# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_compound_2b _database_code_depnum_ccdc_archive 'CCDC 258414' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H126 Cl4 N24 Ni8 O52.50' _chemical_formula_weight 2707.39 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' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 20.3117(3) _cell_length_b 17.8243(3) _cell_length_c 18.3675(3) _cell_angle_alpha 104.4870(10) _cell_angle_beta 115.9840(10) _cell_angle_gamma 92.9850(10) _cell_volume 5686.82(16) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2804 _exptl_absorpt_coefficient_mu 1.487 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52077 _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_av_sigmaI/netI 0.0653 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 28.78 _reflns_number_total 25919 _reflns_number_gt 19048 _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1497P)^2^+14.8975P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0229(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 25919 _refine_ls_number_parameters 1394 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1180 _refine_ls_R_factor_gt 0.0866 _refine_ls_wR_factor_ref 0.2733 _refine_ls_wR_factor_gt 0.2346 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.406 _refine_ls_shift/su_mean 0.099 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 0.37104(3) 0.14094(4) 0.11319(4) 0.03110(14) Uani 1 1 d . . . Ni2 Ni 0.16915(4) 0.41929(4) -0.01738(4) 0.03553(15) Uani 1 1 d . . . Ni3 Ni 0.34152(4) -0.00606(4) -0.20251(4) 0.03698(15) Uani 1 1 d . . . Ni4 Ni 0.18288(4) 0.01783(4) 0.21242(4) 0.04221(16) Uani 1 1 d . . . Ni5 Ni 0.40673(4) 0.66388(4) 0.18596(5) 0.04549(17) Uani 1 1 d . . . Ni6 Ni 0.11320(4) 0.28384(5) -0.34481(4) 0.04589(18) Uani 1 1 d . . . Ni7 Ni 0.60756(4) 0.34805(4) 0.38809(5) 0.04809(18) Uani 1 1 d . . . Ni8 Ni -0.01954(4) 0.35252(5) 0.10557(5) 0.04607(18) Uani 1 1 d . . . O1 O 0.1055(2) 0.4734(2) 0.0360(3) 0.0468(9) Uani 1 1 d . . . O2 O 0.0432(3) 0.4476(2) 0.1030(3) 0.0530(10) Uani 1 1 d . . . O3 O 0.0344(2) 0.2922(2) 0.0415(3) 0.0463(9) Uani 1 1 d . . . O4 O 0.0856(2) 0.4003(2) -0.1433(2) 0.0405(8) Uani 1 1 d . . . O5 O 0.0634(2) 0.3465(3) -0.2773(2) 0.0484(9) Uani 1 1 d . . . O6 O 0.1989(2) 0.3069(3) -0.2224(2) 0.0516(10) Uani 1 1 d . . . O7 O 0.3640(2) 0.5544(2) 0.1880(3) 0.0505(9) Uani 1 1 d . . . O8 O 0.2107(2) 0.5318(2) -0.0114(3) 0.0506(10) Uani 1 1 d . . . O9 O 0.3081(3) 0.6289(2) 0.0692(3) 0.0592(11) Uani 1 1 d . . . O10 O 0.3676(2) 0.0296(2) 0.0374(2) 0.0384(7) Uani 1 1 d . . . O11 O 0.3582(2) -0.0293(2) -0.0901(2) 0.0425(8) Uani 1 1 d . . . O12 O 0.3524(2) 0.1081(2) -0.1261(2) 0.0399(8) Uani 1 1 d . . . O13 O 0.1757(2) 0.0685(3) 0.1178(3) 0.0471(9) Uani 1 1 d . . . O14 O 0.2909(2) 0.0223(2) 0.2289(2) 0.0418(8) Uani 1 1 d . . . O15 O 0.36930(19) 0.0845(2) 0.1992(2) 0.0372(7) Uani 1 1 d . . . O16 O 0.49011(19) 0.1583(2) 0.1760(2) 0.0369(7) Uani 1 1 d . . . O17 O 0.5870(2) 0.2394(2) 0.2921(3) 0.0493(9) Uani 1 1 d . . . O18 O 0.5023(2) 0.3487(2) 0.2996(3) 0.0515(10) Uani 1 1 d . . . N1 N 0.1162(2) 0.3218(2) -0.0085(3) 0.0347(8) Uani 1 1 d . . . N2 N 0.2607(2) 0.4543(2) 0.1027(3) 0.0361(8) Uani 1 1 d . . . N3 N 0.2208(2) 0.3641(2) -0.0847(3) 0.0348(8) Uani 1 1 d . . . N4 N 0.2564(2) 0.1192(2) 0.0760(2) 0.0316(8) Uani 1 1 d . . . N5 N 0.3667(2) 0.1688(2) 0.0083(2) 0.0318(8) Uani 1 1 d . . . N6 N 0.3992(2) 0.2541(2) 0.1977(2) 0.0332(8) Uani 1 1 d . . . N10 N 0.0750(4) 0.1776(4) -0.3338(5) 0.0704(16) Uani 1 1 d . . . N11 N 0.1633(4) 0.3854(4) -0.3516(4) 0.0699(16) Uani 1 1 d . . . N12 N 0.0206(4) 0.2585(4) -0.4654(3) 0.0734(18) Uani 1 1 d . . . N14 N 0.2281(3) -0.0229(4) -0.2326(4) 0.0661(16) Uani 1 1 d . . . N15 N 0.4566(3) 0.0086(3) -0.1554(3) 0.0500(11) Uani 1 1 d . . . N17 N 0.3217(4) 0.0271(4) -0.3116(3) 0.0713(17) Uani 1 1 d . . . N19 N 0.2025(3) -0.0273(4) 0.3139(3) 0.0575(13) Uani 1 1 d . . . N24 N 0.6017(4) 0.4508(3) 0.4690(4) 0.0669(16) Uani 1 1 d . . . N27 N 0.4597(4) 0.6031(4) 0.1195(4) 0.0708(16) Uani 1 1 d . . . N18 N 0.2148(4) 0.1309(4) 0.3012(4) 0.0630(14) Uani 1 1 d . . . N20 N 0.1477(3) -0.0902(3) 0.1174(4) 0.0634(14) Uani 1 1 d . . . N21 N 0.6603(5) 0.4074(4) 0.3421(5) 0.093(2) Uani 1 1 d . . . N23 N 0.7053(4) 0.3278(5) 0.4813(5) 0.091(2) Uani 1 1 d . . . N26 N -0.0847(3) 0.2527(4) 0.0915(5) 0.0672(16) Uani 1 1 d . . . N50 N 0.3406(4) 0.7177(4) 0.2380(5) 0.0713(17) Uani 1 1 d . . . N51 N 0.5048(3) 0.6891(3) 0.3020(3) 0.0623(14) Uani 1 1 d . . . N53 N 0.0682(3) 0.3476(4) 0.2195(4) 0.0627(14) Uani 1 1 d . . . N54 N -0.0685(4) 0.4316(4) 0.1613(4) 0.0691(16) Uani 1 1 d . . . C1 C 0.0737(3) 0.3388(3) 0.0270(3) 0.0372(10) Uani 1 1 d . . . C2 C 0.0739(3) 0.4276(3) 0.0561(3) 0.0426(11) Uani 1 1 d . . . C3 C 0.1814(3) 0.3434(3) -0.1659(3) 0.0378(10) Uani 1 1 d . . . C4 C 0.1035(3) 0.3662(3) -0.1979(3) 0.0387(10) Uani 1 1 d . . . C5 C 0.3021(3) 0.5201(3) 0.1213(3) 0.0392(10) Uani 1 1 d . . . C6 C 0.2710(3) 0.5641(3) 0.0542(4) 0.0444(12) Uani 1 1 d . . . C7 C 0.2393(3) 0.0853(3) 0.1214(3) 0.0359(10) Uani 1 1 d . . . C8 C 0.3051(3) 0.0619(3) 0.1886(3) 0.0333(9) Uani 1 1 d . . . C9 C 0.3606(3) 0.1092(3) -0.0528(3) 0.0328(9) Uani 1 1 d . . . C10 C 0.3628(3) 0.0304(3) -0.0332(3) 0.0343(9) Uani 1 1 d . . . C11 C 0.4695(3) 0.2802(3) 0.2460(3) 0.0363(10) Uani 1 1 d . . . C12 C 0.5197(3) 0.2204(3) 0.2369(3) 0.0344(9) Uani 1 1 d . . . C13 C 0.1278(2) 0.2430(3) -0.0303(3) 0.0319(9) Uani 1 1 d . . . C14 C 0.1793(3) 0.2156(3) 0.0323(3) 0.0319(9) Uani 1 1 d . . . H14 H 0.2015 0.2468 0.0888 0.038 Uiso 1 1 calc R . . C15 C 0.1982(2) 0.1422(3) 0.0114(3) 0.0318(9) Uani 1 1 d . . . C16 C 0.1631(3) 0.0939(3) -0.0731(3) 0.0368(10) Uani 1 1 d . . . H16 H 0.1754 0.0447 -0.0875 0.044 Uiso 1 1 calc R . . C17 C 0.1097(3) 0.1198(3) -0.1351(3) 0.0404(11) Uani 1 1 d . . . H17 H 0.0851 0.0869 -0.1910 0.048 Uiso 1 1 calc R . . C18 C 0.0922(3) 0.1942(3) -0.1154(3) 0.0375(10) Uani 1 1 d . . . H18 H 0.0574 0.2115 -0.1579 0.045 Uiso 1 1 calc R . . C19 C 0.3648(3) 0.2443(3) -0.0034(3) 0.0316(9) Uani 1 1 d . . . C20 C 0.2957(3) 0.2652(3) -0.0454(3) 0.0334(9) Uani 1 1 d . . . H20 H 0.2523 0.2278 -0.0698 0.040 Uiso 1 1 calc R . . C21 C 0.2914(3) 0.3414(3) -0.0509(3) 0.0352(9) Uani 1 1 d . . . C22 C 0.3564(3) 0.3962(3) -0.0171(3) 0.0408(11) Uani 1 1 d . . . H22 H 0.3540 0.4470 -0.0213 0.049 Uiso 1 1 calc R . . C23 C 0.4298(3) 0.2994(3) 0.0315(3) 0.0404(11) Uani 1 1 d . . . H23 H 0.4759 0.2862 0.0602 0.048 Uiso 1 1 calc R . . C24 C 0.2830(3) 0.4075(3) 0.1591(3) 0.0338(9) Uani 1 1 d . . . C25 C 0.3345(3) 0.3587(3) 0.1577(3) 0.0345(9) Uani 1 1 d . . . H25 H 0.3581 0.3613 0.1248 0.041 Uiso 1 1 calc R . . C26 C 0.3503(3) 0.3066(3) 0.2050(3) 0.0330(9) Uani 1 1 d . . . C27 C 0.4250(3) 0.3748(3) 0.0229(4) 0.0443(11) Uani 1 1 d . . . H27 H 0.4685 0.4113 0.0445 0.053 Uiso 1 1 calc R . . C28 C 0.2498(3) 0.4049(3) 0.2107(3) 0.0424(11) Uani 1 1 d . . . H28 H 0.2155 0.4370 0.2120 0.051 Uiso 1 1 calc R . . C29 C 0.2680(3) 0.3543(3) 0.2602(3) 0.0418(11) Uani 1 1 d . . . H29 H 0.2468 0.3538 0.2959 0.050 Uiso 1 1 calc R . . C30 C 0.3178(3) 0.3043(3) 0.2568(3) 0.0405(11) Uani 1 1 d . . . H30 H 0.3290 0.2697 0.2892 0.049 Uiso 1 1 calc R . . C31 C 0.2880(5) 0.1451(5) 0.3771(5) 0.073(2) Uani 1 1 d . . . H31A H 0.3008 0.2000 0.4111 0.087 Uiso 1 1 calc R . . H31B H 0.3260 0.1342 0.3596 0.087 Uiso 1 1 calc R . . C32 C 0.2858(5) 0.0932(6) 0.4294(5) 0.077(2) Uani 1 1 d . . . H32A H 0.3320 0.1090 0.4824 0.092 Uiso 1 1 calc R . . H32B H 0.2454 0.1023 0.4433 0.092 Uiso 1 1 calc R . . C33 C 0.2757(4) 0.0074(5) 0.3882(5) 0.0687(19) Uani 1 1 d . . . H33A H 0.3140 -0.0014 0.3707 0.082 Uiso 1 1 calc R . . H33B H 0.2829 -0.0200 0.4299 0.082 Uiso 1 1 calc R . . C34 C 0.1300(6) -0.1655(5) 0.1310(6) 0.086(3) Uani 1 1 d . . . H34A H 0.1682 -0.1962 0.1319 0.104 Uiso 1 1 calc R . . H34B H 0.0830 -0.1951 0.0832 0.104 Uiso 1 1 calc R . . C35 C 0.1241(6) -0.1560(6) 0.2136(8) 0.102(3) Uani 1 1 d . . . H35A H 0.0844 -0.1272 0.2117 0.122 Uiso 1 1 calc R . . H35B H 0.1104 -0.2079 0.2162 0.122 Uiso 1 1 calc R . . C36 C -0.0456(5) 0.1861(5) 0.1131(6) 0.081(2) Uani 1 1 d . . . H36A H -0.0811 0.1439 0.1080 0.097 Uiso 1 1 calc R . . H36B H -0.0277 0.1656 0.0723 0.097 Uiso 1 1 calc R . . C37 C 0.0188(7) 0.2102(7) 0.2010(7) 0.099(3) Uani 1 1 d . . . H37A H 0.0365 0.1629 0.2126 0.119 Uiso 1 1 calc R . . H37B H 0.0000 0.2317 0.2406 0.119 Uiso 1 1 calc R . . C40 C 0.5370(6) 0.6219(8) 0.1463(8) 0.106(4) Uani 1 1 d . . . H40A H 0.5463 0.6688 0.1319 0.127 Uiso 1 1 calc R . . H40B H 0.5507 0.5792 0.1145 0.127 Uiso 1 1 calc R . . C41 C 0.5862(5) 0.6360(7) 0.2380(7) 0.098(3) Uani 1 1 d . . . H41A H 0.6377 0.6446 0.2491 0.117 Uiso 1 1 calc R . . H41B H 0.5775 0.5892 0.2528 0.117 Uiso 1 1 calc R . . C42 C 0.5743(4) 0.7041(5) 0.2926(6) 0.081(2) Uani 1 1 d . . . H42A H 0.5716 0.7477 0.2693 0.098 Uiso 1 1 calc R . . H42B H 0.6172 0.7200 0.3486 0.098 Uiso 1 1 calc R . . C43 C 0.5054(6) 0.7572(5) 0.3709(5) 0.093(3) Uani 1 1 d . . . H43A H 0.5500 0.7630 0.4236 0.111 Uiso 1 1 calc R . . H43B H 0.5080 0.8052 0.3558 0.111 Uiso 1 1 calc R . . C44 C 0.3730(7) 0.7721(6) 0.3250(7) 0.098(3) Uani 1 1 d . . . H44A H 0.3356 0.7739 0.3444 0.117 Uiso 1 1 calc R . . H44B H 0.3872 0.8248 0.3245 0.117 Uiso 1 1 calc