# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_1_Zn4 _database_code_depnum_ccdc_archive 'CCDC 887296' #TrackingRef '14989_web_deposit_cif_file_0_MuktimoyChaudhury_1351337105.CIF_Zn4_Zn2Tb2_Cd2Tb2 (4).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H72 F12 N4 O12 Zn4' _chemical_formula_weight 1626.78 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' F F 0.0171 0.0103 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n n a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 16.7526(5) _cell_length_b 26.7988(8) _cell_length_c 16.5905(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7448.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9953 _cell_measurement_theta_min 2.301 _cell_measurement_theta_max 27.234 _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3328 _exptl_absorpt_coefficient_mu 1.362 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6031 _exptl_absorpt_correction_T_max 0.7464 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 Apex 2' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 115510 _diffrn_reflns_av_R_equivalents 0.0606 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 32.43 _reflns_number_total 13340 _reflns_number_gt 8693 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex 2' _computing_cell_refinement 'Bruker Apex 2' _computing_data_reduction 'Bruker Apex 2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _refine_special_details ; The 49 restaints arise from the fact that for the CF~3~ groups the atomic displacement parameters were constrained to be equivalent and the metrical parameters of these groups were idealized. 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^)+(0.0556P)^2^] 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 13340 _refine_ls_number_parameters 483 _refine_ls_number_restraints 49 _refine_ls_R_factor_all 0.0812 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1141 _refine_ls_wR_factor_gt 0.1053 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.149 _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 Zn1 Zn 0.510918(12) 0.219985(8) 0.380901(13) 0.01897(6) Uani 1 1 d . . . Zn2 Zn 0.509409(12) 0.326585(8) 0.297174(14) 0.01983(6) Uani 1 1 d . . . F1 F 0.6031(7) 0.4516(5) 0.5029(5) 0.0777(7) Uani 0.082(2) 1 d PD A 1 F2 F 0.6963(6) 0.4126(4) 0.4440(10) 0.0972(9) Uani 0.082(2) 1 d PD A 1 F3 F 0.6575(9) 0.4825(3) 0.3991(8) 0.0964(9) Uani 0.082(2) 1 d PD A 1 F1A F 0.66093(12) 0.41201(7) 0.49100(13) 0.0777(7) Uani 0.918(2) 1 d PD A 2 F2A F 0.69784(12) 0.44950(10) 0.38677(13) 0.0972(9) Uani 0.918(2) 1 d PD A 2 F3A F 0.61629(12) 0.48442(7) 0.46552(15) 0.0964(9) Uani 0.918(2) 1 d PD A 2 F4 F 0.37756(13) 0.50887(7) 0.32932(18) 0.0889(9) Uani 0.809(3) 1 d PD A 1 F5 F 0.34518(17) 0.46285(10) 0.23249(14) 0.1015(11) Uani 0.809(3) 1 d PD A 1 F6 F 0.30412(13) 0.44764(10) 0.3480(2) 0.1231(14) Uani 0.809(3) 1 d PD A 1 F4A F 0.3348(5) 0.4786(3) 0.3748(3) 0.0889(9) Uani 0.191(3) 1 d PD A 2 F5A F 0.3106(5) 0.4401(3) 0.2691(5) 0.1015(11) Uani 0.191(3) 1 d PD A 2 F6A F 0.3888(5) 0.5008(3) 0.2672(6) 0.1231(14) Uani 0.191(3) 1 d PD A 2 O1 O 0.56033(8) 0.16465(4) 0.31512(8) 0.0215(3) Uani 1 1 d . . . O2 O 0.46056(7) 0.28809(4) 0.39284(7) 0.0195(3) Uani 1 1 d . . . O3 O 0.58236(8) 0.37320(5) 0.36355(8) 0.0263(3) Uani 1 1 d . . . O4 O 0.42926(8) 0.38549(5) 0.29173(8) 0.0264(3) Uani 1 1 d . . . O1A O 0.59780(7) 0.26719(4) 0.31127(8) 0.0200(3) Uani 1 1 d . . . O1B O 0.42225(7) 0.21231(5) 0.27800(8) 0.0225(3) Uani 1 1 d . . . N1 N 0.44327(10) 0.16784(6) 0.45082(10) 0.0231(3) Uani 1 1 d . . . N2 N 0.57817(9) 0.22951(6) 0.48923(10) 0.0230(3) Uani 1 1 d . . . C1 C 0.56712(11) 0.11677(7) 0.34063(12) 0.0229(4) Uani 1 1 d . . . C2 C 0.63757(12) 0.09035(8) 0.32352(13) 0.0289(4) Uani 1 1 d . . . C3 C 0.64067(14) 0.03963(8) 0.34122(14) 0.0351(5) Uani 1 1 d . . . H3A H 0.6876 0.0215 0.3279 0.042 Uiso 1 1 calc R . . C4 C 0.57772(15) 0.01457(8) 0.37761(13) 0.0350(5) Uani 1 1 d . . . C5 C 0.51108(13) 0.04228(8) 0.39933(13) 0.0311(5) Uani 1 1 d . . . H5A H 0.4684 0.0262 0.4266 0.037 Uiso 1 1 calc R . . C6 C 0.50508(12) 0.09316(7) 0.38211(12) 0.0254(4) Uani 1 1 d . . . C7 C 0.70791(12) 0.11659(8) 0.28680(15) 0.0374(5) Uani 1 1 d . . . H7A H 0.7509 0.0925 0.2775 0.056 Uiso 1 1 calc R . . H7B H 0.7266 0.1427 0.3235 0.056 Uiso 1 1 calc R . . H7C H 0.6920 0.1317 0.2354 0.056 Uiso 1 1 calc R . . C8 C 0.58189(19) -0.04102(8) 0.39249(15) 0.0513(7) Uani 1 1 d . . . H8A H 0.6277 -0.0485 0.4272 0.077 Uiso 1 1 calc R . . H8B H 0.5880 -0.0585 0.3410 0.077 Uiso 1 1 calc R . . H8C H 0.5327 -0.0521 0.4189 0.077 Uiso 1 1 calc R . . C9 C 0.42994(11) 0.12088(7) 0.40408(12) 0.0250(4) Uani 1 1 d . . . H9A H 0.4009 0.1292 0.3539 0.030 Uiso 1 1 calc R . . H9B H 0.3954 0.0984 0.4362 0.030 Uiso 1 1 calc R . . C10 C 0.36425(12) 0.18969(8) 0.47068(13) 0.0295(4) Uani 1 1 d . . . H10A H 0.3335 0.1659 0.5030 0.044 Uiso 1 1 calc R . . H10B H 0.3353 0.1970 0.4208 0.044 Uiso 1 1 calc R . . H10C H 0.3718 0.2206 0.5014 0.044 Uiso 1 1 calc R . . C11 C 0.48986(12) 0.15883(8) 0.52534(12) 0.0269(4) Uani 1 1 d . . . H11A H 0.5313 0.1333 0.5148 0.032 Uiso 1 1 calc R . . H11B H 0.4541 0.1460 0.5681 0.032 Uiso 1 1 calc R . . C12 C 0.52944(12) 0.20706(7) 0.55386(12) 0.0271(4) Uani 1 1 d . . . H12A H 0.4878 0.2311 0.5709 0.032 Uiso 1 1 calc R . . H12B H 0.5638 0.1999 0.6010 0.032 Uiso 1 1 calc R . . C13 C 0.65560(12) 0.20361(8) 0.48277(14) 0.0321(5) Uani 1 1 d . . . H13A H 0.6845 0.2066 0.5339 0.048 Uiso 1 1 calc R . . H13B H 0.6872 0.2187 0.4395 0.048 Uiso 1 1 calc R . . H13C H 0.6465 0.1683 0.4707 0.048 Uiso 1 1 calc R . . C14 C 0.59327(11) 0.28386(7) 0.50456(12) 0.0246(4) Uani 1 1 d . . . H14A H 0.6222 0.2979 0.4577 0.030 Uiso 1 1 calc R . . H14B H 0.6285 0.2870 0.5522 0.030 Uiso 1 1 calc R . . C15 C 0.51917(11) 0.31440(7) 0.51881(12) 0.0227(4) Uani 1 1 d . . . C16 C 0.51386(12) 0.34441(8) 0.58697(13) 0.0280(4) Uani 1 1 d . . . H16A H 0.5574 0.3451 0.6237 0.034 Uiso 1 1 calc R . . C17 C 0.44748(14) 0.37319(8) 0.60298(13) 0.0317(5) Uani 1 1 d . . . C18 C 0.38353(13) 0.37014(7) 0.55020(13) 0.0306(5) Uani 1 1 d . . . H18A H 0.3371 0.3894 0.5609 0.037 Uiso 1 1 calc R . . C19 C 0.38502(11) 0.33984(7) 0.48190(12) 0.0248(4) Uani 1 1 d . . . C20 C 0.45559(11) 0.31343(7) 0.46366(11) 0.0209(4) Uani 1 1 d . . . C21 C 0.44254(17) 0.40572(10) 0.67807(16) 0.0498(7) Uani 1 1 d . . . H21A H 0.4084 0.4346 0.6672 0.075 Uiso 1 1 calc R . . H21B H 0.4962 0.4172 0.6928 0.075 Uiso 1 1 calc R . . H21C H 0.4199 0.3863 0.7226 0.075 Uiso 1 1 calc R . . C22 C 0.31313(12) 0.33441(8) 0.42877(13) 0.0311(5) Uani 1 1 d . . . H22A H 0.2688 0.3538 0.4512 0.047 Uiso 1 1 calc R . . H22B H 0.2978 0.2992 0.4258 0.047 Uiso 1 1 calc R . . H22C H 0.3257 0.3467 0.3746 0.047 Uiso 1 1 calc R . . C23 C 0.56746(12) 0.41696(7) 0.38514(13) 0.0296(5) Uani 1 1 d . A . C24 C 0.63480(14) 0.44127(8) 0.43317(15) 0.0460(6) Uani 1 1 d D . . C25 C 0.50031(13) 0.44551(8) 0.36898(15) 0.0364(5) Uani 1 1 d . . . H25A H 0.4976 0.4785 0.3897 0.044 Uiso 1 1 calc R A . C26 C 0.43710(12) 0.42757(7) 0.32361(13) 0.0300(5) Uani 1 1 d . A . C27 C 0.36598(13) 0.46259(8) 0.30857(15) 0.0461(6) Uani 1 1 d D . . C1A C 0.63346(14) 0.2500 0.2500 0.0188(5) Uani 1 2 d SD . . C2A C 0.72266(14) 0.2500 0.2500 0.0218(5) Uani 1 2 d SD . . C3A C 0.76432(11) 0.27234(7) 0.31259(13) 0.0275(4) Uani 1 1 d D . . H3AA H 0.7360 0.2879 0.3554 0.033 Uiso 1 1 calc R . . C4A C 0.84721(12) 0.27201(9) 0.31298(15) 0.0377(5) Uani 1 1 d D . . H4AA H 0.8757 0.2868 0.3563 0.045 Uiso 1 1 calc R . . C5A C 0.88793(17) 0.2500 0.2500 0.0441(9) Uani 1 2 d SD . . H5AA H 0.9446 0.2500 0.2500 0.053 Uiso 1 2 calc SR . . C1B C 0.38680(14) 0.2500 0.2500 0.0199(5) Uani 1 2 d SD . . C2B C 0.29768(15) 0.2500 0.2500 0.0335(7) Uani 1 2 d SD . . C3B C 0.25669(14) 0.20532(12) 0.26117(14) 0.0521(7) Uani 1 1 d DU . . H3BA H 0.2849 0.1750 0.2698 0.063 Uiso 1 1 calc R . . C4B C 0.17316(18) 0.20584(15) 0.25947(19) 0.0737(9) Uani 1 1 d DU . . H4BA H 0.1434 0.1759 0.2649 0.088 Uiso 1 1 calc R . . C5B C 0.1364(3) 0.2500 0.2500 0.0763(13) Uani 1 2 d SDU . . H5BA H 0.0797 0.2500 0.2500 0.092 Uiso 1 2 calc SR . . 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 0.01981(10) 0.01679(10) 0.02031(11) 0.00144(8) 0.00009(8) 0.00173(7) Zn2 0.02056(10) 0.01720(11) 0.02175(12) 0.00139(8) -0.00036(8) 0.00099(8) F1 0.0812(13) 0.0610(12) 0.0910(15) 0.0121(11) -0.0604(12) -0.0158(10) F2 0.0682(13) 0.125(2) 0.0986(18) -0.0270(14) 0.0005(12) -0.0635(14) F3 0.0909(15) 0.0549(12) 0.143(2) -0.0640(13) -0.0679(14) 0.0279(10) F1A 0.0812(13) 0.0610(12) 0.0910(15) 0.0121(11) -0.0604(12) -0.0158(10) F2A 0.0682(13) 0.125(2) 0.0986(18) -0.0270(14) 0.0005(12) -0.0635(14) F3A 0.0909(15) 0.0549(12) 0.143(2) -0.0640(13) -0.0679(14) 0.0279(10) F4 0.0729(15) 0.0285(10) 0.165(3) -0.0257(13) -0.0443(16) 0.0276(10) F5 0.124(2) 0.101(2) 0.0795(18) -0.0171(14) -0.0545(16) 0.0786(17) F6 0.0519(13) 0.0748(17) 0.243(4) 0.064(2) 0.0601(18) 0.0399(12) F4A 0.0729(15) 0.0285(10) 0.165(3) -0.0257(13) -0.0443(16) 0.0276(10) F5A 0.124(2) 0.101(2) 0.0795(18) -0.0171(14) -0.0545(16) 0.0786(17) F6A 0.0519(13) 0.0748(17) 0.243(4) 0.064(2) 0.0601(18) 0.0399(12) O1 0.0251(6) 0.0160(6) 0.0236(7) 0.0024(5) -0.0001(5) 0.0030(5) O2 0.0202(6) 0.0191(6) 0.0193(7) -0.0005(5) 0.0013(5) 0.0027(5) O3 0.0263(7) 0.0197(7) 0.0328(8) 0.0002(6) -0.0037(6) 0.0001(5) O4 0.0267(7) 0.0225(7) 0.0300(8) -0.0008(6) -0.0021(6) 0.0039(5) O1A 0.0182(6) 0.0188(6) 0.0230(7) -0.0010(5) 0.0016(5) 0.0018(5) O1B 0.0234(6) 0.0203(6) 0.0238(7) 0.0020(5) 0.0036(5) 0.0006(5) N1 0.0274(8) 0.0197(8) 0.0222(9) 0.0018(6) 0.0017(6) 0.0006(6) N2 0.0216(7) 0.0239(8) 0.0235(9) 0.0012(7) -0.0014(6) 0.0050(6) C1 0.0284(9) 0.0171(8) 0.0232(10) 0.0018(7) -0.0023(7) 0.0012(7) C2 0.0303(10) 0.0262(10) 0.0302(11) 0.0015(9) -0.0025(8) 0.0087(8) C3 0.0459(12) 0.0258(10) 0.0336(12) 0.0007(9) 0.0014(10) 0.0146(9) C4 0.0590(14) 0.0201(10) 0.0260(11) 0.0022(8) 0.0026(10) 0.0084(9) C5 0.0486(12) 0.0190(9) 0.0256(11) 0.0007(8) 0.0030(9) -0.0003(9) C6 0.0340(10) 0.0197(9) 0.0224(10) 0.0011(8) 0.0002(8) 0.0020(7) C7 0.0276(10) 0.0351(12) 0.0494(15) -0.0013(10) 0.0028(9) 0.0086(9) C8 0.093(2) 0.0212(11) 0.0393(15) 0.0048(10) 0.0174(14) 0.0154(12) C9 0.0283(9) 0.0202(9) 0.0266(10) 0.0023(8) 0.0038(8) -0.0036(7) C10 0.0284(10) 0.0284(10) 0.0316(11) 0.0030(9) 0.0082(8) 0.0003(8) C11 0.0352(10) 0.0233(9) 0.0222(10) 0.0055(8) 0.0026(8) 0.0030(8) C12 0.0326(10) 0.0259(10) 0.0227(10) 0.0018(8) -0.0008(8) 0.0035(8) C13 0.0266(10) 0.0347(11) 0.0350(12) 0.0022(9) -0.0034(9) 0.0102(8) C14 0.0210(8) 0.0257(9) 0.0270(10) 0.0001(8) -0.0040(7) -0.0013(7) C15 0.0240(9) 0.0199(9) 0.0242(10) 0.0001(7) 0.0010(7) -0.0022(7) C16 0.0328(10) 0.0273(10) 0.0238(10) -0.0018(8) -0.0042(8) -0.0057(8) C17 0.0453(12) 0.0243(10) 0.0254(11) -0.0059(8) 0.0053(9) -0.0016(9) C18 0.0345(10) 0.0253(10) 0.0319(12) -0.0030(8) 0.0084(9) 0.0056(8) C19 0.0235(9) 0.0265(9) 0.0244(10) 0.0025(8) 0.0034(8) 0.0021(7) C20 0.0234(8) 0.0191(8) 0.0201(9) 0.0017(7) 0.0025(7) -0.0009(7) C21 0.0633(17) 0.0441(14) 0.0419(15) -0.0214(12) 0.0036(12) 0.0028(12) C22 0.0244(9) 0.0372(12) 0.0317(12) -0.0009(9) 0.0024(8) 0.0077(8) C23 0.0330(10) 0.0233(10) 0.0326(12) -0.0004(8) -0.0061(9) -0.0004(8) C24 0.0462(14) 0.0288(12) 0.0629(17) -0.0086(12) -0.0167(13) 0.0014(10) C25 0.0373(12) 0.0230(10) 0.0488(15) -0.0092(10) -0.0103(10) 0.0065(8) C26 0.0317(10) 0.0224(10) 0.0360(12) 0.0000(9) -0.0006(9) 0.0048(8) C27 0.0421(13) 0.0331(13) 0.0630(18) -0.0083(12) -0.0105(12) 0.0129(10) C1A 0.0174(10) 0.0132(11) 0.0260(14) 0.0041(10) 0.000 0.000 C2A 0.0179(11) 0.0182(12) 0.0292(15) -0.0021(10) 0.000 0.000 C3A 0.0199(9) 0.0279(10) 0.0346(11) -0.0048(9) 0.0000(8) -0.0003(7) C4A 0.0211(9) 0.0462(13) 0.0458(14) -0.0094(11) -0.0054(9) -0.0045(9) C5A 0.0153(12) 0.050(2) 0.067(2) -0.0119(18) 0.000 0.000 C1B 0.0155(10) 0.0270(13) 0.0172(13) -0.0041(10) 0.000 0.000 C2B 0.0176(12) 0.064(2) 0.0185(14) -0.0061(14) 0.000 0.000 C3B 0.0327(11) 0.100(2) 0.0239(12) -0.0047(13) 0.0047(9) -0.0331(13) C4B 0.0599(14) 0.1147(18) 0.0466(14) 0.0027(13) 0.0067(12) -0.0393(13) C5B 