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

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#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  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.
#
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#  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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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
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data_complex_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H35 N6 O13 Tb'
_chemical_formula_weight         846.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pna21

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

_cell_length_a                   15.0914(2)
_cell_length_b                   16.7363(3)
_cell_length_c                   13.0708(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3301.35(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3448
_cell_measurement_theta_min      3.94
_cell_measurement_theta_max      62.53

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1704
_exptl_absorpt_coefficient_mu    11.197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8071
_exptl_absorpt_correction_T_max  0.8963
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  Germini
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         2
_diffrn_standards_interval_count 150
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            5838
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.94
_diffrn_reflns_theta_max         62.53
_reflns_number_total             3448
_reflns_number_gt                2936
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0306P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_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   -0.007(5)
_refine_ls_number_reflns         3448
_refine_ls_number_parameters     447
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0297
_refine_ls_wR_factor_ref         0.0666
_refine_ls_wR_factor_gt          0.0655
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.051
_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
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb -0.008413(17) 1.173004(17) 1.26756(4) 0.01925(10) Uani 1 1 d . . .
O1 O 0.0511(3) 1.1020(3) 1.1386(4) 0.0361(13) Uani 1 1 d . . .
O2 O 0.5309(3) 1.5460(2) 0.8307(4) 0.0248(10) Uani 1 1 d . . .
O3 O 0.8644(3) 0.8325(3) 0.8250(4) 0.0280(10) Uani 1 1 d . . .
O4 O -0.1915(4) 1.1946(3) 1.0337(5) 0.0544(18) Uani 1 1 d . . .
O5 O -0.1375(3) 1.1254(3) 1.1590(4) 0.0373(13) Uani 1 1 d . . .
O6 O -0.1066(3) 1.2494(3) 1.1472(4) 0.0422(14) Uani 1 1 d . . .
O7 O 0.1023(4) 1.3981(3) 1.2400(4) 0.0561(17) Uani 1 1 d . . .
O8 O 0.0759(3) 1.2817(3) 1.1733(4) 0.0340(12) Uani 1 1 d . . .
O9 O 0.0137(3) 1.3128(3) 1.3177(4) 0.0356(12) Uani 1 1 d . . .
O10 O -0.1418(3) 1.1936(3) 1.5414(4) 0.0395(14) Uani 1 1 d . . .
O11 O -0.0185(3) 1.1870(3) 1.4591(4) 0.0287(11) Uani 1 1 d . . .
O12 O -0.1411(3) 1.1938(3) 1.3776(4) 0.0293(12) Uani 1 1 d . . .
N1 N 0.2543(3) 1.0502(3) 0.9472(4) 0.0203(12) Uani 1 1 d . . .
N2 N 0.5302(3) 1.3118(3) 0.7398(4) 0.0201(14) Uani 1 1 d . . .
N3 N 0.6896(3) 0.9952(3) 0.9408(4) 0.0165(11) Uani 1 1 d . . .
N4 N -0.1459(4) 1.1895(3) 1.1086(6) 0.0326(16) Uani 1 1 d . . .
N5 N 0.0650(4) 1.3327(3) 1.2422(4) 0.0321(16) Uani 1 1 d . . .
N6 N -0.1000(3) 1.1927(3) 1.4616(5) 0.0195(12) Uani 1 1 d . . .
C1 C 0.4021(3) 1.0740(3) 0.8603(5) 0.0156(10) Uani 1 1 d . . .
C2 C 0.4689(4) 1.0461(3) 0.9247(5) 0.0187(14) Uani 1 1 d . . .
C3 C 0.5549(4) 1.0802(4) 0.9182(5) 0.0172(13) Uani 1 1 d . . .
C4 C 0.5723(4) 1.1387(3) 0.8429(5) 0.0136(9) Uani 1 1 d . . .
C5 C 0.5045(3) 1.1664(3) 0.7829(6) 0.0136(9) Uani 1 1 d . . .
C6 C 0.4172(3) 1.1365(3) 0.7918(5) 0.0156(10) Uani 1 1 d . . .
C7 C 0.4494(4) 0.9831(4) 1.0043(5) 0.0269(17) Uani 1 1 d . . .
H7A H 0.5012 0.9470 1.0101 0.032 Uiso 1 1 calc R . .
H7B H 0.3983 0.9507 0.9813 0.032 Uiso 1 1 calc R . .
C8 C 0.4287(5) 1.0182(5) 1.1103(6) 0.0376(19) Uani 1 1 d . . .
H8A H 0.4153 0.9747 1.1582 0.056 Uiso 1 1 calc R . .
H8B H 0.3775 1.0539 1.1053 0.056 Uiso 1 1 calc R . .
H8C H 0.4801 1.0482 1.1351 0.056 Uiso 1 1 calc R . .
C9 C 0.6671(3) 1.1710(4) 0.8304(5) 0.0207(14) Uani 1 1 d . . .
H9A H 0.6980 1.1676 0.8970 0.025 Uiso 1 1 calc R . .
H9B H 0.6642 1.2280 0.8106 0.025 Uiso 1 1 calc R . .
C10 C 0.7216(3) 1.1248(4) 0.7490(5) 0.028(2) Uani 1 1 d . . .
H10A H 0.7812 1.1477 0.7444 0.042 Uiso 1 1 calc R . .
H10B H 0.6922 1.1290 0.6823 0.042 Uiso 1 1 calc R . .
