# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_p1 _database_code_depnum_ccdc_archive 'CCDC 905582' #TrackingRef '1 (905582).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H66 N28 O26 La2, 2(Cd Cl4), 2Cl, 31(H2 O)' _chemical_formula_sum 'C42 H128 Cl10 La2 N28 O57 Zn2' _chemical_formula_weight 2700.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.1365(14) _cell_length_b 17.9392(15) _cell_length_c 18.5138(15) _cell_angle_alpha 104.378(3) _cell_angle_beta 102.328(3) _cell_angle_gamma 110.919(3) _cell_volume 4854.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2752 _exptl_absorpt_coefficient_mu 1.741 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6143 _exptl_absorpt_correction_T_max 0.6602 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54507 _diffrn_reflns_av_R_equivalents 0.0779 _diffrn_reflns_av_sigmaI/netI 0.0970 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 26.00 _reflns_number_total 18509 _reflns_number_gt 12437 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18509 _refine_ls_number_parameters 991 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0743 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1342 _refine_ls_wR_factor_gt 0.1249 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl9 Cl -0.30242(10) 0.20296(10) 0.29086(10) 0.0539(4) Uani 1 1 d . . . Cl10 Cl -0.11694(14) -0.08918(12) 0.37630(10) 0.0692(5) Uani 1 1 d . . . O1W O 0.2506(2) 0.6015(2) 0.6383(2) 0.0391(9) Uani 1 1 d . . . O2W O 0.3217(3) 0.4723(2) 0.6083(2) 0.0432(10) Uani 1 1 d . . . O3W O 0.2897(3) 0.4313(3) 0.4189(2) 0.0567(12) Uani 1 1 d . . . O4W O 0.3961(3) 0.6430(3) 0.4512(2) 0.0558(12) Uani 1 1 d . . . O5W O 0.2737(3) 0.6902(3) 0.5373(3) 0.0620(13) Uani 1 1 d . . . O6W O 0.4552(3) 0.5469(3) 0.5424(3) 0.0731(16) Uani 1 1 d . . . O7W O -0.0958(2) 0.1669(2) -0.0399(2) 0.0364(9) Uani 1 1 d . . . O8W O -0.2579(3) 0.1679(3) -0.0142(2) 0.0434(10) Uani 1 1 d . . . O9W O -0.1761(3) -0.0069(2) 0.1138(2) 0.0460(10) Uani 1 1 d . . . O10W O -0.0987(3) 0.0134(3) -0.0099(2) 0.0527(11) Uani 1 1 d . . . O11W O 0.0048(3) 0.1611(3) 0.1295(2) 0.0570(12) Uani 1 1 d . . . O12W O -0.2980(3) 0.0897(4) 0.1002(2) 0.0673(14) Uani 1 1 d . . . Cl1 Cl 0.36441(10) 0.51598(10) 0.92494(10) 0.0478(4) Uani 1 1 d . . . Cl2 Cl 0.20568(11) 0.49144(10) 0.74387(9) 0.0500(4) Uani 1 1 d . . . Cl3 Cl 0.31189(12) 0.69573(11) 0.91888(10) 0.0568(4) Uani 1 1 d . . . Cl4 Cl 0.13836(10) 0.50092(14) 0.92166(10) 0.0626(5) Uani 1 1 d . . . Cl5 Cl 0.06709(13) 0.67035(11) 0.38528(11) 0.0631(5) Uani 1 1 d . . . Cl6 Cl 0.16043(15) 0.89686(11) 0.48224(11) 0.0685(5) Uani 1 1 d . . . Cl7 Cl 0.1578(2) 0.80371(14) 0.27313(12) 0.0987(9) Uani 1 1 d . . . Cl8 Cl 0.31354(16) 0.80410(17) 0.43568(17) 0.1000(8) Uani 1 1 d . . . Zn1 Zn 0.25387(5) 0.55099(5) 0.87739(4) 0.04208(18) Uani 1 1 d . . . Zn2 Zn 0.17332(6) 0.79243(5) 0.39427(5) 0.0561(2) Uani 1 1 d . . . La1 La 0.308759(19) 0.56116(2) 0.523435(17) 0.02979(9) Uani 1 1 d . . . La2 La -0.157470(18) 0.114476(18) 0.061552(16) 0.02576(9) Uani 1 1 d . . . C1 C 0.1396(3) 0.5217(3) 0.3371(3) 0.0260(11) Uani 1 1 d . . . C2 C 0.0469(3) 0.4967(3) 0.2130(3) 0.0271(11) Uani 1 1 d . . . H2 H 0.0366 0.5403 0.1938 0.033 Uiso 1 1 calc R . . C3 C -0.0105(3) 0.4699(3) 0.2650(3) 0.0257(11) Uani 1 1 d . . . H3 H -0.0435 0.5045 0.2748 0.031 Uiso 1 1 calc R . . C4 C -0.0478(3) 0.3509(3) 0.1537(3) 0.0254(11) Uani 1 1 d . . . C5 C 0.0353(3) 0.4863(3) 0.4097(3) 0.0309(12) Uani 1 1 d . . . H5A H 0.0864 0.5325 0.4538 0.037 Uiso 1 1 calc R . . H5B H -0.0151 0.5006 0.4073 0.037 Uiso 1 1 calc R . . C6 C -0.1328(3) 0.3273(3) 0.2448(3) 0.0306(12) Uani 1 1 d . . . H6A H -0.1784 0.2785 0.1987 0.037 Uiso 1 1 calc R . . H6B H -0.1618 0.3596 0.2693 0.037 Uiso 1 1 calc R . . C7 C 0.0780(3) 0.3914(3) 0.4663(3) 0.0295(12) Uani 1 1 d . . . C8 C -0.0711(3) 0.3343(3) 0.3863(3) 0.0270(11) Uani 1 1 d . . . H8 H -0.1194 0.3457 0.4003 0.032 Uiso 1 1 calc R . . C9 C -0.0557(3) 0.2655(3) 0.4171(3) 0.0272(11) Uani 1 1 d . . . H9 H -0.0928 0.2482 0.4497 0.033 Uiso 1 1 calc R . . C10 C -0.0998(3) 0.2164(3) 0.2793(3) 0.0254(11) Uani 1 1 d . . . C11 C 0.0796(3) 0.2786(3) 0.5195(3) 0.0292(12) Uani 1 1 d . . . H11A H 0.0368 0.2543 0.5445 0.035 Uiso 1 1 calc R . . H11B H 0.1313 0.3271 0.5610 0.035 Uiso 1 1 calc R . . C12 C -0.0898(3) 0.1118(3) 0.3418(3) 0.0324(12) Uani 1 1 d . . . H12A H -0.1212 0.0950 0.3777 0.039 Uiso 1 1 calc R . . H12B H -0.1264 0.0713 0.2881 0.039 Uiso 1 1 calc R . . C13 C 0.1919(3) 0.2264(3) 0.5038(3) 0.0296(12) Uani 1 1 d . . . C14 C 0.0445(3) 0.1252(3) 0.4428(3) 0.0295(12) Uani 1 1 d . . . H14 H 0.0062 0.1040 0.4733 0.035 Uiso 1 1 calc R . . C15 C 0.1054(3) 0.0806(3) 0.4350(3) 0.0264(11) Uani 1 1 d . . . H15 H 0.0959 0.0375 0.4608 0.032 Uiso 1 1 calc R . . C16 C 0.0119(3) 0.0513(3) 0.3079(3) 0.0310(12) Uani 1 1 d . . . C17 C 0.2705(4) 0.1350(4) 0.4982(3) 0.0345(13) Uani 1 1 d . . . H17A H 0.2538 0.0892 0.5198 0.041 Uiso 1 1 calc R . . H17B H 0.3168 0.1866 0.5412 0.041 Uiso 1 1 calc R . . C18 C 0.1032(4) -0.0266(4) 0.3150(3) 0.0357(13) Uani 1 1 d . . . H18A H 0.0616 -0.0605 0.2610 0.043 Uiso 1 1 calc R . . H18B H 0.0964 -0.0641 0.3460 0.043 Uiso 1 1 calc R . . C19 C 0.3870(3) 0.1622(3) 0.4359(3) 0.0317(12) Uani 1 1 d . . . C20 C 0.2700(3) 0.0249(3) 0.3798(3) 0.0265(11) Uani 1 1 d . . . H20 H 0.2570 -0.0183 0.4055 0.032 Uiso 1 1 calc R . . C21 C 0.3424(3) 0.0259(3) 0.3422(3) 0.0290(12) Uani 1 1 d . . . H21 H 0.3670 -0.0141 0.3529 0.035 Uiso 1 1 calc R . . C22 C 0.2103(3) -0.0126(3) 0.2435(3) 0.0317(12) Uani 1 1 d . . . C23 C 0.4924(3) 0.1461(3) 0.3670(3) 0.0302(12) Uani 1 1 d . . . H23A H 0.5353 0.1964 0.4131 0.036 Uiso 1 1 calc R . . H23B H 0.5142 0.1021 0.3626 0.036 Uiso 1 1 calc R . . C24 C 0.3317(3) -0.0223(3) 0.1968(3) 0.0306(12) Uani 1 1 d . . . H24A H 0.3721 -0.0464 0.2147 0.037 Uiso 1 1 calc R . . H24B H 0.2831 -0.0667 0.1497 0.037 Uiso 1 1 calc R . . C25 C 0.5252(3) 0.2506(3) 0.3001(3) 0.0270(11) Uani 1 1 d . . . C26 C 0.4729(3) 0.1098(3) 0.2204(3) 0.0261(11) Uani 1 1 d . . . H26 H 0.5114 0.0799 0.2238 0.031 Uiso 1 1 calc R . . C27 C 0.4938(3) 0.1670(3) 0.1705(3) 0.0227(10) Uani 1 1 d . . . H27 H 0.5422 0.1638 0.1508 0.027 Uiso 1 1 calc R . . C28 C 0.3489(3) 0.0604(3) 0.1071(3) 0.0285(12) Uani 1 1 d . . . C29 C 0.5619(3) 0.3286(3) 0.2102(3) 0.0270(11) Uani 1 1 d . . . H29A H 0.5989 0.3756 0.2607 0.032 Uiso 1 1 calc R . . H29B H 0.6011 0.3206 0.1806 0.032 Uiso 1 1 calc R . . C30 C 0.4030(3) 0.1557(3) 0.0364(3) 0.0286(12) Uani 1 1 d . . . H30A H 0.3525 0.1088 -0.0077 0.034 Uiso 1 1 calc R . . H30B H 0.4565 0.1637 0.0221 0.034 Uiso 1 1 calc R . . C31 C 0.4932(3) 0.4255(3) 0.1989(3) 0.0311(12) Uani 1 1 d . . . C32 C 0.4639(3) 0.3195(3) 0.0807(3) 0.0287(12) Uani 1 1 d . . . H32 H 0.5099 0.3233 0.0553 0.034 Uiso 1 1 calc R . . C33 C 0.4183(3) 0.3769(3) 0.0640(3) 0.0252(11) Uani 1 1 d . . . H33 H 0.4373 0.4027 0.0256 0.030 Uiso 1 1 calc R . . C34 C 0.3107(3) 0.2348(3) 0.0190(3) 0.0285(12) Uani 1 1 d . . . C35 C 0.4337(3) 0.5185(3) 0.1537(3) 0.0299(12) Uani 1 1 d . . . H35A H 0.4769 0.5609 0.2046 0.036 Uiso 1 1 calc R . . H35B H 0.4461 0.5412 0.1123 0.036 Uiso 1 1 calc R . . C36 C 0.2581(3) 0.3387(3) -0.0094(3) 0.0291(12) Uani 1 1 d . . . H36A H 0.2840 0.3730 -0.0393 0.035 Uiso 1 1 calc R . . H36B H 0.2080 0.2858 -0.0475 0.035 Uiso 1 1 calc R . . C37 C 0.3288(3) 0.5408(3) 0.2208(3) 0.0287(11) Uani 1 1 d . . . C38 C 0.2729(3) 0.4780(3) 0.0822(3) 0.0263(11) Uani 1 1 d . . . H38 H 0.2910 0.5073 0.0457 0.032 Uiso 1 1 calc R . . C39 C 0.2038(3) 0.5005(3) 0.1124(3) 0.0283(11) Uani 1 1 d . . . H39 H 0.1930 0.5441 0.0935 0.034 Uiso 1 1 calc R . . C40 C 0.1385(3) 0.3548(3) 0.0371(3) 0.0272(11) Uani 1 1 d . . . C41 C 0.2134(3) 0.5819(3) 0.2499(3) 0.0321(12) Uani 1 1 d . . . H41A H 0.1982 0.6197 0.2255 0.038 Uiso 1 1 calc R . . H41B H 0.2617 0.6179 0.3002 0.038 Uiso 1 1 calc R . . C42 C 0.0369(3) 0.4127(3) 0.0747(3) 0.0290(12) Uani 1 1 d . . . H42A H 0.0304 0.4592 0.0593 0.035 Uiso 1 1 calc R . . H42B H -0.0072 0.3586 0.0332 0.035 Uiso 1 1 calc R . . N1 N 0.1371(3) 0.5299(3) 0.2658(2) 0.0257(9) Uani 1 1 d . . . N2 N 0.0549(3) 0.4835(2) 0.3369(2) 0.0234(9) Uani 1 1 d . . . N3 N 0.0186(3) 0.4167(2) 0.1478(2) 0.0238(9) Uani 1 1 d . . . N4 N -0.0687(3) 0.3814(2) 0.2183(2) 0.0244(9) Uani 1 1 d . . . N5 N 0.0152(2) 0.4098(2) 0.4261(2) 0.0229(9) Uani 1 1 d . . . N6 N 0.0403(3) 0.3091(3) 0.4640(2) 0.0256(9) Uani 1 1 d . . . N7 N -0.0939(3) 0.2959(2) 0.3012(2) 0.0240(9) Uani 1 1 d . . . N8 N -0.0798(3) 0.1969(2) 0.3453(2) 0.0240(9) Uani 1 1 d . . . N9 N 0.1070(3) 0.2147(3) 0.4845(2) 0.0313(10) Uani 1 1 d . . . N10 N 0.1944(3) 0.1506(3) 0.4718(2) 0.0313(10) Uani 1 1 d . . . N11 N -0.0067(3) 0.1054(3) 0.3626(2) 0.0255(9) Uani 1 1 d . . . N12 N 0.0822(3) 0.0424(3) 0.3494(2) 0.0297(10) Uani 1 1 d . . . N13 N 0.3069(3) 0.1114(3) 0.4370(2) 0.0300(10) Uani 1 1 d . . . N14 N 0.4087(3) 0.1151(3) 0.3802(2) 0.0303(10) Uani 1 1 d . . . N15 N 0.1931(3) 0.0055(3) 0.3131(2) 0.0313(10) Uani 1 1 d . . . N16 N 0.2959(3) 0.0010(3) 0.2585(2) 0.0309(10) Uani 1 1 d . . . N17 N 0.4887(3) 0.1686(3) 0.2973(2) 0.0265(9) Uani 1 1 d . . . N18 N 0.5207(3) 0.2524(3) 0.2260(2) 0.0254(9) Uani 1 1 d . . . N19 N 0.3791(3) 0.0491(3) 0.1754(2) 0.0285(10) Uani 1 1 d . . . N20 N 0.4111(3) 0.1324(3) 0.1055(2) 0.0255(9) Uani 1 1 d . . . N21 N 0.5017(3) 0.3528(3) 0.1668(2) 0.0242(9) Uani 1 1 d . . . N22 N 0.4449(3) 0.4400(3) 0.1403(2) 0.0293(10) Uani 1 1 d . . . N23 N 0.3904(3) 0.2344(3) 0.0477(2) 0.0271(9) Uani 1 1 d . . . N24 N 0.3242(3) 0.3176(3) 0.0328(2) 0.0267(9) Uani 1 1 d . . . N25 N 0.3452(3) 0.5062(3) 0.1536(2) 0.0303(10) Uani 1 1 d . . . N26 N 0.2439(3) 0.5331(3) 0.1991(2) 0.0278(10) Uani 1 1 d . . . N27 N 0.2260(3) 0.3851(3) 0.0422(2) 0.0282(10) Uani 1 1 d . . . N28 N 0.1243(3) 0.4189(3) 0.0794(2) 0.0272(9) Uani 1 1 d . . . O1 O 0.2075(2) 0.5462(2) 0.3939(2) 0.0351(9) Uani 1 1 d . . . O2 O 0.1575(2) 0.4417(2) 0.5008(2) 0.0323(8) Uani 1 1 d . . . O3 O 0.2578(2) 0.2948(2) 0.5445(2) 0.0403(9) Uani 1 1 d . . . O4 O 0.4327(2) 0.2370(2) 0.4785(2) 0.0433(10) Uani 1 1 d . . . O5 O 0.5590(2) 0.3146(2) 0.3609(2) 0.0340(9) Uani 1 1 d . . . O6 O 0.5257(2) 0.4727(2) 0.2695(2) 0.0402(10) Uani 1 1 d . . . O7 O 0.3818(2) 0.5747(3) 0.2886(2) 0.0429(10) Uani 1 1 d . . . O8 O -0.0849(2) 0.2763(2) 0.1062(2) 0.0338(8) Uani 1 1 d . . . O9 O -0.1245(2) 0.1669(2) 0.20959(19) 0.0285(8) Uani 1 1 d . . . O10 O -0.0281(2) 0.0184(2) 0.2379(2) 0.0380(9) Uani 1 1 d . . . O11 O 0.1546(2) -0.0367(2) 0.1775(2) 0.0390(9) Uani 1 1 d . . . O12 O 0.2767(2) 0.0126(2) 0.0547(2) 0.0336(9) Uani 1 1 d . . . O13 O 0.2384(2) 0.1713(2) -0.0150(2) 0.0390(9) Uani 1 1 d . . . O14 O 0.0818(2) 0.2813(2) -0.0014(2) 0.0386(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl9 0.0312(8) 0.0486(10) 0.0630(11) 0.0063(8) 0.0111(7) 0.0085(7) Cl10 0.0856(13) 0.0519(11) 0.0396(10) 0.0095(8) 0.0131(9) 0.0061(10) O1W 0.037(2) 0.039(2) 0.036(2) 0.0074(18) 0.0118(18) 0.0149(19) O2W 0.042(2) 0.039(2) 0.037(2) 0.0065(19) 0.0021(18) 0.016(2) O3W 0.044(3) 0.058(3) 0.037(2) -0.016(2) 0.001(2) 0.019(2) O4W 0.034(2) 0.066(3) 0.032(2) 0.007(2) 0.0090(19) -0.007(2) O5W 0.090(4) 0.063(3) 0.038(3) 0.017(2) 0.015(2) 0.044(3) O6W 0.041(3) 0.082(4) 0.062(3) -0.020(3) 0.009(2) 0.025(3) O7W 0.038(2) 0.035(2) 0.027(2) 0.0026(17) 0.0168(17) 0.0085(18) O8W 0.042(2) 0.042(2) 0.033(2) 0.0007(19) 0.0026(18) 0.018(2) O9W 0.060(3) 0.028(2) 0.031(2) 0.0033(18) 0.003(2) 0.012(2) O10W 0.056(3) 0.053(3) 0.041(2) 0.000(2) 0.011(2) 0.031(2) O11W 0.035(2) 0.073(3) 0.033(2) -0.010(2) -0.0062(19) 0.021(2) O12W 0.028(2) 0.118(4) 0.034(2) 0.025(3) 0.0045(19) 0.013(3) Cl1 0.0358(8) 0.0506(9) 0.0595(10) 0.0283(8) 0.0159(7) 0.0155(7) Cl2 0.0576(10) 0.0538(10) 0.0403(9) 0.0174(8) 0.0172(8) 0.0252(8) Cl3 0.0691(11) 0.0521(10) 0.0586(10) 0.0126(8) 0.0341(9) 0.0339(9) Cl4 0.0364(8) 0.1096(15) 0.0519(10) 0.0464(11) 0.0193(8) 0.0281(9) Cl5 0.0793(12) 0.0352(9) 0.0693(12) 0.0106(8) 0.0322(10) 0.0199(9) Cl6 0.1165(16) 0.0371(9) 0.0529(11) 0.0131(8) 0.0493(11) 0.0243(10) Cl7 0.198(3) 0.0688(14) 0.0530(12) 0.0278(11) 0.0570(15) 0.0702(17) Cl8 0.0781(15) 0.109(2) 0.132(2) 0.0690(18) 0.0504(15) 0.0360(14) Zn1 0.0396(4) 0.0533(5) 0.0400(4) 0.0224(4) 0.0184(3) 0.0205(3) Zn2 0.0847(6) 0.0407(4) 0.0488(5) 0.0175(4) 0.0311(4) 0.0275(4) La1 0.02090(16) 0.02932(18) 0.01957(16) -0.00512(13) 0.00192(12) 0.00183(13) La2 0.02210(16) 0.02440(17) 0.01618(15) -0.00326(12) 0.00042(12) 0.00479(13) C1 0.031(3) 0.017(3) 0.018(3) -0.003(2) 0.004(2) 0.006(2) C2 0.023(3) 0.024(3) 0.019(3) -0.005(2) 0.005(2) 0.004(2) C3 0.029(3) 0.017(3) 0.020(3) -0.001(2) 0.002(2) 0.006(2) C4 0.023(3) 0.033(3) 0.018(3) 0.005(2) 0.006(2) 0.012(2) C5 0.030(3) 0.032(3) 0.016(3) -0.004(2) 0.006(2) 0.008(2) C6 0.024(3) 0.032(3) 0.020(3) 0.000(2) 0.003(2) 0.004(2) C7 0.032(3) 0.037(3) 0.012(2) 0.004(2) 0.009(2) 0.010(3) C8 0.026(3) 0.030(3) 0.022(3) 0.005(2) 0.012(2) 0.011(2) C9 0.026(3) 0.029(3) 0.016(2) 0.001(2) 0.007(2) 0.007(2) C10 0.013(2) 0.028(3) 0.022(3) 0.001(2) 0.003(2) 0.002(2) C11 0.028(3) 0.032(3) 0.016(3) -0.001(2) 0.004(2) 0.010(2) C12 0.027(3) 0.026(3) 0.026(3) 0.000(2) 0.002(2) 0.001(2) C13 0.030(3) 0.026(3) 0.017(3) -0.001(2) 0.004(2) 0.004(2) C14 0.029(3) 0.026(3) 0.022(3) 0.000(2) 0.007(2) 0.006(2) C15 0.029(3) 0.023(3) 0.020(3) 0.008(2) 0.007(2) 0.004(2) C16 0.026(3) 0.035(3) 0.021(3) 0.009(2) 0.002(2) 0.005(2) C17 0.035(3) 0.043(3) 0.014(3) -0.003(2) 0.001(2) 0.018(3) C18 0.035(3) 0.035(3) 0.024(3) -0.004(2) 0.005(2) 0.013(3) C19 0.027(3) 0.033(3) 0.019(3) 0.007(3) -0.001(2) 0.001(2) C20 0.028(3) 0.024(3) 0.018(3) 0.002(2) 0.007(2) 0.005(2) C21 0.030(3) 0.020(3) 0.024(3) 0.000(2) 0.009(2) 0.002(2) C22 0.032(3) 0.021(3) 0.024(3) 0.001(2) 0.002(2) 0.002(2) C23 0.026(3) 0.037(3) 0.014(2) 0.001(2) 0.001(2) 0.008(2) C24 0.032(3) 0.022(3) 0.027(3) 0.001(2) 0.011(2) 0.004(2) C25 0.017(2) 0.025(3) 0.020(3) -0.006(2) 0.000(2) 0.001(2) C26 0.025(3) 0.022(3) 0.018(3) -0.002(2) 0.004(2) 0.004(2) C27 0.023(2) 0.018(3) 0.015(2) -0.002(2) 0.002(2) 0.004(2) C28 0.031(3) 0.025(3) 0.022(3) 0.001(2) 0.006(2) 0.011(2) C29 0.024(3) 0.023(3) 0.021(3) 0.003(2) 0.006(2) 0.000(2) C30 0.032(3) 0.026(3) 0.018(3) 0.000(2) 0.005(2) 0.009(2) C31 0.024(3) 0.028(3) 0.026(3) -0.003(2) 0.003(2) 0.006(2) C32 0.025(3) 0.031(3) 0.025(3) 0.005(2) 0.008(2) 0.010(2) C33 0.020(2) 0.027(3) 0.019(3) 0.001(2) 0.005(2) 0.005(2) C34 0.027(3) 0.031(3) 0.017(3) 0.001(2) 0.004(2) 0.008(2) C35 0.022(3) 0.027(3) 0.030(3) 0.002(2) 0.010(2) 0.003(2) C36 0.025(3) 0.033(3) 0.025(3) 0.006(2) 0.009(2) 0.011(2) C37 0.029(3) 0.026(3) 0.022(3) 0.005(2) 0.005(2) 0.005(2) C38 0.024(3) 0.023(3) 0.024(3) 0.004(2) 0.010(2) 0.005(2) C39 0.023(3) 0.032(3) 0.026(3) 0.008(2) 0.007(2) 0.011(2) C40 0.023(3) 0.035(3) 0.013(2) 0.006(2) 0.005(2) 0.003(2) C41 0.031(3) 0.025(3) 0.024(3) 0.000(2) 0.004(2) 0.002(2) C42 0.022(3) 0.031(3) 0.018(3) 0.004(2) 0.005(2) -0.001(2) N1 0.022(2) 0.028(2) 0.018(2) 0.0018(18) 0.0064(18) 0.0052(18) N2 0.020(2) 0.022(2) 0.015(2) -0.0019(17) 0.0038(17) 0.0027(18) N3 0.021(2) 0.019(2) 0.013(2) -0.0070(17) 0.0024(17) -0.0013(17) N4 0.024(2) 0.017(2) 0.018(2) -0.0042(17) 0.0060(18) 0.0012(17) N5 0.021(2) 0.019(2) 0.013(2) 0.0000(17) -0.0019(17) -0.0004(17) N6 0.024(2) 0.025(2) 0.017(2) 0.0040(18) -0.0011(17) 0.0042(19) N7 0.025(2) 0.022(2) 0.015(2) -0.0005(17) -0.0005(17) 0.0082(18) N8 0.024(2) 0.018(2) 0.016(2) -0.0013(17) -0.0010(17) 0.0035(18) N9 0.025(2) 0.028(2) 0.026(2) -0.003(2) 0.0043(19) 0.0061(19) N10 0.025(2) 0.026(2) 0.022(2) -0.0051(19) 0.0005(19) 0.0000(19) N11 0.024(2) 0.023(2) 0.013(2) -0.0016(18) -0.0018(17) 0.0031(18) N12 0.032(2) 0.027(2) 0.016(2) -0.0058(18) 0.0024(19) 0.008(2) N13 0.021(2) 0.026(2) 0.022(2) -0.0049(19) -0.0001(18) 0.0014(19) N14 0.023(2) 0.025(2) 0.020(2) -0.0048(19) 0.0042(18) -0.0032(19) N15 0.026(2) 0.034(3) 0.019(2) 0.002(2) 0.0028(19) 0.005(2) N16 0.025(2) 0.036(3) 0.014(2) -0.0013(19) 0.0031(18) 0.003(2) N17 0.029(2) 0.025(2) 0.018(2) 0.0062(18) 0.0057(18) 0.0048(19) N18 0.026(2) 0.024(2) 0.014(2) -0.0015(18) 0.0017(18) 0.0058(19) N19 0.026(2) 0.022(2) 0.028(2) 0.008(2) 0.0058(19) 0.0019(19) N20 0.022(2) 0.028(2) 0.017(2) 0.0035(18) 0.0017(17) 0.0055(19) N21 0.024(2) 0.024(2) 0.017(2) 0.0040(18) 0.0018(17) 0.0070(18) N22 0.026(2) 0.022(2) 0.026(2) -0.0018(19) 0.0020(19) 0.0056(19) N23 0.024(2) 0.020(2) 0.022(2) -0.0009(18) 0.0019(18) 0.0017(18) N24 0.021(2) 0.025(2) 0.021(2) 0.0013(19) 0.0033(18) 0.0031(18) N25 0.021(2) 0.030(2) 0.024(2) -0.002(2) 0.0012(19) 0.0056(19) N26 0.024(2) 0.033(2) 0.017(2) 0.0003(19) 0.0067(18) 0.0075(19) N27 0.025(2) 0.023(2) 0.023(2) -0.0011(19) 0.0040(19) 0.0034(19) N28 0.019(2) 0.027(2) 0.024(2) 0.0010(19) 0.0086(18) 0.0010(18) O1 0.029(2) 0.041(2) 0.0187(19) 0.0028(17) -0.0028(16) 0.0086(17) O2 0.0173(18) 0.031(2) 0.0257(19) -0.0006(16) -0.0013(15) -0.0016(16) O3 0.031(2) 0.032(2) 0.034(2) -0.0062(18) -0.0004(18) 0.0061(18) O4 0.033(2) 0.027(2) 0.037(2) -0.0110(19) 0.0025(18) -0.0013(18) O5 0.0242(19) 0.035(2) 0.024(2) -0.0022(17) 0.0015(16) 0.0045(17) O6 0.042(2) 0.039(2) 0.021(2) -0.0072(18) -0.0016(17) 0.0163(19) O7 0.035(2) 0.050(3) 0.024(2) -0.0037(19) 0.0015(18) 0.012(2) O8 0.031(2) 0.029(2) 0.0216(19) -0.0045(17) 0.0089(16) 0.0014(17) O9 0.0269(19) 0.0270(19) 0.0179(18) -0.0029(16) 0.0016(15) 0.0075(16) O10 0.041(2) 0.037(2) 0.019(2) -0.0025(17) 0.0000(17) 0.0138(19) O11 0.039(2) 0.037(2) 0.0139(18) -0.0068(16) -0.0052(17) 0.0061(18) O12 0.0254(19) 0.0224(19) 0.0227(19) -0.0056(16) -0.0054(16) -0.0054(16) O13 0.026(2) 0.027(2) 0.042(2) -0.0034(18) 0.0044(18) 0.0020(17) O14 0.028(2) 0.025(2) 0.040(2) -0.0061(18) 0.0077(18) 0.0007(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1W La1 2.587(4) . ? O2W La1 2.532(4) . ? O3W La1 2.495(4) . ? O4W La1 2.538(4) . ? O5W La1 2.558(4) . ? O6W La1 2.572(4) . ? O7W La2 2.558(4) . ? O8W La2 2.581(4) . ? O9W La2 2.541(4) . ? O10W La2 2.594(4) . ? O11W La2 2.517(4) . ? O12W La2 2.577(4) . ? Cl1 Zn1 2.2737(15) . ? Cl2 Zn1 2.2629(17) . ? Cl3 Zn1 2.2716(18) . ? Cl4 Zn1 2.2771(17) . ? Cl5 Zn2 2.232(2) . ? Cl6 Zn2 2.2683(17) . ? Cl7 Zn2 2.269(2) . ? Cl8 Zn2 2.276(3) . ? La1 O1 2.530(3) . ? La1 O2 2.571(3) . ? La1 O5 2.577(3) 2_666 ? La2 O12 2.523(3) 2 ? La2 O9 2.529(3) . ? La2 O8 2.540(4) . ? C1 O1 1.240(6) . ? C1 N1 1.358(6) . ? C1 N2 1.366(6) . ? C2 N1 1.451(6) . ? C2 N3 1.464(6) . ? C2 C3 1.556(7) . ? C2 H2 0.9900 . ? C3 N4 1.443(6) . ? C3 N2 1.446(6) . ? C3 H3 0.9900 . ? C4 O8 1.240(6) . ? C4 N3 1.363(6) . ? C4 N4 1.364(6) . ? C5 N5 1.419(6) . ? C5 N2 1.449(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.445(6) . ? C6 N7 1.455(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.242(6) . ? C7 N5 1.363(6) . ? C7 N6 1.369(7) . ? C8 N7 1.456(6) . ? C8 N5 1.474(6) . ? C8 C9 1.561(7) . ? C8 H8 0.9900 . ? C9 N8 1.429(6) . ? C9 N6 1.485(6) . ? C9 H9 0.9900 . ? C10 O9 1.250(6) . ? C10 N7 1.342(6) . ? C10 N8 1.360(6) . ? C11 N6 1.431(6) . ? C11 N9 1.449(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.446(6) . ? C12 N8 1.459(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.239(6) . ? C13 N9 1.347(6) . ? C13 N10 1.362(6) . ? C14 N11 1.436(6) . ? C14 N9 1.457(6) . ? C14 C15 1.533(7) . ? C14 H14 0.9900 . ? C15 N10 1.460(6) . ? C15 N12 1.462(6) . ? C15 H15 0.9900 . ? C16 O10 1.204(6) . ? C16 N12 1.367(6) . ? C16 N11 1.393(6) . ? C17 N10 1.440(6) . ? C17 N13 1.450(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.447(6) . ? C18 N15 1.451(7) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.224(6) . ? C19 N13 1.358(6) . ? C19 N14 1.368(7) . ? C20 N13 1.458(6) . ? C20 N15 1.466(6) . ? C20 C21 1.545(7) . ? C20 H20 0.9900 . ? C21 N16 1.454(6) . ? C21 N14 1.465(6) . ? C21 H21 0.9900 . ? C22 O11 1.238(6) . ? C22 N16 1.351(7) . ? C22 N15 1.370(7) . ? C23 N17 1.439(6) . ? C23 N14 1.440(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N19 1.450(6) . ? C24 N16 1.449(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O5 1.236(6) . ? C25 N17 1.360(6) . ? C25 N18 1.366(6) . ? C26 N17 1.450(6) . ? C26 N19 1.479(6) . ? C26 C27 1.544(7) . ? C26 H26 0.9900 . ? C27 N20 1.454(6) . ? C27 N18 1.459(6) . ? C27 H27 0.9900 . ? C28 O12 1.234(6) . ? C28 N19 1.354(6) . ? C28 N20 1.362(6) . ? C29 N21 1.427(6) . ? C29 N18 1.432(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N20 1.437(6) . ? C30 N23 1.474(6) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O6 1.240(6) . ? C31 N22 1.357(6) . ? C31 N21 1.366(6) . ? C32 N23 1.459(6) . ? C32 N21 1.459(6) . ? C32 C33 1.546(7) . ? C32 H32 0.9900 . ? C33 N22 1.431(6) . ? C33 N24 1.463(6) . ? C33 H33 0.9900 . ? C34 O13 1.237(6) . ? C34 N23 1.359(6) . ? C34 N24 1.367(6) . ? C35 N25 1.452(6) . ? C35 N22 1.457(6) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N27 1.437(6) . ? C36 N24 1.453(6) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 O7 1.229(6) . ? C37 N26 1.369(6) . ? C37 N25 1.378(6) . ? C38 N25 1.436(6) . ? C38 N27 1.466(6) . ? C38 C39 1.544(7) . ? C38 H38 0.9900 . ? C39 N28 1.466(6) . ? C39 N26 1.473(6) . ? C39 H39 0.9900 . ? C40 O14 1.229(6) . ? C40 N28 1.353(6) . ? C40 N27 1.373(6) . ? C41 N26 1.434(6) . ? C41 N1 1.447(6) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 N3 1.442(6) . ? C42 N28 1.444(6) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? O5 La1 2.577(3) 2_666 ? O12 La2 2.523(3) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 Zn1 Cl3 111.58(7) . . ? Cl2 Zn1 Cl1 107.29(6) . . ? Cl3 Zn1 Cl1 107.46(7) . . ? Cl2 Zn1 Cl4 109.09(7) . . ? Cl3 Zn1 Cl4 109.46(7) . . ? Cl1 Zn1 Cl4 111.96(6) . . ? Cl5 Zn2 Cl6 105.33(7) . . ? Cl5 Zn2 Cl7 110.27(9) . . ? Cl6 Zn2 Cl7 113.74(8) . . ? Cl5 Zn2 Cl8 114.88(9) . . ? Cl6 Zn2 Cl8 109.48(10) . . ? Cl7 Zn2 Cl8 103.41(11) . . ? O3W La1 O1 71.91(13) . . ? O3W La1 O2W 81.42(14) . . ? O1 La1 O2W 139.06(12) . . ? O3W La1 O4W 85.00(16) . . ? O1 La1 O4W 68.78(13) . . ? O2W La1 O4W 139.91(14) . . ? O3W La1 O5W 140.00(14) . . ? O1 La1 O5W 68.60(13) . . ? O2W La1 O5W 134.71(13) . . ? O4W La1 O5W 75.23(16) . . ? O3W La1 O2 73.03(13) . . ? O1 La1 O2 74.70(12) . . ? O2W La1 O2 68.02(12) . . ? O4W La1 O2 141.74(12) . . ? O5W La1 O2 101.94(14) . . ? O3W La1 O6W 69.04(14) . . ? O1 La1 O6W 125.27(14) . . ? O2W La1 O6W 68.89(16) . . ? O4W La1 O6W 71.02(17) . . ? O5W La1 O6W 132.15(17) . . ? O2 La1 O6W 125.53(15) . . ? O3W La1 O5 134.88(12) . 2_666 ? O1 La1 O5 135.40(12) . 2_666 ? O2W La1 O5 85.24(12) . 2_666 ? O4W La1 O5 78.13(12) . 2_666 ? O5W La1 O5 74.77(13) . 2_666 ? O2 La1 O5 138.92(11) . 2_666 ? O6W La1 O5 65.93(13) . 2_666 ? O3W La1 O1W 139.46(14) . . ? O1 La1 O1W 111.14(11) . . ? O2W La1 O1W 70.98(12) . . ? O4W La1 O1W 134.88(14) . . ? O5W La1 O1W 64.41(13) . . ? O2 La1 O1W 69.39(12) . . ? O6W La1 O1W 123.51(14) . . ? O5 La1 O1W 72.73(11) 2_666 . ? O11W La2 O12 134.31(12) . 2 ? O11W La2 O9 71.11(12) . . ? O12 La2 O9 135.42(11) 2 . ? O11W La2 O8 73.93(13) . . ? O12 La2 O8 139.28(11) 2 . ? O9 La2 O8 74.66(11) . . ? O11W La2 O9W 83.24(15) . . ? O12 La2 O9W 77.89(12) 2 . ? O9 La2 O9W 69.08(11) . . ? O8 La2 O9W 141.80(11) . . ? O11W La2 O7W 80.67(14) . . ? O12 La2 O7W 86.52(12) 2 . ? O9 La2 O7W 137.94(11) . . ? O8 La2 O7W 67.82(11) . . ? O9W La2 O7W 138.38(12) . . ? O11W La2 O12W 137.68(13) . . ? O12 La2 O12W 76.84(13) 2 . ? O9 La2 O12W 67.06(12) . . ? O8 La2 O12W 100.46(15) . . ? O9W La2 O12W 76.34(15) . . ? O7W La2 O12W 137.17(13) . . ? O11W La2 O8W 138.93(15) . . ? O12 La2 O8W 72.45(12) 2 . ? O9 La2 O8W 114.22(11) . . ? O8 La2 O8W 69.15(12) . . ? O9W La2 O8W 137.67(13) . . ? O7W La2 O8W 69.33(12) . . ? O12W La2 O8W 68.07(14) . . ? O11W La2 O10W 67.74(13) . . ? O12 La2 O10W 66.70(12) 2 . ? O9 La2 O10W 123.49(12) . . ? O8 La2 O10W 125.70(13) . . ? O9W La2 O10W 69.17(14) . . ? O7W La2 O10W 69.22(13) . . ? O12W La2 O10W 133.75(16) . . ? O8W La2 O10W 122.28(12) . . ? O1 C1 N1 125.9(5) . . ? O1 C1 N2 125.2(5) . . ? N1 C1 N2 108.9(4) . . ? N1 C2 N3 114.0(4) . . ? N1 C2 C3 103.6(4) . . ? N3 C2 C3 103.7(4) . . ? N1 C2 H2 111.7 . . ? N3 C2 H2 111.7 . . ? C3 C2 H2 111.7 . . ? N4 C3 N2 114.6(4) . . ? N4 C3 C2 102.5(4) . . ? N2 C3 C2 102.6(4) . . ? N4 C3 H3 112.1 . . ? N2 C3 H3 112.1 . . ? C2 C3 H3 112.1 . . ? O8 C4 N3 125.2(4) . . ? O8 C4 N4 125.9(5) . . ? N3 C4 N4 108.8(4) . . ? N5 C5 N2 115.2(4) . . ? N5 C5 H5A 108.5 . . ? N2 C5 H5A 108.5 . . ? N5 C5 H5B 108.5 . . ? N2 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? N4 C6 N7 113.3(4) . . ? N4 C6 H6A 108.9 . . ? N7 C6 H6A 108.9 . . ? N4 C6 H6B 108.9 . . ? N7 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N5 125.3(5) . . ? O2 C7 N6 124.8(5) . . ? N5 C7 N6 109.8(4) . . ? N7 C8 N5 114.9(4) . . ? N7 C8 C9 103.0(4) . . ? N5 C8 C9 103.2(4) . . ? N7 C8 H8 111.7 . . ? N5 C8 H8 111.7 . . ? C9 C8 H8 111.7 . . ? N8 C9 N6 114.9(4) . . ? N8 C9 C8 102.3(4) . . ? N6 C9 C8 103.0(4) . . ? N8 C9 H9 112.0 . . ? N6 C9 H9 112.0 . . ? C8 C9 H9 112.0 . . ? O9 C10 N7 125.4(5) . . ? O9 C10 N8 125.8(5) . . ? N7 C10 N8 108.7(4) . . ? N6 C11 N9 113.9(4) . . ? N6 C11 H11A 108.8 . . ? N9 C11 H11A 108.8 . . ? N6 C11 H11B 108.8 . . ? N9 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? N11 C12 N8 113.9(4) . . ? N11 C12 H12A 108.8 . . ? N8 C12 H12A 108.8 . . ? N11 C12 H12B 108.8 . . ? N8 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N9 125.9(5) . . ? O3 C13 N10 125.0(5) . . ? N9 C13 N10 109.1(4) . . ? N11 C14 N9 114.7(4) . . ? N11 C14 C15 104.2(4) . . ? N9 C14 C15 102.9(4) . . ? N11 C14 H14 111.5 . . ? N9 C14 H14 111.5 . . ? C15 C14 H14 111.5 . . ? N10 C15 N12 112.3(4) . . ? N10 C15 C14 103.8(4) . . ? N12 C15 C14 103.0(4) . . ? N10 C15 H15 112.3 . . ? N12 C15 H15 112.3 . . ? C14 C15 H15 112.3 . . ? O10 C16 N12 127.5(5) . . ? O10 C16 N11 125.6(5) . . ? N12 C16 N11 106.8(4) . . ? N10 C17 N13 114.4(4) . . ? N10 C17 H17A 108.7 . . ? N13 C17 H17A 108.7 . . ? N10 C17 H17B 108.7 . . ? N13 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? N12 C18 N15 111.4(4) . . ? N12 C18 H18A 109.4 . . ? N15 C18 H18A 109.4 . . ? N12 C18 H18B 109.4 . . ? N15 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? O4 C19 N13 125.7(5) . . ? O4 C19 N14 125.8(5) . . ? N13 C19 N14 108.5(4) . . ? N13 C20 N15 113.2(4) . . ? N13 C20 C21 103.8(4) . . ? N15 C20 C21 103.8(4) . . ? N13 C20 H20 111.8 . . ? N15 C20 H20 111.8 . . ? C21 C20 H20 111.8 . . ? N16 C21 N14 114.5(4) . . ? N16 C21 C20 103.0(4) . . ? N14 C21 C20 102.5(4) . . ? N16 C21 H21 112.0 . . ? N14 C21 H21 112.0 . . ? C20 C21 H21 112.0 . . ? O11 C22 N16 126.4(5) . . ? O11 C22 N15 123.8(5) . . ? N16 C22 N15 109.8(4) . . ? N17 C23 N14 114.2(4) . . ? N17 C23 H23A 108.7 . . ? N14 C23 H23A 108.7 . . ? N17 C23 H23B 108.7 . . ? N14 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? N19 C24 N16 113.2(4) . . ? N19 C24 H24A 108.9 . . ? N16 C24 H24A 108.9 . . ? N19 C24 H24B 108.9 . . ? N16 C24 H24B 108.9 . . ? H24A C24 H24B 107.8 . . ? O5 C25 N17 125.0(5) . . ? O5 C25 N18 124.6(5) . . ? N17 C25 N18 110.4(4) . . ? N17 C26 N19 115.4(4) . . ? N17 C26 C27 104.1(4) . . ? N19 C26 C27 102.3(4) . . ? N17 C26 H26 111.5 . . ? N19 C26 H26 111.5 . . ? C27 C26 H26 111.5 . . ? N20 C27 N18 115.6(4) . . ? N20 C27 C26 103.9(4) . . ? N18 C27 C26 103.5(4) . . ? N20 C27 H27 111.1 . . ? N18 C27 H27 111.1 . . ? C26 C27 H27 111.1 . . ? O12 C28 N19 125.2(5) . . ? O12 C28 N20 125.8(5) . . ? N19 C28 N20 109.0(4) . . ? N21 C29 N18 114.7(4) . . ? N21 C29 H29A 108.6 . . ? N18 C29 H29A 108.6 . . ? N21 C29 H29B 108.6 . . ? N18 C29 H29B 108.6 . . ? H29A C29 H29B 107.6 . . ? N20 C30 N23 113.0(4) . . ? N20 C30 H30A 109.0 . . ? N23 C30 H30A 109.0 . . ? N20 C30 H30B 109.0 . . ? N23 C30 H30B 109.0 . . ? H30A C30 H30B 107.8 . . ? O6 C31 N22 124.6(5) . . ? O6 C31 N21 126.5(5) . . ? N22 C31 N21 108.8(4) . . ? N23 C32 N21 114.1(4) . . ? N23 C32 C33 103.0(4) . . ? N21 C32 C33 103.0(4) . . ? N23 C32 H32 112.0 . . ? N21 C32 H32 112.0 . . ? C33 C32 H32 112.0 . . ? N22 C33 N24 114.0(4) . . ? N22 C33 C32 103.4(4) . . ? N24 C33 C32 102.9(4) . . ? N22 C33 H33 112.0 . . ? N24 C33 H33 112.0 . . ? C32 C33 H33 112.0 . . ? O13 C34 N23 126.2(5) . . ? O13 C34 N24 125.6(4) . . ? N23 C34 N24 108.2(4) . . ? N25 C35 N22 112.9(4) . . ? N25 C35 H35A 109.0 . . ? N22 C35 H35A 109.0 . . ? N25 C35 H35B 109.0 . . ? N22 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? N27 C36 N24 112.9(4) . . ? N27 C36 H36A 109.0 . . ? N24 C36 H36A 109.0 . . ? N27 C36 H36B 109.0 . . ? N24 C36 H36B 109.0 . . ? H36A C36 H36B 107.8 . . ? O7 C37 N26 125.5(5) . . ? O7 C37 N25 126.0(5) . . ? N26 C37 N25 108.5(4) . . ? N25 C38 N27 114.5(4) . . ? N25 C38 C39 103.2(4) . . ? N27 C38 C39 103.1(4) . . ? N25 C38 H38 111.8 . . ? N27 C38 H38 111.8 . . ? C39 C38 H38 111.8 . . ? N28 C39 N26 114.6(4) . . ? N28 C39 C38 103.5(4) . . ? N26 C39 C38 104.0(4) . . ? N28 C39 H39 111.4 . . ? N26 C39 H39 111.4 . . ? C38 C39 H39 111.4 . . ? O14 C40 N28 125.6(5) . . ? O14 C40 N27 125.1(5) . . ? N28 C40 N27 109.3(4) . . ? N26 C41 N1 113.5(4) . . ? N26 C41 H41A 108.9 . . ? N1 C41 H41A 108.9 . . ? N26 C41 H41B 108.9 . . ? N1 C41 H41B 108.9 . . ? H41A C41 H41B 107.7 . . ? N3 C42 N28 113.7(4) . . ? N3 C42 H42A 108.8 . . ? N28 C42 H42A 108.8 . . ? N3 C42 H42B 108.8 . . ? N28 C42 H42B 108.8 . . ? H42A C42 H42B 107.7 . . ? C1 N1 C41 123.9(4) . . ? C1 N1 C2 112.0(4) . . ? C41 N1 C2 122.9(4) . . ? C1 N2 C3 112.5(4) . . ? C1 N2 C5 121.7(4) . . ? C3 N2 C5 122.1(4) . . ? C4 N3 C42 122.2(4) . . ? C4 N3 C2 111.4(4) . . ? C42 N3 C2 123.7(4) . . ? C4 N4 C3 113.2(4) . . ? C4 N4 C6 123.2(4) . . ? C3 N4 C6 122.8(4) . . ? C7 N5 C5 123.3(4) . . ? C7 N5 C8 112.0(4) . . ? C5 N5 C8 123.3(4) . . ? C7 N6 C11 123.3(4) . . ? C7 N6 C9 111.5(4) . . ? C11 N6 C9 122.3(4) . . ? C10 N7 C6 121.7(4) . . ? C10 N7 C8 112.3(4) . . ? C6 N7 C8 123.4(4) . . ? C10 N8 C9 113.5(4) . . ? C10 N8 C12 122.6(4) . . ? C9 N8 C12 123.7(4) . . ? C13 N9 C11 123.3(4) . . ? C13 N9 C14 112.6(4) . . ? C11 N9 C14 122.1(4) . . ? C13 N10 C17 123.0(4) . . ? C13 N10 C15 111.3(4) . . ? C17 N10 C15 121.1(4) . . ? C16 N11 C14 112.6(4) . . ? C16 N11 C12 120.6(4) . . ? C14 N11 C12 122.7(4) . . ? C16 N12 C18 120.8(4) . . ? C16 N12 C15 112.8(4) . . ? C18 N12 C15 121.3(4) . . ? C19 N13 C17 123.5(4) . . ? C19 N13 C20 112.4(4) . . ? C17 N13 C20 123.0(4) . . ? C19 N14 C23 124.0(4) . . ? C19 N14 C21 112.6(4) . . ? C23 N14 C21 122.9(4) . . ? C22 N15 C18 121.6(4) . . ? C22 N15 C20 110.6(4) . . ? C18 N15 C20 122.8(4) . . ? C22 N16 C24 123.0(4) . . ? C22 N16 C21 112.4(4) . . ? C24 N16 C21 123.7(4) . . ? C25 N17 C23 123.2(4) . . ? C25 N17 C26 110.5(4) . . ? C23 N17 C26 123.6(4) . . ? C25 N18 C29 123.9(4) . . ? C25 N18 C27 110.3(4) . . ? C29 N18 C27 123.2(4) . . ? C28 N19 C24 124.6(4) . . ? C28 N19 C26 112.1(4) . . ? C24 N19 C26 122.5(4) . . ? C28 N20 C30 122.0(4) . . ? C28 N20 C27 112.0(4) . . ? C30 N20 C27 123.8(4) . . ? C31 N21 C29 122.3(4) . . ? C31 N21 C32 111.3(4) . . ? C29 N21 C32 124.0(4) . . ? C31 N22 C33 112.8(4) . . ? C31 N22 C35 122.2(4) . . ? C33 N22 C35 124.3(4) . . ? C34 N23 C32 112.9(4) . . ? C34 N23 C30 123.5(4) . . ? C32 N23 C30 123.1(4) . . ? C34 N24 C36 121.4(4) . . ? C34 N24 C33 112.3(4) . . ? C36 N24 C33 121.3(4) . . ? C37 N25 C38 113.1(4) . . ? C37 N25 C35 122.4(4) . . ? C38 N25 C35 122.5(4) . . ? C37 N26 C41 122.6(4) . . ? C37 N26 C39 110.8(4) . . ? C41 N26 C39 121.8(4) . . ? C40 N27 C36 122.7(4) . . ? C40 N27 C38 111.5(4) . . ? C36 N27 C38 122.0(4) . . ? C40 N28 C42 123.1(4) . . ? C40 N28 C39 112.0(4) . . ? C42 N28 C39 123.0(4) . . ? C1 O1 La1 160.6(4) . . ? C7 O2 La1 157.4(3) . . ? C25 O5 La1 153.5(3) . 