# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_aaa
_database_code_depnum_ccdc_archive 'CCDC 1857018'
_audit_update_record             
;
2018-07-20 deposited with the CCDC.
2018-12-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C37 H49 Cl2 N17 Ni2 O9'
_chemical_formula_sum            'C37 H49 Cl2 N17 Ni2 O9'
_chemical_formula_weight         1064.25

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   P4(2)/mnm

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

_cell_length_a                   17.031(2)
_cell_length_b                   17.031(2)
_cell_length_c                   17.184(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4984.3(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3088
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.47

_exptl_crystal_description       block
_exptl_crystal_colour            blue-green
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2208
_exptl_absorpt_coefficient_mu    0.929
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7357
_exptl_absorpt_correction_T_max  0.7518
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            56827
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0142
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         27.47
_reflns_number_total             3088
_reflns_number_gt                2815
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXTL

_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)+(0.0783P)²+7.0104P] where P=(Fo²+2Fc²)/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         3088
_refine_ls_number_parameters     133
_refine_ls_number_restraints     67
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0486
_refine_ls_wR_factor_ref         0.1439
_refine_ls_wR_factor_gt          0.1411
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.079
_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
Ni1 Ni 0.78597(2) 0.36547(2) 0.0000 0.02097(16) Uani 1 2 d S . .
Cl1 Cl 0.64572(5) 0.35428(5) 0.0000 0.0304(3) Uani 1 4 d S . .
O1 O 0.78637(10) 0.69356(11) 0.41384(10) 0.0337(4) Uani 1 1 d . A .
O2 O 0.90949(16) 0.38199(17) 0.0000 0.0425(7) Uani 1 2 d SD . .
N1 N 0.74403(15) 0.54245(14) 0.16723(14) 0.0412(6) Uani 1 1 d D . .
N2 N 0.8213(9) 0.5257(10) 0.1865(10) 0.058(4) Uani 0.50 1 d PDU A 1
N2' N 0.8078(9) 0.5074(10) 0.2039(10) 0.058(4) Uani 0.50 1 d PDU A 2
N3 N 0.77953(13) 0.44990(13) 0.08780(13) 0.0351(5) Uani 1 1 d D . .
C1 C 0.64143(19) 0.64143(19) 0.1673(2) 0.0416(10) Uani 1 2 d S . .