H10C H 0.7258 1.0684 0.7687 0.042 Uiso 1 1 calc R . .
C11 C 0.3420(4) 1.1717(4) 0.7302(5) 0.0236(14) Uani 1 1 d . . .
H11A H 0.3544 1.2290 0.7177 0.028 Uiso 1 1 calc R . .
H11B H 0.2867 1.1682 0.7707 0.028 Uiso 1 1 calc R . .
C12 C 0.3278(5) 1.1299(4) 0.6274(6) 0.0321(17) Uani 1 1 d . . .
H12A H 0.2784 1.1553 0.5911 0.048 Uiso 1 1 calc R . .
H12B H 0.3141 1.0734 0.6391 0.048 Uiso 1 1 calc R . .
H12C H 0.3818 1.1343 0.5860 0.048 Uiso 1 1 calc R . .
C13 C 0.3122(3) 1.0325(4) 0.8601(6) 0.0240(15) Uani 1 1 d . . .
H13A H 0.2807 1.0474 0.7965 0.029 Uiso 1 1 calc R . .
H13B H 0.3223 0.9741 0.8579 0.029 Uiso 1 1 calc R . .
C14 C 0.2452(4) 1.1252(4) 0.9825(5) 0.0260(16) Uani 1 1 d . . .
H14A H 0.2846 1.1656 0.9592 0.031 Uiso 1 1 calc R . .
C15 C 0.1798(4) 1.1449(4) 1.0520(6) 0.0281(16) Uani 1 1 d . . .
H15A H 0.1756 1.1980 1.0773 0.034 Uiso 1 1 calc R . .
C16 C 0.1189(4) 1.0862(4) 1.0857(6) 0.0270(16) Uani 1 1 d . . .
C17 C 0.1363(4) 1.0070(4) 1.0519(6) 0.0284(17) Uani 1 1 d . . .
H17A H 0.1011 0.9642 1.0770 0.034 Uiso 1 1 calc R . .
C18 C 0.2011(4) 0.9919(4) 0.9858(6) 0.0272(17) Uani 1 1 d . . .
H18A H 0.2106 0.9383 0.9646 0.033 Uiso 1 1 calc R . .
C19 C 0.5237(4) 1.2286(3) 0.7005(5) 0.0177(13) Uani 1 1 d . . .
H19A H 0.5800 1.2145 0.6662 0.021 Uiso 1 1 calc R . .
H19B H 0.4761 1.2263 0.6485 0.021 Uiso 1 1 calc R . .
C20 C 0.4959(4) 1.3340(3) 0.8303(6) 0.0209(15) Uani 1 1 d . . .
H20A H 0.4698 1.2940 0.8723 0.025 Uiso 1 1 calc R . .
C21 C 0.4965(4) 1.4106(3) 0.8651(5) 0.0250(14) Uani 1 1 d . . .
H21A H 0.4732 1.4228 0.9307 0.030 Uiso 1 1 calc R . .
C22 C 0.5325(4) 1.4728(4) 0.8024(5) 0.0216(16) Uani 1 1 d . . .
C23 C 0.5691(4) 1.4462(4) 0.7080(5) 0.0249(16) Uani 1 1 d . . .
H23A H 0.5956 1.4841 0.6633 0.030 Uiso 1 1 calc R . .
C24 C 0.5672(4) 1.3678(4) 0.6802(5) 0.0239(15) Uani 1 1 d . . .
H24A H 0.5928 1.3523 0.6168 0.029 Uiso 1 1 calc R . .
C25 C 0.6263(4) 1.0534(4) 0.9890(5) 0.0192(14) Uani 1 1 d . . .
H25A H 0.5988 1.0280 1.0497 0.023 Uiso 1 1 calc R . .
H25B H 0.6598 1.1007 1.0129 0.023 Uiso 1 1 calc R . .
C26 C 0.7774(4) 0.9991(4) 0.9655(5) 0.0198(14) Uani 1 1 d . . .
H26A H 0.7973 1.0406 1.0094 0.024 Uiso 1 1 calc R . .
C27 C 0.8367(4) 0.9455(4) 0.9294(5) 0.0201(14) Uani 1 1 d . . .
H27A H 0.8971 0.9493 0.9496 0.024 Uiso 1 1 calc R . .
C28 C 0.8101(4) 0.8839(4) 0.8620(5) 0.0228(15) Uani 1 1 d . . .
C29 C 0.7185(4) 0.8817(4) 0.8371(5) 0.0209(14) Uani 1 1 d . . .
H29A H 0.6968 0.8413 0.7925 0.025 Uiso 1 1 calc R . .
C30 C 0.6611(4) 0.9368(4) 0.8766(5) 0.0197(14) Uani 1 1 d . . .
H30A H 0.6001 0.9343 0.8587 0.024 Uiso 1 1 calc R . .
O1W O 0.1658(4) 1.2860(4) 1.5066(5) 0.0543(17) Uani 1 1 d D . .
H1W H 0.2224(19) 1.301(4) 1.484(4) 0.018(17) Uiso 1 1 d D . .
H2W H 0.130(4) 1.281(6) 1.447(4) 0.09(4) Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O1 2.250(5) . ?
Tb1 O3 2.302(4) 2_675 ?
Tb1 O2 2.306(4) 3_545 ?
Tb1 O9 2.452(5) . ?
Tb1 O12 2.490(5) . ?
Tb1 O6 2.511(5) . ?
Tb1 O11 2.519(5) . ?
Tb1 O5 2.538(5) . ?
Tb1 O8 2.539(5) . ?
Tb1 N6 2.907(6) . ?
Tb1 N5 2.912(6) . ?
Tb1 N4 2.950(6) . ?
O1 C16 1.263(8) . ?
O2 C22 1.280(7) . ?
O2 Tb1 2.306(4) 3_554 ?
O3 C28 1.283(7) . ?
O3 Tb1 2.302(4) 2_674 ?
O4 N4 1.199(8) . ?
O5 N4 1.266(8) . ?
O6 N4 1.269(7) . ?
O7 N5 1.232(7) . ?
O8 N5 1.251(7) . ?
O9 N5 1.299(7) . ?
O10 N6 1.219(7) . ?
O11 N6 1.235(7) . ?
O12 N6 1.261(7) . ?
N1 C14 1.345(8) . ?
N1 C18 1.360(8) . ?
N1 C13 1.466(8) . ?
N2 C24 1.340(8) . ?
N2 C20 1.344(8) . ?
N2 C19 1.487(7) . ?
N3 C30 1.357(8) . ?
N3 C26 1.366(8) . ?
N3 C25 1.503(8) . ?
C1 C2 1.395(9) . ?
C1 C6 1.395(9) . ?
C1 C13 1.524(8) . ?
C2 C3 1.420(8) . ?
C2 C7 1.511(9) . ?
C3 C4 1.414(9) . ?
C3 C25 1.489(9) . ?
C4 C5 1.370(9) . ?
C4 C9 1.538(8) . ?
C5 C6 1.414(7) . ?
C5 C19 1.525(9) . ?
C6 C11 1.512(8) . ?
C7 C8 1.537(10) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.551(9) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.530(10) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.381(10) . ?
C14 H14A 0.9500 . ?
C15 C16 1.416(9) . ?
C15 H15A 0.9500 . ?
C16 C17 1.422(9) . ?
C17 C18 1.329(9) . ?
C17 H17A 0.9500 . ?
C18 H18A 0.9500 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.360(8) . ?
C20 H20A 0.9500 . ?
C21 C22 1.431(9) . ?
C21 H21A 0.9500 . ?
C22 C23 1.424(9) . ?
C23 C24 1.363(9) . ?
C23 H23A 0.9500 . ?
C24 H24A 0.9500 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.352(9) . ?
C26 H26A 0.9500 . ?
C27 C28 1.414(9) . ?
C27 H27A 0.9500 . ?
C28 C29 1.421(9) . ?
C29 C30 1.367(9) . ?
C29 H29A 0.9500 . ?
C30 H30A 0.9500 . ?
O1W H1W 0.94(2) . ?
O1W H2W 0.96(2) . ?

