# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014


data_complex-1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H52 Cl4 Co2 N12 O18'
_chemical_formula_weight         1248.60

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           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5833(5)
_cell_length_b                   10.7937(5)
_cell_length_c                   12.7878(6)
_cell_angle_alpha                82.279(3)
_cell_angle_beta                 71.692(3)
_cell_angle_gamma                64.544(3)
_cell_volume                     1252.20(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    20936
_cell_measurement_theta_min      1.0
_cell_measurement_theta_max      27.48

_exptl_crystal_description       ?
_exptl_crystal_colour            Brown
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             642
_exptl_absorpt_coefficient_mu    0.962
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8692
_exptl_absorpt_correction_T_max  0.9625
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device_type  'CCD AREA DETECTOR'
_diffrn_detector_area_resol_mean 9
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_measurement_method       CCD
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_reflns_number            9526
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0576
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.68
_diffrn_reflns_theta_max         27.44
_reflns_number_total             5644
_reflns_number_gt                4361
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER APEX-II'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'
_computing_cell_refinement       'BRUKER APEX-II'
_computing_data_reduction        'BRUKER APEX-II'

_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)+(0.1450P)²+7.7144P] where P=(Fo²+2Fc²)/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         5644
_refine_ls_number_parameters     326
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1183
_refine_ls_R_factor_gt           0.0945
_refine_ls_wR_factor_ref         0.2426
_refine_ls_wR_factor_gt          0.2130
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.002
_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 0.54336(8) 0.08349(7) 0.82866(5) 0.0194(2) Uani 1 1 d . . .
Cl1 Cl 0.1222(2) -0.2507(2) 0.84715(15) 0.0444(4) Uani 1 1 d . . .
Cl2 Cl 0.0832(2) 0.24357(19) 0.5859(2) 0.0565(6) Uani 1 1 d . . .
O1 O 0.5295(6) 0.0500(5) 0.9778(3) 0.0374(11) Uani 1 1 d . . .
N1 N 0.6280(5) -0.1116(5) 0.7949(3) 0.0207(9) Uani 1 1 d . . .
N5 N 0.5819(5) 0.1138(5) 0.6663(4) 0.0252(10) Uani 1 1 d . . .
N4 N 0.7284(6) 0.0905(5) 0.7973(4) 0.0310(11) Uani 1 1 d . . .
N3 N 0.4575(6) 0.2825(5) 0.8646(4) 0.0275(10) Uani 1 1 d . . .
H3N H 0.4755 0.3284 0.7984 0.033 Uiso 1 1 calc R . .
N6 N 0.5720(7) 0.4280(6) 0.6426(5) 0.0425(14) Uani 1 1 d . . .
C5 C 0.5326(6) -0.1602(6) 0.7876(4) 0.0242(11) Uani 1 1 d . . .
C12 C 0.7789(8) 0.1246(7) 0.8786(5) 0.0336(14) Uani 1 1 d . . .
H12A H 0.8839 0.1056 0.8498 0.040 Uiso 1 1 calc R . .
H12B H 0.7629 0.0724 0.9476 0.040 Uiso 1 1 calc R . .
C1 C 0.7686(7) -0.1983(6) 0.7774(5) 0.0295(12) Uani 1 1 d . . .
H1 H 0.8365 -0.1664 0.7841 0.035 Uiso 1 1 calc R . .
N2 N 0.3650(6) 0.0633(6) 0.8434(4) 0.0309(11) Uani 1 1 d . . .
C18 C 0.4940(7) 0.1349(6) 0.6050(5) 0.0293(12) Uani 1 1 d . . .
H18 H 0.3979 0.1411 0.6400 0.035 Uiso 1 1 calc R . .
C15 C 0.7716(7) 0.1138(6) 0.5022(5) 0.0314(13) Uani 1 1 d . . .
H15 H 0.8692 0.1037 0.4682 0.038 Uiso 1 1 calc R . .
C17 C 0.5378(8) 0.1481(7) 0.4915(5) 0.0364(14) Uani 1 1 d . . .
H17 H 0.4723 0.1632 0.4500 0.044 Uiso 1 1 calc R . .
C14 C 0.7205(7) 0.1035(6) 0.6148(5) 0.0282(12) Uani 1 1 d . . .
C19 C 0.6428(8) 0.4481(6) 0.5598(6) 0.0353(14) Uani 1 1 d . . .
C2 C 0.8167(7) -0.3349(7) 0.7494(5) 0.0355(14) Uani 1 1 d . . .
H2 H 0.9169 -0.3953 0.7374 0.043 Uiso 1 1 calc R . .
C4 C 0.5766(8) -0.2948(7) 0.7591(5) 0.0352(14) Uani 1 1 d . . .
H4 H 0.5078 -0.3262 0.7534 0.042 Uiso 1 1 calc R . .
O8 O 0.0392(7) -0.3292(7) 0.8984(6) 0.070(2) Uani 1 1 d . . .
C11 C 0.6847(10) 0.2784(8) 0.8973(7) 0.050(2) Uani 1 1 d . . .
H11A H 0.7133 0.3108 0.9513 0.060 Uiso 1 1 calc R . .
H11B H 0.7061 0.3270 0.8271 0.060 Uiso 1 1 calc R . .
O2 O 0.2183(10) 0.2181(9) 0.5079(8) 0.0954(13) Uani 1 1 d . . .
C6 C 0.3825(7) -0.0549(7) 0.8181(5) 0.0351(14) Uani 1 1 d . . .
H6 H 0.3021 -0.0734 0.8191 0.042 Uiso 1 1 calc R . .
C16 C 0.6766(8) 0.1394(7) 0.4392(5) 0.0334(14) Uani 1 1 d . . .
H16 H 0.7071 0.1506 0.3617 0.040 Uiso 1 1 calc R . .
C7 C 0.2154(7) 0.1726(7) 0.8818(6) 0.0386(15) Uani 1 1 d . . .
H7A H 0.1766 0.1628 0.9622 0.046 Uiso 1 1 calc R . .
H7B H 0.1516 0.1598 0.8458 0.046 Uiso 1 1 calc R . .
C3 C 0.7215(9) -0.3821(7) 0.7393(5) 0.0380(15) Uani 1 1 d . . .
H3 H 0.7547 -0.4747 0.7186 0.046 Uiso 1 1 calc R . .
O5 O 0.1035(10) 0.1389(10) 0.6728(8) 0.0954(13) Uani 1 1 d . . .
C13 C 0.7954(7) 0.0941(7) 0.6942(6) 0.0339(13) Uani 1 1 d . . .
H13 H 0.8914 0.0906 0.6713 0.041 Uiso 1 1 calc R . .
C8 C 0.2090(8) 0.3147(8) 0.8579(7) 0.051(2) Uani 1 1 d . . .
H8A H 0.1058 0.3821 0.8804 0.061 Uiso 1 1 calc R . .
H8B H 0.2487 0.3246 0.7777 0.061 Uiso 1 1 calc R . .
C9 C 0.2946(9) 0.3461(7) 0.9178(7) 0.0481(19) Uani 1 1 d . . .
H9A H 0.2608 0.4468 0.9209 0.058 Uiso 1 1 calc R . .
H9B H 0.2736 0.3123 0.9945 0.058 Uiso 1 1 calc R . .
O6 O 0.0680(7) -0.1725(9) 0.7573(6) 0.079(2) Uani 1 1 d . . .
C20 C 0.7350(8) 0.4716(8) 0.4548(6) 0.0460(17) Uani 1 1 d . . .
H20A H 0.8248 0.3881 0.4322 0.069 Uiso 1 1 calc R . .
H20B H 0.7598 0.5469 0.4625 0.069 Uiso 1 1 calc R . .
H20C H 0.6826 0.4956 0.3990 0.069 Uiso 1 1 calc R . .
O9 O 0.2709(7) -0.3369(9) 0.8083(7) 0.087(3) Uani 1 1 d . . .
O7 O 0.0990(11) -0.1538(10) 0.9195(9) 0.101(3) Uani 1 1 d . . .
C10 C 0.5228(10) 0.3174(7) 0.9379(6) 0.0454(19) Uani 1 1 d . . .
H10A H 0.5015 0.2722 1.0099 0.055 Uiso 1 1 calc R . .
H10B H 0.4730 0.4177 0.9509 0.055 Uiso 1 1 calc R . .
O4 O 0.0095(10) 0.2134(9) 0.5126(8) 0.0954(13) Uani 1 1 d . . .
O3 O 0.0111(10) 0.3783(10) 0.6168(8) 0.0954(13) Uani 1 1 d . . .


_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 1.864(4) . ?
Co1 N4 1.904(5) . ?
Co1 N2 1.940(5) . ?
Co1 N1 1.949(5) . ?
Co1 N3 1.994(5) . ?
Co1 N5 1.997(5) . ?
Cl1 O7 1.382(8) . ?
Cl1 O9 1.402(7) . ?
Cl1 O8 1.431(6) . ?
Cl1 O6 1.448(7) . ?
Cl2 O3 1.366(9) . ?
Cl2 O2 1.397(9) . ?
Cl2 O5 1.471(10) . ?
Cl2 O4 1.534(10) . ?
O1 O1 1.439(8) 2_657 ?
N1 C1 1.337(8) . ?
N1 C5 1.354(7) . ?
N5 C18 1.326(8) . ?
N5 C14 1.367(8) . ?
N4 C13 1.291(9) . ?
N4 C12 1.457(7) . ?
N3 C10 1.492(8) . ?
N3 C9 1.509(9) . ?
N6 C19 1.144(9) . ?
C5 C4 1.384(9) . ?
C5 C6 1.465(9) . ?
C12 C11 1.530(10) . ?
C1 C2 1.394(9) . ?
N2 C6 1.280(9) . ?
N2 C7 1.483(8) . ?
C18 C17 1.385(9) . ?
C15 C14 1.377(9) . ?
C15 C16 1.394(9) . ?
C17 C16 1.376(10) . ?
C14 C13 1.442(9) . ?
C19 C20 1.455(10) . ?
C2 C3 1.353(10) . ?
C4 C3 1.372(11) . ?
C11 C10 1.504(12) . ?
C7 C8 1.500(11) . ?
C8 C9 1.513(13) . ?

