Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Professor Dirk Volkmer' _publ_contact_author_address ;University of Ulm Inorganic Chemistry 2: Institute of Materials and Catalysis Albert-Einstein-Allee 11 D-89081 Ulm Germany ; _publ_contact_author_email dirk.volkmer@uni-ulm.de _publ_contact_author_phone '49 (0)731 50 23921' _publ_contact_author_fax '49 (0)731 50 23039' loop_ _publ_author_name _publ_author_address D.Volkmer ;University of Ulm Inorganic Chemistry 2: Institute of Materials and Catalysis Albert-Einstein-Allee 11 D-89081 Ulm Germany ; B.Bredenkotter ;University of Ulm Inorganic Chemistry 2: Institute of Materials and Catalysis Albert-Einstein-Allee 11 D-89081 Ulm Germany ; B.Rieger ;University of Ulm Inorganic Chemistry 2: Institute of Materials and Catalysis Albert-Einstein-Allee 11 D-89081 Ulm Germany ; Y.Wang ;Key Laboratory of Polyoxometalate Science of Ministry of Education Faculty of Chemistry Northeast Normal University Changchun, 130024, P.R. China ; data_wan573 _database_code_depnum_ccdc_archive 'CCDC 613447' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H38 Co N2 O14 Zn2, 4(C3 H7 N O)' _chemical_formula_sum 'C60 H66 Co N6 O18 Zn2' _chemical_formula_weight 1348.86 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' Co Co 0.3494 0.9721 '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 'P 21/n' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 20.463(4) _cell_length_b 14.819(3) _cell_length_c 23.023(5) _cell_angle_alpha 90.00 _cell_angle_beta 111.75(3) _cell_angle_gamma 90.00 _cell_volume 6484(2) _cell_formula_units_Z 4 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 1510 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 26.1 _exptl_crystal_description block-shaped _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2796 _exptl_absorpt_coefficient_mu 1.059 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50279 _diffrn_reflns_av_R_equivalents 0.0800 _diffrn_reflns_av_sigmaI/netI 0.0860 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.98 _reflns_number_total 12574 _reflns_number_gt 6790 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE EXPOSE' _computing_cell_refinement 'STOE CELL' _computing_data_reduction 'STOE INTEGRATE' _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^)+(0.0937P)^2^+10.0687P] 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 12574 _refine_ls_number_parameters 787 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1376 _refine_ls_R_factor_gt 0.0755 _refine_ls_wR_factor_ref 0.2047 _refine_ls_wR_factor_gt 0.1814 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 Zn1 Zn 0.37968(4) 1.04109(6) 0.57298(3) 0.0267(2) Uani 1 1 d . . . Co1 Co 0.5000 1.0000 0.5000 0.0193(3) Uani 1 2 d S . . O1 O 0.3256(2) 0.9821(4) 0.4959(2) 0.0397(12) Uani 1 1 d . . . O2 O 0.3962(3) 0.9889(4) 0.4423(2) 0.0488(14) Uani 1 1 d . . . O3 O -0.0468(3) 0.5196(3) 0.1409(2) 0.0387(12) Uani 1 1 d . . . O4 O -0.0156(2) 0.5797(3) 0.0673(2) 0.0388(11) Uani 1 1 d . . . O5 O 0.3946(3) 1.1688(3) 0.5620(2) 0.0397(12) Uani 1 1 d . . . O6 O 0.4844(3) 1.1197(4) 0.5414(3) 0.0551(15) Uani 1 1 d . . . O7 O 0.3029(2) 1.0340(3) 0.6077(2) 0.0350(11) Uani 1 1 d . . . N1 N 0.2554(4) 0.9829(5) 0.6746(3) 0.059(2) Uani 1 1 d . . . C1 C 0.3431(3) 0.9604(5) 0.4506(3) 0.0330(15) Uani 1 1 d . . . C2 C 0.2923(4) 0.9022(5) 0.4008(3) 0.0357(17) Uani 1 1 d . . . C3 C 0.2314(4) 0.8726(6) 0.4059(3) 0.049(2) Uani 1 1 d . . . H3 H 0.2205 0.8901 0.4405 0.058 Uiso 1 1 calc R . . C4 C 0.1854(4) 0.8171(6) 0.3605(4) 0.051(2) Uani 1 1 d . . . H4 H 0.1444 0.7970 0.3658 0.062 Uiso 1 1 calc R . . C5 C 0.1971(4) 0.7909(6) 0.3091(3) 0.0407(18) Uani 1 1 d . . . C6 C 0.2571(4) 0.8266(7) 0.3017(4) 0.061(3) Uani 1 1 d . . . H6 H 0.2655 0.8135 0.2652 0.073 Uiso 1 1 calc R . . C7 C 0.3040(4) 0.8808(7) 0.3472(4) 0.057(2) Uani 1 1 d . . . H7 H 0.3442 0.9032 0.3414 0.068 Uiso 1 1 calc R . . C8 C 0.1483(4) 0.7312(5) 0.2619(3) 0.0375(17) Uani 1 1 d . . . C9 C 0.1054(5) 0.6730(6) 0.2785(3) 0.054(2) Uani 1 1 d . . . H9 H 0.1094 0.6708 0.3204 0.065 Uiso 1 1 calc R . . C10 C 0.0564(4) 0.6174(5) 0.2349(3) 0.045(2) Uani 1 1 d . . . H10 H 0.0287 0.5776 0.2478 0.053 Uiso 1 1 calc R . . C11 C 0.0488(3) 0.6210(5) 0.1724(3) 0.0344(16) Uani 1 1 d . . . C12 C 0.0919(4) 0.6782(7) 0.1550(4) 0.059(3) Uani 1 1 d . . . H12 H 0.0881 0.6801 0.1131 0.070 Uiso 1 1 calc R . . C13 C 0.1406(4) 0.7327(7) 0.1988(4) 0.059(3) Uani 1 1 d . . . H13 H 0.1690 0.7715 0.1859 0.070 Uiso 1 1 calc R . . C14 C -0.0058(4) 0.5673(5) 0.1250(3) 0.0352(17) Uani 1 1 d . . . C15 C 0.4439(4) 1.1813(5) 0.5441(3) 0.0366(17) Uani 1 1 d . . . C16 C 0.4603(4) 1.2761(5) 0.5304(4) 0.0406(18) Uani 1 1 d . . . C17 C 0.5106(5) 1.2915(6) 0.5061(5) 0.071(3) Uani 1 1 d . . . H17 H 0.5361 1.2432 0.4985 0.085 Uiso 1 1 calc R . . C18 C 0.5241(5) 1.3803(6) 0.4925(6) 0.073(3) Uani 1 1 d . . . H18 H 0.5566 1.3899 0.4730 0.088 Uiso 1 1 calc R . . C19 C 0.4918(4) 1.4534(5) 0.5066(4) 0.0430(19) Uani 1 1 d . . . C20 C 0.4430(5) 1.4350(6) 0.5320(5) 0.065(3) Uani 1 1 d . . . H20 H 0.4202 1.4834 0.5431 0.078 Uiso 1 1 calc R . . C21 C 0.4255(5) 1.3478(6) 0.5423(4) 0.060(3) Uani 1 1 d . . . H21 H 0.3894 1.3380 0.5575 0.072 Uiso 1 1 calc R . . C22 C 0.3083(4) 1.0024(5) 0.6590(3) 0.0390(16) Uani 1 1 d . . . H22 H 0.3538 0.9918 0.6885 0.059 Uiso 1 1 calc R . . C23 C 0.2668(7) 0.9428(8) 0.7368(5) 0.096(4) Uani 1 1 d . . . H23A H 0.2565 0.8787 0.7320 0.143 Uiso 1 1 calc R . . H23B H 0.2359 0.9718 0.7544 0.143 Uiso 1 1 calc R . . H23C H 0.3153 0.9516 0.7644 0.143 Uiso 1 1 calc R . . C24 C 0.1842(5) 0.9975(9) 0.6336(6) 0.085(3) Uani 1 1 d . . . H24A H 0.1622 1.0404 0.6524 0.128 Uiso 1 1 calc R . . H24B H 0.1587 0.9408 0.6264 0.128 Uiso 1 1 calc R . . H24C H 0.1835 1.0211 0.5940 0.128 Uiso 1 1 calc R . . Zn2 Zn 0.37687(4) 0.04167(5) 0.06695(3) 0.0256(2) Uani 1 1 d . . . Co2 Co 0.5000 0.0000 0.0000 0.0190(3) Uani 1 2 d S . . O8 O 0.4332(3) -0.0290(3) 0.1412(2) 0.0371(11) Uani 1 1 d . . . O9 O 0.5052(3) -0.0121(4) 0.0906(2) 0.0539(16) Uani 1 1 d . . . O10 O 0.8275(2) -0.4715(3) 0.4928(2) 0.0338(11) Uani 1 1 d . . . O11 O 0.9134(2) -0.4194(3) 0.4651(3) 0.0441(13) Uani 1 1 d . . . O12 O 0.4087(3) 0.1638(3) 0.0656(2) 0.0365(11) Uani 1 1 d . . . O13 O 0.4414(2) 0.1199(3) -0.01234(18) 0.0265(9) Uani 1 1 d . . . O14 O 0.2929(3) 0.0686(4) 0.0873(3) 0.0508(14) Uani 1 1 d . . . N2 N 0.2055(6) 0.0289(8) 0.1187(6) 0.104(4) Uani 1 1 d . . . C25 C 0.4910(4) -0.0437(5) 0.1351(3) 0.0326(16) Uani 1 1 d . . . C26 C 0.5450(4) -0.0984(5) 0.1830(3) 0.0321(16) Uani 1 1 d . . . C27 C 0.5350(3) -0.1269(5) 0.2373(3) 0.0337(16) Uani 1 1 d . . . H27 H 0.4937 -0.1111 0.2438 0.040 Uiso 1 1 calc R . . C28 C 0.5857(4) -0.1778(5) 0.2806(3) 0.0336(16) Uani 1 1 d . . . H28 H 0.5791 -0.1951 0.3174 0.040 Uiso 1 1 calc R . . C29 C 0.6460(3) -0.2045(5) 0.2723(3) 0.0284(15) Uani 1 1 d . . . C30 C 0.6557(4) -0.1769(5) 0.2180(3) 0.0382(17) Uani 1 1 d . . . H30 H 0.6963 -0.1948 0.2110 0.046 Uiso 1 1 calc R . . C31 C 0.6059(4) -0.1234(5) 0.1745(3) 0.0396(18) Uani 1 1 d . . . H31 H 0.6136 -0.1038 0.1387 0.048 Uiso 1 1 calc R . . C32 C 0.6998(4) -0.2616(5) 0.3201(3) 0.0314(15) Uani 1 1 d . . . C33 C 0.6784(4) -0.3285(5) 0.3515(3) 0.0378(17) Uani 1 1 d . . . H33 H 0.6302 -0.3384 0.3421 0.045 Uiso 1 1 calc R . . C34 C 0.7275(4) -0.3804(5) 0.3963(3) 0.0365(17) Uani 1 1 d . . . H34 H 0.7125 -0.4250 0.4176 0.044 Uiso 1 1 calc R . . C35 C 0.7987(3) -0.3674(4) 0.4102(3) 0.0285(14) Uani 1 1 d . . . C36 C 0.8202(4) -0.3051(5) 0.3770(3) 0.0357(16) Uani 1 1 d . . . H36 H 0.8682 -0.2989 0.3841 0.043 Uiso 1 1 calc R . . C37 C 0.7712(3) -0.2518(5) 0.3333(3) 0.0363(16) Uani 1 1 d . . . H37 H 0.7866 -0.2077 0.3119 0.044 Uiso 1 1 calc R . . C38 C 0.8516(4) -0.4241(4) 0.4596(3) 0.0296(15) Uani 1 1 d . . . C39 C 0.4344(3) 0.1781(4) 0.0234(3) 0.0276(14) Uani 1 1 d . . . C40 C 0.4560(4) 0.2727(5) 0.0170(3) 0.0351(16) Uani 1 1 d . . . C41 C 0.4739(5) 0.2987(5) -0.0322(4) 0.049(2) Uani 1 1 d . . . H41 H 0.4741 0.2555 -0.0620 0.059 Uiso 1 1 calc R . . C42 C 0.4915(5) 0.3866(6) -0.0389(4) 0.057(2) Uani 1 1 d . . . H42 H 0.5045 0.4024 -0.0727 0.068 Uiso 1 1 calc R . . C43 C 0.4905(4) 0.4519(5) 0.0038(4) 0.0422(18) Uani 1 1 d . . . C44 C 0.4735(8) 0.4257(6) 0.0530(5) 0.096(4) Uani 1 1 d . . . H44 H 0.4750 0.4684 0.0836 0.115 Uiso 1 1 calc R . . C45 C 0.4544(7) 0.3385(6) 0.0592(5) 0.087(4) Uani 1 1 d . . . H45 H 0.4401 0.3234 0.0924 0.104 Uiso 1 1 calc R . . C46 C 0.2575(7) 0.0153(9) 0.0981(6) 0.100(4) Uani 1 1 d . . . H46 H 0.2666 -0.0452 0.0914 0.150 Uiso 1 1 calc R . . C47 C 0.1871(9) 0.1225(13) 0.1250(10) 0.172(8) Uani 1 1 d . . . H47A H 0.2196 0.1469 0.1640 0.258 Uiso 1 1 calc R . . H47B H 0.1396 0.1251 0.1247 0.258 Uiso 1 1 calc R . . H47C H 0.1897 0.1576 0.0903 0.258 Uiso 1 1 calc R . . C48 C 0.1648(8) -0.0429(11) 0.1308(7) 0.133(6) Uani 1 1 d . . . H48A H 0.1843 -0.1006 0.1255 0.200 Uiso 1 1 calc R . . H48B H 0.1164 -0.0386 0.1017 0.200 Uiso 1 1 calc R . . H48C H 0.1663 -0.0378 0.1733 0.200 Uiso 1 1 calc R . . O15 O 0.2287(14) 0.2891(13) 0.3653(16) 0.342(17) Uani 1 1 d . . . C49 C 0.2422(10) 0.231(2) 0.4205(13) 0.233(16) Uani 1 1 d . . . H49 H 0.2866 0.2055 0.4425 0.349 Uiso 1 1 calc R . . N3 N 0.1890(7) 0.2179(8) 0.4364(6) 0.124(5) Uani 1 1 d . . . C50 C 0.1261(9) 0.2635(13) 0.4133(8) 0.167(8) Uani 1 1 d . . . H50A H 0.1224 0.2946 0.3751 0.251 Uiso 1 1 calc R . . H50B H 0.1240 0.3070 0.4440 0.251 Uiso 1 1 calc R . . H50C H 0.0876 0.2209 0.4044 0.251 Uiso 1 1 calc R . . C51 C 0.1960(10) 0.1529(13) 0.4853(8) 0.178(9) Uani 1 1 d . . . H51A H 0.2318 0.1089 0.4870 0.267 Uiso 1 1 calc R . . H51B H 0.1514 0.1223 0.4764 0.267 Uiso 1 1 calc R . . H51C H 0.2095 0.1837 0.5252 0.267 Uiso 1 1 calc R . . O16 O 0.1758(8) 0.1183(13) 0.7663(8) 0.224(8) Uani 1 1 d . . . C52 C 0.1225(11) 0.0975(18) 0.7769(10) 0.178(9) Uani 1 1 d . . . H52 H 0.1224 0.0399 0.7940 0.266 Uiso 1 1 calc R . . N4 N 0.0712(6) 0.1425(12) 0.7677(6) 0.134(5) Uani 1 1 d . . . C53 C 0.0756(15) 0.234(2) 0.7383(14) 0.30(2) Uani 1 1 d . . . H53A H 0.1223 0.2594 0.7588 0.450 Uiso 1 1 calc R . . H53B H 0.0410 0.2751 0.7434 0.450 Uiso 1 1 calc R . . H53C H 0.0662 0.2264 0.6941 0.450 Uiso 1 1 calc R . . C54 C 0.0138(9) 0.1254(15) 0.7860(10) 0.183(9) Uani 1 1 d . . . H54A H 0.0240 0.0730 0.8131 0.275 Uiso 1 1 calc R . . H54B H -0.0280 0.1141 0.7492 0.275 Uiso 1 1 calc R . . H54C H 0.0060 0.1773 0.8082 0.275 Uiso 1 1 calc R . . O17 O 0.3454(5) 0.5858(6) 0.5652(5) 0.123(3) Uani 1 1 d . . . C55 C 0.2949(7) 0.6314(9) 0.5685(6) 0.092(4) Uani 1 1 d . . . H55 H 0.2539 0.5995 0.5653 0.138 Uiso 1 1 calc R . . N5 N 0.2941(4) 0.7177(6) 0.5760(4) 0.064(2) Uani 1 1 d . . . C56 C 0.2325(7) 0.7607(11) 0.5800(7) 0.120(5) Uani 1 1 d . . . H56A H 0.1959 0.7160 0.5737 0.181 Uiso 1 1 calc R . . H56B H 0.2158 0.8070 0.5481 0.181 Uiso 1 1 calc R . . H56C H 0.2445 0.7880 0.6210 0.181 Uiso 1 1 calc R . . C57 C 0.3527(8) 0.7712(9) 0.5763(8) 0.137(6) Uani 1 1 d . . . H57A H 0.3947 0.7529 0.6111 0.206 Uiso 1 1 calc R . . H57B H 0.3432 0.8344 0.5808 0.206 Uiso 1 1 calc R . . H57C H 0.3599 0.7623 0.5374 0.206 Uiso 1 1 calc R . . O18 O 0.4638(14) 0.5580(9) 0.1701(7) 0.262(11) Uani 1 1 d . . . C58 C 0.466(2) 0.6087(14) 0.2131(11) 0.242(18) Uani 1 1 d . . . H58 H 0.5047 0.6448 0.2354 0.363 Uiso 1 1 calc R . . N6 N 0.401(2) 0.607(2) 0.2260(15) 0.27(2) Uani 1 1 d . . . C59 C 0.328(3) 0.597(4) 0.198(2) 0.59(7) Uani 1 1 d . . . H59A H 0.3087 0.6479 0.1709 0.878 Uiso 1 1 calc R . . H59B H 0.3082 0.5927 0.2296 0.878 Uiso 1 1 calc R . . H59C H 0.3180 0.5417 0.1729 0.878 Uiso 1 1 calc R . . C60 C 0.4287(12) 0.6686(18) 0.2786(11) 0.199(11) Uani 1 1 d . . . H60A H 0.4633 0.6376 0.3136 0.298 Uiso 1 1 calc R . . H60B H 0.3907 0.6899 0.2905 0.298 Uiso 1 1 calc R . . H60C H 0.4507 0.7196 0.2666 0.298 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0275(4) 0.0262(5) 0.0227(4) -0.0001(3) 0.0050(3) 0.0009(3) Co1 0.0198(6) 0.0172(7) 0.0179(5) -0.0004(4) 0.0034(4) -0.0013(5) O1 0.027(2) 0.051(4) 0.037(3) -0.010(2) 0.007(2) -0.003(2) O2 0.033(3) 0.063(4) 0.042(3) 0.000(3) 0.003(2) -0.011(3) O3 0.041(3) 0.042(3) 0.028(2) -0.012(2) 0.007(2) -0.013(2) O4 0.042(3) 0.032(3) 0.042(3) -0.008(2) 0.015(2) -0.003(2) O5 