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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            "[Co(TPTA)0.5(4,4'-bpy)0.5(H2O)2]n"
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H9 Co N O6'
_chemical_formula_sum            'C16 H13 Co N O6'
_chemical_formula_weight         374.20

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           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   18.905(4)
_cell_length_b                   11.646(2)
_cell_length_c                   15.432(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.81(3)
_cell_angle_gamma                90.00
_cell_volume                     3176.0(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3464
_cell_measurement_theta_min      2.0942
_cell_measurement_theta_max      27.9444

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1528
_exptl_absorpt_coefficient_mu    1.113
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8081
_exptl_absorpt_correction_T_max  0.8334
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  Saturn724
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            14441
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         25.49
_reflns_number_total             2912
_reflns_number_gt                2579
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0602P)²+16.9476P] 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         2912
_refine_ls_number_parameters     218
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0657
_refine_ls_wR_factor_ref         0.1441
_refine_ls_wR_factor_gt          0.1363
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_restrained_S_all      0.996
_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 0.22684(3) 0.33325(5) 0.14118(4) 0.0324(2) Uani 1 1 d . . .
O1 O 0.25091(18) 0.2979(3) 0.2772(2) 0.0384(8) Uani 1 1 d . . .
O2 O 0.3411(2) 0.1648(3) 0.3120(2) 0.0505(10) Uani 1 1 d . . .
O3 O 0.23101(18) 0.5675(3) 0.5194(2) 0.0379(8) Uani 1 1 d . . .
O4 O 0.3002(2) 0.5280(3) 0.6635(2) 0.0447(9) Uani 1 1 d . . .
O5 O 0.1360(2) 0.4430(3) 0.1435(3) 0.0501(9) Uani 1 1 d . . .
O6 O 0.31053(19) 0.2136(3) 0.1329(2) 0.0435(8) Uani 1 1 d . . .
N1 N 0.1435(2) 0.2091(3) 0.0874(3) 0.0357(9) Uani 1 1 d . . .
C1 C 0.3044(3) 0.2414(4) 0.3337(3) 0.0327(10) Uani 1 1 d . . .
C2 C 0.3241(2) 0.2718(4) 0.4343(3) 0.0283(9) Uani 1 1 d . . .
C3 C 0.2927(2) 0.3698(4) 0.4573(3) 0.0283(9) Uani 1 1 d . . .
H3 H 0.2580 0.4135 0.4111 0.034 Uiso 1 1 calc R . .
C4 C 0.3136(2) 0.4019(4) 0.5497(3) 0.0272(9) Uani 1 1 d . . .
C5 C 0.2802(2) 0.5057(4) 0.5784(3) 0.0319(10) Uani 1 1 d . . .
C6 C 0.3643(2) 0.3360(4) 0.6180(3) 0.0287(9) Uani 1 1 d . . .
H6A H 0.3778 0.3586 0.6796 0.034 Uiso 1 1 calc R . .
C7 C 0.3959(2) 0.2359(4) 0.5969(3) 0.0279(9) Uani 1 1 d . . .
C8 C 0.3756(2) 0.2062(4) 0.5040(3) 0.0296(9) Uani 1 1 d . . .
H8 H 0.3967 0.1411 0.4880 0.035 Uiso 1 1 calc R . .
C9 C 0.4494(2) 0.1683(4) 0.6737(3) 0.0276(9) Uani 1 1 d . . .
C10 C 0.5000 0.2257(5) 0.7500 0.0284(13) Uani 1 2 d S . .
H10 H 0.5000 0.3056 0.7500 0.034 Uiso 1 2 calc SR . .
C11 C 0.4506(3) 0.0490(4) 0.6745(3) 0.0365(11) Uani 1 1 d . . .
H11 H 0.4182 0.0082 0.6242 0.044 Uiso 1 1 calc R . .
C12 C 0.5000 -0.0094(6) 0.7500 0.0420(17) Uani 1 2 d S . .
H12 H 0.5000 -0.0893 0.7500 0.050 Uiso 1 2 calc SR . .
C13 C 0.1412(3) 0.1159(4) 0.1361(3) 0.0403(11) Uani 1 1 d . . .
H13 H 0.1790 0.1058 0.1938 0.048 Uiso 1 1 calc R . .
C14 C 0.0858(3) 0.0341(4) 0.1052(3) 0.0402(12) Uani 1 1 d . . .
H14 H 0.0859 -0.0286 0.1425 0.048 Uiso 1 1 calc R . .
C15 C 0.0296(2) 0.0445(4) 0.0184(3) 0.0351(10) Uani 1 1 d . . .
C16 C 0.0331(3) 0.1416(5) -0.0317(4) 0.0639(19) Uani 1 1 d . . .
H16 H -0.0031 0.1531 -0.0904 0.077 Uiso 1 1 calc R . .
C17 C 0.0891(3) 0.2202(5) 0.0042(4) 0.0616(18) Uani 1 1 d . . .
H17 H 0.0895 0.2850 -0.0308 0.074 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 O1 2.025(3) . ?
Co1 O4 2.077(3) 6_565 ?
Co1 N1 2.082(4) . ?
Co1 O6 2.146(3) . ?
Co1 O5 2.152(4) . ?
Co1 O3 2.232(3) 6_565 ?
Co1 C5 2.484(4) 6_565 ?
O1 C1 1.261(5) . ?
O2 C1 1.247(6) . ?
O3 C5 1.269(5) . ?
O3 Co1 2.232(3) 6_566 ?
O4 C5 1.258(5) . ?
O4 Co1 2.077(3) 6_566 ?
N1 C17 1.335(6) . ?
N1 C13 1.329(6) . ?
C1 C2 1.503(6) . ?
C2 C3 1.389(6) . ?
C2 C8 1.395(6) . ?
C3 C4 1.389(6) . ?
C3 H3 0.9300 . ?
C4 C6 1.380(6) . ?
C4 C5 1.501(6) . ?
C5 Co1 2.484(4) 6_566 ?
C6 C7 1.401(6) . ?
C6 H6A 0.9300 . ?
C7 C8 1.389(6) . ?
C7 C9 1.482(6) . ?
C8 H8 0.9300 . ?
C9 C11 1.391(6) . ?
C9 C10 1.395(5) . ?
C10 C9 1.395(5) 2_656 ?
C10 H10 0.9300 . ?
C11 C12 1.385(5) . ?
C11 H11 0.9300 . ?
C12 C11 1.385(5) 2_656 ?
C12 H12 0.9300 . ?
C13 C14 1.370(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.387(6) . ?
C14 H14 0.9300 . ?
C15 C16 1.385(7) . ?
C15 C15 1.484(9) 5 ?
C16 C17 1.359(7) . ?
C16 H16 0.9300 . ?
C17 H17 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 Co1 O4 95.50(13) . 6_565 ?
O1 Co1 N1 97.55(14) . . ?
O4 Co1 N1 166.59(14) 6_565 . ?
O1 Co1 O6 91.75(13) . . ?
O4 Co1 O6 92.96(14) 6_565 . ?
N1 Co1 O6 89.72(15) . . ?
O1 Co1 O5 89.44(14) . . ?
O4 Co1 O5 91.46(14) 6_565 . ?
N1 Co1 O5 85.61(15) . . ?
O6 Co1 O5 175.29(13) . . ?
O1 Co1 O3 156.32(12) . 6_565 ?
O4 Co1 O3 60.99(12) 6_565 6_565 ?
N1 Co1 O3 105.80(13) . 6_565 ?
O6 Co1 O3 92.22(13) . 6_565 ?
O5 Co1 O3 88.51(13) . 6_565 ?
O1 Co1 C5 125.80(14) . 6_565 ?
O4 Co1 C5 30.37(13) 6_565 6_565 ?
N1 Co1 C5 136.37(15) . 6_565 ?
O6 Co1 C5 93.24(14) . 6_565 ?
O5 Co1 C5 89.76(14) . 6_565 ?
O3 Co1 C5 30.62(12) 6_565 6_565 ?
C1 O1 Co1 130.8(3) . . ?
C5 O3 Co1 85.7(3) . 6_566 ?
C5 O4 Co1 93.0(3) . 6_566 ?
C17 N1 C13 117.0(4) . . ?
C17 N1 Co1 122.1(3) . . ?
C13 N1 Co1 120.9(3) . . ?
O2 C1 O1 124.9(4) . . ?
O2 C1 C2 119.3(4) . . ?
O1 C1 C2 115.8(4) . . ?
C3 C2 C8 119.8(4) . . ?
C3 C2 C1 119.0(4) . . ?
C8 C2 C1 121.1(4) . . ?
C4 C3 C2 119.5(4) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C6 C4 C3 120.1(4) . . ?
C6 C4 C5 118.3(4) . . ?
C3 C4 C5 121.6(4) . . ?
O4 C5 O3 120.3(4) . . ?
O4 C5 C4 118.2(4) . . ?
O3 C5 C4 121.5(4) . . ?
O4 C5 Co1 56.6(2) . 6_566 ?
O3 C5 Co1 63.6(2) . 6_566 ?
C4 C5 Co1 174.0(3) . 6_566 ?
C4 C6 C7 121.6(4) . . ?
C4 C6 H6A 119.2 . . ?
C7 C6 H6A 119.2 . . ?
C8 C7 C6 117.6(4) . . ?
C8 C7 C9 123.6(4) . . ?
C6 C7 C9 118.8(4) . . ?
C7 C8 C2 121.4(4) . . ?
C7 C8 H8 119.3 . . ?
C2 C8 H8 119.3 . . ?
C11 C9 C10 117.9(4) . . ?
C11 C9 C7 122.8(4) . . ?
C10 C9 C7 119.3(4) . . ?
C9 C10 C9 122.8(5) 2_656 . ?
C9 C10 H10 118.6 2_656 . ?
C9 C10 H10 118.6 . . ?
C12 C11 C9 120.1(4) . . ?
C12 C11 H11 119.9 . . ?
C9 C11 H11 119.9 . . ?
C11 C12 C11 121.2(6) 2_656 . ?
C11 C12 H12 119.4 2_656 . ?
C11 C12 H12 119.4 . . ?
N1 C13 C14 123.1(4) . . ?
N1 C13 H13 118.5 . . ?
C14 C13 H13 118.5 . . ?
C13 C14 C15 120.2(4) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C16 C15 C14 116.0(4) . . ?
C16 C15 C15 122.4(5) . 5 ?
C14 C15 C15 121.6(5) . 5 ?
C17 C16 C15 120.4(5) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
N1 C17 C16 123.3(5) . . ?
N1 C17 H17 118.4 . . ?
C16 C17 H17 118.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 Co1 O1 C1 -82.7(4) 6_565 . . . ?
N1 Co1 O1 C1 100.4(4) . . . . ?
O6 Co1 O1 C1 10.4(4) . . . . ?
O5 Co1 O1 C1 -174.1(4) . . . . ?
O3 Co1 O1 C1 -89.1(5) 6_565 . . . ?
C5 Co1 O1 C1 -84.8(4) 6_565 . . . ?
O1 Co1 N1 C17 154.6(5) . . . . ?
O4 Co1 N1 C17 -12.0(9) 6_565 . . . ?
O6 Co1 N1 C17 -113.7(5) . . . . ?
O5 Co1 N1 C17 65.7(5) . . . . ?
O3 Co1 N1 C17 -21.5(5) 6_565 . . . ?
C5 Co1 N1 C17 -19.3(6) 6_565 . . . ?
O1 Co1 N1 C13 -23.7(4) . . . . ?
O4 Co1 N1 C13 169.7(6) 6_565 . . . ?
O6 Co1 N1 C13 68.0(4) . . . . ?
O5 Co1 N1 C13 -112.6(4) . . . . ?
O3 Co1 N1 C13 160.2(4) 6_565 . . . ?
C5 Co1 N1 C13 162.4(3) 6_565 . . . ?
Co1 O1 C1 O2 -24.3(7) . . . . ?
Co1 O1 C1 C2 155.2(3) . . . . ?
O2 C1 C2 C3 168.8(4) . . . . ?
O1 C1 C2 C3 -10.8(6) . . . . ?
O2 C1 C2 C8 -8.5(7) . . . . ?
O1 C1 C2 C8 171.9(4) . . . . ?
C8 C2 C3 C4 0.7(6) . . . . ?
C1 C2 C3 C4 -176.7(4) . . . . ?
C2 C3 C4 C6 -0.9(6) . . . . ?
C2 C3 C4 C5 -178.9(4) . . . . ?
Co1 O4 C5 O3 0.8(5) 6_566 . . . ?
Co1 O4 C5 C4 -176.6(3) 6_566 . . . ?
Co1 O3 C5 O4 -0.8(4) 6_566 . . . ?
Co1 O3 C5 C4 176.5(4) 6_566 . . . ?
C6 C4 C5 O4 0.1(6) . . . . ?
C3 C4 C5 O4 178.1(4) . . . . ?
C6 C4 C5 O3 -177.2(4) . . . . ?
C3 C4 C5 O3 0.8(7) . . . . ?
C6 C4 C5 Co1 -29(3) . . . 6_566 ?
C3 C4 C5 Co1 149(3) . . . 6_566 ?
C3 C4 C6 C7 -0.1(7) . . . . ?
C5 C4 C6 C7 177.9(4) . . . . ?
C4 C6 C7 C8 1.3(6) . . . . ?
C4 C6 C7 C9 -179.3(4) . . . . ?
C6 C7 C8 C2 -1.6(6) . . . . ?
C9 C7 C8 C2 179.1(4) . . . . ?
C3 C2 C8 C7 0.6(7) . . . . ?
C1 C2 C8 C7 177.9(4) . . . . ?