2_666 ? C4 O8 La2 156.8(3) . . ? C10 O9 La2 160.6(3) . . ? C28 O12 La2 160.6(3) . 2 ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.672 _refine_diff_density_min -1.252 _refine_diff_density_rms 0.119 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.270 0.000 0.685 1176 487 ' ' 2 0.233 0.264 0.254 179 71 ' ' 3 0.766 0.736 0.746 179 66 ' ' _platon_squeeze_details ; ; data_p2 _database_code_depnum_ccdc_archive 'CCDC 905583' #TrackingRef '10 (905583).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H49 Cl5 N14 O21 Yb Zn' _chemical_formula_weight 1249.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.473(4) _cell_length_b 18.878(3) _cell_length_c 19.864(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.752(4) _cell_angle_gamma 90.00 _cell_volume 9600(2) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.729 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5008 _exptl_absorpt_coefficient_mu 2.798 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5911 _exptl_absorpt_correction_T_max 0.6954 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44856 _diffrn_reflns_av_R_equivalents 0.0613 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9344 _reflns_number_gt 7389 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1198P)^2^+28.8532P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9344 _refine_ls_number_parameters 487 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1948 _refine_ls_wR_factor_gt 0.1815 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.121 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl5 Cl 1.2243(2) 0.2216(3) 0.6418(3) 0.1356(18) Uani 1 1 d . . . Cl1 Cl 1.32575(9) 0.34713(12) 0.79717(14) 0.0627(6) Uani 1 1 d . . . Cl2 Cl 1.31481(15) 0.53630(16) 0.7466(3) 0.1147(15) Uani 1 1 d . . . Cl3 Cl 1.3727(6) 0.4716(7) 0.9293(6) 0.186(6) Uani 1 1 d U . . Cl4 Cl 1.44314(19) 0.4463(2) 0.7962(6) 0.179(6) Uani 1 1 d . . . Zn1 Zn 1.36507(7) 0.45157(9) 0.80567(19) 0.1675(13) Uani 1 1 d . . . O1W O 1.1133(2) 0.6074(3) 0.5212(2) 0.0485(14) Uani 1 1 d . . . O2W O 1.1509(2) 0.7585(4) 0.5629(3) 0.0570(16) Uani 1 1 d . . . O3W O 1.0387(2) 0.6344(3) 0.4029(3) 0.0534(15) Uani 1 1 d . . . O4W O 0.9873(2) 0.6976(3) 0.4950(3) 0.0509(14) Uani 1 1 d . . . O5W O 1.0556(2) 0.8251(3) 0.5373(3) 0.0547(15) Uani 1 1 d . . . Yb1 Yb 1.072315(11) 0.713927(15) 0.494483(14) 0.03030(14) Uani 1 1 d . . . C1 C 1.0800(3) 0.7028(3) 0.6716(4) 0.0289(14) Uani 1 1 d . . . C2 C 1.0732(3) 0.7620(4) 0.7729(4) 0.0307(14) Uani 1 1 d . . . H2 H 1.0809 0.8132 0.7801 0.037 Uiso 1 1 calc R . . C3 C 1.1238(3) 0.7163(3) 0.7895(4) 0.0302(15) Uani 1 1 d . . . H3 H 1.1555 0.7456 0.8072 0.036 Uiso 1 1 calc R . . C4 C 1.0708(3) 0.6811(4) 0.8608(4) 0.0340(15) Uani 1 1 d . . . C5 C 1.1677(3) 0.6476(4) 0.7097(4) 0.0355(15) Uani 1 1 d . . . H5A H 1.1993 0.6739 0.7325 0.043 Uiso 1 1 calc R . . H5B H 1.1651 0.6471 0.6596 0.043 Uiso 1 1 calc R . . C6 C 1.1573(3) 0.6267(4) 0.8847(3) 0.0341(15) Uani 1 1 d . . . H6A H 1.1488 0.6169 0.9290 0.041 Uiso 1 1 calc R . . H6B H 1.1892 0.6554 0.8949 0.041 Uiso 1 1 calc R . . C7 C 1.1604(3) 0.5179(4) 0.6909(4) 0.0398(17) Uani 1 1 d . . . C8 C 1.1999(3) 0.5571(4) 0.8038(3) 0.0303(14) Uani 1 1 d . . . H8 H 1.2332 0.5834 0.8198 0.036 Uiso 1 1 calc R . . C9 C 1.2085(3) 0.4758(4) 0.8006(3) 0.0311(14) Uani 1 1 d . . . H9 H 1.2459 0.4639 0.8078 0.037 Uiso 1 1 calc R . . C10 C 1.1641(3) 0.4971(4) 0.8853(4) 0.0349(15) Uani 1 1 d . . . C11 C 1.1841(3) 0.3927(4) 0.6964(4) 0.0372(16) Uani 1 1 d . . . H11A H 1.2214 0.3817 0.7057 0.045 Uiso 1 1 calc R . . H11B H 1.1706 0.3981 0.6460 0.045 Uiso 1 1 calc R . . C12 C 1.2014(3) 0.3778(4) 0.8844(4) 0.0353(15) Uani 1 1 d . . . H12A H 1.1962 0.3769 0.9315 0.042 Uiso 1 1 calc R . . H12B H 1.2386 0.3696 0.8883 0.042 Uiso 1 1 calc R . . C13 C 1.1184(3) 0.2983(4) 0.6752(4) 0.0331(15) Uani 1 1 d . . . C14 C 1.1819(3) 0.2934(3) 0.7808(4) 0.0284(14) Uani 1 1 d . . . H14 H 1.2197 0.2866 0.7858 0.034 Uiso 1 1 calc R . . C15 C 1.1523(2) 0.2233(4) 0.7704(3) 0.0280(14) Uani 1 1 d . . . H15 H 1.1754 0.1831 0.7664 0.034 Uiso 1 1 calc R . . C16 C 1.1442(2) 0.2750(4) 0.8729(4) 0.0282(14) Uani 1 1 d . . . C17 C 1.0786(3) 0.1803(4) 0.6682(4) 0.0347(15) Uani 1 1 d . . . H17A H 1.0987 0.1362 0.6715 0.042 Uiso 1 1 calc R . . H17B H 1.0678 0.1939 0.6190 0.042 Uiso 1 1 calc R . . C18 C 1.1079(2) 0.1548(4) 0.8502(3) 0.0318(14) Uani 1 1 d . . . H18A H 1.1248 0.1129 0.8365 0.038 Uiso 1 1 calc R . . H18B H 1.1138 0.1536 0.9010 0.038 Uiso 1 1 calc R . . C19 C 0.9833(3) 0.1820(4) 0.6522(4) 0.0320(14) Uani 1 1 d . . . C20 C 1.0293(3) 0.1221(4) 0.7501(4) 0.0343(15) Uani 1 1 d . . . H20 H 1.0420 0.0738 0.7445 0.041 Uiso 1 1 calc R . . C21 C 1.0014(3) 0.7706(4) 0.8369(4) 0.0320(15) Uani 1 1 d . . . H21A H 1.0043 0.7665 0.8870 0.038 Uiso 1 1 calc R . . H21B H 1.0038 0.8211 0.8264 0.038 Uiso 1 1 calc R . . N1 N 1.0488(2) 0.7453(3) 0.7000(3) 0.0304(12) Uani 1 1 d . . . N2 N 1.1230(2) 0.6838(3) 0.7216(3) 0.0298(12) Uani 1 1 d . . . N3 N 1.0448(2) 0.7341(3) 0.8213(3) 0.0312(12) Uani 1 1 d . . . N4 N 1.1158(2) 0.6672(3) 0.8418(3) 0.0342(13) Uani 1 1 d . . . N5 N 1.1724(2) 0.5758(3) 0.7352(3) 0.0358(13) Uani 1 1 d . . . N6 N 1.1781(2) 0.4586(3) 0.7292(3) 0.0351(13) Uani 1 1 d . . . N7 N 1.1677(2) 0.5605(3) 0.8546(3) 0.0330(12) Uani 1 1 d . . . N8 N 1.1872(2) 0.4465(3) 0.8544(3) 0.0323(12) Uani 1 1 d . . . N9 N 1.1578(2) 0.3338(3) 0.7192(3) 0.0327(12) Uani 1 1 d . . . N10 N 1.1117(2) 0.2343(3) 0.7060(3) 0.0326(12) Uani 1 1 d . . . N11 N 1.1714(2) 0.3214(3) 0.8439(3) 0.0295(12) Uani 1 1 d . . . N12 N 1.1324(2) 0.2171(3) 0.8315(3) 0.0319(13) Uani 1 1 d . . . N13 N 1.0318(2) 0.1670(3) 0.6929(3) 0.0303(12) Uani 1 1 d . . . N14 N 1.0530(2) 0.1507(3) 0.8191(3) 0.0299(12) Uani 1 1 d . . . O1 O 1.07086(19) 0.6850(3) 0.6103(2) 0.0373(11) Uani 1 1 d . . . O2 O 1.1381(3) 0.5191(3) 0.6309(3) 0.0559(15) Uani 1 1 d . . . O3 O 1.0934(2) 0.3190(3) 0.6186(3) 0.0465(13) Uani 1 1 d . . . O4 O 0.9734(2) 0.2163(3) 0.5981(2) 0.0359(12) Uani 1 1 d . . . O5 O 1.0562(2) 0.6499(3) 0.9068(3) 0.0423(12) Uani 1 1 d . . . O6 O 1.1450(2) 0.4874(3) 0.9347(3) 0.0505(14) Uani 1 1 d . . . O7 O 1.1322(2) 0.2829(3) 0.9288(3) 0.0391(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl5 0.126(4) 0.134(4) 0.157(5) -0.002(3) 0.054(3) 0.047(3) Cl1 0.0677(13) 0.0449(12) 0.0805(17) 0.0134(11) 0.0283(12) 0.0072(10) Cl2 0.111(2) 0.0574(18) 0.204(4) 0.050(2) 0.092(3) 0.0136(16) Cl3 0.186(11) 0.173(10) 0.192(9) -0.113(8) 0.036(8) -0.006(9) Cl4 0.095(3) 0.079(3) 0.409(19) 0.109(6) 0.120(6) 0.009(2) Zn1 0.0795(11) 0.0527(10) 0.353(4) 0.0239(15) 0.0244(16) -0.0007(8) O1W 0.079(4) 0.047(3) 0.022(2) 0.007(2) 0.016(2) 0.019(3) O2W 0.048(3) 0.084(5) 0.038(3) -0.017(3) 0.009(3) -0.017(3) O3W 0.075(4) 0.041(3) 0.037(3) -0.006(2) 0.001(3) -0.007(3) O4W 0.037(3) 0.079(4) 0.034(3) 0.002(3) 0.006(2) -0.015(3) O5W 0.070(4) 0.046(3) 0.046(3) -0.007(3) 0.010(3) 0.004(3) Yb1 0.0377(2) 0.0325(2) 0.0213(2) -0.00043(11) 0.00868(13) -0.00307(11) C1 0.041(4) 0.025(3) 0.024(4) 0.000(3) 0.015(3) -0.002(3) C2 0.035(3) 0.029(3) 0.030(4) -0.005(3) 0.010(3) -0.001(3) C3 0.033(3) 0.032(4) 0.026(4) 0.001(3) 0.009(3) 0.002(3) C4 0.045(4) 0.034(4) 0.026(4) -0.006(3) 0.014(3) 0.004(3) C5 0.046(4) 0.033(4) 0.032(4) 0.007(3) 0.017(3) 0.008(3) C6 0.050(4) 0.033(4) 0.017(3) 0.007(3) 0.005(3) 0.009(3) C7 0.049(4) 0.035(4) 0.035(4) 0.004(3) 0.010(3) 0.005(3) C8 0.037(3) 0.026(3) 0.027(3) 0.002(3) 0.005(3) 0.001(3) C9 0.033(3) 0.033(4) 0.028(3) 0.003(3) 0.009(3) 0.003(3) C10 0.047(4) 0.028(4) 0.029(4) 0.003(3) 0.008(3) 0.000(3) C11 0.052(4) 0.033(4) 0.029(4) -0.002(3) 0.015(3) 0.005(3) C12 0.045(4) 0.030(4) 0.028(4) 0.004(3) 0.005(3) -0.001(3) C13 0.035(3) 0.042(4) 0.023(4) -0.001(3) 0.008(3) 0.005(3) C14 0.029(3) 0.031(4) 0.024(3) 0.004(3) 0.004(3) 0.005(3) C15 0.025(3) 0.035(4) 0.025(3) -0.004(3) 0.010(3) 0.004(3) C16 0.025(3) 0.033(4) 0.026(4) -0.001(3) 0.005(3) 0.000(3) C17 0.035(3) 0.044(4) 0.027(3) -0.005(3) 0.011(3) -0.003(3) C18 0.033(3) 0.035(4) 0.029(3) 0.004(3) 0.010(3) 0.008(3) C19 0.044(4) 0.024(3) 0.030(4) -0.009(3) 0.014(3) -0.003(3) C20 0.042(4) 0.029(4) 0.032(4) -0.003(3) 0.011(3) 0.003(3) C21 0.038(4) 0.035(4) 0.023(4) -0.006(3) 0.007(3) -0.006(3) N1 0.034(3) 0.035(3) 0.024(3) 0.004(2) 0.009(2) 0.001(2) N2 0.035(3) 0.031(3) 0.025(3) -0.004(2) 0.011(2) -0.003(2) N3 0.036(3) 0.038(3) 0.020(3) 0.001(2) 0.006(2) 0.006(3) N4 0.041(3) 0.033(3) 0.032(3) 0.006(2) 0.015(2) 0.008(3) N5 0.048(3) 0.032(3) 0.032(3) 0.004(3) 0.018(3) 0.005(3) N6 0.051(3) 0.027(3) 0.026(3) -0.001(2) 0.007(3) -0.001(3) N7 0.048(3) 0.029(3) 0.025(3) 0.004(2) 0.016(2) 0.005(3) N8 0.050(3) 0.028(3) 0.020(3) 0.004(2) 0.012(2) 0.001(2) N9 0.040(3) 0.028(3) 0.029(3) 0.003(2) 0.006(2) -0.001(2) N10 0.036(3) 0.033(3) 0.027(3) 0.003(2) 0.005(2) 0.001(2) N11 0.035(3) 0.032(3) 0.020(3) 0.001(2) 0.006(2) 0.000(2) N12 0.043(3) 0.027(3) 0.028(3) 0.003(2) 0.013(3) -0.003(2) N13 0.034(3) 0.031(3) 0.029(3) 0.003(2) 0.012(2) 0.001(2) N14 0.036(3) 0.033(3) 0.022(3) 0.000(2) 0.010(2) 0.000(2) O1 0.044(3) 0.042(3) 0.027(3) 0.003(2) 0.009(2) 0.000(2) O2 0.085(4) 0.045(3) 0.029(3) 0.007(2) -0.003(3) 0.003(3) O3 0.054(3) 0.048(3) 0.033(3) 0.011(3) 0.003(2) -0.001(3) O4 0.041(3) 0.046(3) 0.019(2) 0.010(2) 0.005(2) 0.004(2) O5 0.059(3) 0.043(3) 0.033(3) 0.011(2) 0.027(2) 0.010(2) O6 0.072(4) 0.045(3) 0.044(3) 0.009(3) 0.033(3) 0.002(3) O7 0.044(3) 0.045(3) 0.032(3) -0.003(2) 0.016(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 Zn1 2.216(3) . ? Cl2 Zn1 2.216(4) . ? Cl3 Zn1 2.441(12) . ? Cl4 Zn1 2.124(5) . ? O1W Yb1 2.283(5) . ? O2W Yb1 2.334(5) . ? O3W Yb1 2.351(5) . ? O4W Yb1 2.274(5) . ? O5W Yb1 2.350(6) . ? Yb1 O7 2.296(5) 6_565 ? Yb1 O4 2.335(5) 5_766 ? Yb1 O1 2.374(5) . ? C1 O1 1.225(8) . ? C1 N2 1.355(9) . ? C1 N1 1.374(8) . ? C2 N1 1.461(9) . ? C2 N3 1.461(9) . ? C2 C3 1.558(9) . ? C2 H2 0.9900 . ? C3 N4 1.448(8) . ? C3 N2 1.476(8) . ? C3 H3 0.9900 . ? C4 O5 1.228(8) . ? C4 N3 1.349(9) . ? C4 N4 1.361(8) . ? C5 N2 1.436(8) . ? C5 N5 1.441(9) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.430(8) . ? C6 N7 1.442(9) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.187(9) . ? C7 N6 1.367(9) . ? C7 N5 1.389(10) . ? C8 N5 1.417(9) . ? C8 N7 1.480(8) . ? C8 C9 1.555(9) . ? C8 H8 0.9900 . ? C9 N8 1.440(8) . ? C9 N6 1.477(9) . ? C9 H9 0.9900 . ? C10 O6 1.228(8) . ? C10 N7 1.357(9) . ? C10 N8 1.362(9) . ? C11 N6 1.433(9) . ? C11 N9 1.444(9) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.436(9) . ? C12 N11 1.445(9) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.215(9) . ? C13 N9 1.356(9) . ? C13 N10 1.386(9) . ? C14 N9 1.444(9) . ? C14 N11 1.452(8) . ? C14 C15 1.525(9) . ? C14 H14 0.9900 . ? C15 N12 1.445(8) . ? C15 N10 1.461(9) . ? C15 H15 0.9900 . ? C16 O7 1.239(9) . ? C16 N11 1.353(9) . ? C16 N12 1.356(9) . ? C17 N10 1.427(9) . ? C17 N13 1.466(8) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N14 1.429(8) . ? C18 N12 1.438(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.223(8) . ? C19 N13 1.361(9) . ? C19 N14 1.372(8) 2_756 ? C20 N13 1.433(9) . ? C20 N14 1.457(9) . ? C20 C20 1.549(13) 2_756 ? C20 H20 0.9900 . ? C21 N1 1.426(9) 2_756 ? C21 N3 1.441(9) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? N1 C21 1.426(9) 2_756 ? N14 C19 1.372(8) 2_756 ? O4 Yb1 2.335(5) 5_766 ? O7 Yb1 2.296(5) 6_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl4 Zn1 Cl1 113.62(17) . . ? Cl4 Zn1 Cl2 116.9(2) . . ? Cl1 Zn1 Cl2 113.26(15) . . ? Cl4 Zn1 Cl3 105.2(5) . . ? Cl1 Zn1 Cl3 97.5(3) . . ? Cl2 Zn1 Cl3 107.8(4) . . ? O4W Yb1 O1W 107.0(2) . . ? O4W Yb1 O7 146.4(2) . 6_565 ? O1W Yb1 O7 78.37(18) . 6_565 ? O4W Yb1 O2W 141.5(2) . . ? O1W Yb1 O2W 83.2(2) . . ? O7 Yb1 O2W 71.3(2) 6_565 . ? O4W Yb1 O4 76.41(19) . 5_766 ? O1W Yb1 O4 143.17(17) . 5_766 ? O7 Yb1 O4 80.33(18) 6_565 5_766 ? O2W Yb1 O4 117.5(2) . 5_766 ? O4W Yb1 O5W 80.9(2) . . ? O1W Yb1 O5W 145.64(19) . . ? O7 Yb1 O5W 113.8(2) 6_565 . ? O2W Yb1 O5W 71.9(2) . . ? O4 Yb1 O5W 70.95(19) 5_766 . ? O4W Yb1 O3W 74.7(2) . . ? O1W Yb1 O3W 71.4(2) . . ? O7 Yb1 O3W 76.0(2) 6_565 . ? O2W Yb1 O3W 141.9(2) . . ? O4 Yb1 O3W 74.5(2) 5_766 . ? O5W Yb1 O3W 141.4(2) . . ? O4W Yb1 O1 72.80(18) . . ? O1W Yb1 O1 72.35(17) . . ? O7 Yb1 O1 137.76(18) 6_565 . ? O2W Yb1 O1 75.56(19) . . ? O4 Yb1 O1 139.48(17) 5_766 . ? O5W Yb1 O1 78.65(19) . . ? O3W Yb1 O1 120.44(19) . . ? O1 C1 N2 125.0(6) . . ? O1 C1 N1 125.5(7) . . ? N2 C1 N1 109.5(6) . . ? N1 C2 N3 113.6(5) . . ? N1 C2 C3 103.3(5) . . ? N3 C2 C3 102.7(5) . . ? N1 C2 H2 112.2 . . ? N3 C2 H2 112.2 . . ? C3 C2 H2 112.2 . . ? N4 C3 N2 114.8(5) . . ? N4 C3 C2 103.3(5) . . ? N2 C3 C2 103.0(5) . . ? N4 C3 H3 111.7 . . ? N2 C3 H3 111.7 . . ? C2 C3 H3 111.7 . . ? O5 C4 N3 125.2(6) . . ? O5 C4 N4 125.2(7) . . ? N3 C4 N4 109.5(6) . . ? N2 C5 N5 113.0(5) . . ? N2 C5 H5A 109.0 . . ? N5 C5 H5A 109.0 . . ? N2 C5 H5B 109.0 . . ? N5 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N4 C6 N7 114.5(6) . . ? N4 C6 H6A 108.6 . . ? N7 C6 H6A 108.6 . . ? N4 C6 H6B 108.6 . . ? N7 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? O2 C7 N6 125.9(7) . . ? O2 C7 N5 126.6(7) . . ? N6 C7 N5 107.5(6) . . ? N5 C8 N7 113.6(5) . . ? N5 C8 C9 104.6(5) . . ? N7 C8 C9 100.7(5) . . ? N5 C8 H8 112.4 . . ? N7 C8 H8 112.4 . . ? C9 C8 H8 112.4 . . ? N8 C9 N6 114.1(6) . . ? N8 C9 C8 105.1(5) . . ? N6 C9 C8 101.9(5) . . ? N8 C9 H9 111.7 . . ? N6 C9 H9 111.7 . . ? C8 C9 H9 111.7 . . ? O6 C10 N7 125.5(7) . . ? O6 C10 N8 125.4(6) . . ? N7 C10 N8 109.0(6) . . ? N6 C11 N9 114.1(6) . . ? N6 C11 H11A 108.7 . . ? N9 C11 H11A 108.7 . . ? N6 C11 H11B 108.7 . . ? N9 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? N8 C12 N11 112.7(6) . . ? N8 C12 H12A 109.0 . . ? N11 C12 H12A 109.0 . . ? N8 C12 H12B 109.0 . . ? N11 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? O3 C13 N9 125.9(7) . . ? O3 C13 N10 126.1(7) . . ? N9 C13 N10 108.1(6) . . ? N9 C14 N11 113.5(5) . . ? N9 C14 C15 104.1(5) . . ? N11 C14 C15 103.2(5) . . ? N9 C14 H14 111.8 . . ? N11 C14 H14 111.8 . . ? C15 C14 H14 111.8 . . ? N12 C15 N10 113.7(5) . . ? N12 C15 C14 104.0(5) . . ? N10 C15 C14 103.4(5) . . ? N12 C15 H15 111.7 . . ? N10 C15 H15 111.7 . . ? C14 C15 H15 111.7 . . ? O7 C16 N11 126.0(6) . . ? O7 C16 N12 124.8(6) . . ? N11 C16 N12 109.2(6) . . ? N10 C17 N13 113.9(5) . . ? N10 C17 H17A 108.8 . . ? N13 C17 H17A 108.8 . . ? N10 C17 H17B 108.8 . . ? N13 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? N14 C18 N12 114.1(6) . . ? N14 C18 H18A 108.7 . . ? N12 C18 H18A 108.7 . . ? N14 C18 H18B 108.7 . . ? N12 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? O4 C19 N13 126.3(6) . . ? O4 C19 N14 125.2(7) . 2_756 ? N13 C19 N14 108.5(6) . 2_756 ? N13 C20 N14 115.5(6) . . ? N13 C20 C20 104.2(6) . 2_756 ? N14 C20 C20 101.3(6) . 2_756 ? N13 C20 H20 111.7 . . ? N14 C20 H20 111.7 . . ? C20 C20 H20 111.7 2_756 . ? N1 C21 N3 114.6(6) 2_756 . ? N1 C21 H21A 108.6 2_756 . ? N3 C21 H21A 108.6 . . ? N1 C21 H21B 108.6 2_756 . ? N3 C21 H21B 108.6 . . ? H21A C21 H21B 107.6 . . ? C1 N1 C21 124.2(6) . 2_756 ? C1 N1 C2 111.9(5) . . ? C21 N1 C2 123.9(5) 2_756 . ? C1 N2 C5 125.2(6) . . ? C1 N2 C3 112.0(5) . . ? C5 N2 C3 121.8(6) . . ? C4 N3 C21 123.2(6) . . ? C4 N3 C2 112.2(5) . . ? C21 N3 C2 122.8(6) . . ? C4 N4 C6 122.1(6) . . ? C4 N4 C3 112.1(6) . . ? C6 N4 C3 122.5(6) . . ? C7 N5 C8 113.1(6) . . ? C7 N5 C5 122.2(6) . . ? C8 N5 C5 123.4(6) . . ? C7 N6 C11 121.3(6) . . ? C7 N6 C9 112.3(6) . . ? C11 N6 C9 122.0(6) . . ? C10 N7 C6 122.4(5) . . ? C10 N7 C8 112.8(5) . . ? C6 N7 C8 121.6(5) . . ? C10 N8 C12 123.2(6) . . ? C10 N8 C9 111.7(5) . . ? C12 N8 C9 123.0(6) . . ? C13 N9 C11 122.1(6) . . ? C13 N9 C14 112.7(6) . . ? C11 N9 C14 121.9(6) . . ? C13 N10 C17 121.4(6) . . ? C13 N10 C15 111.3(6) . . ? C17 N10 C15 125.1(6) . . ? C16 N11 C12 121.2(6) . . ? C16 N11 C14 111.8(5) . . ? C12 N11 C14 123.4(5) . . ? C16 N12 C18 123.5(6) . . ? C16 N12 C15 111.6(5) . . ? C18 N12 C15 124.7(6) . . ? C19 N13 C20 111.6(5) . . ? C19 N13 C17 120.9(6) . . ? C20 N13 C17 125.5(6) . . ? C19 N14 C18 122.7(6) 2_756 . ? C19 N14 C20 111.7(5) 2_756 . ? C18 N14 C20 125.1(5) . . ? C1 O1 Yb1 148.4(5) . . ? C19 O4 Yb1 160.5(5) . 5_766 ? C16 O7 Yb1 152.1(5) . 6_566 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.889 _refine_diff_density_min -3.611 _refine_diff_density_rms 0.168 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.003 -0.009 0.000 1209 338 ' ' 2 0.001 -0.019 0.500 1209 338 ' ' 3 0.500 0.000 0.257 469 139 ' ' 4 0.000 0.500 0.762 469 139 ' ' _platon_squeeze_details ; ; data_p _database_code_depnum_ccdc_archive 'CCDC 905584' #TrackingRef '11 (905584).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H60 Cl5 Lu N14 O26.50 Zn' _chemical_formula_weight 1350.42 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.2356(12) _cell_length_b 18.6413(9) _cell_length_c 19.8143(9) _cell_angle_alpha 90.00 _cell_angle_beta 105.573(2) _cell_angle_gamma 90.00 _cell_volume 9334.7(8) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.922 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5456 _exptl_absorpt_coefficient_mu 3.005 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5449 _exptl_absorpt_correction_T_max 0.6291 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43671 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9089 _reflns_number_gt 7279 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0927P)^2^+23.4906P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9089 _refine_ls_number_parameters 497 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1490 _refine_ls_wR_factor_gt 0.1403 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl5 Cl 0.22478(12) 0.23205(18) 0.13546(18) 0.0971(9) Uani 1 1 d . . . Cl1 Cl 0.31069(11) 0.53682(12) 0.24239(18) 0.0921(9) Uani 1 1 d . . . Cl2 Cl 0.32576(7) 0.34889(9) 0.29743(11) 0.0512(4) Uani 1 1 d . . . Cl3 Cl 0.44551(13) 0.45981(19) 0.3357(3) 0.157(2) Uani 1 1 d . . . Cl4 Cl 0.3440(3) 0.4903(5) 0.4299(3) 0.219(3) Uani 1 1 d U . . Zn1 Zn 0.36038(6) 0.45858(8) 0.32387(12) 0.0643(7) Uani 0.672(4) 1 d P A 1 Zn1' Zn 0.36421(13) 0.45351(15) 0.2676(2) 0.0632(14) Uani 0.328(4) 1 d P A 2 O1W O 0.11039(18) 0.3918(2) 0.5225(2) 0.0377(10) Uani 1 1 d . . . O2W O -0.01313(17) 0.2950(3) 0.4955(2) 0.0403(11) Uani 1 1 d . . . O3W O 0.03686(19) 0.3623(2) 0.4037(2) 0.0419(11) Uani 1 1 d . . . O4W O 0.15357(19) 0.2416(3) 0.5633(2) 0.0498(13) Uani 1 1 d . . . O5W O 0.0592(2) 0.1672(2) 0.5377(2) 0.0488(12) Uani 1 1 d . . . Lu1 Lu 0.072592(9) 0.281869(12) 0.495531(11) 0.02560(11) Uani 1 1 d . . . O7 O 0.07160(16) 0.6914(2) 0.1112(2) 0.0300(9) Uani 1 1 d . . . O4 O 0.05517(18) 0.6540(2) 0.4064(2) 0.0358(10) Uani 1 1 d . . . C19 C 0.0742(2) 0.7693(3) 0.2747(3) 0.0236(11) Uani 1 1 d . . . H19 H 0.0822 0.8211 0.2819 0.028 Uiso 1 1 calc R . . C20 C 0.0809(2) 0.7104(3) 0.1729(3) 0.0217(11) Uani 1 1 d . . . C21 C 0.0010(2) 0.7803(3) 0.3372(3) 0.0278(13) Uani 1 1 d . . . H21A H 0.0038 0.7765 0.3874 0.033 Uiso 1 1 calc R . . H21B H 0.0031 0.8312 0.3261 0.033 Uiso 1 1 calc R . . N13 N 0.04542(19) 0.7426(3) 0.3224(2) 0.0260(10) Uani 1 1 d . . . N14 N 0.04980(18) 0.7528(3) 0.2016(2) 0.0247(10) Uani 1 1 d . . . C1 C 0.0165(2) 0.1773(3) 0.3479(3) 0.0232(11) Uani 1 1 d . . . C2 C 0.0300(2) 0.1156(3) 0.2524(3) 0.0266(12) Uani 1 1 d . . . H2 H 0.0432 0.0666 0.2477 0.032 Uiso 1 1 calc R . . C3 C 0.1092(2) 0.1506(3) 0.3519(3) 0.0260(12) Uani 1 1 d . . . H3A H 0.1268 0.1086 0.3386 0.031 Uiso 1 1 calc R . . H3B H 0.1154 0.1495 0.4030 0.031 Uiso 1 1 calc R . . C4 C 0.0798(2) 0.1741(3) 0.1704(3) 0.0255(12) Uani 1 1 d . . . H4A H 0.1010 0.1301 0.1770 0.031 Uiso 1 1 calc R . . H4B H 0.0693 0.1851 0.1202 0.031 Uiso 1 1 calc R . . C5 C 0.1440(2) 0.2730(3) 0.3748(3) 0.0243(12) Uani 1 1 d . . . C6 C 0.1533(2) 0.2203(3) 0.2723(3) 0.0238(12) Uani 1 1 d . . . H6 H 0.1771 0.1801 0.2688 0.029 Uiso 1 1 calc R . . C7 C 0.1827(2) 0.2935(3) 0.2836(3) 0.0243(12) Uani 1 1 d . . . H7 H 0.2211 0.2878 0.2894 0.029 Uiso 1 1 calc R . . C8 C 0.1175(2) 0.2959(3) 0.1769(3) 0.0279(12) Uani 1 1 d . . . C9 C 0.2013(2) 0.3785(3) 0.3883(3) 0.0290(12) Uani 1 1 d . . . H9A H 0.1960 0.3773 0.4354 0.035 Uiso 1 1 calc R . . H9B H 0.2389 0.3703 0.3930 0.035 Uiso 1 1 calc R . . C10 C 0.1825(2) 0.3934(3) 0.1989(3) 0.0295(12) Uani 1 1 d . . . H10A H 0.1676 0.3990 0.1482 0.035 Uiso 1 1 calc R . . H10B H 0.2203 0.3832 0.2074 0.035 Uiso 1 1 calc R . . C11 C 0.1644(2) 0.5008(3) 0.3905(3) 0.0290(12) Uani 1 1 d . . . C12 C 0.2083(2) 0.4774(3) 0.3043(3) 0.0236(11) Uani 1 1 d . . . H12 H 0.2459 0.4643 0.3111 0.028 Uiso 1 1 calc R . . C13 C 0.2010(2) 0.5587(3) 0.3104(3) 0.0255(12) Uani 1 1 d . . . H13 H 0.2352 0.5840 0.3278 0.031 Uiso 1 1 calc R . . C14 C 0.1595(2) 0.5217(3) 0.1960(3) 0.0312(13) Uani 1 1 d . . . C15 C 0.1591(2) 0.6314(3) 0.3895(3) 0.0287(12) Uani 1 1 d . . . H15A H 0.1919 0.6594 0.4001 0.034 Uiso 1 1 calc R . . H15B H 0.1504 0.6223 0.4339 0.034 Uiso 1 1 calc R . . C16 C 0.1694(2) 0.6525(3) 0.2141(3) 0.0268(12) Uani 1 1 d . . . H16A H 0.1676 0.6525 0.1641 0.032 Uiso 1 1 calc R . . H16B H 0.2015 0.6784 0.2387 0.032 Uiso 1 1 calc R . . C17 C 0.0710(2) 0.6875(3) 0.3619(3) 0.0265(12) Uani 1 1 d . . . C18 C 0.1255(2) 0.7230(3) 0.2919(3) 0.0242(12) Uani 1 1 d . . . H18 H 0.1577 0.7524 0.3100 0.029 Uiso 1 1 calc R . . N1 N 0.05353(18) 0.1448(2) 0.3201(2) 0.0261(10) Uani 1 1 d . . . N2 N 0.13320(19) 0.2144(2) 0.3333(2) 0.0254(10) Uani 1 1 d . . . N3 N 0.03241(18) 0.1612(2) 0.1934(2) 0.0259(10) Uani 1 1 d . . . N4 N 0.11245(19) 0.2321(3) 0.2071(2) 0.0276(10) Uani 1 1 d . . . N5 N 0.17141(18) 0.3209(2) 0.3477(2) 0.0246(10) Uani 1 1 d . . . N6 N 0.18724(19) 0.4485(2) 0.3588(2) 0.0275(10) Uani 1 1 d . . . N7 N 0.15781(18) 0.3343(2) 0.2220(2) 0.0264(10) Uani 1 1 d . . . N8 N 0.1761(2) 0.4608(2) 0.2336(2) 0.0281(10) Uani 1 1 d . . . N9 N 0.16804(19) 0.5639(3) 0.3595(2) 0.0287(10) Uani 1 1 d . . . N10 N 0.11693(19) 0.6734(2) 0.3443(2) 0.0270(10) Uani 1 1 d . . . N11 N 0.17350(19) 0.5795(3) 0.2387(2) 0.0283(10) Uani 1 1 d . . . N12 N 0.12358(18) 0.6909(3) 0.2242(2) 0.0258(10) Uani 1 1 d . . . O1 O 0.02658(16) 0.2119(2) 0.4030(2) 0.0284(9) Uani 1 1 d . . . O2 O 0.13137(18) 0.2806(2) 0.4306(2) 0.0331(10) Uani 1 1 d . . . O3 O 0.14468(19) 0.4908(2) 0.4388(2) 0.0430(11) Uani 1 1 d . . . O5 O 0.09198(17) 0.3168(2) 0.1194(2) 0.0379(10) Uani 1 1 d . . . O6 O 0.1359(2) 0.5237(2) 0.1328(2) 0.0523(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl5 0.0762(18) 0.120(2) 0.096(2) -0.0084(17) 0.0253(16) 0.0389(16) Cl1 0.0893(18) 0.0521(13) 0.152(3) 0.0417(15) 0.0619(18) 0.0050(12) Cl2 0.0523(10) 0.0355(9) 0.0704(12) 0.0096(8) 0.0242(9) 0.0081(8) Cl3 0.0718(19) 0.101(2) 0.280(6) 0.098(3) 0.015(3) -0.0038(17) Cl4 0.243(7) 0.253(7) 0.147(5) -0.045(5) 0.037(5) -0.086(6) Zn1 0.0548(9) 0.0475(8) 0.0869(17) 0.0162(8) 0.0127(8) -0.0047(6) Zn1' 0.069(2) 0.0405(16) 0.087(3) 0.0170(15) 0.0336(18) 0.0043(13) O1W 0.057(3) 0.041(2) 0.017(2) -0.0023(17) 0.0130(19) -0.007(2) O2W 0.031(2) 0.068(3) 0.022(2) -0.001(2) 0.0072(19) 0.009(2) O3W 0.061(3) 0.037(2) 0.022(2) 0.0052(18) 0.002(2) 0.011(2) O4W 0.045(3) 0.077(3) 0.029(3) 0.016(2) 0.012(2) 0.026(3) O5W 0.076(4) 0.039(3) 0.029(2) 0.007(2) 0.011(2) 0.000(2) Lu1 0.02953(17) 0.03178(16) 0.01631(16) 0.00044(9) 0.00758(11) 0.00354(10) O7 0.035(2) 0.038(2) 0.019(2) -0.0003(17) 0.0102(17) -0.0018(18) O4 0.050(3) 0.040(2) 0.026(2) 0.0033(18) 0.024(2) 0.006(2) C19 0.028(3) 0.023(3) 0.019(3) -0.002(2) 0.004(2) -0.002(2) C20 0.027(3) 0.023(3) 0.017(3) 0.001(2) 0.008(2) 0.000(2) C21 0.027(3) 0.035(3) 0.024(3) -0.005(2) 0.010(3) 0.006(2) N13 0.027(3) 0.030(2) 0.021(2) -0.001(2) 0.007(2) 0.004(2) N14 0.025(2) 0.031(2) 0.016(2) 0.0015(19) 0.0023(19) 0.003(2) C1 0.029(3) 0.023(3) 0.021(3) -0.001(2) 0.011(2) -0.003(2) C2 0.029(3) 0.022(3) 0.030(3) 0.001(2) 0.010(2) 0.005(2) C3 0.028(3) 0.029(3) 0.021(3) 0.005(2) 0.008(2) 0.005(2) C4 0.025(3) 0.037(3) 0.016(3) -0.004(2) 0.007(2) 0.001(2) C5 0.025(3) 0.032(3) 0.018(3) 0.001(2) 0.007(2) 0.004(2) C6 0.024(3) 0.026(3) 0.024(3) 0.002(2) 0.011(2) 0.003(2) C7 0.021(3) 0.030(3) 0.021(3) -0.003(2) 0.004(2) 0.002(2) C8 0.025(3) 0.035(3) 0.024(3) -0.006(2) 0.008(2) 0.002(2) C9 0.035(3) 0.032(3) 0.019(3) 0.003(2) 0.003(2) 0.004(2) C10 0.034(3) 0.036(3) 0.021(3) -0.004(2) 0.009(2) 0.001(2) C11 0.029(3) 0.039(3) 0.019(3) 0.002(2) 0.005(2) 0.005(2) C12 0.023(3) 0.030(3) 0.017(3) 0.003(2) 0.006(2) 0.002(2) C13 0.031(3) 0.031(3) 0.015(3) -0.002(2) 0.006(2) 0.001(2) C14 0.033(3) 0.038(3) 0.024(3) 0.003(2) 0.011(3) 0.003(3) C15 0.037(3) 0.036(3) 0.013(3) -0.002(2) 0.007(2) 0.004(3) C16 0.033(3) 0.033(3) 0.021(3) 0.004(2) 0.019(2) 0.002(2) C17 0.034(3) 0.033(3) 0.016(3) -0.002(2) 0.013(2) 0.001(2) C18 0.025(3) 0.032(3) 0.015(3) 0.000(2) 0.005(2) 0.000(2) N1 0.024(2) 0.029(2) 0.028(3) -0.0009(19) 0.012(2) 0.0025(19) N2 0.027(3) 0.031(3) 0.019(2) -0.0002(18) 0.007(2) -0.0016(19) N3 0.024(2) 0.029(2) 0.025(2) -0.001(2) 0.008(2) 0.0004(19) N4 0.029(3) 0.034(3) 0.020(2) 0.0037(19) 0.007(2) 0.000(2) N5 0.030(3) 0.031(2) 0.013(2) -0.0006(18) 0.0062(19) -0.002(2) N6 0.034(3) 0.031(2) 0.020(2) 0.0005(19) 0.011(2) 0.000(2) N7 0.031(3) 0.031(2) 0.016(2) 0.0010(19) 0.0039(19) -0.004(2) N8 0.037(3) 0.029(2) 0.017(2) 0.0000(19) 0.005(2) 0.000(2) N9 0.032(3) 0.031(3) 0.026(2) -0.001(2) 0.013(2) 0.002(2) N10 0.030(3) 0.033(3) 0.020(2) 0.0021(19) 0.010(2) 0.005(2) N11 0.037(3) 0.030(3) 0.019(2) 0.0026(19) 0.008(2) 0.006(2) N12 0.025(2) 0.028(2) 0.023(2) -0.0002(19) 0.005(2) 0.003(2) O1 0.031(2) 0.035(2) 0.020(2) -0.0036(16) 0.0081(17) 0.0005(16) O2 0.038(2) 0.038(2) 0.028(2) -0.0051(17) 0.016(2) -0.0031(17) O3 0.065(3) 0.039(2) 0.034(2) 0.008(2) 0.029(2) 0.011(2) O5 0.036(2) 0.047(3) 0.026(2) 0.0092(19) 0.0001(19) -0.004(2) O6 0.087(4) 0.032(2) 0.027(3) 0.0013(19) -0.003(2) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 Zn1' 2.063(4) . ? Cl1 Zn1 2.303(3) . ? Cl2 Zn1 2.242(2) . ? Cl2 Zn1' 2.343(3) . ? Cl3 Zn1 2.182(4) . ? Cl3 Zn1' 2.200(5) . ? Cl4 Zn1 2.331(7) . ? O1W Lu1 2.277(4) . ? O2W Lu1 2.262(4) . ? O3W Lu1 2.350(4) . ? O4W Lu1 2.313(5) . ? O5W Lu1 2.355(4) . ? Lu1 O2 2.258(4) . ? Lu1 O1 2.310(4) . ? Lu1 O7 2.352(4) 6_566 ? O7 C20 1.233(7) . ? O7 Lu1 2.352(4) 6_565 ? O4 C17 1.238(7) . ? C19 N13 1.447(7) . ? C19 N14 1.449(7) . ? C19 C18 1.559(8) . ? C19 H19 0.9900 . ? C20 N12 1.345(7) . ? C20 N14 1.366(7) . ? C21 N14 1.441(7) 2 ? C21 N13 1.458(7) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? N13 C17 1.356(8) . ? N14 C21 1.441(7) 2 ? C1 O1 1.233(6) . ? C1 N3 1.358(7) 2 ? C1 N1 1.379(7) . ? C2 N1 1.425(7) . ? C2 N3 1.461(7) . ? C2 C2 1.552(11) 2 ? C2 H2 0.9900 . ? C3 N1 1.431(7) . ? C3 N2 1.439(7) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 N4 1.447(7) . ? C4 N3 1.455(7) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 O2 1.243(7) . ? C5 N5 1.346(7) . ? C5 N2 1.353(7) . ? C6 N2 1.446(7) . ? C6 N4 1.458(7) . ? C6 C7 1.553(7) . ? C6 H6 0.9900 . ? C7 N7 1.437(7) . ? C7 N5 1.470(7) . ? C7 H7 0.9900 . ? C8 O5 1.220(7) . ? C8 N4 1.353(8) . ? C8 N7 1.387(7) . ? C9 N6 1.436(7) . ? C9 N5 1.439(7) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 N7 1.414(7) . ? C10 N8 1.463(7) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 O3 1.219(7) . ? C11 N9 1.342(7) . ? C11 N6 1.381(7) . ? C12 N6 1.443(7) . ? C12 N8 1.462(7) . ? C12 C13 1.536(8) . ? C12 H12 0.9900 . ? C13 N11 1.461(7) . ? C13 N9 1.467(7) . ? C13 H13 0.9900 . ? C14 O6 1.240(7) . ? C14 N11 1.358(8) . ? C14 N8 1.362(7) . ? C15 N9 1.438(7) . ? C15 N10 1.453(7) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 N11 1.441(7) . ? C16 N12 1.457(7) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 N10 1.368(7) . ? C18 N10 1.451(7) . ? C18 N12 1.458(7) . ? C18 H18 0.9900 . ? N3 C1 1.358(7) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Zn1' Cl1 Zn1 29.91(12) . . ? Zn1 Cl2 Zn1' 28.95(10) . . ? Zn1 Cl3 Zn1' 30.43(11) . . ? Cl3 Zn1 Cl2 111.93(14) . . ? Cl3 Zn1 Cl1 116.04(13) . . ? Cl2 Zn1 Cl1 107.24(12) . . ? Cl3 Zn1 Cl4 109.4(3) . . ? Cl2 Zn1 Cl4 106.3(2) . . ? Cl1 Zn1 Cl4 105.3(3) . . ? Cl1 Zn1' Cl3 126.4(2) . . ? Cl1 Zn1' Cl2 112.12(16) . . ? Cl3 Zn1' Cl2 107.57(17) . . ? O2 Lu1 O2W 146.32(16) . . ? O2 Lu1 O1W 79.77(14) . . ? O2W Lu1 O1W 105.84(17) . . ? O2 Lu1 O1 80.37(15) . . ? O2W Lu1 O1 75.73(15) . . ? O1W Lu1 O1 142.83(14) . . ? O2 Lu1 O4W 70.50(16) . . ? O2W Lu1 O4W 142.48(16) . . ? O1W Lu1 O4W 83.19(19) . . ? O1 Lu1 O4W 118.72(17) . . ? O2 Lu1 O3W 75.94(16) . . ? O2W Lu1 O3W 75.00(17) . . ? O1W Lu1 O3W 70.47(15) . . ? O1 Lu1 O3W 74.39(15) . . ? O4W Lu1 O3W 140.36(18) . . ? O2 Lu1 O7 138.18(15) . 6_566 ? O2W Lu1 O7 72.90(15) . 6_566 ? O1W Lu1 O7 72.46(14) . 6_566 ? O1 Lu1 O7 138.86(14) . 6_566 ? O4W Lu1 O7 75.61(15) . 6_566 ? O3W Lu1 O7 120.86(15) . 6_566 ? O2 Lu1 O5W 112.47(16) . . ? O2W Lu1 O5W 81.67(18) . . ? O1W Lu1 O5W 146.15(15) . . ? O1 Lu1 O5W 70.91(15) . . ? O4W Lu1 O5W 72.59(19) . . ? O3W Lu1 O5W 141.92(17) . . ? O7 Lu1 O5W 78.74(15) 6_566 . ? C20 O7 Lu1 148.8(4) . 6_565 ? N13 C19 N14 114.3(5) . . ? N13 C19 C18 103.7(4) . . ? N14 C19 C18 103.0(4) . . ? N13 C19 H19 111.7 . . ? N14 C19 H19 111.7 . . ? C18 C19 H19 111.7 . . ? O7 C20 N12 125.1(5) . . ? O7 C20 N14 126.8(5) . . ? N12 C20 N14 108.1(4) . . ? N14 C21 N13 113.3(4) 2 . ? N14 C21 H21A 108.9 2 . ? N13 C21 H21A 108.9 . . ? N14 C21 H21B 108.9 2 . ? N13 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? C17 N13 C19 112.1(4) . . ? C17 N13 C21 123.1(5) . . ? C19 N13 C21 123.5(5) . . ? C20 N14 C21 123.5(5) . 2 ? C20 N14 C19 112.7(4) . . ? C21 N14 C19 123.7(5) 2 . ? O1 C1 N3 126.3(5) . 2 ? O1 C1 N1 125.2(5) . . ? N3 C1 N1 108.4(4) 2 . ? N1 C2 N3 115.5(4) . . ? N1 C2 C2 103.5(5) . 2 ? N3 C2 C2 102.2(5) . 