# Copyright The Royal Society of Chemistry, 1998 # MANUSCRIPT 8/03442G data_myoung _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C84 H86 N14 Na4 Ni4 O14' _chemical_formula_weight 1842.47 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.1353 0.1239 '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 10.818(4) _cell_length_b 14.336(5) _cell_length_c 16.281(6) _cell_angle_alpha 109.90(2) _cell_angle_beta 100.46(2) _cell_angle_gamma 107.50(2) _cell_volume 2147.8(13) _cell_formula_units_Z 1 _cell_measurement_temperature 150.0(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 10 _cell_measurement_theta_max 22 _exptl_crystal_description plate _exptl_crystal_colour Green _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method ? _exptl_crystal_F_000 956 _exptl_absorpt_coefficient_mu 1.764 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.368 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method Omega-theta _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6659 _diffrn_reflns_av_R_equivalents 0.0659 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 59.99 _reflns_number_total 6251 _reflns_number_observed 4721 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 7 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0962P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6244 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_obs 0.0509 _refine_ls_wR_factor_all 0.1444 _refine_ls_wR_factor_obs 0.1298 _refine_ls_goodness_of_fit_all 1.010 _refine_ls_goodness_of_fit_obs 1.061 _refine_ls_restrained_S_all 1.013 _refine_ls_restrained_S_obs 1.061 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.69904(6) -0.00086(5) 0.75892(4) 0.0243(2) Uani 1 d . . Ni2 Ni 0.53548(6) 0.34605(5) 0.66804(4) 0.0261(2) Uani 1 d . . Na1 Na 0.55986(15) 0.08809(12) 0.61980(10) 0.0271(4) Uani 1 d . . Na2 Na 0.41736(14) 0.16520(11) 0.46050(10) 0.0247(3) Uani 1 d . . N1R N 0.7174(3) 0.1429(3) 0.8548(2) 0.0300(8) Uani 1 d . . C21 C 0.7828(4) 0.1996(3) 0.8136(3) 0.0304(9) Uani 1 d . . O1R O 0.7831(3) 0.1381(2) 0.7330(2) 0.0295(6) Uani 1 d . . C31 C 0.8439(5) 0.3133(4) 0.8575(3) 0.0455(12) Uani 1 d . . H31 H 0.8916(5) 0.3541(4) 0.8294(3) 0.055 Uiso 1 calc R . C41 C 0.8318(6) 0.3628(4) 0.9426(4) 0.057(2) Uani 1 d . . H41 H 0.8713(6) 0.4393(4) 0.9740(4) 0.069 Uiso 1 calc R . C51 C 0.7624(5) 0.3024(4) 0.9831(3) 0.0508(13) Uani 1 d . . H51 H 0.7533(5) 0.3372(4) 1.0415(3) 0.061 Uiso 1 calc R . C61 C 0.7080(5) 0.1938(4) 0.9389(3) 0.0384(11) Uani 1 d . . C1 C 0.6339(6) 0.1207(5) 0.9774(3) 0.0564(14) Uani 1 d . . H1A H 0.6846(6) 0.0772(5) 0.9874(3) 0.085 Uiso 1 d R . H1B H 0.5422(6) 0.0731(5) 0.9338(3) 0.085 Uiso 1 d R . H1C H 0.6265(6) 0.1642(5) 1.0361(3) 0.085 Uiso 1 d R . N2R N 0.5383(3) -0.1184(3) 0.7682(2) 0.0279(8) Uani 1 d . . C22 C 0.4500(4) -0.1188(3) 0.6975(3) 0.0262(9) Uani 1 d . . O2R O 0.5059(3) -0.0545(2) 0.6626(2) 0.0285(6) Uani 1 d . . C32 C 0.3099(4) -0.1879(3) 0.6655(3) 0.0292(9) Uani 1 d . . H32 H 0.2461(4) -0.1869(3) 0.6177(3) 0.035 Uiso 1 calc R . C42 C 0.2698(4) -0.2565(3) 0.7064(3) 0.0329(10) Uani 1 d . . H42 H 0.1768(4) -0.3047(3) 0.6856(3) 0.040 Uiso 1 calc R . C52 C 0.3622(4) -0.2568(3) 0.7772(3) 0.0329(10) Uani 1 d . . H52 H 0.3333(4) -0.3048(3) 0.8047(3) 0.040 Uiso 1 calc R . C62 C 0.4969(4) -0.1862(3) 0.8072(3) 0.0294(9) Uani 1 d . . C2 C 0.6042(5) -0.1781(4) 0.8849(3) 0.0397(11) Uani 1 d . . H2A H 0.5686(5) -0.2394(4) 0.9001(3) 0.060 Uiso 1 d R . H2B H 0.6288(5) -0.1107(4) 0.9389(3) 0.060 Uiso 1 d R . H2C H 0.6853(5) -0.1790(4) 0.8664(3) 0.060 Uiso 1 d R . N3R N 0.8823(3) -0.0079(3) 0.8124(2) 0.0247(7) Uani 1 d . . C23 C 0.8575(4) -0.0950(3) 0.7346(3) 0.0263(9) Uani 1 d . . O3R O 0.7487(3) -0.1205(2) 0.6700(2) 0.0281(6) Uani 1 d . . C33 C 0.9483(4) -0.1484(4) 0.7310(3) 0.0348(10) Uani 1 d . . H33 H 0.9299(4) -0.2122(4) 0.6786(3) 0.042 Uiso 1 calc R . C43 C 1.0637(5) -0.1056(4) 0.8052(3) 0.0449(12) Uani 1 d . . H43 H 1.1260(5) -0.1403(4) 0.8042(3) 0.054 Uiso 1 calc R . C53 C 1.0906(5) -0.0126(4) 0.8814(3) 0.0470(13) Uani 1 d . . H53 H 1.1725(5) 0.0184(4) 0.9315(3) 0.056 Uiso 1 calc R . C63 C 0.9960(4) 0.0347(4) 0.8836(3) 0.0340(10) Uani 1 d . . C3 C 1.0185(5) 0.1360(4) 0.9639(3) 0.0511(14) Uani 1 d . . H3A H 1.0311(5) 0.1951(4) 0.9447(3) 0.077 Uiso 1 d R . H3B H 1.1002(5) 0.1545(4) 1.0137(3) 0.077 Uiso 1 d R . H3C H 0.9390(5) 0.1245(4) 0.9858(3) 0.077 Uiso 1 d R . N4R N 0.7453(3) 0.4206(3) 0.7038(2) 0.0307(8) Uani 1 d . . C24 C 0.7459(4) 0.3519(3) 0.6225(3) 0.0307(9) Uani 1 d . . O4R O 0.6274(3) 0.2769(2) 0.5699(2) 0.0346(7) Uani 1 d . . C34 C 0.8699(4) 0.3661(4) 0.6023(3) 0.0355(10) Uani 1 d . . H34 H 0.8725(4) 0.3179(4) 0.5463(3) 0.043 Uiso 1 calc R . C44 C 0.9860(4) 0.4505(4) 0.6648(3) 0.0424(11) Uani 1 d . . H44 H 1.0703(4) 0.4610(4) 0.6523(3) 0.051 Uiso 1 calc R . C54 C 0.9824(4) 0.5216(4) 0.7469(3) 0.0423(11) Uani 1 d . . H54 H 1.0631(4) 0.5812(4) 0.7897(3) 0.051 Uiso 1 calc R . C64 C 0.8590(4) 0.5040(4) 0.7653(3) 0.0372(10) Uani 1 d . . C4 C 0.8461(5) 0.5759(4) 0.8525(3) 0.0501(13) Uani 1 d . . H4A H 0.8242(5) 0.6338(4) 0.8431(3) 0.075 Uiso 1 d R . H4B H 0.9326(5) 0.6072(4) 0.9024(3) 0.075 Uiso 1 d R . H4C H 0.7731(5) 0.5335(4) 0.8688(3) 0.075 Uiso 1 d R . N5R N 0.4699(3) 0.4436(3) 0.6176(2) 0.0293(8) Uani 1 d . . C25 C 0.3478(4) 0.3630(3) 0.5674(3) 0.0284(9) Uani 1 d . . O5R O 0.3394(3) 0.2701(2) 0.5683(2) 0.0258(6) Uani 1 d . . C35 C 0.2409(5) 0.3813(4) 0.5211(3) 0.0414(11) Uani 1 d . . H35 H 0.1528(5) 0.3252(4) 0.4880(3) 0.050 Uiso 1 calc R . C45 C 0.2681(6) 0.4836(4) 0.5252(4) 0.0487(13) Uani 1 d . . H45 H 0.1981(6) 0.4982(4) 0.4940(4) 0.058 Uiso 1 calc R . C55 C 0.3972(6) 0.5656(4) 0.5746(3) 0.0467(13) Uani 1 d . . H55 H 0.4164(6) 0.6354(4) 0.5762(3) 0.056 Uiso 1 calc R . C65 C 0.4964(5) 0.5438(3) 0.6210(3) 0.0363(11) Uani 1 d . . C5 C 0.6366(5) 0.6277(4) 0.6787(4) 0.0476(13) Uani 1 d . . H5A H 0.6468(5) 0.6946(4) 0.6719(4) 0.071 Uiso 1 d R . H5B H 0.7051(5) 0.6021(4) 0.6585(4) 0.071 Uiso 1 d R . H5C H 0.6497(5) 0.6410(4) 0.7435(4) 0.071 Uiso 1 d R . N6R N 0.4675(3) 0.3621(3) 0.7823(2) 0.0297(8) Uani 1 d . . C26 C 0.4687(4) 0.2651(3) 0.7754(3) 0.0260(9) Uani 1 d . . O6R O 0.5182(3) 0.2222(2) 0.7126(2) 0.0320(7) Uani 1 d . . C36 C 0.4154(5) 0.2180(4) 0.8309(3) 0.0378(10) Uani 1 d . . H36 H 0.4158(5) 0.1502(4) 0.8259(3) 0.045 Uiso 1 calc R . C46 C 0.3629(5) 0.2727(4) 0.8922(3) 0.0432(11) Uani 1 d . . H46 H 0.3261(5) 0.2423(4) 0.9303(3) 0.052 Uiso 1 calc R . C56 C 0.3627(5) 0.3728(4) 0.8994(3) 0.0453(12) Uani 1 d . . H56 H 0.3272(5) 0.4111(4) 0.9425(3) 0.054 Uiso 1 calc R . C66 C 0.4151(4) 0.4147(4) 0.8425(3) 0.0357(10) Uani 1 d . . C6 C 0.4156(6) 0.5196(4) 0.8428(4) 0.0531(14) Uani 1 d . . H6A H 0.3916(6) 0.5575(4) 0.8961(4) 0.080 Uiso 1 d R . H6B H 0.3486(6) 0.5055(4) 0.7860(4) 0.080 Uiso 1 d R . H6C H 0.5068(6) 0.5643(4) 0.8464(4) 0.080 Uiso 1 d R . N7R N 0.8614(3) 0.0997(3) 0.5764(2) 0.0271(7) Uani 1 d . . H7R H 0.8461(3) 0.1182(3) 0.6298(2) 0.033 Uiso 1 calc R . C27 C 0.7539(4) 0.0261(3) 0.5001(3) 0.0253(9) Uani 1 d . . O7R O 0.6378(2) -0.0127(2) 0.5096(2) 0.0240(6) Uani 1 d . . C37 C 0.7810(4) -0.0020(3) 0.4148(3) 0.0274(9) Uani 1 d . . H37 H 0.7101(4) -0.0535(3) 0.3594(3) 0.033 Uiso 1 calc R . C47 C 0.9102(4) 0.0457(3) 0.4131(3) 0.0306(9) Uani 1 d . . H47 H 0.9278(4) 0.0276(3) 0.3558(3) 0.037 Uiso 1 calc R . C57 C 1.0169(4) 0.1205(3) 0.4940(3) 0.0320(10) Uani 1 d . . H57 H 1.1060(4) 0.1524(3) 0.4914(3) 0.038 Uiso 1 calc R . C67 C 0.9924(4) 0.1472(3) 0.5761(3) 0.0289(9) Uani 1 d . . C7 C 1.0950(4) 0.2239(4) 0.6678(3) 0.0395(11) Uani 1 d . . H7A H 1.0973(4) 0.1872(4) 0.7086(3) 0.059 Uiso 1 d R . H7B H 1.0699(4) 0.2852(4) 0.6944(3) 0.059 Uiso 1 d R . H7C H 1.1854(4) 0.2499(4) 0.6606(3) 0.059 Uiso 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 Ni1 0.0239(4) 0.0263(4) 0.0225(3) 0.0108(3) 0.0070(3) 0.0093(3) Ni2 0.0248(4) 0.0232(4) 0.0280(4) 0.0083(3) 0.0088(3) 0.0087(3) Na1 0.0270(8) 0.0290(8) 0.0264(8) 0.0116(7) 0.0080(7) 0.0128(7) Na2 0.0269(8) 0.0224(8) 0.0236(7) 0.0097(6) 0.0071(6) 0.0086(6) N1R 0.030(2) 0.033(2) 0.026(2) 0.010(2) 0.0077(15) 0.014(2) C21 0.027(2) 0.029(2) 0.027(2) 0.009(2) -0.004(2) 0.010(2) O1R 0.0302(15) 0.030(2) 0.028(2) 0.0145(13) 0.0086(12) 0.0099(12) C31 0.044(3) 0.029(3) 0.047(3) 0.013(2) -0.003(2) 0.008(2) C41 0.060(3) 0.030(3) 0.051(3) -0.004(2) -0.010(3) 0.018(2) C51 0.050(3) 0.052(3) 0.035(3) 0.001(2) 0.004(2) 0.026(3) C61 0.040(2) 0.045(3) 0.027(2) 0.006(2) 0.008(2) 0.024(2) C1 0.068(3) 0.075(4) 0.036(3) 0.021(3) 0.033(3) 0.034(3) N2R 0.027(2) 0.034(2) 0.024(2) 0.013(2) 0.0091(15) 0.012(2) C22 0.028(2) 0.028(2) 0.024(2) 0.010(2) 0.011(2) 0.012(2) O2R 0.0260(14) 0.033(2) 0.0315(15) 0.0188(13) 0.0100(12) 0.0118(12) C32 0.026(2) 0.030(2) 0.032(2) 0.012(2) 0.007(2) 0.013(2) C42 0.030(2) 0.032(2) 0.038(2) 0.014(2) 0.016(2) 0.011(2) C52 0.042(3) 0.032(2) 0.031(2) 0.016(2) 0.020(2) 0.015(2) C62 0.037(2) 0.029(2) 0.026(2) 0.012(2) 0.012(2) 0.016(2) C2 0.047(3) 0.046(3) 0.032(2) 0.023(2) 0.011(2) 0.018(2) N3R 0.024(2) 0.027(2) 0.022(2) 0.0095(15) 0.0052(14) 0.0111(14) C23 0.028(2) 0.027(2) 0.027(2) 0.014(2) 0.010(2) 0.011(2) O3R 0.0267(14) 0.030(2) 0.0259(14) 0.0111(12) 0.0052(12) 0.0107(12) C33 0.036(2) 0.041(3) 0.034(2) 0.017(2) 0.014(2) 0.021(2) C43 0.038(3) 0.055(3) 0.049(3) 0.023(3) 0.011(2) 0.029(2) C53 0.032(2) 0.055(3) 0.038(3) 0.009(2) -0.006(2) 0.019(2) C63 0.032(2) 0.039(3) 0.030(2) 0.014(2) 0.006(2) 0.015(2) C3 0.044(3) 0.051(3) 0.031(2) -0.003(2) -0.013(2) 0.019(2) N4R 0.027(2) 0.029(2) 0.030(2) 0.008(2) 0.0055(15) 0.009(2) C24 0.025(2) 0.028(2) 0.033(2) 0.010(2) 0.006(2) 0.008(2) O4R 0.0263(15) 0.031(2) 0.033(2) 0.0023(13) 0.0084(13) 0.0075(13) C34 0.033(2) 0.039(3) 0.038(2) 0.015(2) 0.014(2) 0.017(2) C44 0.024(2) 0.048(3) 0.056(3) 0.025(3) 0.012(2) 0.012(2) C54 0.025(2) 0.038(3) 0.046(3) 0.013(2) 0.000(2) 0.001(2) C64 0.034(2) 0.031(2) 0.038(2) 0.012(2) 0.006(2) 0.008(2) C4 0.043(3) 0.040(3) 0.040(3) -0.002(2) 0.003(2) 0.009(2) N5R 0.035(2) 0.031(2) 0.034(2) 0.019(2) 0.021(2) 0.017(2) C25 0.031(2) 0.032(2) 0.028(2) 0.013(2) 0.016(2) 0.015(2) O5R 0.0255(14) 0.0205(15) 0.0322(15) 0.0114(12) 0.0102(12) 0.0090(11) C35 0.045(3) 0.049(3) 0.039(3) 0.019(2) 0.013(2) 0.029(2) C45 0.062(3) 0.061(4) 0.050(3) 0.036(3) 0.025(3) 0.040(3) C55 0.078(4) 0.037(3) 0.053(3) 0.028(2) 0.038(3) 0.036(3) C65 0.056(3) 0.028(2) 0.041(3) 0.021(2) 0.034(2) 0.020(2) C5 0.058(3) 0.026(2) 0.057(3) 0.018(2) 0.026(3) 0.009(2) N6R 0.028(2) 0.028(2) 0.032(2) 0.010(2) 0.007(2) 0.0124(15) C26 0.023(2) 0.025(2) 0.026(2) 0.010(2) 0.001(2) 0.008(2) O6R 0.0317(15) 0.028(2) 0.036(2) 0.0123(13) 0.0087(13) 0.0127(13) C36 0.041(2) 0.036(3) 0.035(2) 0.020(2) 0.004(2) 0.013(2) C46 0.047(3) 0.052(3) 0.040(3) 0.029(2) 0.016(2) 0.017(2) C56 0.056(3) 0.057(3) 0.037(3) 0.023(2) 0.025(2) 0.030(3) C66 0.038(2) 0.036(3) 0.032(2) 0.011(2) 0.010(2) 0.018(2) C6 0.079(4) 0.039(3) 0.056(3) 0.020(3) 0.035(3) 0.036(3) N7R 0.024(2) 0.030(2) 0.032(2) 0.016(2) 0.0120(15) 0.0114(15) C27 0.022(2) 0.026(2) 0.032(2) 0.017(2) 0.007(2) 0.011(2) O7R 0.0192(13) 0.0275(15) 0.0285(14) 0.0147(12) 0.0099(11) 0.0088(11) C37 0.031(2) 0.028(2) 0.030(2) 0.017(2) 0.011(2) 0.014(2) C47 0.034(2) 0.035(2) 0.036(2) 0.022(2) 0.019(2) 0.017(2) C57 0.024(2) 0.029(2) 0.049(3) 0.022(2) 0.014(2) 0.010(2) C67 0.020(2) 0.027(2) 0.041(2) 0.016(2) 0.009(2) 0.009(2) C7 0.026(2) 0.040(3) 0.045(3) 0.016(2) 0.008(2) 0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1R 2.043(3) . ? Ni1 N3R 2.061(3) . ? Ni1 N2R 2.096(3) . ? Ni1 O2R 2.107(3) . ? Ni1 O3R 2.114(3) . ? Ni1 O1R 2.144(3) . ? Ni2 N4R 2.067(3) . ? Ni2 N5R 2.074(3) . ? Ni2 N6R 2.088(3) . ? Ni2 O6R 2.108(3) . ? Ni2 O5R 2.117(3) . ? Ni2 O4R 2.149(3) . ? Na1 O6R 2.230(3) . ? Na1 O2R 2.325(3) . ? Na1 O7R 2.352(3) . ? Na1 O7R 2.367(3) 2_656 ? Na1 O1R 2.487(3) . ? Na2 O3R 2.269(3) 2_656 ? Na2 O4R 2.302(3) . ? Na2 O7R 2.327(3) 2_656 ? Na2 O5R 2.357(3) . ? Na2 O2R 2.542(3) 2_656 ? N1R C21 1.345(5) . ? N1R C61 1.353(5) . ? C21 O1R 1.309(5) . ? C21 C31 1.412(6) . ? C31 C41 1.376(8) . ? C41 C51 1.387(8) . ? C51 C61 1.349(7) . ? C61 C1 1.502(7) . ? N2R C62 1.346(5) . ? N2R C22 1.352(5) . ? C22 O2R 1.298(5) . ? C22 C32 1.417(6) . ? O2R Na2 2.542(3) 2_656 ? C32 C42 1.375(6) . ? C42 C52 1.384(6) . ? C52 C62 1.380(6) . ? C62 C2 1.499(6) . ? N3R C63 1.334(5) . ? N3R C23 1.354(5) . ? C23 O3R 1.287(5) . ? C23 C33 1.413(6) . ? O3R Na2 2.269(3) 2_656 ? C33 C43 1.372(6) . ? C43 C53 1.383(7) . ? C53 C63 1.386(6) . ? C63 C3 1.502(6) . ? N4R C64 1.340(5) . ? N4R C24 1.357(5) . ? C24 O4R 1.296(5) . ? C24 C34 1.411(6) . ? C34 C44 1.364(6) . ? C44 C54 1.394(7) . ? C54 C64 1.388(6) . ? C64 C4 1.503(6) . ? N5R C25 1.340(5) . ? N5R C65 1.356(5) . ? C25 O5R 1.313(5) . ? C25 C35 1.405(6) . ? C35 C45 1.381(7) . ? C45 C55 1.393(7) . ? C55 C65 1.374(7) . ? C65 C5 1.499(7) . ? N6R C66 1.344(5) . ? N6R C26 1.360(5) . ? C26 O6R 1.295(5) . ? C26 C36 1.405(6) . ? C36 C46 1.369(7) . ? C46 C56 1.401(7) . ? C56 C66 1.380(7) . ? C66 C6 1.500(6) . ? N7R C27 1.362(5) . ? N7R C67 1.377(5) . ? C27 O7R 1.273(4) . ? C27 C37 1.419(6) . ? O7R Na2 2.327(3) 2_656 ? O7R Na1 2.367(3) 2_656 ? C37 C47 1.369(6) . ? C47 C57 1.399(6) . ? C57 C67 1.358(6) . ? C67 C7 1.489(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 N1R Ni1 N3R 101.33(13) . . ? N1R Ni1 N2R 105.25(13) . . ? N3R Ni1 N2R 109.91(13) . . ? N1R Ni1 O2R 102.72(12) . . ? N3R Ni1 O2R 155.94(12) . . ? N2R Ni1 O2R 64.00(12) . . ? N1R Ni1 O3R 161.27(12) . . ? N3R Ni1 O3R 64.01(12) . . ? N2R Ni1 O3R 91.30(12) . . ? O2R Ni1 O3R 92.30(11) . . ? N1R Ni1 O1R 63.73(13) . . ? N3R Ni1 O1R 96.78(12) . . ? N2R Ni1 O1R 152.95(12) . . ? O2R Ni1 O1R 93.25(11) . . ? O3R Ni1 O1R 104.77(11) . . ? N4R Ni2 N5R 101.93(14) . . ? N4R Ni2 N6R 112.80(14) . . ? N5R Ni2 N6R 103.59(13) . . ? N4R Ni2 O6R 100.83(13) . . ? N5R Ni2 O6R 156.99(12) . . ? N6R Ni2 O6R 64.03(12) . . ? N4R Ni2 O5R 150.31(12) . . ? N5R Ni2 O5R 64.06(12) . . ? N6R Ni2 O5R 96.35(12) . . ? O6R Ni2 O5R 96.84(11) . . ? N4R Ni2 O4R 63.89(12) . . ? N5R Ni2 O4R 102.73(12) . . ? N6R Ni2 O4R 153.52(13) . . ? O6R Ni2 O4R 90.22(12) . . ? O5R Ni2 O4R 92.56(11) . . ? O6R Na1 O2R 109.58(12) . . ? O6R Na1 O7R 162.87(12) . . ? O2R Na1 O7R 87.14(11) . . ? O6R Na1 O7R 99.38(11) . 2_656 ? O2R Na1 O7R 97.08(11) . 2_656 ? O7R Na1 O7R 81.58(10) . 2_656 ? O6R Na1 O1R 93.20(11) . . ? O2R Na1 O1R 79.85(11) . . ? O7R Na1 O1R 85.98(10) . . ? O7R Na1 O1R 167.34(11) 2_656 . ? O3R Na2 O4R 151.37(13) 2_656 . ? O3R Na2 O7R 105.42(11) 2_656 2_656 ? O4R Na2 O7R 102.47(12) . 2_656 ? O3R Na2 O5R 98.73(11) 2_656 . ? O4R Na2 O5R 82.84(11) . . ? O7R Na2 O5R 99.39(10) 2_656 . ? O3R Na2 O2R 78.29(10) 2_656 2_656 ? O4R Na2 O2R 99.12(11) . 