# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1567 data_990629b loop_ _publ_author_name 'Lei Zhang' 'Liang-Fu Tang*' 'Peng Cheng*' 'Lin-Hong Weng' 'Zhi-Hong Wang' 'Zong-Hui Jiang' 'Dai-Zheng Liao' 'Shi-Ping Yan' 'Gen-Lin Wang' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H28 Cr2 N8 Na2 O18' _chemical_formula_weight 998.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 '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 9.3366(15) _cell_length_b 9.5519(15) _cell_length_c 22.527(4) _cell_angle_alpha 96.259(3) _cell_angle_beta 95.649(3) _cell_angle_gamma 95.673(3) _cell_volume 1975.1(5) _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 red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 0.664 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11435 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0678 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 26.44 _reflns_number_total 7968 _reflns_number_gt 5230 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0488P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7968 _refine_ls_number_parameters 581 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0783 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.1066 _refine_ls_wR_factor_gt 0.0950 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.973 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr2 Cr 0.19342(5) 0.75462(5) 0.38752(2) 0.02905(13) Uani 1 1 d . . . Na2 Na 0.37184(13) 0.24149(12) 0.28392(5) 0.0391(3) Uani 1 1 d . . . O9 O 0.1681(2) 0.63253(19) 0.31005(8) 0.0323(5) Uani 1 1 d . . . O13 O 0.3724(2) 0.8533(2) 0.36866(9) 0.0341(5) Uani 1 1 d . . . O10 O 0.2999(2) 0.6013(2) 0.41448(9) 0.0370(5) Uani 1 1 d . . . N4 N 0.2020(2) 0.8583(2) 0.47294(10) 0.0324(5) Uani 1 1 d . . . N3 N 0.0024(3) 0.6687(3) 0.41451(11) 0.0349(6) Uani 1 1 d . . . O11 O 0.2391(2) 0.4344(2) 0.26723(9) 0.0424(5) Uani 1 1 d . . . O15 O 0.4506(2) 1.0428(2) 0.32656(12) 0.0505(6) Uani 1 1 d . . . O12 O 0.4043(2) 0.4169(2) 0.37503(10) 0.0473(6) Uani 1 1 d . . . C28 C 0.2016(3) 1.0134(3) 0.34616(13) 0.0310(6) Uani 1 1 d . . . O16 O 0.1795(2) 1.1336(2) 0.33800(10) 0.0436(5) Uani 1 1 d . . . C27 C 0.3558(3) 0.9687(3) 0.34550(13) 0.0323(7) Uani 1 1 d . . . C26 C 0.3240(3) 0.5094(3) 0.37129(13) 0.0324(7) Uani 1 1 d . . . C25 C 0.2385(3) 0.5236(3) 0.31010(13) 0.0308(6) Uani 1 1 d . . . C20 C 0.0901(3) 0.8202(3) 0.50431(13) 0.0330(7) Uani 1 1 d . . . C19 C -0.0191(3) 0.7095(3) 0.47206(14) 0.0356(7) Uani 1 1 