Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Nelson, Jane' 'Dalgaard, Pia' 'Dussart, Yann' 'Harding, Charlie' 'Kadirvelraj, Renuka' 'McKee, V.' 'McKenzie, C. J.' _publ_contact_author_name 'Dr Jane Nelson' _publ_contact_author_address ; Queen's University of Belfast Belfast Northern Ireland BT9 5AG UK ; _publ_contact_author_email 'JANE.NELSON@QUB.AC.UK' _publ_section_title ; Cascade chemistry in azacryptand cages:bridging carbonates and methylcarbonates ; data_Complex_1 #(y148r) _database_code_CSD 181027 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H64 Cl2 Cu2 N8 O13' _chemical_formula_weight 1026.94 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' 'Cu' 'Cu' 0.3201 1.2651 '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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 19.195(3) _cell_length_b 17.909(3) _cell_length_c 24.650(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8474(2) _cell_formula_units_Z 8 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description octagonal _exptl_crystal_colour green _exptl_crystal_size_max .2 _exptl_crystal_size_mid .38 _exptl_crystal_size_min .4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4304 _exptl_absorpt_coefficient_mu 1.205 _exptl_absorpt_correction_type 'Bruker SADABS' _exptl_absorpt_correction_T_min 1.000000 _exptl_absorpt_correction_T_max 0.780742 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 158(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48784 _diffrn_reflns_av_R_equivalents 0.0666 _diffrn_reflns_av_sigmaI/netI 0.0600 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 23.89 _reflns_number_total 6520 _reflns_number_gt 4451 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0491P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6520 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0841 _refine_ls_wR_factor_gt 0.0792 _refine_ls_goodness_of_fit_ref 0.911 _refine_ls_restrained_S_all 0.911 _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 Cu1 Cu 0.05129(2) 0.01696(2) 0.175879(15) 0.01982(12) Uani 1 1 d . . . Cu2 Cu 0.21906(2) -0.08342(2) -0.005252(15) 0.01986(12) Uani 1 1 d . . . N1 N -0.01858(15) 0.04070(14) 0.23624(10) 0.0217(7) Uani 1 1 d . . . C1A C 0.02079(19) 0.05134(19) 0.28762(13) 0.0257(9) Uani 1 1 d . . . H1A1 H -0.0100 0.0398 0.3187 0.031 Uiso 1 1 calc R . . H1A2 H 0.0351 0.1043 0.2907 0.031 Uiso 1 1 calc R . . C2A C 0.08456(19) 0.00225(19) 0.29038(13) 0.0249(9) Uani 1 1 d . . . H2A1 H 0.1112 0.0135 0.3238 0.030 Uiso 1 1 calc R . . H2A2 H 0.0703 -0.0509 0.2916 0.030 Uiso 1 1 calc R . . N3A N 0.12845(15) 0.01543(15) 0.24275(10) 0.0230(7) Uani 1 1 d . . . H3A1 H 0.1438 0.0641 0.2432 0.028 Uiso 1 1 calc R . . H3A2 H 0.1022 0.0088 0.2119 0.028 Uiso 1 1 calc R . . C3A C 0.18945(19) -0.03518(19) 0.24079(13) 0.0252(9) Uani 1 1 d . . . H3A1' H 0.1730 -0.0865 0.2332 0.030 Uiso 1 1 calc R . . H3A2' H 0.2120 -0.0356 0.2769 0.030 Uiso 1 1 calc R . . C4A C 0.24301(18) -0.01393(18) 0.19872(13) 0.0206(8) Uani 1 1 d . . . C5A C 0.26806(19) 0.05863(19) 0.19457(14) 0.0252(9) Uani 1 1 d . . . H5A H 0.2515 0.0960 0.2187 0.030 Uiso 1 1 calc R . . C6A C 0.3170(2) 0.07691(19) 0.15553(14) 0.0273(9) Uani 1 1 d . . . H6A H 0.3336 0.1268 0.1530 0.033 Uiso 1 1 calc R . . C7A C 0.34214(19) 0.02282(19) 0.11999(13) 0.0253(9) Uani 1 1 d . . . H7A H 0.3760 0.0356 0.0935 0.030 Uiso 1 1 calc R . . C8A C 0.31741(19) -0.05023(18) 0.12346(13) 0.0220(8) Uani 1 1 d . . . C9A C 0.26893(18) -0.06739(18) 0.16312(13) 0.0225(8) Uani 1 1 d . . . H9A H 0.2528 -0.1174 0.1661 0.027 Uiso 1 1 calc R . . C10A C 0.34359(19) -0.10923(18) 0.08462(13) 0.0239(9) Uani 1 1 d . . . H10A H 0.3947 -0.1136 0.0886 0.029 Uiso 1 1 calc R . . H10B H 0.3228 -0.1579 0.0947 0.029 Uiso 1 1 calc R . . N4A N 0.32710(15) -0.09353(14) 0.02681(10) 0.0207(7) Uani 1 1 d . . . H4A1 H 0.2795 -0.0921 0.0223 0.025 Uiso 1 1 calc R . . H4A2 H 0.3447 -0.0475 0.0174 0.025 Uiso 1 1 calc R . . C11A C 0.35691(19) -0.15102(18) -0.00915(13) 0.0242(8) Uani 1 1 d . . . H11A H 0.3410 -0.2010 0.0028 0.029 Uiso 1 1 calc R . . H11B H 0.4084 -0.1497 -0.0067 0.029 Uiso 1 1 calc R . . C12A C 0.33499(18) -0.13817(19) -0.06709(13) 0.0238(9) Uani 1 1 d . . . H12A H 0.3550 -0.0905 -0.0802 0.029 Uiso 1 1 calc R . . H12B H 0.3533 -0.1789 -0.0902 0.029 Uiso 1 1 calc R . . N2 N 0.25802(15) -0.13545(14) -0.07191(10) 0.0205(7) Uani 1 1 d . . . C1B C -0.06834(19) -0.02292(18) 0.24039(14) 0.0252(9) Uani 1 1 d . . . H1B1 H -0.1143 -0.0047 0.2530 0.030 Uiso 1 1 calc R . . H1B2 H -0.0509 -0.0599 0.2669 0.030 Uiso 1 1 calc R . . C2B C -0.07563(19) -0.05902(19) 0.18506(14) 0.0266(9) Uani 1 1 d . . . H2B1 H -0.1071 -0.1027 0.1873 0.032 Uiso 1 1 calc R . . H2B2 H -0.0955 -0.0230 0.1589 0.032 Uiso 1 1 calc R . . N3B N -0.00609(15) -0.08254(14) 0.16733(10) 0.0217(7) Uani 1 1 d . . . H3B1 H 0.0247 -0.0441 0.1733 0.026 Uiso 1 1 calc R . . H3B2 H -0.0072 -0.0915 0.1306 0.026 Uiso 1 1 calc R . . C3B C 0.0201(2) -0.15128(17) 0.19569(13) 0.0276(9) Uani 1 1 d . . . H3B1' H -0.0168 -0.1712 0.2197 0.033 Uiso 1 1 calc R . . H3B2' H 0.0608 -0.1382 0.2185 0.033 Uiso 1 1 calc R . . C4B C 0.04091(19) -0.21040(17) 0.15487(13) 0.0222(9) Uani 1 1 d . . . C5B C -0.00056(19) -0.27245(17) 0.14488(13) 0.0236(8) Uani 1 1 d . . . H5B H -0.0420 -0.2798 0.1653 0.028 Uiso 1 1 calc R . . C6B C 0.01817(19) -0.32386(17) 0.10517(13) 0.0230(8) Uani 1 1 d . . . H6B H -0.0096 -0.3670 0.0993 0.028 Uiso 1 1 calc R . . C7B C 0.07729(19) -0.31216(17) 0.07432(13) 0.0232(9) Uani 1 1 d . . . H7B H 0.0894 -0.3468 0.0467 0.028 Uiso 1 1 calc R . . C8B C 0.11918(18) -0.24991(18) 0.08350(13) 0.0227(8) Uani 1 1 d . . . C9B C 0.10135(19) -0.20071(17) 0.12460(13) 0.0240(9) Uani 1 1 d . . . H9B H 0.1310 -0.1596 0.1323 0.029 Uiso 1 1 calc R . . C10B C 0.17960(19) -0.23134(19) 0.04743(14) 0.0294(9) Uani 1 1 d . . . H10C H 0.1983 -0.2777 0.0311 0.035 Uiso 1 1 calc R . . H10D H 0.2171 -0.2080 0.0692 0.035 Uiso 1 1 calc R . . N4B N 0.15720(15) -0.17873(14) 0.00327(10) 0.0222(7) Uani 1 1 d . . . H4B1 H 0.1136 -0.1607 0.0116 0.027 Uiso 1 1 calc R . . H4B2 H 0.1873 -0.1388 0.0028 0.027 Uiso 1 1 calc R . . C11B C 0.1549(2) -0.21157(19) -0.05123(14) 0.0283(9) Uani 1 1 d . . . H11C H 0.1239 -0.1818 -0.0749 0.034 Uiso 1 1 calc R . . H11D H 0.1365 -0.2631 -0.0494 0.034 Uiso 1 1 calc R . . C12B C 0.22768(19) -0.21222(18) -0.07405(14) 0.0262(9) Uani 1 1 d . . . H12C H 0.2571 -0.2469 -0.0528 0.031 Uiso 1 1 calc R . . H12D H 0.2266 -0.2299 -0.1121 0.031 Uiso 1 1 calc R . . C1C C -0.0554(2) 0.11087(18) 0.22011(14) 0.0270(9) Uani 1 1 d . . . H1C1 H -0.0775 0.1338 0.2524 0.032 Uiso 1 1 calc R . . H1C2 H -0.0924 0.0991 0.1935 0.032 Uiso 1 1 calc R . . C2C C -0.0041(2) 0.16521(17) 0.19534(14) 0.0277(9) Uani 1 1 d . . . H2C1 H -0.0291 0.2098 0.1818 0.033 Uiso 1 1 calc R . . H2C2 H 0.0299 0.1815 0.2231 0.033 Uiso 1 1 calc R . . N3C N 0.03274(15) 0.12778(14) 0.14979(11) 0.0244(7) Uani 1 1 d . . . H3C1 H 0.0019 0.1204 0.1217 0.029 Uiso 1 1 calc R . . H3C2 H 0.0481 0.0817 0.1612 0.029 Uiso 1 1 calc R . . C3C C 0.0934(2) 0.17179(19) 0.12958(13) 0.0275(9) Uani 1 1 d . . . H3C1' H 0.1365 0.1537 0.1473 0.033 Uiso 1 1 calc R . . H3C2' H 0.0871 0.2250 0.1394 0.033 Uiso 1 1 calc R . . C4C C 0.10108(19) 0.16501(17) 0.06877(13) 0.0204(8) Uani 1 1 d . . . C5C C 0.0482(2) 0.19102(17) 0.03542(14) 0.0245(9) Uani 1 1 d . . . H5C H 0.0083 0.2140 0.0509 0.029 Uiso 1 1 calc R . . C6C C 0.0533(2) 0.18369(17) -0.02038(14) 0.0238(8) Uani 1 1 d . . . H6C H 0.0168 0.2011 -0.0431 0.029 Uiso 1 1 calc R . . C7C C 0.11190(19) 0.15075(17) -0.04285(14) 0.0243(9) Uani 1 1 d . . . H7C H 0.1159 0.1467 -0.0812 0.029 Uiso 1 1 calc R . . C8C C 0.16475(18) 0.12370(17) -0.01009(14) 0.0214(8) Uani 1 1 d . . . C9C C 0.15880(19) 0.13159(17) 0.04586(14) 0.0217(8) Uani 1 1 d . . . H9C H 0.1950 0.1137 0.0687 0.026 Uiso 1 1 calc R . . C10C C 0.22575(19) 0.08495(17) -0.03584(15) 0.0272(9) Uani 1 1 d . . . H10E H 0.2438 0.1160 -0.0659 0.033 Uiso 1 1 calc R . . H10F H 0.2634 0.0794 -0.0087 0.033 Uiso 1 1 calc R . . N4C N 0.20636(15) 0.00993(13) -0.05719(10) 0.0200(7) Uani 1 1 d . . . H4C1 H 0.2166 -0.0256 -0.0315 0.024 Uiso 1 1 calc R . . H4C2 H 0.1591 0.0086 -0.0633 0.024 Uiso 1 1 calc R . . C11C C 0.2431(2) -0.00859(18) -0.10791(13) 0.0257(9) Uani 1 1 d . . . H11E H 0.2931 0.0043 -0.1045 0.031 Uiso 1 1 calc R . . H11F H 0.2233 0.0207 -0.1383 0.031 Uiso 1 1 calc R . . C12C C 0.23553(19) -0.09083(18) -0.11944(13) 0.0256(9) Uani 1 1 d . . . H12E H 0.1863 -0.1023 -0.1280 0.031 Uiso 1 1 calc R . . H12F H 0.2642 -0.1043 -0.1514 0.031 Uiso 1 1 calc R . . C1 C 0.1233(2) -0.03024(17) 0.07660(13) 0.0197(8) Uani 1 1 d . . . O1 O 0.12110(12) -0.00083(11) 0.12446(8) 0.0224(6) Uani 1 1 d . . . O2 O 0.18523(13) -0.03606(11) 0.05725(8) 0.0219(6) Uani 1 1 d . . . O3 O 0.06872(12) -0.05184(12) 0.05186(9) 0.0237(6) Uani 1 1 d . . . Cl1 Cl 0.18456(6) 0.25310(5) 0.26746(4) 0.0379(3) Uani 1 1 d . . . O11 O 0.13473(17) 0.29231(15) 0.23475(11) 0.0519(8) Uani 1 1 d . . . O12 O 0.24872(18) 0.24683(17) 0.23995(17) 0.0856(12) Uani 1 1 d . . . O13 O 0.19307(19) 0.29279(15) 0.31727(12) 0.0667(10) Uani 1 1 d . . . O14 O 0.15826(15) 0.17960(14) 0.27889(11) 0.0476(8) Uani 1 1 d . . . Cl2 Cl 0.43607(5) 0.42358(5) 0.43403(4) 0.0358(3) Uani 1 1 d . . . O21 O 0.38420(16) 0.39505(15) 0.39635(12) 0.0533(8) Uani 1 1 d . . . O22 O 0.47502(17) 0.48078(17) 0.40881(12) 0.0667(10) Uani 1 1 d . . . O23 O 0.47840(15) 0.36286(15) 0.45047(12) 0.0548(8) Uani 1 1 d . . . O24 O 0.39917(17) 0.45376(16) 0.47964(12) 0.0597(9) Uani 1 1 d . . . O1W O 0.05272(13) -0.03515(12) -0.06103(9) 0.0276(6) Uani 1 1 d . . . H1WA H 0.0166 -0.0094 -0.0565 0.050 Uiso 1 1 d R . . H1WB H 0.0551 -0.0403 -0.0272 0.050 Uiso 1 1 d R . . O2W O 0.3728(2) 0.2883(2) 0.30845(16) 0.1005(14) Uani 1 1 d . . . H2WA H 0.3394 0.2768 0.2896 0.050 Uiso 1 1 d R . . H2WB H 0.3763 0.3185 0.3334 0.050 Uiso 1 1 d 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 Cu1 0.0245(3) 0.0190(2) 0.0161(2) -0.00112(17) 0.0018(2) 0.0001(2) Cu2 0.0229(3) 0.0179(2) 0.0188(2) -0.00150(17) 0.0028(2) 0.00103(19) N1 0.0255(18) 0.0221(15) 0.0176(16) -0.0018(12) 0.0026(14) 0.0012(13) C1A 0.033(2) 0.0278(19) 0.0158(19) -0.0047(15) 0.0050(18) -0.0032(18) C2A 0.029(2) 0.031(2) 0.0148(18) -0.0002(15) 0.0017(17) -0.0029(17) N3A 0.0290(19) 0.0255(16) 0.0146(15) -0.0008(12) -0.0037(14) -0.0016(14) C3A 0.026(2) 0.031(2) 0.0193(19) 0.0008(15) -0.0038(17) 0.0043(17) C4A 0.019(2) 0.028(2) 0.0148(17) 0.0023(15) -0.0052(16) 0.0004(16) C5A 0.027(2) 0.027(2) 0.0219(19) -0.0050(15) -0.0028(17) 0.0009(17) C6A 0.032(2) 0.0218(19) 0.028(2) 0.0008(16) -0.0015(19) -0.0047(17) C7A 0.022(2) 0.030(2) 0.024(2) 0.0001(16) 0.0010(17) -0.0012(17) C8A 0.023(2) 0.0237(19) 0.0196(19) 0.0001(15) -0.0056(17) 0.0031(16) C9A 0.023(2) 0.0222(19) 0.0228(19) 0.0045(15) -0.0060(17) -0.0001(16) C10A 0.023(2) 0.0264(19) 0.023(2) -0.0020(15) -0.0041(17) 0.0012(17) N4A 0.0149(17) 0.0214(15) 0.0258(16) -0.0009(12) -0.0013(13) 0.0011(13) C11A 0.022(2) 0.0219(18) 0.029(2) -0.0058(16) 0.0009(18) 0.0047(16) C12A 0.021(2) 0.0239(19) 0.026(2) -0.0033(15) 0.0059(17) 0.0015(16) N2 0.0233(19) 0.0189(15) 0.0194(15) -0.0004(12) 0.0029(13) 0.0015(13) C1B 0.027(2) 0.0231(19) 0.025(2) -0.0001(15) 0.0066(17) -0.0010(17) C2B 0.028(2) 0.0249(19) 0.027(2) -0.0002(16) 0.0006(18) -0.0030(17) N3B 0.0268(19) 0.0194(14) 0.0190(15) -0.0036(12) -0.0002(14) -0.0051(14) C3B 0.042(3) 0.0203(19) 0.0201(19) 0.0022(15) 0.0037(18) -0.0003(17) C4B 0.032(3) 0.0162(18) 0.0189(18) 0.0064(14) 0.0000(18) 0.0028(16) C5B 0.026(2) 0.0215(18) 0.024(2) 0.0084(15) 0.0020(17) -0.0003(17) C6B 0.030(2) 0.0140(17) 0.024(2) 0.0044(15) -0.0047(18) -0.0049(16) C7B 0.036(3) 0.0156(18) 0.0182(19) 0.0018(14) -0.0040(18) 0.0061(17) C8B 0.023(2) 0.0222(19) 0.0228(19) 0.0073(16) -0.0032(16) 0.0048(17) C9B 0.031(2) 0.0142(18) 0.026(2) 0.0033(15) -0.0067(19) -0.0022(16) C10B 0.030(2) 0.0244(19) 0.034(2) 0.0064(16) 0.0047(19) 0.0042(18) N4B 0.0188(17) 0.0194(14) 0.0285(17) 0.0002(13) 0.0048(14) -0.0032(13) C11B 0.032(3) 0.0239(19) 0.029(2) -0.0040(16) 0.0009(19) -0.0073(17) C12B 0.032(3) 0.0202(18) 0.027(2) -0.0088(15) 0.0015(18) -0.0026(17) C1C 0.030(2) 0.0258(19) 0.025(2) -0.0003(16) 0.0023(18) 0.0070(18) C2C 0.040(3) 0.0195(18) 0.024(2) -0.0019(15) 0.0061(18) 0.0040(18) N3C 0.035(2) 0.0163(15) 0.0222(16) 0.0019(12) 0.0014(14) 0.0025(13) C3C 0.033(2) 0.0227(19) 0.027(2) -0.0002(16) 0.0010(19) -0.0061(17) C4C 0.024(2) 0.0136(17) 0.023(2) 0.0028(15) -0.0008(17) -0.0040(16) C5C 0.026(2) 0.0154(17) 0.032(2) 0.0016(15) 0.0077(19) 0.0011(16) C6C 0.026(2) 0.0169(17) 0.028(2) 0.0044(15) -0.0046(18) 0.0001(17) C7C 0.035(3) 0.0188(18) 0.0186(19) -0.0020(15) -0.0009(18) -0.0052(17) C8C 0.023(2) 0.0108(16) 0.031(2) -0.0001(15) 0.0031(18) -0.0031(15) C9C 0.024(2) 0.0162(18) 0.025(2) 0.0053(15) -0.0026(17) -0.0031(16) C10C 0.026(2) 0.0184(18) 0.038(2) -0.0018(16) 0.0038(18) -0.0028(17) N4C 0.0251(18) 0.0152(14) 0.0197(15) 0.0031(12) 0.0018(14) 0.0013(13) C11C 0.031(2) 0.0251(19) 0.0207(19) 0.0013(16) 0.0063(18) 0.0039(17) C12C 0.026(2) 0.030(2) 0.0208(19) -0.0011(16) 0.0016(17) 0.0008(17) C1 0.030(3) 0.0120(18) 0.0173(19) 0.0062(14) -0.0008(18) 0.0036(16) O1 0.0245(15) 0.0262(13) 0.0166(13) -0.0042(10) 0.0013(11) 0.0013(11) O2 0.0211(15) 0.0232(13) 0.0213(13) -0.0044(10) 0.0030(12) 0.0027(11) O3 0.0214(16) 0.0282(13) 0.0216(13) -0.0021(10) -0.0031(12) 0.0007(11) Cl1 0.0362(7) 0.0298(5) 0.0476(6) -0.0082(5) 0.0018(5) 0.0001(5) O11 0.072(2) 0.0455(18) 0.0382(17) 0.0006(13) -0.0163(16) 0.0088(16) O12 0.050(2) 0.059(2) 0.147(4) -0.009(2) 0.045(2) -0.0007(19) O13 0.091(3) 0.0455(18) 0.063(2) -0.0224(16) -0.041(2) 0.0197(18) O14 0.058(2) 0.0273(15) 0.0571(19) 0.0018(13) 0.0078(16) -0.0024(14) Cl2 0.0358(6) 0.0336(5) 0.0380(6) 0.0147(4) 0.0022(5) 0.0040(5) O21 0.052(2) 0.0535(19) 0.0543(19) 0.0053(15) -0.0131(17) -0.0094(16) O22 0.070(3) 0.069(2) 0.061(2) 0.0348(17) -0.0105(19) -0.0335(19) O23 0.047(2) 0.0557(18) 0.061(2) 0.0207(15) 0.0091(17) 0.0266(16) O24 0.067(2) 0.0564(19) 0.055(2) -0.0053(16) 0.0132(18) 0.0228(18) O1W 0.0290(16) 0.0324(14) 0.0213(13) -0.0018(10) 0.0026(12) 0.0042(12) O2W 0.075(3) 0.115(3) 0.112(3) -0.032(3) -0.017(3) 0.022(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 Cu1 O1 1.872(2) . ? Cu1 N1 2.048(3) . ? Cu1 N3B 2.105(3) . ? Cu1 N3C 2.116(3) . ? Cu1 N3A 2.216(3) . ? Cu1 Cu2 5.7911(8) . ? Cu2 O2 1.875(2) . ? Cu2 N2 2.032(3) . ? Cu2 N4B 2.090(3) . ? Cu2 N4C 2.120(3) . ? Cu2 N4A 2.227(3) . ? N1 C1A 1.487(4) . ? N1 C1B 1.490(4) . ? N1 C1C 1.495(4) . ? C1A C2A 1.509(5) . ? C2A N3A 1.464(4) . ? N3A C3A 1.481(4) . ? C3A C4A 1.509(5) . ? C4A C5A 1.389(5) . ? C4A C9A 1.391(5) . ? C5A C6A 1.384(5) . ? C6A C7A 1.392(5) . ? C7A C8A 1.394(5) . ? C8A C9A 1.384(5) . ? C8A C10A 1.512(4) . ? C10A N4A 1.487(4) . ? N4A C11A 1.474(4) . ? C11A C12A 1.507(4) . ? C12A N2 1.483(4) . ? N2 C12C 1.482(4) . ? N2 C12B 1.494(4) . ? C1B C2B 1.516(5) . ? C2B N3B 1.466(4) . ? N3B C3B 1.503(4) . ? C3B C4B 1.514(4) . ? C4B C5B 1.389(4) . ? C4B C9B 1.390(5) . ? C5B C6B 1.391(5) . ? C6B C7B 1.382(5) . ? C7B C8B 1.393(5) . ? C8B C9B 1.386(5) . ? C8B C10B 1.499(5) . ? C10B N4B 1.503(4) . ? N4B C11B 1.467(4) . ? C11B C12B 1.506(5) . ? C1C C2C 1.512(5) . ? C2C N3C 1.487(4) . ? N3C C3C 1.492(4) . ? C3C C4C 1.511(4) . ? C4C C9C 1.380(5) . ? C4C C5C 1.387(5) . ? C5C C6C 1.385(5) . ? C6C C7C 1.386(5) . ? C7C C8C 1.384(5) . ? C8C C9C 1.391(5) . ? C8C C10C 1.502(5) . ? C10C N4C 1.490(4) . ? N4C C11C 1.474(4) . ? C11C C12C 1.507(4) . ? C1 O3 1.273(4) . ? C1 O2 1.284(4) . ? C1 O1 1.293(4) . ? Cl1 O12 1.410(3) . ? Cl1 O13 1.428(3) . ? Cl1 O11 1.435(3) . ? Cl1 O14 1.438(3) . ? Cl2 O22 1.412(3) . ? Cl2 O23 1.417(3) . ? Cl2 O24 1.434(3) . ? Cl2 O21 1.454(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 O1 Cu1 N1 175.01(11) . . ? O1 Cu1 N3B 99.37(10) . . ? N1 Cu1 N3B 84.59(11) . . ? O1 Cu1 N3C 94.26(10) . . ? N1 Cu1 N3C 85.17(10) . . ? N3B Cu1 N3C 132.47(11) . . ? O1 Cu1 N3A 91.32(10) . . ? N1 Cu1 N3A 84.25(11) . . ? N3B Cu1 N3A 114.44(10) . . ? N3C Cu1 N3A 110.48(11) . . ? O1 Cu1 Cu2 13.35(7) . . ? N1 Cu1 Cu2 171.43(8) . . ? N3B Cu1 Cu2 87.20(7) . . ? N3C Cu1 Cu2 98.65(7) . . ? N3A Cu1 Cu2 101.42(7) . . ? O2 Cu2 N2 178.50(11) . . ? O2 Cu2 N4B 95.17(10) . . ? N2 Cu2 N4B 85.17(11) . . ? O2 Cu2 N4C 95.73(9) . . ? N2 Cu2 N4C 85.16(10) . . ? N4B Cu2 N4C 129.76(11) . . ? O2 Cu2 N4A 93.88(10) . . ? N2 Cu2 N4A 84.66(10) . . ? N4B Cu2 N4A 115.28(10) . . ? N4C Cu2 N4A 112.68(10) . . ? O2 Cu2 Cu1 14.84(7) . . ? N2 Cu2 Cu1 166.08(8) . . ? N4B Cu2 Cu1 81.96(7) . . ? N4C Cu2 Cu1 99.03(7) . . ? N4A Cu2 Cu1 105.64(7) . . ? C1A N1 C1B 111.4(2) . . ? C1A N1 C1C 111.0(3) . . ? C1B N1 C1C 111.0(3) . . ? C1A N1 Cu1 108.2(2) . . ? C1B N1 Cu1 108.11(19) . . ? C1C N1 Cu1 106.88(19) . . ? N1 C1A C2A 112.1(3) . . ? N3A C2A C1A 109.7(3) . . ? C2A N3A C3A 112.5(3) . . ? C2A N3A Cu1 102.3(2) . . ? C3A N3A Cu1 120.8(2) . . ? N3A C3A C4A 114.0(3) . . ? C5A C4A C9A 118.3(3) . . ? C5A C4A C3A 121.5(3) . . ? C9A C4A C3A 120.3(3) . . ? C6A C5A C4A 120.5(3) . . ? C5A C6A C7A 120.5(3) . . ? C6A C7A C8A 119.8(3) . . ? C9A C8A C7A 118.7(3) . . ? C9A C8A C10A 121.0(3) . . ? C7A C8A C10A 120.3(3) . . ? C8A C9A C4A 122.2(3) . . ? N4A C10A C8A 113.8(3) . . ? C11A N4A C10A 111.2(2) . . ? C11A N4A Cu2 101.83(19) . . ? C10A N4A Cu2 123.6(2) . . ? N4A C11A C12A 110.8(3) . . ? N2 C12A C11A 111.1(3) . . ? C12C N2 C12A 111.8(3) . . ? C12C N2 C12B 110.8(3) . . ? C12A N2 C12B 111.2(3) . . ? C12C N2 Cu2 106.54(19) . . ? C12A N2 Cu2 108.5(2) . . ? C12B N2 Cu2 107.9(2) . . ? N1 C1B C2B 108.9(3) . . ? N3B C2B C1B 107.9(3) . . ? C2B N3B C3B 113.7(3) . . ? C2B N3B Cu1 101.73(18) . . ? C3B N3B Cu1 118.1(2) . . ? N3B C3B C4B 110.6(3) . . ? C5B C4B C9B 118.9(3) . . ? C5B C4B C3B 121.8(3) . . ? C9B C4B C3B 119.3(3) . . ? C4B C5B C6B 120.4(3) . . ? C7B C6B C5B 119.9(3) . . ? C6B C7B C8B 120.4(3) . . ? C9B C8B C7B 119.0(3) . . ? C9B C8B C10B 118.9(3) . . ? C7B C8B C10B 121.9(3) . . ? C8B C9B C4B 121.3(3) . . ? C8B C10B N4B 110.3(3) . . ? C11B N4B C10B 114.9(3) . . ? C11B N4B Cu2 104.61(19) . . ? C10B N4B Cu2 115.0(2) . . ? N4B C11B C12B 108.5(3) . . ? N2 C12B C11B 110.0(3) . . ? N1 C1C C2C 110.0(3) . . ? N3C C2C C1C 108.9(3) . . ? C2C N3C C3C 112.7(3) . . ? C2C N3C Cu1 105.87(19) . . ? C3C N3C Cu1 117.7(2) . . ? N3C C3C C4C 111.4(3) . . ? C9C C4C C5C 119.4(3) . . ? C9C C4C C3C 121.3(3) . . ? C5C C4C C3C 119.3(3) . . ? C6C C5C C4C 120.3(3) . . ? C5C C6C C7C 119.6(3) . . ? C8C C7C C6C 120.7(3) . . ? C7C C8C C9C 118.9(3) . . ? C7C C8C C10C 119.1(3) . . ? C9C C8C C10C 122.0(3) . . ? C4C C9C C8C 121.1(3) . . ? N4C C10C C8C 111.8(3) . . ? C11C N4C C10C 112.5(3) . . ? C11C N4C Cu2 106.25(19) . . ? C10C N4C Cu2 118.0(2) . . ? N4C C11C C12C 109.5(3) . . ? N2 C12C C11C 110.5(3) . . ? O3 C1 O2 124.0(3) . . ? O3 C1 O1 122.3(3) . . ? O2 C1 O1 113.7(3) . . ? C1 O1 Cu1 135.3(2) . . ? C1 O2 Cu2 131.5(2) . . ? O12 Cl1 O13 110.7(2) . . ? O12 Cl1 O11 110.5(2) . . ? O13 Cl1 O11 108.42(17) . . ? O12 Cl1 O14 109.14(18) . . ? O13 Cl1 O14 109.11(18) . . ? O11 Cl1 O14 108.91(18) . . ? O22 Cl2 O23 112.3(2) . . ? O22 Cl2 O24 109.5(2) . . ? O23 Cl2 O24 110.38(18) . . ? O22 Cl2 O21 109.64(18) . . ? O23 Cl2 O21 107.79(18) . . ? O24 Cl2 O21 107.1(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3A H3A1 O14 0.92 2.26 3.125(4) 155.4 . N4A H4A2 O24 0.92 1.98 2.864(4) 160.8 ? N3C H3C1 O1W 0.92 2.38 3.198(4) 148.0 5 N4C H4C2 O1W 0.92 2.19 3.059(4) 157.7 . O1W H1WA O3 0.84 1.97 2.813(3) 175.7 5 O1W H1WB O3 0.84 1.98 2.816(3) 175.5 . O2W H2WA O12 0.82 2.19 3.013(6) 179.2 . O2W H2WB O21 0.82 2.08 2.898(5) 179.6 . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 23.89 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.545 _refine_diff_density_min -0.590 _refine_diff_density_rms 0.069 data_complex_2 #(r3bmoh) _database_code_CSD 181028 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41.60 H68.40 Cl3 Cu2 N8.60 O17.40' _chemical_formula_weight 1200.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0015 0.0009 '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' 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.0390 0.0740 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.1970 0.6350 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n 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 12.4559(5) _cell_length_b 30.8743(13) _cell_length_c 13.8395(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.0390(10) _cell_angle_gamma 90.00 _cell_volume 5139.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 27965 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 20.27 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2506 _exptl_absorpt_coefficient_mu 0.561 _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 153(2) _diffrn_radiation_wavelength 0.48480 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37650 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0531 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 19.00 _reflns_number_total 12995 _reflns_number_gt 10369 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SHELXTL' _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. The cation is fully ordered but two of the perchlorate anions are disordered and the solvate acetonitrile is disordered 60:40 with a methanol molecule at the same site. The hydrogen atoms on the methanol molecules were not located or included in the model. ; _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^)+(0.0407P)^2^+12.4708P] 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 12995 _refine_ls_number_parameters 717 _refine_ls_number_restraints 106 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_gt 0.0660 _refine_ls_wR_factor_ref 0.1448 _refine_ls_wR_factor_gt 0.1392 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.178 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.001 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 Cu1 Cu 0.79714(4) 0.160873(14) 0.44170(3) 0.02295(11) Uani 1 1 d . . . Cu2 Cu 0.74408(3) 0.079704(13) 0.79273(3) 0.01939(10) Uani 1 1 d . . . N1 N 0.8185(3) 0.18207(10) 0.3083(2) 0.0268(6) Uani 1 1 d . . . C1A C 0.7447(3) 0.15717(13) 0.2257(3) 0.0297(8) Uani 1 1 d . . . H1A1 H 0.7740 0.1584 0.1658 0.036 Uiso 1 1 calc R . . H1A2 H 0.6695 0.1702 0.2083 0.036 Uiso 1 1 calc R . . C2A C 0.7378(3) 0.11077(12) 0.2567(3) 0.0288(8) Uani 1 1 d . . . H2A1 H 0.6864 0.0946 0.2020 0.035 Uiso 1 1 calc R . . H2A2 H 0.8121 0.0971 0.2695 0.035 Uiso 1 1 calc R . . N3A N 0.6972(3) 0.10860(10) 0.3486(2) 0.0235(6) Uani 1 1 d . . . H3A H 0.7195 0.0822 0.3798 0.028 Uiso 1 1 calc R . . C3A C 0.5750(3) 0.11050(13) 0.3234(3) 0.0259(7) Uani 1 1 d . . . H3A1 H 0.5448 0.0916 0.2649 0.031 Uiso 1 1 calc R . . H3A2 H 0.5511 0.1405 0.3035 0.031 Uiso 1 1 calc R . . C4A C 0.5258(3) 0.09705(11) 0.4066(3) 0.0215(7) Uani 1 1 d . . . C5A C 0.4176(3) 0.10945(14) 0.4029(3) 0.0303(8) Uani 1 1 d . . . H5A H 0.3785 0.1280 0.3509 0.036 Uiso 1 1 calc R . . C6A C 0.3664(3) 0.09496(15) 0.4742(3) 0.0342(9) Uani 1 1 d . . . H6A H 0.2925 0.1038 0.4708 0.041 Uiso 1 1 calc R . . C7A C 0.4212(3) 0.06782(13) 0.5503(3) 0.0290(8) Uani 1 1 d . . . H7A H 0.3854 0.0581 0.5992 0.035 Uiso 1 1 calc R . . C8A C 0.5290(3) 0.05478(11) 0.5549(2) 0.0214(7) Uani 1 1 d . . . C9A C 0.5805(3) 0.06986(11) 0.4836(2) 0.0215(7) Uani 1 1 d . . . H9A H 0.6548 0.0614 0.4876 0.026 Uiso 1 1 calc R . . C10A C 0.5879(3) 0.02135(11) 0.6296(2) 0.0229(7) Uani 1 1 d . . . H10A H 0.5416 -0.0051 0.6214 0.027 Uiso 1 1 calc R . . H10B H 0.6590 0.0137 0.6144 0.027 Uiso 1 1 calc R . . N4A N 0.6114(2) 0.03568(9) 0.7346(2) 0.0200(6) Uani 1 1 d . . . H4A H 0.5465 0.0473 0.7453 0.024 Uiso 1 1 calc R . . C11A C 0.6450(3) -0.00174(12) 0.8025(3) 0.0261(7) Uani 1 1 d . . . H11A H 0.7121 -0.0156 0.7905 0.031 Uiso 1 1 calc R . . H11B H 0.5845 -0.0235 0.7899 0.031 Uiso 1 1 calc R . . C12A C 0.6690(3) 0.01413(12) 0.9086(3) 0.0275(8) Uani 1 1 d . . . H12A H 0.5996 0.0249 0.9224 0.033 Uiso 1 1 calc R . . H12B H 0.6974 -0.0101 0.9551 0.033 Uiso 1 1 calc R . . N2 N 0.7528(3) 0.04951(10) 0.9252(2) 0.0229(6) Uani 1 1 d . . . C1B C 0.7902(4) 0.22871(13) 0.3014(3) 0.0337(9) Uani 1 1 d . . . H1B1 H 0.7783 0.2386 0.2314 0.040 Uiso 1 1 calc R . . H1B2 H 0.8524 0.2456 0.3437 0.040 Uiso 1 1 calc R . . C2B C 0.6869(4) 0.23605(13) 0.3355(3) 0.0357(9) Uani 1 1 d . . . H2B1 H 0.6734 0.2675 0.3395 0.043 Uiso 1 1 calc R . . H2B2 H 0.6222 0.2231 0.2869 0.043 Uiso 1 1 calc R . . N3B N 0.7001(3) 0.21596(10) 0.4350(2) 0.0273(7) Uani 1 1 d . . . H3B H 0.7446 0.2352 0.4797 0.033 Uiso 1 1 calc R . . C3B C 0.5919(3) 0.21565(14) 0.4627(3) 0.0330(9) Uani 1 1 d . . . H3B1 H 0.5518 0.1885 0.4380 0.040 Uiso 1 1 calc R . . H3B2 H 0.5458 0.2401 0.4289 0.040 Uiso 1 1 calc R . . C4B C 0.6054(3) 0.21910(13) 0.5735(3) 0.0278(8) Uani 1 1 d . . . C5B C 0.6428(4) 0.25743(13) 0.6226(3) 0.0341(9) Uani 1 1 d . . . H5B H 0.6619 0.2811 0.5864 0.041 Uiso 1 1 calc R . . C6B C 0.6526(4) 0.26146(14) 0.7240(3) 0.0382(10) Uani 1 1 d . . . H6B H 0.6784 0.2878 0.7576 0.046 Uiso 1 1 calc R . . C7B C 0.6244(3) 0.22683(13) 0.7767(3) 0.0325(8) Uani 1 1 d . . . H7B H 0.6303 0.2297 0.8463 0.039 Uiso 1 1 calc R . . C8B C 0.5878(3) 0.18809(12) 0.7288(3) 0.0264(7) Uani 1 1 d . . . C9B C 0.5776(3) 0.18479(12) 0.6266(3) 0.0270(7) Uani 1 1 d . . . H9B H 0.5512 0.1586 0.5928 0.032 Uiso 1 1 calc R . . C10B C 0.5597(3) 0.15075(13) 0.7875(3) 0.0290(8) Uani 1 1 d . . . H10C H 0.5114 0.1612 0.8292 0.035 Uiso 1 1 calc R . . H10D H 0.5176 0.1288 0.7405 0.035 Uiso 1 1 calc R . . N4B N 0.6606(3) 0.13020(10) 0.8530(2) 0.0237(6) Uani 1 1 d . . . H4B H 0.7122 0.1521 0.8758 0.028 Uiso 1 1 calc R . . C11B C 0.6341(3) 0.11091(13) 0.9416(3) 0.0283(8) Uani 1 1 d . . . H11C H 0.5652 0.0935 0.9206 0.034 Uiso 1 1 calc R . . H11D H 0.6218 0.1341 0.9869 0.034 Uiso 1 1 calc R . . C12B C 0.7287(3) 0.08253(12) 0.9955(3) 0.0273(8) Uani 1 1 d . . . H12C H 0.7956 0.1005 1.0226 0.033 Uiso 1 1 calc R . . H12D H 0.7090 0.0679 1.0522 0.033 Uiso 1 1 calc R . . C1C C 0.9374(3) 0.17513(14) 0.3086(3) 0.0317(8) Uani 1 1 d . . . H1C1 H 0.9614 0.1981 0.2688 0.038 Uiso 1 1 calc R . . H1C2 H 0.9455 0.1468 0.2775 0.038 Uiso 1 1 calc R . . C2C C 1.0094(3) 0.17606(14) 0.4143(3) 0.0340(9) Uani 1 1 d . . . H2C1 H 1.0867 0.1681 0.4156 0.041 Uiso 1 1 calc R . . H2C2 H 1.0099 0.2055 0.4426 0.041 Uiso 1 1 calc R . . N3C N 0.9632(3) 0.14471(11) 0.4737(2) 0.0279(7) Uani 1 1 d . . . H3C H 0.9933 0.1520 0.5404 0.034 Uiso 1 1 calc R . . C3C C 1.0025(3) 0.09994(13) 0.4616(3) 0.0323(8) Uani 1 1 d . . . H3C1 H 1.0842 0.0989 0.4888 0.039 Uiso 1 1 calc R . . H3C2 H 0.9857 0.0931 0.3893 0.039 Uiso 1 1 calc R . . C4C C 0.9506(3) 0.06596(13) 0.5127(3) 0.0273(8) Uani 1 1 d . . . C5C C 0.8861(3) 0.03368(13) 0.4564(3) 0.0294(8) Uani 1 1 d . . . H5C H 0.8712 0.0343 0.3855 0.035 Uiso 1 1 calc R . . C6C C 0.8431(3) 0.00062(13) 0.5025(3) 0.0325(8) Uani 1 1 d . . . H6C H 0.7985 -0.0213 0.4633 0.039 Uiso 1 1 calc R . . C7C C 0.8653(3) -0.00058(13) 0.6061(3) 0.0321(8) Uani 1 1 d . . . H7C H 0.8365 -0.0235 0.6377 0.039 Uiso 1 1 calc R . . C8C C 0.9291(3) 0.03133(13) 0.6633(3) 0.0294(8) Uani 1 1 d . . . C9C C 0.9720(3) 0.06432(13) 0.6157(3) 0.0284(8) Uani 1 1 d . . . H9C H 1.0168 0.0862 0.6549 0.034 Uiso 1 1 calc R . . C10C C 0.9572(3) 0.02886(14) 0.7752(3) 0.0335(9) Uani 1 1 d . . . H10E H 0.9266 0.0016 0.7949 0.040 Uiso 1 1 calc R . . H10F H 1.0390 0.0278 0.8016 0.040 Uiso 1 1 calc R . . N4C N 0.9134(3) 0.06589(10) 0.8218(2) 0.0255(6) Uani 1 1 d . . . H4C H 0.9475 0.0907 0.8056 0.031 Uiso 1 1 calc R . . C11C C 0.9472(3) 0.06220(14) 0.9325(3) 0.0315(8) Uani 1 1 d . . . H11E H 0.9458 0.0911 0.9633 0.038 Uiso 1 1 calc R . . H11F H 1.0237 0.0505 0.9549 0.038 Uiso 1 1 calc R . . C12C C 0.8669(3) 0.03219(12) 0.9637(3) 0.0280(8) Uani 1 1 d . . . H12E H 0.8718 0.0029 0.9363 0.034 Uiso 1 1 calc R . . H12F H 0.8855 0.0301 1.0376 0.034 Uiso 1 1 calc R . . O1 O 0.8105(2) 0.15811(9) 0.5861(2) 0.0320(6) Uani 1 1 d . . . O2 O 0.8515(2) 0.15495(9) 0.7515(2) 0.0346(6) Uani 1 1 d . . . O3 O 0.7420(2) 0.10589(8) 0.66477(18) 0.0246(5) Uani 1 1 d . . . C1 C 0.7991(3) 0.13940(12) 0.6610(3) 0.0242(7) Uani 1 1 d . . . C2 C 0.9136(6) 0.1959(2) 0.7548(5) 0.0681(17) Uani 1 1 d . . . H2A H 0.9665 0.1931 0.7136 0.102 Uiso 1 1 calc R . . H2B H 0.9542 0.2022 0.8240 0.102 Uiso 1 1 calc R . . H2C H 0.8616 0.2195 0.7289 0.102 Uiso 1 1 calc R . . Cl1 Cl 0.96891(10) 0.28979(4) 0.54865(9) 0.0456(3) Uani 0.50 1 d PD A 1 O11 O 0.9172(5) 0.25037(18) 0.5583(4) 0.0956(18) Uani 0.50 1 d PD A 1 O13 O 0.9743(13) 0.3170(4) 0.6297(8) 0.065(5) Uani 0.50 1 