# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p103 #TrackingRef 'submit-103.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H76 Cd Cl16 N24 O29 Zn4' _chemical_formula_weight 2250.29 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 10.5123(7) _cell_length_b 15.0065(10) _cell_length_c 15.3954(16) _cell_angle_alpha 113.108(3) _cell_angle_beta 107.716(3) _cell_angle_gamma 98.386(2) _cell_volume 2028.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.843 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 2.039 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6514 _exptl_absorpt_correction_T_max 0.7105 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20696 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7021 _reflns_number_gt 6118 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.1026P)^2^+67.4450P] 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 7021 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1177 _refine_ls_R_factor_gt 0.1108 _refine_ls_wR_factor_ref 0.3226 _refine_ls_wR_factor_gt 0.3192 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _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 Zn1 Zn 0.11446(16) 0.33684(11) 0.67495(12) 0.0310(4) Uani 1 1 d . . . Zn2 Zn 0.31090(16) 0.59371(11) 1.28726(12) 0.0310(4) Uani 1 1 d . . . Cl1 Cl 0.0256(4) 0.1673(2) 0.6027(3) 0.0389(8) Uani 1 1 d . . . Cl2 Cl -0.0059(4) 0.4231(3) 0.6107(3) 0.0417(8) Uani 1 1 d . . . Cl3 Cl 0.1934(4) 0.4096(3) 0.8468(3) 0.0397(8) Uani 1 1 d . . . Cl4 Cl 0.2917(12) 0.3613(13) 0.6510(11) 0.190(6) Uani 1 1 d . . . Cl5 Cl 0.4035(4) 0.5659(3) 1.1687(3) 0.0441(9) Uani 1 1 d . . . Cl6 Cl 0.3100(4) 0.7563(3) 1.3548(3) 0.0439(9) Uani 1 1 d . . . Cl7 Cl 0.4148(6) 0.5430(4) 1.4012(4) 0.0672(13) Uani 1 1 d . . . Cl8 Cl 0.1157(12) 0.4962(9) 1.2161(11) 0.174(5) Uani 1 1 d . . . O1W O 0.9962(9) 0.2100(7) 1.0218(7) 0.032(2) Uani 1 1 d . . . O2W O 0.9447(9) -0.0812(7) 0.8350(7) 0.035(2) Uani 1 1 d . . . O3W O 0.9419(9) 0.2336(7) 0.8268(7) 0.037(2) Uani 1 1 d . . . O4W O 0.8281(10) 0.0252(8) 0.6663(7) 0.043(2) Uani 1 1 d . . . O5W O 0.8126(12) 0.0191(8) 0.9687(8) 0.051(3) Uani 1 1 d . . . Cd1 Cd 0.8774(2) 0.07154(18) 0.84617(18) 0.0447(6) Uani 0.50 1 d P . . C1 C 0.5942(12) 0.1721(9) 0.8466(9) 0.022(2) Uani 1 1 d . . . C2 C 0.3609(11) 0.1507(8) 0.7554(8) 0.017(2) Uani 1 1 d . . . H2 H 0.3256 0.1694 0.6996 0.020 Uiso 1 1 calc R . . C3 C 0.4144(11) 0.2442(8) 0.8627(9) 0.021(2) Uani 1 1 d . . . H3 H 0.4155 0.3082 0.8579 0.026 Uiso 1 1 calc R . . C4 C 0.2191(11) 0.1276(8) 0.8407(9) 0.020(2) Uani 1 1 d . . . C5 C 0.6584(12) 0.3275(9) 1.0084(9) 0.024(2) Uani 1 1 d . . . H5A H 0.7523 0.3269 1.0102 0.029 Uiso 1 1 calc R . . H5B H 0.6453 0.3909 1.0086 0.029 Uiso 1 1 calc R . . C6 C 0.3108(12) 0.2931(9) 0.9977(9) 0.025(2) Uani 1 1 d . . . H6A H 0.2160 0.2749 0.9954 0.030 Uiso 1 1 calc R . . H6B H 0.3299 0.3601 1.0001 0.030 Uiso 1 1 calc R . . C7 C 0.7583(11) 0.3170(8) 1.1699(9) 0.021(2) Uani 1 1 d . . . C8 C 0.5550(11) 0.3670(8) 1.1420(8) 0.021(2) Uani 1 1 d . . . H8 H 0.5598 0.4358 1.1485 0.025 Uiso 1 1 calc R . . C9 C 0.6042(12) 0.3686(9) 1.2494(9) 0.022(2) Uani 1 1 d . . . H9 H 0.6226 0.4367 1.3059 0.027 Uiso 1 1 calc R . . C10 C 0.3741(12) 0.2582(9) 1.1469(9) 0.025(2) Uani 1 1 d . . . C11 C 0.8241(11) 0.3408(8) 1.3487(9) 0.021(2) Uani 1 1 d . . . H11A H 0.8254 0.3981 1.4088 0.025 Uiso 1 1 calc R . . H11B H 0.9195 0.3521 1.3508 0.025 Uiso 1 1 calc R . . C12 C 0.4760(13) 0.2773(9) 1.3225(9) 0.023(2) Uani 1 1 d . . . H12A H 0.3765 0.2540 1.3085 0.028 Uiso 1 1 calc R . . H12B H 0.5187 0.3421 1.3858 0.028 Uiso 1 1 calc R . . C13 C 0.8437(12) 0.1731(9) 1.3271(9) 0.027(3) Uani 1 1 d . . . C14 C 0.6881(11) 0.2291(8) 1.4017(9) 0.022(2) Uani 1 1 d . . . H14 H 0.7152 0.2842 1.4721 0.026 Uiso 1 1 calc R . . C15 C 0.7012(11) 0.1257(8) 1.4010(9) 0.020(2) Uani 1 1 d . . . H15 H 0.7430 0.1336 1.4715 0.024 Uiso 1 1 calc R . . C16 C 0.4674(11) 0.1074(9) 1.3079(9) 0.022(2) Uani 1 1 d . . . C17 C 0.1550(12) -0.0107(8) 0.6656(9) 0.020(2) Uani 1 1 d . . . H17A H 0.1399 -0.0008 0.6044 0.025 Uiso 1 1 calc R . . H17B H 0.0642 -0.0263 0.6702 0.025 Uiso 1 1 calc R . . C18 C 0.4893(12) 0.0384(8) 0.6667(9) 0.021(2) Uani 1 1 d . . . H18A H 0.4321 0.0413 0.6049 0.026 Uiso 1 1 calc R . . H18B H 0.5864 0.0525 0.6725 0.026 Uiso 1 1 calc R . . N1 N 0.4827(9) 0.1171(8) 0.7546(7) 0.023(2) Uani 1 1 d . . . N2 N 0.5551(9) 0.2422(7) 0.9137(7) 0.0201(19) Uani 1 1 d . . . N3 N 0.2487(9) 0.0819(7) 0.7559(7) 0.0194(19) Uani 1 1 d . . . N4 N 0.3148(10) 0.2200(7) 0.9045(7) 0.023(2) Uani 1 1 d . . . N5 N 0.6502(10) 0.3259(7) 1.0994(7) 0.023(2) Uani 1 1 d . . . N6 N 0.7315(10) 0.3394(8) 1.2561(7) 0.023(2) Uani 1 1 d . . . N7 N 0.4097(9) 0.3002(7) 1.0912(7) 0.022(2) Uani 1 1 d . . . N8 N 0.4885(10) 0.2938(7) 1.2382(7) 0.022(2) Uani 1 1 d . . . N9 N 0.7839(10) 0.2480(7) 1.3556(8) 0.023(2) Uani 1 1 d . . . N10 N 0.7884(10) 0.0969(7) 1.3453(7) 0.022(2) Uani 1 1 d . . . N11 N 0.5421(10) 0.2034(7) 1.3384(7) 0.0200(19) Uani 1 1 d . . . N12 N 0.5563(10) 0.0613(7) 1.3468(8) 0.024(2) Uani 1 1 d . . . O1 O 0.7125(8) 0.1614(6) 0.8659(6) 0.0253(18) Uani 1 1 d . . . O2 O 0.8621(9) 0.2960(7) 1.1591(7) 0.033(2) Uani 1 1 d . . . O3 O 0.9334(10) 0.1740(7) 1.2908(8) 0.040(2) Uani 1 1 d . . . O4 O 0.1182(8) 0.0916(6) 0.8547(7) 0.0270(18) Uani 1 1 d . . . O5 O 0.2595(8) 0.2021(6) 1.1227(7) 0.0270(18) Uani 1 1 d . . . O6 O 0.3401(8) 0.0698(6) 1.2583(7) 0.0292(19) 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 Zn1 0.0309(8) 0.0297(8) 0.0296(8) 0.0152(6) 0.0085(6) 0.0051(6) Zn2 0.0335(8) 0.0317(8) 0.0309(8) 0.0149(6) 0.0155(7) 0.0109(6) Cl1 0.0369(18) 0.0263(15) 0.0416(19) 0.0117(14) 0.0067(15) 0.0077(13) Cl2 0.048(2) 0.0398(18) 0.0368(18) 0.0252(15) 0.0070(15) 0.0113(15) Cl3 0.049(2) 0.0329(17) 0.0286(16) 0.0144(14) 0.0069(15) 0.0066(14) Cl4 0.130(8) 0.270(16) 0.186(12) 0.122(12) 0.072(8) 0.041(9) Cl5 0.057(2) 0.0433(19) 0.047(2) 0.0224(16) 0.0357(18) 0.0181(17) Cl6 0.058(2) 0.0362(18) 0.044(2) 0.0183(16) 0.0251(18) 0.0225(16) Cl7 0.091(3) 0.072(3) 0.049(2) 0.040(2) 0.020(2) 0.039(3) Cl8 0.144(9) 0.154(10) 0.191(12) 0.056(9) 0.061(8) 0.037(7) O1W 0.028(5) 0.045(5) 0.023(4) 0.015(4) 0.010(4) 0.011(4) O2W 0.030(5) 0.035(5) 0.044(6) 0.021(4) 0.018(4) 0.007(4) O3W 0.031(5) 0.045(6) 0.041(5) 0.027(5) 0.013(4) 0.009(4) O4W 0.039(5) 0.049(6) 0.029(5) 0.015(4) 0.008(4) 0.005(5) O5W 0.062(7) 0.045(6) 0.038(6) 0.017(5) 0.021(5) 0.005(5) Cd1 0.0404(12) 0.0449(12) 0.0485(13) 0.0201(10) 0.0191(10) 0.0132(10) C1 0.024(6) 0.026(6) 0.018(6) 0.014(5) 0.009(5) 0.003(5) C2 0.020(5) 0.015(5) 0.022(6) 0.013(4) 0.008(4) 0.010(4) C3 0.017(5) 0.023(6) 0.027(6) 0.010(5) 0.014(5) 0.004(4) C4 0.016(5) 0.020(5) 0.021(6) 0.007(5) 0.008(5) 0.003(4) C5 0.020(6) 0.024(6) 0.024(6) 0.011(5) 0.005(5) 0.001(5) C6 0.023(6) 0.028(6) 0.021(6) 0.008(5) 0.009(5) 0.006(5) C7 0.019(6) 0.020(5) 0.023(6) 0.012(5) 0.006(5) 0.005(4) C8 0.020(6) 0.019(5) 0.019(6) 0.006(4) 0.007(5) 0.000(4) C9 0.023(6) 0.024(6) 0.020(6) 0.014(5) 0.003(5) 0.008(5) C10 0.027(6) 0.021(6) 0.028(6) 0.011(5) 0.010(5) 0.011(5) C11 0.017(5) 0.016(5) 0.022(6) 0.007(4) 0.000(5) 0.002(4) C12 0.031(6) 0.020(6) 0.025(6) 0.011(5) 0.014(5) 0.016(5) C13 0.020(6) 0.025(6) 0.026(6) 0.007(5) 0.008(5) -0.001(5) C14 0.020(6) 0.017(5) 0.020(6) 0.005(4) 0.002(5) 0.007(4) C15 0.020(5) 0.020(5) 0.018(5) 0.008(4) 0.008(5) 0.006(4) C16 0.016(6) 0.029(6) 0.022(6) 0.012(5) 0.010(5) 0.003(5) C17 0.023(6) 0.020(5) 0.019(5) 0.009(4) 0.007(5) 0.007(4) C18 0.024(6) 0.016(5) 0.030(6) 0.014(5) 0.013(5) 0.008(4) N1 0.014(4) 0.030(5) 0.018(5) 0.006(4) 0.008(4) 0.003(4) N2 0.018(5) 0.018(5) 0.021(5) 0.009(4) 0.004(4) 0.004(4) N3 0.012(4) 0.018(4) 0.025(5) 0.005(4) 0.009(4) 0.005(4) N4 0.021(5) 0.025(5) 0.023(5) 0.010(4) 0.011(4) 0.001(4) N5 0.022(5) 0.026(5) 0.019(5) 0.012(4) 0.006(4) 0.005(4) N6 0.015(5) 0.030(5) 0.016(5) 0.007(4) 0.001(4) 0.005(4) N7 0.017(5) 0.027(5) 0.021(5) 0.011(4) 0.007(4) 0.007(4) N8 0.019(5) 0.025(5) 0.025(5) 0.015(4) 0.007(4) 0.006(4) N9 0.022(5) 0.020(5) 0.027(5) 0.010(4) 0.014(4) 0.003(4) N10 0.024(5) 0.025(5) 0.023(5) 0.012(4) 0.015(4) 0.007(4) N11 0.023(5) 0.016(4) 0.023(5) 0.011(4) 0.009(4) 0.007(4) N12 0.018(5) 0.021(5) 0.028(5) 0.009(4) 0.006(4) 0.004(4) O1 0.024(4) 0.021(4) 0.030(5) 0.013(4) 0.009(4) 0.008(3) O2 0.024(4) 0.045(5) 0.035(5) 0.021(4) 0.014(4) 0.015(4) O3 0.042(5) 0.028(5) 0.056(6) 0.013(4) 0.037(5) 0.008(4) O4 0.017(4) 0.025(4) 0.033(5) 0.011(4) 0.009(4) 0.002(3) O5 0.016(4) 0.030(4) 0.034(5) 0.016(4) 0.008(4) 0.005(3) O6 0.022(4) 0.028(4) 0.038(5) 0.018(4) 0.009(4) 0.006(4) _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 Zn1 Cl4 2.017(12) . ? Zn1 Cl2 2.231(4) . ? Zn1 Cl3 2.239(4) . ? Zn1 Cl1 2.244(4) . ? Zn2 Cl8 2.013(12) . ? Zn2 Cl7 2.230(5) . ? Zn2 Cl6 2.248(4) . ? Zn2 Cl5 2.249(4) . ? O1W Cd1 2.443(9) . ? O2W Cd1 2.455(10) . ? O3W Cd1 2.583(10) . ? O4W Cd1 2.436(10) . ? O5W Cd1 2.536(11) . ? Cd1 O1 2.365(8) . ? Cd1 O6 2.446(9) 2_657 ? Cd1 O4 2.462(8) 1_655 ? C1 O1 1.238(14) . ? C1 N1 1.360(15) . ? C1 N2 1.369(15) . ? C2 N1 1.446(14) . ? C2 N3 1.454(14) . ? C2 C3 1.549(15) . ? C2 H2 0.9900 . ? C3 N4 1.458(14) . ? C3 N2 1.460(14) . ? C3 H3 0.9900 . ? C4 O4 1.236(14) . ? C4 N4 1.349(14) . ? C4 N3 1.370(14) . ? C5 N5 1.438(15) . ? C5 N2 1.452(14) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.442(15) . ? C6 N7 1.450(15) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.219(14) . ? C7 N6 1.364(15) . ? C7 N5 1.378(15) . ? C8 N5 1.440(15) . ? C8 N7 1.470(14) . ? C8 C9 1.563(16) . ? C8 H8 0.9900 . ? C9 N8 1.447(15) . ? C9 N6 1.455(15) . ? C9 H9 0.9900 . ? C10 O5 1.218(15) . ? C10 N7 1.351(16) . ? C10 N8 1.379(15) . ? C11 N6 1.451(15) . ? C11 N9 1.450(14) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.451(15) . ? C12 N11 1.451(14) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.234(15) . ? C13 N9 1.356(16) . ? C13 N10 1.371(15) . ? C14 N11 1.441(14) . ? C14 N9 1.451(15) . ? C14 C15 1.573(15) . ? C14 H14 0.9900 . ? C15 N10 1.438(14) . ? C15 N12 1.454(14) . ? C15 H15 0.9900 . ? C16 O6 1.229(14) . ? C16 N11 1.353(15) . ? C16 N12 1.372(15) . ? C17 N3 1.444(14) . ? C17 N10 1.474(14) 2_657 ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.414(14) 2_657 ? C18 N1 1.434(14) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? N10 C17 1.474(14) 2_657 ? N12 C18 1.414(14) 2_657 ? O4 Cd1 2.462(8) 1_455 ? O6 Cd1 2.446(8) 2_657 ? 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 Cl4 Zn1 Cl2 103.5(4) . . ? Cl4 Zn1 Cl3 102.8(4) . . ? Cl2 Zn1 Cl3 111.88(15) . . ? Cl4 Zn1 Cl1 105.4(5) . . ? Cl2 Zn1 Cl1 119.13(15) . . ? Cl3 Zn1 Cl1 112.07(14) . . ? Cl8 Zn2 Cl7 101.6(4) . . ? Cl8 Zn2 Cl6 111.7(4) . . ? Cl7 Zn2 Cl6 115.30(18) . . ? Cl8 Zn2 Cl5 107.3(4) . . ? Cl7 Zn2 Cl5 111.24(19) . . ? Cl6 Zn2 Cl5 109.26(15) . . ? O1 Cd1 O4W 98.2(3) . . ? O1 Cd1 O1W 76.3(3) . . ? O4W Cd1 O1W 144.2(3) . . ? O1 Cd1 O6 80.1(3) . 2_657 ? O4W Cd1 O6 72.4(3) . 2_657 ? O1W Cd1 O6 138.5(3) . 2_657 ? O1 Cd1 O2W 147.2(3) . . ? O4W Cd1 O2W 93.5(4) . . ? O1W Cd1 O2W 110.3(3) . . ? O6 Cd1 O2W 74.4(3) 2_657 . ? O1 Cd1 O4 142.7(3) . 1_655 ? O4W Cd1 O4 81.2(3) . 1_655 ? O1W Cd1 O4 82.7(3) . 1_655 ? O6 Cd1 O4 133.2(3) 2_657 1_655 ? O2W Cd1 O4 69.3(3) . 1_655 ? O1 Cd1 O5W 82.5(3) . . ? O4W Cd1 O5W 145.1(4) . . ? O1W Cd1 O5W 70.1(3) . . ? O6 Cd1 O5W 73.4(3) 2_657 . ? O2W Cd1 O5W 70.7(4) . . ? O4 Cd1 O5W 118.7(4) 1_655 . ? O1 Cd1 O3W 69.5(3) . . ? O4W Cd1 O3W 70.3(3) . . ? O1W Cd1 O3W 74.7(3) . . ? O6 Cd1 O3W 126.9(3) 2_657 . ? O2W Cd1 O3W 143.1(3) . . ? O4 Cd1 O3W 75.5(3) 1_655 . ? O5W Cd1 O3W 139.3(4) . . ? O1 C1 N1 125.4(11) . . ? O1 C1 N2 125.5(10) . . ? N1 C1 N2 109.1(10) . . ? N1 C2 N3 115.2(9) . . ? N1 C2 C3 103.9(8) . . ? N3 C2 C3 103.2(8) . . ? N1 C2 H2 111.3 . . ? N3 C2 H2 111.3 . . ? C3 C2 H2 111.3 . . ? N4 C3 N2 114.4(10) . . ? N4 C3 C2 102.9(8) . . ? N2 C3 C2 102.7(8) . . ? N4 C3 H3 112.0 . . ? N2 C3 H3 112.0 . . ? C2 C3 H3 112.0 . . ? O4 C4 N4 125.5(10) . . ? O4 C4 N3 125.5(10) . . ? N4 C4 N3 109.0(9) . . ? N5 C5 N2 113.2(9) . . ? N5 C5 H5A 108.9 . . ? N2 C5 H5A 108.9 . . ? N5 C5 H5B 108.9 . . ? N2 C5 H5B 108.9 . . ? H5A C5 H5B 107.8 . . ? N4 C6 N7 114.1(10) . . ? N4 C6 H6A 108.7 . . ? N7 C6 H6A 108.7 . . ? N4 C6 H6B 108.7 . . ? N7 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? O2 C7 N6 125.7(11) . . ? O2 C7 N5 126.5(11) . . ? N6 C7 N5 107.8(10) . . ? N5 C8 N7 115.2(9) . . ? N5 C8 C9 103.7(9) . . ? N7 C8 C9 102.0(9) . . ? N5 C8 H8 111.7 . . ? N7 C8 H8 111.7 . . ? C9 C8 H8 111.7 . . ? N8 C9 N6 114.9(9) . . ? N8 C9 C8 103.2(9) . . ? N6 C9 C8 102.0(9) . . ? N8 C9 H9 112.0 . . ? N6 C9 H9 112.0 . . ? C8 C9 H9 112.0 . . ? O5 C10 N7 126.1(11) . . ? O5 C10 N8 126.0(11) . . ? N7 C10 N8 107.9(10) . . ? N6 C11 N9 113.5(9) . . ? N6 C11 H11A 108.9 . . ? N9 C11 H11A 108.9 . . ? N6 C11 H11B 108.9 . . ? N9 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? N8 C12 N11 113.2(9) . . ? N8 C12 H12A 108.9 . . ? N11 C12 H12A 108.9 . . ? N8 C12 H12B 108.9 . . ? N11 C12 H12B 108.9 . . ? H12A C12 H12B 107.8 . . ? O3 C13 N9 125.2(11) . . ? O3 C13 N10 125.9(12) . . ? N9 C13 N10 108.9(10) . . ? N11 C14 N9 114.7(10) . . ? N11 C14 C15 102.8(9) . . ? N9 C14 C15 101.9(9) . . ? N11 C14 H14 112.2 . . ? N9 C14 H14 112.2 . . ? C15 C14 H14 112.2 . . ? N10 C15 N12 114.3(9) . . ? N10 C15 C14 103.7(9) . . ? N12 C15 C14 102.4(9) . . ? N10 C15 H15 111.9 . . ? N12 C15 H15 111.9 . . ? C14 C15 H15 111.9 . . ? O6 C16 N11 125.6(11) . . ? O6 C16 N12 125.9(11) . . ? N11 C16 N12 108.4(9) . . ? N3 C17 N10 111.6(9) . 2_657 ? N3 C17 H17A 109.3 . . ? N10 C17 H17A 109.3 2_657 . ? N3 C17 H17B 109.3 . . ? N10 C17 H17B 109.3 2_657 . ? H17A C17 H17B 108.0 . . ? N12 C18 N1 115.1(10) 2_657 . ? N12 C18 H18A 108.5 2_657 . ? N1 C18 H18A 108.5 . . ? N12 C18 H18B 108.5 2_657 . ? N1 C18 H18B 108.5 . . ? H18A C18 H18B 107.5 . . ? C1 N1 C18 123.3(10) . . ? C1 N1 C2 112.0(9) . . ? C18 N1 C2 124.7(9) . . ? C1 N2 C5 121.4(9) . . ? C1 N2 C3 111.6(9) . . ? C5 N2 C3 122.8(9) . . ? C4 N3 C17 123.1(9) . . ? C4 N3 C2 111.7(9) . . ? C17 N3 C2 122.9(9) . . ? C4 N4 C6 124.7(9) . . ? C4 N4 C3 112.5(9) . . ? C6 N4 C3 122.4(9) . . ? C7 N5 C5 122.2(10) . . ? C7 N5 C8 112.3(9) . . ? C5 N5 C8 122.3(10) . . ? C7 N6 C11 124.0(10) . . ? C7 N6 C9 113.4(9) . . ? C11 N6 C9 122.5(9) . . ? C10 N7 C6 123.9(10) . . ? C10 N7 C8 113.5(9) . . ? C6 N7 C8 122.0(9) . . ? C10 N8 C9 112.8(9) . . ? C10 N8 C12 121.1(10) . . ? C9 N8 C12 124.1(9) . . ? C13 N9 C11 122.0(9) . . ? C13 N9 C14 113.0(9) . . ? C11 N9 C14 124.7(9) . . ? C13 N10 C15 111.7(10) . . ? C13 N10 C17 121.8(9) . 2_657 ? C15 N10 C17 124.4(9) . 2_657 ? C16 N11 C14 113.5(9) . . ? C16 N11 C12 122.3(10) . . ? C14 N11 C12 123.5(9) . . ? C16 N12 C18 123.1(9) . 2_657 ? C16 N12 C15 112.4(9) . . ? C18 N12 C15 124.5(10) 2_657 . ? C1 O1 Cd1 155.5(8) . . ? C4 O4 Cd1 152.4(8) . 1_455 ? C16 O6 Cd1 154.1(8) . 2_657 ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.171 _refine_diff_density_min -1.827 _refine_diff_density_rms 0.230 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.001 0.500 1.000 37 16 ' ' 2 0.242 0.280 0.429 79 31 ' ' 3 0.500 1.000 1.000 90 26 ' ' 4 0.756 0.720 0.570 79 31 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 902604' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p200 #TrackingRef 'submit-200.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H92 Cd Cl5 N24 O40 Y' _chemical_formula_weight 1879.90 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 '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 15.1118(8) _cell_length_b 15.5851(8) _cell_length_c 17.0616(12) _cell_angle_alpha 64.897(2) _cell_angle_beta 80.888(2) _cell_angle_gamma 81.7570(10) _cell_volume 3579.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 1.403 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7118 _exptl_absorpt_correction_T_max 0.7863 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42892 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.0763 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 26.00 _reflns_number_total 13809 _reflns_number_gt 9103 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0821P)^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 13809 _refine_ls_number_parameters 748 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1499 _refine_ls_wR_factor_gt 0.1393 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _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 Cl5 Cl 0.98764(8) -0.19800(10) 0.54416(9) 0.0695(4) Uani 1 1 d . . . O1W O 1.36828(19) 0.0647(2) 0.66403(18) 0.0500(7) Uani 1 1 d . . . O2W O 1.25998(19) 0.23603(19) 0.61283(18) 0.0466(7) Uani 1 1 d . . . O3W O 1.06635(18) 0.1327(2) 0.64330(17) 0.0456(7) Uani 1 1 d . . . O4W O 1.10498(18) -0.0174(2) 0.80194(18) 0.0478(7) Uani 1 1 d . . . Y2 Y 1.20876(2) 0.08445(3) 0.69372(2) 0.03113(11) Uani 1 1 d . . . Cl1 Cl 1.51227(10) -0.75854(12) 0.84861(13) 0.0952(5) Uani 1 1 d . . . Cl2 Cl 1.62507(10) -0.53066(11) 0.80542(16) 0.1126(7) Uani 1 1 d . . . Cl3 Cl 1.35230(10) -0.53187(14) 0.83539(15) 0.1344(9) Uani 1 1 d . . . Cl4 Cl 1.4898(3) -0.6756(3) 1.03896(15) 0.274(3) Uani 1 1 d . . . Cd1 Cd 1.49461(3) -0.61890(3) 0.88433(3) 0.07840(17) Uani 1 1 d . . . C1 C 1.1283(2) 0.2401(3) 0.7922(2) 0.0326(8) Uani 1 1 d . . . C2 C 1.0662(3) 0.3480(3) 0.8509(2) 0.0354(9) Uani 1 1 d . . . H2 H 1.0566 0.4175 0.8170 0.042 Uiso 1 1 calc R . . C3 C 1.1640(3) 0.3157(3) 0.8730(2) 0.0383(9) Uani 1 1 d . . . H3 H 1.2004 0.3707 0.8524 0.046 Uiso 1 1 calc R . . C4 C 1.0666(3) 0.2723(3) 1.0024(3) 0.0422(10) Uani 1 1 d . . . C5 C 1.2853(2) 0.2112(3) 0.8248(2) 0.0356(9) Uani 1 1 d . . . H5A H 1.2997 0.2048 0.7694 0.043 Uiso 1 1 calc R . . H5B H 1.3273 0.2530 0.8259 0.043 Uiso 1 1 calc R . . C6 C 1.2293(3) 0.2303(3) 1.0182(3) 0.0452(10) Uani 1 1 d . . . H6A H 1.2797 0.2696 0.9887 0.054 Uiso 1 1 calc R . . H6B H 1.2113 0.2345 1.0743 0.054 Uiso 1 1 calc R . . C7 C 1.2886(2) 0.0375(3) 0.8894(2) 0.0337(9) Uani 1 1 d . . . C8 C 1.3271(3) 0.1032(3) 0.9776(2) 0.0367(9) Uani 1 1 d . . . H8 H 1.3852 0.1295 0.9705 0.044 Uiso 1 1 calc R . . C9 C 1.3351(2) -0.0060(3) 1.0251(2) 0.0366(9) Uani 1 1 d . . . H9 H 1.3977 -0.0312 1.0371 0.044 Uiso 1 1 calc R . . C10 C 1.2344(3) 0.0576(3) 1.1095(3) 0.0377(9) Uani 1 1 d . . . C11 C 1.3204(3) -0.1346(3) 0.9744(2) 0.0355(9) Uani 1 1 d . . . H11A H 1.3272 -0.1350 0.9165 0.043 Uiso 1 1 calc R . . H11B H 1.3767 -0.1632 1.0002 0.043 Uiso 1 1 calc R . . C12 C 1.2678(3) -0.1154(3) 1.1767(2) 0.0419(10) Uani 1 1 d . . . H12A H 1.3277 -0.1493 1.1857 0.050 Uiso 1 1 calc R . . H12B H 1.2437 -0.1061 1.2296 0.050 Uiso 1 1 calc R . . C13 C 1.1891(3) -0.2201(3) 0.9945(3) 0.0384(9) Uani 1 1 d . . . C14 C 1.2425(3) -0.2376(3) 1.1210(2) 0.0368(9) Uani 1 1 d . . . H14 H 1.2992 -0.2752 1.1418 0.044 Uiso 1 1 calc R . . C15 C 1.1659(2) -0.3003(3) 1.1459(2) 0.0374(9) Uani 1 1 d . . . H15 H 1.1857 -0.3681 1.1784 0.045 Uiso 1 1 calc R . . C16 C 1.1288(3) -0.1951(3) 1.2113(2) 0.0374(9) Uani 1 1 d . . . C17 C 1.0803(3) -0.3424(3) 1.0510(3) 0.0442(10) Uani 1 1 d . . . H17A H 1.0951 -0.3408 0.9924 0.053 Uiso 1 1 calc R . . H17B H 1.0931 -0.4081 1.0927 0.053 Uiso 1 1 calc R . . C18 C 1.0204(3) -0.3142(3) 1.2481(2) 0.0372(9) Uani 1 1 d . . . H18A H 1.0372 -0.3828 1.2720 0.045 Uiso 1 1 calc R . . H18B H 1.0009 -0.2965 1.2972 0.045 Uiso 1 1 calc R . . C19 C 1.2142(2) 0.0930(3) 0.4851(2) 0.0336(9) Uani 1 1 d . . . C20 C 1.2216(3) 0.1117(3) 0.3427(2) 0.0382(9) Uani 1 1 d . . . H20 H 1.1800 0.1561 0.3009 0.046 Uiso 1 1 calc R . . C21 C 1.1798(3) 0.0175(3) 0.4033(2) 0.0380(9) Uani 1 1 d . . . H21 H 1.1181 0.0171 0.3908 0.046 Uiso 1 1 calc R . . C22 C 1.3115(3) -0.0144(3) 0.3230(3) 0.0401(9) Uani 1 1 d . . . C23 C 1.1389(2) -0.0533(3) 0.5685(2) 0.0363(9) Uani 1 1 d . . . H23A H 1.1119 -0.0222 0.6069 0.044 Uiso 1 1 calc R . . H23B H 1.0906 -0.0783 0.5544 0.044 Uiso 1 1 calc R . . C24 C 1.2334(3) -0.1547(3) 0.4295(3) 0.0442(10) Uani 1 1 d . . . H24A H 1.2631 -0.1846 0.3909 0.053 Uiso 1 1 calc R . . H24B H 1.1696 -0.1662 0.4405 0.053 Uiso 1 1 calc R . . C25 C 1.2507(3) -0.1324(3) 0.6738(2) 0.0346(9) Uani 1 1 d . . . C26 C 1.2218(3) -0.2165(3) 0.5964(2) 0.0392(9) Uani 1 1 d . . . H26 H 1.1679 -0.2509 0.6067 0.047 Uiso 1 1 calc R . . C27 C 1.2919(3) -0.2743(3) 0.6595(2) 0.0369(9) Uani 1 1 d . . . H27 H 1.2697 -0.3351 0.7034 0.044 Uiso 1 1 calc R . . C28 C 1.3554(3) -0.2488(3) 0.5198(3) 0.0438(10) Uani 1 1 d . . . C29 C 1.3539(2) -0.2428(3) 0.7761(2) 0.0398(9) Uani 1 1 d . . . H29A H 1.3439 -0.3093 0.8140 0.048 Uiso 1 1 calc R . . H29B H 1.3295 -0.2044 0.8089 0.048 Uiso 1 1 calc R . . C30 C 1.4496(3) -0.3517(3) 0.6337(3) 0.0407(9) Uani 1 1 d . . . H30A H 1.4320 -0.4084 0.6853 0.049 Uiso 1 1 calc R . . H30B H 1.4780 -0.3725 0.5882 0.049 Uiso 1 1 calc R . . C31 C 1.4921(3) -0.1693(3) 0.7630(2) 0.0372(9) Uani 1 1 d . . . C32 C 1.5113(2) -0.3084(3) 0.7404(2) 0.0357(9) Uani 1 1 d . . . H32 H 1.5014 -0.3716 0.7882 0.043 Uiso 1 1 calc R . . C33 C 1.6044(2) -0.2760(3) 0.7380(2) 0.0347(9) Uani 1 1 d . . . H33 H 1.6389 -0.3247 0.7843 0.042 Uiso 1 1 calc R . . C34 C 1.5956(3) -0.2839(3) 0.6063(3) 0.0397(9) Uani 1 1 d . . . C35 C 1.6470(3) -0.1453(3) 0.7746(2) 0.0409(9) Uani 1 1 d . . . H35A H 1.6144 -0.1106 0.8082 0.049 Uiso 1 1 calc R . . H35B H 1.6879 -0.1952 0.8122 0.049 Uiso 1 1 calc R . . C36 C 1.7409(3) -0.2473(3) 0.6253(3) 0.0394(9) Uani 1 1 d . . . H36A H 1.7609 -0.2659 0.5768 0.047 Uiso 1 1 calc R . . H36B H 1.7761 -0.2882 0.6734 0.047 Uiso 1 1 calc R . . N1 N 1.0536(2) 0.2938(2) 0.80205(19) 0.0338(7) Uani 1 1 d . . . N2 N 1.1959(2) 0.2554(2) 0.8280(2) 0.0359(7) Uani 1 1 d . . . N3 N 1.0144(2) 0.3157(2) 0.9367(2) 0.0395(8) Uani 1 1 d . . . N4 N 1.1547(2) 0.2679(2) 0.9660(2) 0.0446(8) Uani 1 1 d . . . N5 N 1.2993(2) 0.1204(2) 0.8936(2) 0.0398(8) Uani 1 1 d . . . N6 N 1.3058(2) -0.0363(2) 0.9649(2) 0.0352(7) Uani 1 1 d . . . N7 N 1.2591(2) 0.1334(2) 1.0337(2) 0.0426(8) Uani 1 1 d . . . N8 N 1.2763(2) -0.0235(2) 1.1046(2) 0.0385(8) Uani 1 1 d . . . N9 N 1.2492(2) -0.1920(2) 1.02730(19) 0.0370(7) Uani 1 1 d . . . N10 N 1.1379(2) -0.2823(2) 1.0615(2) 0.0384(8) Uani 1 1 d . . . N11 N 1.2109(2) -0.1730(2) 1.1641(2) 0.0361(7) Uani 1 1 d . . . N12 N 1.0996(2) -0.2647(2) 1.1986(2) 0.0352(7) Uani 1 1 d . . . N13 N 1.2402(2) 0.1493(2) 0.40184(19) 0.0356(7) Uani 1 1 d . . . N14 N 1.1807(2) 0.0165(2) 0.48900(19) 0.0364(7) Uani 1 1 d . . . N15 N 1.3004(2) 0.0806(2) 0.2994(2) 0.0394(8) Uani 1 1 d . . . N16 N 1.2412(2) -0.0539(2) 0.3862(2) 0.0431(8) Uani 1 1 d . . . N17 N 1.2018(2) -0.1316(2) 0.6142(2) 0.0368(7) Uani 1 1 d . . . N18 N 1.3058(2) -0.2124(2) 0.7003(2) 0.0348(7) Uani 1 1 d . . . N19 N 1.2728(2) -0.1994(3) 0.5118(2) 0.0450(8) Uani 1 1 d . . . N20 N 1.3695(2) -0.2904(2) 0.6040(2) 0.0407(8) Uani 1 1 d . . . N21 N 1.4509(2) -0.2338(2) 0.7533(2) 0.0351(7) Uani 1 1 d . . . N22 N 1.5820(2) -0.1904(2) 0.7519(2) 0.0380(8) Uani 1 1 d . . . N23 N 1.5140(2) -0.3092(2) 0.6549(2) 0.0373(8) Uani 1 1 d . . . N24 N 1.6474(2) -0.2636(2) 0.6528(2) 0.0351(7) Uani 1 1 d . . . O1 O 1.13634(17) 0.18777(18) 0.75354(16) 0.0372(6) Uani 1 1 d . . . O2 O 1.26803(19) 0.02937(19) 0.82551(17) 0.0427(7) Uani 1 1 d . . . O3 O 1.1832(2) -0.1952(2) 0.91639(18) 0.0479(7) Uani 1 1 d . . . O4 O 1.0414(2) 0.2433(2) 1.0793(2) 0.0598(9) Uani 1 1 d . . . O5 O 1.1869(2) 0.0651(2) 1.17089(18) 0.0500(7) Uani 1 1 d . . . O6 O 1.09020(19) -0.1544(2) 1.25780(19) 0.0492(7) Uani 1 1 d . . . O7 O 1.22241(17) 0.10945(18) 0.54833(16) 0.0376(6) Uani 1 1 d . . . O8 O 1.24546(19) -0.06851(18) 0.70003(17) 0.0423(7) Uani 1 1 d . . . O9 O 1.45479(18) -0.10027(19) 0.77863(17) 0.0407(6) Uani 1 1 d . . . O10 O 1.36987(19) -0.0574(2) 0.2935(2) 0.0505(7) Uani 1 1 d . . . O11 O 1.4056(2) -0.2579(3) 0.4591(2) 0.0644(9) Uani 1 1 d . . . O12 O 1.6163(2) -0.2827(2) 0.53329(19) 0.0541(8) 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 Cl5 0.0495(7) 0.0853(9) 0.0762(9) -0.0306(7) -0.0228(6) -0.0044(6) O1W 0.0366(16) 0.0586(18) 0.0442(17) -0.0139(14) 0.0005(13) 0.0000(13) O2W 0.0513(18) 0.0431(16) 0.0484(17) -0.0232(14) 0.0041(14) -0.0095(13) O3W 0.0344(15) 0.0698(19) 0.0361(15) -0.0271(14) -0.0056(12) 0.0043(13) O4W 0.0405(16) 0.0510(17) 0.0428(16) -0.0144(14) 0.0104(13) -0.0082(13) Y2 0.0302(2) 0.0396(2) 0.02614(19) -0.01719(15) -0.00142(14) -0.00071(15) Cl1 0.0477(8) 0.0916(11) 0.1379(15) -0.0359(10) -0.0150(9) -0.0105(7) Cl2 0.0553(8) 0.0572(8) 0.198(2) -0.0339(11) 0.0106(10) -0.0056(7) Cl3 0.0467(8) 0.1014(13) 0.1568(18) 0.0342(12) 0.0002(10) 0.0030(8) Cl4 0.389(6) 0.250(4) 0.0562(13) 0.0001(17) -0.010(2) 0.141(4) Cd1 0.0589(3) 0.0659(3) 0.0710(3) 0.0054(2) -0.0017(2) 0.00204(19) C1 0.035(2) 0.0327(19) 0.0285(19) -0.0112(16) 0.0024(16) -0.0085(16) C2 0.044(2) 0.0288(19) 0.034(2) -0.0120(16) 0.0009(17) -0.0113(16) C3 0.046(2) 0.033(2) 0.035(2) -0.0119(17) 0.0003(18) -0.0123(17) C4 0.048(3) 0.047(2) 0.039(2) -0.026(2) 0.003(2) -0.012(2) C5 0.0265(19) 0.047(2) 0.037(2) -0.0173(18) -0.0026(16) -0.0131(17) C6 0.046(2) 0.053(2) 0.047(2) -0.026(2) -0.012(2) -0.010(2) C7 0.0261(19) 0.043(2) 0.034(2) -0.0178(18) -0.0037(16) -0.0008(16) C8 0.028(2) 0.058(2) 0.032(2) -0.0228(19) -0.0062(16) -0.0090(17) C9 0.0253(19) 0.055(2) 0.032(2) -0.0197(18) -0.0071(16) -0.0022(17) C10 0.032(2) 0.057(3) 0.034(2) -0.026(2) -0.0063(18) -0.0079(18) C11 0.032(2) 0.043(2) 0.032(2) -0.0182(17) -0.0014(16) 0.0022(17) C12 0.038(2) 0.064(3) 0.026(2) -0.0193(19) -0.0086(17) -0.002(2) C13 0.036(2) 0.051(2) 0.030(2) -0.0213(19) -0.0031(17) 0.0062(18) C14 0.036(2) 0.043(2) 0.031(2) -0.0164(17) -0.0059(17) 0.0054(17) C15 0.033(2) 0.039(2) 0.037(2) -0.0155(17) -0.0048(17) 0.0074(17) C16 0.030(2) 0.052(2) 0.031(2) -0.0178(18) -0.0046(17) -0.0004(17) C17 0.051(3) 0.047(2) 0.043(2) -0.030(2) 0.004(2) -0.003(2) C18 0.037(2) 0.039(2) 0.035(2) -0.0163(17) 0.0009(17) -0.0036(17) C19 0.0273(19) 0.043(2) 0.030(2) -0.0170(17) -0.0062(16) 0.0058(16) C20 0.031(2) 0.057(2) 0.031(2) -0.0213(19) -0.0088(16) 0.0007(18) C21 0.036(2) 0.052(2) 0.031(2) -0.0207(18) -0.0046(17) -0.0093(18) C22 0.037(2) 0.059(3) 0.036(2) -0.029(2) -0.0043(18) -0.011(2) C23 0.0277(19) 0.045(2) 0.035(2) -0.0164(17) 0.0035(16) -0.0057(16) C24 0.051(3) 0.050(2) 0.042(2) -0.027(2) -0.008(2) -0.008(2) C25 0.037(2) 0.037(2) 0.030(2) -0.0155(17) 0.0049(17) -0.0082(17) C26 0.040(2) 0.042(2) 0.036(2) -0.0179(18) 0.0022(18) -0.0070(18) C27 0.036(2) 0.041(2) 0.035(2) -0.0183(17) 0.0021(17) -0.0050(17) C28 0.038(2) 0.049(2) 0.049(3) -0.026(2) 0.003(2) -0.0091(19) C29 0.033(2) 0.053(2) 0.032(2) -0.0182(18) 0.0030(17) -0.0055(18) C30 0.041(2) 0.039(2) 0.046(2) -0.0220(19) -0.0017(19) -0.0031(18) C31 0.037(2) 0.049(2) 0.0227(19) -0.0115(17) -0.0076(16) -0.0024(19) C32 0.034(2) 0.042(2) 0.027(2) -0.0108(16) -0.0012(16) -0.0041(17) C33 0.032(2) 0.037(2) 0.028(2) -0.0074(16) -0.0040(16) 0.0005(16) C34 0.046(2) 0.034(2) 0.037(2) -0.0143(17) -0.0027(19) 0.0010(17) C35 0.037(2) 0.061(3) 0.030(2) -0.0224(19) -0.0021(17) -0.0093(19) C36 0.034(2) 0.046(2) 0.037(2) -0.0188(18) -0.0063(17) 0.0072(17) N1 0.0345(17) 0.0399(17) 0.0325(17) -0.0201(14) -0.0045(14) -0.0028(14) N2 0.0321(17) 0.0437(18) 0.0389(18) -0.0237(15) -0.0050(14) -0.0021(14) N3 0.0382(19) 0.0497(19) 0.0371(19) -0.0255(16) -0.0001(15) -0.0037(15) N4 0.050(2) 0.050(2) 0.0360(19) -0.0203(16) -0.0091(16) 0.0018(16) N5 0.0400(19) 0.049(2) 0.0322(18) -0.0160(15) -0.0076(15) -0.0065(15) N6 0.0377(18) 0.0387(17) 0.0318(17) -0.0159(14) -0.0091(14) -0.0007(14) N7 0.043(2) 0.049(2) 0.0405(19) -0.0226(16) -0.0040(16) -0.0038(16) N8 0.0358(18) 0.050(2) 0.0291(17) -0.0143(15) -0.0041(14) -0.0063(15) N9 0.0406(19) 0.0438(18) 0.0276(17) -0.0150(14) -0.0033(14) -0.0059(15) N10 0.0442(19) 0.0435(18) 0.0300(17) -0.0170(15) -0.0034(15) -0.0064(15) N11 0.0347(18) 0.0478(19) 0.0330(17) -0.0235(15) 0.0012(14) -0.0091(15) N12 0.0313(17) 0.0433(18) 0.0345(17) -0.0216(15) 0.0026(14) -0.0033(14) N13 0.0321(17) 0.0490(19) 0.0239(16) -0.0151(14) -0.0022(13) 0.0021(14) N14 0.0383(18) 0.0477(19) 0.0267(17) -0.0188(15) -0.0031(14) -0.0035(15) N15 0.0324(18) 0.055(2) 0.0358(18) -0.0234(16) -0.0015(14) -0.0072(15) N16 0.0396(19) 0.056(2) 0.042(2) -0.0295(17) 0.0005(16) -0.0072(16) N17 0.0376(18) 0.0389(17) 0.0384(18) -0.0205(15) -0.0056(15) -0.0004(14) N18 0.0374(18) 0.0343(16) 0.0348(17) -0.0156(14) -0.0044(14) -0.0042(14) N19 0.049(2) 0.054(2) 0.0339(18) -0.0220(16) -0.0076(16) 0.0038(17) N20 0.0374(19) 0.051(2) 0.0354(19) -0.0231(16) 0.0002(15) 0.0021(15) N21 0.0308(17) 0.0416(18) 0.0361(18) -0.0187(15) -0.0046(14) -0.0026(14) N22 0.0336(18) 0.0500(19) 0.0338(17) -0.0212(15) -0.0034(14) -0.0019(15) N23 0.0321(17) 0.0453(18) 0.0334(17) -0.0172(15) 0.0043(14) -0.0057(14) N24 0.0329(17) 0.0412(18) 0.0315(17) -0.0156(14) -0.0004(14) -0.0053(14) O1 0.0380(15) 0.0428(15) 0.0372(15) -0.0234(13) -0.0056(12) 0.0007(12) O2 0.0474(17) 0.0534(17) 0.0303(15) -0.0215(13) -0.0106(12) 0.0070(13) O3 0.0511(18) 0.0612(18) 0.0350(16) -0.0232(14) -0.0062(13) -0.0037(14) O4 0.065(2) 0.076(2) 0.0380(18) -0.0258(16) -0.0043(15) 0.0036(17) O5 0.0487(18) 0.069(2) 0.0381(16) -0.0293(15) 0.0002(14) -0.0065(15) O6 0.0405(16) 0.0672(19) 0.0539(18) -0.0411(16) 0.0055(14) -0.0066(14) O7 0.0414(15) 0.0472(15) 0.0287(14) -0.0207(12) -0.0016(12) -0.0037(12) O8 0.0537(18) 0.0383(15) 0.0339(15) -0.0165(12) -0.0032(13) 0.0027(12) O9 0.0418(16) 0.0437(15) 0.0449(16) -0.0257(13) -0.0081(13) -0.0010(12) O10 0.0428(17) 0.0676(19) 0.0566(19) -0.0426(17) 0.0046(14) -0.0084(15) O11 0.058(2) 0.088(2) 0.0476(19) -0.0361(18) 0.0011(16) 0.0103(18) O12 0.0504(18) 0.080(2) 0.0391(17) -0.0339(16) 0.0101(14) -0.0134(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1W Y2 2.386(3) . ? O2W Y2 2.346(3) . ? O3W Y2 2.347(3) . ? O4W Y2 2.387(3) . ? Y2 O1 2.317(2) . ? Y2 O2 2.318(3) . ? Y2 O7 2.321(2) . ? Y2 O8 2.329(3) . ? Cl1 Cd1 2.4670(19) . ? Cl2 Cd1 2.4406(16) . ? Cl3 Cd1 2.4358(16) . ? Cl4 Cd1 2.393(3) . ? C1 O1 1.232(4) . ? C1 N1 1.338(5) . ? C1 N2 1.366(5) . ? C2 N3 1.460(5) . ? C2 N1 1.462(5) . ? C2 C3 1.542(6) . ? C2 H2 0.9900 . ? C3 N4 1.431(5) . ? C3 N2 1.439(5) . ? C3 H3 0.9900 . ? C4 O4 1.207(5) . ? C4 N3 1.349(5) . ? C4 N4 1.383(5) . ? C5 N5 1.417(5) . ? C5 N2 1.430(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.434(5) . ? C6 N4 1.447(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.241(4) . ? C7 N6 1.346(5) . ? C7 N5 1.356(5) . ? C8 N7 1.459(5) . ? C8 N5 1.460(5) . ? C8 C9 1.539(6) . ? C8 H8 0.9900 . ? C9 N8 1.441(5) . ? C9 N6 1.445(5) . ? C9 H9 0.9900 . ? C10 O5 1.211(4) . ? C10 N8 1.360(5) . ? C10 N7 1.372(5) . ? C11 N9 1.434(5) . ? C11 N6 1.458(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.425(5) . ? C12 N8 1.445(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.235(5) . ? C13 N9 1.344(5) . ? C13 N10 1.357(5) . ? C14 N9 1.442(5) . ? C14 N11 1.470(5) . ? C14 C15 1.513(6) . ? C14 H14 0.9900 . ? C15 N12 1.449(4) . ? C15 N10 1.465(5) . ? C15 H15 0.9900 . ? C16 O6 1.244(5) . ? C16 N12 1.336(5) . ? C16 N11 1.370(5) . ? C17 N3 1.440(5) 2_757 ? C17 N10 1.447(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N1 1.433(5) 2_757 ? C18 N12 1.460(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O7 1.237(4) . ? C19 N14 1.333(5) . ? C19 N13 1.344(5) . ? C20 N15 1.434(5) . ? C20 N13 1.442(5) . ? C20 C21 1.548(6) . ? C20 H20 0.9900 . ? C21 N16 1.442(5) . ? C21 N14 1.458(5) . ? C21 H21 0.9900 . ? C22 O10 1.206(5) . ? C22 N15 1.352(5) . ? C22 N16 1.390(5) . ? C23 N17 1.447(5) . ? C23 N14 1.448(5) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N16 1.439(5) . ? C24 N19 1.459(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O8 1.241(4) . ? C25 N18 1.340(5) . ? C25 N17 1.344(5) . ? C26 N19 1.459(5) . ? C26 N17 1.460(5) . ? C26 C27 1.535(6) . ? C26 H26 0.9900 . ? C27 N20 1.449(5) . ? C27 N18 1.461(5) . ? C27 H27 0.9900 . ? C28 O11 1.230(5) . ? C28 N20 1.341(5) . ? C28 N19 1.364(5) . ? C29 N18 1.450(5) . ? C29 N21 1.467(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N23 1.420(5) . ? C30 N20 1.444(5) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O9 1.253(5) . ? C31 N21 1.334(5) . ? C31 N22 1.354(5) . ? C32 N21 1.442(5) . ? C32 N23 1.458(5) . ? C32 C33 1.550(5) . ? C32 H32 0.9900 . ? C33 N22 1.437(5) . ? C33 N24 1.439(5) . ? C33 H33 0.9900 . ? C34 O12 1.228(5) . ? C34 N24 1.351(5) . ? C34 N23 1.378(5) . ? C35 N15 1.441(5) 2_856 ? C35 N22 1.470(5) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N24 1.440(5) . ? C36 N13 1.453(5) 2_856 ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? N1 C18 1.433(5) 2_757 ? N3 C17 1.440(5) 2_757 ? N13 C36 1.453(5) 2_856 ? N15 C35 1.441(5) 2_856 ? 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 Y2 O2 77.16(9) . . ? O1 Y2 O7 126.60(9) . . ? O2 Y2 O7 150.98(9) . . ? O1 Y2 O8 151.04(9) . . ? O2 Y2 O8 86.70(9) . . ? O7 Y2 O8 77.28(9) . . ? O1 Y2 O2W 70.65(9) . . ? O2 Y2 O2W 104.84(10) . . ? O7 Y2 O2W 73.43(9) . . ? O8 Y2 O2W 137.56(9) . . ? O1 Y2 O3W 72.74(9) . . ? O2 Y2 O3W 137.36(9) . . ? O7 Y2 O3W 71.07(9) . . ? O8 Y2 O3W 105.85(10) . . ? O2W Y2 O3W 92.96(11) . . ? O1 Y2 O1W 123.44(10) . . ? O2 Y2 O1W 72.91(10) . . ? O7 Y2 O1W 79.22(10) . . ? O8 Y2 O1W 72.60(10) . . ? O2W Y2 O1W 72.28(10) . . ? O3W Y2 O1W 149.64(10) . . ? O1 Y2 O4W 80.29(9) . . ? O2 Y2 O4W 73.02(10) . . ? O7 Y2 O4W 122.84(10) . . ? O8 Y2 O4W 72.00(9) . . ? O2W Y2 O4W 150.40(9) . . ? O3W Y2 O4W 72.70(10) . . ? O1W Y2 O4W 131.53(10) . . ? Cl4 Cd1 Cl3 110.53(11) . . ? Cl4 Cd1 Cl2 113.09(16) . . ? Cl3 Cd1 Cl2 113.33(6) . . ? Cl4 Cd1 Cl1 107.82(12) . . ? Cl3 Cd1 Cl1 106.45(8) . . ? Cl2 Cd1 Cl1 105.10(6) . . ? O1 C1 N1 125.5(4) . . ? O1 C1 N2 124.8(3) . . ? N1 C1 N2 109.6(3) . . ? N3 C2 N1 112.7(3) . . ? N3 C2 C3 102.8(3) . . ? N1 C2 C3 102.8(3) . . ? N3 C2 H2 112.6 . . ? N1 C2 H2 112.6 . . ? C3 C2 H2 112.6 . . ? N4 C3 N2 115.0(3) . . ? N4 C3 C2 103.7(3) . . ? N2 C3 C2 103.7(3) . . ? N4 C3 H3 111.3 . . ? N2 C3 H3 111.3 . . ? C2 C3 H3 111.3 . . ? O4 C4 N3 126.4(4) . . ? O4 C4 N4 125.9(4) . . ? N3 C4 N4 107.7(3) . . ? N5 C5 N2 114.5(3) . . ? N5 C5 H5A 108.6 . . ? N2 C5 H5A 108.6 . . ? N5 C5 H5B 108.6 . . ? N2 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? N7 C6 N4 113.3(3) . . ? N7 C6 H6A 108.9 . . ? N4 C6 H6A 108.9 . . ? N7 C6 H6B 108.9 . . ? N4 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N6 124.2(3) . . ? O2 C7 N5 125.8(3) . . ? N6 C7 N5 109.9(3) . . ? N7 C8 N5 114.6(3) . . ? N7 C8 C9 103.7(3) . . ? N5 C8 C9 103.3(3) . . ? N7 C8 H8 111.6 . . ? N5 C8 H8 111.6 . . ? C9 C8 H8 111.6 . . ? N8 C9 N6 115.6(3) . . ? N8 C9 C8 103.3(3) . . ? N6 C9 C8 103.5(3) . . ? N8 C9 H9 111.3 . . ? N6 C9 H9 111.3 . . ? C8 C9 H9 111.3 . . ? O5 C10 N8 127.4(4) . . ? O5 C10 N7 124.0(4) . . ? N8 C10 N7 108.5(3) . . ? N9 C11 N6 113.9(3) . . ? N9 C11 H11A 108.8 . . ? N6 C11 H11A 108.8 . . ? N9 C11 H11B 108.8 . . ? N6 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? N11 C12 N8 113.6(3) . . ? N11 C12 H12A 108.8 . . ? N8 C12 H12A 108.8 . . ? N11 C12 H12B 108.8 . . ? N8 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N9 125.6(4) . . ? O3 C13 N10 125.7(4) . . ? N9 C13 N10 108.7(3) . . ? N9 C14 N11 114.3(3) . . ? N9 C14 C15 104.1(3) . . ? N11 C14 C15 103.3(3) . . ? N9 C14 H14 111.6 . . ? N11 C14 H14 111.6 . . ? C15 C14 H14 111.6 . . ? N12 C15 N10 113.6(3) . . ? N12 C15 C14 104.4(3) . . ? N10 C15 C14 103.1(3) . . ? N12 C15 H15 111.7 . . ? N10 C15 H15 111.7 . . ? C14 C15 H15 111.7 . . ? O6 C16 N12 127.5(4) . . ? O6 C16 N11 123.1(4) . . ? N12 C16 N11 109.5(3) . . ? N3 C17 N10 114.2(3) 2_757 . ? N3 C17 H17A 108.7 2_757 . ? N10 C17 H17A 108.7 . . ? N3 C17 H17B 108.7 2_757 . ? N10 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? N1 C18 N12 113.8(3) 2_757 . ? N1 C18 H18A 108.8 2_757 . ? N12 C18 H18A 108.8 . . ? N1 C18 H18B 108.8 2_757 . ? N12 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? O7 C19 N14 125.6(3) . . ? O7 C19 N13 124.5(4) . . ? N14 C19 N13 109.9(3) . . ? N15 C20 N13 114.2(3) . . ? N15 C20 C21 102.9(3) . . ? N13 C20 C21 103.8(3) . . ? N15 C20 H20 111.8 . . ? N13 C20 H20 111.8 . . ? C21 C20 H20 111.8 . . ? N16 C21 N14 114.6(3) . . ? N16 C21 C20 103.6(3) . . ? N14 C21 C20 101.8(3) . . ? N16 C21 H21 112.0 . . ? N14 C21 H21 112.0 . . ? C20 C21 H21 112.0 . . ? O10 C22 N15 126.9(4) . . ? O10 C22 N16 125.9(4) . . ? N15 C22 N16 107.2(3) . . ? N17 C23 N14 112.8(3) . . ? N17 C23 H23A 109.0 . . ? N14 C23 H23A 109.0 . . ? N17 C23 H23B 109.0 . . ? N14 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? N16 C24 N19 113.2(3) . . ? N16 C24 H24A 108.9 . . ? N19 C24 H24A 108.9 . . ? N16 C24 H24B 108.9 . . ? N19 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? O8 C25 N18 125.4(4) . . ? O8 C25 N17 125.0(4) . . ? N18 C25 N17 109.6(3) . . ? N19 C26 N17 113.5(3) . . ? N19 C26 C27 102.2(3) . . ? N17 C26 C27 101.7(3) . . ? N19 C26 H26 112.8 . . ? N17 C26 H26 112.8 . . ? C27 C26 H26 112.8 . . ? N20 C27 N18 114.0(3) . . ? N20 C27 C26 104.3(3) . . ? N18 C27 C26 104.2(3) . . ? N20 C27 H27 111.3 . . ? N18 C27 H27 111.3 . . ? C26 C27 H27 111.3 . . ? O11 C28 N20 126.2(4) . . ? O11 C28 N19 124.4(4) . . ? N20 C28 N19 109.3(3) . . ? N18 C29 N21 112.7(3) . . ? N18 C29 H29A 109.1 . . ? N21 C29 H29A 109.1 . . ? N18 C29 H29B 109.1 . . ? N21 C29 H29B 109.1 . . ? H29A C29 H29B 107.8 . . ? N23 C30 N20 114.6(3) . . ? N23 C30 H30A 108.6 . . ? N20 C30 H30A 108.6 . . ? N23 C30 H30B 108.6 . . ? N20 C30 H30B 108.6 . . ? H30A C30 H30B 107.6 . . ? O9 C31 N21 126.4(4) . . ? O9 C31 N22 125.4(4) . . ? N21 C31 N22 108.2(3) . . ? N21 C32 N23 114.5(3) . . ? N21 C32 C33 101.8(3) . . ? N23 C32 C33 103.4(3) . . ? N21 C32 H32 112.1 . . ? N23 C32 H32 112.1 . . ? C33 C32 H32 112.1 . . ? N22 C33 N24 115.6(3) . . ? N22 C33 C32 103.4(3) . . ? N24 C33 C32 103.4(3) . . ? N22 C33 H33 111.3 . . ? N24 C33 H33 111.3 . . ? C32 C33 H33 111.3 . . ? O12 C34 N24 126.9(4) . . ? O12 C34 N23 124.1(4) . . ? N24 C34 N23 109.0(3) . . ? N15 C35 N22 114.0(3) 2_856 . ? N15 C35 H35A 108.7 2_856 . ? N22 C35 H35A 108.7 . . ? N15 C35 H35B 108.7 2_856 . ? N22 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? N24 C36 N13 114.0(3) . 2_856 ? N24 C36 H36A 108.8 . . ? N13 C36 H36A 108.8 2_856 . ? N24 C36 H36B 108.8 . . ? N13 C36 H36B 108.8 2_856 . ? H36A C36 H36B 107.7 . . ? C1 N1 C18 122.8(3) . 2_757 ? C1 N1 C2 111.9(3) . . ? C18 N1 C2 123.4(3) 2_757 . ? C1 N2 C5 123.1(3) . . ? C1 N2 C3 111.5(3) . . ? C5 N2 C3 125.3(3) . . ? C4 N3 C17 123.7(3) . 2_757 ? C4 N3 C2 113.0(3) . . ? C17 N3 C2 122.5(3) 2_757 . ? C4 N4 C3 112.7(3) . . ? C4 N4 C6 122.3(3) . . ? C3 N4 C6 124.5(4) . . ? C7 N5 C5 123.8(3) . . ? C7 N5 C8 111.1(3) . . ? C5 N5 C8 125.0(3) . . ? C7 N6 C9 112.0(3) . . ? C7 N6 C11 123.0(3) . . ? C9 N6 C11 122.4(3) . . ? C10 N7 C6 123.2(3) . . ? C10 N7 C8 111.3(3) . . ? C6 N7 C8 125.1(3) . . ? C10 N8 C9 113.0(3) . . ? C10 N8 C12 121.9(3) . . ? C9 N8 C12 124.9(3) . . ? C13 N9 C11 123.3(3) . . ? C13 N9 C14 112.5(3) . . ? C11 N9 C14 123.6(3) . . ? C13 N10 C17 123.6(3) . . ? C13 N10 C15 111.6(3) . . ? C17 N10 C15 122.8(3) . . ? C16 N11 C12 123.0(3) . . ? C16 N11 C14 110.7(3) . . ? C12 N11 C14 123.9(3) . . ? C16 N12 C15 112.0(3) . . ? C16 N12 C18 123.6(3) . . ? C15 N12 C18 122.9(3) . . ? C19 N13 C20 111.8(3) . . ? C19 N13 C36 122.4(3) . 2_856 ? C20 N13 C36 123.5(3) . 2_856 ? C19 N14 C23 123.4(3) . . ? C19 N14 C21 112.7(3) . . ? C23 N14 C21 123.4(3) . . ? C22 N15 C20 114.2(3) . . ? C22 N15 C35 121.9(3) . 2_856 ? C20 N15 C35 122.8(3) . 2_856 ? C22 N16 C24 122.8(3) . . ? C22 N16 C21 112.1(3) . . ? C24 N16 C21 125.1(3) . . ? C25 N17 C23 124.2(3) . . ? C25 N17 C26 113.0(3) . . ? C23 N17 C26 122.7(3) . . ? C25 N18 C29 122.4(3) . . ? C25 N18 C27 111.3(3) . . ? C29 N18 C27 124.3(3) . . ? C28 N19 C26 111.9(3) . . ? C28 N19 C24 122.6(3) . . ? C26 N19 C24 123.9(3) . . ? C28 N20 C30 122.3(3) . . ? C28 N20 C27 111.8(3) . . ? C30 N20 C27 125.6(3) . . ? C31 N21 C32 114.0(3) . . ? C31 N21 C29 122.6(3) . . ? C32 N21 C29 121.6(3) . . ? C31 N22 C33 112.6(3) . . ? C31 N22 C35 122.4(3) . . ? C33 N22 C35 123.2(3) . . ? C34 N23 C30 124.3(3) . . ? C34 N23 C32 111.2(3) . . ? C30 N23 C32 123.0(3) . . ? C34 N24 C33 113.0(3) . . ? C34 N24 C36 122.7(3) . . ? C33 N24 C36 123.5(3) . . ? C1 O1 Y2 157.4(3) . . ? C7 O2 Y2 154.2(2) . . ? C19 O7 Y2 156.9(3) . . ? C25 O8 Y2 155.5(3) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.891 _refine_diff_density_min -0.630 _refine_diff_density_rms 0.083 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 95 37 ' ' 2 -0.065 0.500 0.269 1090 405 ' ' 3 0.500 1.000 0.500 93 38 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 902605' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p206 #TrackingRef 'submit-206.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H94 Cd Cl5 N24 O41 Sm' _chemical_formula_weight 1959.35 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 '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 15.1400(7) _cell_length_b 15.7332(7) _cell_length_c 17.1707(8) _cell_angle_alpha 64.1840(10) _cell_angle_beta 81.023(2) _cell_angle_gamma 81.956(2) _cell_volume 3624.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.795 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2002 _exptl_absorpt_coefficient_mu 1.393 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7586 _exptl_absorpt_correction_T_max 0.8289 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37877 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0432 _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 -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12587 _reflns_number_gt 10587 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0711P)^2^+10.7091P] 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 12587 _refine_ls_number_parameters 758 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1489 _refine_ls_wR_factor_gt 0.1428 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 Cl6 Cl -0.01385(11) 0.30126(13) 0.55075(13) 0.0620(5) Uani 1 1 d . . . O1W O 0.0621(3) 0.6352(3) 0.6405(3) 0.0446(10) Uani 1 1 d . . . O2W O 0.1031(3) 0.4810(3) 0.8057(3) 0.0459(10) Uani 1 1 d . . . O3W O 0.2632(3) 0.7416(3) 0.6073(3) 0.0463(10) Uani 1 1 d . . . O4W O 0.3723(3) 0.5652(3) 0.6629(3) 0.0476(10) Uani 1 1 d . . . Sm1 Sm 0.209003(17) 0.58667(2) 0.691926(18) 0.03219(10) Uani 1 1 d . . . Cl1 Cl 0.62232(14) -0.02910(15) 0.7976(2) 0.0982(9) Uani 1 1 d . A . Cl2 Cl 0.51202(13) -0.26021(17) 0.84701(18) 0.0872(7) Uani 1 1 d . A . Cl3 Cl 0.34979(14) -0.0368(2) 0.8351(2) 0.1359(15) Uani 1 1 d . A . Cl4 Cl 0.5132(11) -0.1655(6) 1.0348(3) 0.157(5) Uani 0.69(2) 1 d P A 1 Cl4' Cl 0.4603(7) -0.2040(11) 1.0312(6) 0.093(5) Uani 0.31(2) 1 d P A 2 Cd1 Cd 0.49451(4) -0.12094(4) 0.88039(4) 0.0731(2) Uani 1 1 d . . . C1 C 0.2154(3) 0.5950(4) 0.4807(3) 0.0305(11) Uani 1 1 d . . . C2 C 0.2218(3) 0.6142(4) 0.3378(4) 0.0354(12) Uani 1 1 d . . . H2 H 0.1800 0.6578 0.2958 0.042 Uiso 1 1 calc R . . C3 C 0.1814(3) 0.5183(4) 0.4012(3) 0.0347(12) Uani 1 1 d . . . H3 H 0.1200 0.5164 0.3892 0.042 Uiso 1 1 calc R . . C4 C 0.3118(4) 0.4865(5) 0.3221(4) 0.0385(13) Uani 1 1 d . . . C5 C 0.1392(3) 0.4472(4) 0.5671(4) 0.0361(12) Uani 1 1 d . . . H5A H 0.1131 0.4778 0.6053 0.043 Uiso 1 1 calc R . . H5B H 0.0904 0.4229 0.5534 0.043 Uiso 1 1 calc R . . C6 C 0.2348(4) 0.3473(4) 0.4293(4) 0.0436(14) Uani 1 1 d . . . H6A H 0.1711 0.3361 0.4394 0.052 Uiso 1 1 calc R . . H6B H 0.2646 0.3178 0.3912 0.052 Uiso 1 1 calc R . . C7 C 0.2505(3) 0.3686(4) 0.6722(4) 0.0341(12) Uani 1 1 d . . . C8 C 0.2227(4) 0.2860(4) 0.5955(4) 0.0384(13) Uani 1 1 d . . . H8 H 0.1689 0.2515 0.6062 0.046 Uiso 1 1 calc R . . C9 C 0.2919(4) 0.2268(4) 0.6606(4) 0.0359(12) Uani 1 1 d . . . H9 H 0.2688 0.1662 0.7041 0.043 Uiso 1 1 calc R . . C10 C 0.3541(4) 0.2527(4) 0.5197(4) 0.0428(14) Uani 1 1 d . . . C11 C 0.3525(3) 0.2566(4) 0.7766(4) 0.0371(12) Uani 1 1 d . . . H11A H 0.3279 0.2937 0.8096 0.045 Uiso 1 1 calc R . . H11B H 0.3423 0.1901 0.8142 0.045 Uiso 1 1 calc R . . C12 C 0.4474(4) 0.1483(4) 0.6374(4) 0.0417(13) Uani 1 1 d . . . H12A H 0.4763 0.1274 0.5928 0.050 Uiso 1 1 calc R . . H12B H 0.4284 0.0920 0.6891 0.050 Uiso 1 1 calc R . . C13 C 0.4906(3) 0.3303(4) 0.7651(3) 0.0310(11) Uani 1 1 d . . . C14 C 0.5087(4) 0.1918(4) 0.7440(4) 0.0359(12) Uani 1 1 d . . . H14 H 0.4984 0.1284 0.7916 0.043 Uiso 1 1 calc R . . C15 C 0.6028(4) 0.2226(4) 0.7424(4) 0.0374(12) Uani 1 1 d . . . H15 H 0.6366 0.1740 0.7894 0.045 Uiso 1 1 calc R . . C16 C 0.5943(4) 0.2151(4) 0.6108(4) 0.0351(12) Uani 1 1 d . . . C17 C 0.3561(4) 0.6487(4) 0.2216(4) 0.0390(13) Uani 1 1 d . . . H17A H 0.3883 0.6149 0.1880 0.047 Uiso 1 1 calc R . . H17B H 0.3162 0.6995 0.1839 0.047 Uiso 1 1 calc R . . C18 C 0.2601(3) 0.7492(4) 0.3669(4) 0.0376(12) Uani 1 1 d . . . H18A H 0.2269 0.7888 0.3169 0.045 Uiso 1 1 calc R . . H18B H 0.2385 0.7698 0.4133 0.045 Uiso 1 1 calc R . . C19 C 0.1280(3) 0.7424(4) 0.7906(3) 0.0316(11) Uani 1 1 d . . . C20 C 0.0632(4) 0.8488(4) 0.8491(4) 0.0358(12) Uani 1 1 d . . . H20 H 0.0534 0.9181 0.8150 0.043 Uiso 1 1 calc R . . C21 C 0.1620(4) 0.8170(4) 0.8732(4) 0.0367(12) Uani 1 1 d . . . H21 H 0.1986 0.8716 0.8531 0.044 Uiso 1 1 calc R . . C22 C 0.0644(4) 0.7716(4) 1.0008(4) 0.0433(14) Uani 1 1 d . . . C23 C 0.2849(3) 0.7143(4) 0.8250(4) 0.0339(12) Uani 1 1 d . . . H23A H 0.3008 0.7095 0.7694 0.041 Uiso 1 1 calc R . . H23B H 0.3255 0.7561 0.8277 0.041 Uiso 1 1 calc R . . C24 C 0.2265(4) 0.7298(4) 1.0200(4) 0.0414(13) Uani 1 1 d . . . H24A H 0.2763 0.7702 0.9913 0.050 Uiso 1 1 calc R . . H24B H 0.2075 0.7323 1.0763 0.050 Uiso 1 1 calc R . . C25 C 0.2890(3) 0.5409(4) 0.8908(3) 0.0311(11) Uani 1 1 d . . . C26 C 0.3265(3) 0.6060(4) 0.9793(3) 0.0338(12) Uani 1 1 d . . . H26 H 0.3838 0.6337 0.9719 0.041 Uiso 1 1 calc R . . C27 C 0.3352(3) 0.4964(4) 1.0273(3) 0.0326(11) Uani 1 1 d . . . H27 H 0.3978 0.4716 1.0391 0.039 Uiso 1 1 calc R . . C28 C 0.2348(3) 0.5577(4) 1.1108(4) 0.0355(12) Uani 1 1 d . . . C29 C 0.3207(4) 0.3691(4) 0.9768(4) 0.0379(13) Uani 1 1 d . . . H29A H 0.3277 0.3702 0.9187 0.046 Uiso 1 1 calc R . . H29B H 0.3772 0.3413 1.0023 0.046 Uiso 1 1 calc R . . C30 C 0.2681(4) 0.3849(5) 1.1794(4) 0.0424(14) Uani 1 1 d . . . H30A H 0.2433 0.3935 1.2319 0.051 Uiso 1 1 calc R . . H30B H 0.3279 0.3515 1.1891 0.051 Uiso 1 1 calc R . . C31 C 0.1916(4) 0.2804(4) 0.9962(4) 0.0374(12) Uani 1 1 d . . . C32 C 0.2437(3) 0.2649(4) 1.1236(3) 0.0360(12) Uani 1 1 d . . . H32 H 0.3002 0.2279 1.1454 0.043 Uiso 1 1 calc R . . C33 C 0.1656(4) 0.1995(4) 1.1476(4) 0.0371(12) Uani 1 1 d . . . H33 H 0.1857 0.1320 1.1805 0.045 Uiso 1 1 calc R . . C34 C 0.1291(3) 0.3058(4) 1.2126(4) 0.0364(12) Uani 1 1 d . . . C35 C -0.0820(4) 0.8408(4) 0.9479(4) 0.0439(14) Uani 1 1 d . . . H35A H -0.0950 0.9069 0.9074 0.053 Uiso 1 1 calc R . . H35B H -0.0965 0.8364 1.0071 0.053 Uiso 1 1 calc R . . C36 C -0.0223(3) 0.8146(4) 0.7508(4) 0.0365(12) Uani 1 1 d . . . H36A H -0.0393 0.8829 0.7250 0.044 Uiso 1 1 calc R . . H36B H -0.0027 0.7958 0.7030 0.044 Uiso 1 1 calc R . . N1 N 0.2410(3) 0.6510(3) 0.3970(3) 0.0351(10) Uani 1 1 d . . . N2 N 0.1814(3) 0.5179(3) 0.4862(3) 0.0365(10) Uani 1 1 d . . . N3 N 0.3022(3) 0.5834(4) 0.2957(3) 0.0377(11) Uani 1 1 d . . . N4 N 0.2430(3) 0.4487(4) 0.3846(3) 0.0385(11) Uani 1 1 d . . . N5 N 0.2013(3) 0.3693(3) 0.6123(3) 0.0376(10) Uani 1 1 d . . . N6 N 0.3043(3) 0.2878(3) 0.7014(3) 0.0322(10) Uani 1 1 d . . . N7 N 0.2724(3) 0.3013(4) 0.5117(3) 0.0414(11) Uani 1 1 d . . . N8 N 0.3687(3) 0.2108(3) 0.6056(3) 0.0387(11) Uani 1 1 d . . . N9 N 0.4467(3) 0.2651(3) 0.7564(3) 0.0347(10) Uani 1 1 d . . . N10 N 0.5804(3) 0.3103(4) 0.7542(3) 0.0379(11) Uani 1 1 d . . . N11 N 0.5130(3) 0.1914(3) 0.6599(3) 0.0387(11) Uani 1 1 d . . . N12 N 0.6459(3) 0.2359(3) 0.6580(3) 0.0353(10) Uani 1 1 d . . . N13 N 0.0524(3) 0.7964(3) 0.8007(3) 0.0332(10) Uani 1 1 d . . . N14 N 0.1936(3) 0.7560(3) 0.8281(3) 0.0343(10) Uani 1 1 d . . . N15 N 0.0116(3) 0.8158(3) 0.9350(3) 0.0367(10) Uani 1 1 d . . . N16 N 0.1518(3) 0.7668(4) 0.9665(3) 0.0436(12) Uani 1 1 d . . . N17 N 0.2977(3) 0.6217(3) 0.8949(3) 0.0386(11) Uani 1 1 d . . . N18 N 0.3047(3) 0.4655(3) 0.9683(3) 0.0360(10) Uani 1 1 d . . . N19 N 0.2574(3) 0.6337(4) 1.0346(3) 0.0418(11) Uani 1 1 d . . . N20 N 0.2763(3) 0.4768(4) 1.1067(3) 0.0400(11) Uani 1 1 d . . . N21 N 0.2510(3) 0.3097(3) 1.0291(3) 0.0377(11) Uani 1 1 d . . . N22 N 0.1394(3) 0.2170(4) 1.0642(3) 0.0383(11) Uani 1 1 d . . . N23 N 0.2108(3) 0.3268(4) 1.1652(3) 0.0386(11) Uani 1 1 d . . . N24 N 0.0998(3) 0.2337(3) 1.1998(3) 0.0371(10) Uani 1 1 d . . . O1 O 0.2210(2) 0.6125(3) 0.5438(2) 0.0391(9) Uani 1 1 d . . . O2 O 0.2445(3) 0.4303(3) 0.6991(3) 0.0418(9) Uani 1 1 d . . . O3 O 0.4530(2) 0.3975(3) 0.7805(3) 0.0382(9) Uani 1 1 d . . . O4 O 0.3716(3) 0.4435(3) 0.2929(3) 0.0502(11) Uani 1 1 d . . . O5 O 0.4056(3) 0.2438(4) 0.4613(3) 0.0607(12) Uani 1 1 d . . . O6 O 0.6167(3) 0.2135(3) 0.5394(3) 0.0505(11) Uani 1 1 d . . . O7 O 0.1362(2) 0.6915(3) 0.7522(2) 0.0376(9) Uani 1 1 d . . . O8 O 0.2703(3) 0.5329(3) 0.8268(2) 0.0401(9) Uani 1 1 d . . . O9 O 0.1864(3) 0.3054(3) 0.9193(3) 0.0472(10) Uani 1 1 d . . . O10 O 0.0382(3) 0.7416(3) 1.0787(3) 0.0535(11) Uani 1 1 d . . . O11 O 0.1858(3) 0.5631(3) 1.1731(3) 0.0485(10) Uani 1 1 d . . . O12 O 0.0907(3) 0.3436(3) 1.2591(3) 0.0462(10) 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 Cl6 0.0480(9) 0.0633(11) 0.0718(12) -0.0220(9) -0.0211(8) -0.0020(8) O1W 0.035(2) 0.063(3) 0.031(2) -0.019(2) 0.0000(16) 0.0039(18) O2W 0.041(2) 0.051(3) 0.040(2) -0.017(2) 0.0066(18) -0.0089(18) O3W 0.053(2) 0.043(2) 0.037(2) -0.014(2) 0.0079(19) -0.0069(19) O4W 0.037(2) 0.059(3) 0.045(3) -0.021(2) -0.0011(18) -0.0044(19) Sm1 0.03055(15) 0.04110(18) 0.02584(16) -0.01639(13) -0.00183(11) 0.00054(11) Cl1 0.0519(11) 0.0581(12) 0.163(3) -0.0331(15) 0.0061(13) -0.0033(9) Cl2 0.0440(10) 0.0894(15) 0.124(2) -0.0374(15) -0.0131(11) -0.0115(9) Cl3 0.0422(10) 0.0885(17) 0.170(3) 0.0382(18) 0.0038(14) -0.0016(10) Cl4 0.254(14) 0.131(5) 0.060(3) -0.016(3) -0.039(4) 0.011(7) Cl4' 0.090(7) 0.116(9) 0.039(4) 0.000(4) 0.004(4) -0.026(5) Cd1 0.0547(3) 0.0577(3) 0.0666(4) 0.0066(3) 0.0005(3) 0.0023(3) C1 0.025(2) 0.043(3) 0.024(3) -0.016(2) -0.002(2) 0.002(2) C2 0.029(3) 0.050(3) 0.029(3) -0.017(3) -0.008(2) 0.001(2) C3 0.032(3) 0.050(3) 0.029(3) -0.021(3) -0.009(2) -0.006(2) C4 0.034(3) 0.064(4) 0.031(3) -0.031(3) -0.009(2) -0.003(3) C5 0.028(3) 0.048(3) 0.033(3) -0.019(3) 0.000(2) -0.002(2) C6 0.050(3) 0.047(4) 0.037(3) -0.020(3) -0.003(3) -0.012(3) C7 0.033(3) 0.034(3) 0.029(3) -0.008(2) 0.007(2) -0.009(2) C8 0.036(3) 0.039(3) 0.040(3) -0.016(3) -0.003(2) -0.009(2) C9 0.039(3) 0.033(3) 0.032(3) -0.011(2) 0.000(2) -0.007(2) C10 0.049(3) 0.047(3) 0.037(3) -0.024(3) 0.006(3) -0.006(3) C11 0.036(3) 0.045(3) 0.033(3) -0.020(3) -0.004(2) -0.003(2) C12 0.039(3) 0.037(3) 0.052(4) -0.025(3) 0.000(3) 0.001(2) C13 0.031(3) 0.039(3) 0.022(3) -0.011(2) -0.006(2) -0.005(2) C14 0.036(3) 0.036(3) 0.028(3) -0.008(2) -0.003(2) 0.000(2) C15 0.034(3) 0.046(3) 0.025(3) -0.012(3) -0.002(2) 0.007(2) C16 0.038(3) 0.033(3) 0.032(3) -0.013(2) -0.002(2) -0.004(2) C17 0.036(3) 0.058(4) 0.028(3) -0.023(3) -0.005(2) -0.001(3) C18 0.029(3) 0.038(3) 0.041(3) -0.014(3) -0.003(2) 0.002(2) C19 0.030(3) 0.035(3) 0.026(3) -0.012(2) 0.005(2) -0.005(2) C20 0.040(3) 0.032(3) 0.039(3) -0.019(3) -0.001(2) -0.005(2) C21 0.039(3) 0.031(3) 0.038(3) -0.013(3) 0.002(2) -0.005(2) C22 0.049(3) 0.048(4) 0.042(4) -0.028(3) -0.003(3) -0.005(3) C23 0.033(3) 0.041(3) 0.031(3) -0.016(3) -0.006(2) -0.007(2) C24 0.053(3) 0.045(3) 0.034(3) -0.020(3) -0.008(3) -0.013(3) C25 0.022(2) 0.043(3) 0.030(3) -0.017(3) -0.001(2) -0.006(2) C26 0.029(2) 0.057(4) 0.026(3) -0.024(3) -0.007(2) -0.008(2) C27 0.025(2) 0.042(3) 0.028(3) -0.012(2) -0.003(2) -0.005(2) C28 0.028(3) 0.048(3) 0.037(3) -0.023(3) -0.006(2) -0.003(2) C29 0.032(3) 0.050(3) 0.031(3) -0.019(3) 0.000(2) 0.000(2) C30 0.039(3) 0.057(4) 0.031(3) -0.016(3) -0.007(2) -0.009(3) C31 0.040(3) 0.037(3) 0.029(3) -0.011(3) 0.002(2) 0.002(2) C32 0.030(3) 0.047(3) 0.026(3) -0.014(3) -0.002(2) 0.005(2) C33 0.040(3) 0.034(3) 0.028(3) -0.008(2) 0.004(2) 0.002(2) C34 0.028(3) 0.051(3) 0.030(3) -0.017(3) -0.004(2) -0.002(2) C35 0.044(3) 0.044(3) 0.050(4) -0.029(3) 0.001(3) 0.001(3) C36 0.032(3) 0.039(3) 0.031(3) -0.007(3) -0.004(2) -0.004(2) N1 0.033(2) 0.045(3) 0.027(2) -0.017(2) 0.0011(19) -0.003(2) N2 0.036(2) 0.049(3) 0.027(2) -0.017(2) -0.0019(19) -0.004(2) N3 0.033(2) 0.051(3) 0.031(3) -0.020(2) 0.0005(19) -0.005(2) N4 0.036(2) 0.050(3) 0.035(3) -0.023(2) -0.004(2) -0.005(2) N5 0.037(2) 0.042(3) 0.037(3) -0.019(2) -0.004(2) -0.002(2) N6 0.032(2) 0.039(3) 0.028(2) -0.016(2) -0.0046(18) -0.0048(19) N7 0.040(3) 0.054(3) 0.035(3) -0.025(2) -0.004(2) 0.001(2) N8 0.037(2) 0.045(3) 0.038(3) -0.023(2) 0.002(2) -0.004(2) N9 0.031(2) 0.039(3) 0.037(3) -0.018(2) -0.0046(19) -0.0027(19) N10 0.036(2) 0.050(3) 0.029(3) -0.019(2) -0.0021(19) -0.003(2) N11 0.035(2) 0.043(3) 0.039(3) -0.018(2) -0.001(2) -0.007(2) N12 0.033(2) 0.038(3) 0.034(3) -0.015(2) -0.0024(19) -0.0045(19) N13 0.034(2) 0.034(2) 0.030(2) -0.014(2) -0.0039(19) 0.0025(18) N14 0.032(2) 0.041(3) 0.031(2) -0.018(2) 0.0036(19) -0.0072(19) N15 0.039(2) 0.045(3) 0.030(3) -0.020(2) -0.001(2) -0.006(2) N16 0.041(3) 0.054(3) 0.044(3) -0.029(3) -0.003(2) -0.001(2) N17 0.038(2) 0.043(3) 0.033(3) -0.012(2) -0.007(2) -0.003(2) N18 0.033(2) 0.046(3) 0.026(2) -0.014(2) -0.0020(19) -0.001(2) N19 0.045(3) 0.054(3) 0.031(3) -0.022(2) 0.002(2) -0.007(2) N20 0.036(2) 0.055(3) 0.026(2) -0.016(2) 0.0046(19) -0.011(2) N21 0.033(2) 0.050(3) 0.028(2) -0.016(2) -0.0006(19) -0.001(2) N22 0.038(2) 0.049(3) 0.036(3) -0.025(2) -0.001(2) -0.010(2) N23 0.035(2) 0.050(3) 0.033(3) -0.022(2) 0.004(2) -0.005(2) N24 0.034(2) 0.049(3) 0.028(2) -0.018(2) -0.0014(19) 0.003(2) O1 0.037(2) 0.051(2) 0.034(2) -0.0237(19) 0.0008(16) -0.0055(17) O2 0.048(2) 0.040(2) 0.039(2) -0.0197(19) -0.0062(18) 0.0033(18) O3 0.040(2) 0.041(2) 0.038(2) -0.0199(19) -0.0051(17) -0.0042(17) O4 0.044(2) 0.063(3) 0.054(3) -0.037(2) 0.002(2) -0.003(2) O5 0.059(3) 0.078(3) 0.048(3) -0.033(3) 0.000(2) 0.004(2) O6 0.051(2) 0.068(3) 0.040(3) -0.032(2) 0.007(2) -0.013(2) O7 0.0361(19) 0.050(2) 0.029(2) -0.0221(19) 0.0008(16) 0.0004(17) O8 0.043(2) 0.049(2) 0.030(2) -0.0196(19) -0.0067(17) 0.0038(18) O9 0.049(2) 0.052(3) 0.037(3) -0.018(2) -0.0004(19) -0.0030(19) O10 0.061(3) 0.072(3) 0.030(2) -0.025(2) -0.003(2) -0.002(2) O11 0.046(2) 0.068(3) 0.035(2) -0.026(2) 0.0000(19) -0.006(2) O12 0.041(2) 0.063(3) 0.045(3) -0.035(2) 0.0086(19) -0.0099(19) _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 O1W Sm1 2.421(4) . ? O2W Sm1 2.468(4) . ? O3W Sm1 2.414(4) . ? O4W Sm1 2.450(4) . ? Sm1 O7 2.373(4) . ? Sm1 O1 2.376(4) . ? Sm1 O8 2.384(4) . ? Sm1 O2 2.396(4) . ? Cl1 Cd1 2.447(2) . ? Cl2 Cd1 2.467(3) . ? Cl3 Cd1 2.446(2) . ? Cl4 Cd1 2.483(6) . ? Cl4' Cd1 2.347(8) . ? C1 O1 1.246(6) . ? C1 N2 1.342(7) . ? C1 N1 1.346(7) . ? C2 N3 1.451(7) . ? C2 N1 1.452(7) . ? C2 C3 1.567(8) . ? C2 H2 0.9900 . ? C3 N4 1.433(7) . ? C3 N2 1.457(7) . ? C3 H3 0.9900 . ? C4 O4 1.229(7) . ? C4 N4 1.365(7) . ? C4 N3 1.380(8) . ? C5 N5 1.437(7) . ? C5 N2 1.467(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.448(8) . ? C6 N4 1.452(8) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.233(7) . ? C7 N6 1.346(7) . ? C7 N5 1.356(7) . ? C8 N5 1.444(7) . ? C8 N7 1.451(7) . ? C8 C9 1.550(8) . ? C8 H8 0.9900 . ? C9 N8 1.445(7) . ? C9 N6 1.459(7) . ? C9 H9 0.9900 . ? C10 O5 1.216(7) . ? C10 N7 1.353(8) . ? C10 N8 1.369(8) . ? C11 N9 1.425(7) . ? C11 N6 1.443(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.447(7) . ? C12 N11 1.460(7) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.241(6) . ? C13 N10 1.355(7) . ? C13 N9 1.367(7) . ? C14 N11 1.437(7) . ? C14 N9 1.452(7) . ? C14 C15 1.562(8) . ? C14 H14 0.9900 . ? C15 N12 1.433(7) . ? C15 N10 1.466(7) . ? C15 H15 0.9900 . ? C16 O6 1.230(7) . ? C16 N12 1.369(7) . ? C16 N11 1.377(7) . ? C17 N10 1.429(7) 2_666 ? C17 N3 1.453(7) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.441(7) 2_666 ? C18 N1 1.456(7) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O7 1.223(6) . ? C19 N14 1.350(7) . ? C19 N13 1.362(7) . ? C20 N13 1.442(7) . ? C20 N15 1.464(7) . ? C20 C21 1.568(8) . ? C20 H20 0.9900 . ? C21 N16 1.438(8) . ? C21 N14 1.468(7) . ? C21 H21 0.9900 . ? C22 O10 1.227(7) . ? C22 N15 1.357(8) . ? C22 N16 1.367(8) . ? C23 N17 1.438(7) . ? C23 N14 1.449(7) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N19 1.441(8) . ? C24 N16 1.462(8) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O8 1.237(6) . ? C25 N17 1.330(7) . ? C25 N18 1.371(7) . ? C26 N19 1.451(7) . ? C26 N17 1.485(7) . ? C26 C27 1.550(8) . ? C26 H26 0.9900 . ? C27 N20 1.443(7) . ? C27 N18 1.453(7) . ? C27 H27 0.9900 . ? C28 O11 1.232(7) . ? C28 N20 1.363(7) . ? C28 N19 1.368(8) . ? C29 N21 1.429(7) . ? C29 N18 1.449(7) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N20 1.447(8) . ? C30 N23 1.459(7) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O9 1.216(7) . ? C31 N21 1.356(7) . ? C31 N22 1.379(7) . ? C32 N23 1.437(7) . ? C32 N21 1.454(7) . ? C32 C33 1.564(8) . ? C32 H32 0.9900 . ? C33 N24 1.442(7) . ? C33 N22 1.443(7) . ? C33 H33 0.9900 . ? C34 O12 1.225(7) . ? C34 N23 1.367(7) . ? C34 N24 1.386(7) . ? C35 N15 1.426(7) . ? C35 N22 1.438(7) 2_567 ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N24 1.433(7) 2_567 ? C36 N13 1.446(7) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? N10 C17 1.429(7) 2_666 ? N12 C18 1.441(7) 2_666 ? N22 C35 1.438(7) 2_567 ? N24 C36 1.433(7) 2_567 ? 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 Sm1 O1 126.61(13) . . ? O7 Sm1 O8 76.11(13) . . ? O1 Sm1 O8 151.76(13) . . ? O7 Sm1 O2 151.03(14) . . ? O1 Sm1 O2 76.91(14) . . ? O8 Sm1 O2 88.31(13) . . ? O7 Sm1 O3W 71.00(13) . . ? O1 Sm1 O3W 73.61(14) . . ? O8 Sm1 O3W 103.72(14) . . ? O2 Sm1 O3W 137.31(14) . . ? O7 Sm1 O1W 73.12(13) . . ? O1 Sm1 O1W 70.71(13) . . ? O8 Sm1 O1W 137.11(13) . . ? O2 Sm1 O1W 104.89(14) . . ? O3W Sm1 O1W 93.74(15) . . ? O7 Sm1 O4W 123.39(14) . . ? O1 Sm1 O4W 80.09(14) . . ? O8 Sm1 O4W 72.53(14) . . ? O2 Sm1 O4W 72.71(14) . . ? O3W Sm1 O4W 72.35(15) . . ? O1W Sm1 O4W 150.29(14) . . ? O7 Sm1 O2W 80.28(14) . . ? O1 Sm1 O2W 122.94(14) . . ? O8 Sm1 O2W 72.98(14) . . ? O2 Sm1 O2W 71.79(14) . . ? O3W Sm1 O2W 150.89(14) . . ? O1W Sm1 O2W 72.97(14) . . ? O4W Sm1 O2W 130.44(15) . . ? Cl4' Cd1 Cl3 102.0(3) . . ? Cl4' Cd1 Cl1 130.0(4) . . ? Cl3 Cd1 Cl1 113.26(8) . . ? Cl4' Cd1 Cl2 96.3(5) . . ? Cl3 Cd1 Cl2 106.76(11) . . ? Cl1 Cd1 Cl2 105.51(8) . . ? Cl4' Cd1 Cl4 26.0(2) . . ? Cl3 Cd1 Cl4 114.5(3) . . ? Cl1 Cd1 Cl4 104.5(4) . . ? Cl2 Cd1 Cl4 112.0(2) . . ? O1 C1 N2 124.8(5) . . ? O1 C1 N1 125.2(5) . . ? N2 C1 N1 110.0(4) . . ? N3 C2 N1 112.9(4) . . ? N3 C2 C3 102.6(4) . . ? N1 C2 C3 102.6(4) . . ? N3 C2 H2 112.6 . . ? N1 C2 H2 112.6 . . ? C3 C2 H2 112.6 . . ? N4 C3 N2 115.3(4) . . ? N4 C3 C2 103.4(4) . . ? N2 C3 C2 102.6(4) . . ? N4 C3 H3 111.6 . . ? N2 C3 H3 111.6 . . ? C2 C3 H3 111.6 . . ? O4 C4 N4 127.0(6) . . ? O4 C4 N3 125.3(6) . . ? N4 C4 N3 107.7(5) . . ? N5 C5 N2 112.7(4) . . ? N5 C5 H5A 109.0 . . ? N2 C5 H5A 109.0 . . ? N5 C5 H5B 109.0 . . ? N2 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N7 C6 N4 114.5(5) . . ? N7 C6 H6A 108.6 . . ? N4 C6 H6A 108.6 . . ? N7 C6 H6B 108.6 . . ? N4 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? O2 C7 N6 124.5(5) . . ? O2 C7 N5 125.5(5) . . ? N6 C7 N5 109.9(5) . . ? N5 C8 N7 115.4(5) . . ? N5 C8 C9 102.7(4) . . ? N7 C8 C9 103.1(4) . . ? N5 C8 H8 111.6 . . ? N7 C8 H8 111.6 . . ? C9 C8 H8 111.6 . . ? N8 C9 N6 115.5(4) . . ? N8 C9 C8 103.3(4) . . ? N6 C9 C8 103.6(4) . . ? N8 C9 H9 111.3 . . ? N6 C9 H9 111.3 . . ? C8 C9 H9 111.3 . . ? O5 C10 N7 126.4(6) . . ? O5 C10 N8 124.7(6) . . ? N7 C10 N8 108.9(5) . . ? N9 C11 N6 114.0(5) . . ? N9 C11 H11A 108.7 . . ? N6 C11 H11A 108.7 . . ? N9 C11 H11B 108.7 . . ? N6 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? N8 C12 N11 113.9(5) . . ? N8 C12 H12A 108.8 . . ? N11 C12 H12A 108.8 . . ? N8 C12 H12B 108.8 . . ? N11 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N10 125.6(5) . . ? O3 C13 N9 124.6(5) . . ? N10 C13 N9 109.8(5) . . ? N11 C14 N9 114.9(4) . . ? N11 C14 C15 102.7(4) . . ? N9 C14 C15 103.6(4) . . ? N11 C14 H14 111.7 . . ? N9 C14 H14 111.7 . . ? C15 C14 H14 111.7 . . ? N12 C15 N10 114.4(5) . . ? N12 C15 C14 103.5(4) . . ? N10 C15 C14 102.8(4) . . ? N12 C15 H15 111.8 . . ? N10 C15 H15 111.8 . . ? C14 C15 H15 111.8 . . ? O6 C16 N12 127.0(5) . . ? O6 C16 N11 125.6(5) . . ? N12 C16 N11 107.4(5) . . ? N10 C17 N3 113.3(4) 2_666 . ? N10 C17 H17A 108.9 2_666 . ? N3 C17 H17A 108.9 . . ? N10 C17 H17B 108.9 2_666 . ? N3 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? N12 C18 N1 113.6(4) 2_666 . ? N12 C18 H18A 108.9 2_666 . ? N1 C18 H18A 108.9 . . ? N12 C18 H18B 108.9 2_666 . ? N1 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? O7 C19 N14 125.3(5) . . ? O7 C19 N13 125.8(5) . . ? N14 C19 N13 108.8(4) . . ? N13 C20 N15 113.7(4) . . ? N13 C20 C21 103.1(4) . . ? N15 C20 C21 101.9(4) . . ? N13 C20 H20 112.5 . . ? N15 C20 H20 112.5 . . ? C21 C20 H20 112.5 . . ? N16 C21 N14 113.8(5) . . ? N16 C21 C20 104.0(4) . . ? N14 C21 C20 102.2(4) . . ? N16 C21 H21 112.1 . . ? N14 C21 H21 112.1 . . ? C20 C21 H21 112.1 . . ? O10 C22 N15 125.5(6) . . ? O10 C22 N16 125.4(6) . . ? N15 C22 N16 109.1(5) . . ? N17 C23 N14 112.8(4) . . ? N17 C23 H23A 109.0 . . ? N14 C23 H23A 109.0 . . ? N17 C23 H23B 109.0 . . ? N14 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? N19 C24 N16 112.4(4) . . ? N19 C24 H24A 109.1 . . ? N16 C24 H24A 109.1 . . ? N19 C24 H24B 109.1 . . ? N16 C24 H24B 109.1 . . ? H24A C24 H24B 107.8 . . ? O8 C25 N17 126.0(5) . . ? O8 C25 N18 123.8(5) . . ? N17 C25 N18 110.2(5) . . ? N19 C26 N17 114.0(4) . . ? N19 C26 C27 103.3(4) . . ? N17 C26 C27 101.9(4) . . ? N19 C26 H26 112.3 . . ? N17 C26 H26 112.3 . . ? C27 C26 H26 112.3 . . ? N20 C27 N18 114.0(4) . . ? N20 C27 C26 103.6(4) . . ? N18 C27 C26 104.2(4) . . ? N20 C27 H27 111.5 . . ? N18 C27 H27 111.5 . . ? C26 C27 H27 111.5 . . ? O11 C28 N20 126.2(6) . . ? O11 C28 N19 124.5(5) . . ? N20 C28 N19 109.2(5) . . ? N21 C29 N18 114.1(4) . . ? N21 C29 H29A 108.7 . . ? N18 C29 H29A 108.7 . . ? N21 C29 H29B 108.7 . . ? N18 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? N20 C30 N23 112.5(5) . . ? N20 C30 H30A 109.1 . . ? N23 C30 H30A 109.1 . . ? N20 C30 H30B 109.1 . . ? N23 C30 H30B 109.1 . . ? H30A C30 H30B 107.8 . . ? O9 C31 N21 125.2(5) . . ? O9 C31 N22 125.9(6) . . ? N21 C31 N22 108.8(5) . . ? N23 C32 N21 115.2(5) . . ? N23 C32 C33 103.4(4) . . ? N21 C32 C33 102.6(4) . . ? N23 C32 H32 111.7 . . ? N21 C32 H32 111.7 . . ? C33 C32 H32 111.7 . . ? N24 C33 N22 114.7(5) . . ? N24 C33 C32 103.1(4) . . ? N22 C33 C32 103.8(4) . . ? N24 C33 H33 111.5 . . ? N22 C33 H33 111.5 . . ? C32 C33 H33 111.5 . . ? O12 C34 N23 125.2(5) . . ? O12 C34 N24 127.1(5) . . ? N23 C34 N24 107.7(5) . . ? N15 C35 N22 114.6(5) . 2_567 ? N15 C35 H35A 108.6 . . ? N22 C35 H35A 108.6 2_567 . ? N15 C35 H35B 108.6 . . ? N22 C35 H35B 108.6 2_567 . ? H35A C35 H35B 107.6 . . ? N24 C36 N13 114.3(4) 2_567 . ? N24 C36 H36A 108.7 2_567 . ? N13 C36 H36A 108.7 . . ? N24 C36 H36B 108.7 2_567 . ? N13 C36 H36B 108.7 . . ? H36A C36 H36B 107.6 . . ? C1 N1 C2 112.4(5) . . ? C1 N1 C18 123.3(5) . . ? C2 N1 C18 121.9(5) . . ? C1 N2 C3 112.3(4) . . ? C1 N2 C5 123.9(4) . . ? C3 N2 C5 123.4(4) . . ? C4 N3 C2 112.7(5) . . ? C4 N3 C17 123.3(5) . . ? C2 N3 C17 122.9(5) . . ? C4 N4 C3 113.5(5) . . ? C4 N4 C6 122.2(5) . . ? C3 N4 C6 124.3(5) . . ? C7 N5 C5 123.4(5) . . ? C7 N5 C8 112.4(5) . . ? C5 N5 C8 124.2(5) . . ? C7 N6 C11 123.8(5) . . ? C7 N6 C9 111.3(4) . . ? C11 N6 C9 123.6(4) . . ? C10 N7 C6 122.0(5) . . ? C10 N7 C8 112.3(5) . . ? C6 N7 C8 124.8(5) . . ? C10 N8 C9 112.1(5) . . ? C10 N8 C12 123.1(5) . . ? C9 N8 C12 124.4(5) . . ? C13 N9 C11 124.4(5) . . ? C13 N9 C14 111.7(4) . . ? C11 N9 C14 122.4(4) . . ? C13 N10 C17 123.1(5) . 2_666 ? C13 N10 C15 111.9(4) . . ? C17 N10 C15 122.2(4) 2_666 . ? C16 N11 C14 113.2(4) . . ? C16 N11 C12 122.4(5) . . ? C14 N11 C12 122.8(5) . . ? C16 N12 C15 113.1(4) . . ? C16 N12 C18 123.3(5) . 2_666 ? C15 N12 C18 122.4(5) . 2_666 ? C19 N13 C20 113.0(4) . . ? C19 N13 C36 121.8(4) . . ? C20 N13 C36 123.7(4) . . ? C19 N14 C23 123.8(4) . . ? C19 N14 C21 112.6(4) . . ? C23 N14 C21 123.6(4) . . ? C22 N15 C35 123.6(5) . . ? C22 N15 C20 112.6(5) . . ? C35 N15 C20 123.1(5) . . ? C22 N16 C21 112.0(5) . . ? C22 N16 C24 122.8(5) . . ? C21 N16 C24 124.2(5) . . ? C25 N17 C23 124.6(5) . . ? C25 N17 C26 112.3(5) . . ? C23 N17 C26 123.1(5) . . ? C25 N18 C29 122.3(4) . . ? C25 N18 C27 111.0(4) . . ? C29 N18 C27 123.1(4) . . ? C28 N19 C24 122.5(5) . . ? C28 N19 C26 111.4(5) . . ? C24 N19 C26 125.3(5) . . ? C28 N20 C27 111.9(5) . . ? C28 N20 C30 122.1(5) . . ? C27 N20 C30 125.6(5) . . ? C31 N21 C29 123.6(5) . . ? C31 N21 C32 112.9(5) . . ? C29 N21 C32 123.0(4) . . ? C31 N22 C35 122.6(5) . 2_567 ? C31 N22 C33 111.9(4) . . ? C35 N22 C33 123.9(5) 2_567 . ? C34 N23 C32 113.1(5) . . ? C34 N23 C30 120.8(5) . . ? C32 N23 C30 123.3(5) . . ? C34 N24 C36 122.4(4) . 2_567 ? C34 N24 C33 112.5(4) . . ? C36 N24 C33 123.6(5) 2_567 . ? C1 O1 Sm1 157.5(4) . . ? C7 O2 Sm1 155.3(4) . . ? C19 O7 Sm1 157.9(3) . . ? C25 O8 Sm1 154.7(4) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.970 _refine_diff_density_min -0.777 _refine_diff_density_rms 0.112 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.006 0.000 0.010 1104 418 ' ' 2 0.000 0.500 0.000 98 38 ' ' 3 0.500 0.500 0.500 93 37 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 902606' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p207 #TrackingRef 'submit-207.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H96 Cd Cl5 Eu N24 O42' _chemical_formula_weight 1978.98 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 '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 15.1640(14) _cell_length_b 15.6132(14) _cell_length_c 17.1565(15) _cell_angle_alpha 64.327(3) _cell_angle_beta 81.022(3) _cell_angle_gamma 82.192(3) _cell_volume 3605.