# Electronic Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2013

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_MnC4DC
#==============================================================================

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H25 Mn2 N O9'
_chemical_formula_sum            'C16 H25 Mn2 N O9'
_chemical_formula_weight         485.25

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0018 '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 0.0075 0.0037 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0131 0.0069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3595 0.8096 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   8.9470(18)
_cell_length_b                   20.874(4)
_cell_length_c                   10.471(2)
_cell_angle_alpha                90
_cell_angle_beta                 100.02(3)
_cell_angle_gamma                90
_cell_volume                     1925.7(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    95(2)
_cell_measurement_reflns_used    31762
_cell_measurement_theta_min      0.43
_cell_measurement_theta_max      29.57

_exptl_crystal_description       plate
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_F_000             1000
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.567
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_process_details   'HKL3000sm Scalepack'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      95(2)
_diffrn_radiation_wavelength     0.75001
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15811
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.097
_diffrn_reflns_theta_max         29.547
_diffrn_reflns_theta_full        26.744
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measured_fraction_theta_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.955
_reflns_number_total             4378
_reflns_number_gt                4296
_reflns_threshold_expression     'I > 2\s(I)'
_reflns_Friedel_coverage         0.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_cell_refinement       HKL3000sm
_computing_data_reduction        HKL3000sm
_computing_structure_solution    'SHELXL-2013-XS (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013-XL (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP 3'
_computing_publication_material  'enCifer 1.4, WinGX'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+5.6943P]
 where P=(Fo^2^+2Fc^2^)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4378
_refine_ls_number_parameters     256
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.1174
_refine_ls_wR_factor_gt          0.1172
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_restrained_S_all      1.115
_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_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.28992(4) 0.73947(2) 0.84709(4) 0.01306(12) Uani 1 1 d . . . . .
Mn2 Mn 0.34549(5) 0.85563(2) 1.10358(4) 0.01448(12) Uani 1 1 d . . . . .
O1A O 0.2553(2) 0.83442(9) 0.77313(19) 0.0185(4) Uani 1 1 d . . . . .
O2A O 0.2343(2) 0.90054(10) 0.93798(18) 0.0189(4) Uani 1 1 d . . . . .
O3A O 0.2756(2) 0.92178(10) 0.23030(19) 0.0199(4) Uani 1 1 d . . . . .
O4A O 0.3154(2) 0.85837(9) 0.40533(19) 0.0177(4) Uani 1 1 d . . . . .
C1A C 0.2070(3) 0.88449(13) 0.8195(3) 0.0162(5) Uani 1 1 d . . . . .
C2A C 0.1047(4) 0.92926(14) 0.7307(3) 0.0216(6) Uani 1 1 d . . . . .
H2A1 H 0.1190 0.9732 0.7661 0.026 Uiso 1 1 calc R U . . .
H2A2 H -0.0021 0.9169 0.7312 0.026 Uiso 1 1 calc R U . . .
C3A C 0.1309(3) 0.93009(14) 0.5906(3) 0.0212(6) Uani 1 1 d . . . . .
H3A1 H 0.1294 0.8855 0.5581 0.025 Uiso 1 1 calc R U . . .
H3A2 H 0.0466 0.9535 0.5367 0.025 Uiso 1 1 calc R U . . .
C4A C 0.2807(4) 0.96130(14) 0.5752(3) 0.0220(6) Uani 1 1 d . . . . .
H4A1 H 0.3657 0.9337 0.6160 0.026 Uiso 1 1 calc R U . . .
H4A2 H 0.2903 1.0030 0.6209 0.026 Uiso 1 1 calc R U . . .
C5A C 0.2925(4) 0.97202(14) 0.4325(3) 0.0212(6) Uani 1 1 d . . . . .
H5A1 H 0.2059 0.9990 0.3925 0.025 Uiso 1 1 calc R U . . .
H5A2 H 0.3865 0.9965 0.4291 0.025 Uiso 1 1 calc R U . . .
C6A C 0.2939(3) 0.91220(13) 0.3510(3) 0.0159(5) Uani 1 1 d . . . . .
O1B O 0.1005(2) 0.75023(10) 0.95037(19) 0.0185(4) Uani 1 1 d . . . . .
O2B O 0.1664(2) 0.79094(9) 1.14975(17) 0.0150(4) Uani 1 1 d . . . . .
O3B O -0.5519(2) 0.77017(9) 1.01978(18) 0.0155(4) Uani 1 1 d . . . . .
O4B O -0.5199(2) 0.77328(10) 1.23258(18) 0.0165(4) Uani 1 1 d . . . . .
C1B C 0.0788(3) 0.75835(13) 1.0637(3) 0.0153(5) Uani 1 1 d . . . . .
C2B C -0.0594(3) 0.72757(14) 1.1047(3) 0.0180(5) Uani 1 1 d . . . . .
H2B1 H -0.0823 0.7505 1.1818 0.022 Uiso 1 1 calc R U . . .
H2B2 H -0.0341 0.6827 1.1309 0.022 Uiso 1 1 calc R U . . .
C3B C -0.2016(3) 0.72754(14) 1.0002(3) 0.0177(5) Uani 1 1 d . . . . .
H3B1 H -0.1716 0.7201 0.9147 0.021 Uiso 1 1 calc R U . . .
H3B2 H -0.2501 0.7703 0.9978 0.021 Uiso 1 1 calc R U . . .
C4B C -0.3173(3) 0.67667(13) 1.0220(3) 0.0177(5) Uani 1 1 d . . . . .
H4B1 H -0.2656 0.6346 1.0328 0.021 Uiso 1 1 calc R U . . .
H4B2 H -0.3966 0.6742 0.9434 0.021 Uiso 1 1 calc R U . . .
C5B C -0.3945(3) 0.68853(13) 1.1394(3) 0.0175(5) Uani 1 1 d . . . . .
H5B1 H -0.4565 0.6505 1.1518 0.021 Uiso 1 1 calc R U . . .
H5B2 H -0.3149 0.6927 1.2175 0.021 Uiso 1 1 calc R U . . .
C6B C -0.4943(3) 0.74663(13) 1.1304(3) 0.0148(5) Uani 1 1 d . . . . .
O1C O 0.5595(2) 0.90365(11) 1.1266(2) 0.0243(4) Uani 1 1 d . . . . .
N1C N 0.8042(3) 0.90907(12) 1.1053(3) 0.0225(5) Uani 1 1 d . . . . .
C1C C 0.6568(3) 0.91514(14) 1.0575(3) 0.0212(6) Uani 1 1 d . . . . .
C2C C 0.6104(4) 0.93753(17) 0.9197(3) 0.0290(7) Uani 1 1 d . . . . .
H2C1 H 0.5002 0.9333 0.8938 0.044 Uiso 1 1 calc R U . . .
H2C2 H 0.6614 0.9114 0.8624 0.044 Uiso 1 1 calc R U . . .
H2C3 H 0.6394 0.9825 0.9130 0.044 Uiso 1 1 calc R U . . .
C3C C 0.9224(4) 0.92112(18) 1.0289(3) 0.0305(7) Uani 1 1 d . . . . .
H3C1 H 0.9356 0.8831 0.9772 0.046 Uiso 1 1 calc R U . . .
H3C2 H 1.0180 0.9308 1.0870 0.046 Uiso 1 1 calc R U . . .
H3C3 H 0.8933 0.9576 0.9711 0.046 Uiso 1 1 calc R U . . .
C4C C 0.8528(4) 0.88452(17) 1.2371(3) 0.0298(7) Uani 1 1 d . . . . .
H4C1 H 0.8793 0.9205 1.2970 0.045 Uiso 1 1 calc R U . . .
H4C2 H 0.9417 0.8568 1.2392 0.045 Uiso 1 1 calc R U . . .
H4C3 H 0.7701 0.8598 1.2634 0.045 Uiso 1 1 calc R U . . .

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 0.0133(2) 0.0185(2) 0.00822(19) -0.00004(13) 0.00449(14) 0.00050(13)
Mn2 0.0150(2) 0.0192(2) 0.01030(19) 0.00008(13) 0.00524(14) -0.00078(14)
O1A 0.0229(10) 0.0196(9) 0.0144(9) 0.0024(7) 0.0075(8) 0.0037(7)
O2A 0.0221(10) 0.0261(10) 0.0092(8) 0.0006(7) 0.0047(7) 0.0010(8)
O3A 0.0253(10) 0.0239(10) 0.0119(9) -0.0010(7) 0.0075(8) 0.0008(8)
O4A 0.0200(9) 0.0185(9) 0.0151(9) -0.0014(7) 0.0041(7) 0.0006(7)
C1A 0.0168(12) 0.0211(12) 0.0120(11) 0.0015(9) 0.0059(9) -0.0003(10)
C2A 0.0273(14) 0.0247(14) 0.0137(12) 0.0016(10) 0.0061(11) 0.0082(11)
C3A 0.0249(14) 0.0261(14) 0.0127(12) 0.0018(10) 0.0041(10) 0.0058(11)
C4A 0.0297(15) 0.0226(13) 0.0141(12) -0.0018(10) 0.0052(11) 0.0019(11)
C5A 0.0303(15) 0.0205(13) 0.0136(12) -0.0013(10) 0.0057(11) 0.0002(11)
C6A 0.0135(11) 0.0222(13) 0.0130(11) -0.0010(9) 0.0054(9) 0.0002(9)
O1B 0.0132(9) 0.0293(10) 0.0149(9) -0.0021(7) 0.0074(7) -0.0011(7)
O2B 0.0129(8) 0.0222(9) 0.0100(8) 0.0003(7) 0.0024(7) -0.0021(7)
O3B 0.0147(9) 0.0213(9) 0.0106(8) -0.0004(7) 0.0026(7) 0.0005(7)
O4B 0.0145(9) 0.0264(10) 0.0102(8) -0.0021(7) 0.0067(7) -0.0015(7)
C1B 0.0131(11) 0.0210(12) 0.0122(12) 0.0004(9) 0.0035(9) -0.0004(9)
C2B 0.0147(12) 0.0300(14) 0.0101(11) 0.0002(10) 0.0045(9) -0.0037(10)
C3B 0.0144(12) 0.0251(13) 0.0140(12) 0.0006(10) 0.0037(10) -0.0005(10)
C4B 0.0157(12) 0.0222(13) 0.0161(12) -0.0022(10) 0.0047(10) -0.0004(10)
C5B 0.0156(12) 0.0223(13) 0.0156(12) 0.0014(10) 0.0052(10) -0.0006(10)
C6B 0.0122(11) 0.0218(12) 0.0111(11) 0.0003(9) 0.0041(9) -0.0028(9)
O1C 0.0196(10) 0.0315(11) 0.0239(10) -0.0036(8) 0.0096(8) -0.0087(8)
N1C 0.0218(12) 0.0246(12) 0.0232(12) 0.0017(10) 0.0098(10) -0.0004(9)
C1C 0.0251(14) 0.0195(13) 0.0208(13) -0.0039(10) 0.0088(11) -0.0045(10)
C2C 0.0272(15) 0.0404(18) 0.0209(14) 0.0012(13) 0.0082(12) -0.0054(13)
C3C 0.0222(15) 0.0410(18) 0.0319(17) 0.0054(14) 0.0144(13) 0.0013(13)
C4C 0.0308(16) 0.0332(17) 0.0273(16) 0.0064(13) 0.0104(13) 0.0083(13)

_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 O1A 2.131(2) . ?
Mn1 O4A 2.132(2) 4_576 ?
Mn1 O1B 2.175(2) . ?
Mn1 O3B 2.189(2) 1_655 ?
Mn1 O2B 2.2580(19) 4_575 ?
Mn1 O4B 2.261(2) 4_675 ?
Mn2 O2A 2.068(2) . ?
Mn2 O3A 2.085(2) 1_556 ?
Mn2 O1C 2.137(2) . ?
Mn2 O2B 2.2119(19) . ?
Mn2 O3B 2.253(2) 1_655 ?
Mn2 O4B 2.380(2) 1_655 ?
O1A C1A 1.260(3) . ?
O2A C1A 1.267(3) . ?
O3A C6A 1.262(3) . ?
O3A Mn2 2.085(2) 1_554 ?
O4A C6A 1.259(3) . ?
O4A Mn1 2.132(2) 4_575 ?
C1A C2A 1.510(4) . ?
C2A C3A 1.525(4) . ?
C3A C4A 1.524(4) . ?
C4A C5A 1.532(4) . ?
C5A C6A 1.514(4) . ?
O1B C1B 1.247(3) . ?
O2B C1B 1.282(3) . ?
O2B Mn1 2.2581(19) 4_576 ?
O3B C6B 1.281(3) . ?
O3B Mn1 2.189(2) 1_455 ?
O3B Mn2 2.253(2) 1_455 ?
O4B C6B 1.262(3) . ?
O4B Mn1 2.261(2) 4_476 ?
O4B Mn2 2.380(2) 1_455 ?
C1B C2B 1.520(4) . ?
C2B C3B 1.528(4) . ?
C3B C4B 1.528(4) . ?
C4B C5B 1.532(4) . ?
C5B C6B 1.499(4) . ?
O1C C1C 1.248(4) . ?
N1C C1C 1.332(4) . ?
N1C C3C 1.455(4) . ?
N1C C4C 1.466(4) . ?
C1C C2C 1.505(4) . ?