0.0584(18) 0.106(2) 0.0643(19) 0.0020(17) 0.000 0.000 _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 O1 2.0187(13) . ? Zn1 O2 2.0203(12) . ? Zn1 N2 2.1365(16) . ? Zn1 N1 2.1407(16) . ? Zn1 O1A 2.2480(12) . ? Zn1 O1B 2.2723(13) . ? Zn2 O2 2.0623(12) . ? Zn2 O1 2.0624(13) 4 ? Zn2 O3 2.0656(13) . ? Zn2 O4 2.0743(13) . ? Zn2 O1B 2.1848(13) 4 ? Zn2 O1A 2.1865(12) . ? F1 C24 1.303(5) . ? F2 C24 1.298(5) . ? F3 C24 1.297(5) . ? F1A C24 1.314(3) . ? F2A C24 1.325(3) . ? F3A C24 1.312(2) . ? F4 C27 1.302(3) . ? F5 C27 1.310(3) . ? F6 C27 1.289(3) . ? F4A C27 1.289(5) . ? F5A C27 1.286(5) . ? F6A C27 1.292(5) . ? O1 C1 1.356(2) . ? O1 Zn2 2.0624(13) 4 ? O2 C20 1.360(2) . ? O3 C23 1.251(2) . ? O4 C26 1.252(2) . ? O1A C1A 1.2660(16) . ? O1B C1B 1.2605(16) . ? O1B Zn2 2.1848(13) 4 ? N1 C11 1.482(3) . ? N1 C10 1.485(2) . ? N1 C9 1.495(2) . ? N2 C13 1.475(2) . ? N2 C12 1.476(3) . ? N2 C14 1.500(2) . ? C1 C6 1.398(3) . ? C1 C2 1.405(3) . ? C2 C3 1.392(3) . ? C2 C7 1.501(3) . ? C3 C4 1.389(3) . ? C3 H3A 0.9500 . ? C4 C5 1.388(3) . ? C4 C8 1.512(3) . ? C5 C6 1.397(3) . ? C5 H5A 0.9500 . ? C6 C9 1.506(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.528(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.505(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.390(3) . ? C15 C20 1.404(3) . ? C16 C17 1.379(3) . ? C16 H16A 0.9500 . ? C17 C18 1.386(3) . ? C17 C21 1.523(3) . ? C18 C19 1.394(3) . ? C18 H18A 0.9500 . ? C19 C20 1.411(3) . ? C19 C22 1.500(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C25 1.387(3) . ? C23 C24 1.527(3) . ? C25 C26 1.385(3) . ? C25 H25A 0.9500 . ? C26 C27 1.537(3) . ? C1A O1A 1.2660(16) 4 ? C1A C2A 1.494(3) . ? C2A C3A 1.387(2) . ? C2A C3A 1.387(2) 4 ? C3A C4A 1.389(3) . ? C3A H3AA 0.9500 . ? C4A C5A 1.380(3) . ? C4A H4AA 0.9500 . ? C5A C4A 1.380(3) 4 ? C5A H5AA 0.9500 . ? C1B O1B 1.2605(16) 4 ? C1B C2B 1.493(3) . ? C2B C3B 1.393(3) . ? C2B C3B 1.393(3) 4 ? C3B C4B 1.400(4) . ? C3B H3BA 0.9500 . ? C4B C5B 1.344(4) . ? C4B H4BA 0.9500 . ? C5B C4B 1.343(4) 4 ? C5B H5BA 0.9500 . ? 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 Zn1 O2 152.60(5) . . ? O1 Zn1 N2 109.05(6) . . ? O2 Zn1 N2 91.70(5) . . ? O1 Zn1 N1 91.75(6) . . ? O2 Zn1 N1 108.39(6) . . ? N2 Zn1 N1 84.34(6) . . ? O1 Zn1 O1A 82.54(5) . . ? O2 Zn1 O1A 79.18(5) . . ? N2 Zn1 O1A 91.35(5) . . ? N1 Zn1 O1A 171.33(5) . . ? O1 Zn1 O1B 78.19(5) . . ? O2 Zn1 O1B 83.25(5) . . ? N2 Zn1 O1B 170.95(5) . . ? N1 Zn1 O1B 90.11(5) . . ? O1A Zn1 O1B 95.06(5) . . ? O2 Zn2 O1 156.38(5) . 4 ? O2 Zn2 O3 97.30(5) . . ? O1 Zn2 O3 99.67(5) 4 . ? O2 Zn2 O4 99.05(5) . . ? O1 Zn2 O4 98.15(5) 4 . ? O3 Zn2 O4 86.90(5) . . ? O2 Zn2 O1B 86.30(5) . 4 ? O1 Zn2 O1B 79.34(5) 4 4 ? O3 Zn2 O1B 171.19(5) . 4 ? O4 Zn2 O1B 84.58(5) . 4 ? O2 Zn2 O1A 79.76(5) . . ? O1 Zn2 O1A 84.23(5) 4 . ? O3 Zn2 O1A 89.00(5) . . ? O4 Zn2 O1A 175.56(5) . . ? O1B Zn2 O1A 99.58(5) 4 . ? C1 O1 Zn1 124.11(11) . . ? C1 O1 Zn2 115.11(11) . 4 ? Zn1 O1 Zn2 103.60(5) . 4 ? C20 O2 Zn1 124.17(11) . . ? C20 O2 Zn2 116.07(11) . . ? Zn1 O2 Zn2 102.17(5) . . ? C23 O3 Zn2 126.97(13) . . ? C26 O4 Zn2 126.79(13) . . ? C1A O1A Zn2 119.91(10) . . ? C1A O1A Zn1 120.89(9) . . ? Zn2 O1A Zn1 91.50(4) . . ? C1B O1B Zn2 119.13(10) . 4 ? C1B O1B Zn1 120.82(10) . . ? Zn2 O1B Zn1 92.02(5) 4 . ? C11 N1 C10 110.41(15) . . ? C11 N1 C9 111.98(15) . . ? C10 N1 C9 108.30(15) . . ? C11 N1 Zn1 106.24(11) . . ? C10 N1 Zn1 109.56(11) . . ? C9 N1 Zn1 110.34(11) . . ? C13 N2 C12 110.32(15) . . ? C13 N2 C14 108.72(15) . . ? C12 N2 C14 111.46(15) . . ? C13 N2 Zn1 110.27(12) . . ? C12 N2 Zn1 105.71(12) . . ? C14 N2 Zn1 110.34(11) . . ? O1 C1 C6 121.30(16) . . ? O1 C1 C2 118.96(17) . . ? C6 C1 C2 119.73(17) . . ? C3 C2 C1 118.74(19) . . ? C3 C2 C7 120.92(18) . . ? C1 C2 C7 120.35(18) . . ? C4 C3 C2 122.4(2) . . ? C4 C3 H3A 118.8 . . ? C2 C3 H3A 118.8 . . ? C5 C4 C3 117.69(19) . . ? C5 C4 C8 121.5(2) . . ? C3 C4 C8 120.8(2) . . ? C4 C5 C6 121.8(2) . . ? C4 C5 H5A 119.1 . . ? C6 C5 H5A 119.1 . . ? C5 C6 C1 119.27(18) . . ? C5 C6 C9 119.48(18) . . ? C1 C6 C9 121.15(17) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 C6 114.57(16) . . ? N1 C9 H9A 108.6 . . ? C6 C9 H9A 108.6 . . ? N1 C9 H9B 108.6 . . ? C6 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 110.43(16) . . ? N1 C11 H11A 109.6 . . ? C12 C11 H11A 109.6 . . ? N1 C11 H11B 109.6 . . ? C12 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? N2 C12 C11 111.10(16) . . ? N2 C12 H12A 109.4 . . ? C11 C12 H12A 109.4 . . ? N2 C12 H12B 109.4 . . ? C11 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? N2 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C14 C15 114.55(15) . . ? N2 C14 H14A 108.6 . . ? C15 C14 H14A 108.6 . . ? N2 C14 H14B 108.6 . . ? C15 C14 H14B 108.6 . . ? H14A C14 H14B 107.6 . . ? C16 C15 C20 119.46(18) . . ? C16 C15 C14 119.67(17) . . ? C20 C15 C14 120.87(17) . . ? C17 C16 C15 122.12(19) . . ? C17 C16 H16A 118.9 . . ? C15 C16 H16A 118.9 . . ? C16 C17 C18 117.95(19) . . ? C16 C17 C21 121.4(2) . . ? C18 C17 C21 120.6(2) . . ? C17 C18 C19 122.27(19) . . ? C17 C18 H18A 118.9 . . ? C19 C18 H18A 118.9 . . ? C18 C19 C20 118.78(18) . . ? C18 C19 C22 121.33(18) . . ? C20 C19 C22 119.89(18) . . ? O2 C20 C15 121.72(16) . . ? O2 C20 C19 119.16(17) . . ? C15 C20 C19 119.12(18) . . ? C17 C21 H21A 109.5 . . ? C17 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C17 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O3 C23 C25 128.58(19) . . ? O3 C23 C24 113.70(17) . . ? C25 C23 C24 117.69(18) . . ? F3 C24 F2 109.3(5) . . ? F3 C24 F1 109.1(5) . . ? F2 C24 F1 109.0(5) . . ? F3 C24 F3A 59.8(6) . . ? F2 C24 F3A 130.7(7) . . ? F1 C24 F3A 49.7(6) . . ? F3 C24 F1A 136.8(7) . . ? F2 C24 F1A 44.1(7) . . ? F1 C24 F1A 67.3(6) . . ? F3A C24 F1A 107.8(2) . . ? F3 C24 F2A 51.1(6) . . ? F2 C24 F2A 63.0(6) . . ? F1 C24 F2A 143.7(6) . . ? F3A C24 F2A 106.2(2) . . ? F1A C24 F2A 104.9(2) . . ? F3 C24 C23 110.6(8) . . ? F2 C24 C23 114.0(7) . . ? F1 C24 C23 104.6(6) . . ? F3A C24 C23 114.52(19) . . ? F1A C24 C23 111.86(19) . . ? F2A C24 C23 110.9(2) . . ? C26 C25 C23 122.2(2) . . ? C26 C25 H25A 118.9 . . ? C23 C25 H25A 118.9 . . ? O4 C26 C25 128.47(19) . . ? O4 C26 C27 113.58(18) . . ? C25 C26 C27 117.95(18) . . ? F5A C27 F4A 107.4(4) . . ? F5A C27 F6 62.2(4) . . ? F4A C27 F6 49.1(4) . . ? F5A C27 F6A 108.4(4) . . ? F4A C27 F6A 108.0(4) . . ? F6 C27 F6A 139.0(4) . . ? F5A C27 F4 133.6(5) . . ? F4A C27 F4 61.2(4) . . ? F6 C27 F4 106.4(2) . . ? F6A C27 F4 48.7(5) . . ? F5A C27 F5 47.1(4) . . ? F4A C27 F5 135.4(4) . . ? F6 C27 F5 106.1(3) . . ? F6A C27 F5 64.0(5) . . ? F4 C27 F5 106.8(2) . . ? F5A C27 C26 110.8(4) . . ? F4A C27 C26 112.2(4) . . ? F6 C27 C26 110.5(2) . . ? F6A C27 C26 110.0(4) . . ? F4 C27 C26 115.0(2) . . ? F5 C27 C26 111.5(2) . . ? O1A C1A O1A 123.7(2) . 4 ? O1A C1A C2A 118.16(11) . . ? O1A C1A C2A 118.16(11) 4 . ? C3A C2A C3A 119.6(2) . 4 ? C3A C2A C1A 120.21(12) . . ? C3A C2A C1A 120.21(12) 4 . ? C2A C3A C4A 120.3(2) . . ? C2A C3A H3AA 119.9 . . ? C4A C3A H3AA 119.9 . . ? C5A C4A C3A 119.6(2) . . ? C5A C4A H4AA 120.2 . . ? C3A C4A H4AA 120.2 . . ? C4A C5A C4A 120.8(3) . 4 ? C4A C5A H5AA 119.6 . . ? C4A C5A H5AA 119.6 4 . ? O1B C1B O1B 123.8(2) . 4 ? O1B C1B C2B 118.11(11) . . ? O1B C1B C2B 118.11(11) 4 . ? C3B C2B C3B 120.9(3) . 4 ? C3B C2B C1B 119.54(16) . . ? C3B C2B C1B 119.54(16) 4 . ? C2B C3B C4B 118.8(3) . . ? C2B C3B H3BA 120.6 . . ? C4B C3B H3BA 120.6 . . ? C5B C4B C3B 118.0(4) . . ? C5B C4B H4BA 121.0 . . ? C3B C4B H4BA 121.0 . . ? C4B C5B C4B 125.4(5) 4 . ? C4B C5B H5BA 117.3 4 . ? C4B C5B H5BA 117.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Zn1 O1 C1 -161.52(13) . . . . ? N2 Zn1 O1 C1 61.23(14) . . . . ? N1 Zn1 O1 C1 -23.39(14) . . . . ? O1A Zn1 O1 C1 150.08(14) . . . . ? O1B Zn1 O1 C1 -113.14(14) . . . . ? O2 Zn1 O1 Zn2 -27.79(14) . . . 4 ? N2 Zn1 O1 Zn2 -165.04(6) . . . 4 ? N1 Zn1 O1 Zn2 110.34(6) . . . 4 ? O1A Zn1 O1 Zn2 -76.20(5) . . . 4 ? O1B Zn1 O1 Zn2 20.59(5) . . . 4 ? O1 Zn1 O2 C20 -161.28(13) . . . . ? N2 Zn1 O2 C20 -21.22(14) . . . . ? N1 Zn1 O2 C20 63.38(14) . . . . ? O1A Zn1 O2 C20 -112.27(13) . . . . ? O1B Zn1 O2 C20 151.25(13) . . . . ? O1 Zn1 O2 Zn2 -27.68(14) . . . . ? N2 Zn1 O2 Zn2 112.38(6) . . . . ? N1 Zn1 O2 Zn2 -163.02(6) . . . . ? O1A Zn1 O2 Zn2 21.34(5) . . . . ? O1B Zn1 O2 Zn2 -75.15(5) . . . . ? O1 Zn2 O2 C20 164.30(13) 4 . . . ? O3 Zn2 O2 C20 28.59(12) . . . . ? O4 Zn2 O2 C20 -59.42(12) . . . . ? O1B Zn2 O2 C20 -143.33(12) 4 . . . ? O1A Zn2 O2 C20 116.24(12) . . . . ? O1 Zn2 O2 Zn1 26.13(15) 4 . . . ? O3 Zn2 O2 Zn1 -109.57(6) . . . . ? O4 Zn2 O2 Zn1 162.42(5) . . . . ? O1B Zn2 O2 Zn1 78.51(6) 4 . . . ? O1A Zn2 O2 Zn1 -21.92(5) . . . . ? O2 Zn2 O3 C23 -96.74(17) . . . . ? O1 Zn2 O3 C23 99.75(17) 4 . . . ? O4 Zn2 O3 C23 2.01(17) . . . . ? O1B Zn2 O3 C23 16.9(4) 4 . . . ? O1A Zn2 O3 C23 -176.28(17) . . . . ? O2 Zn2 O4 C26 95.28(17) . . . . ? O1 Zn2 O4 C26 -100.96(17) 4 . . . ? O3 Zn2 O4 C26 -1.62(17) . . . . ? O1B Zn2 O4 C26 -179.35(17) 4 . . . ? O1A Zn2 O4 C26 21.1(7) . . . . ? O2 Zn2 O1A C1A 146.56(13) . . . . ? O1 Zn2 O1A C1A -16.01(12) 4 . . . ? O3 Zn2 O1A C1A -115.84(12) . . . . ? O4 Zn2 O1A C1A -138.6(6) . . . . ? O1B Zn2 O1A C1A 62.12(13) 4 . . . ? O2 Zn2 O1A Zn1 19.16(5) . . . . ? O1 Zn2 O1A Zn1 -143.42(5) 4 . . . ? O3 Zn2 O1A Zn1 116.75(5) . . . . ? O4 Zn2 O1A Zn1 94.0(7) . . . . ? O1B Zn2 O1A Zn1 -65.28(5) 4 . . . ? O1 Zn1 O1A C1A 13.23(13) . . . . ? O2 Zn1 O1A C1A -146.26(13) . . . . ? N2 Zn1 O1A C1A 122.27(13) . . . . ? N1 Zn1 O1A C1A 62.3(4) . . . . ? O1B Zn1 O1A C1A -64.13(13) . . . . ? O1 Zn1 O1A Zn2 139.88(5) . . . . ? O2 Zn1 O1A Zn2 -19.61(5) . . . . ? N2 Zn1 O1A Zn2 -111.08(5) . . . . ? N1 Zn1 O1A Zn2 -171.1(3) . . . . ? O1B Zn1 O1A Zn2 62.52(5) . . . . ? O1 Zn1 O1B C1B -144.87(13) . . . . ? O2 Zn1 O1B C1B 14.86(13) . . . . ? N2 Zn1 O1B C1B 71.3(4) . . . . ? N1 Zn1 O1B C1B 123.37(13) . . . . ? O1A Zn1 O1B C1B -63.60(13) . . . . ? O1 Zn1 O1B Zn2 -18.84(5) . . . 4 ? O2 Zn1 O1B Zn2 140.89(5) . . . 4 ? N2 Zn1 O1B Zn2 -162.7(3) . . . 4 ? N1 Zn1 O1B Zn2 -110.60(5) . . . 4 ? O1A Zn1 O1B Zn2 62.44(5) . . . 4 ? O1 Zn1 N1 C11 96.39(12) . . . . ? O2 Zn1 N1 C11 -102.49(12) . . . . ? N2 Zn1 N1 C11 -12.58(12) . . . . ? O1A Zn1 N1 C11 47.9(4) . . . . ? O1B Zn1 N1 C11 174.58(12) . . . . ? O1 Zn1 N1 C10 -144.33(13) . . . . ? O2 Zn1 N1 C10 16.78(14) . . . . ? N2 Zn1 N1 C10 106.70(13) . . . . ? O1A Zn1 N1 C10 167.1(3) . . . . ? O1B Zn1 N1 C10 -66.15(13) . . . . ? O1 Zn1 N1 C9 -25.19(12) . . . . ? O2 Zn1 N1 C9 135.93(11) . . . . ? N2 Zn1 N1 C9 -134.16(12) . . . . ? O1A Zn1 N1 C9 -73.7(4) . . . . ? O1B Zn1 N1 C9 53.00(12) . . . . ? O1 Zn1 N2 C13 14.49(14) . . . . ? O2 Zn1 N2 C13 -147.30(13) . . . . ? N1 Zn1 N2 C13 104.38(13) . . . . ? O1A Zn1 N2 C13 -68.08(13) . . . . ? O1B Zn1 N2 C13 156.8(3) . . . . ? O1 Zn1 N2 C12 -104.75(11) . . . . ? O2 Zn1 N2 C12 93.46(11) . . . . ? N1 Zn1 N2 C12 -14.86(11) . . . . ? O1A Zn1 N2 C12 172.68(11) . . . . ? O1B Zn1 N2 C12 37.6(4) . . . . ? O1 Zn1 N2 C14 134.61(11) . . . . ? O2 Zn1 N2 C14 -27.18(12) . . . . ? N1 Zn1 N2 C14 -135.50(12) . . . . ? O1A Zn1 N2 C14 52.04(12) . . . . ? O1B Zn1 N2 C14 -83.1(4) . . . . ? Zn1 O1 C1 C6 41.5(2) . . . . ? Zn2 O1 C1 C6 -87.65(19) 4 . . . ? Zn1 O1 C1 C2 -139.65(15) . . . . ? Zn2 O1 C1 C2 91.22(18) 4 . . . ? O1 C1 C2 C3 -172.45(18) . . . . ? C6 C1 C2 C3 6.4(3) . . . . ? O1 C1 C2 C7 7.5(3) . . . . ? C6 C1 C2 C7 -173.61(19) . . . . ? C1 C2 C3 C4 -2.2(3) . . . . ? C7 C2 C3 C4 177.8(2) . . . . ? C2 C3 C4 C5 -2.5(3) . . . . ? C2 C3 C4 C8 177.2(2) . . . . ? C3 C4 C5 C6 3.0(3) . . . . ? C8 C4 C5 C6 -176.7(2) . . . . ? C4 C5 C6 C1 1.2(3) . . . . ? C4 C5 C6 C9 177.51(19) . . . . ? O1 C1 C6 C5 172.92(18) . . . . ? C2 C1 C6 C5 -5.9(3) . . . . ? O1 C1 C6 C9 -3.4(3) . . . . ? C2 C1 C6 C9 177.77(19) . . . . ? C11 N1 C9 C6 -55.8(2) . . . . ? C10 N1 C9 C6 -177.76(16) . . . . ? Zn1 N1 C9 C6 62.32(18) . . . . ? C5 C6 C9 N1 129.2(2) . . . . ? C1 C6 C9 N1 -54.5(2) . . . . ? C10 N1 C11 C12 -81.01(19) . . . . ? C9 N1 C11 C12 158.23(16) . . . . ? Zn1 N1 C11 C12 37.70(17) . . . . ? C13 N2 C12 C11 -79.2(2) . . . . ? C14 N2 C12 