2 ? N1 C2 H2 111.6 . . ? N3 C2 H2 111.6 . . ? C2 C2 H2 111.6 2 . ? N1 C3 N2 114.5(5) . . ? N1 C3 H3A 108.6 . . ? N2 C3 H3A 108.6 . . ? N1 C3 H3B 108.6 . . ? N2 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? N4 C4 N3 114.0(4) . . ? N4 C4 H4A 108.7 . . ? N3 C4 H4A 108.7 . . ? N4 C4 H4B 108.7 . . ? N3 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? O2 C5 N5 125.3(5) . . ? O2 C5 N2 124.8(5) . . ? N5 C5 N2 109.8(5) . . ? N2 C6 N4 113.9(5) . . ? N2 C6 C7 103.0(4) . . ? N4 C6 C7 102.3(4) . . ? N2 C6 H6 112.3 . . ? N4 C6 H6 112.3 . . ? C7 C6 H6 112.3 . . ? N7 C7 N5 113.5(4) . . ? N7 C7 C6 104.4(4) . . ? N5 C7 C6 102.9(4) . . ? N7 C7 H7 111.8 . . ? N5 C7 H7 111.8 . . ? C6 C7 H7 111.8 . . ? O5 C8 N4 126.8(6) . . ? O5 C8 N7 124.7(5) . . ? N4 C8 N7 108.5(5) . . ? N6 C9 N5 114.1(5) . . ? N6 C9 H9A 108.7 . . ? N5 C9 H9A 108.7 . . ? N6 C9 H9B 108.7 . . ? N5 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? N7 C10 N8 113.4(4) . . ? N7 C10 H10A 108.9 . . ? N8 C10 H10A 108.9 . . ? N7 C10 H10B 108.9 . . ? N8 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? O3 C11 N9 126.2(5) . . ? O3 C11 N6 125.2(5) . . ? N9 C11 N6 108.6(5) . . ? N6 C12 N8 113.6(5) . . ? N6 C12 C13 103.3(4) . . ? N8 C12 C13 103.4(4) . . ? N6 C12 H12 112.0 . . ? N8 C12 H12 112.0 . . ? C13 C12 H12 112.0 . . ? N11 C13 N9 113.7(5) . . ? N11 C13 C12 103.0(4) . . ? N9 C13 C12 103.0(4) . . ? N11 C13 H13 112.2 . . ? N9 C13 H13 112.2 . . ? C12 C13 H13 112.2 . . ? O6 C14 N11 125.7(6) . . ? O6 C14 N8 125.2(6) . . ? N11 C14 N8 109.1(5) . . ? N9 C15 N10 113.4(5) . . ? N9 C15 H15A 108.9 . . ? N10 C15 H15A 108.9 . . ? N9 C15 H15B 108.9 . . ? N10 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? N11 C16 N12 114.1(4) . . ? N11 C16 H16A 108.7 . . ? N12 C16 H16A 108.7 . . ? N11 C16 H16B 108.7 . . ? N12 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? O4 C17 N13 125.8(5) . . ? O4 C17 N10 124.9(5) . . ? N13 C17 N10 109.3(5) . . ? N10 C18 N12 115.0(4) . . ? N10 C18 C19 102.6(4) . . ? N12 C18 C19 102.1(4) . . ? N10 C18 H18 112.1 . . ? N12 C18 H18 112.1 . . ? C19 C18 H18 112.1 . . ? C1 N1 C2 111.8(4) . . ? C1 N1 C3 122.4(5) . . ? C2 N1 C3 125.2(4) . . ? C5 N2 C3 123.1(5) . . ? C5 N2 C6 112.5(4) . . ? C3 N2 C6 124.1(4) . . ? C1 N3 C4 121.6(4) 2 . ? C1 N3 C2 112.0(4) 2 . ? C4 N3 C2 124.8(4) . . ? C8 N4 C4 123.3(5) . . ? C8 N4 C6 112.9(5) . . ? C4 N4 C6 121.8(5) . . ? C5 N5 C9 122.7(4) . . ? C5 N5 C7 111.6(4) . . ? C9 N5 C7 122.4(4) . . ? C11 N6 C9 123.5(5) . . ? C11 N6 C12 112.1(4) . . ? C9 N6 C12 122.4(4) . . ? C8 N7 C10 122.0(5) . . ? C8 N7 C7 111.6(4) . . ? C10 N7 C7 123.0(5) . . ? C14 N8 C12 111.4(5) . . ? C14 N8 C10 121.3(5) . . ? C12 N8 C10 121.5(5) . . ? C11 N9 C15 122.5(5) . . ? C11 N9 C13 111.9(4) . . ? C15 N9 C13 121.5(5) . . ? C17 N10 C18 112.2(4) . . ? C17 N10 C15 121.5(4) . . ? C18 N10 C15 123.1(5) . . ? C14 N11 C16 123.8(5) . . ? C14 N11 C13 112.1(5) . . ? C16 N11 C13 123.5(5) . . ? C20 N12 C16 125.4(5) . . ? C20 N12 C18 113.7(4) . . ? C16 N12 C18 120.1(5) . . ? C1 O1 Lu1 160.1(4) . . ? C5 O2 Lu1 153.2(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.675 _refine_diff_density_min -1.280 _refine_diff_density_rms 0.154 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.003 -0.007 0.000 1048 434 ' ' 2 0.003 -0.005 0.500 1048 433 ' ' 3 0.500 0.000 0.274 457 139 ' ' 4 0.000 0.500 0.259 457 139 ' ' _platon_squeeze_details ; ; data_p4 _database_code_depnum_ccdc_archive 'CCDC 905585' #TrackingRef '2 (905585).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H66 N28 O26 Ce2, 2(Zn Cl4), 2Cl, 25(H2 O)' _chemical_formula_sum 'C42 H116 Ce2 Cl10 N28 O51 Zn2' _chemical_formula_weight 2595.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.9138(8) _cell_length_b 17.2483(8) _cell_length_c 20.4015(9) _cell_angle_alpha 98.006(2) _cell_angle_beta 112.6410(10) _cell_angle_gamma 109.750(2) _cell_volume 4915.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.753 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2636 _exptl_absorpt_coefficient_mu 1.768 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6101 _exptl_absorpt_correction_T_max 0.6865 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51861 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 25.10 _reflns_number_total 17254 _reflns_number_gt 14335 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1215P)^2^+3.9991P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17254 _refine_ls_number_parameters 1019 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1796 _refine_ls_wR_factor_gt 0.1719 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl9 Cl 0.0000 0.5000 0.5000 0.1158(18) Uani 1 2 d S . . Cl10 Cl 0.3192(3) -0.2004(3) 0.3896(2) 0.0759(12) Uani 0.50 1 d P . . Cl11 Cl 0.4908(5) 0.0426(5) -0.0180(4) 0.193(7) Uani 0.50 1 d P . . Cl12 Cl -0.0186(4) 0.1090(4) -0.0564(4) 0.1054(18) Uani 0.50 1 d P . . Zn2 Zn -0.26006(14) 0.38977(13) 0.07092(11) 0.0723(5) Uani 0.50 1 d PD . . Zn2' Zn -0.3239(2) 0.30749(18) 0.00948(14) 0.1154(9) Uani 0.50 1 d PD . . Cl5 Cl -0.2716(2) 0.2787(2) 0.12099(19) 0.1247(13) Uani 1 1 d D . . Cl6 Cl -0.4052(2) 0.3888(2) 0.0141(2) 0.1259(13) Uani 1 1 d D . . Cl7 Cl -0.2036(3) 0.3812(3) -0.0121(2) 0.220(3) Uani 1 1 d D . . Cl8 Cl -0.1387(4) 0.5215(3) 0.1478(4) 0.1332(18) Uani 0.50 1 d PD . . Cl8' Cl -0.4092(6) 0.1916(3) -0.0967(3) 0.1332(18) Uani 0.50 1 d PD . . O1W O -0.1463(3) 0.1309(3) 0.0188(2) 0.0455(10) Uani 1 1 d . . . O2W O -0.1098(3) -0.0856(3) 0.1292(2) 0.0437(10) Uani 1 1 d . . . O3W O 0.0320(3) 0.1156(3) 0.1652(3) 0.0562(13) Uani 1 1 d . . . O4W O -0.2700(3) -0.0623(3) 0.1339(2) 0.0470(11) Uani 1 1 d . . . O5W O -0.0827(3) -0.0048(4) 0.0213(3) 0.0606(14) Uani 1 1 d . . . O6W O -0.2809(3) 0.0845(3) 0.0866(3) 0.0642(15) Uani 1 1 d . . . O7W O 0.7604(3) 0.3212(2) 0.5227(2) 0.0386(9) Uani 1 1 d . . . O8W O 0.5994(3) 0.3250(3) 0.5411(2) 0.0420(10) Uani 1 1 d . . . O9W O 0.6563(3) 0.5031(2) 0.3943(2) 0.0443(10) Uani 1 1 d . . . O10W O 0.7797(3) 0.4038(3) 0.4138(2) 0.0503(11) Uani 1 1 d . . . O11W O 0.5815(3) 0.4709(3) 0.4973(3) 0.0577(13) Uani 1 1 d . . . O12W O 0.4667(3) 0.3225(3) 0.3739(3) 0.0596(13) Uani 1 1 d . . . Cl1 Cl 0.67683(12) 0.00383(11) 0.25780(9) 0.0476(4) Uani 1 1 d . . . Cl2 Cl 0.80430(12) 0.18567(11) 0.43784(9) 0.0478(4) Uani 1 1 d . . . Cl3 Cl 0.62534(11) -0.02503(13) 0.41527(10) 0.0539(4) Uani 1 1 d . . . Cl4 Cl 0.86288(11) 0.00211(11) 0.42619(11) 0.0554(5) Uani 1 1 d . . . Zn1 Zn 0.74003(5) 0.04015(5) 0.38385(4) 0.03903(18) Uani 1 1 d . . . Ce1 Ce -0.145194(19) 0.042142(18) 0.107377(15) 0.02757(11) Uani 1 1 d . . . Ce2 Ce 0.642876(19) 0.375885(17) 0.444261(15) 0.02352(11) Uani 1 1 d . . . O3 O 0.0153(3) 0.2754(2) 0.0480(2) 0.0420(10) Uani 1 1 d . . . O7 O 0.0687(3) -0.0643(3) 0.2236(2) 0.0408(10) Uani 1 1 d . . . O10 O 0.3401(3) 0.5637(3) 0.3243(2) 0.0410(10) Uani 1 1 d . . . O11 O 0.5017(3) 0.4990(3) 0.2720(2) 0.0444(10) Uani 1 1 d . . . C1 C -0.0348(3) 0.0947(3) 0.3115(3) 0.0248(10) Uani 1 1 d . . . C2 C 0.0699(3) 0.1328(3) 0.4370(3) 0.0229(10) Uani 1 1 d . . . H2 H 0.0571 0.1005 0.4710 0.027 Uiso 1 1 calc R . . C3 C 0.0218(4) 0.1961(3) 0.4264(3) 0.0255(10) Uani 1 1 d . . . H3 H -0.0132 0.1942 0.4559 0.031 Uiso 1 1 calc R . . C4 C 0.1861(4) 0.2751(3) 0.4784(3) 0.0262(11) Uani 1 1 d . . . C5 C -0.1030(3) 0.2009(3) 0.3086(3) 0.0266(11) Uani 1 1 d . . . H5A H -0.1563 0.1564 0.2627 0.032 Uiso 1 1 calc R . . H5B H -0.1289 0.2184 0.3404 0.032 Uiso 1 1 calc R . . C6 C 0.0925(4) 0.3600(3) 0.4626(3) 0.0261(11) Uani 1 1 d . . . H6A H 0.1508 0.4038 0.5057 0.031 Uiso 1 1 calc R . . H6B H 0.0399 0.3528 0.4743 0.031 Uiso 1 1 calc R . . C7 C -0.0586(4) 0.2672(3) 0.2217(3) 0.0271(11) Uani 1 1 d . . . C8 C -0.0163(3) 0.3625(3) 0.3356(3) 0.0237(10) Uani 1 1 d . . . H8 H -0.0599 0.3755 0.3516 0.028 Uiso 1 1 calc R . . C9 C 0.0040(4) 0.4137(3) 0.2830(3) 0.0253(11) Uani 1 1 d . . . H9 H -0.0340 0.4473 0.2705 0.030 Uiso 1 1 calc R . . C10 C 0.1438(4) 0.4573(3) 0.3940(3) 0.0247(11) Uani 1 1 d . . . C11 C -0.0349(4) 0.3614(4) 0.1465(3) 0.0300(11) Uani 1 1 d . . . H11A H -0.0796 0.3065 0.1064 0.036 Uiso 1 1 calc R . . H11B H -0.0639 0.4022 0.1398 0.036 Uiso 1 1 calc R . . C12 C 0.1537(4) 0.5410(3) 0.3062(3) 0.0300(11) Uani 1 1 d . . . H12A H 0.2110 0.5832 0.3510 0.036 Uiso 1 1 calc R . . H12B H 0.1123 0.5696 0.2875 0.036 Uiso 1 1 calc R . . C13 C 0.0643(4) 0.3513(3) 0.0864(3) 0.0305(12) Uani 1 1 d . . . C14 C 0.1155(4) 0.4866(3) 0.1694(3) 0.0261(11) Uani 1 1 d . . . H14 H 0.0813 0.5232 0.1565 0.031 Uiso 1 1 calc R . . C15 C 0.1803(4) 0.4936(3) 0.1332(3) 0.0280(11) Uani 1 1 d . . . H15 H 0.1809 0.5369 0.1060 0.034 Uiso 1 1 calc R . . C16 C 0.2702(4) 0.5352(3) 0.2626(3) 0.0293(11) Uani 1 1 d . . . C17 C 0.1649(4) 0.3875(4) 0.0239(3) 0.0318(12) Uani 1 1 d . . . H17A H 0.1733 0.4355 0.0026 0.038 Uiso 1 1 calc R . . H17B H 0.1119 0.3354 -0.0158 0.038 Uiso 1 1 calc R . . C18 C 0.3611(4) 0.5527(3) 0.1906(3) 0.0318(12) Uani 1 1 d . . . H18A H 0.3566 0.5896 0.1581 0.038 Uiso 1 1 calc R . . H18B H 0.4134 0.5890 0.2403 0.038 Uiso 1 1 calc R . . C19 C 0.2500(4) 0.2967(3) 0.0221(3) 0.0305(12) Uani 1 1 d . . . C20 C 0.3446(3) 0.4439(3) 0.0828(3) 0.0253(10) Uani 1 1 d . . . H20 H 0.3482 0.4865 0.0549 0.030 Uiso 1 1 calc R . . C21 C 0.4067(4) 0.3977(3) 0.0798(3) 0.0263(11) Uani 1 1 d . . . H21 H 0.4425 0.4203 0.0528 0.032 Uiso 1 1 calc R . . C22 C 0.4555(4) 0.4689(3) 0.2043(3) 0.0304(12) Uani 1 1 d . . . C23 C 0.3615(4) 0.2428(3) 0.0088(3) 0.0287(11) Uani 1 1 d . . . H23A H 0.4048 0.2701 -0.0107 0.034 Uiso 1 1 calc R . . H23B H 0.3030 0.1979 -0.0334 0.034 Uiso 1 1 calc R . . C24 C 0.5511(4) 0.3973(3) 0.1828(3) 0.0280(11) Uani 1 1 d . . . H24A H 0.5961 0.4346 0.2343 0.034 Uiso 1 1 calc R . . H24B H 0.5822 0.4123 0.1516 0.034 Uiso 1 1 calc R . . C25 C 0.3603(3) 0.1183(3) 0.0574(3) 0.0233(10) Uani 1 1 d . . . C26 C 0.5040(3) 0.2415(3) 0.1139(3) 0.0240(10) Uani 1 1 d . . . H26 H 0.5444 0.2623 0.0898 0.029 Uiso 1 1 calc R . . C27 C 0.5187(3) 0.1673(3) 0.1445(3) 0.0244(10) Uani 1 1 d . . . H27 H 0.5621 0.1497 0.1314 0.029 Uiso 1 1 calc R . . C28 C 0.5616(3) 0.2850(3) 0.2428(3) 0.0247(11) Uani 1 1 d . . . C29 C 0.4016(4) 0.0140(3) 0.1195(3) 0.0275(11) Uani 1 1 d . . . H29A H 0.3425 -0.0284 0.0762 0.033 Uiso 1 1 calc R . . H29B H 0.4522 -0.0027 0.1213 0.033 Uiso 1 1 calc R . . C30 C 0.5990(3) 0.1668(3) 0.2788(3) 0.0247(10) Uani 1 1 d . . . H30A H 0.6514 0.2135 0.3237 0.030 Uiso 1 1 calc R . . H30B H 0.6256 0.1330 0.2588 0.030 Uiso 1 1 calc R . . C31 C 0.3054(4) -0.0254(3) 0.1851(3) 0.0254(11) Uani 1 1 d . . . C32 C 0.4685(3) 0.0226(3) 0.2565(3) 0.0234(10) Uani 1 1 d . . . H32 H 0.5022 -0.0129 0.2506 0.028 Uiso 1 1 calc R . . C33 C 0.4176(4) -0.0058(3) 0.3039(3) 0.0260(11) Uani 1 1 d . . . H33 H 0.4285 -0.0537 0.3215 0.031 Uiso 1 1 calc R . . C34 C 0.5254(3) 0.1391(3) 0.3609(3) 0.0233(10) Uani 1 1 d . . . C35 C 0.2413(4) -0.0835(3) 0.2657(3) 0.0264(11) Uani 1 1 d . . . H35A H 0.1847 -0.1154 0.2173 0.032 Uiso 1 1 calc R . . H35B H 0.2572 -0.1262 0.2883 0.032 Uiso 1 1 calc R . . C36 C 0.4470(4) 0.0743(3) 0.4318(3) 0.0262(10) Uani 1 1 d . . . H36A H 0.4994 0.1256 0.4727 0.031 Uiso 1 1 calc R . . H36B H 0.4509 0.0232 0.4459 0.031 Uiso 1 1 calc R . . C37 C 0.1309(4) -0.0347(3) 0.2886(3) 0.0328(12) Uani 1 1 d . . . C38 C 0.2727(3) -0.0037(3) 0.3940(3) 0.0246(10) Uani 1 1 d . . . H38 H 0.2845 -0.0503 0.4136 0.030 Uiso 1 1 calc R . . C39 C 0.2080(3) 0.0234(3) 0.4186(3) 0.0241(10) Uani 1 1 d . . . H39 H 0.1925 -0.0071 0.4528 0.029 Uiso 1 1 calc R . . C40 C 0.3539(3) 0.1422(3) 0.4629(3) 0.0268(11) Uani 1 1 d . . . C41 C 0.0359(4) -0.0060(3) 0.3456(3) 0.0305(11) Uani 1 1 d . . . H41A H 0.0253 -0.0355 0.3812 0.037 Uiso 1 1 calc R . . H41B H -0.0150 -0.0427 0.2955 0.037 Uiso 1 1 calc R . . C42 C 0.2447(3) 0.1645(3) 0.5065(3) 0.0256(10) Uani 1 1 d . . . H42A H 0.3026 0.2164 0.5413 0.031 Uiso 1 1 calc R . . H42B H 0.2256 0.1284 0.5357 0.031 Uiso 1 1 calc R . . N1 N 0.0296(3) 0.0759(3) 0.3620(2) 0.0259(9) Uani 1 1 d . . . N2 N -0.0412(3) 0.1627(3) 0.3470(2) 0.0254(9) Uani 1 1 d . . . N3 N 0.1700(3) 0.1900(3) 0.4677(2) 0.0263(9) Uani 1 1 d . . . N4 N 0.1001(3) 0.2790(3) 0.4515(2) 0.0270(9) Uani 1 1 d . . . N5 N -0.0586(3) 0.2732(3) 0.2898(2) 0.0248(9) Uani 1 1 d . . . N6 N -0.0198(3) 0.3470(3) 0.2176(2) 0.0269(9) Uani 1 1 d . . . N7 N 0.0769(3) 0.3906(3) 0.3982(2) 0.0252(9) Uani 1 1 d . . . N8 N 0.1059(3) 0.4700(3) 0.3265(2) 0.0265(9) Uani 1 1 d . . . N9 N 0.0510(3) 0.3952(3) 0.1399(2) 0.0298(10) Uani 1 1 d . . . N10 N 0.1413(3) 0.4069(3) 0.0832(2) 0.0310(10) Uani 1 1 d . . . N11 N 0.1804(3) 0.5156(3) 0.2497(2) 0.0316(10) Uani 1 1 d . . . N12 N 0.2725(3) 0.5190(3) 0.1961(2) 0.0298(10) Uani 1 1 d . . . N13 N 0.2502(3) 0.3738(3) 0.0486(2) 0.0312(10) Uani 1 1 d . . . N14 N 0.3395(3) 0.3072(3) 0.0415(2) 0.0294(10) Uani 1 1 d . . . N15 N 0.3825(3) 0.4859(3) 0.1617(2) 0.0296(10) Uani 1 1 d . . . N16 N 0.4693(3) 0.4153(3) 0.1581(2) 0.0301(10) Uani 1 1 d . . . N17 N 0.4045(3) 0.2024(3) 0.0611(2) 0.0265(9) Uani 1 1 d . . . N18 N 0.4229(3) 0.0982(3) 0.1088(2) 0.0259(9) Uani 1 1 d . . . N19 N 0.5299(3) 0.3079(3) 0.1801(2) 0.0248(9) Uani 1 1 d . . . N20 N 0.5577(3) 0.2045(3) 0.2245(2) 0.0235(9) Uani 1 1 d . . . N21 N 0.3921(3) 0.0100(3) 0.1860(2) 0.0262(9) Uani 1 1 d . . . N22 N 0.3190(3) -0.0324(3) 0.2533(2) 0.0257(9) Uani 1 1 d . . . N23 N 0.5334(3) 0.1116(3) 0.2994(2) 0.0254(9) Uani 1 1 d . . . N24 N 0.4595(3) 0.0733(3) 0.3661(2) 0.0250(9) Uani 1 1 d . . . N25 N 0.2190(3) -0.0335(3) 0.3130(2) 0.0268(9) Uani 1 1 d . . . N26 N 0.1240(3) 0.0020(3) 0.3488(2) 0.0301(10) Uani 1 1 d . . . N27 N 0.3589(3) 0.0751(3) 0.4242(2) 0.0254(9) Uani 1 1 d . . . N28 N 0.2640(3) 0.1171(3) 0.4554(2) 0.0260(9) Uani 1 1 d . . . O1 O -0.0814(3) 0.0549(2) 0.24391(19) 0.0339(8) Uani 1 1 d . . . O2 O -0.0901(3) 0.1987(2) 0.17282(19) 0.0315(8) Uani 1 1 d . . . O4 O 0.1777(3) 0.2276(3) -0.0122(2) 0.0447(10) Uani 1 1 d . . . O5 O 0.2767(2) 0.0682(2) 0.01331(19) 0.0311(8) Uani 1 1 d . . . O6 O 0.2270(3) -0.0475(3) 0.1306(2) 0.0356(9) Uani 1 1 d . . . O8 O 0.2642(3) 0.3360(2) 0.5076(2) 0.0350(9) Uani 1 1 d . . . O9 O 0.2262(3) 0.5006(2) 0.44371(19) 0.0304(8) Uani 1 1 d . . . O12 O 0.5919(3) 0.3309(2) 0.30649(19) 0.0287(8) Uani 1 1 d . . . O13 O 0.5733(3) 0.2127(2) 0.4063(2) 0.0336(8) Uani 1 1 d . . . O14 O 0.4189(3) 0.2147(2) 0.4994(2) 0.0396(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl9 0.0358(14) 0.096(2) 0.132(3) -0.067(2) -0.0108(17) 0.0334(15) Cl10 0.091(3) 0.080(3) 0.069(3) 0.050(2) 0.029(2) 0.050(2) Cl11 0.066(3) 0.243(10) 0.096(5) -0.119(6) 0.068(4) -0.093(6) Cl12 0.085(4) 0.116(4) 0.108(4) 0.013(3) 0.050(3) 0.036(3) Zn2 0.0646(12) 0.0836(13) 0.0691(13) 0.0304(11) 0.0311(11) 0.0294(11) Zn2' 0.124(2) 0.112(2) 0.119(2) 0.0496(19) 0.058(2) 0.0540(19) Cl5 0.0858(18) 0.159(3) 0.188(3) 0.122(3) 0.081(2) 0.070(2) Cl6 0.113(2) 0.179(3) 0.166(3) 0.124(3) 0.093(2) 0.090(2) Cl7 0.275(7) 0.372(9) 0.182(5) 0.200(6) 0.152(5) 0.226(7) Cl8 0.173(5) 0.085(3) 0.119(4) 0.022(2) 0.049(3) 0.056(3) Cl8' 0.173(5) 0.085(3) 0.119(4) 0.022(2) 0.049(3) 0.056(3) O1W 0.049(3) 0.047(2) 0.021(2) 0.0022(18) 0.0111(19) 0.009(2) O2W 0.032(2) 0.042(2) 0.038(2) -0.0084(18) 0.0032(18) 0.0187(18) O3W 0.027(2) 0.059(3) 0.051(3) -0.009(2) 0.010(2) 0.004(2) O4W 0.038(2) 0.053(3) 0.034(2) -0.003(2) 0.019(2) 0.007(2) O5W 0.040(3) 0.084(4) 0.046(3) -0.008(2) 0.024(2) 0.021(2) O6W 0.028(2) 0.056(3) 0.083(4) -0.007(3) 0.017(2) 0.012(2) O7W 0.043(2) 0.040(2) 0.032(2) 0.0098(17) 0.0126(19) 0.0217(19) O8W 0.034(2) 0.046(2) 0.028(2) -0.0035(18) 0.0164(18) 0.0014(18) O9W 0.052(3) 0.0281(19) 0.033(2) 0.0025(17) 0.006(2) 0.0152(19) O10W 0.028(2) 0.079(3) 0.039(2) 0.016(2) 0.0162(19) 0.017(2) O11W 0.054(3) 0.058(3) 0.063(3) 0.003(2) 0.030(3) 0.030(2) O12W 0.035(2) 0.068(3) 0.052(3) -0.008(2) 0.008(2) 0.020(2) Cl1 0.0591(10) 0.0567(9) 0.0409(8) 0.0129(7) 0.0316(8) 0.0314(8) Cl2 0.0551(9) 0.0560(9) 0.0444(9) 0.0122(7) 0.0271(8) 0.0337(8) Cl3 0.0371(8) 0.0906(12) 0.0493(9) 0.0411(9) 0.0256(8) 0.0302(8) Cl4 0.0395(8) 0.0660(10) 0.0897(13) 0.0527(10) 0.0397(9) 0.0321(8) Zn1 0.0380(4) 0.0525(4) 0.0419(4) 0.0251(3) 0.0243(3) 0.0253(3) Ce1 0.01877(17) 0.03006(17) 0.01974(17) -0.00457(13) 0.00484(13) 0.00438(13) Ce2 0.01887(16) 0.02369(16) 0.01780(17) -0.00083(12) 0.00421(13) 0.00569(12) O3 0.041(2) 0.032(2) 0.034(2) -0.0045(18) 0.0153(19) 0.0039(18) O7 0.030(2) 0.050(2) 0.024(2) -0.0048(18) 0.0002(18) 0.0177(19) O10 0.033(2) 0.050(2) 0.024(2) -0.0016(18) 0.0064(18) 0.0125(19) O11 0.053(3) 0.047(2) 0.023(2) 0.0037(18) 0.005(2) 0.028(2) C1 0.021(2) 0.023(2) 0.021(3) 0.001(2) 0.007(2) 0.004(2) C2 0.024(2) 0.021(2) 0.019(2) 0.0049(19) 0.009(2) 0.0062(19) C3 0.026(3) 0.028(2) 0.019(2) 0.003(2) 0.010(2) 0.009(2) C4 0.025(3) 0.023(2) 0.021(2) 0.001(2) 0.007(2) 0.007(2) C5 0.013(2) 0.036(3) 0.023(3) 0.005(2) 0.005(2) 0.008(2) C6 0.028(3) 0.025(2) 0.017(2) 0.001(2) 0.005(2) 0.010(2) C7 0.019(2) 0.032(3) 0.021(3) 0.004(2) 0.006(2) 0.007(2) C8 0.020(2) 0.029(2) 0.015(2) 0.002(2) 0.003(2) 0.011(2) C9 0.025(3) 0.024(2) 0.017(2) 0.002(2) 0.003(2) 0.009(2) C10 0.030(3) 0.020(2) 0.018(3) -0.002(2) 0.008(2) 0.011(2) C11 0.023(3) 0.038(3) 0.019(3) 0.007(2) 0.003(2) 0.012(2) C12 0.034(3) 0.022(2) 0.024(3) -0.002(2) 0.012(2) 0.007(2) C13 0.029(3) 0.035(3) 0.017(2) 0.004(2) 0.006(2) 0.009(2) C14 0.027(3) 0.031(3) 0.015(2) 0.004(2) 0.005(2) 0.012(2) C15 0.033(3) 0.028(2) 0.018(2) 0.006(2) 0.008(2) 0.013(2) C16 0.030(3) 0.028(3) 0.023(3) 0.001(2) 0.011(2) 0.009(2) C17 0.029(3) 0.040(3) 0.020(3) 0.001(2) 0.007(2) 0.015(2) C18 0.034(3) 0.025(2) 0.034(3) 0.002(2) 0.018(3) 0.008(2) C19 0.036(3) 0.028(3) 0.021(3) 0.001(2) 0.012(2) 0.011(2) C20 0.024(3) 0.028(2) 0.021(2) 0.007(2) 0.010(2) 0.009(2) C21 0.031(3) 0.024(2) 0.017(2) 0.005(2) 0.009(2) 0.008(2) C22 0.032(3) 0.024(2) 0.021(3) -0.001(2) 0.004(2) 0.009(2) C23 0.032(3) 0.030(3) 0.017(2) 0.001(2) 0.006(2) 0.013(2) C24 0.021(2) 0.024(2) 0.027(3) 0.003(2) 0.007(2) 0.002(2) C25 0.023(3) 0.027(2) 0.016(2) 0.002(2) 0.009(2) 0.007(2) C26 0.023(2) 0.026(2) 0.017(2) 0.004(2) 0.005(2) 0.009(2) C27 0.020(2) 0.027(2) 0.021(2) 0.001(2) 0.008(2) 0.009(2) C28 0.018(2) 0.022(2) 0.021(3) -0.004(2) 0.004(2) 0.0045(19) C29 0.030(3) 0.021(2) 0.023(3) -0.001(2) 0.012(2) 0.006(2) C30 0.020(2) 0.024(2) 0.026(3) 0.007(2) 0.009(2) 0.006(2) C31 0.026(3) 0.023(2) 0.022(3) 0.001(2) 0.009(2) 0.009(2) C32 0.019(2) 0.022(2) 0.022(2) 0.001(2) 0.007(2) 0.0072(19) C33 0.026(3) 0.021(2) 0.025(3) 0.001(2) 0.009(2) 0.008(2) C34 0.020(2) 0.026(2) 0.020(2) 0.006(2) 0.005(2) 0.010(2) C35 0.027(3) 0.024(2) 0.027(3) 0.005(2) 0.015(2) 0.008(2) C36 0.023(2) 0.036(3) 0.018(2) 0.007(2) 0.007(2) 0.013(2) C37 0.031(3) 0.023(2) 0.032(3) 0.002(2) 0.010(3) 0.005(2) C38 0.023(2) 0.024(2) 0.019(2) 0.003(2) 0.006(2) 0.008(2) C39 0.020(2) 0.020(2) 0.022(2) 0.0017(19) 0.006(2) 0.0034(19) C40 0.022(3) 0.029(3) 0.023(3) 0.006(2) 0.007(2) 0.008(2) C41 0.027(3) 0.021(2) 0.034(3) 0.003(2) 0.012(2) 0.006(2) C42 0.021(2) 0.027(2) 0.022(2) 0.003(2) 0.007(2) 0.009(2) N1 0.025(2) 0.022(2) 0.021(2) -0.0020(17) 0.0065(18) 0.0081(17) N2 0.024(2) 0.027(2) 0.020(2) 0.0037(17) 0.0060(18) 0.0112(18) N3 0.020(2) 0.0209(19) 0.029(2) 0.0020(17) 0.0069(19) 0.0075(17) N4 0.024(2) 0.025(2) 0.023(2) 0.0026(18) 0.0065(19) 0.0088(18) N5 0.024(2) 0.027(2) 0.015(2) -0.0015(17) 0.0060(18) 0.0078(18) N6 0.026(2) 0.031(2) 0.014(2) 0.0044(17) 0.0055(18) 0.0078(19) N7 0.023(2) 0.027(2) 0.016(2) 0.0016(17) 0.0053(18) 0.0065(18) N8 0.023(2) 0.026(2) 0.019(2) 0.0039(17) 0.0056(18) 0.0047(17) N9 0.031(2) 0.027(2) 0.021(2) 0.0013(18) 0.0099(19) 0.0059(19) N10 0.031(2) 0.031(2) 0.022(2) -0.0010(18) 0.010(2) 0.0101(19) N11 0.032(2) 0.036(2) 0.016(2) 0.0016(19) 0.0073(19) 0.010(2) N12 0.024(2) 0.034(2) 0.022(2) 0.0015(18) 0.0055(19) 0.0097(19) N13 0.026(2) 0.029(2) 0.027(2) -0.0002(19) 0.0056(19) 0.0086(19) N14 0.031(2) 0.024(2) 0.024(2) 0.0027(18) 0.008(2) 0.0100(19) N15 0.034(2) 0.029(2) 0.026(2) 0.0045(18) 0.013(2) 0.0150(19) N16 0.031(2) 0.028(2) 0.020(2) 0.0023(18) 0.0044(19) 0.0116(19) N17 0.021(2) 0.026(2) 0.018(2) -0.0001(17) 0.0004(18) 0.0074(17) N18 0.023(2) 0.024(2) 0.019(2) 0.0014(17) 0.0056(18) 0.0041(17) N19 0.024(2) 0.0216(19) 0.017(2) 0.0008(16) 0.0022(17) 0.0075(17) N20 0.024(2) 0.024(2) 0.015(2) 0.0036(16) 0.0051(17) 0.0071(17) N21 0.022(2) 0.028(2) 0.020(2) 0.0009(17) 0.0071(18) 0.0072(18) N22 0.016(2) 0.032(2) 0.019(2) 0.0048(18) 0.0043(17) 0.0059(17) N23 0.022(2) 0.022(2) 0.022(2) 0.0009(17) 0.0085(18) 0.0029(17) N24 0.021(2) 0.028(2) 0.019(2) 0.0011(17) 0.0070(18) 0.0075(17) N25 0.022(2) 0.031(2) 0.021(2) 0.0025(18) 0.0069(18) 0.0108(18) N26 0.024(2) 0.031(2) 0.028(2) 0.0019(19) 0.0089(19) 0.0116(19) N27 0.022(2) 0.030(2) 0.021(2) 0.0053(18) 0.0075(18) 0.0119(18) N28 0.025(2) 0.0204(19) 0.021(2) 0.0025(17) 0.0056(18) 0.0042(17) O1 0.037(2) 0.0325(19) 0.0175(18) -0.0016(15) 0.0066(17) 0.0096(17) O2 0.032(2) 0.0293(19) 0.0204(18) -0.0024(15) 0.0083(16) 0.0074(16) O4 0.028(2) 0.035(2) 0.044(2) -0.0124(19) 0.0084(19) 0.0027(18) O5 0.0225(19) 0.0324(19) 0.0181(18) -0.0011(15) -0.0012(16) 0.0051(16) O6 0.0229(19) 0.046(2) 0.0187(19) 0.0006(16) 0.0025(16) 0.0051(17) O8 0.0241(19) 0.0268(18) 0.039(2) -0.0002(17) 0.0078(17) 0.0065(16) O9 0.0258(19) 0.0270(18) 0.0211(18) -0.0021(15) 0.0030(16) 0.0051(15) O12 0.032(2) 0.0260(17) 0.0175(18) 0.0017(14) 0.0050(15) 0.0103(15) O13 0.033(2) 0.0286(19) 0.0228(19) -0.0042(16) 0.0080(16) 0.0054(16) O14 0.028(2) 0.029(2) 0.046(2) -0.0039(18) 0.0162(19) 0.0024(17) _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 Cl11 Cl11 1.80(2) 2_655 ? Zn2 Zn2' 1.476(4) . ? Zn2 Cl7 2.2517(19) . ? Zn2 Cl6 2.268(3) . ? Zn2 Cl5 2.2796(18) . ? Zn2 Cl8 2.283(2) . ? Zn2' Cl7 2.246(2) . ? Zn2' Cl8' 2.282(2) . ? Zn2' Cl6 2.2877(19) . ? Zn2' Cl5 2.2947(19) . ? O1W Ce1 2.524(4) . ? O2W Ce1 2.525(4) . ? O3W Ce1 2.504(4) . ? O4W Ce1 2.564(4) . ? O5W Ce1 2.543(4) . ? O6W Ce1 2.541(5) . ? O7W Ce2 2.576(4) . ? O8W Ce2 2.527(4) . ? O9W Ce2 2.524(4) . ? O10W Ce2 2.532(4) . ? O11W Ce2 2.541(4) . ? O12W Ce2 2.504(4) . ? Cl1 Zn1 2.2651(17) . ? Cl2 Zn1 2.2712(18) . ? Cl3 Zn1 2.2631(17) . ? Cl4 Zn1 2.2785(16) . ? Ce1 O5 2.500(3) 2 ? Ce1 O2 2.506(3) . ? Ce1 O1 2.515(4) . ? Ce2 O9 2.495(3) 2_666 ? Ce2 O12 2.514(3) . ? Ce2 O13 2.521(4) . ? O3 C13 1.223(6) . ? O7 C37 1.225(7) . ? O10 C16 1.230(6) . ? O11 C22 1.217(6) . ? C1 O1 1.236(6) . ? C1 N1 1.349(6) . ? C1 N2 1.351(6) . ? C2 N1 1.449(6) . ? C2 N3 1.454(6) . ? C2 C3 1.559(7) . ? C2 H2 0.9900 . ? C3 N4 1.434(6) . ? C3 N2 1.445(6) . ? C3 H3 0.9900 . ? C4 O8 1.218(6) . ? C4 N3 1.368(6) . ? C4 N4 1.373(7) . ? C5 N5 1.410(7) . ? C5 N2 1.455(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.440(6) . ? C6 N7 1.449(7) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.230(6) . ? C7 N6 1.341(7) . ? C7 N5 1.377(7) . ? C8 N5 1.448(6) . ? C8 N7 1.452(6) . ? C8 C9 1.546(7) . ? C8 H8 0.9900 . ? C9 N6 1.453(6) . ? C9 N8 1.467(6) . ? C9 H9 0.9900 . ? C10 O9 1.235(6) . ? C10 N7 1.354(7) . ? C10 N8 1.361(6) . ? C11 N9 1.439(7) . ? C11 N6 1.445(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.434(7) . ? C12 N11 1.456(7) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 N10 1.364(7) . ? C13 N9 1.373(7) . ? C14 N9 1.451(6) . ? C14 N11 1.467(6) . ? C14 C15 1.523(8) . ? C14 H14 0.9900 . ? C15 N10 1.450(6) . ? C15 N12 1.453(6) . ? C15 H15 0.9900 . ? C16 N11 1.345(7) . ? C16 N12 1.364(7) . ? C17 N10 1.444(7) . ? C17 N13 1.448(7) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N15 1.437(6) . ? C18 N12 1.469(7) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.237(7) . ? C19 N14 1.348(7) . ? C19 N13 1.361(7) . ? C20 N15 1.446(6) . ? C20 N13 1.449(6) . ? C20 C21 1.532(7) . ? C20 H20 0.9900 . ? C21 N16 1.453(6) . ? C21 N14 1.455(6) . ? C21 H21 0.9900 . ? C22 N15 1.362(7) . ? C22 N16 1.368(7) . ? C23 N14 1.442(6) . ? C23 N17 1.451(7) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N16 1.435(7) . ? C24 N19 1.448(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O5 1.238(6) . ? C25 N18 1.355(6) . ? C25 N17 1.364(6) . ? C26 N17 1.444(6) . ? C26 N19 1.450(6) . ? C26 C27 1.551(7) . ? C26 H26 0.9900 . ? C27 N20 1.451(6) . ? C27 N18 1.456(6) . ? C27 H27 0.9900 . ? C28 O12 1.226(6) . ? C28 N19 1.356(7) . ? C28 N20 1.359(6) . ? C29 N21 1.435(7) . ? C29 N18 1.442(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N20 1.432(6) . ? C30 N23 1.440(7) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O6 1.243(6) . ? C31 N22 1.348(7) . ? C31 N21 1.378(7) . ? C32 N23 1.441(6) . ? C32 N21 1.441(6) . ? C32 C33 1.552(7) . ? C32 H32 0.9900 . ? C33 N22 1.443(6) . ? C33 N24 1.465(6) . ? C33 H33 0.9900 . ? C34 O13 1.236(6) . ? C34 N24 1.346(7) . ? C34 N23 1.351(6) . ? C35 N25 1.445(6) . ? C35 N22 1.451(7) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N24 1.433(6) . ? C36 N27 1.442(6) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 N26 1.366(7) . ? C37 N25 1.368(7) . ? C38 N27 1.445(6) . ? C38 N25 1.453(6) . ? C38 C39 1.540(7) . ? C38 H38 0.9900 . ? C39 N26 1.458(6) . ? C39 N28 1.467(6) . ? C39 H39 0.9900 . ? C40 O14 1.228(6) . ? C40 N27 1.354(6) . ? C40 N28 1.371(7) . ? C41 N26 1.424(7) . ? C41 N1 1.454(6) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 N28 1.438(6) . ? C42 N3 1.456(6) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? O5 Ce1 2.500(3) 2 ? O9 Ce2 2.495(3) 2_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Zn2' Zn2 Cl7 70.63(11) . . ? Zn2' Zn2 Cl6 71.82(13) . . ? Cl7 Zn2 Cl6 109.42(16) . . ? Zn2' Zn2 Cl5 71.74(10) . . ? Cl7 Zn2 Cl5 112.43(16) . . ? Cl6 Zn2 Cl5 109.08(13) . . ? Zn2' Zn2 Cl8 164.3(3) . . ? Cl7 Zn2 Cl8 93.7(3) . . ? Cl6 Zn2 Cl8 115.5(2) . . ? Cl5 Zn2 Cl8 115.8(2) . . ? Zn2 Zn2' Cl7 71.06(11) . . ? Zn2 Zn2' Cl8' 169.9(3) . . ? Cl7 Zn2' Cl8' 99.2(3) . . ? Zn2 Zn2' Cl6 70.38(15) . . ? Cl7 Zn2' Cl6 108.93(17) . . ? Cl8' Zn2' Cl6 111.5(3) . . ? Zn2 Zn2' Cl5 70.63(10) . . ? Cl7 Zn2' Cl5 112.08(15) . . ? Cl8' Zn2' Cl5 116.9(2) . . ? Cl6 Zn2' Cl5 107.87(15) . . ? Zn2 Cl5 Zn2' 37.64(9) . . ? Zn2 Cl6 Zn2' 37.80(10) . . ? Zn2' Cl7 Zn2 38.31(10) . . ? Cl3 Zn1 Cl1 109.26(7) . . ? Cl3 Zn1 Cl2 108.88(7) . . ? Cl1 Zn1 Cl2 111.74(7) . . ? Cl3 Zn1 Cl4 113.47(6) . . ? Cl1 Zn1 Cl4 107.77(7) . . ? Cl2 Zn1 Cl4 105.71(7) . . ? O5 Ce1 O3W 136.03(14) 2 . ? O5 Ce1 O2 136.74(12) 2 . ? O3W Ce1 O2 71.29(14) . . ? O5 Ce1 O1 136.98(12) 2 . ? O3W Ce1 O1 72.61(15) . . ? O2 Ce1 O1 75.07(12) . . ? O5 Ce1 O1W 79.07(13) 2 . ? O3W Ce1 O1W 86.62(16) . . ? O2 Ce1 O1W 68.77(13) . . ? O1 Ce1 O1W 142.54(12) . . ? O5 Ce1 O2W 82.67(12) 2 . ? O3W Ce1 O2W 80.90(15) . . ? O2 Ce1 O2W 140.44(12) . . ? O1 Ce1 O2W 70.00(13) . . ? O1W Ce1 O2W 138.06(14) . . ? O5 Ce1 O6W 76.96(14) 2 . ? O3W Ce1 O6W 137.92(15) . . ? O2 Ce1 O6W 66.97(13) . . ? O1 Ce1 O6W 101.06(16) . . ? O1W Ce1 O6W 73.77(18) . . ? O2W Ce1 O6W 137.35(16) . . ? O5 Ce1 O5W 68.41(14) 2 . ? O3W Ce1 O5W 67.63(15) . . ? O2 Ce1 O5W 121.81(15) . . ? O1 Ce1 O5W 125.88(15) . . ? O1W Ce1 O5W 69.42(17) . . ? O2W Ce1 O5W 68.79(17) . . ? O6W Ce1 O5W 133.05(18) . . ? O5 Ce1 O4W 71.16(13) 2 . ? O3W Ce1 O4W 137.15(17) . . ? O2 Ce1 O4W 113.80(13) . . ? O1 Ce1 O4W 68.49(13) . . ? O1W Ce1 O4W 135.90(15) . . ? O2W Ce1 O4W 69.64(15) . . ? O6W Ce1 O4W 68.42(17) . . ? O5W Ce1 O4W 124.38(16) . . ? O9 Ce2 O12W 135.32(13) 2_666 . ? O9 Ce2 O12 136.48(12) 2_666 . ? O12W Ce2 O12 71.00(15) . . ? O9 Ce2 O13 136.96(12) 2_666 . ? O12W Ce2 O13 73.32(15) . . ? O12 Ce2 O13 76.02(12) . . ? O9 Ce2 O9W 77.95(12) 2_666 . ? O12W Ce2 O9W 87.19(17) . . ? O12 Ce2 O9W 68.54(12) . . ? O13 Ce2 O9W 143.58(12) . . ? O9 Ce2 O8W 82.17(12) 2_666 . ? O12W Ce2 O8W 80.98(16) . . ? O12 Ce2 O8W 141.31(12) . . ? O13 Ce2 O8W 70.63(13) . . ? O9W Ce2 O8W 137.27(14) . . ? O9 Ce2 O10W 78.77(14) 2_666 . ? O12W Ce2 O10W 137.32(15) . . ? O12 Ce2 O10W 66.45(13) . . ? O13 Ce2 O10W 98.91(14) . . ? O9W Ce2 O10W 74.75(16) . . ? O8W Ce2 O10W 137.17(15) . . ? O9 Ce2 O11W 68.40(14) 2_666 . ? O12W Ce2 O11W 66.93(15) . . ? O12 Ce2 O11W 120.28(14) . . ? O13 Ce2 O11W 126.16(15) . . ? O9W Ce2 O11W 68.98(16) . . ? O8W Ce2 O11W 68.59(16) . . ? O10W Ce2 O11W 134.93(17) . . ? O9 Ce2 O7W 71.53(12) 2_666 . ? O12W Ce2 O7W 137.14(16) . . ? O12 Ce2 O7W 115.09(12) . . ? O13 Ce2 O7W 68.01(12) . . ? O9W Ce2 O7W 135.46(14) . . ? O8W Ce2 O7W 69.50(14) . . ? O10W Ce2 O7W 68.15(14) . . ? O11W Ce2 O7W 124.62(15) . . ? O1 C1 N1 125.3(4) . . ? O1 C1 N2 125.7(5) . . ? N1 C1 N2 109.0(4) . . ? N1 C2 N3 113.4(4) . . ? N1 C2 C3 103.7(4) . . ? N3 C2 C3 103.2(4) . . ? N1 C2 H2 112.0 . . ? N3 C2 H2 112.0 . . ? C3 C2 H2 112.0 . . ? N4 C3 N2 115.4(4) . . ? N4 C3 C2 103.3(4) . . ? N2 C3 C2 101.7(4) . . ? N4 C3 H3 111.9 . . ? N2 C3 H3 111.9 . . ? C2 C3 H3 111.9 . . ? O8 C4 N3 124.9(5) . . ? O8 C4 N4 126.9(5) . . ? N3 C4 N4 108.2(4) . . ? N5 C5 N2 114.6(4) . . ? N5 C5 H5A 108.6 . . ? N2 C5 H5A 108.6 . . ? N5 C5 H5B 108.6 . . ? N2 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? N4 C6 N7 113.1(4) . . ? N4 C6 H6A 109.0 . . ? N7 C6 H6A 109.0 . . ? N4 C6 H6B 109.0 . . ? N7 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? O2 C7 N6 126.0(5) . . ? O2 C7 N5 124.6(5) . . ? N6 C7 N5 109.4(4) . . ? N5 C8 N7 114.6(4) . . ? N5 C8 C9 102.9(4) . . ? N7 C8 C9 103.7(4) . . ? N5 C8 H8 111.7 . . ? N7 C8 H8 111.7 . . ? C9 C8 H8 111.7 . . ? N6 C9 N8 113.4(4) . . ? N6 C9 C8 103.7(4) . . ? N8 C9 C8 102.7(4) . . ? N6 C9 H9 112.1 . . ? N8 C9 H9 112.1 . . ? C8 C9 H9 112.1 . . ? O9 C10 N7 125.6(5) . . ? O9 C10 N8 125.1(5) . . ? N7 C10 N8 109.3(4) . . ? N9 C11 N6 113.1(4) . . ? N9 C11 H11A 109.0 . . ? N6 C11 H11A 109.0 . . ? N9 C11 H11B 109.0 . . ? N6 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? N8 C12 N11 113.8(4) . . ? N8 C12 H12A 108.8 . . ? N11 C12 H12A 108.8 . . ? N8 C12 H12B 108.8 . . ? N11 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N10 125.6(5) . . ? O3 C13 N9 126.0(5) . . ? N10 C13 N9 108.4(4) . . ? N9 C14 N11 113.8(4) . . ? N9 C14 C15 103.6(4) . . ? N11 C14 C15 103.8(4) . . ? N9 C14 H14 111.7 . . ? N11 C14 H14 111.7 . . ? C15 C14 H14 111.7 . . ? N10 C15 N12 113.5(4) . . ? N10 C15 C14 104.1(4) . . ? N12 C15 C14 103.4(4) . . ? N10 C15 H15 111.8 . . ? N12 C15 H15 111.8 . . ? C14 C15 H15 111.8 . . ? O10 C16 N11 126.0(5) . . ? O10 C16 N12 124.6(5) . . ? N11 C16 N12 109.3(4) . . ? N10 C17 N13 113.1(4) . . ? N10 C17 H17A 109.0 . . ? N13 C17 H17A 109.0 . . ? N10 C17 H17B 109.0 . . ? N13 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? N15 C18 N12 113.4(4) . . ? N15 C18 H18A 108.9 . . ? N12 C18 H18A 108.9 . . ? N15 C18 H18B 108.9 . . ? N12 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? O4 C19 N14 126.0(5) . . ? O4 C19 N13 124.1(5) . . ? N14 C19 N13 109.9(4) . . ? N15 C20 N13 114.6(4) . . ? N15 C20 C21 104.0(4) . . ? N13 C20 C21 103.4(4) . . ? N15 C20 H20 111.4 . . ? N13 C20 H20 111.4 . . ? C21 C20 H20 111.4 . . ? N16 C21 N14 113.8(4) . . ? N16 C21 C20 103.2(4) . . ? N14 C21 C20 103.9(4) . . ? N16 C21 H21 111.8 . . ? N14 C21 H21 111.8 . . ? C20 C21 H21 111.8 . . ? O11 C22 N15 124.9(5) . . ? O11 C22 N16 126.5(5) . . ? N15 C22 N16 108.5(4) . . ? N14 C23 N17 113.3(4) . . ? N14 C23 H23A 108.9 . . ? N17 C23 H23A 108.9 . . ? N14 C23 H23B 108.9 . . ? N17 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? N16 C24 N19 113.8(4) . . ? N16 C24 H24A 108.8 . . ? N19 C24 H24A 108.8 . . ? N16 C24 H24B 108.8 . . ? N19 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? O5 C25 N18 125.6(4) . . ? O5 C25 N17 125.3(5) . . ? N18 C25 N17 109.1(4) . . ? N17 C26 N19 114.1(4) . . ? N17 C26 C27 103.6(4) . . ? N19 C26 C27 103.3(4) . . ? N17 C26 H26 111.8 . . ? N19 C26 H26 111.8 . . ? C27 C26 H26 111.8 . . ? N20 C27 N18 114.2(4) . . ? N20 C27 C26 103.1(4) . . ? N18 C27 C26 102.8(4) . . ? N20 C27 H27 112.0 . . ? N18 C27 H27 112.0 . . ? C26 C27 H27 112.0 . . ? O12 C28 N19 125.3(4) . . ? O12 C28 N20 125.3(5) . . ? N19 C28 N20 109.4(4) . . ? N21 C29 N18 114.1(4) . . ? N21 C29 H29A 108.7 . . ? N18 C29 H29A 108.7 . . ? N21 C29 H29B 108.7 . . ? N18 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? N20 C30 N23 114.0(4) . . ? N20 C30 H30A 108.8 . . ? N23 C30 H30A 108.8 . . ? N20 C30 H30B 108.8 . . ? N23 C30 H30B 108.8 . . ? H30A C30 H30B 107.7 . . ? O6 C31 N22 125.3(5) . . ? O6 C31 N21 125.7(5) . . ? N22 C31 N21 108.9(4) . . ? N23 C32 N21 115.2(4) . . ? N23 C32 C33 102.5(4) . . ? N21 C32 C33 103.3(4) . . ? N23 C32 H32 111.7 . . ? N21 C32 H32 111.7 . . ? C33 C32 H32 111.7 . . ? N22 C33 N24 114.2(4) . . ? N22 C33 C32 103.4(4) . . ? N24 C33 C32 103.3(4) . . ? N22 C33 H33 111.7 . . ? N24 C33 H33 111.7 . . ? C32 C33 H33 111.7 . . ? O13 C34 N24 125.5(5) . . ? O13 C34 N23 125.0(5) . . ? N24 C34 N23 109.5(4) . . ? N25 C35 N22 114.4(4) . . ? N25 C35 H35A 108.7 . . ? N22 C35 H35A 108.7 . . ? N25 C35 H35B 108.7 . . ? N22 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? N24 C36 N27 115.0(4) . . ? N24 C36 H36A 108.5 . . ? N27 C36 H36A 108.5 . . ? N24 C36 H36B 108.5 . . ? N27 C36 H36B 108.5 . . ? H36A C36 H36B 107.5 . . ? O7 C37 N26 125.9(5) . . ? O7 C37 N25 125.5(5) . . ? N26 C37 N25 108.6(4) . . ? N27 C38 N25 114.5(4) . . ? N27 C38 C39 103.9(4) . . ? N25 C38 C39 102.9(4) . . ? N27 C38 H38 111.6 . . ? N25 C38 H38 111.6 . . ? C39 C38 H38 111.6 . . ? N26 C39 N28 112.8(4) . . ? N26 C39 C38 104.1(4) . . ? N28 C39 C38 103.1(4) . . ? N26 C39 H39 112.1 . . ? N28 C39 H39 112.1 . . ? C38 C39 H39 112.1 . . ? O14 C40 N27 126.2(5) . . ? O14 C40 N28 124.4(5) . . ? N27 C40 N28 109.4(4) . . ? N26 C41 N1 114.5(4) . . ? N26 C41 H41A 108.6 . . ? N1 C41 H41A 108.6 . . ? N26 C41 H41B 108.6 . . ? N1 C41 H41B 108.6 . . ? H41A C41 H41B 107.6 . . ? N28 C42 N3 111.9(4) . . ? N28 C42 H42A 109.2 . . ? N3 C42 H42A 109.2 . . ? N28 C42 H42B 109.2 . . ? N3 C42 H42B 109.2 . . ? H42A C42 H42B 107.9 . . ? C1 N1 C2 112.0(4) . . ? C1 N1 C41 122.2(4) . . ? C2 N1 C41 123.5(4) . . ? C1 N2 C3 113.5(4) . . ? C1 N2 C5 123.2(4) . . ? C3 N2 C5 123.2(4) . . ? C4 N3 C2 112.2(4) . . ? C4 N3 C42 121.9(4) . . ? C2 N3 C42 122.5(4) . . ? C4 N4 C3 112.9(4) . . ? C4 N4 C6 122.1(4) . . ? C3 N4 C6 123.7(4) . . ? C7 N5 C5 123.3(4) . . ? C7 N5 C8 111.7(4) . . ? C5 N5 C8 124.8(4) . . ? C7 N6 C11 121.1(4) . . ? C7 N6 C9 111.8(4) . . ? C11 N6 C9 123.1(4) . . ? C10 N7 C6 124.2(4) . . ? C10 N7 C8 111.8(4) . . ? C6 N7 C8 123.3(4) . . ? C10 N8 C12 124.3(4) . . ? C10 N8 C9 111.8(4) . . ? C12 N8 C9 122.8(4) . . ? C13 N9 C11 122.3(4) . . ? C13 N9 C14 111.7(4) . . ? C11 N9 C14 122.9(4) . . ? C13 N10 C17 123.0(4) . . ? C13 N10 C15 111.9(4) . . ? C17 N10 C15 123.3(4) . . ? C16 N11 C12 124.3(4) . . ? C16 N11 C14 111.5(4) . . ? C12 N11 C14 122.3(4) . . ? C16 N12 C15 111.8(4) . . ? C16 N12 C18 122.3(4) . . ? C15 N12 C18 122.6(4) . . ? C19 N13 C17 122.6(4) . . ? C19 N13 C20 111.4(4) . . ? C17 N13 C20 123.2(4) . . ? C19 N14 C23 122.8(4) . . ? C19 N14 C21 111.2(4) . . ? C23 N14 C21 123.5(4) . . ? C22 N15 C18 122.9(4) . . ? C22 N15 C20 112.0(4) . . ? C18 N15 C20 123.6(4) . . ? C22 N16 C24 123.1(4) . . ? C22 N16 C21 112.0(4) . . ? C24 N16 C21 123.0(4) . . ? C25 N17 C26 112.0(4) . . ? C25 N17 C23 123.9(4) . . ? C26 N17 C23 123.2(4) . . ? C25 N18 C29 124.5(4) . . ? C25 N18 C27 112.0(4) . . ? C29 N18 C27 122.8(4) . . ? C28 N19 C24 121.9(4) . . ? C28 N19 C26 112.0(4) . . ? C24 N19 C26 122.8(4) . . ? C28 N20 C30 123.1(4) . . ? C28 N20 C27 112.0(4) . . ? C30 N20 C27 124.4(4) . . ? C31 N21 C29 122.7(4) . . ? C31 N21 C32 111.8(4) . . ? C29 N21 C32 124.0(4) . . ? C31 N22 C33 112.5(4) . . ? C31 N22 C35 121.6(4) . . ? C33 N22 C35 123.7(4) . . ? C34 N23 C30 122.9(4) . . ? C34 N23 C32 113.1(4) . . ? C30 N23 C32 124.0(4) . . ? C34 N24 C36 124.0(4) . . ? C34 N24 C33 111.5(4) . . ? C36 N24 C33 123.1(4) . . ? C37 N25 C35 121.7(4) . . ? C37 N25 C38 112.5(4) . . ? C35 N25 C38 122.6(4) . . ? C37 N26 C41 122.7(4) . . ? C37 N26 C39 111.6(4) . . ? C41 N26 C39 122.8(4) . . ? C40 N27 C36 123.3(4) . . ? C40 N27 C38 112.0(4) . . ? C36 N27 C38 122.0(4) . . ? C40 N28 C42 121.4(4) . . ? C40 N28 C39 110.7(4) . . ? C42 N28 C39 121.5(4) . . ? C1 O1 Ce1 154.6(3) . . ? C7 O2 Ce1 162.2(4) . . ? C25 O5 Ce1 154.7(3) . 