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
O1A Mn1 O4A 175.14(8) . 4_576 ?
O1A Mn1 O1B 90.47(8) . . ?
O4A Mn1 O1B 90.61(8) 4_576 . ?
O1A Mn1 O3B 93.44(8) . 1_655 ?
O4A Mn1 O3B 91.29(8) 4_576 1_655 ?
O1B Mn1 O3B 90.39(8) . 1_655 ?
O1A Mn1 O2B 84.95(7) . 4_575 ?
O4A Mn1 O2B 90.20(7) 4_576 4_575 ?
O1B Mn1 O2B 100.63(8) . 4_575 ?
O3B Mn1 O2B 168.87(7) 1_655 4_575 ?
O1A Mn1 O4B 89.54(7) . 4_675 ?
O4A Mn1 O4B 89.19(8) 4_576 4_675 ?
O1B Mn1 O4B 177.62(8) . 4_675 ?
O3B Mn1 O4B 91.99(7) 1_655 4_675 ?
O2B Mn1 O4B 77.00(7) 4_575 4_675 ?
O2A Mn2 O3A 94.56(8) . 1_556 ?
O2A Mn2 O1C 99.95(9) . . ?
O3A Mn2 O1C 88.85(9) 1_556 . ?
O2A Mn2 O2B 101.47(8) . . ?
O3A Mn2 O2B 87.49(8) 1_556 . ?
O1C Mn2 O2B 158.49(8) . . ?
O2A Mn2 O3B 101.63(8) . 1_655 ?
O3A Mn2 O3B 163.74(8) 1_556 1_655 ?
O1C Mn2 O3B 89.86(8) . 1_655 ?
O2B Mn2 O3B 87.79(7) . 1_655 ?
O2A Mn2 O4B 157.77(7) . 1_655 ?
O3A Mn2 O4B 107.18(7) 1_556 1_655 ?
O1C Mn2 O4B 85.41(8) . 1_655 ?
O2B Mn2 O4B 75.48(7) . 1_655 ?
O3B Mn2 O4B 56.56(7) 1_655 1_655 ?
C1A O1A Mn1 132.01(17) . . ?
C1A O2A Mn2 133.13(19) . . ?
C6A O3A Mn2 122.09(18) . 1_554 ?
C6A O4A Mn1 136.50(18) . 4_575 ?
O1A C1A O2A 125.2(3) . . ?
O1A C1A C2A 119.2(2) . . ?
O2A C1A C2A 115.6(2) . . ?
C1A C2A C3A 114.9(2) . . ?
C4A C3A C2A 113.1(2) . . ?
C3A C4A C5A 112.2(2) . . ?
C6A C5A C4A 116.0(2) . . ?
O4A C6A O3A 125.2(3) . . ?
O4A C6A C5A 119.8(2) . . ?
O3A C6A C5A 114.9(2) . . ?
C1B O1B Mn1 138.67(19) . . ?
C1B O2B Mn2 123.23(16) . . ?
C1B O2B Mn1 129.49(17) . 4_576 ?
Mn2 O2B Mn1 96.55(7) . 4_576 ?
C6B O3B Mn1 137.32(17) . 1_455 ?
C6B O3B Mn2 94.52(16) . 1_455 ?
Mn1 O3B Mn2 107.75(8) 1_455 1_455 ?
C6B O4B Mn1 131.47(17) . 4_476 ?
C6B O4B Mn2 89.17(16) . 1_455 ?
Mn1 O4B Mn2 91.89(7) 4_476 1_455 ?
O1B C1B O2B 124.3(2) . . ?
O1B C1B C2B 118.7(2) . . ?
O2B C1B C2B 117.0(2) . . ?
C1B C2B C3B 114.5(2) . . ?
C2B C3B C4B 113.3(2) . . ?
C3B C4B C5B 114.8(2) . . ?
C6B C5B C4B 115.3(2) . . ?
O4B C6B O3B 119.6(2) . . ?
O4B C6B C5B 119.8(2) . . ?
O3B C6B C5B 120.6(2) . . ?
C1C O1C Mn2 136.6(2) . . ?
C1C N1C C3C 122.9(3) . . ?
C1C N1C C4C 120.0(3) . . ?
C3C N1C C4C 116.9(3) . . ?
O1C C1C N1C 120.6(3) . . ?
O1C C1C C2C 120.7(3) . . ?
N1C C1C C2C 118.7(3) . . ?

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
Mn1 O1A C1A O2A 36.7(4) . . . . ?
Mn1 O1A C1A C2A -141.4(2) . . . . ?
Mn2 O2A C1A O1A -5.1(4) . . . . ?
Mn2 O2A C1A C2A 173.15(19) . . . . ?
O1A C1A C2A C3A -29.8(4) . . . . ?
O2A C1A C2A C3A 151.8(3) . . . . ?
C1A C2A C3A C4A -70.0(3) . . . . ?
C2A C3A C4A C5A -170.2(2) . . . . ?
C3A C4A C5A C6A -64.1(3) . . . . ?
Mn1 O4A C6A O3A -15.4(4) 4_575 . . . ?
Mn1 O4A C6A C5A 166.1(2) 4_575 . . . ?
Mn2 O3A C6A O4A -20.3(4) 1_554 . . . ?
Mn2 O3A C6A C5A 158.34(19) 1_554 . . . ?
C4A C5A C6A O4A -13.8(4) . . . . ?
C4A C5A C6A O3A 167.5(3) . . . . ?
Mn1 O1B C1B O2B 33.8(4) . . . . ?
Mn1 O1B C1B C2B -145.7(2) . . . . ?
Mn2 O2B C1B O1B 13.3(4) . . . . ?
Mn1 O2B C1B O1B -122.5(3) 4_576 . . . ?
Mn2 O2B C1B C2B -167.14(18) . . . . ?
Mn1 O2B C1B C2B 57.1(3) 4_576 . . . ?
O1B C1B C2B C3B -37.5(4) . . . . ?
O2B C1B C2B C3B 143.0(3) . . . . ?
C1B C2B C3B C4B 158.5(2) . . . . ?
C2B C3B C4B C5B 68.5(3) . . . . ?
C3B C4B C5B C6B 65.6(3) . . . . ?
Mn1 O4B C6B O3B 87.9(3) 4_476 . . . ?
Mn2 O4B C6B O3B -3.9(2) 1_455 . . . ?
Mn1 O4B C6B C5B -93.2(3) 4_476 . . . ?
Mn2 O4B C6B C5B 175.0(2) 1_455 . . . ?
Mn1 O3B C6B O4B -118.3(3) 1_455 . . . ?
Mn2 O3B C6B O4B 4.1(3) 1_455 . . . ?
Mn1 O3B C6B C5B 62.8(4) 1_455 . . . ?
Mn2 O3B C6B C5B -174.7(2) 1_455 . . . ?
C4B C5B C6B O4B -155.4(2) . . . . ?
C4B C5B C6B O3B 23.4(4) . . . . ?
Mn2 O1C C1C N1C -137.6(3) . . . . ?
Mn2 O1C C1C C2C 43.8(4) . . . . ?
C3C N1C C1C O1C 179.3(3) . . . . ?
C4C N1C C1C O1C 4.2(4) . . . . ?
C3C N1C C1C C2C -2.1(4) . . . . ?
C4C N1C C1C C2C -177.2(3) . . . . ?

_refine_diff_density_max         0.986
_refine_diff_density_min         -1.092
_refine_diff_density_rms         0.092
_database_code_depnum_ccdc_archive 'CCDC 922450'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_CoC4DC
#==============================================================================

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H23 Co2 N O9,1(C3 H7 N O),1.5(H2 O)'
_chemical_formula_sum            'C18 H33 Co2 N2 O11.5'
_chemical_formula_weight         579.33

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0048 0.0021 '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 0.0087 0.0042 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0151 0.0080 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3508 1.1967 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   28.365(4)
_cell_length_b                   28.365(4)
_cell_length_c                   13.361(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10750(4)
_cell_formula_units_Z            16
_cell_measurement_temperature    95(2)
_cell_measurement_reflns_used    75694
_cell_measurement_theta_min      0.46
_cell_measurement_theta_max      29.59

