# Supplementary Material (ESI) for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2010
data_global

_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Hegen Zheng'
_publ_contact_author_email       ZHENGHG@NJU.EDU.CN

_publ_section_title              
;
Solvothermal synthesis,
structures and physical properties of four
new complexes constructed from multivariant
tricarboxylate ligand and pyridyl-based ligands
;
loop_
_publ_author_name
'Hegen Zheng.'
'Zijian Guo.'
'Chang-Chun Ji.'
'Jing Li.'
'Yi-Zhi Li.'

# Attachment '1.cif'

data_80508bm
_database_code_depnum_ccdc_archive 'CCDC 764686'
#TrackingRef '1.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ' C30 H32 Cd3 O21, 4(H O0.50), 2(H2 O)'
_chemical_formula_sum            'C30 H42 Cd3 O26'
_chemical_formula_weight         1155.84

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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
_symmetry_space_group_name_Hall  'C 2y'

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                   18.984(3)
_cell_length_b                   7.3315(11)
_cell_length_c                   16.506(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 119.337(2)
_cell_angle_gamma                90.00
_cell_volume                     2002.7(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    2017
_cell_measurement_theta_min      2.15
_cell_measurement_theta_max      23.44

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.917
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1148
_exptl_absorpt_coefficient_mu    1.673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.553
_exptl_absorpt_correction_T_max  0.605
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      291(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 Smart Apex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5434
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0786
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.16
_diffrn_reflns_theta_max         26.00
_reflns_number_total             3733
_reflns_number_gt                2988
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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^)+(0.0411P)^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     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_number_reflns         3733
_refine_ls_number_parameters     272
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0467
_refine_ls_wR_factor_ref         0.0823
_refine_ls_wR_factor_gt          0.0810
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_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
C1 C 0.4093(4) 0.1447(10) 0.7380(5) 0.0371(15) Uani 1 1 d . . .
C2 C 0.3685(4) 0.1920(9) 0.7862(5) 0.0352(15) Uani 1 1 d . . .
H2 H 0.3961 0.1939 0.8509 0.042 Uiso 1 1 calc R . .
C3 C 0.2881(4) 0.2354(9) 0.7388(5) 0.0298(13) Uani 1 1 d . . .
C4 C 0.2452(4) 0.2362(10) 0.6395(5) 0.0358(17) Uani 1 1 d . . .
H4 H 0.1909 0.2686 0.6072 0.043 Uiso 1 1 calc R . .
C5 C 0.2857(4) 0.1879(9) 0.5919(5) 0.0328(14) Uani 1 1 d . . .
C6 C 0.3671(4) 0.1382(10) 0.6416(4) 0.0317(13) Uani 1 1 d . . .
H6 H 0.3934 0.1002 0.6096 0.038 Uiso 1 1 calc R . .
C7 C 0.2422(4) 0.1860(10) 0.4872(5) 0.0327(15) Uani 1 1 d . . .
C8 C 0.1605(4) 0.1483(10) 0.4398(5) 0.0344(15) Uani 1 1 d . . .
H8 H 0.1332 0.1253 0.4726 0.041 Uiso 1 1 calc R . .
C9 C 0.1195(4) 0.1448(11) 0.3444(5) 0.0419(17) Uani 1 1 d . . .
H9 H 0.0644 0.1199 0.3132 0.050 Uiso 1 1 calc R . .
C10 C 0.1583(4) 0.1774(10) 0.2944(5) 0.0383(17) Uani 1 1 d . . .
C11 C 0.2399(5) 0.2151(10) 0.3432(5) 0.0382(17) Uani 1 1 d . . .
H11 H 0.2674 0.2373 0.3106 0.046 Uiso 1 1 calc R . .
C12 C 0.2813(4) 0.2205(10) 0.4378(4) 0.0364(16) Uani 1 1 d . . .
H12 H 0.3362 0.2478 0.4689 0.044 Uiso 1 1 calc R . .
C13 C 0.4976(4) 0.0903(9) 0.7899(5) 0.0335(15) Uani 1 1 d . . .
C14 C 0.1128(4) 0.1667(9) 0.1914(5) 0.0318(15) Uani 1 1 d . . .
C15 C 0.2444(4) 0.3043(11) 0.7879(5) 0.0386(16) Uani 1 1 d . . .
Cd1 Cd 0.65295(3) -0.03663(6) 0.85819(3) 0.03279(12) Uani 1 1 d . . .
Cd2 Cd 0.0000 0.12198(8) 0.0000 0.03379(18) Uani 1 2 d S . .
O1 O 0.5278(3) 0.0285(6) 0.7427(3) 0.0312(10) Uani 1 1 d . . .
O2 O 0.5368(3) 0.1020(7) 0.8752(3) 0.0334(10) Uani 1 1 d . . .
O3 O 0.2756(2) 0.2847(7) 0.8740(3) 0.0322(10) Uani 1 1 d . . .
O4 O 0.1736(3) 0.3640(6) 0.7398(3) 0.0372(11) Uani 1 1 d . . .
O5 O 0.0363(2) 0.1447(7) 0.1495(3) 0.0352(11) Uani 1 1 d . . .
O6 O 0.1495(2) 0.1775(6) 0.1449(3) 0.0302(10) Uani 1 1 d . . .
O7 O 0.6079(3) -0.3228(6) 0.8664(4) 0.0387(12) Uani 1 1 d . . .
H7B H 0.5878 -0.3203 0.9025 0.046 Uiso 1 1 d R . .
H7C H 0.5720 -0.3564 0.8125 0.046 Uiso 1 1 d R . .
O8 O 0.7287(3) 0.0018(7) 1.0140(3) 0.0477(14) Uani 1 1 d . . .
H8A H 0.7760 -0.0389 1.0320 0.072 Uiso 1 1 d R . .
H8B H 0.7312 0.1144 1.0275 0.072 Uiso 1 1 d R . .
O9 O 0.7126(3) 0.2354(6) 0.8533(3) 0.0353(11) Uani 1 1 d . . .
H9B H 0.6883 0.3368 0.8346 0.042 Uiso 1 1 d R . .
H9A H 0.7627 0.2180 0.8730 0.042 Uiso 1 1 d R . .
O10 O -0.0832(3) -0.0928(7) 0.0124(4) 0.0454(14) Uani 1 1 d . . .
H10A H -0.0663 -0.1989 0.0099 0.054 Uiso 1 1 d R . .
H10C H -0.1312 -0.0795 -0.0320 0.054 Uiso 1 1 d R . .
O11 O 0.0000 0.4283(9) 0.0000 0.0405(17) Uani 1 2 d S . .
H11A H 0.0395 0.4670 -0.0059 0.049 Uiso 0.50 1 d PR . .
H11C H 0.0046 0.4670 0.0509 0.049 Uiso 0.50 1 d PR . .
O12 O 0.6034(3) 0.4347(8) 0.7145(4) 0.0495(14) Uani 1 1 d . . .
H12A H 0.6249 0.5348 0.7121 0.059 Uiso 1 1 d R . .
H12B H 0.5870 0.3773 0.6636 0.059 Uiso 1 1 d R . .
O13 O 0.5180(7) 0.1931(15) 0.5589(8) 0.051(3) Uani 0.50 1 d P . .
H13D H 0.5307 0.1186 0.6034 0.061 Uiso 0.50 1 d PR . .
H13A H 0.4810 0.1470 0.5088 0.061 Uiso 0.50 1 d PR . .
O14 O 0.5306(3) 0.7698(8) 0.5779(4) 0.0560(16) Uani 1 1 d . . .
H14D H 0.5144 0.6850 0.5998 0.067 Uiso 1 1 d R . .
H14B H 0.5647 0.8358 0.6221 0.067 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
C1 0.028(3) 0.045(4) 0.031(4) 0.001(3) 0.009(3) -0.001(3)
C2 0.034(4) 0.035(4) 0.032(4) -0.002(3) 0.013(3) -0.006(3)
C3 0.035(3) 0.033(3) 0.031(3) -0.009(3) 0.023(3) -0.010(3)
C4 0.026(3) 0.035(4) 0.028(4) 0.002(3) -0.001(3) 0.009(3)
C5 0.028(3) 0.032(3) 0.028(3) -0.007(3) 0.006(3) -0.011(3)
C6 0.035(3) 0.046(4) 0.023(3) 0.002(3) 0.020(3) 0.010(3)
C7 0.017(3) 0.043(4) 0.030(4) -0.002(3) 0.005(3) 0.010(3)
C8 0.034(3) 0.040(4) 0.029(3) -0.006(3) 0.015(3) 0.011(3)
C9 0.030(3) 0.048(4) 0.040(4) -0.011(3) 0.011(3) -0.011(3)
C10 0.025(3) 0.044(4) 0.035(4) -0.005(3) 0.006(3) -0.001(3)
C11 0.041(4) 0.043(4) 0.030(4) -0.003(3) 0.016(3) -0.013(3)
C12 0.039(4) 0.047(4) 0.015(3) 0.002(3) 0.006(3) -0.001(3)
C13 0.039(3) 0.032(4) 0.023(3) 0.005(3) 0.010(3) 0.014(3)
C14 0.020(3) 0.026(4) 0.040(4) 0.004(3) 0.008(3) -0.001(2)
C15 0.029(3) 0.056(5) 0.037(4) -0.006(4) 0.021(3) 0.005(3)
Cd1 0.0321(2) 0.0311(2) 0.0285(2) -0.0010(2) 0.00955(19) 0.0030(2)
Cd2 0.0341(4) 0.0282(4) 0.0338(4) 0.000 0.0126(3) 0.000
O1 0.037(2) 0.038(2) 0.025(2) 0.0109(17) 0.020(2) 0.0039(18)
O2 0.025(2) 0.039(3) 0.024(2) 0.003(2) 0.0019(19) 0.0071(19)
O3 0.027(2) 0.044(3) 0.021(2) -0.010(2) 0.0076(18) -0.007(2)
O4 0.038(3) 0.032(3) 0.034(3) -0.001(2) 0.012(2) 0.011(2)
O5 0.018(2) 0.040(3) 0.032(2) -0.008(2) 0.0004(18) -0.0036(19)
O6 0.0207(19) 0.034(3) 0.031(2) 0.0027(18) 0.0091(19) 0.0014(17)
O7 0.043(3) 0.035(3) 0.039(3) 0.017(2) 0.021(2) 0.001(2)
O8 0.037(3) 0.056(4) 0.035(3) -0.009(2) 0.005(2) 0.013(2)
O9 0.041(3) 0.036(3) 0.034(3) -0.012(2) 0.022(2) -0.001(2)
O10 0.045(3) 0.040(3) 0.033(3) 0.001(2) 0.005(2) -0.020(2)
O11 0.056(4) 0.034(4) 0.049(4) 0.000 0.039(4) 0.000
O12 0.051(3) 0.038(3) 0.047(3) 0.008(3) 0.014(2) 0.018(3)
O13 0.032(5) 0.049(6) 0.040(6) 0.022(5) -0.006(5) 0.011(5)
O14 0.045(3) 0.048(3) 0.044(4) 0.003(3) -0.002(3) 0.012(3)