H1 H 0.6233 0.6233 0.1195 0.050 Uiso 1 2 calc SR A .
C2 C 0.70465(17) 0.60626(17) 0.20440(16) 0.0374(6) Uani 1 1 d . A .
C3 C 0.73231(16) 0.63220(16) 0.27544(15) 0.0349(6) Uani 1 1 d . . .
H3 H 0.7749 0.6076 0.2990 0.042 Uiso 1 1 calc R A .
C4 C 0.69566(16) 0.69566(16) 0.3114(2) 0.0313(7) Uani 1 2 d S A .
C5 C 0.72540(17) 0.50225(16) 0.10349(16) 0.0364(6) Uani 1 1 d . A .
H5 H 0.6802 0.5102 0.0741 0.044 Uiso 1 1 calc R . .
C6 C 0.8389(11) 0.4685(12) 0.1381(10) 0.052(4) Uani 0.50 1 d PDU A 1
H6 H 0.8872 0.4431 0.1381 0.063 Uiso 0.50 1 calc PR A 1
C6' C 0.8258(11) 0.4529(12) 0.1529(9) 0.052(4) Uani 0.50 1 d PDU A 2
H6' H 0.8674 0.4184 0.1605 0.063 Uiso 0.50 1 calc PR A 2
C7 C 0.72804(15) 0.72804(15) 0.38652(19) 0.0276(7) Uani 1 2 d S . .
N4 N 1.0331(7) 0.3486(7) 0.0424(7) 0.138(2) Uani 0.50 1 d PDU . .
C8 C 0.9535(8) 0.3282(8) 0.0263(8) 0.138(2) Uani 0.50 1 d PDU . .
C9 C 1.0700(7) 0.4110(7) 0.0000 0.138(2) Uani 1 2 d SDU . .
C10 C 1.0723(18) 0.2717(11) 0.0559(18) 0.138(2) Uani 0.25 1 d PDU . 1
H10A H 1.1267 0.2802 0.0682 0.207 Uiso 0.25 1 calc PR . 1
H10B H 1.0684 0.2401 0.0098 0.207 Uiso 0.25 1 calc PR . 1
H10C H 1.0472 0.2451 0.0984 0.207 Uiso 0.25 1 calc PR . 1
C10' C 1.0864(17) 0.3104(16) 0.0992(15) 0.138(2) Uani 0.25 1 d PDU . 2
H10D H 1.1367 0.3357 0.0978 0.207 Uiso 0.25 1 calc PR . 2
H10E H 1.0924 0.2560 0.0859 0.207 Uiso 0.25 1 calc PR . 2
H10F H 1.0646 0.3148 0.1505 0.207 Uiso 0.25 1 calc PR . 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
Ni1 O1 2.0319(17) 3_644 ?
Ni1 O1 2.0319(17) 12_756 ?
Ni1 N3 2.087(2) . ?
Ni1 N3 2.087(2) 10 ?
Ni1 O2 2.122(3) . ?
Ni1 Cl1 2.3963(9) . ?
Cl1 Ni1 2.3963(9) 15_665 ?
O1 C7 1.246(2) . ?
O1 Ni1 2.0319(17) 11_676 ?
O2 C8 1.267(12) 10 ?
O2 C8 1.267(12) . ?
N1 C5 1.330(3) . ?
N1 N2 1.386(14) . ?
N1 N2' 1.390(13) . ?
N1 C2 1.428(3) . ?
N2 C6 1.315(14) . ?
N2' C6' 1.313(14) . ?
N3 C5 1.310(3) . ?
N3 C6 1.367(14) . ?
N3 C6' 1.368(14) . ?
C1 C2 1.387(3) 16 ?
C1 C2 1.387(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.381(3) . ?
C3 C4 1.393(3) . ?
C3 H3 0.9300 . ?
C4 C3 1.393(3) 16 ?
C4 C7 1.508(4) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C6' H6' 0.9300 . ?
C7 O1 1.246(2) 16 ?
N4 C8 1.427(13) . ?
N4 C9 1.433(11) . ?
N4 N4 1.46(2) 10 ?
N4 C10' 1.482(16) . ?
N4 C10 1.489(15) . ?
N4 C8 1.831(15) 10 ?
C8 C8 0.90(3) 10 ?
C8 N4 1.831(15) 10 ?
C9 N4 1.433(11) 10 ?
C10 C10 1.92(6) 10 ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C10' H10D 0.9600 . ?
C10' H10E 0.9600 . ?
C10' H10F 0.9600 . ?