0.054(3) 0.028(3) 0.042(3) 0.007(2) 0.024(2) 0.006(2) O6 0.074(4) 0.030(3) 0.068(4) -0.007(3) 0.034(3) -0.004(3) O7 0.033(2) 0.035(3) 0.041(3) 0.007(2) 0.017(2) 0.000(2) N1 0.079(5) 0.052(5) 0.066(4) -0.006(4) 0.049(4) -0.018(4) C1 0.024(3) 0.036(4) 0.037(3) -0.009(3) 0.009(3) -0.007(3) C2 0.031(3) 0.036(5) 0.037(4) -0.015(3) 0.009(3) -0.007(3) C3 0.038(4) 0.074(6) 0.036(4) -0.028(4) 0.016(3) -0.024(4) C4 0.031(4) 0.074(7) 0.050(4) -0.028(4) 0.017(3) -0.021(4) C5 0.035(4) 0.047(5) 0.038(4) -0.010(3) 0.011(3) -0.014(3) C6 0.046(5) 0.083(7) 0.060(5) -0.037(5) 0.026(4) -0.017(5) C7 0.039(4) 0.079(7) 0.057(5) -0.025(5) 0.024(4) -0.022(4) C8 0.033(4) 0.036(5) 0.042(4) -0.010(3) 0.013(3) -0.012(3) C9 0.077(6) 0.050(6) 0.019(3) -0.004(3) 0.000(3) -0.035(5) C10 0.055(5) 0.040(5) 0.028(3) 0.002(3) 0.003(3) -0.024(4) C11 0.029(3) 0.037(4) 0.035(3) -0.013(3) 0.008(3) -0.007(3) C12 0.059(5) 0.085(7) 0.040(4) -0.024(4) 0.026(4) -0.035(5) C13 0.055(5) 0.076(7) 0.051(5) -0.028(4) 0.027(4) -0.040(5) C14 0.031(4) 0.039(5) 0.031(3) -0.012(3) 0.007(3) -0.010(3) C15 0.051(5) 0.019(4) 0.042(4) -0.008(3) 0.020(3) 0.002(3) C16 0.052(5) 0.028(4) 0.054(4) 0.009(3) 0.032(4) 0.005(3) C17 0.079(7) 0.020(5) 0.149(10) -0.018(5) 0.084(7) -0.004(4) C18 0.092(7) 0.018(4) 0.155(10) -0.006(5) 0.099(8) -0.005(4) C19 0.060(5) 0.012(4) 0.062(5) 0.000(4) 0.029(4) -0.001(4) C20 0.102(8) 0.025(5) 0.102(7) 0.013(4) 0.076(6) 0.018(5) C21 0.084(6) 0.031(5) 0.093(7) 0.019(4) 0.066(6) 0.023(4) C22 0.048(4) 0.032(4) 0.046(4) -0.003(3) 0.027(3) -0.007(3) C23 0.144(11) 0.094(10) 0.085(7) 0.020(6) 0.086(8) -0.015(8) C24 0.060(7) 0.102(10) 0.111(9) -0.002(7) 0.051(6) -0.018(6) Zn2 0.0277(4) 0.0202(4) 0.0252(4) 0.0001(3) 0.0055(3) -0.0007(3) Co2 0.0203(6) 0.0144(6) 0.0200(5) 0.0012(4) 0.0047(4) -0.0003(5) O8 0.039(3) 0.028(3) 0.034(2) 0.006(2) 0.002(2) 0.001(2) O9 0.097(4) 0.042(3) 0.025(2) 0.014(2) 0.025(3) 0.031(3) O10 0.033(3) 0.028(3) 0.034(2) 0.015(2) 0.006(2) 0.009(2) O11 0.024(2) 0.023(3) 0.077(3) 0.019(3) 0.008(2) 0.007(2) O12 0.050(3) 0.020(3) 0.045(3) -0.003(2) 0.024(2) -0.005(2) O13 0.036(2) 0.011(2) 0.029(2) 0.0020(17) 0.0082(18) 0.0039(18) O14 0.044(3) 0.052(4) 0.070(4) -0.013(3) 0.037(3) -0.005(3) N2 0.108(8) 0.089(8) 0.156(10) -0.019(7) 0.097(8) -0.018(6) C25 0.047(4) 0.022(4) 0.021(3) -0.001(3) 0.004(3) 0.000(3) C26 0.052(4) 0.024(4) 0.017(3) 0.002(2) 0.010(3) 0.006(3) C27 0.030(3) 0.035(4) 0.031(3) 0.000(3) 0.005(3) 0.004(3) C28 0.045(4) 0.029(4) 0.027(3) 0.004(3) 0.012(3) 0.004(3) C29 0.038(4) 0.023(4) 0.024(3) 0.003(3) 0.012(3) 0.012(3) C30 0.045(4) 0.040(5) 0.032(3) 0.008(3) 0.016(3) 0.016(3) C31 0.055(5) 0.040(5) 0.023(3) 0.004(3) 0.014(3) 0.001(4) C32 0.040(4) 0.027(4) 0.027(3) -0.001(3) 0.013(3) 0.005(3) C33 0.027(4) 0.036(5) 0.048(4) 0.015(3) 0.012(3) 0.006(3) C34 0.031(4) 0.035(4) 0.043(4) 0.014(3) 0.013(3) 0.003(3) C35 0.030(3) 0.022(4) 0.031(3) -0.002(3) 0.009(3) 0.007(3) C36 0.029(3) 0.035(4) 0.043(4) 0.012(3) 0.014(3) 0.006(3) C37 0.032(4) 0.037(4) 0.042(4) 0.012(3) 0.015(3) 0.007(3) C38 0.039(4) 0.010(3) 0.035(3) -0.001(3) 0.007(3) 0.006(3) C39 0.030(3) 0.017(4) 0.033(3) 0.004(3) 0.008(3) 0.006(3) C40 0.042(4) 0.020(4) 0.044(4) -0.008(3) 0.017(3) -0.003(3) C41 0.079(6) 0.016(4) 0.068(5) -0.005(4) 0.046(5) -0.005(4) C42 0.092(7) 0.030(5) 0.067(5) -0.003(4) 0.051(5) -0.016(4) C43 0.042(4) 0.037(5) 0.058(4) -0.003(4) 0.030(4) -0.001(4) C44 0.210(14) 0.022(5) 0.108(8) -0.025(5) 0.120(9) -0.034(7) C45 0.186(12) 0.018(5) 0.116(8) -0.022(5) 0.125(9) -0.036(6) C46 0.118(10) 0.077(9) 0.146(12) 0.032(8) 0.096(10) 0.038(8) C47 0.152(15) 0.151(18) 0.25(2) -0.067(16) 0.122(16) 0.018(13) C48 0.109(11) 0.155(16) 0.152(13) 0.031(11) 0.068(10) -0.031(11) O15 0.41(3) 0.162(17) 0.66(5) -0.07(2) 0.44(4) -0.068(18) C49 0.071(12) 0.36(5) 0.27(3) 0.03(3) 0.061(15) -0.041(18) N3 0.106(9) 0.069(8) 0.148(11) 0.007(7) -0.011(8) 0.014(7) C50 0.152(16) 0.138(17) 0.167(16) -0.011(13) 0.006(13) 0.061(14) C51 0.173(18) 0.144(18) 0.161(16) 0.043(14) -0.004(13) 0.064(14) O16 0.171(13) 0.33(2) 0.245(16) 0.074(15) 0.157(13) 0.035(13) C52 0.134(16) 0.25(3) 0.188(19) -0.011(18) 0.110(16) -0.003(18) N4 0.074(8) 0.206(17) 0.130(10) -0.001(10) 0.048(7) 0.044(9) C53 0.30(4) 0.32(4) 0.38(4) 0.21(4) 0.25(3) 0.15(3) C54 0.104(13) 0.19(2) 0.26(2) -0.086(18) 0.078(15) -0.022(13) O17 0.118(7) 0.082(7) 0.201(10) -0.025(7) 0.095(7) 0.008(6) C55 0.087(8) 0.070(9) 0.134(11) -0.038(7) 0.059(8) -0.010(7) N5 0.065(5) 0.049(5) 0.082(5) 0.007(4) 0.030(4) 0.005(4) C56 0.084(9) 0.140(14) 0.138(12) -0.033(10) 0.042(8) 0.024(9) C57 0.130(12) 0.072(10) 0.234(19) 0.040(11) 0.095(13) -0.024(9) O18 0.58(4) 0.094(10) 0.140(11) -0.021(8) 0.164(17) -0.001(15) C58 0.40(5) 0.076(14) 0.134(19) -0.039(13) -0.04(2) -0.01(2) N6 0.45(5) 0.25(3) 0.20(3) 0.09(2) 0.22(3) 0.15(3) C59 0.67(11) 0.62(10) 0.33(6) -0.10(6) 0.02(6) -0.52(10) C60 0.20(2) 0.24(3) 0.20(2) -0.06(2) 0.13(2) -0.07(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 Zn1 O1 1.919(5) . ? Zn1 O3 1.942(4) 4_676 ? Zn1 O5 1.948(5) . ? Zn1 O7 2.012(5) . ? Co1 O2 2.052(5) 3_676 ? Co1 O2 2.052(5) . ? Co1 O4 2.066(5) 2 ? Co1 O4 2.066(5) 4_676 ? Co1 O6 2.094(5) . ? Co1 O6 2.094(5) 3_676 ? O1 C1 1.263(8) . ? O2 C1 1.245(8) . ? O3 C14 1.252(8) . ? O3 Zn1 1.942(4) 4_575 ? O4 C14 1.280(8) . ? O4 Co1 2.066(5) 2_545 ? O5 C15 1.237(9) . ? O6 C15 1.250(9) . ? O7 C22 1.236(8) . ? N1 C22 1.293(10) . ? N1 C24 1.429(13) . ? N1 C23 1.486(11) . ? C1 C2 1.502(9) . ? C2 C3 1.367(10) . ? C2 C7 1.378(10) . ? C3 C4 1.387(10) . ? C4 C5 1.350(10) . ? C5 C6 1.403(11) . ? C5 C8 1.468(9) . ? C6 C7 1.385(11) . ? C8 C9 1.381(10) . ? C8 C13 1.403(10) . ? C9 C10 1.394(9) . ? C10 C11 1.391(10) . ? C11 C12 1.386(11) . ? C11 C14 1.472(9) . ? C12 C13 1.384(10) . ? C15 C16 1.504(10) . ? C16 C21 1.362(11) . ? C16 C17 1.362(11) . ? C17 C18 1.403(11) . ? C18 C19 1.369(11) . ? C19 C20 1.361(11) . ? C19 C19 1.478(14) 3_686 ? C20 C21 1.384(12) . ? Zn2 O12 1.927(5) . ? Zn2 O10 1.933(4) 4 ? Zn2 O8 1.972(4) . ? Zn2 O14 1.981(5) . ? Co2 O11 2.039(4) 4 ? Co2 O11 2.039(4) 2_655 ? Co2 O9 2.057(4) 3_655 ? Co2 O9 