d . . . C24 C 0.3016(3) 0.9649(3) 0.49758(14) 0.0420(8) Uani 1 1 d . . . H24A H 0.3788 0.9902 0.4764 0.050 Uiso 1 1 calc R . . C23 C 0.2942(4) 1.0380(4) 0.55287(15) 0.0476(8) Uani 1 1 d . . . H23A H 0.3643 1.1122 0.5687 0.057 Uiso 1 1 calc R . . C21 C 0.0785(4) 0.8901(4) 0.55988(14) 0.0453(8) Uani 1 1 d . . . H21A H 0.0013 0.8635 0.5809 0.054 Uiso 1 1 calc R . . C22 C 0.1810(4) 0.9993(4) 0.58440(15) 0.0501(9) Uani 1 1 d . . . H22A H 0.1739 1.0468 0.6221 0.060 Uiso 1 1 calc R . . C15 C -0.0981(4) 0.5768(4) 0.38058(16) 0.0504(9) Uani 1 1 d . . . H15A H -0.0849 0.5505 0.3407 0.060 Uiso 1 1 calc R . . C18 C -0.1391(4) 0.6542(4) 0.49650(17) 0.0554(10) Uani 1 1 d . . . H18A H -0.1517 0.6819 0.5364 0.067 Uiso 1 1 calc R . . C17 C -0.2403(4) 0.5573(4) 0.4609(2) 0.0707(12) Uani 1 1 d . . . H17A H -0.3213 0.5181 0.4767 0.085 Uiso 1 1 calc R . . C16 C -0.2203(4) 0.5197(4) 0.40254(19) 0.0671(11) Uani 1 1 d . . . H16A H -0.2885 0.4561 0.3778 0.081 Uiso 1 1 calc R . . Cr1 Cr 0.28666(5) 0.17661(5) 0.10587(2) 0.03083(13) Uani 1 1 d . . . O6 O 0.2687(2) 0.1085(2) 0.18449(9) 0.0367(5) Uani 1 1 d . . . O5 O 0.1894(2) -0.0127(2) 0.07558(9) 0.0392(5) Uani 1 1 d . . . O2 O 0.1037(2) 0.2593(2) 0.10388(9) 0.0362(5) Uani 1 1 d . . . O1 O 0.3667(2) 0.3690(2) 0.13910(9) 0.0343(5) Uani 1 1 d . . . N2 N 0.4924(3) 0.1190(2) 0.10247(11) 0.0337(6) Uani 1 1 d . . . N1 N 0.3280(3) 0.2277(3) 0.02263(11) 0.0338(6) Uani 1 1 d . . . O3 O 0.2988(2) 0.5857(2) 0.15875(10) 0.0410(5) Uani 1 1 d . . . O4 O 0.0139(2) 0.4608(2) 0.13277(10) 0.0434(5) Uani 1 1 d . . . C12 C 0.1148(3) 0.3914(3) 0.12577(13) 0.0313(6) Uani 1 1 d . . . C5 C 0.4669(3) 0.2241(3) 0.01099(14) 0.0356(7) Uani 1 1 d . . . C11 C 0.2731(3) 0.4596(3) 0.14336(13) 0.0314(6) Uani 1 1 d . . . C6 C 0.5599(3) 0.1601(3) 0.05536(14) 0.0352(7) Uani 1 1 d . . . O8 O 0.1789(3) -0.0826(2) 0.22310(10) 0.0581(7) Uani 1 1 d . . . C14 C 0.2009(3) -0.0169(3) 0.18098(14) 0.0361(7) Uani 1 1 d . . . C13 C 0.1479(3) -0.0858(3) 0.11641(13) 0.0339(7) Uani 1 1 d . . . O7 O 0.0742(3) -0.2004(2) 0.10818(11) 0.0508(6) Uani 1 1 d . . . C10 C 0.5681(3) 0.0551(3) 0.14322(15) 0.0430(8) Uani 1 1 d . . . H10A H 0.5229 0.0262 0.1755 0.052 Uiso 1 1 calc R . . C1 C 0.2357(3) 0.2769(3) -0.01673(15) 0.0432(8) Uani 1 1 d . . . H1A H 0.1396 0.2767 -0.0092 0.052 Uiso 1 1 calc R . . C9 C 0.7088(4) 0.0304(4) 0.13938(17) 0.0544(9) Uani 1 1 d . . . H9A H 0.7575 -0.0152 0.1683 0.065 Uiso 1 1 calc R . . C3 C 0.4173(4) 0.3289(4) -0.07872(17) 