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.823 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 1.458 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7211 _exptl_absorpt_correction_T_max 0.8110 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40420 _diffrn_reflns_av_R_equivalents 0.0525 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.20 _reflns_number_total 12865 _reflns_number_gt 10463 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0779P)^2^+0.4326P] 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 12865 _refine_ls_number_parameters 748 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1399 _refine_ls_wR_factor_gt 0.1327 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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 Cl5 Cl -0.01265(10) 0.30280(13) 0.04725(12) 0.0719(4) Uani 1 1 d . . . O1W O 0.0641(2) 0.6362(3) 0.1416(2) 0.0536(9) Uani 1 1 d . . . O2W O 0.2638(3) 0.7432(3) 0.1086(2) 0.0564(9) Uani 1 1 d . . . O3W O 0.1052(2) 0.4838(3) 0.3041(2) 0.0529(9) Uani 1 1 d . . . O4W O 0.3718(2) 0.5665(3) 0.1639(3) 0.0563(9) Uani 1 1 d . . . Eu1 Eu 0.210199(13) 0.587930(17) 0.192361(14) 0.03677(10) Uani 1 1 d . . . Cl1 Cl 0.48674(10) 0.26174(15) 0.65167(16) 0.0942(6) Uani 1 1 d . . . Cl2 Cl 0.37624(12) 0.02950(15) 0.6997(2) 0.1193(10) Uani 1 1 d . . . Cl3 Cl 0.64829(12) 0.03687(17) 0.66199(19) 0.1280(11) Uani 1 1 d . . . Cl4 Cl 0.5055(5) 0.1785(4) 0.4635(2) 0.281(4) Uani 1 1 d . . . Cd1 Cd 0.50424(3) 0.12161(4) 0.61761(4) 0.07879(17) Uani 1 1 d . . . C1 C 0.2157(3) 0.5963(4) -0.0182(3) 0.0377(10) Uani 1 1 d . . . C2 C 0.2228(3) 0.6137(4) -0.1612(3) 0.0438(11) Uani 1 1 d . . . H2 H 0.1811 0.6570 -0.2033 0.053 Uiso 1 1 calc R . . C3 C 0.1816(3) 0.5195(4) -0.0990(3) 0.0424(11) Uani 1 1 d . . . H3 H 0.1204 0.5179 -0.1114 0.051 Uiso 1 1 calc R . . C4 C 0.3115(3) 0.4864(4) -0.1761(3) 0.0445(12) Uani 1 1 d . . . C5 C 0.1401(3) 0.4482(4) 0.0680(3) 0.0414(11) Uani 1 1 d . . . H5A H 0.0902 0.4242 0.0553 0.050 Uiso 1 1 calc R . . H5B H 0.1153 0.4795 0.1063 0.050 Uiso 1 1 calc R . . C6 C 0.2346(3) 0.3471(4) -0.0708(3) 0.0487(12) Uani 1 1 d . . . H6A H 0.2645 0.3175 -0.1090 0.058 Uiso 1 1 calc R . . H6B H 0.1709 0.3360 -0.0611 0.058 Uiso 1 1 calc R . . C7 C 0.2503(3) 0.3683(4) 0.1735(3) 0.0406(11) Uani 1 1 d . . . C8 C 0.2224(3) 0.2842(4) 0.0970(3) 0.0430(11) Uani 1 1 d . . . H8 H 0.1685 0.2496 0.1079 0.052 Uiso 1 1 calc R . . C9 C 0.2907(3) 0.2256(4) 0.1612(3) 0.0427(11) Uani 1 1 d . . . H9 H 0.2682 0.1643 0.2047 0.051 Uiso 1 1 calc R . . C10 C 0.3548(4) 0.2525(4) 0.0204(4) 0.0527(13) Uani 1 1 d . . . C11 C 0.3513(3) 0.2566(4) 0.2764(3) 0.0442(11) Uani 1 1 d . . . H11A H 0.3411 0.1897 0.3141 0.053 Uiso 1 1 calc R . . H11B H 0.3271 0.2940 0.3094 0.053 Uiso 1 1 calc R . . C12 C 0.4463(3) 0.1472(4) 0.1360(4) 0.0477(12) Uani 1 1 d . . . H12A H 0.4271 0.0901 0.1871 0.057 Uiso 1 1 calc R . . H12B H 0.4742 0.1272 0.0904 0.057 Uiso 1 1 calc R . . C13 C 0.4892(3) 0.3309(4) 0.2642(3) 0.0407(11) Uani 1 1 d . . . C14 C 0.5081(3) 0.1908(3) 0.2436(3) 0.0402(10) Uani 1 1 d . . . H14 H 0.4972 0.1275 0.2917 0.048 Uiso 1 1 calc R . . C15 C 0.6017(3) 0.2216(3) 0.2418(3) 0.0408(10) Uani 1 1 d . . . H15 H 0.6354 0.1727 0.2887 0.049 Uiso 1 1 calc R . . C16 C 0.5929(3) 0.2125(4) 0.1102(3) 0.0429(11) Uani 1 1 d . . . C17 C 0.3546(3) 0.6482(4) -0.2771(3) 0.0487(12) Uani 1 1 d . . . H17A H 0.3148 0.6992 -0.3147 0.058 Uiso 1 1 calc R . . H17B H 0.3860 0.6136 -0.3106 0.058 Uiso 1 1 calc R . . C18 C 0.7393(3) 0.2514(4) 0.1304(3) 0.0468(12) Uani 1 1 d . . . H18A H 0.7731 0.2107 0.1796 0.056 Uiso 1 1 calc R . . H18B H 0.7602 0.2319 0.0830 0.056 Uiso 1 1 calc R . . C19 C 0.1288(3) 0.7461(4) 0.2910(3) 0.0382(10) Uani 1 1 d . . . C20 C 0.0638(3) 0.8501(3) 0.3515(3) 0.0397(10) Uani 1 1 d . . . H20 H 0.0539 0.9199 0.3176 0.048 Uiso 1 1 calc R . . C21 C 0.1609(3) 0.8198(3) 0.3743(3) 0.0396(10) Uani 1 1 d . . . H21 H 0.1967 0.8753 0.3549 0.047 Uiso 1 1 calc R . . C22 C 0.0634(3) 0.7716(4) 0.5018(3) 0.0451(12) Uani 1 1 d . . . C23 C 0.2841(3) 0.7168(4) 0.3268(3) 0.0418(11) Uani 1 1 d . . . H23A H 0.3250 0.7590 0.3291 0.050 Uiso 1 1 calc R . . H23B H 0.3002 0.7113 0.2714 0.050 Uiso 1 1 calc R . . C24 C 0.2255(4) 0.7313(4) 0.5204(4) 0.0508(12) Uani 1 1 d . . . H24A H 0.2748 0.7726 0.4910 0.061 Uiso 1 1 calc R . . H24B H 0.2070 0.7344 0.5766 0.061 Uiso 1 1 calc R . . C25 C 0.2880(3) 0.5422(4) 0.3912(3) 0.0365(10) Uani 1 1 d . . . C26 C 0.3254(3) 0.6081(4) 0.4793(3) 0.0425(11) Uani 1 1 d . . . H26 H 0.3828 0.6358 0.4716 0.051 Uiso 1 1 calc R . . C27 C 0.3340(3) 0.4971(4) 0.5275(3) 0.0408(11) Uani 1 1 d . . . H27 H 0.3965 0.4724 0.5395 0.049 Uiso 1 1 calc R . . C28 C 0.2337(3) 0.5596(4) 0.6110(3) 0.0402(11) Uani 1 1 d . . . C29 C 0.3203(3) 0.3692(4) 0.4757(3) 0.0432(11) Uani 1 1 d . . . H29A H 0.3261 0.3707 0.4174 0.052 Uiso 1 1 calc R . . H29B H 0.3768 0.3407 0.5005 0.052 Uiso 1 1 calc R . . C30 C 0.2671(3) 0.3862(4) 0.6788(3) 0.0444(11) Uani 1 1 d . . . H30A H 0.2425 0.3948 0.7315 0.053 Uiso 1 1 calc R . . H30B H 0.3268 0.3530 0.6883 0.053 Uiso 1 1 calc R . . C31 C 0.1915(3) 0.2818(4) 0.4960(3) 0.0428(11) Uani 1 1 d . . . C32 C 0.2432(3) 0.2638(4) 0.6228(3) 0.0401(10) Uani 1 1 d . . . H32 H 0.2996 0.2266 0.6440 0.048 Uiso 1 1 calc R . . C33 C 0.1660(3) 0.1999(4) 0.6462(3) 0.0429(11) Uani 1 1 d . . . H33 H 0.1856 0.1320 0.6793 0.052 Uiso 1 1 calc R . . C34 C 0.1288(3) 0.3051(4) 0.7124(3) 0.0394(10) Uani 1 1 d . . . C35 C -0.0823(3) 0.8413(4) 0.4492(4) 0.0478(12) Uani 1 1 d . . . H35A H -0.0955 0.9080 0.4094 0.057 Uiso 1 1 calc R . . H35B H -0.0965 0.8361 0.5087 0.057 Uiso 1 1 calc R . . C36 C -0.0210(3) 0.8153(4) 0.2512(3) 0.0422(11) Uani 1 1 d . . . H36A H -0.0012 0.7969 0.2031 0.051 Uiso 1 1 calc R . . H36B H -0.0379 0.8840 0.2260 0.051 Uiso 1 1 calc R . . N1 N 0.2405(2) 0.6528(3) -0.1024(2) 0.0376(9) Uani 1 1 d . . . N2 N 0.1814(2) 0.5184(3) -0.0129(3) 0.0420(9) Uani 1 1 d . . . N3 N 0.3020(3) 0.5844(3) -0.2038(3) 0.0449(10) Uani 1 1 d . . . N4 N 0.2433(3) 0.4482(3) -0.1149(3) 0.0454(10) Uani 1 1 d . . . N5 N 0.2018(3) 0.3682(3) 0.1137(3) 0.0418(9) Uani 1 1 d . . . N6 N 0.3031(2) 0.2877(3) 0.2014(3) 0.0391(9) Uani 1 1 d . . . N7 N 0.2718(3) 0.2997(3) 0.0128(3) 0.0499(10) Uani 1 1 d . . . N8 N 0.3682(3) 0.2115(3) 0.1057(3) 0.0457(10) Uani 1 1 d . . . N9 N 0.4471(2) 0.2658(3) 0.2549(3) 0.0411(9) Uani 1 1 d . . . N10 N 0.5797(3) 0.3093(3) 0.2537(3) 0.0436(9) Uani 1 1 d . . . N11 N 0.5121(3) 0.1890(3) 0.1587(3) 0.0415(9) Uani 1 1 d . . . N12 N 0.6445(2) 0.2344(3) 0.1568(3) 0.0407(9) Uani 1 1 d . . . N13 N 0.0526(2) 0.7967(3) 0.3014(2) 0.0377(8) Uani 1 1 d . . . N14 N 0.1937(2) 0.7603(3) 0.3283(3) 0.0426(9) Uani 1 1 d . . . N15 N 0.0111(3) 0.8171(3) 0.4354(3) 0.0443(9) Uani 1 1 d . . . N16 N 0.1501(3) 0.7685(3) 0.4678(3) 0.0506(11) Uani 1 1 d . . . N17 N 0.2974(2) 0.6239(3) 0.3969(2) 0.0389(9) Uani 1 1 d . . . N18 N 0.3050(2) 0.4672(3) 0.4682(2) 0.0376(8) Uani 1 1 d . . . N19 N 0.2575(3) 0.6358(3) 0.5359(3) 0.0478(10) Uani 1 1 d . . . N20 N 0.2753(2) 0.4784(3) 0.6069(3) 0.0432(9) Uani 1 1 d . . . N21 N 0.2499(2) 0.3107(3) 0.5288(2) 0.0413(9) Uani 1 1 d . . . N22 N 0.1399(3) 0.2167(3) 0.5634(3) 0.0434(9) Uani 1 1 d . . . N23 N 0.2102(2) 0.3273(3) 0.6653(3) 0.0438(9) Uani 1 1 d . . . N24 N 0.0992(2) 0.2345(3) 0.6990(3) 0.0406(9) Uani 1 1 d . . . O1 O 0.2217(2) 0.6138(3) 0.0439(2) 0.0446(8) Uani 1 1 d . . . O2 O 0.2459(2) 0.4315(3) 0.1990(2) 0.0496(8) Uani 1 1 d . . . O3 O 0.4532(2) 0.3979(3) 0.2795(2) 0.0461(8) Uani 1 1 d . . . O4 O 0.3717(2) 0.4431(3) -0.2052(3) 0.0612(10) Uani 1 1 d . . . O5 O 0.4058(3) 0.2438(4) -0.0382(3) 0.0755(13) Uani 1 1 d . . . O6 O 0.6153(2) 0.2112(3) 0.0395(3) 0.0610(10) Uani 1 1 d . . . O7 O 0.1374(2) 0.6940(3) 0.2520(2) 0.0450(8) Uani 1 1 d . . . O8 O 0.2711(2) 0.5347(3) 0.3272(2) 0.0477(8) Uani 1 1 d . . . O9 O 0.1858(2) 0.3058(3) 0.4185(2) 0.0524(9) Uani 1 1 d . . . O10 O 0.0370(3) 0.7403(3) 0.5798(3) 0.0631(10) Uani 1 1 d . . . O11 O 0.1850(2) 0.5636(3) 0.6736(2) 0.0565(10) Uani 1 1 d . . . O12 O 0.0897(2) 0.3431(3) 0.7588(2) 0.0514(9) 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 Cl5 0.0562(8) 0.0748(11) 0.0840(11) -0.0273(9) -0.0250(7) -0.0040(7) O1W 0.0392(16) 0.084(3) 0.0404(19) -0.031(2) -0.0059(14) 0.0036(17) O2W 0.067(2) 0.053(2) 0.050(2) -0.0250(19) 0.0083(17) -0.0096(17) O3W 0.0474(18) 0.057(2) 0.045(2) -0.0154(18) 0.0055(15) -0.0091(16) O4W 0.0388(17) 0.067(3) 0.056(2) -0.022(2) -0.0012(15) -0.0001(16) Eu1 0.03550(13) 0.04699(17) 0.03138(14) -0.02075(12) -0.00324(9) -0.00029(9) Cl1 0.0502(8) 0.0952(14) 0.1376(18) -0.0463(14) -0.0164(9) -0.0093(8) Cl2 0.0629(10) 0.0642(12) 0.205(3) -0.0411(15) 0.0116(13) -0.0062(8) Cl3 0.0512(9) 0.0900(15) 0.162(2) 0.0176(15) -0.0019(11) -0.0020(9) Cl4 0.400(8) 0.265(6) 0.0661(18) -0.014(2) -0.025(3) 0.147(6) Cd1 0.0626(3) 0.0622(3) 0.0762(4) 0.0007(3) -0.0036(2) 0.0012(2) C1 0.0314(19) 0.049(3) 0.034(3) -0.019(2) -0.0055(18) -0.0001(18) C2 0.039(2) 0.061(3) 0.032(2) -0.019(2) -0.0083(19) -0.004(2) C3 0.035(2) 0.060(3) 0.042(3) -0.027(3) -0.0155(19) -0.001(2) C4 0.044(2) 0.069(4) 0.035(3) -0.031(3) -0.013(2) -0.007(2) C5 0.033(2) 0.048(3) 0.038(3) -0.016(2) 0.0019(18) -0.0019(19) C6 0.053(3) 0.061(4) 0.045(3) -0.031(3) -0.008(2) -0.011(2) C7 0.040(2) 0.040(3) 0.039(3) -0.016(2) 0.0059(19) -0.0090(19) C8 0.042(2) 0.044(3) 0.043(3) -0.015(2) -0.002(2) -0.014(2) C9 0.046(2) 0.045(3) 0.043(3) -0.023(2) 0.000(2) -0.012(2) C10 0.054(3) 0.062(4) 0.050(3) -0.032(3) -0.003(2) -0.005(2) C11 0.041(2) 0.056(3) 0.036(3) -0.021(2) 0.000(2) -0.004(2) C12 0.044(2) 0.053(3) 0.052(3) -0.028(3) -0.004(2) -0.003(2) C13 0.041(2) 0.056(3) 0.030(2) -0.020(2) -0.0100(18) -0.003(2) C14 0.045(2) 0.033(3) 0.033(2) -0.007(2) -0.0046(19) 0.0021(19) C15 0.042(2) 0.040(3) 0.036(2) -0.013(2) -0.0085(19) 0.0057(19) C16 0.048(2) 0.038(3) 0.037(3) -0.014(2) 0.003(2) -0.002(2) C17 0.047(3) 0.069(4) 0.033(3) -0.025(3) -0.005(2) -0.003(2) C18 0.039(2) 0.052(3) 0.046(3) -0.021(3) -0.004(2) 0.008(2) C19 0.034(2) 0.046(3) 0.032(2) -0.015(2) 0.0017(18) -0.0086(19) C20 0.048(2) 0.033(3) 0.041(3) -0.018(2) -0.006(2) -0.0052(19) C21 0.044(2) 0.031(3) 0.043(3) -0.013(2) -0.002(2) -0.0125(18) C22 0.056(3) 0.043(3) 0.047(3) -0.028(3) -0.004(2) -0.004(2) C23 0.035(2) 0.049(3) 0.039(3) -0.017(2) -0.0009(19) -0.0077(19) C24 0.061(3) 0.054(3) 0.049(3) -0.029(3) -0.015(2) -0.008(2) C25 0.034(2) 0.052(3) 0.029(2) -0.019(2) -0.0092(17) -0.0036(19) C26 0.034(2) 0.058(3) 0.040(3) -0.022(3) -0.0056(19) -0.011(2) C27 0.031(2) 0.056(3) 0.039(3) -0.021(2) -0.0046(18) -0.0096(19) C28 0.037(2) 0.051(3) 0.037(3) -0.019(2) -0.008(2) -0.010(2) C29 0.034(2) 0.060(3) 0.037(3) -0.024(2) -0.0019(19) 0.003(2) C30 0.043(2) 0.058(3) 0.033(3) -0.018(3) -0.0039(19) -0.010(2) C31 0.046(2) 0.041(3) 0.040(3) -0.018(2) -0.004(2) 0.006(2) C32 0.038(2) 0.047(3) 0.033(2) -0.017(2) -0.0044(18) 0.0039(19) C33 0.040(2) 0.042(3) 0.041(3) -0.015(2) -0.001(2) 0.005(2) C34 0.038(2) 0.052(3) 0.030(2) -0.018(2) -0.0062(18) -0.003(2) C35 0.050(3) 0.054(3) 0.055(3) -0.038(3) -0.002(2) -0.002(2) C36 0.041(2) 0.053(3) 0.032(2) -0.017(2) -0.0055(19) -0.004(2) N1 0.0364(17) 0.050(3) 0.027(2) -0.0165(19) -0.0051(15) -0.0033(16) N2 0.045(2) 0.052(3) 0.033(2) -0.021(2) -0.0058(17) -0.0056(18) N3 0.0412(19) 0.060(3) 0.038(2) -0.025(2) -0.0026(17) -0.0045(18) N4 0.047(2) 0.056(3) 0.042(2) -0.028(2) -0.0071(18) -0.0050(19) N5 0.048(2) 0.044(2) 0.037(2) -0.019(2) -0.0053(17) -0.0060(17) N6 0.0429(19) 0.039(2) 0.038(2) -0.0172(19) -0.0049(16) -0.0074(16) N7 0.050(2) 0.065(3) 0.045(2) -0.033(2) -0.0086(19) 0.001(2) N8 0.045(2) 0.048(3) 0.044(2) -0.022(2) -0.0004(18) -0.0016(18) N9 0.0395(19) 0.046(2) 0.040(2) -0.020(2) -0.0040(16) -0.0023(16) N10 0.043(2) 0.046(3) 0.042(2) -0.020(2) -0.0046(17) -0.0023(17) N11 0.045(2) 0.038(2) 0.038(2) -0.0141(19) -0.0014(17) -0.0036(17) N12 0.0386(18) 0.044(2) 0.036(2) -0.0145(19) 0.0003(16) -0.0050(16) N13 0.0398(18) 0.036(2) 0.038(2) -0.0172(18) -0.0048(16) -0.0003(15) N14 0.0398(19) 0.052(3) 0.044(2) -0.028(2) -0.0055(17) -0.0044(17) N15 0.051(2) 0.045(2) 0.044(2) -0.026(2) -0.0047(18) -0.0048(18) N16 0.054(2) 0.059(3) 0.048(3) -0.032(2) -0.008(2) -0.003(2) N17 0.0416(19) 0.048(2) 0.032(2) -0.0196(19) -0.0115(16) -0.0025(17) N18 0.0397(18) 0.043(2) 0.032(2) -0.0163(19) -0.0093(15) -0.0027(16) N19 0.048(2) 0.066(3) 0.044(3) -0.035(2) -0.0077(18) -0.008(2) N20 0.044(2) 0.057(3) 0.031(2) -0.020(2) -0.0018(16) -0.0080(18) N21 0.044(2) 0.052(3) 0.031(2) -0.020(2) -0.0051(16) -0.0054(17) N22 0.045(2) 0.055(3) 0.037(2) -0.025(2) -0.0007(17) -0.0067(18) N23 0.0368(18) 0.061(3) 0.039(2) -0.026(2) -0.0019(16) -0.0054(17) N24 0.0384(18) 0.048(2) 0.039(2) -0.022(2) -0.0006(16) -0.0032(16) O1 0.0462(17) 0.060(2) 0.0334(18) -0.0257(17) -0.0001(14) -0.0073(15) O2 0.0571(19) 0.049(2) 0.045(2) -0.0250(18) -0.0026(16) -0.0001(16) O3 0.0480(17) 0.049(2) 0.046(2) -0.0251(18) -0.0074(15) 0.0006(15) O4 0.053(2) 0.084(3) 0.064(3) -0.049(2) 0.0010(18) -0.0065(19) O5 0.070(2) 0.106(4) 0.053(2) -0.044(3) 0.005(2) 0.010(2) O6 0.059(2) 0.084(3) 0.054(2) -0.043(2) 0.0064(18) -0.0154(19) O7 0.0450(17) 0.056(2) 0.046(2) -0.0337(18) -0.0072(14) 0.0040(15) O8 0.0581(19) 0.049(2) 0.0384(19) -0.0206(17) -0.0096(15) 0.0028(16) O9 0.058(2) 0.063(2) 0.037(2) -0.0201(18) -0.0070(16) -0.0070(17) O10 0.070(2) 0.075(3) 0.044(2) -0.027(2) 0.0001(18) -0.003(2) O11 0.056(2) 0.076(3) 0.043(2) -0.032(2) -0.0025(16) -0.0006(18) O12 0.0484(18) 0.067(2) 0.052(2) -0.038(2) 0.0057(16) -0.0113(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1W Eu1 2.412(3) . ? O2W Eu1 2.399(4) . ? O3W Eu1 2.430(3) . ? O4W Eu1 2.429(3) . ? Eu1 O7 2.373(3) . ? Eu1 O1 2.382(3) . ? Eu1 O8 2.385(3) . ? Eu1 O2 2.385(3) . ? Cl1 Cd1 2.470(2) . ? Cl2 Cd1 2.443(2) . ? Cl3 Cd1 2.4419(19) . ? Cl4 Cd1 2.395(3) . ? C1 O1 1.228(5) . ? C1 N2 1.348(6) . ? C1 N1 1.350(6) . ? C2 N3 1.433(6) . ? C2 N1 1.459(6) . ? C2 C3 1.541(8) . ? C2 H2 0.9900 . ? C3 N4 1.445(6) . ? C3 N2 1.469(6) . ? C3 H3 0.9900 . ? C4 O4 1.235(6) . ? C4 N4 1.347(6) . ? C4 N3 1.385(7) . ? C5 N2 1.455(6) . ? C5 N5 1.454(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.440(7) . ? C6 N7 1.463(7) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.232(6) . ? C7 N6 1.333(6) . ? C7 N5 1.353(6) . ? C8 N5 1.444(6) . ? C8 N7 1.454(6) . ? C8 C9 1.533(7) . ? C8 H8 0.9900 . ? C9 N8 1.449(6) . ? C9 N6 1.456(6) . ? C9 H9 0.9900 . ? C10 O5 1.215(6) . ? C10 N7 1.364(7) . ? C10 N8 1.356(7) . ? C11 N6 1.443(6) . ? C11 N9 1.452(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.447(6) . ? C12 N8 1.448(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.225(6) . ? C13 N9 1.348(6) . ? C13 N10 1.371(6) . ? C14 N9 1.454(6) . ? C14 N11 1.461(6) . ? C14 C15 1.552(7) . ? C14 H14 0.9900 . ? C15 N12 1.441(6) . ? C15 N10 1.457(6) . ? C15 H15 0.9900 . ? C16 O6 1.216(6) . ? C16 N11 1.366(6) . ? C16 N12 1.369(6) . ? C17 N3 1.424(7) . ? C17 N10 1.459(6) 2_665 ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N1 1.420(7) 2_665 ? C18 N12 1.463(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O7 1.241(5) . ? C19 N13 1.342(6) . ? C19 N14 1.343(6) . ? C20 N15 1.445(6) . ? C20 N13 1.473(6) . ? C20 C21 1.541(7) . ? C20 H20 0.9900 . ? C21 N16 1.443(7) . ? C21 N14 1.456(6) . ? C21 H21 0.9900 . ? C22 O10 1.228(6) . ? C22 N16 1.356(6) . ? C22 N15 1.362(7) . ? C23 N14 1.447(6) . ? C23 N17 1.440(7) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N19 1.425(7) . ? C24 N16 1.465(7) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O8 1.221(5) . ? C25 N17 1.349(6) . ? C25 N18 1.366(6) . ? C26 N17 1.447(6) . ? C26 N19 1.456(6) . ? C26 C27 1.561(8) . ? C26 H26 0.9900 . ? C27 N18 1.433(6) . ? C27 N20 1.443(6) . ? C27 H27 0.9900 . ? C28 O11 1.224(6) . ? C28 N19 1.360(7) . ? C28 N20 1.363(6) . ? C29 N21 1.430(6) . ? C29 N18 1.467(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N20 1.439(7) . ? C30 N23 1.449(6) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O9 1.228(6) . ? C31 N21 1.337(6) . ? C31 N22 1.378(7) . ? C32 N21 1.448(6) . ? C32 N23 1.464(6) . ? C32 C33 1.534(7) . ? C32 H32 0.9900 . ? C33 N22 1.439(6) . ? C33 N24 1.458(5) . ? C33 H33 0.9900 . ? C34 O12 1.226(5) . ? C34 N24 1.362(6) . ? C34 N23 1.363(6) . ? C35 N15 1.425(6) . ? C35 N22 1.439(6) 2_566 ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N13 1.437(6) . ? C36 N24 1.449(6) 2_566 ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? N1 C18 1.420(7) 2_665 ? N10 C17 1.459(6) 2_665 ? N22 C35 1.439(6) 2_566 ? N24 C36 1.449(6) 2_566 ? 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 Eu1 O1 126.17(12) . . ? O7 Eu1 O8 76.24(11) . . ? O1 Eu1 O8 152.09(11) . . ? O7 Eu1 O2 151.47(12) . . ? O1 Eu1 O2 76.85(12) . . ? O8 Eu1 O2 88.51(12) . . ? O7 Eu1 O2W 70.61(12) . . ? O1 Eu1 O2W 73.80(12) . . ? O8 Eu1 O2W 103.56(13) . . ? O2 Eu1 O2W 137.29(11) . . ? O7 Eu1 O1W 72.77(12) . . ? O1 Eu1 O1W 70.60(11) . . ? O8 Eu1 O1W 136.92(11) . . ? O2 Eu1 O1W 105.14(13) . . ? O2W Eu1 O1W 93.60(14) . . ? O7 Eu1 O4W 123.46(12) . . ? O1 Eu1 O4W 80.48(12) . . ? O8 Eu1 O4W 72.42(12) . . ? O2 Eu1 O4W 72.42(13) . . ? O2W Eu1 O4W 72.67(13) . . ? O1W Eu1 O4W 150.58(12) . . ? O7 Eu1 O3W 80.22(12) . . ? O1 Eu1 O3W 122.71(12) . . ? O8 Eu1 O3W 73.25(13) . . ? O2 Eu1 O3W 72.28(12) . . ? O2W Eu1 O3W 150.41(12) . . ? O1W Eu1 O3W 72.61(13) . . ? O4W Eu1 O3W 130.61(13) . . ? Cl4 Cd1 Cl3 109.76(16) . . ? Cl4 Cd1 Cl2 113.0(2) . . ? Cl3 Cd1 Cl2 113.45(8) . . ? Cl4 Cd1 Cl1 107.75(16) . . ? Cl3 Cd1 Cl1 107.15(9) . . ? Cl2 Cd1 Cl1 105.35(8) . . ? O1 C1 N2 125.1(4) . . ? O1 C1 N1 125.3(4) . . ? N2 C1 N1 109.5(4) . . ? N3 C2 N1 113.9(4) . . ? N3 C2 C3 104.0(4) . . ? N1 C2 C3 103.1(4) . . ? N3 C2 H2 111.8 . . ? N1 C2 H2 111.8 . . ? C3 C2 H2 111.8 . . ? N4 C3 N2 114.6(4) . . ? N4 C3 C2 103.2(4) . . ? N2 C3 C2 103.1(4) . . ? N4 C3 H3 111.7 . . ? N2 C3 H3 111.7 . . ? C2 C3 H3 111.7 . . ? O4 C4 N4 126.6(5) . . ? O4 C4 N3 124.8(5) . . ? N4 C4 N3 108.6(4) . . ? N2 C5 N5 113.4(3) . . ? N2 C5 H5A 108.9 . . ? N5 C5 H5A 108.9 . . ? N2 C5 H5B 108.9 . . ? N5 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N4 C6 N7 114.8(4) . . ? N4 C6 H6A 108.6 . . ? N7 C6 H6A 108.6 . . ? N4 C6 H6B 108.6 . . ? N7 C6 H6B 108.6 . . ? H6A C6 H6B 107.5 . . ? O2 C7 N6 125.5(5) . . ? O2 C7 N5 125.9(5) . . ? N6 C7 N5 108.6(4) . . ? N5 C8 N7 115.2(4) . . ? N5 C8 C9 102.5(4) . . ? N7 C8 C9 103.3(4) . . ? N5 C8 H8 111.7 . . ? N7 C8 H8 111.7 . . ? C9 C8 H8 111.7 . . ? N8 C9 N6 114.2(4) . . ? N8 C9 C8 103.4(4) . . ? N6 C9 C8 103.3(4) . . ? N8 C9 H9 111.8 . . ? N6 C9 H9 111.8 . . ? C8 C9 H9 111.8 . . ? O5 C10 N7 126.0(5) . . ? O5 C10 N8 125.7(5) . . ? N7 C10 N8 108.2(4) . . ? N6 C11 N9 113.7(4) . . ? N6 C11 H11A 108.8 . . ? N9 C11 H11A 108.8 . . ? N6 C11 H11B 108.8 . . ? N9 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? N11 C12 N8 113.2(4) . . ? N11 C12 H12A 108.9 . . ? N8 C12 H12A 108.9 . . ? N11 C12 H12B 108.9 . . ? N8 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N9 126.1(4) . . ? O3 C13 N10 125.6(4) . . ? N9 C13 N10 108.3(4) . . ? N9 C14 N11 114.7(4) . . ? N9 C14 C15 103.3(4) . . ? N11 C14 C15 103.1(4) . . ? N9 C14 H14 111.7 . . ? N11 C14 H14 111.7 . . ? C15 C14 H14 111.7 . . ? N12 C15 N10 114.8(4) . . ? N12 C15 C14 103.1(4) . . ? N10 C15 C14 102.6(3) . . ? N12 C15 H15 111.9 . . ? N10 C15 H15 111.9 . . ? C14 C15 H15 111.9 . . ? O6 C16 N11 125.8(5) . . ? O6 C16 N12 126.4(4) . . ? N11 C16 N12 107.8(4) . . ? N3 C17 N10 113.4(4) . 2_665 ? N3 C17 H17A 108.9 . . ? N10 C17 H17A 108.9 2_665 . ? N3 C17 H17B 108.9 . . ? N10 C17 H17B 108.9 2_665 . ? H17A C17 H17B 107.7 . . ? N1 C18 N12 115.0(4) 2_665 . ? N1 C18 H18A 108.5 2_665 . ? N12 C18 H18A 108.5 . . ? N1 C18 H18B 108.5 2_665 . ? N12 C18 H18B 108.5 . . ? H18A C18 H18B 107.5 . . ? O7 C19 N13 124.3(4) . . ? O7 C19 N14 125.3(4) . . ? N13 C19 N14 110.5(4) . . ? N15 C20 N13 112.9(4) . . ? N15 C20 C21 103.5(4) . . ? N13 C20 C21 103.2(3) . . ? N15 C20 H20 112.2 . . ? N13 C20 H20 112.2 . . ? C21 C20 H20 112.2 . . ? N16 C21 N14 114.3(4) . . ? N16 C21 C20 103.3(4) . . ? N14 C21 C20 102.9(4) . . ? N16 C21 H21 111.9 . . ? N14 C21 H21 111.9 . . ? C20 C21 H21 111.9 . . ? O10 C22 N16 125.2(5) . . ? O10 C22 N15 125.9(5) . . ? N16 C22 N15 108.9(4) . . ? N14 C23 N17 114.4(4) . . ? N14 C23 H23A 108.7 . . ? N17 C23 H23A 108.7 . . ? N14 C23 H23B 108.7 . . ? N17 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? N19 C24 N16 114.2(4) . . ? N19 C24 H24A 108.7 . . ? N16 C24 H24A 108.7 . . ? N19 C24 H24B 108.7 . . ? N16 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? O8 C25 N17 126.5(5) . . ? O8 C25 N18 124.7(4) . . ? N17 C25 N18 108.8(4) . . ? N17 C26 N19 114.9(4) . . ? N17 C26 C27 102.3(4) . . ? N19 C26 C27 103.2(4) . . ? N17 C26 H26 111.9 . . ? N19 C26 H26 111.9 . . ? C27 C26 H26 111.9 . . ? N18 C27 N20 115.3(4) . . ? N18 C27 C26 103.5(4) . . ? N20 C27 C26 103.0(4) . . ? N18 C27 H27 111.5 . . ? N20 C27 H27 111.5 . . ? C26 C27 H27 111.5 . . ? O11 C28 N19 125.4(5) . . ? O11 C28 N20 125.4(5) . . ? N19 C28 N20 109.2(4) . . ? N21 C29 N18 113.0(3) . . ? N21 C29 H29A 109.0 . . ? N18 C29 H29A 109.0 . . ? N21 C29 H29B 109.0 . . ? N18 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? N20 C30 N23 113.1(4) . . ? N20 C30 H30A 109.0 . . ? N23 C30 H30A 109.0 . . ? N20 C30 H30B 109.0 . . ? N23 C30 H30B 109.0 . . ? H30A C30 H30B 107.8 . . ? O9 C31 N21 126.4(5) . . ? O9 C31 N22 124.5(5) . . ? N21 C31 N22 109.1(4) . . ? N21 C32 N23 114.0(4) . . ? N21 C32 C33 103.0(4) . . ? N23 C32 C33 103.1(3) . . ? N21 C32 H32 112.0 . . ? N23 C32 H32 112.0 . . ? C33 C32 H32 112.0 . . ? N22 C33 N24 114.5(4) . . ? N22 C33 C32 104.1(4) . . ? N24 C33 C32 103.8(4) . . ? N22 C33 H33 111.3 . . ? N24 C33 H33 111.3 . . ? C32 C33 H33 111.3 . . ? O12 C34 N24 126.4(4) . . ? O12 C34 N23 124.9(4) . . ? N24 C34 N23 108.6(4) . . ? N15 C35 N22 114.9(4) . 2_566 ? N15 C35 H35A 108.5 . . ? N22 C35 H35A 108.5 2_566 . ? N15 C35 H35B 108.5 . . ? N22 C35 H35B 108.5 2_566 . ? H35A C35 H35B 107.5 . . ? N13 C36 N24 113.9(4) . 2_566 ? N13 C36 H36A 108.8 . . ? N24 C36 H36A 108.8 2_566 . ? N13 C36 H36B 108.8 . . ? N24 C36 H36B 108.8 2_566 . ? H36A C36 H36B 107.7 . . ? C1 N1 C18 122.4(4) . 2_665 ? C1 N1 C2 112.4(4) . . ? C18 N1 C2 123.6(4) 2_665 . ? C1 N2 C5 123.1(4) . . ? C1 N2 C3 111.9(4) . . ? C5 N2 C3 124.7(4) . . ? C4 N3 C17 123.3(4) . . ? C4 N3 C2 111.6(4) . . ? C17 N3 C2 124.1(4) . . ? C4 N4 C3 112.6(4) . . ? C4 N4 C6 122.7(4) . . ? C3 N4 C6 124.7(4) . . ? C7 N5 C8 113.0(4) . . ? C7 N5 C5 122.3(4) . . ? C8 N5 C5 124.6(4) . . ? C7 N6 C11 123.0(4) . . ? C7 N6 C9 112.5(4) . . ? C11 N6 C9 123.2(4) . . ? C10 N7 C8 112.2(4) . . ? C10 N7 C6 121.8(4) . . ? C8 N7 C6 125.3(4) . . ? C10 N8 C9 112.7(4) . . ? C10 N8 C12 121.3(4) . . ? C9 N8 C12 125.1(4) . . ? C13 N9 C14 113.0(4) . . ? C13 N9 C11 123.3(4) . . ? C14 N9 C11 121.8(4) . . ? C13 N10 C17 123.2(4) . 2_665 ? C13 N10 C15 112.6(4) . . ? C17 N10 C15 121.8(4) 2_665 . ? C16 N11 C12 122.7(4) . . ? C16 N11 C14 112.6(4) . . ? C12 N11 C14 123.4(4) . . ? C16 N12 C15 113.4(4) . . ? C16 N12 C18 123.3(4) . . ? C15 N12 C18 122.4(4) . . ? C19 N13 C36 123.1(4) . . ? C19 N13 C20 111.1(4) . . ? C36 N13 C20 123.9(4) . . ? C19 N14 C23 123.6(4) . . ? C19 N14 C21 112.1(4) . . ? C23 N14 C21 124.2(4) . . ? C22 N15 C35 122.9(4) . . ? C22 N15 C20 111.9(4) . . ? C35 N15 C20 124.6(4) . . ? C22 N16 C21 112.2(4) . . ? C22 N16 C24 123.8(4) . . ? C21 N16 C24 123.3(4) . . ? C25 N17 C26 112.9(4) . . ? C25 N17 C23 123.2(4) . . ? C26 N17 C23 123.8(4) . . ? C25 N18 C27 112.2(4) . . ? C25 N18 C29 121.4(4) . . ? C27 N18 C29 123.5(4) . . ? C28 N19 C24 122.7(4) . . ? C28 N19 C26 111.8(4) . . ? C24 N19 C26 125.2(4) . . ? C28 N20 C30 122.2(4) . . ? C28 N20 C27 112.6(4) . . ? C30 N20 C27 124.9(4) . . ? C31 N21 C29 122.7(4) . . ? C31 N21 C32 112.7(4) . . ? C29 N21 C32 123.9(4) . . ? C31 N22 C33 111.1(4) . . ? C31 N22 C35 123.1(4) . 2_566 ? C33 N22 C35 124.5(4) . 2_566 ? C34 N23 C30 121.7(4) . . ? C34 N23 C32 112.2(4) . . ? C30 N23 C32 123.5(4) . . ? C34 N24 C36 122.9(4) . 2_566 ? C34 N24 C33 112.0(4) . . ? C36 N24 C33 123.5(4) 2_566 . ? C1 O1 Eu1 157.4(3) . . ? C7 O2 Eu1 155.9(4) . . ? C19 O7 Eu1 157.9(3) . . ? C25 O8 Eu1 154.9(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.321 _refine_diff_density_min -1.105 _refine_diff_density_rms 0.100 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.004 0.000 -0.002 1104 483 ' ' 2 0.000 0.500 0.500 96 13 ' ' 3 0.500 0.500 0.000 95 15 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 902607' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p208 #TrackingRef 'submit-208.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H102 Cd Cl5 Gd N24 O45' _chemical_formula_weight 2038.32 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 '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 15.136(3) _cell_length_b 15.719(3) _cell_length_c 17.189(3) _cell_angle_alpha 64.678(6) _cell_angle_beta 80.911(6) _cell_angle_gamma 81.763(6) _cell_volume 3637.0(10) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.861 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2086 _exptl_absorpt_coefficient_mu 1.500 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7055 _exptl_absorpt_correction_T_max 0.7740 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40460 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12691 _reflns_number_gt 11129 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0618P)^2^+0.1628P] 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 12691 _refine_ls_number_parameters 759 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.1009 _refine_ls_wR_factor_gt 0.0980 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 Cl5 Cl 0.51207(8) 0.19725(10) -0.04448(8) 0.0725(3) Uani 1 1 d . . . Cl4' Cl 0.0425(6) -0.2950(10) -0.5341(6) 0.126(4) Uani 0.37(3) 1 d P . . O1W O 0.43618(16) -0.1329(2) -0.14293(15) 0.0478(6) Uani 1 1 d . . . O2W O 0.23853(18) -0.23790(19) -0.11164(16) 0.0498(6) Uani 1 1 d . . . O3W O 0.39666(16) 0.02015(19) -0.30341(16) 0.0479(6) Uani 1 1 d . . . O4W O 0.12945(16) -0.0649(2) -0.16502(16) 0.0509(6) Uani 1 1 d . . . Gd1 Gd 0.291285(10) -0.084063(11) -0.194112(9) 0.03206(7) Uani 1 1 d . . . Cl1 Cl -0.12173(10) -0.46764(11) -0.30579(15) 0.1167(7) Uani 1 1 d . . . Cl2 Cl -0.01139(9) -0.23998(12) -0.34765(12) 0.0989(5) Uani 1 1 d . . . Cl3 Cl 0.14942(10) -0.46509(13) -0.33154(14) 0.1449(10) Uani 1 1 d . . . Cl4 Cl -0.0045(16) -0.3334(10) -0.5374(3) 0.195(8) Uani 0.63(3) 1 d P . . Cd1 Cd 0.00774(3) -0.37872(3) -0.38309(3) 0.08244(14) Uani 1 1 d . . . C1 C 0.2117(2) -0.0370(3) -0.39178(19) 0.0348(7) Uani 1 1 d . . . C2 C 0.1642(2) 0.0048(3) -0.5265(2) 0.0388(8) Uani 1 1 d . . . H2 H 0.1014 0.0294 -0.5380 0.047 Uiso 1 1 calc R . . C3 C 0.1731(2) -0.1032(3) -0.4791(2) 0.0385(8) Uani 1 1 d . . . H3 H 0.1156 -0.1305 -0.4712 0.046 Uiso 1 1 calc R . . C4 C 0.2651(2) -0.0566(3) -0.6104(2) 0.0397(8) Uani 1 1 d . . . C5 C 0.2158(2) -0.2113(2) -0.3266(2) 0.0365(7) Uani 1 1 d . . . H5A H 0.2005 -0.2057 -0.2713 0.044 Uiso 1 1 calc R . . H5B H 0.1748 -0.2531 -0.3285 0.044 Uiso 1 1 calc R . . C6 C 0.2730(3) -0.2279(3) -0.5202(2) 0.0478(9) Uani 1 1 d . . . H6A H 0.2919 -0.2307 -0.5763 0.057 Uiso 1 1 calc R . . H6B H 0.2232 -0.2681 -0.4918 0.057 Uiso 1 1 calc R . . C7 C 0.3717(2) -0.2402(2) -0.29228(19) 0.0329(7) Uani 1 1 d . . . C8 C 0.3377(2) -0.3145(2) -0.3747(2) 0.0376(7) Uani 1 1 d . . . H8 H 0.3015 -0.3692 -0.3544 0.045 Uiso 1 1 calc R . . C9 C 0.4350(2) -0.3454(2) -0.3527(2) 0.0376(7) Uani 1 1 d . . . H9 H 0.4444 -0.4145 -0.3189 0.045 Uiso 1 1 calc R . . C10 C 0.4350(2) -0.2699(3) -0.5028(2) 0.0418(8) Uani 1 1 d . . . C11 C 0.5214(2) -0.3136(2) -0.25216(19) 0.0360(7) Uani 1 1 d . . . H11A H 0.5017 -0.2950 -0.2041 0.043 Uiso 1 1 calc R . . H11B H 0.5378 -0.3819 -0.2274 0.043 Uiso 1 1 calc R . . C12 C 0.5811(2) -0.3414(3) -0.4495(2) 0.0440(8) Uani 1 1 d . . . H12A H 0.5955 -0.3385 -0.5081 0.053 Uiso 1 1 calc R . . H12B H 0.5939 -0.4071 -0.4087 0.053 Uiso 1 1 calc R . . C13 C 0.6296(2) -0.1939(3) -0.2889(2) 0.0402(8) Uani 1 1 d . . . C14 C 0.6650(2) -0.2999(3) -0.3540(2) 0.0370(7) Uani 1 1 d . . . H14 H 0.6848 -0.3673 -0.3216 0.044 Uiso 1 1 calc R . . C15 C 0.7436(2) -0.2362(2) -0.3786(2) 0.0363(7) Uani 1 1 d . . . H15 H 0.8000 -0.2738 -0.3573 0.044 Uiso 1 1 calc R . . C16 C 0.6898(2) -0.2200(2) -0.5051(2) 0.0374(8) Uani 1 1 d . . . C17 C 0.7684(2) -0.1158(3) -0.3230(2) 0.0416(8) Uani 1 1 d . . . H17A H 0.8282 -0.1495 -0.3142 0.050 Uiso 1 1 calc R . . H17B H 0.7445 -0.1076 -0.2700 0.050 Uiso 1 1 calc R . . C18 C 0.8207(2) -0.1338(3) -0.5247(2) 0.0382(8) Uani 1 1 d . . . H18A H 0.8270 -0.1332 -0.5826 0.046 Uiso 1 1 calc R . . H18B H 0.8774 -0.1618 -0.4999 0.046 Uiso 1 1 calc R . . C19 C 0.2478(2) 0.1326(2) -0.1734(2) 0.0357(7) Uani 1 1 d . . . C20 C 0.2066(2) 0.2742(2) -0.1600(2) 0.0375(7) Uani 1 1 d . . . H20 H 0.2291 0.3347 -0.2033 0.045 Uiso 1 1 calc R . . C21 C 0.2749(2) 0.2156(2) -0.0961(2) 0.0365(7) Uani 1 1 d . . . H21 H 0.3285 0.2501 -0.1066 0.044 Uiso 1 1 calc R . . C22 C 0.1438(2) 0.2487(3) -0.0194(2) 0.0429(8) Uani 1 1 d . . . C23 C 0.3592(2) 0.0557(3) -0.0692(2) 0.0377(8) Uani 1 1 d . . . H23A H 0.4076 0.0808 -0.0558 0.045 Uiso 1 1 calc R . . H23B H 0.3860 0.0250 -0.1075 0.045 Uiso 1 1 calc R . . C24 C 0.2642(3) 0.1550(3) 0.0698(2) 0.0473(9) Uani 1 1 d . . . H24A H 0.2335 0.1842 0.1081 0.057 Uiso 1 1 calc R . . H24B H 0.3277 0.1671 0.0596 0.057 Uiso 1 1 calc R . . C25 C 0.2847(2) -0.0916(3) 0.0159(2) 0.0357(7) Uani 1 1 d . . . C26 C 0.3201(2) -0.0164(3) 0.0961(2) 0.0374(8) Uani 1 1 d . . . H26 H 0.3816 -0.0152 0.1082 0.045 Uiso 1 1 calc R . . C27 C 0.2784(2) -0.1102(3) 0.1571(2) 0.0369(8) Uani 1 1 d . . . H27 H 0.3208 -0.1538 0.1980 0.044 Uiso 1 1 calc R . . C28 C 0.1891(2) 0.0141(3) 0.1763(2) 0.0405(8) Uani 1 1 d . . . C29 C 0.2419(2) -0.2455(2) 0.1257(2) 0.0389(8) Uani 1 1 d . . . H29A H 0.2619 -0.2636 0.0774 0.047 Uiso 1 1 calc R . . H29B H 0.2771 -0.2862 0.1736 0.047 Uiso 1 1 calc R . . C30 C 0.1474(2) -0.1462(3) 0.2748(2) 0.0450(9) Uani 1 1 d . . . H30A H 0.1150 -0.1123 0.3085 0.054 Uiso 1 1 calc R . . H30B H 0.1880 -0.1963 0.3119 0.054 Uiso 1 1 calc R . . C31 C 0.0970(2) -0.2837(2) 0.1074(2) 0.0372(7) Uani 1 1 d . . . C32 C 0.1053(2) -0.2763(2) 0.23899(19) 0.0363(7) Uani 1 1 d . . . H32 H 0.1398 -0.3247 0.2850 0.044 Uiso 1 1 calc R . . C33 C 0.0129(2) -0.3077(2) 0.2403(2) 0.0374(8) Uani 1 1 d . . . H33 H 0.0031 -0.3710 0.2873 0.045 Uiso 1 1 calc R . . C34 C -0.0069(2) -0.1698(3) 0.26339(19) 0.0369(8) Uani 1 1 d . . . C35 C -0.0492(2) -0.3502(3) 0.1334(2) 0.0422(8) Uani 1 1 d . . . H35A H -0.0204 -0.3697 0.0876 0.051 Uiso 1 1 calc R . . H35B H -0.0670 -0.4072 0.1840 0.051 Uiso 1 1 calc R . . C36 C -0.1443(2) -0.2425(3) 0.2756(2) 0.0381(8) Uani 1 1 d . . . H36A H -0.1686 -0.2041 0.3077 0.046 Uiso 1 1 calc R . . H36B H -0.1546 -0.3084 0.3138 0.046 Uiso 1 1 calc R . . N1 N 0.19464(18) 0.0364(2) -0.46683(16) 0.0358(6) Uani 1 1 d . . . N2 N 0.20174(19) -0.1182(2) -0.39689(17) 0.0390(7) Uani 1 1 d . . . N3 N 0.22295(19) 0.0234(2) -0.60609(17) 0.0410(7) Uani 1 1 d . . . N4 N 0.2410(2) -0.1317(2) -0.53469(18) 0.0421(7) Uani 1 1 d . . . N5 N 0.30561(19) -0.2538(2) -0.32953(17) 0.0372(6) Uani 1 1 d . . . N6 N 0.44674(19) -0.2933(2) -0.30333(17) 0.0361(6) Uani 1 1 d . . . N7 N 0.3474(2) -0.2657(2) -0.46753(19) 0.0455(7) Uani 1 1 d . . . N8 N 0.48701(19) -0.3148(2) -0.43653(18) 0.0419(7) Uani 1 1 d . . . N9 N 0.60012(18) -0.2655(2) -0.30145(17) 0.0375(6) Uani 1 1 d . . . N10 N 0.71145(19) -0.1730(2) -0.33584(17) 0.0395(7) Uani 1 1 d . . . N11 N 0.63898(19) -0.2824(2) -0.43802(17) 0.0400(7) Uani 1 1 d . . . N12 N 0.75062(19) -0.1921(2) -0.47189(16) 0.0377(6) Uani 1 1 d . . . N13 N 0.19269(19) 0.2125(2) -0.19991(17) 0.0359(6) Uani 1 1 d . . . N14 N 0.29755(19) 0.1315(2) -0.11358(17) 0.0377(6) Uani 1 1 d . . . N15 N 0.12842(19) 0.2890(2) -0.10411(18) 0.0407(7) Uani 1 1 d . . . N16 N 0.2262(2) 0.1991(2) -0.01175(18) 0.0425(7) Uani 1 1 d . . . N17 N 0.31847(18) -0.0152(2) 0.01116(16) 0.0363(6) Uani 1 1 d . . . N18 N 0.26014(18) -0.1485(2) 0.09900(16) 0.0361(6) Uani 1 1 d . . . N19 N 0.2573(2) 0.0536(2) 0.11317(18) 0.0414(7) Uani 1 1 d . . . N20 N 0.19958(19) -0.0821(2) 0.20197(17) 0.0398(7) Uani 1 1 d . . . N21 N 0.14839(19) -0.2620(2) 0.15308(17) 0.0399(7) Uani 1 1 d . . . N22 N 0.01590(18) -0.3075(2) 0.15627(17) 0.0386(6) Uani 1 1 d . . . N23 N 0.08323(18) -0.1890(2) 0.25130(17) 0.0383(6) Uani 1 1 d . . . N24 N -0.04907(18) -0.2343(2) 0.25388(17) 0.0369(6) Uani 1 1 d . . . O1 O 0.23099(16) -0.02899(18) -0.32778(14) 0.0417(6) Uani 1 1 d . . . O2 O 0.36412(15) -0.18942(18) -0.25381(14) 0.0400(5) Uani 1 1 d . . . O3 O 0.59090(18) -0.1560(2) -0.24268(16) 0.0514(7) Uani 1 1 d . . . O4 O 0.31299(18) -0.0611(2) -0.67317(16) 0.0541(7) Uani 1 1 d . . . O5 O 0.4613(2) -0.2414(2) -0.57920(17) 0.0609(8) Uani 1 1 d . . . O6 O 0.68501(18) -0.19577(19) -0.58179(15) 0.0483(6) Uani 1 1 d . . . O7 O 0.25302(17) 0.07066(17) -0.20018(15) 0.0427(6) Uani 1 1 d . . . O8 O 0.27844(16) -0.10910(18) -0.04746(14) 0.0410(6) Uani 1 1 d . . . O9 O 0.11799(17) -0.2833(2) 0.03534(16) 0.0504(6) Uani 1 1 d . . . O10 O 0.0923(2) 0.2577(2) 0.03961(18) 0.0630(8) Uani 1 1 d . . . O11 O 0.12998(18) 0.0577(2) 0.20583(17) 0.0525(7) Uani 1 1 d . . . O12 O -0.04447(17) -0.10261(18) 0.27961(15) 0.0433(6) 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 Cl5 0.0545(6) 0.0889(9) 0.0786(7) -0.0335(6) -0.0262(5) -0.0029(6) Cl4' 0.107(6) 0.162(7) 0.058(3) 0.004(3) 0.002(2) -0.033(4) O1W 0.0362(13) 0.0700(18) 0.0402(13) -0.0280(12) -0.0092(10) 0.0085(12) O2W 0.0550(16) 0.0496(16) 0.0456(13) -0.0233(12) 0.0091(11) -0.0113(13) O3W 0.0382(14) 0.0547(16) 0.0465(13) -0.0183(12) 0.0029(11) -0.0075(12) O4W 0.0356(13) 0.0577(17) 0.0511(14) -0.0168(13) 0.0003(11) -0.0031(12) Gd1 0.03116(10) 0.03956(11) 0.02846(9) -0.01798(7) -0.00344(6) 0.00067(7) Cl1 0.0599(8) 0.0616(9) 0.2035(19) -0.0395(10) 0.0057(10) -0.0007(7) Cl2 0.0476(7) 0.0999(11) 0.1453(13) -0.0435(10) -0.0176(7) -0.0100(7) Cl3 0.0486(8) 0.1021(12) 0.1740(17) 0.0400(12) 0.0019(9) 0.0009(7) Cl4 0.266(16) 0.185(8) 0.070(2) -0.007(3) -0.036(4) 0.045(9) Cd1 0.0616(2) 0.0663(3) 0.0772(2) 0.00553(19) -0.00246(18) 0.00404(18) C1 0.0256(16) 0.048(2) 0.0321(16) -0.0183(15) -0.0059(12) 0.0008(14) C2 0.0323(17) 0.053(2) 0.0333(16) -0.0185(15) -0.0077(13) -0.0033(15) C3 0.0329(18) 0.050(2) 0.0372(17) -0.0192(15) -0.0078(13) -0.0087(15) C4 0.0339(18) 0.053(2) 0.0422(18) -0.0268(17) -0.0114(15) -0.0035(16) C5 0.0307(17) 0.046(2) 0.0322(16) -0.0146(15) -0.0021(13) -0.0087(15) C6 0.050(2) 0.058(2) 0.051(2) -0.0332(19) -0.0174(17) -0.0027(18) C7 0.0348(17) 0.0314(18) 0.0280(14) -0.0085(13) 0.0008(12) -0.0062(14) C8 0.045(2) 0.0276(18) 0.0417(17) -0.0149(14) -0.0026(14) -0.0070(15) C9 0.0436(19) 0.0336(19) 0.0372(17) -0.0170(14) -0.0006(14) -0.0045(15) C10 0.048(2) 0.042(2) 0.045(2) -0.0286(17) -0.0057(16) -0.0012(17) C11 0.0369(18) 0.0370(19) 0.0296(15) -0.0108(14) -0.0065(13) 0.0039(14) C12 0.050(2) 0.045(2) 0.0477(19) -0.0310(17) -0.0004(16) -0.0027(17) C13 0.0314(17) 0.058(2) 0.0312(16) -0.0184(16) -0.0030(13) -0.0034(16) C14 0.0393(18) 0.0364(19) 0.0336(16) -0.0143(14) -0.0047(13) 0.0026(15) C15 0.0355(18) 0.0378(19) 0.0323(16) -0.0132(14) -0.0059(13) 0.0048(14) C16 0.0400(19) 0.0350(19) 0.0377(18) -0.0192(15) -0.0031(14) 0.0078(15) C17 0.043(2) 0.055(2) 0.0283(15) -0.0163(15) -0.0099(14) -0.0076(17) C18 0.0313(17) 0.050(2) 0.0358(16) -0.0222(15) 0.0002(13) -0.0011(15) C19 0.0334(17) 0.039(2) 0.0339(16) -0.0149(14) 0.0020(13) -0.0068(15) C20 0.0408(19) 0.0332(19) 0.0418(17) -0.0187(15) -0.0019(14) -0.0063(15) C21 0.0349(18) 0.039(2) 0.0361(16) -0.0157(14) 0.0009(13) -0.0103(15) C22 0.045(2) 0.048(2) 0.0435(19) -0.0265(17) 0.0001(16) -0.0081(17) C23 0.0292(17) 0.047(2) 0.0359(16) -0.0172(15) 0.0005(13) -0.0032(15) C24 0.049(2) 0.059(3) 0.047(2) -0.0316(18) -0.0112(16) -0.0101(18) C25 0.0270(16) 0.045(2) 0.0369(17) -0.0203(15) -0.0039(13) 0.0034(14) C26 0.0309(17) 0.050(2) 0.0372(17) -0.0217(15) -0.0096(13) -0.0025(15) C27 0.0297(17) 0.051(2) 0.0334(16) -0.0195(15) -0.0129(13) 0.0037(15) C28 0.0326(18) 0.064(3) 0.0350(16) -0.0293(17) -0.0080(14) -0.0030(17) C29 0.0343(18) 0.039(2) 0.0409(17) -0.0156(15) -0.0056(14) 0.0047(15) C30 0.044(2) 0.068(3) 0.0283(16) -0.0238(17) -0.0073(14) -0.0045(18) C31 0.0421(19) 0.0325(18) 0.0321(16) -0.0100(14) -0.0051(14) 0.0020(15) C32 0.0372(18) 0.0336(19) 0.0299(15) -0.0069(13) -0.0055(13) 0.0040(14) C33 0.0386(18) 0.0359(19) 0.0316(16) -0.0091(14) -0.0039(13) -0.0004(15) C34 0.0393(19) 0.042(2) 0.0247(14) -0.0090(14) -0.0066(13) -0.0022(16) C35 0.043(2) 0.035(2) 0.055(2) -0.0261(16) -0.0014(16) -0.0018(16) C36 0.0338(18) 0.047(2) 0.0327(16) -0.0163(14) 0.0027(13) -0.0076(15) N1 0.0352(15) 0.0389(16) 0.0340(13) -0.0147(12) -0.0093(11) -0.0003(12) N2 0.0383(16) 0.0468(18) 0.0364(14) -0.0188(13) -0.0111(12) -0.0048(13) N3 0.0407(16) 0.0511(19) 0.0316(14) -0.0174(13) -0.0006(12) -0.0084(14) N4 0.0496(18) 0.0458(18) 0.0374(15) -0.0228(13) -0.0064(13) -0.0036(14) N5 0.0378(16) 0.0400(17) 0.0385(14) -0.0202(12) -0.0023(12) -0.0072(13) N6 0.0380(16) 0.0350(16) 0.0389(14) -0.0195(12) -0.0038(12) -0.0013(12) N7 0.0453(18) 0.057(2) 0.0429(16) -0.0294(15) -0.0084(13) 0.0016(15) N8 0.0403(16) 0.0498(19) 0.0416(15) -0.0256(14) -0.0007(12) -0.0052(14) N9 0.0318(15) 0.0444(17) 0.0400(14) -0.0230(13) -0.0011(11) 0.0008(13) N10 0.0345(15) 0.0518(19) 0.0369(14) -0.0235(13) -0.0013(12) -0.0043(13) N11 0.0398(16) 0.0480(18) 0.0357(14) -0.0210(13) -0.0035(12) -0.0040(13) N12 0.0389(16) 0.0420(17) 0.0312(13) -0.0141(12) -0.0035(11) -0.0040(13) N13 0.0399(16) 0.0369(16) 0.0347(13) -0.0184(12) -0.0044(11) -0.0032(13) N14 0.0389(16) 0.0384(16) 0.0397(14) -0.0198(13) -0.0054(12) -0.0027(13) N15 0.0392(16) 0.0432(18) 0.0469(16) -0.0270(14) -0.0009(13) -0.0030(13) N16 0.0423(17) 0.0512(19) 0.0396(15) -0.0248(14) -0.0044(12) -0.0020(14) N17 0.0367(15) 0.0439(17) 0.0293(13) -0.0156(12) -0.0043(11) -0.0044(13) N18 0.0346(15) 0.0428(17) 0.0299(13) -0.0149(12) -0.0054(11) 0.0012(12) N19 0.0423(17) 0.0484(19) 0.0418(15) -0.0262(14) -0.0021(13) -0.0073(14) N20 0.0380(16) 0.051(2) 0.0362(14) -0.0234(13) -0.0031(12) -0.0059(13) N21 0.0368(16) 0.0448(18) 0.0364(14) -0.0173(13) 0.0008(12) -0.0020(13) N22 0.0342(15) 0.0452(18) 0.0381(14) -0.0202(13) -0.0010(12) -0.0028(13) N23 0.0345(15) 0.0467(18) 0.0358(14) -0.0195(13) -0.0038(11) -0.0022(13) N24 0.0337(15) 0.0391(17) 0.0391(14) -0.0179(12) -0.0049(11) -0.0001(12) O1 0.0440(14) 0.0524(16) 0.0353(12) -0.0238(11) -0.0123(10) 0.0025(11) O2 0.0385(13) 0.0503(15) 0.0420(12) -0.0307(12) -0.0065(10) 0.0036(11) O3 0.0496(15) 0.0659(18) 0.0522(14) -0.0403(14) 0.0077(12) -0.0090(13) O4 0.0509(16) 0.076(2) 0.0420(13) -0.0328(14) -0.0019(12) -0.0010(14) O5 0.0639(18) 0.078(2) 0.0415(15) -0.0295(14) -0.0018(13) 0.0021(16) O6 0.0555(16) 0.0574(17) 0.0359(13) -0.0225(12) -0.0070(11) -0.0045(13) O7 0.0501(15) 0.0431(15) 0.0415(12) -0.0247(11) -0.0059(11) -0.0003(12) O8 0.0418(13) 0.0560(16) 0.0315(11) -0.0254(11) -0.0042(10) 0.0005(11) O9 0.0484(15) 0.0625(18) 0.0450(14) -0.0276(13) 0.0068(11) -0.0148(13) O10 0.0588(18) 0.084(2) 0.0483(15) -0.0356(15) 0.0008(13) 0.0065(15) O11 0.0485(16) 0.0626(18) 0.0584(15) -0.0391(14) 0.0028(12) -0.0059(13) O12 0.0446(14) 0.0465(15) 0.0447(13) -0.0254(12) -0.0089(11) 0.0040(12) _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 Cl4' Cl4 1.019(14) . ? Cl4' Cd1 2.364(7) . ? O1W Gd1 2.392(2) . ? O2W Gd1 2.400(3) . ? O3W Gd1 2.434(2) . ? O4W Gd1 2.423(2) . ? Gd1 O8 2.359(2) . ? Gd1 O2 2.363(2) . ? Gd1 O1 2.366(2) . ? Gd1 O7 2.379(2) . ? Cl1 Cd1 2.4358(16) . ? Cl2 Cd1 2.4720(19) . ? Cl3 Cd1 2.4421(16) . ? Cl4 Cd1 2.465(7) . ? C1 O1 1.242(4) . ? C1 N1 1.345(4) . ? C1 N2 1.346(4) . ? C2 N3 1.449(4) . ? C2 N1 1.469(4) . ? C2 C3 1.534(5) . ? C2 H2 0.9900 . ? C3 N4 1.446(4) . ? C3 N2 1.456(4) . ? C3 H3 0.9900 . ? C4 O4 1.224(4) . ? C4 N3 1.353(5) . ? C4 N4 1.371(5) . ? C5 N5 1.429(4) . ? C5 N2 1.459(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.445(5) . ? C6 N7 1.454(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.220(4) . ? C7 N6 1.349(4) . ? C7 N5 1.355(4) . ? C8 N7 1.438(4) . ? C8 N5 1.459(4) . ? C8 C9 1.536(5) . ? C8 H8 0.9900 . ? C9 N8 1.443(4) . ? C9 N6 1.452(4) . ? C9 H9 0.9900 . ? C10 O5 1.210(4) . ? C10 N8 1.361(5) . ? C10 N7 1.373(5) . ? C11 N9 1.449(4) . ? C11 N6 1.457(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.435(5) . ? C12 N11 1.453(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.220(4) . ? C13 N10 1.367(4) . ? C13 N9 1.375(5) . ? C14 N9 1.434(4) . ? C14 N11 1.458(4) . ? C14 C15 1.556(5) . ? C14 H14 0.9900 . ? C15 N12 1.443(4) . ? C15 N10 1.461(4) . ? C15 H15 0.9900 . ? C16 O6 1.217(4) . ? C16 N11 1.360(4) . ? C16 N12 1.364(4) . ? C17 N10 1.433(4) . ? C17 N3 1.451(5) 2_654 ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.433(4) . ? C18 N1 1.462(5) 2_654 ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O7 1.231(4) . ? C19 N13 1.346(5) . ? C19 N14 1.360(4) . ? C20 N15 1.459(4) . ? C20 N13 1.460(4) . ? C20 C21 1.531(5) . ? C20 H20 0.9900 . ? C21 N16 1.453(4) . ? C21 N14 1.460(4) . ? C21 H21 0.9900 . ? C22 O10 1.224(4) . ? C22 N15 1.361(5) . ? C22 N16 1.366(5) . ? C23 N14 1.415(4) . ? C23 N17 1.463(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N16 1.445(5) . ? C24 N19 1.453(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O8 1.252(4) . ? C25 N17 1.339(4) . ? C25 N18 1.346(4) . ? C26 N19 1.446(5) . ? C26 N17 1.456(4) . ? C26 C27 1.551(5) . ? C26 H26 0.9900 . ? C27 N20 1.437(4) . ? C27 N18 1.444(4) . ? C27 H27 0.9900 . ? C28 O11 1.227(4) . ? C28 N19 1.371(4) . ? C28 N20 1.376(5) . ? C29 N21 1.443(4) . ? C29 N18 1.447(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N20 1.428(5) . ? C30 N23 1.451(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O9 1.226(4) . ? C31 N21 1.356(4) . ? C31 N22 1.374(4) . ? C32 N21 1.453(4) . ? C32 N23 1.461(4) . ? C32 C33 1.542(5) . ? C32 H32 0.9900 . ? C33 N22 1.436(4) . ? C33 N24 1.455(4) . ? C33 H33 0.9900 . ? C34 O12 1.244(4) . ? C34 N24 1.350(4) . ? C34 N23 1.357(4) . ? C35 N15 1.436(5) 2 ? C35 N22 1.455(4) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N24 1.441(4) . ? C36 N13 1.459(4) 2 ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? N1 C18 1.462(5) 2_654 ? N3 C17 1.451(5) 2_654 ? N13 C36 1.459(4) 2 ? N15 C35 1.436(5) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl4 Cl4' Cd1 83.4(5) . . ? O8 Gd1 O2 126.39(8) . . ? O8 Gd1 O1 151.42(8) . . ? O2 Gd1 O1 76.90(8) . . ? O8 Gd1 O7 76.92(8) . . ? O2 Gd1 O7 151.82(8) . . ? O1 Gd1 O7 87.15(8) . . ? O8 Gd1 O1W 70.74(8) . . ? O2 Gd1 O1W 72.97(8) . . ? O1 Gd1 O1W 137.29(8) . . ? O7 Gd1 O1W 105.99(9) . . ? O8 Gd1 O2W 73.74(9) . . ? O2 Gd1 O2W 70.31(8) . . ? O1 Gd1 O2W 104.46(9) . . ? O7 Gd1 O2W 137.05(8) . . ? O1W Gd1 O2W 93.15(10) . . ? O8 Gd1 O4W 79.95(8) . . ? O2 Gd1 O4W 122.62(9) . . ? O1 Gd1 O4W 72.64(9) . . ? O7 Gd1 O4W 72.61(9) . . ? O1W Gd1 O4W 149.95(8) . . ? O2W Gd1 O4W 71.93(9) . . ? O8 Gd1 O3W 122.09(9) . . ? O2 Gd1 O3W 81.20(9) . . ? O1 Gd1 O3W 73.36(9) . . ? O7 Gd1 O3W 71.95(9) . . ? O1W Gd1 O3W 72.70(9) . . ? O2W Gd1 O3W 150.97(9) . . ? O4W Gd1 O3W 131.35(9) . . ? Cl4' Cl4 Cd1 72.4(5) . . ? Cl4' Cd1 Cl1 128.4(4) . . ? Cl4' Cd1 Cl3 104.6(2) . . ? Cl1 Cd1 Cl3 112.76(6) . . ? Cl4' Cd1 Cl4 24.2(3) . . ? Cl1 Cd1 Cl4 104.9(7) . . ? Cl3 Cd1 Cl4 115.3(4) . . ? Cl4' Cd1 Cl2 96.5(5) . . ? Cl1 Cd1 Cl2 105.41(6) . . ? Cl3 Cd1 Cl2 106.13(8) . . ? Cl4 Cd1 Cl2 112.0(3) . . ? O1 C1 N1 124.1(3) . . ? O1 C1 N2 126.4(3) . . ? N1 C1 N2 109.4(3) . . ? N3 C2 N1 114.5(3) . . ? N3 C2 C3 103.5(3) . . ? N1 C2 C3 103.8(3) . . ? N3 C2 H2 111.5 . . ? N1 C2 H2 111.5 . . ? C3 C2 H2 111.5 . . ? N4 C3 N2 114.5(3) . . ? N4 C3 C2 103.4(3) . . ? N2 C3 C2 102.3(3) . . ? N4 C3 H3 112.0 . . ? N2 C3 H3 112.0 . . ? C2 C3 H3 112.0 . . ? O4 C4 N3 125.4(3) . . ? O4 C4 N4 126.1(4) . . ? N3 C4 N4 108.4(3) . . ? N5 C5 N2 113.9(3) . . ? N5 C5 H5A 108.8 . . ? N2 C5 H5A 108.8 . . ? N5 C5 H5B 108.8 . . ? N2 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N4 C6 N7 113.9(3) . . ? N4 C6 H6A 108.8 . . ? N7 C6 H6A 108.8 . . ? N4 C6 H6B 108.8 . . ? N7 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N6 125.6(3) . . ? O2 C7 N5 125.6(3) . . ? N6 C7 N5 108.8(3) . . ? N7 C8 N5 114.5(3) . . ? N7 C8 C9 103.4(3) . . ? N5 C8 C9 103.1(3) . . ? N7 C8 H8 111.8 . . ? N5 C8 H8 111.8 . . ? C9 C8 H8 111.8 . . ? N8 C9 N6 113.9(3) . . ? N8 C9 C8 103.5(3) . . ? N6 C9 C8 103.2(3) . . ? N8 C9 H9 111.8 . . ? N6 C9 H9 111.8 . . ? C8 C9 H9 111.8 . . ? O5 C10 N8 125.9(4) . . ? O5 C10 N7 126.2(4) . . ? N8 C10 N7 107.8(3) . . ? N9 C11 N6 113.5(3) . . ? N9 C11 H11A 108.9 . . ? N6 C11 H11A 108.9 . . ? N9 C11 H11B 108.9 . . ? N6 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? N8 C12 N11 113.9(3) . . ? N8 C12 H12A 108.8 . . ? N11 C12 H12A 108.8 . . ? N8 C12 H12B 108.8 . . ? N11 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N10 125.0(3) . . ? O3 C13 N9 126.5(3) . . ? N10 C13 N9 108.5(3) . . ? N9 C14 N11 115.5(3) . . ? N9 C14 C15 103.8(3) . . ? N11 C14 C15 102.9(2) . . ? N9 C14 H14 111.4 . . ? N11 C14 H14 111.4 . . ? C15 C14 H14 111.4 . . ? N12 C15 N10 115.3(3) . . ? N12 C15 C14 103.1(3) . . ? N10 C15 C14 103.0(3) . . ? N12 C15 H15 111.6 . . ? N10 C15 H15 111.6 . . ? C14 C15 H15 111.6 . . ? O6 C16 N11 126.4(3) . . ? O6 C16 N12 125.2(3) . . ? N11 C16 N12 108.3(3) . . ? N10 C17 N3 114.2(3) . 2_654 ? N10 C17 H17A 108.7 . . ? N3 C17 H17A 108.7 2_654 . ? N10 C17 H17B 108.7 . . ? N3 C17 H17B 108.7 2_654 . ? H17A C17 H17B 107.6 . . ? N12 C18 N1 113.9(3) . 2_654 ? N12 C18 H18A 108.8 . . ? N1 C18 H18A 108.8 2_654 . ? N12 C18 H18B 108.8 . . ? N1 C18 H18B 108.8 2_654 . ? H18A C18 H18B 107.7 . . ? O7 C19 N13 125.0(3) . . ? O7 C19 N14 125.4(3) . . ? N13 C19 N14 109.6(3) . . ? N15 C20 N13 113.4(3) . . ? N15 C20 C21 103.2(3) . . ? N13 C20 C21 103.6(3) . . ? N15 C20 H20 112.0 . . ? N13 C20 H20 112.0 . . ? C21 C20 H20 112.0 . . ? N16 C21 N14 114.8(3) . . ? N16 C21 C20 104.1(3) . . ? N14 C21 C20 103.2(3) . . ? N16 C21 H21 111.4 . . ? N14 C21 H21 111.4 . . ? C20 C21 H21 111.4 . . ? O10 C22 N15 124.9(4) . . ? O10 C22 N16 126.0(3) . . ? N15 C22 N16 109.0(3) . . ? N14 C23 N17 113.5(3) . . ? N14 C23 H23A 108.9 . . ? N17 C23 H23A 108.9 . . ? N14 C23 H23B 108.9 . . ? N17 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? N16 C24 N19 113.5(3) . . ? N16 C24 H24A 108.9 . . ? N19 C24 H24A 108.9 . . ? N16 C24 H24B 108.9 . . ? N19 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? O8 C25 N17 125.1(3) . . ? O8 C25 N18 124.6(3) . . ? N17 C25 N18 110.3(3) . . ? N19 C26 N17 114.0(3) . . ? N19 C26 C27 102.7(3) . . ? N17 C26 C27 102.0(3) . . ? N19 C26 H26 112.4 . . ? N17 C26 H26 112.4 . . ? C27 C26 H26 112.4 . . ? N20 C27 N18 114.3(3) . . ? N20 C27 C26 104.6(3) . . ? N18 C27 C26 104.0(2) . . ? N20 C27 H27 111.2 . . ? N18 C27 H27 111.2 . . ? C26 C27 H27 111.2 . . ? O11 C28 N19 125.4(4) . . ? O11 C28 N20 126.0(3) . . ? N19 C28 N20 108.6(3) . . ? N21 C29 N18 113.7(3) . . ? N21 C29 H29A 108.8 . . ? N18 C29 H29A 108.8 . . ? N21 C29 H29B 108.8 . . ? N18 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? N20 C30 N23 113.6(3) . . ? N20 C30 H30A 108.9 . . ? N23 C30 H30A 108.9 . . ? N20 C30 H30B 108.9 . . ? N23 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? O9 C31 N21 126.9(3) . . ? O9 C31 N22 125.1(3) . . ? N21 C31 N22 108.0(3) . . ? N21 C32 N23 113.6(3) . . ? N21 C32 C33 103.0(3) . . ? N23 C32 C33 103.8(3) . . ? N21 C32 H32 111.9 . . ? N23 C32 H32 111.9 . . ? C33 C32 H32 111.9 . . ? N22 C33 N24 114.5(3) . . ? N22 C33 C32 103.7(2) . . ? N24 C33 C32 102.6(3) . . ? N22 C33 H33 111.8 . . ? N24 C33 H33 111.8 . . ? C32 C33 H33 111.8 . . ? O12 C34 N24 125.5(3) . . ? O12 C34 N23 125.2(3) . . ? N24 C34 N23 109.2(3) . . ? N15 C35 N22 113.9(3) 2 . ? N15 C35 H35A 108.8 2 . ? N22 C35 H35A 108.8 . . ? N15 C35 H35B 108.8 2 . ? N22 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? N24 C36 N13 113.1(3) . 2 ? N24 C36 H36A 109.0 . . ? N13 C36 H36A 109.0 2 . ? N24 C36 H36B 109.0 . . ? N13 C36 H36B 109.0 2 . ? H36A C36 H36B 107.8 . . ? C1 N1 C18 122.5(3) . 2_654 ? C1 N1 C2 111.2(3) . . ? C18 N1 C2 123.3(3) 2_654 . ? C1 N2 C3 113.0(3) . . ? C1 N2 C5 123.5(3) . . ? C3 N2 C5 123.4(3) . . ? C4 N3 C2 112.4(3) . . ? C4 N3 C17 122.7(3) . 2_654 ? C2 N3 C17 124.8(3) . 2_654 ? C4 N4 C3 111.9(3) . . ? C4 N4 C6 121.9(3) . . ? C3 N4 C6 125.7(3) . . ? C7 N5 C5 123.6(3) . . ? C7 N5 C8 112.1(3) . . ? C5 N5 C8 124.3(3) . . ? C7 N6 C9 112.6(3) . . ? C7 N6 C11 121.7(3) . . ? C9 N6 C11 123.9(3) . . ? C10 N7 C8 112.5(3) . . ? C10 N7 C6 122.5(3) . . ? C8 N7 C6 124.4(3) . . ? C10 N8 C12 123.0(3) . . ? C10 N8 C9 112.6(3) . . ? C12 N8 C9 123.8(3) . . ? C13 N9 C14 112.6(3) . . ? C13 N9 C11 122.9(3) . . ? C14 N9 C11 123.3(3) . . ? C13 N10 C17 122.1(3) . . ? C13 N10 C15 112.0(3) . . ? C17 N10 C15 123.5(3) . . ? C16 N11 C12 122.9(3) . . ? C16 N11 C14 112.6(3) . . ? C12 N11 C14 123.0(3) . . ? C16 N12 C18 123.0(3) . . ? C16 N12 C15 113.0(3) . . ? C18 N12 C15 123.5(3) . . ? C19 N13 C36 122.1(3) . 2 ? C19 N13 C20 111.7(3) . . ? C36 N13 C20 124.3(3) 2 . ? C19 N14 C23 124.4(3) . . ? C19 N14 C21 111.6(3) . . ? C23 N14 C21 123.9(3) . . ? C22 N15 C35 122.1(3) . 2 ? C22 N15 C20 111.9(3) . . ? C35 N15 C20 125.4(3) 2 . ? C22 N16 C24 121.7(3) . . ? C22 N16 C21 111.2(3) . . ? C24 N16 C21 125.7(3) . . ? C25 N17 C26 112.4(3) . . ? C25 N17 C23 123.6(3) . . ? C26 N17 C23 123.6(3) . . ? C25 N18 C27 111.3(3) . . ? C25 N18 C29 122.4(3) . . ? C27 N18 C29 124.2(3) . . ? C28 N19 C26 112.6(3) . . ? C28 N19 C24 122.6(3) . . ? C26 N19 C24 124.8(3) . . ? C28 N20 C30 123.2(3) . . ? C28 N20 C27 111.6(3) . . ? C30 N20 C27 124.3(3) . . ? C31 N21 C29 122.6(3) . . ? C31 N21 C32 112.7(3) . . ? C29 N21 C32 123.6(3) . . ? C31 N22 C33 112.5(3) . . ? C31 N22 C35 122.3(3) . . ? C33 N22 C35 123.5(3) . . ? C34 N23 C30 123.0(3) . . ? C34 N23 C32 111.4(3) . . ? C30 N23 C32 123.0(3) . . ? C34 N24 C36 122.9(3) . . ? C34 N24 C33 112.8(3) . . ? C36 N24 C33 122.7(3) . . ? C1 O1 Gd1 154.3(2) . . ? C7 O2 Gd1 157.2(2) . . ? C19 O7 Gd1 154.9(2) . . ? C25 O8 Gd1 157.3(2) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.863 _refine_diff_density_min -0.900 _refine_diff_density_rms 0.083 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 96 28 ' ' 2 -0.113 0.500 0.066 1135 526 ' ' 3 0.500 0.000 0.500 98 27 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 902608' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a #TrackingRef 'submit-209.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H92 Cd Cl5 N24 O40 Tb' _chemical_formula_weight 1949.91 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 '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 15.101(6) _cell_length_b 15.634(6) _cell_length_c 17.210(7) _cell_angle_alpha 64.686(13) _cell_angle_beta 80.871(14) _cell_angle_gamma 81.896(13) _cell_volume 3614(2) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.792 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1988 _exptl_absorpt_coefficient_mu 1.561 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7351 _exptl_absorpt_correction_T_max 0.8111 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37799 _diffrn_reflns_av_R_equivalents 0.0849 _diffrn_reflns_av_sigmaI/netI 0.0912 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12577 _reflns_number_gt 8943 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.1159P)^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 12577 _refine_ls_number_parameters 748 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0874 _refine_ls_R_factor_gt 0.0688 _refine_ls_wR_factor_ref 0.1824 _refine_ls_wR_factor_gt 0.1703 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.946 _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 Cl5 Cl 0.51200(16) 0.69907(19) 0.95462(16) 0.0797(7) Uani 1 1 d . . . O1W O 0.4360(3) 0.3662(4) 0.8575(3) 0.0505(12) Uani 1 1 d . . . O2W O 0.2392(3) 0.2599(3) 0.8904(3) 0.0520(13) Uani 1 1 d . . . O3W O 0.3960(3) 0.5169(4) 0.6970(3) 0.0523(13) Uani 1 1 d . . . O4W O 0.1284(3) 0.4347(4) 0.8355(3) 0.0554(13) Uani 1 1 d . . . Tb1 Tb 0.29133(2) 0.41374(2) 0.807142(18) 0.03811(13) Uani 1 1 d . . . Cl1 Cl -0.01223(18) 0.2586(2) 0.6528(2) 0.1024(9) Uani 1 1 d . . . Cl2 Cl -0.1241(2) 0.0293(2) 0.6979(3) 0.1248(13) Uani 1 1 d . . . Cl3 Cl 0.14924(19) 0.0343(2) 0.6631(3) 0.1387(16) Uani 1 1 d . . . Cl4 Cl 0.0086(6) 0.1788(5) 0.4630(3) 0.287(5) Uani 1 1 d . . . Cd1 Cd 0.00544(5) 0.11968(5) 0.61643(5) 0.0835(3) Uani 1 1 d . . . C1 C 0.2496(5) 0.6313(5) 0.8264(4) 0.0402(15) Uani 1 1 d . . . C2 C 0.2090(5) 0.7747(5) 0.8400(4) 0.0421(16) Uani 1 1 d . . . H2 H 0.2313 0.8356 0.7965 0.051 Uiso 1 1 calc R . . C3 C 0.2787(5) 0.7166(5) 0.9028(4) 0.0403(15) Uani 1 1 d . . . H3 H 0.3327 0.7510 0.8923 0.048 Uiso 1 1 calc R . . C4 C 0.1447(5) 0.7491(5) 0.9810(4) 0.0480(18) Uani 1 1 d . . . C5 C 0.3596(4) 0.5546(5) 0.9311(4) 0.0408(15) Uani 1 1 d . . . H5A H 0.4090 0.5798 0.9434 0.049 Uiso 1 1 calc R . . H5B H 0.3854 0.5228 0.8934 0.049 Uiso 1 1 calc R . . C6 C 0.2663(6) 0.6547(5) 1.0698(4) 0.0522(19) Uani 1 1 d . . . H6A H 0.3304 0.6653 1.0590 0.063 Uiso 1 1 calc R . . H6B H 0.2373 0.6852 1.1077 0.063 Uiso 1 1 calc R . . C7 C 0.2861(4) 0.4060(5) 1.0174(4) 0.0408(16) Uani 1 1 d . . . C8 C 0.3202(5) 0.4833(5) 1.0964(4) 0.0446(17) Uani 1 1 d . . . H8 H 0.3819 0.4848 1.1083 0.054 Uiso 1 1 calc R . . C9 C 0.2786(5) 0.3882(5) 1.1592(4) 0.0415(16) Uani 1 1 d . . . H9 H 0.3206 0.3445 1.2006 0.050 Uiso 1 1 calc R . . C10 C 0.1890(5) 0.5159(6) 1.1755(4) 0.0460(18) Uani 1 1 d . . . C11 C 0.2394(5) 0.2516(5) 1.1287(4) 0.0430(16) Uani 1 1 d . . . H11A H 0.2604 0.2314 1.0818 0.052 Uiso 1 1 calc R . . H11B H 0.2730 0.2113 1.1778 0.052 Uiso 1 1 calc R . . C12 C 0.1454(5) 0.3562(6) 1.2741(4) 0.0491(18) Uani 1 1 d . . . H12A H 0.1124 0.3921 1.3060 0.059 Uiso 1 1 calc R . . H12B H 0.1855 0.3068 1.3127 0.059 Uiso 1 1 calc R . . C13 C 0.0953(5) 0.2152(5) 1.1086(4) 0.0427(16) Uani 1 1 d . . . C14 C 0.1047(5) 0.2228(5) 1.2401(4) 0.0438(16) Uani 1 1 d . . . H14 H 0.1397 0.1743 1.2857 0.053 Uiso 1 1 calc R . . C15 C 0.0123(5) 0.1921(5) 1.2419(4) 0.0406(15) Uani 1 1 d . . . H15 H 0.0021 0.1290 1.2896 0.049 Uiso 1 1 calc R . . C16 C -0.0076(5) 0.3316(5) 1.2635(4) 0.0383(15) Uani 1 1 d . . . C17 C -0.0509(5) 0.1482(5) 1.1351(5) 0.0479(17) Uani 1 1 d . . . H17A H -0.0218 0.1283 1.0898 0.058 Uiso 1 1 calc R . . H17B H -0.0694 0.0911 1.1857 0.058 Uiso 1 1 calc R . . C18 C -0.1475(4) 0.2579(5) 1.2758(4) 0.0442(17) Uani 1 1 d . . . H18A H -0.1578 0.1915 1.3135 0.053 Uiso 1 1 calc R . . H18B H -0.1716 0.2961 1.3083 0.053 Uiso 1 1 calc R . . C19 C 0.2119(4) 0.4601(5) 0.6100(4) 0.0355(14) Uani 1 1 d . . . C20 C 0.1646(4) 0.5037(5) 0.4747(4) 0.0392(15) Uani 1 1 d . . . H20 H 0.1017 0.5281 0.4632 0.047 Uiso 1 1 calc R . . C21 C 0.1730(5) 0.3960(6) 0.5216(4) 0.0475(18) Uani 1 1 d . . . H21 H 0.1150 0.3691 0.5295 0.057 Uiso 1 1 calc R . . C22 C 0.2640(5) 0.4429(5) 0.3901(4) 0.0417(16) Uani 1 1 d . . . C23 C 0.2167(5) 0.2867(5) 0.6746(4) 0.0426(16) Uani 1 1 d . . . H23A H 0.2015 0.2939 0.7291 0.051 Uiso 1 1 calc R . . H23B H 0.1752 0.2442 0.6739 0.051 Uiso 1 1 calc R . . C24 C 0.2720(6) 0.2690(5) 0.4813(5) 0.0512(19) Uani 1 1 d . . . H24A H 0.2898 0.2645 0.4258 0.061 Uiso 1 1 calc R . . H24B H 0.2219 0.2293 0.5113 0.061 Uiso 1 1 calc R . . C25 C 0.3717(4) 0.2570(5) 0.7087(4) 0.0361(15) Uani 1 1 d . . . C26 C 0.3383(5) 0.1830(5) 0.6264(4) 0.0414(15) Uani 1 1 d . . . H26 H 0.3017 0.1282 0.6467 0.050 Uiso 1 1 calc R . . C27 C 0.4350(5) 0.1507(5) 0.6492(4) 0.0433(16) Uani 1 1 d . . . H27 H 0.4441 0.0812 0.6830 0.052 Uiso 1 1 calc R . . C28 C 0.4343(5) 0.2283(5) 0.4972(4) 0.0448(17) Uani 1 1 d . . . C29 C 0.5224(4) 0.1838(5) 0.7485(4) 0.0405(15) Uani 1 1 d . . . H29A H 0.5029 0.2011 0.7974 0.049 Uiso 1 1 calc R . . H29B H 0.5394 0.1154 0.7721 0.049 Uiso 1 1 calc R . . C30 C 0.5809(5) 0.1583(5) 0.5505(4) 0.0457(17) Uani 1 1 d . . . H30A H 0.5951 0.1619 0.4916 0.055 Uiso 1 1 calc R . . H30B H 0.5940 0.0921 0.5906 0.055 Uiso 1 1 calc R . . C31 C 0.6295(5) 0.3066(5) 0.7109(4) 0.0396(15) Uani 1 1 d . . . C32 C 0.6662(5) 0.1980(5) 0.6457(4) 0.0441(17) Uani 1 1 d . . . H32 H 0.6862 0.1303 0.6778 0.053 Uiso 1 1 calc R . . C33 C 0.7442(4) 0.2632(5) 0.6218(4) 0.0398(15) Uani 1 1 d . . . H33 H 0.8013 0.2264 0.6420 0.048 Uiso 1 1 calc R . . C34 C 0.6902(5) 0.2793(5) 0.4945(4) 0.0426(16) Uani 1 1 d . . . C35 C 0.2316(5) 0.6139(5) 0.3234(4) 0.0440(16) Uani 1 1 d . . . H35A H 0.1714 0.6469 0.3147 0.053 Uiso 1 1 calc R . . H35B H 0.2558 0.6052 0.2707 0.053 Uiso 1 1 calc R . . C36 C 0.1797(5) 0.6317(5) 0.5255(4) 0.0432(16) Uani 1 1 d . . . H36A H 0.1230 0.6600 0.5004 0.052 Uiso 1 1 calc R . . H36B H 0.1731 0.6315 0.5832 0.052 Uiso 1 1 calc R . . N1 N 0.1953(4) 0.7115(4) 0.7992(3) 0.0383(12) Uani 1 1 d . . . N2 N 0.2994(4) 0.6307(4) 0.8866(3) 0.0408(13) Uani 1 1 d . . . N3 N 0.1298(4) 0.7900(4) 0.8949(3) 0.0425(13) Uani 1 1 d . . . N4 N 0.2275(4) 0.6998(5) 0.9879(3) 0.0476(15) Uani 1 1 d . . . N5 N 0.3195(4) 0.4846(4) 1.0121(3) 0.0424(14) Uani 1 1 d . . . N6 N 0.2598(4) 0.3502(4) 1.0997(3) 0.0389(13) Uani 1 1 d . . . N7 N 0.2572(4) 0.5545(4) 1.1140(3) 0.0454(14) Uani 1 1 d . . . N8 N 0.1983(4) 0.4181(4) 1.2023(3) 0.0420(13) Uani 1 1 d . . . N9 N 0.1455(4) 0.2371(4) 1.1540(3) 0.0424(13) Uani 1 1 d . . . N10 N 0.0137(4) 0.1902(4) 1.1581(3) 0.0398(13) Uani 1 1 d . . . N11 N 0.0808(4) 0.3104(4) 1.2530(3) 0.0419(13) Uani 1 1 d . . . N12 N -0.0518(4) 0.2664(4) 1.2536(3) 0.0406(13) Uani 1 1 d . . . N13 N 0.1942(4) 0.5353(4) 0.5343(3) 0.0401(13) Uani 1 1 d . . . N14 N 0.2026(4) 0.3777(4) 0.6046(3) 0.0422(13) Uani 1 1 d . . . N15 N 0.2236(4) 0.5221(4) 0.3940(3) 0.0455(14) Uani 1 1 d . . . N16 N 0.2417(4) 0.3652(4) 0.4652(4) 0.0495(15) Uani 1 1 d . . . N17 N 0.3065(4) 0.2430(4) 0.6727(3) 0.0415(13) Uani 1 1 d . . . N18 N 0.4473(4) 0.2043(4) 0.6982(3) 0.0401(13) Uani 1 1 d . . . N19 N 0.3472(4) 0.2322(5) 0.5328(4) 0.0506(15) Uani 1 1 d . . . N20 N 0.4878(4) 0.1829(4) 0.5637(3) 0.0465(15) Uani 1 1 d . . . N21 N 0.6008(4) 0.2335(4) 0.6993(3) 0.0397(13) Uani 1 1 d . . . N22 N 0.7112(4) 0.3264(4) 0.6645(3) 0.0432(14) Uani 1 1 d . . . N23 N 0.6402(4) 0.2166(4) 0.5620(3) 0.0418(13) Uani 1 1 d . . . N24 N 0.7497(4) 0.3099(4) 0.5271(3) 0.0396(13) Uani 1 1 d . . . O1 O 0.2550(3) 0.5688(3) 0.8006(3) 0.0484(12) Uani 1 1 d . . . O2 O 0.2796(3) 0.3880(3) 0.9539(3) 0.0443(11) Uani 1 1 d . . . O3 O 0.1173(4) 0.2139(4) 1.0363(3) 0.0574(14) Uani 1 1 d . . . O4 O 0.0936(4) 0.7585(5) 1.0393(3) 0.0719(17) Uani 1 1 d . . . O5 O 0.1288(4) 0.5593(4) 1.2051(3) 0.0585(14) Uani 1 1 d . . . O6 O -0.0463(3) 0.3994(3) 1.2794(3) 0.0489(12) Uani 1 1 d . . . O7 O 0.2307(3) 0.4682(3) 0.6742(3) 0.0449(11) Uani 1 1 d . . . O8 O 0.3636(3) 0.3096(3) 0.7470(3) 0.0434(11) Uani 1 1 d . . . O9 O 0.5912(3) 0.3435(4) 0.7584(3) 0.0528(13) Uani 1 1 d . . . O10 O 0.3125(4) 0.4357(4) 0.3277(3) 0.0557(13) Uani 1 1 d . . . O11 O 0.4592(4) 0.2583(4) 0.4200(3) 0.0633(15) Uani 1 1 d . . . O12 O 0.6841(4) 0.3041(4) 0.4178(3) 0.0521(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 Cl5 0.0493(13) 0.1018(18) 0.0875(15) -0.0356(13) -0.0143(11) -0.0087(12) O1W 0.029(3) 0.082(4) 0.045(2) -0.035(2) 0.000(2) 0.004(2) O2W 0.050(3) 0.057(3) 0.048(2) -0.026(2) 0.014(2) -0.012(3) O3W 0.042(3) 0.058(3) 0.050(3) -0.021(2) 0.013(2) -0.008(2) O4W 0.030(3) 0.075(4) 0.056(3) -0.027(3) 0.008(2) -0.005(2) Tb1 0.0313(2) 0.0516(2) 0.03698(18) -0.02626(15) 0.00380(13) -0.00303(14) Cl1 0.0465(15) 0.108(2) 0.154(3) -0.0555(19) -0.0040(16) -0.0135(14) Cl2 0.0552(17) 0.0735(18) 0.217(4) -0.044(2) 0.021(2) -0.0093(14) Cl3 0.0432(15) 0.104(2) 0.176(3) 0.022(2) 0.0092(17) -0.0040(15) Cl4 0.399(11) 0.265(7) 0.073(2) -0.010(3) -0.011(4) 0.150(7) Cd1 0.0591(5) 0.0717(5) 0.0831(5) -0.0028(4) 0.0045(4) -0.0015(4) C1 0.037(4) 0.046(4) 0.037(3) -0.018(3) 0.004(3) -0.008(3) C2 0.038(4) 0.049(4) 0.043(3) -0.022(3) 0.009(3) -0.019(3) C3 0.035(4) 0.046(4) 0.046(3) -0.025(3) 0.005(3) -0.012(3) C4 0.044(5) 0.056(4) 0.052(4) -0.031(3) 0.005(3) -0.012(4) C5 0.026(4) 0.054(4) 0.042(3) -0.021(3) 0.003(3) -0.004(3) C6 0.054(5) 0.061(5) 0.056(4) -0.036(4) -0.002(4) -0.016(4) C7 0.027(4) 0.057(4) 0.045(3) -0.030(3) 0.004(3) -0.005(3) C8 0.036(4) 0.066(5) 0.045(3) -0.034(3) -0.003(3) -0.007(3) C9 0.032(4) 0.058(4) 0.041(3) -0.027(3) -0.005(3) -0.002(3) C10 0.038(4) 0.074(5) 0.040(3) -0.037(4) -0.001(3) -0.010(4) C11 0.030(4) 0.052(4) 0.048(3) -0.026(3) 0.005(3) -0.002(3) C12 0.036(4) 0.083(5) 0.040(3) -0.037(4) -0.006(3) -0.001(4) C13 0.042(4) 0.046(4) 0.041(3) -0.019(3) -0.006(3) 0.001(3) C14 0.040(4) 0.050(4) 0.034(3) -0.015(3) 0.000(3) 0.005(3) C15 0.041(4) 0.034(4) 0.041(3) -0.012(3) 0.003(3) -0.003(3) C16 0.034(4) 0.049(4) 0.033(3) -0.020(3) 0.002(3) -0.006(3) C17 0.050(5) 0.043(4) 0.061(4) -0.032(3) 0.000(4) -0.006(3) C18 0.035(4) 0.056(4) 0.041(3) -0.023(3) 0.012(3) -0.009(3) C19 0.020(3) 0.053(4) 0.037(3) -0.023(3) 0.001(3) -0.005(3) C20 0.025(4) 0.060(4) 0.034(3) -0.023(3) 0.004(3) -0.004(3) C21 0.024(4) 0.079(5) 0.055(4) -0.042(4) 0.006(3) -0.016(3) C22 0.031(4) 0.060(4) 0.044(3) -0.032(3) 0.002(3) -0.008(3) C23 0.028(4) 0.057(4) 0.045(3) -0.022(3) 0.006(3) -0.015(3) C24 0.060(5) 0.052(4) 0.056(4) -0.034(4) -0.006(4) -0.009(4) C25 0.033(4) 0.044(4) 0.030(3) -0.015(3) 0.002(3) -0.006(3) C26 0.036(4) 0.043(4) 0.050(3) -0.024(3) 0.003(3) -0.008(3) C27 0.048(4) 0.048(4) 0.040(3) -0.024(3) 0.004(3) -0.010(3) C28 0.050(5) 0.043(4) 0.053(4) -0.031(3) 0.002(4) -0.009(3) C29 0.031(4) 0.050(4) 0.042(3) -0.023(3) 0.005(3) -0.004(3) C30 0.044(5) 0.053(4) 0.054(4) -0.039(3) 0.007(3) -0.006(3) C31 0.036(4) 0.053(4) 0.032(3) -0.022(3) 0.002(3) -0.005(3) C32 0.045(4) 0.042(4) 0.045(3) -0.022(3) 0.006(3) 0.002(3) C33 0.026(4) 0.054(4) 0.043(3) -0.027(3) -0.001(3) 0.005(3) C34 0.042(4) 0.039(4) 0.048(4) -0.024(3) 0.003(3) 0.007(3) C35 0.041(4) 0.059(4) 0.036(3) -0.022(3) -0.004(3) -0.008(3) C36 0.028(4) 0.065(5) 0.044(3) -0.032(3) 0.011(3) -0.012(3) N1 0.041(3) 0.043(3) 0.035(3) -0.021(2) -0.003(2) -0.003(3) N2 0.042(4) 0.043(3) 0.040(3) -0.019(2) 0.000(3) -0.010(3) N3 0.034(3) 0.050(3) 0.051(3) -0.029(3) 0.000(3) -0.001(3) N4 0.033(3) 0.075(4) 0.044(3) -0.036(3) 0.002(3) -0.005(3) N5 0.035(3) 0.058(4) 0.040(3) -0.028(3) 0.007(2) -0.007(3) N6 0.036(3) 0.052(3) 0.033(2) -0.022(2) -0.002(2) -0.003(3) N7 0.044(4) 0.056(4) 0.043(3) -0.026(3) 0.000(3) -0.010(3) N8 0.033(3) 0.060(4) 0.040(3) -0.029(3) 0.003(2) -0.003(3) N9 0.039(3) 0.047(3) 0.040(3) -0.020(2) 0.005(2) -0.004(3) N10 0.033(3) 0.044(3) 0.042(3) -0.021(2) 0.008(2) -0.005(3) N11 0.038(4) 0.056(4) 0.041(3) -0.028(3) 0.004(2) -0.014(3) N12 0.031(3) 0.045(3) 0.050(3) -0.026(3) 0.006(2) -0.007(3) N13 0.029(3) 0.052(3) 0.044(3) -0.026(3) -0.002(2) -0.002(3) N14 0.034(3) 0.050(3) 0.042(3) -0.018(3) -0.002(2) -0.006(3) N15 0.037(3) 0.064(4) 0.038(3) -0.026(3) 0.009(2) -0.012(3) N16 0.046(4) 0.064(4) 0.051(3) -0.038(3) 0.006(3) -0.009(3) N17 0.035(3) 0.051(3) 0.046(3) -0.028(3) 0.005(2) -0.012(3) N18 0.037(3) 0.048(3) 0.042(3) -0.029(3) 0.000(2) 0.000(3) N19 0.049(4) 0.067(4) 0.046(3) -0.034(3) -0.006(3) 0.000(3) N20 0.040(4) 0.063(4) 0.047(3) -0.035(3) 0.012(3) -0.013(3) N21 0.029(3) 0.054(3) 0.042(3) -0.029(3) 0.008(2) -0.005(3) N22 0.038(3) 0.060(4) 0.040(3) -0.030(3) 0.002(2) -0.005(3) N23 0.038(3) 0.054(3) 0.040(3) -0.027(3) 0.006(2) -0.011(3) N24 0.042(3) 0.049(3) 0.031(2) -0.018(2) -0.002(2) -0.006(3) O1 0.056(3) 0.049(3) 0.048(2) -0.030(2) 0.005(2) -0.009(2) O2 0.040(3) 0.067(3) 0.037(2) -0.033(2) 0.001(2) -0.005(2) O3 0.051(3) 0.084(4) 0.049(3) -0.042(3) 0.013(2) -0.015(3) O4 0.062(4) 0.103(5) 0.058(3) -0.049(3) 0.011(3) 0.003(3) O5 0.046(3) 0.081(4) 0.066(3) -0.050(3) 0.010(3) -0.011(3) O6 0.044(3) 0.057(3) 0.054(3) -0.034(2) 0.002(2) -0.002(2) O7 0.045(3) 0.057(3) 0.038(2) -0.025(2) -0.003(2) -0.003(2) O8 0.036(3) 0.054(3) 0.048(2) -0.032(2) 0.000(2) 0.001(2) O9 0.041(3) 0.071(3) 0.062(3) -0.047(3) 0.019(2) -0.017(3) O10 0.052(3) 0.076(4) 0.046(2) -0.035(3) 0.004(2) -0.008(3) O11 0.061(4) 0.090(4) 0.046(3) -0.038(3) -0.001(3) -0.002(3) O12 0.055(3) 0.069(3) 0.042(2) -0.032(2) -0.001(2) -0.010(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 O1W Tb1 2.381(5) . ? O2W Tb1 2.384(5) . ? O3W Tb1 2.418(5) . ? O4W Tb1 2.435(5) . ? Tb1 O8 2.344(4) . ? Tb1 O7 2.361(4) . ? Tb1 O2 2.362(4) . ? Tb1 O1 2.367(5) . ? Cl1 Cd1 2.476(3) . ? Cl2 Cd1 2.451(3) . ? Cl3 Cd1 2.442(3) . ? Cl4 Cd1 2.390(4) . ? C1 O1 1.222(8) . ? C1 N1 1.339(9) . ? C1 N2 1.370(9) . ? C2 N3 1.460(8) . ? C2 N1 1.488(8) . ? C2 C3 1.534(10) . ? C2 H2 0.9900 . ? C3 N2 1.466(8) . ? C3 N4 1.477(8) . ? C3 H3 0.9900 . ? C4 O4 1.212(8) . ? C4 N4 1.367(10) . ? C4 N3 1.382(9) . ? C5 N2 1.402(9) . ? C5 N5 1.457(8) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.435(9) . ? C6 N4 1.458(9) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.260(7) . ? C7 N6 1.337(8) . ? C7 N5 1.355(8) . ? C8 N5 1.444(8) . ? C8 N7 1.462(9) . ? C8 C9 1.564(10) . ? C8 H8 0.9900 . ? C9 N8 1.446(8) . ? C9 N6 1.464(8) . ? C9 H9 0.9900 . ? C10 O5 1.232(8) . ? C10 N7 1.352(9) . ? C10 N8 1.388(9) . ? C11 N9 1.437(9) . ? C11 N6 1.465(9) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.409(9) . ? C12 N11 1.459(9) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.244(7) . ? C13 N9 1.338(9) . ? C13 N10 1.385(8) . ? C14 N9 1.446(7) . ? C14 N11 1.465(9) . ? C14 C15 1.530(10) . ? C14 H14 0.9900 . ? C15 N10 1.451(8) . ? C15 N12 1.466(8) . ? C15 H15 0.9900 . ? C16 O6 1.250(8) . ? C16 N11 1.333(9) . ? C16 N12 1.375(8) . ? C17 N3 1.437(9) 2_567 ? C17 N10 1.437(9) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N1 1.444(9) 2_567 ? C18 N12 1.445(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O7 1.244(7) . ? C19 N14 1.360(8) . ? C19 N13 1.365(8) . ? C20 N15 1.464(7) . ? C20 N13 1.462(8) . ? C20 C21 1.521(10) . ? C20 H20 0.9900 . ? C21 N14 1.461(8) . ? C21 N16 1.480(8) . ? C21 H21 0.9900 . ? C22 O10 1.237(7) . ? C22 N15 1.326(9) . ? C22 N16 1.376(9) . ? C23 N17 1.433(9) . ? C23 N14 1.431(9) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N16 1.427(9) . ? C24 N19 1.452(10) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O8 1.239(7) . ? C25 N17 1.331(8) . ? C25 N18 1.345(8) . ? C26 N19 1.450(8) . ? C26 N17 1.462(8) . ? C26 C27 1.532(10) . ? C26 H26 0.9900 . ? C27 N20 1.469(8) . ? C27 N18 1.466(8) . ? C27 H27 0.9900 . ? C28 O11 1.218(8) . ? C28 N19 1.364(9) . ? C28 N20 1.380(9) . ? C29 N21 1.449(8) . ? C29 N18 1.453(9) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N20 1.413(9) . ? C30 N23 1.453(9) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O9 1.222(7) . ? C31 N22 1.357(8) . ? C31 N21 1.378(8) . ? C32 N23 1.451(8) . ? C32 N21 1.458(8) . ? C32 C33 1.556(10) . ? C32 H32 0.9900 . ? C33 N22 1.459(8) . ? C33 N24 1.466(8) . ? C33 H33 0.9900 . ? C34 O12 1.221(8) . ? C34 N23 1.356(8) . ? C34 N24 1.366(9) . ? C35 N15 1.436(9) . ? C35 N22 1.453(9) 2_666 ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N24 1.433(8) 2_666 ? C36 N13 1.437(9) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? N1 C18 1.444(9) 2_567 ? N3 C17 1.437(9) 2_567 ? N22 C35 1.453(9) 2_666 ? N24 C36 1.433(8) 2_666 ? 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 O8 Tb1 O7 76.48(16) . . ? O8 Tb1 O2 126.42(16) . . ? O7 Tb1 O2 151.81(17) . . ? O8 Tb1 O1 151.05(16) . . ? O7 Tb1 O1 87.46(16) . . ? O2 Tb1 O1 77.29(16) . . ? O8 Tb1 O1W 73.37(16) . . ? O7 Tb1 O1W 137.35(15) . . ? O2 Tb1 O1W 70.30(15) . . ? O1 Tb1 O1W 105.16(18) . . ? O8 Tb1 O2W 70.90(16) . . ? O7 Tb1 O2W 104.79(17) . . ? O2 Tb1 O2W 73.17(16) . . ? O1 Tb1 O2W 137.36(16) . . ? O1W Tb1 O2W 93.09(19) . . ? O8 Tb1 O3W 80.22(16) . . ? O7 Tb1 O3W 72.93(17) . . ? O2 Tb1 O3W 122.74(17) . . ? O1 Tb1 O3W 72.03(16) . . ? O1W Tb1 O3W 72.79(18) . . ? O2W Tb1 O3W 150.56(16) . . ? O8 Tb1 O4W 122.96(17) . . ? O7 Tb1 O4W 72.21(16) . . ? O2 Tb1 O4W 80.61(16) . . ? O1 Tb1 O4W 72.68(18) . . ? O1W Tb1 O4W 150.38(16) . . ? O2W Tb1 O4W 72.72(18) . . ? O3W Tb1 O4W 130.71(18) . . ? Cl4 Cd1 Cl3 110.6(2) . . ? Cl4 Cd1 Cl2 114.0(3) . . ? Cl3 Cd1 Cl2 113.16(11) . . ? Cl4 Cd1 Cl1 107.4(2) . . ? Cl3 Cd1 Cl1 106.26(14) . . ? Cl2 Cd1 Cl1 104.74(11) . . ? O1 C1 N1 125.4(6) . . ? O1 C1 N2 125.1(7) . . ? N1 C1 N2 109.5(6) . . ? N3 C2 N1 113.4(5) . . ? N3 C2 C3 104.7(5) . . ? N1 C2 C3 103.6(5) . . ? N3 C2 H2 111.6 . . ? N1 C2 H2 111.6 . . ? C3 C2 H2 111.6 . . ? N2 C3 N4 113.6(5) . . ? N2 C3 C2 102.9(5) . . ? N4 C3 C2 102.5(5) . . ? N2 C3 H3 112.3 . . ? N4 C3 H3 112.3 . . ? C2 C3 H3 112.3 . . ? O4 C4 N4 126.5(7) . . ? O4 C4 N3 125.2(7) . . ? N4 C4 N3 108.2(6) . . ? N2 C5 N5 114.3(5) . . ? N2 C5 H5A 108.7 . . ? N5 C5 H5A 108.7 . . ? N2 C5 H5B 108.7 . . ? N5 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? N7 C6 N4 113.9(6) . . ? N7 C6 H6A 108.8 . . ? N4 C6 H6A 108.8 . . ? N7 C6 H6B 108.8 . . ? N4 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N6 124.5(6) . . ? O2 C7 N5 125.0(6) . . ? N6 C7 N5 110.5(5) . . ? N5 C8 N7 114.6(6) . . ? N5 C8 C9 103.3(5) . . ? N7 C8 C9 102.6(5) . . ? N5 C8 H8 111.9 . . ? N7 C8 H8 111.9 . . ? C9 C8 H8 111.9 . . ? N8 C9 N6 113.3(6) . . ? N8 C9 C8 104.0(5) . . ? N6 C9 C8 102.5(5) . . ? N8 C9 H9 112.1 . . ? N6 C9 H9 112.1 . . ? C8 C9 H9 112.1 . . ? O5 C10 N7 126.2(7) . . ? O5 C10 N8 124.8(6) . . ? N7 C10 N8 109.0(6) . . ? N9 C11 N6 113.9(6) . . ? N9 C11 H11A 108.8 . . ? N6 C11 H11A 108.8 . . ? N9 C11 H11B 108.8 . . ? N6 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? N8 C12 N11 114.8(5) . . ? N8 C12 H12A 108.6 . . ? N11 C12 H12A 108.6 . . ? N8 C12 H12B 108.6 . . ? N11 C12 H12B 108.6 . . ? H12A C12 H12B 107.5 . . ? O3 C13 N9 127.4(6) . . ? O3 C13 N10 125.0(6) . . ? N9 C13 N10 107.6(5) . . ? N9 C14 N11 114.4(5) . . ? N9 C14 C15 102.0(5) . . ? N11 C14 C15 102.1(5) . . ? N9 C14 H14 112.5 . . ? N11 C14 H14 112.5 . . ? C15 C14 H14 112.5 . . ? N10 C15 N12 113.1(5) . . ? N10 C15 C14 104.6(5) . . ? N12 C15 C14 104.4(5) . . ? N10 C15 H15 111.4 . . ? N12 C15 H15 111.4 . . ? C14 C15 H15 111.4 . . ? O6 C16 N11 127.0(6) . . ? O6 C16 N12 124.1(6) . . ? N11 C16 N12 108.9(6) . . ? N3 C17 N10 114.2(5) 2_567 . ? N3 C17 H17A 108.7 2_567 . ? N10 C17 H17A 108.7 . . ? N3 C17 H17B 108.7 2_567 . ? N10 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? N1 C18 N12 112.7(5) 2_567 . ? N1 C18 H18A 109.1 2_567 . ? N12 C18 H18A 109.1 . . ? N1 C18 H18B 109.1 2_567 . ? N12 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? O7 C19 N14 126.3(6) . . ? O7 C19 N13 123.9(6) . . ? N14 C19 N13 109.8(5) . . ? N15 C20 N13 115.5(5) . . ? N15 C20 C21 103.3(5) . . ? N13 C20 C21 103.9(5) . . ? N15 C20 H20 111.2 . . ? N13 C20 H20 111.2 . . ? C21 C20 H20 111.2 . . ? N14 C21 N16 113.6(6) . . ? N14 C21 C20 104.1(5) . . ? N16 C21 C20 104.1(5) . . ? N14 C21 H21 111.5 . . ? N16 C21 H21 111.5 . . ? C20 C21 H21 111.5 . . ? O10 C22 N15 126.7(7) . . ? O10 C22 N16 122.6(6) . . ? N15 C22 N16 110.7(5) . . ? N17 C23 N14 114.7(5) . . ? N17 C23 H23A 108.6 . . ? N14 C23 H23A 108.6 . . ? N17 C23 H23B 108.6 . . ? N14 C23 H23B 108.6 . . ? H23A C23 H23B 107.6 . . ? N16 C24 N19 113.6(6) . . ? N16 C24 H24A 108.8 . . ? N19 C24 H24A 108.8 . . ? N16 C24 H24B 108.8 . . ? N19 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? O8 C25 N17 125.1(6) . . ? O8 C25 N18 125.3(6) . . ? N17 C25 N18 109.6(6) . . ? N19 C26 N17 115.3(6) . . ? N19 C26 C27 104.7(5) . . ? N17 C26 C27 102.8(5) . . ? N19 C26 H26 111.2 . . ? N17 C26 H26 111.2 . . ? C27 C26 H26 111.2 . . ? N20 C27 N18 113.1(5) . . ? N20 C27 C26 102.6(5) . . ? N18 C27 C26 102.9(5) . . ? N20 C27 H27 112.5 . . ? N18 C27 H27 112.5 . . ? C26 C27 H27 112.5 . . ? O11 C28 N19 125.4(7) . . ? O11 C28 N20 126.6(7) . . ? N19 C28 N20 108.0(6) . . ? N21 C29 N18 113.7(5) . . ? N21 C29 H29A 108.8 . . ? N18 C29 H29A 108.8 . . ? N21 C29 H29B 108.8 . . ? N18 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? N20 C30 N23 115.5(5) . . ? N20 C30 H30A 108.4 . . ? N23 C30 H30A 108.4 . . ? N20 C30 H30B 108.4 . . ? N23 C30 H30B 108.4 . . ? H30A C30 H30B 107.5 . . ? O9 C31 N22 125.8(6) . . ? O9 C31 N21 126.4(6) . . ? N22 C31 N21 107.6(5) . . ? N23 C32 N21 115.5(6) . . ? N23 C32 C33 102.9(5) . . ? N21 C32 C33 102.4(5) . . ? N23 C32 H32 111.8 . . ? N21 C32 H32 111.8 . . ? C33 C32 H32 111.8 . . ? N22 C33 N24 114.2(5) . . ? N22 C33 C32 103.3(5) . . ? N24 C33 C32 102.6(5) . . ? N22 C33 H33 112.0 . . ? N24 C33 H33 112.0 . . ? C32 C33 H33 112.0 . . ? O12 C34 N23 126.6(7) . . ? O12 C34 N24 125.5(6) . . ? N23 C34 N24 107.9(5) . . ? N15 C35 N22 114.4(5) . 2_666 ? N15 C35 H35A 108.7 . . ? N22 C35 H35A 108.7 2_666 . ? N15 C35 H35B 108.7 . . ? N22 C35 H35B 108.7 2_666 . ? H35A C35 H35B 107.6 . . ? N24 C36 N13 114.1(5) 2_666 . ? N24 C36 H36A 108.7 2_666 . ? N13 C36 H36A 108.7 . . ? N24 C36 H36B 108.7 2_666 . ? N13 C36 H36B 108.7 . . ? H36A C36 H36B 107.6 . . ? C1 N1 C18 122.8(5) . 