_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
C1 C6 1.388(9) . ?
C1 C2 1.400(10) . ?
C1 C13 1.516(9) . ?
C2 C3 1.368(10) . ?
C2 H2 0.9300 . ?
C3 C4 1.429(10) . ?
C3 C15 1.503(8) . ?
C4 C5 1.386(11) . ?
C4 H4 0.9300 . ?
C5 C6 1.397(9) . ?
C5 C7 1.508(10) . ?
C6 H6 0.9300 . ?
C7 C12 1.368(11) . ?
C7 C8 1.380(9) . ?
C8 C9 1.373(10) . ?
C8 H8 0.9300 . ?
C9 C10 1.371(11) . ?
C9 H9 0.9300 . ?
C10 C11 1.379(10) . ?
C10 C14 1.483(10) . ?
C11 C12 1.363(10) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 O2 1.232(8) . ?
C13 O1 1.255(8) . ?
C14 O6 1.266(8) . ?
C14 O5 1.278(7) . ?
C15 O3 1.251(8) . ?
C15 O4 1.257(8) . ?
Cd1 O1 2.252(5) . ?
Cd1 O8 2.267(5) . ?
Cd1 O4 2.292(5) 3_545 ?
Cd1 O7 2.295(4) . ?
Cd1 O9 2.314(5) . ?
Cd1 O2 2.564(4) . ?
Cd1 O3 2.572(4) 3_545 ?
Cd2 O5 2.219(5) . ?
Cd2 O5 2.219(5) 2 ?
Cd2 O11 2.246(6) . ?
Cd2 O10 2.309(5) 2 ?
Cd2 O10 2.309(5) . ?
O3 Cd1 2.572(4) 3_455 ?
O4 Cd1 2.292(5) 3_455 ?
O7 H7B 0.8500 . ?
O7 H7C 0.8501 . ?
O8 H8A 0.8499 . ?
O8 H8B 0.8500 . ?
O9 H9B 0.8500 . ?
O9 H9A 0.8500 . ?
O10 H10A 0.8500 . ?
O10 H10C 0.8500 . ?
O11 H11A 0.8499 . ?
O11 H11C 0.8500 . ?
O12 H12A 0.8499 . ?
O12 H12B 0.8501 . ?
O13 O13 1.72(2) 2_656 ?
O13 H13D 0.8499 . ?
O13 H13A 0.8500 . ?
O14 H14D 0.8500 . ?
O14 H14B 0.8500 . ?

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
C6 C1 C2 119.4(6) . . ?
C6 C1 C13 119.8(6) . . ?
C2 C1 C13 120.8(6) . . ?
C3 C2 C1 120.3(6) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C2 C3 C4 120.4(6) . . ?
C2 C3 C15 121.7(6) . . ?
C4 C3 C15 117.5(6) . . ?
C5 C4 C3 119.1(6) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C4 C5 C6 119.7(7) . . ?
C4 C5 C7 120.6(6) . . ?
C6 C5 C7 119.8(6) . . ?
C1 C6 C5 121.0(6) . . ?
C1 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C12 C7 C8 119.1(7) . . ?
C12 C7 C5 122.0(6) . . ?
C8 C7 C5 118.9(7) . . ?
C9 C8 C7 120.1(7) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C10 C9 C8 121.2(6) . . ?
C10 C9 H9 119.4 . . ?
C8 C9 H9 119.4 . . ?
C9 C10 C11 117.7(7) . . ?
C9 C10 C14 119.9(6) . . ?
C11 C10 C14 122.4(7) . . ?
C12 C11 C10 121.8(7) . . ?
C12 C11 H11 119.1 . . ?
C10 C11 H11 119.1 . . ?
C11 C12 C7 120.1(7) . . ?
C11 C12 H12 120.0 . . ?
C7 C12 H12 120.0 . . ?
O2 C13 O1 122.1(6) . . ?
O2 C13 C1 120.6(6) . . ?
O1 C13 C1 117.3(6) . . ?
O6 C14 O5 119.7(6) . . ?
O6 C14 C10 120.5(5) . . ?
O5 C14 C10 119.8(6) . . ?
O3 C15 O4 121.5(6) . . ?
O3 C15 C3 119.6(6) . . ?
O4 C15 C3 118.6(6) . . ?
O1 Cd1 O8 138.92(17) . . ?
O1 Cd1 O4 84.03(16) . 3_545 ?
O8 Cd1 O4 136.77(18) . 3_545 ?
O1 Cd1 O7 88.54(17) . . ?
O8 Cd1 O7 95.38(19) . . ?
O4 Cd1 O7 89.12(18) 3_545 . ?
O1 Cd1 O9 96.87(17) . . ?
O8 Cd1 O9 83.30(19) . . ?
O4 Cd1 O9 87.31(17) 3_545 . ?
O7 Cd1 O9 173.17(18) . . ?
O1 Cd1 O2 53.24(14) . . ?
O8 Cd1 O2 85.86(16) . . ?
O4 Cd1 O2 137.27(16) 3_545 . ?
O7 Cd1 O2 89.45(17) . . ?
O9 Cd1 O2 97.11(16) . . ?
O1 Cd1 O3 136.16(15) . 3_545 ?
O8 Cd1 O3 84.79(15) . 3_545 ?
O4 Cd1 O3 53.10(15) 3_545 3_545 ?
O7 Cd1 O3 82.75(16) . 3_545 ?
O9 Cd1 O3 90.46(16) . 3_545 ?
O2 Cd1 O3 167.20(14) . 3_545 ?
O5 Cd2 O5 171.4(3) . 2 ?
O5 Cd2 O11 85.69(13) . . ?
O5 Cd2 O11 85.69(13) 2 . ?
O5 Cd2 O10 107.25(18) . 2 ?
O5 Cd2 O10 78.81(18) 2 2 ?
O11 Cd2 O10 133.00(15) . 2 ?
O5 Cd2 O10 78.81(18) . . ?
O5 Cd2 O10 107.25(18) 2 . ?
O11 Cd2 O10 133.00(15) . . ?
O10 Cd2 O10 94.0(3) 2 . ?
C13 O1 Cd1 99.4(4) . . ?
C13 O2 Cd1 85.3(4) . . ?
C15 O3 Cd1 85.7(4) . 3_455 ?
C15 O4 Cd1 98.6(4) . 3_455 ?
C14 O5 Cd2 105.3(4) . . ?
Cd1 O7 H7B 109.3 . . ?
Cd1 O7 H7C 109.5 . . ?
H7B O7 H7C 109.5 . . ?
Cd1 O8 H8A 109.1 . . ?
Cd1 O8 H8B 109.9 . . ?
H8A O8 H8B 109.5 . . ?
Cd1 O9 H9B 125.3 . . ?
Cd1 O9 H9A 109.4 . . ?
H9B O9 H9A 125.3 . . ?
Cd2 O10 H10A 109.2 . . ?
Cd2 O10 H10C 109.6 . . ?
H10A O10 H10C 109.5 . . ?
Cd2 O11 H11A 109.5 . . ?
Cd2 O11 H11C 109.5 . . ?
H11A O11 H11C 109.5 . . ?
H12A O12 H12B 109.5 . . ?
O13 O13 H13D 140.0 2_656 . ?
O13 O13 H13A 38.5 2_656 . ?
H13D O13 H13A 109.5 . . ?
H14D O14 H14B 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.369
_refine_diff_density_min         -1.328
_refine_diff_density_rms         0.114

# Attachment '2.cif'

data_90713
_database_code_depnum_ccdc_archive 'CCDC 764687'
#TrackingRef '2.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C45 H36 Cd2 N6 O16, 2(H O0.50), 3(H2 O)'
_chemical_formula_sum            'C45 H44 Cd2 N6 O20'
_chemical_formula_weight         1213.66

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 2/c'
_symmetry_space_group_name_Hall  '-P 2yc'

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

_cell_length_a                   11.845(2)
_cell_length_b                   14.043(3)
_cell_length_c                   17.092(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.750(3)
_cell_angle_gamma                90.00
_cell_volume                     2692.3(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    958
_cell_measurement_theta_min      2.324
_cell_measurement_theta_max      17.904

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1224
_exptl_absorpt_coefficient_mu    0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      291(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 Smart Apex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14338
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5256
_reflns_number_gt                4231
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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.