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 N4 92.5(2) . . ?
O1 Co1 N2 92.9(2) . . ?
N4 Co1 N2 172.8(2) . . ?
O1 Co1 N1 92.56(19) . . ?
N4 Co1 N1 93.8(2) . . ?
N2 Co1 N1 81.2(2) . . ?
O1 Co1 N3 86.9(2) . . ?
N4 Co1 N3 86.0(2) . . ?
N2 Co1 N3 99.0(2) . . ?
N1 Co1 N3 179.40(19) . . ?
O1 Co1 N5 173.6(2) . . ?
N4 Co1 N5 81.3(2) . . ?
N2 Co1 N5 93.1(2) . . ?
N1 Co1 N5 86.20(19) . . ?
N3 Co1 N5 94.3(2) . . ?
O7 Cl1 O9 111.2(6) . . ?
O7 Cl1 O8 110.4(6) . . ?
O9 Cl1 O8 110.6(4) . . ?
O7 Cl1 O6 105.1(6) . . ?
O9 Cl1 O6 110.4(5) . . ?
O8 Cl1 O6 108.9(5) . . ?
O3 Cl2 O2 111.3(6) . . ?
O3 Cl2 O5 118.1(6) . . ?
O2 Cl2 O5 109.0(5) . . ?
O3 Cl2 O4 109.6(6) . . ?
O2 Cl2 O4 98.0(6) . . ?
O5 Cl2 O4 109.0(5) . . ?
O1 O1 Co1 112.4(4) 2_657 . ?
C1 N1 C5 118.5(5) . . ?
C1 N1 Co1 126.4(4) . . ?
C5 N1 Co1 115.1(4) . . ?
C18 N5 C14 118.4(5) . . ?
C18 N5 Co1 128.3(4) . . ?
C14 N5 Co1 113.2(4) . . ?
C13 N4 C12 118.8(5) . . ?
C13 N4 Co1 115.5(4) . . ?
C12 N4 Co1 123.9(4) . . ?
C10 N3 C9 105.7(5) . . ?
C10 N3 Co1 114.4(4) . . ?
C9 N3 Co1 115.4(4) . . ?
N1 C5 C4 122.2(6) . . ?
N1 C5 C6 111.2(5) . . ?
C4 C5 C6 126.6(6) . . ?
N4 C12 C11 103.2(5) . . ?
N1 C1 C2 120.9(6) . . ?
C6 N2 C7 119.7(6) . . ?
C6 N2 Co1 115.4(4) . . ?
C7 N2 Co1 124.9(5) . . ?
N5 C18 C17 122.1(6) . . ?
C14 C15 C16 118.5(6) . . ?
C16 C17 C18 119.8(6) . . ?
N5 C14 C15 122.4(6) . . ?
N5 C14 C13 110.8(5) . . ?
C15 C14 C13 126.5(6) . . ?
N6 C19 C20 179.1(8) . . ?
C3 C2 C1 120.4(6) . . ?
C3 C4 C5 118.7(6) . . ?
C10 C11 C12 114.9(6) . . ?
N2 C6 C5 116.7(6) . . ?
C17 C16 C15 118.8(6) . . ?
N2 C7 C8 113.4(6) . . ?
C2 C3 C4 119.3(6) . . ?
N4 C13 C14 118.2(6) . . ?
C7 C8 C9 112.1(6) . . ?
N3 C9 C8 113.5(6) . . ?
N3 C10 C11 116.5(6) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.44
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         2.015
_refine_diff_density_min         -1.288
_refine_diff_density_rms         0.130
_database_code_depnum_ccdc_archive 'CCDC 959180'

data_complex-2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H54 Cl4 Co2 N10 O18'
_chemical_formula_weight         1222.59

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           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   20.0273(6)
_cell_length_b                   12.7577(5)
_cell_length_c                   21.1058(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.357(2)
_cell_angle_gamma                90.00
_cell_volume                     5055.8(3)
_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       ?
_exptl_crystal_colour            dark-brown
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2520
_exptl_absorpt_coefficient_mu    0.950
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device_type  'CCD AREA DETECTOR'
_diffrn_detector_area_resol_mean 9
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_measurement_method       CCD
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_reflns_number            18412
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.31
_diffrn_reflns_theta_max         26.37
_reflns_number_total             5119
_reflns_number_gt                3970
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER APEX-II'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'
_computing_cell_refinement       'BRUKER APEX-II'
_computing_data_reduction        'BRUKER APEX-II'

_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
 [0.00000+1.00000exp(0.13(sinθ/λ)²)]/
   [σ²(Fo²)+0.0000+39.7468*P+(0.1164P)²+0.0000sinθ/λ]
 where P = 0.33333Fo² + 0.66667Fc²
;
_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         5119
_refine_ls_number_parameters     366
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0789
_refine_ls_wR_factor_ref         0.2272
_refine_ls_wR_factor_gt          0.2089
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.049
_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
Co1 Co 0.27406(4) 0.14116(5) 0.08997(3) 0.0337(2) Uani 1 1 d . . .
Cl1 Cl 0.31622(9) 0.28113(12) 0.36949(7) 0.0555(5) Uani 1 1 d . . .
O1 O 0.2278(2) 0.2114(3) 0.00777(19) 0.0465(10) Uani 1 1 d . . .
N4 N 0.3042(2) 0.0225(3) 0.0499(2) 0.0340(9) Uani 1 1 d . . .
N5 N 0.3244(2) 0.0606(3) 0.1731(2) 0.0352(9) Uani 1 1 d . . .
N1 N 0.3610(2) 0.2196(3) 0.1102(2) 0.0357(9) Uani 1 1 d . . .
C18 C 0.4151(3) -0.0536(4) 0.2807(3) 0.0403(12) Uani 1 1 d . . .
H18 H 0.4455 -0.0917 0.3168 0.048 Uiso 1 1 calc R . .
O4 O 0.2651(3) 0.3635(4) 0.3489(3) 0.0691(14) Uani 1 1 d . . .
O5 O 0.3564(3) 0.2837(4) 0.3245(3) 0.0669(13) Uani 1 1 d . . .
C14 C 0.3417(3) -0.0493(4) 0.0895(2) 0.0335(10) Uani 1 1 d . . .
C19 C 0.3800(3) 0.0324(5) 0.2921(3) 0.0439(13) Uani 1 1 d . . .
H19 H 0.3868 0.0540 0.3360 0.053 Uiso 1 1 calc R . .
C5 C 0.3644(3) 0.3068(4) 0.1479(3) 0.0404(12) Uani 1 1 d . . .
C16 C 0.3599(3) -0.0246(4) 0.1621(2) 0.0333(10) Uani 1 1 d . . .
C7 C 0.2885(4) 0.4257(4) 0.1956(3) 0.0495(14) Uani 1 1 d . . .
H7A H 0.2421 0.4255 0.1992 0.074 Uiso 1 1 calc R . .
H7B H 0.2931 0.4857 0.1699 0.074 Uiso 1 1 calc R . .
H7C H 0.3241 0.4288 0.2399 0.074 Uiso 1 1 calc R . .
C6 C 0.2983(3) 0.3282(4) 0.1608(3) 0.0402(12) Uani 1 1 d . . .
N2 N 0.2500(2) 0.2586(4) 0.1372(2) 0.0412(10) Uani 1 1 d . C .
C8 C 0.1788(4) 0.2743(6) 0.1441(4) 0.068(2) Uani 1 1 d . . .
H8A H 0.1530(19) 0.299(2) 0.113(2) 0.081 Uiso 1 1 calc R A 1
H8B H 0.1821(5) 0.309(3) 0.174(2) 0.081 Uiso 1 1 calc R A 1
C1 C 0.4164(3) 0.1950(4) 0.0918(3) 0.0425(12) Uani 1 1 d . . .
H1 H 0.4134 0.1365 0.0646 0.051 Uiso 1 1 calc R . .
O2 O 0.2916(5) 0.1825(5) 0.3724(4) 0.119(3) Uani 1 1 d . . .
C15 C 0.3639(3) -0.1519(4) 0.0695(3) 0.0469(13) Uani 1 1 d . . .
H15A H 0.3486 -0.1560 0.0211 0.070 Uiso 1 1 calc R . .
H15B H 0.3426 -0.2078 0.0863 0.070 Uiso 1 1 calc R . .
H15C H 0.4148 -0.1579 0.0882 0.070 Uiso 1 1 calc R . .
C2 C 0.4783(3) 0.2544(5) 0.1120(3) 0.0482(14) Uani 1 1 d . . .
H2 H 0.5163 0.2351 0.0988 0.058 Uiso 1 1 calc R . .
C13 C 0.2690(3) 0.0051(4) -0.0230(3) 0.0433(13) Uani 1 1 d . . .
H13A H 0.2959 -0.0443 -0.0396 0.052 Uiso 1 1 calc . . .
H13B H 0.2648 0.0705 -0.0476 0.052 Uiso 1 1 calc . . .
C20 C 0.3339(3) 0.0872(4) 0.2371(3) 0.0411(12) Uani 1 1 d . . .
H20 H 0.3090 0.1442 0.2451 0.049 Uiso 1 1 calc R . .
C12 C 0.1948(4) -0.0393(5) -0.0317(3) 0.0503(15) Uani 1 1 d . C .
H12A H 0.1691 -0.0507 -0.0794 0.060 Uiso 1 1 calc . . .
H12B H 0.2007 -0.1069 -0.0094 0.060 Uiso 1 1 calc . . .
C3 C 0.4835(3) 0.3415(5) 0.1516(3) 0.0523(15) Uani 1 1 d . . .
H3 H 0.5248 0.3817 0.1657 0.063 Uiso 1 1 calc R . .
N3 N 0.1850(2) 0.0570(4) 0.0697(2) 0.0432(11) Uani 1 1 d . C .
H3N H 0.1992 -0.0054 0.0910 0.052 Uiso 1 1 calc R . .
C17 C 0.4048(3) -0.0831(4) 0.2145(3) 0.0369(11) Uani 1 1 d . . .
H17 H 0.4279 -0.1416 0.2058 0.044 Uiso 1 1 calc R . .
O3 O 0.3695(4) 0.3116(7) 0.4355(3) 0.112(3) Uani 1 1 d . . .
C4 C 0.4257(3) 0.3679(5) 0.1700(3) 0.0490(14) Uani 1 1 d . . .
H4 H 0.4279 0.4263 0.1971 0.059 Uiso 1 1 calc R . .
C10 C 0.1324(4) 0.0987(7) 0.0973(5) 0.076(2) Uani 1 1 d . . .
H10A H 0.099(2) 0.135(2) 0.063(2) 0.091 Uiso 1 1 calc R B 1
H10B H 0.1094(16) 0.042(4) 0.1074(8) 0.091 Uiso 1 1 calc R B 1
C11 C 0.1499(3) 0.0298(5) -0.0039(3) 0.0522(15) Uani 1 1 d . . .
H11A H 0.1390 0.0942 -0.0299 0.063 Uiso 1 1 calc . . .
H11B H 0.1053 -0.0056 -0.0100 0.063 Uiso 1 1 calc . . .
C9B C 0.1176(6) 0.2086(9) 0.0905(6) 0.052(3) Uani 0.55 1 d P C 2
H9B1 H 0.0727 0.2222 0.0968 0.063 Uiso 0.55 1 calc PR C 2
H9B2 H 0.1131 0.2310 0.0453 0.063 Uiso 0.55 1 calc PR C 2
C9A C 0.1529(9) 0.1652(18) 0.1547(8) 0.077(5) Uani 0.45 1 d P C 1
H9A1 H 0.1905 0.1308 0.1908 0.092 Uiso 0.45 1 calc PR C 1
H9A2 H 0.1125 0.1732 0.1697 0.092 Uiso 0.45 1 calc PR C 1
Cl3 Cl 0.5000 0.0000 0.0000 0.0598(7) Uani 1 2 d SD . .
Cl2 Cl 0.0113(2) 0.1397(2) 0.23575(18) 0.0541(8) Uani 0.50 1 d P . .
O9 O 0.4921(5) -0.0105(7) 0.0679(4) 0.052(2) Uani 0.50 1 d P . .
O11 O 0.5764(5) -0.0215(9) 0.0171(6) 0.074(3) Uani 0.50 1 d P . .
O10 O 0.5373(6) 0.0912(11) 0.0362(6) 0.085(4) Uani 0.50 1 d P . .
O7 O 0.0062(6) 0.2220(8) 0.1947(6) 0.116(2) Uani 0.70 1 d P . .
O6 O 0.0478(6) 0.0585(8) 0.2193(6) 0.116(2) Uani 0.70 1 d P . .
O12 O 0.5270(6) -0.0853(9) 0.0295(4) 0.073(3) Uani 0.50 1 d PD . .
O8 O 0.0650(7) 0.1293(9) 0.2918(7) 0.116(2) Uani 0.60 1 d P . .