2 ? C10 O9 Ce2 155.5(3) . 2_666 ? C28 O12 Ce2 160.6(3) . . ? C34 O13 Ce2 154.4(3) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.381 _refine_diff_density_min -3.296 _refine_diff_density_rms 0.152 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.106 0.500 1.000 1128 379 ' ' 2 0.252 0.247 0.253 177 66 ' ' 3 0.748 0.753 0.747 176 61 ' ' _platon_squeeze_details ; ; data_p2 _database_code_depnum_ccdc_archive 'CCDC 905586' #TrackingRef '3 (905586).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H124 Cl10 N28 O55 Pr2 Zn2' _chemical_formula_weight 2668.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.8979(14) _cell_length_b 17.2593(15) _cell_length_c 20.3082(17) _cell_angle_alpha 98.015(3) _cell_angle_beta 112.613(3) _cell_angle_gamma 109.997(3) _cell_volume 4880.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.816 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720 _exptl_absorpt_coefficient_mu 1.852 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6065 _exptl_absorpt_correction_T_max 0.6971 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50292 _diffrn_reflns_av_R_equivalents 0.0747 _diffrn_reflns_av_sigmaI/netI 0.0824 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16931 _reflns_number_gt 13322 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1997P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16931 _refine_ls_number_parameters 977 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.1000 _refine_ls_R_factor_gt 0.0892 _refine_ls_wR_factor_ref 0.2679 _refine_ls_wR_factor_gt 0.2524 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl9 Cl 1.0000 0.0000 0.0000 0.114(2) Uani 1 2 d SU . . Cl10 Cl 0.3217(4) 0.3017(4) -0.1105(3) 0.0566(14) Uani 0.50 1 d P . . Cl11 Cl 0.4893(5) 0.5413(5) 0.4813(4) 0.110(3) Uani 0.50 1 d PU . . Cl12 Cl 0.6648(7) 0.3130(8) 0.2721(7) 0.135(4) Uani 0.50 1 d PU . . Cl1 Cl 0.19556(18) 0.31327(16) 0.06100(13) 0.0438(5) Uani 1 1 d . . . Cl2 Cl 0.13931(16) 0.49778(17) 0.07437(16) 0.0487(6) Uani 1 1 d . . . Cl3 Cl 0.32381(18) 0.49554(16) 0.24252(13) 0.0439(5) Uani 1 1 d . . . Cl4 Cl 0.37642(16) 0.5250(2) 0.08559(14) 0.0523(7) Uani 1 1 d . . . Cl5 Cl 1.2707(3) 0.2217(3) 0.3781(4) 0.133(2) Uani 1 1 d D . . Cl6 Cl 1.4057(3) 0.1126(4) 0.4865(3) 0.138(2) Uani 1 1 d D . . Cl7 Cl 1.2092(7) 0.1271(8) 0.5150(4) 0.229(5) Uani 1 1 d D . . Cl8 Cl 1.1364(6) -0.0199(3) 0.3526(5) 0.165(6) Uani 0.50 1 d PD . . Cl8' Cl 1.4125(11) 0.3091(7) 0.5997(8) 0.157(5) Uani 0.50 1 d P . . Zn1 Zn 0.26032(7) 0.45905(7) 0.11598(6) 0.0349(3) Uani 1 1 d . . . Zn2 Zn 1.2600(2) 0.1109(2) 0.42814(19) 0.0852(10) Uani 0.50 1 d PD . . Zn2' Zn 1.3217(4) 0.1921(3) 0.4932(3) 0.1068(13) Uani 0.50 1 d P . . O1W O 1.1467(4) 0.3697(4) 0.4800(3) 0.0422(15) Uani 1 1 d . . . O2W O 1.2797(4) 0.4163(5) 0.4120(4) 0.056(2) Uani 1 1 d . . . O3W O 1.2691(4) 0.5617(4) 0.3655(3) 0.0440(16) Uani 1 1 d . . . O4W O 1.1101(4) 0.5837(4) 0.3697(3) 0.0379(14) Uani 1 1 d . . . O5W O 1.0826(5) 0.5034(5) 0.4770(4) 0.0510(18) Uani 1 1 d . . . O6W O 0.9691(4) 0.3849(5) 0.3340(4) 0.0486(17) Uani 1 1 d . . . O7W O 0.5327(5) 0.1775(5) 0.1264(4) 0.0539(19) Uani 1 1 d . . . O8W O 0.4010(4) 0.1741(4) -0.0402(3) 0.0402(15) Uani 1 1 d . . . O9W O 0.4193(5) 0.0293(4) 0.0044(4) 0.0531(18) Uani 1 1 d . . . O10W O 0.3449(4) -0.0018(4) 0.1051(3) 0.0370(14) Uani 1 1 d . . . O11W O 0.2212(4) 0.0968(5) 0.0853(4) 0.0511(18) Uani 1 1 d . . . O12W O 0.2415(4) 0.1789(4) -0.0220(3) 0.0326(13) Uani 1 1 d . . . Pr1 Pr 1.14480(3) 0.45752(3) 0.39170(2) 0.02380(17) Uani 1 1 d . . . Pr2 Pr 0.35784(3) 0.12437(3) 0.05628(2) 0.02064(16) Uani 1 1 d . . . C1 C 1.0596(5) 0.2328(5) 0.2769(4) 0.0254(17) Uani 1 1 d . . . C2 C 0.9951(5) 0.0858(5) 0.2168(4) 0.0221(15) Uani 1 1 d . . . H2 H 1.0329 0.0522 0.2293 0.027 Uiso 1 1 calc R . . C3 C 1.0158(5) 0.1372(5) 0.1639(4) 0.0201(15) Uani 1 1 d . . . H3 H 1.0600 0.1250 0.1480 0.024 Uiso 1 1 calc R . . C4 C 0.8550(5) 0.0420(4) 0.1057(4) 0.0187(15) Uani 1 1 d . . . C5 C 1.1032(4) 0.2981(4) 0.1891(4) 0.0254(7) Uani 1 1 d D . . H5A H 1.1259 0.2781 0.1555 0.030 Uiso 1 1 calc R . . H5B H 1.1588 0.3425 0.2344 0.030 Uiso 1 1 calc R . . C6 C 0.9056(5) 0.1385(4) 0.0355(3) 0.0254(7) Uani 1 1 d D . . H6A H 0.8468 0.0945 -0.0077 0.030 Uiso 1 1 calc R . . H6B H 0.9581 0.1457 0.0236 0.030 Uiso 1 1 calc R . . C7 C 1.0338(5) 0.4042(5) 0.1872(4) 0.0237(16) Uani 1 1 d . . . C8 C 0.9783(5) 0.3040(5) 0.0726(4) 0.0217(15) Uani 1 1 d . . . H8 H 1.0128 0.3055 0.0426 0.026 Uiso 1 1 calc R . . C9 C 0.9300(5) 0.3663(5) 0.0620(4) 0.0215(15) Uani 1 1 d . . . H9 H 0.9433 0.3986 0.0280 0.026 Uiso 1 1 calc R . . C10 C 0.8144(5) 0.2249(5) 0.0208(4) 0.0230(16) Uani 1 1 d . . . C11 C 0.9651(5) 0.5061(4) 0.1529(4) 0.0254(7) Uani 1 1 d D . . H11A H 1.0172 0.5436 0.2027 0.030 Uiso 1 1 calc R . . H11B H 0.9744 0.5345 0.1162 0.030 Uiso 1 1 calc R . . C12 C 0.7533(5) 0.3349(5) -0.0087(4) 0.0197(15) Uani 1 1 d . . . H12A H 0.7714 0.3708 -0.0385 0.024 Uiso 1 1 calc R . . H12B H 0.6949 0.2828 -0.0431 0.024 Uiso 1 1 calc R . . C13 C 0.8702(5) 0.5337(5) 0.2108(5) 0.0265(17) Uani 1 1 d . . . C14 C 0.7934(5) 0.4765(5) 0.0814(4) 0.0216(15) Uani 1 1 d . . . H14 H 0.8091 0.5074 0.0474 0.026 Uiso 1 1 calc R . . C15 C 0.7293(5) 0.5037(5) 0.1064(4) 0.0214(15) Uani 1 1 d . . . H15 H 0.7172 0.5498 0.0863 0.026 Uiso 1 1 calc R . . C16 C 0.6457(5) 0.3565(5) 0.0367(4) 0.0196(15) Uani 1 1 d . . . C17 C 0.7607(5) 0.5840(5) 0.2343(4) 0.0254(7) Uani 1 1 d . . . H17A H 0.7449 0.6265 0.2115 0.030 Uiso 1 1 calc R . . H17B H 0.8173 0.6162 0.2832 0.030 Uiso 1 1 calc R . . C18 C 0.5531(5) 0.4239(5) 0.0675(4) 0.0217(15) Uani 1 1 d . . . H18A H 0.5491 0.4747 0.0527 0.026 Uiso 1 1 calc R . . H18B H 0.5003 0.3721 0.0268 0.026 Uiso 1 1 calc R . . C19 C 0.6959(5) 0.5261(5) 0.3153(4) 0.0232(16) Uani 1 1 d . . . C20 C 0.5838(5) 0.5052(5) 0.1957(4) 0.0203(15) Uani 1 1 d . . . H20 H 0.5734 0.5529 0.1774 0.024 Uiso 1 1 calc R . . C21 C 0.5330(5) 0.4789(5) 0.2444(4) 0.0214(15) Uani 1 1 d . . . H21 H 0.4998 0.5147 0.2503 0.026 Uiso 1 1 calc R . . C22 C 0.4750(5) 0.3599(5) 0.1390(4) 0.0209(15) Uani 1 1 d . . . C23 C 0.5994(5) 0.4859(4) 0.3819(3) 0.0254(7) Uani 1 1 d D . . H23A H 0.6584 0.5287 0.4256 0.030 Uiso 1 1 calc R . . H23B H 0.5481 0.5016 0.3798 0.030 Uiso 1 1 calc R . . C24 C 0.4012(4) 0.3342(5) 0.2225(4) 0.0254(7) Uani 1 1 d D . . H24A H 0.3767 0.3696 0.2433 0.030 Uiso 1 1 calc R . . H24B H 0.3472 0.2875 0.1779 0.030 Uiso 1 1 calc R . . C25 C 0.6412(5) 0.3832(5) 0.4447(4) 0.0216(16) Uani 1 1 d . . . C26 C 0.4817(5) 0.3329(5) 0.3555(4) 0.0231(16) Uani 1 1 d . . . H26 H 0.4388 0.3511 0.3688 0.028 Uiso 1 1 calc R . . C27 C 0.4954(5) 0.2591(5) 0.3863(4) 0.0243(16) Uani 1 1 d . . . H27 H 0.4545 0.2381 0.4102 0.029 Uiso 1 1 calc R . . C28 C 0.4377(5) 0.2154(5) 0.2578(4) 0.0226(16) Uani 1 1 d . . . C29 C 0.6388(5) 0.2575(5) 0.4927(4) 0.0254(16) Uani 1 1 d . . . H29A H 0.6971 0.3025 0.5356 0.030 Uiso 1 1 calc R . . H29B H 0.5949 0.2295 0.5117 0.030 Uiso 1 1 calc R . . C30 C 0.4494(5) 0.1027(4) 0.3174(4) 0.0215(15) Uani 1 1 d . . . H30A H 0.4182 0.0875 0.3487 0.026 Uiso 1 1 calc R . . H30B H 0.4045 0.0650 0.2657 0.026 Uiso 1 1 calc R . . C31 C 0.7515(6) 0.2048(5) 0.4785(4) 0.0268(17) Uani 1 1 d . . . C32 C 0.5934(5) 0.1022(4) 0.4211(4) 0.0232(16) Uani 1 1 d . . . H32 H 0.5577 0.0794 0.4483 0.028 Uiso 1 1 calc R . . C33 C 0.6553(5) 0.0569(5) 0.4181(4) 0.0230(16) Uani 1 1 d . . . H33 H 0.6525 0.0150 0.4468 0.028 Uiso 1 1 calc R . . C34 C 0.5429(6) 0.0312(5) 0.2950(4) 0.0277(17) Uani 1 1 d . . . C35 C 0.8350(6) 0.1136(6) 0.4770(4) 0.0301(18) Uani 1 1 d . . . H35A H 0.8266 0.0663 0.4991 0.036 Uiso 1 1 calc R . . H35B H 0.8883 0.1662 0.5165 0.036 Uiso 1 1 calc R . . C36 C 0.6376(6) -0.0523(5) 0.3095(5) 0.0289(17) Uani 1 1 d . . . H36A H 0.5850 -0.0882 0.2595 0.035 Uiso 1 1 calc R . . H36B H 0.6416 -0.0897 0.3417 0.035 Uiso 1 1 calc R . . C37 C 0.9347(6) 0.1481(5) 0.4137(4) 0.0274(17) Uani 1 1 d . . . C38 C 0.8190(6) 0.0071(5) 0.3681(4) 0.0270(17) Uani 1 1 d . . . H38 H 0.8176 -0.0360 0.3957 0.032 Uiso 1 1 calc R . . C39 C 0.8831(5) 0.0120(5) 0.3306(4) 0.0212(15) Uani 1 1 d . . . H39 H 0.9172 -0.0246 0.3435 0.025 Uiso 1 1 calc R . . C40 C 0.7298(6) -0.0348(5) 0.2380(4) 0.0283(17) Uani 1 1 d . . . C41 C 1.0350(5) 0.1371(5) 0.3538(4) 0.0251(16) Uani 1 1 d . . . H41A H 1.0611 0.0943 0.3590 0.030 Uiso 1 1 calc R . . H41B H 1.0820 0.1913 0.3944 0.030 Uiso 1 1 calc R . . C42 C 0.8447(6) -0.0412(5) 0.1933(4) 0.0247(16) Uani 1 1 d . . . H42A H 0.8860 -0.0698 0.2121 0.030 Uiso 1 1 calc R . . H42B H 0.7872 -0.0837 0.1483 0.030 Uiso 1 1 calc R . . N1 N 1.0193(4) 0.1521(4) 0.2822(3) 0.0217(13) Uani 1 1 d . . . N2 N 1.0563(4) 0.2257(3) 0.2100(3) 0.0226(7) Uani 1 1 d D . . N3 N 0.8925(4) 0.0290(4) 0.1728(3) 0.0231(13) Uani 1 1 d . . . N4 N 0.9215(4) 0.1087(4) 0.1007(3) 0.0227(13) Uani 1 1 d D . . N5 N 1.0419(4) 0.3370(4) 0.1523(3) 0.0207(13) Uani 1 1 d D . . N6 N 0.9701(4) 0.4244(3) 0.1370(3) 0.0250(14) Uani 1 1 d D . . N7 N 0.8984(4) 0.2200(3) 0.0478(3) 0.0228(13) Uani 1 1 d D . . N8 N 0.8301(4) 0.3091(4) 0.0300(4) 0.0236(13) Uani 1 1 d . . . N9 N 0.8773(4) 0.4976(4) 0.1509(4) 0.0255(14) Uani 1 1 d . . . N10 N 0.7831(4) 0.5347(4) 0.1878(3) 0.0226(13) Uani 1 1 d . . . N11 N 0.7353(4) 0.3825(4) 0.0432(3) 0.0208(13) Uani 1 1 d . . . N12 N 0.6415(4) 0.4232(4) 0.0754(3) 0.0241(14) Uani 1 1 d . . . N13 N 0.6819(4) 0.5321(4) 0.2465(3) 0.0225(13) Uani 1 1 d . . . N14 N 0.6094(4) 0.4907(4) 0.3146(3) 0.0226(7) Uani 1 1 d D . . N15 N 0.5413(4) 0.4261(4) 0.1339(3) 0.0225(13) Uani 1 1 d . . . N16 N 0.4667(4) 0.3878(4) 0.1999(4) 0.0251(14) Uani 1 1 d D . . N17 N 0.5790(4) 0.4017(3) 0.3922(3) 0.0226(7) Uani 1 1 d D . . N18 N 0.5957(4) 0.2988(4) 0.4400(4) 0.0224(13) Uani 1 1 d . . . N19 N 0.4428(4) 0.2959(4) 0.2776(3) 0.0226(7) Uani 1 1 d D . . N20 N 0.4700(4) 0.1926(4) 0.3199(3) 0.0206(13) Uani 1 1 d . . . N21 N 0.6616(4) 0.1935(4) 0.4598(4) 0.0247(14) Uani 1 1 d . . . N22 N 0.7486(4) 0.1274(4) 0.4514(4) 0.0279(14) Uani 1 1 d . . . N23 N 0.5300(5) 0.0851(4) 0.3420(3) 0.0264(14) Uani 1 1 d . . . N24 N 0.6174(5) 0.0138(4) 0.3389(4) 0.0284(14) Uani 1 1 d . . . N25 N 0.8593(5) 0.0923(4) 0.4167(4) 0.0290(15) Uani 1 1 d . . . N26 N 0.9489(4) 0.1063(4) 0.3613(3) 0.0249(14) Uani 1 1 d . . . N27 N 0.7265(4) -0.0184(4) 0.3042(4) 0.0281(15) Uani 1 1 d . . . N28 N 0.8180(4) -0.0160(4) 0.2499(3) 0.0270(14) Uani 1 1 d . . . O1 O 1.0910(4) 0.3018(3) 0.3270(3) 0.0270(12) Uani 1 1 d . . . O2 O 1.0827(4) 0.4447(4) 0.2565(3) 0.0308(13) Uani 1 1 d . . . O3 O 0.9332(4) 0.5642(4) 0.2759(3) 0.0391(14) Uani 1 1 d . . . O4 O 0.7741(4) 0.5470(4) 0.3700(3) 0.0316(13) Uani 1 1 d . . . O5 O 0.7248(4) 0.4328(3) 0.4873(3) 0.0288(12) Uani 1 1 d . . . O6 O 0.8226(4) 0.2736(4) 0.5130(4) 0.0439(16) Uani 1 1 d . . . O8 O 0.7710(4) -0.0013(3) 0.0554(3) 0.0265(12) Uani 1 1 d . . . O9 O 0.7345(4) 0.1627(3) -0.0085(3) 0.0332(13) Uani 1 1 d . . . O10 O 0.5807(4) 0.2842(4) -0.0010(3) 0.0329(13) Uani 1 1 d . . . O11 O 0.4279(4) 0.2863(3) 0.0939(3) 0.0304(12) Uani 1 1 d . . . O12 O 0.4084(4) 0.1689(3) 0.1935(3) 0.0271(12) Uani 1 1 d . . . O13 O 0.4975(5) 0.0021(4) 0.2278(3) 0.0429(16) Uani 1 1 d . . . O14 O 0.6582(4) -0.0626(4) 0.1759(3) 0.0388(14) Uani 1 1 d . . . O7 O 0.9852(5) 0.2240(4) 0.4515(4) 0.0439(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl9 0.046(2) 0.099(4) 0.126(4) -0.062(3) -0.010(2) 0.048(3) Cl10 0.062(3) 0.062(3) 0.054(3) 0.038(3) 0.016(3) 0.042(3) Cl11 0.049(3) 0.131(6) 0.076(4) -0.058(4) 0.048(3) -0.027(4) Cl12 0.099(5) 0.125(7) 0.144(7) -0.023(5) 0.037(5) 0.057(5) Cl1 0.0530(14) 0.0476(14) 0.0442(13) 0.0130(11) 0.0267(11) 0.0323(11) Cl2 0.0357(12) 0.0554(15) 0.0790(18) 0.0440(14) 0.0328(12) 0.0299(11) Cl3 0.0584(14) 0.0511(14) 0.0384(12) 0.0135(11) 0.0294(11) 0.0336(12) Cl4 0.0319(11) 0.089(2) 0.0485(14) 0.0377(14) 0.0241(11) 0.0276(12) Cl5 0.094(3) 0.174(5) 0.205(6) 0.134(5) 0.094(4) 0.081(3) Cl6 0.132(4) 0.189(6) 0.186(5) 0.138(5) 0.111(4) 0.099(4) Cl7 0.267(10) 0.392(14) 0.194(8) 0.214(9) 0.156(8) 0.222(10) Cl8 0.321(19) 0.162(11) 0.140(9) 0.100(9) 0.135(12) 0.191(13) Cl8' 0.194(13) 0.089(7) 0.139(10) 0.011(7) 0.068(9) 0.029(7) Zn1 0.0355(5) 0.0457(6) 0.0394(6) 0.0232(5) 0.0221(5) 0.0257(5) Zn2 0.079(2) 0.096(3) 0.083(2) 0.038(2) 0.0375(19) 0.038(2) Zn2' 0.123(3) 0.106(3) 0.108(3) 0.042(3) 0.062(3) 0.055(3) O1W 0.039(3) 0.041(4) 0.027(3) 0.002(3) 0.007(3) 0.009(3) O2W 0.018(3) 0.047(4) 0.081(5) -0.010(4) 0.012(3) 0.012(3) O3W 0.032(3) 0.051(4) 0.029(3) -0.005(3) 0.013(3) 0.004(3) O4W 0.028(3) 0.042(4) 0.027(3) -0.003(3) -0.002(2) 0.019(3) O5W 0.047(4) 0.064(5) 0.038(4) -0.006(3) 0.022(3) 0.026(4) O6W 0.019(3) 0.053(4) 0.048(4) -0.005(3) 0.005(3) 0.008(3) O7W 0.033(4) 0.066(5) 0.043(4) -0.002(4) 0.006(3) 0.021(3) O8W 0.027(3) 0.035(3) 0.032(3) -0.006(3) 0.010(3) -0.004(3) O9W 0.052(4) 0.039(4) 0.067(5) -0.001(3) 0.032(4) 0.021(3) O10W 0.052(4) 0.027(3) 0.027(3) 0.008(3) 0.008(3) 0.024(3) O11W 0.031(3) 0.082(5) 0.031(3) 0.014(3) 0.012(3) 0.020(3) O12W 0.034(3) 0.039(3) 0.026(3) 0.009(3) 0.009(3) 0.023(3) Pr1 0.0161(3) 0.0244(3) 0.0186(3) -0.00486(19) 0.00310(19) 0.00546(19) Pr2 0.0166(2) 0.0189(3) 0.0168(3) -0.00153(18) 0.00242(18) 0.00613(18) C1 0.017(4) 0.028(4) 0.019(4) 0.000(3) 0.003(3) 0.007(3) C2 0.030(4) 0.014(4) 0.019(4) 0.002(3) 0.007(3) 0.013(3) C3 0.016(3) 0.022(4) 0.017(4) 0.003(3) 0.004(3) 0.008(3) C4 0.019(4) 0.011(4) 0.016(4) -0.006(3) 0.001(3) 0.007(3) C5 0.0140(14) 0.0285(17) 0.0235(16) 0.0019(14) 0.0042(12) 0.0057(12) C6 0.0140(14) 0.0285(17) 0.0235(16) 0.0019(14) 0.0042(12) 0.0057(12) C7 0.019(4) 0.020(4) 0.028(4) 0.006(3) 0.010(3) 0.006(3) C8 0.022(4) 0.015(4) 0.021(4) -0.001(3) 0.010(3) 0.003(3) C9 0.023(4) 0.013(4) 0.014(3) 0.001(3) 0.002(3) 0.002(3) C10 0.023(4) 0.014(4) 0.019(4) -0.006(3) 0.004(3) 0.005(3) C11 0.0140(14) 0.0285(17) 0.0235(16) 0.0019(14) 0.0042(12) 0.0057(12) C12 0.023(4) 0.022(4) 0.018(4) 0.005(3) 0.009(3) 0.015(3) C13 0.019(4) 0.017(4) 0.033(5) -0.001(3) 0.011(4) 0.001(3) C14 0.016(3) 0.016(4) 0.027(4) 0.004(3) 0.007(3) 0.005(3) C15 0.022(4) 0.019(4) 0.028(4) 0.009(3) 0.012(3) 0.012(3) C16 0.015(3) 0.023(4) 0.016(3) 0.002(3) 0.001(3) 0.011(3) C17 0.0140(14) 0.0285(17) 0.0235(16) 0.0019(14) 0.0042(12) 0.0057(12) C18 0.019(4) 0.023(4) 0.021(4) 0.005(3) 0.007(3) 0.011(3) C19 0.029(4) 0.014(4) 0.025(4) 0.002(3) 0.012(3) 0.010(3) C20 0.019(3) 0.015(4) 0.021(4) 0.003(3) 0.005(3) 0.007(3) C21 0.019(4) 0.017(4) 0.021(4) 0.000(3) 0.003(3) 0.011(3) C22 0.020(4) 0.022(4) 0.015(4) 0.003(3) 0.004(3) 0.007(3) C23 0.0140(14) 0.0285(17) 0.0235(16) 0.0019(14) 0.0042(12) 0.0057(12) C24 0.0140(14) 0.0285(17) 0.0235(16) 0.0019(14) 0.0042(12) 0.0057(12) C25 0.021(4) 0.021(4) 0.014(4) -0.002(3) 0.005(3) 0.008(3) C26 0.017(4) 0.019(4) 0.027(4) -0.003(3) 0.009(3) 0.005(3) C27 0.025(4) 0.023(4) 0.024(4) 0.002(3) 0.012(3) 0.013(3) C28 0.019(4) 0.015(4) 0.029(4) 0.006(3) 0.008(3) 0.007(3) C29 0.025(4) 0.028(4) 0.017(4) -0.002(3) 0.000(3) 0.019(3) C30 0.018(3) 0.010(3) 0.017(4) -0.004(3) -0.004(3) 0.001(3) C31 0.031(4) 0.028(4) 0.019(4) 0.003(3) 0.009(3) 0.013(4) C32 0.034(4) 0.012(4) 0.019(4) 0.003(3) 0.011(3) 0.006(3) C33 0.024(4) 0.022(4) 0.017(4) 0.005(3) 0.006(3) 0.009(3) C34 0.032(4) 0.015(4) 0.024(4) 0.000(3) 0.005(3) 0.008(3) C35 0.033(4) 0.036(5) 0.023(4) 0.005(4) 0.012(3) 0.019(4) C36 0.029(4) 0.022(4) 0.033(4) 0.001(3) 0.014(4) 0.011(3) C37 0.030(4) 0.028(5) 0.014(4) 0.003(3) 0.004(3) 0.010(4) C38 0.035(4) 0.029(4) 0.021(4) 0.012(3) 0.012(3) 0.016(4) C39 0.023(4) 0.022(4) 0.017(4) 0.007(3) 0.007(3) 0.010(3) C40 0.031(4) 0.023(4) 0.021(4) 0.004(3) 0.006(3) 0.009(3) C41 0.022(4) 0.025(4) 0.016(4) 0.001(3) 0.002(3) 0.008(3) C42 0.031(4) 0.021(4) 0.021(4) 0.003(3) 0.012(3) 0.011(3) N1 0.026(3) 0.020(3) 0.012(3) 0.005(3) 0.005(3) 0.007(3) N2 0.0214(16) 0.0201(17) 0.0123(15) -0.0028(13) 0.0025(13) 0.0030(13) N3 0.022(3) 0.019(3) 0.018(3) 0.003(3) 0.006(3) 0.004(3) N4 0.022(3) 0.016(3) 0.020(3) 0.001(3) 0.002(3) 0.007(3) N5 0.023(3) 0.024(3) 0.014(3) 0.006(3) 0.004(3) 0.014(3) N6 0.029(3) 0.018(3) 0.022(3) 0.000(3) 0.008(3) 0.010(3) N7 0.022(3) 0.017(3) 0.023(3) 0.003(3) 0.004(3) 0.009(3) N8 0.021(3) 0.016(3) 0.027(3) 0.002(3) 0.006(3) 0.008(3) N9 0.018(3) 0.027(4) 0.024(3) 0.002(3) 0.005(3) 0.009(3) N10 0.024(3) 0.024(3) 0.015(3) 0.002(3) 0.005(3) 0.010(3) N11 0.025(3) 0.012(3) 0.021(3) -0.001(3) 0.008(3) 0.008(3) N12 0.019(3) 0.027(4) 0.024(3) 0.005(3) 0.007(3) 0.011(3) N13 0.017(3) 0.026(3) 0.020(3) 0.007(3) 0.006(3) 0.009(3) N14 0.0214(16) 0.0201(17) 0.0123(15) -0.0028(13) 0.0025(13) 0.0030(13) N15 0.020(3) 0.028(4) 0.019(3) 0.003(3) 0.008(3) 0.013(3) N16 0.030(3) 0.012(3) 0.026(3) 0.004(3) 0.011(3) 0.003(3) N17 0.0214(16) 0.0201(17) 0.0123(15) -0.0028(13) 0.0025(13) 0.0030(13) N18 0.022(3) 0.009(3) 0.026(3) 0.000(3) 0.002(3) 0.008(2) N19 0.0214(16) 0.0201(17) 0.0123(15) -0.0028(13) 0.0025(13) 0.0030(13) N20 0.018(3) 0.012(3) 0.017(3) 0.002(2) -0.003(2) 0.004(2) N21 0.021(3) 0.018(3) 0.022(3) -0.003(3) 0.003(3) 0.007(3) N22 0.020(3) 0.023(4) 0.028(4) -0.005(3) 0.003(3) 0.009(3) N23 0.030(3) 0.016(3) 0.019(3) 0.000(3) 0.001(3) 0.009(3) N24 0.030(3) 0.031(4) 0.021(3) 0.006(3) 0.007(3) 0.015(3) N25 0.039(4) 0.027(4) 0.017(3) 0.000(3) 0.013(3) 0.013(3) N26 0.025(3) 0.012(3) 0.020(3) -0.004(3) 0.002(3) 0.002(3) N27 0.022(3) 0.028(4) 0.023(3) -0.003(3) 0.005(3) 0.007(3) N28 0.027(4) 0.030(4) 0.013(3) -0.003(3) 0.005(3) 0.009(3) O1 0.032(3) 0.021(3) 0.017(3) -0.003(2) 0.004(2) 0.011(2) O2 0.027(3) 0.030(3) 0.015(3) -0.005(2) 0.001(2) 0.005(2) O3 0.025(3) 0.050(4) 0.035(3) 0.004(3) 0.003(3) 0.023(3) O4 0.018(3) 0.042(3) 0.018(3) 0.002(3) -0.001(2) 0.007(2) O5 0.018(3) 0.024(3) 0.023(3) -0.004(2) -0.001(2) 0.003(2) O6 0.031(3) 0.031(4) 0.049(4) -0.010(3) 0.010(3) 0.009(3) O8 0.025(3) 0.019(3) 0.024(3) 0.003(2) 0.003(2) 0.007(2) O9 0.017(3) 0.020(3) 0.045(4) -0.004(3) 0.006(3) 0.005(2) O10 0.028(3) 0.023(3) 0.038(3) 0.000(3) 0.015(3) 0.006(2) O11 0.035(3) 0.019(3) 0.022(3) -0.003(2) 0.008(2) 0.005(2) O12 0.032(3) 0.021(3) 0.013(3) -0.004(2) 0.001(2) 0.010(2) O13 0.054(4) 0.046(4) 0.018(3) -0.002(3) 0.003(3) 0.030(3) O14 0.036(3) 0.043(4) 0.019(3) -0.002(3) 0.004(3) 0.014(3) O7 0.051(4) 0.029(4) 0.037(4) -0.003(3) 0.018(3) 0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl11 Cl11 1.78(2) 2_666 ? Cl1 Zn1 2.273(3) . ? Cl2 Zn1 2.260(2) . ? Cl3 Zn1 2.262(2) . ? Cl4 Zn1 2.264(2) . ? Cl5 Zn2 2.274(2) . ? Cl5 Zn2' 2.358(7) . ? Cl6 Zn2 2.273(2) . ? Cl6 Zn2' 2.312(7) . ? Cl7 Zn2' 2.097(9) . ? Cl7 Zn2 2.263(2) . ? Cl8 Zn2 2.271(2) . ? Cl8' Zn2' 2.285(13) . ? Zn2 Zn2' 1.491(6) . ? O1W Pr1 2.503(6) . ? O2W Pr1 2.518(6) . ? O3W Pr1 2.544(6) . ? O4W Pr1 2.497(6) . ? O5W Pr1 2.514(6) . ? O6W Pr1 2.476(6) . ? O7W Pr2 2.479(6) . ? O8W Pr2 2.499(6) . ? O9W Pr2 2.531(6) . ? O10W Pr2 2.494(6) . ? O11W Pr2 2.505(6) . ? O12W Pr2 2.560(5) . ? Pr1 O2 2.480(5) . ? Pr1 O5 2.483(5) 2_766 ? Pr1 O1 2.490(5) . ? Pr2 O8 2.468(5) 2_655 ? Pr2 O12 2.492(5) . ? Pr2 O11 2.498(5) . ? C1 O1 1.245(9) . ? C1 N2 1.324(9) . ? C1 N1 1.365(10) . ? C2 N1 1.442(9) . ? C2 N3 1.472(10) . ? C2 C3 1.551(10) . ? C2 H2 0.9900 . ? C3 N2 1.439(9) . ? C3 N4 1.465(9) . ? C3 H3 0.9900 . ? C4 O8 1.250(8) . ? C4 N3 1.352(9) . ? C4 N4 1.354(9) . ? C5 N2 1.449(2) . ? C5 N5 1.450(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.449(2) . ? C6 N7 1.449(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.259(9) . ? C7 N5 1.351(9) . ? C7 N6 1.353(10) . ? C8 N5 1.443(9) . ? C8 N7 1.454(9) . ? C8 C9 1.549(11) . ? C8 H8 0.9900 . ? C9 N8 1.444(9) . ? C9 N6 1.448(9) . ? C9 H9 0.9900 . ? C10 O9 1.242(9) . ? C10 N7 1.348(9) . ? C10 N8 1.356(10) . ? C11 N9 1.425(9) . ? C11 N6 1.440(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.433(9) . ? C12 N8 1.486(9) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.223(10) . ? C13 N9 1.355(10) . ? C13 N10 1.369(10) . ? C14 N9 1.449(9) . ? C14 N11 1.474(9) . ? C14 C15 1.534(10) . ? C14 H14 0.9900 . ? C15 N10 1.452(9) . ? C15 N12 1.468(9) . ? C15 H15 0.9900 . ? C16 O10 1.224(9) . ? C16 N12 1.340(9) . ? C16 N11 1.369(9) . ? C17 N10 1.425(10) . ? C17 N13 1.462(9) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N15 1.434(9) . ? C18 N12 1.445(9) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.241(9) . ? C19 N13 1.350(9) . ? C19 N14 1.371(9) . ? C20 N13 1.432(9) . ? C20 N15 1.454(10) . ? C20 C21 1.562(10) . ? C20 H20 0.9900 . ? C21 N14 1.436(9) . ? C21 N16 1.471(9) . ? C21 H21 0.9900 . ? C22 O11 1.229(9) . ? C22 N16 1.340(9) . ? C22 N15 1.348(9) . ? C23 N17 1.440(2) . ? C23 N14 1.450(2) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N19 1.449(2) . ? C24 N16 1.450(2) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O5 1.226(9) . ? C25 N17 1.343(9) . ? C25 N18 1.364(10) . ? C26 N19 1.406(9) . ? C26 N17 1.464(9) . ? C26 C27 1.544(11) . ? C26 H26 0.9900 . ? C27 N18 1.451(10) . ? C27 N20 1.452(10) . ? C27 H27 0.9900 . ? C28 O12 1.239(9) . ? C28 N20 1.340(10) . ? C28 N19 1.355(10) . ? C29 N21 1.449(9) . ? C29 N18 1.467(9) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N23 1.412(10) . ? C30 N20 1.459(9) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O6 1.221(10) . ? C31 N22 1.349(10) . ? C31 N21 1.350(10) . ? C32 N23 1.464(10) . ? C32 N21 1.465(9) . ? C32 C33 1.517(11) . ? C32 H32 0.9900 . ? C33 N22 1.436(9) . ? C33 N24 1.449(10) . ? C33 H33 0.9900 . ? C34 O13 1.202(10) . ? C34 N23 1.370(10) . ? C34 N24 1.393(10) . ? C35 N22 1.466(10) . ? C35 N25 1.471(10) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N24 1.417(10) . ? C36 N27 1.467(10) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 O7 1.218(10) . ? C37 N25 1.340(10) . ? C37 N26 1.346(10) . ? C38 N25 1.413(10) . ? C38 N27 1.460(10) . ? C38 C39 1.533(10) . ? C38 H38 0.9900 . ? C39 N28 1.469(9) . ? C39 N26 1.489(9) . ? C39 H39 0.9900 . ? C40 O14 1.244(9) . ? C40 N28 1.325(10) . ? C40 N27 1.361(10) . ? C41 N26 1.444(10) . ? C41 N1 1.451(9) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 N3 1.423(9) . ? C42 N28 1.451(9) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? O5 Pr1 2.483(5) 2_766 ? O8 Pr2 2.468(5) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Zn2 Cl5 Zn2' 37.50(16) . . ? Zn2 Cl6 Zn2' 37.94(16) . . ? Zn2' Cl7 Zn2 39.76(18) . . ? Cl2 Zn1 Cl3 107.60(10) . . ? Cl2 Zn1 Cl4 113.48(9) . . ? Cl3 Zn1 Cl4 108.70(10) . . ? Cl2 Zn1 Cl1 106.23(10) . . ? Cl3 Zn1 Cl1 112.01(9) . . ? Cl4 Zn1 Cl1 108.86(11) . . ? Zn2' Zn2 Cl7 64.1(4) . . ? Zn2' Zn2 Cl8 159.5(4) . . ? Cl7 Zn2 Cl8 95.4(5) . . ? Zn2' Zn2 Cl6 72.4(3) . . ? Cl7 Zn2 Cl6 107.8(3) . . ? Cl8 Zn2 Cl6 116.7(4) . . ? Zn2' Zn2 Cl5 74.3(3) . . ? Cl7 Zn2 Cl5 110.0(3) . . ? Cl8 Zn2 Cl5 115.8(3) . . ? Cl6 Zn2 Cl5 109.8(2) . . ? Zn2 Zn2' Cl7 76.1(3) . . ? Zn2 Zn2' Cl8' 174.7(4) . . ? Cl7 Zn2' Cl8' 99.5(5) . . ? Zn2 Zn2' Cl6 69.6(2) . . ? Cl7 Zn2' Cl6 112.4(3) . . ? Cl8' Zn2' Cl6 109.9(5) . . ? Zn2 Zn2' Cl5 68.2(2) . . ? Cl7 Zn2' Cl5 113.0(3) . . ? Cl8' Zn2' Cl5 116.7(4) . . ? Cl6 Zn2' Cl5 105.6(3) . . ? O6W Pr1 O2 72.8(2) . . ? O6W Pr1 O5 135.6(2) . 2_766 ? O2 Pr1 O5 137.19(18) . 