R . . C45 C -0.0401(7) 0.4593(6) 0.2490(6) 0.097(3) Uani 1 1 d . . . H45A H -0.0671 0.4255 0.2647 0.116 Uiso 1 1 calc R . . H45B H -0.0518 0.5114 0.2627 0.116 Uiso 1 1 calc R . . C46 C 0.0402(7) 0.4651(6) 0.3039(6) 0.097(3) Uani 1 1 d . . . H46A H 0.0673 0.5016 0.2908 0.116 Uiso 1 1 calc R . . H46B H 0.0504 0.4887 0.3623 0.116 Uiso 1 1 calc R . . C47 C -0.0054(5) 0.1630(6) -0.3531(6) 0.083(2) Uani 1 1 d . . . H47A H -0.0168 0.1138 -0.3436 0.100 Uiso 1 1 calc R . . H47B H -0.0142 0.2052 -0.3152 0.100 Uiso 1 1 calc R . . C48 C -0.0552(5) 0.1588(7) -0.4436(6) 0.095(3) Uani 1 1 d . . . H48A H -0.0435 0.1182 -0.4800 0.114 Uiso 1 1 calc R . . H48B H -0.1063 0.1419 -0.4564 0.114 Uiso 1 1 calc R . . C49 C 0.1204(7) 0.4330(6) -0.4052(7) 0.094(3) Uani 1 1 d . . . H49A H 0.1053 0.4734 -0.3725 0.113 Uiso 1 1 calc R . . H49B H 0.1517 0.4590 -0.4225 0.113 Uiso 1 1 calc R . . C50 C 0.2457(7) 0.0041(8) -0.3833(5) 0.111(4) Uani 1 1 d . . . H50A H 0.2422 0.0360 -0.4202 0.133 Uiso 1 1 calc R . . H50B H 0.2398 -0.0502 -0.4155 0.133 Uiso 1 1 calc R . . C51 C 0.1814(6) 0.0103(7) -0.3656(7) 0.106(4) Uani 1 1 d . . . H51A H 0.1863 0.0652 -0.3358 0.127 Uiso 1 1 calc R . . H51B H 0.1369 -0.0022 -0.4200 0.127 Uiso 1 1 calc R . . C52 C 0.4918(6) 0.0235(10) -0.2053(10) 0.143(6) Uani 1 1 d . . . H52A H 0.5391 0.0588 -0.1663 0.172 Uiso 1 1 calc R . . H52B H 0.5029 -0.0260 -0.2293 0.172 Uiso 1 1 calc R . . C53 C 0.4539(6) 0.0561(6) -0.2734(6) 0.094(3) Uani 1 1 d . . . H53A H 0.4583 0.1119 -0.2471 0.113 Uiso 1 1 calc R . . H53B H 0.4826 0.0526 -0.3042 0.113 Uiso 1 1 calc R . . C54 C 0.3775(7) 0.0278(9) -0.3359(7) 0.113(4) Uani 1 1 d . . . H54A H 0.3658 0.0589 -0.3749 0.135 Uiso 1 1 calc R . . H54B H 0.3738 -0.0259 -0.3682 0.135 Uiso 1 1 calc R . . C55 C 0.1678(5) -0.0350(10) -0.3190(7) 0.119(4) Uani 1 1 d . . . H55A H 0.1576 -0.0903 -0.3509 0.143 Uiso 1 1 calc R . . H55B H 0.1232 -0.0233 -0.3150 0.143 Uiso 1 1 calc R . . C56 C -0.0515(5) 0.2316(8) -0.4669(5) 0.098(3) Uani 1 1 d . . . H56A H -0.0596 0.2735 -0.4281 0.118 Uiso 1 1 calc R . . H56B H -0.0918 0.2235 -0.5235 0.118 Uiso 1 1 calc R . . C57 C 0.6510(6) 0.4775(6) 0.5621(6) 0.093(3) Uani 1 1 d . . . H57A H 0.6845 0.5257 0.5762 0.112 Uiso 1 1 calc R . . H57B H 0.6204 0.4903 0.5902 0.112 Uiso 1 1 calc R . . C58 C 0.7382(7) 0.3855(10) 0.5672(7) 0.143(6) Uani 1 1 d . . . H58A H 0.7659 0.3582 0.6074 0.171 Uiso 1 1 calc R . . H58B H 0.7743 0.4255 0.5701 0.171 Uiso 1 1 calc R . . C59 C 0.7635(6) 0.3106(7) 0.4560(8) 0.105(4) Uani 1 1 d . . . H59A H 0.7462 0.2599 0.4124 0.126 Uiso 1 1 calc R . . H59B H 0.8075 0.3067 0.5047 0.126 Uiso 1 1 calc R . . C60 C 0.7285(7) 0.3771(8) 0.3397(8) 0.114(4) Uani 1 1 d . . . H60A H 0.7124 0.3251 0.2983 0.137 Uiso 1 1 calc R . . H60B H 0.7516 0.4118 0.3209 0.137 Uiso 1 1 calc R . . C61 C 0.0717(8) 0.3932(8) 0.2998(6) 0.129(5) Uani 1 1 d . . . H61A H 0.0471 0.3583 0.3170 0.155 Uiso 1 1 calc R . . H61B H 0.1238 0.4074 0.3422 0.155 Uiso 1 1 calc R . . C62 C 0.0847(5) 0.2690(6) 0.2207(6) 0.089(3) Uani 1 1 d . . . H62A H 0.1245 0.2727 0.2764 0.107 Uiso 1 1 calc R . . H62B H 0.1024 0.2499 0.1794 0.107 Uiso 1 1 calc R . . C63 C 0.1919(7) -0.1154(6) 0.2900(7) 0.097(3) Uani 1 1 d . . . H63A H 0.2340 -0.1316 0.2825 0.117 Uiso 1 1 calc R . . H63B H 0.1922 -0.1317 0.3367 0.117 Uiso 1 1 calc R . . C64 C 0.4397(7) 0.7482(6) 0.3856(6) 0.096(3) Uani 1 1 d . . . H64A H 0.4266 0.6935 0.3811 0.115 Uiso 1 1 calc R . . H64B H 0.4531 0.7798 0.4431 0.115 Uiso 1 1 calc R . . C70 C 0.0106(11) 0.3217(10) -0.5047(9) 0.190(10) Uani 1 1 d . . . H70A H -0.0001 0.2965 -0.5630 0.228 Uiso 1 1 calc R . . H70B H -0.0353 0.3376 -0.5077 0.228 Uiso 1 1 calc R . . C71 C 0.0533(12) 0.3824(12) -0.4818(12) 0.221(12) Uani 1 1 d . . . H71A H 0.0198 0.4195 -0.4951 0.265 Uiso 1 1 calc R . . H71B H 0.0700 0.3734 -0.5248 0.265 Uiso 1 1 calc R . . C72 C 0.6944(11) 0.4235(9) 0.5959(7) 0.170(8) Uani 1 1 d . . . H72A H 0.7266 0.4514 0.6555 0.204 Uiso 1 1 calc R . . H72B H 0.6599 0.3826 0.5943 0.204 Uiso 1 1 calc R . . C73 C 0.7844(6) 0.3724(9) 0.4227(9) 0.126(5) Uani 1 1 d . . . H73A H 0.7963 0.4235 0.4645 0.151 Uiso 1 1 calc R . . H73B H 0.8295 0.3630 0.4187 0.151 Uiso 1 1 calc R . . Cl1 Cl 0.72791(11) 0.64289(12) 0.49269(11) 0.0649(4) Uani 1 1 d . . . O11A O 0.7607(10) 0.6767(8) 0.5789(6) 0.223(7) Uani 1 1 d D . . O12A O 0.6521(5) 0.6261(8) 0.4601(10) 0.211(7) Uani 1 1 d D . . O13A O 0.7581(9) 0.5791(6) 0.4845(14) 0.251(9) Uani 1 1 d D . . O14A O 0.7480(5) 0.7019(6) 0.4666(7) 0.141(3) Uani 1 1 d D . . Cl2 Cl 0.06189(12) 0.07181(15) 0.39214(14) 0.0848(6) Uani 1 1 d . . . O21A O 0.0275(6) 0.0707(8) 0.4399(6) 0.168(5) Uani 1 1 d D . . O22A O 0.1034(7) 0.1472(6) 0.4081(7) 0.174(5) Uani 1 1 d D . . O23A O 0.0187(5) 0.0320(6) 0.3057(5) 0.135(3) Uani 1 1 d D . . O24A O 0.1229(5) 0.0285(8) 0.4253(7) 0.157(4) Uani 1 1 d D . . Cl3 Cl 0.1812(2) 0.7727(2) 0.7710(3) 0.1374(14) Uani 1 1 d . . . O31A O 0.1899(7) 0.7864(6) 0.7043(8) 0.166(5) Uani 1 1 d D . . O32A O 0.1340(8) 0.7066(7) 0.7466(9) 0.197(6) Uani 1 1 d D . . O33A O 0.1707(8) 0.8381(7) 0.8222(9) 0.194(6) Uani 1 1 d D . . O34A O 0.2558(10) 0.7653(12) 0.8220(11) 0.263(9) Uani 1 1 d D . . Cl4 Cl 0.6643(4) 0.4420(3) 0.1459(3) 0.198(3) Uani 1 1 d . . . O41A O 0.6142(9) 0.4390(11) 0.0676(7) 0.222(7) Uani 1 1 d D . . O42A O 0.662(3) 0.4927(17) 0.2157(14) 0.48(3) Uani 1 1 d D . . O43A O 0.6729(18) 0.3681(12) 0.143(2) 0.56(3) Uani 1 1 d D . . O44A O 0.7633(10) 0.4751(10) 0.1695(8) 0.223(8) Uani 1 1 d D . . O1W O 0.0542(3) 0.6167(3) 0.1368(4) 0.0744(14) Uani 1 1 d . . . O2W O 0.4612(3) -0.1304(3) -0.0415(3) 0.0660(12) Uani 1 1 d . . . O3W O 0.2998(3) 0.2099(3) -0.2297(3) 0.0726(14) Uani 1 1 d . . . O4W O 0.4682(3) 0.5078(3) 0.3221(3) 0.0793(16) Uani 1 1 d . . . O5W O 0.4821(4) 0.1349(4) 0.3662(3) 0.0909(19) Uani 1 1 d . . . O6W O -0.0287(3) -0.0843(5) 0.0111(4) 0.0913(19) Uani 1 1 d . . . O7W O 0.4771(4) 0.3874(4) 0.5093(5) 0.103(2) Uani 1 1 d . . . O8W O 0.3336(5) 0.8689(4) 0.1797(6) 0.119(3) Uani 1 1 d . . . O9W O 0.2672(5) -0.0963(5) 0.0265(5) 0.119(3) Uani 1 1 d . . . O10W O 0.5834(6) 0.2516(5) -0.0075(6) 0.134(3) Uani 1 1 d . . . O11W O 0.2075(6) 0.6080(7) 0.2129(8) 0.163(4) Uani 1 1 d . . . O12W O 0.2384(7) 0.7129(10) -0.0417(11) 0.238(8) Uani 1 1 d . . . O13W O 0.1818(3) 0.2158(3) -0.3890(3) 0.0705(13) Uani 1 1 d . . . O14W O 0.4308(3) 0.7692(3) 0.1649(3) 0.0626(12) Uani 1 1 d . . . O15W O -0.1050(3) 0.3582(3) -0.0162(3) 0.0638(12) Uani 1 1 d . . . O16W O 0.5518(3) 0.2842(3) 0.4372(3) 0.0756(14) Uani 1 1 d . . . O17W O 0.3272(2) -0.1280(2) -0.2652(3) 0.0581(11) Uani 1 1 d . . . O18W O 0.0677(3) 0.0197(4) 0.1782(4) 0.0738(14) Uani 1 1 d . . . O19W O 0.5000 0.0000 0.5000 0.0342(10) Uani 1 2 d S . . 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 0.0321(3) 0.0331(3) 0.0264(3) 0.0086(2) 0.0119(2) 0.0094(2) Ni2 0.0357(3) 0.0310(3) 0.0336(3) 0.0095(2) 0.0107(3) 0.0089(2) Ni3 0.0381(3) 0.0386(3) 0.0286(3) 0.0045(2) 0.0136(3) 0.0088(3) Ni4 0.0383(3) 0.0499(4) 0.0393(3) 0.0166(3) 0.0174(3) 0.0070(3) Ni5 0.0488(4) 0.0354(3) 0.0431(4) 0.0097(3) 0.0154(3) 0.0008(3) Ni6 0.0466(4) 0.0536(4) 0.0332(3) 0.0134(3) 0.0142(3) 0.0143(3) Ni7 0.0382(4) 0.0436(4) 0.0425(4) 0.0032(3) 0.0073(3) 0.0027(3) Ni8 0.0455(4) 0.0486(4) 0.0459(4) 0.0120(3) 0.0231(3) 0.0175(3) O1 0.045(2) 0.039(2) 0.056(2) 0.0121(17) 0.0236(19) 0.0162(16) O2 0.059(2) 0.046(2) 0.056(2) 0.0074(18) 0.032(2) 0.0181(19) O3 0.047(2) 0.044(2) 0.051(2) 0.0077(17) 0.0288(18) 0.0100(17) O4 0.0369(18) 0.045(2) 0.0346(17) 0.0127(15) 0.0114(15) 0.0133(15) O5 0.046(2) 0.059(2) 0.0358(19) 0.0154(17) 0.0138(17) 0.0187(18) O6 0.043(2) 0.073(3) 0.0353(19) 0.0153(19) 0.0144(17) 0.021(2) O7 0.053(2) 0.0358(19) 0.042(2) 0.0101(16) 0.0055(17) -0.0019(17) O8 0.047(2) 0.0348(19) 0.052(2) 0.0169(17) 0.0068(18) 0.0037(16) O9 0.056(2) 0.041(2) 0.061(3) 0.024(2) 0.006(2) -0.0008(18) O10 0.048(2) 0.0354(17) 0.0322(17) 0.0100(14) 0.0182(15) 0.0116(15) O11 0.057(2) 0.0323(17) 0.0379(18) 0.0068(14) 0.0236(17) 0.0126(16) O12 0.053(2) 0.0368(18) 0.0276(16) 0.0084(14) 0.0169(15) 0.0146(16) O13 0.0360(18) 0.067(3) 0.044(2) 0.0296(19) 0.0165(16) 0.0121(17) O14 0.0397(19) 0.050(2) 0.045(2) 0.0252(17) 0.0216(16) 0.0133(16) O15 0.0356(17) 0.0461(19) 0.0340(17) 0.0197(15) 0.0153(14) 0.0127(15) O16 0.0346(17) 0.0372(18) 0.0357(17) 0.0077(14) 0.0150(14) 0.0096(14) O17 0.0331(18) 0.048(2) 0.054(2) 0.0062(18) 0.0138(17) 0.0111(16) O18 0.040(2) 0.043(2) 0.043(2) -0.0061(16) 0.0043(16) 0.0104(16) N1 0.034(2) 0.0304(19) 0.034(2) 0.0088(16) 0.0118(16) 0.0090(16) N2 0.037(2) 0.0303(19) 0.034(2) 0.0085(16) 0.0115(17) 0.0090(16) N3 0.036(2) 0.032(2) 0.034(2) 0.0112(16) 0.0135(17) 0.0081(16) N4 0.0294(18) 0.035(2) 0.0287(18) 0.0108(15) 0.0109(15) 0.0086(15) N5 0.0337(19) 0.0333(19) 0.0273(17) 0.0092(15) 0.0129(15) 0.0089(15) N6 0.0344(19) 0.035(2) 0.0258(17) 0.0062(15) 0.0109(15) 0.0111(16) N10 0.070(4) 0.054(3) 0.081(4) 0.020(3) 0.030(3) 0.008(3) N11 0.079(4) 0.072(4) 0.058(3) 0.021(3) 0.034(3) 0.000(3) N12 0.069(4) 0.092(5) 0.035(3) 0.022(3) 0.003(3) 0.011(3) N14 0.034(2) 0.086(4) 0.058(3) 0.003(3) 0.013(2) 0.013(3) N15 0.039(2) 0.057(3) 0.054(3) 0.016(2) 0.022(2) 0.007(2) N17 0.075(4) 0.088(4) 0.031(2) 0.016(3) 0.011(3) -0.011(3) N19 0.058(3) 0.069(3) 0.045(3) 0.026(3) 