_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 1.885(4) . ?
Co1 N1 1.923(4) . ?
Co1 N4 1.930(4) . ?
Co1 N2 1.951(5) . ?
Co1 N5 1.980(4) . ?
Co1 N3 1.996(4) . ?
Cl1 O2 1.361(7) . ?
Cl1 O4 1.426(5) . ?
Cl1 O5 1.442(5) . ?
Cl1 O3 1.482(7) . ?
O1 O1 1.439(7) 7 ?
N4 C14 1.290(7) . ?
N4 C13 1.470(6) . ?
N5 C20 1.341(7) . ?
N5 C16 1.363(6) . ?
N1 C1 1.334(7) . ?
N1 C5 1.356(7) . ?
C18 C19 1.369(8) . ?
C18 C17 1.392(7) . ?
C14 C16 1.480(7) . ?
C14 C15 1.489(7) . ?
C19 C20 1.393(8) . ?
C5 C4 1.391(8) . ?
C5 C6 1.466(8) . ?
C16 C17 1.376(7) . ?
C7 C6 1.492(7) . ?
C6 N2 1.280(7) . ?
N2 C8 1.496(8) . ?
C8 C9A 1.53(2) . ?
C8 C9B 1.587(14) . ?
C1 C2 1.388(8) . ?
C2 C3 1.372(9) . ?
C13 C12 1.542(8) . ?
C12 C11 1.514(10) . ?
C3 C4 1.385(10) . ?
N3 C10 1.470(9) . ?
N3 C11 1.506(8) . ?
C10 C9A 1.418(19) . ?
C10 C9B 1.430(15) . ?
Cl3 O12 1.277(10) 5_655 ?
Cl3 O12 1.277(10) . ?
Cl3 O10 1.449(11) 5_655 ?
Cl3 O10 1.449(11) . ?
Cl3 O11 1.471(10) 5_655 ?
Cl3 O11 1.471(10) . ?
Cl3 O9 1.500(8) . ?
Cl3 O9 1.500(8) 5_655 ?
Cl2 O8 1.300(13) . ?
Cl2 O7 1.342(10) . ?
Cl2 O6 1.381(12) . ?
Cl2 O8 1.439(14) 2 ?
Cl2 O7 1.933(11) 2 ?
Cl2 O6 2.038(13) 2 ?
O7 Cl2 1.933(11) 2 ?
O6 Cl2 2.038(13) 2 ?
O8 Cl2 1.439(14) 2 ?

