# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Song Gao'
_publ_contact_author_email       GAOSONG@PKU.EDU.CN

_publ_section_title              
;
Transition metal coordination frameworks with bridges
of 1,2-bis(4-pyridyl)ethane-N,N'-dioxide incorporating anions of
different size
;
loop_
_publ_author_name
'Song Gao.'
'Stuart Batten'
'Hao-Ling Sun.'
'Zhe-Ming Wang.'

# Attachment 'last-1.cif'

data_last-1
_database_code_depnum_ccdc_archive 'CCDC 691371'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H36 Cl2 Mn N6 O14'
_chemical_formula_weight         902.55

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   P-3

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

_cell_length_a                   13.6564(4)
_cell_length_b                   13.6564(4)
_cell_length_c                   6.1296(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     990.00(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    15800
_cell_measurement_theta_min      3.395
_cell_measurement_theta_max      27.485

_exptl_crystal_description       block
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             465
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean 0.76
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18384
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         3.45
_diffrn_reflns_theta_max         27.40
_reflns_number_total             1517
_reflns_number_gt                1132
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_publ_section_references         
;
collect:
"Collect" data collection software, Nonius B.V., Delft, The Netherlands, 1998.

HKL Scalepack & HKL Denzo:
Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected
in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular
Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet,
Eds., Academic Press.

absorption correction:
R.H. Blessing (1995) Acta Cryst. A51, 33-37.
R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426.

maXus:
S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland
maXus: a computer program for the solution and refinement of crystal
structures from diffraction data, University of Glasgow, Scotland, UK,
Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama,
Japan (1998).

Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray
Instruments Inc., Madison, Wisconsin, USA.

Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen,
Germany.
;

_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)+(0.1240P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1517
_refine_ls_number_parameters     90
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0550
_refine_ls_wR_factor_ref         0.1851
_refine_ls_wR_factor_gt          0.1766
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_restrained_S_all      1.107
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.0000 0.0000 0.5000 0.0336(3) Uani 1 6 d S . .
Cl1 Cl 0.3333 0.6667 0.7384(4) 0.0884(6) Uani 1 3 d S . .
O1 O 0.10531(15) 0.15388(15) 0.3163(3) 0.0479(5) Uani 1 1 d . . .
O2 O 0.4329(5) 0.7483(6) 0.6564(14) 0.274(4) Uani 1 1 d . . .
O3 O 0.3333 0.6667 0.9518(15) 0.280(7) Uani 1 3 d S . .
N1 N 0.07991(17) 0.23494(17) 0.2778(3) 0.0409(5) Uani 1 1 d . . .
C1 C -0.0209(3) 0.2099(2) 0.1992(4) 0.0497(7) Uani 1 1 d . . .
H1 H -0.0753 0.1346 0.1758 0.060 Uiso 1 1 calc R . .
C2 C -0.0458(3) 0.2933(2) 0.1523(5) 0.0551(8) Uani 1 1 d . . .
H2 H -0.1172 0.2742 0.1006 0.066 Uiso 1 1 calc R . .
C3 C 0.0361(3) 0.4070(2) 0.1819(4) 0.0530(8) Uani 1 1 d . . .
C4 C 0.0125(3) 0.5000(3) 0.1210(5) 0.0628(9) Uani 1 1 d . . .
H4A H 0.0774 0.5723 0.1593 0.075 Uiso 1 1 calc R . .
H4B H -0.0516 0.4913 0.2047 0.075 Uiso 1 1 calc R . .
C5 C 0.1381(3) 0.4284(2) 0.2670(5) 0.0619(8) Uani 1 1 d . . .
H5 H 0.1945 0.5028 0.2912 0.074 Uiso 1 1 calc R . .
C6 C 0.1582(3) 0.3427(2) 0.3166(5) 0.0566(8) Uani 1 1 d . . .
H6 H 0.2270 0.3593 0.3782 0.068 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
Mn1 O1 2.1748(17) 5_556 ?
Mn1 O1 2.1748(17) 2 ?
Mn1 O1 2.1748(17) 6_556 ?
Mn1 O1 2.1748(17) 4_556 ?
Mn1 O1 2.1748(17) . ?
Mn1 O1 2.1748(17) 3 ?
Cl1 O3 1.308(9) . ?
Cl1 O2 1.352(5) 2_665 ?
Cl1 O2 1.352(5) . ?
Cl1 O2 1.352(5) 3_565 ?
O1 N1 1.336(3) . ?
N1 C1 1.331(4) . ?
N1 C6 1.339(3) . ?
C1 C2 1.372(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.400(4) . ?
C2 H2 0.9300 . ?
C3 C5 1.376(4) . ?
C3 C4 1.505(4) . ?
C4 C4 1.522(6) 4_565 ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.362(4) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?

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 Mn1 O1 180.00(6) 5_556 2 ?
O1 Mn1 O1 95.62(7) 5_556 6_556 ?
O1 Mn1 O1 84.38(7) 2 6_556 ?
O1 Mn1 O1 95.62(7) 5_556 4_556 ?
O1 Mn1 O1 84.38(7) 2 4_556 ?
O1 Mn1 O1 95.62(7) 6_556 4_556 ?
O1 Mn1 O1 84.38(7) 5_556 . ?
O1 Mn1 O1 95.62(7) 2 . ?
O1 Mn1 O1 84.38(7) 6_556 . ?
O1 Mn1 O1 180.00(8) 4_556 . ?
O1 Mn1 O1 84.38(7) 5_556 3 ?
O1 Mn1 O1 95.62(7) 2 3 ?
O1 Mn1 O1 180.0 6_556 3 ?
O1 Mn1 O1 84.38(7) 4_556 3 ?
O1 Mn1 O1 95.62(7) . 3 ?
O3 Cl1 O2 111.8(4) . 2_665 ?
O3 Cl1 O2 111.8(4) . . ?
O2 Cl1 O2 107.0(4) 2_665 . ?
O3 Cl1 O2 111.8(4) . 3_565 ?
O2 Cl1 O2 107.0(4) 2_665 3_565 ?
O2 Cl1 O2 107.0(4) . 3_565 ?
N1 O1 Mn1 124.88(14) . . ?
C1 N1 O1 120.9(2) . . ?
C1 N1 C6 120.1(2) . . ?
O1 N1 C6 119.0(2) . . ?
N1 C1 C2 121.1(3) . . ?
N1 C1 H1 119.5 . . ?
C2 C1 H1 119.5 . . ?
C1 C2 C3 120.1(3) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
C5 C3 C2 116.5(2) . . ?
C5 C3 C4 122.5(3) . . ?
C2 C3 C4 121.0(3) . . ?
C3 C4 C4 112.6(3) . 4_565 ?
C3 C4 H4A 109.1 . . ?
C4 C4 H4A 109.1 4_565 . ?
C3 C4 H4B 109.1 . . ?
C4 C4 H4B 109.1 4_565 . ?
H4A C4 H4B 107.8 . . ?
C6 C5 C3 121.3(3) . . ?
C6 C5 H5 119.3 . . ?
C3 C5 H5 119.3 . . ?
N1 C6 C5 120.8(3) . . ?
N1 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.40
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.067

# Attachment 'last-2.cif'

data_last-2
_database_code_depnum_ccdc_archive 'CCDC 691372'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H40 Cl2 Cu N6 O16'
_chemical_formula_weight         947.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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                   5.8754(2)
_cell_length_b                   13.3670(3)
_cell_length_c                   14.6338(4)
_cell_angle_alpha                114.664(2)
_cell_angle_beta                 99.7320(10)
_cell_angle_gamma                95.8000(10)
_cell_volume                     1010.34(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    16524
_cell_measurement_theta_min      3.395
_cell_measurement_theta_max      27.485

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             489
_exptl_absorpt_coefficient_mu    0.753
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.829
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean 0.76
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18322
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.42
_diffrn_reflns_theta_max         27.46
_reflns_number_total             4581
_reflns_number_gt                3030
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_publ_section_references         
;
collect:
"Collect" data collection software, Nonius B.V., Delft, The Netherlands, 1998.

HKL Scalepack & HKL Denzo:
Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected
in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular
Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet,
Eds., Academic Press.

absorption correction:
R.H. Blessing (1995) Acta Cryst. A51, 33-37.
R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426.

maXus:
S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland
maXus: a computer program for the solution and refinement of crystal
structures from diffraction data, University of Glasgow, Scotland, UK,
Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama,
Japan (1998).

Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray
Instruments Inc., Madison, Wisconsin, USA.

Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen,
Germany.
;

_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)+(0.0852P)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    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.009(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4581
_refine_ls_number_parameters     286
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.1358
_refine_ls_wR_factor_gt          0.1262
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_restrained_S_all      0.973
_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
Cu2 Cu 0.0000 0.0000 0.0000 0.03365(18) Uani 1 2 d S . .
Cl1 Cl 0.3877(2) -0.28628(10) 0.33507(7) 0.0812(3) Uani 1 1 d . . .
O1 O 0.1445(3) -0.10273(14) 0.04684(13) 0.0378(4) Uani 1 1 d . . .
O2 O -0.0686(3) 0.09170(14) 0.13281(12) 0.0390(4) Uani 1 1 d . . .
O3 O -0.4761(4) 0.2579(2) 0.25799(19) 0.0806(8) Uani 1 1 d . . .
O4 O 0.4098(5) 0.1113(2) 0.0540(2) 0.0574(6) Uani 1 1 d . . .
O5 O 0.3614(8) -0.2091(4) 0.2965(4) 0.185(3) Uani 1 1 d . . .
O6 O 0.5714(11) -0.3438(7) 0.3062(5) 0.239(3) Uani 1 1 d . . .
O7 O 0.1870(9) -0.3664(4) 0.2958(3) 0.1545(19) Uani 1 1 d . . .
O8 O 0.4471(9) -0.2359(3) 0.4403(2) 0.1488(18) Uani 1 1 d . . .
N1 N 0.0174(4) -0.20132(17) 0.03001(15) 0.0341(5) Uani 1 1 d . . .
N2 N -0.0517(4) 0.05685(18) 0.20753(15) 0.0371(5) Uani 1 1 d . . .
N3 N -0.2601(5) 0.3034(2) 0.3146(2) 0.0595(7) Uani 1 1 d . . .
C1 C -0.1035(5) -0.2753(2) -0.0646(2) 0.0423(6) Uani 1 1 d . . .
H1A H -0.1022 -0.2591 -0.1205 0.051 Uiso 1 1 calc R . .
C2 C -0.2292(5) -0.3751(2) -0.0795(2) 0.0479(7) Uani 1 1 d . . .
H2A H -0.3124 -0.4263 -0.1457 0.057 Uiso 1 1 calc R . .
C3 C -0.2345(5) -0.4010(2) 0.0030(2) 0.0448(7) Uani 1 1 d . . .
C4 C -0.3802(6) -0.5081(2) -0.0111(3) 0.0529(7) Uani 1 1 d . . .
H4A H -0.2975 -0.5347 0.0350 0.063 Uiso 1 1 calc R . .
H4B H -0.4000 -0.5649 -0.0815 0.063 Uiso 1 1 calc R . .
C5 C -0.1063(6) -0.3223(3) 0.0985(2) 0.0531(8) Uani 1 1 d . . .
H5A H -0.1057 -0.3363 0.1557 0.064 Uiso 1 1 calc R . .
C6 C 0.0201(5) -0.2243(2) 0.1113(2) 0.0473(7) Uani 1 1 d . . .
H6A H 0.1087 -0.1730 0.1765 0.057 Uiso 1 1 calc R . .
C7 C -0.2446(6) -0.0007(3) 0.2141(2) 0.0506(7) Uani 1 1 d . . .
H7A H -0.3861 -0.0187 0.1660 0.061 Uiso 1 1 calc R . .
C8 C -0.2306(7) -0.0322(3) 0.2918(2) 0.0653(10) Uani 1 1 d . . .
H8A H -0.3642 -0.0725 0.2956 0.078 Uiso 1 1 calc R . .
C9 C -0.0232(8) -0.0059(3) 0.3653(2) 0.0686(11) Uani 1 1 d . . .
C10 C -0.0046(12) -0.0399(3) 0.4523(3) 0.121(2) Uani 1 1 d . . .
H10A H -0.1386 -0.0989 0.4341 0.145 Uiso 1 1 calc R . .
H10B H 0.1354 -0.0721 0.4555 0.145 Uiso 1 1 calc R . .
C11 C 0.1682(7) 0.0547(3) 0.3562(2) 0.0630(9) Uani 1 1 d . . .
H11A H 0.3107 0.0750 0.4043 0.076 Uiso 1 1 calc R . .
C12 C 0.1512(6) 0.0858(2) 0.2764(2) 0.0476(7) Uani 1 1 d . . .
H12A H 0.2817 0.1268 0.2711 0.057 Uiso 1 1 calc R . .
C13 C -0.1806(6) 0.2837(3) 0.3965(3) 0.0619(9) Uani 1 1 d . . .
H13A H -0.2784 0.2355 0.4106 0.074 Uiso 1 1 calc R . .
C14 C 0.0360(6) 0.3317(3) 0.4581(3) 0.0604(8) Uani 1 1 d . . .
H14A H 0.0849 0.3162 0.5139 0.072 Uiso 1 1 calc R . .
C15 C 0.1881(6) 0.4043(3) 0.4396(2) 0.0534(8) Uani 1 1 d . . .
C16 C 0.4284(6) 0.4580(3) 0.5117(3) 0.0603(8) Uani 1 1 d . . .
H16A H 0.5163 0.3994 0.5083 0.072 Uiso 1 1 calc R . .
H16B H 0.4092 0.4957 0.5819 0.072 Uiso 1 1 calc R . .
C17 C 0.1037(6) 0.4233(3) 0.3557(3) 0.0652(9) Uani 1 1 d . . .
H17A H 0.1995 0.4708 0.3401 0.078 Uiso 1 1 calc R . .
C18 C -0.1201(7) 0.3732(3) 0.2942(3) 0.0707(10) Uani 1 1 d . . .
H18A H -0.1739 0.3879 0.2384 0.085 Uiso 1 1 calc R . .
H1W H 0.452(6) 0.164(3) 0.115(3) 0.052(10) Uiso 1 1 d . . .
H2W H 0.521(8) 0.101(4) 0.036(3) 0.082(16) 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
Cu2 O2 1.9541(16) 2 ?
Cu2 O2 1.9541(16) . ?
Cu2 O1 1.9751(16) 2 ?
Cu2 O1 1.9751(16) . ?
Cl1 O8 1.361(3) . ?
Cl1 O7 1.367(4) . ?
Cl1 O5 1.377(4) . ?
Cl1 O6 1.410(6) . ?
O1 N1 1.350(3) . ?
O2 N2 1.349(2) . ?
O3 N3 1.317(4) . ?
O4 H1W 0.85(3) . ?
O4 H2W 0.75(5) . ?
N1 C1 1.335(3) . ?
N1 C6 1.345(3) . ?
N2 C12 1.327(4) . ?
N2 C7 1.344(3) . ?
N3 C18 1.340(4) . ?
N3 C13 1.350(5) . ?
C1 C2 1.370(4) . ?
C1 H1A 0.9300 . ?
C2 C3 1.391(4) . ?
C2 H2A 0.9300 . ?
C3 C5 1.373(4) . ?
C3 C4 1.507(4) . ?
C4 C4 1.513(6) 2_445 ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.362(4) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C7 C8 1.361(4) . ?
C7 H7A 0.9300 . ?
C8 C9 1.386(5) . ?
C8 H8A 0.9300 . ?
C9 C11 1.376(5) . ?
C9 C10 1.512(4) . ?
C10 C10 1.345(8) 2_556 ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.387(4) . ?
C11 H11A 0.9300 . ?
C12 H12A 0.9300 . ?
C13 C14 1.345(5) . ?
C13 H13A 0.9300 . ?
C14 C15 1.393(4) . ?
C14 H14A 0.9300 . ?
C15 C17 1.377(5) . ?
C15 C16 1.510(5) . ?
C16 C16 1.522(6) 2_666 ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.381(5) . ?
C17 H17A 0.9300 . ?
C18 H18A 0.9300 . ?