0.0625(11) Uani 1 1 d . . . H3A H 0.4478 0.3648 -0.1127 0.075 Uiso 1 1 calc R . . C2 C 0.2758(4) 0.3280(4) -0.06778(16) 0.0553(10) Uani 1 1 d . . . H2A H 0.2083 0.3612 -0.0944 0.066 Uiso 1 1 calc R . . C7 C 0.7016(4) 0.1397(4) 0.04991(17) 0.0504(9) Uani 1 1 d . . . H7A H 0.7465 0.1702 0.0178 0.060 Uiso 1 1 calc R . . C8 C 0.7769(4) 0.0735(4) 0.09257(19) 0.0595(10) Uani 1 1 d . . . H8A H 0.8730 0.0585 0.0894 0.071 Uiso 1 1 calc R . . C4 C 0.5153(4) 0.2760(4) -0.03888(16) 0.0528(9) Uani 1 1 d . . . H4A H 0.6118 0.2756 -0.0458 0.063 Uiso 1 1 calc R . . Na1 Na 0.09108(12) 0.67529(12) 0.20020(5) 0.0395(3) Uani 1 1 d . . . N5 N -0.1609(3) 0.6744(3) 0.22959(11) 0.0354(6) Uani 1 1 d . . . N6 N -0.2882(2) 0.5896(3) 0.22229(11) 0.0326(6) Uani 1 1 d . . . N7 N -0.2552(2) 0.3468(2) 0.23305(11) 0.0345(6) Uani 1 1 d . . . N8 N -0.3530(3) 0.2841(3) 0.26556(12) 0.0416(6) Uani 1 1 d . . . C29 C -0.1217(3) 0.3072(3) 0.24589(15) 0.0419(8) Uani 1 1 d . . . H29A H -0.0386 0.3372 0.2291 0.050 Uiso 1 1 calc R . . C32 C -0.2971(3) 0.4466(3) 0.19304(14) 0.0359(7) Uani 1 1 d . . . H32A H -0.3958 0.4175 0.1751 0.043 Uiso 1 1 calc R . . H32B H -0.2352 0.4448 0.1609 0.043 Uiso 1 1 calc R . . C33 C -0.3932(3) 0.6542(4) 0.24679(15) 0.0463(8) Uani 1 1 d . . . H33A H -0.4886 0.6157 0.2471 0.056 Uiso 1 1 calc R . . C35 C -0.1913(4) 0.7940(3) 0.25919(15) 0.0445(8) Uani 1 1 d . . . H35A H -0.1244 0.8735 0.2706 0.053 Uiso 1 1 calc R . . C31 C -0.2751(3) 0.2059(4) 0.29786(16) 0.0499(9) Uani 1 1 d . . . H31A H -0.3131 0.1492 0.3249 0.060 Uiso 1 1 calc R . . C34 C -0.3345(4) 0.7862(4) 0.27107(16) 0.0507(9) Uani 1 1 d . . . H34A H -0.3804 0.8561 0.2913 0.061 Uiso 1 1 calc R . . C30 C -0.1307(3) 0.2168(4) 0.28742(16) 0.0501(9) Uani 1 1 d . . . H30A H -0.0568 0.1716 0.3052 0.060 Uiso 1 1 calc R . . O18 O 0.4903(4) 0.2595(4) 0.47384(18) 0.1137(12) Uani 1 1 d . . . O17 O 0.1314(5) -0.4081(5) 0.0128(2) 0.1450(16) Uani 1 1 d . . . O14 O 0.1071(2) 0.9149(2) 0.35770(9) 0.0321(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr2 0.0291(3) 0.0314(3) 0.0272(3) 0.0040(2) 0.00577(19) 0.0031(2) Na2 0.0422(7) 0.0345(6) 0.0414(7) 0.0045(5) 0.0059(5) 0.0073(5) O9 0.0397(12) 0.0309(11) 0.0272(11) 0.0034(9) 0.0026(9) 0.0098(9) O13 0.0256(10) 0.0358(11) 0.0432(12) 0.0089(9) 0.0070(9) 0.0068(9) O10 0.0455(12) 0.0373(12) 0.0285(11) 0.0050(9) 0.0006(9) 0.0091(10) N4 0.0315(13) 0.0366(14) 0.0284(13) 0.0006(11) 0.0030(10) 0.0038(11) N3 0.0335(14) 0.0360(14) 0.0346(15) 0.0052(11) 