C11 159.91(15) . . . . ? Zn1 N2 C12 C11 40.00(17) . . . . ? N1 C11 C12 N2 -54.6(2) . . . . ? C13 N2 C14 C15 -175.58(17) . . . . ? C12 N2 C14 C15 -53.8(2) . . . . ? Zn1 N2 C14 C15 63.38(18) . . . . ? N2 C14 C15 C16 127.68(19) . . . . ? N2 C14 C15 C20 -53.0(2) . . . . ? C20 C15 C16 C17 0.6(3) . . . . ? C14 C15 C16 C17 179.92(19) . . . . ? C15 C16 C17 C18 2.4(3) . . . . ? C15 C16 C17 C21 179.8(2) . . . . ? C16 C17 C18 C19 -1.0(3) . . . . ? C21 C17 C18 C19 -178.4(2) . . . . ? C17 C18 C19 C20 -3.4(3) . . . . ? C17 C18 C19 C22 175.7(2) . . . . ? Zn1 O2 C20 C15 41.0(2) . . . . ? Zn2 O2 C20 C15 -87.02(18) . . . . ? Zn1 O2 C20 C19 -139.63(14) . . . . ? Zn2 O2 C20 C19 92.37(17) . . . . ? C16 C15 C20 O2 174.32(17) . . . . ? C14 C15 C20 O2 -5.0(3) . . . . ? C16 C15 C20 C19 -5.1(3) . . . . ? C14 C15 C20 C19 175.66(17) . . . . ? C18 C19 C20 O2 -173.02(17) . . . . ? C22 C19 C20 O2 7.8(3) . . . . ? C18 C19 C20 C15 6.4(3) . . . . ? C22 C19 C20 C15 -172.76(18) . . . . ? Zn2 O3 C23 C25 -1.6(3) . . . . ? Zn2 O3 C23 C24 -179.49(14) . . . . ? O3 C23 C24 F3 123.5(7) . . . . ? C25 C23 C24 F3 -54.6(7) . . . . ? O3 C23 C24 F2 -0.2(7) . . . . ? C25 C23 C24 F2 -178.3(7) . . . . ? O3 C23 C24 F1 -119.2(7) . . . . ? C25 C23 C24 F1 62.7(7) . . . . ? O3 C23 C24 F3A -171.3(2) . . . . ? C25 C23 C24 F3A 10.6(3) . . . . ? O3 C23 C24 F1A -48.2(3) . . . . ? C25 C23 C24 F1A 133.7(2) . . . . ? O3 C23 C24 F2A 68.6(3) . . . . ? C25 C23 C24 F2A -109.5(3) . . . . ? O3 C23 C25 C26 0.0(4) . . . . ? C24 C23 C25 C26 177.8(2) . . . . ? Zn2 O4 C26 C25 0.8(3) . . . . ? Zn2 O4 C26 C27 -179.39(14) . . . . ? C23 C25 C26 O4 0.4(4) . . . . ? C23 C25 C26 C27 -179.3(2) . . . . ? O4 C26 C27 F5A 3.3(6) . . . . ? C25 C26 C27 F5A -176.9(5) . . . . ? O4 C26 C27 F4A 123.2(5) . . . . ? C25 C26 C27 F4A -56.9(5) . . . . ? O4 C26 C27 F6 70.2(3) . . . . ? C25 C26 C27 F6 -109.9(3) . . . . ? O4 C26 C27 F6A -116.5(6) . . . . ? C25 C26 C27 F6A 63.3(6) . . . . ? O4 C26 C27 F4 -169.3(2) . . . . ? C25 C26 C27 F4 10.5(3) . . . . ? O4 C26 C27 F5 -47.5(3) . . . . ? C25 C26 C27 F5 132.3(3) . . . . ? Zn2 O1A C1A O1A -54.68(7) . . . 4 ? Zn1 O1A C1A O1A 57.61(8) . . . 4 ? Zn2 O1A C1A C2A 125.33(7) . . . . ? Zn1 O1A C1A C2A -122.38(8) . . . . ? O1A C1A C2A C3A -5.58(11) . . . . ? O1A C1A C2A C3A 174.43(11) 4 . . . ? O1A C1A C2A C3A 174.42(11) . . . 4 ? O1A C1A C2A C3A -5.57(11) 4 . . 4 ? C3A C2A C3A C4A -0.52(15) 4 . . . ? C1A C2A C3A C4A 179.48(15) . . . . ? C2A C3A C4A C5A 1.0(3) . . . . ? C3A C4A C5A C4A -0.52(15) . . . 4 ? Zn2 O1B C1B O1B -55.27(7) 4 . . 4 ? Zn1 O1B C1B O1B 57.03(8) . . . 4 ? Zn2 O1B C1B C2B 124.73(7) 4 . . . ? Zn1 O1B C1B C2B -122.98(8) . . . . ? O1B C1B C2B C3B -15.90(13) . . . . ? O1B C1B C2B C3B 164.10(13) 4 . . . ? O1B C1B C2B C3B 164.10(13) . . . 4 ? O1B C1B C2B C3B -15.90(13) 4 . . 4 ? C3B C2B C3B C4B 1.20(19) 4 . . . ? C1B C2B C3B C4B -178.80(19) . . . . ? C2B C3B C4B C5B -2.4(4) . . . . ? C3B C4B C5B C4B 1.21(19) . . . 4 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C7 H7C O3 0.98 2.47 3.274(3) 139.4 4 C9 H9A O4 0.99 2.49 3.253(2) 133.2 4 C18 H18A F2 0.95 2.44 3.338(7) 157.5 6_556 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.447 _refine_diff_density_min -0.806 _refine_diff_density_rms 0.080 # 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 0.250 0.500 -0.080 180 63 ' ' 2 0.750 0.500 0.080 180 63 ' ' 3 0.679 0.114 0.167 7 0 ' ' 4 0.821 0.886 0.167 7 0 ' ' 5 0.750 0.000 0.420 180 63 ' ' 6 0.679 0.386 0.333 7 0 ' ' 7 0.821 0.614 0.333 7 0 ' ' 8 0.250 0.000 0.580 180 63 ' ' 9 0.179 0.386 0.667 7 0 ' ' 10 0.321 0.614 0.667 7 0 ' ' 11 0.179 0.114 0.833 7 0 ' ' 12 0.321 0.886 0.833 7 0 ' ' _platon_squeeze_details ; ; data_3_Zn2Tb2 _database_code_depnum_ccdc_archive 'CCDC 887297' #TrackingRef '14989_web_deposit_cif_file_0_MuktimoyChaudhury_1351337105.CIF_Zn4_Zn2Tb2_Cd2Tb2 (4).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 H74 F24 N4 O16 Tb2 Zn2' _chemical_formula_sum 'C78 H74 F24 N4 O16 Tb2 Zn2' _chemical_formula_weight 2227.99 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' F F 0.0171 0.0103 '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 'C c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 12.4834(5) _cell_length_b 31.2286(14) _cell_length_c 23.0942(10) _cell_angle_alpha 90.00 _cell_angle_beta 100.656(2) _cell_angle_gamma 90.00 _cell_volume 8847.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9387 _cell_measurement_theta_min 2.565 _cell_measurement_theta_max 25.993 _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4416 _exptl_absorpt_coefficient_mu 2.229 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.604 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 Apex 2' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64568 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 30.15 _reflns_number_total 20587 _reflns_number_gt 16375 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex 2' _computing_cell_refinement 'Bruker Apex 2' _computing_data_reduction 'Bruker Apex 2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _refine_special_details ; The 233 restaints arise from the fact that for the CF~3~ groups the atomic displacement parameters were constrained to be equivalent and the metrical parameters of these groups were idealized. ; _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^)+(0.0728P)^2^] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.407(7) _refine_ls_number_reflns 20587 _refine_ls_number_parameters 1181 _refine_ls_number_restraints 233 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1177 _refine_ls_wR_factor_gt 0.1095 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.507767(16) 0.766720(8) 0.518653(11) 0.03428(6) Uani 1 1 d . . . Tb2 Tb 0.440224(18) 0.938338(8) 0.469440(12) 0.03907(6) Uani 1 1 d . . . Zn1 Zn 0.32001(4) 0.835214(18) 0.41913(2) 0.02579(11) Uani 1 1 d . . . Zn2 Zn 0.63102(4) 0.87048(2) 0.57045(2) 0.03068(13) Uani 1 1 d . . . F1 F 0.5499(7) 0.6921(3) 0.3256(3) 0.132(2) Uani 1 1 d U . . F2 F 0.6931(7) 0.6846(3) 0.3816(4) 0.149(3) Uani 1 1 d U . . F3 F 0.5945(7) 0.6328(2) 0.3599(3) 0.144(3) Uani 1 1 d U . . F4 F 0.3633(9) 0.6267(4) 0.5727(2) 0.135(3) Uani 0.448(6) 1 d PDU A 1 F5 F 0.2670(5) 0.6279(3) 0.4872(4) 0.096(2) Uani 0.448(6) 1 d PDU A 1 F6 F 0.4025(8) 0.5864(2) 0.5059(5) 0.105(3) Uani 0.448(6) 1 d PDU A 1 F4A F 0.3272(7) 0.5998(3) 0.4724(3) 0.135(3) Uani 0.552(6) 1 d PDU A 2 F5A F 0.2888(5) 0.6355(3) 0.5438(3) 0.096(2) Uani 0.552(6) 1 d PDU A 2 F6A F 0.4379(5) 0.6020(3) 0.5536(3) 0.105(3) Uani 0.552(6) 1 d PDU A 2 F7 F 0.3337(2) 0.70146(15) 0.66574(16) 0.0840(15) Uani 1 1 d DU B 2 F8 F 0.4490(3) 0.73290(11) 0.73085(15) 0.0706(12) Uani 1 1 d DU B 2 F9 F 0.4594(3) 0.66594(10) 0.71829(14) 0.0608(10) Uani 1 1 d DU B 2 F10 F 0.8083(5) 0.66173(18) 0.5604(3) 0.1000(17) Uani 1 1 d U B 2 F11 F 0.7120(5) 0.61453(17) 0.5911(3) 0.1024(18) Uani 1 1 d U B 2 F12 F 0.8179(5) 0.6550(2) 0.6502(2) 0.1025(18) Uani 1 1 d U B 2 F13 F 0.1057(15) 0.9816(3) 0.5439(3) 0.114(3) Uani 0.239(7) 1 d PDU C 1 F14 F 0.0761(14) 1.04194(19) 0.5021(5) 0.117(3) Uani 0.239(7) 1 d PDU C 1 F15 F 0.0470(11) 0.9848(4) 0.4519(4) 0.096(2) Uani 0.239(7) 1 d PDU C 1 F13A F 0.1450(5) 1.0096(2) 0.5521(2) 0.114(3) Uani 0.761(7) 1 d PD C 2 F14A F 0.0486(6) 1.03622(16) 0.4756(3) 0.117(3) Uani 0.761(7) 1 d PD C 2 F15A F 0.0461(5) 0.96945(15) 0.4905(3) 0.096(2) Uani 0.761(7) 1 d PD C 2 F16 F 0.3609(4) 1.03794(19) 0.2980(3) 0.157(3) Uani 1 1 d DU . . F17 F 0.1921(4) 1.0444(2) 0.2932(3) 0.161(3) Uani 1 1 d DU . . F18 F 0.3000(5) 1.08585(13) 0.3481(2) 0.1051(19) Uani 1 1 d DU . . F19 F 0.4466(7) 1.1172(2) 0.4971(4) 0.0765(18) Uani 0.365(8) 1 d PDU D 1 F20 F 0.5793(5) 1.0941(4) 0.5599(5) 0.109(3) Uani 0.365(8) 1 d PDU D 1 F21 F 0.4184(6) 1.0773(5) 0.5671(4) 0.105(3) Uani 0.365(8) 1 d PDU D 1 F19A F 0.4448(5) 1.0783(2) 0.5777(2) 0.0765(18) Uani 0.635(8) 1 d PDU D 2 F20A F 0.5618(5) 1.1129(2) 0.5410(4) 0.109(3) Uani 0.635(8) 1 d PDU D 2 F21A F 0.4046(5) 1.1039(3) 0.4914(3) 0.105(3) Uani 0.635(8) 1 d PDU D 2 F22 F 0.6669(6) 0.9996(2) 0.3396(3) 0.117(2) Uani 1 1 d U . . F23 F 0.7917(6) 0.9998(3) 0.4140(4) 0.139(3) Uani 1 1 d U . . F24 F 0.7211(5) 1.05730(19) 0.3800(3) 0.1082(19) Uani 1 1 d U . . O1 O 0.3272(3) 0.78053(11) 0.46845(14) 0.0277(7) Uani 1 1 d . . . O2 O 0.3592(3) 0.89346(11) 0.38983(14) 0.0300(7) Uani 1 1 d . . . O3 O 0.6674(3) 0.80908(12) 0.55285(14) 0.0322(8) Uani 1 1 d . . . O4 O 0.5485(3) 0.92658(12) 0.56581(15) 0.0362(8) Uani 1 1 d . . . O5 O 0.4624(3) 0.83382(11) 0.56691(15) 0.0315(7) Uani 1 1 d . . . O6 O 0.3461(3) 0.87435(11) 0.50510(14) 0.0291(7) Uani 1 1 d . . . O7 O 0.5059(3) 0.81885(11) 0.43678(13) 0.0285(7) Uani 1 1 d . . . O8 O 0.5784(3) 0.88098(12) 0.46985(14) 0.0323(8) Uani 1 1 d . . . O9 O 0.5481(4) 0.72413(14) 0.43705(16) 0.0455(10) Uani 1 1 d . . . O10 O 0.4191(3) 0.69640(13) 0.51600(18) 0.0430(9) Uani 1 1 d . . . O11 O 0.4882(3) 0.74594(13) 0.61751(16) 0.0392(9) Uani 1 1 d . . . O12 O 0.6479(3) 0.71385(13) 0.55851(15) 0.0376(8) Uani 1 1 d . . . O13 O 0.2655(3) 0.96524(12) 0.48384(19) 0.0438(9) Uani 1 1 d . . . O14 O 0.3678(4) 0.98971(13) 0.39062(19) 0.0466(10) Uani 1 1 d . . . O15 O 0.4652(4) 1.01092(14) 0.51036(19) 0.0503(10) Uani 1 1 d . . . O16 O 0.5891(3) 0.97222(13) 0.43429(19) 0.0474(10) Uani 1 1 d . . . N1 N 0.2915(3) 0.80122(14) 0.33692(18) 0.0310(9) Uani 1 1 d . . . N2 N 0.1484(3) 0.84731(13) 0.40153(17) 0.0296(8) Uani 1 1 d . . . N3 N 0.6766(3) 0.86405(16) 0.66470(18) 0.0371(10) Uani 1 1 d . . . N4 N 0.7883(3) 0.90054(16) 0.57613(19) 0.0376(10) Uani 1 1 d . . . C1 C 0.2491(4) 0.75051(16) 0.4479(2) 0.0292(10) Uani 1 1 d . . . C2 C 0.1834(4) 0.73335(17) 0.4847(2) 0.0366(12) Uani 1 1 d . . . C3 C 0.1011(4) 0.70528(18) 0.4617(3) 0.0419(13) Uani 1 1 d . . . H3A H 0.0549 0.6944 0.4866 0.050 Uiso 1 1 calc R . . C4 C 0.0833(5) 0.69214(19) 0.4017(3) 0.0477(14) Uani 1 1 d . . . C5 C 0.1526(5) 0.70838(18) 0.3670(3) 0.0437(13) Uani 1 1 d . . . H5A H 0.1434 0.7000 0.3268 0.052 Uiso 1 1 calc R . . C6 C 0.2359(4) 0.73696(17) 0.3898(2) 0.0327(11) Uani 1 1 d . . . C7 C 0.2020(4) 0.7458(2) 0.5488(2) 0.0410(13) Uani 1 1 d . . . H7A H 0.1831 0.7216 0.5721 0.061 Uiso 1 1 calc R . . H7B H 0.1561 0.7704 0.5539 0.061 Uiso 1 1 calc R . . H7C H 0.2788 0.7533 0.5620 0.061 Uiso 1 1 calc R . . C8 C -0.0071(7) 0.6608(2) 0.3765(4) 0.076(2) Uani 1 1 d . . . H8A H 0.0101 0.6473 0.3409 0.114 Uiso 1 1 calc R . . H8B H -0.0765 0.6762 0.3664 0.114 Uiso 1 1 calc R . . H8C H -0.0130 0.6386 0.4058 0.114 Uiso 1 1 calc R . . C9 C 0.3069(4) 0.75472(16) 0.3501(2) 0.0325(10) Uani 1 1 d . . . H9A H 0.3840 0.7497 0.3684 0.039 Uiso 1 1 calc R . . H9B H 0.2925 0.7387 0.3125 0.039 Uiso 1 1 calc R . . C10 C 0.3651(4) 0.81224(19) 0.2961(2) 0.0371(12) Uani 1 1 d . . . H10A H 0.3434 0.7964 0.2592 0.056 Uiso 1 1 calc R . . H10B H 0.4401 0.8046 0.3140 0.056 Uiso 1 1 calc R . . H10C H 0.3608 0.8431 0.2880 0.056 Uiso 1 1 calc R . . C11 C 0.1777(4) 0.81087(18) 0.3080(2) 0.0338(11) Uani 1 1 d . . . H11A H 0.1491 0.7866 0.2821 0.041 Uiso 1 1 calc R . . H11B H 0.1777 0.8366 0.2829 0.041 Uiso 1 1 calc R . . C12 C 0.1018(4) 0.81876(18) 0.3521(2) 0.0332(11) Uani 1 1 d . . . H12A H 0.0330 0.8315 0.3308 0.040 Uiso 1 1 calc R . . H12B H 0.0837 0.7909 0.3683 0.040 Uiso 1 1 calc R . . C13 C 0.0917(4) 0.83788(18) 0.4521(2) 0.0354(11) Uani 1 1 d . . . H13A H 0.0127 0.8400 0.4388 0.053 Uiso 1 1 calc R . . H13B H 0.1151 0.8586 0.4838 0.053 Uiso 1 1 calc R . . H13C H 0.1104 0.8089 0.4668 0.053 Uiso 1 1 calc R . . C14 C 0.1301(4) 0.89364(16) 0.3863(2) 0.0344(11) Uani 1 1 d . . . H14A H 0.0507 0.8991 0.3769 0.041 Uiso 1 1 calc R . . H14B H 0.1606 0.9110 0.4213 0.041 Uiso 1 1 calc R . . C15 C 0.1793(4) 0.90814(18) 0.3361(2) 0.0371(12) Uani 1 1 d . . . C16 C 0.1115(5) 0.9227(2) 0.2840(3) 0.0479(14) Uani 1 1 d . . . H16A H 0.0347 0.9230 0.2817 0.057 Uiso 1 1 calc R . . C17 C 0.1550(7) 0.9366(2) 0.2365(3) 0.0561(18) Uani 1 1 d . . . C18 C 0.2675(6) 0.9356(2) 0.2410(3) 0.0523(16) Uani 1 1 d . . . H18A H 0.2980 0.9444 0.2082 0.063 Uiso 1 1 calc R . . C19 C 0.3366(5) 0.92234(19) 0.2915(3) 0.0436(13) Uani 1 1 d . . . C20 C 0.2928(4) 0.90831(17) 0.3395(2) 0.0345(11) Uani 1 1 d . . . C21 C 0.0807(8) 0.9525(3) 0.1807(4) 0.091(3) Uani 1 1 d . . . H21A H 0.0588 0.9283 0.1541 0.136 Uiso 1 1 calc R . . H21B H 0.1199 0.9736 0.1610 0.136 Uiso 1 1 calc R . . H21C H 0.0158 0.9659 0.1910 0.136 Uiso 1 1 calc R . . C22 C 0.4592(5) 0.9226(2) 0.2953(3) 0.0556(17) Uani 1 1 d . . . H22A H 0.4759 0.9236 0.2554 0.083 Uiso 1 1 calc R . . H22B H 0.4906 0.8966 0.3153 0.083 Uiso 1 1 calc R . . H22C H 0.4904 0.9478 0.3175 0.083 Uiso 1 1 calc R . . C23 C 0.7616(4) 0.79332(18) 0.5864(2) 0.0340(11) Uani 1 1 d . . . C24 C 0.8382(4) 0.77217(19) 0.5589(2) 0.0359(12) Uani 1 1 d . . . C25 C 0.9318(4) 0.7560(2) 0.5945(3) 0.0436(14) Uani 1 1 d . . . H25A H 0.9841 0.7422 0.5759 0.052 Uiso 1 1 calc R . . C26 C 0.9530(4) 0.7589(2) 0.6551(3) 0.0460(14) Uani 1 1 d . . . C27 C 0.8767(5) 0.7804(2) 0.6809(2) 0.0448(14) Uani 1 1 d . . . H27A H 0.8902 0.7841 0.7224 0.054 Uiso 1 1 calc R . . C28 C 0.7796(4) 0.7971(2) 0.6474(2) 0.0360(12) Uani 1 1 d . . . C29 C 0.8200(5) 0.7669(2) 0.4932(2) 0.0432(14) Uani 1 1 d . . . H29A H 0.8859 0.7550 0.4819 0.065 Uiso 1 1 calc R . . H29B H 0.8039 0.7948 0.4742 0.065 Uiso 1 1 calc R . . H29C H 0.7586 0.7474 0.4805 0.065 Uiso 1 1 calc R . . C30 C 1.0545(5) 0.7403(3) 0.6917(3) 0.0615(19) Uani 1 1 d . . . H30A H 1.1164 0.7451 0.6718 0.092 Uiso 1 1 calc R . . H30B H 1.0445 0.7095 0.6967 0.092 Uiso 1 1 calc R . . H30C H 1.0688 0.7542 0.7304 0.092 Uiso 1 1 calc R . . C31 C 0.6976(4) 0.8177(2) 0.6776(2) 0.0412(13) Uani 1 1 d . . . H31A H 0.7219 0.8143 0.7206 0.049 Uiso 1 1 calc R . . H31B H 0.6278 0.8020 0.6665 0.049 Uiso 1 1 calc R . . C32 C 0.5911(5) 0.8773(2) 0.6979(3) 0.0501(16) Uani 1 1 d . . . H32A H 0.6180 0.8734 0.7402 0.075 Uiso 1 1 calc R . . H32B H 0.5257 0.8598 0.6856 0.075 Uiso 1 1 calc R . . H32C H 0.5731 0.9076 0.6899 0.075 Uiso 1 1 calc R . . C33 C 0.7753(5) 0.8915(2) 0.6826(2) 0.0435(14) Uani 1 1 d . . . H33A H 0.8176 0.8804 0.7202 0.052 Uiso 1 1 calc R . . H33B H 0.7514 0.9209 0.6900 0.052 Uiso 1 1 calc R . . C34 C 0.8497(4) 0.8936(2) 0.6375(2) 0.0409(13) Uani 1 1 d . . . H34A H 0.9026 0.9172 0.6481 0.049 Uiso 1 1 calc R . . H34B H 0.8914 0.8665 0.6388 0.049 Uiso 1 1 calc R . . C35 C 0.8556(4) 0.8834(2) 0.5345(2) 0.0440(14) Uani 1 1 d . . . H35A H 0.9260 0.8982 0.5408 0.066 Uiso 1 1 calc R . . H35B H 0.8176 0.8880 0.4939 0.066 Uiso 1 1 calc R . . H35C H 0.8675 0.8526 0.5415 0.066 Uiso 1 1 calc R . . C36 C 0.7676(5) 0.94623(19) 0.5606(3) 0.0433(13) Uani 1 1 d . . . H36A H 0.7272 0.9480 0.5195 0.052 Uiso 1 1 calc R . . H36B H 0.8384 0.9609 0.5622 0.052 Uiso 1 1 calc R . . C37 C 0.7044(5) 0.9695(2) 0.5997(3) 0.0438(14) Uani 1 1 d . . . C38 C 0.7533(6) 1.0042(3) 0.6332(4) 0.069(2) Uani 1 1 d . . . H38A H 0.8266 1.0116 0.6317 0.083 Uiso 1 1 calc R . . C39 C 0.6971(7) 1.0275(3) 0.6681(4) 0.084(3) Uani 1 1 d . . . C40 C 0.5873(7) 1.0153(3) 0.6698(4) 0.074(2) Uani 1 1 d . . . H40A H 0.5480 1.0310 0.6943 0.089 Uiso 1 1 calc R . . C41 C 0.5362(5) 0.9816(2) 0.6372(3) 0.0544(16) Uani 1 1 d . . . C42 C 0.5960(4) 0.95847(19) 0.6001(2) 0.0395(12) Uani 1 1 d . . . C43 C 0.7464(9) 1.0660(4) 0.7020(6) 0.122(5) Uani 1 1 d . . . H43A H 0.8157 1.0580 0.7270 0.184 Uiso 1 1 calc R . . H43B H 0.6963 1.0767 0.7268 0.184 Uiso 1 1 calc R . . H43C H 0.7592 1.0884 0.6744 0.184 Uiso 1 1 calc R . . C44 C 0.4221(6) 0.9708(3) 0.6391(3) 0.0617(18) Uani 1 1 d . . . H44A H 0.4006 0.9846 0.6733 0.093 Uiso 1 1 calc R . . H44B H 0.4147 0.9397 0.6422 0.093 Uiso 1 1 calc R . . H44C H 0.3749 0.9810 0.6030 0.093 Uiso 1 1 calc R . . C45 C 0.3751(4) 0.85581(17) 0.5542(2) 0.0296(10) Uani 1 1 d . . . C46 C 0.3037(4) 0.85883(18) 0.5994(2) 0.0331(11) Uani 1 1 d . . . C47 C 0.3189(5) 0.8310(2) 0.6480(2) 0.0445(14) Uani 1 1 d . . . H47A H 0.3728 0.8092 0.6517 0.053 Uiso 1 1 calc R . . C48 C 0.2551(6) 0.8355(3) 0.6906(3) 0.0552(17) Uani 1 1 d . . . H48A H 0.2654 0.8169 0.7237 0.066 Uiso 1 1 calc R . . C49 C 0.1750(6) 0.8676(3) 0.6848(3) 0.068(2) Uani 1 1 d . . . H49A H 0.1299 0.8702 0.7136 0.082 Uiso 1 1 calc R . . C50 C 0.1617(5) 0.8952(2) 0.6379(3) 0.0522(16) Uani 1 1 d . . . H50A H 0.1095 0.9176 0.6350 0.063 Uiso 1 1 calc R . . C51 C 0.2245(4) 0.89050(19) 0.5945(3) 0.0402(12) Uani 1 1 d . . . H51A H 0.2132 0.9091 0.5613 0.048 Uiso 1 1 calc R . . C52 C 0.5730(4) 0.84916(17) 0.43561(19) 0.0275(10) Uani 1 1 d . . . C53 C 0.6501(4) 0.8470(2) 0.3934(2) 0.0380(13) Uani 1 1 d . . . C54 C 0.7066(5) 0.8836(2) 0.3836(2) 0.0475(15) Uani 1 1 d . . . H54A H 0.6972 0.9093 0.4041 0.057 Uiso 1 1 calc R . . C55 C 0.7776(5) 0.8825(3) 0.3433(3) 0.068(2) Uani 1 1 d . . . H55A H 0.8164 0.9075 0.3357 0.081 Uiso 1 1 calc R . . C56 C 0.7901(5) 0.8450(4) 0.3152(3) 0.079(3) Uani 1 1 d . . . H56A H 0.8392 0.8440 0.2883 0.095 Uiso 1 1 calc R . . C57 C 0.7337(5) 0.8085(3) 0.3245(3) 0.061(2) Uani 1 1 d . . . H57A H 0.7440 0.7830 0.3038 0.073 Uiso 1 1 calc R . . C58 C 0.6620(5) 0.8085(2) 0.3639(2) 0.0476(15) Uani 1 1 d . . . H58A H 0.6226 0.7835 0.3705 0.057 Uiso 1 1 calc R . . C59 C 0.5387(6) 0.6846(2) 0.4240(3) 0.0524(17) Uani 1 1 d . . . C60 C 0.5936(8) 0.6731(3) 0.3721(4) 0.075(2) Uani 1 1 d . . . C61 C 0.4856(7) 0.6526(2) 0.4462(4) 0.066(2) Uani 1 1 d . . . H61A H 0.4863 0.6244 0.4307 0.079 Uiso 1 1 calc R . . C62 C 0.4295(6) 0.6611(2) 0.4919(3) 0.0554(17) Uani 1 1 d . A . C63 C 0.3668(4) 0.62398(16) 0.5169(2) 0.078(3) Uani 1 1 d D . . C64 C 0.5114(4) 0.71071(17) 0.6453(2) 0.0425(13) Uani 1 1 d D B . C65 C 0.4358(4) 0.70245(14) 0.6915(2) 0.0578(18) Uani 1 1 d D . . C66 C 0.5909(5) 0.6813(2) 0.6406(2) 0.0418(13) Uani 1 1 d . . . H66A H 0.6015 0.6575 0.6667 0.050 Uiso 1 1 calc R B . C67 C 0.6560(5) 0.6858(2) 0.5983(3) 0.0434(14) Uani 1 1 d . B . C68 C 0.7484(6) 0.6542(2) 0.5984(3) 0.0540(16) Uani 1 1 d . . . C69 C 0.2914(8) 1.0160(2) 0.3838(4) 0.071(2) Uani 1 1 d . . . C70 C 0.2869(5) 1.04679(17) 0.3286(3) 0.099(4) Uani 1 1 d D . . C71 C 0.2106(8) 1.0229(2) 0.4157(4) 0.075(2) Uani 1 1 d . . . H71A H 0.1601 1.0456 0.4055 0.090 Uiso 1 1 calc R . . C72 C 0.2028(7) 0.9959(2) 0.4639(4) 0.067(2) Uani 1 1 d . C . C73 C 0.1088(4) 1.00315(14) 0.4961(2) 0.070(2) Uani 1 1 d D . . C74 C 0.6178(6) 1.0106(3) 0.4302(4) 0.065(2) Uani 1 1 d . . . C75 C 0.7012(7) 1.0170(3) 0.3909(4) 0.072(2) Uani 1 1 d . . . C76 C 0.5849(6) 1.0471(3) 0.4603(4) 0.0639(19) Uani 1 1 d . . . H76A H 0.6124 1.0746 0.4535 0.077 Uiso 1 1 calc R . . C77 C 0.5124(8) 1.0425(3) 0.4997(4) 0.070(2) Uani 1 1 d . D . C78 C 0.4823(4) 1.08531(17) 0.5300(2) 0.082(3) Uani 1 1 d 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 Tb1 0.02402(10) 0.04970(14) 0.02852(10) -0.00081(10) 0.00327(8) 0.00217(10) Tb2 0.03243(12) 0.04467(14) 0.03979(13) -0.00459(11) 0.00583(10) -0.00566(11) Zn1 0.0187(2) 0.0354(3) 0.0224(2) -0.0012(2) 0.00144(19) -0.0011(2) Zn2 0.0196(2) 0.0480(3) 0.0242(3) -0.0057(2) 0.0034(2) -0.0033(2) F1 0.160(5) 0.169(5) 0.078(3) -0.002(3) 0.050(4) 0.058(4) F2 0.119(5) 0.213(6) 0.131(5) -0.061(4) 0.061(4) 0.023(5) F3 0.199(6) 0.116(4) 0.137(5) -0.045(4) 0.085(4) 0.029(4) F4 0.154(6) 0.130(5) 0.116(5) -0.021(4) 0.012(5) -0.072(5) F5 0.080(4) 0.077(4) 0.136(5) 0.014(4) 0.036(4) 0.000(3) F6 0.103(5) 0.080(4) 0.132(6) 0.024(4) 0.017(4) 0.007(4) F4A 0.154(6) 0.130(5) 0.116(5) -0.021(4) 0.012(5) -0.072(5) F5A 0.080(4) 0.077(4) 0.136(5) 0.014(4) 0.036(4) 0.000(3) F6A 0.103(5) 0.080(4) 0.132(6) 0.024(4) 0.017(4) 0.007(4) F7 0.0339(19) 0.152(4) 0.066(2) 0.050(3) 0.0086(18) 0.004(2) F8 0.066(2) 0.099(3) 0.052(2) 0.004(2) 0.028(2) 0.021(2) F9 0.048(2) 0.091(3) 0.0445(18) 0.0270(18) 0.0124(16) -0.0070(19) F10 0.091(3) 0.107(4) 0.115(4) 0.032(3) 0.054(3) 0.048(3) F11 0.080(3) 0.071(3) 0.156(5) -0.009(3) 0.021(3) 0.010(3) F12 0.078(3) 0.134(4) 0.082(3) -0.014(3) -0.020(3) 0.046(3) F13 0.102(5) 0.138(6) 0.114(5) -0.030(4) 0.053(4) 0.040(4) F14 0.115(5) 0.099(4) 0.153(6) 0.026(4) 0.062(4) 0.060(3) F15 0.085(4) 0.083(4) 0.134(6) -0.003(4) 0.054(4) 0.007(3) F13A 0.102(5) 0.138(6) 0.114(5) -0.030(4) 0.053(4) 0.040(4) F14A 0.115(5) 0.099(4) 0.153(6) 0.026(4) 0.062(4) 0.060(3) F15A 0.085(4) 0.083(4) 0.134(6) -0.003(4) 0.054(4) 0.007(3) F16 0.202(7) 0.132(5) 0.158(5) 0.064(4) 0.090(5) 0.058(5) F17 0.198(7) 0.148(5) 0.117(5) 0.044(4) -0.022(5) -0.054(5) F18 0.137(5) 0.066(3) 0.111(4) 0.006(3) 0.019(4) -0.017(3) F19 0.107(4) 0.046(3) 0.086(4) 0.003(3) 0.042(3) 0.005(3) F20 0.124(5) 0.067(5) 0.142(5) -0.010(4) 0.042(4) -0.016(4) F21 0.123(5) 0.083(4) 0.114(5) 0.002(4) 0.036(4) 0.017(4) F19A 0.107(4) 0.046(3) 0.086(4) 0.003(3) 0.042(3) 0.005(3) F20A 0.124(5) 0.067(5) 0.142(5) -0.010(4) 0.042(4) -0.016(4) F21A 0.123(5) 0.083(4) 0.114(5) 0.002(4) 0.036(4) 0.017(4) F22 0.141(5) 0.131(4) 0.092(3) -0.021(3) 0.054(3) -0.066(4) F23 0.075(4) 0.179(6) 0.173(6) 0.042(5) 0.049(4) -0.016(4) F24 0.115(4) 0.105(4) 0.118(4) 0.012(3) 0.057(3) -0.045(3) O1 0.0186(14) 0.0388(17) 0.0250(15) 0.0002(13) 0.0024(12) -0.0039(13) O2 0.0277(16) 0.0373(18) 0.0233(15) 0.0040(13) 0.0006(13) -0.0005(13) O3 0.0201(15) 0.050(2) 0.0256(16) -0.0018(14) 0.0028(13) 0.0002(14) O4 0.0297(18) 0.051(2) 0.0285(17) -0.0096(15) 0.0061(14) 0.0040(15) O5 0.0228(15) 0.0429(19) 0.0301(16) -0.0034(14) 0.0081(13) 0.0006(14) O6 0.0219(15) 0.0383(18) 0.0270(16) -0.0034(14) 0.0045(13) -0.0011(13) O7 0.0239(15) 0.0411(18) 0.0203(14) -0.0022(13) 0.0037(12) 0.0014(13) O8 0.0248(16) 0.047(2) 0.0256(16) -0.0017(14) 0.0055(13) -0.0049(14) O9 0.048(2) 0.058(2) 0.0293(18) -0.0067(17) 0.0059(17) 0.0192(19) O10 0.0292(18) 0.044(2) 0.051(2) -0.0028(18) -0.0041(17) 0.0001(16) O11 0.0337(19) 0.053(2) 0.0328(18) 0.0037(16) 0.0123(15) -0.0024(16) O12 0.0311(18) 0.052(2) 0.0283(17) 0.0037(16) 0.0011(15) 0.0059(16) O13 0.039(2) 0.039(2) 0.055(2) -0.0079(17) 0.0135(18) 0.0061(16) O14 0.049(2) 0.041(2) 0.048(2) -0.0031(18) 0.0047(19) -0.0045(18) O15 0.048(2) 0.052(2) 0.052(2) -0.0085(19) 0.012(2) -0.0115(19) O16 0.037(2) 0.052(2) 0.053(2) 0.0036(19) 0.0082(18) -0.0118(18) N1 0.0237(18) 0.041(2) 0.029(2) 0.0013(17) 0.0057(16) -0.0003(16) N2 0.0204(17) 0.041(2) 0.0272(19) 0.0012(16) 0.0032(15) 0.0005(16) N3 0.027(2) 0.062(3) 0.0232(19) -0.0071(18) 0.0076(16) -0.0073(19) N4 0.0224(19) 0.056(3) 0.035(2) -0.0067(19) 0.0089(17) -0.0051(18) C1 0.0158(19) 0.036(2) 0.034(2) 0.005(2) -0.0008(17) -0.0003(17) C2 0.021(2) 0.048(3) 0.039(3) 0.002(2) 0.000(2) 0.001(2) C3 0.029(2) 0.043(3) 0.055(3) 0.011(2) 0.010(2) -0.004(2) C4 0.049(3) 0.042(3) 0.050(3) 0.002(3) 0.002(3) -0.015(3) C5 0.043(3) 0.037(3) 0.046(3) -0.010(2) -0.004(2) -0.008(2) C6 0.029(2) 0.036(3) 0.031(2) 0.002(2) -0.001(2) 0.000(2) C7 0.022(2) 0.069(4) 0.033(3) 0.003(3) 0.009(2) -0.003(2) C8 0.077(5) 0.064(4) 0.080(5) 0.003(4) -0.009(4) -0.035(4) C9 0.032(2) 0.033(2) 0.033(2) -0.002(2) 0.006(2) -0.0001(19) C10 0.028(2) 0.059(3) 0.024(2) -0.005(2) 0.0054(19) -0.001(2) C11 0.027(2) 0.042(3) 0.029(2) -0.004(2) -0.0034(19) 0.001(2) C12 0.022(2) 0.043(3) 0.031(2) -0.007(2) -0.0008(18) -0.0061(19) C13 0.024(2) 0.052(3) 0.030(2) -0.005(2) 0.0063(19) 0.001(2) C14 0.021(2) 0.037(3) 0.044(3) -0.003(2) 0.003(2) 0.0085(19) C15 0.030(2) 0.045(3) 0.033(3) 0.004(2) -0.002(2) 0.005(2) C16 0.040(3) 0.051(3) 0.047(3) 0.010(3) -0.007(3) 0.000(3) C17 0.069(4) 0.043(3) 0.047(3) 0.010(3) -0.012(3) -0.001(3) C18 0.063(4) 0.052(4) 0.040(3) 0.014(3) 0.004(3) -0.004(3) C19 0.043(3) 0.051(3) 0.034(3) 0.007(2) 0.002(2) -0.006(3) C20 0.032(2) 0.040(3) 0.029(2) 0.007(2) -0.002(2) -0.001(2) C21 0.072(6) 0.125(7) 0.062(5) 0.043(5) -0.022(4) -0.002(5) C22 0.048(3) 0.071(4) 0.049(3) 0.011(3) 0.013(3) -0.018(3) C23 0.017(2) 0.051(3) 0.033(2) 0.003(2) 0.0023(18) 0.0008(19) C24 0.021(2) 0.056(3) 0.031(2) 0.004(2) 0.0045(19) 0.005(2) C25 0.021(2) 0.062(4) 0.045(3) 0.008(3) 0.001(2) 0.010(2) C26 0.022(2) 0.077(4) 0.034(3) 0.013(3) -0.005(2) -0.003(2) C27 0.029(3) 0.075(4) 0.028(2) 0.013(3) -0.002(2) -0.010(3) C28 0.018(2) 0.060(3) 0.031(2) 0.007(2) 0.0052(19) -0.005(2) C29 0.030(3) 0.069(4) 0.032(3) 0.002(2) 0.012(2) 0.007(2) C30 0.032(3) 0.099(6) 0.049(4) 0.014(4) -0.003(3) 0.008(3) C31 0.025(2) 0.071(4) 0.027(2) -0.004(2) 0.0041(19) -0.004(2) C32 0.036(3) 0.082(5) 0.036(3) -0.012(3) 