2_567 ? C1 N1 C2 111.6(5) . . ? C18 N1 C2 123.8(6) 2_567 . ? C1 N2 C5 123.9(6) . . ? C1 N2 C3 112.2(6) . . ? C5 N2 C3 123.8(5) . . ? C4 N3 C17 122.2(6) . 2_567 ? C4 N3 C2 111.5(6) . . ? C17 N3 C2 125.6(5) 2_567 . ? C4 N4 C6 121.7(6) . . ? C4 N4 C3 112.5(6) . . ? C6 N4 C3 124.4(6) . . ? C7 N5 C8 111.8(5) . . ? C7 N5 C5 122.7(5) . . ? C8 N5 C5 125.1(5) . . ? C7 N6 C11 123.3(5) . . ? C7 N6 C9 111.9(5) . . ? C11 N6 C9 122.6(5) . . ? C10 N7 C6 123.8(6) . . ? C10 N7 C8 112.8(6) . . ? C6 N7 C8 123.4(6) . . ? C10 N8 C12 122.8(5) . . ? C10 N8 C9 111.6(5) . . ? C12 N8 C9 124.5(6) . . ? C13 N9 C11 122.8(5) . . ? C13 N9 C14 114.6(6) . . ? C11 N9 C14 121.1(6) . . ? C13 N10 C17 122.3(5) . . ? C13 N10 C15 111.1(5) . . ? C17 N10 C15 125.3(5) . . ? C16 N11 C12 121.9(5) . . ? C16 N11 C14 113.6(5) . . ? C12 N11 C14 122.7(6) . . ? C16 N12 C18 123.4(5) . . ? C16 N12 C15 110.7(5) . . ? C18 N12 C15 123.7(5) . . ? C19 N13 C36 123.1(5) . . ? C19 N13 C20 111.0(5) . . ? C36 N13 C20 123.4(6) . . ? C19 N14 C23 122.4(5) . . ? C19 N14 C21 111.1(5) . . ? C23 N14 C21 126.4(6) . . ? C22 N15 C35 123.0(5) . . ? C22 N15 C20 112.2(6) . . ? C35 N15 C20 124.6(6) . . ? C22 N16 C24 125.0(6) . . ? C22 N16 C21 109.3(6) . . ? C24 N16 C21 125.2(6) . . ? C25 N17 C23 123.6(5) . . ? C25 N17 C26 112.5(6) . . ? C23 N17 C26 123.8(5) . . ? C25 N18 C29 123.0(5) . . ? C25 N18 C27 111.8(6) . . ? C29 N18 C27 123.3(6) . . ? C28 N19 C26 112.3(6) . . ? C28 N19 C24 122.7(6) . . ? C26 N19 C24 124.4(6) . . ? C28 N20 C30 123.3(5) . . ? C28 N20 C27 112.3(6) . . ? C30 N20 C27 123.8(6) . . ? C31 N21 C29 123.5(5) . . ? C31 N21 C32 113.3(5) . . ? C29 N21 C32 122.1(5) . . ? C31 N22 C35 121.3(5) . 2_666 ? C31 N22 C33 113.2(5) . . ? C35 N22 C33 123.4(5) 2_666 . ? C34 N23 C32 113.7(6) . . ? C34 N23 C30 122.1(5) . . ? C32 N23 C30 122.8(5) . . ? C34 N24 C36 123.3(5) . 2_666 ? C34 N24 C33 112.8(5) . . ? C36 N24 C33 123.0(5) 2_666 . ? C1 O1 Tb1 155.7(5) . . ? C7 O2 Tb1 157.1(4) . . ? C19 O7 Tb1 154.4(4) . . ? C25 O8 Tb1 157.8(5) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.399 _refine_diff_density_min -2.551 _refine_diff_density_rms 0.164 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.015 0.000 0.001 1108 420 ' ' 2 0.000 0.500 1.000 97 37 ' ' 3 0.500 0.500 0.500 97 31 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 902609' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p210 #TrackingRef 'submit-210.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H96 Cd Cl5 Dy N24 O42' _chemical_formula_weight 1989.52 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 '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 15.1428(19) _cell_length_b 15.569(2) _cell_length_c 17.119(2) _cell_angle_alpha 64.842(4) _cell_angle_beta 80.884(5) _cell_angle_gamma 81.789(4) _cell_volume 3594.2(8) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.838 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2030 _exptl_absorpt_coefficient_mu 1.629 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6767 _exptl_absorpt_correction_T_max 0.7580 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39996 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.10 _reflns_number_total 12679 _reflns_number_gt 10956 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0729P)^2^+0.8943P] 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 12679 _refine_ls_number_parameters 748 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1180 _refine_ls_wR_factor_gt 0.1135 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.005 _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 Cl5 Cl 0.48825(9) 0.30148(12) 1.04399(10) 0.0709(4) Uani 1 1 d . . . O1W O 0.5652(2) 0.6341(2) 1.14283(18) 0.0460(7) Uani 1 1 d . . . O2W O 0.7610(2) 0.7383(2) 1.1122(2) 0.0468(7) Uani 1 1 d . . . O3W O 0.6048(2) 0.4833(2) 1.30242(19) 0.0465(7) Uani 1 1 d . . . O4W O 0.8693(2) 0.5662(2) 1.1640(2) 0.0500(8) Uani 1 1 d . . . Dy1 Dy 0.709024(12) 0.585647(13) 1.193489(11) 0.03187(8) Uani 1 1 d . . . Cl1 Cl 0.98775(10) 0.25940(14) 1.65078(14) 0.0925(5) Uani 1 1 d . . . Cl2 Cl 0.87581(12) 0.02997(12) 1.69640(18) 0.1152(8) Uani 1 1 d . . . Cl3 Cl 1.14843(12) 0.03281(15) 1.66253(17) 0.1309(10) Uani 1 1 d . . . Cl4 Cl 1.0079(4) 0.1765(4) 1.46139(17) 0.281(3) Uani 1 1 d . . . Cd1 Cd 1.00526(3) 0.11898(3) 1.61519(3) 0.07675(15) Uani 1 1 d . . . C1 C 0.7151(3) 0.5931(3) 0.9838(2) 0.0330(8) Uani 1 1 d . . . C2 C 0.7214(3) 0.6121(3) 0.8416(3) 0.0379(9) Uani 1 1 d . . . H2 H 0.6793 0.6555 0.8002 0.045 Uiso 1 1 calc R . . C3 C 0.6811(3) 0.5171(3) 0.9032(2) 0.0383(9) Uani 1 1 d . . . H3 H 0.6196 0.5159 0.8909 0.046 Uiso 1 1 calc R . . C4 C 0.8109(3) 0.4848(3) 0.8234(3) 0.0407(10) Uani 1 1 d . . . C5 C 0.6389(3) 0.4460(3) 1.0682(3) 0.0362(9) Uani 1 1 d . . . H5A H 0.6122 0.4774 1.1064 0.043 Uiso 1 1 calc R . . H5B H 0.5905 0.4210 1.0545 0.043 Uiso 1 1 calc R . . C6 C 0.7337(3) 0.3454(3) 0.9293(3) 0.0439(10) Uani 1 1 d . . . H6A H 0.7632 0.3152 0.8910 0.053 Uiso 1 1 calc R . . H6B H 0.6699 0.3346 0.9397 0.053 Uiso 1 1 calc R . . C7 C 0.7507(3) 0.3681(3) 1.1736(2) 0.0345(9) Uani 1 1 d . . . C8 C 0.7232(3) 0.2832(3) 1.0966(3) 0.0370(9) Uani 1 1 d . . . H8 H 0.6696 0.2484 1.1072 0.044 Uiso 1 1 calc R . . C9 C 0.7917(3) 0.2246(3) 1.1601(3) 0.0365(9) Uani 1 1 d . . . H9 H 0.7693 0.1637 1.2036 0.044 Uiso 1 1 calc R . . C10 C 0.8546(3) 0.2503(3) 1.0193(3) 0.0439(10) Uani 1 1 d . . . C11 C 0.8534(3) 0.2569(3) 1.2756(2) 0.0368(9) Uani 1 1 d . . . H11A H 0.8436 0.1902 1.3131 0.044 Uiso 1 1 calc R . . H11B H 0.8290 0.2949 1.3085 0.044 Uiso 1 1 calc R . . C12 C 0.9483(3) 0.1476(3) 1.1340(3) 0.0411(10) Uani 1 1 d . . . H12A H 0.9767 0.1269 1.0886 0.049 Uiso 1 1 calc R . . H12B H 0.9302 0.0908 1.1852 0.049 Uiso 1 1 calc R . . C13 C 0.9907(3) 0.3316(3) 1.2629(2) 0.0351(9) Uani 1 1 d . . . C14 C 1.0108(3) 0.1918(3) 1.2404(2) 0.0349(9) Uani 1 1 d . . . H14 H 1.0002 0.1285 1.2877 0.042 Uiso 1 1 calc R . . C15 C 1.1037(3) 0.2226(3) 1.2398(2) 0.0372(9) Uani 1 1 d . . . H15 H 1.1379 0.1738 1.2862 0.045 Uiso 1 1 calc R . . C16 C 1.0951(3) 0.2141(3) 1.1073(2) 0.0355(9) Uani 1 1 d . . . C17 C 1.1461(3) 0.3526(4) 1.2755(3) 0.0426(10) Uani 1 1 d . . . H17A H 1.1142 0.3863 1.3101 0.051 Uiso 1 1 calc R . . H17B H 1.1866 0.3015 1.3122 0.051 Uiso 1 1 calc R . . C18 C 0.7588(3) 0.7481(3) 0.8725(3) 0.0387(9) Uani 1 1 d . . . H18A H 0.7376 0.7677 0.9201 0.046 Uiso 1 1 calc R . . H18B H 0.7251 0.7888 0.8234 0.046 Uiso 1 1 calc R . . C19 C 0.6288(3) 0.7430(3) 1.2914(2) 0.0323(8) Uani 1 1 d . . . C20 C 0.5651(3) 0.8489(3) 1.3526(3) 0.0377(9) Uani 1 1 d . . . H20 H 0.5555 0.9186 1.3188 0.045 Uiso 1 1 calc R . . C21 C 0.6629(3) 0.8180(3) 1.3740(3) 0.0381(9) Uani 1 1 d . . . H21 H 0.6991 0.8733 1.3538 0.046 Uiso 1 1 calc R . . C22 C 0.5656(3) 0.7729(3) 1.5031(3) 0.0424(10) Uani 1 1 d . . . C23 C 0.7846(3) 0.7139(3) 1.3263(3) 0.0363(9) Uani 1 1 d . . . H23A H 0.8255 0.7560 1.3286 0.044 Uiso 1 1 calc R . . H23B H 0.8004 0.7082 1.2708 0.044 Uiso 1 1 calc R . . C24 C 0.7275(3) 0.7303(3) 1.5205(3) 0.0482(11) Uani 1 1 d . . . H24A H 0.7773 0.7706 1.4917 0.058 Uiso 1 1 calc R . . H24B H 0.7088 0.7335 1.5767 0.058 Uiso 1 1 calc R . . C25 C 0.7886(3) 0.5389(3) 1.3903(2) 0.0332(8) Uani 1 1 d . . . C26 C 0.8263(3) 0.6049(3) 1.4779(3) 0.0389(9) Uani 1 1 d . . . H26 H 0.8840 0.6322 1.4698 0.047 Uiso 1 1 calc R . . C27 C 0.8357(3) 0.4950(3) 1.5259(2) 0.0343(9) Uani 1 1 d . . . H27 H 0.8984 0.4700 1.5379 0.041 Uiso 1 1 calc R . . C28 C 0.7349(3) 0.5582(3) 1.6101(3) 0.0391(9) Uani 1 1 d . . . C29 C 0.8209(3) 0.3673(3) 1.4739(3) 0.0377(9) Uani 1 1 d . . . H29A H 0.8774 0.3390 1.4990 0.045 Uiso 1 1 calc R . . H29B H 0.8273 0.3679 1.4158 0.045 Uiso 1 1 calc R . . C30 C 0.7679(3) 0.3849(3) 1.6770(3) 0.0409(10) Uani 1 1 d . . . H30A H 0.7440 0.3938 1.7300 0.049 Uiso 1 1 calc R . . H30B H 0.8279 0.3515 1.6856 0.049 Uiso 1 1 calc R . . C31 C 0.6895(3) 0.2797(3) 1.4939(3) 0.0365(9) Uani 1 1 d . . . C32 C 0.7433(3) 0.2625(3) 1.6211(2) 0.0332(8) Uani 1 1 d . . . H32 H 0.7999 0.2251 1.6420 0.040 Uiso 1 1 calc R . . C33 C 0.6654(3) 0.1983(3) 1.6451(3) 0.0371(9) Uani 1 1 d . . . H33 H 0.6853 0.1303 1.6771 0.045 Uiso 1 1 calc R . . C34 C 0.6294(3) 0.3051(3) 1.7121(2) 0.0378(9) Uani 1 1 d . . . C35 C 0.4187(3) 0.8429(3) 1.4504(3) 0.0413(10) Uani 1 1 d . . . H35A H 0.4050 0.9091 1.4102 0.050 Uiso 1 1 calc R . . H35B H 0.4043 0.8393 1.5096 0.050 Uiso 1 1 calc R . . C36 C 0.4791(3) 0.8154(3) 1.2523(2) 0.0375(9) Uani 1 1 d . . . H36A H 0.4989 0.7968 1.2039 0.045 Uiso 1 1 calc R . . H36B H 0.4625 0.8842 1.2277 0.045 Uiso 1 1 calc R . . N1 N 0.7396(2) 0.6511(3) 0.9000(2) 0.0359(7) Uani 1 1 d . . . N2 N 0.6807(2) 0.5159(2) 0.9885(2) 0.0367(8) Uani 1 1 d . . . N3 N 0.8014(2) 0.5821(3) 0.7978(2) 0.0388(8) Uani 1 1 d . . . N4 N 0.7423(2) 0.4463(3) 0.8856(2) 0.0418(8) Uani 1 1 d . . . N5 N 0.7010(2) 0.3679(2) 1.1138(2) 0.0371(8) Uani 1 1 d . . . N6 N 0.8051(2) 0.2875(2) 1.2004(2) 0.0354(7) Uani 1 1 d . . . N7 N 0.7721(3) 0.2994(3) 1.0121(2) 0.0432(8) Uani 1 1 d . . . N8 N 0.8695(2) 0.2094(3) 1.1042(2) 0.0403(8) Uani 1 1 d . . . N9 N 0.9494(2) 0.2661(2) 1.2531(2) 0.0358(7) Uani 1 1 d . . . N10 N 1.0815(2) 0.3107(3) 1.2515(2) 0.0371(8) Uani 1 1 d . . . N11 N 1.0143(2) 0.1908(2) 1.1561(2) 0.0362(8) Uani 1 1 d . . . N12 N 1.1467(2) 0.2364(2) 1.1530(2) 0.0375(8) Uani 1 1 d . . . N13 N 0.5531(2) 0.7957(2) 1.3025(2) 0.0355(7) Uani 1 1 d . . . N14 N 0.6950(2) 0.7568(2) 1.3287(2) 0.0365(8) Uani 1 1 d . . . N15 N 0.5135(2) 0.8181(3) 1.4367(2) 0.0408(8) Uani 1 1 d . . . N16 N 0.6528(3) 0.7683(3) 1.4679(2) 0.0451(9) Uani 1 1 d . . . N17 N 0.7982(2) 0.6207(2) 1.3963(2) 0.0358(7) Uani 1 1 d . . . N18 N 0.8053(2) 0.4635(2) 1.4662(2) 0.0349(7) Uani 1 1 d . . . N19 N 0.7587(3) 0.6344(3) 1.5351(2) 0.0414(8) Uani 1 1 d . . . N20 N 0.7756(2) 0.4772(3) 1.6055(2) 0.0384(8) Uani 1 1 d . . . N21 N 0.7497(2) 0.3087(2) 1.5272(2) 0.0380(8) Uani 1 1 d . . . N22 N 0.6383(2) 0.2166(3) 1.5614(2) 0.0384(8) Uani 1 1 d . . . N23 N 0.7103(2) 0.3258(3) 1.6643(2) 0.0381(8) Uani 1 1 d . . . N24 N 0.6000(2) 0.2334(2) 1.6985(2) 0.0366(8) Uani 1 1 d . . . O1 O 0.72185(19) 0.6107(2) 1.04725(17) 0.0383(6) Uani 1 1 d . . . O2 O 0.7456(2) 0.4313(2) 1.19925(18) 0.0415(7) Uani 1 1 d . . . O3 O 0.9545(2) 0.3983(2) 1.27944(19) 0.0421(7) Uani 1 1 d . . . O4 O 0.8700(2) 0.4415(2) 0.7938(2) 0.0516(8) Uani 1 1 d . . . O5 O 0.9059(2) 0.2423(3) 0.9591(2) 0.0621(10) Uani 1 1 d . . . O6 O 1.1171(2) 0.2135(2) 1.0352(2) 0.0502(8) Uani 1 1 d . . . O7 O 0.63594(19) 0.6899(2) 1.25374(18) 0.0397(7) Uani 1 1 d . . . O8 O 0.7691(2) 0.5315(2) 1.32607(18) 0.0408(7) Uani 1 1 d . . . O9 O 0.6836(2) 0.3039(2) 1.41660(18) 0.0467(7) Uani 1 1 d . . . O10 O 0.5400(3) 0.7426(3) 1.5804(2) 0.0597(9) Uani 1 1 d . . . O11 O 0.6868(2) 0.5642(3) 1.6725(2) 0.0509(8) Uani 1 1 d . . . O12 O 0.5902(2) 0.3433(2) 1.7581(2) 0.0502(8) 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 Cl5 0.0517(8) 0.0882(10) 0.0749(9) -0.0312(8) -0.0218(7) -0.0038(7) O1W 0.0364(16) 0.068(2) 0.0352(15) -0.0256(15) -0.0050(12) 0.0045(14) O2W 0.0526(19) 0.0427(17) 0.0450(16) -0.0217(14) 0.0088(14) -0.0075(14) O3W 0.0393(17) 0.0515(18) 0.0413(16) -0.0154(14) 0.0056(13) -0.0046(13) O4W 0.0332(16) 0.065(2) 0.0451(17) -0.0201(15) 0.0030(13) -0.0003(14) Dy1 0.03041(12) 0.04210(12) 0.02719(11) -0.01998(8) -0.00144(7) 0.00094(8) Cl1 0.0464(8) 0.0930(12) 0.1368(16) -0.0437(11) -0.0140(9) -0.0089(8) Cl2 0.0563(9) 0.0606(9) 0.202(2) -0.0375(12) 0.0094(12) -0.0009(7) Cl3 0.0496(9) 0.0896(13) 0.161(2) 0.0299(12) 0.0035(10) 0.0015(8) Cl4 0.395(7) 0.264(5) 0.0595(14) -0.007(2) -0.020(2) 0.154(5) Cd1 0.0597(3) 0.0638(3) 0.0715(3) 0.0013(2) -0.0014(2) 0.0031(2) C1 0.0267(19) 0.043(2) 0.0310(19) -0.0188(17) -0.0040(16) 0.0045(16) C2 0.029(2) 0.059(3) 0.033(2) -0.0253(19) -0.0091(17) 0.0003(18) C3 0.032(2) 0.058(3) 0.0314(19) -0.0231(19) -0.0092(17) 0.0001(18) C4 0.036(2) 0.064(3) 0.032(2) -0.028(2) -0.0104(18) -0.003(2) C5 0.029(2) 0.048(2) 0.035(2) -0.0227(18) -0.0002(16) 0.0007(17) C6 0.048(3) 0.056(3) 0.042(2) -0.032(2) -0.009(2) -0.006(2) C7 0.029(2) 0.045(2) 0.0302(19) -0.0170(17) 0.0038(16) -0.0056(17) C8 0.035(2) 0.042(2) 0.039(2) -0.0208(18) 0.0009(17) -0.0107(17) C9 0.036(2) 0.040(2) 0.039(2) -0.0220(18) 0.0031(17) -0.0085(17) C10 0.042(3) 0.051(3) 0.045(2) -0.027(2) -0.004(2) -0.004(2) C11 0.034(2) 0.046(2) 0.0313(19) -0.0191(17) 0.0008(16) -0.0017(17) C12 0.043(2) 0.035(2) 0.051(2) -0.0252(19) -0.002(2) -0.0009(18) C13 0.039(2) 0.043(2) 0.0238(18) -0.0140(17) -0.0043(16) -0.0033(18) C14 0.037(2) 0.033(2) 0.0290(18) -0.0105(16) 0.0015(16) 0.0013(16) C15 0.037(2) 0.045(2) 0.0274(18) -0.0158(17) -0.0032(16) 0.0042(18) C16 0.039(2) 0.035(2) 0.0306(19) -0.0136(16) -0.0013(17) -0.0013(17) C17 0.038(2) 0.069(3) 0.030(2) -0.031(2) -0.0035(17) -0.003(2) C18 0.034(2) 0.044(2) 0.040(2) -0.0223(19) -0.0035(18) 0.0076(17) C19 0.031(2) 0.038(2) 0.0295(18) -0.0159(17) 0.0013(16) -0.0038(16) C20 0.045(2) 0.034(2) 0.038(2) -0.0173(17) -0.0023(18) -0.0075(17) C21 0.046(2) 0.031(2) 0.041(2) -0.0170(17) -0.0037(19) -0.0090(17) C22 0.049(3) 0.046(2) 0.042(2) -0.029(2) -0.001(2) -0.002(2) C23 0.033(2) 0.040(2) 0.034(2) -0.0145(17) 0.0016(17) -0.0055(17) C24 0.053(3) 0.059(3) 0.051(3) -0.038(2) -0.013(2) -0.007(2) C25 0.0240(19) 0.044(2) 0.0321(19) -0.0161(17) -0.0036(15) -0.0013(16) C26 0.030(2) 0.056(3) 0.035(2) -0.0221(19) -0.0028(17) -0.0106(18) C27 0.027(2) 0.049(2) 0.0310(19) -0.0203(18) -0.0024(16) -0.0043(17) C28 0.035(2) 0.055(3) 0.036(2) -0.025(2) -0.0066(18) -0.0057(19) C29 0.031(2) 0.052(2) 0.0315(19) -0.0213(18) 0.0027(16) -0.0004(18) C30 0.040(2) 0.059(3) 0.0287(19) -0.0207(19) -0.0056(17) -0.006(2) C31 0.037(2) 0.039(2) 0.036(2) -0.0210(18) -0.0046(17) 0.0077(17) C32 0.030(2) 0.039(2) 0.0290(18) -0.0147(16) -0.0063(16) 0.0066(16) C33 0.034(2) 0.040(2) 0.037(2) -0.0187(18) -0.0012(17) 0.0051(17) C34 0.033(2) 0.051(2) 0.0303(19) -0.0193(18) -0.0020(17) -0.0007(18) C35 0.040(2) 0.048(2) 0.047(2) -0.033(2) 0.0027(19) -0.0028(19) C36 0.042(2) 0.036(2) 0.0305(19) -0.0117(17) -0.0011(17) -0.0028(17) N1 0.0310(18) 0.050(2) 0.0285(16) -0.0198(15) -0.0020(13) -0.0002(15) N2 0.0353(18) 0.047(2) 0.0298(16) -0.0180(15) -0.0046(14) -0.0014(15) N3 0.0334(18) 0.057(2) 0.0334(17) -0.0266(16) -0.0009(14) -0.0054(16) N4 0.037(2) 0.058(2) 0.0402(18) -0.0312(17) -0.0002(15) -0.0027(16) N5 0.0388(19) 0.0398(18) 0.0368(17) -0.0207(15) -0.0015(15) -0.0033(15) N6 0.0367(19) 0.0372(18) 0.0364(17) -0.0201(15) -0.0028(14) -0.0011(14) N7 0.041(2) 0.060(2) 0.0375(18) -0.0301(17) -0.0037(16) -0.0008(17) N8 0.0375(19) 0.049(2) 0.0409(19) -0.0269(17) 0.0033(15) -0.0060(16) N9 0.0351(18) 0.0376(18) 0.0363(17) -0.0186(15) -0.0008(14) -0.0004(14) N10 0.0325(18) 0.049(2) 0.0337(17) -0.0217(15) -0.0020(14) -0.0029(15) N11 0.0335(18) 0.0398(18) 0.0386(17) -0.0213(15) 0.0004(15) -0.0019(14) N12 0.0366(19) 0.0425(19) 0.0307(16) -0.0149(15) 0.0025(14) -0.0029(15) N13 0.0352(18) 0.0422(19) 0.0362(17) -0.0241(15) -0.0015(14) -0.0020(15) N14 0.0330(18) 0.0460(19) 0.0364(17) -0.0225(15) -0.0002(14) -0.0076(15) N15 0.040(2) 0.050(2) 0.0390(18) -0.0272(17) 0.0033(16) -0.0043(16) N16 0.046(2) 0.057(2) 0.0400(19) -0.0272(18) -0.0077(17) -0.0002(17) N17 0.0344(18) 0.0433(19) 0.0325(16) -0.0178(15) -0.0044(14) -0.0043(15) N18 0.0334(18) 0.0446(19) 0.0322(16) -0.0213(15) -0.0057(14) 0.0001(14) N19 0.045(2) 0.049(2) 0.0370(18) -0.0250(16) -0.0044(16) -0.0010(16) N20 0.0387(19) 0.049(2) 0.0330(17) -0.0230(16) -0.0036(15) -0.0008(15) N21 0.042(2) 0.0424(19) 0.0309(17) -0.0177(15) 0.0023(15) -0.0052(15) N22 0.0402(19) 0.046(2) 0.0354(17) -0.0241(16) 0.0023(15) -0.0070(15) N23 0.0322(18) 0.052(2) 0.0362(17) -0.0256(16) -0.0003(14) -0.0016(15) N24 0.0320(18) 0.0459(19) 0.0316(16) -0.0185(15) 0.0017(14) 0.0002(15) O1 0.0412(16) 0.0502(17) 0.0310(14) -0.0256(13) -0.0011(12) -0.0013(13) O2 0.0509(18) 0.0434(16) 0.0399(15) -0.0282(14) -0.0045(13) 0.0015(13) O3 0.0445(17) 0.0459(17) 0.0421(15) -0.0254(14) -0.0058(13) 0.0016(13) O4 0.0467(19) 0.068(2) 0.0550(19) -0.0427(17) 0.0030(15) -0.0023(16) O5 0.054(2) 0.091(3) 0.0444(18) -0.0387(18) 0.0051(16) 0.0079(18) O6 0.0460(18) 0.072(2) 0.0434(17) -0.0361(16) 0.0058(14) -0.0085(15) O7 0.0367(16) 0.0529(17) 0.0388(15) -0.0302(14) -0.0046(12) 0.0044(13) O8 0.0453(17) 0.0466(17) 0.0368(15) -0.0222(13) -0.0121(13) 0.0011(13) O9 0.0540(19) 0.0583(19) 0.0350(15) -0.0250(14) -0.0065(14) -0.0057(15) O10 0.068(2) 0.075(2) 0.0383(17) -0.0287(17) 0.0007(16) -0.0017(18) O11 0.0486(19) 0.072(2) 0.0390(16) -0.0322(16) -0.0014(14) -0.0011(16) O12 0.0445(18) 0.070(2) 0.0508(18) -0.0428(17) 0.0107(15) -0.0104(15) _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 O1W Dy1 2.375(3) . ? O2W Dy1 2.363(3) . ? O3W Dy1 2.402(3) . ? O4W Dy1 2.401(3) . ? Dy1 O7 2.339(3) . ? Dy1 O1 2.344(3) . ? Dy1 O8 2.345(3) . ? Dy1 O2 2.351(3) . ? Cl1 Cd1 2.477(2) . ? Cl2 Cd1 2.4433(19) . ? Cl3 Cd1 2.4410(18) . ? Cl4 Cd1 2.389(3) . ? C1 O1 1.249(5) . ? C1 N2 1.344(5) . ? C1 N1 1.356(5) . ? C2 N3 1.447(5) . ? C2 N1 1.447(5) . ? C2 C3 1.550(6) . ? C2 H2 0.9900 . ? C3 N4 1.437(5) . ? C3 N2 1.451(5) . ? C3 H3 0.9900 . ? C4 O4 1.220(5) . ? C4 N4 1.362(6) . ? C4 N3 1.379(6) . ? C5 N5 1.438(5) . ? C5 N2 1.452(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.440(6) . ? C6 N7 1.463(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.226(5) . ? C7 N6 1.341(5) . ? C7 N5 1.365(5) . ? C8 N7 1.451(5) . ? C8 N5 1.453(5) . ? C8 C9 1.528(6) . ? C8 H8 0.9900 . ? C9 N8 1.453(5) . ? C9 N6 1.466(5) . ? C9 H9 0.9900 . ? C10 O5 1.227(5) . ? C10 N8 1.359(6) . ? C10 N7 1.363(6) . ? C11 N6 1.448(5) . ? C11 N9 1.455(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.435(6) . ? C12 N11 1.456(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.225(5) . ? C13 N9 1.349(5) . ? C13 N10 1.369(5) . ? C14 N11 1.443(5) . ? C14 N9 1.447(5) . ? C14 C15 1.547(6) . ? C14 H14 0.9900 . ? C15 N10 1.455(5) . ? C15 N12 1.462(5) . ? C15 H15 0.9900 . ? C16 O6 1.229(5) . ? C16 N12 1.359(6) . ? C16 N11 1.369(5) . ? C17 N3 1.439(6) 2_767 ? C17 N10 1.444(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N1 1.437(6) . ? C18 N12 1.452(5) 2_767 ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O7 1.232(5) . ? C19 N13 1.349(5) . ? C19 N14 1.356(5) . ? C20 N15 1.441(5) . ? C20 N13 1.466(5) . ? C20 C21 1.542(6) . ? C20 H20 0.9900 . ? C21 N16 1.451(5) . ? C21 N14 1.457(5) . ? C21 H21 0.9900 . ? C22 O10 1.219(5) . ? C22 N15 1.361(6) . ? C22 N16 1.368(6) . ? C23 N14 1.427(5) . ? C23 N17 1.448(5) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N19 1.426(6) . ? C24 N16 1.455(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O8 1.237(5) . ? C25 N17 1.349(5) . ? C25 N18 1.361(5) . ? C26 N17 1.436(5) . ? C26 N19 1.466(5) . ? C26 C27 1.548(6) . ? C26 H26 0.9900 . ? C27 N20 1.456(5) . ? C27 N18 1.462(5) . ? C27 H27 0.9900 . ? C28 O11 1.225(5) . ? C28 N20 1.350(6) . ? C28 N19 1.367(6) . ? C29 N18 1.434(5) . ? C29 N21 1.445(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N20 1.443(5) . ? C30 N23 1.454(6) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O9 1.226(5) . ? C31 N21 1.365(6) . ? C31 N22 1.367(5) . ? C32 N21 1.449(5) . ? C32 N23 1.459(5) . ? C32 C33 1.547(6) . ? C32 H32 0.9900 . ? C33 N24 1.449(5) . ? C33 N22 1.453(5) . ? C33 H33 0.9900 . ? C34 O12 1.214(5) . ? C34 N23 1.359(5) . ? C34 N24 1.377(6) . ? C35 N15 1.441(6) . ? C35 N22 1.446(6) 2_668 ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N13 1.439(6) . ? C36 N24 1.455(5) 2_668 ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? N3 C17 1.439(6) 2_767 ? N12 C18 1.452(5) 2_767 ? N22 C35 1.446(6) 2_668 ? N24 C36 1.455(5) 2_668 ? 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 Dy1 O1 126.55(10) . . ? O7 Dy1 O8 76.74(10) . . ? O1 Dy1 O8 151.39(10) . . ? O7 Dy1 O2 151.13(10) . . ? O1 Dy1 O2 76.96(10) . . ? O8 Dy1 O2 87.57(10) . . ? O7 Dy1 O2W 70.85(10) . . ? O1 Dy1 O2W 73.64(10) . . ? O8 Dy1 O2W 104.19(11) . . ? O2 Dy1 O2W 137.33(10) . . ? O7 Dy1 O1W 72.76(10) . . ? O1 Dy1 O1W 70.78(10) . . ? O8 Dy1 O1W 137.33(10) . . ? O2 Dy1 O1W 105.51(11) . . ? O2W Dy1 O1W 93.24(12) . . ? O7 Dy1 O4W 123.27(11) . . ? O1 Dy1 O4W 79.74(11) . . ? O8 Dy1 O4W 72.71(11) . . ? O2 Dy1 O4W 72.89(11) . . ? O2W Dy1 O4W 71.99(11) . . ? O1W Dy1 O4W 149.84(10) . . ? O7 Dy1 O3W 80.03(11) . . ? O1 Dy1 O3W 122.68(11) . . ? O8 Dy1 O3W 73.30(11) . . ? O2 Dy1 O3W 72.24(11) . . ? O2W Dy1 O3W 150.39(11) . . ? O1W Dy1 O3W 72.62(11) . . ? O4W Dy1 O3W 131.59(11) . . ? Cl4 Cd1 Cl3 110.77(14) . . ? Cl4 Cd1 Cl2 113.54(19) . . ? Cl3 Cd1 Cl2 113.33(7) . . ? Cl4 Cd1 Cl1 107.50(14) . . ? Cl3 Cd1 Cl1 106.38(9) . . ? Cl2 Cd1 Cl1 104.71(7) . . ? O1 C1 N2 125.2(4) . . ? O1 C1 N1 124.4(4) . . ? N2 C1 N1 110.4(3) . . ? N3 C2 N1 113.8(3) . . ? N3 C2 C3 103.4(3) . . ? N1 C2 C3 103.7(3) . . ? N3 C2 H2 111.8 . . ? N1 C2 H2 111.8 . . ? C3 C2 H2 111.8 . . ? N4 C3 N2 115.4(3) . . ? N4 C3 C2 103.6(3) . . ? N2 C3 C2 102.9(3) . . ? N4 C3 H3 111.4 . . ? N2 C3 H3 111.4 . . ? C2 C3 H3 111.4 . . ? O4 C4 N4 126.4(4) . . ? O4 C4 N3 125.2(4) . . ? N4 C4 N3 108.4(4) . . ? N5 C5 N2 113.0(3) . . ? N5 C5 H5A 109.0 . . ? N2 C5 H5A 109.0 . . ? N5 C5 H5B 109.0 . . ? N2 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N4 C6 N7 114.0(4) . . ? N4 C6 H6A 108.7 . . ? N7 C6 H6A 108.7 . . ? N4 C6 H6B 108.7 . . ? N7 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? O2 C7 N6 125.7(4) . . ? O2 C7 N5 125.4(4) . . ? N6 C7 N5 108.9(4) . . ? N7 C8 N5 114.7(3) . . ? N7 C8 C9 103.7(3) . . ? N5 C8 C9 103.2(3) . . ? N7 C8 H8 111.6 . . ? N5 C8 H8 111.6 . . ? C9 C8 H8 111.6 . . ? N8 C9 N6 113.9(3) . . ? N8 C9 C8 103.5(3) . . ? N6 C9 C8 103.4(3) . . ? N8 C9 H9 111.8 . . ? N6 C9 H9 111.8 . . ? C8 C9 H9 111.8 . . ? O5 C10 N8 125.8(4) . . ? O5 C10 N7 125.5(4) . . ? N8 C10 N7 108.7(4) . . ? N6 C11 N9 113.0(3) . . ? N6 C11 H11A 109.0 . . ? N9 C11 H11A 109.0 . . ? N6 C11 H11B 109.0 . . ? N9 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? N8 C12 N11 114.2(3) . . ? N8 C12 H12A 108.7 . . ? N11 C12 H12A 108.7 . . ? N8 C12 H12B 108.7 . . ? N11 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? O3 C13 N9 126.6(4) . . ? O3 C13 N10 125.1(4) . . ? N9 C13 N10 108.3(4) . . ? N11 C14 N9 114.5(3) . . ? N11 C14 C15 103.8(3) . . ? N9 C14 C15 102.9(3) . . ? N11 C14 H14 111.7 . . ? N9 C14 H14 111.7 . . ? C15 C14 H14 111.7 . . ? N10 C15 N12 113.6(3) . . ? N10 C15 C14 103.2(3) . . ? N12 C15 C14 102.4(3) . . ? N10 C15 H15 112.3 . . ? N12 C15 H15 112.3 . . ? C14 C15 H15 112.3 . . ? O6 C16 N12 126.4(4) . . ? O6 C16 N11 125.7(4) . . ? N12 C16 N11 108.0(3) . . ? N3 C17 N10 113.5(3) 2_767 . ? N3 C17 H17A 108.9 2_767 . ? N10 C17 H17A 108.9 . . ? N3 C17 H17B 108.9 2_767 . ? N10 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? N1 C18 N12 114.0(3) . 2_767 ? N1 C18 H18A 108.7 . . ? N12 C18 H18A 108.7 2_767 . ? N1 C18 H18B 108.7 . . ? N12 C18 H18B 108.7 2_767 . ? H18A C18 H18B 107.6 . . ? O7 C19 N13 124.9(4) . . ? O7 C19 N14 125.5(4) . . ? N13 C19 N14 109.6(3) . . ? N15 C20 N13 113.9(3) . . ? N15 C20 C21 103.7(3) . . ? N13 C20 C21 103.1(3) . . ? N15 C20 H20 111.8 . . ? N13 C20 H20 111.8 . . ? C21 C20 H20 111.8 . . ? N16 C21 N14 114.3(3) . . ? N16 C21 C20 102.9(3) . . ? N14 C21 C20 103.3(3) . . ? N16 C21 H21 111.9 . . ? N14 C21 H21 111.9 . . ? C20 C21 H21 111.9 . . ? O10 C22 N15 126.5(4) . . ? O10 C22 N16 125.4(4) . . ? N15 C22 N16 108.0(4) . . ? N14 C23 N17 113.9(3) . . ? N14 C23 H23A 108.8 . . ? N17 C23 H23A 108.8 . . ? N14 C23 H23B 108.8 . . ? N17 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? N19 C24 N16 113.9(4) . . ? N19 C24 H24A 108.8 . . ? N16 C24 H24A 108.8 . . ? N19 C24 H24B 108.8 . . ? N16 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? O8 C25 N17 126.2(4) . . ? O8 C25 N18 124.1(4) . . ? N17 C25 N18 109.7(3) . . ? N17 C26 N19 115.1(3) . . ? N17 C26 C27 103.2(3) . . ? N19 C26 C27 103.5(3) . . ? N17 C26 H26 111.5 . . ? N19 C26 H26 111.5 . . ? C27 C26 H26 111.5 . . ? N20 C27 N18 114.1(3) . . ? N20 C27 C26 103.0(3) . . ? N18 C27 C26 103.4(3) . . ? N20 C27 H27 111.9 . . ? N18 C27 H27 111.9 . . ? C26 C27 H27 111.9 . . ? O11 C28 N20 126.1(4) . . ? O11 C28 N19 124.4(4) . . ? N20 C28 N19 109.4(4) . . ? N18 C29 N21 113.1(3) . . ? N18 C29 H29A 109.0 . . ? N21 C29 H29A 109.0 . . ? N18 C29 H29B 109.0 . . ? N21 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? N20 C30 N23 113.7(3) . . ? N20 C30 H30A 108.8 . . ? N23 C30 H30A 108.8 . . ? N20 C30 H30B 108.8 . . ? N23 C30 H30B 108.8 . . ? H30A C30 H30B 107.7 . . ? O9 C31 N21 126.0(4) . . ? O9 C31 N22 125.6(4) . . ? N21 C31 N22 108.4(3) . . ? N21 C32 N23 114.5(3) . . ? N21 C32 C33 103.3(3) . . ? N23 C32 C33 102.8(3) . . ? N21 C32 H32 111.9 . . ? N23 C32 H32 111.9 . . ? C33 C32 H32 111.9 . . ? N24 C33 N22 114.7(3) . . ? N24 C33 C32 103.3(3) . . ? N22 C33 C32 103.4(3) . . ? N24 C33 H33 111.6 . . ? N22 C33 H33 111.6 . . ? C32 C33 H33 111.6 . . ? O12 C34 N23 126.1(4) . . ? O12 C34 N24 126.5(4) . . ? N23 C34 N24 107.4(3) . . ? N15 C35 N22 114.5(3) . 2_668 ? N15 C35 H35A 108.6 . . ? N22 C35 H35A 108.6 2_668 . ? N15 C35 H35B 108.6 . . ? N22 C35 H35B 108.6 2_668 . ? H35A C35 H35B 107.6 . . ? N13 C36 N24 114.2(3) . 2_668 ? N13 C36 H36A 108.7 . . ? N24 C36 H36A 108.7 2_668 . ? N13 C36 H36B 108.7 . . ? N24 C36 H36B 108.7 2_668 . ? H36A C36 H36B 107.6 . . ? C1 N1 C18 123.2(3) . . ? C1 N1 C2 111.2(3) . . ? C18 N1 C2 123.8(3) . . ? C1 N2 C5 123.6(3) . . ? C1 N2 C3 111.8(3) . . ? C5 N2 C3 124.2(3) . . ? C4 N3 C17 123.8(3) . 2_767 ? C4 N3 C2 111.9(3) . . ? C17 N3 C2 123.3(4) 2_767 . ? C4 N4 C3 112.7(4) . . ? C4 N4 C6 123.1(4) . . ? C3 N4 C6 124.2(4) . . ? C7 N5 C5 123.7(3) . . ? C7 N5 C8 112.2(3) . . ? C5 N5 C8 123.9(3) . . ? C7 N6 C11 122.5(3) . . ? C7 N6 C9 112.1(3) . . ? C11 N6 C9 123.6(3) . . ? C10 N7 C8 111.7(4) . . ? C10 N7 C6 121.8(4) . . ? C8 N7 C6 125.4(4) . . ? C10 N8 C12 122.3(4) . . ? C10 N8 C9 112.0(4) . . ? C12 N8 C9 125.1(4) . . ? C13 N9 C14 113.4(3) . . ? C13 N9 C11 122.8(3) . . ? C14 N9 C11 122.1(3) . . ? C13 N10 C17 123.2(4) . . ? C13 N10 C15 112.1(3) . . ? C17 N10 C15 122.0(3) . . ? C16 N11 C14 112.6(3) . . ? C16 N11 C12 122.8(3) . . ? C14 N11 C12 122.9(3) . . ? C16 N12 C18 123.7(3) . 2_767 ? C16 N12 C15 113.0(3) . . ? C18 N12 C15 122.0(3) 2_767 . ? C19 N13 C36 122.3(3) . . ? C19 N13 C20 111.9(3) . . ? C36 N13 C20 124.0(3) . . ? C19 N14 C23 124.0(3) . . ? C19 N14 C21 111.9(3) . . ? C23 N14 C21 124.1(3) . . ? C22 N15 C20 112.7(4) . . ? C22 N15 C35 122.8(3) . . ? C20 N15 C35 124.0(4) . . ? C22 N16 C21 112.5(4) . . ? C22 N16 C24 122.7(4) . . ? C21 N16 C24 124.2(4) . . ? C25 N17 C26 112.7(3) . . ? C25 N17 C23 123.3(3) . . ? C26 N17 C23 124.0(3) . . ? C25 N18 C29 122.7(3) . . ? C25 N18 C27 110.8(3) . . ? C29 N18 C27 123.2(3) . . ? C28 N19 C24 122.9(4) . . ? C28 N19 C26 111.2(4) . . ? C24 N19 C26 125.6(4) . . ? C28 N20 C30 122.6(3) . . ? C28 N20 C27 112.6(3) . . ? C30 N20 C27 124.4(3) . . ? C31 N21 C32 112.6(3) . . ? C31 N21 C29 123.1(3) . . ? C32 N21 C29 123.6(3) . . ? C31 N22 C35 122.6(3) . 2_668 ? C31 N22 C33 112.3(3) . . ? C35 N22 C33 123.1(3) 2_668 . ? C34 N23 C32 113.3(4) . . ? C34 N23 C30 121.3(3) . . ? C32 N23 C30 123.0(3) . . ? C34 N24 C33 112.9(3) . . ? C34 N24 C36 122.8(3) . 2_668 ? C33 N24 C36 123.0(3) . 2_668 ? C1 O1 Dy1 157.1(3) . . ? C7 O2 Dy1 155.9(3) . . ? C19 O7 Dy1 156.8(3) . . ? C25 O8 Dy1 155.0(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.699 _refine_diff_density_min -0.817 _refine_diff_density_rms 0.099 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.015 0.000 -0.001 1088 473 ' ' 2 0.000 0.500 1.000 97 23 ' ' 3 0.500 0.500 0.500 97 20 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 902610' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p211 #TrackingRef 'submit-211.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H138 Cd Cl5 Ho N24 O63' _chemical_formula_weight 2370.28 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ho Ho -0.2175 4.6783 '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 15.135(3) _cell_length_b 15.617(3) _cell_length_c 17.079(4) _cell_angle_alpha 64.870(8) _cell_angle_beta 80.916(8) _cell_angle_gamma 81.719(8) _cell_volume 3595.4(13) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2452 _exptl_absorpt_coefficient_mu 1.729 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7576 _exptl_absorpt_correction_T_max 0.8064 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42765 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0695 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 26.00 _reflns_number_total 13863 _reflns_number_gt 9346 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.2000P)^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 13863 _refine_ls_number_parameters 750 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1497 _refine_ls_R_factor_gt 0.1247 _refine_ls_wR_factor_ref 0.3823 _refine_ls_wR_factor_gt 0.3566 _refine_ls_goodness_of_fit_ref 1.436 _refine_ls_restrained_S_all 1.436 _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 Cl5 Cl 1.01248(18) 0.1972(2) 0.9559(2) 0.0444(8) Uani 1 1 d . . . Cl1 Cl 1.4877(2) -0.2408(3) 0.6507(3) 0.0663(11) Uani 1 1 d . . . Cl2 Cl 1.3757(2) -0.4686(3) 0.6953(4) 0.0804(15) Uani 1 1 d . . . Cl3 Cl 1.6481(2) -0.4698(4) 0.6627(4) 0.100(2) Uani 1 1 d . . . Cl4 Cl 1.5103(10) -0.3290(8) 0.4606(4) 0.235(8) Uani 1 1 d . . . Cd1 Cd 1.50566(6) -0.38116(7) 0.61544(6) 0.0520(3) Uani 1 1 d . . . O1W O 0.7396(4) -0.2351(5) 0.8867(4) 0.0225(14) Uani 1 1 d . . . O2W O 0.9330(4) -0.1341(5) 0.8562(4) 0.0228(15) Uani 1 1 d . . . O3W O 0.8954(4) 0.0165(5) 0.6974(4) 0.0232(15) Uani 1 1 d . . . O4W O 0.6324(4) -0.0655(5) 0.8363(4) 0.0270(16) Uani 1 1 d . . . Ho1 Ho 0.79115(5) -0.08430(5) 0.80612(4) 0.0550(3) Uani 1 1 d . . . C1 C 0.7496(5) 0.1314(7) 0.8260(5) 0.0146(18) Uani 1 1 d . . . C2 C 0.7076(5) 0.2764(6) 0.8397(6) 0.0124(17) Uani 1 1 d . . . H2 H 0.7292 0.3373 0.7959 0.015 Uiso 1 1 calc R . . C3 C 0.7775(5) 0.2179(6) 0.9033(5) 0.0123(17) Uani 1 1 d . . . H3 H 0.8313 0.2518 0.8937 0.015 Uiso 1 1 calc R . . C4 C 0.6448(7) 0.2476(7) 0.9810(6) 0.023(2) Uani 1 1 d . . . C5 C 0.8621(5) 0.0527(6) 0.9306(5) 0.0137(17) Uani 1 1 d . . . H5A H 0.9108 0.0775 0.9442 0.016 Uiso 1 1 calc R . . H5B H 0.8882 0.0213 0.8923 0.016 Uiso 1 1 calc R . . C6 C 0.7676(7) 0.1553(7) 1.0696(6) 0.023(2) Uani 1 1 d . . . H6A H 0.8313 0.1666 1.0576 0.028 Uiso 1 1 calc R . . H6B H 0.7389 0.1857 1.1081 0.028 Uiso 1 1 calc R . . C7 C 0.7851(5) -0.0925(6) 1.0156(5) 0.0110(17) Uani 1 1 d . . . C8 C 0.8204(6) -0.0167(7) 1.0962(5) 0.0164(18) Uani 1 1 d . . . H8 H 0.8822 -0.0156 1.1077 0.020 Uiso 1 1 calc R . . C9 C 0.7798(5) -0.1120(7) 1.1581(5) 0.0146(18) Uani 1 1 d . . . H9 H 0.8216 -0.1561 1.1997 0.017 Uiso 1 1 calc R . . C10 C 0.6880(5) 0.0133(8) 1.1777(6) 0.020(2) Uani 1 1 d . . . C11 C 0.7417(5) -0.2471(7) 1.1242(5) 0.0157(18) Uani 1 1 d . . . H11A H 0.7776 -0.2879 1.1718 0.019 Uiso 1 1 calc R . . H11B H 0.7610 -0.2654 1.0754 0.019 Uiso 1 1 calc R . . C12 C 0.6470(6) -0.1437(8) 1.2748(5) 0.020(2) Uani 1 1 d . . . H12A H 0.6134 -0.1087 1.3076 0.024 Uiso 1 1 calc R . . H12B H 0.6879 -0.1927 1.3129 0.024 Uiso 1 1 calc R . . C13 C 0.5961(6) -0.2840(6) 1.1050(6) 0.0147(17) Uani 1 1 d . . . C14 C 0.6022(6) -0.2749(7) 1.2382(5) 0.0174(19) Uani 1 1 d . . . H14 H 0.6359 -0.3238 1.2850 0.021 Uiso 1 1 calc R . . C15 C 0.5124(6) -0.3073(6) 1.2399(5) 0.0132(17) Uani 1 1 d . . . H15 H 0.5035 -0.3707 1.2875 0.016 Uiso 1 1 calc R . . C16 C 0.4927(5) -0.1686(7) 1.2623(5) 0.0140(18) Uani 1 1 d . . . C17 C 0.4489(6) -0.3507(7) 1.1341(6) 0.0180(19) Uani 1 1 d . . . H17A H 0.4772 -0.3709 1.0883 0.022 Uiso 1 1 calc R . . H17B H 0.4314 -0.4076 1.1853 0.022 Uiso 1 1 calc R . . C18 C 0.3549(5) -0.2410(7) 1.2757(5) 0.0146(17) Uani 1 1 d . . . H18A H 0.3312 -0.2016 1.3075 0.018 Uiso 1 1 calc R . . H18B H 0.3444 -0.3069 1.3147 0.018 Uiso 1 1 calc R . . C19 C 0.7111(5) -0.0375(6) 0.6106(5) 0.0100(16) Uani 1 1 d . . . C20 C 0.6637(5) 0.0056(7) 0.4754(5) 0.017(2) Uani 1 1 d . . . H20 H 0.6013 0.0314 0.4632 0.020 Uiso 1 1 calc R . . C21 C 0.6711(5) -0.1029(7) 0.5222(5) 0.0144(18) Uani 1 1 d . . . H21 H 0.6133 -0.1295 0.5293 0.017 Uiso 1 1 calc R . . C22 C 0.7646(6) -0.0566(7) 0.3910(6) 0.019(2) Uani 1 1 d . . . C23 C 0.7136(6) -0.2105(7) 0.6748(6) 0.0180(19) Uani 1 1 d . . . H23A H 0.6723 -0.2524 0.6731 0.022 Uiso 1 1 calc R . . H23B H 0.6983 -0.2041 0.7302 0.022 Uiso 1 1 calc R . . C24 C 0.7708(6) -0.2305(7) 0.4808(6) 0.021(2) Uani 1 1 d . . . H24A H 0.7206 -0.2701 0.5091 0.025 Uiso 1 1 calc R . . H24B H 0.7902 -0.2341 0.4246 0.025 Uiso 1 1 calc R . . C25 C 0.8720(6) -0.2407(6) 0.7073(5) 0.0152(18) Uani 1 1 d . . . C26 C 0.8362(6) -0.3164(7) 0.6258(6) 0.021(2) Uani 1 1 d . . . H26 H 0.8001 -0.3714 0.6460 0.025 Uiso 1 1 calc R . . C27 C 0.9342(6) -0.3471(6) 0.6486(5) 0.0121(17) Uani 1 1 d . . . H27 H 0.9442 -0.4164 0.6827 0.014 Uiso 1 1 calc R . . C28 C 0.9327(6) -0.2697(7) 0.4966(6) 0.021(2) Uani 1 1 d . . . C29 C 1.0209(5) -0.3140(7) 0.7488(5) 0.0145(18) Uani 1 1 d . . . H29A H 1.0016 -0.2955 0.7974 0.017 Uiso 1 1 calc R . . H29B H 1.0373 -0.3826 0.7733 0.017 Uiso 1 1 calc R . . C30 C 1.0806(6) -0.3414(7) 0.5499(6) 0.0204(19) Uani 1 1 d . . . H30A H 1.0938 -0.4074 0.5903 0.025 Uiso 1 1 calc R . . H30B H 1.0956 -0.3378 0.4907 0.025 Uiso 1 1 calc R . . C31 C 1.1287(5) -0.1945(8) 0.7118(6) 0.019(2) Uani 1 1 d . . . C32 C 1.1668(6) -0.3009(7) 0.6458(5) 0.0163(18) Uani 1 1 d . . . H32 H 1.1868 -0.3687 0.6782 0.020 Uiso 1 1 calc R . . C33 C 1.2435(5) -0.2384(6) 0.6210(5) 0.0133(17) Uani 1 1 d . . . H33 H 1.3004 -0.2759 0.6413 0.016 Uiso 1 1 calc R . . C34 C 1.1885(6) -0.2211(6) 0.4945(5) 0.0154(18) Uani 1 1 d . . . C35 C 1.2673(6) -0.1168(7) 0.6782(5) 0.0162(18) Uani 1 1 d . . . H35A H 1.3269 -0.1509 0.6885 0.019 Uiso 1 1 calc R . . H35B H 1.2420 -0.1070 0.7306 0.019 Uiso 1 1 calc R . . C36 C 0.6803(5) 0.1332(6) 0.5268(5) 0.0126(17) Uani 1 1 d . . . H36A H 0.6751 0.1320 0.5852 0.015 Uiso 1 1 calc R . . H36B H 0.6233 0.1621 0.5027 0.015 Uiso 1 1 calc R . . N1 N 0.6949(5) 0.2119(5) 0.7994(4) 0.0126(14) Uani 1 1 d . . . N2 N 0.7983(5) 0.1299(5) 0.8868(5) 0.0146(15) Uani 1 1 d . . . N3 N 0.6298(5) 0.2903(6) 0.8948(5) 0.0209(17) Uani 1 1 d . . . N4 N 0.7267(5) 0.1990(6) 0.9881(5) 0.0226(18) Uani 1 1 d . . . N5 N 0.8184(5) -0.0159(5) 1.0108(4) 0.0136(15) Uani 1 1 d . . . N6 N 0.7594(4) -0.1498(6) 1.0974(4) 0.0135(15) Uani 1 1 d . . . N7 N 0.7594(5) 0.0538(6) 1.1141(5) 0.0221(17) Uani 1 1 d . . . N8 N 0.6984(4) -0.0801(6) 1.2016(4) 0.0138(15) Uani 1 1 d . . . N9 N 0.6483(4) -0.2636(6) 1.1527(4) 0.0147(15) Uani 1 1 d . . . N10 N 0.5139(5) -0.3086(6) 1.1559(5) 0.0181(16) Uani 1 1 d . . . N11 N 0.5827(5) -0.1905(6) 1.2517(5) 0.0162(16) Uani 1 1 d . . . N12 N 0.4500(5) -0.2339(5) 1.2542(4) 0.0124(14) Uani 1 1 d . . . N13 N 0.6940(5) 0.0376(5) 0.5341(4) 0.0129(15) Uani 1 1 d . . . N14 N 0.7000(5) -0.1194(5) 0.6056(4) 0.0144(15) Uani 1 1 d . . . N15 N 0.7236(5) 0.0245(6) 0.3953(4) 0.0153(16) Uani 1 1 d . . . N16 N 0.7400(5) -0.1320(6) 0.4658(5) 0.0188(16) Uani 1 1 d . . . N17 N 0.8048(5) -0.2552(5) 0.6727(5) 0.0125(14) Uani 1 1 d . . . N18 N 0.9459(4) -0.2935(5) 0.6980(4) 0.0119(14) Uani 1 1 d . . . N19 N 0.8451(5) -0.2677(6) 0.5350(5) 0.0219(17) Uani 1 1 d . . . N20 N 0.9857(5) -0.3158(6) 0.5626(5) 0.0182(16) Uani 1 1 d . . . N21 N 1.0990(5) -0.2660(5) 0.6994(4) 0.0140(15) Uani 1 1 d . . . N22 N 1.2119(5) -0.1725(5) 0.6638(5) 0.0153(15) Uani 1 1 d . . . N23 N 1.1367(5) -0.2839(6) 0.5622(5) 0.0174(16) Uani 1 1 d . . . N24 N 1.2491(5) -0.1920(5) 0.5270(4) 0.0136(15) Uani 1 1 d . . . O1 O 0.7546(4) 0.0682(4) 0.8001(4) 0.0180(13) Uani 1 1 d . . . O2 O 0.7777(4) -0.1080(5) 0.9507(4) 0.0158(13) Uani 1 1 d . . . O3 O 0.6167(4) -0.2834(6) 1.0343(4) 0.0290(17) Uani 1 1 d . . . O4 O 0.5925(5) 0.2574(6) 1.0408(5) 0.0344(18) Uani 1 1 d . . . O5 O 0.6303(4) 0.0576(6) 1.2067(5) 0.0276(16) Uani 1 1 d . . . O6 O 0.4549(4) -0.1006(5) 1.2793(4) 0.0191(13) Uani 1 1 d . . . O7 O 0.7318(4) -0.0285(5) 0.6745(4) 0.0205(14) Uani 1 1 d . . . O8 O 0.8631(4) -0.1863(4) 0.7467(4) 0.0141(12) Uani 1 1 d . . . O9 O 1.0910(4) -0.1538(6) 0.7573(5) 0.0278(16) Uani 1 1 d . . . O10 O 0.8142(5) -0.0657(6) 0.3288(4) 0.0277(16) Uani 1 1 d . . . O11 O 0.9583(5) -0.2440(6) 0.4215(4) 0.0331(17) Uani 1 1 d . . . O12 O 1.1827(5) -0.1962(6) 0.4159(4) 0.0261(16) 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 Cl5 0.0293(13) 0.055(2) 0.0524(18) -0.0225(15) -0.0174(12) 0.0012(13) Cl1 0.0312(16) 0.060(2) 0.103(3) -0.025(2) -0.0105(17) -0.0106(15) Cl2 0.0390(18) 0.036(2) 0.148(4) -0.027(2) 0.009(2) -0.0026(15) Cl3 0.0294(17) 0.071(3) 0.119(4) 0.033(3) 0.002(2) 0.0032(17) Cl4 0.369(17) 0.208(10) 0.033(3) -0.009(4) -0.021(5) 0.136(11) Cd1 0.0391(5) 0.0385(6) 0.0438(6) 0.0114(4) 0.0010(4) 0.0056(4) O1W 0.032(4) 0.015(3) 0.022(3) -0.012(3) 0.012(3) -0.006(3) O2W 0.010(3) 0.048(5) 0.014(3) -0.019(3) 0.003(2) 0.003(3) O3W 0.018(3) 0.031(4) 0.016(3) -0.009(3) 0.008(2) 0.000(3) O4W 0.020(3) 0.036(4) 0.015(3) -0.005(3) 0.010(3) 0.000(3) Ho1 0.0566(5) 0.0615(5) 0.0488(5) -0.0261(4) -0.0046(3) -0.0011(3) C1 0.013(4) 0.023(5) 0.004(4) -0.002(4) 0.001(3) -0.001(3) C2 0.014(4) 0.007(4) 0.017(4) -0.006(3) -0.002(3) 0.000(3) C3 0.014(4) 0.013(4) 0.011(4) -0.007(3) 0.001(3) -0.001(3) C4 0.029(5) 0.026(6) 0.017(5) -0.014(4) 0.001(4) 0.001(4) C5 0.012(4) 0.018(5) 0.012(4) -0.008(4) 0.001(3) 0.000(3) C6 0.039(5) 0.025(5) 0.013(4) -0.013(4) -0.020(4) 0.008(4) C7 0.001(3) 0.023(5) 0.010(4) -0.010(4) -0.005(3) 0.010(3) C8 0.021(4) 0.026(5) 0.007(4) -0.010(4) -0.004(3) -0.003(4) C9 0.009(4) 0.032(5) 0.010(4) -0.017(4) -0.002(3) 0.003(3) C10 0.008(4) 0.051(7) 0.014(4) -0.026(5) 0.002(3) -0.007(4) C11 0.014(4) 0.024(5) 0.011(4) -0.011(4) -0.005(3) 0.007(3) C12 0.013(4) 0.045(6) 0.004(4) -0.011(4) -0.004(3) -0.006(4) C13 0.018(4) 0.013(5) 0.014(4) -0.008(4) 0.005(3) -0.004(3) C14 0.016(4) 0.023(5) 0.006(4) -0.003(4) 0.002(3) 0.004(4) C15 0.021(4) 0.008(4) 0.007(4) -0.001(3) 0.001(3) 0.002(3) C16 0.013(4) 0.025(5) 0.004(4) -0.008(4) -0.006(3) 0.007(3) C17 0.016(4) 0.018(5) 0.025(5) -0.015(4) -0.004(4) 0.005(3) C18 0.016(4) 0.017(5) 0.009(4) -0.005(3) 0.006(3) -0.001(3) C19 0.004(3) 0.018(5) 0.006(4) -0.005(3) 0.001(3) 0.004(3) C20 0.008(4) 0.046(6) 0.004(4) -0.017(4) -0.003(3) -0.003(4) C21 0.014(4) 0.027(5) 0.010(4) -0.014(4) -0.006(3) -0.001(3) C22 0.016(4) 0.029(6) 0.012(4) -0.007(4) -0.004(3) -0.008(4) C23 0.013(4) 0.025(5) 0.014(4) -0.007(4) -0.002(3) -0.002(4) C24 0.031(5) 0.017(5) 0.021(5) -0.010(4) -0.014(4) 0.001(4) C25 0.023(4) 0.013(5) 0.007(4) -0.003(3) 0.005(3) -0.008(4) C26 0.026(5) 0.019(5) 0.024(5) -0.018(4) 0.007(4) -0.003(4) C27 0.023(4) 0.008(4) 0.008(4) -0.007(3) 0.007(3) -0.008(3) C28 0.028(5) 0.024(5) 0.023(5) -0.025(4) 0.002(4) 0.006(4) C29 0.012(4) 0.024(5) 0.009(4) -0.010(4) 0.004(3) -0.001(3) C30 0.027(5) 0.022(5) 0.016(4) -0.015(4) 0.006(4) 0.003(4) C31 0.010(4) 0.039(6) 0.010(4) -0.016(4) 0.002(3) 0.004(4) C32 0.024(4) 0.019(5) 0.007(4) -0.011(4) 0.002(3) 0.011(4) C33 0.013(4) 0.016(5) 0.006(4) -0.005(3) 0.002(3) 0.010(3) C34 0.022(4) 0.012(4) 0.011(4) -0.005(3) 0.000(3) 0.003(3) C35 0.023(4) 0.020(5) 0.005(4) -0.004(4) -0.005(3) -0.002(4) C36 0.011(4) 0.015(5) 0.008(4) -0.003(3) 0.005(3) 0.000(3) N1 0.016(3) 0.014(4) 0.013(3) -0.008(3) -0.003(3) -0.005(3) N2 0.020(4) 0.016(4) 0.013(3) -0.013(3) 0.001(3) 0.004(3) N3 0.030(4) 0.024(5) 0.012(4) -0.013(3) 0.006(3) -0.004(3) N4 0.026(4) 0.034(5) 0.014(4) -0.017(4) -0.007(3) 0.008(4) N5 0.023(4) 0.020(4) 0.002(3) -0.009(3) 0.005(3) -0.005(3) N6 0.014(3) 0.024(4) 0.003(3) -0.009(3) 0.001(3) 0.006(3) N7 0.026(4) 0.023(5) 0.018(4) -0.011(3) 0.007(3) -0.007(3) N8 0.013(3) 0.024(4) 0.009(3) -0.012(3) 0.005(3) -0.007(3) N9 0.010(3) 0.023(4) 0.009(3) -0.009(3) 0.008(3) 0.000(3) N10 0.015(3) 0.025(4) 0.016(4) -0.011(3) 0.006(3) -0.006(3) N11 0.013(3) 0.030(5) 0.012(3) -0.016(3) 0.004(3) -0.006(3) N12 0.017(3) 0.011(4) 0.007(3) -0.003(3) -0.001(3) -0.002(3) N13 0.019(3) 0.014(4) 0.011(3) -0.010(3) -0.005(3) 0.003(3) N14 0.021(4) 0.016(4) 0.004(3) -0.002(3) -0.005(3) 0.001(3) N15 0.016(3) 0.025(4) 0.005(3) -0.007(3) 0.006(3) -0.007(3) N16 0.017(4) 0.028(5) 0.016(4) -0.015(4) 0.000(3) 0.001(3) N17 0.017(3) 0.014(4) 0.014(3) -0.014(3) -0.004(3) 0.004(3) N18 0.015(3) 0.017(4) 0.011(3) -0.015(3) 0.002(3) 0.002(3) N19 0.026(4) 0.025(5) 0.019(4) -0.013(4) -0.011(3) 0.008(3) N20 0.022(4) 0.025(4) 0.013(4) -0.014(3) 0.005(3) -0.005(3) N21 0.015(3) 0.018(4) 0.011(3) -0.012(3) 0.007(3) 0.001(3) N22 0.022(4) 0.016(4) 0.014(4) -0.013(3) 0.009(3) -0.008(3) N23 0.026(4) 0.025(4) 0.009(3) -0.014(3) 0.004(3) -0.008(3) N24 0.018(3) 0.016(4) 0.007(3) -0.008(3) 0.003(3) 0.001(3) O1 0.031(3) 0.014(3) 0.012(3) -0.009(3) -0.002(2) 0.004(3) O2 0.025(3) 0.021(3) 0.009(3) -0.015(3) 0.005(2) -0.004(3) O3 0.025(3) 0.047(5) 0.022(4) -0.024(3) 0.015(3) -0.012(3) O4 0.031(4) 0.055(5) 0.018(4) -0.023(4) 0.007(3) 0.010(3) O5 0.023(3) 0.038(4) 0.034(4) -0.029(4) 0.006(3) -0.005(3) O6 0.024(3) 0.021(4) 0.018(3) -0.015(3) -0.006(3) 0.004(3) O7 0.030(3) 0.025(4) 0.016(3) -0.018(3) -0.008(3) 0.005(3) O8 0.018(3) 0.013(3) 0.017(3) -0.013(3) 0.000(2) 0.003(2) O9 0.024(3) 0.039(5) 0.031(4) -0.028(4) 0.007(3) -0.004(3) O10 0.028(3) 0.046(5) 0.019(3) -0.025(3) 0.004(3) -0.003(3) O11 0.052(5) 0.032(4) 0.016(4) -0.012(3) -0.005(3) 0.004(4) O12 0.030(4) 0.041(4) 0.011(3) -0.016(3) -0.005(3) 0.004(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 Cl1 Cd1 2.478(5) . ? Cl2 Cd1 2.437(4) . ? Cl3 Cd1 2.441(4) . ? Cl4 Cd1 2.407(6) . ? O1W Ho1 2.342(6) . ? O2W Ho1 2.341(6) . ? O3W Ho1 2.392(6) . ? O4W Ho1 2.380(6) . ? Ho1 O8 2.298(6) . ? Ho1 O2 2.315(5) . ? Ho1 O7 2.318(6) . ? Ho1 O1 2.328(6) . ? C1 O1 1.229(11) . ? C1 N1 1.344(12) . ? C1 N2 1.356(11) . ? C2 N3 1.438(11) . ? C2 N1 1.487(11) . ? C2 C3 1.542(11) . ? C2 H2 0.9900 . ? C3 N4 1.458(11) . ? C3 N2 1.497(11) . ? C3 H3 0.9900 . ? C4 O4 1.239(12) . ? C4 N4 1.351(13) . ? C4 N3 1.376(12) . ? C5 N2 1.439(11) . ? C5 N5 1.460(11) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.452(13) . ? C6 N4 1.460(11) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.255(10) . ? C7 N6 1.330(11) . ? C7 N5 1.331(12) . ? C8 N7 1.436(12) . ? C8 N5 1.459(10) . ? C8 C9 1.559(13) . ? C8 H8 0.9900 . ? C9 N8 1.471(11) . ? C9 N6 1.483(10) . ? C9 H9 0.9900 . ? C10 O5 1.211(11) . ? C10 N8 1.330(13) . ? C10 N7 1.410(12) . ? C11 N6 1.442(13) . ? C11 N9 1.443(11) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.420(11) . ? C12 N11 1.485(11) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.194(11) . ? C13 N9 1.374(11) . ? C13 N10 1.400(11) . ? C14 N11 1.416(12) . ? C14 N9 1.464(10) . ? C14 C15 1.510(12) . ? C14 H14 0.9900 . ? C15 N10 1.439(11) . ? C15 N12 1.456(11) . ? C15 H15 0.9900 . ? C16 O6 1.255(11) . ? C16 N12 1.346(12) . ? C16 N11 1.358(11) . ? C17 N3 1.421(12) 2_657 ? C17 N10 1.432(11) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.436(10) . ? C18 N1 1.460(10) 2_657 ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O7 1.249(10) . ? C19 N14 1.354(12) . ? C19 N13 1.367(11) . ? C20 N13 1.449(10) . ? C20 N15 1.457(10) . ? C20 C21 1.532(14) . ? C20 H20 0.9900 . ? C21 N16 1.463(11) . ? C21 N14 1.463(10) . ? C21 H21 0.9900 . ? C22 O10 1.248(11) . ? C22 N15 1.353(13) . ? C22 N16 1.362(12) . ? C23 N14 1.424(12) . ? C23 N17 1.456(11) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N19 1.464(11) . ? C24 N16 1.464(13) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O8 1.272(11) . ? C25 N18 1.321(12) . ? C25 N17 1.342(11) . ? C26 N19 1.402(13) . ? C26 N17 1.477(11) . ? C26 C27 1.550(13) . ? C26 H26 0.9900 . ? C27 N18 1.461(10) . ? C27 N20 1.464(11) . ? C27 H27 0.9900 . ? C28 O11 1.186(12) . ? C28 N20 1.364(13) . ? C28 N19 1.386(12) . ? C29 N21 1.441(11) . ? C29 N18 1.454(10) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N23 1.415(12) . ? C30 N20 1.443(12) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O9 1.228(11) . ? C31 N21 1.367(12) . ? C31 N22 1.392(11) . ? C32 N21 1.468(10) . ? C32 N23 1.472(10) . ? C32 C33 1.517(13) . ? C32 H32 0.9900 . ? C33 N24 1.447(10) . ? C33 N22 1.488(11) . ? C33 H33 0.9900 . ? C34 O12 1.243(11) . ? C34 N24 1.361(11) . ? C34 N23 1.373(12) . ? C35 N22 1.405(11) . ? C35 N15 1.463(11) 2_756 ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N13 1.431(12) . ? C36 N24 1.445(11) 2_756 ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? N1 C18 1.460(10) 2_657 ? N3 C17 1.421(12) 2_657 ? N15 C35 1.463(11) 2_756 ? N24 C36 1.445(11) 2_756 ? 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 Cl4 Cd1 Cl2 112.7(4) . . ? Cl4 Cd1 Cl3 109.2(3) . . ? Cl2 Cd1 Cl3 113.13(15) . . ? Cl4 Cd1 Cl1 109.3(3) . . ? Cl2 Cd1 Cl1 104.69(15) . . ? Cl3 Cd1 Cl1 107.59(19) . . ? O8 Ho1 O2 127.0(2) . . ? O8 Ho1 O7 77.4(2) . . ? O2 Ho1 O7 150.7(2) . . ? O8 Ho1 O1 151.0(2) . . ? O2 Ho1 O1 76.7(2) . . ? O7 Ho1 O1 86.6(2) . . ? O8 Ho1 O2W 72.1(2) . . ? O2 Ho1 O2W 71.4(2) . . ? O7 Ho1 O2W 137.3(2) . . ? O1 Ho1 O2W 106.4(2) . . ? O8 Ho1 O1W 70.9(2) . . ? O2 Ho1 O1W 73.9(2) . . ? O7 Ho1 O1W 104.9(2) . . ? O1 Ho1 O1W 137.4(2) . . ? O2W Ho1 O1W 92.7(3) . . ? O8 Ho1 O4W 123.4(2) . . ? O2 Ho1 O4W 79.1(2) . . ? O7 Ho1 O4W 73.1(2) . . ? O1 Ho1 O4W 72.9(2) . . ? O2W Ho1 O4W 149.5(2) . . ? O1W Ho1 O4W 71.7(2) . . ? O8 Ho1 O3W 79.7(2) . . ? O2 Ho1 O3W 122.8(2) . . ? O7 Ho1 O3W 72.8(2) . . ? O1 Ho1 O3W 72.5(2) . . ? O2W Ho1 O3W 72.8(2) . . ? O1W Ho1 O3W 150.1(2) . . ? O4W Ho1 O3W 132.1(2) . . ? O1 C1 N1 125.8(7) . . ? O1 C1 N2 124.9(8) . . ? N1 C1 N2 109.4(8) . . ? N3 C2 N1 113.2(7) . . ? N3 C2 C3 104.2(7) . . ? N1 C2 C3 102.7(6) . . ? N3 C2 H2 112.0 . . ? N1 C2 H2 112.0 . . ? C3 C2 H2 112.0 . . ? N4 C3 N2 111.7(7) . . ? N4 C3 C2 102.7(6) . . ? N2 C3 C2 102.8(6) . . ? N4 C3 H3 112.9 . . ? N2 C3 H3 112.9 . . ? C2 C3 H3 112.9 . . ? O4 C4 N4 126.5(9) . . ? O4 C4 N3 124.4(9) . . ? N4 C4 N3 109.0(8) . . ? N2 C5 N5 110.4(7) . . ? N2 C5 H5A 109.6 . . ? N5 C5 H5A 109.6 . . ? N2 C5 H5B 109.6 . . ? N5 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? N7 C6 N4 112.8(8) . . ? N7 C6 H6A 109.0 . . ? N4 C6 H6A 109.0 . . ? N7 C6 H6B 109.0 . . ? N4 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? O2 C7 N6 124.2(8) . . ? O2 C7 N5 124.0(8) . . ? N6 C7 N5 111.8(7) . . ? N7 C8 N5 114.8(7) . . ? N7 C8 C9 103.7(7) . . ? N5 C8 C9 102.1(6) . . ? N7 C8 H8 111.8 . . ? N5 C8 H8 111.9 . . ? C9 C8 H8 111.8 . . ? N8 C9 N6 112.7(6) . . ? N8 C9 C8 102.5(7) . . ? N6 C9 C8 103.2(6) . . ? N8 C9 H9 112.5 . . ? N6 C9 H9 112.5 . . ? C8 C9 H9 112.5 . . ? O5 C10 N8 127.3(9) . . ? O5 C10 N7 124.5(10) . . ? N8 C10 N7 108.1(8) . . ? N6 C11 N9 113.3(7) . . ? N6 C11 H11A 108.9 . . ? N9 C11 H11A 108.9 . . ? N6 C11 H11B 108.9 . . ? N9 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? N8 C12 N11 113.6(6) . . ? N8 C12 H12A 108.8 . . ? N11 C12 H12A 108.8 . . ? N8 C12 H12B 108.8 . . ? N11 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N9 127.1(8) . . ? O3 C13 N10 125.8(8) . . ? N9 C13 N10 107.1(7) . . ? N11 C14 N9 115.5(7) . . ? N11 C14 C15 105.8(7) . . ? N9 C14 C15 103.9(7) . . ? N11 C14 H14 110.4 . . ? N9 C14 H14 110.4 . . ? C15 C14 H14 110.4 . . ? N10 C15 N12 114.7(7) . . ? N10 C15 C14 104.8(7) . . ? N12 C15 C14 102.0(7) . . ? N10 C15 H15 111.6 . . ? N12 C15 H15 111.6 . . ? C14 C15 H15 111.6 . . ? O6 C16 N12 125.2(7) . . ? O6 C16 N11 126.0(8) . . ? N12 C16 N11 108.8(8) . . ? N3 C17 N10 114.7(8) 2_657 . ? N3 C17 H17A 108.6 2_657 . ? N10 C17 H17A 108.6 . . ? N3 C17 H17B 108.6 2_657 . ? N10 C17 H17B 108.6 . . ? H17A C17 H17B 107.6 . . ? N12 C18 N1 114.3(6) . 2_657 ? N12 C18 H18A 108.7 . . ? N1 C18 H18A 108.7 2_657 . ? N12 C18 H18B 108.7 . . ? N1 C18 H18B 108.7 2_657 . ? H18A C18 H18B 107.6 . . ? O7 C19 N14 127.0(8) . . ? O7 C19 N13 123.3(8) . . ? N14 C19 N13 109.6(7) . . ? N13 C20 N15 113.6(7) . . ? N13 C20 C21 105.1(6) . . ? N15 C20 C21 103.8(7) . . ? N13 C20 H20 111.3 . . ? N15 C20 H20 111.3 . . ? C21 C20 H20 111.3 . . ? N16 C21 N14 113.9(7) . . ? N16 C21 C20 103.1(7) . . ? N14 C21 C20 102.3(6) . . ? N16 C21 H21 112.2 . . ? N14 C21 H21 112.2 . . ? C20 C21 H21 112.2 . . ? O10 C22 N15 127.9(9) . . ? O10 C22 N16 122.8(9) . . ? N15 C22 N16 109.2(7) . . ? N14 C23 N17 114.5(7) . . ? N14 C23 H23A 108.6 . . ? N17 C23 H23A 108.6 . . ? N14 C23 H23B 108.6 . . ? N17 C23 H23B 108.6 . . ? H23A C23 H23B 107.6 . . ? N19 C24 N16 112.2(7) . . ? N19 C24 H24A 109.2 . . ? N16 C24 H24A 109.2 . . ? N19 C24 H24B 109.2 . . ? N16 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? O8 C25 N18 125.4(8) . . ? O8 C25 N17 123.7(8) . . ? N18 C25 N17 110.9(7) . . ? N19 C26 N17 114.2(8) . . ? N19 C26 C27 104.1(7) . . ? N17 C26 C27 101.6(7) . . ? N19 C26 H26 112.1 . . ? N17 C26 H26 112.1 . . ? C27 C26 H26 112.1 . . ? N18 C27 N20 114.1(7) . . ? N18 C27 C26 103.6(7) . . ? N20 C27 C26 102.3(7) . . ? N18 C27 H27 112.1 . . ? N20 C27 H27 112.1 . . ? C26 C27 H27 112.1 . . ? O11 C28 N20 125.0(9) . . ? O11 C28 N19 128.1(9) . . ? N20 C28 N19 106.7(8) . . ? N21 C29 N18 113.6(7) . . ? N21 C29 H29A 108.9 . . ? N18 C29 H29A 108.9 . . ? N21 C29 H29B 108.9 . . ? N18 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? N23 C30 N20 114.7(7) . . ? N23 C30 H30A 108.6 . . ? N20 C30 H30A 108.6 . . ? N23 C30 H30B 108.6 . . ? N20 C30 H30B 108.6 . . ? H30A C30 H30B 107.6 . . ? O9 C31 N21 127.8(8) . . ? O9 C31 N22 123.0(9) . . ? N21 C31 N22 109.3(7) . . ? N21 C32 N23 112.6(7) . . ? N21 C32 C33 105.2(7) . . ? N23 C32 C33 104.4(7) . . ? N21 C32 H32 111.4 . . ? N23 C32 H32 111.4 . . ? C33 C32 H32 111.4 . . ? N24 C33 N22 113.3(7) . . ? N24 C33 C32 103.8(7) . . ? N22 C33 C32 103.5(6) . . ? N24 C33 H33 111.9 . . ? N22 C33 H33 111.9 . . ? C32 C33 H33 111.9 . . ? O12 C34 N24 125.1(8) . . ? O12 C34 N23 125.7(8) . . ? N24 C34 N23 109.2(7) . . ? N22 C35 N15 112.3(7) . 2_756 ? N22 C35 H35A 109.2 . . ? N15 C35 H35A 109.2 2_756 . ? N22 C35 H35B 109.2 . . ? N15 C35 H35B 109.2 2_756 . ? H35A C35 H35B 107.9 . . ? N13 C36 N24 114.0(7) . 2_756 ? N13 C36 H36A 108.7 . . ? N24 C36 H36A 108.7 2_756 . ? N13 C36 H36B 108.7 . . ? N24 C36 H36B 108.7 2_756 . ? H36A C36 H36B 107.6 . . ? C1 N1 C18 121.9(7) . 2_657 ? C1 N1 C2 112.9(6) . . ? C18 N1 C2 123.7(7) 2_657 . ? C1 N2 C5 124.1(7) . . ? C1 N2 C3 112.0(7) . . ? C5 N2 C3 124.0(7) . . ? C4 N3 C17 122.3(8) . 2_657 ? C4 N3 C2 111.4(8) . . ? C17 N3 C2 125.7(7) 2_657 . ? C4 N4 C3 112.0(7) . . ? C4 N4 C6 122.6(8) . . ? C3 N4 C6 123.3(8) . . ? C7 N5 C8 112.4(7) . . ? C7 N5 C5 123.4(7) . . ? C8 N5 C5 123.4(7) . . ? C7 N6 C11 123.6(7) . . ? C7 N6 C9 110.4(7) . . ? C11 N6 C9 123.3(7) . . ? C10 N7 C8 112.1(8) . . ? C10 N7 C6 123.6(8) . . ? C8 N7 C6 124.3(8) . . ? C10 N8 C12 122.4(8) . . ? C10 N8 C9 113.5(7) . . ? C12 N8 C9 122.8(8) . . ? C13 N9 C11 121.7(7) . . ? C13 N9 C14 112.2(7) . . ? C11 N9 C14 125.6(7) . . ? C13 N10 C17 122.6(7) . . ? C13 N10 C15 112.0(7) . . ? C17 N10 C15 123.9(7) . . ? C16 N11 C14 111.3(7) . . ? C16 N11 C12 121.1(7) . . ? C14 N11 C12 125.8(7) . . ? C16 N12 C18 123.1(7) . . ? C16 N12 C15 112.2(7) . . ? C18 N12 C15 123.5(7) . . ? C19 N13 C36 121.9(7) . . ? C19 N13 C20 110.6(7) . . ? C36 N13 C20 124.6(7) . . ? C19 N14 C23 123.2(7) . . ? C19 N14 C21 112.2(7) . . ? C23 N14 C21 124.6(7) . . ? C22 N15 C20 111.9(7) . . ? C22 N15 C35 121.6(7) . 2_756 ? C20 N15 C35 126.1(8) . 2_756 ? C22 N16 C21 111.6(8) . . ? C22 N16 C24 123.0(8) . . ? C21 N16 C24 124.9(8) . . ? C25 N17 C23 124.6(7) . . ? C25 N17 C26 111.6(7) . . ? C23 N17 C26 123.6(7) . . ? C25 N18 C29 123.3(7) . . ? C25 N18 C27 111.9(7) . . ? C29 N18 C27 123.1(7) . . ? C28 N19 C26 113.9(8) . . ? C28 N19 C24 120.0(8) . . ? C26 N19 C24 125.4(8) . . ? C28 N20 C30 124.1(7) . . ? C28 N20 C27 112.8(7) . . ? C30 N20 C27 122.7(7) . . ? C31 N21 C29 123.1(7) . . ? C31 N21 C32 111.2(7) . . ? C29 N21 C32 124.3(7) . . ? C31 N22 C35 121.6(7) . . ? C31 N22 C33 110.6(7) . . ? C35 N22 C33 124.9(7) . . ? C34 N23 C30 122.4(7) . . ? C34 N23 C32 110.3(7) . . ? C30 N23 C32 125.2(8) . . ? C34 N24 C36 123.2(7) . 2_756 ? C34 N24 C33 112.3(7) . . ? C36 N24 C33 123.8(7) 2_756 . ? C1 O1 Ho1 155.7(6) . . ? C7 O2 Ho1 158.3(6) . . ? C19 O7 Ho1 153.4(6) . . ? C25 O8 Ho1 157.6(6) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 5.025 _refine_diff_density_min -1.853 _refine_diff_density_rms 0.352 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 96 51 ' ' 2 -0.058 0.500 0.767 1100 836 ' ' 3 0.500 1.000 0.000 94 45 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 902611' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p212 #TrackingRef 'submit-212.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H92 Cd Cl5 Er N24 O40' _chemical_formula_weight 1958.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 '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 15.0779(8) _cell_length_b 15.6080(8) _cell_length_c 17.0335(9) _cell_angle_alpha 65.006(2) _cell_angle_beta 81.067(2) _cell_angle_gamma 81.602(2) _cell_volume 3574.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.819 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1994 _exptl_absorpt_coefficient_mu 1.763 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6770 _exptl_absorpt_correction_T_max 0.7306 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41068 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 26.00 _reflns_number_total 13768 _reflns_number_gt 11659 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0674P)^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 13768 _refine_ls_number_parameters 749 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.1133 _refine_ls_wR_factor_gt 0.1086 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.004 _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 Cl5 Cl -0.01277(8) 0.80072(10) 0.54475(9) 0.0598(3) Uani 1 1 d . . . O1W O 0.06515(18) 1.1315(2) 0.64412(18) 0.0377(7) Uani 1 1 d . . . O2W O 0.2596(2) 1.2324(2) 0.61535(19) 0.0403(7) Uani 1 1 d . . . O3W O 0.10363(19) 0.9819(2) 0.80254(18) 0.0394(7) Uani 1 1 d . . . O4W O 0.36654(18) 1.0610(2) 0.66416(19) 0.0405(7) Uani 1 1 d . . . Er1 Er 0.207406(11) 1.082301(12) 0.694511(10) 0.02727(7) Uani 1 1 d . . . Cl1 Cl 0.62328(10) 0.47054(11) 0.80222(14) 0.0864(5) Uani 1 1 d . . . Cl2 Cl 0.50968(10) 0.24412(12) 0.85127(13) 0.0847(5) Uani 1 1 d . . . Cl3 Cl 0.4956(3) 0.3297(3) 1.04032(16) 0.261(3) Uani 1 1 d . . . Cl4 Cl 0.35077(11) 0.47168(15) 0.83416(17) 0.1442(12) Uani 1 1 d . . . Cd1 Cd 0.49271(3) 0.38536(3) 0.88651(3) 0.07149(15) Uani 1 1 d . . . C1 C 0.1291(2) 1.2389(3) 0.7925(2) 0.0274(8) Uani 1 1 d . . . C2 C 0.0673(3) 1.3460(3) 0.8518(2) 0.0317(8) Uani 1 1 d . . . H2 H 0.0579 1.4154 0.8175 0.038 Uiso 1 1 calc R . . C3 C 0.1658(3) 1.3139(3) 0.8733(3) 0.0326(8) Uani 1 1 d . . . H3 H 0.2028 1.3682 0.8526 0.039 Uiso 1 1 calc R . . C4 C 0.0683(3) 1.2704(3) 1.0033(3) 0.0380(10) Uani 1 1 d . . . C5 C 0.2870(2) 1.2075(3) 0.8244(2) 0.0307(8) Uani 1 1 d . . . H5A H 0.3014 1.2008 0.7690 0.037 Uiso 1 1 calc R . . H5B H 0.3291 1.2489 0.8258 0.037 Uiso 1 1 calc R . . C6 C 0.2321(3) 1.2266(3) 1.0190(3) 0.0419(10) Uani 1 1 d . . . H6A H 0.2825 1.2658 0.9897 0.050 Uiso 1 1 calc R . . H6B H 0.2143 1.2306 1.0753 0.050 Uiso 1 1 calc R . . C7 C 0.2889(2) 1.0340(3) 0.8894(2) 0.0276(8) Uani 1 1 d . . . C8 C 0.3289(3) 1.0995(3) 0.9779(2) 0.0317(8) Uani 1 1 d . . . H8 H 0.3871 1.1259 0.9701 0.038 Uiso 1 1 calc R . . C9 C 0.3376(3) 0.9909(3) 1.0247(3) 0.0325(9) Uani 1 1 d . . . H9 H 0.4006 0.9654 1.0365 0.039 Uiso 1 1 calc R . . C10 C 0.2379(3) 1.0549(3) 1.1096(3) 0.0356(9) Uani 1 1 d . . . C11 C 0.3201(3) 0.8628(3) 0.9733(3) 0.0317(8) Uani 1 1 d . . . H11A H 0.3254 0.8630 0.9152 0.038 Uiso 1 1 calc R . . H11B H 0.3772 0.8337 0.9980 0.038 Uiso 1 1 calc R . . C12 C 0.2700(3) 0.8814(3) 1.1760(2) 0.0354(9) Uani 1 1 d . . . H12A H 0.3300 0.8470 1.1842 0.042 Uiso 1 1 calc R . . H12B H 0.2471 0.8901 1.2295 0.042 Uiso 1 1 calc R . . C13 C 0.1877(3) 0.7779(3) 0.9939(3) 0.0317(8) Uani 1 1 d . . . C14 C 0.2427(3) 0.7610(3) 1.1210(2) 0.0303(8) Uani 1 1 d . . . H14 H 0.2994 0.7230 1.1421 0.036 Uiso 1 1 calc R . . C15 C 0.1643(3) 0.6978(3) 1.1453(3) 0.0323(9) Uani 1 1 d . . . H15 H 0.1839 0.6299 1.1774 0.039 Uiso 1 1 calc R . . C16 C 0.1298(3) 0.8049(3) 1.2110(2) 0.0308(8) Uani 1 1 d . . . C17 C 0.0785(3) 0.6573(3) 1.0504(3) 0.0355(9) Uani 1 1 d . . . H17A H 0.0925 0.6599 0.9913 0.043 Uiso 1 1 calc R . . H17B H 0.0919 0.5915 1.0913 0.043 Uiso 1 1 calc R . . C18 C 0.0204(3) 0.6872(3) 1.2474(2) 0.0317(8) Uani 1 1 d . . . H18A H 0.0014 0.7060 1.2960 0.038 Uiso 1 1 calc R . . H18B H 0.0364 0.6185 1.2721 0.038 Uiso 1 1 calc R . . C19 C 0.2139(2) 1.0910(3) 0.4860(2) 0.0275(8) Uani 1 1 d . . . C20 C 0.2203(2) 1.1112(3) 0.3431(2) 0.0324(9) Uani 1 1 d . . . H20 H 0.1779 1.1556 0.3019 0.039 Uiso 1 1 calc R . . C21 C 0.1791(3) 1.0174(3) 0.4034(2) 0.0294(8) Uani 1 1 d . . . H21 H 0.1174 1.0169 0.3907 0.035 Uiso 1 1 calc R . . C22 C 0.3104(3) 0.9857(3) 0.3228(3) 0.0336(9) Uani 1 1 d . . . C23 C 0.1381(2) 0.9459(3) 0.5684(2) 0.0287(8) Uani 1 1 d . . . H23A H 0.1116 0.9772 0.6069 0.034 Uiso 1 1 calc R . . H23B H 0.0891 0.9216 0.5543 0.034 Uiso 1 1 calc R . . C24 C 0.2339(3) 0.8457(3) 0.4284(3) 0.0378(9) Uani 1 1 d . . . H24A H 0.2636 0.8160 0.3896 0.045 Uiso 1 1 calc R . . H24B H 0.1699 0.8346 0.4389 0.045 Uiso 1 1 calc R . . C25 C 0.2507(3) 0.8671(3) 0.6735(2) 0.0295(8) Uani 1 1 d . . . C26 C 0.2231(3) 0.7840(3) 0.5951(3) 0.0331(9) Uani 1 1 d . . . H26 H 0.1696 0.7492 0.6052 0.040 Uiso 1 1 calc R . . C27 C 0.2922(2) 0.7256(3) 0.6590(3) 0.0306(8) Uani 1 1 d . . . H27 H 0.2700 0.6651 0.7028 0.037 Uiso 1 1 calc R . . C28 C 0.3548(3) 0.7515(3) 0.5173(3) 0.0376(9) Uani 1 1 d . . . C29 C 0.3551(2) 0.7581(3) 0.7737(2) 0.0311(8) Uani 1 1 d . . . H29A H 0.3303 0.7960 0.8069 0.037 Uiso 1 1 calc R . . H29B H 0.3459 0.6916 0.8114 0.037 Uiso 1 1 calc R . . C30 C 0.4511(3) 0.6493(3) 0.6315(3) 0.0341(9) Uani 1 1 d . . . H30A H 0.4340 0.5923 0.6827 0.041 Uiso 1 1 calc R . . H30B H 0.4798 0.6291 0.5856 0.041 Uiso 1 1 calc R . . C31 C 0.4921(3) 0.8314(3) 0.7628(2) 0.0295(8) Uani 1 1 d . . . C32 C 0.5126(2) 0.6923(3) 0.7380(2) 0.0301(8) Uani 1 1 d . . . H32 H 0.5027 0.6289 0.7851 0.036 Uiso 1 1 calc R . . C33 C 0.6058(3) 0.7241(3) 0.7372(2) 0.0306(8) Uani 1 1 d . . . H33 H 0.6409 0.6753 0.7832 0.037 Uiso 1 1 calc R . . C34 C 0.5959(3) 0.7171(3) 0.6042(2) 0.0310(8) Uani 1 1 d . . . C35 C 0.6479(3) 0.8537(3) 0.7745(3) 0.0360(9) Uani 1 1 d . . . H35A H 0.6156 0.8877 0.8089 0.043 Uiso 1 1 calc R . . H35B H 0.6888 0.8031 0.8115 0.043 Uiso 1 1 calc R . . C36 C 0.7418(3) 0.7547(3) 0.6239(3) 0.0327(9) Uani 1 1 d . . . H36A H 0.7623 0.7363 0.5753 0.039 Uiso 1 1 calc R . . H36B H 0.7769 0.7135 0.6724 0.039 Uiso 1 1 calc R . . N1 N 0.0543(2) 1.2921(2) 0.8026(2) 0.0308(7) Uani 1 1 d . . . N2 N 0.1956(2) 1.2522(2) 0.8280(2) 0.0305(7) Uani 1 1 d . . . N3 N 0.0163(2) 1.3161(2) 0.9362(2) 0.0350(8) Uani 1 1 d . . . N4 N 0.1565(2) 1.2653(3) 0.9664(2) 0.0387(8) Uani 1 1 d . . . N5 N 0.2997(2) 1.1161(2) 0.8944(2) 0.0320(7) Uani 1 1 d . . . N6 N 0.3063(2) 0.9598(2) 0.9650(2) 0.0311(7) Uani 1 1 d . . . N7 N 0.2625(2) 1.1290(2) 1.0342(2) 0.0359(8) Uani 1 1 d . . . N8 N 0.2783(2) 0.9736(2) 1.1049(2) 0.0335(7) Uani 1 1 d . . . N9 N 0.2492(2) 0.8059(2) 1.0270(2) 0.0317(7) Uani 1 1 d . . . N10 N 0.1367(2) 0.7167(2) 1.0615(2) 0.0338(7) Uani 1 1 d . . . N11 N 0.2116(2) 0.8249(2) 1.1632(2) 0.0336(7) Uani 1 1 d . . . N12 N 0.0992(2) 0.7339(2) 1.1988(2) 0.0309(7) Uani 1 1 d . . . N13 N 0.2393(2) 1.1481(2) 0.40241(19) 0.0298(7) Uani 1 1 d . . . N14 N 0.1799(2) 1.0155(2) 0.4886(2) 0.0332(7) Uani 1 1 d . . . N15 N 0.3000(2) 1.0819(2) 0.2983(2) 0.0337(7) Uani 1 1 d . . . N16 N 0.2417(2) 0.9464(2) 0.3854(2) 0.0344(7) Uani 1 1 d . . . N17 N 0.2002(2) 0.8678(2) 0.6135(2) 0.0324(7) Uani 1 1 d . . . N18 N 0.3064(2) 0.7879(2) 0.6989(2) 0.0290(7) Uani 1 1 d . . . N19 N 0.2729(2) 0.8002(3) 0.5105(2) 0.0378(8) Uani 1 1 d . . . N20 N 0.3709(2) 0.7099(2) 0.6023(2) 0.0346(7) Uani 1 1 d . . . N21 N 0.4504(2) 0.7674(2) 0.7519(2) 0.0303(7) Uani 1 1 d . . . N22 N 0.5832(2) 0.8112(2) 0.7508(2) 0.0313(7) Uani 1 1 d . . . N23 N 0.5156(2) 0.6928(2) 0.6533(2) 0.0334(7) Uani 1 1 d . . . N24 N 0.6486(2) 0.7386(2) 0.6503(2) 0.0319(7) Uani 1 1 d . . . O1 O 0.13503(17) 1.18441(19) 0.75538(17) 0.0332(6) Uani 1 1 d . . . O2 O 0.26849(19) 1.0270(2) 0.82557(17) 0.0359(6) Uani 1 1 d . . . O3 O 0.1822(2) 0.8024(2) 0.91596(18) 0.0417(7) Uani 1 1 d . . . O4 O 0.0434(2) 1.2420(3) 1.0799(2) 0.0527(8) Uani 1 1 d . . . O5 O 0.1895(2) 1.0612(2) 1.17191(19) 0.0437(7) Uani 1 1 d . . . O6 O 0.0910(2) 0.8437(2) 1.2583(2) 0.0438(7) Uani 1 1 d . . . O7 O 0.22076(18) 1.1071(2) 0.54948(16) 0.0333(6) Uani 1 1 d . . . O8 O 0.2443(2) 0.93017(19) 0.69998(17) 0.0364(6) Uani 1 1 d . . . O9 O 0.45476(19) 0.8976(2) 0.77981(18) 0.0364(6) Uani 1 1 d . . . O10 O 0.3698(2) 0.9422(2) 0.2924(2) 0.0446(7) Uani 1 1 d . . . O11 O 0.4059(2) 0.7425(3) 0.4569(2) 0.0524(8) Uani 1 1 d . . . O12 O 0.6175(2) 0.7176(2) 0.53135(19) 0.0429(7) 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 Cl5 0.0436(6) 0.0746(8) 0.0620(8) -0.0248(7) -0.0190(6) -0.0033(6) O1W 0.0266(14) 0.0567(18) 0.0324(15) -0.0222(14) -0.0057(12) 0.0039(12) O2W 0.0443(17) 0.0391(16) 0.0362(16) -0.0162(13) 0.0076(13) -0.0101(13) O3W 0.0337(15) 0.0467(17) 0.0351(16) -0.0158(13) 0.0033(12) -0.0055(13) O4W 0.0283(14) 0.0528(18) 0.0355(16) -0.0146(14) 0.0009(12) -0.0038(13) Er1 0.02614(10) 0.03480(11) 0.02242(10) -0.01398(7) -0.00189(7) -0.00094(7) Cl1 0.0476(8) 0.0532(8) 0.1422(16) -0.0301(9) 0.0053(9) -0.0025(6) Cl2 0.0429(7) 0.0770(10) 0.1239(15) -0.0254(10) -0.0176(8) -0.0137(7) Cl3 0.355(6) 0.244(4) 0.0502(13) 0.0077(18) -0.007(2) 0.154(4) Cl4 0.0399(8) 0.0982(14) 0.170(2) 0.0554(14) 0.0082(10) 0.0028(8) Cd1 0.0531(2) 0.0620(3) 0.0607(3) 0.0091(2) -0.00185(19) 0.00016(19) C1 0.0260(18) 0.0332(19) 0.0215(18) -0.0103(15) 0.0029(15) -0.0064(15) C2 0.034(2) 0.033(2) 0.029(2) -0.0136(16) -0.0029(16) -0.0028(16) C3 0.032(2) 0.034(2) 0.034(2) -0.0151(17) -0.0001(17) -0.0088(16) C4 0.045(2) 0.038(2) 0.039(2) -0.0230(19) -0.004(2) -0.0031(18) C5 0.0282(19) 0.041(2) 0.0251(19) -0.0140(17) 0.0021(15) -0.0125(16) C6 0.044(2) 0.054(3) 0.041(2) -0.028(2) -0.010(2) -0.009(2) C7 0.0211(17) 0.035(2) 0.0262(19) -0.0131(16) -0.0024(15) -0.0010(15) C8 0.0242(19) 0.047(2) 0.026(2) -0.0130(17) -0.0077(15) -0.0102(16) C9 0.0253(19) 0.049(2) 0.029(2) -0.0194(18) -0.0052(16) -0.0052(17) C10 0.026(2) 0.055(3) 0.032(2) -0.024(2) -0.0094(17) -0.0004(18) C11 0.0274(19) 0.037(2) 0.030(2) -0.0130(17) -0.0003(16) -0.0040(16) C12 0.038(2) 0.046(2) 0.0219(19) -0.0118(17) -0.0057(17) -0.0082(18) C13 0.0284(19) 0.034(2) 0.032(2) -0.0144(17) 0.0016(16) -0.0024(16) C14 0.0251(19) 0.039(2) 0.0251(19) -0.0121(16) -0.0038(15) 0.0017(16) C15 0.032(2) 0.0312(19) 0.031(2) -0.0122(16) -0.0027(16) 0.0035(16) C16 0.0270(19) 0.040(2) 0.0233(19) -0.0106(16) -0.0009(15) -0.0049(16) C17 0.034(2) 0.040(2) 0.039(2) -0.0243(19) 0.0039(18) -0.0072(17) C18 0.035(2) 0.035(2) 0.0239(19) -0.0118(16) -0.0051(16) -0.0007(16) C19 0.0194(17) 0.0330(19) 0.031(2) -0.0139(16) -0.0030(15) -0.0022(14) C20 0.0240(19) 0.047(2) 0.028(2) -0.0164(18) -0.0055(16) 0.0007(16) C21 0.0261(19) 0.038(2) 0.0266(19) -0.0130(16) -0.0055(15) -0.0063(16) C22 0.031(2) 0.049(2) 0.031(2) -0.0231(19) -0.0078(17) -0.0048(18) C23 0.0218(18) 0.0325(19) 0.031(2) -0.0129(16) 0.0022(15) -0.0054(15) C24 0.041(2) 0.046(2) 0.034(2) -0.0215(19) -0.0068(18) -0.0104(19) C25 0.0292(19) 0.0319(19) 0.0250(19) -0.0093(16) 0.0007(16) -0.0067(15) C26 0.032(2) 0.041(2) 0.028(2) -0.0168(17) 0.0028(16) -0.0084(17) C27 0.0246(19) 0.038(2) 0.032(2) -0.0173(17) -0.0007(16) -0.0025(16) C28 0.036(2) 0.043(2) 0.040(2) -0.023(2) -0.0009(19) -0.0034(18) C29 0.0273(19) 0.038(2) 0.029(2) -0.0153(17) 0.0033(16) -0.0065(16) C30 0.034(2) 0.032(2) 0.038(2) -0.0177(18) 0.0020(17) -0.0020(16) C31 0.030(2) 0.037(2) 0.0169(17) -0.0059(15) -0.0062(15) -0.0016(16) C32 0.0277(19) 0.0287(19) 0.0255(19) -0.0048(15) -0.0009(15) 0.0010(15) C33 0.0292(19) 0.034(2) 0.0226(19) -0.0066(16) -0.0022(15) -0.0012(16) C34 0.0278(19) 0.033(2) 0.028(2) -0.0098(16) -0.0004(16) -0.0023(15) C35 0.031(2) 0.057(3) 0.025(2) -0.0208(19) -0.0029(16) -0.0068(18) C36 0.0255(19) 0.039(2) 0.033(2) -0.0162(18) -0.0017(16) 0.0023(16) N1 0.0309(17) 0.0343(17) 0.0300(17) -0.0167(14) -0.0038(14) 0.0003(14) N2 0.0299(17) 0.0355(17) 0.0291(17) -0.0156(14) -0.0012(14) -0.0066(13) N3 0.0347(18) 0.0437(19) 0.0294(18) -0.0184(15) 0.0012(14) -0.0061(15) N4 0.038(2) 0.049(2) 0.0327(19) -0.0205(16) -0.0066(15) -0.0020(16) N5 0.0308(17) 0.0398(18) 0.0263(17) -0.0130(14) -0.0072(14) -0.0025(14) N6 0.0342(18) 0.0375(18) 0.0248(16) -0.0149(14) -0.0074(14) -0.0015(14) N7 0.0376(19) 0.0415(19) 0.0330(19) -0.0185(16) -0.0038(15) -0.0065(15) N8 0.0345(18) 0.0393(18) 0.0272(17) -0.0136(14) 0.0001(14) -0.0081(14) N9 0.0343(18) 0.0358(17) 0.0244(16) -0.0112(14) -0.0004(14) -0.0074(14) N10 0.0384(19) 0.0380(18) 0.0271(17) -0.0157(15) -0.0016(14) -0.0043(15) N11 0.0299(17) 0.0442(19) 0.0293(17) -0.0181(15) -0.0017(14) -0.0031(14) N12 0.0271(16) 0.0382(18) 0.0286(17) -0.0158(14) -0.0003(13) -0.0029(13) N13 0.0296(17) 0.0390(18) 0.0195(15) -0.0108(13) -0.0028(13) -0.0025(14) N14 0.0363(18) 0.0398(18) 0.0235(16) -0.0133(14) -0.0026(14) -0.0030(14) N15 0.0291(17) 0.049(2) 0.0306(18) -0.0232(16) -0.0006(14) -0.0082(15) N16 0.0312(17) 0.0425(19) 0.0345(18) -0.0214(16) -0.0017(15) -0.0028(14) N17 0.0316(17) 0.0357(17) 0.0325(18) -0.0155(15) -0.0040(14) -0.0062(14) N18 0.0275(16) 0.0325(16) 0.0287(17) -0.0138(14) 0.0001(13) -0.0074(13) N19 0.0382(19) 0.049(2) 0.0289(18) -0.0187(16) -0.0051(15) 0.0002(16) N20 0.0311(17) 0.0430(19) 0.0303(18) -0.0176(15) 0.0026(14) -0.0033(14) N21 0.0271(16) 0.0341(17) 0.0316(17) -0.0162(14) -0.0019(13) -0.0010(13) N22 0.0275(16) 0.0378(18) 0.0307(17) -0.0155(14) -0.0027(14) -0.0054(14) N23 0.0299(17) 0.0394(18) 0.0326(18) -0.0174(15) 0.0007(14) -0.0036(14) N24 0.0285(17) 0.0397(18) 0.0297(17) -0.0166(15) 0.0010(14) -0.0065(14) O1 0.0307(14) 0.0427(15) 0.0319(15) -0.0218(13) -0.0037(12) 0.0010(12) O2 0.0390(16) 0.0436(16) 0.0294(15) -0.0188(13) -0.0118(12) 0.0038(12) O3 0.0466(18) 0.0528(18) 0.0271(15) -0.0172(13) -0.0021(13) -0.0083(14) O4 0.057(2) 0.069(2) 0.0299(17) -0.0209(16) -0.0006(15) -0.0016(17) O5 0.0428(17) 0.0588(19) 0.0333(16) -0.0235(15) -0.0005(13) -0.0049(14) O6 0.0414(17) 0.0570(19) 0.0448(18) -0.0336(16) 0.0052(14) -0.0104(14) O7 0.0352(15) 0.0457(16) 0.0225(14) -0.0185(12) -0.0030(11) 0.0005(12) O8 0.0485(17) 0.0355(15) 0.0306(15) -0.0192(12) -0.0032(13) -0.0028(13) O9 0.0363(15) 0.0388(15) 0.0361(15) -0.0185(13) -0.0047(12) 0.0017(12) O10 0.0398(17) 0.0560(19) 0.0490(19) -0.0343(16) 0.0027(14) -0.0054(14) O11 0.0444(18) 0.079(2) 0.0380(18) -0.0330(17) 0.0032(15) 0.0025(16) O12 0.0394(16) 0.0622(19) 0.0334(16) -0.0273(15) 0.0050(13) -0.0087(14) _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 O1W Er1 2.337(3) . ? O2W Er1 2.338(3) . ? O3W Er1 2.382(3) . ? O4W Er1 2.379(3) . ? Er1 O1 2.312(2) . ? Er1 O2 2.314(3) . ? Er1 O7 2.314(2) . ? Er1 O8 2.324(3) . ? Cl1 Cd1 2.4451(16) . ? Cl2 Cd1 2.488(2) . ? Cl3 Cd1 2.392(3) . ? Cl4 Cd1 2.4343(17) . ? C1 O1 1.243(4) . ? C1 N1 1.333(5) . ? C1 N2 1.330(5) . ? C2 N3 1.439(5) . ? C2 N1 1.464(5) . ? C2 C3 1.544(5) . ? C2 H2 0.9900 . ? C3 N4 1.434(5) . ? C3 N2 1.455(5) . ? C3 H3 0.9900 . ? C4 O4 1.204(5) . ? C4 N3 1.362(5) . ? C4 N4 1.386(5) . ? C5 N5 1.431(5) . ? C5 N2 1.455(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.449(6) . ? C6 N4 1.457(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.225(4) . ? C7 N6 1.351(5) . ? C7 N5 1.355(5) . ? C8 N7 1.441(5) . ? C8 N5 1.460(5) . ? C8 C9 1.533(6) . ? C8 H8 0.9900 . ? C9 N8 1.454(5) . ? C9 N6 1.459(5) . ? C9 H9 0.9900 . ? C10 O5 1.223(5) . ? C10 N7 1.358(6) . ? C10 N8 1.355(5) . ? C11 N9 1.434(5) . ? C11 N6 1.447(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.432(5) . ? C12 N8 1.444(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.230(5) . ? C13 N10 1.355(5) . ? C13 N9 1.363(5) . ? C14 N9 1.445(5) . ? C14 N11 1.447(5) . ? C14 C15 1.544(6) . ? C14 H14 0.9900 . ? C15 N10 1.446(5) . ? C15 N12 1.450(5) . ? C15 H15 0.9900 . ? C16 O6 1.233(5) . ? C16 N12 1.364(5) . ? C16 N11 1.367(5) . ? C17 N3 1.439(5) 2_577 ? C17 N10 1.451(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.437(5) . ? C18 N1 1.435(5) 2_577 ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O7 1.231(4) . ? C19 N14 1.335(5) . ? C19 N13 1.351(5) . ? C20 N13 1.436(5) . ? C20 N15 1.444(5) . ? C20 C21 1.543(6) . ? C20 H20 0.9900 . ? C21 N14 1.440(5) . ? C21 N16 1.450(5) . ? C21 H21 0.9900 . ? C22 O10 1.228(5) . ? C22 N15 1.369(5) . ? C22 N16 1.369(5) . ? C23 N17 1.434(5) . ? C23 N14 1.453(5) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N16 1.441(6) . ? C24 N19 1.449(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O8 1.231(5) . ? C25 N18 1.334(5) . ? C25 N17 1.361(5) . ? C26 N17 1.452(5) . ? C26 N19 1.455(5) . ? C26 C27 1.529(5) . ? C26 H26 0.9900 . ? C27 N18 1.454(5) . ? C27 N20 1.470(5) . ? C27 H27 0.9900 . ? C28 O11 1.231(5) . ? C28 N19 1.346(5) . ? C28 N20 1.358(5) . ? C29 N21 1.439(5) . ? C29 N18 1.439(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N23 1.437(5) . ? C30 N20 1.435(5) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O9 1.225(5) . ? C31 N21 1.343(5) . ? C31 N22 1.367(5) . ? C32 N23 1.433(5) . ? C32 N21 1.468(5) . ? C32 C33 1.555(5) . ? C32 H32 0.9900 . ? C33 N24 1.456(5) . ? C33 N22 1.457(5) . ? C33 H33 0.9900 . ? C34 O12 1.230(5) . ? C34 N24 1.363(5) . ? C34 N23 1.365(5) . ? C35 N15 1.429(5) 2_676 ? C35 N22 1.446(5) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N24 1.433(5) . ? C36 N13 1.448(5) 2_676 ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? N1 C18 1.435(5) 2_577 ? N3 C17 1.439(5) 2_577 ? N13 C36 1.448(5) 2_676 ? N15 C35 1.429(5) 2_676 ? 