0.0052(11) -0.0015(11) O11 0.0544(14) 0.0412(12) 0.0320(12) -0.0006(10) 0.0051(10) 0.0121(11) O15 0.0297(12) 0.0465(13) 0.0825(18) 0.0270(13) 0.0188(11) 0.0065(10) O12 0.0555(15) 0.0378(12) 0.0481(14) 0.0033(10) -0.0054(11) 0.0153(11) C28 0.0294(16) 0.0323(16) 0.0319(16) 0.0031(13) 0.0046(12) 0.0055(13) O16 0.0383(12) 0.0346(12) 0.0619(16) 0.0135(11) 0.0115(11) 0.0100(10) C27 0.0296(16) 0.0320(16) 0.0366(17) 0.0041(13) 0.0074(13) 0.0063(13) C26 0.0354(17) 0.0294(16) 0.0326(17) 0.0097(13) 0.0025(13) -0.0007(13) C25 0.0316(16) 0.0327(16) 0.0289(16) 0.0069(13) 0.0057(12) 0.0009(13) C20 0.0363(17) 0.0360(16) 0.0295(16) 0.0066(13) 0.0071(13) 0.0117(14) C19 0.0374(17) 0.0368(17) 0.0345(17) 0.0079(14) 0.0088(13) 0.0044(14) C24 0.0345(17) 0.0475(19) 0.0406(19) -0.0018(15) -0.0007(14) 0.0011(15) C23 0.045(2) 0.049(2) 0.043(2) -0.0090(16) -0.0079(16) 0.0050(16) C21 0.048(2) 0.057(2) 0.0329(18) 0.0063(16) 0.0089(15) 0.0112(17) C22 0.059(2) 0.057(2) 0.0330(19) -0.0079(16) 0.0006(16) 0.0190(19) C15 0.050(2) 0.052(2) 0.044(2) 0.0009(17) 0.0058(16) -0.0107(17) C18 0.056(2) 0.063(2) 0.050(2) 0.0096(18) 0.0234(18) -0.0041(19) C17 0.055(2) 0.078(3) 0.077(3) 0.009(2) 0.025(2) -0.023(2) C16 0.055(2) 0.071(3) 0.067(3) -0.002(2) 0.011(2) -0.030(2) Cr1 0.0311(3) 0.0325(3) 0.0293(3) 0.0051(2) 0.0056(2) 0.0023(2) O6 0.0475(13) 0.0324(11) 0.0285(11) 0.0016(9) 0.0063(9) -0.0040(10) O5 0.0492(13) 0.0374(12) 0.0299(12) 0.0029(9) 0.0048(10) -0.0003(10) O2 0.0277(11) 0.0348(12) 0.0444(13) 0.0001(10) 0.0051(9) -0.0009(9) O1 0.0236(10) 0.0362(11) 0.0431(12) 0.0036(9) 0.0034(9) 0.0044(9) N2 0.0374(14) 0.0310(13) 0.0333(14) 0.0046(11) 0.0035(11) 0.0064(11) N1 0.0333(14) 0.0386(14) 0.0305(14) 0.0062(11) 0.0037(11) 0.0055(11) O3 0.0364(12) 0.0333(12) 0.0522(14) 0.0045(10) 0.0030(10) 0.0014(10) O4 0.0287(11) 0.0440(13) 0.0584(15) 0.0016(11) 0.0087(10) 0.0092(10) C12 0.0277(15) 0.0380(17) 0.0291(16) 0.0086(13) 0.0058(12) 0.0004(13) C5 0.0363(17) 0.0363(17) 0.0337(17) 0.0046(13) 0.0040(13) 0.0011(14) C11 0.0312(16) 0.0358(17) 0.0276(16) 0.0069(13) 0.0058(12) -0.0010(13) C6 0.0336(17) 0.0348(16) 0.0365(17) -0.0001(14) 0.0059(13) 0.0037(13) O8 0.0929(19) 0.0457(14) 0.0334(13) 0.0087(11) 0.0116(13) -0.0127(13) C14 0.0397(18) 0.0358(17) 0.0339(17) 0.0044(14) 0.0101(14) 0.0031(14) C13 0.0333(16) 0.0340(17) 0.0351(17) 0.0052(14) 0.0041(13) 0.0060(14) O7 0.0598(15) 0.0365(13) 0.0502(15) 0.0061(11) -0.0076(11) -0.0108(11) C10 0.046(2) 0.0426(19) 0.0407(19) 0.0095(15) -0.0004(15) 