_exptl_crystal_description       rod
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_F_000             4816.0
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.79
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.618
_exptl_absorpt_correction_T_max  0.842
_exptl_absorpt_process_details   'HKL3000sm Scalepack'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      95(2)
_diffrn_radiation_wavelength     0.80003
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37241
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.286
_diffrn_reflns_theta_max         29.540
_diffrn_reflns_theta_full        28.687
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measured_fraction_theta_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_reflns_number_total             5124
_reflns_number_gt                4790
_reflns_threshold_expression     'I > 2\s(I)'
_reflns_Friedel_coverage         0.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_cell_refinement       HKL3000sm
_computing_data_reduction        HKL3000sm
_computing_structure_solution    'SHELXL-2013-XS (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013-XL (Sheldrick, 2013)'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  'WinGX, enCifer1.4'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[\s^2^(Fo^2^)+(0.0055P)^2^+157.7408P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00177(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         5124
_refine_ls_number_parameters     294
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0614
_refine_ls_wR_factor_ref         0.1423
_refine_ls_wR_factor_gt          0.1411
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_restrained_S_all      1.206
_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_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.85817(2) -0.00639(2) 0.59478(5) 0.0164(2) Uani 1 1 d . . . . .
Co2 Co 0.81324(2) 0.09566(2) 0.61692(5) 0.0165(2) Uani 1 1 d . . . . .
O1A O 0.82215(11) 0.04168(11) 0.5068(3) 0.0188(7) Uani 1 1 d . . . . .
O2A O 0.83615(12) 0.00791(11) 0.3595(3) 0.0202(7) Uani 1 1 d . . . . .
O3A O 0.69729(12) 0.05263(12) 0.1103(3) 0.0217(7) Uani 1 1 d . . . . .
O4A O 0.71495(11) 0.07556(11) -0.0446(3) 0.0182(7) Uani 1 1 d . . . . .
C1A C 0.81859(15) 0.04029(15) 0.4116(4) 0.0150(9) Uani 1 1 d . . . . .
C2A C 0.79200(18) 0.07924(17) 0.3607(4) 0.0220(10) Uani 1 1 d . . . . .
H2A1 H 0.8089 0.1093 0.3724 0.026 Uiso 1 1 calc R U . . .
H2A2 H 0.7605 0.0820 0.3922 0.026 Uiso 1 1 calc R U . . .
C3A C 0.78557(18) 0.07268(18) 0.2490(4) 0.0230(11) Uani 1 1 d . . . . .
H3A1 H 0.7670 0.0437 0.2366 0.028 Uiso 1 1 calc R U . . .
H3A2 H 0.8168 0.0687 0.2171 0.028 Uiso 1 1 calc R U . . .
C4A C 0.76056(19) 0.11452(18) 0.2026(4) 0.0245(11) Uani 1 1 d . . . . .
H4A1 H 0.7778 0.1437 0.2205 0.029 Uiso 1 1 calc R U . . .
H4A2 H 0.7285 0.1169 0.2313 0.029 Uiso 1 1 calc R U . . .
C5A C 0.75675(18) 0.11130(18) 0.0892(4) 0.0240(11) Uani 1 1 d . . . . .
H5A1 H 0.7490 0.1430 0.0628 0.029 Uiso 1 1 calc R U . . .
H5A2 H 0.7880 0.1024 0.0621 0.029 Uiso 1 1 calc R U . . .
C6A C 0.72064(16) 0.07670(16) 0.0500(4) 0.0175(10) Uani 1 1 d . . . . .
O1B O 0.88382(11) 0.10592(11) 0.6120(3) 0.0222(8) Uani 1 1 d . . . . .
O2B O 0.91749(12) 0.03442(12) 0.6032(3) 0.0235(8) Uani 1 1 d . . . . .
O3B O 1.11024(11) 0.05550(11) 0.5070(3) 0.0183(7) Uani 1 1 d . . . . .
O4B O 1.10010(12) 0.06533(12) 0.3455(3) 0.0224(8) Uani 1 1 d . . . . .
C1B C 0.91855(16) 0.07870(17) 0.6131(4) 0.0207(10) Uani 1 1 d . . . . .
C2B C 0.96599(17) 0.10169(18) 0.6260(4) 0.0259(11) Uani 1 1 d . . . . .
H2B1 H 0.9828 0.0862 0.6820 0.031 Uiso 1 1 calc R U . . .
H2B2 H 0.9613 0.1352 0.6442 0.031 Uiso 1 1 calc R U . . .
C3B C 0.99671(17) 0.09902(18) 0.5320(4) 0.0247(11) Uani 1 1 d . . . . .
H3B1 H 1.0062 0.0659 0.5202 0.030 Uiso 1 1 calc R U . . .
H3B2 H 0.9783 0.1097 0.4734 0.030 Uiso 1 1 calc R U . . .
C4B C 1.04047(16) 0.12957(17) 0.5430(4) 0.0224(11) Uani 1 1 d . . . . .
H4B1 H 1.0585 0.1189 0.6023 0.027 Uiso 1 1 calc R U . . .
H4B2 H 1.0307 0.1626 0.5548 0.027 Uiso 1 1 calc R U . . .
C5B C 1.07251(18) 0.12788(17) 0.4513(4) 0.0235(11) Uani 1 1 d . . . . .
H5B1 H 1.0539 0.1369 0.3917 0.028 Uiso 1 1 calc R U . . .
H5B2 H 1.0978 0.1516 0.4597 0.028 Uiso 1 1 calc R U . . .
C6B C 1.09489(16) 0.08044(16) 0.4322(4) 0.0191(10) Uani 1 1 d . . . . .
O1C O 0.80363(12) 0.15534(11) 0.5254(3) 0.0229(8) Uani 1 1 d . . . . .
N1C N 0.75668(17) 0.21731(15) 0.4857(4) 0.0293(10) Uani 1 1 d . . . . .
C1C C 0.77023(17) 0.18248(16) 0.5446(4) 0.0214(10) Uani 1 1 d . . . . .
H1C H 0.7535 0.1778 0.6054 0.026 Uiso 1 1 calc R U . . .
C2C C 0.7805(3) 0.2277(2) 0.3920(5) 0.0441(16) Uani 1 1 d . . . . .
H2C1 H 0.7957 0.2586 0.3965 0.066 Uiso 1 1 calc R U . . .
H2C2 H 0.7574 0.2279 0.3374 0.066 Uiso 1 1 calc R U . . .
H2C3 H 0.8043 0.2035 0.3789 0.066 Uiso 1 1 calc R U . . .
C3C C 0.7189(2) 0.2492(2) 0.5148(5) 0.0382(14) Uani 1 1 d . . . . .
H3C1 H 0.7011 0.2354 0.5704 0.057 Uiso 1 1 calc R U . . .
H3C2 H 0.6978 0.2543 0.4578 0.057 Uiso 1 1 calc R U . . .
H3C3 H 0.7324 0.2794 0.5358 0.057 Uiso 1 1 calc R U . . .
O1S O 0.8529(3) 0.2136(2) 0.1925(6) 0.086(2) Uani 1 1 d . . . . .
N1S N 0.8917(2) 0.1435(3) 0.1675(6) 0.070(2) Uani 1 1 d . . . . .
C1S C 0.8662(3) 0.1799(3) 0.1372(9) 0.072(3) Uani 1 1 d . . . . .
H1S H 0.8572 0.1807 0.0688 0.086 Uiso 1 1 calc R U . . .
C2S C 0.9063(4) 0.1071(4) 0.0938(9) 0.094(3) Uani 1 1 d . . . . .
H2S1 H 0.8935 0.0764 0.1139 0.141 Uiso 1 1 calc R U . . .
H2S2 H 0.9408 0.1053 0.0916 0.141 Uiso 1 1 calc R U . . .
H2S3 H 0.8942 0.1154 0.0274 0.141 Uiso 1 1 calc R U . . .
C3S C 0.9089(4) 0.1390(5) 0.2726(9) 0.115(5) Uani 1 1 d . . . . .
H3S1 H 0.9423 0.1476 0.2757 0.172 Uiso 1 1 calc R U . . .
H3S2 H 0.9049 0.1063 0.2952 0.172 Uiso 1 1 calc R U . . .
H3S3 H 0.8907 0.1600 0.3161 0.172 Uiso 1 1 calc R U . . .

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
Co1 0.0148(3) 0.0140(3) 0.0204(4) -0.0008(2) -0.0007(2) 0.0007(2)
Co2 0.0142(3) 0.0148(3) 0.0207(4) 0.0007(2) 0.0009(2) 0.0010(2)
O1A 0.0183(17) 0.0192(17) 0.0189(19) 0.0003(13) -0.0002(13) 0.0012(13)
O2A 0.0215(17) 0.0153(16) 0.0239(19) 0.0003(14) 0.0014(14) 0.0001(13)
O3A 0.0191(17) 0.0246(18) 0.0214(19) 0.0029(14) -0.0011(14) -0.0036(14)
O4A 0.0142(16) 0.0191(16) 0.0214(19) -0.0004(13) -0.0013(13) -0.0011(12)
C1A 0.011(2) 0.015(2) 0.019(3) -0.0023(18) 0.0011(17) -0.0014(16)
C2A 0.024(3) 0.021(2) 0.021(3) 0.001(2) 0.000(2) 0.0038(19)
C3A 0.026(3) 0.022(2) 0.021(3) 0.000(2) -0.003(2) 0.001(2)
C4A 0.029(3) 0.021(2) 0.024(3) -0.001(2) -0.005(2) -0.003(2)
C5A 0.026(3) 0.023(3) 0.023(3) 0.004(2) -0.003(2) -0.006(2)
C6A 0.015(2) 0.019(2) 0.019(3) 0.0008(18) -0.0007(18) -0.0005(17)
O1B 0.0176(17) 0.0150(16) 0.034(2) -0.0020(14) 0.0036(15) 0.0012(13)
O2B 0.0164(16) 0.0178(17) 0.036(2) -0.0026(15) -0.0001(15) 0.0002(13)
O3B 0.0161(16) 0.0164(16) 0.0225(19) 0.0000(13) 0.0000(13) 0.0016(12)
O4B 0.0211(17) 0.0211(17) 0.025(2) -0.0004(14) -0.0018(14) 0.0021(14)
C1B 0.014(2) 0.018(2) 0.030(3) -0.002(2) 0.0017(19) 0.0001(18)
C2B 0.020(3) 0.023(3) 0.034(3) -0.007(2) 0.003(2) -0.001(2)
C3B 0.016(2) 0.024(3) 0.034(3) -0.004(2) 0.001(2) 0.0001(19)
C4B 0.015(2) 0.017(2) 0.035(3) -0.003(2) -0.001(2) 0.0023(18)
C5B 0.022(2) 0.014(2) 0.034(3) -0.001(2) 0.002(2) 0.0019(19)
C6B 0.014(2) 0.018(2) 0.025(3) 0.0010(19) -0.0030(19) -0.0025(18)
O1C 0.0254(18) 0.0160(16) 0.027(2) 0.0036(14) 0.0024(15) 0.0044(14)
N1C 0.043(3) 0.016(2) 0.029(3) 0.0014(18) -0.006(2) 0.0073(19)
C1C 0.025(3) 0.015(2) 0.024(3) -0.0024(19) -0.002(2) 0.0005(19)
C2C 0.074(5) 0.031(3) 0.027(3) 0.008(3) 0.003(3) 0.008(3)
C3C 0.036(3) 0.025(3) 0.053(4) 0.001(3) -0.002(3) 0.014(2)
O1S 0.093(5) 0.070(4) 0.096(5) -0.010(4) -0.007(4) 0.002(4)
N1S 0.054(4) 0.072(5) 0.083(6) -0.010(4) -0.015(4) 0.009(3)
C1S 0.063(5) 0.056(5) 0.097(7) -0.001(5) -0.009(5) 0.018(4)
C2S 0.082(7) 0.095(8) 0.104(9) -0.032(7) -0.014(6) 0.023(6)
C3S 0.075(7) 0.184(14) 0.086(9) -0.006(9) -0.030(6) 0.016(8)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O2B 2.046(3) . ?
Co1 O3A 2.059(3) 2_655 ?
Co1 O1A 2.070(3) . ?
Co1 O4A 2.103(3) 4 ?
Co1 O3B 2.143(3) 9_756 ?
Co1 O4B 2.198(3) 9_756 ?
Co1 C6B 2.513(5) 9_756 ?
Co2 O1B 2.024(3) . ?
Co2 O2A 2.038(3) 3_545 ?
Co2 O1C 2.106(3) . ?
Co2 O3B 2.110(3) 15_666 ?
Co2 O4A 2.116(3) 4 ?
Co2 O1A 2.139(3) . ?
O1A C1A 1.277(6) . ?
O2A C1A 1.255(6) . ?
O2A Co2 2.039(3) 4_554 ?
O3A C6A 1.247(6) . ?
O3A Co1 2.059(3) 2_654 ?
O4A C6A 1.274(6) . ?
O4A Co1 2.103(3) 3_544 ?
O4A Co2 2.116(3) 3_544 ?
C1A C2A 1.500(6) . ?
C2A C3A 1.515(7) . ?
C3A C4A 1.515(7) . ?
C4A C5A 1.522(7) . ?
C5A C6A 1.512(6) . ?
O1B C1B 1.252(6) . ?
O2B C1B 1.263(6) . ?
O3B C6B 1.300(6) . ?
O3B Co2 2.110(3) 12_757 ?
O3B Co1 2.143(3) 9_756 ?
O4B C6B 1.243(6) . ?
O4B Co1 2.198(3) 9_756 ?
C1B C2B 1.505(7) . ?
C2B C3B 1.531(7) . ?
C3B C4B 1.521(7) . ?
C4B C5B 1.526(7) . ?
C5B C6B 1.510(6) . ?
C6B Co1 2.513(5) 9_756 ?
O1C C1C 1.248(6) . ?
N1C C1C 1.321(6) . ?
N1C C2C 1.452(8) . ?
N1C C3C 1.455(7) . ?
O1S C1S 1.267(11) . ?
N1S C1S 1.322(10) . ?
N1S C2S 1.487(12) . ?
N1S C3S 1.493(13) . ?

