# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Zn2Gd _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H66 Cl7 Gd N12 O13 P2 S2 Zn2' _chemical_formula_weight 1789.42 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.922(5) _cell_length_b 16.340(5) _cell_length_c 19.005(5) _cell_angle_alpha 110.093(5) _cell_angle_beta 91.639(5) _cell_angle_gamma 90.033(5) _cell_volume 3475(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2260 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 22.93 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.095 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.710 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1802 _exptl_absorpt_coefficient_mu 2.072 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.572668 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19138 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.1000 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 25.50 _reflns_number_total 12731 _reflns_number_gt 8128 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+1.3854P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12699 _refine_ls_number_parameters 813 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.1014 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1661 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.010 _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 Gd1 Gd 0.76506(3) 0.25465(2) 0.25608(2) 0.01792(12) Uani 1 1 d . . . Zn1 Zn 0.73040(7) 0.08965(5) 0.31875(4) 0.0154(2) Uani 1 1 d . . . Zn2 Zn 0.79489(7) 0.41296(5) 0.18535(4) 0.0157(2) Uani 1 1 d . . . P1 P 0.69254(16) -0.07467(13) 0.38245(11) 0.0166(4) Uani 1 1 d . . . P2 P 0.82442(17) 0.57037(13) 0.11341(11) 0.0190(4) Uani 1 1 d . . . S1 S 0.66937(17) -0.16842(13) 0.42026(11) 0.0233(5) Uani 1 1 d . . . S2 S 0.84195(18) 0.66183(14) 0.07241(12) 0.0292(5) Uani 1 1 d . . . Cl1 Cl 0.7972(2) 0.0578(2) 0.70119(13) 0.0550(7) Uani 1 1 d . . . Cl2 Cl 0.9245(2) 0.13697(17) 0.84068(13) 0.0463(6) Uani 1 1 d . . . Cl3 Cl 0.71416(19) 0.04748(16) 0.83890(14) 0.0437(6) Uani 1 1 d . . . Cl4 Cl 0.3930(2) 0.7094(2) 0.37641(13) 0.0539(7) Uani 1 1 d . . . Cl5 Cl 0.2454(2) 0.55704(17) 0.32144(14) 0.0526(7) Uani 1 1 d . . . Cl6 Cl 0.15271(19) 0.72853(16) 0.38821(12) 0.0402(6) Uani 1 1 d . . . Cl7 Cl 0.32882(18) 0.69440(14) 0.17455(11) 0.0301(5) Uani 1 1 d . . . O1 O 0.7698(4) 0.0963(3) 0.2142(3) 0.0173(11) Uani 1 1 d U . . O2 O 0.8286(4) 0.1500(3) 0.1060(3) 0.0226(12) Uani 1 1 d . . . O3 O 0.8422(4) 0.1951(3) 0.3481(3) 0.0192(12) Uani 1 1 d . . . O4 O 0.9406(4) 0.3435(3) 0.3630(3) 0.0218(12) Uani 1 1 d . . . O5 O 0.6274(4) 0.1904(3) 0.3122(3) 0.0169(11) Uani 1 1 d . . . O6 O 0.5398(4) 0.3187(3) 0.2766(3) 0.0189(12) Uani 1 1 d . . . O7 O 0.6909(4) 0.2991(3) 0.1563(3) 0.0191(12) Uani 1 1 d . . . O8 O 0.5826(4) 0.1572(3) 0.1548(3) 0.0204(12) Uani 1 1 d . . . O9 O 0.7519(4) 0.4095(3) 0.2891(3) 0.0182(12) Uani 1 1 d . . . O10 O 0.7102(4) 0.3564(3) 0.4001(3) 0.0229(12) Uani 1 1 d . . . O11 O 0.9059(4) 0.3206(3) 0.2042(3) 0.0175(11) Uani 1 1 d . . . O12 O 0.9887(4) 0.1857(3) 0.2306(3) 0.0191(8) Uani 1 1 d . . . O1S O 0.4126(9) 0.4651(5) 0.0771(5) 0.092(3) Uani 1 1 d D . . H1S H 0.4131 0.4117 0.0634 0.138 Uiso 1 1 calc R . . N1 N 0.6486(5) -0.0989(4) 0.2933(3) 0.0230(15) Uani 1 1 d D . . N2 N 0.6979(5) -0.0441(4) 0.2562(3) 0.0212(15) Uani 1 1 d D . . N3 N 0.8287(5) -0.0479(4) 0.3838(3) 0.0219(15) Uani 1 1 d . . . N4 N 0.8479(5) 0.0394(4) 0.3819(4) 0.0249(16) Uani 1 1 d . . . N5 N 0.6285(5) 0.0148(4) 0.4320(3) 0.0219(15) Uani 1 1 d D . . N6 N 0.6071(5) 0.0770(4) 0.3924(3) 0.0197(14) Uani 1 1 d D . . N7 N 0.7209(6) 0.5882(4) 0.1734(3) 0.0259(16) Uani 1 1 d . . . N8 N 0.7297(5) 0.5451(4) 0.2268(3) 0.0200(14) Uani 1 1 d . . . N9 N 0.7926(5) 0.4730(4) 0.0491(3) 0.0199(14) Uani 1 1 d U . . N10 N 0.7428(5) 0.4103(4) 0.0762(3) 0.0197(14) Uani 1 1 d . . . N11 N 0.9414(5) 0.5532(4) 0.1565(3) 0.0224(15) Uani 1 1 d . . . N12 N 0.9479(5) 0.4698(4) 0.1665(3) 0.0188(8) Uani 1 1 d . . . C1 C 0.5290(6) -0.1226(5) 0.2715(4) 0.0241(18) Uani 1 1 d . . . H1A H 0.4848 -0.0707 0.2848 0.036 Uiso 1 1 calc R . . H1B H 0.5025 -0.1599 0.2972 0.036 Uiso 1 1 calc R . . H1C H 0.5223 -0.1526 0.2183 0.036 Uiso 1 1 calc R . . C2 C 0.7316(6) -0.0888(5) 0.1902(4) 0.0194(17) Uani 1 1 d . . . H2 H 0.7248 -0.1492 0.1754 0.023 Uiso 1 1 calc R . . C3 C 0.7785(6) -0.0540(5) 0.1377(4) 0.0187(17) Uani 1 1 d U . . C4 C 0.8089(6) -0.1155(5) 0.0667(4) 0.0217(18) Uani 1 1 d . . . H4 H 0.8043 -0.1749 0.0586 0.026 Uiso 1 1 calc R . . C5 C 0.8443(6) -0.0882(5) 0.0114(4) 0.0250(19) Uani 1 1 d . . . H5 H 0.8632 -0.1288 -0.0344 0.030 Uiso 1 1 calc R . . C6 C 0.8526(6) 0.0006(5) 0.0227(4) 0.0222(18) Uani 1 1 d . . . H6 H 0.8772 0.0187 -0.0156 0.027 Uiso 1 1 calc R . . C7 C 0.8250(6) 0.0612(5) 0.0896(4) 0.0197(17) Uani 1 1 d . . . C8 C 0.7910(6) 0.0364(5) 0.1506(4) 0.0163(16) Uani 1 1 d . . . C9 C 0.8588(6) 0.1786(5) 0.0446(4) 0.0223(18) Uani 1 1 d . . . H9A H 0.9325 0.1582 0.0286 0.034 Uiso 1 1 calc R . . H9B H 0.8582 0.2411 0.0611 0.034 Uiso 1 1 calc R . . H9C H 0.8057 0.1553 0.0036 0.034 Uiso 1 1 calc R . . C10 C 0.9071(7) -0.1131(5) 0.3394(5) 0.028(2) Uani 1 1 d . . . H10A H 0.9099 -0.1101 0.2900 0.042 Uiso 1 1 calc R . . H10B H 0.8821 -0.1701 0.3363 0.042 Uiso 1 1 calc R . . H10C H 0.9805 -0.1017 0.3631 0.042 Uiso 1 1 calc R . . C11 C 0.9264(6) 0.0808(5) 0.4269(4) 0.0205(17) Uani 1 1 d U . . H11 H 0.9601 0.0520 0.4564 0.025 Uiso 1 1 calc R . . C12 C 0.9693(6) 0.1669(5) 0.4377(4) 0.0188(8) Uani 1 1 d . . . C13 C 1.0569(6) 0.2000(5) 0.4918(4) 0.0188(8) Uani 1 1 d . . . H13 H 1.0846 0.1658 0.5185 0.023 Uiso 1 1 calc R . . C14 C 1.1010(6) 0.2801(5) 0.5054(4) 0.0221(10) Uani 1 1 d . . . H14 H 1.1578 0.3009 0.5418 0.027 Uiso 1 1 calc R . . C15 C 1.0618(6) 0.3322(5) 0.4651(4) 0.0221(10) Uani 1 1 d . . . H15 H 1.0912 0.3880 0.4756 0.027 Uiso 1 1 calc R . . C16 C 0.9809(6) 0.3013(5) 0.4106(4) 0.0221(10) Uani 1 1 d . . . C17 C 0.9273(6) 0.2193(5) 0.3973(4) 0.0188(8) Uani 1 1 d . . . C18 C 0.9920(7) 0.4244(5) 0.3707(4) 0.029(2) Uani 1 1 d . . . H18A H 0.9804 0.4650 0.4202 0.043 Uiso 1 1 calc R . . H18B H 0.9594 0.4468 0.3343 0.043 Uiso 1 1 calc R . . H18C H 1.0710 0.4164 0.3629 0.043 Uiso 1 1 calc R . . C19 C 0.6530(7) 0.0587(5) 0.5127(4) 0.0258(19) Uani 1 1 d . . . H19A H 0.7069 0.1047 0.5196 0.039 Uiso 1 1 calc R . . H19B H 0.6829 0.0174 0.5337 0.039 Uiso 1 1 calc R . . H19C H 0.5852 0.0827 0.5372 0.039 Uiso 1 1 calc R . . C20 C 0.5053(7) 0.1065(5) 0.4005(4) 0.0227(18) Uani 1 1 d . . . H20 H 0.4581 0.0853 0.4287 0.027 Uiso 1 1 calc R . . C21 C 0.4593(7) 0.1681(5) 0.3704(4) 0.0216(18) Uani 1 1 d . . . C22 C 0.3447(6) 0.1886(5) 0.3810(4) 0.0192(17) Uani 1 1 d . . . H22 H 0.3021 0.1598 0.4056 0.023 Uiso 1 1 calc R . . C23 C 0.2946(6) 0.2486(5) 0.3568(4) 0.0206(18) Uani 1 1 d . . . H23 H 0.2182 0.2588 0.3631 0.025 Uiso 1 1 calc R . . C24 C 0.3575(6) 0.2950(5) 0.3224(4) 0.0182(17) Uani 1 1 d . . . H24 H 0.3240 0.3387 0.3083 0.022 Uiso 1 1 calc R . . C25 C 0.4712(6) 0.2764(5) 0.3088(4) 0.0185(17) Uani 1 1 d . . . C26 C 0.5234(6) 0.2111(5) 0.3303(4) 0.0165(16) Uani 1 1 d U . . C27 C 0.4903(6) 0.3867(5) 0.2545(4) 0.0237(18) Uani 1 1 d . . . H27A H 0.4284 0.3632 0.2200 0.036 Uiso 1 1 calc R . . H27B H 0.5454 0.4104 0.2308 0.036 Uiso 1 1 calc R . . H27C H 0.4641 0.4319 0.2980 0.036 Uiso 1 1 calc R . . C28 C 0.6300(7) 0.6500(5) 0.1787(5) 0.033(2) Uani 1 1 d . . . H28A H 0.5613 0.6260 0.1888 0.050 Uiso 1 1 calc R . . H28B H 0.6216 0.6606 0.1322 0.050 Uiso 1 1 calc R . . H28C H 0.6474 0.7038 0.2185 0.050 Uiso 1 1 calc R . . C29 C 0.6861(7) 0.5853(5) 0.2912(4) 0.0253(19) Uani 1 1 d . . . H29 H 0.6567 0.6402 0.2985 0.030 Uiso 1 1 calc R . . C30 C 0.6791(6) 0.5522(5) 0.3531(4) 0.0183(17) Uani 1 1 d U . . C31 C 0.6350(6) 0.6092(5) 0.4193(4) 0.0243(18) Uani 1 1 d . . . H31 H 0.6162 0.6655 0.4221 0.029 Uiso 1 1 calc R . . C32 C 0.6186(6) 0.5838(5) 0.4808(4) 0.0248(19) Uani 1 1 d . . . H32 H 0.5894 0.6226 0.5244 0.030 Uiso 1 1 calc R . . C33 C 0.6461(6) 0.5001(5) 0.4768(4) 0.0216(18) Uani 1 1 d . . . H33 H 0.6362 0.4824 0.5178 0.026 Uiso 1 1 calc R . . C34 C 0.6879(6) 0.4438(5) 0.4122(4) 0.0195(17) Uani 1 1 d . . . C35 C 0.7092(6) 0.4680(5) 0.3490(4) 0.0174(17) Uani 1 1 d . . . C36 C 0.6941(6) 0.3287(5) 0.4634(4) 0.0206(17) Uani 1 1 d . . . H36A H 0.7460 0.3594 0.5033 0.031 Uiso 1 1 calc R . . H36B H 0.7068 0.2672 0.4489 0.031 Uiso 1 1 calc R . . H36C H 0.6187 0.3411 0.4801 0.031 Uiso 1 1 calc R . . C37 C 0.8692(7) 0.4351(5) -0.0138(4) 0.0267(19) Uani 1 1 d . . . H37A H 0.9253 0.4013 0.0006 0.040 Uiso 1 1 calc R . . H37B H 0.9047 0.4812 -0.0258 0.040 Uiso 1 1 calc R . . H37C H 0.8270 0.3983 -0.0569 0.040 Uiso 1 1 calc R . . C38 C 0.6731(6) 0.3607(5) 0.0280(4) 0.0216(9) Uani 1 1 d . . . H38 H 0.6602 0.3731 -0.0157 0.026 Uiso 1 1 calc R . . C39 C 0.6116(6) 0.2867(5) 0.0347(4) 0.0216(9) Uani 1 1 d . . . C40 C 0.5418(6) 0.2409(5) -0.0266(4) 0.0216(9) Uani 1 1 d . . . H40 H 0.5363 0.2592 -0.0678 0.026 Uiso 1 1 calc R . . C41 C 0.4818(6) 0.1698(5) -0.0267(4) 0.0216(9) Uani 1 1 d . . . H41 H 0.4338 0.1407 -0.0670 0.026 Uiso 1 1 calc R . . C42 C 0.4933(7) 0.1410(5) 0.0349(4) 0.0240(18) Uani 1 1 d . . . H42 H 0.4530 0.0924 0.0351 0.029 Uiso 1 1 calc R . . C43 C 0.5627(6) 0.1836(5) 0.0940(4) 0.0213(18) Uani 1 1 d . . . C44 C 0.6234(6) 0.2587(5) 0.0972(4) 0.0164(16) Uani 1 1 d . . . C45 C 0.5208(7) 0.0824(5) 0.1545(4) 0.0243(19) Uani 1 1 d . . . H45A H 0.4421 0.0950 0.1566 0.036 Uiso 1 1 calc R . . H45B H 0.5436 0.0673 0.1974 0.036 Uiso 1 1 calc R . . H45C H 0.5351 0.0345 0.1096 0.036 Uiso 1 1 calc R . . C46 C 0.9921(7) 0.6260(5) 0.2191(5) 0.035(2) Uani 1 1 d . . . H46A H 0.9664 0.6236 0.2658 0.053 Uiso 1 1 calc R . . H46B H 0.9705 0.6804 0.2141 0.053 Uiso 1 1 calc R . . H46C H 1.0724 0.6214 0.2182 0.053 Uiso 1 1 calc R . . C47 C 1.0466(6) 0.4359(5) 0.1542(4) 0.0226(18) Uani 1 1 d . . . H47 H 1.1004 0.4670 0.1389 0.027 Uiso 1 1 calc R . . C48 C 1.0813(6) 0.3553(5) 0.1618(4) 0.0174(17) Uani 1 1 d . . . C49 C 1.1934(6) 0.3297(5) 0.1429(4) 0.0221(18) Uani 1 1 d . . . H49 H 1.2384 0.3638 0.1244 0.027 Uiso 1 1 calc R . . C50 C 1.2363(6) 0.2566(5) 0.1513(4) 0.0239(18) Uani 1 1 d . . . H50 H 1.3091 0.2399 0.1372 0.029 Uiso 1 1 calc R . . C51 C 1.1698(6) 0.2061(5) 0.1814(4) 0.0184(17) Uani 1 1 d . . . H51 H 1.1996 0.1570 0.1889 0.022 Uiso 1 1 calc R . . C52 C 1.0607(6) 0.2297(5) 0.1999(4) 0.0191(8) Uani 1 1 d . . . C53 C 1.0121(6) 0.3035(5) 0.1884(4) 0.0175(17) Uani 1 1 d . . . C54 C 1.0310(6) 0.1059(5) 0.2378(4) 0.0191(8) Uani 1 1 d . . . H54A H 1.0557 0.0683 0.1900 0.029 Uiso 1 1 calc R . . H54B H 0.9725 0.0773 0.2546 0.029 Uiso 1 1 calc R . . H54C H 1.0929 0.1192 0.2734 0.029 Uiso 1 1 calc R . . C1S C 0.2620(7) 0.6692(6) 0.3333(5) 0.036(2) Uani 1 1 d . . . H1S1 H 0.2573 0.6759 0.2839 0.044 Uiso 1 1 calc R . . C2S C 0.7897(7) 0.1137(6) 0.8000(5) 0.034(2) Uani 1 1 d . . . H2S H 0.7496 0.1685 0.8088 0.041 Uiso 1 1 calc R . . C3S C 0.3547(12) 0.4970(7) 0.1415(7) 0.092(3) Uani 1 1 d D . . H3S1 H 0.4066 0.5157 0.1837 0.138 Uiso 1 1 calc R . . H3S2 H 0.3062 0.4523 0.1461 0.138 Uiso 1 1 calc R . . H3S3 H 0.3106 0.5456 0.1402 0.138 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.0221(2) 0.0158(2) 0.0191(2) 0.00980(17) 0.00485(16) 0.00160(15) Zn1 0.0185(5) 0.0145(5) 0.0164(4) 0.0093(4) 0.0041(4) 0.0013(4) Zn2 0.0192(5) 0.0136(5) 0.0172(4) 0.0088(4) 0.0043(4) 0.0005(4) P1 0.0183(10) 0.0148(11) 0.0201(10) 0.0101(9) 0.0041(8) 0.0015(8) P2 0.0236(11) 0.0148(11) 0.0231(11) 0.0122(9) 0.0016(9) 0.0001(8) S1 0.0264(11) 0.0217(11) 0.0291(11) 0.0175(9) 0.0045(9) 0.0016(9) S2 0.0330(12) 0.0255(12) 0.0383(13) 0.0224(10) 0.0052(10) 0.0013(9) Cl1 0.0438(16) 0.082(2) 0.0355(14) 0.0148(14) 0.0026(12) -0.0049(14) Cl2 0.0335(14) 0.0572(17) 0.0469(14) 0.0166(13) -0.0013(11) -0.0078(12) Cl3 0.0350(13) 0.0460(15) 0.0574(15) 0.0267(13) 0.0076(12) -0.0014(11) Cl4 0.0322(14) 0.093(2) 0.0394(14) 0.0268(15) -0.0016(11) -0.0019(13) Cl5 0.0706(19) 0.0433(16) 0.0439(15) 0.0148(13) 0.0061(13) 0.0145(13) Cl6 0.0370(13) 0.0450(15) 0.0350(12) 0.0093(11) -0.0011(10) 0.0035(11) Cl7 0.0368(12) 0.0320(12) 0.0247(11) 0.0137(10) 0.0039(9) 0.0036(9) O1 0.0177(14) 0.0177(14) 0.0176(14) 0.0074(10) 0.0010(9) -0.0008(9) O2 0.032(3) 0.018(3) 0.021(3) 0.010(2) 0.004(2) 0.005(2) O3 0.022(3) 0.017(3) 0.018(3) 0.006(2) -0.003(2) -0.002(2) O4 0.024(3) 0.019(3) 0.027(3) 0.015(3) -0.003(2) -0.006(2) O5 0.019(3) 0.019(3) 0.018(3) 0.012(2) 0.005(2) -0.002(2) O6 0.026(3) 0.014(3) 0.022(3) 0.013(2) 0.009(2) 0.004(2) O7 0.023(3) 0.019(3) 0.017(3) 0.008(2) 0.005(2) 0.003(2) O8 0.023(3) 0.019(3) 0.023(3) 0.013(2) 0.002(2) -0.008(2) O9 0.027(3) 0.015(3) 0.014(3) 0.006(2) 0.004(2) 0.007(2) O10 0.032(3) 0.024(3) 0.020(3) 0.016(3) 0.005(2) -0.002(2) O11 0.013(3) 0.015(3) 0.026(3) 0.010(2) 0.005(2) -0.001(2) O12 0.022(2) 0.021(2) 0.022(2) 0.0157(18) 0.0045(16) 0.0031(16) O1S 0.134(7) 0.042(4) 0.096(6) 0.013(4) 0.064(5) 0.009(5) N1 0.031(4) 0.019(4) 0.024(4) 0.014(3) 0.003(3) 0.001(3) N2 0.020(4) 0.017(4) 0.031(4) 0.014(3) 0.005(3) 0.000(3) N3 0.027(4) 0.012(3) 0.029(4) 0.011(3) -0.003(3) -0.002(3) N4 0.022(4) 0.028(4) 0.029(4) 0.016(3) 0.004(3) 0.000(3) N5 0.026(4) 0.021(4) 0.022(3) 0.012(3) 0.006(3) 0.001(3) N6 0.024(4) 0.018(4) 0.022(3) 0.012(3) 0.005(3) 0.002(3) N7 0.036(4) 0.021(4) 0.025(4) 0.013(3) 0.010(3) 0.008(3) N8 0.028(4) 0.012(3) 0.024(4) 0.010(3) 0.004(3) 0.002(3) N9 0.0207(17) 0.0199(17) 0.0200(16) 0.0078(10) 0.0013(10) -0.0005(10) N10 0.020(4) 0.021(4) 0.024(3) 0.014(3) 0.006(3) 0.001(3) N11 0.026(4) 0.013(3) 