d PD A 1 O12 O 0.8897(12) 0.3069(5) 0.4635(9) 0.149(9) Uani 0.50 1 d PD A 1 O14 O 1.0696(7) 0.2849(3) 0.5265(9) 0.053(3) Uani 0.50 1 d PD A 1 Cl1' Cl 0.96891(10) 0.28979(4) 0.54865(9) 0.0456(3) Uani 0.50 1 d PD B 2 O11' O 0.9172(5) 0.25037(18) 0.5583(4) 0.0956(18) Uani 0.50 1 d PD B 2 O13' O 0.9705(19) 0.3198(7) 0.6255(14) 0.149(13) Uani 0.50 1 d PD B 2 O12' O 0.9268(17) 0.3061(4) 0.4537(7) 0.162(10) Uani 0.50 1 d PDU B 2 O14' O 1.0790(10) 0.2739(7) 0.5696(15) 0.181(12) Uani 0.50 1 d PD B 2 Cl2 Cl 0.34693(19) 0.00863(8) 0.80164(16) 0.0371(5) Uani 0.748(6) 1 d PD C 1 O21 O 0.4136(4) -0.01796(18) 0.8798(3) 0.0591(16) Uani 0.748(6) 1 d PD C 1 O22 O 0.2424(4) 0.00793(18) 0.8224(5) 0.105(2) Uani 0.748(6) 1 d PD C 1 O23 O 0.3514(3) -0.01000(11) 0.7117(3) 0.0486(9) Uani 0.748(6) 1 d PD C 1 O24 O 0.3961(3) 0.05157(12) 0.8107(3) 0.0568(11) Uani 0.748(6) 1 d PD C 1 Cl2' Cl 0.3130(5) 0.02350(19) 0.7784(4) 0.0277(11) Uani 0.252(6) 1 d PD C 2 O21' O 0.2288(11) 0.0480(4) 0.7104(9) 0.056(4) Uani 0.252(6) 1 d PD C 2 O22' O 0.2424(4) 0.00793(18) 0.8224(5) 0.105(2) Uani 0.25 1 d PD C 2 O23' O 0.3514(3) -0.01000(11) 0.7117(3) 0.0486(9) Uani 0.25 1 d PD C 2 O24' O 0.3961(3) 0.05157(12) 0.8107(3) 0.0568(11) Uani 0.25 1 d PD C 2 Cl3 Cl 1.08972(8) 0.10387(3) 1.18060(7) 0.02823(19) Uani 1 1 d D . . O31 O 1.0691(3) 0.13916(10) 1.1106(3) 0.0502(9) Uani 1 1 d D . . O32 O 1.1537(3) 0.07164(11) 1.1466(3) 0.0497(8) Uani 1 1 d D . . O33 O 1.1468(3) 0.11967(12) 1.2764(2) 0.0476(8) Uani 1 1 d D . . O34 O 0.9854(3) 0.08538(11) 1.1845(3) 0.0445(8) Uani 1 1 d D . . N20 N 0.6275(9) 0.3697(4) 0.3558(9) 0.079(3) Uani 0.60 1 d P D 1 C21 C 0.7075(9) 0.3815(3) 0.4211(7) 0.097(3) Uani 0.60 1 d P D 1 C22 C 0.7977(8) 0.3967(3) 0.4992(7) 0.051(2) Uani 0.60 1 d P D 1 H22A H 0.7692 0.4149 0.5451 0.077 Uiso 0.60 1 calc PR D 1 H22B H 0.8483 0.4137 0.4706 0.077 Uiso 0.60 1 calc PR D 1 H22C H 0.8378 0.3719 0.5359 0.077 Uiso 0.60 1 calc PR D 1 O20' O 0.6452(14) 0.3981(7) 0.3208(13) 0.112(6) Uani 0.40 1 d P E 2 C21' C 0.7075(9) 0.3815(3) 0.4211(7) 0.097(3) Uani 0.40 1 d P E 2 O30 O 1.1402(4) 0.16266(19) 0.6694(4) 0.0974(18) Uani 1 1 d . . . C30 C 1.2489(6) 0.1614(3) 0.6670(6) 0.092(2) Uani 1 1 d . . . H30A H 1.2949 0.1757 0.7268 0.138 Uiso 1 1 calc R . . H30B H 1.2574 0.1765 0.6072 0.138 Uiso 1 1 calc R . . H30C H 1.2726 0.1312 0.6654 0.138 Uiso 1 1 calc R . . O40 O 0.8552(3) 0.17957(14) 1.0096(3) 0.0669(11) Uani 1 1 d . . . C40 C 0.8448(5) 0.2240(2) 1.0229(4) 0.0599(15) Uani 1 1 d . . . H40A H 0.8974 0.2330 1.0853 0.090 Uiso 1 1 calc R . . H40B H 0.7688 0.2305 1.0261 0.090 Uiso 1 1 calc R . . H40C H 0.8608 0.2396 0.9665 0.090 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 Cu1 0.0276(2) 0.0212(2) 0.0221(2) -0.00014(17) 0.01023(17) -0.00064(17) Cu2 0.0215(2) 0.0205(2) 0.01517(19) 0.00184(16) 0.00307(15) 0.00205(16) N1 0.0333(17) 0.0236(15) 0.0265(16) -0.0010(12) 0.0130(13) -0.0062(13) C1A 0.037(2) 0.0303(19) 0.0238(18) -0.0008(14) 0.0125(16) -0.0064(16) C2A 0.034(2) 0.0287(19) 0.0270(18) -0.0055(15) 0.0143(16) -0.0053(15) N3A 0.0281(15) 0.0222(14) 0.0216(14) 0.0000(11) 0.0093(12) -0.0024(12) C3A 0.0263(18) 0.0308(19) 0.0203(16) 0.0036(14) 0.0055(14) -0.0003(14) C4A 0.0207(16) 0.0239(17) 0.0190(15) -0.0007(13) 0.0035(12) -0.0036(13) C5A 0.0214(17) 0.038(2) 0.0292(19) 0.0076(16) 0.0028(14) 0.0002(15) C6A 0.0212(18) 0.047(2) 0.032(2) 0.0049(18) 0.0036(15) 0.0028(16) C7A 0.0239(18) 0.039(2) 0.0247(18) 0.0007(15) 0.0076(14) -0.0058(15) C8A 0.0233(17) 0.0227(16) 0.0156(15) -0.0028(12) 0.0005(12) -0.0025(13) C9A 0.0222(16) 0.0224(16) 0.0190(15) -0.0027(12) 0.0034(13) -0.0029(13) C10A 0.0282(18) 0.0239(17) 0.0150(15) -0.0030(13) 0.0028(13) -0.0007(14) N4A 0.0247(14) 0.0207(14) 0.0141(13) 0.0004(10) 0.0041(11) 0.0012(11) C11A 0.0332(19) 0.0211(17) 0.0224(17) 0.0008(13) 0.0040(14) -0.0009(14) C12A 0.036(2) 0.0273(18) 0.0193(16) 0.0035(14) 0.0070(15) -0.0048(15) N2 0.0271(15) 0.0230(14) 0.0175(13) -0.0003(11) 0.0039(11) 0.0024(12) C1B 0.051(2) 0.0241(19) 0.029(2) 0.0047(15) 0.0156(18) -0.0057(17) C2B 0.050(3) 0.027(2) 0.031(2) 0.0082(16) 0.0128(18) 0.0075(18) N3B 0.0363(17) 0.0234(15) 0.0235(15) 0.0015(12) 0.0103(13) 0.0024(13) C3B 0.034(2) 0.035(2) 0.029(2) 0.0050(16) 0.0068(16) 0.0095(17) C4B 0.0272(18) 0.0287(19) 0.0282(18) 0.0012(15) 0.0084(15) 0.0116(15) C5B 0.040(2) 0.0246(19) 0.041(2) 0.0025(16) 0.0171(18) 0.0058(16) C6B 0.050(3) 0.026(2) 0.044(2) -0.0077(17) 0.021(2) 0.0038(18) C7B 0.040(2) 0.030(2) 0.032(2) -0.0045(16) 0.0163(17) 0.0054(16) C8B 0.0254(18) 0.0246(18) 0.0291(18) 0.0009(14) 0.0068(14) 0.0110(14) C9B 0.0266(18) 0.0235(18) 0.0291(19) -0.0004(14) 0.0040(14) 0.0072(14) C10B 0.0278(19) 0.031(2) 0.0295(19) 0.0049(15) 0.0103(15) 0.0081(15) N4B 0.0284(15) 0.0242(15) 0.0188(14) 0.0020(11) 0.0069(12) 0.0024(12) C11B 0.034(2) 0.0307(19) 0.0230(17) -0.0013(15) 0.0128(15) 0.0029(16) C12B 0.038(2) 0.0262(18) 0.0173(16) -0.0029(14) 0.0063(14) 0.0033(15) C1C 0.034(2) 0.033(2) 0.034(2) -0.0014(16) 0.0177(17) -0.0088(16) C2C 0.033(2) 0.033(2) 0.040(2) -0.0033(17) 0.0166(18) -0.0094(17) N3C 0.0288(16) 0.0305(16) 0.0272(16) -0.0022(13) 0.0122(13) -0.0020(13) C3C 0.032(2) 0.034(2) 0.036(2) 0.0012(17) 0.0178(17) 0.0050(16) C4C 0.0245(18) 0.0296(19) 0.0315(19) 0.0009(15) 0.0141(15) 0.0082(14) C5C 0.0234(18) 0.036(2) 0.0285(19) -0.0003(16) 0.0065(15) 0.0088(15) C6C 0.0238(18) 0.031(2) 0.042(2) 0.0007(17) 0.0076(16) 0.0042(15) C7C 0.0281(19) 0.031(2) 0.040(2) 0.0090(17) 0.0151(17) 0.0104(16) C8C 0.0276(18) 0.034(2) 0.0295(19) 0.0042(16) 0.0133(15) 0.0146(15) C9C 0.0267(18) 0.0300(19) 0.0308(19) -0.0016(15) 0.0118(15) 0.0070(15) C10C 0.033(2) 0.036(2) 0.032(2) 0.0065(17) 0.0106(16) 0.0176(17) N4C 0.0242(15) 0.0287(16) 0.0228(15) 0.0046(12) 0.0049(12) 0.0052(12) C11C 0.0289(19) 0.034(2) 0.0246(18) -0.0001(15) -0.0050(15) 0.0067(16) C12C 0.034(2) 0.0275(19) 0.0180(16) 0.0015(14) -0.0010(14) 0.0078(15) O1 0.0375(15) 0.0311(14) 0.0297(14) 0.0038(11) 0.0131(12) 0.0055(12) O2 0.0374(16) 0.0337(15) 0.0307(15) -0.0039(12) 0.0052(12) -0.0053(12) O3 0.0253(12) 0.0260(13) 0.0205(12) 0.0018(10) 0.0023(10) -0.0011(10) C1 0.0216(16) 0.0258(18) 0.0256(17) 0.0005(14) 0.0071(14) 0.0068(14) C2 0.078(4) 0.067(4) 0.056(4) -0.010(3) 0.013(3) -0.011(3) Cl1 0.0449(6) 0.0468(6) 0.0464(6) -0.0117(5) 0.0144(5) -0.0143(5) O11 0.112(4) 0.104(4) 0.078(3) 0.001(3) 0.038(3) -0.060(3) O13 0.045(9) 0.095(12) 0.050(7) -0.019(8) 0.003(6) 0.020(7) O12 0.121(10) 0.147(14) 0.118(12) -0.076(10) -0.081(9) 0.105(10) O14 0.044(5) 0.055(5) 0.073(7) -0.016(4) 0.040(5) -0.022(4) Cl1' 0.0449(6) 0.0468(6) 0.0464(6) -0.0117(5) 0.0144(5) -0.0143(5) O11' 0.112(4) 0.104(4) 0.078(3) 0.001(3) 0.038(3) -0.060(3) O13' 0.081(15) 0.18(2) 0.148(18) -0.148(15) -0.032(11) 0.041(13) O12' 0.37(3) 0.073(8) 0.027(5) 0.010(5) 0.029(10) -0.117(13) O14' 0.091(11) 0.23(2) 0.19(2) -0.163(19) -0.018(11) 0.034(12) Cl2 0.0338(10) 0.0484(12) 0.0326(9) -0.0057(8) 0.0145(8) -0.0147(8) O21 0.054(3) 0.086(4) 0.033(2) 0.015(2) 0.004(2) -0.025(3) O22 0.071(3) 0.100(4) 0.174(6) -0.004(4) 0.083(4) -0.010(3) O23 0.063(2) 0.0383(18) 0.0439(19) -0.0052(14) 0.0122(16) -0.0074(16) O24 0.053(2) 0.048(2) 0.076(3) -0.0225(19) 0.0283(19) -0.0138(17) Cl2' 0.026(2) 0.035(3) 0.022(2) 0.0064(17) 0.0046(17) -0.0023(18) O21' 0.070(10) 0.051(9) 0.043(8) -0.003(6) 0.007(7) 0.026(7) O22' 0.071(3) 0.100(4) 0.174(6) -0.004(4) 0.083(4) -0.010(3) O23' 0.063(2) 0.0383(18) 0.0439(19) -0.0052(14) 0.0122(16) -0.0074(16) O24' 0.053(2) 0.048(2) 0.076(3) -0.0225(19) 0.0283(19) -0.0138(17) Cl3 0.0303(4) 0.0248(4) 0.0276(4) -0.0027(3) 0.0039(4) 0.0035(3) O31 0.072(2) 0.0296(16) 0.0459(19) 0.0063(14) 0.0092(17) 0.0048(16) O32 0.050(2) 0.0406(18) 0.061(2) -0.0070(16) 0.0184(17) 0.0158(15) O33 0.0356(17) 0.071(2) 0.0318(16) -0.0152(16) 0.0005(13) -0.0030(16) O34 0.0348(16) 0.0448(19) 0.052(2) -0.0108(15) 0.0082(14) -0.0081(14) N20 0.063(6) 0.110(10) 0.062(6) 0.005(6) 0.012(5) 0.023(6) C21 0.111(7) 0.101(6) 0.098(6) 0.015(5) 0.061(6) 0.049(5) C22 0.051(5) 0.044(5) 0.058(5) 0.000(4) 0.014(4) 0.008(4) O20' 0.098(12) 0.146(17) 0.092(12) 0.010(11) 0.023(9) 0.020(11) C21' 0.111(7) 0.101(6) 0.098(6) 0.015(5) 0.061(6) 0.049(5) O30 0.066(3) 0.112(4) 0.092(4) -0.013(3) -0.019(3) -0.013(3) C30 0.075(5) 0.106(6) 0.092(6) -0.025(5) 0.015(4) -0.014(4) O40 0.061(3) 0.058(2) 0.075(3) -0.015(2) 0.006(2) -0.012(2) C40 0.052(3) 0.071(4) 0.054(3) 0.005(3) 0.010(3) -0.020(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.963(3) . ? Cu1 N1 2.040(3) . ? Cu1 N3C 2.061(3) . ? Cu1 N3B 2.074(3) . ? Cu1 N3A 2.232(3) . ? Cu1 Cu2 5.6554(6) . ? Cu2 O3 1.941(3) . ? Cu2 N2 2.034(3) . ? Cu2 N4C 2.086(3) . ? Cu2 N4A 2.130(3) . ? Cu2 N4B 2.158(3) . ? N1 C1B 1.479(5) . ? N1 C1A 1.482(5) . ? N1 C1C 1.496(5) . ? C1A C2A 1.504(5) . ? C2A N3A 1.487(5) . ? N3A C3A 1.473(5) . ? C3A C4A 1.497(5) . ? C4A C9A 1.388(5) . ? C4A C5A 1.389(5) . ? C5A C6A 1.381(6) . ? C6A C7A 1.380(6) . ? C7A C8A 1.387(5) . ? C8A C9A 1.389(5) . ? C8A C10A 1.509(5) . ? C10A N4A 1.474(4) . ? N4A C11A 1.479(4) . ? C11A C12A 1.503(5) . ? C12A N2 1.488(5) . ? N2 C12C 1.482(5) . ? N2 C12B 1.493(4) . ? C1B C2B 1.499(6) . ? C2B N3B 1.480(5) . ? N3B C3B 1.494(5) . ? C3B C4B 1.503(5) . ? C4B C9B 1.383(5) . ? C4B C5B 1.384(6) . ? C5B C6B 1.383(6) . ? C6B C7B 1.390(6) . ? C7B C8B 1.386(5) . ? C8B C9B 1.390(5) . ? C8B C10B 1.503(5) . ? C10B N4B 1.487(5) . ? N4B C11B 1.475(5) . ? C11B C12B 1.502(5) . ? C1C C2C 1.505(6) . ? C2C N3C 1.480(5) . ? N3C C3C 1.490(5) . ? C3C C4C 1.502(5) . ? C4C C9C 1.382(5) . ? C4C C5C 1.386(6) . ? C5C C6C 1.382(6) . ? C6C C7C 1.389(6) . ? C7C C8C 1.379(6) . ? C8C C9C 1.392(6) . ? C8C C10C 1.499(5) . ? C10C N4C 1.484(5) . ? N4C C11C 1.485(5) . ? C11C C12C 1.507(6) . ? O1 C1 1.228(5) . ? O2 C1 1.342(5) . ? O2 C2 1.476(7) . ? O3 C1 1.264(4) . ? Cl1 O14 1.374(7) . ? Cl1 O13 1.390(9) . ? Cl1 O11 1.400(4) . ? Cl1 O12 1.428(8) . ? Cl2 O23 1.385(4) . ? Cl2 O22 1.405(4) . ? Cl2 O21 1.438(5) . ? Cl2 O24 1.452(4) . ? Cl2' O21' 1.430(11) . ? Cl3 O33 1.419(3) . ? Cl3 O32 1.429(3) . ? Cl3 O34 1.433(3) . ? Cl3 O31 1.436(3) . ? N20 C21 1.215(14) . ? C21 C22 1.422(14) . ? O30 C30 1.364(9) . ? O40 C40 1.393(7) . ? 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 Cu1 N1 159.77(12) . . ? O1 Cu1 N3C 87.44(12) . . ? N1 Cu1 N3C 85.01(13) . . ? O1 Cu1 N3B 88.62(12) . . ? N1 Cu1 N3B 84.70(13) . . ? N3C Cu1 N3B 138.47(13) . . ? O1 Cu1 N3A 116.34(12) . . ? N1 Cu1 N3A 83.89(12) . . ? N3C Cu1 N3A 109.10(12) . . ? N3B Cu1 N3A 109.62(12) . . ? O1 Cu1 Cu2 26.43(9) . . ? N1 Cu1 Cu2 172.40(9) . . ? N3C Cu1 Cu2 92.44(9) . . ? N3B Cu1 Cu2 101.84(9) . . ? N3A Cu1 Cu2 90.21(8) . . ? O3 Cu2 N2 176.52(12) . . ? O3 Cu2 N4C 92.00(11) . . ? N2 Cu2 N4C 85.26(12) . . ? O3 Cu2 N4A 95.49(10) . . ? N2 Cu2 N4A 84.42(11) . . ? N4C Cu2 N4A 126.09(12) . . ? O3 Cu2 N4B 99.08(11) . . ? N2 Cu2 N4B 84.33(11) . . ? N4C Cu2 N4B 129.62(12) . . ? N4A Cu2 N4B 101.67(12) . . ? O3 Cu2 Cu1 7.47(7) . . ? N2 Cu2 Cu1 170.51(9) . . ? N4C Cu2 Cu1 85.33(9) . . ? N4A Cu2 Cu1 102.15(7) . . ? N4B Cu2 Cu1 100.80(8) . . ? C1B N1 C1A 111.4(3) . . ? C1B N1 C1C 111.0(3) . . ? C1A N1 C1C 110.1(3) . . ? C1B N1 Cu1 106.6(2) . . ? C1A N1 Cu1 109.3(2) . . ? C1C N1 Cu1 108.3(2) . . ? N1 C1A C2A 110.1(3) . . ? N3A C2A C1A 110.1(3) . . ? C3A N3A C2A 110.8(3) . . ? C3A N3A Cu1 119.7(2) . . ? C2A N3A Cu1 101.5(2) . . ? N3A C3A C4A 114.2(3) . . ? C9A C4A C5A 118.2(3) . . ? C9A C4A C3A 122.8(3) . . ? C5A C4A C3A 118.8(3) . . ? C6A C5A C4A 120.5(4) . . ? C7A C6A C5A 120.9(4) . . ? C6A C7A C8A 119.4(4) . . ? C7A C8A C9A 119.4(3) . . ? C7A C8A C10A 121.5(3) . . ? C9A C8A C10A 118.9(3) . . ? C4A C9A C8A 121.5(3) . . ? N4A C10A C8A 114.0(3) . . ? C10A N4A C11A 110.1(3) . . ? C10A N4A Cu2 120.0(2) . . ? C11A N4A Cu2 101.2(2) . . ? N4A C11A C12A 108.5(3) . . ? N2 C12A C11A 110.1(3) . . ? C12C N2 C12A 111.1(3) . . ? C12C N2 C12B 110.4(3) . . ? C12A N2 C12B 110.5(3) . . ? C12C N2 Cu2 108.2(2) . . ? C12A N2 Cu2 109.1(2) . . ? C12B N2 Cu2 107.6(2) . . ? N1 C1B C2B 109.6(3) . . ? N3B C2B C1B 109.4(3) . . ? C2B N3B C3B 110.6(3) . . ? C2B N3B Cu1 108.0(2) . . ? C3B N3B Cu1 122.5(2) . . ? N3B C3B C4B 113.1(3) . . ? C9B C4B C5B 119.5(4) . . ? C9B C4B C3B 120.7(4) . . ? C5B C4B C3B 119.7(4) . . ? C6B C5B C4B 120.3(4) . . ? C5B C6B C7B 119.7(4) . . ? C8B C7B C6B 120.6(4) . . ? C7B C8B C9B 118.8(4) . . ? C7B C8B C10B 119.8(4) . . ? C9B C8B C10B 121.4(4) . . ? C4B C9B C8B 121.0(4) . . ? N4B C10B C8B 112.3(3) . . ? C11B N4B C10B 110.1(3) . . ? C11B N4B Cu2 105.3(2) . . ? C10B N4B Cu2 119.2(2) . . ? N4B C11B C12B 109.4(3) . . ? N2 C12B C11B 109.8(3) . . ? N1 C1C C2C 109.8(3) . . ? N3C C2C C1C 108.0(3) . . ? C2C N3C C3C 110.9(3) . . ? C2C N3C Cu1 103.6(2) . . ? C3C N3C Cu1 122.8(2) . . ? N3C C3C C4C 113.6(3) . . ? C9C C4C C5C 118.8(4) . . ? C9C C4C C3C 121.4(4) . . ? C5C C4C C3C 119.7(4) . . ? C6C C5C C4C 120.6(4) . . ? C5C C6C C7C 119.9(4) . . ? C8C C7C C6C 120.3(4) . . ? C7C C8C C9C 119.0(4) . . ? C7C C8C C10C 120.2(4) . . ? C9C C8C C10C 120.7(4) . . ? C4C C9C C8C 121.3(4) . . ? N4C C10C C8C 113.3(3) . . ? C10C N4C C11C 110.6(3) . . ? C10C N4C Cu2 122.8(3) . . ? C11C N4C Cu2 102.5(2) . . ? N4C C11C C12C 108.1(3) . . ? N2 C12C C11C 108.7(3) . . ? C1 O1 Cu1 151.9(3) . . ? C1 O2 C2 117.3(4) . . ? C1 O3 Cu2 120.3(2) . . ? O1 C1 O3 127.6(4) . . ? O1 C1 O2 119.0(3) . . ? O3 C1 O2 113.4(3) . . ? O14 Cl1 O13 112.9(8) . . ? O14 Cl1 O11 113.3(5) . . ? O13 Cl1 O11 112.1(7) . . ? O14 Cl1 O12 109.4(9) . . ? O13 Cl1 O12 108.7(8) . . ? O11 Cl1 O12 99.5(8) . . ? O23 Cl2 O22 115.7(3) . . ? O23 Cl2 O21 106.8(3) . . ? O22 Cl2 O21 102.9(4) . . ? O23 Cl2 O24 110.0(2) . . ? O22 Cl2 O24 112.9(3) . . ? O21 Cl2 O24 107.9(3) . . ? O33 Cl3 O32 111.1(2) . . ? O33 Cl3 O34 110.0(2) . . ? O32 Cl3 O34 108.9(2) . . ? O33 Cl3 O31 109.2(2) . . ? O32 Cl3 O31 108.9(2) . . ? O34 Cl3 O31 108.8(2) . . ? N20 C21 C22 177.3(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3A H3A O23 0.93 2.60 3.173(4) 120.1 3_656 N3A H3A O23' 0.93 2.60 3.173(4) 120.1 3_656 N4A H4A O24' 0.93 2.29 3.163(5) 156.9 . N4A H4A O24 0.93 2.29 3.163(5) 156.9 . N3B H3B O11' 0.93 2.19 2.993(6) 143.5 . N3B H3B O11 0.93 2.19 2.993(6) 143.5 . N4B H4B O40 0.93 2.37 3.189(5) 147.0 . N3C H3C O30 0.93 2.22 3.067(6) 150.3 . N4C H4C O2 0.93 2.34 2.952(4) 123.2 . N4C H4C O20' 0.93 2.44 3.098(17) 127.5 4_666 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 19.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.241 _refine_diff_density_min -0.674 _refine_diff_density_rms 0.087 data_Complex_3 #(y141x) _database_code_CSD 181029 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39.50 H65 Cl2 N8 Ni2 O14' _chemical_formula_weight 1064.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 24.320(3) _cell_length_b 10.8310(16) _cell_length_c 19.546(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5148.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 36 _cell_measurement_theta_min 5.22 _cell_measurement_theta_max 12.49 _exptl_crystal_description plate _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.76 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 0.901 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7654 _exptl_absorpt_correction_T_max 0.8524 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4533 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0931 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max -1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4308 _reflns_number_gt 3112 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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. The non-coordinated solvate methanol and water molecules were refined with half site occupancy. The hydrogen atoms of the water molecule were not located or included in the model. ; _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^)+(0.0774P)^2^+2.7014P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.96(5) _refine_ls_number_reflns 4308 _refine_ls_number_parameters 608 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0994 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1461 _refine_ls_wR_factor_gt 0.1255 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.088 _refine_ls_shift/su_mean 0.005 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 0.07673(5) 0.19271(10) 0.16673(8) 0.0236(3) Uani 1 1 d . . . Ni2 Ni -0.14644(5) 0.23592(10) 0.29754(9) 0.0248(3) Uani 1 1 d . . . N1 N 0.1506(4) 0.1700(7) 0.1119(6) 0.035(2) Uani 1 1 d . . . C1A C 0.1451(5) 0.2312(10) 0.0436(6) 0.042(3) Uani 1 1 d . . . H1A1 H 0.1647 0.3114 0.0442 0.050 Uiso 1 1 calc R . . H1A2 H 0.1623 0.1787 0.0080 0.050 Uiso 1 1 calc R . . C2A C 0.0860(6) 0.2518(11) 0.0263(7) 0.047(3) Uani 1 1 d . . . H2A1 H 0.0834 0.3035 -0.0153 0.056 Uiso 1 1 calc R . . H2A2 H 0.0683 0.1715 0.0165 0.056 Uiso 1 1 calc R . . N3A N 0.0576(4) 0.3117(7) 0.0819(4) 0.0262(19) Uani 1 1 d . . . H3A H 0.0745 0.3874 0.0896 0.031 Uiso 1 1 calc R . . C3A C -0.0016(6) 0.3355(11) 0.0650(7) 0.049(3) Uani 1 1 d . . . H3A1 H -0.0040 0.3609 0.0164 0.059 Uiso 1 1 calc R . . H3A2 H -0.0222 0.2572 0.0699 0.059 Uiso 1 1 calc R . . C4A C -0.0293(7) 0.4323(12) 0.1081(8) 0.053(4) Uani 1 1 d . . . C5A C -0.0050(7) 0.5492(12) 0.1168(8) 0.057(4) Uani 1 1 d . . . H5A H 0.0306 0.5671 0.0995 0.068 Uiso 1 1 calc R . . C6A C -0.0355(7) 0.6369(11) 0.1518(7) 0.058(4) Uani 1 1 d . . . H6A H -0.0199 0.7166 0.1577 0.069 Uiso 1 1 calc R . . C7A C -0.0848(7) 0.6163(12) 0.1774(8) 0.066(5) Uani 1 1 d . . . H7A H -0.1032 0.6799 0.2018 0.080 Uiso 1 1 calc R . . C8A C -0.1096(6) 0.5033(11) 0.1690(8) 0.052(3) Uani 1 1 d . . . C9A C -0.0808(6) 0.4122(11) 0.1346(7) 0.043(3) Uani 1 1 d . . . H9A H -0.0972 0.3331 0.1293 0.052 Uiso 1 1 calc R . . C10A C -0.1660(7) 0.4873(13) 0.1956(9) 0.069(5) Uani 1 1 d . . . H10A H -0.1712 0.5469 0.2334 0.083 Uiso 1 1 calc R . . H10B H -0.1918 0.5112 0.1587 0.083 Uiso 1 1 calc R . . N4A N -0.1825(4) 0.3662(9) 0.2204(6) 0.042(3) Uani 1 1 d . . . H4A H -0.1817 0.3191 0.1806 0.051 Uiso 1 1 calc R . . C11A C -0.2447(7) 0.3661(13) 0.2381(9) 0.065(4) Uani 1 1 d . . . H11A H -0.2532 0.4411 0.2651 0.078 Uiso 1 1 calc R . . H11B H -0.2661 0.3707 0.1951 0.078 Uiso 1 1 calc R . . C12A C -0.2618(5) 0.2630(13) 0.2748(8) 0.056(4) Uani 1 1 d . . . H12A H -0.2609 0.1897 0.2446 0.067 Uiso 1 1 calc R . . H12B H -0.3003 0.2752 0.2899 0.067 Uiso 1 1 calc R . . N2 N -0.2260(4) 0.2394(8) 0.3367(6) 0.040(2) Uani 1 1 d . . . C1B C 0.1953(5) 0.2357(9) 0.1523(6) 0.034(3) Uani 1 1 d . . . H1B1 H 0.2099 0.1803 0.1882 0.041 Uiso 1 1 calc R . . H1B2 H 0.2259 0.2590 0.1215 0.041 Uiso 1 1 calc R . . C2B C 0.1710(5) 0.3487(9) 0.1842(6) 0.034(3) Uani 1 1 d . . . H2B1 H 0.1993 0.3919 0.2116 0.041 Uiso 1 1 calc R . . H2B2 H 0.1581 0.4057 0.1480 0.041 Uiso 1 1 calc R . . N3B N 0.1243(4) 0.3137(7) 0.2287(5) 0.0262(19) Uani 1 1 d . . . H3B H 0.1385 0.2670 0.2645 0.031 Uiso 1 1 calc R . . C3B C 0.0987(5) 0.4265(8) 0.2595(6) 0.029(2) Uani 1 1 d . . . H3B1 H 0.1285 0.4827 0.2745 0.034 Uiso 1 1 calc R . . H3B2 H 0.0774 0.4697 0.2236 0.034 Uiso 1 1 calc R . . C4B C 0.0617(4) 0.4027(8) 0.3189(5) 0.024(2) Uani 1 1 d . . . C5B C 0.0816(5) 0.3514(9) 0.3793(6) 0.033(3) Uani 1 1 d . . . H5B H 0.1190 0.3274 0.3829 0.039 Uiso 1 1 calc R . . C6B C 0.0460(5) 0.3355(10) 0.4348(6) 0.032(3) Uani 1 1 d . . . H6B H 0.0592 0.2998 0.4760 0.038 Uiso 1 1 calc R . . C7B C -0.0078(5) 0.3710(9) 0.4298(5) 0.030(3) Uani 1 1 d . . . H7B H -0.0314 0.3604 0.4681 0.037 Uiso 1 1 calc R . . C8B C -0.0292(4) 0.4232(8) 0.3690(5) 0.021(2) Uani 1 1 d . . . C9B C 0.0066(4) 0.4351(7) 0.3156(5) 0.025(2) Uani 1 1 d . . . H9B H -0.0071 0.4674 0.2737 0.030 Uiso 1 1 calc R . . C10B C -0.0873(5) 0.4641(8) 0.3632(6) 0.031(3) Uani 1 1 d . . . H10C H -0.0932 0.5322 0.3962 0.037 Uiso 1 1 calc R . . H10D H -0.0927 0.4985 0.3168 0.037 Uiso 1 1 calc R . . N4B N -0.1300(4) 0.3698(7) 0.3751(5) 0.025(2) Uani 1 1 d . . . H4B H -0.1212 0.3279 0.4152 0.030 Uiso 1 1 calc R . . C11B C -0.1843(4) 0.4314(9) 0.3853(6) 0.030(3) Uani 1 1 d . . . H11C H -0.1918 0.4874 0.3464 0.035 Uiso 1 1 calc R . . H11D H -0.1834 0.4814 0.4277 0.035 Uiso 1 1 calc R . . C12B C -0.2292(5) 0.3361(9) 0.3904(7) 0.036(3) Uani 1 1 d . . . H12C H -0.2273 0.2961 0.4359 0.043 Uiso 1 1 calc R . . H12D H -0.2653 0.3780 0.3870 0.043 Uiso 1 1 calc R . . C1C C 0.1603(5) 0.0369(10) 0.1099(8) 0.041(3) Uani 1 1 d . . . H1C1 H 0.1980 0.0200 0.0933 0.050 Uiso 1 1 calc R . . H1C2 H 0.1339 -0.0027 0.0781 0.050 Uiso 1 1 calc R . . C2C C 0.1528(5) -0.0171(9) 0.1835(7) 0.038(3) Uani 1 1 d . . . H2C1 H 0.1546 -0.1084 0.1817 0.045 Uiso 1 1 calc R . . H2C2 H 0.1829 0.0125 0.2134 0.045 Uiso 1 1 calc R . . N3C N 0.0994(4) 0.0216(7) 0.2120(5) 0.030(2) Uani 1 1 d . . . H3C H 0.0743 -0.0350 0.1945 0.036 Uiso 1 1 calc R . . C3C C 0.0968(5) 0.0039(9) 0.2876(7) 0.038(3) Uani 1 1 d . . . H3C1 H 0.1033 0.0840 0.3106 0.046 Uiso 1 1 calc R . . H3C2 H 0.1263 -0.0536 0.3019 0.046 Uiso 1 1 calc R . . C4C C 0.0419(5) -0.0470(8) 0.3098(6) 0.030(3) Uani 1 1 d . . . C5C C 0.0281(6) -0.1704(8) 0.2964(8) 0.049(3) Uani 1 1 d . . . H5C H 0.0535 -0.2218 0.2729 0.058 Uiso 1 1 calc R . . C6C C -0.0213(6) -0.2173(8) 0.3166(6) 0.040(3) Uani 1 1 d . . . H6C H -0.0301 -0.3013 0.3076 0.048 Uiso 1 1 calc R . . C7C C -0.0585(6) -0.1431(8) 0.3499(6) 0.037(3) Uani 1 1 d . . . H7C H -0.0928 -0.1764 0.3639 0.044 Uiso 1 1 calc R . . C8C C -0.0466(5) -0.0203(8) 0.3635(6) 0.026(2) Uani 1 1 d . . . C9C C 0.0037(5) 0.0267(8) 0.3431(6) 0.030(2) Uani 1 1 d . . . H9C H 0.0122 0.1107 0.3521 0.036 Uiso 1 1 calc R . . C10C C -0.0876(5) 0.0570(9) 0.4020(6) 0.032(3) Uani 1 1 d . . . H10E H -0.0707 0.1375 0.4133 0.038 Uiso 1 1 calc R . . H10F H -0.0969 0.0151 0.4455 0.038 Uiso 1 1 calc R . . N4C N -0.1395(4) 0.0789(7) 0.3620(5) 0.033(2) Uani 1 1 d . . . H4C H -0.1431 0.0109 0.3333 0.039 Uiso 1 1 calc R . . C11C C -0.1897(6) 0.0778(10) 0.4067(8) 0.047(3) Uani 1 1 d . . . H11E H -0.1956 -0.0064 0.4250 0.056 Uiso 1 1 calc R . . H11F H -0.1843 0.1345 0.4458 0.056 Uiso 1 1 calc R . . C12C C -0.2388(5) 0.1170(10) 0.3665(7) 0.041(3) Uani 1 1 d . . . H12E H -0.2466 0.0566 0.3298 0.049 Uiso 1 1 calc R . . H12F H -0.2714 0.1226 0.3966 0.049 Uiso 1 1 calc R . . O1 O 0.0114(3) 0.2201(5) 0.2221(4) 0.0251(15) Uani 1 1 d . . . O2 O -0.0689(3) 0.2413(5) 0.2688(4) 0.0251(15) Uani 1 1 d . . . O3 O -0.0608(3) 0.1169(6) 0.1792(4) 0.0346(19) Uani 1 1 d . . . C1 C -0.0389(4) 0.1918(8) 0.2238(5) 0.021(2) Uani 1 1 d . . . O41 O 0.0198(4) 0.0408(8) 0.1072(5) 0.052(2) Uani 1 1 d . . . H41 H 0.0074 0.0660 0.1330 0.078 Uiso 1 1 d . . . C42 C 0.0068(7) -0.0475(11) 0.0592(8) 0.058(4) Uani 1 1 d . . . H42A H 0.0362 -0.1092 0.0572 0.087 Uiso 1 1 calc R . . H42B H 0.0028 -0.0083 0.0143 0.087 Uiso 1 1 calc R . . H42C H -0.0278 -0.0876 0.0719 0.087 Uiso 1 1 calc R . . O51 O -0.1606(3) 0.1072(7) 0.2122(4) 0.0348(19) Uani 1 1 d . . . H51 H -0.1314 0.1154 0.1900 0.052 Uiso 1 1 d . . . C52 C -0.1796(7) -0.0132(13) 0.2052(10) 0.075(5) Uani 1 1 d . . . H52A H -0.1505 -0.0709 0.2185 0.112 Uiso 1 1 calc R . . H52B H -0.1899 -0.0281 0.1574 0.112 Uiso 1 1 calc R . . H52C H -0.2117 -0.0254 0.2346 0.112 Uiso 1 1 calc R . . Cl1 Cl 0.14769(15) -0.3367(3) 0.07268(16) 0.0461(8) Uani 1 1 d . . . O11 O 0.1289(4) -0.3290(8) 0.1410(5) 0.060(3) Uani 1 1 d . . . O12 O 0.1301(8) -0.4524(9) 0.0455(7) 0.106(6) Uani 1 1 d . . . O13 O 0.1240(5) -0.2493(7) 0.0298(6) 0.070(3) Uani 1 1 d . . . O14 O 0.2048(6) -0.323(2) 0.0709(10) 0.175(8) Uani 1 1 d . . . Cl2 Cl 0.25227(14) 0.2559(2) 0.3432(2) 0.0518(9) Uani 1 1 d . . . O21 O 0.2248(3) 0.3697(6) 0.3486(6) 0.048(2) Uani 1 1 d . . . O22 O 0.2162(4) 0.1606(6) 0.3190(5) 0.048(2) Uani 1 1 d . . . O23 O 0.2960(5) 0.2678(14) 0.2980(15) 0.184(12) Uani 1 1 d . . . O24 O 0.2779(9) 0.2268(10) 0.4030(11) 0.183(12) Uani 1 1 d . . . O61 O -0.1385(13) 0.105(3) -0.060(3) 0.17(2) Uani 0.50 1 d PU A 1 O71 O -0.1099(12) 0.316(2) -0.0764(16) 0.094(9) Uani 0.50 1 d P B 2 H71 H -0.1311 0.3650 -0.0408 0.040 Uiso 0.50 1 d P C 2 C72 C -0.0969(14) 0.207(3) -0.042(2) 0.080(12) Uani 0.50 1 d P B 2 H72A H -0.1067 0.2155 0.0064 0.060 Uiso 0.50 1 calc PR B 2 H72B H -0.0574 0.1909 -0.0462 0.060 Uiso 0.50 1 calc PR B 2 H72C H -0.1176 0.1384 -0.0621 0.060 Uiso 0.50 1 calc PR B 2 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 0.0235(6) 0.0259(6) 0.0214(6) 0.0000(6) 0.0025(7) -0.0007(5) Ni2 0.0192(6) 0.0280(6) 0.0272(6) -0.0058(6) -0.0018(7) 0.0005(5) N1 0.030(6) 0.034(5) 0.039(6) -0.008(4) 0.007(5) -0.002(4) C1A 0.041(8) 0.050(7) 0.034(6) -0.006(5) 0.009(6) 0.007(5) C2A 0.048(9) 0.062(7) 0.030(7) 0.007(6) 0.009(6) 0.008(6) N3A 0.028(5) 0.031(4) 0.019(4) 0.003(4) 0.000(4) 0.001(4) C3A 0.058(10) 0.064(8) 0.025(6) 0.001(6) -0.011(7) 0.010(6) C4A 0.066(11) 0.057(8) 0.034(8) 0.018(6) -0.013(8) 0.014(7) C5A 0.053(10) 0.075(9) 0.043(9) 0.029(7) -0.001(8) 0.001(7) C6A 0.105(13) 0.037(6) 0.032(8) 0.016(5) 0.014(9) 0.015(7) C7A 0.105(14) 0.054(8) 0.041(10) 0.014(7) 0.026(10) 0.047(8) C8A 0.056(9) 0.063(8) 0.037(7) 0.022(8) 0.009(8) 0.028(6) C9A 0.053(9) 0.044(7) 0.033(7) 0.022(5) -0.012(7) 0.002(6) C10A 0.065(12) 0.083(10) 0.059(10) 0.023(8) 0.007(9) 0.025(8) N4A 0.034(6) 0.055(6) 0.039(6) 0.000(5) -0.008(5) 0.015(4) C11A 0.057(11) 0.074(9) 0.064(11) 0.009(8) -0.023(9) 0.018(7) C12A 0.015(6) 0.093(10) 0.060(10) -0.014(8) -0.010(6) 0.000(6) N2 0.029(6) 0.044(5) 0.048(7) -0.013(5) -0.003(5) -0.005(4) C1B 0.025(6) 0.055(6) 0.021(6) -0.007(5) 0.014(5) -0.003(4) C2B 0.033(7) 0.040(6) 0.029(7) -0.004(4) 0.015(5) -0.013(4) N3B 0.027(5) 0.025(4) 0.026(5) -0.001(4) 0.008(4) 0.002(3) C3B 0.032(7) 0.023(5) 0.031(6) -0.005(4) -0.001(5) -0.002(4) C4B 0.019(6) 0.024(5) 0.028(6) -0.003(4) 0.000(4) -0.001(4) C5B 0.024(6) 0.045(6) 0.030(6) -0.002(5) 0.006(5) 0.006(5) C6B 0.023(7) 0.050(6) 0.023(6) -0.001(5) -0.003(5) -0.005(5) C7B 0.033(7) 0.039(6) 0.019(5) -0.003(4) 0.005(5) -0.006(5) C8B 0.028(6) 0.016(4) 0.019(5) -0.002(4) 0.001(5) -0.004(4) C9B 0.036(6) 0.009(4) 0.030(6) 0.000(4) -0.008(5) -0.001(4) C10B 0.035(7) 0.018(5) 0.038(7) -0.004(4) 0.005(5) 0.000(4) N4B 0.019(5) 0.026(4) 0.031(5) 0.000(4) -0.005(4) 0.004(3) C11B 0.019(6) 0.040(6) 0.030(6) -0.004(5) -0.001(5) 0.014(4) C12B 0.023(7) 0.032(6) 0.053(8) -0.008(5) 0.006(6) 0.002(4) C1C 0.023(7) 0.052(7) 0.050(8) -0.009(6) 0.012(6) 0.004(5) C2C 0.027(6) 0.028(5) 0.058(9) -0.006(5) 0.000(6) 0.004(4) N3C 0.033(5) 0.024(4) 0.034(5) 0.002(4) -0.006(5) 0.000(3) C3C 0.034(7) 0.035(5) 0.045(8) 0.000(6) 0.001(6) 0.000(4) C4C 0.037(7) 0.024(5) 0.030(7) 0.003(4) -0.017(5) 0.010(4) C5C 0.068(9) 0.021(5) 0.057(8) 0.006(6) 0.007(9) 0.012(5) C6C 0.065(9) 0.014(5) 0.042(7) -0.001(4) 0.008(6) -0.016(5) C7C 0.061(9) 0.024(5) 0.026(6) 0.004(4) 0.014(6) -0.005(5) C8C 0.038(7) 0.019(5) 0.021(6) 0.008(4) 0.004(5) 0.009(4) C9C 0.040(7) 0.024(5) 0.026(6) 0.007(4) -0.004(6) 0.002(4) C10C 0.045(8) 0.028(5) 0.024(6) 0.001(4) -0.001(6) 0.008(5) N4C 0.032(6) 0.031(4) 0.034(5) -0.005(4) 0.020(5) -0.006(4) C11C 0.044(8) 0.035(6) 0.062(9) -0.006(6) 0.022(7) -0.013(5) C12C 0.020(7) 0.057(7) 0.045(8) -0.015(6) 0.014(6) -0.011(5) O1 0.023(4) 0.030(4) 0.023(4) -0.007(3) -0.005(3) -0.001(3) O2 0.019(4) 0.027(3) 0.029(4) -0.010(3) 0.000(3) 0.003(3) O3 0.024(4) 0.046(4) 0.033(5) -0.014(3) 0.002(4) -0.010(3) C1 0.016(5) 0.021(5) 0.026(5) 0.002(4) -0.002(5) 0.004(4) O41 0.036(5) 0.075(6) 0.045(6) -0.024(5) 0.000(5) -0.005(4) C42 0.064(10) 0.057(8) 0.054(9) -0.009(7) 0.025(8) -0.023(7) O51 0.025(5) 0.049(4) 0.030(5) -0.018(3) 0.001(4) -0.003(3) C52 0.056(11) 0.080(10) 0.088(14) -0.047(9) 0.018(10) -0.026(8) Cl1 0.055(2) 0.0506(17) 0.0328(16) 0.0159(13) 0.0047(16) 0.0021(14) O11 0.085(8) 0.055(5) 0.039(5) -0.003(4) 0.014(5) -0.024(5) O12 0.200(17) 0.051(6) 0.068(9) -0.003(5) 0.051(10) -0.007(7) O13 0.109(10) 0.041(5) 0.058(7) 0.009(4) -0.026(7) 0.015(5) O14 0.029(9) 0.41(3) 0.081(12) 0.061(14) -0.013(9) 0.008(11) Cl2 0.042(2) 0.0360(14) 0.077(2) -0.0146(15) -0.0242(19) 0.0093(13) O21 0.037(5) 0.028(4) 0.079(7) -0.002(4) -0.003(5) 0.000(3) O22 0.050(6) 0.038(4) 0.057(6) -0.006(4) -0.010(5) -0.008(3) O23 0.046(8) 0.159(12) 0.35(3) -0.157(18) 0.055(16) -0.037(8) O24 0.30(3) 0.063(7) 0.188(18) -0.019(9) -0.21(2) 0.050(10) O61 0.08(2) 0.111(18) 0.32(5) -0.09(2) -0.12(3) -0.001(15) O71 0.08(2) 0.083(15) 0.12(2) -0.006(16) 0.038(18) 0.040(13) C72 0.039(19) 0.10(3) 0.10(3) -0.06(2) 0.016(19) -0.035(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1 1.946(7) . ? Ni1 N1 2.106(10) . ? Ni1 N3A 2.151(8) . ? Ni1 N3C 2.126(8) . ? Ni1 N3B 2.126(8) . ? Ni1 O41 2.445(8) . ? Ni1 Ni2 6.0178(19) . ? Ni2 O2 1.969(7) . ? Ni2 N2 2.081(11) . ? Ni2 N4C 2.124(9) . ? Ni2 N4B 2.136(9) . ? Ni2 