# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2013


#######################################################################
#
#                 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 
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#  except for the purpose of generating routine backup copies 
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data_y
_database_code_depnum_ccdc_archive 'CCDC 900871'
#TrackingRef '900871.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C66 H86 Ce2 N12 O34'
_chemical_formula_sum            'C66 H86 Ce2 N12 O34'
_chemical_formula_weight         1871.68
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'
_cell_length_a                   32.5470(10)
_cell_length_b                   17.5335(6)
_cell_length_c                   13.7923(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7870.8(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4050
_cell_measurement_theta_min      3.0184
_cell_measurement_theta_max      29.0248
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3656
_exptl_absorpt_coefficient_mu    1.231
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7856
_exptl_absorpt_correction_T_max  0.8724
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16969
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0969
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6892
_reflns_number_gt                3737
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
dfix 0.90 0.01 n3 h311 n1 h111 n2 h211
delu 0.008 c15 c20 c9 c10 c12 c13 c15 c20 c17 c18 c18 c19 n3 c29
isor 0.01 o12 c11 c17 c26 c32 c15 c20 o8 o14
'SQUEEZE' command is used to deal with the crystalized water molecules.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6892
_refine_ls_number_parameters     508
_refine_ls_number_restraints     67
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0560
_refine_ls_wR_factor_ref         0.1057
_refine_ls_wR_factor_gt          0.0885
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_restrained_S_all      0.990
_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
C1 C 0.2295(2) 0.3365(4) 0.6419(5) 0.0693(19) Uani 1 1 d . . .
C2 C 0.2060(3) 0.4010(4) 0.6168(5) 0.074(2) Uani 1 1 d . . .
C3 C 0.2227(3) 0.4605(4) 0.5649(5) 0.085(2) Uani 1 1 d . . .
H3 H 0.2066 0.5025 0.5487 0.102 Uiso 1 1 calc R . .
C4 C 0.2644(3) 0.4576(4) 0.5363(5) 0.093(3) Uani 1 1 d . . .
H4 H 0.2759 0.4988 0.5038 0.112 Uiso 1 1 calc R . .
C5 C 0.2873(2) 0.3967(5) 0.5553(5) 0.092(2) Uani 1 1 d . . .
H5 H 0.3144 0.3949 0.5344 0.110 Uiso 1 1 calc R . .
C6 C 0.2706(2) 0.3348(4) 0.6070(5) 0.073(2) Uani 1 1 d . . .
C7 C 0.2958(2) 0.2703(5) 0.6253(5) 0.090(2) Uani 1 1 d . . .
H7 H 0.3224 0.2698 0.6004 0.108 Uiso 1 1 calc R . .
C8 C 0.3069(2) 0.1420(4) 0.7010(6) 0.089(2) Uani 1 1 d . . .
H8 H 0.2997 0.1019 0.6546 0.107 Uiso 1 1 calc R . .
C9 C 0.3534(2) 0.1530(5) 0.6982(6) 0.113(3) Uani 1 1 d U . .
H9A H 0.3667 0.1041 0.7081 0.136 Uiso 1 1 calc R . .
H9B H 0.3612 0.1715 0.6346 0.136 Uiso 1 1 calc R . .
C10 C 0.3681(2) 0.2076(4) 0.7731(7) 0.115(3) Uani 1 1 d U . .
H10A H 0.3568 0.2579 0.7607 0.138 Uiso 1 1 calc R . .
H10B H 0.3978 0.2110 0.7711 0.138 Uiso 1 1 calc R . .
C11 C 0.3542(3) 0.1793(5) 0.8718(7) 0.120(3) Uani 1 1 d U . .
H11A H 0.3633 0.2146 0.9215 0.144 Uiso 1 1 calc R . .
H11B H 0.3665 0.1300 0.8849 0.144 Uiso 1 1 calc R . .
C12 C 0.3061(2) 0.1722(4) 0.8745(5) 0.096(2) Uani 1 1 d U . .
H12A H 0.2972 0.1552 0.9381 0.116 Uiso 1 1 calc R . .
H12B H 0.2936 0.2213 0.8614 0.116 Uiso 1 1 calc R . .
C13 C 0.2937(2) 0.1163(4) 0.8000(6) 0.078(2) Uani 1 1 d U . .
H13 H 0.3069 0.0673 0.8143 0.094 Uiso 1 1 calc R . .
C14 C 0.2305(2) 0.0411(4) 0.7944(5) 0.0720(19) Uani 1 1 d . . .
H14 H 0.2469 -0.0020 0.7887 0.086 Uiso 1 1 calc R . .
C15 C 0.1878(2) 0.0301(3) 0.7941(5) 0.0658(17) Uani 1 1 d U . .
C16 C 0.1706(2) -0.0435(3) 0.7836(5) 0.089(2) Uani 1 1 d . . .
H16 H 0.1878 -0.0857 0.7796 0.107 Uiso 1 1 calc R . .
C17 C 0.1297(3) -0.0533(4) 0.7792(6) 0.104(3) Uani 1 1 d U . .
H17 H 0.1187 -0.1020 0.7730 0.125 Uiso 1 1 calc R . .
C18 C 0.1039(2) 0.0096(4) 0.7841(5) 0.090(2) Uani 1 1 d U . .
H18 H 0.0757 0.0025 0.7801 0.108 Uiso 1 1 calc R . .
C19 C 0.1188(2) 0.0807(4) 0.7943(5) 0.0696(18) Uani 1 1 d U . .
C20 C 0.1613(2) 0.0957(4) 0.7979(5) 0.0623(16) Uani 1 1 d U . .
C21 C 0.05182(19) 0.1387(4) 0.7911(5) 0.102(3) Uani 1 1 d . . .
H21A H 0.0444 0.1184 0.7288 0.153 Uiso 1 1 calc R . .
H21B H 0.0393 0.1878 0.7994 0.153 Uiso 1 1 calc R . .
H21C H 0.0424 0.1049 0.8411 0.153 Uiso 1 1 calc R . .
C22 C 0.1372(2) 0.4461(4) 0.5998(5) 0.099(3) Uani 1 1 d . . .
H22A H 0.1387 0.4958 0.6287 0.148 Uiso 1 1 calc R . .
H22B H 0.1099 0.4263 0.6068 0.148 Uiso 1 1 calc R . .
H22C H 0.1439 0.4497 0.5321 0.148 Uiso 1 1 calc R . .
C23 C 0.0775(2) 0.2590(4) 0.6102(5) 0.0597(17) Uani 1 1 d . . .
C24 C 0.0393(2) 0.2732(4) 0.5689(5) 0.0665(19) Uani 1 1 d . . .
C25 C 0.0246(2) 0.2254(5) 0.4944(6) 0.104(3) Uani 1 1 d . . .
H25 H -0.0013 0.2342 0.4680 0.125 Uiso 1 1 calc R . .
C26 C 0.0474(3) 0.1673(5) 0.4611(6) 0.114(3) Uani 1 1 d U . .
H26 H 0.0375 0.1363 0.4117 0.137 Uiso 1 1 calc R . .
C27 C 0.0865(2) 0.1533(4) 0.5011(5) 0.093(2) Uani 1 1 d . . .
H27 H 0.1020 0.1123 0.4789 0.112 Uiso 1 1 calc R . .
C28 C 0.1015(2) 0.1987(4) 0.5711(5) 0.070(2) Uani 1 1 d . . .
C29 C 0.01541(18) 0.3357(4) 0.6005(5) 0.0693(19) Uani 1 1 d U . .
H29 H -0.0101 0.3427 0.5715 0.083 Uiso 1 1 calc R . .
C30 C 0.00359(19) 0.4521(3) 0.6950(4) 0.0696(19) Uani 1 1 d . . .
H30 H -0.0231 0.4515 0.6622 0.084 Uiso 1 1 calc R . .
C31 C 0.0270(2) 0.5243(4) 0.6647(6) 0.100(3) Uani 1 1 d . . .
H31A H 0.0540 0.5245 0.6943 0.119 Uiso 1 1 calc R . .
H31B H 0.0304 0.5250 0.5949 0.119 Uiso 1 1 calc R . .
C32 C 0.0029(3) 0.5952(4) 0.6970(5) 0.121(3) Uani 1 1 d U . .
H32A H 0.0178 0.6408 0.6780 0.145 Uiso 1 1 calc R . .
H32B H -0.0236 0.5960 0.6652 0.145 Uiso 1 1 calc R . .
C33 C 0.1681(2) 0.1401(4) 0.5678(5) 0.104(3) Uani 1 1 d . . .
H33A H 0.1569 0.0895 0.5708 0.156 Uiso 1 1 calc R . .
H33B H 0.1939 0.1415 0.6017 0.156 Uiso 1 1 calc R . .
H33C H 0.1724 0.1540 0.5012 0.156 Uiso 1 1 calc R . .
Ce1 Ce 0.148763(10) 0.291601(19) 0.79376(3) 0.05901(15) Uani 1 1 d . . .
N1 N 0.28329(18) 0.2113(4) 0.6758(4) 0.0782(17) Uani 1 1 d D . .
H111 H 0.2629(15) 0.237(3) 0.706(5) 0.117 Uiso 1 1 d D . .
N2 N 0.24877(17) 0.1060(3) 0.8019(4) 0.0732(16) Uani 1 1 d D . .
H211 H 0.2319(16) 0.146(2) 0.811(5) 0.110 Uiso 1 1 d D . .
N3 N 0.02641(15) 0.3841(3) 0.6670(4) 0.0624(14) Uani 1 1 d DU . .
H311 H 0.0515(8) 0.373(3) 0.690(4) 0.094 Uiso 1 1 d D . .
N4 N 0.0951(2) 0.2550(4) 0.9757(6) 0.103(2) Uani 1 1 d . . .
N5 N 0.1082(2) 0.4397(4) 0.8950(5) 0.094(2) Uani 1 1 d . . .
N6 N 0.22500(18) 0.3525(4) 0.8983(5) 0.0784(18) Uani 1 1 d . . .
O1 O 0.21275(12) 0.2816(2) 0.6906(3) 0.0632(11) Uani 1 1 d . . .
O2 O 0.16590(16) 0.3959(2) 0.6472(3) 0.0851(15) Uani 1 1 d . . .
O3 O 0.17597(12) 0.1632(2) 0.8071(3) 0.0691(12) Uani 1 1 d . . .
O4 O 0.09558(13) 0.1462(2) 0.7969(3) 0.0808(13) Uani 1 1 d . . .
O5 O 0.09188(12) 0.2982(2) 0.6820(3) 0.0601(11) Uani 1 1 d . . .
O6 O 0.13987(13) 0.1930(2) 0.6120(3) 0.0786(14) Uani 1 1 d . . .
O7 O 0.13205(15) 0.2375(3) 0.9668(3) 0.0903(15) Uani 1 1 d . . .
O8 O 0.0759(2) 0.2451(4) 1.0512(5) 0.160(3) Uani 1 1 d U . .
O9 O 0.07874(14) 0.2839(3) 0.9008(4) 0.0868(15) Uani 1 1 d . . .
O10 O 0.13329(16) 0.4022(3) 0.9469(4) 0.1015(17) Uani 1 1 d . . .
O11 O 0.08723(19) 0.4894(4) 0.9272(5) 0.165(3) Uani 1 1 d . . .
O12 O 0.10708(15) 0.4195(2) 0.8065(4) 0.0908(15) Uani 1 1 d U . .
O13 O 0.20601(14) 0.3950(2) 0.8396(3) 0.0816(14) Uani 1 1 d . . .
O14 O 0.25543(18) 0.3748(3) 0.9365(5) 0.148(2) Uani 1 1 d U . .
O15 O 0.21174(13) 0.2876(2) 0.9105(3) 0.0726(13) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.075(5) 0.081(5) 0.052(5) -0.001(4) -0.003(4) -0.024(4)
C2 0.100(6) 0.065(5) 0.057(5) 0.005(4) 0.004(5) -0.003(5)
C3 0.124(7) 0.064(5) 0.067(6) -0.003(4) 0.000(5) -0.001(5)
C4 0.130(8) 0.077(6) 0.073(6) -0.003(4) 0.016(6) -0.025(6)
C5 0.094(6) 0.105(7) 0.077(6) 0.011(5) 0.014(5) -0.033(5)
C6 0.073(5) 0.082(5) 0.063(5) 0.006(4) 0.000(4) -0.019(4)
C7 0.077(5) 0.121(7) 0.072(6) 0.015(5) 0.014(5) -0.009(5)
C8 0.080(5) 0.104(6) 0.084(6) -0.003(5) -0.003(5) 0.014(5)
C9 0.075(6) 0.130(7) 0.135(8) -0.021(6) 0.017(6) 0.008(5)
C10 0.076(6) 0.130(8) 0.139(9) -0.011(6) -0.002(6) -0.030(5)
C11 0.106(6) 0.137(6) 0.118(7) -0.008(5) -0.024(5) -0.014(5)
C12 0.091(6) 0.113(6) 0.085(6) 0.002(4) 0.004(5) 0.005(5)
C13 0.075(5) 0.066(5) 0.093(6) 0.004(4) 0.011(5) 0.011(4)
C14 0.088(5) 0.058(4) 0.070(5) -0.001(4) 0.006(5) 0.006(4)
C15 0.077(4) 0.052(4) 0.068(4) -0.003(3) 0.009(4) -0.003(3)
C16 0.117(7) 0.043(4) 0.106(7) 0.007(4) 0.016(6) 0.015(4)
C17 0.115(6) 0.071(4) 0.127(7) 0.002(4) 0.015(6) -0.016(4)
C18 0.076(5) 0.080(5) 0.114(7) -0.005(5) 0.005(5) -0.016(3)
C19 0.070(4) 0.061(4) 0.078(5) -0.002(4) 0.013(4) -0.008(3)
C20 0.074(4) 0.064(4) 0.049(4) 0.003(3) 0.003(4) -0.014(3)
C21 0.065(5) 0.111(6) 0.130(7) -0.011(5) -0.010(5) -0.009(4)
C22 0.112(7) 0.086(5) 0.097(7) 0.020(5) -0.004(5) 0.019(5)
C23 0.062(4) 0.071(5) 0.046(5) -0.009(4) -0.001(4) -0.001(4)
C24 0.051(4) 0.086(5) 0.062(5) -0.010(4) -0.007(4) 0.001(4)
C25 0.068(5) 0.148(8) 0.095(7) -0.053(6) -0.016(5) 0.012(5)
C26 0.105(6) 0.135(6) 0.104(6) -0.052(5) -0.027(5) 0.008(5)
C27 0.073(5) 0.111(6) 0.095(7) -0.043(5) 0.003(5) 0.010(5)
C28 0.057(4) 0.089(5) 0.064(5) -0.012(4) -0.007(4) 0.002(4)
C29 0.043(4) 0.097(6) 0.068(5) 0.011(4) -0.003(4) -0.006(4)
C30 0.063(4) 0.060(4) 0.087(5) 0.001(3) 0.002(5) 0.002(4)
C31 0.091(6) 0.082(6) 0.126(7) 0.023(5) 0.018(5) 0.003(5)
C32 0.120(6) 0.082(5) 0.161(8) 0.022(4) -0.001(7) 0.004(5)
C33 0.076(5) 0.148(7) 0.088(6) -0.027(5) 0.011(5) 0.032(5)
Ce1 0.0520(2) 0.0604(3) 0.0646(3) 0.00110(19) -0.0090(2) 0.00388(17)
N1 0.065(4) 0.109(5) 0.060(5) 0.011(4) 0.011(3) 0.011(4)
N2 0.063(4) 0.063(4) 0.093(5) 0.005(4) 0.005(4) 0.008(3)
N3 0.049(3) 0.068(4) 0.069(4) 0.003(3) -0.004(3) 0.004(3)
N4 0.070(5) 0.157(7) 0.081(6) -0.012(5) -0.006(5) -0.012(5)
N5 0.079(5) 0.105(6) 0.098(6) -0.045(5) -0.026(5) 0.013(4)
N6 0.061(4) 0.079(5) 0.096(5) -0.008(4) -0.026(4) -0.009(3)
O1 0.062(3) 0.073(3) 0.054(3) 0.005(2) 0.001(2) -0.005(2)
O2 0.086(4) 0.086(4) 0.083(4) 0.028(3) 0.008(3) 0.010(3)
O3 0.058(3) 0.055(3) 0.094(4) -0.003(2) -0.004(3) -0.005(2)
O4 0.061(3) 0.076(3) 0.105(4) 0.002(3) 0.004(3) -0.004(2)
O5 0.064(3) 0.063(3) 0.054(3) -0.008(2) -0.012(2) 0.012(2)
O6 0.060(3) 0.102(4) 0.073(4) -0.022(3) -0.007(3) 0.014(3)
O7 0.061(3) 0.131(4) 0.080(4) 0.008(3) -0.002(3) 0.007(3)
O8 0.112(5) 0.251(6) 0.117(5) -0.001(5) 0.023(4) -0.026(4)
O9 0.063(3) 0.109(4) 0.088(4) -0.013(3) -0.014(3) 0.011(3)
O10 0.090(4) 0.120(4) 0.094(4) -0.015(3) -0.025(3) -0.003(3)
O11 0.127(5) 0.184(6) 0.183(7) -0.124(5) -0.048(5) 0.072(5)
O12 0.111(4) 0.081(3) 0.080(4) -0.024(3) -0.012(3) 0.015(3)
O13 0.086(4) 0.073(3) 0.085(4) -0.004(3) -0.008(3) -0.007(3)
O14 0.119(4) 0.125(5) 0.199(6) 0.006(4) -0.085(4) -0.036(4)
O15 0.071(3) 0.065(3) 0.081(4) 0.013(3) -0.011(3) -0.013(2)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.293(7) . ?
C1 C2 1.409(9) . ?
C1 C6 1.421(8) . ?
C2 O2 1.373(8) . ?
C2 C3 1.377(8) . ?
C3 C4 1.412(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.328(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.407(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.421(9) . ?
C7 N1 1.311(8) . ?
C7 H7 0.9300 . ?
C8 N1 1.480(8) . ?
C8 C13 1.500(9) . ?
C8 C9 1.526(9) . ?
C8 H8 0.9800 . ?
C9 C10 1.487(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.517(10) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.572(9) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.476(8) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N2 1.475(8) . ?
C13 H13 0.9800 . ?
C14 N2 1.288(7) . ?
C14 C15 1.401(8) . ?
C14 H14 0.9300 . ?
C15 C16 1.415(8) . ?
C15 C20 1.440(8) . ?
C16 C17 1.344(9) . ?
C16 H16 0.9300 . ?
C17 C18 1.387(9) . ?
C17 H17 0.9300 . ?
C18 C19 1.346(7) . ?
C18 H18 0.9300 . ?
C19 O4 1.375(7) . ?
C19 C20 1.408(8) . ?
C20 O3 1.281(6) . ?
C21 O4 1.433(6) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 O2 1.440(7) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 O5 1.292(6) . ?
C23 C24 1.391(8) . ?
C23 C28 1.421(8) . ?
C24 C25 1.411(8) . ?
C24 C29 1.412(8) . ?
C25 C26 1.342(9) . ?
C25 H25 0.9300 . ?
C26 C27 1.407(9) . ?
C26 H26 0.9300 . ?
C27 C28 1.344(8) . ?
C27 H27 0.9300 . ?
C28 O6 1.373(7) . ?
C29 N3 1.301(7) . ?
C29 H29 0.9300 . ?
C30 N3 1.456(7) . ?
C30 C30 1.535(11) 3_556 ?
C30 C31 1.536(8) . ?
C30 H30 0.9800 . ?
C31 C32 1.535(8) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C32 1.473(13) 3_556 ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 O6 1.443(6) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
Ce1 O5 2.412(4) . ?
Ce1 O3 2.427(4) . ?
Ce1 O1 2.529(4) . ?
Ce1 O15 2.608(4) . ?
Ce1 O7 2.625(5) . ?
Ce1 O12 2.627(4) . ?
Ce1 O13 2.675(4) . ?
Ce1 O9 2.719(5) . ?
Ce1 O2 2.783(4) . ?
Ce1 O10 2.911(5) . ?
N1 H111 0.904(11) . ?
N2 H211 0.901(11) . ?
N3 H311 0.895(11) . ?
N4 O8 1.227(8) . ?
N4 O7 1.247(7) . ?
