# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               J.Mater.Chem.
_journal_coden_cambridge         1145
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_name        'Ming-Xing Li'
_publ_contact_author_email       mx_li@mail.shu.edu.cn
loop_
_publ_author_name
'Peng Yang'
'Xiang He'
'Ming-Xing Li'
QiongYe
Jia-ZhenGe
'Zhao Wang'
'Shourong Zhu'
'Hong-Ling Cai'
'Ren-Gen Xiong'

data_100917a_0m
_database_code_depnum_ccdc_archive 'CCDC 846800'
#TrackingRef '- complex 1-cif.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H52 Mn2 N8 O12'
_chemical_formula_weight         994.82
_chemical_absolute_configuration unk

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           Monoclinic
_symmetry_space_group_name_H-M   C2

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

_cell_length_a                   21.756(4)
_cell_length_b                   11.090(2)
_cell_length_c                   11.085(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 119.155(2)
_cell_angle_gamma                90.00
_cell_volume                     2335.7(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3708
_cell_measurement_theta_min      2.60
_cell_measurement_theta_max      27.30

_exptl_crystal_description       ?
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1036
_exptl_absorpt_coefficient_mu    0.610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8381
_exptl_absorpt_correction_T_max  0.8624
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6076
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.10
_diffrn_reflns_theta_max         25.04
_reflns_number_total             3666
_reflns_number_gt                3480
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0276P)^2^+0.2027P] where P=(Fo^2^+2Fc^2^)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.016(13)
_refine_ls_number_reflns         3666
_refine_ls_number_parameters     304
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0246
_refine_ls_wR_factor_ref         0.0632
_refine_ls_wR_factor_gt          0.0621
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 1.0000 0.75381(4) 1.0000 0.03326(12) Uani 1 2 d S . .
Mn2 Mn 0.5000 0.76950(4) 0.5000 0.03263(12) Uani 1 2 d S . .
C1 C 0.87863(12) 0.5822(2) 0.9464(3) 0.0412(5) Uani 1 1 d . . .
C2 C 0.81137(10) 0.52110(18) 0.8400(2) 0.0358(5) Uani 1 1 d . . .
H2 H 0.8198 0.4888 0.7670 0.043 Uiso 1 1 calc R . .
C3 C 0.74787(10) 0.61178(19) 0.7712(2) 0.0345(5) Uani 1 1 d . . .
C4 C 0.68385(11) 0.52519(19) 0.7264(2) 0.0367(5) Uani 1 1 d . . .
C5 C 0.70957(12) 0.4409(2) 0.8518(3) 0.0493(6) Uani 1 1 d . . .
H5A H 0.7049 0.4793 0.9256 0.059 Uiso 1 1 calc R . .
H5B H 0.6828 0.3664 0.8266 0.059 Uiso 1 1 calc R . .
C6 C 0.78651(12) 0.4167(2) 0.8965(3) 0.0484(6) Uani 1 1 d . . .
H6A H 0.7915 0.3405 0.8593 0.058 Uiso 1 1 calc R . .
H6B H 0.8141 0.4136 0.9965 0.058 Uiso 1 1 calc R . .
C7 C 0.74720(13) 0.6811(3) 0.6515(3) 0.0598(7) Uani 1 1 d . . .
H7A H 0.7050 0.7285 0.6061 0.090 Uiso 1 1 calc R . .
H7B H 0.7486 0.6252 0.5869 0.090 Uiso 1 1 calc R . .
H7C H 0.7875 0.7332 0.6863 0.090 Uiso 1 1 calc R . .
C8 C 0.75063(13) 0.7047(2) 0.8753(3) 0.0563(7) Uani 1 1 d . . .
H8A H 0.7913 0.7551 0.9039 0.084 Uiso 1 1 calc R . .
H8B H 0.7534 0.6640 0.9542 0.084 Uiso 1 1 calc R . .
H8C H 0.7089 0.7535 0.8332 0.084 Uiso 1 1 calc R . .
C9 C 0.67015(15) 0.4494(3) 0.6002(3) 0.0646(8) Uani 1 1 d . . .
H9A H 0.6331 0.3927 0.5808 0.097 Uiso 1 1 calc R . .
H9B H 0.7122 0.4066 0.6189 0.097 Uiso 1 1 calc R . .
H9C H 0.6565 0.5013 0.5219 0.097 Uiso 1 1 calc R . .
C10 C 0.61700(11) 0.5944(2) 0.6955(3) 0.0427(5) Uani 1 1 d . . .
C11 C 0.97711(12) 0.8985(2) 0.7418(2) 0.0451(6) Uani 1 1 d . . .
H11 H 0.9813 0.9235 0.6661 0.054 Uiso 1 1 calc R . .
C12 C 0.93661(11) 0.9696(2) 0.7898(2) 0.0413(5) Uani 1 1 d . . .
C13 C 0.91221(13) 1.0836(2) 0.7365(3) 0.0529(6) Uani 1 1 d . . .
H13 H 0.9198 1.1152 0.6672 0.063 Uiso 1 1 calc R . .
C14 C 0.87645(15) 1.1489(2) 0.7884(3) 0.0640(7) Uani 1 1 d . . .
H14 H 0.8602 1.2261 0.7555 0.077 Uiso 1 1 calc R . .
C15 C 0.86500(14) 1.0991(2) 0.8892(3) 0.0567(7) Uani 1 1 d . . .
H15 H 0.8400 1.1410 0.9240 0.068 Uiso 1 1 calc R . .
C16 C 0.89130(12) 0.9863(2) 0.9371(3) 0.0463(6) Uani 1 1 d . . .
H16 H 0.8842 0.9534 1.0065 0.056 Uiso 1 1 calc R . .
C17 C 0.53457(12) 0.9169(2) 0.3010(2) 0.0453(5) Uani 1 1 d . . .
H17 H 0.5316 0.9472 0.2201 0.054 Uiso 1 1 calc R . .
C18 C 0.57938(12) 0.97436(19) 0.4334(2) 0.0406(5) Uani 1 1 d . . .
C19 C 0.62145(14) 1.0706(2) 0.4426(3) 0.0566(7) Uani 1 1 d . . .
H19 H 0.6207 1.1015 0.3639 0.068 Uiso 1 1 calc R . .
C20 C 0.66457(16) 1.1203(2) 0.5703(3) 0.0675(8) Uani 1 1 d . . .
H20 H 0.6942 1.1841 0.5794 0.081 Uiso 1 1 calc R . .
C21 C 0.66334(15) 1.0746(3) 0.6835(3) 0.0649(8) Uani 1 1 d . . .
H21 H 0.6917 1.1077 0.7705 0.078 Uiso 1 1 calc R . .
C22 C 0.61963(13) 0.9792(2) 0.6670(3) 0.0478(6) Uani 1 1 d . . .
H22 H 0.6185 0.9493 0.7443 0.057 Uiso 1 1 calc R . .