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
O2 Cu2 O2 180.00(10) 2 . ?
O2 Cu2 O1 94.81(7) 2 2 ?
O2 Cu2 O1 85.19(7) . 2 ?
O2 Cu2 O1 85.19(7) 2 . ?
O2 Cu2 O1 94.81(7) . . ?
O1 Cu2 O1 180.00(8) 2 . ?
O8 Cl1 O7 112.4(3) . . ?
O8 Cl1 O5 111.4(3) . . ?
O7 Cl1 O5 109.4(2) . . ?
O8 Cl1 O6 104.5(3) . . ?
O7 Cl1 O6 106.1(4) . . ?
O5 Cl1 O6 112.8(4) . . ?
N1 O1 Cu2 121.00(14) . . ?
N2 O2 Cu2 120.63(14) . . ?
H1W O4 H2W 105(4) . . ?
C1 N1 C6 120.6(2) . . ?
C1 N1 O1 121.38(19) . . ?
C6 N1 O1 118.0(2) . . ?
C12 N2 C7 121.6(2) . . ?
C12 N2 O2 119.2(2) . . ?
C7 N2 O2 119.1(2) . . ?
O3 N3 C18 120.5(3) . . ?
O3 N3 C13 120.2(3) . . ?
C18 N3 C13 119.3(3) . . ?
N1 C1 C2 120.1(2) . . ?
N1 C1 H1A 120.0 . . ?
C2 C1 H1A 120.0 . . ?
C1 C2 C3 121.0(3) . . ?
C1 C2 H2A 119.5 . . ?
C3 C2 H2A 119.5 . . ?
C5 C3 C2 116.6(3) . . ?
C5 C3 C4 121.6(3) . . ?
C2 C3 C4 121.8(3) . . ?
C3 C4 C4 112.0(3) . 2_445 ?
C3 C4 H4A 109.2 . . ?
C4 C4 H4A 109.2 2_445 . ?
C3 C4 H4B 109.2 . . ?
C4 C4 H4B 109.2 2_445 . ?
H4A C4 H4B 107.9 . . ?
C6 C5 C3 121.4(3) . . ?
C6 C5 H5A 119.3 . . ?
C3 C5 H5A 119.3 . . ?
N1 C6 C5 120.2(3) . . ?
N1 C6 H6A 119.9 . . ?
C5 C6 H6A 119.9 . . ?
N2 C7 C8 119.3(3) . . ?
N2 C7 H7A 120.3 . . ?
C8 C7 H7A 120.3 . . ?
C7 C8 C9 121.9(3) . . ?
C7 C8 H8A 119.0 . . ?
C9 C8 H8A 119.0 . . ?
C11 C9 C8 116.5(3) . . ?
C11 C9 C10 120.8(4) . . ?
C8 C9 C10 122.7(4) . . ?
C10 C10 C9 117.9(5) 2_556 . ?
C10 C10 H10A 107.8 2_556 . ?
C9 C10 H10A 107.8 . . ?
C10 C10 H10B 107.8 2_556 . ?
C9 C10 H10B 107.8 . . ?
H10A C10 H10B 107.2 . . ?
C9 C11 C12 120.8(3) . . ?
C9 C11 H11A 119.6 . . ?
C12 C11 H11A 119.6 . . ?
N2 C12 C11 119.8(3) . . ?
N2 C12 H12A 120.1 . . ?
C11 C12 H12A 120.1 . . ?
C14 C13 N3 121.9(3) . . ?
C14 C13 H13A 119.1 . . ?
N3 C13 H13A 119.1 . . ?
C13 C14 C15 120.9(3) . . ?
C13 C14 H14A 119.6 . . ?
C15 C14 H14A 119.6 . . ?
C17 C15 C14 116.3(3) . . ?
C17 C15 C16 124.5(3) . . ?
C14 C15 C16 119.2(3) . . ?
C15 C16 C16 114.4(4) . 2_666 ?
C15 C16 H16A 108.7 . . ?
C16 C16 H16A 108.7 2_666 . ?
C15 C16 H16B 108.7 . . ?
C16 C16 H16B 108.7 2_666 . ?
H16A C16 H16B 107.6 . . ?
C15 C17 C18 121.5(3) . . ?
C15 C17 H17A 119.3 . . ?
C18 C17 H17A 119.3 . . ?
N3 C18 C17 120.2(3) . . ?
N3 C18 H18A 119.9 . . ?
C17 C18 H18A 119.9 . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.065

# Attachment 'last-3.cif'

data_last-3
_database_code_depnum_ccdc_archive 'CCDC 691373'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C84 H76 B2 Mn N6 O6'
_chemical_formula_weight         1342.07

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'
B B 0.0013 0.0007 '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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   9.99890(10)
_cell_length_b                   23.9270(3)
_cell_length_c                   15.1820(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.3545(5)
_cell_angle_gamma                90.00
_cell_volume                     3631.18(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    37990
_cell_measurement_theta_min      3.395
_cell_measurement_theta_max      27.485

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1410
_exptl_absorpt_coefficient_mu    0.240
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.885
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean 0.76
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            61562
_diffrn_reflns_av_R_equivalents  0.0726
_diffrn_reflns_av_sigmaI/netI    0.0684
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.44
_diffrn_reflns_theta_max         27.52
_reflns_number_total             8301
_reflns_number_gt                4239
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_publ_section_references         
;
collect:
"Collect" data collection software, Nonius B.V., Delft, The Netherlands, 1998.

HKL Scalepack & HKL Denzo:
Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected
in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular
Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet,
Eds., Academic Press.

absorption correction:
R.H. Blessing (1995) Acta Cryst. A51, 33-37.
R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426.

maXus:
S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland
maXus: a computer program for the solution and refinement of crystal
structures from diffraction data, University of Glasgow, Scotland, UK,
Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama,
Japan (1998).

Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray
Instruments Inc., Madison, Wisconsin, USA.

Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen,
Germany.
;