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 Tb1 O3 81.15(18) . 2_675 ?
O1 Tb1 O2 80.78(17) . 3_545 ?
O3 Tb1 O2 89.15(15) 2_675 3_545 ?
O1 Tb1 O9 130.57(17) . . ?
O3 Tb1 O9 79.78(16) 2_675 . ?
O2 Tb1 O9 143.49(18) 3_545 . ?
O1 Tb1 O12 145.86(16) . . ?
O3 Tb1 O12 125.21(18) 2_675 . ?
O2 Tb1 O12 78.66(16) 3_545 . ?
O9 Tb1 O12 79.73(16) . . ?
O1 Tb1 O6 92.0(2) . . ?
O3 Tb1 O6 141.46(16) 2_675 . ?
O2 Tb1 O6 127.37(16) 3_545 . ?
O9 Tb1 O6 76.23(17) . . ?
O12 Tb1 O6 79.41(18) . . ?
O1 Tb1 O11 144.86(18) . . ?
O3 Tb1 O11 74.72(16) 2_675 . ?
O2 Tb1 O11 73.78(16) 3_545 . ?
O9 Tb1 O11 69.75(16) . . ?
O12 Tb1 O11 50.52(16) . . ?
O6 Tb1 O11 122.66(17) . . ?
O1 Tb1 O5 73.84(18) . . ?
O3 Tb1 O5 153.45(17) 2_675 . ?
O2 Tb1 O5 78.32(16) 3_545 . ?
O9 Tb1 O5 123.60(16) . . ?
O12 Tb1 O5 75.49(17) . . ?
O6 Tb1 O5 49.98(16) . . ?
O11 Tb1 O5 122.56(17) . . ?
O1 Tb1 O8 79.34(17) . . ?
O3 Tb1 O8 73.36(16) 2_675 . ?
O2 Tb1 O8 155.24(15) 3_545 . ?
O9 Tb1 O8 51.56(17) . . ?
O12 Tb1 O8 125.70(16) . . ?
O6 Tb1 O8 68.10(17) . . ?
O11 Tb1 O8 116.49(16) . . ?
O5 Tb1 O8 109.79(17) . . ?
O1 Tb1 N6 154.60(16) . . ?
O3 Tb1 N6 99.73(17) 2_675 . ?
O2 Tb1 N6 73.86(15) 3_545 . ?
O9 Tb1 N6 73.93(16) . . ?
O12 Tb1 N6 25.54(15) . . ?
O6 Tb1 N6 102.01(17) . . ?
O11 Tb1 N6 25.01(15) . . ?
O5 Tb1 N6 99.10(17) . . ?
O8 Tb1 N6 125.49(15) . . ?
O1 Tb1 N5 104.34(17) . . ?
O3 Tb1 N5 73.42(15) 2_675 . ?
O2 Tb1 N5 160.56(15) 3_545 . ?
O9 Tb1 N5 26.28(15) . . ?
O12 Tb1 N5 104.12(16) . . ?
O6 Tb1 N5 71.69(15) . . ?
O11 Tb1 N5 92.93(15) . . ?
O5 Tb1 N5 121.10(15) . . ?
O8 Tb1 N5 25.37(16) . . ?
N6 Tb1 N5 100.16(15) . . ?
O1 Tb1 N4 78.61(19) . . ?
O3 Tb1 N4 153.89(19) 2_675 . ?
O2 Tb1 N4 103.60(16) 3_545 . ?
O9 Tb1 N4 101.23(16) . . ?
O12 Tb1 N4 80.12(19) . . ?
O6 Tb1 N4 25.29(16) . . ?
O11 Tb1 N4 130.47(17) . . ?
O5 Tb1 N4 25.28(16) . . ?
O8 Tb1 N4 86.77(17) . . ?
N6 Tb1 N4 105.6(2) . . ?
N5 Tb1 N4 95.82(16) . . ?
C16 O1 Tb1 147.6(4) . . ?
C22 O2 Tb1 141.4(4) . 3_554 ?
C28 O3 Tb1 138.8(4) . 2_674 ?
N4 O5 Tb1 95.9(4) . . ?
N4 O6 Tb1 97.0(4) . . ?
N5 O8 Tb1 94.2(4) . . ?
N5 O9 Tb1 97.0(4) . . ?
N6 O11 Tb1 95.4(4) . . ?
N6 O12 Tb1 96.1(3) . . ?
C14 N1 C18 118.8(6) . . ?
C14 N1 C13 121.1(5) . . ?
C18 N1 C13 119.7(5) . . ?
C24 N2 C20 118.6(6) . . ?
C24 N2 C19 118.8(6) . . ?
C20 N2 C19 122.5(5) . . ?
C30 N3 C26 119.2(5) . . ?
C30 N3 C25 121.6(5) . . ?
C26 N3 C25 119.1(5) . . ?
O4 N4 O5 122.9(6) . . ?
O4 N4 O6 122.4(6) . . ?
O5 N4 O6 114.5(6) . . ?
O4 N4 Tb1 170.1(6) . . ?
O5 N4 Tb1 58.9(3) . . ?
O6 N4 Tb1 57.7(3) . . ?
O7 N5 O8 122.0(6) . . ?
O7 N5 O9 121.2(6) . . ?
O8 N5 O9 116.8(5) . . ?
O7 N5 Tb1 173.0(5) . . ?
O8 N5 Tb1 60.4(3) . . ?
O9 N5 Tb1 56.7(3) . . ?
O10 N6 O11 122.6(6) . . ?
O10 N6 O12 119.4(5) . . ?
O11 N6 O12 117.9(5) . . ?
O10 N6 Tb1 173.7(4) . . ?
O11 N6 Tb1 59.6(3) . . ?
O12 N6 Tb1 58.4(3) . . ?