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
O2B Co1 O3A 169.62(15) . 2_655 ?
O2B Co1 O1A 93.69(13) . . ?
O3A Co1 O1A 95.73(13) 2_655 . ?
O2B Co1 O4A 90.41(13) . 4 ?
O3A Co1 O4A 87.08(13) 2_655 4 ?
O1A Co1 O4A 79.29(13) . 4 ?
O2B Co1 O3B 93.35(13) . 9_756 ?
O3A Co1 O3B 88.25(13) 2_655 9_756 ?
O1A Co1 O3B 105.91(13) . 9_756 ?
O4A Co1 O3B 173.35(13) 4 9_756 ?
O2B Co1 O4B 88.14(13) . 9_756 ?
O3A Co1 O4B 83.70(13) 2_655 9_756 ?
O1A Co1 O4B 166.58(14) . 9_756 ?
O4A Co1 O4B 114.02(13) 4 9_756 ?
O3B Co1 O4B 60.69(13) 9_756 9_756 ?
O2B Co1 C6B 92.57(14) . 9_756 ?
O3A Co1 C6B 83.50(14) 2_655 9_756 ?
O1A Co1 C6B 136.94(15) . 9_756 ?
O4A Co1 C6B 143.22(15) 4 9_756 ?
O3B Co1 C6B 31.15(14) 9_756 9_756 ?
O4B Co1 C6B 29.64(15) 9_756 9_756 ?
O1B Co2 O2A 175.32(15) . 3_545 ?
O1B Co2 O1C 89.64(14) . . ?
O2A Co2 O1C 87.14(14) 3_545 . ?
O1B Co2 O3B 92.50(13) . 15_666 ?
O2A Co2 O3B 90.81(13) 3_545 15_666 ?
O1C Co2 O3B 88.50(13) . 15_666 ?
O1B Co2 O4A 88.37(13) . 4 ?
O2A Co2 O4A 94.76(13) 3_545 4 ?
O1C Co2 O4A 177.55(14) . 4 ?
O3B Co2 O4A 93.02(13) 15_666 4 ?
O1B Co2 O1A 87.92(13) . . ?
O2A Co2 O1A 89.37(13) 3_545 . ?
O1C Co2 O1A 101.02(13) . . ?
O3B Co2 O1A 170.48(13) 15_666 . ?
O4A Co2 O1A 77.49(13) 4 . ?
C1A O1A Co1 125.8(3) . . ?
C1A O1A Co2 134.3(3) . . ?
Co1 O1A Co2 97.99(14) . . ?
C1A O2A Co2 138.6(3) . 4_554 ?
C6A O3A Co1 133.6(3) . 2_654 ?
C6A O4A Co1 128.0(3) . 3_544 ?
C6A O4A Co2 131.4(3) . 3_544 ?
Co1 O4A Co2 97.69(14) 3_544 3_544 ?
O2A C1A O1A 122.9(4) . . ?
O2A C1A C2A 119.2(4) . . ?
O1A C1A C2A 117.9(4) . . ?
C1A C2A C3A 114.6(4) . . ?
C2A C3A C4A 111.3(4) . . ?
C3A C4A C5A 113.2(4) . . ?
C6A C5A C4A 115.6(4) . . ?
O3A C6A O4A 124.0(4) . . ?
O3A C6A C5A 119.4(4) . . ?
O4A C6A C5A 116.5(4) . . ?
C1B O1B Co2 133.6(3) . . ?
C1B O2B Co1 126.0(3) . . ?
C6B O3B Co2 139.1(3) . 12_757 ?
C6B O3B Co1 90.3(3) . 9_756 ?
Co2 O3B Co1 109.05(14) 12_757 9_756 ?
C6B O4B Co1 89.4(3) . 9_756 ?
O1B C1B O2B 126.4(4) . . ?
O1B C1B C2B 116.0(4) . . ?
O2B C1B C2B 117.7(4) . . ?
C1B C2B C3B 113.1(4) . . ?
C4B C3B C2B 110.9(4) . . ?
C3B C4B C5B 113.0(4) . . ?
C6B C5B C4B 114.5(4) . . ?
O4B C6B O3B 119.2(4) . . ?
O4B C6B C5B 121.0(4) . . ?
O3B C6B C5B 119.7(4) . . ?
O4B C6B Co1 61.0(2) . 9_756 ?
O3B C6B Co1 58.5(2) . 9_756 ?
C5B C6B Co1 172.8(3) . 9_756 ?
C1C O1C Co2 118.3(3) . . ?
C1C N1C C2C 122.0(5) . . ?
C1C N1C C3C 121.3(5) . . ?
C2C N1C C3C 116.5(5) . . ?
O1C C1C N1C 124.0(5) . . ?
C1S N1S C2S 119.5(9) . . ?
C1S N1S C3S 122.2(9) . . ?
C2S N1S C3S 118.2(9) . . ?
O1S C1S N1S 125.0(10) . . ?

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
Co2 O2A C1A O1A 38.3(7) 4_554 . . . ?
Co2 O2A C1A C2A -141.5(4) 4_554 . . . ?
Co1 O1A C1A O2A 1.9(6) . . . . ?
Co2 O1A C1A O2A 162.4(3) . . . . ?
Co1 O1A C1A C2A -178.3(3) . . . . ?
Co2 O1A C1A C2A -17.8(6) . . . . ?
O2A C1A C2A C3A 5.1(6) . . . . ?
O1A C1A C2A C3A -174.7(4) . . . . ?
C1A C2A C3A C4A -177.2(4) . . . . ?
C2A C3A C4A C5A 175.4(4) . . . . ?
C3A C4A C5A C6A 74.6(6) . . . . ?
Co1 O3A C6A O4A -3.3(7) 2_654 . . . ?
Co1 O3A C6A C5A 173.9(3) 2_654 . . . ?
Co1 O4A C6A O3A -172.6(3) 3_544 . . . ?
Co2 O4A C6A O3A 31.3(7) 3_544 . . . ?
Co1 O4A C6A C5A 10.1(6) 3_544 . . . ?
Co2 O4A C6A C5A -146.0(3) 3_544 . . . ?
C4A C5A C6A O3A -1.5(7) . . . . ?
C4A C5A C6A O4A 175.9(4) . . . . ?
Co2 O1B C1B O2B 11.2(9) . . . . ?
Co2 O1B C1B C2B -169.8(4) . . . . ?
Co1 O2B C1B O1B -5.8(8) . . . . ?
Co1 O2B C1B C2B 175.2(3) . . . . ?
O1B C1B C2B C3B -111.1(5) . . . . ?
O2B C1B C2B C3B 68.1(6) . . . . ?
C1B C2B C3B C4B 170.5(4) . . . . ?
C2B C3B C4B C5B 179.6(4) . . . . ?
C3B C4B C5B C6B -65.8(6) . . . . ?
Co1 O4B C6B O3B -6.0(4) 9_756 . . . ?
Co1 O4B C6B C5B 172.0(4) 9_756 . . . ?
Co2 O3B C6B O4B 126.5(4) 12_757 . . . ?
Co1 O3B C6B O4B 6.1(4) 9_756 . . . ?
Co2 O3B C6B C5B -51.5(7) 12_757 . . . ?
Co1 O3B C6B C5B -171.9(4) 9_756 . . . ?
Co2 O3B C6B Co1 120.4(4) 12_757 . . 9_756 ?
C4B C5B C6B O4B 142.1(5) . . . . ?
C4B C5B C6B O3B -39.9(6) . . . . ?
Co2 O1C C1C N1C -170.6(4) . . . . ?
C2C N1C C1C O1C -1.0(8) . . . . ?
C3C N1C C1C O1C -176.9(5) . . . . ?
C2S N1S C1S O1S -177.9(9) . . . . ?
C3S N1S C1S O1S -1.5(16) . . . . ?

_refine_diff_density_max         0.498
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.109

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.250 0.881 409 61 ' '
2 0.000 0.750 0.076 409 61 ' '
3 0.500 0.250 0.183 409 61 ' '
4 0.500 0.750 0.806 409 61 ' '
_platon_squeeze_details          
;
The 244 electrons removed from the unit cell, corresponds with 244/16 = 15.25 electrons per Co~2~ 
formula unit and corresponds with the removal of 1.5 molecules of water from the formula unit, so that the formula unit is
 {[Co~2~(adipate)~2~(DMF)]1DMF1.5(H~2~O)}. 
;
_database_code_depnum_ccdc_archive 'CCDC 922451'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_TbC4DC
#==============================================================================

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H50 N2 O20 Tb3'
_chemical_formula_sum            'C33 H50 N2 O20 Tb3'
_chemical_formula_weight         1271.51

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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   12.108(2)
_cell_length_b                   17.477(4)
_cell_length_c                   20.111(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.99(3)
_cell_angle_gamma                90
_cell_volume                     4253.1(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9693
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      27.48

_exptl_crystal_description       'parallel piped'
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.986
_exptl_crystal_F_000             2468
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    5.013
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.434
_exptl_absorpt_correction_T_max  0.434
_exptl_absorpt_process_details   'DENZO Scalepack'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Enraf-Nonius Kappa CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16558
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.258
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_reflns_number_total             9670
_reflns_number_gt                7249
_reflns_threshold_expression     'I > 2\s(I)'
_reflns_Friedel_coverage         0.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       DENZO
_computing_cell_refinement       DENZO
_computing_data_reduction        DENZO
_computing_structure_solution    'SHELXL-2013-XS (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013-XL (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP 3'
_computing_publication_material  WinGX