2.057(4) . ? Co2 O13 2.103(4) 3_655 ? Co2 O13 2.103(4) . ? O8 C25 1.260(8) . ? O9 C25 1.255(8) . ? O10 C38 1.265(8) . ? O10 Zn2 1.933(4) 4_656 ? O11 C38 1.225(8) . ? O11 Co2 2.039(4) 2_645 ? O12 C39 1.281(8) . ? O13 C39 1.237(7) . ? O14 C46 1.160(13) . ? N2 C46 1.330(14) . ? N2 C48 1.441(15) . ? N2 C47 1.458(18) . ? C25 C26 1.480(9) . ? C26 C31 1.383(10) . ? C26 C27 1.403(9) . ? C27 C28 1.370(9) . ? C28 C29 1.376(9) . ? C29 C30 1.397(9) . ? C29 C32 1.496(9) . ? C30 C31 1.383(9) . ? C32 C37 1.386(9) . ? C32 C33 1.390(10) . ? C33 C34 1.377(9) . ? C34 C35 1.385(9) . ? C35 C36 1.369(9) . ? C35 C38 1.504(9) . ? C36 C37 1.375(9) . ? C39 C40 1.494(10) . ? C40 C41 1.369(10) . ? C40 C45 1.386(10) . ? C41 C42 1.376(11) . ? C42 C43 1.385(11) . ? C43 C44 1.359(11) . ? C43 C43 1.506(15) 3_665 ? C44 C45 1.372(12) . ? O15 C49 1.47(3) . ? C49 N3 1.28(2) . ? N3 C50 1.374(17) . ? N3 C51 1.45(2) . ? O16 C52 1.24(2) . ? C52 N4 1.19(2) . ? N4 C54 1.41(2) . ? N4 C53 1.54(3) . ? O17 C55 1.260(13) . ? C55 N5 1.292(13) . ? N5 C57 1.436(14) . ? N5 C56 1.445(14) . ? O18 C58 1.23(3) . ? C58 N6 1.46(5) . ? N6 C59 1.39(6) . ? N6 C60 1.45(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O3 122.9(2) . 4_676 ? O1 Zn1 O5 112.8(2) . . ? O3 Zn1 O5 116.2(2) 4_676 . ? O1 Zn1 O7 94.4(2) . . ? O3 Zn1 O7 98.1(2) 4_676 . ? O5 Zn1 O7 106.6(2) . . ? O2 Co1 O2 180.000(1) 3_676 . ? O2 Co1 O4 91.7(2) 3_676 2 ? O2 Co1 O4 88.3(2) . 2 ? O2 Co1 O4 88.3(2) 3_676 4_676 ? O2 Co1 O4 91.7(2) . 4_676 ? O4 Co1 O4 180.000(1) 2 4_676 ? O2 Co1 O6 86.2(2) 3_676 . ? O2 Co1 O6 93.8(2) . . ? O4 Co1 O6 87.1(2) 2 . ? O4 Co1 O6 92.9(2) 4_676 . ? O2 Co1 O6 93.8(2) 3_676 3_676 ? O2 Co1 O6 86.2(2) . 3_676 ? O4 Co1 O6 92.9(2) 2 3_676 ? O4 Co1 O6 87.1(2) 4_676 3_676 ? O6 Co1 O6 180.000(1) . 3_676 ? C1 O1 Zn1 129.6(4) . . ? C1 O2 Co1 132.9(5) . . ? C14 O3 Zn1 115.4(4) . 4_575 ? C14 O4 Co1 133.5(5) . 2_545 ? C15 O5 Zn1 112.1(5) . . ? C15 O6 Co1 149.0(5) . . ? C22 O7 Zn1 126.3(5) . . ? C22 N1 C24 122.4(8) . . ? C22 N1 C23 120.6(9) . . ? C24 N1 C23 117.0(8) . . ? O2 C1 O1 124.8(6) . . ? O2 C1 C2 118.3(6) . . ? O1 C1 C2 116.7(6) . . ? C3 C2 C7 118.0(6) . . ? C3 C2 C1 120.9(6) . . ? C7 C2 C1 121.0(7) . . ? C2 C3 C4 120.8(7) . . ? C5 C4 C3 122.6(7) . . ? C4 C5 C6 116.5(7) . . ? C4 C5 C8 121.9(7) . . ? C6 C5 C8 121.5(7) . . ? C7 C6 C5 121.3(7) . . ? C2 C7 C6 120.6(7) . . ? C9 C8 C13 117.1(6) . . ? C9 C8 C5 120.0(6) . . ? C13 C8 C5 122.8(7) . . ? C8 C9 C10 122.2(7) . . ? C11 C10 C9 119.8(7) . . ? C12 C11 C10 118.9(6) . . ? C12 C11 C14 120.4(6) . . ? C10 C11 C14 120.7(7) . . ? C13 C12 C11 120.7(7) . . ? C12 C13 C8 121.3(8) . . ? O3 C14 O4 121.3(6) . . ? O3 C14 C11 119.7(6) . . ? O4 C14 C11 118.4(7) . . ? O5 C15 O6 122.9(7) . . ? O5 C15 C16 118.9(6) . . ? O6 C15 C16 117.9(7) . . ? C21 C16 C17 118.9(8) . . ? C21 C16 C15 120.8(7) . . ? C17 C16 C15 120.3(7) . . ? C16 C17 C18 119.4(8) . . ? C19 C18 C17 122.5(8) . . ? C20 C19 C18 116.1(7) . . ? C20 C19 C19 122.2(9) . 3_686 ? C18 C19 C19 121.7(9) . 3_686 ? C19 C20 C21 122.5(8) . . ? C16 C21 C20 120.5(8) . . ? O7 C22 N1 124.2(8) . . ? O12 Zn2 O10 124.0(2) . 4 ? O12 Zn2 O8 114.8(2) . . ? O10 Zn2 O8 115.2(2) 4 . ? O12 Zn2 O14 98.2(2) . . ? O10 Zn2 O14 95.9(2) 4 . ? O8 Zn2 O14 100.5(2) . . ? O11 Co2 O11 180.0(4) 4 2_655 ? O11 Co2 O9 86.6(2) 4 3_655 ? O11 Co2 O9 93.4(2) 2_655 3_655 ? O11 Co2 O9 93.4(2) 4 . ? O11 Co2 O9 86.6(2) 2_655 . ? O9 Co2 O9 180.0(5) 3_655 . ? O11 Co2 O13 85.84(18) 4 3_655 ? O11 Co2 O13 94.16(18) 2_655 3_655 ? O9 Co2 O13 91.34(18) 3_655 3_655 ? O9 Co2 O13 88.66(18) . 3_655 ? O11 Co2 O13 94.16(18) 4 . ? O11 Co2 O13 85.84(18) 2_655 . ? O9 Co2 O13 88.66(18) 3_655 . ? O9 Co2 O13 91.34(18) . . ? O13 Co2 O13 180.0(3) 3_655 . ? C25 O8 Zn2 105.5(4) . . ? C25 O9 Co2 156.9(5) . . ? C38 O10 Zn2 129.8(4) . 4_656 ? C38 O11 Co2 136.1(5) . 2_645 ? C39 O12 Zn2 113.8(4) . . ? C39 O13 Co2 134.5(4) . . ? C46 O14 Zn2 125.4(7) . . ? C46 N2 C48 123.5(13) . . ? C46 N2 C47 116.8(12) . . ? C48 N2 C47 119.6(12) . . ? O9 C25 O8 122.4(6) . . ? O9 C25 C26 118.6(7) . . ? O8 C25 C26 119.0(6) . . ? C31 C26 C27 118.9(6) . . ? C31 C26 C25 120.2(6) . . ? C27 C26 C25 120.9(7) . . ? C28 C27 C26 119.5(7) . . ? C27 C28 C29 122.2(6) . . ? C28 C29 C30 118.3(6) . . ? C28 C29 C32 120.8(6) . . ? C30 C29 C32 120.9(6) . . ? C31 C30 C29 120.3(7) . . ? C30 C31 C26 120.7(6) . . ? C37 C32 C33 118.0(6) . . ? C37 C32 C29 122.1(6) . . ? C33 C32 C29 119.9(6) . . ? C34 C33 C32 120.4(7) . . ? C33 C34 C35 120.5(7) . . ? C36 C35 C34 119.6(6) . . ? C36 C35 C38 120.5(6) . . ? C34 C35 C38 119.9(6) . . ? C35 C36 C37 119.8(6) . . ? C36 C37 C32 121.6(7) . . ? O11 C38 O10 125.9(6) . . ? O11 C38 C35 118.3(6) . . ? O10 C38 C35 115.8(6) . . ? O13 C39 O12 124.7(6) . . ? O13 C39 C40 118.5(6) . . ? O12 C39 C40 116.7(6) . . ? C41 C40 C45 117.8(7) . . ? C41 C40 C39 121.7(6) . . ? C45 C40 C39 120.4(7) . . ? C40 C41 C42 121.4(7) . . ? C41 C42 C43 120.5(8) . . ? C44 C43 C42 117.9(8) . . ? C44 C43 C43 121.6(9) . 3_665 ? C42 C43 C43 120.5(8) . 3_665 ? C43 C44 C45 121.8(8) . . ? C44 C45 C40 120.4(8) . . ? O14 C46 N2 128.2(12) . . ? N3 C49 O15 115(2) . . ? C49 N3 C50 126(2) . . ? C49 N3 C51 118.2(19) . . ? C50 N3 C51 115.9(17) . . ? N4 C52 O16 127(3) . . ? C52 N4 C54 128(2) . . ? C52 N4 C53 112.4(19) . . ? C54 N4 C53 118.8(16) . . ? O17 C55 N5 126.2(12) . . ? C55 N5 C57 119.7(11) . . ? C55 N5 C56 120.0(11) . . ? C57 N5 C56 120.2(11) . . ? O18 C58 N6 113(3) . . ? C59 N6 C60 119(3) . . ? C59 N6 C58 143(4) . . ? C60 N6 C58 93(3) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.098 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.100 _exptl_crystal_recrystallization_method solvothermal # Attachment 'compound_3.cif' data_wan581 _database_code_depnum_ccdc_archive 'CCDC 613448' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H38 Cd N2 O14 Zn2, 4(C3 H7 N O)' _chemical_formula_sum 'C60 H66 Cd N6 O18 Zn2' _chemical_formula_weight 1402.33 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' Cd Cd -0.8075 1.2024 '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 'P 21/n' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.491(2) _cell_length_b 