_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)+(0.0533P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8301
_refine_ls_number_parameters     448
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1027
_refine_ls_R_factor_gt           0.0398
_refine_ls_wR_factor_ref         0.1028
_refine_ls_wR_factor_gt          0.0907
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_restrained_S_all      0.909
_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
Mn1 Mn 0.0000 0.5000 0.0000 0.04406(12) Uani 1 2 d S . .
O1 O 0.18969(11) 0.52973(6) -0.04445(7) 0.0638(3) Uani 1 1 d . . .
O2 O 0.96418(11) 0.57677(5) 0.06432(8) 0.0650(3) Uani 1 1 d . . .
O3 O -0.11407(11) 0.52368(5) -0.12113(6) 0.0566(3) Uani 1 1 d . . .
N1 N 0.24328(13) 0.57240(7) 0.00137(9) 0.0532(4) Uani 1 1 d . . .
N2 N 0.85978(14) 0.61115(6) 0.06694(9) 0.0519(4) Uani 1 1 d . . .
N3 N -0.08872(13) 0.51102(5) -0.20439(8) 0.0470(3) Uani 1 1 d . . .
B1 B 0.48036(18) 0.64478(9) -0.33259(13) 0.0517(5) Uani 1 1 d . . .
C1 C 0.33192(17) 0.56237(8) 0.06609(13) 0.0640(5) Uani 1 1 d . . .
H1A H 0.3563 0.5258 0.0796 0.077 Uiso 1 1 calc R . .
C2 C 0.38706(19) 0.60563(8) 0.11254(13) 0.0676(5) Uani 1 1 d . . .
H2A H 0.4484 0.5978 0.1579 0.081 Uiso 1 1 calc R . .
C3 C 0.35557(16) 0.66008(8) 0.09488(11) 0.0534(4) Uani 1 1 d . . .
C4 C 0.26242(19) 0.66847(9) 0.02830(14) 0.0709(6) Uani 1 1 d . . .
H4A H 0.2363 0.7047 0.0140 0.085 Uiso 1 1 calc R . .
C5 C 0.20738(18) 0.62467(9) -0.01743(13) 0.0696(5) Uani 1 1 d . . .
H5A H 0.1442 0.6314 -0.0621 0.083 Uiso 1 1 calc R . .
C6 C 0.42660(18) 0.70825(8) 0.13936(13) 0.0670(5) Uani 1 1 d . . .
H6A H 0.4615 0.6964 0.1965 0.080 Uiso 1 1 calc R . .
H6B H 0.3638 0.7385 0.1484 0.080 Uiso 1 1 calc R . .
C7 C 0.54206(18) 0.72911(7) 0.08284(13) 0.0645(5) Uani 1 1 d . . .
H7A H 0.5074 0.7380 0.0243 0.077 Uiso 1 1 calc R . .
H7B H 0.5781 0.7632 0.1085 0.077 Uiso 1 1 calc R . .
C8 C 0.65277(17) 0.68706(7) 0.07551(12) 0.0545(4) Uani 1 1 d . . .
C9 C 0.66389(18) 0.65131(8) 0.00543(12) 0.0612(5) Uani 1 1 d . . .
H9A H 0.6004 0.6527 -0.0403 0.073 Uiso 1 1 calc R . .
C10 C 0.76687(18) 0.61362(8) 0.00148(12) 0.0612(5) Uani 1 1 d . . .
H10A H 0.7725 0.5897 -0.0466 0.073 Uiso 1 1 calc R . .
C11 C 0.74935(19) 0.68244(8) 0.14107(13) 0.0710(6) Uani 1 1 d . . .
H11A H 0.7451 0.7058 0.1899 0.085 Uiso 1 1 calc R . .
C12 C 0.85089(19) 0.64478(8) 0.13656(13) 0.0694(5) Uani 1 1 d . . .
H12A H 0.9143 0.6425 0.1822 0.083 Uiso 1 1 calc R . .
C13 C -0.19149(17) 0.50405(7) -0.26152(11) 0.0566(5) Uani 1 1 d . . .
H13A H -0.2788 0.5074 -0.2424 0.068 Uiso 1 1 calc R . .
C14 C -0.16829(19) 0.49201(8) -0.34844(11) 0.0630(5) Uani 1 1 d . . .
H14A H -0.2403 0.4873 -0.3876 0.076 Uiso 1 1 calc R . .
C15 C -0.03998(19) 0.48688(8) -0.37808(11) 0.0594(5) Uani 1 1 d . . .
C16 C -0.0122(2) 0.47487(9) -0.47401(11) 0.0758(6) Uani 1 1 d . . .
H16A H 0.0652 0.4506 -0.4770 0.091 Uiso 1 1 calc R . .
H16B H -0.0880 0.4550 -0.4999 0.091 Uiso 1 1 calc R . .
C17 C 0.06258(18) 0.49563(8) -0.31799(11) 0.0632(5) Uani 1 1 d . . .
H17A H 0.1506 0.4935 -0.3362 0.076 Uiso 1 1 calc R . .
C18 C 0.03737(17) 0.50752(7) -0.23146(10) 0.0569(5) Uani 1 1 d . . .
H18A H 0.1081 0.5132 -0.1916 0.068 Uiso 1 1 calc R . .
C19 C 0.64461(15) 0.64699(7) -0.33499(11) 0.0525(4) Uani 1 1 d . . .
C20 C 0.71606(16) 0.64616(7) -0.41266(13) 0.0612(5) Uani 1 1 d . . .
H20A H 0.6690 0.6476 -0.4662 0.073 Uiso 1 1 calc R . .
C21 C 0.85458(19) 0.64336(8) -0.41334(16) 0.0736(6) Uani 1 1 d . . .
H21A H 0.8983 0.6431 -0.4667 0.088 Uiso 1 1 calc R . .
C22 C 0.9270(2) 0.64103(8) -0.3363(2) 0.0834(7) Uani 1 1 d . . .
H22A H 1.0198 0.6391 -0.3370 0.100 Uiso 1 1 calc R . .
C23 C 0.8624(2) 0.64155(8) -0.25787(18) 0.0810(7) Uani 1 1 d . . .
H23A H 0.9111 0.6399 -0.2050 0.097 Uiso 1 1 calc R . .
C24 C 0.72357(17) 0.64451(8) -0.25753(13) 0.0680(5) Uani 1 1 d . . .
H24A H 0.6813 0.6449 -0.2036 0.082 Uiso 1 1 calc R . .
C25 C 0.44849(15) 0.57832(7) -0.31264(11) 0.0493(4) Uani 1 1 d . . .
C26 C 0.41212(15) 0.55717(8) -0.23121(11) 0.0568(5) Uani 1 1 d . . .
H26A H 0.3993 0.5822 -0.1853 0.068 Uiso 1 1 calc R . .
C27 C 0.39407(17) 0.50065(9) -0.21517(13) 0.0645(5) Uani 1 1 d . . .
H27A H 0.3703 0.4886 -0.1594 0.077 Uiso 1 1 calc R . .
C28 C 0.41109(17) 0.46254(9) -0.28123(14) 0.0670(5) Uani 1 1 d . . .
H28A H 0.3974 0.4247 -0.2712 0.080 Uiso 1 1 calc R . .
C29 C 0.44862(19) 0.48103(9) -0.36239(13) 0.0701(5) Uani 1 1 d . . .
H29A H 0.4616 0.4557 -0.4078 0.084 Uiso 1 1 calc R . .
C30 C 0.46705(17) 0.53738(9) -0.37644(12) 0.0635(5) Uani 1 1 d . . .
H30A H 0.4935 0.5488 -0.4319 0.076 Uiso 1 1 calc R . .
C31 C 0.41432(16) 0.66591(8) -0.42708(11) 0.0530(4) Uani 1 1 d . . .
C32 C 0.31336(19) 0.63935(9) -0.47396(13) 0.0772(6) Uani 1 1 d . . .
H32A H 0.2802 0.6059 -0.4521 0.093 Uiso 1 1 calc R . .
C33 C 0.2588(2) 0.65993(12) -0.55191(16) 0.1053(8) Uani 1 1 d . . .
H33A H 0.1903 0.6405 -0.5810 0.126 Uiso 1 1 calc R . .
C34 C 0.3056(3) 0.70890(13) -0.58624(15) 0.0987(8) Uani 1 1 d . . .
H34A H 0.2711 0.7224 -0.6395 0.118 Uiso 1 1 calc R . .
C35 C 0.4030(2) 0.73752(10) -0.54155(15) 0.0807(6) Uani 1 1 d . . .
H35A H 0.4343 0.7713 -0.5634 0.097 Uiso 1 1 calc R . .
C36 C 0.45550(18) 0.71624(8) -0.46331(13) 0.0655(5) Uani 1 1 d . . .
H36A H 0.5216 0.7366 -0.4335 0.079 Uiso 1 1 calc R . .
C37 C 0.41632(16) 0.68630(7) -0.25930(11) 0.0526(4) Uani 1 1 d . . .
C38 C 0.48291(19) 0.73152(9) -0.21982(12) 0.0676(5) Uani 1 1 d . . .
H38A H 0.5730 0.7368 -0.2311 0.081 Uiso 1 1 calc R . .
C39 C 0.4195(2) 0.76892(9) -0.16430(14) 0.0817(6) Uani 1 1 d . . .
H39A H 0.4677 0.7982 -0.1388 0.098 Uiso 1 1 calc R . .
C40 C 0.2866(3) 0.76269(10) -0.14713(13) 0.0823(7) Uani 1 1 d . . .
H40A H 0.2440 0.7876 -0.1100 0.099 Uiso 1 1 calc R . .
C41 C 0.2169(2) 0.71928(10) -0.18546(13) 0.0733(6) Uani 1 1 d . . .
H41A H 0.1261 0.7150 -0.1752 0.088 Uiso 1 1 calc R . .
C42 C 0.28121(17) 0.68214(8) -0.23904(12) 0.0594(5) Uani 1 1 d . . .
H42A H 0.2321 0.6526 -0.2631 0.071 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
Mn1 O2 2.1147(11) 3_665 ?
Mn1 O2 2.1147(11) 1_455 ?
Mn1 O1 2.1493(11) . ?
Mn1 O1 2.1493(11) 3_565 ?
Mn1 O3 2.2146(10) . ?
Mn1 O3 2.2146(10) 3_565 ?
O1 N1 1.3400(17) . ?
O2 N2 1.3304(16) . ?
O2 Mn1 2.1147(11) 1_655 ?
O3 N3 1.3301(15) . ?
N1 C1 1.329(2) . ?
N1 C5 1.330(2) . ?
N2 C12 1.333(2) . ?
N2 C10 1.345(2) . ?
N3 C18 1.338(2) . ?
N3 C13 1.339(2) . ?
B1 C37 1.634(3) . ?
B1 C19 1.644(2) . ?
B1 C31 1.645(2) . ?
B1 C25 1.651(3) . ?
C1 C2 1.362(2) . ?
C1 H1A 0.9300 . ?
C2 C3 1.366(2) . ?
C2 H2A 0.9300 . ?
C3 C4 1.373(2) . ?
C3 C6 1.505(2) . ?
C4 C5 1.366(3) . ?
C4 H4A 0.9300 . ?
C5 H5A 0.9300 . ?
C6 C7 1.538(2) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.502(2) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.372(2) . ?
C8 C11 1.375(2) . ?
C9 C10 1.371(2) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.360(2) . ?
C11 H11A 0.9300 . ?
C12 H12A 0.9300 . ?
C13 C14 1.376(2) . ?
C13 H13A 0.9300 . ?
C14 C15 1.375(2) . ?
C14 H14A 0.9300 . ?
C15 C17 1.372(2) . ?
C15 C16 1.517(2) . ?
C16 C16 1.462(4) 3_564 ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.373(2) . ?
C17 H17A 0.9300 . ?
C18 H18A 0.9300 . ?
C19 C20 1.393(2) . ?
C19 C24 1.402(2) . ?
C20 C21 1.387(2) . ?
C20 H20A 0.9300 . ?
C21 C22 1.362(3) . ?
C21 H21A 0.9300 . ?
C22 C23 1.368(3) . ?
C22 H22A 0.9300 . ?
C23 C24 1.390(3) . ?
C23 H23A 0.9300 . ?
C24 H24A 0.9300 . ?
C25 C26 1.392(2) . ?
C25 C30 1.393(2) . ?
C26 C27 1.387(2) . ?
C26 H26A 0.9300 . ?
C27 C28 1.369(3) . ?
C27 H27A 0.9300 . ?
C28 C29 1.370(3) . ?
C28 H28A 0.9300 . ?
C29 C30 1.378(3) . ?
C29 H29A 0.9300 . ?
C30 H30A 0.9300 . ?
C31 C32 1.377(2) . ?
C31 C36 1.390(2) . ?
C32 C33 1.382(3) . ?
C32 H32A 0.9300 . ?
C33 C34 1.369(3) . ?
C33 H33A 0.9300 . ?
C34 C35 1.359(3) . ?
C34 H34A 0.9300 . ?
C35 C36 1.384(3) . ?
C35 H35A 0.9300 . ?
C36 H36A 0.9300 . ?
C37 C42 1.396(2) . ?
C37 C38 1.398(2) . ?
C38 C39 1.392(3) . ?
C38 H38A 0.9300 . ?
C39 C40 1.369(3) . ?
C39 H39A 0.9300 . ?
C40 C41 1.372(3) . ?
C40 H40A 0.9300 . ?
C41 C42 1.375(3) . ?
C41 H41A 0.9300 . ?
C42 H42A 0.9300 . ?