N1 N 1.00637(10) 0.80245(17) 0.8053(2) 0.0416(5) Uani 1 1 d . . .
N2 N 0.92679(10) 0.92080(18) 0.8895(2) 0.0390(4) Uani 1 1 d . . .
N3 N 0.49953(10) 0.82408(18) 0.29850(19) 0.0408(4) Uani 1 1 d . . .
N4 N 0.57865(10) 0.92737(17) 0.5445(2) 0.0391(4) Uani 1 1 d . . .
O1 O 0.91448(9) 0.63643(16) 0.9018(2) 0.0487(4) Uani 1 1 d . . .
O2 O 0.89408(9) 0.57805(18) 1.07055(18) 0.0617(5) Uani 1 1 d . . .
O3 O 0.58541(9) 0.64896(17) 0.58100(19) 0.0498(4) Uani 1 1 d . . .
O4 O 0.59781(10) 0.59461(19) 0.7842(2) 0.0705(6) Uani 1 1 d . . .
O5 O 1.04354(10) 0.74321(19) 0.75277(18) 0.0625(5) Uani 1 1 d . . .
H5 H 1.0623 0.6832 0.7996 0.094 Uiso 1 1 calc R . .
O6 O 0.45787(9) 0.77871(19) 0.16869(16) 0.0596(5) Uani 1 1 d . . .
H6 H 0.4379 0.7178 0.1737 0.089 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.0276(2) 0.0424(3) 0.0327(2) 0.000 0.01701(18) 0.000
Mn2 0.0263(2) 0.0382(3) 0.0316(2) 0.000 0.01269(17) 0.000
C1 0.0307(11) 0.0393(12) 0.0485(15) 0.0099(10) 0.0153(11) 0.0066(10)
C2 0.0306(11) 0.0347(11) 0.0410(13) 0.0037(9) 0.0167(10) 0.0031(9)
C3 0.0293(11) 0.0337(11) 0.0408(12) 0.0030(9) 0.0172(10) 0.0006(8)
C4 0.0311(11) 0.0341(11) 0.0428(13) 0.0008(9) 0.0162(10) 0.0002(9)
C5 0.0388(12) 0.0430(13) 0.0658(16) 0.0180(11) 0.0252(12) 0.0024(10)
C6 0.0388(13) 0.0398(12) 0.0615(15) 0.0118(11) 0.0203(12) 0.0021(10)
C7 0.0456(15) 0.0678(18) 0.0699(19) 0.0341(15) 0.0313(14) 0.0119(13)
C8 0.0431(14) 0.0471(14) 0.0683(18) -0.0148(13) 0.0189(13) 0.0026(11)
C9 0.0553(17) 0.0548(16) 0.0604(18) -0.0213(14) 0.0100(14) 0.0044(13)
C10 0.0293(12) 0.0389(12) 0.0544(15) 0.0075(11) 0.0160(12) -0.0004(9)
C11 0.0435(13) 0.0600(15) 0.0343(13) 0.0064(11) 0.0210(11) -0.0004(11)
C12 0.0371(12) 0.0501(14) 0.0342(12) 0.0019(10) 0.0154(10) -0.0027(10)
C13 0.0597(16) 0.0514(14) 0.0465(14) 0.0081(11) 0.0251(13) -0.0003(12)
C14 0.079(2) 0.0449(14) 0.0653(19) 0.0082(13) 0.0331(16) 0.0143(14)
C15 0.0596(17) 0.0547(16) 0.0551(16) -0.0003(13) 0.0275(14) 0.0160(13)
C16 0.0424(14) 0.0574(15) 0.0404(13) 0.0038(11) 0.0211(11) 0.0065(11)
C17 0.0469(14) 0.0528(14) 0.0417(13) 0.0034(11) 0.0259(11) -0.0016(11)
C18 0.0420(12) 0.0375(12) 0.0486(14) 0.0034(10) 0.0270(11) 0.0013(9)
C19 0.0644(16) 0.0451(14) 0.0751(19) 0.0009(13) 0.0455(16) -0.0078(12)
C20 0.075(2) 0.0515(16) 0.089(2) -0.0204(16) 0.0509(19) -0.0293(15)
C21 0.0612(18) 0.0644(17) 0.073(2) -0.0306(15) 0.0362(16) -0.0252(14)
C22 0.0475(14) 0.0542(14) 0.0442(14) -0.0098(11) 0.0243(12) -0.0076(11)
N1 0.0365(10) 0.0552(13) 0.0372(10) -0.0045(9) 0.0211(9) 0.0011(8)
N2 0.0354(10) 0.0471(11) 0.0357(11) 0.0031(9) 0.0182(9) 0.0037(8)
N3 0.0355(10) 0.0492(11) 0.0359(11) -0.0027(8) 0.0160(9) 0.0007(8)
N4 0.0362(10) 0.0412(11) 0.0401(11) -0.0018(9) 0.0187(9) -0.0035(8)
O1 0.0341(9) 0.0581(11) 0.0548(11) -0.0013(9) 0.0224(8) -0.0088(8)
O2 0.0596(11) 0.0723(12) 0.0397(10) 0.0042(9) 0.0137(9) -0.0167(10)
O3 0.0330(9) 0.0554(11) 0.0528(11) 0.0083(9) 0.0144(8) 0.0098(8)
O4 0.0634(12) 0.0850(14) 0.0888(15) 0.0389(12) 0.0570(12) 0.0316(11)
O5 0.0656(11) 0.0842(14) 0.0540(11) 0.0045(10) 0.0418(10) 0.0219(11)
O6 0.0583(10) 0.0767(13) 0.0358(8) -0.0129(9) 0.0168(8) -0.0151(10)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O1 2.0900(17) 2_757 ?
Mn1 O1 2.0900(17) . ?
Mn1 N1 2.2929(19) 2_757 ?
Mn1 N1 2.2929(19) . ?
Mn1 N2 2.359(2) 2_757 ?
Mn1 N2 2.359(2) . ?
Mn2 O3 2.1025(16) . ?
Mn2 O3 2.1025(16) 2_656 ?
Mn2 N3 2.3093(19) 2_656 ?
Mn2 N3 2.3094(19) . ?
Mn2 N4 2.327(2) . ?
Mn2 N4 2.3269(19) 2_656 ?
C1 O2 1.248(3) . ?
C1 O1 1.261(3) . ?
C1 C2 1.520(3) . ?
C2 C6 1.535(3) . ?
C2 C3 1.573(3) . ?
C2 H2 0.9800 . ?
C3 C8 1.526(3) . ?
C3 C7 1.527(3) . ?
C3 C4 1.560(3) . ?
C4 C10 1.528(3) . ?
C4 C9 1.531(3) . ?
C4 C5 1.537(3) . ?
C5 C6 1.520(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 O4 1.241(3) . ?
C10 O3 1.265(3) . ?
C11 N1 1.265(3) . ?
