 0.12426(17) 0.2192(3) 0.0442(8) Uani 1 1 d . . .
H12A H -0.3558 0.1095 0.2523 0.053 Uiso 1 1 d R . .
C13 C -0.1358(6) 0.18893(18) 0.2752(4) 0.0468(8) Uani 1 1 d . . .
H13A H -0.1387 0.2164 0.3456 0.056 Uiso 1 1 d R . .
O1W O 0.014(3) 0.5203(11) 0.037(2) 0.154(7) Uani 0.30 1 d P . .
H1WA H -0.0472 0.4772 0.0386 0.231 Uiso 0.60 1 d PR . .


_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
Ni1 O1 2.0737(17) . ?
Ni1 O1 2.0737(17) 3_666 ?
Ni1 N5 2.090(2) 4_666 ?
Ni1 N5 2.090(2) 2 ?
Ni1 N2 2.127(2) . ?
Ni1 N2 2.127(2) 3_666 ?
Ni1 C7 2.487(3) . ?
Ni1 C7 2.487(3) 3_666 ?
O1 C7 1.270(3) . ?
N1 C5 1.328(5) . ?
N1 C1 1.340(5) . ?
N2 C6 1.324(3) . ?
N2 C7 1.389(3) . ?
N3 C6 1.331(3) . ?
N3 C8 1.335(3) . ?
N4 C8 1.321(3) . ?
N4 C7 1.358(3) . ?
N5 C11 1.333(3) . ?
N5 C12 1.339(4) . ?
N5 Ni1 2.090(2) 2_545 ?
C1 C2 1.373(5) . ?
C2 C3 1.385(4) . ?
C3 C4 1.381(4) . ?
C3 C6 1.484(4) . ?
C4 C5 1.385(4) . ?
C8 C9 1.496(4) . ?
C9 C10 1.379(4) . ?
C9 C13 1.383(4) . ?
C10 C11 1.370(4) . ?
C12 C13 1.385(4) . ?
O1W O1W 1.03(2) 3_565 ?

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
O1 Ni1 O1 180.00(8) . 3_666 ?
O1 Ni1 N5 89.64(8) . 4_666 ?
O1 Ni1 N5 90.36(8) 3_666 4_666 ?
O1 Ni1 N5 90.36(8) . 2 ?
O1 Ni1 N5 89.64(8) 3_666 2 ?
N5 Ni1 N5 180.000(1) 4_666 2 ?
O1 Ni1 N2 64.46(8) . . ?
O1 Ni1 N2 115.54(8) 3_666 . ?
N5 Ni1 N2 85.53(9) 4_666 . ?
N5 Ni1 N2 94.47(9) 2 . ?
O1 Ni1 N2 115.54(8) . 3_666 ?
O1 Ni1 N2 64.46(8) 3_666 3_666 ?
N5 Ni1 N2 94.47(9) 4_666 3_666 ?
N5 Ni1 N2 85.53(9) 2 3_666 ?
N2 Ni1 N2 180.000(1) . 3_666 ?
O1 Ni1 C7 30.67(8) . . ?
O1 Ni1 C7 149.33(8) 3_666 . ?
N5 Ni1 C7 85.18(9) 4_666 . ?
N5 Ni1 C7 94.82(9) 2 . ?
N2 Ni1 C7 33.91(8) . . ?
N2 Ni1 C7 146.09(8) 3_666 . ?
O1 Ni1 C7 149.33(8) . 3_666 ?
O1 Ni1 C7 30.67(8) 3_666 3_666 ?
N5 Ni1 C7 94.82(9) 4_666 3_666 ?
N5 Ni1 C7 85.18(9) 2 3_666 ?
N2 Ni1 C7 146.09(8) . 3_666 ?
N2 Ni1 C7 33.91(8) 3_666 3_666 ?
C7 Ni1 C7 180.00(7) . 3_666 ?
C7 O1 Ni1 92.95(15) . . ?
C5 N1 C1 115.7(3) . . ?
C6 N2 C7 116.5(2) . . ?
C6 N2 Ni1 154.53(19) . . ?
C7 N2 Ni1 87.38(15) . . ?
C6 N3 C8 115.6(2) . . ?
C8 N4 C7 113.8(2) . . ?
C11 N5 C12 117.1(2) . . ?
C11 N5 Ni1 117.25(17) . 2_545 ?
C12 N5 Ni1 124.52(18) . 2_545 ?
N1 C1 C2 123.8(3) . . ?
C1 C2 C3 119.8(3) . . ?
C4 C3 C2 117.1(3) . . ?
C4 C3 C6 123.1(3) . . ?
C2 C3 C6 119.8(3) . . ?
C3 C4 C5 118.8(3) . . ?
N1 C5 C4 124.7(3) . . ?
N2 C6 N3 123.7(2) . . ?
N2 C6 C3 119.4(2) . . ?
N3 C6 C3 116.9(2) . . ?
O1 C7 N4 122.3(2) . . ?
O1 C7 N2 114.8(2) . . ?
N4 C7 N2 122.9(2) . . ?
O1 C7 Ni1 56.38(12) . . ?
N4 C7 Ni1 173.5(2) . . ?
N2 C7 Ni1 58.71(13) . . ?
N4 C8 N3 127.4(2) . . ?
N4 C8 C9 117.1(2) . . ?
N3 C8 C9 115.5(2) . . ?
C10 C9 C13 117.9(2) . . ?
C10 C9 C8 119.7(2) . . ?
C13 C9 C8 122.4(2) . . ?
C11 C10 C9 119.3(2) . . ?
N5 C11 C10 123.7(2) . . ?
N5 C12 C13 122.8(3) . . ?
C9 C13 C12 119.2(3) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.082