C2 C1 C6 121.3(5) . . ?
C2 C1 C13 119.5(5) . . ?
C6 C1 C13 119.1(6) . . ?
C1 C2 C3 119.3(6) . . ?
C1 C2 C7 120.6(5) . . ?
C3 C2 C7 120.0(6) . . ?
C4 C3 C2 119.3(6) . . ?
C4 C3 C25 120.5(5) . . ?
C2 C3 C25 120.1(6) . . ?
C5 C4 C3 119.6(5) . . ?
C5 C4 C9 121.1(5) . . ?
C3 C4 C9 119.3(5) . . ?
C4 C5 C6 122.0(6) . . ?
C4 C5 C19 119.5(5) . . ?
C6 C5 C19 118.5(5) . . ?
C1 C6 C5 118.1(5) . . ?
C1 C6 C11 120.8(5) . . ?
C5 C6 C11 121.1(5) . . ?
C2 C7 C8 113.2(5) . . ?
C2 C7 H7A 108.9 . . ?
C8 C7 H7A 108.9 . . ?
C2 C7 H7B 108.9 . . ?
C8 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 C10 113.0(5) . . ?
C4 C9 H9A 109.0 . . ?
C10 C9 H9A 109.0 . . ?
C4 C9 H9B 109.0 . . ?
C10 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C6 C11 C12 113.3(5) . . ?
C6 C11 H11A 108.9 . . ?
C12 C11 H11A 108.9 . . ?
C6 C11 H11B 108.9 . . ?
C12 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N1 C13 C1 115.9(5) . . ?
N1 C13 H13A 108.3 . . ?
C1 C13 H13A 108.3 . . ?
N1 C13 H13B 108.3 . . ?
C1 C13 H13B 108.3 . . ?
H13A C13 H13B 107.4 . . ?
N1 C14 C15 121.4(6) . . ?
N1 C14 H14A 119.3 . . ?
C15 C14 H14A 119.3 . . ?
C14 C15 C16 120.2(6) . . ?
C14 C15 H15A 119.9 . . ?
C16 C15 H15A 119.9 . . ?
O1 C16 C15 123.4(6) . . ?
O1 C16 C17 121.0(6) . . ?
C15 C16 C17 115.6(6) . . ?
C18 C17 C16 120.9(6) . . ?
C18 C17 H17A 119.5 . . ?
C16 C17 H17A 119.5 . . ?
C17 C18 N1 122.7(6) . . ?
C17 C18 H18A 118.7 . . ?
N1 C18 H18A 118.7 . . ?
N2 C19 C5 114.1(5) . . ?
N2 C19 H19A 108.7 . . ?
C5 C19 H19A 108.7 . . ?
N2 C19 H19B 108.7 . . ?
C5 C19 H19B 108.7 . . ?
H19A C19 H19B 107.6 . . ?
N2 C20 C21 123.5(6) . . ?
N2 C20 H20A 118.2 . . ?
C21 C20 H20A 118.2 . . ?
C20 C21 C22 119.8(6) . . ?
C20 C21 H21A 120.1 . . ?
C22 C21 H21A 120.1 . . ?
O2 C22 C23 123.8(6) . . ?
O2 C22 C21 121.6(6) . . ?
C23 C22 C21 114.6(6) . . ?
C24 C23 C22 121.5(6) . . ?
C24 C23 H23A 119.2 . . ?
C22 C23 H23A 119.2 . . ?
N2 C24 C23 121.9(6) . . ?
N2 C24 H24A 119.1 . . ?
C23 C24 H24A 119.1 . . ?
C3 C25 N3 113.2(5) . . ?
C3 C25 H25A 108.9 . . ?
N3 C25 H25A 108.9 . . ?
C3 C25 H25B 108.9 . . ?
N3 C25 H25B 108.9 . . ?
H25A C25 H25B 107.8 . . ?
C27 C26 N3 121.9(6) . . ?
C27 C26 H26A 119.0 . . ?
N3 C26 H26A 119.0 . . ?
C26 C27 C28 120.8(6) . . ?
C26 C27 H27A 119.6 . . ?
C28 C27 H27A 119.6 . . ?
O3 C28 C27 122.8(5) . . ?
O3 C28 C29 121.1(6) . . ?
C27 C28 C29 116.0(6) . . ?
C30 C29 C28 120.8(6) . . ?
C30 C29 H29A 119.6 . . ?
C28 C29 H29A 119.6 . . ?
N3 C30 C29 121.2(5) . . ?
N3 C30 H30A 119.4 . . ?
C29 C30 H30A 119.4 . . ?
H1W O1W H2W 106(3) . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        62.53
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.079
_database_code_depnum_ccdc_archive 'CCDC 979152'
#######################################################################
#
#                 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_complex_4


