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

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Miguel Julve'
_publ_contact_author_email       JULVE@UV.ES

_publ_section_title              
;
Novel cobalt(II) coordination polymers based on
1,2,4,5-bezenetetracarboxylic acid and extended bidentate ligands
;
loop_
_publ_author_name
'Miguel Julve'
'Laura Canadillas-Delgado'
'Fernando S Delgado'
'Oscar Fabelo'
'Francesc Lloret'
;
J.Pasan
;
'Catalina Ruiz-Perez'
'Consuelo Yuste'

# Attachment 'Compounds_1_to_4_new.cif'

data_Compound-1
_database_code_depnum_ccdc_archive 'CCDC 728516'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H11 Co N2 O5'
_chemical_formula_weight         358.19

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_int_tables_number      2

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

_cell_length_a                   8.0891(12)
_cell_length_b                   9.4027(9)
_cell_length_c                   10.1213(11)
_cell_angle_alpha                114.699(11)
_cell_angle_beta                 103.187(9)
_cell_angle_gamma                101.465(9)
_cell_volume                     642.21(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Prism
_exptl_crystal_colour            Pink
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.852
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             364
_exptl_absorpt_coefficient_mu    1.367
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6296
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0778
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         6.42
_diffrn_reflns_theta_max         27.49
_reflns_number_total             2857
_reflns_number_gt                2133
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_cell_refinement       ?
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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)+(0.0166P)²+0.4801P] 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         2857
_refine_ls_number_parameters     216
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0540
_refine_ls_wR_factor_ref         0.0811
_refine_ls_wR_factor_gt          0.0731
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_restrained_S_all      1.127
_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 0.13295(6) 0.15190(6) 0.46433(5) 0.01587(14) Uani 1 1 d . . .
C1 C -0.1171(4) 0.4870(4) 0.8655(3) 0.0145(7) Uani 1 1 d . . .
C2 C -0.0318(4) 0.3695(4) 0.8521(3) 0.0153(7) Uani 1 1 d . . .
C3 C 0.0816(4) 0.3851(4) 0.9866(3) 0.0166(7) Uani 1 1 d . . .
C4 C -0.2544(4) 0.4791(4) 0.7313(4) 0.0178(7) Uani 1 1 d . . .
C5 C -0.0413(4) 0.2309(4) 0.7019(3) 0.0180(7) Uani 1 1 d . . .
C6 C -0.1029(5) 0.0476(5) 0.1382(4) 0.0269(8) Uani 1 1 d . . .
C7 C -0.2227(5) 0.0417(5) 0.0143(4) 0.0290(9) Uani 1 1 d . . .
C8 C -0.3057(4) 0.1610(4) 0.0381(4) 0.0186(7) Uani 1 1 d . . .
C9 C -0.2635(5) 0.2783(5) 0.1915(4) 0.0303(9) Uani 1 1 d . . .
C10 C -0.1439(5) 0.2743(5) 0.3101(4) 0.0303(9) Uani 1 1 d . . .
C11 C -0.6246(5) 0.2739(4) -0.2044(4) 0.0267(8) Uani 1 1 d . . .
C12 C -0.5076(5) 0.2829(4) -0.0765(4) 0.0266(8) Uani 1 1 d . . .
C13 C -0.4330(4) 0.1585(4) -0.0953(4) 0.0191(8) Uani 1 1 d . . .
C14 C -0.4848(5) 0.0305(4) -0.2455(4) 0.0240(8) Uani 1 1 d . . .
C15 C -0.6058(4) 0.0287(5) -0.3661(4) 0.0235(8) Uani 1 1 d . . .
N1 N -0.0609(3) 0.1610(4) 0.2859(3) 0.0191(6) Uani 1 1 d . . .
N2 N -0.6779(4) 0.1486(3) -0.3480(3) 0.0194(6) Uani 1 1 d . . .
O1 O -0.2879(3) 0.6106(3) 0.7543(3) 0.0339(6) Uani 1 1 d . . .
O2 O -0.3281(3) 0.3434(3) 0.6100(2) 0.0264(6) Uani 1 1 d . . .
O3 O 0.0201(3) 0.2708(3) 0.6139(2) 0.0229(5) Uani 1 1 d . . .
O4 O -0.0946(3) 0.0861(3) 0.6812(2) 0.0230(5) Uani 1 1 d . . .
O1W O 0.3356(4) 0.2966(3) 0.4549(3) 0.0330(7) Uani 1 1 d . . .
H1WA H 0.328(5) 0.330(5) 0.399(4) 0.033(12) Uiso 1 1 d . . .
H1WB H 0.445(6) 0.319(5) 0.506(4) 0.035(12) Uiso 1 1 d . . .
H3 H 0.1371 0.3054 0.9772 0.020 Uiso 1 1 calc R . .
H6 H -0.0471 -0.0328 0.1178 0.032 Uiso 1 1 calc R . .
H7 H -0.2482 -0.0425 -0.0858 0.035 Uiso 1 1 calc R . .
H9 H -0.3165 0.3607 0.2147 0.036 Uiso 1 1 calc R . .
H10 H -0.1199 0.3542 0.4117 0.036 Uiso 1 1 calc R . .
H11 H -0.6692 0.3612 -0.1893 0.032 Uiso 1 1 calc R . .
H12 H -0.4790 0.3719 0.0217 0.032 Uiso 1 1 calc R . .
H14 H -0.4370 -0.0553 -0.2649 0.029 Uiso 1 1 calc R . .
H15 H -0.6392 -0.0602 -0.4653 0.028 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 N1 2.149(3) . ?
Co1 N2 2.166(3) 1_656 ?
Co1 O1W 1.959(3) . ?
Co1 O3 1.999(2) . ?
Co1 O4 2.009(2) 2_556 ?
C1 C3 1.390(4) 2_567 ?
C1 C4 1.510(4) . ?
C2 C1 1.391(4) . ?
C2 C5 1.505(4) . ?
C3 C1 1.390(4) 2_567 ?
C3 C2 1.388(4) . ?
C4 O1 1.257(4) . ?
C4 O2 1.243(4) . ?
C6 C7 1.372(4) . ?
C7 C8 1.383(4) . ?
C9 C8 1.386(4) . ?
C10 C9 1.378(4) . ?
C11 C12 1.377(4) . ?
C12 C13 1.384(5) . ?
C13 C8 1.488(4) . ?
C14 C13 1.384(4) . ?
C15 C14 1.371(4) . ?
N1 C10 1.337(4) . ?
N1 C6 1.334(4) . ?
N2 C11 1.330(4) . ?
N2 C15 1.335(4) . ?
N2 Co1 2.166(3) 1_454 ?
O3 C5 1.261(4) . ?
O4 C5 1.253(4) . ?
O4 Co1 2.009(2) 2_556 ?