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+14.5087P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9670
_refine_ls_number_parameters     587
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0396
_refine_ls_wR_factor_ref         0.0937
_refine_ls_wR_factor_gt          0.0827
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.002
_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_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 1.01934(2) 0.75097(2) 0.69472(2) 0.01781(7) Uani 1 1 d . . . . .
Tb2 Tb 0.86642(2) 0.76382(2) 0.86985(2) 0.02093(8) Uani 1 1 d . . . . .
Tb3 Tb 0.69952(2) 0.73938(2) 1.03073(2) 0.01591(7) Uani 1 1 d . . . . .
O1A O 1.1105(3) 0.8685(2) 0.7297(2) 0.0355(10) Uani 1 1 d . . . . .
O2A O 1.0164(3) 0.8135(2) 0.80689(17) 0.0273(9) Uani 1 1 d . . . . .
O3A O 1.1309(3) 1.1141(3) 1.0780(2) 0.0366(10) Uani 1 1 d . . . . .
O4A O 1.1730(3) 1.1659(2) 0.9813(2) 0.0335(10) Uani 1 1 d . . . . .
C1A C 1.0656(5) 0.8720(3) 0.7849(3) 0.0299(13) Uani 1 1 d . . . . .
C2A C 1.0634(6) 0.9475(4) 0.8209(3) 0.0506(19) Uani 1 1 d . . . . .
H2A1 H 1.0948 0.9864 0.7928 0.061 Uiso 1 1 calc R U . . .
H2A2 H 0.9871 0.9614 0.8278 0.061 Uiso 1 1 calc R U . . .
C3A C 1.1240(7) 0.9477(4) 0.8857(3) 0.0510(19) Uani 1 1 d . . . . .
H3A1 H 1.2002 0.9330 0.8797 0.061 Uiso 1 1 calc R U . . .
H3A2 H 1.0911 0.9108 0.9152 0.061 Uiso 1 1 calc R U . . .
C4A C 1.1199(8) 1.0285(4) 0.9172(4) 0.065(2) Uani 1 1 d . . . . .
H4A1 H 1.1662 1.0626 0.8922 0.078 Uiso 1 1 calc R U . . .
H4A2 H 1.0447 1.0475 0.9131 0.078 Uiso 1 1 calc R U . . .
C5A C 1.1558(6) 1.0311(4) 0.9866(3) 0.0449(17) Uani 1 1 d . . . . .
H5A1 H 1.2307 1.0115 0.9907 0.054 Uiso 1 1 calc R U . . .
H5A2 H 1.1091 0.9972 1.0116 0.054 Uiso 1 1 calc R U . . .
C6A C 1.1530(4) 1.1094(4) 1.0176(3) 0.0304(14) Uani 1 1 d . . . . .
O1B O 0.8631(3) 0.8288(2) 0.68839(19) 0.0333(10) Uani 1 1 d . . . . .
O2B O 0.7806(3) 0.8383(2) 0.78512(19) 0.0304(9) Uani 1 1 d . . . . .
O3B O 0.6103(3) 1.1887(2) 0.74074(19) 0.0295(9) Uani 1 1 d . . . . .
O4B O 0.7557(3) 1.1681(2) 0.6823(2) 0.0344(10) Uani 1 1 d . . . . .
C1B C 0.7893(5) 0.8537(3) 0.7245(3) 0.0276(13) Uani 1 1 d . . . . .
C2B C 0.7048(6) 0.9066(4) 0.6930(3) 0.0434(17) Uani 1 1 d . . . . .
H2B1 H 0.6381 0.8775 0.6829 0.052 Uiso 1 1 calc R U . . .
H2B2 H 0.7325 0.9246 0.6511 0.052 Uiso 1 1 calc R U . . .
C3B C 0.6743(6) 0.9758(4) 0.7343(4) 0.0477(18) Uani 1 1 d . . . . .
H3B1 H 0.6375 0.9587 0.7737 0.057 Uiso 1 1 calc R U . . .
H3B2 H 0.6228 1.0076 0.7086 0.057 Uiso 1 1 calc R U . . .
C4B C 0.7752(6) 1.0233(4) 0.7552(4) 0.060(2) Uani 1 1 d . . . . .
H4B1 H 0.8191 0.9949 0.7881 0.073 Uiso 1 1 calc R U . . .
H4B2 H 0.8202 1.0312 0.7168 0.073 Uiso 1 1 calc R U . . .
C5B C 0.7461(6) 1.1001(4) 0.7840(3) 0.0416(16) Uani 1 1 d . . . . .
H5B1 H 0.6912 1.0929 0.8175 0.050 Uiso 1 1 calc R U . . .
H5B2 H 0.8115 1.1220 0.8059 0.050 Uiso 1 1 calc R U . . .
C6B C 0.7023(5) 1.1547(3) 0.7329(3) 0.0272(13) Uani 1 1 d . . . . .
O1C O 0.9401(3) 0.6241(3) 0.8950(2) 0.0387(11) Uani 1 1 d . . . . .
O2C O 0.8248(3) 0.6778(2) 0.96167(18) 0.0261(9) Uani 1 1 d . . . . .
C1C C 0.8780(4) 0.6187(3) 0.9420(3) 0.0265(13) Uani 1 1 d . . . . .
C2C C 0.8566(5) 0.5441(4) 0.9763(3) 0.0408(16) Uani 1 1 d . . . . .
H2C1 H 0.7927 0.5201 0.9547 0.049 Uiso 1 1 calc R U . . .
H2C2 H 0.8382 0.5547 1.0220 0.049 Uiso 1 1 calc R U . . .
C3C C 0.9519(5) 0.4882(4) 0.9768(3) 0.0409(16) Uani 1 1 d . . . . .
H3C1 H 0.9781 0.4834 0.9319 0.049 Uiso 1 1 calc R U . . .
H3C2 H 0.9255 0.4383 0.9903 0.049 Uiso 1 1 calc R U . . .
O1D O 0.6853(3) 0.7847(2) 0.91212(17) 0.0237(8) Uani 1 1 d . . . . .
O2D O 0.5570(3) 0.7073(3) 0.94637(19) 0.0351(10) Uani 1 1 d . . . . .
O3D O 0.3502(3) 0.7915(3) 0.6145(2) 0.0350(10) Uani 1 1 d . . . . .
O4D O 0.2016(3) 0.7368(2) 0.65090(18) 0.0270(9) Uani 1 1 d . . . . .
C1D C 0.5943(4) 0.7480(3) 0.9022(3) 0.0251(12) Uani 1 1 d . . . . .
C2D C 0.5312(5) 0.7582(4) 0.8368(3) 0.0328(14) Uani 1 1 d . . . . .
H2D1 H 0.4807 0.8009 0.8408 0.039 Uiso 1 1 calc R U . . .
H2D2 H 0.5830 0.7711 0.8029 0.039 Uiso 1 1 calc R U . . .
C3D C 0.4665(5) 0.6892(4) 0.8146(3) 0.0441(17) Uani 1 1 d . . . . .
H3D1 H 0.4056 0.6819 0.8440 0.053 Uiso 1 1 calc R U . . .
H3D2 H 0.5138 0.6445 0.8183 0.053 Uiso 1 1 calc R U . . .
C4D C 0.4204(6) 0.6953(5) 0.7427(3) 0.0478(18) Uani 1 1 d . . . . .
H4D1 H 0.4815 0.6982 0.7129 0.057 Uiso 1 1 calc R U . . .
H4D2 H 0.3787 0.6493 0.7318 0.057 Uiso 1 1 calc R U . . .
C5D C 0.3474(5) 0.7633(4) 0.7314(3) 0.0416(17) Uani 1 1 d . . . . .
H5D1 H 0.3900 0.8096 0.7394 0.050 Uiso 1 1 calc R U . . .
H5D2 H 0.2884 0.7623 0.7629 0.050 Uiso 1 1 calc R U . . .
C6D C 0.2978(4) 0.7649(3) 0.6613(3) 0.0269(12) Uani 1 1 d . . . . .
O1E O 0.6616(3) 0.6093(2) 1.05855(19) 0.0306(9) Uani 1 1 d . . . . .
O2E O 0.5301(3) 0.6851(2) 1.09093(17) 0.0240(8) Uani 1 1 d . . . . .
C1E C 0.5656(4) 0.6182(3) 1.0790(2) 0.0225(12) Uani 1 1 d . . . . .
C2E C 0.4925(6) 0.5500(4) 1.0858(3) 0.0381(16) Uani 1 1 d . . . . .
H2E1 H 0.4161 0.5662 1.0806 0.046 Uiso 1 1 calc R U . . .
H2E2 H 0.5031 0.5293 1.1303 0.046 Uiso 1 1 calc R U . . .
C3E C 0.5139(6) 0.4869(3) 1.0355(3) 0.0393(16) Uani 1 1 d . . . . .
H3E1 H 0.5910 0.4720 1.0390 0.047 Uiso 1 1 calc R U . . .
H3E2 H 0.4695 0.4425 1.0456 0.047 Uiso 1 1 calc R U . . .
O1F O 0.5816(3) 0.8441(2) 1.0368(2) 0.0393(11) Uani 1 1 d . . . . .
O2F O 0.4687(4) 0.8433(3) 1.1207(2) 0.0432(12) Uani 1 1 d . . . . .
C1F C 0.4960(5) 0.8641(4) 1.0639(3) 0.0357(15) Uani 1 1 d . . . . .
C2F C 0.4188(6) 0.9174(6) 1.0259(4) 0.077(3) Uani 1 1 d . . . . .
H2F1 H 0.3617 0.8868 1.0038 0.092 Uiso 1 1 calc R U . . .
H2F2 H 0.3830 0.9499 1.0578 0.092 Uiso 1 1 calc R U . . .
C3F C 0.4685(8) 0.9668(5) 0.9758(4) 0.085(3) Uani 1 1 d . . . . .
H3F1 H 0.4126 0.9894 0.9462 0.101 Uiso 1 1 calc R U . . .
H3F2 H 0.5211 0.9389 0.9497 0.101 Uiso 1 1 calc R U . . .
O1G O 1.1153(4) 0.6607(3) 0.7614(3) 0.0515(13) Uani 1 1 d . . . . .
N1G N 1.1495(5) 0.5387(4) 0.7911(4) 0.0554(17) Uani 1 1 d . . . . .
C1G C 1.1331(12) 0.6125(9) 0.7985(8) 0.051(4) Uani 0.557(14) 1 d . . P A 1
H1G H 1.1367 0.6285 0.8426 0.061 Uiso 0.557(14) 1 calc R U P A 1
C2G C 1.1374(15) 0.5155(12) 0.7152(9) 0.095(7) Uani 0.557(14) 1 d . . P A 1
H2G1 H 1.1180 0.5599 0.6891 0.142 Uiso 0.557(14) 1 calc R U P A 1
H2G2 H 1.0807 0.4775 0.7095 0.142 Uiso 0.557(14) 1 calc R U P A 1
H2G3 H 1.2063 0.4952 0.7008 0.142 Uiso 0.557(14) 1 calc R U P A 1
C3G C 1.168(2) 0.4802(14) 0.8311(12) 0.124(12) Uani 0.557(14) 1 d . . P A 1
H3G1 H 1.1675 0.4973 0.8765 0.186 Uiso 0.557(14) 1 calc R U P A 1
H3G2 H 1.2385 0.4581 0.8223 0.186 Uiso 0.557(14) 1 calc R U P A 1
H3G3 H 1.1110 0.4426 0.8237 0.186 Uiso 0.557(14) 1 calc R U P A 1
C11G C 1.1009(13) 0.5866(9) 0.7580(9) 0.034(4) Uani 0.443(14) 1 d . . P A 2
H11G H 1.0480 0.5690 0.7271 0.041 Uiso 0.443(14) 1 calc R U P A 2
C21G C 1.130(2) 0.4541(11) 0.7870(15) 0.074(9) Uani 0.443(14) 1 d . . P A 2
H21A H 1.0845 0.4384 0.8226 0.111 Uiso 0.443(14) 1 calc R U P A 2
H21B H 1.1998 0.4278 0.7906 0.111 Uiso 0.443(14) 1 calc R U P A 2
H21C H 1.0941 0.4419 0.7451 0.111 Uiso 0.443(14) 1 calc R U P A 2
C31G C 1.217(2) 0.5595(12) 0.8547(11) 0.098(10) Uani 0.443(14) 1 d . . P A 2
H31A H 1.2854 0.5320 0.8558 0.148 Uiso 0.443(14) 1 calc R U P A 2
H31B H 1.1755 0.5459 0.8929 0.148 Uiso 0.443(14) 1 calc R U P A 2
H31C H 1.2312 0.6135 0.8553 0.148 Uiso 0.443(14) 1 calc R U P A 2
O1H O 1.0307(4) 0.7656(3) 0.9399(3) 0.0605(16) Uani 1 1 d . . . . .
N1H N 1.1758(5) 0.7417(4) 1.0061(3) 0.0520(16) Uani 0.564(17) 1 d . . P B 1
C1H C 1.1164(10) 0.7420(8) 0.9489(7) 0.044(4) Uani 0.564(17) 1 d . . P B 1
H1H H 1.1497 0.7204 0.9124 0.053 Uiso 0.564(17) 1 calc R U P B 1
C2H C 1.2854(13) 0.7016(13) 1.0079(12) 0.093(7) Uani 0.564(17) 1 d . . P B 1
H2H1 H 1.2766 0.6506 1.0246 0.140 Uiso 0.564(17) 1 calc R U P B 1
H2H2 H 1.3366 0.7291 1.0365 0.140 Uiso 0.564(17) 1 calc R U P B 1
H2H3 H 1.3131 0.6995 0.9638 0.140 Uiso 0.564(17) 1 calc R U P B 1
C3H C 1.136(2) 0.7682(15) 1.0654(9) 0.112(9) Uani 0.564(17) 1 d . . P B 1
H3H1 H 1.0625 0.7873 1.0581 0.167 Uiso 0.564(17) 1 calc R U P B 1
H3H2 H 1.1831 0.8086 1.0822 0.167 Uiso 0.564(17) 1 calc R U P B 1
H3H3 H 1.1357 0.7271 1.0971 0.167 Uiso 0.564(17) 1 calc R U P B 1
N11H N 1.1758(5) 0.7417(4) 1.0061(3) 0.0520(16) Uani 0.436(17) 1 d . . P B 2
C11H C 1.0714(13) 0.7545(8) 0.9866(9) 0.034(5) Uani 0.436(17) 1 d . . P B 2
H11H H 1.0233 0.7537 1.0216 0.041 Uiso 0.436(17) 1 calc R U P B 2
C21H C 1.2630(17) 0.7378(17) 0.9612(14) 0.090(10) Uani 0.436(17) 1 d . . P B 2
H21D H 1.2864 0.6856 0.9568 0.135 Uiso 0.436(17) 1 calc R U P B 2
H21E H 1.3239 0.7683 0.9778 0.135 Uiso 0.436(17) 1 calc R U P B 2
H21F H 1.2378 0.7569 0.9185 0.135 Uiso 0.436(17) 1 calc R U P B 2
C31H C 1.207(2) 0.7478(18) 1.0803(11) 0.097(10) Uani 0.436(17) 1 d . . P B 2
H31D H 1.2507 0.7927 1.0881 0.145 Uiso 0.436(17) 1 calc R U P B 2
H31E H 1.2480 0.7033 1.0941 0.145 Uiso 0.436(17) 1 calc R U P B 2
H31F H 1.1406 0.7511 1.1052 0.145 Uiso 0.436(17) 1 calc R U P B 2