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 93.55(11) 3_644 12_756 ?
O1 Ni1 N3 173.01(8) 3_644 . ?
O1 Ni1 N3 86.51(9) 12_756 . ?
O1 Ni1 N3 86.51(9) 3_644 10 ?
O1 Ni1 N3 173.01(8) 12_756 10 ?
N3 Ni1 N3 92.59(13) . 10 ?
O1 Ni1 O2 85.29(8) 3_644 . ?
O1 Ni1 O2 85.29(8) 12_756 . ?
N3 Ni1 O2 87.75(8) . . ?
N3 Ni1 O2 87.75(8) 10 . ?
O1 Ni1 Cl1 96.80(6) 3_644 . ?
O1 Ni1 Cl1 96.80(6) 12_756 . ?
N3 Ni1 Cl1 90.14(6) . . ?
N3 Ni1 Cl1 90.14(6) 10 . ?
O2 Ni1 Cl1 176.94(8) . . ?
Ni1 Cl1 Ni1 99.12(5) 15_665 . ?
C7 O1 Ni1 136.25(19) . 11_676 ?
C8 O2 C8 41.8(13) 10 . ?
C8 O2 Ni1 119.4(7) 10 . ?
C8 O2 Ni1 119.4(7) . . ?
C5 N1 N2 108.5(8) . . ?
C5 N1 N2' 109.8(8) . . ?
N2 N1 N2' 20.3(13) . . ?
C5 N1 C2 130.4(2) . . ?
N2 N1 C2 119.7(8) . . ?
N2' N1 C2 119.4(8) . . ?
C6 N2 N1 102.6(15) . . ?
C6' N2' N1 100.6(15) . . ?
C5 N3 C6 103.4(9) . . ?
C5 N3 C6' 102.2(9) . . ?
C6 N3 C6' 18.1(16) . . ?
C5 N3 Ni1 130.87(18) . . ?
C6 N3 Ni1 125.3(9) . . ?
C6' N3 Ni1 125.9(9) . . ?
C2 C1 C2 117.3(3) 16 . ?
C2 C1 H1 121.3 16 . ?
C2 C1 H1 121.3 . . ?
C3 C2 C1 122.2(3) . . ?
C3 C2 N1 118.6(2) . . ?
C1 C2 N1 119.2(2) . . ?
C2 C3 C4 119.2(2) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C3 C4 C3 119.9(3) 16 . ?
C3 C4 C7 119.97(16) 16 . ?
C3 C4 C7 119.97(16) . . ?
N3 C5 N1 110.6(2) . . ?
N3 C5 H5 124.7 . . ?
N1 C5 H5 124.7 . . ?
N2 C6 N3 113.8(17) . . ?
N2 C6 H6 123.1 . . ?
N3 C6 H6 123.1 . . ?
N2' C6' N3 115.9(17) . . ?
N2' C6' H6' 122.0 . . ?
N3 C6' H6' 122.0 . . ?
O1 C7 O1 127.6(3) 16 . ?
O1 C7 C4 116.21(15) 16 . ?
O1 C7 C4 116.21(15) . . ?
C8 N4 C9 119.9(12) . . ?
C8 N4 N4 78.8(8) . 10 ?
C9 N4 N4 59.4(6) . 10 ?
C8 N4 C10' 127.0(15) . . ?
C9 N4 C10' 113.1(13) . . ?
N4 N4 C10' 131.1(14) 10 . ?
C8 N4 C10 104.0(16) . . ?
C9 N4 C10 122.3(14) . . ?
N4 N4 C10 99.0(13) 10 . ?
C10' N4 C10 40.2(16) . . ?
C8 N4 C8 28.9(9) . 10 ?
C9 N4 C8 97.9(9) . 10 ?
N4 N4 C8 49.9(5) 10 10 ?
C10' N4 C8 142.5(15) . 10 ?
C10 N4 C8 105.4(16) . 10 ?
C8 C8 O2 69.1(7) 10 . ?
C8 C8 N4 101.2(8) 10 . ?
O2 C8 N4 117.1(12) . . ?
C8 C8 N4 49.9(5) 10 10 ?
O2 C8 N4 94.1(9) . 10 ?
N4 C8 N4 51.4(10) . 10 ?
N4 C9 N4 61.1(11) 10 . ?
N4 C10 C10 81.0(13) . 10 ?
N4 C10 H10A 109.5 . . ?
C10 C10 H10A 102.7 10 . ?
N4 C10 H10B 109.5 . . ?
C10 C10 H10B 34.4 10 . ?
H10A C10 H10B 109.5 . . ?
N4 C10 H10C 109.5 . . ?
C10 C10 H10C 139.6 10 . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C10' H10D 109.5 . . ?
N4 C10' H10E 109.5 . . ?
H10D C10' H10E 109.5 . . ?
N4 C10' H10F 109.5 . . ?
H10D C10' H10F 109.5 . . ?
H10E C10' H10F 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.026
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.080
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_aaa_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1857019'
_audit_update_record             
;
2018-07-20 deposited with the CCDC.
2018-12-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C37 H41 Cl Co2 N17 O9'
_chemical_formula_sum            'C37 H41 Cl Co2 N17 O9'
_chemical_formula_weight         1021.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   P4(2)/mnm