C8 C7 C9 C11 -39.2(7) . . . . ?
C6 C7 C9 C11 141.5(5) . . . . ?
C8 C7 C9 C10 142.3(4) . . . . ?
C6 C7 C9 C10 -37.1(6) . . . . ?
C11 C9 C10 C9 -0.5(3) . . . 2_656 ?
C7 C9 C10 C9 178.1(4) . . . 2_656 ?
C10 C9 C11 C12 1.1(6) . . . . ?
C7 C9 C11 C12 -177.5(4) . . . . ?
C9 C11 C12 C11 -0.6(3) . . . 2_656 ?
C17 N1 C13 C14 -1.0(8) . . . . ?
Co1 N1 C13 C14 177.4(4) . . . . ?
N1 C13 C14 C15 1.8(8) . . . . ?
C13 C14 C15 C16 -1.2(8) . . . . ?
C13 C14 C15 C15 177.9(5) . . . 5 ?
C14 C15 C16 C17 0.0(9) . . . . ?
C15 C15 C16 C17 -179.1(6) 5 . . . ?
C13 N1 C17 C16 -0.3(10) . . . . ?
Co1 N1 C17 C16 -178.6(5) . . . . ?
C15 C16 C17 N1 0.8(11) . . . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        25.49
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.075
_database_code_depnum_ccdc_archive 'CCDC 1009774'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            "[Ni(TPTA)0.5(4,4'-bpy)0.5(H2O)2]n"
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H9 N Ni O6'
_chemical_formula_sum            'C16 H13 N Ni O6'
_chemical_formula_weight         373.98

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   18.937(4)
_cell_length_b                   11.546(2)
_cell_length_c                   15.385(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.08(3)
_cell_angle_gamma                90.00
_cell_volume                     3138.7(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4164
_cell_measurement_theta_min      2.1069
_cell_measurement_theta_max      28.2566

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    1.268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7946
_exptl_absorpt_correction_T_max  0.8228
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  Saturn724
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            14699
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.11
_diffrn_reflns_theta_max         25.50
_reflns_number_total             2871
_reflns_number_gt                2620
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0714P)²+5.5255P] 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         2871
_refine_ls_number_parameters     218
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0468
_refine_ls_wR_factor_ref         0.1205
_refine_ls_wR_factor_gt          0.1152
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.22552(2) 0.66735(3) 0.64006(3) 0.02736(17) Uani 1 1 d . . .
O1 O 0.24831(13) 0.7005(2) 0.77572(15) 0.0313(5) Uani 1 1 d . . .
O2 O 0.33923(17) 0.8337(2) 0.81009(17) 0.0447(7) Uani 1 1 d . . .
O3 O 0.22906(13) 0.4292(2) 1.02003(15) 0.0336(5) Uani 1 1 d . . .
O4 O 0.29851(13) 0.4704(2) 1.16433(15) 0.0359(6) Uani 1 1 d . . .
O5 O 0.13706(14) 0.5584(2) 0.64418(19) 0.0441(6) Uani 1 1 d . . .
O6 O 0.30870(13) 0.7809(2) 0.63214(16) 0.0376(6) Uani 1 1 d . . .
N1 N 0.14456(16) 0.7907(3) 0.58836(19) 0.0329(6) Uani 1 1 d . . .
C1 C 0.30197(18) 0.7571(3) 0.8319(2) 0.0272(7) Uani 1 1 d . . .
C2 C 0.32251(17) 0.7263(3) 0.9332(2) 0.0242(6) Uani 1 1 d . . .
C3 C 0.29119(17) 0.6279(3) 0.9569(2) 0.0260(7) Uani 1 1 d . . .
H3 H 0.2561 0.5840 0.9105 0.031 Uiso 1 1 calc R . .
C4 C 0.31212(16) 0.5951(3) 1.0495(2) 0.0251(6) Uani 1 1 d . . .
C5 C 0.27848(17) 0.4922(3) 1.0788(2) 0.0269(7) Uani 1 1 d . . .
C6 C 0.36389(17) 0.6622(3) 1.1183(2) 0.0250(7) Uani 1 1 d . . .
H6A H 0.3776 0.6400 1.1803 0.030 Uiso 1 1 calc R . .
C7 C 0.39554(16) 0.7617(3) 1.0967(2) 0.0240(6) Uani 1 1 d . . .
C8 C 0.37463(17) 0.7923(3) 1.0032(2) 0.0261(7) Uani 1 1 d . . .
H8 H 0.3958 0.8578 0.9871 0.031 Uiso 1 1 calc R . .
C9 C 0.44963(17) 0.8303(3) 1.1736(2) 0.0259(7) Uani 1 1 d . . .
C10 C 0.5000 0.7726(4) 1.2500 0.0259(9) Uani 1 2 d S . .
H10 H 0.5000 0.6921 1.2500 0.031 Uiso 1 2 calc SR . .
C11 C 0.45003(19) 0.9507(3) 1.1743(2) 0.0350(8) Uani 1 1 d . . .
H11 H 0.4168 0.9914 1.1240 0.042 Uiso 1 1 calc R . .
C12 C 0.5000 1.0107(4) 1.2500 0.0376(12) Uani 1 2 d S . .
H12 H 0.5000 1.0912 1.2500 0.045 Uiso 1 2 calc SR . .
C13 C 0.14228(19) 0.8849(3) 0.6366(2) 0.0344(8) Uani 1 1 d . . .
H13 H 0.1803 0.8957 0.6944 0.041 Uiso 1 1 calc R . .
C14 C 0.08677(19) 0.9669(3) 0.6053(2) 0.0358(8) Uani 1 1 d . . .
H14 H 0.0870 1.0306 0.6424 0.043 Uiso 1 1 calc R . .
C15 C 0.03024(18) 0.9553(3) 0.5188(2) 0.0323(7) Uani 1 1 d . . .
C16 C 0.0332(2) 0.8574(4) 0.4694(3) 0.0563(12) Uani 1 1 d . . .
H16 H -0.0037 0.8453 0.4109 0.068 Uiso 1 1 calc R . .
C17 C 0.0895(2) 0.7775(4) 0.5051(3) 0.0546(12) Uani 1 1 d . . .
H17 H 0.0896 0.7117 0.4703 0.065 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
Ni1 O1 2.010(2) . ?
Ni1 N1 2.033(3) . ?
Ni1 O4 2.051(2) 6_565 ?
Ni1 O6 2.087(3) . ?
Ni1 O5 2.114(3) . ?
Ni1 O3 2.178(2) 6_565 ?
Ni1 C5 2.442(3) 6_565 ?
O1 C1 1.255(4) . ?
O2 C1 1.251(4) . ?
O3 C5 1.270(4) . ?
O3 Ni1 2.178(2) 6_566 ?
O4 C5 1.257(4) . ?
O4 Ni1 2.051(2) 6_566 ?
N1 C17 1.338(5) . ?
N1 C13 1.326(5) . ?
C1 C2 1.507(4) . ?
C2 C3 1.389(5) . ?
C2 C8 1.396(4) . ?
C3 C4 1.387(4) . ?
C3 H3 0.9300 . ?
C4 C6 1.392(4) . ?
C4 C5 1.493(4) . ?
C5 Ni1 2.442(3) 6_566 ?
C6 C7 1.390(4) . ?
C6 H6A 0.9300 . ?
C7 C8 1.393(4) . ?
C7 C9 1.486(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.389(4) . ?
C9 C11 1.390(5) . ?
C10 C9 1.389(4) 2_657 ?
C10 H10 0.9300 . ?
C11 C12 1.392(4) . ?
C11 H11 0.9300 . ?
C12 C11 1.392(4) 2_657 ?
C12 H12 0.9300 . ?
C13 C14 1.367(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.382(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.375(5) . ?
C15 C15 1.495(6) 5_576 ?
C16 C17 1.366(5) . ?
C16 H16 0.9300 . ?
C17 H17 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 Ni1 N1 97.05(11) . . ?
O1 Ni1 O4 94.58(9) . 6_565 ?
N1 Ni1 O4 168.00(10) . 6_565 ?
O1 Ni1 O6 93.22(10) . . ?
N1 Ni1 O6 90.91(11) . . ?
O4 Ni1 O6 91.42(10) 6_565 . ?
O1 Ni1 O5 87.64(10) . . ?
N1 Ni1 O5 86.24(11) . . ?
O4 Ni1 O5 91.27(10) 6_565 . ?
O6 Ni1 O5 177.10(10) . . ?
O1 Ni1 O3 156.49(9) . 6_565 ?
N1 Ni1 O3 106.00(10) . 6_565 ?
O4 Ni1 O3 62.19(9) 6_565 6_565 ?
O6 Ni1 O3 91.04(9) . 6_565 ?
O5 Ni1 O3 89.26(10) . 6_565 ?
O1 Ni1 C5 125.43(10) . 6_565 ?
N1 Ni1 C5 137.20(11) . 6_565 ?
O4 Ni1 C5 30.94(10) 6_565 6_565 ?
O6 Ni1 C5 91.62(11) . 6_565 ?
O5 Ni1 C5 90.14(11) . 6_565 ?
O3 Ni1 C5 31.25(9) 6_565 6_565 ?
C1 O1 Ni1 129.3(2) . . ?
C5 O3 Ni1 85.92(18) . 6_566 ?
C5 O4 Ni1 91.98(19) . 6_566 ?
C17 N1 C13 117.2(3) . . ?
C17 N1 Ni1 120.9(2) . . ?
C13 N1 Ni1 121.8(2) . . ?
O2 C1 O1 125.3(3) . . ?
O2 C1 C2 119.0(3) . . ?
O1 C1 C2 115.7(3) . . ?
C3 C2 C8 119.7(3) . . ?
C3 C2 C1 119.2(3) . . ?
C8 C2 C1 121.1(3) . . ?
C4 C3 C2 120.1(3) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C6 119.5(3) . . ?
C3 C4 C5 122.2(3) . . ?
C6 C4 C5 118.3(3) . . ?
O4 C5 O3 119.9(3) . . ?
O4 C5 C4 118.3(3) . . ?
O3 C5 C4 121.7(3) . . ?
O4 C5 Ni1 57.08(16) . 6_566 ?
O3 C5 Ni1 62.83(16) . 6_566 ?
C4 C5 Ni1 174.9(2) . 6_566 ?
C4 C6 C7 121.6(3) . . ?
C4 C6 H6A 119.2 . . ?
C7 C6 H6A 119.2 . . ?
C6 C7 C8 118.0(3) . . ?
C6 C7 C9 118.9(3) . . ?
C8 C7 C9 123.1(3) . . ?
C2 C8 C7 121.1(3) . . ?
C2 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C10 C9 C11 118.2(3) . . ?
C10 C9 C7 119.0(3) . . ?
C11 C9 C7 122.7(3) . . ?
C9 C10 C9 122.7(4) 2_657 . ?
C9 C10 H10 118.7 2_657 . ?
C9 C10 H10 118.7 . . ?
C12 C11 C9 120.2(3) . . ?
C12 C11 H11 119.9 . . ?
C9 C11 H11 119.9 . . ?
C11 C12 C11 120.4(4) . 2_657 ?
C11 C12 H12 119.8 . . ?
C11 C12 H12 119.8 2_657 . ?
N1 C13 C14 123.2(3) . . ?
N1 C13 H13 118.4 . . ?
C14 C13 H13 118.4 . . ?
C13 C14 C15 120.2(3) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C16 C15 C14 116.1(3) . . ?
C16 C15 C15 122.1(4) . 5_576 ?
C14 C15 C15 121.8(4) . 5_576 ?
C17 C16 C15 120.9(4) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
N1 C17 C16 122.3(4) . . ?
N1 C17 H17 118.8 . . ?
C16 C17 H17 118.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Ni1 O1 C1 -100.3(3) . . . . ?
O4 Ni1 O1 C1 82.7(3) 6_565 . . . ?
O6 Ni1 O1 C1 -9.0(3) . . . . ?
O5 Ni1 O1 C1 173.8(3) . . . . ?
O3 Ni1 O1 C1 91.1(3) 6_565 . . . ?
C5 Ni1 O1 C1 85.3(3) 6_565 . . . ?
O1 Ni1 N1 C17 -152.4(3) . . . . ?
O4 Ni1 N1 C17 13.1(7) 6_565 . . . ?
O6 Ni1 N1 C17 114.2(3) . . . . ?
O5 Ni1 N1 C17 -65.3(3) . . . . ?
O3 Ni1 N1 C17 22.9(4) 6_565 . . . ?
C5 Ni1 N1 C17 20.9(4) 6_565 . . . ?
O1 Ni1 N1 C13 25.1(3) . . . . ?
O4 Ni1 N1 C13 -169.4(4) 6_565 . . . ?
O6 Ni1 N1 C13 -68.3(3) . . . . ?
O5 Ni1 N1 C13 112.2(3) . . . . ?
O3 Ni1 N1 C13 -159.6(3) 6_565 . . . ?
C5 Ni1 N1 C13 -161.6(3) 6_565 . . . ?
Ni1 O1 C1 O2 23.6(5) . . . . ?
Ni1 O1 C1 C2 -155.2(2) . . . . ?
O2 C1 C2 C3 -168.3(3) . . . . ?
O1 C1 C2 C3 10.6(4) . . . . ?
O2 C1 C2 C8 9.1(4) . . . . ?
O1 C1 C2 C8 -172.0(3) . . . . ?
C8 C2 C3 C4 -0.5(5) . . . . ?
C1 C2 C3 C4 177.0(3) . . . . ?
C2 C3 C4 C6 0.8(5) . . . . ?
C2 C3 C4 C5 178.2(3) . . . . ?
Ni1 O4 C5 O3 -0.6(3) 6_566 . . . ?