#===END

data_complex_2a
_database_code_depnum_ccdc_archive 'CCDC 705317'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H16 N10 Ni O2'
_chemical_formula_weight         559.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/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                   6.9760(9)
_cell_length_b                   17.636(2)
_cell_length_c                   11.0530(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 121.308(6)
_cell_angle_gamma                90.00
_cell_volume                     1161.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2255
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      25.99

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             572
_exptl_absorpt_coefficient_mu    0.885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7529
_exptl_absorpt_correction_T_max  0.8157
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_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_%        negligible
_diffrn_reflns_number            4938
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.31
_diffrn_reflns_theta_max         25.99
_reflns_number_total             2255
_reflns_number_gt                1930
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0628P)²+0.2147P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2255
_refine_ls_number_parameters     178
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_ref         0.0981
_refine_ls_wR_factor_gt          0.0928
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_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
Ni1 Ni 0.5000 0.5000 0.5000 0.01860(15) Uani 1 2 d S . .
O1 O 0.2600(3) 0.43286(8) 0.50294(16) 0.0243(3) Uani 1 1 d . . .
N1 N 0.7295(4) 0.41586(14) 0.0478(2) 0.0469(6) Uani 1 1 d . . .
N2 N 0.3608(3) 0.41257(9) 0.34420(19) 0.0232(4) Uani 1 1 d . . .
N3 N 0.2442(3) 0.30078(11) 0.2094(2) 0.0319(5) Uani 1 1 d . . .
N4 N 0.1216(3) 0.32436(10) 0.3706(2) 0.0276(4) Uani 1 1 d . . .
N5 N -0.2547(3) 0.07999(10) 0.1263(2) 0.0237(4) Uani 1 1 d . . .
C1 C 0.6055(5) 0.35316(17) 0.0198(3) 0.0488(7) Uani 1 1 d . . .
H1A H 0.6010 0.3193 -0.0459 0.059 Uiso 1 1 d R . .
C2 C 0.4835(5) 0.33641(14) 0.0813(3) 0.0397(6) Uani 1 1 d . . .
H2A H 0.3995 0.2920 0.0559 0.048 Uiso 1 1 d R . .
C3 C 0.4851(4) 0.38581(12) 0.1792(2) 0.0280(5) Uani 1 1 d . . .
C4 C 0.6115(4) 0.45136(13) 0.2085(3) 0.0327(5) Uani 1 1 d . . .
H4A H 0.6187 0.4863 0.2735 0.039 Uiso 1 1 d R . .
C5 C 0.7294(4) 0.46297(16) 0.1413(3) 0.0417(6) Uani 1 1 d . . .
H5A H 0.8140 0.5072 0.1643 0.050 Uiso 1 1 d R . .
C6 C 0.3561(4) 0.36629(12) 0.2479(2) 0.0253(5) Uani 1 1 d . . .
C7 C 0.2426(4) 0.38957(11) 0.4066(2) 0.0236(5) Uani 1 1 d . . .
C8 C 0.1317(4) 0.28392(12) 0.2733(2) 0.0270(5) Uani 1 1 d . . .
C9 C 0.0033(4) 0.21085(12) 0.2287(2) 0.0272(5) Uani 1 1 d . . .
C10 C 0.0117(4) 0.16604(13) 0.1295(2) 0.0310(5) Uani 1 1 d . . .
H10A H 0.1050 0.1783 0.0969 0.037 Uiso 1 1 d R . .
C11 C -0.1187(4) 0.10145(12) 0.0821(3) 0.0295(5) Uani 1 1 d . . .
H11A H -0.1109 0.0710 0.0165 0.035 Uiso 1 1 d R . .
C12 C -0.2538(5) 0.12149(14) 0.2280(3) 0.0387(6) Uani 1 1 d . . .
H12A H -0.3448 0.1067 0.2611 0.046 Uiso 1 1 d R . .
C13 C -0.1268(5) 0.18670(14) 0.2820(3) 0.0410(7) Uani 1 1 d . . .
H13A H -0.1297 0.2142 0.3523 0.049 Uiso 1 1 d R . .


