# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2000 # CCDC Number: 440/182 data_COMPOUND_1 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C58 H67 Cl Li4 N4 O10 Zn' _chemical_formula_weight 1108.74 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' 'Li' 'Li' -0.0003 0.0001 '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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.818(2) _cell_length_b 23.435(5) _cell_length_c 21.975(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.92(3) _cell_angle_gamma 90.00 _cell_volume 6042(2) _cell_formula_units_Z 4 _cell_measurement_temperature 299(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.219 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2328 _exptl_absorpt_coefficient_mu 0.507 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Kuma KM4 automatic diffractometer' _diffrn_measurement_method 'profile data from omega-2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.4 _diffrn_reflns_number 6898 _diffrn_reflns_av_R_equivalents 0.0153 _diffrn_reflns_av_sigmaI/netI 0.0522 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 26.89 _reflns_number_total 6646 _reflns_number_gt 5003 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kuma KM4 software 1996' _computing_cell_refinement 'Kuma KM4 software 1996' _computing_data_reduction 'Kuma KM4 software 1996' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII, 1976' _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 w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+2.8493P] 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 6646 _refine_ls_number_parameters 717 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0736 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.1170 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.589 _refine_ls_shift/su_mean 0.033 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn 0.65904(4) 0.24117(2) 0.31049(2) 0.03542(14) Uani 1 d . . . Cl Cl 0.50850(10) 0.28482(6) 0.34084(6) 0.0586(3) Uani 1 d . . . Li1 Li 0.9117(6) 0.1600(3) 0.2017(3) 0.0439(17) Uani 1 d . . . Li2 Li 0.6341(6) 0.1753(3) 0.1770(3) 0.0429(17) Uani 1 d . . . Li3 Li 0.7761(6) 0.1104(3) 0.2677(3) 0.0411(17) Uani 1 d . . . Li4 Li 0.9004(7) 0.1933(3) 0.3462(3) 0.0526(19) Uani 1 d . . . O10 O 0.9588(2) 0.11836(13) 0.12909(12) 0.0458(7) Uani 1 d . . . O11 O 0.7586(2) 0.12426(11) 0.18233(11) 0.0368(6) Uani 1 d . . . O20 O 0.6189(3) 0.22426(13) 0.10165(13) 0.0630(10) Uani 1 d . . . O21 O 0.6565(2) 0.24543(12) 0.22244(12) 0.0439(7) Uani 1 d . . . O30 O 0.7306(2) 0.04326(12) 0.31198(14) 0.0508(8) Uani 1 d . . . O31 O 0.6791(2) 0.15768(11) 0.31541(12) 0.0375(7) Uani 1 d . . . O40 O 0.9480(3) 0.13635(13) 0.40941(13) 0.0588(9) Uani 1 d . . . O41 O 0.9321(2) 0.13549(12) 0.28423(12) 0.0401(7) Uani 1 d . . . O50 O 1.0404(2) 0.24941(13) 0.36031(17) 0.0628(9) Uani 1 d . . . O51 O 0.8102(2) 0.25884(12) 0.35141(12) 0.0409(6) Uani 1 d . . . C11 C 1.0397(4) 0.1163(2) 0.0823(2) 0.0479(11) Uani 1 d . . . C12 C 0.9969(4) 0.0661(2) 0.0410(2) 0.0660(15) Uani 1 d . . . H12A H 