Ni1 O4 C5 C4 177.3(3) 6_566 . . . ?
Ni1 O3 C5 O4 0.6(3) 6_566 . . . ?
Ni1 O3 C5 C4 -177.3(3) 6_566 . . . ?
C3 C4 C5 O4 -177.6(3) . . . . ?
C6 C4 C5 O4 -0.2(4) . . . . ?
C3 C4 C5 O3 0.3(5) . . . . ?
C6 C4 C5 O3 177.7(3) . . . . ?
C3 C4 C5 Ni1 -151(2) . . . 6_566 ?
C6 C4 C5 Ni1 26(3) . . . 6_566 ?
C3 C4 C6 C7 -0.2(5) . . . . ?
C5 C4 C6 C7 -177.6(3) . . . . ?
C4 C6 C7 C8 -0.7(5) . . . . ?
C4 C6 C7 C9 179.1(3) . . . . ?
C3 C2 C8 C7 -0.4(5) . . . . ?
C1 C2 C8 C7 -177.8(3) . . . . ?
C6 C7 C8 C2 1.0(4) . . . . ?
C9 C7 C8 C2 -178.8(3) . . . . ?
C6 C7 C9 C10 37.3(4) . . . . ?
C8 C7 C9 C10 -142.9(3) . . . . ?
C6 C7 C9 C11 -140.1(3) . . . . ?
C8 C7 C9 C11 39.8(5) . . . . ?
C11 C9 C10 C9 0.0(2) . . . 2_657 ?
C7 C9 C10 C9 -177.5(3) . . . 2_657 ?
C10 C9 C11 C12 0.1(5) . . . . ?
C7 C9 C11 C12 177.4(3) . . . . ?
C9 C11 C12 C11 0.0(2) . . . 2_657 ?
C17 N1 C13 C14 0.4(6) . . . . ?
Ni1 N1 C13 C14 -177.2(3) . . . . ?
N1 C13 C14 C15 -1.5(6) . . . . ?
C13 C14 C15 C16 1.3(6) . . . . ?
C13 C14 C15 C15 -178.3(4) . . . 5_576 ?
C14 C15 C16 C17 -0.3(7) . . . . ?
C15 C15 C16 C17 179.4(5) 5_576 . . . ?
C13 N1 C17 C16 0.7(7) . . . . ?
Ni1 N1 C17 C16 178.3(4) . . . . ?
C15 C16 C17 N1 -0.7(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.076
_database_code_depnum_ccdc_archive 'CCDC 1009775'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            {[Mn2(TPTA)(2,2'-bpy)(H2O)]1.5H2O}n
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H18 Mn2 N2 O9'
_chemical_formula_sum            'C32 H23 Mn2 N2 O10.50'
_chemical_formula_weight         713.40

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'
Mn Mn 0.3368 0.7283 '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_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.7207(19)
_cell_length_b                   10.111(2)
_cell_length_c                   15.286(3)
_cell_angle_alpha                92.87(3)
_cell_angle_beta                 98.72(3)
_cell_angle_gamma                96.33(3)
_cell_volume                     1472.7(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3937
_cell_measurement_theta_min      2.0311
_cell_measurement_theta_max      28.0490

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             726
_exptl_absorpt_coefficient_mu    0.924
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8296
_exptl_absorpt_correction_T_max  0.8663
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  Saturn724
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            15427
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         25.50
_reflns_number_total             5412
_reflns_number_gt                4209
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0584P)²+0.8515P] 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         5412
_refine_ls_number_parameters     406
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0524
_refine_ls_wR_factor_ref         0.1299
_refine_ls_wR_factor_gt          0.1179
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.500 0.500 0.500 86.0 12.1
2 0.500 0.500 1.000 83.1 17.4
_platon_squeeze_details          
; ?
;
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 -0.03612(6) -0.52517(5) 0.83219(4) 0.02679(17) Uani 1 1 d . . .
Mn2 Mn -0.11066(5) 0.23339(5) 0.67532(3) 0.02517(16) Uani 1 1 d . . .
O1 O 0.1294(3) -0.3766(3) 0.91724(18) 0.0383(7) Uani 1 1 d . . .
O2 O -0.0350(3) -0.3094(3) 0.82244(18) 0.0461(8) Uani 1 1 d . . .
O3 O -0.0901(3) 0.1628(3) 0.80236(16) 0.0343(6) Uani 1 1 d . . .
O4 O 0.0421(3) 0.3128(3) 0.89909(18) 0.0398(7) Uani 1 1 d . . .
O5 O 0.2045(3) 0.5726(3) 1.27375(19) 0.0404(7) Uani 1 1 d . . .
O6 O 0.3439(3) 0.7442(3) 1.3366(2) 0.0498(8) Uani 1 1 d . . .
O7 O 0.8492(3) 0.7794(3) 1.30532(19) 0.0411(7) Uani 1 1 d . . .
O8 O 0.9406(2) 0.5952(3) 1.28053(17) 0.0331(6) Uani 1 1 d . . .
O9 O -0.1783(4) -0.5109(5) 0.9299(2) 0.0879(15) Uani 1 1 d . . .
N1 N -0.2112(3) 0.0366(3) 0.6104(2) 0.0315(7) Uani 1 1 d . . .
N2 N -0.0760(3) 0.2333(3) 0.5344(2) 0.0335(7) Uani 1 1 d . . .
C1 C 0.0660(4) -0.2835(4) 0.8849(2) 0.0306(9) Uani 1 1 d . . .
C2 C 0.1107(4) -0.1429(3) 0.9187(2) 0.0263(8) Uani 1 1 d . . .
C3 C 0.0395(4) -0.0437(4) 0.8800(2) 0.0279(8) Uani 1 1 d . . .
H3 H -0.0353 -0.0658 0.8341 0.033 Uiso 1 1 calc R . .
C4 C 0.0799(4) 0.0871(3) 0.9096(2) 0.0267(8) Uani 1 1 d . . .
C5 C 0.0057(4) 0.1948(4) 0.8672(2) 0.0310(9) Uani 1 1 d . . .
C6 C 0.1908(4) 0.1179(4) 0.9778(2) 0.0299(8) Uani 1 1 d . . .
H6 H 0.2183 0.2069 0.9971 0.036 Uiso 1 1 calc R . .
C7 C 0.2635(4) 0.0202(3) 1.0192(2) 0.0263(8) Uani 1 1 d . . .
C8 C 0.2208(4) -0.1109(3) 0.9878(2) 0.0271(8) Uani 1 1 d . . .
H8 H 0.2668 -0.1786 1.0136 0.032 Uiso 1 1 calc R . .
C9 C 0.3829(4) 0.0583(3) 1.0917(2) 0.0261(8) Uani 1 1 d . . .
C10 C 0.4057(4) 0.1863(4) 1.1320(2) 0.0280(8) Uani 1 1 d . . .
H10 H 0.3405 0.2451 1.1160 0.034 Uiso 1 1 calc R . .
C11 C 0.5225(4) 0.2305(4) 1.1955(2) 0.0257(8) Uani 1 1 d . . .
C12 C 0.6164(4) 0.1410(4) 1.2216(3) 0.0324(9) Uani 1 1 d . . .
H12 H 0.6951 0.1678 1.2640 0.039 Uiso 1 1 calc R . .
C13 C 0.5925(4) 0.0126(4) 1.1845(3) 0.0375(10) Uani 1 1 d . . .
H13 H 0.6547 -0.0477 1.2032 0.045 Uiso 1 1 calc R . .
C14 C 0.4786(4) -0.0289(4) 1.1204(3) 0.0330(9) Uani 1 1 d . . .
H14 H 0.4654 -0.1163 1.0960 0.040 Uiso 1 1 calc R . .
C15 C 0.5434(4) 0.3713(3) 1.2311(2) 0.0251(8) Uani 1 1 d . . .
C16 C 0.4305(4) 0.4348(4) 1.2473(2) 0.0284(8) Uani 1 1 d . . .
H16 H 0.3413 0.3875 1.2384 0.034 Uiso 1 1 calc R . .
C17 C 0.4485(4) 0.5687(4) 1.2769(2) 0.0280(8) Uani 1 1 d . . .
C18 C 0.3260(4) 0.6331(4) 1.2966(2) 0.0296(8) Uani 1 1 d . . .
C19 C 0.5788(3) 0.6402(4) 1.2881(2) 0.0283(8) Uani 1 1 d . . .
H19 H 0.5900 0.7304 1.3062 0.034 Uiso 1 1 calc R . .
C20 C 0.6932(4) 0.5789(4) 1.2727(2) 0.0273(8) Uani 1 1 d . . .
C21 C 0.6749(4) 0.4442(4) 1.2454(2) 0.0275(8) Uani 1 1 d . . .
H21 H 0.7525 0.4021 1.2365 0.033 Uiso 1 1 calc R . .
C22 C 0.8340(4) 0.6581(4) 1.2864(2) 0.0292(8) Uani 1 1 d . . .
C23 C -0.2962(4) -0.0475(4) 0.6480(3) 0.0413(10) Uani 1 1 d . . .
H23 H -0.2926 -0.0380 0.7092 0.050 Uiso 1 1 calc R . .
C24 C -0.3879(6) -0.1462(5) 0.6012(3) 0.0612(14) Uani 1 1 d . . .
H24 H -0.4453 -0.2033 0.6299 0.073 Uiso 1 1 calc R . .
C25 C -0.3944(6) -0.1604(6) 0.5113(4) 0.0742(18) Uani 1 1 d . . .
H25 H -0.4564 -0.2273 0.4778 0.089 Uiso 1 1 calc R . .
C26 C -0.3085(6) -0.0748(5) 0.4711(3) 0.0616(15) Uani 1 1 d . . .
H26 H -0.3116 -0.0828 0.4099 0.074 Uiso 1 1 calc R . .
C27 C -0.2174(4) 0.0232(4) 0.5221(2) 0.0334(9) Uani 1 1 d . . .
C28 C -0.1258(4) 0.1224(4) 0.4828(2) 0.0310(9) Uani 1 1 d . . .
C29 C -0.0921(4) 0.1029(4) 0.3994(3) 0.0413(10) Uani 1 1 d . . .
H29 H -0.1248 0.0237 0.3653 0.050 Uiso 1 1 calc R . .
C30 C -0.0093(5) 0.2021(5) 0.3668(3) 0.0486(12) Uani 1 1 d . . .
H30 H 0.0130 0.1911 0.3101 0.058 Uiso 1 1 calc R . .
C31 C 0.0392(5) 0.3148(5) 0.4176(3) 0.0533(12) Uani 1 1 d . . .
H31 H 0.0939 0.3835 0.3963 0.064 Uiso 1 1 calc R . .
C32 C 0.0064(5) 0.3263(5) 0.5012(3) 0.0487(11) Uani 1 1 d . . .
H32 H 0.0434 0.4029 0.5370 0.058 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 O5 2.116(3) 2_557 ?
Mn1 O4 2.125(3) 1_545 ?
Mn1 O9 2.193(3) . ?
Mn1 O2 2.193(3) . ?
Mn1 O8 2.200(3) 2_657 ?
Mn1 O1 2.274(3) . ?
Mn2 O3 2.091(3) . ?
Mn2 N1 2.232(3) . ?
Mn2 N2 2.231(3) . ?
Mn2 O8 2.260(3) 2_667 ?
Mn2 O6 2.284(3) 2_567 ?
Mn2 O5 2.397(3) 2_567 ?
O1 C1 1.262(4) . ?
O2 C1 1.256(5) . ?
O3 C5 1.255(4) . ?
O4 C5 1.258(4) . ?
O4 Mn1 2.125(3) 1_565 ?
O5 C18 1.259(4) . ?
O5 Mn1 2.116(3) 2_557 ?
O5 Mn2 2.397(3) 2_567 ?
O6 C18 1.234(5) . ?
O6 Mn2 2.284(3) 2_567 ?
O7 C22 1.234(4) . ?
O8 C22 1.286(4) . ?
O8 Mn1 2.200(3) 2_657 ?
O8 Mn2 2.260(3) 2_667 ?
N1 C23 1.332(5) . ?
N1 C27 1.341(5) . ?
N2 C32 1.336(5) . ?
N2 C28 1.338(5) . ?
C1 C2 1.483(5) . ?
C2 C8 1.383(5) . ?
C2 C3 1.387(5) . ?
C3 C4 1.371(5) . ?
C3 H3 0.9300 . ?
C4 C6 1.378(5) . ?
C4 C5 1.493(5) . ?
C6 C7 1.398(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.384(5) . ?
C7 C9 1.481(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.385(5) . ?
C9 C14 1.390(5) . ?
C10 C11 1.393(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.386(5) . ?
C11 C15 1.480(5) . ?
C12 C13 1.372(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.374(5) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 C16 1.378(5) . ?
C15 C21 1.385(5) . ?
C16 C17 1.389(5) . ?
C16 H16 0.9300 . ?
C17 C19 1.370(5) . ?
C17 C18 1.480(5) . ?
C19 C20 1.376(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.388(5) . ?
C20 C22 1.487(5) . ?
C21 H21 0.9300 . ?
C23 C24 1.358(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.366(7) . ?
C24 H24 0.9300 . ?
C25 C26 1.369(7) . ?
C25 H25 0.9300 . ?
C26 C27 1.376(6) . ?
C26 H26 0.9300 . ?
C27 C28 1.479(5) . ?
C28 C29 1.374(5) . ?
C29 C30 1.376(6) . ?
C29 H29 0.9300 . ?
C30 C31 1.344(6) . ?
C30 H30 0.9300 . ?
C31 C32 1.366(6) . ?
C31 H31 0.9300 . ?