N4 O9 1.267(7) . ?
N5 O11 1.192(7) . ?
N5 O10 1.269(7) . ?
N5 O12 1.271(7) . ?
N6 O14 1.188(6) . ?
N6 O15 1.229(6) . ?
N6 O13 1.261(6) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 119.7(7) . . ?
O1 C1 C6 123.9(7) . . ?
C2 C1 C6 116.3(7) . . ?
O2 C2 C3 125.7(7) . . ?
O2 C2 C1 112.9(6) . . ?
C3 C2 C1 121.4(8) . . ?
C2 C3 C4 119.8(7) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 120.8(8) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C4 C5 C6 120.2(8) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C7 118.7(8) . . ?
C5 C6 C1 121.3(7) . . ?
C7 C6 C1 120.0(7) . . ?
N1 C7 C6 122.8(7) . . ?
N1 C7 H7 118.6 . . ?
C6 C7 H7 118.6 . . ?
N1 C8 C13 108.2(6) . . ?
N1 C8 C9 113.9(7) . . ?
C13 C8 C9 110.1(6) . . ?
N1 C8 H8 108.1 . . ?
C13 C8 H8 108.1 . . ?
C9 C8 H8 108.1 . . ?
C10 C9 C8 112.5(6) . . ?
C10 C9 H9A 109.1 . . ?
C8 C9 H9A 109.1 . . ?
C10 C9 H9B 109.1 . . ?
C8 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
C9 C10 C11 108.5(7) . . ?
C9 C10 H10A 110.0 . . ?
C11 C10 H10A 110.0 . . ?
C9 C10 H10B 110.0 . . ?
C11 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
C10 C11 C12 110.1(7) . . ?
C10 C11 H11A 109.6 . . ?
C12 C11 H11A 109.6 . . ?
C10 C11 H11B 109.6 . . ?
C12 C11 H11B 109.6 . . ?
H11A C11 H11B 108.2 . . ?
C13 C12 C11 107.9(6) . . ?
C13 C12 H12A 110.1 . . ?
C11 C12 H12A 110.1 . . ?
C13 C12 H12B 110.1 . . ?
C11 C12 H12B 110.1 . . ?
H12A C12 H12B 108.4 . . ?
N2 C13 C12 109.9(6) . . ?
N2 C13 C8 109.6(6) . . ?
C12 C13 C8 110.9(6) . . ?
N2 C13 H13 108.8 . . ?
C12 C13 H13 108.8 . . ?
C8 C13 H13 108.8 . . ?
N2 C14 C15 125.5(6) . . ?
N2 C14 H14 117.3 . . ?
C15 C14 H14 117.3 . . ?
C14 C15 C16 121.3(6) . . ?
C14 C15 C20 118.9(6) . . ?
C16 C15 C20 119.6(6) . . ?
C17 C16 C15 121.0(7) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C16 C17 C18 119.7(7) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
C19 C18 C17 121.6(7) . . ?
C19 C18 H18 119.2 . . ?
C17 C18 H18 119.2 . . ?
C18 C19 O4 125.3(6) . . ?
C18 C19 C20 122.1(7) . . ?
O4 C19 C20 112.5(6) . . ?
O3 C20 C19 122.8(6) . . ?
O3 C20 C15 121.2(6) . . ?
C19 C20 C15 116.0(6) . . ?
O4 C21 H21A 109.5 . . ?
O4 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O4 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O2 C22 H22A 109.5 . . ?
O2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
O2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O5 C23 C24 122.8(6) . . ?
O5 C23 C28 119.2(6) . . ?
C24 C23 C28 118.0(6) . . ?
C23 C24 C25 119.8(6) . . ?
C23 C24 C29 120.3(6) . . ?
C25 C24 C29 119.9(7) . . ?
C26 C25 C24 120.8(7) . . ?
C26 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
C25 C26 C27 119.9(7) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C28 C27 C26 120.5(7) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
C27 C28 O6 125.7(7) . . ?
C27 C28 C23 120.9(7) . . ?
O6 C28 C23 113.4(6) . . ?
N3 C29 C24 125.0(6) . . ?
N3 C29 H29 117.5 . . ?
C24 C29 H29 117.5 . . ?
N3 C30 C30 109.9(4) . 3_556 ?
N3 C30 C31 110.5(5) . . ?
C30 C30 C31 110.1(5) 3_556 . ?
N3 C30 H30 108.8 . . ?
C30 C30 H30 108.8 3_556 . ?
C31 C30 H30 108.8 . . ?
C32 C31 C30 109.7(6) . . ?
C32 C31 H31A 109.7 . . ?
C30 C31 H31A 109.7 . . ?
C32 C31 H31B 109.7 . . ?
C30 C31 H31B 109.7 . . ?
H31A C31 H31B 108.2 . . ?
C32 C32 C31 110.7(6) 3_556 . ?
C32 C32 H32A 109.5 3_556 . ?
C31 C32 H32A 109.5 . . ?
C32 C32 H32B 109.5 3_556 . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 108.1 . . ?
O6 C33 H33A 109.5 . . ?
O6 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
O6 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O5 Ce1 O3 111.89(13) . . ?
O5 Ce1 O1 106.02(13) . . ?
O3 Ce1 O1 71.22(13) . . ?
O5 Ce1 O15 177.99(13) . . ?
O3 Ce1 O15 69.00(13) . . ?
O1 Ce1 O15 72.44(13) . . ?
O5 Ce1 O7 116.04(14) . . ?
O3 Ce1 O7 70.82(15) . . ?
O1 Ce1 O7 131.11(14) . . ?
O15 Ce1 O7 65.91(14) . . ?
O5 Ce1 O12 66.78(14) . . ?
O3 Ce1 O12 167.31(15) . . ?
O1 Ce1 O12 121.46(14) . . ?
O15 Ce1 O12 112.79(14) . . ?
O7 Ce1 O12 98.07(16) . . ?
O5 Ce1 O13 130.80(14) . . ?
O3 Ce1 O13 110.91(14) . . ?
O1 Ce1 O13 66.82(13) . . ?
O15 Ce1 O13 47.52(13) . . ?
O7 Ce1 O13 100.03(15) . . ?
O12 Ce1 O13 76.42(15) . . ?
O5 Ce1 O9 72.89(15) . . ?
O3 Ce1 O9 102.61(14) . . ?
O1 Ce1 O9 173.04(13) . . ?
O15 Ce1 O9 108.79(15) . . ?
O7 Ce1 O9 46.72(14) . . ?
O12 Ce1 O9 64.75(15) . . ?
O13 Ce1 O9 119.28(14) . . ?
O5 Ce1 O2 70.02(14) . . ?
O3 Ce1 O2 126.29(14) . . ?
O1 Ce1 O2 58.08(13) . . ?
O15 Ce1 O2 107.98(14) . . ?
O7 Ce1 O2 159.97(15) . . ?
O12 Ce1 O2 65.86(15) . . ?
O13 Ce1 O2 65.60(15) . . ?
O9 Ce1 O2 126.54(15) . . ?
O5 Ce1 O10 107.40(14) . . ?
O3 Ce1 O10 128.77(15) . . ?
O1 Ce1 O10 126.65(13) . . ?
O15 Ce1 O10 72.88(15) . . ?
O7 Ce1 O10 62.94(15) . . ?
O12 Ce1 O10 45.04(14) . . ?
O13 Ce1 O10 59.84(14) . . ?
O9 Ce1 O10 59.61(14) . . ?
O2 Ce1 O10 97.13(15) . . ?
C7 N1 C8 127.7(7) . . ?
C7 N1 H111 95(5) . . ?
C8 N1 H111 133(5) . . ?
C14 N2 C13 124.5(6) . . ?
C14 N2 H211 115(4) . . ?
C13 N2 H211 121(4) . . ?
C29 N3 C30 125.5(6) . . ?
C29 N3 H311 111(4) . . ?
C30 N3 H311 123(4) . . ?
O8 N4 O7 122.7(9) . . ?
O8 N4 O9 122.3(8) . . ?
O7 N4 O9 115.0(7) . . ?
O11 N5 O10 122.5(8) . . ?
O11 N5 O12 122.9(7) . . ?
O10 N5 O12 114.6(6) . . ?
O14 N6 O15 122.4(7) . . ?
O14 N6 O13 119.9(7) . . ?
O15 N6 O13 117.6(6) . . ?
C1 O1 Ce1 126.0(4) . . ?
C2 O2 C22 116.0(5) . . ?
C2 O2 Ce1 117.0(4) . . ?
C22 O2 Ce1 127.0(4) . . ?
C20 O3 Ce1 135.5(4) . . ?
C19 O4 C21 118.0(5) . . ?
C23 O5 Ce1 137.9(4) . . ?
C28 O6 C33 116.9(5) . . ?
N4 O7 Ce1 101.6(5) . . ?
N4 O9 Ce1 96.3(4) . . ?
N5 O10 Ce1 92.7(4) . . ?
N5 O12 Ce1 106.7(4) . . ?
N6 O13 Ce1 95.3(4) . . ?
N6 O15 Ce1 99.6(4) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H311 O5 0.895(11) 1.86(4) 2.618(6) 141(5) .
N2 H211 O3 0.901(11) 1.85(5) 2.574(6) 136(6) .
N1 H111 O1 0.904(11) 1.82(4) 2.614(7) 145(6) .
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.031
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.069


data_276
_database_code_depnum_ccdc_archive 'CCDC 900872'
#TrackingRef '900872.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H52 Ce N6 O14, F6 P, 2(C2 H3 N)'
_chemical_formula_sum            'C48 H58 Ce F6 N8 O14 P'
_chemical_formula_weight         1256.11
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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 64 2 2'
_symmetry_space_group_name_Hall  'P 64 2C (0 0 -1)'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x-y, x, z+2/3'
'-y, x-y, z+1/3'
'-x, -y, z'
'-x+y, -x, z+2/3'
'y, -x+y, z+1/3'
'-y, -x, -z+1/3'
'x-y, -y, -z'
'x, x-y, -z+2/3'
'y, x, -z+1/3'
'-x+y, y, -z'
'-x, -x+y, -z+2/3'
_cell_length_a                   15.9742(3)
_cell_length_b                   15.9742(3)
_cell_length_c                   19.4383(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     4295.63(17)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3887
_cell_measurement_theta_min      2.9390
_cell_measurement_theta_max      28.9005
_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1923
_exptl_absorpt_coefficient_mu    0.909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8250
_exptl_absorpt_correction_T_max  0.8757
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11069
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.94
_diffrn_reflns_theta_max         26.99
_reflns_number_total             3114
_reflns_number_gt                2537
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0792P)^2^+0.3865P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    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   -0.03(3)
_refine_ls_number_reflns         3114
_refine_ls_number_parameters     197
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.1314
_refine_ls_wR_factor_gt          0.1210
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1726(4) 0.4274(4) 0.3214(3) 0.0540(13) Uani 1 1 d . . .
C2 C 0.1238(5) 0.3574(5) 0.2705(3) 0.0648(15) Uani 1 1 d . . .
C3 C 0.1633(6) 0.3063(5) 0.2422(4) 0.093(2) Uani 1 1 d . . .
H3 H 0.1312 0.2621 0.2071 0.112 Uiso 1 1 calc R . .
C4 C 0.2523(7) 0.3214(6) 0.2666(5) 0.107(3) Uani 1 1 d . . .
H4 H 0.2787 0.2865 0.2472 0.129 Uiso 1 1 calc R . .
C5 C 0.2999(6) 0.3836(6) 0.3164(4) 0.097(3) Uani 1 1 d . . .
H5 H 0.3581 0.3908 0.3321 0.116 Uiso 1 1 calc R . .
C6 C 0.2625(4) 0.4398(4) 0.3463(3) 0.0645(15) Uani 1 1 d . . .
C7 C 0.3172(4) 0.5112(4) 0.3968(2) 0.0558(13) Uani 1 1 d . . .
H7 H 0.3751 0.5162 0.4113 0.067 Uiso 1 1 calc R . .
C8 C 0.3539(4) 0.6509(4) 0.4674(2) 0.0560(12) Uani 1 1 d . . .
H8 H 0.4097 0.6455 0.4820 0.067 Uiso 1 1 calc R . .
C9 C 0.3898(5) 0.7436(4) 0.4270(3) 0.0746(19) Uani 1 1 d . . .
H9A H 0.4302 0.7438 0.3897 0.089 Uiso 1 1 calc R . .
H9B H 0.3346 0.7442 0.4068 0.089 Uiso 1 1 calc R . .
C10 C 0.4465(6) 0.8343(5) 0.4685(4) 0.094(2) Uani 1 1 d . . .
H10A H 0.4623 0.8901 0.4399 0.112 Uiso 1 1 calc R . .
H10B H 0.5065 0.8390 0.4837 0.112 Uiso 1 1 calc R . .
C11 C -0.0216(6) 0.2752(6) 0.2038(5) 0.115(3) Uani 1 1 d . . .
H11A H 0.0194 0.2687 0.1707 0.173 Uiso 1 1 calc R . .
H11B H -0.0636 0.2930 0.1807 0.173 Uiso 1 1 calc R . .
H11C H -0.0598 0.2148 0.2272 0.173 Uiso 1 1 calc R . .
C12 C 0.0990(8) 0.1979(17) 0.0000 0.187(7) Uani 1 2 d SU . .
H12A H 0.1261 0.1748 -0.0340 0.281 Uiso 0.50 1 calc PR . .
H12B H 0.0322 0.1748 -0.0105 0.281 Uiso 0.50 1 calc PR . .
H12C H 0.1039 0.1748 0.0445 0.281 Uiso 0.50 1 calc PR . .
C13 C 0.1496(11) 0.299(2) 0.0000 0.208(8) Uani 1 2 d SU . .
Ce1 Ce 0.0000 0.5000 0.3333 0.04667(19) Uani 1 4 d S . .
F1 F 0.0974(6) 0.0974(6) 0.1667 0.192(5) Uani 1 2 d S . .
F2 F 0.0507(9) -0.0507(9) 0.1667 0.320(18) Uani 1 2 d S . .
F3 F 0.051(2) -0.028(3) 0.107(3) 0.22(3) Uani 0.25 1 d P . .
F4 F 0.0000 0.0000 0.0869(13) 0.228(15) Uani 0.50 2 d SP . .
N1 N 0.2927(4) 0.5685(4) 0.4236(2) 0.0541(11) Uani 1 1 d . . .
N2 N 0.0000 0.5000 0.4927(3) 0.0675(17) Uani 1 2 d S . .
N3 N 0.1901(9) 0.3802(19) 0.0000 0.272(10) Uani 1 2 d SU . .
O1 O 0.1410(2) 0.4823(3) 0.34262(19) 0.0605(9) Uani 1 1 d . . .
O2 O 0.0370(3) 0.3489(3) 0.2531(2) 0.0803(13) Uani 1 1 d . . .
O3 O -0.0765(3) 0.4700(4) 0.4600(2) 0.0755(12) Uani 1 1 d . . .
O4 O 0.0000 0.5000 0.5559(3) 0.113(2) Uani 1 2 d SU . .
P1 P 0.0000 0.0000 0.1667 0.1284(18) Uani 1 4 d S . .
H101 H 0.245(4) 0.556(4) 0.415(3) 0.040(16) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.054(3) 0.053(3) 0.064(3) -0.001(3) 0.001(3) 0.034(2)
C2 0.066(4) 0.065(4) 0.074(3) -0.021(3) -0.014(3) 0.040(3)
C3 0.126(8) 0.085(4) 0.096(5) -0.031(4) -0.028(5) 0.073(6)
C4 0.123(7) 0.114(6) 0.136(7) -0.068(6) -0.045(6) 0.098(6)
C5 0.100(5) 0.122(7) 0.112(6) -0.024(5) -0.026(5) 0.087(5)
C6 0.069(3) 0.069(3) 0.074(4) 0.000(3) -0.003(3) 0.049(3)
C7 0.063(3) 0.071(4) 0.049(3) 0.003(3) -0.005(2) 0.046(3)
C8 0.048(3) 0.068(3) 0.048(2) -0.003(3) -0.012(2) 0.026(2)
C9 0.085(5) 0.076(4) 0.046(3) 0.007(3) -0.002(3) 0.028(4)
C10 0.096(6) 0.061(4) 0.098(5) 0.008(3) -0.009(4) 0.020(4)
C11 0.103(7) 0.105(6) 0.140(7) -0.054(5) -0.051(6) 0.053(5)
C12 0.201(10) 0.173(10) 0.180(10) 0.000 -0.028(9) 0.086(5)
C13 0.205(11) 0.205(11) 0.213(12) 0.000 -0.041(9) 0.102(5)
Ce1 0.0299(3) 0.0516(3) 0.0512(3) 0.000 0.000 0.01494(13)
F1 0.144(5) 0.144(5) 0.230(11) -0.043(5) 0.043(5) 0.029(7)
F2 0.33(3) 0.33(3) 0.40(3) 0.12(2) 0.12(2) 0.24(3)
F3 0.062(12) 0.23(5) 0.34(6) -0.23(5) -0.03(2) 0.059(18)
F4 0.28(4) 0.133(18) 0.142(17) 0.000 0.000 0.01(3)
N1 0.048(3) 0.072(3) 0.046(2) -0.001(2) -0.005(2) 0.033(3)
N2 0.056(3) 0.124(5) 0.045(3) 0.000 0.000 0.061(4)
N3 0.259(12) 0.249(12) 0.304(14) 0.000 -0.044(9) 0.125(6)
O1 0.0507(18) 0.064(2) 0.075(2) -0.016(2) -0.0059(18) 0.0345(18)
O2 0.070(3) 0.079(3) 0.098(3) -0.035(2) -0.027(2) 0.041(2)
O3 0.0470(19) 0.120(4) 0.065(2) 0.016(2) 0.0010(17) 0.046(2)
O4 0.091(4) 0.213(8) 0.069(3) 0.000 0.000 0.101(5)
P1 0.095(2) 0.095(2) 0.199(6) 0.000 0.000 0.050(3)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.281(6) . ?
C1 C2 1.400(8) . ?
C1 C6 1.431(7) . ?
C2 O2 1.367(7) . ?
C2 C3 1.372(9) . ?
C3 C4 1.401(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.322(10) . ?
C4 H4 0.9300 . ?
C5 C6 1.428(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.425(8) . ?
C7 N1 1.274(7) . ?
C7 H7 0.9300 . ?
C8 N1 1.458(7) . ?
C8 C9 1.512(8) . ?
C8 C8 1.560(10) 11_556 ?
C8 H8 0.9800 . ?
C9 C10 1.502(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C10 1.543(16) 11_556 ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 O2 1.441(8) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.40(3) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 N3 1.12(3) . ?
Ce1 O1 2.412(3) 9_565 ?
Ce1 O1 2.412(3) 12 ?
Ce1 O1 2.412(3) 4_565 ?
Ce1 O1 2.412(3) . ?
Ce1 O3 2.682(4) 9_565 ?
Ce1 O3 2.682(4) 12 ?
Ce1 O3 2.682(4) 4_565 ?
Ce1 O3 2.682(4) . ?
F1 P1 1.556(9) . ?
F2 F3 1.21(6) 7 ?
F2 F3 1.21(6) . ?
F2 P1 1.40(2) . ?
F3 F4 1.17(5) . ?
F3 P1 1.60(3) . ?
F4 F3 1.17(5) 4 ?
F4 P1 1.55(2) . ?
N1 H101 0.71(5) . ?
N2 O4 1.229(8) . ?
N2 O3 1.242(5) . ?
N2 O3 1.242(5) 4_565 ?
P1 F2 1.40(2) 4 ?
P1 F4 1.55(2) 7 ?
P1 F1 1.556(9) 4 ?
P1 F3 1.60(3) 10 ?
P1 F3 1.60(3) 7 ?
P1 F3 1.60(3) 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
O1 C1 C2 121.4(5) . . ?
O1 C1 C6 120.5(5) . . ?
C2 C1 C6 118.0(5) . . ?
O2 C2 C3 125.9(6) . . ?
O2 C2 C1 112.7(5) . . ?
C3 C2 C1 121.4(6) . . ?
C2 C3 C4 119.3(6) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 122.0(6) . . ?
C5 C4 H4 119.0 . . ?
C3 C4 H4 119.0 . . ?
C4 C5 C6 120.5(6) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C7 C6 C5 120.1(5) . . ?