0.029(4) 0.009(3) -0.008(3) -0.008(3) N12 0.0165(19) 0.023(2) 0.0183(19) 0.0083(16) 0.0029(15) -0.0029(15) C1 0.017(4) 0.024(5) 0.035(5) 0.015(4) -0.003(4) -0.008(3) C2 0.027(4) 0.015(4) 0.015(4) 0.003(3) 0.004(3) 0.002(3) C3 0.0187(19) 0.0187(19) 0.0189(19) 0.0066(11) 0.0007(10) 0.0010(10) C4 0.022(4) 0.019(4) 0.024(4) 0.007(4) 0.001(3) -0.005(3) C5 0.027(5) 0.026(5) 0.022(4) 0.008(4) 0.007(4) 0.005(4) C6 0.022(4) 0.023(5) 0.024(4) 0.011(4) -0.001(3) -0.005(3) C7 0.027(5) 0.016(4) 0.016(4) 0.005(3) 0.001(3) 0.004(3) C8 0.015(4) 0.015(4) 0.014(4) -0.002(3) 0.006(3) 0.009(3) C9 0.017(4) 0.022(5) 0.035(5) 0.018(4) 0.003(4) -0.001(3) C10 0.030(5) 0.020(5) 0.040(5) 0.018(4) 0.016(4) 0.008(4) C11 0.0203(19) 0.0210(19) 0.0203(19) 0.0074(11) 0.0003(10) 0.0005(10) C12 0.0165(19) 0.023(2) 0.0183(19) 0.0083(16) 0.0029(15) -0.0029(15) C13 0.0165(19) 0.023(2) 0.0183(19) 0.0083(16) 0.0029(15) -0.0029(15) C14 0.021(2) 0.024(3) 0.021(2) 0.007(2) 0.0045(19) 0.0023(19) C15 0.021(2) 0.024(3) 0.021(2) 0.007(2) 0.0045(19) 0.0023(19) C16 0.021(2) 0.024(3) 0.021(2) 0.007(2) 0.0045(19) 0.0023(19) C17 0.0165(19) 0.023(2) 0.0183(19) 0.0083(16) 0.0029(15) -0.0029(15) C18 0.037(5) 0.019(5) 0.028(5) 0.006(4) -0.006(4) 0.001(4) C19 0.034(5) 0.024(5) 0.022(4) 0.010(4) 0.002(4) 0.003(4) C20 0.028(5) 0.021(4) 0.021(4) 0.009(4) 0.006(4) -0.001(4) C21 0.027(5) 0.017(4) 0.023(4) 0.011(4) -0.001(4) -0.004(3) C22 0.026(4) 0.017(4) 0.011(4) 0.000(3) 0.011(3) 0.002(3) C23 0.015(4) 0.024(5) 0.025(4) 0.011(4) 0.002(3) 0.005(3) C24 0.016(4) 0.015(4) 0.023(4) 0.006(3) 0.003(3) 0.007(3) C25 0.022(4) 0.011(4) 0.019(4) 0.000(3) 0.001(3) -0.004(3) C26 0.0167(18) 0.0169(18) 0.0164(18) 0.0061(11) 0.0010(10) 0.0004(10) C27 0.021(4) 0.025(5) 0.028(4) 0.012(4) 0.004(4) 0.006(3) C28 0.030(5) 0.033(5) 0.041(5) 0.018(4) -0.003(4) 0.012(4) C29 0.025(5) 0.019(5) 0.033(5) 0.011(4) 0.006(4) 0.003(4) C30 0.0184(19) 0.0182(19) 0.0185(19) 0.0064(11) 0.0010(10) -0.0001(10) C31 0.025(5) 0.014(4) 0.031(5) 0.004(4) 0.000(4) -0.002(3) C32 0.026(5) 0.017(4) 0.025(4) -0.003(4) 0.008(4) -0.005(3) C33 0.027(5) 0.020(4) 0.019(4) 0.007(4) 0.006(3) -0.004(3) C34 0.023(4) 0.014(4) 0.022(4) 0.007(3) -0.003(3) -0.008(3) C35 0.016(4) 0.018(4) 0.015(4) 0.000(3) 0.006(3) 0.001(3) C36 0.022(4) 0.026(5) 0.017(4) 0.011(4) 0.004(3) 0.001(3) C37 0.030(5) 0.028(5) 0.025(4) 0.012(4) 0.000(4) -0.008(4) C38 0.019(2) 0.025(2) 0.022(2) 0.0099(18) -0.0010(16) -0.0033(17) C39 0.019(2) 0.025(2) 0.022(2) 0.0099(18) -0.0010(16) -0.0033(17) C40 0.019(2) 0.025(2) 0.022(2) 0.0099(18) -0.0010(16) -0.0033(17) C41 0.019(2) 0.025(2) 0.022(2) 0.0099(18) -0.0010(16) -0.0033(17) C42 0.028(5) 0.019(4) 0.029(4) 0.013(4) 0.002(4) -0.002(4) C43 0.021(4) 0.027(5) 0.017(4) 0.010(4) 0.005(3) 0.006(3) C44 0.013(4) 0.017(4) 0.018(4) 0.005(3) -0.002(3) 0.002(3) C45 0.033(5) 0.024(5) 0.017(4) 0.007(4) 0.004(4) 0.001(4) C46 0.028(5) 0.021(5) 0.056(6) 0.013(5) -0.010(4) -0.005(4) C47 0.021(4) 0.029(5) 0.017(4) 0.007(4) 0.003(3) -0.004(4) C48 0.023(4) 0.015(4) 0.016(4) 0.007(3) 0.006(3) 0.003(3) C49 0.019(4) 0.030(5) 0.022(4) 0.017(4) -0.006(3) -0.001(3) C50 0.015(4) 0.031(5) 0.026(4) 0.010(4) -0.002(3) -0.005(3) C51 0.018(4) 0.023(4) 0.015(4) 0.007(3) -0.001(3) 0.003(3) C52 0.022(2) 0.021(2) 0.022(2) 0.0157(18) 0.0045(16) 0.0031(16) C53 0.013(4) 0.029(5) 0.011(4) 0.007(3) 0.000(3) -0.008(3) C54 0.022(2) 0.021(2) 0.022(2) 0.0157(18) 0.0045(16) 0.0031(16) C1S 0.037(5) 0.051(6) 0.025(5) 0.019(5) -0.002(4) -0.002(5) C2S 0.027(5) 0.045(6) 0.033(5) 0.017(5) -0.006(4) -0.006(4) C3S 0.134(7) 0.042(4) 0.096(6) 0.013(4) 0.064(5) 0.009(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O9 2.395(5) . ? Gd1 O7 2.398(5) . ? Gd1 O11 2.402(5) . ? Gd1 O5 2.409(5) . ? Gd1 O1 2.432(5) . ? Gd1 O3 2.435(5) . ? Gd1 O10 2.768(5) . ? Gd1 O6 2.871(5) . ? Gd1 O12 2.883(5) . ? Gd1 O4 2.888(5) . ? Gd1 O2 2.899(5) . ? Gd1 O8 2.937(5) . ? Zn1 O3 2.086(5) . ? Zn1 O5 2.090(5) . ? Zn1 O1 2.095(5) . ? Zn1 N6 2.116(6) . ? Zn1 N2 2.127(6) . ? Zn1 N4 2.157(6) . ? Zn2 O9 2.070(5) . ? Zn2 O11 2.123(5) . ? Zn2 O7 2.134(5) . ? Zn2 N10 2.134(6) . ? Zn2 N12 2.141(6) . ? Zn2 N8 2.180(6) . ? P1 N5 1.645(6) . ? P1 N1 1.669(6) . ? P1 N3 1.678(7) . ? P1 S1 1.925(3) . ? P2 N7 1.661(7) . ? P2 N11 1.670(6) . ? P2 N9 1.675(6) . ? P2 S2 1.922(3) . ? Cl1 C2S 1.788(9) . ? Cl2 C2S 1.747(8) . ? Cl3 C2S 1.766(9) . ? Cl4 C1S 1.760(9) . ? Cl5 C1S 1.778(9) . ? Cl6 C1S 1.764(9) . ? O1 C8 1.299(8) . ? O2 C7 1.375(9) . ? O2 C9 1.452(8) . ? O3 C17 1.323(8) . ? O4 C16 1.389(8) . ? O4 C18 1.416(9) . ? O5 C26 1.309(8) . ? O6 C25 1.357(9) . ? O6 C27 1.437(8) . ? O7 C44 1.336(8) . ? O8 C43 1.380(8) . ? O8 C45 1.426(9) . ? O9 C35 1.325(8) . ? O10 C34 1.393(8) . ? O10 C36 1.441(8) . ? O11 C53 1.318(8) . ? O12 C52 1.383(9) . ? O12 C54 1.446(8) . ? O1S C3S 1.362(12) . ? N1 N2 1.451(8) . ? N1 C1 1.488(9) . ? N2 C2 1.292(9) . ? N3 N4 1.458(8) . ? N3 C10 1.465(9) . ? N4 C11 1.274(9) . ? N5 C19 1.473(9) . ? N5 N6 1.475(8) . ? N6 C20 1.301(9) . ? N7 N8 1.423(8) . ? N7 C28 1.463(9) . ? N8 C29 1.298(9) . ? N9 N10 1.432(8) . ? N9 C37 1.482(9) . ? N10 C38 1.277(9) . ? N11 N12 1.441(8) . ? N11 C46 1.477(10) . ? N12 C47 1.294(9) . ? C2 C3 1.433(10) . ? C3 C8 1.419(10) . ? C3 C4 1.435(10) . ? C4 C5 1.352(10) . ? C5 C6 1.394(10) . ? C6 C7 1.366(10) . ? C7 C8 1.422(10) . ? C11 C12 1.441(10) . ? C12 C13 1.412(10) . ? C12 C17 1.416(10) . ? C13 C14 1.347(10) . ? C14 C15 1.399(10) . ? C15 C16 1.356(10) . ? C16 C17 1.423(10) . ? C20 C21 1.423(10) . ? C21 C22 1.410(10) . ? C21 C26 1.435(10) . ? C22 C23 1.350(10) . ? C23 C24 1.391(10) . ? C24 C25 1.401(10) . ? C25 C26 1.405(10) . ? C29 C30 1.459(10) . ? C30 C35 1.398(10) . ? C30 C31 1.401(10) . ? C31 C32 1.387(10) . ? C32 C33 1.383(10) . ? C33 C34 1.363(10) . ? C34 C35 1.418(10) . ? C38 C39 1.457(10) . ? C39 C40 1.397(10) . ? C39 C44 1.416(10) . ? C40 C41 1.364(10) . ? C41 C42 1.407(10) . ? C42 C43 1.356(10) . ? C43 C44 1.406(10) . ? C47 C48 1.433(10) . ? C48 C53 1.403(10) . ? C48 C49 1.419(10) . ? C49 C50 1.356(10) . ? C50 C51 1.409(10) . ? C51 C52 1.378(10) . ? C52 C53 1.418(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 O9 Gd1 O7 66.53(16) . . ? O9 Gd1 O11 64.99(16) . . ? O7 Gd1 O11 67.79(16) . . ? O9 Gd1 O5 114.53(16) . . ? O7 Gd1 O5 113.96(17) . . ? O11 Gd1 O5 177.99(16) . . ? O9 Gd1 O1 175.68(15) . . ? O7 Gd1 O1 109.24(16) . . ? O11 Gd1 O1 114.74(16) . . ? O5 Gd1 O1 65.90(16) . . ? O9 Gd1 O3 119.04(16) . . ? O7 Gd1 O3 174.29(16) . . ? O11 Gd1 O3 112.74(16) . . ? O5 Gd1 O3 65.64(16) . . ? O1 Gd1 O3 65.21(16) . . ? O9 Gd1 O10 60.00(15) . . ? O7 Gd1 O10 116.54(15) . . ? O11 Gd1 O10 113.06(16) . . ? O5 Gd1 O10 65.40(16) . . ? O1 Gd1 O10 122.86(15) . . ? O3 Gd1 O10 68.77(15) . . ? O9 Gd1 O6 65.96(16) . . ? O7 Gd1 O6 65.59(15) . . ? O11 Gd1 O6 121.96(15) . . ? O5 Gd1 O6 58.81(15) . . ? O1 Gd1 O6 111.87(15) . . ? O3 Gd1 O6 117.09(15) . . ? O10 Gd1 O6 63.24(14) . . ? O9 Gd1 O12 115.39(16) . . ? O7 Gd1 O12 113.35(15) . . ? O11 Gd1 O12 58.34(15) . . ? O5 Gd1 O12 120.97(15) . . ? O1 Gd1 O12 66.68(15) . . ? O3 Gd1 O12 63.81(15) . . ? O10 Gd1 O12 118.65(14) . . ? O6 Gd1 O12 177.99(14) . . ? O9 Gd1 O4 68.73(15) . . ? O7 Gd1 O4 125.71(15) . . ? O11 Gd1 O4 66.43(15) . . ? O5 Gd1 O4 111.55(15) . . ? O1 Gd1 O4 115.34(15) . . ? O3 Gd1 O4 58.13(15) . . ? O10 Gd1 O4 60.36(15) . . ? O6 Gd1 O4 119.64(14) . . ? O12 Gd1 O4 62.37(14) . . ? O9 Gd1 O2 119.46(15) . . ? O7 Gd1 O2 63.90(15) . . ? O11 Gd1 O2 65.62(16) . . ? O5 Gd1 O2 115.90(16) . . ? O1 Gd1 O2 57.78(15) . . ? O3 Gd1 O2 110.85(15) . . ? O10 Gd1 O2 178.46(15) . . ? O6 Gd1 O2 118.03(14) . . ? O12 Gd1 O2 60.09(14) . . ? O4 Gd1 O2 118.13(15) . . ? O9 Gd1 O8 113.87(15) . . ? O7 Gd1 O8 58.38(15) . . ? O11 Gd1 O8 117.55(15) . . ? O5 Gd1 O8 64.46(15) . . ? O1 Gd1 O8 62.18(15) . . ? O3 Gd1 O8 117.89(15) . . ? O10 Gd1 O8 117.56(15) . . ? O6 Gd1 O8 60.07(14) . . ? O12 Gd1 O8 117.94(14) . . ? O4 Gd1 O8 175.76(13) . . ? O2 Gd1 O8 63.96(14) . . ? O3 Zn1 O5 77.91(19) . . ? O3 Zn1 O1 77.70(19) . . ? O5 Zn1 O1 78.00(18) . . ? O3 Zn1 N6 122.2(2) . . ? O5 Zn1 N6 83.1(2) . . ? O1 Zn1 N6 148.8(2) . . ? O3 Zn1 N2 148.1(2) . . ? O5 Zn1 N2 123.3(2) . . ? O1 Zn1 N2 83.7(2) . . ? N6 Zn1 N2 86.3(2) . . ? O3 Zn1 N4 83.6(2) . . ? O5 Zn1 N4 149.6(2) . . ? O1 Zn1 N4 121.5(2) . . ? N6 Zn1 N4 86.7(2) . . ? N2 Zn1 N4 84.3(2) . . ? O3 Zn1 Gd1 46.77(13) . . ? O5 Zn1 Gd1 46.08(13) . . ? O1 Zn1 Gd1 46.73(13) . . ? N6 Zn1 Gd1 127.38(16) . . ? N2 Zn1 Gd1 128.67(17) . . ? N4 Zn1 Gd1 128.55(18) . . ? O9 Zn2 O11 75.85(18) . . ? O9 Zn2 O7 77.40(19) . . ? O11 Zn2 O7 77.93(18) . . ? O9 Zn2 N10 148.7(2) . . ? O11 Zn2 N10 123.3(2) . . ? O7 Zn2 N10 82.7(2) . . ? O9 Zn2 N12 123.4(2) . . ? O11 Zn2 N12 82.7(2) . . ? O7 Zn2 N12 146.9(2) . . ? N10 Zn2 N12 85.9(2) . . ? O9 Zn2 N8 84.4(2) . . ? O11 Zn2 N8 147.1(2) . . ? O7 Zn2 N8 123.4(2) . . ? N10 Zn2 N8 86.6(2) . . ? N12 Zn2 N8 86.7(2) . . ? O9 Zn2 Gd1 45.81(13) . . ? O11 Zn2 Gd1 46.14(13) . . ? O7 Zn2 Gd1 46.05(13) . . ? N10 Zn2 Gd1 127.08(17) . . ? N12 Zn2 Gd1 127.71(16) . . ? N8 Zn2 Gd1 128.51(16) . . ? N5 P1 N1 107.3(3) . . ? N5 P1 N3 106.3(3) . . ? N1 P1 N3 105.1(3) . . ? N5 P1 S1 112.2(2) . . ? N1 P1 S1 113.1(2) . . ? N3 P1 S1 112.3(2) . . ? N7 P2 N11 108.1(3) . . ? N7 P2 N9 104.1(3) . . ? N11 P2 N9 104.4(3) . . ? N7 P2 S2 113.0(2) . . ? N11 P2 S2 112.6(2) . . ? N9 P2 S2 113.9(2) . . ? C8 O1 Zn1 132.0(5) . . ? C8 O1 Gd1 133.6(4) . . ? Zn1 O1 Gd1 94.44(18) . . ? C7 O2 C9 115.5(6) . . ? C7 O2 Gd1 115.8(4) . . ? C9 O2 Gd1 128.6(4) . . ? C17 O3 Zn1 132.7(4) . . ? C17 O3 Gd1 132.7(4) . . ? Zn1 O3 Gd1 94.60(18) . . ? C16 O4 C18 116.5(6) . . ? C16 O4 Gd1 116.5(4) . . ? C18 O4 Gd1 126.9(4) . . ? C26 O5 Zn1 133.0(4) . . ? C26 O5 Gd1 131.7(4) . . ? Zn1 O5 Gd1 95.25(18) . . ? C25 O6 C27 116.7(6) . . ? C25 O6 Gd1 114.9(4) . . ? C27 O6 Gd1 128.4(4) . . ? C44 O7 Zn2 133.1(4) . . ? C44 O7 Gd1 131.9(4) . . ? Zn2 O7 Gd1 94.10(18) . . ? C43 O8 C45 115.8(6) . . ? C43 O8 Gd1 113.6(4) . . ? C45 O8 Gd1 130.2(4) . . ? C35 O9 Zn2 133.0(4) . . ? C35 O9 Gd1 129.8(4) . . ? Zn2 O9 Gd1 95.89(18) . . ? C34 O10 C36 115.4(6) . . ? C34 O10 Gd1 116.7(4) . . ? C36 O10 Gd1 127.7(4) . . ? C53 O11 Zn2 131.8(4) . . ? C53 O11 Gd1 133.8(4) . . ? Zn2 O11 Gd1 94.28(18) . . ? C52 O12 C54 115.9(5) . . ? C52 O12 Gd1 115.4(4) . . ? C54 O12 Gd1 128.3(4) . . ? N2 N1 C1 114.1(5) . . ? N2 N1 P1 113.8(5) . . ? C1 N1 P1 120.1(5) . . ? C2 N2 N1 112.1(6) . . ? C2 N2 Zn1 128.0(5) . . ? N1 N2 Zn1 119.0(4) . . ? N4 N3 C10 114.0(6) . . ? N4 N3 P1 113.8(4) . . ? C10 N3 P1 119.3(5) . . ? C11 N4 N3 113.2(6) . . ? C11 N4 Zn1 127.6(5) . . ? N3 N4 Zn1 118.5(5) . . ? C19 N5 N6 112.5(6) . . ? C19 N5 P1 122.3(5) . . ? N6 N5 P1 114.7(4) . . ? C20 N6 N5 112.3(6) . . ? C20 N6 Zn1 129.1(5) . . ? N5 N6 Zn1 117.7(4) . . ? N8 N7 C28 119.3(6) . . ? N8 N7 P2 115.8(5) . . ? C28 N7 P2 124.7(5) . . ? C29 N8 N7 115.8(6) . . ? C29 N8 Zn2 127.9(5) . . ? N7 N8 Zn2 115.8(4) . . ? N10 N9 C37 114.2(6) . . ? N10 N9 P2 116.2(5) . . ? C37 N9 P2 119.1(5) . . ? C38 N10 N9 111.5(6) . . ? C38 N10 Zn2 131.1(5) . . ? N9 N10 Zn2 117.4(4) . . ? N12 N11 C46 114.3(6) . . ? N12 N11 P2 115.6(4) . . ? C46 N11 P2 119.2(5) . . ? C47 N12 N11 112.8(6) . . ? C47 N12 Zn2 129.1(5) . . ? N11 N12 Zn2 117.6(4) . . ? N2 C2 C3 125.9(7) . . ? C8 C3 C2 124.0(7) . . ? C8 C3 C4 119.1(7) . . ? C2 C3 C4 116.8(7) . . ? C5 C4 C3 120.8(7) . . ? C4 C5 C6 120.4(7) . . ? C7 C6 C5 120.6(7) . . ? C6 C7 O2 125.1(7) . . ? C6 C7 C8 121.5(7) . . ? O2 C7 C8 113.4(6) . . ? O1 C8 C3 123.2(7) . . ? O1 C8 C7 119.3(7) . . ? C3 C8 C7 117.5(6) . . ? N4 C11 C12 127.8(7) . . ? C13 C12 C17 119.1(7) . . ? C13 C12 C11 117.8(7) . . ? C17 C12 C11 123.1(7) . . ? C14 C13 C12 121.3(7) . . ? C13 C14 C15 120.4(8) . . ? C16 C15 C14 120.0(8) . . ? C15 C16 O4 125.8(7) . . ? C15 C16 C17 121.5(7) . . ? O4 C16 C17 112.7(7) . . ? O3 C17 C12 123.1(7) . . ? O3 C17 C16 119.4(7) . . ? C12 C17 C16 117.5(7) . . ? N6 C20 C21 126.0(7) . . ? C22 C21 C20 118.2(7) . . ? C22 C21 C26 118.2(7) . . ? C20 C21 C26 123.5(7) . . ? C23 C22 C21 122.5(7) . . ? C22 C23 C24 119.8(7) . . ? C23 C24 C25 120.3(7) . . ? O6 C25 C24 124.6(7) . . ? O6 C25 C26 114.7(7) . . ? C24 C25 C26 120.6(7) . . ? O5 C26 C25 119.6(7) . . ? O5 C26 C21 122.1(6) . . ? C25 C26 C21 118.3(7) . . ? N8 C29 C30 125.9(7) . . ? C35 C30 C31 119.5(7) . . ? C35 C30 C29 124.3(7) . . ? C31 C30 C29 116.1(7) . . ? C32 C31 C30 121.5(7) . . ? C33 C32 C31 119.4(7) . . ? C34 C33 C32 119.5(7) . . ? C33 C34 O10 124.2(7) . . ? C33 C34 C35 122.9(7) . . ? O10 C34 C35 112.8(6) . . ? O9 C35 C30 124.0(7) . . ? O9 C35 C34 118.9(6) . . ? C30 C35 C34 117.1(6) . . ? N10 C38 C39 126.7(7) . . ? C40 C39 C44 120.4(7) . . ? C40 C39 C38 116.1(7) . . ? C44 C39 C38 123.5(7) . . ? C41 C40 C39 120.8(7) . . ? C40 C41 C42 119.2(7) . . ? C43 C42 C41 120.5(7) . . ? C42 C43 O8 124.0(7) . . ? C42 C43 C44 121.9(7) . . ? O8 C43 C44 114.0(7) . . ? O7 C44 C43 120.3(6) . . ? O7 C44 C39 122.7(7) . . ? C43 C44 C39 117.0(7) . . ? N12 C47 C48 126.5(7) . . ? C53 C48 C49 119.8(7) . . ? C53 C48 C47 123.6(7) . . ? C49 C48 C47 116.6(7) . . ? C50 C49 C48 121.3(7) . . ? C49 C50 C51 119.7(7) . . ? C52 C51 C50 119.8(7) . . ? C51 C52 O12 124.7(7) . . ? C51 C52 C53 121.6(7) . . ? O12 C52 C53 113.7(6) . . ? O11 C53 C48 123.7(7) . . ? O11 C53 C52 118.7(6) . . ? C48 C53 C52 117.6(7) . . ? Cl4 C1S Cl6 110.1(5) . . ? Cl4 C1S Cl5 110.8(5) . . ? Cl6 C1S Cl5 109.1(5) . . ? Cl2 C2S Cl3 111.1(5) . . ? Cl2 C2S Cl1 110.3(5) . . ? Cl3 C2S Cl1 108.4(5) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.940 _refine_diff_density_min -1.463 _refine_diff_density_rms 0.175 _database_code_depnum_ccdc_archive 'CCDC 941521' ####################################################################### # # 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_Zn2Tb _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H66 Cl7 N12 O13 P2 S2 Tb Zn2' _chemical_formula_weight 1791.