C11 C12 1.462(3) . ?
C11 H11 0.9300 . ?
C12 N2 1.338(3) . ?
C12 C13 1.387(3) . ?
C13 C14 1.377(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.373(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.371(3) . ?
C15 H15 0.9300 . ?
C16 N2 1.342(3) . ?
C16 H16 0.9300 . ?
C17 N3 1.273(3) . ?
C17 C18 1.455(3) . ?
C17 H17 0.9300 . ?
C18 N4 1.344(3) . ?
C18 C19 1.377(3) . ?
C19 C20 1.375(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.366(4) . ?
C20 H20 0.9300 . ?
C21 C22 1.375(4) . ?
C21 H21 0.9300 . ?
C22 N4 1.338(3) . ?
C22 H22 0.9300 . ?
N1 O5 1.373(2) . ?
N3 O6 1.369(2) . ?
O5 H5 0.8200 . ?
O6 H6 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mn1 O1 102.95(10) 2_757 . ?
O1 Mn1 N1 95.93(7) 2_757 2_757 ?
O1 Mn1 N1 100.94(7) . 2_757 ?
O1 Mn1 N1 100.94(7) 2_757 . ?
O1 Mn1 N1 95.93(7) . . ?
N1 Mn1 N1 152.79(10) 2_757 . ?
O1 Mn1 N2 90.81(7) 2_757 2_757 ?
O1 Mn1 N2 164.55(7) . 2_757 ?
N1 Mn1 N2 70.24(7) 2_757 2_757 ?
N1 Mn1 N2 88.21(7) . 2_757 ?
O1 Mn1 N2 164.55(7) 2_757 . ?
O1 Mn1 N2 90.81(7) . . ?
N1 Mn1 N2 88.21(7) 2_757 . ?
N1 Mn1 N2 70.24(7) . . ?
N2 Mn1 N2 76.56(10) 2_757 . ?
O3 Mn2 O3 101.04(10) . 2_656 ?
O3 Mn2 N3 99.62(7) . 2_656 ?
O3 Mn2 N3 99.57(7) 2_656 2_656 ?
O3 Mn2 N3 99.57(7) . . ?
O3 Mn2 N3 99.62(7) 2_656 . ?
N3 Mn2 N3 149.61(10) 2_656 . ?
O3 Mn2 N4 88.98(7) . . ?
O3 Mn2 N4 167.06(7) 2_656 . ?
N3 Mn2 N4 86.65(7) 2_656 . ?
N3 Mn2 N4 70.36(7) . . ?
O3 Mn2 N4 167.06(7) . 2_656 ?
O3 Mn2 N4 88.98(7) 2_656 2_656 ?
N3 Mn2 N4 70.37(7) 2_656 2_656 ?
N3 Mn2 N4 86.65(6) . 2_656 ?
N4 Mn2 N4 82.40(10) . 2_656 ?
O2 C1 O1 124.3(2) . . ?
O2 C1 C2 118.6(2) . . ?
O1 C1 C2 117.0(2) . . ?
C1 C2 C6 114.65(19) . . ?
C1 C2 C3 112.15(17) . . ?
C6 C2 C3 106.21(16) . . ?
C1 C2 H2 107.9 . . ?
C6 C2 H2 107.9 . . ?
C3 C2 H2 107.9 . . ?
C8 C3 C7 107.3(2) . . ?
C8 C3 C4 110.87(17) . . ?
C7 C3 C4 113.83(19) . . ?
C8 C3 C2 111.30(18) . . ?
C7 C3 C2 112.18(17) . . ?
C4 C3 C2 101.40(16) . . ?
C10 C4 C9 109.29(19) . . ?
C10 C4 C5 113.29(18) . . ?
C9 C4 C5 108.4(2) . . ?
C10 C4 C3 111.52(17) . . ?
C9 C4 C3 112.02(19) . . ?
C5 C4 C3 102.19(17) . . ?
C6 C5 C4 105.06(18) . . ?
C6 C5 H5A 110.7 . . ?
C4 C5 H5A 110.7 . . ?
C6 C5 H5B 110.7 . . ?
C4 C5 H5B 110.7 . . ?
H5A C5 H5B 108.8 . . ?
C5 C6 C2 106.56(18) . . ?
C5 C6 H6A 110.4 . . ?
C2 C6 H6A 110.4 . . ?
C5 C6 H6B 110.4 . . ?
C2 C6 H6B 110.4 . . ?
H6A C6 H6B 108.6 . . ?
C3 C7 H7A 109.5 . . ?
C3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O4 C10 O3 124.4(2) . . ?
O4 C10 C4 118.3(2) . . ?
O3 C10 C4 117.2(2) . . ?
N1 C11 C12 118.8(2) . . ?
N1 C11 H11 120.6 . . ?
C12 C11 H11 120.6 . . ?
N2 C12 C13 122.6(2) . . ?
N2 C12 C11 116.7(2) . . ?
C13 C12 C11 120.7(2) . . ?
C14 C13 C12 118.6(2) . . ?
C14 C13 H13 120.7 . . ?
C12 C13 H13 120.7 . . ?
C15 C14 C13 119.4(2) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C16 C15 C14 118.4(2) . . ?
C16 C15 H15 120.8 . . ?
C14 C15 H15 120.8 . . ?
N2 C16 C15 123.6(2) . . ?
N2 C16 H16 118.2 . . ?
C15 C16 H16 118.2 . . ?
N3 C17 C18 118.4(2) . . ?
N3 C17 H17 120.8 . . ?
C18 C17 H17 120.8 . . ?
N4 C18 C19 122.5(2) . . ?
N4 C18 C17 116.94(19) . . ?
C19 C18 C17 120.6(2) . . ?
C20 C19 C18 118.8(3) . . ?
C20 C19 H19 120.6 . . ?
C18 C19 H19 120.6 . . ?
C21 C20 C19 119.2(2) . . ?
C21 C20 H20 120.4 . . ?
C19 C20 H20 120.4 . . ?
C20 C21 C22 119.1(3) . . ?
C20 C21 H21 120.5 . . ?
C22 C21 H21 120.5 . . ?
N4 C22 C21 122.8(2) . . ?
N4 C22 H22 118.6 . . ?
C21 C22 H22 118.6 . . ?
C11 N1 O5 114.07(19) . . ?
C11 N1 Mn1 118.50(15) . . ?
O5 N1 Mn1 127.24(15) . . ?
C12 N2 C16 117.4(2) . . ?
C12 N2 Mn1 114.02(14) . . ?
C16 N2 Mn1 126.41(16) . . ?
C17 N3 O6 113.75(19) . . ?
C17 N3 Mn2 118.07(15) . . ?
O6 N3 Mn2 127.51(14) . . ?
C22 N4 C18 117.7(2) . . ?
C22 N4 Mn2 126.55(16) . . ?
C18 N4 Mn2 115.68(15) . . ?
C1 O1 Mn1 131.05(18) . . ?