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
Tb1 0.02088(13) 0.01831(13) 0.01439(13) 0.00072(10) 0.00254(10) -0.00128(10)
Tb2 0.01982(13) 0.02499(15) 0.01804(13) 0.00640(11) 0.00137(9) -0.00045(11)
Tb3 0.01761(12) 0.01935(14) 0.01064(12) 0.00035(9) -0.00153(9) -0.00062(10)
O1A 0.038(2) 0.037(3) 0.033(2) -0.004(2) 0.0141(19) -0.014(2)
O2A 0.032(2) 0.034(2) 0.0168(19) -0.0039(17) 0.0025(16) -0.0064(18)
O3A 0.038(2) 0.040(3) 0.033(2) -0.005(2) 0.0065(19) -0.004(2)
O4A 0.034(2) 0.027(2) 0.039(2) -0.001(2) -0.0037(19) -0.0085(19)
C1A 0.028(3) 0.029(3) 0.032(3) -0.008(3) -0.004(3) -0.007(3)
C2A 0.067(5) 0.041(4) 0.045(4) -0.010(3) 0.011(4) -0.016(4)
C3A 0.073(5) 0.035(4) 0.045(4) -0.007(3) -0.004(4) -0.006(4)
C4A 0.106(7) 0.042(5) 0.045(5) -0.006(4) -0.015(4) -0.003(5)
C5A 0.054(4) 0.025(3) 0.056(5) -0.009(3) 0.018(4) -0.002(3)
C6A 0.017(3) 0.033(3) 0.042(4) -0.011(3) 0.003(3) -0.001(2)
O1B 0.034(2) 0.043(3) 0.023(2) 0.0085(19) 0.0053(17) 0.014(2)
O2B 0.033(2) 0.036(2) 0.023(2) 0.0070(18) 0.0028(17) 0.0091(19)
O3B 0.035(2) 0.028(2) 0.026(2) -0.0038(17) 0.0071(17) 0.0116(18)
O4B 0.036(2) 0.035(2) 0.033(2) 0.004(2) 0.0115(19) 0.0041(19)
C1B 0.028(3) 0.023(3) 0.032(3) 0.004(3) 0.002(3) 0.006(2)
C2B 0.047(4) 0.049(4) 0.034(4) 0.011(3) 0.000(3) 0.025(3)
C3B 0.042(4) 0.038(4) 0.062(5) 0.009(4) 0.000(3) 0.021(3)
C4B 0.051(5) 0.050(5) 0.080(6) 0.016(4) -0.001(4) 0.020(4)
C5B 0.056(4) 0.039(4) 0.030(4) 0.006(3) 0.000(3) 0.016(3)
C6B 0.041(3) 0.011(3) 0.029(3) -0.004(2) -0.002(3) 0.001(2)
O1C 0.042(2) 0.047(3) 0.028(2) 0.011(2) 0.0173(19) 0.018(2)
O2C 0.027(2) 0.027(2) 0.025(2) 0.0022(17) 0.0044(16) 0.0034(17)
C1C 0.024(3) 0.032(3) 0.023(3) 0.005(2) 0.000(2) 0.009(3)
C2C 0.037(4) 0.034(4) 0.052(4) 0.017(3) 0.004(3) 0.009(3)
C3C 0.052(4) 0.023(3) 0.048(4) 0.006(3) 0.004(3) 0.012(3)
O1D 0.0201(18) 0.033(2) 0.0179(18) 0.0032(17) -0.0038(14) -0.0020(17)
O2D 0.031(2) 0.053(3) 0.021(2) 0.009(2) -0.0044(17) -0.015(2)
O3D 0.027(2) 0.048(3) 0.029(2) 0.002(2) -0.0042(17) -0.010(2)
O4D 0.0219(19) 0.039(2) 0.0194(19) -0.0024(17) -0.0052(15) -0.0021(18)
C1D 0.024(3) 0.033(3) 0.019(3) 0.001(2) -0.004(2) -0.001(2)
C2D 0.027(3) 0.049(4) 0.021(3) 0.010(3) -0.010(2) 0.000(3)
C3D 0.038(4) 0.052(4) 0.041(4) 0.012(3) -0.018(3) -0.004(3)
C4D 0.051(4) 0.062(5) 0.029(4) -0.001(3) -0.018(3) 0.004(4)
C5D 0.036(3) 0.062(5) 0.026(3) -0.007(3) -0.015(3) 0.006(3)
C6D 0.027(3) 0.033(3) 0.020(3) -0.002(3) -0.005(2) 0.008(3)
O1E 0.031(2) 0.027(2) 0.035(2) -0.0042(18) 0.0091(18) -0.0023(18)
O2E 0.030(2) 0.025(2) 0.0165(19) 0.0002(16) 0.0022(16) -0.0012(17)
C1E 0.031(3) 0.026(3) 0.011(2) -0.003(2) -0.001(2) -0.006(2)
C2E 0.052(4) 0.032(3) 0.031(3) -0.013(3) 0.016(3) -0.016(3)
C3E 0.055(4) 0.022(3) 0.040(4) -0.007(3) -0.001(3) -0.011(3)
O1F 0.044(3) 0.034(2) 0.041(3) 0.012(2) 0.012(2) 0.015(2)
O2F 0.056(3) 0.039(3) 0.036(3) 0.019(2) 0.016(2) 0.023(2)
C1F 0.035(3) 0.038(4) 0.034(4) 0.009(3) 0.002(3) 0.012(3)
C2F 0.050(5) 0.099(7) 0.082(6) 0.064(6) 0.012(4) 0.024(5)
C3F 0.088(7) 0.078(7) 0.088(8) 0.048(6) 0.010(5) 0.029(6)
O1G 0.044(3) 0.042(3) 0.069(4) 0.028(3) 0.006(2) 0.012(2)
N1G 0.051(4) 0.037(4) 0.078(5) 0.014(4) 0.010(3) 0.015(3)
C1G 0.053(9) 0.050(9) 0.052(10) 0.016(8) 0.021(8) 0.028(8)
C2G 0.094(14) 0.107(17) 0.085(14) -0.029(12) 0.029(11) 0.002(12)
C3G 0.16(3) 0.09(2) 0.12(2) 0.051(17) 0.035(19) 0.06(2)
C11G 0.035(8) 0.032(9) 0.037(10) -0.003(7) 0.005(7) -0.004(7)
C21G 0.069(14) 0.016(9) 0.14(3) 0.002(12) 0.002(15) 0.005(9)
C31G 0.14(2) 0.051(13) 0.102(19) 0.019(13) -0.093(16) -0.004(13)
O1H 0.037(3) 0.077(4) 0.066(4) 0.034(3) -0.020(3) -0.009(3)
N1H 0.038(3) 0.068(5) 0.049(4) 0.004(3) -0.022(3) 0.003(3)
C1H 0.033(7) 0.064(9) 0.036(7) -0.002(6) 0.006(6) 0.006(6)
C2H 0.062(11) 0.111(17) 0.105(17) 0.009(14) -0.034(11) 0.026(11)
C3H 0.118(18) 0.16(2) 0.051(12) -0.007(13) -0.043(12) 0.039(17)
N11H 0.038(3) 0.068(5) 0.049(4) 0.004(3) -0.022(3) 0.003(3)
C11H 0.027(8) 0.034(9) 0.041(10) 0.010(7) -0.004(7) -0.010(6)
C21H 0.039(11) 0.13(3) 0.10(2) -0.021(18) 0.010(12) 0.011(14)
C31H 0.091(19) 0.14(3) 0.054(14) 0.026(15) -0.040(13) -0.028(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
Tb1 O2F 2.290(4) 4_675 ?
Tb1 O1B 2.330(4) . ?
Tb1 O3B 2.340(4) 2_646 ?
Tb1 O1G 2.350(5) . ?
Tb1 O2E 2.375(4) 4_675 ?
Tb1 O4D 2.417(4) 1_655 ?
Tb1 O1A 2.425(4) . ?
Tb1 O2A 2.508(4) . ?
Tb1 C1A 2.830(6) . ?
Tb2 O2B 2.357(4) . ?
Tb2 O3A 2.377(4) 3_777 ?
Tb2 O1H 2.397(5) . ?
Tb2 O1D 2.407(3) . ?
Tb2 O2A 2.411(4) . ?
Tb2 O4B 2.445(4) 2_646 ?
Tb2 O2C 2.447(4) . ?
Tb2 O3B 2.607(4) 2_646 ?
Tb2 O1C 2.643(4) . ?
Tb2 C6B 2.912(6) 2_646 ?
Tb2 C1C 2.923(6) . ?
Tb2 Tb3 3.8972(11) . ?
Tb3 O4A 2.282(4) 3_777 ?
Tb3 O1F 2.328(4) . ?
Tb3 O2C 2.352(4) . ?
Tb3 O1E 2.390(4) . ?
Tb3 O2D 2.443(4) . ?
Tb3 O4D 2.452(4) 4_676 ?
Tb3 O3D 2.499(4) 4_676 ?
Tb3 O1D 2.514(3) . ?
Tb3 O2E 2.597(4) . ?
Tb3 C1D 2.845(5) . ?
Tb3 C6D 2.846(5) 4_676 ?
Tb3 C1E 2.858(5) . ?
O1A C1A 1.255(7) . ?
O2A C1A 1.271(7) . ?
O3A C6A 1.255(7) . ?
O3A Tb2 2.377(4) 3_777 ?
O4A C6A 1.255(7) . ?
O4A Tb3 2.282(4) 3_777 ?
C1A C2A 1.506(9) . ?
C2A C3A 1.473(9) . ?
C3A C4A 1.548(10) . ?
C4A C5A 1.449(9) . ?
C5A C6A 1.506(8) . ?
O1B C1B 1.249(6) . ?
O2B C1B 1.257(6) . ?
O3B C6B 1.278(7) . ?
O3B Tb1 2.340(4) 2_656 ?
O3B Tb2 2.607(4) 2_656 ?
O4B C6B 1.246(7) . ?
O4B Tb2 2.445(4) 2_656 ?
C1B C2B 1.503(8) . ?
C2B C3B 1.520(9) . ?
C3B C4B 1.525(10) . ?
C4B C5B 1.508(10) . ?
C5B C6B 1.487(8) . ?
C6B Tb2 2.912(6) 2_656 ?
O1C C1C 1.232(6) . ?
O2C C1C 1.287(7) . ?
C1C C2C 1.501(8) . ?
C2C C3C 1.512(8) . ?
C3C C3C 1.525(13) 3_767 ?
O1D C1D 1.285(6) . ?
O2D C1D 1.235(6) . ?
O3D C6D 1.244(7) . ?
O3D Tb3 2.499(4) 4_575 ?
O4D C6D 1.275(7) . ?
O4D Tb1 2.417(4) 1_455 ?
O4D Tb3 2.452(4) 4_575 ?
C1D C2D 1.509(7) . ?
C2D C3D 1.498(9) . ?
C3D C4D 1.534(8) . ?
C4D C5D 1.494(9) . ?
C5D C6D 1.514(8) . ?
C6D Tb3 2.846(5) 4_575 ?
O1E C1E 1.256(6) . ?
O2E C1E 1.271(6) . ?
O2E Tb1 2.376(4) 4_576 ?
C1E C2E 1.494(8) . ?
C2E C3E 1.525(8) . ?
C3E C3E 1.524(12) 3_667 ?
O1F C1F 1.238(7) . ?
O2F C1F 1.254(7) . ?
O2F Tb1 2.290(4) 4_576 ?
C1F C2F 1.508(9) . ?
C2F C3F 1.472(11) . ?
C3F C3F 1.682(19) 3_677 ?
O1G C1G 1.142(13) . ?
O1G C11G 1.308(16) . ?
N1G C11G 1.210(17) . ?
N1G C1G 1.314(16) . ?
N1G C3G 1.31(2) . ?
N1G C21G 1.499(19) . ?
N1G C31G 1.536(19) . ?
N1G C2G 1.582(17) . ?
O1H C11H 1.062(16) . ?
O1H C1H 1.126(13) . ?
N1H C1H 1.335(14) . ?
N1H C3H 1.38(2) . ?
N1H C2H 1.500(17) . ?