For the disordered C24 and N4 occupied the same position ,

the instructions of
eadp c24 n4
exyz c24 n4

were used.
;

_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^)+(0.0900P)^2^+1.9900P] 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_number_reflns         5256
_refine_ls_number_parameters     346
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0547
_refine_ls_wR_factor_ref         0.1501
_refine_ls_wR_factor_gt          0.1447
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_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
C1 C -0.0460(4) 1.1247(4) 0.8605(3) 0.0410(11) Uani 1 1 d . . .
C2 C -0.0835(3) 1.02709(16) 0.82599(18) 0.0520(13) Uani 1 1 d G . .
C3 C -0.1296(3) 1.00689(18) 0.74208(16) 0.0420(11) Uani 1 1 d G . .
H3 H -0.1407 1.0557 0.7035 0.050 Uiso 1 1 calc R . .
C4 C -0.1591(3) 0.9138(2) 0.71580(15) 0.0496(12) Uani 1 1 d G . .
H4 H -0.1900 0.9003 0.6597 0.060 Uiso 1 1 calc R . .
C5 C -0.1425(3) 0.84091(15) 0.7734(2) 0.0442(12) Uani 1 1 d G . .
C6 C -0.0964(3) 0.86111(19) 0.85733(19) 0.0539(14) Uani 1 1 d G . .
H6 H -0.0854 0.8123 0.8959 0.065 Uiso 1 1 calc R . .
C7 C -0.0669(3) 0.9542(2) 0.88362(14) 0.0474(12) Uani 1 1 d G . .
H7 H -0.0361 0.9677 0.9398 0.057 Uiso 1 1 calc R . .
C8 C -0.1579(4) 0.7412(3) 0.7534(3) 0.0373(10) Uani 1 1 d . . .
C9 C -0.2535(4) 0.7243(3) 0.6818(3) 0.0355(10) Uani 1 1 d . . .
H9 H -0.2944 0.7752 0.6506 0.043 Uiso 1 1 calc R . .
C10 C -0.2878(4) 0.6310(4) 0.6568(3) 0.0442(12) Uani 1 1 d . . .
C11 C -0.2284(4) 0.5551(3) 0.7034(3) 0.0361(10) Uani 1 1 d . . .
H11 H -0.2514 0.4930 0.6868 0.043 Uiso 1 1 calc R . .
C12 C -0.1344(4) 0.5721(3) 0.7749(3) 0.0369(10) Uani 1 1 d . . .
C13 C -0.1001(4) 0.6634(3) 0.8001(3) 0.0400(11) Uani 1 1 d . . .
H13 H -0.0377 0.6735 0.8489 0.048 Uiso 1 1 calc R . .
C14 C -0.3730(4) 0.6106(3) 0.5726(3) 0.0392(10) Uani 1 1 d . . .
C15 C -0.0652(4) 0.4957(3) 0.8317(3) 0.0391(10) Uani 1 1 d . . .
C16 C 0.2481(4) 1.2718(3) 1.0617(3) 0.0373(10) Uani 1 1 d . . .
H16 H 0.2316 1.2069 1.0558 0.045 Uiso 1 1 calc R . .
C17 C 0.2384(4) 1.4231(3) 1.0405(3) 0.0379(10) Uani 1 1 d . . .
H17 H 0.2131 1.4828 1.0180 0.045 Uiso 1 1 calc R . .
C18 C 0.3379(4) 1.4058(3) 1.1081(3) 0.0420(11) Uani 1 1 d . . .
H18 H 0.3927 1.4501 1.1389 0.050 Uiso 1 1 calc R . .
C19 C 0.4209(4) 1.2565(3) 1.1857(3) 0.0371(10) Uani 1 1 d . . .
C20 C 0.4210(5) 1.1576(3) 1.1839(3) 0.0451(12) Uani 1 1 d . . .
H20 H 0.3707 1.1223 1.1406 0.054 Uiso 1 1 calc R . .
C21 C 0.5000 1.1175(6) 1.2500 0.061(2) Uani 1 2 d S . .
C22 C 0.5000 1.3075(5) 1.2500 0.0399(15) Uani 1 2 d S . .
H22 H 0.5000 1.3737 1.2500 0.048 Uiso 1 2 calc SR . .
C23 C 0.4220(4) 0.9537(3) 1.1908(3) 0.0410(11) Uani 1 1 d . . .
H23A H 0.3588 0.9740 1.1427 0.049 Uiso 1 1 d R . .
C24 C 0.4528(5) 0.8639(4) 1.2144(3) 0.0546(12) Uani 0.50 1 d P . .
H4Y H 0.4173 0.8116 1.1870 0.065 Uiso 0.50 1 d PR . .
Cd1 Cd 0.02009(3) 1.31559(2) 0.90587(2) 0.04112(15) Uani 1 1 d . . .
N1 N 0.1835(4) 1.3396(3) 1.0122(2) 0.0425(9) Uani 1 1 d . . .
N2 N 0.3383(4) 1.3099(3) 1.1198(3) 0.0427(9) Uani 1 1 d . . .
N3 N 0.5000 1.0116(4) 1.2500 0.0498(16) Uani 1 2 d S . .
N4 N 0.4528(5) 0.8639(4) 1.2144(3) 0.0546(12) Uani 0.50 1 d P . .
O1 O -0.0978(3) 1.1981(2) 0.8236(2) 0.0521(10) Uani 1 1 d . . .
O2 O 0.0441(3) 1.1459(2) 0.9266(2) 0.0403(7) Uani 1 1 d . . .
O3 O -0.4282(3) 0.6744(3) 0.5291(2) 0.0538(10) Uani 1 1 d . . .
H3A H -0.3940 0.6876 0.4864 0.081 Uiso 1 1 d R . .
O4 O -0.4192(3) 0.5286(2) 0.55559(19) 0.0378(7) Uani 1 1 d . . .
O5 O -0.0995(3) 0.4100(2) 0.80986(19) 0.0378(7) Uani 1 1 d . . .
O6 O 0.0165(3) 0.5135(3) 0.8965(2) 0.0505(9) Uani 1 1 d . . .
O7 O 0.1468(3) 1.2975(2) 0.8244(2) 0.0472(8) Uani 1 1 d . . .
H7A H 0.1849 1.3490 0.8252 0.057 Uiso 1 1 d R . .
H7C H 0.1054 1.2845 0.7749 0.057 Uiso 1 1 d R . .
O8 O -0.0944(3) 1.3366(2) 0.9930(2) 0.0477(9) Uani 1 1 d . . .
H8A H -0.0842 1.3927 1.0128 0.057 Uiso 1 1 d R . .
H8B H -0.1677 1.3283 0.9660 0.057 Uiso 1 1 d R . .
O9 O 0.3950(8) 0.7141(6) 0.3891(5) 0.048(2) Uani 0.40 1 d P . .
H9B H 0.3771 0.7440 0.3436 0.058 Uiso 0.40 1 d PR . .
H9D H 0.3645 0.7420 0.4217 0.058 Uiso 0.40 1 d PR . .
O10 O 0.2682(9) 0.1509(7) 0.5137(6) 0.062(3) Uani 0.40 1 d P . .
H10A H 0.2945 0.1126 0.4851 0.074 Uiso 0.40 1 d PR . .
H10C H 0.1938 0.1423 0.5035 0.074 Uiso 0.40 1 d PR . .
O11 O 0.2560(7) 0.9504(6) 0.4962(5) 0.0431(19) Uani 0.40 1 d P . .
H11D H 0.2260 0.9684 0.5327 0.052 Uiso 0.40 1 d PR . .
H11B H 0.2308 0.9860 0.4540 0.052 Uiso 0.40 1 d PR . .
O12 O 0.6727(6) 0.6617(5) 0.3830(4) 0.050(2) Uani 0.50 1 d P . .
H12A H 0.6401 0.7040 0.3473 0.061 Uiso 0.50 1 d PR . .
H12C H 0.6581 0.6069 0.3609 0.061 Uiso 0.50 1 d PR . .
O13 O 0.4999(11) 0.1147(9) 0.4867(7) 0.049(3) Uani 0.30 1 d P . .
H13A H 0.4818 0.0689 0.4524 0.058 Uiso 0.30 1 d PR . .
H13B H 0.5704 0.1069 0.5195 0.058 Uiso 0.30 1 d PR . .