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
O2 Mn1 O2 180.00(3) 3_665 1_455 ?
O2 Mn1 O1 88.98(5) 3_665 . ?
O2 Mn1 O1 91.02(5) 1_455 . ?
O2 Mn1 O1 91.02(5) 3_665 3_565 ?
O2 Mn1 O1 88.98(5) 1_455 3_565 ?
O1 Mn1 O1 180.0 . 3_565 ?
O2 Mn1 O3 85.89(4) 3_665 . ?
O2 Mn1 O3 94.11(4) 1_455 . ?
O1 Mn1 O3 95.49(4) . . ?
O1 Mn1 O3 84.51(4) 3_565 . ?
O2 Mn1 O3 94.11(4) 3_665 3_565 ?
O2 Mn1 O3 85.89(4) 1_455 3_565 ?
O1 Mn1 O3 84.51(4) . 3_565 ?
O1 Mn1 O3 95.49(4) 3_565 3_565 ?
O3 Mn1 O3 180.00(6) . 3_565 ?
N1 O1 Mn1 115.73(8) . . ?
N2 O2 Mn1 133.82(9) . 1_655 ?
N3 O3 Mn1 128.68(9) . . ?
C1 N1 C5 120.01(16) . . ?
C1 N1 O1 119.84(16) . . ?
C5 N1 O1 120.15(15) . . ?
O2 N2 C12 117.65(15) . . ?
O2 N2 C10 122.26(14) . . ?
C12 N2 C10 120.08(15) . . ?
O3 N3 C18 120.55(13) . . ?
O3 N3 C13 118.90(13) . . ?
C18 N3 C13 120.50(14) . . ?
C37 B1 C19 113.78(14) . . ?
C37 B1 C31 104.56(13) . . ?
C19 B1 C31 110.58(13) . . ?
C37 B1 C25 112.35(14) . . ?
C19 B1 C25 103.42(13) . . ?
C31 B1 C25 112.38(14) . . ?
N1 C1 C2 120.02(18) . . ?
N1 C1 H1A 120.0 . . ?
C2 C1 H1A 120.0 . . ?
C1 C2 C3 122.34(17) . . ?
C1 C2 H2A 118.8 . . ?
C3 C2 H2A 118.8 . . ?
C2 C3 C4 115.68(17) . . ?
C2 C3 C6 122.57(17) . . ?
C4 C3 C6 121.53(17) . . ?
C5 C4 C3 121.35(18) . . ?
C5 C4 H4A 119.3 . . ?
C3 C4 H4A 119.3 . . ?
N1 C5 C4 120.60(17) . . ?
N1 C5 H5A 119.7 . . ?
C4 C5 H5A 119.7 . . ?
C3 C6 C7 110.53(15) . . ?
C3 C6 H6A 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
C8 C7 C6 112.84(15) . . ?
C8 C7 H7A 109.0 . . ?
C6 C7 H7A 109.0 . . ?
C8 C7 H7B 109.0 . . ?
C6 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C9 C8 C11 116.30(16) . . ?
C9 C8 C7 123.27(17) . . ?
C11 C8 C7 120.43(16) . . ?
C10 C9 C8 121.25(17) . . ?
C10 C9 H9A 119.4 . . ?
C8 C9 H9A 119.4 . . ?
N2 C10 C9 120.18(16) . . ?
N2 C10 H10A 119.9 . . ?
C9 C10 H10A 119.9 . . ?
C12 C11 C8 121.94(17) . . ?
C12 C11 H11A 119.0 . . ?
C8 C11 H11A 119.0 . . ?
N2 C12 C11 120.24(18) . . ?
N2 C12 H12A 119.9 . . ?
C11 C12 H12A 119.9 . . ?
N3 C13 C14 120.20(16) . . ?
N3 C13 H13A 119.9 . . ?
C14 C13 H13A 119.9 . . ?
C15 C14 C13 120.82(17) . . ?
C15 C14 H14A 119.6 . . ?
C13 C14 H14A 119.6 . . ?
C17 C15 C14 117.21(15) . . ?
C17 C15 C16 121.09(17) . . ?
C14 C15 C16 121.63(17) . . ?
C16 C16 C15 113.5(2) 3_564 . ?
C16 C16 H16A 108.9 3_564 . ?
C15 C16 H16A 108.9 . . ?
C16 C16 H16B 108.9 3_564 . ?
C15 C16 H16B 108.9 . . ?
H16A C16 H16B 107.7 . . ?
C15 C17 C18 121.08(16) . . ?
C15 C17 H17A 119.5 . . ?
C18 C17 H17A 119.5 . . ?
N3 C18 C17 120.16(16) . . ?
N3 C18 H18A 119.9 . . ?
C17 C18 H18A 119.9 . . ?
C20 C19 C24 114.80(15) . . ?
C20 C19 B1 123.41(15) . . ?
C24 C19 B1 121.53(15) . . ?
C21 C20 C19 122.62(18) . . ?
C21 C20 H20A 118.7 . . ?
C19 C20 H20A 118.7 . . ?
C22 C21 C20 120.4(2) . . ?
C22 C21 H21A 119.8 . . ?
C20 C21 H21A 119.8 . . ?
C21 C22 C23 119.66(19) . . ?
C21 C22 H22A 120.2 . . ?
C23 C22 H22A 120.2 . . ?
C22 C23 C24 119.7(2) . . ?
C22 C23 H23A 120.1 . . ?
C24 C23 H23A 120.1 . . ?
C23 C24 C19 122.8(2) . . ?
C23 C24 H24A 118.6 . . ?
C19 C24 H24A 118.6 . . ?
C26 C25 C30 113.80(16) . . ?
C26 C25 B1 124.66(16) . . ?
C30 C25 B1 121.34(15) . . ?
C27 C26 C25 123.26(17) . . ?
C27 C26 H26A 118.4 . . ?
C25 C26 H26A 118.4 . . ?
C28 C27 C26 120.13(18) . . ?
C28 C27 H27A 119.9 . . ?
C26 C27 H27A 119.9 . . ?
C27 C28 C29 119.02(19) . . ?
C27 C28 H28A 120.5 . . ?
C29 C28 H28A 120.5 . . ?
C28 C29 C30 119.72(19) . . ?
C28 C29 H29A 120.1 . . ?
C30 C29 H29A 120.1 . . ?
C29 C30 C25 124.05(17) . . ?
C29 C30 H30A 118.0 . . ?
C25 C30 H30A 118.0 . . ?
C32 C31 C36 114.57(17) . . ?
C32 C31 B1 125.69(16) . . ?
C36 C31 B1 119.65(16) . . ?
C31 C32 C33 123.2(2) . . ?
C31 C32 H32A 118.4 . . ?
C33 C32 H32A 118.4 . . ?
C34 C33 C32 120.0(2) . . ?
C34 C33 H33A 120.0 . . ?
C32 C33 H33A 120.0 . . ?
C35 C34 C33 119.2(2) . . ?
C35 C34 H34A 120.4 . . ?
C33 C34 H34A 120.4 . . ?
C34 C35 C36 119.7(2) . . ?
C34 C35 H35A 120.1 . . ?
C36 C35 H35A 120.1 . . ?
C35 C36 C31 123.25(19) . . ?
C35 C36 H36A 118.4 . . ?
C31 C36 H36A 118.4 . . ?
C42 C37 C38 114.48(16) . . ?
C42 C37 B1 120.23(16) . . ?
C38 C37 B1 124.91(15) . . ?
C39 C38 C37 122.55(19) . . ?
C39 C38 H38A 118.7 . . ?
C37 C38 H38A 118.7 . . ?
C40 C39 C38 120.2(2) . . ?
C40 C39 H39A 119.9 . . ?
C38 C39 H39A 119.9 . . ?
C39 C40 C41 119.2(2) . . ?
C39 C40 H40A 120.4 . . ?
C41 C40 H40A 120.4 . . ?
C40 C41 C42 120.0(2) . . ?
C40 C41 H41A 120.0 . . ?
C42 C41 H41A 120.0 . . ?
C41 C42 C37 123.57(19) . . ?
C41 C42 H42A 118.2 . . ?
C37 C42 H42A 118.2 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.183
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.034