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
O2F Tb1 O1B 100.72(16) 4_675 . ?
O2F Tb1 O3B 81.71(14) 4_675 2_646 ?
O1B Tb1 O3B 75.11(14) . 2_646 ?
O2F Tb1 O1G 90.21(19) 4_675 . ?
O1B Tb1 O1G 143.82(15) . . ?
O3B Tb1 O1G 72.50(15) 2_646 . ?
O2F Tb1 O2E 77.83(15) 4_675 4_675 ?
O1B Tb1 O2E 75.31(13) . 4_675 ?
O3B Tb1 O2E 139.88(14) 2_646 4_675 ?
O1G Tb1 O2E 140.87(15) . 4_675 ?
O2F Tb1 O4D 85.20(14) 4_675 1_655 ?
O1B Tb1 O4D 142.16(13) . 1_655 ?
O3B Tb1 O4D 142.46(14) 2_646 1_655 ?
O1G Tb1 O4D 72.52(15) . 1_655 ?
O2E Tb1 O4D 69.47(13) 4_675 1_655 ?
O2F Tb1 O1A 155.12(14) 4_675 . ?
O1B Tb1 O1A 83.21(15) . . ?
O3B Tb1 O1A 122.74(13) 2_646 . ?
O1G Tb1 O1A 101.07(17) . . ?
O2E Tb1 O1A 79.51(13) 4_675 . ?
O4D Tb1 O1A 77.33(13) 1_655 . ?
O2F Tb1 O2A 152.40(14) 4_675 . ?
O1B Tb1 O2A 75.98(13) . . ?
O3B Tb1 O2A 70.90(13) 2_646 . ?
O1G Tb1 O2A 78.55(16) . . ?
O2E Tb1 O2A 126.05(13) 4_675 . ?
O4D Tb1 O2A 114.49(12) 1_655 . ?
O1A Tb1 O2A 52.46(13) . . ?
O2F Tb1 C1A 175.66(17) 4_675 . ?
O1B Tb1 C1A 74.96(16) . . ?
O3B Tb1 C1A 96.55(16) 2_646 . ?
O1G Tb1 C1A 93.06(19) . . ?
O2E Tb1 C1A 101.28(16) 4_675 . ?
O4D Tb1 C1A 98.50(15) 1_655 . ?
O1A Tb1 C1A 26.20(14) . . ?
O2A Tb1 C1A 26.69(14) . . ?
O2B Tb2 O3A 79.78(15) . 3_777 ?
O2B Tb2 O1H 138.92(16) . . ?
O3A Tb2 O1H 74.39(18) 3_777 . ?
O2B Tb2 O1D 77.73(12) . . ?
O3A Tb2 O1D 72.91(13) 3_777 . ?
O1H Tb2 O1D 122.53(17) . . ?
O2B Tb2 O2A 75.07(13) . . ?
O3A Tb2 O2A 84.84(14) 3_777 . ?
O1H Tb2 O2A 71.33(16) . . ?
O1D Tb2 O2A 147.42(13) . . ?
O2B Tb2 O4B 79.80(15) . 2_646 ?
O3A Tb2 O4B 143.34(14) 3_777 2_646 ?
O1H Tb2 O4B 137.54(17) . 2_646 ?
O1D Tb2 O4B 73.19(13) . 2_646 ?
O2A Tb2 O4B 118.43(12) . 2_646 ?
O2B Tb2 O2C 141.97(13) . . ?
O3A Tb2 O2C 102.58(14) 3_777 . ?
O1H Tb2 O2C 75.68(15) . . ?
O1D Tb2 O2C 67.21(12) . . ?
O2A Tb2 O2C 142.77(13) . . ?
O4B Tb2 O2C 76.47(13) 2_646 . ?
O2B Tb2 O3B 73.70(13) . 2_646 ?
O3A Tb2 O3B 145.97(13) 3_777 2_646 ?
O1H Tb2 O3B 113.33(18) . 2_646 ?
O1D Tb2 O3B 120.31(12) . 2_646 ?
O2A Tb2 O3B 68.13(12) . 2_646 ?
O4B Tb2 O3B 51.00(12) 2_646 2_646 ?
O2C Tb2 O3B 111.45(13) . 2_646 ?
O2B Tb2 O1C 141.83(14) . . ?
O3A Tb2 O1C 138.20(15) 3_777 . ?
O1H Tb2 O1C 68.39(17) . . ?
O1D Tb2 O1C 112.23(13) . . ?
O2A Tb2 O1C 100.25(13) . . ?
O4B Tb2 O1C 69.19(14) 2_646 . ?
O2C Tb2 O1C 50.59(12) . . ?
O3B Tb2 O1C 69.63(13) 2_646 . ?
O2B Tb2 C6B 74.98(15) . 2_646 ?
O3A Tb2 C6B 154.18(15) 3_777 2_646 ?
O1H Tb2 C6B 129.51(19) . 2_646 ?
O1D Tb2 C6B 96.23(15) . 2_646 ?
O2A Tb2 C6B 93.73(14) . 2_646 ?
O4B Tb2 C6B 24.99(14) 2_646 2_646 ?
O2C Tb2 C6B 94.11(14) . 2_646 ?
O3B Tb2 C6B 26.02(14) 2_646 2_646 ?
O1C Tb2 C6B 67.47(15) . 2_646 ?
O2B Tb2 C1C 148.27(16) . . ?
O3A Tb2 C1C 124.03(16) 3_777 . ?
O1H Tb2 C1C 72.23(17) . . ?
O1D Tb2 C1C 89.13(14) . . ?
O2A Tb2 C1C 123.32(14) . . ?
O4B Tb2 C1C 68.72(15) 2_646 . ?
O2C Tb2 C1C 25.83(13) . . ?
O3B Tb2 C1C 88.96(14) 2_646 . ?
O1C Tb2 C1C 24.93(13) . . ?
C6B Tb2 C1C 77.97(16) 2_646 . ?
O2B Tb2 Tb3 115.64(9) . . ?
O3A Tb2 Tb3 74.40(10) 3_777 . ?
O1H Tb2 Tb3 87.52(14) . . ?
O1D Tb2 Tb3 38.60(8) . . ?
O2A Tb2 Tb3 153.79(9) . . ?
O4B Tb2 Tb3 87.59(9) 2_646 . ?
O2C Tb2 Tb3 34.89(9) . . ?
O3B Tb2 Tb3 136.69(8) 2_646 . ?
O1C Tb2 Tb3 85.47(8) . . ?
C6B Tb2 Tb3 111.93(11) 2_646 . ?
C1C Tb2 Tb3 60.65(11) . . ?
O4A Tb3 O1F 81.56(15) 3_777 . ?
O4A Tb3 O2C 79.47(14) 3_777 . ?
O1F Tb3 O2C 143.12(14) . . ?
O4A Tb3 O1E 148.35(14) 3_777 . ?
O1F Tb3 O1E 127.79(14) . . ?
O2C Tb3 O1E 80.58(13) . . ?
O4A Tb3 O2D 123.86(14) 3_777 . ?
O1F Tb3 O2D 78.27(16) . . ?
O2C Tb3 O2D 86.53(14) . . ?
O1E Tb3 O2D 78.90(14) . . ?
O4A Tb3 O4D 89.82(14) 3_777 4_676 ?
O1F Tb3 O4D 78.46(14) . 4_676 ?
O2C Tb3 O4D 132.47(12) . 4_676 ?
O1E Tb3 O4D 85.79(13) . 4_676 ?
O2D Tb3 O4D 134.94(13) . 4_676 ?
O4A Tb3 O3D 75.36(15) 3_777 4_676 ?
O1F Tb3 O3D 124.73(15) . 4_676 ?
O2C Tb3 O3D 80.13(13) . 4_676 ?
O1E Tb3 O3D 77.21(14) . 4_676 ?
O2D Tb3 O3D 154.20(16) . 4_676 ?
O4D Tb3 O3D 52.42(12) 4_676 4_676 ?
O4A Tb3 O1D 72.26(13) 3_777 . ?
O1F Tb3 O1D 77.27(13) . . ?
O2C Tb3 O1D 66.94(12) . . ?
O1E Tb3 O1D 120.98(13) . . ?
O2D Tb3 O1D 52.40(12) . . ?
O4D Tb3 O1D 151.61(13) 4_676 . ?
O3D Tb3 O1D 137.06(12) 4_676 . ?
O4A Tb3 O2E 149.58(13) 3_777 . ?
O1F Tb3 O2E 76.53(13) . . ?
O2C Tb3 O2E 130.08(13) . . ?
O1E Tb3 O2E 51.82(12) . . ?
O2D Tb3 O2E 71.91(12) . . ?
O4D Tb3 O2E 65.41(12) 4_676 . ?
O3D Tb3 O2E 100.19(13) 4_676 . ?
O1D Tb3 O2E 121.89(12) . . ?
O4A Tb3 C1D 98.56(15) 3_777 . ?
O1F Tb3 C1D 75.51(16) . . ?
O2C Tb3 C1D 76.42(14) . . ?
O1E Tb3 C1D 100.32(15) . . ?
O2D Tb3 C1D 25.59(14) . . ?
O4D Tb3 C1D 151.08(14) 4_676 . ?
O3D Tb3 C1D 156.49(14) 4_676 . ?
O1D Tb3 C1D 26.84(13) . . ?
O2E Tb3 C1D 96.13(14) . . ?
O4A Tb3 C6D 81.60(15) 3_777 4_676 ?
O1F Tb3 C6D 102.13(17) . 4_676 ?
O2C Tb3 C6D 105.98(15) . 4_676 ?
O1E Tb3 C6D 80.59(15) . 4_676 ?
O2D Tb3 C6D 153.81(14) . 4_676 ?
O4D Tb3 C6D 26.54(14) 4_676 4_676 ?
O3D Tb3 C6D 25.88(14) 4_676 4_676 ?
O1D Tb3 C6D 153.70(14) . 4_676 ?
O2E Tb3 C6D 82.65(14) . 4_676 ?
C1D Tb3 C6D 177.57(16) . 4_676 ?
O4A Tb3 C1E 165.33(14) 3_777 . ?
O1F Tb3 C1E 102.04(16) . . ?
O2C Tb3 C1E 104.29(15) . . ?
O1E Tb3 C1E 25.77(14) . . ?
O2D Tb3 C1E 70.76(14) . . ?
O4D Tb3 C1E 77.15(14) 4_676 . ?
O3D Tb3 C1E 91.18(15) 4_676 . ?
O1D Tb3 C1E 122.35(13) . . ?
O2E Tb3 C1E 26.39(13) . . ?
C1D Tb3 C1E 96.10(15) . . ?
C6D Tb3 C1E 83.74(15) 4_676 . ?
C1A O1A Tb1 95.2(3) . . ?
C1A O2A Tb2 147.5(4) . . ?
C1A O2A Tb1 90.9(3) . . ?
Tb2 O2A Tb1 110.51(15) . . ?
C6A O3A Tb2 119.1(4) . 3_777 ?
C6A O4A Tb3 140.9(4) . 3_777 ?
O1A C1A O2A 119.5(5) . . ?
O1A C1A C2A 118.9(6) . . ?
O2A C1A C2A 121.4(5) . . ?
O1A C1A Tb1 58.6(3) . . ?
O2A C1A Tb1 62.4(3) . . ?
C2A C1A Tb1 163.1(5) . . ?
C3A C2A C1A 114.3(6) . . ?
C2A C3A C4A 110.0(6) . . ?
C5A C4A C3A 114.2(6) . . ?
C4A C5A C6A 114.6(6) . . ?
O4A C6A O3A 124.3(6) . . ?
O4A C6A C5A 117.8(5) . . ?
O3A C6A C5A 117.9(6) . . ?
C1B O1B Tb1 140.1(4) . . ?
C1B O2B Tb2 140.4(4) . . ?
C6B O3B Tb1 152.9(4) . 2_656 ?
C6B O3B Tb2 90.5(3) . 2_656 ?
Tb1 O3B Tb2 109.47(15) 2_656 2_656 ?
C6B O4B Tb2 99.0(3) . 2_656 ?
O1B C1B O2B 125.1(5) . . ?
O1B C1B C2B 117.4(5) . . ?
O2B C1B C2B 117.5(5) . . ?
C1B C2B C3B 115.7(6) . . ?
C2B C3B C4B 112.1(6) . . ?
C5B C4B C3B 113.3(6) . . ?
C6B C5B C4B 112.8(6) . . ?
O4B C6B O3B 119.5(5) . . ?
O4B C6B C5B 120.2(5) . . ?
O3B C6B C5B 120.3(5) . . ?
O4B C6B Tb2 56.0(3) . 2_656 ?
O3B C6B Tb2 63.5(3) . 2_656 ?
C5B C6B Tb2 175.7(5) . 2_656 ?
C1C O1C Tb2 90.3(3) . . ?
C1C O2C Tb3 152.7(4) . . ?
C1C O2C Tb2 98.2(3) . . ?
Tb3 O2C Tb2 108.59(15) . . ?
O1C C1C O2C 120.0(5) . . ?
O1C C1C C2C 122.6(5) . . ?
O2C C1C C2C 117.4(5) . . ?
O1C C1C Tb2 64.7(3) . . ?
O2C C1C Tb2 55.9(3) . . ?
C2C C1C Tb2 167.3(4) . . ?
C1C C2C C3C 114.9(5) . . ?
C2C C3C C3C 113.2(7) . 3_767 ?
C1D O1D Tb2 131.0(3) . . ?
C1D O1D Tb3 91.1(3) . . ?
Tb2 O1D Tb3 104.71(13) . . ?
C1D O2D Tb3 95.7(3) . . ?
C6D O3D Tb3 92.8(3) . 4_575 ?
C6D O4D Tb1 137.8(4) . 1_455 ?
C6D O4D Tb3 94.2(3) . 4_575 ?
Tb1 O4D Tb3 111.33(14) 1_455 4_575 ?
O2D C1D O1D 120.6(5) . . ?
O2D C1D C2D 120.5(5) . . ?
O1D C1D C2D 118.8(5) . . ?
O2D C1D Tb3 58.7(3) . . ?
O1D C1D Tb3 62.0(3) . . ?
C2D C1D Tb3 174.5(4) . . ?
C3D C2D C1D 114.2(5) . . ?
C2D C3D C4D 113.3(6) . . ?
C5D C4D C3D 113.1(6) . . ?
C4D C5D C6D 111.7(5) . . ?
O3D C6D O4D 120.5(5) . . ?
O3D C6D C5D 121.1(5) . . ?
O4D C6D C5D 118.4(5) . . ?
O3D C6D Tb3 61.3(3) . 4_575 ?
O4D C6D Tb3 59.2(3) . 4_575 ?
C5D C6D Tb3 177.1(5) . 4_575 ?
C1E O1E Tb3 98.4(3) . . ?
C1E O2E Tb1 128.9(3) . 4_576 ?
C1E O2E Tb3 88.3(3) . . ?
Tb1 O2E Tb3 107.81(14) 4_576 . ?
O1E C1E O2E 119.9(5) . . ?
O1E C1E C2E 119.2(5) . . ?
O2E C1E C2E 120.8(5) . . ?
O1E C1E Tb3 55.8(3) . . ?
O2E C1E Tb3 65.3(3) . . ?
C2E C1E Tb3 165.3(4) . . ?
C1E C2E C3E 113.7(5) . . ?
C3E C3E C2E 111.6(7) 3_667 . ?
C1F O1F Tb3 140.3(4) . . ?
C1F O2F Tb1 136.7(4) . 4_576 ?
O1F C1F O2F 124.8(6) . . ?
O1F C1F C2F 117.7(6) . . ?
O2F C1F C2F 117.5(6) . . ?
C3F C2F C1F 116.6(7) . . ?
C2F C3F C3F 101.3(9) . 3_677 ?
C1G O1G Tb1 161.2(8) . . ?
C11G O1G Tb1 125.0(9) . . ?
C1G N1G C3G 135.8(16) . . ?
C11G N1G C21G 125.5(15) . . ?
C11G N1G C31G 121.9(13) . . ?
C21G N1G C31G 110.9(14) . . ?
C1G N1G C2G 110.5(12) . . ?
C3G N1G C2G 113.6(15) . . ?
O1G C1G N1G 132.6(17) . . ?
N1G C11G O1G 126.6(16) . . ?
C11H O1H Tb2 150.1(10) . . ?
C1H O1H Tb2 146.3(9) . . ?
C1H N1H C3H 123.4(11) . . ?
C1H N1H C2H 118.2(11) . . ?
C3H N1H C2H 118.0(12) . . ?
O1H C1H N1H 127.3(13) . . ?