2_656 ? O7R Na2 O2R 82.79(10) 2_656 2_656 ? O5R Na2 O2R 176.72(11) . 2_656 ? C21 N1R C61 120.6(4) . . ? C21 N1R Ni1 93.0(2) . . ? C61 N1R Ni1 145.2(3) . . ? O1R C21 N1R 112.9(4) . . ? O1R C21 C31 126.5(4) . . ? N1R C21 C31 120.6(4) . . ? C21 O1R Ni1 89.6(2) . . ? C21 O1R Na1 107.1(2) . . ? Ni1 O1R Na1 90.66(11) . . ? C41 C31 C21 117.4(5) . . ? C31 C41 C51 120.8(5) . . ? C61 C51 C41 119.5(5) . . ? C51 C61 N1R 121.1(5) . . ? C51 C61 C1 123.8(4) . . ? N1R C61 C1 115.1(4) . . ? C62 N2R C22 121.1(4) . . ? C62 N2R Ni1 148.5(3) . . ? C22 N2R Ni1 90.3(2) . . ? O2R C22 N2R 114.3(3) . . ? O2R C22 C32 125.3(4) . . ? N2R C22 C32 120.4(4) . . ? C22 O2R Ni1 91.3(2) . . ? C22 O2R Na1 160.9(2) . . ? Ni1 O2R Na1 96.22(11) . . ? C22 O2R Na2 105.1(2) . 2_656 ? Ni1 O2R Na2 89.21(10) . 2_656 ? Na1 O2R Na2 92.49(10) . 2_656 ? C42 C32 C22 117.5(4) . . ? C32 C42 C52 121.3(4) . . ? C62 C52 C42 118.9(4) . . ? N2R C62 C52 120.7(4) . . ? N2R C62 C2 116.1(4) . . ? C52 C62 C2 123.1(4) . . ? C63 N3R C23 121.9(3) . . ? C63 N3R Ni1 147.0(3) . . ? C23 N3R Ni1 91.1(2) . . ? O3R C23 N3R 113.9(3) . . ? O3R C23 C33 126.6(4) . . ? N3R C23 C33 119.5(4) . . ? C23 O3R Ni1 90.7(2) . . ? C23 O3R Na2 169.3(2) . 2_656 ? Ni1 O3R Na2 96.79(11) . 2_656 ? C43 C33 C23 118.2(4) . . ? C33 C43 C53 120.8(4) . . ? C43 C53 C63 119.0(4) . . ? N3R C63 C53 120.3(4) . . ? N3R C63 C3 117.7(4) . . ? C53 C63 C3 121.9(4) . . ? C64 N4R C24 122.0(4) . . ? C64 N4R Ni2 146.0(3) . . ? C24 N4R Ni2 91.7(2) . . ? O4R C24 N4R 114.5(3) . . ? O4R C24 C34 125.9(4) . . ? N4R C24 C34 119.6(4) . . ? C24 O4R Ni2 89.8(2) . . ? C24 O4R Na2 168.4(3) . . ? Ni2 O4R Na2 91.93(11) . . ? C44 C34 C24 118.6(4) . . ? C34 C44 C54 120.8(4) . . ? C64 C54 C44 119.0(4) . . ? N4R C64 C54 120.0(4) . . ? N4R C64 C4 117.5(4) . . ? C54 C64 C4 122.5(4) . . ? C25 N5R C65 121.0(4) . . ? C25 N5R Ni2 91.4(2) . . ? C65 N5R Ni2 147.4(3) . . ? O5R C25 N5R 113.8(4) . . ? O5R C25 C35 125.2(4) . . ? N5R C25 C35 120.9(4) . . ? C25 O5R Ni2 90.3(2) . . ? C25 O5R Na2 116.4(2) . . ? Ni2 O5R Na2 91.22(10) . . ? C45 C35 C25 117.8(5) . . ? C35 C45 C55 120.6(5) . . ? C65 C55 C45 119.0(4) . . ? N5R C65 C55 120.6(4) . . ? N5R C65 C5 116.6(4) . . ? C55 C65 C5 122.8(4) . . ? C66 N6R C26 120.5(4) . . ? C66 N6R Ni2 148.3(3) . . ? C26 N6R Ni2 90.5(2) . . ? O6R C26 N6R 113.8(3) . . ? O6R C26 C36 125.4(4) . . ? N6R C26 C36 120.8(4) . . ? C26 O6R Ni2 91.4(2) . . ? C26 O6R Na1 154.5(3) . . ? Ni2 O6R Na1 112.71(13) . . ? C46 C36 C26 118.1(4) . . ? C36 C46 C56 120.8(4) . . ? C66 C56 C46 118.5(4) . . ? N6R C66 C56 121.2(4) . . ? N6R C66 C6 116.1(4) . . ? C56 C66 C6 122.6(4) . . ? C27 N7R C67 124.7(4) . . ? O7R C27 N7R 118.6(3) . . ? O7R C27 C37 124.7(4) . . ? N7R C27 C37 116.6(3) . . ? C27 O7R Na2 119.3(2) . 2_656 ? C27 O7R Na1 123.1(2) . . ? Na2 O7R Na1 97.51(11) 2_656 . ? C27 O7R Na1 118.3(2) . 2_656 ? Na2 O7R Na1 94.32(11) 2_656 2_656 ? Na1 O7R Na1 98.42(10) . 2_656 ? C47 C37 C27 119.5(4) . . ? C37 C47 C57 121.4(4) . . ? C67 C57 C47 119.7(4) . . ? C57 C67 N7R 118.2(4) . . ? C57 C67 C7 126.1(4) . . ? N7R C67 C7 115.7(4) . . ? _refine_diff_density_max 0.403 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.078 #==END data_nifnaf _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38 H32 Cl6 N10 Na2 Ni2 O7' _chemical_formula_weight 1116.84 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M I2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 15.667(2) _cell_length_b 9.1628(5) _cell_length_c 16.4418(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.525(10) _cell_angle_gamma 90.00 _cell_volume 2360.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 220.0(2) _cell_measurement_reflns_used 68 _cell_measurement_theta_min 20 _cell_measurement_theta_max 22 _exptl_crystal_description block _exptl_crystal_colour Green _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_method ? _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 4.791 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.359 _exptl_absorpt_correction_T_max 0.541 _exptl_special_details ; ? ; _diffrn_ambient_temperature 220.0(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method omega-theta _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3932 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.88 _diffrn_reflns_theta_max 60.10 _reflns_number_total 2929 _reflns_number_observed 2751 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0633P)^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 ? _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 0.04(2) _refine_ls_number_reflns 2928 _refine_ls_number_parameters 294 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_obs 0.0338 _refine_ls_wR_factor_all 0.0882 _refine_ls_wR_factor_obs 0.0850 _refine_ls_goodness_of_fit_all 1.038 _refine_ls_goodness_of_fit_obs 1.053 _refine_ls_restrained_S_all 1.056 _refine_ls_restrained_S_obs 1.053 _refine_ls_shift/esd_max 0.198 _refine_ls_shift/esd_mean 0.018 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni -0.21028(4) -0.38192(8) -0.00157(4) 0.0234(2) Uani 1 d . . Na1 Na 0.01202(10) -0.4894(2) 0.09989(9) 0.0326(4) Uani 1 d . . O1W O 0.0000 -0.3082(5) 0.0000 0.0311(9) Uani 1 d S . H1W H -0.0455 -0.2515(5) 0.0107 0.037 Uiso 1 d R . N1R N -0.2662(2) -0.3043(4) 0.1046(2) 0.0260(8) Uani 1 d . . C21 C -0.2043(3) -0.2014(5) 0.1134(2) 0.0264(9) Uani 1 d . . C31 C -0.2047(3) -0.1092(6) 0.1807(3) 0.0385(12) Uani 1 d . . H31 H -0.1615(3) -0.0389(6) 0.1877(3) 0.046 Uiso 1 calc R . C41 C -0.2685(3) -0.1218(6) 0.2365(3) 0.0443(13) Uani 1 d . . H41 H -0.2687(3) -0.0607(6) 0.2824(3) 0.053 Uiso 1 calc R . C51 C -0.3331(3) -0.2244(6) 0.2257(3) 0.0388(12) Uani 1 d . . H51 H -0.3780(3) -0.2335(6) 0.2630(3) 0.047 Uiso 1 calc R . C61 C -0.3282(3) -0.3116(5) 0.1581(2) 0.0279(10) Uani 1 d . . O1R O -0.1499(2) -0.2010(4) 0.0543(2) 0.0311(7) Uani 1 d . . Cl1 Cl -0.40629(7) -0.44201(15) 0.13900(8) 0.0458(3) Uani 1 d . . N2R N -0.2532(2) -0.5908(4) -0.0143(2) 0.0265(8) Uani 1 d . . C22 C -0.1802(3) -0.6490(5) 0.0195(2) 0.0295(10) Uani 1 d . . C32 C -0.1696(3) -0.7983(5) 0.0218(3) 0.0363(11) Uani 1 d . . H32 H -0.1210(3) -0.8394(5) 0.0468(3) 0.044 Uiso 1 calc R . C42 C -0.2314(3) -0.8868(6) -0.0132(2) 0.0371(10) Uani 1 d . . H42 H -0.2239(3) -0.9886(6) -0.0128(2) 0.045 Uiso 1 calc R . C52 C -0.3038(3) -0.8280(5) -0.0486(2) 0.0340(11) Uani 1 d . . H52 H -0.3457(3) -0.8872(5) -0.0733(2) 0.041 Uiso 1 calc R . C62 C -0.3116(2) -0.6800(5) -0.0461(2) 0.0266(10) Uani 1 d . . O2R O -0.1280(2) -0.5494(4) 0.0455(2) 0.0363(8) Uani 1 d . . Cl2 Cl -0.40112(7) -0.59390(14) -0.08726(8) 0.0447(3) Uani 1 d . . N3R N -0.2713(2) -0.2766(4) -0.0965(2) 0.0252(8) Uani 1 d . . C23 C -0.2081(2) -0.3144(5) -0.1489(2) 0.0250(9) Uani 1 d . . C33 C -0.2136(3) -0.2722(5) -0.2309(3) 0.0344(11) Uani 1 d . . H33 H -0.1706(3) -0.2979(5) -0.2677(3) 0.041 Uiso 1 calc R . C43 C -0.2828(3) -0.1930(6) -0.2561(3) 0.0424(13) Uani 1 d . . H43 H -0.2866(3) -0.1626(6) -0.3106(3) 0.051 Uiso 1 calc R . C53 C -0.3484(3) -0.1561(6) -0.2022(3) 0.0390(12) Uani 1 d . . H53 H -0.3966(3) -0.1026(6) -0.2190(3) 0.047 Uiso 1 calc R . C63 C -0.3379(2) -0.2025(5) -0.1242(2) 0.0275(9) Uani 1 d . . O3R O -0.1479(2) -0.3879(4) -0.11449(15) 0.0307(6) Uani 1 d . . Cl3 Cl -0.41721(7) -0.16876(13) -0.05272(7) 0.0397(3) Uani 1 d . . N1A N 0.0330(3) -0.3932(7) -0.2307(3) 0.0607(12) Uani 1 d . . C2A C 0.0605(3) -0.3778(7) -0.2922(3) 0.0458(12) Uani 1 d . . C3A C 0.0977(4) -0.3576(8) -0.3724(3) 0.069(2) Uani 1 d . . H3A1 H 0.1548(4) -0.3178(8) -0.3665(3) 0.103 Uiso 1 d R . H3A2 H 0.0626(4) -0.2908(8) -0.4039(3) 0.103 Uiso 1 d R . H3A3 H 0.1005(4) -0.4509(8) -0.4001(3) 0.103 Uiso 1 d R . N1B N 0.0270(3) -0.7504(6) 0.1357(3) 0.0496(12) Uani 1 d . . C2B C 0.0421(3) -0.8673(8) 0.1479(3) 0.0490(13) Uani 1 d . . C3B C 0.0626(6) -1.0183(9) 0.1639(6) 0.108(3) Uani 1 d . . H3B1 H 0.0113(6) -1.0700(9) 0.1798(6) 0.162 Uiso 1 d R . H3B2 H 0.1046(6) -1.0240(9) 0.2074(6) 0.162 Uiso 1 d R . H3B3 H 0.0855(6) -1.0625(9) 0.1151(6) 0.162 Uiso 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 Ni1 0.0205(3) 0.0229(4) 0.0266(3) -0.0004(3) -0.0034(3) 0.0009(3) Na1 0.0279(9) 0.0367(11) 0.0332(9) 0.0040(8) -0.0061(7) -0.0041(7) O1W 0.016(2) 0.036(3) 0.041(2) 0.000 -0.001(2) 0.000 N1R 0.026(2) 0.024(2) 0.028(2) 0.0002(15) -0.0031(14) -0.001(2) C21 0.026(2) 0.025(3) 0.028(2) 0.000(2) -0.004(2) 0.007(2) C31 0.031(3) 0.038(3) 0.046(3) -0.011(2) -0.004(2) 0.001(2) C41 0.057(3) 0.039(3) 0.037(3) -0.011(2) 0.000(2) 0.008(3) C51 0.037(3) 0.046(4) 0.033(2) -0.003(2) 0.005(2) 0.005(2) C61 0.026(2) 0.025(2) 0.032(2) 0.006(2) -0.004(2) 0.001(2) O1R 0.027(2) 0.031(2) 0.036(2) -0.0040(14) 0.0011(13) -0.0003(14) Cl1 0.0332(6) 0.0524(8) 0.0518(7) 0.0047(5) 0.0005(5) -0.0160(5) N2R 0.023(2) 0.027(2) 0.029(2) -0.001(2) -0.0044(14) 0.006(2) C22 0.029(2) 0.028(3) 0.031(2) 0.004(2) -0.004(2) 0.000(2) C32 0.040(3) 0.026(3) 0.043(2) 0.008(2) -0.010(2) 0.004(2) C42 0.051(3) 0.020(2) 0.040(2) 0.007(2) 0.006(2) -0.002(3) C52 0.038(3) 0.031(3) 0.032(2) 0.000(2) 0.001(2) -0.009(2) C62 0.023(2) 0.031(3) 0.026(2) -0.001(2) -0.001(2) -0.007(2) O2R 0.030(2) 0.026(2) 0.053(2) 0.0022(15) -0.0195(15) -0.0013(14) Cl2 0.0277(6) 0.0480(8) 0.0581(7) -0.0035(6) -0.0181(5) -0.0006(5) N3R 0.024(2) 0.021(2) 0.031(2) 0.0013(15) -0.0029(14) -0.001(2) C23 0.017(2) 0.029(2) 0.028(2) -0.002(2) 0.001(2) -0.006(2) C33 0.030(2) 0.045(3) 0.028(2) -0.003(2) 0.002(2) -0.003(2) C43 0.044(3) 0.057(4) 0.025(2) 0.006(2) -0.004(2) 0.003(3) C53 0.035(2) 0.044(3) 0.038(3) 0.007(2) -0.013(2) 0.006(2) C63 0.017(2) 0.031(3) 0.034(2) -0.003(2) 0.000(2) 0.001(2) O3R 0.0228(14) 0.039(2) 0.0304(14) -0.0008(15) -0.0006(11) 0.006(2) Cl3 0.0272(6) 0.0401(8) 0.0518(7) -0.0017(6) 0.0093(5) 0.0064(5) N1A 0.056(3) 0.078(4) 0.048(3) 0.004(3) 0.014(2) 0.004(3) C2A 0.047(3) 0.046(3) 0.045(3) 0.003(3) 0.010(2) 0.005(3) C3A 0.091(4) 0.065(5) 0.051(3) 0.011(3) 0.020(3) 0.010(4) N1B 0.043(2) 0.049(4) 0.057(3) 0.003(2) -0.009(2) 0.007(2) C2B 0.042(3) 0.042(4) 0.063(3) 0.005(3) -0.006(2) 0.008(3) C3B 0.125(7) 0.056(5) 0.142(8) 0.034(5) 0.017(6) 0.036(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1R 2.115(3) . ? Ni1 O2R 2.144(3) . ? Ni1 O3R 2.107(3) . ? Ni1 N1R 2.086(3) . ? Ni1 N2R 2.038(4) . ? Ni1 N3R 2.062(3) . ? Na1 O1W 2.342(4) . ? Na1 O2R 2.425(3) . ? Na1 O3R 2.334(3) 2 ? Na1 N1A 2.434(5) 2 ? Na1 N1B 2.473(6) . ? N1R C21 1.360(5) . ? N1R C61 1.318(5) . ? C21 O1R 1.298(5) . ? C21 C31 1.391(6) . ? C31 C41 1.368(7) . ? C41 C51 1.392(7) . ? C51 C61 1.372(6) . ? C61 Cl1 1.737(4) . ? N2R C22 1.374(5) . ? N2R C62 1.331(5) . ? C22 O2R 1.295(5) . ? C22 C32 1.379(7) . ? C32 C42 1.384(7) . ? C42 C52 1.381(6) . ? C52 C62 1.362(6) . ? C62 Cl2 1.740(4) . ? N3R C23 1.364(5) . ? N3R C63 1.322(5) . ? C23 O3R 1.285(5) . ? C23 C33 1.405(6) . ? C33 C43 1.365(6) . ? C43 C53 1.405(7) . ? C53 C63 1.359(6) . ? C63 Cl3 1.746(4) . ? N1A C2A 1.112(6) . ? C2A C3A 1.458(7) . ? N1B C2B 1.115(7) . ? C2B C3B 1.444(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2R Ni1 N3R 102.20(13) . . ? N2R Ni1 N1R 105.42(14) . . ? N3R Ni1 N1R 106.17(13) . . ? N2R Ni1 O3R 92.28(14) . . ? N3R Ni1 O3R 63.95(12) . . ? N1R Ni1 O3R 161.52(14) . . ? N2R Ni1 O1R 157.89(12) . . ? N3R Ni1 O1R 99.46(13) . . ? N1R Ni1 O1R 63.80(13) . . ? O3R Ni1 O1R 101.20(12) . . ? N2R Ni1 O2R 63.99(12) . . ? N3R Ni1 O2R 151.75(13) . . ? N1R Ni1 O2R 101.42(13) . . ? O3R Ni1 O2R 90.98(13) . . ? O1R Ni1 O2R 98.02(11) . . ? O3R Na1 O1W 81.78(10) 2 . ? O3R Na1 O2R 161.77(13) 2 . ? O1W Na1 O2R 80.52(10) . . ? O3R Na1 N1A 92.08(14) 2 2 ? O1W Na1 N1A 109.9(2) . 2 ? O2R Na1 N1A 98.03(15) . 2 ? O3R Na1 N1B 106.03(14) 2 . ? O1W Na1 N1B 149.2(2) . . ? O2R Na1 N1B 87.27(14) . . ? N1A Na1 N1B 99.6(2) 2 . ? Na1 O1W Na1 89.7(2) 2 . ? C61 N1R C21 119.6(4) . . ? C61 N1R Ni1 149.2(3) . . ? C21 N1R Ni1 91.2(2) . . ? O1R C21 N1R 113.3(4) . . ? O1R C21 C31 126.9(4) . . ? N1R C21 C31 119.8(4) . . ? C41 C31 C21 119.4(5) . . ? C31 C41 C51 120.4(5) . . ? C61 C51 C41 116.7(4) . . ? N1R C61 C51 124.0(4) . . ? N1R C61 Cl1 115.9(3) . . ? C51 C61 Cl1 120.2(3) . . ? C21 O1R Ni1 91.7(2) . . ? C62 N2R C22 119.2(4) . . ? C62 N2R Ni1 147.4(3) . . ? C22 N2R Ni1 92.9(3) . . ? O2R C22 N2R 112.3(4) . . ? O2R C22 C32 127.9(4) . . ? N2R C22 C32 119.8(4) . . ? C22 C32 C42 119.1(4) . . ? C52 C42 C32 121.1(5) . . ? C62 C52 C42 116.7(4) . . ? N2R C62 C52 124.2(4) . . ? N2R C62 Cl2 115.0(3) . . ? C52 C62 Cl2 120.8(3) . . ? C22 O2R Ni1 90.6(2) . . ? C22 O2R Na1 148.0(3) . . ? Ni1 O2R Na1 120.64(15) . . ? C63 N3R C23 119.2(3) . . ? C63 N3R Ni1 149.3(3) . . ? C23 N3R Ni1 91.4(2) . . ? O3R C23 N3R 112.9(3) . . ? O3R C23 C33 127.3(4) . . ? N3R C23 C33 119.8(4) . . ? C43 C33 C23 118.7(4) . . ? C33 C43 C53 121.3(4) . . ? C63 C53 C43 115.9(4) . . ? N3R C63 C53 125.0(4) . . ? N3R C63 Cl3 115.0(3) . . ? C53 C63 Cl3 119.9(3) . . ? C23 O3R Ni1 91.7(2) . . ? C23 O3R Na1 156.7(2) . 2 ? Ni1 O3R Na1 110.47(12) . 2 ? C2A N1A Na1 165.3(6) . 2 ? N1A C2A C3A 179.2(6) . . ? C2B N1B Na1 172.5(4) . . ? N1B C2B C3B 179.4(7) . . ? 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 O3R Na1 O1W Na1 115.20(10) 2 . . 2 ? O2R Na1 O1W Na1 -60.41(9) . . . 2 ? N1A Na1 O1W Na1 -155.57(15) 2 . . 2 ? N1B Na1 O1W Na1 7.6(2) . . . 