0.020(2) 0.005(3) N24 0.081(4) 0.049(3) 0.043(3) -0.006(2) 0.016(3) 0.002(3) N27 0.071(4) 0.080(4) 0.059(3) 0.010(3) 0.032(3) 0.022(3) N18 0.066(4) 0.058(3) 0.060(3) 0.011(3) 0.028(3) 0.020(3) N20 0.063(3) 0.053(3) 0.056(3) 0.002(2) 0.021(3) -0.005(3) N21 0.111(6) 0.072(4) 0.101(6) 0.000(4) 0.072(5) -0.012(4) N23 0.054(4) 0.110(6) 0.068(4) 0.013(4) -0.001(3) 0.018(4) N26 0.059(3) 0.061(3) 0.092(5) 0.030(3) 0.041(3) 0.014(3) N50 0.081(4) 0.058(3) 0.087(5) 0.014(3) 0.054(4) 0.011(3) N51 0.065(3) 0.053(3) 0.043(3) 0.011(2) 0.006(2) -0.004(3) N53 0.061(3) 0.068(4) 0.051(3) 0.020(3) 0.018(3) 0.023(3) N54 0.081(4) 0.068(4) 0.068(4) 0.013(3) 0.046(3) 0.035(3) C1 0.035(2) 0.041(3) 0.030(2) 0.0074(19) 0.0115(19) 0.0115(19) C2 0.036(2) 0.044(3) 0.041(3) 0.007(2) 0.014(2) 0.013(2) C3 0.040(2) 0.038(2) 0.034(2) 0.015(2) 0.013(2) 0.012(2) C4 0.038(2) 0.036(2) 0.038(2) 0.014(2) 0.013(2) 0.0066(19) C5 0.040(3) 0.033(2) 0.037(2) 0.0075(19) 0.013(2) 0.0079(19) C6 0.041(3) 0.034(3) 0.045(3) 0.011(2) 0.009(2) 0.009(2) C7 0.033(2) 0.038(2) 0.032(2) 0.0099(19) 0.0118(19) 0.0109(19) C8 0.036(2) 0.035(2) 0.028(2) 0.0098(18) 0.0135(18) 0.0118(18) C9 0.035(2) 0.034(2) 0.029(2) 0.0102(18) 0.0139(18) 0.0112(18) C10 0.034(2) 0.035(2) 0.031(2) 0.0093(18) 0.0123(18) 0.0128(18) C11 0.037(2) 0.038(2) 0.027(2) 0.0079(18) 0.0095(18) 0.0104(19) C12 0.035(2) 0.037(2) 0.032(2) 0.0128(19) 0.0145(19) 0.0108(19) C13 0.030(2) 0.032(2) 0.033(2) 0.0094(18) 0.0141(18) 0.0076(17) C14 0.031(2) 0.035(2) 0.028(2) 0.0084(17) 0.0116(17) 0.0099(17) C15 0.029(2) 0.033(2) 0.031(2) 0.0099(17) 0.0120(17) 0.0065(17) C16 0.039(2) 0.034(2) 0.033(2) 0.0065(19) 0.014(2) 0.0082(19) C17 0.042(3) 0.040(3) 0.024(2) -0.0004(18) 0.0081(19) 0.005(2) C18 0.034(2) 0.039(2) 0.030(2) 0.0082(19) 0.0070(18) 0.0059(19) C19 0.036(2) 0.032(2) 0.0247(19) 0.0063(16) 0.0126(17) 0.0084(17) C20 0.031(2) 0.030(2) 0.032(2) 0.0065(17) 0.0111(18) 0.0058(17) C21 0.038(2) 0.035(2) 0.030(2) 0.0098(18) 0.0136(19) 0.0097(19) C22 0.043(3) 0.032(2) 0.046(3) 0.013(2) 0.019(2) 0.005(2) C23 0.032(2) 0.041(3) 0.043(3) 0.009(2) 0.014(2) 0.009(2) C24 0.034(2) 0.030(2) 0.029(2) 0.0044(17) 0.0093(18) 0.0060(17) C25 0.036(2) 0.034(2) 0.029(2) 0.0059(18) 0.0132(18) 0.0067(18) C26 0.032(2) 0.033(2) 0.0252(19) 0.0042(17) 0.0078(17) 0.0084(17) C27 0.036(3) 0.042(3) 0.053(3) 0.016(2) 0.020(2) 0.003(2) C28 0.040(3) 0.044(3) 0.035(2) 0.003(2) 0.015(2) 0.013(2) C29 0.047(3) 0.051(3) 0.032(2) 0.012(2) 0.022(2) 0.017(2) C30 0.044(3) 0.043(3) 0.033(2) 0.014(2) 0.016(2) 0.012(2) C31 0.077(5) 0.065(4) 0.055(4) -0.009(3) 0.028(4) 0.003(4) C32 0.067(5) 0.102(6) 0.042(3) 0.005(4) 0.019(3) 0.003(4) C33 0.066(4) 0.093(6) 0.049(4) 0.034(4) 0.022(3) 0.016(4) C34 0.085(6) 0.054(4) 0.080(6) 0.006(4) 0.014(5) -0.012(4) C35 0.092(7) 0.077(6) 0.127(9) 0.044(6) 0.040(6) -0.014(5) C36 0.081(6) 0.067(5) 0.090(6) 0.017(4) 0.039(5) 0.015(4) C37 0.118(8) 0.095(7) 0.094(7) 0.056(6) 0.043(6) 0.039(6) C40 0.101(7) 0.147(10) 0.112(8) 0.068(8) 0.067(7) 0.062(7) C41 0.063(5) 0.140(10) 0.111(8) 0.072(7) 0.039(5) 0.038(6) C42 0.048(4) 0.082(5) 0.087(6) 0.038(5) 0.003(4) -0.001(4) C43 0.113(7) 0.071(5) 0.048(4) 0.000(4) 0.010(4) -0.011(5) C44 0.142(10) 0.071(6) 0.104(7) 0.023(5) 0.080(8) 0.028(6) C45 0.148(10) 0.083(6) 0.078(6) 0.024(5) 0.066(7) 0.064(6) C46 0.114(8) 0.086(6) 0.060(5) -0.004(4) 0.028(5) 0.017(6) C47 0.077(5) 0.080(6) 0.079(5) 0.005(4) 0.037(5) -0.011(4) C48 0.066(5) 0.112(8) 0.070(5) -0.005(5) 0.019(4) -0.012(5) C49 0.125(9) 0.082(6) 0.108(8) 0.051(6) 0.069(7) 0.031(6) C50 0.118(9) 0.156(10) 0.041(4) 0.028(5) 0.018(5) 0.067(8) C51 0.066(6) 0.122(9) 0.086(7) 0.039(6) -0.007(5) 0.011(6) C52 0.079(6) 0.229(15) 0.228(15) 0.184(14) 0.097(9) 0.072(8) C53 0.108(7) 0.105(7) 0.071(5) 0.015(5) 0.055(5) -0.026(6) C54 0.118(9) 0.181(12) 0.092(7) 0.075(8) 0.074(7) 0.064(9) C55 0.054(5) 0.201(14) 0.082(7) 0.039(8) 0.016(5) 0.036(7) C56 0.052(4) 0.149(10) 0.051(4) 0.004(5) 0.001(3) 0.024(5) C57 0.095(7) 0.095(7) 0.060(5) -0.009(5) 0.030(5) -0.003(5) C58 0.089(7) 0.192(14) 0.064(6) -0.014(7) -0.011(5) 0.052(9) C59 0.064(5) 0.109(8) 0.110(8) 0.007(6) 0.026(5) 0.022(5) C60 0.099(8) 0.122(9) 0.118(9) -0.004(7) 0.071(8) -0.006(7) C61 0.148(11) 0.132(10) 0.058(5) 0.012(6) 0.009(6) 0.074(9) C62 0.082(6) 0.090(6) 0.080(6) 0.034(5) 0.018(5) 0.039(5) C63 0.116(8) 0.080(6) 0.093(7) 0.049(5) 0.034(6) 0.012(6) C64 0.150(10) 0.081(6) 0.060(5) 0.016(4) 0.057(6) 0.015(6) C70 0.218(18) 0.131(11) 0.101(9) 0.081(9) -0.050(10) -0.014(12) C71 0.212(19) 0.166(16) 0.172(16) 0.134(14) -0.046(14) -0.022(15) C72 0.212(17) 0.135(11) 0.052(6) -0.016(6) -0.013(8) 0.059(12) C73 0.059(5) 0.159(12) 0.114(9) -0.021(8) 0.038(6) -0.007(6) Cl1 0.0679(10) 0.0717(11) 0.0558(9) 0.0166(8) 0.0312(8) 0.0104(8) O11A 0.37(2) 0.202(12) 0.081(6) 0.040(7) 0.087(10) 0.097(13) O12A 0.072(5) 0.254(13) 0.356(18) 0.227(14) 0.072(8) 0.028(7) O13A 0.240(16) 0.103(8) 0.47(3) 0.034(12) 0.241(19) 0.054(9) O14A 0.129(7) 0.167(9) 0.179(9) 0.096(8) 0.095(7) 0.016(6) Cl2 0.0684(11) 0.0990(15) 0.0669(11) -0.0104(10) 0.0353(10) -0.0049(11) O21A 0.127(7) 0.263(14) 0.109(7) 0.009(7) 0.080(6) 0.005(8) O22A 0.183(11) 0.110(7) 0.151(9) -0.001(6) 0.038(8) -0.016(7) O23A 0.149(8) 0.143(7) 0.076(4) -0.022(4) 0.054(5) -0.022(6) O24A 0.112(7) 0.241(12) 0.166(9) 0.105(9) 0.080(7) 0.083(8) Cl3 0.148(3) 0.128(3) 0.154(3) -0.003(2) 0.115(3) -0.020(2) O31A 0.215(12) 0.150(9) 0.176(10) 0.024(7) 0.147(10) -0.008(8) O32A 0.222(13) 0.143(9) 0.239(14) 0.014(9) 0.154(12) -0.061(9) O33A 0.230(13) 0.155(9) 0.215(12) -0.031(9) 0.173(12) -0.027(9) O34A 0.207(16) 0.29(2) 0.178(14) 0.040(13) 0.008(12) 0.084(15) Cl4 0.319(8) 0.142(4) 0.114(3) 0.037(3) 0.090(4) 0.020(4) O41A 0.199(13) 0.32(2) 0.092(7) 0.058(10) 0.021(8) 0.024(13) O42A 0.88(8) 0.32(3) 0.200(19) -0.035(18) 0.29(4) -0.04(4) O43A 0.78(7) 0.157(17) 0.52(5) 0.18(2) 0.08(5) 0.10(3) O44A 0.266(17) 0.227(15) 0.122(9) 0.015(9) 0.079(10) -0.098(13) O1W 0.064(3) 0.062(3) 0.093(4) 0.025(3) 0.033(3) 0.016(2) O2W 0.065(3) 0.076(3) 0.064(3) 0.028(2) 0.030(2) 0.027(2) O3W 0.092(4) 0.082(3) 0.054(3) 0.024(3) 0.037(3) 0.041(3) O4W 0.083(4) 0.058(3) 0.061(3) 0.010(2) 0.008(3) 0.007(3) O5W 0.106(5) 0.075(4) 0.052(3) 0.014(3) 0.009(3) -0.017(3) O6W 0.053(3) 0.152(6) 0.072(4) 0.047(4) 0.025(3) 0.011(3) O7W 0.093(5) 0.102(5) 0.109(5) 0.019(4) 0.049(4) 0.026(4) O8W 0.152(7) 0.079(4) 0.206(9) 0.075(5) 0.131(7) 0.060(5) O9W 0.123(6) 0.097(5) 0.117(6) 0.012(4) 0.054(5) -0.018(4) O10W 0.207(10) 0.128(7) 0.129(7) 0.062(6) 0.118(7) 0.039(6) O11W 0.107(7) 0.184(10) 0.185(10) 0.068(9) 0.051(7) 0.019(7) O12W 0.146(9) 0.318(18) 0.36(2) 0.277(18) 0.115(12) 0.124(11) O13W 0.071(3) 0.082(4) 0.058(3) 0.012(2) 0.033(3) 0.025(3) O14W 0.063(3) 0.045(2) 0.075(3) 0.024(2) 0.026(2) 0.002(2) O15W 0.060(3) 0.060(3) 0.056(3) 0.012(2) 0.015(2) 0.022(2) O16W 0.096(4) 0.066(3) 0.061(3) 0.014(2) 0.037(3) 0.000(3) O17W 0.054(2) 0.043(2) 0.070(3) -0.004(2) 0.033(2) 0.0054(18) O18W 0.049(3) 0.103(4) 0.075(3) 0.028(3) 0.033(2) 0.018(3) O19W 0.053(3) 0.031(2) 0.028(2) 0.0201(18) 0.018(2) 0.030(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 N5 2.073(4) . ? Ni1 N6 2.083(4) . ? Ni1 O15 2.086(3) . ? Ni1 O10 2.097(3) . ? Ni1 N4 2.102(4) . ? Ni1 O16 2.139(3) . ? Ni2 N3 2.058(4) . ? Ni2 N1 2.074(4) . ? Ni2 N2 2.076(4) . ? Ni2 O1 2.081(4) . ? Ni2 O8 2.093(4) . ? Ni2 O4 2.110(4) . ? Ni3 N15 2.081(5) . ? Ni3 O11 2.093(4) . ? Ni3 O12 2.100(3) . ? Ni3 N17 2.106(5) . ? Ni3 N14 2.104(5) . ? Ni3 O17W 2.126(4) . ? Ni4 O14 2.073(4) . ? Ni4 N20 2.085(6) . ? Ni4 N19 2.100(5) . ? Ni4 O13 2.106(4) . ? Ni4 N18 2.105(6) . ? Ni4 O18W 2.146(5) . ? Ni5 O14W 2.085(4) . ? Ni5 N51 2.103(5) . ? Ni5 N50 2.106(6) . ? Ni5 N27 2.105(6) . ? Ni5 O9 2.107(4) . ? Ni5 O7 2.109(4) . ? Ni6 O6 2.071(4) . ? Ni6 O5 2.081(4) . ? Ni6 N11 2.088(6) . ? Ni6 N10 2.098(6) . ? Ni6 N12 2.099(5) . ? Ni6 O13W 2.177(5) . ? Ni7 N21 2.025(7) . ? Ni7 O18 2.045(4) . ? Ni7 N24 2.096(6) . ? Ni7 N23 2.099(7) . ? Ni7 O17 2.144(4) . ? Ni7 O16W 2.160(5) . ? Ni8 N26 2.052(6) . ? Ni8 N54 2.083(5) . ? Ni8 O3 2.088(4) . ? Ni8 O2 2.089(5) . ? Ni8 N53 2.098(6) . ? Ni8 O15W 2.180(5) . ? O1 C2 1.232(6) . ? O2 C2 1.264(5) . ? O3 C1 1.275(5) . ? O4 C4 1.244(5) . ? O5 C4 1.259(5) . ? O6 C3 1.280(5) . ? O7 C5 1.284(5) . ? O8 C6 1.254(5) . ? O9 C6 1.243(6) . ? O10 C10 1.261(5) . ? O11 C10 1.256(5) . ? O12 C9 1.276(5) . ? O13 C7 1.279(5) . ? O14 C8 1.249(5) . ? O15 C8 1.258(5) . ? O16 C12 1.249(5) . ? O17 C12 1.256(5) . ? O18 C11 1.282(5) . ? N1 C1 1.298(5) . ? N1 C13 1.423(4) . ? N2 C5 1.283(5) . ? N2 C24 1.426(5) . ? N3 C3 1.284(5) . ? N3 C21 1.418(5) . ? N4 C7 1.291(5) . ? N4 C15 1.427(4) . ? N5 C9 1.293(5) . ? N5 C19 1.416(5) . ? N6 C11 1.288(5) . ? N6 C26 1.425(4) . ? N10 C47 1.505(9) . ? N11 C49 1.481(10) . ? N12 C70 1.461(13) . ? N12 C56 1.504(11) . ? N14 C55 1.472(10) . ? N15 C52 1.447(10) . ? N17 C54 1.389(10) . ? N17 C50 1.474(11) . ? N19 C33 1.470(8) . ? N19 C63 1.497(10) . ? N24 C57 1.481(9) . ? N27 C40 1.417(11) . ? N18 C31 1.478(8) . ? N20 C34 1.480(9) . ? N21 C60 1.527(11) . ? N23 C59 1.468(11) . ? N23 C58 1.480(11) . ? N26 C36 1.501(9) . ? N50 C44 1.471(10) . ? N51 C42 1.513(9) . ? N51 C43 1.514(9) . ? N53 C62 1.461(9) . ? N53 C61 1.464(11) . ? N54 C45 1.389(9) . ? C1 C2 1.538(7) . ? C3 C4 1.544(7) . ? C5 C6 1.545(7) . ? C7 C8 1.533(6) . ? C9 C10 1.533(7) . ? C11 C12 1.541(6) . ? C13 C14 1.391(6) . ? C13 C18 1.409(7) . ? C14 C15 1.392(6) . ? C15 C16 1.399(7) . ? C16 C17 1.387(7) . ? C17 C18 1.391(7) . ? C19 C23 1.387(7) . ? C19 C20 1.397(6) . ? C20 C21 1.392(7) . ? C21 C22 1.389(7) . ? C22 C27 1.387(8) . ? C23 C27 1.395(8) . ? C24 C28 1.390(7) . ? C24 C25 1.399(6) . ? C25 C26 1.382(7) . ? C26 C30 1.383(7) . ? C28 C29 1.388(8) . ? C29 C30 1.393(7) . ? C31 C32 1.502(13) . ? C32 C33 1.486(12) . ? C34 C35 1.542(15) . ? C35 C63 1.445(15) . ? C36 C37 1.499(14) . ? C37 C62 1.504(15) . ? C40 C41 1.478(15) . ? C41 C42 1.474(15) . ? C43 C64 1.481(16) . ? C44 C64 1.494(15) . ? C45 C46 1.476(15) . ? C46 C61 1.462(14) . ? C47 C48 1.501(14) . ? C48 C56 1.472(16) . ? C49 C71 1.49(2) . ? C50 C51 1.481(16) . ? C51 C55 1.409(17) . ? C52 C53 1.435(15) . ? C53 C54 1.432(16) . ? C57 C72 1.413(17) . ? C58 C72 1.35(2) . ? C59 C73 1.512(19) . ? C60 C73 1.476(19) . ? C70 C71 1.21(2) . ? Cl1 O13A 1.327(10) . ? Cl1 O11A 1.368(10) . ? Cl1 O12A 1.369(8) . ? Cl1 O14A 1.372(8) . ? Cl2 O21A 1.342(8) . ? Cl2 O23A 1.395(8) . ? Cl2 O22A 1.440(11) . ? Cl2 O24A 1.475(9) . ? Cl3 O32A 1.323(10) . ? Cl3 O31A 1.388(10) . ? Cl3 O33A 1.394(11) . ? Cl3 O34A 1.425(15) . ? Cl4 O43A 1.328(19) . ? Cl4 O41A 1.334(12) . ? Cl4 O42A 1.39(2) . ? Cl4 O44A 1.888(18) . ? 