# Attachment 'last-4.cif'

data_last-4
_database_code_depnum_ccdc_archive 'CCDC 691374'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C84 H76 B2 Co N6 O6'
_chemical_formula_weight         1346.06

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'
B B 0.0013 0.0007 '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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   9.72030(10)
_cell_length_b                   25.4382(4)
_cell_length_c                   14.5710(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.7020(10)
_cell_angle_gamma                90.00
_cell_volume                     3595.41(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    36481
_cell_measurement_theta_min      3.395
_cell_measurement_theta_max      27.485

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1414
_exptl_absorpt_coefficient_mu    0.298
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean 0.76
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            52358
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.43
_diffrn_reflns_theta_max         27.52
_reflns_number_total             8249
_reflns_number_gt                4824
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_publ_section_references         
;
collect:
"Collect" data collection software, Nonius B.V., Delft, The Netherlands, 1998.

HKL Scalepack & HKL Denzo:
Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected
in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular
Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet,
Eds., Academic Press.

absorption correction:
R.H. Blessing (1995) Acta Cryst. A51, 33-37.
R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426.

maXus:
S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland
maXus: a computer program for the solution and refinement of crystal
structures from diffraction data, University of Glasgow, Scotland, UK,
Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama,
Japan (1998).

Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray
Instruments Inc., Madison, Wisconsin, USA.

Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen,
Germany.
;