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
C1 C2 C5 125.5(3) . . ?
C2 C1 C4 124.3(3) . . ?
C2 C3 C1 123.7(3) . 2_567 ?
C3 C1 C2 117.8(3) 2_567 . ?
C3 C1 C4 117.7(3) 2_567 . ?
C3 C2 C1 118.4(3) . . ?
C3 C2 C5 115.9(3) . . ?
C5 O3 Co1 129.5(2) . . ?
C5 O4 Co1 143.4(2) . 2_556 ?
C6 C7 C8 120.0(3) . . ?
C6 N1 C10 116.0(3) . . ?
C6 N1 Co1 119.0(2) . . ?
C7 C8 C13 120.7(3) . . ?
C7 C8 C9 115.8(3) . . ?
C9 C8 C13 123.5(3) . . ?
C10 C9 C8 120.8(3) . . ?
C10 N1 Co1 125.1(2) . . ?
C11 C12 C13 119.5(3) . . ?
C11 N2 C15 116.2(3) . . ?
C11 N2 Co1 119.5(2) . 1_454 ?
C12 C13 C8 122.1(3) . . ?
C14 C13 C12 116.1(3) . . ?
C14 C13 C8 121.8(3) . . ?
C15 C14 C13 120.7(3) . . ?
C15 N2 Co1 124.3(2) . 1_454 ?
N1 C10 C9 123.0(3) . . ?
N1 C6 C7 124.3(3) . . ?
N1 Co1 N2 177.21(11) . 1_656 ?
N2 C11 C12 124.3(3) . . ?
N2 C15 C14 123.2(3) . . ?
O1 C4 C1 116.5(3) . . ?
O2 C4 C1 117.8(3) . . ?
O2 C4 O1 125.7(3) . . ?
O3 C5 C2 117.3(3) . . ?
O3 Co1 N1 88.50(9) . . ?
O3 Co1 N2 88.72(9) . 1_656 ?
O3 Co1 O4 135.85(10) . 2_556 ?
O4 C5 C2 117.2(3) . . ?
O4 C5 O3 125.2(3) . . ?
O4 Co1 N1 90.35(10) 2_556 . ?
O4 Co1 N2 91.58(10) 2_556 1_656 ?
O1W Co1 N1 92.93(11) . . ?
O1W Co1 N2 88.32(12) . 1_656 ?
O1W Co1 O3 114.74(11) . . ?
O1W Co1 O4 109.40(11) . 2_556 ?