C7 C6 C1 121.1(5) . . ?
C5 C6 C1 118.7(6) . . ?
N1 C7 C6 124.7(5) . . ?
N1 C7 H7 117.6 . . ?
C6 C7 H7 117.6 . . ?
N1 C8 C9 109.6(4) . . ?
N1 C8 C8 110.3(4) . 11_556 ?
C9 C8 C8 111.0(4) . 11_556 ?
N1 C8 H8 108.6 . . ?
C9 C8 H8 108.6 . . ?
C8 C8 H8 108.6 11_556 . ?
C10 C9 C8 114.7(5) . . ?
C10 C9 H9A 108.6 . . ?
C8 C9 H9A 108.6 . . ?
C10 C9 H9B 108.6 . . ?
C8 C9 H9B 108.6 . . ?
H9A C9 H9B 107.6 . . ?
C9 C10 C10 110.7(6) . 11_556 ?
C9 C10 H10A 109.5 . . ?
C10 C10 H10A 109.5 11_556 . ?
C9 C10 H10B 109.5 . . ?
C10 C10 H10B 109.5 11_556 . ?
H10A C10 H10B 108.1 . . ?
O2 C11 H11A 109.5 . . ?
O2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C13 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C13 C12 180.000(3) . . ?
O1 Ce1 O1 171.42(18) 9_565 12 ?
O1 Ce1 O1 108.57(17) 9_565 4_565 ?
O1 Ce1 O1 72.11(17) 12 4_565 ?
O1 Ce1 O1 72.11(17) 9_565 . ?
O1 Ce1 O1 108.57(17) 12 . ?
O1 Ce1 O1 171.42(18) 4_565 . ?
O1 Ce1 O3 106.19(12) 9_565 9_565 ?
O1 Ce1 O3 65.40(11) 12 9_565 ?
O1 Ce1 O3 77.19(13) 4_565 9_565 ?
O1 Ce1 O3 111.04(13) . 9_565 ?
O1 Ce1 O3 65.40(11) 9_565 12 ?
O1 Ce1 O3 106.19(12) 12 12 ?
O1 Ce1 O3 111.04(13) 4_565 12 ?
O1 Ce1 O3 77.19(13) . 12 ?
O3 Ce1 O3 46.85(15) 9_565 12 ?
O1 Ce1 O3 77.19(13) 9_565 4_565 ?
O1 Ce1 O3 111.04(14) 12 4_565 ?
O1 Ce1 O3 106.19(12) 4_565 4_565 ?
O1 Ce1 O3 65.40(11) . 4_565 ?
O3 Ce1 O3 174.4(2) 9_565 4_565 ?
O3 Ce1 O3 133.53(16) 12 4_565 ?
O1 Ce1 O3 111.04(14) 9_565 . ?
O1 Ce1 O3 77.19(13) 12 . ?
O1 Ce1 O3 65.40(11) 4_565 . ?
O1 Ce1 O3 106.19(12) . . ?
O3 Ce1 O3 133.53(16) 9_565 . ?
O3 Ce1 O3 174.4(2) 12 . ?
O3 Ce1 O3 46.85(15) 4_565 . ?
F3 F2 F3 150(4) 7 . ?
F3 F2 P1 75.1(19) 7 . ?
F3 F2 P1 75.1(19) . . ?
F4 F3 F2 122(3) . . ?
F4 F3 P1 65.9(16) . . ?
F2 F3 P1 57.9(16) . . ?
F3 F4 F3 141(5) . 4 ?
F3 F4 P1 70(3) . . ?
F3 F4 P1 70(3) 4 . ?
C7 N1 C8 125.4(5) . . ?
C7 N1 H101 112(5) . . ?
C8 N1 H101 122(5) . . ?
O4 N2 O3 120.8(3) . . ?
O4 N2 O3 120.8(3) . 4_565 ?
O3 N2 O3 118.4(5) . 4_565 ?
C1 O1 Ce1 140.1(3) . . ?
C2 O2 C11 117.3(5) . . ?
N2 O3 Ce1 97.4(3) . . ?
F2 P1 F2 180.000(3) . 4 ?
F2 P1 F4 90.0 . 7 ?
F2 P1 F4 90.0 4 7 ?
F2 P1 F4 90.0 . . ?
F2 P1 F4 90.0 4 . ?
F4 P1 F4 180.000(1) 7 . ?
F2 P1 F1 90.000(1) . . ?
F2 P1 F1 90.000(1) 4 . ?
F4 P1 F1 90.000(1) 7 . ?
F4 P1 F1 90.000(1) . . ?
F2 P1 F1 90.000(1) . 4 ?
F2 P1 F1 90.000(1) 4 4 ?
F4 P1 F1 90.000(1) 7 4 ?
F4 P1 F1 90.000(1) . 4 ?
F1 P1 F1 180.0(12) . 4 ?
F2 P1 F3 133(2) . 10 ?
F2 P1 F3 47(2) 4 10 ?
F4 P1 F3 44(2) 7 10 ?
F4 P1 F3 136(2) . 10 ?
F1 P1 F3 83.3(14) . 10 ?
F1 P1 F3 96.7(14) 4 10 ?
F2 P1 F3 47(2) . 7 ?
F2 P1 F3 133(2) 4 7 ?
F4 P1 F3 44(2) 7 7 ?
F4 P1 F3 136(2) . 7 ?
F1 P1 F3 96.7(14) . 7 ?
F1 P1 F3 83.3(14) 4 7 ?
F3 P1 F3 88(4) 10 7 ?
F2 P1 F3 47(2) . . ?
F2 P1 F3 133(2) 4 . ?
F4 P1 F3 136(2) 7 . ?
F4 P1 F3 44(2) . . ?
F1 P1 F3 83.3(14) . . ?
F1 P1 F3 96.7(14) 4 . ?
F3 P1 F3 167(3) 10 . ?
F3 P1 F3 94(4) 7 . ?
F2 P1 F3 133(2) . 4 ?
F2 P1 F3 47(2) 4 4 ?
F4 P1 F3 136(2) 7 4 ?
F4 P1 F3 44(2) . 4 ?
F1 P1 F3 96.7(14) . 4 ?
F1 P1 F3 83.3(14) 4 4 ?
F3 P1 F3 94(4) 10 4 ?
F3 P1 F3 167(3) 7 4 ?
F3 P1 F3 88(4) . 4 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 O2 -6.5(9) . . . . ?
C6 C1 C2 O2 177.1(6) . . . . ?
O1 C1 C2 C3 172.4(6) . . . . ?
C6 C1 C2 C3 -4.0(10) . . . . ?
O2 C2 C3 C4 -178.5(8) . . . . ?
C1 C2 C3 C4 2.8(12) . . . . ?
C2 C3 C4 C5 0.0(15) . . . . ?
C3 C4 C5 C6 -1.4(15) . . . . ?
C4 C5 C6 C7 -175.9(8) . . . . ?
C4 C5 C6 C1 0.1(12) . . . . ?
O1 C1 C6 C7 2.1(9) . . . . ?
C2 C1 C6 C7 178.5(6) . . . . ?
O1 C1 C6 C5 -173.9(6) . . . . ?
C2 C1 C6 C5 2.5(10) . . . . ?
C5 C6 C7 N1 175.9(6) . . . . ?
C1 C6 C7 N1 -0.1(9) . . . . ?
N1 C8 C9 C10 174.7(6) . . . . ?
C8 C8 C9 C10 52.6(8) 11_556 . . . ?
C8 C9 C10 C10 -54.6(10) . . . 11_556 ?
F3 F2 F3 F4 -14(3) 7 . . . ?
P1 F2 F3 F4 -14(3) . . . . ?
F3 F2 F3 P1 0.000(5) 7 . . . ?
F2 F3 F4 F3 13(3) . . . 4 ?
P1 F3 F4 F3 0.000(6) . . . 4 ?
F2 F3 F4 P1 13(3) . . . . ?
C6 C7 N1 C8 -170.4(5) . . . . ?
C9 C8 N1 C7 104.7(6) . . . . ?
C8 C8 N1 C7 -132.8(6) 11_556 . . . ?
C2 C1 O1 Ce1 9.6(9) . . . . ?
C6 C1 O1 Ce1 -174.1(4) . . . . ?
O1 Ce1 O1 C1 -137.6(6) 9_565 . . . ?
O1 Ce1 O1 C1 33.4(5) 12 . . . ?
O1 Ce1 O1 C1 126.4(5) 4_565 . . . ?
O3 Ce1 O1 C1 -36.7(6) 9_565 . . . ?
O3 Ce1 O1 C1 -69.7(5) 12 . . . ?
O3 Ce1 O1 C1 138.6(6) 4_565 . . . ?
O3 Ce1 O1 C1 115.0(5) . . . . ?
C3 C2 O2 C11 4.4(11) . . . . ?
C1 C2 O2 C11 -176.7(6) . . . . ?
O4 N2 O3 Ce1 180.0 . . . . ?
O3 N2 O3 Ce1 0.0 4_565 . . . ?
O1 Ce1 O3 N2 -46.7(3) 9_565 . . . ?
O1 Ce1 O3 N2 135.9(3) 12 . . . ?
O1 Ce1 O3 N2 -148.2(3) 4_565 . . . ?
O1 Ce1 O3 N2 30.0(3) . . . . ?
O3 Ce1 O3 N2 172.3(3) 9_565 . . . ?
O3 Ce1 O3 N2 -96.5(2) 12 . . . ?
O3 Ce1 O3 N2 0.0 4_565 . . . ?
F3 F2 P1 F2 176.9(17) 7 . . 4 ?
F3 F2 P1 F2 -3.1(17) . . . 4 ?
F3 F2 P1 F4 9.1(17) 7 . . 7 ?
F3 F2 P1 F4 -170.9(17) . . . 7 ?
F3 F2 P1 F4 -170.9(17) 7 . . . ?
F3 F2 P1 F4 9.1(17) . . . . ?
F3 F2 P1 F1 99.1(17) 7 . . . ?
F3 F2 P1 F1 -80.9(17) . . . . ?
F3 F2 P1 F1 -80.9(17) 7 . . 4 ?
F3 F2 P1 F1 99.1(17) . . . 4 ?
F3 F2 P1 F3 18(3) 7 . . 10 ?
F3 F2 P1 F3 -162(3) . . . 10 ?
F3 F2 P1 F3 180.000(7) . . . 7 ?
F3 F2 P1 F3 180.000(3) 7 . . . ?
F3 F2 P1 F3 -162(3) 7 . . 4 ?
F3 F2 P1 F3 18(3) . . . 4 ?
F3 F4 P1 F2 -10(2) . . . . ?
F3 F4 P1 F2 170(2) 4 . . . ?
F3 F4 P1 F2 170(2) . . . 4 ?
F3 F4 P1 F2 -10(2) 4 . . 4 ?
F3 F4 P1 F4 0(100) . . . 7 ?
F3 F4 P1 F4 0(100) 4 . . 7 ?
F3 F4 P1 F1 80(2) . . . . ?
F3 F4 P1 F1 -100(2) 4 . . . ?
F3 F4 P1 F1 -100(2) . . . 4 ?
F3 F4 P1 F1 80(2) 4 . . 4 ?
F3 F4 P1 F3 161(5) . . . 10 ?
F3 F4 P1 F3 -19(5) 4 . . 10 ?
F3 F4 P1 F3 -19(5) . . . 7 ?
F3 F4 P1 F3 161(5) 4 . . 7 ?
F3 F4 P1 F3 180.000(2) 4 . . . ?
F3 F4 P1 F3 180.000(2) . . . 4 ?
F4 F3 P1 F2 167(3) . . . . ?
F4 F3 P1 F2 -13(3) . . . 4 ?
F2 F3 P1 F2 180.000(5) . . . 4 ?
F4 F3 P1 F4 180.000(3) . . . 7 ?
F2 F3 P1 F4 13(3) . . . 7 ?
F2 F3 P1 F4 -167(3) . . . . ?
F4 F3 P1 F1 -97.0(18) . . . . ?
F2 F3 P1 F1 96.2(11) . . . . ?
F4 F3 P1 F1 83.0(18) . . . 4 ?
F2 F3 P1 F1 -83.8(11) . . . 4 ?
F4 F3 P1 F3 -97.0(18) . . . 10 ?
F2 F3 P1 F3 96.2(11) . . . 10 ?
F4 F3 P1 F3 167(3) . . . 7 ?
F2 F3 P1 F3 0.000(1) . . . 7 ?
F4 F3 P1 F3 0.000(5) . . . 4 ?
F2 F3 P1 F3 -167(3) . . . 4 ?
_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        26.99
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.078


data_c
_database_code_depnum_ccdc_archive 'CCDC 900873'
#TrackingRef '900873.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H30 Ce N5 O14'
_chemical_formula_sum            'C23 H30 Ce N5 O14'
_chemical_formula_weight         740.64
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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a                   29.134(6)
_cell_length_b                   14.254(3)
_cell_length_c                   14.244(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.10(3)
_cell_angle_gamma                90.00
_cell_volume                     5737(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    13927
_cell_measurement_theta_min      3.20
_cell_measurement_theta_max      27.49
_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2984
_exptl_absorpt_coefficient_mu    1.664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7109
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       '\w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            20095
_diffrn_reflns_av_R_equivalents  0.0836
_diffrn_reflns_av_sigmaI/netI    0.0750
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.20
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4993
_reflns_number_gt                3506
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'RAPID-AUTO (Rigaku 1998 <i>RAPID-AUTO</i>)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku 1998 <i>RAPID-AUTO</i>)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXL-97
_refine_special_details          
;
acta 52
omit -14 2 4
omit 8 2 4
omit -6 0 4
omit -6 0 2
omit 0 2 6
omit -14 0 4
omit -10 0 4
omit 3 1 1
omit 0 0 6
omit -6 6 2
omit -5 11 4
omit 7 3 4
omit 1 5 2
omit 8 0 4
omit 7 3 1
omit 7 1 4
omit -1 1 4
omit -18 0 4
omit -14 4 4
omit 16 4 4
omit 4 0 4
omit -3 50
twin 1 0 1 0 -1 0 0 0 -1
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1042P)^2^+151.2850P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4993
_refine_ls_number_parameters     396
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1183
_refine_ls_R_factor_gt           0.0838
_refine_ls_wR_factor_ref         0.2347
_refine_ls_wR_factor_gt          0.2104
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.11532(3) 0.22949(5) 0.21375(6) 0.0417(3) Uani 1 1 d . . .
O13 O 0.0387(6) -0.0245(10) 0.1589(12) 0.113(5) Uani 1 1 d . . .
C1 C 0.0363(6) 0.1751(15) -0.0393(13) 0.078(5) Uani 1 1 d . . .
H1A H 0.0360 0.1542 -0.1035 0.117 Uiso 1 1 calc R . .
H1B H 0.0231 0.2371 -0.0422 0.117 Uiso 1 1 calc R . .
H1C H 0.0178 0.1330 -0.0109 0.117 Uiso 1 1 calc R . .
C18 C 0.2094(5) 0.0876(11) 0.6099(9) 0.052(4) Uani 1 1 d . . .
H18A H 0.2137 0.0694 0.6742 0.062 Uiso 1 1 calc R . .
C9 C 0.3079(6) 0.1170(12) 0.2157(12) 0.066(4) Uani 1 1 d . . .
H9A H 0.3067 0.0527 0.2393 0.079 Uiso 1 1 calc R . .
O14 O 0.0761(6) 0.4217(12) 0.4190(10) 0.105(5) Uani 1 1 d . . .
C5 C 0.1964(6) 0.1083(12) -0.1043(10) 0.061(4) Uani 1 1 d . . .
H5A H 0.2217 0.0939 -0.1309 0.073 Uiso 1 1 calc R . .
C13 C 0.3654(5) 0.1635(13) 0.3704(10) 0.057(4) Uani 1 1 d . . .
H13A H 0.3704 0.2075 0.4238 0.069 Uiso 1 1 calc R . .
H13B H 0.3661 0.1006 0.3966 0.069 Uiso 1 1 calc R . .
C14 C 0.3160(5) 0.1822(13) 0.3000(11) 0.061(4) Uani 1 1 d . . .
H14A H 0.3159 0.2465 0.2756 0.073 Uiso 1 1 calc R . .
C4 C 0.1506(6) 0.1052(11) -0.1601(11) 0.065(4) Uani 1 1 d . . .
H4A H 0.1447 0.0878 -0.2249 0.078 Uiso 1 1 calc R . .
C22 C 0.0697(5) 0.1166(13) 0.4275(13) 0.067(5) Uani 1 1 d . . .
H22A H 0.0788 0.0878 0.4902 0.100 Uiso 1 1 calc R . .
H22B H 0.0506 0.0737 0.3824 0.100 Uiso 1 1 calc R . .
H22C H 0.0518 0.1725 0.4313 0.100 Uiso 1 1 calc R . .
O12 O 0.1904(5) 0.4471(8) 0.0998(9) 0.076(3) Uani 1 1 d . . .
C19 C 0.1634(5) 0.0962(10) 0.5512(10) 0.050(3) Uani 1 1 d . . .
H19A H 0.1376 0.0803 0.5759 0.060 Uiso 1 1 calc R . .
C6 C 0.2042(5) 0.1341(9) -0.0054(10) 0.048(3) Uani 1 1 d . . .
N4 N 0.0616(6) 0.0473(10) 0.1778(10) 0.066(4) Uani 1 1 d . . .
N5 N 0.0846(6) 0.3620(10) 0.3633(10) 0.066(4) Uani 1 1 d . . .
C15 C 0.2806(5) 0.1439(9) 0.4360(9) 0.044(3) Uani 1 1 d . . .
H15A H 0.3104 0.1296 0.4749 0.053 Uiso 1 1 calc R . .
C7 C 0.1652(5) 0.1547(10) 0.0358(10) 0.048(3) Uani 1 1 d . . .
C12 C 0.4054(7) 0.1741(17) 0.3174(14) 0.086(6) Uani 1 1 d . . .
H12A H 0.4062 0.2381 0.2947 0.103 Uiso 1 1 calc R . .
H12B H 0.4356 0.1606 0.3617 0.103 Uiso 1 1 calc R . .
C3 C 0.1132(5) 0.1279(9) -0.1199(10) 0.049(3) Uani 1 1 d . . .
H3A H 0.0827 0.1269 -0.1593 0.059 Uiso 1 1 calc R . .
C8 C 0.2504(5) 0.1267(10) 0.0552(11) 0.053(4) Uani 1 1 d . . .
H8A H 0.2747 0.1118 0.0258 0.063 Uiso 1 1 calc R . .
C17 C 0.2479(5) 0.1053(10) 0.5745(9) 0.046(3) Uani 1 1 d . . .
H17A H 0.2784 0.0999 0.6137 0.055 Uiso 1 1 calc R . .
C20 C 0.1560(5) 0.1274(9) 0.4587(10) 0.043(3) Uani 1 1 d . . .
C2 C 0.1193(6) 0.1511(10) -0.0266(10) 0.050(3) Uani 1 1 d . . .
C11 C 0.3972(7) 0.1082(18) 0.2336(16) 0.094(7) Uani 1 1 d . . .
H11A H 0.3986 0.0443 0.2574 0.113 Uiso 1 1 calc R . .
H11B H 0.4224 0.1159 0.2005 0.113 Uiso 1 1 calc R . .
C16 C 0.2402(4) 0.1326(9) 0.4756(9) 0.039(3) Uani 1 1 d . . .
C21 C 0.1946(5) 0.1472(9) 0.4175(9) 0.041(3) Uani 1 1 d . . .
C10 C 0.3496(5) 0.1239(13) 0.1612(11) 0.064(4) Uani 1 1 d . . .
H10A H 0.3450 0.0770 0.1104 0.077 Uiso 1 1 calc R . .
H10B H 0.3492 0.1853 0.1316 0.077 Uiso 1 1 calc R . .
N3 N 0.1707(5) 0.3893(9) 0.1383(9) 0.055(3) Uani 1 1 d . . .
C23 C 0.0321(8) 0.4067(17) 0.0576(17) 0.116(9) Uani 1 1 d . . .
H23A H -0.0006 0.4246 0.0433 0.174 Uiso 1 1 calc R . .
H23B H 0.0403 0.3884 -0.0011 0.174 Uiso 1 1 calc R . .
H23C H 0.0514 0.4587 0.0861 0.174 Uiso 1 1 calc R . .