_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
Ni1 O1 2.0644(14) . ?
Ni1 O1 2.0644(14) 3_666 ?
Ni1 N5 2.0938(17) 4_666 ?
Ni1 N5 2.0938(17) 2 ?
Ni1 N2 2.1326(17) . ?
Ni1 N2 2.1326(17) 3_666 ?
Ni1 C7 2.481(2) . ?
Ni1 C7 2.481(2) 3_666 ?
O1 C7 1.263(3) . ?
N1 C5 1.327(3) . ?
N1 C1 1.338(4) . ?
N2 C6 1.328(3) . ?
N2 C7 1.383(3) . ?
N3 C8 1.334(3) . ?
N3 C6 1.334(3) . ?
N4 C8 1.323(3) . ?
N4 C7 1.358(3) . ?
N5 C11 1.328(3) . ?
N5 C12 1.339(3) . ?
N5 Ni1 2.0938(17) 2_545 ?
C1 C2 1.369(4) . ?
C1 H1A 0.9273 . ?
C2 C3 1.385(3) . ?
C2 H2A 0.9298 . ?
C3 C4 1.386(3) . ?
C3 C6 1.489(3) . ?
C4 C5 1.380(3) . ?
C4 H4A 0.9277 . ?
C5 H5A 0.9296 . ?
C8 C9 1.499(3) . ?
C9 C13 1.382(3) . ?
C9 C10 1.377(3) . ?
C10 C11 1.380(3) . ?
C10 H10A 0.9191 . ?
C11 H11A 0.9261 . ?
C12 C13 1.383(3) . ?
C12 H12A 0.9198 . ?
C13 H13A 0.9252 . ?