_diffrn_measured_fraction_theta_max 0.966
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.966
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.098

data_Compound-2
_database_code_depnum_ccdc_archive 'CCDC 728517'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H28 Co N4 O10'
_chemical_formula_weight         711.54

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_int_tables_number      2

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

_cell_length_a                   9.0734(4)
_cell_length_b                   9.5955(7)
_cell_length_c                   10.1366(7)
_cell_angle_alpha                93.025(6)
_cell_angle_beta                 113.334(5)
_cell_angle_gamma                106.250(4)
_cell_volume                     764.46(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            orange-pink
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             367
_exptl_absorpt_coefficient_mu    0.631
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6600
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         5.05
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3479
_reflns_number_gt                2686
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_cell_refinement       ?
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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)+(0.0314P)²+0.3629P] 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         3479
_refine_ls_number_parameters     239
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0427
_refine_ls_wR_factor_ref         0.0891
_refine_ls_wR_factor_gt          0.0823
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_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 0.0000 0.0000 0.0000 0.01536(13) Uani 1 2 d S . .
C1 C 0.4849(3) 0.3606(2) -0.0637(2) 0.0181(4) Uani 1 1 d . . .
C2 C 0.3435(3) 0.3855(2) -0.0570(2) 0.0165(4) Uani 1 1 d . . .
C3 C 0.3603(3) 0.5251(2) 0.0049(2) 0.0201(5) Uani 1 1 d . . .
C4 C 0.4803(3) 0.2151(2) -0.1327(3) 0.0228(5) Uani 1 1 d . . .
C5 C 0.1766(3) 0.2648(2) -0.0988(2) 0.0171(4) Uani 1 1 d . . .
C6 C 0.0342(3) 0.1149(2) 0.3000(3) 0.0285(5) Uani 1 1 d . . .
C7 C 0.0432(3) 0.2073(2) 0.4138(3) 0.0299(5) Uani 1 1 d . . .
C8 C 0.0278(3) 0.3457(2) 0.3934(2) 0.0240(5) Uani 1 1 d . . .
C9 C 0.0132(3) 0.3856(2) 0.2611(3) 0.0286(5) Uani 1 1 d . . .
C10 C 0.0098(3) 0.2878(2) 0.1552(3) 0.0269(5) Uani 1 1 d . . .
C11 C 0.0232(3) 0.4402(2) 0.5095(3) 0.0294(5) Uani 1 1 d . . .
C12 C 0.6612(4) 0.1241(3) 0.4899(3) 0.0385(6) Uani 1 1 d . . .
C13 C 0.6301(4) 0.2377(3) 0.5494(3) 0.0418(7) Uani 1 1 d . . .
C14 C 0.5589(3) 0.3282(2) 0.4627(3) 0.0311(6) Uani 1 1 d . . .
C15 C 0.5228(4) 0.2986(3) 0.3163(3) 0.0455(7) Uani 1 1 d . . .
C16 C 0.5576(4) 0.1819(3) 0.2640(3) 0.0424(7) Uani 1 1 d . . .
C17 C 0.5251(4) 0.4487(3) 0.5304(3) 0.0405(6) Uani 1 1 d . . .
N1 N 0.0176(2) 0.15246(18) 0.1716(2) 0.0221(4) Uani 1 1 d . . .
N2 N 0.6258(3) 0.0967(2) 0.3494(2) 0.0285(5) Uani 1 1 d . . .
O1 O 0.6054(2) 0.1765(2) -0.0795(2) 0.0528(6) Uani 1 1 d . . .
O2 O 0.3445(2) 0.14278(18) -0.24509(19) 0.0328(4) Uani 1 1 d . . .