14.837(3) _cell_length_c 19.386(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.53(3) _cell_angle_gamma 90.00 _cell_volume 3238.3(11) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 1532 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 25.9 _exptl_crystal_description 'block shaped' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 1.132 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25084 _diffrn_reflns_av_R_equivalents 0.0713 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.93 _reflns_number_total 6015 _reflns_number_gt 4445 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE EXPOSE' _computing_cell_refinement 'STOE CELL' _computing_data_reduction 'STOE INTEGRATE' _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^)+(0.1034P)^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 6015 _refine_ls_number_parameters 394 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1537 _refine_ls_wR_factor_gt 0.1442 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.0000 0.0000 0.0000 0.02776(16) Uani 1 2 d S . . Zn1 Zn 0.26799(5) 0.04379(3) 0.12524(2) 0.02061(16) Uani 1 1 d . . . O1 O 0.1676(3) -0.0171(2) 0.17963(17) 0.0320(8) Uani 1 1 d . . . O2 O 0.0582(3) -0.0902(2) 0.08836(16) 0.0336(8) Uani 1 1 d . . . O3 O -0.1674(3) -0.4725(2) 0.55708(17) 0.0311(7) Uani 1 1 d . . . O4 O -0.3238(3) -0.5063(2) 0.47489(18) 0.0353(8) Uani 1 1 d . . . O5 O 0.2251(3) 0.1673(2) 0.10003(18) 0.0328(8) Uani 1 1 d . . . O6 O 0.0380(3) 0.1218(2) 0.06585(17) 0.0305(7) Uani 1 1 d . . . C1 C 0.0889(4) -0.0741(3) 0.1522(2) 0.0272(10) Uani 1 1 d . . . C2 C 0.0362(4) -0.1293(3) 0.2032(2) 0.0276(10) Uani 1 1 d . . . C3 C 0.0701(5) -0.1155(3) 0.2750(3) 0.0379(12) Uani 1 1 d . . . H3 H 0.1248 -0.0687 0.2922 0.045 Uiso 1 1 calc R . . C4 C 0.0259(5) -0.1683(4) 0.3212(3) 0.0405(13) Uani 1 1 d . . . H4 H 0.0512 -0.1581 0.3703 0.049 Uiso 1 1 calc R . . C5 C -0.0546(4) -0.2363(3) 0.2986(2) 0.0295(10) Uani 1 1 d . . . C6 C -0.0910(5) -0.2487(4) 0.2267(3) 0.0418(13) Uani 1 1 d . . . H6 H -0.1471 -0.2946 0.2096 0.050 Uiso 1 1 calc R . . C7 C -0.0467(5) -0.1950(4) 0.1793(3) 0.0382(12) Uani 1 1 d . . . H7 H -0.0736 -0.2036 0.1302 0.046 Uiso 1 1 calc R . . C8 C -0.1000(5) -0.2951(3) 0.3494(2) 0.0307(11) Uani 1 1 d . . . C9 C -0.0242(4) -0.3230(3) 0.4110(2) 0.0298(10) Uani 1 1 d . . . H9 H 0.0564 -0.3042 0.4203 0.036 Uiso 1 1 calc R . . C10 C -0.0650(4) -0.3780(3) 0.4590(2) 0.0280(10) Uani 1 1 d . . . H10 H -0.0127 -0.3962 0.5011 0.034 Uiso 1 1 calc R . . C11 C -0.1828(4) -0.4064(3) 0.4453(2) 0.0273(10) Uani 1 1 d . . . C12 C -0.2576(5) -0.3791(4) 0.3839(3) 0.0364(12) Uani 1 1 d . . . H12 H -0.3380 -0.3985 0.3742 0.044 Uiso 1 1 calc R . . C13 C -0.2165(5) -0.3238(4) 0.3362(3) 0.0392(12) Uani 1 1 d . . . H13 H -0.2690 -0.3056 0.2943 0.047 Uiso 1 1 calc R . . C14 C -0.2297(4) -0.4658(3) 0.4959(2) 0.0272(10) Uani 1 1 d . . . C15 C 0.1162(5) 0.1808(3) 0.0735(2) 0.0291(10) Uani 1 1 d . . . C16 C 0.0818(5) 0.2755(3) 0.0531(3) 0.0321(11) Uani 1 1 d . . . C17 C -0.0316(6) 0.2957(3) 0.0193(4) 0.062(2) Uani 1 1 d . . . H17 H -0.0894 0.2491 0.0100 0.074 Uiso 1 1 calc R . . C18 C -0.0636(6) 0.3838(4) -0.0016(4) 0.067(2) Uani 1 1 d . . . H18 H -0.1427 0.3963 -0.0251 0.081 Uiso 1 1 calc R . . C19 C 0.0171(5) 0.4522(3) 0.0111(3) 0.0402(13) Uani 1 1 d . . . C20 C 0.1285(6) 0.4327(4) 0.0463(5) 0.081(3) Uani 1 1 d . . . H20 H 0.1854 0.4797 0.0570 0.097 Uiso 1 1 calc R . . C21 C 0.1610(6) 0.3446(4) 0.0671(5) 0.071(2) Uani 1 1 d . . . H21 H 0.2398 0.3326 0.0914 0.085 Uiso 1 1 calc R . . O7 O 0.4136(3) 0.0397(2) 0.20213(17) 0.0362(8) Uani 1 1 d . . . C22 C 0.5084(5) 0.0040(4) 0.1968(3) 0.0428(13) Uani 1 1 d . . . H22 H 0.5244 -0.0018 0.1508 0.051 Uiso 1 1 calc R . . N1 N 0.5862(6) -0.0255(5) 0.2477(4) 0.0758(19) Uani 1 1 d . . . C23 C 0.6957(8) -0.0696(8) 0.2366(7) 0.127(5) Uani 1 1 d . . . H23A H 0.6890 -0.1349 0.2423 0.191 Uiso 1 1 calc R . . H23B H 0.7636 -0.0468 0.2711 0.191 Uiso 1 1 calc R . . H23C H 0.7076 -0.0564 0.1889 0.191 Uiso 1 1 calc R . . C24 C 0.5648(11) -0.0216(12) 0.3202(5) 0.172(7) Uani 1 1 d . . . H24A H 0.5098 0.0278 0.3240 0.258 Uiso 1 1 calc R . . H24B H 0.6401 -0.0113 0.3531 0.258 Uiso 1 1 calc R . . H24C H 0.5302 -0.0787 0.3316 0.258 Uiso 1 1 calc R . . O8 O 0.3739(13) -0.4465(14) 0.0574(13) 0.316(11) Uani 1 1 d . . . C25 C 0.4490(18) -0.3833(18) 0.0424(12) 0.214(12) Uani 1 1 d . . . H25 H 0.4195 -0.3386 0.0082 0.257 Uiso 1 1 calc R . . N2 N 0.5526(19) -0.3814(11) 0.0708(8) 0.175(5) Uani 1 1 d . . . C26 C 0.6349(15) -0.3142(16) 0.0678(9) 0.215(11) Uani 1 1 d . . . H26A H 0.6122 -0.2811 0.0234 0.322 Uiso 1 1 calc R . . H26B H 0.7135 -0.3413 0.0705 0.322 Uiso 1 1 calc R . . H26C H 0.6374 -0.2727 0.1074 0.322 Uiso 1 1 calc R . . C27 C 0.580(4) -0.4580(18) 0.1146(17) 0.44(3) Uani 1 1 d . . . H27A H 0.6283 -0.5000 0.0930 0.666 Uiso 1 1 calc R . . H27B H 0.5065 -0.4878 0.1201 0.666 Uiso 1 1 calc R . . H27C H 0.6248 -0.4393 0.1608 0.666 Uiso 1 1 calc R . . O9 O 0.5460(10) -0.2856(11) 0.2208(7) 0.228(7) Uani 1 1 d . . . C28 C 0.4493(11) -0.3228(11) 0.2306(8) 0.147(6) Uani 1 1 d . . . H28 H 0.4510 -0.3736 0.2606 0.177 Uiso 1 1 calc R . . N3 N 0.3506(6) -0.2887(4) 0.1985(4) 0.0779(19) Uani 1 1 d . . . C29 C 0.2417(10) -0.3341(8) 0.2046(6) 0.112(4) Uani 1 1 d . . . H29A H 0.2213 -0.3191 0.2500 0.168 Uiso 1 1 calc R . . H29B H 0.2525 -0.3994 0.2016 0.168 Uiso 1 1 calc R . . H29C H 0.1774 -0.3145 0.1663 0.168 Uiso 1 1 calc R . . C30 C 0.3441(17) -0.2120(9) 0.1574(12) 0.240(11) Uani 1 1 d . . . H30A H 0.3047 -0.1639 0.1786 0.360 Uiso 1 1 calc R . . H30B H 0.2987 -0.2252 0.1101 0.360 Uiso 1 1 calc R . . H30C H 0.4245 -0.1927 0.1543 0.360 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0330(3) 0.0229(3) 0.0287(3) 0.00145(18) 0.0095(2) 0.00303(19) Zn1 0.0272(3) 0.0135(2) 0.0240(3) 0.00266(18) 0.0119(2) 0.00342(19) O1 0.040(2) 0.0291(17) 0.0300(16) 0.0065(13) 0.0155(15) -0.0084(15) O2 0.052(2) 0.0270(17) 0.0248(16) 0.0070(13) 0.0143(15) -0.0022(16) O3 0.036(2) 0.0294(17) 0.0310(17) 0.0063(13) 0.0135(15) -0.0049(14) O4 0.037(2) 0.0335(18) 