2 ? N2R Ni1 N1R C61 -23.8(6) . . . . ? N3R Ni1 N1R C61 84.2(6) . . . . ? O3R Ni1 N1R C61 139.1(5) . . . . ? O1R Ni1 N1R C61 176.9(6) . . . . ? O2R Ni1 N1R C61 -89.7(6) . . . . ? N2R Ni1 N1R C21 157.5(2) . . . . ? N3R Ni1 N1R C21 -94.5(2) . . . . ? O3R Ni1 N1R C21 -39.6(5) . . . . ? O1R Ni1 N1R C21 -1.8(2) . . . . ? O2R Ni1 N1R C21 91.6(2) . . . . ? C61 N1R C21 O1R -176.4(4) . . . . ? Ni1 N1R C21 O1R 2.8(3) . . . . ? C61 N1R C21 C31 2.9(6) . . . . ? Ni1 N1R C21 C31 -177.8(4) . . . . ? O1R C21 C31 C41 178.1(4) . . . . ? N1R C21 C31 C41 -1.1(7) . . . . ? C21 C31 C41 C51 -0.8(7) . . . . ? C31 C41 C51 C61 1.0(7) . . . . ? C21 N1R C61 C51 -2.8(6) . . . . ? Ni1 N1R C61 C51 178.7(4) . . . . ? C21 N1R C61 Cl1 177.5(3) . . . . ? Ni1 N1R C61 Cl1 -1.0(7) . . . . ? C41 C51 C61 N1R 0.8(7) . . . . ? C41 C51 C61 Cl1 -179.5(4) . . . . ? N1R C21 O1R Ni1 -2.7(3) . . . . ? C31 C21 O1R Ni1 177.9(4) . . . . ? N2R Ni1 O1R C21 -63.1(4) . . . . ? N3R Ni1 O1R C21 105.3(2) . . . . ? N1R Ni1 O1R C21 1.8(2) . . . . ? O3R Ni1 O1R C21 170.4(2) . . . . ? O2R Ni1 O1R C21 -97.0(2) . . . . ? N3R Ni1 N2R C62 -18.5(5) . . . . ? N1R Ni1 N2R C62 92.3(5) . . . . ? O3R Ni1 N2R C62 -82.3(5) . . . . ? O1R Ni1 N2R C62 149.8(4) . . . . ? O2R Ni1 N2R C62 -172.3(5) . . . . ? N3R Ni1 N2R C22 151.2(2) . . . . ? N1R Ni1 N2R C22 -98.0(2) . . . . ? O3R Ni1 N2R C22 87.4(2) . . . . ? O1R Ni1 N2R C22 -40.5(4) . . . . ? O2R Ni1 N2R C22 -2.6(2) . . . . ? C62 N2R C22 O2R 177.8(3) . . . . ? Ni1 N2R C22 O2R 4.2(4) . . . . ? C62 N2R C22 C32 -1.4(6) . . . . ? Ni1 N2R C22 C32 -175.1(4) . . . . ? O2R C22 C32 C42 -176.6(4) . . . . ? N2R C22 C32 C42 2.5(6) . . . . ? C22 C32 C42 C52 -1.3(7) . . . . ? C32 C42 C52 C62 -1.0(6) . . . . ? C22 N2R C62 C52 -1.0(6) . . . . ? Ni1 N2R C62 C52 167.2(4) . . . . ? C22 N2R C62 Cl2 -180.0(3) . . . . ? Ni1 N2R C62 Cl2 -11.8(6) . . . . ? C42 C52 C62 N2R 2.2(6) . . . . ? C42 C52 C62 Cl2 -178.9(3) . . . . ? N2R C22 O2R Ni1 -3.9(3) . . . . ? C32 C22 O2R Ni1 175.2(4) . . . . ? N2R C22 O2R Na1 -171.6(4) . . . . ? C32 C22 O2R Na1 7.6(9) . . . . ? N2R Ni1 O2R C22 2.7(2) . . . . ? N3R Ni1 O2R C22 -63.0(4) . . . . ? N1R Ni1 O2R C22 104.5(3) . . . . ? O3R Ni1 O2R C22 -89.3(3) . . . . ? O1R Ni1 O2R C22 169.2(3) . . . . ? N2R Ni1 O2R Na1 175.2(2) . . . . ? N3R Ni1 O2R Na1 109.5(3) . . . . ? N1R Ni1 O2R Na1 -83.1(2) . . . . ? O3R Ni1 O2R Na1 83.1(2) . . . . ? O1R Ni1 O2R Na1 -18.3(2) . . . . ? O3R Na1 O2R C22 119.8(6) 2 . . . ? O1W Na1 O2R C22 133.8(6) . . . . ? N1A Na1 O2R C22 -117.2(6) 2 . . . ? N1B Na1 O2R C22 -17.9(6) . . . . ? O3R Na1 O2R Ni1 -45.9(5) 2 . . . ? O1W Na1 O2R Ni1 -31.9(2) . . . . ? N1A Na1 O2R Ni1 77.1(2) 2 . . . ? N1B Na1 O2R Ni1 176.5(2) . . . . ? Na1 N1A C2A C3A -73.8(526) 2 . . . ? N2R Ni1 N3R C63 90.8(6) . . . . ? N1R Ni1 N3R C63 -19.5(6) . . . . ? O3R Ni1 N3R C63 177.3(6) . . . . ? O1R Ni1 N3R C63 -84.8(6) . . . . ? O2R Ni1 N3R C63 147.7(5) . . . . ? N2R Ni1 N3R C23 -86.0(2) . . . . ? N1R Ni1 N3R C23 163.8(2) . . . . ? O3R Ni1 N3R C23 0.6(2) . . . . ? O1R Ni1 N3R C23 98.5(2) . . . . ? O2R Ni1 N3R C23 -29.0(4) . . . . ? C63 N3R C23 O3R -179.0(4) . . . . ? Ni1 N3R C23 O3R -0.9(4) . . . . ? C63 N3R C23 C33 1.2(6) . . . . ? Ni1 N3R C23 C33 179.3(4) . . . . ? O3R C23 C33 C43 -179.6(5) . . . . ? N3R C23 C33 C43 0.3(7) . . . . ? C23 C33 C43 C53 -1.2(8) . . . . ? C33 C43 C53 C63 0.7(8) . . . . ? C23 N3R C63 C53 -1.7(7) . . . . ? Ni1 N3R C63 C53 -178.0(4) . . . . ? C23 N3R C63 Cl3 176.8(3) . . . . ? Ni1 N3R C63 Cl3 0.5(8) . . . . ? C43 C53 C63 N3R 0.8(8) . . . . ? C43 C53 C63 Cl3 -177.6(4) . . . . ? N3R C23 O3R Ni1 0.9(4) . . . . ? C33 C23 O3R Ni1 -179.3(4) . . . . ? N3R C23 O3R Na1 -162.1(6) . . . 2 ? C33 C23 O3R Na1 17.8(11) . . . 2 ? N2R Ni1 O3R C23 101.9(3) . . . . ? N3R Ni1 O3R C23 -0.6(2) . . . . ? N1R Ni1 O3R C23 -61.6(4) . . . . ? O1R Ni1 O3R C23 -95.7(3) . . . . ? O2R Ni1 O3R C23 165.9(3) . . . . ? N2R Ni1 O3R Na1 -85.2(2) . . . 2 ? N3R Ni1 O3R Na1 172.3(2) . . . 2 ? N1R Ni1 O3R Na1 111.3(4) . . . 2 ? O1R Ni1 O3R Na1 77.2(2) . . . 2 ? O2R Ni1 O3R Na1 -21.2(2) . . . 2 ? O3R Na1 N1B C2B -36.5(34) 2 . . . ? O1W Na1 N1B C2B 64.6(34) . . . . ? O2R Na1 N1B C2B 130.8(34) . . . . ? N1A Na1 N1B C2B -131.5(34) 2 . . . ? Na1 N1B C2B C3B 33.3(621) . . . . ? _refine_diff_density_max 0.238 _refine_diff_density_min -0.483 _refine_diff_density_rms 0.059 #==END data_ni3bzx _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C38 H34 N10 O8 Cl6 Na2 Ni2 + C38 H32 N10 O7 Cl6 Na2 Ni2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C76 H66 Cl12 N20 Na4 Ni4 O15' _chemical_formula_weight 2251.69 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 16.4177(15) _cell_length_b 9.1699(5) _cell_length_c 31.597(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.096(11) _cell_angle_gamma 90.00 _cell_volume 4756.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 220.0(2) _cell_measurement_reflns_used 58 _cell_measurement_theta_min 20 _cell_measurement_theta_max 22 _exptl_crystal_description block _exptl_crystal_colour Green _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_method ? _exptl_crystal_F_000 2284 _exptl_absorpt_coefficient_mu 4.768 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.338 _exptl_absorpt_correction_T_max 0.516 _exptl_special_details ; ? ; _diffrn_ambient_temperature 220.0(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method Omega _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8871 _diffrn_reflns_av_R_equivalents 0.1109 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 60.09 _reflns_number_total 6939 _reflns_number_observed 4801 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+8.0415P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6889 _refine_ls_number_parameters 591 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0892 _refine_ls_R_factor_obs 0.0532 _refine_ls_wR_factor_all 0.1268 _refine_ls_wR_factor_obs 0.1019 _refine_ls_goodness_of_fit_all 1.052 _refine_ls_goodness_of_fit_obs 1.073 _refine_ls_restrained_S_all 1.090 _refine_ls_restrained_S_obs 1.073 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni -0.00165(5) -0.47565(9) -0.64523(3) 0.0312(2) Uani 1 d . . Na1 Na -0.10100(12) -0.3714(2) -0.75831(6) 0.0405(5) Uani 1 d . . O1W O 0.0000 -0.5478(6) -0.7500 0.0405(13) Uani 1 d S . H1W H -0.0163 -0.6078(6) -0.7266 0.049 Uiso 1 d R . N1R N 0.0126(2) -0.2653(5) -0.62474(13) 0.0328(10) Uani 1 d . . C21 C -0.0220(3) -0.2106(6) -0.6606(2) 0.0385(14) Uani 1 d . . O1R O -0.0482(2) -0.3093(4) -0.68652(12) 0.0440(10) Uani 1 d . . C31 C -0.0251(3) -0.0575(6) -0.6664(2) 0.0419(14) Uani 1 d . . H31 H -0.0517(3) -0.0165(6) -0.6902(2) 0.050 Uiso 1 calc R . C41 C 0.0117(4) 0.0287(6) -0.6364(2) 0.049(2) Uani 1 d . . H41 H 0.0120(4) 0.1303(6) -0.6404(2) 0.059 Uiso 1 calc R . C51 C 0.0486(3) -0.0286(7) -0.6005(2) 0.0449(15) Uani 1 d . . H51 H 0.0741(3) 0.0311(7) -0.5800(2) 0.054 Uiso 1 calc R . C61 C 0.0458(3) -0.1774(6) -0.5963(2) 0.0361(13) Uani 1 d . . Cl1 Cl 0.08713(9) -0.2599(2) -0.55102(5) 0.0535(4) Uani 1 d . . N2R N -0.1083(2) -0.5508(5) -0.61980(13) 0.0326(10) Uani 1 d . . C22 C -0.1174(3) -0.6534(6) -0.6509(2) 0.0342(13) Uani 1 d . . O2R O -0.0562(2) -0.6571(4) -0.67639(11) 0.0367(9) Uani 1 d . . C32 C -0.1857(3) -0.7436(7) -0.6521(2) 0.047(2) Uani 1 d . . H32 H -0.1922(3) -0.8141(7) -0.6735(2) 0.057 Uiso 1 calc R . C42 C -0.2436(3) -0.7280(7) -0.6213(2) 0.052(2) Uani 1 d . . H42 H -0.2903(3) -0.7875(7) -0.6220(2) 0.062 Uiso 1 calc R . C52 C -0.2336(3) -0.6254(7) -0.5894(2) 0.047(2) Uani 1 d . . H52 H -0.2723(3) -0.6140(7) -0.5681(2) 0.057 Uiso 1 calc R . C62 C -0.1645(3) -0.5411(6) -0.5902(2) 0.0350(13) Uani 1 d . . Cl2 Cl -0.14484(9) -0.4163(2) -0.55023(5) 0.0540(4) Uani 1 d . . N3R N 0.0903(2) -0.5840(5) -0.61262(12) 0.0293(10) Uani 1 d . . C23 C 0.1448(3) -0.5480(6) -0.6433(2) 0.0348(13) Uani 1 d . . O3R O 0.1133(2) -0.4742(4) -0.67385(11) 0.0400(9) Uani 1 d . . C33 C 0.2265(3) -0.5922(7) -0.6390(2) 0.0406(14) Uani 1 d . . H33 H 0.2648(3) -0.5670(7) -0.6595(2) 0.049 Uiso 1 calc R . C43 C 0.2492(3) -0.6727(7) -0.6043(2) 0.051(2) Uani 1 d . . H43 H 0.3033(3) -0.7057(7) -0.6015(2) 0.061 Uiso 1 calc R . C53 C 0.1931(3) -0.7073(6) -0.5725(2) 0.0437(15) Uani 1 d . . H53 H 0.2082(3) -0.7615(6) -0.5483(2) 0.052 Uiso 1 calc R . C63 C 0.1161(3) -0.6576(6) -0.5789(2) 0.0327(12) Uani 1 d . . Cl3 Cl 0.04227(9) -0.6906(2) -0.54107(4) 0.0458(4) Uani 1 d . . N1A N -0.2347(3) -0.4578(7) -0.7373(2) 0.071(2) Uani 1 d . . C2A C -0.2951(4) -0.4706(7) -0.7222(2) 0.055(2) Uani 1 d . . C3A C -0.3748(4) -0.4839(9) -0.7031(2) 0.076(2) Uani 1 d . . H3A1 H -0.3687(4) -0.5258(9) -0.6750(2) 0.091 Uiso 1 d R . H3A2 H -0.3996(4) -0.3882(9) -0.7011(2) 0.091 Uiso 1 d R . H3A3 H -0.4091(4) -0.5467(9) -0.7206(2) 0.091 Uiso 1 d R . N1B N -0.1374(3) -0.1121(7) -0.7676(2) 0.0556(14) Uani 1 d . . C2B C -0.1483(4) 0.0065(9) -0.7741(2) 0.055(2) Uani 1 d . . C3B C -0.1629(6) 0.1597(9) -0.7833(3) 0.113(4) Uani 1 d . . H3B1 H -0.1953(6) 0.1683(9) -0.8092(3) 0.136 Uiso 1 d R . H3B2 H -0.1919(6) 0.2039(9) -0.7601(3) 0.136 Uiso 1 d R . H3B3 H -0.1112(6) 0.2091(9) -0.7868(3) 0.136 Uiso 1 d R . Ni2 Ni -0.48884(5) -0.93538(10) -0.60723(3) 0.0315(2) Uani 1 d . . Na2 Na -0.59836(12) -0.9176(3) -0.50051(6) 0.0496(6) Uani 1 d . . O2W O -0.4573(2) -0.8406(5) -0.49459(12) 0.0538(11) Uani 1 d . . H2W1 H -0.4484(2) -0.8112(5) -0.52261(12) 0.065 Uiso 1 d R . H2W2 H -0.4727(2) -0.7585(5) -0.47828(12) 0.065 Uiso 1 d R . N4R N -0.3882(2) -1.0239(5) -0.63681(13) 0.0330(10) Uani 1 d . . C24 C -0.3763(3) -1.1190(6) -0.6041(2) 0.0303(12) Uani 1 d . . O4R O -0.4294(2) -1.1053(4) -0.57450(10) 0.0366(9) Uani 1 d . . C34 C -0.3108(3) -1.2184(6) -0.6046(2) 0.0389(14) Uani 1 d . . H34 H -0.3016(3) -1.2835(6) -0.5820(2) 0.047 Uiso 1 calc R . C44 C -0.2608(3) -1.2177(7) -0.6390(2) 0.048(2) Uani 1 d . . H44 H -0.2167(3) -1.2829(7) -0.6398(2) 0.058 Uiso 1 calc R . C54 C -0.2743(3) -1.1223(6) -0.6726(2) 0.0427(14) Uani 1 d . . H54 H -0.2402(3) -1.1216(6) -0.6962(2) 0.051 Uiso 1 calc R . C64 C -0.3390(3) -1.0300(6) -0.6699(2) 0.0343(13) Uani 1 d . . Cl4 Cl -0.36146(9) -0.9065(2) -0.71000(4) 0.0521(4) Uani 1 d . . N5R N -0.5855(2) -1.0498(5) -0.63392(13) 0.0315(10) Uani 1 d . . C25 C -0.6341(3) -1.0179(6) -0.6011(2) 0.0314(12) Uani 1 d . . O5R O -0.5986(2) -0.9367(4) -0.57290(10) 0.0368(9) Uani 1 d . . C35 C -0.7142(3) -1.0706(6) -0.6008(2) 0.0401(14) Uani 1 d . . H35 H -0.7483(3) -1.0506(6) -0.5779(2) 0.048 Uiso 1 calc R . C45 C -0.7415(3) -1.1514(7) -0.6343(2) 0.049(2) Uani 1 d . . H45 H -0.7948(3) -1.1889(7) -0.6340(2) 0.059 Uiso 1 calc R . C55 C -0.6930(3) -1.1801(7) -0.6690(2) 0.0434(15) Uani 1 d . . H55 H -0.7127(3) -1.2324(7) -0.6926(2) 0.052 Uiso 1 calc R . C65 C -0.6157(3) -1.1280(6) -0.6665(2) 0.0340(13) Uani 1 d . . Cl5 Cl -0.54876(9) -1.1568(2) -0.70752(4) 0.0470(4) Uani 1 d . . N6R N -0.5096(2) -0.7295(5) -0.63096(13) 0.0298(10) Uani 1 d . . C26 C -0.4694(3) -0.6656(6) -0.5975(2) 0.0359(13) Uani 1 d . . O6R O -0.4322(2) -0.7587(4) -0.57340(11) 0.0408(9) Uani 1 d . . C36 C -0.4724(3) -0.5130(6) -0.5918(2) 0.0436(15) Uani 1 d . . H36 H -0.4445(3) -0.4681(6) -0.5690(2) 0.052 Uiso 1 calc R . C46 C -0.5170(4) -0.4323(7) -0.6204(2) 0.049(2) Uani 1 d . . H46 H -0.5201(4) -0.3307(7) -0.6169(2) 0.059 Uiso 1 calc R . C56 C -0.5581(3) -0.4978(6) -0.6545(2) 0.0427(14) Uani 1 d . . H56 H -0.5889(3) -0.4429(6) -0.6742(2) 0.051 Uiso 1 calc R . C66 C -0.5513(3) -0.6454(6) -0.6578(2) 0.0322(12) Uani 1 d . . Cl6 Cl -0.59742(9) -0.7362(2) -0.70003(5) 0.0507(4) Uani 1 d . . N1C N -0.6296(4) -0.6366(8) -0.5054(2) 0.069(2) Uani 1 d . . C2C C -0.6581(4) -0.5325(9) -0.5168(2) 0.057(2) Uani 1 d . . C3C C -0.6963(5) -0.3987(8) -0.5315(3) 0.079(2) Uani 1 d . . H3C1 H -0.6824(5) -0.3198(8) -0.5122(3) 0.094 Uiso 1 d R . H3C2 H -0.6771(5) -0.3753(8) -0.5596(3) 0.094 Uiso 1 d R . H3C3 H -0.7549(5) -0.4115(8) -0.5326(3) 0.094 Uiso 1 d R . N1D N -0.7381(3) -0.9902(7) -0.4881(2) 0.068(2) Uani 1 d . . C2D C -0.7973(4) -1.0009(8) -0.4710(2) 0.054(2) Uani 1 d . . C3D C -0.8735(4) -1.0094(9) -0.4486(3) 0.082(3) Uani 1 d . . H3D1 H -0.8832(4) -1.1094(9) -0.4401(3) 0.098 Uiso 1 d R . H3D2 H -0.8706(4) -0.9475(9) -0.4237(3) 0.098 Uiso 1 d R . H3D3 H -0.9178(4) -0.9768(9) -0.4671(3) 0.098 Uiso 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 Ni1 0.0300(5) 0.0361(5) 0.0275(5) 0.0013(4) -0.0013(4) -0.0013(4) Na1 0.0377(11) 0.0467(14) 0.0370(12) -0.0032(10) -0.0008(9) 0.0043(10) O1W 0.049(3) 0.046(3) 0.026(3) 0.000 0.004(2) 0.000 N1R 0.032(2) 0.032(3) 0.034(3) -0.001(2) -0.002(2) -0.001(2) C21 0.033(3) 0.044(4) 0.039(3) 0.001(3) -0.001(3) 0.001(3) O1R 0.054(2) 0.041(2) 0.036(2) 0.002(2) -0.016(2) 0.001(2) C31 0.044(3) 0.035(4) 0.047(4) 0.009(3) 0.002(3) 0.009(3) C41 0.047(4) 0.028(3) 0.072(5) -0.008(3) 0.013(3) -0.001(3) C51 0.043(3) 0.045(4) 0.047(4) -0.011(3) 0.008(3) 0.000(3) C61 0.027(3) 0.041(4) 0.040(3) -0.007(3) 0.005(2) 0.001(2) Cl1 0.0546(9) 0.0649(11) 0.0405(9) -0.0071(8) -0.0114(7) 0.0004(8) N2R 0.032(2) 0.039(3) 0.027(2) -0.002(2) -0.002(2) 0.001(2) C22 0.035(3) 0.035(3) 0.032(3) 0.004(3) 0.002(2) -0.007(3) O2R 0.042(2) 0.039(2) 0.030(2) 0.001(2) 0.004(2) -0.007(2) C32 0.050(4) 0.047(4) 0.045(4) -0.013(3) 0.005(3) -0.016(3) C42 0.041(3) 0.061(4) 0.054(4) -0.002(3) 0.003(3) -0.023(3) C52 0.033(3) 0.067(4) 0.042(3) -0.006(3) 0.010(3) -0.007(3) C62 0.037(3) 0.041(3) 0.027(3) -0.006(3) -0.003(2) 0.004(3) Cl2 0.0463(8) 0.0705(11) 0.0454(9) -0.0232(8) 0.0017(7) -0.0010(8) N3R 0.032(2) 0.031(2) 0.025(2) 0.001(2) -0.001(2) -0.001(2) C23 0.042(3) 0.039(3) 0.023(3) -0.003(3) -0.002(2) 0.000(3) O3R 0.034(2) 0.053(3) 0.034(2) 0.003(2) 0.002(2) 0.000(2) C33 0.028(3) 0.056(4) 0.038(3) -0.007(3) 0.003(2) 0.002(3) C43 0.032(3) 0.059(4) 0.061(4) -0.008(4) -0.010(3) 0.012(3) C53 0.049(4) 0.042(4) 0.040(3) 0.008(3) -0.012(3) 0.002(3) C63 0.042(3) 0.034(3) 0.022(3) -0.005(2) -0.003(2) -0.004(3) Cl3 0.0552(9) 0.0520(9) 0.0303(7) 0.0032(7) 0.0022(6) -0.0078(7) N1A 0.057(4) 0.095(5) 0.063(4) -0.011(4) 0.023(3) -0.013(3) C2A 0.053(4) 0.062(5) 0.050(4) -0.010(3) 0.011(3) -0.007(3) C3A 0.052(4) 0.086(6) 0.091(6) -0.020(5) 0.028(4) -0.013(4) N1B 0.055(3) 0.061(4) 0.051(3) 0.008(3) -0.007(3) 0.003(3) C2B 0.052(4) 0.064(5) 0.050(4) 0.016(4) 0.002(3) 0.005(4) C3B 0.130(8) 0.070(6) 0.142(9) 0.044(6) 0.042(7) 0.029(6) Ni2 0.0312(5) 0.0389(6) 0.0244(5) 0.0010(4) 0.0004(4) 0.0004(4) Na2 0.0352(12) 0.083(2) 0.0309(12) 0.0091(12) 0.0035(9) 0.0037(12) O2W 0.048(2) 0.070(3) 0.044(2) 0.005(2) 0.008(2) 0.005(2) N4R 0.032(2) 0.043(3) 0.024(2) 0.003(2) -0.002(2) -0.004(2) C24 0.026(3) 0.035(3) 0.030(3) 0.001(2) -0.004(2) -0.004(2) O4R 0.037(2) 0.046(2) 0.026(2) 0.004(2) 0.002(2) 0.004(2) C34 0.036(3) 0.042(4) 0.039(3) 0.007(3) -0.001(2) 0.000(3) C44 0.045(3) 0.048(4) 0.052(4) -0.005(3) 0.008(3) 0.007(3) C54 0.040(3) 0.049(4) 0.039(3) -0.008(3) 0.013(3) -0.002(3) C64 0.039(3) 0.038(3) 0.025(3) -0.002(2) -0.002(2) -0.010(3) Cl4 0.0612(9) 0.0637(10) 0.0312(7) 0.0108(7) 0.0012(7) -0.0081(8) N5R 0.032(2) 0.037(3) 0.025(2) 0.004(2) 0.000(2) 0.005(2) C25 0.033(3) 0.028(3) 0.033(3) 0.005(2) 0.001(2) 0.004(2) O5R 0.039(2) 0.047(2) 0.025(2) -0.005(2) 0.003(2) -0.002(2) C35 0.029(3) 0.054(4) 0.038(3) 0.000(3) 0.004(2) 0.004(3) C45 0.035(3) 0.055(4) 0.058(4) -0.006(3) 0.000(3) -0.004(3) C55 0.039(3) 0.054(4) 0.037(3) -0.014(3) -0.004(3) 0.002(3) C65 0.043(3) 0.036(3) 0.023(3) 0.002(2) 0.004(2) 0.007(3) Cl5 0.0566(9) 0.0553(9) 0.0295(7) -0.0055(7) 0.0122(6) -0.0015(7) N6R 0.033(2) 0.030(2) 0.026(2) -0.002(2) 0.001(2) -0.003(2) C26 0.031(3) 0.047(4) 0.030(3) 0.004(3) 0.003(2) -0.003(3) O6R 0.044(2) 0.048(2) 0.030(2) 0.004(2) -0.008(2) -0.005(2) C36 0.044(3) 0.037(4) 0.050(4) -0.006(3) -0.001(3) -0.006(3) C46 0.049(4) 0.038(4) 0.060(4) -0.002(3) 0.007(3) -0.007(3) C56 0.040(3) 0.040(4) 0.048(4) 0.006(3) 0.000(3) 0.000(3) C66 0.032(3) 0.038(3) 0.026(3) 0.002(2) 0.001(2) -0.002(2) Cl6 0.0590(9) 0.0545(10) 0.0380(8) -0.0040(7) -0.0156(7) 0.0034(8) N1C 0.075(4) 0.084(5) 0.048(4) -0.002(3) -0.010(3) 0.009(4) C2C 0.056(4) 0.072(5) 0.043(4) -0.001(4) -0.011(3) -0.003(4) C3C 0.081(5) 0.066(5) 0.088(6) 0.006(5) -0.016(4) -0.004(4) N1D 0.053(4) 0.103(5) 0.050(4) -0.008(3) 0.010(3) -0.007(3) C2D 0.043(4) 0.075(5) 0.044(4) -0.008(3) 