O3 O 0.18625(18) 0.15926(14) -0.03143(16) 0.0223(3) Uani 1 1 d . . .
O4 O 0.0439(2) 0.28233(16) -0.18692(19) 0.0320(4) Uani 1 1 d . . .
O1W O 0.1902(2) -0.06512(17) 0.15993(18) 0.0236(4) Uani 1 1 d . . .
H1WA H 0.254(4) -0.088(3) 0.135(3) 0.035(8) Uiso 1 1 d . . .
H1WB H 0.125(4) -0.141(3) 0.175(3) 0.058(9) Uiso 1 1 d . . .
H2A H 0.355(6) 0.067(6) -0.278(6) 0.028(13) Uiso 0.50 1 d P . .
H2B H 0.635(5) 0.023(6) 0.319(5) 0.013(11) Uiso 0.50 1 d P . .
H3 H 0.2654 0.5426 0.0070 0.024 Uiso 1 1 calc R . .
H6 H 0.0400 0.0211 0.3137 0.034 Uiso 1 1 calc R . .
H7 H 0.0594 0.1776 0.5030 0.036 Uiso 1 1 calc R . .
H9 H 0.0056 0.4782 0.2437 0.034 Uiso 1 1 calc R . .
H10 H 0.0017 0.3174 0.0673 0.032 Uiso 1 1 calc R . .
H11 H 0.0546 0.4148 0.6016 0.035 Uiso 1 1 calc R . .
H12 H 0.7090 0.0638 0.5503 0.046 Uiso 1 1 calc R . .
H13 H 0.6571 0.2537 0.6488 0.050 Uiso 1 1 calc R . .
H15 H 0.4752 0.3571 0.2533 0.055 Uiso 1 1 calc R . .
H16 H 0.5320 0.1627 0.1651 0.051 Uiso 1 1 calc R . .
H17 H 0.5421 0.4504 0.6272 0.049 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 N1 2.1377(16) . ?
Co1 N1 2.1377(16) 2 ?
Co1 O1W 2.1195(16) . ?
Co1 O1W 2.1195(16) 2 ?
Co1 O3 2.0797(13) . ?
Co1 O3 2.0797(13) 2 ?
C1 C3 1.392(3) 2_665 ?
C1 C4 1.510(3) . ?
C2 C1 1.394(3) . ?
C2 C5 1.507(3) . ?
C3 C1 1.392(3) 2_665 ?
C3 C2 1.391(3) . ?
C4 O1 1.221(3) . ?
C4 O2 1.275(3) . ?
C5 O3 1.255(2) . ?
C5 O4 1.247(3) . ?
C6 C7 1.379(3) . ?
C7 C8 1.391(3) . ?
C8 C11 1.469(3) . ?
C8 C9 1.380(3) . ?
C10 C9 1.374(3) . ?
C11 C11 1.326(4) 2_566 ?
C12 C13 1.367(3) . ?
C14 C13 1.375(4) . ?
C14 C15 1.381(4) . ?
C14 C17 1.477(3) . ?
C15 C16 1.380(3) . ?
C17 C17 1.285(5) 2_666 ?
N1 C10 1.336(3) . ?
N1 C6 1.331(3) . ?
N2 C12 1.324(3) . ?
N2 C16 1.317(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
C1 C2 C5 123.42(16) . . ?
C2 C1 C4 123.58(18) . . ?
C2 C3 C1 121.84(19) . 2_665 ?
C3 C1 C2 119.18(17) 2_665 . ?
C3 C1 C4 117.24(18) 2_665 . ?
C3 C2 C1 118.97(18) . . ?
C3 C2 C5 117.29(17) . . ?
C5 O3 Co1 130.48(14) . . ?
C6 C7 C8 119.1(2) . . ?
C6 N1 C10 116.85(17) . . ?
C6 N1 Co1 120.90(13) . . ?
C7 C8 C11 119.5(2) . . ?
C9 C8 C11 123.1(2) . . ?
C9 C8 C7 117.36(19) . . ?
C10 C9 C8 119.6(2) . . ?
C10 N1 Co1 122.24(15) . . ?
C11 C11 C8 123.8(3) 2_566 . ?
C12 C13 C14 120.1(2) . . ?
C13 C14 C15 116.9(2) . . ?
C13 C14 C17 118.6(2) . . ?
C15 C14 C17 124.5(2) . . ?
C16 C15 C14 119.8(3) . . ?
C16 N2 C12 118.7(2) . . ?
C17 C17 C14 126.8(3) 2_666 . ?
N1 C10 C9 123.5(2) . . ?
N1 C6 C7 123.6(2) . . ?
N1 Co1 N1 180.00(9) 2 . ?
N2 C12 C13 122.4(3) . . ?
N2 C16 C15 122.2(2) . . ?
O1 C4 C1 118.61(19) . . ?
O1 C4 O2 124.89(19) . . ?
O2 C4 C1 116.5(2) . . ?
O3 C5 C2 114.82(19) . . ?
O3 Co1 N1 89.13(6) . 2 ?
O3 Co1 N1 89.13(6) 2 . ?
O3 Co1 N1 90.87(6) . . ?
O3 Co1 N1 90.87(6) 2 2 ?
O3 Co1 O1W 89.93(6) . 2 ?
O3 Co1 O1W 89.93(6) 2 . ?
O3 Co1 O1W 90.07(6) . . ?
O3 Co1 O1W 90.07(6) 2 2 ?
O3 Co1 O3 180.00(9) 2 . ?
O4 C5 C2 118.58(18) . . ?
O4 C5 O3 126.40(19) . . ?
O1W Co1 N1 88.19(7) . . ?
O1W Co1 N1 88.19(7) 2 2 ?
O1W Co1 N1 91.81(7) . 2 ?
O1W Co1 N1 91.81(7) 2 . ?
O1W Co1 O1W 180.00(11) . 2 ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.066