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 Er1 O2 77.24(9) . . ? O1 Er1 O7 127.05(9) . . ? O2 Er1 O7 150.38(10) . . ? O1 Er1 O8 150.84(10) . . ? O2 Er1 O8 86.67(9) . . ? O7 Er1 O8 77.02(9) . . ? O1 Er1 O1W 72.64(9) . . ? O2 Er1 O1W 137.86(10) . . ? O7 Er1 O1W 71.21(9) . . ? O8 Er1 O1W 106.07(10) . . ? O1 Er1 O2W 70.98(10) . . ? O2 Er1 O2W 104.02(10) . . ? O7 Er1 O2W 73.91(10) . . ? O8 Er1 O2W 137.33(10) . . ? O1W Er1 O2W 93.35(11) . . ? O1 Er1 O4W 124.20(10) . . ? O2 Er1 O4W 72.80(10) . . ? O7 Er1 O4W 78.66(10) . . ? O8 Er1 O4W 71.98(11) . . ? O1W Er1 O4W 149.27(10) . . ? O2W Er1 O4W 72.19(10) . . ? O1 Er1 O3W 79.62(10) . . ? O2 Er1 O3W 73.38(10) . . ? O7 Er1 O3W 123.07(10) . . ? O8 Er1 O3W 72.48(10) . . ? O1W Er1 O3W 72.76(10) . . ? O2W Er1 O3W 150.18(10) . . ? O4W Er1 O3W 131.60(10) . . ? Cl3 Cd1 Cl4 114.10(12) . . ? Cl3 Cd1 Cl1 112.96(16) . . ? Cl4 Cd1 Cl1 112.56(6) . . ? Cl3 Cd1 Cl2 107.74(13) . . ? Cl4 Cd1 Cl2 105.22(9) . . ? Cl1 Cd1 Cl2 103.21(6) . . ? O1 C1 N1 124.4(4) . . ? O1 C1 N2 125.2(3) . . ? N1 C1 N2 110.4(3) . . ? N3 C2 N1 113.6(3) . . ? N3 C2 C3 103.5(3) . . ? N1 C2 C3 102.8(3) . . ? N3 C2 H2 112.1 . . ? N1 C2 H2 112.1 . . ? C3 C2 H2 112.1 . . ? N4 C3 N2 114.3(3) . . ? N4 C3 C2 103.1(3) . . ? N2 C3 C2 102.6(3) . . ? N4 C3 H3 112.0 . . ? N2 C3 H3 112.0 . . ? C2 C3 H3 112.0 . . ? O4 C4 N3 127.0(4) . . ? O4 C4 N4 126.2(4) . . ? N3 C4 N4 106.8(4) . . ? N5 C5 N2 113.1(3) . . ? N5 C5 H5A 109.0 . . ? N2 C5 H5A 109.0 . . ? N5 C5 H5B 109.0 . . ? N2 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N7 C6 N4 113.7(3) . . ? N7 C6 H6A 108.8 . . ? N4 C6 H6A 108.8 . . ? N7 C6 H6B 108.8 . . ? N4 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N6 124.6(4) . . ? O2 C7 N5 125.7(3) . . ? N6 C7 N5 109.7(3) . . ? N7 C8 N5 114.9(3) . . ? N7 C8 C9 103.8(3) . . ? N5 C8 C9 102.8(3) . . ? N7 C8 H8 111.6 . . ? N5 C8 H8 111.6 . . ? C9 C8 H8 111.6 . . ? N8 C9 N6 114.4(3) . . ? N8 C9 C8 102.8(3) . . ? N6 C9 C8 104.0(3) . . ? N8 C9 H9 111.7 . . ? N6 C9 H9 111.7 . . ? C8 C9 H9 111.7 . . ? O5 C10 N7 125.6(4) . . ? O5 C10 N8 126.0(4) . . ? N7 C10 N8 108.4(3) . . ? N9 C11 N6 113.5(3) . . ? N9 C11 H11A 108.9 . . ? N6 C11 H11A 108.9 . . ? N9 C11 H11B 108.9 . . ? N6 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? N11 C12 N8 113.9(3) . . ? N11 C12 H12A 108.8 . . ? N8 C12 H12A 108.8 . . ? N11 C12 H12B 108.8 . . ? N8 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N10 126.8(4) . . ? O3 C13 N9 125.1(4) . . ? N10 C13 N9 108.2(3) . . ? N9 C14 N11 114.5(3) . . ? N9 C14 C15 103.4(3) . . ? N11 C14 C15 103.5(3) . . ? N9 C14 H14 111.6 . . ? N11 C14 H14 111.6 . . ? C15 C14 H14 111.6 . . ? N10 C15 N12 114.5(3) . . ? N10 C15 C14 102.9(3) . . ? N12 C15 C14 103.3(3) . . ? N10 C15 H15 111.8 . . ? N12 C15 H15 111.8 . . ? C14 C15 H15 111.8 . . ? O6 C16 N12 125.9(4) . . ? O6 C16 N11 125.6(4) . . ? N12 C16 N11 108.5(3) . . ? N3 C17 N10 114.2(3) 2_577 . ? N3 C17 H17A 108.7 2_577 . ? N10 C17 H17A 108.7 . . ? N3 C17 H17B 108.7 2_577 . ? N10 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? N12 C18 N1 114.4(3) . 2_577 ? N12 C18 H18A 108.7 . . ? N1 C18 H18A 108.7 2_577 . ? N12 C18 H18B 108.7 . . ? N1 C18 H18B 108.7 2_577 . ? H18A C18 H18B 107.6 . . ? O7 C19 N14 125.6(4) . . ? O7 C19 N13 124.9(3) . . ? N14 C19 N13 109.4(3) . . ? N13 C20 N15 113.8(3) . . ? N13 C20 C21 103.7(3) . . ? N15 C20 C21 103.9(3) . . ? N13 C20 H20 111.7 . . ? N15 C20 H20 111.7 . . ? C21 C20 H20 111.7 . . ? N14 C21 N16 114.6(3) . . ? N14 C21 C20 102.4(3) . . ? N16 C21 C20 103.2(3) . . ? N14 C21 H21 112.0 . . ? N16 C21 H21 112.0 . . ? C20 C21 H21 112.0 . . ? O10 C22 N15 125.9(4) . . ? O10 C22 N16 125.7(4) . . ? N15 C22 N16 108.4(3) . . ? N17 C23 N14 112.9(3) . . ? N17 C23 H23A 109.0 . . ? N14 C23 H23A 109.0 . . ? N17 C23 H23B 109.0 . . ? N14 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? N16 C24 N19 113.7(3) . . ? N16 C24 H24A 108.8 . . ? N19 C24 H24A 108.8 . . ? N16 C24 H24B 108.8 . . ? N19 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? O8 C25 N18 126.1(4) . . ? O8 C25 N17 124.4(4) . . ? N18 C25 N17 109.4(3) . . ? N17 C26 N19 115.1(3) . . ? N17 C26 C27 102.8(3) . . ? N19 C26 C27 103.4(3) . . ? N17 C26 H26 111.6 . . ? N19 C26 H26 111.6 . . ? C27 C26 H26 111.6 . . ? N18 C27 N20 113.6(3) . . ? N18 C27 C26 103.7(3) . . ? N20 C27 C26 103.2(3) . . ? N18 C27 H27 111.9 . . ? N20 C27 H27 111.9 . . ? C26 C27 H27 111.9 . . ? O11 C28 N19 125.8(4) . . ? O11 C28 N20 124.9(4) . . ? N19 C28 N20 109.2(3) . . ? N21 C29 N18 113.4(3) . . ? N21 C29 H29A 108.9 . . ? N18 C29 H29A 108.9 . . ? N21 C29 H29B 108.9 . . ? N18 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? N23 C30 N20 114.1(3) . . ? N23 C30 H30A 108.7 . . ? N20 C30 H30A 108.7 . . ? N23 C30 H30B 108.7 . . ? N20 C30 H30B 108.7 . . ? H30A C30 H30B 107.6 . . ? O9 C31 N21 125.6(4) . . ? O9 C31 N22 125.6(4) . . ? N21 C31 N22 108.8(3) . . ? N23 C32 N21 114.4(3) . . ? N23 C32 C33 103.7(3) . . ? N21 C32 C33 101.9(3) . . ? N23 C32 H32 112.0 . . ? N21 C32 H32 112.0 . . ? C33 C32 H32 112.0 . . ? N24 C33 N22 114.0(3) . . ? N24 C33 C32 102.7(3) . . ? N22 C33 C32 103.8(3) . . ? N24 C33 H33 111.9 . . ? N22 C33 H33 111.9 . . ? C32 C33 H33 111.9 . . ? O12 C34 N24 125.9(4) . . ? O12 C34 N23 125.7(4) . . ? N24 C34 N23 108.4(3) . . ? N15 C35 N22 113.9(3) 2_676 . ? N15 C35 H35A 108.8 2_676 . ? N22 C35 H35A 108.8 . . ? N15 C35 H35B 108.8 2_676 . ? N22 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? N24 C36 N13 114.2(3) . 2_676 ? N24 C36 H36A 108.7 . . ? N13 C36 H36A 108.7 2_676 . ? N24 C36 H36B 108.7 . . ? N13 C36 H36B 108.7 2_676 . ? H36A C36 H36B 107.6 . . ? C1 N1 C18 123.1(3) . 2_577 ? C1 N1 C2 111.7(3) . . ? C18 N1 C2 123.3(3) 2_577 . ? C1 N2 C3 112.3(3) . . ? C1 N2 C5 123.7(3) . . ? C3 N2 C5 123.9(3) . . ? C4 N3 C2 113.3(3) . . ? C4 N3 C17 122.5(3) . 2_577 ? C2 N3 C17 123.6(3) . 2_577 ? C4 N4 C3 113.0(3) . . ? C4 N4 C6 122.1(4) . . ? C3 N4 C6 124.2(4) . . ? C7 N5 C5 123.3(3) . . ? C7 N5 C8 112.0(3) . . ? C5 N5 C8 124.7(3) . . ? C7 N6 C11 122.5(3) . . ? C7 N6 C9 111.2(3) . . ? C11 N6 C9 123.4(3) . . ? C10 N7 C8 112.2(3) . . ? C10 N7 C6 122.3(4) . . ? C8 N7 C6 125.1(4) . . ? C10 N8 C12 122.9(3) . . ? C10 N8 C9 112.4(3) . . ? C12 N8 C9 124.4(3) . . ? C13 N9 C11 122.8(3) . . ? C13 N9 C14 112.5(3) . . ? C11 N9 C14 124.1(3) . . ? C13 N10 C15 113.0(3) . . ? C13 N10 C17 122.6(3) . . ? C15 N10 C17 122.4(3) . . ? C16 N11 C12 122.0(3) . . ? C16 N11 C14 112.2(3) . . ? C12 N11 C14 123.2(3) . . ? C16 N12 C18 123.4(3) . . ? C16 N12 C15 112.3(3) . . ? C18 N12 C15 123.2(3) . . ? C19 N13 C36 122.5(3) . 2_676 ? C19 N13 C20 111.7(3) . . ? C36 N13 C20 123.6(3) 2_676 . ? C19 N14 C21 112.8(3) . . ? C19 N14 C23 122.6(3) . . ? C21 N14 C23 124.2(3) . . ? C22 N15 C35 123.1(3) . 2_676 ? C22 N15 C20 112.2(3) . . ? C35 N15 C20 123.7(3) 2_676 . ? C22 N16 C24 123.2(3) . . ? C22 N16 C21 112.4(3) . . ? C24 N16 C21 124.4(3) . . ? C25 N17 C23 123.8(3) . . ? C25 N17 C26 111.9(3) . . ? C23 N17 C26 124.1(3) . . ? C25 N18 C29 122.0(3) . . ? C25 N18 C27 111.9(3) . . ? C29 N18 C27 124.0(3) . . ? C28 N19 C24 121.8(4) . . ? C28 N19 C26 112.3(3) . . ? C24 N19 C26 124.6(3) . . ? C28 N20 C30 122.8(3) . . ? C28 N20 C27 111.4(3) . . ? C30 N20 C27 125.4(3) . . ? C31 N21 C29 123.3(3) . . ? C31 N21 C32 113.4(3) . . ? C29 N21 C32 121.4(3) . . ? C31 N22 C35 123.1(3) . . ? C31 N22 C33 111.9(3) . . ? C35 N22 C33 122.6(3) . . ? C34 N23 C30 122.8(3) . . ? C34 N23 C32 112.8(3) . . ? C30 N23 C32 122.7(3) . . ? C34 N24 C36 123.7(3) . . ? C34 N24 C33 112.4(3) . . ? C36 N24 C33 122.8(3) . . ? C1 O1 Er1 156.2(3) . . ? C7 O2 Er1 154.5(3) . . ? C19 O7 Er1 157.5(3) . . ? C25 O8 Er1 155.9(3) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.467 _refine_diff_density_min -1.237 _refine_diff_density_rms 0.099 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 96 38 ' ' 2 -0.048 0.500 0.270 1089 393 ' ' 3 0.500 1.000 0.500 94 41 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 902612' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p213 #TrackingRef 'submit-213.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H98 Cd Cl5 N24 O43 Tm' _chemical_formula_weight 2013.96 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -0.3139 5.2483 '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 15.127(4) _cell_length_b 15.586(5) _cell_length_c 17.087(5) _cell_angle_alpha 65.083(10) _cell_angle_beta 80.892(12) _cell_angle_gamma 81.824(12) _cell_volume 3594.5(18) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.861 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 1.826 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7004 _exptl_absorpt_correction_T_max 0.7841 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38720 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0475 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12532 _reflns_number_gt 10774 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0687P)^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 12532 _refine_ls_number_parameters 748 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1150 _refine_ls_wR_factor_gt 0.1097 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 Cl5 Cl 1.01183(10) 1.19858(12) 0.45721(10) 0.0721(4) Uani 1 1 d . . . O1W O 0.9339(2) 0.8679(2) 0.35567(19) 0.0465(8) Uani 1 1 d . . . O2W O 0.7404(2) 0.7662(2) 0.3851(2) 0.0493(8) Uani 1 1 d . . . O3W O 0.8941(2) 1.0164(2) 0.19794(19) 0.0469(8) Uani 1 1 d . . . O4W O 0.6338(2) 0.9362(3) 0.3353(2) 0.0515(8) Uani 1 1 d . . . Tm1 Tm 0.791619(12) 0.916157(13) 0.305819(10) 0.03374(8) Uani 1 1 d . . . Cl1 Cl 0.37501(13) 0.53002(13) 0.19496(18) 0.1127(8) Uani 1 1 d . . . Cl2 Cl 0.48793(12) 0.75796(15) 0.15023(15) 0.0962(6) Uani 1 1 d . . . Cl3 Cl 0.64742(13) 0.52954(16) 0.16298(17) 0.1313(10) Uani 1 1 d . . . Cl4 Cl 0.5080(4) 0.6727(3) -0.04005(16) 0.265(3) Uani 1 1 d . . . Cd1 Cd 0.50561(3) 0.61720(4) 0.11370(3) 0.07993(16) Uani 1 1 d . . . C1 C 0.7116(3) 0.9634(3) 0.1111(3) 0.0369(9) Uani 1 1 d . . . C2 C 0.6632(3) 1.0063(3) -0.0241(3) 0.0386(10) Uani 1 1 d . . . H2 H 0.6006 1.0316 -0.0361 0.046 Uiso 1 1 calc R . . C3 C 0.6717(3) 0.8981(3) 0.0234(3) 0.0406(10) Uani 1 1 d . . . H3 H 0.6136 0.8715 0.0316 0.049 Uiso 1 1 calc R . . C4 C 0.7634(3) 0.9421(3) -0.1088(3) 0.0405(10) Uani 1 1 d . . . C5 C 0.7143(3) 0.7884(3) 0.1756(3) 0.0383(10) Uani 1 1 d . . . H5A H 0.6993 0.7943 0.2311 0.046 Uiso 1 1 calc R . . H5B H 0.6727 0.7468 0.1735 0.046 Uiso 1 1 calc R . . C6 C 0.7693(3) 0.7705(4) -0.0188(3) 0.0513(12) Uani 1 1 d . . . H6A H 0.7875 0.7665 -0.0749 0.062 Uiso 1 1 calc R . . H6B H 0.7189 0.7311 0.0102 0.062 Uiso 1 1 calc R . . C7 C 0.8705(3) 0.7604(3) 0.2081(2) 0.0331(9) Uani 1 1 d . . . C8 C 0.8348(3) 0.6832(3) 0.1274(3) 0.0409(10) Uani 1 1 d . . . H8 H 0.7983 0.6282 0.1481 0.049 Uiso 1 1 calc R . . C9 C 0.9334(3) 0.6517(3) 0.1487(3) 0.0372(9) Uani 1 1 d . . . H9 H 0.9432 0.5824 0.1828 0.045 Uiso 1 1 calc R . . C10 C 0.9320(3) 0.7280(3) -0.0025(3) 0.0450(11) Uani 1 1 d . . . C11 C 1.0210(3) 0.6862(3) 0.2481(3) 0.0376(9) Uani 1 1 d . . . H11A H 1.0019 0.7051 0.2965 0.045 Uiso 1 1 calc R . . H11B H 1.0375 0.6176 0.2727 0.045 Uiso 1 1 calc R . . C12 C 1.0784(3) 0.6576(3) 0.0497(3) 0.0445(11) Uani 1 1 d . . . H12A H 1.0922 0.6614 -0.0096 0.053 Uiso 1 1 calc R . . H12B H 1.0921 0.5915 0.0895 0.053 Uiso 1 1 calc R . . C13 C 1.1288(3) 0.8060(3) 0.2115(3) 0.0393(10) Uani 1 1 d . . . C14 C 1.1648(3) 0.6990(3) 0.1448(3) 0.0397(10) Uani 1 1 d . . . H14 H 1.1846 0.6312 0.1767 0.048 Uiso 1 1 calc R . . C15 C 1.2426(3) 0.7623(3) 0.1209(3) 0.0372(9) Uani 1 1 d . . . H15 H 1.2993 0.7249 0.1415 0.045 Uiso 1 1 calc R . . C16 C 1.1881(3) 0.7785(3) -0.0063(3) 0.0373(9) Uani 1 1 d . . . C17 C 1.2684(3) 0.8847(3) 0.1756(3) 0.0417(10) Uani 1 1 d . . . H17A H 1.3283 0.8510 0.1837 0.050 Uiso 1 1 calc R . . H17B H 1.2452 0.8937 0.2287 0.050 Uiso 1 1 calc R . . C18 C 0.6798(3) 1.1355(3) 0.0268(3) 0.0383(10) Uani 1 1 d . . . H18A H 0.6233 1.1642 0.0017 0.046 Uiso 1 1 calc R . . H18B H 0.6738 1.1359 0.0846 0.046 Uiso 1 1 calc R . . C19 C 0.7487(3) 1.1321(3) 0.3261(3) 0.0382(10) Uani 1 1 d . . . C20 C 0.7082(3) 1.2751(3) 0.3404(3) 0.0379(10) Uani 1 1 d . . . H20 H 0.7308 1.3357 0.2970 0.046 Uiso 1 1 calc R . . C21 C 0.7763(3) 1.2176(3) 0.4030(3) 0.0387(10) Uani 1 1 d . . . H21 H 0.8297 1.2527 0.3924 0.046 Uiso 1 1 calc R . . C22 C 0.6455(3) 1.2492(3) 0.4820(3) 0.0444(11) Uani 1 1 d . . . C23 C 0.8622(3) 1.0539(3) 0.4308(3) 0.0402(10) Uani 1 1 d . . . H23A H 0.8886 1.0224 0.3925 0.048 Uiso 1 1 calc R . . H23B H 0.9110 1.0785 0.4447 0.048 Uiso 1 1 calc R . . C24 C 0.7667(3) 1.1550(3) 0.5701(3) 0.0470(11) Uani 1 1 d . . . H24A H 0.8306 1.1661 0.5590 0.056 Uiso 1 1 calc R . . H24B H 0.7377 1.1852 0.6087 0.056 Uiso 1 1 calc R . . C25 C 0.7851(3) 0.9090(3) 0.5139(3) 0.0346(9) Uani 1 1 d . . . C26 C 0.8205(3) 0.9831(3) 0.5964(3) 0.0405(10) Uani 1 1 d . . . H26 H 0.8821 0.9843 0.6084 0.049 Uiso 1 1 calc R . . C27 C 0.7801(3) 0.8889(3) 0.6569(3) 0.0383(10) Uani 1 1 d . . . H27 H 0.8222 0.8451 0.6982 0.046 Uiso 1 1 calc R . . C28 C 0.6905(3) 1.0143(4) 0.6772(3) 0.0429(11) Uani 1 1 d . . . C29 C 0.7416(3) 0.7533(3) 0.6241(3) 0.0406(10) Uani 1 1 d . . . H29A H 0.7617 0.7347 0.5756 0.049 Uiso 1 1 calc R . . H29B H 0.7763 0.7121 0.6723 0.049 Uiso 1 1 calc R . . C30 C 0.6482(3) 0.8535(4) 0.7745(3) 0.0430(11) Uani 1 1 d . . . H30A H 0.6164 0.8870 0.8094 0.052 Uiso 1 1 calc R . . H30B H 0.6893 0.8030 0.8107 0.052 Uiso 1 1 calc R . . C31 C 0.5950(3) 0.7151(3) 0.6048(3) 0.0397(10) Uani 1 1 d . . . C32 C 0.6054(3) 0.7242(3) 0.7375(2) 0.0352(9) Uani 1 1 d . . . H32 H 0.6400 0.6757 0.7835 0.042 Uiso 1 1 calc R . . C33 C 0.5117(3) 0.6921(3) 0.7392(3) 0.0385(10) Uani 1 1 d . . . H33 H 0.5015 0.6288 0.7864 0.046 Uiso 1 1 calc R . . C34 C 0.4933(3) 0.8320(3) 0.7617(2) 0.0341(9) Uani 1 1 d . . . C35 C 0.5503(3) 1.3520(3) 0.3676(3) 0.0440(11) Uani 1 1 d . . . H35A H 0.5679 1.4087 0.3163 0.053 Uiso 1 1 calc R . . H35B H 0.5223 1.3726 0.4133 0.053 Uiso 1 1 calc R . . C36 C 0.6447(3) 1.2424(3) 0.2249(3) 0.0392(10) Uani 1 1 d . . . H36A H 0.6544 1.3088 0.1870 0.047 Uiso 1 1 calc R . . H36B H 0.6685 1.2041 0.1919 0.047 Uiso 1 1 calc R . . N1 N 0.6940(2) 1.0374(3) 0.0357(2) 0.0362(8) Uani 1 1 d . . . N2 N 0.7007(3) 0.8818(3) 0.1055(2) 0.0413(9) Uani 1 1 d . . . N3 N 0.7237(2) 1.0235(3) -0.1042(2) 0.0384(8) Uani 1 1 d . . . N4 N 0.7389(3) 0.8675(3) -0.0340(2) 0.0434(9) Uani 1 1 d . . . N5 N 0.8036(2) 0.7448(3) 0.1725(2) 0.0371(8) Uani 1 1 d . . . N6 N 0.9458(2) 0.7063(2) 0.1974(2) 0.0355(8) Uani 1 1 d . . . N7 N 0.8444(3) 0.7316(3) 0.0340(2) 0.0470(9) Uani 1 1 d . . . N8 N 0.9840(3) 0.6825(3) 0.0642(2) 0.0441(9) Uani 1 1 d . . . N9 N 1.0988(2) 0.7340(3) 0.1987(2) 0.0388(8) Uani 1 1 d . . . N10 N 1.2105(2) 0.8267(3) 0.1633(2) 0.0406(8) Uani 1 1 d . . . N11 N 1.1367(3) 0.7165(3) 0.0613(2) 0.0415(9) Uani 1 1 d . . . N12 N 1.2483(3) 0.8070(3) 0.0270(2) 0.0385(8) Uani 1 1 d . . . N13 N 0.6945(2) 1.2124(3) 0.2998(2) 0.0362(8) Uani 1 1 d . . . N14 N 0.7998(2) 1.1318(3) 0.3860(2) 0.0388(8) Uani 1 1 d . . . N15 N 0.6295(3) 1.2910(3) 0.3964(2) 0.0419(9) Uani 1 1 d . . . N16 N 0.7276(3) 1.2006(3) 0.4884(2) 0.0465(9) Uani 1 1 d . . . N17 N 0.8196(3) 0.9848(3) 0.5104(2) 0.0392(8) Uani 1 1 d . . . N18 N 0.7613(2) 0.8509(3) 0.5975(2) 0.0374(8) Uani 1 1 d . . . N19 N 0.7587(3) 1.0540(3) 0.6143(2) 0.0417(9) Uani 1 1 d . . . N20 N 0.7000(2) 0.9190(3) 0.7008(2) 0.0415(9) Uani 1 1 d . . . N21 N 0.6482(2) 0.7376(3) 0.6509(2) 0.0404(8) Uani 1 1 d . . . N22 N 0.5162(2) 0.6917(3) 0.6540(2) 0.0383(8) Uani 1 1 d . . . N23 N 0.5827(2) 0.8104(3) 0.7508(2) 0.0377(8) Uani 1 1 d . . . N24 N 0.4499(2) 0.7665(3) 0.7519(2) 0.0382(8) Uani 1 1 d . . . O1 O 0.7317(2) 0.9712(2) 0.17475(18) 0.0436(7) Uani 1 1 d . . . O2 O 0.8649(2) 0.8139(2) 0.24524(18) 0.0407(7) Uani 1 1 d . . . O3 O 1.0902(2) 0.8456(3) 0.2571(2) 0.0532(9) Uani 1 1 d . . . O4 O 0.8119(2) 0.9357(3) -0.1716(2) 0.0522(8) Uani 1 1 d . . . O5 O 0.9568(3) 0.7559(3) -0.0795(2) 0.0637(10) Uani 1 1 d . . . O6 O 1.1822(2) 0.8025(2) -0.0835(2) 0.0505(8) Uani 1 1 d . . . O7 O 0.7551(2) 1.0689(2) 0.29949(18) 0.0429(7) Uani 1 1 d . . . O8 O 0.7777(2) 0.8916(2) 0.45032(17) 0.0394(7) Uani 1 1 d . . . O9 O 0.6173(2) 0.7150(2) 0.53253(19) 0.0496(8) Uani 1 1 d . . . O10 O 0.5941(3) 1.2581(3) 0.5416(2) 0.0643(10) Uani 1 1 d . . . O11 O 0.6302(2) 1.0587(3) 0.7066(2) 0.0529(9) Uani 1 1 d . . . O12 O 0.4553(2) 0.8980(2) 0.77925(19) 0.0433(7) 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 Cl5 0.0533(8) 0.0908(11) 0.0732(9) -0.0301(8) -0.0200(7) -0.0049(8) O1W 0.0367(18) 0.070(2) 0.0374(16) -0.0265(16) -0.0092(14) 0.0038(16) O2W 0.059(2) 0.0512(19) 0.0391(16) -0.0216(15) 0.0116(15) -0.0165(16) O3W 0.0409(18) 0.056(2) 0.0386(16) -0.0159(15) 0.0053(14) -0.0086(15) O4W 0.0387(19) 0.065(2) 0.0432(17) -0.0176(16) -0.0002(14) 0.0008(16) Tm1 0.03386(13) 0.04353(13) 0.02636(11) -0.01827(9) -0.00006(8) -0.00177(8) Cl1 0.0608(11) 0.0617(10) 0.193(2) -0.0395(13) 0.0126(12) -0.0032(8) Cl2 0.0530(10) 0.0939(13) 0.1329(16) -0.0343(12) -0.0116(10) -0.0157(9) Cl3 0.0512(10) 0.0982(15) 0.1518(19) 0.0332(13) 0.0001(11) -0.0017(10) Cl4 0.364(6) 0.253(5) 0.0571(13) 0.0034(19) -0.014(2) 0.130(4) Cd1 0.0622(3) 0.0690(3) 0.0704(3) 0.0042(2) -0.0008(2) 0.0013(2) C1 0.029(2) 0.050(3) 0.034(2) -0.021(2) -0.0004(18) -0.0028(19) C2 0.031(2) 0.057(3) 0.030(2) -0.020(2) -0.0029(18) -0.004(2) C3 0.035(2) 0.058(3) 0.037(2) -0.024(2) -0.0056(19) -0.009(2) C4 0.033(2) 0.062(3) 0.034(2) -0.025(2) -0.0079(19) -0.005(2) C5 0.036(2) 0.046(3) 0.031(2) -0.0134(19) -0.0004(18) -0.008(2) C6 0.054(3) 0.066(3) 0.053(3) -0.039(3) -0.009(2) -0.012(3) C7 0.032(2) 0.039(2) 0.0257(18) -0.0129(17) 0.0043(17) -0.0053(18) C8 0.054(3) 0.034(2) 0.036(2) -0.0142(19) -0.002(2) -0.012(2) C9 0.042(3) 0.036(2) 0.037(2) -0.0187(19) -0.0002(19) -0.0059(19) C10 0.055(3) 0.046(3) 0.043(3) -0.027(2) -0.007(2) -0.003(2) C11 0.039(2) 0.042(2) 0.0282(19) -0.0122(18) 0.0009(18) -0.0037(19) C12 0.043(3) 0.051(3) 0.050(3) -0.034(2) 0.005(2) -0.005(2) C13 0.034(2) 0.053(3) 0.033(2) -0.020(2) -0.0032(19) -0.002(2) C14 0.041(3) 0.040(2) 0.037(2) -0.0185(19) -0.0034(19) 0.011(2) C15 0.034(2) 0.043(2) 0.031(2) -0.0153(19) -0.0030(18) 0.0078(19) C16 0.038(2) 0.041(2) 0.035(2) -0.0192(19) -0.0007(19) 0.0006(19) C17 0.041(3) 0.059(3) 0.029(2) -0.020(2) -0.0056(19) -0.008(2) C18 0.028(2) 0.055(3) 0.032(2) -0.020(2) 0.0047(18) -0.0034(19) C19 0.040(3) 0.046(3) 0.028(2) -0.0144(19) 0.0067(18) -0.014(2) C20 0.037(2) 0.042(2) 0.037(2) -0.0204(19) 0.0057(19) -0.0094(19) C21 0.034(2) 0.047(3) 0.038(2) -0.021(2) 0.0065(19) -0.013(2) C22 0.045(3) 0.055(3) 0.040(2) -0.028(2) 0.009(2) -0.012(2) C23 0.033(2) 0.054(3) 0.037(2) -0.021(2) -0.0004(19) -0.007(2) C24 0.051(3) 0.058(3) 0.044(2) -0.031(2) -0.009(2) -0.007(2) C25 0.025(2) 0.047(3) 0.032(2) -0.0186(19) -0.0017(17) 0.0028(18) C26 0.037(3) 0.059(3) 0.032(2) -0.022(2) -0.0075(19) -0.007(2) C27 0.030(2) 0.056(3) 0.030(2) -0.020(2) -0.0047(18) -0.001(2) C28 0.036(3) 0.070(3) 0.032(2) -0.027(2) -0.0048(19) -0.011(2) C29 0.036(2) 0.048(3) 0.036(2) -0.020(2) 0.0020(19) 0.003(2) C30 0.041(3) 0.066(3) 0.0254(19) -0.021(2) 0.0001(18) -0.011(2) C31 0.044(3) 0.037(2) 0.035(2) -0.0129(19) -0.004(2) 0.002(2) C32 0.034(2) 0.039(2) 0.0233(18) -0.0057(17) -0.0001(17) 0.0015(18) C33 0.043(3) 0.036(2) 0.031(2) -0.0100(18) 0.0006(19) -0.0028(19) C34 0.039(2) 0.041(2) 0.0206(17) -0.0099(17) -0.0034(17) -0.0061(19) C35 0.046(3) 0.043(3) 0.048(2) -0.025(2) 0.000(2) -0.003(2) C36 0.036(2) 0.050(3) 0.031(2) -0.0181(19) 0.0062(18) -0.007(2) N1 0.037(2) 0.044(2) 0.0301(17) -0.0174(16) -0.0064(15) -0.0014(16) N2 0.040(2) 0.051(2) 0.0346(18) -0.0182(17) -0.0055(16) -0.0051(18) N3 0.037(2) 0.049(2) 0.0288(17) -0.0168(16) 0.0006(15) -0.0072(17) N4 0.048(2) 0.050(2) 0.0347(19) -0.0202(18) -0.0002(17) -0.0063(18) N5 0.035(2) 0.042(2) 0.0397(19) -0.0221(16) -0.0003(16) -0.0059(16) N6 0.037(2) 0.0376(19) 0.0365(18) -0.0204(16) -0.0030(16) -0.0023(16) N7 0.049(2) 0.057(3) 0.039(2) -0.0237(19) -0.0067(18) -0.0016(19) N8 0.044(2) 0.057(2) 0.0391(19) -0.0289(18) 0.0008(17) -0.0058(18) N9 0.036(2) 0.048(2) 0.0343(18) -0.0209(17) 0.0030(16) -0.0041(17) N10 0.039(2) 0.056(2) 0.0317(17) -0.0248(17) 0.0038(16) -0.0076(18) N11 0.045(2) 0.047(2) 0.0358(18) -0.0213(17) 0.0034(17) -0.0079(17) N12 0.046(2) 0.041(2) 0.0273(17) -0.0138(15) 0.0002(16) -0.0049(17) N13 0.038(2) 0.040(2) 0.0328(17) -0.0168(16) -0.0036(15) -0.0026(16) N14 0.037(2) 0.046(2) 0.0362(18) -0.0200(17) -0.0016(16) -0.0048(17) N15 0.040(2) 0.048(2) 0.043(2) -0.0250(18) 0.0002(17) -0.0020(18) N16 0.047(2) 0.061(3) 0.0370(19) -0.0258(19) -0.0030(18) -0.003(2) N17 0.044(2) 0.051(2) 0.0244(16) -0.0174(16) 0.0007(15) -0.0060(17) N18 0.036(2) 0.048(2) 0.0284(17) -0.0172(16) -0.0002(15) -0.0041(16) N19 0.040(2) 0.055(2) 0.0348(18) -0.0250(18) 0.0068(16) -0.0090(18) N20 0.036(2) 0.060(3) 0.0360(18) -0.0277(18) -0.0012(16) -0.0045(18) N21 0.038(2) 0.048(2) 0.0328(17) -0.0162(16) 0.0027(16) -0.0050(17) N22 0.037(2) 0.043(2) 0.0333(17) -0.0160(16) 0.0029(16) -0.0070(16) N23 0.036(2) 0.046(2) 0.0315(17) -0.0171(16) -0.0055(15) -0.0009(16) N24 0.039(2) 0.043(2) 0.0342(18) -0.0177(16) -0.0043(16) -0.0022(16) O1 0.0486(19) 0.0543(19) 0.0308(15) -0.0215(14) -0.0086(14) 0.0047(15) O2 0.0444(18) 0.0501(18) 0.0329(14) -0.0246(14) -0.0006(13) 0.0001(14) O3 0.053(2) 0.069(2) 0.0494(18) -0.0405(18) 0.0101(16) -0.0078(17) O4 0.050(2) 0.073(2) 0.0387(17) -0.0299(17) -0.0024(15) -0.0026(17) O5 0.078(3) 0.076(3) 0.0368(18) -0.0270(18) 0.0037(17) -0.006(2) O6 0.060(2) 0.059(2) 0.0378(17) -0.0247(15) -0.0060(15) -0.0055(17) O7 0.053(2) 0.0399(17) 0.0374(15) -0.0192(14) -0.0043(14) 0.0007(14) O8 0.0413(18) 0.0537(19) 0.0281(14) -0.0228(13) -0.0008(13) -0.0028(14) O9 0.048(2) 0.070(2) 0.0385(17) -0.0311(16) 0.0066(14) -0.0126(16) O10 0.058(2) 0.088(3) 0.0466(19) -0.0342(19) 0.0032(18) 0.007(2) O11 0.047(2) 0.070(2) 0.0547(19) -0.0419(19) 0.0053(16) -0.0047(17) O12 0.0460(19) 0.0472(18) 0.0418(16) -0.0242(15) -0.0061(14) 0.0007(15) _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 O1W Tm1 2.346(3) . ? O2W Tm1 2.327(3) . ? O3W Tm1 2.367(3) . ? O4W Tm1 2.364(3) . ? Tm1 O8 2.313(3) . ? Tm1 O2 2.315(3) . ? Tm1 O1 2.319(3) . ? Tm1 O7 2.327(3) . ? Cl1 Cd1 2.446(2) . ? Cl2 Cd1 2.492(2) . ? Cl3 Cd1 2.438(2) . ? Cl4 Cd1 2.391(3) . ? C1 O1 1.232(5) . ? C1 N2 1.348(6) . ? C1 N1 1.353(5) . ? C2 N1 1.459(5) . ? C2 N3 1.466(5) . ? C2 C3 1.528(7) . ? C2 H2 0.9900 . ? C3 N2 1.446(5) . ? C3 N4 1.471(6) . ? C3 H3 0.9900 . ? C4 O4 1.232(5) . ? C4 N3 1.353(6) . ? C4 N4 1.358(6) . ? C5 N5 1.427(6) . ? C5 N2 1.456(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.440(6) . ? C6 N7 1.462(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.231(5) . ? C7 N5 1.358(5) . ? C7 N6 1.353(5) . ? C8 N7 1.442(6) . ? C8 N5 1.455(5) . ? C8 C9 1.552(7) . ? C8 H8 0.9900 . ? C9 N8 1.439(5) . ? C9 N6 1.464(5) . ? C9 H9 0.9900 . ? C10 O5 1.213(6) . ? C10 N8 1.365(6) . ? C10 N7 1.377(6) . ? C11 N9 1.433(5) . ? C11 N6 1.459(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.437(6) . ? C12 N11 1.448(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.218(5) . ? C13 N10 1.370(6) . ? C13 N9 1.378(5) . ? C14 N11 1.455(5) . ? C14 N9 1.457(5) . ? C14 C15 1.538(6) . ? C14 H14 0.9900 . ? C15 N12 1.447(5) . ? C15 N10 1.460(5) . ? C15 H15 0.9900 . ? C16 O6 1.224(5) . ? C16 N12 1.358(5) . ? C16 N11 1.365(6) . ? C17 N10 1.439(5) . ? C17 N3 1.442(6) 2_775 ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.449(5) 2_775 ? C18 N1 1.459(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O7 1.233(5) . ? C19 N13 1.338(6) . ? C19 N14 1.375(5) . ? C20 N15 1.466(5) . ? C20 N13 1.469(5) . ? C20 C21 1.512(7) . ? C20 H20 0.9900 . ? C21 N16 1.461(5) . ? C21 N14 1.468(5) . ? C21 H21 0.9900 . ? C22 O10 1.224(5) . ? C22 N16 1.355(6) . ? C22 N15 1.374(6) . ? C23 N17 1.452(6) . ? C23 N14 1.440(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N19 1.445(6) . ? C24 N16 1.452(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O8 1.250(5) . ? C25 N17 1.333(5) . ? C25 N18 1.353(5) . ? C26 N19 1.444(6) . ? C26 N17 1.461(5) . ? C26 C27 1.541(6) . ? C26 H26 0.9900 . ? C27 N20 1.450(5) . ? C27 N18 1.451(5) . ? C27 H27 0.9900 . ? C28 O11 1.237(6) . ? C28 N20 1.356(6) . ? C28 N19 1.369(6) . ? C29 N21 1.437(6) . ? C29 N18 1.453(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N20 1.440(6) . ? C30 N23 1.464(5) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O9 1.227(5) . ? C31 N22 1.346(6) . ? C31 N21 1.380(6) . ? C32 N23 1.441(5) . ? C32 N21 1.460(5) . ? C32 C33 1.560(6) . ? C32 H32 0.9900 . ? C33 N24 1.451(5) . ? C33 N22 1.449(5) . ? C33 H33 0.9900 . ? C34 O12 1.232(5) . ? C34 N23 1.349(5) . ? C34 N24 1.367(5) . ? C35 N15 1.431(6) . ? C35 N22 1.463(6) 2_676 ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N24 1.434(5) 2_676 ? C36 N13 1.456(5) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? N3 C17 1.442(6) 2_775 ? N12 C18 1.449(5) 2_775 ? N22 C35 1.463(6) 2_676 ? N24 C36 1.434(5) 2_676 ? 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 O8 Tm1 O2 126.89(11) . . ? O8 Tm1 O1 150.54(11) . . ? O2 Tm1 O1 77.40(10) . . ? O8 Tm1 O2W 73.63(10) . . ? O2 Tm1 O2W 71.10(11) . . ? O1 Tm1 O2W 104.54(11) . . ? O8 Tm1 O7 77.35(10) . . ? O2 Tm1 O7 150.46(11) . . ? O1 Tm1 O7 86.41(10) . . ? O2W Tm1 O7 137.68(11) . . ? O8 Tm1 O1W 71.34(10) . . ? O2 Tm1 O1W 72.34(10) . . ? O1 Tm1 O1W 137.53(10) . . ? O2W Tm1 O1W 93.14(13) . . ? O7 Tm1 O1W 106.01(11) . . ? O8 Tm1 O3W 123.45(11) . . ? O2 Tm1 O3W 79.37(11) . . ? O1 Tm1 O3W 72.78(11) . . ? O2W Tm1 O3W 150.07(11) . . ? O7 Tm1 O3W 72.25(11) . . ? O1W Tm1 O3W 72.92(12) . . ? O8 Tm1 O4W 79.03(11) . . ? O2 Tm1 O4W 124.10(11) . . ? O1 Tm1 O4W 72.64(11) . . ? O2W Tm1 O4W 72.36(12) . . ? O7 Tm1 O4W 72.40(12) . . ? O1W Tm1 O4W 149.75(11) . . ? O3W Tm1 O4W 131.31(12) . . ? Cl4 Cd1 Cl3 111.42(13) . . ? Cl4 Cd1 Cl1 113.22(18) . . ? Cl3 Cd1 Cl1 112.85(7) . . ? Cl4 Cd1 Cl2 108.17(14) . . ? Cl3 Cd1 Cl2 106.53(9) . . ? Cl1 Cd1 Cl2 104.04(7) . . ? O1 C1 N2 126.4(4) . . ? O1 C1 N1 124.4(4) . . ? N2 C1 N1 109.2(3) . . ? N1 C2 N3 114.2(3) . . ? N1 C2 C3 103.3(3) . . ? N3 C2 C3 103.1(3) . . ? N1 C2 H2 111.9 . . ? N3 C2 H2 111.9 . . ? C3 C2 H2 111.9 . . ? N2 C3 N4 114.9(4) . . ? N2 C3 C2 103.5(3) . . ? N4 C3 C2 103.7(3) . . ? N2 C3 H3 111.4 . . ? N4 C3 H3 111.4 . . ? C2 C3 H3 111.4 . . ? O4 C4 N3 125.8(4) . . ? O4 C4 N4 125.0(4) . . ? N3 C4 N4 109.1(4) . . ? N5 C5 N2 114.2(3) . . ? N5 C5 H5A 108.7 . . ? N2 C5 H5A 108.7 . . ? N5 C5 H5B 108.7 . . ? N2 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? N4 C6 N7 114.2(3) . . ? N4 C6 H6A 108.7 . . ? N7 C6 H6A 108.7 . . ? N4 C6 H6B 108.7 . . ? N7 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? O2 C7 N5 126.4(4) . . ? O2 C7 N6 124.6(4) . . ? N5 C7 N6 109.0(3) . . ? N7 C8 N5 114.4(4) . . ? N7 C8 C9 103.1(4) . . ? N5 C8 C9 103.2(3) . . ? N7 C8 H8 111.8 . . ? N5 C8 H8 111.8 . . ? C9 C8 H8 111.8 . . ? N8 C9 N6 113.4(3) . . ? N8 C9 C8 103.0(3) . . ? N6 C9 C8 102.7(3) . . ? N8 C9 H9 112.3 . . ? N6 C9 H9 112.3 . . ? C8 C9 H9 112.3 . . ? O5 C10 N8 127.0(5) . . ? O5 C10 N7 125.8(5) . . ? N8 C10 N7 107.1(4) . . ? N9 C11 N6 113.5(3) . . ? N9 C11 H11A 108.9 . . ? N6 C11 H11A 108.9 . . ? N9 C11 H11B 108.9 . . ? N6 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? N8 C12 N11 114.9(3) . . ? N8 C12 H12A 108.6 . . ? N11 C12 H12A 108.6 . . ? N8 C12 H12B 108.6 . . ? N11 C12 H12B 108.6 . . ? H12A C12 H12B 107.5 . . ? O3 C13 N10 125.2(4) . . ? O3 C13 N9 126.7(4) . . ? N10 C13 N9 108.0(3) . . ? N11 C14 N9 114.2(4) . . ? N11 C14 C15 104.0(3) . . ? N9 C14 C15 103.9(3) . . ? N11 C14 H14 111.4 . . ? N9 C14 H14 111.4 . . ? C15 C14 H14 111.4 . . ? N12 C15 N10 114.4(4) . . ? N12 C15 C14 102.4(3) . . ? N10 C15 C14 103.3(3) . . ? N12 C15 H15 112.0 . . ? N10 C15 H15 112.0 . . ? C14 C15 H15 112.0 . . ? O6 C16 N12 126.1(4) . . ? O6 C16 N11 126.0(4) . . ? N12 C16 N11 108.0(3) . . ? N10 C17 N3 113.7(3) . 2_775 ? N10 C17 H17A 108.8 . . ? N3 C17 H17A 108.8 2_775 . ? N10 C17 H17B 108.8 . . ? N3 C17 H17B 108.8 2_775 . ? H17A C17 H17B 107.7 . . ? N12 C18 N1 113.4(3) 2_775 . ? N12 C18 H18A 108.9 2_775 . ? N1 C18 H18A 108.9 . . ? N12 C18 H18B 108.9 2_775 . ? N1 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? O7 C19 N13 126.2(4) . . ? O7 C19 N14 124.4(4) . . ? N13 C19 N14 109.3(4) . . ? N15 C20 N13 113.8(3) . . ? N15 C20 C21 104.0(3) . . ? N13 C20 C21 103.6(3) . . ? N15 C20 H20 111.6 . . ? N13 C20 H20 111.6 . . ? C21 C20 H20 111.6 . . ? N16 C21 N14 114.2(4) . . ? N16 C21 C20 104.1(4) . . ? N14 C21 C20 103.9(3) . . ? N16 C21 H21 111.4 . . ? N14 C21 H21 111.4 . . ? C20 C21 H21 111.4 . . ? O10 C22 N16 126.3(5) . . ? O10 C22 N15 124.6(5) . . ? N16 C22 N15 109.1(4) . . ? N17 C23 N14 112.2(4) . . ? N17 C23 H23A 109.2 . . ? N14 C23 H23A 109.2 . . ? N17 C23 H23B 109.2 . . ? N14 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? N19 C24 N16 114.6(3) . . ? N19 C24 H24A 108.6 . . ? N16 C24 H24A 108.6 . . ? N19 C24 H24B 108.6 . . ? N16 C24 H24B 108.6 . . ? H24A C24 H24B 107.6 . . ? O8 C25 N17 125.8(4) . . ? O8 C25 N18 124.1(4) . . ? N17 C25 N18 110.0(3) . . ? N19 C26 N17 114.6(4) . . ? N19 C26 C27 103.7(3) . . ? N17 C26 C27 102.5(3) . . ? N19 C26 H26 111.8 . . ? N17 C26 H26 111.8 . . ? C27 C26 H26 111.8 . . ? N20 C27 N18 113.5(3) . . ? N20 C27 C26 103.1(4) . . ? N18 C27 C26 103.6(3) . . ? N20 C27 H27 112.0 . . ? N18 C27 H27 112.0 . . ? C26 C27 H27 112.0 . . ? O11 C28 N20 126.3(4) . . ? O11 C28 N19 125.2(5) . . ? N20 C28 N19 108.5(4) . . ? N21 C29 N18 114.1(4) . . ? N21 C29 H29A 108.7 . . ? N18 C29 H29A 108.7 . . ? N21 C29 H29B 108.7 . . ? N18 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? N20 C30 N23 113.6(3) . . ? N20 C30 H30A 108.9 . . ? N23 C30 H30A 108.9 . . ? N20 C30 H30B 108.9 . . ? N23 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? O9 C31 N22 126.9(4) . . ? O9 C31 N21 125.5(4) . . ? N22 C31 N21 107.7(3) . . ? N23 C32 N21 114.7(3) . . ? N23 C32 C33 103.1(3) . . ? N21 C32 C33 102.8(3) . . ? N23 C32 H32 111.9 . . ? N21 C32 H32 111.9 . . ? C33 C32 H32 111.9 . . ? N24 C33 N22 114.4(3) . . ? N24 C33 C32 102.8(3) . . ? N22 C33 C32 102.6(3) . . ? N24 C33 H33 112.1 . . ? N22 C33 H33 112.1 . . ? C32 C33 H33 112.1 . . ? O12 C34 N23 126.8(4) . . ? O12 C34 N24 124.5(4) . . ? N23 C34 N24 108.7(4) . . ? N15 C35 N22 114.3(4) . 2_676 ? N15 C35 H35A 108.7 . . ? N22 C35 H35A 108.7 2_676 . ? N15 C35 H35B 108.7 . . ? N22 C35 H35B 108.7 2_676 . ? H35A C35 H35B 107.6 . . ? N24 C36 N13 113.2(3) 2_676 . ? N24 C36 H36A 108.9 2_676 . ? N13 C36 H36A 108.9 . . ? N24 C36 H36B 108.9 2_676 . ? N13 C36 H36B 108.9 . . ? H36A C36 H36B 107.8 . . ? C1 N1 C2 111.6(3) . . ? C1 N1 C18 122.8(3) . . ? C2 N1 C18 122.9(3) . . ? C1 N2 C3 112.3(4) . . ? C1 N2 C5 123.5(3) . . ? C3 N2 C5 124.2(4) . . ? C4 N3 C17 122.9(4) . 2_775 ? C4 N3 C2 112.4(4) . . ? C17 N3 C2 124.2(4) 2_775 . ? C4 N4 C6 122.8(4) . . ? C4 N4 C3 111.5(4) . . ? C6 N4 C3 125.4(4) . . ? C7 N5 C5 123.2(3) . . ? C7 N5 C8 112.3(3) . . ? C5 N5 C8 124.4(3) . . ? C7 N6 C11 122.3(3) . . ? C7 N6 C9 112.5(3) . . ? C11 N6 C9 123.3(3) . . ? C10 N7 C8 113.0(4) . . ? C10 N7 C6 122.0(4) . . ? C8 N7 C6 124.5(4) . . ? C10 N8 C9 113.6(4) . . ? C10 N8 C12 122.2(4) . . ? C9 N8 C12 123.7(4) . . ? C13 N9 C11 122.8(3) . . ? C13 N9 C14 112.1(3) . . ? C11 N9 C14 123.8(4) . . ? C13 N10 C17 121.9(3) . . ? C13 N10 C15 112.5(4) . . ? C17 N10 C15 123.0(4) . . ? C16 N11 C12 122.5(3) . . ? C16 N11 C14 111.9(3) . . ? C12 N11 C14 123.7(4) . . ? C16 N12 C15 113.6(4) . . ? C16 N12 C18 122.5(3) . 2_775 ? C15 N12 C18 123.1(3) . 2_775 ? C19 N13 C36 122.5(3) . . ? C19 N13 C20 112.1(3) . . ? C36 N13 C20 123.9(4) . . ? C19 N14 C23 123.9(4) . . ? C19 N14 C21 110.8(4) . . ? C23 N14 C21 125.0(3) . . ? C22 N15 C35 122.6(4) . . ? C22 N15 C20 110.9(4) . . ? C35 N15 C20 126.0(4) . . ? C22 N16 C24 122.1(4) . . ? C22 N16 C21 111.5(4) . . ? C24 N16 C21 125.2(4) . . ? C25 N17 C23 123.1(3) . . ? C25 N17 C26 112.3(3) . . ? C23 N17 C26 124.1(3) . . ? C25 N18 C29 122.9(3) . . ? C25 N18 C27 111.5(3) . . ? C29 N18 C27 123.9(3) . . ? C28 N19 C24 123.7(4) . . ? C28 N19 C26 112.0(4) . . ? C24 N19 C26 124.2(4) . . ? C28 N20 C30 123.4(4) . . ? C28 N20 C27 112.5(4) . . ? C30 N20 C27 122.8(4) . . ? C31 N21 C29 123.4(3) . . ? C31 N21 C32 112.5(4) . . ? C29 N21 C32 122.8(3) . . ? C31 N22 C33 114.3(3) . . ? C31 N22 C35 122.4(3) . 2_676 ? C33 N22 C35 121.8(3) . 2_676 ? C34 N23 C32 113.1(3) . . ? C34 N23 C30 122.8(3) . . ? C32 N23 C30 122.0(4) . . ? C34 N24 C36 123.2(4) . 2_676 ? C34 N24 C33 112.2(4) . . ? C36 N24 C33 122.5(4) 2_676 . ? C1 O1 Tm1 154.2(3) . . ? C7 O2 Tm1 155.6(3) . . ? C19 O7 Tm1 155.5(3) . . ? C25 O8 Tm1 156.7(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.359 _refine_diff_density_min -0.918 _refine_diff_density_rms 0.097 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 97 23 ' ' 2 -0.065 0.500 0.268 1091 496 ' ' 3 0.500 1.000 0.500 96 23 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 902613' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p214 #TrackingRef 'submit-214.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H112 Cd Cl5 N24 O50 Yb' _chemical_formula_weight 2144.19 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 '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 15.076(3) _cell_length_b 15.570(3) _cell_length_c 17.006(4) _cell_angle_alpha 64.892(7) _cell_angle_beta 80.960(7) _cell_angle_gamma 81.779(7) _cell_volume 3556.7(13) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _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 2.002 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2198 _exptl_absorpt_coefficient_mu 1.926 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6767 _exptl_absorpt_correction_T_max 0.7610 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32642 _diffrn_reflns_av_R_equivalents 0.0990 _diffrn_reflns_av_sigmaI/netI 0.1084 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11947 _reflns_number_gt 8493 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1610P)^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 11947 _refine_ls_number_parameters 748 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1082 _refine_ls_R_factor_gt 0.0896 _refine_ls_wR_factor_ref 0.2432 _refine_ls_wR_factor_gt 0.2242 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _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 Cl5 Cl 0.01236(19) 1.1989(3) 0.4564(2) 0.0725(9) Uani 1 1 d . . . O1W O -0.0665(4) 0.8695(5) 0.3542(5) 0.0469(17) Uani 1 1 d . . . O2W O -0.1059(4) 1.0160(5) 0.1985(4) 0.0429(16) Uani 1 1 d . . . O3W O -0.2588(5) 0.7642(4) 0.3873(4) 0.0468(17) Uani 1 1 d . . . O4W O -0.3667(4) 0.9362(5) 0.3358(4) 0.0513(19) Uani 1 1 d . . . Yb1 Yb -0.20867(2) 0.91598(3) 0.30634(2) 0.03415(17) Uani 1 1 d . . . Cl1 Cl 0.3752(2) 0.5293(3) 0.1985(4) 0.1129(18) Uani 1 1 d . . . Cl2 Cl 0.4883(2) 0.7587(3) 0.1503(3) 0.0990(14) Uani 1 1 d . . . Cl3 Cl 0.6485(2) 0.5287(3) 0.1608(4) 0.135(2) Uani 1 1 d . . . Cl4 Cl 0.5018(8) 0.6678(7) -0.0392(4) 0.272(7) Uani 1 1 d . . . Cd1 Cd 0.50527(6) 0.61637(7) 0.11423(7) 0.0795(4) Uani 1 1 d . . . C1 C -0.1306(6) 0.7616(6) 0.2084(6) 0.036(2) Uani 1 1 d . . . C2 C -0.1673(6) 0.6861(7) 0.1284(6) 0.044(2) Uani 1 1 d . . . H2 H -0.2037 0.6309 0.1496 0.053 Uiso 1 1 calc R . . C3 C -0.0677(6) 0.6540(6) 0.1507(6) 0.036(2) Uani 1 1 d . . . H3 H -0.0580 0.5844 0.1846 0.043 Uiso 1 1 calc R . . C4 C -0.0669(6) 0.7305(7) -0.0025(7) 0.045(2) Uani 1 1 d . . . C5 C 0.0208(6) 0.6857(6) 0.2483(6) 0.040(2) Uani 1 1 d . . . H5A H 0.0018 0.7025 0.2982 0.048 Uiso 1 1 calc R . . H5B H 0.0378 0.6170 0.2716 0.048 Uiso 1 1 calc R . . C6 C 0.0793(6) 0.6589(7) 0.0525(7) 0.045(2) Uani 1 1 d . . . H6A H 0.0914 0.5931 0.0945 0.054 Uiso 1 1 calc R . . H6B H 0.0939 0.6602 -0.0062 0.054 Uiso 1 1 calc R . . C7 C 0.1282(6) 0.8062(7) 0.2115(6) 0.040(2) Uani 1 1 d . . . C8 C 0.1634(6) 0.6984(7) 0.1441(6) 0.039(2) Uani 1 1 d . . . H8 H 0.1838 0.6306 0.1764 0.047 Uiso 1 1 calc R . . C9 C 0.2404(6) 0.7624(6) 0.1213(6) 0.038(2) Uani 1 1 d . . . H9 H 0.2966 0.7240 0.1432 0.046 Uiso 1 1 calc R . . C10 C 0.1886(6) 0.7780(6) -0.0052(7) 0.043(2) Uani 1 1 d . . . C11 C 0.2678(7) 0.8836(7) 0.1777(6) 0.043(2) Uani 1 1 d . . . H11A H 0.2427 0.8927 0.2306 0.051 Uiso 1 1 calc R . . H11B H 0.3277 0.8494 0.1878 0.051 Uiso 1 1 calc R . . C12 C 0.3186(6) 0.8641(7) -0.0279(6) 0.039(2) Uani 1 1 d . . . H12A H 0.3233 0.8644 -0.0862 0.047 Uiso 1 1 calc R . . H12B H 0.3760 0.8354 -0.0041 0.047 Uiso 1 1 calc R . . C13 C 0.2369(6) 1.0571(7) 0.1074(6) 0.038(2) Uani 1 1 d . . . C14 C 0.3374(6) 0.9927(7) 0.0236(6) 0.038(2) Uani 1 1 d . . . H14 H 0.4004 0.9671 0.0349 0.046 Uiso 1 1 calc R . . C15 C 0.3289(6) 1.1031(7) -0.0233(6) 0.038(2) Uani 1 1 d . . . H15 H 0.3867 1.1306 -0.0315 0.046 Uiso 1 1 calc R . . C16 C 0.2897(5) 1.0349(6) -0.1121(5) 0.0274(17) Uani 1 1 d . . . C17 C -0.2325(7) 0.7715(9) -0.0174(7) 0.054(3) Uani 1 1 d . . . H17A H -0.2151 0.7666 -0.0734 0.065 Uiso 1 1 calc R . . H17B H -0.2837 0.7332 0.0125 0.065 Uiso 1 1 calc R . . C18 C -0.2852(6) 0.7888(7) 0.1766(6) 0.048(3) Uani 1 1 d . . . H18A H -0.3008 0.7939 0.2327 0.057 Uiso 1 1 calc R . . H18B H -0.3269 0.7476 0.1737 0.057 Uiso 1 1 calc R . . C19 C -0.2488(6) 1.1303(6) 0.3260(6) 0.036(2) Uani 1 1 d . . . C20 C -0.2906(6) 1.2734(6) 0.3380(6) 0.036(2) Uani 1 1 d . . . H20 H -0.2675 1.3336 0.2935 0.044 Uiso 1 1 calc R . . C21 C -0.2220(6) 1.2157(7) 0.4025(6) 0.041(2) Uani 1 1 d . . . H21 H -0.1683 1.2505 0.3921 0.050 Uiso 1 1 calc R . . C22 C -0.3529(6) 1.2480(7) 0.4829(7) 0.044(2) Uani 1 1 d . . . C23 C -0.1383(6) 1.0533(7) 0.4306(6) 0.044(2) Uani 1 1 d . . . H23A H -0.0888 1.0770 0.4447 0.053 Uiso 1 1 calc R . . H23B H -0.1125 1.0228 0.3912 0.053 Uiso 1 1 calc R . . C24 C -0.2338(7) 1.1546(7) 0.5695(6) 0.045(2) Uani 1 1 d . . . H24A H -0.1700 1.1665 0.5585 0.054 Uiso 1 1 calc R . . H24B H -0.2636 1.1852 0.6076 0.054 Uiso 1 1 calc R . . C25 C -0.2136(5) 0.9089(6) 0.5147(6) 0.035(2) Uani 1 1 d . . . C26 C -0.1801(6) 0.9831(7) 0.5965(6) 0.035(2) Uani 1 1 d . . . H26 H -0.1182 0.9827 0.6094 0.043 Uiso 1 1 calc R . . C27 C -0.2214(6) 0.8887(6) 0.6570(6) 0.037(2) Uani 1 1 d . . . H27 H -0.1793 0.8444 0.6986 0.044 Uiso 1 1 calc R . . C28 C -0.3086(6) 1.0142(7) 0.6779(6) 0.040(2) Uani 1 1 d . . . C29 C -0.2596(6) 0.7535(7) 0.6234(6) 0.041(2) Uani 1 1 d . . . H29A H -0.2412 0.7382 0.5726 0.049 Uiso 1 1 calc R . . H29B H -0.2227 0.7109 0.6697 0.049 Uiso 1 1 calc R . . C30 C -0.3528(7) 0.8513(8) 0.7750(6) 0.049(3) Uani 1 1 d . . . H30A H -0.3120 0.7995 0.8109 0.059 Uiso 1 1 calc R . . H30B H -0.3838 0.8844 0.8108 0.059 Uiso 1 1 calc R . . C31 C -0.4049(6) 0.7148(7) 0.6063(6) 0.042(2) Uani 1 1 d . . . C32 C -0.3934(5) 0.7250(6) 0.7380(5) 0.038(2) Uani 1 1 d . . . H32 H -0.3597 0.6760 0.7850 0.045 Uiso 1 1 calc R . . C33 C -0.4887(6) 0.6949(6) 0.7380(6) 0.038(2) Uani 1 1 d . . . H33 H -0.4991 0.6314 0.7854 0.046 Uiso 1 1 calc R . . C34 C -0.5072(6) 0.8314(6) 0.7619(5) 0.038(2) Uani 1 1 d . . . C35 C -0.4479(6) 1.3514(6) 0.3664(6) 0.040(2) Uani 1 1 d . . . H35A H -0.4307 1.4084 0.3146 0.048 Uiso 1 1 calc R . . H35B H -0.4760 1.3718 0.4124 0.048 Uiso 1 1 calc R . . C36 C -0.3544(6) 1.2392(7) 0.2253(6) 0.037(2) Uani 1 1 d . . . H36A H -0.3309 1.1989 0.1941 0.045 Uiso 1 1 calc R . . H36B H -0.3438 1.3051 0.1854 0.045 Uiso 1 1 calc R . . N1 N -0.1966(5) 0.7446(5) 0.1747(5) 0.0379(17) Uani 1 1 d . . . N2 N -0.0547(5) 0.7062(5) 0.1990(5) 0.0376(17) Uani 1 1 d . . . N3 N -0.1575(5) 0.7326(6) 0.0354(5) 0.047(2) Uani 1 1 d . . . N4 N -0.0149(5) 0.6862(6) 0.0644(5) 0.051(2) Uani 1 1 d . . . N5 N 0.0985(5) 0.7343(6) 0.1999(5) 0.0388(18) Uani 1 1 d . . . N6 N 0.2106(5) 0.8252(6) 0.1635(5) 0.0385(17) Uani 1 1 d . . . N7 N 0.1362(5) 0.7151(6) 0.0623(5) 0.047(2) Uani 1 1 d . . . N8 N 0.2492(5) 0.8047(6) 0.0264(5) 0.0393(18) Uani 1 1 d . . . N9 N 0.2776(5) 0.9759(6) 0.1059(5) 0.0389(18) Uani 1 1 d . . . N10 N 0.2603(5) 1.1318(6) 0.0335(5) 0.0422(19) Uani 1 1 d . . . N11 N 0.3060(5) 0.9632(5) -0.0373(5) 0.0372(17) Uani 1 1 d . . . N12 N 0.2991(5) 1.1165(6) -0.1065(5) 0.0419(19) Uani 1 1 d . . . N13 N -0.3048(5) 1.2115(5) 0.2993(5) 0.0371(17) Uani 1 1 d . . . N14 N -0.1999(5) 1.1320(6) 0.3865(5) 0.0382(18) Uani 1 1 d . . . N15 N -0.3695(5) 1.2913(6) 0.3946(5) 0.0415(18) Uani 1 1 d . . . N16 N -0.2722(5) 1.1996(6) 0.4875(5) 0.0419(19) Uani 1 1 d . . . N17 N -0.1796(5) 0.9833(6) 0.5098(5) 0.045(2) Uani 1 1 d . . . N18 N -0.2409(5) 0.8513(5) 0.5995(5) 0.0386(18) Uani 1 1 d . . . N19 N -0.2402(5) 1.0537(6) 0.6156(5) 0.046(2) Uani 1 1 d . . . N20 N -0.3000(5) 0.9176(6) 0.7006(5) 0.046(2) Uani 1 1 d . . . N21 N -0.3529(5) 0.7347(5) 0.6531(5) 0.0421(19) Uani 1 1 d . . . N22 N -0.4863(5) 0.6934(6) 0.6547(5) 0.0414(18) Uani 1 1 d . . . N23 N -0.4180(5) 0.8115(6) 0.7513(5) 0.0404(18) Uani 1 1 d . . . N24 N -0.5495(5) 0.7677(5) 0.7526(5) 0.0336(16) Uani 1 1 d . . . O1 O -0.1364(4) 0.8141(5) 0.2457(4) 0.0391(14) Uani 1 1 d . . . O2 O 0.0893(5) 0.8456(5) 0.2582(4) 0.0489(17) Uani 1 1 d . . . O3 O 0.1888(5) 1.0615(5) 0.1726(4) 0.0490(17) Uani 1 1 d . . . O4 O -0.0435(5) 0.7576(6) -0.0782(4) 0.059(2) Uani 1 1 d . . . O5 O 0.1811(4) 0.8029(5) -0.0823(4) 0.0479(17) Uani 1 1 d . . . O6 O 0.2686(4) 1.0294(5) -0.1755(4) 0.0442(16) Uani 1 1 d . . . O7 O -0.2455(4) 1.0695(5) 0.2984(5) 0.0494(17) Uani 1 1 d . . . O8 O -0.2213(4) 0.8915(5) 0.4504(4) 0.0428(15) Uani 1 1 d . . . O9 O -0.3812(5) 0.7133(5) 0.5334(5) 0.0540(18) Uani 1 1 d . . . O10 O -0.4056(5) 1.2565(6) 0.5416(5) 0.061(2) Uani 1 1 d . . . O11 O -0.3687(5) 1.0578(6) 0.7073(5) 0.0534(18) Uani 1 1 d . . . O12 O -0.5441(4) 0.8992(5) 0.7785(4) 0.0426(15) 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 Cl5 0.0537(14) 0.077(2) 0.078(2) -0.0179(17) -0.0256(14) -0.0023(14) O1W 0.035(3) 0.052(4) 0.055(4) -0.023(3) -0.009(3) 0.000(3) O2W 0.050(3) 0.039(4) 0.032(3) -0.012(3) 0.015(3) -0.007(3) O3W 0.060(4) 0.021(3) 0.050(4) -0.005(3) 0.007(3) -0.017(3) O4W 0.029(3) 0.052(4) 0.051(4) -0.002(3) -0.006(3) 0.005(3) Yb1 0.0351(2) 0.0298(3) 0.0320(3) -0.00811(18) -0.00399(16) 0.00029(16) Cl1 0.0645(19) 0.051(2) 0.192(5) -0.027(2) 0.006(2) -0.0037(16) Cl2 0.0547(16) 0.079(2) 0.146(4) -0.022(2) -0.024(2) -0.0125(17) Cl3 0.0509(16) 0.084(3) 0.165(4) 0.044(3) -0.005(2) 0.0014(17) Cl4 0.360(13) 0.248(10) 0.069(3) 0.017(5) -0.020(5) 0.137(10) Cd1 0.0634(5) 0.0542(6) 0.0740(6) 0.0153(5) -0.0050(5) 0.0031(4) C1 0.038(4) 0.013(4) 0.038(5) 0.004(4) -0.001(4) -0.001(3) C2 0.040(5) 0.032(5) 0.044(5) 0.003(4) -0.011(4) -0.004(4) C3 0.046(5) 0.025(5) 0.032(5) -0.009(4) -0.003(4) 0.000(4) C4 0.046(5) 0.035(5) 0.049(6) -0.013(5) -0.007(4) -0.001(4) C5 0.053(5) 0.025(5) 0.037(5) -0.008(4) -0.007(4) -0.009(4) C6 0.042(5) 0.033(5) 0.057(6) -0.019(5) -0.004(4) 0.003(4) C7 0.038(4) 0.030(5) 0.044(5) -0.010(4) 0.001(4) 0.000(4) C8 0.039(4) 0.031(5) 0.041(5) -0.015(4) -0.003(4) 0.011(4) C9 0.041(4) 0.030(5) 0.032(5) -0.001(4) -0.009(4) 0.003(4) C10 0.046(5) 0.018(4) 0.045(6) 0.000(4) 0.002(4) 0.013(4) C11 0.050(5) 0.046(6) 0.031(5) -0.010(4) -0.005(4) -0.017(4) C12 0.039(4) 0.037(5) 0.037(5) -0.015(4) -0.001(4) 0.001(4) C13 0.032(4) 0.040(5) 0.040(5) -0.012(4) -0.014(4) 0.002(4) C14 0.032(4) 0.033(5) 0.036(5) -0.003(4) -0.004(4) 0.002(4) C15 0.037(4) 0.046(6) 0.034(5) -0.013(4) -0.010(4) -0.012(4) C16 0.031(4) 0.027(4) 0.028(4) -0.016(4) -0.008(3) 0.004(3) C17 0.051(5) 0.073(8) 0.054(6) -0.039(6) -0.011(5) -0.005(5) C18 0.045(5) 0.042(6) 0.042(5) 0.000(4) -0.005(4) -0.017(4) C19 0.037(4) 0.015(4) 0.048(5) 0.000(4) -0.014(4) -0.009(3) C20 0.035(4) 0.029(5) 0.040(5) -0.007(4) -0.002(4) -0.011(4) C21 0.041(5) 0.050(6) 0.032(5) -0.014(4) -0.001(4) -0.010(4) C22 0.046(5) 0.035(5) 0.048(6) -0.017(5) 0.002(4) -0.003(4) C23 0.030(4) 0.030(5) 0.052(6) 0.001(4) -0.001(4) 0.002(4) C24 0.054(5) 0.040(6) 0.042(5) -0.016(5) -0.006(4) -0.006(4) C25 0.022(3) 0.030(5) 0.044(5) -0.008(4) -0.009(3) 0.006(3) C26 0.039(4) 0.039(5) 0.034(5) -0.017(4) -0.008(4) -0.012(4) C27 0.042(4) 0.031(5) 0.033(5) -0.010(4) -0.006(4) 0.001(4) C28 0.043(5) 0.039(5) 0.032(5) -0.008(4) -0.004(4) -0.004(4) C29 0.038(4) 0.036(5) 0.046(5) -0.016(4) -0.006(4) 0.006(4) C30 0.047(5) 0.057(7) 0.031(5) -0.009(5) 0.002(4) -0.006(5) C31 0.042(5) 0.035(5) 0.037(5) -0.002(4) -0.002(4) -0.008(4) C32 0.038(4) 0.031(5) 0.024(4) 0.005(4) -0.007(3) 0.010(4) C33 0.047(5) 0.023(4) 0.032(5) -0.001(4) -0.005(4) -0.001(4) C34 0.045(5) 0.026(5) 0.026(4) 0.005(4) -0.002(4) -0.001(4) C35 0.045(5) 0.020(4) 0.048(5) -0.007(4) -0.007(4) 0.000(4) C36 0.040(4) 0.030(5) 0.038(5) -0.007(4) -0.014(4) -0.001(4) N1 0.038(4) 0.035(4) 0.044(4) -0.016(4) -0.008(3) -0.011(3) N2 0.043(4) 0.028(4) 0.039(4) -0.012(3) -0.002(3) -0.005(3) N3 0.048(4) 0.052(5) 0.042(5) -0.021(4) -0.012(4) 0.010(4) N4 0.051(5) 0.052(5) 0.038(4) -0.008(4) -0.003(4) -0.003(4) N5 0.037(4) 0.040(5) 0.035(4) -0.014(4) -0.005(3) 0.007(3) N6 0.040(4) 0.042(5) 0.036(4) -0.019(4) 0.001(3) -0.008(3) N7 0.050(4) 0.037(5) 0.045(5) -0.011(4) -0.001(4) 0.002(4) N8 0.038(4) 0.037(4) 0.034(4) -0.003(3) -0.012(3) -0.003(3) N9 0.044(4) 0.037(4) 0.030(4) -0.008(3) -0.007(3) -0.002(3) N10 0.042(4) 0.037(5) 0.043(4) -0.011(4) -0.013(3) -0.001(3) N11 0.035(3) 0.034(4) 0.035(4) -0.006(3) -0.008(3) 0.003(3) N12 0.042(4) 0.038(5) 0.037(4) -0.002(4) -0.017(3) -0.002(3) N13 0.039(4) 0.033(4) 0.042(4) -0.017(3) -0.006(3) -0.001(3) N14 0.047(4) 0.035(4) 0.028(4) -0.010(3) 0.000(3) -0.007(3) N15 0.043(4) 0.044(5) 0.043(4) -0.025(4) 0.005(3) -0.007(4) N16 0.042(4) 0.045(5) 0.042(4) -0.020(4) -0.008(3) -0.003(4) N17 0.041(4) 0.042(5) 0.041(4) -0.004(4) -0.007(3) -0.010(4) N18 0.036(4) 0.035(4) 0.030(4) 0.002(3) -0.006(3) 0.000(3) N19 0.048(4) 0.044(5) 0.047(5) -0.022(4) -0.002(4) -0.005(4) N20 0.038(4) 0.048(5) 0.045(5) -0.013(4) -0.002(3) -0.006(4) N21 0.047(4) 0.030(4) 0.043(4) -0.011(4) -0.004(3) -0.003(3) N22 0.046(4) 0.033(4) 0.043(4) -0.015(4) 0.003(3) -0.003(3) N23 0.044(4) 0.034(4) 0.035(4) -0.005(3) -0.002(3) -0.008(3) N24 0.037(4) 0.025(4) 0.033(4) -0.007(3) -0.002(3) 0.000(3) O1 0.040(3) 0.041(4) 0.045(4) -0.026(3) -0.015(3) 0.007(3) O2 0.055(4) 0.055(4) 0.043(4) -0.026(4) 0.001(3) -0.011(3) O3 0.054(4) 0.055(4) 0.041(4) -0.025(3) -0.008(3) 0.004(3) O4 0.074(5) 0.066(5) 0.031(4) -0.013(4) -0.005(3) -0.012(4) O5 0.052(4) 0.053(4) 0.040(4) -0.020(3) -0.005(3) -0.008(3) O6 0.046(3) 0.039(4) 0.047(4) -0.019(3) -0.008(3) 0.008(3) O7 0.052(4) 0.029(4) 0.062(5) -0.014(3) -0.012(3) 0.003(3) O8 0.055(4) 0.045(4) 0.030(3) -0.015(3) -0.015(3) 0.003(3) O9 0.058(4) 0.055(5) 0.047(4) -0.022(4) 0.009(3) -0.011(3) O10 0.059(4) 0.071(5) 0.053(5) -0.031(4) 0.000(4) 0.006(4) O11 0.046(4) 0.062(5) 0.066(5) -0.041(4) 0.005(3) -0.009(3) O12 0.048(3) 0.035(4) 0.041(4) -0.012(3) -0.008(3) -0.002(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 O1W Yb1 2.321(6) . ? O2W Yb1 2.358(5) . ? O3W Yb1 2.340(5) . ? O4W Yb1 2.361(6) . ? Yb1 O8 2.294(6) . ? Yb1 O6 2.301(7) 2_575 ? Yb1 O1 2.304(7) . ? Yb1 O7 2.327(7) . ? Cl1 Cd1 2.443(4) . ? Cl2 Cd1 2.509(5) . ? Cl3 Cd1 2.435(4) . ? Cl4 Cd1 2.389(7) . ? C1 O1 1.217(11) . ? C1 N1 1.331(12) . ? C1 N2 1.362(11) . ? C2 N3 1.426(12) . ? C2 N1 1.424(13) . ? C2 C3 1.565(12) . ? C2 H2 0.9900 . ? C3 N2 1.427(12) . ? C3 N4 1.471(11) . ? C3 H3 0.9900 . ? C4 O4 1.182(12) . ? C4 N4 1.357(13) . ? C4 N3 1.418(12) . ? C5 N5 1.430(11) . ? C5 N2 1.438(12) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.383(13) . ? C6 N4 1.431(12) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.232(12) . ? C7 N5 1.360(13) . ? C7 N6 1.371(11) . ? C8 N7 1.418(13) . ? C8 N5 1.475(11) . ? C8 C9 1.534(13) . ? C8 H8 0.9900 . ? C9 N6 1.429(12) . ? C9 N8 1.453(11) . ? C9 H9 0.9900 . ? C10 O5 1.218(12) . ? C10 N8 1.322(13) . ? C10 N7 1.372(12) . ? C11 N9 1.447(11) . ? C11 N6 1.450(12) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.432(11) . ? C12 N11 1.470(12) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.249(12) . ? C13 N9 1.332(12) . ? C13 N10 1.339(12) . ? C14 N11 1.458(13) . ? C14 N9 1.484(11) . ? C14 C15 1.554(13) . ? C14 H14 0.9900 . ? C15 N10 1.455(12) . ? C15 N12 1.473(11) . ? C15 H15 0.9900 . ? C16 O6 1.211(10) . ? C16 N11 1.319(11) . ? C16 N12 1.342(12) . ? C17 N10 1.422(14) 2_575 ? C17 N3 1.454(13) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N1 1.415(13) . ? C18 N12 1.462(12) 2_575 ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O7 1.214(12) . ? C19 N13 1.358(12) . ? C19 N14 1.367(12) . ? C20 N13 1.431(12) . ? C20 N15 1.480(11) . ? C20 C21 1.529(13) . ? C20 H20 0.9900 . ? C21 N14 1.426(13) . ? C21 N16 1.457(12) . ? C21 H21 0.9900 . ? C22 O10 1.216(12) . ? C22 N16 1.332(13) . ? C22 N15 1.408(13) . ? C23 N14 1.429(12) . ? C23 N17 1.440(11) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N19 1.437(13) . ? C24 N16 1.442(12) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O8 1.258(11) . ? C25 N17 1.299(12) . ? C25 N18 1.370(11) . ? C26 N19 1.435(12) . ? C26 N17 1.472(12) . ? C26 C27 1.543(12) . ? C26 H26 0.9900 . ? C27 N18 1.416(12) . ? C27 N20 1.418(12) . ? C27 H27 0.9900 . ? C28 O11 1.226(12) . ? C28 N19 1.360(12) . ? C28 N20 1.377(13) . ? C29 N21 1.444(11) . ? C29 N18 1.458(12) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N23 1.422(13) . ? C30 N20 1.453(12) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O9 1.245(12) . ? C31 N21 1.348(13) . ? C31 N22 1.364(11) . ? C32 N21 1.430(12) . ? C32 N23 1.445(12) . ? C32 C33 1.574(12) . ? C32 H32 0.9900 . ? C33 N22 1.420(12) . ? C33 N24 1.435(11) . ? C33 H33 0.9900 . ? C34 O12 1.241(11) . ? C34 N24 1.328(12) . ? C34 N23 1.338(12) . ? C35 N15 1.408(12) . ? C35 N22 1.457(12) 2_476 ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N13 1.439(11) . ? C36 N24 1.445(10) 2_476 ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? N10 C17 1.422(14) 2_575 ? N12 C18 1.462(12) 2_575 ? N22 C35 1.457(12) 2_476 ? N24 C36 1.445(11) 2_476 ? O6 Yb1 2.301(7) 2_575 ? 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 O8 Yb1 O6 150.9(2) . 2_575 ? O8 Yb1 O1 126.9(2) . . ? O6 Yb1 O1 77.0(2) 2_575 . ? O8 Yb1 O1W 71.6(2) . . ? O6 Yb1 O1W 136.8(2) 2_575 . ? O1 Yb1 O1W 72.5(2) . . ? O8 Yb1 O7 77.8(3) . . ? O6 Yb1 O7 86.1(2) 2_575 . ? O1 Yb1 O7 150.1(2) . . ? O1W Yb1 O7 106.0(3) . . ? O8 Yb1 O3W 73.6(2) . . ? O6 Yb1 O3W 104.9(2) 2_575 . ? O1 Yb1 O3W 70.8(2) . . ? O1W Yb1 O3W 93.3(3) . . ? O7 Yb1 O3W 138.2(2) . . ? O8 Yb1 O2W 123.0(2) . . ? O6 Yb1 O2W 73.0(2) 2_575 . ? O1 Yb1 O2W 79.5(2) . . ? O1W Yb1 O2W 71.9(2) . . ? O7 Yb1 O2W 72.0(2) . . ? O3W Yb1 O2W 149.7(2) . . ? O8 Yb1 O4W 79.4(2) . . ? O6 Yb1 O4W 72.7(2) 2_575 . ? O1 Yb1 O4W 123.8(3) . . ? O1W Yb1 O4W 150.5(2) . . ? O7 Yb1 O4W 72.4(3) . . ? O3W Yb1 O4W 72.9(2) . . ? O2W Yb1 O4W 131.5(2) . . ? Cl4 Cd1 Cl3 111.4(3) . . ? Cl4 Cd1 Cl1 111.7(4) . . ? Cl3 Cd1 Cl1 113.04(13) . . ? Cl4 Cd1 Cl2 109.5(3) . . ? Cl3 Cd1 Cl2 107.07(19) . . ? Cl1 Cd1 Cl2 103.68(15) . . ? O1 C1 N1 126.7(8) . . ? O1 C1 N2 124.3(9) . . ? N1 C1 N2 108.9(9) . . ? N3 C2 N1 116.9(8) . . ? N3 C2 C3 103.1(7) . . ? N1 C2 C3 101.7(8) . . ? N3 C2 H2 111.4 . . ? N1 C2 H2 111.4 . . ? C3 C2 H2 111.4 . . ? N2 C3 N4 112.7(7) . . ? N2 C3 C2 103.5(8) . . ? N4 C3 C2 103.4(7) . . ? N2 C3 H3 112.2 . . ? N4 C3 H3 112.2 . . ? C2 C3 H3 112.2 . . ? O4 C4 N4 127.7(9) . . ? O4 C4 N3 125.3(9) . . ? N4 C4 N3 106.9(8) . . ? N5 C5 N2 114.7(7) . . ? N5 C5 H5A 108.6 . . ? N2 C5 H5A 108.6 . . ? N5 C5 H5B 108.6 . . ? N2 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? N7 C6 N4 115.3(9) . . ? N7 C6 H6A 108.5 . . ? N4 C6 H6A 108.5 . . ? N7 C6 H6B 108.5 . . ? N4 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? O2 C7 N5 126.3(8) . . ? O2 C7 N6 126.1(9) . . ? N5 C7 N6 107.6(8) . . ? N7 C8 N5 116.0(7) . . ? N7 C8 C9 104.7(7) . . ? N5 C8 C9 101.5(8) . . ? N7 C8 H8 111.3 . . ? N5 C8 H8 111.3 . . ? C9 C8 H8 111.3 . . ? N6 C9 N8 116.8(7) . . ? N6 C9 C8 105.1(7) . . ? N8 C9 C8 102.2(7) . . ? N6 C9 H9 110.7 . . ? N8 C9 H9 110.7 . . ? C8 C9 H9 110.7 . . ? O5 C10 N8 125.8(8) . . ? O5 C10 N7 124.5(10) . . ? N8 C10 N7 109.6(9) . . ? N9 C11 N6 114.0(7) . . ? N9 C11 H11A 108.8 . . ? N6 C11 H11A 108.8 . . ? N9 C11 H11B 108.8 . . ? N6 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? N8 C12 N11 115.7(7) . . ? N8 C12 H12A 108.3 . . ? N11 C12 H12A 108.3 . . ? N8 C12 H12B 108.3 . . ? N11 C12 H12B 108.3 . . ? H12A C12 H12B 107.4 . . ? O3 C13 N9 123.1(8) . . ? O3 C13 N10 125.5(9) . . ? N9 C13 N10 111.2(8) . . ? N11 C14 N9 115.8(7) . . ? N11 C14 C15 103.6(7) . . ? N9 C14 C15 101.8(7) . . ? N11 C14 H14 111.7 . . ? N9 C14 H14 111.7 . . ? C15 C14 H14 111.7 . . ? N10 C15 N12 114.5(7) . . ? N10 C15 C14 103.6(7) . . ? N12 C15 C14 100.3(7) . . ? N10 C15 H15 112.5 . . ? N12 C15 H15 112.5 . . ? C14 C15 H15 112.5 . . ? O6 C16 N11 126.4(8) . . ? O6 C16 N12 124.9(8) . . ? N11 C16 N12 108.7(7) . . ? N10 C17 N3 113.3(9) 2_575 . ? N10 C17 H17A 108.9 2_575 . ? N3 C17 H17A 108.9 . . ? N10 C17 H17B 108.9 2_575 . ? N3 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? N1 C18 N12 115.0(7) . 2_575 ? N1 C18 H18A 108.5 . . ? N12 C18 H18A 108.5 2_575 . ? N1 C18 H18B 108.5 . . ? N12 C18 H18B 108.5 2_575 . ? H18A C18 H18B 107.5 . . ? O7 C19 N13 123.7(8) . . ? O7 C19 N14 128.5(8) . . ? N13 C19 N14 107.8(8) . . ? N13 C20 N15 114.3(7) . . ? N13 C20 C21 104.1(8) . . ? N15 C20 C21 103.1(7) . . ? N13 C20 H20 111.6 . . ? N15 C20 H20 111.6 . . ? C21 C20 H20 111.6 . . ? N14 C21 N16 114.2(8) . . ? N14 C21 C20 103.0(8) . . ? N16 C21 C20 103.6(7) . . ? N14 C21 H21 111.8 . . ? N16 C21 H21 111.8 . . ? C20 C21 H21 111.8 . . ? O10 C22 N16 128.8(10) . . ? O10 C22 N15 123.5(9) . . ? N16 C22 N15 107.7(8) . . ? N14 C23 N17 113.1(7) . . ? N14 C23 H23A 109.0 . . ? N17 C23 H23A 109.0 . . ? N14 C23 H23B 109.0 . . ? N17 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? N19 C24 N16 115.9(9) . . ? N19 C24 H24A 108.3 . . ? N16 C24 H24A 108.3 . . ? N19 C24 H24B 108.3 . . ? N16 C24 H24B 108.3 . . ? H24A C24 H24B 107.4 . . ? O8 C25 N17 125.0(8) . . ? O8 C25 N18 123.9(8) . . ? N17 C25 N18 111.1(9) . . ? N19 C26 N17 116.9(8) . . ? N19 C26 C27 103.7(7) . . ? N17 C26 C27 101.7(7) . . ? N19 C26 H26 111.2 . . ? N17 C26 H26 111.2 . . ? C27 C26 H26 111.2 . . ? N18 C27 N20 112.9(8) . . ? N18 C27 C26 104.6(7) . . ? N20 C27 C26 103.8(8) . . ? N18 C27 H27 111.7 . . ? N20 C27 H27 111.7 . . ? C26 C27 H27 111.7 . . ? O11 C28 N19 125.6(10) . . ? O11 C28 N20 125.9(8) . . ? N19 C28 N20 108.4(9) . . ? N21 C29 N18 114.6(8) . . ? N21 C29 H29A 108.6 . . ? N18 C29 H29A 108.6 . . ? N21 C29 H29B 108.6 . . ? N18 C29 H29B 108.6 . . ? H29A C29 H29B 107.6 . . ? N23 C30 N20 113.6(8) . . ? N23 C30 H30A 108.8 . . ? N20 C30 H30A 108.8 . . ? N23 C30 H30B 108.8 . . ? N20 C30 H30B 108.8 . . ? H30A C30 H30B 107.7 . . ? O9 C31 N21 125.8(8) . . ? O9 C31 N22 126.5(9) . . ? N21 C31 N22 107.7(9) . . ? N21 C32 N23 117.2(7) . . ? N21 C32 C33 100.4(7) . . ? N23 C32 C33 101.4(7) . . ? N21 C32 H32 112.2 . . ? N23 C32 H32 112.2 . . ? C33 C32 H32 112.2 . . ? N22 C33 N24 115.6(7) . . ? N22 C33 C32 104.6(7) . . ? N24 C33 C32 103.0(7) . . ? N22 C33 H33 111.1 . . ? N24 C33 H33 111.1 . . ? C32 C33 H33 111.1 . . ? O12 C34 N24 125.6(8) . . ? O12 C34 N23 124.6(9) . . ? N24 C34 N23 109.8(9) . . ? N15 C35 N22 113.5(8) . 2_476 ? N15 C35 H35A 108.9 . . ? N22 C35 H35A 108.9 2_476 . ? N15 C35 H35B 108.9 . . ? N22 C35 H35B 108.9 2_476 . ? H35A C35 H35B 107.7 . . ? N13 C36 N24 114.2(7) . 2_476 ? N13 C36 H36A 108.7 . . ? N24 C36 H36A 108.7 2_476 . ? N13 C36 H36B 108.7 . . ? N24 C36 H36B 108.7 2_476 . ? H36A C36 H36B 107.6 . . ? C1 N1 C18 123.0(9) . . ? C1 N1 C2 113.6(8) . . ? C18 N1 C2 123.1(8) . . ? C1 N2 C3 111.5(8) . . ? C1 N2 C5 123.7(8) . . ? C3 N2 C5 123.3(8) . . ? C4 N3 C2 113.6(8) . . ? C4 N3 C17 122.1(8) . . ? C2 N3 C17 124.1(8) . . ? C4 N4 C6 123.5(8) . . ? C4 N4 C3 113.0(8) . . ? C6 N4 C3 122.7(8) . . ? C7 N5 C5 124.4(8) . . ? C7 N5 C8 113.1(7) . . ? C5 N5 C8 121.6(8) . . ? C7 N6 C9 112.5(8) . . ? C7 N6 C11 120.0(8) . . ? C9 N6 C11 125.2(7) . . ? C10 N7 C6 124.4(9) . . ? C10 N7 C8 111.0(8) . . ? C6 N7 C8 123.1(8) . . ? C10 N8 C12 122.9(8) . . ? C10 N8 C9 112.5(7) . . ? C12 N8 C9 124.5(7) . . ? C13 N9 C11 123.9(8) . . ? C13 N9 C14 111.6(7) . . ? C11 N9 C14 124.4(8) . . ? C13 N10 C17 124.7(9) . 2_575 ? C13 N10 C15 111.4(8) . . ? C17 N10 C15 123.3(8) 2_575 . ? C16 N11 C14 113.1(7) . . ? C16 N11 C12 121.8(8) . . ? C14 N11 C12 122.4(7) . . ? C16 N12 C18 124.4(8) . 2_575 ? C16 N12 C15 114.0(7) . . ? C18 N12 C15 121.6(8) 2_575 . ? C19 N13 C20 112.0(8) . . ? C19 N13 C36 121.5(8) . . ? C20 N13 C36 124.8(8) . . ? C19 N14 C21 112.8(8) . . ? C19 N14 C23 121.2(9) . . ? C21 N14 C23 125.9(8) . . ? C35 N15 C22 122.4(8) . . ? C35 N15 C20 126.3(8) . . ? C22 N15 C20 111.0(8) . . ? C22 N16 C24 120.0(8) . . ? C22 N16 C21 113.9(8) . . ? C24 N16 C21 124.6(8) . . ? C25 N17 C23 124.5(9) . . ? C25 N17 C26 111.9(7) . . ? C23 N17 C26 123.3(8) . . ? C25 N18 C27 110.6(8) . . ? C25 N18 C29 120.5(8) . . ? C27 N18 C29 126.2(7) . . ? C28 N19 C26 111.8(8) . . ? C28 N19 C24 123.6(9) . . ? C26 N19 C24 124.4(8) . . ? C28 N20 C27 112.1(7) . . ? C28 N20 C30 123.1(9) . . ? C27 N20 C30 123.3(9) . . ? C31 N21 C32 115.1(7) . . ? C31 N21 C29 122.0(8) . . ? C32 N21 C29 122.5(8) . . ? C31 N22 C33 112.1(8) . . ? C31 N22 C35 122.7(8) . 2_476 ? C33 N22 C35 123.1(7) . 2_476 ? C34 N23 C30 124.9(9) . . ? C34 N23 C32 113.0(8) . . ? C30 N23 C32 119.7(8) . . ? C34 N24 C33 112.7(7) . . ? C34 N24 C36 122.6(8) . 2_476 ? C33 N24 C36 123.3(7) . 2_476 ? C1 O1 Yb1 156.0(6) . . ? C16 O6 Yb1 155.8(6) . 2_575 ? C19 O7 Yb1 153.0(6) . . ? C25 O8 Yb1 156.9(6) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 2.688 _refine_diff_density_min -3.444 _refine_diff_density_rms 0.219 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 91 35 ' ' 2 -0.069 0.500 0.264 1071 604 ' ' 3 0.500 1.000 0.500 94 35 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 902614' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p215 #TrackingRef 'submit-215.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H138 Cd Cl5 Lu N24 O63' _chemical_formula_weight 2380.32 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Lu Lu -0.4720 5.8584 '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 15.064(10) _cell_length_b 15.606(10) _cell_length_c 16.975(11) _cell_angle_alpha 64.896(18) _cell_angle_beta 80.645(19) _cell_angle_gamma 81.170(19) _cell_volume 3550(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2460 _exptl_absorpt_coefficient_mu 2.028 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6993 _exptl_absorpt_correction_T_max 0.7644 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33959 _diffrn_reflns_av_R_equivalents 0.0850 _diffrn_reflns_av_sigmaI/netI 0.1401 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12118 _reflns_number_gt 8976 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1714P)^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 12118 _refine_ls_number_parameters 748 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1358 _refine_ls_R_factor_gt 0.0800 _refine_ls_wR_factor_ref 0.2513 _refine_ls_wR_factor_gt 0.2253 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 Cl5 Cl 0.5120(2) 1.1986(2) 0.9566(2) 0.0705(9) Uani 1 1 d . . . O1W O 0.4320(4) 0.8682(5) 0.8558(4) 0.0419(15) Uani 1 1 d . . . O2W O 0.2404(5) 0.7685(5) 0.8853(4) 0.0446(16) Uani 1 1 d . . . O3W O 0.3938(4) 1.0157(5) 0.6981(5) 0.0468(16) Uani 1 1 d . . . O4W O 0.1344(5) 0.9376(5) 0.8364(5) 0.0502(17) Uani 1 1 d . . . Lu1 Lu 0.29156(2) 0.91702(2) 0.80578(2) 0.03365(17) Uani 1 1 d . . . Cl1 Cl -0.1247(2) 0.5292(3) 0.6965(4) 0.1083(17) Uani 1 1 d . . . Cl2 Cl -0.0123(3) 0.7562(3) 0.6500(4) 0.1012(14) Uani 1 1 d . . . Cl3 Cl 0.1482(3) 0.5274(3) 0.6638(4) 0.133(2) Uani 1 1 d . . . Cl4 Cl 0.0019(8) 0.6690(7) 0.4602(4) 0.244(6) Uani 1 1 d . . . Cd1 Cd 0.00553(7) 0.61623(7) 0.61385(8) 0.0790(3) Uani 1 1 d . . . C1 C 0.2507(6) 1.1311(6) 0.8245(6) 0.0343(19) Uani 1 1 d . . . C2 C 0.2100(6) 1.2745(7) 0.8378(6) 0.037(2) Uani 1 1 d . . . H2 H 0.2329 1.3349 0.7943 0.044 Uiso 1 1 calc R . . C3 C 0.2776(7) 1.2141(7) 0.9034(6) 0.038(2) Uani 1 1 d . . . H3 H 0.3318 1.2475 0.8938 0.046 Uiso 1 1 calc R . . C4 C 0.1462(7) 1.2485(7) 0.9812(7) 0.044(2) Uani 1 1 d . . . C5 C 0.3623(5) 1.0531(6) 0.9300(7) 0.035(2) Uani 1 1 d . . . H5A H 0.4114 1.0773 0.9436 0.042 Uiso 1 1 calc R . . H5B H 0.3886 1.0214 0.8915 0.042 Uiso 1 1 calc R . . C6 C 0.2657(7) 1.1529(8) 1.0698(7) 0.050(3) Uani 1 1 d . . . H6A H 0.2367 1.1834 1.1087 0.060 Uiso 1 1 calc R . . H6B H 0.3299 1.1634 1.0583 0.060 Uiso 1 1 calc R . . C7 C 0.2874(5) 0.9089(6) 1.0118(6) 0.0333(19) Uani 1 1 d . . . C8 C 0.3203(6) 0.9821(6) 1.0961(6) 0.0305(18) Uani 1 1 d . . . H8 H 0.3822 0.9829 1.1083 0.037 Uiso 1 1 calc R . . C9 C 0.2799(6) 0.8888(6) 1.1577(6) 0.038(2) Uani 1 1 d . . . H9 H 0.3227 0.8447 1.1988 0.045 Uiso 1 1 calc R . . C10 C 0.1910(6) 1.0145(7) 1.1762(7) 0.041(2) Uani 1 1 d . . . C11 C 0.2431(6) 0.7555(7) 1.1238(6) 0.040(2) Uani 1 1 d . . . H11A H 0.2781 0.7149 1.1727 0.048 Uiso 1 1 calc R . . H11B H 0.2648 0.7367 1.0753 0.048 Uiso 1 1 calc R . . C12 C 0.1489(7) 0.8533(8) 1.2749(7) 0.047(2) Uani 1 1 d . . . H12A H 0.1165 0.8867 1.3101 0.056 Uiso 1 1 calc R . . H12B H 0.1903 0.8024 1.3114 0.056 Uiso 1 1 calc R . . C13 C 0.0947(6) 0.7151(6) 1.1061(6) 0.037(2) Uani 1 1 d . . . C14 C 0.1063(6) 0.7242(7) 1.2380(6) 0.038(2) Uani 1 1 d . . . H14 H 0.1409 0.6749 1.2844 0.045 Uiso 1 1 calc R . . C15 C 0.0137(6) 0.6932(7) 1.2369(6) 0.041(2) Uani 1 1 d . . . H15 H 0.0034 0.6300 1.2845 0.049 Uiso 1 1 calc R . . C16 C -0.0087(6) 0.8309(6) 1.2638(6) 0.0342(19) Uani 1 1 d . . . C17 C -0.0510(6) 0.6504(6) 1.1327(6) 0.0356(19) Uani 1 1 d . . . H17A H -0.0225 0.6308 1.0860 0.043 Uiso 1 1 calc R . . H17B H -0.0682 0.5930 1.1838 0.043 Uiso 1 1 calc R . . C18 C -0.1451(6) 0.7575(7) 1.2759(6) 0.039(2) Uani 1 1 d . . . H18A H -0.1525 0.6903 1.3130 0.047 Uiso 1 1 calc R . . H18B H -0.1701 0.7941 1.3106 0.047 Uiso 1 1 calc R . . C19 C 0.2099(6) 0.9654(7) 0.6123(6) 0.036(2) Uani 1 1 d . . . C20 C 0.1634(6) 1.0076(7) 0.4742(6) 0.039(2) Uani 1 1 d . . . H20 H 0.1005 1.0334 0.4619 0.047 Uiso 1 1 calc R . . C21 C 0.1726(6) 0.9003(6) 0.5213(7) 0.040(2) Uani 1 1 d . . . H21 H 0.1140 0.8749 0.5289 0.048 Uiso 1 1 calc R . . C22 C 0.2623(6) 0.9421(8) 0.3929(7) 0.042(2) Uani 1 1 d . . . C23 C 0.2144(6) 0.7915(6) 0.6757(7) 0.038(2) Uani 1 1 d . . . H23A H 0.1990 0.7963 0.7322 0.046 Uiso 1 1 calc R . . H23B H 0.1728 0.7506 0.6731 0.046 Uiso 1 1 calc R . . C24 C 0.2667(7) 0.7724(7) 0.4830(7) 0.049(3) Uani 1 1 d . . . H24A H 0.2846 0.7680 0.4266 0.058 Uiso 1 1 calc R . . H24B H 0.2161 0.7336 0.5126 0.058 Uiso 1 1 calc R . . C25 C 0.3708(6) 0.7617(6) 0.7074(5) 0.0277(17) Uani 1 1 d . . . C26 C 0.3348(6) 0.6849(6) 0.6281(5) 0.0328(19) Uani 1 1 d . . . H26 H 0.2984 0.6301 0.6491 0.039 Uiso 1 1 calc R . . C27 C 0.4343(6) 0.6531(6) 0.6497(7) 0.038(2) Uani 1 1 d . . . H27 H 0.4447 0.5837 0.6839 0.046 Uiso 1 1 calc R . . C28 C 0.4299(7) 0.7286(8) 0.4996(8) 0.051(3) Uani 1 1 d . . . C29 C 0.5193(6) 0.6864(7) 0.7489(6) 0.038(2) Uani 1 1 d . . . H29A H 0.5362 0.6177 0.7731 0.046 Uiso 1 1 calc R . . H29B H 0.4998 0.7044 0.7982 0.046 Uiso 1 1 calc R . . C30 C 0.5778(6) 0.6575(7) 0.5506(7) 0.045(2) Uani 1 1 d . . . H30A H 0.5915 0.6600 0.4913 0.055 Uiso 1 1 calc R . . H30B H 0.5916 0.5917 0.5918 0.055 Uiso 1 1 calc R . . C31 C 0.6281(6) 0.8078(7) 0.7106(6) 0.039(2) Uani 1 1 d . . . C32 C 0.6644(6) 0.6988(6) 0.6458(6) 0.037(2) Uani 1 1 d . . . H32 H 0.6852 0.6310 0.6779 0.044 Uiso 1 1 calc R . . C33 C 0.7430(6) 0.7635(6) 0.6185(5) 0.0338(19) Uani 1 1 d . . . H33 H 0.8004 0.7259 0.6386 0.041 Uiso 1 1 calc R . . C34 C 0.6857(6) 0.7777(7) 0.4951(6) 0.036(2) Uani 1 1 d . . . C35 C 0.2308(7) 1.1169(7) 0.3238(6) 0.045(2) Uani 1 1 d . . . H35A H 0.2532 1.1078 0.2701 0.054 Uiso 1 1 calc R . . H35B H 0.1705 1.1514 0.3163 0.054 Uiso 1 1 calc R . . C36 C 0.1798(6) 1.1376(7) 0.5278(6) 0.037(2) Uani 1 1 d . . . H36A H 0.1224 1.1665 0.5034 0.044 Uiso 1 1 calc R . . H36B H 0.1750 1.1377 0.5860 0.044 Uiso 1 1 calc R . . N1 N 0.1950(5) 1.2123(5) 0.7977(5) 0.0379(17) Uani 1 1 d . . . N2 N 0.2991(5) 1.1322(5) 0.8844(5) 0.0399(18) Uani 1 1 d . . . N3 N 0.1301(6) 1.2894(5) 0.8952(6) 0.0415(19) Uani 1 1 d . . . N4 N 0.2266(6) 1.1988(6) 0.9886(5) 0.0411(18) Uani 1 1 d . . . N5 N 0.3199(6) 0.9837(6) 1.0111(6) 0.045(2) Uani 1 1 d . . . N6 N 0.2604(5) 0.8502(5) 1.0975(5) 0.0335(16) Uani 1 1 d . . . N7 N 0.2579(6) 1.0527(6) 1.1146(6) 0.045(2) Uani 1 1 d . . . N8 N 0.1992(5) 0.9168(6) 1.2030(6) 0.0431(19) Uani 1 1 d . . . N9 N 0.1493(5) 0.7381(6) 1.1504(5) 0.0397(17) Uani 1 1 d . . . N10 N 0.0155(5) 0.6925(6) 1.1556(6) 0.0440(19) Uani 1 1 d . . . N11 N 0.0842(5) 0.8113(6) 1.2507(5) 0.0397(18) Uani 1 1 d . . . N12 N -0.0497(5) 0.7694(5) 1.2509(5) 0.0342(16) Uani 1 1 d . . . N13 N 0.1957(5) 1.0398(5) 0.5357(5) 0.0364(17) Uani 1 1 d . . . N14 N 0.1989(5) 0.8848(6) 0.6073(5) 0.0390(18) Uani 1 1 d . . . N15 N 0.2234(5) 1.0249(6) 0.3959(5) 0.0388(18) Uani 1 1 d . . . N16 N 0.2366(6) 0.8686(6) 0.4673(6) 0.0436(19) Uani 1 1 d . . . N17 N 0.3038(5) 0.7462(5) 0.6735(5) 0.0333(16) Uani 1 1 d . . . N18 N 0.4453(5) 0.7072(5) 0.6991(5) 0.0367(17) Uani 1 1 d . . . N19 N 0.3444(6) 0.7316(6) 0.5372(6) 0.048(2) Uani 1 1 d . . . N20 N 0.4849(5) 0.6841(6) 0.5648(5) 0.0400(18) Uani 1 1 d . . . N21 N 0.5969(5) 0.7338(5) 0.7001(5) 0.0398(18) Uani 1 1 d . . . N22 N 0.7099(5) 0.8262(6) 0.6644(5) 0.0377(17) Uani 1 1 d . . . N23 N 0.6350(6) 0.7171(6) 0.5610(5) 0.0421(19) Uani 1 1 d . . . N24 N 0.7482(5) 0.8067(6) 0.5277(5) 0.0368(17) Uani 1 1 d . . . O1 O 0.2543(5) 1.0703(4) 0.7978(4) 0.0411(15) Uani 1 1 d . . . O2 O 0.2782(4) 0.8932(5) 0.9500(4) 0.0418(16) Uani 1 1 d . . . O3 O 0.1178(5) 0.7142(5) 1.0328(5) 0.0481(17) Uani 1 1 d . . . O4 O 0.0960(6) 1.2581(7) 1.0402(6) 0.068(2) Uani 1 1 d . . . O5 O 0.1307(5) 1.0567(5) 1.2079(5) 0.0513(18) Uani 1 1 d . . . O6 O -0.0448(4) 0.8982(5) 1.2794(5) 0.0424(15) Uani 1 1 d . . . O7 O 0.2305(4) 0.9718(5) 0.6761(4) 0.0411(15) Uani 1 1 d . . . O8 O 0.3640(4) 0.8163(5) 0.7447(4) 0.0417(16) Uani 1 1 d . . . O9 O 0.5891(5) 0.8441(5) 0.7591(5) 0.0500(18) Uani 1 1 d . . . O10 O 0.3106(5) 0.9367(6) 0.3284(5) 0.0529(18) Uani 1 1 d . . . O11 O 0.4548(6) 0.7569(6) 0.4209(5) 0.057(2) Uani 1 1 d . . . O12 O 0.6824(5) 0.8021(5) 0.4177(5) 0.0527(19) 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 Cl5 0.0476(16) 0.082(2) 0.081(2) -0.0296(18) -0.0222(16) 0.0002(14) O1W 0.038(4) 0.055(4) 0.025(4) -0.015(3) 0.002(3) 0.005(3) O2W 0.051(4) 0.042(3) 0.037(4) -0.015(3) 0.008(3) -0.009(3) O3W 0.036(4) 0.058(4) 0.043(4) -0.021(4) 0.004(3) -0.001(3) O4W 0.040(4) 0.069(5) 0.042(4) -0.027(4) 0.003(3) -0.001(3) Lu1 0.0333(3) 0.0396(3) 0.0303(3) -0.0185(2) -0.00361(18) 0.00270(16) Cl1 0.0537(19) 0.060(2) 0.187(5) -0.036(3) 0.010(2) -0.0004(16) Cl2 0.055(2) 0.088(3) 0.154(4) -0.038(3) -0.023(2) -0.0091(18) Cl3 0.050(2) 0.099(3) 0.151(5) 0.037(3) -0.005(2) 0.003(2) Cl4 0.331(13) 0.215(8) 0.071(4) 0.010(5) -0.029(6) 0.104(9) Cd1 0.0596(6) 0.0646(6) 0.0731(7) 0.0050(5) -0.0050(5) 0.0060(5) C1 0.032(4) 0.045(5) 0.025(5) -0.016(4) 0.008(4) -0.010(4) C2 0.034(5) 0.041(5) 0.036(5) -0.019(4) 0.002(4) -0.006(4) C3 0.050(6) 0.052(5) 0.017(4) -0.017(4) -0.004(4) -0.009(4) C4 0.047(6) 0.039(5) 0.043(6) -0.017(5) -0.002(5) -0.001(4) C5 0.021(4) 0.038(5) 0.047(6) -0.021(4) 0.003(4) -0.003(3) C6 0.048(6) 0.061(6) 0.050(7) -0.029(6) -0.011(5) -0.008(5) C7 0.023(4) 0.035(4) 0.040(5) -0.018(4) 0.000(4) 0.006(3) C8 0.028(4) 0.035(4) 0.027(5) -0.014(4) -0.002(4) 0.000(3) C9 0.028(4) 0.040(5) 0.041(6) -0.012(4) -0.013(4) 0.004(4) C10 0.030(5) 0.056(6) 0.052(6) -0.040(5) -0.004(5) 0.001(4) C11 0.039(5) 0.054(6) 0.028(5) -0.024(5) -0.007(4) 0.021(4) C12 0.039(5) 0.064(6) 0.045(6) -0.029(5) -0.014(5) 0.009(5) C13 0.046(5) 0.031(4) 0.030(5) -0.011(4) -0.002(4) 0.000(4) C14 0.033(5) 0.045(5) 0.024(5) -0.007(4) 0.002(4) 0.001(4) C15 0.043(5) 0.037(5) 0.036(6) -0.010(4) -0.014(4) 0.011(4) C16 0.041(5) 0.032(4) 0.024(5) -0.009(4) -0.003(4) 0.004(4) C17 0.041(5) 0.035(4) 0.027(5) -0.014(4) 0.003(4) 0.003(4) C18 0.029(5) 0.060(6) 0.039(6) -0.033(5) 0.003(4) -0.001(4) C19 0.029(4) 0.050(5) 0.029(5) -0.020(4) -0.003(4) 0.005(4) C20 0.027(4) 0.063(6) 0.029(5) -0.019(5) -0.006(4) -0.001(4) C21 0.035(5) 0.040(5) 0.043(6) -0.013(4) -0.008(4) -0.006(4) C22 0.022(4) 0.067(6) 0.055(7) -0.038(6) -0.019(5) 0.002(4) C23 0.038(5) 0.037(5) 0.039(6) -0.011(4) -0.014(4) -0.004(4) C24 0.059(6) 0.056(6) 0.047(6) -0.032(5) -0.015(5) -0.006(5) C25 0.034(4) 0.031(4) 0.012(4) -0.008(3) 0.013(3) -0.006(3) C26 0.038(5) 0.034(4) 0.020(4) -0.005(4) 0.004(4) -0.013(4) C27 0.042(5) 0.027(4) 0.048(6) -0.019(4) -0.008(5) 0.002(4) C28 0.046(6) 0.055(6) 0.070(9) -0.042(6) -0.015(6) 0.001(5) C29 0.031(5) 0.043(5) 0.042(6) -0.020(4) -0.002(4) 0.002(4) C30 0.040(5) 0.050(5) 0.057(7) -0.035(5) 0.000(5) 0.001(4) C31 0.029(4) 0.057(6) 0.040(6) -0.029(5) 0.000(4) -0.005(4) C32 0.047(5) 0.037(5) 0.023(5) -0.014(4) -0.014(4) 0.016(4) C33 0.042(5) 0.033(4) 0.018(4) -0.004(4) -0.007(4) 0.008(4) C34 0.027(4) 0.052(5) 0.031(5) -0.024(4) -0.001(4) 0.006(4) C35 0.056(6) 0.051(6) 0.029(5) -0.017(5) -0.009(5) 0.000(5) C36 0.029(4) 0.053(5) 0.030(5) -0.020(4) -0.003(4) 0.004(4) N1 0.041(4) 0.041(4) 0.036(5) -0.021(4) -0.003(4) -0.003(3) N2 0.044(4) 0.043(4) 0.034(5) -0.017(4) -0.012(4) -0.001(3) N3 0.046(5) 0.036(4) 0.044(5) -0.021(4) -0.003(4) 0.002(3) N4 0.046(5) 0.048(4) 0.023(4) -0.010(4) -0.001(4) -0.006(4) N5 0.043(5) 0.047(5) 0.052(6) -0.026(4) -0.018(4) 0.007(4) N6 0.036(4) 0.042(4) 0.021(4) -0.014(3) -0.005(3) 0.009(3) N7 0.039(4) 0.046(4) 0.061(6) -0.032(4) -0.013(4) 0.004(4) N8 0.039(4) 0.054(5) 0.040(5) -0.025(4) 0.002(4) -0.004(4) N9 0.040(4) 0.048(4) 0.023(4) -0.009(3) 0.009(3) -0.008(3) N10 0.041(4) 0.047(5) 0.045(5) -0.023(4) 0.008(4) -0.007(4) N11 0.037(4) 0.055(5) 0.036(5) -0.028(4) 0.001(4) -0.008(4) N12 0.032(4) 0.031(4) 0.034(4) -0.011(3) -0.006(3) 0.008(3) N13 0.038(4) 0.035(4) 0.037(5) -0.016(4) -0.013(4) 0.005(3) N14 0.027(4) 0.053(5) 0.037(5) -0.016(4) -0.008(3) -0.006(3) N15 0.033(4) 0.049(4) 0.037(5) -0.022(4) 0.000(4) -0.005(3) N16 0.043(5) 0.058(5) 0.038(5) -0.027(4) -0.004(4) -0.007(4) N17 0.025(4) 0.040(4) 0.037(4) -0.019(3) 0.004(3) -0.008(3) N18 0.043(4) 0.034(4) 0.036(5) -0.018(4) -0.010(4) 0.005(3) N19 0.048(5) 0.060(5) 0.041(5) -0.022(4) -0.015(4) 0.004(4) N20 0.048(5) 0.052(5) 0.023(4) -0.021(4) 0.013(4) -0.010(4) N21 0.047(5) 0.041(4) 0.032(4) -0.019(4) -0.008(4) 0.008(3) N22 0.037(4) 0.050(4) 0.030(4) -0.024(4) 0.012(3) -0.012(3) N23 0.048(5) 0.043(4) 0.037(5) -0.020(4) 0.001(4) -0.006(4) N24 0.034(4) 0.052(4) 0.025(4) -0.016(4) -0.001(3) -0.005(3) O1 0.052(4) 0.039(3) 0.036(4) -0.021(3) -0.001(3) -0.002(3) O2 0.045(4) 0.062(4) 0.027(4) -0.030(3) -0.005(3) 0.005(3) O3 0.052(4) 0.063(4) 0.034(4) -0.026(3) 0.013(3) -0.019(3) O4 0.058(5) 0.088(6) 0.060(6) -0.040(5) 0.000(4) 0.008(4) O5 0.042(4) 0.067(5) 0.058(5) -0.042(4) 0.006(4) -0.007(3) O6 0.045(4) 0.042(3) 0.042(4) -0.021(3) -0.005(3) 0.003(3) O7 0.042(4) 0.050(4) 0.036(4) -0.024(3) -0.013(3) 0.006(3) O8 0.047(4) 0.052(4) 0.036(4) -0.029(3) -0.011(3) 0.007(3) O9 0.039(4) 0.067(5) 0.058(5) -0.042(4) 0.006(3) -0.005(3) O10 0.056(4) 0.073(5) 0.036(4) -0.031(4) -0.003(4) -0.001(4) O11 0.064(5) 0.079(5) 0.027(4) -0.023(4) -0.001(4) -0.003(4) O12 0.072(5) 0.049(4) 0.040(4) -0.016(3) -0.018(4) -0.009(4) _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 O1W Lu1 2.306(6) . ? O2W Lu1 2.311(7) . ? O3W Lu1 2.347(7) . ? O4W Lu1 2.343(7) . ? Lu1 O8 2.286(6) . ? Lu1 O7 2.290(6) . ? Lu1 O2 2.294(6) . ? Lu1 O1 2.322(6) . ? Cl1 Cd1 2.443(4) . ? Cl2 Cd1 2.475(5) . ? Cl3 Cd1 2.437(4) . ? Cl4 Cd1 2.386(7) . ? C1 O1 1.204(10) . ? C1 N2 1.351(11) . ? C1 N1 1.352(12) . ? C2 N1 1.460(10) . ? C2 N3 1.476(12) . ? C2 C3 1.532(12) . ? C2 H2 0.9900 . ? C3 N2 1.425(11) . ? C3 N4 1.463(12) . ? C3 H3 0.9900 . ? C4 O4 1.202(13) . ? C4 N4 1.327(13) . ? C4 N3 1.369(13) . ? C5 N2 1.449(11) . ? C5 N5 1.461(13) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.434(13) . ? C6 N7 1.435(14) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.208(10) . ? C7 N5 1.328(11) . ? C7 N6 1.382(12) . ? C8 N5 1.434(11) . ? C8 N7 1.440(11) . ? C8 C9 1.536(13) . ? C8 H8 0.9900 . ? C9 N8 1.443(12) . ? C9 N6 1.471(10) . ? C9 H9 0.9900 . ? C10 O5 1.228(11) . ? C10 N7 1.333(14) . ? C10 N8 1.385(12) . ? C11 N6 1.404(13) . ? C11 N9 1.444(12) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.396(14) . ? C12 N11 1.450(11) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.242(11) . ? C13 N10 1.344(13) . ? C13 N9 1.375(11) . ? C14 N11 1.447(11) . ? C14 N9 1.460(12) . ? C14 C15 1.550(13) . ? C14 H14 0.9900 . ? C15 N10 1.381(12) . ? C15 N12 1.483(11) . ? C15 H15 0.9900 . ? C16 O6 1.219(10) . ? C16 N12 1.324(11) . ? C16 N11 1.388(12) . ? C17 N3 1.410(11) 2_577 ? C17 N10 1.460(11) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N1 1.431(11) 2_577 ? C18 N12 1.448(11) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O7 1.221(10) . ? C19 N14 1.332(12) . ? C19 N13 1.348(12) . ? C20 N15 1.426(12) . ? C20 N13 1.506(10) . ? C20 C21 1.513(13) . ? C20 H20 0.9900 . ? C21 N16 1.401(13) . ? C21 N14 1.486(11) . ? C21 H21 0.9900 . ? C22 O10 1.238(13) . ? C22 N16 1.345(14) . ? C22 N15 1.354(12) . ? C23 N17 1.424(11) . ? C23 N14 1.440(12) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N16 1.423(13) . ? C24 N19 1.498(12) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O8 1.244(9) . ? C25 N18 1.327(11) . ? C25 N17 1.337(10) . ? C26 N19 1.393(12) . ? C26 N17 1.450(11) . ? C26 C27 1.556(12) . ? C26 H26 0.9900 . ? C27 N20 1.434(12) . ? C27 N18 1.460(10) . ? C27 H27 0.9900 . ? C28 O11 1.227(14) . ? C28 N19 1.345(14) . ? C28 N20 1.366(13) . ? C29 N18 1.423(11) . ? C29 N21 1.425(13) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N20 1.408(12) . ? C30 N23 1.439(11) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O9 1.217(11) . ? C31 N22 1.348(12) . ? C31 N21 1.399(11) . ? C32 N21 1.459(11) . ? C32 N23 1.474(11) . ? C32 C33 1.557(13) . ? C32 H32 0.9900 . ? C33 N24 1.389(11) . ? C33 N22 1.479(10) . ? C33 H33 0.9900 . ? C34 O12 1.209(11) . ? C34 N23 1.333(13) . ? C34 N24 1.383(11) . ? C35 N22 1.442(12) 2_676 ? C35 N15 1.443(13) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N24 1.443(13) 2_676 ? C36 N13 1.459(11) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? N1 C18 1.431(11) 2_577 ? N3 C17 1.410(11) 2_577 ? N22 C35 1.442(12) 2_676 ? N24 C36 1.443(13) 2_676 ? 