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 N5 Ni1 N6 99.64(16) . . ? N5 Ni1 O15 165.82(15) . . ? N6 Ni1 O15 94.53(15) . . ? N5 Ni1 O10 79.40(14) . . ? N6 Ni1 O10 167.62(15) . . ? O15 Ni1 O10 86.67(14) . . ? N5 Ni1 N4 99.33(15) . . ? N6 Ni1 N4 98.77(15) . . ? O15 Ni1 N4 78.78(14) . . ? O10 Ni1 N4 93.56(15) . . ? N5 Ni1 O16 93.26(15) . . ? N6 Ni1 O16 78.36(14) . . ? O15 Ni1 O16 89.16(13) . . ? O10 Ni1 O16 89.35(14) . . ? N4 Ni1 O16 167.40(14) . . ? N3 Ni2 N1 99.95(16) . . ? N3 Ni2 N2 98.07(16) . . ? N1 Ni2 N2 99.11(16) . . ? N3 Ni2 O1 172.83(16) . . ? N1 Ni2 O1 79.92(16) . . ? N2 Ni2 O1 89.01(16) . . ? N3 Ni2 O8 93.16(17) . . ? N1 Ni2 O8 166.89(17) . . ? N2 Ni2 O8 79.23(16) . . ? O1 Ni2 O8 87.04(17) . . ? N3 Ni2 O4 79.21(15) . . ? N1 Ni2 O4 91.26(15) . . ? N2 Ni2 O4 169.60(16) . . ? O1 Ni2 O4 93.63(15) . . ? O8 Ni2 O4 90.85(15) . . ? N15 Ni3 O11 87.02(18) . . ? N15 Ni3 O12 90.51(18) . . ? O11 Ni3 O12 79.68(13) . . ? N15 Ni3 N17 94.9(2) . . ? O11 Ni3 N17 174.7(2) . . ? O12 Ni3 N17 95.3(2) . . ? N15 Ni3 N14 171.5(2) . . ? O11 Ni3 N14 84.5(2) . . ? O12 Ni3 N14 87.3(2) . . ? N17 Ni3 N14 93.5(3) . . ? N15 Ni3 O17W 91.83(15) . . ? O11 Ni3 O17W 91.39(14) . . ? O12 Ni3 O17W 170.64(13) . . ? N17 Ni3 O17W 93.5(2) . . ? N14 Ni3 O17W 89.05(18) . . ? O14 Ni4 N20 91.0(2) . . ? O14 Ni4 N19 94.68(19) . . ? N20 Ni4 N19 97.1(2) . . ? O14 Ni4 O13 79.72(14) . . ? N20 Ni4 O13 85.8(2) . . ? N19 Ni4 O13 173.73(19) . . ? O14 Ni4 N18 89.9(2) . . ? N20 Ni4 N18 175.7(2) . . ? N19 Ni4 N18 87.0(2) . . ? O13 Ni4 N18 90.2(2) . . ? O14 Ni4 O18W 170.87(15) . . ? N20 Ni4 O18W 87.50(18) . . ? N19 Ni4 O18W 94.44(16) . . ? O13 Ni4 O18W 91.19(15) . . ? N18 Ni4 O18W 91.00(17) . . ? O14W Ni5 N51 93.77(16) . . ? O14W Ni5 N50 88.81(18) . . ? N51 Ni5 N50 96.2(3) . . ? O14W Ni5 N27 92.6(2) . . ? N51 Ni5 N27 91.0(3) . . ? N50 Ni5 N27 172.5(3) . . ? O14W Ni5 O9 90.54(14) . . ? N51 Ni5 O9 175.37(19) . . ? N50 Ni5 O9 85.6(3) . . ? N27 Ni5 O9 87.1(2) . . ? O14W Ni5 O7 169.83(14) . . ? N51 Ni5 O7 96.34(19) . . ? N50 Ni5 O7 89.0(2) . . ? N27 Ni5 O7 88.3(2) . . ? O9 Ni5 O7 79.39(15) . . ? O6 Ni6 O5 80.64(15) . . ? O6 Ni6 N11 88.2(2) . . ? O5 Ni6 N11 93.5(2) . . ? O6 Ni6 N10 87.8(2) . . ? O5 Ni6 N10 91.2(2) . . ? N11 Ni6 N10 173.3(3) . . ? O6 Ni6 N12 175.6(2) . . ? O5 Ni6 N12 96.1(2) . . ? N11 Ni6 N12 95.0(3) . . ? N10 Ni6 N12 89.3(3) . . ? O6 Ni6 O13W 87.50(14) . . ? O5 Ni6 O13W 167.61(14) . . ? N11 Ni6 O13W 89.72(19) . . ? N10 Ni6 O13W 84.76(19) . . ? N12 Ni6 O13W 95.5(2) . . ? N21 Ni7 O18 95.3(3) . . ? N21 Ni7 N24 93.9(3) . . ? O18 Ni7 N24 88.5(2) . . ? N21 Ni7 N23 95.2(4) . . ? O18 Ni7 N23 168.6(3) . . ? N24 Ni7 N23 95.2(3) . . ? N21 Ni7 O17 91.9(2) . . ? O18 Ni7 O17 79.63(15) . . ? N24 Ni7 O17 167.2(2) . . ? N23 Ni7 O17 95.6(3) . . ? N21 Ni7 O16W 179.6(3) . . ? O18 Ni7 O16W 84.95(17) . . ? N24 Ni7 O16W 86.33(19) . . ? N23 Ni7 O16W 84.5(3) . . ? O17 Ni7 O16W 87.91(14) . . ? N26 Ni8 N54 95.7(3) . . ? N26 Ni8 O3 94.8(2) . . ? N54 Ni8 O3 168.3(2) . . ? N26 Ni8 O2 172.4(2) . . ? N54 Ni8 O2 89.3(2) . . ? O3 Ni8 O2 79.81(15) . . ? N26 Ni8 N53 93.2(3) . . ? N54 Ni8 N53 96.5(2) . . ? O3 Ni8 N53 88.2(2) . . ? O2 Ni8 N53 91.9(2) . . ? N26 Ni8 O15W 89.2(2) . . ? N54 Ni8 O15W 86.49(19) . . ? O3 Ni8 O15W 88.41(13) . . ? O2 Ni8 O15W 85.31(14) . . ? N53 Ni8 O15W 175.94(18) . . ? C2 O1 Ni2 112.4(2) . . ? C2 O2 Ni8 113.6(3) . . ? C1 O3 Ni8 112.2(2) . . ? C4 O4 Ni2 113.5(2) . . ? C4 O5 Ni6 113.3(2) . . ? C3 O6 Ni6 112.5(2) . . ? C5 O7 Ni5 112.7(2) . . ? C6 O8 Ni2 113.4(3) . . ? C6 O9 Ni5 113.9(3) . . ? C10 O10 Ni1 113.1(2) . . ? C10 O11 Ni3 113.6(2) . . ? C9 O12 Ni3 112.4(2) . . ? C7 O13 Ni4 112.0(2) . . ? C8 O14 Ni4 113.2(2) . . ? C8 O15 Ni1 114.3(2) . . ? C12 O16 Ni1 113.0(2) . . ? C12 O17 Ni7 111.4(2) . . ? C11 O18 Ni7 112.0(2) . . ? C1 N1 C13 119.8(3) . . ? C1 N1 Ni2 113.9(2) . . ? C13 N1 Ni2 126.1(2) . . ? C5 N2 C24 120.1(3) . . ? C5 N2 Ni2 114.8(3) . . ? C24 N2 Ni2 124.7(3) . . ? C3 N3 C21 117.9(3) . . ? C3 N3 Ni2 115.0(2) . . ? C21 N3 Ni2 126.8(3) . . ? C7 N4 C15 118.1(3) . . ? C7 N4 Ni1 114.3(2) . . ? C15 N4 Ni1 127.4(2) . . ? C9 N5 C19 119.0(3) . . ? C9 N5 Ni1 114.8(2) . . ? C19 N5 Ni1 126.1(2) . . ? C11 N6 C26 116.9(3) . . ? C11 N6 Ni1 115.3(2) . . ? C26 N6 Ni1 127.7(2) . . ? C47 N10 Ni6 116.1(4) . . ? C49 N11 Ni6 122.8(5) . . ? C70 N12 C56 108.2(11) . . ? C70 N12 Ni6 115.7(6) . . ? C56 N12 Ni6 113.1(3) . . ? C55 N14 Ni3 122.7(5) . . ? C52 N15 Ni3 121.5(5) . . ? C54 N17 C50 113.9(7) . . ? C54 N17 Ni3 118.6(4) . . ? C50 N17 Ni3 118.0(5) . . ? C33 N19 C63 109.7(5) . . ? C33 N19 Ni4 113.3(3) . . ? C63 N19 Ni4 114.0(4) . . ? C57 N24 Ni7 122.7(4) . . ? C40 N27 Ni5 123.3(5) . . ? C31 N18 Ni4 115.1(3) . . ? C34 N20 Ni4 122.4(4) . . ? C60 N21 Ni7 115.6(6) . . ? C59 N23 C58 110.2(7) . . ? C59 N23 Ni7 115.5(5) . . ? C58 N23 Ni7 116.6(5) . . ? C36 N26 Ni8 116.4(4) . . ? C44 N50 Ni5 122.4(5) . . ? C42 N51 C43 109.9(6) . . ? C42 N51 Ni5 112.4(3) . . ? C43 N51 Ni5 112.8(4) . . ? C62 N53 C61 111.9(7) . . ? C62 N53 Ni8 115.3(4) . . ? C61 N53 Ni8 118.3(4) . . ? C45 N54 Ni8 121.3(4) . . ? O3 C1 N1 128.6(4) . . ? O3 C1 C2 117.9(4) . . ? N1 C1 C2 113.5(4) . . ? O1 C2 O2 125.2(4) . . ? O1 C2 C1 119.5(4) . . ? O2 C2 C1 115.2(5) . . ? O6 C3 N3 128.0(4) . . ? O6 C3 C4 117.0(4) . . ? N3 C3 C4 115.0(4) . . ? O4 C4 O5 126.2(4) . . ? O4 C4 C3 117.3(4) . . ? O5 C4 C3 116.5(4) . . ? N2 C5 O7 129.1(4) . . ? N2 C5 C6 114.3(4) . . ? O7 C5 C6 116.6(4) . . ? O9 C6 O8 124.8(4) . . ? O9 C6 C5 117.4(4) . . ? O8 C6 C5 117.8(4) . . ? O13 C7 N4 129.1(4) . . ? O13 C7 C8 116.3(4) . . ? N4 C7 C8 114.6(4) . . ? O14 C8 O15 125.0(4) . . ? O14 C8 C7 117.4(4) . . ? O15 C8 C7 117.6(4) . . ? O12 C9 N5 128.4(4) . . ? O12 C9 C10 117.2(4) . . ? N5 C9 C10 114.3(4) . . ? O11 C10 O10 124.9(4) . . ? O11 C10 C9 116.9(4) . . ? O10 C10 C9 118.2(4) . . ? O18 C11 N6 128.4(4) . . ? O18 C11 C12 116.8(4) . . ? N6 C11 C12 114.8(4) . . ? O16 C12 O17 126.3(4) . . ? O16 C12 C11 117.5(4) . . ? O17 C12 C11 116.2(4) . . ? C14 C13 C18 119.3(4) . . ? C14 C13 N1 119.5(4) . . ? C18 C13 N1 121.0(4) . . ? C15 C14 C13 120.9(4) . . ? C14 C15 C16 119.8(4) . . ? C14 C15 N4 119.3(4) . . ? C16 C15 N4 120.8(4) . . ? C17 C16 C15 119.4(4) . . ? C16 C17 C18 121.2(4) . . ? C17 C18 C13 119.4(4) . . ? C23 C19 C20 119.9(4) . . ? C23 C19 N5 121.1(4) . . ? C20 C19 N5 118.8(4) . . ? C21 C20 C19 120.5(4) . . ? C22 C21 C20 119.6(4) . . ? C22 C21 N3 120.5(4) . . ? C20 C21 N3 119.6(4) . . ? C27 C22 C21 119.6(5) . . ? C19 C23 C27 119.2(5) . . ? C28 C24 C25 119.3(4) . . ? C28 C24 N2 120.8(4) . . ? C25 C24 N2 119.7(4) . . ? C26 C25 C24 120.3(4) . . ? C25 C26 C30 120.4(4) . . ? C25 C26 N6 118.8(4) . . ? C30 C26 N6 120.7(4) . . ? C22 C27 C23 121.1(5) . . ? C29 C28 C24 119.9(5) . . ? C28 C29 C30 120.5(5) . . ? C26 C30 C29 119.4(5) . . ? N18 C31 C32 110.5(6) . . ? C33 C32 C31 115.1(6) . . ? N19 C33 C32 114.5(6) . . ? N20 C34 C35 114.4(7) . . ? C63 C35 C34 113.9(9) . . ? C37 C36 N26 113.0(7) . . ? C36 C37 C62 118.3(8) . . ? N27 C40 C41 115.4(8) . . ? C40 C41 C42 113.2(8) . . ? C41 C42 N51 114.5(7) . . ? C64 C43 N51 114.4(7) . . ? N50 C44 C64 112.3(7) . . ? N54 C45 C46 119.2(8) . . ? C61 C46 C45 118.7(10) . . ? C48 C47 N10 110.1(7) . . ? C56 C48 C47 117.0(8) . . ? C71 C49 N11 110.8(9) . . ? C51 C50 N17 119.1(7) . . ? C55 C51 C50 120.8(10) . . ? C53 C52 N15 120.0(8) . . ? C54 C53 C52 123.5(9) . . ? N17 C54 C53 120.4(8) . . ? C51 C55 N14 116.0(10) . . ? C48 C56 N12 115.0(8) . . ? C72 C57 N24 116.0(8) . . ? C72 C58 N23 120.6(10) . . ? N23 C59 C73 113.1(9) . . ? C73 C60 N21 113.2(9) . . ? C46 C61 N53 119.4(9) . . ? N53 C62 C37 113.4(7) . . ? C35 C63 N19 114.6(8) . . ? C44 C64 C43 113.8(8) . . ? C71 C70 N12 128.1(12) . . ? C70 C71 C49 139.8(13) . . ? C58 C72 C57 126.1(16) . . ? C60 C73 C59 117.2(10) . . ? O13A Cl1 O11A 102.8(12) . . ? O13A Cl1 O12A 113.3(9) . . ? O11A Cl1 O12A 110.1(9) . . ? O13A Cl1 O14A 116.9(8) . . ? O11A Cl1 O14A 102.0(9) . . ? O12A Cl1 O14A 110.6(6) . . ? O21A Cl2 O23A 115.1(6) . . ? O21A Cl2 O22A 115.7(7) . . ? O23A Cl2 O22A 112.9(7) . . ? O21A Cl2 O24A 103.4(7) . . ? O23A Cl2 O24A 106.9(6) . . ? O22A Cl2 O24A 100.9(7) . . ? O32A Cl3 O31A 112.3(8) . . ? O32A Cl3 O33A 115.3(8) . . ? O31A Cl3 O33A 114.5(8) . . ? O32A Cl3 O34A 111.0(12) . . ? O31A Cl3 O34A 98.3(11) . . ? O33A Cl3 O34A 103.7(9) . . ? O43A Cl4 O41A 105.7(17) . . ? O43A Cl4 O42A 121(2) . . ? O41A Cl4 O42A 119.4(19) . . ? O43A Cl4 O44A 93.4(16) . . ? O41A Cl4 O44A 113.0(9) . . ? O42A Cl4 O44A 101.1(18) . . ? _diffrn_measured_fraction_theta_max 0.875 _diffrn_reflns_theta_full 28.78 _diffrn_measured_fraction_theta_full 0.875 _refine_diff_density_max 1.908 _refine_diff_density_min -0.991 _refine_diff_density_rms 0.154 data_compound_Monomer _database_code_depnum_ccdc_archive 'CCDC 611876' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H44 Cu2 Li0 N4 Na4 O18' _chemical_formula_weight 1135.87 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' Cu Cu 0.3201 1.2651 '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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 23.4405(15) _cell_length_b 19.8751(15) _cell_length_c 14.5335(15) _cell_angle_alpha 84.359(3) _cell_angle_beta 57.542(4) _cell_angle_gamma 38.099(16) _cell_volume 2759.