2_766 ? O6W Pr1 O1 71.9(2) . . ? O2 Pr1 O1 75.31(18) . . ? O5 Pr1 O1 136.27(18) 2_766 . ? O6W Pr1 O4W 80.7(2) . . ? O2 Pr1 O4W 69.98(19) . . ? O5 Pr1 O4W 82.80(18) 2_766 . ? O1 Pr1 O4W 140.78(17) . . ? O6W Pr1 O1W 87.2(2) . . ? O2 Pr1 O1W 142.66(19) . . ? O5 Pr1 O1W 78.61(19) 2_766 . ? O1 Pr1 O1W 68.52(19) . . ? O4W Pr1 O1W 138.5(2) . . ? O6W Pr1 O5W 67.4(2) . . ? O2 Pr1 O5W 126.2(2) . . ? O5 Pr1 O5W 68.2(2) 2_766 . ? O1 Pr1 O5W 121.8(2) . . ? O4W Pr1 O5W 69.1(2) . . ? O1W Pr1 O5W 69.6(2) . . ? O6W Pr1 O2W 138.2(2) . . ? O2 Pr1 O2W 100.5(2) . . ? O5 Pr1 O2W 77.3(2) 2_766 . ? O1 Pr1 O2W 66.58(19) . . ? O4W Pr1 O2W 137.0(2) . . ? O1W Pr1 O2W 73.7(2) . . ? O5W Pr1 O2W 133.3(3) . . ? O6W Pr1 O3W 136.9(2) . . ? O2 Pr1 O3W 68.22(18) . . ? O5 Pr1 O3W 71.57(18) 2_766 . ? O1 Pr1 O3W 113.68(19) . . ? O4W Pr1 O3W 69.4(2) . . ? O1W Pr1 O3W 135.6(2) . . ? O5W Pr1 O3W 124.5(2) . . ? O2W Pr1 O3W 68.2(2) . . ? O8 Pr2 O7W 134.7(2) 2_655 . ? O8 Pr2 O12 136.65(17) 2_655 . ? O7W Pr2 O12 71.0(2) . . ? O8 Pr2 O10W 77.66(18) 2_655 . ? O7W Pr2 O10W 86.9(2) . . ? O12 Pr2 O10W 68.79(18) . . ? O8 Pr2 O11 137.17(17) 2_655 . ? O7W Pr2 O11 73.3(2) . . ? O12 Pr2 O11 76.34(17) . . ? O10W Pr2 O11 143.98(18) . . ? O8 Pr2 O8W 81.72(17) 2_655 . ? O7W Pr2 O8W 81.1(2) . . ? O12 Pr2 O8W 141.62(17) . . ? O10W Pr2 O8W 136.5(2) . . ? O11 Pr2 O8W 70.63(19) . . ? O8 Pr2 O11W 79.0(2) 2_655 . ? O7W Pr2 O11W 137.8(2) . . ? O12 Pr2 O11W 66.86(19) . . ? O10W Pr2 O11W 75.7(2) . . ? O11 Pr2 O11W 99.1(2) . . ? O8W Pr2 O11W 136.7(2) . . ? O8 Pr2 O9W 68.0(2) 2_655 . ? O7W Pr2 O9W 66.7(2) . . ? O12 Pr2 O9W 119.6(2) . . ? O10W Pr2 O9W 67.9(2) . . ? O11 Pr2 O9W 126.1(2) . . ? O8W Pr2 O9W 68.9(2) . . ? O11W Pr2 O9W 134.8(2) . . ? O8 Pr2 O12W 72.09(18) 2_655 . ? O7W Pr2 O12W 137.0(2) . . ? O12 Pr2 O12W 115.17(18) . . ? O10W Pr2 O12W 135.9(2) . . ? O11 Pr2 O12W 67.91(19) . . ? O8W Pr2 O12W 69.5(2) . . ? O11W Pr2 O12W 67.8(2) . . ? O9W Pr2 O12W 125.2(2) . . ? O1 C1 N2 126.0(7) . . ? O1 C1 N1 124.2(7) . . ? N2 C1 N1 109.7(6) . . ? N1 C2 N3 113.7(6) . . ? N1 C2 C3 103.7(6) . . ? N3 C2 C3 102.8(6) . . ? N1 C2 H2 112.0 . . ? N3 C2 H2 112.0 . . ? C3 C2 H2 112.0 . . ? N2 C3 N4 113.7(6) . . ? N2 C3 C2 102.1(5) . . ? N4 C3 C2 103.4(5) . . ? N2 C3 H3 112.3 . . ? N4 C3 H3 112.3 . . ? C2 C3 H3 112.3 . . ? O8 C4 N3 124.9(6) . . ? O8 C4 N4 124.8(6) . . ? N3 C4 N4 110.3(6) . . ? N2 C5 N5 113.1(5) . . ? N2 C5 H5A 109.0 . . ? N5 C5 H5A 109.0 . . ? N2 C5 H5B 109.0 . . ? N5 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N4 C6 N7 111.9(5) . . ? N4 C6 H6A 109.2 . . ? N7 C6 H6A 109.2 . . ? N4 C6 H6B 109.2 . . ? N7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? O2 C7 N5 124.0(7) . . ? O2 C7 N6 125.3(7) . . ? N5 C7 N6 110.6(6) . . ? N5 C8 N7 114.9(6) . . ? N5 C8 C9 102.4(5) . . ? N7 C8 C9 102.7(5) . . ? N5 C8 H8 112.0 . . ? N7 C8 H8 112.0 . . ? C9 C8 H8 112.0 . . ? N8 C9 N6 114.2(6) . . ? N8 C9 C8 103.6(6) . . ? N6 C9 C8 104.5(6) . . ? N8 C9 H9 111.3 . . ? N6 C9 H9 111.3 . . ? C8 C9 H9 111.3 . . ? O9 C10 N7 126.0(7) . . ? O9 C10 N8 124.5(7) . . ? N7 C10 N8 109.5(6) . . ? N9 C11 N6 113.3(6) . . ? N9 C11 H11A 108.9 . . ? N6 C11 H11A 108.9 . . ? N9 C11 H11B 108.9 . . ? N6 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? N11 C12 N8 112.1(6) . . ? N11 C12 H12A 109.2 . . ? N8 C12 H12A 109.2 . . ? N11 C12 H12B 109.2 . . ? N8 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? O3 C13 N9 125.5(7) . . ? O3 C13 N10 124.4(7) . . ? N9 C13 N10 110.1(7) . . ? N9 C14 N11 113.5(6) . . ? N9 C14 C15 104.3(6) . . ? N11 C14 C15 102.8(5) . . ? N9 C14 H14 111.9 . . ? N11 C14 H14 111.9 . . ? C15 C14 H14 111.9 . . ? N10 C15 N12 115.0(6) . . ? N10 C15 C14 103.6(6) . . ? N12 C15 C14 103.5(6) . . ? N10 C15 H15 111.4 . . ? N12 C15 H15 111.4 . . ? C14 C15 H15 111.4 . . ? O10 C16 N12 127.0(6) . . ? O10 C16 N11 124.0(7) . . ? N12 C16 N11 108.9(6) . . ? N10 C17 N13 114.3(6) . . ? N10 C17 H17A 108.7 . . ? N13 C17 H17A 108.7 . . ? N10 C17 H17B 108.7 . . ? N13 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? N15 C18 N12 114.6(6) . . ? N15 C18 H18A 108.6 . . ? N12 C18 H18A 108.6 . . ? N15 C18 H18B 108.6 . . ? N12 C18 H18B 108.6 . . ? H18A C18 H18B 107.6 . . ? O4 C19 N13 125.7(7) . . ? O4 C19 N14 125.4(7) . . ? N13 C19 N14 108.9(6) . . ? N13 C20 N15 114.8(6) . . ? N13 C20 C21 103.0(6) . . ? N15 C20 C21 104.0(5) . . ? N13 C20 H20 111.5 . . ? N15 C20 H20 111.5 . . ? C21 C20 H20 111.5 . . ? N14 C21 N16 114.7(6) . . ? N14 C21 C20 103.2(5) . . ? N16 C21 C20 100.9(5) . . ? N14 C21 H21 112.4 . . ? N16 C21 H21 112.4 . . ? C20 C21 H21 112.4 . . ? O11 C22 N16 125.4(6) . . ? O11 C22 N15 125.4(7) . . ? N16 C22 N15 109.2(6) . . ? N17 C23 N14 113.9(5) . . ? N17 C23 H23A 108.8 . . ? N14 C23 H23A 108.8 . . ? N17 C23 H23B 108.8 . . ? N14 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? N19 C24 N16 114.1(5) . . ? N19 C24 H24A 108.7 . . ? N16 C24 H24A 108.7 . . ? N19 C24 H24B 108.7 . . ? N16 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? O5 C25 N17 125.8(7) . . ? O5 C25 N18 126.3(7) . . ? N17 C25 N18 107.8(6) . . ? N19 C26 N17 115.2(6) . . ? N19 C26 C27 103.0(6) . . ? N17 C26 C27 102.1(6) . . ? N19 C26 H26 111.9 . . ? N17 C26 H26 111.9 . . ? C27 C26 H26 111.9 . . ? N18 C27 N20 114.0(6) . . ? N18 C27 C26 103.3(6) . . ? N20 C27 C26 103.1(6) . . ? N18 C27 H27 111.9 . . ? N20 C27 H27 111.9 . . ? C26 C27 H27 111.9 . . ? O12 C28 N20 124.2(7) . . ? O12 C28 N19 126.8(7) . . ? N20 C28 N19 109.0(6) . . ? N21 C29 N18 113.6(6) . . ? N21 C29 H29A 108.9 . . ? N18 C29 H29A 108.9 . . ? N21 C29 H29B 108.9 . . ? N18 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? N23 C30 N20 114.6(6) . . ? N23 C30 H30A 108.6 . . ? N20 C30 H30A 108.6 . . ? N23 C30 H30B 108.6 . . ? N20 C30 H30B 108.6 . . ? H30A C30 H30B 107.6 . . ? O6 C31 N22 126.2(7) . . ? O6 C31 N21 125.6(7) . . ? N22 C31 N21 108.2(7) . . ? N23 C32 N21 113.2(6) . . ? N23 C32 C33 103.8(6) . . ? N21 C32 C33 103.5(6) . . ? N23 C32 H32 111.9 . . ? N21 C32 H32 111.9 . . ? C33 C32 H32 111.9 . . ? N22 C33 N24 114.1(6) . . ? N22 C33 C32 103.1(6) . . ? N24 C33 C32 104.6(6) . . ? N22 C33 H33 111.5 . . ? N24 C33 H33 111.5 . . ? C32 C33 H33 111.5 . . ? O13 C34 N23 126.8(8) . . ? O13 C34 N24 125.2(8) . . ? N23 C34 N24 108.0(6) . . ? N22 C35 N25 113.4(6) . . ? N22 C35 H35A 108.9 . . ? N25 C35 H35A 108.9 . . ? N22 C35 H35B 108.9 . . ? N25 C35 H35B 108.9 . . ? H35A C35 H35B 107.7 . . ? N24 C36 N27 113.1(6) . . ? N24 C36 H36A 109.0 . . ? N27 C36 H36A 109.0 . . ? N24 C36 H36B 109.0 . . ? N27 C36 H36B 109.0 . . ? H36A C36 H36B 107.8 . . ? O7 C37 N25 127.8(8) . . ? O7 C37 N26 123.6(7) . . ? N25 C37 N26 108.7(7) . . ? N25 C38 N27 114.1(7) . . ? N25 C38 C39 104.0(6) . . ? N27 C38 C39 102.4(6) . . ? N25 C38 H38 111.9 . . ? N27 C38 H38 111.9 . . ? C39 C38 H38 111.9 . . ? N28 C39 N26 113.1(6) . . ? N28 C39 C38 104.3(6) . . ? N26 C39 C38 101.7(6) . . ? N28 C39 H39 112.3 . . ? N26 C39 H39 112.3 . . ? C38 C39 H39 112.3 . . ? O14 C40 N28 126.3(7) . . ? O14 C40 N27 122.9(7) . . ? N28 C40 N27 110.8(6) . . ? N26 C41 N1 112.6(6) . . ? N26 C41 H41A 109.1 . . ? N1 C41 H41A 109.1 . . ? N26 C41 H41B 109.1 . . ? N1 C41 H41B 109.1 . . ? H41A C41 H41B 107.8 . . ? N3 C42 N28 114.1(6) . . ? N3 C42 H42A 108.7 . . ? N28 C42 H42A 108.7 . . ? N3 C42 H42B 108.7 . . ? N28 C42 H42B 108.7 . . ? H42A C42 H42B 107.6 . . ? C1 N1 C2 110.7(6) . . ? C1 N1 C41 122.4(6) . . ? C2 N1 C41 122.6(6) . . ? C1 N2 C3 113.4(5) . . ? C1 N2 C5 123.9(6) . . ? C3 N2 C5 121.9(6) . . ? C4 N3 C42 124.6(6) . . ? C4 N3 C2 111.6(6) . . ? C42 N3 C2 122.7(6) . . ? C4 N4 C6 124.6(6) . . ? C4 N4 C3 111.2(5) . . ? C6 N4 C3 123.4(6) . . ? C7 N5 C8 112.1(5) . . ? C7 N5 C5 125.2(6) . . ? C8 N5 C5 122.6(6) . . ? C7 N6 C11 123.1(6) . . ? C7 N6 C9 110.3(6) . . ? C11 N6 C9 124.2(6) . . ? C10 N7 C6 122.7(6) . . ? C10 N7 C8 112.2(5) . . ? C6 N7 C8 123.3(6) . . ? C10 N8 C9 111.9(6) . . ? C10 N8 C12 122.5(6) . . ? C9 N8 C12 123.3(6) . . ? C13 N9 C11 123.6(6) . . ? C13 N9 C14 111.0(6) . . ? C11 N9 C14 122.2(6) . . ? C13 N10 C17 123.6(6) . . ? C13 N10 C15 110.9(6) . . ? C17 N10 C15 122.8(6) . . ? C16 N11 C12 121.0(6) . . ? C16 N11 C14 111.7(6) . . ? C12 N11 C14 121.7(6) . . ? C16 N12 C18 123.0(6) . . ? C16 N12 C15 112.6(6) . . ? C18 N12 C15 121.7(6) . . ? C19 N13 C20 112.8(6) . . ? C19 N13 C17 121.1(6) . . ? C20 N13 C17 123.8(6) . . ? C19 N14 C21 111.8(5) . . ? C19 N14 C23 123.0(6) . . ? C21 N14 C23 123.6(6) . . ? C22 N15 C18 123.3(6) . . ? C22 N15 C20 112.2(6) . . ? C18 N15 C20 123.2(6) . . ? C22 N16 C24 124.4(6) . . ? C22 N16 C21 113.7(5) . . ? C24 N16 C21 121.9(6) . . ? C25 N17 C23 124.3(6) . . ? C25 N17 C26 113.3(5) . . ? C23 N17 C26 121.3(6) . . ? C25 N18 C27 112.8(6) . . ? C25 N18 C29 123.4(6) . . ? C27 N18 C29 122.9(6) . . ? C28 N19 C26 113.3(6) . . ? C28 N19 C24 122.3(6) . . ? C26 N19 C24 124.0(6) . . ? C28 N20 C27 111.3(6) . . ? C28 N20 C30 122.5(6) . . ? C27 N20 C30 122.7(6) . . ? C31 N21 C29 123.4(6) . . ? C31 N21 C32 111.6(6) . . ? C29 N21 C32 122.7(6) . . ? C31 N22 C33 113.3(6) . . ? C31 N22 C35 121.1(6) . . ? C33 N22 C35 122.4(7) . . ? C34 N23 C30 122.5(6) . . ? C34 N23 C32 111.9(6) . . ? C30 N23 C32 123.7(6) . . ? C34 N24 C36 122.3(7) . . ? C34 N24 C33 111.5(6) . . ? C36 N24 C33 124.9(7) . . ? C37 N25 C38 114.0(6) . . ? C37 N25 C35 121.9(7) . . ? C38 N25 C35 122.8(7) . . ? C37 N26 C41 125.0(6) . . ? C37 N26 C39 111.3(6) . . ? C41 N26 C39 120.2(6) . . ? C40 N27 C38 111.4(6) . . ? C40 N27 C36 122.8(6) . . ? C38 N27 C36 122.2(6) . . ? C40 N28 C42 125.2(6) . . ? C40 N28 C39 110.8(6) . . ? C42 N28 C39 122.0(6) . . ? C1 O1 Pr1 161.5(5) . . ? C7 O2 Pr1 154.5(5) . . ? C25 O5 Pr1 152.8(5) . 2_766 ? C4 O8 Pr2 154.1(5) . 2_655 ? C22 O11 Pr2 154.7(5) . . ? C28 O12 Pr2 160.2(5) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.155 _refine_diff_density_min -2.282 _refine_diff_density_rms 0.242 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.007 0.000 0.500 1103 456 ' ' 2 0.228 0.789 0.777 114 51 ' ' 3 0.467 0.892 0.086 16 11 ' ' 4 0.533 0.108 0.914 16 9 ' ' 5 0.772 0.211 0.223 114 44 ' ' _platon_squeeze_details ; ; data_p6 _database_code_depnum_ccdc_archive 'CCDC 905587' #TrackingRef '4 (905587).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H66 N28 O26 Nd2, 2(Zn Cl4), 2Cl, 25(H2 O)' _chemical_formula_sum 'C42 H116 Cl10 N28 Nd2 O51 Zn2' _chemical_formula_weight 2603.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.9105(10) _cell_length_b 17.3140(10) _cell_length_c 20.3622(18) _cell_angle_alpha 98.271(2) _cell_angle_beta 112.638(3) _cell_angle_gamma 109.941(2) _cell_volume 4905.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour coloress _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.762 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2644 _exptl_absorpt_coefficient_mu 1.902 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6688 _exptl_absorpt_correction_T_max 0.7258 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51329 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.0539 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 25.10 _reflns_number_total 17247 _reflns_number_gt 14030 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1421P)^2^+2.9738P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17247 _refine_ls_number_parameters 1024 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0740 _refine_ls_R_factor_gt 0.0654 _refine_ls_wR_factor_ref 0.2078 _refine_ls_wR_factor_gt 0.1968 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl9 Cl 1.0000 0.5000 0.5000 0.164(3) Uani 1 2 d S . . Cl10 Cl 1.3207(4) -0.1979(3) 0.3914(3) 0.0654(12) Uani 0.50 1 d P . . Cl11 Cl 0.5135(4) -0.0419(4) 0.0216(4) 0.126(2) Uani 0.50 1 d PU . . Cl12 Cl 1.3371(5) 0.1857(6) 0.2321(6) 0.174(5) Uani 0.50 1 d P . . O1W O 0.8531(4) 0.1282(3) 0.0203(3) 0.0482(13) Uani 1 1 d . . . O2W O 0.8907(3) -0.0827(3) 0.1295(3) 0.0455(12) Uani 1 1 d . . . O3W O 0.7333(4) -0.0612(3) 0.1349(3) 0.0501(13) Uani 1 1 d . . . O4W O 1.0300(4) 0.1157(4) 0.1653(3) 0.0559(15) Uani 1 1 d . . . O5W O 0.9163(4) -0.0044(4) 0.0227(3) 0.0601(15) Uani 1 1 d . . . O6W O 0.7213(4) 0.0823(4) 0.0895(4) 0.0633(17) Uani 1 1 d . . . O7W O 1.7582(3) 0.3228(3) 0.5221(3) 0.0414(11) Uani 1 1 d . . . O8W O 1.5991(4) 0.3299(3) 0.5381(3) 0.0488(13) Uani 1 1 d . . . O9W O 1.4698(4) 0.3240(4) 0.3736(3) 0.0539(14) Uani 1 1 d . . . O10W O 1.6547(4) 0.5009(3) 0.3948(3) 0.0500(13) Uani 1 1 d . . . O11W O 1.7779(4) 0.4036(4) 0.4152(3) 0.0541(14) Uani 1 1 d . . . O12W O 1.5818(4) 0.4714(4) 0.4964(4) 0.0657(16) Uani 1 1 d . . . Nd1 Nd 0.85546(2) 0.04257(2) 0.108386(18) 0.02911(13) Uani 1 1 d . . . Nd2 Nd 1.64270(2) 0.375726(19) 0.443233(17) 0.02654(13) Uani 1 1 d . . . C1 C 0.9668(4) 0.0957(4) 0.3122(3) 0.0257(12) Uani 1 1 d . . . C2 C 1.0701(4) 0.1338(3) 0.4376(3) 0.0253(12) Uani 1 1 d . . . H2 H 1.0563 0.1012 0.4710 0.030 Uiso 1 1 calc R . . C3 C 1.0227(4) 0.1964(3) 0.4271(3) 0.0250(12) Uani 1 1 d . . . H3 H 0.9875 0.1946 0.4565 0.030 Uiso 1 1 calc R . . C4 C 1.1864(4) 0.2751(4) 0.4794(3) 0.0276(13) Uani 1 1 d . . . C5 C 0.8977(4) 0.2010(4) 0.3097(3) 0.0287(13) Uani 1 1 d . . . H5A H 0.8436 0.1563 0.2637 0.034 Uiso 1 1 calc R . . H5B H 0.8727 0.2193 0.3421 0.034 Uiso 1 1 calc R . . C6 C 1.0954(4) 0.3619(4) 0.4645(3) 0.0278(13) Uani 1 1 d . . . H6A H 1.0434 0.3554 0.4768 0.033 Uiso 1 1 calc R . . H6B H 1.1545 0.4061 0.5073 0.033 Uiso 1 1 calc R . . C7 C 0.9427(4) 0.2670(4) 0.2232(3) 0.0248(12) Uani 1 1 d . . . C8 C 0.9860(4) 0.3618(4) 0.3368(3) 0.0250(12) Uani 1 1 d . . . H8 H 0.9420 0.3744 0.3527 0.030 Uiso 1 1 calc R . . C9 C 1.0066(4) 0.4137(4) 0.2844(3) 0.0268(12) Uani 1 1 d . . . H9 H 0.9686 0.4470 0.2721 0.032 Uiso 1 1 calc R . . C10 C 1.1463(4) 0.4577(3) 0.3953(3) 0.0246(13) Uani 1 1 d . . . C11 C 0.9655(4) 0.3610(4) 0.1473(3) 0.0325(14) Uani 1 1 d . . . H11A H 0.9193 0.3064 0.1067 0.039 Uiso 1 1 calc R . . H11B H 0.9381 0.4027 0.1417 0.039 Uiso 1 1 calc R . . C12 C 1.1571(5) 0.5404(4) 0.3080(4) 0.0315(14) Uani 1 1 d . . . H12A H 1.2155 0.5819 0.3529 0.038 Uiso 1 1 calc R . . H12B H 1.1168 0.5701 0.2903 0.038 Uiso 1 1 calc R . . C13 C 1.0650(4) 0.3495(4) 0.0870(3) 0.0311(13) Uani 1 1 d . . . C14 C 1.1165(4) 0.4849(4) 0.1696(3) 0.0266(12) Uani 1 1 d . . . H14 H 1.0825 0.5215 0.1567 0.032 Uiso 1 1 calc R . . C15 C 1.1820(4) 0.4915(4) 0.1335(3) 0.0312(13) Uani 1 1 d . . . H15 H 1.1829 0.5342 0.1059 0.037 Uiso 1 1 calc R . . C16 C 1.2724(5) 0.5336(4) 0.2639(3) 0.0307(14) Uani 1 1 d . . . C17 C 1.1636(5) 0.3837(4) 0.0240(4) 0.0338(14) Uani 1 1 d . . . H17A H 1.1713 0.4307 0.0019 0.041 Uiso 1 1 calc R . . H17B H 1.1102 0.3309 -0.0153 0.041 Uiso 1 1 calc R . . C18 C 1.3626(5) 0.5505(4) 0.1912(4) 0.0321(14) Uani 1 1 d . . . H18A H 1.3589 0.5880 0.1594 0.038 Uiso 1 1 calc R . . H18B H 1.4154 0.5860 0.2413 0.038 Uiso 1 1 calc R . . C19 C 1.2492(5) 0.2940(4) 0.0222(3) 0.0323(14) Uani 1 1 d . . . C20 C 1.3446(4) 0.4415(4) 0.0822(3) 0.0285(13) Uani 1 1 d . . . H20 H 1.3476 0.4835 0.0540 0.034 Uiso 1 1 calc R . . C21 C 1.4074(4) 0.3953(3) 0.0794(3) 0.0278(13) Uani 1 1 d . . . H21 H 1.4430 0.4177 0.0522 0.033 Uiso 1 1 calc R . . C22 C 1.4567(4) 0.4679(4) 0.2046(3) 0.0299(13) Uani 1 1 d . . . C23 C 1.3619(5) 0.2421(4) 0.0084(3) 0.0325(14) Uani 1 1 d . . . H23A H 1.4063 0.2702 -0.0101 0.039 Uiso 1 1 calc R . . H23B H 1.3037 0.1975 -0.0349 0.039 Uiso 1 1 calc R . . C24 C 1.5514(4) 0.3959(4) 0.1827(4) 0.0297(13) Uani 1 1 d . . . H24A H 1.5963 0.4335 0.2345 0.036 Uiso 1 1 calc R . . H24B H 1.5830 0.4105 0.1518 0.036 Uiso 1 1 calc R . . C25 C 1.3587(4) 0.1162(4) 0.0557(3) 0.0267(13) Uani 1 1 d . . . C26 C 1.5037(4) 0.2404(4) 0.1136(3) 0.0262(12) Uani 1 1 d . . . H26 H 1.5445 0.2612 0.0898 0.031 Uiso 1 1 calc R . . C27 C 1.5177(4) 0.1667(3) 0.1439(3) 0.0246(12) Uani 1 1 d . . . H27 H 1.5609 0.1491 0.1306 0.029 Uiso 1 1 calc R . . C28 C 1.5618(4) 0.2850(4) 0.2423(3) 0.0249(12) Uani 1 1 d . . . C29 C 1.4010(5) 0.0134(4) 0.1187(3) 0.0304(14) Uani 1 1 d . . . H29A H 1.3421 -0.0299 0.0751 0.036 Uiso 1 1 calc R . . H29B H 1.4523 -0.0023 0.1211 0.036 Uiso 1 1 calc R . . C30 C 1.5981(4) 0.1670(4) 0.2760(4) 0.0296(14) Uani 1 1 d . . . H30A H 1.6522 0.2137 0.3206 0.036 Uiso 1 1 calc R . . H30B H 1.6227 0.1321 0.2548 0.036 Uiso 1 1 calc R . . C31 C 1.3043(4) -0.0253(3) 0.1834(3) 0.0262(13) Uani 1 1 d . . . C32 C 1.4679(4) 0.0230(3) 0.2552(3) 0.0264(12) Uani 1 1 d . . . H32 H 1.5013 -0.0125 0.2494 0.032 Uiso 1 1 calc R . . C33 C 1.4175(4) -0.0040(4) 0.3045(3) 0.0268(12) Uani 1 1 d . . . H33 H 1.4288 -0.0510 0.3231 0.032 Uiso 1 1 calc R . . C34 C 1.5246(4) 0.1406(4) 0.3603(3) 0.0267(12) Uani 1 1 d . . . C35 C 1.2416(4) -0.0827(4) 0.2660(3) 0.0293(13) Uani 1 1 d . . . H35A H 1.1846 -0.1159 0.2175 0.035 Uiso 1 1 calc R . . H35B H 1.2584 -0.1242 0.2896 0.035 Uiso 1 1 calc R . . C36 C 1.4482(4) 0.0770(4) 0.4326(3) 0.0300(13) Uani 1 1 d . . . H36A H 1.4520 0.0261 0.4467 0.036 Uiso 1 1 calc R . . H36B H 1.5010 0.1286 0.4735 0.036 Uiso 1 1 calc R . . C37 C 1.1306(4) -0.0335(4) 0.2882(3) 0.0309(14) Uani 1 1 d . . . C38 C 1.2731(4) -0.0019(4) 0.3936(3) 0.0265(12) Uani 1 1 d . . . H38 H 1.2854 -0.0479 0.4135 0.032 Uiso 1 1 calc R . . C39 C 1.2076(4) 0.0254(3) 0.4185(3) 0.0258(12) Uani 1 1 d . . . H39 H 1.1914 -0.0052 0.4523 0.031 Uiso 1 1 calc R . . C40 C 1.3551(4) 0.1443(4) 0.4638(3) 0.0298(13) Uani 1 1 d . . . C41 C 1.0363(4) -0.0041(4) 0.3462(4) 0.0298(13) Uani 1 1 d U . . H41A H 1.0270 -0.0324 0.3827 0.036 Uiso 1 1 calc R . . H41B H 0.9845 -0.0419 0.2963 0.036 Uiso 1 1 calc R . . C42 C 1.2458(4) 0.1666(4) 0.5077(3) 0.0288(13) Uani 1 1 d . . . H42A H 1.2276 0.1311 0.5374 0.035 Uiso 1 1 calc R . . H42B H 1.3039 0.2190 0.5422 0.035 Uiso 1 1 calc R . . N1 N 1.0305(4) 0.0772(3) 0.3619(3) 0.0290(11) Uani 1 1 d . . . N2 N 0.9598(4) 0.1635(3) 0.3478(3) 0.0268(11) Uani 1 1 d . . . N3 N 1.1712(4) 0.1906(3) 0.4693(3) 0.0294(11) Uani 1 1 d . . . N4 N 1.1022(3) 0.2799(3) 0.4532(3) 0.0266(11) Uani 1 1 d . . . N5 N 0.9436(4) 0.2737(3) 0.2905(3) 0.0300(11) Uani 1 1 d . . . N6 N 0.9815(4) 0.3464(3) 0.2189(3) 0.0272(11) Uani 1 1 d . . . N7 N 1.0788(4) 0.3911(3) 0.3996(3) 0.0268(11) Uani 1 1 d . . . N8 N 1.1082(3) 0.4698(3) 0.3282(3) 0.0272(11) Uani 1 1 d . . . N9 N 1.0518(4) 0.3934(3) 0.1398(3) 0.0283(11) Uani 1 1 d . . . N10 N 1.1411(4) 0.4047(3) 0.0840(3) 0.0330(12) Uani 1 1 d . . . N11 N 1.1816(4) 0.5137(3) 0.2500(3) 0.0315(12) Uani 1 1 d . . . N12 N 1.2738(4) 0.5171(3) 0.1964(3) 0.0345(12) Uani 1 1 d . . . N13 N 1.2499(4) 0.3705(3) 0.0485(3) 0.0314(12) Uani 1 1 d . . . N14 N 1.3395(4) 0.3051(3) 0.0408(3) 0.0301(11) Uani 1 1 d . . . N15 N 1.3822(4) 0.4836(3) 0.1609(3) 0.0316(11) Uani 1 1 d . . . N16 N 1.4700(4) 0.4141(3) 0.1573(3) 0.0317(12) Uani 1 1 d . . . N17 N 1.4038(3) 0.2005(3) 0.0598(3) 0.0266(11) Uani 1 1 d . . . N18 N 1.4214(4) 0.0975(3) 0.1073(3) 0.0276(11) Uani 1 1 d . . . N19 N 1.5298(4) 0.3069(3) 0.1801(3) 0.0264(11) Uani 1 1 d . . . N20 N 1.5573(3) 0.2040(3) 0.2232(3) 0.0264(11) Uani 1 1 d . . . N21 N 1.3912(4) 0.0095(3) 0.1850(3) 0.0268(11) Uani 1 1 d . . . N22 N 1.3186(3) -0.0315(3) 0.2531(3) 0.0264(10) Uani 1 1 d . . . N23 N 1.5340(3) 0.1129(3) 0.2991(3) 0.0270(11) Uani 1 1 d . . . N24 N 1.4590(3) 0.0753(3) 0.3647(3) 0.0256(10) Uani 1 1 d . . . N25 N 1.2196(4) -0.0323(3) 0.3126(3) 0.0281(11) Uani 1 1 d . . . N26 N 1.1249(4) 0.0043(3) 0.3485(3) 0.0298(11) Uani 1 1 d U . . N27 N 1.3591(3) 0.0776(3) 0.4240(3) 0.0288(11) Uani 1 1 d . . . N28 N 1.2647(4) 0.1185(3) 0.4558(3) 0.0289(11) Uani 1 1 d . . . O1 O 0.9196(3) 0.0562(3) 0.2439(2) 0.0361(10) Uani 1 1 d . . . O2 O 0.9112(3) 0.1982(3) 0.1734(2) 0.0326(10) Uani 1 1 d . . . O3 O 1.0147(4) 0.2732(3) 0.0484(3) 0.0447(12) Uani 1 1 d . . . O4 O 1.1771(3) 0.2246(3) -0.0123(3) 0.0461(12) Uani 1 1 d . . . O5 O 1.2758(3) 0.0666(3) 0.0120(2) 0.0327(10) Uani 1 1 d . . . O6 O 1.2267(3) -0.0474(3) 0.1296(2) 0.0383(11) Uani 1 1 d . . . O7 O 1.0689(3) -0.0618(3) 0.2232(3) 0.0426(12) Uani 1 1 d . . . O8 O 1.2662(3) 0.3366(3) 0.5088(3) 0.0383(11) Uani 1 1 d . . . O9 O 1.2292(3) 0.5008(3) 0.4455(2) 0.0329(10) Uani 1 1 d . . . O10 O 1.3416(3) 0.5621(3) 0.3249(2) 0.0421(11) Uani 1 1 d . . . O11 O 1.5030(4) 0.4972(3) 0.2721(3) 0.0461(12) Uani 1 1 d . . . O12 O 1.5927(3) 0.3312(3) 0.3061(2) 0.0323(10) Uani 1 1 d . . . O13 O 1.5717(3) 0.2152(3) 0.4053(2) 0.0380(11) Uani 1 1 d . . . O14 O 1.4208(3) 0.2167(3) 0.5011(3) 0.0401(11) Uani 1 1 d . . . Cl1 Cl 1.67838(15) 0.00562(13) 0.25926(11) 0.0517(5) Uani 1 1 d . . . Cl2 Cl 1.80583(15) 0.18862(13) 0.43950(12) 0.0527(5) Uani 1 1 d . . . Cl3 Cl 1.86297(15) 0.00494(14) 0.42863(15) 0.0617(6) Uani 1 1 d . . . Cl4 Cl 1.62574(14) -0.02253(17) 0.41621(12) 0.0611(6) Uani 1 1 d . . . Cl5 Cl 0.7279(3) 0.2744(4) 0.1184(3) 0.168(2) Uani 1 1 d D . . Cl6 Cl 0.5935(4) 0.3849(3) 0.0116(3) 0.1581(18) Uani 1 1 d DU . . Cl7 Cl 0.7984(5) 0.3908(5) -0.0078(5) 0.237(3) Uani 1 1 d DU . . Cl8 Cl 0.5859(11) 0.1920(7) -0.0976(6) 0.234(6) Uani 0.50 1 d PDU . . Cl8' Cl 0.8687(6) 0.5200(4) 0.1492(6) 0.179(4) Uani 0.50 1 d PDU . . Zn1 Zn 1.74113(6) 0.04281(6) 0.38557(5) 0.0431(2) Uani 1 1 d . . . Zn2 Zn 0.6771(3) 0.3067(2) 0.0096(2) 0.1329(13) Uani 0.50 1 d PD . . Zn2' Zn 0.7426(3) 0.3913(3) 0.0717(3) 0.1400(14) Uani 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl9 0.051(2) 0.138(4) 0.183(5) -0.101(4) -0.022(3) 0.058(3) Cl10 0.078(3) 0.070(3) 0.060(3) 0.044(2) 0.022(2) 0.045(2) Cl11 0.070(3) 0.141(4) 0.102(3) -0.048(3) 0.069(3) -0.024(3) Cl12 0.069(4) 0.137(7) 0.195(9) -0.085(7) -0.004(5) 0.044(4) O1W 0.048(3) 0.049(3) 0.032(3) 0.007(2) 0.014(2) 0.012(2) O2W 0.035(3) 0.044(3) 0.041(3) -0.006(2) 0.008(2) 0.017(2) O3W 0.041(3) 0.056(3) 0.042(3) 0.003(2) 0.024(2) 0.008(2) O4W 0.027(3) 0.061(3) 0.059(3) -0.004(3) 0.018(3) 0.009(2) O5W 0.048(3) 0.077(4) 0.053(3) 0.001(3) 0.031(3) 0.024(3) O6W 0.030(3) 0.050(3) 0.085(4) -0.006(3) 0.018(3) 0.013(2) O7W 0.044(3) 0.042(3) 0.036(3) 0.009(2) 0.013(2) 0.023(2) O8W 0.037(3) 0.048(3) 0.039(3) -0.004(2) 0.021(2) -0.002(2) O9W 0.031(3) 0.064(3) 0.049(3) -0.001(3) 0.009(2) 0.019(3) O10W 0.058(3) 0.031(2) 0.040(3) 0.007(2) 0.004(3) 0.019(2) O11W 0.033(3) 0.085(4) 0.043(3) 0.021(3) 0.018(2) 0.025(3) O12W 0.059(4) 0.058(3) 0.075(4) 0.001(3) 0.033(3) 0.027(3) Nd1 0.0201(2) 0.0294(2) 0.0257(2) -0.00157(14) 0.00726(16) 0.00549(15) Nd2 0.0211(2) 0.02393(19) 0.0242(2) 0.00206(14) 0.00595(15) 0.00597(14) C1 0.020(3) 0.023(3) 0.028(3) 0.006(2) 0.011(3) 0.004(2) C2 0.023(3) 0.022(3) 0.028(3) 0.006(2) 0.011(3) 0.008(2) C3 0.022(3) 0.021(3) 0.027(3) 0.006(2) 0.011(3) 0.004(2) C4 0.026(3) 0.019(3) 0.029(3) 0.002(2) 0.008(3) 0.007(2) C5 0.013(3) 0.046(3) 0.019(3) 0.011(3) 0.005(2) 0.008(3) C6 0.030(3) 0.023(3) 0.024(3) 0.001(2) 0.007(3) 0.014(3) C7 0.017(3) 0.031(3) 0.017(3) 0.006(2) 0.004(2) 0.006(2) C8 0.022(3) 0.028(3) 0.021(3) 0.006(2) 0.008(2) 0.011(2) C9 0.026(3) 0.027(3) 0.021(3) 0.005(2) 0.007(3) 0.011(2) C10 0.025(3) 0.019(3) 0.026(3) 0.001(2) 0.011(3) 0.009(3) C11 0.024(3) 0.037(3) 0.027(3) 0.009(3) 0.007(3) 0.010(3) C12 0.035(4) 0.022(3) 0.036(3) 0.004(2) 0.019(3) 0.011(3) C13 0.027(3) 0.035(3) 0.021(3) 0.007(3) 0.003(3) 0.012(3) C14 0.026(3) 0.025(3) 0.026(3) 0.010(2) 0.009(3) 0.011(2) C15 0.032(3) 0.032(3) 0.026(3) 0.008(3) 0.009(3) 0.014(3) C16 0.032(4) 0.028(3) 0.028(3) 0.005(3) 0.013(3) 0.012(3) C17 0.030(3) 0.044(4) 0.026(3) 0.007(3) 0.012(3) 0.018(3) C18 0.033(3) 0.026(3) 0.034(3) 0.005(3) 0.016(3) 0.012(3) C19 0.031(4) 0.030(3) 0.027(3) 0.001(3) 0.009(3) 0.011(3) C20 0.025(3) 0.027(3) 0.027(3) 0.006(2) 0.010(3) 0.008(2) C21 0.035(3) 0.021(3) 0.023(3) 0.005(2) 0.009(3) 0.013(3) C22 0.030(3) 0.023(3) 0.030(4) 0.003(2) 0.011(3) 0.009(3) C23 0.033(4) 0.031(3) 0.025(3) 0.001(3) 0.008(3) 0.015(3) C24 0.023(3) 0.022(3) 0.029(3) 0.004(2) 0.004(3) 0.004(2) C25 0.030(4) 0.029(3) 0.024(3) 0.006(3) 0.016(3) 0.013(3) C26 0.023(3) 0.026(3) 0.026(3) 0.006(2) 0.010(3) 0.009(2) C27 0.021(3) 0.021(3) 0.026(3) 0.001(2) 0.009(3) 0.008(2) C28 0.015(3) 0.020(3) 0.029(3) 0.000(2) 0.006(2) 0.005(2) C29 0.030(3) 0.021(3) 0.032(3) -0.001(2) 0.017(3) 0.003(2) C30 0.016(3) 0.017(3) 0.042(4) 0.003(2) 0.005(3) 0.005(2) C31 0.027(3) 0.018(3) 0.030(3) 0.003(2) 0.013(3) 0.009(2) C32 0.020(3) 0.018(3) 0.031(3) 0.003(2) 0.006(3) 0.006(2) C33 0.028(3) 0.023(3) 0.028(3) 0.006(2) 0.011(3) 0.011(2) C34 0.026(3) 0.026(3) 0.028(3) 0.009(2) 0.010(3) 0.014(3) C35 0.030(3) 0.023(3) 0.031(3) 0.006(2) 0.014(3) 0.010(2) C36 0.024(3) 0.037(3) 0.024(3) 0.006(3) 0.010(3) 0.010(3) C37 0.025(3) 0.020(3) 0.029(3) -0.003(2) 0.004(3) 0.004(2) C38 0.028(3) 0.027(3) 0.025(3) 0.007(2) 0.012(3) 0.012(2) C39 0.022(3) 0.018(3) 0.032(3) 0.008(2) 0.012(3) 0.005(2) C40 0.025(3) 0.028(3) 0.028(3) 0.008(3) 0.009(3) 0.007(3) C41 0.025(3) 0.022(3) 0.035(3) 0.001(2) 0.013(3) 0.007(2) C42 0.031(3) 0.029(3) 0.026(3) 0.006(2) 0.011(3) 0.015(3) N1 0.028(3) 0.024(2) 0.028(3) 0.004(2) 0.009(2) 0.010(2) N2 0.027(3) 0.026(2) 0.023(3) 0.005(2) 0.010(2) 0.010(2) N3 0.026(3) 0.017(2) 0.041(3) 0.006(2) 0.014(2) 0.008(2) N4 0.025(3) 0.020(2) 0.028(3) 0.003(2) 0.007(2) 0.011(2) N5 0.027(3) 0.027(2) 0.029(3) 0.005(2) 0.012(2) 0.008(2) N6 0.028(3) 0.028(3) 0.021(2) 0.007(2) 0.010(2) 0.009(2) N7 0.026(3) 0.025(2) 0.028(3) 0.008(2) 0.012(2) 0.011(2) N8 0.024(3) 0.024(2) 0.027(3) 0.007(2) 0.009(2) 0.007(2) N9 0.031(3) 0.026(2) 0.022(3) 0.005(2) 0.012(2) 0.009(2) N10 0.040(3) 0.027(3) 0.025(3) 0.000(2) 0.013(2) 0.013(2) N11 0.030(3) 0.034(3) 0.022(3) 0.001(2) 0.008(2) 0.011(2) N12 0.026(3) 0.037(3) 0.029(3) 0.000(2) 0.009(2) 0.010(2) N13 0.023(3) 0.028(2) 0.033(3) 0.000(2) 0.007(2) 0.010(2) N14 0.025(3) 0.026(2) 0.027(3) 0.002(2) 0.006(2) 0.006(2) N15 0.032(3) 0.033(3) 0.028(3) 0.005(2) 0.015(2) 0.013(2) N16 0.037(3) 0.025(2) 0.023(3) 0.006(2) 0.005(2) 0.014(2) N17 0.019(2) 0.020(2) 0.025(3) 0.0010(19) 0.003(2) 0.002(2) N18 0.025(3) 0.025(2) 0.026(3) 0.005(2) 0.009(2) 0.009(2) N19 0.030(3) 0.019(2) 0.025(3) 0.008(2) 0.009(2) 0.008(2) N20 0.023(3) 0.024(2) 0.016(2) -0.0014(19) 0.002(2) 0.005(2) N21 0.025(3) 0.024(2) 0.026(3) 0.003(2) 0.012(2) 0.007(2) N22 0.016(2) 0.029(2) 0.024(3) 0.005(2) 0.005(2) 0.004(2) N23 0.025(3) 0.020(2) 0.028(3) 0.005(2) 0.010(2) 0.006(2) N24 0.023(3) 0.025(2) 0.025(3) 0.004(2) 0.008(2) 0.010(2) N25 0.025(3) 0.027(2) 0.023(3) 0.002(2) 0.006(2) 0.010(2) N26 0.021(2) 0.028(2) 0.032(3) 0.002(2) 0.009(2) 0.009(2) N27 0.023(3) 0.032(3) 0.031(3) 0.009(2) 0.013(2) 0.012(2) N28 0.028(3) 0.020(2) 0.029(3) 0.003(2) 0.009(2) 0.007(2) O1 0.036(3) 0.034(2) 0.024(2) 0.0024(19) 0.007(2) 0.010(2) O2 0.028(2) 0.028(2) 0.029(2) 0.0007(17) 0.0096(19) 0.0064(18) O3 0.045(3) 0.033(2) 0.038(3) -0.002(2) 0.018(2) 0.005(2) O4 0.027(2) 0.035(2) 0.051(3) -0.009(2) 0.011(2) 0.005(2) O5 0.024(2) 0.031(2) 0.026(2) -0.0005(18) 0.0048(19) 0.0054(19) O6 0.023(2) 0.048(3) 0.029(2) 0.002(2) 0.008(2) 0.008(2) O7 0.032(3) 0.049(3) 0.035(3) 0.001(2) 0.006(2) 0.020(2) O8 0.023(2) 0.024(2) 0.050(3) -0.0003(19) 0.008(2) 0.0045(19) O9 0.028(2) 0.026(2) 0.028(2) 0.0031(18) 0.005(2) 0.0056(19) O10 0.030(3) 0.056(3) 0.024(2) -0.001(2) 0.005(2) 0.016(2) O11 0.047(3) 0.050(3) 0.028(3) 0.003(2) 0.002(2) 0.028(2) O12 0.033(2) 0.030(2) 0.021(2) 0.0006(17) 0.0051(18) 0.0112(19) O13 0.044(3) 0.024(2) 0.031(2) -0.0016(18) 0.013(2) 0.007(2) O14 0.029(2) 0.033(2) 0.045(3) 0.000(2) 0.018(2) 0.003(2) Cl1 0.0640(12) 0.0574(11) 0.0511(11) 0.0169(9) 0.0362(10) 0.0346(10) Cl2 0.0602(12) 0.0598(11) 0.0555(11) 0.0177(9) 0.0341(10) 0.0370(10) Cl3 0.0460(11) 0.0701(13) 0.1045(17) 0.0613(13) 0.0466(12) 0.0370(10) Cl4 0.0403(11) 0.1022(17) 0.0602(12) 0.0490(12) 0.0304(10) 0.0348(11) Cl5 0.110(3) 0.207(5) 0.264(6) 0.156(5) 0.114(4) 0.090(3) Cl6 0.148(3) 0.182(4) 0.182(4) 0.102(3) 0.097(3) 0.073(3) Cl7 0.253(5) 0.250(5) 0.215(5) 0.116(4) 0.109(4) 0.103(4) Cl8 0.246(8) 0.212(8) 0.230(8) 0.083(5) 0.095(5) 0.097(5) Cl8' 0.203(6) 0.166(5) 0.181(6) 0.071(4) 0.075(4) 0.106(5) Zn1 0.0422(5) 0.0565(5) 0.0519(5) 0.0316(4) 0.0298(4) 0.0298(4) Zn2 0.148(4) 0.109(3) 0.138(3) 0.037(2) 0.069(3) 0.050(3) Zn2' 0.125(3) 0.169(4) 0.135(3) 0.071(3) 0.063(3) 0.061(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl11 Cl11 1.898(19) 2_655 ? O1W Nd1 2.483(5) . ? O2W Nd1 2.488(5) . ? O3W Nd1 2.529(5) . ? O4W Nd1 2.460(5) . ? O5W Nd1 2.511(5) . ? O6W Nd1 2.498(5) . ? O7W Nd2 2.543(5) . ? O8W Nd2 2.458(5) . ? O9W Nd2 2.454(5) . ? O10W Nd2 2.485(5) . ? O11W Nd2 2.473(5) . ? O12W Nd2 2.546(5) . ? Nd1 O5 2.474(4) 2_755 ? Nd1 O1 2.486(4) . ? Nd1 O2 2.486(4) . ? Nd2 O9 2.462(4) 2_866 ? Nd2 O13 2.481(4) . ? Nd2 O12 2.496(4) . ? C1 O1 1.241(7) . ? C1 N1 1.333(8) . ? C1 N2 1.354(7) . ? C2 N1 1.452(7) . ? C2 N3 1.458(7) . ? C2 C3 1.546(8) . ? C2 H2 0.9900 . ? C3 N2 1.435(8) . ? C3 N4 1.444(7) . ? C3 H3 0.9900 . ? C4 O8 1.236(7) . ? C4 N4 1.351(8) . ? C4 N3 1.366(7) . ? C5 N5 1.432(8) . ? C5 N2 1.454(8) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.442(8) . ? C6 N4 1.456(7) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.239(7) . ? C7 N6 1.338(8) . ? C7 N5 1.352(8) . ? C8 N5 1.431(7) . ? C8 N7 1.443(8) . ? C8 C9 1.556(8) . ? C8 H8 0.9900 . ? C9 N6 1.447(7) . ? C9 N8 1.457(8) . ? C9 H9 0.9900 . ? C10 O9 1.238(7) . ? C10 N8 1.351(8) . ? C10 N7 1.359(7) . ? C11 N9 1.449(8) . ? C11 N6 1.454(8) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.435(8) . ? C12 N11 1.460(8) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.228(7) . ? C13 N10 1.345(8) . ? C13 N9 1.361(8) . ? C14 N9 1.450(7) . ? C14 N11 1.465(8) . ? C14 C15 1.531(9) . ? C14 H14 0.9900 . ? C15 N10 1.440(7) . ? C15 N12 1.444(8) . ? C15 H15 0.9900 . ? C16 O10 1.211(8) . ? C16 N11 1.353(8) . ? C16 N12 1.373(8) . ? C17 N10 1.448(8) . ? C17 N13 1.459(8) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N15 1.430(7) . ? C18 N12 1.466(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.234(7) . ? C19 N13 1.349(8) . ? C19 N14 1.359(8) . ? C20 N15 1.438(8) . ? C20 N13 1.454(8) . ? C20 C21 1.543(8) . ? C20 H20 0.9900 . ? C21 N16 1.438(8) . ? C21 N14 1.451(7) . ? C21 H21 0.9900 . ? C22 O11 1.208(8) . ? C22 N15 1.376(8) . ? C22 N16 1.377(8) . ? C23 N14 1.428(8) . ? C23 N17 1.452(8) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N16 1.435(8) . ? C24 N19 1.445(7) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O5 1.222(7) . ? C25 N18 1.344(8) . ? C25 N17 1.371(8) . ? C26 N17 1.446(8) . ? C26 N19 1.448(7) . ? C26 C27 1.544(8) . ? C26 H26 0.9900 . ? C27 N20 1.430(7) . ? C27 N18 1.456(7) . ? C27 H27 0.9900 . ? C28 O12 1.222(7) . ? C28 N19 1.338(8) . ? C28 N20 1.369(7) . ? C29 N21 1.430(8) . ? C29 N18 1.453(8) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N20 1.404(8) . ? C30 N23 1.449(8) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O6 1.225(7) . ? C31 N22 1.371(8) . ? C31 N21 1.371(8) . ? C32 N21 1.431(8) . ? C32 N23 1.455(7) . ? C32 C33 1.572(8) . ? C32 H32 0.9900 . ? C33 N24 1.441(7) . ? C33 N22 1.443(8) . ? C33 H33 0.9900 . ? C34 O13 1.241(7) . ? C34 N24 1.329(8) . ? C34 N23 1.357(8) . ? C35 N25 1.433(7) . ? C35 N22 1.448(8) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N27 1.452(8) . ? C36 N24 1.461(7) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 O7 1.218(8) . ? C37 N26 1.360(8) . ? C37 N25 1.382(8) . ? C38 N27 1.445(7) . ? C38 N25 1.447(8) . ? C38 C39 1.558(8) . ? C38 H38 0.9900 . ? C39 N26 1.445(8) . ? C39 N28 1.460(7) . ? C39 H39 0.9900 . ? C40 O14 1.229(7) . ? C40 N27 1.350(8) . ? C40 N28 1.372(8) . ? C41 N26 1.435(8) . ? C41 N1 1.444(7) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 N3 1.438(8) . ? C42 N28 1.450(7) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? O5 Nd1 2.474(4) 2_755 ? O9 Nd2 2.462(4) 2_866 ? Cl1 Zn1 2.261(2) . ? Cl2 Zn1 2.274(2) . ? Cl3 Zn1 2.267(2) . ? Cl4 Zn1 2.261(2) . ? Cl5 Zn2 2.276(2) . ? Cl5 Zn2' 2.336(6) . ? Cl6 Zn2 2.273(2) . ? Cl6 Zn2' 2.293(6) . ? Cl7 Zn2' 2.164(8) . ? Cl7 Zn2 2.263(2) . ? Cl8 Zn2 2.271(2) . ? Cl8' Zn2' 2.272(2) . ? Zn2 Zn2' 1.502(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4W Nd1 O5 136.10(16) . 2_755 ? O4W Nd1 O1W 86.8(2) . . ? O5 Nd1 O1W 78.32(16) 2_755 . ? O4W Nd1 O1 72.59(18) . . ? O5 Nd1 O1 137.34(15) 2_755 . ? O1W Nd1 O1 142.91(15) . . ? O4W Nd1 O2 70.98(16) . . ? O5 Nd1 O2 136.36(15) 2_755 . ? O1W Nd1 O2 68.88(15) . . ? O1 Nd1 O2 75.26(14) . . ? O4W Nd1 O2W 80.93(18) . . ? O5 Nd1 O2W 83.03(15) 2_755 . ? O1W Nd1 O2W 137.72(17) . . ? O1 Nd1 O2W 70.09(15) . . ? O2 Nd1 O2W 140.51(15) . . ? O4W Nd1 O6W 138.18(18) . . ? O5 Nd1 O6W 76.84(16) 2_755 . ? O1W Nd1 O6W 74.6(2) . . ? O1 Nd1 O6W 100.42(19) . . ? O2 Nd1 O6W 67.43(16) . . ? O2W Nd1 O6W 136.74(19) . . ? O4W Nd1 O5W 67.80(18) . . ? O5 Nd1 O5W 68.30(16) 2_755 . ? O1W Nd1 O5W 69.4(2) . . ? O1 Nd1 O5W 125.82(18) . . ? O2 Nd1 O5W 121.68(17) . . ? O2W Nd1 O5W 68.5(2) . . ? O6W Nd1 O5W 133.7(2) . . ? O4W Nd1 O3W 136.8(2) . . ? O5 Nd1 O3W 71.46(15) 2_755 . ? O1W Nd1 O3W 136.15(18) . . ? O1 Nd1 O3W 68.31(16) . . ? O2 Nd1 O3W 114.49(15) . . ? O2W Nd1 O3W 69.21(18) . . ? O6W Nd1 O3W 68.2(2) . . ? O5W Nd1 O3W 123.83(18) . . ? O9W Nd2 O8W 80.76(19) . . ? O9W Nd2 O9 134.13(16) . 2_866 ? O8W Nd2 O9 81.42(15) . 