0.0079(15) C1 0.0390(19) 0.050(2) 0.042(2) 0.0137(16) 0.0007(15) 0.0071(15) C9 0.046(2) 0.055(2) 0.062(2) 0.0136(19) -0.0098(18) 0.0145(18) C3 0.066(3) 0.081(3) 0.042(2) 0.027(2) 0.0105(19) -0.007(2) C2 0.056(2) 0.070(3) 0.044(2) 0.0269(19) 0.0014(17) 0.0062(19) C7 0.0374(19) 0.060(2) 0.055(2) 0.0070(18) 0.0110(16) 0.0067(17) C8 0.036(2) 0.067(3) 0.075(3) 0.001(2) 0.0002(19) 0.0136(18) C4 0.041(2) 0.074(3) 0.047(2) 0.0222(19) 0.0093(16) 0.0025(18) Na1 0.0377(7) 0.0360(7) 0.0450(7) 0.0057(5) 0.0082(5) 0.0009(5) N5 0.0282(13) 0.0353(14) 0.0412(15) 0.0027(12) 0.0034(11) -0.0020(11) N6 0.0284(13) 0.0362(14) 0.0333(14) 0.0064(11) 0.0031(10) 0.0021(11) N7 0.0273(13) 0.0344(14) 0.0431(16) 0.0125(12) 0.0040(11) 0.0008(11) N8 0.0281(14) 0.0464(16) 0.0520(17) 0.0183(13) 0.0046(12) -0.0012(12) C29 0.0219(16) 0.051(2) 0.054(2) 0.0115(17) 0.0063(14) 0.0001(14) C32 0.0338(17) 0.0358(17) 0.0364(17) 0.0050(14) 0.0005(13) -0.0018(13) C33 0.0306(17) 0.062(2) 0.046(2) 0.0005(17) 0.0064(15) 0.0067(16) C35 0.046(2) 0.0379(18) 0.046(2) -0.0029(15) 0.0023(15) -0.0010(15) C31 0.0350(19) 0.057(2) 0.062(2) 0.0314(19) 0.0033(16) -0.0019(16) C34 0.045(2) 0.052(2) 0.053(2) -0.0097(18) 0.0048(16) 0.0138(17) C30 0.0350(19) 0.055(2) 0.065(2) 0.0293(19) 0.0036(16) 0.0081(16) O18 0.119(3) 0.096(3) 0.122(3) 0.033(2) -0.016(2) 0.001(2) O17 0.147(4) 0.140(4) 0.144(4) 0.018(3) 0.020(3) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr2 O13 1.9436(19) . ? Cr2 O14 1.9512(19) . ? Cr2 O10 1.9657(19) . ? Cr2 O9 1.9703(19) . ? Cr2 N4 2.056(2) . ? Cr2 N3 2.063(2) . ? Na2 O11 2.362(2) . ? Na2 O15 2.366(2) 1_545 ? Na2 O16 2.472(2) 1_545 ? Na2 O12 2.478(2) . ? Na2 O6 2.504(2) . ? Na2 N8 2.642(3) 1_655 ? Na2 C27 3.080(3) 1_545 ? Na2 C25 3.102(3) . ? Na2 C28 3.108(3) 1_545 ? O9 C25 1.284(3) . ? O9 Na1 2.595(2) . ? O13 C27 1.287(3) . ? O10 C26 1.290(3) . ? N4 C24 1.340(4) . ? N4 C20 1.360(4) . ? N3 C15 1.336(4) . ? N3 C19 1.352(4) . ? O11 C25 1.217(3) . ? O15 C27 1.218(3) . ? O15 Na2 2.366(2) 1_565 ? O12 C26 1.218(3) . ? C28 O16 1.217(3) . ? C28 O14 1.290(3) . ? C28 C27 1.543(4) . ? C28 Na2 3.108(3) 1_565 ? O16 Na2 2.472(2) 1_565 ? C27 Na2 3.080(3) 1_565 ? C26 C25 1.550(4) . ? C20 C21 1.373(4) . ? C20 C19 1.469(4) . ? C19 C18 1.381(4) . ? C24 C23 1.372(4) . ? C23 C22 1.373(5) . ? C21 C22 1.372(5) . ? C15 C16 1.376(5) . ? C18 C17 1.381(5) . ? C17 C16 1.361(5) . ? Cr1 O2 1.950(2) . ? Cr1 O1 1.953(2) . ? Cr1 O5 1.961(2) . ? Cr1 O6 1.969(2) . ? Cr1 N1 2.051(2) . ? Cr1 N2 