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.367 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164 _exptl_absorpt_coefficient_mu 0.871 _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 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11917 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.1239 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 6.40 _diffrn_reflns_theta_max 27.49 _reflns_number_total 9569 _reflns_number_gt 4981 _reflns_threshold_expression >2sigma(I) _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^)+(0.0546P)^2^+1.8672P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9569 _refine_ls_number_parameters 667 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1491 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1427 _refine_ls_wR_factor_gt 0.1165 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.814 _refine_ls_shift/su_mean 0.010 _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' 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 O2W O -0.2880(3) 0.0157(3) -0.0502(3) 0.0401(9) Uani 1 1 d . . . O3W O 0.0154(3) -0.2877(3) -0.1774(3) 0.0410(9) Uani 1 1 d . . . O10 O -0.3405(3) 0.2041(3) 0.1877(3) 0.0416(9) Uani 1 1 d . . . C45 C -0.2242(5) 0.1238(5) 0.1188(5) 0.0342(13) Uani 1 1 d . . . O1W O -0.2432(6) -0.2436(6) -0.0059(11) 0.220(6) Uani 1 1 d . . . O13 O -0.1983(3) 0.1584(3) 0.1274(3) 0.0435(10) Uani 1 1 d . . . O11 O -0.3727(4) -0.0874(3) 0.3017(3) 0.0448(10) Uani 1 1 d . . . O6W O -0.6772(3) 0.4496(3) 0.5152(3) 0.0415(9) Uani 1 1 d . . . O5W O -0.5506(3) 0.3229(3) 0.2127(3) 0.0424(9) Uani 1 1 d . . . O4W O -0.5060(11) 0.4925(11) 0.2567(6) 0.220(5) Uani 1 1 d . . . Cu1 Cu 0.0000 0.0000 0.0000 0.0354(3) Uani 1 2 d S . . Cu2 Cu 0.0000 0.0000 -0.5000 0.0358(3) Uani 1 2 d S . . Cu3 Cu -0.5000 0.0000 0.5000 0.0357(3) Uani 1 2 d S . . Cu4 Cu 0.0000 -0.5000 -0.5000 0.0354(3) Uani 1 2 d S . . Na3 Na -0.35043(18) 0.10047(19) 0.14975(18) 0.0324(5) Uani 1 1 d . . . Na1 Na 0.10028(19) -0.35045(19) -0.39974(18) 0.0326(5) Uani 1 1 d . . . Na4 Na -0.56732(19) 0.4326(2) 0.3171(2) 0.0479(6) Uani 1 1 d . . . Na2 Na -0.1823(2) -0.1830(2) -0.06754(19) 0.0475(6) Uani 1 1 d . . . O6 O -0.0877(3) -0.3728(4) -0.3412(3) 0.0427(10) Uani 1 1 d . . . O1 O -0.1145(3) -0.0744(3) -0.0029(3) 0.0443(10) Uani 1 1 d . . . O7 O 0.1584(3) -0.1981(3) -0.5873(3) 0.0430(10) Uani 1 1 d . . . O3 O -0.3117(3) -0.0519(3) 0.1590(3) 0.0406(9) Uani 1 1 d . . . N4 N -0.1071(4) 0.0216(4) -0.3565(4) 0.0320(10) Uani 1 1 d . . . O4 O 0.1912(3) -0.5023(3) -0.5739(3) 0.0436(10) Uani 1 1 d . . . O9 O -0.0742(3) -0.1147(3) -0.3087(3) 0.0441(10) Uani 1 1 d . . . N2 N -0.5582(4) 0.1435(4) 0.5216(4) 0.0329(10) Uani 1 1 d . . . N1 N 0.0218(4) -0.1072(4) -0.0580(4) 0.0312(10) Uani 1 1 d . . . O2 O -0.5026(3) 0.1915(3) 0.3858(3) 0.0441(10) Uani 1 1 d . . . O8 O 0.2042(3) -0.3406(3) -0.5514(3) 0.0419(10) Uani 1 1 d . . . N3 N 0.1433(4) -0.5582(4) -0.6073(4) 0.0341(11) Uani 1 1 d . . . C42 C -0.2539(5) 0.1518(5) -0.2326(5) 0.0322(13) Uani 1 1 d . . . C11 C -0.0960(5) -0.0339(5) 0.0105(5) 0.0295(12) Uani 1 1 d . . . O5 O -0.0511(3) -0.3126(3) -0.2960(3) 0.0415(10) Uani 1 1 d . . . C33 C -0.0184(5) -0.3813(5) -0.3761(5) 0.0324(12) Uani 1 1 d . . . C21 C -0.4901(5) 0.1194(5) 0.4045(5) 0.0315(12) Uani 1 1 d . . . C1 C 0.1517(5) -0.2541(5) -0.1651(5) 0.0320(13) Uani 1 1 d . . . C43 C -0.0342(5) -0.0956(5) -0.3803(5) 0.0295(12) Uani 1 1 d . . . C17 C -0.6649(5) 0.2669(5) 0.6512(5) 0.0321(13) Uani 1 1 d . . . C27 C 0.2675(5) -0.6653(6) -0.7546(5) 0.0342(13) Uani 1 1 d . . . C32 C 0.1195(5) -0.4900(5) -0.5339(5) 0.0310(12) Uani 1 1 d . . . C22 C -0.3805(5) -0.0192(5) 0.2754(5) 0.0329(13) Uani 1 1 d . . . C44 C 0.1237(5) -0.2241(5) -0.5183(5) 0.0313(12) Uani 1 1 d . . . C40 C -0.3059(6) 0.2310(6) -0.1218(5) 0.0416(14) Uani 1 1 d . . . C18 C -0.8033(6) 0.3781(5) 0.7310(5) 0.0414(14) Uani 1 1 d . . . C2 C 0.2311(5) -0.3058(5) -0.3031(6) 0.0413(15) Uani 1 1 d . . . C26 C 0.3791(5) -0.8041(6) -0.8064(5) 0.0428(15) Uani 1 1 d . . . C3 C 0.3646(6) -0.4497(6) -0.4088(6) 0.0512(17) Uani 1 1 d . . . H3 H 0.4188 -0.4842 -0.5011 0.061 Uiso 1 1 calc R . . C35 C -0.3440(6) 0.2037(6) -0.2250(6) 0.0533(17) Uani 1 1 d . . . C15 C -0.6343(6) 0.2746(6) 0.7041(6) 0.0533(17) Uani 1 1 d . . . C39 C -0.4508(6) 0.3651(6) -0.0057(5) 0.0527(18) Uani 1 1 d . . . H39 H -0.4856 0.4193 0.0673 0.063 Uiso 1 1 calc R . . C25 C 0.4943(6) -0.9084(6) -0.9501(6) 0.0541(18) Uani 1 1 d . . . H25 H 0.5676 -1.0009 -0.9850 0.065 Uiso 1 1 calc R . . C28 C 0.2749(6) -0.6343(6) -0.8441(6) 0.0521(16) Uani 1 1 d . . . C19 C -0.9077(6) 0.4932(5) 0.8632(6) 0.0512(17) Uani 1 1 d . . . H19 H -1.0001 0.5663 0.9170 0.061 Uiso 1 1 calc R . . C24 C 0.5039(7) -0.8809(8) -1.0406(6) 0.0594(19) Uani 1 1 d . . . C6 C 0.2037(6) -0.3439(6) -0.1344(6) 0.0556(17) Uani 1 1 d . . . C23 C 0.6334(7) -1.0001(8) -1.1978(6) 0.101(3) Uani 1 1 d . . . H23A H 0.6951 -1.0170 -1.2366 0.151 Uiso 1 1 calc R . . H23B H 0.6060 -0.9751 -1.2410 0.151 Uiso 1 1 calc R . . H23C H 0.6802 -1.0829 -1.2144 0.151 Uiso 1 1 calc R . . C31 C 0.3730(7) -0.8384(7) -0.7084(6) 0.072(2) Uani 1 1 d . . . H31A H 0.3730 -0.8077 -0.6612 0.109 Uiso 1 1 calc R . . H31B H 0.4527 -0.9372 -0.7602 0.109 Uiso 1 1 calc R . . H31C H 0.2895 -0.7920 -0.6413 0.109 Uiso 1 1 calc R . . C12 C -0.9993(8) 0.6329(7) 1.0638(7) 0.100(3) Uani 1 1 d . . . H12A H -0.9624 0.6177 1.0907 0.149 Uiso 1 1 calc R . . H12B H -1.0622 0.6513 1.1283 0.149 Uiso 1 1 calc R . . H12C H -1.0483 0.7112 1.0643 0.149 Uiso 1 1 calc R . . C10 C 0.5644(7) -0.6978(6) -0.4991(8) 0.099(3) Uani 1 1 d . . . H10A H 0.5826 -0.7206 -0.5760 0.148 Uiso 1 1 calc R . . H10B H 0.5718 -0.7466 -0.4670 0.148 Uiso 1 1 calc R . . H10C H 0.6311 -0.7248 -0.5286 0.148 Uiso 1 1 calc R . . C38 C -0.6968(6) 0.5630(7) 0.1334(7) 0.100(3) Uani 1 1 d . . . H38A H -0.7393 0.5566 0.1795 0.150 Uiso 1 1 calc R . . H38B H -0.7364 0.6191 0.1070 0.150 Uiso 1 1 calc R . . H38C H -0.7132 0.6048 0.1953 0.150 Uiso 1 1 calc R . . C14 C -0.7439(8) 0.3942(7) 0.8369(7) 0.066(2) Uani 1 1 d . . . H14 H -0.7231 0.3997 0.8717 0.079 Uiso 1 1 calc R . . C41 C -0.2083(7) 0.1743(7) -0.1277(6) 0.071(2) Uani 1 1 d . . . H41A H -0.1553 0.0920 -0.1352 0.106 Uiso 1 1 calc R . . H41B H -0.2611 0.2431 -0.0443 0.106 Uiso 1 1 calc R . . H41C H -0.1461 0.1515 -0.2072 0.106 Uiso 1 1 calc R . . C9 C 0.1747(7) -0.2094(7) -0.3387(7) 0.070(2) Uani 1 1 d . . . H9A H 0.0934 -0.1580 -0.3029 0.105 Uiso 1 1 calc R . . H9B H 0.2441 -0.2625 -0.4380 0.105 Uiso 1 1 calc R . . H9C H 0.1503 -0.1458 -0.2978 0.105 Uiso 1 1 calc R . . C5 C 0.3360(7) -0.4870(6) -0.2444(8) 0.0632(19) Uani 1 1 d . . . H5 H 0.3698 -0.5481 -0.2236 0.076 Uiso 1 1 calc R . . C13 C -0.8801(7) 0.5034(6) 0.9176(6) 0.0577(18) Uani 1 1 d . . . C8 C 0.1187(8) -0.2864(8) 0.0163(7) 0.093(3) Uani 1 1 d . . . H8A H 0.0994 -0.2289 0.0589 0.140 Uiso 1 1 calc R . . H8B H 0.1702 -0.3621 0.0202 0.140 Uiso 1 1 calc R . . H8C H 0.0326 -0.2319 0.0653 0.140 Uiso 1 1 calc R . . C37 C -0.5413(6) 0.4182(6) 0.0043(6) 0.0595(19) Uani 1 1 d . . . C4 C 0.4176(6) -0.5409(6) -0.3808(7) 0.0575(18) Uani 1 1 d . . . C36 C -0.4857(6) 0.3349(7) -0.1058(7) 0.066(2) Uani 1 1 d . . . H36 H -0.5465 0.3684 -0.0998 0.079 Uiso 1 1 calc R . . C29 C 0.3951(7) -0.7444(8) -0.9868(6) 0.066(2) Uani 1 1 d . . . H29 H 0.4014 -0.7239 -1.0482 0.079 Uiso 1 1 calc R . . C16 C -0.4833(8) 0.1519(8) 0.6187(8) 0.093(3) Uani 1 1 d . . . H16A H -0.4454 0.0760 0.6149 0.139 Uiso 1 1 calc R . . H16B H -0.4785 0.1791 0.6612 0.139 Uiso 1 1 calc R . . H16C H -0.4306 0.1230 0.5259 0.139 Uiso 1 1 calc R . . C20 C -0.8384(7) 0.3723(7) 0.6747(7) 0.070(2) Uani 1 1 d . . . H20A H -0.7985 0.3611 0.5904 0.105 Uiso 1 1 calc R . . H20B H -0.9377 0.4571 0.7422 0.105 Uiso 1 1 calc R . . H20C H -0.8013 0.2948 0.6554 0.105 Uiso 1 1 calc R . . C34 C -0.2874(9) 0.1184(9) -0.3475(8) 0.103(3) Uani 1 1 d . . . H34A H -0.2431 0.1121 -0.4245 0.154 Uiso 1 1 calc R . . H34B