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
C1 0.035(2) 0.047(3) 0.036(2) 0.009(2) 0.0046(19) -0.018(2)
C2 0.042(3) 0.046(3) 0.057(3) 0.014(2) -0.001(2) -0.004(2)
C3 0.047(3) 0.028(2) 0.046(3) -0.0012(19) 0.009(2) 0.0072(19)
C4 0.048(3) 0.035(3) 0.056(3) -0.008(2) 0.003(2) 0.004(2)
C5 0.029(2) 0.030(2) 0.072(3) -0.003(2) 0.014(2) -0.0131(18)
C6 0.057(3) 0.037(3) 0.063(3) 0.012(2) 0.013(3) 0.011(2)
C7 0.053(3) 0.040(3) 0.045(3) 0.010(2) 0.010(2) -0.006(2)
C8 0.042(3) 0.028(2) 0.038(2) -0.0071(18) 0.007(2) -0.0176(19)
C9 0.041(3) 0.035(2) 0.028(2) 0.0106(18) 0.0069(18) 0.0166(19)
C10 0.043(3) 0.041(3) 0.034(2) 0.007(2) -0.008(2) -0.018(2)
C11 0.042(2) 0.025(2) 0.035(2) -0.0024(17) 0.0021(19) -0.0140(18)
C12 0.035(2) 0.041(2) 0.034(2) 0.0013(19) 0.0105(19) 0.0064(19)
C13 0.032(2) 0.044(3) 0.034(2) 0.0112(19) -0.0042(19) -0.0128(19)
C14 0.039(2) 0.036(2) 0.033(2) 0.0068(19) -0.0023(19) -0.0018(19)
C15 0.042(3) 0.046(3) 0.026(2) -0.0091(19) 0.0055(18) 0.009(2)
C16 0.046(3) 0.039(2) 0.028(2) 0.0013(18) 0.0132(19) 0.014(2)
C17 0.045(3) 0.032(2) 0.036(2) 0.0039(18) 0.012(2) 0.0111(19)
C18 0.040(3) 0.035(2) 0.040(2) -0.008(2) -0.004(2) -0.0087(19)
C19 0.038(2) 0.032(2) 0.031(2) -0.0026(18) -0.0034(19) 0.0058(18)
C20 0.043(3) 0.034(2) 0.044(3) 0.002(2) -0.004(2) -0.017(2)
C21 0.062(5) 0.038(4) 0.050(4) 0.000 -0.029(4) 0.000
C22 0.042(4) 0.038(3) 0.032(3) 0.000 0.001(3) 0.000
C23 0.034(2) 0.043(3) 0.047(3) -0.018(2) 0.013(2) 0.013(2)
C24 0.054(3) 0.046(3) 0.060(3) -0.007(2) 0.011(2) -0.019(2)
Cd1 0.0400(2) 0.0354(2) 0.0310(2) 0.00078(13) -0.01226(14) -0.00274(14)
N1 0.044(2) 0.044(2) 0.0295(19) -0.0009(17) -0.0028(17) -0.0001(18)
N2 0.045(2) 0.043(2) 0.040(2) 0.0004(17) 0.0123(19) 0.0137(18)
N3 0.064(4) 0.029(3) 0.034(3) 0.000 -0.015(3) 0.000
N4 0.054(3) 0.046(3) 0.060(3) -0.007(2) 0.011(2) -0.019(2)
O1 0.051(2) 0.042(2) 0.0411(19) 0.0111(15) -0.0157(16) -0.0123(16)
O2 0.0315(16) 0.0417(18) 0.0392(17) 0.0049(14) -0.0004(13) 0.0033(14)
O3 0.050(2) 0.044(2) 0.043(2) 0.0066(15) -0.0185(16) -0.0001(16)
O4 0.0302(16) 0.0321(16) 0.0439(18) -0.0003(13) 0.0018(14) 0.0082(13)
O5 0.0447(18) 0.0249(15) 0.0371(16) 0.0064(12) 0.0040(14) 0.0127(13)
O6 0.0381(19) 0.048(2) 0.0413(19) 0.0106(15) -0.0215(15) -0.0071(15)
O7 0.0441(19) 0.0386(18) 0.0434(19) 0.0030(14) -0.0074(15) 0.0030(15)
O8 0.0332(17) 0.0407(19) 0.055(2) 0.0158(16) -0.0052(15) 0.0065(14)
O9 0.040(5) 0.042(4) 0.043(5) -0.021(4) -0.013(4) 0.002(4)
O10 0.057(6) 0.060(6) 0.048(5) -0.017(4) -0.010(4) 0.041(5)
O11 0.034(4) 0.038(4) 0.053(5) -0.005(4) 0.010(4) 0.010(3)
O12 0.042(4) 0.029(3) 0.049(4) -0.010(3) -0.030(3) 0.009(3)
O13 0.056(7) 0.051(7) 0.030(5) -0.002(5) 0.002(5) 0.009(6)

_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
C1 O1 1.261(6) . ?
C1 O2 1.314(5) . ?
C1 C2 1.502(5) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C3 H3 0.9300 . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.3900 . ?
C5 C8 1.440(5) . ?
C6 C7 1.3900 . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.396(6) . ?
C8 C13 1.396(7) . ?
C9 C10 1.397(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.380(7) . ?
C10 C14 1.497(6) . ?
C11 C12 1.384(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.372(7) . ?
C12 C15 1.501(6) . ?
C13 H13 0.9300 . ?
C14 O3 1.212(6) . ?
C14 O4 1.269(6) . ?
C15 O6 1.239(5) . ?
C15 O5 1.287(6) . ?
C16 N2 1.316(7) . ?
C16 N1 1.339(6) . ?
C16 H16 0.9300 . ?
C17 N1 1.353(6) . ?
C17 C18 1.381(7) . ?
C17 H17 0.9300 . ?
C18 N2 1.362(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.389(7) . ?
C19 C22 1.392(6) . ?
C19 N2 1.442(6) . ?
C20 C21 1.338(6) . ?
C20 H20 0.9300 . ?
C21 C20 1.338(6) 2_657 ?
C21 N3 1.487(9) . ?
C22 C19 1.392(6) 2_657 ?
C22 H22 0.9300 . ?
C23 C24 1.338(7) . ?
C23 N3 1.393(6) . ?
C23 H23A 0.9600 . ?
C24 N4 1.361(10) 2_657 ?
C24 C24 1.361(10) 2_657 ?
C24 H4Y 0.9000 . ?
Cd1 N1 2.214(4) . ?
Cd1 O5 2.228(3) 1_565 ?
Cd1 O1 2.321(3) . ?
Cd1 O8 2.333(4) . ?
Cd1 O7 2.366(4) . ?
Cd1 O2 2.413(3) . ?
N3 C23 1.393(6) 2_657 ?
O3 H3A 0.9601 . ?
O5 Cd1 2.228(3) 1_545 ?
O7 H7A 0.8499 . ?
O7 H7C 0.8500 . ?
O8 H8A 0.8499 . ?
O8 H8B 0.8500 . ?
O9 H9B 0.8499 . ?
O9 H9D 0.8500 . ?
O10 H10A 0.8500 . ?
O10 H10C 0.8500 . ?
O11 H11D 0.8500 . ?
O11 H11B 0.8499 . ?
O12 H12A 0.8501 . ?
O12 H12C 0.8500 . ?
O13 H13A 0.8500 . ?
O13 H13B 0.8500 . ?

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 C1 O2 112.0(4) . . ?
O1 C1 C2 121.0(4) . . ?
O2 C1 C2 126.9(4) . . ?
C3 C2 C7 120.0 . . ?
C3 C2 C1 124.1(3) . . ?
C7 C2 C1 115.9(3) . . ?
C4 C3 C2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.0 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 C8 114.9(3) . . ?
C4 C5 C8 124.8(3) . . ?
C7 C6 C5 120.0 . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C2 120.0 . . ?
C6 C7 H7 120.0 . . ?
C2 C7 H7 120.0 . . ?
C9 C8 C13 118.7(4) . . ?
C9 C8 C5 112.2(4) . . ?
C13 C8 C5 128.6(4) . . ?
C8 C9 C10 120.1(4) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C11 C10 C9 120.3(4) . . ?
C11 C10 C14 117.9(4) . . ?
C9 C10 C14 120.8(4) . . ?
C10 C11 C12 119.4(4) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C13 C12 C11 120.8(4) . . ?
C13 C12 C15 114.7(4) . . ?
C11 C12 C15 124.4(4) . . ?
C12 C13 C8 120.7(4) . . ?
C12 C13 H13 119.7 . . ?
C8 C13 H13 119.7 . . ?
O3 C14 O4 115.0(4) . . ?
O3 C14 C10 120.8(4) . . ?
O4 C14 C10 120.1(4) . . ?
O6 C15 O5 122.1(4) . . ?
O6 C15 C12 122.8(4) . . ?
O5 C15 C12 115.1(4) . . ?
N2 C16 N1 110.3(4) . . ?
N2 C16 H16 124.8 . . ?
N1 C16 H16 124.8 . . ?
N1 C17 C18 109.2(4) . . ?
N1 C17 H17 125.4 . . ?
C18 C17 H17 125.4 . . ?
N2 C18 C17 104.9(4) . . ?
N2 C18 H18 127.5 . . ?
C17 C18 H18 127.5 . . ?
C20 C19 C22 121.7(4) . . ?
C20 C19 N2 120.5(4) . . ?
C22 C19 N2 117.7(4) . . ?
C21 C20 C19 114.1(5) . . ?
C21 C20 H20 123.0 . . ?
C19 C20 H20 123.0 . . ?
C20 C21 C20 130.2(7) 2_657 . ?
C20 C21 N3 114.9(4) 2_657 . ?
C20 C21 N3 114.9(4) . . ?
C19 C22 C19 118.1(6) . 2_657 ?
C19 C22 H22 120.9 . . ?
C19 C22 H22 120.9 2_657 . ?
C24 C23 N3 106.1(4) . . ?
C24 C23 H23A 126.9 . . ?
N3 C23 H23A 126.9 . . ?
C23 C24 N4 109.6(3) . 2_657 ?
C23 C24 C24 109.6(3) . 2_657 ?
N4 C24 C24 0.0(4) 2_657 2_657 ?
C23 C24 H4Y 125.1 . . ?
N4 C24 H4Y 125.3 2_657 . ?
C24 C24 H4Y 125.3 2_657 . ?
N1 Cd1 O5 134.03(14) . 1_565 ?
N1 Cd1 O1 143.40(14) . . ?
O5 Cd1 O1 81.97(12) 1_565 . ?
N1 Cd1 O8 89.46(14) . . ?
O5 Cd1 O8 91.85(12) 1_565 . ?
O1 Cd1 O8 96.71(15) . . ?
N1 Cd1 O7 86.97(14) . . ?
O5 Cd1 O7 90.22(12) 1_565 . ?
O1 Cd1 O7 86.51(14) . . ?
O8 Cd1 O7 176.39(12) . . ?
N1 Cd1 O2 89.97(13) . . ?
O5 Cd1 O2 135.48(11) 1_565 . ?
O1 Cd1 O2 53.60(11) . . ?
O8 Cd1 O2 95.55(12) . . ?
O7 Cd1 O2 85.02(11) . . ?
C16 N1 C17 106.3(4) . . ?
C16 N1 Cd1 125.5(3) . . ?
C17 N1 Cd1 128.2(3) . . ?
C16 N2 C18 109.2(4) . . ?
C16 N2 C19 124.1(4) . . ?
C18 N2 C19 126.7(4) . . ?
C23 N3 C23 108.5(6) . 2_657 ?
C23 N3 C21 125.7(3) . . ?
C23 N3 C21 125.7(3) 2_657 . ?
C1 O1 Cd1 100.2(3) . . ?
C1 O2 Cd1 94.2(3) . . ?
C14 O3 H3A 109.5 . . ?
C15 O5 Cd1 106.0(3) . 1_545 ?
Cd1 O7 H7A 109.4 . . ?
Cd1 O7 H7C 109.7 . . ?
H7A O7 H7C 109.5 . . ?
Cd1 O8 H8A 109.5 . . ?
Cd1 O8 H8B 109.8 . . ?
H8A O8 H8B 109.5 . . ?
H9B O9 H9D 109.8 . . ?
H10A O10 H10C 109.8 . . ?
H11D O11 H11B 109.5 . . ?
H12A O12 H12C 109.5 . . ?
H13A O13 H13B 109.5 . . ?