N1 N 0.2777(4) 0.1734(10) 0.3472(9) 0.056(3) Uani 1 1 d D . .
H111 H 0.250(3) 0.201(11) 0.320(12) 0.084 Uiso 1 1 d D . .
N2 N 0.2618(4) 0.1388(10) 0.1478(9) 0.058(3) Uani 1 1 d D . .
H21 H 0.234(3) 0.165(12) 0.150(13) 0.088 Uiso 1 1 d D . .
O1 O 0.1892(5) 0.3548(10) 0.2183(9) 0.088(4) Uani 1 1 d . . .
O2 O 0.1055(4) 0.0503(8) 0.1890(9) 0.070(3) Uani 1 1 d . . .
O3 O 0.1249(4) 0.3580(8) 0.3438(9) 0.075(3) Uani 1 1 d . . .
O4 O 0.0534(4) 0.3047(9) 0.3216(8) 0.066(3) Uani 1 1 d . . .
O5 O 0.0418(3) 0.1265(8) 0.1880(8) 0.060(3) Uani 1 1 d . . .
O6 O 0.0842(3) 0.1765(8) 0.0186(7) 0.060(3) Uani 1 1 d . . .
O7 O 0.1865(3) 0.1788(7) 0.3292(6) 0.049(2) Uani 1 1 d . . .
O8 O 0.1717(3) 0.1738(8) 0.1264(7) 0.056(3) Uani 1 1 d . . .
O9 O 0.1126(3) 0.1412(7) 0.3945(6) 0.051(2) Uani 1 1 d . . .
O10 O 0.1311(5) 0.3576(10) 0.0945(10) 0.087(4) Uani 1 1 d . . .
O11 O 0.0401(4) 0.3268(8) 0.1261(8) 0.065(3) Uani 1 1 d . . .
H11 H 0.0127 0.3001 0.1454 0.05(4) Uiso 1 1 d R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ce1 0.0339(4) 0.0480(4) 0.0402(4) 0.0018(4) 0.0032(3) 0.0004(4)
O13 0.118(13) 0.077(9) 0.128(13) -0.019(9) -0.002(10) -0.054(9)
C1 0.042(10) 0.112(16) 0.072(11) -0.024(11) -0.002(8) -0.006(9)
C18 0.066(10) 0.061(9) 0.028(6) 0.003(6) 0.011(7) -0.001(7)
C9 0.069(11) 0.067(11) 0.063(10) -0.001(8) 0.020(9) 0.002(8)
O14 0.107(12) 0.124(12) 0.088(10) -0.051(9) 0.029(8) 0.008(9)
C5 0.066(11) 0.076(11) 0.041(8) -0.005(8) 0.017(8) 0.006(8)
C13 0.037(8) 0.087(12) 0.043(7) -0.002(8) 0.001(6) -0.002(7)
C14 0.042(9) 0.088(12) 0.052(9) 0.001(9) 0.009(7) 0.000(8)
C4 0.084(13) 0.065(10) 0.043(8) -0.005(8) 0.008(8) -0.022(9)
C22 0.045(9) 0.081(12) 0.081(11) -0.002(9) 0.028(8) -0.012(8)
O12 0.093(9) 0.063(7) 0.087(8) -0.005(6) 0.051(7) -0.018(7)
C19 0.045(8) 0.057(8) 0.055(8) 0.000(7) 0.027(7) -0.008(7)
C6 0.061(9) 0.040(7) 0.043(7) -0.004(6) 0.015(7) -0.001(6)
N4 0.077(11) 0.060(9) 0.052(8) 0.002(7) -0.001(7) -0.013(8)
N5 0.073(10) 0.068(9) 0.055(8) -0.006(7) 0.008(7) 0.004(8)
C15 0.044(8) 0.049(8) 0.034(7) 0.002(6) -0.002(6) 0.004(6)
C7 0.061(9) 0.042(7) 0.039(7) 0.001(6) 0.008(7) 0.001(6)
C12 0.053(11) 0.126(18) 0.075(12) 0.013(12) 0.009(9) 0.000(11)
C3 0.046(8) 0.047(8) 0.048(8) 0.008(6) 0.000(7) -0.010(6)
C8 0.043(8) 0.059(9) 0.060(9) -0.009(7) 0.020(7) -0.002(7)
C17 0.041(8) 0.056(8) 0.035(7) 0.000(6) -0.001(6) -0.007(6)
C20 0.038(7) 0.045(7) 0.046(7) -0.003(6) 0.013(6) 0.002(6)
C2 0.058(9) 0.049(8) 0.044(8) 0.000(6) 0.012(7) -0.013(7)
C11 0.051(11) 0.14(2) 0.095(15) -0.001(14) 0.027(11) 0.013(12)
C16 0.040(7) 0.044(7) 0.031(6) 0.001(6) 0.004(5) 0.003(6)
C21 0.040(7) 0.041(7) 0.039(7) -0.003(6) 0.003(6) -0.002(6)
C10 0.048(9) 0.092(13) 0.054(9) -0.003(9) 0.017(7) 0.002(8)
N3 0.054(8) 0.063(8) 0.051(7) -0.005(6) 0.020(6) -0.010(6)
C23 0.101(17) 0.117(18) 0.105(17) 0.059(15) -0.024(14) 0.013(14)
N1 0.032(7) 0.086(10) 0.051(7) 0.009(7) 0.011(5) 0.007(6)
N2 0.037(7) 0.093(10) 0.044(7) -0.012(7) 0.008(6) 0.008(6)
O1 0.110(11) 0.091(9) 0.056(7) -0.003(7) 0.008(7) -0.038(8)
O2 0.065(8) 0.063(7) 0.083(8) -0.005(6) 0.020(6) 0.003(6)
O3 0.063(8) 0.074(8) 0.088(9) -0.028(7) 0.018(7) -0.011(6)
O4 0.053(7) 0.074(7) 0.069(7) -0.001(6) 0.010(5) -0.002(6)
O5 0.043(6) 0.060(7) 0.072(7) 0.001(6) 0.005(5) -0.013(5)
O6 0.038(6) 0.076(7) 0.058(6) 0.000(5) -0.003(5) -0.005(5)
O7 0.042(5) 0.065(6) 0.041(5) 0.017(5) 0.009(4) 0.007(5)
O8 0.044(6) 0.088(8) 0.038(5) -0.014(5) 0.011(4) -0.002(5)
O9 0.025(5) 0.078(7) 0.047(5) 0.005(5) 0.003(4) -0.005(4)
O10 0.062(8) 0.095(10) 0.098(10) 0.017(8) 0.005(7) -0.009(7)
O11 0.044(6) 0.080(8) 0.067(7) 0.020(6) 0.009(5) 0.011(5)
_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 O7 2.422(9) . ?
Ce1 O8 2.423(9) . ?
Ce1 O5 2.548(9) . ?
Ce1 O3 2.572(11) . ?
Ce1 O2 2.584(11) . ?
Ce1 O10 2.610(13) . ?
Ce1 O11 2.637(10) . ?
Ce1 O1 2.786(13) . ?
Ce1 O6 2.809(10) . ?
Ce1 O4 2.848(11) . ?
Ce1 O9 2.884(9) . ?
Ce1 N4 3.010(14) . ?
O13 N4 1.216(17) . ?
C1 O6 1.438(17) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C18 C17 1.361(19) . ?
C18 C19 1.40(2) . ?
C18 H18A 0.9300 . ?
C9 N2 1.48(2) . ?
C9 C14 1.49(2) . ?
C9 C10 1.60(2) . ?
C9 H9A 0.9800 . ?
O14 N5 1.229(18) . ?
C5 C4 1.38(2) . ?
C5 C6 1.420(19) . ?
C5 H5A 0.9300 . ?
C13 C12 1.54(2) . ?
C13 C14 1.56(2) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 N1 1.444(18) . ?
C14 H14A 0.9800 . ?
C4 C3 1.39(2) . ?
C4 H4A 0.9300 . ?
C22 O9 1.482(16) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
O12 N3 1.208(15) . ?
C19 C20 1.359(19) . ?
C19 H19A 0.9300 . ?
C6 C8 1.42(2) . ?
C6 C7 1.43(2) . ?
N4 O2 1.251(17) . ?
N4 O5 1.291(17) . ?
N5 O4 1.257(17) . ?
N5 O3 1.272(17) . ?
C15 N1 1.315(17) . ?
C15 C16 1.433(18) . ?
C15 H15A 0.9300 . ?
C7 O8 1.288(16) . ?
C7 C2 1.42(2) . ?
C12 C11 1.49(3) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C3 C2 1.338(19) . ?
C3 H3A 0.9300 . ?
C8 N2 1.291(19) . ?
C8 H8A 0.9300 . ?
C17 C16 1.426(18) . ?
C17 H17A 0.9300 . ?
C20 O9 1.382(16) . ?
C20 C21 1.417(18) . ?
C2 O6 1.382(18) . ?
C11 C10 1.53(2) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C16 C21 1.400(18) . ?
C21 O7 1.302(15) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
N3 O1 1.238(17) . ?
N3 O10 1.255(17) . ?
C23 O11 1.48(2) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
N1 H111 0.900(10) . ?
N2 H21 0.900(10) . ?
O11 H11 0.9815 . ?
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
O7 Ce1 O8 71.1(3) . . ?
O7 Ce1 O5 118.4(3) . . ?
O8 Ce1 O5 112.9(4) . . ?
O7 Ce1 O3 78.4(4) . . ?
O8 Ce1 O3 129.4(4) . . ?
O5 Ce1 O3 117.0(4) . . ?
O7 Ce1 O2 81.1(4) . . ?
O8 Ce1 O2 70.9(4) . . ?
O5 Ce1 O2 49.5(4) . . ?
O3 Ce1 O2 142.3(4) . . ?
O7 Ce1 O10 113.2(4) . . ?
O8 Ce1 O10 69.3(4) . . ?
O5 Ce1 O10 125.8(4) . . ?
O3 Ce1 O10 88.0(4) . . ?
O2 Ce1 O10 129.3(4) . . ?
O7 Ce1 O11 162.5(4) . . ?
O8 Ce1 O11 121.2(3) . . ?
O5 Ce1 O11 70.3(4) . . ?
O3 Ce1 O11 84.1(4) . . ?
O2 Ce1 O11 113.8(4) . . ?
O10 Ce1 O11 65.3(4) . . ?
O7 Ce1 O1 69.3(4) . . ?
O8 Ce1 O1 66.8(4) . . ?
O5 Ce1 O1 172.0(4) . . ?
O3 Ce1 O1 65.1(4) . . ?
O2 Ce1 O1 134.1(4) . . ?
O10 Ce1 O1 46.3(4) . . ?
O11 Ce1 O1 102.8(4) . . ?
O7 Ce1 O6 127.5(3) . . ?
O8 Ce1 O6 60.0(3) . . ?
O5 Ce1 O6 69.2(3) . . ?
O3 Ce1 O6 148.9(4) . . ?
O2 Ce1 O6 66.5(4) . . ?
O10 Ce1 O6 67.0(4) . . ?
O11 Ce1 O6 69.0(3) . . ?
O1 Ce1 O6 104.9(3) . . ?
O7 Ce1 O4 107.2(3) . . ?
O8 Ce1 O4 176.2(3) . . ?
O5 Ce1 O4 71.0(4) . . ?
O3 Ce1 O4 46.8(4) . . ?
O2 Ce1 O4 112.5(4) . . ?
O10 Ce1 O4 108.8(4) . . ?
O11 Ce1 O4 59.7(3) . . ?
O1 Ce1 O4 109.5(4) . . ?
O6 Ce1 O4 122.7(3) . . ?
O7 Ce1 O9 57.9(3) . . ?
O8 Ce1 O9 119.0(3) . . ?
O5 Ce1 O9 70.9(3) . . ?
O3 Ce1 O9 71.9(4) . . ?
O2 Ce1 O9 70.4(3) . . ?
O10 Ce1 O9 159.0(4) . . ?
O11 Ce1 O9 116.9(3) . . ?
O1 Ce1 O9 116.6(3) . . ?
O6 Ce1 O9 133.9(3) . . ?
O4 Ce1 O9 61.6(3) . . ?
O7 Ce1 N4 100.5(4) . . ?
O8 Ce1 N4 91.1(4) . . ?
O5 Ce1 N4 25.1(4) . . ?
O3 Ce1 N4 134.2(4) . . ?
O2 Ce1 N4 24.3(4) . . ?
O10 Ce1 N4 131.3(4) . . ?
O11 Ce1 N4 92.0(4) . . ?
O1 Ce1 N4 157.5(5) . . ?
O6 Ce1 N4 64.6(3) . . ?
O4 Ce1 N4 92.6(4) . . ?
O9 Ce1 N4 69.5(3) . . ?
O6 C1 H1A 109.5 . . ?
O6 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O6 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C17 C18 C19 121.2(12) . . ?
C17 C18 H18A 119.4 . . ?
C19 C18 H18A 119.4 . . ?
N2 C9 C14 109.7(13) . . ?
N2 C9 C10 110.2(13) . . ?
C14 C9 C10 111.2(14) . . ?
N2 C9 H9A 108.6 . . ?
C14 C9 H9A 108.6 . . ?
C10 C9 H9A 108.6 . . ?
C4 C5 C6 118.6(15) . . ?
C4 C5 H5A 120.7 . . ?
C6 C5 H5A 120.7 . . ?
C12 C13 C14 110.9(13) . . ?
C12 C13 H13A 109.5 . . ?
C14 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 108.0 . . ?
N1 C14 C9 109.4(14) . . ?
N1 C14 C13 112.5(13) . . ?
C9 C14 C13 110.6(14) . . ?
N1 C14 H14A 108.1 . . ?
C9 C14 H14A 108.1 . . ?
C13 C14 H14A 108.1 . . ?
C5 C4 C3 120.2(14) . . ?
C5 C4 H4A 119.9 . . ?
C3 C4 H4A 119.9 . . ?
O9 C22 H22A 109.5 . . ?
O9 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
O9 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C19 C18 120.6(12) . . ?
C20 C19 H19A 119.7 . . ?
C18 C19 H19A 119.7 . . ?
C8 C6 C5 118.9(13) . . ?
C8 C6 C7 119.8(12) . . ?
C5 C6 C7 120.7(14) . . ?
O13 N4 O2 123.0(17) . . ?
O13 N4 O5 121.7(17) . . ?
O2 N4 O5 115.3(13) . . ?
O13 N4 Ce1 176.8(13) . . ?
O2 N4 Ce1 58.4(8) . . ?
O5 N4 Ce1 57.0(7) . . ?
O14 N5 O4 121.3(16) . . ?
O14 N5 O3 120.9(15) . . ?
O4 N5 O3 117.8(13) . . ?
N1 C15 C16 123.1(12) . . ?
N1 C15 H15A 118.4 . . ?
C16 C15 H15A 118.4 . . ?
O8 C7 C2 121.4(13) . . ?
O8 C7 C6 121.2(13) . . ?
C2 C7 C6 117.3(12) . . ?
C11 C12 C13 109.8(16) . . ?
C11 C12 H12A 109.7 . . ?
C13 C12 H12A 109.7 . . ?
C11 C12 H12B 109.7 . . ?
C13 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
C2 C3 C4 122.8(15) . . ?
C2 C3 H3A 118.6 . . ?
C4 C3 H3A 118.6 . . ?
N2 C8 C6 125.6(13) . . ?
N2 C8 H8A 117.2 . . ?
C6 C8 H8A 117.2 . . ?
C18 C17 C16 118.2(12) . . ?
C18 C17 H17A 120.9 . . ?
C16 C17 H17A 120.9 . . ?
C19 C20 O9 126.3(12) . . ?
C19 C20 C21 120.9(13) . . ?
O9 C20 C21 112.8(11) . . ?
C3 C2 O6 126.4(14) . . ?
C3 C2 C7 120.5(14) . . ?
O6 C2 C7 113.0(12) . . ?
C12 C11 C10 112.8(17) . . ?
C12 C11 H11A 109.0 . . ?
C10 C11 H11A 109.0 . . ?
C12 C11 H11B 109.0 . . ?
C10 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
C21 C16 C17 121.5(12) . . ?
C21 C16 C15 120.2(11) . . ?
C17 C16 C15 118.3(12) . . ?
O7 C21 C16 123.1(12) . . ?
O7 C21 C20 119.5(12) . . ?
C16 C21 C20 117.4(12) . . ?
C11 C10 C9 109.6(14) . . ?
C11 C10 H10A 109.7 . . ?
C9 C10 H10A 109.7 . . ?
C11 C10 H10B 109.7 . . ?
C9 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
O12 N3 O1 122.8(14) . . ?
O12 N3 O10 119.9(14) . . ?
O1 N3 O10 117.1(13) . . ?
O11 C23 H23A 109.5 . . ?
O11 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
O11 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C15 N1 C14 126.8(13) . . ?
C15 N1 H111 114(10) . . ?
C14 N1 H111 118(10) . . ?
C8 N2 C9 127.2(13) . . ?
C8 N2 H21 95(10) . . ?
C9 N2 H21 138(10) . . ?
N3 O1 Ce1 94.2(9) . . ?
N4 O2 Ce1 97.3(9) . . ?
N5 O3 Ce1 104.2(9) . . ?
N5 O4 Ce1 91.2(9) . . ?
N4 O5 Ce1 97.9(9) . . ?
C2 O6 C1 116.9(12) . . ?
C2 O6 Ce1 115.8(8) . . ?
C1 O6 Ce1 127.3(9) . . ?
C21 O7 Ce1 133.1(8) . . ?
C7 O8 Ce1 129.2(9) . . ?
C20 O9 C22 117.6(11) . . ?
C20 O9 Ce1 115.7(7) . . ?
C22 O9 Ce1 126.5(9) . . ?
N3 O10 Ce1 102.4(10) . . ?
C23 O11 Ce1 134.1(12) . . ?
C23 O11 H11 118.4 . . ?
Ce1 O11 H11 107.5 . . ?
_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         4.249
_refine_diff_density_min         -1.390
_refine_diff_density_rms         0.160


data_gb-89
_database_code_depnum_ccdc_archive 'CCDC 900874'
#TrackingRef '900874.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H48 Ce N4 O8'
_chemical_formula_sum            'C44 H48 Ce N4 O8'
_chemical_formula_weight         900.98
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a                   17.751(4)
_cell_length_b                   10.493(2)
_cell_length_c                   22.403(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.44(3)
_cell_angle_gamma                90.00
_cell_volume                     4041.0(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    23567
_cell_measurement_theta_min      3.02
_cell_measurement_theta_max      27.79
_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.29
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1848
_exptl_absorpt_coefficient_mu    1.185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5966
_exptl_absorpt_correction_T_max  0.7280
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       '\w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            28509
_diffrn_reflns_av_R_equivalents  0.0866
_diffrn_reflns_av_sigmaI/netI    0.0712
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7105
_reflns_number_gt                4855
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'RAPID-AUTO (Rigaku 1998 <i>RAPID-AUTO</i>)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku 1998 <i>RAPID-AUTO</i>)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXL-97
_refine_special_details          
;
isor 0.01 c33 c31' c36 c32 O8 C26 C36
ISOR 0.01 C9 C12 C17 C18 C21 C22 C30 C37 C38 C39 C40
DELU 0.01 O4 C21 C26 C27 C6 C7 N4 C35'
DELU 0.008 N2 C14 N3 C30 N4 C35 C4 C5 C10 C11
DELU 0.008 C32 C31' C32 C33' C33 C34 C37 C38 C40 C41
OMIT -13 0 10
OMIT -8 1 8
OMIT -19 3 13
OMIT -9 2 5
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+11.5473P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0010(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         7105
_refine_ls_number_parameters     565
_refine_ls_number_restraints     128
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0615
_refine_ls_wR_factor_ref         0.1317
_refine_ls_wR_factor_gt          0.1154
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4102(5) 1.1016(6) 0.2628(4) 0.0565(19) Uani 1 1 d . B .
C2 C 0.4363(5) 1.1844(7) 0.2221(4) 0.069(2) Uani 1 1 d . . .
C3 C 0.5039(6) 1.2531(8) 0.2426(5) 0.085(3) Uani 1 1 d . . .
H3 H 0.5204 1.3070 0.2154 0.102 Uiso 1 1 calc R . .