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 N1 94.29(17) . . ?
O1 Co1 N4 95.65(18) . . ?
N1 Co1 N4 96.20(18) . . ?
O1 Co1 N2 88.59(19) . . ?
N1 Co1 N2 81.53(19) . . ?
N4 Co1 N2 175.35(19) . . ?
O1 Co1 N5 176.48(18) . . ?
N1 Co1 N5 86.04(18) . . ?
N4 Co1 N5 80.83(17) . . ?
N2 Co1 N5 94.93(18) . . ?
O1 Co1 N3 86.67(18) . . ?
N1 Co1 N3 178.8(2) . . ?
N4 Co1 N3 82.92(19) . . ?
N2 Co1 N3 99.3(2) . . ?
N5 Co1 N3 92.96(19) . . ?
O2 Cl1 O4 117.5(5) . . ?
O2 Cl1 O5 110.2(4) . . ?
O4 Cl1 O5 106.8(3) . . ?
O2 Cl1 O3 110.7(5) . . ?
O4 Cl1 O3 107.4(4) . . ?
O5 Cl1 O3 103.2(4) . . ?
O1 O1 Co1 113.0(4) 7 . ?
C14 N4 C13 122.0(4) . . ?
C14 N4 Co1 118.3(3) . . ?
C13 N4 Co1 117.9(4) . . ?
C20 N5 C16 118.3(4) . . ?
C20 N5 Co1 127.7(4) . . ?
C16 N5 Co1 113.4(3) . . ?
C1 N1 C5 119.1(5) . . ?
C1 N1 Co1 126.4(4) . . ?
C5 N1 Co1 114.5(4) . . ?
C19 C18 C17 119.1(5) . . ?
N4 C14 C16 113.4(4) . . ?
N4 C14 C15 127.2(5) . . ?
C16 C14 C15 119.3(5) . . ?
C18 C19 C20 119.2(5) . . ?
N1 C5 C4 121.0(5) . . ?
N1 C5 C6 113.3(5) . . ?
C4 C5 C6 125.6(5) . . ?
N5 C16 C17 121.9(5) . . ?
N5 C16 C14 113.0(4) . . ?
C17 C16 C14 125.0(5) . . ?
N2 C6 C5 114.2(5) . . ?
N2 C6 C7 124.0(5) . . ?
C5 C6 C7 121.8(5) . . ?
C6 N2 C8 119.1(5) . . ?
C6 N2 Co1 116.3(4) . . ?
C8 N2 Co1 124.5(4) . . ?
N2 C8 C9A 106.0(8) . . ?
N2 C8 C9B 112.6(6) . . ?
C9A C8 C9B 53.6(8) . . ?
N1 C1 C2 121.8(5) . . ?
C3 C2 C1 120.0(6) . . ?
N4 C13 C12 105.7(4) . . ?
N5 C20 C19 122.2(5) . . ?
C11 C12 C13 114.7(5) . . ?
C2 C3 C4 118.4(6) . . ?
C10 N3 C11 110.5(5) . . ?
C10 N3 Co1 115.5(4) . . ?
C11 N3 Co1 114.0(3) . . ?
C16 C17 C18 119.2(5) . . ?
C3 C4 C5 119.7(5) . . ?
C9A C10 C9B 59.1(10) . . ?
C9A C10 N3 121.4(8) . . ?
C9B C10 N3 117.9(8) . . ?
N3 C11 C12 114.0(5) . . ?
C10 C9B C8 111.4(8) . . ?
C10 C9A C8 115.6(12) . . ?
O12 Cl3 O12 180.0(14) 5_655 . ?
O12 Cl3 O10 112.0(7) 5_655 5_655 ?
O12 Cl3 O10 68.0(7) . 5_655 ?
O12 Cl3 O10 68.0(7) 5_655 . ?
O12 Cl3 O10 112.0(7) . . ?
O10 Cl3 O10 180.0(13) 5_655 . ?
O12 Cl3 O11 59.5(7) 5_655 5_655 ?
O12 Cl3 O11 120.5(7) . 5_655 ?
O10 Cl3 O11 73.7(6) 5_655 5_655 ?
O10 Cl3 O11 106.3(6) . 5_655 ?
O12 Cl3 O11 120.5(7) 5_655 . ?
O12 Cl3 O11 59.5(7) . . ?
O10 Cl3 O11 106.3(6) 5_655 . ?
O10 Cl3 O11 73.7(6) . . ?
O11 Cl3 O11 180.0(11) 5_655 . ?
O12 Cl3 O9 112.0(5) 5_655 . ?
O12 Cl3 O9 68.0(5) . . ?
O10 Cl3 O9 103.0(6) 5_655 . ?
O10 Cl3 O9 77.0(6) . . ?
O11 Cl3 O9 78.7(6) 5_655 . ?
O11 Cl3 O9 101.3(6) . . ?
O12 Cl3 O9 68.0(5) 5_655 5_655 ?
O12 Cl3 O9 112.0(5) . 5_655 ?
O10 Cl3 O9 77.0(6) 5_655 5_655 ?
O10 Cl3 O9 103.0(6) . 5_655 ?
O11 Cl3 O9 101.3(6) 5_655 5_655 ?
O11 Cl3 O9 78.7(6) . 5_655 ?
O9 Cl3 O9 180.0(6) . 5_655 ?
O8 Cl2 O7 121.3(8) . . ?
O8 Cl2 O6 78.9(8) . . ?
O7 Cl2 O6 110.6(7) . . ?
O8 Cl2 O8 141.7(6) . 2 ?
O7 Cl2 O8 88.9(8) . 2 ?
O6 Cl2 O8 114.2(7) . 2 ?
O8 Cl2 O7 71.1(7) . 2 ?
O7 Cl2 O7 94.2(9) . 2 ?
O6 Cl2 O7 148.2(6) . 2 ?
O8 Cl2 O7 84.8(6) 2 2 ?
O8 Cl2 O6 87.5(7) . 2 ?
O7 Cl2 O6 140.5(6) . 2 ?
O6 Cl2 O6 100.4(8) . 2 ?
O8 Cl2 O6 55.6(7) 2 2 ?
O7 Cl2 O6 68.6(4) 2 2 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Co1 O1 O1 1.3(5) . . . 7 ?
N4 Co1 O1 O1 -95.4(5) . . . 7 ?
N2 Co1 O1 O1 82.7(5) . . . 7 ?
N5 Co1 O1 O1 -94(3) . . . 7 ?
N3 Co1 O1 O1 -177.9(5) . . . 7 ?
O1 Co1 N4 C14 178.2(4) . . . . ?
N1 Co1 N4 C14 83.2(4) . . . . ?
N2 Co1 N4 C14 23(2) . . . . ?
N5 Co1 N4 C14 -1.7(4) . . . . ?
N3 Co1 N4 C14 -95.9(4) . . . . ?
O1 Co1 N4 C13 -17.0(4) . . . . ?
N1 Co1 N4 C13 -111.9(4) . . . . ?
N2 Co1 N4 C13 -173(2) . . . . ?
N5 Co1 N4 C13 163.1(4) . . . . ?
N3 Co1 N4 C13 68.9(4) . . . . ?
O1 Co1 N5 C20 177(54) . . . . ?
N1 Co1 N5 C20 81.6(5) . . . . ?
N4 Co1 N5 C20 178.6(5) . . . . ?
N2 Co1 N5 C20 0.5(5) . . . . ?
N3 Co1 N5 C20 -99.1(5) . . . . ?
O1 Co1 N5 C16 6(3) . . . . ?
N1 Co1 N5 C16 -89.6(4) . . . . ?
N4 Co1 N5 C16 7.3(3) . . . . ?
N2 Co1 N5 C16 -170.7(3) . . . . ?
N3 Co1 N5 C16 89.7(4) . . . . ?
O1 Co1 N1 C1 -89.4(5) . . . . ?
N4 Co1 N1 C1 6.8(5) . . . . ?
N2 Co1 N1 C1 -177.3(5) . . . . ?
N5 Co1 N1 C1 87.1(5) . . . . ?
N3 Co1 N1 C1 51(9) . . . . ?
O1 Co1 N1 C5 91.7(4) . . . . ?
N4 Co1 N1 C5 -172.1(4) . . . . ?
N2 Co1 N1 C5 3.8(4) . . . . ?
N5 Co1 N1 C5 -91.8(4) . . . . ?
N3 Co1 N1 C5 -128(9) . . . . ?
C13 N4 C14 C16 -168.0(4) . . . . ?
Co1 N4 C14 C16 -3.8(5) . . . . ?
C13 N4 C14 C15 8.8(8) . . . . ?
Co1 N4 C14 C15 173.0(4) . . . . ?
C17 C18 C19 C20 1.0(8) . . . . ?
C1 N1 C5 C4 -3.0(8) . . . . ?
Co1 N1 C5 C4 176.1(4) . . . . ?
C1 N1 C5 C6 176.2(5) . . . . ?
Co1 N1 C5 C6 -4.8(5) . . . . ?
C20 N5 C16 C17 0.0(7) . . . . ?
Co1 N5 C16 C17 172.1(4) . . . . ?
C20 N5 C16 C14 176.7(4) . . . . ?
Co1 N5 C16 C14 -11.1(5) . . . . ?
N4 C14 C16 N5 9.9(6) . . . . ?
C15 C14 C16 N5 -167.2(5) . . . . ?
N4 C14 C16 C17 -173.5(5) . . . . ?
C15 C14 C16 C17 9.4(7) . . . . ?
N1 C5 C6 N2 3.1(7) . . . . ?
C4 C5 C6 N2 -177.7(5) . . . . ?
N1 C5 C6 C7 -174.0(5) . . . . ?
C4 C5 C6 C7 5.1(8) . . . . ?
C5 C6 N2 C8 -177.0(5) . . . . ?
C7 C6 N2 C8 0.1(8) . . . . ?
C5 C6 N2 Co1 0.0(6) . . . . ?
C7 C6 N2 Co1 177.1(4) . . . . ?
O1 Co1 N2 C6 -96.6(4) . . . . ?
N1 Co1 N2 C6 -2.0(4) . . . . ?
N4 Co1 N2 C6 59(2) . . . . ?
N5 Co1 N2 C6 83.2(4) . . . . ?
N3 Co1 N2 C6 177.0(4) . . . . ?
O1 Co1 N2 C8 80.2(5) . . . . ?
N1 Co1 N2 C8 174.8(5) . . . . ?
N4 Co1 N2 C8 -124(2) . . . . ?
N5 Co1 N2 C8 -100.0(5) . . . . ?
N3 Co1 N2 C8 -6.2(5) . . . . ?
C6 N2 C8 C9A -145.2(8) . . . . ?
Co1 N2 C8 C9A 38.1(10) . . . . ?
C6 N2 C8 C9B 158.1(6) . . . . ?
Co1 N2 C8 C9B -18.6(9) . . . . ?
C5 N1 C1 C2 2.2(8) . . . . ?
Co1 N1 C1 C2 -176.7(4) . . . . ?
N1 C1 C2 C3 -0.6(9) . . . . ?
C14 N4 C13 C12 89.4(6) . . . . ?
Co1 N4 C13 C12 -74.8(5) . . . . ?
C16 N5 C20 C19 1.6(8) . . . . ?
Co1 N5 C20 C19 -169.3(4) . . . . ?
C18 C19 C20 N5 -2.1(9) . . . . ?
N4 C13 C12 C11 57.2(6) . . . . ?
C1 C2 C3 C4 -0.3(9) . . . . ?
O1 Co1 N3 C10 -91.7(5) . . . . ?
N1 Co1 N3 C10 128(9) . . . . ?
N4 Co1 N3 C10 172.1(5) . . . . ?
N2 Co1 N3 C10 -3.7(6) . . . . ?
N5 Co1 N3 C10 91.8(5) . . . . ?
O1 Co1 N3 C11 37.9(4) . . . . ?
N1 Co1 N3 C11 -103(9) . . . . ?
N4 Co1 N3 C11 -58.2(4) . . . . ?
N2 Co1 N3 C11 125.9(4) . . . . ?
N5 Co1 N3 C11 -138.6(4) . . . . ?
N5 C16 C17 C18 -1.0(8) . . . . ?
C14 C16 C17 C18 -177.4(5) . . . . ?
C19 C18 C17 C16 0.5(8) . . . . ?
C2 C3 C4 C5 -0.4(9) . . . . ?
N1 C5 C4 C3 2.1(8) . . . . ?
C6 C5 C4 C3 -177.0(5) . . . . ?
C11 N3 C10 C9A -155.8(12) . . . . ?
Co1 N3 C10 C9A -24.5(14) . . . . ?
C11 N3 C10 C9B -86.7(9) . . . . ?
Co1 N3 C10 C9B 44.5(10) . . . . ?
C10 N3 C11 C12 -164.6(6) . . . . ?
Co1 N3 C11 C12 63.3(6) . . . . ?
C13 C12 C11 N3 -56.2(6) . . . . ?
C9A C10 C9B C8 34.4(9) . . . . ?
N3 C10 C9B C8 -77.4(11) . . . . ?
N2 C8 C9B C10 59.7(10) . . . . ?
C9A C8 C9B C10 -33.9(10) . . . . ?
C9B C10 C9A C8 -37.2(11) . . . . ?
N3 C10 C9A C8 68.7(18) . . . . ?
N2 C8 C9A C10 -71.1(14) . . . . ?
C9B C8 C9A C10 35.5(10) . . . . ?
O12 Cl3 O9 O12 180.0 5_655 . . . ?
O10 Cl3 O9 O12 59.5(8) 5_655 . . . ?
O10 Cl3 O9 O12 -120.5(8) . . . . ?
O11 Cl3 O9 O12 129.6(7) 5_655 . . . ?
O11 Cl3 O9 O12 -50.4(7) . . . . ?
O9 Cl3 O9 O12 -83.3(6) 5_655 . . . ?
O12 Cl3 O11 O12 180.0 5_655 . . . ?
O10 Cl3 O11 O12 -51.3(8) 5_655 . . . ?
O10 Cl3 O11 O12 128.7(8) . . . . ?
O11 Cl3 O11 O12 138(100) 5_655 . . . ?
O9 Cl3 O11 O12 56.0(7) . . . . ?
O9 Cl3 O11 O12 -124.0(7) 5_655 . . . ?
O12 Cl3 O11 O10 51.3(8) 5_655 . . . ?
O12 Cl3 O11 O10 -128.7(8) . . . . ?
O10 Cl3 O11 O10 180.0 5_655 . . . ?
O11 Cl3 O11 O10 9(100) 5_655 . . . ?
O9 Cl3 O11 O10 -72.7(7) . . . . ?
O9 Cl3 O11 O10 107.3(7) 5_655 . . . ?
O12 Cl3 O10 O12 180.0 . . . 5_655 ?
O10 Cl3 O10 O12 46(100) 5_655 . . 5_655 ?
O11 Cl3 O10 O12 -46.6(7) 5_655 . . 5_655 ?
O11 Cl3 O10 O12 133.4(7) . . . 5_655 ?
O9 Cl3 O10 O12 -120.5(6) . . . 5_655 ?
O9 Cl3 O10 O12 59.5(6) 5_655 . . 5_655 ?
O12 Cl3 O10 O11 -133.4(7) 5_655 . . . ?
O12 Cl3 O10 O11 46.6(7) . . . . ?
O10 Cl3 O10 O11 -87(100) 5_655 . . . ?
O11 Cl3 O10 O11 180.0 5_655 . . . ?
O9 Cl3 O10 O11 106.1(6) . . . . ?
O9 Cl3 O10 O11 -73.9(6) 5_655 . . . ?
O12 O11 O10 Cl3 -38.7(6) . . . . ?
O12 O11 O10 O12 -72.9(9) . . . 5_655 ?
Cl3 O11 O10 O12 -34.2(6) . . . 5_655 ?
O8 Cl2 O7 Cl2 -97.7(11) . . . 2 ?
O6 Cl2 O7 Cl2 173.0(11) . . . 2 ?
O8 Cl2 O7 Cl2 57.4(8) 2 . . 2 ?
O7 Cl2 O7 Cl2 -27.3(8) 2 . . 2 ?
O6 Cl2 O7 Cl2 33.5(8) 2 . . 2 ?
Cl2 Cl2 O6 O8 -68.2(11) 2 . . . ?
O7 Cl2 O6 O8 119.5(9) . . . . ?
O8 Cl2 O6 O8 -142.1(9) 2 . . . ?
O7 Cl2 O6 O8 -19.5(12) 2 . . . ?
O6 Cl2 O6 O8 -85.3(7) 2 . . . ?
O8 Cl2 O6 Cl2 68.2(11) . . . 2 ?
O7 Cl2 O6 Cl2 -172.3(13) . . . 2 ?
O8 Cl2 O6 Cl2 -73.8(10) 2 . . 2 ?
O7 Cl2 O6 Cl2 48.8(10) 2 . . 2 ?
O6 Cl2 O6 Cl2 -17.1(9) 2 . . 2 ?
O12 Cl3 O12 O11 -27(100) 5_655 . . . ?
O10 Cl3 O12 O11 126.1(7) 5_655 . . . ?
O10 Cl3 O12 O11 -53.9(7) . . . . ?
O11 Cl3 O12 O11 180.0 5_655 . . . ?
O9 Cl3 O12 O11 -118.8(7) . . . . ?
O9 Cl3 O12 O11 61.2(7) 5_655 . . . ?
O12 Cl3 O12 O10 -153(100) 5_655 . . 5_655 ?
O10 Cl3 O12 O10 180.0 . . . 5_655 ?
O11 Cl3 O12 O10 53.9(7) 5_655 . . 5_655 ?
O11 Cl3 O12 O10 -126.1(7) . . . 5_655 ?
O9 Cl3 O12 O10 115.2(7) . . . 5_655 ?
O9 Cl3 O12 O10 -64.8(7) 5_655 . . 5_655 ?
O12 Cl3 O12 O9 92(100) 5_655 . . . ?
O10 Cl3 O12 O9 -115.2(7) 5_655 . . . ?
O10 Cl3 O12 O9 64.8(7) . . . . ?
O11 Cl3 O12 O9 -61.2(7) 5_655 . . . ?
O11 Cl3 O12 O9 118.8(7) . . . . ?
O9 Cl3 O12 O9 180.0 5_655 . . . ?
O10 O11 O12 Cl3 38.4(5) . . . . ?
Cl3 O11 O12 O10 47.8(6) . . . 5_655 ?
O10 O11 O12 O10 86.2(8) . . . 5_655 ?
Cl3 O11 O12 O9 -53.0(5) . . . . ?
O10 O11 O12 O9 -14.7(8) . . . . ?
Cl3 O9 O12 O11 55.9(7) . . . . ?
Cl3 O9 O12 O10 -53.0(6) . . . 5_655 ?
O7 Cl2 O8 Cl2 119.9(7) . . . 2 ?
O6 Cl2 O8 Cl2 -132.5(5) . . . 2 ?
O8 Cl2 O8 Cl2 -17.3(15) 2 . . 2 ?
O7 Cl2 O8 Cl2 36.8(4) 2 . . 2 ?
O6 Cl2 O8 Cl2 -31.4(3) 2 . . 2 ?
Cl2 Cl2 O8 O6 132.5(5) 2 . . . ?
O7 Cl2 O8 O6 -107.5(9) . . . . ?
O8 Cl2 O8 O6 115.3(14) 2 . . . ?
O7 Cl2 O8 O6 169.3(7) 2 . . . ?
O6 Cl2 O8 O6 101.1(8) 2 . . . ?
Cl2 O6 O8 Cl2 -26.4(4) 2 . . . ?
Cl2 O6 O8 Cl2 26.4(4) . . . 2 ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.734
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.120
_database_code_depnum_ccdc_archive 'CCDC 959181'

data_complex-3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H30 Cl2 Co N6 O9'
_chemical_formula_weight         640.34