data_Compound-3
_database_code_depnum_ccdc_archive 'CCDC 728518'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H24 Co N8 O10'
_chemical_formula_weight         715.50

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_int_tables_number      2

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

_cell_length_a                   8.9901(14)
_cell_length_b                   9.5945(9)
_cell_length_c                   10.2763(12)
_cell_angle_alpha                96.211(7)
_cell_angle_beta                 114.225(12)
_cell_angle_gamma                105.727(12)
_cell_volume                     753.37(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Prism
_exptl_crystal_colour            orange-pink
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             367
_exptl_absorpt_coefficient_mu    0.644
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13601
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         6.42
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3409
_reflns_number_gt                2883
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_cell_refinement       ?
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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)+(0.0378P)²+0.6423P] 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         3409
_refine_ls_number_parameters     235
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0433
_refine_ls_wR_factor_ref         0.1035
_refine_ls_wR_factor_gt          0.0979
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.104
_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 0.0000 0.0000 0.0000 0.02000(13) Uani 1 2 d S . .
C1 C 0.4781(3) 0.3548(2) -0.0621(2) 0.0238(5) Uani 1 1 d . . .
C2 C 0.3394(3) 0.3848(2) -0.0523(2) 0.0231(4) Uani 1 1 d . . .
C3 C 0.3629(3) 0.5303(2) 0.0085(3) 0.0254(5) Uani 1 1 d . . .
C4 C 0.4675(3) 0.2037(2) -0.1295(3) 0.0279(5) Uani 1 1 d . . .
C5 C 0.1694(3) 0.2644(2) -0.0897(2) 0.0239(4) Uani 1 1 d . . .
C6 C 0.0517(4) 0.1327(3) 0.3067(3) 0.0340(6) Uani 1 1 d . . .
C7 C 0.0613(4) 0.2286(3) 0.4226(3) 0.0349(6) Uani 1 1 d . . .
C8 C 0.0339(3) 0.3609(3) 0.4003(3) 0.0292(5) Uani 1 1 d . . .
C9 C 0.0076(3) 0.3962(3) 0.2683(3) 0.0312(5) Uani 1 1 d . . .
C10 C 0.0056(3) 0.2951(3) 0.1610(3) 0.0305(5) Uani 1 1 d . . .
C11 C 0.6645(4) 0.1433(3) 0.4970(3) 0.0487(7) Uani 1 1 d . . .
C12 C 0.6255(5) 0.2561(4) 0.5545(3) 0.0532(8) Uani 1 1 d . . .
C13 C 0.5603(4) 0.3442(3) 0.4670(3) 0.0411(6) Uani 1 1 d . . .
C14 C 0.5366(4) 0.3172(3) 0.3240(3) 0.0481(7) Uani 1 1 d . . .
C15 C 0.5773(4) 0.2007(3) 0.2749(3) 0.0443(7) Uani 1 1 d . . .
H2 H 0.334(5) 0.023(5) -0.292(5) 0.089(13) Uiso 1 1 d . . .
H3 H 0.2700 0.5513 0.0135 0.030 Uiso 1 1 calc R . .
H6 H 0.0648 0.0415 0.3195 0.041 Uiso 1 1 calc R . .
H7 H 0.0855 0.2049 0.5128 0.042 Uiso 1 1 calc R . .
H9 H -0.0085 0.4856 0.2518 0.037 Uiso 1 1 calc R . .
H10 H -0.0098 0.3195 0.0723 0.037 Uiso 1 1 calc R . .
H11 H 0.7095 0.0840 0.5571 0.058 Uiso 1 1 calc R . .
H12 H 0.6432 0.2723 0.6514 0.064 Uiso 1 1 calc R . .
H14 H 0.4942 0.3763 0.2624 0.058 Uiso 1 1 calc R . .
H15 H 0.5595 0.1811 0.1780 0.053 Uiso 1 1 calc R . .
H1WA H 0.262(5) -0.076(4) 0.131(4) 0.057(11) Uiso 1 1 d . . .
H1WB H 0.141(5) -0.133(4) 0.171(4) 0.061(11) Uiso 1 1 d . . .
N1 N 0.0247(3) 0.1639(2) 0.1779(2) 0.0278(4) Uani 1 1 d . . .
N2 N 0.0366(3) 0.4546(2) 0.5198(2) 0.0350(5) Uani 1 1 d . . .
N3 N 0.6407(3) 0.1153(2) 0.3592(2) 0.0354(5) Uani 1 1 d . . .
N4 N 0.5235(4) 0.4600(3) 0.5388(3) 0.0505(6) Uani 1 1 d . . .
O1 O 0.5884(3) 0.1602(2) -0.0734(2) 0.0497(5) Uani 1 1 d . . .
O2 O 0.3261(2) 0.12853(19) -0.2502(2) 0.0390(4) Uani 1 1 d . . .
O3 O 0.1831(2) 0.15663(17) -0.03236(18) 0.0275(4) Uani 1 1 d . . .
O4 O 0.0319(2) 0.2853(2) -0.1647(2) 0.0394(4) Uani 1 1 d . . .
O1W O 0.1999(2) -0.05470(19) 0.1591(2) 0.0291(4) 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 N1 2.1725(18) . ?
Co1 N1 2.1725(18) 2 ?
Co1 O1W 2.1128(17) . ?
Co1 O1W 2.1128(17) 2 ?
Co1 O3 2.0727(15) . ?
Co1 O3 2.0727(15) 2 ?
C1 C3 1.389(3) 2_665 ?
C1 C4 1.498(3) . ?
C2 C1 1.393(3) . ?
C2 C5 1.512(3) . ?
C3 C1 1.389(3) 2_665 ?
C3 C2 1.388(3) . ?
C4 O1 1.213(3) . ?
C4 O2 1.300(3) . ?
C5 O3 1.254(3) . ?
C5 O4 1.244(3) . ?
C6 C7 1.382(3) . ?
C6 N1 1.328(3) . ?
C7 C8 1.382(3) . ?
C8 N2 1.429(3) . ?
C9 C8 1.375(3) . ?
C10 C9 1.378(3) . ?
C10 N1 1.335(3) . ?
C11 C12 1.371(4) . ?
C11 N3 1.327(4) . ?
C12 C13 1.366(4) . ?
C13 N4 1.453(3) . ?
C14 C13 1.380(4) . ?
C15 C14 1.374(4) . ?
C15 N3 1.323(4) . ?
N2 N2 1.234(4) 2_566 ?
N4 N4 1.198(5) 2_666 ?