0.016(2) -0.005(3) C33 0.032(3) 0.070(4) 0.027(3) -0.005(2) 0.003(2) -0.006(3) C34 0.024(2) 0.067(4) 0.031(3) -0.008(2) 0.002(2) -0.011(2) C35 0.023(2) 0.077(4) 0.033(3) -0.005(3) 0.010(2) -0.006(2) C36 0.032(3) 0.053(3) 0.044(3) -0.010(3) 0.005(2) -0.017(2) C37 0.035(3) 0.053(3) 0.044(3) -0.017(3) 0.008(2) -0.009(2) C38 0.047(4) 0.083(5) 0.075(5) -0.036(4) 0.006(3) -0.014(4) C39 0.060(5) 0.107(6) 0.086(5) -0.060(5) 0.014(4) -0.031(4) C40 0.057(4) 0.089(5) 0.074(4) -0.058(4) 0.006(4) -0.007(4) C41 0.042(3) 0.069(4) 0.054(3) -0.028(3) 0.012(3) -0.005(3) C42 0.035(3) 0.050(3) 0.031(2) -0.022(2) 0.001(2) -0.005(2) C43 0.072(6) 0.120(8) 0.166(11) -0.091(8) -0.004(7) -0.020(6) C44 0.051(4) 0.076(5) 0.062(4) -0.026(3) 0.020(3) -0.005(3) C45 0.020(2) 0.042(3) 0.026(2) -0.012(2) 0.0002(17) -0.0059(19) C46 0.023(2) 0.045(3) 0.032(2) -0.012(2) 0.0059(19) -0.009(2) C47 0.033(3) 0.072(4) 0.029(2) -0.004(3) 0.008(2) -0.008(3) C48 0.047(3) 0.088(5) 0.034(3) -0.005(3) 0.016(3) -0.005(3) C49 0.052(4) 0.106(6) 0.055(4) -0.021(4) 0.034(3) -0.002(4) C50 0.036(3) 0.072(4) 0.055(4) -0.019(3) 0.025(3) -0.002(3) C51 0.025(2) 0.050(3) 0.048(3) -0.016(2) 0.013(2) -0.002(2) C52 0.0161(18) 0.048(3) 0.018(2) 0.0022(19) 0.0022(16) 0.0023(18) C53 0.021(2) 0.074(4) 0.020(2) -0.005(2) 0.0051(18) 0.001(2) C54 0.028(2) 0.085(4) 0.031(3) 0.008(3) 0.009(2) -0.011(3) C55 0.032(3) 0.141(7) 0.033(3) 0.006(4) 0.014(2) -0.016(4) C56 0.025(3) 0.178(9) 0.039(3) 0.001(4) 0.016(3) 0.011(4) C57 0.031(3) 0.124(6) 0.026(3) -0.015(3) -0.003(2) 0.015(4) C58 0.025(2) 0.089(5) 0.026(2) -0.010(3) -0.002(2) 0.015(3) C59 0.056(4) 0.062(4) 0.037(3) -0.014(3) 0.003(3) 0.020(3) C60 0.087(6) 0.083(6) 0.059(4) -0.019(4) 0.021(4) 0.027(5) C61 0.073(5) 0.052(4) 0.069(5) -0.010(3) 0.007(4) 0.013(4) C62 0.044(3) 0.058(4) 0.061(4) -0.006(3) 0.001(3) 0.010(3) C63 0.084(6) 0.042(4) 0.092(6) -0.001(4) -0.021(5) -0.009(4) C64 0.028(2) 0.069(4) 0.029(2) 0.010(2) 0.005(2) -0.006(2) C65 0.035(3) 0.101(5) 0.036(3) 0.016(3) 0.002(2) 0.010(3) C66 0.038(3) 0.055(3) 0.031(3) 0.009(2) 0.002(2) 0.004(2) C67 0.034(3) 0.046(3) 0.045(3) -0.003(3) -0.004(2) -0.001(2) C68 0.050(4) 0.058(4) 0.053(4) 0.015(3) 0.009(3) 0.020(3) C69 0.098(6) 0.036(4) 0.081(5) 0.007(3) 0.021(5) 0.011(4) C70 0.144(10) 0.043(4) 0.107(8) 0.028(5) 0.014(7) 0.008(5) C71 0.078(5) 0.051(4) 0.096(6) 0.011(4) 0.019(5) 0.023(4) C72 0.057(4) 0.059(4) 0.089(5) -0.008(4) 0.028(4) 0.002(3) C73 0.079(5) 0.058(4) 0.079(5) -0.008(4) 0.031(4) 0.027(4) C74 0.047(4) 0.080(5) 0.069(5) 0.013(4) 0.012(3) -0.018(3) C75 0.067(5) 0.081(5) 0.075(5) -0.007(4) 0.029(4) -0.035(4) C76 0.061(4) 0.060(4) 0.075(5) -0.007(4) 0.025(4) -0.018(3) C77 0.085(6) 0.058(4) 0.071(5) -0.017(4) 0.023(4) -0.020(4) C78 0.076(6) 0.072(5) 0.108(7) -0.024(5) 0.039(5) -0.015(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 Tb1 O1 2.376(3) . ? Tb1 O3 2.401(3) . ? Tb1 O11 2.429(4) . ? Tb1 O9 2.434(4) . ? Tb1 O10 2.455(4) . ? Tb1 O12 2.457(4) . ? Tb1 O5 2.487(3) . ? Tb1 O7 2.492(3) . ? Tb2 O2 2.383(3) . ? Tb2 O16 2.406(4) . ? Tb2 O4 2.409(4) . ? Tb2 O13 2.417(4) . ? Tb2 O15 2.453(4) . ? Tb2 O14 2.469(4) . ? Tb2 O8 2.485(4) . ? Tb2 O6 2.532(3) . ? Zn1 O2 2.032(3) . ? Zn1 O1 2.045(3) . ? Zn1 N2 2.139(4) . ? Zn1 N1 2.147(4) . ? Zn1 O6 2.303(3) . ? Zn1 O7 2.337(3) . ? Zn2 O4 2.025(4) . ? Zn2 O3 2.029(4) . ? Zn2 N3 2.155(4) . ? Zn2 N4 2.158(4) . ? Zn2 O8 2.318(3) . ? Zn2 O5 2.385(3) . ? F1 C60 1.260(11) . ? F2 C60 1.273(12) . ? F3 C60 1.292(10) . ? F4 C63 1.301(5) . ? F5 C63 1.311(5) . ? F6 C63 1.296(5) . ? F4A C63 1.297(5) . ? F5A C63 1.299(5) . ? F6A C63 1.305(5) . ? F7 C65 1.304(4) . ? F8 C65 1.304(4) . ? F9 C65 1.304(4) . ? F10 C68 1.276(9) . ? F11 C68 1.320(9) . ? F12 C68 1.341(8) . ? F13 C73 1.300(5) . ? F14 C73 1.294(5) . ? F15 C73 1.293(5) . ? F13A C73 1.304(4) . ? F14A C73 1.313(4) . ? F15A C73 1.304(5) . ? F16 C70 1.293(5) . ? F17 C70 1.310(5) . ? F18 C70 1.300(4) . ? F19 C78 1.281(5) . ? F20 C78 1.308(5) . ? F21 C78 1.298(5) . ? F19A C78 1.294(5) . ? F20A C78 1.303(5) . ? F21A C78 1.323(5) . ? F22 C75 1.301(10) . ? F23 C75 1.277(12) . ? F24 C75 1.314(10) . ? O1 C1 1.372(6) . ? O2 C20 1.377(6) . ? O3 C23 1.374(6) . ? O4 C42 1.340(6) . ? O5 C45 1.275(6) . ? O6 C45 1.264(6) . ? O7 C52 1.268(6) . ? O8 C52 1.264(6) . ? O9 C59 1.271(8) . ? O10 C62 1.251(8) . ? O11 C64 1.279(6) . ? O12 C67 1.261(7) . ? O13 C72 1.269(9) . ? O14 C69 1.245(10) . ? O15 C77 1.198(9) . ? O16 C74 1.259(9) . ? N1 C10 1.473(6) . ? N1 C11 1.485(6) . ? N1 C9 1.489(7) . ? N2 C12 1.481(6) . ? N2 C14 1.496(6) . ? N2 C13 1.503(6) . ? N3 C32 1.484(7) . ? N3 C31 1.492(8) . ? N3 C33 1.495(7) . ? N4 C36 1.482(8) . ? N4 C35 1.489(7) . ? N4 C34 1.498(7) . ? C1 C6 1.387(7) . ? C1 C2 1.393(7) . ? C2 C3 1.380(8) . ? C2 C7 1.505(8) . ? C3 C4 1.423(9) . ? C3 H3A 0.9500 . ? C4 C5 1.380(9) . ? C4 C8 1.527(9) . ? C5 C6 1.398(8) . ? C5 H5A 0.9500 . ? C6 C9 1.496(7) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.533(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.480(8) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.404(8) . ? C15 C16 1.410(8) . ? C16 C17 1.382(10) . ? C16 H16A 0.9500 . ? C17 C18 1.389(11) . ? C17 C21 1.526(10) . ? C18 C19 1.379(9) . ? C18 H18A 0.9500 . ? C19 C20 1.396(8) . ? C19 C22 1.517(9) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C28 1.391(7) . ? C23 C24 1.405(7) . ? C24 C25 1.393(7) . ? C24 C29 1.503(8) . ? C25 C26 1.379(8) . ? C25 H25A 0.9500 . ? C26 C27 1.386(9) . ? C26 C30 1.503(8) . ? C27 C28 1.411(8) . ? C27 H27A 0.9500 . ? C28 C31 1.487(8) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.520(8) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.492(8) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C42 1.399(8) . ? C37 C38 1.404(9) . ? C38 C39 1.372(11) . ? C38 H38A 0.9500 . ? C39 C40 1.431(12) . ? C39 C43 1.504(11) . ? C40 C41 1.381(9) . ? C40 H40A 0.9500 . ? C41 C42 1.432(8) . ? C41 C44 1.472(10) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.496(7) . ? C46 C51 1.388(8) . ? C46 C47 1.405(8) . ? C47 C48 1.381(8) . ? C47 H47A 0.9500 . ? C48 C49 1.404(11) . ? C48 H48A 0.9500 . ? C49 C50 1.370(11) . ? C49 H49A 0.9500 . ? C50 C51 1.390(8) . ? C50 H50A 0.9500 . ? C51 H51A 0.9500 . ? C52 C53 1.493(6) . ? C53 C54 1.384(9) . ? C53 C58 1.404(9) . ? C54 C55 1.400(8) . ? C54 H54A 0.9500 . ? C55 C56 1.364(13) . ? C55 H55A 0.9500 . ? C56 C57 1.377(13) . ? C56 H56A 0.9500 . ? C57 C58 1.388(9) . ? C57 H57A 0.9500 . ? C58 H58A 0.9500 . ? C59 C61 1.352(11) . ? C59 C60 1.529(10) . ? C61 C62 1.397(11) . ? C61 H61A 0.9500 . ? C62 C63 1.568(10) . ? C64 C66 1.372(8) . ? C64 C65 1.571(7) . ? C66 C67 1.389(9) . ? C66 H66A 0.9500 . ? C67 C68 1.516(9) . ? C69 C71 1.372(13) . ? C69 C70 1.590(11) . ? C71 C72 1.412(12) . ? C71 H71A 0.9500 . ? C72 C73 1.518(9) . ? C74 C76 1.434(12) . ? C74 C75 1.517(11) . ? C76 C77 1.404(12) . ? C76 H76A 0.9500 . ? C77 C78 1.586(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Tb1 O3 135.68(12) . . ? O1 Tb1 O11 104.83(12) . . ? O3 Tb1 O11 93.43(12) . . ? O1 Tb1 O9 91.98(13) . . ? O3 Tb1 O9 106.14(14) . . ? O11 Tb1 O9 130.77(14) . . ? O1 Tb1 O10 76.55(12) . . ? O3 Tb1 O10 147.59(12) . . ? O11 Tb1 O10 70.20(14) . . ? O9 Tb1 O10 69.43(15) . . ? O1 Tb1 O12 148.25(12) . . ? O3 Tb1 O12 75.92(13) . . ? O11 Tb1 O12 69.93(12) . . ? O9 Tb1 O12 71.83(13) . . ? O10 Tb1 O12 72.24(13) . . ? O1 Tb1 O5 77.97(11) . . ? O3 Tb1 O5 68.44(11) . . ? O11 Tb1 O5 74.52(12) . . ? O9 Tb1 O5 154.69(13) . . ? O10 Tb1 O5 128.74(13) . . ? O12 Tb1 O5 127.12(12) . . ? O1 Tb1 O7 68.67(11) . . ? O3 Tb1 O7 77.31(11) . . ? O11 Tb1 O7 154.07(12) . . ? O9 Tb1 O7 75.15(13) . . ? O10 Tb1 O7 128.65(12) . . ? O12 Tb1 O7 128.99(12) . . ? O5 Tb1 O7 79.55(11) . . ? O2 Tb2 O16 104.02(13) . . ? O2 Tb2 O4 135.13(12) . . ? O16 Tb2 O4 92.42(14) . . ? O2 Tb2 O13 92.61(13) . . ? O16 Tb2 O13 131.79(14) . . ? O4 Tb2 O13 107.01(13) . . ? O2 Tb2 O15 147.79(13) . . ? O16 Tb2 O15 70.89(15) . . ? O4 Tb2 O15 77.02(14) . . ? O13 Tb2 O15 71.31(14) . . ? O2 Tb2 O14 76.59(12) . . ? O16 Tb2 O14 70.49(15) . . ? O4 Tb2 O14 147.85(13) . . ? O13 Tb2 O14 70.04(15) . . ? O15 Tb2 O14 71.75(14) . . ? O2 Tb2 O8 76.95(11) . . ? O16 Tb2 O8 74.91(13) . . ? O4 Tb2 O8 67.42(11) . . ? O13 Tb2 O8 153.27(13) . . ? O15 Tb2 O8 128.74(13) . . ? O14 Tb2 O8 129.09(13) . . ? O2 Tb2 O6 68.32(11) . . ? O16 Tb2 O6 152.95(13) . . ? O4 Tb2 O6 78.12(12) . . ? O13 Tb2 O6 75.21(12) . . ? O15 Tb2 O6 129.60(13) . . ? O14 Tb2 O6 128.60(13) . . ? O8 Tb2 O6 78.07(11) . . ? O2 Zn1 O1 160.79(13) . . ? O2 Zn1 N2 94.20(15) . . ? O1 Zn1 N2 101.11(14) . . ? O2 Zn1 N1 99.14(15) . . ? O1 Zn1 N1 93.59(14) . . ? N2 Zn1 N1 85.59(15) . . ? O2 Zn1 O6 78.90(13) . . ? O1 Zn1 O6 88.76(12) . . ? N2 Zn1 O6 92.71(14) . . ? N1 Zn1 O6 177.32(14) . . ? O2 Zn1 O7 87.77(13) . . ? O1 Zn1 O7 77.31(12) . . ? N2 Zn1 O7 177.42(14) . . ? N1 Zn1 O7 92.45(13) . . ? O6 Zn1 O7 89.31(11) . . ? O4 Zn2 O3 159.64(14) . . ? O4 Zn2 N3 99.84(16) . . ? O3 Zn2 N3 95.00(16) . . ? O4 Zn2 N4 94.29(17) . . ? O3 Zn2 N4 100.86(16) . . ? N3 Zn2 N4 84.93(17) . . ? O4 Zn2 O8 77.13(13) . . ? O3 Zn2 O8 88.02(13) . . ? N3 Zn2 O8 176.96(16) . . ? N4 Zn2 O8 94.91(15) . . ? O4 Zn2 O5 88.66(13) . . ? O3 Zn2 O5 76.60(13) . . ? N3 Zn2 O5 93.24(14) . . ? N4 Zn2 O5 176.76(16) . . ? O8 Zn2 O5 87.05(12) . . ? C1 O1 Zn1 115.0(3) . . ? C1 O1 Tb1 126.4(3) . . ? Zn1 O1 Tb1 111.31(14) . . ? C20 O2 Zn1 116.0(3) . . ? C20 O2 Tb2 123.8(3) . . ? Zn1 O2 Tb2 111.32(14) . . ? C23 O3 Zn2 115.2(3) . . ? C23 O3 Tb1 124.1(3) . . ? Zn2 O3 Tb1 112.56(14) . . ? C42 O4 Zn2 116.5(3) . . ? C42 O4 Tb2 122.9(3) . . ? Zn2 O4 Tb2 111.95(15) . . ? C45 O5 Zn2 117.4(3) . . ? C45 O5 Tb1 127.3(3) . . ? Zn2 O5 Tb1 98.46(12) . . ? C45 O6 Zn1 120.1(3) . . ? C45 O6 Tb2 125.4(3) . . ? Zn1 O6 Tb2 97.97(12) . . ? C52 O7 Zn1 118.2(3) . . ? C52 O7 Tb1 126.2(3) . . ? Zn1 O7 Tb1 98.32(12) . . ? C52 O8 Zn2 119.2(3) . . ? C52 O8 Tb2 127.5(3) . . ? Zn2 O8 Tb2 100.01(12) . . ? C59 O9 Tb1 133.7(4) . . ? C62 O10 Tb1 135.7(5) . . ? C64 O11 Tb1 130.4(3) . . ? C67 O12 Tb1 134.1(4) . . ? C72 O13 Tb2 136.4(5) . . ? C69 O14 Tb2 133.5(5) . . ? C77 O15 Tb2 135.6(5) . . ? C74 O16 Tb2 133.8(5) . . ? C10 N1 C11 108.8(4) . . ? C10 N1 C9 106.6(4) . . ? C11 N1 C9 111.5(4) . . ? C10 N1 Zn1 115.4(3) . . ? C11 N1 Zn1 106.6(3) . . ? C9 N1 Zn1 107.9(3) . . ? C12 N2 C14 112.3(4) . . ? C12 N2 C13 107.9(4) . . ? C14 N2 C13 107.4(4) . . ? C12 N2 Zn1 106.1(3) . . ? C14 N2 Zn1 108.6(3) . . ? C13 N2 Zn1 114.6(3) . . ? C32 N3 C31 106.5(4) . . ? C32 N3 C33 109.3(4) . . ? C31 N3 C33 113.3(4) . . ? C32 N3 Zn2 114.5(3) . . ? C31 N3 Zn2 107.2(3) . . ? C33 N3 Zn2 106.1(3) . . ? C36 N4 C35 106.5(5) . . ? C36 N4 C34 113.9(4) . . ? C35 N4 C34 107.9(4) . . ? C36 N4 Zn2 106.7(3) . . ? C35 N4 Zn2 114.8(3) . . ? C34 N4 Zn2 107.2(3) . . ? O1 C1 C6 119.5(4) . . ? O1 C1 C2 120.9(4) . . ? C6 C1 C2 119.6(5) . . ? C3 C2 C1 119.3(5) . . ? C3 C2 C7 120.7(5) . . ? C1 C2 C7 119.9(5) . . ? C2 C3 C4 122.0(5) . . ? C2 C3 H3A 119.0 . . ? C4 C3 H3A 119.0 . . ? C5 C4 C3 117.3(5) . . ? C5 C4 C8 120.9(6) . . ? C3 C4 C8 121.9(6) . . ? C4 C5 C6 121.2(6) . . ? C4 C5 H5A 119.4 . . ? C6 C5 H5A 119.4 . . ? C1 C6 C5 120.5(5) . . ? C1 C6 C9 120.2(5) . . ? C5 C6 C9 119.3(5) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 C6 114.7(4) . . ? N1 C9 H9A 108.6 . . ? C6 C9 H9A 108.6 . . ? N1 C9 H9B 108.6 . . ? C6 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 113.1(4) . . ? N1 C11 H11A 109.0 . . ? C12 C11 H11A 109.0 . . ? N1 C11 H11B 109.0 . . ? C12 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? N2 C12 C11 113.9(4) . . ? N2 C12 H12A 108.8 . . ? C11 C12 H12A 108.8 . . ? N2 C12 H12B 108.8 . . ? C11 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? N2 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 N2 114.4(4) . . ? C15 C14 H14A 108.7 . . ? N2 C14 H14A 108.7 . . ? C15 C14 H14B 108.7 . . ? N2 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? C20 C15 C16 119.2(5) . . ? C20 C15 C14 121.1(5) . . ? C16 C15 C14 119.7(5) . . ? C17 C16 C15 121.1(6) . . ? C17 C16 H16A 119.5 . . ? C15 C16 H16A 119.5 . . ? C16 C17 C18 118.3(6) . . ? C16 C17 C21 120.5(7) . . ? C18 C17 C21 121.2(7) . . ? C19 C18 C17 122.4(6) . . ? C19 C18 H18A 118.8 . . ? C17 C18 H18A 118.8 . . ? C18 C19 C20 119.4(6) . . ? C18 C19 C22 120.9(6) . . ? C20 C19 C22 119.7(5) . . ? O2 C20 C19 120.9(5) . . ? O2 C20 C15 119.4(5) . . ? C19 C20 C15 119.7(5) . . ? C17 C21 H21A 109.5 . . ? C17 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C17 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O3 C23 C28 120.1(5) . . ? O3 C23 C24 119.8(4) . . ? C28 C23 C24 120.1(5) . . ? C25 C24 C23 118.1(5) . . ? C25 C24 C29 120.6(5) . . ? C23 C24 C29 121.3(5) . . ? C26 C25 C24 123.9(5) . . ? C26 C25 H25A 118.1 . . ? C24 C25 H25A 118.1 . . ? C25 C26 C27 116.7(5) . . ? C25 C26 C30 121.9(6) . . ? C27 C26 C30 121.4(6) . . ? C26 C27 C28 122.2(5) . . ? C26 C27 H27A 118.9 . . ? C28 C27 H27A 118.9 . . ? C23 C28 C27 119.0(5) . . ? C23 C28 C31 121.0(5) . . ? C27 C28 C31 120.0(5) . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C26 C30 H30A 109.5 . . ? C26 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C26 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 N3 115.9(5) . . ? C28 C31 H31A 108.3 . . ? N3 C31 H31A 108.3 . . ? C28 C31 H31B 108.3 . . ? N3 C31 H31B 108.3 . . ? H31A C31 H31B 107.4 . . ? N3 C32 H32A 109.5 . . ? N3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N3 C33 C34 114.3(4) . . ? N3 C33 H33A 108.7 . . ? C34 C33 H33A 108.7 . . ? N3 C33 H33B 108.7 . . ? C34 C33 H33B 108.7 . . ? H33A C33 H33B 107.6 . . ? N4 C34 C33 112.6(4) . . ? N4 C34 H34A 109.1 . . ? C33 C34 H34A 109.1 . . ? N4 C34 H34B 109.1 . . ? C33 C34 H34B 109.1 . . ? H34A C34 H34B 107.8 . . ? N4 C35 H35A 109.5 . . ? N4 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N4 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N4 C36 C37 114.2(5) . . ? N4 C36 H36A 108.7 . . ? C37 C36 H36A 108.7 . . ? N4 C36 H36B 108.7 . . ? C37 C36 H36B 108.7 . . ? H36A C36 H36B 107.6 . . ? C42 C37 C38 120.6(6) . . ? C42 C37 C36 120.3(5) . . ? C38 C37 C36 119.0(6) . . ? C39 C38 C37 121.1(7) . . ? C39 C38 H38A 119.5 . . ? C37 C38 H38A 119.5 . . ? C38 C39 C40 118.2(7) . . ? C38 C39 C43 121.8(8) . . ? C40 C39 C43 120.0(8) . . ? C41 C40 C39 122.4(7) . . ? C41 C40 H40A 118.8 . . ? C39 C40 H40A 118.8 . . ? C40 C41 C42 118.2(6) . . ? C40 C41 C44 120.7(6) . . ? C42 C41 C44 121.1(6) . . ? O4 C42 C37 120.1(5) . . ? O4 C42 C41 120.4(5) . . ? C37 C42 C41 119.5(5) . . ? C39 C43 H43A 109.5 . . ? C39 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C39 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O6 C45 O5 123.0(4) . . ? O6 C45 C46 119.2(4) . . ? O5 C45 C46 117.8(5) . . ? C51 C46 C47 119.6(5) . . ? C51 C46 C45 119.7(5) . . ? C47 C46 C45 120.6(5) . . ? C48 C47 C46 119.7(6) . . ? C48 C47 H47A 120.2 . . ? C46 C47 H47A 120.2 . . ? C47 C48 C49 120.0(7) . . ? C47 C48 H48A 120.0 . . ? C49 C48 H48A 120.0 . . ? C50 C49 C48 120.2(6) . . ? C50 C49 H49A 119.9 . . ? C48 C49 H49A 119.9 . . ? C49 C50 C51 120.2(6) . . ? C49 C50 H50A 119.9 . . ? C51 C50 H50A 119.9 . . ? C46 C51 C50 120.3(6) . . ? C46 C51 H51A 119.9 . . ? C50 C51 H51A 119.9 . . ? O8 C52 O7 122.2(4) . . ? O8 C52 C53 118.6(5) . . ? O7 C52 C53 119.3(5) . . ? C54 C53 C58 121.8(5) . . ? C54 C53 C52 118.6(5) . . ? C58 C53 C52 119.6(5) . . ? C53 C54 C55 119.5(7) . . ? C53 C54 H54A 120.3 . . ? C55 C54 H54A 120.3 . . ? C56 C55 C54 118.7(8) . . ? C56 C55 H55A 120.7 . . ? C54 C55 H55A 120.7 . . ? C55 C56 C57 122.0(6) . . ? C55 C56 H56A 119.0 . . ? C57 C56 H56A 119.0 . . ? C56 C57 C58 120.9(7) . . ? C56 C57 H57A 119.6 . . ? C58 C57 H57A 119.6 . . ? C57 C58 C53 117.1(7) . . ? C57 C58 H58A 121.4 . . ? C53 C58 H58A 121.4 . . ? O9 C59 C61 131.2(6) . . ? O9 C59 C60 112.3(7) . . ? C61 C59 C60 116.5(7) . . ? F1 C60 F2 105.6(10) . . ? F1 C60 F3 107.0(8) . . ? F2 C60 F3 105.4(8) . . ? F1 C60 C59 111.9(7) . . ? F2 C60 C59 111.3(7) . . ? F3 C60 C59 115.0(8) . . ? C59 C61 C62 119.7(7) . . ? C59 C61 H61A 120.2 . . ? C62 C61 H61A 120.2 . . ? O10 C62 C61 127.7(7) . . ? O10 C62 C63 112.9(6) . . ? C61 C62 C63 119.4(6) . . ? F6 C63 F4A 54.0(5) . . ? F6 C63 F5A 131.3(7) . . ? F4A C63 F5A 109.3(5) . . ? F6 C63 F4 109.2(5) . . ? F4A C63 F4 138.1(7) . . ? F5A C63 F4 48.9(5) . . ? F6 C63 F6A 55.5(5) . . ? F4A C63 F6A 108.8(5) . . ? F5A C63 F6A 108.3(5) . . ? F4 C63 F6A 62.2(6) . . ? F6 C63 F5 108.0(5) . . ? F4A C63 F5 56.9(5) . . ? F5A C63 F5 60.1(5) . . ? F4 C63 F5 108.0(5) . . ? F6A C63 F5 148.7(7) . . ? F6 C63 C62 112.6(6) . . ? F4A C63 C62 106.5(6) . . ? F5A C63 C62 116.1(6) . . ? F4 C63 C62 115.2(6) . . ? F6A C63 C62 107.7(6) . . ? F5 C63 C62 103.3(6) . . ? O11 C64 C66 129.6(5) . . ? O11 C64 C65 111.9(4) . . ? C66 C64 C65 118.5(4) . . ? F7 C65 F8 108.8(4) . . ? F7 C65 F9 108.2(4) . . ? F8 C65 F9 108.6(4) . . ? F7 C65 C64 110.6(3) . . ? F8 C65 C64 109.8(4) . . ? F9 C65 C64 110.7(4) . . ? C64 C66 C67 120.9(5) . . ? C64 C66 H66A 119.5 . . ? C67 C66 H66A 119.5 . . ? O12 C67 C66 127.2(6) . . ? O12 C67 C68 114.3(6) . . ? C66 C67 C68 118.5(6) . . ? F10 C68 F11 108.4(7) . . ? F10 C68 F12 104.1(6) . . ? F11 C68 F12 106.4(6) . . ? F10 C68 C67 115.0(6) . . ? F11 C68 C67 111.5(6) . . ? F12 C68 C67 110.9(6) . . ? O14 C69 C71 131.1(8) . . ? O14 C69 C70 114.4(7) . . ? C71 C69 C70 114.5(7) . . ? F16 C70 F18 109.5(5) . . ? F16 C70 F17 107.6(5) . . ? F18 C70 F17 108.1(5) . . ? F16 C70 C69 112.7(6) . . ? F18 C70 C69 107.8(5) . . ? F17 C70 C69 111.1(6) . . ? C69 C71 C72 119.6(7) . . ? C69 C71 H71A 120.2 . . ? C72 C71 H71A 120.2 . . ? O13 C72 C71 127.5(7) . . ? O13 C72 C73 114.5(7) . . ? C71 C72 C73 118.0(7) . . ? F15 C73 F14 110.2(5) . . ? F15 C73 F13 109.5(5) . . ? F14 C73 F13 109.6(5) . . ? F15 C73 F13A 153.8(7) . . ? F14 C73 F13A 78.9(6) . . ? F13 C73 F13A 45.3(6) . . ? F15 C73 F15A 45.9(6) . . ? F14 C73 F15A 124.8(9) . . ? F13 C73 F15A 63.5(6) . . ? F13A C73 F15A 108.3(4) . . ? F15 C73 F14A 81.1(7) . . ? F14 C73 F14A 29.7(7) . . ? F13 C73 F14A 127.5(9) . . ? F13A C73 F14A 107.9(4) . . ? F15A C73 F14A 107.8(4) . . ? F15 C73 C72 87.1(8) . . ? F14 C73 C72 118.6(9) . . ? F13 C73 C72 119.1(9) . . ? F13A C73 C72 110.6(6) . . ? F15A C73 C72 109.6(5) . . ? F14A C73 C72 112.5(6) . . ? O16 C74 C76 127.5(7) . . ? O16 C74 C75 114.1(7) . . ? C76 C74 C75 118.3(7) . . ? F23 C75 F22 108.7(9) . . ? F23 C75 F24 107.5(7) . . ? F22 C75 F24 105.7(8) . . ? F23 C75 C74 110.2(8) . . ? F22 C75 C74 110.0(7) . . ? F24 C75 C74 114.6(8) . . ? C77 C76 C74 120.7(7) . . ? C77 C76 H76A 119.7 . . ? C74 C76 H76A 119.7 . . ? O15 C77 C76 128.1(8) . . ? O15 C77 C78 115.9(7) . . ? C76 C77 C78 115.7(6) . . ? F19 C78 F19A 119.7(7) . . ? F19 C78 F21 110.6(5) . . ? F19A C78 F21 16.6(6) . . ? F19 C78 F20A 76.7(5) . . ? F19A C78 F20A 109.1(5) . . ? F21 C78 F20A 122.4(8) . . ? F19 C78 F20 109.7(5) . . ? F19A C78 F20 91.7(6) . . ? F21 C78 F20 108.2(5) . . ? F20A C78 F20 32.9(5) . . ? F19 C78 F21A 29.5(5) . . ? F19A C78 F21A 108.3(5) . . ? F21 C78 F21A 93.8(6) . . ? F20A C78 F21A 106.2(4) . . ? F20 C78 F21A 139.1(6) . . ? F19 C78 C77 118.7(6) . . ? F19A C78 C77 112.7(6) . . ? F21 C78 C77 110.7(8) . . ? F20A C78 C77 114.2(6) . . ? F20 C78 C77 97.9(8) . . ? F21A C78 C77 106.0(6) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.127 _refine_diff_density_min -0.722 _refine_diff_density_rms 0.117 # 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 -0.092 0.057 0.303 92 11 ' ' 2 -0.092 -0.057 0.803 92 11 ' ' 3 0.085 0.362 0.166 20 1 ' ' 4 0.085 0.638 0.666 20 1 ' ' 5 0.408 0.443 0.803 92 11 ' ' 6 0.408 0.557 0.303 92 11 ' ' 7 0.585 0.138 0.666 20 1 ' ' 8 0.585 0.862 0.166 20 1 ' ' _platon_squeeze_details ; ; data_4_Cd2Tb2 _database_code_depnum_ccdc_archive 'CCDC 887298' #TrackingRef '14989_web_deposit_cif_file_0_MuktimoyChaudhury_1351337105.CIF_Zn4_Zn2Tb2_Cd2Tb2 (4).CIF' _vrf_PLAT973_I ; PROBLEM: Large Calcd. Positive Residual Density on Tb1 2.51 eA-3 RESPONSE: These peaks are near Tb, the heaviest atom in the molecule. This is a result of absorption effects even though an absorption correction has been applied to this data. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 H74 Cd2 F24 N4 O16 Tb2' _chemical_formula_sum 'C78 H74 Cd2 F24 N4 O16 Tb2' _chemical_formula_weight 2322.05 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' F F 0.0171 0.0103 '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 orthorhombic _symmetry_space_group_name_H-M 'P b c n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.7645(7) _cell_length_b 28.2743(12) _cell_length_c 18.2405(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8646.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9863 _cell_measurement_theta_min 2.233 _cell_measurement_theta_max 32.170 _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.784 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4560 _exptl_absorpt_coefficient_mu 2.218 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5094 _exptl_absorpt_correction_T_max 0.7478 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 Apex 2' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 171547 _diffrn_reflns_av_R_equivalents 0.0700 _diffrn_reflns_av_sigmaI/netI 0.0589 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -50 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 39.60 _reflns_number_total 26029 _reflns_number_gt 13992 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex 2' _computing_cell_refinement 'Bruker Apex 2' _computing_data_reduction 'Bruker Apex 2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _refine_special_details ; The 57 restaints arise from the fact that for the CF~3~ groups the atomic displacement parameters were constrained to be equivalent and the metrical parameters of these groups were idealized. ; _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^)+(0.0730P)^2^+1.6043P] 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 26029 _refine_ls_number_parameters 627 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.1115 _refine_ls_R_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.1682 _refine_ls_wR_factor_gt 0.1470 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.096 _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 Tb1 Tb 0.5000 0.180331(7) 0.7500 0.02120(5) Uani 1 2 d S . . Tb2 Tb 0.5000 0.383658(7) 0.7500 0.01949(5) Uani 1 2 d S . . Cd1 Cd 0.640080(14) 0.282404(7) 0.741155(12) 0.02196(5) Uani 1 1 d . . . F1 F 0.4085(15) -0.0027(6) 0.7082(15) 0.182(4) Uani 0.166(6) 1 d PD A 1 F2 F 0.3026(6) 0.0373(8) 0.7178(12) 0.1048(19) Uani 0.166(6) 1 d PD A 1 F3 F 0.3742(16) 0.0435(9) 0.6231(5) 0.123(2) Uani 0.166(6) 1 d PD A 1 F1A F 0.4325(3) 0.0161(3) 0.6606(4) 0.182(4) Uani 0.834(6) 1 d PD . 