C10 O3 Mn2 131.92(16) . . ?
N1 O5 H5 109.5 . . ?
N3 O6 H6 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O6 H6 O4 0.82 1.74 2.554(3) 169.7 2_656
O5 H5 O2 0.82 1.73 2.538(3) 167.1 2_757

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.04
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.032

# Attachment '- complex 2.cif.cif'

data_101129b_0m
_database_code_depnum_ccdc_archive 'CCDC 846801'
#TrackingRef '- complex 2.cif.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H64 Co2 N12 O16'
_chemical_formula_sum            'C44 H64 Co2 N12 O16'
_chemical_formula_weight         1134.93

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   P21

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

_cell_length_a                   7.521(12)
_cell_length_b                   17.21(3)
_cell_length_c                   19.15(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.26(2)
_cell_angle_gamma                90.00
_cell_volume                     2468(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1595
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      18.80

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1188
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8636
_exptl_absorpt_correction_T_max  0.8636
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(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  .
_diffrn_measurement_method       .
_diffrn_detector_area_resol_mean .
_diffrn_standards_number         .
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            12048
_diffrn_reflns_av_R_equivalents  0.0909
_diffrn_reflns_av_sigmaI/netI    0.2067
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8390
_reflns_number_gt                3866
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0115P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0211(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_number_reflns         8390
_refine_ls_number_parameters     674
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1661
_refine_ls_R_factor_gt           0.0738
_refine_ls_wR_factor_ref         0.1502
_refine_ls_wR_factor_gt          0.1243
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O6W O 0.8699(12) 0.2371(4) 0.3993(5) 0.091(3) Uani 1 1 d . . .
H7WA H 1.0090 0.0650 0.4222 0.110 Uiso 1 1 d R . .
O7W O 0.9390(18) 0.0365(7) 0.4387(6) 0.161(5) Uani 1 1 d . . .
N7 N 1.3555(14) 0.0673(5) 0.5207(4) 0.051(3) Uani 1 1 d . . .
C13 C 1.3818(18) 0.0084(6) 0.4761(5) 0.054(3) Uani 1 1 d . . .
C14 C 1.3564(19) -0.0659(6) 0.4911(6) 0.067(4) Uani 1 1 d . . .
C17 C 1.3031(15) 0.0465(5) 0.5809(4) 0.042(3) Uani 1 1 d D . .
C15 C 1.3019(17) -0.0860(5) 0.5546(5) 0.050(3) Uani 1 1 d . . .
C16 C 1.2752(16) -0.0293(5) 0.6029(5) 0.042(3) Uani 1 1 d . . .
N1 N 0.3180(13) 0.2991(4) 0.4289(4) 0.043(2) Uani 1 1 d . . .
C18 C 1.2197(15) -0.0549(5) 0.6683(5) 0.038(3) Uani 1 1 d . . .
N10 N 1.1970(12) -0.0144(4) 0.7290(4) 0.040(2) Uani 1 1 d . . .
N9 N 1.1165(12) -0.1334(4) 0.7465(4) 0.045(2) Uani 1 1 d . . .
C19 C 1.1416(15) -0.0640(5) 0.7772(5) 0.041(3) Uani 1 1 d . . .
C20 C 1.1088(15) -0.0480(5) 0.8476(5) 0.040(3) Uani 1 1 d . . .
C22 C 1.1255(16) -0.0892(5) 0.9669(6) 0.048(3) Uani 1 1 d . . .
C23 C 1.0683(17) -0.0162(7) 0.9829(5) 0.056(3) Uani 1 1 d . . .
C24 C 1.0466(15) 0.0223(5) 0.8686(5) 0.042(3) Uani 1 1 d . . .
N12 N 1.0220(12) 0.0397(4) 0.9352(4) 0.040(2) Uani 1 1 d . . .
Co1 Co 0.3555(2) 0.18619(7) 0.48355(7) 0.0448(5) Uani 1 1 d . . .
Co2 Co 0.9342(2) 0.15074(7) 0.95755(6) 0.0430(5) Uani 1 1 d . . .
O1 O 0.5308(11) 0.2246(4) 0.5640(3) 0.058(2) Uani 1 1 d . . .
O1W O 0.5682(10) 0.1632(3) 0.4277(3) 0.053(2) Uani 1 1 d . . .
O2 O 0.3529(13) 0.2919(4) 0.6269(4) 0.068(3) Uani 1 1 d . . .
O2W O 0.1404(11) 0.2148(4) 0.5382(4) 0.061(2) Uani 1 1 d . . .
O3 O 0.8138(11) 0.2859(4) 0.9011(4) 0.065(2) Uani 1 1 d . . .
O3W O 0.1833(10) 0.1435(4) 0.3969(3) 0.052(2) Uani 1 1 d . . .
O4 O 0.9118(11) 0.1778(4) 0.8583(3) 0.055(2) Uani 1 1 d . . .
O5 O 0.6975(10) 0.1262(4) 0.9932(4) 0.055(2) Uani 1 1 d . . .
O6 O 0.9230(11) 0.1164(4) 1.0667(4) 0.053(2) Uani 1 1 d . . .
O7 O 0.5553(12) 0.0608(4) 1.3290(4) 0.064(2) Uani 1 1 d . . .
O8 O 0.3312(11) 0.1296(4) 1.2805(3) 0.057(2) Uani 1 1 d . . .
N2 N 0.4231(14) 0.4256(5) 0.2189(4) 0.053(3) Uani 1 1 d . . .
N3 N 0.4172(13) 0.4073(4) 0.1477(4) 0.053(3) Uani 1 1 d . . .
N4 N 0.2729(12) 0.3186(4) 0.1992(4) 0.035(2) Uani 1 1 d . . .
N5 N 0.1543(12) 0.2583(4) 0.2089(3) 0.047(3) Uani 1 1 d D . .
H5A H 0.1112 0.2327 0.1727 0.057 Uiso 1 1 d R . .
H5B H 0.1254 0.2458 0.2499 0.057 Uiso 1 1 d R . .
N6 N 0.1548(13) 0.2176(4) -0.0121(4) 0.048(3) Uani 1 1 d . . .
N8 N 1.1627(13) -0.1260(4) 0.6782(4) 0.050(3) Uani 1 1 d . . .
N11 N 1.2720(13) 0.0602(4) 0.7428(3) 0.059(3) Uani 1 1 d D . .
H11A H 1.2865 0.0782 0.7848 0.071 Uiso 1 1 d R . .
H11B H 1.3037 0.0874 0.7084 0.071 Uiso 1 1 d R . .
C1 C 0.2585(16) 0.3617(6) 0.4612(5) 0.052(3) Uani 1 1 d . . .
H1 H 0.2402 0.3590 0.5085 0.063 Uiso 1 1 calc R . .
C2 C 0.2237(18) 0.4315(5) 0.4241(6) 0.062(4) Uani 1 1 d . . .