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

_cell_length_a                   17.274(2)
_cell_length_b                   17.274(2)
_cell_length_c                   17.178(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5125.6(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2496
_cell_measurement_theta_min      1.67
_cell_measurement_theta_max      25.15

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2100
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7357
_exptl_absorpt_correction_T_max  0.7518
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            32057
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         25.15
_reflns_number_total             2496
_reflns_number_gt                2138
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXTL

_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)+(0.0805P)²+6.7250P] where P=(Fo²+2Fc²)/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         2496
_refine_ls_number_parameters     125
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.1462
_refine_ls_wR_factor_gt          0.1419
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_restrained_S_all      1.107
_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 0.13398(3) 0.28369(3) 0.0000 0.0188(2) Uani 1 2 d S . .
Cl1 Cl 0.14301(6) 0.14301(6) 0.0000 0.0315(4) Uani 1 4 d S . .
O1 O -0.19621(12) 0.28765(12) 0.41221(12) 0.0292(5) Uani 1 1 d . . .
O2 O 0.1159(2) 0.40743(19) 0.0000 0.0450(9) Uani 1 2 d S . .
N1 N -0.04489(16) 0.24388(16) 0.16722(16) 0.0372(7) Uani 1 1 d . . .
N2 N -0.0180(2) 0.3122(2) 0.1958(2) 0.0753(14) Uani 1 1 d . . .
N3 N 0.04767(15) 0.27761(16) 0.08921(15) 0.0344(6) Uani 1 1 d . . .
C1 C -0.1435(2) 0.1435(2) 0.1678(3) 0.0381(12) Uani 1 2 d S . .
H1 H -0.1256 0.1256 0.1200 0.046 Uiso 1 2 calc SR . .
C2 C -0.10875(19) 0.20557(19) 0.20400(19) 0.0346(8) Uani 1 1 d . . .
C3 C -0.13553(18) 0.23395(19) 0.27409(18) 0.0310(7) Uani 1 1 d . . .
H3 H -0.1119 0.2765 0.2973 0.037 Uiso 1 1 calc R . .
C4 C -0.19819(18) 0.19819(18) 0.3095(2) 0.0258(9) Uani 1 2 d S . .
C5 C -0.00503(18) 0.22504(19) 0.10410(18) 0.0335(7) Uani 1 1 d . . .
H5 H -0.0133 0.1807 0.0745 0.040 Uiso 1 1 calc R . .
C6 C 0.0370(3) 0.3292(3) 0.1466(2) 0.0640(13) Uani 1 1 d . . .
H6 H 0.0667 0.3740 0.1510 0.077 Uiso 1 1 calc R . .
C7 C -0.23021(16) 0.23021(16) 0.3847(2) 0.0227(8) Uani 1 2 d S . .
N4 N 0.1456(7) 0.5303(7) 0.0275(6) 0.115(2) Uani 0.50 1 d PDU . .
C8 C 0.1524(8) 0.4519(8) 0.0332(8) 0.115(2) Uani 0.50 1 d PDU . .
C9 C 0.0914(8) 0.5632(8) -0.0319(7) 0.115(2) Uani 0.50 1 d PDU . .
C10 C 0.1575(9) 0.5796(8) 0.0851(8) 0.115(2) Uani 0.50 1 d PDU . .


_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 2.0561(19) 12_666 ?
Co1 O1 2.0561(19) 3_554 ?
Co1 N3 2.141(3) 10 ?
Co1 N3 2.141(3) . ?
Co1 O2 2.160(3) . ?
Co1 Cl1 2.4351(12) . ?
Cl1 Co1 2.4351(12) 7 ?
O1 C7 1.246(3) . ?
O1 Co1 2.0561(19) 11_566 ?
O2 C8 1.145(14) . ?
O2 C8 1.145(14) 10 ?
N1 C5 1.325(4) . ?
N1 N2 1.359(4) . ?
N1 C2 1.433(4) . ?
N2 C6 1.305(5) . ?
N3 C5 1.311(4) . ?
N3 C6 1.342(4) . ?
C1 C2 1.377(4) 15 ?
C1 C2 1.377(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.380(4) . ?
C3 C4 1.386(4) . ?
C3 H3 0.9300 . ?
C4 C3 1.386(4) 15 ?
C4 C7 1.511(5) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 O1 1.246(3) 15 ?
N4 N4 0.94(2) 10 ?
N4 C9 1.097(14) 10 ?
N4 C10 1.322(13) . ?
N4 C8 1.364(13) . ?
N4 C9 1.496(12) . ?
N4 C8 1.714(14) 10 ?
C8 C8 1.14(3) 10 ?
C8 N4 1.714(14) 10 ?
C9 C9 1.10(2) 10 ?
C9 N4 1.097(14) 10 ?
C9 C10 1.490(18) 10 ?
C10 C9 1.490(18) 10 ?