2.056(2) . ? O6 C14 1.289(3) . ? O5 C13 1.281(3) . ? O2 C12 1.294(3) . ? O1 C11 1.292(3) . ? N2 C10 1.339(4) . ? N2 C6 1.360(4) . ? N1 C1 1.331(4) . ? N1 C5 1.351(4) . ? O3 C11 1.210(3) . ? O3 Na1 2.424(2) . ? O4 C12 1.217(3) . ? O4 Na1 2.416(2) . ? C12 C11 1.550(4) . ? C12 Na1 3.068(3) . ? C5 C4 1.374(4) . ? C5 C6 1.481(4) . ? C11 Na1 3.053(3) . ? C6 C7 1.372(4) . ? O8 C14 1.216(4) . ? O8 Na1 2.360(3) 1_545 ? C14 C13 1.542(4) . ? C14 Na1 3.107(3) 1_545 ? C13 O7 1.220(3) . ? O7 Na1 2.498(3) 1_545 ? C10 C9 1.367(4) . ? C1 C2 1.368(4) . ? C9 C8 1.364(5) . ? C3 C2 1.368(5) . ? C3 C4 1.388(5) . ? C7 C8 1.380(5) . ? Na1 O8 2.360(3) 1_565 ? Na1 O7 2.498(3) 1_565 ? Na1 N5 2.505(3) . ? Na1 C14 3.107(3) 1_565 ? N5 C35 1.329(4) . ? N5 N6 1.355(3) . ? N6 C33 1.341(4) . ? N6 C32 1.442(4) . ? N7 C29 1.352(4) . ? N7 N8 1.359(3) . ? N7 C32 1.438(4) . ? N8 C31 1.318(4) . ? N8 Na2 2.642(3) 1_455 ? C29 C30 1.344(4) . ? C33 C34 1.358(5) . ? C35 C34 1.386(4) . ? C31 C30 1.387(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O13 Cr2 O14 83.64(8) . . ? O13 Cr2 O10 90.23(8) . . ? O14 Cr2 O10 173.82(9) . . ? O13 Cr2 O9 92.02(8) . . ? O14 Cr2 O9 96.39(8) . . ? O10 Cr2 O9 82.93(8) . . ? O13 Cr2 N4 95.54(9) . . ? O14 Cr2 N4 88.07(9) . . ? O10 Cr2 N4 93.39(9) . . ? O9 Cr2 N4 171.61(9) . . ? O13 Cr2 N3 173.70(9) . . ? O14 Cr2 N3 93.62(9) . . ? O10 Cr2 N3 92.55(9) . . ? O9 Cr2 N3 93.92(9) . . ? N4 Cr2 N3 78.66(10) . . ? O11 Na2 O15 160.25(9) . 1_545 ? O11 Na2 O16 91.33(8) . 1_545 ? O15 Na2 O16 70.17(8) 1_545 1_545 ? O11 Na2 O12 69.94(8) . . ? O15 Na2 O12 99.61(9) 1_545 . ? O16 Na2 O12 81.63(8) 1_545 . ? O11 Na2 O6 91.89(8) . . ? O15 Na2 O6 95.96(9) 1_545 . ? O16 Na2 O6 93.49(8) 1_545 . ? O12 Na2 O6 160.94(8) . . ? O11 Na2 N8 114.13(9) . 1_655 ? O15 Na2 N8 82.36(8) 1_545 1_655 ? O16 Na2 N8 150.55(9) 1_545 1_655 ? O12 Na2 N8 93.05(9) . 1_655 ? O6 Na2 N8 99.88(8) . 1_655 ? O11 Na2 C27 140.94(9) . 1_545 ? O15 Na2 C27 21.05(7) 1_545 1_545 ? O16 Na2 C27 49.64(7) 1_545 1_545 ? O12 Na2 C27 98.61(8) . 1_545 ? O6 Na2 C27 91.98(8) . 1_545 ? N8 Na2 C27 103.41(8) 1_655 1_545 ? O11 Na2 C25 20.58(7) . . ? O15 Na2 C25 144.54(9) 1_545 . ? O16 Na2 C25 86.32(8) 1_545 . ? O12 Na2 C25 49.44(7) . . ? O6 Na2 C25 112.10(8) . . ? N8 Na2 C25 112.12(8) 1_655 . ? C27 Na2 C25 131.72(8) 1_545 . ? O11 Na2 C28 112.49(8) . 1_545 ? O15 Na2 C28 49.88(7) 1_545 1_545 ? O16 Na2 C28 21.57(7) 1_545 1_545 ? O12 Na2 C28 93.10(8) . 1_545 ? O6 Na2 C28 88.56(8) . 