2 F2A F 0.3187(3) 0.04835(14) 0.6465(3) 0.1048(19) Uani 0.834(6) 1 d PD A 2 F3A F 0.3411(4) 0.00351(18) 0.7346(3) 0.123(2) Uani 0.834(6) 1 d PD A 2 F4 F 0.4488(3) 0.1124(3) 0.9926(3) 0.124(2) Uani 0.672(5) 1 d PD B 1 F5 F 0.3332(3) 0.13607(16) 0.9712(3) 0.0885(19) Uani 0.672(5) 1 d PD B 1 F6 F 0.3590(4) 0.06296(13) 0.9715(4) 0.108(3) Uani 0.672(5) 1 d PD B 1 F4A F 0.3133(4) 0.1062(5) 0.9279(6) 0.124(2) Uani 0.328(5) 1 d PD B 2 F5A F 0.3971(8) 0.1368(3) 1.0000(4) 0.0885(19) Uani 0.328(5) 1 d PD B 2 F6A F 0.3970(9) 0.0634(2) 0.9824(8) 0.108(3) Uani 0.328(5) 1 d PD B 2 F7 F 0.6054(11) 0.4286(6) 0.9830(4) 0.122(2) Uani 0.137(5) 1 d PD C 1 F8 F 0.7163(4) 0.4503(7) 0.9423(6) 0.0931(16) Uani 0.137(5) 1 d PD C 1 F9 F 0.6270(12) 0.5006(3) 0.9625(6) 0.0919(17) Uani 0.137(5) 1 d PD C 1 F7A F 0.5739(2) 0.4608(2) 0.98130(19) 0.122(2) Uani 0.863(5) 1 d PD C 2 F8A F 0.6758(3) 0.42168(11) 0.9641(2) 0.0931(16) Uani 0.863(5) 1 d PD C 2 F9A F 0.6770(3) 0.49661(11) 0.95210(18) 0.0919(17) Uani 0.863(5) 1 d PD C 2 F10 F 0.6892(3) 0.55100(15) 0.7129(2) 0.0960(15) Uani 0.905(5) 1 d PD C 1 F11 F 0.5761(2) 0.55258(14) 0.6665(3) 0.0896(13) Uani 0.905(5) 1 d PD C 1 F12 F 0.6654(3) 0.50925(9) 0.62014(17) 0.0714(12) Uani 0.905(5) 1 d PD C 1 F10A F 0.601(2) 0.5120(11) 0.6211(11) 0.0960(15) Uani 0.095(5) 1 d PD C 2 F11A F 0.7101(4) 0.5240(11) 0.675(2) 0.0896(13) Uani 0.095(5) 1 d PD C 2 F12A F 0.608(2) 0.5637(5) 0.7039(16) 0.0714(12) Uani 0.095(5) 1 d PD C 2 O1 O 0.62261(13) 0.20921(7) 0.78458(12) 0.0251(4) Uani 1 1 d . . . O2 O 0.61730(12) 0.35583(7) 0.70122(11) 0.0244(4) Uani 1 1 d . . . O3 O 0.53271(13) 0.24958(7) 0.67067(11) 0.0236(4) Uani 1 1 d . . . O4 O 0.45562(13) 0.31391(7) 0.67559(11) 0.0231(4) Uani 1 1 d . . . O5 O 0.42689(14) 0.11176(8) 0.71334(14) 0.0324(5) Uani 1 1 d . . . O6 O 0.43964(15) 0.14962(8) 0.85646(13) 0.0330(5) Uani 1 1 d . . . O7 O 0.57302(13) 0.41354(7) 0.84880(12) 0.0276(4) Uani 1 1 d . . . O8 O 0.56880(13) 0.45206(7) 0.70668(12) 0.0275(4) Uani 1 1 d . . . N1 N 0.74057(16) 0.25574(9) 0.66366(14) 0.0276(5) Uani 1 1 d . . . N2 N 0.75206(16) 0.30878(9) 0.80440(15) 0.0276(5) Uani 1 1 d . . . C1 C 0.69321(18) 0.18724(10) 0.79880(17) 0.0246(5) Uani 1 1 d . . . C2 C 0.70797(19) 0.16893(11) 0.86916(17) 0.0277(6) Uani 1 1 d . . . C3 C 0.7798(2) 0.14642(11) 0.88236(18) 0.0320(7) Uani 1 1 d . . . H3A H 0.7896 0.1341 0.9299 0.038 Uiso 1 1 calc R . . C4 C 0.8379(2) 0.14118(11) 0.8292(2) 0.0322(7) Uani 1 1 d . . . C5 C 0.8239(2) 0.15981(11) 0.76036(18) 0.0298(6) Uani 1 1 d . . . H5A H 0.8633 0.1565 0.7233 0.036 Uiso 1 1 calc R . . C6 C 0.7525(2) 0.18349(11) 0.74440(17) 0.0279(6) Uani 1 1 d . . . C7 C 0.6465(2) 0.17329(13) 0.92857(18) 0.0341(7) Uani 1 1 d . . . H7A H 0.6662 0.1580 0.9733 0.051 Uiso 1 1 calc R . . H7B H 0.5970 0.1579 0.9128 0.051 Uiso 1 1 calc R . . H7C H 0.6362 0.2068 0.9384 0.051 Uiso 1 1 calc R . . C8 C 0.9146(2) 0.11419(13) 0.8438(2) 0.0420(9) Uani 1 1 d . . . H8A H 0.9291 0.1173 0.8956 0.063 Uiso 1 1 calc R . . H8B H 0.9574 0.1271 0.8131 0.063 Uiso 1 1 calc R . . H8C H 0.9067 0.0807 0.8319 0.063 Uiso 1 1 calc R . . C9 C 0.7391(2) 0.20267(11) 0.66889(17) 0.0288(6) Uani 1 1 d . . . H9A H 0.6868 0.1913 0.6510 0.035 Uiso 1 1 calc R . . H9B H 0.7806 0.1897 0.6359 0.035 Uiso 1 1 calc R . . C10 C 0.7271(2) 0.26808(13) 0.58554(19) 0.0375(8) Uani 1 1 d . . . H10A H 0.7716 0.2562 0.5559 0.056 Uiso 1 1 calc R . . H10B H 0.7236 0.3025 0.5805 0.056 Uiso 1 1 calc R . . H10C H 0.6773 0.2537 0.5687 0.056 Uiso 1 1 calc R . . C11 C 0.8167(2) 0.27742(12) 0.6877(2) 0.0326(7) Uani 1 1 d . . . H11A H 0.8233 0.3081 0.6624 0.039 Uiso 1 1 calc R . . H11B H 0.8613 0.2567 0.6722 0.039 Uiso 1 1 calc R . . C12 C 0.8228(2) 0.28565(12) 0.7710(2) 0.0346(7) Uani 1 1 d . . . H12A H 0.8312 0.2548 0.7953 0.041 Uiso 1 1 calc R . . H12B H 0.8703 0.3054 0.7809 0.041 Uiso 1 1 calc R . . C13 C 0.7497(2) 0.29707(14) 0.88319(19) 0.0379(8) Uani 1 1 d . . . H13A H 0.7968 0.3103 0.9075 0.057 Uiso 1 1 calc R . . H13B H 0.7492 0.2626 0.8893 0.057 Uiso 1 1 calc R . . H13C H 0.7014 0.3105 0.9052 0.057 Uiso 1 1 calc R . . C14 C 0.7531(2) 0.36193(11) 0.79789(19) 0.0317(7) Uani 1 1 d . . . H14A H 0.7057 0.3747 0.8234 0.038 Uiso 1 1 calc R . . H14B H 0.8010 0.3741 0.8236 0.038 Uiso 1 1 calc R . . C15 C 0.7537(2) 0.38038(10) 0.7208(2) 0.0309(7) Uani 1 1 d . . . C16 C 0.8219(2) 0.40125(12) 0.6923(2) 0.0372(8) Uani 1 1 d . . . H16A H 0.8681 0.4032 0.7223 0.045 Uiso 1 1 calc R . . C17 C 0.8252(2) 0.41929(13) 0.6218(2) 0.0423(9) Uani 1 1 d . . . C18 C 0.7576(2) 0.41622(12) 0.5792(2) 0.0373(8) Uani 1 1 d . . . H18A H 0.7591 0.4287 0.5308 0.045 Uiso 1 1 calc R . . C19 C 0.6868(2) 0.39555(11) 0.60396(18) 0.0287(6) Uani 1 1 d . . . C20 C 0.68484(18) 0.37694(10) 0.67630(17) 0.0257(6) Uani 1 1 d . . . C21 C 0.9009(3) 0.44116(18) 0.5926(3) 0.0658(14) Uani 1 1 d . . . H21A H 0.8878 0.4638 0.5538 0.099 Uiso 1 1 calc R . . H21B H 0.9355 0.4163 0.5728 0.099 Uiso 1 1 calc R . . H21C H 0.9287 0.4576 0.6324 0.099 Uiso 1 1 calc R . . C22 C 0.6147(2) 0.39314(13) 0.55667(18) 0.0334(7) Uani 1 1 d . . . H22A H 0.6233 0.4120 0.5123 0.050 Uiso 1 1 calc R . . H22B H 0.5686 0.4056 0.5836 0.050 Uiso 1 1 calc R . . H22C H 0.6045 0.3602 0.5430 0.050 Uiso 1 1 calc R . . C23 C 0.49150(16) 0.28164(10) 0.64034(16) 0.0217(5) Uani 1 1 d . . . C24 C 0.48608(19) 0.28209(10) 0.55879(16) 0.0243(6) Uani 1 1 d . . . C25 C 0.4496(2) 0.32006(11) 0.52314(17) 0.0300(6) Uani 1 1 d . . . H25A H 0.4265 0.3451 0.5508 0.036 Uiso 1 1 calc R . . C26 C 0.4472(2) 0.32107(14) 0.44676(19) 0.0392(8) Uani 1 1 d . . . H26A H 0.4214 0.3464 0.4221 0.047 Uiso 1 1 calc R . . C27 C 0.4825(3) 0.28500(15) 0.4071(2) 0.0441(10) Uani 1 1 d . . . H27A H 0.4827 0.2864 0.3551 0.053 Uiso 1 1 calc R . . C28 C 0.5177(3) 0.24694(16) 0.4423(2) 0.0429(9) Uani 1 1 d . . . H28A H 0.5404 0.2220 0.4144 0.052 Uiso 1 1 calc R . . C29 C 0.5199(2) 0.24518(13) 0.51826(18) 0.0324(7) Uani 1 1 d . . . H29A H 0.5441 0.2191 0.5425 0.039 Uiso 1 1 calc R . . C31 C 0.3739(2) 0.03656(13) 0.6928(3) 0.0661(15) Uani 1 1 d D . . C30 C 0.3959(4) 0.07877(18) 0.7467(3) 0.0365(10) Uani 0.694(4) 1 d PD A 1 C32 C 0.3822(4) 0.07532(19) 0.8208(3) 0.0436(12) Uani 0.694(4) 1 d PD A 1 H32A H 0.3571 0.0477 0.8396 0.052 Uiso 0.694(4) 1 calc PR A 1 C33 C 0.4041(3) 0.11116(16) 0.8690(3) 0.0343(10) Uani 0.694(4) 1 d PD A 1 C30A C 0.5624(7) 0.0769(4) 0.8279(7) 0.0365(10) Uani 0.306(4) 1 d PD . 2 C32A C 0.5030(7) 0.0736(4) 0.8812(8) 0.0436(12) Uani 0.306(4) 1 d PD B 2 H1A H 0.4986 0.0457 0.9099 0.052 Uiso 0.306(4) 1 calc PR A 2 C33A C 0.4499(7) 0.1111(4) 0.8925(7) 0.0343(10) Uani 0.306(4) 1 d PD B 2 C34 C 0.3855(2) 0.10421(11) 0.9519(2) 0.0518(11) Uani 1 1 d D . . C35 C 0.6116(2) 0.45159(12) 0.8594(2) 0.0469(10) Uani 1 1 d D C . C36 C 0.6387(2) 0.45808(11) 0.93818(18) 0.0440(9) Uani 1 1 d D . . C37 C 0.6357(3) 0.48515(14) 0.8083(2) 0.0497(10) Uani 1 1 d . . . H37A H 0.6689 0.5105 0.8239 0.060 Uiso 1 1 calc R C . C38 C 0.6131(3) 0.48296(13) 0.7354(2) 0.0455(10) Uani 1 1 d . C . C39 C 0.6340(2) 0.52347(11) 0.6821(2) 0.0517(12) Uani 1 1 d 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 Tb1 0.02030(9) 0.01865(9) 0.02465(9) 0.000 -0.00060(7) 0.000 Tb2 0.02021(9) 0.01776(8) 0.02050(8) 0.000 -0.00007(6) 0.000 Cd1 0.01911(9) 0.02000(9) 0.02676(9) 0.00070(7) -0.00008(7) 0.00050(7) F1 0.112(5) 0.187(7) 0.248(10) -0.098(7) 0.052(5) 0.036(5) F2 0.109(4) 0.065(3) 0.140(5) 0.007(3) -0.062(4) -0.015(3) F3 0.177(6) 0.077(3) 0.114(4) 0.016(3) 0.011(4) -0.012(4) F1A 0.112(5) 0.187(7) 0.248(10) -0.098(7) 0.052(5) 0.036(5) F2A 0.109(4) 0.065(3) 0.140(5) 0.007(3) -0.062(4) -0.015(3) F3A 0.177(6) 0.077(3) 0.114(4) 0.016(3) 0.011(4) -0.012(4) F4 0.077(4) 0.218(7) 0.078(3) 0.070(4) -0.011(3) -0.018(4) F5 0.132(5) 0.075(3) 0.059(3) 0.018(2) 0.041(3) 0.036(3) F6 0.178(8) 0.0454(17) 0.100(4) 0.0190(19) 0.086(5) -0.017(3) F4A 0.077(4) 0.218(7) 0.078(3) 0.070(4) -0.011(3) -0.018(4) F5A 0.132(5) 0.075(3) 0.059(3) 0.018(2) 0.041(3) 0.036(3) F6A 0.178(8) 0.0454(17) 0.100(4) 0.0190(19) 0.086(5) -0.017(3) F7 0.102(4) 0.210(6) 0.055(2) -0.048(3) 0.014(2) -0.029(4) F8 0.145(4) 0.053(2) 0.082(3) 0.0039(17) -0.075(3) -0.011(2) F9 0.150(4) 0.067(2) 0.059(2) -0.0019(15) -0.042(2) -0.063(3) F7A 0.102(4) 0.210(6) 0.055(2) -0.048(3) 0.014(2) -0.029(4) F8A 0.145(4) 0.053(2) 0.082(3) 0.0039(17) -0.075(3) -0.011(2) F9A 0.150(4) 0.067(2) 0.059(2) -0.0019(15) -0.042(2) -0.063(3) F10 0.110(3) 0.085(3) 0.093(3) 0.014(2) -0.021(3) -0.032(3) F11 0.067(2) 0.075(3) 0.127(4) 0.007(2) -0.001(2) 0.028(2) F12 0.119(3) 0.0351(14) 0.0604(19) 0.0008(12) 0.0442(19) 0.0043(17) F10A 0.110(3) 0.085(3) 0.093(3) 0.014(2) -0.021(3) -0.032(3) F11A 0.067(2) 0.075(3) 0.127(4) 0.007(2) -0.001(2) 0.028(2) F12A 0.119(3) 0.0351(14) 0.0604(19) 0.0008(12) 0.0442(19) 0.0043(17) O1 0.0214(10) 0.0241(10) 0.0298(10) 0.0028(8) -0.0036(8) 0.0005(8) O2 0.0232(10) 0.0222(9) 0.0278(10) -0.0010(7) 0.0037(8) -0.0007(8) O3 0.0224(10) 0.0223(9) 0.0261(9) 0.0010(7) -0.0009(8) 0.0016(8) O4 0.0253(11) 0.0215(9) 0.0224(9) -0.0003(7) -0.0002(8) -0.0009(8) O5 0.0288(12) 0.0261(11) 0.0424(13) -0.0039(9) -0.0027(10) -0.0031(9) O6 0.0391(13) 0.0233(10) 0.0367(12) 0.0053(9) 0.0062(10) 0.0004(9) O7 0.0327(12) 0.0224(10) 0.0276(10) -0.0021(8) -0.0040(9) -0.0017(9) O8 0.0312(12) 0.0217(10) 0.0296(10) 0.0003(8) 0.0024(9) -0.0019(8) N1 0.0279(13) 0.0242(12) 0.0306(12) 0.0018(9) 0.0019(10) 0.0002(10) N2 0.0234(13) 0.0267(12) 0.0328(13) -0.0034(10) -0.0048(10) -0.0003(10) C1 0.0231(14) 0.0196(12) 0.0311(14) 0.0006(10) -0.0049(11) 0.0016(10) C2 0.0257(15) 0.0257(14) 0.0316(14) 0.0017(11) -0.0023(12) 0.0020(12) C3 0.0339(17) 0.0280(15) 0.0342(15) 0.0010(11) -0.0102(13) 0.0056(13) C4 0.0282(16) 0.0247(14) 0.0438(18) -0.0016(12) -0.0097(14) 0.0040(12) C5 0.0290(16) 0.0254(14) 0.0351(16) -0.0004(11) -0.0004(12) 0.0017(12) C6 0.0300(16) 0.0215(13) 0.0323(15) 0.0017(10) -0.0087(12) -0.0009(11) C7 0.0357(18) 0.0403(18) 0.0265(14) 0.0030(12) -0.0026(13) 0.0025(15) C8 0.037(2) 0.0365(19) 0.052(2) -0.0031(16) -0.0082(17) 0.0098(15) C9 0.0295(16) 0.0255(14) 0.0313(14) 0.0009(11) 0.0074(12) 0.0011(12) C10 0.044(2) 0.0370(18) 0.0316(16) 0.0062(13) 0.0069(15) 0.0037(16) C11 0.0251(15) 0.0289(16) 0.0439(18) -0.0029(12) 0.0077(14) -0.0020(12) C12 0.0228(15) 0.0309(16) 0.0500(19) -0.0053(14) -0.0044(15) 0.0022(13) C13 0.040(2) 0.0430(19) 0.0310(16) 0.0014(14) -0.0078(14) -0.0003(16) C14 0.0318(17) 0.0247(14) 0.0387(17) -0.0062(12) -0.0067(13) 0.0034(13) C15 0.0377(19) 0.0140(12) 0.0411(17) -0.0004(11) 0.0072(15) 0.0004(12) C16 0.0253(16) 0.0303(17) 0.056(2) -0.0004(14) 0.0001(15) -0.0042(13) C17 0.039(2) 0.0301(17) 0.058(2) -0.0007(15) 0.0174(18) -0.0103(15) C18 0.042(2) 0.0250(15) 0.0449(19) 0.0022(13) 0.0190(16) 0.0007(14) C19 0.0294(16) 0.0213(13) 0.0354(15) -0.0011(11) 0.0059(13) 0.0013(12) C20 0.0235(14) 0.0194(12) 0.0341(15) 0.0018(10) 0.0066(12) -0.0005(11) C21 0.043(3) 0.061(3) 0.094(4) 0.010(3) 0.024(3) -0.021(2) C22 0.0379(19) 0.0359(17) 0.0263(14) 0.0021(12) 0.0034(13) 0.0003(14) C23 0.0218(14) 0.0222(12) 0.0211(11) 0.0013(9) -0.0019(9) -0.0038(10) C24 0.0279(15) 0.0243(13) 0.0208(11) 0.0004(10) -0.0014(10) -0.0055(11) C25 0.0315(17) 0.0309(15) 0.0276(14) 0.0049(11) -0.0045(12) -0.0054(13) C26 0.0378(19) 0.051(2) 0.0291(15) 0.0132(14) -0.0077(14) -0.0082(16) C27 0.045(2) 0.064(3) 0.0231(14) 0.0038(15) -0.0016(15) -0.0185(19) C28 0.047(2) 0.056(2) 0.0263(15) -0.0094(15) 0.0053(15) -0.0105(19) C29 0.0330(16) 0.0387(18) 0.0256(14) -0.0087(12) 0.0020(12) -0.0051(14) C31 0.056(3) 0.0246(19) 0.117(5) -0.002(2) -0.029(3) -0.0136(19) C30 0.036(3) 0.0207(19) 0.053(3) -0.0020(17) -0.003(2) -0.0044(18) C32 0.046(3) 0.027(2) 0.057(3) 0.009(2) 0.002(2) -0.007(2) C33 0.036(3) 0.0224(18) 0.045(3) 0.0080(17) 0.010(2) 0.002(2) C30A 0.036(3) 0.0207(19) 0.053(3) -0.0020(17) -0.003(2) -0.0044(18) C32A 0.046(3) 0.027(2) 0.057(3) 0.009(2) 0.002(2) -0.007(2) C33A 0.036(3) 0.0224(18) 0.045(3) 0.0080(17) 0.010(2) 0.002(2) C34 0.061(3) 0.042(2) 0.052(2) 0.0145(18) 0.019(2) 0.007(2) C35 0.062(3) 0.0319(18) 0.047(2) -0.0033(15) -0.0173(19) -0.0006(18) C36 0.053(2) 0.041(2) 0.0382(18) -0.0102(15) -0.0122(18) -0.0062(18) C37 0.058(3) 0.037(2) 0.055(2) -0.0016(17) -0.006(2) -0.0067(19) C38 0.069(3) 0.0233(16) 0.044(2) 0.0022(14) 0.011(2) 0.0098(18) C39 0.048(2) 0.0190(15) 0.088(3) 0.0060(17) 0.037(2) -0.0029(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 Tb1 O1 2.300(2) . ? Tb1 O1 2.300(2) 3_656 ? Tb1 O6 2.356(2) . ? Tb1 O6 2.356(2) 3_656 ? Tb1 O5 2.389(2) . ? Tb1 O5 2.389(2) 3_656 ? Tb1 O3 2.496(2) . ? Tb1 O3 2.496(2) 3_656 ? Tb1 Cd1 3.7243(3) . ? Tb1 Cd1 3.7244(3) 3_656 ? Tb2 O2 2.297(2) . ? Tb2 O2 2.297(2) 3_656 ? Tb2 O7 2.337(2) . ? Tb2 O7 2.337(2) 3_656 ? Tb2 O8 2.386(2) . ? Tb2 O8 2.386(2) 3_656 ? Tb2 O4 2.507(2) 3_656 ? Tb2 O4 2.507(2) . ? Tb2 Cd1 3.7063(3) 3_656 ? Tb2 Cd1 3.7063(3) . ? Cd1 O2 2.233(2) . ? Cd1 O1 2.235(2) . ? Cd1 N1 2.325(3) . ? Cd1 N2 2.326(3) . ? Cd1 O4 2.382(2) 3_656 ? Cd1 O3 2.399(2) . ? F1 C31 1.283(5) . ? F2 C31 1.279(5) . ? F3 C31 1.286(5) . ? F1A C31 1.282(4) . ? F1A C30A 1.733(13) 3_656 ? F2A C31 1.296(4) . ? F3A C31 1.326(4) . ? F4 C34 1.316(4) . ? F5 C34 1.305(4) . ? F6 C34 1.298(4) . ? F4A C34 1.289(5) . ? F5A C34 1.288(5) . ? F6A C34 1.295(5) . ? F7 C36 1.294(5) . ? F8 C36 1.321(5) . ? F9 C36 1.297(5) . ? F7A C36 1.343(4) . ? F8A C36 1.292(4) . ? F9A C36 1.289(3) . ? F10 C39 1.333(4) . ? F11 C39 1.305(4) . ? F12 C39 1.310(4) . ? F10A C39 1.288(5) . ? F11A C39 1.283(5) . ? F12A C39 1.279(5) . ? O1 C1 1.362(4) . ? O2 C20 1.358(4) . ? O3 C23 1.267(3) . ? O4 C23 1.268(3) . ? O4 Cd1 2.382(2) 3_656 ? O5 C30 1.229(6) . ? O5 C30A 1.253(11) 3_656 ? O6 C33 1.261(5) . ? O6 C33A 1.284(11) . ? O7 C35 1.270(4) . ? O8 C38 1.261(5) . ? N1 C11 1.483(4) . ? N1 C10 1.484(4) . ? N1 C9 1.504(4) . ? N2 C13 1.475(4) . ? N2 C12 1.485(4) . ? N2 C14 1.508(4) . ? C1 C2 1.406(4) . ? C1 C6 1.409(5) . ? C2 C3 1.384(4) . ? C2 C7 1.500(5) . ? C3 C4 1.382(5) . ? C3 H3A 0.9500 . ? C4 C5 1.382(5) . ? C4 C8 1.518(5) . ? C5 C6 1.402(5) . ? C5 H5A 0.9500 . ? C6 C9 1.497(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.540(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.500(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.389(5) . ? C15 C20 1.414(5) . ? C16 C17 1.385(6) . ? C16 H16A 0.9500 . ? C17 C18 1.377(6) . ? C17 C21 1.508(5) . ? C18 C19 1.397(5) . ? C18 H18A 0.9500 . ? C19 C20 1.421(4) . ? C19 C22 1.487(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.490(4) . ? C24 C25 1.396(4) . ? C24 C29 1.399(5) . ? C25 C26 1.394(5) . ? C25 H25A 0.9500 . ? C26 C27 1.383(6) . ? C26 H26A 0.9500 . ? C27 C28 1.385(6) . ? C27 H27A 0.9500 . ? C28 C29 1.387(5) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C31 C30 1.589(6) . ? C31 C30A 1.608(12) 3_656 ? C30 C32 1.376(7) . ? C32 C33 1.391(8) . ? C32 H32A 0.9500 . ? C33 C34 1.556(6) . ? C30A O5 1.253(11) 3_656 ? C30A C32A 1.393(14) . ? C30A C31 1.608(12) 3_656 ? C30A F1A 1.733(13) 3_656 ? C32A C33A 1.399(13) . ? C32A H1A 0.9500 . ? C33A C34 1.542(11) . ? C35 C37 1.390(6) . ? C35 C36 1.518(5) . ? C37 C38 1.384(6) . ? C37 H37A 0.9500 . ? C38 C39 1.542(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Tb1 O1 138.41(10) . 