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.914(5) _cell_length_b 16.320(5) _cell_length_c 18.988(5) _cell_angle_alpha 109.819(5) _cell_angle_beta 91.748(5) _cell_angle_gamma 90.064(5) _cell_volume 3471(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6010 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 28.22 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.105 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1804 _exptl_absorpt_coefficient_mu 2.138 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.801603 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18938 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0508 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 25.50 _reflns_number_total 12624 _reflns_number_gt 10038 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+21.6157P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12598 _refine_ls_number_parameters 867 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1349 _refine_ls_wR_factor_gt 0.1059 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.26478(2) 0.254851(18) 0.756241(15) 0.01588(9) Uani 1 1 d . . . Zn2 Zn 0.29469(5) 0.41280(4) 0.68557(3) 0.01325(15) Uani 1 1 d . . . Zn1 Zn 0.23041(5) 0.08980(4) 0.81845(3) 0.01333(15) Uani 1 1 d . . . Cl1 Cl 0.82850(14) 0.69339(11) 0.67388(9) 0.0279(3) Uani 1 1 d . . . Cl2 Cl 0.89319(15) 0.71177(15) 0.87673(10) 0.0437(5) Uani 1 1 d . . . Cl3 Cl 0.65230(14) 0.72918(12) 0.88836(10) 0.0341(4) Uani 1 1 d . . . Cl4 Cl 0.74726(18) 0.55834(13) 0.82212(11) 0.0452(5) Uani 1 1 d . . . Cl5 Cl 0.57510(15) 0.86243(13) 0.65939(11) 0.0410(4) Uani 1 1 d . . . Cl6 Cl 0.70337(17) 0.94102(16) 0.79865(11) 0.0516(5) Uani 1 1 d . . . Cl7 Cl 0.78484(15) 0.95200(13) 0.66073(11) 0.0401(4) Uani 1 1 d . . . P1 P 0.19284(12) -0.07501(10) 0.88215(8) 0.0154(3) Uani 1 1 d . . . P2 P 0.32406(12) 0.57059(10) 0.61358(9) 0.0167(3) Uani 1 1 d . . . S1 S 0.16942(13) -0.16940(10) 0.91996(9) 0.0210(3) Uani 1 1 d . . . S2 S 0.34229(14) 0.66247(11) 0.57256(10) 0.0259(4) Uani 1 1 d . . . O1 O 0.1281(3) 0.1915(3) 0.8122(2) 0.0155(8) Uani 1 1 d . . . O2 O 0.0395(3) 0.3190(3) 0.7754(2) 0.0185(9) Uani 1 1 d . . . O3 O 0.3419(3) 0.1954(2) 0.8476(2) 0.0153(8) Uani 1 1 d . . . O4 O 0.4404(3) 0.3439(2) 0.8628(2) 0.0174(9) Uani 1 1 d . . . O5 O 0.2700(3) 0.0977(2) 0.7146(2) 0.0161(8) Uani 1 1 d . . . O6 O 0.3293(4) 0.1507(3) 0.6053(2) 0.0196(9) Uani 1 1 d . . . O7 O 0.2519(3) 0.4081(3) 0.7887(2) 0.0174(8) Uani 1 1 d . . . O8 O 0.2115(3) 0.3552(3) 0.9003(2) 0.0204(9) Uani 1 1 d . . . O9 O 0.4051(3) 0.3205(3) 0.7050(2) 0.0163(8) Uani 1 1 d . . . O10 O 0.4891(3) 0.1840(3) 0.7312(2) 0.0195(9) Uani 1 1 d . . . O11 O 0.1909(3) 0.2986(3) 0.6568(2) 0.0162(8) Uani 1 1 d . . . O12 O 0.0821(3) 0.1571(3) 0.6551(2) 0.0196(9) Uani 1 1 d . . . O1S O 0.9136(8) 0.4635(5) 0.5760(5) 0.093(3) Uani 1 1 d D . . H1S H 0.9268 0.4117 0.5670 0.139 Uiso 1 1 calc R . . N1 N 0.1268(4) 0.0156(3) 0.9311(3) 0.0183(6) Uani 1 1 d U . . N2 N 0.1067(4) 0.0765(3) 0.8926(3) 0.0183(6) Uani 1 1 d . . . N3 N 0.3294(4) -0.0479(3) 0.8837(3) 0.0202(11) Uani 1 1 d . . . N4 N 0.3470(4) 0.0390(3) 0.8808(3) 0.0195(11) Uani 1 1 d . . . N5 N 0.1483(4) -0.0989(3) 0.7933(3) 0.0195(11) Uani 1 1 d . . . N6 N 0.1961(4) -0.0438(3) 0.7553(3) 0.0171(10) Uani 1 1 d . . . N7 N 0.2208(4) 0.5886(3) 0.6743(3) 0.0190(11) Uani 1 1 d . . . N8 N 0.2301(4) 0.5455(3) 0.7274(3) 0.0166(10) Uani 1 1 d . . . N9 N 0.4421(4) 0.5531(3) 0.6564(3) 0.0204(11) Uani 1 1 d . . . N10 N 0.4474(4) 0.4693(3) 0.6666(3) 0.0196(11) Uani 1 1 d . . . N11 N 0.2935(4) 0.4738(3) 0.5490(3) 0.0198(11) Uani 1 1 d . . . N12 N 0.2430(4) 0.4114(3) 0.5771(3) 0.0187(11) Uani 1 1 d . . . C2 C 0.0058(5) 0.1060(4) 0.9003(3) 0.0229(13) Uani 1 1 d . . . H2 H -0.0410 0.0854 0.9290 0.027 Uiso 1 1 calc R . . C3 C -0.0417(5) 0.1679(4) 0.8689(3) 0.0169(12) Uani 1 1 d . . . C4 C -0.1554(5) 0.1877(4) 0.8813(3) 0.0241(14) Uani 1 1 d . . . H4 H -0.1972 0.1591 0.9067 0.029 Uiso 1 1 calc R . . C5 C -0.2059(5) 0.2486(4) 0.8566(3) 0.0220(13) Uani 1 1 d . . . H5 H -0.2821 0.2596 0.8633 0.026 Uiso 1 1 calc R . . C6 C -0.1415(5) 0.2948(4) 0.8207(3) 0.0190(12) Uani 1 1 d . . . H6 H -0.1751 0.3374 0.8050 0.023 Uiso 1 1 calc R . . C7 C -0.0303(5) 0.2773(4) 0.8088(3) 0.0151(12) Uani 1 1 d . . . C8 C 0.0236(5) 0.2104(4) 0.8299(3) 0.0189(12) Uani 1 1 d . . . C9 C -0.0096(5) 0.3861(4) 0.7525(3) 0.0169(12) Uani 1 1 d . . . H9A H -0.0712 0.3622 0.7177 0.025 Uiso 1 1 calc R . . H9B H 0.0457 0.4098 0.7289 0.025 Uiso 1 1 calc R . . H9C H -0.0365 0.4313 0.7955 0.025 Uiso 1 1 calc R . . C10 C 0.4073(5) -0.1129(4) 0.8391(3) 0.0218(13) Uani 1 1 d . . . H10A H 0.4070 -0.1115 0.7890 0.033 Uiso 1 1 calc R . . H10B H 0.3843 -0.1697 0.8380 0.033 Uiso 1 1 calc R . . H10C H 0.4816 -0.1001 0.8612 0.033 Uiso 1 1 calc R . . C11 C 0.4273(5) 0.0805(4) 0.9267(3) 0.0213(13) Uani 1 1 d . . . H11 H 0.4623 0.0512 0.9555 0.026 Uiso 1 1 calc R . . C12 C 0.4679(5) 0.1668(4) 0.9376(3) 0.0168(12) Uani 1 1 d . . . C13 C 0.5565(5) 0.1994(4) 0.9916(3) 0.0218(13) Uani 1 1 d . . . H13 H 0.5845 0.1643 1.0177 0.026 Uiso 1 1 calc R . . C14 C 0.6021(5) 0.2808(4) 1.0067(3) 0.0207(13) Uani 1 1 d . . . H14 H 0.6580 0.3018 1.0438 0.025 Uiso 1 1 calc R . . C15 C 0.5626(5) 0.3319(4) 0.9648(3) 0.0213(13) Uani 1 1 d . . . H15 H 0.5927 0.3874 0.9745 0.026 Uiso 1 1 calc R . . C16 C 0.4809(5) 0.3014(4) 0.9103(3) 0.0162(12) Uani 1 1 d . . . C17 C 0.4257(4) 0.2194(4) 0.8972(3) 0.0143(11) Uani 1 1 d . . . C18 C 0.4936(5) 0.4251(4) 0.8700(4) 0.0248(14) Uani 1 1 d . . . H18A H 0.4794 0.4667 0.9184 0.037 Uiso 1 1 calc R . . H18B H 0.4641 0.4461 0.8318 0.037 Uiso 1 1 calc R . . H18C H 0.5731 0.4169 0.8647 0.037 Uiso 1 1 calc R . . C19 C 0.0287(5) -0.1216(4) 0.7713(4) 0.0244(14) Uani 1 1 d . . . H19A H -0.0152 -0.0696 0.7864 0.037 Uiso 1 1 calc R . . H19B H 0.0024 -0.1609 0.7952 0.037 Uiso 1 1 calc R . . H19C H 0.0216 -0.1491 0.7179 0.037 Uiso 1 1 calc R . . C20 C 0.2320(5) -0.0877(4) 0.6905(3) 0.0182(12) Uani 1 1 d . . . H20 H 0.2277 -0.1480 0.6767 0.022 Uiso 1 1 calc R . . C21 C 0.2789(5) -0.0533(4) 0.6363(3) 0.0161(12) Uani 1 1 d . . . C22 C 0.3071(5) -0.1139(4) 0.5676(3) 0.0207(13) Uani 1 1 d . . . H22 H 0.2999 -0.1730 0.5599 0.025 Uiso 1 1 calc R . . C23 C 0.3451(5) -0.0877(4) 0.5115(3) 0.0226(13) Uani 1 1 d . . . H23 H 0.3658 -0.1287 0.4666 0.027 Uiso 1 1 calc R . . C24 C 0.3530(5) 0.0017(4) 0.5220(3) 0.0193(13) Uani 1 1 d . . . H24 H 0.3766 0.0201 0.4835 0.023 Uiso 1 1 calc R . . C25 C 0.3257(5) 0.0615(4) 0.5895(3) 0.0196(13) Uani 1 1 d . . . C26 C 0.2897(5) 0.0374(4) 0.6499(3) 0.0182(12) Uani 1 1 d . . . C27 C 0.3594(5) 0.1797(4) 0.5453(3) 0.0200(13) Uani 1 1 d . . . H27A H 0.4342 0.1613 0.5307 0.030 Uiso 1 1 calc R . . H27B H 0.3562 0.2421 0.5615 0.030 Uiso 1 1 calc R . . H27C H 0.3079 0.1552 0.5035 0.030 Uiso 1 1 calc R . . C28 C 0.1320(5) 0.6504(5) 0.6782(4) 0.0295(15) Uani 1 1 d . . . H28A H 0.0623 0.6271 0.6877 0.044 Uiso 1 1 calc R . . H28B H 0.1253 0.6609 0.6315 0.044 Uiso 1 1 calc R . . H28C H 0.1495 0.7041 0.7179 0.044 Uiso 1 1 calc R . . C29 C 0.1853(5) 0.5842(4) 0.7910(4) 0.0207(13) Uani 1 1 d . . . H29 H 0.1540 0.6385 0.7980 0.025 Uiso 1 1 calc R . . C30 C 0.1791(5) 0.5508(4) 0.8531(3) 0.0184(12) Uani 1 1 d . . . C31 C 0.1347(5) 0.6077(4) 0.9190(3) 0.0180(12) Uani 1 1 d . . . H31 H 0.1147 0.6636 0.9212 0.022 Uiso 1 1 calc R . . C32 C 0.1201(5) 0.5829(4) 0.9800(3) 0.0189(12) Uani 1 1 d . . . H32 H 0.0922 0.6222 1.0236 0.023 Uiso 1 1 calc R . . C33 C 0.1471(5) 0.4985(4) 0.9767(3) 0.0185(12) Uani 1 1 d . . . H33 H 0.1376 0.4813 1.0181 0.022 Uiso 1 1 calc R . . C34 C 0.1880(5) 0.4410(4) 0.9114(3) 0.0160(12) Uani 1 1 d . . . C35 C 0.2084(4) 0.4663(4) 0.8487(3) 0.0130(11) Uani 1 1 d . . . C36 C 0.1945(5) 0.3280(4) 0.9632(3) 0.0227(13) Uani 1 1 d . . . H36A H 0.2413 0.3625 1.0048 0.034 Uiso 1 1 calc R . . H36B H 0.2137 0.2677 0.9506 0.034 Uiso 1 1 calc R . . H36C H 0.1172 0.3356 0.9765 0.034 Uiso 1 1 calc R . . C37 C 0.4932(6) 0.6248(4) 0.7191(4) 0.0291(15) Uani 1 1 d . . . H37A H 0.4651 0.6232 0.7655 0.044 Uiso 1 1 calc R . . H37B H 0.4745 0.6795 0.7134 0.044 Uiso 1 1 calc R . . H37C H 0.5733 0.6186 0.7194 0.044 Uiso 1 1 calc R . . C38 C 0.5462(5) 0.4362(4) 0.6550(3) 0.0177(12) Uani 1 1 d . . . H38 H 0.5999 0.4679 0.6402 0.021 Uiso 1 1 calc R . . C39 C 0.5820(5) 0.3556(4) 0.6628(3) 0.0168(12) Uani 1 1 d . . . C40 C 0.6918(5) 0.3300(4) 0.6432(3) 0.0230(13) Uani 1 1 d . . . H40 H 0.7362 0.3639 0.6241 0.028 Uiso 1 1 calc R . . C41 C 0.7364(5) 0.2554(4) 0.6515(3) 0.0214(13) Uani 1 1 d . . . H41 H 0.8094 0.2389 0.6377 0.026 Uiso 1 1 calc R . . C42 C 0.6688(5) 0.2052(4) 0.6812(3) 0.0215(13) Uani 1 1 d . . . H42 H 0.6981 0.1556 0.6882 0.026 Uiso 1 1 calc R . . C43 C 0.5609(5) 0.2283(4) 0.7000(3) 0.0178(12) Uani 1 1 d . . . C44 C 0.5109(5) 0.3021(4) 0.6887(3) 0.0162(12) Uani 1 1 d . . . C45 C 0.5315(5) 0.1051(4) 0.7380(4) 0.0226(13) Uani 1 1 d . . . H45A H 0.5503 0.0659 0.6894 0.034 Uiso 1 1 calc R . . H45B H 0.4754 0.0786 0.7587 0.034 Uiso 1 1 calc R . . H45C H 0.5975 0.1178 0.7704 0.034 Uiso 1 1 calc R . . C46 C 0.3689(5) 0.4355(4) 0.4867(3) 0.0228(13) Uani 1 1 d . . . H46A H 0.4263 0.4032 0.5019 0.034 Uiso 1 1 calc R . . H46B H 0.4029 0.4811 0.4731 0.034 Uiso 1 1 calc R . . H46C H 0.3267 0.3973 0.4445 0.034 Uiso 1 1 calc R . . C47 C 0.1739(5) 0.3598(4) 0.5278(3) 0.0196(13) Uani 1 1 d . . . H47 H 0.1628 0.3711 0.4833 0.024 Uiso 1 1 calc R . . C48 C 0.1119(5) 0.2863(4) 0.5344(3) 0.0192(13) Uani 1 1 d . . . C49 C 0.0417(5) 0.2413(4) 0.4739(3) 0.0194(12) Uani 1 1 d . . . H49 H 0.0357 0.2601 0.4328 0.023 Uiso 1 1 calc R . . C50 C -0.0187(5) 0.1701(4) 0.4735(3) 0.0226(13) Uani 1 1 d . . . H50 H -0.0666 0.1414 0.4330 0.027 Uiso 1 1 calc R . . C51 C -0.0079(5) 0.1405(4) 0.5343(3) 0.0212(13) Uani 1 1 d . . . H51 H -0.0485 0.0916 0.5340 0.025 Uiso 1 1 calc R . . C52 C 0.0615(5) 0.1825(4) 0.5941(3) 0.0157(12) Uani 1 1 d . . . C53 C 0.1256(4) 0.2584(4) 0.5970(3) 0.0145(11) Uani 1 1 d . . . C54 C 0.0200(5) 0.0816(4) 0.6554(3) 0.0204(13) Uani 1 1 d . . . H54A H -0.0587 0.0943 0.6583 0.031 Uiso 1 1 calc R . . H54B H 0.0442 0.0659 0.6978 0.031 Uiso 1 1 calc R . . H54C H 0.0331 0.0340 0.6101 0.031 Uiso 1 1 calc R . . C1A C 0.1557(5) 0.0585(4) 1.0117(3) 0.0183(6) Uani 1 1 d . . . H1A1 H 0.2170 0.0987 1.0174 0.027 Uiso 1 1 calc R . . H1A2 H 0.1771 0.0153 1.0333 0.027 Uiso 1 1 calc R . . H1A3 H 0.0916 0.0894 1.0367 0.027 Uiso 1 1 calc R . . C1S C 0.7623(5) 0.6700(4) 0.8335(3) 0.0265(14) Uani 1 1 d . . . H1S1 H 0.7572 0.6766 0.7840 0.032 Uiso 1 1 calc R . . C2S C 0.7101(5) 0.8861(4) 0.7004(4) 0.0273(14) Uani 1 1 d . . . H2S H 0.7504 0.8314 0.6916 0.033 Uiso 1 1 calc R . . C3S C 0.8595(7) 0.4967(6) 0.6450(4) 0.048(2) Uani 1 1 d DU . . H3S1 H 0.9021 0.5450 0.6782 0.071 Uiso 1 1 calc R . . H3S2 H 0.8539 0.4518 0.6669 0.071 Uiso 1 1 calc R . . H3S3 H 0.7856 0.5156 0.6366 0.071 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.01936(16) 0.01438(16) 0.01661(15) 0.00865(12) 0.00240(11) -0.00004(11) Zn2 0.0156(3) 0.0125(3) 0.0139(3) 0.0073(3) 0.0012(2) -0.0007(2) Zn1 0.0150(3) 0.0133(3) 0.0137(3) 0.0072(3) 0.0013(2) -0.0003(3) Cl1 0.0335(9) 0.0296(9) 0.0227(8) 0.0115(7) 0.0026(6) 0.0036(7) Cl2 0.0261(9) 0.0766(15) 0.0303(9) 0.0209(10) -0.0031(7) -0.0023(9) Cl3 0.0308(9) 0.0389(10) 0.0300(9) 0.0081(8) 0.0010(7) 0.0046(7) Cl4 0.0621(13) 0.0344(10) 0.0392(11) 0.0122(9) 0.0053(9) 0.0092(9) Cl5 0.0290(9) 0.0508(12) 0.0402(10) 0.0119(9) -0.0012(8) -0.0099(8) Cl6 0.0404(11) 0.0762(16) 0.0339(10) 0.0129(10) 0.0041(8) -0.0063(10) Cl7 0.0317(9) 0.0419(11) 0.0543(12) 0.0260(9) 0.0039(8) -0.0042(8) P1 0.0166(7) 0.0152(8) 0.0176(7) 0.0097(6) 0.0021(6) -0.0001(6) P2 0.0193(8) 0.0148(8) 0.0204(8) 0.0117(6) 0.0010(6) -0.0008(6) S1 0.0243(8) 0.0191(8) 0.0260(8) 0.0161(7) 0.0015(6) -0.0008(6) S2 0.0300(9) 0.0216(8) 0.0334(9) 0.0189(7) 0.0020(7) -0.0012(7) O1 0.0077(18) 0.019(2) 0.022(2) 0.0099(18) 0.0047(15) -0.0009(15) O2 0.021(2) 0.021(2) 0.020(2) 0.0140(18) 0.0013(17) 0.0011(17) O3 0.020(2) 0.013(2) 0.014(2) 0.0074(16) -0.0030(16) -0.0039(16) O4 0.017(2) 0.012(2) 0.025(2) 0.0098(17) -0.0017(17) -0.0074(16) O5 0.021(2) 0.014(2) 0.015(2) 0.0064(17) 0.0010(16) -0.0036(16) O6 0.036(2) 0.013(2) 0.011(2) 0.0057(17) 0.0084(17) 0.0033(18) O7 0.020(2) 0.014(2) 0.017(2) 0.0041(17) 0.0018(16) -0.0001(16) O8 0.026(2) 0.012(2) 0.025(2) 0.0086(18) 0.0053(18) 0.0028(17) O9 0.0086(18) 0.020(2) 0.024(2) 0.0113(18) 0.0031(16) -0.0031(16) O10 0.021(2) 0.022(2) 0.020(2) 0.0131(18) 0.0028(17) 0.0028(17) O11 0.021(2) 0.018(2) 0.0117(19) 0.0088(17) -0.0068(16) -0.0041(17) O12 0.027(2) 0.016(2) 0.018(2) 0.0098(18) -0.0002(17) -0.0046(17) O1S 0.098(6) 0.076(6) 0.097(6) 0.018(5) 0.014(5) 0.001(5) N1 0.0201(10) 0.0185(10) 0.0179(10) 0.0081(8) 0.0006(8) -0.0003(8) N2 0.0201(10) 0.0185(10) 0.0179(10) 0.0081(8) 0.0006(8) -0.0003(8) N3 0.023(3) 0.016(3) 0.025(3) 0.011(2) -0.003(2) -0.002(2) N4 0.017(3) 0.021(3) 0.022(3) 0.010(2) 0.001(2) 0.000(2) N5 0.019(3) 0.019(3) 0.024(3) 0.013(2) 0.000(2) -0.005(2) N6 0.022(3) 0.013(2) 0.021(3) 0.011(2) 0.001(2) -0.004(2) N7 0.030(3) 0.016(3) 0.016(2) 0.012(2) 0.004(2) 0.005(2) N8 0.014(2) 0.020(3) 0.015(2) 0.004(2) -0.0003(19) 0.000(2) N9 0.020(3) 0.016(3) 0.027(3) 0.010(2) -0.005(2) -0.004(2) N10 0.022(3) 0.019(3) 0.022(3) 0.013(2) 