C32 H32 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
O5 Mn1 O4 116.95(11) 2_557 1_545 ?
O5 Mn1 O9 92.40(13) 2_557 . ?
O4 Mn1 O9 88.33(13) 1_545 . ?
O5 Mn1 O2 93.58(11) 2_557 . ?
O4 Mn1 O2 149.33(11) 1_545 . ?
O9 Mn1 O2 87.44(15) . . ?
O5 Mn1 O8 74.63(10) 2_557 2_657 ?
O4 Mn1 O8 86.57(11) 1_545 2_657 ?
O9 Mn1 O8 161.95(15) . 2_657 ?
O2 Mn1 O8 105.55(11) . 2_657 ?
O5 Mn1 O1 151.59(11) 2_557 . ?
O4 Mn1 O1 91.34(10) 1_545 . ?
O9 Mn1 O1 90.86(15) . . ?
O2 Mn1 O1 58.38(10) . . ?
O8 Mn1 O1 106.55(10) 2_657 . ?
O3 Mn2 N1 93.19(11) . . ?
O3 Mn2 N2 154.23(11) . . ?
N1 Mn2 N2 73.65(12) . . ?
O3 Mn2 O8 91.89(10) . 2_667 ?
N1 Mn2 O8 158.26(10) . 2_667 ?
N2 Mn2 O8 93.07(11) . 2_667 ?
O3 Mn2 O6 96.09(12) . 2_567 ?
N1 Mn2 O6 77.57(11) . 2_567 ?
N2 Mn2 O6 102.34(12) . 2_567 ?
O8 Mn2 O6 122.85(10) 2_667 2_567 ?
O3 Mn2 O5 91.18(11) . 2_567 ?
N1 Mn2 O5 132.61(10) . 2_567 ?
N2 Mn2 O5 114.13(11) . 2_567 ?
O8 Mn2 O5 68.33(9) 2_667 2_567 ?
O6 Mn2 O5 55.05(10) 2_567 2_567 ?
C1 O1 Mn1 88.7(2) . . ?
C1 O2 Mn1 92.5(2) . . ?
C5 O3 Mn2 128.8(2) . . ?
C5 O4 Mn1 120.4(2) . 1_565 ?
C18 O5 Mn1 145.1(3) . 2_557 ?
C18 O5 Mn2 89.1(2) . 2_567 ?
Mn1 O5 Mn2 92.90(10) 2_557 2_567 ?
C18 O6 Mn2 95.0(2) . 2_567 ?
C22 O8 Mn1 133.2(2) . 2_657 ?
C22 O8 Mn2 98.2(2) . 2_667 ?
Mn1 O8 Mn2 94.54(10) 2_657 2_667 ?
C23 N1 C27 118.3(3) . . ?
C23 N1 Mn2 123.3(3) . . ?
C27 N1 Mn2 115.5(3) . . ?
C32 N2 C28 117.5(3) . . ?
C32 N2 Mn2 125.1(3) . . ?
C28 N2 Mn2 116.6(3) . . ?
O2 C1 O1 119.9(3) . . ?
O2 C1 C2 119.3(3) . . ?
O1 C1 C2 120.8(3) . . ?
C8 C2 C3 120.4(3) . . ?
C8 C2 C1 120.8(3) . . ?
C3 C2 C1 118.8(3) . . ?
C4 C3 C2 119.8(3) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C6 119.3(3) . . ?
C3 C4 C5 120.1(3) . . ?
C6 C4 C5 120.6(3) . . ?
O3 C5 O4 123.7(3) . . ?
O3 C5 C4 118.4(3) . . ?
O4 C5 C4 117.9(3) . . ?
C4 C6 C7 122.4(3) . . ?
C4 C6 H6 118.8 . . ?
C7 C6 H6 118.8 . . ?
C8 C7 C6 117.1(3) . . ?
C8 C7 C9 122.5(3) . . ?
C6 C7 C9 120.4(3) . . ?
C7 C8 C2 121.0(3) . . ?
C7 C8 H8 119.5 . . ?
C2 C8 H8 119.5 . . ?
C10 C9 C14 117.1(3) . . ?
C10 C9 C7 120.3(3) . . ?
C14 C9 C7 122.6(3) . . ?
C9 C10 C11 122.6(3) . . ?
C9 C10 H10 118.7 . . ?
C11 C10 H10 118.7 . . ?
C12 C11 C10 118.4(3) . . ?
C12 C11 C15 122.5(3) . . ?
C10 C11 C15 119.1(3) . . ?
C13 C12 C11 119.6(3) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C12 C13 C14 121.4(4) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C13 C14 C9 120.8(3) . . ?
C13 C14 H14 119.6 . . ?
C9 C14 H14 119.6 . . ?
C16 C15 C21 118.3(3) . . ?
C16 C15 C11 120.4(3) . . ?
C21 C15 C11 121.2(3) . . ?
C15 C16 C17 120.7(3) . . ?
C15 C16 H16 119.6 . . ?
C17 C16 H16 119.6 . . ?
C19 C17 C16 120.1(3) . . ?
C19 C17 C18 120.4(3) . . ?
C16 C17 C18 119.5(3) . . ?
O6 C18 O5 120.6(3) . . ?
O6 C18 C17 119.9(3) . . ?
O5 C18 C17 119.6(3) . . ?
C17 C19 C20 120.2(3) . . ?
C17 C19 H19 119.9 . . ?
C20 C19 H19 119.9 . . ?
C19 C20 C21 119.3(3) . . ?
C19 C20 C22 119.3(3) . . ?
C21 C20 C22 121.4(3) . . ?
C15 C21 C20 121.3(3) . . ?
C15 C21 H21 119.3 . . ?
C20 C21 H21 119.3 . . ?
O7 C22 O8 120.7(3) . . ?
O7 C22 C20 121.5(3) . . ?
O8 C22 C20 117.7(3) . . ?
N1 C23 C24 123.0(4) . . ?
N1 C23 H23 118.5 . . ?
C24 C23 H23 118.5 . . ?
C23 C24 C25 118.9(5) . . ?
C23 C24 H24 120.6 . . ?
C25 C24 H24 120.6 . . ?
C24 C25 C26 119.1(5) . . ?
C24 C25 H25 120.4 . . ?
C26 C25 H25 120.4 . . ?
C25 C26 C27 119.3(4) . . ?
C25 C26 H26 120.3 . . ?
C27 C26 H26 120.3 . . ?
N1 C27 C26 121.4(4) . . ?
N1 C27 C28 116.3(3) . . ?
C26 C27 C28 122.2(4) . . ?
N2 C28 C29 121.6(4) . . ?
N2 C28 C27 115.5(3) . . ?
C29 C28 C27 122.8(4) . . ?
C28 C29 C30 119.1(4) . . ?
C28 C29 H29 120.4 . . ?
C30 C29 H29 120.4 . . ?
C31 C30 C29 119.6(4) . . ?
C31 C30 H30 120.2 . . ?
C29 C30 H30 120.2 . . ?
C30 C31 C32 118.5(5) . . ?
C30 C31 H31 120.7 . . ?
C32 C31 H31 120.7 . . ?
N2 C32 C31 123.5(4) . . ?
N2 C32 H32 118.2 . . ?
C31 C32 H32 118.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O5 Mn1 O1 C1 14.4(4) 2_557 . . . ?
O4 Mn1 O1 C1 -170.6(2) 1_545 . . . ?
O9 Mn1 O1 C1 -82.3(2) . . . . ?
O2 Mn1 O1 C1 4.2(2) . . . . ?
O8 Mn1 O1 C1 102.5(2) 2_657 . . . ?
O5 Mn1 O2 C1 -179.4(2) 2_557 . . . ?
O4 Mn1 O2 C1 6.0(4) 1_545 . . . ?
O9 Mn1 O2 C1 88.4(3) . . . . ?
O8 Mn1 O2 C1 -104.3(2) 2_657 . . . ?
O1 Mn1 O2 C1 -4.2(2) . . . . ?
N1 Mn2 O3 C5 145.7(3) . . . . ?
N2 Mn2 O3 C5 87.9(4) . . . . ?
O8 Mn2 O3 C5 -13.2(3) 2_667 . . . ?
O6 Mn2 O3 C5 -136.5(3) 2_567 . . . ?
O5 Mn2 O3 C5 -81.5(3) 2_567 . . . ?
O3 Mn2 N1 C23 34.0(3) . . . . ?
N2 Mn2 N1 C23 -168.5(3) . . . . ?
O8 Mn2 N1 C23 137.3(3) 2_667 . . . ?
O6 Mn2 N1 C23 -61.5(3) 2_567 . . . ?
O5 Mn2 N1 C23 -60.5(4) 2_567 . . . ?
O3 Mn2 N1 C27 -165.6(3) . . . . ?
N2 Mn2 N1 C27 -8.1(3) . . . . ?
O8 Mn2 N1 C27 -62.3(4) 2_667 . . . ?
O6 Mn2 N1 C27 98.9(3) 2_567 . . . ?
O5 Mn2 N1 C27 99.9(3) 2_567 . . . ?
O3 Mn2 N2 C32 -109.7(4) . . . . ?
N1 Mn2 N2 C32 -171.4(4) . . . . ?
O8 Mn2 N2 C32 -8.9(3) 2_667 . . . ?
O6 Mn2 N2 C32 115.7(3) 2_567 . . . ?
O5 Mn2 N2 C32 58.7(4) 2_567 . . . ?
O3 Mn2 N2 C28 60.4(4) . . . . ?
N1 Mn2 N2 C28 -1.3(3) . . . . ?
O8 Mn2 N2 C28 161.2(3) 2_667 . . . ?
O6 Mn2 N2 C28 -74.2(3) 2_567 . . . ?
O5 Mn2 N2 C28 -131.2(3) 2_567 . . . ?
Mn1 O2 C1 O1 7.4(4) . . . . ?
Mn1 O2 C1 C2 -173.6(3) . . . . ?
Mn1 O1 C1 O2 -7.2(4) . . . . ?
Mn1 O1 C1 C2 173.9(3) . . . . ?
O2 C1 C2 C8 179.5(4) . . . . ?
O1 C1 C2 C8 -1.5(6) . . . . ?
O2 C1 C2 C3 -0.2(5) . . . . ?
O1 C1 C2 C3 178.8(4) . . . . ?
C8 C2 C3 C4 0.9(5) . . . . ?
C1 C2 C3 C4 -179.4(3) . . . . ?
C2 C3 C4 C6 -0.2(5) . . . . ?
C2 C3 C4 C5 178.8(3) . . . . ?
Mn2 O3 C5 O4 55.7(5) . . . . ?
Mn2 O3 C5 C4 -125.0(3) . . . . ?
Mn1 O4 C5 O3 -9.6(5) 1_565 . . . ?
Mn1 O4 C5 C4 171.0(2) 1_565 . . . ?
C3 C4 C5 O3 -2.5(5) . . . . ?
C6 C4 C5 O3 176.5(3) . . . . ?
C3 C4 C5 O4 176.8(3) . . . . ?
C6 C4 C5 O4 -4.1(5) . . . . ?
C3 C4 C6 C7 -0.7(6) . . . . ?
C5 C4 C6 C7 -179.8(3) . . . . ?
C4 C6 C7 C8 0.9(6) . . . . ?
C4 C6 C7 C9 179.4(3) . . . . ?
C6 C7 C8 C2 -0.1(5) . . . . ?
C9 C7 C8 C2 -178.6(3) . . . . ?
C3 C2 C8 C7 -0.8(6) . . . . ?
C1 C2 C8 C7 179.5(3) . . . . ?
C8 C7 C9 C10 -168.0(3) . . . . ?
C6 C7 C9 C10 13.6(5) . . . . ?
C8 C7 C9 C14 14.1(6) . . . . ?
C6 C7 C9 C14 -164.3(4) . . . . ?
C14 C9 C10 C11 3.3(6) . . . . ?
C7 C9 C10 C11 -174.8(3) . . . . ?
C9 C10 C11 C12 -2.6(6) . . . . ?
C9 C10 C11 C15 176.2(3) . . . . ?
C10 C11 C12 C13 0.2(6) . . . . ?
C15 C11 C12 C13 -178.6(4) . . . . ?
C11 C12 C13 C14 1.4(6) . . . . ?
C12 C13 C14 C9 -0.6(6) . . . . ?
C10 C9 C14 C13 -1.7(6) . . . . ?
C7 C9 C14 C13 176.3(4) . . . . ?
C12 C11 C15 C16 -142.9(4) . . . . ?
C10 C11 C15 C16 38.4(5) . . . . ?
C12 C11 C15 C21 39.9(5) . . . . ?
C10 C11 C15 C21 -138.8(4) . . . . ?
C21 C15 C16 C17 0.3(5) . . . . ?
C11 C15 C16 C17 -177.0(3) . . . . ?
C15 C16 C17 C19 1.7(6) . . . . ?
C15 C16 C17 C18 -178.0(3) . . . . ?
Mn2 O6 C18 O5 -6.1(4) 2_567 . . . ?
Mn2 O6 C18 C17 175.2(3) 2_567 . . . ?
Mn1 O5 C18 O6 99.5(5) 2_557 . . . ?
Mn2 O5 C18 O6 5.8(4) 2_567 . . . ?
Mn1 O5 C18 C17 -81.8(5) 2_557 . . . ?
Mn2 O5 C18 C17 -175.6(3) 2_567 . . . ?
C19 C17 C18 O6 -11.8(6) . . . . ?
C16 C17 C18 O6 167.8(4) . . . . ?
C19 C17 C18 O5 169.6(4) . . . . ?
C16 C17 C18 O5 -10.8(5) . . . . ?