H -0.3626 0.1628 -0.3207 0.154 Uiso 1 1 calc R . . H34C H -0.2208 0.0266 -0.3744 0.154 Uiso 1 1 calc R . . C30 C 0.1503(8) -0.4830(8) -0.7862(8) 0.100(3) Uani 1 1 d . . . H30A H 0.0714 -0.4428 -0.7330 0.150 Uiso 1 1 calc R . . H30B H 0.1722 -0.4787 -0.8617 0.150 Uiso 1 1 calc R . . H30C H 0.1289 -0.4320 -0.7272 0.150 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 O2W 0.036(2) 0.042(2) 0.0300(19) 0.0178(17) -0.0209(17) -0.0341(19) O3W 0.043(2) 0.038(2) 0.0326(19) 0.0183(17) -0.0261(18) -0.0354(19) O10 0.0202(19) 0.0287(19) 0.047(2) 0.0109(17) -0.0182(18) -0.0201(18) C45 0.025(3) 0.024(3) 0.032(3) 0.010(2) -0.018(3) -0.020(3) O1W 0.067(4) 0.066(4) 0.333(11) 0.083(6) -0.094(6) -0.058(4) O13 0.0246(18) 0.0280(19) 0.049(2) 0.0080(17) -0.0197(18) -0.0219(18) O11 0.052(2) 0.0341(19) 0.0230(18) 0.0160(16) -0.0196(18) -0.038(2) O6W 0.034(2) 0.0299(19) 0.043(2) 0.0190(17) -0.0267(18) -0.0268(18) O5W 0.0286(19) 0.0342(19) 0.040(2) 0.0204(17) -0.0221(17) -0.0258(18) O4W 0.330(11) 0.325(11) 0.072(4) 0.085(5) -0.095(6) -0.320(11) Cu1 0.0253(5) 0.0277(5) 0.0406(5) 0.0118(4) -0.0210(4) -0.0226(4) Cu2 0.0282(5) 0.0253(5) 0.0304(5) 0.0182(4) -0.0170(4) -0.0230(4) Cu3 0.0400(5) 0.0296(5) 0.0245(5) 0.0175(4) -0.0200(4) -0.0309(5) Cu4 0.0293(5) 0.0398(5) 0.0265(5) 0.0106(4) -0.0158(4) -0.0307(5) Na3 0.0322(10) 0.0333(10) 0.0320(10) 0.0189(9) -0.0216(9) -0.0297(10) Na1 0.0348(10) 0.0332(10) 0.0320(10) 0.0192(9) -0.0227(9) -0.0311(10) Na4 0.0267(11) 0.0272(11) 0.0499(12) 0.0156(10) -0.0199(10) -0.0222(10) Na2 0.0508(13) 0.0498(12) 0.0251(11) 0.0149(10) -0.0197(10) -0.0455(12) O6 0.0319(19) 0.050(2) 0.0261(18) 0.0074(17) -0.0121(17) -0.037(2) O1 0.0312(19) 0.0320(19) 0.050(2) 0.0110(17) -0.0234(18) -0.0276(18) O7 0.0266(19) 0.0245(18) 0.035(2) 0.0189(17) -0.0147(17) -0.0212(17) O3 0.043(2) 0.041(2) 0.0212(19) 0.0186(17) -0.0174(18) -0.038(2) N4 0.026(2) 0.022(2) 0.028(2) 0.017(2) -0.017(2) -0.020(2) O4 0.0289(19) 0.046(2) 0.0303(19) 0.0073(17) -0.0126(17) -0.0328(19) O9 0.0316(19) 0.0319(19) 0.034(2) 0.0196(17) -0.0162(17) -0.0275(18) N2 0.036(2) 0.031(2) 0.019(2) 0.017(2) -0.017(2) -0.030(2) N1 0.021(2) 0.024(2) 0.038(2) 0.012(2) -0.020(2) -0.019(2) O2 0.046(2) 0.0327(19) 0.0287(19) 0.0171(17) -0.0205(18) -0.035(2) O8 0.0269(19) 0.0187(18) 0.037(2) 0.0149(16) -0.0167(17) -0.0179(18) N3 0.029(2) 0.036(2) 0.025(2) 0.010(2) -0.015(2) -0.028(2) C42 0.027(3) 0.025(3) 0.030(3) 0.020(3) -0.019(3) -0.023(3) C11 0.026(3) 0.025(3) 0.032(3) 0.014(2) -0.020(2) -0.022(3) O5 0.040(2) 0.045(2) 0.0285(19) 0.0104(17) -0.0199(18) -0.037(2) C33 0.025(3) 0.032(3) 0.026(3) 0.014(2) -0.016(2) -0.025(3) C21 0.031(3) 0.025(3) 0.033(3) 0.017(2) -0.023(3) -0.024(3) C1 0.026(3) 0.024(3) 0.042(3) 0.014(3) -0.024(3) -0.021(3) C43 0.031(3) 0.027(3) 0.025(3) 0.016(2) -0.018(2) -0.026(3) C17 0.042(3) 0.031(3) 0.028(3) 0.022(3) -0.026(3) -0.033(3) C27 0.033(3) 0.043(3) 0.026(3) 0.015(3) -0.018(3) -0.035(3) C32 0.022(3) 0.028(3) 0.031(3) 0.014(2) -0.018(2) -0.021(3) C22 0.034(3) 0.026(3) 0.028(3) 0.016(3) -0.021(3) -0.026(3) C44 0.027(3) 0.029(3) 0.022(3) 0.015(2) -0.015(2) -0.024(3) C40 0.037(3) 0.037(3) 0.036(3) 0.027(3) -0.026(3) -0.031(3) C18 0.043(4) 0.032(3) 0.034(3) 0.022(3) -0.026(3) -0.032(3) C2 0.030(3) 0.030(3) 0.044(4) 0.013(3) -0.026(3) -0.024(3) C26 0.034(3) 0.048(4) 0.034(3) 0.016(3) -0.023(3) -0.035(3) C3 0.037(3) 0.042(3) 0.043(3) 0.010(3) -0.024(3) -0.032(3) C35 0.043(4) 0.047(4) 0.048(4) 0.028(3) -0.034(3) -0.037(4) C15 0.054(4) 0.052(4) 0.049(4) 0.030(3) -0.038(3) -0.046(4) C39 0.035(4) 0.031(3) 0.028(3) 0.014(3) -0.015(3) -0.025(3) C25 0.030(3) 0.046(4) 0.038(4) 0.009(3) -0.017(3) -0.030(3) C28 0.049(4) 0.056(4) 0.042(4) 0.031(3) -0.033(3) -0.045(4) C19 0.038(3) 0.025(3) 0.038(3) 0.017(3) -0.023(3) -0.024(3) C24 0.044(4) 0.067(5) 0.031(4) 0.015(4) -0.023(3) -0.045(4) C6 0.048(4) 0.041(4) 0.051(4) 0.022(3) -0.035(3) -0.035(3) C23 0.061(5) 0.093(6) 0.030(4) 0.007(4) -0.019(4) -0.058(5) C31 0.052(4) 0.053(4) 0.054(4) 0.028(4) -0.035(4) -0.041(4) C12 0.095(6) 0.062(4) 0.046(4) 0.017(4) -0.045(4) -0.059(5) C10 0.054(4) 0.030(4) 0.095(6) 0.014(4) -0.051(4) -0.022(4) C38 0.026(4) 0.043(4) 0.052(4) 0.011(4) -0.013(3) -0.014(4) C14 0.080(5) 0.058(4) 0.063(4) 0.035(4) -0.058(4) -0.059(5) C41 0.064(4) 0.070(4) 0.051(4) 0.032(4) -0.041(4) -0.056(4) C9 0.066(4) 0.054(4) 0.056(4) 0.031(4) -0.044(4) -0.048(4) C5 0.056(4) 0.033(3) 0.081(5) 0.035(4) -0.054(4) -0.035(4) C13 0.065(5) 0.041(4) 0.043(4) 0.025(3) -0.040(4) -0.043(4) C8 0.095(6) 0.077(5) 0.077(5) 0.058(5) -0.066(5) -0.072(5) C37 0.030(4) 0.041(4) 0.043(4) 0.026(3) -0.023(3) -0.025(3) C4 0.043(4) 0.033(3) 0.069(5) 0.020(3) -0.041(4) -0.029(3) C36 0.032(4) 0.057(4) 0.061(5) 0.031(4) -0.032(4) -0.034(4) C29 0.070(5) 0.084(5) 0.034(4) 0.039(4) -0.037(4) -0.067(5) C16 0.077(5) 0.088(6) 0.097(6) 0.044(5) -0.067(5) -0.068(5) C20 0.056(4) 0.056(4) 0.064(4) 0.028(4) -0.044(4) -0.044(4) C34 0.086(6) 0.106(6) 0.091(6) 0.040(5) -0.064(5) -0.080(6) C30 0.089(6) 0.072(5) 0.077(5) 0.056(5) -0.061(5) -0.064(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O2W Na2 2.434(4) . ? O2W Na3 2.437(4) . ? O3W Na2 2.427(4) . ? O3W Na1 2.437(4) . ? O10 C45 1.232(6) . ? O10 Na4 2.318(4) . ? O10 Na3 2.391(4) . ? C45 O13 1.270(6) . ? C45 C11 1.549(7) . ? O1W Na2 2.326(7) . ? O13 Cu1 1.955(3) . ? O11 C22 1.266(6) . ? O11 Cu3 1.955(3) . ? O6W Na4 2.429(4) . ? O6W Na1 2.439(4) 1_466 ? O5W Na4 2.423(4) . ? O5W Na3 2.436(4) . ? O4W Na4 2.322(7) . ? Cu1 N1 1.922(4) 2 ? Cu1 N1 1.922(4) . ? Cu1 O13 1.955(3) 2 ? Cu2 N4 1.923(4) . ? Cu2 N4 1.923(4) 2_554 ? Cu2 O7 1.953(3) 2_554 ? Cu2 O7 1.953(3) . ? Cu3 N2 1.920(4) . ? Cu3 N2 1.920(4) 2_456 ? Cu3 O11 1.955(3) 2_456 ? Cu4 N3 1.917(4) . ? Cu4 N3 1.917(4) 2_544 ? Cu4 O6 1.954(3) 2_544 ? Cu4 O6 1.954(3) . ? Na3 O1 2.383(4) . ? Na3 O2 2.386(4) . ? Na3 O3 2.395(4) . ? Na3 Na4 3.521(3) . ? Na3 Na2 3.527(3) . ? Na1 O4 2.376(4) . ? Na1 O9 2.384(4) . ? Na1 O5 2.389(4) . ? Na1 O8 2.394(4) . ? Na1 O6W 2.439(4) 1_644 ? Na1 Na2 3.521(3) . ? Na1 Na4 3.525(3) 1_644 ? Na4 O8 2.317(4) 1_466 ? Na4 Na1 3.525(3) 1_466 ? Na2 O3 2.315(4) . ? Na2 O5 2.317(4) . ? O6 C33 1.273(6) . ? O1 C11 1.244(5) . ? O7 C44 1.272(6) . ? O3 C22 1.234(6) . ? N4 C43 1.313(6) . ? N4 C42 1.425(6) . ? O4 C32 1.247(5) . ? O9 C43 1.241(5) . ? N2 C21 1.309(6) . ? N2 C17 1.420(6) . ? N1 C11 1.318(6) . ? N1 C1 1.425(6) . ? O2 C21 1.249(6) . ? O8 C44 1.234(6) . ? O8 Na4 2.317(4) 1_644 ? N3 C32 1.318(6) . ? N3 C27 1.429(6) . ? C42 C35 1.372(8) . ? C42 C40 1.388(7) . ? O5 C33 1.232(6) . ? C33 C32 1.550(7) . ? C21 C22 1.554(7) . ? C1 C6 1.369(8) . ? C1 C2 1.390(8) . ? C43 C44 1.551(7) . ? C17 C15 1.385(8) . ? C17 C18 1.391(7) . ? C27 C28 1.368(8) . ? C27 C26 1.399(8) . ? C40 C39 1.404(8) . ? C40 C41 1.505(8) . ? C18 C19 1.386(7) . ? C18 C20 1.500(8) . ? C2 C3 1.396(7) . ? C2 C9 1.495(8) . ? C26 C25 1.392(7) . ? C26 C31 1.502(9) . ? C3 C4 1.359(9) . ? C35 C36 1.383(8) . ? C35 C34 1.523(9) . ? C15 C14 1.394(8) . ? C15 C16 1.520(9) . ? C39 C37 1.345(9) . ? C25 C24 1.347(9) . ? C28 C29 1.394(8) . ? C28 C30 1.523(9) . ? C19 C13 1.368(9) . ? C24 C29 1.365(9) . ? C24 C23 1.533(8) . ? C6 C5 1.397(8) . ? C6 C8 1.516(9) . ? C12 C13 1.527(8) . ? C10 C4 1.529(8) . ? C38 C37 1.517(8) . ? C14 C13 1.362(9) . ? C5 C4 1.363(9) . ? C37 C36 1.374(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Na2 O2W Na3 92.79(14) . . ? Na2 O3W Na1 92.75(14) . . ? C45 O10 Na4 145.0(3) . . ? C45 O10 Na3 116.5(3) . . ? Na4 O10 Na3 96.78(14) . . ? O10 C45 O13 125.8(4) . . ? O10 C45 C11 118.5(5) . . ? O13 C45 C11 115.7(4) . . ? C45 O13 Cu1 113.3(3) . . ? C22 O11 Cu3 113.5(3) . . ? Na4 O6W Na1 92.82(14) . 1_466 ? Na4 O5W Na3 92.88(14) . . ? N1 Cu1 N1 180.0(2) 2 . ? N1 Cu1 O13 95.77(15) 2 . ? N1 Cu1 O13 84.23(15) . . ? N1 Cu1 O13 84.22(15) 2 2 ? N1 Cu1 O13 95.78(15) . 2 ? O13 Cu1 O13 180.0(4) . 2 ? N4 Cu2 N4 180.0(5) . 2_554 ? N4 Cu2 O7 95.80(15) . 2_554 ? N4 Cu2 O7 84.20(15) 2_554 2_554 ? N4 Cu2 O7 84.20(15) . . ? N4 Cu2 O7 95.80(15) 2_554 . ? O7 Cu2 O7 180.0(3) 2_554 . ? N2 Cu3 N2 180.0(3) . 2_456 ? N2 Cu3 O11 84.14(15) . . ? N2 Cu3 O11 95.86(15) 2_456 . ? N2 Cu3 O11 95.86(15) . 2_456 ? N2 Cu3 O11 84.14(15) 2_456 2_456 ? O11 Cu3 O11 180.000(1) . 2_456 ? N3 Cu4 N3 180.00(18) . 2_544 ? N3 Cu4 O6 95.52(15) . 2_544 ? N3 Cu4 O6 84.48(15) 2_544 2_544 ? N3 Cu4 O6 84.48(15) . . ? N3 Cu4 O6 95.52(15) 2_544 . ? O6 Cu4 O6 180.00(19) 2_544 . ? O1 Na3 O2 123.43(16) . . ? O1 Na3 O10 69.95(12) . . ? O2 Na3 O10 95.01(14) . . ? O1 Na3 O3 94.83(14) . . ? O2 Na3 O3 69.99(12) . . ? O10 Na3 O3 148.56(16) . . ? O1 Na3 O5W 136.98(15) . . ? O2 Na3 O5W 89.53(14) . . ? O10 Na3 O5W 81.36(14) . . ? O3 Na3 O5W 124.35(15) . . ? O1 Na3 O2W 89.47(13) . . ? O2 Na3 O2W 136.95(15) . . ? O10 Na3 O2W 124.24(15) . . ? O3 Na3 O2W 81.31(13) . . ? O5W Na3 O2W 80.72(13) . . ? O1 Na3 Na4 109.65(12) . . ? O2 Na3 Na4 81.13(11) . . ? O10 Na3 Na4 40.82(9) . . ? O3 Na3 Na4 149.46(10) . . ? O5W Na3 Na4 43.41(10) . . ? O2W Na3 Na4 115.82(11) . . ? O1 Na3 Na2 80.92(11) . . ? O2 Na3 Na2 109.55(11) . . ? O10 Na3 Na2 149.24(11) . . ? O3 Na3 Na2 40.65(9) . . ? O5W Na3 Na2 116.01(12) . . ? O2W Na3 Na2 43.56(10) . . ? Na4 Na3 Na2 158.18(9) . . ? O4 Na1 O9 123.49(15) . . ? O4 Na1 O5 69.91(12) . . ? O9 Na1 O5 95.14(14) . . ? O4 Na1 O8 95.06(14) . . ? O9 Na1 O8 69.82(13) . . ? O5 Na1 O8 148.71(16) . . ? O4 Na1 O3W 136.99(15) . . ? O9 Na1 O3W 89.51(13) . . ? O5 Na1 O3W 81.41(13) . . ? O8 Na1 O3W 124.10(15) . . ? O4 Na1 O6W 89.56(14) . 