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
C1 C2 C5 123.26(19) . . ?
C2 C1 C4 123.91(19) . . ?
C2 C3 C1 121.6(2) . 2_665 ?
C3 C1 C2 119.54(19) 2_665 . ?
C3 C1 C4 116.55(19) 2_665 . ?
C3 C2 C1 118.9(2) . . ?
C3 C2 C5 117.51(19) . . ?
C5 O3 Co1 129.37(14) . . ?
C6 C7 C8 117.9(2) . . ?
C6 N1 C10 117.6(2) . . ?
C6 N1 Co1 120.13(15) . . ?
C7 C8 N2 116.7(2) . . ?
C8 C9 C10 118.1(2) . . ?
C9 C8 C7 119.6(2) . . ?
C9 C8 N2 123.8(2) . . ?
C10 N1 Co1 122.24(16) . . ?
C12 C13 C14 118.9(2) . . ?
C12 C13 N4 114.4(3) . . ?
C13 C12 C11 118.9(3) . . ?
C14 C13 N4 126.7(3) . . ?
C15 C14 C13 118.3(3) . . ?
C15 N3 C11 118.1(2) . . ?
N1 C10 C9 123.4(2) . . ?
N1 C6 C7 123.4(2) . . ?
N1 Co1 N1 180.00(10) . 2 ?
N2 N2 C8 112.7(3) 2_566 . ?
N3 C11 C12 122.8(3) . . ?
N3 C15 C14 123.0(3) . . ?
N4 N4 C13 112.1(3) 2_666 . ?
O1 C4 C1 120.0(2) . . ?
O1 C4 O2 124.1(2) . . ?
O2 C4 C1 115.8(2) . . ?
O3 C5 C2 115.27(19) . . ?
O3 Co1 N1 88.52(7) . 2 ?
O3 Co1 N1 88.52(7) 2 . ?
O3 Co1 N1 91.48(7) . . ?
O3 Co1 N1 91.48(7) 2 2 ?
O3 Co1 O1W 89.80(7) . 2 ?
O3 Co1 O1W 89.80(7) 2 . ?
O3 Co1 O1W 90.20(7) . . ?
O3 Co1 O1W 90.20(7) 2 2 ?
O3 Co1 O3 180.00(8) . 2 ?
O4 C5 C2 118.00(19) . . ?
O4 C5 O3 126.6(2) . . ?
O1W Co1 N1 88.06(7) . . ?
O1W Co1 N1 88.06(7) 2 2 ?
O1W Co1 N1 91.94(7) . 2 ?
O1W Co1 N1 91.94(7) 2 . ?
O1W Co1 O1W 180.00(15) 2 . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.062

data_Compound-4
_database_code_depnum_ccdc_archive 'CCDC 728519'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H25 Co N2 O10'
_chemical_formula_weight         476.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3490 0.9720 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 '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'
_symmetry_int_tables_number      2

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

_cell_length_a                   9.3705(10)
_cell_length_b                   11.4792(13)
_cell_length_c                   11.6886(9)
_cell_angle_alpha                60.996(8)
_cell_angle_beta                 66.612(8)
_cell_angle_gamma                66.832(8)
_cell_volume                     977.13(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Prism
_exptl_crystal_colour            Pink
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             496
_exptl_absorpt_coefficient_mu    0.939
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_correction_T_min  0.9120
_exptl_absorpt_correction_T_max  0.9634
_exptl_absorpt_process_details   ?

