#\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-01-15 at 14:16:59 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\program files\wingx\files\archive.dat # CIF files read : mk108 import struct data_mk108 _audit_creation_date 2010-01-15T14:16:59-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common mk108 _chemical_formula_moiety 'C42 H70 Ce2 N26 O17 W2' _chemical_formula_sum 'C42 H60 Ce2 N26 O17 W2' _chemical_formula_weight 1849.1 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Cmca _symmetry_space_group_name_Hall '-C 2ac 2' _symmetry_Int_Tables_number 64 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x, -y, -z' '-x+1/2, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' 'x+1/2, -y+1/2, -z' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x, y, z' 'x-1/2, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' '-x+1/2, y+1/2, z' 'x, -y+1/2, z-1/2' _cell_length_a 19.362(5) _cell_length_b 19.545(5) _cell_length_c 18.653(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 7059(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 26730 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 34.972 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.74 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3576 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.589 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details '(DENZO-SMN; Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.3933 _exptl_absorpt_correction_T_max 0.4922 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.0279295 _diffrn_orient_matrix_ub_12 -0.0356838 _diffrn_orient_matrix_ub_13 -0.0247818 _diffrn_orient_matrix_ub_21 0.0154246 _diffrn_orient_matrix_ub_22 -0.0191009 _diffrn_orient_matrix_ub_23 0.0448874 _diffrn_orient_matrix_ub_31 -0.0420996 _diffrn_orient_matrix_ub_32 -0.0331896 _diffrn_orient_matrix_ub_33 0.0003434 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_unetI/netI 0.0256 _diffrn_reflns_number 45230 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 34.96 _diffrn_reflns_theta_full 34.96 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 7929 _reflns_number_gt 6422 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0372P)^2^+13.1911P] 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_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.000185(19) _refine_ls_number_reflns 7929 _refine_ls_number_parameters 216 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.046 _refine_ls_R_factor_gt 0.031 _refine_ls_wR_factor_ref 0.0774 _refine_ls_wR_factor_gt 0.0713 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.978 _refine_diff_density_min -1.367 _refine_diff_density_rms 0.144 