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H35 Ce N6 O13'
_chemical_formula_weight         827.76

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -1.8482 9.6596 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   15.1122(2)
_cell_length_b                   16.7251(2)
_cell_length_c                   13.2575(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3350.87(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4079
_cell_measurement_theta_min      3.942
_cell_measurement_theta_max      62.478

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_F_000             1676
_exptl_transmission_factor_min   0.023
_exptl_transmission_factor_max   0.103
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    11.151
_shelx_estimated_absorpt_T_min   0.135
_shelx_estimated_absorpt_T_max   0.214
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   multi-scan

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  Germini
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         2
_diffrn_standards_interval_count 150
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            8885
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.942
_diffrn_reflns_theta_max         62.478
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.872
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.872
_diffrn_reflns_point_group_measured_fraction_max 0.841
_diffrn_reflns_point_group_measured_fraction_full 0.743
_reflns_number_total             4497
_reflns_number_gt                4079
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.628
_reflns_Friedel_fraction_max     0.682
_reflns_Friedel_fraction_full    0.602

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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/[σ²(Fo²)+(0.0414P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.004(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4497
_refine_ls_number_parameters     459
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0289
_refine_ls_wR_factor_ref         0.0692
_refine_ls_wR_factor_gt          0.0683
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_restrained_S_all      0.997
_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_site_symmetry_order
_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
Ce1 Ce 0.51138(2) 0.17553(2) 0.37391(5) 0.02184(11) Uani 1 1 d . . . . .
N1 N 0.2445(4) 0.0471(3) 0.0550(4) 0.0241(12) Uani 1 1 d . . . . .
N2 N -0.1901(4) -0.0032(3) 0.0453(4) 0.0214(11) Uani 1 1 d . . . . .
N3 N -0.0270(4) 0.3104(3) -0.1535(4) 0.0225(14) Uani 1 1 d . . . . .
N4 N 0.6054(4) 0.1963(3) 0.5727(4) 0.0262(14) Uani 1 1 d . . . . .
N5 N 0.4288(5) 0.3375(4) 0.3411(5) 0.0390(17) Uani 1 1 d . . . . .
N6 N 0.6478(5) 0.1925(3) 0.2067(5) 0.0382(18) Uani 1 1 d . . . . .
O1 O 0.4431(4) 0.0990(3) 0.2495(5) 0.0545(17) Uani 1 1 d . . . . .
O2 O -0.3636(3) -0.1703(3) -0.0601(4) 0.0347(11) Uani 1 1 d . . . . .
O3 O -0.0390(3) 0.5434(3) -0.0615(3) 0.0317(11) Uani 1 1 d . . . . .
O4 O 0.6485(3) 0.1966(3) 0.4905(4) 0.0319(12) Uani 1 1 d . . . . .
O5 O 0.5233(3) 0.1942(3) 0.5684(4) 0.0364(12) Uani 1 1 d . . . . .
O6 O 0.6453(4) 0.1963(3) 0.6548(4) 0.0429(14) Uani 1 1 d . . . . .
O7 O 0.4801(4) 0.3235(3) 0.4169(4) 0.0406(14) Uani 1 1 d . . . . .
O8 O 0.4239(4) 0.2849(3) 0.2744(4) 0.0361(12) Uani 1 1 d . . . . .
O9 O 0.3882(5) 0.3999(3) 0.3350(4) 0.064(2) Uani 1 1 d . . . . .
O10 O 0.6156(4) 0.2523(3) 0.2506(4) 0.0508(15) Uani 1 1 d . . . . .
O11 O 0.6387(4) 0.1269(3) 0.2537(4) 0.0523(16) Uani 1 1 d . . . . .
O12 O 0.6887(5) 0.1964(3) 0.1293(5) 0.059(2) Uani 1 1 d . . . . .
C1 C 0.0698(6) 0.0189(5) 0.2137(5) 0.0422(19) Uani 1 1 d . . . . .
H1A H 0.0813 -0.0242 0.2622 0.063 Uiso 1 1 calc R U . . .
H1B H 0.0199 0.0512 0.2372 0.063 Uiso 1 1 calc R U . . .
H1C H 0.1225 0.0527 0.2077 0.063 Uiso 1 1 calc R U . . .
C2 C 0.0477(5) -0.0173(4) 0.1108(5) 0.0334(17) Uani 1 1 d . . . . .
H2A H 0.0976 -0.0513 0.0886 0.040 Uiso 1 1 calc R U . . .
H2B H -0.0051 -0.0519 0.1177 0.040 Uiso 1 1 calc R U . . .
C3 C 0.1744(5) 0.1251(4) -0.2628(5) 0.0345(16) Uani 1 1 d . . . . .
H3A H 0.2242 0.1493 -0.2990 0.052 Uiso 1 1 calc R U . . .
H3B H 0.1206 0.1298 -0.3036 0.052 Uiso 1 1 calc R U . . .
H3C H 0.1870 0.0685 -0.2502 0.052 Uiso 1 1 calc R U . . .
C4 C 0.1611(5) 0.1682(4) -0.1625(5) 0.0273(15) Uani 1 1 d . . . . .
H4A H 0.2162 0.1641 -0.1223 0.033 Uiso 1 1 calc R U . . .
H4B H 0.1499 0.2255 -0.1757 0.033 Uiso 1 1 calc R U . . .
C5 C -0.2193(5) 0.1257(4) -0.1462(5) 0.0315(18) Uani 1 1 d . . . . .
H5A H -0.2780 0.1502 -0.1518 0.047 Uiso 1 1 calc R U . . .
H5B H -0.2255 0.0698 -0.1254 0.047 Uiso 1 1 calc R U . . .
H5C H -0.1895 0.1282 -0.2118 0.047 Uiso 1 1 calc R U . . .
C6 C -0.1642(4) 0.1713(4) -0.0673(5) 0.0281(15) Uani 1 1 d . . . . .
H6A H -0.1597 0.2280 -0.0882 0.034 Uiso 1 1 calc R U . . .
H6B H -0.1959 0.1698 -0.0019 0.034 Uiso 1 1 calc R U . . .