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
O1 Ni1 O1 180.00(6) . 3_666 ?
O1 Ni1 N5 89.51(7) . 4_666 ?
O1 Ni1 N5 90.49(7) 3_666 4_666 ?
O1 Ni1 N5 90.49(7) . 2 ?
O1 Ni1 N5 89.51(7) 3_666 2 ?
N5 Ni1 N5 180.0 4_666 2 ?
O1 Ni1 N2 64.23(6) . . ?
O1 Ni1 N2 115.77(6) 3_666 . ?
N5 Ni1 N2 85.57(7) 4_666 . ?
N5 Ni1 N2 94.43(7) 2 . ?
O1 Ni1 N2 115.77(6) . 3_666 ?
O1 Ni1 N2 64.23(6) 3_666 3_666 ?
N5 Ni1 N2 94.43(7) 4_666 3_666 ?
N5 Ni1 N2 85.57(7) 2 3_666 ?
N2 Ni1 N2 180.0 . 3_666 ?
O1 Ni1 C7 30.55(6) . . ?
O1 Ni1 C7 149.45(6) 3_666 . ?
N5 Ni1 C7 84.99(7) 4_666 . ?
N5 Ni1 C7 95.01(7) 2 . ?
N2 Ni1 C7 33.82(7) . . ?
N2 Ni1 C7 146.18(7) 3_666 . ?
O1 Ni1 C7 149.45(6) . 3_666 ?
O1 Ni1 C7 30.55(6) 3_666 3_666 ?
N5 Ni1 C7 95.01(7) 4_666 3_666 ?
N5 Ni1 C7 84.99(7) 2 3_666 ?
N2 Ni1 C7 146.18(7) . 3_666 ?
N2 Ni1 C7 33.82(7) 3_666 3_666 ?
C7 Ni1 C7 180.0 . 3_666 ?
C7 O1 Ni1 93.29(12) . . ?
C5 N1 C1 115.8(2) . . ?
C6 N2 C7 116.53(18) . . ?
C6 N2 Ni1 154.52(15) . . ?
C7 N2 Ni1 87.05(12) . . ?
C8 N3 C6 115.58(19) . . ?
C8 N4 C7 114.03(19) . . ?
C11 N5 C12 117.41(19) . . ?
C11 N5 Ni1 116.07(14) . 2_545 ?
C12 N5 Ni1 125.02(16) . 2_545 ?
N1 C1 C2 123.9(3) . . ?
N1 C1 H1A 117.9 . . ?
C2 C1 H1A 118.2 . . ?
C1 C2 C3 119.8(2) . . ?
C1 C2 H2A 119.2 . . ?
C3 C2 H2A 120.9 . . ?
C2 C3 C4 117.0(2) . . ?
C2 C3 C6 119.4(2) . . ?
C4 C3 C6 123.6(2) . . ?
C5 C4 C3 118.8(2) . . ?
C5 C4 H4A 120.7 . . ?
C3 C4 H4A 120.4 . . ?
N1 C5 C4 124.6(2) . . ?
N1 C5 H5A 118.7 . . ?
C4 C5 H5A 116.6 . . ?
N2 C6 N3 123.7(2) . . ?
N2 C6 C3 119.79(19) . . ?
N3 C6 C3 116.48(19) . . ?
O1 C7 N4 122.14(19) . . ?
O1 C7 N2 114.95(18) . . ?
N4 C7 N2 122.89(19) . . ?
O1 C7 Ni1 56.16(10) . . ?
N4 C7 Ni1 172.68(17) . . ?
N2 C7 Ni1 59.13(10) . . ?
N4 C8 N3 127.2(2) . . ?
N4 C8 C9 117.09(19) . . ?
N3 C8 C9 115.68(19) . . ?
C13 C9 C10 118.1(2) . . ?
C13 C9 C8 122.5(2) . . ?
C10 C9 C8 119.33(19) . . ?
C11 C10 C9 119.0(2) . . ?
C11 C10 H10A 120.5 . . ?
C9 C10 H10A 120.5 . . ?
N5 C11 C10 123.5(2) . . ?
N5 C11 H11A 117.8 . . ?
C10 C11 H11A 118.7 . . ?
N5 C12 C13 122.6(2) . . ?
N5 C12 H12A 118.5 . . ?
C13 C12 H12A 118.9 . . ?
C9 C13 C12 119.2(2) . . ?
C9 C13 H13A 120.2 . . ?
C12 C13 H13A 120.6 . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.073

#===END

data_complex_2'
_database_code_depnum_ccdc_archive 'CCDC 705318'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H17.20 N10 Ni O2.60'
_chemical_formula_weight         569.99

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/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                   7.0848(9)
_cell_length_b                   17.511(2)
_cell_length_c                   11.1614(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 121.096(6)
_cell_angle_gamma                90.00
_cell_volume                     1185.7(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2321
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      26.00