0.007(3) -0.003(3) C3D 0.062(5) 0.096(6) 0.088(6) -0.001(5) 0.033(4) -0.009(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 Ni1 N1R 2.046(4) . ? Ni1 N2R 2.059(4) . ? Ni1 N3R 2.066(4) . ? Ni1 O3R 2.108(3) . ? Ni1 O2R 2.123(4) . ? Ni1 O1R 2.139(4) . ? Na1 O1W 2.328(4) . ? Na1 O3R 2.347(4) 2_553 ? Na1 N1A 2.438(6) . ? Na1 N1B 2.468(6) . ? Na1 O1R 2.479(4) . ? O1W Na1 2.328(4) 2_553 ? N1R C61 1.317(6) . ? N1R C21 1.354(7) . ? C21 O1R 1.289(6) . ? C21 C31 1.417(8) . ? C31 C41 1.366(8) . ? C41 C51 1.380(8) . ? C51 C61 1.372(8) . ? C61 Cl1 1.745(6) . ? N2R C62 1.328(6) . ? N2R C22 1.367(6) . ? C22 O2R 1.300(6) . ? C22 C32 1.393(7) . ? C32 C42 1.380(8) . ? C42 C52 1.387(8) . ? C52 C62 1.373(7) . ? C62 Cl2 1.731(5) . ? N3R C63 1.323(6) . ? N3R C23 1.372(6) . ? C23 O3R 1.280(6) . ? C23 C33 1.406(7) . ? O3R Na1 2.347(4) 2_553 ? C33 C43 1.367(8) . ? C43 C53 1.413(8) . ? C53 C63 1.355(7) . ? C63 Cl3 1.746(5) . ? N1A C2A 1.115(7) . ? C2A C3A 1.455(8) . ? N1B C2B 1.121(8) . ? C2B C3B 1.453(10) . ? Ni2 N6R 2.057(4) . ? Ni2 N5R 2.069(4) . ? Ni2 N4R 2.078(4) . ? Ni2 O4R 2.100(4) . ? Ni2 O5R 2.121(3) . ? Ni2 O6R 2.144(4) . ? Na2 O5R 2.294(4) . ? Na2 O2W 2.404(5) 3_434 ? Na2 O4R 2.414(4) 3_434 ? Na2 O2W 2.425(4) . ? Na2 N1D 2.428(6) . ? Na2 N1C 2.631(7) . ? O2W Na2 2.404(5) 3_434 ? N4R C64 1.334(6) . ? N4R C24 1.363(6) . ? C24 O4R 1.297(6) . ? C24 C34 1.410(7) . ? O4R Na2 2.414(4) 3_434 ? C34 C44 1.373(7) . ? C44 C54 1.391(8) . ? C54 C64 1.362(7) . ? C64 Cl4 1.735(5) . ? N5R C65 1.343(6) . ? N5R C25 1.352(6) . ? C25 O5R 1.293(6) . ? C25 C35 1.401(7) . ? C35 C45 1.362(8) . ? C45 C55 1.392(8) . ? C55 C65 1.357(7) . ? C65 Cl5 1.735(5) . ? N6R C66 1.327(6) . ? N6R C26 1.368(6) . ? C26 O6R 1.289(6) . ? C26 C36 1.412(8) . ? C36 C46 1.369(8) . ? C46 C56 1.396(8) . ? C56 C66 1.362(8) . ? C66 Cl6 1.735(5) . ? N1C C2C 1.120(8) . ? C2C C3C 1.451(10) . ? N1D C2D 1.125(7) . ? C2D C3D 1.452(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1R Ni1 N2R 106.5(2) . . ? N1R Ni1 N3R 102.6(2) . . ? N2R Ni1 N3R 105.3(2) . . ? N1R Ni1 O3R 91.8(2) . . ? N2R Ni1 O3R 160.8(2) . . ? N3R Ni1 O3R 64.23(15) . . ? N1R Ni1 O2R 158.4(2) . . ? N2R Ni1 O2R 64.17(15) . . ? N3R Ni1 O2R 98.8(2) . . ? O3R Ni1 O2R 100.33(14) . . ? N1R Ni1 O1R 63.8(2) . . ? N2R Ni1 O1R 100.4(2) . . ? N3R Ni1 O1R 153.7(2) . . ? O3R Ni1 O1R 92.65(15) . . ? O2R Ni1 O1R 97.65(14) . . ? O1W Na1 O3R 82.68(12) . 2_553 ? O1W Na1 N1A 112.8(2) . . ? O3R Na1 N1A 93.2(2) 2_553 . ? O1W Na1 N1B 148.6(2) . . ? O3R Na1 N1B 105.2(2) 2_553 . ? N1A Na1 N1B 97.4(2) . . ? O1W Na1 O1R 79.66(12) . . ? O3R Na1 O1R 161.9(2) 2_553 . ? N1A Na1 O1R 97.3(2) . . ? N1B Na1 O1R 88.1(2) . . ? Na1 O1W Na1 92.0(2) 2_553 . ? C61 N1R C21 120.4(5) . . ? C61 N1R Ni1 146.7(4) . . ? C21 N1R Ni1 92.4(3) . . ? O1R C21 N1R 113.6(5) . . ? O1R C21 C31 127.0(5) . . ? N1R C21 C31 119.3(5) . . ? C21 O1R Ni1 90.1(3) . . ? C21 O1R Na1 148.1(4) . . ? Ni1 O1R Na1 120.6(2) . . ? C41 C31 C21 117.9(6) . . ? C31 C41 C51 122.2(6) . . ? C61 C51 C41 116.3(6) . . ? N1R C61 C51 123.9(6) . . ? N1R C61 Cl1 116.3(4) . . ? C51 C61 Cl1 119.8(5) . . ? C62 N2R C22 118.9(4) . . ? C62 N2R Ni1 149.2(4) . . ? C22 N2R Ni1 91.8(3) . . ? O2R C22 N2R 112.8(4) . . ? O2R C22 C32 126.8(5) . . ? N2R C22 C32 120.3(5) . . ? C22 O2R Ni1 91.0(3) . . ? C42 C32 C22 119.0(5) . . ? C32 C42 C52 120.6(5) . . ? C62 C52 C42 117.0(5) . . ? N2R C62 C52 124.2(5) . . ? N2R C62 Cl2 115.8(4) . . ? C52 C62 Cl2 120.0(4) . . ? C63 N3R C23 119.2(4) . . ? C63 N3R Ni1 150.0(4) . . ? C23 N3R Ni1 90.7(3) . . ? O3R C23 N3R 113.6(5) . . ? O3R C23 C33 126.6(5) . . ? N3R C23 C33 119.8(5) . . ? C23 O3R Ni1 91.4(3) . . ? C23 O3R Na1 158.1(3) . 2_553 ? Ni1 O3R Na1 109.4(2) . 2_553 ? C43 C33 C23 118.6(5) . . ? C33 C43 C53 121.3(5) . . ? C63 C53 C43 115.9(5) . . ? N3R C63 C53 125.1(5) . . ? N3R C63 Cl3 115.1(4) . . ? C53 C63 Cl3 119.8(4) . . ? C2A N1A Na1 164.5(6) . . ? N1A C2A C3A 178.4(8) . . ? C2B N1B Na1 174.0(6) . . ? N1B C2B C3B 178.9(9) . . ? N6R Ni2 N5R 101.3(2) . . ? N6R Ni2 N4R 108.8(2) . . ? N5R Ni2 N4R 103.2(2) . . ? N6R Ni2 O4R 158.79(15) . . ? N5R Ni2 O4R 99.8(2) . . ? N4R Ni2 O4R 64.27(15) . . ? N6R Ni2 O5R 93.18(15) . . ? N5R Ni2 O5R 63.44(15) . . ? N4R Ni2 O5R 156.6(2) . . ? O4R Ni2 O5R 97.77(14) . . ? N6R Ni2 O6R 63.60(15) . . ? N5R Ni2 O6R 155.4(2) . . ? N4R Ni2 O6R 100.3(2) . . ? O4R Ni2 O6R 97.00(14) . . ? O5R Ni2 O6R 96.56(14) . . ? O5R Na2 O2W 81.9(2) . 3_434 ? O5R Na2 O4R 169.21(15) . 3_434 ? O2W Na2 O4R 94.51(15) 3_434 3_434 ? O5R Na2 O2W 94.74(14) . . ? O2W Na2 O2W 84.8(2) 3_434 . ? O4R Na2 O2W 74.75(14) 3_434 . ? O5R Na2 N1D 99.0(2) . . ? O2W Na2 N1D 96.8(2) 3_434 . ? O4R Na2 N1D 91.5(2) 3_434 . ? O2W Na2 N1D 166.3(2) . . ? O5R Na2 N1C 91.1(2) . . ? O2W Na2 N1C 166.7(2) 3_434 . ? O4R Na2 N1C 90.3(2) 3_434 . ? O2W Na2 N1C 84.5(2) . . ? N1D Na2 N1C 95.4(2) . . ? Na2 O2W Na2 95.2(2) 3_434 . ? C64 N4R C24 119.1(5) . . ? C64 N4R Ni2 150.1(4) . . ? C24 N4R Ni2 90.7(3) . . ? O4R C24 N4R 113.3(4) . . ? O4R C24 C34 126.5(5) . . ? N4R C24 C34 120.2(5) . . ? C24 O4R Ni2 91.7(3) . . ? C24 O4R Na2 126.8(3) . 3_434 ? Ni2 O4R Na2 119.7(2) . 3_434 ? C44 C34 C24 118.2(5) . . ? C34 C44 C54 121.2(5) . . ? C64 C54 C44 117.1(5) . . ? N4R C64 C54 124.1(5) . . ? N4R C64 Cl4 114.9(4) . . ? C54 C64 Cl4 121.0(4) . . ? C65 N5R C25 119.2(4) . . ? C65 N5R Ni2 148.6(4) . . ? C25 N5R Ni2 92.2(3) . . ? O5R C25 N5R 112.8(4) . . ? O5R C25 C35 127.1(5) . . ? N5R C25 C35 120.0(5) . . ? C25 O5R Ni2 91.5(3) . . ? C25 O5R Na2 136.4(3) . . ? Ni2 O5R Na2 121.6(2) . . ? C45 C35 C25 118.4(5) . . ? C35 C45 C55 122.1(5) . . ? C65 C55 C45 115.9(5) . . ? N5R C65 C55 124.3(5) . . ? N5R C65 Cl5 115.1(4) . . ? C55 C65 Cl5 120.6(4) . . ? C66 N6R C26 118.8(5) . . ? C66 N6R Ni2 147.8(4) . . ? C26 N6R Ni2 92.1(3) . . ? O6R C26 N6R 112.9(5) . . ? O6R C26 C36 126.7(5) . . ? N6R C26 C36 120.4(5) . . ? C26 O6R Ni2 90.6(3) . . ? C46 C36 C26 118.1(6) . . ? C36 C46 C56 121.4(6) . . ? C66 C56 C46 116.6(6) . . ? N6R C66 C56 124.8(5) . . ? N6R C66 Cl6 115.2(4) . . ? C56 C66 Cl6 120.1(4) . . ? C2C N1C Na2 159.0(6) . . ? N1C C2C C3C 179.1(8) . . ? C2D N1D Na2 158.2(5) . . ? N1D C2D C3D 178.0(8) . . ? 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 O3R Na1 O1W Na1 116.03(12) 2_553 . . 2_553 ? N1A Na1 O1W Na1 -153.5(2) . . . 2_553 ? N1B Na1 O1W Na1 8.8(3) . . . 2_553 ? O1R Na1 O1W Na1 -59.94(10) . . . 2_553 ? N2R Ni1 N1R C61 94.9(6) . . . . ? N3R Ni1 N1R C61 -15.4(7) . . . . ? O3R Ni1 N1R C61 -79.4(6) . . . . ? O2R Ni1 N1R C61 155.9(5) . . . . ? O1R Ni1 N1R C61 -171.4(7) . . . . ? N2R Ni1 N1R C21 -95.5(3) . . . . ? N3R Ni1 N1R C21 154.1(3) . . . . ? O3R Ni1 N1R C21 90.1(3) . . . . ? O2R Ni1 N1R C21 -34.6(6) . . . . ? O1R Ni1 N1R C21 -1.9(3) . . . . ? C61 N1R C21 O1R 176.5(4) . . . . ? Ni1 N1R C21 O1R 3.1(5) . . . . ? C61 N1R C21 C31 -2.6(7) . . . . ? Ni1 N1R C21 C31 -175.9(4) . . . . ? N1R C21 O1R Ni1 -3.0(4) . . . . ? C31 C21 O1R Ni1 176.0(5) . . . . ? N1R C21 O1R Na1 -168.3(4) . . . . ? C31 C21 O1R Na1 10.6(11) . . . . ? N1R Ni1 O1R C21 2.0(3) . . . . ? N2R Ni1 O1R C21 105.5(3) . . . . ? N3R Ni1 O1R C21 -61.3(5) . . . . ? O3R Ni1 O1R C21 -88.7(3) . . . . ? O2R Ni1 O1R C21 170.5(3) . . . . ? N1R Ni1 O1R Na1 173.1(3) . . . . ? N2R Ni1 O1R Na1 -83.5(2) . . . . ? N3R Ni1 O1R Na1 109.7(3) . . . . ? O3R Ni1 O1R Na1 82.3(2) . . . . ? O2R Ni1 O1R Na1 -18.4(2) . . . . ? O1W Na1 O1R C21 131.0(7) . . . . ? O3R Na1 O1R C21 118.0(7) 2_553 . . . ? N1A Na1 O1R C21 -117.1(7) . . . . ? N1B Na1 O1R C21 -19.9(7) . . . . ? O1W Na1 O1R Ni1 -31.9(2) . . . . ? O3R Na1 O1R Ni1 -44.9(6) 2_553 . . . ? N1A Na1 O1R Ni1 80.0(2) . . . . ? N1B Na1 O1R Ni1 177.2(2) . . . . ? O1R C21 C31 C41 -175.0(5) . . . . ? N1R C21 C31 C41 3.9(8) . . . . ? C21 C31 C41 C51 -2.4(9) . . . . ? C31 C41 C51 C61 -0.4(9) . . . . ? C21 N1R C61 C51 -0.3(8) . . . . ? Ni1 N1R C61 C51 167.5(5) . . . . ? C21 N1R C61 Cl1 179.0(4) . . . . ? Ni1 N1R C61 Cl1 -13.1(8) . . . . ? C41 C51 C61 N1R 1.8(8) . . . . ? C41 C51 C61 Cl1 -177.5(4) . . . . ? N1R Ni1 N2R C62 -22.4(8) . . . . ? N3R Ni1 N2R C62 86.0(7) . . . . ? O3R Ni1 N2R C62 140.1(7) . . . . ? O2R Ni1 N2R C62 178.5(8) . . . . ? O1R Ni1 N2R C62 -88.0(7) . . . . ? N1R Ni1 N2R C22 156.3(3) . . . . ? N3R Ni1 N2R C22 -95.2(3) . . . . ? O3R Ni1 N2R C22 -41.1(6) . . . . ? O2R Ni1 N2R C22 -2.7(3) . . . . ? O1R Ni1 N2R C22 90.8(3) . . . . ? C62 N2R C22 O2R -176.3(5) . . . . ? Ni1 N2R C22 O2R 4.4(4) . . . . ? C62 N2R C22 C32 1.7(8) . . . . ? Ni1 N2R C22 C32 -177.6(5) . . . . ? N2R C22 O2R Ni1 -4.2(4) . . . . ? C32 C22 O2R Ni1 177.9(6) . . . . ? N1R Ni1 O2R C22 -65.8(5) . . . . ? N2R Ni1 O2R C22 2.9(3) . . . . ? N3R Ni1 O2R C22 105.7(3) . . . . ? O3R Ni1 O2R C22 170.9(3) . . . . ? O1R Ni1 O2R C22 -95.0(3) . . . . ? O2R C22 C32 C42 177.5(6) . . . . ? N2R C22 C32 C42 -0.3(9) . . . . ? C22 C32 C42 C52 -0.8(10) . . . . ? C32 C42 C52 C62 0.4(10) . . . . ? C22 N2R C62 C52 -2.1(8) . . . . ? Ni1 N2R C62 C52 176.5(5) . . . . ? C22 N2R C62 Cl2 176.0(4) . . . . ? Ni1 N2R C62 Cl2 -5.4(9) . . . . ? C42 C52 C62 N2R 1.1(9) . . . . ? C42 C52 C62 Cl2 -177.0(5) . . . . ? N1R Ni1 N3R C63 90.6(7) . . . . ? N2R Ni1 N3R C63 -20.7(7) . . . . ? O3R Ni1 N3R C63 176.5(8) . . . . ? O2R Ni1 N3R C63 -86.2(7) . . . . ? O1R Ni1 N3R C63 145.8(6) . . . . ? N1R Ni1 N3R C23 -85.4(3) . . . . ? N2R Ni1 N3R C23 163.3(3) . . . . ? O3R Ni1 N3R C23 0.5(3) . . . . ? O2R Ni1 N3R C23 97.8(3) . . . . ? O1R Ni1 N3R C23 -30.2(5) . . . . ? C63 N3R C23 O3R -178.5(4) . . . . ? Ni1 N3R C23 O3R -0.8(5) . . . . ? C63 N3R C23 C33 1.3(7) . . . . ? Ni1 N3R C23 C33 179.0(5) . . . . ? N3R C23 O3R Ni1 0.8(4) . . . . ? C33 C23 O3R Ni1 -179.1(5) . . . . ? N3R C23 O3R Na1 -161.6(7) . . . 2_553 ? C33 C23 O3R Na1 18.6(13) . . . 2_553 ? N1R Ni1 O3R C23 102.5(3) . . . . ? N2R Ni1 O3R C23 -60.8(6) . . . . ? N3R Ni1 O3R C23 -0.5(3) . . . . ? O2R Ni1 O3R C23 -95.4(3) . . . . ? O1R Ni1 O3R C23 166.4(3) . . . . ? N1R Ni1 O3R Na1 -84.3(2) . . . 2_553 ? N2R Ni1 O3R Na1 112.3(5) . . . 2_553 ? N3R Ni1 O3R Na1 172.6(2) . . . 2_553 ? O2R Ni1 O3R Na1 77.8(2) . . . 2_553 ? O1R Ni1 O3R Na1 -20.5(2) . . . 2_553 ? O3R C23 C33 C43 -179.1(5) . . . . ? N3R C23 C33 C43 1.1(8) . . . . ? C23 C33 C43 C53 -2.1(9) . . . . ? C33 C43 C53 C63 0.8(9) . . . . ? C23 N3R C63 C53 -2.9(8) . . . . ? Ni1 N3R C63 C53 -178.3(5) . . . . ? C23 N3R C63 Cl3 177.5(4) . . . . ? Ni1 N3R C63 Cl3 2.0(9) . . . . ? C43 C53 C63 N3R 1.8(9) . . . . ? C43 C53 C63 Cl3 -178.6(4) . . . . ? O1W Na1 N1A C2A 125.3(23) . . . . ? O3R Na1 N1A C2A -151.3(23) 2_553 . . . ? N1B Na1 N1A C2A -45.5(24) . . . . ? O1R Na1 N1A C2A 43.5(24) . . . . ? Na1 N1A C2A C3A 74.8(260) . . . . ? O1W Na1 N1B C2B 40.2(55) . . . . ? O3R Na1 N1B C2B -60.8(54) 2_553 . . . ? N1A Na1 N1B C2B -156.2(53) . . . . ? O1R Na1 N1B C2B 106.7(54) . . . . ? Na1 N1B C2B C3B 62.8(424) . . . . ? O5R Na2 O2W Na2 -81.4(2) . . . 3_434 ? O2W Na2 O2W Na2 0.0 3_434 . . 3_434 ? O4R Na2 O2W Na2 96.1(2) 3_434 . . 3_434 ? N1D Na2 O2W Na2 97.7(9) . . . 3_434 ? N1C Na2 O2W Na2 -172.0(2) . . . 3_434 ? N6R Ni2 N4R C64 -25.1(8) . . . . ? N5R Ni2 N4R C64 82.0(7) . . . . ? O4R Ni2 N4R C64 176.6(8) . . . . ? O5R Ni2 N4R C64 134.1(7) . . . . ? O6R Ni2 N4R C64 -90.5(7) . . . . ? N6R Ni2 N4R C24 158.3(3) . . . . ? N5R Ni2 N4R C24 -94.7(3) . . . . ? O4R Ni2 N4R C24 0.0(3) . . . . ? O5R Ni2 N4R C24 -42.6(5) . . . . ? O6R Ni2 N4R C24 92.8(3) . . . . ? C64 N4R C24 O4R -178.0(4) . . . . ? Ni2 N4R C24 O4R 0.1(4) . . . . ? C64 N4R C24 C34 2.5(7) . . . . ? Ni2 N4R C24 C34 -179.4(4) . . . . ? N4R C24 O4R Ni2 -0.1(4) . . . . ? C34 C24 O4R Ni2 179.4(5) . . . . ? N4R C24 O4R Na2 -130.0(4) . . . 3_434 ? C34 C24 O4R Na2 49.4(7) . . . 3_434 ? N6R Ni2 O4R C24 -75.2(5) . . . . ? N5R Ni2 O4R C24 100.1(3) . . . . ? N4R Ni2 O4R C24 0.0(3) . . . . ? O5R Ni2 O4R C24 164.4(3) . . . . ? O6R Ni2 O4R C24 -98.0(3) . . . . ? N6R Ni2 O4R Na2 59.8(5) . . . 3_434 ? N5R Ni2 O4R Na2 -124.9(2) . . . 3_434 ? N4R Ni2 O4R Na2 135.1(2) . . . 3_434 ? O5R Ni2 O4R Na2 -60.6(2) . . . 3_434 ? O6R Ni2 O4R Na2 37.0(2) . . . 3_434 ? O4R C24 C34 C44 179.6(5) . . . . ? N4R C24 C34 C44 -0.9(8) . . . . ? C24 C34 C44 C54 -0.3(9) . . . . ? C34 C44 C54 C64 0.1(9) . . . . ? C24 N4R C64 C54 -2.9(8) . . . . ? Ni2 N4R C64 C54 -179.1(5) . . . . ? C24 N4R C64 Cl4 178.6(4) . . . . ? Ni2 N4R C64 Cl4 2.4(9) . . . . ? C44 C54 C64 N4R 1.6(8) . . . . ? C44 C54 C64 Cl4 180.0(4) . . . . ? N6R Ni2 N5R C65 88.5(7) . . . . ? N4R Ni2 N5R C65 -24.1(7) . . . . ? O4R Ni2 N5R C65 -89.8(7) . . . . ? O5R Ni2 N5R C65 176.4(7) . . . . ? O6R Ni2 N5R C65 138.0(6) . . . . ? N6R Ni2 N5R C25 -88.7(3) . . . . ? N4R Ni2 N5R C25 158.7(3) . . . . ? O4R Ni2 N5R C25 93.0(3) . . . . ? O5R Ni2 N5R C25 -0.8(3) . . . . ? O6R Ni2 N5R C25 -39.2(5) . . . . ? C65 N5R C25 O5R -177.1(4) . . . . ? Ni2 N5R C25 O5R 1.3(4) . . . . ? C65 N5R C25 C35 2.2(7) . . . . ? Ni2 N5R C25 C35 -179.5(4) . . . . ? N5R C25 O5R Ni2 -1.2(4) . . . . ? C35 C25 O5R Ni2 179.6(5) . . . . ? N5R C25 O5R Na2 -143.3(4) . . . . ? C35 C25 O5R Na2 37.5(8) . . . . ? N6R Ni2 O5R C25 101.9(3) . . . . ? N5R Ni2 O5R C25 0.8(3) . . . . ? N4R Ni2 O5R C25 -58.4(5) . . . . ? O4R Ni2 O5R C25 -96.3(3) . . . . ? O6R Ni2 O5R C25 165.7(3) . . . . ? N6R Ni2 O5R Na2 -107.9(2) . . . . ? N5R Ni2 O5R Na2 151.0(3) . . . . ? N4R Ni2 O5R Na2 91.8(4) . . . . ? O4R Ni2 O5R Na2 53.9(2) . . . . ? O6R Ni2 O5R Na2 -44.1(2) . . . . ? O2W Na2 O5R C25 63.3(5) 3_434 . . . ? O4R Na2 O5R C25 134.4(9) 3_434 . . . ? O2W Na2 O5R C25 147.4(5) . . . . ? N1D Na2 O5R C25 -32.4(5) . . . . ? N1C Na2 O5R C25 -128.0(5) . . . . ? O2W Na2 O5R Ni2 -70.5(2) 3_434 . . . ? O4R Na2 O5R Ni2 0.5(11) 3_434 . . . ? O2W Na2 O5R Ni2 13.5(2) . . . . ? N1D Na2 O5R Ni2 -166.2(2) . . . . ? N1C Na2 O5R Ni2 98.1(2) . . . . ? O5R C25 C35 C45 178.0(5) . . . . ? N5R C25 C35 C45 -1.1(8) . . . . ? C25 C35 C45 C55 -1.4(9) . . . . ? C35 C45 C55 C65 2.7(9) . . . . ? C25 N5R C65 C55 -0.7(8) . . . . ? Ni2 N5R C65 C55 -177.5(5) . . . . ? C25 N5R C65 Cl5 177.9(4) . . . . ? Ni2 N5R C65 Cl5 1.1(9) . . . . ? C45 C55 C65 N5R -1.7(9) . . . . ? C45 C55 C65 Cl5 179.8(4) . . . . ? N5R Ni2 N6R C66 -10.2(7) . . . . ? N4R Ni2 N6R C66 98.2(6) . . . . ? O4R Ni2 N6R C66 165.2(5) . . . . ? O5R Ni2 N6R C66 -73.7(6) . . . . ? O6R Ni2 N6R C66 -169.4(7) . . . . ? N5R Ni2 N6R C26 153.9(3) . . . . ? N4R Ni2 N6R C26 -97.7(3) . . . . ? O4R Ni2 N6R C26 -30.7(6) . . . . ? O5R Ni2 N6R C26 90.4(3) . . . . ? O6R Ni2 N6R C26 -5.3(3) . . . . ? C66 N6R C26 O6R 179.1(4) . . . . ? Ni2 N6R C26 O6R 8.6(4) . . . . ? C66 N6R C26 C36 0.0(7) . . . . ? Ni2 N6R C26 C36 -170.4(5) . . . . ? N6R C26 O6R Ni2 -8.3(4) . . . . ? C36 C26 O6R Ni2 170.7(5) . . . . ? N6R Ni2 O6R C26 5.7(3) . . . . ? N5R Ni2 O6R C26 -50.6(5) . . . . ? N4R Ni2 O6R C26 111.6(3) . . . . ? O4R Ni2 O6R