0.001(2) -0.001(2) N11 0.025(3) 0.023(3) 0.014(2) 0.009(2) 0.001(2) -0.006(2) N12 0.021(3) 0.016(3) 0.022(3) 0.010(2) 0.002(2) 0.002(2) C2 0.014(3) 0.034(4) 0.022(3) 0.012(3) 0.003(2) -0.006(3) C3 0.016(3) 0.020(3) 0.017(3) 0.008(2) 0.003(2) -0.003(2) C4 0.022(3) 0.027(4) 0.022(3) 0.007(3) 0.006(3) 0.001(3) C5 0.020(3) 0.022(3) 0.021(3) 0.003(3) 0.002(2) 0.007(3) C6 0.021(3) 0.019(3) 0.019(3) 0.010(3) -0.002(2) 0.002(2) C7 0.018(3) 0.016(3) 0.008(3) 0.000(2) -0.001(2) -0.003(2) C8 0.024(3) 0.017(3) 0.011(3) -0.002(2) 0.001(2) 0.005(2) C9 0.016(3) 0.014(3) 0.021(3) 0.006(2) 0.000(2) 0.006(2) C10 0.019(3) 0.024(3) 0.026(3) 0.013(3) 0.000(2) 0.000(2) C11 0.020(3) 0.027(3) 0.021(3) 0.015(3) 0.006(2) 0.008(3) C12 0.012(3) 0.020(3) 0.019(3) 0.007(2) 0.003(2) 0.001(2) C13 0.016(3) 0.027(3) 0.022(3) 0.008(3) 0.001(2) -0.002(2) C14 0.014(3) 0.023(3) 0.025(3) 0.008(3) 0.000(2) -0.006(2) C15 0.018(3) 0.027(3) 0.017(3) 0.005(3) 0.002(2) 0.000(3) C16 0.013(3) 0.026(3) 0.013(3) 0.010(2) 0.003(2) -0.001(2) C17 0.007(3) 0.018(3) 0.017(3) 0.005(2) 0.006(2) -0.001(2) C18 0.029(3) 0.019(3) 0.023(3) 0.003(3) -0.006(3) -0.006(3) C19 0.026(3) 0.025(3) 0.023(3) 0.009(3) -0.006(3) -0.009(3) C20 0.023(3) 0.017(3) 0.016(3) 0.007(2) 0.000(2) 0.006(2) C21 0.023(3) 0.014(3) 0.012(3) 0.005(2) -0.001(2) 0.003(2) C22 0.020(3) 0.020(3) 0.028(3) 0.016(3) 0.003(3) 0.000(2) C23 0.025(3) 0.023(3) 0.015(3) -0.001(3) 0.003(2) 0.004(3) C24 0.024(3) 0.023(3) 0.013(3) 0.008(2) 0.005(2) 0.000(3) C25 0.022(3) 0.017(3) 0.025(3) 0.013(3) 0.001(2) 0.003(2) C26 0.017(3) 0.021(3) 0.016(3) 0.006(2) 0.000(2) 0.003(2) C27 0.033(3) 0.016(3) 0.012(3) 0.004(2) 0.005(2) 0.001(3) C28 0.024(3) 0.034(4) 0.033(4) 0.014(3) 0.001(3) 0.009(3) C29 0.019(3) 0.013(3) 0.034(4) 0.012(3) 0.005(3) -0.001(2) C30 0.012(3) 0.013(3) 0.030(3) 0.008(3) 0.005(2) -0.005(2) C31 0.020(3) 0.009(3) 0.021(3) 0.001(2) -0.002(2) -0.006(2) C32 0.025(3) 0.017(3) 0.010(3) -0.002(2) 0.004(2) 0.000(2) C33 0.021(3) 0.019(3) 0.014(3) 0.004(2) 0.000(2) 0.001(2) C34 0.012(3) 0.020(3) 0.020(3) 0.012(3) -0.001(2) -0.003(2) C35 0.012(3) 0.013(3) 0.013(3) 0.003(2) 0.000(2) -0.003(2) C36 0.035(4) 0.025(3) 0.013(3) 0.012(3) 0.006(3) 0.001(3) C37 0.042(4) 0.015(3) 0.030(4) 0.008(3) -0.010(3) -0.005(3) C38 0.016(3) 0.018(3) 0.018(3) 0.004(2) 0.001(2) -0.004(2) C39 0.017(3) 0.016(3) 0.019(3) 0.007(2) 0.004(2) 0.001(2) C40 0.024(3) 0.022(3) 0.024(3) 0.009(3) 0.003(3) -0.004(3) C41 0.019(3) 0.025(3) 0.022(3) 0.010(3) 0.003(2) 0.000(3) C42 0.025(3) 0.019(3) 0.022(3) 0.008(3) 0.002(3) 0.000(3) C43 0.023(3) 0.016(3) 0.016(3) 0.006(2) 0.007(2) 0.002(2) C44 0.019(3) 0.019(3) 0.011(3) 0.006(2) -0.003(2) 0.003(2) C45 0.025(3) 0.019(3) 0.030(3) 0.016(3) 0.004(3) 0.003(3) C46 0.023(3) 0.022(3) 0.023(3) 0.007(3) 0.006(3) -0.006(3) C47 0.015(3) 0.020(3) 0.024(3) 0.008(3) 0.005(2) -0.002(2) C48 0.021(3) 0.016(3) 0.023(3) 0.008(3) 0.004(2) 0.007(2) C49 0.023(3) 0.018(3) 0.018(3) 0.008(3) 0.002(2) 0.001(2) C50 0.028(3) 0.022(3) 0.015(3) 0.003(3) -0.004(2) -0.005(3) C51 0.022(3) 0.015(3) 0.025(3) 0.004(3) 0.001(3) -0.005(2) C52 0.016(3) 0.016(3) 0.015(3) 0.004(2) 0.002(2) 0.003(2) C53 0.011(3) 0.014(3) 0.020(3) 0.009(2) 0.007(2) 0.000(2) C54 0.020(3) 0.015(3) 0.022(3) 0.002(2) -0.003(2) -0.010(2) C1A 0.0201(10) 0.0185(10) 0.0179(10) 0.0081(8) 0.0006(8) -0.0003(8) C1S 0.033(4) 0.030(4) 0.017(3) 0.008(3) -0.001(3) -0.003(3) C2S 0.025(3) 0.029(4) 0.029(4) 0.011(3) 0.003(3) 0.001(3) C3S 0.050(2) 0.046(2) 0.047(2) 0.0169(12) 0.0065(10) -0.0012(10) _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 O7 2.371(4) . ? Tb1 O11 2.380(4) . ? Tb1 O9 2.386(4) . ? Tb1 O1 2.388(4) . ? Tb1 O5 2.415(4) . ? Tb1 O3 2.416(4) . ? Tb1 O8 2.764(4) . ? Tb1 O2 2.871(4) . ? Tb1 O4 2.885(4) . ? Tb1 O10 2.901(4) . ? Tb1 O6 2.920(4) . ? Tb1 Zn2 3.3084(10) . ? Zn2 O7 2.065(4) . ? Zn2 O9 2.118(4) . ? Zn2 N12 2.125(5) . ? Zn2 N10 2.134(5) . ? Zn2 O11 2.137(4) . ? Zn2 N8 2.188(5) . ? Zn1 O3 2.084(4) . ? Zn1 O5 2.087(4) . ? Zn1 O1 2.093(4) . ? Zn1 N2 2.129(5) . ? Zn1 N6 2.134(5) . ? Zn1 N4 2.141(5) . ? Cl2 C1S 1.764(7) . ? Cl3 C1S 1.772(7) . ? Cl4 C1S 1.769(7) . ? Cl5 C2S 1.749(7) . ? Cl6 C2S 1.780(7) . ? Cl7 C2S 1.762(7) . ? P1 N5 1.666(5) . ? P1 N1 1.669(5) . ? P1 N3 1.683(5) . ? P1 S1 1.931(2) . ? P2 N7 1.669(5) . ? P2 N11 1.671(5) . ? P2 N9 1.675(5) . ? P2 S2 1.925(2) . ? O1 C8 1.309(7) . ? O2 C7 1.372(7) . ? O2 C9 1.427(6) . ? O3 C17 1.315(7) . ? O4 C16 1.388(7) . ? O4 C18 1.431(7) . ? O5 C26 1.316(7) . ? O6 C25 1.385(7) . ? O6 C27 1.428(7) . ? O7 C35 1.331(7) . ? O8 C34 1.374(7) . ? O8 C36 1.427(7) . ? O9 C44 1.318(7) . ? O10 C43 1.387(7) . ? O10 C45 1.429(7) . ? O11 C53 1.329(7) . ? O12 C52 1.371(7) . ? O12 C54 1.438(7) . ? O1S C3S 1.412(7) . ? N1 N2 1.437(7) . ? N1 C1A 1.481(7) . ? N2 C2 1.289(8) . ? N3 N4 1.453(7) . ? N3 C10 1.463(8) . ? N4 C11 1.297(8) . ? N5 N6 1.455(6) . ? N5 C19 1.483(8) . ? N6 C20 1.284(7) . ? N7 N8 1.414(6) . ? N7 C28 1.448(8) . ? N8 C29 1.290(8) . ? N9 N10 1.447(7) . ? N9 C37 1.473(8) . ? N10 C38 1.289(7) . ? N11 N12 1.438(6) . ? N11 C46 1.469(7) . ? N12 C47 1.296(8) . ? C2 C3 1.443(8) . ? C3 C4 1.401(8) . ? C3 C8 1.421(8) . ? C4 C5 1.367(9) . ? C5 C6 1.415(8) . ? C6 C7 1.365(8) . ? C7 C8 1.431(8) . ? C11 C12 1.432(8) . ? C12 C17 1.416(8) . ? C12 C13 1.419(8) . ? C13 C14 1.369(9) . ? C14 C15 1.406(9) . ? C15 C16 1.361(8) . ? C16 C17 1.432(8) . ? C20 C21 1.454(8) . ? C21 C22 1.395(8) . ? C21 C26 1.418(8) . ? C22 C23 1.363(8) . ? C23 C24 1.406(9) . ? C24 C25 1.371(8) . ? C25 C26 1.410(8) . ? C29 C30 1.460(8) . ? C30 C35 1.399(8) . ? C30 C31 1.400(8) . ? C31 C32 1.366(8) . ? C32 C33 1.396(8) . ? C33 C34 1.381(8) . ? C34 C35 1.413(8) . ? C38 C39 1.436(8) . ? C39 C40 1.397(8) . ? C39 C44 1.428(8) . ? C40 C41 1.383(9) . ? C41 C42 1.406(8) . ? C42 C43 1.364(8) . ? C43 C44 1.421(8) . ? C47 C48 1.451(8) . ? C48 C49 1.389(8) . ? C48 C53 1.413(8) . ? C49 C50 1.363(8) . ? C50 C51 1.398(8) . ? C51 C52 1.363(8) . ? C52 C53 1.440(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Tb1 O11 66.86(13) . . ? O7 Tb1 O9 65.05(13) . . ? O11 Tb1 O9 68.07(13) . . ? O7 Tb1 O1 114.29(13) . . ? O11 Tb1 O1 113.85(13) . . ? O9 Tb1 O1 177.72(14) . . ? O7 Tb1 O5 175.73(13) . . ? O11 Tb1 O5 108.92(13) . . ? O9 Tb1 O5 114.47(13) . . ? O1 Tb1 O5 66.36(13) . . ? O7 Tb1 O3 119.01(13) . . ? O11 Tb1 O3 173.98(13) . . ? O9 Tb1 O3 112.44(13) . . ? O1 Tb1 O3 65.80(13) . . ? O5 Tb1 O3 65.23(13) . . ? O7 Tb1 O8 60.31(12) . . ? O11 Tb1 O8 117.25(13) . . ? O9 Tb1 O8 113.04(13) . . ? O1 Tb1 O8 65.12(13) . . ? O5 Tb1 O8 122.70(12) . . ? O3 Tb1 O8 68.37(12) . . ? O7 Tb1 O2 65.82(12) . . ? O11 Tb1 O2 65.23(12) . . ? O9 Tb1 O2 121.74(12) . . ? O1 Tb1 O2 59.02(12) . . ? O5 Tb1 O2 112.19(12) . . ? O3 Tb1 O2 117.65(12) . . ? O8 Tb1 O2 63.98(12) . . ? O7 Tb1 O4 68.50(12) . . ? O11 Tb1 O4 125.74(12) . . ? O9 Tb1 O4 66.13(12) . . ? O1 Tb1 O4 111.59(12) . . ? O5 Tb1 O4 115.43(12) . . ? O3 Tb1 O4 58.27(12) . . ? O8 Tb1 O4 60.09(12) . . ? O2 Tb1 O4 119.75(12) . . ? O7 Tb1 O10 115.93(13) . . ? O11 Tb1 O10 113.61(12) . . ? O9 Tb1 O10 58.78(12) . . ? O1 Tb1 O10 120.57(12) . . ? O5 Tb1 O10 65.94(12) . . ? O3 Tb1 O10 63.29(12) . . ? O8 Tb1 O10 118.25(12) . . ? O2 Tb1 O10 177.56(12) . . ? O4 Tb1 O10 62.68(12) . . ? O7 Tb1 O6 119.23(12) . . ? O11 Tb1 O6 63.57(13) . . ? O9 Tb1 O6 65.38(13) . . ? O1 Tb1 O6 116.43(13) . . ? O5 Tb1 O6 57.88(12) . . ? O3 Tb1 O6 110.89(12) . . ? O8 Tb1 O6 178.00(12) . . ? O2 Tb1 O6 117.79(12) . . ? O4 Tb1 O6 117.91(12) . . ? O10 Tb1 O6 60.00(12) . . ? O7 Tb1 Zn2 38.35(9) . . ? O11 Tb1 Zn2 40.11(9) . . ? O9 Tb1 Zn2 39.68(9) . . ? O1 Tb1 Zn2 141.10(9) . . ? O5 Tb1 Zn2 138.58(9) . . ? O3 Tb1 Zn2 143.69(9) . . ? O8 Tb1 Zn2 98.65(8) . . ? O2 Tb1 Zn2 82.09(8) . . ? O4 Tb1 Zn2 85.64(8) . . ? O10 Tb1 Zn2 98.33(8) . . ? O6 Tb1 Zn2 80.88(8) . . ? O7 Zn2 O9 75.36(15) . . ? O7 Zn2 N12 148.82(17) . . ? O9 Zn2 N12 123.72(17) . . ? O7 Zn2 N10 123.60(17) . . ? O9 Zn2 N10 82.77(17) . . ? N12 Zn2 N10 85.55(19) . . ? O7 Zn2 O11 77.04(15) . . ? O9 Zn2 O11 77.63(15) . . ? N12 Zn2 O11 83.26(17) . . ? N10 Zn2 O11 146.61(18) . . ? O7 Zn2 N8 84.60(16) . . ? O9 Zn2 N8 146.67(17) . . ? N12 Zn2 N8 86.62(18) . . ? N10 Zn2 N8 86.69(18) . . ? O11 Zn2 N8 123.76(17) . . ? O7 Zn2 Tb1 45.43(11) . . ? O9 Zn2 Tb1 45.97(10) . . ? N12 Zn2 Tb1 127.48(14) . . ? N10 Zn2 Tb1 127.69(13) . . ? O11 Zn2 Tb1 45.86(10) . . ? N8 Zn2 Tb1 128.37(13) . . ? O3 Zn1 O5 77.26(15) . . ? O3 Zn1 O1 77.32(15) . . ? O5 Zn1 O1 77.93(15) . . ? O3 Zn1 N2 122.21(17) . . ? O5 Zn1 N2 149.13(17) . . ? O1 Zn1 N2 83.31(17) . . ? O3 Zn1 N6 148.56(17) . . ? O5 Zn1 N6 83.87(17) . . ? O1 Zn1 N6 123.10(17) . . ? N2 Zn1 N6 86.18(19) . . ? O3 Zn1 N4 84.09(17) . . ? O5 Zn1 N4 121.34(17) . . ? O1 Zn1 N4 149.52(18) . . ? N2 Zn1 N4 86.54(18) . . ? N6 Zn1 N4 84.60(19) . . ? O3 Zn1 Tb1 46.55(10) . . ? O5 Zn1 Tb1 46.53(11) . . ? O1 Zn1 Tb1 45.79(10) . . ? N2 Zn1 Tb1 127.40(13) . . ? N6 Zn1 Tb1 128.46(13) . . ? N4 Zn1 Tb1 128.75(13) . . ? N5 P1 N1 106.4(3) . . ? N5 P1 N3 105.4(2) . . ? N1 P1 N3 106.6(3) . . ? N5 P1 S1 112.89(19) . . ? N1 P1 S1 112.64(19) . . ? N3 P1 S1 112.42(18) . . ? N7 P2 N11 105.1(3) . . ? N7 P2 N9 108.0(3) . . ? N11 P2 N9 104.0(3) . . ? N7 P2 S2 113.24(18) . . ? N11 P2 S2 113.57(19) . . ? N9 P2 S2 112.19(19) . . ? C8 O1 Zn1 131.7(4) . . ? C8 O1 Tb1 132.9(4) . . ? Zn1 O1 Tb1 95.29(14) . . ? C7 O2 C9 116.4(4) . . ? C7 O2 Tb1 115.0(3) . . ? C9 O2 Tb1 128.5(3) . . ? C17 O3 Zn1 132.2(3) . . ? C17 O3 Tb1 133.1(3) . . ? Zn1 O3 Tb1 94.68(14) . . ? C16 O4 C18 116.3(4) . . ? C16 O4 Tb1 116.3(3) . . ? C18 O4 Tb1 127.3(3) . . ? C26 O5 Zn1 131.9(4) . . ? C26 O5 Tb1 133.5(3) . . ? Zn1 O5 Tb1 94.64(15) . . ? C25 O6 C27 116.3(4) . . ? C25 O6 Tb1 115.1(3) . . ? C27 O6 Tb1 128.5(3) . . ? C35 O7 Zn2 132.9(3) . . ? C35 O7 Tb1 129.5(3) . . ? Zn2 O7 Tb1 96.22(15) . . ? C34 O8 C36 115.3(4) . . ? C34 O8 Tb1 115.9(3) . . ? C36 O8 Tb1 128.5(3) . . ? C44 O9 Zn2 132.3(3) . . ? C44 O9 Tb1 133.2(3) . . ? Zn2 O9 Tb1 94.35(14) . . ? C43 O10 C45 115.7(4) . . ? C43 O10 Tb1 114.6(3) . . ? C45 O10 Tb1 129.2(3) . . ? C53 O11 Zn2 132.2(3) . . ? C53 O11 Tb1 132.7(3) . . ? Zn2 O11 Tb1 94.04(14) . . ? C52 O12 C54 115.4(5) . . ? N2 N1 C1A 113.0(4) . . ? N2 N1 P1 115.2(4) . . ? C1A N1 P1 119.8(4) . . ? C2 N2 N1 112.4(5) . . ? C2 N2 Zn1 128.6(4) . . ? N1 N2 Zn1 118.1(3) . . ? N4 N3 C10 114.2(4) . . ? N4 N3 P1 113.1(4) . . ? C10 N3 P1 119.0(4) . . ? C11 N4 N3 111.9(5) . . ? C11 N4 Zn1 127.7(4) . . ? N3 N4 Zn1 119.7(3) . . ? N6 N5 C19 112.6(4) . . ? N6 N5 P1 114.4(4) . . ? C19 N5 P1 120.6(4) . . ? C20 N6 N5 112.7(5) . . ? C20 N6 Zn1 127.3(4) . . ? N5 N6 Zn1 118.5(3) . . ? N8 N7 C28 120.8(5) . . ? N8 N7 P2 115.8(4) . . ? C28 N7 P2 123.2(4) . . ? C29 N8 N7 116.0(5) . . ? C29 N8 Zn2 127.7(4) . . ? N7 N8 Zn2 115.6(3) . . ? N10 N9 C37 113.8(5) . . ? N10 N9 P2 115.0(4) . . ? C37 N9 P2 119.5(4) . . ? C38 N10 N9 112.0(5) . . ? C38 N10 Zn2 129.6(4) . . ? N9 N10 Zn2 118.0(3) . . ? N12 N11 C46 114.2(5) . . ? N12 N11 P2 115.0(4) . . ? C46 N11 P2 120.3(4) . . ? C47 N12 N11 111.4(5) . . ? C47 N12 Zn2 130.4(4) . . ? N11 N12 Zn2 118.1(3) . . ? N2 C2 C3 126.6(5) . . ? C4 C3 C8 120.6(5) . . ? C4 C3 C2 117.1(5) . . ? C8 C3 C2 122.3(5) . . ? C5 C4 C3 120.9(6) . . ? C4 C5 C6 119.6(6) . . ? C7 C6 C5 120.4(5) . . ? C6 C7 O2 124.8(5) . . ? C6 C7 C8 121.5(5) . . ? O2 C7 C8 113.7(5) . . ? O1 C8 C3 124.0(5) . . ? O1 C8 C7 119.1(5) . . ? C3 C8 C7 116.8(5) . . ? N4 C11 C12 126.9(5) . . ? C17 C12 C13 119.3(5) . . ? C17 C12 C11 123.7(5) . . ? C13 C12 C11 117.0(5) . . ? C14 C13 C12 122.1(6) . . ? C13 C14 C15 118.6(6) . . ? C16 C15 C14 121.0(6) . . ? C15 C16 O4 126.0(5) . . ? C15 C16 C17 121.7(5) . . ? O4 C16 C17 112.4(5) . . ? O3 C17 C12 123.4(5) . . ? O3 C17 C16 119.5(5) . . ? C12 C17 C16 117.1(5) . . ? N6 C20 C21 127.0(5) . . ? C22 C21 C26 120.9(5) . . ? C22 C21 C20 116.7(5) . . ? C26 C21 C20 122.3(5) . . ? C23 C22 C21 121.0(6) . . ? C22 C23 C24 119.8(6) . . ? C25 C24 C23 119.4(5) . . ? C24 C25 O6 124.0(5) . . ? C24 C25 C26 122.8(5) . . ? O6 C25 C26 113.2(5) . . ? O5 C26 C25 120.1(5) . . ? O5 C26 C21 123.8(5) . . ? C25 C26 C21 116.1(5) . . ? N8 C29 C30 126.1(5) . . ? C35 C30 C31 119.8(5) . . ? C35 C30 C29 124.3(5) . . ? C31 C30 C29 115.8(5) . . ? C32 C31 C30 121.5(5) . . ? C31 C32 C33 119.9(5) . . ? C34 C33 C32 119.2(5) . . ? O8 C34 C33 124.4(5) . . ? O8 C34 C35 113.8(5) . . ? C33 C34 C35 121.8(5) . . ? O7 C35 C30 124.0(5) . . ? O7 C35 C34 118.4(5) . . ? C30 C35 C34 117.7(5) . . ? N10 C38 C39 126.7(5) . . ? C40 C39 C44 119.9(5) . . ? C40 C39 C38 116.9(5) . . ? C44 C39 C38 123.2(5) . . ? C41 C40 C39 121.7(6) . . ? C40 C41 C42 118.6(6) . . ? C43 C42 C41 120.9(6) . . ? C42 C43 O10 124.9(5) . . ? C42 C43 C44 122.0(5) . . ? O10 C43 C44 113.1(5) . . ? O9 C44 C43 120.2(5) . . ? O9 C44 C39 123.0(5) . . ? C43 C44 C39 116.7(5) . . ? N12 C47 C48 127.2(6) . . ? C49 C48 C53 121.1(6) . . ? C49 C48 C47 116.4(5) . . ? C53 C48 C47 122.5(6) . . ? C50 C49 C48 121.3(6) . . ? C49 C50 C51 119.5(6) . . ? C52 C51 C50 120.7(6) . . ? C51 C52 O12 125.6(5) . . ? C51 C52 C53 121.4(5) . . ? O12 C52 C53 113.0(5) . . ? O11 C53 C48 124.2(5) . . ? O11 C53 C52 119.7(5) . . ? C48 C53 C52 116.1(5) . . ? Cl2 C1S Cl4 111.1(4) . . ? Cl2 C1S Cl3 109.7(4) . . ? Cl4 C1S Cl3 109.4(4) . . ? Cl5 C2S Cl7 110.7(4) . . ? Cl5 C2S Cl6 110.6(4) . . ? Cl7 C2S Cl6 108.9(4) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 2.737 _refine_diff_density_min -1.214 _refine_diff_density_rms 0.162 _database_code_depnum_ccdc_archive 'CCDC 941522' ####################################################################### # # 