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             584
_exptl_absorpt_coefficient_mu    0.870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8053
_exptl_absorpt_correction_T_max  0.8316
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_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_%        negligible
_diffrn_reflns_number            6184
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.43
_diffrn_reflns_theta_max         26.00
_reflns_number_total             2321
_reflns_number_gt                2004
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0743P)²+0.8748P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2321
_refine_ls_number_parameters     187
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0455
_refine_ls_wR_factor_ref         0.1195
_refine_ls_wR_factor_gt          0.1137
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_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
Ni1 Ni 0.5000 0.5000 0.5000 0.01875(18) Uani 1 2 d S . .
O1 O 0.2633(3) 0.43261(10) 0.5047(2) 0.0250(4) Uani 1 1 d . . .
N1 N 0.7242(5) 0.41765(18) 0.0536(3) 0.0509(8) Uani 1 1 d . . .
N2 N 0.3599(4) 0.41245(12) 0.3458(2) 0.0248(5) Uani 1 1 d . . .
N3 N 0.2397(4) 0.30140(13) 0.2089(3) 0.0335(6) Uani 1 1 d . . .
N4 N 0.1213(4) 0.32470(13) 0.3704(2) 0.0288(5) Uani 1 1 d . . .
N5 N -0.2600(4) 0.08115(12) 0.1225(2) 0.0244(5) Uani 1 1 d . . .
C1 C 0.5989(7) 0.3549(2) 0.0231(4) 0.0531(9) Uani 1 1 d . . .
H1A H 0.5945 0.3211 -0.0425 0.064 Uiso 1 1 d R . .
C2 C 0.4777(6) 0.33740(19) 0.0829(4) 0.0429(8) Uani 1 1 d . . .
H2A H 0.3937 0.2930 0.0576 0.051 Uiso 1 1 d R . .
C3 C 0.4797(5) 0.38655(16) 0.1815(3) 0.0295(6) Uani 1 1 d . . .
C4 C 0.6078(5) 0.45182(17) 0.2134(3) 0.0365(7) Uani 1 1 d . . .
H4A H 0.6150 0.4868 0.2783 0.044 Uiso 1 1 d R . .
C5 C 0.7245(6) 0.4641(2) 0.1476(4) 0.0456(8) Uani 1 1 d . . .
H5A H 0.8091 0.5083 0.1706 0.055 Uiso 1 1 d R . .
C6 C 0.3523(5) 0.36662(15) 0.2488(3) 0.0265(6) Uani 1 1 d . . .
C7 C 0.2431(5) 0.38930(14) 0.4076(3) 0.0239(6) Uani 1 1 d . . .
C8 C 0.1284(5) 0.28462(15) 0.2724(3) 0.0275(6) Uani 1 1 d . . .
C9 C -0.0008(5) 0.21169(16) 0.2265(3) 0.0282(6) Uani 1 1 d . . .
C10 C 0.0083(5) 0.16620(16) 0.1286(3) 0.0328(7) Uani 1 1 d . . .
H10A H 0.1016 0.1785 0.0960 0.039 Uiso 1 1 d R . .
C11 C -0.1228(5) 0.10203(16) 0.0806(3) 0.0317(7) Uani 1 1 d . . .
H11A H -0.1150 0.0716 0.0150 0.038 Uiso 1 1 d R . .
C12 C -0.2613(6) 0.12358(18) 0.2218(3) 0.0400(8) Uani 1 1 d . . .
H12A H -0.3523 0.1088 0.2549 0.048 Uiso 1 1 d R . .
C13 C -0.1329(6) 0.18824(18) 0.2775(4) 0.0419(8) Uani 1 1 d . . .
H13A H -0.1358 0.2157 0.3478 0.050 Uiso 1 1 d R . .
O1W O 0.024(4) 0.5169(14) 0.0437(19) 0.171(9) Uani 0.30 1 d P . .
H1WA H -0.0378 0.4738 0.0451 0.256 Uiso 0.60 1 d PR . .


_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
Ni1 O1 2.0734(18) . ?
Ni1 O1 2.0734(18) 3_666 ?
Ni1 N5 2.093(2) 2 ?
Ni1 N5 2.093(2) 4_666 ?
Ni1 N2 2.129(2) 3_666 ?
Ni1 N2 2.129(2) . ?
Ni1 C7 2.489(3) 3_666 ?
Ni1 C7 2.489(3) . ?
O1 C7 1.269(3) . ?
N1 C5 1.327(5) . ?
N1 C1 1.341(5) . ?
N2 C6 1.327(4) . ?
N2 C7 1.384(3) . ?
N3 C6 1.331(3) . ?
N3 C8 1.337(4) . ?
N4 C8 1.322(4) . ?
N4 C7 1.351(3) . ?
N5 C11 1.330(4) . ?
N5 C12 1.338(4) . ?
N5 Ni1 2.093(2) 2_545 ?
C1 C2 1.367(5) . ?
C1 H1A 0.9300 . ?
C2 C3 1.392(4) . ?
C2 H2A 0.9300 . ?
C3 C4 1.387(4) . ?
C3 C6 1.483(4) . ?
C4 C5 1.377(5) . ?
C4 H4A 0.9300 . ?
C5 H5A 0.9300 . ?
C8 C9 1.499(4) . ?
C9 C10 1.380(4) . ?
C9 C13 1.386(4) . ?
C10 C11 1.378(4) . ?
C10 H10A 0.9299 . ?
C11 H11A 0.9300 . ?
C12 C13 1.383(4) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
O1W O1W 1.04(3) 3_565 ?
O1W H1WA 0.8760 . ?