C26 176.7(3) . . . . ? O5R Ni2 O6R C26 -84.6(3) . . . . ? O6R C26 C36 C46 -178.4(5) . . . . ? N6R C26 C36 C46 0.6(8) . . . . ? C26 C36 C46 C56 -0.5(9) . . . . ? C36 C46 C56 C66 -0.1(9) . . . . ? C26 N6R C66 C56 -0.7(8) . . . . ? Ni2 N6R C66 C56 161.1(5) . . . . ? C26 N6R C66 Cl6 178.1(4) . . . . ? Ni2 N6R C66 Cl6 -20.1(8) . . . . ? C46 C56 C66 N6R 0.7(8) . . . . ? C46 C56 C66 Cl6 -178.0(4) . . . . ? O5R Na2 N1C C2C 41.9(17) . . . . ? O2W Na2 N1C C2C 99.8(18) 3_434 . . . ? O4R Na2 N1C C2C -148.8(17) 3_434 . . . ? O2W Na2 N1C C2C 136.5(17) . . . . ? N1D Na2 N1C C2C -57.2(17) . . . . ? Na2 N1C C2C C3C 48.7(455) . . . . ? O5R Na2 N1D C2D -159.3(17) . . . . ? O2W Na2 N1D C2D 117.9(17) 3_434 . . . ? O4R Na2 N1D C2D 23.1(17) 3_434 . . . ? O2W Na2 N1D C2D 21.6(23) . . . . ? N1C Na2 N1D C2D -67.3(17) . . . . ? Na2 N1D C2D C3D 49.8(226) . . . . ? _refine_diff_density_max 0.283 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.075 #==END data_eb2209 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C30 H20 Cl6 N6 Na2 Ni2 O7' _chemical_formula_weight 952.62 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.407(6) _cell_length_b 11.860(3) _cell_length_c 13.912(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.04(2) _cell_angle_gamma 90.00 _cell_volume 3531.5(14) _cell_formula_units_Z 4 _cell_measurement_temperature 220(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 0.35 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.792 _exptl_crystal_density_method ? _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 6.243 _exptl_absorpt_correction_type Difabs _exptl_absorpt_correction_T_min 0.462 _exptl_absorpt_correction_T_max 1.323 _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method omega-2theta _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4501 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.1041 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.13 _diffrn_reflns_theta_max 59.95 _reflns_number_total 2584 _reflns_number_observed 1414 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0358P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2579 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1166 _refine_ls_R_factor_obs 0.0515 _refine_ls_wR_factor_all 0.1091 _refine_ls_wR_factor_obs 0.0881 _refine_ls_goodness_of_fit_all 0.966 _refine_ls_goodness_of_fit_obs 1.115 _refine_ls_restrained_S_all 0.971 _refine_ls_restrained_S_obs 1.115 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.55288(5) 0.09230(9) 0.01109(8) 0.0348(3) Uani 1 d . . N11 N 0.6518(2) 0.0879(5) 0.0182(4) 0.0353(14) Uani 1 d . . C21 C 0.6538(3) 0.0736(6) -0.0798(5) 0.035(2) Uani 1 d . . C31 C 0.7104(3) 0.0790(6) -0.1270(5) 0.043(2) Uani 1 d . . H31 H 0.7117(3) 0.0709(6) -0.1942(5) 0.052 Uiso 1 calc R . C41 C 0.7639(3) 0.0964(6) -0.0745(6) 0.052(2) Uani 1 d . . H41 H 0.8025(3) 0.1000(6) -0.1055(6) 0.063 Uiso 1 calc R . C51 C 0.7615(3) 0.1089(6) 0.0258(5) 0.050(2) Uani 1 d . . H51 H 0.7980(3) 0.1195(6) 0.0632(5) 0.060 Uiso 1 calc R . C61 C 0.7048(3) 0.1051(6) 0.0664(5) 0.039(2) Uani 1 d . . O21 O 0.5993(2) 0.0594(4) -0.1189(3) 0.0425(12) Uani 1 d . . Cl1 Cl 0.69836(9) 0.1264(2) 0.18868(13) 0.0620(6) Uani 1 d . . N12 N 0.5538(2) 0.2652(4) 0.0119(4) 0.0289(12) Uani 1 d . . C22 C 0.5493(3) 0.2724(6) 0.1092(5) 0.033(2) Uani 1 d . . C32 C 0.5568(3) 0.3753(6) 0.1559(5) 0.037(2) Uani 1 d . . H32 H 0.5533(3) 0.3795(6) 0.2230(5) 0.044 Uiso 1 calc R . C42 C 0.5691(3) 0.4693(6) 0.1048(5) 0.042(2) Uani 1 d . . H42 H 0.5755(3) 0.5384(6) 0.1366(5) 0.051 Uiso 1 calc R . C52 C 0.5725(3) 0.4636(6) 0.0029(5) 0.041(2) Uani 1 d . . H52 H 0.5799(3) 0.5277(6) -0.0350(5) 0.049 Uiso 1 calc R . C62 C 0.5644(3) 0.3592(6) -0.0359(5) 0.036(2) Uani 1 d . . O22 O 0.5388(2) 0.1742(4) 0.1494(3) 0.0360(11) Uani 1 d . . Cl2 Cl 0.56906(10) 0.3444(2) -0.16046(12) 0.0543(6) Uani 1 d . . N13 N 0.3989(3) 0.1973(5) 0.0397(4) 0.0369(15) Uani 1 d . . C23 C 0.4160(3) 0.1478(6) -0.0427(5) 0.038(2) Uani 1 d . . C33 C 0.3856(3) 0.1718(6) -0.1305(5) 0.038(2) Uani 1 d . . H33 H 0.3981(3) 0.1364(6) -0.1875(5) 0.045 Uiso 1 calc R . C43 C 0.3370(3) 0.2486(6) -0.1318(5) 0.043(2) Uani 1 d . . H43 H 0.3160(3) 0.2655(6) -0.1900(5) 0.052 Uiso 1 calc R . C53 C 0.3191(3) 0.3005(6) -0.0480(5) 0.038(2) Uani 1 d . . H53 H 0.2867(3) 0.3539(6) -0.0467(5) 0.046 Uiso 1 calc R . C63 C 0.3517(3) 0.2693(6) 0.0332(5) 0.036(2) Uani 1 d . . O23 O 0.4626(2) 0.0737(4) -0.0387(3) 0.0439(13) Uani 1 d . . Cl3 Cl 0.33164(10) 0.3323(2) 0.14257(13) 0.0577(6) Uani 1 d . . Na1 Na 0.43658(12) 0.1091(2) 0.1925(2) 0.0406(7) Uani 1 d . . O1 O 0.5000 -0.0406(5) 0.2500 0.047(2) Uani 1 d S . H1A H 0.4846 -0.0784(5) 0.2909 0.057 Uiso 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 Ni1 0.0314(6) 0.0321(7) 0.0407(7) -0.0010(6) 0.0007(5) -0.0006(6) N11 0.035(3) 0.028(3) 0.043(3) -0.005(3) -0.001(3) -0.003(3) C21 0.028(4) 0.027(4) 0.050(4) -0.001(4) -0.005(3) -0.005(3) C31 0.038(4) 0.040(5) 0.052(4) -0.007(4) 0.005(4) -0.002(4) C41 0.036(4) 0.046(5) 0.076(6) -0.002(5) 0.016(4) 0.011(4) C51 0.031(4) 0.052(6) 0.068(6) -0.001(4) -0.003(4) 0.008(4) C61 0.037(4) 0.031(4) 0.047(4) 0.000(4) -0.003(3) -0.006(4) O21 0.044(3) 0.044(3) 0.040(3) -0.005(2) 0.002(2) 0.001(3) Cl1 0.0591(13) 0.079(2) 0.0476(11) -0.0014(11) -0.0109(10) -0.0099(12) N12 0.027(3) 0.024(3) 0.035(3) 0.003(3) -0.001(2) -0.001(3) C22 0.027(4) 0.036(4) 0.035(4) 0.003(4) 0.005(3) -0.002(3) C32 0.034(4) 0.035(4) 0.041(4) -0.012(4) 0.005(3) 0.008(3) C42 0.038(4) 0.034(4) 0.055(5) -0.011(4) 0.006(4) -0.004(4) C52 0.036(4) 0.036(4) 0.051(5) 0.007(4) 0.003(4) -0.006(4) C62 0.030(4) 0.039(5) 0.039(4) -0.005(4) -0.002(3) 0.004(3) O22 0.036(3) 0.038(3) 0.035(2) 0.001(2) 0.008(2) -0.001(2) Cl2 0.0718(14) 0.0552(13) 0.0359(10) 0.0096(10) 0.0048(10) -0.0008(12) N13 0.034(3) 0.034(4) 0.042(4) 0.006(3) -0.009(3) -0.008(3) C23 0.032(4) 0.031(4) 0.050(5) 0.002(4) 0.000(4) -0.004(3) C33 0.045(4) 0.030(4) 0.039(4) 0.001(4) 0.005(4) 0.002(4) C43 0.042(5) 0.042(5) 0.046(4) 0.009(4) -0.002(4) 0.001(4) C53 0.034(4) 0.034(4) 0.046(4) 0.005(4) 0.004(4) 0.001(4) C63 0.034(4) 0.031(4) 0.042(4) -0.003(4) -0.004(3) -0.008(4) O23 0.033(3) 0.032(3) 0.067(3) -0.002(3) -0.004(2) 0.005(2) Cl3 0.0646(13) 0.0615(14) 0.0474(11) -0.0061(11) 0.0098(10) 0.0007(12) Na1 0.041(2) 0.041(2) 0.0395(14) -0.0003(13) -0.0034(12) 0.0010(14) O1 0.053(4) 0.047(5) 0.042(4) 0.000 0.006(3) 0.000 _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 O23 2.035(5) 5_655 ? Ni1 N12 2.051(5) . ? Ni1 O23 2.052(4) . ? Ni1 O21 2.116(4) . ? Ni1 N11 2.119(5) . ? Ni1 O22 2.181(4) . ? Ni1 Na1 3.583(3) . ? N11 C61 1.323(7) . ? N11 C21 1.376(8) . ? C21 O21 1.289(7) . ? C21 C31 1.390(8) . ? C31 C41 1.363(9) . ? C41 C51 1.405(9) . ? C51 C61 1.348(9) . ? C61 Cl1 1.728(7) . ? O21 Na1 2.367(5) 5_655 ? N12 C62 1.320(8) . ? N12 C22 1.361(7) . ? C22 O22 1.313(7) . ? C22 C32 1.391(9) . ? C32 C42 1.350(9) . ? C42 C52 1.423(8) . ? C52 C62 1.361(9) . ? C62 Cl2 1.747(7) . ? O22 Na1 2.381(5) 2_655 ? O22 Na1 2.406(5) . ? N13 C63 1.325(8) . ? N13 C23 1.344(8) . ? N13 Na1 2.490(6) . ? C23 O23 1.330(8) . ? C23 C33 1.402(8) . ? C33 C43 1.383(9) . ? C43 C53 1.379(9) . ? C53 C63 1.369(8) . ? C63 Cl3 1.756(7) . ? O23 Ni1 2.035(5) 5_655 ? Na1 O1 2.366(6) . ? Na1 O21 2.367(5) 5_655 ? Na1 O22 2.381(5) 2_655 ? Na1 Na1 3.126(5) 2_655 ? O1 Na1 2.366(6) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O23 Ni1 N12 165.5(2) 5_655 . ? O23 Ni1 O23 78.7(2) 5_655 . ? N12 Ni1 O23 96.8(2) . . ? O23 Ni1 O21 93.7(2) 5_655 . ? N12 Ni1 O21 100.7(2) . . ? O23 Ni1 O21 98.4(2) . . ? O23 Ni1 N11 97.7(2) 5_655 . ? N12 Ni1 N11 90.8(2) . . ? O23 Ni1 N11 161.3(2) . . ? O21 Ni1 N11 63.3(2) . . ? O23 Ni1 O22 103.8(2) 5_655 . ? N12 Ni1 O22 63.3(2) . . ? O23 Ni1 O22 101.6(2) . . ? O21 Ni1 O22 155.6(2) . . ? N11 Ni1 O22 97.1(2) . . ? O23 Ni1 Na1 78.62(14) 5_655 . ? N12 Ni1 Na1 87.0(2) . . ? O23 Ni1 Na1 65.30(14) . . ? O21 Ni1 Na1 162.88(14) . . ? N11 Ni1 Na1 132.45(15) . . ? O22 Ni1 Na1 40.94(12) . . ? C61 N11 C21 118.7(6) . . ? C61 N11 Ni1 150.1(5) . . ? C21 N11 Ni1 90.3(4) . . ? O21 C21 N11 113.0(6) . . ? O21 C21 C31 126.6(6) . . ? N11 C21 C31 120.4(6) . . ? C41 C31 C21 119.0(7) . . ? C31 C41 C51 120.1(7) . . ? C61 C51 C41 117.6(7) . . ? N11 C61 C51 124.2(7) . . ? N11 C61 Cl1 116.0(5) . . ? C51 C61 Cl1 119.8(6) . . ? C21 O21 Ni1 92.9(4) . . ? C21 O21 Na1 125.3(4) . 5_655 ? Ni1 O21 Na1 111.8(2) . 5_655 ? C62 N12 C22 117.7(6) . . ? C62 N12 Ni1 147.5(5) . . ? C22 N12 Ni1 93.9(4) . . ? O22 C22 N12 112.6(6) . . ? O22 C22 C32 126.8(6) . . ? N12 C22 C32 120.6(6) . . ? C42 C32 C22 120.1(6) . . ? C32 C42 C52 120.0(7) . . ? C62 C52 C42 115.4(7) . . ? N12 C62 C52 126.2(6) . . ? N12 C62 Cl2 115.4(5) . . ? C52 C62 Cl2 118.4(6) . . ? C22 O22 Ni1 89.5(4) . . ? C22 O22 Na1 130.1(4) . 2_655 ? Ni1 O22 Na1 129.7(2) . 2_655 ? C22 O22 Na1 123.6(4) . . ? Ni1 O22 Na1 102.6(2) . . ? Na1 O22 Na1 81.5(2) 2_655 . ? C63 N13 C23 116.2(6) . . ? C63 N13 Na1 124.3(5) . . ? C23 N13 Na1 117.2(4) . . ? O23 C23 N13 117.9(6) . . ? O23 C23 C33 120.5(6) . . ? N13 C23 C33 121.7(6) . . ? C43 C33 C23 118.9(6) . . ? C53 C43 C33 120.2(7) . . ? C63 C53 C43 115.6(7) . . ? N13 C63 C53 127.4(6) . . ? N13 C63 Cl3 114.5(5) . . ? C53 C63 Cl3 118.1(6) . . ? C23 O23 Ni1 121.4(4) . 5_655 ? C23 O23 Ni1 130.2(4) . . ? Ni1 O23 Ni1 101.3(2) 5_655 . ? O1 Na1 O21 72.1(2) . 5_655 ? O1 Na1 O22 79.3(2) . 2_655 ? O21 Na1 O22 137.5(2) 5_655 2_655 ? O1 Na1 O22 78.8(2) . . ? O21 Na1 O22 116.9(2) 5_655 . ? O22 Na1 O22 86.5(2) 2_655 . ? O1 Na1 N13 141.1(2) . . ? O21 Na1 N13 83.5(2) 5_655 . ? O22 Na1 N13 135.7(2) 2_655 . ? O22 Na1 N13 86.2(2) . . ? O1 Na1 Na1 48.64(12) . 2_655 ? O21 Na1 Na1 119.57(13) 5_655 2_655 ? O22 Na1 Na1 49.57(12) 2_655 2_655 ? O22 Na1 Na1 48.89(12) . 2_655 ? N13 Na1 Na1 134.5(2) . 2_655 ? O1 Na1 Ni1 78.14(7) . . ? O21 Na1 Ni1 82.69(13) 5_655 . ? O22 Na1 Ni1 121.57(13) 2_655 . ? O22 Na1 Ni1 36.44(10) . . ? N13 Na1 Ni1 68.90(15) . . ? Na1 Na1 Ni1 75.65(9) 2_655 . ? Na1 O1 Na1 82.7(2) 2_655 . ? _refine_diff_density_max 0.305 _refine_diff_density_min -0.289 _refine_diff_density_rms 0.075 #==END data_eb2207 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C30 H20 Cl6 Co2 N6 Na2 O7' _chemical_formula_weight 953.06 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.590(13) _cell_length_b 11.916(9) _cell_length_c 13.879(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.37(6) _cell_angle_gamma 90.00 _cell_volume 3569.6(43) _cell_formula_units_Z 4 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 25 _cell_measurement_theta_max 27 _exptl_crystal_description 'plate developed in (001)' _exptl_crystal_colour Pink _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.773 _exptl_crystal_density_method ? _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 12.147 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.0919 _exptl_absorpt_correction_T_max 0.5274 _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method omega _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 11 _diffrn_reflns_number 2185 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.10 _diffrn_reflns_theta_max 54.96 _reflns_number_total 2185 _reflns_number_observed 1563 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 35 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0847P)^2^+53.1420P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00021(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2150 _refine_ls_number_parameters 244 _refine_ls_number_restraints 259 _refine_ls_R_factor_all 0.1174 _refine_ls_R_factor_obs 0.0775 _refine_ls_wR_factor_all 0.2167 _refine_ls_wR_factor_obs 0.1735 _refine_ls_goodness_of_fit_all 1.127 _refine_ls_goodness_of_fit_obs 1.157 _refine_ls_restrained_S_all 1.136 _refine_ls_restrained_S_obs 1.070 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.44749(7) 0.09268(13) 0.98887(11) 0.0257(5) Uani 1 d U . Na1 Na 0.4359(2) 0.1122(3) 0.6929(3) 0.0312(10) Uani 1 d U . O1 O 0.5000 -0.0364(8) 0.7500 0.037(2) Uani 1 d SDU . H1 H 0.4961(53) -0.0794(19) 0.7015(11) 0.044 Uiso 1 d D . N11 N 0.3465(3) 0.0906(6) 0.9821(5) 0.029(2) Uani 1 d DU . C21 C 0.3450(4) 0.0718(8) 1.0784(6) 0.029(2) Uani 1 d DU . C31 C 0.2888(4) 0.0771(9) 1.1280(7) 0.039(2) Uani 1 d DU . H31 H 0.2879(4) 0.0689(9) 1.1953(7) 0.047 Uiso 1 calc R . C41 C 0.2358(5) 0.0946(10) 1.0744(8) 0.049(3) Uani 1 d DU . H41 H 0.1976(5) 0.0970(10) 1.1054(8) 0.059 Uiso 1 calc R . C51 C 0.2370(5) 0.1088(9) 0.9757(7) 0.046(3) Uani 1 d DU . H51 H 0.2002(5) 0.1190(9) 0.9391(7) 0.055 Uiso 1 calc R . C61 C 0.2932(4) 0.1075(8) 0.9332(6) 0.033(2) Uani 1 d DU . O21 O 0.3995(3) 0.0563(6) 1.1193(4) 0.034(2) Uani 1 d DU . Cl1 Cl 0.29959(14) 0.1315(3) 0.8112(2) 0.0552(9) Uani 1 d DU . N12 N 0.4460(4) 0.2705(6) 0.9871(5) 0.027(2) Uani 1 d DU . C22 C 0.4503(4) 0.2751(7) 0.8901(6) 0.024(2) Uani 1 d DU . C32 C 0.4426(5) 0.3787(7) 0.8416(6) 0.030(2) Uani 1 d DU . H32 H 0.4452(5) 0.3828(7) 0.7742(6) 0.037 Uiso 1 calc R . C42 C 0.4314(5) 0.4725(8) 0.8946(7) 0.033(2) Uani 1 d DU . H42 H 0.4269(5) 0.5420(8) 0.8632(7) 0.039 Uiso 1 calc R . C52 C 0.4265(5) 0.4672(8) 0.9941(6) 0.032(2) Uani 1 d DU . H52 H 0.4176(5) 0.5312(8) 1.0308(6) 0.038 Uiso 1 calc R . C62 C 0.4353(5) 0.3647(8) 1.0360(6) 0.032(2) Uani 1 d DU . O22 O 0.4613(3) 0.1772(5) 0.8504(4) 0.031(2) Uani 1 d DU . Cl2 Cl 0.43052(14) 0.3490(2) 1.1601(2) 0.0456(8) Uani 1 d DU . N13 N 0.6018(3) 0.1971(6) 0.9636(5) 0.028(2) Uani 1 d DU . C23 C 0.5839(4) 0.1483(7) 1.0458(7) 0.030(2) Uani 1 d DU . C33 C 0.6145(4) 0.1722(8) 1.1349(7) 0.032(2) Uani 1 d DU . H33 H 0.6018(4) 0.1382(8) 1.1923(7) 0.038 Uiso 1 calc R . C43 C 0.6627(5) 0.2459(9) 1.1350(7) 0.037(3) Uani 1 d DU . H43 H 0.6838(5) 0.2623(9) 1.1934(7) 0.044 Uiso 1 calc R . C53 C 0.6815(5) 0.2976(8) 1.0502(6) 0.033(2) Uani 1 d DU . H53 H 0.7148(5) 0.3484(8) 1.0497(6) 0.040 Uiso 1 calc R . C63 C 0.6487(4) 0.2702(8) 0.9682(6) 0.028(2) Uani 1 d DU . O23 O 0.5371(3) 0.0764(5) 1.0407(5) 0.035(2) Uani 1 d DU . Cl3 Cl 0.66864(14) 0.3305(3) 0.8599(2) 0.0484(8) Uani 1 d DU . 