2_866 ? O9W Nd2 O11W 137.87(18) . . ? O8W Nd2 O11W 137.62(19) . . ? O9 Nd2 O11W 78.91(17) 2_866 . ? O9W Nd2 O13 73.16(18) . . ? O8W Nd2 O13 71.50(16) . . ? O9 Nd2 O13 137.82(15) 2_866 . ? O11W Nd2 O13 99.78(18) . . ? O9W Nd2 O10W 86.2(2) . . ? O8W Nd2 O10W 134.99(18) . . ? O9 Nd2 O10W 77.43(15) 2_866 . ? O11W Nd2 O10W 75.8(2) . . ? O13 Nd2 O10W 143.79(15) . . ? O9W Nd2 O12 71.19(17) . . ? O8W Nd2 O12 142.25(15) . . ? O9 Nd2 O12 136.33(15) 2_866 . ? O11W Nd2 O12 66.82(16) . . ? O13 Nd2 O12 76.43(14) . . ? O10W Nd2 O12 68.76(15) . . ? O9W Nd2 O7W 137.42(19) . . ? O8W Nd2 O7W 70.07(18) . . ? O9 Nd2 O7W 72.07(15) 2_866 . ? O11W Nd2 O7W 68.26(18) . . ? O13 Nd2 O7W 68.60(16) . . ? O10W Nd2 O7W 136.28(17) . . ? O12 Nd2 O7W 115.68(14) . . ? O9W Nd2 O12W 66.76(18) . . ? O8W Nd2 O12W 67.4(2) . . ? O9 Nd2 O12W 67.37(17) 2_866 . ? O11W Nd2 O12W 134.5(2) . . ? O13 Nd2 O12W 125.76(19) . . ? O10W Nd2 O12W 67.9(2) . . ? O12 Nd2 O12W 120.15(19) . . ? O7W Nd2 O12W 124.15(19) . . ? O1 C1 N1 125.6(5) . . ? O1 C1 N2 124.8(6) . . ? N1 C1 N2 109.5(5) . . ? N1 C2 N3 112.8(5) . . ? N1 C2 C3 103.8(5) . . ? N3 C2 C3 103.8(4) . . ? N1 C2 H2 112.0 . . ? N3 C2 H2 112.0 . . ? C3 C2 H2 112.0 . . ? N2 C3 N4 115.6(5) . . ? N2 C3 C2 102.1(4) . . ? N4 C3 C2 103.1(4) . . ? N2 C3 H3 111.8 . . ? N4 C3 H3 111.8 . . ? C2 C3 H3 111.8 . . ? O8 C4 N4 126.5(5) . . ? O8 C4 N3 123.8(6) . . ? N4 C4 N3 109.8(5) . . ? N5 C5 N2 113.7(5) . . ? N5 C5 H5A 108.8 . . ? N2 C5 H5A 108.8 . . ? N5 C5 H5B 108.8 . . ? N2 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N7 C6 N4 113.0(5) . . ? N7 C6 H6A 109.0 . . ? N4 C6 H6A 109.0 . . ? N7 C6 H6B 109.0 . . ? N4 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? O2 C7 N6 125.4(5) . . ? O2 C7 N5 125.3(5) . . ? N6 C7 N5 109.3(5) . . ? N5 C8 N7 115.6(5) . . ? N5 C8 C9 102.7(4) . . ? N7 C8 C9 103.3(5) . . ? N5 C8 H8 111.5 . . ? N7 C8 H8 111.5 . . ? C9 C8 H8 111.5 . . ? N6 C9 N8 114.3(5) . . ? N6 C9 C8 102.7(4) . . ? N8 C9 C8 102.7(5) . . ? N6 C9 H9 112.1 . . ? N8 C9 H9 112.1 . . ? C8 C9 H9 112.1 . . ? O9 C10 N8 125.6(5) . . ? O9 C10 N7 125.1(6) . . ? N8 C10 N7 109.3(5) . . ? N9 C11 N6 112.9(5) . . ? N9 C11 H11A 109.0 . . ? N6 C11 H11A 109.0 . . ? N9 C11 H11B 109.0 . . ? N6 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? N8 C12 N11 113.7(5) . . ? N8 C12 H12A 108.8 . . ? N11 C12 H12A 108.8 . . ? N8 C12 H12B 108.8 . . ? N11 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N10 126.6(6) . . ? O3 C13 N9 125.3(6) . . ? N10 C13 N9 108.1(5) . . ? N9 C14 N11 113.4(5) . . ? N9 C14 C15 103.5(5) . . ? N11 C14 C15 103.4(5) . . ? N9 C14 H14 112.0 . . ? N11 C14 H14 112.0 . . ? C15 C14 H14 112.0 . . ? N10 C15 N12 114.0(5) . . ? N10 C15 C14 102.8(5) . . ? N12 C15 C14 103.5(5) . . ? N10 C15 H15 111.9 . . ? N12 C15 H15 111.9 . . ? C14 C15 H15 111.9 . . ? O10 C16 N11 126.7(6) . . ? O10 C16 N12 124.9(6) . . ? N11 C16 N12 108.4(5) . . ? N10 C17 N13 113.4(5) . . ? N10 C17 H17A 108.9 . . ? N13 C17 H17A 108.9 . . ? N10 C17 H17B 108.9 . . ? N13 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? N15 C18 N12 113.2(5) . . ? N15 C18 H18A 108.9 . . ? N12 C18 H18A 108.9 . . ? N15 C18 H18B 108.9 . . ? N12 C18 H18B 108.9 . . ? H18A C18 H18B 107.8 . . ? O4 C19 N13 124.7(6) . . ? O4 C19 N14 125.6(6) . . ? N13 C19 N14 109.7(5) . . ? N15 C20 N13 113.7(5) . . ? N15 C20 C21 104.1(5) . . ? N13 C20 C21 103.2(5) . . ? N15 C20 H20 111.8 . . ? N13 C20 H20 111.8 . . ? C21 C20 H20 111.8 . . ? N16 C21 N14 114.5(5) . . ? N16 C21 C20 103.2(5) . . ? N14 C21 C20 103.5(5) . . ? N16 C21 H21 111.7 . . ? N14 C21 H21 111.7 . . ? C20 C21 H21 111.7 . . ? O11 C22 N15 126.1(5) . . ? O11 C22 N16 126.3(6) . . ? N15 C22 N16 107.6(5) . . ? N14 C23 N17 114.0(5) . . ? N14 C23 H23A 108.8 . . ? N17 C23 H23A 108.8 . . ? N14 C23 H23B 108.8 . . ? N17 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? N16 C24 N19 114.3(5) . . ? N16 C24 H24A 108.7 . . ? N19 C24 H24A 108.7 . . ? N16 C24 H24B 108.7 . . ? N19 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? O5 C25 N18 126.2(6) . . ? O5 C25 N17 125.5(6) . . ? N18 C25 N17 108.3(5) . . ? N17 C26 N19 114.7(5) . . ? N17 C26 C27 103.3(5) . . ? N19 C26 C27 103.3(5) . . ? N17 C26 H26 111.6 . . ? N19 C26 H26 111.6 . . ? C27 C26 H26 111.6 . . ? N20 C27 N18 115.1(5) . . ? N20 C27 C26 103.1(4) . . ? N18 C27 C26 102.7(5) . . ? N20 C27 H27 111.7 . . ? N18 C27 H27 111.7 . . ? C26 C27 H27 111.7 . . ? O12 C28 N19 125.3(5) . . ? O12 C28 N20 125.6(6) . . ? N19 C28 N20 109.1(5) . . ? N21 C29 N18 114.3(5) . . ? N21 C29 H29A 108.7 . . ? N18 C29 H29A 108.7 . . ? N21 C29 H29B 108.7 . . ? N18 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? N20 C30 N23 114.8(5) . . ? N20 C30 H30A 108.6 . . ? N23 C30 H30A 108.6 . . ? N20 C30 H30B 108.6 . . ? N23 C30 H30B 108.6 . . ? H30A C30 H30B 107.5 . . ? O6 C31 N22 125.2(5) . . ? O6 C31 N21 126.5(6) . . ? N22 C31 N21 108.3(5) . . ? N21 C32 N23 115.7(5) . . ? N21 C32 C33 103.6(5) . . ? N23 C32 C33 101.5(4) . . ? N21 C32 H32 111.8 . . ? N23 C32 H32 111.8 . . ? C33 C32 H32 111.8 . . ? N24 C33 N22 114.1(5) . . ? N24 C33 C32 103.2(4) . . ? N22 C33 C32 102.5(5) . . ? N24 C33 H33 112.1 . . ? N22 C33 H33 112.1 . . ? C32 C33 H33 112.1 . . ? O13 C34 N24 126.0(6) . . ? O13 C34 N23 124.6(6) . . ? N24 C34 N23 109.4(5) . . ? N25 C35 N22 113.8(5) . . ? N25 C35 H35A 108.8 . . ? N22 C35 H35A 108.8 . . ? N25 C35 H35B 108.8 . . ? N22 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? N27 C36 N24 113.2(5) . . ? N27 C36 H36A 108.9 . . ? N24 C36 H36A 108.9 . . ? N27 C36 H36B 108.9 . . ? N24 C36 H36B 108.9 . . ? H36A C36 H36B 107.7 . . ? O7 C37 N26 126.0(6) . . ? O7 C37 N25 125.3(6) . . ? N26 C37 N25 108.6(5) . . ? N27 C38 N25 114.3(5) . . ? N27 C38 C39 103.4(4) . . ? N25 C38 C39 103.1(5) . . ? N27 C38 H38 111.8 . . ? N25 C38 H38 111.8 . . ? C39 C38 H38 111.8 . . ? N26 C39 N28 112.9(5) . . ? N26 C39 C38 103.7(5) . . ? N28 C39 C38 102.6(4) . . ? N26 C39 H39 112.3 . . ? N28 C39 H39 112.3 . . ? C38 C39 H39 112.3 . . ? O14 C40 N27 126.2(6) . . ? O14 C40 N28 124.9(6) . . ? N27 C40 N28 108.9(5) . . ? N26 C41 N1 113.9(5) . . ? N26 C41 H41A 108.8 . . ? N1 C41 H41A 108.8 . . ? N26 C41 H41B 108.8 . . ? N1 C41 H41B 108.8 . . ? H41A C41 H41B 107.7 . . ? N3 C42 N28 111.9(5) . . ? N3 C42 H42A 109.2 . . ? N28 C42 H42A 109.2 . . ? N3 C42 H42B 109.2 . . ? N28 C42 H42B 109.2 . . ? H42A C42 H42B 107.9 . . ? C1 N1 C41 122.9(5) . . ? C1 N1 C2 111.5(5) . . ? C41 N1 C2 122.9(5) . . ? C1 N2 C3 113.0(5) . . ? C1 N2 C5 123.7(5) . . ? C3 N2 C5 123.3(5) . . ? C4 N3 C42 122.2(5) . . ? C4 N3 C2 110.8(5) . . ? C42 N3 C2 124.0(5) . . ? C4 N4 C3 112.4(5) . . ? C4 N4 C6 122.6(5) . . ? C3 N4 C6 123.9(5) . . ? C7 N5 C8 112.7(5) . . ? C7 N5 C5 123.3(5) . . ? C8 N5 C5 123.6(5) . . ? C7 N6 C9 112.2(5) . . ? C7 N6 C11 121.6(5) . . ? C9 N6 C11 122.2(5) . . ? C10 N7 C6 123.7(5) . . ? C10 N7 C8 112.0(5) . . ? C6 N7 C8 123.7(5) . . ? C10 N8 C12 123.9(5) . . ? C10 N8 C9 112.1(5) . . ? C12 N8 C9 123.0(5) . . ? C13 N9 C11 123.4(5) . . ? C13 N9 C14 111.8(5) . . ? C11 N9 C14 121.8(5) . . ? C13 N10 C15 113.4(5) . . ? C13 N10 C17 122.0(5) . . ? C15 N10 C17 122.8(5) . . ? C16 N11 C12 122.7(5) . . ? C16 N11 C14 112.1(5) . . ? C12 N11 C14 123.2(5) . . ? C16 N12 C15 112.3(5) . . ? C16 N12 C18 121.9(5) . . ? C15 N12 C18 122.6(5) . . ? C19 N13 C20 111.8(5) . . ? C19 N13 C17 122.4(5) . . ? C20 N13 C17 122.9(5) . . ? C19 N14 C23 123.6(5) . . ? C19 N14 C21 111.6(5) . . ? C23 N14 C21 122.5(5) . . ? C22 N15 C18 121.3(5) . . ? C22 N15 C20 112.2(5) . . ? C18 N15 C20 124.8(5) . . ? C22 N16 C24 122.4(5) . . ? C22 N16 C21 112.8(5) . . ? C24 N16 C21 123.3(5) . . ? C25 N17 C26 112.3(5) . . ? C25 N17 C23 124.6(5) . . ? C26 N17 C23 122.4(5) . . ? C25 N18 C29 124.8(5) . . ? C25 N18 C27 112.8(5) . . ? C29 N18 C27 121.8(5) . . ? C28 N19 C24 122.0(5) . . ? C28 N19 C26 112.1(5) . . ? C24 N19 C26 122.5(5) . . ? C28 N20 C30 123.3(5) . . ? C28 N20 C27 112.2(5) . . ? C30 N20 C27 124.0(5) . . ? C31 N21 C29 122.5(5) . . ? C31 N21 C32 112.7(5) . . ? C29 N21 C32 123.5(5) . . ? C31 N22 C33 112.8(5) . . ? C31 N22 C35 121.9(5) . . ? C33 N22 C35 123.0(5) . . ? C34 N23 C30 124.7(5) . . ? C34 N23 C32 112.7(5) . . ? C30 N23 C32 122.5(5) . . ? C34 N24 C33 113.1(5) . . ? C34 N24 C36 122.9(5) . . ? C33 N24 C36 122.1(5) . . ? C37 N25 C35 122.3(5) . . ? C37 N25 C38 111.9(5) . . ? C35 N25 C38 122.4(5) . . ? C37 N26 C41 122.7(5) . . ? C37 N26 C39 112.3(5) . . ? C41 N26 C39 121.4(5) . . ? C40 N27 C38 112.7(5) . . ? C40 N27 C36 122.7(5) . . ? C38 N27 C36 121.3(5) . . ? C40 N28 C42 120.8(5) . . ? C40 N28 C39 111.6(5) . . ? C42 N28 C39 121.4(5) . . ? C1 O1 Nd1 155.2(4) . . ? C7 O2 Nd1 161.7(4) . . ? C25 O5 Nd1 154.7(4) . 2_755 ? C10 O9 Nd2 154.2(4) . 2_866 ? C28 O12 Nd2 160.2(4) . . ? C34 O13 Nd2 155.4(4) . . ? Zn2 Cl5 Zn2' 37.98(16) . . ? Zn2 Cl6 Zn2' 38.40(17) . . ? Zn2' Cl7 Zn2 39.58(17) . . ? Cl4 Zn1 Cl1 109.20(9) . . ? Cl4 Zn1 Cl3 113.06(8) . . ? Cl1 Zn1 Cl3 107.81(9) . . ? Cl4 Zn1 Cl2 109.19(9) . . ? Cl1 Zn1 Cl2 111.57(8) . . ? Cl3 Zn1 Cl2 106.02(9) . . ? Zn2' Zn2 Cl7 66.7(3) . . ? Zn2' Zn2 Cl8 169.7(5) . . ? Cl7 Zn2 Cl8 104.2(5) . . ? Zn2' Zn2 Cl6 71.5(3) . . ? Cl7 Zn2 Cl6 105.2(3) . . ? Cl8 Zn2 Cl6 107.7(5) . . ? Zn2' Zn2 Cl5 73.2(3) . . ? Cl7 Zn2 Cl5 112.8(3) . . ? Cl8 Zn2 Cl5 116.0(5) . . ? Cl6 Zn2 Cl5 110.1(2) . . ? Zn2 Zn2' Cl7 73.7(3) . . ? Zn2 Zn2' Cl8' 163.3(5) . . ? Cl7 Zn2' Cl8' 90.0(4) . . ? Zn2 Zn2' Cl6 70.1(2) . . ? Cl7 Zn2' Cl6 107.8(3) . . ? Cl8' Zn2' Cl6 120.0(4) . . ? Zn2 Zn2' Cl5 68.9(2) . . ? Cl7 Zn2' Cl5 114.3(3) . . ? Cl8' Zn2' Cl5 116.3(4) . . ? Cl6 Zn2' Cl5 107.3(2) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.006 _refine_diff_density_min -2.759 _refine_diff_density_rms 0.176 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.035 0.500 1.000 1168 413 ' ' 2 0.230 0.290 0.276 113 45 ' ' 3 0.770 0.710 0.723 113 46 ' ' _platon_squeeze_details ; ; data_p7 _database_code_depnum_ccdc_archive 'CCDC 905588' #TrackingRef '5 (905588).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H55 Cl5 N14 O24 Sm Zn' _chemical_formula_weight 1280.76 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.2615(14) _cell_length_b 18.7064(11) _cell_length_c 20.1780(11) _cell_angle_alpha 90.00 _cell_angle_beta 105.513(2) _cell_angle_gamma 90.00 _cell_volume 9551.5(9) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.781 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5184 _exptl_absorpt_coefficient_mu 2.092 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6123 _exptl_absorpt_correction_T_max 0.6677 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42961 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9250 _reflns_number_gt 7603 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0953P)^2^+53.1290P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9250 _refine_ls_number_parameters 506 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1647 _refine_ls_wR_factor_gt 0.1591 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.187 _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 Cl6 Cl 0.27524(9) -0.22711(13) 0.35703(13) 0.0863(7) Uani 1 1 d . . . Zn1 Zn 0.36025(4) 0.04254(6) 0.32058(6) 0.0580(4) Uani 0.6666(18) 1 d PD A 1 Zn1' Zn 0.36481(10) 0.04729(12) 0.26701(16) 0.0626(8) Uani 0.3334(18) 1 d P A 2 Cl1 Cl 0.32679(6) 0.15231(8) 0.29700(8) 0.0500(4) Uani 1 1 d . . . Cl2 Cl 0.31245(7) -0.03376(9) 0.24005(11) 0.0825(6) Uani 1 1 d D . . Cl3 Cl 0.44732(7) 0.04342(17) 0.3295(2) 0.1648(14) Uani 1 1 d DU . . Cl4 Cl 0.3462(2) 0.0112(3) 0.42260(16) 0.168(2) Uani 0.6666(18) 1 d PDU . . Cl4' Cl 0.4008(3) 0.0541(3) 0.1725(5) 0.111(2) Uani 0.3334(18) 1 d P . . O1W O -0.01909(15) 0.2035(2) 0.49480(18) 0.0456(10) Uani 1 1 d . . . O2W O 0.03406(16) 0.1335(2) 0.40200(19) 0.0428(10) Uani 1 1 d . . . O3W O 0.11239(16) 0.1011(2) 0.52193(18) 0.0425(9) Uani 1 1 d . . . O4W O 0.15510(16) 0.2592(3) 0.5662(2) 0.0530(11) Uani 1 1 d . . . O5W O 0.05612(19) 0.3346(2) 0.5389(2) 0.0546(12) Uani 1 1 d . . . Sm1 Sm 0.071198(9) 0.215647(13) 0.495559(11) 0.02493(7) Uani 1 1 d . . . C1 C 0.14449(18) 0.2261(2) 0.3734(2) 0.0247(10) Uani 1 1 d . . . C2 C 0.18299(18) 0.2070(2) 0.2836(2) 0.0246(10) Uani 1 1 d . . . H2 H 0.2213 0.2130 0.2889 0.030 Uiso 1 1 calc R . . C3 C 0.15338(18) 0.2793(2) 0.2731(2) 0.0239(10) Uani 1 1 d . . . H3 H 0.1771 0.3196 0.2702 0.029 Uiso 1 1 calc R . . C4 C 0.11893(19) 0.2051(3) 0.1787(2) 0.0274(11) Uani 1 1 d . . . C5 C 0.10879(18) 0.3474(2) 0.3511(2) 0.0259(10) Uani 1 1 d . . . H5A H 0.1261 0.3894 0.3379 0.031 Uiso 1 1 calc R . . H5B H 0.1148 0.3486 0.4011 0.031 Uiso 1 1 calc R . . C6 C -0.08082(18) 0.3259(3) 0.3273(2) 0.0280(11) Uani 1 1 d . . . H6A H -0.0710 0.3154 0.3767 0.034 Uiso 1 1 calc R . . H6B H -0.1019 0.3698 0.3201 0.034 Uiso 1 1 calc R . . C7 C 0.01517(18) 0.3225(2) 0.3458(2) 0.0246(10) Uani 1 1 d . . . C8 C -0.02975(18) 0.3827(2) 0.2476(2) 0.0267(10) Uani 1 1 d . . . H8 H -0.0431 0.4316 0.2513 0.032 Uiso 1 1 calc R . . C9 C 0.1833(2) 0.1077(3) 0.1991(2) 0.0306(11) Uani 1 1 d . . . H9A H 0.2209 0.1185 0.2071 0.037 Uiso 1 1 calc R . . H9B H 0.1682 0.1018 0.1495 0.037 Uiso 1 1 calc R . . C10 C 0.20261(19) 0.1218(2) 0.3855(2) 0.0283(11) Uani 1 1 d . . . H10A H 0.2401 0.1299 0.3890 0.034 Uiso 1 1 calc R . . H10B H 0.1982 0.1226 0.4322 0.034 Uiso 1 1 calc R . . C11 C 0.1593(2) -0.0186(3) 0.1951(3) 0.0346(12) Uani 1 1 d . . . C12 C 0.20841(18) 0.0247(3) 0.3019(2) 0.0258(10) Uani 1 1 d . . . H12 H 0.2461 0.0374 0.3088 0.031 Uiso 1 1 calc R . . C13 C 0.20094(18) -0.0575(3) 0.3066(2) 0.0269(10) Uani 1 1 d . . . H13 H 0.2352 -0.0828 0.3222 0.032 Uiso 1 1 calc R . . C14 C 0.16675(19) 0.0004(3) 0.3875(2) 0.0288(11) Uani 1 1 d . . . C15 C 0.16843(18) -0.1498(2) 0.2118(2) 0.0273(10) Uani 1 1 d . . . H15A H 0.1654 -0.1491 0.1624 0.033 Uiso 1 1 calc R . . H15B H 0.2007 -0.1760 0.2345 0.033 Uiso 1 1 calc R . . C16 C 0.16083(19) -0.1305(3) 0.3857(2) 0.0285(11) Uani 1 1 d . . . H16A H 0.1530 -0.1218 0.4299 0.034 Uiso 1 1 calc R . . H16B H 0.1932 -0.1592 0.3947 0.034 Uiso 1 1 calc R . . C17 C 0.07933(18) -0.2056(2) 0.1735(2) 0.0249(10) Uani 1 1 d . . . C18 C 0.12507(18) -0.2203(2) 0.2897(2) 0.0237(10) Uani 1 1 d . . . H18 H 0.1571 -0.2500 0.3068 0.028 Uiso 1 1 calc R . . C19 C 0.07387(18) -0.2658(2) 0.2734(2) 0.0249(10) Uani 1 1 d . . . H19 H 0.0816 -0.3176 0.2795 0.030 Uiso 1 1 calc R . . C20 C 0.07307(19) -0.1844(3) 0.3604(2) 0.0278(10) Uani 1 1 d . . . C21 C -0.00200(18) -0.2756(2) 0.1638(2) 0.0261(10) Uani 1 1 d . . . H21A H -0.0051 -0.2715 0.1144 0.031 Uiso 1 1 calc R . . H21B H -0.0037 -0.3265 0.1745 0.031 Uiso 1 1 calc R . . N1 N 0.17201(15) 0.1796(2) 0.34621(18) 0.0257(9) Uani 1 1 d . . . N2 N 0.13316(16) 0.2846(2) 0.3332(2) 0.0286(9) Uani 1 1 d . . . N3 N 0.15769(15) 0.1670(2) 0.22251(19) 0.0277(9) Uani 1 1 d . . . N4 N 0.11280(15) 0.2683(2) 0.20850(19) 0.0265(9) Uani 1 1 d . . . N5 N 0.05279(15) 0.3523(2) 0.31931(19) 0.0260(8) Uani 1 1 d . . . N6 N -0.03299(14) 0.3382(2) 0.30571(19) 0.0254(8) Uani 1 1 d . . . N7 N 0.17764(16) 0.0415(2) 0.2334(2) 0.0294(9) Uani 1 1 d . . . N8 N 0.17294(16) -0.0768(2) 0.23738(19) 0.0285(9) Uani 1 1 d . . . N9 N 0.18794(16) 0.0526(2) 0.35620(19) 0.0277(9) Uani 1 1 d . . . N10 N 0.17004(16) -0.0628(2) 0.35652(19) 0.0289(9) Uani 1 1 d . . . N11 N 0.12329(15) -0.1871(2) 0.22355(19) 0.0260(9) Uani 1 1 d . . . N12 N 0.04880(14) -0.2478(2) 0.20162(18) 0.0250(9) Uani 1 1 d . . . N13 N 0.11758(15) -0.1711(2) 0.34167(19) 0.0272(9) Uani 1 1 d . . . N14 N 0.04625(15) -0.2394(2) 0.32133(19) 0.0247(8) Uani 1 1 d . . . O1 O 0.13273(14) 0.21753(18) 0.42863(17) 0.0330(8) Uani 1 1 d . . . O2 O 0.02490(13) 0.28877(17) 0.40124(17) 0.0295(8) Uani 1 1 d . . . O3 O 0.09397(15) 0.1847(2) 0.12179(18) 0.0384(9) Uani 1 1 d . . . O4 O 0.13551(19) -0.0200(2) 0.13417(19) 0.0499(11) Uani 1 1 d . . . O5 O 0.06986(13) -0.18680(19) 0.11259(15) 0.0295(8) Uani 1 1 d . . . O6 O 0.05853(14) -0.1530(2) 0.40611(17) 0.0364(8) Uani 1 1 d . . . O7 O 0.14804(16) 0.0085(2) 0.43731(18) 0.0426(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl6 0.0741(11) 0.1005(15) 0.0910(14) -0.0025(11) 0.0338(11) 0.0333(11) Zn1 0.0520(6) 0.0451(6) 0.0712(8) -0.0179(5) 0.0063(6) 0.0058(5) Zn1' 0.0680(14) 0.0371(12) 0.0897(19) -0.0127(11) 0.0334(13) -0.0017(10) Cl1 0.0538(8) 0.0365(7) 0.0646(9) -0.0073(6) 0.0244(7) -0.0073(6) Cl2 0.0865(12) 0.0520(9) 0.1223(15) -0.0337(10) 0.0511(11) -0.0025(9) Cl3 0.0808(16) 0.1126(18) 0.280(3) -0.091(2) 0.012(2) 0.0078(14) Cl4 0.210(4) 0.171(4) 0.112(3) 0.035(3) 0.025(3) 0.046(3) Cl4' 0.162(5) 0.048(3) 0.162(6) -0.016(3) 0.112(5) -0.023(3) O1W 0.0340(19) 0.082(3) 0.0205(17) 0.0013(17) 0.0070(15) -0.0158(18) O2W 0.059(2) 0.036(2) 0.0276(19) -0.0034(15) 0.0028(17) -0.0088(17) O3W 0.068(2) 0.039(2) 0.0234(17) 0.0067(15) 0.0178(16) 0.0120(18) O4W 0.045(2) 0.080(3) 0.033(2) -0.019(2) 0.0073(17) -0.018(2) O5W 0.084(3) 0.042(2) 0.035(2) -0.0130(17) 0.010(2) 0.004(2) Sm1 0.03058(13) 0.03081(14) 0.01439(12) -0.00042(8) 0.00774(9) -0.00388(9) C1 0.023(2) 0.032(2) 0.019(2) -0.0004(17) 0.0048(17) -0.0022(18) C2 0.024(2) 0.031(2) 0.019(2) 0.0001(17) 0.0075(17) -0.0027(18) C3 0.025(2) 0.029(2) 0.019(2) 0.0024(16) 0.0089(17) -0.0004(17) C4 0.027(2) 0.035(2) 0.020(2) 0.0052(18) 0.0053(18) -0.0005(19) C5 0.031(2) 0.026(2) 0.021(2) -0.0033(17) 0.0059(18) -0.0021(18) C6 0.026(2) 0.038(3) 0.020(2) -0.0055(18) 0.0064(17) -0.0002(19) C7 0.033(2) 0.022(2) 0.022(2) -0.0029(17) 0.0128(17) 0.0020(18) C8 0.037(2) 0.024(2) 0.021(2) 0.0002(17) 0.0103(18) 0.0070(19) C9 0.039(2) 0.035(3) 0.021(2) 0.0008(19) 0.0132(19) 0.000(2) C10 0.035(2) 0.029(2) 0.019(2) -0.0002(18) 0.0031(18) -0.0007(19) C11 0.049(3) 0.030(2) 0.029(2) -0.0056(19) 0.017(2) -0.001(2) C12 0.025(2) 0.033(2) 0.021(2) -0.0016(18) 0.0087(17) -0.0004(18) C13 0.028(2) 0.032(2) 0.022(2) 0.0000(18) 0.0084(18) -0.0007(19) C14 0.031(2) 0.038(3) 0.018(2) 0.0009(18) 0.0065(18) -0.002(2) C15 0.032(2) 0.032(2) 0.023(2) -0.0055(18) 0.0168(17) -0.0069(19) C16 0.036(2) 0.036(3) 0.012(2) -0.0020(18) 0.0039(18) -0.005(2) C17 0.030(2) 0.026(2) 0.022(2) 0.0003(17) 0.0123(18) 0.0043(18) C18 0.025(2) 0.031(2) 0.015(2) 0.0026(16) 0.0055(17) 0.0024(17) C19 0.029(2) 0.025(2) 0.022(2) 0.0019(17) 0.0080(18) 0.0011(18) C20 0.034(2) 0.030(2) 0.020(2) 0.0044(18) 0.0096(18) 0.0003(19) C21 0.030(2) 0.032(2) 0.016(2) -0.0056(17) 0.0064(18) -0.0013(18) N1 0.0295(19) 0.031(2) 0.0154(17) -0.0011(15) 0.0048(15) -0.0003(16) N2 0.035(2) 0.035(2) 0.0197(19) -0.0009(15) 0.0136(16) -0.0003(16) N3 0.034(2) 0.0282(19) 0.0214(19) -0.0033(15) 0.0083(16) -0.0018(16) N4 0.0292(19) 0.031(2) 0.0185(18) 0.0008(15) 0.0059(15) -0.0003(16) N5 0.0301(19) 0.0270(19) 0.0228(18) 0.0004(15) 0.0102(15) -0.0023(16) N6 0.0291(18) 0.0273(19) 0.0225(18) -0.0003(15) 0.0118(15) -0.0006(15) N7 0.038(2) 0.0264(19) 0.024(2) -0.0033(15) 0.0079(16) -0.0009(16) N8 0.038(2) 0.030(2) 0.0187(18) -0.0010(15) 0.0103(16) -0.0053(17) N9 0.035(2) 0.029(2) 0.0196(18) -0.0025(15) 0.0086(15) -0.0025(16) N10 0.037(2) 0.032(2) 0.0202(18) -0.0007(15) 0.0115(16) -0.0038(17) N11 0.0325(19) 0.0289(19) 0.0194(18) 0.0007(15) 0.0115(15) -0.0028(16) N12 0.0247(18) 0.035(2) 0.0141(17) 0.0004(15) 0.0038(14) -0.0035(16) N13 0.0305(19) 0.034(2) 0.0177(18) -0.0042(15) 0.0083(15) -0.0057(16) N14 0.0256(18) 0.0316(19) 0.0172(18) -0.0023(15) 0.0062(15) -0.0054(16) O1 0.0377(18) 0.042(2) 0.0229(17) 0.0038(13) 0.0136(14) -0.0013(14) O2 0.0315(17) 0.0376(18) 0.0187(16) 0.0052(13) 0.0055(13) -0.0005(14) O3 0.046(2) 0.044(2) 0.0213(17) -0.0057(15) 0.0025(15) 0.0026(17) O4 0.085(3) 0.036(2) 0.0195(18) -0.0024(15) -0.0026(19) 0.000(2) O5 0.0334(17) 0.0407(18) 0.0141(15) 0.0018(13) 0.0057(13) 0.0003(15) O6 0.0453(18) 0.045(2) 0.0252(16) -0.0071(14) 0.0198(14) -0.0061(16) O7 0.066(2) 0.040(2) 0.0301(18) -0.0067(15) 0.0277(16) -0.0052(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 Cl1 2.2343(18) . ? Zn1 Cl3 2.2450(17) . ? Zn1 Cl4 2.264(2) . ? Zn1 Cl2 2.2720(16) . ? Zn1' Cl2 2.021(3) . ? Zn1' Cl3 2.198(4) . ? Zn1' Cl4' 2.347(8) . ? Zn1' Cl1 2.355(3) . ? O1W Sm1 2.378(4) . ? O2W Sm1 2.427(4) . ? O3W Sm1 2.395(4) . ? O4W Sm1 2.423(4) . ? O5W Sm1 2.461(4) . ? Sm1 O1 2.367(4) . ? Sm1 O2 2.395(3) . ? Sm1 O5 2.432(3) 6_556 ? C1 O1 1.243(6) . ? C1 N1 1.339(6) . ? C1 N2 1.349(6) . ? C2 N3 1.442(6) . ? C2 N1 1.462(6) . ? C2 C3 1.547(6) . ? C2 H2 0.9900 . ? C3 N2 1.451(6) . ? C3 N4 1.461(6) . ? C3 H3 0.9900 . ? C4 O3 1.221(6) . ? C4 N4 1.355(6) . ? C4 N3 1.358(6) . ? C5 N2 1.428(6) . ? C5 N5 1.441(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.436(6) 2 ? C6 N6 1.454(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.249(5) . ? C7 N6 1.339(6) . ? C7 N5 1.362(6) . ? C8 N5 1.440(6) 2 ? C8 N6 1.460(6) . ? C8 C8 1.539(9) 2 ? C8 H8 0.9900 . ? C9 N3 1.440(6) . ? C9 N7 1.445(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 N9 1.432(6) . ? C10 N1 1.450(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 O4 1.222(6) . ? C11 N8 1.371(6) . ? C11 N7 1.376(6) . ? C12 N7 1.438(6) . ? C12 N9 1.442(6) . ? C12 C13 1.556(7) . ? C12 H12 0.9900 . ? C13 N8 1.440(6) . ? C13 N10 1.456(6) . ? C13 H13 0.9900 . ? C14 O7 1.241(6) . ? C14 N10 1.351(6) . ? C14 N9 1.361(6) . ? C15 N11 1.448(6) . ? C15 N8 1.452(6) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 N10 1.444(6) . ? C16 N13 1.455(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 O5 1.239(5) . ? C17 N12 1.353(6) . ? C17 N11 1.359(6) . ? C18 N13 1.446(6) . ? C18 N11 1.461(6) . ? C18 C19 1.551(6) . ? C18 H18 0.9900 . ? C19 N14 1.443(6) . ? C19 N12 1.461(6) . ? C19 H19 0.9900 . ? C20 O6 1.236(6) . ? C20 N13 1.345(6) . ? C20 N14 1.372(6) . ? C21 N14 1.444(6) 2 ? C21 N12 1.446(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? N4 C6 1.436(6) 2 ? N5 C8 1.440(6) 2 ? N14 C21 1.444(6) 2 ? O5 Sm1 2.432(3) 6 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Zn1 Cl3 110.15(11) . . ? Cl1 Zn1 Cl4 106.31(17) . . ? Cl3 Zn1 Cl4 109.84(19) . . ? Cl1 Zn1 Cl2 108.32(8) . . ? Cl3 Zn1 Cl2 114.73(11) . . ? Cl4 Zn1 Cl2 107.12(16) . . ? Cl2 Zn1' Cl3 128.70(16) . . ? Cl2 Zn1' Cl4' 102.4(2) . . ? Cl3 Zn1' Cl4' 85.4(3) . . ? Cl2 Zn1' Cl1 112.96(13) . . ? Cl3 Zn1' Cl1 107.50(14) . . ? Cl4' Zn1' Cl1 117.0(2) . . ? Zn1 Cl1 Zn1' 28.16(8) . . ? Zn1' Cl2 Zn1 29.58(9) . . ? Zn1' Cl3 Zn1 29.24(8) . . ? O1 Sm1 O1W 146.03(12) . . ? O1 Sm1 O2 79.46(12) . . ? O1W Sm1 O2 75.87(13) . . ? O1 Sm1 O3W 78.66(12) . . ? O1W Sm1 O3W 107.84(15) . . ? O2 Sm1 O3W 142.26(12) . . ? O1 Sm1 O4W 71.25(13) . . ? O1W Sm1 O4W 141.65(14) . . ? O2 Sm1 O4W 117.65(14) . . ? O3W Sm1 O4W 83.36(15) . . ? O1 Sm1 O2W 76.07(13) . . ? O1W Sm1 O2W 75.04(14) . . ? O2 Sm1 O2W 74.35(12) . . ? O3W Sm1 O2W 70.76(13) . . ? O4W Sm1 O2W 141.58(15) . . ? O1 Sm1 O5 138.30(11) . 6_556 ? O1W Sm1 O5 73.25(12) . 6_556 ? O2 Sm1 O5 139.68(12) . 6_556 ? O3W Sm1 O5 73.06(12) . 6_556 ? O4W Sm1 O5 75.54(13) . 6_556 ? O2W Sm1 O5 120.52(12) . 6_556 ? O1 Sm1 O5W 112.87(14) . . ? O1W Sm1 O5W 80.43(16) . . ? O2 Sm1 O5W 70.75(13) . . ? O3W Sm1 O5W 146.69(13) . . ? O4W Sm1 O5W 72.20(16) . . ? O2W Sm1 O5W 141.19(14) . . ? O5 Sm1 O5W 79.05(13) 6_556 . ? O1 C1 N1 125.1(4) . . ? O1 C1 N2 125.1(4) . . ? N1 C1 N2 109.7(4) . . ? N3 C2 N1 113.9(4) . . ? N3 C2 C3 103.7(4) . . ? N1 C2 C3 102.5(4) . . ? N3 C2 H2 112.0 . . ? N1 C2 H2 112.0 . . ? C3 C2 H2 112.0 . . ? N2 C3 N4 114.4(4) . . ? N2 C3 C2 103.3(3) . . ? N4 C3 C2 102.6(3) . . ? N2 C3 H3 112.0 . . ? N4 C3 H3 112.0 . . ? C2 C3 H3 112.0 . . ? O3 C4 N4 126.3(4) . . ? O3 C4 N3 124.6(5) . . ? N4 C4 N3 109.0(4) . . ? N2 C5 N5 114.4(4) . . ? N2 C5 H5A 108.7 . . ? N5 C5 H5A 108.7 . . ? N2 C5 H5B 108.7 . . ? N5 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? N4 C6 N6 113.8(4) 2 . ? N4 C6 H6A 108.8 2 . ? N6 C6 H6A 108.8 . . ? N4 C6 H6B 108.8 2 . ? N6 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N6 125.9(4) . . ? O2 C7 N5 124.2(4) . . ? N6 C7 N5 109.9(4) . . ? N5 C8 N6 115.3(4) 2 . ? N5 C8 C8 103.0(4) 2 2 ? N6 C8 C8 103.0(4) . 2 ? N5 C8 H8 111.6 2 . ? N6 C8 H8 111.6 . . ? C8 C8 H8 111.6 2 . ? N3 C9 N7 112.8(4) . . ? N3 C9 H9A 109.0 . . ? N7 C9 H9A 109.0 . . ? N3 C9 H9B 109.0 . . ? N7 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? N9 C10 N1 113.5(4) . . ? N9 C10 H10A 108.9 . . ? N1 C10 H10A 108.9 . . ? N9 C10 H10B 108.9 . . ? N1 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? O4 C11 N8 126.0(5) . . ? O4 C11 N7 126.1(5) . . ? N8 C11 N7 107.9(4) . . ? N7 C12 N9 115.1(4) . . ? N7 C12 C13 103.2(4) . . ? N9 C12 C13 103.5(4) . . ? N7 C12 H12 111.5 . . ? N9 C12 H12 111.5 . . ? C13 C12 H12 111.5 . . ? N8 C13 N10 114.8(4) . . ? N8 C13 C12 103.2(4) . . ? N10 C13 C12 102.3(4) . . ? N8 C13 H13 111.9 . . ? N10 C13 H13 111.9 . . ? C12 C13 H13 111.9 . . ? O7 C14 N10 124.8(5) . . ? O7 C14 N9 125.9(5) . . ? N10 C14 N9 109.3(4) . . ? N11 C15 N8 112.8(4) . . ? N11 C15 H15A 109.0 . . ? N8 C15 H15A 109.0 . . ? N11 C15 H15B 109.0 . . ? N8 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? N10 C16 N13 113.4(4) . . ? N10 C16 H16A 108.9 . . ? N13 C16 H16A 108.9 . . ? N10 C16 H16B 108.9 . . ? N13 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? O5 C17 N12 126.7(4) . . ? O5 C17 N11 124.8(4) . . ? N12 C17 N11 108.5(4) . . ? N13 C18 N11 114.6(4) . . ? N13 C18 C19 103.0(4) . . ? N11 C18 C19 103.0(3) . . ? N13 C18 H18 111.9 . . ? N11 C18 H18 111.9 . . ? C19 C18 H18 111.9 . . ? N14 C19 N12 114.3(4) . . ? N14 C19 C18 103.4(4) . . ? N12 C19 C18 102.6(3) . . ? N14 C19 H19 111.9 . . ? N12 C19 H19 111.9 . . ? C18 C19 H19 111.9 . . ? O6 C20 N13 126.0(4) . . ? O6 C20 N14 124.9(4) . . ? N13 C20 N14 109.1(4) . . ? N14 C21 N12 113.7(4) 2 . ? N14 C21 H21A 108.8 2 . ? N12 C21 H21A 108.8 . . ? N14 C21 H21B 108.8 2 . ? N12 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C1 N1 C10 122.7(4) . . ? C1 N1 C2 112.3(4) . . ? C10 N1 C2 121.7(4) . . ? C1 N2 C5 123.9(4) . . ? C1 N2 C3 112.0(4) . . ? C5 N2 C3 123.8(4) . . ? C4 N3 C9 121.7(4) . . ? C4 N3 C2 112.2(4) . . ? C9 N3 C2 122.0(4) . . ? C4 N4 C6 123.6(4) . 2 ? C4 N4 C3 112.0(4) . . ? C6 N4 C3 122.1(4) 2 . ? C7 N5 C8 111.3(4) . 2 ? C7 N5 C5 124.1(4) . . ? C8 N5 C5 124.4(4) 2 . ? C7 N6 C6 122.4(4) . . ? C7 N6 C8 111.2(4) . . ? C6 N6 C8 124.9(4) . . ? C11 N7 C12 112.5(4) . . ? C11 N7 C9 119.9(4) . . ? C12 N7 C9 123.0(4) . . ? C11 N8 C13 112.6(4) . . ? C11 N8 C15 122.9(4) . . ? C13 N8 C15 123.5(4) . . ? C14 N9 C10 123.8(4) . . ? C14 N9 C12 111.9(4) . . ? C10 N9 C12 121.9(4) . . ? C14 N10 C16 122.7(4) . . ? C14 N10 C13 112.1(4) . . ? C16 N10 C13 121.8(4) . . ? C17 N11 C15 124.8(4) . . ? C17 N11 C18 112.6(4) . . ? C15 N11 C18 121.7(4) . . ? C17 N12 C21 123.7(4) . . ? C17 N12 C19 112.9(4) . . ? C21 N12 C19 123.2(4) . . ? C20 N13 C18 112.6(4) . . ? C20 N13 C16 121.3(4) . . ? C18 N13 C16 122.6(4) . . ? C20 N14 C19 111.7(4) . . ? C20 N14 C21 123.4(4) . 2 ? C19 N14 C21 123.8(4) . 2 ? C1 O1 Sm1 152.1(3) . . ? C7 O2 Sm1 159.8(3) . . ? C17 O5 Sm1 148.2(3) . 6 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.117 _refine_diff_density_min -2.001 _refine_diff_density_rms 0.171 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.005 479 130 ' ' 2 0.326 0.119 0.000 995 346 ' ' 3 0.305 -0.145 0.500 995 346 ' ' 4 0.500 0.500 0.779 478 130 ' ' _platon_squeeze_details ; ; data_p8 _database_code_depnum_ccdc_archive 'CCDC 905589' #TrackingRef '6 (905589).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H58 Cl5 Gd N14 O25.50 Zn' _chemical_formula_weight 1314.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.6201(19) _cell_length_b 18.9954(14) _cell_length_c 20.0385(15) _cell_angle_alpha 90.00 _cell_angle_beta 104.030(2) _cell_angle_gamma 90.00 _cell_volume 9830.4(12) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.777 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5320 _exptl_absorpt_coefficient_mu 2.192 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5316 _exptl_absorpt_correction_T_max 0.5891 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43314 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9494 _reflns_number_gt 7860 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0811P)^2^+7.7670P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9494 _refine_ls_number_parameters 497 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0515 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1297 _refine_ls_wR_factor_gt 0.1244 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl5 Cl 0.22426(9) 0.21664(10) 0.14622(12) 0.0850(6) Uani 1 1 d . . . Zn1 Zn 0.36548(3) 0.44707(5) 0.30998(8) 0.0475(5) Uani 0.840(6) 1 d P A 1 Zn1' Zn 0.3615(4) 0.4446(5) 0.2600(12) 0.124(6) Uani 0.160(6) 1 d P A 2 Cl1 Cl 0.32328(5) 0.34370(6) 0.29530(7) 0.0464(3) Uani 1 1 d . . . Cl2 Cl 0.31812(7) 0.53489(8) 0.24963(11) 0.0746(5) Uani 1 1 d . . . Cl3 Cl 0.44048(6) 0.43943(8) 0.27668(13) 0.0826(6) Uani 1 1 d . . . Cl4 Cl 0.38413(12) 0.46924(14) 0.42488(13) 0.1229(10) Uani 1 1 d . . . O1W O 0.15159(13) 0.2403(2) 0.56328(18) 0.0492(9) Uani 1 1 d . . . O2W O -0.01563(13) 0.3018(2) 0.49528(17) 0.0444(8) Uani 1 1 d . . . O3W O 0.03808(14) 0.36766(17) 0.40129(16) 0.0445(8) Uani 1 1 d . . . O4W O 0.11380(14) 0.39697(17) 0.51990(16) 0.0414(8) Uani 1 1 d . . . O5W O 0.05495(15) 0.17380(17) 0.53968(18) 0.0486(9) Uani 1 1 d . . . Gd1 Gd 0.071905(8) 0.287267(10) 0.494213(9) 0.02480(9) Uani 1 1 d . . . C1 C 0.01584(16) 0.18256(19) 0.3469(2) 0.0240(8) Uani 1 1 d . . . C2 C 0.02952(16) 0.1228(2) 0.2512(2) 0.0257(9) Uani 1 1 d . . . H2 H 0.0426 0.0747 0.2468 0.031 Uiso 1 1 calc R . . C3 C 0.10664(15) 0.1555(2) 0.3480(2) 0.0259(9) Uani 1 1 d . . . H3A H 0.1230 0.1136 0.3340 0.031 Uiso 1 1 calc R . . H3B H 0.1121 0.1540 0.3981 0.031 Uiso 1 1 calc R . . C4 C 0.07871(16) 0.1788(2) 0.1691(2) 0.0275(9) Uani 1 1 d . . . H4A H 0.0987 0.1350 0.1743 0.033 Uiso 1 1 calc R . . H4B H 0.0691 0.1905 0.1200 0.033 Uiso 1 1 calc R . . C5 C 0.14395(15) 0.2743(2) 0.3705(2) 0.0240(8) Uani 1 1 d . . . C6 C 0.15112(16) 0.2229(2) 0.2682(2) 0.0237(8) Uani 1 1 d . . . H6 H 0.1737 0.1827 0.2639 0.028 Uiso 1 1 calc R . . C7 C 0.18096(16) 0.2929(2) 0.2779(2) 0.0244(8) Uani 1 1 d . . . H7 H 0.2184 0.2858 0.2816 0.029 Uiso 1 1 calc R . . C8 C 0.11780(17) 0.2971(2) 0.1747(2) 0.0282(9) Uani 1 1 d . . . C9 C 0.20160(17) 0.3771(2) 0.3798(2) 0.0297(9) Uani 1 1 d . . . H9A H 0.1974 0.3765 0.4271 0.036 Uiso 1 1 calc R . . H9B H 0.2383 0.3690 0.3818 0.036 Uiso 1 1 calc R . . C10 C 0.18291(19) 0.3913(2) 0.1939(2) 0.0334(10) Uani 1 1 d . . . H10A H 0.2199 0.3802 0.2022 0.040 Uiso 1 1 calc R . . H10B H 0.1692 0.3964 0.1442 0.040 Uiso 1 1 calc R . . C11 C 0.16456(16) 0.4957(2) 0.3821(2) 0.0288(9) Uani 1 1 d . . . C12 C 0.20733(17) 0.4747(2) 0.2958(2) 0.0278(9) Uani 1 1 d . . . H12 H 0.2445 0.4634 0.3017 0.033 Uiso 1 1 calc R . . C13 C 0.19854(17) 0.5546(2) 0.3007(2) 0.0304(9) Uani 1 1 d . . . H13 H 0.2315 0.5807 0.3160 0.036 Uiso 1 1 calc R . . C14 C 0.15952(19) 0.5161(2) 0.1899(2) 0.0368(10) Uani 1 1 d . . . C15 C 0.15705(17) 0.6247(2) 0.3816(2) 0.0301(9) Uani 1 1 d . . . H15A H 0.1489 0.6149 0.4258 0.036 Uiso 1 1 calc R . . H15B H 0.1885 0.6536 0.3907 0.036 Uiso 1 1 calc R . . C16 C 0.16560(17) 0.6452(2) 0.2064(2) 0.0287(9) Uani 1 1 d . . . H16A H 0.1972 0.6715 0.2274 0.034 Uiso 1 1 calc R . . H16B H 0.1620 0.6446 0.1566 0.034 Uiso 1 1 calc R . . C17 C 0.07108(16) 0.6781(2) 0.3590(2) 0.0276(9) Uani 1 1 d . . . C18 C 0.12244(17) 0.7140(2) 0.2857(2) 0.0256(9) Uani 1 1 d . . . H18 H 0.1536 0.7435 0.3024 0.031 Uiso 1 1 calc R . . C19 C 0.07245(16) 0.7581(2) 0.2712(2) 0.0253(8) Uani 1 1 d . . . H19 H 0.0800 0.8089 0.2780 0.030 Uiso 1 1 calc R . . C20 C 0.07893(17) 0.6995(2) 0.1710(2) 0.0264(9) Uani 1 1 d . . . C21 C -0.00139(16) 0.7682(2) 0.1633(2) 0.0264(9) Uani 1 1 d . . . H21A H -0.0045 0.7641 0.1138 0.032 Uiso 1 1 calc R . . H21B H -0.0035 0.8183 0.1740 0.032 Uiso 1 1 calc R . . N1 N 0.05238(12) 0.15296(17) 0.31729(16) 0.0236(7) Uani 1 1 d . . . N2 N 0.13177(14) 0.21788(17) 0.32929(18) 0.0266(8) Uani 1 1 d . . . N3 N 0.03175(13) 0.16687(17) 0.19233(17) 0.0247(7) Uani 1 1 d . . . N4 N 0.11134(13) 0.23433(18) 0.20545(17) 0.0270(7) Uani 1 1 d . . . N5 N 0.17129(13) 0.32028(17) 0.34133(17) 0.0251(7) Uani 1 1 d . . . N6 N 0.18721(14) 0.44544(17) 0.35058(17) 0.0269(7) Uani 1 1 d . . . N7 N 0.15685(14) 0.33340(18) 0.21796(17) 0.0288(8) Uani 1 1 d . . . N8 N 0.17713(15) 0.45722(18) 0.22685(18) 0.0312(8) Uani 1 1 d . . . N9 N 0.16724(14) 0.55846(18) 0.35078(17) 0.0297(8) Uani 1 1 d . . . N10 N 0.11470(14) 0.66460(18) 0.33857(17) 0.0283(8) Uani 1 1 d . . . N11 N 0.17121(14) 0.57378(18) 0.23166(18) 0.0299(8) Uani 1 1 d . . . N12 N 0.12197(13) 0.68128(18) 0.22049(17) 0.0262(7) Uani 1 1 d . . . N13 N 0.04476(14) 0.73174(18) 