1_545 ? N8 Na2 C28 132.19(8) 1_655 1_545 ? C27 Na2 C28 28.87(7) 1_545 1_545 ? C25 Na2 C28 107.61(8) . 1_545 ? C25 O9 Cr2 113.83(17) . . ? C25 O9 Na1 109.67(16) . . ? Cr2 O9 Na1 133.51(9) . . ? C27 O13 Cr2 114.01(18) . . ? C26 O10 Cr2 113.78(18) . . ? C24 N4 C20 118.7(3) . . ? C24 N4 Cr2 125.4(2) . . ? C20 N4 Cr2 115.69(19) . . ? C15 N3 C19 118.6(3) . . ? C15 N3 Cr2 125.7(2) . . ? C19 N3 Cr2 115.6(2) . . ? C25 O11 Na2 116.41(19) . . ? C27 O15 Na2 114.66(19) . 1_565 ? C26 O12 Na2 112.38(19) . . ? O16 C28 O14 126.2(3) . . ? O16 C28 C27 120.0(3) . . ? O14 C28 C27 113.8(2) . . ? O16 C28 Na2 48.32(15) . 1_565 ? O14 C28 Na2 163.5(2) . 1_565 ? C27 C28 Na2 74.57(16) . 1_565 ? C28 O16 Na2 110.11(18) . 1_565 ? O15 C27 O13 125.5(3) . . ? O15 C27 C28 120.7(3) . . ? O13 C27 C28 113.7(3) . . ? O15 C27 Na2 44.28(15) . 1_565 ? O13 C27 Na2 169.7(2) . 1_565 ? C28 C27 Na2 76.56(16) . 1_565 ? O12 C26 O10 126.3(3) . . ? O12 C26 C25 119.9(3) . . ? O10 C26 C25 113.8(2) . . ? O11 C25 O9 125.1(3) . . ? O11 C25 C26 120.4(3) . . ? O9 C25 C26 114.5(2) . . ? O11 C25 Na2 43.02(14) . . ? O9 C25 Na2 167.9(2) . . ? C26 C25 Na2 77.38(16) . . ? N4 C20 C21 120.7(3) . . ? N4 C20 C19 114.9(2) . . ? C21 C20 C19 124.2(3) . . ? N3 C19 C18 121.3(3) . . ? N3 C19 C20 114.9(3) . . ? C18 C19 C20 123.8(3) . . ? N4 C24 C23 122.6(3) . . ? C24 C23 C22 118.6(3) . . ? C22 C21 C20 119.9(3) . . ? C21 C22 C23 119.5(3) . . ? N3 C15 C16 122.4(3) . . ? C19 C18 C17 119.1(3) . . ? C16 C17 C18 119.4(3) . . ? C17 C16 C15 119.2(4) . . ? O2 Cr1 O1 82.95(8) . . ? O2 Cr1 O5 92.24(9) . . ? O1 Cr1 O5 174.61(8) . . ? O2 Cr1 O6 93.90(9) . . ? O1 Cr1 O6 95.00(8) . . ? O5 Cr1 O6 82.87(8) . . ? O2 Cr1 N1 94.13(9) . . ? O1 Cr1 N1 88.29(9) . . ? O5 Cr1 N1 94.50(9) . . ? O6 Cr1 N1 171.64(9) . . ? O2 Cr1 N2 170.62(9) . . ? O1 Cr1 N2 90.25(9) . . ? O5 Cr1 N2 94.80(9) . . ? O6 Cr1 N2 93.13(9) . . ? N1 Cr1 N2 79.15(9) . . ? C14 O6 Cr1 113.67(18) . . ? C14 O6 Na2 121.04(18) . . ? Cr1 O6 Na2 125.25(9) . . ? C13 O5 Cr1 114.49(19) . . ? C12 O2 Cr1 114.59(18) . . ? C11 O1 Cr1 115.12(17) . . ? C10 N2 C6 117.9(3) . . ? C10 N2 Cr1 127.0(2) . . ? C6 N2 Cr1 114.94(19) . . ? C1 N1 C5 118.7(3) . . ? C1 N1 Cr1 125.9(2) . . ? C5 N1 Cr1 114.99(19) . . ? C11 O3 Na1 109.72(18) . . ? C12 O4 Na1 110.83(19) . . ? O4 C12 O2 125.5(3) . . ? O4 C12 C11 120.6(3) . . ? O2 C12 C11 113.9(2) . . ? O4 C12 Na1 47.40(15) . . ? O2 C12 Na1 165.41(19) . . ? C11 C12 Na1 74.78(16) . . ? N1 C5 C4 121.4(3) . . ? N1 C5 C6 115.0(3) . . ? C4 C5 C6 123.6(3) . . ? O3 C11 O1 126.6(3) . . ? O3 C11 C12 120.4(3) . . ? O1 C11 C12 113.1(2) . . ? O3 C11 Na1 48.37(15) . . ? O1 C11 Na1 159.65(19) . . ? C12 C11 Na1 75.88(16) . . ? N2 C6 C7 121.6(3) . . ? N2 C6 C5 114.5(3) . . ? C7 C6 C5 124.0(3) . . ? C14 O8 Na1 117.0(2) . 