C7 C 0.0299(5) 0.0451(4) 0.0313(5) 0.0241(14) Uani 1 1 d . . . . .
C8 C 0.0990(4) 0.0715(3) -0.0324(5) 0.0218(14) Uani 1 1 d . . . . .
C9 C 0.0847(4) 0.1345(3) -0.1011(4) 0.0199(14) Uani 1 1 d . . . . .
C10 C -0.0013(3) 0.1651(3) -0.1129(8) 0.0192(15) Uani 1 1 d . . . . .
C11 C -0.0716(4) 0.1384(3) -0.0522(4) 0.0195(13) Uani 1 1 d . . . . .
C12 C -0.0544(4) 0.0799(3) 0.0221(5) 0.0208(13) Uani 1 1 d . . . . .
C13 C 0.1873(4) 0.0282(4) -0.0321(5) 0.0277(14) Uani 1 1 d . . . . .
H13A H 0.1762 -0.0301 -0.0331 0.033 Uiso 1 1 calc R U . . .
H13B H 0.2196 0.0420 -0.0948 0.033 Uiso 1 1 calc R U . . .
C14 C 0.2964(5) -0.0124(4) 0.0938(5) 0.0302(16) Uani 1 1 d . . . . .
H14A H 0.2873 -0.0660 0.0721 0.036 Uiso 1 1 calc R U . . .
C15 C 0.3594(5) 0.0031(4) 0.1615(6) 0.0351(17) Uani 1 1 d . . . . .
H15A H 0.3933 -0.0397 0.1885 0.042 Uiso 1 1 calc R U . . .
C16 C 0.3769(5) 0.0828(4) 0.1943(6) 0.0356(18) Uani 1 1 d . . . . .
C17 C 0.3180(5) 0.1418(4) 0.1583(5) 0.0344(17) Uani 1 1 d . . . . .
H17A H 0.3226 0.1952 0.1820 0.041 Uiso 1 1 calc R U . . .
C18 C 0.2550(5) 0.1224(4) 0.0899(5) 0.0299(15) Uani 1 1 d . . . . .
H18A H 0.2168 0.1631 0.0656 0.036 Uiso 1 1 calc R U . . .
C19 C -0.1275(5) 0.0540(4) 0.0921(5) 0.0258(14) Uani 1 1 d . . . . .
H19A H -0.1009 0.0289 0.1526 0.031 Uiso 1 1 calc R U . . .
H19B H -0.1606 0.1019 0.1146 0.031 Uiso 1 1 calc R U . . .
C20 C -0.1624(5) -0.0622(4) -0.0180(5) 0.0244(14) Uani 1 1 d . . . . .
H20A H -0.1018 -0.0642 -0.0370 0.029 Uiso 1 1 calc R U . . .
C21 C -0.2186(4) -0.1183(4) -0.0548(5) 0.0255(14) Uani 1 1 d . . . . .
H21A H -0.1968 -0.1586 -0.0987 0.031 Uiso 1 1 calc R U . . .
C22 C -0.3099(4) -0.1173(4) -0.0284(5) 0.0258(14) Uani 1 1 d . . . . .
C23 C -0.3368(5) -0.0553(4) 0.0374(5) 0.0263(15) Uani 1 1 d . . . . .
H23A H -0.3969 -0.0518 0.0577 0.032 Uiso 1 1 calc R U . . .
C24 C -0.2774(5) -0.0005(4) 0.0718(5) 0.0267(15) Uani 1 1 d . . . . .
H24A H -0.2973 0.0408 0.1156 0.032 Uiso 1 1 calc R U . . .
C25 C -0.0188(4) 0.2269(3) -0.1942(5) 0.0226(14) Uani 1 1 d . . . . .
H25A H 0.0301 0.2254 -0.2439 0.027 Uiso 1 1 calc R U . . .
H25B H -0.0741 0.2128 -0.2299 0.027 Uiso 1 1 calc R U . . .
C26 C 0.0065(5) 0.3326(4) -0.0629(6) 0.0286(17) Uani 1 1 d . . . . .
H26A H 0.0339 0.2934 -0.0216 0.034 Uiso 1 1 calc R U . . .
C27 C 0.0021(5) 0.4092(4) -0.0294(5) 0.0300(16) Uani 1 1 d . . . . .
H27A H 0.0251 0.4225 0.0352 0.036 Uiso 1 1 calc R U . . .
C28 C -0.0371(5) 0.4701(4) -0.0909(5) 0.0260(15) Uani 1 1 d . . . . .
C29 C -0.0730(5) 0.4439(4) -0.1836(5) 0.0298(16) Uani 1 1 d . . . . .
H29A H -0.1017 0.4814 -0.2263 0.036 Uiso 1 1 calc R U . . .
C30 C -0.0673(5) 0.3658(4) -0.2131(5) 0.0291(16) Uani 1 1 d . . . . .
H30A H -0.0918 0.3500 -0.2760 0.035 Uiso 1 1 calc R U . . .
O1W O 0.8377(4) 0.2156(5) 0.6181(5) 0.0602(18) Uani 1 1 d D . . . .
H1W2 H 0.779(3) 0.204(7) 0.614(7) 0.09(4) Uiso 1 1 d D . . . .
H1W1 H 0.863(6) 0.227(9) 0.556(4) 0.14(6) Uiso 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ce1 O1 2.329(5) . Yes
Ce1 O2 2.400(5) 2 Yes
Ce1 O3 2.406(4) 4_545 Yes
Ce1 O7 2.582(5) . Yes
Ce1 O5 2.603(5) . Yes
Ce1 O10 2.609(5) . Yes
Ce1 O4 2.610(5) . Yes
Ce1 O8 2.615(5) . Yes
Ce1 O11 2.628(6) . Yes
Ce1 N4 3.014(6) . ?
Ce1 N5 3.014(6) . ?
N1 C18 1.350(8) . ?
N1 C14 1.368(8) . ?
N1 C13 1.477(8) . ?
N2 C20 1.363(8) . ?
N2 C24 1.366(9) . ?
N2 C19 1.482(8) . ?
N3 C26 1.356(10) . ?
N3 C30 1.362(8) . ?
N3 C25 1.501(8) . ?
N4 O5 1.242(8) . ?
N4 O6 1.245(7) . ?
N4 O4 1.269(8) . ?
N5 O9 1.214(8) . ?
N5 O8 1.249(8) . ?
N5 O7 1.291(8) . ?
N6 O12 1.199(8) . ?
N6 O10 1.256(8) . ?
N6 O11 1.269(8) . ?
O1 C16 1.269(9) . ?
O2 C22 1.273(8) . ?
O2 Ce1 2.400(5) 2_554 ?
O3 C28 1.287(8) . ?
O3 Ce1 2.406(4) 4_554 ?
C1 C2 1.529(10) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C7 1.507(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.526(9) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C9 1.520(9) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.540(9) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C11 1.517(9) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C12 1.406(9) . ?
C7 C8 1.414(9) . ?
C8 C9 1.409(9) . ?
C8 C13 1.518(9) . ?
C9 C10 1.406(8) . ?
C10 C11 1.406(10) . ?
C10 C25 1.516(10) . ?
C11 C12 1.413(8) . ?
C12 C19 1.507(9) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.335(10) . ?
C14 H14A 0.9500 . ?
C15 C16 1.427(10) . ?
C15 H15A 0.9500 . ?
C16 C17 1.412(10) . ?
C17 C18 1.355(10) . ?
C17 H17A 0.9500 . ?
C18 H18A 0.9500 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.356(9) . ?
C20 H20A 0.9500 . ?
C21 C22 1.424(9) . ?
C21 H21A 0.9500 . ?
C22 C23 1.415(10) . ?
C23 C24 1.362(10) . ?
C23 H23A 0.9500 . ?
C24 H24A 0.9500 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.357(10) . ?
C26 H26A 0.9500 . ?
C27 C28 1.433(10) . ?
C27 H27A 0.9500 . ?
C28 C29 1.413(9) . ?
C29 C30 1.365(10) . ?
C29 H29A 0.9500 . ?
C30 H30A 0.9500 . ?
O1W H1W2 0.90(3) . ?
O1W H1W1 0.93(3) . ?