0.31976(17) 0.0264(7) Uani 1 1 d . . . N14 N 0.04856(13) 0.74186(18) 0.19946(16) 0.0270(7) Uani 1 1 d . . . O1 O 0.02565(12) 0.21617(14) 0.40042(15) 0.0304(7) Uani 1 1 d . . . O2 O 0.13315(13) 0.28242(15) 0.42681(16) 0.0326(7) Uani 1 1 d . . . O3 O 0.14541(14) 0.48646(17) 0.43152(17) 0.0434(8) Uani 1 1 d . . . O4 O 0.05666(13) 0.64735(16) 0.40523(16) 0.0371(7) Uani 1 1 d . . . O5 O 0.09345(12) 0.31731(17) 0.11837(15) 0.0384(7) Uani 1 1 d . . . O6 O 0.13584(18) 0.51690(18) 0.12942(16) 0.0579(11) Uani 1 1 d . . . O7 O 0.06929(12) 0.68126(16) 0.11004(14) 0.0322(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl5 0.0975(14) 0.0829(13) 0.0886(14) 0.0089(9) 0.0498(12) 0.0354(10) Zn1 0.0519(5) 0.0294(5) 0.0649(9) 0.0018(4) 0.0216(4) -0.0009(3) Zn1' 0.120(6) 0.090(5) 0.182(17) 0.069(7) 0.072(7) 0.025(4) Cl1 0.0529(7) 0.0330(6) 0.0579(8) 0.0071(5) 0.0227(6) 0.0010(5) Cl2 0.0742(10) 0.0416(8) 0.1233(16) 0.0321(9) 0.0539(10) 0.0121(7) Cl3 0.0637(10) 0.0390(8) 0.1565(19) 0.0009(9) 0.0487(11) -0.0015(7) Cl4 0.164(2) 0.1003(17) 0.0898(16) -0.0297(13) 0.0016(15) 0.0297(16) O1W 0.047(2) 0.067(2) 0.0369(19) 0.0157(17) 0.0159(16) 0.0154(17) O2W 0.0353(17) 0.074(2) 0.0262(17) -0.0064(16) 0.0117(14) 0.0123(16) O3W 0.068(2) 0.0324(18) 0.0295(17) 0.0042(13) 0.0046(15) 0.0072(15) O4W 0.065(2) 0.0354(17) 0.0289(17) -0.0069(13) 0.0219(15) -0.0154(15) O5W 0.071(2) 0.0345(19) 0.0403(19) 0.0101(15) 0.0144(17) -0.0023(16) Gd1 0.03525(14) 0.02536(14) 0.01625(13) -0.00015(7) 0.01100(9) 0.00177(7) C1 0.037(2) 0.0173(19) 0.0198(19) 0.0005(15) 0.0117(16) -0.0020(16) C2 0.038(2) 0.022(2) 0.0184(19) 0.0004(15) 0.0103(16) 0.0019(16) C3 0.036(2) 0.020(2) 0.025(2) 0.0050(15) 0.0129(17) 0.0052(16) C4 0.035(2) 0.033(2) 0.0177(19) -0.0046(16) 0.0129(16) 0.0002(17) C5 0.028(2) 0.025(2) 0.023(2) -0.0003(15) 0.0124(16) 0.0007(15) C6 0.031(2) 0.023(2) 0.020(2) 0.0000(15) 0.0112(16) 0.0024(15) C7 0.030(2) 0.027(2) 0.019(2) 0.0005(15) 0.0118(16) 0.0037(15) C8 0.033(2) 0.031(2) 0.024(2) -0.0029(17) 0.0135(18) 0.0050(17) C9 0.042(2) 0.024(2) 0.022(2) 0.0002(16) 0.0072(17) -0.0026(17) C10 0.053(3) 0.025(2) 0.027(2) -0.0032(17) 0.0174(19) -0.0032(18) C11 0.033(2) 0.033(2) 0.022(2) 0.0039(17) 0.0105(17) 0.0003(17) C12 0.038(2) 0.024(2) 0.024(2) 0.0006(16) 0.0150(17) 0.0004(16) C13 0.040(2) 0.029(2) 0.027(2) 0.0015(17) 0.0162(18) 0.0020(17) C14 0.057(3) 0.027(2) 0.033(2) 0.0068(18) 0.023(2) -0.0001(19) C15 0.045(2) 0.030(2) 0.0172(19) 0.0008(16) 0.0111(17) 0.0077(18) C16 0.040(2) 0.026(2) 0.026(2) 0.0059(17) 0.0195(18) 0.0016(17) C17 0.040(2) 0.023(2) 0.023(2) -0.0023(16) 0.0135(18) 0.0007(17) C18 0.035(2) 0.024(2) 0.020(2) 0.0011(15) 0.0118(17) -0.0020(15) C19 0.036(2) 0.022(2) 0.0205(19) -0.0004(15) 0.0116(16) -0.0023(16) C20 0.041(2) 0.021(2) 0.020(2) 0.0019(15) 0.0141(18) -0.0043(16) C21 0.036(2) 0.025(2) 0.021(2) 0.0021(16) 0.0124(17) -0.0026(16) N1 0.0312(17) 0.0213(17) 0.0206(16) -0.0005(13) 0.0112(13) -0.0007(13) N2 0.0353(19) 0.0268(19) 0.0214(18) 0.0002(13) 0.0139(15) -0.0032(13) N3 0.0295(17) 0.0231(17) 0.0245(17) 0.0011(13) 0.0127(14) -0.0009(13) N4 0.0327(18) 0.0252(17) 0.0249(18) 0.0012(14) 0.0103(14) -0.0027(14) N5 0.0353(18) 0.0233(18) 0.0194(16) -0.0010(13) 0.0122(14) -0.0019(14) N6 0.042(2) 0.0226(17) 0.0201(17) 0.0019(13) 0.0151(15) 0.0020(14) N7 0.041(2) 0.0279(18) 0.0194(17) 0.0023(14) 0.0121(15) 0.0003(15) N8 0.049(2) 0.0264(19) 0.0207(17) 0.0010(14) 0.0124(15) 0.0022(15) N9 0.047(2) 0.0255(18) 0.0234(18) 0.0040(14) 0.0210(16) 0.0058(15) N10 0.042(2) 0.0271(18) 0.0207(17) 0.0068(14) 0.0169(15) 0.0064(15) N11 0.046(2) 0.0217(18) 0.0252(18) 0.0031(14) 0.0161(15) 0.0025(14) N12 0.0385(19) 0.0254(18) 0.0186(16) 0.0000(13) 0.0146(14) -0.0021(14) N13 0.0367(19) 0.0266(17) 0.0195(17) 0.0018(14) 0.0137(14) 0.0048(14) N14 0.0374(19) 0.0288(19) 0.0181(16) 0.0007(14) 0.0130(14) 0.0000(14) O1 0.0398(17) 0.0331(17) 0.0211(15) -0.0053(12) 0.0124(13) -0.0005(12) O2 0.0436(18) 0.0352(17) 0.0236(16) -0.0019(12) 0.0171(13) -0.0015(12) O3 0.071(2) 0.0326(17) 0.0376(18) 0.0087(14) 0.0339(17) 0.0050(15) O4 0.0530(19) 0.0363(17) 0.0301(16) 0.0093(13) 0.0256(14) 0.0076(14) O5 0.0491(19) 0.0397(18) 0.0234(16) 0.0069(13) 0.0029(14) -0.0012(14) O6 0.110(3) 0.0365(19) 0.0195(17) 0.0063(14) 0.0015(18) 0.0031(19) O7 0.0490(18) 0.0333(17) 0.0176(14) 0.0023(12) 0.0143(13) 0.0015(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 Cl1 2.2458(15) . ? Zn1 Cl2 2.257(2) . ? Zn1 Cl3 2.258(2) . ? Zn1 Cl4 2.274(3) . ? Zn1' Cl2 2.049(8) . ? Zn1' Cl3 2.050(9) . ? Zn1' Cl1 2.358(8) . ? O1W Gd1 2.406(3) . ? O2W Gd1 2.352(3) . ? O3W Gd1 2.408(3) . ? O4W Gd1 2.361(3) . ? O5W Gd1 2.425(3) . ? Gd1 O2 2.357(3) . ? Gd1 O1 2.398(3) . ? Gd1 O7 2.414(3) 6_566 ? C1 O1 1.221(5) . ? C1 N3 1.352(5) 2 ? C1 N1 1.376(5) . ? C2 N1 1.435(5) . ? C2 N3 1.460(5) . ? C2 C2 1.560(8) 2 ? C2 H2 0.9900 . ? C3 N1 1.427(5) . ? C3 N2 1.454(5) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 N4 1.446(5) . ? C4 N3 1.454(5) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 O2 1.241(5) . ? C5 N2 1.344(5) . ? C5 N5 1.356(5) . ? C6 N2 1.442(5) . ? C6 N4 1.450(5) . ? C6 C7 1.536(6) . ? C6 H6 0.9900 . ? C7 N7 1.441(5) . ? C7 N5 1.453(5) . ? C7 H7 0.9900 . ? C8 O5 1.219(5) . ? C8 N7 1.367(5) . ? C8 N4 1.373(5) . ? C9 N6 1.437(5) . ? C9 N5 1.453(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 N8 1.441(5) . ? C10 N7 1.444(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 O3 1.232(5) . ? C11 N9 1.357(5) . ? C11 N6 1.363(5) . ? C12 N6 1.445(5) . ? C12 N8 1.458(5) . ? C12 C13 1.543(6) . ? C12 H12 0.9900 . ? C13 N11 1.444(5) . ? C13 N9 1.454(6) . ? C13 H13 0.9900 . ? C14 O6 1.223(6) . ? C14 N8 1.360(6) . ? C14 N11 1.368(6) . ? C15 N10 1.455(5) . ? C15 N9 1.456(5) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 N12 1.434(5) . ? C16 N11 1.443(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 O4 1.232(5) . ? C17 N10 1.346(6) . ? C17 N13 1.372(5) . ? C18 N12 1.445(5) . ? C18 N10 1.466(5) . ? C18 C19 1.539(6) . ? C18 H18 0.9900 . ? C19 N13 1.444(5) . ? C19 N14 1.457(5) . ? C19 H19 0.9900 . ? C20 O7 1.235(5) . ? C20 N14 1.361(6) . ? C20 N12 1.366(5) . ? C21 N14 1.441(5) . ? C21 N13 1.455(5) 2 ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? N3 C1 1.352(5) 2 ? N13 C21 1.455(5) 2 ? O7 Gd1 2.414(3) 6_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Zn1 Cl2 112.29(7) . . ? Cl1 Zn1 Cl3 110.80(6) . . ? Cl2 Zn1 Cl3 107.95(9) . . ? Cl1 Zn1 Cl4 105.91(11) . . ? Cl2 Zn1 Cl4 111.23(9) . . ? Cl3 Zn1 Cl4 108.63(11) . . ? Cl2 Zn1' Cl3 126.0(5) . . ? Cl2 Zn1' Cl1 116.0(4) . . ? Cl3 Zn1' Cl1 114.3(4) . . ? Zn1 Cl1 Zn1' 24.5(6) . . ? Zn1' Cl2 Zn1 25.8(6) . . ? Zn1' Cl3 Zn1 25.8(6) . . ? O2W Gd1 O2 146.52(11) . . ? O2W Gd1 O4W 108.15(13) . . ? O2 Gd1 O4W 78.67(11) . . ? O2W Gd1 O1 75.60(11) . . ? O2 Gd1 O1 79.87(11) . . ? O4W Gd1 O1 142.53(11) . . ? O2W Gd1 O1W 140.86(12) . . ? O2 Gd1 O1W 71.30(11) . . ? O4W Gd1 O1W 84.14(13) . . ? O1 Gd1 O1W 117.10(12) . . ? O2W Gd1 O3W 75.35(13) . . ? O2 Gd1 O3W 76.27(12) . . ? O4W Gd1 O3W 71.16(11) . . ? O1 Gd1 O3W 74.12(11) . . ? O1W Gd1 O3W 142.41(13) . . ? O2W Gd1 O7 72.70(11) . 6_566 ? O2 Gd1 O7 138.21(10) . 6_566 ? O4W Gd1 O7 72.18(10) . 6_566 ? O1 Gd1 O7 139.82(11) . 6_566 ? O1W Gd1 O7 76.45(11) . 6_566 ? O3W Gd1 O7 119.60(11) . 6_566 ? O2W Gd1 O5W 79.95(13) . . ? O2 Gd1 O5W 113.46(12) . . ? O4W Gd1 O5W 145.48(11) . . ? O1 Gd1 O5W 71.75(11) . . ? O1W Gd1 O5W 70.89(13) . . ? O3W Gd1 O5W 141.78(12) . . ? O7 Gd1 O5W 78.90(11) 6_566 . ? O1 C1 N3 126.6(4) . 2 ? O1 C1 N1 124.7(4) . . ? N3 C1 N1 108.7(3) 2 . ? N1 C2 N3 115.2(3) . . ? N1 C2 C2 103.2(4) . 2 ? N3 C2 C2 102.3(3) . 2 ? N1 C2 H2 111.8 . . ? N3 C2 H2 111.8 . . ? C2 C2 H2 111.8 2 . ? N1 C3 N2 113.4(3) . . ? N1 C3 H3A 108.9 . . ? N2 C3 H3A 108.9 . . ? N1 C3 H3B 108.9 . . ? N2 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? N4 C4 N3 114.2(3) . . ? N4 C4 H4A 108.7 . . ? N3 C4 H4A 108.7 . . ? N4 C4 H4B 108.7 . . ? N3 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? O2 C5 N2 125.7(4) . . ? O2 C5 N5 125.4(4) . . ? N2 C5 N5 108.9(4) . . ? N2 C6 N4 114.2(3) . . ? N2 C6 C7 103.3(3) . . ? N4 C6 C7 103.1(3) . . ? N2 C6 H6 111.9 . . ? N4 C6 H6 111.9 . . ? C7 C6 H6 111.9 . . ? N7 C7 N5 113.6(3) . . ? N7 C7 C6 104.1(3) . . ? N5 C7 C6 103.0(3) . . ? N7 C7 H7 111.8 . . ? N5 C7 H7 111.8 . . ? C6 C7 H7 111.8 . . ? O5 C8 N7 125.5(4) . . ? O5 C8 N4 126.3(4) . . ? N7 C8 N4 108.1(3) . . ? N6 C9 N5 113.3(3) . . ? N6 C9 H9A 108.9 . . ? N5 C9 H9A 108.9 . . ? N6 C9 H9B 108.9 . . ? N5 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? N8 C10 N7 113.3(4) . . ? N8 C10 H10A 108.9 . . ? N7 C10 H10A 108.9 . . ? N8 C10 H10B 108.9 . . ? N7 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? O3 C11 N9 125.1(4) . . ? O3 C11 N6 126.1(4) . . ? N9 C11 N6 108.8(4) . . ? N6 C12 N8 114.3(3) . . ? N6 C12 C13 103.9(3) . . ? N8 C12 C13 103.1(3) . . ? N6 C12 H12 111.6 . . ? N8 C12 H12 111.6 . . ? C13 C12 H12 111.6 . . ? N11 C13 N9 114.1(4) . . ? N11 C13 C12 103.7(3) . . ? N9 C13 C12 102.4(3) . . ? N11 C13 H13 112.0 . . ? N9 C13 H13 112.0 . . ? C12 C13 H13 112.0 . . ? O6 C14 N8 125.2(4) . . ? O6 C14 N11 125.6(4) . . ? N8 C14 N11 109.2(4) . . ? N10 C15 N9 113.3(3) . . ? N10 C15 H15A 108.9 . . ? N9 C15 H15A 108.9 . . ? N10 C15 H15B 108.9 . . ? N9 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? N12 C16 N11 113.6(3) . . ? N12 C16 H16A 108.9 . . ? N11 C16 H16A 108.9 . . ? N12 C16 H16B 108.9 . . ? N11 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? O4 C17 N10 126.0(4) . . ? O4 C17 N13 125.0(4) . . ? N10 C17 N13 109.0(4) . . ? N12 C18 N10 114.0(3) . . ? N12 C18 C19 104.2(3) . . ? N10 C18 C19 102.6(3) . . ? N12 C18 H18 111.8 . . ? N10 C18 H18 111.8 . . ? C19 C18 H18 111.8 . . ? N13 C19 N14 114.8(3) . . ? N13 C19 C18 104.1(3) . . ? N14 C19 C18 102.8(3) . . ? N13 C19 H19 111.5 . . ? N14 C19 H19 111.5 . . ? C18 C19 H19 111.5 . . ? O7 C20 N14 125.4(4) . . ? O7 C20 N12 125.7(4) . . ? N14 C20 N12 108.9(3) . . ? N14 C21 N13 113.9(3) . 2 ? N14 C21 H21A 108.8 . . ? N13 C21 H21A 108.8 2 . ? N14 C21 H21B 108.8 . . ? N13 C21 H21B 108.8 2 . ? H21A C21 H21B 107.7 . . ? C1 N1 C3 123.3(3) . . ? C1 N1 C2 112.0(3) . . ? C3 N1 C2 124.7(3) . . ? C5 N2 C6 112.7(3) . . ? C5 N2 C3 123.4(4) . . ? C6 N2 C3 123.6(3) . . ? C1 N3 C4 122.5(3) 2 . ? C1 N3 C2 112.3(3) 2 . ? C4 N3 C2 123.7(3) . . ? C8 N4 C4 122.2(3) . . ? C8 N4 C6 112.0(3) . . ? C4 N4 C6 123.4(3) . . ? C5 N5 C7 111.9(3) . . ? C5 N5 C9 122.5(3) . . ? C7 N5 C9 122.5(3) . . ? C11 N6 C9 123.2(3) . . ? C11 N6 C12 111.7(3) . . ? C9 N6 C12 123.1(3) . . ? C8 N7 C7 112.1(3) . . ? C8 N7 C10 121.7(4) . . ? C7 N7 C10 122.2(3) . . ? C14 N8 C10 121.8(4) . . ? C14 N8 C12 111.5(3) . . ? C10 N8 C12 122.4(3) . . ? C11 N9 C13 112.2(3) . . ? C11 N9 C15 121.8(3) . . ? C13 N9 C15 122.2(3) . . ? C17 N10 C15 121.4(3) . . ? C17 N10 C18 112.4(3) . . ? C15 N10 C18 122.5(4) . . ? C14 N11 C16 123.4(4) . . ? C14 N11 C13 111.8(3) . . ? C16 N11 C13 123.9(3) . . ? C20 N12 C16 123.7(3) . . ? C20 N12 C18 111.7(3) . . ? C16 N12 C18 123.6(3) . . ? C17 N13 C19 111.7(3) . . ? C17 N13 C21 123.0(4) . 2 ? C19 N13 C21 123.7(3) . 2 ? C20 N14 C21 124.4(3) . . ? C20 N14 C19 112.2(3) . . ? C21 N14 C19 123.5(3) . . ? C1 O1 Gd1 160.5(3) . . ? C5 O2 Gd1 150.6(3) . . ? C20 O7 Gd1 146.5(3) . 6_565 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.010 _refine_diff_density_min -1.841 _refine_diff_density_rms 0.122 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.003 -0.013 0.000 1256 376 ' ' 2 0.011 -0.001 0.500 1256 376 ' ' 3 0.500 0.000 0.256 464 159 ' ' 4 0.000 0.500 0.261 464 159 ' ' _platon_squeeze_details ; ; data_p9 _database_code_depnum_ccdc_archive 'CCDC 905590' #TrackingRef '7 (905590).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H58 Cl5 N14 O25.50 Tb Zn' _chemical_formula_weight 1316.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.375(2) _cell_length_b 18.8405(17) _cell_length_c 20.0249(18) _cell_angle_alpha 90.00 _cell_angle_beta 104.690(3) _cell_angle_gamma 90.00 _cell_volume 9625.3(15) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.817 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5328 _exptl_absorpt_coefficient_mu 2.330 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5616 _exptl_absorpt_correction_T_max 0.6163 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43254 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9335 _reflns_number_gt 7734 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1018P)^2^+20.9351P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9335 _refine_ls_number_parameters 501 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1541 _refine_ls_wR_factor_gt 0.1468 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.113 _refine_ls_shift/su_max 0.003 _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 0.071970(6) 0.785860(9) 0.494681(8) 0.02613(5) Uani 1 1 d . . . Zn1 Zn -0.36494(3) 1.04842(4) 0.68714(5) 0.0642(2) Uani 0.77 1 d P . . Zn1' Zn -0.36596(12) 1.04865(15) 0.73250(18) 0.0736(9) Uani 0.23 1 d P . . Cl1 Cl -0.37913(18) 1.0257(2) 0.5743(2) 0.2108(16) Uani 1 1 d U . . Cl2 Cl -0.44271(7) 1.05624(10) 0.7126(2) 0.2246(17) Uani 1 1 d . . . Cl3 Cl -0.31551(6) 0.96493(7) 0.75457(10) 0.0927(5) Uani 1 1 d . . . Cl4 Cl -0.32548(4) 1.15380(6) 0.70293(6) 0.0481(3) Uani 1 1 d . . . Cl5 Cl 0.0000 0.83166(10) 0.2500 0.0890(8) Uani 1 2 d SU . . Cl5' Cl -0.22436(10) 1.27745(15) 0.85644(16) 0.0739(7) Uani 0.50 1 d PU . . O1W O 0.15262(12) 0.7393(2) 0.56385(15) 0.0571(9) Uani 1 1 d . . . O2W O 0.03760(12) 0.86724(15) 0.40273(14) 0.0442(8) Uani 1 1 d . . . O3W O -0.01567(10) 0.80055(17) 0.49487(14) 0.0433(8) Uani 1 1 d . . . O4W O 0.11335(12) 0.89597(15) 0.52098(13) 0.0439(7) Uani 1 1 d . . . O5W O 0.05454(13) 0.67134(16) 0.53811(15) 0.0508(8) Uani 1 1 d . . . O1 O 0.07057(10) 1.18495(14) 0.11039(12) 0.0327(6) Uani 1 1 d . . . O2 O 0.13660(15) 1.01936(16) 0.13121(14) 0.0563(9) Uani 1 1 d . . . O3 O -0.02618(10) 0.71512(12) 0.09857(13) 0.0309(6) Uani 1 1 d . . . O4 O 0.13330(10) 0.78191(13) 0.42817(13) 0.0341(6) Uani 1 1 d . . . O5 O 0.09304(10) 0.81870(15) 0.12030(13) 0.0393(7) Uani 1 1 d . . . O6 O -0.05719(10) 1.14990(14) 0.09412(13) 0.0373(6) Uani 1 1 d . . . O7 O 0.14639(11) 0.98839(15) 0.43463(13) 0.0430(7) Uani 1 1 d . . . N1 N 0.13362(12) 0.71636(15) 0.33117(15) 0.0292(7) Uani 1 1 d . . . N2 N 0.17286(11) 1.07602(16) 0.23460(15) 0.0310(7) Uani 1 1 d . . . N3 N -0.05243(11) 0.65166(15) 0.18231(14) 0.0279(7) Uani 1 1 d . . . N4 N 0.03178(11) 0.66532(15) 0.19264(14) 0.0272(7) Uani 1 1 d . . . N5 N 0.04889(11) 1.24494(16) 0.20035(14) 0.0265(7) Uani 1 1 d . . . N6 N 0.16850(11) 1.06123(16) 0.35344(14) 0.0306(7) Uani 1 1 d . . . N7 N 0.17235(11) 0.82080(16) 0.34389(14) 0.0280(7) Uani 1 1 d . . . N8 N 0.15790(11) 0.83370(16) 0.22006(14) 0.0277(7) Uani 1 1 d . . . N9 N 0.18737(11) 0.94650(16) 0.35319(14) 0.0295(7) Uani 1 1 d . . . N10 N 0.12300(11) 1.18490(16) 0.22225(14) 0.0270(7) Uani 1 1 d . . . N11 N -0.04500(11) 1.23513(16) 0.17924(14) 0.0276(7) Uani 1 1 d . . . N12 N -0.11640(11) 1.16842(16) 0.15923(14) 0.0285(7) Uani 1 1 d . . . N13 N 0.11129(11) 0.73379(16) 0.20653(15) 0.0286(7) Uani 1 1 d . . . N14 N 0.17798(12) 0.95865(16) 0.22989(15) 0.0307(7) Uani 1 1 d . . . C1 C 0.16759(14) 1.1474(2) 0.20925(19) 0.0323(9) Uani 1 1 d . . . H1A H 0.1642 1.1466 0.1594 0.039 Uiso 1 1 calc R . . H1B H 0.1996 1.1737 0.2309 0.039 Uiso 1 1 calc R . . C2 C 0.15884(14) 1.1278(2) 0.38379(18) 0.0313(9) Uani 1 1 d . . . H2A H 0.1909 1.1564 0.3931 0.038 Uiso 1 1 calc R . . H2B H 0.1507 1.1182 0.4281 0.038 Uiso 1 1 calc R . . C3 C 0.20087(14) 1.05655(19) 0.30440(18) 0.0296(8) Uani 1 1 d . . . H3A H 0.2345 1.0822 0.3204 0.036 Uiso 1 1 calc R . . C4 C 0.14490(13) 0.77372(19) 0.37238(18) 0.0280(8) Uani 1 1 d . . . C5 C 0.15273(13) 0.72226(19) 0.27034(18) 0.0271(8) Uani 1 1 d . . . H5A H 0.1758 0.6821 0.2659 0.033 Uiso 1 1 calc R . . C6 C -0.07129(13) 1.1811(2) 0.14023(17) 0.0289(8) Uani 1 1 d . . . C7 C 0.07952(13) 1.20284(17) 0.17195(18) 0.0253(8) Uani 1 1 d . . . C8 C -0.01596(13) 0.68127(18) 0.15350(16) 0.0253(8) Uani 1 1 d . . . C9 C 0.11785(13) 0.79742(19) 0.17649(19) 0.0296(9) Uani 1 1 d . . . C10 C 0.07904(13) 0.6788(2) 0.16954(17) 0.0309(9) Uani 1 1 d . . . H10A H 0.0996 0.6349 0.1742 0.037 Uiso 1 1 calc R . . H10B H 0.0689 0.6913 0.1205 0.037 Uiso 1 1 calc R . . C11 C -0.00160(13) 1.27180(19) 0.16313(18) 0.0276(8) Uani 1 1 d . . . H11A H -0.0037 1.3223 0.1738 0.033 Uiso 1 1 calc R . . H11B H -0.0046 1.2677 0.1135 0.033 Uiso 1 1 calc R . . C12 C 0.07270(13) 1.26205(19) 0.27266(17) 0.0265(8) Uani 1 1 d . . . H12A H 0.0800 1.3135 0.2793 0.032 Uiso 1 1 calc R . . C13 C 0.02949(13) 0.62088(18) 0.25159(18) 0.0278(8) Uani 1 1 d . . . H13A H 0.0429 0.5724 0.2475 0.033 Uiso 1 1 calc R . . C14 C 0.18232(13) 0.79306(18) 0.28044(18) 0.0271(8) Uani 1 1 d . . . H14A H 0.2203 0.7863 0.2848 0.033 Uiso 1 1 calc R . . C15 C -0.10808(13) 0.65408(19) 0.15011(18) 0.0280(8) Uani 1 1 d . . . H15A H -0.1246 0.6116 0.1634 0.034 Uiso 1 1 calc R . . H15B H -0.1135 0.6532 0.0999 0.034 Uiso 1 1 calc R . . C16 C 0.20172(14) 0.87772(19) 0.38307(18) 0.0310(9) Uani 1 1 d . . . H16A H 0.2391 0.8698 0.3870 0.037 Uiso 1 1 calc R . . H16B H 0.1964 0.8770 0.4298 0.037 Uiso 1 1 calc R . . C17 C 0.20846(12) 0.97528(19) 0.29918(17) 0.0270(8) Uani 1 1 d . . . H17A H 0.2459 0.9627 0.3059 0.032 Uiso 1 1 calc R . . C18 C 0.16497(13) 0.9977(2) 0.38442(17) 0.0303(8) Uani 1 1 d . . . C19 C 0.18410(14) 0.89296(19) 0.19607(19) 0.0327(9) Uani 1 1 d . . . H19A H 0.2215 0.8822 0.2044 0.039 Uiso 1 1 calc R . . H19B H 0.1698 0.8986 0.1462 0.039 Uiso 1 1 calc R . . C20 C 0.12415(14) 1.21765(18) 0.28819(18) 0.0264(8) Uani 1 1 d . . . H20A H 0.1556 1.2476 0.3051 0.032 Uiso 1 1 calc R . . C21 C 0.16006(16) 1.0183(2) 0.19190(19) 0.0364(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.03517(9) 0.02820(10) 0.01597(9) 0.00089(6) 0.00822(7) 0.00471(6) Zn1 0.0529(4) 0.0355(4) 0.1011(6) 0.0151(4) 0.0140(4) -0.0043(3) Zn1' 0.0817(17) 0.0483(15) 0.098(2) 0.0346(15) 0.0358(16) 0.0109(13) Cl1 0.254(3) 0.174(2) 0.180(3) -0.047(2) 0.010(2) 0.003(2) Cl2 0.0775(9) 0.0573(10) 0.562(5) 0.0702(18) 0.1228(17) 0.0101(8) Cl3 0.0863(7) 0.0484(7) 0.1621(13) 0.0466(7) 0.0661(8) 0.0140(6) Cl4 0.0535(5) 0.0345(5) 0.0607(6) 0.0095(5) 0.0225(4) 0.0054(4) Cl5 0.178(2) 0.0474(10) 0.0341(9) 0.000 0.0140(11) 0.000 Cl5' 0.0746(12) 0.0764(15) 0.0845(15) 0.0094(12) 0.0457(11) 0.0391(11) O1W 0.0505(16) 0.085(2) 0.0341(16) 0.0231(16) 0.0076(13) 0.0226(16) O2W 0.0644(17) 0.0335(15) 0.0295(14) 0.0042(12) 0.0023(13) 0.0093(13) O3W 0.0412(13) 0.0676(19) 0.0224(13) -0.0015(12) 0.0106(11) 0.0126(13) O4W 0.0731(16) 0.0393(15) 0.0223(12) -0.0047(11) 0.0177(12) -0.0140(14) O5W 0.0733(18) 0.0369(16) 0.0392(16) 0.0118(13) 0.0089(14) -0.0007(14) O1 0.0437(12) 0.0381(14) 0.0171(11) 0.0000(10) 0.0093(10) 0.0000(12) O2 0.098(2) 0.0402(16) 0.0235(14) 0.0090(12) 0.0016(15) 0.0010(16) O3 0.0381(12) 0.0338(14) 0.0221(12) 0.0061(10) 0.0100(10) -0.0004(10) O4 0.0448(12) 0.0379(15) 0.0247(12) 0.0011(10) 0.0183(10) 0.0017(11) O5 0.0448(13) 0.0422(15) 0.0266(13) 0.0073(12) 0.0012(11) -0.0011(12) O6 0.0527(13) 0.0340(14) 0.0315(13) -0.0057(11) 0.0222(10) -0.0056(12) O7 0.0623(14) 0.0429(15) 0.0318(13) 0.0083(12) 0.0267(11) 0.0036(13) N1 0.0379(14) 0.0306(16) 0.0212(14) -0.0022(11) 0.0116(12) 0.0010(12) N2 0.0442(14) 0.0279(15) 0.0245(14) 0.0012(12) 0.0150(12) 0.0054(13) N3 0.0348(13) 0.0266(15) 0.0227(14) 0.0000(12) 0.0081(11) -0.0042(12) N4 0.0358(13) 0.0243(14) 0.0232(14) 0.0024(11) 0.0108(11) 0.0013(12) N5 0.0329(13) 0.0324(16) 0.0142(13) -0.0006(11) 0.0059(10) -0.0022(12) N6 0.0458(14) 0.0287(15) 0.0215(13) 0.0055(12) 0.0164(11) 0.0079(13) N7 0.0332(13) 0.0329(16) 0.0178(13) 0.0029(12) 0.0065(11) 0.0037(12) N8 0.0336(13) 0.0297(15) 0.0195(14) 0.0038(11) 0.0063(11) 0.0024(12) N9 0.0409(14) 0.0289(15) 0.0190(14) 0.0028(12) 0.0084(11) 0.0054(13) N10 0.0357(13) 0.0289(15) 0.0181(13) -0.0022(11) 0.0102(11) -0.0027(12) N11 0.0359(13) 0.0279(15) 0.0198(14) 0.0004(12) 0.0086(11) -0.0046(12) N12 0.0360(13) 0.0296(15) 0.0225(14) -0.0053(12) 0.0125(11) -0.0058(12) N13 0.0332(14) 0.0292(15) 0.0218(14) 0.0032(12) 0.0040(11) -0.0002(12) N14 0.0420(15) 0.0267(15) 0.0222(14) 0.0010(12) 0.0061(12) 0.0012(13) C1 0.0415(17) 0.0328(19) 0.0254(17) 0.0037(15) 0.0136(14) 0.0020(15) C2 0.0406(17) 0.0346(19) 0.0184(16) 0.0038(14) 0.0071(13) 0.0040(16) C3 0.0374(16) 0.0302(19) 0.0230(16) 0.0003(14) 0.0109(13) 0.0017(15) C4 0.0274(15) 0.0324(19) 0.0245(17) 0.0041(14) 0.0073(13) 0.0058(14) C5 0.0298(15) 0.0325(19) 0.0190(16) 0.0002(13) 0.0060(13) 0.0064(14) C6 0.0405(17) 0.0299(18) 0.0174(16) 0.0030(14) 0.0093(13) -0.0016(15) C7 0.0370(16) 0.0195(16) 0.0216(16) 0.0034(13) 0.0114(13) -0.0044(13) C8 0.0369(15) 0.0225(16) 0.0185(15) -0.0003(13) 0.0108(12) -0.0002(14) C9 0.0310(15) 0.0322(19) 0.0276(18) 0.0007(14) 0.0112(13) 0.0057(14) C10 0.0372(16) 0.039(2) 0.0191(16) -0.0039(15) 0.0123(13) 0.0027(16) C11 0.0362(16) 0.0253(17) 0.0221(17) 0.0013(13) 0.0089(13) -0.0006(14) C12 0.0346(15) 0.0238(16) 0.0207(16) -0.0015(14) 0.0061(13) -0.0029(14) C13 0.0400(17) 0.0182(16) 0.0260(17) -0.0031(13) 0.0100(14) 0.0027(14) C14 0.0311(15) 0.0321(19) 0.0205(16) 0.0018(13) 0.0109(13) 0.0068(14) C15 0.0324(15) 0.0261(18) 0.0257(17) -0.0054(14) 0.0076(13) -0.0071(14) C16 0.0352(16) 0.0328(19) 0.0223(17) 0.0035(15) 0.0021(14) 0.0036(15) C17 0.0273(14) 0.0296(18) 0.0244(17) 0.0027(14) 0.0073(13) 0.0040(14) C18 0.0383(16) 0.0344(19) 0.0197(16) 0.0019(14) 0.0098(13) 0.0022(15) C19 0.0426(17) 0.0294(19) 0.0289(18) -0.0008(15) 0.0146(14) 0.0004(15) C20 0.0322(16) 0.0285(18) 0.0182(16) 0.0042(13) 0.0057(13) -0.0003(13) C21 0.053(2) 0.030(2) 0.0291(19) 0.0026(15) 0.0147(16) -0.0002(17) _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 O3W 2.329(3) . ? Tb1 O4W 2.341(3) . ? Tb1 O4 2.343(3) . ? Tb1 O3 2.362(2) 2 ? Tb1 O1 2.391(2) 6_576 ? Tb1 O2W 2.391(3) . ? Tb1 O1W 2.391(3) . ? Tb1 O5W 2.414(3) . ? Zn1 Zn1' 0.915(4) . ? Zn1 Cl4 2.2266(13) . ? Zn1 Cl1 2.237(4) . ? Zn1 Cl2 2.241(3) . ? Zn1 Cl3 2.2595(17) . ? Zn1' Cl2 1.967(4) . ? Zn1' Cl3 2.039(3) . ? Zn1' Cl4 2.395(3) . ? O1 C7 1.241(4) . ? O1 Tb1 2.391(2) 6_575 ? O2 C21 1.216(5) . ? O3 C8 1.241(4) . ? O3 Tb1 2.362(2) 2 ? O4 C4 1.241(5) . ? O5 C9 1.217(4) . ? O6 C6 1.229(4) . ? O7 C18 1.237(5) . ? N1 C4 1.346(5) . ? N1 C5 1.436(5) . ? N1 C15 1.449(5) 2 ? N2 C21 1.371(5) . ? N2 C1 1.432(5) . ? N2 C3 1.453(4) . ? N3 C8 1.361(4) . ? N3 C13 1.431(4) 2 ? N3 C15 1.447(4) . ? N4 C8 1.338(4) . ? N4 C10 1.458(5) . ? N4 C13 1.461(5) . ? N5 C7 1.356(5) . ? N5 C11 1.443(4) . ? N5 C12 1.461(4) . ? N6 C18 1.362(5) . ? N6 C2 1.445(5) . ? N6 C3 1.458(5) . ? N7 C4 1.359(5) . ? N7 C16 1.434(5) . ? N7 C14 1.458(5) . ? N8 C9 1.370(4) . ? N8 C14 1.438(4) . ? N8 C19 1.457(5) . ? N9 C18 1.363(5) . ? N9 C16 1.437(5) . ? N9 C17 1.442(5) . ? N10 C7 1.363(4) . ? N10 C20 1.451(4) . ? N10 C1 1.451(5) . ? N11 C6 1.361(5) . ? N11 C12 1.441(5) 2 ? N11 C11 1.442(5) . ? N12 C6 1.359(5) . ? N12 C2 1.446(4) 2 ? N12 C20 1.456(4) 2 ? N13 C9 1.372(5) . ? N13 C10 1.424(5) . ? N13 C5 1.472(4) . ? N14 C21 1.373(5) . ? N14 C19 1.439(5) . ? N14 C17 1.451(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C2 N12 1.446(4) 2 ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C3 C17 1.551(5) . ? C3 H3A 0.9900 . ? C5 C14 1.533(5) . ? C5 H5A 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.441(5) 2 ? C12 C20 1.557(5) . ? C12 H12A 0.9900 . ? C13 N3 1.431(4) 2 ? C13 C13 1.541(7) 2 ? C13 H13A 0.9900 . ? C14 H14A 0.9900 . ? C15 N1 1.449(5) 2 ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 H17A 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C20 N12 1.456(4) 2 ? C20 H20A 0.9900 . ? 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 O3W Tb1 O4W 107.49(11) . . ? O3W Tb1 O4 146.44(9) . . ? O4W Tb1 O4 78.84(9) . . ? O3W Tb1 O3 76.09(9) . 2 ? O4W Tb1 O3 142.53(9) . 2 ? O4 Tb1 O3 79.69(9) . 2 ? O3W Tb1 O1 73.25(9) . 6_576 ? O4W Tb1 O1 72.48(9) . 6_576 ? O4 Tb1 O1 137.81(9) . 6_576 ? O3 Tb1 O1 139.96(9) 2 6_576 ? O3W Tb1 O2W 75.07(11) . . ? O4W Tb1 O2W 70.67(9) . . ? O4 Tb1 O2W 76.36(10) . . ? O3 Tb1 O2W 74.63(9) 2 . ? O1 Tb1 O2W 120.19(9) 6_576 . ? O3W Tb1 O1W 141.27(10) . . ? O4W Tb1 O1W 84.21(12) . . ? O4 Tb1 O1W 71.14(10) . . ? O3 Tb1 O1W 116.91(11) 2 . ? O1 Tb1 O1W 75.70(10) 6_576 . ? O2W Tb1 O1W 142.10(11) . . ? O3W Tb1 O5W 79.97(11) . . ? O4W Tb1 O5W 146.26(9) . . ? O4 Tb1 O5W 113.49(10) . . ? O3 Tb1 O5W 71.00(9) 2 . ? O1 Tb1 O5W 78.77(10) 6_576 . ? O2W Tb1 O5W 141.36(10) . . ? O1W Tb1 O5W 71.71(12) . . ? Zn1' Zn1 Cl4 89.2(2) . . ? Zn1' Zn1 Cl1 164.6(2) . . ? Cl4 Zn1 Cl1 105.46(12) . . ? Zn1' Zn1 Cl2 61.0(2) . . ? Cl4 Zn1 Cl2 109.33(7) . . ? Cl1 Zn1 Cl2 108.34(17) . . ? Zn1' Zn1 Cl3 64.40(19) . . ? Cl4 Zn1 Cl3 110.96(6) . . ? Cl1 Zn1 Cl3 113.20(12) . . ? Cl2 Zn1 Cl3 109.42(10) . . ? Zn1 Zn1' Cl2 95.0(3) . . ? Zn1 Zn1' Cl3 91.7(2) . . ? Cl2 Zn1' Cl3 133.00(16) . . ? Zn1 Zn1' Cl4 68.37(18) . . ? Cl2 Zn1' Cl4 112.97(14) . . ? Cl3 Zn1' Cl4 112.72(15) . . ? Zn1' Cl2 Zn1 24.02(11) . . ? Zn1' Cl3 Zn1 23.89(10) . . ? Zn1 Cl4 Zn1' 22.47(9) . . ? C7 O1 Tb1 148.6(2) . 6_575 ? C8 O3 Tb1 160.7(2) . 2 ? C4 O4 Tb1 151.6(2) . . ? C4 N1 C5 112.8(3) . . ? C4 N1 C15 122.4(3) . 2 ? C5 N1 C15 124.6(3) . 2 ? C21 N2 C1 122.5(3) . . ? C21 N2 C3 112.6(3) . . ? C1 N2 C3 123.9(3) . . ? C8 N3 C13 112.3(3) . 2 ? C8 N3 C15 123.0(3) . . ? C13 N3 C15 124.6(3) 2 . ? C8 N4 C10 121.9(3) . . ? C8 N4 C13 112.1(3) . . ? C10 N4 C13 124.7(3) . . ? C7 N5 C11 123.9(3) . . ? C7 N5 C12 113.1(3) . . ? C11 N5 C12 122.9(3) . . ? C18 N6 C2 122.1(3) . . ? C18 N6 C3 111.9(3) . . ? C2 N6 C3 122.1(3) . . ? C4 N7 C16 122.0(3) . . ? C4 N7 C14 111.4(3) . . ? C16 N7 C14 123.6(3) . . ? C9 N8 C14 112.2(3) . . ? C9 N8 C19 121.7(3) . . ? C14 N8 C19 122.4(3) . . ? C18 N9 C16 123.1(3) . . ? C18 N9 C17 111.9(3) . . ? C16 N9 C17 122.7(3) . . ? C7 N10 C20 112.7(3) . . ? C7 N10 C1 123.8(3) . . ? C20 N10 C1 122.7(3) . . ? C6 N11 C12 112.1(3) . 2 ? C6 N11 C11 123.2(3) . . ? C12 N11 C11 123.1(3) 2 . ? C6 N12 C2 121.8(3) . 2 ? C6 N12 C20 112.6(3) . 2 ? C2 N12 C20 122.6(3) 2 2 ? C9 N13 C10 122.2(3) . . ? C9 N13 C5 111.2(3) . . ? C10 N13 C5 123.9(3) . . ? C21 N14 C19 120.5(3) . . ? C21 N14 C17 112.5(3) . . ? C19 N14 C17 122.3(3) . . ? N2 C1 N10 113.8(3) . . ? N2 C1 H1A 108.8 . . ? N10 C1 H1A 108.8 . . ? N2 C1 H1B 108.8 . . ? N10 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? N6 C2 N12 113.7(3) . 2 ? N6 C2 H2A 108.8 . . ? N12 C2 H2A 108.8 2 . ? N6 C2 H2B 108.8 . . ? N12 C2 H2B 108.8 2 . ? H2A C2 H2B 107.7 . . ? N2 C3 N6 113.0(3) . . ? N2 C3 C17 103.1(3) . . ? N6 C3 C17 102.3(3) . . ? N2 C3 H3A 112.5 . . ? N6 C3 H3A 112.5 . . ? C17 C3 H3A 112.5 . . ? O4 C4 N1 125.8(3) . . ? O4 C4 N7 125.2(3) . . ? N1 C4 N7 109.0(3) . . ? N1 C5 N13 113.9(3) . . ? N1 C5 C14 103.4(3) . . ? N13 C5 C14 103.1(3) . . ? N1 C5 H5A 111.9 . . ? N13 C5 H5A 111.9 . . ? C14 C5 H5A 111.9 . . ? O6 C6 N12 125.4(3) . . ? O6 C6 N11 125.6(3) . . ? N12 C6 N11 109.0(3) . . ? O1 C7 N5 126.3(3) . . ? O1 C7 N10 125.4(3) . . ? N5 C7 N10 108.3(3) . . ? O3 C8 N4 126.6(3) . . ? O3 C8 N3 124.7(3) . . ? N4 C8 N3 108.7(3) . . ? O5 C9 N8 124.9(3) . . ? O5 C9 N13 126.5(3) . . ? N8 C9 N13 108.6(3) . . ? N13 C10 N4 114.1(3) . . ? N13 C10 H10A 108.7 . . ? N4 C10 H10A 108.7 . . ? N13 C10 H10B 108.7 . . ? N4 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? N11 C11 N5 113.4(3) . . ? N11 C11 H11A 108.9 . . ? N5 C11 H11A 108.9 . . ? N11 C11 H11B 108.9 . . ? N5 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? N11 C12 N5 114.9(3) 2 . ? N11 C12 C20 104.0(3) 2 . ? N5 C12 C20 102.3(3) . . ? N11 C12 H12A 111.7 2 . ? N5 C12 H12A 111.7 . . ? C20 C12 H12A 111.7 . . ? N3 C13 N4 114.9(3) 2 . ? N3 C13 C13 102.9(3) 2 2 ? N4 C13 C13 102.4(3) . 2 ? N3 C13 H13A 112.0 2 . ? N4 C13 H13A 112.0 . . ? C13 C13 H13A 112.0 2 . ? N8 C14 N7 113.6(3) . . ? N8 C14 C5 104.4(3) . . ? N7 C14 C5 103.2(3) . . ? N8 C14 H14A 111.7 . . ? N7 C14 H14A 111.7 . . ? C5 C14 H14A 111.7 . . ? N3 C15 N1 113.3(3) . 2 ? N3 C15 H15A 108.9 . . ? N1 C15 H15A 108.9 2 . ? N3 C15 H15B 108.9 . . ? N1 C15 H15B 108.9 2 . ? H15A C15 H15B 107.7 . . ? N7 C16 N9 113.4(3) . . ? N7 C16 H16A 108.9 . . ? N9 C16 H16A 108.9 . . ? N7 C16 H16B 108.9 . . ? N9 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? N9 C17 N14 114.2(3) . . ? N9 C17 C3 103.9(3) . . ? N14 C17 C3 103.2(3) . . ? N9 C17 H17A 111.7 . . ? N14 C17 H17A 111.7 . . ? C3 C17 H17A 111.7 . . ? O7 C18 N6 125.5(3) . . ? O7 C18 N9 125.4(3) . . ? N6 C18 N9 109.0(3) . . ? N14 C19 N8 112.6(3) . . ? N14 C19 H19A 109.1 . . ? N8 C19 H19A 109.1 . . ? N14 C19 H19B 109.1 . . ? N8 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? N10 C20 N12 114.4(3) . 2 ? N10 C20 C12 103.3(3) . . ? N12 C20 C12 102.2(3) 2 . ? N10 C20 H20A 112.0 . . ? N12 C20 H20A 112.0 2 . ? C12 C20 H20A 112.0 . . ? O2 C21 N2 126.4(4) . . ? O2 C21 N14 125.7(4) . . ? N2 C21 N14 107.9(3) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.845 _refine_diff_density_min -1.823 _refine_diff_density_rms 0.142 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.003 -0.010 0.000 1183 403 ' ' 2 0.009 0.001 0.500 1183 403 ' ' 3 0.500 0.000 0.256 477 139 ' ' 4 0.000 0.500 0.261 477 139 ' ' _platon_squeeze_details ; ; data_p10 _database_code_depnum_ccdc_archive 'CCDC 905591' #TrackingRef '8 (905591).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H64 Cl5 Er N14 O28.50 Zn' _chemical_formula_weight 1378.