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_Zn2Nd _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H66 Cl7 N12 Nd O13 P2 S2 Zn2' _chemical_formula_weight 1776.41 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.944(5) _cell_length_b 16.435(5) _cell_length_c 19.025(5) _cell_angle_alpha 69.237(5) _cell_angle_beta 88.533(5) _cell_angle_gamma 89.435(5) _cell_volume 3491(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.095 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1794 _exptl_absorpt_coefficient_mu 1.857 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.729207 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19092 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0711 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.50 _reflns_number_total 12781 _reflns_number_gt 9001 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0941P)^2^+1.9902P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12781 _refine_ls_number_parameters 879 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0859 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1829 _refine_ls_wR_factor_gt 0.1498 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.26487(3) 0.25503(2) 0.244536(18) 0.01705(12) Uani 1 1 d . . . Zn1 Zn 0.23022(6) 0.09044(4) 0.17965(4) 0.01589(18) Uani 1 1 d . . . Zn2 Zn 0.29406(6) 0.41410(4) 0.31601(4) 0.01631(18) Uani 1 1 d . . . Cl1 Cl 0.82749(17) 0.69932(13) 0.32127(11) 0.0385(5) Uani 1 1 d . . . Cl2 Cl 0.6993(2) 0.94913(19) 0.19911(14) 0.0703(7) Uani 1 1 d . . . Cl3 Cl 0.7872(2) 0.95416(16) 0.33706(14) 0.0591(6) Uani 1 1 d . . . Cl4 Cl 0.5771(2) 0.86620(18) 0.34075(14) 0.0627(7) Uani 1 1 d . . . Cl5 Cl 0.6533(2) 0.72512(16) 0.11187(13) 0.0567(6) Uani 1 1 d . . . Cl6 Cl 0.8905(2) 0.6946(3) 0.12615(16) 0.0998(12) Uani 1 1 d . . . Cl7 Cl 0.7349(3) 0.54950(19) 0.18264(15) 0.0790(9) Uani 1 1 d . . . P1 P 0.19326(14) -0.07236(11) 0.11632(9) 0.0192(4) Uani 1 1 d . . . P2 P 0.32263(15) 0.56925(11) 0.38852(10) 0.0210(4) Uani 1 1 d . . . S1 S 0.17036(15) -0.16518(11) 0.07840(10) 0.0270(4) Uani 1 1 d . . . S2 S 0.33929(16) 0.65925(12) 0.43015(11) 0.0333(4) Uani 1 1 d . . . O1 O 0.3423(3) 0.1942(3) 0.1509(2) 0.0186(10) Uani 1 1 d . . . O2 O 0.4403(4) 0.3409(3) 0.1371(2) 0.0236(10) Uani 1 1 d . . . O3 O 0.1277(3) 0.1924(3) 0.1848(2) 0.0174(9) Uani 1 1 d . . . O4 O 0.0395(4) 0.3195(3) 0.2209(2) 0.0199(10) Uani 1 1 d . . . O5 O 0.2688(4) 0.0944(3) 0.2845(2) 0.0197(10) Uani 1 1 d . . . O6 O 0.3254(4) 0.1459(3) 0.3939(2) 0.0201(10) Uani 1 1 d . . . O7 O 0.4044(3) 0.3223(3) 0.2976(2) 0.0181(9) Uani 1 1 d . . . O8 O 0.4879(4) 0.1874(3) 0.2711(2) 0.0205(10) Uani 1 1 d . . . O9 O 0.1904(3) 0.3020(3) 0.3456(2) 0.0176(9) Uani 1 1 d . . . O10 O 0.0841(4) 0.1618(3) 0.3458(2) 0.0213(10) Uani 1 1 d . . . O11 O 0.2520(4) 0.4133(3) 0.2113(2) 0.0204(10) Uani 1 1 d . . . O12 O 0.2125(4) 0.3624(3) 0.0996(2) 0.0227(10) Uani 1 1 d . . . O1S O 0.9122(8) 0.4655(6) 0.4199(6) 0.120(3) Uani 1 1 d D . . H1S H 0.9295 0.4163 0.4221 0.180 Uiso 1 1 calc R . . N1 N 0.3286(5) -0.0461(4) 0.1145(3) 0.0272(13) Uani 1 1 d . . . N2 N 0.3470(5) 0.0405(4) 0.1162(3) 0.0263(13) Uani 1 1 d . . . N3 N 0.1266(5) 0.0179(4) 0.0665(3) 0.0266(13) Uani 1 1 d . . . N4 N 0.1070(5) 0.0792(3) 0.1063(3) 0.0214(12) Uani 1 1 d . . . N5 N 0.1493(5) -0.0983(3) 0.2060(3) 0.0231(12) Uani 1 1 d . . . N6 N 0.1969(5) -0.0437(3) 0.2431(3) 0.0254(13) Uani 1 1 d . . . N7 N 0.2930(4) 0.4714(4) 0.4538(3) 0.0220(12) Uani 1 1 d . . . N8 N 0.2415(4) 0.4106(3) 0.4256(3) 0.0206(12) Uani 1 1 d . . . N9 N 0.2177(5) 0.5885(3) 0.3277(3) 0.0246(13) Uani 1 1 d . . . N10 N 0.2282(5) 0.5470(3) 0.2740(3) 0.0225(12) Uani 1 1 d . . . N11 N 0.4401(5) 0.5528(3) 0.3462(3) 0.0231(12) Uani 1 1 d . . . N12 N 0.4458(4) 0.4694(3) 0.3359(3) 0.0202(12) Uani 1 1 d . . . C1 C 0.4079(6) -0.1118(5) 0.1598(4) 0.0338(18) Uani 1 1 d . . . H1A H 0.4823 -0.0974 0.1390 0.051 Uiso 1 1 calc R . . H1B H 0.3877 -0.1680 0.1593 0.051 Uiso 1 1 calc R . . H1C H 0.4054 -0.1129 0.2106 0.051 Uiso 1 1 calc R . . C2 C 0.4266(6) 0.0809(5) 0.0721(4) 0.0270(16) Uani 1 1 d . . . H2 H 0.4619 0.0516 0.0438 0.032 Uiso 1 1 calc R . . C3 C 0.4679(6) 0.1666(5) 0.0611(4) 0.0246(15) Uani 1 1 d . . . C4 C 0.5561(6) 0.1989(5) 0.0071(4) 0.0278(16) Uani 1 1 d . . . H4 H 0.5840 0.1650 -0.0195 0.033 Uiso 1 1 calc R . . C5 C 0.5998(6) 0.2781(5) -0.0059(4) 0.0300(17) Uani 1 1 d . . . H5 H 0.6559 0.2991 -0.0425 0.036 Uiso 1 1 calc R . . C6 C 0.5619(5) 0.3295(4) 0.0352(4) 0.0240(15) Uani 1 1 d . . . H6 H 0.5932 0.3841 0.0256 0.029 Uiso 1 1 calc R . . C7 C 0.4789(5) 0.2997(4) 0.0894(4) 0.0215(14) Uani 1 1 d . . . C8 C 0.4255(5) 0.2179(4) 0.1020(3) 0.0207(14) Uani 1 1 d . . . C9 C 0.4913(6) 0.4222(4) 0.1279(4) 0.0264(16) Uani 1 1 d . . . H9A H 0.5706 0.4143 0.1344 0.040 Uiso 1 1 calc R . . H9B H 0.4605 0.4442 0.1648 0.040 Uiso 1 1 calc R . . H9C H 0.4772 0.4630 0.0785 0.040 Uiso 1 1 calc R . . C10 C 0.0035(6) 0.1082(4) 0.0991(4) 0.0255(15) Uani 1 1 d . . . H10 H -0.0443 0.0869 0.0718 0.031 Uiso 1 1 calc R . . C11 C -0.0417(5) 0.1695(4) 0.1296(4) 0.0216(15) Uani 1 1 d . . . C12 C -0.1568(5) 0.1894(4) 0.1187(4) 0.0226(15) Uani 1 1 d . . . H12 H -0.1997 0.1608 0.0946 0.027 Uiso 1 1 calc R . . C13 C -0.2054(5) 0.2499(4) 0.1432(3) 0.0215(14) Uani 1 1 d . . . H13 H -0.2817 0.2611 0.1367 0.026 Uiso 1 1 calc R . . C14 C -0.1429(5) 0.2953(4) 0.1779(4) 0.0219(15) Uani 1 1 d . . . H14 H -0.1773 0.3372 0.1934 0.026 Uiso 1 1 calc R . . C15 C -0.0292(5) 0.2783(4) 0.1894(3) 0.0177(13) Uani 1 1 d . . . C16 C 0.0228(5) 0.2126(4) 0.1679(3) 0.0160(13) Uani 1 1 d . . . C17 C -0.0102(6) 0.3867(4) 0.2437(4) 0.0241(15) Uani 1 1 d . . . H17A H -0.0329 0.4342 0.2000 0.036 Uiso 1 1 calc R . . H17B H 0.0436 0.4069 0.2704 0.036 Uiso 1 1 calc R . . H17C H -0.0743 0.3638 0.2759 0.036 Uiso 1 1 calc R . . C18 C 0.1511(6) 0.0627(5) -0.0147(4) 0.0295(17) Uani 1 1 d . . . H18A H 0.0876 0.0972 -0.0379 0.044 Uiso 1 1 calc R . . H18B H 0.1664 0.0203 -0.0378 0.044 Uiso 1 1 calc R . . H18C H 0.2151 0.0997 -0.0212 0.044 Uiso 1 1 calc R . . C19 C 0.0303(6) -0.1196(5) 0.2264(4) 0.0283(16) Uani 1 1 d . . . H19A H 0.0233 -0.1533 0.2790 0.042 Uiso 1 1 calc R . . H19B H 0.0023 -0.1525 0.1978 0.042 Uiso 1 1 calc R . . H19C H -0.0120 -0.0668 0.2155 0.042 Uiso 1 1 calc R . . C20 C 0.2335(6) -0.0891(4) 0.3097(4) 0.0231(15) Uani 1 1 d . . . H20 H 0.2296 -0.1493 0.3241 0.028 Uiso 1 1 calc R . . C21 C 0.2788(5) -0.0558(4) 0.3624(3) 0.0187(14) Uani 1 1 d . . . C22 C 0.3077(6) -0.1185(4) 0.4336(4) 0.0257(15) Uani 1 1 d . . . H22 H 0.3012 -0.1777 0.4421 0.031 Uiso 1 1 calc R . . C23 C 0.3443(6) -0.0918(5) 0.4885(4) 0.0276(16) Uani 1 1 d . . . H23 H 0.3657 -0.1328 0.5341 0.033 Uiso 1 1 calc R . . C24 C 0.3505(6) -0.0032(4) 0.4774(4) 0.0240(15) Uani 1 1 d . . . H24 H 0.3735 0.0140 0.5163 0.029 Uiso 1 1 calc R . . C25 C 0.3233(5) 0.0584(4) 0.4102(3) 0.0175(13) Uani 1 1 d . . . C26 C 0.2896(5) 0.0342(4) 0.3491(3) 0.0175(13) Uani 1 1 d . . . C27 C 0.3574(6) 0.1732(4) 0.4541(4) 0.0251(15) Uani 1 1 d . . . H27A H 0.3050 0.1507 0.4955 0.038 Uiso 1 1 calc R . . H27B H 0.3577 0.2356 0.4372 0.038 Uiso 1 1 calc R . . H27C H 0.4310 0.1515 0.4700 0.038 Uiso 1 1 calc R . . C28 C 0.4891(7) 0.6245(4) 0.2842(4) 0.0370(19) Uani 1 1 d . . . H28A H 0.5680 0.6148 0.2805 0.056 Uiso 1 1 calc R . . H28B H 0.4770 0.6779 0.2931 0.056 Uiso 1 1 calc R . . H28C H 0.4545 0.6282 0.2382 0.056 Uiso 1 1 calc R . . C29 C 0.5452(6) 0.4361(4) 0.3477(3) 0.0215(14) Uani 1 1 d . . . H29 H 0.5984 0.4670 0.3629 0.026 Uiso 1 1 calc R . . C30 C 0.5817(5) 0.3555(4) 0.3395(3) 0.0190(14) Uani 1 1 d . . . C31 C 0.6931(5) 0.3306(4) 0.3567(4) 0.0219(14) Uani 1 1 d . . . H31 H 0.7381 0.3643 0.3748 0.026 Uiso 1 1 calc R . . C32 C 0.7371(6) 0.2582(4) 0.3475(4) 0.0257(15) Uani 1 1 d . . . H32 H 0.8109 0.2421 0.3602 0.031 Uiso 1 1 calc R . . C33 C 0.6696(5) 0.2075(4) 0.3185(3) 0.0208(14) Uani 1 1 d . . . H33 H 0.6993 0.1584 0.3114 0.025 Uiso 1 1 calc R . . C34 C 0.5607(6) 0.2309(4) 0.3009(3) 0.0207(14) Uani 1 1 d . . . C35 C 0.5123(5) 0.3044(4) 0.3128(3) 0.0181(13) Uani 1 1 d . . . C36 C 0.5311(6) 0.1085(4) 0.2642(4) 0.0252(15) Uani 1 1 d . . . H36A H 0.5899 0.1223 0.2265 0.038 Uiso 1 1 calc R . . H36B H 0.4721 0.0786 0.2501 0.038 Uiso 1 1 calc R . . H36C H 0.5602 0.0718 0.3116 0.038 Uiso 1 1 calc R . . C37 C 0.3682(6) 0.4320(5) 0.5143(4) 0.0315(17) Uani 1 1 d . . . H37A H 0.3268 0.3953 0.5576 0.047 Uiso 1 1 calc R . . H37B H 0.4054 0.4767 0.5265 0.047 Uiso 1 1 calc R . . H37C H 0.4229 0.3979 0.4991 0.047 Uiso 1 1 calc R . . C38 C 0.1739(5) 0.3590(4) 0.4740(3) 0.0211(14) Uani 1 1 d . . . H38 H 0.1629 0.3689 0.5189 0.025 Uiso 1 1 calc R . . C39 C 0.1130(5) 0.2878(4) 0.4666(4) 0.0190(14) Uani 1 1 d . . . C40 C 0.0416(6) 0.2412(5) 0.5280(4) 0.0300(17) Uani 1 1 d . . . H40 H 0.0351 0.2592 0.5691 0.036 Uiso 1 1 calc R . . C41 C -0.0183(6) 0.1704(5) 0.5284(4) 0.0274(16) Uani 1 1 d . . . H41 H -0.0658 0.1411 0.5688 0.033 Uiso 1 1 calc R . . C42 C -0.0067(6) 0.1431(4) 0.4668(4) 0.0238(15) Uani 1 1 d . . . H42 H -0.0467 0.0949 0.4666 0.029 Uiso 1 1 calc R . . C43 C 0.0618(6) 0.1854(4) 0.4075(4) 0.0202(14) Uani 1 1 d . . . C44 C 0.1251(5) 0.2615(4) 0.4046(3) 0.0185(14) Uani 1 1 d . . . C45 C 0.0235(6) 0.0861(4) 0.3461(4) 0.0266(16) Uani 1 1 d . . . H45A H 0.0449 0.0366 0.3886 0.040 Uiso 1 1 calc R . . H45B H 0.0407 0.0753 0.3006 0.040 Uiso 1 1 calc R . . H45C H -0.0555 0.0961 0.3494 0.040 Uiso 1 1 calc R . . C46 C 0.1294(6) 0.6517(5) 0.3226(4) 0.0353(18) Uani 1 1 d . . . H46A H 0.1503 0.7068 0.2855 0.053 Uiso 1 1 calc R . . H46B H 0.1184 0.6581 0.3705 0.053 Uiso 1 1 calc R . . H46C H 0.0611 0.6320 0.3084 0.053 Uiso 1 1 calc R . . C47 C 0.1836(6) 0.5867(4) 0.2105(4) 0.0288(16) Uani 1 1 d . . . H47 H 0.1525 0.6410 0.2036 0.035 Uiso 1 1 calc R . . C48 C 0.1765(6) 0.5559(4) 0.1476(4) 0.0248(15) Uani 1 1 d . . . C49 C 0.1317(6) 0.6142(4) 0.0814(4) 0.0258(16) Uani 1 1 d . . . H49 H 0.1121 0.6701 0.0787 0.031 Uiso 1 1 calc R . . C50 C 0.1166(6) 0.5900(5) 0.0211(4) 0.0302(17) Uani 1 1 d . . . H50 H 0.0872 0.6297 -0.0225 0.036 Uiso 1 1 calc R . . C51 C 0.1442(6) 0.5070(4) 0.0235(4) 0.0249(15) Uani 1 1 d . . . H51 H 0.1340 0.4912 -0.0182 0.030 Uiso 1 1 calc R . . C52 C 0.1870(5) 0.4483(4) 0.0884(4) 0.0199(14) Uani 1 1 d . . . C53 C 0.2075(5) 0.4713(4) 0.1518(4) 0.0203(14) Uani 1 1 d . . . C54 C 0.1979(6) 0.3373(5) 0.0357(3) 0.0250(15) Uani 1 1 d . . . H54A H 0.1212 0.3461 0.0207 0.037 Uiso 1 1 calc R . . H54B H 0.2169 0.2769 0.0485 0.037 Uiso 1 1 calc R . . H54C H 0.2457 0.3719 -0.0050 0.037 Uiso 1 1 calc R . . C1S C 0.7120(7) 0.8905(6) 0.2979(5) 0.050(2) Uani 1 1 d . . . H1S1 H 0.7527 0.8361 0.3054 0.061 Uiso 1 1 calc R . . C2S C 0.7607(7) 0.6650(7) 0.1681(5) 0.057(3) Uani 1 1 d . . . H2S H 0.7580 0.6731 0.2167 0.068 Uiso 1 1 calc R . . C3S C 0.8387(10) 0.5027(5) 0.3602(6) 0.081(4) Uani 1 1 d D . . H3S1 H 0.7826 0.4609 0.3611 0.122 Uiso 1 1 calc R . . H3S2 H 0.8800 0.5195 0.3133 0.122 Uiso 1 1 calc R . . H3S3 H 0.8034 0.5530 0.3655 0.122 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0208(2) 0.0162(2) 0.0165(2) -0.00862(15) -0.00326(14) 0.00047(13) Zn1 0.0187(4) 0.0168(4) 0.0156(4) -0.0098(3) -0.0025(3) 0.0003(3) Zn2 0.0196(4) 0.0147(4) 0.0171(4) -0.0086(3) -0.0030(3) 0.0006(3) Cl1 0.0436(12) 0.0396(11) 0.0366(11) -0.0188(9) -0.0023(9) 0.0004(9) Cl2 0.0663(17) 0.089(2) 0.0513(15) -0.0194(14) -0.0044(13) -0.0073(14) Cl3 0.0493(14) 0.0658(16) 0.0706(17) -0.0341(14) -0.0068(12) -0.0028(12) Cl4 0.0469(14) 0.0770(18) 0.0620(16) -0.0220(14) 0.0019(12) -0.0066(12) Cl5 0.0513(14) 0.0622(15) 0.0480(13) -0.0093(12) 0.0022(11) 0.0030(11) Cl6 0.0397(15) 0.215(4) 0.0554(17) -0.061(2) 0.0067(12) -0.0112(19) Cl7 0.109(2) 0.0707(19) 0.0580(16) -0.0243(14) -0.0088(16) 0.0324(17) P1 0.0220(9) 0.0206(9) 0.0210(9) -0.0146(7) -0.0033(7) 0.0005(7) P2 0.0236(9) 0.0186(9) 0.0266(9) -0.0149(8) -0.0023(7) 0.0002(7) S1 0.0325(10) 0.0244(9) 0.0321(10) -0.0199(8) -0.0016(8) 0.0009(7) S2 0.0383(11) 0.0270(10) 0.0452(12) -0.0257(9) -0.0050(9) 0.0011(8) O1 0.016(2) 0.022(2) 0.020(2) -0.0102(19) -0.0046(18) 0.0009(18) O2 0.027(3) 0.018(2) 0.025(3) -0.007(2) 0.004(2) 0.0005(19) O3 0.020(2) 0.021(2) 0.014(2) -0.0091(19) -0.0052(18) 0.0028(18) O4 0.020(2) 0.023(2) 0.021(2) -0.012(2) -0.0049(19) 0.0026(18) O5 0.029(3) 0.015(2) 0.017(2) -0.0079(19) -0.0023(19) 0.0009(18) O6 0.034(3) 0.014(2) 0.017(2) -0.0110(19) -0.0052(19) 0.0004(19) O7 0.020(2) 0.017(2) 0.021(2) -0.0095(19) -0.0036(19) 0.0014(18) O8 0.020(2) 0.019(2) 0.026(2) -0.013(2) -0.0041(19) 0.0054(18) O9 0.020(2) 0.023(2) 0.012(2) -0.0084(19) -0.0013(18) -0.0018(18) O10 0.025(3) 0.024(2) 0.018(2) -0.011(2) 0.0012(19) -0.0075(19) O11 0.027(3) 0.019(2) 0.016(2) -0.0059(19) -0.0028(19) 0.0037(19) O12 0.029(3) 0.023(3) 0.019(2) -0.012(2) -0.005(2) 0.004(2) O1S 0.105(8) 0.076(6) 0.184(11) -0.053(7) -0.004(7) 0.002(6) N1 0.025(3) 0.030(3) 0.033(3) -0.020(3) -0.007(3) 0.004(2) N2 0.026(3) 0.028(3) 0.032(3) -0.020(3) -0.003(3) 0.000(3) N3 0.034(3) 0.026(3) 0.025(3) -0.015(3) 0.004(3) -0.001(3) N4 0.027(3) 0.020(3) 0.022(3) -0.013(2) -0.008(2) 0.002(2) N5 0.024(3) 0.022(3) 0.028(3) -0.014(3) -0.007(2) -0.001(2) N6 0.038(4) 0.017(3) 0.026(3) -0.014(3) 0.005(3) 0.001(2) N7 0.021(3) 0.027(3) 0.024(3) -0.016(3) 0.000(2) -0.005(2) N8 0.021(3) 0.020(3) 0.025(3) -0.013(2) -0.004(2) -0.001(2) N9 0.028(3) 0.019(3) 0.030(3) -0.014(3) -0.002(3) 0.006(2) N10 0.022(3) 0.021(3) 0.025(3) -0.009(3) -0.004(2) -0.002(2) N11 0.026(3) 0.016(3) 0.030(3) -0.011(2) 0.003(3) -0.004(2) N12 0.022(3) 0.020(3) 0.024(3) -0.015(2) -0.003(2) 0.001(2) C1 0.029(4) 0.034(4) 