3_656 ? O1 Tb1 O6 106.78(8) . . ? O1 Tb1 O6 88.46(8) 3_656 . ? O1 Tb1 O6 88.46(8) . 3_656 ? O1 Tb1 O6 106.78(8) 3_656 3_656 ? O6 Tb1 O6 136.74(11) . 3_656 ? O1 Tb1 O5 145.42(8) . . ? O1 Tb1 O5 75.69(8) 3_656 . ? O6 Tb1 O5 73.22(8) . . ? O6 Tb1 O5 71.97(8) 3_656 . ? O1 Tb1 O5 75.69(8) . 3_656 ? O1 Tb1 O5 145.42(8) 3_656 3_656 ? O6 Tb1 O5 71.97(8) . 3_656 ? O6 Tb1 O5 73.22(8) 3_656 3_656 ? O5 Tb1 O5 71.52(12) . 3_656 ? O1 Tb1 O3 71.59(7) . . ? O1 Tb1 O3 76.04(7) 3_656 . ? O6 Tb1 O3 149.49(7) . . ? O6 Tb1 O3 73.55(7) 3_656 . ? O5 Tb1 O3 125.95(8) . . ? O5 Tb1 O3 133.33(8) 3_656 . ? O1 Tb1 O3 76.04(7) . 3_656 ? O1 Tb1 O3 71.58(7) 3_656 3_656 ? O6 Tb1 O3 73.55(7) . 3_656 ? O6 Tb1 O3 149.49(7) 3_656 3_656 ? O5 Tb1 O3 133.33(8) . 3_656 ? O5 Tb1 O3 125.95(8) 3_656 3_656 ? O3 Tb1 O3 76.64(9) . 3_656 ? O1 Tb1 Cd1 34.23(5) . . ? O1 Tb1 Cd1 106.05(5) 3_656 . ? O6 Tb1 Cd1 126.31(6) . . ? O6 Tb1 Cd1 88.80(6) 3_656 . ? O5 Tb1 Cd1 160.08(6) . . ? O5 Tb1 Cd1 108.51(6) 3_656 . ? O3 Tb1 Cd1 39.50(5) . . ? O3 Tb1 Cd1 63.62(5) 3_656 . ? O1 Tb1 Cd1 106.05(5) . 3_656 ? O1 Tb1 Cd1 34.23(5) 3_656 3_656 ? O6 Tb1 Cd1 88.80(6) . 3_656 ? O6 Tb1 Cd1 126.32(6) 3_656 3_656 ? O5 Tb1 Cd1 108.51(6) . 3_656 ? O5 Tb1 Cd1 160.08(6) 3_656 3_656 ? O3 Tb1 Cd1 63.62(5) . 3_656 ? O3 Tb1 Cd1 39.50(5) 3_656 3_656 ? Cd1 Tb1 Cd1 78.403(8) . 3_656 ? O2 Tb2 O2 139.95(10) . 3_656 ? O2 Tb2 O7 88.51(8) . . ? O2 Tb2 O7 105.88(8) 3_656 . ? O2 Tb2 O7 105.88(8) . 3_656 ? O2 Tb2 O7 88.51(8) 3_656 3_656 ? O7 Tb2 O7 137.60(10) . 3_656 ? O2 Tb2 O8 74.66(7) . . ? O2 Tb2 O8 145.03(7) 3_656 . ? O7 Tb2 O8 73.09(8) . . ? O7 Tb2 O8 72.83(8) 3_656 . ? O2 Tb2 O8 145.03(7) . 3_656 ? O2 Tb2 O8 74.67(7) 3_656 3_656 ? O7 Tb2 O8 72.83(8) . 3_656 ? O7 Tb2 O8 73.09(7) 3_656 3_656 ? O8 Tb2 O8 71.73(10) . 3_656 ? O2 Tb2 O4 71.72(7) . 3_656 ? O2 Tb2 O4 77.00(7) 3_656 3_656 ? O7 Tb2 O4 73.22(7) . 3_656 ? O7 Tb2 O4 149.04(7) 3_656 3_656 ? O8 Tb2 O4 132.32(7) . 3_656 ? O8 Tb2 O4 126.99(7) 3_656 3_656 ? O2 Tb2 O4 77.00(7) . . ? O2 Tb2 O4 71.72(7) 3_656 . ? O7 Tb2 O4 149.04(7) . . ? O7 Tb2 O4 73.23(7) 3_656 . ? O8 Tb2 O4 126.99(7) . . ? O8 Tb2 O4 132.32(7) 3_656 . ? O4 Tb2 O4 76.26(9) 3_656 . ? O2 Tb2 Cd1 107.14(5) . 3_656 ? O2 Tb2 Cd1 34.54(5) 3_656 3_656 ? O7 Tb2 Cd1 125.29(5) . 3_656 ? O7 Tb2 Cd1 88.91(5) 3_656 3_656 ? O8 Tb2 Cd1 161.20(5) . 3_656 ? O8 Tb2 Cd1 107.78(5) 3_656 3_656 ? O4 Tb2 Cd1 63.70(5) 3_656 3_656 ? O4 Tb2 Cd1 39.46(5) . 3_656 ? O2 Tb2 Cd1 34.54(5) . . ? O2 Tb2 Cd1 107.14(5) 3_656 . ? O7 Tb2 Cd1 88.91(5) . . ? O7 Tb2 Cd1 125.29(5) 3_656 . ? O8 Tb2 Cd1 107.78(5) . . ? O8 Tb2 Cd1 161.20(5) 3_656 . ? O4 Tb2 Cd1 39.46(5) 3_656 . ? O4 Tb2 Cd1 63.70(5) . . ? Cd1 Tb2 Cd1 78.857(8) 3_656 . ? O2 Cd1 O1 162.55(8) . . ? O2 Cd1 N1 103.13(8) . . ? O1 Cd1 N1 90.58(9) . . ? O2 Cd1 N2 90.10(9) . . ? O1 Cd1 N2 103.11(9) . . ? N1 Cd1 N2 79.67(9) . . ? O2 Cd1 O4 75.23(7) . 3_656 ? O1 Cd1 O4 91.84(7) . 3_656 ? N1 Cd1 O4 175.58(8) . 3_656 ? N2 Cd1 O4 96.17(8) . 3_656 ? O2 Cd1 O3 93.24(7) . . ? O1 Cd1 O3 74.54(7) . . ? N1 Cd1 O3 95.30(8) . . ? N2 Cd1 O3 174.50(8) . . ? O4 Cd1 O3 88.91(7) 3_656 . ? O2 Cd1 Tb2 35.68(5) . . ? O1 Cd1 Tb2 128.08(6) . . ? N1 Cd1 Tb2 137.40(6) . . ? N2 Cd1 Tb2 104.01(6) . . ? O4 Cd1 Tb2 41.98(5) 3_656 . ? O3 Cd1 Tb2 81.18(5) . . ? O2 Cd1 Tb1 128.81(5) . . ? O1 Cd1 Tb1 35.37(5) . . ? N1 Cd1 Tb1 103.41(6) . . ? N2 Cd1 Tb1 137.38(7) . . ? O4 Cd1 Tb1 80.65(5) 3_656 . ? O3 Cd1 Tb1 41.43(5) . . ? Tb2 Cd1 Tb1 101.371(7) . . ? C31 F1A C30A 62.4(5) . 3_656 ? C1 O1 Cd1 112.09(17) . . ? C1 O1 Tb1 131.85(18) . . ? Cd1 O1 Tb1 110.40(9) . . ? C20 O2 Cd1 112.03(17) . . ? C20 O2 Tb2 133.85(18) . . ? Cd1 O2 Tb2 109.78(8) . . ? C23 O3 Cd1 111.50(17) . . ? C23 O3 Tb1 134.01(18) . . ? Cd1 O3 Tb1 99.07(7) . . ? C23 O4 Cd1 111.94(17) . 3_656 ? C23 O4 Tb2 134.41(18) . . ? Cd1 O4 Tb2 98.56(7) 3_656 . ? C30 O5 C30A 76.2(6) . 3_656 ? C30 O5 Tb1 134.0(3) . . ? C30A O5 Tb1 137.1(5) 3_656 . ? C33 O6 C33A 40.4(6) . . ? C33 O6 Tb1 132.1(3) . . ? C33A O6 Tb1 132.6(5) . . ? C35 O7 Tb2 133.7(2) . . ? C38 O8 Tb2 135.2(2) . . ? C11 N1 C10 108.5(3) . . ? C11 N1 C9 114.1(3) . . ? C10 N1 C9 107.0(3) . . ? C11 N1 Cd1 108.08(19) . . ? C10 N1 Cd1 113.4(2) . . ? C9 N1 Cd1 105.85(18) . . ? C13 N2 C12 108.8(3) . . ? C13 N2 C14 107.5(3) . . ? C12 N2 C14 113.4(3) . . ? C13 N2 Cd1 112.9(2) . . ? C12 N2 Cd1 107.4(2) . . ? C14 N2 Cd1 106.87(18) . . ? O1 C1 C2 119.7(3) . . ? O1 C1 C6 120.9(3) . . ? C2 C1 C6 119.4(3) . . ? C3 C2 C1 118.8(3) . . ? C3 C2 C7 120.6(3) . . ? C1 C2 C7 120.6(3) . . ? C4 C3 C2 122.7(3) . . ? C4 C3 H3A 118.6 . . ? C2 C3 H3A 118.6 . . ? C3 C4 C5 118.5(3) . . ? C3 C4 C8 121.9(3) . . ? C5 C4 C8 119.6(3) . . ? C4 C5 C6 121.0(3) . . ? C4 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? C5 C6 C1 119.5(3) . . ? C5 C6 C9 119.5(3) . . ? C1 C6 C9 120.9(3) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 N1 114.7(3) . . ? C6 C9 H9A 108.6 . . ? N1 C9 H9A 108.6 . . ? C6 C9 H9B 108.6 . . ? N1 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 114.2(3) . . ? N1 C11 H11A 108.7 . . ? C12 C11 H11A 108.7 . . ? N1 C11 H11B 108.7 . . ? C12 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? N2 C12 C11 114.8(3) . . ? N2 C12 H12A 108.6 . . ? C11 C12 H12A 108.6 . . ? N2 C12 H12B 108.6 . . ? C11 C12 H12B 108.6 . . ? H12A C12 H12B 107.6 . . ? N2 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 N2 114.9(3) . . ? C15 C14 H14A 108.6 . . ? N2 C14 H14A 108.6 . . ? C15 C14 H14B 108.6 . . ? N2 C14 H14B 108.6 . . ? H14A C14 H14B 107.5 . . ? C16 C15 C20 119.2(3) . . ? C16 C15 C14 120.2(3) . . ? C20 C15 C14 120.6(3) . . ? C17 C16 C15 122.5(4) . . ? C17 C16 H16A 118.8 . . ? C15 C16 H16A 118.8 . . ? C18 C17 C16 117.9(3) . . ? C18 C17 C21 121.3(4) . . ? C16 C17 C21 120.8(4) . . ? C17 C18 C19 122.9(3) . . ? C17 C18 H18A 118.6 . . ? C19 C18 H18A 118.6 . . ? C18 C19 C20 118.4(3) . . ? C18 C19 C22 121.5(3) . . ? C20 C19 C22 120.2(3) . . ? O2 C20 C15 121.2(3) . . ? O2 C20 C19 119.5(3) . . ? C15 C20 C19 119.2(3) . . ? C17 C21 H21A 109.5 . . ? C17 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C17 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O3 C23 O4 123.5(3) . . ? O3 C23 C24 118.4(3) . . ? O4 C23 C24 118.1(3) . . ? C25 C24 C29 120.3(3) . . ? C25 C24 C23 119.9(3) . . ? C29 C24 C23 119.8(3) . . ? C26 C25 C24 119.6(3) . . ? C26 C25 H25A 120.2 . . ? C24 C25 H25A 120.2 . . ? C27 C26 C25 119.6(3) . . ? C27 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? C26 C27 C28 120.9(3) . . ? C26 C27 H27A 119.6 . . ? C28 C27 H27A 119.6 . . ? C27 C28 C29 120.1(4) . . ? C27 C28 H28A 119.9 . . ? C29 C28 H28A 119.9 . . ? C28 C29 C24 119.4(4) . . ? C28 C29 H29A 120.3 . . ? C24 C29 H29A 120.3 . . ? F2 C31 F1A 152.4(10) . . ? F2 C31 F1 111.0(6) . . ? F1A C31 F1 50.5(10) . . ? F2 C31 F3 110.7(6) . . ? F1A C31 F3 67.1(11) . . ? F1 C31 F3 110.2(6) . . ? F2 C31 F2A 63.9(10) . . ? F1A C31 F2A 111.3(4) . . ? F1 C31 F2A 133.4(15) . . ? F3 C31 F2A 47.2(11) . . ? F2 C31 F3A 54.5(10) . . ? F1A C31 F3A 105.3(4) . . ? F1 C31 F3A 56.8(10) . . ? F3 C31 F3A 132.6(13) . . ? F2A C31 F3A 105.1(4) . . ? F2 C31 C30 89.1(10) . . ? F1A C31 C30 116.3(5) . . ? F1 C31 C30 114.1(15) . . ? F3 C31 C30 119.8(12) . . ? F2A C31 C30 112.1(4) . . ? F3A C31 C30 105.7(4) . . ? F2 C31 C30A 133.9(11) . 3_656 ? F1A C31 C30A 72.7(5) . 3_656 ? F1 C31 C30A 111.4(13) . 3_656 ? F3 C31 C30A 69.9(13) . 3_656 ? F2A C31 C30A 98.0(5) . 3_656 ? F3A C31 C30A 155.7(6) . 3_656 ? C30 C31 C30A 57.2(5) . 3_656 ? O5 C30 C32 127.7(5) . . ? O5 C30 C31 111.3(4) . . ? C32 C30 C31 121.1(5) . . ? C30 C32 C33 121.7(5) . . ? C30 C32 H32A 119.1 . . ? C33 C32 H32A 119.1 . . ? O6 C33 C32 129.7(5) . . ? O6 C33 C34 112.3(4) . . ? C32 C33 C34 118.0(4) . . ? O5 C30A C32A 125.0(10) 3_656 . ? O5 C30A C31 108.7(8) 3_656 3_656 ? C32A C30A C31 126.2(9) . 3_656 ? O5 C30A F1A 147.7(9) 3_656 3_656 ? C32A C30A F1A 83.4(8) . 3_656 ? C31 C30A F1A 44.9(3) 3_656 3_656 ? C30A C32A C33A 120.4(11) . . ? C30A C32A H1A 119.8 . . ? C33A C32A H1A 119.8 . . ? O6 C33A C32A 130.7(10) . . ? O6 C33A C34 111.8(7) . . ? C32A C33A C34 117.0(9) . . ? F5A C34 F4A 110.1(5) . . ? F5A C34 F6A 108.8(5) . . ? F4A C34 F6A 108.9(5) . . ? F5A C34 F6 120.5(7) . . ? F4A C34 F6 79.1(6) . . ? F6A C34 F6 29.8(7) . . ? F5A C34 F5 54.8(5) . . ? F4A C34 F5 55.3(6) . . ? F6A C34 F5 126.7(9) . . ? F6 C34 F5 108.4(4) . . ? F5A C34 F4 50.8(5) . . ? F4A C34 F4 160.4(6) . . ? F6A C34 F4 78.1(6) . . ? F6 C34 F4 106.2(4) . . ? F5 C34 F4 105.6(4) . . ? F5A C34 C33A 106.4(7) . . ? F4A C34 C33A 114.4(8) . . ? F6A C34 C33A 108.1(9) . . ? F6 C34 C33A 123.1(6) . . ? F5 C34 C33A 125.0(5) . . ? F4 C34 C33A 79.0(6) . . ? F5A C34 C33 122.8(5) . . ? F4A C34 C33 81.6(6) . . ? F6A C34 C33 120.0(8) . . ? F6 C34 C33 116.7(5) . . ? F5 C34 C33 108.1(4) . . ? F4 C34 C33 111.3(4) . . ? C33A C34 C33 32.9(5) . . ? O7 C35 C37 128.6(4) . . ? O7 C35 C36 113.5(3) . . ? C37 C35 C36 117.7(3) . . ? F9A C36 F8A 111.2(3) . . ? F9A C36 F7 129.4(6) . . ? F8A C36 F7 57.5(9) . . ? F9A C36 F9 39.2(8) . . ? F8A C36 F9 133.4(5) . . ? F7 C36 F9 108.4(5) . . ? F9A C36 F8 68.9(8) . . ? F8A C36 F8 51.2(8) . . ? F7 C36 F8 106.3(4) . . ? F9 C36 F8 106.5(4) . . ? F9A C36 F7A 103.8(3) . . ? F8A C36 F7A 102.7(3) . . ? F7 C36 F7A 47.0(9) . . ? F9 C36 F7A 67.9(9) . . ? F8 C36 F7A 140.5(6) . . ? F9A C36 C35 115.9(3) . . ? F8A C36 C35 113.2(3) . . ? F7 C36 C35 113.0(4) . . ? F9 C36 C35 113.0(4) . . ? F8 C36 C35 109.2(4) . . ? F7A C36 C35 108.6(3) . . ? C38 C37 C35 122.3(4) . . ? C38 C37 H37A 118.9 . . ? C35 C37 H37A 118.9 . . ? O8 C38 C37 126.2(4) . . ? O8 C38 C39 112.8(4) . . ? C37 C38 C39 120.6(4) . . ? F12A C39 F11A 111.0(6) . . ? F12A C39 F10A 110.3(6) . . ? F11A C39 F10A 110.0(6) . . ? F12A C39 F11 41.9(15) . . ? F11A C39 F11 135.2(14) . . ? F10A C39 F11 69.4(15) . . ? F12A C39 F12 132.5(12) . . ? F11A C39 F12 60.9(17) . . ? F10A C39 F12 49.4(17) . . ? F11 C39 F12 107.6(3) . . ? F12A C39 F10 65.5(15) . . ? F11A C39 F10 49.3(16) . . ? F10A C39 F10 144.4(16) . . ? F11 C39 F10 103.9(3) . . ? F12 C39 F10 105.3(3) . . ? F12A C39 C38 112.9(12) . . ? F11A C39 C38 107.5(15) . . ? F10A C39 C38 105.0(15) . . ? F11 C39 C38 116.0(3) . . ? F12 C39 C38 114.0(3) . . ? F10 C39 C38 109.0(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.373 _refine_diff_density_min -1.635 _refine_diff_density_rms 0.174 # 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 0.358 0.750 83 12 ' ' 2 0.000 0.642 0.250 83 12 ' ' 3 0.500 0.142 0.250 83 12 ' ' 4 0.500 0.858 0.750 83 12 ' ' _platon_squeeze_details ; ; #================================END