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           Monoclinic
_symmetry_space_group_name_H-M   P21

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

_cell_length_a                   9.324(4)
_cell_length_b                   7.978(2)
_cell_length_c                   18.741(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.935(2)
_cell_angle_gamma                90.00
_cell_volume                     1390.8(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    17532
_cell_measurement_theta_min      1.0
_cell_measurement_theta_max      30.03

_exptl_crystal_description       ?
_exptl_crystal_colour            dark-red
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             662
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8122
_exptl_absorpt_correction_T_max  0.9030
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device_type  'CCD AREA DETECTOR'
_diffrn_detector_area_resol_mean 9
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_measurement_method       CCD
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_reflns_number            8951
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_sigmaI/netI    0.0680
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.98
_diffrn_reflns_theta_max         29.95
_reflns_number_total             6274
_reflns_number_gt                5430
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER APEX-II'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'
_computing_cell_refinement       'BRUKER APEX-II'
_computing_data_reduction        'BRUKER APEX-II'

_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/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     SHELXL
_refine_ls_extinction_coef       0.181(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.31(3)
_refine_ls_number_reflns         6274
_refine_ls_number_parameters     340
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1170
_refine_ls_R_factor_gt           0.1080
_refine_ls_wR_factor_ref         0.2755
_refine_ls_wR_factor_gt          0.2657
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_restrained_S_all      1.135
_refine_ls_shift/su_max          0.007
_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 0.20332(9) 0.96593(10) 0.74978(4) 0.0346(3) Uani 1 1 d . . .
Cl1 Cl 0.7143(2) 1.1755(3) 0.82772(11) 0.0562(5) Uani 1 1 d . . .
Cl2 Cl -0.2223(3) 0.5890(3) 0.54904(12) 0.0603(5) Uani 1 1 d . . .
N4 N 0.3023(7) 1.0861(8) 0.8453(3) 0.0415(11) Uani 1 1 d . . .
H4N H 0.3950 1.1185 0.8360 0.050 Uiso 1 1 calc R . .
N5 N 0.1084(7) 0.8339(7) 0.8369(3) 0.0420(12) Uani 1 1 d . . .
N1 N 0.2802(6) 0.7343(8) 0.6975(3) 0.0376(10) Uani 1 1 d . . .
C11 C 0.2212(9) 1.2356(9) 0.8616(4) 0.0461(14) Uani 1 1 d . . .
H11A H 0.2828 1.3139 0.8909 0.055 Uiso 1 1 calc R . .
H11B H 0.1379 1.2049 0.8889 0.055 Uiso 1 1 calc R . .
O8 O -0.0717(19) 0.546(3) 0.5531(11) 0.162(4) Uani 1 1 d . . .
O4 O 0.6142(16) 1.289(2) 0.8536(8) 0.137(6) Uani 1 1 d . . .
N3 N 0.0808(7) 1.1957(8) 0.7508(4) 0.0453(13) Uani 1 1 d . . .
H3N H -0.0023 1.1765 0.7743 0.054 Uiso 1 1 calc R . .
C6 C 0.2223(8) 0.7166(9) 0.6303(3) 0.0402(13) Uani 1 1 d . . .
C5 C 0.2645(10) 0.5988(12) 0.5833(5) 0.0548(18) Uani 1 1 d . . .
H5 H 0.2154 0.5866 0.5374 0.066 Uiso 1 1 calc R . .
N6 N 0.3774(7) 1.0669(8) 0.6919(3) 0.0428(12) Uani 1 1 d . . .
C1 C 0.3893(9) 0.6334(8) 0.7172(4) 0.0458(15) Uani 1 1 d . . .
C2 C 0.4622(10) 0.6602(12) 0.7904(5) 0.057(2) Uani 1 1 d . . .
H2A H 0.3906 0.6557 0.8263 0.086 Uiso 1 1 calc R . .
H2B H 0.5095 0.7699 0.7923 0.086 Uiso 1 1 calc R . .
H2C H 0.5342 0.5722 0.8004 0.086 Uiso 1 1 calc R . .
N2 N 0.0802(6) 0.9480(10) 0.6519(3) 0.0451(13) Uani 1 1 d . . .
C3 C 0.4432(10) 0.5167(10) 0.6713(5) 0.0526(18) Uani 1 1 d . . .
H3 H 0.5240 0.4504 0.6868 0.063 Uiso 1 1 calc R . .
C12 C 0.3123(8) 0.9622(12) 0.9065(3) 0.0479(13) Uani 1 1 d . . .
H12 H 0.3980 0.8888 0.9016 0.057 Uiso 1 1 calc R . .
C14 C 0.1350(14) 0.7773(12) 0.9632(4) 0.063(2) Uani 1 1 d . . .
H14 H 0.1863 0.7961 1.0081 0.076 Uiso 1 1 calc R . .
O9 O -0.261(2) 0.687(3) 0.6028(13) 0.162(4) Uani 1 1 d . . .
C7 C 0.1091(9) 0.8419(11) 0.6087(4) 0.0479(15) Uani 1 1 d . . .
H7 H 0.0609 0.8389 0.5624 0.058 Uiso 1 1 calc R . .
C10 C 0.1697(11) 1.3184(10) 0.7915(5) 0.0547(18) Uani 1 1 d . . .
H10A H 0.1128 1.4200 0.8007 0.066 Uiso 1 1 calc R . .
H10B H 0.2528 1.3515 0.7644 0.066 Uiso 1 1 calc R . .
C13 C 0.1788(9) 0.8546(9) 0.9011(4) 0.0448(15) Uani 1 1 d . . .
C9 C 0.0399(11) 1.2413(12) 0.6762(5) 0.059(2) Uani 1 1 d . . .
H9A H 0.1249 1.2858 0.6535 0.071 Uiso 1 1 calc R . .
H9B H -0.0341 1.3304 0.6750 0.071 Uiso 1 1 calc R . .
C8 C -0.0173(8) 1.0931(14) 0.6353(4) 0.059(2) Uani 1 1 d . . .
H8A H -0.0221 1.1173 0.5834 0.071 Uiso 1 1 calc R . .
H8B H -0.1155 1.0666 0.6490 0.071 Uiso 1 1 calc R . .
O6 O -0.301(2) 0.449(3) 0.5322(10) 0.162(4) Uani 1 1 d . . .
O7 O -0.244(2) 0.694(3) 0.4934(13) 0.162(4) Uani 1 1 d . . .
O3 O 0.6463(16) 1.0245(19) 0.8344(10) 0.127(5) Uani 1 1 d . . .
C16 C -0.0535(13) 0.6532(13) 0.8917(6) 0.071(3) Uani 1 1 d . . .
H16 H -0.1356 0.5823 0.8883 0.085 Uiso 1 1 calc R . .
C17 C -0.0071(10) 0.7318(11) 0.8320(4) 0.0526(18) Uani 1 1 d . . .
C18 C -0.0868(11) 0.7150(13) 0.7598(6) 0.064(2) Uani 1 1 d . . .
H18A H -0.0177 0.7060 0.7229 0.096 Uiso 1 1 calc R . .
H18B H -0.1476 0.8138 0.7505 0.096 Uiso 1 1 calc R . .
H18C H -0.1470 0.6142 0.7591 0.096 Uiso 1 1 calc R . .
C4 C 0.3812(10) 0.4967(9) 0.6041(5) 0.0543(19) Uani 1 1 d . . .
H4 H 0.4162 0.4158 0.5724 0.065 Uiso 1 1 calc R . .
C15 C 0.0242(14) 0.6806(15) 0.9585(5) 0.074(3) Uani 1 1 d . . .
H15 H -0.0058 0.6269 1.0002 0.089 Uiso 1 1 calc R . .
C20 C 0.4643(7) 1.0755(10) 0.6525(4) 0.0435(14) Uani 1 1 d . . .
C21 C 0.5753(9) 1.0850(16) 0.6031(5) 0.060(2) Uani 1 1 d . . .
H21A H 0.6462 0.9964 0.6140 0.090 Uiso 1 1 calc R . .
H21B H 0.6224 1.1946 0.6074 0.090 Uiso 1 1 calc R . .
H21C H 0.5328 1.0704 0.5542 0.090 Uiso 1 1 calc R . .
O5 O 0.8462(8) 1.183(2) 0.8666(5) 0.121(6) Uani 1 1 d . . .
O2 O 0.7418(15) 1.208(4) 0.7557(5) 0.168(11) Uani 1 1 d . . .
O1 O 0.3240(11) 1.0379(11) 0.9747(4) 0.075(2) Uani 1 1 d . . .
C19 C 0.472(2) 1.088(3) 0.9957(9) 0.126(8) Uani 1 1 d . . .
H19A H 0.5368 1.0401 0.9620 0.190 Uiso 1 1 calc R . .
H19C H 0.4989 1.0460 1.0440 0.190 Uiso 1 1 calc R . .
H19B H 0.4794 1.2102 0.9952 0.190 Uiso 1 1 calc 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 N2 2.101(6) . ?
Co1 N3 2.161(6) . ?
Co1 N6 2.168(7) . ?
Co1 N4 2.179(6) . ?
Co1 N5 2.182(6) . ?
Co1 N1 2.233(6) . ?
Cl1 O3 1.371(15) . ?
Cl1 O5 1.388(8) . ?
Cl1 O4 1.408(10) . ?
Cl1 O2 1.415(11) . ?
Cl2 O7 1.34(3) . ?
Cl2 O9 1.35(2) . ?
Cl2 O6 1.37(2) . ?
Cl2 O8 1.442(19) . ?
N4 C11 1.456(9) . ?
N4 C12 1.511(9) . ?
N5 C13 1.341(10) . ?
N5 C17 1.348(12) . ?
N1 C1 1.329(10) . ?
N1 C6 1.343(8) . ?
C11 C10 1.518(12) . ?
N3 C10 1.463(12) . ?
N3 C9 1.469(11) . ?
C6 C5 1.364(10) . ?
C6 C7 1.490(11) . ?
C5 C4 1.394(13) . ?
N6 C20 1.136(10) . ?
C1 C3 1.386(11) . ?
C1 C2 1.504(12) . ?
N2 C7 1.214(11) . ?
N2 C8 1.491(11) . ?
C3 C4 1.357(13) . ?
C12 O1 1.411(9) . ?
C12 C13 1.509(12) . ?
C14 C15 1.288(16) . ?
C14 C13 1.402(9) . ?
C9 C8 1.488(15) . ?
C16 C17 1.378(11) . ?
C16 C15 1.419(16) . ?
C17 C18 1.505(15) . ?
C20 C21 1.437(11) . ?
O1 C19 1.464(19) . ?