0.0412(19) -0.0008(15) 0.0215(16) -0.0145(15) O5 0.032(2) 0.0163(15) 0.050(2) 0.0070(14) 0.0094(16) 0.0056(13) O6 0.0342(19) 0.0148(14) 0.0449(19) -0.0015(13) 0.0137(15) 0.0036(13) C1 0.032(3) 0.021(2) 0.033(2) 0.0084(18) 0.016(2) 0.0032(19) C2 0.030(3) 0.027(2) 0.028(2) 0.0087(18) 0.0103(19) -0.0019(19) C3 0.046(3) 0.036(3) 0.031(2) 0.006(2) 0.008(2) -0.015(2) C4 0.050(4) 0.045(3) 0.027(2) 0.008(2) 0.010(2) -0.016(3) C5 0.026(3) 0.034(3) 0.031(2) 0.0134(19) 0.011(2) 0.0001(19) C6 0.043(3) 0.043(3) 0.040(3) 0.007(2) 0.011(2) -0.017(2) C7 0.043(3) 0.045(3) 0.027(2) 0.006(2) 0.007(2) -0.011(2) C8 0.032(3) 0.028(2) 0.034(2) 0.0104(19) 0.013(2) -0.004(2) C9 0.024(3) 0.032(2) 0.036(3) 0.007(2) 0.012(2) -0.0057(19) C10 0.032(3) 0.026(2) 0.028(2) 0.0069(18) 0.012(2) -0.0023(19) C11 0.030(3) 0.025(2) 0.032(2) 0.0018(18) 0.018(2) -0.0050(19) C12 0.028(3) 0.040(3) 0.044(3) 0.009(2) 0.013(2) -0.008(2) C13 0.030(3) 0.049(3) 0.039(3) 0.018(2) 0.007(2) -0.003(2) C14 0.033(3) 0.019(2) 0.034(2) 0.0001(18) 0.019(2) 0.0006(19) C15 0.040(3) 0.016(2) 0.034(2) 0.0010(18) 0.013(2) 0.005(2) C16 0.037(3) 0.017(2) 0.043(3) 0.0038(19) 0.008(2) 0.0068(19) C17 0.058(4) 0.014(2) 0.096(5) 0.001(3) -0.024(4) 0.000(2) C18 0.065(4) 0.019(2) 0.096(5) 0.003(3) -0.035(4) 0.010(3) C19 0.052(4) 0.014(2) 0.053(3) 0.005(2) 0.008(3) 0.007(2) C20 0.038(4) 0.022(3) 0.174(8) 0.028(4) 0.006(4) 0.001(2) C21 0.034(3) 0.022(3) 0.150(7) 0.029(4) 0.002(4) 0.006(2) O7 0.033(2) 0.041(2) 0.0333(18) 0.0014(15) 0.0038(15) 0.0039(16) C22 0.040(3) 0.038(3) 0.050(3) 0.011(2) 0.007(3) 0.001(2) N1 0.051(4) 0.099(5) 0.074(4) 0.040(4) 0.004(3) 0.024(3) C23 0.060(6) 0.152(10) 0.171(11) 0.080(9) 0.025(6) 0.047(6) C24 0.088(8) 0.36(2) 0.060(6) 0.081(9) -0.002(6) 0.029(10) O8 0.124(11) 0.34(2) 0.48(3) -0.15(2) 0.055(15) -0.089(13) C25 0.114(14) 0.30(3) 0.22(2) 0.010(19) 0.014(15) -0.086(18) N2 0.210(17) 0.161(13) 0.167(13) 0.042(10) 0.071(13) 0.006(12) C26 0.145(15) 0.31(3) 0.172(16) 0.117(17) -0.006(12) -0.079(16) C27 0.80(10) 0.23(3) 0.40(4) 0.21(3) 0.35(6) 0.25(4) O9 0.084(7) 0.328(18) 0.244(14) 0.030(12) -0.035(8) -0.005(9) C28 0.069(7) 0.182(14) 0.171(13) 0.063(10) -0.024(8) -0.007(8) N3 0.073(5) 0.054(4) 0.104(5) 0.018(3) 0.011(4) 0.006(3) C29 0.106(9) 0.110(8) 0.121(8) 0.034(7) 0.022(7) -0.006(6) C30 0.24(2) 0.084(10) 0.39(3) 0.108(14) 0.05(2) 0.002(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O2 2.171(3) . ? Cd1 O2 2.171(3) 3 ? Cd1 O4 2.177(4) 4_655 ? Cd1 O4 2.177(4) 2_455 ? Cd1 O6 2.205(3) 3 ? Cd1 O6 2.205(3) . ? Zn1 O5 1.934(3) . ? Zn1 O1 1.935(3) . ? Zn1 O3 1.952(3) 4_655 ? Zn1 O7 2.007(3) . ? O1 C1 1.274(6) . ? O2 C1 1.241(6) . ? O3 C14 1.262(6) . ? O3 Zn1 1.952(3) 4_556 ? O4 C14 1.232(6) . ? O4 Cd1 2.177(4) 2_445 ? O5 C15 1.270(6) . ? O6 C15 1.241(6) . ? C1 C2 1.501(6) . ? C2 C7 1.377(7) . ? C2 C3 1.384(7) . ? C3 C4 1.364(7) . ? C4 C5 1.379(7) . ? C5 C6 1.385(7) . ? C5 C8 1.486(6) . ? C6 C7 1.387(7) . ? C8 C13 1.380(7) . ? C8 C9 1.393(7) . ? C9 C10 1.387(6) . ? C10 C11 1.392(7) . ? C11 C12 1.382(7) . ? C11 C14 1.497(6) . ? C12 C13 1.386(7) . ? C15 C16 1.492(6) . ? C16 C21 1.362(8) . ? C16 C17 1.369(8) . ? C17 C18 1.396(7) . ? C18 C19 1.363(8) . ? C19 C20 1.357(9) . ? C19 C19 1.511(9) 3_565 ? C20 C21 1.396(8) . ? O7 C22 1.234(7) . ? C22 N1 1.270(8) . ? N1 C23 1.472(11) . ? N1 C24 1.476(12) . ? O8 C25 1.34(3) . ? C25 N2 1.21(2) . ? N2 C26 1.38(2) . ? N2 C27 1.42(2) . ? O9 C28 1.288(16) . ? C28 N3 1.283(13) . ? N3 C30 1.382(14) . ? N3 C29 1.447(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cd1 O2 180.00(17) . 3 ? O2 Cd1 O4 92.84(13) . 4_655 ? O2 Cd1 O4 87.16(13) 3 4_655 ? O2 Cd1 O4 87.16(13) . 2_455 ? O2 Cd1 O4 92.84(13) 3 2_455 ? O4 Cd1 O4 180.00(16) 4_655 2_455 ? O2 Cd1 O6 86.89(12) . 3 ? O2 Cd1 O6 93.11(12) 3 3 ? O4 Cd1 O6 89.50(13) 4_655 3 ? O4 Cd1 O6 90.50(13) 2_455 3 ? O2 Cd1 O6 93.11(12) . . ? O2 Cd1 O6 86.89(12) 3 . ? O4 Cd1 O6 90.50(13) 4_655 . ? O4 Cd1 O6 89.50(13) 2_455 . ? O6 Cd1 O6 180.00(17) 3 . ? O5 Zn1 O1 115.45(15) . . ? O5 Zn1 O3 117.02(14) . 4_655 ? O1 Zn1 O3 117.74(15) . 4_655 ? O5 Zn1 O7 110.41(14) . . ? O1 Zn1 O7 94.63(15) . . ? O3 Zn1 O7 96.49(15) 4_655 . ? C1 O1 Zn1 122.2(3) . . ? C1 O2 Cd1 130.6(3) . . ? C14 O3 Zn1 117.3(3) . 4_556 ? C14 O4 Cd1 134.3(3) . 2_445 ? C15 O5 Zn1 115.6(3) . . ? C15 O6 Cd1 134.6(3) . . ? O2 C1 O1 125.5(4) . . ? O2 C1 C2 118.7(4) . . ? O1 C1 C2 115.7(4) . . ? C7 C2 C3 118.7(4) . . ? C7 C2 C1 120.6(4) . . ? C3 C2 C1 120.8(4) . . ? C4 C3 C2 120.6(5) . . ? C3 C4 C5 121.7(5) . . ? C4 C5 C6 117.8(4) . . ? C4 C5 C8 121.3(4) . . ? C6 C5 C8 120.9(4) . . ? C5 C6 C7 120.9(5) . . ? C2 C7 C6 120.4(5) . . ? C13 C8 C9 118.9(4) . . ? C13 C8 C5 121.0(4) . . ? C9 C8 C5 120.1(4) . . ? C10 C9 C8 120.9(4) . . ? C9 C10 C11 119.7(4) . . ? C12 C11 C10 119.3(4) . . ? C12 C11 C14 119.6(4) . . ? C10 C11 C14 121.1(4) . . ? C11 C12 C13 120.7(5) . . ? C8 C13 C12 120.5(5) . . ? O4 C14 O3 124.6(4) . . ? O4 C14 C11 118.6(4) . . ? O3 C14 C11 116.8(4) . . ? O6 C15 O5 124.6(4) . . ? O6 C15 C16 119.0(4) . . ? O5 C15 C16 116.3(4) . . ? C21 C16 C17 117.7(5) . . ? C21 C16 C15 121.7(5) . . ? C17 C16 C15 120.6(5) . . ? C16 C17 C18 120.9(5) . . ? C19 C18 C17 121.0(6) . . ? C20 C19 C18 118.1(5) . . ? C20 C19 C19 120.6(6) . 3_565 ? C18 C19 C19 121.2(6) . 