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 O8 Lu1 O7 77.3(2) . . ? O8 Lu1 O2 127.4(2) . . ? O7 Lu1 O2 150.1(2) . . ? O8 Lu1 O1W 72.9(2) . . ? O7 Lu1 O1W 138.4(2) . . ? O2 Lu1 O1W 70.9(2) . . ? O8 Lu1 O2W 71.4(3) . . ? O7 Lu1 O2W 104.1(2) . . ? O2 Lu1 O2W 74.0(2) . . ? O1W Lu1 O2W 93.2(2) . . ? O8 Lu1 O1 149.8(3) . . ? O7 Lu1 O1 85.8(2) . . ? O2 Lu1 O1 77.7(2) . . ? O1W Lu1 O1 106.3(2) . . ? O2W Lu1 O1 137.9(2) . . ? O8 Lu1 O4W 124.1(2) . . ? O7 Lu1 O4W 72.5(2) . . ? O2 Lu1 O4W 78.8(2) . . ? O1W Lu1 O4W 149.0(2) . . ? O2W Lu1 O4W 72.0(3) . . ? O1 Lu1 O4W 72.4(2) . . ? O8 Lu1 O3W 79.3(3) . . ? O7 Lu1 O3W 73.5(2) . . ? O2 Lu1 O3W 123.0(2) . . ? O1W Lu1 O3W 73.0(2) . . ? O2W Lu1 O3W 150.2(2) . . ? O1 Lu1 O3W 71.9(2) . . ? O4W Lu1 O3W 131.8(3) . . ? Cl4 Cd1 Cl3 113.0(3) . . ? Cl4 Cd1 Cl1 111.1(4) . . ? Cl3 Cd1 Cl1 112.41(16) . . ? Cl4 Cd1 Cl2 109.1(3) . . ? Cl3 Cd1 Cl2 106.42(19) . . ? Cl1 Cd1 Cl2 104.29(16) . . ? O1 C1 N2 128.0(9) . . ? O1 C1 N1 124.1(8) . . ? N2 C1 N1 107.9(7) . . ? N1 C2 N3 112.3(7) . . ? N1 C2 C3 103.8(7) . . ? N3 C2 C3 102.4(7) . . ? N1 C2 H2 112.5 . . ? N3 C2 H2 112.5 . . ? C3 C2 H2 112.5 . . ? N2 C3 N4 115.8(8) . . ? N2 C3 C2 102.1(6) . . ? N4 C3 C2 103.9(8) . . ? N2 C3 H3 111.5 . . ? N4 C3 H3 111.5 . . ? C2 C3 H3 111.5 . . ? O4 C4 N4 125.5(10) . . ? O4 C4 N3 125.1(10) . . ? N4 C4 N3 109.4(9) . . ? N2 C5 N5 112.6(7) . . ? N2 C5 H5A 109.1 . . ? N5 C5 H5A 109.1 . . ? N2 C5 H5B 109.1 . . ? N5 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? N4 C6 N7 115.1(7) . . ? N4 C6 H6A 108.5 . . ? N7 C6 H6A 108.5 . . ? N4 C6 H6B 108.5 . . ? N7 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? O2 C7 N5 127.9(10) . . ? O2 C7 N6 123.4(8) . . ? N5 C7 N6 108.6(8) . . ? N5 C8 N7 115.1(7) . . ? N5 C8 C9 103.0(7) . . ? N7 C8 C9 102.9(7) . . ? N5 C8 H8 111.7 . . ? N7 C8 H8 111.7 . . ? C9 C8 H8 111.7 . . ? N8 C9 N6 112.8(7) . . ? N8 C9 C8 105.0(7) . . ? N6 C9 C8 103.4(7) . . ? N8 C9 H9 111.7 . . ? N6 C9 H9 111.7 . . ? C8 C9 H9 111.7 . . ? O5 C10 N7 126.8(9) . . ? O5 C10 N8 122.9(10) . . ? N7 C10 N8 110.3(7) . . ? N6 C11 N9 114.7(7) . . ? N6 C11 H11A 108.6 . . ? N9 C11 H11A 108.6 . . ? N6 C11 H11B 108.6 . . ? N9 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? N8 C12 N11 113.4(8) . . ? N8 C12 H12A 108.9 . . ? N11 C12 H12A 108.9 . . ? N8 C12 H12B 108.9 . . ? N11 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N10 126.8(8) . . ? O3 C13 N9 124.1(9) . . ? N10 C13 N9 109.1(8) . . ? N11 C14 N9 113.8(8) . . ? N11 C14 C15 104.6(7) . . ? N9 C14 C15 101.1(7) . . ? N11 C14 H14 112.2 . . ? N9 C14 H14 112.2 . . ? C15 C14 H14 112.2 . . ? N10 C15 N12 114.3(7) . . ? N10 C15 C14 106.0(8) . . ? N12 C15 C14 101.5(7) . . ? N10 C15 H15 111.5 . . ? N12 C15 H15 111.5 . . ? C14 C15 H15 111.5 . . ? O6 C16 N12 126.6(9) . . ? O6 C16 N11 123.9(8) . . ? N12 C16 N11 109.3(7) . . ? N3 C17 N10 114.8(7) 2_577 . ? N3 C17 H17A 108.6 2_577 . ? N10 C17 H17A 108.6 . . ? N3 C17 H17B 108.6 2_577 . ? N10 C17 H17B 108.6 . . ? H17A C17 H17B 107.5 . . ? N1 C18 N12 112.8(8) 2_577 . ? N1 C18 H18A 109.0 2_577 . ? N12 C18 H18A 109.0 . . ? N1 C18 H18B 109.0 2_577 . ? N12 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? O7 C19 N14 125.6(9) . . ? O7 C19 N13 124.4(8) . . ? N14 C19 N13 109.9(7) . . ? N15 C20 N13 113.0(7) . . ? N15 C20 C21 103.2(8) . . ? N13 C20 C21 103.7(7) . . ? N15 C20 H20 112.1 . . ? N13 C20 H20 112.1 . . ? C21 C20 H20 112.1 . . ? N16 C21 N14 117.0(8) . . ? N16 C21 C20 105.3(8) . . ? N14 C21 C20 102.5(7) . . ? N16 C21 H21 110.5 . . ? N14 C21 H21 110.5 . . ? C20 C21 H21 110.5 . . ? O10 C22 N16 126.3(9) . . ? O10 C22 N15 123.7(11) . . ? N16 C22 N15 109.9(9) . . ? N17 C23 N14 116.1(8) . . ? N17 C23 H23A 108.3 . . ? N14 C23 H23A 108.3 . . ? N17 C23 H23B 108.3 . . ? N14 C23 H23B 108.3 . . ? H23A C23 H23B 107.4 . . ? N16 C24 N19 114.4(7) . . ? N16 C24 H24A 108.7 . . ? N19 C24 H24A 108.7 . . ? N16 C24 H24B 108.7 . . ? N19 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? O8 C25 N18 124.2(8) . . ? O8 C25 N17 125.4(8) . . ? N18 C25 N17 110.3(7) . . ? N19 C26 N17 114.7(7) . . ? N19 C26 C27 102.9(8) . . ? N17 C26 C27 102.5(6) . . ? N19 C26 H26 112.0 . . ? N17 C26 H26 112.0 . . ? C27 C26 H26 112.0 . . ? N20 C27 N18 113.8(7) . . ? N20 C27 C26 103.0(7) . . ? N18 C27 C26 102.4(6) . . ? N20 C27 H27 112.3 . . ? N18 C27 H27 112.3 . . ? C26 C27 H27 112.3 . . ? O11 C28 N19 126.8(10) . . ? O11 C28 N20 125.3(10) . . ? N19 C28 N20 107.8(10) . . ? N18 C29 N21 113.9(8) . . ? N18 C29 H29A 108.8 . . ? N21 C29 H29A 108.8 . . ? N18 C29 H29B 108.8 . . ? N21 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? N20 C30 N23 113.3(7) . . ? N20 C30 H30A 108.9 . . ? N23 C30 H30A 108.9 . . ? N20 C30 H30B 108.9 . . ? N23 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? O9 C31 N22 126.4(8) . . ? O9 C31 N21 124.1(9) . . ? N22 C31 N21 109.3(7) . . ? N21 C32 N23 113.3(7) . . ? N21 C32 C33 105.3(7) . . ? N23 C32 C33 102.6(7) . . ? N21 C32 H32 111.7 . . ? N23 C32 H32 111.7 . . ? C33 C32 H32 111.7 . . ? N24 C33 N22 116.0(7) . . ? N24 C33 C32 104.1(6) . . ? N22 C33 C32 101.7(7) . . ? N24 C33 H33 111.4 . . ? N22 C33 H33 111.4 . . ? C32 C33 H33 111.4 . . ? O12 C34 N23 126.9(8) . . ? O12 C34 N24 123.3(9) . . ? N23 C34 N24 109.7(8) . . ? N22 C35 N15 113.4(7) 2_676 . ? N22 C35 H35A 108.9 2_676 . ? N15 C35 H35A 108.9 . . ? N22 C35 H35B 108.9 2_676 . ? N15 C35 H35B 108.9 . . ? H35A C35 H35B 107.7 . . ? N24 C36 N13 111.4(7) 2_676 . ? N24 C36 H36A 109.3 2_676 . ? N13 C36 H36A 109.3 . . ? N24 C36 H36B 109.3 2_676 . ? N13 C36 H36B 109.3 . . ? H36A C36 H36B 108.0 . . ? C1 N1 C18 123.0(7) . 2_577 ? C1 N1 C2 111.4(7) . . ? C18 N1 C2 124.0(7) 2_577 . ? C1 N2 C3 114.4(7) . . ? C1 N2 C5 122.3(7) . . ? C3 N2 C5 123.2(7) . . ? C4 N3 C17 121.9(8) . 2_577 ? C4 N3 C2 111.5(8) . . ? C17 N3 C2 126.0(8) 2_577 . ? C4 N4 C6 122.8(9) . . ? C4 N4 C3 112.2(8) . . ? C6 N4 C3 123.6(8) . . ? C7 N5 C8 114.3(9) . . ? C7 N5 C5 120.7(8) . . ? C8 N5 C5 124.4(7) . . ? C7 N6 C11 123.2(7) . . ? C7 N6 C9 110.5(7) . . ? C11 N6 C9 123.7(7) . . ? C10 N7 C6 123.9(8) . . ? C10 N7 C8 112.5(8) . . ? C6 N7 C8 123.6(9) . . ? C10 N8 C12 125.4(8) . . ? C10 N8 C9 109.4(8) . . ? C12 N8 C9 124.0(8) . . ? C13 N9 C11 125.8(8) . . ? C13 N9 C14 111.1(8) . . ? C11 N9 C14 122.0(7) . . ? C13 N10 C15 112.6(8) . . ? C13 N10 C17 121.9(8) . . ? C15 N10 C17 124.0(8) . . ? C16 N11 C14 110.9(7) . . ? C16 N11 C12 123.5(7) . . ? C14 N11 C12 122.7(8) . . ? C16 N12 C18 123.4(7) . . ? C16 N12 C15 113.2(7) . . ? C18 N12 C15 120.6(7) . . ? C19 N13 C36 122.3(7) . . ? C19 N13 C20 110.5(7) . . ? C36 N13 C20 123.2(7) . . ? C19 N14 C23 124.4(7) . . ? C19 N14 C21 112.9(8) . . ? C23 N14 C21 122.6(7) . . ? C22 N15 C20 110.7(9) . . ? C22 N15 C35 124.2(9) . . ? C20 N15 C35 124.5(8) . . ? C22 N16 C21 110.8(8) . . ? C22 N16 C24 122.7(9) . . ? C21 N16 C24 126.3(9) . . ? C25 N17 C23 123.5(7) . . ? C25 N17 C26 112.1(7) . . ? C23 N17 C26 124.2(7) . . ? C25 N18 C29 123.8(7) . . ? C25 N18 C27 112.1(7) . . ? C29 N18 C27 122.6(7) . . ? C28 N19 C26 114.4(8) . . ? C28 N19 C24 121.1(9) . . ? C26 N19 C24 124.1(9) . . ? C28 N20 C30 124.0(9) . . ? C28 N20 C27 111.7(8) . . ? C30 N20 C27 123.5(8) . . ? C31 N21 C29 124.7(8) . . ? C31 N21 C32 110.3(8) . . ? C29 N21 C32 123.8(7) . . ? C31 N22 C35 123.1(7) . 2_676 ? C31 N22 C33 113.4(7) . . ? C35 N22 C33 121.7(8) 2_676 . ? C34 N23 C30 123.9(8) . . ? C34 N23 C32 110.9(7) . . ? C30 N23 C32 123.0(9) . . ? C34 N24 C33 112.6(8) . . ? C34 N24 C36 122.5(7) . 2_676 ? C33 N24 C36 124.1(7) . 2_676 ? C1 O1 Lu1 153.5(6) . . ? C7 O2 Lu1 156.8(7) . . ? C19 O7 Lu1 154.9(6) . . ? C25 O8 Lu1 156.4(6) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 2.243 _refine_diff_density_min -2.343 _refine_diff_density_rms 0.223 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 97 60 ' ' 2 -0.105 0.500 0.061 1082 834 ' ' 3 0.500 0.000 0.500 93 51 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 902615' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p306 #TrackingRef 'submit-306.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H116 Cl10 N24 O52 Sm2 Zn2' _chemical_formula_weight 2503.47 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 '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 10.4581(11) _cell_length_b 26.990(3) _cell_length_c 29.150(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.840(3) _cell_angle_gamma 90.00 _cell_volume 8198.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.028 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5080 _exptl_absorpt_coefficient_mu 2.437 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6162 _exptl_absorpt_correction_T_max 0.6821 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 77241 _diffrn_reflns_av_R_equivalents 0.0873 _diffrn_reflns_av_sigmaI/netI 0.0788 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 26.00 _reflns_number_total 15963 _reflns_number_gt 9813 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.2000P)^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 15963 _refine_ls_number_parameters 865 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1450 _refine_ls_R_factor_gt 0.1112 _refine_ls_wR_factor_ref 0.3369 _refine_ls_wR_factor_gt 0.3127 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.153 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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 Cl9 Cl 0.98511(14) 0.24865(9) 0.62100(5) 0.0558(6) Uani 1 1 d . . . Cl10 Cl -0.48797(15) 0.25394(10) 0.12063(5) 0.0660(7) Uani 1 1 d . . . Cl1 Cl 0.75515(15) 0.60614(6) 0.38199(5) 0.0407(4) Uani 1 1 d . . . Cl2 Cl 0.5479(3) 0.52051(10) 0.30892(10) 0.1071(9) Uani 1 1 d . . . Cl3 Cl 0.5101(3) 0.53617(11) 0.43450(10) 0.1308(8) Uani 1 1 d . . . Cl4 Cl 0.7888(3) 0.47169(11) 0.39153(15) 0.1253(14) Uani 1 1 d . . . Cl5 Cl -0.2721(3) -0.11348(9) 0.37350(7) 0.0888(8) Uani 1 1 d . . . Cl6 Cl -0.0494(3) -0.04275(11) 0.30629(11) 0.1348(10) Uani 1 1 d . . . Cl7 Cl -0.2881(3) 0.02312(17) 0.3688(2) 0.224(3) Uani 1 1 d . . . Cl8 Cl -0.0296(4) -0.03509(15) 0.43382(13) 0.1818(14) Uani 1 1 d . . . Zn1 Zn 0.64778(8) 0.53462(3) 0.37937(3) 0.0516(2) Uani 1 1 d . . . Zn2 Zn -0.16153(11) -0.04328(4) 0.36906(4) 0.0781(4) Uani 1 1 d . . . O1W O 0.7812(3) 0.31277(17) 0.40433(13) 0.0329(11) Uani 1 1 d . . . O2W O 0.7520(3) 0.34578(14) 0.51366(13) 0.0284(10) Uani 1 1 d . . . O3W O 0.7084(3) 0.18466(16) 0.45587(15) 0.0373(11) Uani 1 1 d . . . O4W O 0.7434(3) 0.24313(18) 0.54889(13) 0.0381(12) Uani 1 1 d . . . O5W O 0.5737(5) 0.2481(2) 0.39111(18) 0.0626(17) Uani 1 1 d . . . O6W O -0.2571(4) 0.14295(16) 0.22566(13) 0.0333(11) Uani 1 1 d . . . O7W O -0.2119(3) 0.30258(17) 0.28923(16) 0.0450(12) Uani 1 1 d . . . O8W O -0.2864(3) 0.17650(16) 0.33790(13) 0.0334(11) Uani 1 1 d . . . O9W O -0.2470(3) 0.2460(2) 0.19159(13) 0.0418(13) Uani 1 1 d . . . O10W O -0.0789(5) 0.2379(2) 0.3484(2) 0.0670(18) Uani 1 1 d . . . Sm1 Sm 0.69713(3) 0.272760(16) 0.469517(13) 0.04670(11) Uani 1 1 d . . . Sm2 Sm -0.20209(3) 0.216645(17) 0.271906(13) 0.04910(12) Uani 1 1 d . . . C1 C 0.0907(4) 0.38176(18) 0.43044(17) 0.0176(12) Uani 1 1 d . . . C2 C 0.2733(4) 0.39773(17) 0.48109(16) 0.0123(11) Uani 1 1 d . . . H2 H 0.2689 0.4216 0.5067 0.015 Uiso 1 1 calc R . . C3 C 0.2904(4) 0.42324(18) 0.43536(15) 0.0130(11) Uani 1 1 d . . . H3 H 0.3052 0.4593 0.4392 0.016 Uiso 1 1 calc R . . C4 C 0.4501(4) 0.36488(18) 0.45001(17) 0.0154(12) Uani 1 1 d . . . C5 C 0.1376(5) 0.43500(18) 0.36323(17) 0.0204(13) Uani 1 1 d . . . H5A H 0.1701 0.4691 0.3638 0.024 Uiso 1 1 calc R . . H5B H 0.0438 0.4366 0.3584 0.024 Uiso 1 1 calc R . . C6 C 0.4685(4) 0.41365(19) 0.37968(16) 0.0170(12) Uani 1 1 d . . . H6A H 0.4652 0.4499 0.3777 0.020 Uiso 1 1 calc R . . H6B H 0.5590 0.4040 0.3847 0.020 Uiso 1 1 calc R . . C7 C 0.3099(4) 0.41738(18) 0.30829(15) 0.0114(11) Uani 1 1 d . . . H7 H 0.3263 0.4529 0.3028 0.014 Uiso 1 1 calc R . . C8 C 0.3037(4) 0.38714(16) 0.26330(16) 0.0106(11) Uani 1 1 d . . . H8 H 0.3088 0.4087 0.2360 0.013 Uiso 1 1 calc R . . C9 C 0.1120(5) 0.37722(18) 0.29789(17) 0.0184(12) Uani 1 1 d . . . C10 C 0.4775(4) 0.35980(19) 0.31384(16) 0.0161(12) Uani 1 1 d . . . C11 C 0.1278(4) 0.33427(18) 0.22409(17) 0.0154(12) Uani 1 1 d . . . H11A H 0.1482 0.3510 0.1958 0.018 Uiso 1 1 calc R . . H11B H 0.0342 0.3345 0.2247 0.018 Uiso 1 1 calc R . . C12 C 0.4664(4) 0.32461(18) 0.23513(16) 0.0144(11) Uani 1 1 d . . . H12A H 0.5587 0.3196 0.2423 0.017 Uiso 1 1 calc R . . H12B H 0.4547 0.3428 0.2060 0.017 Uiso 1 1 calc R . . C13 C 0.0934(4) 0.24456(18) 0.22968(14) 0.0117(11) Uani 1 1 d . . . C14 C 0.2868(4) 0.26878(18) 0.20090(15) 0.0114(11) Uani 1 1 d . . . H14 H 0.2903 0.2834 0.1699 0.014 Uiso 1 1 calc R . . C15 C 0.2721(4) 0.21177(18) 0.19907(14) 0.0095(11) Uani 1 1 d . . . H15 H 0.2729 0.1993 0.1672 0.011 Uiso 1 1 calc R . . C16 C 0.0838(4) 0.15479(19) 0.21378(15) 0.0149(12) Uani 1 1 d . . . H16A H -0.0088 0.1611 0.2100 0.018 Uiso 1 1 calc R . . H16B H 0.1073 0.1373 0.1863 0.018 Uiso 1 1 calc R . . C17 C 0.4138(4) 0.14272(19) 0.23502(17) 0.0194(12) Uani 1 1 d . . . H17A H 0.5061 0.1394 0.2436 0.023 Uiso 1 1 calc R . . H17B H 0.3943 0.1250 0.2059 0.023 Uiso 1 1 calc R . . C18 C 0.0446(4) 0.12469(19) 0.29084(15) 0.0132(11) Uani 1 1 d . . . C19 C 0.4024(4) 0.10699(18) 0.31262(17) 0.0165(12) Uani 1 1 d . . . C20 C 0.2251(4) 0.09174(17) 0.26039(16) 0.0138(11) Uani 1 1 d . . . H20 H 0.2311 0.0680 0.2348 0.017 Uiso 1 1 calc R . . C21 C 0.2038(4) 0.06569(18) 0.30554(17) 0.0158(12) Uani 1 1 d . . . H21 H 0.1880 0.0298 0.3009 0.019 Uiso 1 1 calc R . . C23 C 0.0274(4) 0.07527(19) 0.36077(16) 0.0154(12) Uani 1 1 d . . . H23A H 0.0304 0.0390 0.3626 0.019 Uiso 1 1 calc R . . H23B H -0.0629 0.0850 0.3554 0.019 Uiso 1 1 calc R . . C24 C 0.3580(5) 0.0533(2) 0.37816(17) 0.0221(13) Uani 1 1 d . . . H24A H 0.4517 0.0514 0.3828 0.026 Uiso 1 1 calc R . . H24B H 0.3247 0.0193 0.3785 0.026 Uiso 1 1 calc R . . C25 C 0.0173(4) 0.13047(18) 0.42769(16) 0.0165(12) Uani 1 1 d . . . C26 C 0.1850(4) 0.07264(18) 0.43324(16) 0.0140(11) Uani 1 1 d . . . H26 H 0.1695 0.0371 0.4389 0.017 Uiso 1 1 calc R . . C27 C 0.1896(4) 0.10333(19) 0.47835(18) 0.0177(12) Uani 1 1 d . . . H27 H 0.1833 0.0819 0.5056 0.021 Uiso 1 1 calc R . . C28 C 0.3825(4) 0.11127(18) 0.44475(16) 0.0160(12) Uani 1 1 d . . . C29 C 0.0293(4) 0.16566(18) 0.50633(16) 0.0143(11) Uani 1 1 d . . . H29A H -0.0633 0.1702 0.4993 0.017 Uiso 1 1 calc R . . H29B H 0.0423 0.1478 0.5356 0.017 Uiso 1 1 calc R . . C30 C 0.3659(4) 0.1548(2) 0.51850(17) 0.0197(13) Uani 1 1 d . . . H30A H 0.4596 0.1542 0.5188 0.024 Uiso 1 1 calc R . . H30B H 0.3426 0.1383 0.5466 0.024 Uiso 1 1 calc R . . C31 C 0.2091(4) 0.22101(18) 0.54090(14) 0.0109(11) Uani 1 1 d . . . H31 H 0.2055 0.2062 0.5719 0.013 Uiso 1 1 calc R . . C32 C 0.2200(4) 0.27780(18) 0.54268(15) 0.0129(11) Uani 1 1 d . . . H32 H 0.2195 0.2906 0.5745 0.015 Uiso 1 1 calc R . . C34 C 0.3995(4) 0.2444(2) 0.51150(14) 0.0148(12) Uani 1 1 d . . . C35 C 0.0795(4) 0.34665(19) 0.50692(16) 0.0171(12) Uani 1 1 d . . . H35A H 0.0981 0.3643 0.5361 0.020 Uiso 1 1 calc R . . H35B H -0.0128 0.3495 0.4982 0.020 Uiso 1 1 calc R . . C36 C 0.4139(4) 0.33272(19) 0.52728(15) 0.0168(12) Uani 1 1 d . . . H36A H 0.5062 0.3258 0.5302 0.020 Uiso 1 1 calc R . . H36B H 0.3926 0.3497 0.5554 0.020 Uiso 1 1 calc R . . C37 C 0.0340(4) 0.2564(2) 0.49854(15) 0.0143(11) Uani 1 1 d . . . C38 C 0.4630(4) 0.23281(17) 0.24363(14) 0.0082(10) Uani 1 1 d . . . N1 N 0.3119(3) 0.12751(16) 0.47929(14) 0.0168(10) Uani 1 1 d . . . N2 N 0.3098(3) 0.08090(15) 0.41660(14) 0.0163(10) Uani 1 1 d . . . N3 N 0.3228(3) 0.07483(16) 0.33369(14) 0.0180(10) Uani 1 1 d . . . N4 N 0.3439(3) 0.11956(15) 0.27038(14) 0.0158(10) Uani 1 1 d . . . N5 N 0.3839(3) 0.19384(15) 0.22823(13) 0.0140(10) Uani 1 1 d . . . N6 N 0.4039(3) 0.27611(14) 0.22919(12) 0.0085(9) Uani 1 1 d . . . N7 N 0.4181(3) 0.35389(15) 0.27059(13) 0.0116(9) Uani 1 1 d . . . N8 N 0.4178(3) 0.39387(15) 0.33761(13) 0.0122(9) Uani 1 1 d . . . N9 N 0.4023(3) 0.39794(14) 0.41976(12) 0.0116(9) Uani 1 1 d . . . N10 N 0.3835(3) 0.36524(15) 0.48768(13) 0.0133(10) Uani 1 1 d . . . N12 N 0.3453(3) 0.28718(15) 0.52296(13) 0.0117(9) Uani 1 1 d . . . N13 N 0.3232(3) 0.20542(14) 0.51889(12) 0.0080(9) Uani 1 1 d . . . N14 N 0.1122(3) 0.29549(14) 0.51337(13) 0.0110(9) Uani 1 1 d . . . N15 N 0.0892(3) 0.21365(16) 0.51158(13) 0.0144(10) Uani 1 1 d . . . N16 N 0.0784(3) 0.13603(15) 0.47062(14) 0.0137(10) Uani 1 1 d . . . N17 N 0.0784(3) 0.09533(15) 0.40409(13) 0.0138(10) Uani 1 1 d . . . N18 N 0.0931(3) 0.09068(15) 0.32245(13) 0.0128(9) Uani 1 1 d . . . N19 N 0.1118(3) 0.12367(14) 0.25324(13) 0.0116(9) Uani 1 1 d . . . N20 N 0.1515(3) 0.20199(14) 0.21727(13) 0.0112(9) Uani 1 1 d . . . N21 N 0.1704(3) 0.28386(15) 0.22243(13) 0.0128(10) Uani 1 1 d . . . N22 N 0.1822(3) 0.36158(15) 0.26223(14) 0.0154(10) Uani 1 1 d . . . N23 N 0.1853(3) 0.40946(16) 0.32530(14) 0.0182(10) Uani 1 1 d . . . N24 N 0.1721(4) 0.41270(16) 0.40675(13) 0.0171(10) Uani 1 1 d . . . N25 N 0.1511(3) 0.37012(15) 0.47108(14) 0.0150(10) Uani 1 1 d . . . O1 O -0.0118(3) 0.24706(14) 0.24445(11) 0.0190(9) Uani 1 1 d . . . O2 O -0.0006(3) 0.36574(14) 0.30167(13) 0.0251(10) Uani 1 1 d . . . O3 O -0.0148(3) 0.37090(15) 0.41358(14) 0.0319(11) Uani 1 1 d . . . O4 O -0.0800(3) 0.15320(13) 0.41260(11) 0.0180(9) Uani 1 1 d . . . O5 O -0.0524(3) 0.15052(14) 0.29545(11) 0.0195(9) Uani 1 1 d . . . O6 O 0.5091(3) 0.11851(17) 0.32870(15) 0.0397(12) Uani 1 1 d . . . O7 O 0.4969(3) 0.12365(15) 0.43969(14) 0.0292(10) Uani 1 1 d . . . O8 O 0.5081(3) 0.24093(14) 0.49626(12) 0.0206(9) Uani 1 1 d . . . O9 O 0.5473(3) 0.33781(13) 0.44539(12) 0.0205(9) Uani 1 1 d . . . O10 O 0.5781(3) 0.33696(14) 0.32905(11) 0.0199(9) Uani 1 1 d . . . O11 O 0.5694(3) 0.22828(13) 0.26537(11) 0.0166(9) Uani 1 1 d . . . O12 O -0.0736(3) 0.26115(13) 0.47636(11) 0.0168(9) 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 Cl9 0.0220(7) 0.1198(16) 0.0244(7) -0.0105(9) -0.0046(6) 0.0063(9) Cl10 0.0259(7) 0.1484(19) 0.0227(7) -0.0088(10) -0.0033(6) 0.0183(10) Cl1 0.0552(9) 0.0356(9) 0.0323(7) -0.0007(6) 0.0102(7) -0.0139(7) Cl2 0.139(2) 0.0882(16) 0.0877(17) 0.0187(14) -0.0265(16) -0.0633(15) Cl3 0.1477(15) 0.1124(17) 0.1480(17) -0.0737(14) 0.1047(13) -0.0873(13) Cl4 0.0572(14) 0.0801(18) 0.239(4) 0.041(2) 0.0143(19) 0.0123(13) Cl5 0.1437(18) 0.0699(14) 0.0597(11) -0.0103(10) 0.0485(11) -0.0391(13) Cl6 0.185(2) 0.0992(18) 0.133(2) -0.0461(15) 0.0895(17) -0.0832(16) Cl7 0.0898(18) 0.120(3) 0.478(8) 0.077(4) 0.110(3) 0.038(2) Cl8 0.217(3) 0.196(3) 0.123(2) 0.066(2) -0.038(2) -0.144(2) Zn1 0.0552(5) 0.0387(5) 0.0612(5) 0.0023(4) 0.0067(4) -0.0092(4) Zn2 0.0867(7) 0.0651(7) 0.0846(7) 0.0037(6) 0.0189(6) -0.0150(6) O1W 0.0096(16) 0.060(3) 0.0278(19) 0.0116(19) -0.0032(15) 0.0015(18) O2W 0.0199(17) 0.029(2) 0.034(2) -0.0148(17) -0.0124(16) 0.0029(16) O3W 0.0028(15) 0.046(2) 0.064(3) -0.025(2) 0.0090(16) 0.0019(16) O4W 0.0185(18) 0.072(3) 0.0209(18) 0.004(2) -0.0136(15) -0.013(2) O5W 0.045(3) 0.078(4) 0.065(3) -0.014(3) 0.007(2) 0.012(3) O6W 0.0214(18) 0.046(3) 0.030(2) -0.0174(18) -0.0112(16) 0.0049(18) O7W 0.0146(17) 0.053(3) 0.069(3) -0.039(2) 0.0135(18) -0.0016(18) O8W 0.0143(16) 0.057(3) 0.0293(19) 0.0153(19) 0.0058(15) 0.0073(18) O9W 0.0061(16) 0.093(3) 0.0244(19) 0.015(2) -0.0104(14) -0.008(2) O10W 0.046(3) 0.080(4) 0.076(4) -0.013(3) 0.006(3) 0.006(3) Sm1 0.02443(16) 0.0689(3) 0.0465(2) -0.00039(18) 0.00105(15) 0.00179(16) Sm2 0.02675(17) 0.0728(3) 0.0476(2) -0.00026(19) 0.00194(15) 0.00226(17) C1 0.012(2) 0.014(2) 0.026(2) -0.004(2) -0.0003(19) -0.0017(19) C2 0.0011(18) 0.008(2) 0.026(2) -0.0056(19) -0.0070(17) 0.0009(17) C3 0.0075(19) 0.013(2) 0.019(2) -0.0072(19) 0.0018(17) 0.0001(18) C4 0.0000(18) 0.014(2) 0.032(2) -0.016(2) 0.0003(18) -0.0041(17) C5 0.017(2) 0.011(2) 0.032(3) -0.008(2) -0.005(2) 0.0151(19) C6 0.0039(19) 0.018(3) 0.028(2) 0.001(2) -0.0048(18) -0.0107(18) C7 0.0019(18) 0.011(2) 0.020(2) 0.0074(19) -0.0043(17) 0.0004(17) C8 0.0072(19) 0.005(2) 0.019(2) 0.0043(18) -0.0042(17) 0.0001(17) C9 0.016(2) 0.012(2) 0.026(2) 0.003(2) -0.004(2) 0.0075(19) C10 0.0041(19) 0.020(3) 0.023(2) 0.005(2) -0.0036(18) -0.0061(18) C11 0.0037(19) 0.014(2) 0.027(2) 0.003(2) -0.0046(18) 0.0086(18) C12 0.0000(18) 0.017(2) 0.027(2) 0.000(2) 0.0024(17) -0.0088(17) C13 0.0016(18) 0.022(3) 0.0112(19) -0.0067(19) -0.0011(15) -0.0009(18) C14 0.0000(17) 0.022(3) 0.013(2) -0.0005(18) 0.0065(15) -0.0042(17) C15 0.0000(17) 0.027(3) 0.0015(17) -0.0035(18) -0.0024(14) 0.0028(17) C16 0.0026(18) 0.026(3) 0.015(2) -0.013(2) -0.0051(16) -0.0032(19) C17 0.0054(19) 0.024(3) 0.030(2) 0.000(2) 0.0097(18) -0.0007(19) C18 0.0031(19) 0.024(3) 0.012(2) -0.0054(19) -0.0032(16) 0.0008(18) C19 0.011(2) 0.014(2) 0.024(2) 0.005(2) -0.0002(18) -0.0024(19) C20 0.016(2) 0.005(2) 0.021(2) -0.0056(18) 0.0006(18) -0.0031(18) C21 0.0000(18) 0.011(2) 0.036(3) -0.006(2) -0.0006(18) 0.0049(17) C23 0.0054(19) 0.019(3) 0.022(2) 0.001(2) -0.0002(17) -0.0086(18) C24 0.015(2) 0.021(3) 0.032(3) 0.004(2) 0.009(2) 0.010(2) C25 0.017(2) 0.015(2) 0.019(2) 0.0067(19) 0.0039(18) -0.0083(19) C26 0.009(2) 0.008(2) 0.025(2) 0.0032(19) 0.0046(18) -0.0004(17) C27 0.0025(19) 0.016(2) 0.033(3) 0.014(2) -0.0037(18) 0.0017(18) C28 0.009(2) 0.015(2) 0.025(2) 0.001(2) 0.0038(18) 0.0073(18) C29 0.0014(18) 0.015(2) 0.027(2) 0.003(2) 0.0054(17) -0.0021(17) C30 0.005(2) 0.031(3) 0.023(2) -0.003(2) -0.0041(18) -0.001(2) C31 0.0000(18) 0.027(3) 0.0049(19) -0.0023(18) -0.0074(15) -0.0049(18) C32 0.0027(19) 0.024(3) 0.012(2) 0.0061(19) 0.0020(16) 0.0019(18) C34 0.0000(18) 0.042(3) 0.0022(18) 0.004(2) -0.0023(14) 0.003(2) C35 0.0000(18) 0.030(3) 0.022(2) -0.002(2) 0.0016(17) 0.0015(19) C36 0.012(2) 0.030(3) 0.007(2) -0.0059(19) -0.0020(17) -0.009(2) C37 0.0000(18) 0.031(3) 0.012(2) 0.000(2) 0.0016(15) -0.0021(19) C38 0.0050(18) 0.015(2) 0.0055(17) -0.0008(17) 0.0069(15) -0.0041(16) N1 0.0072(17) 0.019(2) 0.024(2) 0.0028(17) -0.0004(15) -0.0068(16) N2 0.0087(17) 0.016(2) 0.026(2) -0.0020(17) 0.0102(15) -0.0020(16) N3 0.0015(16) 0.023(2) 0.029(2) 0.0044(19) -0.0011(15) -0.0013(16) N4 0.0013(16) 0.017(2) 0.028(2) -0.0008(18) -0.0016(15) -0.0086(15) N5 0.0000(15) 0.023(2) 0.0180(19) -0.0020(17) -0.0050(14) 0.0026(15) N6 0.0000(15) 0.013(2) 0.0117(17) 0.0028(15) -0.0059(13) 0.0003(14) N7 0.0027(16) 0.015(2) 0.0163(18) -0.0030(16) -0.0027(14) 0.0016(15) N8 0.0004(15) 0.015(2) 0.0196(19) 0.0007(16) -0.0087(14) 0.0046(15) N9 0.0064(16) 0.014(2) 0.0142(18) 0.0047(16) -0.0007(14) 0.0078(15) N10 0.0005(15) 0.020(2) 0.0186(19) 0.0013(17) -0.0052(14) 0.0013(15) N12 0.0000(15) 0.020(2) 0.0153(18) -0.0005(16) -0.0013(14) 0.0008(15) N13 0.0000(15) 0.0129(19) 0.0110(16) -0.0040(15) -0.0004(13) -0.0015(14) N14 0.0000(15) 0.013(2) 0.0191(18) 0.0029(16) -0.0050(14) 0.0020(14) N15 0.0000(16) 0.026(2) 0.0178(19) 0.0061(17) 0.0008(14) -0.0005(15) N16 0.0021(16) 0.013(2) 0.025(2) 0.0044(17) -0.0043(15) 0.0021(15) N17 0.0090(17) 0.014(2) 0.0177(19) 0.0023(16) -0.0032(15) 0.0056(15) N18 0.0000(15) 0.018(2) 0.0210(19) -0.0060(16) 0.0018(14) 0.0055(15) N19 0.0056(16) 0.0107(19) 0.0191(18) -0.0041(16) 0.0049(14) 0.0005(14) N20 0.0000(15) 0.0087(19) 0.0249(19) -0.0029(16) 0.0005(14) -0.0033(14) N21 0.0000(15) 0.017(2) 0.0215(19) -0.0049(16) 0.0017(14) 0.0019(14) N22 0.0057(17) 0.014(2) 0.026(2) -0.0002(17) -0.0024(15) 0.0015(15) N23 0.0029(16) 0.018(2) 0.035(2) -0.0003(18) 0.0079(16) -0.0012(15) N24 0.0087(17) 0.021(2) 0.020(2) 0.0050(18) -0.0101(15) 0.0068(16) N25 0.0001(16) 0.014(2) 0.030(2) 0.0037(17) -0.0060(15) -0.0051(15) O1 0.0000(13) 0.032(2) 0.0242(17) 0.0003(16) -0.0017(12) 0.0043(14) O2 0.0026(14) 0.030(2) 0.043(2) -0.0103(17) 0.0059(14) -0.0058(14) O3 0.0130(17) 0.037(2) 0.043(2) 0.0125(19) -0.0151(16) -0.0147(16) O4 0.0080(14) 0.0246(19) 0.0203(16) -0.0019(15) -0.0052(13) 0.0101(14) O5 0.0041(14) 0.033(2) 0.0215(17) 0.0007(15) 0.0015(12) 0.0108(14) O6 0.0117(17) 0.049(3) 0.056(3) 0.016(2) -0.0091(18) -0.0107(18) O7 0.0054(15) 0.037(2) 0.045(2) -0.0137(18) 0.0039(15) -0.0067(15) O8 0.0013(14) 0.032(2) 0.0282(18) -0.0064(16) -0.0004(13) 0.0022(14) O9 0.0043(14) 0.028(2) 0.0289(18) -0.0018(16) -0.0013(13) 0.0093(14) O10 0.0067(14) 0.030(2) 0.0221(17) -0.0033(15) -0.0048(13) 0.0069(14) O11 0.0000(13) 0.0268(19) 0.0216(17) -0.0034(14) -0.0072(12) 0.0014(13) O12 0.0000(13) 0.0219(18) 0.0270(17) 0.0018(15) -0.0070(12) 0.0032(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 Zn1 2.2314(19) . ? Cl2 Zn1 2.257(3) . ? Cl3 Zn1 2.247(3) . ? Cl4 Zn1 2.258(3) . ? Cl5 Zn2 2.229(3) . ? Cl6 Zn2 2.255(3) . ? Cl7 Zn2 2.227(4) . ? Cl8 Zn2 2.253(4) . ? O1W Sm1 2.415(4) . ? O2W Sm1 2.397(4) . ? O3W Sm1 2.415(4) . ? O4W Sm1 2.457(4) . ? O5W Sm1 2.615(5) . ? O6W Sm2 2.444(4) . ? O7W Sm2 2.378(4) . ? O8W Sm2 2.437(4) . ? O9W Sm2 2.479(4) . ? O10W Sm2 2.544(6) . ? Sm1 O8 2.348(3) . ? Sm1 O12 2.409(3) 1_655 ? Sm1 O9 2.418(3) . ? Sm2 O1 2.355(3) . ? Sm2 O11 2.402(3) 1_455 ? Sm2 O5 2.434(3) . ? C1 O3 1.205(6) . ? C1 N25 1.332(6) . ? C1 N24 1.413(6) . ? C2 N10 1.449(6) . ? C2 N25 1.486(5) . ? C2 C3 1.524(7) . ? C2 H2 0.9900 . ? C3 N9 1.460(6) . ? C3 N24 1.461(6) . ? C3 H3 0.9900 . ? C4 O9 1.268(5) . ? C4 N9 1.322(6) . ? C4 N10 1.349(6) . ? C5 N24 1.423(6) . ? C5 N23 1.428(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N8 1.400(6) . ? C6 N9 1.470(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 N23 1.449(5) . ? C7 N8 1.497(5) . ? C7 C8 1.541(6) . ? C7 H7 0.9900 . ? C8 N22 1.444(6) . ? C8 N7 1.496(5) . ? C8 H8 0.9900 . ? C9 O2 1.231(6) . ? C9 N23 1.371(6) . ? C9 N22 1.388(6) . ? C10 O10 1.267(6) . ? C10 N8 1.338(6) . ? C10 N7 1.367(6) . ? C11 N22 1.413(6) . ? C11 N21 1.434(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N7 1.427(6) . ? C12 N6 1.467(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O1 1.216(5) . ? C13 N21 1.359(6) . ? C13 N20 1.363(6) . ? C14 N6 1.432(5) . ? C14 N21 1.473(5) . ? C14 C15 1.547(7) . ? C14 H14 0.9900 . ? C15 N20 1.434(5) . ? C15 N5 1.468(5) . ? C15 H15 0.9900 . ? C16 N19 1.434(6) . ? C16 N20 1.457(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 N5 1.425(7) . ? C17 N4 1.454(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 O5 1.248(5) . ? C18 N19 1.352(6) . ? C18 N18 1.367(6) . ? C19 O6 1.214(6) . ? C19 N4 1.371(6) . ? C19 N3 1.382(6) . ? C20 N4 1.460(6) . ? C20 N19 1.465(6) . ? C20 C21 1.525(7) . ? C20 H20 0.9900 . ? C21 N3 1.452(6) . ? C21 N18 1.461(6) . ? C21 H21 0.9900 . ? C23 N18 1.422(6) . ? C23 N17 1.435(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N3 1.440(6) . ? C24 N2 1.470(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O4 1.237(6) . ? C25 N17 1.362(6) . ? C25 N16 1.364(6) . ? C26 N2 1.448(6) . ? C26 N17 1.477(6) . ? C26 C27 1.551(7) . ? C26 H26 0.9900 . ? C27 N1 1.434(6) . ? C27 N16 1.462(6) . ? C27 H27 0.9900 . ? C28 O7 1.262(6) . ? C28 N2 1.348(6) . ? C28 N1 1.370(6) . ? C29 N15 1.441(6) . ? C29 N16 1.441(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N1 1.434(6) . ? C30 N13 1.438(6) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 N13 1.464(5) . ? C31 N15 1.470(5) . ? C31 C32 1.538(7) . ? C31 H31 0.9900 . ? C32 N14 1.437(5) . ? C32 N12 1.496(5) . ? C32 H32 0.9900 . ? C34 O8 1.258(5) . ? C34 N12 1.341(6) . ? C34 N13 1.348(6) . ? C35 N14 1.431(6) . ? C35 N25 1.479(6) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N12 1.423(6) . ? C36 N10 1.464(6) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 O12 1.256(5) . ? C37 N15 1.331(6) . ? C37 N14 1.382(6) . ? C38 O11 1.239(5) . ? C38 N6 1.371(6) . ? C38 N5 1.389(6) . ? O11 Sm2 2.402(3) 1_655 ? O12 Sm1 2.409(3) 1_455 ? 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 Cl1 Zn1 Cl3 108.08(9) . . ? Cl1 Zn1 Cl2 111.73(9) . . ? Cl3 Zn1 Cl2 112.25(11) . . ? Cl1 Zn1 Cl4 108.98(9) . . ? Cl3 Zn1 Cl4 110.57(13) . . ? Cl2 Zn1 Cl4 105.19(13) . . ? Cl7 Zn2 Cl5 111.91(13) . . ? Cl7 Zn2 Cl8 104.23(19) . . ? Cl5 Zn2 Cl8 108.59(12) . . ? Cl7 Zn2 Cl6 109.96(18) . . ? Cl5 Zn2 Cl6 111.11(11) . . ? Cl8 Zn2 Cl6 110.83(14) . . ? O8 Sm1 O2W 107.02(13) . . ? O8 Sm1 O12 141.69(12) . 1_655 ? O2W Sm1 O12 82.59(12) . 1_655 ? O8 Sm1 O1W 142.88(11) . . ? O2W Sm1 O1W 88.18(14) . . ? O12 Sm1 O1W 72.39(12) 1_655 . ? O8 Sm1 O3W 75.45(12) . . ? O2W Sm1 O3W 152.26(13) . . ? O12 Sm1 O3W 79.83(11) 1_655 . ? O1W Sm1 O3W 106.53(14) . . ? O8 Sm1 O9 79.58(12) . . ? O2W Sm1 O9 71.28(12) . . ? O12 Sm1 O9 137.26(12) 1_655 . ? O1W Sm1 O9 73.53(12) . . ? O3W Sm1 O9 134.95(12) . . ? O8 Sm1 O4W 70.90(12) . . ? O2W Sm1 O4W 75.10(15) . . ? O12 Sm1 O4W 76.36(12) 1_655 . ? O1W Sm1 O4W 146.16(12) . . ? O3W Sm1 O4W 79.99(15) . . ? O9 Sm1 O4W 125.55(13) . . ? O8 Sm1 O5W 80.18(14) . . ? O2W Sm1 O5W 139.20(16) . . ? O12 Sm1 O5W 116.99(14) 1_655 . ? O1W Sm1 O5W 67.16(15) . . ? O3W Sm1 O5W 68.45(16) . . ? O9 Sm1 O5W 70.77(15) . . ? O4W Sm1 O5W 141.59(17) . . ? O1 Sm2 O7W 77.58(13) . . ? O1 Sm2 O11 142.31(12) . 1_455 ? O7W Sm2 O11 80.14(12) . 1_455 ? O1 Sm2 O5 79.02(12) . . ? O7W Sm2 O5 133.92(13) . . ? O11 Sm2 O5 136.89(11) 1_455 . ? O1 Sm2 O8W 142.73(11) . . ? O7W Sm2 O8W 103.95(15) . . ? O11 Sm2 O8W 72.35(12) 1_455 . ? O5 Sm2 O8W 73.64(12) . . ? O1 Sm2 O6W 105.23(13) . . ? O7W Sm2 O6W 153.97(14) . . ? O11 Sm2 O6W 82.90(12) 1_455 . ? O5 Sm2 O6W 71.01(12) . . ? O8W Sm2 O6W 89.40(14) . . ? O1 Sm2 O9W 70.48(11) . . ? O7W Sm2 O9W 83.15(17) . . ? O11 Sm2 O9W 77.02(11) 1_455 . ? O5 Sm2 O9W 124.52(13) . . ? O8W Sm2 O9W 146.66(12) . . ? O6W Sm2 O9W 73.86(15) . . ? O1 Sm2 O10W 80.72(15) . . ? O7W Sm2 O10W 67.76(17) . . ? O11 Sm2 O10W 117.84(14) 1_455 . ? O5 Sm2 O10W 69.66(16) . . ? O8W Sm2 O10W 66.37(16) . . ? O6W Sm2 O10W 138.17(17) . . ? O9W Sm2 O10W 142.83(18) . . ? O3 C1 N25 130.9(5) . . ? O3 C1 N24 120.8(4) . . ? N25 C1 N24 108.3(4) . . ? N10 C2 N25 112.6(4) . . ? N10 C2 C3 103.8(4) . . ? N25 C2 C3 102.5(3) . . ? N10 C2 H2 112.4 . . ? N25 C2 H2 112.4 . . ? C3 C2 H2 112.4 . . ? N9 C3 N24 113.2(4) . . ? N9 C3 C2 102.6(4) . . ? N24 C3 C2 104.8(4) . . ? N9 C3 H3 111.9 . . ? N24 C3 H3 111.9 . . ? C2 C3 H3 111.9 . . ? O9 C4 N9 125.4(4) . . ? O9 C4 N10 124.3(4) . . ? N9 C4 N10 110.2(4) . . ? N24 C5 N23 114.0(4) . . ? N24 C5 H5A 108.7 . . ? N23 C5 H5A 108.7 . . ? N24 C5 H5B 108.7 . . ? N23 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? N8 C6 N9 114.7(4) . . ? N8 C6 H6A 108.6 . . ? N9 C6 H6A 108.6 . . ? N8 C6 H6B 108.6 . . ? N9 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? N23 C7 N8 113.5(4) . . ? N23 C7 C8 103.8(3) . . ? N8 C7 C8 103.7(3) . . ? N23 C7 H7 111.8 . . ? N8 C7 H7 111.8 . . ? C8 C7 H7 111.8 . . ? N22 C8 N7 114.1(4) . . ? N22 C8 C7 104.2(4) . . ? N7 C8 C7 102.8(3) . . ? N22 C8 H8 111.7 . . ? N7 C8 H8 111.7 . . ? C7 C8 H8 111.7 . . ? O2 C9 N23 126.8(5) . . ? O2 C9 N22 124.1(4) . . ? N23 C9 N22 108.9(4) . . ? O10 C10 N8 124.3(4) . . ? O10 C10 N7 124.4(4) . . ? N8 C10 N7 111.2(4) . . ? N22 C11 N21 114.6(4) . . ? N22 C11 H11A 108.6 . . ? N21 C11 H11A 108.6 . . ? N22 C11 H11B 108.6 . . ? N21 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? N7 C12 N6 113.5(4) . . ? N7 C12 H12A 108.9 . . ? N6 C12 H12A 108.9 . . ? N7 C12 H12B 108.9 . . ? N6 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? O1 C13 N21 125.3(5) . . ? O1 C13 N20 125.3(4) . . ? N21 C13 N20 109.5(4) . . ? N6 C14 N21 114.5(4) . . ? N6 C14 C15 103.6(3) . . ? N21 C14 C15 101.9(3) . . ? N6 C14 H14 112.0 . . ? N21 C14 H14 112.0 . . ? C15 C14 H14 112.0 . . ? N20 C15 N5 114.0(4) . . ? N20 C15 C14 104.9(3) . . ? N5 C15 C14 103.7(3) . . ? N20 C15 H15 111.2 . . ? N5 C15 H15 111.2 . . ? C14 C15 H15 111.3 . . ? N19 C16 N20 113.0(3) . . ? N19 C16 H16A 109.0 . . ? N20 C16 H16A 109.0 . . ? N19 C16 H16B 109.0 . . ? N20 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? N5 C17 N4 113.4(4) . . ? N5 C17 H17A 108.9 . . ? N4 C17 H17A 108.9 . . ? N5 C17 H17B 108.9 . . ? N4 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? O5 C18 N19 125.6(4) . . ? O5 C18 N18 124.1(4) . . ? N19 C18 N18 110.1(4) . . ? O6 C19 N4 127.6(5) . . ? O6 C19 N3 123.9(5) . . ? N4 C19 N3 108.4(4) . . ? N4 C20 N19 112.9(4) . . ? N4 C20 C21 104.4(4) . . ? N19 C20 C21 102.7(4) . . ? N4 C20 H20 112.1 . . ? N19 C20 H20 112.1 . . ? C21 C20 H20 112.1 . . ? N3 C21 N18 113.3(4) . . ? N3 C21 C20 103.3(4) . . ? N18 C21 C20 104.8(4) . . ? N3 C21 H21 111.6 . . ? N18 C21 H21 111.6 . . ? C20 C21 H21 111.6 . . ? N18 C23 N17 114.3(4) . . ? N18 C23 H23A 108.7 . . ? N17 C23 H23A 108.7 . . ? N18 C23 H23B 108.7 . . ? N17 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? N3 C24 N2 113.8(4) . . ? N3 C24 H24A 108.8 . . ? N2 C24 H24A 108.8 . . ? N3 C24 H24B 108.8 . . ? N2 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? O4 C25 N17 124.9(4) . . ? O4 C25 N16 125.4(4) . . ? N17 C25 N16 109.7(4) . . ? N2 C26 N17 113.7(4) . . ? N2 C26 C27 103.8(4) . . ? N17 C26 C27 103.5(4) . . ? N2 C26 H26 111.8 . . ? N17 C26 H26 111.8 . . ? C27 C26 H26 111.8 . . ? N1 C27 N16 115.1(4) . . ? N1 C27 C26 102.9(4) . . ? N16 C27 C26 103.0(4) . . ? N1 C27 H27 111.7 . . ? N16 C27 H27 111.7 . . ? C26 C27 H27 111.7 . . ? O7 C28 N2 125.5(4) . . ? O7 C28 N1 125.2(4) . . ? N2 C28 N1 109.3(4) . . ? N15 C29 N16 113.4(4) . . ? N15 C29 H29A 108.9 . . ? N16 C29 H29A 108.9 . . ? N15 C29 H29B 108.9 . . ? N16 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? N1 C30 N13 113.1(4) . . ? N1 C30 H30A 109.0 . . ? N13 C30 H30A 109.0 . . ? N1 C30 H30B 109.0 . . ? N13 C30 H30B 109.0 . . ? H30A C30 H30B 107.8 . . ? N13 C31 N15 113.2(3) . . ? N13 C31 C32 103.9(3) . . ? N15 C31 C32 102.2(3) . . ? N13 C31 H31 112.3 . . ? N15 C31 H31 112.3 . . ? C32 C31 H31 112.3 . . ? N14 C32 N12 112.6(4) . . ? N14 C32 C31 105.0(3) . . ? N12 C32 C31 102.7(3) . . ? N14 C32 H32 112.0 . . ? N12 C32 H32 112.0 . . ? C31 C32 H32 112.0 . . ? O8 C34 N12 124.4(5) . . ? O8 C34 N13 124.2(5) . . ? N12 C34 N13 111.4(4) . . ? N14 C35 N25 112.1(4) . . ? N14 C35 H35A 109.2 . . ? N25 C35 H35A 109.2 . . ? N14 C35 H35B 109.2 . . ? N25 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? N12 C36 N10 112.0(4) . . ? N12 C36 H36A 109.2 . . ? N10 C36 H36A 109.2 . . ? N12 C36 H36B 109.2 . . ? N10 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? O12 C37 N15 125.7(5) . . ? O12 C37 N14 124.3(5) . . ? N15 C37 N14 110.0(4) . . ? O11 C38 N6 127.1(4) . . ? O11 C38 N5 125.1(4) . . ? N6 C38 N5 107.8(3) . . ? C28 N1 C27 112.1(4) . . ? C28 N1 C30 123.3(4) . . ? C27 N1 C30 122.6(4) . . ? C28 N2 C26 111.6(4) . . ? C28 N2 C24 124.1(4) . . ? C26 N2 C24 123.6(4) . . ? C19 N3 C24 122.4(4) . . ? C19 N3 C21 112.0(4) . . ? C24 N3 C21 125.6(4) . . ? C19 N4 C17 122.0(4) . . ? C19 N4 C20 111.1(4) . . ? C17 N4 C20 123.4(4) . . ? C38 N5 C17 124.8(4) . . ? C38 N5 C15 111.2(4) . . ? C17 N5 C15 123.7(4) . . ? C38 N6 C14 113.6(4) . . ? C38 N6 C12 122.7(3) . . ? C14 N6 C12 122.9(4) . . ? C10 N7 C12 124.9(4) . . ? C10 N7 C8 110.9(4) . . ? C12 N7 C8 123.8(3) . . ? C10 N8 C6 123.8(4) . . ? C10 N8 C7 111.0(4) . . ? C6 N8 C7 123.4(4) . . ? C4 N9 C3 112.1(4) . . ? C4 N9 C6 123.2(4) . . ? C3 N9 C6 123.8(4) . . ? C4 N10 C2 110.9(4) . . ? C4 N10 C36 123.0(4) . . ? C2 N10 C36 125.8(4) . . ? C34 N12 C36 123.1(4) . . ? C34 N12 C32 110.6(4) . . ? C36 N12 C32 124.3(4) . . ? C34 N13 C30 123.5(4) . . ? C34 N13 C31 111.2(4) . . ? C30 N13 C31 122.8(4) . . ? C37 N14 C35 124.6(4) . . ? C37 N14 C32 110.2(4) . . ? C35 N14 C32 124.4(4) . . ? C37 N15 C29 125.1(4) . . ? C37 N15 C31 112.1(4) . . ? C29 N15 C31 121.7(4) . . ? C25 N16 C29 123.8(4) . . ? C25 N16 C27 112.3(4) . . ? C29 N16 C27 123.4(4) . . ? C25 N17 C23 123.5(4) . . ? C25 N17 C26 111.2(4) . . ? C23 N17 C26 123.8(4) . . ? C18 N18 C23 123.3(4) . . ? C18 N18 C21 110.0(4) . . ? C23 N18 C21 125.4(4) . . ? C18 N19 C16 123.6(4) . . ? C18 N19 C20 111.5(4) . . ? C16 N19 C20 124.5(4) . . ? C13 N20 C15 111.7(4) . . ? C13 N20 C16 122.1(4) . . ? C15 N20 C16 124.9(4) . . ? C13 N21 C11 123.0(4) . . ? C13 N21 C14 111.9(4) . . ? C11 N21 C14 123.2(4) . . ? C9 N22 C11 123.0(4) . . ? C9 N22 C8 111.0(4) . . ? C11 N22 C8 124.2(4) . . ? C9 N23 C5 122.9(4) . . ? C9 N23 C7 111.7(4) . . ? C5 N23 C7 125.2(4) . . ? C1 N24 C5 124.6(4) . . ? C1 N24 C3 110.6(4) . . ? C5 N24 C3 124.4(4) . . ? C1 N25 C35 119.9(4) . . ? C1 N25 C2 113.1(4) . . ? C35 N25 C2 123.7(4) . . ? C13 O1 Sm2 156.4(4) . . ? C18 O5 Sm2 152.7(3) . . ? C34 O8 Sm1 154.3(4) . . ? C4 O9 Sm1 153.3(3) . . ? C38 O11 Sm2 153.9(3) . 1_655 ? C37 O12 Sm1 153.9(3) . 1_455 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.839 _refine_diff_density_min -1.715 _refine_diff_density_rms 0.362 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.006 0.000 -0.006 1040 532 ' ' 2 0.248 0.244 0.371 89 33 ' ' 3 0.248 0.255 0.871 89 32 ' ' 4 0.665 0.500 0.132 1040 527 ' ' 5 0.752 0.744 0.129 89 32 ' ' 6 0.752 0.756 0.629 89 31 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 902616' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p307 #TrackingRef 'submit-307.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H98 Cl10 Eu2 N24 O43 Zn2' _chemical_formula_weight 2344.54 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 '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 10.3737(18) _cell_length_b 27.124(5) _cell_length_c 29.044(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.595(6) _cell_angle_gamma 90.00 _cell_volume 8133(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.915 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4728 _exptl_absorpt_coefficient_mu 2.540 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5693 _exptl_absorpt_correction_T_max 0.6578 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 70955 _diffrn_reflns_av_R_equivalents 0.0671 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14262 _reflns_number_gt 10891 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0994P)^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 14262 _refine_ls_number_parameters 865 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1615 _refine_ls_wR_factor_gt 0.1541 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 Cl9 Cl 0.4864(2) 0.25268(12) 0.12068(7) 0.0772(7) Uani 1 1 d . . . Cl10 Cl 1.0150(2) 0.24640(14) -0.37879(8) 0.0944(10) Uani 1 1 d . . . Cl1 Cl 1.2544(2) -0.10740(8) -0.11769(6) 0.0558(5) Uani 1 1 d . . . Cl2 Cl 1.0385(4) -0.02341(13) -0.18998(11) 0.1263(14) Uani 1 1 d . . . Cl3 Cl 1.0162(4) -0.03452(13) -0.06297(13) 0.1470(18) Uani 1 1 d . . . Cl4 Cl 1.2912(3) 0.02695(12) -0.10981(16) 0.1308(14) Uani 1 1 d . . . Cl5 Cl 0.2316(3) 0.61319(10) -0.12599(8) 0.0931(9) Uani 1 1 d . . . Cl6 Cl 0.4587(4) 0.54439(14) -0.19125(13) 0.1561(19) Uani 1 1 d . . . Cl7 Cl 0.4662(5) 0.5305(2) -0.06429(14) 0.202(3) Uani 1 1 d . . . Cl8 Cl 0.2084(5) 0.4784(2) -0.1371(3) 0.286(4) Uani 1 1 d . . . Zn1 Zn 1.14792(10) -0.03510(4) -0.11986(4) 0.0633(3) Uani 1 1 d . . . Zn2 Zn 0.34192(13) 0.54312(5) -0.13073(5) 0.0857(4) Uani 1 1 d . . . O1W O 1.2147(4) 0.31678(18) -0.04361(17) 0.0436(12) Uani 1 1 d . . . O2W O 1.2539(4) 0.15624(17) 0.01203(16) 0.0436(12) Uani 1 1 d . . . O3W O 1.2798(4) 0.1884(2) -0.09648(15) 0.0475(13) Uani 1 1 d . . . O4W O 1.0656(5) 0.2522(2) -0.10360(17) 0.0566(14) Uani 1 1 d . . . O5W O 1.2446(5) 0.2556(2) 0.04762(16) 0.0525(14) Uani 1 1 d . . . O6W O 0.2848(4) 0.19404(18) -0.21462(16) 0.0425(11) Uani 1 1 d . . . O7W O 0.2438(4) 0.35335(19) -0.27283(15) 0.0454(12) Uani 1 1 d . . . O8W O 0.4346(5) 0.2593(2) -0.15536(17) 0.0542(14) Uani 1 1 d . . . O9W O 0.2553(5) 0.2538(2) -0.30670(16) 0.0540(14) Uani 1 1 d . . . O10W O 0.2212(4) 0.3230(2) -0.16225(15) 0.0473(13) Uani 1 1 d . . . Eu1 Eu 1.19483(3) 0.228883(12) -0.032742(11) 0.02812(11) Uani 1 1 d . . . Eu2 Eu 0.30395(3) 0.281591(12) -0.226204(11) 0.02899(11) Uani 1 1 d . . . C1 C 0.9015(5) 0.2548(2) 0.0120(2) 0.0278(13) Uani 1 1 d . . . C2 C 0.7097(6) 0.2790(2) 0.0412(2) 0.0293(14) Uani 1 1 d . . . H2 H 0.7072 0.2930 0.0726 0.035 Uiso 1 1 calc R . . C3 C 0.7221(5) 0.2222(2) 0.0421(2) 0.0261(13) Uani 1 1 d . . . H3 H 0.7209 0.2091 0.0738 0.031 Uiso 1 1 calc R . . C4 C 0.5320(5) 0.2439(2) -0.0023(2) 0.0281(13) Uani 1 1 d . . . C5 C 0.9104(6) 0.1659(2) 0.0279(2) 0.0310(14) Uani 1 1 d . . . H5A H 1.0040 0.1719 0.0326 0.037 Uiso 1 1 calc R . . H5B H 0.8852 0.1483 0.0550 0.037 Uiso 1 1 calc R . . C6 C 0.5778(6) 0.1540(2) 0.0047(2) 0.0335(15) Uani 1 1 d . . . H6A H 0.4847 0.1507 -0.0043 0.040 Uiso 1 1 calc R . . H6B H 0.5978 0.1359 0.0338 0.040 Uiso 1 1 calc R . . C7 C 0.9518(5) 0.1363(2) -0.0494(2) 0.0272(13) Uani 1 1 d . . . C8 C 0.7698(5) 0.1042(2) -0.0196(2) 0.0292(14) Uani 1 1 d . . . H8 H 0.7636 0.0806 0.0061 0.035 Uiso 1 1 calc R . . C9 C 0.7881(5) 0.0779(2) -0.0657(2) 0.0293(14) Uani 1 1 d . . . H9 H 0.8029 0.0421 -0.0615 0.035 Uiso 1 1 calc R . . C10 C 0.5904(6) 0.1188(2) -0.0730(2) 0.0362(16) Uani 1 1 d . . . C11 C 0.9687(6) 0.0866(2) -0.1196(2) 0.0319(14) Uani 1 1 d . . . H11A H 1.0597 0.0965 -0.1139 0.038 Uiso 1 1 calc R . . H11B H 0.9660 0.0505 -0.1208 0.038 Uiso 1 1 calc R . . C12 C 0.6344(6) 0.0663(2) -0.1388(2) 0.0344(15) Uani 1 1 d . . . H12A H 0.5396 0.0655 -0.1440 0.041 Uiso 1 1 calc R . . H12B H 0.6651 0.0321 -0.1382 0.041 Uiso 1 1 calc R . . C13 C 0.9830(6) 0.1393(2) -0.1873(2) 0.0305(14) Uani 1 1 d . . . C14 C 0.8099(6) 0.0838(2) -0.1922(2) 0.0311(14) Uani 1 1 d . . . H14 H 0.8256 0.0484 -0.1978 0.037 Uiso 1 1 calc R . . C15 C 0.8055(5) 0.1136(2) -0.2374(2) 0.0288(14) Uani 1 1 d . . . H15 H 0.8087 0.0918 -0.2646 0.035 Uiso 1 1 calc R . . C16 C 0.6100(6) 0.1236(2) -0.2049(2) 0.0336(15) Uani 1 1 d . . . C17 C 0.9683(6) 0.1744(2) -0.2658(2) 0.0288(13) Uani 1 1 d . . . H17A H 0.9535 0.1567 -0.2952 0.035 Uiso 1 1 calc R . . H17B H 1.0621 0.1785 -0.2588 0.035 Uiso 1 1 calc R . . C18 C 0.6284(6) 0.1668(2) -0.2782(2) 0.0314(14) Uani 1 1 d . . . H18A H 0.6500 0.1503 -0.3064 0.038 Uiso 1 1 calc R . . H18B H 0.5338 0.1668 -0.2784 0.038 Uiso 1 1 calc R . . C19 C 0.9683(5) 0.2655(2) -0.2565(2) 0.0266(13) Uani 1 1 d . . . C20 C 0.7891(5) 0.2315(2) -0.2998(2) 0.0264(13) Uani 1 1 d . . . H20 H 0.7907 0.2175 -0.3313 0.032 Uiso 1 1 calc R . . C21 C 0.7777(5) 0.2881(2) -0.3008(2) 0.0283(14) Uani 1 1 d . . . H21 H 0.7800 0.3013 -0.3325 0.034 Uiso 1 1 calc R . . C22 C 0.5976(5) 0.2553(2) -0.2707(2) 0.0280(13) Uani 1 1 d . . . C23 C 0.9214(6) 0.3556(2) -0.2624(2) 0.0331(15) Uani 1 1 d . . . H23A H 1.0141 0.3580 -0.2521 0.040 Uiso 1 1 calc R . . H23B H 0.9060 0.3736 -0.2916 0.040 Uiso 1 1 calc R . . C24 C 0.5881(5) 0.3445(2) -0.2872(2) 0.0278(13) Uani 1 1 d . . . H24A H 0.6124 0.3623 -0.3144 0.033 Uiso 1 1 calc R . . H24B H 0.4947 0.3382 -0.2917 0.033 Uiso 1 1 calc R . . C25 C 0.9066(6) 0.3913(2) -0.1858(2) 0.0367(16) Uani 1 1 d . . . C26 C 0.7312(6) 0.4063(2) -0.2392(2) 0.0332(14) Uani 1 1 d . . . H26 H 0.7373 0.4300 -0.2648 0.040 Uiso 1 1 calc R . . C27 C 0.7101(6) 0.4322(2) -0.1935(2) 0.0338(15) Uani 1 1 d . . . H27 H 0.6952 0.4680 -0.1981 0.041 Uiso 1 1 calc R . . C28 C 0.5465(6) 0.3747(2) -0.2101(2) 0.0311(14) Uani 1 1 d . . . C29 C 0.8651(6) 0.4438(2) -0.1196(2) 0.0372(15) Uani 1 1 d . . . H29A H 0.9598 0.4447 -0.1142 0.045 Uiso 1 1 calc R . . H29B H 0.8340 0.4779 -0.1194 0.045 Uiso 1 1 calc R . . C30 C 0.5311(6) 0.4237(2) -0.1392(2) 0.0364(15) Uani 1 1 d . . . H30A H 0.5359 0.4597 -0.1374 0.044 Uiso 1 1 calc R . . H30B H 0.4395 0.4147 -0.1449 0.044 Uiso 1 1 calc R . . C31 C 0.8903(6) 0.3866(2) -0.0540(2) 0.0343(15) Uani 1 1 d . . . C32 C 0.6872(5) 0.4266(2) -0.0670(2) 0.0297(14) Uani 1 1 d . . . H32 H 0.6708 0.4619 -0.0615 0.036 Uiso 1 1 calc R . . C33 C 0.6913(5) 0.3958(2) -0.0216(2) 0.0328(15) Uani 1 1 d . . . H33 H 0.6859 0.4172 0.0057 0.039 Uiso 1 1 calc R . . C34 C 0.5195(5) 0.3699(2) -0.0722(2) 0.0275(13) Uani 1 1 d . . . C35 C 0.8717(6) 0.3432(2) 0.0190(2) 0.0333(15) Uani 1 1 d . . . H35A H 0.9660 0.3425 0.0184 0.040 Uiso 1 1 calc R . . H35B H 0.8530 0.3601 0.0474 0.040 Uiso 1 1 calc R . . C36 C 0.5305(6) 0.3352(2) 0.0070(2) 0.0327(15) Uani 1 1 d . . . H36A H 0.5450 0.3531 0.0364 0.039 Uiso 1 1 calc R . . H36B H 0.4369 0.3310 -0.0001 0.039 Uiso 1 1 calc R . . N1 N 0.8248(4) 0.29399(19) 0.01994(17) 0.0267(11) Uani 1 1 d . . . N2 N 0.8442(4) 0.21268(18) 0.02427(18) 0.0268(11) Uani 1 1 d . . . N3 N 0.5907(4) 0.28673(18) 0.01250(17) 0.0278(11) Uani 1 1 d . . . N4 N 0.6092(4) 0.20580(19) 0.01220(17) 0.0281(11) Uani 1 1 d . . . N5 N 0.8830(4) 0.13543(18) -0.01216(17) 0.0274(11) Uani 1 1 d . . . N6 N 0.9012(4) 0.10291(19) -0.08094(17) 0.0299(12) Uani 1 1 d . . . N7 N 0.6486(4) 0.13201(19) -0.03069(18) 0.0307(12) Uani 1 1 d . . . N8 N 0.6706(4) 0.08810(18) -0.09422(18) 0.0299(12) Uani 1 1 d . . . N9 N 0.9174(5) 0.10557(18) -0.16376(17) 0.0299(12) Uani 1 1 d . . . N10 N 0.9210(5) 0.14521(18) -0.23041(17) 0.0295(12) Uani 1 1 d . . . N11 N 0.6841(5) 0.09138(19) -0.17720(18) 0.0328(12) Uani 1 1 d . . . N12 N 0.6838(4) 0.13894(18) -0.23837(18) 0.0301(12) Uani 1 1 d . . . N13 N 0.9096(5) 0.22287(17) -0.27143(17) 0.0268(11) Uani 1 1 d . . . N14 N 0.8886(4) 0.30350(18) -0.27083(17) 0.0285(11) Uani 1 1 d . . . N15 N 0.6729(5) 0.21646(18) -0.27846(18) 0.0286(12) Uani 1 1 d . . . N16 N 0.6570(4) 0.29768(18) -0.28335(17) 0.0260(11) Uani 1 1 d . . . N17 N 0.8502(5) 0.37882(19) -0.22871(18) 0.0322(12) Uani 1 1 d . . . N18 N 0.8289(5) 0.42254(19) -0.16557(19) 0.0355(13) Uani 1 1 d . . . N19 N 0.6165(4) 0.37470(18) -0.24685(17) 0.0283(11) Uani 1 1 d . . . N20 N 0.5972(4) 0.40764(19) -0.17842(17) 0.0292(11) Uani 1 1 d . . . N21 N 0.8163(5) 0.41815(19) -0.0825(2) 0.0363(13) Uani 1 1 d . . . N22 N 0.8158(5) 0.37116(19) -0.02015(18) 0.0316(12) Uani 1 1 d . . . N23 N 0.5813(5) 0.40365(18) -0.09553(17) 0.0310(12) Uani 1 1 d . . . N24 N 0.5803(5) 0.36486(18) -0.02949(17) 0.0301(12) Uani 1 1 d . . . O1 O 1.0086(4) 0.25809(17) -0.00252(15) 0.0337(10) Uani 1 1 d . . . O2 O 1.0480(4) 0.16230(16) -0.05394(14) 0.0360(10) Uani 1 1 d . . . O3 O 1.0836(4) 0.15993(17) -0.17205(14) 0.0381(11) Uani 1 1 d . . . O4 O 1.0743(4) 0.26896(16) -0.23418(15) 0.0345(10) Uani 1 1 d . . . O5 O 1.0140(5) 0.3784(2) -0.16878(19) 0.0608(16) Uani 1 1 d . . . O6 O 0.9999(4) 0.37571(18) -0.05869(17) 0.0452(12) Uani 1 1 d . . . O7 O 0.4256(4) 0.24105(17) -0.02430(15) 0.0360(11) Uani 1 1 d . . . O8 O 0.4836(4) 0.1316(2) -0.08941(18) 0.0557(14) Uani 1 1 d . . . O9 O 0.4985(4) 0.13397(18) -0.20096(17) 0.0430(12) Uani 1 1 d . . . O10 O 0.4915(4) 0.25290(17) -0.25649(15) 0.0350(10) Uani 1 1 d . . . O11 O 0.4513(4) 0.34930(16) -0.20584(15) 0.0366(11) Uani 1 1 d . . . O12 O 0.4166(4) 0.34925(18) -0.08727(15) 0.0410(11) 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 Cl9 0.0391(12) 0.150(2) 0.0415(12) 0.0085(13) -0.0026(9) -0.0112(13) Cl10 0.0410(13) 0.199(3) 0.0409(12) 0.0136(16) -0.0052(9) -0.0267(16) Cl1 0.0749(15) 0.0478(11) 0.0477(12) 0.0011(8) 0.0212(10) 0.0168(9) Cl2 0.153(3) 0.107(2) 0.108(2) -0.0319(19) -0.040(2) 0.070(2) Cl3 0.175(3) 0.132(3) 0.154(3) 0.080(2) 0.118(3) 0.097(3) Cl4 0.080(2) 0.079(2) 0.235(4) -0.023(2) 0.024(2) -0.0139(16) Cl5 0.139(3) 0.0793(18) 0.0681(17) 0.0084(13) 0.0460(16) 0.0404(16) Cl6 0.215(4) 0.125(3) 0.149(3) 0.063(2) 0.118(3) 0.095(3) Cl7 0.250(5) 0.237(5) 0.112(3) -0.037(3) -0.017(3) 0.180(5) Cl8 0.133(4) 0.149(4) 0.601(13) -0.134(6) 0.165(6) -0.069(3) Zn1 0.0711(7) 0.0495(6) 0.0708(7) -0.0006(5) 0.0148(5) 0.0091(5) Zn2 0.0974(9) 0.0681(8) 0.0943(9) 0.0008(6) 0.0231(7) 0.0151(7) O1W 0.022(2) 0.052(3) 0.056(3) 0.011(2) 0.004(2) -0.001(2) O2W 0.032(3) 0.054(3) 0.043(3) 0.010(2) -0.003(2) -0.006(2) O3W 0.031(3) 0.078(4) 0.033(3) -0.009(2) -0.002(2) 0.011(2) O4W 0.036(3) 0.083(4) 0.046(3) 0.017(3) -0.017(2) -0.010(3) O5W 0.038(3) 0.087(4) 0.030(3) -0.015(3) -0.005(2) 0.007(3) O6W 0.028(2) 0.050(3) 0.050(3) 0.009(2) 0.008(2) 0.000(2) O7W 0.032(3) 0.064(3) 0.039(3) 0.011(2) -0.002(2) -0.007(2) O8W 0.042(3) 0.072(4) 0.044(3) 0.015(3) -0.018(2) -0.004(3) O9W 0.033(3) 0.090(4) 0.037(3) -0.007(3) -0.002(2) 0.008(3) O10W 0.033(3) 0.080(4) 0.029(3) -0.010(2) 0.002(2) 0.007(2) Eu1 0.01240(18) 0.0448(2) 0.02696(19) 0.00068(13) 0.00083(12) -0.00218(12) Eu2 0.01269(18) 0.0471(2) 0.02704(19) 0.00122(13) 0.00119(12) -0.00231(12) C1 0.017(3) 0.043(4) 0.023(3) -0.004(3) -0.004(2) -0.001(3) C2 0.019(3) 0.039(4) 0.030(4) 0.001(3) 0.002(3) 0.000(2) C3 0.015(3) 0.043(4) 0.020(3) 0.003(3) 0.004(2) 0.001(2) C4 0.013(3) 0.044(4) 0.027(3) -0.004(3) 0.003(2) -0.003(3) C5 0.020(3) 0.046(4) 0.025(3) 0.006(3) -0.004(2) 0.010(3) C6 0.015(3) 0.043(4) 0.044(4) 0.000(3) 0.009(3) -0.003(3) C7 0.016(3) 0.037(3) 0.027(3) 0.005(3) -0.003(2) 0.005(2) C8 0.017(3) 0.030(3) 0.040(4) 0.005(3) 0.004(3) 0.002(2) C9 0.023(3) 0.029(3) 0.035(4) 0.005(3) 0.004(3) 0.003(2) C10 0.021(3) 0.036(4) 0.050(4) 0.008(3) -0.002(3) -0.006(3) C11 0.019(3) 0.036(4) 0.040(4) 0.006(3) 0.002(3) 0.007(2) C12 0.027(3) 0.034(4) 0.042(4) 0.006(3) 0.003(3) -0.006(3) C13 0.023(3) 0.035(3) 0.033(4) -0.009(3) 0.005(3) 0.001(3) C14 0.024(3) 0.031(3) 0.038(4) -0.007(3) -0.001(3) -0.001(2) C15 0.022(3) 0.031(3) 0.034(4) -0.010(3) 0.000(3) 0.002(2) C16 0.026(4) 0.031(3) 0.043(4) -0.003(3) -0.002(3) -0.002(3) C17 0.021(3) 0.035(3) 0.031(3) -0.003(3) 0.009(3) 0.006(2) C18 0.018(3) 0.035(3) 0.040(4) 0.001(3) -0.006(3) -0.004(2) C19 0.012(3) 0.037(3) 0.032(3) 0.002(3) 0.008(2) -0.004(2) C20 0.014(3) 0.041(4) 0.025(3) 0.001(3) 0.003(2) -0.003(2) C21 0.016(3) 0.043(4) 0.025(3) 0.005(3) 0.001(2) 0.000(2) C22 0.016(3) 0.044(4) 0.024(3) 0.005(3) -0.002(2) 0.001(3) C23 0.019(3) 0.035(4) 0.047(4) 0.003(3) 0.012(3) -0.006(3) C24 0.018(3) 0.037(3) 0.029(3) 0.009(3) 0.004(2) 0.002(2) C25 0.022(3) 0.032(4) 0.056(5) 0.000(3) 0.006(3) -0.001(3) C26 0.027(3) 0.032(3) 0.042(4) 0.006(3) 0.012(3) 0.000(3) C27 0.022(3) 0.033(4) 0.047(4) 0.005(3) 0.005(3) 0.002(3) C28 0.020(3) 0.043(4) 0.030(4) 0.007(3) -0.001(3) 0.004(3) C29 0.028(4) 0.037(4) 0.048(4) 0.001(3) 0.007(3) -0.006(3) C30 0.026(3) 0.038(4) 0.045(4) -0.005(3) 0.001(3) 0.008(3) C31 0.026(4) 0.033(4) 0.044(4) 0.002(3) 0.003(3) -0.005(3) C32 0.016(3) 0.031(3) 0.043(4) -0.007(3) 0.005(3) -0.002(2) C33 0.020(3) 0.038(4) 0.041(4) -0.014(3) 0.006(3) 0.004(3) C34 0.018(3) 0.031(3) 0.034(4) -0.008(3) 0.005(3) 0.002(2) C35 0.015(3) 0.052(4) 0.032(4) -0.008(3) 0.001(3) -0.004(3) C36 0.014(3) 0.045(4) 0.038(4) -0.007(3) -0.001(3) 0.008(3) N1 0.011(2) 0.037(3) 0.032(3) -0.002(2) 0.003(2) 0.000(2) N2 0.012(2) 0.035(3) 0.034(3) 0.001(2) 0.004(2) 0.000(2) N3 0.014(3) 0.039(3) 0.031(3) -0.004(2) 0.001(2) 0.000(2) N4 0.014(2) 0.037(3) 0.034(3) -0.005(2) 0.003(2) -0.002(2) N5 0.016(3) 0.037(3) 0.030(3) 0.002(2) 0.000(2) -0.002(2) N6 0.014(3) 0.040(3) 0.035(3) -0.002(2) 0.001(2) -0.004(2) N7 0.014(3) 0.038(3) 0.039(3) -0.002(2) 0.001(2) 0.000(2) N8 0.019(3) 0.031(3) 0.039(3) -0.010(2) -0.001(2) -0.003(2) N9 0.021(3) 0.036(3) 0.034(3) 0.000(2) 0.005(2) -0.002(2) N10 0.020(3) 0.035(3) 0.034(3) -0.001(2) 0.002(2) -0.001(2) N11 0.020(3) 0.037(3) 0.041(3) 0.006(2) 0.005(2) 0.000(2) N12 0.016(3) 0.034(3) 0.040(3) 0.007(2) 0.003(2) -0.002(2) N13 0.020(3) 0.034(3) 0.026(3) -0.003(2) -0.001(2) 0.003(2) N14 0.013(2) 0.036(3) 0.036(3) -0.003(2) 0.001(2) -0.006(2) N15 0.012(2) 0.039(3) 0.034(3) 0.004(2) 0.001(2) 0.000(2) N16 0.013(2) 0.034(3) 0.032(3) 0.000(2) 0.005(2) -0.001(2) N17 0.018(3) 0.035(3) 0.044(3) 0.000(2) 0.004(2) -0.001(2) N18 0.021(3) 0.035(3) 0.050(4) -0.007(3) 0.000(2) 0.000(2) N19 0.014(3) 0.036(3) 0.035(3) 0.002(2) 0.005(2) -0.003(2) N20 0.017(3) 0.040(3) 0.031(3) 0.004(2) 0.003(2) -0.002(2) N21 0.020(3) 0.034(3) 0.056(4) 0.005(3) 0.010(2) 0.003(2) N22 0.021(3) 0.038(3) 0.035(3) 0.000(2) 0.000(2) -0.002(2) N23 0.025(3) 0.034(3) 0.034(3) -0.001(2) 0.002(2) -0.001(2) N24 0.021(3) 0.034(3) 0.036(3) 0.003(2) 0.004(2) -0.002(2) O1 0.015(2) 0.046(3) 0.040(3) 0.002(2) 0.0067(18) 0.0017(18) O2 0.021(2) 0.052(3) 0.035(3) -0.003(2) 0.0007(18) -0.010(2) O3 0.024(2) 0.059(3) 0.032(2) 0.003(2) 0.0002(19) -0.011(2) O4 0.012(2) 0.046(3) 0.044(3) -0.001(2) -0.0028(19) -0.0009(17) O5 0.034(3) 0.070(4) 0.075(4) -0.025(3) -0.010(3) 0.017(3) O6 0.025(3) 0.051(3) 0.061(3) 0.011(2) 0.013(2) 0.009(2) O7 0.012(2) 0.046(3) 0.048(3) 0.000(2) -0.0058(19) -0.0020(18) O8 0.026(3) 0.070(4) 0.067(4) -0.017(3) -0.014(2) 0.011(2) O9 0.018(2) 0.054(3) 0.057(3) 0.006(2) 0.006(2) 0.004(2) O10 0.011(2) 0.052(3) 0.043(3) 0.004(2) 0.0052(18) -0.0056(18) O11 0.023(2) 0.047(3) 0.040(3) -0.001(2) 0.0062(19) -0.013(2) O12 0.025(2) 0.058(3) 0.040(3) -0.002(2) 0.003(2) -0.008(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 Cl1 Zn1 2.248(2) . ? Cl2 Zn1 2.255(3) . ? Cl3 Zn1 2.245(3) . ? Cl4 Zn1 2.245(3) . ? Cl5 Zn2 2.230(3) . ? Cl6 Zn2 2.230(3) . ? Cl7 Zn2 2.240(4) . ? Cl8 Zn2 2.232(4) . ? O1W Eu1 2.416(5) . ? O2W Eu1 2.407(5) . ? O3W Eu1 2.393(5) . ? O4W Eu1 2.428(5) . ? O5W Eu1 2.450(4) . ? O6W Eu2 2.409(5) . ? O7W Eu2 2.418(5) . ? O8W Eu2 2.427(4) . ? O9W Eu2 2.461(5) . ? O10W Eu2 2.400(4) . ? Eu1 O1 2.337(4) . ? Eu1 O7 2.405(4) 1_655 ? Eu1 O2 2.403(4) . ? Eu2 O10 2.345(4) . ? Eu2 O4 2.395(4) 1_455 ? Eu2 O11 2.425(4) . ? C1 O1 1.229(7) . ? C1 N2 1.353(8) . ? C1 N1 1.361(8) . ? C2 N3 1.437(7) . ? C2 N1 1.455(8) . ? C2 C3 1.544(8) . ? C2 H2 0.9900 . ? C3 N2 1.437(7) . ? C3 N4 1.457(7) . ? C3 H3 0.9900 . ? C4 O7 1.223(7) . ? C4 N4 1.350(8) . ? C4 N3 1.361(8) . ? C5 N5 1.433(8) . ? C5 N2 1.441(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.455(8) . ? C6 N7 1.449(8) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.240(7) . ? C7 N5 1.353(7) . ? C7 N6 1.357(8) . ? C8 N5 1.447(7) . ? C8 N7 1.475(7) . ? C8 C9 1.545(9) . ? C8 H8 0.9900 . ? C9 N8 1.432(7) . ? C9 N6 1.460(7) . ? C9 H9 0.9900 . ? C10 O8 1.214(7) . ? C10 N7 1.362(8) . ? C10 N8 1.367(8) . ? C11 N9 1.436(7) . ? C11 N6 1.448(8) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.439(8) . ? C12 N11 1.444(8) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.228(7) . ? C13 N10 1.361(8) . ? C13 N9 1.363(8) . ? C14 N11 1.429(8) . ? C14 N9 1.447(7) . ? C14 C15 1.540(9) . ? C14 H14 0.9900 . ? C15 N12 1.436(7) . ? C15 N10 1.471(7) . ? C15 H15 0.9900 . ? C16 O9 1.207(7) . ? C16 N12 1.360(8) . ? C16 N11 1.371(8) . ? C17 N10 1.423(8) . ? C17 N13 1.450(7) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N15 1.424(8) . ? C18 N12 1.452(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.224(7) . ? C19 N13 1.359(7) . ? C19 N14 1.361(7) . ? C20 N13 1.449(7) . ? C20 N15 1.466(7) . ? C20 C21 1.541(8) . ? C20 H20 0.9900 . ? C21 N16 1.420(7) . ? C21 N14 1.435(7) . ? C21 H21 0.9900 . ? C22 O10 1.215(7) . ? C22 N15 1.342(8) . ? C22 N16 1.372(8) . ? C23 N17 1.429(8) . ? C23 N14 1.468(8) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N19 1.436(8) . ? C24 N16 1.456(7) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O5 1.225(8) . ? C25 N18 1.343(8) . ? C25 N17 1.367(8) . ? C26 N17 1.448(8) . ? C26 N19 1.465(7) . ? C26 C27 1.534(9) . ? C26 H26 0.9900 . ? C27 N18 1.432(7) . ? C27 N20 1.452(7) . ? C27 H27 0.9900 . ? C28 O11 1.220(7) . ? C28 N20 1.353(8) . ? C28 N19 1.347(7) . ? C29 N21 1.415(8) . ? C29 N18 1.470(8) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N23 1.432(8) . ? C30 N20 1.452(8) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O6 1.195(7) . ? C31 N21 1.372(8) . ? C31 N22 1.375(8) . ? C32 N23 1.450(7) . ? C32 N21 1.472(7) . ? C32 C33 1.556(9) . ? C32 H32 0.9900 . ? C33 N24 1.424(7) . ? C33 N22 1.451(7) . ? C33 H33 0.9900 . ? C34 O12 1.246(7) . ? C34 N23 1.338(8) . ? C34 N24 1.343(8) . ? C35 N1 1.423(8) . ? C35 N22 1.439(8) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N3 1.457(8) . ? C36 N24 1.465(8) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? O4 Eu2 2.395(4) 1_655 ? O7 Eu1 2.405(4) 1_455 ? 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 Cl3 Zn1 Cl4 109.98(17) . . ? Cl3 Zn1 Cl1 108.54(10) . . ? Cl4 Zn1 Cl1 109.46(11) . . ? Cl3 Zn1 Cl2 112.02(16) . . ? Cl4 Zn1 Cl2 106.28(16) . . ? Cl1 Zn1 Cl2 110.51(10) . . ? Cl5 Zn2 Cl6 110.91(11) . . ? Cl5 Zn2 Cl8 110.93(18) . . ? Cl6 Zn2 Cl8 109.1(2) . . ? Cl5 Zn2 Cl7 109.44(13) . . ? Cl6 Zn2 Cl7 111.71(19) . . ? Cl8 Zn2 Cl7 104.6(3) . . ? O1 Eu1 O3W 145.74(15) . . ? O1 Eu1 O7 140.01(15) . 1_655 ? O3W Eu1 O7 72.76(15) . 1_655 ? O1 Eu1 O2W 104.54(16) . . ? O3W Eu1 O2W 87.07(17) . . ? O7 Eu1 O2W 81.88(15) 1_655 . ? O1 Eu1 O2 79.90(15) . . ? O3W Eu1 O2 74.30(16) . . ? O7 Eu1 O2 136.77(15) 1_655 . ? O2W Eu1 O2 69.20(15) . . ? O1 Eu1 O1W 78.39(15) . . ? O3W Eu1 O1W 107.98(17) . . ? O7 Eu1 O1W 77.35(15) 1_655 . ? O2W Eu1 O1W 149.06(15) . . ? O2 Eu1 O1W 140.17(14) . . ? O1 Eu1 O4W 79.72(17) . . ? O3W Eu1 O4W 71.24(18) . . ? O7 Eu1 O4W 120.84(16) 1_655 . ? O2W Eu1 O4W 139.60(18) . . ? O2 Eu1 O4W 72.23(16) . . ? O1W Eu1 O4W 71.31(17) . . ? O1 Eu1 O5W 69.34(15) . . ? O3W Eu1 O5W 144.40(15) . . ? O7 Eu1 O5W 75.35(16) 1_655 . ? O2W Eu1 O5W 73.05(18) . . ? O2 Eu1 O5W 122.38(17) . . ? O1W Eu1 O5W 79.63(18) . . ? O4W Eu1 O5W 141.09(19) . . ? O10 Eu2 O4 140.35(15) . 1_455 ? O10 Eu2 O10W 144.88(15) . . ? O4 Eu2 O10W 73.41(15) 1_455 . ? O10 Eu2 O6W 78.94(15) . . ? O4 Eu2 O6W 77.16(14) 1_455 . ? O10W Eu2 O6W 108.21(17) . . ? O10 Eu2 O7W 103.62(16) . . ? O4 Eu2 O7W 82.00(15) 1_455 . ? O10W Eu2 O7W 87.97(17) . . ? O6W Eu2 O7W 148.34(15) . . ? O10 Eu2 O11 79.43(15) . . ? O4 Eu2 O11 136.80(15) 1_455 . ? O10W Eu2 O11 73.81(16) . . ? O6W Eu2 O11 140.44(15) . . ? O7W Eu2 O11 69.46(15) . . ? O10 Eu2 O8W 79.65(17) . . ? O4 Eu2 O8W 120.94(16) 1_455 . ? O10W Eu2 O8W 70.88(17) . . ? O6W Eu2 O8W 71.53(17) . . ? O7W Eu2 O8W 140.12(17) . . ? O11 Eu2 O8W 72.26(16) . . ? O10 Eu2 O9W 69.09(15) . . ? O4 Eu2 O9W 75.78(15) 1_455 . ? O10W Eu2 O9W 145.36(15) . . ? O6W Eu2 O9W 79.57(18) . . ? O7W Eu2 O9W 72.33(18) . . ? O11 Eu2 O9W 121.96(17) . . ? O8W Eu2 O9W 140.81(19) . . ? O1 C1 N2 125.9(6) . . ? O1 C1 N1 124.4(6) . . ? N2 C1 N1 109.6(5) . . ? N3 C2 N1 114.0(5) . . ? N3 C2 C3 102.8(5) . . ? N1 C2 C3 102.4(5) . . ? N3 C2 H2 112.3 . . ? N1 C2 H2 112.3 . . ? C3 C2 H2 112.3 . . ? N2 C3 N4 114.6(5) . . ? N2 C3 C2 104.4(5) . . ? N4 C3 C2 103.6(5) . . ? N2 C3 H3 111.3 . . ? N4 C3 H3 111.3 . . ? C2 C3 H3 111.3 . . ? O7 C4 N4 126.3(6) . . ? O7 C4 N3 124.9(6) . . ? N4 C4 N3 108.7(5) . . ? N5 C5 N2 113.2(5) . . ? N5 C5 H5A 108.9 . . ? N2 C5 H5A 108.9 . . ? N5 C5 H5B 108.9 . . ? N2 C5 H5B 108.9 . . ? H5A C5 H5B 107.8 . . ? N4 C6 N7 112.4(5) . . ? N4 C6 H6A 109.1 . . ? N7 C6 H6A 109.1 . . ? N4 C6 H6B 109.1 . . ? N7 C6 H6B 109.1 . . ? H6A C6 H6B 107.9 . . ? O2 C7 N5 126.0(5) . . ? O2 C7 N6 124.8(6) . . ? N5 C7 N6 109.2(5) . . ? N5 C8 N7 113.2(5) . . ? N5 C8 C9 103.5(5) . . ? N7 C8 C9 102.8(5) . . ? N5 C8 H8 112.2 . . ? N7 C8 H8 112.2 . . ? C9 C8 H8 112.2 . . ? N8 C9 N6 113.6(5) . . ? N8 C9 C8 104.0(5) . . ? N6 C9 C8 102.6(5) . . ? N8 C9 H9 112.0 . . ? N6 C9 H9 112.0 . . ? C8 C9 H9 112.0 . . ? O8 C10 N7 126.0(7) . . ? O8 C10 N8 124.7(6) . . ? N7 C10 N8 109.3(5) . . ? N9 C11 N6 114.7(5) . . ? N9 C11 H11A 108.6 . . ? N6 C11 H11A 108.6 . . ? N9 C11 H11B 108.6 . . ? N6 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? N8 C12 N11 114.8(5) . . ? N8 C12 H12A 108.6 . . ? N11 C12 H12A 108.6 . . ? N8 C12 H12B 108.6 . . ? N11 C12 H12B 108.6 . . ? H12A C12 H12B 107.5 . . ? O3 C13 N10 125.9(6) . . ? O3 C13 N9 125.1(6) . . ? N10 C13 N9 109.0(5) . . ? N11 C14 N9 116.4(5) . . ? N11 C14 C15 103.4(5) . . ? N9 C14 C15 103.3(5) . . ? N11 C14 H14 111.1 . . ? N9 C14 H14 111.1 . . ? C15 C14 H14 111.1 . . ? N12 C15 N10 115.2(5) . . ? N12 C15 C14 102.7(5) . . ? N10 C15 C14 103.4(4) . . ? N12 C15 H15 111.6 . . ? N10 C15 H15 111.6 . . ? C14 C15 H15 111.6 . . ? O9 C16 N12 127.5(6) . . ? O9 C16 N11 125.5(6) . . ? N12 C16 N11 107.0(5) . . ? N10 C17 N13 114.6(5) . . ? N10 C17 H17A 108.6 . . ? N13 C17 H17A 108.6 . . ? N10 C17 H17B 108.6 . . ? N13 C17 H17B 108.6 . . ? H17A C17 H17B 107.6 . . ? N15 C18 N12 113.2(5) . . ? N15 C18 H18A 108.9 . . ? N12 C18 H18A 108.9 . . ? N15 C18 H18B 108.9 . . ? N12 C18 H18B 108.9 . . ? H18A C18 H18B 107.8 . . ? O4 C19 N13 125.8(6) . . ? O4 C19 N14 126.4(5) . . ? N13 C19 N14 107.8(5) . . ? N13 C20 N15 114.4(5) . . ? N13 C20 C21 103.4(4) . . ? N15 C20 C21 102.7(5) . . ? N13 C20 H20 111.9 . . ? N15 C20 H20 111.9 . . ? C21 C20 H20 111.9 . . ? N16 C21 N14 114.4(5) . . ? N16 C21 C20 104.1(5) . . ? N14 C21 C20 102.9(5) . . ? N16 C21 H21 111.6 . . ? N14 C21 H21 111.6 . . ? C20 C21 H21 111.6 . . ? O10 C22 N15 125.2(6) . . ? O10 C22 N16 125.5(6) . . ? N15 C22 N16 109.2(5) . . ? N17 C23 N14 114.3(5) . . ? N17 C23 H23A 108.7 . . ? N14 C23 H23A 108.7 . . ? N17 C23 H23B 108.7 . . ? N14 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? N19 C24 N16 112.0(5) . . ? N19 C24 H24A 109.2 . . ? N16 C24 H24A 109.2 . . ? N19 C24 H24B 109.2 . . ? N16 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? O5 C25 N18 124.4(7) . . ? O5 C25 N17 126.0(6) . . ? N18 C25 N17 109.4(5) . . ? N17 C26 N19 113.2(5) . . ? N17 C26 C27 104.2(5) . . ? N19 C26 C27 102.6(5) . . ? N17 C26 H26 112.1 . . ? N19 C26 H26 112.1 . . ? C27 C26 H26 112.1 . . ? N18 C27 N20 114.8(5) . . ? N18 C27 C26 102.7(5) . . ? N20 C27 C26 103.8(5) . . ? N18 C27 H27 111.7 . . ? N20 C27 H27 111.7 . . ? C26 C27 H27 111.7 . . ? O11 C28 N20 124.6(6) . . ? O11 C28 N19 125.8(6) . . ? N20 C28 N19 109.5(5) . . ? N21 C29 N18 114.8(5) . . ? N21 C29 H29A 108.6 . . ? N18 C29 H29A 108.6 . . ? N21 C29 H29B 108.6 . . ? N18 C29 H29B 108.6 . . ? H29A C29 H29B 107.5 . . ? N23 C30 N20 115.0(5) . . ? N23 C30 H30A 108.5 . . ? N20 C30 H30A 108.5 . . ? N23 C30 H30B 108.5 . . ? N20 C30 H30B 108.5 . . ? H30A C30 H30B 107.5 . . ? O6 C31 N21 124.7(6) . . ? O6 C31 N22 127.8(6) . . ? N21 C31 N22 107.5(5) . . ? N23 C32 N21 114.8(5) . . ? N23 C32 C33 102.2(5) . . ? N21 C32 C33 103.1(5) . . ? N23 C32 H32 112.0 . . ? N21 C32 H32 112.0 . . ? C33 C32 H32 112.0 . . ? N24 C33 N22 115.9(5) . . ? N24 C33 C32 103.0(5) . . ? N22 C33 C32 102.9(5) . . ? N24 C33 H33 111.5 . . ? N22 C33 H33 111.5 . . ? C32 C33 H33 111.5 . . ? O12 C34 N23 124.5(6) . . ? O12 C34 N24 126.0(6) . . ? N23 C34 N24 109.4(5) . . ? N1 C35 N22 113.4(5) . . ? N1 C35 H35A 108.9 . . ? N22 C35 H35A 108.9 . . ? N1 C35 H35B 108.9 . . ? N22 C35 H35B 108.9 . . ? H35A C35 H35B 107.7 . . ? N3 C36 N24 113.4(5) . . ? N3 C36 H36A 108.9 . . ? N24 C36 H36A 108.9 . . ? N3 C36 H36B 108.9 . . ? N24 C36 H36B 108.9 . . ? H36A C36 H36B 107.7 . . ? C1 N1 C35 121.5(5) . . ? C1 N1 C2 111.8(5) . . ? C35 N1 C2 124.6(5) . . ? C1 N2 C3 111.6(5) . . ? C1 N2 C5 122.9(5) . . ? C3 N2 C5 124.3(5) . . ? C4 N3 C2 113.0(5) . . ? C4 N3 C36 124.2(5) . . ? C2 N3 C36 122.0(5) . . ? C4 N4 C3 111.7(5) . . ? C4 N4 C6 125.2(5) . . ? C3 N4 C6 122.7(5) . . ? C7 N5 C5 124.0(5) . . ? C7 N5 C8 112.0(5) . . ? C5 N5 C8 123.6(5) . . ? C7 N6 C11 122.8(5) . . ? C7 N6 C9 112.0(5) . . ? C11 N6 C9 123.8(5) . . ? C10 N7 C6 122.4(5) . . ? C10 N7 C8 110.9(5) . . ? C6 N7 C8 122.4(5) . . ? C10 N8 C9 112.2(5) . . ? C10 N8 C12 122.7(5) . . ? C9 N8 C12 125.0(5) . . ? C13 N9 C11 121.9(5) . . ? C13 N9 C14 112.6(5) . . ? C11 N9 C14 124.2(5) . . ? C13 N10 C17 124.4(5) . . ? C13 N10 C15 111.3(5) . . ? C17 N10 C15 124.0(5) . . ? C16 N11 C14 112.9(5) . . ? C16 N11 C12 122.1(5) . . ? C14 N11 C12 124.9(5) . . ? C16 N12 C15 113.3(5) . . ? C16 N12 C18 121.4(5) . . ? C15 N12 C18 123.0(5) . . ? C19 N13 C17 124.4(5) . . ? C19 N13 C20 112.3(5) . . ? C17 N13 C20 122.7(5) . . ? C19 N14 C21 113.2(5) . . ? C19 N14 C23 123.5(5) . . ? C21 N14 C23 122.7(5) . . ? C22 N15 C18 123.1(5) . . ? C22 N15 C20 111.6(5) . . ? C18 N15 C20 123.1(5) . . ? C22 N16 C21 112.1(5) . . ? C22 N16 C24 121.5(5) . . ? C21 N16 C24 125.1(5) . . ? C25 N17 C23 121.9(5) . . ? C25 N17 C26 110.1(5) . . ? C23 N17 C26 124.8(5) . . ? C25 N18 C27 112.8(5) . . ? C25 N18 C29 122.2(5) . . ? C27 N18 C29 125.0(5) . . ? C28 N19 C24 124.2(5) . . ? C28 N19 C26 111.8(5) . . ? C24 N19 C26 123.8(5) . . ? C28 N20 C30 123.4(5) . . ? C28 N20 C27 111.6(5) . . ? C30 N20 C27 123.8(5) . . ? C31 N21 C29 122.9(5) . . ? C31 N21 C32 112.6(5) . . ? C29 N21 C32 124.1(5) . . ? C31 N22 C35 120.9(5) . . ? C31 N22 C33 113.5(5) . . ? C35 N22 C33 123.7(5) . . ? C34 N23 C30 123.9(5) . . ? C34 N23 C32 112.2(5) . . ? C30 N23 C32 122.3(5) . . ? C34 N24 C33 112.8(5) . . ? C34 N24 C36 123.9(5) . . ? C33 N24 C36 122.9(5) . . ? C1 O1 Eu1 155.8(4) . . ? C7 O2 Eu1 153.7(4) . . ? C19 O4 Eu2 153.6(4) . 1_655 ? C4 O7 Eu1 154.3(4) . 