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 94.36(12) 12_666 3_554 ?
O1 Co1 N3 172.72(10) 12_666 10 ?
O1 Co1 N3 86.66(10) 3_554 10 ?
O1 Co1 N3 86.66(10) 12_666 . ?
O1 Co1 N3 172.72(10) 3_554 . ?
N3 Co1 N3 91.44(15) 10 . ?
O1 Co1 O2 85.86(9) 12_666 . ?
O1 Co1 O2 85.86(9) 3_554 . ?
N3 Co1 O2 87.03(10) 10 . ?
N3 Co1 O2 87.03(10) . . ?
O1 Co1 Cl1 97.26(6) 12_666 . ?
O1 Co1 Cl1 97.26(6) 3_554 . ?
N3 Co1 Cl1 89.75(8) 10 . ?
N3 Co1 Cl1 89.75(8) . . ?
O2 Co1 Cl1 175.38(10) . . ?
Co1 Cl1 Co1 97.35(6) . 7 ?
C7 O1 Co1 136.3(2) . 11_566 ?
C8 O2 C8 59.7(14) . 10 ?
C8 O2 Co1 125.7(8) . . ?
C8 O2 Co1 125.7(8) 10 . ?
C5 N1 N2 109.3(3) . . ?
C5 N1 C2 130.3(3) . . ?
N2 N1 C2 120.3(3) . . ?
C6 N2 N1 102.2(3) . . ?
C5 N3 C6 102.8(3) . . ?
C5 N3 Co1 131.1(2) . . ?
C6 N3 Co1 126.1(2) . . ?
C2 C1 C2 118.3(4) 15 . ?
C2 C1 H1 120.8 15 . ?
C2 C1 H1 120.8 . . ?
C1 C2 C3 121.6(3) . . ?
C1 C2 N1 119.7(3) . . ?
C3 C2 N1 118.6(3) . . ?
C2 C3 C4 119.1(3) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C3 C4 C3 120.2(4) 15 . ?
C3 C4 C7 119.84(19) 15 . ?
C3 C4 C7 119.84(19) . . ?
N3 C5 N1 110.5(3) . . ?
N3 C5 H5 124.7 . . ?
N1 C5 H5 124.7 . . ?
N2 C6 N3 115.2(3) . . ?
N2 C6 H6 122.4 . . ?
N3 C6 H6 122.4 . . ?
O1 C7 O1 127.3(3) 15 . ?
O1 C7 C4 116.33(17) 15 . ?
O1 C7 C4 116.33(17) . . ?
N4 N4 C9 94.0(9) 10 10 ?
N4 N4 C10 138.5(8) 10 . ?
C9 N4 C10 75.4(11) 10 . ?
N4 N4 C8 94.1(8) 10 . ?
C9 N4 C8 125.7(14) 10 . ?
C10 N4 C8 124.9(12) . . ?
N4 N4 C9 47.0(6) 10 . ?
C9 N4 C9 47.0(12) 10 . ?
C10 N4 C9 111.4(12) . . ?
C8 N4 C9 118.7(12) . . ?
N4 N4 C8 52.6(5) 10 10 ?
C9 N4 C8 120.7(13) 10 10 ?
C10 N4 C8 162.5(12) . 10 ?
C8 N4 C8 41.5(10) . 10 ?
C9 N4 C8 85.9(9) . 10 ?
C8 C8 O2 60.2(7) 10 . ?
C8 C8 N4 85.9(8) 10 . ?
O2 C8 N4 125.6(13) . . ?
C8 C8 N4 52.6(5) 10 10 ?
O2 C8 N4 101.0(10) . 10 ?
N4 C8 N4 33.3(8) . 10 ?
C9 C9 N4 86.0(9) 10 10 ?
C9 C9 C10 127.8(8) 10 10 ?
N4 C9 C10 59.2(9) 10 10 ?
C9 C9 N4 47.0(6) 10 . ?
N4 C9 N4 39.0(10) 10 . ?
C10 C9 N4 90.6(10) 10 . ?
N4 C10 C9 45.4(7) . 10 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.15
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.076