C4 C 0.5469(6) 1.2437(9) 0.3015(6) 0.090(3) Uani 1 1 d U . .
H4 H 0.5911 1.2937 0.3151 0.108 Uiso 1 1 calc R . .
C5 C 0.5250(5) 1.1604(9) 0.3413(5) 0.082(2) Uani 1 1 d U . .
H5 H 0.5563 1.1515 0.3811 0.098 Uiso 1 1 calc R . .
C6 C 0.4561(5) 1.0879(7) 0.3230(4) 0.066(2) Uani 1 1 d U . .
C7 C 0.4384(5) 0.9988(8) 0.3662(4) 0.067(2) Uani 1 1 d U . .
H7 H 0.4760 0.9897 0.4032 0.081 Uiso 1 1 calc R . .
C8 C 0.3761(5) 0.8412(9) 0.4103(4) 0.089(3) Uani 1 1 d . . .
H8 H 0.3865 0.8969 0.4465 0.107 Uiso 1 1 calc R . .
C9 C 0.4407(6) 0.7495(9) 0.4257(5) 0.101(3) Uani 1 1 d U . .
H9A H 0.4893 0.7964 0.4365 0.121 Uiso 1 1 calc R . .
H9B H 0.4405 0.6993 0.3893 0.121 Uiso 1 1 calc R . .
C10 C 0.4382(8) 0.6613(12) 0.4770(6) 0.136(5) Uani 1 1 d U . .
H10A H 0.4716 0.5891 0.4750 0.163 Uiso 1 1 calc R . .
H10B H 0.4601 0.7051 0.5156 0.163 Uiso 1 1 calc R . .
C11 C 0.3633(9) 0.6139(12) 0.4785(7) 0.152(6) Uani 1 1 d U . .
H11A H 0.3663 0.5823 0.5197 0.182 Uiso 1 1 calc R . .
H11B H 0.3516 0.5416 0.4507 0.182 Uiso 1 1 calc R . .
C12 C 0.2954(6) 0.7067(9) 0.4614(4) 0.096(3) Uani 1 1 d U . .
H12A H 0.2471 0.6592 0.4503 0.116 Uiso 1 1 calc R . .
H12B H 0.2946 0.7591 0.4969 0.116 Uiso 1 1 calc R . .
C13 C 0.3011(6) 0.7906(9) 0.4089(5) 0.094(3) Uani 1 1 d . . .
H13 H 0.2945 0.7286 0.3752 0.112 Uiso 1 1 calc R . .
C14 C 0.1873(5) 0.9080(9) 0.4142(4) 0.078(2) Uani 1 1 d U . .
H14 H 0.1961 0.8732 0.4535 0.093 Uiso 1 1 calc R . .
C15 C 0.1187(5) 0.9880(8) 0.3945(4) 0.077(2) Uani 1 1 d . . .
C16 C 0.0788(6) 1.0288(10) 0.4384(5) 0.105(3) Uani 1 1 d . . .
H16 H 0.0970 1.0062 0.4796 0.126 Uiso 1 1 calc R . .
C17 C 0.0127(7) 1.1024(11) 0.4196(6) 0.113(4) Uani 1 1 d U . .
H17 H -0.0123 1.1313 0.4489 0.136 Uiso 1 1 calc R . .
C18 C -0.0169(6) 1.1339(10) 0.3590(6) 0.107(3) Uani 1 1 d U . .
H18 H -0.0627 1.1809 0.3473 0.129 Uiso 1 1 calc R . .
C19 C 0.0216(5) 1.0953(8) 0.3146(5) 0.079(3) Uani 1 1 d . . .
C20 C 0.0902(4) 1.0224(7) 0.3325(4) 0.065(2) Uani 1 1 d . B .
C21 C -0.0628(6) 1.2173(11) 0.2364(6) 0.127(4) Uani 1 1 d U . .
H21A H -0.1100 1.1833 0.2436 0.191 Uiso 1 1 calc R . .
H21B H -0.0707 1.2375 0.1935 0.191 Uiso 1 1 calc R . .
H21C H -0.0485 1.2931 0.2605 0.191 Uiso 1 1 calc R . .
C22 C 0.3840(6) 1.0936(9) 0.1247(5) 0.104(3) Uani 1 1 d U . .
H22A H 0.4340 1.0633 0.1218 0.155 Uiso 1 1 calc R . .
H22B H 0.3532 1.1152 0.0844 0.155 Uiso 1 1 calc R . .
H22C H 0.3582 1.0281 0.1421 0.155 Uiso 1 1 calc R . .
C23 C 0.2603(5) 0.6999(7) 0.2160(4) 0.063(2) Uani 1 1 d . B .
C24 C 0.2977(5) 0.5794(8) 0.2313(5) 0.076(3) Uani 1 1 d . . .
C25 C 0.3041(6) 0.4963(9) 0.1843(6) 0.102(3) Uani 1 1 d . . .
H25 H 0.3289 0.4181 0.1937 0.122 Uiso 1 1 calc R . .
C26 C 0.2736(7) 0.5307(12) 0.1237(6) 0.114(4) Uani 1 1 d U . .
H26 H 0.2783 0.4747 0.0927 0.137 Uiso 1 1 calc R . .
C27 C 0.2365(7) 0.6444(11) 0.1078(5) 0.105(3) Uani 1 1 d U . .
H27 H 0.2161 0.6650 0.0665 0.126 Uiso 1 1 calc R . .
C28 C 0.2293(6) 0.7311(9) 0.1549(4) 0.078(3) Uani 1 1 d . . .
C29 C 0.1902(6) 0.8478(10) 0.1355(4) 0.092(3) Uani 1 1 d . B .
H29 H 0.1665 0.8541 0.0936 0.111 Uiso 1 1 calc R . .
C32 C 0.0291(8) 1.1506(12) 0.0643(7) 0.151(5) Uani 1 1 d U . .
H32A H -0.0010 1.1551 0.0949 0.181 Uiso 1 1 calc R A 1
H32B H -0.0061 1.1419 0.0238 0.181 Uiso 1 1 calc R A 1
C30 C 0.1151(17) 1.060(2) 0.1487(11) 0.082(5) Uani 0.50(2) 1 d PU B 1
H30 H 0.0735 1.0482 0.1699 0.098 Uiso 0.50(2) 1 calc PR B 1
C31 C 0.0835(15) 1.048(2) 0.0770(12) 0.109(10) Uani 0.50(2) 1 d P B 1
H31A H 0.1247 1.0594 0.0560 0.131 Uiso 0.50(2) 1 calc PR B 1
H31B H 0.0582 0.9666 0.0653 0.131 Uiso 0.50(2) 1 calc PR B 1
C33 C 0.088(2) 1.282(3) 0.0679(14) 0.126(8) Uani 0.50(2) 1 d PU B 1
H33A H 0.1335 1.2645 0.0530 0.151 Uiso 0.50(2) 1 calc PR B 1
H33B H 0.0600 1.3546 0.0459 0.151 Uiso 0.50(2) 1 calc PR B 1
C34 C 0.1070(19) 1.300(2) 0.1354(12) 0.097(7) Uani 0.50(2) 1 d PU B 1
H34A H 0.0598 1.3043 0.1497 0.117 Uiso 0.50(2) 1 calc PR B 1
H34B H 0.1354 1.3794 0.1465 0.117 Uiso 0.50(2) 1 calc PR B 1
C35 C 0.157(2) 1.188(4) 0.1648(18) 0.100(11) Uani 0.50(2) 1 d PU B 1
H35 H 0.2004 1.1860 0.1455 0.120 Uiso 0.50(2) 1 calc PR B 1
C30' C 0.1505(12) 1.0475(16) 0.1250(10) 0.065(6) Uani 0.50(2) 1 d P B 2
H30' H 0.1594 1.0308 0.0843 0.079 Uiso 0.50(2) 1 calc PR B 2
C31' C 0.0661(12) 1.043(2) 0.1225(14) 0.086(6) Uani 0.50(2) 1 d PU B 2
H31C H 0.0560 1.0702 0.1612 0.103 Uiso 0.50(2) 1 calc PR B 2
H31D H 0.0448 0.9587 0.1122 0.103 Uiso 0.50(2) 1 calc PR B 2
C33' C 0.0547(13) 1.279(2) 0.0991(16) 0.095(8) Uani 0.50(2) 1 d PU B 2
H33C H 0.0310 1.3515 0.0745 0.114 Uiso 0.50(2) 1 calc PR B 2
H33D H 0.0410 1.2811 0.1384 0.114 Uiso 0.50(2) 1 calc PR B 2
C34' C 0.1444(15) 1.279(2) 0.1082(16) 0.097(9) Uani 0.50(2) 1 d P B 2
H34C H 0.1554 1.2684 0.0682 0.116 Uiso 0.50(2) 1 calc PR B 2
H34D H 0.1644 1.3616 0.1240 0.116 Uiso 0.50(2) 1 calc PR B 2
C35' C 0.189(2) 1.176(4) 0.1516(17) 0.094(10) Uani 0.50(2) 1 d PU B 2
H35' H 0.2428 1.1759 0.1485 0.112 Uiso 0.50(2) 1 calc PR B 2
C36 C 0.1678(6) 1.2853(10) 0.2519(6) 0.108(3) Uani 1 1 d U B .
H36 H 0.1427 1.3494 0.2257 0.130 Uiso 1 1 calc R . .
C37 C 0.1781(6) 1.3086(9) 0.3154(6) 0.101(3) Uani 1 1 d U . .
C38 C 0.1352(8) 1.4130(12) 0.3321(8) 0.141(5) Uani 1 1 d U . .
H38 H 0.1036 1.4656 0.3028 0.169 Uiso 1 1 calc R . .
C39 C 0.1436(9) 1.4293(15) 0.3919(9) 0.160(6) Uani 1 1 d U . .
H39 H 0.1122 1.4926 0.4020 0.192 Uiso 1 1 calc R . .
C40 C 0.1902(8) 1.3693(13) 0.4413(7) 0.144(5) Uani 1 1 d U . .
H40 H 0.1923 1.3908 0.4820 0.173 Uiso 1 1 calc R . .
C41 C 0.2353(7) 1.2705(11) 0.4244(7) 0.109(4) Uani 1 1 d U . .
C42 C 0.2285(5) 1.2394(8) 0.3624(5) 0.082(3) Uani 1 1 d . B .
C43 C 0.3544(8) 1.2008(12) 0.4741(6) 0.138(5) Uani 1 1 d . . .
H43A H 0.3637 1.1664 0.4369 0.207 Uiso 1 1 calc R . .
H43B H 0.3816 1.1509 0.5087 0.207 Uiso 1 1 calc R . .
H43C H 0.3725 1.2873 0.4792 0.207 Uiso 1 1 calc R . .
C44 C 0.3707(7) 0.4435(9) 0.3092(6) 0.127(4) Uani 1 1 d . . .
H44A H 0.3397 0.3709 0.2925 0.191 Uiso 1 1 calc R . .
H44B H 0.3861 0.4369 0.3534 0.191 Uiso 1 1 calc R . .
H44C H 0.4162 0.4465 0.2934 0.191 Uiso 1 1 calc R . .
Ce1 Ce 0.24637(2) 0.98202(3) 0.283082(19) 0.05067(17) Uani 1 1 d . B .
N1 N 0.3770(4) 0.9302(5) 0.3599(3) 0.0546(15) Uani 1 1 d . . .
N2 N 0.2368(4) 0.8802(6) 0.3837(3) 0.0640(17) Uani 1 1 d U . .
N3 N 0.1832(4) 0.9453(7) 0.1680(3) 0.086(2) Uani 1 1 d U . .
N4 N 0.1886(4) 1.1862(7) 0.2252(4) 0.090(3) Uani 1 1 d U . .
O1 O 0.3445(3) 1.0396(5) 0.2434(2) 0.0634(13) Uani 1 1 d . . .
O2 O 0.3938(4) 1.2033(5) 0.1632(3) 0.0889(19) Uani 1 1 d . . .
O3 O 0.1254(3) 0.9867(4) 0.2898(2) 0.0614(12) Uani 1 1 d . . .
O4 O -0.0011(4) 1.1234(6) 0.2540(4) 0.098(2) Uani 1 1 d U . .
O5 O 0.2555(3) 0.7771(4) 0.2611(2) 0.0601(13) Uani 1 1 d . . .
O6 O 0.3261(4) 0.5574(5) 0.2921(3) 0.0856(18) Uani 1 1 d . . .
O7 O 0.2700(3) 1.1433(4) 0.3476(2) 0.0642(14) Uani 1 1 d . . .
O8 O 0.2770(7) 1.1978(10) 0.4706(5) 0.140(3) Uani 1 1 d 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
C1 0.057(5) 0.046(4) 0.072(5) -0.010(4) 0.025(4) 0.006(4)
C2 0.084(7) 0.050(4) 0.089(7) -0.009(4) 0.048(6) -0.001(4)
C3 0.094(7) 0.058(5) 0.119(9) -0.013(5) 0.053(7) -0.007(5)
C4 0.061(6) 0.077(6) 0.143(10) -0.026(6) 0.048(7) -0.015(5)
C5 0.066(6) 0.088(6) 0.091(7) -0.023(5) 0.019(5) 0.008(5)
C6 0.058(5) 0.060(5) 0.080(6) -0.010(4) 0.020(5) 0.007(4)
C7 0.057(5) 0.081(6) 0.060(5) -0.013(4) 0.007(4) 0.017(5)
C8 0.077(7) 0.105(7) 0.090(7) 0.034(6) 0.033(5) 0.039(6)
C9 0.090(6) 0.084(5) 0.120(7) 0.025(5) 0.009(5) 0.027(5)
C10 0.161(11) 0.129(11) 0.121(10) 0.054(8) 0.039(10) 0.071(9)
C11 0.175(12) 0.112(9) 0.154(12) 0.087(9) 0.014(11) 0.031(10)
C12 0.127(7) 0.082(5) 0.090(6) 0.027(5) 0.045(5) 0.015(5)
C13 0.088(7) 0.088(6) 0.104(8) 0.049(6) 0.021(6) 0.005(6)
C14 0.078(6) 0.094(6) 0.063(6) 0.005(5) 0.021(5) -0.009(5)
C15 0.082(6) 0.070(5) 0.088(6) -0.010(5) 0.038(5) -0.008(5)
C16 0.107(8) 0.113(8) 0.108(8) -0.010(7) 0.053(7) -0.003(7)
C17 0.111(7) 0.116(7) 0.133(8) -0.020(6) 0.068(6) 0.001(6)
C18 0.094(7) 0.109(7) 0.128(8) -0.002(6) 0.045(6) 0.020(5)
C19 0.063(6) 0.072(6) 0.115(8) -0.009(5) 0.046(6) 0.001(4)
C20 0.052(4) 0.055(4) 0.094(6) -0.011(4) 0.031(4) 0.000(4)
C21 0.104(7) 0.123(7) 0.152(8) 0.014(6) 0.026(6) 0.041(6)
C22 0.131(7) 0.097(6) 0.088(6) -0.002(5) 0.038(6) -0.008(6)
C23 0.060(5) 0.062(5) 0.077(6) -0.019(4) 0.037(4) -0.024(4)
C24 0.081(6) 0.056(5) 0.107(8) -0.025(5) 0.051(6) -0.014(4)
C25 0.114(8) 0.072(6) 0.136(9) -0.030(6) 0.064(7) -0.018(6)
C26 0.123(7) 0.124(7) 0.110(7) -0.047(6) 0.057(6) -0.022(6)
C27 0.120(9) 0.132(8) 0.072(7) -0.022(6) 0.044(6) -0.043(7)
C28 0.091(7) 0.083(6) 0.067(6) -0.018(5) 0.034(5) -0.042(5)
C29 0.115(9) 0.100(8) 0.054(6) 0.001(5) 0.004(5) -0.050(7)
C32 0.137(8) 0.131(7) 0.152(8) 0.005(6) -0.027(7) -0.006(6)
C30 0.093(9) 0.084(8) 0.066(9) 0.006(7) 0.014(7) -0.012(6)
C31 0.114(19) 0.103(16) 0.083(18) -0.014(13) -0.029(15) 0.004(14)
C33 0.131(12) 0.129(10) 0.115(11) 0.014(9) 0.025(9) 0.001(8)
C34 0.085(19) 0.089(14) 0.102(12) 0.042(11) -0.006(14) 0.006(13)
C35 0.09(3) 0.076(8) 0.109(14) 0.024(14) -0.016(17) -0.004(13)
C30' 0.066(13) 0.059(10) 0.065(12) 0.021(8) 0.005(9) -0.007(9)
C31' 0.072(10) 0.079(8) 0.106(10) -0.007(7) 0.023(8) -0.004(7)
C33' 0.053(13) 0.092(8) 0.12(2) 0.037(9) -0.006(13) 0.009(11)
C34' 0.072(17) 0.082(14) 0.12(2) 0.035(15) 0.003(15) -0.006(12)
C35' 0.08(2) 0.068(15) 0.100(11) 0.025(12) -0.038(14) -0.031(18)
C36 0.098(6) 0.076(5) 0.129(6) 0.015(5) -0.013(5) 0.004(5)
C37 0.078(6) 0.065(5) 0.149(8) -0.006(5) 0.007(6) 0.008(4)
C38 0.117(8) 0.111(7) 0.182(9) -0.008(7) 0.014(7) 0.033(6)
C39 0.142(9) 0.150(9) 0.190(10) -0.025(8) 0.044(8) 0.017(7)
C40 0.151(9) 0.130(8) 0.164(9) -0.056(7) 0.062(7) 0.005(6)
C41 0.092(8) 0.089(7) 0.162(13) -0.050(8) 0.065(9) -0.018(6)
C42 0.062(6) 0.055(5) 0.128(9) -0.017(5) 0.021(6) -0.005(4)
C43 0.147(13) 0.134(10) 0.113(10) -0.052(8) -0.003(9) 0.010(10)
C44 0.144(11) 0.062(6) 0.179(12) 0.000(7) 0.044(9) 0.038(7)
Ce1 0.0522(3) 0.0393(2) 0.0580(3) 0.00296(19) 0.00910(17) -0.0001(2)
N1 0.059(4) 0.051(3) 0.055(4) 0.002(3) 0.014(3) 0.016(3)
N2 0.064(4) 0.058(4) 0.074(5) 0.011(3) 0.024(3) 0.004(3)
N3 0.096(6) 0.068(4) 0.077(5) 0.013(4) -0.010(4) -0.030(4)
N4 0.074(5) 0.056(4) 0.116(7) 0.016(4) -0.023(5) -0.005(4)
O1 0.065(3) 0.064(3) 0.062(3) 0.002(2) 0.017(3) -0.006(3)
O2 0.123(6) 0.061(3) 0.092(5) 0.010(3) 0.044(4) -0.004(4)
O3 0.056(3) 0.060(3) 0.067(3) -0.006(3) 0.014(2) 0.004(3)
O4 0.072(4) 0.093(4) 0.128(6) 0.005(4) 0.025(4) 0.029(3)
O5 0.070(3) 0.044(3) 0.071(4) -0.003(2) 0.025(3) 0.002(2)
O6 0.100(5) 0.050(3) 0.114(5) -0.006(3) 0.042(4) 0.018(3)
O7 0.066(3) 0.043(3) 0.080(4) -0.008(2) 0.012(3) 0.006(2)
O8 0.157(7) 0.144(6) 0.127(6) -0.035(5) 0.052(6) -0.014(6)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.311(8) . ?
C1 C6 1.399(11) . ?
C1 C2 1.417(10) . ?
C2 O2 1.362(10) . ?
C2 C3 1.377(12) . ?
C3 C4 1.355(13) . ?
C3 H3 0.9300 . ?
C4 C5 1.371(12) . ?
C4 H4 0.9300 . ?
C5 C6 1.413(11) . ?
C5 H5 0.9300 . ?
C6 C7 1.434(11) . ?
C7 N1 1.284(9) . ?
C7 H7 0.9300 . ?
C8 C13 1.426(12) . ?
C8 N1 1.469(10) . ?
C8 C9 1.470(11) . ?
C8 H8 0.9800 . ?
C9 C10 1.486(13) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.428(16) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.522(14) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.494(11) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N2 1.478(10) . ?
C13 H13 0.9800 . ?
C14 N2 1.272(10) . ?
C14 C15 1.455(12) . ?
C14 H14 0.9300 . ?