0.045(5) -0.022(4) -0.004(3) 0.006(3) C2 0.025(4) 0.036(4) 0.021(4) -0.011(3) 0.003(3) 0.003(3) C3 0.026(4) 0.033(4) 0.019(3) -0.013(3) 0.003(3) -0.003(3) C4 0.023(4) 0.039(4) 0.024(4) -0.015(3) -0.001(3) -0.003(3) C5 0.020(4) 0.041(4) 0.028(4) -0.011(3) 0.004(3) -0.002(3) C6 0.018(3) 0.028(4) 0.023(4) -0.004(3) -0.004(3) -0.005(3) C7 0.020(3) 0.025(4) 0.017(3) -0.005(3) -0.001(3) 0.001(3) C8 0.015(3) 0.027(4) 0.018(3) -0.005(3) 0.000(3) -0.002(3) C9 0.028(4) 0.019(4) 0.030(4) -0.007(3) -0.003(3) -0.005(3) C10 0.023(4) 0.027(4) 0.026(4) -0.008(3) -0.003(3) -0.003(3) C11 0.020(3) 0.025(4) 0.019(3) -0.008(3) -0.001(3) 0.005(3) C12 0.021(4) 0.026(4) 0.020(3) -0.007(3) -0.006(3) -0.006(3) C13 0.013(3) 0.030(4) 0.021(3) -0.007(3) -0.008(3) 0.001(3) C14 0.022(4) 0.021(4) 0.021(3) -0.006(3) 0.002(3) 0.007(3) C15 0.023(3) 0.016(3) 0.014(3) -0.005(3) -0.004(3) 0.000(3) C16 0.017(3) 0.020(3) 0.012(3) -0.007(3) -0.006(2) 0.003(2) C17 0.027(4) 0.020(4) 0.030(4) -0.014(3) -0.008(3) 0.005(3) C18 0.040(4) 0.032(4) 0.016(3) -0.008(3) 0.000(3) -0.002(3) C19 0.033(4) 0.026(4) 0.031(4) -0.017(3) 0.004(3) -0.004(3) C20 0.026(4) 0.019(3) 0.023(4) -0.007(3) -0.002(3) 0.001(3) C21 0.019(3) 0.023(4) 0.017(3) -0.011(3) -0.003(3) 0.004(3) C22 0.034(4) 0.013(3) 0.026(4) -0.002(3) -0.001(3) -0.005(3) C23 0.033(4) 0.027(4) 0.016(3) 0.001(3) -0.005(3) 0.004(3) C24 0.029(4) 0.027(4) 0.022(4) -0.016(3) -0.002(3) 0.004(3) C25 0.017(3) 0.020(3) 0.017(3) -0.007(3) -0.007(3) 0.005(3) C26 0.019(3) 0.021(3) 0.015(3) -0.010(3) -0.005(3) 0.002(3) C27 0.031(4) 0.023(4) 0.024(4) -0.012(3) -0.002(3) 0.002(3) C28 0.043(5) 0.018(4) 0.048(5) -0.010(4) 0.017(4) -0.009(3) C29 0.029(4) 0.022(4) 0.016(3) -0.010(3) -0.004(3) -0.003(3) C30 0.020(3) 0.021(3) 0.018(3) -0.009(3) -0.001(3) 0.003(3) C31 0.022(4) 0.025(4) 0.024(4) -0.016(3) -0.004(3) -0.005(3) C32 0.017(4) 0.032(4) 0.028(4) -0.011(3) -0.005(3) 0.002(3) C33 0.020(3) 0.024(4) 0.018(3) -0.007(3) -0.001(3) -0.002(3) C34 0.028(4) 0.023(4) 0.015(3) -0.011(3) -0.003(3) 0.002(3) C35 0.017(3) 0.021(3) 0.017(3) -0.008(3) 0.000(3) -0.002(3) C36 0.027(4) 0.020(4) 0.033(4) -0.015(3) -0.006(3) 0.007(3) C37 0.040(5) 0.032(4) 0.026(4) -0.014(3) -0.003(3) 0.001(3) C38 0.027(4) 0.023(4) 0.015(3) -0.009(3) -0.005(3) 0.006(3) C39 0.020(3) 0.017(3) 0.022(3) -0.010(3) 0.000(3) -0.001(3) C40 0.031(4) 0.041(4) 0.023(4) -0.019(3) 0.006(3) -0.002(3) C41 0.029(4) 0.033(4) 0.020(4) -0.009(3) 0.003(3) -0.011(3) C42 0.027(4) 0.021(4) 0.027(4) -0.012(3) -0.004(3) -0.007(3) C43 0.026(4) 0.022(4) 0.018(3) -0.013(3) -0.004(3) 0.003(3) C44 0.016(3) 0.020(3) 0.020(3) -0.007(3) -0.002(3) 0.002(3) C45 0.038(4) 0.024(4) 0.023(4) -0.015(3) 0.003(3) -0.006(3) C46 0.031(4) 0.045(5) 0.037(4) -0.022(4) -0.009(3) 0.013(4) C47 0.024(4) 0.019(4) 0.042(4) -0.010(3) -0.001(3) -0.003(3) C48 0.025(4) 0.020(4) 0.029(4) -0.009(3) 0.000(3) -0.005(3) C49 0.023(4) 0.018(3) 0.030(4) -0.001(3) -0.007(3) -0.001(3) C50 0.031(4) 0.029(4) 0.024(4) -0.001(3) -0.010(3) -0.004(3) C51 0.029(4) 0.024(4) 0.020(3) -0.006(3) -0.011(3) 0.001(3) C52 0.021(3) 0.023(4) 0.018(3) -0.009(3) -0.004(3) -0.004(3) C53 0.016(3) 0.021(3) 0.024(4) -0.008(3) 0.001(3) -0.006(3) C54 0.030(4) 0.035(4) 0.015(3) -0.016(3) -0.001(3) 0.001(3) C1S 0.050(6) 0.054(6) 0.049(5) -0.021(5) 0.005(4) 0.003(4) C2S 0.036(5) 0.101(8) 0.043(5) -0.038(5) -0.010(4) 0.013(5) C3S 0.149(11) 0.019(5) 0.072(7) -0.007(5) -0.080(8) 0.000(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O7 2.437(4) . ? Nd1 O3 2.448(4) . ? Nd1 O11 2.454(4) . ? Nd1 O9 2.457(4) . ? Nd1 O5 2.474(4) . ? Nd1 O1 2.488(4) . ? Nd1 O12 2.779(4) . ? Nd1 O8 2.863(4) . ? Nd1 O4 2.871(4) . ? Nd1 O6 2.878(4) . ? Nd1 O2 2.891(4) . ? Nd1 O10 2.911(4) . ? Zn1 O5 2.082(4) . ? Zn1 O1 2.085(4) . ? Zn1 O3 2.095(4) . ? Zn1 N4 2.108(5) . ? Zn1 N6 2.141(6) . ? Zn1 N2 2.161(5) . ? Zn2 O11 2.071(4) . ? Zn2 O7 2.109(4) . ? Zn2 O9 2.126(4) . ? Zn2 N12 2.136(5) . ? Zn2 N8 2.143(5) . ? Zn2 N10 2.189(5) . ? Cl2 C1S 1.792(9) . ? Cl3 C1S 1.750(9) . ? Cl4 C1S 1.771(9) . ? Cl5 C2S 1.751(9) . ? Cl6 C2S 1.719(9) . ? Cl7 C2S 1.846(11) . ? P1 N3 1.658(6) . ? P1 N1 1.673(6) . ? P1 N5 1.676(6) . ? P1 S1 1.929(2) . ? P2 N11 1.668(6) . ? P2 N9 1.678(6) . ? P2 N7 1.681(6) . ? P2 S2 1.924(2) . ? O1 C8 1.306(7) . ? O2 C7 1.379(8) . ? O2 C9 1.426(8) . ? O3 C16 1.312(7) . ? O4 C15 1.347(7) . ? O4 C17 1.440(7) . ? O5 C26 1.305(7) . ? O6 C25 1.360(7) . ? O6 C27 1.431(7) . ? O7 C35 1.335(7) . ? O8 C34 1.384(8) . ? O8 C36 1.439(7) . ? O9 C44 1.322(7) . ? O10 C43 1.381(7) . ? O10 C45 1.444(8) . ? O11 C53 1.314(8) . ? O12 C52 1.383(7) . ? O12 C54 1.432(7) . ? O1S C3S 1.409(8) . ? N1 N2 1.454(7) . ? N1 C1 1.472(9) . ? N2 C2 1.275(9) . ? N3 N4 1.474(7) . ? N3 C18 1.480(8) . ? N4 C10 1.312(8) . ? N5 N6 1.451(7) . ? N5 C19 1.476(9) . ? N6 C20 1.306(8) . ? N7 C37 1.437(9) . ? N7 N8 1.439(7) . ? N8 C38 1.281(8) . ? N9 N10 1.417(7) . ? N9 C46 1.455(8) . ? N10 C47 1.279(9) . ? N11 C28 1.453(9) . ? N11 N12 1.453(7) . ? N12 C29 1.293(8) . ? C2 C3 1.440(10) . ? C3 C8 1.418(9) . ? C3 C4 1.419(9) . ? C4 C5 1.344(10) . ? C5 C6 1.403(9) . ? C6 C7 1.374(9) . ? C7 C8 1.433(9) . ? C10 C11 1.426(9) . ? C11 C12 1.414(9) . ? C11 C16 1.424(9) . ? C12 C13 1.358(9) . ? C13 C14 1.391(9) . ? C14 C15 1.391(9) . ? C15 C16 1.417(8) . ? C20 C21 1.422(9) . ? C21 C26 1.417(9) . ? C21 C22 1.429(9) . ? C22 C23 1.352(9) . ? C23 C24 1.398(9) . ? C24 C25 1.364(9) . ? C25 C26 1.423(8) . ? C29 C30 1.449(8) . ? C30 C31 1.401(9) . ? C30 C35 1.409(9) . ? C31 C32 1.361(9) . ? C32 C33 1.419(9) . ? C33 C34 1.368(9) . ? C34 C35 1.422(8) . ? C38 C39 1.433(9) . ? C39 C44 1.397(9) . ? C39 C40 1.416(9) . ? C40 C41 1.369(10) . ? C41 C42 1.400(9) . ? C42 C43 1.354(9) . ? C43 C44 1.450(9) . ? C47 C48 1.460(10) . ? C48 C49 1.399(9) . ? C48 C53 1.411(9) . ? C49 C50 1.358(10) . ? C50 C51 1.385(10) . ? C51 C52 1.377(9) . ? C52 C53 1.412(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Nd1 O3 177.08(14) . . ? O7 Nd1 O11 63.41(14) . . ? O3 Nd1 O11 114.96(14) . . ? O7 Nd1 O9 66.32(14) . . ? O3 Nd1 O9 115.52(14) . . ? O11 Nd1 O9 65.36(14) . . ? O7 Nd1 O5 116.91(14) . . ? O3 Nd1 O5 64.89(14) . . ? O11 Nd1 O5 176.35(13) . . ? O9 Nd1 O5 111.23(14) . . ? O7 Nd1 O1 114.13(14) . . ? O3 Nd1 O1 64.26(14) . . ? O11 Nd1 O1 119.63(14) . . ? O9 Nd1 O1 174.86(13) . . ? O5 Nd1 O1 63.81(14) . . ? O7 Nd1 O12 111.09(14) . . ? O3 Nd1 O12 66.18(13) . . ? O11 Nd1 O12 59.18(13) . . ? O9 Nd1 O12 115.33(13) . . ? O5 Nd1 O12 122.80(13) . . ? O1 Nd1 O12 69.54(13) . . ? O7 Nd1 O8 58.71(13) . . ? O3 Nd1 O8 121.28(13) . . ? O11 Nd1 O8 114.19(14) . . ? O9 Nd1 O8 112.82(13) . . ? O5 Nd1 O8 68.01(14) . . ? O1 Nd1 O8 64.63(13) . . ? O12 Nd1 O8 118.20(13) . . ? O7 Nd1 O4 121.62(13) . . ? O3 Nd1 O4 58.46(13) . . ? O11 Nd1 O4 66.79(14) . . ? O9 Nd1 O4 66.62(13) . . ? O5 Nd1 O4 110.96(14) . . ? O1 Nd1 O4 115.83(12) . . ? O12 Nd1 O4 63.02(13) . . ? O8 Nd1 O4 178.67(12) . . ? O7 Nd1 O6 67.50(13) . . ? O3 Nd1 O6 115.21(13) . . ? O11 Nd1 O6 120.19(13) . . ? O9 Nd1 O6 65.04(13) . . ? O5 Nd1 O6 57.92(12) . . ? O1 Nd1 O6 110.14(13) . . ? O12 Nd1 O6 178.37(13) . . ? O8 Nd1 O6 60.47(13) . . ? O4 Nd1 O6 118.32(12) . . ? O7 Nd1 O2 67.41(14) . . ? O3 Nd1 O2 109.87(13) . . ? O11 Nd1 O2 69.65(13) . . ? O9 Nd1 O2 125.76(13) . . ? O5 Nd1 O2 113.94(13) . . ? O1 Nd1 O2 57.62(13) . . ? O12 Nd1 O2 59.55(13) . . ? O8 Nd1 O2 61.57(13) . . ? O4 Nd1 O2 119.76(12) . . ? O6 Nd1 O2 118.88(13) . . ? O7 Nd1 O10 116.48(13) . . ? O3 Nd1 O10 66.27(13) . . ? O11 Nd1 O10 112.87(13) . . ? O9 Nd1 O10 58.18(13) . . ? O5 Nd1 O10 63.59(13) . . ? O1 Nd1 O10 118.54(13) . . ? O12 Nd1 O10 118.55(13) . . ? O8 Nd1 O10 118.85(13) . . ? O4 Nd1 O10 59.82(13) . . ? O6 Nd1 O10 63.05(13) . . ? O2 Nd1 O10 175.91(11) . . ? O5 Zn1 O1 78.02(16) . . ? O5 Zn1 O3 78.43(16) . . ? O1 Zn1 O3 77.83(16) . . ? O5 Zn1 N4 148.2(2) . . ? O1 Zn1 N4 122.87(19) . . ? O3 Zn1 N4 83.01(18) . . ? O5 Zn1 N6 83.16(19) . . ? O1 Zn1 N6 148.0(2) . . ? O3 Zn1 N6 123.40(19) . . ? N4 Zn1 N6 85.9(2) . . ? O5 Zn1 N2 121.82(19) . . ? O1 Zn1 N2 83.50(19) . . ? O3 Zn1 N2 148.84(19) . . ? N4 Zn1 N2 86.6(2) . . ? N6 Zn1 N2 84.8(2) . . ? O5 Zn1 Nd1 46.78(11) . . ? O1 Zn1 Nd1 47.17(11) . . ? O3 Zn1 Nd1 46.07(11) . . ? N4 Zn1 Nd1 127.65(14) . . ? N6 Zn1 Nd1 128.11(15) . . ? N2 Zn1 Nd1 128.88(15) . . ? O11 Zn2 O7 75.90(16) . . ? O11 Zn2 O9 78.37(16) . . ? O7 Zn2 O9 78.40(16) . . ? O11 Zn2 N12 123.16(19) . . ? O7 Zn2 N12 82.95(18) . . ? O9 Zn2 N12 146.83(18) . . ? O11 Zn2 N8 148.90(19) . . ? O7 Zn2 N8 123.46(18) . . ? O9 Zn2 N8 82.17(18) . . ? N12 Zn2 N8 85.7(2) . . ? O11 Zn2 N10 84.16(18) . . ? O7 Zn2 N10 147.11(19) . . ? O9 Zn2 N10 123.10(19) . . ? N12 Zn2 N10 86.6(2) . . ? N8 Zn2 N10 86.5(2) . . ? O11 Zn2 Nd1 46.39(12) . . ? O7 Zn2 Nd1 46.00(11) . . ? O9 Zn2 Nd1 46.59(11) . . ? N12 Zn2 Nd1 127.92(13) . . ? N8 Zn2 Nd1 127.01(14) . . ? N10 Zn2 Nd1 128.70(14) . . ? N3 P1 N1 106.7(3) . . ? N3 P1 N5 107.1(3) . . ? N1 P1 N5 105.8(3) . . ? N3 P1 S1 112.0(2) . . ? N1 P1 S1 112.2(2) . . ? N5 P1 S1 112.6(2) . . ? N11 P2 N9 108.7(3) . . ? N11 P2 N7 104.3(3) . . ? N9 P2 N7 104.6(3) . . ? N11 P2 S2 112.2(2) . . ? N9 P2 S2 113.1(2) . . ? N7 P2 S2 113.2(2) . . ? C8 O1 Zn1 132.6(4) . . ? C8 O1 Nd1 132.5(4) . . ? Zn1 O1 Nd1 94.91(16) . . ? C7 O2 C9 116.2(5) . . ? C7 O2 Nd1 117.2(4) . . ? C9 O2 Nd1 126.6(4) . . ? C16 O3 Zn1 132.6(4) . . ? C16 O3 Nd1 131.3(4) . . ? Zn1 O3 Nd1 95.88(16) . . ? C15 O4 C17 116.5(5) . . ? C15 O4 Nd1 116.1(3) . . ? C17 O4 Nd1 127.2(4) . . ? C26 O5 Zn1 133.0(4) . . ? C26 O5 Nd1 131.5(4) . . ? Zn1 O5 Nd1 95.41(16) . . ? C25 O6 C27 115.5(5) . . ? C25 O6 Nd1 117.2(3) . . ? C27 O6 Nd1 127.3(3) . . ? C35 O7 Zn2 132.4(4) . . ? C35 O7 Nd1 132.1(4) . . ? Zn2 O7 Nd1 95.50(16) . . ? C34 O8 C36 115.2(5) . . ? C34 O8 Nd1 116.6(3) . . ? C36 O8 Nd1 127.9(4) . . ? C44 O9 Zn2 133.5(4) . . ? C44 O9 Nd1 131.0(4) . . ? Zn2 O9 Nd1 94.46(15) . . ? C43 O10 C45 114.3(5) . . ? C43 O10 Nd1 116.4(4) . . ? C45 O10 Nd1 128.8(4) . . ? C53 O11 Zn2 133.7(4) . . ? C53 O11 Nd1 128.7(4) . . ? Zn2 O11 Nd1 95.96(16) . . ? C52 O12 C54 115.1(5) . . ? C52 O12 Nd1 117.4(3) . . ? C54 O12 Nd1 127.2(4) . . ? N2 N1 C1 113.7(5) . . ? N2 N1 P1 113.8(4) . . ? C1 N1 P1 119.2(5) . . ? C2 N2 N1 112.9(5) . . ? C2 N2 Zn1 128.0(5) . . ? N1 N2 Zn1 118.7(4) . . ? N4 N3 C18 112.5(5) . . ? N4 N3 P1 114.2(4) . . ? C18 N3 P1 121.7(4) . . ? C10 N4 N3 111.5(5) . . ? C10 N4 Zn1 129.0(4) . . ? N3 N4 Zn1 118.5(4) . . ? N6 N5 C19 113.3(5) . . ? N6 N5 P1 113.4(4) . . ? C19 N5 P1 119.7(4) . . ? C20 N6 N5 112.2(5) . . ? C20 N6 Zn1 127.1(5) . . ? N5 N6 Zn1 119.4(4) . . ? C37 N7 N8 114.0(5) . . ? C37 N7 P2 120.2(5) . . ? N8 N7 P2 115.0(4) . . ? C38 N8 N7 112.2(5) . . ? C38 N8 Zn2 130.3(4) . . ? N7 N8 Zn2 117.4(4) . . ? N10 N9 C46 120.9(5) . . ? N10 N9 P2 115.2(4) . . ? C46 N9 P2 123.4(5) . . ? C47 N10 N9 116.0(5) . . ? C47 N10 Zn2 127.6(5) . . ? N9 N10 Zn2 115.6(4) . . ? C28 N11 N12 114.3(5) . . ? C28 N11 P2 119.3(5) . . ? N12 N11 P2 114.5(4) . . ? C29 N12 N11 111.6(5) . . ? C29 N12 Zn2 129.6(4) . . ? N11 N12 Zn2 118.4(4) . . ? N2 C2 C3 127.3(6) . . ? C8 C3 C4 120.0(6) . . ? C8 C3 C2 123.0(6) . . ? C4 C3 C2 117.1(6) . . ? C5 C4 C3 120.6(6) . . ? C4 C5 C6 120.9(7) . . ? C7 C6 C5 120.4(7) . . ? C6 C7 O2 125.9(6) . . ? C6 C7 C8 120.5(6) . . ? O2 C7 C8 113.5(6) . . ? O1 C8 C3 123.8(6) . . ? O1 C8 C7 118.7(6) . . ? C3 C8 C7 117.4(6) . . ? N4 C10 C11 125.5(6) . . ? C12 C11 C10 116.9(6) . . ? C12 C11 C16 119.2(6) . . ? C10 C11 C16 123.8(6) . . ? C13 C12 C11 120.7(6) . . ? C12 C13 C14 121.0(6) . . ? C13 C14 C15 120.4(6) . . ? O4 C15 C14 125.3(6) . . ? O4 C15 C16 114.7(5) . . ? C14 C15 C16 120.0(6) . . ? O3 C16 C15 119.2(5) . . ? O3 C16 C11 122.2(5) . . ? C15 C16 C11 118.6(6) . . ? N6 C20 C21 126.6(6) . . ? C26 C21 C20 123.5(6) . . ? C26 C21 C22 120.1(6) . . ? C20 C21 C22 116.3(6) . . ? C23 C22 C21 119.9(6) . . ? C22 C23 C24 120.7(6) . . ? C25 C24 C23 120.9(6) . . ? O6 C25 C24 125.5(6) . . ? O6 C25 C26 113.6(5) . . ? C24 C25 C26 120.9(6) . . ? O5 C26 C21 122.9(5) . . ? O5 C26 C25 119.6(5) . . ? C21 C26 C25 117.4(6) . . ? N12 C29 C30 126.4(6) . . ? C31 C30 C35 119.8(6) . . ? C31 C30 C29 117.0(6) . . ? C35 C30 C29 123.2(6) . . ? C32 C31 C30 121.6(6) . . ? C31 C32 C33 119.5(6) . . ? C34 C33 C32 120.0(6) . . ? C33 C34 O8 125.0(6) . . ? C33 C34 C35 121.2(6) . . ? O8 C34 C35 113.8(6) . . ? O7 C35 C30 123.3(5) . . ? O7 C35 C34 118.8(6) . . ? C30 C35 C34 117.9(6) . . ? N8 C38 C39 127.3(6) . . ? C44 C39 C40 120.2(6) . . ? C44 C39 C38 123.3(6) . . ? C40 C39 C38 116.4(6) . . ? C41 C40 C39 121.8(6) . . ? C40 C41 C42 118.7(6) . . ? C43 C42 C41 121.2(6) . . ? C42 C43 O10 126.2(6) . . ? C42 C43 C44 121.6(6) . . ? O10 C43 C44 112.1(6) . . ? O9 C44 C39 123.3(6) . . ? O9 C44 C43 120.2(5) . . ? C39 C44 C43 116.5(6) . . ? N10 C47 C48 126.9(6) . . ? C49 C48 C53 120.0(6) . . ? C49 C48 C47 116.3(6) . . ? C53 C48 C47 123.6(6) . . ? C50 C49 C48 120.6(6) . . ? C49 C50 C51 121.1(6) . . ? C52 C51 C50 119.1(6) . . ? C51 C52 O12 125.0(6) . . ? C51 C52 C53 121.9(6) . . ? O12 C52 C53 113.1(5) . . ? O11 C53 C52 119.1(6) . . ? O11 C53 C48 123.7(6) . . ? C52 C53 C48 117.2(6) . . ? Cl3 C1S Cl4 110.6(5) . . ? Cl3 C1S Cl2 108.8(5) . . ? Cl4 C1S Cl2 109.7(5) . . ? Cl6 C2S Cl5 112.0(6) . . ? Cl6 C2S Cl7 109.3(5) . . ? Cl5 C2S Cl7 106.9(5) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.983 _refine_diff_density_min -1.357 _refine_diff_density_rms 0.188 _database_code_depnum_ccdc_archive 'CCDC 941523' ####################################################################### # # 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_Zn2Eu _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H66 Cl7 Eu N12 O13 P2 S2 Zn2' _chemical_formula_weight 1784.13 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.931(5) _cell_length_b 16.354(5) _cell_length_c 19.001(5) _cell_angle_alpha 69.881(5) _cell_angle_beta 88.344(5) _cell_angle_gamma 89.959(5) _cell_volume 3480(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4298 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 27.57 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.125 _exptl_crystal_size_min 0.105 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 2.018 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.605724 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19009 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0662 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 25.50 _reflns_number_total 12706 _reflns_number_gt 9443 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+12.1758P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12029 _refine_ls_number_parameters 873 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0716 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1393 _refine_ls_wR_factor_gt 0.1202 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.989 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.26516(2) 0.254326(19) 0.244152(16) 0.01654(10) Uani 1 1 d . . . Zn1 Zn 0.23056(5) 0.08936(4) 0.18103(3) 0.01410(16) Uani 1 1 d . . . Zn2 Zn 0.29498(5) 0.41306(4) 0.31471(3) 0.01483(16) Uani 1 1 d . . . Cl1 Cl 0.82834(14) 0.69497(11) 0.32501(9) 0.0303(4) Uani 1 1 d . . . Cl2 Cl 0.65259(14) 0.72807(12) 0.11158(10) 0.0383(4) Uani 1 1 d . . . Cl3 Cl 0.74543(19) 0.55694(14) 0.17881(11) 0.0519(5) Uani 1 1 d . . . Cl4 Cl 0.89291(16) 0.70886(16) 0.12368(11) 0.0531(6) Uani 1 1 d . . . Cl5 Cl 0.57548(15) 0.86382(14) 0.34088(11) 0.0455(5) Uani 1 1 d . . . Cl6 Cl 0.78603(15) 0.95261(13) 0.33854(11) 0.0433(5) Uani 1 1 d . . . Cl7 Cl 0.70233(17) 0.94302(16) 0.20099(11) 0.0542(6) Uani 1 1 d . . . P1 P 0.19281(12) -0.07494(10) 0.11756(8) 0.0165(3) Uani 1 1 d . . . P2 P 0.32430(12) 0.57029(10) 0.38662(9) 0.0176(3) Uani 1 1 d . . . S1 S 0.16943(13) -0.16859(10) 0.07976(9) 0.0229(3) Uani 1 1 d . . . S2 S 0.34181(14) 0.66183(11) 0.42762(10) 0.0277(4) Uani 1 1 d . . . N1 N 0.3289(4) -0.0474(3) 0.1160(3) 0.0215(11) Uani 1 1 d . . . N2 N 0.3475(4) 0.0390(3) 0.1177(3) 0.0223(11) Uani 1 1 d . . . N3 N 0.1270(4) 0.0159(3) 0.0673(3) 0.0226(11) Uani 1 1 d . . . N4 N 0.1066(4) 0.0767(3) 0.1068(3) 0.0209(11) Uani 1 1 d . . . N5 N 0.1483(4) -0.0992(3) 0.2067(3) 0.0201(11) Uani 1 1 d . . . N6 N 0.1968(4) -0.0443(3) 0.2439(3) 0.0196(11) Uani 1 1 d . . . N7 N 0.4418(4) 0.5533(3) 0.3438(3) 0.0207(11) Uani 1 1 d . . . N8 N 0.4474(4) 0.4692(3) 0.3335(3) 0.0182(11) Uani 1 1 d . . . N9 N 0.2932(4) 0.4733(3) 0.4512(3) 0.0184(11) Uani 1 1 d . . . N10 N 0.2420(4) 0.4107(3) 0.4237(3) 0.0193(11) Uani 1 1 d . . . N11 N 0.2207(4) 0.5888(3) 0.3262(3) 0.0221(8) Uani 1 1 d . . . N12 N 0.2302(4) 0.5455(3) 0.2729(3) 0.0221(8) Uani 1 1 d . . . O1 O 0.3420(3) 0.1941(3) 0.1518(2) 0.0177(9) Uani 1 1 d . . . O2 O 0.4411(3) 0.3423(3) 0.1373(2) 0.0223(9) Uani 1 1 d . . . O3 O 0.1282(3) 0.1906(3) 0.1870(2) 0.0164(8) Uani 1 1 d . . . O4 O 0.0401(3) 0.3180(3) 0.2237(2) 0.0198(9) Uani 1 1 d . . . O5 O 0.2697(3) 0.0959(3) 0.2851(2) 0.0192(9) Uani 1 1 d . . . O6 O 0.3280(3) 0.1491(3) 0.3938(2) 0.0208(9) Uani 1 1 d . . . O7 O 0.4059(3) 0.3205(3) 0.2962(2) 0.0160(8) Uani 1 1 d . . . O8 O 0.4892(3) 0.1852(3) 0.2699(2) 0.0212(9) Uani 1 1 d . . . O9 O 0.1906(3) 0.2996(3) 0.3440(2) 0.0190(9) Uani 1 1 d . . . O10 O 0.0834(3) 0.1582(3) 0.3455(2) 0.0198(9) Uani 1 1 d . . . O11 O 0.2520(3) 0.4097(3) 0.2111(2) 0.0186(9) Uani 1 1 d . . . O12 O 0.2122(3) 0.3568(3) 0.0999(2) 0.0214(9) Uani 1 1 d . . . O1S O 0.9128(8) 0.4637(5) 0.4223(5) 0.109(3) Uani 1 1 d D . . H1S H 0.9245 0.4120 0.4300 0.163 Uiso 1 1 calc R . . C1 C 0.4074(5) -0.1131(4) 0.1610(4) 0.0260(14) Uani 1 1 d . . . H1A H 0.4807 -0.1022 0.1373 0.039 Uiso 1 1 calc R . . H1B H 0.3821 -0.1701 0.1645 0.039 Uiso 1 1 calc R . . H1C H 0.4106 -0.1097 0.2103 0.039 Uiso 1 1 calc R . . C2 C 0.4281(5) 0.0799(4) 0.0729(3) 0.0230(14) Uani 1 1 d . . . H2 H 0.4636 0.0510 0.0442 0.028 Uiso 1 1 calc R . . C3 C 0.4686(5) 0.1664(4) 0.0631(3) 0.0191(13) Uani 1 1 d . . . C4 C 0.5577(5) 0.1989(4) 0.0080(3) 0.0247(14) Uani 1 1 d . . . H4 H 0.5856 0.1639 -0.0180 0.030 Uiso 1 1 calc R . . C5 C 0.6022(5) 0.2802(4) -0.0069(3) 0.0235(14) Uani 1 1 d . . . H5 H 0.6577 0.3014 -0.0441 0.028 Uiso 1 1 calc R . . C6 C 0.5635(5) 0.3310(4) 0.0344(3) 0.0233(14) Uani 1 1 d . . . H6 H 0.5940 0.3863 0.0246 0.028 Uiso 1 1 calc R . . C7 C 0.4799(5) 0.3004(4) 0.0898(3) 0.0179(13) Uani 1 1 d . . . C8 C 0.4270(5) 0.2187(4) 0.1025(3) 0.0182(13) Uani 1 1 d . . . C9 C 0.4925(5) 0.4238(4) 0.1293(4) 0.0258(14) Uani 1 1 d . . . H9A H 0.5720 0.4164 0.1345 0.039 Uiso 1 1 calc R . . H9B H 0.4626 0.4449 0.1672 0.039 Uiso 1 1 calc R . . H9C H 0.4776 0.4651 0.0806 0.039 Uiso 1 1 calc R . . C10 C 0.1546(5) 0.0592(4) -0.0124(3) 0.0233(14) Uani 1 1 d . . . H10A H 0.0893 0.0879 -0.0375 0.035 Uiso 1 1 calc R . . H10B H 0.1794 0.0168 -0.0338 0.035 Uiso 1 1 calc R . . H10C H 0.2132 0.1014 -0.0181 0.035 Uiso 1 1 calc R . . C11 C 0.0050(5) 0.1057(4) 0.0999(3) 0.0211(13) Uani 1 1 d . . . H11 H -0.0426 0.0843 0.0723 0.025 Uiso 1 1 calc R . . C12 C -0.0410(5) 0.1673(4) 0.1307(3) 0.0189(13) Uani 1 1 d . . . C13 C -0.1554(5) 0.1882(4) 0.1186(3) 0.0196(13) Uani 1 1 d . . . H13 H -0.1972 0.1604 0.0927 0.024 Uiso 1 1 calc R . . C14 C -0.2060(5) 0.2478(4) 0.1438(3) 0.0202(13) Uani 1 1 d . . . H14 H -0.2826 0.2575 0.1383 0.024 Uiso 1 1 calc R . . C15 C -0.1423(5) 0.2948(4) 0.1782(3) 0.0188(13) Uani 1 1 d . . . H15 H -0.1756 0.3383 0.1925 0.023 Uiso 1 1 calc R . . C16 C -0.0290(5) 0.2762(4) 0.1909(3) 0.0178(12) Uani 1 1 d . . . C17 C 0.0240(5) 0.2102(4) 0.1697(3) 0.0173(12) Uani 1 1 d . . . C18 C -0.0095(5) 0.3860(4) 0.2455(3) 0.0221(13) Uani 1 1 d . . . H18A H -0.0385 0.4299 0.2022 0.033 Uiso 1 1 calc R . . H18B H 0.0462 0.4114 0.2673 0.033 Uiso 1 1 calc R . . H18C H -0.0695 0.3622 0.2816 0.033 Uiso 1 1 calc R . . C19 C 0.0294(5) -0.1217(4) 0.2278(3) 0.0243(14) Uani 1 1 d . . . H19A H 0.0224 -0.1539 0.2805 0.036 Uiso 1 1 calc R . . H19B H 0.0019 -0.1566 0.2002 0.036 Uiso 1 1 calc R . . H19C H -0.0136 -0.0694 0.2162 0.036 Uiso 1 1 calc R . . C20 C 0.2322(5) -0.0889(4) 0.3096(3) 0.0189(13) Uani 1 1 d . . . H20 H 0.2270 -0.1492 0.3240 0.023 Uiso 1 1 calc R . . C21 C 0.2786(5) -0.0544(4) 0.3625(3) 0.0185(13) Uani 1 1 d . . . C22 C 0.3080(5) -0.1162(4) 0.4327(3) 0.0201(13) Uani 1 1 d . . . H22 H 0.3021 -0.1754 0.4406 0.024 Uiso 1 1 calc R . . C23 C 0.3451(5) -0.0891(4) 0.4889(3) 0.0229(14) Uani 1 1 d . . . H23 H 0.3656 -0.1298 0.5343 0.027 Uiso 1 1 calc R . . C24 C 0.3520(5) -0.0003(4) 0.4777(3) 0.0207(13) Uani 1 1 d . . . H24 H 0.3751 0.0176 0.5165 0.025 Uiso 1 1 calc R . . C25 C 0.3253(5) 0.0609(4) 0.4107(3) 0.0181(13) Uani 1 1 d . . . C26 C 0.2902(5) 0.0356(4) 0.3497(3) 0.0179(12) Uani 1 1 d . . . C27 C 0.3589(5) 0.1774(4) 0.4544(3) 0.0219(13) Uani 1 1 d . . . H27A H 0.3060 0.1545 0.4956 0.033 Uiso 1 1 calc R . . H27B H 0.3587 0.2399 0.4377 0.033 Uiso 1 1 calc R . . H27C H 0.4325 0.1567 0.4702 0.033 Uiso 1 1 calc R . . C28 C 0.4935(6) 0.6255(4) 0.2814(4) 0.0319(16) Uani 1 1 d . . . H28A H 0.5731 0.6174 0.2801 0.048 Uiso 1 1 calc R . . H28B H 0.4778 0.6797 0.2887 0.048 Uiso 1 1 calc R . . H28C H 0.4632 0.6263 0.2349 0.048 Uiso 1 1 calc R . . C29 C 0.5463(5) 0.4357(4) 0.3457(3) 0.0218(13) Uani 1 1 d . . . H29 H 0.5998 0.4668 0.3610 0.026 Uiso 1 1 calc R . . C30 C 0.5818(5) 0.3555(4) 0.3378(3) 0.0182(13) Uani 1 1 d . . . C31 C 0.6936(5) 0.3301(4) 0.3565(3) 0.0220(13) Uani 1 1 d . . . H31 H 0.7387 0.3644 0.3746 0.026 Uiso 1 1 calc R . . C32 C 0.7367(5) 0.2565(4) 0.3484(3) 0.0225(14) Uani 1 1 d . . . H32 H 0.8097 0.2399 0.3622 0.027 Uiso 1 1 calc R . . C33 C 0.6702(5) 0.2060(4) 0.3190(3) 0.0188(13) Uani 1 1 d . . . H33 H 0.7000 0.1567 0.3121 0.023 Uiso 1 1 calc R . . C34 C 0.5604(5) 0.2291(4) 0.3000(3) 0.0181(13) Uani 1 1 d . . . C35 C 0.5115(5) 0.3033(4) 0.3116(3) 0.0176(12) Uani 1 1 d . . . C36 C 0.5322(5) 0.1060(4) 0.2634(3) 0.0199(13) Uani 1 1 d . . . H36A H 0.5977 0.1189 0.2308 0.030 Uiso 1 1 calc R . . H36B H 0.4761 0.0793 0.2430 0.030 Uiso 1 1 calc R . . H36C H 0.5514 0.0670 0.3121 0.030 Uiso 1 1 calc R . . C37 C 0.3696(5) 0.4357(4) 0.5135(3) 0.0244(14) Uani 1 1 d . . . H37A H 0.3279 0.3982 0.5564 0.037 Uiso 1 1 calc R . . H37B H 0.4044 0.4816 0.5260 0.037 Uiso 1 1 calc R . . H37C H 0.4263 0.4026 0.4987 0.037 Uiso 1 1 calc R . . C38 C 0.1743(5) 0.3596(4) 0.4725(3) 0.0200(13) Uani 1 1 d . . . H38 H 0.1631 0.3705 0.5171 0.024 Uiso 1 1 calc R . . C39 C 0.1132(5) 0.2867(4) 0.4653(3) 0.0196(13) Uani 1 1 d . . . C40 C 0.0411(5) 0.2414(4) 0.5275(3) 0.0239(14) Uani 1 1 d . . . H40 H 0.0338 0.2605 0.5681 0.029 Uiso 1 1 calc R . . C41 C -0.0175(5) 0.1698(4) 0.5273(3) 0.0240(14) Uani 1 1 d . . . H41 H -0.0646 0.1403 0.5680 0.029 Uiso 1 1 calc R . . C42 C -0.0072(5) 0.1406(4) 0.4665(3) 0.0214(13) Uani 1 1 d . . . H42 H -0.0477 0.0919 0.4668 0.026 Uiso 1 1 calc R . . C43 C 0.0626(5) 0.1837(4) 0.4065(3) 0.0185(13) Uani 1 1 d . . . C44 C 0.1240(4) 0.2596(4) 0.4027(3) 0.0160(12) Uani 1 1 d . . . C45 C 0.0222(5) 0.0833(4) 0.3446(4) 0.0227(14) Uani 1 1 d . . . H45A H 0.0404 0.0340 0.3877 0.034 Uiso 1 1 calc R . . H45B H 0.0419 0.0714 0.2998 0.034 Uiso 1 1 calc R . . H45C H -0.0568 0.0942 0.3459 0.034 Uiso 1 1 calc R . . C46 C 0.1303(5) 0.6502(5) 0.3222(4) 0.0321(16) Uani 1 1 d . . . H46A H 0.1451 0.7031 0.2808 0.048 Uiso 1 1 calc R . . H46B H 0.1259 0.6628 0.3680 0.048 Uiso 1 1 calc R . . H46C H 0.0606 0.6252 0.3152 0.048 Uiso 1 1 calc R . . C47 C 0.1852(5) 0.5847(4) 0.2093(4) 0.0239(14) Uani 1 1 d . . . H47 H 0.1537 0.6388 0.2026 0.029 Uiso 1 1 calc R . . C48 C 0.1791(5) 0.5526(4) 0.1469(3) 0.0187(13) Uani 1 1 d . . . C49 C 0.1342(5) 0.6099(4) 0.0804(3) 0.0227(14) Uani 1 1 d . . . H49 H 0.1144 0.6658 0.0779 0.027 Uiso 1 1 calc R . . C50 C 0.1192(5) 0.5854(4) 0.0194(3) 0.0232(14) Uani 1 1 d . . . H50 H 0.0913 0.6246 -0.0244 0.028 Uiso 1 1 calc R . . C51 C 0.1464(5) 0.5004(4) 0.0239(3) 0.0194(13) Uani 1 1 d . . . H51 H 0.1359 0.4831 -0.0172 0.023 Uiso 1 1 calc R . . C52 C 0.1882(4) 0.4428(4) 0.0880(3) 0.0157(12) Uani 1 1 d . . . C53 C 0.2093(4) 0.4677(4) 0.1513(3) 0.0160(12) Uani 1 1 d . . . C54 C 0.1954(5) 0.3300(4) 0.0362(3) 0.0217(13) Uani 1 1 d . . . H54A H 0.1194 0.3414 0.0206 0.032 Uiso 1 1 calc R . . H54B H 0.2099 0.2689 0.0497 0.032 Uiso 1 1 calc R . . H54C H 0.2457 0.3620 -0.0043 0.032 Uiso 1 1 calc R . . C1S C 0.7623(5) 0.6685(5) 0.1667(4) 0.0338(17) Uani 1 1 d . . . H1S1 H 0.7576 0.6752 0.2160 0.041 Uiso 1 1 calc R . . C2S C 0.7108(6) 0.8880(5) 0.2981(4) 0.0345(17) Uani 1 1 d . . . H2S H 0.7509 0.8333 0.3065 0.041 Uiso 1 1 calc R . . C3S C 0.8521(7) 0.4976(6) 0.3585(5) 0.054(2) Uani 1 1 d DU . . H3S1 H 0.7829 0.5205 0.3706 0.081 Uiso 1 1 calc R . . H3S2 H 0.8364 0.4526 0.3384 0.081 Uiso 1 1 calc R . . H3S3 H 0.8946 0.5434 0.3221 0.081 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.02042(17) 0.01543(17) 0.01566(17) -0.00764(13) -0.00232(12) 0.00030(12) Zn1 0.0166(3) 0.0133(3) 0.0141(3) -0.0069(3) -0.0012(3) -0.0003(3) Zn2 0.0185(3) 0.0133(4) 0.0142(3) -0.0067(3) -0.0015(3) -0.0002(3) Cl1 0.0375(9) 0.0316(9) 0.0244(8) -0.0128(7) -0.0030(7) 0.0039(7) Cl2 0.0330(9) 0.0451(11) 0.0326(10) -0.0080(8) 0.0003(7) 0.0025(8) Cl3 0.0717(14) 0.0423(12) 0.0408(11) -0.0129(9) -0.0056(10) 0.0160(10) Cl4 0.0320(10) 0.0929(18) 0.0358(11) -0.0245(11) 0.0050(8) -0.0049(10) Cl5 0.0337(10) 0.0572(13) 0.0442(11) -0.0159(10) 0.0014(8) -0.0088(9) Cl6 0.0361(10) 0.0459(12) 0.0542(12) -0.0253(10) -0.0051(9) -0.0034(8) Cl7 0.0460(12) 0.0791(16) 0.0338(11) -0.0144(10) -0.0022(9) -0.0076(11) P1 0.0184(8) 0.0168(8) 0.0176(8) -0.0101(7) -0.0006(6) 0.0003(6) P2 0.0217(8) 0.0142(8) 0.0204(8) -0.0101(7) -0.0022(6) 0.0004(6) S1 0.0281(8) 0.0214(8) 0.0255(8) -0.0161(7) -0.0020(7) -0.0006(6) S2 0.0333(9) 0.0236(9) 0.0337(9) -0.0190(8) -0.0037(7) -0.0002(7) N1 0.024(3) 0.020(3) 0.024(3) -0.011(2) -0.005(2) 0.002(2) N2 0.023(3) 0.020(3) 0.029(3) -0.015(2) -0.003(2) 0.001(2) N3 0.027(3) 0.024(3) 0.019(3) -0.010(2) 0.000(2) 0.000(2) N4 0.027(3) 0.024(3) 0.017(3) -0.013(2) -0.001(2) 0.004(2) N5 0.024(3) 0.019(3) 0.021(3) -0.011(2) 0.000(2) -0.001(2) N6 0.027(3) 0.016(3) 0.018(3) -0.008(2) 0.000(2) -0.004(2) N7 0.021(3) 0.017(3) 0.027(3) -0.010(2) 0.002(2) -0.002(2) N8 0.018(3) 0.015(3) 0.024(3) -0.009(2) 0.001(2) 0.000(2) N9 0.028(3) 0.015(3) 0.013(2) -0.005(2) -0.004(2) -0.006(2) N10 0.021(3) 0.021(3) 0.018(3) -0.010(2) -0.002(2) 0.002(2) N11 0.027(2) 0.019(2) 0.025(2) -0.0133(16) -0.0022(16) 0.0026(15) N12 0.027(2) 0.019(2) 0.025(2) -0.0133(16) -0.0022(16) 0.0026(15) O1 0.019(2) 0.016(2) 0.019(2) -0.0060(17) -0.0011(17) -0.0008(16) O2 0.025(2) 0.022(2) 0.022(2) -0.0091(19) 0.0016(18) -0.0031(18) O3 0.014(2) 0.020(2) 0.016(2) -0.0074(17) -0.0035(16) 0.0004(16) O4 0.020(2) 0.021(2) 0.024(2) -0.0142(19) -0.0063(17) 0.0025(17) O5 0.023(2) 0.017(2) 0.018(2) -0.0067(18) -0.0029(17) 0.0012(17) O6 0.032(2) 0.017(2) 0.016(2) -0.0090(18) -0.0053(18) 0.0016(18) O7 0.014(2) 0.019(2) 0.018(2) -0.0091(17) -0.0039(16) -0.0009(16) O8 0.021(2) 0.022(2) 0.026(2) -0.0145(19) -0.0046(18) 0.0030(17) O9 0.023(2) 0.019(2) 0.017(2) -0.0087(18) -0.0020(17) -0.0018(17) O10 0.024(2) 0.019(2) 0.018(2) -0.0078(18) 0.0035(17) -0.0058(17) O11 0.022(2) 0.018(2) 0.017(2) -0.0074(18) 0.0001(17) 0.0024(17) O12 0.030(2) 