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 0.0285(9) 0.0241(9) 0.0246(9) 0.0012(7) -0.0002(7) 0.0014(8) Na1 0.037(2) 0.034(2) 0.023(2) -0.004(2) -0.005(2) 0.003(2) O1 0.051(6) 0.034(5) 0.026(5) 0.000 -0.007(5) 0.000 N11 0.037(4) 0.028(4) 0.024(4) 0.001(4) -0.003(3) 0.007(4) C21 0.041(4) 0.023(5) 0.022(4) 0.001(4) -0.003(4) -0.004(5) C31 0.041(5) 0.041(6) 0.035(5) 0.005(5) 0.012(4) -0.012(6) C41 0.040(5) 0.054(7) 0.054(6) -0.001(6) 0.010(5) -0.004(6) C51 0.039(5) 0.049(7) 0.050(5) -0.001(6) -0.004(5) -0.002(6) C61 0.038(5) 0.035(6) 0.025(5) 0.001(5) -0.008(4) 0.002(5) O21 0.034(3) 0.038(4) 0.028(3) 0.005(3) -0.004(3) 0.003(3) Cl1 0.053(2) 0.078(2) 0.034(2) 0.0042(15) -0.0081(14) 0.016(2) N12 0.035(5) 0.029(4) 0.018(3) -0.002(3) 0.001(4) -0.002(4) C22 0.027(5) 0.030(4) 0.017(4) 0.000(3) 0.003(4) -0.001(5) C32 0.033(5) 0.037(5) 0.021(5) 0.007(4) 0.002(5) 0.004(5) C42 0.035(6) 0.022(5) 0.041(5) 0.009(4) 0.000(5) -0.012(5) C52 0.028(5) 0.028(5) 0.039(5) -0.008(4) 0.000(5) 0.015(5) C62 0.037(6) 0.036(5) 0.022(4) -0.002(4) 0.003(5) -0.006(5) O22 0.036(4) 0.036(4) 0.020(3) -0.005(3) 0.004(3) 0.010(3) Cl2 0.066(2) 0.049(2) 0.0219(14) -0.0078(12) 0.0045(13) 0.002(2) N13 0.024(4) 0.028(5) 0.032(4) -0.002(3) -0.005(3) 0.009(3) C23 0.037(5) 0.013(5) 0.041(5) -0.009(4) -0.004(4) -0.004(4) C33 0.041(6) 0.023(5) 0.032(5) 0.001(4) -0.002(4) 0.000(4) C43 0.041(6) 0.042(6) 0.027(5) -0.009(5) -0.007(5) -0.006(5) C53 0.038(6) 0.025(6) 0.036(5) -0.004(4) -0.006(4) -0.006(5) C63 0.029(5) 0.024(5) 0.030(5) -0.001(4) -0.001(4) 0.007(4) O23 0.028(3) 0.025(4) 0.052(4) -0.002(3) -0.003(3) -0.004(3) Cl3 0.054(2) 0.058(2) 0.0338(15) 0.0046(13) 0.0091(13) -0.001(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 Co1 O23 2.057(7) . Y Co1 O23 2.084(7) 5_657 Y Co1 N12 2.119(8) . Y Co1 O21 2.152(7) . Y Co1 N11 2.180(8) . Y Co1 O22 2.197(6) . Y Na1 O22 2.371(7) . Y Na1 O1 2.372(8) . Y Na1 O21 2.377(8) 6 Y Na1 O22 2.439(8) 2_656 Y Na1 N13 2.513(8) 2_656 Y Na1 Na1 3.157(8) 2_656 Y O1 Na1 2.372(8) 2_656 Y N11 C61 1.338(11) . ? N11 C21 1.355(10) . ? C21 O21 1.307(10) . ? C21 C31 1.411(12) . ? C31 C41 1.367(13) . ? C41 C51 1.381(13) . ? C51 C61 1.362(12) . ? C61 Cl1 1.726(9) . ? O21 Na1 2.377(8) 6_556 Y N12 C62 1.335(11) . ? N12 C22 1.353(10) . ? C22 O22 1.314(10) . ? C22 C32 1.415(11) . ? C32 C42 1.362(12) . ? C42 C52 1.389(12) . ? C52 C62 1.364(12) . ? C62 Cl2 1.737(9) . ? O22 Na1 2.439(8) 2_656 Y N13 C63 1.335(11) . ? N13 C23 1.346(11) . ? N13 Na1 2.513(8) 2_656 Y C23 O23 1.325(10) . ? C23 C33 1.417(12) . ? C33 C43 1.362(12) . ? C43 C53 1.398(12) . ? C53 C63 1.367(11) . ? C63 Cl3 1.730(9) . ? O23 Co1 2.084(7) 5_657 Y 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 O23 Co1 O23 79.9(3) . 5_657 Y O23 Co1 N12 96.4(3) . . Y O23 Co1 N12 165.1(3) 5_657 . Y O23 Co1 O21 98.9(3) . . Y O23 Co1 O21 93.1(3) 5_657 . Y N12 Co1 O21 101.7(3) . . Y O23 Co1 N11 160.9(3) . . Y O23 Co1 N11 98.3(3) 5_657 . Y N12 Co1 N11 89.8(3) . . Y O21 Co1 N11 62.1(2) . . Y O23 Co1 O22 101.7(3) . . Y O23 Co1 O22 104.2(3) 5_657 . Y N12 Co1 O22 62.2(2) . . Y O21 Co1 O22 155.1(2) . . Y N11 Co1 O22 97.1(3) . . Y O22 Na1 O1 79.4(2) . . Y O22 Na1 O21 137.6(3) . 6 Y O1 Na1 O21 72.4(2) . 6 Y O22 Na1 O22 86.0(3) . 2_656 Y O1 Na1 O22 78.0(2) . 2_656 Y O21 Na1 O22 117.2(3) 6 2_656 Y O22 Na1 N13 136.7(3) . 2_656 Y O1 Na1 N13 139.8(2) . 2_656 Y O21 Na1 N13 82.7(3) 6 2_656 Y O22 Na1 N13 86.4(3) 2_656 2_656 Y O22 Na1 Na1 49.9(2) . 2_656 Y O1 Na1 Na1 48.3(2) . 2_656 Y O21 Na1 Na1 119.5(2) 6 2_656 Y O22 Na1 Na1 48.1(2) 2_656 2_656 Y N13 Na1 Na1 134.1(2) 2_656 2_656 Y Na1 O1 Na1 83.5(4) 2_656 . Y C61 N11 C21 119.0(8) . . ? C61 N11 Co1 150.2(6) . . ? C21 N11 Co1 90.4(5) . . ? O21 C21 N11 114.2(8) . . ? O21 C21 C31 124.7(8) . . ? N11 C21 C31 121.0(8) . . ? C41 C31 C21 117.4(9) . . ? C31 C41 C51 121.6(9) . . ? C61 C51 C41 117.8(9) . . ? N11 C61 C51 123.1(8) . . ? N11 C61 Cl1 115.8(7) . . ? C51 C61 Cl1 121.1(7) . . ? C21 O21 Co1 93.0(5) . . ? C21 O21 Na1 126.2(6) . 6_556 Y Co1 O21 Na1 111.7(3) . 6_556 Y C62 N12 C22 119.3(7) . . ? C62 N12 Co1 146.9(6) . . ? C22 N12 Co1 92.9(5) . . ? O22 C22 N12 113.6(7) . . ? O22 C22 C32 126.5(7) . . ? N12 C22 C32 119.9(8) . . ? C42 C32 C22 118.7(8) . . ? C32 C42 C52 121.2(8) . . ? C62 C52 C42 116.8(8) . . ? N12 C62 C52 124.1(8) . . ? N12 C62 Cl2 115.4(7) . . ? C52 C62 Cl2 120.5(7) . . ? C22 O22 Co1 90.5(5) . . ? C22 O22 Na1 129.6(5) . . ? Co1 O22 Na1 128.5(3) . . ? C22 O22 Na1 124.1(6) . 2_656 Y Co1 O22 Na1 102.3(3) . 2_656 Y Na1 O22 Na1 82.0(2) . 2_656 Y C63 N13 C23 118.3(7) . . ? C63 N13 Na1 122.3(6) . 2_656 Y C23 N13 Na1 117.6(6) . 2_656 Y O23 C23 N13 118.0(8) . . ? O23 C23 C33 121.0(8) . . ? N13 C23 C33 121.0(8) . . ? C43 C33 C23 118.2(8) . . ? C33 C43 C53 121.4(8) . . ? C63 C53 C43 116.2(8) . . ? N13 C63 C53 125.0(8) . . ? N13 C63 Cl3 115.7(6) . . ? C53 C63 Cl3 119.3(7) . . ? C23 O23 Co1 131.8(6) . . ? C23 O23 Co1 120.7(6) . 5_657 Y Co1 O23 Co1 100.1(3) . 5_657 Y _refine_diff_density_max 0.572 _refine_diff_density_min -1.256 _refine_diff_density_rms 0.127 #==END data_cosnat _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C15 H9 Cl3 Co N3 Na O3' _chemical_formula_weight 467.52 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.2614(19) _cell_length_b 11.316(2) _cell_length_c 12.105(3) _cell_angle_alpha 112.204(10) _cell_angle_beta 93.119(14) _cell_angle_gamma 105.192(13) _cell_volume 875.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.773 _exptl_crystal_density_method ? _exptl_crystal_F_000 466 _exptl_absorpt_coefficient_mu 1.484 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3702 _diffrn_reflns_av_R_equivalents 0.0878 _diffrn_reflns_av_sigmaI/netI 0.1036 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.04 _reflns_number_total 3100 _reflns_number_observed 1959 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-96 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-96 (Sheldrick, 1996)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0502P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3100 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1090 _refine_ls_R_factor_obs 0.0538 _refine_ls_wR_factor_all 0.1196 _refine_ls_wR_factor_obs 0.1019 _refine_ls_goodness_of_fit_all 0.981 _refine_ls_goodness_of_fit_obs 1.074 _refine_ls_restrained_S_all 0.981 _refine_ls_restrained_S_obs 1.074 _refine_ls_shift/esd_max 0.014 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.41994(11) 0.44619(8) 0.59286(7) 0.0218(2) Uani 1 d . . Na1 Na 0.0069(3) 0.4211(2) 0.3606(2) 0.0285(6) Uani 1 d . . N11 N 0.2356(6) 0.2657(4) 0.5934(4) 0.0224(11) Uani 1 d . . C21 C 0.0715(8) 0.2917(5) 0.5621(5) 0.0223(13) Uani 1 d . . O21 O 0.1074(5) 0.3923(4) 0.5320(3) 0.0245(9) Uani 1 d . . C31 C -0.1111(8) 0.2154(6) 0.5690(6) 0.0326(15) Uani 1 d . . H31 H -0.2253 0.2298 0.5444 0.039 Uiso 1 calc R . C41 C -0.1170(8) 0.1202(6) 0.6125(6) 0.0327(16) Uani 1 d . . H41 H -0.2381 0.0692 0.6185 0.039 Uiso 1 calc R . C51 C 0.0479(8) 0.0949(6) 0.6483(6) 0.0302(15) Uani 1 d . . H51 H 0.0430 0.0300 0.6796 0.036 Uiso 1 calc R . C61 C 0.2180(8) 0.1711(6) 0.6350(5) 0.0275(14) Uani 1 d . . Cl1 Cl 0.4352(2) 0.14431(18) 0.67180(16) 0.0400(4) Uani 1 d . . N12 N 0.4357(7) 0.5367(5) 0.7861(4) 0.0252(11) Uani 1 d . . C22 C 0.6335(8) 0.5805(6) 0.8039(5) 0.0261(13) Uani 1 d . . O22 O 0.7037(5) 0.5401(4) 0.7063(4) 0.0299(10) Uani 1 d . . C32 C 0.7382(9) 0.6623(6) 0.9218(5) 0.0337(16) Uani 1 d . . H32 H 0.8741 0.6950 0.9348 0.040 Uiso 1 calc R . C42 C 0.6411(9) 0.6936(7) 1.0169(6) 0.0419(18) Uani 1 d . . H42 H 0.7111 0.7474 1.0956 0.050 Uiso 1 calc R . C52 C 0.4404(9) 0.6471(7) 0.9991(6) 0.0382(17) Uani 1 d . . H52 H 0.3716 0.6671 1.0639 0.046 Uiso 1 calc R . C62 C 0.3478(8) 0.5701(6) 0.8814(6) 0.0296(15) Uani 1 d . . Cl2 Cl 0.0955(2) 0.5054(2) 0.84970(16) 0.0469(5) Uani 1 d . . N13 N 0.6753(6) 0.2471(5) 0.3012(4) 0.0240(11) Uani 1 d . . C23 C 0.5179(8) 0.2666(5) 0.3504(5) 0.0225(13) Uani 1 d . . O23 O 0.5434(5) 0.3830(4) 0.4418(3) 0.0234(9) Uani 1 d . . C33 C 0.3365(8) 0.1695(6) 0.3036(5) 0.0268(14) Uani 1 d . . H33 H 0.2279 0.1834 0.3392 0.032 Uiso 1 calc R . C43 C 0.3197(8) 0.0530(6) 0.2044(6) 0.0317(15) Uani 1 d . . H43 H 0.1977 -0.0119 0.1707 0.038 Uiso 1 calc R . C53 C 0.4788(8) 0.0305(6) 0.1542(6) 0.0284(14) Uani 1 d . . H53 H 0.4712 -0.0492 0.0877 0.034 Uiso 1 calc R . C63 C 0.6495(8) 0.1319(6) 0.2074(5) 0.0252(13) Uani 1 d . . Cl3 Cl 0.8615(2) 0.11267(18) 0.14881(17) 0.0471(5) Uani 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 Co1 0.0194(4) 0.0276(5) 0.0179(4) 0.0100(4) 0.0043(3) 0.0047(3) Na1 0.0252(12) 0.0375(14) 0.0258(14) 0.0147(12) 0.0057(10) 0.0116(10) N11 0.021(2) 0.026(3) 0.025(3) 0.014(2) 0.003(2) 0.008(2) C21 0.026(3) 0.021(3) 0.020(3) 0.009(3) 0.011(3) 0.005(2) O21 0.019(2) 0.028(2) 0.030(2) 0.017(2) -0.0001(18) 0.0045(17) C31 0.021(3) 0.038(4) 0.045(4) 0.024(3) 0.007(3) 0.008(3) C41 0.022(3) 0.036(4) 0.044(4) 0.021(3) 0.011(3) 0.006(3) C51 0.032(3) 0.037(4) 0.034(4) 0.023(3) 0.015(3) 0.013(3) C61 0.028(3) 0.035(4) 0.023(3) 0.014(3) 0.002(3) 0.012(3) Cl1 0.0318(9) 0.0612(12) 0.0425(10) 0.0307(9) 0.0082(8) 0.0244(8) N12 0.026(3) 0.031(3) 0.022(3) 0.013(2) 0.007(2) 0.011(2) C22 0.025(3) 0.028(3) 0.026(4) 0.011(3) 0.002(3) 0.007(3) O22 0.022(2) 0.042(3) 0.022(2) 0.008(2) 0.0055(18) 0.0102(19) C32 0.025(3) 0.042(4) 0.026(4) 0.009(3) -0.001(3) 0.004(3) C42 0.037(4) 0.059(5) 0.018(4) 0.008(3) -0.005(3) 0.010(3) C52 0.037(4) 0.058(5) 0.022(4) 0.014(3) 0.011(3) 0.021(3) C62 0.024(3) 0.038(4) 0.032(4) 0.017(3) 0.008(3) 0.013(3) Cl2 0.0270(8) 0.0807(14) 0.0370(11) 0.0267(10) 0.0128(8) 0.0175(8) N13 0.024(3) 0.029(3) 0.021(3) 0.012(2) 0.003(2) 0.009(2) C23 0.027(3) 0.021(3) 0.021(3) 0.011(3) 0.003(3) 0.005(2) O23 0.025(2) 0.024(2) 0.023(2) 0.0099(19) 0.0099(18) 0.0091(17) C33 0.020(3) 0.030(3) 0.028(4) 0.011(3) 0.008(3) 0.003(3) C43 0.026(3) 0.033(4) 0.030(4) 0.013(3) 0.000(3) 0.001(3) C53 0.037(4) 0.020(3) 0.030(4) 0.011(3) 0.007(3) 0.009(3) C63 0.024(3) 0.034(4) 0.025(4) 0.015(3) 0.008(3) 0.015(3) Cl3 0.0329(9) 0.0603(12) 0.0430(11) 0.0096(9) 0.0143(8) 0.0218(8) _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 O23 2.0451(36) . ? Co1 O23 2.0831(37) 2_666 ? Co1 N11 2.1314(43) . ? Co1 N12 2.1525(48) . ? Co1 O22 2.1682(40) . ? Co1 O21 2.1951(36) . ? Na1 O22 2.2885(41) 2_666 ? Na1 O21 2.3270(44) . ? Na1 O21 2.4088(44) 2_566 ? Na1 N13 2.5392(50) 1_455 ? Na1 Cl2 3.0731(28) 2_566 ? Na1 Cl3 3.2982(30) 1_455 ? N11 C61 1.3261(68) . ? N11 C21 1.3672(69) . ? C21 O21 1.2906(60) . ? C21 C31 1.4059(71) . ? O21 Na1 2.4088(44) 2_566 ? C31 C41 1.3592(81) . ? C41 C51 1.3853(81) . ? C51 C61 1.3647(76) . ? C61 Cl1 1.7473(59) . ? N12 C62 1.3258(70) . ? N12 C22 1.3672(70) . ? C22 O22 1.2819(66) . ? C22 C32 1.4089(82) . ? O22 Na1 2.2885(41) 2_666 ? C32 C42 1.3632(81) . ? C42 C52 1.3871(86) . ? C52 C62 1.3759(86) . ? C62 Cl2 1.7453(57) . ? Cl2 Na1 3.0731(28) 2_566 ? N13 C63 1.3244(71) . ? N13 C23 1.3480(66) . ? N13 Na1 2.5392(50) 1_655 ? C23 O23 1.3196(65) . ? C23 C33 1.3978(74) . ? O23 Co1 2.0831(36) 2_666 ? C33 C43 1.3778(81) . ? C43 C53 1.3722(78) . ? C53 C63 1.3706(78) . ? C63 Cl3 1.7602(54) . ? Cl3 Na1 3.2982(30) 1_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O23 Co1 O23 83.40(15) . 2_666 ? O23 Co1 N11 104.14(16) . . ? O23 Co1 N11 150.05(16) 2_666 . ? O23 Co1 N12 152.05(16) . . ? O23 Co1 N12 98.71(16) 2_666 . ? N11 Co1 N12 87.96(17) . . ? O23 Co1 O22 90.57(15) . . ? O23 Co1 O22 88.72(15) 2_666 . ? N11 Co1 O22 119.66(17) . . ? N12 Co1 O22 61.74(16) . . ? O23 Co1 O21 107.40(15) . . ? O23 Co1 O21 88.52(14) 2_666 . ? N11 Co1 O21 61.53(15) . . ? N12 Co1 O21 100.52(16) . . ? O22 Co1 O21 161.36(14) . . ? O22 Na1 O21 99.10(16) 2_666 . ? O22 Na1 O21 119.23(16) 2_666 2_566 ? O21 Na1 O21 95.37(14) . 2_566 ? O22 Na1 N13 140.60(18) 2_666 1_455 ? O21 Na1 N13 96.60(15) . 1_455 ? O21 Na1 N13 94.80(15) 2_566 1_455 ? O22 Na1 Cl2 78.30(12) 2_666 2_566 ? O21 Na1 Cl2 173.07(14) . 2_566 ? O21 Na1 Cl2 80.54(11) 2_566 2_566 ? N13 Na1 Cl2 89.34(13) 1_455 2_566 ? O22 Na1 Cl3 90.21(12) 2_666 1_455 ? O21 Na1 Cl3 103.04(13) . 1_455 ? O21 Na1 Cl3 142.29(12) 2_566 1_455 ? N13 Na1 Cl3 50.96(12) 1_455 1_455 ? Cl2 Na1 Cl3 83.47(8) 2_566 1_455 ? C61 N11 C21 118.2(4) . . ? C61 N11 Co1 146.1(4) . . ? C21 N11 Co1 92.7(3) . . ? O21 C21 N11 112.8(4) . . ? O21 C21 C31 126.8(5) . . ? N11 C21 C31 120.4(5) . . ? C21 O21 Co1 92.0(3) . . ? C21 O21 Na1 134.0(4) . . ? Co1 O21 Na1 117.91(16) . . ? C21 O21 Na1 119.1(3) . 2_566 ? Co1 O21 Na1 109.60(16) . 2_566 ? Na1 O21 Na1 84.63(14) . 2_566 ? C41 C31 C21 117.8(6) . . ? C31 C41 C51 122.8(5) . . ? C61 C51 C41 115.3(5) . . ? N11 C61 C51 125.5(5) . . ? N11 C61 Cl1 114.9(4) . . ? C51 C61 Cl1 119.6(5) . . ? C62 N12 C22 118.7(5) . . ? C62 N12 Co1 149.8(4) . . ? C22 N12 Co1 91.4(3) . . ? O22 C22 N12 113.6(5) . . ? O22 C22 C32 126.9(5) . . ? N12 C22 C32 119.5(5) . . ? C22 O22 Co1 93.1(3) . . ? C22 O22 Na1 139.6(4) . 2_666 ? Co1 O22 Na1 125.68(19) . 2_666 ? C42 C32 C22 119.6(6) . . ? C32 C42 C52 120.9(6) . . ? C62 C52 C42 116.3(6) . . ? N12 C62 C52 125.0(6) . . ? N12 C62 Cl2 115.2(5) . . ? C52 C62 Cl2 119.8(5) . . ? C62 Cl2 Na1 102.2(2) . 2_566 ? C63 N13 C23 116.9(5) . . ? C63 N13 Na1 117.6(3) . 1_655 ? C23 N13 Na1 125.2(4) . 1_655 ? O23 C23 N13 116.6(5) . . ? O23 C23 C33 122.2(5) . . ? N13 C23 C33 121.1(5) . . ? C23 O23 Co1 134.7(3) . . ? C23 O23 Co1 119.0(3) . 2_666 ? Co1 O23 Co1 96.60(15) . 2_666 ? C43 C33 C23 118.9(5) . . ? C53 C43 C33 120.8(6) . . ? C63 C53 C43 115.5(6) . . ? N13 C63 C53 126.8(5) . . ? N13 C63 Cl3 114.4(4) . . ? C53 C63 Cl3 118.9(5) . . ? C63 Cl3 Na1 76.8(2) . 1_655 ? _refine_diff_density_max 0.529 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.106 #==END data_cobime _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C42 H45 Co2 N7 Na2 O8' _chemical_formula_weight 939.69 _chemical_melting_point ? _chemical_compound_source ? 