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' W W -0.849 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 W1 W 0.75 -0.065802(6) 0.25 0.02124(4) Uani 1 2 d S . . Ce2 Ce 0.5 0.173757(9) 0.443369(10) 0.02186(5) Uani 1 2 d S . . C1 C 0.80419(16) -0.03305(15) 0.34490(16) 0.0383(6) Uani 1 1 d . . . N1 N 0.83443(19) -0.01627(19) 0.39469(17) 0.0632(9) Uani 1 1 d . . . C2 C 0.80706(14) 0.02371(14) 0.21705(15) 0.0346(5) Uani 1 1 d . . . N2 N 0.83651(16) 0.07173(15) 0.19991(17) 0.0522(7) Uani 1 1 d . . . C3 C 0.70524(18) -0.15450(16) 0.19872(17) 0.0440(7) Uani 1 1 d . . . N3 N 0.6799(2) -0.20068(17) 0.1721(2) 0.0737(11) Uani 1 1 d . . . C4 C 0.66794(16) -0.09729(15) 0.32038(17) 0.0411(6) Uani 1 1 d . . . N4 N 0.62244(18) -0.11282(18) 0.35603(19) 0.0671(9) Uani 1 1 d . . . O11 O 0.58890(17) 0.24154(16) 0.50624(13) 0.0697(9) Uani 1 1 d . . . C12 C 0.6067(2) 0.2630(2) 0.5650(2) 0.0618(10) Uani 1 1 d . . . H12 H 0.5818 0.2476 0.6045 0.074 Uiso 1 1 calc R . . N13 N 0.65687(18) 0.30505(16) 0.5771(2) 0.0576(8) Uani 1 1 d . . . C14 C 0.6759(4) 0.3247(3) 0.6500(3) 0.103(2) Uani 1 1 d . . . H14A H 0.7139 0.3562 0.6484 0.154 Uiso 1 1 calc R . . H14B H 0.6891 0.2847 0.6765 0.154 Uiso 1 1 calc R . . H14C H 0.6371 0.3461 0.673 0.154 Uiso 1 1 calc R . . C15 C 0.6975(4) 0.3337(4) 0.5211(4) 0.133(3) Uani 1 1 d . . . H15A H 0.7318 0.3635 0.5412 0.199 Uiso 1 1 calc R . . H15B H 0.6683 0.3593 0.4893 0.199 Uiso 1 1 calc R . . H15C H 0.7198 0.2976 0.4949 0.199 Uiso 1 1 calc R . . O21 O 0.5 0.09519(17) 0.33709(18) 0.0459(7) Uani 1 2 d S . . C22 C 0.5 0.0379(3) 0.3106(3) 0.0492(11) Uani 1 2 d S . . H22 H 0.5 0.0014 0.3426 0.059 Uiso 1 2 calc SR . . N23 N 0.5 0.0224(3) 0.2433(2) 0.0541(11) Uani 1 2 d S . . C24 C 0.5 0.0736(4) 0.1882(4) 0.100(3) Uani 1 2 d S . . H24A H 0.5 0.0518 0.1421 0.149 Uiso 1 2 calc SR . . H24B H 0.5405 0.1016 0.1929 0.149 Uiso 0.5 1 calc PR . . H24C H 0.4595 0.1016 0.1929 0.149 Uiso 0.5 1 calc PR . . C25 C 0.5 -0.0489(4) 0.2193(4) 0.079(2) Uani 1 2 d S . . H25A H 0.5 -0.0503 0.1678 0.119 Uiso 1 2 calc SR . . H25B H 0.4595 -0.0716 0.2371 0.119 Uiso 0.5 1 calc PR . . H25C H 0.5405 -0.0716 0.2371 0.119 Uiso 0.5 1 calc PR . . C31 C 0.46140(15) 0 0.5 0.0222(5) Uani 1 2 d S . . N32 N 0.42986(10) 0.05684(10) 0.47663(12) 0.0261(4) Uani 1 1 d . . . C33 C 0.36053(12) 0.05577(13) 0.47720(15) 0.0315(5) Uani 1 1 d . . . H33 H 0.3368 0.0943 0.4615 0.038 Uiso 1 1 calc R . . C34 C 0.32317(17) 0 0.5 0.0320(7) Uani 1 2 d S . . 