O51 2.202(8) . ? Ni2 N4A 2.243(10) . ? N1 C1C 1.461(13) . ? N1 C1A 1.497(16) . ? N1 C1B 1.519(15) . ? C1A C2A 1.493(19) . ? C2A N3A 1.441(15) . ? N3A C3A 1.500(16) . ? C3A C4A 1.504(19) . ? C4A C9A 1.37(2) . ? C4A C5A 1.408(19) . ? C5A C6A 1.39(2) . ? C6A C7A 1.32(2) . ? C7A C8A 1.38(2) . ? C8A C9A 1.385(19) . ? C8A C10A 1.48(2) . ? C10A N4A 1.455(17) . ? N4A C11A 1.552(19) . ? C11A C12A 1.391(19) . ? C12A N2 1.513(17) . ? N2 C12C 1.481(14) . ? N2 C12B 1.484(15) . ? C1B C2B 1.496(14) . ? C2B N3B 1.480(13) . ? N3B C3B 1.497(12) . ? C3B C4B 1.491(15) . ? C4B C9B 1.388(14) . ? C4B C5B 1.392(15) . ? C5B C6B 1.398(16) . ? C6B C7B 1.366(16) . ? C7B C8B 1.415(14) . ? C8B C9B 1.367(14) . ? C8B C10B 1.484(15) . ? C10B N4B 1.475(13) . ? N4B C11B 1.493(13) . ? C11B C12B 1.507(16) . ? C1C C2C 1.564(19) . ? C2C N3C 1.474(14) . ? N3C C3C 1.492(17) . ? C3C C4C 1.509(16) . ? C4C C9C 1.387(16) . ? C4C C5C 1.402(14) . ? C5C C6C 1.364(18) . ? C6C C7C 1.375(17) . ? C7C C8C 1.386(13) . ? C8C C9C 1.383(16) . ? C8C C10C 1.504(15) . ? C10C N4C 1.503(15) . ? N4C C11C 1.500(16) . ? C11C C12C 1.49(2) . ? O1 C1 1.262(12) . ? O2 C1 1.261(12) . ? O3 C1 1.305(12) . ? O41 C42 1.376(16) . ? O51 C52 1.389(14) . ? Cl1 O13 1.390(10) . ? Cl1 O14 1.398(16) . ? Cl1 O12 1.427(12) . ? Cl1 O11 1.414(10) . ? Cl2 O24 1.361(14) . ? Cl2 O23 1.39(2) . ? Cl2 O21 1.405(7) . ? Cl2 O22 1.435(8) . ? O71 C72 1.39(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 Ni1 N1 176.0(3) . . ? O1 Ni1 N3A 99.3(3) . . ? N1 Ni1 N3A 82.1(4) . . ? O1 Ni1 N3C 96.5(3) . . ? N1 Ni1 N3C 83.6(4) . . ? N3A Ni1 N3C 154.0(4) . . ? O1 Ni1 N3B 91.9(3) . . ? N1 Ni1 N3B 84.1(3) . . ? N3A Ni1 N3B 100.8(3) . . ? N3C Ni1 N3B 99.2(3) . . ? O1 Ni1 O41 84.6(3) . . ? N1 Ni1 O41 99.3(3) . . ? N3A Ni1 O41 85.1(3) . . ? N3C Ni1 O41 76.0(3) . . ? N3B Ni1 O41 173.6(3) . . ? O1 Ni1 Ni2 10.0(2) . . ? N1 Ni1 Ni2 174.0(3) . . ? N3A Ni1 Ni2 94.9(2) . . ? N3C Ni1 Ni2 97.2(3) . . ? N3B Ni1 Ni2 101.6(2) . . ? O41 Ni1 Ni2 75.2(2) . . ? O2 Ni2 N2 174.3(4) . . ? O2 Ni2 N4C 96.7(3) . . ? N2 Ni2 N4C 82.5(4) . . ? O2 Ni2 N4B 90.2(3) . . ? N2 Ni2 N4B 84.3(4) . . ? N4C Ni2 N4B 96.2(4) . . ? O2 Ni2 O51 87.3(3) . . ? N2 Ni2 O51 98.3(3) . . ? N4C Ni2 O51 87.4(3) . . ? N4B Ni2 O51 175.8(4) . . ? O2 Ni2 N4A 99.5(4) . . ? N2 Ni2 N4A 82.7(4) . . ? N4C Ni2 N4A 159.0(4) . . ? N4B Ni2 N4A 97.1(3) . . ? O51 Ni2 N4A 80.1(4) . . ? O2 Ni2 Ni1 10.61(19) . . ? N2 Ni2 Ni1 175.0(3) . . ? N4C Ni2 Ni1 96.8(3) . . ? N4B Ni2 Ni1 100.7(2) . . ? O51 Ni2 Ni1 76.7(2) . . ? N4A Ni2 Ni1 96.7(3) . . ? C1C N1 C1A 115.3(9) . . ? C1C N1 C1B 111.1(9) . . ? C1A N1 C1B 108.6(8) . . ? C1C N1 Ni1 105.4(7) . . ? C1A N1 Ni1 109.1(7) . . ? C1B N1 Ni1 106.9(7) . . ? C2A C1A N1 110.6(10) . . ? N3A C2A C1A 111.0(11) . . ? C2A N3A C3A 111.8(9) . . ? C2A N3A Ni1 102.0(6) . . ? C3A N3A Ni1 118.7(7) . . ? C4A C3A N3A 115.3(11) . . ? C9A C4A C5A 118.7(13) . . ? C9A C4A C3A 120.7(13) . . ? C5A C4A C3A 120.4(15) . . ? C6A C5A C4A 116.8(16) . . ? C7A C6A C5A 124.0(14) . . ? C6A C7A C8A 120.3(12) . . ? C7A C8A C9A 118.1(14) . . ? C7A C8A C10A 118.1(13) . . ? C9A C8A C10A 123.9(14) . . ? C4A C9A C8A 122.2(12) . . ? N4A C10A C8A 118.7(11) . . ? C10A N4A C11A 110.1(10) . . ? C10A N4A Ni2 133.1(9) . . ? C11A N4A Ni2 103.4(8) . . ? C12A C11A N4A 114.0(11) . . ? C11A C12A N2 112.1(11) . . ? C12C N2 C12B 110.0(10) . . ? C12C N2 C12A 110.2(9) . . ? C12B N2 C12A 114.6(9) . . ? C12C N2 Ni2 108.9(7) . . ? C12B N2 Ni2 108.8(7) . . ? C12A N2 Ni2 104.1(8) . . ? C2B C1B N1 108.5(9) . . ? N3B C2B C1B 109.8(8) . . ? C2B N3B C3B 110.2(7) . . ? C2B N3B Ni1 103.9(6) . . ? C3B N3B Ni1 120.5(7) . . ? C4B C3B N3B 115.0(8) . . ? C9B C4B C5B 118.4(10) . . ? C9B C4B C3B 120.2(9) . . ? C5B C4B C3B 121.4(9) . . ? C4B C5B C6B 119.5(10) . . ? C7B C6B C5B 120.2(11) . . ? C6B C7B C8B 121.7(10) . . ? C9B C8B C7B 116.4(9) . . ? C9B C8B C10B 121.3(9) . . ? C7B C8B C10B 122.3(10) . . ? C8B C9B C4B 123.8(10) . . ? N4B C10B C8B 116.8(8) . . ? C10B N4B C11B 109.5(7) . . ? C10B N4B Ni2 119.3(7) . . ? C11B N4B Ni2 103.4(6) . . ? N4B C11B C12B 110.1(8) . . ? N2 C12B C11B 113.5(10) . . ? N1 C1C C2C 109.0(9) . . ? N3C C2C C1C 110.1(9) . . ? C2C N3C C3C 112.0(9) . . ? C2C N3C Ni1 108.6(7) . . ? C3C N3C Ni1 120.9(7) . . ? N3C C3C C4C 111.7(10) . . ? C9C C4C C5C 118.5(11) . . ? C9C C4C C3C 121.2(9) . . ? C5C C4C C3C 120.3(10) . . ? C6C C5C C4C 120.7(11) . . ? C5C C6C C7C 119.9(9) . . ? C8C C7C C6C 121.0(11) . . ? C7C C8C C9C 118.8(9) . . ? C7C C8C C10C 119.4(10) . . ? C9C C8C C10C 121.7(9) . . ? C8C C9C C4C 121.1(9) . . ? C8C C10C N4C 112.6(9) . . ? C11C N4C C10C 112.3(10) . . ? C11C N4C Ni2 106.7(7) . . ? C10C N4C Ni2 120.1(6) . . ? C12C C11C N4C 110.1(12) . . ? N2 C12C C11C 107.1(9) . . ? C1 O1 Ni1 140.3(7) . . ? C1 O2 Ni2 137.7(6) . . ? O1 C1 O2 118.3(9) . . ? O1 C1 O3 122.0(9) . . ? O2 C1 O3 119.7(9) . . ? C42 O41 Ni1 157.3(8) . . ? C52 O51 Ni2 136.1(9) . . ? O13 Cl1 O14 108.8(9) . . ? O13 Cl1 O12 104.4(9) . . ? O14 Cl1 O12 112.6(12) . . ? O13 Cl1 O11 113.3(7) . . ? O14 Cl1 O11 109.7(10) . . ? O12 Cl1 O11 107.9(6) . . ? O24 Cl2 O23 102.5(14) . . ? O24 Cl2 O21 110.8(8) . . ? O23 Cl2 O21 109.3(9) . . ? O24 Cl2 O22 113.3(8) . . ? O23 Cl2 O22 109.0(8) . . ? O21 Cl2 O22 111.4(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ni1 Ni2 O2 9.2(14) . . . . ? N1 Ni1 Ni2 O2 -167(3) . . . . ? N3A Ni1 Ni2 O2 -107.2(11) . . . . ? N3C Ni1 Ni2 O2 95.9(11) . . . . ? N3B Ni1 Ni2 O2 -5.1(11) . . . . ? O41 Ni1 Ni2 O2 169.3(11) . . . . ? O1 Ni1 Ni2 N2 -163(4) . . . . ? N1 Ni1 Ni2 N2 21(4) . . . . ? N3A Ni1 Ni2 N2 81(3) . . . . ? N3C Ni1 Ni2 N2 -76(3) . . . . ? N3B Ni1 Ni2 N2 -177(3) . . . . ? O41 Ni1 Ni2 N2 -3(3) . . . . ? O1 Ni1 Ni2 N4C -81.0(11) . . . . ? N1 Ni1 Ni2 N4C 103(2) . . . . ? N3A Ni1 Ni2 N4C 162.7(3) . . . . ? N3C Ni1 Ni2 N4C 5.7(4) . . . . ? N3B Ni1 Ni2 N4C -95.2(4) . . . . ? O41 Ni1 Ni2 N4C 79.1(4) . . . . ? O1 Ni1 Ni2 N4B 16.6(11) . . . . ? N1 Ni1 Ni2 N4B -160(2) . . . . ? N3A Ni1 Ni2 N4B -99.7(3) . . . . ? N3C Ni1 Ni2 N4B 103.3(4) . . . . ? N3B Ni1 Ni2 N4B 2.4(3) . . . . ? O41 Ni1 Ni2 N4B 176.7(3) . . . . ? O1 Ni1 Ni2 O51 -166.7(11) . . . . ? N1 Ni1 Ni2 O51 17(2) . . . . ? N3A Ni1 Ni2 O51 76.9(3) . . . . ? N3C Ni1 Ni2 O51 -80.0(3) . . . . ? N3B Ni1 Ni2 O51 179.0(3) . . . . ? O41 Ni1 Ni2 O51 -6.6(3) . . . . ? O1 Ni1 Ni2 N4A 115.2(11) . . . . ? N1 Ni1 Ni2 N4A -61(2) . . . . ? N3A Ni1 Ni2 N4A -1.2(4) . . . . ? N3C Ni1 Ni2 N4A -158.1(4) . . . . ? N3B Ni1 Ni2 N4A 100.9(3) . . . . ? O41 Ni1 Ni2 N4A -84.7(4) . . . . ? O1 Ni1 N1 C1C 118(5) . . . . ? N3A Ni1 N1 C1C -132.2(8) . . . . ? N3C Ni1 N1 C1C 26.0(7) . . . . ? N3B Ni1 N1 C1C 126.0(8) . . . . ? O41 Ni1 N1 C1C -48.6(8) . . . . ? Ni2 Ni1 N1 C1C -72(3) . . . . ? O1 Ni1 N1 C1A -118(5) . . . . ? N3A Ni1 N1 C1A -7.9(7) . . . . ? N3C Ni1 N1 C1A 150.4(7) . . . . ? N3B Ni1 N1 C1A -109.7(7) . . . . ? O41 Ni1 N1 C1A 75.7(7) . . . . ? Ni2 Ni1 N1 C1A 53(3) . . . . ? O1 Ni1 N1 C1B -1(5) . . . . ? N3A Ni1 N1 C1B 109.4(7) . . . . ? N3C Ni1 N1 C1B -92.3(7) . . . . ? N3B Ni1 N1 C1B 7.6(6) . . . . ? O41 Ni1 N1 C1B -167.0(7) . . . . ? Ni2 Ni1 N1 C1B 169.8(19) . . . . ? C1C N1 C1A C2A 99.9(11) . . . . ? C1B N1 C1A C2A -134.6(10) . . . . ? Ni1 N1 C1A C2A -18.4(11) . . . . ? N1 C1A C2A N3A 50.4(12) . . . . ? C1A C2A N3A C3A 178.8(9) . . . . ? C1A C2A N3A Ni1 -53.3(10) . . . . ? O1 Ni1 N3A C2A -151.2(7) . . . . ? N1 Ni1 N3A C2A 32.6(7) . . . . ? N3C Ni1 N3A C2A -24.5(12) . . . . ? N3B Ni1 N3A C2A 115.1(8) . . . . ? O41 Ni1 N3A C2A -67.5(8) . . . . ? Ni2 Ni1 N3A C2A -142.1(7) . . . . ? O1 Ni1 N3A C3A -27.8(8) . . . . ? N1 Ni1 N3A C3A 156.0(8) . . . . ? N3C Ni1 N3A C3A 98.8(10) . . . . ? N3B Ni1 N3A C3A -121.6(8) . . . . ? O41 Ni1 N3A C3A 55.8(7) . . . . ? Ni2 Ni1 N3A C3A -18.8(7) . . . . ? C2A N3A C3A C4A -160.6(11) . . . . ? Ni1 N3A C3A C4A 81.1(12) . . . . ? N3A C3A C4A C9A -134.7(12) . . . . ? N3A C3A C4A C5A 50.9(16) . . . . ? C9A C4A C5A C6A -0.4(19) . . . . ? C3A C4A C5A C6A 174.1(12) . . . . ? C4A C5A C6A C7A 1(2) . . . . ? C5A C6A C7A C8A -1(2) . . . . ? C6A C7A C8A C9A 2(2) . . . . ? C6A C7A C8A C10A -176.8(14) . . . . ? C5A C4A C9A C8A 0.7(19) . . . . ? C3A C4A C9A C8A -173.8(12) . . . . ? C7A C8A C9A C4A -1.3(19) . . . . ? C10A C8A C9A C4A 177.0(13) . . . . ? C7A C8A C10A N4A -148.2(14) . . . . ? C9A C8A C10A N4A 34(2) . . . . ? C8A C10A N4A C11A -173.7(15) . . . . ? C8A C10A N4A Ni2 53(2) . . . . ? O2 Ni2 N4A C10A -46.2(13) . . . . ? N2 Ni2 N4A C10A 128.5(13) . . . . ? N4C Ni2 N4A C10A 173.9(12) . . . . ? N4B Ni2 N4A C10A 45.2(13) . . . . ? O51 Ni2 N4A C10A -131.7(13) . . . . ? Ni1 Ni2 N4A C10A -56.5(13) . . . . ? O2 Ni2 N4A C11A 178.9(8) . . . . ? N2 Ni2 N4A C11A -6.5(8) . . . . ? N4C Ni2 N4A C11A 38.9(15) . . . . ? N4B Ni2 N4A C11A -89.8(8) . . . . ? O51 Ni2 N4A C11A 93.3(8) . . . . ? Ni1 Ni2 N4A C11A 168.5(8) . . . . ? C10A N4A C11A C12A -167.8(13) . . . . ? Ni2 N4A C11A C12A -21.2(15) . . . . ? N4A C11A C12A N2 50.7(18) . . . . ? C11A C12A N2 C12C -169.3(12) . . . . ? C11A C12A N2 C12B 66.0(15) . . . . ? C11A C12A N2 Ni2 -52.7(13) . . . . ? O2 Ni2 N2 C12C -101(3) . . . . ? N4C Ni2 N2 C12C -18.2(8) . . . . ? N4B Ni2 N2 C12C -115.2(8) . . . . ? O51 Ni2 N2 C12C 68.1(8) . . . . ? N4A Ni2 N2 C12C 146.9(8) . . . . ? Ni1 Ni2 N2 C12C 64(4) . . . . ? O2 Ni2 N2 C12B 19(4) . . . . ? N4C Ni2 N2 C12B 101.8(8) . . . . ? N4B Ni2 N2 C12B 4.8(8) . . . . ? O51 Ni2 N2 C12B -171.9(8) . . . . ? N4A Ni2 N2 C12B -93.2(8) . . . . ? Ni1 Ni2 N2 C12B -176(3) . . . . ? O2 Ni2 N2 C12A 142(3) . . . . ? N4C Ni2 N2 C12A -135.6(7) . . . . ? N4B Ni2 N2 C12A 127.4(7) . . . . ? O51 Ni2 N2 C12A -49.4(7) . . . . ? N4A Ni2 N2 C12A 29.4(7) . . . . ? Ni1 Ni2 N2 C12A -53(4) . . . . ? C1C N1 C1B C2B -150.3(9) . . . . ? C1A N1 C1B C2B 81.9(10) . . . . ? Ni1 N1 C1B C2B -35.7(10) . . . . ? N1 C1B C2B N3B 58.1(12) . . . . ? C1B C2B N3B C3B -178.6(9) . . . . ? C1B C2B N3B Ni1 -48.2(10) . . . . ? O1 Ni1 N3B C2B -159.2(6) . . . . ? N1 Ni1 N3B C2B 21.4(6) . . . . ? N3A Ni1 N3B C2B -59.4(7) . . . . ? N3C Ni1 N3B C2B 103.9(7) . . . . ? O41 Ni1 N3B C2B 144(3) . . . . ? Ni2 Ni1 N3B C2B -156.8(6) . . . . ? O1 Ni1 N3B C3B -35.2(8) . . . . ? N1 Ni1 N3B C3B 145.4(8) . . . . ? N3A Ni1 N3B C3B 64.6(8) . . . . ? N3C Ni1 N3B C3B -132.1(8) . . . . ? O41 Ni1 N3B C3B -92(3) . . . . ? Ni2 Ni1 N3B C3B -32.8(8) . . . . ? C2B N3B C3B C4B -164.3(9) . . . . ? Ni1 N3B C3B C4B 74.7(11) . . . . ? N3B C3B C4B C9B -118.7(10) . . . . ? N3B C3B C4B C5B 63.3(13) . . . . ? C9B C4B C5B C6B -0.8(14) . . . . ? C3B C4B C5B C6B 177.3(9) . . . . ? C4B C5B C6B C7B -0.6(15) . . . . ? C5B C6B C7B C8B 0.7(15) . . . . ? C6B C7B C8B C9B 0.5(14) . . . . ? C6B C7B C8B C10B -179.0(9) . . . . ? C7B C8B C9B C4B -2.0(13) . . . . ? C10B C8B C9B C4B 177.5(8) . . . . ? C5B C4B C9B C8B 2.2(14) . . . . ? C3B C4B C9B C8B -176.0(8) . . . . ? C9B C8B C10B N4B 121.7(10) . . . . ? C7B C8B C10B N4B -58.8(13) . . . . ? C8B C10B N4B C11B 165.4(9) . . . . ? C8B C10B N4B Ni2 -75.8(11) . . . . ? O2 Ni2 N4B C10B 31.7(7) . . . . ? N2 Ni2 N4B C10B -149.7(8) . . . . ? N4C Ni2 N4B C10B 128.5(7) . . . . ? O51 Ni2 N4B C10B -21(5) . . . . ? N4A Ni2 N4B C10B -67.9(8) . . . . ? Ni1 Ni2 N4B C10B 30.4(7) . . . . ? O2 Ni2 N4B C11B 153.6(6) . . . . ? N2 Ni2 N4B C11B -27.8(7) . . . . ? N4C Ni2 N4B C11B -109.6(6) . . . . ? O51 Ni2 N4B C11B 101(5) . . . . ? N4A Ni2 N4B C11B 54.1(7) . . . . ? Ni1 Ni2 N4B C11B 152.3(6) . . . . ? C10B N4B C11B C12B 174.3(10) . . . . ? Ni2 N4B C11B C12B 46.1(10) . . . . ? C12C N2 C12B C11B 139.5(10) . . . . ? C12A N2 C12B C11B -95.8(12) . . . . ? Ni2 N2 C12B C11B 20.3(12) . . . . ? N4B C11B C12B N2 -46.5(13) . . . . ? C1A N1 C1C C2C -168.3(10) . . . . ? C1B N1 C1C C2C 67.5(11) . . . . ? Ni1 N1 C1C C2C -48.0(10) . . . . ? N1 C1C C2C N3C 52.2(12) . . . . ? C1C C2C N3C C3C -163.8(9) . . . . ? C1C C2C N3C Ni1 -27.7(10) . . . . ? O1 Ni1 N3C C2C -174.4(7) . . . . ? N1 Ni1 N3C C2C 1.6(7) . . . . ? N3A Ni1 N3C C2C 58.4(11) . . . . ? N3B Ni1 N3C C2C -81.4(7) . . . . ? O41 Ni1 N3C C2C 102.9(7) . . . . ? Ni2 Ni1 N3C C2C 175.6(7) . . . . ? O1 Ni1 N3C C3C -42.9(9) . . . . ? N1 Ni1 N3C C3C 133.0(9) . . . . ? N3A Ni1 N3C C3C -170.1(8) . . . . ? N3B Ni1 N3C C3C 50.1(9) . . . . ? O41 Ni1 N3C C3C -125.7(9) . . . . ? Ni2 Ni1 N3C C3C -52.9(8) . . . . ? C2C N3C C3C C4C -138.6(8) . . . . ? Ni1 N3C C3C C4C 91.4(9) . . . . ? N3C C3C C4C C9C -106.6(12) . . . . ? N3C C3C C4C C5C 72.6(13) . . . . ? C9C C4C C5C C6C -1.1(18) . . . . ? C3C C4C C5C C6C 179.7(12) . . . . ? C4C C5C C6C C7C 1(2) . . . . ? C5C C6C C7C C8C 0.1(19) . . . . ? C6C C7C C8C C9C -0.4(17) . . . . ? C6C C7C C8C C10C -178.1(11) . . . . ? C7C C8C C9C C4C -0.1(16) . . . . ? C10C C8C C9C C4C 177.6(10) . . . . ? C5C C4C C9C C8C 0.8(16) . . . . ? C3C C4C C9C C8C -180.0(10) . . . . ? C7C C8C C10C N4C -67.2(13) . . . . ? C9C C8C C10C N4C 115.1(11) . . . . ? C8C C10C N4C C11C 142.8(9) . . . . ? C8C C10C N4C Ni2 -90.6(9) . . . . ? O2 Ni2 N4C C11C 163.4(8) . . . . ? N2 Ni2 N4C C11C -10.8(8) . . . . ? N4B Ni2 N4C C11C 72.5(8) . . . . ? O51 Ni2 N4C C11C -109.6(8) . . . . ? N4A Ni2 N4C C11C -56.3(14) . . . . ? Ni1 Ni2 N4C C11C 174.1(7) . . . . ? O2 Ni2 N4C C10C 34.2(8) . . . . ? N2 Ni2 N4C C10C -140.0(8) . . . . ? N4B Ni2 N4C C10C -56.7(8) . . . . ? O51 Ni2 N4C C10C 121.2(7) . . . . ? N4A Ni2 N4C C10C 174.5(9) . . . . ? Ni1 Ni2 N4C C10C 44.9(7) . . . . ? C10C N4C C11C C12C 172.2(8) . . . . ? Ni2 N4C C11C C12C 38.6(10) . . . . ? C12B N2 C12C C11C -75.2(12) . . . . ? C12A N2 C12C C11C 157.5(10) . . . . ? Ni2 N2 C12C C11C 44.0(11) . . . . ? N4C C11C C12C N2 -55.6(12) . . . . ? N1 Ni1 O1 C1 -176(4) . . . . ? N3A Ni1 O1 C1 74.6(10) . . . . ? N3C Ni1 O1 C1 -84.7(10) . . . . ? N3B Ni1 O1 C1 175.8(10) . . . . ? O41 Ni1 O1 C1 -9.5(10) . . . . ? Ni2 Ni1 O1 C1 9.8(8) . . . . ? N2 Ni2 O2 C1 167(3) . . . . ? N4C Ni2 O2 C1 84.9(10) . . . . ? N4B Ni2 O2 C1 -178.8(10) . . . . ? O51 Ni2 O2 C1 -2.2(10) . . . . ? N4A Ni2 O2 C1 -81.6(10) . . . . ? Ni1 Ni2 O2 C1 -6.2(7) . . . . ? Ni1 O1 C1 O2 -173.9(6) . . . . ? Ni1 O1 C1 O3 3.6(16) . . . . ? Ni2 O2 C1 O1 -179.6(6) . . . . ? Ni2 O2 C1 O3 2.8(15) . . . . ? O1 Ni1 O41 C42 178(3) . . . . ? N1 Ni1 O41 C42 -3(3) . . . . ? N3A Ni1 O41 C42 78(3) . . . . ? N3C Ni1 O41 C42 -84(3) . . . . ? N3B Ni1 O41 C42 -125(3) . . . . ? Ni2 Ni1 O41 C42 174(3) . . . . ? O2 Ni2 O51 C52 120.5(13) . . . . ? N2 Ni2 O51 C52 -58.4(13) . . . . ? N4C Ni2 O51 C52 23.6(13) . . . . ? N4B Ni2 O51 C52 173(4) . . . . ? N4A Ni2 O51 C52 -139.4(13) . . . . ? Ni1 Ni2 O51 C52 121.3(13) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O41 H41 O3 0.65 1.97 2.552(12) 150.2 . O51 H51 O3 0.84 1.73 2.513(11) 155.1 . N3A H3A O12 0.93 2.36 3.184(15) 147.3 1_565 N4B H4B O13 0.93 2.40 3.295(14) 162.5 2 N3B H3B O22 0.93 2.46 3.296(12) 150.2 . N3C H3C O41 0.93 2.31 2.825(14) 114.4 . _diffrn_measured_fraction_theta_max 0.866 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.866 _refine_diff_density_max 0.673 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.084 data_Complex_4 #(y317) _database_code_CSD 181030 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41.50 H62.25 Cl3 N9.75 Ni2 O15' _chemical_formula_weight 1161.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n 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 16.790(3) _cell_length_b 17.247(3) _cell_length_c 19.352(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.757(12) _cell_angle_gamma 90.00 _cell_volume 5167.5(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.19 _cell_measurement_theta_max 12.46 _exptl_crystal_description irregular _exptl_crystal_colour green _exptl_crystal_size_max .3 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2426 _exptl_absorpt_coefficient_mu 0.957 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.78922 _exptl_absorpt_correction_T_max 0.98914 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6962 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.1186 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 22.50 _reflns_number_total 6694 _reflns_number_gt 3651 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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. The methylcarbonate anion is disordered 60:40 over the two equivalent syn anti coordination sites bridging the nickel ions. Possibly as a consequence of this, the saturated sections of one of the strands of the cryptate ligand is also disordered 60:40 between two related positions. One of the three perchlorate ions is ordered, one shows a 60:40 disorder over two positions related by rotation about one of the Cl-O bonds, and the third has been modelled as split over four overlapping positions (40:30:20:10). ; _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^)+(0.1071P)^2^+15.9739P] 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 6694 _refine_ls_number_parameters 738 _refine_ls_number_restraints 1515 _refine_ls_R_factor_all 0.1621 _refine_ls_R_factor_gt 0.0814 _refine_ls_wR_factor_ref 0.2332 _refine_ls_wR_factor_gt 0.1891 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.683 _refine_ls_shift/su_mean 0.010 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 0.59857(8) -0.11606(8) 0.22680(7) 0.0326(4) Uani 1 1 d U . . Ni2 Ni 0.37802(8) 0.12152(7) 0.24568(6) 0.0292(4) Uani 1 1 d U A . N1 N 0.6909(5) -0.1926(5) 0.2190(4) 0.0391(18) Uani 1 1 d U A . C1A C 0.7371(8) -0.2252(7) 0.2945(6) 0.057(3) Uani 0.60 1 d PU A 1 H1A1 H 0.7946 -0.2450 0.2999 0.050 Uiso 0.60 1 calc PR A 1 H1A2 H 0.7037 -0.2680 0.3044 0.050 Uiso 0.60 1 calc PR A 1 C2A C 0.7467(16) -0.1528(13) 0.3513(13) 0.048(5) Uani 0.60 1 d PU A 1 H2A1 H 0.7771 -0.1699 0.4038 0.050 Uiso 0.60 1 calc PR A 1 H2A2 H 0.7807 -0.1107 0.3411 0.050 Uiso 0.60 1 calc PR A 1 N3A N 0.6599(10) -0.1246(9) 0.3398(8) 0.035(3) Uani 0.60 1 d PU A 1 H3A H 0.6666 -0.0743 0.3586 0.050 Uiso 0.60 1 calc PR A 1 C3A C 0.6170(12) -0.1696(11) 0.3810(11) 0.039(4) Uani 0.60 1 d PU A 1 H3A1 H 0.6609 -0.1857 0.4301 0.050 Uiso 0.60 1 calc PR A 1 H3A2 H 0.5916 -0.2172 0.3523 0.050 Uiso 0.60 1 calc PR A 1 C4A C 0.5440(7) -0.1225(7) 0.3942(5) 0.041(2) Uani 0.60 1 d PU A 1 C1A' C 0.7371(8) -0.2252(7) 0.2945(6) 0.057(3) Uani 0.40 1 d PU A 2 H1A3 H 0.7174 -0.2794 0.2937 0.050 Uiso 0.40 1 calc PR A 2 H1A4 H 0.7992 -0.2273 0.3032 0.050 Uiso 0.40 1 calc PR A 2 C2A' C 0.731(2) -0.1904(18) 0.354(2) 0.042(6) Uani 0.40 1 d PU A 2 H2A3 H 0.7686 -0.1442 0.3670 0.050 Uiso 0.40 1 calc PR A 2 H2A4 H 0.7509 -0.2263 0.3969 0.050 Uiso 0.40 1 calc PR A 2 N3A' N 0.6399(16) -0.1662(14) 0.3386(13) 0.033(4) Uani 0.40 1 d PU A 2 H3A' H 0.6077 -0.2110 0.3349 0.050 Uiso 0.40 1 calc PR A 2 C3A' C 0.6375(17) -0.1212(19) 0.4019(14) 0.039(4) Uani 0.40 1 d PU A 2 H3A3 H 0.6568 -0.0673 0.4000 0.050 Uiso 0.40 1 calc PR A 2 H3A4 H 0.6755 -0.1449 0.4500 0.050 Uiso 0.40 1 calc PR A 2 C4A' C 0.5440(7) -0.1225(7) 0.3942(5) 0.041(2) Uani 0.40 1 d PU A 2 C5A C 0.4886(7) -0.1738(6) 0.4079(5) 0.037(2) Uani 1 1 d U . . H5A H 0.5004 -0.2278 0.4107 0.050 Uiso 1 1 calc R A 1 C6A C 0.4174(8) -0.1473(7) 0.4174(6) 0.046(3) Uani 1 1 d U A . H6A H 0.3793 -0.1831 0.4261 0.050 Uiso 1 1 calc R . . C7A C 0.3998(8) -0.0698(7) 0.4145(6) 0.050(3) Uani 1 1 d U . . H7A H 0.3497 -0.0519 0.4212 0.050 Uiso 1 1 calc R A 1 C9A C 0.5253(7) -0.0447(6) 0.3917(5) 0.042(2) Uani 1 1 d U . . H9A H 0.5628 -0.0087 0.3824 0.050 Uiso 1 1 calc R A 1 C8A C 0.4548(9) -0.0177(6) 0.4020(5) 0.048(2) Uani 0.60 1 d PU A 1 C10A C 0.4677(14) 0.0721(10) 0.4110(9) 0.038(4) Uani 0.60 1 d PU A 1 H10A H 0.4761 0.0880 0.4625 0.050 Uiso 0.60 1 calc PR A 1 H10B H 0.5193 0.0879 0.4016 0.050 Uiso 0.60 1 calc PR A 1 N4A N 0.3910(12) 0.1088(10) 0.3571(9) 0.041(4) Uani 0.60 1 d PU A 1 H4A H 0.3416 0.0864 0.3591 0.050 Uiso 0.60 1 calc PR A 1 C11A C 0.3980(10) 0.1946(6) 0.3819(6) 0.064(3) Uani 0.60 1 d PU A 1 H11A H 0.4036 0.1996 0.4345 0.050 Uiso 0.60 1 calc PR A 1 H11B H 0.4475 0.2208 0.3759 0.050 Uiso 0.60 1 calc PR A 1 C8A' C 0.4548(9) -0.0177(6) 0.4020(5) 0.048(2) Uani 0.40 1 d PU A 2 C10' C 0.403(2) 0.0611(16) 0.3983(16) 0.045(5) Uani 0.40 1 d PU A 2 H10C H 0.3401 0.0528 0.3702 0.050 Uiso 0.40 1 calc PR A 2 H10D H 0.4120 0.0789 0.4495 0.050 Uiso 0.40 1 calc PR A 2 N4A' N 0.4362(19) 0.1200(15) 0.3595(13) 0.042(4) Uani 0.40 1 d PU A 2 H4A' H 0.4961 0.1206 0.3768 0.050 Uiso 0.40 1 calc PR A 2 C11' C 0.3980(10) 0.1946(6) 0.3819(6) 0.064(3) Uani 0.40 1 d PU A 2 H11C H 0.3917 0.1835 0.4297 0.050 Uiso 0.40 1 calc PR A 2 H11D H 0.4416 0.2364 0.3920 0.050 Uiso 0.40 1 calc PR A 2 C12A C 0.3141(8) 0.2260(6) 0.3287(6) 0.054(3) Uani 1 1 d U . . H12A H 0.2660 0.1968 0.3339 0.050 Uiso 1 1 calc R A 1 H12B H 0.3086 0.2811 0.3408 0.050 Uiso 1 1 calc R A 1 N2 N 0.3091(6) 0.2198(5) 0.2523(5) 0.0401(19) Uani 1 1 d U A . C1B C 0.6418(7) -0.2522(6) 0.1632(6) 0.043(2) Uani 1 1 d U . . H1B1 H 0.6785 -0.2985 0.1683 0.050 Uiso 1 1 calc R A . H1B2 H 0.6258 -0.2313 0.1119 0.050 Uiso 1 1 calc R . . C2B C 0.5606(7) -0.2751(6) 0.1750(6) 0.045(3) Uani 1 1 d U A . H2B1 H 0.5245 -0.3095 0.1338 0.050 Uiso 1 1 calc R . . H2B2 H 0.5764 -0.3038 0.2228 0.050 Uiso 1 1 calc R . . N3B N 0.5117(5) -0.2052(4) 0.1769(4) 0.0325(18) Uani 1 1 d U A . H3B H 0.4855 -0.1903 0.1269 0.039 Uiso 1 1 calc R . . C3B C 0.4370(7) -0.2246(6) 0.1988(6) 0.037(2) Uani 1 1 d U . . H3B1 H 0.4192 -0.2789 0.1848 0.050 Uiso 1 1 calc R A . H3B2 H 0.4560 -0.2201 0.2539 0.050 Uiso 1 1 calc R . . C4B C 0.3611(7) -0.1722(6) 0.1617(5) 0.034(2) Uani 1 1 d U A . C5B C 0.3105(7) -0.1818(6) 0.0861(5) 0.038(2) Uani 1 1 d U . . H5B H 0.3264 -0.2192 0.0578 0.050 Uiso 1 1 calc R A . C6B C 0.2383(8) -0.1382(7) 0.0523(6) 0.049(3) Uani 1 1 d U A . H6B H 0.2037 -0.1458 0.0007 0.050 Uiso 1 1 calc R . . C7B C 0.2151(7) -0.0827(7) 0.0928(6) 0.045(3) Uani 1 1 d U . . H7B H 0.1650 -0.0519 0.0689 0.050 Uiso 1 1 calc R A . C8B C 0.2660(6) -0.0719(6) 0.1696(5) 0.033(2) Uani 1 1 d U A . C9B C 0.3372(6) -0.1165(6) 0.2020(5) 0.032(2) Uani 1 1 d U . . H9B H 0.3719 -0.1095 0.2537 0.050 Uiso 1 1 calc R A . C10B C 0.2388(7) -0.0122(6) 0.2126(6) 0.038(2) Uani 1 1 d U . . H10C' H 0.1762 -0.0182 0.2008 0.050 Uiso 1 1 calc R A . H10D' H 0.2698 -0.0220 0.2669 0.050 Uiso 1 1 calc R . . N4B N 0.2559(5) 0.0693(5) 0.1960(4) 0.0355(18) Uani 1 1 d U A . H4B H 0.2439 0.0697 0.1449 0.043 Uiso 1 1 calc R . . C11B C 0.1929(7) 0.1242(6) 0.2054(7) 0.051(3) Uani 1 1 d U . . H11C' H 0.1900 0.1163 0.2551 0.050 Uiso 1 1 calc R A . H11D' H 0.1348 0.1143 0.1664 0.050 Uiso 1 1 calc R . . C12B C 0.2195(7) 0.2056(6) 0.1991(6) 0.048(3) Uani 1 1 d U A . H12C H 0.2152 0.2153 0.1474 0.050 Uiso 1 1 calc R . . H12D H 0.1801 0.2420 0.2097 0.050 Uiso 1 1 calc R . . C1C C 0.7507(7) -0.1464(7) 0.1931(6) 0.043(2) Uani 1 1 d U . . H1C1 H 0.8009 -0.1281 0.2371 0.050 Uiso 1 1 calc R A . H1C2 H 0.7725 -0.1800 0.1627 0.050 Uiso 1 1 calc R . . C2C C 0.7038(7) -0.0777(6) 0.1469(6) 0.046(3) Uani 1 1 d U A . H2C1 H 0.7438 -0.0463 0.1319 0.050 Uiso 1 1 calc R . . H2C2 H 0.6557 -0.0955 0.1010 0.050 Uiso 1 1 calc R . . N3C N 0.6694(5) -0.0302(5) 0.1945(5) 0.0387(19) Uani 1 1 d U A . H3C H 0.6272 0.0010 0.1604 0.046 Uiso 1 1 calc R . . C3C C 0.7324(7) 0.0241(6) 0.2424(6) 0.044(3) Uani 1 1 d U . . H3C1 H 0.7498 0.0600 0.2109 0.050 Uiso 1 1 calc R A . H3C2 H 0.7845 -0.0049 0.2747 0.050 Uiso 1 1 calc R . . C4C C 0.6986(6) 0.0704(5) 0.2913(6) 0.033(2) Uani 1 1 d U A . C5C C 0.7370(7) 0.0623(6) 0.3692(6) 0.041(3) Uani 1 1 d U . . H5C H 0.7813 0.0252 0.3916 0.050 Uiso 1 1 calc R A . C6C C 0.7084(7) 0.1102(6) 0.4133(6) 0.044(3) Uani 1 1 d U A . H6C H 0.7339 0.1052 0.4663 0.050 Uiso 1 1 calc R . . C7C C 0.6458(7) 0.1632(6) 0.3826(6) 0.040(2) Uani 1 1 d U . . H7C H 0.6282 0.1949 0.4143 0.050 Uiso 1 1 calc R A . C8C C 0.6058(6) 0.1723(5) 0.3044(6) 0.032(2) Uani 1 1 d U A . C9C C 0.6344(6) 0.1255(5) 0.2597(5) 0.030(2) Uani 1 1 d U . . H9C H 0.6096 0.1314 0.2068 0.050 Uiso 1 1 calc R A . C10C C 0.5382(7) 0.2349(6) 0.2692(6) 0.044(2) Uani 1 1 d U . . H10E H 0.5284 0.2638 0.3095 0.050 Uiso 1 1 calc R A . H10F H 0.5604 0.2719 0.2419 0.050 Uiso 1 1 calc R . . N4C N 0.4547(5) 0.2030(5) 0.2168(4) 0.0349(18) Uani 1 1 d U A . H4C H 0.4671 0.1794 0.1789 0.042 Uiso 1 1 calc R . . C11C C 0.3917(7) 0.2645(6) 0.1794(6) 0.043(3) Uani 1 1 d U . . H11E H 0.3482 0.2448 0.1317 0.050 Uiso 1 1 calc R A . H11F H 0.4217 0.3092 0.1679 0.050 Uiso 1 1 calc R . . C12C C 0.3482(8) 0.2897(6) 0.2302(6) 0.046(3) Uani 1 1 d U A . H12E H 0.3025 0.3280 0.2042 0.050 Uiso 1 1 calc R . . H12F H 0.3908 0.3146 0.2756 0.050 Uiso 1 1 calc R . . C1 C 0.4606(7) 0.0050(6) 0.1876(6) 0.036(2) Uani 0.60 1 d PU A 1 O1 O 0.4976(7) -0.0419(7) 0.1749(7) 0.034(3) Uiso 0.60 1 d PU A 1 O2 O 0.4542(6) 0.0307(6) 0.2484(6) 0.026(2) Uiso 0.60 1 d PU A 1 O3 O 0.3952(7) 0.0466(6) 0.1278(6) 0.036(3) Uiso 0.60 1 d PU A 1 C2 C 0.3941(10) 0.0153(7) 0.0535(6) 0.071(4) Uani 0.60 1 d PU A 1 H2A H 0.4449 0.0344 0.0456 0.050 Uiso 0.60 1 calc PR A 1 H2B H 0.3416 0.0330 0.0124 0.050 Uiso 0.60 1 calc PR A 1 H2C H 0.3951 -0.0415 0.0548 0.050 Uiso 0.60 1 calc PR A 1 C1' C 0.4606(7) 0.0050(6) 0.1876(6) 0.036(2) Uani 0.40 1 d PU A 2 O1' O 0.5227(10) -0.0385(9) 0.2440(8) 0.029(4) Uiso 0.40 1 d PU A 2 O2' O 0.4203(11) 0.0484(10) 0.1915(10) 0.035(4) Uiso 0.40 1 d PU A 2 O3' O 0.4745(10) -0.0236(9) 0.1242(9) 0.031(4) Uiso 0.40 1 d PU A 2 C2' C 0.3941(10) 0.0153(7) 0.0535(6) 0.071(4) Uani 0.40 1 d PU A 2 H2'1 H 0.3529 -0.0253 0.0266 0.050 Uiso 0.40 1 calc PR A 2 H2'2 H 0.4167 0.0402 0.0193 0.050 Uiso 0.40 1 calc PR A 2 H2'3 H 0.3650 0.0540 0.0725 0.050 Uiso 0.40 1 calc PR A 2 Cl1 Cl 0.55344(19) 0.17606(17) 0.04160(15) 0.0452(7) Uani 1 1 d DU . . O11 O 0.5063(5) 0.1996(5) 0.0855(4) 0.065(2) Uani 1 1 d DU . . O12 O 0.4964(5) 0.1419(5) -0.0266(4) 0.059(2) Uani 1 1 d DU . . O13 O 0.6171(6) 0.1227(6) 0.0821(4) 0.092(3) Uani 1 1 d DU . . O14 O 0.5902(6) 0.2421(5) 0.0227(5) 0.086(3) Uani 1 1 d DU . . Cl2 Cl 0.3238(2) 0.5482(2) 0.0829(2) 0.0675(10) Uani 0.60 1 d PDU B 1 O21 O 0.3235(6) 0.4708(5) 0.1068(6) 0.101(3) Uani 0.60 1 d PDU B 1 O22 O 0.2461(10) 0.5802(11) 0.0805(11) 0.108(6) Uani 0.60 1 d PDU B 1 O23 O 0.3399(14) 0.5476(11) 0.0194(9) 0.102(6) Uani 0.60 1 d PDU B 1 O24 O 0.3904(12) 0.5845(10) 0.1441(9) 0.115(7) Uani 0.60 1 d PDU B 1 Cl2' Cl 0.3238(2) 0.5482(2) 0.0829(2) 0.0675(10) Uani 0.40 1 d PDU C 2 O21' O 0.3235(6) 0.4708(5) 0.1068(6) 0.101(3) Uani 0.40 1 d PDU C 2 O22' O 0.314(2) 0.6042(14) 0.1283(16) 0.135(10) Uani 0.40 1 d PDU C 2 O23' O 0.2483(14) 0.5541(14) 0.0132(11) 0.107(8) Uani 0.40 1 d PDU C 2 O24' O 0.3947(15) 0.5676(18) 0.064(2) 0.127(10) Uani 0.40 1 d PDU C 2 Cl3 Cl 0.3537(5) -0.3545(4) 0.5164(4) 0.0417(19) Uiso 0.40 1 d PDU D 1 O31 O 0.3839(12) -0.3716(11) 0.5940(7) 0.185(8) Uiso 0.40 1 d PDU D 1 O32 O 0.4191(10) -0.3032(8) 0.5108(10) 0.168(7) Uiso 0.40 1 d PDU D 1 O33 O 0.361(2) -0.4216(11) 0.4772(14) 0.132(11) Uiso 0.40 1 d PDU D 1 O34 O 0.2779(13) -0.3125(17) 0.4815(17) 0.137(13) Uiso 0.40 1 d PDU D 1 Cl3A' Cl 0.3924(8) -0.3747(6) 0.5249(5) 0.061(3) Uiso 0.30 1 d PDU E 2 O31A' O 0.3839(12) -0.3716(11) 0.5940(7) 0.185(8) Uiso 0.30 1 d PDU E 2 O32A' O 0.4191(10) -0.3032(8) 0.5108(10) 0.168(7) Uiso 0.30 1 d PDU E 2 O33A' O 0.3074(14) -0.394(2) 0.4748(14) 0.111(13) Uiso 0.30 1 d PDU E 2 O34A' O 0.4518(19) -0.4283(14) 0.5174(19) 0.206(16) Uiso 0.30 1 d PDU E 2 Cl3B' Cl 0.2785(10) -0.3347(9) 0.5044(9) 0.060(5) Uiso 0.20 1 d PDU F 3 O31B' O 0.3149(17) -0.2744(13) 0.4772(14) 0.027(7) Uiso 0.20 1 d PDU F 3 O32B' O 0.2063(17) -0.306(2) 0.516(2) 0.079(13) Uiso 0.20 1 d PDU F 3 O33B' O 0.252(3) -0.3912(18) 0.4486(17) 0.102(17) Uiso 0.20 1 d PDU F 3 O34B' O 0.3357(16) -0.3641(15) 0.5744(11) 0.023(7) Uiso 0.20 1 d PDU F 3 Cl3C' Cl 0.4485(14) -0.3645(13) 0.5621(12) 0.108(12) Uiso 0.10 1 d PDU G 4 O31C' O 0.3839(12) -0.3716(11) 0.5940(7) 0.185(8) Uiso 0.10 1 d PDU G 4 O32C' O 0.4191(10) -0.3032(8) 0.5108(10) 0.168(7) Uiso 0.10 1 d PDU G 4 O33C' O 0.5285(17) -0.355(3) 0.618(2) 0.07(2) Uiso 0.10 1 d PDU G 4 O34C' O 0.4518(19) -0.4283(14) 0.5174(19) 0.206(16) Uiso 0.10 1 d PDU G 4 N11 N 0.4279(8) 0.5811(8) -0.1482(7) 0.100(5) Uani 1 1 d U . . C12 C 0.4752(9) 0.5926(8) -0.0882(8) 0.069(4) Uani 1 1 d U . . C13 C 0.5379(9) 0.6081(9) -0.0148(7) 0.084(5) Uani 1 1 d U . . H13A H 0.5589 0.6614 -0.0125 0.050 Uiso 1 1 calc R . . H13B H 0.5864 0.5720 -0.0034 0.050 Uiso 1 1 calc R . . H13C H 0.5114 0.6014 0.0220 0.050 Uiso 1 1 calc R . . N21 N 0.5734(12) -0.3590(12) 0.3492(9) 0.089(6) Uani 0.75 1 d PU . . C22 C 0.5536(13) -0.4188(14) 0.3249(10) 0.068(5) Uani 0.75 1 d PU . . C23 C 0.5226(13) -0.4982(11) 0.2917(12) 0.090(6) Uani 0.75 1 d PU . . H23A H 0.4607 -0.4960 0.2606 0.050 Uiso 0.75 1 calc PR . . H23B H 0.5328 -0.5358 0.3322 0.050 Uiso 0.75 1 calc PR . . H23C H 0.5544 -0.5141 0.2609 0.050 Uiso 0.75 1 calc PR . . 