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 Ce1 O2 80.0(2) . 2 Yes
O1 Ce1 O3 79.88(18) . 4_545 Yes
O2 Ce1 O3 89.90(17) 2 4_545 Yes
O1 Ce1 O7 126.98(18) . . Yes
O2 Ce1 O7 77.52(18) 2 . Yes
O3 Ce1 O7 146.42(17) 4_545 . Yes
O1 Ce1 O5 143.0(2) . . Yes
O2 Ce1 O5 73.01(17) 2 . Yes
O3 Ce1 O5 75.27(16) 4_545 . Yes
O7 Ce1 O5 71.30(17) . . Yes
O1 Ce1 O10 95.4(2) . . Yes
O2 Ce1 O10 143.91(17) 2 . Yes
O3 Ce1 O10 124.80(17) 4_545 . Yes
O7 Ce1 O10 77.11(17) . . Yes
O5 Ce1 O10 121.33(18) . . Yes
O1 Ce1 O4 147.74(17) . . Yes
O2 Ce1 O4 121.86(16) 2 . Yes
O3 Ce1 O4 77.02(16) 4_545 . Yes
O7 Ce1 O4 83.43(17) . . Yes
O5 Ce1 O4 48.85(15) . . Yes
O10 Ce1 O4 79.95(18) . . Yes
O1 Ce1 O8 78.64(17) . . Yes
O2 Ce1 O8 74.86(17) 2 . Yes
O3 Ce1 O8 155.48(16) 4_545 . Yes
O7 Ce1 O8 49.33(16) . . Yes
O5 Ce1 O8 116.80(16) . . Yes
O10 Ce1 O8 69.16(18) . . Yes
O4 Ce1 O8 127.32(15) . . Yes
O1 Ce1 O11 74.0(2) . . Yes
O2 Ce1 O11 153.05(18) 2 . Yes
O3 Ce1 O11 78.75(17) 4_545 . Yes
O7 Ce1 O11 124.34(17) . . Yes
O5 Ce1 O11 125.95(19) . . Yes
O10 Ce1 O11 47.92(15) . . Yes
O4 Ce1 O11 79.60(18) . . Yes
O8 Ce1 O11 106.29(17) . . Yes
O1 Ce1 N4 153.08(18) . . ?
O2 Ce1 N4 97.12(18) 2 . ?
O3 Ce1 N4 73.33(15) 4_545 . ?
O7 Ce1 N4 77.46(16) . . ?
O5 Ce1 N4 24.16(16) . . ?
O10 Ce1 N4 101.93(18) . . ?
O4 Ce1 N4 24.77(16) . . ?
O8 Ce1 N4 126.79(15) . . ?
O11 Ce1 N4 102.76(19) . . ?
O1 Ce1 N5 102.01(19) . . ?
O2 Ce1 N5 72.54(17) 2 . ?
O3 Ce1 N5 161.53(17) 4_545 . ?
O7 Ce1 N5 25.18(17) . . ?
O5 Ce1 N5 93.67(17) . . ?
O10 Ce1 N5 73.55(17) . . ?
O4 Ce1 N5 107.05(18) . . ?
O8 Ce1 N5 24.34(16) . . ?
O11 Ce1 N5 119.57(17) . . ?
N4 Ce1 N5 102.58(17) . . ?
C18 N1 C14 118.8(6) . . ?
C18 N1 C13 122.4(5) . . ?
C14 N1 C13 118.3(5) . . ?
C20 N2 C24 118.7(6) . . ?
C20 N2 C19 122.0(6) . . ?
C24 N2 C19 119.2(5) . . ?
C26 N3 C30 119.6(6) . . ?
C26 N3 C25 122.8(5) . . ?
C30 N3 C25 117.5(5) . . ?
O5 N4 O6 121.6(6) . . ?
O5 N4 O4 118.3(5) . . ?
O6 N4 O4 120.1(6) . . ?
O5 N4 Ce1 59.1(3) . . ?
O6 N4 Ce1 173.3(4) . . ?
O4 N4 Ce1 59.5(3) . . ?
O9 N5 O8 121.9(7) . . ?
O9 N5 O7 120.8(6) . . ?
O8 N5 O7 117.3(6) . . ?
O9 N5 Ce1 172.7(5) . . ?
O8 N5 Ce1 59.6(4) . . ?
O7 N5 Ce1 58.4(3) . . ?
O12 N6 O10 123.5(6) . . ?
O12 N6 O11 121.5(6) . . ?
O10 N6 O11 114.8(6) . . ?
C16 O1 Ce1 151.1(5) . . ?
C22 O2 Ce1 137.6(4) . 2_554 ?
C28 O3 Ce1 139.8(4) . 4_554 ?
N4 O4 Ce1 95.7(4) . . ?
N4 O5 Ce1 96.8(4) . . ?
N5 O7 Ce1 96.5(4) . . ?
N5 O8 Ce1 96.1(4) . . ?
N6 O10 Ce1 97.6(4) . . ?
N6 O11 Ce1 96.3(4) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C7 C2 C1 112.9(6) . . ?
C7 C2 H2A 109.0 . . ?
C1 C2 H2A 109.0 . . ?
C7 C2 H2B 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C4 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C9 C4 C3 113.1(5) . . ?