1_455 ? C22 O10 Eu2 157.3(4) . . ? C28 O11 Eu2 154.1(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.380 _refine_diff_density_min -2.037 _refine_diff_density_rms 0.144 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.507 0.000 0.007 977 347 ' ' 2 0.752 0.245 0.371 87 34 ' ' 3 0.752 0.255 0.871 87 35 ' ' 4 0.156 0.500 0.156 977 347 ' ' 5 0.248 0.745 0.129 87 34 ' ' 6 0.248 0.755 0.629 87 35 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 902617' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p308 #TrackingRef 'submit-308.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H94 Cl10 Gd2 N24 O41 Zn2' _chemical_formula_weight 2319.09 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 '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 10.380(2) _cell_length_b 26.980(5) _cell_length_c 29.004(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.530(6) _cell_angle_gamma 90.00 _cell_volume 8085(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.905 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4656 _exptl_absorpt_coefficient_mu 2.641 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5818 _exptl_absorpt_correction_T_max 0.6624 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 72852 _diffrn_reflns_av_R_equivalents 0.0810 _diffrn_reflns_av_sigmaI/netI 0.0777 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 26.00 _reflns_number_total 15670 _reflns_number_gt 10699 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1254P)^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 15670 _refine_ls_number_parameters 866 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0900 _refine_ls_R_factor_gt 0.0648 _refine_ls_wR_factor_ref 0.2065 _refine_ls_wR_factor_gt 0.1920 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Cl9 Cl -0.0165(2) 0.24681(14) 0.12139(8) 0.0781(8) Uani 1 1 d . . . Cl10 Cl 0.5167(2) 0.25440(16) 0.62115(8) 0.0929(11) Uani 1 1 d . . . O1W O 0.7137(5) 0.3146(2) 0.45725(19) 0.0475(14) Uani 1 1 d . . . O2W O 0.7774(5) 0.1880(2) 0.40408(17) 0.0484(14) Uani 1 1 d . . . O3W O 0.7527(5) 0.1547(2) 0.5126(2) 0.0504(14) Uani 1 1 d . . . O4W O 0.5655(5) 0.2515(3) 0.3976(2) 0.0603(17) Uani 1 1 d . . . O5W O 0.7410(5) 0.2544(2) 0.54829(17) 0.0500(15) Uani 1 1 d . . . O6W O -0.2158(5) 0.1935(2) 0.2857(2) 0.0495(14) Uani 1 1 d . . . O7W O -0.2563(5) 0.3531(2) 0.22775(18) 0.0508(15) Uani 1 1 d . . . O8W O -0.2794(5) 0.3218(2) 0.33794(17) 0.0503(15) Uani 1 1 d . . . O9W O -0.2442(5) 0.2533(3) 0.19404(18) 0.0545(15) Uani 1 1 d . . . O10W O -0.0657(6) 0.2589(3) 0.3447(2) 0.0581(16) Uani 1 1 d . . . Gd1 Gd 0.69316(3) 0.227833(15) 0.468204(12) 0.03318(14) Uani 1 1 d . . . Gd2 Gd -0.19595(3) 0.281409(15) 0.274011(12) 0.03414(14) Uani 1 1 d . . . Cl1 Cl 0.7567(2) -0.10593(10) 0.38169(8) 0.0668(7) Uani 1 1 d . . . Cl2 Cl 0.5376(5) -0.02302(18) 0.30805(16) 0.157(2) Uani 1 1 d . . . Cl3 Cl 0.5115(5) -0.03564(19) 0.43533(19) 0.193(3) Uani 1 1 d . . . Cl4 Cl 0.7908(4) 0.02788(17) 0.3894(2) 0.158(2) Uani 1 1 d . . . Cl5 Cl -0.2711(4) 0.61220(13) 0.37352(10) 0.1032(12) Uani 1 1 d . . . Cl6 Cl -0.0449(5) 0.54266(17) 0.30799(15) 0.162(2) Uani 1 1 d . . . Cl7 Cl -0.0250(6) 0.5337(2) 0.43456(17) 0.204(3) Uani 1 1 d . . . Cl8 Cl -0.2908(6) 0.4772(2) 0.3661(3) 0.271(5) Uani 1 1 d . . . Zn1 Zn 0.64800(15) -0.03472(5) 0.37889(5) 0.0876(4) Uani 1 1 d . . . Zn2 Zn -0.15910(16) 0.54241(6) 0.36980(6) 0.0943(5) Uani 1 1 d . . . C1 C 0.3999(6) 0.2537(3) 0.5127(2) 0.0318(16) Uani 1 1 d . . . C2 C 0.2083(7) 0.2774(3) 0.5418(3) 0.0335(17) Uani 1 1 d . . . H2 H 0.2064 0.2916 0.5732 0.040 Uiso 1 1 calc R . . C3 C 0.2206(7) 0.2210(3) 0.5432(2) 0.0316(17) Uani 1 1 d . . . H3 H 0.2189 0.2082 0.5752 0.038 Uiso 1 1 calc R . . C4 C 0.0284(7) 0.2436(3) 0.4986(2) 0.0306(16) Uani 1 1 d . . . C5 C 0.4095(7) 0.1641(3) 0.5285(2) 0.0342(17) Uani 1 1 d . . . H5A H 0.5028 0.1704 0.5329 0.041 Uiso 1 1 calc R . . H5B H 0.3858 0.1462 0.5558 0.041 Uiso 1 1 calc R . . C6 C 0.0755(7) 0.1525(3) 0.5052(3) 0.0367(18) Uani 1 1 d . . . H6A H 0.0929 0.1343 0.5344 0.044 Uiso 1 1 calc R . . H6B H -0.0173 0.1496 0.4954 0.044 Uiso 1 1 calc R . . C7 C 0.4521(6) 0.1344(3) 0.4514(2) 0.0320(16) Uani 1 1 d . . . C8 C 0.2679(6) 0.1013(3) 0.4809(2) 0.0324(16) Uani 1 1 d . . . H8 H 0.2618 0.0772 0.5064 0.039 Uiso 1 1 calc R . . C9 C 0.2867(6) 0.0760(3) 0.4349(3) 0.0361(17) Uani 1 1 d . . . H9 H 0.3013 0.0399 0.4387 0.043 Uiso 1 1 calc R . . C10 C 0.0889(7) 0.1177(3) 0.4274(3) 0.0382(18) Uani 1 1 d . . . C11 C 0.4690(7) 0.0848(3) 0.3803(2) 0.0358(17) Uani 1 1 d . . . H11A H 0.5602 0.0943 0.3861 0.043 Uiso 1 1 calc R . . H11B H 0.4653 0.0485 0.3784 0.043 Uiso 1 1 calc R . . C12 C 0.1313(7) 0.0651(3) 0.3611(3) 0.0422(19) Uani 1 1 d . . . H12A H 0.1597 0.0305 0.3611 0.051 Uiso 1 1 calc R . . H12B H 0.0366 0.0653 0.3560 0.051 Uiso 1 1 calc R . . C13 C 0.4832(6) 0.1381(3) 0.3136(2) 0.0313(16) Uani 1 1 d . . . C14 C 0.3079(7) 0.0826(3) 0.3077(2) 0.0352(17) Uani 1 1 d . . . H14 H 0.3236 0.0470 0.3022 0.042 Uiso 1 1 calc R . . C15 C 0.3038(7) 0.1120(3) 0.2627(3) 0.0352(17) Uani 1 1 d . . . H15 H 0.3071 0.0900 0.2356 0.042 Uiso 1 1 calc R . . C16 C 0.1087(7) 0.1220(3) 0.2949(3) 0.0377(18) Uani 1 1 d . . . C17 C 0.4672(7) 0.1738(3) 0.2334(2) 0.0349(17) Uani 1 1 d . . . H17A H 0.5614 0.1773 0.2392 0.042 Uiso 1 1 calc R . . H17B H 0.4489 0.1562 0.2040 0.042 Uiso 1 1 calc R . . C18 C 0.1287(7) 0.1656(3) 0.2225(3) 0.0378(18) Uani 1 1 d . . . H18A H 0.0343 0.1657 0.2224 0.045 Uiso 1 1 calc R . . H18B H 0.1499 0.1490 0.1942 0.045 Uiso 1 1 calc R . . C19 C 0.4684(7) 0.2646(3) 0.2440(2) 0.0326(17) Uani 1 1 d . . . C20 C 0.2892(7) 0.2315(3) 0.2000(3) 0.0337(17) Uani 1 1 d . . . H20 H 0.2911 0.2175 0.1686 0.040 Uiso 1 1 calc R . . C21 C 0.2772(7) 0.2884(3) 0.1991(2) 0.0320(16) Uani 1 1 d . . . H21 H 0.2789 0.3017 0.1674 0.038 Uiso 1 1 calc R . . C22 C 0.0972(6) 0.2557(3) 0.2293(2) 0.0301(15) Uani 1 1 d . . . C23 C 0.4208(7) 0.3561(3) 0.2380(3) 0.0396(18) Uani 1 1 d . . . H23A H 0.5133 0.3591 0.2481 0.048 Uiso 1 1 calc R . . H23B H 0.4043 0.3743 0.2088 0.048 Uiso 1 1 calc R . . C24 C 0.0887(7) 0.3449(3) 0.2134(2) 0.0344(17) Uani 1 1 d . . . H24A H 0.1133 0.3628 0.1861 0.041 Uiso 1 1 calc R . . H24B H -0.0046 0.3386 0.2087 0.041 Uiso 1 1 calc R . . C25 C 0.4049(7) 0.3914(3) 0.3148(3) 0.0419(19) Uani 1 1 d . . . C26 C 0.2329(7) 0.4077(3) 0.2617(2) 0.0346(17) Uani 1 1 d . . . H26 H 0.2402 0.4320 0.2365 0.042 Uiso 1 1 calc R . . C27 C 0.2112(7) 0.4323(3) 0.3073(3) 0.0361(17) Uani 1 1 d . . . H27 H 0.1958 0.4683 0.3031 0.043 Uiso 1 1 calc R . . C28 C 0.0447(6) 0.3751(3) 0.2904(2) 0.0326(16) Uani 1 1 d . . . C29 C 0.3660(7) 0.4449(3) 0.3811(3) 0.044(2) Uani 1 1 d . . . H29A H 0.4606 0.4457 0.3864 0.053 Uiso 1 1 calc R . . H29B H 0.3349 0.4792 0.3812 0.053 Uiso 1 1 calc R . . C30 C 0.0299(7) 0.4241(3) 0.3618(3) 0.0387(18) Uani 1 1 d . . . H30A H 0.0338 0.4604 0.3636 0.046 Uiso 1 1 calc R . . H30B H -0.0614 0.4146 0.3564 0.046 Uiso 1 1 calc R . . C31 C 0.3887(7) 0.3870(3) 0.4472(3) 0.0397(18) Uani 1 1 d . . . C32 C 0.1883(7) 0.4270(3) 0.4341(2) 0.0360(17) Uani 1 1 d . . . H32 H 0.1721 0.4625 0.4396 0.043 Uiso 1 1 calc R . . C33 C 0.1908(6) 0.3952(3) 0.4800(3) 0.0327(16) Uani 1 1 d . . . H33 H 0.1856 0.4165 0.5076 0.039 Uiso 1 1 calc R . . C34 C 0.0172(7) 0.3698(3) 0.4286(2) 0.0310(16) Uani 1 1 d . . . C35 C 0.3698(7) 0.3423(3) 0.5200(3) 0.0402(19) Uani 1 1 d . . . H35A H 0.4641 0.3415 0.5198 0.048 Uiso 1 1 calc R . . H35B H 0.3504 0.3590 0.5486 0.048 Uiso 1 1 calc R . . C36 C 0.0290(6) 0.3345(3) 0.5086(2) 0.0345(17) Uani 1 1 d . . . H36A H 0.0433 0.3524 0.5381 0.041 Uiso 1 1 calc R . . H36B H -0.0646 0.3303 0.5015 0.041 Uiso 1 1 calc R . . N1 N 0.3230(5) 0.2930(2) 0.5206(2) 0.0316(13) Uani 1 1 d . . . N2 N 0.3427(6) 0.2105(2) 0.5255(2) 0.0347(14) Uani 1 1 d . . . N3 N 0.0892(6) 0.2859(2) 0.5139(2) 0.0334(14) Uani 1 1 d . . . N4 N 0.1071(5) 0.2043(2) 0.51318(19) 0.0292(13) Uani 1 1 d . . . N5 N 0.3821(5) 0.1334(2) 0.48869(19) 0.0315(14) Uani 1 1 d . . . N6 N 0.3998(5) 0.1011(2) 0.4198(2) 0.0317(13) Uani 1 1 d . . . N7 N 0.1473(5) 0.1294(2) 0.4703(2) 0.0359(14) Uani 1 1 d . . . N8 N 0.1699(6) 0.0864(2) 0.4065(2) 0.0381(15) Uani 1 1 d . . . N9 N 0.4178(6) 0.1050(2) 0.3367(2) 0.0341(14) Uani 1 1 d . . . N10 N 0.4213(5) 0.1438(2) 0.2702(2) 0.0329(14) Uani 1 1 d . . . N11 N 0.1821(6) 0.0903(2) 0.3228(2) 0.0393(15) Uani 1 1 d . . . N12 N 0.1832(5) 0.1379(2) 0.2615(2) 0.0361(14) Uani 1 1 d . . . N13 N 0.4101(5) 0.2227(2) 0.2290(2) 0.0299(14) Uani 1 1 d . . . N14 N 0.3907(5) 0.3042(2) 0.2294(2) 0.0313(13) Uani 1 1 d . . . N15 N 0.1731(6) 0.2158(2) 0.2218(2) 0.0333(14) Uani 1 1 d . . . N16 N 0.1568(5) 0.2978(2) 0.2169(2) 0.0302(13) Uani 1 1 d . . . N17 N 0.3493(5) 0.3791(2) 0.2720(2) 0.0334(14) Uani 1 1 d . . . N18 N 0.3291(6) 0.4233(2) 0.3350(2) 0.0406(16) Uani 1 1 d . . . N19 N 0.1152(5) 0.3755(2) 0.2534(2) 0.0310(13) Uani 1 1 d . . . N20 N 0.0974(6) 0.4077(2) 0.3224(2) 0.0341(14) Uani 1 1 d . . . N21 N 0.3155(6) 0.4182(2) 0.4195(2) 0.0424(16) Uani 1 1 d . . . N22 N 0.3151(6) 0.3711(2) 0.4807(2) 0.0382(15) Uani 1 1 d . . . N23 N 0.0831(5) 0.4038(2) 0.4052(2) 0.0340(14) Uani 1 1 d . . . N24 N 0.0797(6) 0.3648(2) 0.4716(2) 0.0341(14) Uani 1 1 d . . . O1 O 0.5070(4) 0.2567(2) 0.49823(17) 0.0372(12) Uani 1 1 d . . . O2 O 0.5471(4) 0.1609(2) 0.44733(17) 0.0404(13) Uani 1 1 d . . . O3 O 0.5818(5) 0.1593(2) 0.32812(17) 0.0424(13) Uani 1 1 d . . . O4 O 0.5752(4) 0.26818(19) 0.26580(18) 0.0376(12) Uani 1 1 d . . . O5 O 0.5136(6) 0.3789(3) 0.3325(2) 0.069(2) Uani 1 1 d . . . O6 O 0.4993(5) 0.3755(2) 0.4416(2) 0.0521(15) Uani 1 1 d . . . O7 O -0.0775(4) 0.2404(2) 0.47675(17) 0.0365(12) Uani 1 1 d . . . O8 O -0.0190(5) 0.1303(3) 0.4108(2) 0.0597(17) Uani 1 1 d . . . O9 O -0.0023(5) 0.1326(2) 0.2994(2) 0.0494(14) Uani 1 1 d . . . O10 O -0.0096(4) 0.2523(2) 0.24413(17) 0.0384(12) Uani 1 1 d . . . O11 O -0.0505(4) 0.3494(2) 0.29421(17) 0.0405(13) Uani 1 1 d . . . O12 O -0.0839(5) 0.3489(2) 0.41397(18) 0.0444(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 Cl9 0.0387(14) 0.155(3) 0.0395(12) -0.0064(15) 0.0001(10) 0.0110(16) Cl10 0.0405(14) 0.198(4) 0.0396(13) -0.0131(18) -0.0004(11) 0.0169(18) O1W 0.030(3) 0.059(4) 0.053(3) 0.009(3) 0.006(3) 0.006(3) O2W 0.034(3) 0.075(4) 0.035(3) -0.010(3) -0.001(2) 0.010(3) O3W 0.032(3) 0.061(4) 0.059(4) 0.010(3) 0.004(3) 0.002(3) O4W 0.035(3) 0.091(5) 0.051(4) 0.019(3) -0.015(3) -0.004(3) O5W 0.043(3) 0.078(4) 0.028(3) -0.009(3) 0.001(2) 0.003(3) O6W 0.032(3) 0.042(3) 0.074(4) 0.009(3) 0.006(3) -0.001(2) O7W 0.035(3) 0.071(4) 0.046(3) 0.006(3) 0.000(3) -0.008(3) O8W 0.030(3) 0.086(4) 0.034(3) -0.013(3) 0.001(2) 0.002(3) O9W 0.041(3) 0.087(5) 0.035(3) -0.004(3) 0.003(3) 0.010(3) O10W 0.041(4) 0.077(4) 0.052(4) 0.015(3) -0.015(3) -0.005(3) Gd1 0.0161(2) 0.0525(3) 0.0313(2) 0.00044(15) 0.00394(15) -0.00217(15) Gd2 0.0164(2) 0.0549(3) 0.0315(2) 0.00087(16) 0.00418(15) -0.00210(15) Cl1 0.088(2) 0.0649(16) 0.0513(14) 0.0010(11) 0.0238(13) 0.0156(13) Cl2 0.178(4) 0.140(4) 0.145(4) -0.039(3) -0.037(3) 0.083(3) Cl3 0.218(5) 0.160(4) 0.226(5) 0.109(4) 0.158(4) 0.115(4) Cl4 0.096(3) 0.107(3) 0.277(6) -0.028(4) 0.038(3) -0.017(2) Cl5 0.159(3) 0.090(2) 0.0689(19) 0.0095(15) 0.051(2) 0.040(2) Cl6 0.212(5) 0.137(4) 0.156(4) 0.061(3) 0.119(4) 0.099(3) Cl7 0.251(6) 0.224(6) 0.132(4) -0.043(4) -0.014(4) 0.164(5) Cl8 0.139(4) 0.140(5) 0.559(14) -0.094(7) 0.156(6) -0.048(4) Zn1 0.0964(11) 0.0737(9) 0.0959(10) -0.0004(7) 0.0262(8) 0.0106(8) Zn2 0.1081(12) 0.0778(10) 0.1015(11) 0.0004(8) 0.0340(9) 0.0155(9) C1 0.020(4) 0.047(5) 0.029(4) -0.002(3) 0.004(3) -0.005(3) C2 0.023(4) 0.049(5) 0.028(4) -0.004(3) 0.001(3) -0.001(3) C3 0.018(4) 0.054(5) 0.025(4) -0.001(3) 0.008(3) 0.000(3) C4 0.023(4) 0.045(4) 0.024(3) -0.002(3) 0.006(3) -0.004(3) C5 0.021(4) 0.053(5) 0.028(4) 0.004(3) 0.002(3) 0.008(3) C6 0.017(4) 0.048(5) 0.048(4) 0.004(4) 0.014(3) -0.001(3) C7 0.014(4) 0.043(4) 0.039(4) 0.009(3) 0.001(3) 0.003(3) C8 0.023(4) 0.040(4) 0.034(4) 0.001(3) 0.001(3) -0.001(3) C9 0.015(4) 0.043(5) 0.050(5) 0.004(3) -0.001(3) -0.002(3) C10 0.031(4) 0.032(4) 0.053(5) -0.006(3) 0.011(4) -0.003(3) C11 0.028(4) 0.039(4) 0.040(4) 0.002(3) 0.001(3) 0.005(3) C12 0.033(4) 0.039(5) 0.055(5) -0.004(4) 0.010(4) -0.013(4) C13 0.017(4) 0.046(5) 0.030(4) -0.003(3) 0.000(3) 0.007(3) C14 0.029(4) 0.034(4) 0.042(4) -0.010(3) 0.002(3) 0.001(3) C15 0.034(4) 0.033(4) 0.039(4) -0.007(3) 0.005(3) -0.004(3) C16 0.025(4) 0.039(4) 0.049(5) -0.008(4) 0.003(3) -0.003(3) C17 0.026(4) 0.048(5) 0.033(4) -0.005(3) 0.012(3) 0.007(3) C18 0.022(4) 0.045(5) 0.047(4) 0.001(4) 0.004(3) -0.009(3) C19 0.014(4) 0.055(5) 0.031(4) -0.001(3) 0.010(3) -0.005(3) C20 0.027(4) 0.045(5) 0.030(4) -0.001(3) 0.009(3) -0.001(3) C21 0.020(4) 0.049(5) 0.027(4) 0.001(3) 0.002(3) 0.001(3) C22 0.017(4) 0.043(4) 0.030(4) 0.002(3) -0.001(3) 0.003(3) C23 0.024(4) 0.042(5) 0.055(5) 0.000(4) 0.011(4) -0.010(3) C24 0.026(4) 0.045(5) 0.032(4) 0.006(3) 0.004(3) -0.005(3) C25 0.024(4) 0.037(4) 0.065(6) -0.008(4) 0.007(4) 0.004(3) C26 0.028(4) 0.038(4) 0.039(4) 0.006(3) 0.009(3) -0.005(3) C27 0.029(4) 0.036(4) 0.044(4) -0.001(3) 0.006(3) 0.000(3) C28 0.016(4) 0.048(5) 0.034(4) 0.004(3) 0.001(3) 0.007(3) C29 0.036(5) 0.044(5) 0.054(5) -0.001(4) 0.014(4) -0.008(4) C30 0.030(4) 0.041(4) 0.048(5) -0.004(3) 0.017(4) 0.007(3) C31 0.024(4) 0.041(5) 0.054(5) -0.005(4) 0.002(4) -0.006(3) C32 0.025(4) 0.043(4) 0.042(4) -0.010(3) 0.011(3) -0.001(3) C33 0.024(4) 0.032(4) 0.043(4) -0.012(3) 0.006(3) -0.004(3) C34 0.021(4) 0.040(4) 0.032(4) -0.004(3) 0.002(3) 0.002(3) C35 0.026(4) 0.052(5) 0.043(5) -0.009(4) 0.002(3) -0.004(3) C36 0.018(4) 0.050(5) 0.036(4) -0.001(3) 0.005(3) 0.007(3) N1 0.014(3) 0.041(4) 0.039(3) 0.002(3) 0.002(3) 0.000(3) N2 0.016(3) 0.048(4) 0.041(4) 0.000(3) 0.006(3) 0.003(3) N3 0.018(3) 0.046(4) 0.037(3) 0.003(3) 0.003(3) 0.001(3) N4 0.018(3) 0.039(4) 0.031(3) -0.003(3) 0.003(2) 0.000(3) N5 0.020(3) 0.043(4) 0.032(3) -0.001(3) 0.004(3) -0.009(3) N6 0.016(3) 0.041(4) 0.039(3) -0.002(3) 0.006(3) -0.004(2) N7 0.017(3) 0.046(4) 0.044(4) -0.001(3) 0.003(3) 0.000(3) N8 0.029(3) 0.036(4) 0.050(4) -0.003(3) 0.005(3) 0.001(3) N9 0.024(3) 0.037(4) 0.041(4) -0.001(3) -0.001(3) -0.003(3) N10 0.019(3) 0.045(4) 0.035(3) -0.006(3) 0.008(3) -0.006(3) N11 0.025(3) 0.048(4) 0.046(4) 0.012(3) 0.006(3) -0.001(3) N12 0.016(3) 0.047(4) 0.045(4) 0.006(3) 0.000(3) 0.001(3) N13 0.017(3) 0.043(4) 0.029(3) -0.001(3) -0.003(2) 0.001(2) N14 0.018(3) 0.040(4) 0.037(3) -0.002(3) 0.005(3) -0.001(3) N15 0.016(3) 0.048(4) 0.037(3) 0.001(3) 0.003(3) -0.003(3) N16 0.013(3) 0.044(4) 0.034(3) 0.001(3) 0.007(2) -0.003(3) N17 0.016(3) 0.038(4) 0.046(4) -0.004(3) 0.002(3) 0.002(3) N18 0.022(3) 0.046(4) 0.055(4) -0.008(3) 0.006(3) -0.001(3) N19 0.021(3) 0.036(3) 0.037(3) 0.004(3) 0.005(3) -0.004(2) N20 0.025(3) 0.040(4) 0.037(3) -0.003(3) 0.005(3) -0.001(3) N21 0.023(3) 0.042(4) 0.064(4) 0.002(3) 0.013(3) 0.000(3) N22 0.027(3) 0.042(4) 0.046(4) 0.005(3) 0.005(3) 0.004(3) N23 0.025(3) 0.045(4) 0.033(3) -0.001(3) 0.007(3) -0.003(3) N24 0.025(3) 0.039(4) 0.039(4) 0.003(3) 0.006(3) 0.002(3) O1 0.014(2) 0.058(3) 0.040(3) 0.002(2) 0.008(2) 0.004(2) O2 0.019(3) 0.065(4) 0.036(3) -0.001(2) -0.002(2) -0.010(2) O3 0.029(3) 0.068(4) 0.030(3) 0.000(2) 0.003(2) -0.012(3) O4 0.013(3) 0.056(3) 0.044(3) 0.003(2) 0.003(2) -0.001(2) O5 0.039(4) 0.082(5) 0.085(5) -0.029(4) -0.006(3) 0.015(3) O6 0.025(3) 0.065(4) 0.069(4) 0.013(3) 0.016(3) 0.008(3) O7 0.013(3) 0.052(3) 0.044(3) 0.001(2) -0.002(2) -0.003(2) O8 0.028(3) 0.082(5) 0.067(4) -0.012(3) -0.005(3) 0.016(3) O9 0.024(3) 0.056(4) 0.069(4) 0.005(3) 0.010(3) 0.010(3) O10 0.014(2) 0.059(3) 0.043(3) 0.005(3) 0.009(2) -0.001(2) O11 0.022(3) 0.056(3) 0.044(3) -0.002(2) 0.005(2) -0.010(2) O12 0.029(3) 0.062(4) 0.042(3) -0.002(3) 0.003(2) -0.009(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 O1W Gd1 2.374(6) . ? O2W Gd1 2.386(5) . ? O3W Gd1 2.403(6) . ? O4W Gd1 2.414(6) . ? O5W Gd1 2.436(5) . ? O6W Gd2 2.408(5) . ? O7W Gd2 2.403(6) . ? O8W Gd2 2.385(5) . ? O9W Gd2 2.446(5) . ? O10W Gd2 2.421(6) . ? Gd1 O1 2.329(4) . ? Gd1 O7 2.394(5) 1_655 ? Gd1 O2 2.397(5) . ? Gd2 O10 2.330(5) . ? Gd2 O4 2.391(5) 1_455 ? Gd2 O11 2.411(5) . ? Cl1 Zn1 2.226(3) . ? Cl2 Zn1 2.276(5) . ? Cl3 Zn1 2.266(4) . ? Cl4 Zn1 2.248(5) . ? Cl5 Zn2 2.221(3) . ? Cl6 Zn2 2.243(4) . ? Cl7 Zn2 2.240(5) . ? Cl8 Zn2 2.224(6) . ? C1 O1 1.229(8) . ? C1 N1 1.361(9) . ? C1 N2 1.373(10) . ? C2 N3 1.429(9) . ? C2 N1 1.454(9) . ? C2 C3 1.530(10) . ? C2 H2 0.9900 . ? C3 N2 1.441(8) . ? C3 N4 1.468(9) . ? C3 H3 0.9900 . ? C4 O7 1.217(8) . ? C4 N3 1.357(9) . ? C4 N4 1.381(9) . ? C5 N5 1.427(9) . ? C5 N2 1.430(9) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.453(9) . ? C6 N4 1.450(9) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.233(8) . ? C7 N5 1.360(8) . ? C7 N6 1.359(9) . ? C8 N5 1.468(9) . ? C8 N7 1.469(9) . ? C8 C9 1.529(10) . ? C8 H8 0.9900 . ? C9 N8 1.426(9) . ? C9 N6 1.458(8) . ? C9 H9 0.9900 . ? C10 O8 1.223(9) . ? C10 N7 1.369(10) . ? C10 N8 1.373(9) . ? C11 N9 1.431(9) . ? C11 N6 1.478(8) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.443(9) . ? C12 N8 1.457(10) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.212(8) . ? C13 N9 1.339(9) . ? C13 N10 1.367(9) . ? C14 N11 1.432(9) . ? C14 N9 1.480(9) . ? C14 C15 1.524(10) . ? C14 H14 0.9900 . ? C15 N12 1.432(9) . ? C15 N10 1.491(9) . ? C15 H15 0.9900 . ? C16 O9 1.207(8) . ? C16 N11 1.360(10) . ? C16 N12 1.366(9) . ? C17 N13 1.447(9) . ? C17 N10 1.455(9) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.426(9) . ? C18 N15 1.431(9) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.226(9) . ? C19 N13 1.336(9) . ? C19 N14 1.381(9) . ? C20 N13 1.460(9) . ? C20 N15 1.477(8) . ? C20 C21 1.540(10) . ? C20 H20 0.9900 . ? C21 N16 1.419(8) . ? C21 N14 1.463(9) . ? C21 H21 0.9900 . ? C22 O10 1.231(8) . ? C22 N16 1.360(9) . ? C22 N15 1.362(9) . ? C23 N17 1.431(9) . ? C23 N14 1.450(9) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N19 1.430(9) . ? C24 N16 1.454(9) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O5 1.240(9) . ? C25 N18 1.337(9) . ? C25 N17 1.359(10) . ? C26 N17 1.441(9) . ? C26 N19 1.499(9) . ? C26 C27 1.516(10) . ? C26 H26 0.9900 . ? C27 N18 1.419(9) . ? C27 N20 1.457(9) . ? C27 H27 0.9900 . ? C28 O11 1.223(8) . ? C28 N20 1.354(9) . ? C28 N19 1.355(8) . ? C29 N21 1.464(9) . ? C29 N18 1.475(10) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N23 1.435(9) . ? C30 N20 1.466(8) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O6 1.215(9) . ? C31 N21 1.347(10) . ? C31 N22 1.362(9) . ? C32 N21 1.445(9) . ? C32 N23 1.453(9) . ? C32 C33 1.581(10) . ? C32 H32 0.9900 . ? C33 N24 1.417(9) . ? C33 N22 1.444(9) . ? C33 H33 0.9900 . ? C34 O12 1.230(8) . ? C34 N24 1.357(9) . ? C34 N23 1.363(9) . ? C35 N1 1.416(10) . ? C35 N22 1.451(10) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N3 1.455(9) . ? C36 N24 1.485(9) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? O4 Gd2 2.391(5) 1_655 ? O7 Gd1 2.394(5) 1_455 ? 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 Gd1 O1W 78.95(18) . . ? O1 Gd1 O2W 145.27(18) . . ? O1W Gd1 O2W 107.2(2) . . ? O1 Gd1 O7 140.05(18) . 1_655 ? O1W Gd1 O7 76.90(18) . 1_655 ? O2W Gd1 O7 73.07(18) . 1_655 ? O1 Gd1 O2 79.59(18) . . ? O1W Gd1 O2 140.46(18) . . ? O2W Gd1 O2 74.59(18) . . ? O7 Gd1 O2 136.97(18) 1_655 . ? O1 Gd1 O3W 104.75(18) . . ? O1W Gd1 O3W 149.18(19) . . ? O2W Gd1 O3W 87.3(2) . . ? O7 Gd1 O3W 81.85(18) 1_655 . ? O2 Gd1 O3W 68.99(18) . . ? O1 Gd1 O4W 79.69(19) . . ? O1W Gd1 O4W 71.0(2) . . ? O2W Gd1 O4W 70.8(2) . . ? O7 Gd1 O4W 120.65(18) 1_655 . ? O2 Gd1 O4W 72.7(2) . . ? O3W Gd1 O4W 139.7(2) . . ? O1 Gd1 O5W 69.21(18) . . ? O1W Gd1 O5W 79.9(2) . . ? O2W Gd1 O5W 145.06(18) . . ? O7 Gd1 O5W 75.54(17) 1_655 . ? O2 Gd1 O5W 121.91(19) . . ? O3W Gd1 O5W 73.3(2) . . ? O4W Gd1 O5W 140.8(2) . . ? O10 Gd2 O8W 145.07(18) . . ? O10 Gd2 O4 139.88(18) . 1_455 ? O8W Gd2 O4 73.37(18) . 1_455 ? O10 Gd2 O7W 104.16(18) . . ? O8W Gd2 O7W 88.4(2) . . ? O4 Gd2 O7W 82.04(17) 1_455 . ? O10 Gd2 O6W 78.79(18) . . ? O8W Gd2 O6W 107.4(2) . . ? O4 Gd2 O6W 76.66(18) 1_455 . ? O7W Gd2 O6W 148.26(19) . . ? O10 Gd2 O11 79.87(18) . . ? O8W Gd2 O11 74.29(18) . . ? O4 Gd2 O11 136.92(17) 1_455 . ? O7W Gd2 O11 69.31(18) . . ? O6W Gd2 O11 140.82(18) . . ? O10 Gd2 O10W 79.3(2) . . ? O8W Gd2 O10W 70.8(2) . . ? O4 Gd2 O10W 121.03(19) 1_455 . ? O7W Gd2 O10W 140.2(2) . . ? O6W Gd2 O10W 71.5(2) . . ? O11 Gd2 O10W 72.5(2) . . ? O10 Gd2 O9W 69.16(18) . . ? O8W Gd2 O9W 145.34(18) . . ? O4 Gd2 O9W 75.45(18) 1_455 . ? O7W Gd2 O9W 72.6(2) . . ? O6W Gd2 O9W 79.4(2) . . ? O11 Gd2 O9W 122.15(19) . . ? O10W Gd2 O9W 140.5(2) . . ? Cl1 Zn1 Cl4 108.57(15) . . ? Cl1 Zn1 Cl3 108.32(13) . . ? Cl4 Zn1 Cl3 111.1(2) . . ? Cl1 Zn1 Cl2 111.22(13) . . ? Cl4 Zn1 Cl2 106.6(2) . . ? Cl3 Zn1 Cl2 111.0(2) . . ? Cl8 Zn2 Cl5 110.5(2) . . ? Cl8 Zn2 Cl7 106.6(3) . . ? Cl5 Zn2 Cl7 109.52(16) . . ? Cl8 Zn2 Cl6 109.5(3) . . ? Cl5 Zn2 Cl6 110.84(14) . . ? Cl7 Zn2 Cl6 109.7(2) . . ? O1 C1 N1 124.7(7) . . ? O1 C1 N2 125.3(7) . . ? N1 C1 N2 109.9(6) . . ? N3 C2 N1 114.4(6) . . ? N3 C2 C3 103.9(6) . . ? N1 C2 C3 103.3(5) . . ? N3 C2 H2 111.5 . . ? N1 C2 H2 111.5 . . ? C3 C2 H2 111.5 . . ? N2 C3 N4 114.3(6) . . ? N2 C3 C2 105.0(6) . . ? N4 C3 C2 103.2(6) . . ? N2 C3 H3 111.3 . . ? N4 C3 H3 111.3 . . ? C2 C3 H3 111.3 . . ? O7 C4 N3 126.8(7) . . ? O7 C4 N4 125.6(7) . . ? N3 C4 N4 107.6(6) . . ? N5 C5 N2 113.7(6) . . ? N5 C5 H5A 108.8 . . ? N2 C5 H5A 108.8 . . ? N5 C5 H5B 108.8 . . ? N2 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N7 C6 N4 113.7(5) . . ? N7 C6 H6A 108.8 . . ? N4 C6 H6A 108.8 . . ? N7 C6 H6B 108.8 . . ? N4 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N5 125.6(7) . . ? O2 C7 N6 126.2(6) . . ? N5 C7 N6 108.2(6) . . ? N5 C8 N7 112.9(6) . . ? N5 C8 C9 103.2(5) . . ? N7 C8 C9 103.0(6) . . ? N5 C8 H8 112.4 . . ? N7 C8 H8 112.4 . . ? C9 C8 H8 112.4 . . ? N8 C9 N6 113.6(6) . . ? N8 C9 C8 104.1(6) . . ? N6 C9 C8 103.2(6) . . ? N8 C9 H9 111.8 . . ? N6 C9 H9 111.8 . . ? C8 C9 H9 111.8 . . ? O8 C10 N7 127.0(7) . . ? O8 C10 N8 125.0(8) . . ? N7 C10 N8 107.8(7) . . ? N9 C11 N6 113.8(6) . . ? N9 C11 H11A 108.8 . . ? N6 C11 H11A 108.8 . . ? N9 C11 H11B 108.8 . . ? N6 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? N11 C12 N8 114.9(6) . . ? N11 C12 H12A 108.6 . . ? N8 C12 H12A 108.6 . . ? N11 C12 H12B 108.6 . . ? N8 C12 H12B 108.6 . . ? H12A C12 H12B 107.5 . . ? O3 C13 N9 126.4(7) . . ? O3 C13 N10 124.9(7) . . ? N9 C13 N10 108.7(6) . . ? N11 C14 N9 116.2(6) . . ? N11 C14 C15 103.6(6) . . ? N9 C14 C15 103.3(6) . . ? N11 C14 H14 111.0 . . ? N9 C14 H14 111.0 . . ? C15 C14 H14 111.0 . . ? N12 C15 N10 115.0(6) . . ? N12 C15 C14 103.2(6) . . ? N10 C15 C14 102.8(6) . . ? N12 C15 H15 111.7 . . ? N10 C15 H15 111.7 . . ? C14 C15 H15 111.7 . . ? O9 C16 N11 124.8(7) . . ? O9 C16 N12 127.9(8) . . ? N11 C16 N12 107.3(6) . . ? N13 C17 N10 114.3(5) . . ? N13 C17 H17A 108.7 . . ? N10 C17 H17A 108.7 . . ? N13 C17 H17B 108.7 . . ? N10 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? N12 C18 N15 113.8(6) . . ? N12 C18 H18A 108.8 . . ? N15 C18 H18A 108.8 . . ? N12 C18 H18B 108.8 . . ? N15 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? O4 C19 N13 126.5(7) . . ? O4 C19 N14 124.7(7) . . ? N13 C19 N14 108.8(6) . . ? N13 C20 N15 113.5(6) . . ? N13 C20 C21 103.7(6) . . ? N15 C20 C21 103.0(5) . . ? N13 C20 H20 112.0 . . ? N15 C20 H20 112.0 . . ? C21 C20 H20 112.0 . . ? N16 C21 N14 114.6(6) . . ? N16 C21 C20 104.1(6) . . ? N14 C21 C20 102.8(6) . . ? N16 C21 H21 111.6 . . ? N14 C21 H21 111.6 . . ? C20 C21 H21 111.6 . . ? O10 C22 N16 127.1(7) . . ? O10 C22 N15 123.5(7) . . ? N16 C22 N15 109.4(6) . . ? N17 C23 N14 114.8(6) . . ? N17 C23 H23A 108.6 . . ? N14 C23 H23A 108.6 . . ? N17 C23 H23B 108.6 . . ? N14 C23 H23B 108.6 . . ? H23A C23 H23B 107.5 . . ? N19 C24 N16 113.2(6) . . ? N19 C24 H24A 108.9 . . ? N16 C24 H24A 108.9 . . ? N19 C24 H24B 108.9 . . ? N16 C24 H24B 108.9 . . ? H24A C24 H24B 107.8 . . ? O5 C25 N18 122.9(8) . . ? O5 C25 N17 126.9(7) . . ? N18 C25 N17 109.9(7) . . ? N17 C26 N19 112.2(6) . . ? N17 C26 C27 104.2(6) . . ? N19 C26 C27 101.9(5) . . ? N17 C26 H26 112.6 . . ? N19 C26 H26 112.6 . . ? C27 C26 H26 112.6 . . ? N18 C27 N20 115.7(6) . . ? N18 C27 C26 103.1(6) . . ? N20 C27 C26 104.8(6) . . ? N18 C27 H27 110.9 . . ? N20 C27 H27 110.9 . . ? C26 C27 H27 110.9 . . ? O11 C28 N20 125.7(6) . . ? O11 C28 N19 125.4(7) . . ? N20 C28 N19 108.9(6) . . ? N21 C29 N18 114.5(6) . . ? N21 C29 H29A 108.6 . . ? N18 C29 H29A 108.6 . . ? N21 C29 H29B 108.6 . . ? N18 C29 H29B 108.6 . . ? H29A C29 H29B 107.6 . . ? N23 C30 N20 113.4(6) . . ? N23 C30 H30A 108.9 . . ? N20 C30 H30A 108.9 . . ? N23 C30 H30B 108.9 . . ? N20 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? O6 C31 N21 124.4(7) . . ? O6 C31 N22 128.2(8) . . ? N21 C31 N22 107.4(6) . . ? N21 C32 N23 114.7(6) . . ? N21 C32 C33 102.6(6) . . ? N23 C32 C33 101.8(5) . . ? N21 C32 H32 112.3 . . ? N23 C32 H32 112.3 . . ? C33 C32 H32 112.3 . . ? N24 C33 N22 116.8(6) . . ? N24 C33 C32 102.8(6) . . ? N22 C33 C32 101.4(5) . . ? N24 C33 H33 111.7 . . ? N22 C33 H33 111.7 . . ? C32 C33 H33 111.7 . . ? O12 C34 N24 126.0(7) . . ? O12 C34 N23 126.2(7) . . ? N24 C34 N23 107.8(6) . . ? N1 C35 N22 113.7(6) . . ? N1 C35 H35A 108.8 . . ? N22 C35 H35A 108.8 . . ? N1 C35 H35B 108.8 . . ? N22 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? N3 C36 N24 113.2(5) . . ? N3 C36 H36A 108.9 . . ? N24 C36 H36A 108.9 . . ? N3 C36 H36B 108.9 . . ? N24 C36 H36B 108.9 . . ? H36A C36 H36B 107.8 . . ? C1 N1 C35 121.6(6) . . ? C1 N1 C2 111.3(6) . . ? C35 N1 C2 124.9(6) . . ? C1 N2 C5 122.6(6) . . ? C1 N2 C3 110.4(6) . . ? C5 N2 C3 125.9(6) . . ? C4 N3 C2 113.6(6) . . ? C4 N3 C36 122.8(6) . . ? C2 N3 C36 122.9(6) . . ? C4 N4 C6 125.0(6) . . ? C4 N4 C3 111.4(6) . . ? C6 N4 C3 123.2(6) . . ? C7 N5 C5 123.4(6) . . ? C7 N5 C8 112.1(6) . . ? C5 N5 C8 124.1(5) . . ? C7 N6 C9 112.7(6) . . ? C7 N6 C11 121.9(6) . . ? C9 N6 C11 124.0(6) . . ? C10 N7 C6 121.3(6) . . ? C10 N7 C8 111.5(6) . . ? C6 N7 C8 124.0(6) . . ? C10 N8 C9 112.9(6) . . ? C10 N8 C12 121.0(6) . . ? C9 N8 C12 126.0(6) . . ? C13 N9 C11 122.2(6) . . ? C13 N9 C14 112.9(6) . . ? C11 N9 C14 123.1(6) . . ? C13 N10 C17 125.5(6) . . ? C13 N10 C15 112.0(6) . . ? C17 N10 C15 122.4(6) . . ? C16 N11 C14 112.6(6) . . ? C16 N11 C12 121.9(6) . . ? C14 N11 C12 125.4(6) . . ? C16 N12 C15 112.4(6) . . ? C16 N12 C18 121.3(6) . . ? C15 N12 C18 123.7(6) . . ? C19 N13 C17 125.0(6) . . ? C19 N13 C20 112.8(6) . . ? C17 N13 C20 121.5(6) . . ? C19 N14 C23 125.8(6) . . ? C19 N14 C21 111.8(6) . . ? C23 N14 C21 122.1(6) . . ? C22 N15 C18 123.5(6) . . ? C22 N15 C20 110.6(6) . . ? C18 N15 C20 123.6(6) . . ? C22 N16 C21 112.7(6) . . ? C22 N16 C24 121.2(6) . . ? C21 N16 C24 124.7(6) . . ? C25 N17 C23 122.1(6) . . ? C25 N17 C26 109.4(6) . . ? C23 N17 C26 124.7(6) . . ? C25 N18 C27 112.0(7) . . ? C25 N18 C29 122.6(7) . . ? C27 N18 C29 125.4(6) . . ? C28 N19 C24 124.2(6) . . ? C28 N19 C26 111.8(6) . . ? C24 N19 C26 123.7(5) . . ? C28 N20 C27 112.0(6) . . ? C28 N20 C30 122.6(6) . . ? C27 N20 C30 123.9(6) . . ? C31 N21 C32 113.9(6) . . ? C31 N21 C29 122.6(6) . . ? C32 N21 C29 123.2(7) . . ? C31 N22 C33 114.3(6) . . ? C31 N22 C35 121.7(6) . . ? C33 N22 C35 122.2(6) . . ? C34 N23 C30 121.7(6) . . ? C34 N23 C32 112.8(6) . . ? C30 N23 C32 123.1(6) . . ? C34 N24 C33 114.2(6) . . ? C34 N24 C36 123.2(6) . . ? C33 N24 C36 122.3(6) . . ? C1 O1 Gd1 156.3(5) . . ? C7 O2 Gd1 154.8(5) . . ? C19 O4 Gd2 154.6(5) . 1_655 ? C4 O7 Gd1 154.6(4) . 1_455 ? C22 O10 Gd2 155.9(5) . . ? C28 O11 Gd2 154.6(5) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.311 _refine_diff_density_min -2.674 _refine_diff_density_rms 0.176 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.495 0.000 -0.005 960 331 ' ' 2 0.250 0.246 0.871 88 28 ' ' 3 0.250 0.254 0.371 88 29 ' ' 4 1.111 0.500 0.111 960 332 ' ' 5 0.750 0.746 0.629 88 28 ' ' 6 0.750 0.754 0.129 88 28 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 902618' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p309 #TrackingRef 'submit-309.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H124 Cl10 N24 O56 Tb2 Zn2' _chemical_formula_weight 2592.67 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 10.3566(9) _cell_length_b 27.003(3) _cell_length_c 28.938(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.463(3) _cell_angle_gamma 90.00 _cell_volume 8056.0(13) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5264 _exptl_absorpt_coefficient_mu 2.785 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5668 _exptl_absorpt_correction_T_max 0.6801 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74424 _diffrn_reflns_av_R_equivalents 0.0770 _diffrn_reflns_av_sigmaI/netI 0.0628 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 26.00 _reflns_number_total 15592 _reflns_number_gt 12494 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1431P)^2^+131.5981P] 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 15592 _refine_ls_number_parameters 835 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1098 _refine_ls_R_factor_gt 0.0960 _refine_ls_wR_factor_ref 0.2689 _refine_ls_wR_factor_gt 0.2589 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 Cl9 Cl 1.4840(3) 0.2527(2) 0.62141(12) 0.0685(12) Uani 1 1 d . . . Cl10 Cl 0.0164(4) 0.2458(2) 0.12118(13) 0.0814(15) Uani 1 1 d . . . Cl1 Cl 1.2553(4) -0.10623(14) 0.38185(13) 0.0592(10) Uani 1 1 d . . . Cl2 Cl 1.0383(9) -0.0232(3) 0.3075(3) 0.143(3) Uani 1 1 d . . . Cl3 Cl 1.2898(7) 0.0273(3) 0.3891(4) 0.155(4) Uani 1 1 d . . . Cl4 Cl 1.0081(10) -0.0364(3) 0.4346(4) 0.193(5) Uani 1 1 d . . . Cl5 Cl 0.2301(6) 0.6127(2) 0.37414(16) 0.0886(16) Uani 1 1 d . . . Cl6 Cl 0.4620(9) 0.5447(3) 0.3094(3) 0.156(4) Uani 1 1 d . . . Cl7 Cl 0.4699(13) 0.5313(5) 0.4353(3) 0.244(8) Uani 1 1 d . . . Cl8 Cl 0.2091(10) 0.4787(4) 0.3639(7) 0.285(10) Uani 1 1 d . . . Zn1 Zn 1.1461(2) -0.03487(8) 0.37866(9) 0.0765(6) Uani 1 1 d . . . Zn2 Zn 0.3410(3) 0.54306(8) 0.36980(9) 0.0836(7) Uani 1 1 d . . . O1W O 0.2441(8) 0.3527(3) 0.2280(3) 0.041(2) Uani 1 1 d . . . O2W O 0.2851(7) 0.1943(3) 0.2854(3) 0.0352(18) Uani 1 1 d . . . O3W O 0.4345(9) 0.2591(4) 0.3444(3) 0.052(2) Uani 1 1 d . . . O4W O 0.2202(8) 0.3204(4) 0.3378(3) 0.042(2) Uani 1 1 d . . . O5W O 0.2563(8) 0.2540(4) 0.1944(3) 0.048(2) Uani 1 1 d . . . O6W O 1.2783(8) 0.1888(4) 0.4043(3) 0.046(2) Uani 1 1 d . . . O7W O 1.2516(8) 0.1557(3) 0.5115(3) 0.044(2) Uani 1 1 d . . . O8W O 1.0647(9) 0.2499(4) 0.3967(3) 0.050(2) Uani 1 1 d . . . O9W O 1.2149(7) 0.3136(3) 0.4570(3) 0.0375(18) Uani 1 1 d . . . O10W O 1.2430(8) 0.2543(4) 0.5476(3) 0.045(2) Uani 1 1 d . . . Tb1 Tb 0.30386(4) 0.28134(2) 0.274082(17) 0.02685(17) Uani 1 1 d . . . Tb2 Tb 1.19316(4) 0.227826(19) 0.468039(17) 0.02625(17) Uani 1 1 d . . . C1 C 0.5471(9) 0.3750(4) 0.2905(4) 0.0282(16) Uani 1 1 d . . . C2 C 0.7098(10) 0.4323(4) 0.3066(4) 0.031(2) Uani 1 1 d . . . H2 H 0.6950 0.4683 0.3021 0.037 Uiso 1 1 calc R . . C3 C 0.7299(10) 0.4072(4) 0.2617(4) 0.030(2) Uani 1 1 d . . . H3 H 0.7372 0.4312 0.2363 0.036 Uiso 1 1 calc R . . C4 C 0.9069(10) 0.3904(4) 0.3146(4) 0.034(3) Uani 1 1 d . . . C5 C 0.5883(9) 0.3448(4) 0.2128(4) 0.0278(13) Uani 1 1 d . . . H5A H 0.6134 0.3625 0.1854 0.033 Uiso 1 1 calc R . . H5B H 0.4947 0.3387 0.2081 0.033 Uiso 1 1 calc R . . C6 C 0.9216(9) 0.3556(4) 0.2379(4) 0.0278(13) Uani 1 1 d . . . H6A H 0.9064 0.3740 0.2087 0.033 Uiso 1 1 calc R . . H6B H 1.0142 0.3582 0.2483 0.033 Uiso 1 1 calc R . . C7 C 0.5972(10) 0.2554(4) 0.2295(4) 0.028(2) Uani 1 1 d . . . C8 C 0.7766(10) 0.2884(4) 0.1991(4) 0.027(2) Uani 1 1 d . . . H8 H 0.7781 0.3017 0.1673 0.033 Uiso 1 1 calc R . . C9 C 0.7882(9) 0.2316(4) 0.1998(4) 0.024(2) Uani 1 1 d . . . H9 H 0.7895 0.2177 0.1682 0.029 Uiso 1 1 calc R . . C10 C 0.9681(10) 0.2649(4) 0.2438(4) 0.026(2) Uani 1 1 d . . . C11 C 0.6245(10) 0.1661(4) 0.2224(4) 0.032(2) Uani 1 1 d . . . H11A H 0.6433 0.1493 0.1938 0.038 Uiso 1 1 calc R . . H11B H 0.5301 0.1669 0.2231 0.038 Uiso 1 1 calc R . . C12 C 0.9683(9) 0.1735(4) 0.2332(4) 0.0278(13) Uani 1 1 d . . . H12A H 0.9507 0.1559 0.2037 0.033 Uiso 1 1 calc R . . H12B H 1.0626 0.1768 0.2394 0.033 Uiso 1 1 calc R . . C13 C 0.6102(11) 0.1220(4) 0.2950(4) 0.035(3) Uani 1 1 d . . . C14 C 0.8046(9) 0.1127(4) 0.2623(4) 0.026(2) Uani 1 1 d . . . H14 H 0.8080 0.0908 0.2350 0.032 Uiso 1 1 calc R . . C15 C 0.8104(10) 0.0828(4) 0.3084(4) 0.031(2) Uani 1 1 d . . . H15 H 0.8256 0.0472 0.3027 0.037 Uiso 1 1 calc R . . C16 C 0.9829(10) 0.1389(4) 0.3135(4) 0.027(2) Uani 1 1 d . . . C17 C 0.6347(11) 0.0645(4) 0.3619(4) 0.034(2) Uani 1 1 d . . . H17A H 0.5399 0.0629 0.3567 0.041 Uiso 1 1 calc R . . H17B H 0.6675 0.0305 0.3622 0.041 Uiso 1 1 calc R . . C18 C 0.9682(10) 0.0848(4) 0.3811(4) 0.031(2) Uani 1 1 d . . . H18A H 0.9629 0.0486 0.3797 0.037 Uiso 1 1 calc R . . H18B H 1.0601 0.0936 0.3870 0.037 Uiso 1 1 calc R . . C19 C 0.5884(10) 0.1170(4) 0.4282(4) 0.035(3) Uani 1 1 d . . . C20 C 0.7870(10) 0.0765(4) 0.4347(4) 0.030(2) Uani 1 1 d . . . H20 H 0.8019 0.0404 0.4387 0.036 Uiso 1 1 calc R . . C21 C 0.7678(10) 0.1023(4) 0.4814(4) 0.028(2) Uani 1 1 d . . . H21 H 0.7623 0.0783 0.5070 0.034 Uiso 1 1 calc R . . C22 C 0.9508(9) 0.1343(4) 0.4512(4) 0.0282(16) Uani 1 1 d . . . C23 C 0.5730(10) 0.1531(4) 0.5058(4) 0.030(2) Uani 1 1 d . . . H23A H 0.4802 0.1507 0.4957 0.036 Uiso 1 1 calc R . . H23B H 0.5887 0.1352 0.5353 0.036 Uiso 1 1 calc R . . C24 C 0.9097(10) 0.1638(4) 0.5284(4) 0.031(2) Uani 1 1 d . . . H24A H 1.0034 0.1697 0.5331 0.037 Uiso 1 1 calc R . . H24B H 0.8844 0.1460 0.5557 0.037 Uiso 1 1 calc R . . C25 C 0.5290(9) 0.2426(4) 0.4991(4) 0.027(2) Uani 1 1 d . . . C26 C 0.7197(9) 0.2204(4) 0.5429(4) 0.023(2) Uani 1 1 d . . . H26 H 0.7183 0.2075 0.5749 0.028 Uiso 1 1 calc R . . C27 C 0.7099(10) 0.2774(4) 0.5417(4) 0.026(2) Uani 1 1 d . . . H27 H 0.7088 0.2915 0.5732 0.031 Uiso 1 1 calc R . . C28 C 0.8990(9) 0.2537(4) 0.5127(4) 0.027(2) Uani 1 1 d . . . C29 C 0.5285(10) 0.3337(4) 0.5083(4) 0.027(2) Uani 1 1 d . . . H29A H 0.5409 0.3515 0.5379 0.032 Uiso 1 1 calc R . . H29B H 0.4351 0.3291 0.5006 0.032 Uiso 1 1 calc R . . C30 C 0.8709(10) 0.3427(4) 0.5197(4) 0.030(2) Uani 1 1 d . . . H30A H 0.9653 0.3425 0.5191 0.036 Uiso 1 1 calc R . . H30B H 0.8514 0.3591 0.5484 0.036 Uiso 1 1 calc R . . C31 C 0.5160(10) 0.3698(4) 0.4288(4) 0.027(2) Uani 1 1 d . . . C32 C 0.6904(9) 0.3951(4) 0.4800(4) 0.026(2) Uani 1 1 d . . . H32 H 0.6852 0.4164 0.5076 0.031 Uiso 1 1 calc R . . C33 C 0.6884(10) 0.4262(4) 0.4348(4) 0.028(2) Uani 1 1 d . . . H33 H 0.6721 0.4617 0.4404 0.033 Uiso 1 1 calc R . . C34 C 0.8895(10) 0.3857(4) 0.4466(4) 0.032(2) Uani 1 1 d . . . C35 C 0.5288(10) 0.4235(4) 0.3617(4) 0.031(2) Uani 1 1 d . . . H35A H 0.5326 0.4597 0.3638 0.037 Uiso 1 1 calc R . . H35B H 0.4373 0.4141 0.3562 0.037 Uiso 1 1 calc R . . C36 C 0.8638(11) 0.4446(4) 0.3805(4) 0.036(3) Uani 1 1 d . . . H36A H 0.8305 0.4786 0.3802 0.043 Uiso 1 1 calc R . . H36B H 0.9585 0.4463 0.3860 0.043 Uiso 1 1 calc R . . N1 N 0.5953(8) 0.4079(3) 0.3221(3) 0.0271(18) Uani 1 1 d . . . N2 N 0.6163(8) 0.3752(3) 0.2531(3) 0.0279(19) Uani 1 1 d . . . N3 N 0.8299(9) 0.4228(4) 0.3355(3) 0.033(2) Uani 1 1 d . . . N4 N 0.8482(8) 0.3790(3) 0.2723(3) 0.0280(19) Uani 1 1 d . . . N5 N 0.6565(8) 0.2977(3) 0.2170(3) 0.0265(18) Uani 1 1 d . . . N6 N 0.6720(8) 0.2160(3) 0.2217(3) 0.0240(18) Uani 1 1 d . . . N7 N 0.8901(8) 0.3039(3) 0.2290(3) 0.0280(19) Uani 1 1 d . . . N8 N 0.9115(8) 0.2225(3) 0.2287(3) 0.0244(18) Uani 1 1 d . . . N9 N 0.6810(8) 0.1377(3) 0.2620(3) 0.032(2) Uani 1 1 d . . . N10 N 0.6833(9) 0.0907(4) 0.3230(4) 0.035(2) Uani 1 1 d . . . N11 N 0.9202(8) 0.1442(3) 0.2698(3) 0.030(2) Uani 1 1 d . . . N12 N 0.9195(8) 0.1045(3) 0.3361(3) 0.0285(19) Uani 1 1 d . . . N13 N 0.6699(8) 0.0865(3) 0.4069(3) 0.032(2) Uani 1 1 d . . . N14 N 0.6479(8) 0.1290(3) 0.4706(3) 0.030(2) Uani 1 1 d . . . N15 N 0.9012(8) 0.1017(3) 0.4196(3) 0.0267(18) Uani 1 1 d . . . N16 N 0.8821(8) 0.1337(3) 0.4887(3) 0.0272(13) Uani 1 1 d . . . N17 N 0.6067(8) 0.2046(3) 0.5134(3) 0.0261(18) Uani 1 1 d . . . N18 N 0.5890(8) 0.2859(3) 0.5138(3) 0.030(2) Uani 1 1 d . . . N19 N 0.8431(8) 0.2110(3) 0.5249(3) 0.0280(19) Uani 1 1 d . . . N20 N 0.8253(8) 0.2925(3) 0.5201(3) 0.0272(13) Uani 1 1 d . . . N21 N 0.5803(8) 0.3643(3) 0.4718(3) 0.0283(19) Uani 1 1 d . . . N22 N 0.5806(8) 0.4031(3) 0.4051(3) 0.031(2) Uani 1 1 d . . . N23 N 0.8135(8) 0.3707(3) 0.4807(3) 0.0294(19) Uani 1 1 d . . . N24 N 0.8145(8) 0.4182(3) 0.4184(3) 0.032(2) Uani 1 1 d . . . O1 O 0.4477(7) 0.3491(3) 0.2949(3) 0.0348(13) Uani 1 1 d . . . O2 O 0.4906(7) 0.2529(3) 0.2447(3) 0.0316(17) Uani 1 1 d . . . O3 O 0.4964(8) 0.1333(3) 0.2990(3) 0.043(2) Uani 1 1 d . . . O4 O 0.4824(8) 0.1295(4) 0.4117(3) 0.054(3) Uani 1 1 d . . . O5 O 0.4205(7) 0.2398(3) 0.4771(3) 0.0348(13) Uani 1 1 d . . . O6 O 0.4154(7) 0.3486(3) 0.4141(3) 0.0371(18) Uani 1 1 d . . . O7 O 1.0162(9) 0.3788(4) 0.3314(4) 0.061(3) Uani 1 1 d . . . O8 O 1.0739(7) 0.2689(3) 0.2661(3) 0.0314(17) Uani 1 1 d . . . O9 O 1.0832(7) 0.1594(3) 0.3291(3) 0.0368(19) Uani 1 1 d . . . O10 O 1.0471(7) 0.1614(3) 0.4464(3) 0.0383(19) Uani 1 1 d . . . O11 O 1.0059(7) 0.2555(3) 0.4978(3) 0.0347(17) Uani 1 1 d . . . O12 O 1.0001(8) 0.3757(3) 0.4421(3) 0.044(2) 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 Cl9 0.0342(18) 0.134(4) 0.0374(18) 0.007(2) 0.0013(14) -0.014(2) Cl10 0.038(2) 0.169(5) 0.0365(19) 0.007(2) -0.0004(15) -0.015(3) Cl1 0.078(3) 0.0516(19) 0.051(2) 0.0053(15) 0.0212(19) 0.0098(17) Cl2 0.165(7) 0.118(5) 0.136(6) -0.032(4) -0.039(5) 0.074(5) Cl3 0.090(4) 0.081(4) 0.295(12) -0.037(5) 0.030(6) -0.019(3) Cl4 0.206(9) 0.153(7) 0.246(10) 0.122(7) 0.164(8) 0.116(7) Cl5 0.132(5) 0.080(3) 0.061(3) 0.009(2) 0.044(3) 0.033(3) Cl6 0.223(9) 0.124(5) 0.141(6) 0.060(5) 0.121(6) 0.102(6) Cl7 0.304(14) 0.300(14) 0.115(6) -0.069(7) -0.038(7) 0.243(13) Cl8 0.129(7) 0.144(8) 0.61(3) -0.119(13) 0.186(12) -0.055(6) Zn1 0.0822(15) 0.0596(11) 0.0896(15) -0.0011(10) 0.0186(12) 0.0088(10) Zn2 0.0974(17) 0.0653(13) 0.0918(16) 0.0002(11) 0.0286(13) 0.0167(12) O1W 0.032(4) 0.053(5) 0.036(4) 0.017(4) 0.000(3) -0.006(4) O2W 0.019(4) 0.033(4) 0.055(5) -0.001(4) 0.009(3) -0.001(3) O3W 0.039(5) 0.065(6) 0.049(5) 0.017(5) -0.005(4) -0.004(4) O4W 0.030(4) 0.067(6) 0.027(4) -0.006(4) -0.004(3) 0.005(4) O5W 0.027(4) 0.088(7) 0.028(4) -0.010(4) 0.000(3) 0.009(4) O6W 0.034(5) 0.059(5) 0.043(5) -0.013(4) -0.004(4) 0.006(4) O7W 0.032(4) 0.056(5) 0.041(5) 0.016(4) -0.005(4) -0.003(4) O8W 0.034(5) 0.066(6) 0.049(5) 0.015(5) -0.008(4) -0.006(4) O9W 0.021(4) 0.042(4) 0.051(5) 0.000(4) 0.014(3) 0.005(3) O10W 0.025(4) 0.079(6) 0.031(4) -0.011(4) 0.001(3) 0.008(4) Tb1 0.0111(3) 0.0427(3) 0.0269(3) 0.0012(2) 0.00239(18) -0.00141(19) Tb2 0.0112(3) 0.0412(3) 0.0264(3) 0.0011(2) 0.00216(18) -0.00179(18) C1 0.009(3) 0.039(4) 0.037(4) 0.010(3) 0.005(3) 0.007(3) C2 0.020(5) 0.030(5) 0.042(6) -0.003(5) 0.001(4) 0.007(4) C3 0.020(5) 0.024(5) 0.047(7) 0.006(4) 0.009(5) -0.004(4) C4 0.020(5) 0.030(5) 0.054(7) -0.004(5) 0.008(5) 0.003(4) C5 0.010(3) 0.037(3) 0.039(3) -0.001(3) 0.010(2) -0.003(2) C6 0.010(3) 0.037(3) 0.039(3) -0.001(3) 0.010(2) -0.003(2) C7 0.016(5) 0.035(5) 0.031(5) 0.000(4) -0.007(4) 0.002(4) C8 0.016(5) 0.032(5) 0.033(6) 0.004(4) -0.004(4) 0.002(4) C9 0.009(4) 0.035(5) 0.027(5) 0.003(4) 0.002(4) -0.001(4) C10 0.015(5) 0.037(5) 0.026(5) -0.001(4) 0.000(4) -0.002(4) C11 0.018(5) 0.036(6) 0.041(6) 0.005(5) 0.001(4) -0.002(4) C12 0.010(3) 0.037(3) 0.039(3) -0.001(3) 0.010(2) -0.003(2) C13 0.027(6) 0.026(5) 0.051(7) 0.001(5) -0.007(5) -0.007(4) C14 0.009(4) 0.027(5) 0.043(6) -0.008(4) 0.000(4) 0.001(4) C15 0.017(5) 0.033(5) 0.042(6) -0.011(5) 0.009(4) -0.006(4) C16 0.017(5) 0.033(5) 0.033(6) -0.006(4) 0.007(4) 0.004(4) C17 0.024(6) 0.036(6) 0.041(6) 0.006(5) 0.003(5) -0.010(4) C18 0.013(5) 0.036(5) 0.043(6) -0.005(5) 0.000(4) 0.010(4) C19 0.019(5) 0.034(6) 0.052(7) -0.003(5) 0.007(5) -0.004(4) C20 0.016(5) 0.033(5) 0.041(6) 0.005(5) -0.002(4) 0.004(4) C21 0.020(5) 0.033(5) 0.031(6) 0.002(4) 0.000(4) 0.009(4) C22 0.009(3) 0.039(4) 0.037(4) 0.010(3) 0.005(3) 0.007(3) C23 0.021(5) 0.029(5) 0.041(6) -0.003(4) 0.013(4) 0.002(4) C24 0.024(5) 0.037(6) 0.030(6) 0.003(4) -0.005(4) 0.009(4) C25 0.015(5) 0.039(6) 0.028(5) 0.008(4) 0.006(4) -0.009(4) C26 0.009(4) 0.038(5) 0.025(5) -0.002(4) 0.010(4) 0.001(4) C27 0.018(5) 0.029(5) 0.030(6) -0.009(4) -0.003(4) 0.003(4) C28 0.006(4) 0.044(6) 0.030(5) -0.001(5) 0.003(4) -0.003(4) C29 0.021(5) 0.037(5) 0.024(5) -0.002(4) 0.006(4) 0.007(4) C30 0.017(5) 0.039(6) 0.034(6) 0.001(5) 0.000(4) -0.002(4) C31 0.018(5) 0.032(5) 0.033(6) -0.004(4) 0.006(4) 0.006(4) C32 0.014(5) 0.032(5) 0.031(5) -0.009(4) 0.003(4) -0.002(4) C33 0.016(5) 0.026(5) 0.042(6) -0.008(4) 0.006(4) 0.004(4) C34 0.020(5) 0.036(6) 0.040(6) -0.004(5) -0.001(5) 0.003(4) C35 0.015(5) 0.033(5) 0.045(7) -0.002(5) 0.012(4) 0.008(4) C36 0.022(5) 0.034(6) 0.053(7) 0.000(5) 0.005(5) -0.014(4) N1 0.017(4) 0.034(5) 0.031(5) -0.001(4) 0.005(3) 0.002(3) N2 0.012(4) 0.038(5) 0.035(5) 0.002(4) 0.007(3) -0.002(3) N3 0.020(5) 0.039(5) 0.042(6) -0.010(4) 0.009(4) 0.002(4) N4 0.007(4) 0.034(5) 0.044(5) -0.006(4) 0.006(3) 0.001(3) N5 0.011(4) 0.038(5) 0.031(5) 0.006(4) 0.003(3) -0.002(3) N6 0.009(4) 0.033(4) 0.030(5) -0.002(4) 0.005(3) 0.003(3) N7 0.009(4) 0.026(4) 0.050(6) 0.004(4) 0.009(4) 0.001(3) N8 0.017(4) 0.031(4) 0.025(4) -0.006(3) -0.002(3) 0.004(3) N9 0.015(4) 0.038(5) 0.043(5) 0.008(4) 0.001(4) 0.001(4) N10 0.019(5) 0.037(5) 0.049(6) 0.010(4) 0.004(4) 0.004(4) N11 0.018(4) 0.035(5) 0.036(5) 0.003(4) -0.004(4) -0.009(4) N12 0.022(4) 0.033(5) 0.031(5) 0.003(4) 0.005(4) -0.005(4) N13 0.017(4) 0.030(4) 0.047(6) -0.005(4) -0.003(4) 0.001(3) N14 0.020(4) 0.033(5) 0.038(5) -0.002(4) 0.004(4) -0.002(4) N15 0.016(4) 0.035(5) 0.030(5) -0.003(4) 0.008(3) -0.003(3) N16 0.010(3) 0.037(3) 0.035(3) 0.004(3) 0.005(2) -0.002(2) N17 0.013(4) 0.033(4) 0.034(5) -0.005(4) 0.007(3) -0.005(3) N18 0.008(4) 0.038(5) 0.043(5) 0.004(4) -0.001(4) -0.002(3) N19 0.015(4) 0.033(5) 0.037(5) -0.002(4) 0.005(4) 0.002(3) N20 0.010(3) 0.037(3) 0.035(3) 0.004(3) 0.005(2) -0.002(2) N21 0.021(4) 0.033(4) 0.032(5) -0.006(4) 0.008(4) -0.008(4) N22 0.020(4) 0.036(5) 0.035(5) -0.009(4) 0.003(4) -0.007(4) N23 0.012(4) 0.039(5) 0.037(5) 0.002(4) 0.002(3) -0.005(3) N24 0.018(4) 0.039(5) 0.043(6) 0.005(4) 0.020(4) 0.000(4) O1 0.012(2) 0.044(3) 0.048(3) 0.000(3) 0.004(2) -0.010(2) O2 0.014(4) 0.044(4) 0.038(4) 0.005(3) 0.011(3) 0.001(3) O3 0.021(4) 0.053(5) 0.057(5) 0.008(4) 0.012(4) 0.003(4) O4 0.028(5) 0.071(6) 0.059(6) -0.019(5) -0.013(4) 0.020(4) O5 0.012(2) 0.044(3) 0.048(3) 0.000(3) 0.004(2) -0.010(2) O6 0.023(4) 0.050(5) 0.039(5) 0.001(4) 0.005(3) -0.007(3) O7 0.026(5) 0.081(7) 0.072(7) -0.031(6) -0.007(5) 0.018(5) O8 0.018(4) 0.033(4) 0.041(4) -0.003(3) -0.006(3) 0.004(3) O9 0.023(4) 0.064(5) 0.024(4) -0.006(4) 0.004(3) -0.015(4) O10 0.019(4) 0.057(5) 0.039(4) -0.006(4) 0.002(3) -0.013(4) O11 0.017(4) 0.046(4) 0.041(4) 0.005(4) 0.006(3) 0.006(3) O12 0.026(4) 0.046(5) 0.063(6) 0.009(4) 0.018(4) 0.009(4) _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 Cl1 Zn1 2.232(4) . ? Cl2 Zn1 2.270(7) . ? Cl3 Zn1 2.244(7) . ? Cl4 Zn1 2.259(7) . ? Cl5 Zn2 2.213(5) . ? Cl6 Zn2 2.245(6) . ? Cl7 Zn2 2.235(9) . ? Cl8 Zn2 2.208(9) . ? O1W Tb1 2.390(8) . ? O2W Tb1 2.383(8) . ? O3W Tb1 2.410(9) . ? O4W Tb1 2.358(8) . ? O5W Tb1 2.427(8) . ? O6W Tb2 2.366(9) . ? O7W Tb2 2.367(8) . ? O8W Tb2 2.421(8) . ? O9W Tb2 2.353(8) . ? O10W Tb2 2.418(8) . ? Tb1 O2 2.317(7) . ? Tb1 O8 2.395(7) 1_455 ? Tb1 O1 2.400(7) . ? Tb2 O11 2.318(8) . ? Tb2 O5 2.366(7) 1_655 ? Tb2 O10 2.391(8) . ? C1 O1 1.262(13) . ? C1 N1 1.336(14) . ? C1 N2 1.354(14) . ? C2 N3 1.454(14) . ? C2 N1 1.463(14) . ? C2 C3 1.497(16) . ? C2 H2 0.9900 . ? C3 N4 1.450(13) . ? C3 N2 1.461(13) . ? C3 H3 0.9900 . ? C4 O7 1.229(14) . ? C4 N4 1.350(15) . ? C4 N3 1.364(14) . ? C5 N2 1.433(14) . ? C5 N5 1.455(14) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.451(13) . ? C6 N4 1.452(13) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.228(13) . ? C7 N6 1.348(13) . ? C7 N5 1.362(14) . ? C8 N5 1.414(14) . ? C8 N7 1.453(13) . ? C8 C9 1.537(14) . ? C8 H8 0.9900 . ? C9 N6 1.472(13) . ? C9 N8 1.478(12) . ? C9 H9 0.9900 . ? C10 O8 1.222(12) . ? C10 N8 1.340(13) . ? C10 N7 1.372(13) . ? C11 N6 1.436(14) . ? C11 N9 1.455(14) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.448(14) . ? C12 N8 1.449(13) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.234(14) . ? C13 N9 1.327(16) . ? C13 N10 1.352(14) . ? C14 N9 1.447(12) . ? C14 N11 1.467(12) . ? C14 C15 1.553(16) . ? C14 H14 0.9900 . ? C15 N10 1.436(14) . ? C15 N12 1.446(13) . ? C15 H15 0.9900 . ? C16 O9 1.225(13) . ? C16 N12 1.344(14) . ? C16 N11 1.374(14) . ? C17 N13 1.447(15) . ? C17 N10 1.458(15) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N15 1.444(14) . ? C18 N12 1.450(14) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.203(14) . ? C19 N14 1.359(15) . ? C19 N13 1.369(15) . ? C20 N13 1.416(13) . ? C20 N15 1.466(14) . ? C20 C21 1.551(16) . ? C20 H20 0.9900 . ? C21 N14 1.444(13) . ? C21 N16 1.455(13) . ? C21 H21 0.9900 . ? C22 O10 1.255(13) . ? C22 N15 1.335(14) . ? C22 N16 1.353(13) . ? C23 N17 1.445(13) . ? C23 N14 1.487(14) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N16 1.415(14) . ? C24 N19 1.448(13) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O5 1.240(12) . ? C25 N17 1.345(14) . ? C25 N18 1.372(14) . ? C26 N17 1.446(13) . ? C26 N19 1.448(12) . ? C26 C27 1.544(14) . ? C26 H26 0.9900 . ? C27 N18 1.442(12) . ? C27 N20 1.458(14) . ? C27 H27 0.9900 . ? C28 O11 1.227(13) . ? C28 N20 1.326(14) . ? C28 N19 1.352(14) . ? C29 N18 1.436(13) . ? C29 N21 1.482(14) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N20 1.435(14) . ? C30 N23 1.441(14) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O6 1.229(13) . ? C31 N22 1.349(14) . ? C31 N21 1.362(14) . ? C32 N21 1.413(12) . ? C32 N23 1.434(13) . ? C32 C33 1.552(15) . ? C32 H32 0.9900 . ? C33 N24 1.448(13) . ? C33 N22 1.480(13) . ? C33 H33 0.9900 . ? C34 O12 1.196(14) . ? C34 N23 1.378(15) . ? C34 N24 1.387(14) . ? C35 N22 1.428(14) . ? C35 N1 1.455(13) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N3 1.442(15) . ? C36 N24 1.441(15) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? O5 Tb2 2.366(7) 1_455 ? O8 Tb1 2.395(7) 1_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 Cl1 Zn1 Cl3 108.2(2) . . ? Cl1 Zn1 Cl4 107.9(2) . . ? Cl3 Zn1 Cl4 111.9(4) . . ? Cl1 Zn1 Cl2 111.2(2) . . ? Cl3 Zn1 Cl2 106.3(4) . . ? Cl4 Zn1 Cl2 111.3(4) . . ? Cl8 Zn2 Cl5 110.7(4) . . ? Cl8 Zn2 Cl7 105.6(7) . . ? Cl5 Zn2 Cl7 110.1(3) . . ? Cl8 Zn2 Cl6 110.0(5) . . ? Cl5 Zn2 Cl6 111.0(2) . . ? Cl7 Zn2 Cl6 109.2(4) . . ? O2 Tb1 O4W 144.8(3) . . ? O2 Tb1 O2W 78.8(3) . . ? O4W Tb1 O2W 107.0(3) . . ? O2 Tb1 O1W 104.0(3) . . ? O4W Tb1 O1W 88.9(3) . . ? O2W Tb1 O1W 148.4(3) . . ? O2 Tb1 O8 140.9(3) . 1_455 ? O4W Tb1 O8 72.6(3) . 1_455 ? O2W Tb1 O8 77.4(2) . 1_455 ? O1W Tb1 O8 81.8(3) . 1_455 ? O2 Tb1 O1 79.9(3) . . ? O4W Tb1 O1 74.3(3) . . ? O2W Tb1 O1 140.7(3) . . ? O1W Tb1 O1 69.4(3) . . ? O8 Tb1 O1 136.0(3) 1_455 . ? O2 Tb1 O3W 78.9(3) . . ? O4W Tb1 O3W 70.7(3) . . ? O2W Tb1 O3W 71.6(3) . . ? O1W Tb1 O3W 140.0(3) . . ? O8 Tb1 O3W 121.3(3) 1_455 . ? O1 Tb1 O3W 72.1(3) . . ? O2 Tb1 O5W 69.6(3) . . ? O4W Tb1 O5W 145.3(3) . . ? O2W Tb1 O5W 79.6(3) . . ? O1W Tb1 O5W 72.4(3) . . ? O8 Tb1 O5W 75.9(3) 1_455 . ? O1 Tb1 O5W 122.4(3) . . ? O3W Tb1 O5W 140.7(4) . . ? O11 Tb2 O9W 80.1(3) . . ? O11 Tb2 O5 140.7(3) . 1_655 ? O9W Tb2 O5 76.9(3) . 1_655 ? O11 Tb2 O6W 145.0(3) . . ? O9W Tb2 O6W 106.6(3) . . ? O5 Tb2 O6W 72.9(3) 1_655 . ? O11 Tb2 O7W 104.4(3) . . ? O9W Tb2 O7W 149.3(3) . . ? O5 Tb2 O7W 81.5(3) 1_655 . ? O6W Tb2 O7W 87.3(3) . . ? O11 Tb2 O10 78.9(3) . . ? O9W Tb2 O10 140.3(3) . . ? O5 Tb2 O10 136.9(3) 1_655 . ? O6W Tb2 O10 74.6(3) . . ? O7W Tb2 O10 69.2(3) . . ? O11 Tb2 O10W 70.3(3) . . ? O9W Tb2 O10W 79.9(3) . . ? O5 Tb2 O10W 74.6(3) 1_655 . ? O6W Tb2 O10W 144.3(3) . . ? O7W Tb2 O10W 73.5(3) . . ? O10 Tb2 O10W 122.9(3) . . ? O11 Tb2 O8W 80.0(3) . . ? O9W Tb2 O8W 72.2(3) . . ? O5 Tb2 O8W 121.4(3) 1_655 . ? O6W Tb2 O8W 70.2(3) . . ? O7W Tb2 O8W 138.4(3) . . ? O10 Tb2 O8W 71.3(3) . . ? O10W Tb2 O8W 142.1(3) . . ? O1 C1 N1 123.7(10) . . ? O1 C1 N2 125.6(10) . . ? N1 C1 N2 110.6(9) . . ? N3 C2 N1 114.7(9) . . ? N3 C2 C3 103.7(8) . . ? N1 C2 C3 104.2(8) . . ? N3 C2 H2 111.2 . . ? N1 C2 H2 111.2 . . ? C3 C2 H2 111.2 . . ? N4 C3 N2 112.1(8) . . ? N4 C3 C2 103.9(9) . . ? N2 C3 C2 103.9(9) . . ? N4 C3 H3 112.1 . . ? N2 C3 H3 112.1 . . ? C2 C3 H3 112.1 . . ? O7 C4 N4 128.3(11) . . ? O7 C4 N3 122.9(11) . . ? N4 C4 N3 108.4(9) . . ? N2 C5 N5 112.0(9) . . ? N2 C5 H5A 109.2 . . ? N5 C5 H5A 109.2 . . ? N2 C5 H5B 109.2 . . ? N5 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? N7 C6 N4 114.6(8) . . ? N7 C6 H6A 108.6 . . ? N4 C6 H6A 108.6 . . ? N7 C6 H6B 108.6 . . ? N4 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? O2 C7 N6 124.6(10) . . ? O2 C7 N5 125.8(10) . . ? N6 C7 N5 109.6(9) . . ? N5 C8 N7 114.9(9) . . ? N5 C8 C9 104.0(8) . . ? N7 C8 C9 102.9(8) . . ? N5 C8 H8 111.5 . . ? N7 C8 H8 111.5 . . ? C9 C8 H8 111.5 . . ? N6 C9 N8 114.0(8) . . ? N6 C9 C8 103.0(8) . . ? N8 C9 C8 103.6(8) . . ? N6 C9 H9 111.9 . . ? N8 C9 H9 111.9 . . ? C8 C9 H9 111.9 . . ? O8 C10 N8 126.2(10) . . ? O8 C10 N7 124.6(10) . . ? N8 C10 N7 109.1(8) . . ? N6 C11 N9 113.3(9) . . ? N6 C11 H11A 108.9 . . ? N9 C11 H11A 108.9 . . ? N6 C11 H11B 108.9 . . ? N9 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? N11 C12 N8 113.6(9) . . ? N11 C12 H12A 108.8 . . ? N8 C12 H12A 108.8 . . ? N11 C12 H12B 108.8 . . ? N8 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N9 125.9(11) . . ? O3 C13 N10 125.8(12) . . ? N9 C13 N10 108.3(10) . . ? N9 C14 N11 116.1(8) . . ? N9 C14 C15 102.1(9) . . ? N11 C14 C15 102.2(8) . . ? N9 C14 H14 111.9 . . ? N11 C14 H14 111.9 . . ? C15 C14 H14 111.9 . . ? N10 C15 N12 117.7(9) . . ? N10 C15 C14 102.3(9) . . ? N12 C15 C14 103.3(8) . . ? N10 C15 H15 110.9 . . ? N12 C15 H15 110.9 . . ? C14 C15 H15 110.9 . . ? O9 C16 N12 124.8(10) . . ? O9 C16 N11 127.0(10) . . ? N12 C16 N11 108.1(9) . . ? N13 C17 N10 114.9(9) . . ? N13 C17 H17A 108.5 . . ? N10 C17 H17A 108.5 . . ? N13 C17 H17B 108.5 . . ? N10 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? N15 C18 N12 115.2(8) . . ? N15 C18 H18A 108.5 . . ? N12 C18 H18A 108.5 . . ? N15 C18 H18B 108.5 . . ? N12 C18 H18B 108.5 . . ? H18A C18 H18B 107.5 . . ? O4 C19 N14 127.6(11) . . ? O4 C19 N13 124.6(11) . . ? N14 C19 N13 107.8(9) . . ? N13 C20 N15 114.5(9) . . ? N13 C20 C21 103.6(8) . . ? N15 C20 C21 102.9(8) . . ? N13 C20 H20 111.8 . . ? N15 C20 H20 111.8 . . ? C21 C20 H20 111.8 . . ? N14 C21 N16 114.2(9) . . ? N14 C21 C20 102.5(8) . . ? N16 C21 C20 102.6(9) . . ? N14 C21 H21 112.2 . . ? N16 C21 H21 112.2 . . ? C20 C21 H21 112.2 . . ? O10 C22 N15 124.6(10) . . ? O10 C22 N16 125.3(10) . . ? N15 C22 N16 110.0(9) . . ? N17 C23 N14 112.9(9) . . ? N17 C23 H23A 109.0 . . ? N14 C23 H23A 109.0 . . ? N17 C23 H23B 109.0 . . ? N14 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? N16 C24 N19 113.0(8) . . ? N16 C24 H24A 109.0 . . ? N19 C24 H24A 109.0 . . ? N16 C24 H24B 109.0 . . ? N19 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? O5 C25 N17 126.7(10) . . ? O5 C25 N18 125.0(10) . . ? N17 C25 N18 108.4(8) . . ? N17 C26 N19 115.4(8) . . ? N17 C26 C27 103.5(8) . . ? N19 C26 C27 103.0(8) . . ? N17 C26 H26 111.5 . . ? N19 C26 H26 111.5 . . ? C27 C26 H26 111.5 . . ? N18 C27 N20 114.8(9) . . ? N18 C27 C26 102.9(8) . . ? N20 C27 C26 103.5(8) . . ? N18 C27 H27 111.7 . . ? N20 C27 H27 111.7 . . ? C26 C27 H27 111.7 . . ? O11 C28 N20 125.4(10) . . ? O11 C28 N19 123.3(10) . . ? N20 C28 N19 111.3(9) . . ? N18 C29 N21 113.3(8) . . ? N18 C29 H29A 108.9 . . ? N21 C29 H29A 108.9 . . ? N18 C29 H29B 108.9 . . ? N21 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? N20 C30 N23 113.1(8) . . ? N20 C30 H30A 109.0 . . ? N23 C30 H30A 109.0 . . ? N20 C30 H30B 109.0 . . ? N23 C30 H30B 109.0 . . ? H30A C30 H30B 107.8 . . ? O6 C31 N22 125.4(10) . . ? O6 C31 N21 126.3(10) . . ? N22 C31 N21 108.3(9) . . ? N21 C32 N23 115.6(9) . . ? N21 C32 C33 103.4(8) . . ? N23 C32 C33 101.6(8) . . ? N21 C32 H32 111.8 . . ? N23 C32 H32 111.8 . . ? C33 C32 H32 111.8 . . ? N24 C33 N22 113.6(9) . . ? N24 C33 C32 104.8(8) . . ? N22 C33 C32 102.2(8) . . ? N24 C33 H33 111.9 . . ? N22 C33 H33 111.9 . . ? C32 C33 H33 111.9 . . ? O12 C34 N23 129.1(11) . . ? O12 C34 N24 124.5(11) . . ? N23 C34 N24 106.4(9) . . ? N22 C35 N1 114.5(8) . . ? N22 C35 H35A 108.6 . . ? N1 C35 H35A 108.6 . . ? N22 C35 H35B 108.6 . . ? N1 C35 H35B 108.6 . . ? H35A C35 H35B 107.6 . . ? N3 C36 N24 114.3(9) . . ? N3 C36 H36A 108.7 . . ? N24 C36 H36A 108.7 . . ? N3 C36 H36B 108.7 . . ? N24 C36 H36B 108.7 . . ? H36A C36 H36B 107.6 . . ? C1 N1 C35 123.8(9) . . ? C1 N1 C2 110.6(9) . . ? C35 N1 C2 124.7(9) . . ? C1 N2 C5 124.5(9) . . ? C1 N2 C3 110.1(9) . . ? C5 N2 C3 125.1(9) . . ? C4 N3 C36 124.1(10) . . ? C4 N3 C2 111.3(9) . . ? C36 N3 C2 124.6(9) . . ? C4 N4 C3 111.7(9) . . ? C4 N4 C6 120.0(8) . . ? C3 N4 C6 124.8(9) . . ? C7 N5 C8 112.5(9) . . ? C7 N5 C5 121.9(8) . . ? C8 N5 C5 124.2(8) . . ? C7 N6 C11 122.3(9) . . ? C7 N6 C9 110.7(8) . . ? C11 N6 C9 124.8(9) . . ? C10 N7 C6 124.6(9) . . ? C10 N7 C8 112.5(8) . . ? C6 N7 C8 122.6(8) . . ? C10 N8 C12 126.0(8) . . ? C10 N8 C9 111.7(8) . . ? C12 N8 C9 121.7(8) . . ? C13 N9 C14 113.3(9) . . ? C13 N9 C11 121.7(9) . . ? C14 N9 C11 122.8(9) . . ? C13 N10 C15 113.2(10) . . ? C13 N10 C17 123.4(10) . . ? C15 N10 C17 123.3(9) . . ? C16 N11 C12 124.3(8) . . ? C16 N11 C14 112.5(9) . . ? C12 N11 C14 122.9(9) . . ? C16 N12 C15 113.7(9) . . ? C16 N12 C18 123.1(9) . . ? C15 N12 C18 122.5(9) . . ? C19 N13 C20 113.0(10) . . ? C19 N13 C17 122.7(9) . . ? C20 N13 C17 124.2(9) . . ? C19 N14 C21 112.4(9) . . ? C19 N14 C23 120.1(9) . . ? C21 N14 C23 124.4(9) . . ? C22 N15 C18 123.7(9) . . ? C22 N15 C20 111.9(9) . . ? C18 N15 C20 122.9(9) . . ? C22 N16 C24 124.4(9) . . ? C22 N16 C21 111.9(9) . . ? C24 N16 C21 123.4(9) . . ? C25 N17 C23 124.0(9) . . ? C25 N17 C26 112.6(8) . . ? C23 N17 C26 122.9(9) . . ? C25 N18 C29 123.4(8) . . ? C25 N18 C27 112.4(9) . . ? C29 N18 C27 123.5(9) . . ? C28 N19 C26 111.1(8) . . ? C28 N19 C24 123.8(9) . . ? C26 N19 C24 124.0(9) . . ? C28 N20 C30 123.3(9) . . ? C28 N20 C27 110.9(8) . . ? C30 N20 C27 123.4(9) . . ? C31 N21 C32 114.0(9) . . ? C31 N21 C29 122.2(9) . . ? C32 N21 C29 123.4(9) . . ? C31 N22 C35 122.8(9) . . ? C31 N22 C33 111.6(9) . . ? C35 N22 C33 123.2(9) . . ? C34 N23 C32 115.0(9) . . ? C34 N23 C30 119.6(9) . . ? C32 N23 C30 123.5(9) . . ? C34 N24 C36 122.9(9) . . ? C34 N24 C33 111.9(9) . . ? C36 N24 C33 124.8(9) . . ? C1 O1 Tb1 153.0(8) . . ? C7 O2 Tb1 157.4(8) . . ? C25 O5 Tb2 155.3(7) . 1_455 ? C10 O8 Tb1 153.8(8) . 1_655 ? C22 O10 Tb2 154.0(8) . . ? C28 O11 Tb2 158.8(8) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.206 _refine_diff_density_min -2.420 _refine_diff_density_rms 0.256 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.005 0.000 -0.005 997 584 ' ' 2 0.748 0.246 0.871 87 47 ' ' 3 0.748 0.254 0.371 87 46 ' ' 4 0.617 0.500 0.117 997 585 ' ' 5 0.252 0.746 0.629 87 45 ' ' 6 0.252 0.754 0.129 87 45 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 902619' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p310 #TrackingRef 'submit-310-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H72 Cl6 Dy2 N24 O30' _chemical_formula_weight 1858.88 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 '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 12.166(4) _cell_length_b 19.686(6) _cell_length_c 14.752(5) _cell_angle_alpha 90.00 _cell_angle_beta 112.805(9) _cell_angle_gamma 90.00 _cell_volume 3256.9(17) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.895 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1860 _exptl_absorpt_coefficient_mu 2.627 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5267 _exptl_absorpt_correction_T_max 0.6085 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28018 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5720 _reflns_number_gt 5165 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0419P)^2^+3.2335P] 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 5720 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_ref 0.0729 _refine_ls_wR_factor_gt 0.0713 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Cl1 Cl 0.02967(10) -0.25507(5) 0.06965(7) 0.0464(2) Uani 1 1 d . . . Cl2 Cl 0.63305(11) -0.11620(5) -0.44920(8) 0.0530(3) Uani 1 1 d . . . Cl3 Cl 0.18706(11) -0.10011(6) -0.61047(8) 0.0582(3) Uani 1 1 d . . . O1W O 0.3756(2) 0.24389(12) -0.1616(2) 0.0419(6) Uani 1 1 d . . . O2W O 0.0534(2) 0.14977(14) -0.39563(18) 0.0412(6) Uani 1 1 d . . . O3W O 0.0082(3) 0.17722(15) -0.2293(2) 0.0551(9) Uani 1 1 d . . . O4W O 0.2649(3) 0.15385(15) -0.0706(2) 0.0486(7) Uani 1 1 d . . . O5W O 0.1534(3) 0.28683(14) -0.1721(2) 0.0488(7) Uani 1 1 d . . . O6W O 0.2016(3) 0.26405(16) -0.3541(2) 0.0577(8) Uani 1 1 d . . . Dy1 Dy 0.198763(14) 0.181104(7) -0.236883(11) 0.02548(7) Uani 1 1 d . . . C1 C 0.3943(3) 0.08160(16) -0.3050(2) 0.0258(7) Uani 1 1 d . . . C2 C 0.5398(3) 0.01692(16) -0.3302(2) 0.0279(7) Uani 1 1 d . . . H2 H 0.5722 0.0271 -0.3808 0.033 Uiso 1 1 calc R . . C3 C 0.4197(3) -0.02105(16) -0.3737(2) 0.0274(7) Uani 1 1 d . . . H3 H 0.3955 -0.0303 -0.4448 0.033 Uiso 1 1 calc R . . C4 C 0.5585(3) -0.08843(18) -0.2534(3) 0.0324(8) Uani 1 1 d . . . C5 C 0.2134(3) 0.01288(17) -0.3859(2) 0.0288(7) Uani 1 1 d . . . H5A H 0.1856 -0.0117 -0.4486 0.035 Uiso 1 1 calc R . . H5B H 0.1717 0.0566 -0.3974 0.035 Uiso 1 1 calc R . . C6 C 0.3596(3) -0.13971(17) -0.3366(3) 0.0331(8) Uani 1 1 d . . . H6A H 0.3103 -0.1405 -0.4072 0.040 Uiso 1 1 calc R . . H6B H 0.4045 -0.1824 -0.3199 0.040 Uiso 1 1 calc R . . C7 C 0.1555(3) 0.00294(16) -0.2438(2) 0.0247(7) Uani 1 1 d . . . C8 C 0.1701(3) -0.09899(16) -0.3184(3) 0.0291(7) Uani 1 1 d . . . H8 H 0.1151 -0.1156 -0.3836 0.035 Uiso 1 1 calc R . . C9 C 0.1215(3) -0.11319(16) -0.2376(3) 0.0284(7) Uani 1 1 d . . . H9 H 0.0393 -0.1316 -0.2657 0.034 Uiso 1 1 calc R . . C10 C 0.2968(3) -0.17514(16) -0.2028(3) 0.0295(8) Uani 1 1 d . . . C11 C 0.0582(3) -0.03111(17) -0.1341(3) 0.0289(7) Uani 1 1 d . . . H11A H 0.0323 0.0164 -0.1448 0.035 Uiso 1 1 calc R . . H11B H -0.0135 -0.0596 -0.1561 0.035 Uiso 1 1 calc R . . C12 C 0.1896(3) -0.19457(17) -0.0923(3) 0.0329(8) Uani 1 1 d . . . H12A H 0.2384 -0.2358 -0.0756 0.039 Uiso 1 1 calc R . . H12B H 0.1061 -0.2083 -0.1123 0.039 Uiso 1 1 calc R . . C13 C 0.1611(3) 0.01036(17) 0.0350(3) 0.0290(8) Uani 1 1 d . . . C14 C 0.1405(3) -0.10792(16) 0.0165(3) 0.0288(7) Uani 1 1 d . . . H14 H 0.0635 -0.1308 0.0040 0.035 Uiso 1 1 calc R . . C15 C 0.2070(3) -0.09028(17) 0.1269(3) 0.0298(8) Uani 1 1 d . . . H15 H 0.1640 -0.1079 0.1668 0.036 Uiso 1 1 calc R . . C16 C 0.3234(3) -0.16291(17) 0.0755(3) 0.0291(7) Uani 1 1 d . . . C17 C 0.2572(3) 0.02421(18) 0.2156(3) 0.0329(8) Uani 1 1 d . . . H17A H 0.2233 0.0700 0.2005 0.039 Uiso 1 1 calc R . . H17B H 0.2316 0.0046 0.2653 0.039 Uiso 1 1 calc R . . C18 C 0.5942(3) 0.13406(17) -0.2514(3) 0.0307(8) Uani 1 1 d . . . H18A H 0.5494 0.1759 -0.2540 0.037 Uiso 1 1 calc R . . H18B H 0.6382 0.1403 -0.2941 0.037 Uiso 1 1 calc R . . N1 N 0.5108(3) 0.07870(13) -0.2892(2) 0.0278(6) Uani 1 1 d . . . N2 N 0.3385(3) 0.02517(14) -0.3548(2) 0.0284(6) Uani 1 1 d . . . N3 N 0.6156(2) -0.02933(14) -0.2560(2) 0.0293(6) Uani 1 1 d . . . N4 N 0.4432(3) -0.08345(14) -0.3161(2) 0.0324(7) Uani 1 1 d . . . N5 N 0.1823(3) -0.02548(13) -0.3165(2) 0.0273(6) Uani 1 1 d . . . N6 N 0.1252(2) -0.04623(13) -0.1934(2) 0.0261(6) Uani 1 1 d . . . N7 N 0.2828(3) -0.13584(15) -0.2829(2) 0.0325(7) Uani 1 1 d . . . N8 N 0.2042(3) -0.16177(14) -0.1744(2) 0.0294(6) Uani 1 1 d . . . N9 N 0.1233(3) -0.04176(14) -0.0308(2) 0.0304(6) Uani 1 1 d . . . N10 N 0.2099(3) -0.01686(14) 0.1272(2) 0.0312(6) Uani 1 1 d . . . N11 N 0.2225(3) -0.15209(14) -0.0051(2) 0.0301(6) Uani 1 1 d . . . N12 N 0.3212(3) -0.12388(14) 0.1516(2) 0.0315(7) Uani 1 1 d . . . O1 O 0.3449(2) 0.12860(12) -0.27958(18) 0.0328(5) Uani 1 1 d . . . O2 O 0.1574(2) 0.06415(11) -0.22601(18) 0.0326(5) Uani 1 1 d . . . O3 O 0.1486(2) 0.07078(12) 0.01576(19) 0.0370(6) Uani 1 1 d . . . O4 O 0.6040(2) -0.13818(13) -0.2036(2) 0.0469(7) Uani 1 1 d . . . O5 O 0.3760(2) -0.21641(13) -0.1650(2) 0.0433(7) Uani 1 1 d . . . O6 O 0.4019(2) -0.20290(14) 0.0789(2) 0.0446(7) 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 Cl1 0.0708(7) 0.0318(5) 0.0439(6) -0.0071(4) 0.0301(5) -0.0020(4) Cl2 0.0747(8) 0.0376(5) 0.0484(6) 0.0032(5) 0.0258(6) 0.0104(5) Cl3 0.0563(7) 0.0688(7) 0.0480(6) -0.0135(6) 0.0185(5) -0.0261(6) O1W 0.0326(14) 0.0290(13) 0.0634(18) -0.0061(13) 0.0178(14) -0.0016(11) O2W 0.0428(16) 0.0471(16) 0.0298(13) 0.0059(12) 0.0098(12) 0.0049(13) O3W 0.0362(16) 0.066(2) 0.068(2) -0.0358(16) 0.0258(16) -0.0116(13) O4W 0.0622(19) 0.0413(16) 0.0359(15) -0.0013(13) 0.0122(14) -0.0161(14) O5W 0.0466(17) 0.0328(15) 0.070(2) -0.0109(14) 0.0260(16) 0.0023(12) O6W 0.0566(19) 0.0528(18) 0.0591(19) 0.0206(15) 0.0173(16) -0.0109(15) Dy1 0.02656(11) 0.01970(10) 0.03038(11) 0.00067(6) 0.01126(8) 0.00171(6) C1 0.0331(19) 0.0235(17) 0.0225(16) 0.0044(13) 0.0128(15) 0.0046(14) C2 0.0347(19) 0.0265(17) 0.0278(18) 0.0014(14) 0.0180(16) 0.0039(14) C3 0.0345(19) 0.0254(17) 0.0256(17) -0.0018(14) 0.0152(15) 0.0036(14) C4 0.037(2) 0.0296(19) 0.0346(19) 0.0018(16) 0.0178(17) 0.0075(15) C5 0.0324(19) 0.0273(17) 0.0225(17) 0.0005(14) 0.0059(15) 0.0056(14) C6 0.035(2) 0.0233(17) 0.044(2) -0.0072(15) 0.0179(17) 0.0014(14) C7 0.0195(16) 0.0237(17) 0.0271(17) 0.0001(14) 0.0049(14) -0.0005(13) C8 0.0255(18) 0.0231(16) 0.0334(19) -0.0041(15) 0.0057(15) -0.0022(13) C9 0.0236(17) 0.0231(16) 0.0359(19) -0.0024(14) 0.0087(15) -0.0032(13) C10 0.0269(19) 0.0219(17) 0.036(2) -0.0042(15) 0.0084(16) 0.0011(14) C11 0.0219(17) 0.0285(18) 0.0361(19) 0.0037(15) 0.0109(15) 0.0042(13) C12 0.037(2) 0.0198(16) 0.040(2) -0.0009(15) 0.0130(18) -0.0032(14) C13 0.0238(17) 0.0289(19) 0.040(2) 0.0016(16) 0.0190(16) 0.0009(14) C14 0.0235(17) 0.0237(16) 0.040(2) 0.0044(15) 0.0138(16) -0.0002(13) C15 0.0264(18) 0.0279(18) 0.039(2) 0.0045(15) 0.0171(16) -0.0003(14) C16 0.0270(19) 0.0213(16) 0.037(2) 0.0000(15) 0.0100(16) 0.0007(14) C17 0.0307(19) 0.0324(19) 0.041(2) -0.0030(16) 0.0205(17) 0.0057(15) C18 0.036(2) 0.0225(16) 0.0339(19) 0.0074(15) 0.0140(17) 0.0012(14) N1 0.0317(16) 0.0229(14) 0.0290(15) 0.0010(12) 0.0118(13) 0.0035(12) N2 0.0314(16) 0.0235(14) 0.0318(16) -0.0008(12) 0.0139(13) 0.0041(12) N3 0.0281(15) 0.0248(14) 0.0367(17) 0.0020(12) 0.0144(14) 0.0035(12) N4 0.0332(17) 0.0241(15) 0.0386(17) 0.0031(13) 0.0125(14) 0.0037(12) N5 0.0319(16) 0.0211(14) 0.0291(15) -0.0025(12) 0.0120(13) -0.0011(11) N6 0.0250(15) 0.0209(14) 0.0309(15) -0.0022(12) 0.0094(13) -0.0004(11) N7 0.0293(16) 0.0282(16) 0.0402(18) 0.0008(13) 0.0138(14) 0.0056(12) N8 0.0297(16) 0.0227(14) 0.0338(16) 0.0024(12) 0.0101(13) 0.0033(12) N9 0.0326(16) 0.0236(14) 0.0360(16) 0.0037(13) 0.0143(14) 0.0024(12) N10 0.0328(16) 0.0262(15) 0.0359(17) -0.0004(13) 0.0147(14) 0.0032(12) N11 0.0262(15) 0.0251(15) 0.0359(16) 0.0002(13) 0.0087(14) 0.0038(12) N12 0.0286(16) 0.0280(15) 0.0374(17) 0.0028(13) 0.0122(14) 0.0040(12) O1 0.0357(14) 0.0261(12) 0.0396(14) -0.0003(11) 0.0179(12) 0.0057(10) O2 0.0435(15) 0.0215(12) 0.0331(13) -0.0003(10) 0.0152(12) 0.0004(10) O3 0.0451(16) 0.0228(13) 0.0452(15) 0.0029(11) 0.0197(13) 0.0049(11) O4 0.0435(16) 0.0331(15) 0.0601(18) 0.0146(13) 0.0157(15) 0.0089(12) O5 0.0394(15) 0.0342(14) 0.0568(18) 0.0077(13) 0.0191(14) 0.0130(12) O6 0.0348(15) 0.0421(15) 0.0476(17) -0.0051(13) 0.0058(13) 0.0144(12) _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 O1W Dy1 2.353(3) . ? O2W Dy1 2.405(3) . ? O3W Dy1 2.365(3) . ? O4W Dy1 2.329(3) . ? O5W Dy1 2.441(3) . ? O6W Dy1 2.388(3) . ? Dy1 O1 2.344(2) . ? Dy1 O2 2.375(2) . ? C1 O1 1.238(4) . ? C1 N1 1.346(4) . ? C1 N2 1.360(4) . ? C2 N3 1.448(4) . ? C2 N1 1.462(4) . ? C2 C3 1.542(5) . ? C2 H2 0.9900 . ? C3 N2 1.448(4) . ? C3 N4 1.458(4) . ? C3 H3 0.9900 . ? C4 O4 1.220(4) . ? C4 N4 1.352(5) . ? C4 N3 1.363(5) . ? C5 N2 1.429(4) . ? C5 N5 1.437(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.441(4) . ? C6 N4 1.454(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.232(4) . ? C7 N5 1.356(4) . ? C7 N6 1.356(4) . ? C8 N5 1.454(4) . ? C8 N7 1.458(4) . ? C8 C9 1.548(5) . ? C8 H8 0.9900 . ? C9 N8 1.439(4) . ? C9 N6 1.463(4) . ? C9 H9 0.9900 . ? C10 O5 1.218(4) . ? C10 N7 1.367(5) . ? C10 N8 1.371(5) . ? C11 N9 1.434(4) . ? C11 N6 1.439(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.443(5) . ? C12 N11 1.455(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.219(4) . ? C13 N9 1.365(5) . ? C13 N10 1.365(5) . ? C14 N11 1.448(4) . ? C14 N9 1.454(4) . ? C14 C15 1.551(5) . ? C14 H14 0.9900 . ? C15 N10 1.446(4) . ? C15 N12 1.452(4) . ? C15 H15 0.9900 . ? C16 O6 1.224(4) . ? C16 N11 1.355(5) . ? C16 N12 1.368(5) . ? C17 N3 1.430(5) 3_655 ? C17 N10 1.450(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N1 1.446(4) . ? C18 N12 1.446(5) 3_655 ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? N3 C17 1.430(5) 3_655 ? N12 C18 1.446(5) 3_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 O4W Dy1 O1 101.13(10) . . ? O4W Dy1 O1W 75.19(10) . . ? O1 Dy1 O1W 73.06(9) . . ? O4W Dy1 O3W 83.54(12) . . ? O1 Dy1 O3W 149.09(9) . . ? O1W Dy1 O3W 136.74(9) . . ? O4W Dy1 O2 72.63(9) . . ? O1 Dy1 O2 78.07(8) . . ? O1W Dy1 O2 131.00(9) . . ? O3W Dy1 O2 74.23(10) . . ? O4W Dy1 O6W 145.50(10) . . ? O1 Dy1 O6W 83.21(10) . . ? O1W Dy1 O6W 73.47(11) . . ? O3W Dy1 O6W 110.23(12) . . ? O2 Dy1 O6W 140.76(10) . . ? O4W Dy1 O2W 142.21(10) . . ? O1 Dy1 O2W 88.48(9) . . ? O1W Dy1 O2W 141.93(10) . . ? O3W Dy1 O2W 70.93(10) . . ? O2 Dy1 O2W 73.86(9) . . ? O6W Dy1 O2W 71.45(10) . . ? O4W Dy1 O5W 79.75(11) . . ? O1 Dy1 O5W 142.33(9) . . ? O1W Dy1 O5W 70.83(9) . . ? O3W Dy1 O5W 68.55(9) . . ? O2 Dy1 O5W 135.55(9) . . ? O6W Dy1 O5W 76.68(11) . . ? O2W Dy1 O5W 114.04(10) . . ? O1 C1 N1 125.6(3) . . ? O1 C1 N2 125.1(3) . . ? N1 C1 N2 109.3(3) . . ? N3 C2 N1 113.3(3) . . ? N3 C2 C3 103.5(3) . . ? N1 C2 C3 103.5(3) . . ? N3 C2 H2 112.0 . . ? N1 C2 H2 112.0 . . ? C3 C2 H2 112.0 . . ? N2 C3 N4 114.3(3) . . ? N2 C3 C2 102.9(3) . . ? N4 C3 C2 103.1(3) . . ? N2 C3 H3 112.0 . . ? N4 C3 H3 112.0 . . ? C2 C3 H3 112.0 . . ? O4 C4 N4 125.3(3) . . ? O4 C4 N3 125.8(4) . . ? N4 C4 N3 108.9(3) . . ? N2 C5 N5 113.7(3) . . ? N2 C5 H5A 108.8 . . ? N5 C5 H5A 108.8 . . ? N2 C5 H5B 108.8 . . ? N5 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N7 C6 N4 113.3(3) . . ? N7 C6 H6A 108.9 . . ? N4 C6 H6A 108.9 . . ? N7 C6 H6B 108.9 . . ? N4 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N5 125.6(3) . . ? O2 C7 N6 124.6(3) . . ? N5 C7 N6 109.8(3) . . ? N5 C8 N7 114.4(3) . . ? N5 C8 C9 103.4(3) . . ? N7 C8 C9 102.7(3) . . ? N5 C8 H8 111.9 . . ? N7 C8 H8 111.9 . . ? C9 C8 H8 111.9 . . ? N8 C9 N6 114.6(3) . . ? N8 C9 C8 103.8(3) . . ? N6 C9 C8 103.0(3) . . ? N8 C9 H9 111.6 . . ? N6 C9 H9 111.6 . . ? C8 C9 H9 111.6 . . ? O5 C10 N7 125.8(3) . . ? O5 C10 N8 125.9(3) . . ? N7 C10 N8 108.3(3) . . ? N9 C11 N6 113.9(3) . . ? N9 C11 H11A 108.8 . . ? N6 C11 H11A 108.8 . . ? N9 C11 H11B 108.8 . . ? N6 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? N8 C12 N11 113.9(3) . . ? N8 C12 H12A 108.8 . . ? N11 C12 H12A 108.8 . . ? N8 C12 H12B 108.8 . . ? N11 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N9 126.2(3) . . ? O3 C13 N10 125.6(3) . . ? N9 C13 N10 108.1(3) . . ? N11 C14 N9 114.5(3) . . ? N11 C14 C15 104.0(3) . . ? N9 C14 C15 102.9(3) . . ? N11 C14 H14 111.6 . . ? N9 C14 H14 111.6 . . ? C15 C14 H14 111.6 . . ? N10 C15 N12 115.8(3) . . ? N10 C15 C14 103.3(3) . . ? N12 C15 C14 102.8(3) . . ? N10 C15 H15 111.4 . . ? N12 C15 H15 111.4 . . ? C14 C15 H15 111.4 . . ? O6 C16 N11 124.4(3) . . ? O6 C16 N12 126.2(3) . . ? N11 C16 N12 109.4(3) . . ? N3 C17 N10 113.7(3) 3_655 . ? N3 C17 H17A 108.8 3_655 . ? N10 C17 H17A 108.8 . . ? N3 C17 H17B 108.8 3_655 . ? N10 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? N1 C18 N12 113.8(3) . 3_655 ? N1 C18 H18A 108.8 . . ? N12 C18 H18A 108.8 3_655 . ? N1 C18 H18B 108.8 . . ? N12 C18 H18B 108.8 3_655 . ? H18A C18 H18B 107.7 . . ? C1 N1 C18 124.7(3) . . ? C1 N1 C2 111.8(3) . . ? C18 N1 C2 122.8(3) . . ? C1 N2 C5 123.9(3) . . ? C1 N2 C3 112.5(3) . . ? C5 N2 C3 123.6(3) . . ? C4 N3 C17 121.9(3) . 3_655 ? C4 N3 C2 112.1(3) . . ? C17 N3 C2 122.7(3) 3_655 . ? C4 N4 C6 122.9(3) . . ? C4 N4 C3 112.1(3) . . ? C6 N4 C3 123.9(3) . . ? C7 N5 C5 123.9(3) . . ? C7 N5 C8 111.9(3) . . ? C5 N5 C8 124.2(3) . . ? C7 N6 C11 121.6(3) . . ? C7 N6 C9 111.5(3) . . ? C11 N6 C9 122.0(3) . . ? C10 N7 C6 123.7(3) . . ? C10 N7 C8 112.1(3) . . ? C6 N7 C8 123.3(3) . . ? C10 N8 C9 112.4(3) . . ? C10 N8 C12 123.6(3) . . ? C9 N8 C12 123.9(3) . . ? C13 N9 C11 122.8(3) . . ? C13 N9 C14 112.7(3) . . ? C11 N9 C14 123.9(3) . . ? C13 N10 C15 112.9(3) . . ? C13 N10 C17 123.0(3) . . ? C15 N10 C17 124.1(3) . . ? C16 N11 C14 111.6(3) . . ? C16 N11 C12 122.1(3) . . ? C14 N11 C12 124.2(3) . . ? C16 N12 C18 121.6(3) . 