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 0.0345(8) 0.0325(8) 0.0341(8) -0.0075(6) 0.0169(6) 0.0016(7) Ni2 0.0388(8) 0.0259(7) 0.0257(7) 0.0039(6) 0.0155(6) 0.0086(6) N1 0.037(5) 0.043(5) 0.035(4) -0.003(3) 0.012(4) 0.008(3) C1A 0.061(7) 0.063(7) 0.047(5) 0.011(4) 0.022(5) 0.035(5) C2A 0.045(9) 0.064(13) 0.033(8) 0.003(9) 0.014(7) 0.013(10) N3A 0.045(7) 0.030(8) 0.032(5) 0.000(6) 0.016(5) 0.009(6) C3A 0.047(9) 0.031(9) 0.033(8) 0.011(8) 0.010(8) 0.001(7) C4A 0.045(5) 0.058(5) 0.021(5) 0.011(5) 0.014(4) 0.006(5) C1A' 0.061(7) 0.063(7) 0.047(5) 0.011(4) 0.022(5) 0.035(5) C2A' 0.047(11) 0.041(15) 0.041(7) 0.011(11) 0.021(9) 0.010(11) N3A' 0.044(10) 0.022(10) 0.034(7) -0.004(7) 0.016(6) 0.004(8) C3A' 0.044(8) 0.045(13) 0.021(8) -0.006(10) 0.004(9) 0.002(8) C4A' 0.045(5) 0.058(5) 0.021(5) 0.011(5) 0.014(4) 0.006(5) C5A 0.074(7) 0.021(5) 0.021(5) -0.001(4) 0.023(5) 0.004(4) C6A 0.066(7) 0.049(5) 0.032(6) 0.000(5) 0.028(6) -0.019(6) C7A 0.070(7) 0.051(5) 0.037(6) 0.014(6) 0.028(6) 0.023(5) C9A 0.057(6) 0.039(4) 0.019(5) 0.008(5) 0.004(5) -0.008(5) C8A 0.099(7) 0.030(4) 0.016(5) 0.005(4) 0.021(5) 0.009(4) C10A 0.063(10) 0.038(6) 0.017(7) -0.003(7) 0.020(7) 0.007(6) N4A 0.076(10) 0.025(6) 0.023(5) 0.000(5) 0.021(6) 0.010(7) C11A 0.135(9) 0.029(5) 0.030(5) 0.003(4) 0.036(5) 0.023(6) C8A' 0.099(7) 0.030(4) 0.016(5) 0.005(4) 0.021(5) 0.009(4) C10' 0.086(14) 0.032(7) 0.022(9) 0.001(9) 0.025(11) 0.005(9) N4A' 0.079(12) 0.025(8) 0.027(7) 0.002(6) 0.026(6) 0.013(8) C11' 0.135(9) 0.029(5) 0.030(5) 0.003(4) 0.036(5) 0.023(6) C12A 0.098(8) 0.031(6) 0.057(6) 0.003(5) 0.056(5) 0.021(6) N2 0.055(5) 0.030(4) 0.049(4) 0.011(4) 0.035(4) 0.017(4) C1B 0.051(6) 0.033(6) 0.052(6) -0.011(5) 0.027(5) 0.014(5) C2B 0.060(7) 0.033(5) 0.051(7) -0.015(5) 0.030(6) -0.001(5) N3B 0.039(4) 0.029(4) 0.035(4) -0.007(4) 0.020(4) -0.001(3) C3B 0.048(6) 0.035(6) 0.036(6) 0.001(5) 0.024(5) -0.005(4) C4B 0.039(5) 0.038(6) 0.033(5) 0.001(4) 0.023(4) -0.003(4) C5B 0.037(6) 0.055(7) 0.032(5) -0.006(5) 0.022(4) -0.013(5) C6B 0.053(7) 0.062(8) 0.025(5) -0.005(5) 0.007(5) -0.014(5) C7B 0.041(6) 0.052(7) 0.041(5) 0.000(5) 0.015(5) -0.011(5) C8B 0.033(6) 0.033(5) 0.037(5) 0.002(4) 0.016(4) -0.008(4) C9B 0.032(5) 0.040(6) 0.027(5) -0.006(4) 0.016(4) -0.009(4) C10B 0.039(6) 0.036(5) 0.043(6) 0.004(5) 0.020(5) 0.001(4) N4B 0.039(4) 0.033(4) 0.035(4) 0.010(4) 0.015(4) 0.010(3) C11B 0.042(6) 0.048(5) 0.071(8) 0.014(6) 0.030(6) 0.013(5) C12B 0.053(6) 0.043(5) 0.062(6) 0.021(5) 0.037(5) 0.026(5) C1C 0.030(6) 0.066(7) 0.035(6) -0.008(5) 0.015(5) 0.006(4) C2C 0.059(8) 0.045(6) 0.041(6) 0.001(4) 0.026(5) 0.001(5) N3C 0.037(5) 0.036(4) 0.048(5) 0.002(4) 0.020(4) 0.003(3) C3C 0.046(7) 0.033(6) 0.056(6) -0.003(5) 0.025(6) 0.000(4) C4C 0.027(6) 0.024(5) 0.043(5) 0.001(4) 0.008(5) -0.001(4) C5C 0.043(7) 0.028(6) 0.039(5) 0.010(5) 0.002(5) 0.000(5) C6C 0.053(7) 0.034(6) 0.036(5) 0.001(5) 0.008(5) -0.006(5) C7C 0.046(7) 0.032(6) 0.048(5) -0.005(5) 0.025(5) -0.012(4) C8C 0.036(5) 0.022(5) 0.042(5) -0.009(4) 0.017(4) -0.008(4) C9C 0.033(6) 0.026(5) 0.034(5) 0.009(4) 0.015(4) 0.001(4) C10C 0.053(6) 0.029(6) 0.054(6) -0.003(5) 0.026(5) -0.004(4) N4C 0.041(4) 0.035(5) 0.034(5) 0.006(4) 0.021(4) 0.009(3) C11C 0.057(7) 0.035(6) 0.047(6) 0.018(5) 0.032(5) 0.013(5) C12C 0.061(7) 0.024(5) 0.063(7) 0.017(5) 0.035(6) 0.022(5) C1 0.048(6) 0.029(5) 0.036(5) -0.003(4) 0.021(4) -0.001(4) C2 0.126(12) 0.057(8) 0.023(5) -0.009(6) 0.020(7) -0.018(8) C1' 0.048(6) 0.029(5) 0.036(5) -0.003(4) 0.021(4) -0.001(4) C2' 0.126(12) 0.057(8) 0.023(5) -0.009(6) 0.020(7) -0.018(8) Cl1 0.0500(18) 0.0531(18) 0.0364(15) 0.0022(14) 0.0211(14) -0.0001(15) O11 0.082(6) 0.068(6) 0.069(5) 0.033(4) 0.056(5) 0.034(5) O12 0.050(5) 0.072(6) 0.051(4) 0.004(4) 0.016(4) -0.017(4) O13 0.088(7) 0.143(8) 0.046(5) 0.020(5) 0.026(5) 0.066(6) O14 0.116(8) 0.076(6) 0.101(7) -0.028(5) 0.078(6) -0.041(5) Cl2 0.0476(19) 0.060(2) 0.093(3) -0.0385(19) 0.0253(18) -0.0080(17) O21 0.081(7) 0.082(5) 0.124(8) -0.001(5) 0.020(6) -0.019(5) O22 0.080(9) 0.144(15) 0.109(14) -0.015(12) 0.047(10) 0.036(11) O23 0.134(16) 0.105(13) 0.098(11) -0.029(10) 0.076(11) 0.010(14) O24 0.107(11) 0.084(11) 0.111(11) -0.044(11) -0.006(11) -0.019(10) Cl2' 0.0476(19) 0.060(2) 0.093(3) -0.0385(19) 0.0253(18) -0.0080(17) O21' 0.081(7) 0.082(5) 0.124(8) -0.001(5) 0.020(6) -0.019(5) O22' 0.13(2) 0.130(13) 0.14(2) -0.095(17) 0.046(17) 0.00(2) O23' 0.110(14) 0.094(17) 0.084(13) -0.003(11) 0.001(11) -0.032(16) O24' 0.105(15) 0.13(2) 0.18(3) 0.01(2) 0.089(15) -0.007(18) N11 0.086(10) 0.115(11) 0.072(8) 0.007(8) 0.000(7) 0.008(9) C12 0.068(10) 0.065(9) 0.064(8) 0.006(8) 0.015(6) 0.015(8) C13 0.079(10) 0.096(11) 0.066(8) -0.024(8) 0.016(6) 0.025(9) N21 0.093(13) 0.117(14) 0.040(9) -0.002(9) 0.005(9) 0.002(12) C22 0.064(13) 0.104(13) 0.032(11) 0.018(10) 0.016(10) 0.014(12) C23 0.079(15) 0.093(13) 0.097(16) 0.023(11) 0.033(13) 0.017(12) _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 O1' 1.962(15) . ? Ni1 N3A 2.030(14) . ? Ni1 O1 2.049(12) . ? Ni1 N3B 2.081(8) . ? Ni1 N1 2.085(8) . ? Ni1 N3C 2.139(8) . ? Ni1 N3A' 2.18(2) . ? Ni1 Ni2 5.6287(18) . ? Ni2 O2' 1.941(18) . ? Ni2 O2 2.010(10) . ? Ni2 N4A' 2.03(2) . ? Ni2 N2 2.084(8) . ? Ni2 N4A 2.093(16) . ? Ni2 N4B 2.102(8) . ? Ni2 N4C 2.121(8) . ? N1 C1A 1.475(13) . ? N1 C1B 1.489(12) . ? N1 C1C 1.511(13) . ? C1A C2A 1.63(3) . ? C2A N3A 1.47(3) . ? N3A C3A 1.48(2) . ? C3A C4A 1.57(2) . ? C4A C9A 1.375(15) . ? C4A C5A 1.381(14) . ? C2A' N3A' 1.50(4) . ? N3A' C3A' 1.46(3) . ? C5A C6A 1.357(14) . ? C6A C7A 1.365(15) . ? C7A C8A 1.376(16) . ? C9A C8A 1.357(15) . ? C8A C10A 1.56(2) . ? C10A N4A 1.45(2) . ? N4A C11A 1.546(19) . ? C11A C12A 1.488(16) . ? C10' N4A' 1.50(4) . ? C12A N2 1.453(12) . ? N2 C12B 1.477(14) . ? N2 C12C 1.511(13) . ? C1B C2B 1.520(14) . ? C2B N3B 1.467(12) . ? N3B C3B 1.509(11) . ? C3B C4B 1.499(14) . ? C4B C5B 1.389(13) . ? C4B C9B 1.390(13) . ? C5B C6B 1.359(15) . ? C6B C7B 1.385(15) . ? C7B C8B 1.411(14) . ? C8B C9B 1.354(13) . ? C8B C10B 1.503(13) . ? C10B N4B 1.494(12) . ? N4B C11B 1.481(12) . ? C11B C12B 1.494(14) . ? C1C C2C 1.510(14) . ? C2C N3C 1.504(12) . ? N3C C3C 1.447(13) . ? C3C C4C 1.507(14) . ? C4C C9C 1.388(13) . ? C4C C5C 1.398(13) . ? C5C C6C 1.401(14) . ? C6C C7C 1.345(14) . ? C7C C8C 1.407(14) . ? C8C C9C 1.398(13) . ? C8C C10C 1.522(14) . ? C10C N4C 1.482(13) . ? N4C C11C 1.476(12) . ? C11C C12C 1.499(13) . ? C1 O1 1.104(13) . ? C1 O2 1.301(14) . ? C1 O3 1.440(15) . ? O3 C2 1.530(15) . ? Cl1 O13 1.398(8) . ? Cl1 O14 1.410(8) . ? Cl1 O12 1.424(7) . ? Cl1 O11 1.426(7) . ? Cl2 O23 1.356(11) . ? Cl2 O22 1.401(11) . ? Cl2 O21 1.414(8) . ? Cl2 O24 1.421(11) . ? Cl3 O34 1.391(13) . ? Cl3 O33 1.412(13) . ? Cl3 O31 1.419(12) . ? Cl3 O32 1.446(12) . ? Cl3A' O34A' 1.408(13) . ? Cl3A' O33A' 1.419(14) . ? Cl3B' O33B' 1.395(14) . ? Cl3B' O32B' 1.408(14) . ? Cl3B' O31B' 1.408(14) . ? Cl3B' O34B' 1.416(14) . ? Cl3C' O33C' 1.368(15) . ? N11 C12 1.141(16) . ? C12 C13 1.429(18) . ? N21 C22 1.13(2) . ? C22 C23 1.52(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 O1' Ni1 N3A 87.6(6) . . ? O1' Ni1 O1 35.9(5) . . ? N3A Ni1 O1 123.5(5) . . ? O1' Ni1 N3B 101.4(5) . . ? N3A Ni1 N3B 114.8(5) . . ? O1 Ni1 N3B 86.3(4) . . ? O1' Ni1 N1 173.3(5) . . ? N3A Ni1 N1 87.2(5) . . ? O1 Ni1 N1 148.9(4) . . ? N3B Ni1 N1 84.6(3) . . ? O1' Ni1 N3C 92.8(5) . . ? N3A Ni1 N3C 104.9(5) . . ? O1 Ni1 N3C 82.7(4) . . ? N3B Ni1 N3C 138.1(3) . . ? N1 Ni1 N3C 84.5(3) . . ? O1' Ni1 N3A' 94.6(7) . . ? N3A Ni1 N3A' 21.2(6) . . ? O1 Ni1 N3A' 128.3(7) . . ? N3B Ni1 N3A' 93.7(7) . . ? N1 Ni1 N3A' 82.0(7) . . ? N3C Ni1 N3A' 124.4(7) . . ? O1' Ni1 Ni2 6.4(4) . . ? N3A Ni1 Ni2 93.2(4) . . ? O1 Ni1 Ni2 30.4(3) . . ? N3B Ni1 Ni2 101.9(2) . . ? N1 Ni1 Ni2 172.5(2) . . ? N3C Ni1 Ni2 88.2(2) . . ? N3A' Ni1 Ni2 100.9(6) . . ? O2' Ni2 O2 31.3(5) . . ? O2' Ni2 N4A' 116.9(9) . . ? O2 Ni2 N4A' 85.9(8) . . ? O2' Ni2 N2 152.8(6) . . ? O2 Ni2 N2 174.3(4) . . ? N4A' Ni2 N2 89.4(8) . . ? O2' Ni2 N4A 125.0(7) . . ? O2 Ni2 N4A 94.6(5) . . ? N4A' Ni2 N4A 21.3(8) . . ? N2 Ni2 N4A 82.0(5) . . ? O2' Ni2 N4B 88.3(5) . . ? O2 Ni2 N4B 100.2(4) . . ? N4A' Ni2 N4B 117.7(8) . . ? N2 Ni2 N4B 84.8(3) . . ? N4A Ni2 N4B 96.9(6) . . ? O2' Ni2 N4C 84.4(5) . . ? O2 Ni2 N4C 94.5(4) . . ? N4A' Ni2 N4C 102.0(8) . . ? N2 Ni2 N4C 83.4(3) . . ? N4A Ni2 N4C 120.6(6) . . ? N4B Ni2 N4C 138.4(3) . . ? O2' Ni2 Ni1 26.5(5) . . ? O2 Ni2 Ni1 6.5(3) . . ? N4A' Ni2 Ni1 90.5(7) . . ? N2 Ni2 Ni1 172.3(2) . . ? N4A Ni2 Ni1 100.5(5) . . ? N4B Ni2 Ni1 102.0(2) . . ? N4C Ni2 Ni1 89.0(2) . . ? C1A N1 C1B 112.7(9) . . ? C1A N1 C1C 111.5(9) . . ? C1B N1 C1C 112.1(8) . . ? C1A N1 Ni1 106.9(6) . . ? C1B N1 Ni1 105.7(6) . . ? C1C N1 Ni1 107.4(6) . . ? N1 C1A C2A 104.6(11) . . ? N3A C2A C1A 108.6(16) . . ? C2A N3A C3A 113.9(15) . . ? C2A N3A Ni1 104.3(12) . . ? C3A N3A Ni1 117.8(13) . . ? N3A C3A C4A 112.8(14) . . ? C9A C4A C5A 118.0(10) . . ? C9A C4A C3A 132.9(12) . . ? C5A C4A C3A 109.0(11) . . ? C3A' N3A' C2A' 110(2) . . ? C3A' N3A' Ni1 121.3(18) . . ? C2A' N3A' Ni1 102.3(19) . . ? C6A C5A C4A 120.3(10) . . ? C5A C6A C7A 120.8(11) . . ? C6A C7A C8A 119.8(11) . . ? C8A C9A C4A 122.0(11) . . ? C9A C8A C7A 119.0(10) . . ? C9A C8A C10A 105.4(13) . . ? C7A C8A C10A 134.5(13) . . ? N4A C10A C8A 107.7(15) . . ? C10A N4A C11A 104.7(13) . . ? C10A N4A Ni2 119.7(12) . . ? C11A N4A Ni2 100.6(9) . . ? C12A C11A N4A 101.3(11) . . ? C10' N4A' Ni2 116(2) . . ? N2 C12A C11A 110.1(9) . . ? C12A N2 C12B 111.4(9) . . ? C12A N2 C12C 111.6(9) . . ? C12B N2 C12C 111.8(8) . . ? C12A N2 Ni2 107.9(6) . . ? C12B N2 Ni2 105.2(6) . . ? C12C N2 Ni2 108.6(6) . . ? N1 C1B C2B 110.3(8) . . ? N3B C2B C1B 109.5(8) . . ? C2B N3B C3B 111.0(8) . . ? C2B N3B Ni1 108.7(6) . . ? C3B N3B Ni1 122.9(6) . . ? C4B C3B N3B 112.1(8) . . ? C5B C4B C9B 118.8(10) . . ? C5B C4B C3B 119.5(9) . . ? C9B C4B C3B 121.6(9) . . ? C6B C5B C4B 120.7(10) . . ? C5B C6B C7B 120.2(10) . . ? C6B C7B C8B 119.9(11) . . ? C9B C8B C7B 118.7(10) . . ? C9B C8B C10B 122.4(9) . . ? C7B C8B C10B 118.9(10) . . ? C8B C9B C4B 121.8(9) . . ? N4B C10B C8B 113.6(8) . . ? C11B N4B C10B 111.7(8) . . ? C11B N4B Ni2 106.6(6) . . ? C10B N4B Ni2 122.6(6) . . ? N4B C11B C12B 109.9(8) . . ? N2 C12B C11B 110.8(9) . . ? C2C C1C N1 110.4(8) . . ? N3C C2C C1C 107.5(8) . . ? C3C N3C C2C 112.7(8) . . ? C3C N3C Ni1 127.7(7) . . ? C2C N3C Ni1 101.0(6) . . ? N3C C3C C4C 112.7(9) . . ? C9C C4C C5C 119.9(9) . . ? C9C C4C C3C 120.2(9) . . ? C5C C4C C3C 119.7(9) . . ? C4C C5C C6C 118.4(10) . . ? C7C C6C C5C 121.7(10) . . ? C6C C7C C8C 121.2(10) . . ? C9C C8C C7C 117.7(9) . . ? C9C C8C C10C 120.6(9) . . ? C7C C8C C10C 121.6(9) . . ? C4C C9C C8C 121.2(9) . . ? N4C C10C C8C 112.8(8) . . ? C11C N4C C10C 112.1(8) . . ? C11C N4C Ni2 102.3(6) . . ? C10C N4C Ni2 125.1(6) . . ? N4C C11C C12C 108.9(8) . . ? C11C C12C N2 109.3(8) . . ? O1 C1 O2 134.5(13) . . ? O1 C1 O3 120.5(11) . . ? O2 C1 O3 104.6(10) . . ? C1 O1 Ni1 141.2(11) . . ? C1 O2 Ni2 121.1(8) . . ? C1 O3 C2 107.9(10) . . ? O13 Cl1 O14 111.2(6) . . ? O13 Cl1 O12 109.9(6) . . ? O14 Cl1 O12 107.4(5) . . ? O13 Cl1 O11 109.6(5) . . ? O14 Cl1 O11 108.9(5) . . ? O12 Cl1 O11 109.9(5) . . ? O23 Cl2 O22 118.9(12) . . ? O23 Cl2 O21 108.4(9) . . ? O22 Cl2 O21 105.1(9) . . ? O23 Cl2 O24 113.0(12) . . ? O22 Cl2 O24 106.1(11) . . ? O21 Cl2 O24 104.2(9) . . ? O34 Cl3 O33 114.7(16) . . ? O34 Cl3 O31 120.4(15) . . ? O33 Cl3 O31 109.2(13) . . ? O34 Cl3 O32 102.9(14) . . ? O33 Cl3 O32 103.8(13) . . ? O31 Cl3 O32 103.6(9) . . ? O34A' Cl3A' O33A' 109.9(16) . . ? O33B' Cl3B' O32B' 109.3(19) . . ? O33B' Cl3B' O31B' 106.4(17) . . ? O32B' Cl3B' O31B' 109.3(17) . . ? O33B' Cl3B' O34B' 112.8(18) . . ? O32B' Cl3B' O34B' 106.1(16) . . ? O31B' Cl3B' O34B' 113.0(16) . . ? N11 C12 C13 176.8(17) . . ? N21 C22 C23 177(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1' Ni1 Ni2 O2' -147(4) . . . . ? N3A Ni1 Ni2 O2' -177.7(12) . . . . ? O1 Ni1 Ni2 O2' -1.1(13) . . . . ? N3B Ni1 Ni2 O2' -61.5(11) . . . . ? N1 Ni1 Ni2 O2' 90(2) . . . . ? N3C Ni1 Ni2 O2' 77.5(11) . . . . ? N3A' Ni1 Ni2 O2' -157.7(13) . . . . ? O1' Ni1 Ni2 O2 -13(5) . . . . ? N3A Ni1 Ni2 O2 -43(3) . . . . ? O1 Ni1 Ni2 O2 133(3) . . . . ? N3B Ni1 Ni2 O2 73(3) . . . . ? N1 Ni1 Ni2 O2 -136(3) . . . . ? N3C Ni1 Ni2 O2 -148(3) . . . . ? N3A' Ni1 Ni2 O2 -24(3) . . . . ? O1' Ni1 Ni2 N4A' 32(4) . . . . ? N3A Ni1 Ni2 N4A' 1.1(9) . . . . ? O1 Ni1 Ni2 N4A' 177.7(10) . . . . ? N3B Ni1 Ni2 N4A' 117.2(8) . . . . ? N1 Ni1 Ni2 N4A' -91.3(19) . . . . ? N3C Ni1 Ni2 N4A' -103.8(8) . . . . ? N3A' Ni1 Ni2 N4A' 21.0(10) . . . . ? O1' Ni1 Ni2 N2 121(4) . . . . ? N3A Ni1 Ni2 N2 90.2(18) . . . . ? O1 Ni1 Ni2 N2 -93.2(19) . . . . ? N3B Ni1 Ni2 N2 -153.6(18) . . . . ? N1 Ni1 Ni2 N2 -2(2) . . . . ? N3C Ni1 Ni2 N2 -14.6(18) . . . . ? N3A' Ni1 Ni2 N2 110.2(19) . . . . ? O1' Ni1 Ni2 N4A 13(4) . . . . ? N3A Ni1 Ni2 N4A -17.9(7) . . . . ? O1 Ni1 Ni2 N4A 158.7(8) . . . . ? N3B Ni1 Ni2 N4A 98.2(6) . . . . ? N1 Ni1 Ni2 N4A -110.3(18) . . . . ? N3C Ni1 Ni2 N4A -122.7(6) . . . . ? N3A' Ni1 Ni2 N4A 2.0(9) . . . . ? O1' Ni1 Ni2 N4B -87(4) . . . . ? N3A Ni1 Ni2 N4B -117.4(5) . . . . ? O1 Ni1 Ni2 N4B 59.2(6) . . . . ? N3B Ni1 Ni2 N4B -1.2(3) . . . . ? N1 Ni1 Ni2 N4B 150.3(18) . . . . ? N3C Ni1 Ni2 N4B 137.8(3) . . . . ? N3A' Ni1 Ni2 N4B -97.4(7) . . . . ? O1' Ni1 Ni2 N4C 134(4) . . . . ? N3A Ni1 Ni2 N4C 103.1(5) . . . . ? O1 Ni1 Ni2 N4C -80.3(6) . . . . ? N3B Ni1 Ni2 N4C -140.8(3) . . . . ? N1 Ni1 Ni2 N4C 10.7(18) . . . . ? N3C Ni1 Ni2 N4C -1.8(3) . . . . ? N3A' Ni1 Ni2 N4C 123.0(7) . . . . ? O1' Ni1 N1 C1A 52(4) . . . . ? N3A Ni1 N1 C1A 12.4(8) . . . . ? O1 Ni1 N1 C1A -176.4(8) . . . . ? N3B Ni1 N1 C1A -102.8(7) . . . . ? N3C Ni1 N1 C1A 117.7(7) . . . . ? N3A' Ni1 N1 C1A -8.3(10) . . . . ? Ni2 Ni1 N1 C1A 105.2(18) . . . . ? O1' Ni1 N1 C1B 172(4) . . . . ? N3A Ni1 N1 C1B 132.8(8) . . . . ? O1 Ni1 N1 C1B -56.0(10) . . . . ? N3B Ni1 N1 C1B 17.6(6) . . . . ? N3C Ni1 N1 C1B -122.0(7) . . . . ? N3A' Ni1 N1 C1B 112.1(9) . . . . ? Ni2 Ni1 N1 C1B -134.5(16) . . . . ? O1' Ni1 N1 C1C -68(4) . . . . ? N3A Ni1 N1 C1C -107.4(7) . . . . ? O1 Ni1 N1 C1C 63.8(10) . . . . ? N3B Ni1 N1 C1C 137.4(6) . . . . ? N3C Ni1 N1 C1C -2.1(6) . . . . ? N3A' Ni1 N1 C1C -128.1(9) . . . . ? Ni2 Ni1 N1 C1C -15(2) . . . . ? C1B N1 C1A C2A -154.2(12) . . . . ? C1C N1 C1A C2A 78.7(13) . . . . ? Ni1 N1 C1A C2A -38.4(13) . . . . ? N1 C1A C2A N3A 59.3(17) . . . . ? C1A C2A N3A C3A 83(2) . . . . ? C1A C2A N3A Ni1 -47.0(16) . . . . ? O1' Ni1 N3A C2A -155.5(13) . . . . ? O1 Ni1 N3A C2A -154.3(11) . . . . ? N3B Ni1 N3A C2A 103.0(12) . . . . ? N1 Ni1 N3A C2A 20.3(12) . . . . ? N3C Ni1 N3A C2A -63.3(13) . . . . ? N3A' Ni1 N3A C2A 95(3) . . . . ? Ni2 Ni1 N3A C2A -152.3(12) . . . . ? O1' Ni1 N3A C3A 77.1(14) . . . . ? O1 Ni1 N3A C3A 78.3(15) . . . . ? N3B Ni1 N3A C3A -24.3(15) . . . . ? N1 Ni1 N3A C3A -107.1(14) . . . . ? N3C Ni1 N3A C3A 169.4(13) . . . . ? N3A' Ni1 N3A C3A -32(2) . . . . ? Ni2 Ni1 N3A C3A 80.4(14) . . . . ? C2A N3A C3A C4A 157.7(15) . . . . ? Ni1 N3A C3A C4A -79.7(18) . . . . ? N3A C3A C4A C9A -18(2) . . . . ? N3A C3A C4A C5A 159.2(13) . . . . ? O1' Ni1 N3A' C3A' -25(2) . . . . ? N3A Ni1 N3A' C3A' 47(2) . . . . ? O1 Ni1 N3A' C3A' -38(3) . . . . ? N3B Ni1 N3A' C3A' -126(2) . . . . ? N1 Ni1 N3A' C3A' 150(2) . . . . ? N3C Ni1 N3A' C3A' 72(2) . . . . ? Ni2 Ni1 N3A' C3A' -23(2) . . . . ? O1' Ni1 N3A' C2A' -147.3(17) . . . . ? N3A Ni1 N3A' C2A' -76(3) . . . . ? O1 Ni1 N3A' C2A' -160.9(14) . . . . ? N3B Ni1 N3A' C2A' 110.9(17) . . . . ? N1 Ni1 N3A' C2A' 26.9(16) . . . . ? N3C Ni1 N3A' C2A' -50.7(19) . . . . ? Ni2 Ni1 N3A' C2A' -146.1(16) . . . . ? C9A C4A C5A C6A 1.0(15) . . . . ? C3A C4A C5A C6A -176.7(11) . . . . ? C4A C5A C6A C7A -0.9(16) . . . . ? C5A C6A C7A C8A 0.0(16) . . . . ? C5A C4A C9A C8A -0.1(15) . . . . ? C3A C4A C9A C8A 176.8(13) . . . . ? C4A C9A C8A C7A -0.8(16) . . . . ? C4A C9A C8A C10A 168.8(10) . . . . ? C6A C7A C8A C9A 0.9(16) . . . . ? C6A C7A C8A C10A -165.0(14) . . . . ? C9A C8A C10A N4A 126.4(14) . . . . ? C7A C8A C10A N4A -66.4(19) . . . . ? C8A C10A N4A C11A 166.4(12) . . . . ? C8A C10A N4A Ni2 -81.9(17) . . . . ? O2' Ni2 N4A C10A 34.3(18) . . . . ? O2 Ni2 N4A C10A 26.3(15) . . . . ? N4A' Ni2 N4A C10A -40(2) . . . . ? N2 Ni2 N4A C10A -149.2(15) . . . . ? N4B Ni2 N4A C10A 127.1(14) . . . . ? N4C Ni2 N4A C10A -71.7(15) . . . . ? Ni1 Ni2 N4A C10A 23.4(15) . . . . ? O2' Ni2 N4A C11A 148.1(10) . . . . ? O2 Ni2 N4A C11A 140.1(10) . . . . ? N4A' Ni2 N4A C11A 74(3) . . . . ? N2 Ni2 N4A C11A -35.3(10) . . . . ? N4B Ni2 N4A C11A -119.0(10) . . . . ? N4C Ni2 N4A C11A 42.2(12) . . . . ? Ni1 Ni2 N4A C11A 137.3(9) . . . . ? C10A N4A C11A C12A -175.0(13) . . . . ? Ni2 N4A C11A C12A 60.2(11) . . . . ? O2' Ni2 N4A' C10' -84(2) . . . . ? O2 Ni2 N4A' C10' -80(2) . . . . ? N2 Ni2 N4A' C10' 103(2) . . . . ? N4A Ni2 N4A' C10' 34(2) . . . . ? N4B Ni2 N4A' C10' 19(2) . . . . ? N4C Ni2 N4A' C10' -174(2) . . . . ? Ni1 Ni2 N4A' C10' -85(2) . . . . ? N4A C11A C12A N2 -62.8(13) . . . . ? C11A C12A N2 C12B 146.9(9) . . . . ? C11A C12A N2 C12C -87.4(11) . . . . ? C11A C12A N2 Ni2 31.8(11) . . . . ? O2' Ni2 N2 C12A 177.5(12) . . . . ? O2 Ni2 N2 C12A -50(4) . . . . ? N4A' Ni2 N2 C12A -16.4(11) . . . . ? N4A Ni2 N2 C12A 3.7(9) . . . . ? N4B Ni2 N2 C12A 101.4(8) . . . . ? N4C Ni2 N2 C12A -118.6(8) . . . . ? Ni1 Ni2 N2 C12A -105.6(17) . . . . ? O2' Ni2 N2 C12B 58.5(14) . . . . ? O2 Ni2 N2 C12B -169(3) . . . . ? N4A' Ni2 N2 C12B -135.4(10) . . . . ? N4A Ni2 N2 C12B -115.3(8) . . . . ? N4B Ni2 N2 C12B -17.6(6) . . . . ? N4C Ni2 N2 C12B 122.4(6) . . . . ? Ni1 Ni2 N2 C12B 135.4(16) . . . . ? O2' Ni2 N2 C12C -61.4(14) . . . . ? O2 Ni2 N2 C12C 71(4) . . . . ? N4A' Ni2 N2 C12C 104.7(10) . . . . ? N4A Ni2 N2 C12C 124.8(9) . . . . ? N4B Ni2 N2 C12C -137.5(7) . . . . ? N4C Ni2 N2 C12C 2.6(7) . . . . ? Ni1 Ni2 N2 C12C 15(2) . . . . ? C1A N1 C1B C2B 75.0(11) . . . . ? C1C N1 C1B C2B -158.2(9) . . . . ? Ni1 N1 C1B C2B -41.5(9) . . . . ? N1 C1B C2B N3B 52.1(11) . . . . ? C1B C2B N3B C3B -172.4(8) . . . . ? C1B C2B N3B Ni1 -34.4(10) . . . . ? O1' Ni1 N3B C2B -167.7(7) . . . . ? N3A Ni1 N3B C2B -75.0(8) . . . . ? O1 Ni1 N3B C2B 159.7(7) . . . . ? N1 Ni1 N3B C2B 9.4(6) . . . . ? N3C Ni1 N3B C2B 84.9(8) . . . . ? N3A' Ni1 N3B C2B -72.2(9) . . . . ? Ni2 Ni1 N3B C2B -174.2(6) . . . . ? O1' Ni1 N3B C3B -35.7(8) . . . . ? N3A Ni1 N3B C3B 57.0(9) . . . . ? O1 Ni1 N3B C3B -68.4(7) . . . . ? N1 Ni1 N3B C3B 141.3(7) . . . . ? N3C Ni1 N3B C3B -143.1(7) . . . . ? N3A' Ni1 N3B C3B 59.7(9) . . . . ? Ni2 Ni1 N3B C3B -42.2(7) . . . . ? C2B N3B C3B C4B -147.4(9) . . . . ? Ni1 N3B C3B C4B 81.6(9) . . . . ? N3B C3B C4B C5B 74.2(11) . . . . ? N3B C3B C4B C9B -109.1(10) . . . . ? C9B C4B C5B C6B -0.8(15) . . . . ? C3B C4B C5B C6B 176.0(9) . . . . ? C4B C5B C6B C7B 0.9(16) . . . . ? C5B C6B C7B C8B -0.7(16) . . . . ? C6B C7B C8B C9B 0.3(15) . . . . ? C6B C7B C8B C10B -179.1(9) . . . . ? C7B C8B C9B C4B -0.1(15) . . . . ? C10B C8B C9B C4B 179.2(9) . . . . ? C5B C4B C9B C8B 0.4(14) . . . . ? C3B C4B C9B C8B -176.4(9) . . . . ? C9B C8B C10B N4B 105.8(11) . . . . ? C7B C8B C10B N4B -74.9(12) . . . . ? C8B C10B N4B C11B 150.7(9) . . . . ? C8B C10B N4B Ni2 -81.0(10) . . . . ? O2' Ni2 N4B C11B -163.3(8) . . . . ? O2 Ni2 N4B C11B 167.6(6) . . . . ? N4A' Ni2 N4B C11B 77.0(10) . . . . ? N2 Ni2 N4B C11B -9.6(6) . . . . ? N4A Ni2 N4B C11B 71.7(8) . . . . ? N4C Ni2 N4B C11B -83.7(7) . . . . ? Ni1 Ni2 N4B C11B 174.0(6) . . . . ? O2' Ni2 N4B C10B 66.3(9) . . . . ? O2 Ni2 N4B C10B 37.1(8) . . . . ? N4A' Ni2 N4B C10B -53.5(11) . . . . ? N2 Ni2 N4B C10B -140.1(7) . . . . ? N4A Ni2 N4B C10B -58.8(8) . . . . ? N4C Ni2 N4B C10B 145.9(7) . . . . ? Ni1 Ni2 N4B C10B 43.5(7) . . . . ? C10B N4B C11B C12B 171.9(9) . . . . ? Ni2 N4B C11B C12B 35.5(10) . . . . ? C12A N2 C12B C11B -73.9(11) . . . . ? C12C N2 C12B C11B 160.5(8) . . . . ? Ni2 N2 C12B C11B 42.8(9) . . . . ? N4B C11B C12B N2 -54.4(12) . . . . ? C1A N1 C1C C2C -144.7(9) . . . . ? C1B N1 C1C C2C 87.8(10) . . . . ? Ni1 N1 C1C C2C -27.9(9) . . . . ? N1 C1C C2C N3C 57.3(11) . . . . ? C1C C2C N3C C3C 85.2(10) . . . . ? C1C C2C N3C Ni1 -53.9(9) . . . . ? O1' Ni1 N3C C3C 74.0(9) . . . . ? N3A Ni1 N3C C3C -14.3(10) . . . . ? O1 Ni1 N3C C3C 108.5(9) . . . . ? N3B Ni1 N3C C3C -175.4(7) . . . . ? N1 Ni1 N3C C3C -99.9(8) . . . . ? N3A' Ni1 N3C C3C -23.5(12) . . . . ? Ni2 Ni1 N3C C3C 78.5(8) . . . . ? O1' Ni1 N3C C2C -155.7(7) . . . . ? N3A Ni1 N3C C2C 116.0(7) . . . . ? O1 Ni1 N3C C2C -121.2(7) . . . . ? N3B Ni1 N3C C2C -45.2(8) . . . . ? N1 Ni1 N3C C2C 30.4(6) . . . . ? N3A' Ni1 N3C C2C 106.8(9) . . . . ? Ni2 Ni1 N3C C2C -151.2(6) . . . . ? C2C N3C C3C C4C -178.7(8) . . . . ? Ni1 N3C C3C C4C -53.0(12) . . . . ? N3C C3C C4C C9C -69.1(12) . . . . ? N3C C3C C4C C5C 116.1(10) . . . . ? C9C C4C C5C C6C 0.6(15) . . . . ? C3C C4C C5C C6C 175.4(9) . . . . ? C4C C5C C6C C7C -0.1(16) . . . . ? C5C C6C C7C C8C 0.4(16) . . . . ? C6C C7C C8C C9C -1.1(15) . . . . ? C6C C7C C8C C10C -176.8(9) . . . . ? C5C C4C C9C C8C -1.4(14) . . . . ? C3C C4C C9C C8C -176.1(9) . . . . ? C7C C8C C9C C4C 1.6(14) . . . . ? C10C C8C C9C C4C 177.3(9) . . . . ? C9C C8C C10C N4C 61.8(12) . . . . ? C7C C8C C10C N4C -122.6(10) . . . . ? C8C C10C N4C C11C -176.2(8) . . . . ? C8C C10C N4C Ni2 59.3(11) . . . . ? O2' Ni2 N4C C11C 125.6(8) . . . . ? O2 Ni2 N4C C11C 155.3(6) . . . . ? N4A' Ni2 N4C C11C -118.0(9) . . . . ? N2 Ni2 N4C C11C -30.0(6) . . . . ? N4A Ni2 N4C C11C -106.7(8) . . . . ? N4B Ni2 N4C C11C 44.5(8) . . . . ? Ni1 Ni2 N4C C11C 151.7(6) . . . . ? O2' Ni2 N4C C10C -105.7(9) . . . . ? O2 Ni2 N4C C10C -76.1(8) . . . . ? N4A' Ni2 N4C C10C 10.6(11) . . . . ? N2 Ni2 N4C C10C 98.6(8) . . . . ? N4A Ni2 N4C C10C 22.0(10) . . . . ? N4B Ni2 N4C C10C 173.2(7) . . . . ? Ni1 Ni2 N4C C10C -79.6(7) . . . . ? C10C N4C C11C C12C -82.9(11) . . . . ? Ni2 N4C C11C C12C 53.5(9) . . . . ? N4C C11C C12C N2 -55.0(12) . . . . ? C12A N2 C12C C11C 144.8(9) . . . . ? C12B N2 C12C C11C -89.7(10) . . . . ? Ni2 N2 C12C C11C 26.0(10) . . . . ? O2 C1 O1 Ni1 -14(3) . . . . ? O3 C1 O1 Ni1 174.7(10) . . . . ? O1' Ni1 O1 C1 7.7(15) . . . . ? N3A Ni1 O1 C1 5.7(18) . . . . ? N3B Ni1 O1 C1 123.1(16) . . . . ? N1 Ni1 O1 C1 -163.8(13) . . . . ? N3C Ni1 O1 C1 -97.4(16) . . . . ? N3A' Ni1 O1 C1 31.3(19) . . . . ? Ni2 Ni1 O1 C1 1.6(12) . . . . ? O1 C1 O2 Ni2 179.0(13) . . . . ? O3 C1 O2 Ni2 -8.6(12) . . . . ? O2' Ni2 O2 C1 3.8(11) . . . . ? N4A' Ni2 O2 C1 -169.4(12) . . . . ? N2 Ni2 O2 C1 -136(3) . . . . ? N4A Ni2 O2 C1 171.1(10) . . . . ? N4B Ni2 O2 C1 73.2(9) . . . . ? N4C Ni2 O2 C1 -67.7(9) . . . . ? Ni1 Ni2 O2 C1 -34(2) . . . . ? O1 C1 O3 C2 -2.3(16) . . . . ? O2 C1 O3 C2 -176.0(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4A H4A O22 0.93 2.21 3.02(2) 146.2 2_545 N3B H3B O12 0.93 2.24 3.060(10) 146.8 3_655 N4B H4B O33# 0.93 1.96 2.83(3) 156.2 2 N4B H4B O33' 0.93 2.23 3.12(3) 161.1 2 N4B H4B O33 0.93 2.34 3.17(3) 147.5 2 N4C H4C O11 0.93 2.18 2.986(10) 144.8 . _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.964 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.109 data_Complex_5 #(corbm) _database_code_CSD 181031 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H120 Cl4 Co4 N16 O25' _chemical_formula_weight 2011.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 21.5207(11) _cell_length_b 21.7232(11) _cell_length_c 20.0882(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9391.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max .25 _exptl_crystal_size_mid .36 _exptl_crystal_size_min .64 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4208 _exptl_absorpt_coefficient_mu 0.886 _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 163(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 '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59921 _diffrn_reflns_av_R_equivalents 0.0682 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 24.00 _reflns_number_total 14563 _reflns_number_gt 11668 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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. This structure contains two independent (and different) cations, each with disorder about one amine in the saturated section of one strand. One of the water molecules is disordered over two positions and one perchlorate anion shows disorder over two positions related by rotation about one of the Cl-O bonds. All of these have been modelled with 50:50 occupancy of each site. The hydrogen atoms bonded to water were not located and have not been included in the refinement. ; _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^)+(0.1373P)^2^+7.8180P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.14(2) _refine_ls_number_reflns 14563 _refine_ls_number_parameters 1181 _refine_ls_number_restraints 228 _refine_ls_R_factor_all 0.0986 _refine_ls_R_factor_gt 0.0776 _refine_ls_wR_factor_ref 0.2220 _refine_ls_wR_factor_gt 0.2035 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.613 _refine_ls_shift/su_mean 0.015 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 Co1 Co 0.56764(5) 0.13120(5) 0.37864(6) 0.0424(3) Uani 1 1 d . . . Co2 Co 0.33235(5) 0.12840(5) 0.22417(6) 0.0412(3) Uani 1 1 d . B . N1 N 0.6520(4) 0.1324(4) 0.4398(4) 0.053(2) Uani 1 1 d . B . C1A C 0.6986(5) 0.0912(6) 0.4087(6) 0.072(3) Uani 1 1 d . . . H1A1 H 0.7220 0.1140 0.3742 0.087 Uiso 1 1 calc R B . H1A2 H 0.7285 0.0769 0.4429 0.087 Uiso 1 1 calc R . . C2A C 0.6671(5) 0.0376(5) 0.3782(6) 0.066(3) Uani 1 1 d . B . H2A1 H 0.6980 0.0113 0.3554 0.079 Uiso 1 1 calc R . . H2A2 H 0.6466 0.0128 0.4132 0.079 Uiso 1 1 calc R . . N3A N 0.6204(3) 0.0595(3) 0.3299(4) 0.0428(16) Uani 1 1 d . B . H3A H 0.6419 0.0778 0.2949 0.051 Uiso 1 1 calc R . . C3A C 0.5855(5) 0.0075(4) 0.3020(5) 0.055(2) Uani 1 1 d . . . H3A1 H 0.5543 -0.0059 0.3352 0.065 Uiso 1 1 calc R B . H3A2 H 0.6146 -0.0272 0.2949 0.065 Uiso 1 1 calc R . . C4A C 0.5531(4) 0.0207(4) 0.2381(4) 0.041(2) Uani 1 1 d . . . C5A C 0.5837(4) 0.0412(4) 0.1838(5) 0.050(2) Uani 1 1 d . . . H5A H 0.6272 0.0484 0.1855 0.059 Uiso 1 1 calc R B . C6A C 0.5512(5) 0.0517(5) 0.1257(5) 0.058(3) Uani 1 1 d . . . H6A H 0.5723 0.0672 0.0877 0.070 Uiso 1 1 calc R . . C7A C 0.4880(4) 0.0400(4) 0.1224(5) 0.049(2) Uani 1 1 d . . . H7A H 0.4666 0.0470 0.0817 0.059 Uiso 1 1 calc R B . C8A C 0.4560(4) 0.0190(4) 0.1754(4) 0.0375(18) Uani 1 1 d . . . C9A C 0.4876(4) 0.0092(3) 0.2337(4) 0.0368(18) Uani 1 1 d . . . H9A H 0.4658 -0.0053 0.2717 0.044 Uiso 1 1 calc R B . C10A C 0.3890(4) 0.0044(4) 0.1726(5) 0.047(2) Uani 1 1 d . . . H10A H 0.3752 -0.0096 0.2171 0.057 Uiso 1 1 calc R B . H10B H 0.3826 -0.0300 0.1410 0.057 Uiso 1 1 calc R . . N4A N 0.3497(3) 0.0572(3) 0.1516(3) 0.0413(16) Uani 1 1 d . B . H4A H 0.3703 0.0759 0.1163 0.050 Uiso 1 1 calc R . . C11A C 0.2897(4) 0.0366(4) 0.1259(5) 0.048(2) Uani 1 1 d . . . H11A H 0.2684 0.0109 0.1597 0.058 Uiso 1 1 calc R B . H11B H 0.2959 0.0114 0.0854 0.058 Uiso 1 1 calc R . . C12A C 0.2505(5) 0.0917(5) 0.1096(5) 0.058(3) Uani 1 1 d . . . H12A H 0.2701 0.1154 0.0732 0.069 Uiso 1 1 calc R . . H12B H 0.2089 0.0781 0.0945 0.069 Uiso 1 1 calc R . . N2 N 0.2441(3) 0.1314(3) 0.1699(4) 0.0475(18) Uani 1 1 d . . . C1B C 0.6727(5) 0.1963(5) 0.4392(5) 0.058(3) Uani 1 1 d . . . H1B1 H 0.7158 0.1985 0.4563 0.069 Uiso 1 1 calc R B . H1B2 H 0.6459 0.2208 0.4692 0.069 Uiso 1 1 calc R . . C2B C 0.6705(4) 0.2230(5) 0.3713(5) 0.060(3) Uani 1 1 d . B . H2B1 H 0.6804 0.2675 0.3733 0.072 Uiso 1 1 calc R . . H2B2 H 0.7019 0.2027 0.3427 0.072 Uiso 1 1 calc R . . N3B N 0.6080(3) 0.2142(3) 0.3428(4) 0.0433(17) Uani 1 1 d . B . H3B H 0.5837 0.2459 0.3597 0.052 Uiso 1 1 calc R . . C3B C 0.6076(4) 0.2222(4) 0.2684(5) 0.053(2) Uani 1 1 d . . . H3B1 H 0.6118 0.1814 0.2468 0.063 Uiso 1 1 calc R B . H3B2 H 0.6436 0.2477 0.2549 0.063 Uiso 1 1 calc R . . C4B C 0.5480(4) 0.2528(4) 0.2450(4) 0.043(2) Uani 1 1 d . . . C5B C 0.5348(5) 0.3117(4) 0.2635(5) 0.057(2) Uani 1 1 d . . . H5B H 0.5625 0.3329 0.2922 0.069 Uiso 1 1 calc R B . C6B C 0.4823(5) 0.3409(4) 0.2416(5) 0.057(3) Uani 1 1 d . . . H6B H 0.4743 0.3822 0.2542 0.069 Uiso 1 1 calc R . . C7B C 0.4416(4) 0.3101(4) 0.2013(5) 0.050(2) Uani 1 1 d . . . H7B H 0.4050 0.3304 0.1865 0.060 Uiso 1 1 calc R B . C8B C 0.4524(4) 0.2501(4) 0.1817(4) 0.0409(19) Uani 1 1 d . . . C9B C 0.5078(4) 0.2223(4) 0.2036(4) 0.0396(19) Uani 1 1 d . . . H9B H 0.5175 0.1817 0.1894 0.048 Uiso 1 1 calc R B . C10B C 0.4083(4) 0.2179(4) 0.1364(4) 0.044(2) Uani 1 1 d . . . H10C H 0.4247 0.1765 0.1256 0.052 Uiso 1 1 calc R B . H10D H 0.4043 0.2413 