_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)+(0.0510P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8249
_refine_ls_number_parameters     448
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0391
_refine_ls_wR_factor_ref         0.0995
_refine_ls_wR_factor_gt          0.0900
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_restrained_S_all      0.959
_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 0.5000 0.03917(10) Uani 1 2 d S . .
B1 B 0.4939(2) 0.14585(8) 0.14476(13) 0.0469(5) Uani 1 1 d . . .
N1 N 0.16112(15) 0.09790(5) 0.57097(8) 0.0462(3) Uani 1 1 d . . .
N2 N 0.76466(14) 0.07212(5) 0.55498(8) 0.0424(3) Uani 1 1 d . . .
N3 N 0.01825(14) 0.03633(5) 0.30937(8) 0.0409(3) Uani 1 1 d . . .
O1 O 0.07339(13) 0.05951(4) 0.58902(7) 0.0550(3) Uani 1 1 d . . .
O2 O 0.80481(12) 0.02337(4) 0.53645(7) 0.0520(3) Uani 1 1 d . . .
O3 O 0.00698(12) 0.05427(4) 0.39482(6) 0.0499(3) Uani 1 1 d . . .
C1 C 0.26472(18) 0.09020(7) 0.51613(10) 0.0501(4) Uani 1 1 d . . .
H1A H 0.2760 0.0576 0.4888 0.060 Uiso 1 1 calc R . .
C2 C 0.35417(18) 0.13039(7) 0.50028(11) 0.0523(4) Uani 1 1 d . . .
H2A H 0.4243 0.1247 0.4610 0.063 Uiso 1 1 calc R . .
C3 C 0.34303(18) 0.17921(6) 0.54114(11) 0.0487(4) Uani 1 1 d . . .
C4 C 0.2350(2) 0.18521(7) 0.59621(12) 0.0622(5) Uani 1 1 d . . .
H4A H 0.2224 0.2174 0.6249 0.075 Uiso 1 1 calc R . .
C5 C 0.1449(2) 0.14489(7) 0.61003(12) 0.0635(5) Uani 1 1 d . . .
H5A H 0.0717 0.1503 0.6470 0.076 Uiso 1 1 calc R . .
C6 C 0.44529(19) 0.22251(6) 0.52843(12) 0.0579(5) Uani 1 1 d . . .
H6A H 0.3999 0.2561 0.5354 0.069 Uiso 1 1 calc R . .
H6B H 0.4755 0.2208 0.4664 0.069 Uiso 1 1 calc R . .
C7 C 0.57228(19) 0.21969(6) 0.59694(12) 0.0582(5) Uani 1 1 d . . .
H7A H 0.6323 0.2493 0.5868 0.070 Uiso 1 1 calc R . .
H7B H 0.5428 0.2222 0.6591 0.070 Uiso 1 1 calc R . .
C8 C 0.65088(17) 0.16951(6) 0.58685(11) 0.0467(4) Uani 1 1 d . . .
C9 C 0.7257(2) 0.15977(7) 0.51168(12) 0.0612(5) Uani 1 1 d . . .
H9A H 0.7384 0.1868 0.4701 0.073 Uiso 1 1 calc R . .
C10 C 0.78181(19) 0.11158(7) 0.49620(11) 0.0582(5) Uani 1 1 d . . .
H10A H 0.8319 0.1062 0.4448 0.070 Uiso 1 1 calc R . .
C11 C 0.6442(2) 0.12873(7) 0.64827(11) 0.0563(5) Uani 1 1 d . . .
H11A H 0.6003 0.1339 0.7024 0.068 Uiso 1 1 calc R . .
C12 C 0.70084(19) 0.08066(7) 0.63163(11) 0.0553(5) Uani 1 1 d . . .
H12A H 0.6946 0.0537 0.6743 0.066 Uiso 1 1 calc R . .
C13 C -0.09376(19) 0.02043(8) 0.26015(11) 0.0627(5) Uani 1 1 d . . .
H13A H -0.1787 0.0208 0.2860 0.075 Uiso 1 1 calc R . .
C14 C -0.0849(2) 0.00357(8) 0.17166(12) 0.0682(6) Uani 1 1 d . . .
H14A H -0.1641 -0.0078 0.1382 0.082 Uiso 1 1 calc R . .
C15 C 0.03919(19) 0.00314(6) 0.13112(10) 0.0505(4) Uani 1 1 d . . .
C16 C 0.0509(2) -0.01238(8) 0.03257(11) 0.0700(6) Uani 1 1 d . . .
H16A H 0.1425 -0.0034 0.0149 0.084 Uiso 1 1 calc R . .
H16B H 0.0411 -0.0502 0.0276 0.084 Uiso 1 1 calc R . .
C17 C 0.15221(18) 0.01986(7) 0.18460(10) 0.0489(4) Uani 1 1 d . . .
H17A H 0.2382 0.0202 0.1601 0.059 Uiso 1 1 calc R . .
C18 C 0.14049(17) 0.03599(6) 0.27273(10) 0.0447(4) Uani 1 1 d . . .
H18A H 0.2186 0.0469 0.3078 0.054 Uiso 1 1 calc R . .
C19 C 0.56397(18) 0.18997(7) 0.21501(10) 0.0487(4) Uani 1 1 d . . .
C20 C 0.4991(2) 0.23560(7) 0.24346(11) 0.0594(5) Uani 1 1 d . . .
H20A H 0.4067 0.2409 0.2251 0.071 Uiso 1 1 calc R . .
C21 C 0.5675(3) 0.27333(8) 0.29812(13) 0.0717(6) Uani 1 1 d . . .
H21A H 0.5201 0.3028 0.3167 0.086 Uiso 1 1 calc R . .
C22 C 0.7047(3) 0.26730(9) 0.32484(13) 0.0780(7) Uani 1 1 d . . .
H22A H 0.7506 0.2925 0.3615 0.094 Uiso 1 1 calc R . .
C23 C 0.7728(2) 0.22369(9) 0.29674(12) 0.0740(6) Uani 1 1 d . . .
H23A H 0.8662 0.2195 0.3134 0.089 Uiso 1 1 calc R . .
C24 C 0.70364(19) 0.18605(8) 0.24396(11) 0.0596(5) Uani 1 1 d . . .
H24A H 0.7521 0.1565 0.2267 0.071 Uiso 1 1 calc R . .
C25 C 0.52289(17) 0.08601(7) 0.18402(12) 0.0498(4) Uani 1 1 d . . .
C26 C 0.51199(19) 0.04141(8) 0.12815(14) 0.0629(5) Uani 1 1 d . . .
H26A H 0.4934 0.0458 0.0652 0.076 Uiso 1 1 calc R . .
C27 C 0.5278(2) -0.00948(8) 0.16269(19) 0.0799(7) Uani 1 1 d . . .
H27A H 0.5217 -0.0382 0.1230 0.096 Uiso 1 1 calc R . .
C28 C 0.5524(2) -0.01700(9) 0.2555(2) 0.0896(8) Uani 1 1 d . . .
H28A H 0.5642 -0.0508 0.2791 0.108 Uiso 1 1 calc R . .
C29 C 0.5594(2) 0.02526(10) 0.31305(16) 0.0805(6) Uani 1 1 d . . .
H29A H 0.5731 0.0202 0.3762 0.097 Uiso 1 1 calc R . .
C30 C 0.54627(19) 0.07539(8) 0.27796(12) 0.0615(5) Uani 1 1 d . . .
H30A H 0.5533 0.1036 0.3187 0.074 Uiso 1 1 calc R . .
C31 C 0.32574(18) 0.14957(6) 0.13334(12) 0.0483(4) Uani 1 1 d . . .
C32 C 0.25049(19) 0.14262(7) 0.04958(13) 0.0593(5) Uani 1 1 d . . .
H32A H 0.2981 0.1383 -0.0032 0.071 Uiso 1 1 calc R . .
C33 C 0.1079(2) 0.14193(7) 0.04165(16) 0.0704(6) Uani 1 1 d . . .
H33A H 0.0622 0.1377 -0.0159 0.084 Uiso 1 1 calc R . .
C34 C 0.0337(2) 0.14734(7) 0.11745(19) 0.0752(6) Uani 1 1 d . . .
H34A H -0.0621 0.1466 0.1120 0.090 Uiso 1 1 calc R . .
C35 C 0.1025(2) 0.15390(7) 0.20176(17) 0.0698(6) Uani 1 1 d . . .
H35A H 0.0534 0.1577 0.2541 0.084 Uiso 1 1 calc R . .
C36 C 0.24565(19) 0.15491(6) 0.20891(13) 0.0583(5) Uani 1 1 d . . .
H36A H 0.2902 0.1594 0.2668 0.070 Uiso 1 1 calc R . .
C37 C 0.56422(17) 0.15823(7) 0.04676(11) 0.0485(4) Uani 1 1 d . . .
C38 C 0.66368(19) 0.12779(8) 0.00665(12) 0.0612(5) Uani 1 1 d . . .
H38A H 0.6894 0.0959 0.0340 0.073 Uiso 1 1 calc R . .
C39 C 0.7256(2) 0.14287(9) -0.07185(14) 0.0773(6) Uani 1 1 d . . .
H39A H 0.7908 0.1211 -0.0962 0.093 Uiso 1 1 calc R . .
C40 C 0.6922(2) 0.18920(11) -0.11378(13) 0.0804(7) Uani 1 1 d . . .
H40A H 0.7337 0.1992 -0.1668 0.097 Uiso 1 1 calc R . .
C41 C 0.5963(2) 0.22119(9) -0.07682(13) 0.0768(6) Uani 1 1 d . . .
H41A H 0.5736 0.2533 -0.1042 0.092 Uiso 1 1 calc R . .
C42 C 0.5334(2) 0.20542(8) 0.00150(12) 0.0646(5) Uani 1 1 d . . .
H42A H 0.4676 0.2274 0.0248 0.077 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 O3 2.0671(10) . ?
Co1 O3 2.0671(10) 3_556 ?
Co1 O1 2.0889(10) . ?
Co1 O1 2.0889(10) 3_556 ?
Co1 O2 2.0893(11) 3_656 ?
Co1 O2 2.0893(11) 1_455 ?
B1 C31 1.635(3) . ?
B1 C19 1.638(3) . ?
B1 C25 1.644(2) . ?
B1 C37 1.653(2) . ?
N1 O1 1.3338(16) . ?
N1 C5 1.338(2) . ?
N1 C1 1.340(2) . ?
N2 C12 1.3301(19) . ?
N2 O2 1.3331(15) . ?
N2 C10 1.3368(19) . ?
N3 C13 1.328(2) . ?
N3 C18 1.3337(19) . ?
N3 O3 1.3372(14) . ?
O2 Co1 2.0893(11) 1_655 ?
C1 C2 1.371(2) . ?
C1 H1A 0.9300 . ?
C2 C3 1.384(2) . ?
C2 H2A 0.9300 . ?
C3 C4 1.371(2) . ?
C3 C6 1.503(2) . ?
C4 C5 1.372(2) . ?
C4 H4A 0.9300 . ?
C5 H5A 0.9300 . ?
C6 C7 1.538(2) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.500(2) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C11 1.374(2) . ?
C8 C9 1.376(2) . ?
C9 C10 1.366(2) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.369(2) . ?
C11 H11A 0.9300 . ?
C12 H12A 0.9300 . ?
C13 C14 1.367(2) . ?
C13 H13A 0.9300 . ?
C14 C15 1.377(2) . ?
C14 H14A 0.9300 . ?
C15 C17 1.373(2) . ?
C15 C16 1.501(2) . ?
C16 C16 1.468(4) 3 ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.360(2) . ?
C17 H17A 0.9300 . ?
C18 H18A 0.9300 . ?
C19 C20 1.397(2) . ?
C19 C24 1.399(2) . ?
C20 C21 1.389(3) . ?
C20 H20A 0.9300 . ?
C21 C22 1.373(3) . ?
C21 H21A 0.9300 . ?
C22 C23 1.368(3) . ?
C22 H22A 0.9300 . ?
C23 C24 1.376(3) . ?
C23 H23A 0.9300 . ?
C24 H24A 0.9300 . ?
C25 C26 1.396(2) . ?
C25 C30 1.399(2) . ?
C26 C27 1.394(3) . ?
C26 H26A 0.9300 . ?
C27 C28 1.371(3) . ?
C27 H27A 0.9300 . ?
C28 C29 1.362(3) . ?
C28 H28A 0.9300 . ?
C29 C30 1.377(3) . ?
C29 H29A 0.9300 . ?
C30 H30A 0.9300 . ?
C31 C32 1.393(2) . ?
C31 C36 1.396(2) . ?
C32 C33 1.383(3) . ?
C32 H32A 0.9300 . ?
C33 C34 1.365(3) . ?
C33 H33A 0.9300 . ?
C34 C35 1.370(3) . ?
C34 H34A 0.9300 . ?
C35 C36 1.389(2) . ?
C35 H35A 0.9300 . ?
C36 H36A 0.9300 . ?
C37 C42 1.393(2) . ?
C37 C38 1.396(2) . ?
C38 C39 1.381(2) . ?
C38 H38A 0.9300 . ?
C39 C40 1.357(3) . ?
C39 H39A 0.9300 . ?
C40 C41 1.373(3) . ?
C40 H40A 0.9300 . ?
C41 C42 1.388(2) . ?
C41 H41A 0.9300 . ?
C42 H42A 0.9300 . ?