3_565 ? C19 C20 C21 121.0(6) . . ? C16 C21 C20 121.2(6) . . ? C22 O7 Zn1 124.7(4) . . ? O7 C22 N1 125.4(6) . . ? C22 N1 C23 122.0(8) . . ? C22 N1 C24 120.0(7) . . ? C23 N1 C24 117.8(8) . . ? N2 C25 O8 122(3) . . ? C25 N2 C26 128.2(19) . . ? C25 N2 C27 110(3) . . ? C26 N2 C27 122(3) . . ? N3 C28 O9 117.6(13) . . ? C28 N3 C30 123.0(12) . . ? C28 N3 C29 118.1(9) . . ? C30 N3 C29 118.8(10) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 25.93 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 1.151 _refine_diff_density_min -1.657 _refine_diff_density_rms 0.125 _exptl_crystal_recrystallization_method solvothermal # Attachment 'compound_2.cif' data_wan588 _database_code_depnum_ccdc_archive 'CCDC 613449' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H38 N2 Ni O14 Zn2, 4(C3 H7 N O)' _chemical_formula_sum 'C60 H66 N6 Ni O18 Zn2' _chemical_formula_weight 1348.64 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' Ni Ni 0.3393 1.1124 '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 'P 21/n' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.670(2) _cell_length_b 14.742(3) _cell_length_c 19.391(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.29(3) _cell_angle_gamma 90.00 _cell_volume 3259.5(11) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 1128 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 25.8 _exptl_crystal_description 'block shaped' _exptl_crystal_colour 'light green' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 1.088 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24998 _diffrn_reflns_av_R_equivalents 0.1365 _diffrn_reflns_av_sigmaI/netI 0.1078 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.88 _reflns_number_total 6008 _reflns_number_gt 3708 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE EXPOSE' _computing_cell_refinement 'STOE CELL' _computing_data_reduction 'STOE INTEGRATE' _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^)+(0.1616P)^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 6008 _refine_ls_number_parameters 394 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.1252 _refine_ls_R_factor_gt 0.0838 _refine_ls_wR_factor_ref 0.2515 _refine_ls_wR_factor_gt 0.2247 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.003 _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 Ni1 Ni 0.0000 0.0000 0.0000 0.0263(3) Uani 1 2 d S . . Zn1 Zn 0.26121(7) 0.03903(5) 0.12237(4) 0.0368(3) Uani 1 1 d . . . O1 O 0.1619(5) -0.0252(4) 0.1741(3) 0.0514(13) Uani 1 1 d . . . O2 O 0.0292(8) -0.0818(5) 0.0845(3) 0.101(3) Uani 1 1 d . . . O3 O -0.1677(5) -0.4712(4) 0.5564(3) 0.0595(15) Uani 1 1 d . . . O4 O -0.3347(7) -0.4805(9) 0.4864(6) 0.152(5) Uani 1 1 d . . . O5 O 0.2268(5) 0.1651(3) 0.0965(3) 0.0566(14) Uani 1 1 d . . . O6 O 0.0431(6) 0.1187(4) 0.0582(3) 0.0778(19) Uani 1 1 d . . . C1 C 0.0723(8) -0.0698(6) 0.1498(4) 0.061(2) Uani 1 1 d . . . C2 C 0.0217(7) -0.1240(6) 0.2005(4) 0.055(2) Uani 1 1 d . . . C3 C 0.0733(8) -0.1250(6) 0.2706(4) 0.060(2) Uani 1 1 d . . . H3 H 0.1400 -0.0879 0.2875 0.071 Uiso 1 1 calc R . . C4 C 0.0302(8) -0.1789(7) 0.3172(4) 0.068(3) Uani 1 1 d . . . H4 H 0.0697 -0.1787 0.3654 0.081 Uiso 1 1 calc R . . C5 C -0.0656(7) -0.2320(6) 0.2976(4) 0.056(2) Uani 1 1 d . . . C6 C -0.1162(11) -0.2327(10) 0.2262(6) 0.122(6) Uani 1 1 d . . . H6 H -0.1833 -0.2696 0.2099 0.146 Uiso 1 1 calc R . . C7 C -0.0730(11) -0.1824(10) 0.1784(6) 0.119(6) Uani 1 1 d . . . H7 H -0.1078 -0.1871 0.1296 0.143 Uiso 1 1 calc R . . C8 C -0.1108(7) -0.2898(5) 0.3488(4) 0.0519(19) Uani 1 1 d . . . C9 C -0.0333(7) -0.3264(5) 0.4051(5) 0.056(2) Uani 1 1 d . . . H9 H 0.0484 -0.3158 0.4103 0.067 Uiso 1 1 calc R . . C10 C -0.0742(7) -0.3794(5) 0.4552(5) 0.054(2) Uani 1 1 d . . . H10 H -0.0199 -0.4046 0.4939 0.065 Uiso 1 1 calc R . . C11 C -0.1914(7) -0.3948(5) 0.4485(4) 0.0524(19) Uani 1 1 d . . . C12 C -0.2674(9) -0.3630(9) 0.3891(6) 0.094(4) Uani 1 1 d . . . H12 H -0.3487 -0.3766 0.3817 0.113 Uiso 1 1 calc R . . C13 C -0.2262(8) -0.3121(9) 0.3409(5) 0.092(4) Uani 1 1 d . . . H13 H -0.2802 -0.2912 0.3002 0.110 Uiso 1 1 calc R . . C14 C -0.2359(8) -0.4505(6) 0.5013(5) 0.061(2) Uani 1 1 d . . . C15 C 0.1229(8) 0.1781(5) 0.0655(4) 0.050(2) Uani 1 1 d . . . C16 C 0.0868(7) 0.2735(4) 0.0453(4) 0.0492(19) Uani 1 1 d . . . C17 C -0.0253(10) 0.2936(6) 0.0131(7) 0.101(4) Uani 1 1 d . . . H17 H -0.0821 0.2466 0.0026 0.121 Uiso 1 1 calc R . . C18 C -0.0572(10) 0.3835(6) -0.0047(7) 0.106(5) Uani 1 1 d . . . H18 H -0.1359 0.3960 -0.0276 0.128 Uiso 1 1 calc R . . C19 C 0.0181(7) 0.4518(4) 0.0090(4) 0.053(2) Uani 1 1 d . . . C20 C 0.1289(9) 0.4317(6) 0.0430(8) 0.112(5) Uani 1 1 d . . . H20 H 0.1851 0.4789 0.0551 0.135 Uiso 1 1 calc R . . C21 C 0.1610(9) 0.3421(7) 0.0603(9) 0.120(6) Uani 1 1 d . . . H21 H 0.2395 0.3298 0.0839 0.145 Uiso 1 1 calc R . . O7 O 0.4034(6) 0.0425(4) 0.2019(3) 0.0729(18) Uani 1 1 d . . . C22 C 0.5028(10) 0.0070(8) 0.1993(7) 0.092(4) Uani 1 1 d . . . H22 H 0.5179 -0.0093 0.1547 0.111 Uiso 1 1 calc R . . N1 N 0.5837(11) -0.0072(10) 0.2558(8) 0.148(6) Uani 1 1 d . . . C23 C 0.6982(15) -0.0513(18) 0.2486(18) 0.267(17) Uani 1 1 d . . . H23A H 0.6899 -0.0759 0.2008 0.400 Uiso 1 1 calc R . . H23B H 0.7177 -0.1005 0.2831 0.400 Uiso 1 1 calc R . . H23C H 0.7610 -0.0059 0.2571 0.400 Uiso 1 1 calc R . . C24 C 0.5686(19) 0.002(3) 0.3240(11) 0.31(2) Uani 1 1 d . . . H24A H 0.5503 0.0649 0.3327 0.468 Uiso 1 1 calc R . . H24B H 0.6409 -0.0163 0.3570 0.468 Uiso 1 1 calc R . . H24C H 0.5040 -0.0375 0.3308 0.468 Uiso 1 1 calc R . . O8 O 0.355(2) -0.430(2) 0.040(3) 0.42(2) Uani 1 1 d . . . C25 C 0.444(3) -0.3851(15) 0.025(2) 0.200(12) Uani 1 1 d . . . H25 H 0.4341 -0.3550 -0.0188 0.240 Uiso 1 1 calc R . . N2 N 0.545(3) -0.380(2) 0.0692(11) 0.206(10) Uani 1 1 d . . . C26 C 0.634(3) -0.331(3) 0.0640(18) 0.37(4) Uani 1 1 d . . . H26A H 0.6321 -0.3183 0.0142 0.554 Uiso 1 1 calc R . . H26B H 0.7065 -0.3643 0.0844 0.554 Uiso 1 1 calc R . . H26C H 0.6323 -0.2741 0.0896 0.554 Uiso 1 1 calc R . . C27 C 0.544(6) -0.439(3) 0.128(2) 0.51(5) Uani 1 1 d . . . H27A H 0.6102 -0.4813 0.1327 0.762 Uiso 1 1 calc R . . H27B H 0.4705 -0.4730 0.1193 0.762 Uiso 1 1 calc R . . H27C H 0.5517 -0.4028 0.1707 0.762 Uiso 1 1 calc R . . O9 O 0.528(3) -0.2170(19) 0.197(2) 0.43(2) Uani 1 1 d DU . . C28 C 0.468(3) -0.262(4) 0.2390(15) 0.51(4) Uani 1 1 d DU . . H28 H 0.4959 -0.2787 0.2870 0.607 Uiso 1 1 calc R . . N3 N 0.3581(14) -0.2797(9) 0.1990(7) 0.133(5) Uani 1 1 d DU . . C29 C 0.261(3) -0.340(3) 0.204(2) 0.35(2) Uani 1 1 d U . . H29A H 0.1972 -0.3046 0.2171 0.521 Uiso 1 1 calc R . . H29B H 0.2879 -0.3859 0.2408 0.521 Uiso 1 1 calc R . . H29C H 0.2318 -0.3701 0.1589 0.521 Uiso 1 1 calc R . . C30 C 0.314(3) -0.2311(15) 0.1420(14) 0.282(18) Uani 1 1 d U . . H30A H 0.2761 -0.1767 0.1557 0.423 Uiso 1 1 calc R . . H30B H 0.2561 -0.2674 0.1094 0.423 Uiso 1 1 calc R . . H30C H 0.3772 -0.2132 0.1186 0.423 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0399(6) 