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
O1 Ni1 O1 180.00(8) . 3_666 ?
O1 Ni1 N5 90.47(8) . 2 ?
O1 Ni1 N5 89.53(8) 3_666 2 ?
O1 Ni1 N5 89.53(8) . 4_666 ?
O1 Ni1 N5 90.47(8) 3_666 4_666 ?
N5 Ni1 N5 180.000(1) 2 4_666 ?
O1 Ni1 N2 115.79(8) . 3_666 ?
O1 Ni1 N2 64.21(8) 3_666 3_666 ?
N5 Ni1 N2 85.50(9) 2 3_666 ?
N5 Ni1 N2 94.50(9) 4_666 3_666 ?
O1 Ni1 N2 64.21(8) . . ?
O1 Ni1 N2 115.79(8) 3_666 . ?
N5 Ni1 N2 94.50(9) 2 . ?
N5 Ni1 N2 85.50(9) 4_666 . ?
N2 Ni1 N2 180.00(8) 3_666 . ?
O1 Ni1 C7 149.41(8) . 3_666 ?
O1 Ni1 C7 30.59(8) 3_666 3_666 ?
N5 Ni1 C7 85.15(9) 2 3_666 ?
N5 Ni1 C7 94.85(9) 4_666 3_666 ?
N2 Ni1 C7 33.74(9) 3_666 3_666 ?
N2 Ni1 C7 146.26(9) . 3_666 ?
O1 Ni1 C7 30.59(8) . . ?
O1 Ni1 C7 149.41(8) 3_666 . ?
N5 Ni1 C7 94.85(9) 2 . ?
N5 Ni1 C7 85.15(9) 4_666 . ?
N2 Ni1 C7 146.26(9) 3_666 . ?
N2 Ni1 C7 33.74(9) . . ?
C7 Ni1 C7 180.0 3_666 . ?
C7 O1 Ni1 93.14(15) . . ?
C5 N1 C1 115.7(3) . . ?
C6 N2 C7 116.6(2) . . ?
C6 N2 Ni1 154.3(2) . . ?
C7 N2 Ni1 87.56(15) . . ?
C6 N3 C8 115.2(2) . . ?
C8 N4 C7 114.0(2) . . ?
C11 N5 C12 117.3(2) . . ?
C11 N5 Ni1 116.84(18) . 2_545 ?
C12 N5 Ni1 124.6(2) . 2_545 ?
N1 C1 C2 124.1(3) . . ?
N1 C1 H1A 118.0 . . ?
C2 C1 H1A 117.9 . . ?
C1 C2 C3 119.7(3) . . ?
C1 C2 H2A 120.2 . . ?
C3 C2 H2A 120.1 . . ?
C4 C3 C2 116.8(3) . . ?
C4 C3 C6 123.6(3) . . ?
C2 C3 C6 119.6(3) . . ?
C5 C4 C3 119.1(3) . . ?
C5 C4 H4A 120.5 . . ?
C3 C4 H4A 120.4 . . ?
N1 C5 C4 124.7(3) . . ?
N1 C5 H5A 117.8 . . ?
C4 C5 H5A 117.5 . . ?
N2 C6 N3 123.9(3) . . ?
N2 C6 C3 119.5(2) . . ?
N3 C6 C3 116.6(2) . . ?
O1 C7 N4 122.4(2) . . ?
O1 C7 N2 114.7(2) . . ?
N4 C7 N2 122.9(2) . . ?
O1 C7 Ni1 56.28(13) . . ?
N4 C7 Ni1 173.4(2) . . ?
N2 C7 Ni1 58.70(13) . . ?
N4 C8 N3 127.4(2) . . ?
N4 C8 C9 117.3(2) . . ?
N3 C8 C9 115.4(2) . . ?
C10 C9 C13 118.1(3) . . ?
C10 C9 C8 119.5(2) . . ?
C13 C9 C8 122.3(2) . . ?
C11 C10 C9 118.8(3) . . ?
C11 C10 H10A 120.6 . . ?
C9 C10 H10A 120.6 . . ?
N5 C11 C10 123.7(3) . . ?
N5 C11 H11A 118.1 . . ?
C10 C11 H11A 118.1 . . ?
N5 C12 C13 122.9(3) . . ?
N5 C12 H12A 118.5 . . ?
C13 C12 H12A 118.6 . . ?
C12 C13 C9 119.0(3) . . ?
C12 C13 H13A 120.5 . . ?
C9 C13 H13A 120.5 . . ?
O1W O1W H1WA 66.6 3_565 . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.075

#===END