0.019(2) 0.018(2) -0.0104(18) -0.0070(18) 0.0056(18) O1S 0.099(6) 0.078(6) 0.151(8) -0.039(6) -0.038(6) 0.013(5) C1 0.027(3) 0.025(4) 0.028(4) -0.012(3) -0.005(3) 0.005(3) C2 0.020(3) 0.028(4) 0.025(3) -0.015(3) 0.001(3) -0.001(3) C3 0.018(3) 0.027(3) 0.017(3) -0.012(3) -0.003(2) 0.001(2) C4 0.026(3) 0.028(4) 0.024(3) -0.015(3) -0.003(3) -0.002(3) C5 0.018(3) 0.033(4) 0.018(3) -0.006(3) 0.003(2) -0.002(3) C6 0.018(3) 0.023(3) 0.023(3) -0.001(3) -0.002(3) -0.005(3) C7 0.018(3) 0.022(3) 0.013(3) -0.005(3) -0.003(2) -0.001(2) C8 0.018(3) 0.026(3) 0.010(3) -0.006(3) -0.003(2) 0.001(2) C9 0.035(4) 0.013(3) 0.030(4) -0.008(3) 0.002(3) -0.006(3) C10 0.030(3) 0.025(4) 0.016(3) -0.009(3) -0.001(3) -0.001(3) C11 0.021(3) 0.022(3) 0.020(3) -0.007(3) -0.003(3) -0.001(3) C12 0.019(3) 0.017(3) 0.019(3) -0.004(3) 0.002(2) -0.005(2) C13 0.018(3) 0.023(3) 0.017(3) -0.005(3) -0.005(2) -0.001(2) C14 0.013(3) 0.023(3) 0.021(3) -0.003(3) 0.000(2) 0.000(2) C15 0.022(3) 0.023(3) 0.013(3) -0.009(3) 0.000(2) -0.001(2) C16 0.019(3) 0.021(3) 0.014(3) -0.006(3) 0.002(2) 0.000(2) C17 0.025(3) 0.020(3) 0.007(3) -0.005(2) -0.002(2) 0.003(2) C18 0.029(3) 0.019(3) 0.024(3) -0.014(3) -0.002(3) 0.005(3) C19 0.027(3) 0.025(4) 0.023(3) -0.012(3) 0.003(3) 0.001(3) C20 0.022(3) 0.015(3) 0.019(3) -0.005(3) 0.005(2) 0.004(2) C21 0.017(3) 0.022(3) 0.017(3) -0.007(3) 0.001(2) 0.004(2) C22 0.023(3) 0.018(3) 0.016(3) -0.001(3) 0.000(2) 0.000(2) C23 0.027(3) 0.022(3) 0.014(3) 0.002(3) -0.001(3) 0.002(3) C24 0.026(3) 0.024(3) 0.014(3) -0.008(3) -0.003(2) 0.002(3) C25 0.017(3) 0.017(3) 0.021(3) -0.008(3) 0.000(2) -0.002(2) C26 0.017(3) 0.016(3) 0.019(3) -0.004(3) 0.000(2) 0.002(2) C27 0.028(3) 0.019(3) 0.025(3) -0.015(3) -0.004(3) 0.000(3) C28 0.039(4) 0.021(4) 0.033(4) -0.008(3) 0.012(3) -0.005(3) C29 0.023(3) 0.022(3) 0.020(3) -0.008(3) 0.003(3) -0.006(3) C30 0.025(3) 0.019(3) 0.010(3) -0.003(2) -0.003(2) 0.001(2) C31 0.015(3) 0.029(4) 0.023(3) -0.011(3) 0.002(2) -0.001(3) C32 0.019(3) 0.029(4) 0.017(3) -0.004(3) -0.005(2) 0.004(3) C33 0.021(3) 0.020(3) 0.016(3) -0.006(3) 0.000(2) 0.000(2) C34 0.019(3) 0.019(3) 0.018(3) -0.007(3) 0.000(2) -0.001(2) C35 0.017(3) 0.020(3) 0.015(3) -0.005(3) 0.001(2) -0.001(2) C36 0.019(3) 0.016(3) 0.028(3) -0.012(3) -0.003(3) 0.002(2) C37 0.030(3) 0.027(4) 0.017(3) -0.009(3) -0.008(3) -0.002(3) C38 0.019(3) 0.028(4) 0.015(3) -0.010(3) -0.001(2) 0.002(3) C39 0.019(3) 0.021(3) 0.020(3) -0.009(3) -0.003(2) 0.003(2) C40 0.025(3) 0.033(4) 0.018(3) -0.014(3) 0.003(3) -0.003(3) C41 0.024(3) 0.027(4) 0.017(3) -0.004(3) 0.008(3) -0.007(3) C42 0.022(3) 0.018(3) 0.021(3) -0.003(3) 0.000(3) -0.006(3) C43 0.021(3) 0.020(3) 0.013(3) -0.005(3) 0.000(2) 0.003(2) C44 0.015(3) 0.019(3) 0.013(3) -0.004(2) 0.001(2) -0.002(2) C45 0.024(3) 0.018(3) 0.027(3) -0.009(3) 0.005(3) -0.004(3) C46 0.029(4) 0.041(4) 0.030(4) -0.017(3) -0.005(3) 0.013(3) C47 0.026(3) 0.012(3) 0.035(4) -0.010(3) 0.000(3) 0.000(3) C48 0.018(3) 0.016(3) 0.022(3) -0.007(3) 0.002(2) -0.005(2) C49 0.028(3) 0.016(3) 0.022(3) -0.005(3) -0.002(3) 0.000(3) C50 0.021(3) 0.024(4) 0.021(3) -0.002(3) -0.004(3) -0.005(3) C51 0.024(3) 0.016(3) 0.016(3) -0.003(3) 0.001(2) -0.006(2) C52 0.015(3) 0.015(3) 0.015(3) -0.004(2) 0.003(2) -0.001(2) C53 0.014(3) 0.015(3) 0.017(3) -0.003(2) -0.002(2) -0.003(2) C54 0.030(3) 0.028(4) 0.011(3) -0.013(3) -0.002(2) 0.004(3) C1S 0.026(4) 0.054(5) 0.023(4) -0.015(3) -0.004(3) 0.008(3) C2S 0.032(4) 0.028(4) 0.046(4) -0.015(3) -0.002(3) 0.000(3) C3S 0.056(2) 0.053(2) 0.054(2) -0.0187(12) -0.0076(10) -0.0017(10) _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 Eu1 O7 2.409(4) . ? Eu1 O11 2.406(4) . ? Eu1 O9 2.410(4) . ? Eu1 O3 2.412(4) . ? Eu1 O5 2.436(4) . ? Eu1 O1 2.446(4) . ? Eu1 O12 2.768(4) . ? Eu1 O4 2.868(4) . ? Eu1 O2 2.889(4) . ? Eu1 O8 2.890(4) . ? Eu1 O6 2.893(4) . ? Eu1 O10 2.926(4) . ? Zn1 O1 2.078(4) . ? Zn1 O5 2.083(4) . ? Zn1 O3 2.089(4) . ? Zn1 N4 2.131(5) . ? Zn1 N6 2.131(5) . ? Zn1 N2 2.158(5) . ? Zn2 O11 2.067(4) . ? Zn2 O7 2.122(4) . ? Zn2 N8 2.132(5) . ? Zn2 O9 2.135(4) . ? Zn2 N10 2.135(5) . ? Zn2 N12 2.184(5) . ? Cl2 C1S 1.770(7) . ? Cl3 C1S 1.769(8) . ? Cl4 C1S 1.758(7) . ? Cl5 C2S 1.768(7) . ? Cl6 C2S 1.764(7) . ? Cl7 C2S 1.759(7) . ? P1 N5 1.671(5) . ? P1 N3 1.674(5) . ? P1 N1 1.683(5) . ? P1 S1 1.926(2) . ? P2 N11 1.668(5) . ? P2 N7 1.671(5) . ? P2 N9 1.671(5) . ? P2 S2 1.924(2) . ? N1 N2 1.442(7) . ? N1 C1 1.474(7) . ? N2 C2 1.288(7) . ? N3 C10 1.460(7) . ? N3 N4 1.455(7) . ? N4 C11 1.295(7) . ? N5 N6 1.450(6) . ? N5 C19 1.475(7) . ? N6 C20 1.294(7) . ? N7 N8 1.455(7) . ? N7 C28 1.475(8) . ? N8 C29 1.294(7) . ? N9 N10 1.444(6) . ? N9 C37 1.474(7) . ? N10 C38 1.278(7) . ? N11 N12 1.424(7) . ? N11 C46 1.458(7) . ? N12 C47 1.290(8) . ? O1 C8 1.325(7) . ? O2 C7 1.379(7) . ? O2 C9 1.426(7) . ? O3 C17 1.306(7) . ? O4 C16 1.363(7) . ? O4 C18 1.436(7) . ? O5 C26 1.313(7) . ? O6 C25 1.367(7) . ? O6 C27 1.437(6) . ? O7 C35 1.310(6) . ? O8 C34 1.369(7) . ? O8 C36 1.435(7) . ? O9 C44 1.324(6) . ? O10 C43 1.375(7) . ? O10 C45 1.432(7) . ? O11 C53 1.320(7) . ? O12 C52 1.378(7) . ? O12 C54 1.441(6) . ? O1S C3S 1.374(9) . ? C2 C3 1.443(8) . ? C3 C8 1.399(8) . ? C3 C4 1.437(8) . ? C4 C5 1.365(9) . ? C5 C6 1.395(9) . ? C6 C7 1.389(8) . ? C7 C8 1.419(8) . ? C11 C12 1.431(8) . ? C12 C13 1.412(8) . ? C12 C17 1.426(8) . ? C13 C14 1.360(8) . ? C14 C15 1.403(8) . ? C15 C16 1.395(8) . ? C16 C17 1.418(8) . ? C20 C21 1.434(8) . ? C21 C26 1.413(8) . ? C21 C22 1.422(8) . ? C22 C23 1.373(8) . ? C23 C24 1.395(8) . ? C24 C25 1.368(8) . ? C25 C26 1.432(8) . ? C29 C30 1.432(8) . ? C30 C35 1.414(8) . ? C30 C31 1.415(8) . ? C31 C32 1.364(8) . ? C32 C33 1.403(8) . ? C33 C34 1.386(8) . ? C34 C35 1.429(8) . ? C38 C39 1.445(8) . ? C39 C44 1.408(8) . ? C39 C40 1.423(8) . ? C40 C41 1.365(9) . ? C41 C42 1.395(8) . ? C42 C43 1.374(8) . ? C43 C44 1.421(8) . ? C47 C48 1.455(8) . ? C48 C53 1.409(8) . ? C48 C49 1.410(8) . ? C49 C50 1.365(8) . ? C50 C51 1.401(8) . ? C51 C52 1.366(8) . ? C52 C53 1.424(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Eu1 O11 64.82(13) . . ? O7 Eu1 O9 67.64(13) . . ? O11 Eu1 O9 66.25(13) . . ? O7 Eu1 O3 177.61(13) . . ? O11 Eu1 O3 114.48(13) . . ? O9 Eu1 O3 114.35(13) . . ? O7 Eu1 O5 115.19(13) . . ? O11 Eu1 O5 176.00(12) . . ? O9 Eu1 O5 109.89(13) . . ? O3 Eu1 O5 65.68(13) . . ? O7 Eu1 O1 113.06(13) . . ? O11 Eu1 O1 119.24(13) . . ? O9 Eu1 O1 174.42(13) . . ? O3 Eu1 O1 65.10(12) . . ? O5 Eu1 O1 64.64(13) . . ? O7 Eu1 O12 112.55(13) . . ? O11 Eu1 O12 59.85(12) . . ? O9 Eu1 O12 116.43(12) . . ? O3 Eu1 O12 65.53(12) . . ? O5 Eu1 O12 122.62(12) . . ? O1 Eu1 O12 68.72(12) . . ? O7 Eu1 O4 121.92(12) . . ? O11 Eu1 O4 66.11(12) . . ? O9 Eu1 O4 65.52(12) . . ? O3 Eu1 O4 58.86(12) . . ? O5 Eu1 O4 111.66(12) . . ? O1 Eu1 O4 116.91(12) . . ? O12 Eu1 O4 63.70(12) . . ? O7 Eu1 O2 66.52(12) . . ? O11 Eu1 O2 69.01(12) . . ? O9 Eu1 O2 125.73(12) . . ? O3 Eu1 O2 111.10(12) . . ? O5 Eu1 O2 114.84(12) . . ? O1 Eu1 O2 58.15(12) . . ? O12 Eu1 O2 60.02(12) . . ? O4 Eu1 O2 119.96(12) . . ? O7 Eu1 O8 58.40(12) . . ? O11 Eu1 O8 115.32(12) . . ? O9 Eu1 O8 113.37(12) . . ? O3 Eu1 O8 120.91(12) . . ? O5 Eu1 O8 66.82(12) . . ? O1 Eu1 O8 64.02(12) . . ? O12 Eu1 O8 118.31(12) . . ? O4 Eu1 O8 177.87(11) . . ? O2 Eu1 O8 62.17(12) . . ? O7 Eu1 O6 65.95(12) . . ? O11 Eu1 O6 119.67(12) . . ? O9 Eu1 O6 64.27(12) . . ? O3 Eu1 O6 115.93(12) . . ? O5 Eu1 O6 57.97(12) . . ? O1 Eu1 O6 110.66(12) . . ? O12 Eu1 O6 178.14(12) . . ? O4 Eu1 O6 117.94(11) . . ? O2 Eu1 O6 118.13(12) . . ? O8 Eu1 O6 60.07(11) . . ? O7 Eu1 O10 117.25(12) . . ? O11 Eu1 O10 113.56(12) . . ? O9 Eu1 O10 58.20(12) . . ? O3 Eu1 O10 65.14(12) . . ? O5 Eu1 O10 62.67(12) . . ? O1 Eu1 O10 118.02(12) . . ? O12 Eu1 O10 118.12(12) . . ? O4 Eu1 O10 59.86(12) . . ? O2 Eu1 O10 175.96(11) . . ? O8 Eu1 O10 118.03(12) . . ? O6 Eu1 O10 63.74(11) . . ? O1 Zn1 O5 77.70(15) . . ? O1 Zn1 O3 77.71(15) . . ? O5 Zn1 O3 78.14(15) . . ? O1 Zn1 N4 122.23(18) . . ? O5 Zn1 N4 148.85(17) . . ? O3 Zn1 N4 83.08(16) . . ? O1 Zn1 N6 148.39(17) . . ? O5 Zn1 N6 83.69(17) . . ? O3 Zn1 N6 123.20(17) . . ? N4 Zn1 N6 86.15(19) . . ? O1 Zn1 N2 83.71(17) . . ? O5 Zn1 N2 121.64(17) . . ? O3 Zn1 N2 149.22(17) . . ? N4 Zn1 N2 86.44(18) . . ? N6 Zn1 N2 84.65(19) . . ? O1 Zn1 Eu1 46.90(11) . . ? O5 Zn1 Eu1 46.64(11) . . ? O3 Zn1 Eu1 46.00(10) . . ? N4 Zn1 Eu1 127.44(13) . . ? N6 Zn1 Eu1 128.46(13) . . ? N2 Zn1 Eu1 128.77(13) . . ? O11 Zn2 O7 76.04(14) . . ? O11 Zn2 N8 123.37(17) . . ? O7 Zn2 N8 82.54(16) . . ? O11 Zn2 O9 77.54(15) . . ? O7 Zn2 O9 78.11(15) . . ? N8 Zn2 O9 146.82(17) . . ? O11 Zn2 N10 148.37(17) . . ? O7 Zn2 N10 123.38(17) . . ? N8 Zn2 N10 86.13(18) . . ? O9 Zn2 N10 82.44(17) . . ? O11 Zn2 N12 84.32(17) . . ? O7 Zn2 N12 147.07(17) . . ? N8 Zn2 N12 86.71(18) . . ? O9 Zn2 N12 123.34(17) . . ? N10 Zn2 N12 86.58(18) . . ? O11 Zn2 Eu1 45.94(11) . . ? O7 Zn2 Eu1 46.17(10) . . ? N8 Zn2 Eu1 127.60(12) . . ? O9 Zn2 Eu1 46.22(10) . . ? N10 Zn2 Eu1 126.99(14) . . ? N12 Zn2 Eu1 128.56(13) . . ? N5 P1 N3 107.0(2) . . ? N5 P1 N1 105.4(2) . . ? N3 P1 N1 106.2(3) . . ? N5 P1 S1 112.98(19) . . ? N3 P1 S1 112.03(19) . . ? N1 P1 S1 112.74(19) . . ? N11 P2 N7 108.3(3) . . ? N11 P2 N9 104.7(3) . . ? N7 P2 N9 104.4(3) . . ? N11 P2 S2 112.84(19) . . ? N7 P2 S2 112.36(19) . . ? N9 P2 S2 113.63(19) . . ? N2 N1 C1 114.3(4) . . ? N2 N1 P1 114.0(4) . . ? C1 N1 P1 118.8(4) . . ? C2 N2 N1 112.9(5) . . ? C2 N2 Zn1 128.0(4) . . ? N1 N2 Zn1 118.7(4) . . ? C10 N3 N4 112.9(5) . . ? C10 N3 P1 121.0(4) . . ? N4 N3 P1 114.2(4) . . ? C11 N4 N3 112.4(5) . . ? C11 N4 Zn1 128.4(4) . . ? N3 N4 Zn1 118.2(3) . . ? N6 N5 C19 113.7(4) . . ? N6 N5 P1 113.8(4) . . ? C19 N5 P1 120.0(4) . . ? C20 N6 N5 112.3(5) . . ? C20 N6 Zn1 127.4(4) . . ? N5 N6 Zn1 119.1(3) . . ? N8 N7 C28 114.1(4) . . ? N8 N7 P2 115.0(4) . . ? C28 N7 P2 119.7(4) . . ? C29 N8 N7 112.1(5) . . ? C29 N8 Zn2 129.5(4) . . ? N7 N8 Zn2 117.9(3) . . ? N10 N9 C37 114.6(5) . . ? N10 N9 P2 115.7(3) . . ? C37 N9 P2 119.3(4) . . ? C38 N10 N9 111.8(5) . . ? C38 N10 Zn2 131.0(4) . . ? N9 N10 Zn2 117.1(3) . . ? N12 N11 C46 120.6(5) . . ? N12 N11 P2 115.3(4) . . ? C46 N11 P2 123.9(4) . . ? C47 N12 N11 115.6(5) . . ? C47 N12 Zn2 127.8(4) . . ? N11 N12 Zn2 115.9(4) . . ? C8 O1 Zn1 133.0(4) . . ? C8 O1 Eu1 132.2(3) . . ? Zn1 O1 Eu1 94.77(14) . . ? C7 O2 C9 116.8(5) . . ? C7 O2 Eu1 116.4(3) . . ? C9 O2 Eu1 126.8(3) . . ? C17 O3 Zn1 132.5(4) . . ? C17 O3 Eu1 132.0(3) . . ? Zn1 O3 Eu1 95.47(14) . . ? C16 O4 C18 116.3(4) . . ? C16 O4 Eu1 115.3(3) . . ? C18 O4 Eu1 128.4(3) . . ? C26 O5 Zn1 132.2(4) . . ? C26 O5 Eu1 132.9(4) . . ? Zn1 O5 Eu1 94.92(15) . . ? C25 O6 C27 115.0(4) . . ? C25 O6 Eu1 116.6(3) . . ? C27 O6 Eu1 128.3(3) . . ? C35 O7 Zn2 132.2(3) . . ? C35 O7 Eu1 133.4(3) . . ? Zn2 O7 Eu1 94.38(14) . . ? C34 O8 C36 115.4(4) . . ? C34 O8 Eu1 115.4(3) . . ? C36 O8 Eu1 128.8(3) . . ? C44 O9 Zn2 133.3(3) . . ? C44 O9 Eu1 131.8(3) . . ? Zn2 O9 Eu1 94.02(14) . . ? C43 O10 C45 116.0(4) . . ? C43 O10 Eu1 114.6(3) . . ? C45 O10 Eu1 129.0(3) . . ? C53 O11 Zn2 133.4(4) . . ? C53 O11 Eu1 129.4(3) . . ? Zn2 O11 Eu1 95.93(15) . . ? C52 O12 C54 114.6(4) . . ? C52 O12 Eu1 116.9(3) . . ? C54 O12 Eu1 128.2(3) . . ? N2 C2 C3 126.2(5) . . ? C8 C3 C4 119.5(5) . . ? C8 C3 C2 124.8(5) . . ? C4 C3 C2 115.6(5) . . ? C5 C4 C3 121.0(6) . . ? C4 C5 C6 119.3(6) . . ? C5 C6 C7 121.0(6) . . ? O2 C7 C6 125.9(5) . . ? O2 C7 C8 113.5(5) . . ? C6 C7 C8 120.6(5) . . ? O1 C8 C3 122.5(5) . . ? O1 C8 C7 119.2(5) . . ? C3 C8 C7 118.2(5) . . ? N4 C11 C12 126.3(5) . . ? C13 C12 C17 119.6(5) . . ? C13 C12 C11 117.3(5) . . ? C17 C12 C11 123.1(5) . . ? C14 C13 C12 121.7(5) . . ? C13 C14 C15 119.8(5) . . ? C16 C15 C14 120.0(5) . . ? O4 C16 C15 124.6(5) . . ? O4 C16 C17 114.2(5) . . ? C15 C16 C17 121.2(5) . . ? O3 C17 C12 123.0(5) . . ? O3 C17 C16 119.5(5) . . ? C12 C17 C16 117.5(5) . . ? N6 C20 C21 126.4(6) . . ? C26 C21 C22 119.9(5) . . ? C26 C21 C20 123.6(5) . . ? C22 C21 C20 116.4(5) . . ? C23 C22 C21 120.5(6) . . ? C22 C23 C24 119.9(6) . . ? C25 C24 C23 121.1(5) . . ? O6 C25 C24 126.1(5) . . ? O6 C25 C26 113.1(5) . . ? C24 C25 C26 120.9(5) . . ? O5 C26 C21 123.1(5) . . ? O5 C26 C25 119.3(5) . . ? C21 C26 C25 117.6(5) . . ? N8 C29 C30 126.6(6) . . ? C35 C30 C31 120.1(5) . . ? C35 C30 C29 123.0(5) . . ? C31 C30 C29 116.9(5) . . ? C32 C31 C30 121.4(6) . . ? C31 C32 C33 119.5(6) . . ? C34 C33 C32 120.6(6) . . ? O8 C34 C33 125.2(5) . . ? O8 C34 C35 113.9(5) . . ? C33 C34 C35 120.9(5) . . ? O7 C35 C30 123.7(5) . . ? O7 C35 C34 118.9(5) . . ? C30 C35 C34 117.3(5) . . ? N10 C38 C39 126.6(5) . . ? C44 C39 C40 120.9(5) . . ? C44 C39 C38 123.8(5) . . ? C40 C39 C38 115.3(5) . . ? C41 C40 C39 119.9(5) . . ? C40 C41 C42 120.5(6) . . ? C43 C42 C41 120.0(6) . . ? O10 C43 C42 125.0(5) . . ? O10 C43 C44 113.0(5) . . ? C42 C43 C44 122.0(5) . . ? O9 C44 C39 122.8(5) . . ? O9 C44 C43 120.6(5) . . ? C39 C44 C43 116.6(5) . . ? N12 C47 C48 126.3(6) . . ? C53 C48 C49 119.7(5) . . ? C53 C48 C47 123.9(5) . . ? C49 C48 C47 116.4(5) . . ? C50 C49 C48 121.6(6) . . ? C49 C50 C51 119.2(6) . . ? C52 C51 C50 120.6(6) . . ? C51 C52 O12 125.5(5) . . ? C51 C52 C53 121.4(5) . . ? O12 C52 C53 113.1(5) . . ? O11 C53 C48 123.9(5) . . ? O11 C53 C52 118.7(5) . . ? C48 C53 C52 117.4(5) . . ? Cl4 C1S Cl3 111.3(4) . . ? Cl4 C1S Cl2 110.1(4) . . ? Cl3 C1S Cl2 109.1(4) . . ? Cl7 C2S Cl6 109.6(4) . . ? Cl7 C2S Cl5 110.9(4) . . ? Cl6 C2S Cl5 110.0(4) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 2.411 _refine_diff_density_min -0.966 _refine_diff_density_rms 0.145 _database_code_depnum_ccdc_archive 'CCDC 941524'