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' 'Na' 'Na' 0.0362 0.0249 '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 11.618(5) _cell_length_b 12.931(5) _cell_length_c 17.540(6) _cell_angle_alpha 87.86(10) _cell_angle_beta 71.45(10) _cell_angle_gamma 64.36(10) _cell_volume 2236.6(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method ? _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 0.819 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6218 _diffrn_reflns_av_R_equivalents 0.1119 _diffrn_reflns_av_sigmaI/netI 0.0794 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 22.53 _reflns_number_total 5783 _reflns_number_observed 3455 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 25 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+4.9325P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5758 _refine_ls_number_parameters 838 _refine_ls_number_restraints 2149 _refine_ls_R_factor_all 0.1194 _refine_ls_R_factor_obs 0.0478 _refine_ls_wR_factor_all 0.1453 _refine_ls_wR_factor_obs 0.1122 _refine_ls_goodness_of_fit_all 1.012 _refine_ls_goodness_of_fit_obs 1.097 _refine_ls_restrained_S_all 0.973 _refine_ls_restrained_S_obs 0.977 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Na1 Na 0.4148(2) 0.6584(3) 0.65619(12) 0.0658(8) Uani 1 d U . Na2 Na 0.2316(2) 0.8410(2) 0.84566(12) 0.0605(7) Uani 1 d U . Co1 Co 0.10906(7) 1.03031(7) 1.01834(4) 0.0511(3) Uani 1 d U . Co2 Co 0.63567(15) 0.50813(13) 0.48736(9) 0.0255(3) Uani 0.50 d PU 1 N11 N 0.3791(13) 0.8222(6) 0.5593(4) 0.041(2) Uani 0.50 d PDU 1 C21 C 0.4205(9) 0.7512(6) 0.4908(4) 0.024(2) Uani 0.50 d PDU 1 C31 C 0.4278(12) 0.7973(7) 0.4165(4) 0.032(3) Uani 0.50 d PDU 1 H31 H 0.4560(12) 0.7498(7) 0.3692(4) 0.038 Uiso 0.50 calc PR 1 C41 C 0.3932(11) 0.9124(7) 0.4143(5) 0.042(3) Uani 0.50 d PDU 1 H41 H 0.3968(11) 0.9431(7) 0.3652(5) 0.050 Uiso 0.50 calc PR 1 C51 C 0.3528(11) 0.9844(7) 0.4843(5) 0.049(3) Uani 0.50 d PDU 1 H51 H 0.3321(11) 1.0623(7) 0.4824(5) 0.059 Uiso 0.50 calc PR 1 C61 C 0.3442(11) 0.9370(7) 0.5570(5) 0.048(3) Uani 0.50 d PDU 1 C1 C 0.2999(14) 1.0070(8) 0.6361(5) 0.065(4) Uani 0.50 d PDU 1 H1A H 0.3009(14) 0.9581(8) 0.6787(5) 0.098 Uiso 0.50 calc PR 1 H1B H 0.2097(14) 1.0675(8) 0.6468(5) 0.098 Uiso 0.50 calc PR 1 H1C H 0.3605(14) 1.0401(8) 0.6334(5) 0.098 Uiso 0.50 calc PR 1 O21 O 0.4513(11) 0.6446(6) 0.5005(4) 0.034(2) Uani 0.50 d PDU 1 N12 N 0.7758(11) 0.3739(6) 0.5364(4) 0.030(3) Uani 0.50 d PDU 1 C22 C 0.7186(10) 0.4450(6) 0.6078(5) 0.028(3) Uani 0.50 d PDU 1 C32 C 0.7526(15) 0.3997(8) 0.6756(5) 0.035(4) Uani 0.50 d PDU 1 H32 H 0.7122(15) 0.4461(8) 0.7249(5) 0.042 Uiso 0.50 calc PR 1 C42 C 0.8454(21) 0.2871(10) 0.6692(7) 0.045(4) Uani 0.50 d PDU 1 H42 H 0.8661(21) 0.2568(10) 0.7147(7) 0.054 Uiso 0.50 calc PR 1 C52 C 0.9093(16) 0.2174(9) 0.5953(6) 0.040(3) Uani 0.50 d PDU 1 H52 H 0.9778(16) 0.1429(9) 0.5896(6) 0.048 Uiso 0.50 calc PR 1 C62 C 0.8676(14) 0.2623(8) 0.5302(6) 0.030(3) Uani 0.50 d PDU 1 C2 C 0.9235(12) 0.1915(10) 0.4498(6) 0.045(4) Uani 0.50 d PDU 1 H2A H 0.8822(12) 0.2377(10) 0.4130(6) 0.067 Uiso 0.50 calc PR 1 H2B H 0.9041(12) 0.1260(10) 0.4565(6) 0.067 Uiso 0.50 calc PR 1 H2C H 1.0197(12) 0.1653(10) 0.4282(6) 0.067 Uiso 0.50 calc PR 1 O22 O 0.6322(6) 0.5478(5) 0.6050(4) 0.032(2) Uani 0.50 d PDU 1 N13 N 0.7410(8) 0.5959(6) 0.4113(4) 0.029(2) Uani 0.50 d PDU 1 C23 C 0.7714(11) 0.5239(8) 0.3452(4) 0.030(3) Uani 0.50 d PDU 1 C33 C 0.8393(18) 0.5423(11) 0.2683(4) 0.037(4) Uani 0.50 d PDU 1 H33 H 0.8582(18) 0.4956(11) 0.2226(4) 0.045 Uiso 0.50 calc PR 1 C43 C 0.8779(15) 0.6296(10) 0.2607(4) 0.047(4) Uani 0.50 d PDU 1 H43 H 0.9264(15) 0.6397(10) 0.2098(4) 0.057 Uiso 0.50 calc PR 1 C53 C 0.8457(10) 0.7031(8) 0.3279(4) 0.045(3) Uani 0.50 d PDU 1 H53 H 0.8701(10) 0.7633(8) 0.3226(4) 0.054 Uiso 0.50 calc PR 1 C63 C 0.7757(9) 0.6842(7) 0.4033(4) 0.034(2) Uani 0.50 d PDU 1 C3 C 0.7324(11) 0.7615(8) 0.4789(5) 0.049(3) Uani 0.50 d PDU 1 H31 H 0.6858(11) 0.7344(8) 0.5245(5) 0.073 Uiso 0.50 calc PR 1 H32 H 0.6730(11) 0.8388(8) 0.4738(5) 0.073 Uiso 0.50 calc PR 1 H33 H 0.8108(11) 0.7606(8) 0.4869(5) 0.073 Uiso 0.50 calc PR 1 O23 O 0.7278(11) 0.4467(7) 0.3619(6) 0.033(2) Uani 0.50 d PDU 1 Co2' Co 0.67108(15) 0.43836(13) 0.48511(9) 0.0255(3) Uani 0.50 d PU 2 N11' N 0.4250(10) 0.7505(6) 0.5419(4) 0.040(2) Uani 0.50 d PDU 2 C21' C 0.4637(16) 0.6760(6) 0.4754(4) 0.036(3) Uani 0.50 d PDU 2 C31' C 0.4792(10) 0.7174(7) 0.3994(4) 0.037(2) Uani 0.50 d PDU 2 H31' H 0.5057(10) 0.6682(7) 0.3533(4) 0.044 Uiso 0.50 calc PR 2 C41' C 0.4553(13) 0.8301(8) 0.3932(5) 0.040(3) Uani 0.50 d PDU 2 H41' H 0.4688(13) 0.8562(8) 0.3425(5) 0.048 Uiso 0.50 calc PR 2 C51' C 0.4115(12) 0.9061(7) 0.4613(5) 0.049(3) Uani 0.50 d PDU 2 H51' H 0.3932(12) 0.9832(7) 0.4572(5) 0.059 Uiso 0.50 calc PR 2 C61' C 0.3956(19) 0.8635(7) 0.5362(5) 0.054(4) Uani 0.50 d PDU 2 C1' C 0.3481(19) 0.9393(9) 0.6134(5) 0.081(5) Uani 0.50 d PDU 2 H1'1 H 0.3436(19) 0.8945(9) 0.6582(5) 0.122 Uiso 0.50 calc PR 2 H1'2 H 0.2599(19) 1.0011(9) 0.6207(5) 0.122 Uiso 0.50 calc PR 2 H1'3 H 0.4105(19) 0.9706(9) 0.6105(5) 0.122 Uiso 0.50 calc PR 2 O21' O 0.4886(7) 0.5710(5) 0.4881(4) 0.033(2) Uani 0.50 d PDU 2 N12' N 0.8056(10) 0.3206(8) 0.5387(4) 0.027(3) Uani 0.50 d PDU 2 C22' C 0.7318(8) 0.3855(7) 0.6128(4) 0.025(3) Uani 0.50 d PDU 2 C32' C 0.7731(14) 0.3460(10) 0.6795(5) 0.037(4) Uani 0.50 d PDU 2 H32' H 0.7234(14) 0.3887(10) 0.7303(5) 0.045 Uiso 0.50 calc PR 2 C42' C 0.8872(17) 0.2442(13) 0.6697(7) 0.044(3) Uani 0.50 d PDU 2 H42' H 0.9185(17) 0.2209(13) 0.7131(7) 0.052 Uiso 0.50 calc PR 2 C52' C 0.9563(16) 0.1754(12) 0.5955(7) 0.047(4) Uani 0.50 d PDU 2 H52' H 1.0280(16) 0.1028(12) 0.5900(7) 0.057 Uiso 0.50 calc PR 2 C62' C 0.9158(15) 0.2178(11) 0.5299(6) 0.037(3) Uani 0.50 d PDU 2 C2' C 0.9863(11) 0.1514(11) 0.4469(6) 0.050(4) Uani 0.50 d PDU 2 H2'1 H 0.9430(11) 0.1953(11) 0.4102(6) 0.075 Uiso 0.50 calc PR 2 H2'2 H 0.9813(11) 0.0790(11) 0.4489(6) 0.075 Uiso 0.50 calc PR 2 H2'3 H 1.0795(11) 0.1372(11) 0.4285(6) 0.075 Uiso 0.50 calc PR 2 O22' O 0.6319(7) 0.4812(6) 0.6115(4) 0.039(2) Uani 0.50 d PDU 2 N13' N 0.7868(8) 0.5208(7) 0.4150(4) 0.040(2) Uani 0.50 d PDU 2 C23' C 0.7995(13) 0.4669(9) 0.3453(5) 0.045(3) Uani 0.50 d PDU 2 C33' C 0.8574(21) 0.4985(14) 0.2707(5) 0.058(5) Uani 0.50 d PDU 2 H33' H 0.8671(21) 0.4626(14) 0.2226(5) 0.070 Uiso 0.50 calc PR 2 C43' C 0.8996(16) 0.5826(11) 0.2692(5) 0.069(5) Uani 0.50 d PDU 2 H43' H 0.9359(16) 0.6048(11) 0.2199(5) 0.083 Uiso 0.50 calc PR 2 C53' C 0.8890(12) 0.6351(10) 0.3405(6) 0.072(4) Uani 0.50 d PDU 2 H53' H 0.9195(12) 0.6910(10) 0.3393(6) 0.087 Uiso 0.50 calc PR 2 C63' C 0.8318(11) 0.6022(9) 0.4135(5) 0.051(3) Uani 0.50 d PDU 2 C3' C 0.8172(13) 0.6517(11) 0.4939(6) 0.079(4) Uani 0.50 d PDU 2 H3'A H 0.7752(13) 0.6172(11) 0.5363(6) 0.118 Uiso 0.50 calc PR 2 H3'B H 0.7619(13) 0.7337(11) 0.5014(6) 0.118 Uiso 0.50 calc PR 2 H3'C H 0.9050(13) 0.6358(11) 0.4956(6) 0.118 Uiso 0.50 calc PR 2 O23' O 0.7502(11) 0.3935(8) 0.3566(6) 0.043(3) Uani 0.50 d PDU 2 N14 N -0.2304(4) 1.2856(4) 1.0492(3) 0.066(2) Uani 1 d U . C24 C -0.1347(5) 1.2171(5) 0.9822(3) 0.051(2) Uani 1 d U . C34 C -0.1081(5) 1.2603(5) 0.9075(3) 0.0473(15) Uani 1 d U . H34 H -0.0397(5) 1.2121(5) 0.8618(3) 0.057 Uiso 1 calc R . C44 C -0.1834(5) 1.3731(5) 0.9026(3) 0.054(2) Uani 1 d U . H44 H -0.1691(5) 1.4026(5) 0.8531(3) 0.065 Uiso 1 calc R . C54 C -0.2816(6) 1.4442(5) 0.9716(4) 0.062(2) Uani 1 d U . H54 H -0.3323(6) 1.5224(5) 0.9696(4) 0.074 Uiso 1 calc R . C64 C -0.3029(6) 1.3972(5) 1.0435(4) 0.063(2) Uani 1 d U . C4 C -0.4087(7) 1.4681(6) 1.1223(4) 0.097(3) Uani 1 d U . H4A H -0.4074(7) 1.4194(6) 1.1650(4) 0.145 Uiso 1 calc R . H4B H -0.4967(7) 1.5011(6) 1.1166(4) 0.145 Uiso 1 calc R . H4C H -0.3890(7) 1.5288(6) 1.1352(4) 0.145 Uiso 1 calc R . O24 O -0.0660(3) 1.1067(3) 0.9903(2) 0.0555(11) Uani 1 d U . N15 N 0.2204(4) 0.9497(4) 1.0982(2) 0.0600(14) Uani 1 d DU . C25 C 0.1134(5) 1.0179(4) 1.1629(3) 0.0507(15) Uani 1 d DU . C35 C 0.1217(5) 1.0042(5) 1.2410(3) 0.065(2) Uani 1 d DU . H35 H 0.0491(5) 1.0505(5) 1.2858(3) 0.078 Uiso 1 calc R . C45 C 0.2386(6) 0.9216(5) 1.2502(3) 0.068(2) Uani 1 d DU . H45 H 0.2459(6) 0.9132(5) 1.3016(3) 0.082 Uiso 1 calc R . C55 C 0.3454(5) 0.8510(5) 1.1841(3) 0.073(2) Uani 1 d DU . H55 H 0.4236(5) 0.7942(5) 1.1909(3) 0.088 Uiso 1 calc R . C65 C 0.3349(5) 0.8655(5) 1.1073(3) 0.082(2) Uani 1 d DU . O25 O 0.0120(3) 1.0918(3) 1.1436(2) 0.0545(10) Uani 1 d DU . C5 C 0.4599(7) 0.8261(13) 1.0322(4) 0.072(5) Uani 0.50 d PDU 1 H5A H 0.4330(7) 0.8431(13) 0.9850(4) 0.108 Uiso 0.50 calc PR 1 H5B H 0.5139(7) 0.7444(13) 1.0290(4) 0.108 Uiso 0.50 calc PR 1 H5C H 0.5119(7) 0.8659(13) 1.0349(4) 0.108 Uiso 0.50 calc PR 1 C5' C 0.4189(9) 0.7667(8) 1.0391(5) 0.058(3) Uani 0.50 d PDU 2 H5'1 H 0.3987(9) 0.7921(8) 0.9907(5) 0.087 Uiso 0.50 calc PR 2 H5'2 H 0.3977(9) 0.7032(8) 1.0539(5) 0.087 Uiso 0.50 calc PR 2 H5'3 H 0.5135(9) 0.7424(8) 1.0296(5) 0.087 Uiso 0.50 calc PR 2 N16 N 0.1738(4) 1.1583(4) 0.9689(2) 0.0548(12) Uani 1 d DU . C26 C 0.2525(5) 1.0872(5) 0.8980(3) 0.0565(15) Uani 1 d DU . C36 C 0.3184(6) 1.1295(5) 0.8324(3) 0.073(2) Uani 1 d DU . H36 H 0.3726(6) 1.0825(5) 0.7835(3) 0.087 Uiso 1 calc R . C46 C 0.3029(6) 1.2400(6) 0.8404(3) 0.081(2) Uani 1 d DU . H46 H 0.3473(6) 1.2675(6) 0.7968(3) 0.097 Uiso 1 calc R . C56 C 0.2219(5) 1.3116(5) 0.9128(3) 0.068(2) Uani 1 d DU . H56 H 0.2120(5) 1.3865(5) 0.9185(3) 0.081 Uiso 1 calc R . C66 C 0.1560(5) 1.2683(4) 0.9765(3) 0.061(2) Uani 1 d DU . C6 C 0.0622(6) 1.3404(5) 1.0559(3) 0.092(3) Uani 1 d DU . H6A H 0.0270(6) 1.2951(5) 1.0917(3) 0.138 Uiso 1 calc R . H6B H -0.0113(6) 1.4062(5) 1.0472(3) 0.138 Uiso 1 calc R . H6C H 0.1109(6) 1.3659(5) 1.0795(3) 0.138 Uiso 1 calc R . O26 O 0.2582(3) 0.9856(3) 0.9002(2) 0.0557(10) Uani 1 d DU . N17 N 0.6795(7) 0.6879(9) 0.6915(6) 0.029(3) Uani 0.50 d PDU 1 H17 H 0.6712(7) 0.6462(9) 0.6585(6) 0.034 Uiso 0.50 calc PR 1 C27 C 0.5652(7) 0.7655(12) 0.7502(7) 0.034(3) Uani 0.50 d PDU 1 C37 C 0.5810(7) 0.8321(10) 0.8035(6) 0.032(3) Uani 0.50 d PDU 1 H37 H 0.5054(7) 0.8851(10) 0.8441(6) 0.038 Uiso 0.50 calc PR 1 C47 C 0.7073(8) 0.8196(10) 0.7961(6) 0.046(3) Uani 0.50 d PDU 1 H47 H 0.7167(8) 0.8636(10) 0.8323(6) 0.055 Uiso 0.50 calc PR 1 C57 C 0.8221(7) 0.7421(10) 0.7352(6) 0.048(3) Uani 0.50 d PDU 1 H57 H 0.9075(7) 0.7355(10) 0.7291(6) 0.058 Uiso 0.50 calc PR 1 C67 C 0.8050(7) 0.6750(8) 0.6840(5) 0.031(3) Uani 0.50 d PDU 1 C7 C 0.9210(7) 0.5863(8) 0.6174(5) 0.046(3) Uani 0.50 d PDU 1 H7A H 0.8870(7) 0.5498(8) 0.5894(5) 0.069 Uiso 0.50 calc PR 1 H7B H 0.9828(7) 0.5292(8) 0.6401(5) 0.069 Uiso 0.50 calc PR 1 H7C H 0.9673(7) 0.6232(8) 0.5800(5) 0.069 Uiso 0.50 calc PR 1 O27 O 0.4550(8) 0.7695(12) 0.7472(8) 0.034(3) Uani 0.50 d PDU 1 N17' N 0.5352(5) 0.8118(7) 0.8204(5) 0.037(3) Uani 0.50 d PGDU 2 H17' H 0.4538(5) 0.8575(7) 0.8499(5) 0.045 Uiso 0.50 calc PR 2 C27' C 0.5575(7) 0.7321(8) 0.7599(6) 0.033(4) Uani 0.50 d PGDU 2 C37' C 0.6891(8) 0.6582(8) 0.7122(6) 0.044(5) Uani 0.50 d PGDU 2 H37' H 0.7040(11) 0.6048(11) 0.6717(8) 0.053 Uiso 0.50 calc PR 2 C47' C 0.7984(6) 0.6640(8) 0.7249(5) 0.059(4) Uani 0.50 d PGDU 2 H47' H 0.8864(7) 0.6146(11) 0.6930(7) 0.071 Uiso 0.50 calc PR 2 C57' C 0.7760(5) 0.7438(8) 0.7854(5) 0.055(4) Uani 0.50 d PGDU 2 H57' H 0.8491(6) 0.7477(12) 0.7940(8) 0.066 Uiso 0.50 calc PR 2 C67' C 0.6445(6) 0.8177(7) 0.8332(5) 0.037(3) Uani 0.50 d PGDU 2 C7' C 0.6095(9) 0.9056(8) 0.8998(5) 0.050(3) Uani 0.50 d PDU 2 H7'1 H 0.5128(9) 0.9463(8) 0.9241(5) 0.075 Uiso 0.50 calc PR 2 H7'2 H 0.6449(9) 0.9592(8) 0.8783(5) 0.075 Uiso 0.50 calc PR 2 H7'3 H 0.6483(9) 0.8678(8) 0.9399(5) 0.075 Uiso 0.50 calc PR 2 O27' O 0.4473(9) 0.7351(12) 0.7570(8) 0.038(4) Uani 0.50 d PDU 2 O1 O 0.1935(4) 0.7387(5) 0.7505(3) 0.116(2) Uani 1 d U . H1D H 0.1718(4) 0.6902(5) 0.7702(3) 0.139 Uiso 1 calc R . H1E H 0.1388(4) 0.7814(5) 0.7314(3) 0.139 Uiso 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 Na1 0.0427(12) 0.142(2) 0.0227(11) 0.0069(12) -0.0105(9) -0.0500(14) Na2 0.0400(12) 0.0586(15) 0.0334(12) 0.0141(10) 0.0100(9) 0.0054(11) Co1 0.0241(4) 0.0566(6) 0.0366(4) 0.0208(4) 0.0041(3) 0.0024(4) Co2 0.0252(7) 0.0264(8) 0.0211(4) -0.0015(7) -0.0051(4) -0.0098(7) N11 0.032(6) 0.037(5) 0.049(5) -0.014(4) -0.022(5) -0.002(5) C21 0.016(5) 0.032(5) 0.037(5) 0.006(4) -0.015(5) -0.016(4) C31 0.028(7) 0.043(6) 0.034(5) 0.006(5) -0.012(5) -0.024(6) C41 0.047(7) 0.042(6) 0.049(6) 0.018(5) -0.030(6) -0.023(6) C51 0.040(7) 0.041(6) 0.064(6) 0.003(5) -0.030(6) -0.007(6) C61 0.033(6) 0.043(5) 0.049(6) -0.022(5) -0.014(6) 0.002(6) C1 0.082(10) 0.037(8) 0.072(8) -0.017(6) -0.044(8) -0.008(8) O21 0.037(4) 0.031(4) 0.036(4) 0.009(4) -0.018(4) -0.013(4) N12 0.033(5) 0.034(6) 0.032(5) 0.007(4) -0.017(4) -0.020(4) C22 0.050(6) 0.031(6) 0.024(5) 0.011(4) -0.010(4) -0.039(5) C32 0.037(7) 0.041(8) 0.031(5) 0.002(5) -0.011(5) -0.021(6) C42 0.051(14) 0.055(11) 0.033(6) 0.013(6) -0.025(7) -0.020(8) C52 0.040(10) 0.036(8) 0.048(6) 0.011(5) -0.025(6) -0.015(6) C62 0.020(12) 0.041(10) 0.031(5) 0.000(5) -0.009(6) -0.014(6) C2 0.033(9) 0.042(8) 0.035(6) -0.002(5) -0.008(6) 0.003(6) O22 0.032(3) 0.038(4) 0.027(3) 0.006(3) -0.010(3) -0.016(3) N13 0.023(4) 0.032(5) 0.030(4) 0.008(4) -0.009(3) -0.010(4) C23 0.025(6) 0.039(7) 0.018(5) 0.003(4) -0.002(4) -0.011(6) C33 0.028(7) 0.048(10) 0.028(5) 0.008(5) -0.005(5) -0.012(8) C43 0.040(8) 0.057(10) 0.040(5) 0.024(5) -0.013(5) -0.021(8) C53 0.033(6) 0.051(7) 0.053(5) 0.022(5) -0.015(5) -0.021(6) C63 0.025(5) 0.038(6) 0.042(5) 0.021(4) -0.017(4) -0.014(5) C3 0.059(7) 0.037(7) 0.054(6) 0.008(5) -0.024(6) -0.022(6) O23 0.040(5) 0.029(6) 0.026(4) 0.001(4) -0.009(3) -0.011(5) Co2' 0.0252(7) 0.0264(8) 0.0211(4) -0.0015(7) -0.0051(4) -0.0098(7) N11' 0.047(6) 0.032(4) 0.042(4) -0.005(4) -0.015(5) -0.016(5) C21' 0.031(7) 0.024(5) 0.038(5) -0.001(4) -0.019(5) 0.006(6) C31' 0.036(6) 0.033(5) 0.030(4) 0.002(4) -0.005(5) -0.009(5) C41' 0.042(8) 0.041(7) 0.037(6) 0.009(5) -0.010(6) -0.022(6) C51' 0.059(7) 0.037(6) 0.046(6) 0.004(5) -0.017(6) -0.018(6) C61' 0.059(9) 0.039(6) 0.046(6) -0.016(5) -0.014(7) -0.009(8) C1' 0.140(15) 0.050(9) 0.048(7) -0.008(7) -0.017(10) -0.045(11) O21' 0.030(4) 0.030(4) 0.041(4) 0.004(3) -0.018(3) -0.011(4) N12' 0.024(8) 0.037(8) 0.021(4) 0.003(4) -0.004(4) -0.018(5) C22' 0.030(5) 0.041(6) 0.019(5) -0.001(5) -0.008(4) -0.030(4) C32' 0.048(9) 0.045(11) 0.019(5) 0.004(6) -0.013(5) -0.021(7) C42' 0.040(10) 0.055(10) 0.043(6) 0.010(6) -0.020(5) -0.022(7) C52' 0.038(10) 0.047(9) 0.048(6) 0.009(6) -0.020(5) -0.007(6) C62' 0.025(9) 0.039(8) 0.039(6) 0.000(5) -0.009(5) -0.009(5) C2' 0.037(9) 0.060(10) 0.044(6) -0.019(7) -0.006(6) -0.016(7) O22' 0.035(4) 0.058(5) 0.024(3) 0.003(4) -0.012(3) -0.020(4) N13' 0.026(4) 0.037(5) 0.041(4) 0.002(4) 0.003(4) -0.009(4) C23' 0.031(7) 0.053(9) 0.036(5) 0.009(5) -0.001(5) -0.012(7) C33' 0.039(8) 0.074(12) 0.047(6) 0.030(6) -0.010(6) -0.017(9) C43' 0.032(8) 0.078(11) 0.078(7) 0.048(7) -0.007(7) -0.018(8) C53' 0.039(7) 0.070(9) 0.103(7) 0.038(7) -0.014(7) -0.028(6) C63' 0.028(6) 0.037(7) 0.082(6) 0.015(6) -0.012(5) -0.016(5) C3' 0.067(9) 0.076(10) 0.107(8) -0.008(8) -0.015(8) -0.053(8) O23' 0.046(6) 0.048(8) 0.031(4) 0.003(5) -0.006(4) -0.022(6) N14 0.033(3) 0.063(3) 0.053(3) 0.025(3) 0.005(2) 0.005(2) C24 0.022(3) 0.056(4) 0.053(3) 0.024(3) -0.004(2) -0.005(3) C34 0.035(3) 0.051(3) 0.044(3) 0.019(3) -0.008(2) -0.013(3) C44 0.045(3) 0.058(4) 0.049(3) 0.026(3) -0.014(3) -0.016(3) C54 0.045(3) 0.052(4) 0.057(4) 0.020(3) -0.014(3) 0.003(3) C64 0.039(3) 0.057(4) 0.055(4) 0.018(3) -0.002(3) 0.001(3) C4 0.068(5) 0.075(5) 0.065(4) 0.008(4) 0.009(4) 0.019(4) O24 0.026(2) 0.050(2) 0.066(3) 0.029(2) -0.007(2) -0.004(2) N15 0.046(3) 0.067(3) 0.041(3) 0.020(2) -0.012(2) -0.005(2) C25 0.056(3) 0.044(4) 0.045(3) 0.007(3) -0.010(3) -0.021(3) C35 0.078(4) 0.084(5) 0.039(3) -0.007(3) -0.014(3) -0.042(4) C45 0.089(4) 0.104(6) 0.053(4) 0.032(4) -0.040(3) -0.070(4) C55 0.073(4) 0.094(5) 0.062(4) 0.041(4) -0.038(3) -0.038(4) C65 0.057(4) 0.092(5) 0.051(4) 0.024(3) -0.020(3) 0.007(4) O25 0.051(2) 0.037(2) 0.055(2) -0.001(2) -0.006(2) -0.009(2) C5 0.030(6) 0.106(13) 0.058(6) -0.006(8) -0.018(5) -0.006(7) C5' 0.025(6) 0.063(8) 0.088(8) 0.020(6) -0.032(6) -0.013(5) N16 