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
O3 Co1 O3 180.00(4) . 3_556 ?
O3 Co1 O1 87.14(4) . . ?
O3 Co1 O1 92.86(4) 3_556 . ?
O3 Co1 O1 92.86(4) . 3_556 ?
O3 Co1 O1 87.14(4) 3_556 3_556 ?
O1 Co1 O1 180.00(4) . 3_556 ?
O3 Co1 O2 85.86(4) . 3_656 ?
O3 Co1 O2 94.14(4) 3_556 3_656 ?
O1 Co1 O2 94.86(4) . 3_656 ?
O1 Co1 O2 85.14(4) 3_556 3_656 ?
O3 Co1 O2 94.14(4) . 1_455 ?
O3 Co1 O2 85.86(4) 3_556 1_455 ?
O1 Co1 O2 85.14(4) . 1_455 ?
O1 Co1 O2 94.86(4) 3_556 1_455 ?
O2 Co1 O2 180.0 3_656 1_455 ?
C31 B1 C19 113.38(14) . . ?
C31 B1 C25 103.71(13) . . ?
C19 B1 C25 111.22(14) . . ?
C31 B1 C37 111.57(14) . . ?
C19 B1 C37 103.34(13) . . ?
C25 B1 C37 113.93(14) . . ?
O1 N1 C5 118.43(14) . . ?
O1 N1 C1 121.69(13) . . ?
C5 N1 C1 119.88(15) . . ?
C12 N2 O2 118.72(12) . . ?
C12 N2 C10 119.97(14) . . ?
O2 N2 C10 121.24(12) . . ?
C13 N3 C18 120.17(14) . . ?
C13 N3 O3 119.55(13) . . ?
C18 N3 O3 120.24(13) . . ?
N1 O1 Co1 127.25(8) . . ?
N2 O2 Co1 126.78(9) . 1_655 ?
N3 O3 Co1 118.09(8) . . ?
N1 C1 C2 120.05(15) . . ?
N1 C1 H1A 120.0 . . ?
C2 C1 H1A 120.0 . . ?
C1 C2 C3 121.89(16) . . ?
C1 C2 H2A 119.1 . . ?
C3 C2 H2A 119.1 . . ?
C4 C3 C2 115.84(16) . . ?
C4 C3 C6 121.88(15) . . ?
C2 C3 C6 122.26(16) . . ?
C3 C4 C5 121.53(16) . . ?
C3 C4 H4A 119.2 . . ?
C5 C4 H4A 119.2 . . ?
N1 C5 C4 120.79(17) . . ?
N1 C5 H5A 119.6 . . ?
C4 C5 H5A 119.6 . . ?
C3 C6 C7 113.27(14) . . ?
C3 C6 H6A 108.9 . . ?
C7 C6 H6A 108.9 . . ?
C3 C6 H6B 108.9 . . ?
C7 C6 H6B 108.9 . . ?
H6A C6 H6B 107.7 . . ?
C8 C7 C6 111.64(14) . . ?
C8 C7 H7A 109.3 . . ?
C6 C7 H7A 109.3 . . ?
C8 C7 H7B 109.3 . . ?
C6 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
C11 C8 C9 115.59(15) . . ?
C11 C8 C7 122.20(15) . . ?
C9 C8 C7 122.02(15) . . ?
C10 C9 C8 122.02(16) . . ?
C10 C9 H9A 119.0 . . ?
C8 C9 H9A 119.0 . . ?
N2 C10 C9 120.02(15) . . ?
N2 C10 H10A 120.0 . . ?
C9 C10 H10A 120.0 . . ?
C12 C11 C8 121.51(15) . . ?
C12 C11 H11A 119.2 . . ?
C8 C11 H11A 119.2 . . ?
N2 C12 C11 120.61(15) . . ?
N2 C12 H12A 119.7 . . ?
C11 C12 H12A 119.7 . . ?
N3 C13 C14 120.38(17) . . ?
N3 C13 H13A 119.8 . . ?
C14 C13 H13A 119.8 . . ?
C13 C14 C15 121.16(17) . . ?
C13 C14 H14A 119.4 . . ?
C15 C14 H14A 119.4 . . ?
C17 C15 C14 116.44(15) . . ?
C17 C15 C16 121.16(17) . . ?
C14 C15 C16 122.35(17) . . ?
C16 C16 C15 114.62(19) 3 . ?
C16 C16 H16A 108.6 3 . ?
C15 C16 H16A 108.6 . . ?
C16 C16 H16B 108.6 3 . ?
C15 C16 H16B 108.6 . . ?
H16A C16 H16B 107.6 . . ?
C18 C17 C15 121.11(16) . . ?
C18 C17 H17A 119.4 . . ?
C15 C17 H17A 119.4 . . ?
N3 C18 C17 120.73(15) . . ?
N3 C18 H18A 119.6 . . ?
C17 C18 H18A 119.6 . . ?
C20 C19 C24 114.69(17) . . ?
C20 C19 B1 125.27(16) . . ?
C24 C19 B1 119.75(15) . . ?
C21 C20 C19 122.41(19) . . ?
C21 C20 H20A 118.8 . . ?
C19 C20 H20A 118.8 . . ?
C22 C21 C20 120.4(2) . . ?
C22 C21 H21A 119.8 . . ?
C20 C21 H21A 119.8 . . ?
C23 C22 C21 119.1(2) . . ?
C23 C22 H22A 120.5 . . ?
C21 C22 H22A 120.5 . . ?
C22 C23 C24 120.2(2) . . ?
C22 C23 H23A 119.9 . . ?
C24 C23 H23A 119.9 . . ?
C23 C24 C19 123.28(19) . . ?
C23 C24 H24A 118.4 . . ?
C19 C24 H24A 118.4 . . ?
C26 C25 C30 114.51(17) . . ?
C26 C25 B1 123.00(15) . . ?
C30 C25 B1 122.17(16) . . ?
C27 C26 C25 122.8(2) . . ?
C27 C26 H26A 118.6 . . ?
C25 C26 H26A 118.6 . . ?
C28 C27 C26 119.6(2) . . ?
C28 C27 H27A 120.2 . . ?
C26 C27 H27A 120.2 . . ?
C29 C28 C27 119.7(2) . . ?
C29 C28 H28A 120.1 . . ?
C27 C28 H28A 120.1 . . ?
C28 C29 C30 120.2(2) . . ?
C28 C29 H29A 119.9 . . ?
C30 C29 H29A 119.9 . . ?
C29 C30 C25 123.2(2) . . ?
C29 C30 H30A 118.4 . . ?
C25 C30 H30A 118.4 . . ?
C32 C31 C36 114.55(17) . . ?
C32 C31 B1 123.15(15) . . ?
C36 C31 B1 122.02(15) . . ?
C33 C32 C31 122.78(19) . . ?
C33 C32 H32A 118.6 . . ?
C31 C32 H32A 118.6 . . ?
C34 C33 C32 120.7(2) . . ?
C34 C33 H33A 119.7 . . ?
C32 C33 H33A 119.7 . . ?
C33 C34 C35 119.0(2) . . ?
C33 C34 H34A 120.5 . . ?
C35 C34 H34A 120.5 . . ?
C34 C35 C36 119.9(2) . . ?
C34 C35 H35A 120.1 . . ?
C36 C35 H35A 120.1 . . ?
C35 C36 C31 123.11(19) . . ?
C35 C36 H36A 118.4 . . ?
C31 C36 H36A 118.4 . . ?
C42 C37 C38 114.41(16) . . ?
C42 C37 B1 119.01(16) . . ?
C38 C37 B1 126.33(15) . . ?
C39 C38 C37 122.91(19) . . ?
C39 C38 H38A 118.5 . . ?
C37 C38 H38A 118.5 . . ?
C40 C39 C38 120.7(2) . . ?
C40 C39 H39A 119.7 . . ?
C38 C39 H39A 119.7 . . ?
C39 C40 C41 119.13(19) . . ?
C39 C40 H40A 120.4 . . ?
C41 C40 H40A 120.4 . . ?
C40 C41 C42 119.8(2) . . ?
C40 C41 H41A 120.1 . . ?
C42 C41 H41A 120.1 . . ?
C41 C42 C37 123.1(2) . . ?
C41 C42 H42A 118.5 . . ?
C37 C42 H42A 118.5 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.035