0.0204(5) 0.0168(5) 0.0014(4) 0.0023(4) 0.0016(4) Zn1 0.0525(5) 0.0295(4) 0.0272(4) 0.0001(3) 0.0057(3) 0.0007(3) O1 0.064(3) 0.059(3) 0.030(3) 0.013(2) 0.007(2) -0.008(3) O2 0.160(7) 0.085(5) 0.050(4) 0.020(3) 0.004(4) -0.053(5) O3 0.079(4) 0.052(3) 0.051(3) 0.012(2) 0.021(3) -0.007(3) O4 0.073(5) 0.230(12) 0.147(9) 0.118(9) 0.011(6) -0.026(6) O5 0.063(3) 0.036(3) 0.067(4) 0.007(2) 0.004(3) 0.007(2) O6 0.105(5) 0.048(3) 0.068(4) -0.007(3) -0.007(4) -0.010(3) C1 0.085(6) 0.068(5) 0.026(4) 0.020(4) 0.002(4) -0.010(5) C2 0.064(5) 0.064(5) 0.034(4) 0.017(3) 0.007(4) -0.011(4) C3 0.075(5) 0.065(5) 0.030(4) 0.010(3) -0.007(4) -0.029(4) C4 0.076(6) 0.089(7) 0.033(4) 0.023(4) 0.000(4) -0.024(5) C5 0.058(5) 0.065(5) 0.044(4) 0.016(4) 0.005(4) -0.016(4) C6 0.119(9) 0.171(13) 0.056(6) 0.041(7) -0.026(6) -0.098(9) C7 0.116(9) 0.170(12) 0.054(6) 0.049(7) -0.022(6) -0.083(9) C8 0.055(5) 0.060(5) 0.039(4) 0.012(3) 0.007(4) -0.014(4) C9 0.057(5) 0.055(5) 0.063(5) 0.015(4) 0.028(4) 0.002(4) C10 0.057(5) 0.052(4) 0.057(5) 0.018(4) 0.021(4) 0.012(4) C11 0.057(5) 0.051(4) 0.050(5) 0.011(3) 0.013(4) -0.014(3) C12 0.058(6) 0.136(10) 0.084(8) 0.052(7) 0.003(5) -0.023(6) C13 0.061(6) 0.142(10) 0.065(7) 0.051(7) -0.006(5) -0.019(6) C14 0.059(5) 0.065(6) 0.058(5) 0.022(4) 0.011(4) -0.011(4) C15 0.086(6) 0.028(3) 0.034(4) -0.005(3) 0.004(4) -0.006(4) C16 0.065(5) 0.025(3) 0.051(4) -0.002(3) -0.003(4) -0.002(3) C17 0.092(8) 0.037(4) 0.140(10) 0.002(5) -0.050(7) -0.008(5) C18 0.102(8) 0.032(4) 0.145(11) 0.013(5) -0.063(7) 0.000(5) C19 0.071(5) 0.029(4) 0.052(5) 0.002(3) -0.005(4) -0.001(3) C20 0.062(6) 0.036(5) 0.216(15) 0.021(7) -0.019(7) 0.004(4) C21 0.054(6) 0.048(5) 0.233(17) 0.042(8) -0.029(7) 0.002(4) O7 0.080(4) 0.077(4) 0.052(4) 0.006(3) -0.008(3) -0.023(3) C22 0.078(7) 0.091(8) 0.092(8) 0.023(6) -0.017(6) -0.008(6) N1 0.111(9) 0.170(12) 0.131(11) 0.073(9) -0.044(8) -0.021(8) C23 0.080(11) 0.27(3) 0.41(5) 0.06(3) -0.045(18) 0.036(14) C24 0.129(17) 0.74(7) 0.075(13) -0.04(2) 0.041(13) -0.07(3) O8 0.25(2) 0.28(3) 0.77(8) -0.04(4) 0.16(4) -0.09(2) C25 0.21(3) 0.129(16) 0.30(4) 0.02(2) 0.12(3) -0.052(18) N2 0.21(2) 0.27(3) 0.139(16) 0.033(17) 0.036(17) 0.05(2) C26 0.32(4) 0.56(8) 0.22(4) 0.09(4) 0.03(3) -0.27(5) C27 0.90(13) 0.38(6) 0.38(6) 0.26(5) 0.42(8) 0.38(7) O9 0.48(4) 0.19(2) 0.58(6) 0.01(3) 0.04(4) -0.02(3) C28 0.49(6) 0.64(8) 0.23(3) 0.00(4) -0.28(4) 0.09(5) N3 0.186(13) 0.096(8) 0.118(10) 0.018(7) 0.036(10) 0.029(8) C29 0.39(5) 0.35(4) 0.31(4) 0.09(4) 0.12(4) -0.13(4) C30 0.54(5) 0.113(16) 0.21(2) 0.069(17) 0.11(3) 0.10(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 Ni1 O2 2.004(6) 3 ? Ni1 O2 2.004(6) . ? Ni1 O4 2.022(8) 4_655 ? Ni1 O4 2.022(8) 2_455 ? Ni1 O6 2.086(6) 3 ? Ni1 O6 2.086(6) . ? Zn1 O1 1.934(5) . ? Zn1 O3 1.942(5) 4_655 ? Zn1 O5 1.944(5) . ? Zn1 O7 2.012(6) . ? O1 C1 1.240(10) . ? O2 C1 1.271(10) . ? O3 C14 1.227(10) . ? O3 Zn1 1.942(5) 4_556 ? O4 C14 1.211(11) . ? O4 Ni1 2.022(8) 2_445 ? O5 C15 1.248(9) . ? O6 C15 1.264(10) . ? C1 C2 1.484(11) . ? C2 C3 1.364(10) . ? C2 C7 1.395(13) . ? C3 C4 1.376(11) . ? C4 C5 1.352(11) . ? C5 C6 1.386(12) . ? C5 C8 1.487(10) . ? C6 C7 1.365(14) . ? C8 C13 1.363(12) . ? C8 C9 1.371(11) . ? C9 C10 1.407(11) . ? C10 C11 1.365(11) . ? C11 C12 1.378(12) . ? C11 C14 1.490(11) . ? C12 C13 1.363(13) . ? C15 C16 1.496(10) . ? C16 C21 1.324(12) . ? C16 C17 1.357(12) . ? C17 C18 1.400(12) . ? C18 C19 1.326(12) . ? C19 C20 1.353(12) . ? C19 C19 1.502(13) 3_565 ? C20 C21 1.394(13) . ? O7 C22 1.283(14) . ? C22 N1 1.302(15) . ? N1 C24 1.38(2) . ? N1 C23 1.52(2) . ? O8 C25 1.32(3) . ? C25 N2 1.30(3) . ? N2 C26 1.29(3) . ? N2 C27 1.43(4) . ? O9 C28 1.352(19) . ? C28 N3 1.371(17) . ? N3 C30 1.33(2) . ? N3 C29 1.47(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ni1 O2 180.0(4) 3 . ? O2 Ni1 O4 88.9(5) 3 4_655 ? O2 Ni1 O4 91.1(5) . 4_655 ? O2 Ni1 O4 91.1(5) 3 2_455 ? O2 Ni1 O4 88.9(5) . 2_455 ? O4 Ni1 O4 180.0(6) 4_655 2_455 ? O2 Ni1 O6 94.8(3) 3 3 ? O2 Ni1 O6 85.2(3) . 3 ? O4 Ni1 O6 86.4(3) 4_655 3 ? O4 Ni1 O6 93.6(3) 2_455 3 ? O2 Ni1 O6 85.2(3) 3 . ? O2 Ni1 O6 94.8(3) . . ? O4 Ni1 O6 93.6(3) 4_655 . ? O4 Ni1 O6 86.4(3) 2_455 . ? O6 Ni1 O6 180.0(4) 3 . ? O1 Zn1 O3 118.4(3) . 4_655 ? O1 Zn1 O5 119.2(2) . . ? O3 Zn1 O5 114.6(3) 4_655 . ? O1 Zn1 O7 95.9(2) . . ? O3 Zn1 O7 96.9(3) 4_655 . ? O5 Zn1 O7 105.4(2) . . ? C1 O1 Zn1 127.8(5) . . ? C1 O2 Ni1 133.9(6) . . ? C14 O3 Zn1 114.4(6) . 4_556 ? C14 O4 Ni1 155.1(12) . 2_445 ? C15 O5 Zn1 113.4(5) . . ? C15 O6 Ni1 136.8(6) . . ? O1 C1 O2 125.1(8) . . ? O1 C1 C2 117.1(6) . . ? O2 C1 C2 117.2(8) . . ? C3 C2 C7 116.9(8) . . ? C3 C2 C1 120.8(7) . . ? C7 C2 C1 122.0(7) . . ? C2 C3 C4 120.9(7) . . ? C5 C4 C3 123.2(7) . . ? C4 C5 C6 115.8(8) . . ? C4 C5 C8 122.3(7) . . ? C6 C5 C8 121.8(7) . . ? C7 C6 C5 122.3(9) . . ? C6 C7 C2 120.7(9) . . ? C13 C8 C9 117.6(8) . . ? C13 C8 C5 123.0(7) . . ? C9 C8 C5 119.3(7) . . ? C8 C9 C10 120.3(8) . . ? C11 C10 C9 120.5(8) . . ? C10 C11 C12 118.4(8) . . ? C10 C11 C14 121.0(7) . . ? C12 C11 C14 120.4(7) . . ? C13 C12 C11 120.2(9) . . ? C12 C13 C8 122.6(8) . . ? O4 C14 O3 121.7(8) . . ? O4 C14 C11 119.4(8) . . ? O3 C14 C11 118.7(7) . . ? O5 C15 O6 124.4(7) . . ? O5 C15 C16 117.5(6) . . ? O6 C15 C16 117.5(7) . . ? C21 C16 C17 117.1(7) . . ? C21 C16 C15 121.7(7) . . ? C17 C16 C15 121.1(7) . . ? C16 C17 C18 120.0(9) . . ? C19 C18 C17 122.7(9) . . ? C18 C19 C20 117.1(8) . . ? C18 C19 C19 122.0(9) . 3_565 ? C20 C19 C19 120.8(9) . 3_565 ? C19 C20 C21 120.3(9) . . ? C16 C21 C20 122.8(9) . . ? C22 O7 Zn1 124.4(8) . . ? O7 C22 N1 122.2(15) . . ? C22 N1 C24 125.1(18) . . ? C22 N1 C23 119.1(19) . . ? C24 N1 C23 115.1(18) . . ? N2 C25 O8 123(4) . . ? C26 N2 C25 128(3) . . ? C26 N2 C27 123(4) . . ? C25 N2 C27 109(4) . . ? O9 C28 N3 107(2) . . ? C30 N3 C28 121(2) . . ? C30 N3 C29 103(2) . . ? C28 N3 C29 136(2) . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 25.88 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 1.513 _refine_diff_density_min -0.971 _refine_diff_density_rms 0.133 _exptl_crystal_recrystallization_method solvothermal