C16 C17 C19 C20 -1.9(6) . . . . ?
C18 C17 C19 C20 177.7(3) . . . . ?
C17 C19 C20 C21 0.3(6) . . . . ?
C17 C19 C20 C22 -179.3(3) . . . . ?
C16 C15 C21 C20 -2.0(5) . . . . ?
C11 C15 C21 C20 175.3(3) . . . . ?
C19 C20 C21 C15 1.7(6) . . . . ?
C22 C20 C21 C15 -178.7(3) . . . . ?
Mn1 O8 C22 O7 -99.5(4) 2_657 . . . ?
Mn2 O8 C22 O7 4.7(4) 2_667 . . . ?
Mn1 O8 C22 C20 82.6(4) 2_657 . . . ?
Mn2 O8 C22 C20 -173.2(3) 2_667 . . . ?
C19 C20 C22 O7 -5.0(6) . . . . ?
C21 C20 C22 O7 175.5(4) . . . . ?
C19 C20 C22 O8 172.9(3) . . . . ?
C21 C20 C22 O8 -6.7(5) . . . . ?
C27 N1 C23 C24 0.4(7) . . . . ?
Mn2 N1 C23 C24 160.3(4) . . . . ?
N1 C23 C24 C25 -0.3(8) . . . . ?
C23 C24 C25 C26 0.0(9) . . . . ?
C24 C25 C26 C27 0.1(9) . . . . ?
C23 N1 C27 C26 -0.2(6) . . . . ?
Mn2 N1 C27 C26 -161.6(4) . . . . ?
C23 N1 C27 C28 177.3(3) . . . . ?
Mn2 N1 C27 C28 15.9(4) . . . . ?
C25 C26 C27 N1 0.0(8) . . . . ?
C25 C26 C27 C28 -177.5(5) . . . . ?
C32 N2 C28 C29 1.1(6) . . . . ?
Mn2 N2 C28 C29 -169.8(3) . . . . ?
C32 N2 C28 C27 -179.4(4) . . . . ?
Mn2 N2 C28 C27 9.7(4) . . . . ?
N1 C27 C28 N2 -17.2(5) . . . . ?
C26 C27 C28 N2 160.3(4) . . . . ?
N1 C27 C28 C29 162.3(4) . . . . ?
C26 C27 C28 C29 -20.2(6) . . . . ?
N2 C28 C29 C30 -2.4(6) . . . . ?
C27 C28 C29 C30 178.1(4) . . . . ?
C28 C29 C30 C31 1.2(7) . . . . ?
C29 C30 C31 C32 1.2(7) . . . . ?
C28 N2 C32 C31 1.5(6) . . . . ?
Mn2 N2 C32 C31 171.5(4) . . . . ?
C30 C31 C32 N2 -2.6(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.076
_database_code_depnum_ccdc_archive 'CCDC 1009776'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Mn(H2TPTA)(phen)]n'
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H20 Mn N2 O8'
_chemical_formula_sum            'C34 H20 Mn N2 O8'
_chemical_formula_weight         639.46

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.507(6)
_cell_length_b                   10.687(2)
_cell_length_c                   18.199(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.48(3)
_cell_angle_gamma                90.00
_cell_volume                     5497(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7549
_cell_measurement_theta_min      2.0373
_cell_measurement_theta_max      27.8764

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2616
_exptl_absorpt_coefficient_mu    0.542
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8901
_exptl_absorpt_correction_T_max  0.9088
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  Saturn724
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            19786
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.26
_diffrn_reflns_theta_max         25.50
_reflns_number_total             5056
_reflns_number_gt                4539
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0436P)²+7.9680P] 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         5056
_refine_ls_number_parameters     408
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0538
_refine_ls_wR_factor_ref         0.1118
_refine_ls_wR_factor_gt          0.1061
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_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 0.036300(14) 0.31186(4) -0.15332(2) 0.02746(14) Uani 1 1 d . . .
O1 O 0.09791(7) 0.2715(2) -0.05625(10) 0.0389(5) Uani 1 1 d . . .
O2 O 0.04496(7) 0.4169(2) -0.04942(10) 0.0423(5) Uani 1 1 d . . .
O3 O 0.03141(7) 0.6179(2) 0.19293(11) 0.0444(5) Uani 1 1 d . . .
O4 O 0.07811(7) 0.5575(2) 0.29247(10) 0.0396(5) Uani 1 1 d . . .
O5 O 0.15522(9) -0.0790(2) 0.43463(12) 0.0572(7) Uani 1 1 d . . .
H5 H 0.1398 -0.1375 0.4481 0.086 Uiso 1 1 calc R . .
O6 O 0.17761(9) -0.0544(3) 0.55552(13) 0.0626(7) Uani 1 1 d . . .
O7 O 0.35040(8) 0.0396(3) 0.60397(12) 0.0578(7) Uani 1 1 d . . .
H7 H 0.3773 0.0372 0.6264 0.087 Uiso 1 1 calc R . .
O8 O 0.38086(10) 0.1878(3) 0.53878(16) 0.0845(10) Uani 1 1 d . . .
N1 N 0.06181(8) 0.1307(2) -0.19944(12) 0.0329(6) Uani 1 1 d . . .
N2 N -0.00671(8) 0.1587(2) -0.11044(13) 0.0348(6) Uani 1 1 d . . .
C1 C 0.08034(10) 0.3576(3) -0.02086(14) 0.0296(6) Uani 1 1 d . . .
C2 C 0.10155(10) 0.3870(2) 0.05731(14) 0.0275(6) Uani 1 1 d . . .
C3 C 0.07603(10) 0.4597(2) 0.10127(14) 0.0283(6) Uani 1 1 d . . .
H3 H 0.0477 0.4963 0.0810 0.034 Uiso 1 1 calc R . .
C4 C 0.09298(9) 0.4777(2) 0.17554(14) 0.0276(6) Uani 1 1 d . . .
C5 C 0.06544(10) 0.5549(3) 0.22317(15) 0.0302(6) Uani 1 1 d . . .
C6 C 0.13628(10) 0.4255(2) 0.20462(14) 0.0282(6) Uani 1 1 d . . .
H6 H 0.1477 0.4386 0.2543 0.034 Uiso 1 1 calc R . .
C7 C 0.16281(9) 0.3545(2) 0.16113(14) 0.0274(6) Uani 1 1 d . . .
C8 C 0.14480(10) 0.3355(3) 0.08711(14) 0.0308(6) Uani 1 1 d . . .
H8 H 0.1619 0.2879 0.0571 0.037 Uiso 1 1 calc R . .
C9 C 0.20867(10) 0.2990(3) 0.19401(15) 0.0302(6) Uani 1 1 d . . .
C10 C 0.21437(10) 0.2586(3) 0.26752(14) 0.0316(6) Uani 1 1 d . . .
H10 H 0.1894 0.2677 0.2953 0.038 Uiso 1 1 calc R . .
C11 C 0.25641(10) 0.2048(3) 0.30036(16) 0.0334(7) Uani 1 1 d . . .
C12 C 0.29356(10) 0.1944(3) 0.25843(17) 0.0403(7) Uani 1 1 d . . .
H12 H 0.3222 0.1605 0.2798 0.048 Uiso 1 1 calc R . .
C13 C 0.28866(11) 0.2337(3) 0.18533(17) 0.0476(8) Uani 1 1 d . . .
H13 H 0.3139 0.2261 0.1579 0.057 Uiso 1 1 calc R . .
C14 C 0.24623(10) 0.2843(3) 0.15319(16) 0.0385(7) Uani 1 1 d . . .
H14 H 0.2428 0.3086 0.1037 0.046 Uiso 1 1 calc R . .
C15 C 0.25973(10) 0.1542(3) 0.37698(16) 0.0334(7) Uani 1 1 d . . .
C16 C 0.22152(10) 0.0893(3) 0.39919(16) 0.0355(7) Uani 1 1 d . . .
H16 H 0.1941 0.0794 0.3659 0.043 Uiso 1 1 calc R . .
C17 C 0.22344(10) 0.0393(3) 0.46964(16) 0.0355(7) Uani 1 1 d . . .
C18 C 0.18352(11) -0.0343(3) 0.49216(17) 0.0399(7) Uani 1 1 d . . .
C19 C 0.26431(11) 0.0514(3) 0.51923(16) 0.0383(7) Uani 1 1 d . . .
H19 H 0.2657 0.0183 0.5667 0.046 Uiso 1 1 calc R . .
C20 C 0.30313(10) 0.1128(3) 0.49812(16) 0.0369(7) Uani 1 1 d . . .
C21 C 0.30062(10) 0.1655(3) 0.42761(16) 0.0374(7) Uani 1 1 d . . .
H21 H 0.3265 0.2086 0.4142 0.045 Uiso 1 1 calc R . .
C22 C 0.34903(12) 0.1204(3) 0.54807(17) 0.0453(8) Uani 1 1 d . . .
C23 C 0.09626(11) 0.1166(3) -0.24092(17) 0.0460(8) Uani 1 1 d . . .
H23 H 0.1098 0.1880 -0.2584 0.055 Uiso 1 1 calc R . .
C24 C 0.11331(13) -0.0003(4) -0.2598(2) 0.0617(11) Uani 1 1 d . . .
H24 H 0.1376 -0.0065 -0.2891 0.074 Uiso 1 1 calc R . .
C25 C 0.09346(14) -0.1046(4) -0.2342(2) 0.0628(11) Uani 1 1 d . . .
H25 H 0.1044 -0.1832 -0.2460 0.075 Uiso 1 1 calc R . .
C26 C 0.05708(12) -0.0952(3) -0.19066(19) 0.0479(8) Uani 1 1 d . . .
C27 C 0.04236(10) 0.0257(3) -0.17335(16) 0.0355(7) Uani 1 1 d . . .
C28 C 0.03379(15) -0.2008(3) -0.1619(2) 0.0640(12) Uani 1 1 d . . .
H28 H 0.0437 -0.2813 -0.1716 0.077 Uiso 1 1 calc R . .
C29 C -0.00179(16) -0.1856(4) -0.1215(2) 0.0645(11) Uani 1 1 d . . .
H29 H -0.0166 -0.2558 -0.1049 0.077 Uiso 1 1 calc R . .
C30 C -0.01746(13) -0.0650(3) -0.10345(18) 0.0485(9) Uani 1 1 d . . .
C31 C 0.00520(11) 0.0414(3) -0.12786(15) 0.0363(7) Uani 1 1 d . . .
C32 C -0.05461(14) -0.0431(4) -0.0611(2) 0.0622(11) Uani 1 1 d . . .
H32 H -0.0709 -0.1105 -0.0444 0.075 Uiso 1 1 calc R . .
C33 C -0.06690(13) 0.0758(4) -0.0444(2) 0.0588(10) Uani 1 1 d . . .
H33 H -0.0916 0.0907 -0.0168 0.071 Uiso 1 1 calc R . .
C34 C -0.04150(11) 0.1739(3) -0.06979(16) 0.0438(8) Uani 1 1 d . . .
H34 H -0.0494 0.2550 -0.0575 0.053 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 O3 2.109(2) 5_565 ?
Mn1 O4 2.156(2) 6_565 ?
Mn1 O2 2.185(2) . ?
Mn1 N2 2.245(2) . ?
Mn1 N1 2.267(2) . ?
Mn1 O1 2.363(2) . ?
Mn1 C1 2.615(3) . ?
O1 C1 1.264(3) . ?
O2 C1 1.246(3) . ?
O3 C5 1.248(3) . ?
O3 Mn1 2.109(2) 5_565 ?
O4 C5 1.266(3) . ?
O4 Mn1 2.156(2) 6_566 ?
O5 C18 1.325(4) . ?
O5 H5 0.8200 . ?
O6 C18 1.206(4) . ?
O7 C22 1.331(4) . ?
O7 H7 0.8200 . ?
O8 C22 1.188(4) . ?
N1 C23 1.323(4) . ?
N1 C27 1.364(4) . ?
N2 C34 1.322(4) . ?
N2 C31 1.347(4) . ?
C1 C2 1.505(4) . ?
C2 C3 1.387(4) . ?
C2 C8 1.393(4) . ?
C3 C4 1.388(4) . ?
C3 H3 0.9300 . ?
C4 C6 1.395(4) . ?
C4 C5 1.491(4) . ?
C6 C7 1.390(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.393(4) . ?
C7 C9 1.488(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.395(4) . ?
C9 C14 1.389(4) . ?
C10 C11 1.392(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.388(4) . ?
C11 C15 1.487(4) . ?
C12 C13 1.385(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.383(4) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 C21 1.394(4) . ?
C15 C16 1.395(4) . ?
C16 C17 1.384(4) . ?
C16 H16 0.9300 . ?
C17 C19 1.384(4) . ?
C17 C18 1.484(4) . ?
C19 C20 1.383(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.395(4) . ?
C20 C22 1.495(4) . ?
C21 H21 0.9300 . ?
C23 C24 1.400(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.359(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.388(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.407(4) . ?
C26 C28 1.442(5) . ?
C27 C31 1.437(4) . ?
C28 C29 1.337(6) . ?
C28 H28 0.9300 . ?
C29 C30 1.416(5) . ?
C29 H29 0.9300 . ?
C30 C31 1.408(4) . ?
C30 C32 1.408(5) . ?
C32 C33 1.363(5) . ?
C32 H32 0.9300 . ?
C33 C34 1.387(5) . ?
C33 H33 0.9300 . ?
C34 H34 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 Mn1 O4 98.56(9) 5_565 6_565 ?
O3 Mn1 O2 96.21(8) 5_565 . ?
O4 Mn1 O2 93.23(8) 6_565 . ?
O3 Mn1 N2 82.04(9) 5_565 . ?