0.024(2) 0.078(3) 0.042(3) 0.032(2) -0.011(2) -0.007(2) C26 0.034(3) 0.102(4) 0.041(3) 0.034(3) -0.020(3) -0.035(3) C36 0.062(4) 0.144(6) 0.038(3) 0.031(4) -0.015(3) -0.071(5) C46 0.073(4) 0.158(7) 0.050(4) 0.044(4) -0.027(3) -0.083(5) C56 0.050(4) 0.111(5) 0.065(4) 0.044(4) -0.036(3) -0.047(4) C66 0.033(3) 0.078(4) 0.061(4) 0.041(3) -0.023(3) -0.013(3) C6 0.056(4) 0.079(5) 0.080(5) 0.024(4) 0.004(4) 0.003(4) O26 0.037(2) 0.095(3) 0.034(2) 0.022(2) -0.006(2) -0.033(2) N17 0.026(4) 0.019(5) 0.030(5) -0.008(4) -0.005(4) -0.003(4) C27 0.026(4) 0.038(7) 0.026(6) 0.001(5) -0.013(4) -0.002(5) C37 0.019(5) 0.032(7) 0.027(6) -0.019(5) 0.000(5) 0.000(5) C47 0.031(7) 0.057(8) 0.041(7) -0.021(6) -0.010(5) -0.012(6) C57 0.031(5) 0.055(8) 0.051(7) -0.017(6) -0.013(5) -0.010(5) C67 0.026(4) 0.033(6) 0.031(6) -0.004(4) -0.013(4) -0.008(4) C7 0.023(5) 0.049(7) 0.046(6) -0.014(5) -0.003(4) -0.003(5) O27 0.027(4) 0.049(8) 0.020(4) 0.009(5) -0.002(3) -0.018(4) N17' 0.022(5) 0.046(6) 0.033(6) -0.008(4) -0.005(4) -0.008(4) C27' 0.029(4) 0.035(8) 0.032(7) -0.006(6) -0.003(4) -0.017(5) C37' 0.023(5) 0.052(10) 0.045(8) -0.013(7) -0.011(5) -0.006(5) C47' 0.023(5) 0.058(9) 0.079(10) -0.029(7) -0.020(6) 0.002(6) C57' 0.024(6) 0.055(8) 0.081(9) -0.020(7) -0.020(6) -0.009(6) C67' 0.023(6) 0.038(6) 0.051(8) -0.002(5) -0.014(5) -0.013(5) C7' 0.058(7) 0.054(7) 0.043(7) -0.002(5) -0.024(5) -0.025(6) O27' 0.026(4) 0.058(8) 0.022(4) 0.005(5) -0.001(3) -0.017(4) O1 0.039(2) 0.158(5) 0.118(4) -0.046(4) 0.023(3) -0.045(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 Na1 O22 2.182(7) . ? Na1 O27' 2.266(10) . ? Na1 N11' 2.290(7) . ? Na1 O1 2.352(6) . ? Na1 O23' 2.360(10) 2_666 ? Na1 O27 2.461(10) . ? Na1 O22' 2.470(8) . ? Na1 O21 2.628(7) . ? Na1 N11 2.640(8) . ? Na1 O23 2.646(9) 2_666 ? Na1 O21' 2.917(7) . ? Na1 C21' 3.056(7) . ? Na2 O27' 2.299(11) . ? Na2 O26 2.309(5) . ? Na2 O27 2.401(11) . ? Na2 N14 2.421(5) 2_577 ? Na2 O1 2.424(6) . ? Na2 O25 2.518(5) 2_577 ? Na2 O24 2.817(5) 2_577 ? Na2 C24 3.058(6) 2_577 ? Na2 Co1 3.462(5) . ? Na2 Co1 3.565(6) 2_577 ? Co1 O24 2.053(4) . ? Co1 O24 2.061(4) 2_577 ? Co1 O25 2.124(4) . ? Co1 O26 2.137(5) . ? Co1 N15 2.145(4) . ? Co1 N16 2.147(5) . ? Co1 Na2 3.565(6) 2_577 ? Co2 O21' 2.042(7) 2_666 ? Co2 O21 2.049(10) . ? Co2 O23 2.125(10) . ? Co2 O22 2.128(7) . ? Co2 N13 2.148(7) . ? Co2 N12 2.177(7) . ? N11 C21 1.361(6) . ? N11 C61 1.362(6) . ? C21 O21 1.285(6) . ? C21 C31 1.405(6) . ? C31 C41 1.367(7) . ? C41 C51 1.391(7) . ? C51 C61 1.389(6) . ? C61 C1 1.497(7) . ? N12 C62 1.355(6) . ? N12 C22 1.372(6) . ? C22 O22 1.283(6) . ? C22 C32 1.400(6) . ? C32 C42 1.368(7) . ? C42 C52 1.393(7) . ? C52 C62 1.390(6) . ? C62 C2 1.501(7) . ? N13 C63 1.355(6) . ? N13 C23 1.368(6) . ? C23 O23 1.289(6) . ? C23 C33 1.400(6) . ? C33 C43 1.372(7) . ? C43 C53 1.389(7) . ? C53 C63 1.391(6) . ? C63 C3 1.500(7) . ? O23 Na1 2.646(9) 2_666 ? Co2' O21' 1.821(7) 2_666 ? Co2' O21' 2.056(7) . ? Co2' O21 2.075(10) 2_666 ? Co2' N12' 2.101(7) . ? Co2' N13' 2.132(7) . ? Co2' O23' 2.140(10) . ? Co2' O22' 2.159(7) . ? Co2' Na1 3.404(3) 2_666 ? N11' C61' 1.356(6) . ? N11' C21' 1.366(6) . ? C21' O21' 1.286(6) . ? C21' C31' 1.405(6) . ? C31' C41' 1.367(7) . ? C41' C51' 1.385(7) . ? C51' C61' 1.394(6) . ? C61' C1' 1.500(7) . ? O21' O21' 1.792(12) 2_666 ? O21' Co2' 1.821(7) 2_666 ? N12' C62' 1.358(6) . ? N12' C22' 1.370(6) . ? C22' O22' 1.285(6) . ? C22' C32' 1.401(6) . ? C32' C42' 1.372(7) . ? C42' C52' 1.391(7) . ? C52' C62' 1.386(6) . ? C62' C2' 1.501(7) . ? N13' C63' 1.359(6) . ? N13' C23' 1.364(6) . ? C23' O23' 1.286(6) . ? C23' C33' 1.403(6) . ? C33' C43' 1.369(7) . ? C43' C53' 1.389(7) . ? C53' C63' 1.387(6) . ? C63' C3' 1.501(7) . ? O23' Na1 2.360(9) 2_666 ? N14 C64 1.338(7) . ? N14 C24 1.340(7) . ? N14 Na2 2.421(5) 2_577 ? C24 O24 1.330(6) . ? C24 C34 1.400(7) . ? C24 Na2 3.058(6) 2_577 ? C34 C44 1.355(8) . ? C44 C54 1.381(8) . ? C54 C64 1.377(8) . ? C64 C4 1.517(9) . ? O24 Co1 2.061(4) 2_577 ? O24 Na2 2.817(5) 2_577 ? N15 C25 1.356(5) . ? N15 C65 1.360(5) . ? C25 O25 1.293(5) . ? C25 C35 1.402(5) . ? C35 C45 1.372(6) . ? C45 C55 1.378(6) . ? C55 C65 1.390(5) . ? C65 C5 1.515(7) . ? C65 C5' 1.519(7) . ? O25 Na2 2.518(5) 2_577 ? N16 C66 1.352(5) . ? N16 C26 1.365(5) . ? C26 O26 1.286(5) . ? C26 C36 1.401(5) . ? C36 C46 1.368(6) . ? C46 C56 1.390(6) . ? C56 C66 1.388(5) . ? C66 C6 1.499(6) . ? N17 C67 1.356(6) . ? N17 C27 1.372(6) . ? C27 O27 1.276(6) . ? C27 C37 1.399(6) . ? C37 C47 1.368(6) . ? C47 C57 1.393(7) . ? C57 C67 1.385(6) . ? C67 C7 1.503(7) . ? N17' C27' 1.39 . ? N17' C67' 1.39 . ? C27' O27' 1.281(5) . ? C27' C37' 1.39 . ? C37' C47' 1.39 . ? C47' C57' 1.39 . ? C57' C67' 1.39 . ? C67' C7' 1.490(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 O27' Na1 N11' 115.6(4) . . ? O22 Na1 O1 159.2(3) . . ? O27' Na1 O1 79.9(3) . . ? N11' Na1 O1 111.3(3) . . ? O27' Na1 O23' 136.5(4) . 2_666 ? N11' Na1 O23' 93.7(4) . 2_666 ? O1 Na1 O23' 58.9(3) . 2_666 ? O22 Na1 O27 90.1(3) . . ? O1 Na1 O27 83.7(3) . . ? O27' Na1 O22' 98.7(4) . . ? N11' Na1 O22' 102.0(3) . . ? O1 Na1 O22' 143.6(3) . . ? O23' Na1 O22' 106.1(3) 2_666 . ? O22 Na1 O21 78.3(3) . . ? O1 Na1 O21 119.7(3) . . ? O27 Na1 O21 134.6(4) . . ? O22 Na1 N11 102.1(3) . . ? O1 Na1 N11 97.9(3) . . ? O27 Na1 N11 91.1(4) . . ? O21 Na1 N11 50.3(2) . . ? O22 Na1 O23 111.7(3) . 2_666 ? O1 Na1 O23 67.5(3) . 2_666 ? O27 Na1 O23 148.0(4) . 2_666 ? O21 Na1 O23 74.8(3) . 2_666 ? N11 Na1 O23 106.0(3) . 2_666 ? O27' Na1 O21' 152.9(3) . . ? N11' Na1 O21' 49.4(2) . . ? O1 Na1 O21' 125.0(2) . . ? O23' Na1 O21' 70.6(3) 2_666 . ? O22' Na1 O21' 68.1(2) . . ? O27' Na1 C21' 136.8(4) . . ? N11' Na1 C21' 24.68(15) . . ? O1 Na1 C21' 120.8(4) . . ? O23' Na1 C21' 81.3(4) 2_666 . ? O22' Na1 C21' 85.0(3) . . ? O21' Na1 C21' 24.73(13) . . ? O27' Na2 O26 100.6(3) . . ? O26 Na2 O27 91.4(3) . . ? O27' Na2 N14 99.8(4) . 2_577 ? O26 Na2 N14 103.3(2) . 2_577 ? O27 Na2 N14 109.8(4) . 2_577 ? O27' Na2 O1 77.8(3) . . ? O26 Na2 O1 158.5(2) . . ? O27 Na2 O1 83.5(3) . . ? N14 Na2 O1 98.1(2) 2_577 . ? O27' Na2 O25 140.5(3) . 2_577 ? O26 Na2 O25 110.6(2) . 2_577 ? O27 Na2 O25 141.3(3) . 2_577 ? N14 Na2 O25 96.1(2) 2_577 2_577 ? O1 Na2 O25 64.2(2) . 2_577 ? O27' Na2 O24 144.8(4) . 2_577 ? O26 Na2 O24 73.2(2) . 2_577 ? O27 Na2 O24 148.5(3) . 2_577 ? N14 Na2 O24 50.8(2) 2_577 2_577 ? O1 Na2 O24 120.3(2) . 2_577 ? O25 Na2 O24 70.1(2) 2_577 2_577 ? O27' Na2 C24 122.5(4) . 2_577 ? O26 Na2 C24 87.9(2) . 2_577 ? O27 Na2 C24 130.6(4) . 2_577 ? N14 Na2 C24 25.0(2) 2_577 2_577 ? O1 Na2 C24 111.3(2) . 2_577 ? O25 Na2 C24 83.3(2) 2_577 2_577 ? O24 Na2 C24 25.75(13) 2_577 2_577 ? O27' Na2 Co1 131.8(2) . . ? O26 Na2 Co1 37.11(10) . . ? O27 Na2 Co1 125.7(3) . . ? N14 Na2 Co1 78.1(2) 2_577 . ? O1 Na2 Co1 150.34(13) . . ? O25 Na2 Co1 86.7(2) 2_577 . ? O24 Na2 Co1 36.53(11) 2_577 . ? C24 Na2 Co1 56.02(14) 2_577 . ? O27' Na2 Co1 172.0(3) . 2_577 ? O26 Na2 Co1 86.90(15) . 2_577 ? O27 Na2 Co1 174.7(4) . 2_577 ? N14 Na2 Co1 75.5(2) 2_577 2_577 ? O1 Na2 Co1 96.3(2) . 2_577 ? O25 Na2 Co1 35.92(10) 2_577 2_577 ? O24 Na2 Co1 35.11(11) 2_577 2_577 ? C24 Na2 Co1 54.39(14) 2_577 2_577 ? Co1 Na2 Co1 54.17(11) . 2_577 ? O27' Na2 Na1 37.8(2) . . ? O26 Na2 Na1 131.83(13) . . ? O27 Na2 Na1 43.1(2) . . ? N14 Na2 Na1 106.6(2) 2_577 . ? O1 Na2 Na1 40.52(11) . . ? O25 Na2 Na1 102.9(2) 2_577 . ? O24 Na2 Na1 153.13(14) 2_577 . ? C24 Na2 Na1 130.5(2) 2_577 . ? Co1 Na2 Na1 168.57(9) . . ? Co1 Na2 Na1 136.74(12) 2_577 . ? O24 Co1 O24 77.8(2) . 2_577 ? O24 Co1 O25 94.8(2) . . ? O24 Co1 O25 102.2(2) 2_577 . ? O24 Co1 O26 100.8(2) . . ? O24 Co1 O26 94.5(2) 2_577 . ? O25 Co1 O26 159.2(2) . . ? O24 Co1 N15 152.8(2) . . ? O24 Co1 N15 91.9(2) 2_577 . ? O25 Co1 N15 62.5(2) . . ? O26 Co1 N15 105.1(2) . . ? O24 Co1 N16 92.9(2) . . ? O24 Co1 N16 153.6(2) 2_577 . ? O25 Co1 N16 103.2(2) . . ? O26 Co1 N16 62.6(2) . . ? N15 Co1 N16 106.1(2) . . ? O24 Co1 Na2 85.1(2) . . ? O24 Co1 Na2 54.45(13) 2_577 . ? O25 Co1 Na2 156.27(12) . . ? O26 Co1 Na2 40.67(13) . . ? N15 Co1 Na2 109.55(15) . . ? N16 Co1 Na2 100.53(13) . . ? O24 Co1 Na2 52.11(12) . 2_577 ? O24 Co1 Na2 82.26(15) 2_577 2_577 ? O25 Co1 Na2 44.08(14) . 2_577 ? O26 Co1 Na2 152.86(12) . 2_577 ? N15 Co1 Na2 101.95(13) . 2_577 ? N16 Co1 Na2 111.69(15) . 2_577 ? Na2 Co1 Na2 125.83(11) . 2_577 ? O21 Co2 O23 106.3(4) . . ? O21 Co2 O22 94.1(3) . . ? O23 Co2 O22 155.4(3) . . ? O21 Co2 N13 91.6(3) . . ? O23 Co2 N13 62.8(2) . . ? O22 Co2 N13 103.8(3) . . ? O21 Co2 N12 151.6(3) . . ? O23 Co2 N12 100.8(4) . . ? O22 Co2 N12 62.3(2) . . ? N13 Co2 N12 108.4(4) . . ? O21' Co2 Na1 80.2(2) 2_666 . ? O21 Co2 Na1 54.4(2) . . ? O23 Co2 Na1 160.6(3) . . ? O22 Co2 Na1 42.2(2) . . ? N13 Co2 Na1 114.3(2) . . ? N12 Co2 Na1 98.2(2) . . ? C21 N11 C61 121.1(5) . . ? C21 N11 Na1 95.8(4) . . ? C61 N11 Na1 143.0(4) . . ? O21 C21 N11 115.4(5) . . ? O21 C21 C31 125.4(6) . . ? N11 C21 C31 119.2(5) . . ? O21 C21 Na1 57.3(4) . . ? N11 C21 Na1 58.2(3) . . ? C31 C21 Na1 176.1(6) . . ? C41 C31 C21 119.6(5) . . ? C31 C41 C51 120.9(5) . . ? C61 C51 C41 118.2(5) . . ? N11 C61 C51 120.8(5) . . ? N11 C61 C1 116.5(6) . . ? C51 C61 C1 122.7(6) . . ? C21 O21 Co2 130.2(8) . . ? C21 O21 Na1 98.5(5) . . ? Co2 O21 Na1 86.3(3) . . ? C62 N12 C22 121.0(5) . . ? C62 N12 Co2 148.9(6) . . ? C22 N12 Co2 89.2(4) . . ? O22 C22 N12 114.1(5) . . ? O22 C22 C32 126.8(6) . . ? N12 C22 C32 119.0(5) . . ? C42 C32 C22 119.9(5) . . ? C32 C42 C52 120.7(5) . . ? C62 C52 C42 118.1(5) . . ? N12 C62 C52 121.0(5) . . ? N12 C62 C2 116.8(6) . . ? C52 C62 C2 122.1(6) . . ? C22 O22 Co2 93.8(5) . . ? C22 O22 Na1 139.0(7) . . ? Co2 O22 Na1 96.9(3) . . ? C63 N13 C23 121.0(5) . . ? C63 N13 Co2 148.7(4) . . ? C23 N13 Co2 90.0(4) . . ? O23 C23 N13 113.9(5) . . ? O23 C23 C33 126.8(6) . . ? N13 C23 C33 119.2(5) . . ? C43 C33 C23 119.6(5) . . ? C33 C43 C53 120.9(5) . . ? C43 C53 C63 118.1(5) . . ? N13 C63 C53 121.1(5) . . ? N13 C63 C3 117.0(5) . . ? C53 C63 C3 121.9(5) . . ? C23 O23 Co2 93.2(4) . . ? C23 O23 Na1 152.0(7) . 2_666 ? Co2 O23 Na1 101.5(4) . 2_666 ? O21' Co2' O21' 54.7(3) 2_666 . ? O21' Co2' N12' 112.8(4) 2_666 . ? O21' Co2' N12' 153.6(3) . . ? O21' Co2' N13' 144.9(3) 2_666 . ? O21' Co2' N13' 93.8(3) . . ? N12' Co2' N13' 102.2(4) . . ? O21' Co2' O23' 102.0(4) 2_666 . ? O21' Co2' O23' 96.0(4) . . ? N12' Co2' O23' 110.0(4) . . ? N13' Co2' O23' 62.7(2) . . ? O21' Co2' O22' 89.7(3) 2_666 . ? O21' Co2' O22' 92.2(3) . . ? N12' Co2' O22' 62.9(2) . . ? N13' Co2' O22' 108.3(3) . . ? O23' Co2' O22' 168.2(3) . . ? O21' Co2' Na1 58.9(2) 2_666 2_666 ? O21' Co2' Na1 75.6(2) . 2_666 ? O21 Co2' Na1 50.5(2) 2_666 2_666 ? N12' Co2' Na1 120.3(3) . 2_666 ? N13' Co2' Na1 102.1(2) . 2_666 ? O23' Co2' Na1 43.3(3) . 2_666 ? O22' Co2' Na1 147.9(2) . 2_666 ? C61' N11' C21' 121.5(5) . . ? C61' N11' Na1 127.7(4) . . ? C21' N11' Na1 110.9(4) . . ? O21' C21' N11' 116.0(6) . . ? O21' C21' C31' 125.4(6) . . ? N11' C21' C31' 118.5(5) . . ? O21' C21' Na1 71.6(4) . . ? N11' C21' Na1 44.4(3) . . ? C31' C21' Na1 162.9(5) . . ? C41' C31' C21' 120.0(5) . . ? C31' C41' C51' 121.0(5) . . ? C41' C51' C61' 118.0(5) . . ? N11' C61' C51' 120.9(5) . . ? N11' C61' C1' 117.3(6) . . ? C51' C61' C1' 121.8(6) . . ? C21' O21' O21' 175.6(9) . 2_666 ? C21' O21' Co2' 107.2(8) . 2_666 ? O21' O21' Co2' 69.4(4) 2_666 2_666 ? C21' O21' Co2' 127.4(8) . . ? O21' O21' Co2' 56.0(4) 2_666 . ? Co2' O21' Co2' 125.3(3) 2_666 . ? C21' O21' Na1 83.7(4) . . ? O21' O21' Na1 93.4(4) 2_666 . ? Co2' O21' Na1 88.7(3) 2_666 . ? Co2' O21' Na1 94.1(3) . . ? C62' N12' C22' 120.9(5) . . ? C62' N12' Co2' 147.4(5) . . ? C22' N12' Co2' 91.6(4) . . ? O22' C22' N12' 113.8(5) . . ? O22' C22' C32' 127.0(6) . . ? N12' C22' C32' 119.2(5) . . ? C42' C32' C22' 119.8(5) . . ? C32' C42' C52' 120.5(6) . . ? C62' C52' C42' 118.5(5) . . ? N12' C62' C52' 121.0(5) . . ? N12' C62' C2' 116.6(6) . . ? C52' C62' C2' 122.4(6) . . ? C22' O22' Co2' 91.5(4) . . ? C22' O22' Na1 161.4(5) . . ? Co2' O22' Na1 105.4(3) . . ? C63' N13' C23' 121.4(5) . . ? C63' N13' Co2' 147.5(5) . . ? C23' N13' Co2' 90.5(4) . . ? O23' C23' N13' 114.1(6) . . ? O23' C23' C33' 126.8(6) . . ? N13' C23' C33' 119.0(5) . . ? C43' C33' C23' 119.6(5) . . ? C33' C43' C53' 120.9(5) . . ? C63' C53' C43' 118.4(5) . . ? N13' C63' C53' 120.6(5) . . ? N13' C63' C3' 116.4(5) . . ? C53' C63' C3' 123.0(6) . . ? C23' O23' Co2' 92.3(5) . . ? C23' O23' Na1 147.7(9) . 2_666 ? Co2' O23' Na1 98.2(4) . 2_666 ? C64 N14 C24 118.7(5) . . ? C64 N14 Na2 136.1(4) . 2_577 ? C24 N14 Na2 105.1(4) . 2_577 ? O24 C24 N14 116.8(5) . . ? O24 C24 C34 121.7(5) . . ? N14 C24 C34 121.5(5) . . ? O24 C24 Na2 67.0(3) . 2_577 ? N14 C24 Na2 49.8(3) . 2_577 ? C34 C24 Na2 171.2(4) . 2_577 ? C44 C34 C24 119.1(5) . . ? C34 C44 C54 119.6(5) . . ? C64 C54 C44 118.7(6) . . ? N14 C64 C54 122.4(6) . . ? N14 C64 C4 115.1(5) . . ? C54 C64 C4 122.6(6) . . ? C24 O24 Co1 128.3(4) . . ? C24 O24 Co1 129.5(4) . 2_577 ? Co1 O24 Co1 102.2(2) . 2_577 ? C24 O24 Na2 87.3(3) . 2_577 ? Co1 O24 Na2 92.8(2) . 2_577 ? Co1 O24 Na2 89.0(2) 2_577 2_577 ? C25 N15 C65 121.5(4) . . ? C25 N15 Co1 90.6(3) . . ? C65 N15 Co1 147.7(3) . . ? O25 C25 N15 113.4(4) . . ? O25 C25 C35 126.9(4) . . ? N15 C25 C35 119.7(4) . . ? C45 C35 C25 119.0(4) . . ? C35 C45 C55 120.7(4) . . ? C45 C55 C65 119.4(4) . . ? N15 C65 C55 119.7(4) . . ? N15 C65 C5 114.8(5) . . ? C55 C65 C5 121.3(5) . . ? N15 C65 C5' 115.5(5) . . ? C55 C65 C5' 120.9(5) . . ? C25 O25 Co1 93.4(3) . . ? C25 O25 Na2 146.6(4) . 2_577 ? Co1 O25 Na2 100.0(2) . 2_577 ? C66 N16 C26 121.6(4) . . ? C66 N16 Co1 147.6(3) . . ? C26 N16 Co1 90.1(3) . . ? O26 C26 N16 114.1(4) . . ? O26 C26 C36 127.2(5) . . ? N16 C26 C36 118.7(4) . . ? C46 C36 C26 119.8(5) . . ? C36 C46 C56 120.9(4) . . ? C66 C56 C46 118.1(4) . . ? N16 C66 C56 120.8(4) . . ? N16 C66 C6 117.0(4) . . ? C56 C66 C6 122.1(5) . . ? C26 O26 Co1 92.7(3) . . ? C26 O26 Na2 148.8(3) . . ? Co1 O26 Na2 102.2(2) . . ? C67 N17 C27 122.1(5) . . ? O27 C27 N17 114.1(6) . . ? O27 C27 C37 127.9(6) . . ? N17 C27 C37 118.0(5) . . ? C47 C37 C27 120.2(5) . . ? C37 C47 C57 121.1(5) . . ? C67 C57 C47 117.9(5) . . ? N17 C67 C57 120.6(5) . . ? N17 C67 C7 116.3(5) . . ? C57 C67 C7 123.0(6) . . ? C27 O27 Na2 132.0(7) . . ? C27 O27 Na1 130.7(6) . . ? Na2 O27 Na1 95.2(3) . . ? C27' N17' C67' 120.0 . . ? O27' C27' N17' 112.7(4) . . ? O27' C27' C37' 127.3(4) . . ? N17' C27' C37' 120.0 . . ? C47' C37' C27' 120.0 . . ? C37' C47' C57' 120.0 . . ? C67' C57' C47' 120.0 . . ? C57' C67' N17' 120.0 . . ? C57' C67' C7' 124.3(4) . . ? N17' C67' C7' 115.7(4) . . ? C27' O27' Na1 128.4(6) . . ? C27' O27' Na2 127.4(6) . . ? Na1 O27' Na2 103.7(3) . . ? Na1 O1 Na2 97.4(2) . . ? _refine_diff_density_max 0.308 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.063