34 H 0.2751 0 0.5 0.038 Uiso 1 2 calc SR . . O4 O 0.5 0.14695(16) 0.57661(15) 0.0371(6) Uani 1 2 d S . . H4A H 0.5369 0.1311 0.6037 0.079(14) Uiso 1 1 d R . . O5 O 0.60703(13) 0.18287(10) 0.37099(15) 0.0511(7) Uani 1 1 d . . . H5A H 0.6264 0.1472 0.346 0.061 Uiso 1 1 d R . . H5B H 0.6321 0.2222 0.3629 0.061 Uiso 1 1 d R . . O6 O 0.5 0.29362(18) 0.3882(2) 0.0697(12) Uani 1 2 d S . . O7 O 0.9365(4) 0 0.5 0.064(2) Uiso 0.5 2 d SP . . O8 O 0.5423(4) 0.4051(4) 0.4670(4) 0.0835(19) Uiso 0.5 1 d P . . 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 W1 0.02103(6) 0.01961(6) 0.02307(7) 0 0.00236(4) 0 Ce2 0.02355(8) 0.01677(7) 0.02527(8) 0.00200(6) 0 0 C1 0.0411(14) 0.0363(14) 0.0375(14) -0.0021(11) -0.0037(11) -0.0040(11) N1 0.071(2) 0.070(2) 0.0484(17) -0.0100(15) -0.0193(15) -0.0094(17) C2 0.0330(12) 0.0317(12) 0.0392(14) 0.0002(10) 0.0089(10) -0.0031(10) N2 0.0528(17) 0.0404(14) 0.0634(19) 0.0056(13) 0.0174(14) -0.0138(12) C3 0.0557(18) 0.0344(14) 0.0417(16) -0.0004(12) -0.0089(14) -0.0107(13) N3 0.105(3) 0.0456(17) 0.070(2) -0.0072(16) -0.027(2) -0.0260(19) C4 0.0431(15) 0.0358(15) 0.0444(16) 0.0019(12) 0.0131(12) -0.0072(12) N4 0.065(2) 0.066(2) 0.071(2) 0.0071(17) 0.0329(17) -0.0185(16) O11 0.080(2) 0.083(2) 0.0461(14) -0.0059(13) -0.0071(12) -0.0516(16) C12 0.074(3) 0.055(2) 0.056(2) -0.0020(17) -0.0063(18) -0.0271(19) N13 0.0574(18) 0.0470(16) 0.068(2) -0.0095(14) -0.0185(16) -0.0152(14) C14 0.120(5) 0.087(4) 0.101(4) -0.033(3) -0.054(4) -0.007(3) C15 0.116(5) 0.150(6) 0.132(6) -0.013(5) 0.016(5) -0.091(5) O21 0.0427(16) 0.0460(18) 0.0491(18) -0.0164(14) 0 0 C22 0.045(2) 0.056(3) 0.047(3) -0.011(2) 0 0 N23 0.043(2) 0.077(3) 0.043(2) -0.022(2) 0 0 C24 0.139(8) 0.088(6) 0.072(5) -0.009(4) 0 0 C25 0.086(5) 0.078(4) 0.074(4) -0.034(4) 0 0 C31 0.0207(12) 0.0195(12) 0.0264(14) 0.0029(10) 0 0 N32 0.0215(8) 0.0214(9) 0.0353(10) 0.0071(7) -0.0013(7) 0.0020(7) C33 0.0219(10) 0.0290(12) 0.0435(14) 0.0075(10) -0.0018(9) 0.0044(8) C34 0.0186(13) 0.0343(17) 0.043(2) 0.0072(15) 0 0 O4 0.0307(13) 0.0506(17) 0.0299(13) 0.0099(12) 0 0 O5 0.0534(13) 0.0274(10) 0.0724(17) -0.0077(9) 0.0369(13) -0.0094(8) O6 0.113(4) 0.0298(16) 0.066(2) 0.0154(16) 0 0 #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 W1 C4 2.151(3) 4_655 ? W1 C4 2.151(3) . ? W1 C1 2.155(3) . ? W1 C1 2.155(3) 4_655 ? W1 C2 2.158(3) . ? W1 C2 2.158(3) 4_655 ? W1 C3 2.161(3) 4_655 ? W1 C3 2.161(3) . ? Ce2 O11 2.469(2) . ? Ce2 O11 2.469(2) 11_655 ? Ce2 O5 2.480(2) 11_655 ? Ce2 O5 2.480(2) . ? Ce2 O21 2.508(3) . ? Ce2 O4 2.540(3) . ? Ce2 O6 2.559(3) . ? Ce2 N32 2.730(2) . ? Ce2 N32 2.730(2) 11_655 ? C1 N1 1.146(4) . ? C2 N2 1.144(4) . ? C3 N3 1.140(4) . ? C4 N4 1.145(4) . ? O11 C12 1.222(4) . ? C12 N13 1.293(5) . ? C12 H12 0.93 . ? N13 C15 1.423(7) . ? N13 C14 1.460(6) . ? C14 H14A 0.96 . ? C14 H14B 0.96 . ? C14 H14C 0.96 . ? C15 H15A 0.96 . ? C15 H15B 0.96 . ? C15 H15C 0.96 . ? O21 C22 1.223(6) . ? C22 