C15 C20 1.402(11) . ?
C15 C16 1.414(12) . ?
C16 C17 1.380(14) . ?
C16 H16 0.9300 . ?
C17 C18 1.369(14) . ?
C17 H17 0.9300 . ?
C18 C19 1.399(13) . ?
C18 H18 0.9300 . ?
C19 O4 1.350(11) . ?
C19 C20 1.409(11) . ?
C20 O3 1.321(8) . ?
C21 O4 1.453(11) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 O2 1.423(10) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 O5 1.314(8) . ?
C23 C28 1.383(11) . ?
C23 C24 1.429(12) . ?
C24 O6 1.349(11) . ?
C24 C25 1.395(12) . ?
C25 C26 1.378(15) . ?
C25 H25 0.9300 . ?
C26 C27 1.367(15) . ?
C26 H26 0.9300 . ?
C27 C28 1.422(12) . ?
C27 H27 0.9300 . ?
C28 C29 1.421(13) . ?
C29 N3 1.282(12) . ?
C29 H29 0.9300 . ?
C32 C31 1.43(2) . ?
C32 C33' 1.57(3) . ?
C32 C33 1.72(3) . ?
C32 C31' 1.72(3) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C30 C35 1.54(5) . ?
C30 C31 1.57(4) . ?
C30 N3 1.68(3) . ?
C30 H30 0.9800 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C33 C34 1.48(4) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.52(5) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 N4 1.33(4) . ?
C35 H35 0.9800 . ?
C30' N3 1.461(16) . ?
C30' C31' 1.49(3) . ?
C30' C35' 1.56(4) . ?
C30' H30' 0.9800 . ?
C31' H31C 0.9700 . ?
C31' H31D 0.9700 . ?
C33' C34' 1.55(4) . ?
C33' H33C 0.9700 . ?
C33' H33D 0.9700 . ?
C34' C35' 1.53(5) . ?
C34' H34C 0.9700 . ?
C34' H34D 0.9700 . ?
C35' N4 1.65(4) . ?
C35' H35' 0.9800 . ?
C36 N4 1.299(13) . ?
C36 C37 1.408(14) . ?
C36 H36 0.9300 . ?
C37 C42 1.402(13) . ?
C37 C38 1.437(14) . ?
C38 C39 1.323(18) . ?
C38 H38 0.9300 . ?
C39 C40 1.360(18) . ?
C39 H39 0.9300 . ?
C40 C41 1.418(15) . ?
C40 H40 0.9300 . ?
C41 O8 1.349(15) . ?
C41 C42 1.401(15) . ?
C42 O7 1.340(9) . ?
C43 O8 1.356(13) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 O6 1.431(10) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
Ce1 O3 2.190(5) . ?
Ce1 O7 2.197(5) . ?
Ce1 O5 2.221(4) . ?
Ce1 O1 2.228(5) . ?
Ce1 N2 2.539(6) . ?
Ce1 N3 2.570(7) . ?
Ce1 N1 2.578(6) . ?
Ce1 N4 2.580(7) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C6 121.6(7) . . ?
O1 C1 C2 119.9(8) . . ?
C6 C1 C2 118.5(8) . . ?
O2 C2 C3 118.1(8) . . ?
O2 C2 C1 121.4(8) . . ?
C3 C2 C1 120.4(9) . . ?
C4 C3 C2 121.2(9) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C5 119.9(9) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 121.4(9) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C1 C6 C5 118.6(8) . . ?
C1 C6 C7 123.0(8) . . ?
C5 C6 C7 118.3(8) . . ?
N1 C7 C6 127.8(7) . . ?
N1 C7 H7 116.1 . . ?
C6 C7 H7 116.1 . . ?
C13 C8 N1 114.1(7) . . ?
C13 C8 C9 115.5(9) . . ?
N1 C8 C9 116.1(7) . . ?
C13 C8 H8 102.8 . . ?
N1 C8 H8 102.8 . . ?
C9 C8 H8 102.8 . . ?
C8 C9 C10 114.7(9) . . ?
C8 C9 H9A 108.6 . . ?
C10 C9 H9A 108.6 . . ?
C8 C9 H9B 108.6 . . ?
C10 C9 H9B 108.6 . . ?
H9A C9 H9B 107.6 . . ?
C11 C10 C9 116.3(11) . . ?
C11 C10 H10A 108.2 . . ?
C9 C10 H10A 108.2 . . ?
C11 C10 H10B 108.2 . . ?
C9 C10 H10B 108.2 . . ?
H10A C10 H10B 107.4 . . ?
C10 C11 C12 117.0(10) . . ?
C10 C11 H11A 108.0 . . ?
C12 C11 H11A 108.0 . . ?
C10 C11 H11B 108.0 . . ?
C12 C11 H11B 108.0 . . ?
H11A C11 H11B 107.3 . . ?
C13 C12 C11 111.7(9) . . ?
C13 C12 H12A 109.3 . . ?
C11 C12 H12A 109.3 . . ?
C13 C12 H12B 109.3 . . ?
C11 C12 H12B 109.3 . . ?
H12A C12 H12B 107.9 . . ?
C8 C13 N2 113.6(7) . . ?
C8 C13 C12 116.6(9) . . ?
N2 C13 C12 118.5(8) . . ?
C8 C13 H13 101.3 . . ?
N2 C13 H13 101.3 . . ?
C12 C13 H13 101.3 . . ?
N2 C14 C15 127.4(8) . . ?
N2 C14 H14 116.3 . . ?
C15 C14 H14 116.3 . . ?
C20 C15 C16 119.5(9) . . ?
C20 C15 C14 121.1(7) . . ?
C16 C15 C14 119.4(9) . . ?
C17 C16 C15 119.5(11) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C18 C17 C16 121.6(11) . . ?
C18 C17 H17 119.2 . . ?
C16 C17 H17 119.2 . . ?
C17 C18 C19 120.0(11) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
O4 C19 C18 125.2(9) . . ?
O4 C19 C20 115.1(8) . . ?
C18 C19 C20 119.7(10) . . ?
O3 C20 C15 121.7(7) . . ?
O3 C20 C19 118.7(8) . . ?
C15 C20 C19 119.6(8) . . ?
O4 C21 H21A 109.5 . . ?
O4 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O4 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O2 C22 H22A 109.5 . . ?
O2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
O2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O5 C23 C28 122.0(8) . . ?
O5 C23 C24 118.4(8) . . ?
C28 C23 C24 119.6(8) . . ?
O6 C24 C25 125.1(9) . . ?
O6 C24 C23 115.4(7) . . ?
C25 C24 C23 119.5(10) . . ?
C26 C25 C24 119.6(11) . . ?
C26 C25 H25 120.2 . . ?
C24 C25 H25 120.2 . . ?
C27 C26 C25 122.1(10) . . ?
C27 C26 H26 119.0 . . ?
C25 C26 H26 119.0 . . ?
C26 C27 C28 119.4(11) . . ?
C26 C27 H27 120.3 . . ?
C28 C27 H27 120.3 . . ?
C23 C28 C29 123.4(8) . . ?
C23 C28 C27 119.8(10) . . ?
C29 C28 C27 116.8(10) . . ?
N3 C29 C28 128.6(9) . . ?
N3 C29 H29 115.7 . . ?
C28 C29 H29 115.7 . . ?
C31 C32 C33' 116.9(14) . . ?
C31 C32 C33 102.9(19) . . ?
C33' C32 C33 35.7(11) . . ?
C31 C32 C31' 41.0(12) . . ?
C33' C32 C31' 100.3(15) . . ?
C33 C32 C31' 112.1(15) . . ?
C31 C32 H32A 111.2 . . ?
C33' C32 H32A 75.5 . . ?
C33 C32 H32A 111.2 . . ?
C31' C32 H32A 70.8 . . ?
C31 C32 H32B 111.2 . . ?
C33' C32 H32B 125.9 . . ?
C33 C32 H32B 111.2 . . ?
C31' C32 H32B 133.0 . . ?
H32A C32 H32B 109.1 . . ?
C35 C30 C31 110(2) . . ?
C35 C30 N3 107(2) . . ?
C31 C30 N3 105.1(19) . . ?
C35 C30 H30 111.6 . . ?
C31 C30 H30 111.6 . . ?
N3 C30 H30 111.6 . . ?
C32 C31 C30 101(2) . . ?
C32 C31 H31A 111.5 . . ?
C30 C31 H31A 111.5 . . ?
C32 C31 H31B 111.5 . . ?
C30 C31 H31B 111.5 . . ?
H31A C31 H31B 109.3 . . ?
C34 C33 C32 98(2) . . ?
C34 C33 H33A 112.2 . . ?
C32 C33 H33A 112.2 . . ?
C34 C33 H33B 112.2 . . ?
C32 C33 H33B 112.2 . . ?
H33A C33 H33B 109.8 . . ?
C33 C34 C35 108(3) . . ?
C33 C34 H34A 110.2 . . ?
C35 C34 H34A 110.2 . . ?
C33 C34 H34B 110.2 . . ?
C35 C34 H34B 110.2 . . ?
H34A C34 H34B 108.5 . . ?
N4 C35 C34 120(3) . . ?
N4 C35 C30 107(3) . . ?
C34 C35 C30 113(3) . . ?
N4 C35 H35 105.3 . . ?
C34 C35 H35 105.3 . . ?
C30 C35 H35 105.3 . . ?
N3 C30' C31' 103.6(18) . . ?
N3 C30' C35' 108.7(19) . . ?
C31' C30' C35' 112(2) . . ?
N3 C30' H30' 110.7 . . ?
C31' C30' H30' 110.7 . . ?
C35' C30' H30' 110.7 . . ?
C30' C31' C32 101.6(17) . . ?
C30' C31' H31C 111.4 . . ?
C32 C31' H31C 111.4 . . ?
C30' C31' H31D 111.4 . . ?
C32 C31' H31D 111.4 . . ?
H31C C31' H31D 109.3 . . ?
C34' C33' C32 103(2) . . ?
C34' C33' H33C 111.2 . . ?
C32 C33' H33C 111.2 . . ?
C34' C33' H33D 111.2 . . ?
C32 C33' H33D 111.2 . . ?
H33C C33' H33D 109.1 . . ?
C35' C34' C33' 116(2) . . ?
C35' C34' H34C 108.4 . . ?
C33' C34' H34C 108.4 . . ?
C35' C34' H34D 108.4 . . ?
C33' C34' H34D 108.4 . . ?
H34C C34' H34D 107.5 . . ?
C34' C35' C30' 105(2) . . ?
C34' C35' N4 117(3) . . ?
C30' C35' N4 109(2) . . ?
C34' C35' H35' 108.2 . . ?
C30' C35' H35' 108.2 . . ?
N4 C35' H35' 108.2 . . ?
N4 C36 C37 128.6(10) . . ?
N4 C36 H36 115.7 . . ?
C37 C36 H36 115.7 . . ?
C42 C37 C36 124.5(10) . . ?
C42 C37 C38 118.6(12) . . ?
C36 C37 C38 116.8(11) . . ?
C39 C38 C37 115.4(14) . . ?
C39 C38 H38 122.3 . . ?
C37 C38 H38 122.3 . . ?
C38 C39 C40 131.1(16) . . ?
C38 C39 H39 114.5 . . ?
C40 C39 H39 114.5 . . ?
C39 C40 C41 113.0(15) . . ?
C39 C40 H40 123.5 . . ?
C41 C40 H40 123.5 . . ?
O8 C41 C42 121.6(10) . . ?
O8 C41 C40 116.5(14) . . ?
C42 C41 C40 121.3(14) . . ?
O7 C42 C41 120.3(10) . . ?
O7 C42 C37 119.3(10) . . ?
C41 C42 C37 120.4(10) . . ?
O8 C43 H43A 109.5 . . ?
O8 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
O8 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O6 C44 H44A 109.5 . . ?
O6 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
O6 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O3 Ce1 O7 88.13(18) . . ?
O3 Ce1 O5 99.43(18) . . ?
O7 Ce1 O5 151.57(18) . . ?
O3 Ce1 O1 154.03(18) . . ?
O7 Ce1 O1 90.75(19) . . ?
O5 Ce1 O1 93.82(18) . . ?
O3 Ce1 N2 70.4(2) . . ?
O7 Ce1 N2 77.6(2) . . ?
O5 Ce1 N2 79.29(19) . . ?
O1 Ce1 N2 134.5(2) . . ?
O3 Ce1 N3 83.2(2) . . ?
O7 Ce1 N3 137.6(2) . . ?
O5 Ce1 N3 70.8(2) . . ?
O1 Ce1 N3 80.2(2) . . ?
N2 Ce1 N3 135.9(2) . . ?
O3 Ce1 N1 133.88(18) . . ?
O7 Ce1 N1 74.39(18) . . ?
O5 Ce1 N1 80.84(18) . . ?
O1 Ce1 N1 70.16(19) . . ?
N2 Ce1 N1 64.3(2) . . ?
N3 Ce1 N1 137.1(2) . . ?
O3 Ce1 N4 75.1(2) . . ?
O7 Ce1 N4 71.2(2) . . ?
O5 Ce1 N4 137.2(2) . . ?
O1 Ce1 N4 80.0(2) . . ?
N2 Ce1 N4 133.6(3) . . ?
N3 Ce1 N4 66.5(3) . . ?
N1 Ce1 N4 133.5(2) . . ?
C7 N1 C8 116.4(7) . . ?
C7 N1 Ce1 123.6(5) . . ?
C8 N1 Ce1 117.8(5) . . ?
C14 N2 C13 120.9(8) . . ?
C14 N2 Ce1 126.0(6) . . ?
C13 N2 Ce1 112.9(5) . . ?
C29 N3 C30' 106.8(12) . . ?
C29 N3 C30 126.1(11) . . ?
C30' N3 C30 33.3(8) . . ?
C29 N3 Ce1 127.6(7) . . ?
C30' N3 Ce1 123.6(9) . . ?
C30 N3 Ce1 105.0(9) . . ?
C36 N4 C35 111(2) . . ?
C36 N4 C35' 125.6(16) . . ?
C35 N4 C35' 25(2) . . ?
C36 N4 Ce1 123.8(7) . . ?
C35 N4 Ce1 123(2) . . ?
C35' N4 Ce1 110.4(15) . . ?
C1 O1 Ce1 136.2(5) . . ?
C2 O2 C22 115.0(7) . . ?
C20 O3 Ce1 134.8(5) . . ?
C19 O4 C21 115.9(8) . . ?
C23 O5 Ce1 142.2(5) . . ?
C24 O6 C44 117.1(7) . . ?
C42 O7 Ce1 135.8(5) . . ?
C41 O8 C43 112.7(12) . . ?
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.776
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.090


data_c2
_database_code_depnum_ccdc_archive 'CCDC 900875'
#TrackingRef '900875.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C45 H56 Ce N4 O9, 3(F6 P), C H2 Cl2, 2(H2 O)'
_chemical_formula_sum            'C46 H62 Ce Cl2 F18 N4 O11 P3'
_chemical_formula_weight         1492.93
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   14.560(3)
_cell_length_b                   15.267(3)
_cell_length_c                   16.804(3)
_cell_angle_alpha                70.46(3)
_cell_angle_beta                 72.52(3)
_cell_angle_gamma                64.76(3)
_cell_volume                     3129.1(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    18483
_cell_measurement_theta_min      3.00
_cell_measurement_theta_max      27.49
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.35
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1474
_exptl_absorpt_coefficient_mu    0.994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6104
_exptl_absorpt_correction_T_max  0.7249
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       '\w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            23971
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0764
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         25.00
_reflns_number_total             10864
_reflns_number_gt                7424
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'RAPID-AUTO (Rigaku 1998 <i>RAPID-AUTO</i>)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku 1998 <i>RAPID-AUTO</i>)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXL-97
_refine_special_details          
;
omit 2 0 1
omit -1 0 4
omit -1 0 5
omit -3 1 5
omit -2 1 0
omit -3 1 4
OMIT -3.00 50.00
isor 0.01 c9 c11 c13 n1 c33
DFIX 1.45 0.01 C10 C11
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1379P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10864
_refine_ls_number_parameters     778
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_gt           0.0727
_refine_ls_wR_factor_ref         0.2160
_refine_ls_wR_factor_gt          0.1905
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.033
_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
C1 C -0.0456(6) 0.0590(6) 0.1963(5) 0.065(2) Uani 1 1 d . . .
C2 C -0.1453(6) 0.1158(5) 0.2351(5) 0.0606(19) Uani 1 1 d . . .
C3 C -0.2309(6) 0.0952(7) 0.2376(6) 0.080(3) Uani 1 1 d . . .
H3 H -0.2963 0.1333 0.2619 0.097 Uiso 1 1 calc R . .
C4 C -0.2195(7) 0.0178(8) 0.2040(8) 0.092(3) Uani 1 1 d . . .
H4 H -0.2771 0.0048 0.2058 0.110 Uiso 1 1 calc R . .
C5 C -0.1257(7) -0.0373(7) 0.1693(7) 0.087(3) Uani 1 1 d . . .
H5 H -0.1188 -0.0894 0.1483 0.104 Uiso 1 1 calc R . .
C6 C -0.0367(6) -0.0185(6) 0.1635(6) 0.068(2) Uani 1 1 d . . .
C7 C 0.0612(7) -0.0813(7) 0.1280(7) 0.084(3) Uani 1 1 d . A .
H7 H 0.0644 -0.1337 0.1095 0.101 Uiso 1 1 calc R . .
C8 C 0.2592(12) -0.1550(9) 0.1145(9) 0.057(4) Uani 0.50 1 d P A 1
H8 H 0.2707 -0.2072 0.1676 0.068 Uiso 0.50 1 calc PR A 1
C8' C 0.2443(11) -0.0961(13) 0.0518(13) 0.065(4) Uani 0.50 1 d P A 2
H8' H 0.2381 -0.0422 -0.0006 0.078 Uiso 0.50 1 calc PR A 2
C9 C 0.2558(9) -0.1937(10) 0.0327(9) 0.113(4) Uani 1 1 d U . .
H9A H 0.2410 -0.2545 0.0569 0.136 Uiso 1 1 calc R A 1
H9B H 0.1984 -0.1438 0.0056 0.136 Uiso 1 1 calc R A 1
C10 C 0.3563(12) -0.2145(19) -0.0401(15) 0.092(6) Uani 0.50 1 d PD A 1
H10A H 0.3652 -0.2699 -0.0614 0.111 Uiso 0.50 1 calc PR A 1
H10B H 0.3498 -0.1561 -0.0878 0.111 Uiso 0.50 1 calc PR A 1
C10' C 0.377(2) -0.2794(14) 0.0256(15) 0.096(7) Uani 0.50 1 d P A 2
H10C H 0.3873 -0.3228 0.0820 0.116 Uiso 0.50 1 calc PR A 2
H10D H 0.3863 -0.3200 -0.0120 0.116 Uiso 0.50 1 calc PR A 2
C11 C 0.4432(11) -0.2377(13) -0.0035(11) 0.141(5) Uani 1 1 d DU . .
H11A H 0.5018 -0.2379 -0.0502 0.169 Uiso 1 1 calc R A 1
H11B H 0.4589 -0.3052 0.0320 0.169 Uiso 1 1 calc R A 1
C12 C 0.4363(7) -0.1741(8) 0.0484(8) 0.097(3) Uani 1 1 d . A .
H12A H 0.4728 -0.1297 0.0135 0.117 Uiso 1 1 calc R . .
H12B H 0.4717 -0.2161 0.0960 0.117 Uiso 1 1 calc R . .
C13 C 0.3283(9) -0.1120(10) 0.0840(10) 0.114(4) Uani 1 1 d U . .
H13 H 0.3045 -0.0649 0.0315 0.137 Uiso 1 1 calc R A 1
C14 C 0.3949(6) -0.0479(6) 0.1604(5) 0.066(2) Uani 1 1 d . . .
H14 H 0.4584 -0.0997 0.1541 0.079 Uiso 1 1 calc R A .
C15 C 0.3841(6) 0.0242(6) 0.2017(5) 0.0636(19) Uani 1 1 d . A .
C16 C 0.4700(7) 0.0174(9) 0.2290(7) 0.098(4) Uani 1 1 d . . .
H16 H 0.5335 -0.0335 0.2195 0.118 Uiso 1 1 calc R A .