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
O1 C1 C2 C3 31.6(6) . . . . ?
O2 C1 C2 C3 -144.2(4) . . . . ?
O1 C1 C2 C7 -150.0(4) . . . . ?
O2 C1 C2 C7 34.3(6) . . . . ?
C7 C2 C3 C4 0.0 . . . . ?
C1 C2 C3 C4 178.4(4) . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C3 C4 C5 C8 -173.1(4) . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C8 C5 C6 C7 173.7(3) . . . . ?
C5 C6 C7 C2 0.0 . . . . ?
C3 C2 C7 C6 0.0 . . . . ?
C1 C2 C7 C6 -178.5(3) . . . . ?
C6 C5 C8 C9 149.0(3) . . . . ?
C4 C5 C8 C9 -37.6(5) . . . . ?
C6 C5 C8 C13 -23.1(6) . . . . ?
C4 C5 C8 C13 150.3(4) . . . . ?
C13 C8 C9 C10 -1.7(7) . . . . ?
C5 C8 C9 C10 -174.6(4) . . . . ?
C8 C9 C10 C11 0.8(7) . . . . ?
C8 C9 C10 C14 -167.8(5) . . . . ?
C9 C10 C11 C12 -0.2(8) . . . . ?
C14 C10 C11 C12 168.8(4) . . . . ?
C10 C11 C12 C13 0.3(7) . . . . ?
C10 C11 C12 C15 178.3(5) . . . . ?
C11 C12 C13 C8 -1.2(8) . . . . ?
C15 C12 C13 C8 -179.4(4) . . . . ?
C9 C8 C13 C12 1.9(7) . . . . ?
C5 C8 C13 C12 173.5(4) . . . . ?
C11 C10 C14 O3 179.6(5) . . . . ?
C9 C10 C14 O3 -11.6(8) . . . . ?
C11 C10 C14 O4 23.3(7) . . . . ?
C9 C10 C14 O4 -167.9(5) . . . . ?
C13 C12 C15 O6 0.1(7) . . . . ?
C11 C12 C15 O6 -178.0(5) . . . . ?
C13 C12 C15 O5 177.7(4) . . . . ?
C11 C12 C15 O5 -0.3(7) . . . . ?
N1 C17 C18 N2 -1.3(6) . . . . ?
C22 C19 C20 C21 2.2(7) . . . . ?
N2 C19 C20 C21 -178.3(4) . . . . ?
C19 C20 C21 C20 -1.1(3) . . . 2_657 ?
C19 C20 C21 N3 178.9(3) . . . . ?
C20 C19 C22 C19 -1.2(4) . . . 2_657 ?
N2 C19 C22 C19 179.3(5) . . . 2_657 ?
N3 C23 C24 N4 -0.4(7) . . . 2_657 ?
N3 C23 C24 C24 -0.4(7) . . . 2_657 ?
N2 C16 N1 C17 1.3(6) . . . . ?
N2 C16 N1 Cd1 -178.9(3) . . . . ?
C18 C17 N1 C16 0.1(6) . . . . ?
C18 C17 N1 Cd1 -179.8(3) . . . . ?
O5 Cd1 N1 C16 -176.2(3) 1_565 . . . ?
O1 Cd1 N1 C16 -8.8(6) . . . . ?
O8 Cd1 N1 C16 91.7(4) . . . . ?
O7 Cd1 N1 C16 -88.9(4) . . . . ?
O2 Cd1 N1 C16 -3.8(4) . . . . ?
O5 Cd1 N1 C17 3.6(5) 1_565 . . . ?
O1 Cd1 N1 C17 171.0(4) . . . . ?
O8 Cd1 N1 C17 -88.5(4) . . . . ?
O7 Cd1 N1 C17 90.9(4) . . . . ?
O2 Cd1 N1 C17 176.0(4) . . . . ?
N1 C16 N2 C18 -2.2(6) . . . . ?
N1 C16 N2 C19 176.3(4) . . . . ?
C17 C18 N2 C16 2.1(6) . . . . ?
C17 C18 N2 C19 -176.3(4) . . . . ?
C20 C19 N2 C16 10.6(7) . . . . ?
C22 C19 N2 C16 -169.9(4) . . . . ?
C20 C19 N2 C18 -171.1(5) . . . . ?
C22 C19 N2 C18 8.4(7) . . . . ?
C24 C23 N3 C23 0.2(3) . . . 2_657 ?
C24 C23 N3 C21 -179.8(3) . . . . ?
C20 C21 N3 C23 176.2(4) 2_657 . . . ?
C20 C21 N3 C23 -3.8(4) . . . . ?
C20 C21 N3 C23 -3.8(4) 2_657 . . 2_657 ?
C20 C21 N3 C23 176.2(4) . . . 2_657 ?
O2 C1 O1 Cd1 1.7(5) . . . . ?
C2 C1 O1 Cd1 -174.6(3) . . . . ?
N1 Cd1 O1 C1 5.1(5) . . . . ?
O5 Cd1 O1 C1 176.0(3) 1_565 . . . ?
O8 Cd1 O1 C1 -93.1(3) . . . . ?
O7 Cd1 O1 C1 85.3(3) . . . . ?
O2 Cd1 O1 C1 -1.1(3) . . . . ?
O1 C1 O2 Cd1 -1.7(4) . . . . ?
C2 C1 O2 Cd1 174.4(4) . . . . ?
N1 Cd1 O2 C1 -175.3(3) . . . . ?
O5 Cd1 O2 C1 -3.1(3) 1_565 . . . ?
O1 Cd1 O2 C1 1.0(3) . . . . ?
O8 Cd1 O2 C1 95.3(3) . . . . ?
O7 Cd1 O2 C1 -88.3(3) . . . . ?
O6 C15 O5 Cd1 -2.4(6) . . . 1_545 ?
C12 C15 O5 Cd1 179.9(3) . . . 1_545 ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.916
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.091

# Attachment '3.cif'

data_80627cm
_database_code_depnum_ccdc_archive 'CCDC 764688'
#TrackingRef '3.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H14 Mn N O7'
_chemical_formula_sum            'C20 H14 Mn N O7'
_chemical_formula_weight         435.26

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           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                   6.940(3)
_cell_length_b                   9.896(4)
_cell_length_c                   13.149(5)
_cell_angle_alpha                94.652(7)
_cell_angle_beta                 99.553(7)
_cell_angle_gamma                96.088(8)
_cell_volume                     881.0(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    703
_cell_measurement_theta_min      2.482
_cell_measurement_theta_max      22.2915