N23 1.292(6) . ? C22 H22 0.93 . ? N23 C24 1.433(10) . ? N23 C25 1.465(8) . ? C24 H24A 0.96 . ? C24 H24B 0.96 . ? C24 H24C 0.96 . ? C25 H25A 0.96 . ? C25 H25B 0.96 . ? C25 H25C 0.96 . ? C31 N32 1.341(2) 3_556 ? C31 N32 1.341(2) . ? C31 C31 1.495(6) 9_656 ? N32 C33 1.342(3) . ? C33 C34 1.376(3) . ? C33 H33 0.93 . ? C34 C33 1.376(3) 3_556 ? C34 34 0.93 . ? O4 H4A 0.9283 . ? O5 H5A 0.9178 . ? O5 H5B 0.9225 . ? O8 O8 1.636(14) 11_655 ? 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 C4 W1 C4 146.75(16) 4_655 . ? C4 W1 C1 103.10(12) 4_655 . ? C4 W1 C1 86.75(12) . . ? C4 W1 C1 86.75(12) 4_655 4_655 ? C4 W1 C1 103.10(12) . 4_655 ? C1 W1 C1 145.44(16) . 4_655 ? C4 W1 C2 71.34(11) 4_655 . ? C4 W1 C2 141.61(11) . . ? C1 W1 C2 75.17(11) . . ? C1 W1 C2 76.97(11) 4_655 . ? C4 W1 C2 141.61(11) 4_655 4_655 ? C4 W1 C2 71.34(11) . 4_655 ? C1 W1 C2 76.97(11) . 4_655 ? C1 W1 C2 75.17(11) 4_655 4_655 ? C2 W1 C2 71.71(15) . 4_655 ? C4 W1 C3 75.19(13) 4_655 4_655 ? C4 W1 C3 78.26(13) . 4_655 ? C1 W1 C3 71.30(12) . 4_655 ? C1 W1 C3 142.84(12) 4_655 4_655 ? C2 W1 C3 124.81(13) . 4_655 ? C2 W1 C3 136.83(12) 4_655 4_655 ? C4 W1 C3 78.26(13) 4_655 . ? C4 W1 C3 75.19(13) . . ? C1 W1 C3 142.84(12) . . ? C1 W1 C3 71.30(12) 4_655 . ? C2 W1 C3 136.83(12) . . ? C2 W1 C3 124.81(13) 4_655 . ? C3 W1 C3 73.34(18) 4_655 . ? O11 Ce2 O11 88.43(17) . 11_655 ? O11 Ce2 O5 143.40(10) . 11_655 ? O11 Ce2 O5 68.74(9) 11_655 11_655 ? O11 Ce2 O5 68.74(9) . . ? O11 Ce2 O5 143.40(10) 11_655 . ? O5 Ce2 O5 113.38(14) 11_655 . ? O11 Ce2 O21 134.77(8) . . ? O11 Ce2 O21 134.77(8) 11_655 . ? O5 Ce2 O21 67.27(7) 11_655 . ? O5 Ce2 O21 67.27(7) . . ? O11 Ce2 O4 69.26(8) . . ? O11 Ce2 O4 69.26(8) 11_655 . ? O5 Ce2 O4 123.20(7) 11_655 . ? O5 Ce2 O4 123.20(7) . . ? O21 Ce2 O4 130.33(11) . . ? O11 Ce2 O6 72.52(10) . . ? O11 Ce2 O6 72.52(10) 11_655 . ? O5 Ce2 O6 73.46(7) 11_655 . ? O5 Ce2 O6 73.46(7) . . ? O21 Ce2 O6 104.05(13) . . ? O4 Ce2 O6 125.62(12) . . ? O11 Ce2 N32 133.49(8) . . ? O11 Ce2 N32 89.68(10) 11_655 . ? O5 Ce2 N32 76.59(7) 11_655 . ? O5 Ce2 N32 126.84(6) . . ? O21 Ce2 N32 70.55(9) . . ? O4 Ce2 N32 66.73(8) . . ? O6 Ce2 N32 149.08(5) . . ? O11 Ce2 N32 89.68(10) . 11_655 ? O11 Ce2 N32 133.49(8) 11_655 11_655 ? O5 Ce2 N32 126.85(6) 11_655 11_655 ? O5 Ce2 N32 76.59(7) . 11_655 ? O21 Ce2 N32 70.55(9) . 11_655 ? O4 Ce2 N32 66.73(8) . 11_655 ? O6 Ce2 N32 149.08(5) . 11_655 ? N32 Ce2 N32 59.67(8) . 