1_644 ? O9 Na1 O6W 136.78(15) . 1_644 ? O5 Na1 O6W 124.26(15) . 1_644 ? O8 Na1 O6W 81.27(13) . 1_644 ? O3W Na1 O6W 80.65(13) . 1_644 ? O4 Na1 Na2 109.59(11) . . ? O9 Na1 Na2 81.15(11) . . ? O5 Na1 Na2 40.79(9) . . ? O8 Na1 Na2 149.29(11) . . ? O3W Na1 Na2 43.52(10) . . ? O6W Na1 Na2 115.87(12) 1_644 . ? O4 Na1 Na4 81.07(10) . 1_644 ? O9 Na1 Na4 109.45(12) . 1_644 ? O5 Na1 Na4 149.31(11) . 1_644 ? O8 Na1 Na4 40.72(9) . 1_644 ? O3W Na1 Na4 115.84(11) . 1_644 ? O6W Na1 Na4 43.48(10) 1_644 1_644 ? Na2 Na1 Na4 158.12(8) . 1_644 ? O8 Na4 O10 178.41(17) 1_466 . ? O8 Na4 O4W 91.0(3) 1_466 . ? O10 Na4 O4W 90.6(3) . . ? O8 Na4 O5W 95.77(15) 1_466 . ? O10 Na4 O5W 83.14(13) . . ? O4W Na4 O5W 137.4(2) . . ? O8 Na4 O6W 83.05(13) 1_466 . ? O10 Na4 O6W 95.71(15) . . ? O4W Na4 O6W 136.9(2) . . ? O5W Na4 O6W 85.67(13) . . ? O8 Na4 Na3 136.20(13) 1_466 . ? O10 Na4 Na3 42.40(10) . . ? O4W Na4 Na3 128.7(3) . . ? O5W Na4 Na3 43.71(9) . . ? O6W Na4 Na3 78.73(10) . . ? O8 Na4 Na1 42.38(10) 1_466 1_466 ? O10 Na4 Na1 136.12(13) . 1_466 ? O4W Na4 Na1 128.9(3) . 1_466 ? O5W Na4 Na1 78.65(10) . 1_466 ? O6W Na4 Na1 43.70(9) . 1_466 ? Na3 Na4 Na1 102.39(8) . 1_466 ? O3 Na2 O5 178.38(16) . . ? O3 Na2 O1W 90.6(3) . . ? O5 Na2 O1W 91.1(3) . . ? O3 Na2 O3W 95.71(14) . . ? O5 Na2 O3W 83.09(13) . . ? O1W Na2 O3W 137.1(2) . . ? O3 Na2 O2W 83.02(13) . . ? O5 Na2 O2W 95.80(14) . . ? O1W Na2 O2W 137.1(2) . . ? O3W Na2 O2W 85.75(14) . . ? O3 Na2 Na1 136.18(13) . . ? O5 Na2 Na1 42.34(10) . . ? O1W Na2 Na1 129.0(3) . . ? O3W Na2 Na1 43.74(9) . . ? O2W Na2 Na1 78.81(11) . . ? O3 Na2 Na3 42.37(10) . . ? O5 Na2 Na3 136.15(13) . . ? O1W Na2 Na3 128.6(3) . . ? O3W Na2 Na3 78.73(11) . . ? O2W Na2 Na3 43.64(9) . . ? Na1 Na2 Na3 102.46(8) . . ? C33 O6 Cu4 113.1(3) . . ? C11 O1 Na3 116.1(3) . . ? C44 O7 Cu2 113.2(3) . . ? C22 O3 Na2 144.8(3) . . ? C22 O3 Na3 116.5(3) . . ? Na2 O3 Na3 96.97(14) . . ? C43 N4 C42 120.7(4) . . ? C43 N4 Cu2 114.6(3) . . ? C42 N4 Cu2 124.7(3) . . ? C32 O4 Na1 116.6(3) . . ? C43 O9 Na1 116.6(3) . . ? C21 N2 C17 120.7(4) . . ? C21 N2 Cu3 114.5(3) . . ? C17 N2 Cu3 124.8(3) . . ? C11 N1 C1 120.5(4) . . ? C11 N1 Cu1 114.5(3) . . ? C1 N1 Cu1 125.0(3) . . ? C21 O2 Na3 116.3(3) . . ? C44 O8 Na4 145.0(3) . 1_644 ? C44 O8 Na1 116.4(3) . . ? Na4 O8 Na1 96.89(14) 1_644 . ? C32 N3 C27 120.5(4) . . ? C32 N3 Cu4 114.5(3) . . ? C27 N3 Cu4 125.1(3) . . ? C35 C42 C40 119.8(5) . . ? C35 C42 N4 121.0(5) . . ? C40 C42 N4 119.0(5) . . ? O1 C11 N1 129.0(4) . . ? O1 C11 C45 118.8(4) . . ? N1 C11 C45 112.2(4) . . ? C33 O5 Na2 144.9(3) . . ? C33 O5 Na1 116.5(3) . . ? Na2 O5 Na1 96.88(14) . . ? O5 C33 O6 125.8(4) . . ? O5 C33 C32 118.5(5) . . ? O6 C33 C32 115.7(4) . . ? O2 C21 N2 128.9(4) . . ? O2 C21 C22 118.5(4) . . ? N2 C21 C22 112.6(4) . . ? C6 C1 C2 120.0(5) . . ? C6 C1 N1 121.0(5) . . ? C2 C1 N1 118.7(5) . . ? O9 C43 N4 129.3(4) . . ? O9 C43 C44 118.5(4) . . ? N4 C43 C44 112.2(4) . . ? C15 C17 C18 119.5(5) . . ? C15 C17 N2 121.3(5) . . ? C18 C17 N2 119.1(5) . . ? C28 C27 C26 120.2(5) . . ? C28 C27 N3 121.2(5) . . ? C26 C27 N3 118.5(5) . . ? O4 C32 N3 129.3(4) . . ? O4 C32 C33 118.3(4) . . ? N3 C32 C33 112.3(4) . . ? O3 C22 O11 126.1(4) . . ? O3 C22 C21 118.6(5) . . ? O11 C22 C21 115.2(4) . . ? O8 C44 O7 125.7(4) . . ? O8 C44 C43 118.6(4) . . ? O7 C44 C43 115.7(4) . . ? C42 C40 C39 118.6(6) . . ? C42 C40 C41 120.4(5) . . ? C39 C40 C41 121.0(6) . . ? C19 C18 C17 119.1(6) . . ? C19 C18 C20 120.7(6) . . ? C17 C18 C20 120.2(5) . . ? C1 C2 C3 119.0(6) . . ? C1 C2 C9 120.8(5) . . ? C3 C2 C9 120.3(5) . . ? C25 C26 C27 118.3(6) . . ? C25 C26 C31 121.4(6) . . ? C27 C26 C31 120.4(5) . . ? C4 C3 C2 122.0(6) . . ? C42 C35 C36 118.6(6) . . ? C42 C35 C34 120.0(5) . . ? C36 C35 C34 121.4(6) . . ? C17 C15 C14 118.8(6) . . ? C17 C15 C16 119.6(5) . . ? C14 C15 C16 121.6(6) . . ? C37 C39 C40 122.6(6) . . ? C24 C25 C26 122.7(6) . . ? C27 C28 C29 118.2(6) . . ? C27 C28 C30 119.6(5) . . ? C29 C28 C30 122.1(6) . . ? C13 C19 C18 122.5(6) . . ? C25 C24 C29 117.5(6) . . ? C25 C24 C23 120.4(7) . . ? C29 C24 C23 122.0(7) . . ? C1 C6 C5 118.5(6) . . ? C1 C6 C8 119.6(5) . . ? C5 C6 C8 121.9(6) . . ? C13 C14 C15 122.7(6) . . ? C4 C5 C6 122.9(6) . . ? C14 C13 C19 117.4(6) . . ? C14 C13 C12 122.3(7) . . ? C19 C13 C12 120.3(7) . . ? C39 C37 C36 116.9(5) . . ? C39 C37 C38 120.3(7) . . ? C36 C37 C38 122.8(7) . . ? C3 C4 C5 117.6(6) . . ? C3 C4 C10 120.6(7) . . ? C5 C4 C10 121.8(7) . . ? C37 C36 C35 123.3(6) . . ? C24 C29 C28 123.0(6) . . ? _diffrn_measured_fraction_theta_max 0.753 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.753 _refine_diff_density_max 0.589 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.070 data_compound3 _database_code_depnum_ccdc_archive 'CCDC 758079' #TrackingRef 'compound_3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H150 Cl6 Cu6 N24 Na2 Ni2 O54' _chemical_formula_weight 3119.58 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' Cu Cu 0.3201 1.2651 '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' Ni Ni 0.3393 1.1124 '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' Na Na 0.0362 0.0249 '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 Hexagonal _symmetry_space_group_name_H-M P-6c2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, y, -z+1/2' '-y, -x, -z' '-y, -x, z+1/2' '-x+y, y, z+1/2' '-x+y, y, -z' 'x, x-y, -z' 'x, x-y, z+1/2' '-y, x-y, z' '-y, x-y, -z+1/2' '-x+y, -x, -z+1/2' '-x+y, -x, z' _cell_length_a 17.426(3) _cell_length_b 17.426(3) _cell_length_c 31.674(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8330(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'hexagonal prisms' _exptl_crystal_colour blue _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3216 _exptl_absorpt_coefficient_mu 1.148 _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 293(2) _diffrn_radiation_wavelength 0.72930 _diffrn_source synchrotron _diffrn_source_type 'ESRF-CRG BM16' _diffrn_radiation_monochromator 'Si 111' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9.6 _diffrn_radiation_detector 'ADSC Q210r CCD (binned mode)' _diffrn_measurement_device_type 'Single-axis HUBER diffractometer' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 72097 _diffrn_reflns_av_R_equivalents 0.0962 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 23.93 _reflns_number_total 4112 _reflns_number_gt 3833 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MxCube (ESRF, 2006)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.12(3) _refine_ls_number_reflns 4112 _refine_ls_number_parameters 277 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0992 _refine_ls_R_factor_gt 0.0970 _refine_ls_wR_factor_ref 0.2504 _refine_ls_wR_factor_gt 0.2465 _refine_ls_goodness_of_fit_ref 1.173 _refine_ls_restrained_S_all 1.180 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.002 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 C1 C 0.7751(5) 0.5067(4) 0.8870(2) 0.0470(16) Uani 1 1 d . . . C2 C 0.8235(4) 0.5020(4) 0.8476(2) 0.0457(15) Uani 1 1 d . . . C3 C 0.8158(4) 0.4168(4) 0.7883(2) 0.0408(14) Uani 1 1 d . . . C4 C 0.7900(5) 0.4350(5) 0.7500 0.0392(18) Uani 1 2 d S . . H4 H 0.7539 0.4602 0.7500 0.047 Uiso 1 2 calc SR . . C5 C 0.8729(4) 0.3811(5) 0.7880(2) 0.0497(15) Uani 1 1 d . . . H5 H 0.8913 0.3683 0.8132 0.060 Uiso 1 1 calc R . . C6 C 0.9011(7) 0.3652(7) 0.7500 0.052(2) Uani 1 2 d S . . H6 H 0.9401 0.3434 0.7500 0.062 Uiso 1 2 calc SR . . C7 C 0.8442(14) 0.7075(13) 0.8173(9) 0.167(9) Uani 1 1 d . . . H15A H 0.8360 0.6566 0.8017 0.251 Uiso 1 1 calc R . . H15B H 0.8422 0.7493 0.7982 0.251 Uiso 1 1 calc R . . H15C H 0.7980 0.6896 0.8379 0.251 Uiso 1 1 calc R . . C8 C 1.0077(16) 0.7807(9) 0.8093(4) 0.150(8) Uani 1 1 d . . . H14A H 1.0026 0.7308 0.7940 0.225 Uiso 1 1 calc R . . H14B H 1.0626 0.8088 0.8246 0.225 Uiso 1 1 calc R . . H14C H 1.0063 0.8222 0.7898 0.225 Uiso 1 1 calc R . . C9 C 0.9461(15) 0.8290(9) 0.8636(5) 0.128(6) Uani 1 1 d . . . H9A H 0.8913 0.8167 0.8773 0.154 Uiso 1 1 calc R . . H9B H 0.9650 0.8796 0.8451 0.154 Uiso 1 1 calc R . . C10 C 1.0190(12) 0.8478(8) 0.8973(5) 0.129(7) Uani 1 1 d . . . H8A H 1.0753 0.8658 0.8835 0.155 Uiso 1 1 calc R . . H8B H 1.0264 0.8949 0.9161 0.155 Uiso 1 1 calc R . . C11 C 0.9218(11) 0.7512(7) 0.9547(4) 0.142(7) Uani 1 1 d . . . H11A H 0.9046 0.6970 0.9696 0.213 Uiso 1 1 calc R . . H11B H 0.8708 0.7481 0.9414 0.213 Uiso 1 1 calc R . . H11C H 0.9470 0.7999 0.9742 0.213 Uiso 1 1 calc R . . C12 C 1.0684(10) 0.7670(11) 0.9412(5) 0.146(8) Uani 1 1 d . . . H7A H 1.0818 0.7997 0.9675 0.176 Uiso 1 1 calc R . . H7B H 1.1191 0.7982 0.9227 0.176 Uiso 1 1 calc R . . C13 C 1.0542(10) 0.6765(12) 0.9500(4) 0.148(7) Uani 1 1 d . . . H10A H 1.1096 0.6801 0.9580 0.178 Uiso 1 1 calc R . . H10B H 1.0122 0.6490 0.9729 0.178 Uiso 1 1 calc R . . C14 C 1.0920(11) 0.6385(13) 0.8838(5) 0.135(6) Uani 1 1 d . . . H13A H 1.1215 0.6985 0.8738 0.203 Uiso 1 1 calc R . . H13B H 1.0693 0.5986 0.8603 0.203 Uiso 1 1 calc R . . H13C H 1.1332 0.6279 0.8992 0.203 Uiso 1 1 calc R . . C15 C 0.9741(10) 0.5348(10) 0.9257(5) 0.121(5) Uani 