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
N2 Co1 N3 78.9(3) . . ?
N2 Co1 N6 88.4(2) . . ?
N3 Co1 N6 95.9(2) . . ?
N2 Co1 N4 157.3(3) . . ?
N3 Co1 N4 79.3(3) . . ?
N6 Co1 N4 87.6(2) . . ?
N2 Co1 N5 113.3(3) . . ?
N3 Co1 N5 99.3(2) . . ?
N6 Co1 N5 155.5(2) . . ?
N4 Co1 N5 76.6(3) . . ?
N2 Co1 N1 74.5(2) . . ?
N3 Co1 N1 153.1(2) . . ?
N6 Co1 N1 79.3(2) . . ?
N4 Co1 N1 126.4(2) . . ?
N5 Co1 N1 95.1(2) . . ?
O3 Cl1 O5 113.0(11) . . ?
O3 Cl1 O4 102.1(10) . . ?
O5 Cl1 O4 112.0(10) . . ?
O3 Cl1 O2 111.3(14) . . ?
O5 Cl1 O2 106.3(7) . . ?
O4 Cl1 O2 112.3(12) . . ?
O7 Cl2 O9 100.7(15) . . ?
O7 Cl2 O6 106.4(13) . . ?
O9 Cl2 O6 118.7(11) . . ?
O7 Cl2 O8 106.3(12) . . ?
O9 Cl2 O8 114.3(12) . . ?
O6 Cl2 O8 109.1(13) . . ?
C11 N4 C12 112.5(6) . . ?
C11 N4 Co1 109.6(5) . . ?
C12 N4 Co1 109.6(4) . . ?
C13 N5 C17 118.4(6) . . ?
C13 N5 Co1 114.4(5) . . ?
C17 N5 Co1 127.2(5) . . ?
C1 N1 C6 116.6(6) . . ?
C1 N1 Co1 129.9(5) . . ?
C6 N1 Co1 112.2(5) . . ?
N4 C11 C10 108.3(6) . . ?
C10 N3 C9 115.5(7) . . ?
C10 N3 Co1 106.9(5) . . ?
C9 N3 Co1 107.7(5) . . ?
N1 C6 C5 124.2(7) . . ?
N1 C6 C7 114.6(6) . . ?
C5 C6 C7 121.1(7) . . ?
C6 C5 C4 118.4(8) . . ?
C20 N6 Co1 160.0(6) . . ?
N1 C1 C3 122.5(8) . . ?
N1 C1 C2 117.2(6) . . ?
C3 C1 C2 120.1(8) . . ?
C7 N2 C8 124.2(7) . . ?
C7 N2 Co1 119.8(6) . . ?
C8 N2 Co1 114.7(5) . . ?
C4 C3 C1 120.4(8) . . ?
O1 C12 C13 108.4(7) . . ?
O1 C12 N4 113.8(8) . . ?
C13 C12 N4 108.3(5) . . ?
C15 C14 C13 119.0(9) . . ?
N2 C7 C6 118.2(6) . . ?
N3 C10 C11 107.1(6) . . ?
N5 C13 C14 122.5(8) . . ?
N5 C13 C12 118.7(6) . . ?
C14 C13 C12 118.7(8) . . ?
N3 C9 C8 110.7(7) . . ?
C9 C8 N2 108.5(6) . . ?
C17 C16 C15 118.4(9) . . ?
N5 C17 C16 120.9(9) . . ?
N5 C17 C18 117.2(7) . . ?
C16 C17 C18 121.8(9) . . ?
C3 C4 C5 117.8(7) . . ?
C14 C15 C16 120.8(8) . . ?
N6 C20 C21 179.3(9) . . ?
C12 O1 C19 111.9(12) . . ?

_diffrn_measured_fraction_theta_max 0.954
_diffrn_reflns_theta_full        29.95
_diffrn_measured_fraction_theta_full 0.954
_refine_diff_density_max         1.709
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.160
_database_code_depnum_ccdc_archive 'CCDC 959182'

data_complex-4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H29 Cl2 Co N5 O9'
_chemical_formula_weight         613.31

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           Monoclinic
_symmetry_space_group_name_H-M   P21/a

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

_cell_length_a                   18.261(1)
_cell_length_b                   8.2488(5)
_cell_length_c                   19.086(1)
_cell_angle_alpha                90.00
_cell_angle_beta                 117.836(3)
_cell_angle_gamma                90.00
_cell_volume                     2542.3(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    38502
_cell_measurement_theta_min      1.0
_cell_measurement_theta_max      27.48

_exptl_crystal_description       ?
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1268
_exptl_absorpt_coefficient_mu    0.945
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8335
_exptl_absorpt_correction_T_max  0.9543
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device_type  'CCD AREA DETECTOR'
_diffrn_detector_area_resol_mean 9
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_measurement_method       CCD
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_reflns_number            8013
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0712
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.45
_diffrn_reflns_theta_max         27.51
_reflns_number_total             5136
_reflns_number_gt                3484
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER APEX-II'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'
_computing_cell_refinement       'BRUKER APEX-II'
_computing_data_reduction        'BRUKER APEX-II'

_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/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         5136
_refine_ls_number_parameters     311
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1399
_refine_ls_R_factor_gt           0.0995
_refine_ls_wR_factor_ref         0.2840
_refine_ls_wR_factor_gt          0.2549
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.004

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 0.99223(6) 0.44140(10) 0.25149(6) 0.0326(4) Uani 1 1 d . . .
Cl1 Cl 1.32727(13) 0.2805(2) 0.40856(13) 0.0487(5) Uani 1 1 d . . .
Cl2 Cl 1.17547(14) 0.1767(4) 0.07921(14) 0.0639(7) Uani 1 1 d . . .
O1 O 0.8897(3) 0.3169(7) 0.2570(3) 0.0479(13) Uani 1 1 d . . .
H1A H 0.8680 0.2443 0.2190 0.072 Uiso 1 1 d R . .
H1B H 0.8513 0.3874 0.2516 0.072 Uiso 1 1 d R . .
N1 N 0.9149(4) 0.6543(7) 0.2372(4) 0.0381(13) Uani 1 1 d . . .
N4 N 1.0706(4) 0.4225(8) 0.3717(4) 0.0473(16) Uani 1 1 d . . .
N2 N 0.9198(6) 0.4436(9) 0.1294(4) 0.055(2) Uani 1 1 d . . .
N5 N 1.0969(4) 0.6076(8) 0.2675(4) 0.0431(15) Uani 1 1 d . . .
C2 C 0.9635(6) 0.7309(13) 0.3745(6) 0.062(2) Uani 1 1 d . . .
H2A H 0.9520 0.8122 0.4055 0.092 Uiso 1 1 calc R . .
H2B H 1.0210 0.7417 0.3844 0.092 Uiso 1 1 calc R . .
H2C H 0.9549 0.6222 0.3901 0.092 Uiso 1 1 calc R . .
O5 O 1.3656(5) 0.1397(10) 0.3945(7) 0.092(3) Uani 1 1 d . . .
C17 C 1.2244(7) 0.8316(13) 0.3257(9) 0.079(4) Uani 1 1 d . . .
H17 H 1.2670 0.9110 0.3458 0.095 Uiso 1 1 calc R . .
C14 C 1.1388(5) 0.5074(12) 0.3992(5) 0.0507(19) Uani 1 1 d . . .
H14 H 1.1808 0.4938 0.4523 0.061 Uiso 1 1 calc R . .
C1 C 0.9079(5) 0.7555(10) 0.2905(6) 0.055(2) Uani 1 1 d . . .
C16 C 1.2120(6) 0.7323(14) 0.3751(7) 0.063(3) Uani 1 1 d . . .
H16 H 1.2477 0.7394 0.4305 0.076 Uiso 1 1 calc R . .
C8 C 0.9187(10) 0.3253(17) 0.0734(7) 0.089(4) Uani 1 1 d . . .
H8A H 0.8688 0.2570 0.0574 0.106 Uiso 1 1 calc R . .
H8B H 0.9123 0.3838 0.0256 0.106 Uiso 1 1 calc R . .
C11 C 1.0417(7) 0.0925(11) 0.3072(8) 0.0891(18) Uani 1 1 d D . .
H11A H 1.0622 -0.0136 0.2994 0.107 Uiso 1 1 calc R . .
H11B H 0.9834 0.0762 0.2958 0.107 Uiso 1 1 calc R . .
O4 O 1.3859(6) 0.4090(11) 0.4314(7) 0.106(4) Uani 1 1 d . . .
C15 C 1.1496(5) 0.6225(11) 0.3475(6) 0.052(2) Uani 1 1 d . . .
C6 C 0.8618(5) 0.6761(12) 0.1601(6) 0.063(3) Uani 1 1 d . . .
C3 C 0.8484(7) 0.8831(12) 0.2638(11) 0.091(5) Uani 1 1 d . . .
H3 H 0.8446 0.9543 0.3012 0.110 Uiso 1 1 calc R . .
N3 N 1.0407(6) 0.1995(9) 0.2482(6) 0.077(3) Uani 1 1 d D . .
H3N H 1.0943 0.2099 0.2548 0.092 Uiso 1 1 calc R . .
C20 C 1.0577(8) 0.6894(13) 0.1324(7) 0.077(3) Uani 1 1 d . . .
H20A H 1.0764 0.7668 0.1051 0.115 Uiso 1 1 calc R . .
H20B H 1.0004 0.7138 0.1200 0.115 Uiso 1 1 calc R . .
H20C H 1.0608 0.5791 0.1149 0.115 Uiso 1 1 calc R . .
O3 O 1.3102(5) 0.2693(18) 0.4712(5) 0.111(4) Uani 1 1 d . . .
C12 C 1.0916(6) 0.1349(15) 0.3961(8) 0.088(4) Uani 1 1 d D . .
H12A H 1.0851 0.0450 0.4271 0.105 Uiso 1 1 calc R . .
H12B H 1.1509 0.1405 0.4098 0.105 Uiso 1 1 calc R . .
C19 C 1.1113(6) 0.7021(10) 0.2187(7) 0.056(2) Uani 1 1 d . . .
O2 O 1.2555(4) 0.3199(10) 0.3382(4) 0.078(2) Uani 1 1 d . . .
C13 C 1.0693(6) 0.2849(14) 0.4210(6) 0.067(3) Uani 1 1 d . . .
H13A H 1.1088 0.3062 0.4773 0.080 Uiso 1 1 calc R . .
H13B H 1.0133 0.2744 0.4165 0.080 Uiso 1 1 calc R . .
C7 C 0.8658(7) 0.5548(14) 0.1047(5) 0.067(3) Uani 1 1 d . . .
H7 H 0.8273 0.5606 0.0499 0.081 Uiso 1 1 calc R . .
C5 C 0.8036(6) 0.8011(15) 0.1306(8) 0.083(4) Uani 1 1 d . . .
H5 H 0.7697 0.8161 0.0753 0.099 Uiso 1 1 calc R . .
C18 C 1.1727(6) 0.8152(12) 0.2435(7) 0.065(3) Uani 1 1 d . . .
H18 H 1.1805 0.8808 0.2066 0.078 Uiso 1 1 calc R . .
C10 C 0.9814(9) 0.1237(15) 0.1603(9) 0.104(2) Uani 1 1 d D . .
H10A H 1.0010 0.0135 0.1567 0.124 Uiso 1 1 calc R . .
H10B H 0.9240 0.1147 0.1523 0.124 Uiso 1 1 calc R . .
C9 C 0.9827(11) 0.229(2) 0.0965(10) 0.133(4) Uani 1 1 d D . .
H9A H 1.0346 0.2930 0.1177 0.159 Uiso 1 1 calc R . .
H9B H 0.9785 0.1623 0.0518 0.159 Uiso 1 1 calc R . .
C4 C 0.7976(7) 0.9031(18) 0.1861(13) 0.114(7) Uani 1 1 d . . .
H4 H 0.7574 0.9871 0.1688 0.136 Uiso 1 1 calc R . .
O7 O 1.1322(10) 0.320(2) 0.0635(10) 0.171(3) Uani 1 1 d . . .
O6 O 1.2026(10) 0.150(2) 0.1615(10) 0.171(3) Uani 1 1 d . . .
O8 O 1.2554(10) 0.246(3) 0.0874(9) 0.171(3) Uani 1 1 d . . .
O9 O 1.1451(11) 0.040(2) 0.0494(10) 0.171(3) Uani 1 1 d . . .