C9 C4 H4A 109.0 . . ?
C3 C4 H4A 109.0 . . ?
C9 C4 H4B 109.0 . . ?
C3 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
C6 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C6 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C11 C6 C5 114.1(5) . . ?
C11 C6 H6A 108.7 . . ?
C5 C6 H6A 108.7 . . ?
C11 C6 H6B 108.7 . . ?
C5 C6 H6B 108.7 . . ?
H6A C6 H6B 107.6 . . ?
C12 C7 C8 119.2(6) . . ?
C12 C7 C2 120.6(6) . . ?
C8 C7 C2 120.1(6) . . ?
C9 C8 C7 120.4(6) . . ?
C9 C8 C13 119.5(6) . . ?
C7 C8 C13 120.0(6) . . ?
C10 C9 C8 119.1(6) . . ?
C10 C9 C4 120.5(6) . . ?
C8 C9 C4 120.4(6) . . ?
C9 C10 C11 121.3(7) . . ?
C9 C10 C25 119.3(6) . . ?
C11 C10 C25 119.4(5) . . ?
C10 C11 C12 118.7(6) . . ?
C10 C11 C6 120.5(5) . . ?
C12 C11 C6 120.8(6) . . ?
C7 C12 C11 121.0(6) . . ?
C7 C12 C19 119.4(5) . . ?
C11 C12 C19 119.6(6) . . ?
N1 C13 C8 114.5(5) . . ?
N1 C13 H13A 108.6 . . ?
C8 C13 H13A 108.6 . . ?
N1 C13 H13B 108.6 . . ?
C8 C13 H13B 108.6 . . ?
H13A C13 H13B 107.6 . . ?
C15 C14 N1 121.4(6) . . ?
C15 C14 H14A 119.3 . . ?
N1 C14 H14A 119.3 . . ?
C14 C15 C16 121.3(6) . . ?
C14 C15 H15A 119.4 . . ?
C16 C15 H15A 119.4 . . ?
O1 C16 C17 122.8(7) . . ?
O1 C16 C15 121.4(7) . . ?
C17 C16 C15 115.7(6) . . ?
C18 C17 C16 120.1(6) . . ?
C18 C17 H17A 120.0 . . ?
C16 C17 H17A 120.0 . . ?
N1 C18 C17 122.4(6) . . ?
N1 C18 H18A 118.8 . . ?
C17 C18 H18A 118.8 . . ?
N2 C19 C12 113.3(5) . . ?
N2 C19 H19A 108.9 . . ?
C12 C19 H19A 108.9 . . ?
N2 C19 H19B 108.9 . . ?
C12 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
C21 C20 N2 122.0(6) . . ?
C21 C20 H20A 119.0 . . ?
N2 C20 H20A 119.0 . . ?
C20 C21 C22 120.8(6) . . ?
C20 C21 H21A 119.6 . . ?
C22 C21 H21A 119.6 . . ?
O2 C22 C23 122.1(6) . . ?
O2 C22 C21 121.9(6) . . ?
C23 C22 C21 115.9(6) . . ?
C24 C23 C22 120.8(6) . . ?
C24 C23 H23A 119.6 . . ?
C22 C23 H23A 119.6 . . ?
C23 C24 N2 121.8(6) . . ?
C23 C24 H24A 119.1 . . ?
N2 C24 H24A 119.1 . . ?
N3 C25 C10 113.1(5) . . ?
N3 C25 H25A 109.0 . . ?
C10 C25 H25A 109.0 . . ?
N3 C25 H25B 109.0 . . ?
C10 C25 H25B 109.0 . . ?
H25A C25 H25B 107.8 . . ?
N3 C26 C27 122.1(7) . . ?
N3 C26 H26A 119.0 . . ?
C27 C26 H26A 119.0 . . ?
C26 C27 C28 120.3(7) . . ?
C26 C27 H27A 119.8 . . ?
C28 C27 H27A 119.8 . . ?
O3 C28 C29 123.4(6) . . ?
O3 C28 C27 120.9(6) . . ?
C29 C28 C27 115.7(6) . . ?
C30 C29 C28 121.4(6) . . ?
C30 C29 H29A 119.3 . . ?
C28 C29 H29A 119.3 . . ?
N3 C30 C29 120.9(6) . . ?
N3 C30 H30A 119.6 . . ?
C29 C30 H30A 119.6 . . ?
H1W2 O1W H1W1 113(4) . . ?

_refine_diff_density_max         0.429
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.075

_shelxl_version_number           2013-4




#================================#

_database_code_depnum_ccdc_archive 'CCDC 992360'