1_545 ? O8 C14 O6 125.9(3) . . ? O8 C14 C13 119.5(3) . . ? O6 C14 C13 114.6(3) . . ? O8 C14 Na1 42.59(16) . 1_545 ? O6 C14 Na1 165.8(2) . 1_545 ? C13 C14 Na1 77.44(16) . 1_545 ? O7 C13 O5 126.2(3) . . ? O7 C13 C14 119.9(3) . . ? O5 C13 C14 113.9(3) . . ? C13 O7 Na1 111.4(2) . 1_545 ? N2 C10 C9 122.8(3) . . ? N1 C1 C2 123.1(3) . . ? C8 C9 C10 119.2(3) . . ? C2 C3 C4 119.7(3) . . ? C3 C2 C1 118.4(3) . . ? C6 C7 C8 119.3(3) . . ? C9 C8 C7 119.2(3) . . ? C5 C4 C3 118.7(3) . . ? O8 Na1 O4 153.99(9) 1_565 . ? O8 Na1 O3 99.90(9) 1_565 . ? O4 Na1 O3 70.25(8) . . ? O8 Na1 O7 68.95(8) 1_565 1_565 ? O4 Na1 O7 85.76(8) . 1_565 ? O3 Na1 O7 83.53(8) . 1_565 ? O8 Na1 N5 101.42(9) 1_565 . ? O4 Na1 N5 89.31(8) . . ? O3 Na1 N5 158.54(9) . . ? O7 Na1 N5 101.94(9) 1_565 . ? O8 Na1 O9 90.44(8) 1_565 . ? O4 Na1 O9 114.05(8) . . ? O3 Na1 O9 95.88(8) . . ? O7 Na1 O9 158.83(8) 1_565 . ? N5 Na1 O9 86.36(8) . . ? O8 Na1 C11 121.81(9) 1_565 . ? O4 Na1 C11 50.67(8) . . ? O3 Na1 C11 21.91(7) . . ? O7 Na1 C11 91.98(8) 1_565 . ? N5 Na1 C11 136.69(9) . . ? O9 Na1 C11 95.17(8) . . ? O8 Na1 C12 147.19(9) 1_565 . ? O4 Na1 C12 21.77(7) . . ? O3 Na1 C12 50.17(7) . . ? O7 Na1 C12 91.66(8) 1_565 . ? N5 Na1 C12 108.57(8) . . ? O9 Na1 C12 104.24(8) . . ? C11 Na1 C12 29.34(8) . . ? O8 Na1 C14 20.41(8) 1_565 1_565 ? O4 Na1 C14 133.58(9) . 1_565 ? O3 Na1 C14 91.26(8) . 1_565 ? O7 Na1 C14 49.16(8) 1_565 1_565 ? N5 Na1 C14 108.10(8) . 1_565 ? O9 Na1 C14 109.82(8) . 1_565 ? C11 Na1 C14 111.87(8) . 1_565 ? C12 Na1 C14 130.73(8) . 1_565 ? C35 N5 N6 103.9(2) . . ? C35 N5 Na1 115.9(2) . . ? N6 N5 Na1 140.02(19) . . ? C33 N6 N5 111.9(3) . . ? C33 N6 C32 127.8(3) . . ? N5 N6 C32 120.3(2) . . ? C29 N7 N8 111.6(2) . . ? C29 N7 C32 127.6(3) . . ? N8 N7 C32 120.8(2) . . ? C31 N8 N7 103.3(2) . . ? C31 N8 Na2 110.2(2) . 1_455 ? N7 N8 Na2 146.25(19) . 1_455 ? C30 C29 N7 107.6(3) . . ? N7 C32 N6 113.3(2) . . ? N6 C33 C34 107.3(3) . . ? N5 C35 C34 111.9(3) . . ? N8 C31 C30 113.1(3) . . ? C33 C34 C35 105.0(3) . . ? C29 C30 C31 104.5(3) . . ? C28 O14 Cr2 113.28(17) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 26.44 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.389 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.070 #######