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
Tb1 O1A C1A O2A 14.5(6) . . . . ?
Tb1 O1A C1A C2A -160.7(5) . . . . ?
Tb2 O2A C1A O1A -146.5(5) . . . . ?
Tb1 O2A C1A O1A -13.9(6) . . . . ?
Tb2 O2A C1A C2A 28.5(11) . . . . ?
Tb1 O2A C1A C2A 161.1(6) . . . . ?
Tb2 O2A C1A Tb1 -132.6(7) . . . . ?
O1A C1A C2A C3A -117.3(7) . . . . ?
O2A C1A C2A C3A 67.7(9) . . . . ?
Tb1 C1A C2A C3A 165.9(12) . . . . ?
C1A C2A C3A C4A 178.0(6) . . . . ?
C2A C3A C4A C5A 167.3(7) . . . . ?
C3A C4A C5A C6A 179.5(6) . . . . ?
Tb3 O4A C6A O3A 65.7(8) 3_777 . . . ?
Tb3 O4A C6A C5A -114.3(6) 3_777 . . . ?
Tb2 O3A C6A O4A -2.7(8) 3_777 . . . ?
Tb2 O3A C6A C5A 177.3(4) 3_777 . . . ?
C4A C5A C6A O4A -33.1(9) . . . . ?
C4A C5A C6A O3A 146.9(7) . . . . ?
Tb1 O1B C1B O2B -0.8(11) . . . . ?
Tb1 O1B C1B C2B 178.6(5) . . . . ?
Tb2 O2B C1B O1B -2.4(10) . . . . ?
Tb2 O2B C1B C2B 178.1(4) . . . . ?
O1B C1B C2B C3B -137.2(6) . . . . ?
O2B C1B C2B C3B 42.3(9) . . . . ?
C1B C2B C3B C4B 55.6(8) . . . . ?
C2B C3B C4B C5B 168.4(6) . . . . ?
C3B C4B C5B C6B -72.3(8) . . . . ?
Tb2 O4B C6B O3B 1.7(6) 2_656 . . . ?
Tb2 O4B C6B C5B -177.6(5) 2_656 . . . ?
Tb1 O3B C6B O4B -139.9(6) 2_656 . . . ?
Tb2 O3B C6B O4B -1.6(5) 2_656 . . . ?
Tb1 O3B C6B C5B 39.4(11) 2_656 . . . ?
Tb2 O3B C6B C5B 177.7(5) 2_656 . . . ?
Tb1 O3B C6B Tb2 -138.3(8) 2_656 . . 2_656 ?
C4B C5B C6B O4B -53.4(8) . . . . ?
C4B C5B C6B O3B 127.3(6) . . . . ?
Tb2 O1C C1C O2C -9.0(6) . . . . ?
Tb2 O1C C1C C2C 168.0(5) . . . . ?
Tb3 O2C C1C O1C 178.5(5) . . . . ?
Tb2 O2C C1C O1C 9.8(6) . . . . ?
Tb3 O2C C1C C2C 1.4(11) . . . . ?
Tb2 O2C C1C C2C -167.4(5) . . . . ?
Tb3 O2C C1C Tb2 168.7(8) . . . . ?
O1C C1C C2C C3C 30.5(9) . . . . ?
O2C C1C C2C C3C -152.4(6) . . . . ?
Tb2 C1C C2C C3C 152.3(16) . . . . ?
C1C C2C C3C C3C 71.8(9) . . . 3_767 ?
Tb3 O2D C1D O1D 3.5(6) . . . . ?
Tb3 O2D C1D C2D -173.6(5) . . . . ?
Tb2 O1D C1D O2D 107.3(6) . . . . ?
Tb3 O1D C1D O2D -3.4(6) . . . . ?
Tb2 O1D C1D C2D -75.5(6) . . . . ?
Tb3 O1D C1D C2D 173.8(5) . . . . ?
Tb2 O1D C1D Tb3 110.7(4) . . . . ?
O2D C1D C2D C3D -33.4(8) . . . . ?
O1D C1D C2D C3D 149.4(6) . . . . ?
C1D C2D C3D C4D -169.5(5) . . . . ?
C2D C3D C4D C5D -57.8(8) . . . . ?
C3D C4D C5D C6D -176.5(6) . . . . ?
Tb3 O3D C6D O4D -0.4(6) 4_575 . . . ?
Tb3 O3D C6D C5D 178.0(5) 4_575 . . . ?
Tb1 O4D C6D O3D -128.2(5) 1_455 . . . ?
Tb3 O4D C6D O3D 0.4(6) 4_575 . . . ?
Tb1 O4D C6D C5D 53.3(8) 1_455 . . . ?
Tb3 O4D C6D C5D -178.0(5) 4_575 . . . ?
Tb1 O4D C6D Tb3 -128.7(5) 1_455 . . 4_575 ?
C4D C5D C6D O3D -83.3(8) . . . . ?
C4D C5D C6D O4D 95.2(7) . . . . ?
Tb3 O1E C1E O2E -13.2(5) . . . . ?
Tb3 O1E C1E C2E 163.8(4) . . . . ?
Tb1 O2E C1E O1E -99.6(5) 4_576 . . . ?
Tb3 O2E C1E O1E 12.0(5) . . . . ?
Tb1 O2E C1E C2E 83.4(6) 4_576 . . . ?
Tb3 O2E C1E C2E -164.9(5) . . . . ?
Tb1 O2E C1E Tb3 -111.7(3) 4_576 . . . ?
O1E C1E C2E C3E -31.2(8) . . . . ?
O2E C1E C2E C3E 145.8(5) . . . . ?
Tb3 C1E C2E C3E 35(2) . . . . ?
C1E C2E C3E C3E -65.0(9) . . . 3_667 ?
Tb3 O1F C1F O2F 33.4(12) . . . . ?
Tb3 O1F C1F C2F -146.6(6) . . . . ?
Tb1 O2F C1F O1F -16.0(12) 4_576 . . . ?
Tb1 O2F C1F C2F 163.9(6) 4_576 . . . ?
O1F C1F C2F C3F -25.8(12) . . . . ?
O2F C1F C2F C3F 154.3(8) . . . . ?
C1F C2F C3F C3F -75.7(11) . . . 3_677 ?
C11G O1G C1G N1G 23.0(14) . . . . ?
Tb1 O1G C1G N1G 96(3) . . . . ?
C11G N1G C1G O1G -25.5(15) . . . . ?
C3G N1G C1G O1G -178(2) . . . . ?
C21G N1G C1G O1G -96(5) . . . . ?
C31G N1G C1G O1G 151(2) . . . . ?
C2G N1G C1G O1G -2(2) . . . . ?
C1G N1G C11G O1G 20.1(11) . . . . ?
C3G N1G C11G O1G 126(5) . . . . ?
C21G N1G C11G O1G 179.0(16) . . . . ?
C31G N1G C11G O1G 16(2) . . . . ?
C2G N1G C11G O1G -136.3(18) . . . . ?
C1G O1G C11G N1G -22.9(13) . . . . ?
Tb1 O1G C11G N1G 179.3(10) . . . . ?
C11H O1H C1H N1H -14.0(13) . . . . ?
Tb2 O1H C1H N1H -159.3(7) . . . . ?
C3H N1H C1H O1H 3(2) . . . . ?
C2H N1H C1H O1H 175.3(15) . . . . ?
C2C C3C C3C C2C 180.000(3) . . 3_767 3_767 ?
C2E C3E C3E C2E 180.000(4) . . 3_667 3_667 ?
C2F C3F C3F C2F 180.000(3) . . 3_677 3_677 ?

_refine_diff_density_max         1.634
_refine_diff_density_min         -2.285
_refine_diff_density_rms         0.171

_database_code_depnum_ccdc_archive 'CCDC 922452'