H2 H 0.1821 0.4746 0.4470 0.074 Uiso 1 1 calc R . .
C3 C 0.2506(16) 0.4361(6) 0.3550(5) 0.053(3) Uani 1 1 d . . .
H3 H 0.2299 0.4823 0.3305 0.064 Uiso 1 1 calc R . .
C4 C 0.3102(15) 0.3698(5) 0.3213(5) 0.041(3) Uani 1 1 d . . .
C5 C 0.3408(15) 0.3028(5) 0.3601(5) 0.047(3) Uani 1 1 d . . .
H5 H 0.3787 0.2586 0.3379 0.056 Uiso 1 1 calc R . .
C6 C 0.3351(16) 0.3715(5) 0.2472(5) 0.043(3) Uani 1 1 d . . .
C7 C 0.3267(16) 0.3427(5) 0.1383(5) 0.042(3) Uani 1 1 d . . .
C8 C 0.3096(16) 0.3041(5) 0.0705(5) 0.039(3) Uani 1 1 d . . .
C9 C 0.4298(16) 0.3171(6) 0.0223(5) 0.050(3) Uani 1 1 d . . .
H9 H 0.5247 0.3508 0.0335 0.060 Uiso 1 1 calc R . .
C10 C 0.4136(18) 0.2818(6) -0.0415(5) 0.056(4) Uani 1 1 d . . .
H10 H 0.4943 0.2923 -0.0742 0.068 Uiso 1 1 calc R . .
C11 C 0.2792(15) 0.2316(6) -0.0562(5) 0.048(3) Uani 1 1 d . . .
H11 H 0.2719 0.2055 -0.0989 0.057 Uiso 1 1 calc R . .
C12 C 0.1700(16) 0.2521(5) 0.0476(4) 0.049(3) Uani 1 1 d D . .
H12 H 0.0831 0.2423 0.0781 0.059 Uiso 1 1 calc R . .
H13 H 1.4217 0.0206 0.4340 0.059 Uiso 1 1 d R . .
H14 H 1.3721 -0.1047 0.4585 0.059 Uiso 1 1 d R . .
H15 H 1.2821 -0.1394 0.5658 0.059 Uiso 1 1 d R . .
H17 H 1.2912 0.0848 0.6140 0.059 Uiso 1 1 d R . .
C21 C 1.1408(15) -0.1047(5) 0.8973(5) 0.046(3) Uani 1 1 d . . .
H21 H 1.1734 -0.1542 0.8838 0.055 Uiso 1 1 calc R . .
H22 H 1.1500 -0.1244 1.0004 0.055 Uiso 1 1 d R . .
H23 H 1.0521 -0.0026 1.0293 0.055 Uiso 1 1 d R . .
H24 H 1.0172 0.0618 0.8346 0.055 Uiso 1 1 d R . .
C25 C 0.501(2) 0.2692(6) 0.6158(6) 0.055(4) Uani 1 1 d . . .
C26 C 0.6734(19) 0.2878(5) 0.6651(5) 0.063(4) Uani 1 1 d . . .
H26 H 0.7793 0.2850 0.6389 0.076 Uiso 1 1 calc R . .
C27 C 0.656(2) 0.3711(6) 0.6978(6) 0.098(6) Uani 1 1 d . . .
H27A H 0.7061 0.4106 0.6691 0.117 Uiso 1 1 calc R . .
H27B H 0.5325 0.3838 0.7031 0.117 Uiso 1 1 calc R . .
C28 C 0.768(2) 0.3633(6) 0.7713(5) 0.080(5) Uani 1 1 d . . .
H28A H 0.6941 0.3754 0.8088 0.096 Uiso 1 1 calc R . .
H28B H 0.8688 0.3986 0.7743 0.096 Uiso 1 1 calc R . .
C29 C 0.8339(15) 0.2773(5) 0.7774(5) 0.039(3) Uani 1 1 d . . .
C30 C 0.6946(18) 0.2320(6) 0.7308(6) 0.050(3) Uani 1 1 d . . .
C31 C 0.7499(19) 0.1509(6) 0.7092(5) 0.077(4) Uani 1 1 d . . .
H31A H 0.8433 0.1549 0.6784 0.116 Uiso 1 1 calc R . .
H31B H 0.6490 0.1248 0.6854 0.116 Uiso 1 1 calc R . .
H31C H 0.7923 0.1218 0.7502 0.116 Uiso 1 1 calc R . .
C32 C 0.5209(18) 0.2262(6) 0.7652(6) 0.073(4) Uani 1 1 d . . .
H32A H 0.5385 0.1941 0.8063 0.109 Uiso 1 1 calc R . .
H32B H 0.4304 0.2036 0.7328 0.109 Uiso 1 1 calc R . .
H32C H 0.4840 0.2772 0.7782 0.109 Uiso 1 1 calc R . .
C33 C 1.0138(19) 0.2741(7) 0.7522(6) 0.082(4) Uani 1 1 d . . .
H33A H 1.0943 0.3058 0.7817 0.123 Uiso 1 1 calc R . .
H33B H 1.0082 0.2930 0.7049 0.123 Uiso 1 1 calc R . .
H33C H 1.0557 0.2214 0.7536 0.123 Uiso 1 1 calc R . .
C34 C 0.8526(14) 0.2481(7) 0.8510(5) 0.042(3) Uani 1 1 d . . .
C35 C 0.764(2) 0.1068(5) 1.0556(5) 0.050(4) Uani 1 1 d . . .
C36 C 0.6523(15) 0.0632(5) 1.1016(4) 0.038(3) Uani 1 1 d . . .
C37 C 0.4436(16) 0.0710(6) 1.0787(5) 0.056(3) Uani 1 1 d . . .
H37A H 0.4152 0.1218 1.0588 0.067 Uiso 1 1 calc R . .
H37B H 0.4039 0.0314 1.0447 0.067 Uiso 1 1 calc R . .
C38 C 0.3586(17) 0.0595(6) 1.1473(5) 0.057(4) Uani 1 1 d . . .
H38A H 0.2810 0.1030 1.1552 0.069 Uiso 1 1 calc R . .
H38B H 0.2872 0.0125 1.1448 0.069 Uiso 1 1 calc R . .
C39 C 0.5029(15) 0.0536(5) 1.2066(5) 0.042(3) Uani 1 1 d . . .
H39 H 0.5294 -0.0018 1.2131 0.051 Uiso 1 1 calc R . .
C40 C 0.6674(15) 0.0905(5) 1.1789(5) 0.042(3) Uani 1 1 d . . .
C41 C 0.4622(18) 0.0838(6) 1.2752(6) 0.047(3) Uani 1 1 d . . .
C42 C 0.702(2) -0.0236(5) 1.0949(6) 0.087(5) Uani 1 1 d . . .
H42A H 0.6962 -0.0376 1.0462 0.131 Uiso 1 1 calc R . .