0.0944 0.052 Uiso 1 1 calc R . . N4B N 0.3456(3) 0.2116(3) 0.1683(4) 0.0410(16) Uani 1 1 d . B . H4B H 0.3427 0.2437 0.1989 0.049 Uiso 1 1 calc R . . C11B C 0.2949(4) 0.2210(5) 0.1209(5) 0.052(2) Uani 1 1 d . . . H11C H 0.3044 0.1996 0.0786 0.062 Uiso 1 1 calc R B . H11D H 0.2903 0.2655 0.1113 0.062 Uiso 1 1 calc R . . C12B C 0.2349(4) 0.1962(5) 0.1496(5) 0.055(2) Uani 1 1 d . . . H12C H 0.2224 0.2211 0.1887 0.067 Uiso 1 1 calc R . . H12D H 0.2014 0.1987 0.1159 0.067 Uiso 1 1 calc R . . C1C C 0.6343(7) 0.1114(6) 0.5062(6) 0.077(4) Uani 1 1 d . . . H1C1 H 0.6409 0.0663 0.5091 0.093 Uiso 1 1 calc R A 1 H1C2 H 0.6617 0.1312 0.5395 0.093 Uiso 1 1 calc R A 1 C2C C 0.5724(7) 0.1244(7) 0.5222(6) 0.093(5) Uani 0.50 1 d PD B 1 H2C1 H 0.5701 0.1685 0.5346 0.111 Uiso 0.50 1 calc PR B 1 H2C2 H 0.5616 0.1003 0.5624 0.111 Uiso 0.50 1 calc PR B 1 N3C N 0.5216(10) 0.1121(13) 0.4691(9) 0.069(6) Uani 0.50 1 d PD B 1 H3C H 0.5052 0.1516 0.4725 0.083 Uiso 0.50 1 calc PR B 1 C3C C 0.4734(9) 0.0873(13) 0.4911(11) 0.064(7) Uani 0.50 1 d PD B 1 H3C1 H 0.4444 0.1205 0.5044 0.076 Uiso 0.50 1 calc PR B 1 H3C2 H 0.4846 0.0644 0.5319 0.076 Uiso 0.50 1 calc PR B 1 C2C' C 0.5724(7) 0.1244(7) 0.5222(6) 0.093(5) Uani 0.50 1 d PD B 2 H2C3 H 0.5619 0.1683 0.5149 0.111 Uiso 0.50 1 calc PR B 2 H2C4 H 0.5619 0.1124 0.5684 0.111 Uiso 0.50 1 calc PR B 2 N3C' N 0.5421(8) 0.0818(9) 0.4702(9) 0.049(5) Uani 0.50 1 d PD B 2 H3C' H 0.5690 0.0483 0.4696 0.059 Uiso 0.50 1 calc PR B 2 C3C' C 0.4923(13) 0.0579(15) 0.4851(14) 0.078(9) Uani 0.50 1 d PDU B 2 H3C3 H 0.4751 0.0847 0.5204 0.094 Uiso 0.50 1 calc PR B 2 H3C4 H 0.5039 0.0190 0.5076 0.094 Uiso 0.50 1 calc PR B 2 C4C C 0.4365(6) 0.0410(7) 0.4426(6) 0.080(4) Uani 1 1 d . . . C5C C 0.4435(6) -0.0214(7) 0.4251(7) 0.089(4) Uani 1 1 d . B . H5C H 0.4788 -0.0441 0.4396 0.107 Uiso 1 1 calc R . . C6C C 0.3986(6) -0.0492(5) 0.3866(6) 0.074(3) Uani 1 1 d . . . H6C H 0.4026 -0.0912 0.3740 0.089 Uiso 1 1 calc R B . C7C C 0.3476(5) -0.0154(5) 0.3665(5) 0.066(3) Uani 1 1 d . B . H7C H 0.3164 -0.0346 0.3404 0.080 Uiso 1 1 calc R . . C8C C 0.3411(5) 0.0448(5) 0.3833(5) 0.059(3) Uani 1 1 d . . . C9C C 0.3854(6) 0.0697(5) 0.4202(5) 0.068(3) Uani 1 1 d . B . H9C H 0.3805 0.1118 0.4318 0.082 Uiso 1 1 calc R . . C10C C 0.2847(6) 0.0834(7) 0.3661(6) 0.086(4) Uani 1 1 d . B . H10E H 0.2479 0.0663 0.3891 0.104 Uiso 1 1 calc R . . H10F H 0.2912 0.1259 0.3825 0.104 Uiso 1 1 calc R . . N4C N 0.2725(4) 0.0852(4) 0.2941(5) 0.064(2) Uani 1 1 d . . . H4C H 0.2692 0.0444 0.2806 0.077 Uiso 1 1 calc R B . C11C C 0.2105(5) 0.1137(5) 0.2813(6) 0.065(3) Uani 1 1 d . B . H11E H 0.1787 0.0935 0.3095 0.079 Uiso 1 1 calc R . . H11F H 0.2117 0.1579 0.2931 0.079 Uiso 1 1 calc R . . C12C C 0.1938(5) 0.1070(5) 0.2120(6) 0.062(3) Uani 1 1 d . B . H12E H 0.1548 0.1296 0.2029 0.075 Uiso 1 1 calc R . . H12F H 0.1869 0.0630 0.2016 0.075 Uiso 1 1 calc R . . C20 C 0.4452(4) 0.1462(3) 0.3092(4) 0.0336(18) Uani 1 1 d . . . O21 O 0.4984(3) 0.1236(2) 0.3201(3) 0.0416(13) Uani 1 1 d U B . O22 O 0.4132(3) 0.1215(2) 0.2639(3) 0.0417(13) Uani 1 1 d U B . O23 O 0.4245(3) 0.1904(3) 0.3431(3) 0.0457(14) Uani 1 1 d U B . Co3 Co 1.00194(6) 0.09195(5) -0.07582(7) 0.0471(3) Uani 1 1 d . . . Co4 Co 1.17716(5) 0.15356(5) -0.23556(6) 0.0417(3) Uani 1 1 d . D . N5 N 0.9077(3) 0.1070(4) -0.0264(4) 0.0508(19) Uani 1 1 d . D . C1D C 0.8680(4) 0.0554(5) -0.0450(5) 0.060(3) Uani 1 1 d . . . H1D1 H 0.8240 0.0689 -0.0456 0.072 Uiso 1 1 calc R D . H1D2 H 0.8721 0.0222 -0.0116 0.072 Uiso 1 1 calc R . . C2D C 0.8854(4) 0.0314(5) -0.1117(5) 0.056(2) Uani 1 1 d . D . H2D1 H 0.8603 -0.0054 -0.1225 0.067 Uiso 1 1 calc R . . H2D2 H 0.8775 0.0631 -0.1461 0.067 Uiso 1 1 calc R . . N3D N 0.9517(4) 0.0154(3) -0.1102(4) 0.055(2) Uani 1 1 d . D . H3D H 0.9543 -0.0121 -0.0749 0.066 Uiso 1 1 calc R . . C3D C 0.9749(5) -0.0209(4) -0.1673(5) 0.061(3) Uani 1 1 d . . . H3D1 H 0.9460 -0.0558 -0.1747 0.073 Uiso 1 1 calc R D . H3D2 H 1.0158 -0.0385 -0.1551 0.073 Uiso 1 1 calc R . . C4D C 0.9818(4) 0.0132(4) -0.2308(5) 0.048(2) Uani 1 1 d . D . C5D C 0.9316(5) 0.0325(5) -0.2686(6) 0.065(3) Uani 1 1 d . . . H5D H 0.8910 0.0244 -0.2523 0.078 Uiso 1 1 calc R D . C6D C 0.9372(5) 0.0615(6) -0.3260(7) 0.076(4) Uani 1 1 d . D . H6D H 0.9011 0.0733 -0.3500 0.091 Uiso 1 1 calc R . . C7D C 0.9979(5) 0.0753(5) -0.3525(6) 0.063(3) Uani 1 1 d . . . H7D H 1.0029 0.0975 -0.3929 0.076 Uiso 1 1 calc R D . C8D C 1.0490(4) 0.0545(4) -0.3161(5) 0.048(2) Uani 1 1 d . D . C9D C 1.0396(4) 0.0251(4) -0.2566(5) 0.052(2) Uani 1 1 d . . . H9D H 1.0750 0.0122 -0.2319 0.062 Uiso 1 1 calc R D . C10D C 1.1113(5) 0.0626(6) -0.3472(5) 0.068(3) Uani 1 1 d . . . H10G H 1.1205 0.0252 -0.3736 0.082 Uiso 1 1 calc R D . H10H H 1.1086 0.0974 -0.3789 0.082 Uiso 1 1 calc R . . N4D N 1.1636(3) 0.0738(4) -0.3038(4) 0.0480(18) Uani 1 1 d . D . H4D H 1.1625 0.0403 -0.2749 0.058 Uiso 1 1 calc R . . C11D C 1.2221(5) 0.0632(5) -0.3426(6) 0.064(3) Uani 1 1 d . . . H11G H 1.2228 0.0894 -0.3830 0.076 Uiso 1 1 calc R D . H11H H 1.2253 0.0196 -0.3565 0.076 Uiso 1 1 calc R . . C12D C 1.2758(5) 0.0801(5) -0.2962(5) 0.060(3) Uani 1 1 d . D . H12G H 1.2758 0.0523 -0.2572 0.071 Uiso 1 1 calc R . . H12H H 1.3158 0.0750 -0.3199 0.071 Uiso 1 1 calc R . . N6 N 1.2695(3) 0.1443(3) -0.2735(4) 0.0517(19) Uani 1 1 d . . . C1E C 0.8851(5) 0.1659(4) -0.0520(5) 0.056(2) Uani 1 1 d . . . H1E1 H 0.8564 0.1842 -0.0190 0.068 Uiso 1 1 calc R D . H1E2 H 0.8614 0.1585 -0.0934 0.068 Uiso 1 1 calc R . . C2E C 0.9356(5) 0.2103(4) -0.0660(5) 0.058(3) Uani 1 1 d . D . H2E1 H 0.9185 0.2477 -0.0873 0.069 Uiso 1 1 calc R . . H2E2 H 0.9565 0.2224 -0.0241 0.069 Uiso 1 1 calc R . . N3E N 0.9803(3) 0.1798(3) -0.1112(4) 0.0469(18) Uani 1 1 d . D . H3E H 1.0168 0.2025 -0.1085 0.056 Uiso 1 1 calc R . . C3E C 0.9602(4) 0.1823(4) -0.1836(5) 0.044(2) Uani 1 1 d . . . H3E1 H 0.9721 0.1436 -0.2064 0.053 Uiso 1 1 calc R D . H3E2 H 0.9144 0.1864 -0.1862 0.053 Uiso 1 1 calc R . . C4E C 0.9908(4) 0.2366(4) -0.2179(5) 0.053(3) Uani 1 1 d . D . C5E C 0.9794(5) 0.2964(4) -0.1994(6) 0.064(3) Uani 1 1 d . . . H5E H 0.9496 0.3054 -0.1660 0.077 Uiso 1 1 calc R D . C6E C 1.0130(5) 0.3445(5) -0.2310(8) 0.078(4) Uani 1 1 d . D . H6E H 1.0036 0.3862 -0.2206 0.093 Uiso 1 1 calc R . . C7E C 1.0570(4) 0.3320(5) -0.2744(7) 0.065(3) Uani 1 1 d . . . H7E H 1.0806 0.3649 -0.2928 0.079 Uiso 1 1 calc R D . C8E C 1.0696(4) 0.2725(4) -0.2940(5) 0.049(2) Uani 1 1 d . D . C9E C 1.0357(4) 0.2247(4) -0.2657(5) 0.046(2) Uani 1 1 d . . . H9E H 1.0434 0.1835 -0.2792 0.056 Uiso 1 1 calc R D . C10E C 1.1215(4) 0.2538(4) -0.3417(5) 0.054(2) Uani 1 1 d . . . H10I H 1.1057 0.2217 -0.3723 0.065 Uiso 1 1 calc R D . H10J H 1.1334 0.2899 -0.3689 0.065 Uiso 1 1 calc R . . N4E N 1.1761(3) 0.2306(4) -0.3076(4) 0.0487(18) Uani 1 1 d . D . H4E H 1.1928 0.2641 -0.2850 0.058 Uiso 1 1 calc R . . C11E C 1.2214(5) 0.2143(5) -0.3574(5) 0.062(3) Uani 1 1 d . . . H11I H 1.2316 0.2511 -0.3844 0.074 Uiso 1 1 calc R D . H11J H 1.2036 0.1828 -0.3875 0.074 Uiso 1 1 calc R . . C12E C 1.2807(4) 0.1891(5) -0.3259(7) 0.068(3) Uani 1 1 d . D . H12I H 1.3063 0.1697 -0.3611 0.082 Uiso 1 1 calc R . . H12J H 1.3048 0.2239 -0.3072 0.082 Uiso 1 1 calc R . . C1F C 0.9184(6) 0.1110(5) 0.0446(6) 0.073(3) Uani 1 1 d . . . H1F1 H 0.8803 0.0988 0.0688 0.088 Uiso 1 1 calc R D . H1F2 H 0.9283 0.1541 0.0568 0.088 Uiso 1 1 calc R . . C2F C 0.9717(5) 0.0694(5) 0.0649(5) 0.066(3) Uani 1 1 d . D . H2F1 H 0.9800 0.0742 0.1131 0.079 Uiso 1 1 calc R C 1 H2F2 H 0.9604 0.0259 0.0565 0.079 Uiso 1 1 calc R C 1 N3F N 1.0281(5) 0.0853(5) 0.0266(5) 0.077(3) Uani 0.60 1 d P D 1 H3F H 1.0561 0.0529 0.0308 0.092 Uiso 0.60 1 calc PR D 1 C3F C 1.0582(11) 0.1455(9) 0.0639(11) 0.058(6) Uani 0.60 1 d P D 1 H3F1 H 1.0244 0.1693 0.0852 0.070 Uiso 0.60 1 calc PR D 1 H3F2 H 1.0865 0.1312 0.0996 0.070 Uiso 0.60 1 calc PR D 1 N3F' N 1.0281(5) 0.0853(5) 0.0266(5) 0.077(3) Uani 0.40 1 d P D 2 H3F' H 1.0424 0.0450 0.0235 0.092 Uiso 0.40 1 calc PR D 2 C3F' C 1.0808(19) 0.107(3) 0.055(2) 0.11(2) Uani 0.40 1 d P D 2 H3F3 H 1.1168 0.0814 0.0427 0.136 Uiso 0.40 1 calc PR D 2 H3F4 H 1.0769 0.1083 0.1038 0.136 Uiso 0.40 1 calc PR D 2 C4F C 1.0902(6) 0.1833(8) 0.0226(6) 0.096(5) Uani 1 1 d . . . C5F C 1.0698(6) 0.2533(7) 0.0196(7) 0.089(4) Uani 1 1 d . D . H5F H 1.0373 0.2690 0.0467 0.107 Uiso 1 1 calc R . . C6F C 1.1000(9) 0.2882(7) -0.0224(7) 0.095(4) Uani 1 1 d . . . H6F H 1.0858 0.3294 -0.0265 0.115 Uiso 1 1 calc R D . C7F C 1.1459(11) 0.2734(9) -0.0580(8) 0.118(6) Uani 1 1 d . D . H7F H 1.1659 0.3030 -0.0854 0.142 Uiso 1 1 calc R . . C8F C 1.1644(6) 0.2193(6) -0.0563(5) 0.069(3) Uani 1 1 d . . . C9F C 1.1389(4) 0.1745(4) -0.0219(5) 0.053(2) Uani 1 1 d . D . H9F H 1.1546 0.1340 -0.0278 0.063 Uiso 1 1 calc R . . C10F C 1.2291(6) 0.1968(9) -0.0929(7) 0.100(5) Uani 1 1 d . D . H10K H 1.2649 0.2178 -0.0718 0.120 Uiso 1 1 calc R . . H10L H 1.2344 0.1520 -0.0863 0.120 Uiso 1 1 calc R . . N4F N 1.2292(5) 0.2094(5) -0.1599(5) 0.082(3) Uani 1 1 d . . . H4F H 1.2136 0.2492 -0.1637 0.098 Uiso 1 1 calc R D . C11F C 1.2930(5) 0.2130(5) -0.1823(7) 0.075(3) Uani 1 1 d . D . H11K H 1.3206 0.2194 -0.1435 0.090 Uiso 1 1 calc R . . H11L H 1.2979 0.2487 -0.2125 0.090 Uiso 1 1 calc R . . C12F C 1.3120(4) 0.1547(5) -0.2184(6) 0.062(3) Uani 1 1 d . D . H12K H 1.3550 0.1588 -0.2353 0.074 Uiso 1 1 calc R . . H12L H 1.3106 0.1193 -0.1874 0.074 Uiso 1 1 calc R . . C30 C 1.1185(4) 0.0962(4) -0.1497(4) 0.047(2) Uani 1 1 d . . . O31 O 1.0840(3) 0.0682(3) -0.1080(3) 0.0503(15) Uani 1 1 d U D . O32 O 1.1732(3) 0.0775(3) -0.1628(3) 0.0528(16) Uani 1 1 d U D . O33 O 1.0989(3) 0.1446(3) -0.1806(3) 0.0466(15) Uani 1 1 d U D . Cl5 Cl 0.27955(14) 0.38991(13) 0.2214(2) 0.0812(9) Uani 1 1 d . . . O51 O 0.2866(7) 0.3361(7) 0.2484(11) 0.214(10) Uani 1 1 d U . . O52 O 0.2309(5) 0.4278(6) 0.2367(7) 0.136(5) Uani 1 1 d U . . O53 O 0.3319(6) 0.4287(7) 0.2285(14) 0.224(11) Uani 1 1 d U . . O54 O 0.2961(9) 0.3855(8) 0.1544(9) 0.178(7) Uani 1 1 d U . . Cl6 Cl 0.39426(17) 0.11762(15) -0.03182(13) 0.0784(9) Uani 1 1 d . . . O61 O 0.4580(7) 0.1383(6) -0.0074(8) 0.162(7) Uani 1 1 d U . . O62 O 0.4017(5) 0.1110(4) -0.0986(4) 0.085(3) Uani 1 1 d U . . O63 O 0.3815(5) 0.0614(6) -0.0007(5) 0.122(4) Uani 1 1 d U . . O64 O 0.3642(7) 0.1670(7) -0.0104(7) 0.160(6) Uani 1 1 d U . . Cl7 Cl 0.76409(13) 0.11921(12) -0.2517(2) 0.0814(10) Uani 1 1 d . . . O71 O 0.8145(5) 0.1507(5) -0.2640(9) 0.154(7) Uani 1 1 d U . . O72 O 0.7705(3) 0.0554(3) -0.2464(5) 0.080(2) Uani 1 1 d U . . O73 O 0.7162(6) 0.1466(5) -0.2214(10) 0.161(7) Uani 1 1 d U . . O74 O 0.7289(10) 0.1230(8) -0.3092(13) 0.206(8) Uani 1 1 d U . . Cl8 Cl 0.8971(2) -0.13390(14) -0.02459(14) 0.0833(10) Uani 0.50 1 d PD E 1 O81 O 0.9009(7) -0.1456(5) -0.0927(5) 0.119(4) Uani 0.50 1 d PDU E 1 O82 O 0.9447(15) -0.0930(17) -0.0073(16) 0.20(2) Uani 0.50 1 d PDU E 1 O83 O 0.9043(17) -0.1846(11) 0.0146(13) 0.134(17) Uani 0.50 1 d PDU E 1 O84 O 0.8389(10) -0.1088(19) -0.0094(11) 0.184(19) Uani 0.50 1 d PDU E 1 Cl8' Cl 0.8971(2) -0.13390(14) -0.02459(14) 0.0833(10) Uani 0.50 1 d PD F 2 O81' O 0.9009(7) -0.1456(5) -0.0927(5) 0.119(4) Uani 0.50 1 d PDU F 2 O82' O 0.9332(10) -0.0825(6) -0.0079(9) 0.065(6) Uani 0.50 1 d PDU F 2 O83' O 0.9255(18) -0.1802(9) 0.0122(11) 0.132(16) Uani 0.50 1 d PDU F 2 O84' O 0.8365(8) -0.131(2) 0.000(2) 0.31(4) Uani 0.50 1 d PDU F 2 O1W O 0.4996(19) 0.2386(16) 0.4369(19) 0.143(16) Uani 0.50 1 d PU B 1 O1W' O 0.5075(11) 0.2110(9) 0.4300(10) 0.064(5) Uani 0.50 1 d PU B 2 O2W O 0.3138(4) 0.2194(5) 0.3062(5) 0.092(3) Uani 1 1 d U . . O3W O 1.2237(7) 0.0350(8) -0.0451(7) 0.078(5) Uani 0.50 1 d PU . . O4W O 1.1324(8) 0.0027(8) 0.0286(11) 0.096(5) Uani 0.50 1 d PU . . 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 Co1 0.0433(6) 0.0363(6) 0.0477(7) 0.0052(5) -0.0048(5) 0.0006(5) Co2 0.0381(6) 0.0399(6) 0.0455(6) 0.0056(5) -0.0001(5) -0.0059(5) N1 0.054(5) 0.048(5) 0.058(5) -0.006(4) -0.012(4) 0.003(4) C1A 0.058(6) 0.074(7) 0.085(8) -0.016(6) -0.021(6) 0.020(6) C2A 0.059(6) 0.058(6) 0.081(7) -0.029(6) -0.018(6) 0.024(5) N3A 0.045(4) 0.031(4) 0.052(4) -0.002(3) -0.010(3) 0.002(3) C3A 0.060(6) 0.040(5) 0.064(6) 0.003(4) -0.013(5) 0.011(4) C4A 0.054(5) 0.036(5) 0.033(4) 0.000(3) 0.008(4) 0.013(4) C5A 0.050(5) 0.052(6) 0.047(5) -0.009(4) 0.003(4) 0.014(4) C6A 0.073(7) 0.063(6) 0.040(5) 0.005(4) 0.007(5) 0.007(5) C7A 0.050(5) 0.054(6) 0.044(5) -0.002(4) -0.006(4) 0.013(4) C8A 0.041(4) 0.029(4) 0.043(5) -0.010(4) -0.005(4) 0.008(3) C9A 0.044(4) 0.028(4) 0.038(4) 0.001(3) 0.000(4) 0.002(3) C10A 0.058(5) 0.027(4) 0.057(5) 0.003(4) -0.004(5) 0.000(4) N4A 0.047(4) 0.030(4) 0.047(4) 0.002(3) -0.005(3) 0.006(3) C11A 0.040(5) 0.045(5) 0.060(6) -0.013(4) -0.001(4) -0.003(4) C12A 0.051(6) 0.059(6) 0.065(6) -0.018(5) -0.020(5) 0.009(5) N2 0.043(4) 0.034(4) 0.066(5) -0.006(3) 0.003(4) -0.004(3) C1B 0.057(6) 0.066(7) 0.050(6) -0.009(5) -0.024(4) 0.001(5) C2B 0.055(6) 0.058(6) 0.067(7) 0.006(5) -0.006(5) -0.014(5) N3B 0.038(4) 0.035(4) 0.057(5) 0.007(3) -0.005(3) -0.003(3) C3B 0.044(5) 0.050(5) 0.065(6) 0.005(5) 0.002(5) -0.003(4) C4B 0.059(5) 0.034(5) 0.038(5) 0.003(3) 0.006(4) -0.002(4) C5B 0.072(6) 0.046(6) 0.054(6) 0.004(5) -0.016(5) -0.014(5) C6B 0.085(7) 0.026(5) 0.061(6) 0.000(4) -0.013(5) 0.004(5) C7B 0.052(5) 0.037(5) 0.060(6) 0.002(4) -0.002(4) 0.005(4) C8B 0.050(5) 0.025(4) 0.048(5) 0.003(4) 0.013(4) -0.004(4) C9B 0.055(5) 0.028(4) 0.037(4) 0.007(3) 0.007(4) -0.007(4) C10B 0.048(5) 0.039(5) 0.044(5) 0.000(4) 0.011(4) -0.014(4) N4B 0.050(4) 0.021(3) 0.052(4) -0.002(3) 0.003(3) -0.004(3) C11B 0.050(5) 0.055(6) 0.051(5) 0.003(4) -0.004(4) 0.010(4) C12B 0.047(5) 0.053(6) 0.066(6) 0.005(5) -0.009(5) 0.015(4) C1C 0.116(11) 0.064(7) 0.053(7) 0.003(5) -0.033(7) 0.006(7) C2C 0.111(11) 0.130(13) 0.037(6) -0.007(6) -0.005(6) -0.044(9) N3C 0.059(13) 0.11(2) 0.036(10) 0.015(12) -0.003(9) -0.001(13) C3C 0.060(14) 0.082(17) 0.049(12) 0.014(12) 0.024(11) 0.016(13) C2C' 0.111(11) 0.130(13) 0.037(6) -0.007(6) -0.005(6) -0.044(9) N3C' 0.035(10) 0.062(12) 0.052(10) 0.003(9) -0.016(8) 0.002(8) C3C' 0.087(12) 0.081(12) 0.068(11) 0.017(9) 0.002(9) -0.003(9) C4C 0.074(8) 0.097(10) 0.068(8) 0.045(7) -0.011(6) -0.028(7) C5C 0.072(8) 0.108(11) 0.087(9) 0.066(9) 0.005(7) -0.002(7) C6C 0.091(8) 0.052(7) 0.078(8) 0.018(6) 0.000(7) -0.014(6) C7C 0.070(7) 0.068(8) 0.061(7) 0.026(6) -0.009(5) -0.018(6) C8C 0.082(7) 0.056(7) 0.040(5) 0.020(5) -0.002(5) -0.013(5) C9C 0.105(9) 0.053(6) 0.047(6) 0.019(5) 0.007(6) -0.013(6) C10C 0.082(8) 0.107(11) 0.070(8) 0.005(7) 0.006(7) 0.013(7) N4C 0.059(5) 0.054(5) 0.078(6) 0.020(4) 0.018(4) 0.013(4) C11C 0.051(6) 0.060(6) 0.086(8) 0.026(6) 0.019(5) 0.008(5) C12C 0.047(5) 0.055(6) 0.084(8) -0.014(6) 0.008(5) 0.002(5) C20 0.037(4) 0.022(4) 0.042(5) 0.010(4) 0.002(4) -0.001(3) O21 0.044(3) 0.032(3) 0.049(3) -0.001(3) -0.009(3) 0.007(2) O22 0.040(3) 0.040(3) 0.045(3) 0.003(3) -0.006(3) 0.005(2) O23 0.053(3) 0.038(3) 0.046(3) 0.003(3) 0.006(3) 0.006(3) Co3 0.0492(6) 0.0401(6) 0.0519(7) 0.0044(6) 0.0045(5) 0.0023(5) Co4 0.0418(6) 0.0368(6) 0.0465(6) 0.0038(5) -0.0035(5) -0.0012(5) N5 0.049(4) 0.045(4) 0.059(5) -0.009(4) 0.010(4) 0.003(3) C1D 0.048(5) 0.056(6) 0.077(7) -0.003(5) 0.018(5) 0.003(5) C2D 0.050(5) 0.046(5) 0.073(6) -0.018(5) 0.013(5) -0.012(4) N3D 0.066(5) 0.031(4) 0.069(5) -0.003(4) 0.014(4) -0.007(3) C3D 0.072(6) 0.035(5) 0.076(7) -0.022(5) 0.027(5) -0.007(5) C4D 0.043(5) 0.026(4) 0.074(6) -0.012(4) 0.005(5) -0.008(3) C5D 0.052(6) 0.075(7) 0.067(7) -0.022(6) 0.002(5) -0.015(5) C6D 0.063(7) 0.081(8) 0.083(9) -0.035(7) -0.016(6) 0.019(6) C7D 0.081(8) 0.051(6) 0.057(6) -0.009(5) -0.005(5) 0.005(5) C8D 0.046(5) 0.047(5) 0.052(5) -0.014(4) 0.002(4) -0.012(4) C9D 0.043(5) 0.046(5) 0.067(7) -0.005(4) -0.001(4) -0.001(4) C10D 0.075(7) 0.080(8) 0.051(6) -0.013(5) -0.002(5) -0.029(6) N4D 0.046(4) 0.044(4) 0.054(5) -0.009(3) 0.005(3) -0.006(3) C11D 0.061(6) 0.057(6) 0.073(7) -0.011(5) 0.004(5) 0.001(5) C12D 0.048(5) 0.062(7) 0.069(7) -0.009(5) 0.005(5) -0.006(5) N6 0.042(4) 0.045(4) 0.069(5) -0.001(4) 0.003(4) 0.000(3) C1E 0.059(6) 0.048(6) 0.062(6) -0.010(5) 0.012(5) 0.012(5) C2E 0.074(6) 0.037(5) 0.062(6) -0.009(4) -0.017(5) 0.011(4) N3E 0.046(4) 0.030(4) 0.065(5) 0.006(3) -0.010(4) -0.014(3) C3E 0.040(5) 0.030(4) 0.062(6) -0.001(4) -0.009(4) -0.001(4) C4E 0.045(5) 0.035(5) 0.078(7) 0.012(4) -0.025(5) -0.001(4) C5E 0.056(6) 0.034(5) 0.101(8) -0.003(5) -0.008(6) -0.003(4) C6E 0.066(7) 0.026(5) 0.141(12) -0.014(6) -0.011(8) 0.009(5) C7E 0.043(5) 0.051(7) 0.103(8) 0.027(6) -0.021(6) -0.007(4) C8E 0.051(5) 0.041(5) 0.054(6) 0.020(4) -0.017(4) -0.009(4) C9E 0.048(5) 0.046(5) 0.046(5) -0.006(4) -0.013(4) 0.004(4) C10E 0.058(6) 0.044(5) 0.060(6) 0.012(4) -0.019(5) 0.003(4) N4E 0.052(4) 0.040(4) 0.054(5) 0.007(3) -0.011(4) -0.005(3) C11E 0.064(6) 0.061(6) 0.060(6) 0.023(5) 0.002(5) -0.003(5) C12E 0.042(5) 0.069(7) 0.095(8) 0.022(6) 0.002(5) -0.008(5) C1F 0.072(7) 0.061(7) 0.086(8) -0.020(6) 0.017(6) 0.013(6) C2F 0.085(7) 0.061(7) 0.052(6) 0.005(5) 0.010(6) -0.014(6) N3F 0.067(6) 0.101(8) 0.063(6) 0.023(5) 0.004(5) 0.007(6) C3F 0.075(14) 0.042(10) 0.058(11) -0.002(9) -0.025(10) 0.003(9) N3F' 0.067(6) 0.101(8) 0.063(6) 0.023(5) 0.004(5) 0.007(6) C3F' 0.09(3) 0.17(5) 0.08(3) 0.10(3) -0.04(2) -0.09(3) C4F 0.067(8) 0.159(15) 0.063(8) 0.008(9) -0.022(6) -0.047(9) C5F 0.087(9) 0.096(10) 0.085(9) -0.001(8) 0.018(7) 0.041(8) C6F 0.146(14) 0.080(9) 0.060(8) -0.006(7) 0.012(9) -0.024(9) C7F 0.185(19) 0.097(14) 0.073(10) -0.011(9) -0.007(11) -0.049(13) C8F 0.093(8) 0.057(7) 0.056(7) -0.014(5) -0.022(6) -0.027(6) C9F 0.052(5) 0.033(5) 0.073(6) -0.004(4) -0.008(5) -0.001(4) C10F 0.072(8) 0.137(13) 0.090(10) 0.010(9) -0.022(7) -0.023(8) N4F 0.080(7) 0.089(7) 0.076(7) -0.050(6) -0.041(5) 0.024(5) C11F 0.060(7) 0.060(7) 0.105(9) -0.019(6) -0.024(6) -0.004(5) C12F 0.044(5) 0.060(6) 0.081(8) 0.002(5) -0.011(5) -0.007(5) C30 0.050(6) 0.050(6) 0.041(5) 0.002(4) -0.013(4) -0.002(4) O31 0.049(3) 0.054(4) 0.048(4) 0.012(3) 0.007(3) 0.000(3) O32 0.045(4) 0.055(4) 0.058(4) 0.009(3) 0.004(3) 0.005(3) O33 0.037(3) 0.050(4) 0.053(4) 0.014(3) 0.000(3) 0.003(3) Cl5 0.0740(18) 0.0499(15) 0.120(3) 0.0125(17) 0.0337(18) 0.0167(13) O51 0.149(11) 0.150(12) 0.34(2) 0.141(15) 0.129(14) 0.072(9) O52 0.097(7) 0.147(10) 0.164(11) 0.051(9) 0.050(7) 0.052(7) O53 0.113(10) 0.121(11) 0.44(3) -0.032(17) -0.077(15) 0.002(8) O54 0.196(16) 0.157(13) 0.181(15) 0.024(11) 0.084(13) 0.053(11) Cl6 0.120(2) 0.0738(19) 0.0418(14) 0.0097(13) 0.0089(15) 0.0318(18) O61 0.209(14) 0.092(8) 0.186(14) 0.018(8) -0.124(12) -0.033(9) O62 0.140(8) 0.067(5) 0.049(4) 0.007(4) 0.010(5) -0.013(5) O63 0.138(9) 0.153(10) 0.075(6) 0.053(6) -0.037(6) -0.077(8) O64 0.196(13) 0.146(12) 0.138(11) -0.060(9) 0.075(11) -0.038(10) Cl7 0.0541(15) 0.0486(16) 0.141(3) -0.0021(17) 0.0074(17) 0.0046(12) O71 0.093(7) 0.073(6) 0.30(2) -0.043(9) 0.055(10) -0.018(5) O72 0.070(4) 0.046(4) 0.124(7) -0.005(4) 0.002(5) 0.001(3) O73 0.131(10) 0.068(7) 0.28(2) 0.005(9) 0.082(12) 0.013(6) O74 0.216(19) 0.137(13) 0.27(2) 0.018(14) -0.073(19) 0.007(12) Cl8 0.138(3) 0.0661(19) 0.0456(15) -0.0021(13) 0.0001(18) -0.0162(19) O81 0.184(11) 0.104(8) 0.069(6) -0.003(5) -0.009(7) -0.030(7) O82 0.19(3) 0.31(6) 0.09(2) -0.02(3) -0.03(2) -0.13(3) O83 0.22(3) 0.10(2) 0.08(2) 0.047(16) -0.028(18) -0.09(2) O84 0.12(3) 0.39(5) 0.048(12) -0.03(2) 0.012(13) -0.03(3) Cl8' 0.138(3) 0.0661(19) 0.0456(15) -0.0021(13) 0.0001(18) -0.0162(19) O81' 0.184(11) 0.104(8) 0.069(6) -0.003(5) -0.009(7) -0.030(7) O82' 0.120(13) 0.018(6) 0.056(11) 0.013(6) 0.008(9) -0.012(7) O83' 0.23(4) 0.065(17) 0.10(2) -0.025(15) -0.09(2) 0.05(2) O84' 0.08(3) 0.50(8) 0.34(7) 0.09(6) -0.06(3) 0.04(3) O1W 0.14(2) 0.15(3) 0.13(2) -0.10(2) 0.015(17) -0.07(2) O1W' 0.074(10) 0.072(13) 0.046(9) -0.043(10) 0.021(7) -0.039(10) O2W 0.059(5) 0.133(8) 0.084(6) 0.008(5) 0.005(4) 0.004(5) O3W 0.082(10) 0.101(12) 0.049(8) 0.004(8) -0.002(7) 0.059(9) O4W 0.081(11) 0.081(12) 0.125(15) 0.007(11) -0.007(11) 0.015(9) _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 Co1 O21 1.904(6) . ? Co1 N3C 2.11(2) . ? Co1 N3B 2.127(7) . ? Co1 N3A 2.161(7) . ? Co1 N1 2.193(8) . ? Co1 N3C' 2.20(2) . ? Co1 O1W' 2.40(2) . ? Co1 O1W 2.99(3) . ? Co1 Co2 5.9389(16) . ? Co2 O22 1.920(6) . ? Co2 N4C 2.123(8) . ? Co2 N4B 2.148(7) . ? Co2 N4A 2.158(7) . ? Co2 N2 2.191(8) . ? Co2 O2W 2.604(11) . ? N1 C1B 1.457(13) . ? N1 C1C 1.460(15) . ? N1 C1A 1.483(14) . ? C1A C2A 1.480(15) . ? C2A N3A 1.477(12) . ? N3A C3A 1.467(12) . ? C3A C4A 1.489(13) . ? C4A C5A 1.350(13) . ? C4A C9A 1.435(12) . ? C5A C6A 1.378(14) . ? C6A C7A 1.385(14) . ? C7A C8A 1.348(13) . ? C8A C9A 1.370(12) . ? C8A C10A 1.478(12) . ? C10A N4A 1.485(11) . ? N4A C11A 1.462(11) . ? C11A C12A 1.500(13) . ? C12A N2 1.492(12) . ? N2 C12C 1.472(13) . ? N2 C12B 1.479(12) . ? C1B C2B 1.484(15) . ? C2B N3B 1.474(12) . ? N3B C3B 1.504(13) . ? C3B C4B 1.520(13) . ? C4B C5B 1.361(13) . ? C4B C9B 1.371(12) . ? C5B C6B 1.367(14) . ? C6B C7B 1.368(13) . ? C7B C8B 1.381(13) . ? C8B C9B 1.406(12) . ? C8B C10B 1.489(12) . ? C10B N4B 1.499(11) . ? N4B C11B 1.463(12) . ? C11B C12B 1.514(14) . ? C1C C2C 1.398(19) . ? C2C N3C 1.551(19) . ? N3C C3C 1.25(2) . ? C3C C4C 1.61(3) . ? N3C' C3C' 1.23(2) . ? C3C' C4C 1.52(3) . ? C4C C9C 1.344(17) . ? C4C C5C 1.41(2) . ? C5C C6C 1.378(18) . ? C6C C7C 1.381(17) . ? C7C C8C 1.356(16) . ? C8C C9C 1.322(15) . ? C8C C10C 1.516(17) . ? C10C N4C 1.471(16) . ? N4C C11C 1.494(13) . ? C11C C12C 1.444(16) . ? C20 O23 1.259(10) . ? C20 O22 1.260(10) . ? C20 O21 1.266(10) . ? Co3 O31 1.951(6) . ? Co3 N3E 2.088(7) . ? Co3 N3D 2.099(8) . ? Co3 N3F 2.138(10) . ? Co3 N5 2.281(7) . ? Co3 Co4 5.1291(17) . ? Co4 O33 2.024(6) . ? Co4 N6 2.139(7) . ? Co4 O32 2.208(6) . ? Co4 N4E 2.212(7) . ? Co4 N4D 2.229(7) . ? Co4 N4F 2.244(8) . ? Co4 C30 2.474(10) . ? N5 C1F 1.448(15) . ? N5 C1D 1.460(13) . ? N5 C1E 1.462(13) . ? C1D C2D 1.485(14) . ? C2D N3D 1.470(12) . ? N3D C3D 1.479(12) . ? C3D C4D 1.483(15) . ? C4D C9D 1.373(13) . ? C4D C5D 1.386(15) . ? C5D C6D 1.319(18) . ? C6D C7D 1.443(16) . ? C7D C8D 1.396(14) . ? C8D C9D 1.371(14) . ? C8D C10D 1.490(14) . ? C10D N4D 1.443(13) . ? N4D C11D 1.500(13) . ? C11D C12D 1.530(14) . ? C12D N6 1.473(13) . ? N6 C12F 1.454(13) . ? N6 C12E 1.453(13) . ? C1E C2E 1.479(14) . ? C2E N3E 1.479(13) . ? N3E C3E 1.520(12) . ? C3E C4E 1.518(13) . ? C4E C5E 1.373(14) . ? C4E C9E 1.386(14) . ? C5E C6E 1.421(17) . ? C6E C7E 1.315(17) . ? C7E C8E 1.379(15) . ? C8E C9E 1.391(13) . ? C8E C10E 1.526(14) . ? C10E N4E 1.452(11) . ? N4E C11E 1.441(13) . ? C11E C12E 1.525(14) . ? C1F C2F 1.515(16) . ? C2F N3F 1.479(14) . ? N3F C3F 1.64(2) . ? C3F C4F 1.35(3) . ? C3F' C4F 1.78(4) . ? C4F C9F 1.392(17) . ? C4F C5F 1.58(2) . ? C5F C6F 1.307(19) . ? C6F C7F 1.26(2) . ? C7F C8F 1.24(2) . ? C8F C9F 1.313(15) . ? C8F C10F 1.65(2) . ? C10F N4F 1.373(17) . ? N4F C11F 1.448(16) . ? C11F C12F 1.516(16) . ? C30 O32 1.273(11) . ? C30 O31 1.273(11) . ? C30 O33 1.291(11) . ? Cl5 O51 1.297(13) . ? Cl5 O52 1.367(10) . ? Cl5 O54 1.397(16) . ? Cl5 O53 1.415(14) . ? Cl6 O64 1.324(14) . ? Cl6 O62 1.358(8) . ? Cl6 O63 1.399(10) . ? Cl6 O61 1.525(13) . ? Cl7 O71 1.306(10) . ? Cl7 O73 1.337(12) . ? Cl7 O74 1.38(2) . ? Cl7 O72 1.398(8) . ? Cl8 O83 1.362(13) . ? Cl8 O81 1.394(10) . ? Cl8 O82 1.400(14) . ? Cl8 O84 1.400(16) . ? 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 O21 Co1 N3C 98.5(5) . . ? O21 Co1 N3B 100.6(3) . . ? N3C Co1 N3B 130.6(8) . . ? O21 Co1 N3A 93.9(2) . . ? N3C Co1 N3A 119.6(9) . . ? N3B Co1 N3A 104.0(3) . . ? O21 Co1 N1 174.0(3) . . ? N3C Co1 N1 84.7(5) . . ? N3B Co1 N1 80.9(3) . . ? N3A Co1 N1 80.1(3) . . ? O21 Co1 N3C' 106.2(5) . . ? N3C Co1 N3C' 21.0(7) . . ? N3B Co1 N3C' 143.0(4) . . ? N3A Co1 N3C' 99.1(5) . . ? N1 Co1 N3C' 75.1(5) . . ? O21 Co1 O1W' 84.6(6) . . ? N3C Co1 O1W' 61.2(10) . . ? N3B Co1 O1W' 75.7(5) . . ? N3A Co1 O1W' 178.4(6) . . ? N1 Co1 O1W' 101.3(6) . . ? N3C' Co1 O1W' 81.8(7) . . ? O21 Co1 O1W 85.8(8) . . ? N3C Co1 O1W 65.6(12) . . ? N3B Co1 O1W 70.8(8) . . ? N3A Co1 O1W 174.7(8) . . ? N1 Co1 O1W 100.2(8) . . ? N3C' Co1 O1W 86.0(10) . . ? O1W' Co1 O1W 4.9(11) . . ? O21 Co1 Co2 8.06(18) . . ? N3C Co1 Co2 92.7(5) . . ? N3B Co1 Co2 100.38(19) . . ? N3A Co1 Co2 101.74(18) . . ? N1 Co1 Co2 177.4(2) . . ? N3C' Co1 Co2 102.7(4) . . ? O1W' Co1 Co2 76.8(6) . . ? O1W Co1 Co2 78.2(8) . . ? O22 Co2 N4C 103.9(3) . . ? O22 Co2 N4B 99.3(3) . . ? N4C Co2 N4B 142.9(3) . . ? O22 Co2 N4A 93.9(3) . . ? N4C Co2 N4A 103.6(3) . . ? N4B Co2 N4A 103.1(3) . . ? O22 Co2 N2 174.1(3) . . ? N4C Co2 N2 79.4(3) . . ? N4B Co2 N2 80.2(3) . . ? N4A Co2 N2 80.5(3) . . ? O22 Co2 O2W 86.3(2) . . ? N4C Co2 O2W 79.9(3) . . ? N4B Co2 O2W 73.3(3) . . ? N4A Co2 O2W 176.4(3) . . ? N2 Co2 O2W 99.2(3) . . ? O22 Co2 Co1 8.52(18) . . ? N4C Co2 Co1 100.1(3) . . ? N4B Co2 Co1 98.71(19) . . ? N4A Co2 Co1 102.27(18) . . ? N2 Co2 Co1 177.2(2) . . ? O2W Co2 Co1 78.02(18) . . ? C1B N1 C1C 112.7(8) . . ? C1B N1 C1A 111.3(9) . . ? C1C N1 C1A 111.9(9) . . ? C1B N1 Co1 105.1(5) . . ? C1C N1 Co1 107.0(7) . . ? C1A N1 Co1 108.5(6) . . ? C2A C1A N1 109.8(9) . . ? N3A C2A C1A 109.3(9) . . ? C3A N3A C2A 110.5(7) . . ? C3A N3A Co1 117.3(6) . . ? C2A N3A Co1 107.0(5) . . ? N3A C3A C4A 114.8(8) . . ? C5A C4A C9A 119.1(8) . . ? C5A C4A C3A 122.2(8) . . ? C9A C4A C3A 118.7(8) . . ? C4A C5A C6A 119.5(9) . . ? C5A C6A C7A 120.6(9) . . ? C8A C7A C6A 121.6(8) . . ? C7A C8A C9A 118.4(8) . . ? C7A C8A C10A 122.7(8) . . ? C9A C8A C10A 118.9(8) . . ? C8A C9A C4A 120.9(8) . . ? C8A C10A N4A 113.6(7) . . ? C11A N4A C10A 111.5(7) . . ? C11A N4A Co2 107.7(5) . . ? C10A N4A Co2 117.4(6) . . ? N4A C11A C12A 109.3(7) . . ? N2 C12A C11A 109.6(8) . . ? C12C N2 C12B 113.7(7) . . ? C12C N2 C12A 109.0(7) . . ? C12B N2 C12A 109.9(8) . . ? C12C N2 Co2 109.9(6) . . ? C12B N2 Co2 106.3(5) . . ? C12A N2 Co2 107.9(5) . . ? N1 C1B C2B 111.8(8) . . ? N3B C2B C1B 109.6(8) . . ? C2B N3B C3B 112.1(7) . . ? C2B N3B Co1 110.6(6) . . ? C3B N3B Co1 115.6(5) . . ? N3B C3B C4B 111.3(7) . . ? C5B C4B C9B 119.2(9) . . ? C5B C4B C3B 120.2(8) . . ? C9B C4B C3B 120.6(8) . . ? C4B C5B C6B 121.3(9) . . ? C7B C6B C5B 119.5(9) . . ? C6B C7B C8B 121.5(9) . . ? C7B C8B C9B 117.3(8) . . ? C7B C8B C10B 120.7(8) . . ? C9B C8B C10B 122.0(8) . . ? C4B C9B C8B 121.2(8) . . ? C8B C10B N4B 110.8(7) . . ? C11B N4B C10B 112.4(7) . . ? C11B N4B Co2 111.0(5) . . ? C10B N4B Co2 114.7(5) . . ? N4B C11B C12B 109.8(8) . . ? N2 C12B C11B 109.3(7) . . ? C2C C1C N1 113.3(10) . . ? C1C C2C N3C 118.6(14) . . ? C3C N3C C2C 114.7(16) . . ? C3C N3C Co1 141.1(15) . . ? C2C N3C Co1 103.1(11) . . ? N3C C3C C4C 117.7(19) . . ? C3C' N3C' Co1 128.9(18) . . ? N3C' C3C' C4C 131(2) . . ? C9C C4C C5C 116.8(12) . . ? C9C C4C C3C' 136.4(19) . . ? C5C C4C C3C' 106.8(17) . . ? C9C C4C C3C 108.4(15) . . ? C5C C4C C3C 134.5(14) . . ? C3C' C4C C3C 28.2(13) . . ? C6C C5C C4C 119.1(12) . . ? C5C C6C C7C 119.2(12) . . ? C8C C7C C6C 121.4(11) . . ? C9C C8C C7C 117.4(11) . . ? C9C C8C C10C 118.6(11) . . ? C7C C8C C10C 123.9(11) . . ? C8C C9C C4C 126.0(12) . . ? N4C C10C C8C 112.5(10) . . ? C10C N4C C11C 109.9(9) . . ? C10C N4C Co2 123.7(8) . . ? C11C N4C Co2 104.2(6) . . ? C12C C11C N4C 110.2(9) . . ? C11C C12C N2 109.6(8) . . ? O23 C20 O22 121.5(7) . . ? O23 C20 O21 121.4(8) . . ? O22 C20 O21 117.1(7) . . ? C20 O21 Co1 141.4(6) . . ? C20 O22 Co2 139.6(5) . . ? O31 Co3 N3E 109.3(3) . . ? O31 Co3 N3D 98.5(3) . . ? N3E Co3 N3D 119.8(3) . . ? O31 Co3 N3F 93.6(3) . . ? N3E Co3 N3F 116.6(4) . . ? N3D Co3 N3F 113.5(4) . . ? O31 Co3 N5 170.9(3) . . ? N3E Co3 N5 79.5(3) . . ? N3D Co3 N5 78.4(3) . . ? N3F Co3 N5 79.9(3) . . ? O31 Co3 Co4 36.44(18) . . ? N3E Co3 Co4 73.3(2) . . ? N3D Co3 Co4 112.3(2) . . ? N3F Co3 Co4 115.2(3) . . ? N5 Co3 Co4 152.6(2) . . ? O33 Co4 N6 163.6(3) . . ? O33 Co4 O32 62.3(2) . . ? N6 Co4 O32 101.7(3) . . ? O33 Co4 N4E 114.9(3) . . ? N6 Co4 N4E 81.2(3) . . ? O32 Co4 N4E 177.2(3) . . ? O33 Co4 N4D 98.7(3) . . ? N6 Co4 N4D 80.2(3) . . ? O32 Co4 N4D 79.6(3) . . ? N4E Co4 N4D 100.6(3) . . ? O33 Co4 N4F 95.6(3) . . ? N6 Co4 N4F 80.1(3) . . ? O32 Co4 N4F 88.6(4) . . ? N4E Co4 N4F 92.2(4) . . ? N4D Co4 N4F 154.5(3) . . ? O33 Co4 C30 31.4(3) . . ? N6 Co4 C30 132.5(3) . . ? O32 Co4 C30 30.9(3) . . ? N4E Co4 C30 146.3(3) . . ? N4D Co4 C30 88.3(3) . . ? N4F Co4 C30 93.2(4) . . ? O33 Co4 Co3 11.91(17) . . ? N6 Co4 Co3 151.9(2) . . ? O32 Co4 Co3 50.37(16) . . ? N4E Co4 Co3 126.8(2) . . ? N4D Co4 Co3 94.89(19) . . ? N4F Co4 Co3 94.8(3) . . ? C30 Co4 Co3 19.5(2) . . ? C1F N5 C1D 113.0(9) . . ? C1F N5 C1E 110.3(8) . . ? C1D N5 C1E 