_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 N4 2.067(7) . ?
Co1 N2 2.074(7) . ?
Co1 O1 2.181(5) . ?
Co1 N1 2.189(6) . ?
Co1 N3 2.196(8) . ?
Co1 N5 2.255(6) . ?
Cl1 O3 1.372(8) . ?
Cl1 O2 1.409(7) . ?
Cl1 O4 1.423(8) . ?
Cl1 O5 1.445(8) . ?
Cl2 O9 1.268(17) . ?
Cl2 O7 1.377(19) . ?
Cl2 O6 1.425(17) . ?
Cl2 O8 1.506(15) . ?
N1 C6 1.344(11) . ?
N1 C1 1.368(11) . ?
N4 C14 1.307(11) . ?
N4 C13 1.481(11) . ?
N2 C7 1.266(14) . ?
N2 C8 1.440(13) . ?
N5 C19 1.330(11) . ?
N5 C15 1.379(12) . ?
C2 C1 1.456(15) . ?
C17 C16 1.346(17) . ?
C17 C18 1.409(18) . ?
C14 C15 1.446(13) . ?
C1 C3 1.425(14) . ?
C16 C15 1.354(14) . ?
C8 C9 1.31(2) . ?
C11 N3 1.425(12) . ?
C11 C12 1.545(15) . ?
C6 C5 1.396(15) . ?
C6 C7 1.483(17) . ?
C3 C4 1.34(2) . ?
N3 C10 1.637(14) . ?
C20 C19 1.475(17) . ?
C12 C13 1.450(19) . ?
C19 C18 1.362(13) . ?
C5 C4 1.40(2) . ?
C10 C9 1.505(17) . ?

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
N4 Co1 N2 174.8(3) . . ?
N4 Co1 O1 94.3(2) . . ?
N2 Co1 O1 87.0(3) . . ?
N4 Co1 N1 105.7(3) . . ?
N2 Co1 N1 79.5(3) . . ?
O1 Co1 N1 82.3(2) . . ?
N4 Co1 N3 83.4(3) . . ?
N2 Co1 N3 91.7(4) . . ?
O1 Co1 N3 86.6(3) . . ?
N1 Co1 N3 166.1(3) . . ?
N4 Co1 N5 78.0(3) . . ?
N2 Co1 N5 101.7(3) . . ?
O1 Co1 N5 166.6(2) . . ?
N1 Co1 N5 89.2(2) . . ?
N3 Co1 N5 103.2(3) . . ?
O3 Cl1 O2 111.0(5) . . ?
O3 Cl1 O4 103.2(8) . . ?
O2 Cl1 O4 110.6(6) . . ?
O3 Cl1 O5 115.8(7) . . ?
O2 Cl1 O5 108.9(6) . . ?
O4 Cl1 O5 107.1(6) . . ?
O9 Cl2 O7 125.6(11) . . ?
O9 Cl2 O6 102.3(9) . . ?
O7 Cl2 O6 103.9(10) . . ?
O9 Cl2 O8 125.6(13) . . ?
O7 Cl2 O8 97.3(11) . . ?
O6 Cl2 O8 97.0(9) . . ?
C6 N1 C1 117.5(8) . . ?
C6 N1 Co1 109.8(6) . . ?
C1 N1 Co1 132.5(6) . . ?
C14 N4 C13 116.8(7) . . ?
C14 N4 Co1 116.2(6) . . ?
C13 N4 Co1 123.7(6) . . ?
C7 N2 C8 118.4(10) . . ?
C7 N2 Co1 113.7(6) . . ?
C8 N2 Co1 127.5(9) . . ?
C19 N5 C15 117.3(8) . . ?
C19 N5 Co1 133.9(7) . . ?
C15 N5 Co1 108.2(5) . . ?
C16 C17 C18 118.5(9) . . ?
N4 C14 C15 119.1(8) . . ?
N1 C1 C3 120.4(11) . . ?
N1 C1 C2 118.3(8) . . ?
C3 C1 C2 121.3(11) . . ?
C17 C16 C15 121.4(11) . . ?
C9 C8 N2 117.4(12) . . ?
N3 C11 C12 120.7(9) . . ?
C16 C15 N5 121.0(9) . . ?
C16 C15 C14 122.1(9) . . ?
N5 C15 C14 116.8(7) . . ?
N1 C6 C5 124.4(12) . . ?
N1 C6 C7 116.1(9) . . ?
C5 C6 C7 119.5(10) . . ?
C4 C3 C1 120.2(15) . . ?
C11 N3 C10 109.3(10) . . ?
C11 N3 Co1 113.4(6) . . ?
C10 N3 Co1 107.1(7) . . ?
C13 C12 C11 116.2(8) . . ?
N5 C19 C18 123.9(11) . . ?
N5 C19 C20 119.6(8) . . ?
C18 C19 C20 116.5(9) . . ?
C12 C13 N4 110.8(9) . . ?
N2 C7 C6 120.8(8) . . ?
C6 C5 C4 117.0(11) . . ?
C19 C18 C17 117.8(10) . . ?
C9 C10 N3 110.8(10) . . ?
C8 C9 C10 105.9(15) . . ?
C3 C4 C5 120.4(11) . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         1.797
_refine_diff_density_min         -1.447
_refine_diff_density_rms         0.157
_database_code_depnum_ccdc_archive 'CCDC 959183'

data_complex-5

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H31 Cl2 Co N5 O9'
_chemical_formula_weight         627.34

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           monoclinic
_symmetry_space_group_name_H-M   P21/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                   8.3498(1)
_cell_length_b                   20.2191(3)
_cell_length_c                   15.6642(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.775(1)
_cell_angle_gamma                90.00
_cell_volume                     2606.12(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    26882
_cell_measurement_theta_min      1.0
_cell_measurement_theta_max      27.48

_exptl_crystal_description       ?
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1300
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.895
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
 ?
;

_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_detector_area_resol_mean 9
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_measurement_method       CCD
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11684
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.61
_diffrn_reflns_theta_max         27.49
_reflns_number_total             5959
_reflns_number_gt                5003
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'