3_655 ? C16 N12 C15 111.7(3) . . ? C18 N12 C15 123.5(3) 3_655 . ? C1 O1 Dy1 156.8(2) . . ? C7 O2 Dy1 157.0(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.791 _refine_diff_density_min -0.649 _refine_diff_density_rms 0.083 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.104 0.073 0.402 19 9 ' ' 2 0.104 0.427 0.902 19 9 ' ' 3 0.500 0.500 0.500 107 29 ' ' 4 0.500 0.000 1.000 108 29 ' ' 5 0.389 0.260 0.083 10 8 ' ' 6 0.389 0.240 0.583 10 8 ' ' 7 0.611 0.760 0.417 10 8 ' ' 8 0.611 0.740 0.917 10 8 ' ' 9 0.896 0.573 0.098 19 9 ' ' 10 0.896 0.927 0.598 19 9 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 902620' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p310_2 #TrackingRef 'submit-310-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H74 Cl8 N24 O29 Zn2' _chemical_formula_weight 1721.53 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' Zn Zn 0.2839 1.4301 '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' _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 12.3060(7) _cell_length_b 20.5511(12) _cell_length_c 13.7026(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.421(2) _cell_angle_gamma 90.00 _cell_volume 3449.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1772 _exptl_absorpt_coefficient_mu 1.102 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7262 _exptl_absorpt_correction_T_max 0.7935 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32216 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6731 _reflns_number_gt 5130 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0719P)^2^+0.4701P] 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 6731 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1303 _refine_ls_wR_factor_gt 0.1233 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _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 O1W O 0.8490(4) -0.05336(18) 0.5889(4) 0.1614(19) Uani 1 1 d . . . O3W O 0.8900(5) -0.0959(3) 0.7850(6) 0.246(4) Uani 1 1 d . . . Zn1 Zn 0.90846(3) 0.145694(17) 0.54891(2) 0.05280(14) Uani 1 1 d . . . Cl1 Cl 0.90572(7) 0.22666(4) 0.66187(6) 0.0631(2) Uani 1 1 d . . . Cl2 Cl 1.02771(12) 0.07098(7) 0.61194(10) 0.1190(5) Uani 1 1 d . . . Cl3 Cl 0.96062(7) 0.18837(6) 0.40808(6) 0.0827(3) Uani 1 1 d . . . Cl4 Cl 0.74174(8) 0.10098(5) 0.51624(6) 0.0729(3) Uani 1 1 d . . . C1 C 0.6757(2) 0.17762(13) 1.0843(2) 0.0485(6) Uani 1 1 d . . . C2 C 0.8386(2) 0.11859(14) 1.1056(2) 0.0469(6) Uani 1 1 d . . . H2 H 0.9034 0.1350 1.1466 0.056 Uiso 1 1 calc R . . C3 C 0.8274(2) 0.15080(13) 1.0035(2) 0.0455(6) Uani 1 1 d . . . H3 H 0.8863 0.1828 0.9966 0.055 Uiso 1 1 calc R . . C4 C 0.8503(2) 0.03811(14) 0.9865(2) 0.0480(6) Uani 1 1 d . . . C5 C 0.6832(2) 0.22770(13) 0.9218(2) 0.0504(7) Uani 1 1 d . . . H5A H 0.6383 0.2610 0.9498 0.061 Uiso 1 1 calc R . . H5B H 0.7463 0.2496 0.8979 0.061 Uiso 1 1 calc R . . C6 C 0.8337(2) 0.10194(15) 0.83282(19) 0.0494(7) Uani 1 1 d . . . H6A H 0.8708 0.0642 0.8075 0.059 Uiso 1 1 calc R . . H6B H 0.8750 0.1409 0.8178 0.059 Uiso 1 1 calc R . . C7 C 0.5089(2) 0.19558(13) 0.8301(2) 0.0475(6) Uani 1 1 d . . . C8 C 0.6672(2) 0.16635(13) 0.75853(19) 0.0450(6) Uani 1 1 d . . . H8 H 0.7123 0.1972 0.7242 0.054 Uiso 1 1 calc R . . C9 C 0.5657(2) 0.14383(14) 0.69177(19) 0.0457(6) Uani 1 1 d . . . H9 H 0.5639 0.1628 0.6252 0.055 Uiso 1 1 calc R . . C10 C 0.6734(2) 0.05404(14) 0.73895(19) 0.0470(6) Uani 1 1 d . . . C11 C 0.3626(2) 0.15630(14) 0.7085(2) 0.0519(7) Uani 1 1 d . . . H11A H 0.3535 0.1638 0.6375 0.062 Uiso 1 1 calc R . . H11B H 0.3184 0.1887 0.7392 0.062 Uiso 1 1 calc R . . C12 C 0.5168(2) 0.03244(15) 0.62028(19) 0.0494(7) Uani 1 1 d . . . H12A H 0.5645 -0.0028 0.6019 0.059 Uiso 1 1 calc R . . H12B H 0.4950 0.0578 0.5611 0.059 Uiso 1 1 calc R . . C13 C 0.2518(2) 0.08175(14) 0.7994(2) 0.0498(7) Uani 1 1 d . . . C14 C 0.3183(2) 0.03851(14) 0.65941(19) 0.0454(6) Uani 1 1 d . . . H14 H 0.2871 0.0521 0.5933 0.054 Uiso 1 1 calc R . . C15 C 0.2458(2) -0.01234(13) 0.70459(19) 0.0459(6) Uani 1 1 d . . . H15 H 0.1826 -0.0249 0.6583 0.055 Uiso 1 1 calc R . . C16 C 0.4180(2) -0.05645(14) 0.69370(19) 0.0484(6) Uani 1 1 d . . . C17 C 0.1207(2) -0.00165(15) 0.8411(2) 0.0521(7) Uani 1 1 d . . . H17A H 0.0647 -0.0200 0.7933 0.063 Uiso 1 1 calc R . . H17B H 0.0886 0.0357 0.8722 0.063 Uiso 1 1 calc R . . C18 C 0.2797(3) -0.13026(14) 0.7515(2) 0.0511(7) Uani 1 1 d . . . H18A H 0.3329 -0.1630 0.7348 0.061 Uiso 1 1 calc R . . H18B H 0.2109 -0.1389 0.7115 0.061 Uiso 1 1 calc R . . N1 N 0.73790(19) 0.13699(11) 1.14582(17) 0.0480(5) Uani 1 1 d . . . N2 N 0.72158(18) 0.18176(11) 0.99848(16) 0.0491(5) Uani 1 1 d . . . N3 N 0.84860(19) 0.05034(11) 1.08443(16) 0.0488(5) Uani 1 1 d . . . N4 N 0.83478(19) 0.09589(11) 0.93771(16) 0.0485(5) Uani 1 1 d . . . N5 N 0.62018(18) 0.19714(11) 0.84010(16) 0.0468(5) Uani 1 1 d . . . N6 N 0.47587(18) 0.16625(12) 0.74312(17) 0.0484(5) Uani 1 1 d . . . N7 N 0.72499(18) 0.10644(11) 0.78270(16) 0.0459(5) Uani 1 1 d . . . N8 N 0.57771(17) 0.07393(11) 0.69049(15) 0.0446(5) Uani 1 1 d . . . N9 N 0.32168(18) 0.09199(11) 0.72841(17) 0.0480(5) Uani 1 1 d . . . N10 N 0.21150(18) 0.02062(11) 0.79004(16) 0.0462(5) Uani 1 1 d . . . N11 N 0.42053(18) 0.00435(12) 0.65562(17) 0.0485(5) Uani 1 1 d . . . N12 N 0.31853(18) -0.06676(11) 0.72741(15) 0.0458(5) Uani 1 1 d . . . O1 O 0.59395(17) 0.20627(10) 1.10476(16) 0.0613(5) Uani 1 1 d . . . O2 O 0.44993(17) 0.21859(11) 0.88779(16) 0.0619(5) Uani 1 1 d . . . O3 O 0.2310(2) 0.12179(11) 0.86127(18) 0.0716(6) Uani 1 1 d . . . O4 O 0.86489(19) -0.01471(10) 0.94946(16) 0.0632(6) Uani 1 1 d . . . O5 O 0.70796(18) -0.00209(11) 0.74132(17) 0.0647(6) Uani 1 1 d . . . O6 O 0.49162(18) -0.09665(11) 0.69647(17) 0.0639(6) 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 O1W 0.182(4) 0.092(3) 0.227(5) -0.007(3) 0.107(4) 0.016(3) O3W 0.146(4) 0.197(6) 0.389(10) -0.125(6) -0.009(5) 0.025(4) Zn1 0.0610(2) 0.0552(2) 0.0420(2) 0.00529(14) 0.00417(15) 0.01342(16) Cl1 0.0792(5) 0.0526(5) 0.0591(4) -0.0030(3) 0.0158(4) -0.0054(4) Cl2 0.1309(10) 0.1100(9) 0.1104(9) 0.0179(7) -0.0175(7) 0.0703(8) Cl3 0.0698(5) 0.1296(9) 0.0505(4) 0.0155(5) 0.0146(4) -0.0062(5) Cl4 0.0810(5) 0.0865(6) 0.0534(4) -0.0106(4) 0.0179(4) -0.0206(5) C1 0.0531(16) 0.0353(15) 0.0563(16) -0.0045(12) 0.0005(13) -0.0033(13) C2 0.0469(14) 0.0434(16) 0.0493(15) -0.0011(12) -0.0020(12) -0.0039(12) C3 0.0429(14) 0.0423(15) 0.0502(15) 0.0040(12) -0.0014(11) -0.0051(11) C4 0.0426(14) 0.0480(17) 0.0529(16) 0.0043(13) 0.0019(12) 0.0001(12) C5 0.0578(16) 0.0369(15) 0.0547(16) 0.0028(12) -0.0048(13) -0.0014(12) C6 0.0423(14) 0.0575(18) 0.0490(15) 0.0030(13) 0.0075(11) 0.0032(12) C7 0.0528(15) 0.0390(15) 0.0508(15) 0.0038(12) 0.0052(12) 0.0022(12) C8 0.0481(14) 0.0428(15) 0.0447(14) 0.0068(12) 0.0072(11) -0.0040(12) C9 0.0479(14) 0.0497(17) 0.0397(14) 0.0056(11) 0.0051(11) -0.0005(12) C10 0.0521(15) 0.0483(17) 0.0416(14) 0.0016(12) 0.0097(11) 0.0043(13) C11 0.0480(15) 0.0431(16) 0.0636(18) 0.0037(13) -0.0004(13) 0.0035(12) C12 0.0527(15) 0.0560(18) 0.0405(14) -0.0068(12) 0.0104(12) -0.0004(13) C13 0.0516(15) 0.0483(17) 0.0481(15) -0.0004(13) -0.0019(12) 0.0074(13) C14 0.0489(14) 0.0476(16) 0.0382(13) 0.0007(11) -0.0034(11) -0.0003(12) C15 0.0487(14) 0.0469(16) 0.0406(13) -0.0008(11) -0.0031(11) -0.0003(12) C16 0.0547(16) 0.0491(17) 0.0403(14) -0.0063(12) -0.0012(11) 0.0020(14) C17 0.0470(15) 0.0544(18) 0.0551(16) 0.0118(13) 0.0056(12) 0.0076(13) C18 0.0654(18) 0.0420(16) 0.0453(15) -0.0090(12) 0.0025(13) -0.0038(13) N1 0.0539(13) 0.0418(13) 0.0481(13) 0.0009(10) 0.0034(10) 0.0011(10) N2 0.0513(13) 0.0460(14) 0.0493(13) 0.0042(10) 0.0005(10) 0.0013(11) N3 0.0556(13) 0.0416(13) 0.0492(13) 0.0056(10) 0.0043(10) 0.0043(10) N4 0.0531(13) 0.0459(14) 0.0458(12) 0.0025(10) 0.0019(10) -0.0015(10) N5 0.0459(12) 0.0454(13) 0.0486(12) -0.0032(10) 0.0008(10) 0.0027(10) N6 0.0438(12) 0.0482(13) 0.0524(13) -0.0025(11) 0.0000(10) 0.0030(10) N7 0.0461(12) 0.0458(13) 0.0453(12) -0.0004(10) 0.0020(9) 0.0042(10) N8 0.0469(12) 0.0460(13) 0.0406(11) -0.0031(10) 0.0027(9) -0.0009(10) N9 0.0493(12) 0.0430(13) 0.0522(13) -0.0009(10) 0.0068(10) 0.0013(10) N10 0.0500(12) 0.0438(13) 0.0449(12) 0.0007(10) 0.0045(10) 0.0003(10) N11 0.0494(12) 0.0455(14) 0.0502(13) -0.0027(10) 0.0029(10) -0.0010(10) N12 0.0518(12) 0.0420(13) 0.0429(11) 0.0012(10) 0.0014(9) 0.0009(10) O1 0.0636(13) 0.0530(13) 0.0675(13) 0.0005(10) 0.0076(10) 0.0118(10) O2 0.0600(12) 0.0611(14) 0.0655(13) -0.0132(10) 0.0111(10) 0.0094(10) O3 0.0847(16) 0.0553(13) 0.0787(15) -0.0164(12) 0.0278(13) 0.0001(12) O4 0.0784(14) 0.0471(13) 0.0645(13) -0.0033(10) 0.0091(11) 0.0121(11) O5 0.0681(13) 0.0522(13) 0.0723(14) -0.0063(10) -0.0007(11) 0.0144(11) O6 0.0628(13) 0.0561(13) 0.0735(14) 0.0015(11) 0.0107(11) 0.0137(11) _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 Zn1 Cl2 2.2400(10) . ? Zn1 Cl4 2.2540(10) . ? Zn1 Cl3 2.2669(9) . ? Zn1 Cl1 2.2751(8) . ? C1 O1 1.221(3) . ? C1 N2 1.354(4) . ? C1 N1 1.368(4) . ? C2 N3 1.440(4) . ? C2 N1 1.453(4) . ? C2 C3 1.543(4) . ? C2 H2 0.9900 . ? C3 N2 1.445(4) . ? C3 N4 1.453(4) . ? C3 H3 0.9900 . ? C4 O4 1.219(3) . ? C4 N4 1.367(4) . ? C4 N3 1.368(4) . ? C5 N5 1.444(3) . ? C5 N2 1.458(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.441(3) . ? C6 N7 1.448(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.219(3) . ? C7 N6 1.363(4) . ? C7 N5 1.363(4) . ? C8 N7 1.445(4) . ? C8 N5 1.451(3) . ? C8 C9 1.547(4) . ? C8 H8 0.9900 . ? C9 N6 1.441(3) . ? C9 N8 1.444(4) . ? C9 H9 0.9900 . ? C10 O5 1.229(3) . ? C10 N8 1.359(4) . ? C10 N7 1.360(4) . ? C11 N6 1.444(4) . ? C11 N9 1.450(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.442(4) . ? C12 N11 1.442(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.226(3) . ? C13 N10 1.352(4) . ? C13 N9 1.374(4) . ? C14 N11 1.445(4) . ? C14 N9 1.448(4) . ? C14 C15 1.542(4) . ? C14 H14 0.9900 . ? C15 N12 1.448(3) . ? C15 N10 1.449(3) . ? C15 H15 0.9900 . ? C16 O6 1.224(3) . ? C16 N11 1.356(4) . ? C16 N12 1.366(4) . ? C17 N10 1.448(3) . ? C17 N3 1.453(3) 3_657 ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.439(4) . ? C18 N1 1.450(4) 3_657 ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? N1 C18 1.450(4) 3_657 ? N3 C17 1.453(3) 3_657 ? 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 Cl2 Zn1 Cl4 110.36(5) . . ? Cl2 Zn1 Cl3 111.44(5) . . ? Cl4 Zn1 Cl3 108.32(3) . . ? Cl2 Zn1 Cl1 106.87(4) . . ? Cl4 Zn1 Cl1 111.19(3) . . ? Cl3 Zn1 Cl1 108.65(4) . . ? O1 C1 N2 126.1(3) . . ? O1 C1 N1 125.3(3) . . ? N2 C1 N1 108.5(2) . . ? N3 C2 N1 115.0(2) . . ? N3 C2 C3 103.7(2) . . ? N1 C2 C3 103.0(2) . . ? N3 C2 H2 111.5 . . ? N1 C2 H2 111.5 . . ? C3 C2 H2 111.5 . . ? N2 C3 N4 115.0(2) . . ? N2 C3 C2 103.6(2) . . ? N4 C3 C2 103.0(2) . . ? N2 C3 H3 111.6 . . ? N4 C3 H3 111.6 . . ? C2 C3 H3 111.6 . . ? O4 C4 N4 126.1(3) . . ? O4 C4 N3 126.0(3) . . ? N4 C4 N3 107.8(2) . . ? N5 C5 N2 113.0(2) . . ? N5 C5 H5A 109.0 . . ? N2 C5 H5A 109.0 . . ? N5 C5 H5B 109.0 . . ? N2 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N4 C6 N7 113.6(2) . . ? N4 C6 H6A 108.9 . . ? N7 C6 H6A 108.9 . . ? N4 C6 H6B 108.9 . . ? N7 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N6 126.3(3) . . ? O2 C7 N5 125.4(3) . . ? N6 C7 N5 108.2(2) . . ? N7 C8 N5 114.7(2) . . ? N7 C8 C9 103.5(2) . . ? N5 C8 C9 103.2(2) . . ? N7 C8 H8 111.6 . . ? N5 C8 H8 111.6 . . ? C9 C8 H8 111.6 . . ? N6 C9 N8 114.1(2) . . ? N6 C9 C8 103.3(2) . . ? N8 C9 C8 103.1(2) . . ? N6 C9 H9 111.9 . . ? N8 C9 H9 111.9 . . ? C8 C9 H9 111.9 . . ? O5 C10 N8 125.3(3) . . ? O5 C10 N7 125.8(3) . . ? N8 C10 N7 108.9(2) . . ? N6 C11 N9 114.1(2) . . ? N6 C11 H11A 108.7 . . ? N9 C11 H11A 108.7 . . ? N6 C11 H11B 108.7 . . ? N9 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? N8 C12 N11 113.9(2) . . ? N8 C12 H12A 108.8 . . ? N11 C12 H12A 108.8 . . ? N8 C12 H12B 108.8 . . ? N11 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N10 126.2(3) . . ? O3 C13 N9 124.9(3) . . ? N10 C13 N9 108.9(2) . . ? N11 C14 N9 114.9(2) . . ? N11 C14 C15 102.9(2) . . ? N9 C14 C15 103.5(2) . . ? N11 C14 H14 111.6 . . ? N9 C14 H14 111.6 . . ? C15 C14 H14 111.6 . . ? N12 C15 N10 114.1(2) . . ? N12 C15 C14 103.9(2) . . ? N10 C15 C14 103.4(2) . . ? N12 C15 H15 111.6 . . ? N10 C15 H15 111.6 . . ? C14 C15 H15 111.6 . . ? O6 C16 N11 126.2(3) . . ? O6 C16 N12 124.7(3) . . ? N11 C16 N12 109.1(2) . . ? N10 C17 N3 113.3(2) . 3_657 ? N10 C17 H17A 108.9 . . ? N3 C17 H17A 108.9 3_657 . ? N10 C17 H17B 108.9 . . ? N3 C17 H17B 108.9 3_657 . ? H17A C17 H17B 107.7 . . ? N12 C18 N1 113.1(2) . 3_657 ? N12 C18 H18A 109.0 . . ? N1 C18 H18A 109.0 3_657 . ? N12 C18 H18B 109.0 . . ? N1 C18 H18B 109.0 3_657 . ? H18A C18 H18B 107.8 . . ? C1 N1 C18 122.0(2) . 3_657 ? C1 N1 C2 111.9(2) . . ? C18 N1 C2 123.6(2) 3_657 . ? C1 N2 C3 112.3(2) . . ? C1 N2 C5 122.2(2) . . ? C3 N2 C5 123.2(2) . . ? C4 N3 C2 112.7(2) . . ? C4 N3 C17 122.4(2) . 3_657 ? C2 N3 C17 123.4(2) . 3_657 ? C4 N4 C6 123.4(2) . . ? C4 N4 C3 112.7(2) . . ? C6 N4 C3 123.8(2) . . ? C7 N5 C5 123.3(2) . . ? C7 N5 C8 112.4(2) . . ? C5 N5 C8 124.2(2) . . ? C7 N6 C9 112.9(2) . . ? C7 N6 C11 123.3(2) . . ? C9 N6 C11 123.7(2) . . ? C10 N7 C8 112.0(2) . . ? C10 N7 C6 122.0(2) . . ? C8 N7 C6 125.2(2) . . ? C10 N8 C12 121.3(2) . . ? C10 N8 C9 112.2(2) . . ? C12 N8 C9 123.3(2) . . ? C13 N9 C14 111.4(2) . . ? C13 N9 C11 121.7(2) . . ? C14 N9 C11 123.9(2) . . ? C13 N10 C17 122.7(2) . . ? C13 N10 C15 112.2(2) . . ? C17 N10 C15 122.7(2) . . ? C16 N11 C12 123.2(2) . . ? C16 N11 C14 112.5(2) . . ? C12 N11 C14 124.2(2) . . ? C16 N12 C18 123.1(2) . . ? C16 N12 C15 111.3(2) . . ? C18 N12 C15 122.5(2) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.483 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.056 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.372 0.360 829 268 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 902621' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p311 #TrackingRef 'submit-311.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H100 Cl5 Ho N24 O44 Zn' _chemical_formula_weight 1980.95 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ho Ho -0.2175 4.6783 '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 15.31(2) _cell_length_b 15.81(2) _cell_length_c 17.28(2) _cell_angle_alpha 64.156(15) _cell_angle_beta 81.043(17) _cell_angle_gamma 81.527(17) _cell_volume 3704(9) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.776 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2036 _exptl_absorpt_coefficient_mu 1.681 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7191 _exptl_absorpt_correction_T_max 0.7987 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24423 _diffrn_reflns_av_R_equivalents 0.0815 _diffrn_reflns_av_sigmaI/netI 0.1463 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12591 _reflns_number_gt 6678 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0824P)^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 12591 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1101 _refine_ls_R_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.1841 _refine_ls_wR_factor_gt 0.1657 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.004 _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 Cl5 Cl 1.0107(2) 0.2032(2) 0.9496(2) 0.1023(11) Uani 1 1 d . . . O5W O 0.2923(9) -0.0882(9) 1.3094(9) 0.224(8) Uani 1 1 d . . . O1W O 0.9350(4) -0.1336(4) 0.8579(4) 0.0597(17) Uani 1 1 d . . . O2W O 0.6314(4) -0.0644(5) 0.8358(4) 0.0622(18) Uani 1 1 d . . . O3W O 0.7408(4) -0.2386(4) 0.8928(4) 0.0625(17) Uani 1 1 d . . . O4W O 0.8948(4) 0.0174(4) 0.6980(4) 0.0578(17) Uani 1 1 d . . . Ho2 Ho 0.79144(3) -0.08585(3) 0.80800(3) 0.04236(16) Uani 1 1 d . . . Cl1 Cl 0.3592(2) 0.4527(2) 0.3321(3) 0.1405(17) Uani 1 1 d . . . Cl2 Cl 0.6075(2) 0.4583(2) 0.3113(3) 0.1320(15) Uani 1 1 d . . . Cl3 Cl 0.5123(2) 0.2424(2) 0.3444(3) 0.1130(12) Uani 1 1 d . . . Cl4 Cl 0.4815(5) 0.3153(5) 0.5239(3) 0.252(4) Uani 1 1 d . . . Zn1 Zn 0.49025(9) 0.36863(9) 0.37899(9) 0.0894(5) Uani 1 1 d . . . C1 C 0.7466(6) 0.1287(7) 0.8269(6) 0.051(2) Uani 1 1 d . . . C2 C 0.7063(5) 0.2756(6) 0.8354(5) 0.042(2) Uani 1 1 d . . . H2 H 0.7292 0.3354 0.7919 0.051 Uiso 1 1 calc R . . C3 C 0.7742(6) 0.2164(6) 0.9021(6) 0.050(2) Uani 1 1 d . . . H3 H 0.8274 0.2504 0.8911 0.060 Uiso 1 1 calc R . . C4 C 0.6435(6) 0.2499(7) 0.9770(7) 0.055(2) Uani 1 1 d . . . C5 C 0.8594(5) 0.0534(6) 0.9313(6) 0.050(2) Uani 1 1 d . . . H5A H 0.9072 0.0787 0.9442 0.060 Uiso 1 1 calc R . . H5B H 0.8858 0.0222 0.8939 0.060 Uiso 1 1 calc R . . C6 C 0.7645(6) 0.1534(6) 1.0681(6) 0.057(3) Uani 1 1 d . . . H6A H 0.7365 0.1829 1.1064 0.068 Uiso 1 1 calc R . . H6B H 0.8277 0.1634 1.0572 0.068 Uiso 1 1 calc R . . C7 C 0.7856(5) -0.0929(6) 1.0144(6) 0.042(2) Uani 1 1 d . . . C8 C 0.8177(6) -0.0165(6) 1.0982(6) 0.048(2) Uani 1 1 d . . . H8 H 0.8779 -0.0147 1.1112 0.058 Uiso 1 1 calc R . . C9 C 0.7774(5) -0.1128(6) 1.1610(5) 0.042(2) Uani 1 1 d . . . H9 H 0.8192 -0.1560 1.2026 0.051 Uiso 1 1 calc R . . C10 C 0.6864(7) 0.0159(8) 1.1767(7) 0.060(3) Uani 1 1 d . . . C11 C 0.7396(6) -0.2477(6) 1.1310(6) 0.054(2) Uani 1 1 d . . . H11A H 0.7593 -0.2661 1.0833 0.065 Uiso 1 1 calc R . . H11B H 0.7747 -0.2884 1.1789 0.065 Uiso 1 1 calc R . . C12 C 0.6458(6) -0.1471(6) 1.2780(6) 0.052(2) Uani 1 1 d . . . H12A H 0.6856 -0.1970 1.3162 0.062 Uiso 1 1 calc R . . H12B H 0.6130 -0.1126 1.3104 0.062 Uiso 1 1 calc R . . C13 C 0.5941(6) -0.2870(6) 1.1116(6) 0.050(2) Uani 1 1 d . . . C14 C 0.6061(5) -0.2771(6) 1.2431(5) 0.046(2) Uani 1 1 d . . . H14 H 0.6403 -0.3252 1.2896 0.055 Uiso 1 1 calc R . . C15 C 0.5113(5) -0.3091(6) 1.2460(5) 0.044(2) Uani 1 1 d . . . H15 H 0.5025 -0.3723 1.2934 0.052 Uiso 1 1 calc R . . C16 C 0.4909(6) -0.1685(7) 1.2673(5) 0.047(2) Uani 1 1 d . . . C17 C 0.4505(6) -0.3517(6) 1.1390(6) 0.051(2) Uani 1 1 d . . . H17A H 0.4337 -0.4081 1.1906 0.062 Uiso 1 1 calc R . . H17B H 0.4785 -0.3724 1.0944 0.062 Uiso 1 1 calc R . . C18 C 0.3555(5) -0.2415(6) 1.2789(5) 0.045(2) Uani 1 1 d . . . H18A H 0.3318 -0.2013 1.3088 0.053 Uiso 1 1 calc R . . H18B H 0.3445 -0.3066 1.3189 0.053 Uiso 1 1 calc R . . C19 C 0.7118(5) -0.0382(6) 0.6114(6) 0.048(2) Uani 1 1 d . . . C20 C 0.6654(5) 0.0046(6) 0.4758(5) 0.047(2) Uani 1 1 d . . . H20 H 0.6032 0.0294 0.4643 0.056 Uiso 1 1 calc R . . C21 C 0.6734(6) -0.1036(7) 0.5226(6) 0.061(3) Uani 1 1 d . . . H21 H 0.6160 -0.1296 0.5304 0.073 Uiso 1 1 calc R . . C22 C 0.7662(6) -0.0590(7) 0.3913(7) 0.052(2) Uani 1 1 d . . . C23 C 0.7146(5) -0.2127(6) 0.6784(6) 0.055(2) Uani 1 1 d . . . H23A H 0.6728 -0.2536 0.6775 0.066 Uiso 1 1 calc R . . H23B H 0.7009 -0.2065 0.7331 0.066 Uiso 1 1 calc R . . C24 C 0.7715(6) -0.2310(7) 0.4856(6) 0.055(2) Uani 1 1 d . . . H24A H 0.7886 -0.2366 0.4309 0.066 Uiso 1 1 calc R . . H24B H 0.7220 -0.2699 0.5162 0.066 Uiso 1 1 calc R . . C25 C 0.8716(6) -0.2396(6) 0.7122(6) 0.053(3) Uani 1 1 d . . . C26 C 0.8391(6) -0.3180(6) 0.6299(5) 0.047(2) Uani 1 1 d . . . H26 H 0.8041 -0.3730 0.6501 0.057 Uiso 1 1 calc R . . C27 C 0.9371(6) -0.3492(6) 0.6540(6) 0.050(2) Uani 1 1 d . . . H27 H 0.9475 -0.4181 0.6884 0.060 Uiso 1 1 calc R . . C28 C 0.9329(7) -0.2714(7) 0.5015(7) 0.056(3) Uani 1 1 d . . . C29 C 1.0220(5) -0.3141(6) 0.7523(5) 0.043(2) Uani 1 1 d . . . H29A H 1.0387 -0.3822 0.7791 0.051 Uiso 1 1 calc R . . H29B H 1.0016 -0.2941 0.7989 0.051 Uiso 1 1 calc R . . C30 C 1.0822(6) -0.3424(6) 0.5548(6) 0.056(2) Uani 1 1 d . . . H30A H 1.0959 -0.4081 0.5954 0.067 Uiso 1 1 calc R . . H30B H 1.0962 -0.3388 0.4962 0.067 Uiso 1 1 calc R . . C31 C 1.1300(6) -0.1936(6) 0.7153(6) 0.046(2) Uani 1 1 d . . . C32 C 1.1655(6) -0.3018(6) 0.6504(5) 0.051(2) Uani 1 1 d . . . H32 H 1.1861 -0.3689 0.6835 0.061 Uiso 1 1 calc R . . C33 C 1.2411(5) -0.2371(6) 0.6248(5) 0.043(2) Uani 1 1 d . . . H33 H 1.2972 -0.2748 0.6456 0.052 Uiso 1 1 calc R . . C34 C 1.1886(6) -0.2218(6) 0.5000(6) 0.045(2) Uani 1 1 d . . . C35 C 0.7315(6) 0.1163(6) 0.3213(6) 0.051(2) Uani 1 1 d . . . H35A H 0.7545 0.1076 0.2688 0.062 Uiso 1 1 calc R . . H35B H 0.6721 0.1497 0.3125 0.062 Uiso 1 1 calc R . . C36 C 0.6814(6) 0.1316(6) 0.5243(6) 0.052(2) Uani 1 1 d . . . H36A H 0.6768 0.1297 0.5822 0.062 Uiso 1 1 calc R . . H36B H 0.6247 0.1603 0.5006 0.062 Uiso 1 1 calc R . . N1 N 0.6930(5) 0.2136(5) 0.7955(4) 0.0488(19) Uani 1 1 d . . . N2 N 0.7969(5) 0.1296(5) 0.8861(5) 0.0482(18) Uani 1 1 d . . . N3 N 0.6296(5) 0.2923(5) 0.8911(5) 0.054(2) Uani 1 1 d . . . N4 N 0.7260(5) 0.2010(6) 0.9871(5) 0.057(2) Uani 1 1 d . . . N5 N 0.8192(5) -0.0157(5) 1.0112(5) 0.0510(19) Uani 1 1 d . . . N6 N 0.7589(4) -0.1514(5) 1.1031(5) 0.0507(19) Uani 1 1 d . . . N7 N 0.7561(5) 0.0528(6) 1.1130(5) 0.054(2) Uani 1 1 d . . . N8 N 0.6991(4) -0.0821(6) 1.2034(5) 0.052(2) Uani 1 1 d . . . N9 N 0.6476(4) -0.2655(5) 1.1586(5) 0.0489(19) Uani 1 1 d . . . N10 N 0.5154(5) -0.3100(5) 1.1597(4) 0.0466(18) Uani 1 1 d . . . N11 N 0.5837(4) -0.1896(5) 1.2544(4) 0.0470(18) Uani 1 1 d . . . N12 N 0.4487(5) -0.2359(5) 1.2597(5) 0.0501(19) Uani 1 1 d . . . N13 N 0.6951(4) 0.0379(5) 0.5318(5) 0.0479(19) Uani 1 1 d . . . N14 N 0.7021(4) -0.1196(5) 0.6067(4) 0.0452(18) Uani 1 1 d . . . N15 N 0.7232(5) 0.0229(5) 0.3936(4) 0.0491(19) Uani 1 1 d . . . N16 N 0.7411(5) -0.1344(5) 0.4670(5) 0.0527(19) Uani 1 1 d . . . N17 N 0.8051(4) -0.2574(5) 0.6746(5) 0.0488(19) Uani 1 1 d . . . N18 N 0.9491(5) -0.2958(5) 0.7007(4) 0.0509(19) Uani 1 1 d . . . N19 N 0.8476(5) -0.2691(5) 0.5384(5) 0.052(2) Uani 1 1 d . . . N20 N 0.9874(5) -0.3169(5) 0.5682(5) 0.056(2) Uani 1 1 d . . . N21 N 1.1004(4) -0.2660(5) 0.7029(5) 0.0493(19) Uani 1 1 d . . . N22 N 1.2118(5) -0.1750(5) 0.6680(4) 0.0484(18) Uani 1 1 d . . . N23 N 1.1384(5) -0.2846(5) 0.5657(5) 0.054(2) Uani 1 1 d . . . N24 N 1.2490(4) -0.1915(5) 0.5301(4) 0.0458(18) Uani 1 1 d . . . O1 O 0.7543(4) 0.0668(4) 0.8004(4) 0.0509(16) Uani 1 1 d . . . O2 O 0.7782(4) -0.1121(4) 0.9560(3) 0.0501(16) Uani 1 1 d . . . O3 O 0.6179(4) -0.2851(5) 1.0388(4) 0.0623(18) Uani 1 1 d . . . O4 O 0.5909(5) 0.2597(5) 1.0370(5) 0.082(2) Uani 1 1 d . . . O5 O 0.6285(4) 0.0564(5) 1.2070(4) 0.0613(18) Uani 1 1 d . . . O6 O 0.4527(4) -0.1024(4) 1.2829(4) 0.0517(16) Uani 1 1 d . . . O7 O 0.7326(4) -0.0324(4) 0.6758(4) 0.0497(15) Uani 1 1 d . . . O8 O 0.8633(4) -0.1901(4) 0.7512(4) 0.0506(16) Uani 1 1 d . . . O9 O 1.0899(4) -0.1573(4) 0.7600(4) 0.0575(17) Uani 1 1 d . . . O10 O 0.8145(4) -0.0641(4) 0.3285(4) 0.0577(17) Uani 1 1 d . . . O11 O 0.9604(4) -0.2430(5) 0.4220(4) 0.073(2) Uani 1 1 d . . . O12 O 1.1823(4) -0.1964(4) 0.4196(4) 0.0611(17) 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 Cl5 0.072(2) 0.120(3) 0.119(3) -0.051(2) -0.0233(19) -0.0062(18) O5W 0.251(16) 0.225(14) 0.244(15) -0.161(13) -0.121(13) 0.139(13) O1W 0.042(4) 0.086(5) 0.061(4) -0.047(4) -0.001(3) 0.011(3) O2W 0.039(3) 0.087(5) 0.060(4) -0.036(4) 0.009(3) -0.004(3) O3W 0.062(4) 0.059(4) 0.070(5) -0.032(4) 0.002(3) -0.011(3) O4W 0.045(4) 0.065(4) 0.051(4) -0.018(3) 0.004(3) 0.001(3) Ho2 0.0414(3) 0.0520(3) 0.0371(3) -0.0235(2) -0.00310(17) 0.00006(18) Cl1 0.0613(19) 0.092(2) 0.174(4) 0.022(2) 0.007(2) 0.0010(17) Cl2 0.072(2) 0.077(2) 0.224(5) -0.045(3) -0.011(2) -0.0042(17) Cl3 0.0598(19) 0.103(2) 0.174(4) -0.054(3) -0.016(2) -0.0086(17) Cl4 0.313(8) 0.244(6) 0.081(3) -0.010(4) -0.011(4) 0.126(6) Zn1 0.0713(9) 0.0744(9) 0.0876(10) -0.0091(8) -0.0015(7) 0.0086(7) C1 0.047(6) 0.054(6) 0.047(6) -0.016(5) 0.005(5) -0.011(5) C2 0.037(5) 0.047(5) 0.037(5) -0.017(4) 0.003(4) 0.001(4) C3 0.049(5) 0.061(6) 0.050(6) -0.031(5) -0.008(5) -0.005(5) C4 0.046(6) 0.067(7) 0.067(7) -0.046(6) 0.005(5) -0.009(5) C5 0.043(5) 0.044(5) 0.056(6) -0.016(5) 0.000(4) 0.000(4) C6 0.060(6) 0.060(6) 0.059(7) -0.035(6) 0.007(5) -0.011(5) C7 0.035(5) 0.056(6) 0.039(6) -0.024(5) -0.006(4) -0.001(4) C8 0.050(6) 0.061(6) 0.053(6) -0.039(5) -0.012(5) -0.005(5) C9 0.036(5) 0.065(6) 0.032(5) -0.027(5) -0.006(4) 0.001(4) C10 0.057(7) 0.082(8) 0.062(7) -0.044(6) -0.027(6) -0.009(6) C11 0.054(6) 0.059(6) 0.053(6) -0.028(5) -0.009(5) 0.002(5) C12 0.050(6) 0.063(6) 0.044(6) -0.023(5) -0.009(4) -0.007(5) C13 0.051(6) 0.044(6) 0.054(6) -0.023(5) 0.000(5) 0.001(4) C14 0.041(5) 0.055(6) 0.035(5) -0.018(4) 0.004(4) 0.005(4) C15 0.045(5) 0.040(5) 0.044(5) -0.019(4) 0.004(4) -0.004(4) C16 0.053(6) 0.055(6) 0.029(5) -0.011(4) -0.010(4) -0.005(5) C17 0.048(6) 0.047(6) 0.061(6) -0.031(5) 0.005(5) 0.003(4) C18 0.045(5) 0.061(6) 0.029(5) -0.023(4) -0.002(4) 0.002(4) C19 0.032(5) 0.055(6) 0.064(7) -0.032(6) 0.000(5) -0.005(4) C20 0.039(5) 0.049(6) 0.046(6) -0.017(5) -0.004(4) 0.003(4) C21 0.049(6) 0.082(8) 0.052(6) -0.024(6) -0.014(5) -0.012(5) C22 0.050(6) 0.069(7) 0.054(7) -0.039(6) -0.013(5) -0.004(5) C23 0.034(5) 0.062(6) 0.059(6) -0.018(5) 0.003(4) -0.010(4) C24 0.059(6) 0.070(7) 0.045(6) -0.030(5) -0.009(5) -0.008(5) C25 0.047(6) 0.042(6) 0.048(6) -0.002(5) 0.007(5) -0.007(5) C26 0.057(6) 0.043(5) 0.044(6) -0.020(5) -0.008(4) 0.000(4) C27 0.056(6) 0.048(6) 0.060(6) -0.037(5) -0.004(5) -0.001(4) C28 0.059(7) 0.057(6) 0.062(7) -0.036(6) -0.003(6) -0.002(5) C29 0.046(5) 0.041(5) 0.031(5) -0.006(4) 0.000(4) -0.007(4) C30 0.043(6) 0.057(6) 0.071(7) -0.034(5) 0.011(5) -0.009(5) C31 0.042(5) 0.054(6) 0.043(6) -0.020(5) -0.007(4) -0.005(4) C32 0.054(6) 0.059(6) 0.035(5) -0.021(5) 0.001(4) 0.002(5) C33 0.044(5) 0.039(5) 0.041(5) -0.015(4) -0.007(4) 0.005(4) C34 0.044(5) 0.044(5) 0.047(6) -0.022(5) -0.001(5) 0.002(4) C35 0.049(6) 0.064(6) 0.050(6) -0.032(5) -0.009(4) -0.002(5) C36 0.048(6) 0.069(7) 0.045(6) -0.035(5) 0.008(4) -0.002(5) N1 0.052(5) 0.059(5) 0.037(4) -0.021(4) -0.006(4) -0.005(4) N2 0.051(4) 0.050(5) 0.049(5) -0.027(4) -0.006(4) 0.001(4) N3 0.049(5) 0.066(5) 0.055(5) -0.037(4) -0.006(4) 0.007(4) N4 0.055(5) 0.083(6) 0.034(5) -0.028(4) 0.007(4) -0.006(4) N5 0.046(4) 0.054(5) 0.043(5) -0.012(4) 0.000(4) -0.008(4) N6 0.047(4) 0.053(5) 0.052(5) -0.020(4) -0.014(4) -0.002(4) N7 0.046(5) 0.075(6) 0.042(5) -0.022(4) 0.001(4) -0.018(4) N8 0.039(4) 0.075(6) 0.044(5) -0.026(4) -0.003(4) -0.009(4) N9 0.036(4) 0.061(5) 0.046(5) -0.023(4) 0.002(4) 0.001(3) N10 0.045(4) 0.051(5) 0.043(4) -0.025(4) 0.013(4) -0.006(4) N11 0.038(4) 0.063(5) 0.048(5) -0.030(4) -0.012(3) 0.002(4) N12 0.040(4) 0.053(5) 0.058(5) -0.026(4) -0.001(4) -0.002(4) N13 0.044(4) 0.051(5) 0.053(5) -0.023(4) -0.021(4) 0.004(4) N14 0.048(4) 0.052(5) 0.036(4) -0.018(4) -0.006(3) -0.005(4) N15 0.047(4) 0.056(5) 0.043(5) -0.021(4) 0.000(4) -0.008(4) N16 0.055(5) 0.060(5) 0.046(5) -0.028(4) 0.003(4) -0.003(4) N17 0.039(4) 0.057(5) 0.053(5) -0.029(4) -0.001(4) 0.003(4) N18 0.041(4) 0.062(5) 0.044(5) -0.018(4) -0.004(4) -0.002(4) N19 0.052(5) 0.067(5) 0.037(5) -0.024(4) -0.003(4) 0.004(4) N20 0.055(5) 0.065(5) 0.052(5) -0.033(4) 0.004(4) 0.001(4) N21 0.037(4) 0.060(5) 0.053(5) -0.031(4) 0.006(4) -0.001(4) N22 0.047(5) 0.057(5) 0.046(5) -0.027(4) -0.006(4) -0.004(4) N23 0.061(5) 0.053(5) 0.051(5) -0.024(4) -0.001(4) -0.011(4) N24 0.045(4) 0.055(5) 0.040(4) -0.021(4) -0.001(3) -0.012(4) O1 0.058(4) 0.057(4) 0.048(4) -0.032(3) -0.013(3) 0.002(3) O2 0.053(4) 0.079(4) 0.030(3) -0.036(3) 0.002(3) -0.004(3) O3 0.061(4) 0.083(5) 0.054(4) -0.044(4) 0.011(3) -0.010(3) O4 0.081(5) 0.101(6) 0.064(5) -0.045(4) 0.012(4) 0.002(4) O5 0.061(4) 0.076(5) 0.063(4) -0.047(4) 0.001(3) -0.002(4) O6 0.049(4) 0.053(4) 0.057(4) -0.030(3) -0.005(3) 0.006(3) O7 0.044(4) 0.065(4) 0.054(4) -0.042(3) -0.006(3) 0.006(3) O8 0.055(4) 0.062(4) 0.047(4) -0.038(3) -0.005(3) 0.005(3) O9 0.051(4) 0.066(4) 0.060(4) -0.038(4) 0.008(3) 0.002(3) O10 0.061(4) 0.067(4) 0.048(4) -0.028(4) -0.009(3) 0.002(3) O11 0.071(5) 0.086(5) 0.056(5) -0.030(4) 0.004(4) 0.002(4) O12 0.064(4) 0.064(4) 0.053(4) -0.023(4) -0.006(3) -0.006(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 O5W Ho2 2.869(12) 2_657 ? O1W Ho2 2.383(6) . ? O2W Ho2 2.426(6) . ? O3W Ho2 2.386(7) . ? O4W Ho2 2.429(6) . ? Ho2 O8 2.330(6) . ? Ho2 O7 2.341(7) . ? Ho2 O1 2.347(7) . ? Ho2 O2 2.387(6) . ? Ho2 O5W 2.869(12) 2_657 ? Cl1 Zn1 2.286(4) . ? Cl2 Zn1 2.291(4) . ? Cl3 Zn1 2.286(5) . ? Cl4 Zn1 2.256(6) . ? C1 O1 1.233(10) . ? C1 N2 1.379(11) . ? C1 N1 1.396(11) . ? C2 N3 1.468(10) . ? C2 N1 1.472(10) . ? C2 C3 1.558(11) . ? C2 H2 0.9900 . ? C3 N4 1.471(10) . ? C3 N2 1.496(10) . ? C3 H3 0.9900 . ? C4 O4 1.262(10) . ? C4 N4 1.374(11) . ? C4 N3 1.374(12) . ? C5 N2 1.432(10) . ? C5 N5 1.447(10) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.442(11) . ? C6 N7 1.448(11) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.198(9) . ? C7 N5 1.370(11) . ? C7 N6 1.432(11) . ? C8 N7 1.421(11) . ? C8 N5 1.494(10) . ? C8 C9 1.582(12) . ? C8 H8 0.9900 . ? C9 N8 1.441(10) . ? C9 N6 1.458(10) . ? C9 H9 0.9900 . ? C10 O5 1.205(11) . ? C10 N7 1.396(12) . ? C10 N8 1.401(12) . ? C11 N9 1.442(10) . ? C11 N6 1.443(11) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.439(10) . ? C12 N8 1.466(10) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.243(10) . ? C13 N10 1.351(11) . ? C13 N9 1.407(11) . ? C14 N9 1.443(10) . ? C14 N11 1.464(10) . ? C14 C15 1.592(11) . ? C14 H14 0.9900 . ? C15 N12 1.468(10) . ? C15 N10 1.490(10) . ? C15 H15 0.9900 . ? C16 O6 1.235(10) . ? C16 N12 1.386(11) . ? C16 N11 1.417(11) . ? C17 N10 1.435(10) . ? C17 N3 1.445(10) 2_657 ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.421(10) . ? C18 N1 1.452(10) 2_657 ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O7 1.248(10) . ? C19 N14 1.354(11) . ? C19 N13 1.407(11) . ? C20 N13 1.440(10) . ? C20 N15 1.487(10) . ? C20 C21 1.535(12) . ? C20 H20 0.9900 . ? C21 N16 1.478(11) . ? C21 N14 1.489(11) . ? C21 H21 0.9900 . ? C22 O10 1.240(10) . ? C22 N16 1.378(11) . ? C22 N15 1.379(11) . ? C23 N14 1.463(10) . ? C23 N17 1.465(10) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N16 1.435(11) . ? C24 N19 1.483(10) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O8 1.221(10) . ? C25 N17 1.409(11) . ? C25 N18 1.416(11) . ? C26 N19 1.418(10) . ? C26 N17 1.470(10) . ? C26 C27 1.570(12) . ? C26 H26 0.9900 . ? C27 N18 1.443(10) . ? C27 N20 1.467(11) . ? C27 H27 0.9900 . ? C28 O11 1.267(11) . ? C28 N19 1.363(11) . ? C28 N20 1.394(11) . ? C29 N18 1.454(10) . ? C29 N21 1.460(10) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N23 1.429(11) . ? C30 N20 1.459(10) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O9 1.199(10) . ? C31 N22 1.380(11) . ? C31 N21 1.401(11) . ? C32 N21 1.461(10) . ? C32 N23 1.483(11) . ? C32 C33 1.542(11) . ? C32 H32 0.9900 . ? C33 N22 1.458(10) . ? C33 N24 1.466(10) . ? C33 H33 0.9900 . ? C34 O12 1.281(10) . ? C34 N23 1.355(10) . ? C34 N24 1.361(10) . ? C35 N22 1.445(10) 2_756 ? C35 N15 1.467(11) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N13 1.416(11) . ? C36 N24 1.458(10) 2_756 ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? N1 C18 1.452(10) 2_657 ? N3 C17 1.445(10) 2_657 ? N22 C35 1.445(10) 2_756 ? N24 C36 1.458(10) 2_756 ? 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 O8 Ho2 O7 76.8(2) . . ? O8 Ho2 O1 151.8(2) . . ? O7 Ho2 O1 87.60(19) . . ? O8 Ho2 O1W 72.4(2) . . ? O7 Ho2 O1W 136.50(19) . . ? O1 Ho2 O1W 105.7(2) . . ? O8 Ho2 O3W 70.7(2) . . ? O7 Ho2 O3W 105.1(2) . . ? O1 Ho2 O3W 136.9(2) . . ? O1W Ho2 O3W 93.1(2) . . ? O8 Ho2 O2 125.9(2) . . ? O7 Ho2 O2 151.62(19) . . ? O1 Ho2 O2 77.3(2) . . ? O1W Ho2 O2 71.4(2) . . ? O3W Ho2 O2 72.5(2) . . ? O8 Ho2 O2W 123.4(2) . . ? O7 Ho2 O2W 72.7(2) . . ? O1 Ho2 O2W 72.2(2) . . ? O1W Ho2 O2W 150.8(2) . . ? O3W Ho2 O2W 72.8(2) . . ? O2 Ho2 O2W 79.8(2) . . ? O8 Ho2 O4W 80.9(2) . . ? O7 Ho2 O4W 73.1(2) . . ? O1 Ho2 O4W 72.1(2) . . ? O1W Ho2 O4W 72.3(2) . . ? O3W Ho2 O4W 151.0(2) . . ? O2 Ho2 O4W 122.9(2) . . ? O2W Ho2 O4W 130.7(2) . . ? O8 Ho2 O5W 117.3(3) . 2_657 ? O7 Ho2 O5W 43.9(3) . 2_657 ? O1 Ho2 O5W 43.7(3) . 2_657 ? O1W Ho2 O5W 134.3(4) . 2_657 ? O3W Ho2 O5W 132.6(4) . 2_657 ? O2 Ho2 O5W 116.8(3) . 2_657 ? O2W Ho2 O5W 64.5(4) . 2_657 ? O4W Ho2 O5W 66.2(4) . 2_657 ? Cl4 Zn1 Cl1 108.9(2) . . ? Cl4 Zn1 Cl3 109.0(2) . . ? Cl1 Zn1 Cl3 108.80(17) . . ? Cl4 Zn1 Cl2 111.7(3) . . ? Cl1 Zn1 Cl2 111.00(16) . . ? Cl3 Zn1 Cl2 107.33(16) . . ? O1 C1 N2 125.2(8) . . ? O1 C1 N1 125.9(9) . . ? N2 C1 N1 108.6(8) . . ? N3 C2 N1 115.1(7) . . ? N3 C2 C3 101.9(7) . . ? N1 C2 C3 104.4(6) . . ? N3 C2 H2 111.6 . . ? N1 C2 H2 111.6 . . ? C3 C2 H2 111.6 . . ? N4 C3 N2 115.0(7) . . ? N4 C3 C2 105.3(7) . . ? N2 C3 C2 102.6(6) . . ? N4 C3 H3 111.2 . . ? N2 C3 H3 111.2 . . ? C2 C3 H3 111.2 . . ? O4 C4 N4 124.9(10) . . ? O4 C4 N3 124.9(9) . . ? N4 C4 N3 110.0(8) . . ? N2 C5 N5 112.6(7) . . ? N2 C5 H5A 109.1 . . ? N5 C5 H5A 109.1 . . ? N2 C5 H5B 109.1 . . ? N5 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? N4 C6 N7 115.6(8) . . ? N4 C6 H6A 108.4 . . ? N7 C6 H6A 108.4 . . ? N4 C6 H6B 108.4 . . ? N7 C6 H6B 108.4 . . ? H6A C6 H6B 107.4 . . ? O2 C7 N5 128.6(8) . . ? O2 C7 N6 123.4(8) . . ? N5 C7 N6 108.0(7) . . ? N7 C8 N5 114.7(7) . . ? N7 C8 C9 103.8(7) . . ? N5 C8 C9 102.7(6) . . ? N7 C8 H8 111.7 . . ? N5 C8 H8 111.7 . . ? C9 C8 H8 111.7 . . ? N8 C9 N6 114.0(7) . . ? N8 C9 C8 102.4(7) . . ? N6 C9 C8 104.1(6) . . ? N8 C9 H9 111.9 . . ? N6 C9 H9 111.9 . . ? C8 C9 H9 111.9 . . ? O5 C10 N7 129.0(10) . . ? O5 C10 N8 125.2(10) . . ? N7 C10 N8 105.7(9) . . ? N9 C11 N6 115.6(7) . . ? N9 C11 H11A 108.4 . . ? N6 C11 H11A 108.4 . . ? N9 C11 H11B 108.4 . . ? N6 C11 H11B 108.4 . . ? H11A C11 H11B 107.4 . . ? N11 C12 N8 113.3(7) . . ? N11 C12 H12A 108.9 . . ? N8 C12 H12A 108.9 . . ? N11 C12 H12B 108.9 . . ? N8 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N10 127.7(9) . . ? O3 C13 N9 124.1(8) . . ? N10 C13 N9 108.2(8) . . ? N9 C14 N11 115.1(7) . . ? N9 C14 C15 103.0(7) . . ? N11 C14 C15 102.9(6) . . ? N9 C14 H14 111.7 . . ? N11 C14 H14 111.7 . . ? C15 C14 H14 111.7 . . ? N12 C15 N10 115.6(7) . . ? N12 C15 C14 103.7(6) . . ? N10 C15 C14 102.3(6) . . ? N12 C15 H15 111.5 . . ? N10 C15 H15 111.5 . . ? C14 C15 H15 111.5 . . ? O6 C16 N12 124.9(8) . . ? O6 C16 N11 127.1(8) . . ? N12 C16 N11 108.0(8) . . ? N10 C17 N3 116.3(7) . 2_657 ? N10 C17 H17A 108.2 . . ? N3 C17 H17A 108.2 2_657 . ? N10 C17 H17B 108.2 . . ? N3 C17 H17B 108.2 2_657 . ? H17A C17 H17B 107.4 . . ? N12 C18 N1 115.0(7) . 2_657 ? N12 C18 H18A 108.5 . . ? N1 C18 H18A 108.5 2_657 . ? N12 C18 H18B 108.5 . . ? N1 C18 H18B 108.5 2_657 . ? H18A C18 H18B 107.5 . . ? O7 C19 N14 125.2(9) . . ? O7 C19 N13 126.1(8) . . ? N14 C19 N13 108.8(8) . . ? N13 C20 N15 114.8(7) . . ? N13 C20 C21 106.5(7) . . ? N15 C20 C21 102.9(7) . . ? N13 C20 H20 110.7 . . ? N15 C20 H20 110.7 . . ? C21 C20 H20 110.7 . . ? N16 C21 N14 114.8(7) . . ? N16 C21 C20 104.5(7) . . ? N14 C21 C20 101.6(7) . . ? N16 C21 H21 111.8 . . ? N14 C21 H21 111.8 . . ? C20 C21 H21 111.8 . . ? O10 C22 N16 125.9(9) . . ? O10 C22 N15 125.1(9) . . ? N16 C22 N15 108.8(8) . . ? N14 C23 N17 112.7(7) . . ? N14 C23 H23A 109.0 . . ? N17 C23 H23A 109.0 . . ? N14 C23 H23B 109.0 . . ? N17 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? N16 C24 N19 114.6(7) . . ? N16 C24 H24A 108.6 . . ? N19 C24 H24A 108.6 . . ? N16 C24 H24B 108.6 . . ? N19 C24 H24B 108.6 . . ? H24A C24 H24B 107.6 . . ? O8 C25 N17 127.1(8) . . ? O8 C25 N18 126.4(9) . . ? N17 C25 N18 106.3(8) . . ? N19 C26 N17 114.0(7) . . ? N19 C26 C27 104.7(7) . . ? N17 C26 C27 103.2(7) . . ? N19 C26 H26 111.5 . . ? N17 C26 H26 111.5 . . ? C27 C26 H26 111.5 . . ? N18 C27 N20 113.0(7) . . ? N18 C27 C26 104.0(6) . . ? N20 C27 C26 101.5(7) . . ? N18 C27 H27 112.5 . . ? N20 C27 H27 112.5 . . ? C26 C27 H27 112.5 . . ? O11 C28 N19 128.3(9) . . ? O11 C28 N20 124.1(9) . . ? N19 C28 N20 107.5(9) . . ? N18 C29 N21 113.7(6) . . ? N18 C29 H29A 108.8 . . ? N21 C29 H29A 108.8 . . ? N18 C29 H29B 108.8 . . ? N21 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? N23 C30 N20 114.5(7) . . ? N23 C30 H30A 108.6 . . ? N20 C30 H30A 108.6 . . ? N23 C30 H30B 108.6 . . ? N20 C30 H30B 108.6 . . ? H30A C30 H30B 107.6 . . ? O9 C31 N22 128.6(9) . . ? O9 C31 N21 124.5(8) . . ? N22 C31 N21 106.9(8) . . ? N21 C32 N23 115.1(7) . . ? N21 C32 C33 102.9(7) . . ? N23 C32 C33 102.9(7) . . ? N21 C32 H32 111.8 . . ? N23 C32 H32 111.8 . . ? C33 C32 H32 111.8 . . ? N22 C33 N24 116.0(7) . . ? N22 C33 C32 104.5(7) . . ? N24 C33 C32 104.6(7) . . ? N22 C33 H33 110.4 . . ? N24 C33 H33 110.4 . . ? C32 C33 H33 110.4 . . ? O12 C34 N23 124.5(8) . . ? O12 C34 N24 124.1(8) . . ? N23 C34 N24 111.4(8) . . ? N22 C35 N15 115.2(7) 2_756 . ? N22 C35 H35A 108.5 2_756 . ? N15 C35 H35A 108.5 . . ? N22 C35 H35B 108.5 2_756 . ? N15 C35 H35B 108.5 . . ? H35A C35 H35B 107.5 . . ? N13 C36 N24 114.4(7) . 2_756 ? N13 C36 H36A 108.7 . . ? N24 C36 H36A 108.7 2_756 . ? N13 C36 H36B 108.7 . . ? N24 C36 H36B 108.7 2_756 . ? H36A C36 H36B 107.6 . . ? C1 N1 C18 121.8(8) . 2_657 ? C1 N1 C2 111.8(7) . . ? C18 N1 C2 125.4(7) 2_657 . ? C1 N2 C5 123.7(8) . . ? C1 N2 C3 112.3(7) . . ? C5 N2 C3 123.9(7) . . ? C4 N3 C17 122.1(8) . 2_657 ? C4 N3 C2 112.6(7) . . ? C17 N3 C2 125.2(7) 2_657 . ? C4 N4 C6 124.6(8) . . ? C4 N4 C3 110.0(7) . . ? C6 N4 C3 124.8(7) . . ? C7 N5 C5 121.7(8) . . ? C7 N5 C8 113.1(7) . . ? C5 N5 C8 124.9(7) . . ? C7 N6 C11 121.8(7) . . ? C7 N6 C9 112.1(7) . . ? C11 N6 C9 124.1(7) . . ? C10 N7 C8 114.1(8) . . ? C10 N7 C6 121.9(8) . . ? C8 N7 C6 123.9(7) . . ? C10 N8 C9 114.0(8) . . ? C10 N8 C12 121.9(8) . . ? C9 N8 C12 123.3(8) . . ? C13 N9 C11 123.3(7) . . ? C13 N9 C14 113.3(7) . . ? C11 N9 C14 122.7(7) . . ? C13 N10 C17 123.4(8) . . ? C13 N10 C15 113.1(7) . . ? C17 N10 C15 122.1(7) . . ? C16 N11 C12 121.4(7) . . ? C16 N11 C14 112.5(7) . . ? C12 N11 C14 123.2(7) . . ? C16 N12 C18 122.3(7) . . ? C16 N12 C15 112.7(7) . . ? C18 N12 C15 124.1(7) . . ? C19 N13 C36 120.6(8) . . ? C19 N13 C20 110.1(7) . . ? C36 N13 C20 126.0(7) . . ? C19 N14 C23 123.4(8) . . ? C19 N14 C21 112.7(7) . . ? C23 N14 C21 123.8(7) . . ? C22 N15 C35 123.2(8) . . ? C22 N15 C20 112.0(7) . . ? C35 N15 C20 124.7(7) . . ? C22 N16 C24 123.9(8) . . ? C22 N16 C21 111.3(8) . . ? C24 N16 C21 124.5(8) . . ? C25 N17 C23 120.4(7) . . ? C25 N17 C26 112.6(7) . . ? C23 N17 C26 126.9(7) . . ? C25 N18 C27 113.3(7) . . ? C25 N18 C29 119.7(8) . . ? C27 N18 C29 125.0(7) . . ? C28 N19 C26 113.6(8) . . ? C28 N19 C24 121.7(8) . . ? C26 N19 C24 124.1(7) . . ? C28 N20 C30 123.8(8) . . ? C28 N20 C27 112.5(8) . . ? C30 N20 C27 123.0(7) . . ? C31 N21 C29 122.8(7) . . ? C31 N21 C32 113.0(7) . . ? C29 N21 C32 123.0(7) . . ? C31 N22 C35 121.3(7) . 2_756 ? C31 N22 C33 112.6(7) . . ? C35 N22 C33 124.6(7) 2_756 . ? C34 N23 C30 124.0(8) . . ? C34 N23 C32 110.8(7) . . ? C30 N23 C32 123.7(8) . . ? C34 N24 C36 124.5(7) . 2_756 ? C34 N24 C33 110.3(7) . . ? C36 N24 C33 124.8(7) 2_756 . ? C1 O1 Ho2 155.4(6) . . ? C7 O2 Ho2 154.8(6) . . ? C19 O7 Ho2 156.4(6) . . ? C25 O8 Ho2 157.1(6) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.321 _refine_diff_density_min -1.839 _refine_diff_density_rms 0.133 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 104 35 ' ' 2 -0.060 0.500 0.756 1165 461 ' ' 3 0.500 1.000 0.000 103 35 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 902622' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p312 #TrackingRef 'submit-312.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H92 Cl5 Er N24 O40 Zn' _chemical_formula_weight 1911.22 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 '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 15.142(2) _cell_length_b 15.540(2) _cell_length_c 16.992(2) _cell_angle_alpha 63.894(5) _cell_angle_beta 80.645(5) _cell_angle_gamma 81.604(5) _cell_volume 3530.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.798 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1958 _exptl_absorpt_coefficient_mu 1.824 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6485 _exptl_absorpt_correction_T_max 0.7006 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36305 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.0633 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12259 _reflns_number_gt 10017 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0953P)^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 12259 _refine_ls_number_parameters 748 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1484 _refine_ls_wR_factor_gt 0.1420 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 Cl5 Cl -0.01118(13) 0.79640(17) 0.55089(15) 0.0827(6) Uani 1 1 d . . . O1W O 0.0677(2) 1.1355(3) 0.6400(3) 0.0479(10) Uani 1 1 d . . . O2W O 0.2606(3) 1.2411(3) 0.6073(3) 0.0500(10) Uani 1 1 d . . . O3W O 0.1062(3) 0.9856(3) 0.8012(3) 0.0519(10) Uani 1 1 d . . . O4W O 0.3675(2) 1.0682(3) 0.6622(3) 0.0515(10) Uani 1 1 d . . . Er1 Er 0.209295(14) 1.088299(18) 0.690808(15) 0.03530(11) Uani 1 1 d . . . Cl1 Cl 0.48715(12) 0.75705(17) 1.15429(19) 0.0932(7) Uani 1 1 d . . . Cl2 Cl 0.64017(13) 0.54737(18) 1.1631(2) 0.1195(11) Uani 1 1 d . . . Cl3 Cl 0.39054(14) 0.53962(16) 1.1911(2) 0.1130(10) Uani 1 1 d . . . Cl4 Cl 0.5122(4) 0.6823(4) 0.9758(2) 0.227(3) Uani 1 1 d . . . Zn1 Zn 0.50699(6) 0.62928(6) 1.12063(6) 0.0728(3) Uani 1 1 d . . . C1 C 0.1289(3) 1.2450(4) 0.7868(3) 0.0378(12) Uani 1 1 d . . . C2 C 0.0633(4) 1.3514(4) 0.8470(4) 0.0416(13) Uani 1 1 d . . . H2 H 0.0528 1.4217 0.8121 0.050 Uiso 1 1 calc R . . C3 C 0.1618(4) 1.3209(4) 0.8698(4) 0.0383(12) Uani 1 1 d . . . H3 H 0.1971 1.3773 0.8486 0.046 Uiso 1 1 calc R . . C4 C 0.0656(4) 1.2731(4) 1.0001(4) 0.0470(14) Uani 1 1 d . . . C5 C 0.2843(3) 1.2169(4) 0.8214(3) 0.0388(12) Uani 1 1 d . . . H5A H 0.3254 1.2590 0.8233 0.047 Uiso 1 1 calc R . . H5B H 0.2995 1.2124 0.7650 0.047 Uiso 1 1 calc R . . C6 C 0.2268(4) 1.2338(5) 1.0156(4) 0.0488(14) Uani 1 1 d . . . H6A H 0.2085 1.2374 1.0721 0.059 Uiso 1 1 calc R . . H6B H 0.2762 1.2750 0.9851 0.059 Uiso 1 1 calc R . . C7 C 0.2888(3) 1.0406(4) 0.8880(3) 0.0342(11) Uani 1 1 d . . . C8 C 0.3270(3) 1.1050(4) 0.9766(3) 0.0375(12) Uani 1 1 d . . . H8 H 0.3850 1.1315 0.9688 0.045 Uiso 1 1 calc R . . C9 C 0.3348(3) 0.9956(4) 1.0254(3) 0.0384(12) Uani 1 1 d . . . H9 H 0.3973 0.9700 1.0380 0.046 Uiso 1 1 calc R . . C10 C 0.2342(4) 1.0584(4) 1.1098(4) 0.0398(13) Uani 1 1 d . . . C11 C 0.3194(3) 0.8687(4) 0.9731(4) 0.0427(13) Uani 1 1 d . . . H11A H 0.3767 0.8394 0.9969 0.051 Uiso 1 1 calc R . . H11B H 0.3237 0.8705 0.9143 0.051 Uiso 1 1 calc R . . C12 C 0.2674(4) 0.8848(4) 1.1785(3) 0.0411(13) Uani 1 1 d . . . H12A H 0.2436 0.8934 1.2319 0.049 Uiso 1 1 calc R . . H12B H 0.3275 0.8513 1.1873 0.049 Uiso 1 1 calc R . . C13 C 0.1883(3) 0.7804(4) 0.9957(4) 0.0379(12) Uani 1 1 d . . . C14 C 0.2425(3) 0.7629(4) 1.1246(3) 0.0377(12) Uani 1 1 d . . . H14 H 0.2993 0.7253 1.1455 0.045 Uiso 1 1 calc R . . C15 C 0.1650(3) 0.6971(4) 1.1495(4) 0.0391(12) Uani 1 1 d . . . H15 H 0.1854 0.6287 1.1836 0.047 Uiso 1 1 calc R . . C16 C 0.1281(3) 0.8042(4) 1.2152(3) 0.0379(12) Uani 1 1 d . . . C17 C 0.0812(4) 0.6554(5) 1.0533(4) 0.0475(14) Uani 1 1 d . . . H17A H 0.0953 0.6605 0.9931 0.057 Uiso 1 1 calc R . . H17B H 0.0946 0.5881 1.0939 0.057 Uiso 1 1 calc R . . C18 C 0.0221(3) 0.6830(4) 1.2533(3) 0.0375(12) Uani 1 1 d . . . H18A H 0.0022 0.7019 1.3017 0.045 Uiso 1 1 calc R . . H18B H 0.0393 0.6136 1.2794 0.045 Uiso 1 1 calc R . . C19 C 0.2156(3) 1.0967(4) 0.4812(3) 0.0354(12) Uani 1 1 d . . . C20 C 0.2229(3) 1.1156(4) 0.3369(3) 0.0399(13) Uani 1 1 d . . . H20 H 0.1814 1.1601 0.2943 0.048 Uiso 1 1 calc R . . C21 C 0.1808(3) 1.0208(4) 0.4008(3) 0.0406(13) Uani 1 1 d . . . H21 H 0.1193 1.0202 0.3884 0.049 Uiso 1 1 calc R . . C22 C 0.3124(4) 0.9872(5) 0.3208(4) 0.0436(14) Uani 1 1 d . . . C23 C 0.1405(3) 0.9484(4) 0.5689(3) 0.0400(12) Uani 1 1 d . . . H23A H 0.1147 0.9801 0.6072 0.048 Uiso 1 1 calc R . . H23B H 0.0913 0.9236 0.5563 0.048 Uiso 1 1 calc R . . C24 C 0.2323(4) 0.8474(5) 0.4306(4) 0.0504(15) Uani 1 1 d . . . H24A H 0.2604 0.8167 0.3921 0.060 Uiso 1 1 calc R . . H24B H 0.1682 0.8374 0.4423 0.060 Uiso 1 1 calc R . . C25 C 0.2509(3) 0.8699(4) 0.6748(3) 0.0396(13) Uani 1 1 d . . . C26 C 0.2213(4) 0.7847(4) 0.5992(4) 0.0433(13) Uani 1 1 d . . . H26 H 0.1674 0.7501 0.6104 0.052 Uiso 1 1 calc R . . C27 C 0.2907(4) 0.7249(4) 0.6646(4) 0.0405(13) Uani 1 1 d . . . H27 H 0.2679 0.6636 0.7095 0.049 Uiso 1 1 calc R . . C28 C 0.3533(4) 0.7505(5) 0.5219(4) 0.0468(14) Uani 1 1 d . . . C29 C 0.3526(3) 0.7570(4) 0.7802(3) 0.0402(12) Uani 1 1 d . . . H29A H 0.3287 0.7960 0.8125 0.048 Uiso 1 1 calc R . . H29B H 0.3416 0.6900 0.8196 0.048 Uiso 1 1 calc R . . C30 C 0.4467(4) 0.6475(4) 0.6394(4) 0.0424(13) Uani 1 1 d . . . H30A H 0.4756 0.6259 0.5945 0.051 Uiso 1 1 calc R . . H30B H 0.4281 0.5904 0.6922 0.051 Uiso 1 1 calc R . . C31 C 0.4895(3) 0.8304(4) 0.7671(3) 0.0385(12) Uani 1 1 d . . . C32 C 0.5086(3) 0.6902(4) 0.7464(3) 0.0393(12) Uani 1 1 d . . . H32 H 0.4983 0.6259 0.7948 0.047 Uiso 1 1 calc R . . C33 C 0.6020(3) 0.7208(4) 0.7451(3) 0.0407(12) Uani 1 1 d . . . H33 H 0.6351 0.6710 0.7931 0.049 Uiso 1 1 calc R . . C34 C 0.5917(4) 0.7127(4) 0.6119(4) 0.0426(13) Uani 1 1 d . . . C35 C 0.6453(4) 0.8504(5) 0.7809(4) 0.0481(14) Uani 1 1 d . . . H35A H 0.6132 0.8852 0.8145 0.058 Uiso 1 1 calc R . . H35B H 0.6855 0.7990 0.8191 0.058 Uiso 1 1 calc R . . C36 C 0.2609(3) 1.2508(4) 0.3673(4) 0.0433(13) Uani 1 1 d . . . H36A H 0.2401 1.2701 0.4154 0.052 Uiso 1 1 calc R . . H36B H 0.2265 1.2922 0.3178 0.052 Uiso 1 1 calc R . . N1 N 0.0530(3) 1.2980(3) 0.7976(3) 0.0377(10) Uani 1 1 d . . . N2 N 0.1954(3) 1.2599(3) 0.8245(3) 0.0383(10) Uani 1 1 d . . . N3 N 0.0131(3) 1.3192(4) 0.9324(3) 0.0446(11) Uani 1 1 d . . . N4 N 0.1528(3) 1.2707(4) 0.9639(3) 0.0458(11) Uani 1 1 d . . . N5 N 0.2987(3) 1.1231(3) 0.8913(3) 0.0388(10) Uani 1 1 d . . . N6 N 0.3056(3) 0.9646(3) 0.9654(3) 0.0385(10) Uani 1 1 d . . . N7 N 0.2597(3) 1.1354(4) 1.0326(3) 0.0450(11) Uani 1 1 d . . . N8 N 0.2751(3) 0.9773(4) 1.1062(3) 0.0402(11) Uani 1 1 d . . . N9 N 0.2483(3) 0.8087(3) 1.0297(3) 0.0402(10) Uani 1 1 d . . . N10 N 0.1391(3) 0.7135(4) 1.0653(3) 0.0434(11) Uani 1 1 d . . . N11 N 0.2103(3) 0.8243(4) 1.1677(3) 0.0406(10) Uani 1 1 d . . . N12 N 0.1000(3) 0.7326(4) 1.2025(3) 0.0422(11) Uani 1 1 d . . . N13 N 0.2415(3) 1.1546(3) 0.3959(3) 0.0382(10) Uani 1 1 d . . . N14 N 0.1810(3) 1.0190(4) 0.4870(3) 0.0423(11) Uani 1 1 d . . . N15 N 0.3021(3) 1.0850(4) 0.2940(3) 0.0418(11) Uani 1 1 d . . . N16 N 0.2421(3) 0.9483(4) 0.3851(3) 0.0462(12) Uani 1 1 d . . . N17 N 0.2003(3) 0.8715(3) 0.6141(3) 0.0400(10) Uani 1 1 d . . . N18 N 0.3035(3) 0.7882(3) 0.7040(3) 0.0384(10) Uani 1 1 d . . . N19 N 0.2721(3) 0.8002(4) 0.5141(3) 0.0471(12) Uani 1 1 d . . . N20 N 0.3688(3) 0.7087(4) 0.6080(3) 0.0454(11) Uani 1 1 d . . . N21 N 0.4469(3) 0.7639(3) 0.7594(3) 0.0396(10) Uani 1 1 d . . . N22 N 0.5801(3) 0.8073(4) 0.7570(3) 0.0415(11) Uani 1 1 d . . . N23 N 0.5117(3) 0.6896(4) 0.6607(3) 0.0424(11) Uani 1 1 d . . . N24 N 0.6457(3) 0.7320(3) 0.6599(3) 0.0414(10) Uani 1 1 d . . . O1 O 0.1371(2) 1.1915(3) 0.7490(2) 0.0417(9) Uani 1 1 d . . . O2 O 0.2689(2) 1.0333(3) 0.8238(2) 0.0450(9) Uani 1 1 d . . . O3 O 0.1827(3) 0.8046(3) 0.9184(3) 0.0504(10) Uani 1 1 d . . . O4 O 0.0399(3) 1.2453(4) 1.0775(3) 0.0605(12) Uani 1 1 d . . . O5 O 0.1852(3) 1.0639(3) 1.1726(3) 0.0492(10) Uani 1 1 d . . . O6 O 0.0893(2) 0.8418(3) 1.2618(3) 0.0492(10) Uani 1 1 d . . . O7 O 0.2224(2) 1.1143(3) 0.5447(2) 0.0415(9) Uani 1 1 d . . . O8 O 0.2459(2) 0.9348(3) 0.6990(2) 0.0430(9) Uani 1 1 d . . . O9 O 0.4524(2) 0.8988(3) 0.7823(3) 0.0445(9) Uani 1 1 d . . . O10 O 0.3703(3) 0.9443(4) 0.2920(3) 0.0565(11) Uani 1 1 d . . . O11 O 0.4051(3) 0.7414(4) 0.4627(3) 0.0712(14) Uani 1 1 d . . . O12 O 0.6151(3) 0.7116(3) 0.5403(3) 0.0539(11) 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 Cl5 0.0635(10) 0.0867(15) 0.0949(15) -0.0326(12) -0.0224(10) -0.0024(10) O1W 0.0398(19) 0.069(3) 0.039(2) -0.030(2) -0.0013(16) 0.0032(18) O2W 0.057(2) 0.048(3) 0.042(2) -0.020(2) 0.0066(18) -0.0036(19) O3W 0.048(2) 0.056(3) 0.047(2) -0.021(2) 0.0100(18) -0.0103(19) O4W 0.043(2) 0.061(3) 0.042(2) -0.018(2) 0.0053(17) -0.0023(19) Er1 0.03497(14) 0.04452(17) 0.02903(15) -0.02043(12) 0.00080(9) -0.00033(10) Cl1 0.0529(10) 0.0840(15) 0.144(2) -0.0489(15) -0.0106(11) -0.0105(9) Cl2 0.0512(10) 0.0761(15) 0.149(2) 0.0197(14) 0.0055(12) -0.0013(10) Cl3 0.0611(11) 0.0546(13) 0.199(3) -0.0370(15) -0.0021(14) -0.0037(9) Cl4 0.313(6) 0.217(5) 0.0622(18) -0.021(2) -0.023(3) 0.118(5) Zn1 0.0616(5) 0.0561(5) 0.0685(6) -0.0028(4) 0.0008(4) 0.0041(4) C1 0.035(3) 0.040(3) 0.031(3) -0.009(2) 0.001(2) -0.008(2) C2 0.050(3) 0.037(3) 0.040(3) -0.022(3) 0.005(2) -0.009(2) C3 0.049(3) 0.028(3) 0.037(3) -0.013(2) -0.003(2) -0.004(2) C4 0.059(3) 0.037(3) 0.051(4) -0.027(3) 0.001(3) -0.006(3) C5 0.036(3) 0.047(3) 0.030(3) -0.014(3) 0.003(2) -0.009(2) C6 0.063(3) 0.052(4) 0.043(3) -0.030(3) -0.010(3) -0.002(3) C7 0.027(2) 0.048(3) 0.028(3) -0.017(2) -0.002(2) -0.001(2) C8 0.032(2) 0.050(3) 0.032(3) -0.018(3) -0.006(2) -0.005(2) C9 0.028(2) 0.056(4) 0.032(3) -0.018(3) -0.003(2) -0.006(2) C10 0.045(3) 0.044(3) 0.035(3) -0.018(3) -0.011(2) -0.007(2) C11 0.038(3) 0.049(4) 0.040(3) -0.024(3) 0.011(2) -0.002(2) C12 0.044(3) 0.054(4) 0.030(3) -0.021(3) -0.007(2) -0.005(3) C13 0.043(3) 0.037(3) 0.035(3) -0.021(3) 0.004(2) 0.001(2) C14 0.036(3) 0.043(3) 0.031(3) -0.017(2) 0.000(2) 0.001(2) C15 0.043(3) 0.033(3) 0.037(3) -0.013(2) -0.006(2) 0.006(2) C16 0.038(3) 0.042(3) 0.031(3) -0.015(3) -0.003(2) 0.003(2) C17 0.053(3) 0.051(4) 0.051(4) -0.038(3) 0.003(3) 0.001(3) C18 0.040(3) 0.042(3) 0.029(3) -0.014(2) 0.003(2) -0.009(2) C19 0.027(2) 0.048(3) 0.028(3) -0.016(2) 0.001(2) 0.000(2) C20 0.033(2) 0.058(4) 0.028(3) -0.019(3) -0.008(2) 0.000(2) C21 0.034(3) 0.062(4) 0.030(3) -0.022(3) -0.005(2) -0.009(2) C22 0.040(3) 0.068(4) 0.031(3) -0.028(3) -0.003(2) -0.009(3) C23 0.035(3) 0.053(4) 0.034(3) -0.022(3) 0.001(2) -0.005(2) C24 0.057(3) 0.064(4) 0.042(3) -0.034(3) -0.001(3) -0.011(3) C25 0.037(3) 0.052(4) 0.027(3) -0.016(3) 0.009(2) -0.011(3) C26 0.041(3) 0.051(4) 0.044(3) -0.027(3) 0.004(2) -0.006(2) C27 0.047(3) 0.039(3) 0.039(3) -0.022(3) 0.012(2) -0.016(2) C28 0.051(3) 0.055(4) 0.041(3) -0.030(3) 0.007(3) -0.007(3) C29 0.040(3) 0.048(3) 0.030(3) -0.017(3) 0.006(2) -0.007(2) C30 0.046(3) 0.043(3) 0.038(3) -0.020(3) 0.005(2) -0.003(2) C31 0.043(3) 0.049(4) 0.020(2) -0.013(2) 0.002(2) -0.003(2) C32 0.044(3) 0.036(3) 0.029(3) -0.008(2) 0.001(2) 0.000(2) C33 0.041(3) 0.042(3) 0.029(3) -0.008(2) -0.004(2) 0.002(2) C34 0.048(3) 0.037(3) 0.040(3) -0.016(3) -0.001(3) -0.001(2) C35 0.049(3) 0.071(4) 0.029(3) -0.026(3) -0.003(2) -0.007(3) C36 0.035(3) 0.055(4) 0.036(3) -0.021(3) -0.002(2) 0.011(2) N1 0.041(2) 0.039(3) 0.036(2) -0.020(2) -0.0050(19) 0.0034(19) N2 0.038(2) 0.044(3) 0.037(2) -0.022(2) 0.0019(19) -0.0047(19) N3 0.047(2) 0.055(3) 0.037(3) -0.025(2) 0.003(2) -0.009(2) N4 0.049(3) 0.052(3) 0.041(3) -0.025(2) 0.000(2) -0.005(2) N5 0.043(2) 0.047(3) 0.027(2) -0.017(2) 0.0007(19) -0.008(2) N6 0.042(2) 0.043(3) 0.034(2) -0.020(2) 0.0012(19) -0.008(2) N7 0.051(3) 0.050(3) 0.037(3) -0.022(2) -0.002(2) -0.006(2) N8 0.042(2) 0.051(3) 0.033(2) -0.025(2) 0.0002(19) -0.005(2) N9 0.041(2) 0.050(3) 0.031(2) -0.019(2) 0.0015(19) -0.007(2) N10 0.046(2) 0.054(3) 0.035(2) -0.025(2) 0.005(2) -0.010(2) N11 0.038(2) 0.051(3) 0.036(2) -0.024(2) 0.0031(19) -0.006(2) N12 0.039(2) 0.049(3) 0.042(3) -0.026(2) 0.004(2) -0.003(2) N13 0.037(2) 0.047(3) 0.033(2) -0.021(2) 0.0001(18) -0.0008(19) N14 0.042(2) 0.057(3) 0.030(2) -0.023(2) 0.0032(19) -0.002(2) N15 0.039(2) 0.056(3) 0.034(2) -0.024(2) 0.0026(19) -0.006(2) N16 0.044(2) 0.060(3) 0.045(3) -0.033(3) 0.001(2) -0.009(2) N17 0.043(2) 0.045(3) 0.035(2) -0.020(2) -0.001(2) -0.006(2) N18 0.037(2) 0.043(3) 0.032(2) -0.016(2) 0.0009(19) -0.002(2) N19 0.049(3) 0.056(3) 0.036(3) -0.021(2) -0.004(2) 0.000(2) N20 0.044(2) 0.053(3) 0.046(3) -0.030(3) 0.005(2) -0.006(2) N21 0.041(2) 0.040(3) 0.037(2) -0.017(2) -0.0026(19) -0.001(2) N22 0.039(2) 0.051(3) 0.035(2) -0.019(2) -0.0043(19) -0.005(2) N23 0.044(2) 0.049(3) 0.037(3) -0.024(2) 0.008(2) -0.006(2) N24 0.044(2) 0.047(3) 0.032(2) -0.019(2) 0.0053(19) -0.006(2) O1 0.0414(19) 0.053(2) 0.041(2) -0.034(2) 0.0018(16) 0.0018(17) O2 0.051(2) 0.053(3) 0.035(2) -0.0242(19) -0.0053(17) 0.0039(18) O3 0.058(2) 0.057(3) 0.041(2) -0.026(2) -0.0016(19) -0.004(2) O4 0.070(3) 0.072(3) 0.039(3) -0.028(2) 0.006(2) -0.001(2) O5 0.048(2) 0.065(3) 0.040(2) -0.029(2) 0.0002(18) -0.0012(19) O6 0.046(2) 0.061(3) 0.046(2) -0.032(2) 0.0053(18) -0.0006(19) O7 0.047(2) 0.053(2) 0.0274(19) -0.0206(18) -0.0019(16) -0.0013(17) O8 0.055(2) 0.042(2) 0.039(2) -0.0244(19) -0.0028(17) -0.0029(17) O9 0.049(2) 0.048(2) 0.043(2) -0.026(2) -0.0044(17) -0.0011(18) O10 0.048(2) 0.076(3) 0.059(3) -0.045(3) 0.005(2) -0.005(2) O11 0.067(3) 0.097(4) 0.049(3) -0.039(3) 0.009(2) 0.002(3) O12 0.054(2) 0.073(3) 0.042(2) -0.034(2) 0.0090(19) -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 O1W Er1 2.338(4) . ? O2W Er1 2.339(4) . ? O3W Er1 2.376(4) . ? O4W Er1 2.368(4) . ? Er1 O1 2.297(3) . ? Er1 O7 2.312(3) . ? Er1 O8 2.316(4) . ? Er1 O2 2.322(4) . ? Cl1 Zn1 2.265(3) . ? Cl2 Zn1 2.263(2) . ? Cl3 Zn1 2.246(2) . ? Cl4 Zn1 2.217(3) . ? C1 O1 1.238(6) . ? C1 N1 1.350(7) . ? C1 N2 1.372(6) . ? C2 N3 1.431(7) . ? C2 N1 1.452(7) . ? C2 C3 1.555(8) . ? C2 H2 0.9900 . ? C3 N4 1.431(7) . ? C3 N2 1.458(7) . ? C3 H3 0.9900 . ? C4 O4 1.204(7) . ? C4 N4 1.366(7) . ? C4 N3 1.369(8) . ? C5 N2 1.417(7) . ? C5 N5 1.432(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.429(7) . ? C6 N7 1.450(8) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.232(6) . ? C7 N5 1.338(7) . ? C7 N6 1.358(7) . ? C8 N7 1.452(7) . ? C8 N5 1.474(6) . ? C8 C9 1.524(8) . ? C8 H8 0.9900 . ? C9 N8 1.452(7) . ? C9 N6 1.452(6) . ? C9 H9 0.9900 . ? C10 O5 1.225(7) . ? C10 N8 1.342(7) . ? C10 N7 1.375(7) . ? C11 N6 1.425(7) . ? C11 N9 1.456(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.428(7) . ? C12 N11 1.451(7) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.210(6) . ? C13 N9 1.365(7) . ? C13 N10 1.376(7) . ? C14 N11 1.431(7) . ? C14 N9 1.441(7) . ? C14 C15 1.552(7) . ? C14 H14 0.9900 . ? C15 N12 1.441(7) . ? C15 N10 1.449(7) . ? C15 H15 0.9900 . ? C16 O6 1.213(6) . ? C16 N12 1.359(7) . ? C16 N11 1.364(7) . ? C17 N3 1.436(7) 2_577 ? C17 N10 1.440(7) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.442(7) . ? C18 N1 1.458(6) 2_577 ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O7 1.246(6) . ? C19 N14 1.344(7) . ? C19 N13 1.355(7) . ? C20 N15 1.432(7) . ? C20 N13 1.458(6) . ? C20 C21 1.548(8) . ? C20 H20 0.9900 . ? C21 N16 1.443(7) . ? C21 N14 1.453(6) . ? C21 H21 0.9900 . ? C22 O10 1.195(7) . ? C22 N15 1.374(8) . ? C22 N16 1.386(7) . ? C23 N17 1.393(7) . ? C23 N14 1.446(7) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N16 1.429(8) . ? C24 N19 1.465(8) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O8 1.235(7) . ? C25 N18 1.330(7) . ? C25 N17 1.371(7) . ? C26 N19 1.459(7) . ? C26 N17 1.459(7) . ? C26 C27 1.545(8) . ? C26 H26 0.9900 . ? C27 N18 1.461(7) . ? C27 N20 1.464(7) . ? C27 H27 0.9900 . ? C28 O11 1.218(7) . ? C28 N19 1.346(8) . ? C28 N20 1.360(8) . ? C29 N21 1.423(6) . ? C29 N18 1.456(7) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N20 1.418(7) . ? C30 N23 1.428(7) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O9 1.238(7) . ? C31 N21 1.357(7) . ? C31 N22 1.368(7) . ? C32 N21 1.440(7) . ? C32 N23 1.452(7) . ? C32 C33 1.551(7) . ? C32 H32 0.9900 . ? C33 N22 1.431(7) . ? C33 N24 1.436(7) . ? C33 H33 0.9900 . ? C34 O12 1.218(7) . ? C34 N23 1.351(7) . ? C34 N24 1.390(7) . ? C35 N15 1.428(7) 2_676 ? C35 N22 1.467(7) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N13 1.415(7) . ? C36 N24 1.439(7) 2_676 ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? N1 C18 1.458(6) 2_577 ? N3 C17 1.436(7) 2_577 ? N15 C35 1.428(7) 2_676 ? N24 C36 1.439(7) 2_676 ? 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 Er1 O7 126.32(14) . . ? O1 Er1 O8 151.13(14) . . ? O7 Er1 O8 77.30(13) . . ? O1 Er1 O2 77.07(13) . . ? O7 Er1 O2 151.21(13) . . ? O8 Er1 O2 87.15(13) . . ? O1 Er1 O1W 73.08(13) . . ? O7 Er1 O1W 70.62(13) . . ? O8 Er1 O1W 105.24(14) . . ? O2 Er1 O1W 137.62(13) . . ? O1 Er1 O2W 70.78(14) . . ? O7 Er1 O2W 73.43(14) . . ? O8 Er1 O2W 137.38(13) . . ? O2 Er1 O2W 104.34(14) . . ? O1W Er1 O2W 93.52(15) . . ? O1 Er1 O4W 123.39(14) . . ? O7 Er1 O4W 79.92(13) . . ? O8 Er1 O4W 72.56(14) . . ? O2 Er1 O4W 72.30(13) . . ? O1W Er1 O4W 150.02(14) . . ? O2W Er1 O4W 72.36(15) . . ? O1 Er1 O3W 80.13(14) . . ? O7 Er1 O3W 122.87(14) . . ? O8 Er1 O3W 72.17(14) . . ? O2 Er1 O3W 73.25(14) . . ? O1W Er1 O3W 72.55(15) . . ? O2W Er1 O3W 150.43(15) . . ? O4W Er1 O3W 131.15(15) . . ? Cl4 Zn1 Cl3 111.2(2) . . ? Cl4 Zn1 Cl2 108.52(16) . . ? Cl3 Zn1 Cl2 112.29(9) . . ? Cl4 Zn1 Cl1 108.88(17) . . ? Cl3 Zn1 Cl1 107.49(10) . . ? Cl2 Zn1 Cl1 108.40(11) . . ? O1 C1 N1 125.4(5) . . ? O1 C1 N2 125.6(5) . . ? N1 C1 N2 109.0(5) . . ? N3 C2 N1 114.4(4) . . ? N3 C2 C3 102.3(4) . . ? N1 C2 C3 103.2(4) . . ? N3 C2 H2 112.1 . . ? N1 C2 H2 112.1 . . ? C3 C2 H2 112.1 . . ? N4 C3 N2 114.2(5) . . ? N4 C3 C2 104.0(4) . . ? N2 C3 C2 103.0(4) . . ? N4 C3 H3 111.7 . . ? N2 C3 H3 111.7 . . ? C2 C3 H3 111.7 . . ? O4 C4 N4 126.2(6) . . ? O4 C4 N3 126.0(6) . . ? N4 C4 N3 107.7(5) . . ? N2 C5 N5 114.5(4) . . ? N2 C5 H5A 108.6 . . ? N5 C5 H5A 108.6 . . ? N2 C5 H5B 108.6 . . ? N5 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? N4 C6 N7 114.5(5) . . ? N4 C6 H6A 108.6 . . ? N7 C6 H6A 108.6 . . ? N4 C6 H6B 108.6 . . ? N7 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? O2 C7 N5 125.5(5) . . ? O2 C7 N6 124.1(5) . . ? N5 C7 N6 110.3(4) . . ? N7 C8 N5 114.6(4) . . ? N7 C8 C9 103.9(4) . . ? N5 C8 C9 103.4(4) . . ? N7 C8 H8 111.5 . . ? N5 C8 H8 111.5 . . ? C9 C8 H8 111.5 . . ? N8 C9 N6 115.1(4) . . ? N8 C9 C8 103.3(4) . . ? N6 C9 C8 103.8(4) . . ? N8 C9 H9 111.4 . . ? N6 C9 H9 111.4 . . ? C8 C9 H9 111.4 . . ? O5 C10 N8 126.0(5) . . ? O5 C10 N7 125.2(6) . . ? N8 C10 N7 108.7(5) . . ? N6 C11 N9 113.4(4) . . ? N6 C11 H11A 108.9 . . ? N9 C11 H11A 108.9 . . ? N6 C11 H11B 108.9 . . ? N9 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? N8 C12 N11 114.7(4) . . ? N8 C12 H12A 108.6 . . ? N11 C12 H12A 108.6 . . ? N8 C12 H12B 108.6 . . ? N11 C12 H12B 108.6 . . ? H12A C12 H12B 107.6 . . ? O3 C13 N9 126.6(5) . . ? O3 C13 N10 125.6(5) . . ? N9 C13 N10 107.6(4) . . ? N11 C14 N9 115.7(5) . . ? N11 C14 C15 103.3(4) . . ? N9 C14 C15 102.3(4) . . ? N11 C14 H14 111.6 . . ? N9 C14 H14 111.6 . . ? C15 C14 H14 111.6 . . ? N12 C15 N10 115.6(4) . . ? N12 C15 C14 102.5(4) . . ? N10 C15 C14 104.0(4) . . ? N12 C15 H15 111.4 . . ? N10 C15 H15 111.4 . . ? C14 C15 H15 111.4 . . ? O6 C16 N12 126.9(5) . . ? O6 C16 N11 125.9(5) . . ? N12 C16 N11 107.2(4) . . ? N3 C17 N10 114.7(5) 2_577 . ? N3 C17 H17A 108.6 2_577 . ? N10 C17 H17A 108.6 . . ? N3 C17 H17B 108.6 2_577 . ? N10 C17 H17B 108.6 . . ? H17A C17 H17B 107.6 . . ? N12 C18 N1 114.0(4) . 2_577 ? N12 C18 H18A 108.8 . . ? N1 C18 H18A 108.8 2_577 . ? N12 C18 H18B 108.8 . . ? N1 C18 H18B 108.8 2_577 . ? H18A C18 H18B 107.6 . . ? O7 C19 N14 125.3(5) . . ? O7 C19 N13 124.4(5) . . ? N14 C19 N13 110.3(4) . . ? N15 C20 N13 113.7(4) . . ? N15 C20 C21 104.0(5) . . ? N13 C20 C21 103.2(4) . . ? N15 C20 H20 111.8 . . ? N13 C20 H20 111.8 . . ? C21 C20 H20 111.8 . . ? N16 C21 N14 114.3(4) . . ? N16 C21 C20 103.2(4) . . ? N14 C21 C20 103.3(4) . . ? N16 C21 H21 111.8 . . ? N14 C21 H21 111.8 . . ? C20 C21 H21 111.8 . . ? O10 C22 N15 125.9(5) . . ? O10 C22 N16 126.6(6) . . ? N15 C22 N16 107.4(5) . . ? N17 C23 N14 113.8(4) . . ? N17 C23 H23A 108.8 . . ? N14 C23 H23A 108.8 . . ? N17 C23 H23B 108.8 . . ? N14 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? N16 C24 N19 113.9(5) . . ? N16 C24 H24A 108.8 . . ? N19 C24 H24A 108.8 . . ? N16 C24 H24B 108.8 . . ? N19 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? O8 C25 N18 126.0(5) . . ? O8 C25 N17 124.0(5) . . ? N18 C25 N17 110.0(5) . . ? N19 C26 N17 114.1(5) . . ? N19 C26 C27 102.5(4) . . ? N17 C26 C27 103.2(4) . . ? N19 C26 H26 112.1 . . ? N17 C26 H26 112.1 . . ? C27 C26 H26 112.1 . . ? N18 C27 N20 114.7(4) . . ? N18 C27 C26 103.2(4) . . ? N20 C27 C26 103.5(4) . . ? N18 C27 H27 111.6 . . ? N20 C27 H27 111.6 . . ? C26 C27 H27 111.6 . . ? O11 C28 N19 126.5(6) . . ? O11 C28 N20 124.2(6) . . ? N19 C28 N20 109.3(5) . . ? N21 C29 N18 114.4(4) . . ? N21 C29 H29A 108.6 . . ? N18 C29 H29A 108.6 . . ? N21 C29 H29B 108.6 . . ? N18 C29 H29B 108.6 . . ? H29A C29 H29B 107.6 . . ? N20 C30 N23 115.3(5) . . ? N20 C30 H30A 108.5 . . ? N23 C30 H30A 108.5 . . ? N20 C30 H30B 108.5 . . ? N23 C30 H30B 108.5 . . ? H30A C30 H30B 107.5 . . ? O9 C31 N21 125.6(5) . . ? O9 C31 N22 126.2(5) . . ? N21 C31 N22 108.1(5) . . ? N21 C32 N23 114.9(4) . . ? N21 C32 C33 103.5(4) . . ? N23 C32 C33 104.0(4) . . ? N21 C32 H32 111.3 . . ? N23 C32 H32 111.3 . . ? C33 C32 H32 111.3 . . ? N22 C33 N24 115.9(5) . . ? N22 C33 C32 102.9(4) . . ? N24 C33 C32 102.9(4) . . ? N22 C33 H33 111.5 . . ? N24 C33 H33 111.5 . . ? C32 C33 H33 111.5 . . ? O12 C34 N23 126.4(5) . . ? O12 C34 N24 125.2(5) . . ? N23 C34 N24 108.2(5) . . ? N15 C35 N22 113.0(4) 2_676 . ? N15 C35 H35A 109.0 2_676 . ? N22 C35 H35A 109.0 . . ? N15 C35 H35B 109.0 2_676 . ? N22 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? N13 C36 N24 115.1(5) . 2_676 ? N13 C36 H36A 108.5 . . ? N24 C36 H36A 108.5 2_676 . ? N13 C36 H36B 108.5 . . ? N24 C36 H36B 108.5 2_676 . ? H36A C36 H36B 107.5 . . ? C1 N1 C2 112.7(4) . . ? C1 N1 C18 122.0(4) . 2_577 ? C2 N1 C18 123.7(4) . 2_577 ? C1 N2 C5 122.7(5) . . ? C1 N2 C3 111.8(4) . . ? C5 N2 C3 125.5(4) . . ? C4 N3 C2 113.5(5) . . ? C4 N3 C17 122.4(5) . 2_577 ? C2 N3 C17 123.5(5) . 2_577 ? C4 N4 C6 123.0(5) . . ? C4 N4 C3 112.3(5) . . ? C6 N4 C3 124.2(5) . . ? C7 N5 C5 124.9(4) . . ? C7 N5 C8 111.1(4) . . ? C5 N5 C8 124.1(4) . . ? C7 N6 C11 121.6(5) . . ? C7 N6 C9 111.2(4) . . ? C11 N6 C9 124.4(5) . . ? C10 N7 C6 122.5(5) . . ? C10 N7 C8 111.2(5) . . ? C6 N7 C8 126.2(5) . . ? C10 N8 C12 122.8(5) . . ? C10 N8 C9 112.6(5) . . ? C12 N8 C9 124.2(5) . . ? C13 N9 C14 114.0(4) . . ? C13 N9 C11 121.5(4) . . ? C14 N9 C11 123.9(4) . . ? C13 N10 C17 122.4(5) . . ? C13 N10 C15 112.1(4) . . ? C17 N10 C15 124.6(5) . . ? C16 N11 C14 113.4(4) . . ? C16 N11 C12 121.9(4) . . ? C14 N11 C12 123.0(4) . . ? C16 N12 C15 113.6(4) . . ? C16 N12 C18 122.2(4) . . ? C15 N12 C18 122.7(5) . . ? C19 N13 C36 122.9(4) . . ? C19 N13 C20 111.4(4) . . ? C36 N13 C20 123.8(5) . . ? C19 N14 C23 123.1(4) . . ? C19 N14 C21 111.8(4) . . ? C23 N14 C21 124.8(4) . . ? C22 N15 C35 122.6(5) . 2_676 ? C22 N15 C20 112.8(4) . . ? C35 N15 C20 123.5(5) 2_676 . ? C22 N16 C24 123.3(5) . . ? C22 N16 C21 112.5(5) . . ? C24 N16 C21 124.2(5) . . ? C25 N17 C23 124.2(5) . . ? C25 N17 C26 111.1(5) . . ? C23 N17 C26 124.6(4) . . ? C25 N18 C29 123.1(5) . . ? C25 N18 C27 112.4(4) . . ? C29 N18 C27 123.3(5) . . ? C28 N19 C26 112.7(5) . . ? C28 N19 C24 122.8(5) . . ? C26 N19 C24 123.3(5) . . ? C28 N20 C30 123.6(5) . . ? C28 N20 C27 111.5(5) . . ? C30 N20 C27 124.5(5) . . ? C31 N21 C29 122.9(5) . . ? C31 N21 C32 112.5(4) . . ? C29 N21 C32 123.4(4) . . ? C31 N22 C33 113.0(4) . . ? C31 N22 C35 122.5(5) . . ? C33 N22 C35 122.4(5) . . ? C34 N23 C30 123.0(4) . . ? C34 N23 C32 112.3(4) . . ? C30 N23 C32 123.2(4) . . ? C34 N24 C33 112.7(4) . . ? C34 N24 C36 123.8(4) . 2_676 ? C33 N24 C36 123.1(4) . 2_676 ? C1 O1 Er1 157.3(3) . . ? C7 O2 Er1 154.9(4) . . ? C19 O7 Er1 156.8(4) . . ? C25 O8 Er1 156.3(4) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 4.006 _refine_diff_density_min -1.087 _refine_diff_density_rms 0.120 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 93 26 ' ' 2 -0.062 0.500 0.258 1056 431 ' ' 3 0.500 1.000 0.500 92 30 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 902623' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p313 #TrackingRef 'submit-313.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H94 Cl5 N24 O41 Tm Zn' _chemical_formula_weight 1930.90 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -0.3139 5.2483 '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 15.1322(15) _cell_length_b 15.5741(15) _cell_length_c 16.9621(16) _cell_angle_alpha 64.032(4) _cell_angle_beta 81.003(4) _cell_angle_gamma 81.418(4) _cell_volume 3535.