C17 C 0.4592(9) 0.0853(12) 0.2690(10) 0.136(6) Uani 1 1 d . A .
H17 H 0.5169 0.0823 0.2844 0.163 Uiso 1 1 calc R . .
C18 C 0.3661(7) 0.1586(9) 0.2877(8) 0.101(4) Uani 1 1 d . . .
H18 H 0.3613 0.2038 0.3160 0.121 Uiso 1 1 calc R A .
C19 C 0.2795(6) 0.1656(6) 0.2647(6) 0.068(2) Uani 1 1 d . A .
C20 C 0.2869(6) 0.1003(6) 0.2182(5) 0.0579(18) Uani 1 1 d . . .
C21 C 0.1689(9) 0.3105(8) 0.3186(9) 0.113(4) Uani 1 1 d . . .
H21A H 0.1934 0.2812 0.3721 0.169 Uiso 1 1 calc R . .
H21B H 0.0974 0.3526 0.3286 0.169 Uiso 1 1 calc R . .
H21C H 0.2085 0.3495 0.2796 0.169 Uiso 1 1 calc R . .
C22 C -0.2387(7) 0.2370(8) 0.3202(7) 0.092(3) Uani 1 1 d . . .
H22A H -0.2900 0.2766 0.2846 0.138 Uiso 1 1 calc R . .
H22B H -0.2262 0.2797 0.3433 0.138 Uiso 1 1 calc R . .
H22C H -0.2629 0.1900 0.3664 0.138 Uiso 1 1 calc R . .
C23 C -0.1704(6) 0.4217(5) 0.1670(5) 0.0610(19) Uani 1 1 d . . .
C24 C -0.1607(6) 0.3750(5) 0.1039(5) 0.0588(18) Uani 1 1 d . . .
C25 C -0.2373(6) 0.4122(7) 0.0559(6) 0.073(2) Uani 1 1 d . . .
H25 H -0.2300 0.3819 0.0135 0.087 Uiso 1 1 calc R . .
C26 C -0.3246(8) 0.4941(8) 0.0709(7) 0.094(3) Uani 1 1 d . . .
H26 H -0.3757 0.5182 0.0383 0.112 Uiso 1 1 calc R . .
C27 C -0.3372(7) 0.5391(7) 0.1305(7) 0.085(3) Uani 1 1 d . . .
H27 H -0.3971 0.5938 0.1396 0.102 Uiso 1 1 calc R . .
C28 C -0.2605(6) 0.5048(5) 0.1802(5) 0.065(2) Uani 1 1 d . . .
C29 C -0.2715(8) 0.5525(6) 0.2446(6) 0.081(3) Uani 1 1 d . . .
H29 H -0.3324 0.6062 0.2537 0.097 Uiso 1 1 calc R . .
C30 C -0.2073(12) 0.5738(7) 0.3562(6) 0.122(5) Uani 1 1 d . . .
H30 H -0.1371 0.5721 0.3484 0.147 Uiso 1 1 calc R . .
C31 C -0.2770(11) 0.6799(8) 0.3499(8) 0.121(5) Uani 1 1 d . . .
H31A H -0.3478 0.6853 0.3575 0.145 Uiso 1 1 calc R . .
H31B H -0.2593 0.7195 0.2931 0.145 Uiso 1 1 calc R . .
C32 C -0.2683(16) 0.7202(11) 0.4170(10) 0.161(7) Uani 1 1 d . . .
H32A H -0.1989 0.7195 0.4070 0.193 Uiso 1 1 calc R . .
H32B H -0.3161 0.7886 0.4130 0.193 Uiso 1 1 calc R . .
C33 C -0.2919(14) 0.6591(12) 0.5030(10) 0.148(5) Uani 1 1 d U . .
H33A H -0.3622 0.6617 0.5135 0.178 Uiso 1 1 calc R . .
H33B H -0.2869 0.6858 0.5457 0.178 Uiso 1 1 calc R . .
C34 C -0.2201(12) 0.5547(8) 0.5114(7) 0.136(6) Uani 1 1 d . . .
H34A H -0.2366 0.5159 0.5689 0.163 Uiso 1 1 calc R . .
H34B H -0.1500 0.5517 0.5026 0.163 Uiso 1 1 calc R . .
C35 C -0.2277(10) 0.5081(7) 0.4430(6) 0.101(4) Uani 1 1 d . . .
H35 H -0.2974 0.5072 0.4540 0.121 Uiso 1 1 calc R . .
C36 C -0.1024(7) 0.3448(6) 0.5111(5) 0.075(2) Uani 1 1 d . . .
H36 H -0.1138 0.3683 0.5589 0.090 Uiso 1 1 calc R . .
C37 C -0.0345(7) 0.2459(6) 0.5106(5) 0.072(2) Uani 1 1 d . . .
C38 C 0.0120(9) 0.1897(8) 0.5825(6) 0.092(3) Uani 1 1 d . . .
H38 H -0.0045 0.2171 0.6290 0.111 Uiso 1 1 calc R . .
C39 C 0.0820(9) 0.0942(8) 0.5845(6) 0.102(4) Uani 1 1 d . . .
H39 H 0.1140 0.0567 0.6317 0.122 Uiso 1 1 calc R . .
C40 C 0.1039(9) 0.0547(7) 0.5146(6) 0.095(3) Uani 1 1 d . . .
H40 H 0.1492 -0.0109 0.5168 0.114 Uiso 1 1 calc R . .
C41 C 0.0618(7) 0.1083(6) 0.4433(5) 0.068(2) Uani 1 1 d . . .
C42 C -0.0086(6) 0.2072(5) 0.4388(5) 0.0593(19) Uani 1 1 d . . .
C43 C -0.0403(7) 0.2579(8) 0.0201(6) 0.085(3) Uani 1 1 d . . .
H43A H -0.0901 0.2327 0.0191 0.127 Uiso 1 1 calc R . .
H43B H 0.0263 0.2052 0.0206 0.127 Uiso 1 1 calc R . .
H43C H -0.0368 0.3110 -0.0299 0.127 Uiso 1 1 calc R . .
C44 C 0.1452(8) -0.0273(6) 0.3729(6) 0.089(3) Uani 1 1 d . . .
H44A H 0.2124 -0.0378 0.3801 0.133 Uiso 1 1 calc R . .
H44B H 0.1511 -0.0414 0.3197 0.133 Uiso 1 1 calc R . .
H44C H 0.1167 -0.0709 0.4197 0.133 Uiso 1 1 calc R . .
C45 C 0.1059(12) 0.4159(9) 0.0676(9) 0.152(7) Uani 1 1 d . . .
H45A H 0.1619 0.4314 0.0706 0.228 Uiso 1 1 d R . .
H45B H 0.0424 0.4556 0.0975 0.228 Uiso 1 1 d R . .
H45C H 0.1011 0.4299 0.0085 0.228 Uiso 1 1 d R . .
C46 C 0.422(2) 0.4538(19) 0.2378(17) 0.225(10) Uani 1 1 d . . .
H46A H 0.4565 0.4995 0.2288 0.270 Uiso 1 1 calc R . .
H46B H 0.3503 0.4817 0.2644 0.270 Uiso 1 1 calc R . .
Ce1 Ce 0.03084(3) 0.21898(3) 0.22995(3) 0.05217(18) Uani 1 1 d . . .
Cl1 Cl 0.4352(10) 0.4226(11) 0.1421(8) 0.375(7) Uani 1 1 d . . .
Cl2 Cl 0.4809(7) 0.3437(9) 0.2926(9) 0.409(9) Uani 1 1 d . . .
F1 F 0.2693(6) 0.1357(6) 0.8607(5) 0.129(2) Uani 1 1 d . . .
F2 F 0.3005(5) 0.2276(6) 0.9883(4) 0.114(2) Uani 1 1 d . . .
F3 F 0.3769(4) 0.0830(4) 0.9500(4) 0.105(2) Uani 1 1 d . . .
F4 F 0.2060(4) 0.1406(4) 0.9996(4) 0.1006(19) Uani 1 1 d . . .
F5 F 0.1919(4) 0.2828(4) 0.8981(4) 0.107(2) Uani 1 1 d . . .
F6 F 0.3651(4) 0.2233(4) 0.8492(4) 0.0908(16) Uani 1 1 d . . .
F7 F 0.0240(12) 0.7079(7) 0.1927(12) 0.263(8) Uani 1 1 d . . .
F8 F 0.1729(13) 0.5219(8) 0.2855(10) 0.245(7) Uani 1 1 d . . .
F9 F 0.0227(12) 0.6243(14) 0.3295(8) 0.256(8) Uani 1 1 d . . .
F10 F 0.1618(11) 0.6016(13) 0.1589(7) 0.244(6) Uani 1 1 d . . .
F11 F 0.0373(8) 0.5529(7) 0.2296(6) 0.165(3) Uani 1 1 d . . .
F12 F 0.1453(8) 0.6747(7) 0.2591(6) 0.166(4) Uani 1 1 d . . .
F13 F 0.4147(18) 0.7940(14) 0.3419(14) 0.323(10) Uani 1 1 d . . .
F14 F 0.4825(9) 0.6430(13) 0.3999(11) 0.292(9) Uani 1 1 d . . .
F15 F 0.4475(11) 0.6843(12) 0.2771(9) 0.278(9) Uani 1 1 d . . .
F16 F 0.3240(14) 0.7231(16) 0.4489(9) 0.279(8) Uani 1 1 d . . .
F17 F 0.2954(11) 0.7781(10) 0.3206(9) 0.251(7) Uani 1 1 d . . .
F18 F 0.3508(12) 0.6147(11) 0.3887(13) 0.286(9) Uani 1 1 d . . .
N1 N 0.1465(7) -0.0689(7) 0.1205(7) 0.111(3) Uani 1 1 d U . .
H1A H 0.1400 -0.0178 0.1356 0.133 Uiso 1 1 d R A .
N2 N 0.3217(5) -0.0452(5) 0.1313(5) 0.079(2) Uani 1 1 d . A .
H2A H 0.2635 0.0030 0.1384 0.094 Uiso 1 1 d R . .
N3 N -0.2048(7) 0.5274(5) 0.2901(4) 0.087(3) Uani 1 1 d . . .
H3A H -0.1511 0.4751 0.2826 0.105 Uiso 1 1 d R . .
N4 N -0.1505(6) 0.4053(5) 0.4473(4) 0.080(2) Uani 1 1 d . . .
H4A H -0.1357 0.3823 0.4029 0.096 Uiso 1 1 d R . .
O1 O 0.2055(4) 0.1094(4) 0.1945(3) 0.0593(13) Uani 1 1 d . A .
O2 O 0.1800(4) 0.2332(4) 0.2822(4) 0.0713(15) Uani 1 1 d . A .
O3 O 0.0340(4) 0.0792(4) 0.1929(4) 0.0680(14) Uani 1 1 d . A .
O4 O -0.1453(4) 0.1849(4) 0.2702(4) 0.0682(14) Uani 1 1 d . A .
O5 O -0.0962(4) 0.3850(4) 0.2117(3) 0.0635(14) Uani 1 1 d . A .
O6 O -0.0706(4) 0.2945(4) 0.0955(3) 0.0664(14) Uani 1 1 d . A .
O7 O -0.0451(4) 0.2598(4) 0.3672(3) 0.0631(13) Uani 1 1 d . A .
O8 O 0.0787(5) 0.0746(4) 0.3718(3) 0.0718(16) Uani 1 1 d . A .
O9 O 0.1241(5) 0.3151(4) 0.1054(4) 0.0796(17) Uani 1 1 d . A .
H9 H 0.1842 0.2809 0.0898 0.119 Uiso 1 1 d R . .
P1 P 0.28416(17) 0.18263(17) 0.92253(15) 0.0696(6) Uani 1 1 d . . .
P2 P 0.0910(3) 0.6146(2) 0.24353(18) 0.1051(10) Uani 1 1 d . . .
P3 P 0.3867(3) 0.7001(4) 0.3634(3) 0.1508(19) Uani 1 1 d . . .
O10 O 0.3531(19) 1.0159(18) 0.5220(15) 0.316(10) Uiso 1 1 d . . .
O11 O 0.453(2) 0.873(2) 0.5395(19) 0.376(14) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.061(5) 0.063(5) 0.071(5) -0.019(4) -0.008(4) -0.024(4)
C2 0.052(4) 0.053(4) 0.070(5) -0.020(4) -0.006(4) -0.012(3)
C3 0.049(5) 0.086(6) 0.101(7) -0.025(5) -0.011(4) -0.020(4)
C4 0.048(5) 0.106(7) 0.141(9) -0.059(7) -0.003(5) -0.032(5)
C5 0.070(6) 0.083(6) 0.135(9) -0.045(6) -0.021(6) -0.036(5)
C6 0.055(4) 0.066(5) 0.090(6) -0.034(4) -0.004(4) -0.022(4)
C7 0.059(5) 0.093(6) 0.125(8) -0.061(6) -0.004(5) -0.033(5)
C8 0.072(10) 0.022(6) 0.052(8) -0.010(6) 0.013(7) -0.010(6)
C8' 0.043(8) 0.066(10) 0.102(13) -0.043(10) -0.014(8) -0.015(7)
C9 0.089(6) 0.130(7) 0.152(8) -0.086(6) 0.001(6) -0.044(5)
C10 0.071(12) 0.110(16) 0.104(15) -0.068(14) -0.022(11) -0.005(11)
C10' 0.120(17) 0.059(10) 0.100(15) -0.062(11) 0.024(14) -0.021(11)
C11 0.136(9) 0.146(9) 0.162(9) -0.087(7) -0.010(7) -0.044(7)
C12 0.049(5) 0.097(7) 0.162(10) -0.085(7) -0.020(6) -0.001(4)
C13 0.084(6) 0.118(7) 0.167(8) -0.089(6) -0.022(6) -0.020(5)
C14 0.050(4) 0.064(5) 0.083(5) -0.029(4) -0.017(4) -0.008(3)
C15 0.054(4) 0.073(5) 0.070(5) -0.032(4) -0.003(4) -0.022(4)
C16 0.047(5) 0.147(10) 0.126(8) -0.089(8) -0.010(5) -0.020(5)
C17 0.066(7) 0.203(15) 0.197(14) -0.137(13) -0.008(8) -0.045(8)
C18 0.069(6) 0.141(9) 0.134(9) -0.091(8) -0.010(6) -0.040(6)
C19 0.055(4) 0.071(5) 0.088(5) -0.039(4) 0.001(4) -0.028(4)
C20 0.057(4) 0.063(4) 0.059(4) -0.022(4) -0.003(3) -0.027(3)
C21 0.098(8) 0.095(7) 0.180(12) -0.089(8) -0.020(8) -0.029(6)
C22 0.069(6) 0.095(7) 0.104(7) -0.050(6) 0.021(5) -0.027(5)
C23 0.071(5) 0.050(4) 0.053(4) -0.009(3) -0.004(4) -0.021(4)
C24 0.059(4) 0.057(4) 0.056(4) -0.012(3) -0.008(3) -0.019(3)
C25 0.069(5) 0.080(6) 0.079(5) -0.021(5) -0.024(4) -0.028(4)
C26 0.079(6) 0.092(7) 0.098(7) -0.014(6) -0.036(6) -0.013(5)
C27 0.072(6) 0.072(6) 0.090(6) -0.020(5) -0.018(5) -0.003(4)
C28 0.069(5) 0.050(4) 0.062(4) -0.008(4) -0.017(4) -0.011(4)
C29 0.091(6) 0.047(4) 0.071(5) -0.016(4) -0.002(5) -0.002(4)
C30 0.196(13) 0.062(5) 0.067(6) -0.032(5) -0.051(7) 0.022(7)
C31 0.144(11) 0.078(7) 0.104(8) -0.038(6) -0.019(8) 0.004(7)
C32 0.25(2) 0.107(10) 0.145(13) -0.070(10) -0.011(13) -0.068(12)
C33 0.163(9) 0.144(9) 0.134(8) -0.059(7) -0.030(7) -0.032(7)
C34 0.206(14) 0.094(8) 0.072(6) -0.048(6) -0.066(8) 0.026(8)
C35 0.131(9) 0.070(6) 0.071(6) -0.035(5) -0.015(6) 0.002(6)
C36 0.101(7) 0.067(5) 0.054(4) -0.021(4) -0.012(4) -0.024(5)
C37 0.100(6) 0.059(5) 0.058(4) -0.017(4) -0.015(4) -0.028(4)
C38 0.129(9) 0.088(7) 0.053(5) -0.017(5) -0.024(5) -0.028(6)
C39 0.134(9) 0.083(7) 0.067(5) -0.010(5) -0.047(6) -0.007(6)
C40 0.123(9) 0.065(5) 0.080(6) -0.013(5) -0.025(6) -0.018(5)
C41 0.089(6) 0.054(4) 0.049(4) -0.006(4) -0.015(4) -0.019(4)
C42 0.069(5) 0.051(4) 0.049(4) -0.008(3) -0.010(3) -0.017(3)
C43 0.068(5) 0.120(8) 0.075(5) -0.055(6) -0.004(4) -0.024(5)
C44 0.108(7) 0.049(4) 0.086(6) -0.023(4) -0.003(5) -0.012(4)
C45 0.164(13) 0.080(8) 0.148(12) 0.000(8) 0.031(10) -0.046(8)
C46 0.26(3) 0.20(2) 0.22(3) -0.05(2) -0.06(2) -0.08(2)
Ce1 0.0521(3) 0.0503(3) 0.0529(2) -0.02136(18) -0.00544(17) -0.01352(17)
Cl1 0.359(14) 0.505(19) 0.346(13) -0.268(14) 0.045(11) -0.185(13)
Cl2 0.209(8) 0.358(14) 0.52(2) 0.063(14) -0.111(11) -0.078(8)
F1 0.133(6) 0.158(6) 0.146(6) -0.079(5) -0.016(5) -0.074(5)
F2 0.093(4) 0.148(6) 0.118(5) -0.073(4) 0.001(4) -0.042(4)
F3 0.069(3) 0.080(3) 0.129(5) -0.013(3) -0.006(3) -0.011(3)
F4 0.063(3) 0.090(4) 0.112(4) -0.007(3) 0.007(3) -0.024(3)
F5 0.069(3) 0.085(4) 0.127(5) 0.000(3) -0.015(3) -0.011(3)
F6 0.070(3) 0.098(4) 0.092(3) -0.014(3) 0.000(3) -0.035(3)
F7 0.316(17) 0.105(7) 0.39(2) -0.029(9) -0.217(16) -0.013(8)
F8 0.360(19) 0.131(8) 0.289(15) 0.004(9) -0.209(15) -0.071(10)
F9 0.292(16) 0.44(2) 0.170(9) -0.187(13) 0.093(10) -0.256(17)
F10 0.263(14) 0.40(2) 0.131(7) -0.141(10) 0.015(8) -0.149(14)
F11 0.223(10) 0.174(8) 0.159(7) -0.087(6) -0.025(7) -0.099(7)
F12 0.226(10) 0.184(8) 0.154(7) -0.075(6) -0.012(7) -0.124(8)
F13 0.39(3) 0.255(18) 0.36(2) -0.075(17) 0.00(2) -0.194(19)
F14 0.122(8) 0.328(19) 0.302(18) 0.036(14) -0.072(10) -0.029(9)
F15 0.201(12) 0.253(15) 0.214(13) -0.050(11) 0.059(10) 0.001(10)
F16 0.294(19) 0.39(2) 0.165(11) -0.060(13) -0.018(12) -0.161(17)
F17 0.216(12) 0.211(12) 0.242(14) -0.106(10) -0.092(11) 0.071(10)
F18 0.251(15) 0.209(12) 0.37(2) -0.064(13) 0.069(14) -0.151(12)
N1 0.089(5) 0.126(6) 0.151(7) -0.098(5) 0.013(5) -0.044(5)
N2 0.053(4) 0.080(5) 0.120(6) -0.066(4) -0.021(4) -0.005(3)
N3 0.121(7) 0.059(4) 0.059(4) -0.025(3) -0.021(4) 0.000(4)
N4 0.110(6) 0.061(4) 0.058(4) -0.028(3) -0.011(4) -0.014(4)
O1 0.048(3) 0.055(3) 0.078(3) -0.034(2) -0.018(2) -0.003(2)
O2 0.070(3) 0.074(3) 0.086(4) -0.048(3) -0.007(3) -0.024(3)
O3 0.047(3) 0.074(3) 0.091(4) -0.040(3) 0.002(3) -0.024(2)
O4 0.061(3) 0.067(3) 0.074(3) -0.026(3) 0.000(3) -0.022(3)
O5 0.068(3) 0.059(3) 0.056(3) -0.025(2) -0.020(2) -0.001(2)
O6 0.072(3) 0.078(3) 0.058(3) -0.036(3) -0.012(3) -0.020(3)
O7 0.076(3) 0.062(3) 0.047(3) -0.021(2) -0.009(2) -0.017(3)
O8 0.092(4) 0.042(3) 0.063(3) -0.010(2) -0.008(3) -0.013(3)
O9 0.078(4) 0.067(3) 0.074(3) -0.010(3) 0.007(3) -0.027(3)
P1 0.0570(12) 0.0676(13) 0.0775(13) -0.0212(11) -0.0037(10) -0.0194(10)
P2 0.162(3) 0.0850(18) 0.0753(16) -0.0261(14) -0.0331(19) -0.0383(19)
P3 0.104(3) 0.128(3) 0.153(4) 0.024(3) -0.009(3) -0.034(2)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O3 1.303(10) . ?