H42B H 0.6194 -0.0550 1.1180 0.131 Uiso 1 1 calc R . .
H42C H 0.8207 -0.0321 1.1163 0.131 Uiso 1 1 calc R . .
C43 C 0.8449(17) 0.0676(7) 1.2181(6) 0.077(4) Uani 1 1 d . . .
H43A H 0.8437 0.0804 1.2668 0.115 Uiso 1 1 calc R . .
H43B H 0.9399 0.0953 1.1988 0.115 Uiso 1 1 calc R . .
H43C H 0.8631 0.0127 1.2132 0.115 Uiso 1 1 calc R . .
C44 C 0.6504(18) 0.1816(5) 1.1787(5) 0.065(4) Uani 1 1 d . . .
H44A H 0.5579 0.1972 1.1437 0.098 Uiso 1 1 calc R . .
H44B H 0.7617 0.2043 1.1685 0.098 Uiso 1 1 calc R . .
H44C H 0.6212 0.1990 1.2239 0.098 Uiso 1 1 calc R . .
O4W O 0.8499(12) 0.1254(5) 0.5497(4) 0.099(3) Uani 1 1 d . . .
H4WA H 0.9405 0.1543 0.5466 0.119 Uiso 1 1 d R . .
H4WB H 0.7598 0.1542 0.5541 0.119 Uiso 1 1 d R . .
O5W O 0.4551(13) 0.0602(4) 0.8874(4) 0.090(3) Uani 1 1 d . . .
H5WA H 0.5279 0.0798 0.9192 0.108 Uiso 1 1 d R . .
H5WB H 0.4930 0.0155 0.8772 0.108 Uiso 1 1 d R . .
H6WA H 0.8703 0.2795 0.3742 0.108 Uiso 1 1 d R . .
H6WB H 0.9659 0.2140 0.3960 0.108 Uiso 1 1 d R . .
H7WB H 0.8913 0.0057 0.4079 0.108 Uiso 1 1 d R . .
O8W O 0.2122(16) 0.4359(5) 0.6457(6) 0.142(5) Uani 1 1 d . . .
H8WA H 0.2645 0.3928 0.6406 0.171 Uiso 1 1 d R . .
H8WB H 0.2909 0.4711 0.6533 0.171 Uiso 1 1 d R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O6W 0.079(7) 0.048(5) 0.152(9) 0.043(5) 0.043(7) 0.014(5)
O7W 0.159(13) 0.153(11) 0.175(10) -0.018(9) 0.046(10) -0.076(10)
N7 0.080(8) 0.051(5) 0.024(5) 0.003(4) 0.017(5) 0.010(5)
C13 0.082(11) 0.049(6) 0.033(6) -0.002(5) 0.013(7) 0.006(7)
C14 0.121(13) 0.029(5) 0.054(8) -0.002(5) 0.027(8) 0.026(7)
C17 0.048(8) 0.033(6) 0.044(6) -0.001(5) 0.004(6) -0.008(6)
C15 0.082(10) 0.032(6) 0.038(6) -0.002(5) 0.018(7) 0.004(6)
C16 0.063(9) 0.048(6) 0.018(5) -0.003(4) 0.015(6) 0.007(6)
N1 0.064(7) 0.035(5) 0.031(5) -0.007(4) 0.006(5) -0.003(5)
C18 0.048(8) 0.035(6) 0.033(6) -0.007(5) 0.013(6) 0.006(5)
N10 0.052(7) 0.035(5) 0.032(5) -0.005(4) 0.012(5) -0.007(4)
N9 0.058(7) 0.024(4) 0.055(6) -0.006(4) 0.019(5) 0.002(4)
C19 0.056(9) 0.036(6) 0.034(6) 0.012(5) 0.016(6) 0.008(6)
C20 0.053(9) 0.030(5) 0.038(6) 0.009(5) 0.016(6) 0.001(5)
C22 0.065(10) 0.029(6) 0.052(7) 0.004(5) 0.012(7) 0.001(6)
C23 0.068(10) 0.072(8) 0.028(6) -0.010(6) 0.007(6) -0.021(7)
C24 0.052(9) 0.037(6) 0.040(6) 0.009(5) 0.020(6) 0.009(6)
N12 0.048(7) 0.033(5) 0.037(5) 0.015(4) 0.006(5) 0.000(4)
Co1 0.0651(12) 0.0335(7) 0.0369(8) 0.0005(6) 0.0108(8) -0.0008(8)
Co2 0.0599(12) 0.0360(7) 0.0348(8) -0.0017(7) 0.0138(8) -0.0017(8)
O1 0.093(7) 0.064(5) 0.016(4) -0.008(3) -0.008(4) -0.005(5)
O1W 0.078(6) 0.038(4) 0.042(4) -0.001(3) 0.005(4) 0.004(4)
O2 0.070(7) 0.078(6) 0.054(5) -0.026(4) -0.009(5) 0.025(6)
O2W 0.081(7) 0.049(4) 0.058(5) -0.007(3) 0.028(5) -0.001(4)
O3 0.077(7) 0.068(5) 0.053(5) -0.006(4) 0.019(5) -0.003(5)
O3W 0.077(6) 0.040(4) 0.038(4) -0.001(3) -0.002(4) -0.005(4)
O4 0.082(6) 0.032(4) 0.050(4) -0.003(3) -0.009(4) 0.002(4)
O5 0.061(6) 0.046(4) 0.057(5) 0.005(3) 0.006(5) 0.000(4)
O6 0.035(6) 0.060(5) 0.065(5) -0.005(4) 0.017(5) -0.017(4)
O7 0.093(7) 0.059(5) 0.042(5) -0.003(4) 0.005(5) 0.014(5)
O8 0.081(7) 0.045(5) 0.047(4) 0.002(3) 0.011(5) 0.022(4)
N2 0.078(8) 0.044(5) 0.039(5) 0.007(4) 0.011(6) -0.015(5)
N3 0.078(8) 0.041(5) 0.038(5) 0.007(4) 0.003(6) -0.012(5)
N4 0.047(7) 0.028(4) 0.032(5) -0.001(4) 0.014(5) -0.005(4)
N5 0.081(8) 0.037(5) 0.024(4) 0.005(3) 0.010(5) -0.029(5)
N6 0.067(8) 0.042(5) 0.037(5) -0.010(4) 0.017(5) -0.006(5)
N8 0.072(8) 0.032(5) 0.050(6) -0.003(4) 0.028(6) -0.007(5)
N11 0.122(10) 0.020(4) 0.035(5) 0.008(4) 0.001(6) -0.033(5)
C1 0.077(10) 0.034(6) 0.047(7) -0.009(5) 0.012(7) -0.003(6)
C2 0.104(12) 0.028(6) 0.053(8) -0.001(5) 0.006(8) -0.007(6)
C3 0.073(10) 0.042(6) 0.044(7) 0.001(5) 0.004(7) 0.005(6)