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.4821(16) _cell_length_b 18.9227(12) _cell_length_c 19.9297(13) _cell_angle_alpha 90.00 _cell_angle_beta 104.577(2) _cell_angle_gamma 90.00 _cell_volume 9665.5(11) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.895 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5592 _exptl_absorpt_coefficient_mu 2.602 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4993 _exptl_absorpt_correction_T_max 0.5624 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45460 _diffrn_reflns_av_R_equivalents 0.0659 _diffrn_reflns_av_sigmaI/netI 0.0536 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9438 _reflns_number_gt 7329 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1083P)^2^+15.2481P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9438 _refine_ls_number_parameters 487 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1873 _refine_ls_wR_factor_gt 0.1746 _refine_ls_goodness_of_fit_ref 1.154 _refine_ls_restrained_S_all 1.163 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl5 Cl 0.77631(10) 0.78035(14) 0.85643(15) 0.0924(8) Uani 1 1 d . . . Cl1 Cl 0.67528(6) 0.65424(9) 0.70490(9) 0.0504(4) Uani 1 1 d . . . Cl2 Cl 0.68392(9) 0.46417(11) 0.75225(15) 0.0899(7) Uani 1 1 d . . . Cl3 Cl 0.55803(11) 0.55681(14) 0.7136(3) 0.189(2) Uani 1 1 d . . . Cl4 Cl 0.6194(2) 0.5305(3) 0.5715(3) 0.206(2) Uani 1 1 d U . . Zn1 Zn 0.63528(4) 0.55000(6) 0.69271(10) 0.1139(6) Uani 1 1 d . . . O1W O 0.96173(17) 0.3657(2) 1.0978(2) 0.0436(11) Uani 1 1 d . . . O2W O 1.01400(15) 0.3009(2) 1.0042(2) 0.0414(11) Uani 1 1 d . . . O3W O 0.88689(17) 0.3944(2) 0.97860(18) 0.0388(10) Uani 1 1 d . . . O4W O 0.84884(16) 0.2408(3) 0.9368(2) 0.0489(12) Uani 1 1 d . . . O5W O 0.94419(18) 0.1737(2) 0.9615(2) 0.0479(12) Uani 1 1 d . . . Er1 Er 0.927786(9) 0.286063(12) 1.005332(11) 0.02612(8) Uani 1 1 d . . . C19 C 1.0016(2) 0.2298(3) 0.8371(3) 0.0258(12) Uani 1 1 d . . . H19A H 1.0037 0.1795 0.8262 0.031 Uiso 1 1 calc R . . H19B H 1.0049 0.2337 0.8870 0.031 Uiso 1 1 calc R . . C21 C 1.01649(19) 0.8178(3) 0.8469(2) 0.0240(11) Uani 1 1 d . . . N13 N 0.94742(16) 0.8489(2) 0.6820(2) 0.0259(10) Uani 1 1 d . . . C1 C 0.9204(2) 0.2982(3) 0.8291(3) 0.0251(12) Uani 1 1 d . . . C2 C 0.8762(2) 0.2836(3) 0.7116(3) 0.0252(12) Uani 1 1 d . . . H2 H 0.8447 0.2541 0.6941 0.030 Uiso 1 1 calc R . . C3 C 0.92684(19) 0.2392(3) 0.7270(2) 0.0237(11) Uani 1 1 d . . . H3 H 0.9194 0.1881 0.7201 0.028 Uiso 1 1 calc R . . C4 C 0.9286(2) 0.3196(3) 0.6390(3) 0.0297(12) Uani 1 1 d . . . C5 C 0.8421(2) 0.3730(3) 0.6158(3) 0.0303(13) Uani 1 1 d . . . H5A H 0.8104 0.3439 0.6066 0.036 Uiso 1 1 calc R . . H5B H 0.8501 0.3824 0.5713 0.036 Uiso 1 1 calc R . . C6 C 0.8325(2) 0.3541(3) 0.7903(3) 0.0288(12) Uani 1 1 d . . . H6A H 0.8006 0.3284 0.7677 0.035 Uiso 1 1 calc R . . H6B H 0.8350 0.3546 0.8402 0.035 Uiso 1 1 calc R . . C7 C 0.83581(19) 0.5035(3) 0.6144(3) 0.0278(12) Uani 1 1 d . . . C8 C 0.8002(2) 0.4446(3) 0.6966(3) 0.0274(12) Uani 1 1 d . . . H8 H 0.7668 0.4187 0.6809 0.033 Uiso 1 1 calc R . . C9 C 0.7916(2) 0.5252(3) 0.7005(3) 0.0278(12) Uani 1 1 d . . . H9 H 0.7542 0.5371 0.6937 0.033 Uiso 1 1 calc R . . C10 C 0.8395(2) 0.4824(3) 0.8089(3) 0.0330(13) Uani 1 1 d . . . C11 C 0.7983(2) 0.6221(3) 0.6158(3) 0.0279(12) Uani 1 1 d . . . H11A H 0.7611 0.6302 0.6116 0.034 Uiso 1 1 calc R . . H11B H 0.8040 0.6226 0.5691 0.034 Uiso 1 1 calc R . . C12 C 0.8166(2) 0.6077(3) 0.8043(3) 0.0316(13) Uani 1 1 d . . . H12A H 0.8306 0.6022 0.8545 0.038 Uiso 1 1 calc R . . H12B H 0.7794 0.6189 0.7958 0.038 Uiso 1 1 calc R . . C13 C 0.85610(19) 0.7256(3) 0.6281(3) 0.0239(12) Uani 1 1 d . . . C14 C 0.8181(2) 0.7069(2) 0.7198(3) 0.0233(11) Uani 1 1 d . . . H14 H 0.7804 0.7138 0.7153 0.028 Uiso 1 1 calc R . . C15 C 0.8482(2) 0.7772(3) 0.7304(3) 0.0245(12) Uani 1 1 d . . . H15 H 0.8253 0.8175 0.7346 0.029 Uiso 1 1 calc R . . C16 C 0.8820(2) 0.7027(3) 0.8244(3) 0.0305(13) Uani 1 1 d . . . C17 C 0.89175(18) 0.8449(3) 0.6504(2) 0.0245(11) Uani 1 1 d . . . H17A H 0.8748 0.8866 0.6643 0.029 Uiso 1 1 calc R . . H17B H 0.8860 0.8464 0.5999 0.029 Uiso 1 1 calc R . . C18 C 0.9212(2) 0.8206(3) 0.8315(3) 0.0292(12) Uani 1 1 d . . . H18A H 0.9313 0.8078 0.8807 0.035 Uiso 1 1 calc R . . H18B H 0.9009 0.8644 0.8272 0.035 Uiso 1 1 calc R . . C20 C 0.97043(19) 0.8778(3) 0.7486(3) 0.0271(12) Uani 1 1 d . . . H20 H 0.9575 0.9262 0.7533 0.032 Uiso 1 1 calc R . . N1 N 0.87677(16) 0.3163(2) 0.7784(2) 0.0249(10) Uani 1 1 d . . . N2 N 0.95127(16) 0.2561(2) 0.80055(19) 0.0238(10) Uani 1 1 d . . . N3 N 0.88438(17) 0.3337(2) 0.6591(2) 0.0287(10) Uani 1 1 d . . . N4 N 0.95486(17) 0.2663(2) 0.6792(2) 0.0276(10) Uani 1 1 d . . . N5 N 0.83161(17) 0.4402(2) 0.6462(2) 0.0286(10) Uani 1 1 d . . . N6 N 0.81255(17) 0.5540(2) 0.6466(2) 0.0284(10) Uani 1 1 d . . . N7 N 0.82771(17) 0.4248(2) 0.7657(2) 0.0303(11) Uani 1 1 d . . . N8 N 0.82210(18) 0.5420(2) 0.7712(2) 0.0281(10) Uani 1 1 d . . . N9 N 0.82832(16) 0.6789(2) 0.6564(2) 0.0264(10) Uani 1 1 d . . . N10 N 0.86747(17) 0.7827(2) 0.6688(2) 0.0269(11) Uani 1 1 d . . . N11 N 0.84270(16) 0.6659(2) 0.7809(2) 0.0278(10) Uani 1 1 d . . . N12 N 0.88851(16) 0.7658(2) 0.7941(2) 0.0275(10) Uani 1 1 d . . . N14 N 0.96838(15) 0.8338(2) 0.8080(2) 0.0245(10) Uani 1 1 d . . . O1 O 0.92957(15) 0.3160(2) 0.89024(17) 0.0313(9) Uani 1 1 d . . . O2 O 0.94338(15) 0.3509(2) 0.59373(19) 0.0367(10) Uani 1 1 d . . . O3 O 0.85469(17) 0.5127(2) 0.5658(2) 0.0427(10) Uani 1 1 d . . . O4 O 0.86708(15) 0.71776(19) 0.57086(19) 0.0326(9) Uani 1 1 d . . . O5 O 1.02604(14) 0.78415(18) 0.90145(18) 0.0290(9) Uani 1 1 d . . . O6 O 0.90669(16) 0.6815(2) 0.88157(19) 0.0379(10) Uani 1 1 d . . . O7 O 0.8624(2) 0.4821(2) 0.8694(2) 0.0541(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl5 0.0877(14) 0.1008(18) 0.0985(18) 0.0054(13) 0.0418(13) 0.0366(12) Cl1 0.0533(8) 0.0391(8) 0.0635(10) 0.0085(7) 0.0232(7) 0.0059(7) Cl2 0.0833(12) 0.0472(11) 0.159(2) 0.0372(12) 0.0673(13) 0.0107(10) Cl3 0.0721(15) 0.0565(15) 0.452(7) 0.052(3) 0.093(3) 0.0072(12) Cl4 0.231(4) 0.181(3) 0.189(3) -0.036(3) 0.022(3) 0.016(3) Zn1 0.0625(6) 0.0443(6) 0.2239(17) 0.0088(8) 0.0151(8) -0.0023(5) O1W 0.066(3) 0.033(2) 0.029(2) -0.0055(17) 0.0049(19) -0.006(2) O2W 0.0307(19) 0.067(3) 0.026(2) 0.0029(19) 0.0060(16) -0.0124(19) O3W 0.065(2) 0.032(2) 0.0229(18) 0.0057(16) 0.0182(17) 0.0147(18) O4W 0.039(2) 0.072(3) 0.037(2) -0.017(2) 0.0103(18) -0.015(2) O5W 0.061(3) 0.041(2) 0.041(2) -0.0078(19) 0.011(2) 0.001(2) Er1 0.03263(14) 0.02858(15) 0.01837(13) -0.00020(9) 0.00871(10) -0.00214(9) C19 0.031(2) 0.028(3) 0.020(2) 0.002(2) 0.011(2) 0.002(2) C21 0.033(2) 0.019(2) 0.023(2) -0.0053(19) 0.013(2) -0.002(2) N13 0.028(2) 0.025(2) 0.027(2) -0.0013(17) 0.0113(17) -0.0023(17) C1 0.036(3) 0.021(2) 0.022(2) -0.0001(19) 0.013(2) -0.003(2) C2 0.033(3) 0.024(3) 0.019(2) -0.0020(19) 0.008(2) 0.001(2) C3 0.025(2) 0.023(2) 0.024(2) -0.008(2) 0.0090(19) 0.001(2) C4 0.039(3) 0.033(3) 0.022(2) -0.006(2) 0.016(2) 0.003(2) C5 0.037(3) 0.028(3) 0.026(3) 0.002(2) 0.008(2) 0.007(2) C6 0.041(3) 0.026(3) 0.024(2) 0.004(2) 0.016(2) 0.007(2) C7 0.030(2) 0.030(3) 0.025(2) -0.001(2) 0.009(2) 0.000(2) C8 0.033(3) 0.025(3) 0.024(2) -0.002(2) 0.007(2) 0.003(2) C9 0.030(2) 0.029(3) 0.026(3) 0.001(2) 0.008(2) -0.001(2) C10 0.046(3) 0.020(3) 0.034(3) 0.003(2) 0.013(2) 0.004(2) C11 0.035(3) 0.022(3) 0.028(3) 0.005(2) 0.009(2) 0.001(2) C12 0.042(3) 0.025(3) 0.031(3) -0.001(2) 0.016(2) -0.001(2) C13 0.021(2) 0.026(3) 0.026(3) 0.000(2) 0.0080(19) 0.0020(19) C14 0.026(2) 0.026(3) 0.020(2) 0.0062(19) 0.0099(19) 0.0026(19) C15 0.028(2) 0.026(3) 0.021(2) -0.0031(19) 0.007(2) 0.002(2) C16 0.030(3) 0.037(3) 0.025(3) -0.002(2) 0.008(2) 0.005(2) C17 0.029(2) 0.025(3) 0.021(2) 0.0021(19) 0.0073(19) 0.001(2) C18 0.033(3) 0.037(3) 0.019(2) -0.002(2) 0.009(2) -0.001(2) C20 0.035(3) 0.017(2) 0.031(3) 0.001(2) 0.012(2) 0.002(2) N1 0.033(2) 0.026(2) 0.0184(19) -0.0015(17) 0.0103(17) 0.0018(18) N2 0.030(2) 0.030(2) 0.0134(18) 0.0015(17) 0.0099(16) -0.0021(18) N3 0.039(2) 0.027(2) 0.024(2) 0.0070(18) 0.0149(18) 0.0050(19) N4 0.028(2) 0.035(2) 0.021(2) 0.0022(18) 0.0083(17) 0.0072(19) N5 0.042(2) 0.028(2) 0.019(2) 0.0026(17) 0.0140(17) 0.0064(19) N6 0.040(2) 0.024(2) 0.022(2) 0.0047(17) 0.0101(18) 0.0029(18) N7 0.038(2) 0.028(2) 0.024(2) 0.0036(18) 0.0076(18) 0.0086(19) N8 0.042(2) 0.024(2) 0.017(2) 0.0009(17) 0.0049(18) 0.0013(19) N9 0.030(2) 0.029(2) 0.020(2) -0.0019(17) 0.0074(17) -0.0030(18) N10 0.030(2) 0.029(2) 0.025(2) 0.0038(17) 0.0125(18) -0.0009(17) N11 0.031(2) 0.027(2) 0.026(2) 0.0041(18) 0.0085(18) 0.0011(18) N12 0.025(2) 0.027(2) 0.029(2) 0.0005(18) 0.0042(18) -0.0008(18) N14 0.0268(19) 0.030(2) 0.0199(19) 0.0045(17) 0.0117(16) 0.0000(17) O1 0.043(2) 0.034(2) 0.0181(17) -0.0012(15) 0.0103(15) 0.0016(17) O2 0.053(2) 0.037(2) 0.0274(18) 0.0085(16) 0.0239(16) 0.0059(18) O3 0.065(2) 0.039(2) 0.036(2) 0.0121(17) 0.0329(19) 0.003(2) O4 0.0366(19) 0.040(2) 0.0251(19) 0.0021(15) 0.0147(16) -0.0002(16) O5 0.0330(19) 0.036(2) 0.0194(17) 0.0054(14) 0.0092(15) -0.0006(15) O6 0.046(2) 0.040(2) 0.0247(19) 0.0061(17) 0.0033(17) -0.0061(18) O7 0.089(3) 0.036(2) 0.027(2) 0.0030(18) -0.005(2) 0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 Zn1 2.223(2) . ? Cl2 Zn1 2.222(2) . ? Cl3 Zn1 2.192(4) . ? Cl4 Zn1 2.374(6) . ? O1W Er1 2.374(4) . ? O2W Er1 2.306(4) . ? O3W Er1 2.317(4) . ? O4W Er1 2.352(4) . ? O5W Er1 2.380(4) . ? Er1 O4 2.313(4) 6_566 ? Er1 O5 2.360(3) 5_767 ? Er1 O1 2.375(3) . ? C19 N2 1.438(6) . ? C19 N4 1.449(7) 2_756 ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C21 O5 1.229(6) . ? C21 N14 1.349(6) . ? C21 N13 1.368(7) 2_756 ? N13 C21 1.368(7) 2_756 ? N13 C20 1.423(6) . ? N13 C17 1.452(6) . ? C1 O1 1.229(6) . ? C1 N2 1.364(7) . ? C1 N1 1.373(6) . ? C2 N1 1.464(6) . ? C2 N3 1.470(7) . ? C2 C3 1.547(7) . ? C2 H2 0.9900 . ? C3 N4 1.442(7) . ? C3 N2 1.480(6) . ? C3 H3 0.9900 . ? C4 O2 1.223(7) . ? C4 N3 1.355(7) . ? C4 N4 1.366(7) . ? C5 N3 1.437(6) . ? C5 N5 1.464(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.419(7) . ? C6 N1 1.444(7) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O3 1.209(7) . ? C7 N5 1.373(7) . ? C7 N6 1.380(7) . ? C8 N7 1.436(6) . ? C8 N5 1.460(7) . ? C8 C9 1.547(7) . ? C8 H8 0.9900 . ? C9 N6 1.435(7) . ? C9 N8 1.471(6) . ? C9 H9 0.9900 . ? C10 O7 1.205(7) . ? C10 N8 1.368(7) . ? C10 N7 1.375(7) . ? C11 N6 1.436(6) . ? C11 N9 1.456(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.432(7) . ? C12 N11 1.439(7) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O4 1.255(7) . ? C13 N10 1.339(7) . ? C13 N9 1.359(7) . ? C14 N11 1.453(6) . ? C14 N9 1.456(7) . ? C14 C15 1.537(7) . ? C14 H14 0.9900 . ? C15 N10 1.447(7) . ? C15 N12 1.455(6) . ? C15 H15 0.9900 . ? C16 O6 1.230(6) . ? C16 N11 1.366(7) . ? C16 N12 1.368(7) . ? C17 N10 1.433(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.434(7) . ? C18 N14 1.462(7) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C20 N14 1.460(7) . ? C20 C20 1.553(10) 2_756 ? C20 H20 0.9900 . ? N4 C19 1.449(7) 2_756 ? O4 Er1 2.313(4) 6_565 ? O5 Er1 2.360(3) 5_767 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl3 Zn1 Cl2 112.64(14) . . ? Cl3 Zn1 Cl1 111.65(11) . . ? Cl2 Zn1 Cl1 113.20(9) . . ? Cl3 Zn1 Cl4 105.5(2) . . ? Cl2 Zn1 Cl4 111.13(16) . . ? Cl1 Zn1 Cl4 101.93(17) . . ? O2W Er1 O4 147.13(13) . 6_566 ? O2W Er1 O3W 107.27(16) . . ? O4 Er1 O3W 78.84(14) 6_566 . ? O2W Er1 O4W 140.87(15) . . ? O4 Er1 O4W 70.98(14) 6_566 . ? O3W Er1 O4W 83.86(16) . . ? O2W Er1 O5 76.00(14) . 5_767 ? O4 Er1 O5 80.45(13) 6_566 5_767 ? O3W Er1 O5 143.01(13) . 5_767 ? O4W Er1 O5 117.44(15) . 5_767 ? O2W Er1 O1W 75.43(16) . . ? O4 Er1 O1W 76.29(15) 6_566 . ? O3W Er1 O1W 71.38(14) . . ? O4W Er1 O1W 142.12(16) . . ? O5 Er1 O1W 74.13(13) 5_767 . ? O2W Er1 O1 72.59(13) . . ? O4 Er1 O1 137.59(13) 6_566 . ? O3W Er1 O1 71.87(13) . . ? O4W Er1 O1 75.92(14) . . ? O5 Er1 O1 139.67(13) 5_767 . ? O1W Er1 O1 120.16(14) . . ? O2W Er1 O5W 80.33(16) . . ? O4 Er1 O5W 113.36(15) 6_566 . ? O3W Er1 O5W 145.47(13) . . ? O4W Er1 O5W 71.28(16) . . ? O5 Er1 O5W 71.33(13) 5_767 . ? O1W Er1 O5W 141.57(14) . . ? O1 Er1 O5W 78.95(14) . . ? N2 C19 N4 114.2(4) . 2_756 ? N2 C19 H19A 108.7 . . ? N4 C19 H19A 108.7 2_756 . ? N2 C19 H19B 108.7 . . ? N4 C19 H19B 108.7 2_756 . ? H19A C19 H19B 107.6 . . ? O5 C21 N14 125.4(5) . . ? O5 C21 N13 125.9(5) . 2_756 ? N14 C21 N13 108.7(4) . 2_756 ? C21 N13 C20 112.2(4) 2_756 . ? C21 N13 C17 122.4(4) 2_756 . ? C20 N13 C17 125.1(4) . . ? O1 C1 N2 125.7(5) . . ? O1 C1 N1 125.5(5) . . ? N2 C1 N1 108.7(4) . . ? N1 C2 N3 113.9(4) . . ? N1 C2 C3 103.8(4) . . ? N3 C2 C3 102.4(4) . . ? N1 C2 H2 112.0 . . ? N3 C2 H2 112.0 . . ? C3 C2 H2 112.0 . . ? N4 C3 N2 114.1(4) . . ? N4 C3 C2 104.0(4) . . ? N2 C3 C2 102.8(4) . . ? N4 C3 H3 111.8 . . ? N2 C3 H3 111.8 . . ? C2 C3 H3 111.8 . . ? O2 C4 N3 125.8(5) . . ? O2 C4 N4 125.4(5) . . ? N3 C4 N4 108.8(5) . . ? N3 C5 N5 113.6(4) . . ? N3 C5 H5A 108.8 . . ? N5 C5 H5A 108.8 . . ? N3 C5 H5B 108.8 . . ? N5 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N7 C6 N1 114.6(5) . . ? N7 C6 H6A 108.6 . . ? N1 C6 H6A 108.6 . . ? N7 C6 H6B 108.6 . . ? N1 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? O3 C7 N5 126.4(5) . . ? O3 C7 N6 126.5(5) . . ? N5 C7 N6 107.0(4) . . ? N7 C8 N5 113.9(4) . . ? N7 C8 C9 104.7(4) . . ? N5 C8 C9 102.0(4) . . ? N7 C8 H8 111.9 . . ? N5 C8 H8 111.9 . . ? C9 C8 H8 111.9 . . ? N6 C9 N8 114.3(4) . . ? N6 C9 C8 104.3(4) . . ? N8 C9 C8 102.1(4) . . ? N6 C9 H9 111.8 . . ? N8 C9 H9 111.8 . . ? C8 C9 H9 111.8 . . ? O7 C10 N8 124.7(5) . . ? O7 C10 N7 126.8(5) . . ? N8 C10 N7 108.5(4) . . ? N6 C11 N9 112.1(4) . . ? N6 C11 H11A 109.2 . . ? N9 C11 H11A 109.2 . . ? N6 C11 H11B 109.2 . . ? N9 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? N8 C12 N11 113.8(5) . . ? N8 C12 H12A 108.8 . . ? N11 C12 H12A 108.8 . . ? N8 C12 H12B 108.8 . . ? N11 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O4 C13 N10 125.3(5) . . ? O4 C13 N9 125.0(5) . . ? N10 C13 N9 109.6(5) . . ? N11 C14 N9 113.0(4) . . ? N11 C14 C15 103.9(4) . . ? N9 C14 C15 103.4(4) . . ? N11 C14 H14 112.0 . . ? N9 C14 H14 112.0 . . ? C15 C14 H14 112.0 . . ? N10 C15 N12 114.4(4) . . ? N10 C15 C14 103.1(4) . . ? N12 C15 C14 103.4(4) . . ? N10 C15 H15 111.8 . . ? N12 C15 H15 111.8 . . ? C14 C15 H15 111.8 . . ? O6 C16 N11 124.3(5) . . ? O6 C16 N12 126.7(5) . . ? N11 C16 N12 109.0(4) . . ? N10 C17 N13 113.8(4) . . ? N10 C17 H17A 108.8 . . ? N13 C17 H17A 108.8 . . ? N10 C17 H17B 108.8 . . ? N13 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? N12 C18 N14 114.2(4) . . ? N12 C18 H18A 108.7 . . ? N14 C18 H18A 108.7 . . ? N12 C18 H18B 108.7 . . ? N14 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? N13 C20 N14 116.3(4) . . ? N13 C20 C20 103.0(5) . 2_756 ? N14 C20 C20 102.4(4) . 2_756 ? N13 C20 H20 111.5 . . ? N14 C20 H20 111.5 . . ? C20 C20 H20 111.5 2_756 . ? C1 N1 C6 124.9(4) . . ? C1 N1 C2 112.2(4) . . ? C6 N1 C2 122.4(4) . . ? C1 N2 C19 124.6(4) . . ? C1 N2 C3 112.3(4) . . ? C19 N2 C3 123.1(4) . . ? C4 N3 C5 121.7(4) . . ? C4 N3 C2 112.2(4) . . ? C5 N3 C2 121.9(4) . . ? C4 N4 C3 112.3(4) . . ? C4 N4 C19 122.5(4) . 2_756 ? C3 N4 C19 123.3(4) . 2_756 ? C7 N5 C8 113.2(4) . . ? C7 N5 C5 121.4(4) . . ? C8 N5 C5 122.3(4) . . ? C7 N6 C11 121.5(4) . . ? C7 N6 C9 112.7(4) . . ? C11 N6 C9 123.5(4) . . ? C10 N7 C6 123.0(4) . . ? C10 N7 C8 112.0(4) . . ? C6 N7 C8 123.8(4) . . ? C10 N8 C12 121.4(4) . . ? C10 N8 C9 112.1(4) . . ? C12 N8 C9 122.2(4) . . ? C13 N9 C11 121.7(4) . . ? C13 N9 C14 111.2(4) . . ? C11 N9 C14 123.8(4) . . ? C13 N10 C17 123.8(5) . . ? C13 N10 C15 112.5(4) . . ? C17 N10 C15 123.5(4) . . ? C16 N11 C12 122.4(4) . . ? C16 N11 C14 111.6(4) . . ? C12 N11 C14 122.0(4) . . ? C16 N12 C18 121.9(4) . . ? C16 N12 C15 111.6(4) . . ? C18 N12 C15 124.1(4) . . ? C21 N14 C20 111.8(4) . . ? C21 N14 C18 122.5(4) . . ? C20 N14 C18 124.5(4) . . ? C1 O1 Er1 147.8(4) . . ? C13 O4 Er1 150.4(3) . 6_565 ? C21 O5 Er1 159.7(4) . 5_767 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 4.340 _refine_diff_density_min -3.660 _refine_diff_density_rms 0.175 data_p11 _database_code_depnum_ccdc_archive 'CCDC 905592' #TrackingRef '9 (905592).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H58 Cl5 N14 O25.50 Tm Zn' _chemical_formula_weight 1326.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.4242(16) _cell_length_b 18.8983(11) _cell_length_c 19.8907(11) _cell_angle_alpha 90.00 _cell_angle_beta 104.698(2) _cell_angle_gamma 90.00 _cell_volume 9607.8(10) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.834 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5360 _exptl_absorpt_coefficient_mu 2.709 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5176 _exptl_absorpt_correction_T_max 0.5747 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45548 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9378 _reflns_number_gt 7433 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1183P)^2^+72.7058P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9378 _refine_ls_number_parameters 488 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1911 _refine_ls_wR_factor_gt 0.1817 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl5 Cl 0.22365(11) 0.27835(15) -0.35700(16) 0.0812(8) Uani 1 1 d . . . Cl1 Cl 0.32545(7) 0.15345(10) -0.20404(11) 0.0501(5) Uani 1 1 d . . . Cl2 Cl 0.31616(11) -0.03621(13) -0.25236(18) 0.0904(8) Uani 1 1 d . . . Cl3 Cl 0.44292(14) 0.05519(19) -0.2076(4) 0.165(3) Uani 1 1 d . . . Cl4 Cl 0.3730(4) 0.0301(4) -0.0695(4) 0.210(4) Uani 1 1 d U . . Zn1 Zn 0.36487(6) 0.04914(7) -0.19403(15) 0.1495(10) Uani 1 1 d . . . O1W O -0.01319(18) 0.2003(3) -0.0046(2) 0.0400(12) Uani 1 1 d . . . O2W O 0.0389(2) 0.1354(2) -0.0971(2) 0.0416(12) Uani 1 1 d . . . O3W O 0.11378(19) 0.1069(2) 0.0212(2) 0.0389(11) Uani 1 1 d . . . O4W O 0.15122(18) 0.2593(3) 0.0633(3) 0.0458(13) Uani 1 1 d . . . O5W O 0.0562(2) 0.3259(3) 0.0387(3) 0.0436(12) Uani 1 1 d . . . Tm1 Tm 0.072736(9) 0.214606(13) -0.005053(12) 0.02364(8) Uani 1 1 d . . . C1 C 0.1443(2) 0.2252(3) -0.1269(3) 0.0228(13) Uani 1 1 d . . . C2 C 0.1823(2) 0.2058(3) -0.2188(3) 0.0224(12) Uani 1 1 d . . . H2 H 0.2202 0.2124 -0.2140 0.027 Uiso 1 1 calc R . . C3 C 0.1520(2) 0.2765(3) -0.2295(3) 0.0247(13) Uani 1 1 d . . . H3 H 0.1751 0.3167 -0.2337 0.030 Uiso 1 1 calc R . . C4 C 0.1182(2) 0.2016(3) -0.3246(3) 0.0254(13) Uani 1 1 d . . . C5 C 0.1083(2) 0.3449(3) -0.1504(3) 0.0241(12) Uani 1 1 d . . . H5A H 0.1251 0.3867 -0.1644 0.029 Uiso 1 1 calc R . . H5B H 0.1145 0.3461 -0.0997 0.029 Uiso 1 1 calc R . . C6 C 0.0787(2) 0.3197(3) -0.3311(3) 0.0277(13) Uani 1 1 d . . . H6A H 0.0682 0.3073 -0.3805 0.033 Uiso 1 1 calc R . . H6B H 0.0990 0.3636 -0.3267 0.033 Uiso 1 1 calc R . . C7 C 0.0164(2) 0.3180(3) -0.1527(3) 0.0257(13) Uani 1 1 d . . . C8 C 0.0296(2) 0.3785(3) -0.2489(3) 0.0243(13) Uani 1 1 d . . . H8 H 0.0428 0.4267 -0.2541 0.029 Uiso 1 1 calc R . . C9 C 0.1846(2) 0.1072(3) -0.3042(3) 0.0292(14) Uani 1 1 d . . . H9A H 0.1707 0.1021 -0.3546 0.035 Uiso 1 1 calc R . . H9B H 0.2219 0.1186 -0.2952 0.035 Uiso 1 1 calc R . . C10 C 0.2023(2) 0.1226(3) -0.1156(3) 0.0280(14) Uani 1 1 d . . . H10A H 0.1975 0.1236 -0.0683 0.034 Uiso 1 1 calc R . . H10B H 0.2394 0.1311 -0.1125 0.034 Uiso 1 1 calc R . . C11 C 0.1620(2) -0.0183(3) -0.3089(3) 0.0307(14) Uani 1 1 d . . . C12 C 0.2094(2) 0.0242(3) -0.2000(3) 0.0244(13) Uani 1 1 d . . . H12 H 0.2469 0.0363 -0.1930 0.029 Uiso 1 1 calc R . . C13 C 0.2009(2) -0.0572(3) -0.1959(3) 0.0257(13) Uani 1 1 d . . . H13 H 0.2343 -0.0833 -0.1798 0.031 Uiso 1 1 calc R . . C14 C 0.1649(2) 0.0023(3) -0.1147(3) 0.0280(13) Uani 1 1 d . . . C15 C 0.1685(2) -0.1475(3) -0.2896(3) 0.0290(13) Uani 1 1 d . . . H15A H 0.2001 -0.1738 -0.2667 0.035 Uiso 1 1 calc R . . H15B H 0.1660 -0.1474 -0.3396 0.035 Uiso 1 1 calc R . . C16 C 0.1589(2) -0.1273(3) -0.1148(3) 0.0291(14) Uani 1 1 d . . . H16A H 0.1908 -0.1560 -0.1057 0.035 Uiso 1 1 calc R . . H16B H 0.1510 -0.1180 -0.0700 0.035 Uiso 1 1 calc R . . C17 C 0.0804(2) -0.2018(3) -0.3280(3) 0.0233(13) Uani 1 1 d . . . C18 C 0.1239(2) -0.2165(3) -0.2113(3) 0.0232(13) Uani 1 1 d . . . H18 H 0.1554 -0.2462 -0.1940 0.028 Uiso 1 1 calc R . . C19 C 0.0733(2) -0.2613(3) -0.2270(3) 0.0228(12) Uani 1 1 d . . . H19 H 0.0811 -0.3124 -0.2205 0.027 Uiso 1 1 calc R . . C20 C 0.0715(2) -0.1812(3) -0.1386(3) 0.0272(13) Uani 1 1 d . . . C21 C -0.0014(2) -0.2707(3) -0.3372(3) 0.0261(13) Uani 1 1 d . . . H21A H -0.0033 -0.3211 -0.3265 0.031 Uiso 1 1 calc R . . H21B H -0.0045 -0.2666 -0.3872 0.031 Uiso 1 1 calc R . . N1 N 0.17155(19) 0.1788(3) -0.1557(2) 0.0245(11) Uani 1 1 d . . . N2 N 0.1325(2) 0.2829(2) -0.1695(3) 0.0258(11) Uani 1 1 d . . . N3 N 0.15759(19) 0.1653(2) -0.2798(2) 0.0255(11) Uani 1 1 d . . . N4 N 0.11171(19) 0.2648(3) -0.2943(3) 0.0263(11) Uani 1 1 d . . . N5 N 0.05264(18) 0.3490(2) -0.1812(2) 0.0237(11) Uani 1 1 d . . . N6 N 0.03164(18) 0.3328(3) -0.3072(2) 0.0237(11) Uani 1 1 d . . . N7 N 0.1788(2) 0.0408(3) -0.2710(2) 0.0273(11) Uani 1 1 d . . . N8 N 0.1735(2) -0.0762(3) -0.2648(3) 0.0303(12) Uani 1 1 d . . . N9 N 0.18802(19) 0.0534(3) -0.1454(2) 0.0266(11) Uani 1 1 d . . . N11 N 0.12355(18) -0.1839(3) -0.2776(2) 0.0233(10) Uani 1 1 d . . . N12 N 0.04867(18) -0.2442(3) -0.3002(2) 0.0248(11) Uani 1 1 d . . . N13 N 0.11627(19) -0.1673(3) -0.1582(2) 0.0277(11) Uani 1 1 d . . . N14 N 0.04507(19) -0.2353(3) -0.1785(2) 0.0252(11) Uani 1 1 d . . . N19 N 0.1687(2) -0.0603(3) -0.1453(2) 0.0275(11) Uani 1 1 d . . . O1 O 0.13354(17) 0.2179(2) -0.0706(2) 0.0298(10) Uani 1 1 d . . . O2 O 0.02668(16) 0.2839(2) -0.0982(2) 0.0271(10) Uani 1 1 d . . . O3 O 0.09323(18) 0.1808(2) -0.3815(2) 0.0356(11) Uani 1 1 d . . . O4 O 0.1399(2) -0.0196(3) -0.3697(2) 0.0470(14) Uani 1 1 d . . . O5 O 0.07088(16) -0.1845(2) -0.3899(2) 0.0293(10) Uani 1 1 d . . . O6 O 0.05704(18) -0.1501(2) -0.0926(2) 0.0363(11) Uani 1 1 d . . . O7 O 0.14534(19) 0.0121(2) -0.0652(2) 0.0404(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl5 0.0770(15) 0.0932(18) 0.0812(17) -0.0047(13) 0.0344(13) -0.0363(13) Cl1 0.0534(10) 0.0374(9) 0.0640(12) -0.0096(8) 0.0232(9) -0.0081(8) Cl2 0.0886(15) 0.0502(12) 0.153(2) -0.0358(14) 0.0682(16) -0.0101(12) Cl3 0.078(2) 0.078(2) 0.362(11) -0.102(4) 0.108(4) -0.0120(17) Cl4 0.201(7) 0.217(6) 0.194(5) 0.076(5) 0.032(5) 0.019(5) Zn1 0.0653(8) 0.0457(7) 0.320(3) -0.0149(11) 0.0162(13) 0.0027(6) O1W 0.034(2) 0.063(3) 0.022(2) 0.003(2) 0.0038(19) -0.012(2) O2W 0.063(3) 0.032(2) 0.026(2) -0.0082(19) 0.004(2) -0.008(2) O3W 0.059(3) 0.036(2) 0.026(2) 0.0041(19) 0.018(2) 0.009(2) O4W 0.037(2) 0.067(3) 0.035(3) -0.018(2) 0.010(2) -0.014(2) O5W 0.056(3) 0.035(3) 0.040(3) -0.007(2) 0.011(2) -0.001(2) Tm1 0.02855(14) 0.02740(15) 0.01579(13) -0.00069(9) 0.00711(10) -0.00267(10) C1 0.021(3) 0.028(3) 0.019(3) -0.002(2) 0.005(2) -0.003(2) C2 0.021(3) 0.029(3) 0.018(3) -0.002(2) 0.007(2) -0.001(2) C3 0.024(3) 0.026(3) 0.026(3) 0.000(2) 0.010(2) -0.004(2) C4 0.024(3) 0.033(3) 0.019(3) 0.002(2) 0.005(2) -0.005(2) C5 0.030(3) 0.022(3) 0.022(3) 0.000(2) 0.010(2) -0.001(2) C6 0.032(3) 0.034(3) 0.018(3) 0.003(2) 0.009(2) 0.001(3) C7 0.027(3) 0.020(3) 0.032(3) -0.005(2) 0.012(2) -0.001(2) C8 0.033(3) 0.022(3) 0.017(3) 0.002(2) 0.007(2) -0.005(2) C9 0.038(3) 0.024(3) 0.027(3) 0.000(2) 0.011(3) -0.003(2) C10 0.029(3) 0.027(3) 0.024(3) -0.002(2) 0.000(2) 0.003(2) C11 0.035(3) 0.030(3) 0.027(3) 0.005(3) 0.007(3) 0.000(3) C12 0.027(3) 0.024(3) 0.023(3) -0.002(2) 0.009(2) -0.004(2) C13 0.033(3) 0.022(3) 0.022(3) -0.003(2) 0.006(2) -0.004(2) C14 0.036(3) 0.030(3) 0.019(3) 0.003(2) 0.009(2) 0.001(3) C15 0.038(3) 0.032(3) 0.021(3) -0.009(2) 0.013(2) -0.010(3) C16 0.038(3) 0.029(3) 0.020(3) -0.005(2) 0.006(2) -0.005(3) C17 0.032(3) 0.017(3) 0.023(3) 0.000(2) 0.010(2) 0.000(2) C18 0.025(3) 0.028(3) 0.017(3) 0.003(2) 0.007(2) 0.000(2) C19 0.028(3) 0.025(3) 0.017(3) 0.003(2) 0.006(2) 0.000(2) C20 0.034(3) 0.027(3) 0.022(3) 0.002(2) 0.010(2) -0.004(2) C21 0.028(3) 0.031(3) 0.020(3) 0.000(2) 0.008(2) 0.000(2) N1 0.029(2) 0.026(2) 0.018(2) 0.0008(19) 0.0051(19) 0.000(2) N2 0.029(2) 0.029(3) 0.022(2) -0.0020(19) 0.011(2) 0.0038(19) N3 0.029(2) 0.022(2) 0.024(2) -0.0004(19) 0.004(2) 0.0001(19) N4 0.027(2) 0.026(2) 0.026(3) 0.000(2) 0.005(2) 0.001(2) N5 0.027(2) 0.023(2) 0.023(2) -0.0002(19) 0.0094(19) 0.0007(19) N6 0.026(2) 0.031(3) 0.016(2) -0.0031(19) 0.0082(18) -0.0014(19) N7 0.038(3) 0.024(2) 0.020(2) 0.0017(19) 0.008(2) 0.003(2) N8 0.038(3) 0.027(3) 0.029(3) -0.002(2) 0.015(2) -0.006(2) N9 0.036(3) 0.027(3) 0.018(2) -0.0025(19) 0.009(2) 0.001(2) N11 0.029(2) 0.026(2) 0.018(2) -0.0008(19) 0.0120(19) 0.001(2) N12 0.027(2) 0.032(3) 0.016(2) -0.001(2) 0.0064(18) 0.000(2) N13 0.034(2) 0.030(3) 0.022(2) -0.008(2) 0.013(2) -0.008(2) N14 0.027(2) 0.031(3) 0.018(2) -0.001(2) 0.0078(19) -0.005(2) N19 0.042(3) 0.025(2) 0.019(2) -0.0017(19) 0.014(2) -0.007(2) O1 0.031(2) 0.040(2) 0.021(2) 0.0032(17) 0.0123(17) 0.0021(17) O2 0.030(2) 0.039(2) 0.0125(19) 0.0096(16) 0.0061(16) -0.0006(17) O3 0.040(2) 0.037(2) 0.027(2) -0.0072(19) 0.0022(19) 0.001(2) O4 0.076(3) 0.036(3) 0.022(2) 0.000(2) 0.000(2) -0.009(2) O5 0.035(2) 0.034(2) 0.020(2) 0.0014(17) 0.0083(17) 0.0003(18) O6 0.050(2) 0.036(2) 0.030(2) -0.0075(19) 0.0241(19) -0.004(2) O7 0.056(3) 0.040(3) 0.033(2) -0.008(2) 0.026(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 Zn1 2.215(2) . ? Cl2 Zn1 2.202(3) . ? Cl3 Zn1 2.150(4) . ? Cl4 Zn1 2.459(8) . ? O1W Tm1 2.289(5) . ? O2W Tm1 2.358(4) . ? O3W Tm1 2.304(4) . ? O4W Tm1 2.331(5) . ? O5W Tm1 2.358(5) . ? Tm1 O1 2.312(4) . ? Tm1 O2 2.342(4) . ? Tm1 O5 2.372(4) 6_556 ? C1 O1 1.232(7) . ? C1 N1 1.351(8) . ? C1 N2 1.367(7) . ? C2 N3 1.444(7) . ? C2 N1 1.446(7) . ? C2 C3 1.545(8) . ? C2 H2 0.9900 . ? C3 N2 1.422(8) . ? C3 N4 1.466(7) . ? C3 H3 0.9900 . ? C4 O3 1.221(7) . ? C4 N4 1.368(8) . ? C4 N3 1.371(7) . ? C5 N2 1.430(7) . ? C5 N5 1.445(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.433(8) . ? C6 N6 1.460(8) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.231(7) . ? C7 N6 1.347(7) 2_554 ? C7 N5 1.362(7) . ? C8 N5 1.442(7) . ? C8 N6 1.457(7) . ? C8 C8 1.555(12) 2_554 ? C8 H8 0.9900 . ? C9 N7 1.444(8) . ? C9 N3 1.457(8) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 N1 1.447(7) . ? C10 N9 1.447(7) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 O4 1.202(8) . ? C11 N7 1.358(8) . ? C11 N8 1.387(8) . ? C12 N9 1.455(7) . ? C12 N7 1.472(7) . ? C12 C13 1.560(8) . ? C12 H12 0.9900 . ? C13 N8 1.425(7) . ? C13 N19 1.477(8) . ? C13 H13 0.9900 . ? C14 O7 1.236(8) . ? C14 N19 1.346(8) . ? C14 N9 1.367(8) . ? C15 N8 1.430(8) . ? C15 N11 1.443(8) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 N13 1.448(7) . ? C16 N19 1.456(8) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 O5 1.236(7) . ? C17 N11 1.357(7) . ? C17 N12 1.373(8) . ? C18 N11 1.453(7) . ? C18 N13 1.459(7) . ? C18 C19 1.545(8) . ? C18 H18 0.9900 . ? C19 N14 1.448(8) . ? C19 N12 1.472(7) . ? C19 H19 0.9900 . ? C20 O6 1.228(7) . ? C20 N13 1.362(8) . ? C20 N14 1.371(8) . ? C21 N12 1.433(7) . ? C21 N14 1.434(8) 2_554 ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? N6 C7 1.347(7) 2_554 ? N14 C21 1.434(8) 2_554 ? O5 Tm1 2.372(4) 6 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl3 Zn1 Cl2 115.08(18) . . ? Cl3 Zn1 Cl1 112.69(14) . . ? Cl2 Zn1 Cl1 113.95(11) . . ? Cl3 Zn1 Cl4 107.1(3) . . ? Cl2 Zn1 Cl4 108.3(2) . . ? Cl1 Zn1 Cl4 98.0(2) . . ? O1W Tm1 O3W 107.78(18) . . ? O1W Tm1 O1 146.87(15) . . ? O3W Tm1 O1 78.28(16) . . ? O1W Tm1 O4W 140.98(17) . . ? O3W Tm1 O4W 83.70(19) . . ? O1 Tm1 O4W 71.13(16) . . ? O1W Tm1 O2 75.66(16) . . ? O3W Tm1 O2 142.54(15) . . ? O1 Tm1 O2 80.50(15) . . ? O4W Tm1 O2 117.74(17) . . ? O1W Tm1 O5W 80.04(18) . . ? O3W Tm1 O5W 145.60(16) . . ? O1 Tm1 O5W 113.83(16) . . ? O4W Tm1 O5W 71.46(18) . . ? O2 Tm1 O5W 71.66(16) . . ? O1W Tm1 O2W 75.39(18) . . ? O3W Tm1 O2W 71.26(16) . . ? O1 Tm1 O2W 76.10(17) . . ? O4W Tm1 O2W 142.07(18) . . ? O2 Tm1 O2W 73.88(16) . . ? O5W Tm1 O2W 141.56(17) . . ? O1W Tm1 O5 72.79(15) . 6_556 ? O3W Tm1 O5 72.12(15) . 6_556 ? O1 Tm1 O5 137.56(14) . 6_556 ? O4W Tm1 O5 75.94(16) . 6_556 ? O2 Tm1 O5 139.82(15) . 6_556 ? O5W Tm1 O5 78.87(16) . 6_556 ? O2W Tm1 O5 120.05(16) . 6_556 ? O1 C1 N1 125.8(5) . . ? O1 C1 N2 125.7(5) . . ? N1 C1 N2 108.6(5) . . ? N3 C2 N1 113.4(5) . . ? N3 C2 C3 103.6(4) . . ? N1 C2 C3 102.5(5) . . ? N3 C2 H2 112.2 . . ? N1 C2 H2 112.2 . . ? C3 C2 H2 112.2 . . ? N2 C3 N4 114.4(5) . . ? N2 C3 C2 104.1(5) . . ? N4 C3 C2 103.0(4) . . ? N2 C3 H3 111.6 . . ? N4 C3 H3 111.6 . . ? C2 C3 H3 111.6 . . ? O3 C4 N4 126.3(6) . . ? O3 C4 N3 125.7(6) . . ? N4 C4 N3 108.0(5) . . ? N2 C5 N5 114.0(5) . . ? N2 C5 H5A 108.8 . . ? N5 C5 H5A 108.8 . . ? N2 C5 H5B 108.8 . . ? N5 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N4 C6 N6 114.5(5) . . ? N4 C6 H6A 108.6 . . ? N6 C6 H6A 108.6 . . ? N4 C6 H6B 108.6 . . ? N6 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? O2 C7 N6 126.4(5) . 2_554 ? O2 C7 N5 124.8(5) . . ? N6 C7 N5 108.7(5) 2_554 . ? N5 C8 N6 115.0(5) . . ? N5 C8 C8 102.0(5) . 2_554 ? N6 C8 C8 102.6(4) . 2_554 ? N5 C8 H8 112.1 . . ? N6 C8 H8 112.1 . . ? C8 C8 H8 112.1 2_554 . ? N7 C9 N3 112.6(5) . . ? N7 C9 H9A 109.1 . . ? N3 C9 H9A 109.1 . . ? N7 C9 H9B 109.1 . . ? N3 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? N1 C10 N9 112.7(5) . . ? N1 C10 H10A 109.1 . . ? N9 C10 H10A 109.1 . . ? N1 C10 H10B 109.1 . . ? N9 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? O4 C11 N7 125.7(6) . . ? O4 C11 N8 126.3(6) . . ? N7 C11 N8 108.0(5) . . ? N9 C12 N7 114.3(5) . . ? N9 C12 C13 104.3(5) . . ? N7 C12 C13 102.1(4) . . ? N9 C12 H12 111.9 . . ? N7 C12 H12 111.9 . . ? C13 C12 H12 111.9 . . ? N8 C13 N19 113.9(5) . . ? N8 C13 C12 104.1(5) . . ? N19 C13 C12 100.9(4) . . ? N8 C13 H13 112.3 . . ? N19 C13 H13 112.3 . . ? C12 C13 H13 112.3 . . ? O7 C14 N19 125.8(6) . . ? O7 C14 N9 125.1(6) . . ? N19 C14 N9 109.0(5) . . ? N8 C15 N11 113.6(5) . . ? N8 C15 H15A 108.8 . . ? N11 C15 H15A 108.8 . . ? N8 C15 H15B 108.8 . . ? N11 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? N13 C16 N19 113.5(5) . . ? N13 C16 H16A 108.9 . . ? N19 C16 H16A 108.9 . . ? N13 C16 H16B 108.9 . . ? N19 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? O5 C17 N11 126.2(5) . . ? O5 C17 N12 124.5(5) . . ? N11 C17 N12 109.4(5) . . ? N11 C18 N13 114.6(5) . . ? N11 C18 C19 104.1(4) . . ? N13 C18 C19 102.9(5) . . ? N11 C18 H18 111.6 . . ? N13 C18 H18 111.6 . . ? C19 C18 H18 111.6 . . ? N14 C19 N12 114.3(5) . . ? N14 C19 C18 104.2(4) . . ? N12 C19 C18 102.9(4) . . ? N14 C19 H19 111.6 . . ? N12 C19 H19 111.6 . . ? C18 C19 H19 111.6 . . ? O6 C20 N13 125.3(5) . . ? O6 C20 N14 125.4(6) . . ? N13 C20 N14 109.3(5) . . ? N12 C21 N14 114.4(5) . 2_554 ? N12 C21 H21A 108.6 . . ? N14 C21 H21A 108.6 2_554 . ? N12 C21 H21B 108.6 . . ? N14 C21 H21B 108.6 2_554 . ? H21A C21 H21B 107.6 . . ? C1 N1 C2 112.5(5) . . ? C1 N1 C10 121.7(5) . . ? C2 N1 C10 122.1(5) . . ? C1 N2 C3 112.2(5) . . ? C1 N2 C5 122.5(5) . . ? C3 N2 C5 125.0(5) . . ? C4 N3 C2 112.8(5) . . ? C4 N3 C9 121.1(5) . . ? C2 N3 C9 121.6(5) . . ? C4 N4 C6 122.3(5) . . ? C4 N4 C3 112.1(5) . . ? C6 N4 C3 123.5(5) . . ? C7 N5 C8 112.4(5) . . ? C7 N5 C5 123.2(5) . . ? C8 N5 C5 124.0(5) . . ? C7 N6 C8 112.0(5) 2_554 . ? C7 N6 C6 121.7(5) 2_554 . ? C8 N6 C6 124.4(5) . . ? C11 N7 C9 121.2(5) . . ? C11 N7 C12 112.3(5) . . ? C9 N7 C12 121.9(5) . . ? C11 N8 C13 112.7(5) . . ? C11 N8 C15 122.7(5) . . ? C13 N8 C15 123.3(5) . . ? C14 N9 C10 123.7(5) . . ? C14 N9 C12 111.6(5) . . ? C10 N9 C12 122.6(5) . . ? C17 N11 C15 124.7(5) . . ? C17 N11 C18 112.0(5) . . ? C15 N11 C18 122.4(5) . . ? C17 N12 C21 125.2(5) . . ? C17 N12 C19 111.4(5) . . ? C21 N12 C19 123.4(5) . . ? C20 N13 C16 122.1(5) . . ? C20 N13 C18 112.0(5) . . ? C16 N13 C18 122.4(5) . . ? C20 N14 C21 122.9(5) . 2_554 ? C20 N14 C19 111.4(5) . . ? C21 N14 C19 124.4(5) 2_554 . ? C14 N19 C16 122.4(5) . . ? C14 N19 C13 113.3(5) . . ? C16 N19 C13 120.8(5) . . ? C1 O1 Tm1 150.5(4) . . ? C7 O2 Tm1 160.7(4) . . ? C17 O5 Tm1 148.1(4) . 6 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 3.874 _refine_diff_density_min -4.386 _refine_diff_density_rms 0.176 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.007 472 124 ' ' 2 0.311 -0.145 0.000 1196 416 ' ' 3 0.332 0.119 0.500 1196 416 ' ' 4 0.500 0.500 0.284 472 124 ' ' _platon_squeeze_details ; ;