O4 Mn1 N2 172.10(8) 6_565 . ?
O2 Mn1 N2 94.53(9) . . ?
O3 Mn1 N1 120.06(8) 5_565 . ?
O4 Mn1 N1 99.24(9) 6_565 . ?
O2 Mn1 N1 138.89(8) . . ?
N2 Mn1 N1 73.86(9) . . ?
O3 Mn1 O1 151.49(8) 5_565 . ?
O4 Mn1 O1 93.38(8) 6_565 . ?
O2 Mn1 O1 57.15(7) . . ?
N2 Mn1 O1 89.62(8) . . ?
N1 Mn1 O1 82.98(7) . . ?
O3 Mn1 C1 123.83(9) 5_565 . ?
O4 Mn1 C1 94.19(8) 6_565 . ?
O2 Mn1 C1 28.31(8) . . ?
N2 Mn1 C1 91.96(9) . . ?
N1 Mn1 C1 111.24(9) . . ?
O1 Mn1 C1 28.84(8) . . ?
C1 O1 Mn1 86.72(16) . . ?
C1 O2 Mn1 95.39(17) . . ?
C5 O3 Mn1 165.2(2) . 5_565 ?
C5 O4 Mn1 111.54(17) . 6_566 ?
C18 O5 H5 109.5 . . ?
C22 O7 H7 109.5 . . ?
C23 N1 C27 118.1(3) . . ?
C23 N1 Mn1 127.3(2) . . ?
C27 N1 Mn1 114.14(19) . . ?
C34 N2 C31 118.5(3) . . ?
C34 N2 Mn1 126.0(2) . . ?
C31 N2 Mn1 115.5(2) . . ?
O2 C1 O1 120.7(2) . . ?
O2 C1 C2 119.5(3) . . ?
O1 C1 C2 119.8(2) . . ?
O2 C1 Mn1 56.29(14) . . ?
O1 C1 Mn1 64.44(14) . . ?
C2 C1 Mn1 175.0(2) . . ?
C3 C2 C8 120.0(2) . . ?
C3 C2 C1 119.1(2) . . ?
C8 C2 C1 120.8(2) . . ?
C2 C3 C4 119.8(2) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C6 C4 C3 119.5(2) . . ?
C6 C4 C5 120.5(2) . . ?
C3 C4 C5 120.0(2) . . ?
O3 C5 O4 122.1(3) . . ?
O3 C5 C4 118.7(2) . . ?
O4 C5 C4 119.2(2) . . ?
C4 C6 C7 121.5(2) . . ?
C4 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C8 C7 C6 118.1(2) . . ?
C8 C7 C9 121.7(2) . . ?
C6 C7 C9 120.2(2) . . ?
C2 C8 C7 121.0(3) . . ?
C2 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
C10 C9 C14 118.4(3) . . ?
C10 C9 C7 119.7(2) . . ?
C14 C9 C7 121.9(2) . . ?
C11 C10 C9 121.7(3) . . ?
C11 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
C10 C11 C12 118.2(3) . . ?
C10 C11 C15 119.9(3) . . ?
C12 C11 C15 121.8(3) . . ?
C13 C12 C11 121.0(3) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C14 C13 C12 119.9(3) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C13 C14 C9 120.7(3) . . ?
C13 C14 H14 119.6 . . ?
C9 C14 H14 119.6 . . ?
C21 C15 C16 118.0(3) . . ?
C21 C15 C11 122.3(3) . . ?
C16 C15 C11 119.7(2) . . ?
C17 C16 C15 121.5(3) . . ?
C17 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
C19 C17 C16 119.8(3) . . ?
C19 C17 C18 118.7(3) . . ?
C16 C17 C18 121.4(3) . . ?
O6 C18 O5 123.0(3) . . ?
O6 C18 C17 124.5(3) . . ?
O5 C18 C17 112.5(3) . . ?
C20 C19 C17 120.0(3) . . ?
C20 C19 H19 120.0 . . ?
C17 C19 H19 120.0 . . ?
C19 C20 C21 120.0(3) . . ?
C19 C20 C22 121.7(3) . . ?
C21 C20 C22 118.3(3) . . ?
C15 C21 C20 120.8(3) . . ?
C15 C21 H21 119.6 . . ?
C20 C21 H21 119.6 . . ?
O8 C22 O7 123.7(3) . . ?
O8 C22 C20 124.8(3) . . ?
O7 C22 C20 111.4(3) . . ?
N1 C23 C24 123.3(4) . . ?
N1 C23 H23 118.4 . . ?
C24 C23 H23 118.4 . . ?
C25 C24 C23 118.4(4) . . ?
C25 C24 H24 120.8 . . ?
C23 C24 H24 120.8 . . ?
C24 C25 C26 120.7(4) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C25 C26 C27 117.5(3) . . ?
C25 C26 C28 124.3(4) . . ?
C27 C26 C28 118.2(3) . . ?
N1 C27 C26 122.1(3) . . ?
N1 C27 C31 117.9(3) . . ?
C26 C27 C31 120.0(3) . . ?
C29 C28 C26 121.5(4) . . ?
C29 C28 H28 119.2 . . ?
C26 C28 H28 119.2 . . ?
C28 C29 C30 121.5(4) . . ?
C28 C29 H29 119.3 . . ?
C30 C29 H29 119.3 . . ?
C31 C30 C32 116.5(3) . . ?
C31 C30 C29 119.4(4) . . ?
C32 C30 C29 124.1(4) . . ?
N2 C31 C30 122.5(3) . . ?
N2 C31 C27 118.2(3) . . ?
C30 C31 C27 119.4(3) . . ?
C33 C32 C30 120.7(3) . . ?
C33 C32 H32 119.7 . . ?
C30 C32 H32 119.7 . . ?
C32 C33 C34 118.0(4) . . ?
C32 C33 H33 121.0 . . ?
C34 C33 H33 121.0 . . ?
N2 C34 C33 123.7(3) . . ?
N2 C34 H34 118.1 . . ?
C33 C34 H34 118.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 Mn1 O1 C1 -22.4(3) 5_565 . . . ?
O4 Mn1 O1 C1 92.55(17) 6_565 . . . ?
O2 Mn1 O1 C1 0.89(16) . . . . ?
N2 Mn1 O1 C1 -94.76(17) . . . . ?
N1 Mn1 O1 C1 -168.54(18) . . . . ?
O3 Mn1 O2 C1 168.18(18) 5_565 . . . ?
O4 Mn1 O2 C1 -92.84(18) 6_565 . . . ?
N2 Mn1 O2 C1 85.71(18) . . . . ?
N1 Mn1 O2 C1 15.2(2) . . . . ?
O1 Mn1 O2 C1 -0.90(16) . . . . ?
O3 Mn1 N1 C23 111.9(2) 5_565 . . . ?
O4 Mn1 N1 C23 6.3(2) 6_565 . . . ?
O2 Mn1 N1 C23 -99.6(2) . . . . ?
N2 Mn1 N1 C23 -177.7(2) . . . . ?
O1 Mn1 N1 C23 -86.0(2) . . . . ?
C1 Mn1 N1 C23 -91.9(2) . . . . ?
O3 Mn1 N1 C27 -76.19(19) 5_565 . . . ?
O4 Mn1 N1 C27 178.24(17) 6_565 . . . ?
O2 Mn1 N1 C27 72.4(2) . . . . ?
N2 Mn1 N1 C27 -5.71(17) . . . . ?
O1 Mn1 N1 C27 85.93(18) . . . . ?
C1 Mn1 N1 C27 80.03(19) . . . . ?
O3 Mn1 N2 C34 -52.2(2) 5_565 . . . ?
O4 Mn1 N2 C34 -147.1(5) 6_565 . . . ?
O2 Mn1 N2 C34 43.5(2) . . . . ?
N1 Mn1 N2 C34 -176.7(2) . . . . ?
O1 Mn1 N2 C34 100.5(2) . . . . ?
C1 Mn1 N2 C34 71.7(2) . . . . ?
O3 Mn1 N2 C31 128.6(2) 5_565 . . . ?
O4 Mn1 N2 C31 33.7(7) 6_565 . . . ?
O2 Mn1 N2 C31 -135.71(19) . . . . ?
N1 Mn1 N2 C31 4.09(18) . . . . ?
O1 Mn1 N2 C31 -78.71(19) . . . . ?
C1 Mn1 N2 C31 -107.5(2) . . . . ?
Mn1 O2 C1 O1 1.6(3) . . . . ?
Mn1 O2 C1 C2 -176.8(2) . . . . ?
Mn1 O1 C1 O2 -1.5(3) . . . . ?
Mn1 O1 C1 C2 177.0(2) . . . . ?
O3 Mn1 C1 O2 -14.2(2) 5_565 . . . ?
O4 Mn1 C1 O2 89.04(18) 6_565 . . . ?
N2 Mn1 C1 O2 -95.92(18) . . . . ?
N1 Mn1 C1 O2 -169.36(17) . . . . ?
O1 Mn1 C1 O2 178.4(3) . . . . ?
O3 Mn1 C1 O1 167.38(16) 5_565 . . . ?
O4 Mn1 C1 O1 -89.40(17) 6_565 . . . ?
O2 Mn1 C1 O1 -178.4(3) . . . . ?
N2 Mn1 C1 O1 85.65(17) . . . . ?
N1 Mn1 C1 O1 12.21(19) . . . . ?
O3 Mn1 C1 C2 19(2) 5_565 . . . ?
O4 Mn1 C1 C2 123(2) 6_565 . . . ?
O2 Mn1 C1 C2 33(2) . . . . ?
N2 Mn1 C1 C2 -62(2) . . . . ?
N1 Mn1 C1 C2 -136(2) . . . . ?
O1 Mn1 C1 C2 -148(2) . . . . ?
O2 C1 C2 C3 13.4(4) . . . . ?
O1 C1 C2 C3 -165.1(3) . . . . ?
Mn1 C1 C2 C3 -18(2) . . . . ?
O2 C1 C2 C8 -170.7(3) . . . . ?
O1 C1 C2 C8 10.8(4) . . . . ?
Mn1 C1 C2 C8 157(2) . . . . ?
C8 C2 C3 C4 -2.1(4) . . . . ?
C1 C2 C3 C4 173.8(2) . . . . ?
C2 C3 C4 C6 1.9(4) . . . . ?
C2 C3 C4 C5 -179.4(2) . . . . ?
Mn1 O3 C5 O4 -76.1(8) 5_565 . . . ?
Mn1 O3 C5 C4 106.1(7) 5_565 . . . ?
Mn1 O4 C5 O3 -2.8(4) 6_566 . . . ?
Mn1 O4 C5 C4 174.95(19) 6_566 . . . ?
C6 C4 C5 O3 167.6(3) . . . . ?
C3 C4 C5 O3 -11.1(4) . . . . ?
C6 C4 C5 O4 -10.3(4) . . . . ?
C3 C4 C5 O4 171.1(3) . . . . ?
C3 C4 C6 C7 -0.7(4) . . . . ?
C5 C4 C6 C7 -179.3(3) . . . . ?
C4 C6 C7 C8 -0.5(4) . . . . ?
C4 C6 C7 C9 -179.4(3) . . . . ?
C3 C2 C8 C7 0.9(4) . . . . ?
C1 C2 C8 C7 -174.9(2) . . . . ?
C6 C7 C8 C2 0.4(4) . . . . ?
C9 C7 C8 C2 179.3(3) . . . . ?
C8 C7 C9 C10 -144.9(3) . . . . ?
C6 C7 C9 C10 34.0(4) . . . . ?
C8 C7 C9 C14 34.1(4) . . . . ?
C6 C7 C9 C14 -147.0(3) . . . . ?
C14 C9 C10 C11 0.2(4) . . . . ?
C7 C9 C10 C11 179.3(3) . . . . ?
C9 C10 C11 C12 1.3(4) . . . . ?
C9 C10 C11 C15 -175.4(3) . . . . ?
C10 C11 C12 C13 -1.4(5) . . . . ?
C15 C11 C12 C13 175.2(3) . . . . ?
C11 C12 C13 C14 0.0(5) . . . . ?
C12 C13 C14 C9 1.6(5) . . . . ?
C10 C9 C14 C13 -1.7(5) . . . . ?
C7 C9 C14 C13 179.3(3) . . . . ?
C10 C11 C15 C21 -142.5(3) . . . . ?
C12 C11 C15 C21 40.9(4) . . . . ?
C10 C11 C15 C16 39.7(4) . . . . ?
C12 C11 C15 C16 -136.9(3) . . . . ?
C21 C15 C16 C17 1.2(4) . . . . ?
C11 C15 C16 C17 179.1(3) . . . . ?
C15 C16 C17 C19 -1.2(5) . . . . ?
C15 C16 C17 C18 -177.4(3) . . . . ?
C19 C17 C18 O6 22.5(5) . . . . ?
C16 C17 C18 O6 -161.2(3) . . . . ?
C19 C17 C18 O5 -155.9(3) . . . . ?
C16 C17 C18 O5 20.4(4) . . . . ?
C16 C17 C19 C20 -0.4(5) . . . . ?
C18 C17 C19 C20 176.0(3) . . . . ?
C17 C19 C20 C21 1.8(5) . . . . ?
C17 C19 C20 C22 -175.8(3) . . . . ?
C16 C15 C21 C20 0.3(4) . . . . ?
C11 C15 C21 C20 -177.6(3) . . . . ?
C19 C20 C21 C15 -1.7(5) . . . . ?
C22 C20 C21 C15 175.9(3) . . . . ?
C19 C20 C22 O8 -167.1(4) . . . . ?
C21 C20 C22 O8 15.3(5) . . . . ?