_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)+(0.0332P)²+1.4821P] where P=(Fo²+2Fc²)/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         5959
_refine_ls_number_parameters     354
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0290
_refine_ls_wR_factor_ref         0.0742
_refine_ls_wR_factor_gt          0.0695
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_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 0.11296(3) 0.130847(10) 0.251984(14) 0.01538(7) Uani 1 1 d . . .
Cl1 Cl 0.36646(5) -0.139558(19) 0.36133(3) 0.02145(10) Uani 1 1 d . . .
Cl2 Cl 0.31155(5) -0.35173(2) 0.58732(3) 0.02294(10) Uani 1 1 d . . .
O1 O 0.20033(16) 0.17908(7) 0.14694(9) 0.0231(3) Uani 1 1 d . . .
N5 N -0.01264(16) 0.06064(6) 0.33008(9) 0.0167(3) Uani 1 1 d . . .
N4 N 0.16940(17) 0.03809(7) 0.20709(9) 0.0184(3) Uani 1 1 d . . .
N3 N 0.36322(17) 0.12611(7) 0.32472(9) 0.0193(3) Uani 1 1 d . . .
N2 N 0.06619(17) 0.22469(7) 0.29847(9) 0.0180(3) Uani 1 1 d . . .
O7 O 0.43605(18) -0.34317(7) 0.66106(9) 0.0401(4) Uani 1 1 d . . .
O6 O 0.24096(18) -0.28867(7) 0.56049(10) 0.0378(3) Uani 1 1 d . . .
N1 N -0.13583(16) 0.15536(7) 0.17492(9) 0.0180(3) Uani 1 1 d . . .
C3 C -0.3772(2) 0.15427(9) 0.06743(12) 0.0246(4) Uani 1 1 d . . .
H3 H -0.4418 0.1324 0.0219 0.030 Uiso 1 1 calc R . .
C5 C -0.3252(2) 0.24681(9) 0.16092(12) 0.0240(4) Uani 1 1 d . . .
H5 H -0.3539 0.2879 0.1805 0.029 Uiso 1 1 calc R . .
C7 C -0.0697(2) 0.25049(8) 0.26604(11) 0.0194(3) Uani 1 1 d . . .
H7 H -0.0977 0.2918 0.2852 0.023 Uiso 1 1 calc R . .
O3 O 0.40624(19) -0.11735(7) 0.28086(9) 0.0373(3) Uani 1 1 d . . .
O2 O 0.3274(2) -0.08416(7) 0.41036(10) 0.0408(4) Uani 1 1 d . . .
C16 C -0.0132(2) -0.00123(8) 0.29562(11) 0.0187(3) Uani 1 1 d . . .
C8 C 0.1760(2) 0.26613(8) 0.36078(11) 0.0238(4) Uani 1 1 d . . .
H8A H 0.1129 0.2879 0.3992 0.029 Uiso 1 1 calc R . .
H8B H 0.2232 0.3002 0.3292 0.029 Uiso 1 1 calc R . .
C20 C -0.09642(19) 0.06972(8) 0.39532(11) 0.0187(3) Uani 1 1 d . . .
C2 C -0.1841(2) 0.05819(9) 0.08018(13) 0.0295(4) Uani 1 1 d . . .
H2A H -0.0772 0.0609 0.0655 0.044 Uiso 1 1 calc R . .
H2B H -0.2599 0.0442 0.0303 0.044 Uiso 1 1 calc R . .
H2C H -0.1838 0.0268 0.1262 0.044 Uiso 1 1 calc R . .
C1 C -0.2330(2) 0.12472(9) 0.10900(11) 0.0213(4) Uani 1 1 d . . .
C4 C -0.4240(2) 0.21522(9) 0.09339(12) 0.0265(4) Uani 1 1 d . . .
H4 H -0.5200 0.2348 0.0661 0.032 Uiso 1 1 calc R . .
C6 C -0.1823(2) 0.21589(8) 0.19893(11) 0.0191(3) Uani 1 1 d . . .
C19 C -0.1858(2) 0.01843(9) 0.42456(12) 0.0222(4) Uani 1 1 d . . .
H19 H -0.2411 0.0257 0.4705 0.027 Uiso 1 1 calc R . .
C11 C 0.3726(2) 0.07840(9) 0.39744(12) 0.0239(4) Uani 1 1 d . . .
H11A H 0.3413 0.0353 0.3750 0.036 Uiso 1 1 calc R . .
H11B H 0.3005 0.0922 0.4357 0.036 Uiso 1 1 calc R . .
H11C H 0.4819 0.0769 0.4287 0.036 Uiso 1 1 calc R . .
C18 C -0.1924(2) -0.04293(9) 0.38555(12) 0.0248(4) Uani 1 1 d . . .
H18 H -0.2562 -0.0766 0.4026 0.030 Uiso 1 1 calc R . .
O8 O 0.3806(3) -0.37974(9) 0.51777(11) 0.0607(5) Uani 1 1 d . . .
C13 C 0.4628(2) 0.03760(9) 0.22685(13) 0.0256(4) Uani 1 1 d . . .
H13A H 0.4677 0.0052 0.2729 0.031 Uiso 1 1 calc R . .
H13B H 0.5546 0.0296 0.1977 0.031 Uiso 1 1 calc R . .
C21 C -0.0909(2) 0.13640(9) 0.43777(12) 0.0252(4) Uani 1 1 d . . .
H21A H 0.0194 0.1518 0.4496 0.038 Uiso 1 1 calc R . .
H21B H -0.1328 0.1330 0.4910 0.038 Uiso 1 1 calc R . .
H21C H -0.1559 0.1670 0.3998 0.038 Uiso 1 1 calc R . .
C15 C 0.0983(2) -0.01162(8) 0.23387(11) 0.0196(3) Uani 1 1 d . . .
H15 H 0.1168 -0.0540 0.2145 0.024 Uiso 1 1 calc R . .
C12 C 0.4814(2) 0.10624(9) 0.26755(12) 0.0236(4) Uani 1 1 d . . .
H12A H 0.5899 0.1094 0.3012 0.028 Uiso 1 1 calc R . .
H12B H 0.4743 0.1384 0.2211 0.028 Uiso 1 1 calc R . .
O5 O 0.22967(19) -0.18369(7) 0.34445(11) 0.0448(4) Uani 1 1 d . . .
C9 C 0.3113(2) 0.22705(9) 0.41455(11) 0.0234(4) Uani 1 1 d . . .
H9A H 0.2638 0.1944 0.4482 0.028 Uiso 1 1 calc R . .
H9B H 0.3764 0.2568 0.4549 0.028 Uiso 1 1 calc R . .
O4 O 0.5031(2) -0.17427(9) 0.40815(11) 0.0541(5) Uani 1 1 d . . .
O9 O 0.1892(2) -0.39469(8) 0.60934(13) 0.0555(5) Uani 1 1 d . . .
C14 C 0.3067(2) 0.02636(9) 0.16212(12) 0.0238(4) Uani 1 1 d . . .
H14A H 0.3020 0.0565 0.1136 0.029 Uiso 1 1 calc R . .
H14B H 0.3034 -0.0186 0.1402 0.029 Uiso 1 1 calc R . .
C10 C 0.4215(2) 0.19198(9) 0.36117(13) 0.0256(4) Uani 1 1 d . . .
H10A H 0.4366 0.2207 0.3135 0.031 Uiso 1 1 calc R . .
H10B H 0.5271 0.1859 0.3972 0.031 Uiso 1 1 calc R . .
C17 C -0.1018(2) -0.05322(9) 0.32052(12) 0.0241(4) Uani 1 1 d . . .
H17 H -0.1007 -0.0944 0.2941 0.029 Uiso 1 1 calc R . .
H1A H 0.204(3) 0.2204(14) 0.1444(17) 0.052(8) Uiso 1 1 d . . .
H1B H 0.172(3) 0.1666(13) 0.0999(18) 0.047(8) Uiso 1 1 d . . .


_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 N4 2.0848(14) . ?
Co1 N2 2.0926(14) . ?
Co1 O1 2.1444(13) . ?
Co1 N3 2.2057(14) . ?
Co1 N5 2.2466(14) . ?
Co1 N1 2.2731(14) . ?
Cl1 O2 1.4269(14) . ?
Cl1 O3 1.4292(14) . ?
Cl1 O4 1.4312(15) . ?
Cl1 O5 1.4382(15) . ?
Cl2 O9 1.4270(16) . ?
Cl2 O7 1.4273(14) . ?
Cl2 O8 1.4331(16) . ?
Cl2 O6 1.4372(14) . ?
N5 C20 1.345(2) . ?
N5 C16 1.362(2) . ?
N4 C15 1.274(2) . ?
N4 C14 1.463(2) . ?
N3 C11 1.485(2) . ?
N3 C12 1.495(2) . ?
N3 C10 1.498(2) . ?
N2 C7 1.273(2) . ?
N2 C8 1.480(2) . ?
N1 C1 1.351(2) . ?
N1 C6 1.356(2) . ?
C3 C4 1.375(3) . ?
C3 C1 1.401(2) . ?
C5 C4 1.382(3) . ?
C5 C6 1.389(2) . ?
C7 C6 1.464(2) . ?
C16 C17 1.380(2) . ?
C16 C15 1.467(2) . ?
C8 C9 1.512(2) . ?
C20 C19 1.400(2) . ?
C20 C21 1.500(2) . ?
C2 C1 1.498(2) . ?
C19 C18 1.380(3) . ?
C18 C17 1.384(3) . ?
C13 C12 1.524(3) . ?
C13 C14 1.526(3) . ?
C9 C10 1.520(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
N4 Co1 N2 177.73(5) . . ?
N4 Co1 O1 91.40(5) . . ?
N2 Co1 O1 87.85(5) . . ?
N4 Co1 N3 83.49(5) . . ?
N2 Co1 N3 94.36(5) . . ?
O1 Co1 N3 90.01(5) . . ?
N4 Co1 N5 76.61(5) . . ?
N2 Co1 N5 104.56(5) . . ?
O1 Co1 N5 163.00(5) . . ?
N3 Co1 N5 100.38(5) . . ?
N4 Co1 N1 104.81(5) . . ?
N2 Co1 N1 77.26(5) . . ?
O1 Co1 N1 83.84(5) . . ?
N3 Co1 N1 169.74(5) . . ?
N5 Co1 N1 87.59(5) . . ?
O2 Cl1 O3 109.67(9) . . ?
O2 Cl1 O4 110.14(10) . . ?
O3 Cl1 O4 108.76(10) . . ?
O2 Cl1 O5 109.82(9) . . ?
O3 Cl1 O5 109.21(10) . . ?
O4 Cl1 O5 109.22(11) . . ?
O9 Cl2 O7 109.33(10) . . ?
O9 Cl2 O8 109.89(12) . . ?
O7 Cl2 O8 109.35(11) . . ?
O9 Cl2 O6 109.62(10) . . ?
O7 Cl2 O6 109.59(9) . . ?
O8 Cl2 O6 109.05(10) . . ?
C20 N5 C16 117.33(14) . . ?
C20 N5 Co1 132.72(11) . . ?
C16 N5 Co1 109.57(10) . . ?
C15 N4 C14 118.54(14) . . ?
C15 N4 Co1 116.99(11) . . ?
C14 N4 Co1 123.27(11) . . ?
C11 N3 C12 109.32(13) . . ?
C11 N3 C10 108.30(14) . . ?
C12 N3 C10 105.22(13) . . ?
C11 N3 Co1 110.26(10) . . ?
C12 N3 Co1 111.45(10) . . ?
C10 N3 Co1 112.11(10) . . ?
C7 N2 C8 116.18(14) . . ?
C7 N2 Co1 116.03(11) . . ?
C8 N2 Co1 127.69(11) . . ?
C1 N1 C6 117.58(14) . . ?
C1 N1 Co1 133.02(12) . . ?
C6 N1 Co1 109.15(10) . . ?
C4 C3 C1 120.63(17) . . ?
C4 C5 C6 118.53(17) . . ?
N2 C7 C6 120.72(15) . . ?
N5 C16 C17 123.62(16) . . ?
N5 C16 C15 115.67(14) . . ?
C17 C16 C15 120.54(15) . . ?
N2 C8 C9 113.08(14) . . ?
N5 C20 C19 121.50(15) . . ?
N5 C20 C21 118.59(15) . . ?
C19 C20 C21 119.91(15) . . ?
N1 C1 C3 121.12(16) . . ?
N1 C1 C2 118.90(15) . . ?
C3 C1 C2 119.97(16) . . ?
C3 C4 C5 118.55(16) . . ?
N1 C6 C5 123.56(16) . . ?
N1 C6 C7 116.83(14) . . ?
C5 C6 C7 119.55(16) . . ?
C18 C19 C20 120.31(16) . . ?
C19 C18 C17 118.39(16) . . ?
C12 C13 C14 115.34(14) . . ?
N4 C15 C16 119.17(15) . . ?
N3 C12 C13 117.69(14) . . ?
C8 C9 C10 113.72(15) . . ?
N4 C14 C13 107.85(14) . . ?
N3 C10 C9 115.88(14) . . ?
C16 C17 C18 118.69(16) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.057
_database_code_depnum_ccdc_archive 'CCDC 959184'