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             444
_exptl_absorpt_coefficient_mu    0.796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      291(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 Smart Apex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4785
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_sigmaI/netI    0.1332
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.58
_diffrn_reflns_theta_max         26.00
_reflns_number_total             3375
_reflns_number_gt                2063
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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^)+(0.0062P)^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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3375
_refine_ls_number_parameters     262
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0616
_refine_ls_wR_factor_ref         0.0949
_refine_ls_wR_factor_gt          0.0882
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.002
_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
C1 C 0.8622(9) 0.2979(5) -0.1149(4) 0.0372(14) Uani 1 1 d . . .
C2 C 0.8373(8) 0.3348(5) -0.0053(4) 0.0299(13) Uani 1 1 d . . .
C3 C 0.7493(8) 0.4466(5) 0.0228(3) 0.0356(14) Uani 1 1 d . . .
H3 H 0.7020 0.5020 -0.0272 0.043 Uiso 1 1 calc R . .
C4 C 0.9069(8) 0.2536(5) 0.0689(4) 0.0371(14) Uani 1 1 d . . .
H4 H 0.9657 0.1774 0.0501 0.045 Uiso 1 1 calc R . .
C5 C 0.8902(7) 0.2844(5) 0.1714(3) 0.0327(13) Uani 1 1 d . . .
H5 H 0.9398 0.2294 0.2211 0.039 Uiso 1 1 calc R . .
C6 C 0.7303(8) 0.4776(4) 0.1253(3) 0.0326(14) Uani 1 1 d . . .
H6 H 0.6700 0.5534 0.1434 0.039 Uiso 1 1 calc R . .
C7 C 0.8005(7) 0.3965(4) 0.2009(3) 0.0263(12) Uani 1 1 d . . .
C8 C 0.7800(7) 0.4279(4) 0.3105(3) 0.0253(12) Uani 1 1 d . . .
C9 C 0.7894(7) 0.5601(4) 0.3554(3) 0.0265(12) Uani 1 1 d . . .
H9 H 0.8098 0.6320 0.3155 0.032 Uiso 1 1 calc R . .
C10 C 0.7695(7) 0.5898(4) 0.4585(3) 0.0226(12) Uani 1 1 d . . .
C11 C 0.7731(7) 0.7315(5) 0.5057(4) 0.0288(12) Uani 1 1 d . . .
C12 C 0.7401(7) 0.4817(4) 0.5177(3) 0.0230(12) Uani 1 1 d . . .
H12 H 0.7297 0.4994 0.5870 0.028 Uiso 1 1 calc R . .
C13 C 0.7501(7) 0.3220(4) 0.3720(3) 0.0260(12) Uani 1 1 d . . .
H13 H 0.7459 0.2321 0.3441 0.031 Uiso 1 1 calc R . .
C14 C 0.4798(8) 1.0601(5) 0.7745(4) 0.0354(14) Uani 1 1 d . . .
H14 H 0.4286 1.1182 0.7277 0.043 Uiso 1 1 calc R . .
C15 C 0.6497(8) 0.8815(5) 0.8098(4) 0.0441(16) Uani 1 1 d . . .
H15 H 0.7197 0.8126 0.7883 0.053 Uiso 1 1 calc R . .
C16 C 0.6173(8) 0.8911(5) 0.9103(4) 0.0472(17) Uani 1 1 d . . .
H16 H 0.6645 0.8291 0.9549 0.057 Uiso 1 1 calc R . .
C17 C 0.4421(8) 1.0758(5) 0.8741(4) 0.0358(14) Uani 1 1 d . . .
H17 H 0.3672 1.1430 0.8932 0.043 Uiso 1 1 calc R . .
C18 C 0.5162(7) 0.9913(5) 0.9451(3) 0.0270(12) Uani 1 1 d . . .
C19 C 0.7262(7) 0.3486(4) 0.4746(3) 0.0222(11) Uani 1 1 d . . .
C20 C 0.6905(7) 0.2322(5) 0.5390(4) 0.0252(12) Uani 1 1 d . . .
Mn1 Mn 0.68649(12) 0.95789(7) 0.59005(5) 0.0263(2) Uani 1 1 d U . .
N1 N 0.5854(6) 0.9665(4) 0.7418(3) 0.0261(10) Uani 1 1 d . . .
O1 O 0.9593(6) 0.2118(4) -0.1407(3) 0.0515(11) Uani 1 1 d . . .
O2 O 0.7621(6) 0.3721(3) -0.1796(2) 0.0512(11) Uani 1 1 d . . .
H2A H 0.7796 0.3476 -0.2405 0.077 Uiso 1 1 d R . .
O3 O 0.7413(5) 0.7489(3) 0.5972(2) 0.0325(9) Uani 1 1 d . . .
O4 O 0.7910(5) 0.8319(3) 0.4525(2) 0.0339(9) Uani 1 1 d U . .
O5 O 0.6351(5) 0.1128(3) 0.4903(2) 0.0300(9) Uani 1 1 d . . .
O6 O 0.7133(6) 0.2528(3) 0.6335(2) 0.0472(11) Uani 1 1 d . . .
O7 O 0.9828(5) 1.0410(3) 0.6716(2) 0.0387(10) Uani 1 1 d . . .
H7C H 0.9568 1.0476 0.7326 0.046 Uiso 1 1 d R . .
H7A H 1.0222 1.1248 0.6690 0.046 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
C1 0.043(4) 0.042(4) 0.022(3) -0.001(3) 0.002(3) -0.008(3)
C2 0.033(4) 0.035(3) 0.021(3) -0.003(2) 0.009(3) -0.002(3)
C3 0.050(4) 0.037(3) 0.020(3) 0.005(2) 0.006(3) 0.003(3)
C4 0.052(4) 0.033(3) 0.028(3) -0.005(2) 0.014(3) 0.007(3)
C5 0.040(4) 0.037(3) 0.023(3) 0.005(2) 0.007(3) 0.012(3)
C6 0.049(4) 0.026(3) 0.023(3) -0.001(2) 0.010(3) 0.007(3)
C7 0.032(3) 0.027(3) 0.018(3) 0.000(2) 0.003(2) -0.003(2)
C8 0.034(4) 0.018(3) 0.023(3) -0.002(2) 0.007(2) 0.000(2)
C9 0.030(3) 0.027(3) 0.025(3) 0.013(2) 0.006(2) 0.004(2)
C10 0.026(3) 0.020(3) 0.025(3) 0.005(2) 0.008(2) 0.008(2)
C11 0.023(3) 0.026(3) 0.037(3) 0.000(2) 0.007(3) 0.006(2)
C12 0.025(3) 0.029(3) 0.017(3) 0.001(2) 0.009(2) 0.005(2)
C13 0.026(3) 0.020(3) 0.031(3) -0.001(2) 0.005(2) 0.002(2)
C14 0.044(4) 0.040(3) 0.024(3) 0.005(2) 0.003(3) 0.013(3)
C15 0.060(5) 0.046(4) 0.034(3) 0.008(3) 0.019(3) 0.026(3)
C16 0.065(5) 0.060(4) 0.026(3) 0.018(3) 0.015(3) 0.032(3)
C17 0.041(4) 0.050(4) 0.022(3) 0.002(2) 0.014(3) 0.021(3)
C18 0.029(3) 0.027(3) 0.025(3) -0.001(2) 0.007(3) 0.003(2)
C19 0.025(3) 0.022(3) 0.020(3) 0.000(2) 0.005(2) 0.005(2)
C20 0.029(3) 0.022(3) 0.025(3) 0.006(2) 0.004(3) 0.004(2)
Mn1 0.0395(6) 0.0220(4) 0.0186(4) 0.0028(3) 0.0073(4) 0.0052(4)
N1 0.029(3) 0.031(3) 0.017(2) -0.0004(18) 0.003(2) 0.003(2)
O1 0.063(3) 0.063(3) 0.030(2) -0.0117(19) 0.015(2) 0.018(2)
O2 0.074(3) 0.058(3) 0.021(2) -0.0035(18) 0.009(2) 0.012(2)
O3 0.050(3) 0.026(2) 0.023(2) -0.0032(15) 0.0129(18) 0.0064(17)
O4 0.052(3) 0.0232(19) 0.030(2) 0.0060(14) 0.0159(18) 0.0050(17)
O5 0.043(3) 0.0198(19) 0.026(2) 0.0029(15) 0.0054(18) 0.0015(17)
O6 0.082(3) 0.039(2) 0.020(2) 0.0059(17) 0.012(2) 0.000(2)
O7 0.046(3) 0.037(2) 0.032(2) 0.0037(16) 0.0091(19) -0.0029(18)

_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
C1 O1 1.202(6) . ?
C1 O2 1.327(6) . ?
C1 C2 1.500(6) . ?
C2 C4 1.372(6) . ?
C2 C3 1.373(6) . ?
C3 C6 1.389(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.384(5) . ?
C4 H4 0.9300 . ?
C5 C7 1.387(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.386(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.483(5) . ?
C8 C9 1.382(5) . ?
C8 C13 1.393(5) . ?
C9 C10 1.397(5) . ?
C9 H9 0.9300 . ?
C10 C12 1.390(5) . ?
C10 C11 1.482(6) . ?
C11 O3 1.260(5) . ?
C11 O4 1.267(5) . ?
C12 C19 1.379(5) . ?
C12 H12 0.9300 . ?
C13 C19 1.393(5) . ?
C13 H13 0.9300 . ?
C14 N1 1.328(5) . ?
C14 C17 1.377(5) . ?
C14 H14 0.9300 . ?
C15 N1 1.333(5) . ?
C15 C16 1.375(6) . ?
C15 H15 0.9300 . ?
C16 C18 1.365(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.377(6) . ?
C17 H17 0.9300 . ?
C18 C18 1.496(8) 2_677 ?
C19 C20 1.508(5) . ?
C20 O6 1.223(5) . ?
C20 O5 1.286(5) . ?
Mn1 O5 2.118(3) 1_565 ?
Mn1 O3 2.149(3) . ?
Mn1 O7 2.196(3) . ?
Mn1 N1 2.221(3) . ?
Mn1 O5 2.314(4) 2_666 ?
Mn1 O4 2.369(3) . ?
O2 H2A 0.8500 . ?
O5 Mn1 2.118(3) 1_545 ?
O5 Mn1 2.314(4) 2_666 ?
O7 H7C 0.8499 . ?
O7 H7A 0.8500 . ?