11_655 ? N1 C1 W1 178.4(3) . . ? N2 C2 W1 179.0(3) . . ? N3 C3 W1 178.2(4) . . ? N4 C4 W1 177.3(3) . . ? C12 O11 Ce2 143.7(3) . . ? O11 C12 N13 125.9(4) . . ? O11 C12 H12 117.1 . . ? N13 C12 H12 117.1 . . ? C12 N13 C15 122.5(4) . . ? C12 N13 C14 121.3(4) . . ? C15 N13 C14 116.2(4) . . ? N13 C14 H14A 109.5 . . ? N13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N13 C15 H15A 109.5 . . ? N13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C22 O21 Ce2 151.5(4) . . ? O21 C22 N23 127.3(6) . . ? O21 C22 H22 116.3 . . ? N23 C22 H22 116.3 . . ? C22 N23 C24 122.2(6) . . ? C22 N23 C25 121.4(6) . . ? C24 N23 C25 116.4(5) . . ? N23 C24 H24A 109.5 . . ? N23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N23 C25 H25A 109.5 . . ? N23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N32 C31 N32 125.8(3) 3_556 . ? N32 C31 C31 117.11(14) 3_556 9_656 ? N32 C31 C31 117.11(14) . 9_656 ? C31 N32 C33 116.1(2) . . ? C31 N32 Ce2 122.75(16) . . ? C33 N32 Ce2 120.81(15) . . ? N32 C33 C34 122.7(2) . . ? N32 C33 H33 118.6 . . ? C34 C33 H33 118.6 . . ? C33 C34 C33 116.5(3) . 3_556 ? C33 C34 34 121.7 . . ? C33 C34 34 121.7 3_556 . ? Ce2 O4 H4A 127 . . ? Ce2 O5 H5A 124.2 . . ? Ce2 O5 H5B 126.2 . . ? H5A O5 H5B 109.6 . . ? 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 O11 Ce2 O11 C12 48.6(6) 11_655 . . . ? O5 Ce2 O11 C12 98.4(6) 11_655 . . . ? O5 Ce2 O11 C12 -160.6(6) . . . . ? O21 Ce2 O11 C12 -146.6(5) . . . . ? O4 Ce2 O11 C12 -19.8(5) . . . . ? O6 Ce2 O11 C12 120.8(6) . . . . ? N32 Ce2 O11 C12 -39.5(6) . . . . ? N32 Ce2 O11 C12 -84.9(6) 11_655 . . . ? Ce2 O11 C12 N13 -173.1(3) . . . . ? O11 C12 N13 C15 1.8(8) . . . . ? O11 C12 N13 C14 -176.9(5) . . . . ? O11 Ce2 O21 C22 100.83(13) . . . . ? O11 Ce2 O21 C22 -100.83(13) 11_655 . . . ? O5 Ce2 O21 C22 -115.03(7) 11_655 . . . ? O5 Ce2 O21 C22 115.03(7) . . . . ? O4 Ce2 O21 C22 0.000(3) . . . . ? O6 Ce2 O21 C22 180.000(2) . . . . ? N32 Ce2 O21 C22 -31.85(5) . . . . ? N32 Ce2 O21 C22 31.85(5) 11_655 . . . ? Ce2 O21 C22 N23 180 . . . . ? O21 C22 N23 C24 0.000(2) . . . . ? O21 C22 N23 C25 180.0000(10) . . . . ? N32 C31 N32 C33 0.11(18) 3_556 . . . ? C31 C31 N32 C33 -179.89(18) 9_656 . . . ? N32 C31 N32 Ce2 173.56(17) 3_556 . . . ? C31 C31 N32 Ce2 -6.44(17) 9_656 . . . ? O11 Ce2 N32 C31 -49.1(2) . . . . ? O11 Ce2 N32 C31 -136.59(16) 11_655 . . . ? O5 Ce2 N32 C31 155.22(17) 11_655 . . . ? O5 Ce2 N32 C31 45.88(19) . . . . ? O21 Ce2 N32 C31 84.92(15) . . . . ? O4 Ce2 N32 C31 -69.11(15) . . . . ? O6 Ce2 N32 C31 169.8(2) . . . . ? N32 Ce2 N32 C31 6.61(17) 11_655 . . . ? O11 Ce2 N32 C33 124.1(2) . . . . ? O11 Ce2 N32 C33 36.6(2) 11_655 . . . ? O5 Ce2 N32 C33 -31.6(2) 11_655 . . . ? O5 Ce2 N32 C33 -141.0(2) . . . . ? O21 Ce2 N32 C33 -101.9(2) . . . . ? O4 Ce2 N32 C33 104.0(2) . . . . ? O6 Ce2 N32 C33 -17.0(3) . . . . ? N32 Ce2 N32 C33 179.76(19) 11_655 . . . ? C31 N32 C33 C34 -0.2(4) . . . . ? Ce2 N32 C33 C34 -173.81(16) . . . . ? N32 C33 C34 C33 0.12(19) . . . 3_556 ?