_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  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19033
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.45
_diffrn_reflns_theta_max         27.50
_reflns_number_total             4468
_reflns_number_gt                3187
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_cell_refinement       'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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)+(0.1377P)²+1.1229P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.023(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4468
_refine_ls_number_parameters     275
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0723
_refine_ls_wR_factor_ref         0.2283
_refine_ls_wR_factor_gt          0.2005
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.072
_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 1.0000 0.0000 1.0000 0.0314(3) Uani 1 2 d S . .
Co2 Co 0.5000 0.5000 0.5000 0.0274(3) Uani 1 2 d S . .
C1 C 0.5998(5) 0.3778(4) 0.9856(4) 0.0248(8) Uani 1 1 d . . .
C2 C 0.5287(5) 0.4829(4) 0.8818(4) 0.0242(8) Uani 1 1 d . . .
C3 C 0.4292(5) 0.6036(4) 0.8980(4) 0.0264(9) Uani 1 1 d . . .
C4 C 0.6932(5) 0.2389(4) 0.9778(4) 0.0270(9) Uani 1 1 d . . .
C5 C 0.5786(5) 0.4729(4) 0.7453(4) 0.0264(9) Uani 1 1 d . . .
C6 C 1.2441(6) 0.0612(5) 0.7263(5) 0.0410(11) Uani 1 1 d . . .
C7 C 1.3075(6) 0.1110(5) 0.5875(5) 0.0395(11) Uani 1 1 d . . .
C8 C 1.2092(6) 0.1853(5) 0.5008(5) 0.0370(11) Uani 1 1 d . . .
C9 C 1.0457(6) 0.2144(5) 0.5616(5) 0.0403(11) Uani 1 1 d . . .
C10 C 0.9895(6) 0.1638(5) 0.7005(5) 0.0379(11) Uani 1 1 d . . .
C11 C 1.2716(7) 0.2250(5) 0.3519(5) 0.0453(12) Uani 1 1 d . . .
C12 C 1.2139(7) 0.1589(5) 0.2971(5) 0.0465(13) Uani 1 1 d . . .
C13 C 1.2792(6) 0.0053(5) 0.3440(5) 0.0387(11) Uani 1 1 d . . .
C14 C 1.2289(6) -0.0841(5) 0.4768(5) 0.0392(11) Uani 1 1 d . . .
C15 C 1.2955(6) -0.2233(5) 0.5151(5) 0.0364(10) Uani 1 1 d . . .
C16 C 1.4546(6) -0.1961(5) 0.3011(5) 0.0365(10) Uani 1 1 d . . .
C17 C 1.3951(6) -0.0554(5) 0.2551(5) 0.0384(11) Uani 1 1 d . . .
O1 O 0.8315(4) 0.1900(3) 0.9975(3) 0.0356(8) Uani 1 1 d . . .
O2 O 0.6252(4) 0.1809(3) 0.9556(4) 0.0407(8) Uani 1 1 d . . .
O3 O 0.4697(4) 0.4952(3) 0.6950(3) 0.0337(7) Uani 1 1 d . . .
O4 O 0.7259(4) 0.4469(4) 0.6916(3) 0.0386(8) Uani 1 1 d . . .
O1W O 1.1702(4) 0.0650(4) 1.0165(4) 0.0466(9) Uani 1 1 d . . .
O2W O 0.7369(4) 0.5155(4) 0.4382(3) 0.0435(9) Uani 1 1 d . . .
O3W O 0.9944(5) 0.4071(5) 0.7704(4) 0.0641(12) Uani 1 1 d . . .
O4W O 0.9483(10) 0.2108(9) 1.1685(9) 0.140(3) Uani 1 1 d . . .
O5W O 1.2795(15) 0.2872(14) 0.9540(11) 0.203(5) Uani 1 1 d . . .
O6W O 0.9070(16) 0.4659(9) 1.1346(11) 0.198(5) Uani 1 1 d . . .
N1 N 1.0861(4) 0.0857(4) 0.7834(4) 0.0348(9) Uani 1 1 d . . .
N2 N 1.4063(5) -0.2813(4) 0.4297(4) 0.0341(9) Uani 1 1 d . . .
H3 H 0.3811 0.6732 0.8295 0.032 Uiso 1 1 calc R . .
H6 H 1.3141 0.0086 0.7820 0.049 Uiso 1 1 calc R . .
H7 H 1.4183 0.0938 0.5524 0.047 Uiso 1 1 calc R . .
H9 H 0.9734 0.2685 0.5080 0.048 Uiso 1 1 calc R . .
H10 H 0.8793 0.1851 0.7382 0.045 Uiso 1 1 calc R . .
H11A H 1.3881 0.1985 0.3294 0.054 Uiso 1 1 calc R . .
H11B H 1.2381 0.3243 0.3074 0.054 Uiso 1 1 calc R . .