112.8(8) . . ? C1F N5 Co3 107.2(6) . . ? C1D N5 Co3 107.4(5) . . ? C1E N5 Co3 105.6(6) . . ? N5 C1D C2D 110.6(8) . . ? N3D C2D C1D 108.0(9) . . ? C2D N3D C3D 115.9(8) . . ? C2D N3D Co3 108.7(5) . . ? C3D N3D Co3 120.3(6) . . ? N3D C3D C4D 115.7(8) . . ? C9D C4D C5D 116.3(10) . . ? C9D C4D C3D 120.7(9) . . ? C5D C4D C3D 123.0(9) . . ? C6D C5D C4D 123.5(10) . . ? C5D C6D C7D 120.3(11) . . ? C8D C7D C6D 116.9(11) . . ? C9D C8D C7D 119.5(9) . . ? C9D C8D C10D 123.6(9) . . ? C7D C8D C10D 116.8(10) . . ? C8D C9D C4D 123.4(9) . . ? N4D C10D C8D 117.8(8) . . ? C10D N4D C11D 108.3(8) . . ? C10D N4D Co4 127.2(7) . . ? C11D N4D Co4 109.2(6) . . ? N4D C11D C12D 106.3(8) . . ? N6 C12D C11D 110.3(8) . . ? C12F N6 C12E 110.2(8) . . ? C12F N6 C12D 108.9(8) . . ? C12E N6 C12D 113.3(9) . . ? C12F N6 Co4 107.3(6) . . ? C12E N6 Co4 110.4(6) . . ? C12D N6 Co4 106.5(5) . . ? N5 C1E C2E 113.1(8) . . ? N3E C2E C1E 107.6(7) . . ? C2E N3E C3E 112.7(7) . . ? C2E N3E Co3 110.2(6) . . ? C3E N3E Co3 114.9(5) . . ? C4E C3E N3E 109.8(7) . . ? C5E C4E C9E 119.2(9) . . ? C5E C4E C3E 122.4(10) . . ? C9E C4E C3E 118.2(8) . . ? C4E C5E C6E 119.0(11) . . ? C7E C6E C5E 120.7(10) . . ? C6E C7E C8E 121.7(10) . . ? C7E C8E C9E 118.7(10) . . ? C7E C8E C10E 125.0(8) . . ? C9E C8E C10E 116.2(8) . . ? C4E C9E C8E 120.6(9) . . ? N4E C10E C8E 112.9(8) . . ? C11E N4E C10E 107.8(8) . . ? C11E N4E Co4 105.2(6) . . ? C10E N4E Co4 125.4(6) . . ? N4E C11E C12E 111.4(9) . . ? N6 C12E C11E 113.7(8) . . ? N5 C1F C2F 110.5(9) . . ? N3F C2F C1F 110.0(9) . . ? C2F N3F C3F 105.8(11) . . ? C2F N3F Co3 107.4(7) . . ? C3F N3F Co3 119.4(9) . . ? C4F C3F N3F 113.8(16) . . ? C3F C4F C9F 133.9(17) . . ? C3F C4F C5F 117.7(15) . . ? C9F C4F C5F 108.4(11) . . ? C3F C4F C3F' 33(2) . . ? C9F C4F C3F' 101(2) . . ? C5F C4F C3F' 151(2) . . ? C6F C5F C4F 116.3(12) . . ? C7F C6F C5F 127.5(17) . . ? C8F C7F C6F 118.5(17) . . ? C7F C8F C9F 125.6(15) . . ? C7F C8F C10F 122.6(15) . . ? C9F C8F C10F 111.5(12) . . ? C8F C9F C4F 123.4(12) . . ? N4F C10F C8F 112.2(11) . . ? C10F N4F C11F 108.4(10) . . ? C10F N4F Co4 123.7(10) . . ? C11F N4F Co4 107.0(7) . . ? N4F C11F C12F 111.1(9) . . ? N6 C12F C11F 108.9(8) . . ? O32 C30 O31 121.4(8) . . ? O32 C30 O33 117.6(8) . . ? O31 C30 O33 121.0(8) . . ? O32 C30 Co4 62.9(5) . . ? O31 C30 Co4 175.1(7) . . ? O33 C30 Co4 54.7(4) . . ? C30 O31 Co3 128.3(6) . . ? C30 O32 Co4 86.2(5) . . ? C30 O33 Co4 93.9(5) . . ? O51 Cl5 O52 122.6(8) . . ? O51 Cl5 O54 108.1(12) . . ? O52 Cl5 O54 116.9(9) . . ? O51 Cl5 O53 113.7(11) . . ? O52 Cl5 O53 103.3(9) . . ? O54 Cl5 O53 86.2(13) . . ? O64 Cl6 O62 117.6(8) . . ? O64 Cl6 O63 117.7(9) . . ? O62 Cl6 O63 111.8(7) . . ? O64 Cl6 O61 95.5(9) . . ? O62 Cl6 O61 104.1(9) . . ? O63 Cl6 O61 106.8(7) . . ? O71 Cl7 O73 119.6(7) . . ? O71 Cl7 O74 105.4(13) . . ? O73 Cl7 O74 86.1(12) . . ? O71 Cl7 O72 116.8(6) . . ? O73 Cl7 O72 118.9(7) . . ? O74 Cl7 O72 100.1(9) . . ? O83 Cl8 O81 114.4(15) . . ? O83 Cl8 O82 106.7(18) . . ? O81 Cl8 O82 108.5(15) . . ? O83 Cl8 O84 106.9(17) . . ? O81 Cl8 O84 109.7(11) . . ? O82 Cl8 O84 110.7(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O21 Co1 Co2 O22 3.4(17) . . . . ? N3C Co1 Co2 O22 -132.2(14) . . . . ? N3B Co1 Co2 O22 95.7(12) . . . . ? N3A Co1 Co2 O22 -11.2(12) . . . . ? N1 Co1 Co2 O22 -146(5) . . . . ? N3C' Co1 Co2 O22 -113.5(12) . . . . ? O1W' Co1 Co2 O22 168.2(13) . . . . ? O1W Co1 Co2 O22 163.4(14) . . . . ? O21 Co1 Co2 N4C 120.5(13) . . . . ? N3C Co1 Co2 N4C -15.1(9) . . . . ? N3B Co1 Co2 N4C -147.2(3) . . . . ? N3A Co1 Co2 N4C 105.9(3) . . . . ? N1 Co1 Co2 N4C -29(5) . . . . ? N3C' Co1 Co2 N4C 3.6(5) . . . . ? O1W' Co1 Co2 N4C -74.7(6) . . . . ? O1W Co1 Co2 N4C -79.5(9) . . . . ? O21 Co1 Co2 N4B -91.6(13) . . . . ? N3C Co1 Co2 N4B 132.8(8) . . . . ? N3B Co1 Co2 N4B 0.7(3) . . . . ? N3A Co1 Co2 N4B -106.2(3) . . . . ? N1 Co1 Co2 N4B 119(5) . . . . ? N3C' Co1 Co2 N4B 151.6(5) . . . . ? O1W' Co1 Co2 N4B 73.2(6) . . . . ? O1W Co1 Co2 N4B 68.4(8) . . . . ? O21 Co1 Co2 N4A 14.0(13) . . . . ? N3C Co1 Co2 N4A -121.6(8) . . . . ? N3B Co1 Co2 N4A 106.3(3) . . . . ? N3A Co1 Co2 N4A -0.6(3) . . . . ? N1 Co1 Co2 N4A -135(5) . . . . ? N3C' Co1 Co2 N4A -102.9(5) . . . . ? O1W' Co1 Co2 N4A 178.8(6) . . . . ? O1W Co1 Co2 N4A 174.0(8) . . . . ? O21 Co1 Co2 N2 -159(5) . . . . ? N3C Co1 Co2 N2 66(4) . . . . ? N3B Co1 Co2 N2 -66(4) . . . . ? N3A Co1 Co2 N2 -173(4) . . . . ? N1 Co1 Co2 N2 52(6) . . . . ? N3C' Co1 Co2 N2 85(4) . . . . ? O1W' Co1 Co2 N2 6(4) . . . . ? O1W Co1 Co2 N2 1(4) . . . . ? O21 Co1 Co2 O2W -162.3(13) . . . . ? N3C Co1 Co2 O2W 62.1(8) . . . . ? N3B Co1 Co2 O2W -70.0(3) . . . . ? N3A Co1 Co2 O2W -176.9(3) . . . . ? N1 Co1 Co2 O2W 49(5) . . . . ? N3C' Co1 Co2 O2W 80.8(5) . . . . ? O1W' Co1 Co2 O2W 2.5(6) . . . . ? O1W Co1 Co2 O2W -2.3(8) . . . . ? O21 Co1 N1 C1B 125(3) . . . . ? N3C Co1 N1 C1B -112.1(10) . . . . ? N3B Co1 N1 C1B 20.4(6) . . . . ? N3A Co1 N1 C1B 126.5(7) . . . . ? N3C' Co1 N1 C1B -131.2(8) . . . . ? O1W' Co1 N1 C1B -52.9(8) . . . . ? O1W Co1 N1 C1B -48.1(10) . . . . ? Co2 Co1 N1 C1B -99(5) . . . . ? O21 Co1 N1 C1C -115(3) . . . . ? N3C Co1 N1 C1C 7.9(10) . . . . ? N3B Co1 N1 C1C 140.4(7) . . . . ? N3A Co1 N1 C1C -113.5(7) . . . . ? N3C' Co1 N1 C1C -11.2(8) . . . . ? O1W' Co1 N1 C1C 67.1(8) . . . . ? O1W Co1 N1 C1C 71.9(10) . . . . ? Co2 Co1 N1 C1C 21(5) . . . . ? O21 Co1 N1 C1A 6(3) . . . . ? N3C Co1 N1 C1A 128.7(11) . . . . ? N3B Co1 N1 C1A -98.7(8) . . . . ? N3A Co1 N1 C1A 7.4(7) . . . . ? N3C' Co1 N1 C1A 109.7(9) . . . . ? O1W' Co1 N1 C1A -172.1(9) . . . . ? O1W Co1 N1 C1A -167.2(11) . . . . ? Co2 Co1 N1 C1A 142(4) . . . . ? C1B N1 C1A C2A -150.5(9) . . . . ? C1C N1 C1A C2A 82.5(12) . . . . ? Co1 N1 C1A C2A -35.3(11) . . . . ? N1 C1A C2A N3A 56.5(13) . . . . ? C1A C2A N3A C3A -176.3(9) . . . . ? C1A C2A N3A Co1 -47.5(10) . . . . ? O21 Co1 N3A C3A -34.2(6) . . . . ? N3C Co1 N3A C3A 67.9(8) . . . . ? N3B Co1 N3A C3A -136.1(6) . . . . ? N1 Co1 N3A C3A 146.0(7) . . . . ? N3C' Co1 N3A C3A 73.0(7) . . . . ? O1W' Co1 N3A C3A -56(20) . . . . ? O1W Co1 N3A C3A -121(8) . . . . ? Co2 Co1 N3A C3A -32.1(6) . . . . ? O21 Co1 N3A C2A -158.9(7) . . . . ? N3C Co1 N3A C2A -56.9(8) . . . . ? N3B Co1 N3A C2A 99.1(7) . . . . ? N1 Co1 N3A C2A 21.2(7) . . . . ? N3C' Co1 N3A C2A -51.8(8) . . . . ? O1W' Co1 N3A C2A 179(100) . . . . ? O1W Co1 N3A C2A 114(8) . . . . ? Co2 Co1 N3A C2A -156.9(6) . . . . ? C2A N3A C3A C4A -160.4(8) . . . . ? Co1 N3A C3A C4A 76.6(9) . . . . ? N3A C3A C4A C5A 57.0(12) . . . . ? N3A C3A C4A C9A -125.1(9) . . . . ? C9A C4A C5A C6A 1.1(13) . . . . ? C3A C4A C5A C6A 179.0(9) . . . . ? C4A C5A C6A C7A -1.6(15) . . . . ? C5A C6A C7A C8A 1.0(15) . . . . ? C6A C7A C8A C9A 0.0(13) . . . . ? C6A C7A C8A C10A -178.2(8) . . . . ? C7A C8A C9A C4A -0.4(12) . . . . ? C10A C8A C9A C4A 177.8(7) . . . . ? C5A C4A C9A C8A -0.2(12) . . . . ? C3A C4A C9A C8A -178.2(7) . . . . ? C7A C8A C10A N4A -57.7(11) . . . . ? C9A C8A C10A N4A 124.1(8) . . . . ? C8A C10A N4A C11A 158.9(8) . . . . ? C8A C10A N4A Co2 -76.1(9) . . . . ? O22 Co2 N4A C11A 161.9(6) . . . . ? N4C Co2 N4A C11A 56.6(6) . . . . ? N4B Co2 N4A C11A -97.5(6) . . . . ? N2 Co2 N4A C11A -20.0(6) . . . . ? O2W Co2 N4A C11A -106(4) . . . . ? Co1 Co2 N4A C11A 160.4(5) . . . . ? O22 Co2 N4A C10A 35.1(6) . . . . ? N4C Co2 N4A C10A -70.2(6) . . . . ? N4B Co2 N4A C10A 135.6(6) . . . . ? N2 Co2 N4A C10A -146.8(6) . . . . ? O2W Co2 N4A C10A 128(4) . . . . ? Co1 Co2 N4A C10A 33.5(6) . . . . ? C10A N4A C11A C12A 176.4(8) . . . . ? Co2 N4A C11A C12A 46.2(9) . . . . ? N4A C11A C12A N2 -56.4(11) . . . . ? C11A C12A N2 C12C -83.0(10) . . . . ? C11A C12A N2 C12B 151.8(8) . . . . ? C11A C12A N2 Co2 36.3(9) . . . . ? O22 Co2 N2 C12C 129(2) . . . . ? N4C Co2 N2 C12C 3.9(6) . . . . ? N4B Co2 N2 C12C -145.0(6) . . . . ? N4A Co2 N2 C12C 109.8(6) . . . . ? O2W Co2 N2 C12C -73.9(6) . . . . ? Co1 Co2 N2 C12C -78(4) . . . . ? O22 Co2 N2 C12B -108(2) . . . . ? N4C Co2 N2 C12B 127.4(6) . . . . ? N4B Co2 N2 C12B -21.5(6) . . . . ? N4A Co2 N2 C12B -126.7(6) . . . . ? O2W Co2 N2 C12B 49.6(6) . . . . ? Co1 Co2 N2 C12B 46(5) . . . . ? O22 Co2 N2 C12A 10(3) . . . . ? N4C Co2 N2 C12A -114.8(7) . . . . ? N4B Co2 N2 C12A 96.3(7) . . . . ? N4A Co2 N2 C12A -9.0(6) . . . . ? O2W Co2 N2 C12A 167.4(6) . . . . ? Co1 Co2 N2 C12A 164(4) . . . . ? C1C N1 C1B C2B -161.2(9) . . . . ? C1A N1 C1B C2B 72.2(11) . . . . ? Co1 N1 C1B C2B -45.0(9) . . . . ? N1 C1B C2B N3B 53.2(11) . . . . ? C1B C2B N3B C3B -162.5(8) . . . . ? C1B C2B N3B Co1 -32.0(10) . . . . ? O21 Co1 N3B C2B -167.9(6) . . . . ? N3C Co1 N3B C2B 81.1(10) . . . . ? N3A Co1 N3B C2B -71.1(7) . . . . ? N1 Co1 N3B C2B 6.2(6) . . . . ? N3C' Co1 N3B C2B 56.0(11) . . . . ? O1W' Co1 N3B C2B 110.5(9) . . . . ? O1W Co1 N3B C2B 110.4(11) . . . . ? Co2 Co1 N3B C2B -176.1(6) . . . . ? O21 Co1 N3B C3B -39.2(6) . . . . ? N3C Co1 N3B C3B -150.1(9) . . . . ? N3A Co1 N3B C3B 57.6(6) . . . . ? N1 Co1 N3B C3B 134.9(6) . . . . ? N3C' Co1 N3B C3B -175.2(9) . . . . ? O1W' Co1 N3B C3B -120.8(8) . . . . ? O1W Co1 N3B C3B -120.9(10) . . . . ? Co2 Co1 N3B C3B -47.4(6) . . . . ? C2B N3B C3B C4B -143.8(8) . . . . ? Co1 N3B C3B C4B 88.2(8) . . . . ? N3B C3B C4B C5B 64.7(11) . . . . ? N3B C3B C4B C9B -117.1(9) . . . . ? C9B C4B C5B C6B -0.1(14) . . . . ? C3B C4B C5B C6B 178.1(9) . . . . ? C4B C5B C6B C7B 1.3(16) . . . . ? C5B C6B C7B C8B -0.5(15) . . . . ? C6B C7B C8B C9B -1.4(13) . . . . ? C6B C7B C8B C10B -178.5(8) . . . . ? C5B C4B C9B C8B -1.9(12) . . . . ? C3B C4B C9B C8B 179.9(7) . . . . ? C7B C8B C9B C4B 2.6(12) . . . . ? C10B C8B C9B C4B 179.7(7) . . . . ? C7B C8B C10B N4B -62.6(10) . . . . ? C9B C8B C10B N4B 120.4(8) . . . . ? C8B C10B N4B C11B 141.0(8) . . . . ? C8B C10B N4B Co2 -90.9(7) . . . . ? O22 Co2 N4B C11B 167.5(6) . . . . ? N4C Co2 N4B C11B -64.0(8) . . . . ? N4A Co2 N4B C11B 71.3(6) . . . . ? N2 Co2 N4B C11B -6.5(6) . . . . ? O2W Co2 N4B C11B -109.3(6) . . . . ? Co1 Co2 N4B C11B 176.1(5) . . . . ? O22 Co2 N4B C10B 38.7(6) . . . . ? N4C Co2 N4B C10B 167.2(6) . . . . ? N4A Co2 N4B C10B -57.5(6) . . . . ? N2 Co2 N4B C10B -135.3(6) . . . . ? O2W Co2 N4B C10B 121.9(6) . . . . ? Co1 Co2 N4B C10B 47.3(5) . . . . ? C10B N4B C11B C12B 163.3(7) . . . . ? Co2 N4B C11B C12B 33.3(9) . . . . ? C12C N2 C12B C11B 166.9(8) . . . . ? C12A N2 C12B C11B -70.7(10) . . . . ? Co2 N2 C12B C11B 45.8(9) . . . . ? N4B C11B C12B N2 -53.9(10) . . . . ? C1B N1 C1C C2C 86.5(12) . . . . ? C1A N1 C1C C2C -147.2(11) . . . . ? Co1 N1 C1C C2C -28.5(12) . . . . ? N1 C1C C2C N3C 44.2(19) . . . . ? C1C C2C N3C C3C 137(3) . . . . ? C1C C2C N3C Co1 -34(2) . . . . ? O21 Co1 N3C C3C 20(4) . . . . ? N3B Co1 N3C C3C 132(4) . . . . ? N3A Co1 N3C C3C -80(4) . . . . ? N1 Co1 N3C C3C -155(4) . . . . ? N3C' Co1 N3C C3C -94(5) . . . . ? O1W' Co1 N3C C3C 99(4) . . . . ? O1W Co1 N3C C3C 101(4) . . . . ? Co2 Co1 N3C C3C 26(4) . . . . ? O21 Co1 N3C C2C -173.7(14) . . . . ? N3B Co1 N3C C2C -61.8(19) . . . . ? N3A Co1 N3C C2C 86.9(16) . . . . ? N1 Co1 N3C C2C 11.4(15) . . . . ? N3C' Co1 N3C C2C 72.9(14) . . . . ? O1W' Co1 N3C C2C -94.6(17) . . . . ? O1W Co1 N3C C2C -92.2(18) . . . . ? Co2 Co1 N3C C2C -168.0(15) . . . . ? C2C N3C C3C C4C -147(2) . . . . ? Co1 N3C C3C C4C 18(5) . . . . ? O21 Co1 N3C' C3C' -5(3) . . . . ? N3C Co1 N3C' C3C' 65(3) . . . . ? N3B Co1 N3C' C3C' 129(2) . . . . ? N3A Co1 N3C' C3C' -102(3) . . . . ? N1 Co1 N3C' C3C' -179(3) . . . . ? O1W' Co1 N3C' C3C' 76(3) . . . . ? O1W Co1 N3C' C3C' 79(3) . . . . ? Co2 Co1 N3C' C3C' 2(3) . . . . ? Co1 N3C' C3C' C4C 15(5) . . . . ? N3C' C3C' C4C C9C -86(4) . . . . ? N3C' C3C' C4C C5C 95(4) . . . . ? N3C' C3C' C4C C3C -95(4) . . . . ? N3C C3C C4C C9C -105(3) . . . . ? N3C C3C C4C C5C 82(3) . . . . ? N3C C3C C4C C3C' 69(3) . . . . ? C9C C4C C5C C6C 0.1(17) . . . . ? C3C' C4C C5C C6C 179.4(14) . . . . ? C3C C4C C5C C6C 172.9(14) . . . . ? C4C C5C C6C C7C -0.5(17) . . . . ? C5C C6C C7C C8C 0.7(17) . . . . ? C6C C7C C8C C9C -0.5(16) . . . . ? C6C C7C C8C C10C -176.6(10) . . . . ? C7C C8C C9C C4C 0.1(16) . . . . ? C10C C8C C9C C4C 176.4(11) . . . . ? C5C C4C C9C C8C 0.1(17) . . . . ? C3C' C4C C9C C8C -178.9(18) . . . . ? C3C C4C C9C C8C -174.5(11) . . . . ? C9C C8C C10C N4C 126.7(12) . . . . ? C7C C8C C10C N4C -57.3(16) . . . . ? C8C C10C N4C C11C 169.4(10) . . . . ? C8C C10C N4C Co2 -66.9(14) . . . . ? O22 Co2 N4C C10C 29.1(9) . . . . ? N4B Co2 N4C C10C -98.1(9) . . . . ? N4A Co2 N4C C10C 126.7(9) . . . . ? N2 Co2 N4C C10C -155.9(9) . . . . ? O2W Co2 N4C C10C -54.4(9) . . . . ? Co1 Co2 N4C C10C 21.3(9) . . . . ? O22 Co2 N4C C11C 155.3(7) . . . . ? N4B Co2 N4C C11C 28.0(10) . . . . ? N4A Co2 N4C C11C -107.1(7) . . . . ? N2 Co2 N4C C11C -29.7(7) . . . . ? O2W Co2 N4C C11C 71.8(7) . . . . ? Co1 Co2 N4C C11C 147.5(7) . . . . ? C10C N4C C11C C12C -171.0(10) . . . . ? Co2 N4C C11C C12C 54.5(10) . . . . ? N4C C11C C12C N2 -53.5(11) . . . . ? C12B N2 C12C C11C -94.5(10) . . . . ? C12A N2 C12C C11C 142.6(9) . . . . ? Co2 N2 C12C C11C 24.6(10) . . . . ? O23 C20 O21 Co1 2.8(13) . . . . ? O22 C20 O21 Co1 -175.5(6) . . . . ? N3C Co1 O21 C20 59.4(12) . . . . ? N3B Co1 O21 C20 -74.8(9) . . . . ? N3A Co1 O21 C20 -179.9(9) . . . . ? N1 Co1 O21 C20 -179(100) . . . . ? N3C' Co1 O21 C20 79.4(10) . . . . ? O1W' Co1 O21 C20 -0.4(10) . . . . ? O1W Co1 O21 C20 -5.2(12) . . . . ? Co2 Co1 O21 C20 14.4(8) . . . . ? O23 C20 O22 Co2 -1.2(13) . . . . ? O21 C20 O22 Co2 177.1(5) . . . . ? N4C Co2 O22 C20 -77.0(8) . . . . ? N4B Co2 O22 C20 73.9(8) . . . . ? N4A Co2 O22 C20 178.0(8) . . . . ? N2 Co2 O22 C20 159(2) . . . . ? O2W Co2 O22 C20 1.6(8) . . . . ? Co1 Co2 O22 C20 -12.4(8) . . . . ? O31 Co3 Co4 O33 177.4(10) . . . . ? N3E Co3 Co4 O33 -11.9(9) . . . . ? N3D Co3 Co4 O33 104.0(9) . . . . ? N3F Co3 Co4 O33 -123.9(10) . . . . ? N5 Co3 Co4 O33 -4.6(10) . . . . ? O31 Co3 Co4 N6 -10.4(6) . . . . ? N3E Co3 Co4 N6 160.3(5) . . . . ? N3D Co3 Co4 N6 -83.8(5) . . . . ? N3F Co3 Co4 N6 48.3(6) . . . . ? N5 Co3 Co4 N6 167.6(6) . . . . ? O31 Co3 Co4 O32 -4.2(4) . . . . ? N3E Co3 Co4 O32 166.5(3) . . . . ? N3D Co3 Co4 O32 -77.6(3) . . . . ? N3F Co3 Co4 O32 54.4(4) . . . . ? N5 Co3 Co4 O32 173.8(5) . . . . ? O31 Co3 Co4 N4E 175.2(4) . . . . ? N3E Co3 Co4 N4E -14.2(3) . . . . ? N3D Co3 Co4 N4E 101.8(4) . . . . ? N3F Co3 Co4 N4E -126.2(4) . . . . ? N5 Co3 Co4 N4E -6.9(5) . . . . ? O31 Co3 Co4 N4D 68.0(4) . . . . ? N3E Co3 Co4 N4D -121.3(3) . . . . ? N3D Co3 Co4 N4D -5.4(3) . . . . ? N3F Co3 Co4 N4D 126.6(4) . . . . ? N5 Co3 Co4 N4D -114.1(5) . . . . ? O31 Co3 Co4 N4F -88.4(4) . . . . ? N3E Co3 Co4 N4F 82.3(3) . . . . ? N3D Co3 Co4 N4F -161.8(4) . . . . ? N3F Co3 Co4 N4F -29.7(4) . . . . ? N5 Co3 Co4 N4F 89.6(5) . . . . ? O31 Co3 Co4 C30 -2.6(7) . . . . ? N3E Co3 Co4 C30 168.1(6) . . . . ? N3D Co3 Co4 C30 -76.0(7) . . . . ? N3F Co3 Co4 C30 56.1(7) . . . . ? N5 Co3 Co4 C30 175.4(8) . . . . ? O31 Co3 N5 C1F 52(2) . . . . ? N3E Co3 N5 C1F -113.2(7) . . . . ? N3D Co3 N5 C1F 123.2(7) . . . . ? N3F Co3 N5 C1F 6.5(7) . . . . ? Co4 Co3 N5 C1F -120.3(7) . . . . ? O31 Co3 N5 C1D -70(2) . . . . ? N3E Co3 N5 C1D 125.1(7) . . . . ? N3D Co3 N5 C1D 1.5(7) . . . . ? N3F Co3 N5 C1D -115.3(7) . . . . ? Co4 Co3 N5 C1D 118.0(6) . . . . ? O31 Co3 N5 C1E 169.7(16) . . . . ? N3E Co3 N5 C1E 4.4(6) . . . . ? N3D Co3 N5 C1E -119.2(7) . . . . ? N3F Co3 N5 C1E 124.1(7) . . . . ? Co4 Co3 N5 C1E -2.7(9) . . . . ? C1F N5 C1D C2D -148.2(9) . . . . ? C1E N5 C1D C2D 85.8(10) . . . . ? Co3 N5 C1D C2D -30.1(10) . . . . ? N5 C1D C2D N3D 55.6(11) . . . . ? C1D C2D N3D C3D 167.9(8) . . . . ? C1D C2D N3D Co3 -52.9(9) . . . . ? O31 Co3 N3D C2D -161.4(7) . . . . ? N3E Co3 N3D C2D -43.3(8) . . . . ? N3F Co3 N3D C2D 100.9(7) . . . . ? N5 Co3 N3D C2D 27.4(7) . . . . ? Co4 Co3 N3D C2D -126.2(6) . . . . ? O31 Co3 N3D C3D -24.3(8) . . . . ? N3E Co3 N3D C3D 93.8(8) . . . . ? N3F Co3 N3D C3D -122.0(8) . . . . ? N5 Co3 N3D C3D 164.4(8) . . . . ? Co4 Co3 N3D C3D 10.8(8) . . . . ? C2D N3D C3D C4D 73.7(11) . . . . ? Co3 N3D C3D C4D -60.5(11) . . . . ? N3D C3D C4D C9D 110.9(10) . . . . ? N3D C3D C4D C5D -71.8(12) . . . . ? C9D C4D C5D C6D -0.8(15) . . . . ? C3D C4D C5D C6D -178.2(10) . . . . ? C4D C5D C6D C7D -0.6(17) . . . . ? C5D C6D C7D C8D 2.4(16) . . . . ? C6D C7D C8D C9D -2.9(14) . . . . ? C6D C7D C8D C10D 173.3(9) . . . . ? C7D C8D C9D C4D 1.6(14) . . . . ? C10D C8D C9D C4D -174.3(9) . . . . ? C5D C4D C9D C8D 0.3(13) . . . . ? C3D C4D C9D C8D 177.8(8) . . . . ? C9D C8D C10D N4D -36.4(15) . . . . ? C7D C8D C10D N4D 147.5(10) . . . . ? C8D C10D N4D C11D 164.7(9) . . . . ? C8D C10D N4D Co4 -62.0(13) . . . . ? O33 Co4 N4D C10D 57.2(8) . . . . ? N6 Co4 N4D C10D -139.3(8) . . . . ? O32 Co4 N4D C10D 116.8(8) . . . . ? N4E Co4 N4D C10D -60.3(8) . . . . ? N4F Co4 N4D C10D -179.3(10) . . . . ? C30 Co4 N4D C10D 86.9(8) . . . . ? Co3 Co4 N4D C10D 68.6(8) . . . . ? O33 Co4 N4D C11D -169.8(6) . . . . ? N6 Co4 N4D C11D -6.4(7) . . . . ? O32 Co4 N4D C11D -110.2(7) . . . . ? N4E Co4 N4D C11D 72.6(7) . . . . ? N4F Co4 N4D C11D -46.4(12) . . . . ? C30 Co4 N4D C11D -140.1(7) . . . . ? Co3 Co4 N4D C11D -158.4(6) . . . . ? C10D N4D C11D C12D 175.9(9) . . . . ? Co4 N4D C11D C12D 33.8(10) . . . . ? N4D C11D C12D N6 -57.8(11) . . . . ? C11D C12D N6 C12F 166.9(8) . . . . ? C11D C12D N6 C12E -70.1(10) . . . . ? C11D C12D N6 Co4 51.5(9) . . . . ? O33 Co4 N6 C12F -52.4(13) . . . . ? O32 Co4 N6 C12F -63.0(6) . . . . ? N4E Co4 N6 C12F 117.4(6) . . . . ? N4D Co4 N6 C12F -140.1(6) . . . . ? N4F Co4 N6 C12F 23.5(6) . . . . ? C30 Co4 N6 C12F -61.7(7) . . . . ? Co3 Co4 N6 C12F -58.1(8) . . . . ? O33 Co4 N6 C12E -172.6(9) . . . . ? O32 Co4 N6 C12E 176.9(7) . . . . ? N4E Co4 N6 C12E -2.7(7) . . . . ? N4D Co4 N6 C12E 99.8(7) . . . . ? N4F Co4 N6 C12E -96.6(8) . . . . ? C30 Co4 N6 C12E 178.2(7) . . . . ? Co3 Co4 N6 C12E -178.3(6) . . . . ? O33 Co4 N6 C12D 64.1(13) . . . . ? O32 Co4 N6 C12D 53.5(7) . . . . ? N4E Co4 N6 C12D -126.1(7) . . . . ? N4D Co4 N6 C12D -23.6(6) . . . . ? N4F Co4 N6 C12D 140.0(7) . . . . ? C30 Co4 N6 C12D 54.8(8) . . . . ? Co3 Co4 N6 C12D 58.4(9) . . . . ? C1F N5 C1E C2E 83.1(11) . . . . ? C1D N5 C1E C2E -149.5(8) . . . . ? Co3 N5 C1E C2E -32.4(9) . . . . ? N5 C1E C2E N3E 54.2(11) . . . . ? C1E C2E N3E C3E 82.1(9) . . . . ? C1E C2E N3E Co3 -47.8(9) . . . . ? O31 Co3 N3E C2E -154.1(5) . . . . ? N3D Co3 N3E C2E 93.5(6) . . . . ? N3F Co3 N3E C2E -49.7(7) . . . . ? N5 Co3 N3E C2E 23.4(6) . . . . ? Co4 Co3 N3E C2E -160.0(6) . . . . ? O31 Co3 N3E C3E 77.2(6) . . . . ? N3D Co3 N3E C3E -35.2(7) . . . . ? N3F Co3 N3E C3E -178.3(5) . . . . ? N5 Co3 N3E C3E -105.2(6) . . . . ? Co4 Co3 N3E C3E 71.4(5) . . . . ? C2E N3E C3E C4E 95.4(8) . . . . ? Co3 N3E C3E C4E -137.1(6) . . . . ? N3E C3E C4E C5E -63.4(11) . . . . ? N3E C3E C4E C9E 111.1(9) . . . . ? C9E C4E C5E C6E 1.5(15) . . . . ? C3E C4E C5E C6E 175.9(9) . . . . ? C4E C5E C6E C7E -4.0(18) . . . . ? C5E C6E C7E C8E 4.0(18) . . . . ? C6E C7E C8E C9E -1.5(15) . . . . ? C6E C7E C8E C10E -177.1(10) . . . . ? C5E C4E C9E C8E 0.9(13) . . . . ? C3E C4E C9E C8E -173.7(8) . . . . ? C7E C8E C9E C4E -1.0(13) . . . . ? C10E C8E C9E C4E 175.0(8) . . . . ? C7E C8E C10E N4E 99.7(11) . . . . ? C9E C8E C10E N4E -76.0(10) . . . . ? C8E C10E N4E C11E 179.7(8) . . . . ? C8E C10E N4E Co4 55.3(10) . . . . ? O33 Co4 N4E C11E -157.4(6) . . . . ? N6 Co4 N4E C11E 25.7(6) . . . . ? O32 Co4 N4E C11E -147(6) . . . . ? N4D Co4 N4E C11E -52.5(6) . . . . ? N4F Co4 N4E C11E 105.4(6) . . . . ? C30 Co4 N4E C11E -155.5(6) . . . . ? Co3 Co4 N4E C11E -156.9(5) . . . . ? O33 Co4 N4E C10E -31.9(8) . . . . ? N6 Co4 N4E C10E 151.3(8) . . . . ? O32 Co4 N4E C10E -22(6) . . . . ? N4D Co4 N4E C10E 73.1(8) . . . . ? N4F Co4 N4E C10E -129.1(8) . . . . ? C30 Co4 N4E C10E -30.0(10) . . . . ? Co3 Co4 N4E C10E -31.4(8) . . . . ? C10E N4E C11E C12E -179.9(8) . . . . ? Co4 N4E C11E C12E -44.0(10) . . . . ? C12F N6 C12E C11E -139.0(10) . . . . ? C12D N6 C12E C11E 98.8(11) . . . . ? Co4 N6 C12E C11E -20.6(12) . . . . ? N4E C11E C12E N6 45.5(13) . . . . ? C1D N5 C1F C2F 84.5(11) . . . . ? C1E N5 C1F C2F -148.2(9) . . . . ? Co3 N5 C1F C2F -33.7(11) . . . . ? N5 C1F C2F N3F 56.4(13) . . . . ? C1F C2F N3F C3F 80.6(13) . . . . ? C1F C2F N3F Co3 -47.9(11) . . . . ? O31 Co3 N3F C2F -151.4(7) . . . . ? N3E Co3 N3F C2F 94.9(8) . . . . ? N3D Co3 N3F C2F -50.5(8) . . . . ? N5 Co3 N3F C2F 22.1(7) . . . . ? Co4 Co3 N3F C2F 178.1(6) . . . . ? O31 Co3 N3F C3F 88.3(11) . . . . ? N3E Co3 N3F C3F -25.4(12) . . . . ? N3D Co3 N3F C3F -170.8(11) . . . . ? N5 Co3 N3F C3F -98.3(11) . . . . ? Co4 Co3 N3F C3F 57.7(11) . . . . ? C2F N3F C3F C4F -150.6(15) . . . . ? Co3 N3F C3F C4F -30(2) . . . . ? N3F C3F C4F C9F -54(2) . . . . ? N3F C3F C4F C5F 123.8(14) . . . . ? N3F C3F C4F C3F' -56(3) . . . . ? C3F C4F C5F C6F -177.7(15) . . . . ? C9F C4F C5F C6F 0.8(16) . . . . ? C3F' C4F C5F C6F -177(3) . . . . ? C4F C5F C6F C7F -4(2) . . . . ? C5F C6F C7F C8F 3(3) . . . . ? C6F C7F C8F C9F 2(2) . . . . ? C6F C7F C8F C10F -171.8(14) . . . . ? C7F C8F C9F C4F -6.0(19) . . . . ? C10F C8F C9F C4F 168.8(10) . . . . ? C3F C4F C9F C8F -178.0(16) . . . . ? C5F C4F C9F C8F 3.8(15) . . . . ? C3F' C4F C9F C8F -177.1(14) . . . . ? C7F C8F C10F N4F -57.5(18) . . . . ? C9F C8F C10F N4F 127.6(13) . . . . ? C8F C10F N4F C11F 156.4(10) . . . . ? C8F C10F N4F Co4 -77.3(15) . . . . ? O33 Co4 N4F C10F 42.6(11) . . . . ? N6 Co4 N4F C10F -121.4(11) . . . . ? O32 Co4 N4F C10F -19.3(11) . . . . ? N4E Co4 N4F C10F 157.9(11) . . . . ? N4D Co4 N4F C10F -81.4(14) . . . . ? C30 Co4 N4F C10F 11.2(11) . . . . ? Co3 Co4 N4F C10F 30.7(11) . . . . ? O33 Co4 N4F C11F 169.6(8) . . . . ? N6 Co4 N4F C11F 5.6(8) . . . . ? O32 Co4 N4F C11F 107.6(8) . . . . ? N4E Co4 N4F C11F -75.1(8) . . . . ? N4D Co4 N4F C11F 45.6(14) . . . . ? C30 Co4 N4F C11F 138.2(8) . . . . ? Co3 Co4 N4F C11F 157.7(8) . . . . ? C10F N4F C11F C12F 102.3(13) . . . . ? Co4 N4F C11F C12F -33.3(12) . . . . ? C12E N6 C12F C11F 71.6(11) . . . . ? C12D N6 C12F C11F -163.6(9) . . . . ? Co4 N6 C12F C11F -48.7(10) . . . . ? N4F C11F C12F N6 56.8(13) . . . . ? O33 Co4 C30 O32 -177.5(8) . . . . ? N6 Co4 C30 O32 -2.5(7) . . . . ? N4E Co4 C30 O32 179.2(5) . . . . ? N4D Co4 C30 O32 72.5(5) . . . . ? N4F Co4 C30 O32 -82.0(5) . . . . ? Co3 Co4 C30 O32 -177.5(10) . . . . ? O33 Co4 C30 O31 29(8) . . . . ? N6 Co4 C30 O31 -156(8) . . . . ? O32 Co4 C30 O31 -154(9) . . . . ? N4E Co4 C30 O31 25(9) . . . . ? N4D Co4 C30 O31 -81(8) . . . . ? N4F Co4 C30 O31 124(8) . . . . ? Co3 Co4 C30 O31 29(8) . . . . ? N6 Co4 C30 O33 175.0(5) . . . . ? O32 Co4 C30 O33 177.5(8) . . . . ? N4E Co4 C30 O33 -3.3(8) . . . . ? N4D Co4 C30 O33 -110.0(5) . . . . ? N4F Co4 C30 O33 95.5(5) . . . . ? Co3 Co4 C30 O33 0.0(4) . . . . ? O32 C30 O31 Co3 175.1(6) . . . . ? O33 C30 O31 Co3 -5.2(12) . . . . ? Co4 C30 O31 Co3 -32(9) . . . . ? N3E Co3 O31 C30 -7.3(8) . . . . ? N3D Co3 O31 C30 118.4(8) . . . . ? N3F Co3 O31 C30 -127.1(8) . . . . ? N5 Co3 O31 C30 -172.0(16) . . . . ? Co4 Co3 O31 C30 2.1(6) . . . . ? O31 C30 O32 Co4 177.5(8) . . . . ? O33 C30 O32 Co4 -2.3(8) . . . . ? O33 Co4 O32 C30 1.5(5) . . . . ? N6 Co4 O32 C30 178.1(5) . . . . ? N4E Co4 O32 C30 -9(6) . . . . ? N4D Co4 O32 C30 -104.3(5) . . . . ? N4F Co4 O32 C30 98.5(6) . . . . ? Co3 Co4 O32 C30 1.1(4) . . . . ? O32 C30 O33 Co4 2.5(8) . . . . ? O31 C30 O33 Co4 -177.3(7) . . . . ? N6 Co4 O33 C30 -13.1(13) . . . . ? O32 Co4 O33 C30 -1.4(5) . . . . ? N4E Co4 O33 C30 178.0(5) . . . . ? N4D Co4 O33 C30 71.9(5) . . . . ? N4F Co4 O33 C30 -86.9(6) . . . . ? Co3 Co4 O33 C30 0.0(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3A H3A O52 0.93 2.25 3.039(13) 142.6 3 N4A H4A O63 0.93 2.38 3.136(12) 138.0 . N3B H3B O1W 0.93 2.39 3.05(4) 127.9 . N3B H3B O1W' 0.93 2.29 2.78(2) 112.5 . N3C H3C O1W 0.93 2.02 2.86(5) 149.2 . N4B H4B O2W 0.93 2.30 2.859(12) 117.7 . N3D H3D O82 0.93 2.23 3.14(4) 165.0 . N3D H3D O82' 0.93 2.09 2.985(17) 161.8 . N3F H3F O4W 0.93 1.97 2.87(2) 162.9 . N3F' H3F' O4W 0.93 2.15 2.87(2) 134.3 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.033 _refine_diff_density_min -0.590 _refine_diff_density_rms 0.118 data_Complex_8 #(y198r) _database_code_CSD 181032 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H50 Cl2 Co2 N8 O15' _chemical_formula_weight 963.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.870(6) _cell_length_b 12.320(6) _cell_length_c 16.954(9) _cell_angle_alpha 71.358(7) _cell_angle_beta 74.496(7) _cell_angle_gamma 88.330(8) _cell_volume 2259.4(19) _cell_formula_units_Z 2 _cell_measurement_temperature 169(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block? _exptl_crystal_colour orange _exptl_crystal_size_max .7 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 0.921 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.440075 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 169(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14824 _diffrn_reflns_av_R_equivalents 0.0885 _diffrn_reflns_av_sigmaI/netI 0.1954 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 24.00 _reflns_number_total 7018 _reflns_number_gt 3317 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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. One perchlorate anion shows disorder (55:46) over two positions related by rotation about one of the Cl-O bonds. The hydrogen atoms bonded to water were not located and have not been included in the refinement. ; _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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7018 _refine_ls_number_parameters 551 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.2035 _refine_ls_R_factor_gt 0.1156 _refine_ls_wR_factor_ref 0.3724 _refine_ls_wR_factor_gt 0.3298 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.125 _refine_ls_shift/su_max 0.487 _refine_ls_shift/su_mean 0.021 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 Co1 Co 1.00275(16) 0.06662(14) 0.26883(12) 0.0300(6) Uani 1 1 d . . . Co2 Co 0.81078(16) 0.32031(14) 0.36426(12) 0.0285(6) Uani 1 1 d . . . N1 N 1.1076(10) -0.0771(9) 0.2531(7) 0.035(3) Uani 1 1 d . . . C1A C 1.0441(15) -0.1875(11) 0.3097(11) 0.052(5) Uani 1 1 d . . . H1A1 H 1.1006 -0.2451 0.3265 0.063 Uiso 1 1 calc R . . H1A2 H 0.9987 -0.2160 0.2784 0.063 Uiso 1 1 calc R . . C2A C 0.9604(13) -0.1705(11) 0.3915(11) 0.045(4) Uani 1 1 d . . . H2A1 H 0.9147 -0.2433 0.4286 0.054 Uiso 1 1 calc R . . H2A2 H 1.0061 -0.1474 0.4252 0.054 Uiso 1 1 calc R . . N3A N 0.8786(10) -0.0782(8) 0.3640(7) 0.031(3) Uani 1 1 d . . . H3A H 0.8488 -0.0546 0.4120 0.037 Uiso 1 1 calc R . . C3A C 0.7732(12) -0.1238(11) 0.3484(10) 0.036(4) Uani 1 1 d . . . H3A1 H 0.7973 -0.1428 0.2940 0.044 Uiso 1 1 calc R . . H3A2 H 0.7400 -0.1951 0.3963 0.044 Uiso 1 1 calc R . . C4A C 0.6841(14) -0.0399(11) 0.3424(10) 0.039(4) Uani 1 1 d . . . C5A C 0.6061(14) -0.0036(13) 0.2975(11) 0.050(5) Uani 1 1 d . . . H5A H 0.5951 -0.0286 0.2524 0.060 Uiso 1 1 calc R . . C6A C 0.5410(13) 0.0816(13) 0.3308(11) 0.045(4) Uani 1 1 d . . . H6A H 0.4775 0.1208 0.3127 0.054 Uiso 1 1 calc R . . C7A C 0.5862(14) 0.0948(12) 0.3910(10) 0.040(4) Uani 1 1 d . . . O1A O 0.6737(8) 0.0182(8) 0.4026(6) 0.039(3) Uani 1 1 d . . . C8A C 0.5668(12) 0.1634(11) 0.4515(10) 0.034(4) Uani 1 1 d . . . H8A1 H 0.5287 0.2342 0.4276 0.041 Uiso 1 1 calc R . . H8A2 H 0.5133 0.1183 0.5078 0.041 Uiso 1 1 calc R . . N4A N 0.6768(9) 0.1945(8) 0.4655(7) 0.031(3) Uani 1 1 d . . . H4A H 0.7141 0.1265 0.4802 0.037 Uiso 1 1 calc R . . C9A C 0.6555(14) 0.2356(11) 0.5413(10) 0.042(4) Uani 1 1 d . . . H9A1 H 0.7250 0.2239 0.5642 0.051 Uiso 1 1 calc R . . H9A2 H 0.5877 0.1906 0.5876 0.051 Uiso 1 1 calc R . . C10A C 0.6312(13) 0.3618(12) 0.5160(10) 0.043(4) Uani 1 1 d . . . H10A H 0.5576 0.3733 0.4982 0.052 Uiso 1 1 calc R . . H10B H 0.6226 0.3898 0.5657 0.052 Uiso 1 1 calc R . . N2 N 0.7310(9) 0.4261(8) 0.4429(8) 0.032(3) Uani 1 1 d . . . C1B C 1.1372(14) -0.0700(12) 0.1571(10) 0.046(4) Uani 1 1 d . . . H1B1 H 1.2053 -0.0151 0.1225 0.055 Uiso 1 1 calc R . . H1B2 H 1.1564 -0.1462 0.1511 0.055 Uiso 1 1 calc R . . C2B C 1.0279(14) -0.0292(13) 0.1262(11) 0.047(4) Uani 1 1 d . . . H2B1 H 1.0473 -0.0148 0.0631 0.057 Uiso 1 1 calc R . . H2B2 H 0.9655 -0.0918 0.1544 0.057 Uiso 1 1 calc R . . N3B N 0.9815(11) 0.0754(9) 0.1441(8) 0.036(3) Uani 1 1 d . . . H3B H 1.0334 0.1352 0.1042 0.044 Uiso 1 1 calc R . . C3B C 0.8703(14) 0.0950(12) 0.1196(10) 0.046(4) Uani 1 1 d . . . H3B1 H 0.8101 0.0366 0.1631 0.055 Uiso 1 1 calc R . . H3B2 H 0.8815 0.0819 0.0634 0.055 Uiso 1 1 calc R . . C4B C 0.8235(13) 0.2111(12) 0.1118(11) 0.041(4) Uani 1 1 d . . . C5B C 0.8190(14) 0.3026(14) 0.0422(11) 0.050(4) Uani 1 1 d . . . H5B H 0.8522 0.3092 -0.0168 0.060 Uiso 1 1 calc R . . C6B C 0.7571(14) 0.3847(13) 0.0731(12) 0.051(5) Uani 1 1 d . . . H6B H 0.7396 0.4576 0.0394 0.061 Uiso 1 1 calc R . . C7B C 0.7264(13) 0.3410(12) 0.1604(10) 0.038(4) Uani 1 1 d . . . O1B O 0.7669(8) 0.2337(8) 0.1884(6) 0.036(2) Uani 1 1 d . . . C8B C 0.6503(13) 0.3867(14) 0.2295(10) 0.046(4) Uani 1 1 d . . . H8B1 H 0.6072 0.4510 0.2014 0.055 Uiso 1 1 calc R . . H8B2 H 0.5916 0.3252 0.2708 0.055 Uiso 1 1 calc R . . N4B N 0.7173(10) 0.4274(10) 0.2784(8) 0.040(3) Uani 1 1 d . . . H4B H 0.7732 0.4819 0.2366 0.048 Uiso 1 1 calc R . . C9B C 0.6894(13) 0.5289(11) 0.3873(10) 0.042(4) Uani 1 1 d . . . H9B1 H 0.7562 0.5853 0.3525 0.050 Uiso 1 1 calc R . . H9B2 H 0.6319 0.5651 0.4237 0.050 Uiso 1 1 calc R . . C10B C 0.6327(14) 0.4949(13) 0.3275(11) 0.050(4) Uani 1 1 d . . . H10C H 0.6128 0.5645 0.2859 0.060 Uiso 1 1 calc R . . H10D H 0.5595 0.4471 0.3617 0.060 Uiso 1 1 calc R . . C1C C 1.2164(14) -0.0648(12) 0.2792(11) 0.052(5) Uani 1 1 d . . . H1C1 H 1.2709 -0.1232 0.2666 0.062 Uiso 1 1 calc R . . H1C2 H 1.1960 -0.0775 0.3422 0.062 Uiso 1 1 calc R . . C2C C 1.2774(14) 0.0584(12) 0.2285(10) 0.048(4) Uani 1 1 d . . . H2C1 H 1.3321 0.0754 0.2587 0.057 Uiso 1 1 calc R . . H2C2 H 1.3232 0.0615 0.1696 0.057 Uiso 1 1 calc R . . N3C N 1.1880(9) 0.1455(9) 0.2226(8) 0.036(3) Uani 1 1 d . . . H3C H 1.1917 0.1761 0.2655 0.043 Uiso 1 1 calc R . . C3C C 1.2319(13) 0.2447(12) 0.1411(9) 0.042(4) Uani 1 1 d . . . H3C1 H 1.3081 0.2766 0.1400 0.051 Uiso 1 1 calc R . . H3C2 H 1.2439 0.2181 0.0904 0.051 Uiso 1 1 calc R . . C4C C 1.1492(13) 0.3324(12) 0.1364(10) 0.038(4) Uani 1 1 d . . . C5C C 1.0749(15) 0.3779(13) 0.0867(10) 0.046(4) Uani 1 1 d . . . H5C H 1.0667 0.3573 0.0390 0.055 Uiso 1 1 calc R . . C6C C 1.0126(15) 0.4611(13) 0.1189(11) 0.052(5) Uani 1 1 d . . . H6C H 0.9545 0.5057 0.0968 0.062 Uiso 1 1 calc R . . C7C C 1.0494(13) 0.4664(12) 0.1859(10) 0.040(4) Uani 1 1 d . . . O1C O 1.1338(8) 0.3860(8) 0.2002(6) 0.039(3) Uani 1 1 d . . . C8C C 1.0195(14) 0.5272(12) 0.2498(10) 0.046(4) Uani 1 1 d . . . H8C1 H 0.9672 0.5889 0.2321 0.055 Uiso 1 1 calc R . . H8C2 H 1.0918 0.5632 0.2517 0.055 Uiso 1 1 calc R . . N4C N 0.9596(9) 0.4468(9) 0.3384(7) 0.032(3) Uani 1 1 d . . . H4C H 1.0186 0.4004 0.3538 0.039 Uiso 1 1 calc R . . C9C C 0.9344(13) 0.5117(12) 0.4004(10) 0.048(5) Uani 1 1 d . . . H9C1 H 0.9191 0.5917 0.3707 0.058 Uiso 1 1 calc R . . H9C2 H 1.0033 0.5136 0.4225 0.058 Uiso 1 1 calc R . . C10C C 0.8261(13) 0.4547(12) 0.4773(10) 0.045(4) Uani 1 1 d . . . H10E H 0.8481 0.3839 0.5166 0.054 Uiso 1 1 calc R . . H10F H 0.7980 0.5079 0.5105 0.054 Uiso 1 1 calc R . . O1 O 0.9133(8) 0.1985(7) 0.3144(6) 0.031(2) Uani 1 1 d . . . O2 O 1.0233(7) 0.0843(7) 0.3862(6) 0.028(2) Uani 1 1 d . . . O3 O 0.9206(7) 0.2162(7) 0.4379(6) 0.028(2) Uani 1 1 d . . . C1 C 0.9540(12) 0.1641(11) 0.3849(10) 0.032(4) Uani 1 1 d . . . Cl1 Cl 1.2965(3) 0.3558(3) 0.3653(3) 0.0452(11) Uani 1 1 d . . . O11 O 1.1762(9) 0.3664(13) 0.3918(9) 0.087(5) Uani 1 1 d . . . O12 O 1.3189(14) 0.2646(12) 0.3281(11) 0.104(5) Uani 1 1 d . . . O13 O 1.3484(12) 0.3384(12) 0.4360(9) 0.086(4) Uani 1 1 d . . . O14 O 1.3535(18) 0.4557(13) 0.3024(12) 0.148(8) Uani 1 1 d . . . Cl2 Cl 0.7946(4) -0.2424(3) 0.1108(3) 0.0512(19) Uani 0.553(15) 1 d PD A 1 O21 O 0.7413(14) -0.3420(9) 0.1106(8) 0.104(6) Uani 0.553(15) 1 d PD A 1 O22 O 0.781(3) -0.240(2) 0.1928(10) 0.070(7) Uani 0.553(15) 1 d PDU A 1 O23 O 0.9144(19) -0.232(3) 0.063(2) 0.111(14) Uani 0.553(15) 1 d PD A 1 O24 O 0.750(3) -0.1512(19) 0.058(2) 0.106(12) Uani 0.553(15) 1 d PD A 1 Cl2' Cl 0.7946(4) -0.2424(3) 0.1108(3) 0.0512(19) Uani 0.45 1 d PD A 2 O21' O 0.7413(14) -0.3420(9) 0.1106(8) 0.104(6) Uani 0.45 1 d PD A 2 O22' O 0.852(4) -0.281(3) 0.175(2) 0.105(14) Uani 0.447(15) 1 d PDU A 2 O23' O 0.848(5) -0.167(2) 0.0317(14) 0.108(19) Uani 0.447(15) 1 d PD A 2 O24' O 0.701(3) -0.180(4) 0.145(4) 0.16(2) Uani 0.447(15) 1 d PD A 2 O1W O 1.2068(8) 0.0333(8) 0.4602(6) 0.040(3) Uani 1 1 d . B 2 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 Co1 0.0435(12) 0.0213(10) 0.0313(13) -0.0132(9) -0.0136(9) -0.0046(8) Co2 0.0342(12) 0.0202(9) 0.0335(13) -0.0108(8) -0.0102(9) -0.0040(8) N1 0.045(7) 0.032(6) 0.034(8) -0.026(6) -0.001(6) -0.005(5) C1A 0.071(12) 0.026(8) 0.073(13) -0.030(8) -0.024(10) 0.008(8) C2A 0.055(10) 0.025(8) 0.064(12) -0.021(8) -0.022(9) -0.001(7) N3A 0.045(7) 0.017(5) 0.036(7) -0.015(5) -0.009(6) -0.009(5) C3A 0.044(9) 0.031(8) 0.039(10) -0.018(7) -0.010(7) -0.008(7) C4A 0.044(10) 0.029(8) 0.035(10) -0.005(7) 0.001(8) -0.022(7) C5A 0.043(10) 0.054(10) 0.058(12) -0.018(9) -0.022(9) -0.018(8) C6A 0.039(9) 0.040(9) 0.058(12) 0.000(8) -0.032(9) -0.010(7) C7A 0.053(10) 0.028(8) 0.036(10) -0.004(7) -0.013(8) -0.014(7) O1A 0.044(6) 0.031(5) 0.053(7) -0.021(5) -0.020(5) -0.006(5) C8A 0.033(8) 0.026(7) 0.041(10) -0.009(7) -0.010(7) 0.002(6) N4A 0.027(6) 0.022(6) 0.043(8) -0.014(5) -0.006(6) -0.006(5) C9A 0.052(10) 0.028(8) 0.048(10) -0.011(7) -0.014(8) -0.014(7) C10A 0.045(10) 0.045(9) 0.032(10) -0.008(7) -0.003(8) -0.007(7) N2 0.031(7) 0.019(6) 0.046(8) -0.017(6) -0.005(6) 0.003(5) C1B 0.060(11) 0.032(8) 0.049(11) -0.031(8) 0.002(9) -0.007(7) C2B 0.055(11) 0.049(9) 0.048(11) -0.013(8) -0.030(9) -0.009(8) N3B 0.049(8) 0.028(6) 0.036(8) -0.011(6) -0.018(6) -0.003(5) C3B 0.063(11) 0.039(9) 0.037(10) -0.018(8) -0.005(8) -0.025(8) C4B 0.043(9) 0.034(8) 0.044(11) -0.015(8) 0.000(8) -0.019(7) C5B 0.062(11) 0.058(11) 0.032(11) -0.020(9) -0.007(8) -0.001(9) C6B 0.064(11) 0.031(8) 0.064(13) -0.006(9) -0.039(10) 0.000(8) C7B 0.038(9) 0.041(9) 0.031(10) -0.002(8) -0.015(8) -0.007(7) O1B 0.045(6) 0.034(5) 0.032(6) -0.015(5) -0.009(5) -0.004(5) C8B 0.033(9) 0.060(10) 0.037(10) 0.002(8) -0.017(8) -0.009(7) N4B 0.030(7) 0.042(7) 0.052(9) -0.021(6) -0.012(6) -0.003(5) C9B 0.050(10) 0.022(7) 0.047(10) -0.011(7) 0.000(8) -0.014(7) C10B 0.048(10) 0.039(9) 0.066(12) -0.014(9) -0.024(9) 0.003(7) C1C 0.063(12) 0.043(9) 0.053(12) -0.017(8) -0.020(9) -0.002(8) C2C 0.057(11) 0.047(9) 0.046(11) -0.023(8) -0.014(9) -0.002(8) N3C 0.036(7) 0.032(6) 0.048(8) -0.023(6) -0.014(6) 0.000(5) C3C 0.050(10) 0.037(8) 0.032(10) -0.013(7) 0.004(8) -0.015(7) C4C 0.038(9) 0.029(8) 0.048(11) -0.016(8) -0.005(8) -0.016(7) C5C 0.071(12) 0.041(9) 0.020(9) -0.011(7) 0.001(9) -0.015(8) C6C 0.064(12) 0.042(9) 0.039(11) -0.002(8) -0.009(9) -0.014(8) C7C 0.035(9) 0.043(9) 0.035(10) -0.008(8) -0.001(8) -0.021(7) O1C 0.043(6) 0.037(6) 0.048(7) -0.022(5) -0.017(5) -0.003(5) C8C 0.062(11) 0.029(8) 0.043(11) -0.013(8) -0.002(9) -0.009(7) N4C 0.031(7) 0.029(6) 0.045(8) -0.022(6) -0.012(6) 0.002(5) C9C 0.050(10) 0.038(9) 0.066(12) -0.035(8) -0.007(9) -0.012(7) C10C 0.051(10) 0.044(9) 0.052(11) -0.040(8) -0.001(8) -0.015(7) O1 0.036(5) 0.024(5) 0.029(6) -0.007(4) -0.004(5) -0.007(4) O2 0.032(5) 0.028(5) 0.032(6) -0.015(4) -0.014(4) 0.003(4) O3 0.039(6) 0.028(5) 0.026(6) -0.023(4) -0.003(4) 0.002(4) C1 0.035(9) 0.026(7) 0.043(11) -0.011(7) -0.022(8) -0.004(7) Cl1 0.046(3) 0.043(2) 0.050(3) -0.015(2) -0.016(2) -0.0040(18) O11 0.026(7) 0.166(14) 0.104(11) -0.087(10) -0.024(7) 0.017(7) O12 0.132(13) 0.083(10) 0.131(14) -0.082(10) -0.034(11) 0.032(9) O13 0.100(11) 0.097(10) 0.071(10) -0.028(8) -0.044(9) 0.035(8) O14 0.191(18) 0.076(11) 0.135(16) 0.024(11) -0.037(14) -0.060(12) Cl2 0.080(4) 0.030(2) 0.049(3) -0.014(2) -0.023(3) -0.009(2) O21 0.184(15) 0.052(8) 0.067(9) -0.020(7) -0.013(9) -0.076(9) O22 0.095(14) 0.088(12) 0.038(11) -0.046(10) 0.002(9) -0.039(10) O23 0.14(3) 0.07(2) 0.11(3) -0.078(19) 0.06(2) -0.053(19) O24 0.15(3) 0.051(17) 0.12(3) -0.02(2) -0.06(3) 0.05(2) Cl2' 0.080(4) 0.030(2) 0.049(3) -0.014(2) -0.023(3) -0.009(2) O21' 0.184(15) 0.052(8) 0.067(9) -0.020(7) -0.013(9) -0.076(9) O22' 0.101(18) 0.101(18) 0.105(19) -0.009(13) -0.047(14) 0.006(13) O23' 0.22(6) 0.016(17) 0.06(2) -0.003(16) 0.01(3) 0.00(2) O24' 0.09(3) 0.20(5) 0.24(6) -0.15(5) -0.05(4) 0.07(3) O1W 0.046(6) 0.033(5) 0.051(7) -0.017(5) -0.024(5) 0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O2 2.146(9) . ? Co1 O1 2.151(9) . ? Co1 N3B 2.165(12) . ? Co1 N1 2.180(11) . ? Co1 N3A 2.236(10) . ? Co1 N3C 2.261(11) . ? Co1 Co2 4.292(3) . ? Co2 O1 2.145(9) . ? Co2 N4B 2.154(12) . ? Co2 O3 2.157(9) . ? Co2 N2 2.177(10) . ? Co2 N4A 2.205(10) . ? Co2 N4C 2.247(10) . ? N1 C1A 1.476(17) . ? N1 C1C 1.499(18) . ? N1 C1B 1.543(18) . ? C1A C2A 1.55(2) . ? C2A N3A 1.514(17) . ? N3A C3A 1.504(16) . ? C3A C4A 1.46(2) . ? C4A C5A 1.33(2) . ? C4A O1A 1.401(17) . ? C5A C6A 1.46(2) . ? C6A C7A 1.33(2) . ? C7A O1A 1.393(17) . ? C7A C8A 1.50(2) . ? C8A N4A 1.470(16) . ? N4A C9A 1.485(18) . ? C9A C10A 1.516(19) . ? C10A N2 1.486(16) . ? N2 C9B 1.479(18) . ? N2 C10C 1.497(17) . ? C1B C2B 1.54(2) . ? C2B N3B 1.474(18) . ? N3B C3B 1.478(18) . ? C3B C4B 1.50(2) . ? C4B C5B 1.36(2) . ? C4B O1B 1.403(17) . ? C5B C6B 1.39(2) . ? C6B C7B 1.35(2) . ? C7B O1B 1.373(16) . ? C7B C8B 1.53(2) . ? C8B N4B 1.489(17) . ? N4B C10B 1.529(19) . ? C9B C10B 1.52(2) . ? C1C C2C 1.569(19) . ? C2C N3C 1.486(17) . ? N3C C3C 1.499(17) . ? C3C C4C 1.44(2) . ? C4C C5C 1.37(2) . ? C4C O1C 1.409(17) . ? C5C C6C 1.41(2) . ? C6C C7C 1.34(2) . ? C7C O1C 1.400(18) . ? C7C C8C 1.47(2) . ? C8C N4C 1.503(17) . ? N4C C9C 1.479(17) . ? C9C C10C 1.554(19) . ? O1 C1 1.346(16) . ? O2 C1 1.262(16) . ? O3 C1 1.241(16) . ? Cl1 O14 1.390(13) . ? Cl1 O11 1.393(11) . ? Cl1 O12 1.440(12) . ? Cl1 O13 1.445(14) . ? Cl2 O22 1.364(14) . ? Cl2 O24 1.389(15) . ? Cl2 O21 1.398(9) . ? Cl2 O23 1.420(17) . ? 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 Co1 O1 61.4(4) . . ? O2 Co1 N3B 171.8(4) . . ? O1 Co1 N3B 111.8(4) . . ? O2 Co1 N1 103.8(4) . . ? O1 Co1 N1 165.2(4) . . ? N3B Co1 N1 83.0(4) . . ? O2 Co1 N3A 81.2(4) . . ? O1 Co1 N3A 95.6(4) . . ? N3B Co1 N3A 104.8(4) . . ? N1 Co1 N3A 80.7(4) . . ? O2 Co1 N3C 79.4(4) . . ? O1 Co1 N3C 99.2(3) . . ? N3B Co1 N3C 97.8(4) . . ? N1 Co1 N3C 77.2(4) . . ? N3A Co1 N3C 146.0(4) . . ? O2 Co1 Co2 61.8(2) . . ? O1 Co1 Co2 2.5(2) . . ? N3B Co1 Co2 111.6(3) . . ? N1 Co1 Co2 165.4(3) . . ? N3A Co1 Co2 93.3(3) . . ? N3C Co1 Co2 101.6(3) . . ? O1 Co2 N4B 114.1(4) . . ? O1 Co2 O3 61.4(3) . . ? N4B Co2 O3 173.7(4) . . ? O1 Co2 N2 164.1(4) . . ? N4B Co2 N2 81.7(4) . . ? O3 Co2 N2 102.7(4) . . ? O1 Co2 N4A 96.5(3) . . ? N4B Co2 N4A 105.1(4) . . ? O3 Co2 N4A 80.3(4) . . ? N2 Co2 N4A 80.3(4) . . ? O1 Co2 N4C 97.1(4) . . ? N4B Co2 N4C 98.5(4) . . ? O3 Co2 N4C 78.3(4) . . ? N2 Co2 N4C 77.9(4) . . ? N4A Co2 N4C 145.0(4) . . ? O1 Co2 Co1 2.5(2) . . ? N4B Co2 Co1 113.9(3) . . ? O3 Co2 Co1 61.9(2) . . ? N2 Co2 Co1 164.4(3) . . ? N4A Co2 Co1 94.2(3) . . ? N4C Co2 Co1 99.5(3) . . ? C1A N1 C1C 108.8(12) . . ? C1A N1 C1B 110.8(10) . . ? C1C N1 C1B 111.2(11) . . ? C1A N1 Co1 110.9(9) . . ? C1C N1 Co1 106.9(8) . . ? C1B N1 Co1 108.2(9) . . ? N1 C1A C2A 109.4(10) . . ? N3A C2A C1A 108.8(13) . . ? C3A N3A C2A 112.9(9) . . ? C3A N3A Co1 125.1(9) . . ? C2A N3A Co1 102.5(8) . . ? C4A C3A N3A 111.1(10) . . ? C5A C4A O1A 109.5(14) . . ? C5A C4A C3A 138.3(15) . . ? O1A C4A C3A 112.1(14) . . ? C4A C5A C6A 106.7(14) . . ? C7A C6A C5A 107.7(14) . . ? C6A C7A O1A 109.3(14) . . ? C6A C7A C8A 138.5(16) . . ? O1A C7A C8A 112.1(13) . . ? C7A O1A C4A 106.7(12) . . ? N4A C8A C7A 112.2(11) . . ? C8A N4A C9A 111.9(10) . . ? C8A N4A Co2 122.6(9) . . ? C9A N4A Co2 104.0(7) . . ? N4A C9A C10A 110.5(12) . . ? N2 C10A C9A 108.2(11) . . ? C9B N2 C10A 109.8(11) . . ? C9B N2 C10C 112.8(10) . . ? C10A N2 C10C 109.8(11) . . ? C9B N2 Co2 108.3(9) . . ? C10A N2 Co2 111.0(8) . . ? C10C N2 Co2 105.1(8) . . ? C2B C1B N1 106.6(12) . . ? N3B C2B C1B 114.9(11) . . ? C2B N3B C3B 107.8(10) . . ? C2B N3B Co1 107.2(9) . . ? C3B N3B Co1 124.8(9) . . ? N3B C3B C4B 116.3(11) . . ? C5B C4B O1B 109.9(13) . . ? C5B C4B C3B 132.2(15) . . ? O1B C4B C3B 117.8(13) . . ? C4B C5B C6B 107.5(15) . . ? C7B C6B C5B 106.9(14) . . ? C6B C7B O1B 111.6(14) . . ? C6B C7B C8B 131.2(15) . . ? O1B C7B C8B 117.0(13) . . ? C7B O1B C4B 104.1(11) . . ? N4B C8B C7B 113.9(12) . . ? C8B N4B C10B 105.8(11) . . ? C8B N4B Co2 125.3(9) . . ? C10B N4B Co2 108.5(9) . . ? N2 C9B C10B 109.8(11) . . ? C9B C10B N4B 109.6(12) . . ? N1 C1C C2C 110.1(13) . . ? N3C C2C C1C 110.1(12) . . ? C2C N3C C3C 109.4(11) . . ? C2C N3C Co1 112.9(8) . . ? C3C N3C Co1 123.1(9) . . ? C4C C3C N3C 110.3(12) . . ? C5C C4C O1C 108.1(13) . . ? C5C C4C C3C 136.8(15) . . ? O1C C4C C3C 115.1(14) . . ? C4C C5C C6C 107.8(14) . . ? C7C C6C C5C 108.4(16) . . ? C6C C7C O1C 109.1(14) . . ? C6C C7C C8C 137.2(17) . . ? O1C C7C C8C 113.5(14) . . ? C7C O1C C4C 106.6(12) . . ? C7C C8C N4C 111.3(10) . . ? C9C N4C C8C 109.0(10) . . ? C9C N4C Co2 111.6(8) . . ? C8C N4C Co2 123.4(9) . . ? N4C C9C C10C 110.4(10) . . ? N2 C10C C9C 109.2(12) . . ? C1 O1 Co2 90.0(8) . . ? C1 O1 Co1 90.7(8) . . ? Co2 O1 Co1 175.1(4) . . ? C1 O2 Co1 93.3(8) . . ? C1 O3 Co2 92.4(9) . . ? O3 C1 O2 129.4(14) . . ? O3 C1 O1 116.2(13) . . ? O2 C1 O1 114.5(13) . . ? O14 Cl1 O11 111.6(12) . . ? O14 Cl1 O12 107.4(11) . . ? O11 Cl1 O12 109.7(9) . . ? O14 Cl1 O13 105.1(10) . . ? O11 Cl1 O13 111.0(8) . . ? O12 Cl1 O13 111.9(9) . . ? O22 Cl2 O24 115.2(18) . . ? O22 Cl2 O21 111.9(10) . . ? O24 Cl2 O21 106.1(15) . . ? O22 Cl2 O23 112.2(17) . . ? O24 Cl2 O23 101.5(17) . . ? O21 Cl2 O23 109.3(11) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.502 _refine_diff_density_min -0.907 _refine_diff_density_rms 0.213 data_Complex_10 #(yzn6) _database_code_CSD 181033 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H62.50 Cl3 N8.50 O16 Zn2' _chemical_formula_weight 1155.58 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 27.9616(15) _cell_length_b 33.7851(17) _cell_length_c 10.9883(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10380.5(9) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11619 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 28.30 _exptl_crystal_description block _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4808 _exptl_absorpt_coefficient_mu 1.151 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8024 _exptl_absorpt_correction_T_max 0.9554 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.68850 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32089 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9961 _reflns_number_gt 5912 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SHELXTL' _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. The methylcarbonate anion is disordered 75:25 over the two equivalent syn anti coordination sites bridging the zinc ions. Two of the perchlorate anions are disordered, one is disordered over two positions (60:40), sharing two of the oxygen sites while the other shows disorder over two positions related by rotation about one of the Cl-O bonds (50:50). Two molecules of methanol and one of acetonitrile have been refined at 50% site occupancy; no hydrogen atoms have been inserted for these solvates. ; _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^)+(0.1600P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9961 _refine_ls_number_parameters 733 _refine_ls_number_restraints 604 _refine_ls_R_factor_all 0.1084 _refine_ls_R_factor_gt 0.0721 _refine_ls_wR_factor_ref 0.2271 _refine_ls_wR_factor_gt 0.2073 _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_restrained_S_all 0.959 _refine_ls_shift/su_max 1.488 _refine_ls_shift/su_mean 0.014 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 0.39652(2) 0.13234(2) 0.81580(5) 0.0433(2) Uani 1 1 d U . . Zn2 Zn 0.610336(19) 0.126626(17) 0.81605(5) 0.0370(2) Uani 1 1 d U A . N1 N 0.31569(18) 0.1431(2) 0.8223(5) 0.0702(16) Uani 1 1 d U A . C1A C 0.2947(2) 0.1197(3) 0.7162(7) 0.106(3) Uani 1 1 d U . . H1A1 H 0.2645 0.1323 0.6893 0.128 Uiso 1 1 calc R A . H1A2 H 0.2873 0.0924 0.7431 0.128 Uiso 1 1 calc R . . C2A C 0.3302(2) 0.1184(3) 0.6092(7) 0.105(3) Uani 1 1 d U A . H2A1 H 0.3171 0.1022 0.5421 0.127 Uiso 1 1 calc R . . H2A2 H 0.3362 0.1455 0.5781 0.127 Uiso 1 1 calc R . . N3A N 0.37663(17) 0.10029(19) 0.6559(4) 0.0696(16) Uani 1 1 d U A . H3A H 0.3689 0.0749 0.6818 0.084 Uiso 1 1 calc R . . C3A C 0.4108(2) 0.0954(2) 0.5533(6) 0.0686(19) Uani 1 1 d U . . H3A1 H 0.4206 0.1218 0.5238 0.082 Uiso 1 1 calc R A . H3A2 H 0.3944 0.0816 0.4855 0.082 Uiso 1 1 calc R . . C4A C 0.45561(19) 0.07175(17) 0.5888(5) 0.0495(14) Uani 1 1 d U A . C5A C 0.4536(2) 0.03321(19) 0.6361(6) 0.0604(16) Uani 1 1 d U . . H5A H 0.4235 0.0211 0.6503 0.072 Uiso 1 1 calc R A . C6A C 0.4962(2) 0.01234(19) 0.6627(7) 0.0634(18) Uani 1 1 d U A . H6A H 0.4946 -0.0136 0.6955 0.076 Uiso 1 1 calc R . . C7A C 0.5408(2) 0.02999(18) 0.6405(6) 0.0578(16) Uani 1 1 d U . . H7A H 0.5694 0.0160 0.6581 0.069 Uiso 1 1 calc R A . C8A C 0.54274(19) 0.06911(16) 0.5913(5) 0.0463(13) Uani 1 1 d U A . C9A C 0.50009(16) 0.08921(17) 0.5679(4) 0.0422(12) Uani 1 1 d U . . H9A H 0.5014 0.1154 0.5370 0.051 Uiso 1 1 calc R A . C10A C 0.5908(2) 0.0892(2) 0.5578(5) 0.0592(16) Uani 1 1 d U . . H10A H 0.6059 0.0744 0.4901 0.071 Uiso 1 1 calc R A . H10B H 0.5845 0.1165 0.5292 0.071 Uiso 1 1 calc R . . N4A N 0.62470(16) 0.09074(15) 0.6624(4) 0.0553(13) Uani 1 1 d U A . H4A H 0.6272 0.0650 0.6913 0.066 Uiso 1 1 calc R . . C11A C 0.6740(2) 0.1019(2) 0.6167(7) 0.081(2) Uani 1 1 d U . . H11A H 0.6732 0.1287 0.5801 0.097 Uiso 1 1 calc R A . H11B H 0.6846 0.0829 0.5537 0.097 Uiso 1 1 calc R . . C12A C 0.7096(2) 0.1013(3) 0.7274(7) 0.083(2) Uani 1 1 d U A . H12A H 0.7115 0.0742 0.7616 0.099 Uiso 1 1 calc R . . H12B H 0.7419 0.1092 0.7002 0.099 Uiso 1 1 calc R . . N2 N 0.69170(17) 0.12975(16) 0.8234(6) 0.0701(17) Uani 1 1 d U . . C1B C 0.2982(2) 0.1267(2) 0.9400(7) 0.071(2) Uani 1 1 d U . . H1B1 H 0.2638 0.1201 0.9331 0.086 Uiso 1 1 calc R A . H1B2 H 0.3019 0.1467 1.0051 0.086 Uiso 1 1 calc R . . C2B C 0.32690(19) 0.08893(19) 0.9735(6) 0.0611(17) Uani 1 1 d U A . H2B1 H 0.3169 0.0795 1.0549 0.073 Uiso 1 1 calc R . . H2B2 H 0.3199 0.0678 0.9138 0.073 Uiso 1 1 calc R . . N3B N 0.37992(14) 0.09746(13) 0.9742(4) 0.0462(11) Uani 1 1 d U A . H3B H 0.3856 0.1136 1.0412 0.055 Uiso 1 1 calc R . . C3B C 0.4089(2) 0.05970(16) 0.9947(5) 0.0526(14) Uani 1 1 d U . . H3B1 H 0.4151 0.0470 0.9151 0.063 Uiso 1 1 calc R A . H3B2 H 0.3897 0.0411 1.0443 0.063 Uiso 1 1 calc R . . C4B C 0.45678(19) 0.06731(15) 1.0592(5) 0.0435(12) Uani 1 1 d U A . C5B C 0.4570(2) 0.08489(16) 1.1780(5) 0.0548(15) Uani 1 1 d U . . H5B H 0.4276 0.0916 1.2165 0.066 Uiso 1 1 calc R A . C6B C 0.5007(2) 0.09227(19) 1.2380(5) 0.0612(18) Uani 1 1 d U A . H6B H 0.5006 0.1037 1.3170 0.073 Uiso 1 1 calc R . . C7B C 0.5441(2) 0.08290(17) 1.1818(5) 0.0546(15) Uani 1 1 d U . . H7B H 0.5733 0.0881 1.2228 0.065 Uiso 1 1 calc R A . C8B C 0.54476(19) 0.06552(14) 1.0632(5) 0.0437(12) Uani 1 1 d U A . C9B C 0.50078(17) 0.05826(15) 1.0025(5) 0.0421(12) Uani 1 1 d U . . H9B H 0.5010 0.0472 0.9230 0.051 Uiso 1 1 calc R A . C10B C 0.59278(19) 0.05575(16) 1.0015(5) 0.0504(13) Uani 1 1 d U . . H10C H 0.6107 0.0370 1.0536 0.060 Uiso 1 1 calc R A . H10D H 0.5864 0.0424 0.9229 0.060 Uiso 1 1 calc R . . N4B N 0.62357(15) 0.09201(13) 0.9788(4) 0.0471(11) Uani 1 1 d U A . H4B H 0.6180 0.1089 1.0439 0.057 Uiso 1 1 calc R . . C11B C 0.67574(19) 0.08145(19) 0.9848(7) 0.0653(18) Uani 1 1 d U . . H11C H 0.6821 0.0587 0.9305 0.078 Uiso 1 1 calc R A . H11D H 0.6840 0.0735 1.0689 0.078 Uiso 1 1 calc R . . C12B C 0.7068(2) 0.1164(2) 0.9467(7) 0.076(2) Uani 1 1 d U A . H12C H 0.7031 0.1384 1.0057 0.091 Uiso 1 1 calc R . . H12D H 0.7409 0.1084 0.9453 0.091 Uiso 1 1 calc R . . C1C C 0.3078(3) 0.1870(3) 0.8146(7) 0.090(3) Uani 1 1 d U . . H1C1 H 0.2773 0.1939 0.8552 0.107 Uiso 1 1 calc R A . H1C2 H 0.3055 0.1950 0.7281 0.107 Uiso 1 1 calc R . . C2C C 0.3488(2) 0.2092(2) 0.8752(7) 0.076(2) Uani 1 1 d U A . H2C1 H 0.3502 0.2024 0.9628 0.091 Uiso 1 1 calc R . . H2C2 H 0.3438 0.2381 0.8676 0.091 Uiso 1 1 calc R . . N3C N 0.3956(2) 0.19720(18) 0.8126(6) 0.086(2) Uani 1 1 d U A . H3C H 0.4181 0.2033 0.8721 0.103 Uiso 1 1 calc R . . C3C C 0.4098(3) 0.2222(2) 0.7164(10) 0.111(4) Uani 1 1 d U . . H3C1 H 0.4087 0.2499 0.7462 0.134 Uiso 1 1 calc R A . H3C2 H 0.3858 0.2199 0.6505 0.134 Uiso 1 1 calc R . . C4C C 0.45868(19) 0.21509(17) 0.6619(6) 0.0537(15) Uani 1 1 d U A . C5C C 0.4633(3) 0.20543(18) 0.5348(8) 0.082(3) Uani 1 1 d U . . H5C H 0.4361 0.2022 0.4841 0.098 Uiso 1 1 calc R A . C6C C 0.5120(3) 0.2008(2) 0.4870(7) 0.085(2) Uani 1 1 d U A . H6C H 0.5166 0.1948 0.4034 0.102 Uiso 1 1 calc R . . C7C C 0.5515(3) 0.20505(19) 0.5624(8) 0.0719(19) Uani 1 1 d U . . H7C H 0.5828 0.2020 0.5302 0.086 Uiso 1 1 calc R A . C8C C 0.54539(19) 0.21349(15) 0.6810(6) 0.0537(15) Uani 1 1 d U A . C9C C 0.50041(17) 0.21921(16) 0.7299(5) 0.0439(12) Uani 1 1 d U . . H9C H 0.4978 0.2263 0.8133 0.053 Uiso 1 1 calc R A . C10C C 0.5896(2) 0.21902(19) 0.7696(9) 0.092(3) Uani 1 1 d U . . H10E H 0.6071 0.2432 0.7447 0.110 Uiso 1 1 calc R A . H10F H 0.5772 0.2236 0.8528 0.110 Uiso 1 1 calc R . . N4C N 0.6218(2) 0.18825(16) 0.7746(7) 0.0812(19) Uani 1 1 d U A . H4C H 0.6330 0.1872 0.6950 0.097 Uiso 1 1 calc R . . C11C C 0.6668(2) 0.1998(2) 0.8456(8) 0.083(2) Uani 1 1 d U . . H11E H 0.6755 0.2277 0.8289 0.100 Uiso 1 1 calc R A . H11F H 0.6615 0.1967 0.9341 0.100 Uiso 1 1 calc R . . C12C C 0.7065(3) 0.1719(2) 0.8021(9) 0.093(3) Uani 1 1 d U A . H12E H 0.7126 0.1762 0.7144 0.111 Uiso 1 1 calc R . . H12F H 0.7364 0.1776 0.8471 0.111 Uiso 1 1 calc R . . C1 C 0.50099(16) 0.14230(13) 0.8862(4) 0.0309(11) Uani 0.752(5) 1 d PU A 1 O1 O 0.47121(16) 0.12646(13) 0.8102(4) 0.0364(11) Uani 0.752(5) 1 d PU A 1 O2 O 0.54430(15) 0.14136(13) 0.8860(4) 0.0364(12) Uani 0.752(5) 1 d PU A 1 O3 O 0.47617(15) 0.16319(12) 0.9775(4) 0.0349(11) Uani 0.752(5) 1 d PU A 1 C2 C 0.50521(19) 0.18187(17) 1.0733(5) 0.0489(14) Uani 0.752(5) 1 d PU A 1 H2A H 0.5298 0.1633 1.1008 0.073 Uiso 0.752(5) 1 calc PR A 1 H2B H 0.4846 0.1890 1.1421 0.073 Uiso 0.752(5) 1 calc PR A 1 H2C H 0.5205 0.2057 1.0409 0.073 Uiso 0.752(5) 1 calc PR A 1 C1' C 0.50099(16) 0.14230(13) 0.8862(4) 0.0309(11) Uani 0.25 1 d PU A 2 O1' O 0.5329(5) 0.1239(4) 0.8096(14) 0.040(4) Uiso 0.248(5) 1 d P A 2 O2' O 0.4619(5) 0.1429(4) 0.8900(14) 0.039(4) Uiso 0.248(5) 1 d P A 2 O3' O 0.5317(5) 0.1611(4) 0.9754(14) 0.045(4) Uiso 0.248(5) 1 d P A 2 C2' C 0.50521(19) 0.18187(17) 1.0733(5) 0.0489(14) Uani 0.25 1 d PU A 2 H2'1 H 0.4900 0.2056 1.0399 0.073 Uiso 0.248(5) 1 calc PR A 2 H2'2 H 0.5275 0.1895 1.1381 0.073 Uiso 0.248(5) 1 calc PR A 2 H2'3 H 0.4807 0.1642 1.1066 0.073 Uiso 0.248(5) 1 calc PR A 2 Cl1 Cl 0.35022(4) 0.16740(4) 1.26314(12) 0.0460(3) Uani 1 1 d DU . . O11 O 0.33388(19) 0.12691(13) 1.2660(5) 0.0829(15) Uani 1 1 d DU . . O12 O 0.3705(4) 0.1795(2) 1.3701(7) 0.214(5) Uani 1 1 d DU . . O13 O 0.3837(2) 0.17225(18) 1.1647(7) 0.130(3) Uani 1 1 d DU . . O14 O 0.31176(18) 0.19363(17) 1.2349(8) 0.127(3) Uani 1 1 d DU . . Cl2 Cl 0.6444(2) 0.1677(2) 0.2483(6) 0.0524(14) Uani 0.609(7) 1 d PDU B 1 O21 O 0.6665(2) 0.12934(14) 0.2597(7) 0.105(2) Uani 0.609(7) 1 d PDU B 1 O22 O 0.6010(2) 0.1692(2) 0.3106(7) 0.151(4) Uani 0.609(7) 1 d PDU B 1 O23 O 0.6781(3) 0.1987(2) 0.2850(9) 0.072(2) Uiso 0.609(7) 1 d PD B 1 O24 O 0.6262(3) 0.1755(3) 0.1304(7) 0.095(3) Uani 0.609(7) 1 d PDU B 1 Cl2' Cl 0.6490(3) 0.1695(3) 0.2832(9) 0.055(3) Uani 0.391(7) 1 d PDU B 2 O21' O 0.6665(2) 0.12934(14) 0.2597(7) 0.105(2) Uani 0.39 1 d PDU B 2 O22' O 0.6010(2) 0.1692(2) 0.3106(7) 0.151(4) Uani 0.39 1 d PDU B 2 O23' O 0.6762(6) 0.1963(4) 0.1995(13) 0.113(6) Uani 0.391(7) 1 d PDU B 2 O24' O 0.6614(5) 0.1845(5) 0.4013(12) 0.112(6) Uani 0.391(7) 1 d PDU B 2 Cl3 Cl 0.69112(10) 0.00689(7) 0.3281(3) 0.1073(11) Uani 0.527(7) 1 d PDU C 1 O31 O 0.6657(3) -0.0116(3) 0.2361(9) 0.076(3) Uani 0.527(7) 1 d PDU C 1 O32 O 0.7316(5) -0.0170(5) 0.3717(13) 0.151(6) Uani 0.527(7) 1 d PDU C 1 O33 O 0.6576(4) 0.0051(4) 0.4429(10) 0.130(5) Uani 0.527(7) 1 d PDU C 1 O34 O 0.7074(9) 0.0438(5) 0.325(2) 0.198(11) Uani 0.527(7) 1 d PDU C 1 Cl3' Cl 0.69112(10) 0.00689(7) 0.3281(3) 0.1073(11) Uani 0.47 1 d PDU C 2 O31' O 0.6477(7) 0.0316(7) 0.313(2) 0.259(15) Uani 0.473(7) 1 d PDU C 2 O32' O 0.7243(9) 0.0272(8) 0.3877(16) 0.197(15) Uani 0.473(7) 1 d PDU C 2 O33' O 0.7118(7) 0.0128(6) 0.1931(12) 0.188(9) Uani 0.473(7) 1 d PDU C 2 O34' O 0.6820(6) -0.0315(3) 0.3331(18) 0.152(8) Uani 0.473(7) 1 d PDU C 2 O41 O 0.6841(3) 0.2115(3) 0.5450(8) 0.089(3) Uani 0.50 1 d PU . . C42 C 0.7253(5) 0.2391(5) 0.5660(16) 0.100(5) Uani 0.50 1 d PU . . N51 N 0.6580(16) 0.0003(10) 0.764(2) 0.086(9) Uani 0.50 1 d PU D 1 C52 C 0.6752(12) -0.0181(12) 0.710(4) 0.088(10) Uani 0.50 1 d PU D 1 C53 C 0.7148(6) -0.0406(6) 0.645(2) 0.122(8) Uani 0.50 1 d PU D 1 O51' O 0.6629(10) 0.0075(8) 0.728(3) 0.127(10) Uani 0.50 1 d PU E 2 C52' C 0.673(2) -0.0228(17) 0.666(5) 0.16(2) Uani 0.50 1 d PU E 2 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 0.0386(3) 0.0597(4) 0.0315(3) -0.0030(3) -0.0037(2) 0.0088(3) Zn2 0.0354(3) 0.0378(3) 0.0379(4) 0.0013(3) 0.0022(2) -0.0008(2) N1 0.042(3) 0.111(5) 0.058(4) -0.019(3) -0.003(2) 0.017(3) C1A 0.050(4) 0.204(10) 0.065(5) -0.048(6) -0.023(4) 0.028(5) C2A 0.051(4) 0.209(10) 0.057(5) -0.037(6) -0.018(3) 0.032(5) N3A 0.044(3) 0.121(5) 0.044(3) -0.022(3) -0.015(2) 0.006(3) C3A 0.060(4) 0.107(5) 0.039(3) -0.022(4) -0.007(3) 0.007(4) C4A 0.057(3) 0.059(4) 0.033(3) -0.022(3) 0.000(2) 0.002(3) C5A 0.057(3) 0.060(4) 0.064(4) -0.020(3) 0.010(3) -0.019(3) C6A 0.078(4) 0.039(3) 0.074(5) -0.005(3) 0.011(3) -0.011(3) C7A 0.061(4) 0.050(4) 0.062(4) -0.011(3) 0.013(3) 0.006(3) C8A 0.058(3) 0.048(3) 0.033(3) -0.017(2) 0.013(2) -0.010(2) C9A 0.060(3) 0.046(3) 0.021(2) -0.007(2) 0.003(2) 0.001(2) C10A 0.061(3) 0.076(4) 0.041(3) -0.006(3) 0.016(3) -0.005(3) N4A 0.041(2) 0.067(3) 0.057(3) -0.008(2) 0.013(2) -0.007(2) C11A 0.061(4) 0.110(6) 0.071(5) -0.020(4) 0.034(4) -0.023(4) C12A 0.042(3) 0.108(6) 0.099(6) -0.021(5) 0.022(4) -0.009(3) N2 0.039(3) 0.069(4) 0.102(5) -0.013(3) 0.006(3) -0.008(2) C1B 0.048(3) 0.091(5) 0.076(5) -0.034(4) 0.004(3) -0.002(3) C2B 0.050(3) 0.072(4) 0.061(4) -0.021(3) 0.011(3) -0.018(3) N3B 0.043(2) 0.050(3) 0.045(3) -0.015(2) 0.005(2) -0.0036(19) C3B 0.067(3) 0.042(3) 0.050(3) -0.005(3) 0.008(3) -0.007(3) C4B 0.065(3) 0.034(3) 0.031(3) 0.007(2) 0.004(2) 0.003(2) C5B 0.086(4) 0.047(3) 0.031(3) 0.009(3) 0.014(3) 0.008(3) C6B 0.109(5) 0.054(4) 0.020(2) 0.004(3) -0.002(3) 0.010(3) C7B 0.082(4) 0.051(3) 0.031(3) 0.009(3) -0.013(3) 0.001(3) C8B 0.068(3) 0.031(3) 0.032(3) 0.009(2) 0.002(3) 0.002(2) C9B 0.068(3) 0.026(3) 0.032(3) -0.001(2) 0.007(2) -0.001(2) C10B 0.063(3) 0.041(3) 0.048(3) 0.005(3) -0.003(3) 0.012(3) N4B 0.048(2) 0.043(3) 0.050(3) -0.002(2) -0.011(2) 0.0083(19) C11B 0.050(3) 0.068(4) 0.078(5) -0.004(3) -0.021(3) 0.020(3) C12B 0.042(3) 0.083(5) 0.103(6) -0.020(4) -0.020(4) 0.009(3) C1C 0.075(5) 0.115(7) 0.079(5) 0.008(5) 0.007(4) 0.048(5) C2C 0.069(4) 0.071(5) 0.088(5) 0.020(4) 0.027(4) 0.026(3) N3C 0.083(4) 0.078(4) 0.097(5) 0.042(4) 0.037(3) 0.040(3) C3C 0.066(4) 0.088(6) 0.181(10) 0.061(6) 0.029(5) 0.022(4) C4C 0.041(3) 0.046(3) 0.074(5) 0.022(3) 0.002(3) 0.005(2) C5C 0.114(6) 0.040(3) 0.091(6) 0.026(4) -0.071(5) -0.017(4) C6C 0.161(8) 0.049(4) 0.044(4) 0.008(3) 0.026(5) 0.006(5) C7C 0.080(4) 0.052(4) 0.083(5) 0.018(4) 0.016(4) 0.011(3) C8C 0.047(3) 0.033(3) 0.081(5) 0.013(3) 0.005(3) 0.007(2) C9C 0.057(3) 0.040(3) 0.035(3) 0.008(2) 0.002(2) 0.001(2) C10C 0.055(4) 0.047(4) 0.173(9) -0.011(5) -0.027(5) 0.001(3) N4C 0.075(4) 0.053(3) 0.115(5) 0.023(3) -0.043(4) -0.010(3) C11C 0.081(5) 0.056(4) 0.111(6) 0.024(4) -0.047(4) -0.033(4) C12C 0.065(4) 0.087(6) 0.126(7) 0.009(5) 0.000(5) -0.034(4) C1 0.045(3) 0.026(2) 0.022(2) 0.0089(18) 0.002(2) 0.0022(19) O1 0.042(2) 0.040(3) 0.027(3) -0.003(2) -0.001(2) 0.0080(19) O2 0.043(3) 0.037(3) 0.029(3) 0.004(2) -0.001(2) 0.0059(19) O3 0.045(2) 0.036(2) 0.024(2) -0.0024(19) -0.0010(19) 0.0064(19) C2 0.072(4) 0.042(3) 0.032(3) -0.008(2) -0.002(3) 0.002(2) C1' 0.045(3) 0.026(2) 0.022(2) 0.0089(18) 0.002(2) 0.0022(19) C2' 0.072(4) 0.042(3) 0.032(3) -0.008(2) -0.002(3) 0.002(2) Cl1 0.0469(7) 0.0545(8) 0.0366(7) -0.0057(6) -0.0050(6) -0.0097(6) O11 0.094(4) 0.064(3) 0.091(4) 0.002(3) -0.005(3) -0.024(3) O12 0.385(13) 0.147(7) 0.109(6) 0.035(5) -0.156(8) -0.142(8) O13 0.136(5) 0.082(4) 0.171(7) -0.015(4) 0.095(5) -0.012(3) O14 0.072(3) 0.086(4) 0.222(8) -0.004(5) -0.006(4) 0.017(3) Cl2 0.0424(18) 0.073(3) 0.042(3) -0.0235(19) -0.0010(16) 0.0119(14) O21 0.103(4) 0.066(3) 0.147(6) -0.022(3) -0.011(4) 0.024(3) O22 0.084(4) 0.166(7) 0.202(9) -0.060(6) 0.042(5) 0.004(4) O24 0.102(6) 0.125(8) 