C19 C20 C22 O7 14.4(4) . . . . ?
C21 C20 C22 O7 -163.2(3) . . . . ?
C27 N1 C23 C24 0.6(4) . . . . ?
Mn1 N1 C23 C24 172.3(2) . . . . ?
N1 C23 C24 C25 0.0(5) . . . . ?
C23 C24 C25 C26 0.2(5) . . . . ?
C24 C25 C26 C27 -1.0(5) . . . . ?
C24 C25 C26 C28 179.4(3) . . . . ?
C23 N1 C27 C26 -1.5(4) . . . . ?
Mn1 N1 C27 C26 -174.2(2) . . . . ?
C23 N1 C27 C31 179.5(2) . . . . ?
Mn1 N1 C27 C31 6.8(3) . . . . ?
C25 C26 C27 N1 1.7(4) . . . . ?
C28 C26 C27 N1 -178.7(3) . . . . ?
C25 C26 C27 C31 -179.4(3) . . . . ?
C28 C26 C27 C31 0.3(4) . . . . ?
C25 C26 C28 C29 -178.5(3) . . . . ?
C27 C26 C28 C29 1.9(5) . . . . ?
C26 C28 C29 C30 -1.7(6) . . . . ?
C28 C29 C30 C31 -0.6(5) . . . . ?
C28 C29 C30 C32 -179.9(3) . . . . ?
C34 N2 C31 C30 -1.0(4) . . . . ?
Mn1 N2 C31 C30 178.2(2) . . . . ?
C34 N2 C31 C27 178.7(2) . . . . ?
Mn1 N2 C31 C27 -2.1(3) . . . . ?
C32 C30 C31 N2 1.8(4) . . . . ?
C29 C30 C31 N2 -177.5(3) . . . . ?
C32 C30 C31 C27 -178.0(3) . . . . ?
C29 C30 C31 C27 2.7(4) . . . . ?
N1 C27 C31 N2 -3.3(4) . . . . ?
C26 C27 C31 N2 177.7(3) . . . . ?
N1 C27 C31 C30 176.5(2) . . . . ?
C26 C27 C31 C30 -2.5(4) . . . . ?
C31 C30 C32 C33 -1.0(5) . . . . ?
C29 C30 C32 C33 178.3(3) . . . . ?
C30 C32 C33 C34 -0.5(5) . . . . ?
C31 N2 C34 C33 -0.6(4) . . . . ?
Mn1 N2 C34 C33 -179.7(2) . . . . ?
C32 C33 C34 N2 1.4(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.051
_database_code_depnum_ccdc_archive 'CCDC 1009777'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_5

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Co(H2TPTA)(phen)]n'
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H20 Co N2 O8'
_chemical_formula_sum            'C34 H20 Co N2 O8'
_chemical_formula_weight         643.45

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.427(6)
_cell_length_b                   10.685(2)
_cell_length_c                   17.978(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.49(3)
_cell_angle_gamma                90.00
_cell_volume                     5414.1(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8141
_cell_measurement_theta_min      2.0383
_cell_measurement_theta_max      27.9604

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2632
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8791
_exptl_absorpt_correction_T_max  0.9027
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  Saturn724
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            22030
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.04
_diffrn_reflns_theta_max         25.50
_reflns_number_total             5025
_reflns_number_gt                4736
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0434P)²+7.0583P] 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         5025
_refine_ls_number_parameters     408
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_ref         0.0909
_refine_ls_wR_factor_gt          0.0884
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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 0.464639(10) 0.69431(3) 0.151857(14) 0.02348(10) Uani 1 1 d . . .
O1 O 0.42543(5) 0.56415(14) 0.20512(8) 0.0322(4) Uani 1 1 d . . .
O2 O 0.47094(5) 0.62236(15) 0.30849(8) 0.0351(4) Uani 1 1 d . . .
O3 O 0.45838(6) 0.41165(16) 0.55103(8) 0.0382(4) Uani 1 1 d . . .
O4 O 0.40371(6) 0.27104(15) 0.55740(8) 0.0363(4) Uani 1 1 d . . .
O5 O 0.34549(7) -0.0805(2) 0.06349(10) 0.0541(5) Uani 1 1 d . . .
H5 H 0.3631 -0.1342 0.0497 0.081 Uiso 1 1 calc R . .
O6 O 0.32323(7) -0.0570(2) -0.05930(10) 0.0574(5) Uani 1 1 d . . .
O7 O 0.11834(8) 0.1811(2) -0.04173(14) 0.0816(8) Uani 1 1 d . . .
O8 O 0.14793(6) 0.02662(19) -0.10414(10) 0.0500(5) Uani 1 1 d . . .
H8 H 0.1212 0.0263 -0.1277 0.075 Uiso 1 1 calc R . .
N1 N 0.50616(6) 0.83527(17) 0.10798(10) 0.0294(4) Uani 1 1 d . . .
N2 N 0.43918(6) 0.86040(17) 0.19835(10) 0.0291(4) Uani 1 1 d . . .
C1 C 0.43759(7) 0.55965(19) 0.27577(11) 0.0250(4) Uani 1 1 d . . .
C2 C 0.40983(7) 0.48021(18) 0.32304(11) 0.0239(4) Uani 1 1 d . . .
C3 C 0.42704(8) 0.45958(19) 0.39845(11) 0.0253(4) Uani 1 1 d . . .
H3 H 0.4558 0.4945 0.4190 0.030 Uiso 1 1 calc R . .
C4 C 0.40121(7) 0.38707(19) 0.44255(11) 0.0250(4) Uani 1 1 d . . .
C5 C 0.42201(8) 0.3559(2) 0.52150(11) 0.0271(5) Uani 1 1 d . . .
C6 C 0.35747(8) 0.3378(2) 0.41244(11) 0.0274(5) Uani 1 1 d . . .
H6 H 0.3401 0.2905 0.4427 0.033 Uiso 1 1 calc R . .
C7 C 0.33929(7) 0.35829(19) 0.33743(11) 0.0251(4) Uani 1 1 d . . .
C8 C 0.36621(7) 0.42926(19) 0.29341(11) 0.0254(4) Uani 1 1 d . . .
H8A H 0.3548 0.4429 0.2432 0.031 Uiso 1 1 calc R . .
C9 C 0.29326(8) 0.30346(19) 0.30440(12) 0.0275(5) Uani 1 1 d . . .
C10 C 0.25556(8) 0.2902(2) 0.34653(13) 0.0350(5) Uani 1 1 d . . .
H10 H 0.2590 0.3167 0.3962 0.042 Uiso 1 1 calc R . .
C11 C 0.21326(9) 0.2379(3) 0.31471(14) 0.0421(6) Uani 1 1 d . . .
H11 H 0.1883 0.2298 0.3431 0.051 Uiso 1 1 calc R . .
C12 C 0.20771(8) 0.1975(2) 0.24089(14) 0.0383(6) Uani 1 1 d . . .
H12 H 0.1789 0.1632 0.2199 0.046 Uiso 1 1 calc R . .
C13 C 0.24472(8) 0.2075(2) 0.19782(12) 0.0307(5) Uani 1 1 d . . .
C14 C 0.28696(8) 0.2621(2) 0.23006(12) 0.0289(5) Uani 1 1 d . . .
H14 H 0.3117 0.2713 0.2013 0.035 Uiso 1 1 calc R . .
C15 C 0.24116(8) 0.1550(2) 0.12068(12) 0.0302(5) Uani 1 1 d . . .
C16 C 0.27925(8) 0.0901(2) 0.09826(12) 0.0327(5) Uani 1 1 d . . .
H16 H 0.3070 0.0818 0.1316 0.039 Uiso 1 1 calc R . .
C17 C 0.27706(8) 0.0371(2) 0.02724(13) 0.0327(5) Uani 1 1 d . . .
C18 C 0.31733(9) -0.0370(2) 0.00475(14) 0.0374(5) Uani 1 1 d . . .
C19 C 0.23537(8) 0.0463(2) -0.02243(13) 0.0351(5) Uani 1 1 d . . .
H19 H 0.2336 0.0113 -0.0701 0.042 Uiso 1 1 calc R . .
C20 C 0.19659(8) 0.1078(2) -0.00056(12) 0.0326(5) Uani 1 1 d . . .
C21 C 0.15023(9) 0.1121(2) -0.05053(13) 0.0400(6) Uani 1 1 d . . .
C22 C 0.19960(8) 0.1633(2) 0.06991(13) 0.0346(5) Uani 1 1 d . . .
H22 H 0.1736 0.2065 0.0834 0.041 Uiso 1 1 calc R . .
C23 C 0.40427(8) 0.8718(2) 0.24020(13) 0.0382(6) Uani 1 1 d . . .
H23 H 0.3911 0.7996 0.2576 0.046 Uiso 1 1 calc R . .
C24 C 0.38642(9) 0.9884(3) 0.25928(16) 0.0505(7) Uani 1 1 d . . .
H24 H 0.3616 0.9929 0.2881 0.061 Uiso 1 1 calc R . .
C25 C 0.40591(10) 1.0942(3) 0.23510(16) 0.0524(7) Uani 1 1 d . . .
H25 H 0.3948 1.1719 0.2483 0.063 Uiso 1 1 calc R . .
C26 C 0.44262(9) 1.0872(2) 0.19032(14) 0.0412(6) Uani 1 1 d . . .
C27 C 0.45790(8) 0.9667(2) 0.17279(12) 0.0308(5) Uani 1 1 d . . .
C28 C 0.46612(11) 1.1943(2) 0.16290(17) 0.0549(8) Uani 1 1 d . . .
H28 H 0.4560 1.2744 0.1735 0.066 Uiso 1 1 calc R . .
C29 C 0.50238(11) 1.1803(2) 0.12222(17) 0.0528(7) Uani 1 1 d . . .
H29 H 0.5174 1.2510 0.1063 0.063 Uiso 1 1 calc R . .
C30 C 0.51828(9) 1.0590(2) 0.10313(14) 0.0409(6) Uani 1 1 d . . .
C31 C 0.49523(8) 0.9532(2) 0.12664(12) 0.0301(5) Uani 1 1 d . . .
C32 C 0.55579(10) 1.0377(3) 0.06044(15) 0.0519(7) Uani 1 1 d . . .
H32 H 0.5726 1.1048 0.0443 0.062 Uiso 1 1 calc R . .
C33 C 0.56728(10) 0.9186(3) 0.04300(15) 0.0485(7) Uani 1 1 d . . .
H33 H 0.5922 0.9038 0.0153 0.058 Uiso 1 1 calc R . .
C34 C 0.54141(8) 0.8190(2) 0.06698(13) 0.0375(6) Uani 1 1 d . . .
H34 H 0.5491 0.7381 0.0538 0.045 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 O2 2.0279(15) 2_655 ?
Co1 O1 2.0909(15) . ?
Co1 O3 2.1249(16) 6_565 ?
Co1 N1 2.1276(18) . ?
Co1 N2 2.1283(18) . ?
Co1 O4 2.2921(17) 6_565 ?
O1 C1 1.273(2) . ?
O2 C1 1.244(2) . ?
O2 Co1 2.0280(15) 2_655 ?
O3 C5 1.250(3) . ?
O3 Co1 2.1249(16) 6_566 ?
O4 C5 1.264(3) . ?
O4 Co1 2.2921(17) 6_566 ?
O5 C18 1.324(3) . ?
O5 H5 0.8200 . ?
O6 C18 1.204(3) . ?
O7 C21 1.195(3) . ?
O8 C21 1.323(3) . ?
O8 H8 0.8200 . ?
N1 C34 1.330(3) . ?
N1 C31 1.351(3) . ?
N2 C23 1.327(3) . ?
N2 C27 1.359(3) . ?
C1 C2 1.497(3) . ?
C2 C8 1.395(3) . ?
C2 C3 1.398(3) . ?
C3 C4 1.386(3) . ?
C3 H3 0.9300 . ?
C4 C6 1.393(3) . ?
C4 C5 1.502(3) . ?
C6 C7 1.397(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.395(3) . ?
C7 C9 1.485(3) . ?
C8 H8A 0.9300 . ?
C9 C14 1.397(3) . ?
C9 C10 1.398(3) . ?
C10 C11 1.381(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.385(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.389(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.392(3) . ?
C13 C15 1.487(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.389(3) . ?
C15 C22 1.399(3) . ?
C16 C17 1.391(3) . ?
C16 H16 0.9300 . ?
C17 C19 1.391(3) . ?
C17 C18 1.490(3) . ?
C19 C20 1.384(3) . ?
C19 H19 0.9300 . ?
C20 C22 1.391(3) . ?
C20 C21 1.496(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.405(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.355(4) . ?
C24 H24 0.9300 . ?
C25 C26 1.401(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.408(3) . ?
C26 C28 1.444(4) . ?
C27 C31 1.437(3) . ?
C28 C29 1.348(4) . ?
C28 H28 0.9300 . ?
C29 C30 1.429(4) . ?
C29 H29 0.9300 . ?
C30 C31 1.400(3) . ?
C30 C32 1.411(4) . ?
C32 C33 1.360(4) . ?
C32 H32 0.9300 . ?
C33 C34 1.394(3) . ?
C33 H33 0.9300 . ?
C34 H34 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 Co1 O1 95.61(7) 2_655 . ?
O2 Co1 O3 93.97(7) 2_655 6_565 ?
O1 Co1 O3 92.63(7) . 6_565 ?
O2 Co1 N1 83.08(7) 2_655 . ?
O1 Co1 N1 174.44(6) . . ?
O3 Co1 N1 92.85(7) 6_565 . ?
O2 Co1 N2 121.05(7) 2_655 . ?
O1 Co1 N2 98.39(7) . . ?