H12A H 1.0975 0.1798 0.3254 0.056 Uiso 1 1 calc R . .
H12B H 1.2456 0.1995 0.1990 0.056 Uiso 1 1 calc R . .
H14 H 1.1500 -0.0495 0.5396 0.047 Uiso 1 1 calc R . .
H15 H 1.2618 -0.2803 0.6050 0.044 Uiso 1 1 calc R . .
H16 H 1.5320 -0.2340 0.2401 0.044 Uiso 1 1 calc R . .
H17 H 1.4319 -0.0007 0.1649 0.046 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
O2W Co2 2.096(3) . ?
O1W Co1 2.112(4) . ?
Co2 O2W 2.096(3) 2_666 ?
Co2 N2 2.142(4) 1_465 ?
Co2 N2 2.142(4) 2_756 ?
Co2 O3 2.158(3) . ?
Co2 O3 2.158(3) 2_666 ?
Co1 O1W 2.112(4) 2_757 ?
Co1 O1 2.125(3) . ?
Co1 O1 2.125(3) 2_757 ?
Co1 N1 2.149(4) . ?
Co1 N1 2.149(4) 2_757 ?
O2 C4 1.245(5) . ?
O1 C4 1.260(5) . ?
O3 C5 1.256(5) . ?
O4 C5 1.249(5) . ?
N1 C10 1.333(6) . ?
N1 C6 1.336(6) . ?
C2 C3 1.387(6) . ?
C2 C1 1.401(5) . ?
C2 C5 1.523(5) . ?
C4 C1 1.515(6) . ?
N2 C15 1.340(6) . ?
N2 C16 1.343(6) . ?
N2 Co2 2.142(4) 1_645 ?
C3 C1 1.383(5) 2_667 ?
C1 C3 1.383(5) 2_667 ?
C14 C15 1.373(7) . ?
C14 C13 1.393(7) . ?
C13 C17 1.398(7) . ?
C13 C12 1.505(7) . ?
C17 C16 1.377(7) . ?
C9 C10 1.378(7) . ?
C9 C8 1.388(7) . ?
C6 C7 1.383(7) . ?
C7 C8 1.374(7) . ?
C8 C11 1.487(7) . ?
C12 C11 1.533(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 C2 C5 120.1(4) . . ?
C1 C3 C2 121.1(4) 2_667 . ?
C2 C1 C4 120.4(3) . . ?
C3 C1 C2 119.6(4) 2_667 . ?
C3 C1 C4 119.7(4) 2_667 . ?
C3 C2 C1 119.3(4) . . ?
C3 C2 C5 120.0(3) . . ?
C4 O1 Co1 130.1(3) . . ?
C5 O3 Co2 127.0(3) . . ?
C6 N1 Co1 119.6(3) . . ?
C7 C8 C11 122.7(5) . . ?
C7 C8 C9 115.7(4) . . ?
C8 C11 C12 113.4(4) . . ?
C8 C7 C6 121.0(5) . . ?
C9 C8 C11 121.5(5) . . ?
C10 C9 C8 120.6(4) . . ?
C10 N1 C6 117.1(4) . . ?
C10 N1 Co1 123.4(3) . . ?
C13 C12 C11 113.6(4) . . ?
C14 C13 C12 122.5(5) . . ?
C14 C13 C17 116.3(5) . . ?
C15 C14 C13 120.1(5) . . ?
C15 N2 C16 116.9(4) . . ?
C15 N2 Co2 120.3(3) . 1_645 ?
C16 C17 C13 120.0(5) . . ?
C16 N2 Co2 122.8(3) . 1_645 ?
C17 C13 C12 121.2(5) . . ?
N1 C10 C9 122.9(4) . . ?
N1 C6 C7 122.5(4) . . ?
N1 Co1 N1 180.0 . 2_757 ?
N2 C15 C14 123.5(4) . . ?
N2 C16 C17 123.1(4) . . ?
N2 Co2 N2 180.000(1) 1_465 2_756 ?
N2 Co2 O3 89.11(13) 1_465 . ?
N2 Co2 O3 89.11(13) 2_756 2_666 ?
N2 Co2 O3 90.89(13) 1_465 2_666 ?
N2 Co2 O3 90.89(13) 2_756 . ?
O1 C4 C1 117.5(4) . . ?
O1 Co1 N1 88.93(13) . 2_757 ?
O1 Co1 N1 88.93(13) 2_757 . ?
O1 Co1 N1 91.07(13) . . ?
O1 Co1 N1 91.07(13) 2_757 2_757 ?
O1 Co1 O1 180.0(2) . 2_757 ?
O2 C4 C1 117.2(4) . . ?
O2 C4 O1 125.3(4) . . ?
O3 C5 C2 118.0(4) . . ?
O3 Co2 O3 180.00(18) . 2_666 ?
O4 C5 C2 116.2(4) . . ?
O4 C5 O3 125.8(4) . . ?
O1W Co1 N1 89.72(15) . . ?
O1W Co1 N1 89.72(15) 2_757 2_757 ?
O1W Co1 N1 90.28(15) . 2_757 ?
O1W Co1 N1 90.28(15) 2_757 . ?
O1W Co1 O1 89.20(13) . . ?
O1W Co1 O1 89.20(13) 2_757 2_757 ?
O1W Co1 O1 90.80(13) . 2_757 ?
O1W Co1 O1 90.80(13) 2_757 . ?
O1W Co1 O1W 180.00(17) 2_757 . ?
O2W Co2 N2 87.46(15) . 2_756 ?
O2W Co2 N2 87.46(15) 2_666 1_465 ?
O2W Co2 N2 92.54(15) . 1_465 ?
O2W Co2 N2 92.54(15) 2_666 2_756 ?
O2W Co2 O2W 180.0(2) . 2_666 ?
O2W Co2 O3 89.38(12) . 2_666 ?
O2W Co2 O3 89.38(12) 2_666 . ?
O2W Co2 O3 90.62(12) . . ?
O2W Co2 O3 90.62(12) 2_666 2_666 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.999
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.162