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.814 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1980 _exptl_absorpt_coefficient_mu 1.891 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6922 _exptl_absorpt_correction_T_max 0.7646 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37793 _diffrn_reflns_av_R_equivalents 0.0827 _diffrn_reflns_av_sigmaI/netI 0.0971 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12288 _reflns_number_gt 9084 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0927P)^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 12288 _refine_ls_number_parameters 761 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_gt 0.0602 _refine_ls_wR_factor_ref 0.1583 _refine_ls_wR_factor_gt 0.1488 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _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 Cl5 Cl 0.51050(16) 1.2029(2) 0.45088(19) 0.0750(10) Uani 0.892(6) 1 d P A 1 Cl5' Cl 0.5139(11) 1.2163(12) 0.3659(15) 0.058(8) Uani 0.108(6) 1 d P A 2 O1W O 0.2094(2) 1.0899(3) 0.1898(2) 0.0236(6) Uani 1 1 d . . . O2W O 0.4330(3) 0.8673(4) 0.3591(3) 0.0509(13) Uani 1 1 d . . . O3W O 0.3930(3) 1.0149(4) 0.1981(3) 0.0510(12) Uani 1 1 d . . . O4W O 0.2410(2) 0.7617(3) 0.3917(2) 0.0236(6) Uani 1 1 d . . . O5W O 0.1330(3) 0.9354(4) 0.3374(3) 0.0520(13) Uani 1 1 d . . . Tm1 Tm 0.291102(17) 0.91301(2) 0.308651(18) 0.03437(12) Uani 1 1 d . . . Cl1 Cl -0.01228(15) 0.7580(2) 0.1550(2) 0.0962(9) Uani 1 1 d . . . Cl2 Cl -0.10849(17) 0.5418(2) 0.1905(3) 0.1162(12) Uani 1 1 d . . . Cl3 Cl 0.14062(16) 0.5484(2) 0.1667(2) 0.1208(13) Uani 1 1 d . . . Cl4 Cl 0.0154(5) 0.6846(4) -0.0245(2) 0.229(3) Uani 1 1 d . . . Zn1 Zn 0.00834(7) 0.63095(8) 0.12107(7) 0.0754(3) Uani 1 1 d . . . C1 C 0.2485(4) 1.1307(5) 0.3246(4) 0.0406(16) Uani 1 1 d . . . C2 C 0.2071(4) 1.2754(5) 0.3342(4) 0.0362(14) Uani 1 1 d . . . H2 H 0.2300 1.3361 0.2891 0.043 Uiso 1 1 calc R . . C3 C 0.2766(4) 1.2146(5) 0.4008(4) 0.0420(16) Uani 1 1 d . . . H3 H 0.3307 1.2487 0.3895 0.050 Uiso 1 1 calc R . . C4 C 0.1463(4) 1.2518(6) 0.4765(5) 0.0470(18) Uani 1 1 d . . . C5 C 0.3596(4) 1.0530(5) 0.4307(4) 0.0415(16) Uani 1 1 d . . . H5A H 0.4085 1.0782 0.4434 0.050 Uiso 1 1 calc R . . H5B H 0.3855 1.0219 0.3920 0.050 Uiso 1 1 calc R . . C6 C 0.2662(5) 1.1528(6) 0.5686(4) 0.0481(18) Uani 1 1 d . . . H6A H 0.3306 1.1613 0.5570 0.058 Uiso 1 1 calc R . . H6B H 0.2393 1.1842 0.6068 0.058 Uiso 1 1 calc R . . C7 C 0.2852(4) 0.9054(5) 0.5164(4) 0.0344(14) Uani 1 1 d . . . C8 C 0.3177(4) 0.9831(5) 0.5984(4) 0.0397(16) Uani 1 1 d . . . H8 H 0.3787 0.9845 0.6119 0.048 Uiso 1 1 calc R . . C9 C 0.2769(4) 0.8859(5) 0.6625(4) 0.0371(15) Uani 1 1 d . . . H9 H 0.3188 0.8420 0.7056 0.045 Uiso 1 1 calc R . . C10 C 0.1862(5) 1.0142(6) 0.6788(4) 0.0478(19) Uani 1 1 d . . . C11 C 0.2399(4) 0.7533(5) 0.6306(4) 0.0356(15) Uani 1 1 d . . . H11A H 0.2749 0.7121 0.6799 0.043 Uiso 1 1 calc R . . H11B H 0.2609 0.7343 0.5824 0.043 Uiso 1 1 calc R . . C12 C 0.1459(5) 0.8518(6) 0.7788(4) 0.0482(18) Uani 1 1 d . . . H12A H 0.1867 0.8001 0.8163 0.058 Uiso 1 1 calc R . . H12B H 0.1142 0.8855 0.8135 0.058 Uiso 1 1 calc R . . C13 C 0.0941(4) 0.7144(5) 0.6112(4) 0.0404(15) Uani 1 1 d . . . C14 C 0.1048(4) 0.7219(5) 0.7436(4) 0.0355(14) Uani 1 1 d . . . H14 H 0.1393 0.6726 0.7910 0.043 Uiso 1 1 calc R . . C15 C 0.0124(4) 0.6912(5) 0.7471(4) 0.0331(14) Uani 1 1 d . . . H15 H 0.0034 0.6272 0.7959 0.040 Uiso 1 1 calc R . . C16 C -0.0092(4) 0.8307(5) 0.7668(4) 0.0356(14) Uani 1 1 d . . . C17 C 0.0503(4) 1.3528(5) 0.3594(5) 0.0395(15) Uani 1 1 d . . . H17A H 0.0219 1.3743 0.4045 0.047 Uiso 1 1 calc R . . H17B H 0.0673 1.4099 0.3064 0.047 Uiso 1 1 calc R . . C18 C 0.1460(4) 1.2399(5) 0.2204(4) 0.0382(15) Uani 1 1 d . . . H18A H 0.1577 1.3058 0.1791 0.046 Uiso 1 1 calc R . . H18B H 0.1692 1.1984 0.1905 0.046 Uiso 1 1 calc R . . C19 C 0.2123(4) 0.9588(5) 0.1121(4) 0.0370(15) Uani 1 1 d . . . C20 C 0.1665(4) 1.0046(5) -0.0252(4) 0.0371(15) Uani 1 1 d . . . H20 H 0.1037 1.0303 -0.0375 0.045 Uiso 1 1 calc R . . C21 C 0.1732(4) 0.8953(6) 0.0223(4) 0.0449(17) Uani 1 1 d . . . H21 H 0.1148 0.8697 0.0299 0.054 Uiso 1 1 calc R . . C22 C 0.2651(4) 0.9401(5) -0.1092(4) 0.0363(15) Uani 1 1 d . . . C23 C 0.2159(4) 0.7843(5) 0.1784(4) 0.0374(15) Uani 1 1 d . . . H23A H 0.2002 0.7891 0.2348 0.045 Uiso 1 1 calc R . . H23B H 0.1750 0.7426 0.1758 0.045 Uiso 1 1 calc R . . C24 C 0.2732(5) 0.7680(6) -0.0161(5) 0.0527(19) Uani 1 1 d . . . H24A H 0.2914 0.7649 -0.0729 0.063 Uiso 1 1 calc R . . H24B H 0.2239 0.7270 0.0137 0.063 Uiso 1 1 calc R . . C25 C 0.3711(4) 0.7559(5) 0.2126(4) 0.0344(14) Uani 1 1 d . . . C26 C 0.3393(4) 0.6805(5) 0.1318(4) 0.0387(15) Uani 1 1 d . . . H26 H 0.3040 0.6245 0.1529 0.046 Uiso 1 1 calc R . . C27 C 0.4378(4) 0.6490(5) 0.1539(4) 0.0358(14) Uani 1 1 d . . . H27 H 0.4486 0.5790 0.1891 0.043 Uiso 1 1 calc R . . C28 C 0.4342(4) 0.7265(5) 0.0006(5) 0.0410(16) Uani 1 1 d . . . C29 C 0.5216(4) 0.6855(4) 0.2528(4) 0.0317(13) Uani 1 1 d . . . H29A H 0.5387 0.6162 0.2796 0.038 Uiso 1 1 calc R . . H29B H 0.5011 0.7051 0.3007 0.038 Uiso 1 1 calc R . . C30 C 0.5825(4) 0.6567(5) 0.0531(5) 0.0465(17) Uani 1 1 d . . . H30A H 0.5977 0.5896 0.0928 0.056 Uiso 1 1 calc R . . H30B H 0.5954 0.6627 -0.0075 0.056 Uiso 1 1 calc R . . C31 C 0.6276(4) 0.8051(5) 0.2153(4) 0.0363(14) Uani 1 1 d . . . C32 C 0.6661(4) 0.6986(5) 0.1504(4) 0.0401(15) Uani 1 1 d . . . H32 H 0.6866 0.6303 0.1845 0.048 Uiso 1 1 calc R . . C33 C 0.7428(4) 0.7626(5) 0.1252(4) 0.0322(14) Uani 1 1 d . . . H33 H 0.7998 0.7247 0.1464 0.039 Uiso 1 1 calc R . . C34 C 0.6885(4) 0.7798(5) -0.0029(5) 0.0394(15) Uani 1 1 d . . . C35 C 0.2313(4) 1.1155(5) -0.1780(4) 0.0385(15) Uani 1 1 d . . . H35A H 0.2539 1.1068 -0.2317 0.046 Uiso 1 1 calc R . . H35B H 0.1713 1.1500 -0.1866 0.046 Uiso 1 1 calc R . . C36 C 0.1837(4) 1.1308(5) 0.0265(4) 0.0427(16) Uani 1 1 d . . . H36A H 0.1817 1.1280 0.0856 0.051 Uiso 1 1 calc R . . H36B H 0.1254 1.1607 0.0046 0.051 Uiso 1 1 calc R . . N1 N 0.1944(3) 1.2115(4) 0.2962(4) 0.0387(12) Uani 1 1 d . . . N2 N 0.2974(3) 1.1296(4) 0.3864(3) 0.0340(12) Uani 1 1 d . . . N3 N 0.1311(3) 1.2922(4) 0.3904(4) 0.0414(13) Uani 1 1 d . . . N4 N 0.2273(4) 1.1994(5) 0.4874(4) 0.0478(15) Uani 1 1 d . . . N5 N 0.3201(3) 0.9823(4) 0.5121(3) 0.0406(13) Uani 1 1 d . . . N6 N 0.2595(3) 0.8470(4) 0.6029(3) 0.0382(12) Uani 1 1 d . . . N7 N 0.2554(4) 1.0542(5) 0.6141(4) 0.0455(14) Uani 1 1 d . . . N8 N 0.1984(3) 0.9181(4) 0.7040(3) 0.0396(13) Uani 1 1 d . . . N9 N 0.1470(4) 0.7336(4) 0.6580(4) 0.0435(13) Uani 1 1 d . . . N10 N 0.0143(3) 0.6900(4) 0.6609(3) 0.0382(12) Uani 1 1 d . . . N11 N 0.0824(3) 0.8109(4) 0.7561(3) 0.0424(13) Uani 1 1 d . . . N12 N -0.0513(3) 0.7648(4) 0.7590(3) 0.0387(12) Uani 1 1 d . . . N13 N 0.1948(3) 1.0362(4) 0.0337(3) 0.0363(12) Uani 1 1 d . . . N14 N 0.2023(3) 0.8782(4) 0.1078(3) 0.0327(12) Uani 1 1 d . . . N15 N 0.2229(4) 1.0225(4) -0.1058(3) 0.0401(13) Uani 1 1 d . . . N16 N 0.2408(4) 0.8631(4) -0.0320(4) 0.0431(13) Uani 1 1 d . . . N17 N 0.3050(3) 0.7414(4) 0.1759(3) 0.0366(12) Uani 1 1 d . . . N18 N 0.4483(3) 0.7037(4) 0.2020(3) 0.0375(12) Uani 1 1 d . . . N19 N 0.3480(4) 0.7298(4) 0.0365(4) 0.0421(13) Uani 1 1 d . . . N20 N 0.4872(4) 0.6810(4) 0.0694(4) 0.0439(13) Uani 1 1 d . . . N21 N 0.6005(3) 0.7341(4) 0.2030(4) 0.0392(13) Uani 1 1 d . . . N22 N 0.7109(3) 0.8257(4) 0.1678(3) 0.0384(12) Uani 1 1 d . . . N23 N 0.6383(3) 0.7149(4) 0.0649(3) 0.0396(13) Uani 1 1 d . . . N24 N 0.7485(3) 0.8088(4) 0.0297(3) 0.0398(13) Uani 1 1 d . . . O1 O 0.2556(3) 1.0650(3) 0.3010(3) 0.0416(11) Uani 1 1 d . . . O2 O 0.2780(3) 0.8884(3) 0.4547(3) 0.0410(11) Uani 1 1 d . . . O3 O 0.1166(3) 0.7125(4) 0.5404(3) 0.0537(13) Uani 1 1 d . . . O4 O 0.0916(4) 1.2607(5) 0.5373(4) 0.0726(16) Uani 1 1 d . . . O5 O 0.1293(3) 1.0583(4) 0.7055(3) 0.0542(13) Uani 1 1 d . . . O6 O -0.0460(3) 0.8988(3) 0.7821(3) 0.0437(11) Uani 1 1 d . . . O7 O 0.2324(3) 0.9658(3) 0.1776(3) 0.0418(11) Uani 1 1 d . . . O8 O 0.3632(3) 0.8089(3) 0.2512(3) 0.0420(11) Uani 1 1 d . . . O9 O 0.5895(3) 0.8427(4) 0.2617(3) 0.0494(12) Uani 1 1 d . . . O10 O 0.3152(3) 0.9351(4) -0.1719(3) 0.0471(12) Uani 1 1 d . . . O11 O 0.4596(4) 0.7549(4) -0.0761(4) 0.0625(14) Uani 1 1 d . . . O12 O 0.6820(3) 0.8037(3) -0.0809(3) 0.0480(12) 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 Cl5 0.0510(14) 0.094(2) 0.084(2) -0.0392(16) -0.0215(13) 0.0013(12) Cl5' 0.038(9) 0.037(10) 0.099(18) -0.030(10) 0.009(9) -0.014(7) O1W 0.0191(13) 0.0346(16) 0.0141(12) -0.0107(12) 0.0077(10) -0.0026(11) O2W 0.034(2) 0.086(4) 0.038(3) -0.033(3) -0.006(2) 0.007(2) O3W 0.038(3) 0.063(3) 0.050(3) -0.026(3) 0.010(2) -0.007(2) O4W 0.0191(13) 0.0346(16) 0.0141(12) -0.0107(12) 0.0077(10) -0.0026(11) O5W 0.030(2) 0.078(4) 0.048(3) -0.031(3) 0.004(2) -0.001(2) Tm1 0.02963(16) 0.0468(2) 0.02844(17) -0.02047(14) -0.00139(11) 0.00409(12) Cl1 0.0491(12) 0.094(2) 0.142(3) -0.0462(19) -0.0123(14) -0.0056(12) Cl2 0.0575(14) 0.0620(17) 0.204(4) -0.037(2) -0.0059(18) -0.0013(12) Cl3 0.0441(12) 0.0797(19) 0.155(3) 0.0196(18) 0.0042(15) 0.0030(12) Cl4 0.330(7) 0.204(5) 0.060(2) -0.018(3) -0.023(3) 0.129(5) Zn1 0.0553(6) 0.0632(7) 0.0722(7) -0.0026(5) -0.0014(5) 0.0100(5) C1 0.037(4) 0.045(4) 0.033(4) -0.013(3) 0.007(3) -0.004(3) C2 0.032(3) 0.037(4) 0.031(3) -0.013(3) 0.012(3) 0.002(3) C3 0.031(3) 0.059(5) 0.039(4) -0.025(4) 0.002(3) -0.005(3) C4 0.035(4) 0.068(5) 0.052(5) -0.042(4) 0.009(3) -0.008(3) C5 0.034(3) 0.056(5) 0.037(4) -0.023(3) 0.000(3) -0.004(3) C6 0.049(4) 0.061(5) 0.038(4) -0.027(4) 0.000(3) -0.006(4) C7 0.022(3) 0.045(4) 0.038(4) -0.020(3) -0.007(3) 0.007(3) C8 0.034(3) 0.061(5) 0.033(3) -0.028(3) -0.005(3) -0.003(3) C9 0.024(3) 0.067(5) 0.023(3) -0.022(3) -0.003(2) 0.000(3) C10 0.039(4) 0.084(6) 0.031(4) -0.032(4) -0.011(3) -0.005(4) C11 0.024(3) 0.048(4) 0.027(3) -0.014(3) -0.001(3) 0.011(3) C12 0.045(4) 0.076(5) 0.027(3) -0.027(4) -0.004(3) -0.002(4) C13 0.048(4) 0.035(4) 0.035(4) -0.015(3) -0.007(3) 0.009(3) C14 0.027(3) 0.041(4) 0.029(3) -0.011(3) 0.000(3) 0.007(3) C15 0.029(3) 0.035(4) 0.024(3) -0.005(3) 0.004(2) 0.001(3) C16 0.031(3) 0.048(4) 0.024(3) -0.013(3) -0.001(3) 0.002(3) C17 0.036(3) 0.028(4) 0.053(4) -0.018(3) -0.002(3) 0.002(3) C18 0.035(3) 0.054(4) 0.027(3) -0.020(3) 0.002(3) -0.002(3) C19 0.027(3) 0.051(4) 0.030(3) -0.015(3) -0.004(3) 0.001(3) C20 0.027(3) 0.051(4) 0.027(3) -0.012(3) -0.002(3) 0.001(3) C21 0.028(3) 0.076(5) 0.039(4) -0.030(4) -0.003(3) -0.009(3) C22 0.040(4) 0.043(4) 0.031(4) -0.019(3) -0.012(3) -0.002(3) C23 0.032(3) 0.044(4) 0.030(3) -0.009(3) 0.000(3) -0.007(3) C24 0.059(5) 0.070(6) 0.044(4) -0.035(4) -0.006(4) -0.014(4) C25 0.043(4) 0.034(4) 0.020(3) -0.008(3) 0.004(3) -0.005(3) C26 0.048(4) 0.026(4) 0.041(4) -0.015(3) -0.007(3) 0.002(3) C27 0.046(4) 0.028(4) 0.039(4) -0.019(3) -0.003(3) -0.003(3) C28 0.041(4) 0.041(4) 0.041(4) -0.021(3) 0.004(3) -0.003(3) C29 0.029(3) 0.031(4) 0.030(3) -0.008(3) -0.002(3) -0.003(3) C30 0.039(4) 0.055(5) 0.052(4) -0.034(4) 0.002(3) 0.008(3) C31 0.029(3) 0.042(4) 0.031(3) -0.014(3) 0.002(3) 0.003(3) C32 0.030(3) 0.050(4) 0.038(4) -0.019(3) -0.004(3) 0.004(3) C33 0.024(3) 0.047(4) 0.023(3) -0.017(3) 0.001(2) 0.008(3) C34 0.036(3) 0.042(4) 0.044(4) -0.024(3) -0.008(3) 0.008(3) C35 0.036(3) 0.057(5) 0.028(3) -0.023(3) -0.012(3) 0.005(3) C36 0.037(4) 0.059(5) 0.033(4) -0.026(3) 0.014(3) -0.004(3) N1 0.035(3) 0.040(3) 0.037(3) -0.015(3) -0.005(2) 0.004(2) N2 0.033(3) 0.041(3) 0.031(3) -0.019(3) -0.005(2) 0.003(2) N3 0.036(3) 0.052(4) 0.041(3) -0.029(3) 0.001(2) 0.003(3) N4 0.039(3) 0.069(4) 0.040(3) -0.029(3) 0.001(3) -0.007(3) N5 0.029(3) 0.055(4) 0.029(3) -0.013(3) -0.001(2) 0.006(2) N6 0.036(3) 0.048(4) 0.028(3) -0.016(3) -0.006(2) 0.006(2) N7 0.046(3) 0.064(4) 0.029(3) -0.023(3) 0.002(3) -0.013(3) N8 0.033(3) 0.056(4) 0.032(3) -0.022(3) 0.000(2) -0.001(3) N9 0.036(3) 0.053(4) 0.036(3) -0.014(3) -0.003(2) -0.001(3) N10 0.038(3) 0.038(3) 0.034(3) -0.014(3) 0.002(2) -0.002(2) N11 0.037(3) 0.057(4) 0.031(3) -0.016(3) -0.010(2) 0.003(3) N12 0.035(3) 0.043(3) 0.038(3) -0.018(3) -0.003(2) 0.000(2) N13 0.030(3) 0.045(3) 0.032(3) -0.016(3) -0.008(2) 0.006(2) N14 0.031(3) 0.041(3) 0.026(3) -0.014(2) -0.006(2) -0.002(2) N15 0.045(3) 0.046(4) 0.029(3) -0.019(3) -0.002(2) 0.004(3) N16 0.044(3) 0.049(4) 0.039(3) -0.025(3) 0.005(3) -0.002(3) N17 0.031(3) 0.045(3) 0.034(3) -0.018(3) -0.007(2) 0.003(2) N18 0.041(3) 0.036(3) 0.034(3) -0.018(3) -0.003(2) 0.007(2) N19 0.047(3) 0.046(4) 0.036(3) -0.022(3) -0.005(3) 0.003(3) N20 0.045(3) 0.053(4) 0.036(3) -0.023(3) -0.002(3) -0.001(3) N21 0.030(3) 0.042(3) 0.047(3) -0.022(3) 0.001(2) -0.001(2) N22 0.034(3) 0.051(4) 0.031(3) -0.019(3) 0.002(2) -0.006(2) N23 0.038(3) 0.047(4) 0.036(3) -0.023(3) 0.005(2) -0.005(3) N24 0.037(3) 0.049(4) 0.034(3) -0.020(3) 0.004(2) -0.005(3) O1 0.042(2) 0.052(3) 0.044(3) -0.035(3) -0.001(2) 0.000(2) O2 0.047(3) 0.056(3) 0.026(2) -0.026(2) 0.000(2) 0.000(2) O3 0.047(3) 0.072(4) 0.045(3) -0.033(3) 0.013(2) -0.007(2) O4 0.075(4) 0.091(5) 0.049(3) -0.037(3) 0.008(3) 0.009(3) O5 0.046(3) 0.073(4) 0.056(3) -0.042(3) 0.000(2) 0.004(3) O6 0.043(3) 0.043(3) 0.049(3) -0.024(2) -0.012(2) 0.009(2) O7 0.037(2) 0.063(3) 0.032(2) -0.028(2) -0.0016(19) 0.000(2) O8 0.037(2) 0.060(3) 0.035(2) -0.030(2) 0.001(2) 0.007(2) O9 0.043(3) 0.070(4) 0.039(3) -0.031(3) 0.005(2) 0.000(2) O10 0.045(3) 0.061(3) 0.034(3) -0.022(2) -0.003(2) 0.002(2) O11 0.069(4) 0.071(4) 0.045(3) -0.026(3) -0.007(3) 0.003(3) O12 0.057(3) 0.051(3) 0.036(3) -0.018(2) -0.006(2) -0.002(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 O1W Tm1 2.843(4) . ? O2W Tm1 2.332(4) . ? O3W Tm1 2.373(5) . ? O4W Tm1 2.325(4) . ? O5W Tm1 2.369(4) . ? Tm1 O7 2.281(4) . ? Tm1 O1 2.298(4) . ? Tm1 O8 2.301(4) . ? Tm1 O2 2.316(4) . ? Cl1 Zn1 2.259(3) . ? Cl2 Zn1 2.256(3) . ? Cl3 Zn1 2.259(3) . ? Cl4 Zn1 2.224(4) . ? C1 O1 1.237(8) . ? C1 N1 1.331(9) . ? C1 N2 1.367(8) . ? C2 N3 1.444(7) . ? C2 N1 1.450(8) . ? C2 C3 1.555(9) . ? C2 H2 0.9900 . ? C3 N2 1.432(8) . ? C3 N4 1.474(8) . ? C3 H3 0.9900 . ? C4 O4 1.262(8) . ? C4 N3 1.355(9) . ? C4 N4 1.358(9) . ? C5 N2 1.405(8) . ? C5 N5 1.443(8) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.406(9) . ? C6 N4 1.422(9) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.209(7) . ? C7 N5 1.349(8) . ? C7 N6 1.375(8) . ? C8 N7 1.432(9) . ? C8 N5 1.465(8) . ? C8 C9 1.575(10) . ? C8 H8 0.9900 . ? C9 N8 1.423(8) . ? C9 N6 1.460(7) . ? C9 H9 0.9900 . ? C10 O5 1.181(8) . ? C10 N8 1.357(10) . ? C10 N7 1.387(9) . ? C11 N6 1.386(8) . ? C11 N9 1.443(8) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.410(8) . ? C12 N8 1.446(9) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.208(7) . ? C13 N9 1.355(8) . ? C13 N10 1.362(8) . ? C14 N9 1.436(8) . ? C14 N11 1.475(8) . ? C14 C15 1.527(8) . ? C14 H14 0.9900 . ? C15 N12 1.448(8) . ? C15 N10 1.466(8) . ? C15 H15 0.9900 . ? C16 O6 1.232(7) . ? C16 N12 1.349(8) . ? C16 N11 1.376(8) . ? C17 N10 1.421(8) 2_576 ? C17 N3 1.444(8) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.426(8) 2_576 ? C18 N1 1.445(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O7 1.250(7) . ? C19 N14 1.320(8) . ? C19 N13 1.380(8) . ? C20 N15 1.431(8) . ? C20 N13 1.433(8) . ? C20 C21 1.526(10) . ? C20 H20 0.9900 . ? C21 N16 1.450(8) . ? C21 N14 1.480(8) . ? C21 H21 0.9900 . ? C22 O10 1.230(7) . ? C22 N15 1.366(8) . ? C22 N16 1.377(8) . ? C23 N17 1.416(8) . ? C23 N14 1.439(8) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N16 1.408(9) . ? C24 N19 1.444(9) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O8 1.243(7) . ? C25 N17 1.349(8) . ? C25 N18 1.355(8) . ? C26 N17 1.444(8) . ? C26 N19 1.447(8) . ? C26 C27 1.549(9) . ? C26 H26 0.9900 . ? C27 N20 1.418(8) . ? C27 N18 1.452(7) . ? C27 H27 0.9900 . ? C28 O11 1.194(8) . ? C28 N19 1.354(8) . ? C28 N20 1.380(9) . ? C29 N18 1.428(8) . ? C29 N21 1.452(7) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N23 1.418(8) . ? C30 N20 1.451(8) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O9 1.207(7) . ? C31 N21 1.341(8) . ? C31 N22 1.384(8) . ? C32 N21 1.442(8) . ? C32 N23 1.478(8) . ? C32 C33 1.530(9) . ? C32 H32 0.9900 . ? C33 N22 1.446(8) . ? C33 N24 1.450(8) . ? C33 H33 0.9900 . ? C34 O12 1.224(8) . ? C34 N24 1.353(8) . ? C34 N23 1.364(8) . ? C35 N22 1.435(8) 2_675 ? C35 N15 1.438(9) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N13 1.410(9) . ? C36 N24 1.430(8) 2_675 ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? N10 C17 1.421(8) 2_576 ? N12 C18 1.426(8) 2_576 ? N22 C35 1.435(8) 2_675 ? N24 C36 1.430(8) 2_675 ? 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 Tm1 O1 87.94(16) . . ? O7 Tm1 O8 76.84(15) . . ? O1 Tm1 O8 151.35(17) . . ? O7 Tm1 O2 151.20(16) . . ? O1 Tm1 O2 76.72(16) . . ? O8 Tm1 O2 126.46(16) . . ? O7 Tm1 O4W 104.28(14) . . ? O1 Tm1 O4W 137.54(14) . . ? O8 Tm1 O4W 70.55(14) . . ? O2 Tm1 O4W 73.51(14) . . ? O7 Tm1 O2W 137.20(15) . . ? O1 Tm1 O2W 104.28(17) . . ? O8 Tm1 O2W 73.29(15) . . ? O2 Tm1 O2W 71.02(15) . . ? O4W Tm1 O2W 93.92(16) . . ? O7 Tm1 O5W 72.91(16) . . ? O1 Tm1 O5W 72.18(17) . . ? O8 Tm1 O5W 124.17(16) . . ? O2 Tm1 O5W 79.19(16) . . ? O4W Tm1 O5W 73.03(16) . . ? O2W Tm1 O5W 149.89(16) . . ? O7 Tm1 O3W 72.97(16) . . ? O1 Tm1 O3W 72.03(16) . . ? O8 Tm1 O3W 80.29(17) . . ? O2 Tm1 O3W 123.12(16) . . ? O4W Tm1 O3W 150.39(15) . . ? O2W Tm1 O3W 72.35(18) . . ? O5W Tm1 O3W 130.66(18) . . ? O7 Tm1 O1W 44.43(13) . . ? O1 Tm1 O1W 43.51(13) . . ? O8 Tm1 O1W 117.33(13) . . ? O2 Tm1 O1W 116.21(13) . . ? O4W Tm1 O1W 133.21(11) . . ? O2W Tm1 O1W 132.87(15) . . ? O5W Tm1 O1W 65.18(15) . . ? O3W Tm1 O1W 65.49(14) . . ? Cl4 Zn1 Cl2 111.8(2) . . ? Cl4 Zn1 Cl1 108.68(18) . . ? Cl2 Zn1 Cl1 107.37(12) . . ? Cl4 Zn1 Cl3 108.93(18) . . ? Cl2 Zn1 Cl3 111.83(11) . . ? Cl1 Zn1 Cl3 108.10(13) . . ? O1 C1 N1 127.3(6) . . ? O1 C1 N2 123.4(6) . . ? N1 C1 N2 109.3(6) . . ? N3 C2 N1 115.3(5) . . ? N3 C2 C3 102.5(5) . . ? N1 C2 C3 102.3(5) . . ? N3 C2 H2 112.0 . . ? N1 C2 H2 112.0 . . ? C3 C2 H2 112.0 . . ? N2 C3 N4 114.3(6) . . ? N2 C3 C2 103.5(5) . . ? N4 C3 C2 103.9(5) . . ? N2 C3 H3 111.5 . . ? N4 C3 H3 111.5 . . ? C2 C3 H3 111.5 . . ? O4 C4 N3 124.3(7) . . ? O4 C4 N4 125.5(7) . . ? N3 C4 N4 110.2(6) . . ? N2 C5 N5 112.9(5) . . ? N2 C5 H5A 109.0 . . ? N5 C5 H5A 109.0 . . ? N2 C5 H5B 109.0 . . ? N5 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N7 C6 N4 114.5(6) . . ? N7 C6 H6A 108.6 . . ? N4 C6 H6A 108.6 . . ? N7 C6 H6B 108.6 . . ? N4 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? O2 C7 N5 126.3(6) . . ? O2 C7 N6 124.2(6) . . ? N5 C7 N6 109.5(5) . . ? N7 C8 N5 116.1(5) . . ? N7 C8 C9 103.6(5) . . ? N5 C8 C9 102.3(5) . . ? N7 C8 H8 111.4 . . ? N5 C8 H8 111.4 . . ? C9 C8 H8 111.4 . . ? N8 C9 N6 114.6(5) . . ? N8 C9 C8 102.0(5) . . ? N6 C9 C8 103.4(5) . . ? N8 C9 H9 112.1 . . ? N6 C9 H9 112.1 . . ? C8 C9 H9 112.1 . . ? O5 C10 N8 128.4(7) . . ? O5 C10 N7 124.6(8) . . ? N8 C10 N7 107.0(6) . . ? N6 C11 N9 117.3(5) . . ? N6 C11 H11A 108.0 . . ? N9 C11 H11A 108.0 . . ? N6 C11 H11B 108.0 . . ? N9 C11 H11B 108.0 . . ? H11A C11 H11B 107.2 . . ? N11 C12 N8 114.1(5) . . ? N11 C12 H12A 108.7 . . ? N8 C12 H12A 108.7 . . ? N11 C12 H12B 108.7 . . ? N8 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? O3 C13 N9 125.7(6) . . ? O3 C13 N10 125.9(6) . . ? N9 C13 N10 108.2(5) . . ? N9 C14 N11 115.6(5) . . ? N9 C14 C15 103.7(5) . . ? N11 C14 C15 102.8(5) . . ? N9 C14 H14 111.4 . . ? N11 C14 H14 111.4 . . ? C15 C14 H14 111.4 . . ? N12 C15 N10 113.6(5) . . ? N12 C15 C14 105.1(5) . . ? N10 C15 C14 103.2(5) . . ? N12 C15 H15 111.5 . . ? N10 C15 H15 111.5 . . ? C14 C15 H15 111.5 . . ? O6 C16 N12 125.9(6) . . ? O6 C16 N11 124.0(6) . . ? N12 C16 N11 110.0(6) . . ? N10 C17 N3 115.6(5) 2_576 . ? N10 C17 H17A 108.4 2_576 . ? N3 C17 H17A 108.4 . . ? N10 C17 H17B 108.4 2_576 . ? N3 C17 H17B 108.4 . . ? H17A C17 H17B 107.4 . . ? N12 C18 N1 114.0(5) 2_576 . ? N12 C18 H18A 108.7 2_576 . ? N1 C18 H18A 108.7 . . ? N12 C18 H18B 108.7 2_576 . ? N1 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? O7 C19 N14 125.9(6) . . ? O7 C19 N13 123.9(6) . . ? N14 C19 N13 110.1(5) . . ? N15 C20 N13 116.4(5) . . ? N15 C20 C21 103.2(5) . . ? N13 C20 C21 105.7(5) . . ? N15 C20 H20 110.4 . . ? N13 C20 H20 110.4 . . ? C21 C20 H20 110.4 . . ? N16 C21 N14 113.8(5) . . ? N16 C21 C20 104.9(5) . . ? N14 C21 C20 101.6(5) . . ? N16 C21 H21 111.9 . . ? N14 C21 H21 111.9 . . ? C20 C21 H21 111.9 . . ? O10 C22 N15 125.6(6) . . ? O10 C22 N16 125.4(6) . . ? N15 C22 N16 109.0(5) . . ? N17 C23 N14 113.6(5) . . ? N17 C23 H23A 108.8 . . ? N14 C23 H23A 108.8 . . ? N17 C23 H23B 108.8 . . ? N14 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? N16 C24 N19 114.7(5) . . ? N16 C24 H24A 108.6 . . ? N19 C24 H24A 108.6 . . ? N16 C24 H24B 108.6 . . ? N19 C24 H24B 108.6 . . ? H24A C24 H24B 107.6 . . ? O8 C25 N17 125.5(6) . . ? O8 C25 N18 124.0(6) . . ? N17 C25 N18 110.5(5) . . ? N17 C26 N19 114.4(5) . . ? N17 C26 C27 104.8(5) . . ? N19 C26 C27 103.4(5) . . ? N17 C26 H26 111.3 . . ? N19 C26 H26 111.3 . . ? C27 C26 H26 111.3 . . ? N20 C27 N18 113.3(5) . . ? N20 C27 C26 102.8(5) . . ? N18 C27 C26 102.0(5) . . ? N20 C27 H27 112.6 . . ? N18 C27 H27 112.6 . . ? C26 C27 H27 112.6 . . ? O11 C28 N19 126.5(7) . . ? O11 C28 N20 126.3(6) . . ? N19 C28 N20 107.1(6) . . ? N18 C29 N21 114.5(5) . . ? N18 C29 H29A 108.6 . . ? N21 C29 H29A 108.6 . . ? N18 C29 H29B 108.6 . . ? N21 C29 H29B 108.6 . . ? H29A C29 H29B 107.6 . . ? N23 C30 N20 113.9(5) . . ? N23 C30 H30A 108.8 . . ? N20 C30 H30A 108.8 . . ? N23 C30 H30B 108.8 . . ? N20 C30 H30B 108.8 . . ? H30A C30 H30B 107.7 . . ? O9 C31 N21 127.4(6) . . ? O9 C31 N22 125.0(6) . . ? N21 C31 N22 107.5(5) . . ? N21 C32 N23 114.8(5) . . ? N21 C32 C33 103.6(5) . . ? N23 C32 C33 104.1(5) . . ? N21 C32 H32 111.3 . . ? N23 C32 H32 111.3 . . ? C33 C32 H32 111.3 . . ? N22 C33 N24 114.9(5) . . ? N22 C33 C32 103.1(5) . . ? N24 C33 C32 103.2(5) . . ? N22 C33 H33 111.7 . . ? N24 C33 H33 111.7 . . ? C32 C33 H33 111.7 . . ? O12 C34 N24 126.2(6) . . ? O12 C34 N23 124.2(6) . . ? N24 C34 N23 109.6(6) . . ? N22 C35 N15 115.4(5) 2_675 . ? N22 C35 H35A 108.4 2_675 . ? N15 C35 H35A 108.4 . . ? N22 C35 H35B 108.4 2_675 . ? N15 C35 H35B 108.4 . . ? H35A C35 H35B 107.5 . . ? N13 C36 N24 115.6(5) . 2_675 ? N13 C36 H36A 108.4 . . ? N24 C36 H36A 108.4 2_675 . ? N13 C36 H36B 108.4 . . ? N24 C36 H36B 108.4 2_675 . ? H36A C36 H36B 107.4 . . ? C1 N1 C18 121.5(5) . . ? C1 N1 C2 112.8(5) . . ? C18 N1 C2 124.1(5) . . ? C1 N2 C5 123.4(5) . . ? C1 N2 C3 111.9(5) . . ? C5 N2 C3 124.7(5) . . ? C4 N3 C2 112.7(5) . . ? C4 N3 C17 122.3(5) . . ? C2 N3 C17 124.7(6) . . ? C4 N4 C6 124.5(6) . . ? C4 N4 C3 110.0(6) . . ? C6 N4 C3 124.3(6) . . ? C7 N5 C5 122.6(5) . . ? C7 N5 C8 113.0(5) . . ? C5 N5 C8 124.3(5) . . ? C7 N6 C11 123.0(5) . . ? C7 N6 C9 111.7(5) . . ? C11 N6 C9 123.6(5) . . ? C10 N7 C6 125.3(6) . . ? C10 N7 C8 112.4(6) . . ? C6 N7 C8 122.3(6) . . ? C10 N8 C9 115.0(6) . . ? C10 N8 C12 122.3(6) . . ? C9 N8 C12 121.7(6) . . ? C13 N9 C14 113.2(5) . . ? C13 N9 C11 124.5(5) . . ? C14 N9 C11 122.0(5) . . ? C13 N10 C17 123.5(5) . 2_576 ? C13 N10 C15 111.8(5) . . ? C17 N10 C15 123.2(5) 2_576 . ? C16 N11 C12 124.7(6) . . ? C16 N11 C14 110.7(5) . . ? C12 N11 C14 122.3(5) . . ? C16 N12 C18 121.7(5) . 2_576 ? C16 N12 C15 111.2(5) . . ? C18 N12 C15 125.7(5) 2_576 . ? C19 N13 C36 121.3(5) . . ? C19 N13 C20 110.1(5) . . ? C36 N13 C20 126.4(5) . . ? C19 N14 C23 124.2(5) . . ? C19 N14 C21 112.3(5) . . ? C23 N14 C21 123.4(5) . . ? C22 N15 C20 112.5(5) . . ? C22 N15 C35 122.8(5) . . ? C20 N15 C35 124.6(5) . . ? C22 N16 C24 122.3(6) . . ? C22 N16 C21 109.9(6) . . ? C24 N16 C21 127.5(6) . . ? C25 N17 C23 123.6(5) . . ? C25 N17 C26 110.5(5) . . ? C23 N17 C26 125.9(5) . . ? C25 N18 C29 122.2(5) . . ? C25 N18 C27 111.9(5) . . ? C29 N18 C27 123.8(5) . . ? C28 N19 C24 122.6(6) . . ? C28 N19 C26 112.7(6) . . ? C24 N19 C26 124.3(6) . . ? C28 N20 C27 113.8(5) . . ? C28 N20 C30 120.7(6) . . ? C27 N20 C30 124.8(6) . . ? C31 N21 C32 113.4(5) . . ? C31 N21 C29 122.3(5) . . ? C32 N21 C29 123.1(5) . . ? C31 N22 C35 123.5(5) . 2_675 ? C31 N22 C33 112.2(5) . . ? C35 N22 C33 122.5(5) 2_675 . ? C34 N23 C30 123.3(5) . . ? C34 N23 C32 110.4(5) . . ? C30 N23 C32 124.9(6) . . ? C34 N24 C36 121.8(5) . 2_675 ? C34 N24 C33 112.7(5) . . ? C36 N24 C33 125.0(5) 2_675 . ? C1 O1 Tm1 157.8(4) . . ? C7 O2 Tm1 156.8(5) . . ? C19 O7 Tm1 155.5(5) . . ? C25 O8 Tm1 156.9(4) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 4.137 _refine_diff_density_min -2.297 _refine_diff_density_rms 0.135 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.064 -0.500 0.444 1069 424 ' ' 2 0.000 0.000 0.500 94 27 ' ' 3 0.500 0.000 1.000 96 28 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 902624' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p314 #TrackingRef 'submit-314.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H94 Cl5 N24 O41 Yb Zn' _chemical_formula_weight 1935.01 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 '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 15.138(2) _cell_length_b 15.585(2) _cell_length_c 16.967(2) _cell_angle_alpha 64.023(5) _cell_angle_beta 80.796(5) _cell_angle_gamma 81.440(6) _cell_volume 3538.3(9) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.816 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1982 _exptl_absorpt_coefficient_mu 1.957 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6301 _exptl_absorpt_correction_T_max 0.6840 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38062 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0532 _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 -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12288 _reflns_number_gt 10208 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0919P)^2^+3.3457P] 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 12288 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1489 _refine_ls_wR_factor_gt 0.1435 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 Cl5 Cl 0.48889(14) 0.29581(18) 0.55040(17) 0.0830(6) Uani 1 1 d . . . O1W O 0.2100(4) 0.5883(4) 0.1909(4) 0.0837(19) Uani 1 1 d . . . O2W O 0.4316(3) 0.3661(3) 0.3593(3) 0.0458(10) Uani 1 1 d . . . O3W O 0.2411(3) 0.2619(3) 0.3920(3) 0.0497(11) Uani 1 1 d . . . O4W O 0.3932(3) 0.5142(3) 0.1987(3) 0.0495(11) Uani 1 1 d . . . O5W O 0.1338(3) 0.4344(4) 0.3368(3) 0.0521(11) Uani 1 1 d . . . Yb1 Yb 0.291108(15) 0.413241(18) 0.308712(15) 0.03308(10) Uani 1 1 d . . . Cl1 Cl -0.01217(14) 0.25682(18) 0.1546(2) 0.0924(8) Uani 1 1 d . . . Cl2 Cl -0.10900(15) 0.04028(17) 0.1918(2) 0.1117(11) Uani 1 1 d . . . Cl3 Cl 0.14059(15) 0.04748(19) 0.1652(2) 0.1204(12) Uani 1 1 d . . . Cl4 Cl 0.0163(5) 0.1837(4) -0.0245(2) 0.229(3) Uani 1 1 d . . . Zn1 Zn 0.00795(6) 0.12946(7) 0.12090(7) 0.0735(3) Uani 1 1 d . . . C17 C 0.0511(4) 0.8517(4) 0.3613(4) 0.0397(13) Uani 1 1 d . . . H17A H 0.0227 0.8721 0.4072 0.048 Uiso 1 1 calc R . . H17B H 0.0682 0.9093 0.3089 0.048 Uiso 1 1 calc R . . C18 C 0.1466(4) 0.7410(5) 0.2192(4) 0.0399(13) Uani 1 1 d . . . H18A H 0.1700 0.6996 0.1893 0.048 Uiso 1 1 calc R . . H18B H 0.1584 0.8069 0.1781 0.048 Uiso 1 1 calc R . . C35 C 0.2325(4) 0.6156(4) -0.1788(4) 0.0379(13) Uani 1 1 d . . . H35A H 0.2568 0.6057 -0.2316 0.046 Uiso 1 1 calc R . . H35B H 0.1726 0.6498 -0.1889 0.046 Uiso 1 1 calc R . . C36 C 0.1817(4) 0.6322(5) 0.0267(4) 0.0397(14) Uani 1 1 d . . . H36A H 0.1780 0.6309 0.0855 0.048 Uiso 1 1 calc R . . H36B H 0.1240 0.6615 0.0034 0.048 Uiso 1 1 calc R . . C1 C 0.2494(4) 0.6308(4) 0.3248(4) 0.0386(13) Uani 1 1 d . . . C2 C 0.2073(4) 0.7753(4) 0.3341(4) 0.0364(13) Uani 1 1 d . . . H2 H 0.2300 0.8362 0.2890 0.044 Uiso 1 1 calc R . . C3 C 0.2765(4) 0.7152(4) 0.4003(4) 0.0392(13) Uani 1 1 d . . . H3 H 0.3304 0.7498 0.3887 0.047 Uiso 1 1 calc R . . C4 C 0.1465(4) 0.7501(5) 0.4769(4) 0.0423(14) Uani 1 1 d . . . C5 C 0.3600(4) 0.5521(5) 0.4309(4) 0.0404(14) Uani 1 1 d . . . H5A H 0.4094 0.5774 0.4428 0.049 Uiso 1 1 calc R . . H5B H 0.3855 0.5199 0.3930 0.049 Uiso 1 1 calc R . . C6 C 0.2666(5) 0.6539(5) 0.5683(4) 0.0479(15) Uani 1 1 d . . . H6A H 0.2382 0.6848 0.6065 0.057 Uiso 1 1 calc R . . H6B H 0.3306 0.6641 0.5567 0.057 Uiso 1 1 calc R . . C7 C 0.2844(4) 0.4045(4) 0.5175(4) 0.0358(13) Uani 1 1 d . . . C8 C 0.3181(4) 0.4821(4) 0.5980(4) 0.0361(13) Uani 1 1 d . . . H8 H 0.3792 0.4828 0.6114 0.043 Uiso 1 1 calc R . . C9 C 0.2772(4) 0.3862(5) 0.6620(4) 0.0384(13) Uani 1 1 d . . . H9 H 0.3193 0.3424 0.7046 0.046 Uiso 1 1 calc R . . C10 C 0.1872(4) 0.5145(5) 0.6785(4) 0.0424(15) Uani 1 1 d . . . C11 C 0.2404(4) 0.2505(4) 0.6309(4) 0.0416(14) Uani 1 1 d . . . H11A H 0.2755 0.2091 0.6800 0.050 Uiso 1 1 calc R . . H11B H 0.2610 0.2318 0.5823 0.050 Uiso 1 1 calc R . . C12 C 0.1457(4) 0.3509(5) 0.7796(4) 0.0448(15) Uani 1 1 d . . . H12A H 0.1862 0.2991 0.8171 0.054 Uiso 1 1 calc R . . H12B H 0.1140 0.3848 0.8141 0.054 Uiso 1 1 calc R . . C13 C 0.0948(4) 0.2137(4) 0.6113(4) 0.0372(13) Uani 1 1 d . . . C14 C 0.1038(4) 0.2219(4) 0.7440(4) 0.0385(13) Uani 1 1 d . . . H14 H 0.1380 0.1727 0.7916 0.046 Uiso 1 1 calc R . . C15 C 0.0103(4) 0.1907(4) 0.7472(4) 0.0335(12) Uani 1 1 d . . . H15 H 0.0006 0.1267 0.7958 0.040 Uiso 1 1 calc R . . C16 C -0.0089(4) 0.3312(4) 0.7668(4) 0.0369(13) Uani 1 1 d . . . C19 C 0.2118(4) 0.4602(5) 0.1121(4) 0.0375(13) Uani 1 1 d . . . C20 C 0.1650(3) 0.5054(4) -0.0252(4) 0.0343(12) Uani 1 1 d . . . H20 H 0.1024 0.5312 -0.0378 0.041 Uiso 1 1 calc R . . C21 C 0.1725(4) 0.3968(5) 0.0237(4) 0.0404(14) Uani 1 1 d . . . H21 H 0.1143 0.3708 0.0315 0.049 Uiso 1 1 calc R . . C22 C 0.2651(4) 0.4410(5) -0.1083(4) 0.0388(13) Uani 1 1 d . . . C23 C 0.2141(4) 0.2861(4) 0.1799(4) 0.0369(13) Uani 1 1 d . . . H23A H 0.1727 0.2442 0.1785 0.044 Uiso 1 1 calc R . . H23B H 0.1990 0.2920 0.2358 0.044 Uiso 1 1 calc R . . C24 C 0.2720(5) 0.2675(5) -0.0143(4) 0.0476(16) Uani 1 1 d . . . H24A H 0.2223 0.2274 0.0170 0.057 Uiso 1 1 calc R . . H24B H 0.2894 0.2624 -0.0703 0.057 Uiso 1 1 calc R . . C25 C 0.3708(4) 0.2577(4) 0.2126(3) 0.0342(12) Uani 1 1 d . . . C26 C 0.3371(4) 0.1808(4) 0.1326(4) 0.0390(13) Uani 1 1 d . . . H26 H 0.3017 0.1248 0.1544 0.047 Uiso 1 1 calc R . . C27 C 0.4365(4) 0.1500(4) 0.1538(4) 0.0369(13) Uani 1 1 d . . . H27 H 0.4471 0.0800 0.1890 0.044 Uiso 1 1 calc R . . C28 C 0.4332(4) 0.2253(4) 0.0018(4) 0.0437(15) Uani 1 1 d . . . C29 C 0.5208(4) 0.1846(4) 0.2538(4) 0.0337(12) Uani 1 1 d . . . H29A H 0.5372 0.1153 0.2807 0.040 Uiso 1 1 calc R . . H29B H 0.5011 0.2047 0.3015 0.040 Uiso 1 1 calc R . . C30 C 0.5807(4) 0.1547(5) 0.0546(4) 0.0429(14) Uani 1 1 d . . . H30A H 0.5944 0.1586 -0.0052 0.051 Uiso 1 1 calc R . . H30B H 0.5945 0.0880 0.0959 0.051 Uiso 1 1 calc R . . C31 C 0.6283(4) 0.3050(4) 0.2154(4) 0.0385(13) Uani 1 1 d . . . C32 C 0.6640(4) 0.1973(4) 0.1507(4) 0.0386(13) Uani 1 1 d . . . H32 H 0.6840 0.1290 0.1847 0.046 Uiso 1 1 calc R . . C33 C 0.7424(4) 0.2620(4) 0.1247(4) 0.0333(12) Uani 1 1 d . . . H33 H 0.7992 0.2238 0.1458 0.040 Uiso 1 1 calc R . . C34 C 0.6883(4) 0.2791(4) -0.0033(4) 0.0375(13) Uani 1 1 d . . . N1 N 0.1945(3) 0.7122(3) 0.2960(3) 0.0351(10) Uani 1 1 d . . . N2 N 0.2983(3) 0.6301(3) 0.3848(3) 0.0370(11) Uani 1 1 d . . . N3 N 0.1314(3) 0.7912(4) 0.3914(3) 0.0431(12) Uani 1 1 d . . . N4 N 0.2281(3) 0.6992(4) 0.4871(3) 0.0471(13) Uani 1 1 d . . . N5 N 0.3207(3) 0.4829(4) 0.5127(3) 0.0387(11) Uani 1 1 d . . . N8 N 0.1981(3) 0.4163(4) 0.7047(3) 0.0408(12) Uani 1 1 d . . . N9 N 0.1461(3) 0.2326(4) 0.6588(3) 0.0398(11) Uani 1 1 d . . . N10 N 0.0138(3) 0.1901(4) 0.6599(3) 0.0393(11) Uani 1 1 d . . . N11 N 0.0816(3) 0.3101(4) 0.7560(3) 0.0395(11) Uani 1 1 d . . . N12 N -0.0511(3) 0.2642(3) 0.7591(3) 0.0381(11) Uani 1 1 d . . . N13 N 0.1944(3) 0.5361(4) 0.0355(3) 0.0373(11) Uani 1 1 d . . . N15 N 0.2008(3) 0.3791(4) 0.1086(3) 0.0378(11) Uani 1 1 d . . . N16 N 0.2230(3) 0.5221(4) -0.1044(3) 0.0389(11) Uani 1 1 d . . . N17 N 0.3040(3) 0.2424(3) 0.1770(3) 0.0362(11) Uani 1 1 d . . . N18 N 0.4473(3) 0.2041(3) 0.2026(3) 0.0348(10) Uani 1 1 d . . . N19 N 0.3454(3) 0.2307(4) 0.0364(3) 0.0408(11) Uani 1 1 d . . . N20 N 0.4852(3) 0.1810(4) 0.0692(3) 0.0400(11) Uani 1 1 d . . . N21 N 0.5999(3) 0.2326(3) 0.2026(3) 0.0364(11) Uani 1 1 d . . . N22 N 0.7105(3) 0.3244(4) 0.1681(3) 0.0384(11) Uani 1 1 d . . . N23 N 0.6380(3) 0.2143(4) 0.0654(3) 0.0409(11) Uani 1 1 d . . . N24 N 0.7481(3) 0.3074(4) 0.0301(3) 0.0403(11) Uani 1 1 d . . . N043 N 0.2406(3) 0.3648(4) -0.0326(3) 0.0422(12) Uani 1 1 d . . . N6 N 0.2593(3) 0.3468(4) 0.6028(3) 0.0445(12) Uani 1 1 d . . . N7 N 0.2575(4) 0.5525(4) 0.6146(4) 0.0525(14) Uani 1 1 d . . . O1 O 0.2554(3) 0.5654(3) 0.2999(3) 0.0401(9) Uani 1 1 d . . . O2 O 0.2777(3) 0.3876(3) 0.4544(3) 0.0401(9) Uani 1 1 d . . . O3 O 0.1162(3) 0.2135(3) 0.5392(3) 0.0527(11) Uani 1 1 d . . . O4 O 0.0934(4) 0.7584(4) 0.5385(3) 0.0668(14) Uani 1 1 d . . . O5 O 0.1300(3) 0.5578(4) 0.7069(3) 0.0532(11) Uani 1 1 d . . . O6 O -0.0460(3) 0.3984(3) 0.7829(3) 0.0434(10) Uani 1 1 d . . . O7 O 0.2321(3) 0.4675(3) 0.1779(3) 0.0400(9) Uani 1 1 d . . . O8 O 0.3634(3) 0.3101(3) 0.2504(3) 0.0404(9) Uani 1 1 d . . . O9 O 0.5890(3) 0.3432(3) 0.2616(3) 0.0473(10) Uani 1 1 d . . . O10 O 0.3146(3) 0.4354(3) -0.1718(3) 0.0490(11) Uani 1 1 d . . . O11 O 0.4593(4) 0.2555(4) -0.0766(3) 0.0618(13) Uani 1 1 d . . . O12 O 0.6813(3) 0.3041(3) -0.0816(3) 0.0475(10) 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 Cl5 0.0606(12) 0.0929(16) 0.0977(17) -0.0383(14) -0.0237(11) -0.0036(11) O1W 0.095(5) 0.081(4) 0.081(4) -0.047(4) 0.011(4) -0.002(3) O2W 0.036(2) 0.067(3) 0.035(2) -0.026(2) -0.0012(18) 0.004(2) O3W 0.056(3) 0.049(3) 0.042(2) -0.020(2) 0.007(2) -0.005(2) O4W 0.043(2) 0.057(3) 0.046(3) -0.022(2) 0.008(2) -0.009(2) O5W 0.044(2) 0.069(3) 0.042(3) -0.024(2) 0.003(2) -0.007(2) Yb1 0.03182(15) 0.04313(17) 0.02653(15) -0.01887(12) -0.00042(10) 0.00039(10) Cl1 0.0504(11) 0.0859(16) 0.138(2) -0.0430(16) -0.0127(12) -0.0099(10) Cl2 0.0571(12) 0.0607(14) 0.195(3) -0.0390(17) -0.0025(16) -0.0024(10) Cl3 0.0478(11) 0.0788(16) 0.148(3) 0.0245(16) 0.0046(13) 0.0006(10) Cl4 0.322(7) 0.208(5) 0.0609(19) -0.018(2) -0.015(3) 0.122(5) Zn1 0.0580(5) 0.0579(6) 0.0699(6) -0.0012(5) -0.0002(5) 0.0058(4) C17 0.043(3) 0.033(3) 0.043(3) -0.020(3) 0.003(3) -0.001(2) C18 0.034(3) 0.056(4) 0.030(3) -0.022(3) 0.007(2) -0.002(3) C35 0.039(3) 0.050(4) 0.028(3) -0.020(3) -0.006(2) -0.003(3) C36 0.035(3) 0.057(4) 0.029(3) -0.023(3) 0.007(2) -0.003(3) C1 0.036(3) 0.048(4) 0.029(3) -0.015(3) 0.003(2) -0.007(3) C2 0.034(3) 0.036(3) 0.038(3) -0.018(3) 0.005(2) -0.002(2) C3 0.035(3) 0.046(3) 0.040(3) -0.021(3) 0.002(3) -0.010(3) C4 0.044(3) 0.049(4) 0.039(3) -0.027(3) 0.007(3) -0.007(3) C5 0.024(3) 0.055(4) 0.041(3) -0.022(3) 0.002(2) -0.002(2) C6 0.052(4) 0.050(4) 0.051(4) -0.028(3) -0.002(3) -0.011(3) C7 0.027(3) 0.048(3) 0.030(3) -0.019(3) 0.000(2) 0.006(2) C8 0.036(3) 0.046(3) 0.034(3) -0.023(3) -0.008(2) -0.001(2) C9 0.032(3) 0.058(4) 0.028(3) -0.022(3) -0.006(2) 0.001(3) C10 0.035(3) 0.076(5) 0.027(3) -0.031(3) -0.001(2) -0.009(3) C11 0.031(3) 0.044(4) 0.045(4) -0.018(3) -0.005(3) 0.010(2) C12 0.041(3) 0.070(4) 0.025(3) -0.023(3) -0.002(2) -0.002(3) C13 0.040(3) 0.034(3) 0.031(3) -0.011(3) 0.000(3) 0.000(2) C14 0.036(3) 0.040(3) 0.034(3) -0.013(3) -0.007(2) 0.007(2) C15 0.036(3) 0.030(3) 0.026(3) -0.007(2) 0.002(2) 0.002(2) C16 0.038(3) 0.046(4) 0.022(3) -0.009(3) -0.005(2) -0.004(3) C19 0.025(3) 0.058(4) 0.028(3) -0.019(3) 0.002(2) 0.000(2) C20 0.024(3) 0.044(3) 0.030(3) -0.012(3) -0.004(2) 0.000(2) C21 0.029(3) 0.061(4) 0.036(3) -0.024(3) -0.002(2) -0.008(3) C22 0.040(3) 0.054(4) 0.029(3) -0.021(3) -0.008(3) -0.007(3) C23 0.032(3) 0.049(4) 0.031(3) -0.017(3) 0.002(2) -0.010(2) C24 0.058(4) 0.059(4) 0.039(3) -0.032(3) -0.005(3) -0.007(3) C25 0.040(3) 0.035(3) 0.024(3) -0.011(2) 0.002(2) -0.006(2) C26 0.048(3) 0.030(3) 0.040(3) -0.015(3) -0.003(3) -0.007(2) C27 0.044(3) 0.031(3) 0.038(3) -0.016(3) -0.004(3) -0.001(2) C28 0.050(4) 0.038(3) 0.048(4) -0.024(3) 0.002(3) -0.007(3) C29 0.036(3) 0.038(3) 0.027(3) -0.012(2) -0.002(2) -0.006(2) C30 0.047(3) 0.045(4) 0.043(4) -0.027(3) -0.005(3) 0.005(3) C31 0.038(3) 0.043(3) 0.032(3) -0.015(3) -0.006(3) 0.004(3) C32 0.038(3) 0.041(3) 0.033(3) -0.013(3) -0.007(2) 0.005(2) C33 0.030(3) 0.040(3) 0.031(3) -0.019(3) -0.002(2) -0.001(2) C34 0.037(3) 0.041(3) 0.037(3) -0.022(3) -0.001(3) 0.005(2) N1 0.038(3) 0.035(3) 0.031(3) -0.013(2) -0.004(2) -0.002(2) N2 0.037(3) 0.041(3) 0.039(3) -0.021(2) -0.005(2) -0.004(2) N3 0.045(3) 0.050(3) 0.039(3) -0.027(3) 0.001(2) 0.000(2) N4 0.043(3) 0.066(4) 0.037(3) -0.029(3) 0.001(2) -0.003(3) N5 0.036(3) 0.050(3) 0.027(2) -0.015(2) -0.002(2) 0.001(2) N8 0.036(3) 0.058(3) 0.033(3) -0.023(2) 0.001(2) -0.010(2) N9 0.040(3) 0.045(3) 0.029(3) -0.013(2) 0.003(2) -0.006(2) N10 0.044(3) 0.041(3) 0.033(3) -0.017(2) 0.002(2) -0.005(2) N11 0.033(2) 0.057(3) 0.029(3) -0.020(2) -0.004(2) 0.000(2) N12 0.041(3) 0.040(3) 0.034(3) -0.016(2) -0.004(2) -0.002(2) N13 0.036(2) 0.044(3) 0.035(3) -0.020(2) -0.007(2) 0.001(2) N15 0.044(3) 0.045(3) 0.028(2) -0.017(2) -0.006(2) -0.006(2) N16 0.044(3) 0.045(3) 0.030(3) -0.019(2) -0.005(2) -0.001(2) N17 0.031(2) 0.041(3) 0.039(3) -0.020(2) -0.002(2) -0.002(2) N18 0.038(3) 0.035(3) 0.034(3) -0.019(2) -0.005(2) 0.002(2) N19 0.043(3) 0.049(3) 0.035(3) -0.025(2) 0.000(2) 0.002(2) N20 0.037(3) 0.048(3) 0.038(3) -0.024(2) 0.001(2) 0.000(2) N21 0.034(2) 0.041(3) 0.032(3) -0.015(2) 0.002(2) -0.002(2) N22 0.036(3) 0.051(3) 0.031(3) -0.021(2) 0.001(2) -0.004(2) N23 0.044(3) 0.044(3) 0.037(3) -0.021(2) -0.001(2) -0.003(2) N24 0.036(3) 0.049(3) 0.035(3) -0.019(2) 0.001(2) -0.004(2) N043 0.044(3) 0.051(3) 0.034(3) -0.022(3) 0.002(2) -0.008(2) N6 0.040(3) 0.059(3) 0.038(3) -0.024(3) -0.008(2) 0.002(2) N7 0.051(3) 0.073(4) 0.041(3) -0.031(3) -0.001(3) -0.010(3) O1 0.046(2) 0.046(2) 0.036(2) -0.025(2) -0.0017(18) -0.0026(18) O2 0.045(2) 0.052(3) 0.029(2) -0.0242(19) -0.0012(17) -0.0013(19) O3 0.054(3) 0.067(3) 0.045(3) -0.033(2) 0.007(2) -0.008(2) O4 0.064(3) 0.086(4) 0.048(3) -0.035(3) 0.002(2) 0.010(3) O5 0.051(3) 0.067(3) 0.054(3) -0.039(3) -0.003(2) -0.001(2) O6 0.045(2) 0.047(3) 0.044(2) -0.025(2) -0.0083(19) 0.0053(19) O7 0.042(2) 0.053(3) 0.032(2) -0.025(2) -0.0089(18) 0.0041(18) O8 0.041(2) 0.053(3) 0.038(2) -0.032(2) -0.0021(18) 0.0039(18) O9 0.044(2) 0.064(3) 0.041(2) -0.034(2) 0.0078(19) -0.004(2) O10 0.048(2) 0.066(3) 0.036(2) -0.028(2) -0.001(2) -0.001(2) O11 0.074(3) 0.071(3) 0.037(3) -0.025(2) -0.002(2) 0.003(3) O12 0.057(3) 0.053(3) 0.036(2) -0.022(2) -0.005(2) -0.008(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 O1W Yb1 2.820(6) . ? O2W Yb1 2.317(4) . ? O3W Yb1 2.324(4) . ? O4W Yb1 2.361(4) . ? O5W Yb1 2.356(4) . ? Yb1 O7 2.282(4) . ? Yb1 O8 2.298(4) . ? Yb1 O1 2.295(4) . ? Yb1 O2 2.304(4) . ? Cl1 Zn1 2.262(3) . ? Cl2 Zn1 2.258(3) . ? Cl3 Zn1 2.260(2) . ? Cl4 Zn1 2.219(4) . ? C17 N10 1.423(7) 2_566 ? C17 N3 1.437(8) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N1 1.454(7) . ? C18 N12 1.440(7) 2_566 ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C35 N22 1.446(7) 2_665 ? C35 N16 1.460(8) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N13 1.425(8) . ? C36 N24 1.456(7) 2_665 ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C1 O1 1.250(7) . ? C1 N1 1.347(8) . ? C1 N2 1.347(7) . ? C2 N3 1.448(7) . ? C2 N1 1.442(7) . ? C2 C3 1.549(9) . ? C2 H2 0.9900 . ? C3 N2 1.445(7) . ? C3 N4 1.468(7) . ? C3 H3 0.9900 . ? C4 O4 1.254(7) . ? C4 N3 1.348(8) . ? C4 N4 1.356(8) . ? C5 N2 1.424(8) . ? C5 N5 1.435(8) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.421(9) . ? C6 N7 1.442(9) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.231(7) . ? C7 N6 1.355(8) . ? C7 N5 1.379(8) . ? C8 N7 1.419(8) . ? C8 N5 1.435(7) . ? C8 C9 1.560(8) . ? C8 H8 0.9900 . ? C9 N8 1.425(7) . ? C9 N6 1.460(7) . ? C9 H9 0.9900 . ? C10 O5 1.189(7) . ? C10 N8 1.386(9) . ? C10 N7 1.384(8) . ? C11 N6 1.421(8) . ? C11 N9 1.458(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.426(8) . ? C12 N8 1.438(8) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.217(7) . ? C13 N9 1.348(8) . ? C13 N10 1.365(7) . ? C14 N9 1.432(7) . ? C14 N11 1.459(8) . ? C14 C15 1.550(8) . ? C14 H14 0.9900 . ? C15 N12 1.430(7) . ? C15 N10 1.478(7) . ? C15 H15 0.9900 . ? C16 O6 1.231(7) . ? C16 N11 1.363(7) . ? C16 N12 1.363(7) . ? C19 O7 1.258(7) . ? C19 N15 1.328(8) . ? C19 N13 1.353(8) . ? C20 N16 1.424(7) . ? C20 N13 1.459(7) . ? C20 C21 1.520(9) . ? C20 H20 0.9900 . ? C21 N15 1.466(7) . ? C21 N043 1.474(7) . ? C21 H21 0.9900 . ? C22 O10 1.239(7) . ? C22 N043 1.357(8) . ? C22 N16 1.351(8) . ? C23 N15 1.435(8) . ? C23 N17 1.432(7) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N19 1.410(8) . ? C24 N043 1.429(8) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O8 1.225(6) . ? C25 N18 1.357(7) . ? C25 N17 1.355(7) . ? C26 N17 1.453(7) . ? C26 N19 1.460(8) . ? C26 C27 1.559(8) . ? C26 H26 0.9900 . ? C27 N20 1.414(7) . ? C27 N18 1.456(7) . ? C27 H27 0.9900 . ? C28 O11 1.218(8) . ? C28 N20 1.356(8) . ? C28 N19 1.371(8) . ? C29 N18 1.437(7) . ? C29 N21 1.454(7) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N20 1.454(8) . ? C30 N23 1.447(8) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O9 1.214(7) . ? C31 N22 1.365(7) . ? C31 N21 1.376(7) . ? C32 N21 1.419(7) . ? C32 N23 1.460(7) . ? C32 C33 1.555(8) . ? C32 H32 0.9900 . ? C33 N24 1.436(7) . ? C33 N22 1.447(7) . ? C33 H33 0.9900 . ? C34 O12 1.228(7) . ? C34 N24 1.355(7) . ? C34 N23 1.368(8) . ? N10 C17 1.423(7) 2_566 ? N12 C18 1.440(7) 2_566 ? N22 C35 1.446(7) 2_665 ? N24 C36 1.456(7) 2_665 ? 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 Yb1 O8 77.25(14) . . ? O7 Yb1 O1 86.81(14) . . ? O8 Yb1 O1 150.72(15) . . ? O7 Yb1 O2 150.87(14) . . ? O8 Yb1 O2 126.39(15) . . ? O1 Yb1 O2 77.61(14) . . ? O7 Yb1 O2W 137.66(14) . . ? O8 Yb1 O2W 72.97(14) . . ? O1 Yb1 O2W 105.22(15) . . ? O2 Yb1 O2W 70.91(14) . . ? O7 Yb1 O3W 104.82(15) . . ? O8 Yb1 O3W 70.81(15) . . ? O1 Yb1 O3W 137.81(14) . . ? O2 Yb1 O3W 73.03(15) . . ? O2W Yb1 O3W 93.11(16) . . ? O7 Yb1 O5W 72.22(15) . . ? O8 Yb1 O5W 123.65(15) . . ? O1 Yb1 O5W 72.58(15) . . ? O2 Yb1 O5W 79.64(15) . . ? O2W Yb1 O5W 150.07(15) . . ? O3W Yb1 O5W 72.86(16) . . ? O7 Yb1 O4W 72.99(15) . . ? O8 Yb1 O4W 79.88(15) . . ? O1 Yb1 O4W 71.97(15) . . ? O2 Yb1 O4W 123.40(15) . . ? O2W Yb1 O4W 72.70(16) . . ? O3W Yb1 O4W 150.18(16) . . ? O5W Yb1 O4W 130.93(16) . . ? O7 Yb1 O1W 43.68(15) . . ? O8 Yb1 O1W 117.01(15) . . ? O1 Yb1 O1W 43.13(15) . . ? O2 Yb1 O1W 116.60(15) . . ? O2W Yb1 O1W 133.69(17) . . ? O3W Yb1 O1W 133.20(17) . . ? O5W Yb1 O1W 65.14(17) . . ? O4W Yb1 O1W 65.80(16) . . ? Cl4 Zn1 Cl3 108.25(18) . . ? Cl4 Zn1 Cl1 108.27(18) . . ? Cl3 Zn1 Cl1 108.09(13) . . ? Cl4 Zn1 Cl2 112.8(2) . . ? Cl3 Zn1 Cl2 111.99(10) . . ? Cl1 Zn1 Cl2 107.24(11) . . ? N10 C17 N3 115.8(5) 2_566 . ? N10 C17 H17A 108.3 2_566 . ? N3 C17 H17A 108.3 . . ? N10 C17 H17B 108.3 2_566 . ? N3 C17 H17B 108.3 . . ? H17A C17 H17B 107.4 . . ? N1 C18 N12 113.1(4) . 2_566 ? N1 C18 H18A 109.0 . . ? N12 C18 H18A 109.0 2_566 . ? N1 C18 H18B 109.0 . . ? N12 C18 H18B 109.0 2_566 . ? H18A C18 H18B 107.8 . . ? N22 C35 N16 115.0(5) 2_665 . ? N22 C35 H35A 108.5 2_665 . ? N16 C35 H35A 108.5 . . ? N22 C35 H35B 108.5 2_665 . ? N16 C35 H35B 108.5 . . ? H35A C35 H35B 107.5 . . ? N13 C36 N24 114.7(5) . 2_665 ? N13 C36 H36A 108.6 . . ? N24 C36 H36A 108.6 2_665 . ? N13 C36 H36B 108.6 . . ? N24 C36 H36B 108.6 2_665 . ? H36A C36 H36B 107.6 . . ? O1 C1 N1 125.9(5) . . ? O1 C1 N2 124.4(6) . . ? N1 C1 N2 109.6(5) . . ? N3 C2 N1 115.2(5) . . ? N3 C2 C3 101.9(5) . . ? N1 C2 C3 102.9(4) . . ? N3 C2 H2 112.0 . . ? N1 C2 H2 112.0 . . ? C3 C2 H2 112.0 . . ? N2 C3 N4 114.6(5) . . ? N2 C3 C2 103.1(4) . . ? N4 C3 C2 104.6(5) . . ? N2 C3 H3 111.3 . . ? N4 C3 H3 111.3 . . ? C2 C3 H3 111.3 . . ? O4 C4 N3 125.0(6) . . ? O4 C4 N4 124.6(6) . . ? N3 C4 N4 110.3(5) . . ? N2 C5 N5 113.7(5) . . ? N2 C5 H5A 108.8 . . ? N5 C5 H5A 108.8 . . ? N2 C5 H5B 108.8 . . ? N5 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N4 C6 N7 114.2(5) . . ? N4 C6 H6A 108.7 . . ? N7 C6 H6A 108.7 . . ? N4 C6 H6B 108.7 . . ? N7 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? O2 C7 N6 124.8(6) . . ? O2 C7 N5 125.6(5) . . ? N6 C7 N5 109.6(5) . . ? N7 C8 N5 116.4(5) . . ? N7 C8 C9 103.4(5) . . ? N5 C8 C9 103.5(4) . . ? N7 C8 H8 111.0 . . ? N5 C8 H8 111.0 . . ? C9 C8 H8 111.0 . . ? N8 C9 N6 113.8(5) . . ? N8 C9 C8 103.5(5) . . ? N6 C9 C8 103.4(4) . . ? N8 C9 H9 111.8 . . ? N6 C9 H9 111.8 . . ? C8 C9 H9 111.8 . . ? O5 C10 N8 126.8(6) . . ? O5 C10 N7 126.5(7) . . ? N8 C10 N7 106.6(5) . . ? N6 C11 N9 115.2(5) . . ? N6 C11 H11A 108.5 . . ? N9 C11 H11A 108.5 . . ? N6 C11 H11B 108.5 . . ? N9 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? N11 C12 N8 113.3(5) . . ? N11 C12 H12A 108.9 . . ? N8 C12 H12A 108.9 . . ? N11 C12 H12B 108.9 . . ? N8 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N9 127.2(5) . . ? O3 C13 N10 124.6(5) . . ? N9 C13 N10 108.2(5) . . ? N9 C14 N11 115.9(5) . . ? N9 C14 C15 103.1(4) . . ? N11 C14 C15 103.0(4) . . ? N9 C14 H14 111.4 . . ? N11 C14 H14 111.4 . . ? C15 C14 H14 111.4 . . ? N12 C15 N10 114.4(5) . . ? N12 C15 C14 103.7(4) . . ? N10 C15 C14 102.6(4) . . ? N12 C15 H15 111.8 . . ? N10 C15 H15 111.8 . . ? C14 C15 H15 111.8 . . ? O6 C16 N11 125.4(5) . . ? O6 C16 N12 125.8(5) . . ? N11 C16 N12 108.7(5) . . ? O7 C19 N15 125.8(6) . . ? O7 C19 N13 123.8(6) . . ? N15 C19 N13 110.4(5) . . ? N16 C20 N13 115.8(4) . . ? N16 C20 C21 103.0(5) . . ? N13 C20 C21 103.6(4) . . ? N16 C20 H20 111.3 . . ? N13 C20 H20 111.3 . . ? C21 C20 H20 111.3 . . ? N15 C21 N043 114.6(5) . . ? N15 C21 C20 103.3(5) . . ? N043 C21 C20 104.2(5) . . ? N15 C21 H21 111.4 . . ? N043 C21 H21 111.4 . . ? C20 C21 H21 111.4 . . ? O10 C22 N043 124.6(6) . . ? O10 C22 N16 126.3(6) . . ? N043 C22 N16 108.9(5) . . ? N15 C23 N17 113.5(5) . . ? N15 C23 H23A 108.9 . . ? N17 C23 H23A 108.9 . . ? N15 C23 H23B 108.9 . . ? N17 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? N19 C24 N043 114.8(5) . . ? N19 C24 H24A 108.6 . . ? N043 C24 H24A 108.6 . . ? N19 C24 H24B 108.6 . . ? N043 C24 H24B 108.6 . . ? H24A C24 H24B 107.6 . . ? O8 C25 N18 124.4(5) . . ? O8 C25 N17 125.5(5) . . ? N18 C25 N17 110.1(5) . . ? N17 C26 N19 114.2(5) . . ? N17 C26 C27 104.0(4) . . ? N19 C26 C27 103.4(5) . . ? N17 C26 H26 111.6 . . ? N19 C26 H26 111.6 . . ? C27 C26 H26 111.6 . . ? N20 C27 N18 114.4(5) . . ? N20 C27 C26 102.8(5) . . ? N18 C27 C26 102.3(4) . . ? N20 C27 H27 112.1 . . ? N18 C27 H27 112.1 . . ? C26 C27 H27 112.1 . . ? O11 C28 N20 126.2(6) . . ? O11 C28 N19 125.3(6) . . ? N20 C28 N19 108.5(5) . . ? N18 C29 N21 113.5(4) . . ? N18 C29 H29A 108.9 . . ? N21 C29 H29A 108.9 . . ? N18 C29 H29B 108.9 . . ? N21 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? N20 C30 N23 113.9(5) . . ? N20 C30 H30A 108.8 . . ? N23 C30 H30A 108.8 . . ? N20 C30 H30B 108.8 . . ? N23 C30 H30B 108.8 . . ? H30A C30 H30B 107.7 . . ? O9 C31 N22 126.2(5) . . ? O9 C31 N21 126.8(5) . . ? N22 C31 N21 107.0(5) . . ? N21 C32 N23 115.6(5) . . ? N21 C32 C33 103.4(5) . . ? N23 C32 C33 103.0(5) . . ? N21 C32 H32 111.4 . . ? N23 C32 H32 111.4 . . ? C33 C32 H32 111.4 . . ? N24 C33 N22 115.4(5) . . ? N24 C33 C32 103.1(4) . . ? N22 C33 C32 102.7(4) . . ? N24 C33 H33 111.6 . . ? N22 C33 H33 111.6 . . ? C32 C33 H33 111.6 . . ? O12 C34 N24 126.7(6) . . ? O12 C34 N23 124.9(5) . . ? N24 C34 N23 108.3(5) . . ? C1 N1 C18 121.6(5) . . ? C1 N1 C2 112.2(5) . . ? C18 N1 C2 124.4(5) . . ? C1 N2 C5 123.8(5) . . ? C1 N2 C3 111.9(5) . . ? C5 N2 C3 124.2(5) . . ? C4 N3 C17 122.2(5) . . ? C4 N3 C2 113.0(5) . . ? C17 N3 C2 124.5(5) . . ? C4 N4 C6 123.8(5) . . ? C4 N4 C3 109.7(5) . . ? C6 N4 C3 125.2(5) . . ? C7 N5 C8 111.9(5) . . ? C7 N5 C5 121.8(5) . . ? C8 N5 C5 126.2(5) . . ? C10 N8 C12 122.7(5) . . ? C10 N8 C9 113.0(5) . . ? C12 N8 C9 123.2(5) . . ? C13 N9 C14 114.3(5) . . ? C13 N9 C11 122.9(5) . . ? C14 N9 C11 122.4(5) . . ? C13 N10 C17 123.9(5) . 2_566 ? C13 N10 C15 111.8(5) . . ? C17 N10 C15 122.7(5) 2_566 . ? C16 N11 C12 123.7(5) . . ? C16 N11 C14 111.8(5) . . ? C12 N11 C14 122.0(5) . . ? C16 N12 C15 112.7(5) . . ? C16 N12 C18 121.4(5) . 2_566 ? C15 N12 C18 124.5(5) . 2_566 ? C19 N13 C36 122.6(5) . . ? C19 N13 C20 111.0(5) . . ? C36 N13 C20 124.1(5) . . ? C19 N15 C23 123.7(5) . . ? C19 N15 C21 111.6(5) . . ? C23 N15 C21 124.7(5) . . ? C22 N16 C20 113.6(5) . . ? C22 N16 C35 121.4(5) . . ? C20 N16 C35 124.8(5) . . ? C25 N17 C23 123.4(5) . . ? C25 N17 C26 111.1(5) . . ? C23 N17 C26 125.4(5) . . ? C25 N18 C29 122.3(5) . . ? C25 N18 C27 112.2(4) . . ? C29 N18 C27 123.6(5) . . ? C28 N19 C24 124.2(5) . . ? C28 N19 C26 110.9(5) . . ? C24 N19 C26 124.3(5) . . ? C28 N20 C27 114.1(5) . . ? C28 N20 C30 122.0(5) . . ? C27 N20 C30 123.2(5) . . ? C31 N21 C32 113.7(5) . . ? C31 N21 C29 121.5(5) . . ? C32 N21 C29 123.6(5) . . ? C31 N22 C35 121.9(5) . 2_665 ? C31 N22 C33 113.1(5) . . ? C35 N22 C33 123.4(5) 2_665 . ? C34 N23 C32 112.0(5) . . ? C34 N23 C30 123.3(5) . . ? C32 N23 C30 123.3(5) . . ? C34 N24 C33 113.5(5) . . ? C34 N24 C36 121.5(5) . 2_665 ? C33 N24 C36 124.5(5) . 2_665 ? C22 N043 C24 124.2(5) . . ? C22 N043 C21 110.1(5) . . ? C24 N043 C21 125.6(5) . . ? C7 N6 C11 122.5(5) . . ? C7 N6 C9 111.5(5) . . ? C11 N6 C9 124.1(5) . . ? C10 N7 C8 113.4(6) . . ? C10 N7 C6 122.9(6) . . ? C8 N7 C6 123.6(5) . . ? C1 O1 Yb1 156.2(4) . . ? C7 O2 Yb1 156.9(4) . . ? C19 O7 Yb1 154.8(4) . . ? C25 O8 Yb1 156.7(4) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.073 _refine_diff_density_min -1.285 _refine_diff_density_rms 0.115 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.064 -0.500 0.444 1069 424 ' ' 2 0.000 0.000 0.500 94 27 ' ' 3 0.500 0.000 1.000 96 28 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 902625' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p315 #TrackingRef 'submit-315.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H100 Cl5 Lu N24 O44 Zn' _chemical_formula_weight 1990.99 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Lu Lu -0.4720 5.8584 '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 15.1379(10) _cell_length_b 15.6777(11) _cell_length_c 16.9861(12) _cell_angle_alpha 63.936(2) _cell_angle_beta 80.761(2) _cell_angle_gamma 81.111(2) _cell_volume 3558.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.858 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2044 _exptl_absorpt_coefficient_mu 2.025 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6315 _exptl_absorpt_correction_T_max 0.6996 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39833 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0535 _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 -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12438 _reflns_number_gt 10406 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0817P)^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 12438 _refine_ls_number_parameters 748 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0526 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1238 _refine_ls_wR_factor_gt 0.1187 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _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 Cl5 Cl 1.01070(12) 0.70467(15) 0.94924(14) 0.0819(5) Uani 1 1 d . . . O1W O 0.7426(2) 0.2647(2) 0.8902(2) 0.0458(8) Uani 1 1 d . . . O2W O 0.9328(2) 0.3675(3) 0.8597(2) 0.0446(8) Uani 1 1 d . . . O3W O 0.6357(2) 0.4356(3) 0.8376(2) 0.0475(9) Uani 1 1 d . . . O4W O 0.8933(2) 0.5139(3) 0.6995(2) 0.0459(8) Uani 1 1 d . . . Lu1 Lu 0.791720(12) 0.414870(14) 0.808298(11) 0.03283(9) Uani 1 1 d . . . Cl1 Cl 0.48863(12) 0.25600(15) 0.65497(17) 0.0949(6) Uani 1 1 d . . . Cl2 Cl 0.39308(13) 0.04077(14) 0.69145(19) 0.1078(8) Uani 1 1 d . . . Cl3 Cl 0.64213(13) 0.04598(16) 0.66711(19) 0.1359(12) Uani 1 1 d . . . Cl4 Cl 0.5162(4) 0.1829(3) 0.47595(18) 0.248(3) Uani 1 1 d . . . Zn1 Zn 0.50977(5) 0.12929(6) 0.62115(5) 0.0766(3) Uani 1 1 d . . . C1 C 0.7114(3) 0.4623(4) 0.6131(3) 0.0358(11) Uani 1 1 d . . . C2 C 0.6644(3) 0.5077(3) 0.4751(3) 0.0346(10) Uani 1 1 d . . . H2 H 0.6017 0.5336 0.4627 0.042 Uiso 1 1 calc R . . C3 C 0.6723(3) 0.3990(4) 0.5240(3) 0.0373(11) Uani 1 1 d . . . H3 H 0.6142 0.3731 0.5320 0.045 Uiso 1 1 calc R . . C4 C 0.7643(3) 0.4418(4) 0.3925(3) 0.0415(12) Uani 1 1 d . . . C5 C 0.7141(3) 0.2884(3) 0.6798(3) 0.0364(10) Uani 1 1 d . . . H5A H 0.6985 0.2936 0.7359 0.044 Uiso 1 1 calc R . . H5B H 0.6730 0.2472 0.6775 0.044 Uiso 1 1 calc R . . C6 C 0.7702(4) 0.2689(4) 0.4860(3) 0.0453(12) Uani 1 1 d . . . H6A H 0.7201 0.2296 0.5166 0.054 Uiso 1 1 calc R . . H6B H 0.7879 0.2643 0.4298 0.054 Uiso 1 1 calc R . . C7 C 0.8711(3) 0.2584(3) 0.7132(3) 0.0316(10) Uani 1 1 d . . . C8 C 0.8372(3) 0.1826(3) 0.6330(3) 0.0368(10) Uani 1 1 d . . . H8 H 0.8018 0.1270 0.6551 0.044 Uiso 1 1 calc R . . C9 C 0.9359(3) 0.1519(3) 0.6552(3) 0.0360(10) Uani 1 1 d . . . H9 H 0.9461 0.0823 0.6913 0.043 Uiso 1 1 calc R . . C10 C 0.9330(3) 0.2268(4) 0.5025(3) 0.0409(11) Uani 1 1 d . . . C11 C 1.0221(3) 0.1860(3) 0.7533(3) 0.0341(10) Uani 1 1 d . . . H11A H 1.0026 0.2047 0.8019 0.041 Uiso 1 1 calc R . . H11B H 1.0389 0.1171 0.7792 0.041 Uiso 1 1 calc R . . C12 C 1.0804(3) 0.1557(4) 0.5557(4) 0.0437(12) Uani 1 1 d . . . H12A H 1.0940 0.1600 0.4958 0.052 Uiso 1 1 calc R . . H12B H 1.0949 0.0892 0.5966 0.052 Uiso 1 1 calc R . . C13 C 1.1288(3) 0.3053(3) 0.7153(3) 0.0353(10) Uani 1 1 d . . . C14 C 1.1654(3) 0.1974(3) 0.6511(3) 0.0370(11) Uani 1 1 d . . . H14 H 1.1861 0.1294 0.6849 0.044 Uiso 1 1 calc R . . C15 C 1.2422(3) 0.2622(4) 0.6252(3) 0.0370(11) Uani 1 1 d . . . H15 H 1.2994 0.2245 0.6460 0.044 Uiso 1 1 calc R . . C16 C 1.1878(3) 0.2785(3) 0.4972(3) 0.0364(11) Uani 1 1 d . . . C17 C 1.2683(3) 0.3835(4) 0.6785(3) 0.0399(11) Uani 1 1 d . . . H17A H 1.3282 0.3490 0.6879 0.048 Uiso 1 1 calc R . . H17B H 1.2447 0.3928 0.7317 0.048 Uiso 1 1 calc R . . C18 C 1.3187(3) 0.3649(4) 0.4746(3) 0.0377(11) Uani 1 1 d . . . H18A H 1.3232 0.3657 0.4161 0.045 Uiso 1 1 calc R . . H18B H 1.3758 0.3350 0.4992 0.045 Uiso 1 1 calc R . . C19 C 0.7488(3) 0.6298(3) 0.8247(3) 0.0342(10) Uani 1 1 d . . . C20 C 0.7077(3) 0.7754(3) 0.8351(3) 0.0375(11) Uani 1 1 d . . . H20 H 0.7309 0.8359 0.7907 0.045 Uiso 1 1 calc R . . C21 C 0.7748(3) 0.7145(4) 0.9013(3) 0.0391(11) Uani 1 1 d . . . H21 H 0.8285 0.7486 0.8906 0.047 Uiso 1 1 calc R . . C22 C 0.6462(4) 0.7494(4) 0.9775(3) 0.0449(12) Uani 1 1 d . . . C23 C 0.8600(3) 0.5535(4) 0.9299(3) 0.0387(11) Uani 1 1 d . . . H23A H 0.9087 0.5784 0.9427 0.046 Uiso 1 1 calc R . . H23B H 0.8864 0.5223 0.8915 0.046 Uiso 1 1 calc R . . C24 C 0.7670(4) 0.6539(4) 1.0680(3) 0.0443(12) Uani 1 1 d . . . H24A H 0.8310 0.6641 1.0563 0.053 Uiso 1 1 calc R . . H24B H 0.7384 0.6844 1.1064 0.053 Uiso 1 1 calc R . . C25 C 0.7848(3) 0.4061(3) 1.0169(3) 0.0327(10) Uani 1 1 d . . . C26 C 0.8194(3) 0.4818(4) 1.0984(3) 0.0380(11) Uani 1 1 d . . . H26 H 0.8808 0.4821 1.1114 0.046 Uiso 1 1 calc R . . C27 C 0.7788(3) 0.3863(4) 1.1612(3) 0.0388(11) Uani 1 1 d . . . H27 H 0.8208 0.3418 1.2037 0.047 Uiso 1 1 calc R . . C28 C 0.6878(3) 0.5132(4) 1.1780(3) 0.0423(12) Uani 1 1 d . . . C29 C 0.7420(3) 0.2521(4) 1.1313(3) 0.0413(11) Uani 1 1 d . . . H29A H 0.7767 0.2115 1.1809 0.050 Uiso 1 1 calc R . . H29B H 0.7631 0.2325 1.0835 0.050 Uiso 1 1 calc R . . C30 C 0.6474(3) 0.3527(4) 1.2791(3) 0.0434(12) Uani 1 1 d . . . H30A H 0.6149 0.3869 1.3130 0.052 Uiso 1 1 calc R . . H30B H 0.6886 0.3021 1.3170 0.052 Uiso 1 1 calc R . . C31 C 0.5950(3) 0.2150(3) 1.1114(3) 0.0347(10) Uani 1 1 d . . . C32 C 0.6057(3) 0.2234(3) 1.2435(3) 0.0360(10) Uani 1 1 d . . . H32 H 0.6405 0.1744 1.2906 0.043 Uiso 1 1 calc R . . C33 C 0.5122(3) 0.1907(3) 1.2467(3) 0.0330(10) Uani 1 1 d . . . H33 H 0.5030 0.1268 1.2949 0.040 Uiso 1 1 calc R . . C34 C 0.4921(3) 0.3319(4) 1.2668(3) 0.0377(11) Uani 1 1 d . . . C35 C 0.5494(3) 0.8512(3) 0.8606(3) 0.0397(11) Uani 1 1 d . . . H35A H 0.5662 0.9081 0.8077 0.048 Uiso 1 1 calc R . . H35B H 0.5210 0.8721 0.9060 0.048 Uiso 1 1 calc R . . C36 C 0.6453(3) 0.7420(4) 0.7193(3) 0.0383(11) Uani 1 1 d . . . H36A H 0.6555 0.8084 0.6798 0.046 Uiso 1 1 calc R . . H36B H 0.6698 0.7029 0.6875 0.046 Uiso 1 1 calc R . . N1 N 0.6943(3) 0.5384(3) 0.5347(2) 0.0355(9) Uani 1 1 d . . . N2 N 0.7012(3) 0.3815(3) 0.6087(2) 0.0349(9) Uani 1 1 d . . . N3 N 0.7229(3) 0.5241(3) 0.3946(2) 0.0363(9) Uani 1 1 d . . . N4 N 0.7395(3) 0.3681(3) 0.4683(3) 0.0415(10) Uani 1 1 d . . . N5 N 0.8043(3) 0.2444(3) 0.6774(3) 0.0371(9) Uani 1 1 d . . . N6 N 0.9475(3) 0.2060(3) 0.7030(2) 0.0355(9) Uani 1 1 d . . . N7 N 0.8452(3) 0.2311(3) 0.5386(3) 0.0418(10) Uani 1 1 d . . . N8 N 0.9855(3) 0.1805(3) 0.5704(3) 0.0409(9) Uani 1 1 d . . . N9 N 1.0999(3) 0.2334(3) 0.7038(2) 0.0364(9) Uani 1 1 d . . . N10 N 1.2112(3) 0.3256(3) 0.6676(2) 0.0373(9) Uani 1 1 d . . . N11 N 1.1384(3) 0.2148(3) 0.5667(2) 0.0389(9) Uani 1 1 d . . . N12 N 1.2479(3) 0.3078(3) 0.5301(2) 0.0366(9) Uani 1 1 d . . . N13 N 0.6936(2) 0.7119(3) 0.7954(2) 0.0355(9) Uani 1 1 d . . . N14 N 0.7986(3) 0.6303(3) 0.8845(3) 0.0377(9) Uani 1 1 d . . . N15 N 0.6294(3) 0.7910(3) 0.8906(3) 0.0414(10) Uani 1 1 d . . . N16 N 0.7271(3) 0.6997(3) 0.9853(3) 0.0431(10) Uani 1 1 d . . . N17 N 0.8204(3) 0.4824(3) 1.0122(2) 0.0389(9) Uani 1 1 d . . . N18 N 0.7601(3) 0.3492(3) 1.1019(2) 0.0367(9) Uani 1 1 d . . . N19 N 0.7586(3) 0.5527(3) 1.1141(3) 0.0433(10) Uani 1 1 d . . . N20 N 0.6989(3) 0.4176(3) 1.2044(2) 0.0401(10) Uani 1 1 d . . . N21 N 0.6483(3) 0.2355(3) 1.1583(2) 0.0388(9) Uani 1 1 d . . . N22 N 0.5164(3) 0.1922(3) 1.1600(2) 0.0378(9) Uani 1 1 d . . . N23 N 0.5828(3) 0.3092(3) 1.2565(2) 0.0382(9) Uani 1 1 d . . . N24 N 0.4502(3) 0.2654(3) 1.2592(2) 0.0367(9) Uani 1 1 d . . . O1 O 0.7321(2) 0.4698(2) 0.6769(2) 0.0408(8) Uani 1 1 d . . . O2 O 0.8642(2) 0.3137(2) 0.7496(2) 0.0377(7) Uani 1 1 d . . . O3 O 1.0899(2) 0.3440(3) 0.7612(2) 0.0464(8) Uani 1 1 d . . . O4 O 0.8129(2) 0.4360(3) 0.3288(2) 0.0476(9) Uani 1 1 d . . . O5 O 0.9584(3) 0.2563(3) 0.4241(2) 0.0579(10) Uani 1 1 d . . . O6 O 1.1818(2) 0.3031(3) 0.4190(2) 0.0449(8) Uani 1 1 d . . . O7 O 0.7546(2) 0.5675(2) 0.7994(2) 0.0410(8) Uani 1 1 d . . . O8 O 0.7778(2) 0.3902(2) 0.95310(19) 0.0378(7) Uani 1 1 d . . . O9 O 0.6168(2) 0.2158(3) 1.0380(2) 0.0510(9) Uani 1 1 d . . . O10 O 0.5928(3) 0.7589(3) 1.0371(2) 0.0648(11) Uani 1 1 d . . . O11 O 0.6296(2) 0.5581(3) 1.2060(2) 0.0507(9) Uani 1 1 d . . . O12 O 0.4548(2) 0.3986(2) 1.2827(2) 0.0408(8) 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 Cl5 0.0568(10) 0.0920(13) 0.1006(13) -0.0403(11) -0.0252(9) -0.0019(9) O1W 0.051(2) 0.048(2) 0.0411(18) -0.0237(17) 0.0092(16) -0.0114(17) O2W 0.0317(18) 0.067(2) 0.0361(17) -0.0253(17) -0.0040(14) 0.0025(16) O3W 0.0356(19) 0.058(2) 0.0443(19) -0.0192(17) -0.0017(15) -0.0024(16) O4W 0.0379(19) 0.051(2) 0.0410(19) -0.0141(16) 0.0062(15) -0.0082(16) Lu1 0.03118(13) 0.04141(14) 0.02908(12) -0.01913(9) -0.00257(8) -0.00014(8) Cl1 0.0504(10) 0.0834(13) 0.1428(18) -0.0368(13) -0.0166(11) -0.0117(9) Cl2 0.0576(11) 0.0598(12) 0.193(2) -0.0454(14) -0.0079(13) -0.0001(9) Cl3 0.0475(10) 0.0830(15) 0.172(2) 0.0315(14) 0.0070(12) 0.0054(10) Cl4 0.348(6) 0.214(4) 0.0614(15) -0.0085(19) -0.006(2) 0.138(4) Zn1 0.0583(5) 0.0585(5) 0.0744(5) -0.0001(4) -0.0001(4) 0.0091(4) C1 0.026(2) 0.049(3) 0.032(2) -0.018(2) -0.0032(18) 0.002(2) C2 0.023(2) 0.049(3) 0.030(2) -0.016(2) -0.0057(18) -0.001(2) C3 0.027(2) 0.055(3) 0.039(3) -0.027(2) -0.0078(19) -0.005(2) C4 0.039(3) 0.056(3) 0.042(3) -0.027(3) -0.017(2) -0.007(2) C5 0.031(2) 0.040(3) 0.030(2) -0.006(2) -0.0035(19) -0.008(2) C6 0.046(3) 0.059(3) 0.046(3) -0.033(3) -0.007(2) -0.010(2) C7 0.034(2) 0.032(2) 0.025(2) -0.0108(19) 0.0005(18) -0.0015(19) C8 0.047(3) 0.026(2) 0.036(2) -0.011(2) -0.003(2) -0.008(2) C9 0.042(3) 0.034(3) 0.037(2) -0.019(2) -0.007(2) -0.003(2) C10 0.043(3) 0.042(3) 0.043(3) -0.024(2) -0.002(2) -0.002(2) C11 0.030(2) 0.043(3) 0.029(2) -0.015(2) -0.0019(18) -0.003(2) C12 0.048(3) 0.044(3) 0.051(3) -0.032(3) -0.002(2) -0.002(2) C13 0.034(2) 0.044(3) 0.026(2) -0.014(2) -0.0037(18) 0.000(2) C14 0.040(3) 0.034(3) 0.036(2) -0.016(2) -0.005(2) 0.005(2) C15 0.033(2) 0.044(3) 0.035(2) -0.021(2) -0.0029(19) 0.004(2) C16 0.032(2) 0.042(3) 0.041(3) -0.026(2) 0.000(2) 0.002(2) C17 0.044(3) 0.051(3) 0.030(2) -0.019(2) -0.011(2) -0.005(2) C18 0.031(2) 0.051(3) 0.034(2) -0.023(2) 0.003(2) -0.006(2) C19 0.036(3) 0.038(3) 0.028(2) -0.014(2) 0.0000(19) -0.004(2) C20 0.037(3) 0.035(3) 0.041(3) -0.017(2) 0.003(2) -0.007(2) C21 0.028(2) 0.052(3) 0.047(3) -0.029(2) -0.001(2) -0.009(2) C22 0.048(3) 0.050(3) 0.046(3) -0.031(3) 0.003(2) -0.005(2) C23 0.026(2) 0.055(3) 0.036(2) -0.022(2) 0.0050(19) -0.008(2) C24 0.044(3) 0.052(3) 0.048(3) -0.029(3) -0.005(2) -0.009(2) C25 0.021(2) 0.040(3) 0.034(2) -0.015(2) -0.0030(18) 0.0012(19) C26 0.030(2) 0.057(3) 0.035(2) -0.025(2) -0.0061(19) -0.007(2) C27 0.029(2) 0.060(3) 0.032(2) -0.024(2) -0.0093(19) 0.003(2) C28 0.036(3) 0.068(4) 0.037(3) -0.033(3) -0.008(2) -0.009(2) C29 0.035(3) 0.041(3) 0.045(3) -0.018(2) -0.004(2) 0.004(2) C30 0.039(3) 0.070(4) 0.029(2) -0.027(2) -0.003(2) -0.008(2) C31 0.039(3) 0.028(2) 0.032(2) -0.0090(19) -0.001(2) -0.0012(19) C32 0.036(3) 0.038(3) 0.028(2) -0.0085(19) -0.0053(19) 0.000(2) C33 0.030(2) 0.033(3) 0.031(2) -0.0086(19) 0.0000(18) -0.0043(19) C34 0.038(3) 0.049(3) 0.023(2) -0.013(2) -0.0022(19) -0.004(2) C35 0.042(3) 0.031(3) 0.045(3) -0.017(2) 0.000(2) -0.002(2) C36 0.034(3) 0.047(3) 0.032(2) -0.017(2) 0.004(2) -0.007(2) N1 0.037(2) 0.037(2) 0.032(2) -0.0146(17) -0.0091(16) 0.0000(17) N2 0.036(2) 0.040(2) 0.0290(19) -0.0122(17) -0.0080(16) -0.0074(17) N3 0.035(2) 0.044(2) 0.031(2) -0.0174(18) -0.0029(16) -0.0045(18) N4 0.044(2) 0.049(3) 0.034(2) -0.021(2) -0.0015(18) -0.004(2) N5 0.031(2) 0.045(2) 0.043(2) -0.0263(19) -0.0038(17) -0.0033(17) N6 0.042(2) 0.035(2) 0.0311(19) -0.0170(17) -0.0047(17) 0.0013(17) N7 0.043(2) 0.046(3) 0.037(2) -0.0183(19) -0.0054(18) -0.0038(19) N8 0.040(2) 0.048(3) 0.038(2) -0.0228(19) -0.0016(18) -0.0005(19) N9 0.034(2) 0.041(2) 0.032(2) -0.0162(18) 0.0006(16) -0.0016(17) N10 0.035(2) 0.046(2) 0.035(2) -0.0218(19) 0.0009(17) -0.0063(18) N11 0.041(2) 0.045(2) 0.036(2) -0.0220(19) -0.0003(18) -0.0081(19) N12 0.036(2) 0.044(2) 0.0277(19) -0.0157(18) -0.0008(16) 0.0002(18) N13 0.033(2) 0.041(2) 0.037(2) -0.0195(18) -0.0041(16) -0.0047(17) N14 0.035(2) 0.040(2) 0.041(2) -0.0192(19) -0.0073(17) -0.0039(18) N15 0.040(2) 0.052(3) 0.037(2) -0.026(2) 0.0027(18) -0.0025(19) N16 0.040(2) 0.054(3) 0.035(2) -0.020(2) -0.0030(18) -0.004(2) N17 0.037(2) 0.051(3) 0.030(2) -0.0177(19) -0.0013(16) -0.0069(19) N18 0.032(2) 0.050(3) 0.031(2) -0.0196(18) -0.0050(16) -0.0009(18) N19 0.043(2) 0.054(3) 0.038(2) -0.025(2) -0.0020(18) -0.006(2) N20 0.033(2) 0.059(3) 0.036(2) -0.025(2) -0.0047(17) -0.0065(19) N21 0.035(2) 0.047(3) 0.034(2) -0.0178(18) 0.0021(17) -0.0058(18) N22 0.037(2) 0.043(2) 0.036(2) -0.0193(18) 0.0030(17) -0.0096(18) N23 0.033(2) 0.047(2) 0.034(2) -0.0166(18) -0.0052(16) -0.0044(18) N24 0.039(2) 0.035(2) 0.038(2) -0.0160(18) -0.0068(17) -0.0029(17) O1 0.0442(19) 0.053(2) 0.0307(16) -0.0226(15) -0.0117(14) 0.0041(16) O2 0.0355(18) 0.048(2) 0.0358(17) -0.0255(16) -0.0047(14) 0.0031(15) O3 0.0387(19) 0.060(2) 0.051(2) -0.0358(19) 0.0028(16) -0.0039(16) O4 0.045(2) 0.064(2) 0.0375(18) -0.0273(18) -0.0017(16) -0.0009(17) O5 0.065(3) 0.065(3) 0.041(2) -0.0230(19) 0.0005(18) -0.003(2) O6 0.051(2) 0.050(2) 0.0346(18) -0.0188(16) -0.0036(15) -0.0060(17) O7 0.045(2) 0.045(2) 0.0393(18) -0.0243(16) -0.0048(15) -0.0014(15) O8 0.0386(18) 0.051(2) 0.0296(16) -0.0227(15) -0.0035(13) -0.0051(15) O9 0.046(2) 0.069(3) 0.046(2) -0.0338(19) 0.0046(16) -0.0124(18) O10 0.065(3) 0.086(3) 0.042(2) -0.033(2) 0.0052(19) 0.006(2) O11 0.041(2) 0.069(3) 0.057(2) -0.042(2) 0.0004(17) -0.0048(18) O12 0.0420(19) 0.044(2) 0.0416(18) -0.0240(16) -0.0064(15) 0.0015(15) _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 O1W Lu1 2.315(3) . ? O2W Lu1 2.326(3) . ? O3W Lu1 2.337(3) . ? O4W Lu1 2.344(3) . ? Lu1 O2 2.283(3) . ? Lu1 O1 2.293(3) . ? Lu1 O8 2.295(3) . ? Lu1 O7 2.314(3) . ? Cl1 Zn1 2.264(2) . ? Cl2 Zn1 2.257(2) . ? Cl3 Zn1 2.264(2) . ? Cl4 Zn1 2.219(3) . ? C1 O1 1.231(5) . ? C1 N2 1.334(6) . ? C1 N1 1.372(6) . ? C2 N3 1.446(5) . ? C2 N1 1.451(6) . ? C2 C3 1.528(7) . ? C2 H2 0.9900 . ? C3 N4 1.451(6) . ? C3 N2 1.469(6) . ? C3 H3 0.9900 . ? C4 O4 1.236(6) . ? C4 N4 1.344(7) . ? C4 N3 1.357(6) . ? C5 N5 1.435(6) . ? C5 N2 1.438(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.446(7) . ? C6 N4 1.461(7) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.252(5) . ? C7 N6 1.346(6) . ? C7 N5 1.350(6) . ? C8 N7 1.435(6) . ? C8 N5 1.458(6) . ? C8 C9 1.552(7) . ? C8 H8 0.9900 . ? C9 N8 1.424(6) . ? C9 N6 1.452(6) . ? C9 H9 0.9900 . ? C10 O5 1.218(6) . ? C10 N8 1.367(6) . ? C10 N7 1.376(6) . ? C11 N9 1.432(6) . ? C11 N6 1.437(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.441(6) . ? C12 N11 1.455(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.216(5) . ? C13 N9 1.369(6) . ? C13 N10 1.374(6) . ? C14 N9 1.446(5) . ? C14 N11 1.452(6) . ? C14 C15 1.545(7) . ? C14 H14 0.9900 . ? C15 N12 1.445(6) . ? C15 N10 1.449(6) . ? C15 H15 0.9900 . ? C16 O6 1.225(6) . ? C16 N11 1.363(6) . ? C16 N12 1.367(6) . ? C17 N10 1.431(6) . ? C17 N3 1.443(6) 2_766 ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.438(6) . ? C18 N1 1.438(6) 2_766 ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O7 1.216(5) . ? C19 N13 1.357(6) . ? C19 N14 1.361(6) . ? C20 N15 1.452(6) . ? C20 N13 1.482(6) . ? C20 C21 1.526(7) . ? C20 H20 0.9900 . ? C21 N16 1.429(6) . ? C21 N14 1.452(6) . ? C21 H21 0.9900 . ? C22 O10 1.237(6) . ? C22 N16 1.338(7) . ? C22 N15 1.376(7) . ? C23 N14 1.406(6) . ? C23 N17 1.457(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N19 1.444(7) . ? C24 N16 1.452(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O8 1.237(5) . ? C25 N18 1.348(6) . ? C25 N17 1.353(6) . ? C26 N19 1.421(6) . ? C26 N17 1.457(6) . ? C26 C27 1.557(7) . ? C26 H26 0.9900 . ? C27 N20 1.445(6) . ? C27 N18 1.446(6) . ? C27 H27 0.9900 . ? C28 O11 1.211(6) . ? C28 N20 1.354(7) . ? C28 N19 1.396(6) . ? C29 N18 1.436(6) . ? C29 N21 1.445(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N20 1.430(6) . ? C30 N23 1.458(6) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O9 1.232(5) . ? C31 N22 1.335(6) . ? C31 N21 1.378(6) . ? C32 N21 1.429(5) . ? C32 N23 1.439(6) . ? C32 C33 1.562(6) . ? C32 H32 0.9900 . ? C33 N24 1.452(6) . ? C33 N22 1.454(6) . ? C33 H33 0.9900 . ? C34 O12 1.226(6) . ? C34 N24 1.363(6) . ? C34 N23 1.367(6) . ? C35 N15 1.428(6) . ? C35 N22 1.451(6) 2_667 ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N24 1.443(6) 2_667 ? C36 N13 1.445(6) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? N1 C18 1.438(6) 2_766 ? N3 C17 1.443(6) 2_766 ? N22 C35 1.451(6) 2_667 ? N24 C36 1.443(6) 2_667 ? 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 O2 Lu1 O1 77.11(11) . . ? O2 Lu1 O8 127.11(11) . . ? O1 Lu1 O8 150.48(11) . . ? O2 Lu1 O7 150.43(12) . . ? O1 Lu1 O7 86.59(11) . . ? O8 Lu1 O7 77.26(11) . . ? O2 Lu1 O1W 70.79(11) . . ? O1 Lu1 O1W 104.52(12) . . ? O8 Lu1 O1W 73.74(11) . . ? O7 Lu1 O1W 138.02(11) . . ? O2 Lu1 O2W 73.28(11) . . ? O1 Lu1 O2W 137.97(11) . . ? O8 Lu1 O2W 70.91(11) . . ? O7 Lu1 O2W 105.27(12) . . ? O1W Lu1 O2W 93.21(13) . . ? O2 Lu1 O3W 124.12(12) . . ? O1 Lu1 O3W 72.79(12) . . ? O8 Lu1 O3W 78.78(12) . . ? O7 Lu1 O3W 72.32(12) . . ? O1W Lu1 O3W 72.77(13) . . ? O2W Lu1 O3W 149.21(12) . . ? O2 Lu1 O4W 79.35(12) . . ? O1 Lu1 O4W 73.16(12) . . ? O8 Lu1 O4W 123.26(12) . . ? O7 Lu1 O4W 72.32(12) . . ? O1W Lu1 O4W 149.63(12) . . ? O2W Lu1 O4W 72.58(12) . . ? O3W Lu1 O4W 131.61(12) . . ? Cl4 Zn1 Cl2 111.9(2) . . ? Cl4 Zn1 Cl1 108.49(15) . . ? Cl2 Zn1 Cl1 107.20(8) . . ? Cl4 Zn1 Cl3 109.35(15) . . ? Cl2 Zn1 Cl3 111.42(8) . . ? Cl1 Zn1 Cl3 108.31(11) . . ? O1 C1 N2 126.6(4) . . ? O1 C1 N1 123.9(4) . . ? N2 C1 N1 109.5(4) . . ? N3 C2 N1 115.6(4) . . ? N3 C2 C3 102.7(4) . . ? N1 C2 C3 104.1(3) . . ? N3 C2 H2 111.3 . . ? N1 C2 H2 111.3 . . ? C3 C2 H2 111.3 . . ? N4 C3 N2 114.4(4) . . ? N4 C3 C2 103.9(4) . . ? N2 C3 C2 102.9(4) . . ? N4 C3 H3 111.7 . . ? N2 C3 H3 111.7 . . ? C2 C3 H3 111.7 . . ? O4 C4 N4 125.9(5) . . ? O4 C4 N3 125.0(5) . . ? N4 C4 N3 108.9(4) . . ? N5 C5 N2 113.4(4) . . ? N5 C5 H5A 108.9 . . ? N2 C5 H5A 108.9 . . ? N5 C5 H5B 108.9 . . ? N2 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N7 C6 N4 113.3(4) . . ? N7 C6 H6A 108.9 . . ? N4 C6 H6A 108.9 . . ? N7 C6 H6B 108.9 . . ? N4 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N6 124.1(4) . . ? O2 C7 N5 125.2(4) . . ? N6 C7 N5 110.7(4) . . ? N7 C8 N5 114.4(4) . . ? N7 C8 C9 103.9(4) . . ? N5 C8 C9 103.1(4) . . ? N7 C8 H8 111.6 . . ? N5 C8 H8 111.6 . . ? C9 C8 H8 111.6 . . ? N8 C9 N6 114.8(4) . . ? N8 C9 C8 102.8(4) . . ? N6 C9 C8 103.2(3) . . ? N8 C9 H9 111.8 . . ? N6 C9 H9 111.8 . . ? C8 C9 H9 111.8 . . ? O5 C10 N8 126.6(5) . . ? O5 C10 N7 125.8(5) . . ? N8 C10 N7 107.6(4) . . ? N9 C11 N6 114.5(4) . . ? N9 C11 H11A 108.6 . . ? N6 C11 H11A 108.6 . . ? N9 C11 H11B 108.6 . . ? N6 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? N8 C12 N11 114.9(4) . . ? N8 C12 H12A 108.5 . . ? N11 C12 H12A 108.5 . . ? N8 C12 H12B 108.5 . . ? N11 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? O3 C13 N9 126.6(4) . . ? O3 C13 N10 125.1(5) . . ? N9 C13 N10 108.3(4) . . ? N9 C14 N11 114.8(4) . . ? N9 C14 C15 102.9(4) . . ? N11 C14 C15 103.3(4) . . ? N9 C14 H14 111.7 . . ? N11 C14 H14 111.7 . . ? C15 C14 H14 111.7 . . ? N12 C15 N10 114.9(4) . . ? N12 C15 C14 103.2(4) . . ? N10 C15 C14 104.2(3) . . ? N12 C15 H15 111.3 . . ? N10 C15 H15 111.3 . . ? C14 C15 H15 111.3 . . ? O6 C16 N11 126.4(4) . . ? O6 C16 N12 125.6(5) . . ? N11 C16 N12 108.0(4) . . ? N10 C17 N3 114.9(4) . 2_766 ? N10 C17 H17A 108.5 . . ? N3 C17 H17A 108.5 2_766 . ? N10 C17 H17B 108.5 . . ? N3 C17 H17B 108.5 2_766 . ? H17A C17 H17B 107.5 . . ? N12 C18 N1 113.7(4) . 2_766 ? N12 C18 H18A 108.8 . . ? N1 C18 H18A 108.8 2_766 . ? N12 C18 H18B 108.8 . . ? N1 C18 H18B 108.8 2_766 . ? H18A C18 H18B 107.7 . . ? O7 C19 N13 125.2(4) . . ? O7 C19 N14 125.7(4) . . ? N13 C19 N14 109.0(4) . . ? N15 C20 N13 113.0(4) . . ? N15 C20 C21 103.0(4) . . ? N13 C20 C21 103.0(4) . . ? N15 C20 H20 112.3 . . ? N13 C20 H20 112.3 . . ? C21 C20 H20 112.3 . . ? N16 C21 N14 116.0(4) . . ? N16 C21 C20 104.6(4) . . ? N14 C21 C20 103.9(4) . . ? N16 C21 H21 110.6 . . ? N14 C21 H21 110.6 . . ? C20 C21 H21 110.6 . . ? O10 C22 N16 127.3(5) . . ? O10 C22 N15 123.3(5) . . ? N16 C22 N15 109.4(4) . . ? N14 C23 N17 114.0(4) . . ? N14 C23 H23A 108.8 . . ? N17 C23 H23A 108.8 . . ? N14 C23 H23B 108.8 . . ? N17 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? N19 C24 N16 113.9(4) . . ? N19 C24 H24A 108.8 . . ? N16 C24 H24A 108.8 . . ? N19 C24 H24B 108.8 . . ? N16 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? O8 C25 N18 125.4(4) . . ? O8 C25 N17 125.1(4) . . ? N18 C25 N17 109.5(4) . . ? N19 C26 N17 115.4(4) . . ? N19 C26 C27 104.2(4) . . ? N17 C26 C27 102.2(4) . . ? N19 C26 H26 111.5 . . ? N17 C26 H26 111.5 . . ? C27 C26 H26 111.5 . . ? N20 C27 N18 113.6(4) . . ? N20 C27 C26 102.7(4) . . ? N18 C27 C26 103.6(4) . . ? N20 C27 H27 112.1 . . ? N18 C27 H27 112.1 . . ? C26 C27 H27 112.1 . . ? O11 C28 N20 127.3(5) . . ? O11 C28 N19 124.8(5) . . ? N20 C28 N19 107.9(4) . . ? N18 C29 N21 114.5(4) . . ? N18 C29 H29A 108.6 . . ? N21 C29 H29A 108.6 . . ? N18 C29 H29B 108.6 . . ? N21 C29 H29B 108.6 . . ? H29A C29 H29B 107.6 . . ? N20 C30 N23 113.9(4) . . ? N20 C30 H30A 108.8 . . ? N23 C30 H30A 108.8 . . ? N20 C30 H30B 108.8 . . ? N23 C30 H30B 108.8 . . ? H30A C30 H30B 107.7 . . ? O9 C31 N22 125.9(4) . . ? O9 C31 N21 125.9(4) . . ? N22 C31 N21 108.2(4) . . ? N21 C32 N23 115.9(4) . . ? N21 C32 C33 103.4(4) . . ? N23 C32 C33 103.5(4) . . ? N21 C32 H32 111.2 . . ? N23 C32 H32 111.2 . . ? C33 C32 H32 111.2 . . ? N24 C33 N22 114.2(4) . . ? N24 C33 C32 102.3(4) . . ? N22 C33 C32 102.1(3) . . ? N24 C33 H33 112.4 . . ? N22 C33 H33 112.4 . . ? C32 C33 H33 112.4 . . ? O12 C34 N24 125.9(4) . . ? O12 C34 N23 126.2(5) . . ? N24 C34 N23 107.9(4) . . ? N15 C35 N22 115.3(4) . 2_667 ? N15 C35 H35A 108.5 . . ? N22 C35 H35A 108.5 2_667 . ? N15 C35 H35B 108.5 . . ? N22 C35 H35B 108.5 2_667 . ? H35A C35 H35B 107.5 . . ? N24 C36 N13 113.6(4) 2_667 . ? N24 C36 H36A 108.8 2_667 . ? N13 C36 H36A 108.8 . . ? N24 C36 H36B 108.8 2_667 . ? N13 C36 H36B 108.8 . . ? H36A C36 H36B 107.7 . . ? C1 N1 C18 122.2(4) . 2_766 ? C1 N1 C2 111.1(4) . . ? C18 N1 C2 124.1(4) 2_766 . ? C1 N2 C5 123.9(4) . . ? C1 N2 C3 112.2(4) . . ? C5 N2 C3 123.9(4) . . ? C4 N3 C17 123.1(4) . 2_766 ? C4 N3 C2 112.4(4) . . ? C17 N3 C2 124.3(4) 2_766 . ? C4 N4 C3 111.7(4) . . ? C4 N4 C6 122.7(4) . . ? C3 N4 C6 125.2(4) . . ? C7 N5 C5 123.9(4) . . ? C7 N5 C8 111.1(4) . . ? C5 N5 C8 124.9(4) . . ? C7 N6 C11 123.2(4) . . ? C7 N6 C9 111.5(4) . . ? C11 N6 C9 123.2(4) . . ? C10 N7 C8 111.9(4) . . ? C10 N7 C6 122.8(4) . . ? C8 N7 C6 124.8(4) . . ? C10 N8 C9 113.6(4) . . ? C10 N8 C12 122.0(4) . . ? C9 N8 C12 124.1(4) . . ? C13 N9 C11 123.0(4) . . ? C13 N9 C14 112.8(4) . . ? C11 N9 C14 123.0(4) . . ? C13 N10 C17 122.7(4) . . ? C13 N10 C15 111.6(4) . . ? C17 N10 C15 123.7(4) . . ? C16 N11 C14 112.6(4) . . ? C16 N11 C12 122.3(4) . . ? C14 N11 C12 123.6(4) . . ? C16 N12 C18 122.3(4) . . ? C16 N12 C15 112.8(4) . . ? C18 N12 C15 124.0(4) . . ? C19 N13 C36 122.5(4) . . ? C19 N13 C20 111.5(4) . . ? C36 N13 C20 124.3(4) . . ? C19 N14 C23 123.2(4) . . ? C19 N14 C21 112.2(4) . . ? C23 N14 C21 124.4(4) . . ? C22 N15 C35 122.9(4) . . ? C22 N15 C20 110.7(4) . . ? C35 N15 C20 125.9(4) . . ? C22 N16 C21 111.8(4) . . ? C22 N16 C24 122.5(4) . . ? C21 N16 C24 124.5(4) . . ? C25 N17 C23 122.9(4) . . ? C25 N17 C26 112.5(4) . . ? C23 N17 C26 124.5(4) . . ? C25 N18 C29 122.9(4) . . ? C25 N18 C27 112.2(4) . . ? C29 N18 C27 122.7(4) . . ? C28 N19 C26 112.0(4) . . ? C28 N19 C24 123.6(4) . . ? C26 N19 C24 124.4(4) . . ? C28 N20 C30 123.1(4) . . ? C28 N20 C27 113.1(4) . . ? C30 N20 C27 122.6(4) . . ? C31 N21 C32 112.7(4) . . ? C31 N21 C29 123.9(4) . . ? C32 N21 C29 122.7(4) . . ? C31 N22 C35 123.3(4) . 2_667 ? C31 N22 C33 113.6(4) . . ? C35 N22 C33 121.2(4) 2_667 . ? C34 N23 C32 113.0(4) . . ? C34 N23 C30 122.4(4) . . ? C32 N23 C30 122.8(4) . . ? C34 N24 C36 122.8(4) . 2_667 ? C34 N24 C33 113.2(4) . . ? C36 N24 C33 122.6(4) 2_667 . ? C1 O1 Lu1 154.5(3) . . ? C7 O2 Lu1 156.4(3) . . ? C19 O7 Lu1 155.2(3) . . ? C25 O8 Lu1 157.5(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.194 _refine_diff_density_min -1.202 _refine_diff_density_rms 0.115 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.003 0.000 -0.002 1092 515 ' ' 2 0.000 0.500 0.500 98 23 ' ' 3 0.500 0.500 0.000 94 22 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 902626'