C4 0.048(8) 0.023(5) 0.052(7) 0.003(5) 0.000(6) -0.005(5)
C5 0.061(9) 0.031(5) 0.049(7) -0.004(5) 0.010(7) 0.001(6)
C6 0.059(9) 0.036(6) 0.035(6) 0.005(5) 0.011(6) 0.000(6)
C7 0.062(9) 0.025(5) 0.040(6) -0.004(5) 0.012(6) 0.000(6)
C8 0.045(8) 0.044(6) 0.031(6) 0.006(5) 0.012(6) 0.005(6)
C9 0.059(9) 0.050(7) 0.042(7) -0.001(5) 0.015(7) -0.017(6)
C10 0.070(10) 0.054(7) 0.048(7) 0.007(6) 0.019(7) -0.021(7)
C11 0.051(9) 0.053(7) 0.042(7) -0.002(5) 0.021(7) -0.004(6)
C12 0.053(9) 0.037(6) 0.059(7) 0.005(5) 0.018(7) -0.001(6)
C21 0.052(9) 0.028(5) 0.058(7) 0.004(5) 0.013(7) -0.008(5)
C25 0.085(12) 0.038(6) 0.040(7) 0.007(5) -0.003(8) -0.009(7)
C26 0.123(13) 0.024(5) 0.038(6) 0.007(5) -0.021(7) 0.001(7)
C27 0.187(18) 0.028(6) 0.067(8) 0.006(6) -0.046(10) -0.002(8)
C28 0.134(14) 0.036(6) 0.064(8) 0.001(5) -0.017(9) -0.002(8)
C29 0.034(8) 0.035(6) 0.050(7) -0.007(5) 0.016(6) -0.010(5)
C30 0.064(10) 0.037(6) 0.048(7) 0.003(5) 0.000(7) -0.001(6)
C31 0.129(12) 0.034(6) 0.063(7) -0.005(6) -0.029(8) 0.001(8)
C32 0.086(12) 0.057(8) 0.073(9) 0.014(6) -0.004(9) -0.006(8)
C33 0.081(13) 0.078(9) 0.087(10) 0.003(8) 0.004(10) -0.002(9)
C34 0.032(8) 0.069(8) 0.026(6) -0.014(5) 0.017(6) -0.006(6)
C35 0.103(13) 0.029(6) 0.023(6) 0.004(5) 0.032(8) -0.002(7)
C36 0.055(8) 0.035(5) 0.028(5) -0.007(4) 0.025(6) 0.001(5)
C37 0.060(10) 0.066(8) 0.045(7) -0.003(5) 0.023(7) -0.008(7)
C38 0.075(11) 0.044(6) 0.054(7) -0.008(6) 0.011(7) -0.002(7)
C39 0.068(9) 0.028(5) 0.033(6) 0.003(4) 0.020(6) -0.009(6)
C40 0.042(8) 0.032(5) 0.051(7) 0.004(5) 0.006(6) 0.001(5)
C41 0.065(10) 0.043(6) 0.036(7) 0.006(5) 0.028(7) -0.008(7)
C42 0.169(16) 0.023(6) 0.078(9) -0.006(5) 0.056(10) -0.003(8)
C43 0.081(12) 0.086(9) 0.062(8) 0.011(7) -0.002(8) -0.004(9)
C44 0.105(11) 0.030(5) 0.061(7) -0.016(5) 0.007(7) -0.017(7)
O4W 0.066(7) 0.105(7) 0.125(7) 0.019(6) 0.003(6) -0.015(6)
O5W 0.135(9) 0.050(5) 0.080(6) -0.015(4) -0.016(6) 0.017(6)
O8W 0.136(11) 0.068(6) 0.214(13) -0.022(7) -0.033(10) 0.021(7)

_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
N7 C17 1.302(10) . ?
N7 C13 1.351(12) . ?
N7 Co1 2.166(9) 1_655 ?
C13 C14 1.330(14) . ?
C14 C15 1.363(13) . ?
C17 C16 1.394(12) . ?
C15 C16 1.372(12) . ?
C16 C18 1.424(12) . ?
N1 C1 1.339(12) . ?
N1 C5 1.346(11) . ?
N1 Co1 2.213(8) . ?
C18 N8 1.316(11) . ?
C18 N10 1.379(11) . ?
N10 C19 1.351(11) . ?
N10 N11 1.417(10) . ?
N9 C19 1.336(11) . ?
N9 N8 1.391(10) . ?
C19 C20 1.420(12) . ?
C20 C21 1.368(12) . ?
C20 C24 1.370(12) . ?
C22 C21 1.376(13) . ?
C22 C23 1.372(14) . ?
C23 N12 1.350(12) . ?
C24 N12 1.340(11) . ?
N12 Co2 2.078(8) . ?
Co1 O1 2.043(7) . ?
Co1 O1W 2.043(8) . ?
Co1 O2W 2.065(8) . ?
Co1 O3W 2.139(7) . ?
Co1 N7 2.166(9) 1_455 ?
Co2 O4 1.949(7) . ?
Co2 O5 2.009(8) . ?
Co2 N6 2.058(9) 1_656 ?
O1 C25 1.291(13) . ?
O2 C25 1.219(14) . ?
O3 C34 1.217(10) . ?
O4 C34 1.293(12) . ?
O5 C35 1.296(12) . ?
O6 C35 1.207(14) . ?
O7 C41 1.256(12) . ?
O8 C41 1.272(13) . ?
N2 C6 1.289(11) . ?
N2 N3 1.396(10) . ?
N3 C7 1.307(11) . ?
N4 C7 1.335(11) . ?
N4 C6 1.347(11) . ?
N4 N5 1.393(10) . ?
N6 C12 1.285(10) . ?
N6 C11 1.339(11) . ?
N6 Co2 2.058(9) 1_454 ?
C1 C2 1.408(13) . ?
C2 C3 1.359(13) . ?
C3 C4 1.405(13) . ?
C4 C5 1.378(12) . ?
C4 C6 1.449(12) . ?
C7 C8 1.452(12) . ?
C8 C9 1.368(12) . ?
C8 C12 1.418(14) . ?
C9 C10 1.360(13) . ?
C10 C11 1.340(14) . ?
C25 C26 1.564(16) . ?
C26 C30 1.581(13) . ?
C26 C27 1.575(13) . ?
C27 C28 1.578(14) . ?
C28 C29 1.562(14) . ?
C29 C33 1.479(15) . ?
C29 C34 1.490(13) . ?
C29 C30 1.526(14) . ?
C30 C31 1.524(14) . ?
C30 C32 1.519(15) . ?
C35 C36 1.478(13) . ?
C36 C42 1.548(12) . ?
C36 C40 1.548(12) . ?
C36 C37 1.596(15) . ?
C37 C38 1.527(13) . ?
C38 C39 1.500(14) . ?
C39 C41 1.472(12) . ?
C39 C40 1.528(14) . ?