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 C1 O2 124.5(5) . . ?
O1 C1 C2 124.4(5) . . ?
O2 C1 C2 111.1(5) . . ?
C4 C2 C3 119.5(4) . . ?
C4 C2 C1 118.2(5) . . ?
C3 C2 C1 122.3(5) . . ?
C2 C3 C6 120.5(4) . . ?
C2 C3 H3 119.8 . . ?
C6 C3 H3 119.8 . . ?
C2 C4 C5 120.4(5) . . ?
C2 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C4 C5 C7 120.8(4) . . ?
C4 C5 H5 119.6 . . ?
C7 C5 H5 119.6 . . ?
C7 C6 C3 120.5(4) . . ?
C7 C6 H6 119.7 . . ?
C3 C6 H6 119.7 . . ?
C6 C7 C5 118.3(4) . . ?
C6 C7 C8 121.1(4) . . ?
C5 C7 C8 120.6(4) . . ?
C9 C8 C13 117.7(4) . . ?
C9 C8 C7 122.3(4) . . ?
C13 C8 C7 119.9(4) . . ?
C8 C9 C10 122.4(4) . . ?
C8 C9 H9 118.8 . . ?
C10 C9 H9 118.8 . . ?
C12 C10 C9 118.3(4) . . ?
C12 C10 C11 119.2(4) . . ?
C9 C10 C11 122.4(4) . . ?
O3 C11 O4 120.7(4) . . ?
O3 C11 C10 118.3(4) . . ?
O4 C11 C10 120.7(4) . . ?
C19 C12 C10 120.6(4) . . ?
C19 C12 H12 119.7 . . ?
C10 C12 H12 119.7 . . ?
C19 C13 C8 121.1(4) . . ?
C19 C13 H13 119.5 . . ?
C8 C13 H13 119.5 . . ?
N1 C14 C17 123.6(4) . . ?
N1 C14 H14 118.2 . . ?
C17 C14 H14 118.2 . . ?
N1 C15 C16 122.9(5) . . ?
N1 C15 H15 118.5 . . ?
C16 C15 H15 118.5 . . ?
C18 C16 C15 120.4(5) . . ?
C18 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C18 C17 C14 119.4(4) . . ?
C18 C17 H17 120.3 . . ?
C14 C17 H17 120.3 . . ?
C16 C18 C17 117.0(4) . . ?
C16 C18 C18 122.2(5) . 2_677 ?
C17 C18 C18 120.8(5) . 2_677 ?
C12 C19 C13 119.7(4) . . ?
C12 C19 C20 120.1(4) . . ?
C13 C19 C20 120.1(4) . . ?
O6 C20 O5 122.4(4) . . ?
O6 C20 C19 120.4(4) . . ?
O5 C20 C19 117.1(4) . . ?
O5 Mn1 O3 144.66(11) 1_565 . ?
O5 Mn1 O7 98.87(12) 1_565 . ?
O3 Mn1 O7 93.97(12) . . ?
O5 Mn1 N1 120.58(13) 1_565 . ?
O3 Mn1 N1 92.35(12) . . ?
O7 Mn1 N1 88.69(13) . . ?
O5 Mn1 O5 78.77(12) 1_565 2_666 ?
O3 Mn1 O5 90.37(12) . 2_666 ?
O7 Mn1 O5 175.10(12) . 2_666 ?
N1 Mn1 O5 88.85(13) . 2_666 ?
O5 Mn1 O4 87.95(11) 1_565 . ?
O3 Mn1 O4 57.91(10) . . ?
O7 Mn1 O4 96.03(12) . . ?
N1 Mn1 O4 150.08(12) . . ?
O5 Mn1 O4 88.21(12) 2_666 . ?
C14 N1 C15 116.6(4) . . ?
C14 N1 Mn1 124.4(3) . . ?
C15 N1 Mn1 118.6(3) . . ?
C1 O2 H2A 107.9 . . ?
C11 O3 Mn1 95.4(3) . . ?
C11 O4 Mn1 85.2(3) . . ?
C20 O5 Mn1 111.2(3) . 1_545 ?
C20 O5 Mn1 122.8(3) . 2_666 ?
Mn1 O5 Mn1 101.23(12) 1_545 2_666 ?
Mn1 O7 H7C 97.5 . . ?
Mn1 O7 H7A 118.7 . . ?
H7C O7 H7A 97.9 . . ?

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.080

# Attachment '4.cif'

data_80919bm
_database_code_depnum_ccdc_archive 'CCDC 764689'
#TrackingRef '4.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H14 Co N O7'
_chemical_formula_sum            'C20 H14 Co N O7'
_chemical_formula_weight         439.25

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   6.930(2)
_cell_length_b                   9.658(3)
_cell_length_c                   13.022(4)
_cell_angle_alpha                93.719(6)
_cell_angle_beta                 99.179(6)
_cell_angle_gamma                94.856(7)
_cell_volume                     854.6(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    510
_cell_measurement_theta_min      2.549
_cell_measurement_theta_max      18.5158

_exptl_crystal_description       block
_exptl_crystal_colour            violet
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             448
_exptl_absorpt_coefficient_mu    1.052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_T_max  0.793
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      291(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 Smart Apex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4604
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0833
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         26.00
_reflns_number_total             3272
_reflns_number_gt                2233
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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^)+(0.0965P)^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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3272
_refine_ls_number_parameters     262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0640
_refine_ls_wR_factor_ref         0.1655
_refine_ls_wR_factor_gt          0.1560
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_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
C1 C 0.8579(7) 0.2951(5) -0.1185(4) 0.0368(10) Uani 1 1 d . . .
C2 C 0.8374(7) 0.3330(5) -0.0070(3) 0.0352(10) Uani 1 1 d . . .
C3 C 0.7462(7) 0.4493(5) 0.0192(4) 0.0403(11) Uani 1 1 d . . .
H3 H 0.6946 0.5043 -0.0324 0.048 Uiso 1 1 calc R . .
C4 C 0.7318(7) 0.4840(5) 0.1244(4) 0.0417(12) Uani 1 1 d . . .
H4 H 0.6751 0.5634 0.1439 0.050 Uiso 1 1 calc R . .
C5 C 0.8069(7) 0.3933(5) 0.1995(4) 0.0385(11) Uani 1 1 d . . .
C6 C 0.8919(7) 0.2738(5) 0.1730(4) 0.0361(10) Uani 1 1 d . . .
H6 H 0.9346 0.2149 0.2239 0.043 Uiso 1 1 calc R . .
C7 C 0.9128(8) 0.2425(5) 0.0695(4) 0.0427(12) Uani 1 1 d . . .
H7 H 0.9741 0.1650 0.0507 0.051 Uiso 1 1 calc R . .
C8 C 0.7849(7) 0.4277(5) 0.3120(4) 0.0465(13) Uani 1 1 d . . .
C9 C 0.7963(8) 0.5644(5) 0.3554(4) 0.0426(12) Uani 1 1 d . . .
H9 H 0.8206 0.6381 0.3152 0.051 Uiso 1 1 calc R . .
C10 C 0.7716(7) 0.5911(5) 0.4588(3) 0.0390(11) Uani 1 1 d . . .
C11 C 0.7399(7) 0.4815(5) 0.5200(4) 0.0402(11) Uani 1 1 d . . .
H11 H 0.7293 0.4992 0.5898 0.048 Uiso 1 1 calc R . .
C12 C 0.7243(7) 0.3466(5) 0.4766(4) 0.0386(11) Uani 1 1 d . . .
C13 C 0.7493(7) 0.3136(5) 0.3720(4) 0.0367(11) Uani 1 1 d . . .
H13 H 0.7427 0.2219 0.3442 0.044 Uiso 1 1 calc R . .
C14 C 0.7706(8) 0.7377(5) 0.5015(4) 0.0407(11) Uani 1 1 d . . .
C15 C 0.6863(7) 0.2279(5) 0.5402(4) 0.0387(11) Uani 1 1 d . . .
C16 C 0.4701(7) 1.0626(5) 0.7688(4) 0.0355(10) Uani 1 1 d . . .
H16 H 0.4183 1.1217 0.7202 0.043 Uiso 1 1 calc R . .
C17 C 0.4325(7) 1.0824(5) 0.8723(4) 0.0412(11) Uani 1 1 d . . .
H17 H 0.3580 1.1521 0.8922 0.049 Uiso 1 1 calc R . .
C18 C 0.5145(7) 0.9901(5) 0.9439(3) 0.0350(10) Uani 1 1 d . . .
C19 C 0.6183(8) 0.8834(6) 0.9097(4) 0.0440(12) Uani 1 1 d . . .
H19 H 0.6673 0.8194 0.9550 0.053 Uiso 1 1 calc R . .
C20 C 0.6468(7) 0.8749(5) 0.8064(4) 0.0397(11) Uani 1 1 d . . .
H20 H 0.7179 0.8051 0.7832 0.048 Uiso 1 1 calc R . .
Co1 Co 0.67711(10) 0.95672(7) 0.59388(5) 0.0389(2) Uani 1 1 d . . .
N1 N 0.5733(6) 0.9660(4) 0.7380(3) 0.0378(9) Uani 1 1 d . . .
O1 O 0.9536(5) 0.2030(4) -0.1433(2) 0.0403(8) Uani 1 1 d . . .
O2 O 0.7624(5) 0.3737(4) -0.1834(3) 0.0429(8) Uani 1 1 d . . .
H2A H 0.7799 0.3492 -0.2444 0.064 Uiso 1 1 d R . .
O3 O 0.7212(5) 0.7534(3) 0.5903(2) 0.0386(8) Uani 1 1 d . . .
O4 O 0.8026(5) 0.8383(4) 0.4526(3) 0.0443(8) Uani 1 1 d . . .
O5 O 0.6351(5) 0.1084(3) 0.4944(2) 0.0381(7) Uani 1 1 d . . .
O6 O 0.7042(5) 0.2486(3) 0.6360(2) 0.0405(8) Uani 1 1 d . . .
O7 O 0.9629(5) 1.0257(4) 0.6691(3) 0.0467(9) Uani 1 1 d . . .
H7C H 0.9369 1.0323 0.7301 0.056 Uiso 1 1 d R . .
H7A H 1.0023 1.1095 0.6665 0.056 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
C1 0.037(3) 0.036(2) 0.036(2) -0.0044(19) 0.0076(19) 0.001(2)
C2 0.028(2) 0.039(2) 0.034(2) -0.0119(19) 0.0036(18) -0.0025(19)
C3 0.042(3) 0.040(3) 0.037(2) 0.001(2) 0.008(2) -0.008(2)
C4 0.035(3) 0.045(3) 0.040(3) -0.013(2) -0.004(2) 0.012(2)
C5 0.039(3) 0.038(3) 0.038(2) 0.004(2) 0.008(2) -0.006(2)
C6 0.036(3) 0.037(3) 0.033(2) 0.0071(19) 0.0014(19) -0.004(2)
C7 0.047(3) 0.043(3) 0.039(3) -0.005(2) 0.008(2) 0.011(2)
C8 0.033(3) 0.041(3) 0.055(3) -0.019(2) -0.007(2) -0.009(2)
C9 0.044(3) 0.044(3) 0.040(3) -0.004(2) 0.008(2) 0.006(2)
C10 0.043(3) 0.045(3) 0.029(2) 0.011(2) 0.0048(19) 0.003(2)
C11 0.040(3) 0.044(3) 0.033(2) -0.004(2) 0.005(2) -0.009(2)
C12 0.034(2) 0.045(3) 0.035(2) 0.003(2) 0.0044(19) -0.009(2)
C13 0.031(2) 0.034(2) 0.040(2) -0.012(2) -0.0028(19) -0.0009(19)
C14 0.045(3) 0.038(3) 0.034(2) -0.004(2) -0.007(2) 0.007(2)
C15 0.031(2) 0.036(2) 0.045(3) 0.000(2) -0.001(2) -0.006(2)
C16 0.032(2) 0.034(2) 0.039(2) 0.0003(19) 0.0076(19) -0.0056(19)
C17 0.036(3) 0.045(3) 0.043(3) -0.006(2) 0.011(2) 0.009(2)
C18 0.029(2) 0.040(2) 0.033(2) -0.0131(19) 0.0049(18) -0.0050(19)
C19 0.047(3) 0.045(3) 0.046(3) 0.013(2) 0.015(2) 0.015(2)
C20 0.036(3) 0.047(3) 0.037(2) -0.003(2) 0.0101(19) 0.006(2)
Co1 0.0390(4) 0.0407(4) 0.0381(4) 0.0040(3) 0.0082(3) 0.0066(3)
N1 0.036(2) 0.038(2) 0.038(2) -0.0088(17) 0.0091(17) -0.0038(17)
O1 0.0437(19) 0.0449(19) 0.0333(17) -0.0060(14) 0.0091(14) 0.0119(16)
O2 0.044(2) 0.048(2) 0.0400(18) 0.0082(16) 0.0078(15) 0.0141(16)
O3 0.0344(17) 0.0414(19) 0.0355(17) -0.0188(15) 0.0057(13) -0.0043(14)
O4 0.041(2) 0.050(2) 0.0445(19) 0.0066(17) 0.0138(15) 0.0025(16)
O5 0.0384(18) 0.0429(18) 0.0304(16) 0.0016(14) 0.0017(13) -0.0022(14)
O6 0.0424(19) 0.0380(18) 0.0392(19) -0.0081(15) 0.0137(14) -0.0114(14)
O7 0.056(2) 0.0380(18) 0.0441(19) -0.0033(15) 0.0057(16) 0.0021(16)