O3 Co1 N2 141.66(6) 6_565 . ?
N1 Co1 N2 77.81(7) . . ?
O2 Co1 O4 151.91(6) 2_655 6_565 ?
O1 Co1 O4 92.88(6) . 6_565 ?
O3 Co1 O4 58.86(6) 6_565 6_565 ?
N1 Co1 O4 90.75(7) . 6_565 ?
N2 Co1 O4 83.88(6) . 6_565 ?
C1 O1 Co1 112.98(13) . . ?
C1 O2 Co1 165.41(15) . 2_655 ?
C5 O3 Co1 94.64(13) . 6_566 ?
C5 O4 Co1 86.61(12) . 6_566 ?
C18 O5 H5 109.5 . . ?
C21 O8 H8 109.5 . . ?
C34 N1 C31 118.28(19) . . ?
C34 N1 Co1 127.39(16) . . ?
C31 N1 Co1 114.31(14) . . ?
C23 N2 C27 118.0(2) . . ?
C23 N2 Co1 128.09(17) . . ?
C27 N2 Co1 113.31(14) . . ?
O2 C1 O1 122.84(19) . . ?
O2 C1 C2 117.56(18) . . ?
O1 C1 C2 119.55(18) . . ?
C8 C2 C3 119.37(19) . . ?
C8 C2 C1 120.85(18) . . ?
C3 C2 C1 119.75(18) . . ?
C4 C3 C2 119.90(19) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C6 120.12(18) . . ?
C3 C4 C5 119.47(19) . . ?
C6 C4 C5 120.31(19) . . ?
O3 C5 O4 119.86(19) . . ?
O3 C5 C4 119.84(19) . . ?
O4 C5 C4 120.28(19) . . ?
C4 C6 C7 120.98(19) . . ?
C4 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C8 C7 C6 118.15(19) . . ?
C8 C7 C9 120.50(18) . . ?
C6 C7 C9 121.32(19) . . ?
C2 C8 C7 121.45(18) . . ?
C2 C8 H8A 119.3 . . ?
C7 C8 H8A 119.3 . . ?
C14 C9 C10 118.3(2) . . ?
C14 C9 C7 120.26(19) . . ?
C10 C9 C7 121.40(19) . . ?
C11 C10 C9 120.3(2) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 120.5(2) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C11 C12 C13 120.7(2) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C12 C13 C14 118.4(2) . . ?
C12 C13 C15 121.7(2) . . ?
C14 C13 C15 119.8(2) . . ?
C13 C14 C9 121.8(2) . . ?
C13 C14 H14 119.1 . . ?
C9 C14 H14 119.1 . . ?
C16 C15 C22 117.8(2) . . ?
C16 C15 C13 119.9(2) . . ?
C22 C15 C13 122.2(2) . . ?
C15 C16 C17 121.8(2) . . ?
C15 C16 H16 119.1 . . ?
C17 C16 H16 119.1 . . ?
C19 C17 C16 119.5(2) . . ?
C19 C17 C18 118.9(2) . . ?
C16 C17 C18 121.4(2) . . ?
O6 C18 O5 123.7(2) . . ?
O6 C18 C17 124.2(2) . . ?
O5 C18 C17 112.1(2) . . ?
C20 C19 C17 119.6(2) . . ?
C20 C19 H19 120.2 . . ?
C17 C19 H19 120.2 . . ?
C19 C20 C22 120.3(2) . . ?
C19 C20 C21 121.1(2) . . ?
C22 C20 C21 118.6(2) . . ?
O7 C21 O8 123.8(2) . . ?
O7 C21 C20 124.3(2) . . ?
O8 C21 C20 111.8(2) . . ?
C20 C22 C15 120.9(2) . . ?
C20 C22 H22 119.5 . . ?
C15 C22 H22 119.5 . . ?
N2 C23 C24 122.7(3) . . ?
N2 C23 H23 118.6 . . ?
C24 C23 H23 118.6 . . ?
C25 C24 C23 119.1(3) . . ?
C25 C24 H24 120.5 . . ?
C23 C24 H24 120.5 . . ?
C24 C25 C26 120.4(2) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C27 116.9(2) . . ?
C25 C26 C28 124.5(2) . . ?
C27 C26 C28 118.6(2) . . ?
N2 C27 C26 122.9(2) . . ?
N2 C27 C31 117.55(19) . . ?
C26 C27 C31 119.6(2) . . ?
C29 C28 C26 121.2(2) . . ?
C29 C28 H28 119.4 . . ?
C26 C28 H28 119.4 . . ?
C28 C29 C30 121.3(3) . . ?
C28 C29 H29 119.4 . . ?
C30 C29 H29 119.4 . . ?
C31 C30 C32 116.8(2) . . ?
C31 C30 C29 119.0(3) . . ?
C32 C30 C29 124.2(2) . . ?
N1 C31 C30 123.1(2) . . ?
N1 C31 C27 116.62(19) . . ?
C30 C31 C27 120.2(2) . . ?
C33 C32 C30 119.9(2) . . ?
C33 C32 H32 120.1 . . ?
C30 C32 H32 120.1 . . ?
C32 C33 C34 119.4(3) . . ?
C32 C33 H33 120.3 . . ?
C34 C33 H33 120.3 . . ?
N1 C34 C33 122.5(2) . . ?
N1 C34 H34 118.7 . . ?
C33 C34 H34 118.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Co1 O1 C1 55.53(15) 2_655 . . . ?
O3 Co1 O1 C1 149.78(15) 6_565 . . . ?
N1 Co1 O1 C1 -20.5(8) . . . . ?
N2 Co1 O1 C1 -67.04(15) . . . . ?
O4 Co1 O1 C1 -151.28(15) 6_565 . . . ?
O2 Co1 N1 C34 51.37(19) 2_655 . . . ?
O1 Co1 N1 C34 128.0(6) . . . . ?
O3 Co1 N1 C34 -42.28(19) 6_565 . . . ?
N2 Co1 N1 C34 175.3(2) . . . . ?
O4 Co1 N1 C34 -101.14(19) 6_565 . . . ?
O2 Co1 N1 C31 -126.84(15) 2_655 . . . ?
O1 Co1 N1 C31 -50.2(7) . . . . ?
O3 Co1 N1 C31 139.50(15) 6_565 . . . ?
N2 Co1 N1 C31 -2.94(14) . . . . ?
O4 Co1 N1 C31 80.64(15) 6_565 . . . ?
O2 Co1 N2 C23 -109.50(18) 2_655 . . . ?
O1 Co1 N2 C23 -7.72(19) . . . . ?
O3 Co1 N2 C23 97.4(2) 6_565 . . . ?
N1 Co1 N2 C23 176.41(19) . . . . ?
O4 Co1 N2 C23 84.30(18) 6_565 . . . ?
O2 Co1 N2 C27 79.45(15) 2_655 . . . ?
O1 Co1 N2 C27 -178.77(14) . . . . ?
O3 Co1 N2 C27 -73.62(18) 6_565 . . . ?
N1 Co1 N2 C27 5.36(14) . . . . ?
O4 Co1 N2 C27 -86.74(15) 6_565 . . . ?
Co1 O2 C1 O1 -69.8(7) 2_655 . . . ?
Co1 O2 C1 C2 112.8(6) 2_655 . . . ?
Co1 O1 C1 O2 -3.2(3) . . . . ?
Co1 O1 C1 C2 174.13(14) . . . . ?
O2 C1 C2 C8 165.9(2) . . . . ?
O1 C1 C2 C8 -11.6(3) . . . . ?
O2 C1 C2 C3 -12.3(3) . . . . ?
O1 C1 C2 C3 170.23(19) . . . . ?
C8 C2 C3 C4 1.2(3) . . . . ?
C1 C2 C3 C4 179.38(19) . . . . ?
C2 C3 C4 C6 -1.9(3) . . . . ?
C2 C3 C4 C5 174.54(19) . . . . ?
Co1 O3 C5 O4 1.7(2) 6_566 . . . ?
Co1 O3 C5 C4 -176.29(17) 6_566 . . . ?
Co1 O4 C5 O3 -1.5(2) 6_566 . . . ?
Co1 O4 C5 C4 176.40(18) 6_566 . . . ?
C3 C4 C5 O3 11.9(3) . . . . ?
C6 C4 C5 O3 -171.7(2) . . . . ?
C3 C4 C5 O4 -166.0(2) . . . . ?
C6 C4 C5 O4 10.4(3) . . . . ?
C3 C4 C6 C7 1.2(3) . . . . ?
C5 C4 C6 C7 -175.21(19) . . . . ?
C4 C6 C7 C8 0.2(3) . . . . ?
C4 C6 C7 C9 178.46(19) . . . . ?
C3 C2 C8 C7 0.1(3) . . . . ?
C1 C2 C8 C7 -178.00(19) . . . . ?
C6 C7 C8 C2 -0.8(3) . . . . ?
C9 C7 C8 C2 -179.13(19) . . . . ?
C8 C7 C9 C14 34.2(3) . . . . ?
C6 C7 C9 C14 -144.0(2) . . . . ?
C8 C7 C9 C10 -146.7(2) . . . . ?
C6 C7 C9 C10 35.1(3) . . . . ?
C14 C9 C10 C11 -0.3(3) . . . . ?
C7 C9 C10 C11 -179.4(2) . . . . ?
C9 C10 C11 C12 0.3(4) . . . . ?
C10 C11 C12 C13 0.7(4) . . . . ?
C11 C12 C13 C14 -1.7(4) . . . . ?
C11 C12 C13 C15 174.6(2) . . . . ?
C12 C13 C14 C9 1.7(3) . . . . ?
C15 C13 C14 C9 -174.7(2) . . . . ?
C10 C9 C14 C13 -0.7(3) . . . . ?
C7 C9 C14 C13 178.4(2) . . . . ?
C12 C13 C15 C16 -136.7(2) . . . . ?
C14 C13 C15 C16 39.6(3) . . . . ?
C12 C13 C15 C22 40.3(3) . . . . ?
C14 C13 C15 C22 -143.5(2) . . . . ?
C22 C15 C16 C17 1.5(3) . . . . ?
C13 C15 C16 C17 178.6(2) . . . . ?
C15 C16 C17 C19 -1.6(3) . . . . ?
C15 C16 C17 C18 -177.4(2) . . . . ?
C19 C17 C18 O6 24.4(4) . . . . ?
C16 C17 C18 O6 -159.7(3) . . . . ?
C19 C17 C18 O5 -154.3(2) . . . . ?
C16 C17 C18 O5 21.5(3) . . . . ?
C16 C17 C19 C20 -0.1(3) . . . . ?
C18 C17 C19 C20 175.8(2) . . . . ?
C17 C19 C20 C22 1.8(3) . . . . ?
C17 C19 C20 C21 -175.9(2) . . . . ?
C19 C20 C21 O7 -165.8(3) . . . . ?
C22 C20 C21 O7 16.4(4) . . . . ?
C19 C20 C21 O8 16.8(3) . . . . ?
C22 C20 C21 O8 -161.0(2) . . . . ?
C19 C20 C22 C15 -1.9(4) . . . . ?
C21 C20 C22 C15 175.9(2) . . . . ?
C16 C15 C22 C20 0.2(3) . . . . ?
C13 C15 C22 C20 -176.8(2) . . . . ?
C27 N2 C23 C24 -0.5(3) . . . . ?
Co1 N2 C23 C24 -171.17(18) . . . . ?
N2 C23 C24 C25 -1.0(4) . . . . ?
C23 C24 C25 C26 1.4(4) . . . . ?
C24 C25 C26 C27 -0.4(4) . . . . ?
C24 C25 C26 C28 -178.9(3) . . . . ?
C23 N2 C27 C26 1.6(3) . . . . ?
Co1 N2 C27 C26 173.59(17) . . . . ?
C23 N2 C27 C31 -179.15(19) . . . . ?
Co1 N2 C27 C31 -7.1(2) . . . . ?
C25 C26 C27 N2 -1.1(3) . . . . ?
C28 C26 C27 N2 177.5(2) . . . . ?
C25 C26 C27 C31 179.6(2) . . . . ?
C28 C26 C27 C31 -1.8(3) . . . . ?
C25 C26 C28 C29 177.6(3) . . . . ?
C27 C26 C28 C29 -0.9(4) . . . . ?
C26 C28 C29 C30 1.5(4) . . . . ?
C28 C29 C30 C31 0.7(4) . . . . ?
C28 C29 C30 C32 179.6(3) . . . . ?
C34 N1 C31 C30 1.9(3) . . . . ?
Co1 N1 C31 C30 -179.72(17) . . . . ?
C34 N1 C31 C27 -178.23(19) . . . . ?
Co1 N1 C31 C27 0.2(2) . . . . ?
C32 C30 C31 N1 -2.5(3) . . . . ?
C29 C30 C31 N1 176.5(2) . . . . ?
C32 C30 C31 C27 177.6(2) . . . . ?
C29 C30 C31 C27 -3.4(3) . . . . ?
N2 C27 C31 N1 4.8(3) . . . . ?
C26 C27 C31 N1 -175.9(2) . . . . ?
N2 C27 C31 C30 -175.4(2) . . . . ?
C26 C27 C31 C30 4.0(3) . . . . ?
C31 C30 C32 C33 1.2(4) . . . . ?
C29 C30 C32 C33 -177.8(3) . . . . ?
C30 C32 C33 C34 0.7(4) . . . . ?
C31 N1 C34 C33 0.2(3) . . . . ?
Co1 N1 C34 C33 -178.00(18) . . . . ?
C32 C33 C34 N1 -1.4(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.048
_database_code_depnum_ccdc_archive 'CCDC 1009778'