1 1 d . . . H16A H 0.9259 0.5258 0.9437 0.181 Uiso 1 1 calc R . . H16B H 1.0142 0.5228 0.9411 0.181 Uiso 1 1 calc R . . H16C H 0.9513 0.4956 0.9019 0.181 Uiso 1 1 calc R . . Cu1 Cu 0.94262(6) 0.66471(6) 0.88038(3) 0.0646(4) Uani 1 1 d . . . N1 N 0.7808(3) 0.4284(3) 0.82627(15) 0.0399(12) Uani 1 1 d . . . N2 N 0.9332(7) 0.7503(6) 0.8392(3) 0.087(2) Uani 1 1 d . . . N3 N 0.9899(7) 0.7650(6) 0.9213(3) 0.106(4) Uani 1 1 d . . . N4 N 1.0196(6) 0.6242(7) 0.9113(3) 0.100(3) Uani 1 1 d . . . Ni1 Ni 0.6667 0.3333 0.85534(4) 0.0387(4) Uani 1 3 d S . . O1 O 0.7038(3) 0.4402(3) 0.89691(15) 0.0490(11) Uani 1 1 d . . . O2 O 0.8983(3) 0.5698(3) 0.83797(17) 0.0619(13) Uani 1 1 d . . . O1W O 0.6059(3) 0.2118(5) 1.0000 0.0625(19) Uani 1 2 d S . . O3 O 0.8139(4) 0.5787(3) 0.90754(18) 0.0661(15) Uani 1 1 d . . . O4 O 1.2315(15) 0.9148(18) 0.8605(8) 0.227(7) Uani 0.67 1 d PD . . O3W O 0.4292(4) 0.1197(5) 0.9701(2) 0.098(2) Uani 1 1 d . . . O5 O 1.3064(18) 0.8525(15) 0.8828(8) 0.227(7) Uani 0.67 1 d PD . . O2W O 0.9964(8) 0.6042(8) 0.7500 0.134(5) Uani 1 2 d S . . O6 O 1.3764(16) 1.0048(19) 0.8727(10) 0.227(7) Uani 0.67 1 d PD . . O7 O 1.2919(16) 0.9432(17) 0.9285(6) 0.227(7) Uani 0.67 1 d PD . . O8 O 1.0761(11) 0.9922(12) 0.7500 0.173(11) Uani 0.80 2 d SP . . O9 O 1.0000 1.0000 0.7932(6) 0.24(2) Uani 0.80 3 d SPD . . O10 O 1.0447(4) 1.0893(8) 1.0000 0.25(2) Uani 0.80 2 d SPD . . O11 O 1.0000 1.0000 1.0433(6) 0.60(9) Uani 0.80 3 d SPD . . Na1 Na 0.6667 0.3333 0.95171(14) 0.0561(11) Uani 1 3 d S . . Cl1 Cl 1.0000 1.0000 1.0000 0.0724(13) Uani 1 6 d SD . . Cl2 Cl 1.0000 1.0000 0.7500 0.0798(15) Uani 1 6 d SD . . Cl3 Cl 1.3027(3) 0.9331(4) 0.8868(3) 0.139(2) Uani 0.67 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 C1 0.045(4) 0.032(4) 0.059(3) -0.001(3) -0.002(3) 0.016(3) C2 0.041(4) 0.037(4) 0.054(3) 0.000(3) 0.007(3) 0.016(3) C3 0.034(3) 0.033(3) 0.048(3) -0.002(2) 0.002(3) 0.011(2) C4 0.027(4) 0.035(4) 0.052(4) 0.000 0.000 0.012(3) C5 0.042(3) 0.054(4) 0.062(4) -0.001(3) -0.009(3) 0.031(3) C6 0.051(5) 0.055(6) 0.054(5) 0.000 0.000 0.030(5) C7 0.147(15) 0.146(14) 0.25(2) -0.002(16) -0.051(16) 0.101(13) C8 0.28(2) 0.082(8) 0.085(7) 0.025(6) 0.052(11) 0.083(11) C9 0.204(17) 0.066(7) 0.120(10) -0.006(7) 0.032(12) 0.072(10) C10 0.157(14) 0.048(6) 0.133(10) -0.028(6) 0.051(10) 0.014(7) C11 0.177(14) 0.049(5) 0.124(9) -0.030(5) 0.071(10) 0.000(7) C12 0.116(11) 0.123(12) 0.100(8) -0.040(9) -0.018(7) -0.015(9) C13 0.107(10) 0.128(12) 0.107(8) -0.011(9) -0.022(7) -0.019(9) C14 0.088(10) 0.142(16) 0.147(12) 0.025(10) 0.025(8) 0.036(9) C15 0.121(11) 0.115(11) 0.148(11) 0.009(9) -0.027(9) 0.075(9) Cu1 0.0574(6) 0.0362(5) 0.0734(7) -0.0093(4) 0.0094(4) 0.0033(5) N1 0.039(3) 0.032(3) 0.047(2) -0.002(2) -0.004(2) 0.016(2) N2 0.102(7) 0.053(4) 0.103(6) 0.002(4) 0.018(5) 0.036(5) N3 0.100(7) 0.063(5) 0.084(5) -0.019(4) 0.019(5) -0.011(5) N4 0.057(5) 0.105(7) 0.100(6) 0.008(5) -0.003(4) 0.011(4) Ni1 0.0329(5) 0.0329(5) 0.0502(7) 0.000 0.000 0.0165(3) O1 0.044(3) 0.039(3) 0.064(3) 0.000(2) 0.005(2) 0.020(2) O2 0.041(3) 0.034(3) 0.088(3) -0.006(2) 0.013(2) 0.001(2) O1W 0.065(4) 0.052(4) 0.066(4) 0.000 -0.004(3) 0.026(2) O3 0.065(3) 0.042(3) 0.075(3) -0.010(2) 0.014(3) 0.014(3) O4 0.142(10) 0.211(14) 0.246(13) 0.038(10) 0.003(9) 0.027(8) O3W 0.070(4) 0.100(5) 0.105(4) 0.043(4) 0.008(3) 0.029(3) O5 0.142(10) 0.211(14) 0.246(13) 0.038(10) 0.003(9) 0.027(8) O2W 0.092(8) 0.069(7) 0.207(15) 0.000 0.000 0.015(6) O6 0.142(10) 0.211(14) 0.246(13) 0.038(10) 0.003(9) 0.027(8) O7 0.142(10) 0.211(14) 0.246(13) 0.038(10) 0.003(9) 0.027(8) O8 0.068(9) 0.093(11) 0.36(3) 0.000 0.000 0.043(9) O9 0.30(3) 0.30(3) 0.12(3) 0.000 0.000 0.151(17) O10 0.186(18) 0.042(7) 0.47(5) 0.000 0.21(3) 0.021(4) O11 0.85(14) 0.85(14) 0.10(3) 0.000 0.000 0.42(7) Na1 0.0605(17) 0.0605(17) 0.047(2) 0.000 0.000 0.0303(8) Cl1 0.0607(18) 0.0607(18) 0.096(4) 0.000 0.000 0.0303(9) Cl2 0.062(2) 0.062(2) 0.114(5) 0.000 0.000 0.0312(10) Cl3 0.056(3) 0.099(3) 0.220(7) 0.047(4) 0.007(3) 0.008(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.243(9) . ? C1 O3 1.267(9) . ? C1 C2 1.531(10) . ? C2 O2 1.284(9) . ? C2 N1 1.304(9) . ? C3 C4 1.385(8) . ? C3 N1 1.408(8) . ? C3 C5 1.413(10) . ? C4 C3 1.385(8) 2_556 ? C5 C6 1.379(9) . ? C6 C5 1.379(9) 2_556 ? C7 N2 1.51(2) . ? C8 N2 1.48(2) . ? C9 N2 1.490(15) . ? C9 C10 1.56(3) . ? C10 N3 1.479(19) . ? C11 N3 1.516(15) . ? C12 N3 1.49(2) . ? C12 C13 1.50(3) . ? C13 N4 1.465(17) . ? C14 N4 1.447(18) . ? C15 N4 1.423(18) . ? Cu1 O2 1.965(5) . ? Cu1 N3 1.993(8) . ? Cu1 N2 2.049(9) . ? Cu1 N4 2.050(11) . ? Cu1 O3 2.158(6) . ? N1 Ni1 2.062(5) . ? Ni1 N1 2.062(5) 12_665 ? Ni1 N1 2.062(5) 9_655 ? Ni1 O1 2.102(5) 12_665 ? Ni1 O1 2.102(5) . ? Ni1 O1 2.102(5) 9_655 ? Ni1 Na1 3.052(5) . ? O1 Na1 2.387(6) . ? O1W Na1 2.389(7) 3_667 ? O1W Na1 2.389(7) . ? O4 Cl3 1.392(15) . ? O5 Cl3 1.443(16) . ? O6 Cl3 1.344(16) . ? O7 Cl3 1.358(16) . ? O8 Cl2 1.400(16) . ? O9 Cl2 1.367(18) . ? O10 Cl1 1.348(12) . ? O11 Cl1 1.373(19) . ? Na1 O1 2.387(6) 12_665 ? Na1 O1 2.387(6) 9_655 ? Na1 O1W 2.389(7) 3_667 ? Na1 O1W 2.389(7) 7_557 ? Na1 Na1 3.059(9) 3_667 ? Cl1 O10 1.348(12) 7_567 ? Cl1 O10 1.348(12) 3_777 ? Cl1 O11 1.373(19) 3_777 ? Cl2 O9 1.367(18) 2_556 ? Cl2 O8 1.400(16) 11_676 ? Cl2 O8 1.400(16) 9_765 ? 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 C1 O3 125.7(7) . . ? O1 C1 C2 118.5(6) . . ? O3 C1 C2 115.8(6) . . ? O2 C2 N1 126.8(6) . . ? O2 C2 C1 118.5(6) . . ? N1 C2 C1 114.6(6) . . ? C4 C3 N1 120.1(6) . . ? C4 C3 C5 118.3(6) . . ? N1 C3 C5 121.4(6) . . ? C3 C4 C3 122.4(8) . 2_556 ? C6 C5 C3 119.7(6) . . ? C5 C6 C5 121.5(9) . 2_556 ? N2 C9 C10 106.2(13) . . ? N3 C10 C9 107.4(11) . . ? N3 C12 C13 112.8(10) . . ? N4 C13 C12 107.5(13) . . ? O2 Cu1 N3 177.4(3) . . ? O2 Cu1 N2 92.1(3) . . ? N3 Cu1 N2 85.6(4) . . ? O2 Cu1 N4 94.9(4) . . ? N3 Cu1 N4 86.4(5) . . ? N2 Cu1 N4 149.2(4) . . ? O2 Cu1 O3 81.56(19) . . ? N3 Cu1 O3 100.4(3) . . ? N2 Cu1 O3 109.0(3) . . ? N4 Cu1 O3 101.7(3) . . ? C2 N1 C3 120.5(5) . . ? C2 N1 Ni1 113.9(4) . . ? C3 N1 Ni1 125.4(4) . . ? C8 N2 C9 107.6(11) . . ? C8 N2 C7 112.5(15) . . ? C9 N2 C7 109.7(13) . . ? C8 N2 Cu1 107.1(9) . . ? C9 N2 Cu1 108.0(8) . . ? C7 N2 Cu1 111.7(9) . . ? C10 N3 C12 109.4(12) . . ? C10 N3 C11 111.9(11) . . ? C12 N3 C11 110.1(11) . . ? C10 N3 Cu1 108.1(7) . . ? C12 N3 Cu1 105.6(9) . . ? C11 N3 Cu1 111.5(6) . . ? C15 N4 C14 110.0(13) . . ? C15 N4 C13 104.1(11) . . ? C14 N4 C13 110.1(12) . . ? C15 N4 Cu1 115.3(8) . . ? C14 N4 Cu1 108.5(9) . . ? C13 N4 Cu1 108.7(12) . . ? N1 Ni1 N1 101.59(17) 12_665 . ? N1 Ni1 N1 101.59(17) 12_665 9_655 ? N1 Ni1 N1 101.59(17) . 9_655 ? N1 Ni1 O1 79.73(18) 12_665 12_665 ? N1 Ni1 O1 93.0(2) . 12_665 ? N1 Ni1 O1 164.6(2) 9_655 12_665 ? N1 Ni1 O1 164.64(19) 12_665 . ? N1 Ni1 O1 79.73(18) . . ? N1 Ni1 O1 93.0(2) 9_655 . ? O1 Ni1 O1 84.92(19) 12_665 . ? N1 Ni1 O1 93.0(2) 12_665 9_655 ? N1 Ni1 O1 164.64(19) . 9_655 ? N1 Ni1 O1 79.73(18) 9_655 9_655 ? O1 Ni1 O1 84.92(19) 12_665 9_655 ? O1 Ni1 O1 84.92(19) . 9_655 ? N1 Ni1 Na1 116.52(13) 12_665 . ? N1 Ni1 Na1 116.52(14) . . ? N1 Ni1 Na1 116.52(13) 9_655 . ? O1 Ni1 Na1 51.21(13) 12_665 . ? O1 Ni1 Na1 51.21(13) . . ? O1 Ni1 Na1 51.21(13) 9_655 . ? C1 O1 Ni1 112.9(4) . . ? C1 O1 Na1 131.7(4) . . ? Ni1 O1 Na1 85.44(19) . . ? C2 O2 Cu1 113.8(4) . . ? Na1 O1W Na1 79.6(3) 3_667 . ? C1 O3 Cu1 109.7(5) . . ? O1 Na1 O1 72.9(2) 12_665 9_655 ? O1 Na1 O1 72.9(2) 12_665 . ? O1 Na1 O1 72.9(2) 9_655 . ? O1 Na1 O1W 97.28(15) 12_665 3_667 ? O1 Na1 O1W 170.01(18) 9_655 3_667 ? O1 Na1 O1W 106.59(15) . 3_667 ? O1 Na1 O1W 106.59(15) 12_665 . ? O1 Na1 O1W 97.28(16) 9_655 . ? O1 Na1 O1W 170.01(18) . . ? O1W Na1 O1W 83.4(2) 3_667 . ? O1 Na1 O1W 170.01(18) 12_665 7_557 ? O1 Na1 O1W 106.59(15) 9_655 7_557 ? O1 Na1 O1W 97.28(15) . 7_557 ? O1W Na1 O1W 83.4(2) 3_667 7_557 ? O1W Na1 O1W 83.4(2) . 7_557 ? O1 Na1 Ni1 43.35(14) 12_665 . ? O1 Na1 Ni1 43.35(14) 9_655 . ? O1 Na1 Ni1 43.35(14) . . ? O1W Na1 Ni1 129.82(14) 3_667 . ? O1W Na1 Ni1 129.82(14) . . ? O1W Na1 Ni1 129.82(14) 7_557 . ? O1 Na1 Na1 136.65(14) 12_665 3_667 ? O1 Na1 Na1 136.65(14) 9_655 3_667 ? O1 Na1 Na1 136.65(14) . 3_667 ? O1W Na1 Na1 50.18(14) 3_667 3_667 ? O1W Na1 Na1 50.18(14) . 3_667 ? O1W Na1 Na1 50.18(14) 7_557 3_667 ? Ni1 Na1 Na1 180.000(1) . 3_667 ? O10 Cl1 O10 119.999(9) 7_567 . ? O10 Cl1 O10 120.000(5) 7_567 3_777 ? O10 Cl1 O10 120.001(5) . 3_777 ? O10 Cl1 O11 90.000(1) 7_567 3_777 ? O10 Cl1 O11 90.000(6) . 3_777 ? O10 Cl1 O11 90.000(6) 3_777 3_777 ? O10 Cl1 O11 90.000(1) 7_567 . ? O10 Cl1 O11 90.000(6) . . ? O10 Cl1 O11 90.000(6) 3_777 . ? O11 Cl1 O11 180.00(2) 3_777 . ? O9 Cl2 O9 180.000(16) . 2_556 ? O9 Cl2 O8 90.000(11) . . ? O9 Cl2 O8 90.000(11) 2_556 . ? O9 Cl2 O8 90.000(18) . 11_676 ? O9 Cl2 O8 90.000(18) 2_556 11_676 ? O8 Cl2 O8 120.000(8) . 11_676 ? O9 Cl2 O8 90.000(8) . 9_765 ? O9 Cl2 O8 90.000(8) 2_556 9_765 ? O8 Cl2 O8 120.000(9) . 9_765 ? O8 Cl2 O8 120.000(10) 11_676 9_765 ? O6 Cl3 O7 109.4(19) . . ? O6 Cl3 O4 110.1(19) . . ? O7 Cl3 O4 116.4(14) . . ? O6 Cl3 O5 113(2) . . ? O7 Cl3 O5 106.7(13) . . ? O4 Cl3 O5 101.2(12) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.93 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.896 _refine_diff_density_min -0.635 _refine_diff_density_rms 0.146