_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
C1 O1 1.211(5) . ?
C1 O2 1.311(5) . ?
C1 C2 1.506(6) . ?
C2 C3 1.384(7) . ?
C2 C7 1.433(7) . ?
C3 C4 1.410(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.422(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.388(7) . ?
C5 C8 1.515(7) . ?
C6 C7 1.395(7) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.392(7) . ?
C8 C13 1.418(8) . ?
C9 C10 1.395(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.389(7) . ?
C10 C14 1.488(7) . ?
C11 C12 1.375(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.419(7) . ?
C12 C15 1.486(7) . ?
C13 H13 0.9300 . ?
C14 O4 1.220(6) . ?
C14 O3 1.262(6) . ?
C15 O6 1.235(6) . ?
C15 O5 1.260(6) . ?
C16 N1 1.303(6) . ?
C16 C17 1.417(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.418(7) . ?
C17 H17 0.9300 . ?
C18 C19 1.395(7) . ?
C18 C18 1.508(9) 2_677 ?
C19 C20 1.389(7) . ?
C19 H19 0.9300 . ?
C20 N1 1.364(6) . ?
C20 H20 0.9300 . ?
Co1 O3 2.012(3) . ?
Co1 O5 2.027(3) 1_565 ?
Co1 O7 2.097(4) . ?
Co1 N1 2.114(4) . ?
Co1 O5 2.298(3) 2_666 ?
O2 H2A 0.8435 . ?
O5 Co1 2.027(3) 1_545 ?
O5 Co1 2.298(3) 2_666 ?
O7 H7C 0.8418 . ?
O7 H7A 0.8361 . ?

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 C1 O2 125.0(4) . . ?
O1 C1 C2 122.9(4) . . ?
O2 C1 C2 112.1(4) . . ?
C3 C2 C7 122.0(4) . . ?
C3 C2 C1 120.9(4) . . ?
C7 C2 C1 117.2(4) . . ?
C2 C3 C4 119.8(5) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C3 C4 C5 117.7(4) . . ?
C3 C4 H4 121.2 . . ?
C5 C4 H4 121.2 . . ?
C6 C5 C4 122.6(4) . . ?
C6 C5 C8 119.6(4) . . ?
C4 C5 C8 117.7(4) . . ?
C5 C6 C7 119.6(4) . . ?
C5 C6 H6 120.2 . . ?
C7 C6 H6 120.2 . . ?
C6 C7 C2 118.2(4) . . ?
C6 C7 H7 120.9 . . ?
C2 C7 H7 120.9 . . ?
C9 C8 C13 120.8(5) . . ?
C9 C8 C5 122.2(5) . . ?
C13 C8 C5 116.9(4) . . ?
C8 C9 C10 120.2(5) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
C11 C10 C9 120.2(5) . . ?
C11 C10 C14 120.3(4) . . ?
C9 C10 C14 119.4(4) . . ?
C12 C11 C10 119.5(4) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C11 C12 C13 122.5(5) . . ?
C11 C12 C15 120.3(4) . . ?
C13 C12 C15 117.2(4) . . ?
C8 C13 C12 116.7(4) . . ?
C8 C13 H13 121.7 . . ?
C12 C13 H13 121.7 . . ?
O4 C14 O3 120.6(4) . . ?
O4 C14 C10 123.4(5) . . ?
O3 C14 C10 115.9(5) . . ?
O6 C15 O5 121.6(5) . . ?
O6 C15 C12 119.6(4) . . ?
O5 C15 C12 118.8(4) . . ?
N1 C16 C17 123.6(4) . . ?
N1 C16 H16 118.2 . . ?
C17 C16 H16 118.2 . . ?
C16 C17 C18 116.4(4) . . ?
C16 C17 H17 121.8 . . ?
C18 C17 H17 121.8 . . ?
C19 C18 C17 119.9(4) . . ?
C19 C18 C18 121.5(5) . 2_677 ?
C17 C18 C18 118.6(5) . 2_677 ?
C20 C19 C18 118.5(4) . . ?
C20 C19 H19 120.7 . . ?
C18 C19 H19 120.7 . . ?
N1 C20 C19 121.8(4) . . ?
N1 C20 H20 119.1 . . ?
C19 C20 H20 119.1 . . ?
O3 Co1 O5 139.33(13) . 1_565 ?
O3 Co1 O7 94.68(13) . . ?
O5 Co1 O7 99.20(14) 1_565 . ?
O3 Co1 N1 96.25(15) . . ?
O5 Co1 N1 121.38(15) 1_565 . ?
O7 Co1 N1 90.89(15) . . ?
O3 Co1 O5 87.80(13) . 2_666 ?
O5 Co1 O5 77.53(14) 1_565 2_666 ?
O7 Co1 O5 176.73(13) . 2_666 ?
N1 Co1 O5 90.95(14) . 2_666 ?
C16 N1 C20 119.8(4) . . ?
C16 N1 Co1 124.4(3) . . ?
C20 N1 Co1 115.0(3) . . ?
C1 O2 H2A 108.4 . . ?
C14 O3 Co1 99.7(3) . . ?
C15 O5 Co1 111.6(3) . 1_545 ?
C15 O5 Co1 122.8(3) . 2_666 ?
Co1 O5 Co1 102.47(14) 1_545 2_666 ?
Co1 O7 H7C 96.5 . . ?
Co1 O7 H7A 117.6 . . ?
H7C O7 H7A 97.4 . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.080