0.9994 0.0753 -0.0019 0.079 Uiso 1 calc R . . H12B H 1.0420 0.0322 0.0512 0.079 Uiso 1 calc R . . C13 C 0.8765(4) 0.0580(2) 0.0543(2) 0.0507(12) Uani 1 d . . . C14 C 0.7854(5) 0.0281(2) 0.0253(2) 0.0679(15) Uani 1 d . . . H14 H 0.7916 0.0080 -0.0107 0.082 Uiso 1 calc R . . C15 C 0.6848(4) 0.0287(2) 0.0509(2) 0.0660(15) Uani 1 d . . . H15 H 0.6227 0.0083 0.0321 0.079 Uiso 1 calc R . . C16 C 0.6737(4) 0.05917(19) 0.1045(2) 0.0495(11) Uani 1 d . . . H16 H 0.6050 0.0581 0.1210 0.059 Uiso 1 calc R . . C17 C 0.7636(3) 0.09103(17) 0.13346(18) 0.0373(10) Uani 1 d . . . C18 C 0.8634(3) 0.08854(18) 0.10583(19) 0.0407(10) Uani 1 d . . . C111 C 1.0275(5) 0.1723(2) 0.0491(3) 0.0797(17) Uani 1 d . . . H11A H 0.9526 0.1750 0.0269 0.096 Uiso 1 calc R . . H11B H 1.0835 0.1748 0.0210 0.096 Uiso 1 calc R . . H11C H 1.0387 0.2029 0.0783 0.096 Uiso 1 calc R . . C112 C 1.1548(4) 0.1076(3) 0.1157(3) 0.0798(17) Uani 1 d . . . H11D H 1.1731 0.1389 0.1434 0.096 Uiso 1 calc R . . H11E H 1.2097 0.1057 0.0870 0.096 Uiso 1 calc R . . H11F H 1.1561 0.0727 0.1386 0.096 Uiso 1 calc R . . C21 C 0.5939(5) 0.2260(2) 0.0336(2) 0.0621(14) Uani 1 d . . . C22 C 0.5831(7) 0.2905(2) 0.0175(2) 0.095(2) Uani 1 d . . . H22A H 0.6375 0.3015 -0.0100 0.114 Uiso 1 calc R . . H22B H 0.5068 0.2995 -0.0015 0.114 Uiso 1 calc R . . C23 C 0.6082(4) 0.3198(2) 0.0779(2) 0.0605(14) Uani 1 d . . . C24 C 0.6090(5) 0.3767(2) 0.0948(3) 0.0689(15) Uani 1 d . . . H24 H 0.5981 0.4053 0.0654 0.083 Uiso 1 calc R . . C25 C 0.6265(4) 0.3900(2) 0.1564(3) 0.0621(14) Uani 1 d . . . H25 H 0.6271 0.4281 0.1684 0.074 Uiso 1 calc R . . C26 C 0.6434(4) 0.3472(2) 0.2012(2) 0.0543(12) Uani 1 d . . . H26 H 0.6544 0.3573 0.2424 0.065 Uiso 1 calc R . . C27 C 0.6438(3) 0.29019(18) 0.18469(19) 0.0411(10) Uani 1 d . . . C28 C 0.6250(4) 0.2794(2) 0.1227(2) 0.0496(12) Uani 1 d . . . C212 C 0.4861(5) 0.1943(3) 0.0173(2) 0.0855(18) Uani 1 d . . . H21A H 0.4952 0.1557 0.0317 0.103 Uiso 1 calc R . . H21B H 0.4671 0.1942 -0.0265 0.103 Uiso 1 calc R . . H21C H 0.4260 0.2124 0.0359 0.103 Uiso 1 calc R . . C211 C 0.6930(5) 0.1987(3) 0.0091(2) 0.0756(17) Uani 1 d . . . H21D H 0.6992 0.1597 0.0225 0.091 Uiso 1 calc R . . H21E H 0.7615 0.2188 0.0239 0.091 Uiso 1 calc R . . H21F H 0.6819 0.1999 -0.0349 0.091 Uiso 1 calc R . . C31 C 0.7244(4) -0.0196(2) 0.3129(3) 0.0615(14) Uani 1 d . . . C32 C 0.6578(4) -0.0334(2) 0.3664(3) 0.0700(16) Uani 1 d . . . H32A H 0.6023 -0.0633 0.3555 0.084 Uiso 1 calc R . . H32B H 0.7085 -0.0453 0.4021 0.084 Uiso 1 calc R . . C33 C 0.6002(4) 0.0219(2) 0.3780(2) 0.0519(12) Uani 1 d . . . C34 C 0.5165(5) 0.0366(2) 0.4136(2) 0.0660(15) Uani 1 d . . . H34 H 0.4822 0.0091 0.4358 0.079 Uiso 1 calc R . . C35 C 0.4846(5) 0.0937(2) 0.4155(2) 0.0653(15) Uani 1 d . . . H35 H 0.4275 0.1043 0.4389 0.078 Uiso 1 calc R . . C36 C 0.5367(4) 0.1351(2) 0.3830(2) 0.0507(12) Uani 1 d . . . H36 H 0.5135 0.1729 0.3849 0.061 Uiso 1 calc R . . C37 C 0.6229(3) 0.12099(18) 0.34760(17) 0.0391(10) Uani 1 d . . . C38 C 0.6482(3) 0.06343(19) 0.34627(19) 0.0415(10) Uani 1 d . . . C311 C 