C40 C43 1.521(14) . ?
C40 C44 1.573(12) . ?

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
C17 N7 C13 115.3(8) . . ?
C17 N7 Co1 124.0(7) . 1_655 ?
C13 N7 Co1 119.7(6) . 1_655 ?
C14 C13 N7 123.6(10) . . ?
C13 C14 C15 119.8(9) . . ?
N7 C17 C16 126.3(8) . . ?
C14 C15 C16 119.8(9) . . ?
C17 C16 C15 115.2(8) . . ?
C17 C16 C18 128.3(8) . . ?
C15 C16 C18 116.5(9) . . ?
C1 N1 C5 119.5(8) . . ?
C1 N1 Co1 121.4(7) . . ?
C5 N1 Co1 118.9(6) . . ?
N8 C18 N10 106.3(8) . . ?
N8 C18 C16 122.6(8) . . ?
N10 C18 C16 130.8(9) . . ?
C19 N10 C18 109.1(8) . . ?
C19 N10 N11 126.0(7) . . ?
C18 N10 N11 122.4(8) . . ?
C19 N9 N8 107.1(7) . . ?
N9 C19 N10 107.7(8) . . ?
N9 C19 C20 124.1(9) . . ?
N10 C19 C20 128.1(9) . . ?
C21 C20 C24 118.0(9) . . ?
C21 C20 C19 119.1(9) . . ?
C24 C20 C19 122.9(9) . . ?
C21 C22 C23 116.7(9) . . ?
N12 C23 C22 124.7(9) . . ?
N12 C24 C20 123.9(8) . . ?
C24 N12 C23 115.7(8) . . ?
C24 N12 Co2 118.4(6) . . ?
C23 N12 Co2 125.7(7) . . ?
O1 Co1 O1W 88.6(3) . . ?
O1 Co1 O2W 91.3(3) . . ?
O1W Co1 O2W 177.3(3) . . ?
O1 Co1 O3W 177.0(3) . . ?
O1W Co1 O3W 88.5(3) . . ?
O2W Co1 O3W 91.6(3) . . ?
O1 Co1 N7 94.4(3) . 1_455 ?
O1W Co1 N7 90.7(3) . 1_455 ?
O2W Co1 N7 92.0(3) . 1_455 ?
O3W Co1 N7 85.0(3) . 1_455 ?
O1 Co1 N1 96.8(3) . . ?
O1W Co1 N1 89.7(3) . . ?
O2W Co1 N1 87.6(3) . . ?
O3W Co1 N1 83.9(3) . . ?
N7 Co1 N1 168.8(3) 1_455 . ?
O4 Co2 O5 112.4(3) . . ?
O4 Co2 N6 97.9(3) . 1_656 ?
O5 Co2 N6 137.6(3) . 1_656 ?
O4 Co2 N12 91.1(3) . . ?
O5 Co2 N12 100.6(3) . . ?
N6 Co2 N12 108.0(4) 1_656 . ?
C25 O1 Co1 128.9(9) . . ?
C34 O4 Co2 109.1(6) . . ?
C35 O5 Co2 95.1(8) . . ?
C6 N2 N3 106.0(8) . . ?
C7 N3 N2 107.3(8) . . ?
C7 N4 C6 105.8(8) . . ?
C7 N4 N5 126.7(8) . . ?
C6 N4 N5 126.8(8) . . ?
C12 N6 C11 117.9(10) . . ?
C12 N6 Co2 120.9(8) . 1_454 ?
C11 N6 Co2 120.9(7) . 1_454 ?
C18 N8 N9 109.5(7) . . ?
N1 C1 C2 120.5(10) . . ?
C3 C2 C1 120.2(10) . . ?
C2 C3 C4 118.9(10) . . ?
C5 C4 C3 118.4(9) . . ?
C5 C4 C6 121.0(9) . . ?
C3 C4 C6 120.6(9) . . ?
N1 C5 C4 122.5(9) . . ?
N2 C6 N4 111.2(8) . . ?
N2 C6 C4 122.9(9) . . ?
N4 C6 C4 125.9(9) . . ?
N3 C7 N4 109.8(8) . . ?
N3 C7 C8 121.0(10) . . ?
N4 C7 C8 129.0(9) . . ?
C9 C8 C12 114.3(9) . . ?
C9 C8 C7 121.2(10) . . ?
C12 C8 C7 124.5(10) . . ?
C10 C9 C8 121.5(11) . . ?
C11 C10 C9 118.8(11) . . ?
N6 C11 C10 122.7(10) . . ?
N6 C12 C8 124.7(10) . . ?
C22 C21 C20 120.7(9) . . ?
O2 C25 O1 123.4(13) . . ?
O2 C25 C26 123.4(11) . . ?
O1 C25 C26 113.2(12) . . ?
C25 C26 C30 111.9(9) . . ?
C25 C26 C27 109.4(11) . . ?
C30 C26 C27 104.1(8) . . ?
C28 C27 C26 102.7(9) . . ?
C27 C28 C29 106.7(8) . . ?
C33 C29 C34 106.6(10) . . ?
C33 C29 C30 112.9(9) . . ?
C34 C29 C30 112.4(8) . . ?
C33 C29 C28 107.7(9) . . ?
C34 C29 C28 113.1(8) . . ?
C30 C29 C28 104.1(9) . . ?
C31 C30 C32 108.9(10) . . ?
C31 C30 C29 115.9(10) . . ?
C32 C30 C29 110.6(9) . . ?
C31 C30 C26 110.6(9) . . ?
C32 C30 C26 110.9(10) . . ?
C29 C30 C26 99.7(8) . . ?
O3 C34 O4 121.4(9) . . ?
O3 C34 C29 123.9(10) . . ?
O4 C34 C29 114.8(8) . . ?
O6 C35 O5 114.8(11) . . ?
O6 C35 C36 124.9(11) . . ?
O5 C35 C36 119.3(13) . . ?
C35 C36 C42 106.7(8) . . ?
C35 C36 C40 114.9(9) . . ?
C42 C36 C40 112.1(8) . . ?
C35 C36 C37 113.0(9) . . ?
C42 C36 C37 107.3(9) . . ?
C40 C36 C37 102.8(8) . . ?
C38 C37 C36 103.4(8) . . ?
C39 C38 C37 109.2(10) . . ?
C41 C39 C38 117.1(10) . . ?
C41 C39 C40 113.8(9) . . ?
C38 C39 C40 105.2(8) . . ?
C43 C40 C39 115.1(9) . . ?
C43 C40 C44 109.1(10) . . ?
C39 C40 C44 110.3(9) . . ?
C43 C40 C36 112.1(9) . . ?
C39 C40 C36 102.4(8) . . ?
C44 C40 C36 107.6(8) . . ?
O7 C41 O8 120.5(10) . . ?
O7 C41 C39 118.4(11) . . ?
O8 C41 C39 121.1(11) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.095