0.057(5) -0.010(5) -0.037(5) 0.023(6) Cl2' 0.052(3) 0.050(3) 0.065(6) 0.004(4) 0.006(4) 0.003(2) O21' 0.103(4) 0.066(3) 0.147(6) -0.022(3) -0.011(4) 0.024(3) O22' 0.084(4) 0.166(7) 0.202(9) -0.060(6) 0.042(5) 0.004(4) O23' 0.161(15) 0.120(13) 0.058(10) 0.033(9) 0.042(10) 0.029(11) O24' 0.122(12) 0.110(12) 0.104(12) -0.049(10) 0.018(10) -0.013(9) Cl3 0.116(2) 0.0759(16) 0.130(2) -0.0322(14) 0.0034(16) -0.0290(13) O31 0.078(6) 0.084(7) 0.066(6) -0.020(5) 0.000(5) -0.014(5) O32 0.162(14) 0.170(15) 0.121(12) -0.035(11) -0.050(10) 0.021(13) O33 0.097(8) 0.211(15) 0.082(8) -0.061(9) 0.031(7) -0.041(8) O34 0.25(2) 0.153(16) 0.19(2) -0.009(15) -0.04(2) -0.137(16) Cl3' 0.116(2) 0.0759(16) 0.130(2) -0.0322(14) 0.0034(16) -0.0290(13) O31' 0.27(3) 0.17(2) 0.33(4) 0.06(2) 0.14(3) 0.09(2) O32' 0.23(3) 0.26(3) 0.099(14) 0.022(16) -0.024(14) -0.19(2) O33' 0.25(2) 0.23(2) 0.089(12) 0.069(13) 0.045(12) 0.050(17) O34' 0.156(15) 0.092(11) 0.21(2) -0.015(11) 0.041(14) -0.079(10) O41 0.105(7) 0.127(9) 0.035(5) 0.007(5) -0.004(5) -0.054(6) C42 0.093(11) 0.100(13) 0.108(14) 0.012(11) -0.010(10) -0.016(9) N51 0.16(2) 0.055(13) 0.046(8) 0.005(8) 0.008(10) -0.012(13) C52 0.081(13) 0.062(17) 0.12(3) 0.005(16) -0.011(15) 0.037(11) C53 0.082(11) 0.098(13) 0.18(2) -0.038(14) -0.029(13) 0.041(10) O51' 0.111(15) 0.093(18) 0.18(3) -0.005(16) -0.012(15) 0.052(13) C52' 0.20(4) 0.10(3) 0.17(4) -0.02(2) 0.08(3) 0.00(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 O2' 2.032(14) . ? Zn1 O1 2.099(4) . ? Zn1 N3A 2.138(5) . ? Zn1 N3B 2.152(5) . ? Zn1 N3C 2.192(6) . ? Zn1 N1 2.291(5) . ? Zn1 Zn2 5.9817(9) . ? Zn2 O2 2.061(4) . ? Zn2 N4A 2.117(5) . ? Zn2 N4C 2.155(5) . ? Zn2 O1' 2.168(14) . ? Zn2 N4B 2.168(4) . ? Zn2 N2 2.279(5) . ? N1 C1B 1.491(9) . ? N1 C1C 1.501(10) . ? N1 C1A 1.526(9) . ? C1A C2A 1.541(10) . ? C2A N3A 1.524(8) . ? N3A C3A 1.487(8) . ? C3A C4A 1.537(8) . ? C4A C9A 1.395(7) . ? C4A C5A 1.403(8) . ? C5A C6A 1.414(9) . ? C6A C7A 1.404(8) . ? C7A C8A 1.429(8) . ? C8A C9A 1.396(7) . ? C8A C10A 1.550(7) . ? C10A N4A 1.490(7) . ? N4A C11A 1.514(7) . ? C11A C12A 1.572(10) . ? C12A N2 1.513(9) . ? N2 C12B 1.489(9) . ? N2 C12C 1.502(8) . ? C1B C2B 1.552(9) . ? C2B N3B 1.510(6) . ? N3B C3B 1.527(7) . ? C3B C4B 1.537(7) . ? C4B C9B 1.413(7) . ? C4B C5B 1.435(7) . ? C5B C6B 1.410(8) . ? C6B C7B 1.397(8) . ? C7B C8B 1.430(7) . ? C8B C9B 1.420(7) . ? C8B C10B 1.540(7) . ? C10B N4B 1.518(7) . ? N4B C11B 1.503(6) . ? C11B C12B 1.526(9) . ? C1C C2C 1.523(10) . ? C2C N3C 1.533(7) . ? N3C C3C 1.410(9) . ? C3C C4C 1.512(9) . ? C4C C9C 1.392(7) . ? C4C C5C 1.440(10) . ? C5C C6C 1.468(11) . ? C6C C7C 1.387(10) . ? C7C C8C 1.345(9) . ? C8C C9C 1.381(7) . ? C8C C10C 1.586(9) . ? C10C N4C 1.376(8) . ? N4C C11C 1.532(8) . ? C11C C12C 1.531(11) . ? C1 O2 1.212(6) . ? C1 O1 1.295(6) . ? C1 O3 1.409(6) . ? O3 C2 1.472(6) . ? Cl1 O12 1.367(6) . ? Cl1 O14 1.428(5) . ? Cl1 O13 1.440(5) . ? Cl1 O11 1.442(4) . ? Cl2 O22 1.396(8) . ? Cl2 O24 1.417(9) . ? Cl2 O21 1.441(8) . ? Cl2 O23 1.465(9) . ? Cl2' O24' 1.436(13) . ? Cl2' O23' 1.499(12) . ? Cl3 O34 1.327(12) . ? Cl3 O31 1.385(8) . ? Cl3 O32 1.470(11) . ? Cl3 O33 1.574(9) . ? O41 C42 1.502(16) . ? C42 C42 1.56(3) 2_655 ? N51 C52 0.98(5) . ? C52 C53 1.52(4) . ? O51' C52' 1.26(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2' Zn1 O1 30.0(4) . . ? O2' Zn1 N3A 130.7(4) . . ? O1 Zn1 N3A 100.76(18) . . ? O2' Zn1 N3B 88.0(4) . . ? O1 Zn1 N3B 100.76(16) . . ? N3A Zn1 N3B 109.3(2) . . ? O2' Zn1 N3C 80.9(4) . . ? O1 Zn1 N3C 96.08(19) . . ? N3A Zn1 N3C 119.4(3) . . ? N3B Zn1 N3C 123.9(2) . . ? O2' Zn1 N1 147.9(4) . . ? O1 Zn1 N1 176.3(2) . . ? N3A Zn1 N1 81.35(19) . . ? N3B Zn1 N1 81.32(19) . . ? N3C Zn1 N1 80.2(2) . . ? O2' Zn1 Zn2 26.7(4) . . ? O1 Zn1 Zn2 3.97(12) . . ? N3A Zn1 Zn2 104.13(13) . . ? N3B Zn1 Zn2 101.39(11) . . ? N3C Zn1 Zn2 92.53(15) . . ? N1 Zn1 Zn2 172.47(16) . . ? O2 Zn2 N4A 127.27(18) . . ? O2 Zn2 N4C 88.8(2) . . ? N4A Zn2 N4C 110.9(2) . . ? O2 Zn2 O1' 29.3(4) . . ? N4A Zn2 O1' 98.0(4) . . ? N4C Zn2 O1' 100.6(4) . . ? O2 Zn2 N4B 88.61(16) . . ? N4A Zn2 N4B 108.44(19) . . ? N4C Zn2 N4B 132.1(2) . . ? O1' Zn2 N4B 100.0(4) . . ? O2 Zn2 N2 150.5(2) . . ? N4A Zn2 N2 82.26(19) . . ? N4C Zn2 N2 79.3(2) . . ? O1' Zn2 N2 179.8(5) . . ? N4B Zn2 N2 80.0(2) . . ? O2 Zn2 Zn1 25.44(13) . . ? N4A Zn2 Zn1 101.99(12) . . ? N4C Zn2 Zn1 96.75(15) . . ? O1' Zn2 Zn1 4.7(4) . . ? N4B Zn2 Zn1 100.85(11) . . ? N2 Zn2 Zn1 175.07(14) . . ? C1B N1 C1C 111.7(5) . . ? C1B N1 C1A 110.1(6) . . ? C1C N1 C1A 114.3(6) . . ? C1B N1 Zn1 107.0(4) . . ? C1C N1 Zn1 107.5(4) . . ? C1A N1 Zn1 105.9(4) . . ? N1 C1A C2A 110.5(6) . . ? N3A C2A C1A 107.7(6) . . ? C3A N3A C2A 109.6(5) . . ? C3A N3A Zn1 120.9(4) . . ? C2A N3A Zn1 107.2(4) . . ? N3A C3A C4A 112.9(5) . . ? C9A C4A C5A 119.2(5) . . ? C9A C4A C3A 117.8(6) . . ? C5A C4A C3A 122.9(6) . . ? C4A C5A C6A 120.4(5) . . ? C7A C6A C5A 120.0(6) . . ? C6A C7A C8A 119.5(6) . . ? C9A C8A C7A 119.1(5) . . ? C9A C8A C10A 119.0(5) . . ? C7A C8A C10A 121.9(5) . . ? C4A C9A C8A 121.7(5) . . ? N4A C10A C8A 112.6(5) . . ? C10A N4A C11A 109.3(5) . . ? C10A N4A Zn2 121.0(4) . . ? C11A N4A Zn2 107.1(4) . . ? N4A C11A C12A 108.4(5) . . ? N2 C12A C11A 108.7(6) . . ? C12B N2 C12C 110.5(6) . . ? C12B N2 C12A 110.4(6) . . ? C12C N2 C12A 113.9(6) . . ? C12B N2 Zn2 107.5(4) . . ? C12C N2 Zn2 108.2(4) . . ? C12A N2 Zn2 106.0(4) . . ? N1 C1B C2B 110.0(5) . . ? N3B C2B C1B 110.6(5) . . ? C2B N3B C3B 111.2(4) . . ? C2B N3B Zn1 108.2(4) . . ? C3B N3B Zn1 117.6(3) . . ? N3B C3B C4B 113.0(4) . . ? C9B C4B C5B 119.2(5) . . ? C9B C4B C3B 121.3(5) . . ? C5B C4B C3B 119.5(5) . . ? C6B C5B C4B 120.1(5) . . ? C7B C6B C5B 120.4(5) . . ? C6B C7B C8B 120.5(6) . . ? C9B C8B C7B 119.2(5) . . ? C9B C8B C10B 120.7(5) . . ? C7B C8B C10B 120.1(5) . . ? C4B C9B C8B 120.6(5) . . ? N4B C10B C8B 113.2(4) . . ? C11B N4B C10B 110.6(4) . . ? C11B N4B Zn2 109.3(4) . . ? C10B N4B Zn2 118.3(3) . . ? N4B C11B C12B 110.9(5) . . ? N2 C12B C11B 108.8(5) . . ? N1 C1C C2C 110.5(5) . . ? C1C C2C N3C 108.5(6) . . ? C3C N3C C2C 114.7(5) . . ? C3C N3C Zn1 127.5(6) . . ? C2C N3C Zn1 105.5(4) . . ? N3C C3C C4C 117.1(6) . . ? C9C C4C C5C 117.9(5) . . ? C9C C4C C3C 121.9(7) . . ? C5C C4C C3C 120.1(7) . . ? C4C C5C C6C 117.0(6) . . ? C7C C6C C5C 120.9(7) . . ? C8C C7C C6C 120.0(7) . . ? C7C C8C C9C 121.4(6) . . ? C7C C8C C10C 121.4(6) . . ? C9C C8C C10C 117.1(6) . . ? C8C C9C C4C 122.7(6) . . ? N4C C10C C8C 116.5(6) . . ? C10C N4C C11C 111.4(6) . . ? C10C N4C Zn2 129.9(5) . . ? C11C N4C Zn2 105.2(4) . . ? C12C C11C N4C 106.2(6) . . ? N2 C12C C11C 109.7(5) . . ? O2 C1 O1 129.1(5) . . ? O2 C1 O3 120.4(5) . . ? O1 C1 O3 110.5(4) . . ? C1 O1 Zn1 125.6(3) . . ? C1 O2 Zn2 154.5(4) . . ? C1 O3 C2 116.9(4) . . ? O12 Cl1 O14 108.3(6) . . ? O12 Cl1 O13 110.0(5) . . ? O14 Cl1 O13 104.8(5) . . ? O12 Cl1 O11 113.3(4) . . ? O14 Cl1 O11 110.8(3) . . ? O13 Cl1 O11 109.3(3) . . ? O22 Cl2 O24 97.4(6) . . ? O22 Cl2 O21 111.3(6) . . ? O24 Cl2 O21 113.6(6) . . ? O22 Cl2 O23 113.5(6) . . ? O24 Cl2 O23 110.5(7) . . ? O21 Cl2 O23 110.1(6) . . ? O24' Cl2' O23' 102.6(10) . . ? O34 Cl3 O31 125.4(11) . . ? O34 Cl3 O32 105.2(12) . . ? O31 Cl3 O32 112.7(7) . . ? O34 Cl3 O33 105.2(11) . . ? O31 Cl3 O33 105.1(6) . . ? O32 Cl3 O33 100.2(8) . . ? O41 C42 C42 166.0(16) . 2_655 ? N51 C52 C53 163(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3A H3A O34' 0.93 2.05 2.847(12) 142.8 5_656 N3A H3A O31 0.93 2.51 3.432(13) 169.7 5_656 N4A H4A O51' 0.93 2.22 3.09(3) 156.2 . N3B H3B O13 0.93 2.40 3.283(8) 158.0 . N4B H4B O24 0.93 2.45 3.276(10) 147.9 1_556 N3C H3C O3 0.93 2.41 3.111(7) 131.9 . N4C H4C O41 0.93 2.33 3.164(11) 149.1 . _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.433 _refine_diff_density_min -0.571 _refine_diff_density_rms 0.103 data_Complex_11 #(yzn5) _database_code_CSD 181034 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H67 Cl2 N8 O17.50 Zn2' _chemical_formula_weight 1105.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 12.7298(6) _cell_length_b 13.8296(7) _cell_length_c 14.6010(7) _cell_angle_alpha 74.8170(10) _cell_angle_beta 81.7380(10) _cell_angle_gamma 75.4030(10) _cell_volume 2392.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1158 _exptl_absorpt_coefficient_mu 1.193 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6802 _exptl_absorpt_correction_T_max 0.7964 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17593 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0632 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8406 _reflns_number_gt 6057 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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. The cation is fully ordered. One of the perchlorate anions is disordered (67:33) over two sites sharing three of the oxygen sites. The lattice contains three full-occupancy water molecules; additional lattice water molecules have been inserted at 50% occupancy in six positions and at one quarter occupancy in two positions. No hydrogen atoms have been included for the partial occupancy molecules ; _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^)+(0.0689P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8406 _refine_ls_number_parameters 649 _refine_ls_number_restraints 444 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1201 _refine_ls_wR_factor_gt 0.1130 _refine_ls_goodness_of_fit_ref 0.942 _refine_ls_restrained_S_all 0.929 _refine_ls_shift/su_max 0.102 _refine_ls_shift/su_mean 0.003 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 0.30011(3) 0.64439(3) 0.14910(3) 0.02293(12) Uani 1 1 d U . . Zn2 Zn 0.25858(3) 0.26373(3) 0.32175(3) 0.02479(12) Uani 1 1 d U . . N1 N 0.3266(2) 0.8031(2) 0.0891(2) 0.0246(6) Uani 1 1 d U . . C1A C 0.2994(3) 0.8340(3) -0.0106(3) 0.0305(9) Uani 1 1 d U . . H1A1 H 0.3601 0.8012 -0.0508 0.037 Uiso 1 1 calc R . . H1A2 H 0.2887 0.9095 -0.0339 0.037 Uiso 1 1 calc R . . C2A C 0.1952(3) 0.8013(3) -0.0180(3) 0.0303(8) Uani 1 1 d U . . H2A1 H 0.1329 0.8394 0.0168 0.036 Uiso 1 1 calc R . . H2A2 H 0.1798 0.8175 -0.0856 0.036 Uiso 1 1 calc R . . N3A N 0.2095(2) 0.6895(2) 0.0233(2) 0.0276(7) Uani 1 1 d U . . C3A C 0.1060(3) 0.6567(3) 0.0234(3) 0.0296(8) Uani 1 1 d U . . H3A1 H 0.0668 0.7005 -0.0322 0.036 Uiso 1 1 calc R . . H3A2 H 0.0588 0.6669 0.0817 0.036 Uiso 1 1 calc R . . C4A C 0.1269(3) 0.5453(3) 0.0193(2) 0.0255(8) Uani 1 1 d U . . C5A C 0.1693(3) 0.5163(3) -0.0641(3) 0.0305(9) Uani 1 1 d U . . H5A H 0.1860 0.5666 -0.1188 0.037 Uiso 1 1 calc R . . C6A C 0.1881(3) 0.4144(3) -0.0693(3) 0.0307(9) Uani 1 1 d U . . H6A H 0.2181 0.3950 -0.1270 0.037 Uiso 1 1 calc R . . C7A C 0.1628(3) 0.3413(3) 0.0102(3) 0.0299(9) Uani 1 1 d U . . H7A H 0.1756 0.2716 0.0068 0.036 Uiso 1 1 calc R . . C8A C 0.1188(3) 0.3689(3) 0.0951(2) 0.0255(8) Uani 1 1 d U . . C9A C 0.1016(3) 0.4707(3) 0.0990(3) 0.0264(8) Uani 1 1 d U . . H9A H 0.0721 0.4902 0.1568 0.032 Uiso 1 1 calc R . . C10A C 0.0900(3) 0.2887(3) 0.1795(3) 0.0308(9) Uani 1 1 d U . . H10A H 0.0457 0.3230 0.2284 0.037 Uiso 1 1 calc R . . H10B H 0.0450 0.2500 0.1598 0.037 Uiso 1 1 calc R . . N4A N 0.1879(2) 0.2148(2) 0.2224(2) 0.0248(7) Uani 1 1 d U . . C11A C 0.1649(3) 0.1120(3) 0.2680(3) 0.0315(9) Uani 1 1 d U . . H11A H 0.1549 0.0790 0.2184 0.038 Uiso 1 1 calc R . . H11B H 0.0966 0.1200 0.3102 0.038 Uiso 1 1 calc R . . C12A C 0.2575(3) 0.0446(3) 0.3256(3) 0.0306(9) Uani 1 1 d U . . H12A H 0.2401 -0.0227 0.3575 0.037 Uiso 1 1 calc R . . H12B H 0.3249 0.0324 0.2829 0.037 Uiso 1 1 calc R . . N2 N 0.2748(2) 0.0957(2) 0.3977(2) 0.0289(7) Uani 1 1 d U . . C1B C 0.4417(3) 0.8021(3) 0.0968(3) 0.0276(8) Uani 1 1 d U . . H1B1 H 0.4481 0.8189 0.1574 0.033 Uiso 1 1 calc R . . H1B2 H 0.4661 0.8548 0.0437 0.033 Uiso 1 1 calc R . . C2B C 0.5136(3) 0.6967(3) 0.0937(3) 0.0288(8) Uani 1 1 d U . . H2B1 H 0.5124 0.6822 0.0311 0.035 Uiso 1 1 calc R . . H2B2 H 0.5897 0.6953 0.1025 0.035 Uiso 1 1 calc R . . N3B N 0.4726(2) 0.6176(2) 0.1707(2) 0.0260(7) Uani 1 1 d U . . C3B C 0.5130(3) 0.6077(3) 0.2641(3) 0.0298(8) Uani 1 1 d U . . H3B1 H 0.4993 0.6768 0.2771 0.036 Uiso 1 1 calc R . . H3B2 H 0.5926 0.5794 0.2610 0.036 Uiso 1 1 calc R . . C4B C 0.4584(3) 0.5386(3) 0.3452(3) 0.0272(8) Uani 1 1 d U . . C5B C 0.3936(3) 0.5778(3) 0.4188(3) 0.0310(9) Uani 1 1 d U . . H5B H 0.3805 0.6491 0.4164 0.037 Uiso 1 1 calc R . . C6B C 0.3489(3) 0.5144(3) 0.4943(3) 0.0318(9) Uani 1 1 d U . . H6B H 0.3039 0.5421 0.5433 0.038 Uiso 1 1 calc R . . C7B C 0.3691(3) 0.4097(3) 0.4993(3) 0.0315(9) Uani 1 1 d U . . H7B H 0.3384 0.3661 0.5523 0.038 Uiso 1 1 calc R . . C8B C 0.4335(3) 0.3681(3) 0.4280(3) 0.0282(8) Uani 1 1 d U . . C9B C 0.4776(3) 0.4330(3) 0.3514(3) 0.0290(8) Uani 1 1 d U . . H9B H 0.5218 0.4052 0.3021 0.035 Uiso 1 1 calc R . . C10B C 0.4605(3) 0.2539(3) 0.4362(3) 0.0328(9) Uani 1 1 d U . . H10C H 0.5402 0.2277 0.4387 0.039 Uiso 1 1 calc R . . H10D H 0.4249 0.2201 0.4968 0.039 Uiso 1 1 calc R . . N4B N 0.4257(2) 0.2252(2) 0.3564(2) 0.0275(7) Uani 1 1 d U . . C11B C 0.4640(3) 0.1130(3) 0.3628(3) 0.0303(8) Uani 1 1 d U . . H11C H 0.5374 0.0884 0.3865 0.036 Uiso 1 1 calc R . . H11D H 0.4690 0.0994 0.2988 0.036 Uiso 1 1 calc R . . C12B C 0.3862(3) 0.0563(3) 0.4291(3) 0.0322(9) Uani 1 1 d U . . H12C H 0.4101 -0.0180 0.4307 0.039 Uiso 1 1 calc R . . H12D H 0.3863 0.0649 0.4943 0.039 Uiso 1 1 calc R . . C1C C 0.2531(3) 0.8671(3) 0.1492(3) 0.0286(8) Uani 1 1 d U . . H1C1 H 0.1798 0.8904 0.1253 0.034 Uiso 1 1 calc R . . H1C2 H 0.2811 0.9286 0.1458 0.034 Uiso 1 1 calc R . . C2C C 0.2456(3) 0.8062(3) 0.2508(3) 0.0295(8) Uani 1 1 d U . . H2C1 H 0.3178 0.7884 0.2763 0.035 Uiso 1 1 calc R . . H2C2 H 0.1936 0.8487 0.2899 0.035 Uiso 1 1 calc R . . N3C N 0.2086(2) 0.7095(2) 0.2581(2) 0.0255(7) Uani 1 1 d U . . C3C C 0.0886(3) 0.7320(3) 0.2553(3) 0.0295(8) Uani 1 1 d U . . H3C1 H 0.0705 0.7644 0.1888 0.035 Uiso 1 1 calc R . . H3C2 H 0.0544 0.7823 0.2942 0.035 Uiso 1 1 calc R . . C4C C 0.0402(3) 0.6389(3) 0.2910(2) 0.0243(8) Uani 1 1 d U . . C5C C -0.0654(3) 0.6472(3) 0.2714(3) 0.0288(8) Uani 1 1 d U . . H5C H -0.1032 0.7084 0.2316 0.035 Uiso 1 1 calc R . . C6C C -0.1160(3) 0.5655(3) 0.3100(3) 0.0322(9) Uani 1 1 d U . . H6C H -0.1880 0.5707 0.2957 0.039 Uiso 1 1 calc R . . C7C C -0.0614(3) 0.4762(3) 0.3697(3) 0.0294(8) Uani 1 1 d U . . H7C H -0.0968 0.4211 0.3966 0.035 Uiso 1 1 calc R . . C8C C 0.0435(3) 0.4673(3) 0.3897(2) 0.0244(8) Uani 1 1 d U . . C9C C 0.0944(3) 0.5491(3) 0.3490(2) 0.0245(8) Uani 1 1 d U . . H9C H 0.1673 0.5429 0.3613 0.029 Uiso 1 1 calc R . . C10C C 0.1008(3) 0.3761(3) 0.4619(3) 0.0279(8) Uani 1 1 d U . . H10E H 0.1675 0.3915 0.4766 0.033 Uiso 1 1 calc R . . H10F H 0.0525 0.3662 0.5215 0.033 Uiso 1 1 calc R . . N4C N 0.1311(2) 0.2795(2) 0.4291(2) 0.0275(7) Uani 1 1 d U . . C11C C 0.1624(3) 0.1908(3) 0.5108(3) 0.0326(9) Uani 1 1 d U . . H11E H 0.1014 0.1894 0.5612 0.039 Uiso 1 1 calc R . . H11F H 0.2261 0.1982 0.5379 0.039 Uiso 1 1 calc R . . C12C C 0.1903(3) 0.0913(3) 0.4780(3) 0.0354(9) Uani 1 1 d U . . H12E H 0.2168 0.0330 0.5314 0.042 Uiso 1 1 calc R . . H12F H 0.1241 0.0798 0.4581 0.042 Uiso 1 1 calc R . . C1 C 0.3405(3) 0.4147(3) 0.1753(3) 0.0264(8) Uani 1 1 d U . . O1 O 0.34367(19) 0.50455(18) 0.12394(17) 0.0286(6) Uani 1 1 d U . . O2 O 0.26866(19) 0.40321(18) 0.24661(17) 0.0289(6) Uani 1 1 d U . . O3 O 0.4116(2) 0.33671(19) 0.15509(19) 0.0358(6) Uani 1 1 d U . . Cl1 Cl 0.59891(8) -0.11946(7) 0.26285(7) 0.0340(2) Uani 1 1 d U . . O11 O 0.5780(3) -0.0310(2) 0.1844(2) 0.0600(9) Uani 1 1 d U . . O12 O 0.4979(2) -0.1421(3) 0.3086(2) 0.0544(8) Uani 1 1 d U . . O13 O 0.6622(2) -0.2041(2) 0.2258(2) 0.0568(9) Uani 1 1 d U . . O14 O 0.6556(3) -0.0982(2) 0.3300(2) 0.0539(8) Uani 1 1 d U . . Cl2 Cl 0.13433(18) 0.80585(17) 0.50327(19) 0.0387(6) Uani 0.668(4) 1 d PU A 2 O21 O 0.0784(4) 0.8995(3) 0.4460(4) 0.0587(15) Uani 0.668(4) 1 d PU A 2 O22 O 0.2436(3) 0.8181(3) 0.5081(3) 0.0858(14) Uani 0.668(4) 1 d PU A 2 O23 O 0.1369(3) 0.7239(2) 0.4677(2) 0.0581(10) Uani 0.668(4) 1 d PU A 2 O24 O 0.0765(3) 0.7918(3) 0.5992(2) 0.0721(12) Uani 0.668(4) 1 d PU A 2 Cl2' Cl 0.1695(4) 0.7739(3) 0.5491(4) 0.0397(11) Uani 0.332(4) 1 d PU A 1 O21' O 0.2320(11) 0.6932(9) 0.6177(9) 0.095(4) Uani 0.332(4) 1 d PU A 1 O22' O 0.2436(3) 0.8181(3) 0.5081(3) 0.0858(14) Uani 0.33 1 d PU A 1 O23' O 0.1369(3) 0.7239(2) 0.4677(2) 0.0581(10) Uani 0.33 1 d PU A 1 O24' O 0.0765(3) 0.7918(3) 0.5992(2) 0.0721(12) Uani 0.33 1 d PU A 1 O1W O 0.4100(2) 0.15750(19) 0.11499(18) 0.0359(6) Uani 1 1 d U . . O2W O 0.3096(2) 0.0846(2) -0.00236(19) 0.0438(7) Uani 1 1 d U . . O3W O 0.5916(2) 0.4251(3) 0.0816(2) 0.0587(9) Uani 1 1 d U . . O4W O 0.9161(9) -0.1020(10) 0.0255(7) 0.055(3) Uani 0.50 1 d PU B 1 O4W' O 0.9099(10) -0.0989(10) -0.0206(6) 0.057(3) Uani 0.50 1 d PU C 2 O5W O 0.9787(13) -0.0297(12) 0.1194(9) 0.070(4) Uani 0.50 1 d PU D 2 O5W' O 0.9742(15) -0.0156(13) 0.1600(9) 0.075(4) Uani 0.50 1 d PU E 1 O6W O 0.6855(6) 0.2482(5) 0.2447(6) 0.083(2) Uani 0.50 1 d PU F 1 O7W O 0.8075(9) 0.0350(9) 0.2578(6) 0.115(3) Uani 0.50 1 d PU G 1 O7W' O 0.9037(17) -0.0078(14) 0.2390(14) 0.092(5) Uiso 0.25 1 d P H 2 O7W" O 0.8141(17) 0.2040(16) 0.2501(15) 0.117(6) Uiso 0.25 1 d P I 3 H3AC H 0.2634 0.6584 -0.0144 0.040 Uiso 1 1 d . . . H4AC H 0.2449 0.2048 0.1760 0.040 Uiso 1 1 d . . . H3BC H 0.4963 0.5601 0.1544 0.040 Uiso 1 1 d . . . H4BC H 0.4576 0.2641 0.3007 0.040 Uiso 1 1 d . . . H3CC H 0.2253 0.6629 0.3228 0.040 Uiso 1 1 d . . . H4CC H 0.0591 0.2741 0.4058 0.040 Uiso 1 1 d . . . H1WA H 0.4162 0.2131 0.1260 0.040 Uiso 1 1 d . . . H1WB H 0.4594 0.1059 0.1382 0.040 Uiso 1 1 d . . . H2WA H 0.3323 0.1007 -0.0603 0.040 Uiso 1 1 d . . . H2WB H 0.3408 0.1071 0.0341 0.040 Uiso 1 1 d . . . H3WA H 0.6105 0.4471 0.0193 0.040 Uiso 1 1 d . . . H3WB H 0.5274 0.4175 0.0817 0.040 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0212(2) 0.0236(2) 0.0259(2) -0.00818(17) -0.00195(17) -0.00606(17) Zn2 0.0276(2) 0.0234(2) 0.0240(2) -0.00911(18) -0.00558(17) -0.00126(17) N1 0.0229(15) 0.0260(16) 0.0256(16) -0.0074(13) 0.0010(12) -0.0074(13) C1A 0.036(2) 0.029(2) 0.028(2) -0.0059(16) -0.0013(16) -0.0108(17) C2A 0.031(2) 0.027(2) 0.030(2) 0.0012(16) -0.0082(16) -0.0076(16) N3A 0.0266(16) 0.0292(17) 0.0294(17) -0.0081(13) -0.0047(13) -0.0080(13) C3A 0.026(2) 0.031(2) 0.034(2) -0.0059(17) -0.0101(16) -0.0087(16) C4A 0.0196(18) 0.031(2) 0.030(2) -0.0090(16) -0.0067(15) -0.0086(15) C5A 0.0230(19) 0.042(2) 0.028(2) -0.0067(17) -0.0055(15) -0.0099(17) C6A 0.025(2) 0.042(2) 0.028(2) -0.0163(18) -0.0052(16) -0.0020(17) C7A 0.026(2) 0.031(2) 0.037(2) -0.0160(17) -0.0112(16) -0.0004(16) C8A 0.0193(18) 0.031(2) 0.0280(19) -0.0082(16) -0.0077(15) -0.0039(15) C9A 0.0216(18) 0.035(2) 0.0256(19) -0.0113(16) -0.0072(15) -0.0051(16) C10A 0.027(2) 0.032(2) 0.034(2) -0.0083(17) -0.0085(16) -0.0044(16) N4A 0.0221(15) 0.0249(16) 0.0284(16) -0.0096(13) -0.0031(12) -0.0029(12) C11A 0.037(2) 0.028(2) 0.033(2) -0.0102(17) -0.0042(17) -0.0093(17) C12A 0.040(2) 0.0240(19) 0.031(2) -0.0116(16) -0.0056(17) -0.0059(17) N2 0.0345(18) 0.0260(17) 0.0262(16) -0.0080(13) -0.0059(14) -0.0030(14) C1B 0.0271(19) 0.030(2) 0.029(2) -0.0088(16) 0.0015(15) -0.0130(16) C2B 0.0240(19) 0.035(2) 0.029(2) -0.0098(17) 0.0033(15) -0.0109(16) N3B 0.0234(16) 0.0259(16) 0.0311(17) -0.0103(13) -0.0038(13) -0.0053(13) C3B 0.027(2) 0.033(2) 0.034(2) -0.0098(17) -0.0078(16) -0.0092(16) C4B 0.0233(19) 0.030(2) 0.032(2) -0.0091(16) -0.0123(16) -0.0065(16) C5B 0.029(2) 0.030(2) 0.039(2) -0.0156(18) -0.0121(17) -0.0026(16) C6B 0.026(2) 0.042(2) 0.030(2) -0.0144(18) -0.0045(16) -0.0053(17) C7B 0.029(2) 0.042(2) 0.027(2) -0.0068(17) -0.0087(16) -0.0110(17) C8B 0.0253(19) 0.031(2) 0.031(2) -0.0077(17) -0.0115(16) -0.0051(16) C9B 0.0260(19) 0.037(2) 0.029(2) -0.0128(17) -0.0091(16) -0.0061(16) C10B 0.039(2) 0.031(2) 0.029(2) -0.0060(17) -0.0135(17) -0.0059(17) N4B 0.0291(16) 0.0250(16) 0.0271(16) -0.0057(13) -0.0098(13) 0.0002(13) C11B 0.033(2) 0.027(2) 0.029(2) -0.0091(16) -0.0088(16) 0.0020(16) C12B 0.042(2) 0.026(2) 0.027(2) -0.0093(16) -0.0105(17) 0.0015(17) C1C 0.0268(19) 0.0233(19) 0.036(2) -0.0099(16) 0.0024(16) -0.0067(15) C2C 0.030(2) 0.030(2) 0.033(2) -0.0148(17) 0.0041(16) -0.0120(16) N3C 0.0231(15) 0.0257(16) 0.0279(16) -0.0064(13) 0.0003(13) -0.0069(13) C3C 0.0263(19) 0.026(2) 0.034(2) -0.0065(16) -0.0004(16) -0.0028(16) C4C 0.0213(18) 0.030(2) 0.0230(18) -0.0096(15) 0.0030(14) -0.0069(15) C5C 0.027(2) 0.032(2) 0.0250(19) -0.0040(16) -0.0030(15) -0.0036(16) C6C 0.0238(19) 0.048(2) 0.028(2) -0.0118(18) 0.0000(16) -0.0126(18) C7C 0.036(2) 0.028(2) 0.027(2) -0.0085(16) 0.0006(16) -0.0118(17) C8C 0.0266(19) 0.0240(19) 0.0236(18) -0.0119(15) 0.0013(15) -0.0030(15) C9C 0.0208(18) 0.028(2) 0.0266(19) -0.0135(16) 0.0008(15) -0.0036(15) C10C 0.030(2) 0.028(2) 0.028(2) -0.0134(16) -0.0007(16) -0.0050(16) N4C 0.0335(17) 0.0244(16) 0.0241(16) -0.0077(13) -0.0047(13) -0.0023(13) C11C 0.042(2) 0.028(2) 0.024(2) -0.0043(16) -0.0020(17) -0.0038(17) C12C 0.043(2) 0.030(2) 0.029(2) -0.0037(17) -0.0009(18) -0.0056(18) C1 0.0205(18) 0.037(2) 0.028(2) -0.0166(17) -0.0078(16) -0.0047(16) O1 0.0276(14) 0.0256(14) 0.0343(14) -0.0094(11) -0.0034(11) -0.0063(11) O2 0.0264(13) 0.0304(14) 0.0300(14) -0.0086(11) -0.0044(11) -0.0037(11) O3 0.0343(15) 0.0326(15) 0.0416(16) -0.0178(12) -0.0065(12) 0.0018(12) Cl1 0.0360(5) 0.0348(5) 0.0337(5) -0.0145(4) -0.0087(4) -0.0025(4) O11 0.079(2) 0.0510(19) 0.0387(17) -0.0034(15) -0.0158(16) 0.0046(17) O12 0.0416(18) 0.075(2) 0.057(2) -0.0342(17) 0.0107(15) -0.0195(16) O13 0.0437(18) 0.0504(19) 0.083(2) -0.0413(18) 0.0049(16) -0.0016(15) O14 0.060(2) 0.067(2) 0.0440(18) -0.0172(16) -0.0228(15) -0.0175(17) Cl2 0.0371(11) 0.0405(11) 0.0427(13) -0.0160(10) 0.0091(9) -0.0167(9) O21 0.057(3) 0.034(3) 0.079(4) -0.012(2) 0.015(3) -0.011(2) O22 0.058(2) 0.121(3) 0.084(3) -0.016(2) 0.002(2) -0.044(2) O23 0.081(2) 0.0430(19) 0.0490(19) -0.0116(15) 0.0106(17) -0.0193(17) O24 0.059(2) 0.106(3) 0.066(2) -0.045(2) 0.0139(18) -0.030(2) Cl2' 0.040(2) 0.036(2) 0.046(3) -0.0109(19) -0.0017(19) -0.0141(17) O21' 0.125(9) 0.078(8) 0.099(8) -0.034(7) -0.049(7) -0.017(7) O22' 0.058(2) 0.121(3) 0.084(3) -0.016(2) 0.002(2) -0.044(2) O23' 0.081(2) 0.0430(19) 0.0490(19) -0.0116(15) 0.0106(17) -0.0193(17) O24' 0.059(2) 0.106(3) 0.066(2) -0.045(2) 0.0139(18) -0.030(2) O1W 0.0413(16) 0.0330(15) 0.0341(15) -0.0118(12) -0.0030(12) -0.0055(12) O2W 0.0474(17) 0.0529(18) 0.0396(16) -0.0172(14) 0.0076(13) -0.0263(14) O3W 0.0343(17) 0.079(2) 0.079(2) -0.048(2) 0.0138(16) -0.0192(16) O4W 0.033(4) 0.050(5) 0.074(7) -0.004(6) -0.003(5) -0.007(3) O4W' 0.052(5) 0.047(4) 0.066(6) -0.002(6) -0.011(5) -0.008(3) O5W 0.039(5) 0.054(6) 0.100(9) 0.004(7) -0.013(7) 0.000(4) O5W' 0.064(6) 0.064(7) 0.082(8) 0.007(6) -0.021(7) -0.001(5) O6W 0.098(6) 0.063(5) 0.092(5) -0.051(4) 0.051(4) -0.021(4) O7W 0.140(8) 0.153(8) 0.073(5) -0.017(5) 0.003(5) -0.085(7) _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 1.989(2) . ? Zn1 N3C 2.095(3) . ? Zn1 N3A 2.177(3) . ? Zn1 N3B 2.188(3) . ? Zn1 N1 2.232(3) . ? Zn1 Zn2 5.3308(6) . ? Zn2 O2 1.979(2) . ? Zn2 N4C 2.100(3) . ? Zn2 N4A 2.137(3) . ? Zn2 N4B 2.159(3) . ? Zn2 N2 2.269(3) . ? N1 C1A 1.471(4) . ? N1 C1C 1.477(4) . ? N1 C1B 1.481(4) . ? C1A C2A 1.531(5) . ? C2A N3A 1.479(4) . ? N3A C3A 1.497(4) . ? C3A C4A 1.511(5) . ? C4A C5A 1.377(5) . ? C4A C9A 1.397(5) . ? C5A C6A 1.389(5) . ? C6A C7A 1.383(5) . ? C7A C8A 1.392(5) . ? C8A C9A 1.385(5) . ? C8A C10A 1.497(5) . ? C10A N4A 1.495(4) . ? N4A C11A 1.487(4) . ? C11A C12A 1.512(5) . ? C12A N2 1.480(4) . ? N2 C12C 1.474(5) . ? N2 C12B 1.478(5) . ? C1B C2B 1.521(5) . ? C2B N3B 1.486(4) . ? N3B C3B 1.487(4) . ? C3B C4B 1.518(5) . ? C4B C5B 1.398(5) . ? C4B C9B 1.400(5) . ? C5B C6B 1.368(5) . ? C6B C7B 1.390(5) . ? C7B C8B 1.385(5) . ? C8B C9B 1.385(5) . ? C8B C10B 1.505(5) . ? C10B N4B 1.481(4) . ? N4B C11B 1.487(4) . ? C11B C12B 1.500(5) . ? C1C C2C 1.506(5) . ? C2C N3C 1.499(4) . ? N3C C3C 1.485(4) . ? C3C C4C 1.504(5) . ? C4C C5C 1.386(5) . ? C4C C9C 1.386(5) . ? C5C C6C 1.392(5) . ? C6C C7C 1.395(5) . ? C7C C8C 1.377(5) . ? C8C C9C 1.400(5) . ? C8C C10C 1.514(5) . ? C10C N4C 1.479(4) . ? N4C C11C 1.487(4) . ? C11C C12C 1.516(5) . ? C1 O1 1.279(4) . ? C1 O2 1.288(4) . ? C1 O3 1.292(4) . ? Cl1 O14 1.425(3) . ? Cl1 O13 1.429(3) . ? Cl1 O12 1.430(3) . ? Cl1 O11 1.439(3) . ? Cl2 O23 1.356(3) . ? Cl2 O21 1.422(6) . ? Cl2 O22 1.456(4) . ? Cl2 O24 1.475(4) . ? Cl2' O21' 1.442(14) . ? 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 N3C 135.72(11) . . ? O1 Zn1 N3A 86.53(10) . . ? N3C Zn1 N3A 110.42(11) . . ? O1 Zn1 N3B 83.66(10) . . ? N3C Zn1 N3B 107.96(11) . . ? N3A Zn1 N3B 133.72(11) . . ? O1 Zn1 N1 140.98(10) . . ? N3C Zn1 N1 83.20(11) . . ? N3A Zn1 N1 79.77(11) . . ? N3B Zn1 N1 80.08(10) . . ? O1 Zn1 Zn2 41.49(7) . . ? N3C Zn1 Zn2 94.27(8) . . ? N3A Zn1 Zn2 105.97(8) . . ? N3B Zn1 Zn2 95.86(8) . . ? N1 Zn1 Zn2 174.24(7) . . ? O2 Zn2 N4C 107.88(11) . . ? O2 Zn2 N4A 99.67(10) . . ? N4C Zn2 N4A 102.33(11) . . ? O2 Zn2 N4B 92.82(10) . . ? N4C Zn2 N4B 120.07(11) . . ? N4A Zn2 N4B 129.32(11) . . ? O2 Zn2 N2 170.76(10) . . ? N4C Zn2 N2 80.88(11) . . ? N4A Zn2 N2 80.87(11) . . ? N4B Zn2 N2 79.94(11) . . ? O2 Zn2 Zn1 5.61(7) . . ? N4C Zn2 Zn1 105.88(8) . . ? N4A Zn2 Zn1 105.26(8) . . ? N4B Zn2 Zn1 89.43(8) . . ? N2 Zn2 Zn1 169.29(8) . . ? C1A N1 C1C 112.7(3) . . ? C1A N1 C1B 111.9(3) . . ? C1C N1 C1B 110.4(3) . . ? C1A N1 Zn1 107.3(2) . . ? C1C N1 Zn1 105.4(2) . . ? C1B N1 Zn1 108.7(2) . . ? N1 C1A C2A 109.8(3) . . ? N3A C2A C1A 109.2(3) . . ? C2A N3A C3A 110.3(3) . . ? C2A N3A Zn1 110.1(2) . . ? C3A N3A Zn1 122.0(2) . . ? N3A C3A C4A 112.0(3) . . ? C5A C4A C9A 119.0(3) . . ? C5A C4A C3A 120.1(3) . . ? C9A C4A C3A 120.9(3) . . ? C4A C5A C6A 120.9(4) . . ? C7A C6A C5A 119.5(3) . . ? C6A C7A C8A 120.7(3) . . ? C9A C8A C7A 118.8(3) . . ? C9A C8A C10A 121.5(3) . . ? C7A C8A C10A 119.6(3) . . ? C8A C9A C4A 121.1(3) . . ? N4A C10A C8A 112.8(3) . . ? C11A N4A C10A 111.5(3) . . ? C11A N4A Zn2 108.9(2) . . ? C10A N4A Zn2 115.6(2) . . ? N4A C11A C12A 110.5(3) . . ? N2 C12A C11A 109.5(3) . . ? C12C N2 C12B 112.5(3) . . ? C12C N2 C12A 112.5(3) . . ? C12B N2 C12A 111.4(3) . . ? C12C N2 Zn2 107.0(2) . . ? C12B N2 Zn2 107.5(2) . . ? C12A N2 Zn2 105.4(2) . . ? N1 C1B C2B 110.2(3) . . ? N3B C2B C1B 109.1(3) . . ? C2B N3B C3B 112.4(3) . . ? C2B N3B Zn1 104.5(2) . . ? C3B N3B Zn1 123.5(2) . . ? N3B C3B C4B 112.3(3) . . ? C5B C4B C9B 118.4(3) . . ? C5B C4B C3B 120.7(3) . . ? C9B C4B C3B 120.8(3) . . ? C6B C5B C4B 120.6(3) . . ? C5B C6B C7B 120.1(4) . . ? C8B C7B C6B 120.8(4) . . ? C9B C8B C7B 118.6(3) . . ? C9B C8B C10B 120.5(3) . . ? C7B C8B C10B 120.7(3) . . ? C8B C9B C4B 121.4(3) . . ? N4B C10B C8B 113.2(3) . . ? C10B N4B C11B 111.0(3) . . ? C10B N4B Zn2 123.3(2) . . ? C11B N4B Zn2 105.5(2) . . ? N4B C11B C12B 109.8(3) . . ? N2 C12B C11B 110.5(3) . . ? N1 C1C C2C 110.1(3) . . ? N3C C2C C1C 111.2(3) . . ? C3C N3C C2C 110.5(3) . . ? C3C N3C Zn1 115.4(2) . . ? C2C N3C Zn1 105.9(2) . . ? N3C C3C C4C 114.1(3) . . ? C5C C4C C9C 119.4(3) . . ? C5C C4C C3C 118.3(3) . . ? C9C C4C C3C 122.1(3) . . ? C4C C5C C6C 119.8(3) . . ? C5C C6C C7C 120.2(3) . . ? C8C C7C C6C 120.4(3) . . ? C7C C8C C9C 118.9(3) . . ? C7C C8C C10C 121.6(3) . . ? C9C C8C C10C 119.2(3) . . ? C4C C9C C8C 121.2(3) . . ? N4C C10C C8C 113.5(3) . . ? C10C N4C C11C 109.8(3) . . ? C10C N4C Zn2 118.4(2) . . ? C11C N4C Zn2 105.9(2) . . ? N4C C11C C12C 109.9(3) . . ? N2 C12C C11C 110.2(3) . . ? O1 C1 O2 120.2(3) . . ? O1 C1 O3 118.7(3) . . ? O2 C1 O3 121.1(3) . . ? C1 O1 Zn1 133.6(2) . . ? C1 O2 Zn2 120.2(2) . . ? O14 Cl1 O13 111.01(19) . . ? O14 Cl1 O12 108.84(18) . . ? O13 Cl1 O12 110.02(19) . . ? O14 Cl1 O11 109.5(2) . . ? O13 Cl1 O11 108.0(2) . . ? O12 Cl1 O11 109.5(2) . . ? O23 Cl2 O21 112.0(3) . . ? O23 Cl2 O22 111.6(3) . . ? O21 Cl2 O22 106.6(3) . . ? O23 Cl2 O24 109.0(2) . . ? O21 Cl2 O24 107.8(3) . . ? O22 Cl2 O24 109.8(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3A H3AC O3W 0.91 2.17 3.067(4) 169.6 2_665 N4A H4AC O1W 0.93 2.17 3.053(4) 158.7 . N3B H3BC O3W 0.86 2.37 3.208(4) 165.3 . N4B H4BC O3 0.95 2.19 2.947(4) 135.5 . O1W H1WA O3 0.85 1.85 2.697(3) 172.9 . O1W H1WB O11 0.85 2.12 2.971(4) 173.3 . O2W H2WB O1W 0.87 1.92 2.788(4) 179.9 . O2W H2WA O11 0.84 2.30 3.011(4) 142.4 2_655 O2W H2WA O13 0.84 2.47 3.263(4) 157.6 2_655 O3W H3WA O1 0.90 2.07 2.966(4) 179.0 2_665 O3W H3WB O3 0.85 2.08 2.812(4) 144.4 . O3W H3WB O1 0.85 2.42 3.098(4) 137.3 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.999 _refine_diff_density_min -0.546 _refine_diff_density_rms 0.090