C1 C6 1.408(12) . ?
C1 C2 1.421(11) . ?
C2 O4 1.369(10) . ?
C2 C3 1.396(12) . ?
C3 C4 1.403(14) . ?
C3 H3 0.9300 . ?
C4 C5 1.335(13) . ?
C4 H4 0.9300 . ?
C5 C6 1.412(12) . ?
C5 H5 0.9300 . ?
C6 C7 1.418(12) . ?
C7 N1 1.296(12) . ?
C7 H7 0.9300 . ?
C8 C13 1.317(19) . ?
C8 N1 1.607(17) . ?
C8 C9 1.69(2) . ?
C8 H8 0.9800 . ?
C8' C13 1.379(19) . ?
C8' N1 1.537(18) . ?
C8' C9 1.558(19) . ?
C8' H8' 0.9800 . ?
C9 C10 1.59(2) . ?
C9 C10' 1.69(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.430(10) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10' C11 1.27(2) . ?
C10' H10C 0.9700 . ?
C10' H10D 0.9700 . ?
C11 C12 1.464(16) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.508(13) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N2 1.447(13) . ?
C13 H13 0.9800 . ?
C14 N2 1.280(10) . ?
C14 C15 1.419(11) . ?
C14 H14 0.9300 . ?
C15 C16 1.410(12) . ?
C15 C20 1.418(11) . ?
C16 C17 1.347(15) . ?
C16 H16 0.9300 . ?
C17 C18 1.369(15) . ?
C17 H17 0.9300 . ?
C18 C19 1.379(12) . ?
C18 H18 0.9300 . ?
C19 O2 1.386(9) . ?
C19 C20 1.412(11) . ?
C20 O1 1.299(9) . ?
C21 O2 1.434(11) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 O4 1.423(10) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 O5 1.317(9) . ?
C23 C28 1.405(10) . ?
C23 C24 1.407(11) . ?
C24 O6 1.371(9) . ?
C24 C25 1.383(11) . ?
C25 C26 1.381(13) . ?
C25 H25 0.9300 . ?
C26 C27 1.324(14) . ?
C26 H26 0.9300 . ?
C27 C28 1.409(13) . ?
C27 H27 0.9300 . ?
C28 C29 1.432(13) . ?
C29 N3 1.269(13) . ?
C29 H29 0.9300 . ?
C30 C31 1.488(13) . ?
C30 N3 1.489(13) . ?
C30 C35 1.496(15) . ?
C30 H30 0.9800 . ?
C31 C32 1.512(18) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.47(2) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C34 1.473(17) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.590(14) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 N4 1.484(11) . ?
C35 H35 0.9800 . ?
C36 N4 1.316(11) . ?
C36 C37 1.410(12) . ?
C36 H36 0.9300 . ?
C37 C38 1.398(12) . ?
C37 C42 1.400(11) . ?
C38 C39 1.373(14) . ?
C38 H38 0.9300 . ?
C39 C40 1.389(14) . ?
C39 H39 0.9300 . ?
C40 C41 1.356(12) . ?
C40 H40 0.9300 . ?
C41 O8 1.377(10) . ?
C41 C42 1.410(11) . ?
C42 O7 1.322(9) . ?
C43 O6 1.428(9) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 O8 1.437(9) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 O9 1.393(12) . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 Cl2 1.62(2) . ?
C46 Cl1 1.76(3) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
Ce1 O3 2.393(6) . ?
Ce1 O1 2.398(5) . ?
Ce1 O5 2.401(5) . ?
Ce1 O7 2.403(5) . ?
Ce1 O9 2.513(5) . ?
Ce1 O4 2.678(6) . ?
Ce1 O8 2.684(5) . ?
Ce1 O2 2.685(6) . ?
Ce1 O6 2.726(5) . ?
F1 P1 1.552(7) . ?
F2 P1 1.597(7) . ?
F3 P1 1.582(6) . ?
F4 P1 1.602(6) . ?
F5 P1 1.572(5) . ?
F6 P1 1.591(6) . ?
F7 P2 1.486(10) . ?
F8 P2 1.524(11) . ?
F9 P2 1.501(10) . ?
F10 P2 1.502(11) . ?
F11 P2 1.561(9) . ?
F12 P2 1.563(9) . ?
F13 P3 1.555(17) . ?
F14 P3 1.484(12) . ?
F15 P3 1.491(14) . ?
F16 P3 1.516(16) . ?
F17 P3 1.535(11) . ?
F18 P3 1.493(13) . ?
N1 H1A 0.8600 . ?
N2 H2A 0.8600 . ?
N3 H3A 0.8600 . ?
N4 H4A 0.8599 . ?
O9 H9 0.8200 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 C1 C6 122.3(7) . . ?
O3 C1 C2 119.4(7) . . ?
C6 C1 C2 118.3(8) . . ?
O4 C2 C3 126.3(7) . . ?
O4 C2 C1 114.0(7) . . ?
C3 C2 C1 119.6(8) . . ?
C2 C3 C4 120.8(8) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 119.8(9) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 121.8(9) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C1 C6 C5 119.7(8) . . ?
C1 C6 C7 121.0(8) . . ?
C5 C6 C7 119.2(8) . . ?
N1 C7 C6 122.9(9) . . ?
N1 C7 H7 118.6 . . ?
C6 C7 H7 118.6 . . ?
C13 C8 N1 108.0(10) . . ?
C13 C8 C9 105.9(11) . . ?
N1 C8 C9 98.4(11) . . ?
C13 C8 H8 114.3 . . ?
N1 C8 H8 114.3 . . ?
C9 C8 H8 114.3 . . ?
C13 C8' N1 108.8(14) . . ?
C13 C8' C9 110.1(12) . . ?
N1 C8' C9 107.4(12) . . ?
C13 C8' H8' 110.2 . . ?
N1 C8' H8' 110.2 . . ?
C9 C8' H8' 110.2 . . ?
C8' C9 C10 104.0(13) . . ?
C8' C9 C10' 114.5(12) . . ?
C10 C9 C10' 43.9(11) . . ?
C8' C9 C8 40.9(8) . . ?
C10 C9 C8 117.5(11) . . ?
C10' C9 C8 96.7(12) . . ?
C8' C9 H9A 144.3 . . ?
C10 C9 H9A 107.9 . . ?
C10' C9 H9A 79.8 . . ?
C8 C9 H9A 107.9 . . ?
C8' C9 H9B 77.0 . . ?
C10 C9 H9B 107.9 . . ?
C10' C9 H9B 150.2 . . ?
C8 C9 H9B 107.9 . . ?
H9A C9 H9B 107.2 . . ?
C11 C10 C9 108.0(16) . . ?
C11 C10 H10A 110.1 . . ?
C9 C10 H10A 110.1 . . ?
C11 C10 H10B 110.1 . . ?
C9 C10 H10B 110.1 . . ?
H10A C10 H10B 108.4 . . ?
C11 C10' C9 110.9(15) . . ?
C11 C10' H10C 109.5 . . ?
C9 C10' H10C 109.5 . . ?
C11 C10' H10D 109.5 . . ?
C9 C10' H10D 109.5 . . ?
H10C C10' H10D 108.0 . . ?
C10' C11 C10 53.7(15) . . ?
C10' C11 C12 114.2(16) . . ?
C10 C11 C12 119.0(13) . . ?
C10' C11 H11A 138.1 . . ?
C10 C11 H11A 107.6 . . ?
C12 C11 H11A 107.6 . . ?
C10' C11 H11B 57.9 . . ?
C10 C11 H11B 107.6 . . ?
C12 C11 H11B 107.6 . . ?
H11A C11 H11B 107.0 . . ?
C11 C12 C13 115.5(10) . . ?
C11 C12 H12A 108.4 . . ?
C13 C12 H12A 108.4 . . ?
C11 C12 H12B 108.4 . . ?
C13 C12 H12B 108.4 . . ?
H12A C12 H12B 107.5 . . ?
C8 C13 C8' 50.0(11) . . ?
C8 C13 N2 115.9(12) . . ?
C8' C13 N2 120.2(10) . . ?
C8 C13 C12 117.1(11) . . ?
C8' C13 C12 121.4(11) . . ?
N2 C13 C12 115.4(9) . . ?
C8 C13 H13 101.5 . . ?
C8' C13 H13 51.5 . . ?
N2 C13 H13 101.5 . . ?
C12 C13 H13 101.5 . . ?
N2 C14 C15 123.3(7) . . ?
N2 C14 H14 118.3 . . ?
C15 C14 H14 118.3 . . ?
C16 C15 C20 120.1(8) . . ?
C16 C15 C14 119.5(8) . . ?
C20 C15 C14 120.3(7) . . ?
C17 C16 C15 119.4(9) . . ?
C17 C16 H16 120.3 . . ?
C15 C16 H16 120.3 . . ?
C16 C17 C18 122.2(10) . . ?
C16 C17 H17 118.9 . . ?
C18 C17 H17 118.9 . . ?
C17 C18 C19 120.1(9) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C18 C19 O2 126.5(8) . . ?
C18 C19 C20 120.4(8) . . ?
O2 C19 C20 113.1(7) . . ?
O1 C20 C19 120.0(7) . . ?
O1 C20 C15 122.3(7) . . ?
C19 C20 C15 117.6(7) . . ?
O2 C21 H21A 109.5 . . ?
O2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O4 C22 H22A 109.5 . . ?
O4 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
O4 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O5 C23 C28 123.1(7) . . ?
O5 C23 C24 119.0(7) . . ?
C28 C23 C24 117.9(8) . . ?
O6 C24 C25 125.8(7) . . ?
O6 C24 C23 114.0(7) . . ?
C25 C24 C23 120.2(7) . . ?
C26 C25 C24 120.0(9) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C27 C26 C25 121.6(9) . . ?
C27 C26 H26 119.2 . . ?
C25 C26 H26 119.2 . . ?
C26 C27 C28 120.4(9) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 H27 119.8 . . ?
C23 C28 C27 119.9(8) . . ?
C23 C28 C29 118.3(8) . . ?
C27 C28 C29 121.7(8) . . ?
N3 C29 C28 125.2(8) . . ?
N3 C29 H29 117.4 . . ?
C28 C29 H29 117.4 . . ?
C31 C30 N3 116.1(9) . . ?
C31 C30 C35 112.7(10) . . ?
N3 C30 C35 108.4(10) . . ?
C31 C30 H30 106.4 . . ?
N3 C30 H30 106.4 . . ?
C35 C30 H30 106.4 . . ?
C30 C31 C32 111.1(12) . . ?
C30 C31 H31A 109.4 . . ?
C32 C31 H31A 109.4 . . ?
C30 C31 H31B 109.4 . . ?
C32 C31 H31B 109.4 . . ?
H31A C31 H31B 108.0 . . ?
C33 C32 C31 109.9(13) . . ?
C33 C32 H32A 109.7 . . ?
C31 C32 H32A 109.7 . . ?
C33 C32 H32B 109.7 . . ?
C31 C32 H32B 109.7 . . ?
H32A C32 H32B 108.2 . . ?
C32 C33 C34 111.0(14) . . ?
C32 C33 H33A 109.4 . . ?
C34 C33 H33A 109.4 . . ?
C32 C33 H33B 109.4 . . ?
C34 C33 H33B 109.4 . . ?
H33A C33 H33B 108.0 . . ?
C33 C34 C35 110.7(10) . . ?
C33 C34 H34A 109.5 . . ?
C35 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C35 C34 H34B 109.5 . . ?
H34A C34 H34B 108.1 . . ?
N4 C35 C30 110.0(8) . . ?
N4 C35 C34 110.8(9) . . ?
C30 C35 C34 107.1(10) . . ?
N4 C35 H35 109.6 . . ?
C30 C35 H35 109.6 . . ?
C34 C35 H35 109.6 . . ?
N4 C36 C37 123.2(8) . . ?
N4 C36 H36 118.4 . . ?
C37 C36 H36 118.4 . . ?
C38 C37 C42 120.9(8) . . ?
C38 C37 C36 117.4(8) . . ?
C42 C37 C36 121.6(8) . . ?
C39 C38 C37 120.2(9) . . ?
C39 C38 H38 119.9 . . ?
C37 C38 H38 119.9 . . ?
C38 C39 C40 118.6(9) . . ?
C38 C39 H39 120.7 . . ?
C40 C39 H39 120.7 . . ?
C41 C40 C39 122.4(9) . . ?
C41 C40 H40 118.8 . . ?
C39 C40 H40 118.8 . . ?
C40 C41 O8 126.0(8) . . ?
C40 C41 C42 120.2(8) . . ?
O8 C41 C42 113.8(7) . . ?
O7 C42 C37 123.1(7) . . ?
O7 C42 C41 119.3(7) . . ?
C37 C42 C41 117.6(7) . . ?
O6 C43 H43A 109.5 . . ?
O6 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
O6 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O8 C44 H44A 109.5 . . ?
O8 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
O8 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O9 C45 H45A 109.3 . . ?
O9 C45 H45B 109.7 . . ?
H45A C45 H45B 109.5 . . ?
O9 C45 H45C 109.4 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
Cl2 C46 Cl1 98.7(15) . . ?
Cl2 C46 H46A 112.0 . . ?
Cl1 C46 H46A 112.0 . . ?
Cl2 C46 H46B 112.0 . . ?
Cl1 C46 H46B 112.0 . . ?
H46A C46 H46B 109.7 . . ?
O3 Ce1 O1 69.62(17) . . ?
O3 Ce1 O5 128.00(18) . . ?
O1 Ce1 O5 148.9(2) . . ?
O3 Ce1 O7 125.43(19) . . ?
O1 Ce1 O7 123.99(17) . . ?
O5 Ce1 O7 70.32(17) . . ?
O3 Ce1 O9 110.1(2) . . ?
O1 Ce1 O9 71.57(19) . . ?
O5 Ce1 O9 77.80(19) . . ?
O7 Ce1 O9 124.4(2) . . ?
O3 Ce1 O4 61.99(17) . . ?
O1 Ce1 O4 129.58(17) . . ?
O5 Ce1 O4 77.94(19) . . ?
O7 Ce1 O4 77.67(19) . . ?
O9 Ce1 O4 137.8(2) . . ?
O3 Ce1 O8 78.91(19) . . ?
O1 Ce1 O8 72.34(18) . . ?
O5 Ce1 O8 131.37(17) . . ?
O7 Ce1 O8 61.60(16) . . ?
O9 Ce1 O8 136.3(2) . . ?
O4 Ce1 O8 85.05(18) . . ?
O3 Ce1 O2 127.88(17) . . ?
O1 Ce1 O2 61.50(17) . . ?
O5 Ce1 O2 103.70(18) . . ?
O7 Ce1 O2 73.85(18) . . ?
O9 Ce1 O2 71.1(2) . . ?
O4 Ce1 O2 148.81(18) . . ?
O8 Ce1 O2 70.42(19) . . ?
O3 Ce1 O6 73.42(18) . . ?
O1 Ce1 O6 112.14(17) . . ?
O5 Ce1 O6 60.71(16) . . ?
O7 Ce1 O6 123.87(17) . . ?
O9 Ce1 O6 70.8(2) . . ?
O4 Ce1 O6 67.23(17) . . ?
O8 Ce1 O6 147.56(19) . . ?
O2 Ce1 O6 141.16(18) . . ?
C7 N1 C8' 126.8(10) . . ?
C7 N1 C8 124.8(10) . . ?
C8' N1 C8 42.5(8) . . ?
C7 N1 H1A 115.8 . . ?
C8' N1 H1A 110.2 . . ?
C8 N1 H1A 116.5 . . ?
C14 N2 C13 126.6(8) . . ?
C14 N2 H2A 116.7 . . ?
C13 N2 H2A 116.6 . . ?
C29 N3 C30 129.4(9) . . ?
C29 N3 H3A 115.2 . . ?
C30 N3 H3A 115.4 . . ?
C36 N4 C35 127.7(7) . . ?
C36 N4 H4A 116.1 . . ?
C35 N4 H4A 116.2 . . ?
C20 O1 Ce1 127.8(5) . . ?
C19 O2 C21 116.2(7) . . ?
C19 O2 Ce1 117.3(5) . . ?
C21 O2 Ce1 126.1(6) . . ?
C1 O3 Ce1 126.7(5) . . ?
C2 O4 C22 118.7(7) . . ?
C2 O4 Ce1 116.2(4) . . ?
C22 O4 Ce1 124.9(6) . . ?
C23 O5 Ce1 126.0(5) . . ?
C24 O6 C43 118.4(6) . . ?
C24 O6 Ce1 114.8(4) . . ?
C43 O6 Ce1 126.8(5) . . ?
C42 O7 Ce1 124.6(4) . . ?
C41 O8 C44 117.5(7) . . ?
C41 O8 Ce1 114.7(4) . . ?
C44 O8 Ce1 125.1(5) . . ?
C45 O9 Ce1 134.9(6) . . ?
C45 O9 H9 110.8 . . ?
Ce1 O9 H9 112.7 . . ?
F1 P1 F5 92.3(4) . . ?
F1 P1 F3 89.7(4) . . ?
F5 P1 F3 178.0(4) . . ?
F1 P1 F6 91.0(4) . . ?
F5 P1 F6 91.8(3) . . ?
F3 P1 F6 88.7(3) . . ?
F1 P1 F2 178.2(5) . . ?
F5 P1 F2 89.2(4) . . ?
F3 P1 F2 88.8(4) . . ?
F6 P1 F2 90.0(4) . . ?
F1 P1 F4 91.1(4) . . ?
F5 P1 F4 89.8(3) . . ?
F3 P1 F4 89.7(3) . . ?
F6 P1 F4 177.2(4) . . ?
F2 P1 F4 87.8(4) . . ?
F7 P2 F9 96.2(10) . . ?
F7 P2 F10 85.7(9) . . ?
F9 P2 F10 178.1(11) . . ?
F7 P2 F8 171.5(11) . . ?
F9 P2 F8 91.1(9) . . ?
F10 P2 F8 87.0(9) . . ?
F7 P2 F11 90.9(7) . . ?
F9 P2 F11 92.1(6) . . ?
F10 P2 F11 87.8(6) . . ?
F8 P2 F11 93.2(6) . . ?
F7 P2 F12 90.1(7) . . ?
F9 P2 F12 87.3(6) . . ?
F10 P2 F12 92.7(7) . . ?
F8 P2 F12 85.8(7) . . ?
F11 P2 F12 178.8(6) . . ?
F14 P3 F15 89.7(9) . . ?
F14 P3 F18 95.8(10) . . ?
F15 P3 F18 96.8(12) . . ?
F14 P3 F16 91.6(10) . . ?
F15 P3 F16 176.3(11) . . ?
F18 P3 F16 86.5(9) . . ?
F14 P3 F17 167.6(11) . . ?
F15 P3 F17 89.1(8) . . ?
F18 P3 F17 96.6(11) . . ?
F16 P3 F17 88.8(9) . . ?
F14 P3 F13 86.9(12) . . ?
F15 P3 F13 87.6(10) . . ?
F18 P3 F13 174.8(11) . . ?
F16 P3 F13 89.1(12) . . ?
F17 P3 F13 80.7(10) . . ?
_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.124
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.109