0.8430(5) -0.0407(3) 0.3216(4) 0.139(4) Uani 1 d . . . H31A H 0.8778 -0.0340 0.2850 0.167 Uiso 1 calc R . . H31B H 0.8431 -0.0809 0.3300 0.167 Uiso 1 calc R . . H31C H 0.8850 -0.0210 0.3553 0.167 Uiso 1 calc R . . C312 C 0.6553(7) -0.0364(3) 0.2529(3) 0.101(2) Uani 1 d . . . H31D H 0.5809 -0.0195 0.2506 0.121 Uiso 1 calc R . . H31E H 0.6482 -0.0772 0.2509 0.121 Uiso 1 calc R . . H31F H 0.6930 -0.0232 0.2193 0.121 Uiso 1 calc R . . C41 C 0.9606(6) 0.1201(3) 0.4749(2) 0.0758(17) Uani 1 d . . . C42 C 1.0684(6) 0.0818(3) 0.4818(3) 0.098(2) Uani 1 d . . . H42A H 1.1344 0.1028 0.5004 0.118 Uiso 1 calc R . . H42B H 1.0575 0.0485 0.5067 0.118 Uiso 1 calc R . . C43 C 1.0822(4) 0.0650(2) 0.4174(3) 0.0677(15) Uani 1 d . . . C44 C 1.1488(5) 0.0251(3) 0.3899(4) 0.093(2) Uani 1 d . . . H44 H 1.1979 0.0008 0.4138 0.111 Uiso 1 calc R . . C45 C 1.1402(5) 0.0225(3) 0.3270(4) 0.093(2) Uani 1 d . . . H45 H 1.1836 -0.0041 0.3086 0.111 Uiso 1 calc R . . C46 C 1.0689(4) 0.0583(2) 0.2907(3) 0.0645(15) Uani 1 d . . . H46 H 1.0653 0.0556 0.2483 0.077 Uiso 1 calc R . . C47 C 1.0020(3) 0.09869(18) 0.3161(2) 0.0424(11) Uani 1 d . . . C48 C 1.0118(4) 0.09871(19) 0.3793(2) 0.0498(12) Uani 1 d . . . C411 C 0.8547(6) 0.0874(3) 0.4844(3) 0.094(2) Uani 1 d . . . H41A H 0.7889 0.1107 0.4722 0.113 Uiso 1 calc R . . H41B H 0.8568 0.0775 0.5269 0.113 Uiso 1 calc R . . H41C H 0.8506 0.0533 0.4600 0.113 Uiso 1 calc R . . C412 C 0.9731(7) 0.1750(3) 0.5105(2) 0.113(3) Uani 1 d . . . H41D H 1.0348 0.1968 0.4978 0.136 Uiso 1 calc R . . H41E H 0.9887 0.1666 0.5535 0.136 Uiso 1 calc R . . H41F H 0.9037 0.1965 0.5031 0.136 Uiso 1 calc R . . C51 C 1.1644(4) 0.2581(3) 0.3604(3) 0.0714(15) Uani 1 d . . . C52 C 1.1820(5) 0.3234(3) 0.3674(4) 0.120(3) Uani 1 d . . . H52A H 1.2245 0.3326 0.4067 0.144 Uiso 1 calc R . . H52B H 1.2225 0.3384 0.3350 0.144 Uiso 1 calc R . . C53 C 1.0629(4) 0.3472(2) 0.3628(2) 0.0638(14) Uani 1 d . . . C54 C 1.0214(5) 0.4013(3) 0.3627(3) 0.0729(16) Uani 1 d . . . H54 H 1.0702 0.4326 0.3649 0.087 Uiso 1 calc R . . C55 C 0.9037(5) 0.4086(2) 0.3592(2) 0.0677(15) Uani 1 d . . . H55 H 0.8736 0.4453 0.3591 0.081 Uiso 1 calc R . . C56 C 0.8307(4) 0.3617(2) 0.3558(2) 0.0537(12) Uani 1 d . . . H56 H 0.7525 0.3678 0.3538 0.064 Uiso 1 calc R . . C57 C 0.8714(4) 0.30638(18) 0.35535(18) 0.0387(10) Uani 1 d . . . C58 C 0.9894(4) 0.3018(2) 0.3598(2) 0.0509(12) Uani 1 d . . . C511 C 1.1924(5) 0.2362(4) 0.3007(3) 0.108(3) Uani 1 d . . . H51A H 1.1680 0.1972 0.2957 0.129 Uiso 1 calc R . . H51B H 1.2733 0.2383 0.2996 0.129 Uiso 1 calc R . . H51C H 1.1542 0.2589 0.2681 0.129 Uiso 1 calc R . . C512 C 1.2228(5) 0.2274(3) 0.4137(3) 0.091(2) Uani 1 d . . . H51D H 1.2072 0.2460 0.4507 0.109 Uiso 1 calc R . . H51E H 1.3035 0.2276 0.4116 0.109 Uiso 1 calc R . . H51F H 1.1959 0.1888 0.4135 0.109 Uiso 1 calc R . . N1 N 0.9299(4) 0.24510(18) 0.19331(19) 0.0600(11) Uani 1 d . . . N2 N 0.4878(3) 0.13553(19) 0.19634(19) 0.0601(11) Uani 1 d . . . N3 N 0.1793(9) 0.1841(4) 0.6314(5) 0.201(4) Uani 1 d . . . N4 N 0.3622(8) -0.0053(5) 0.1433(6) 0.222(6) Uani 1 d . . . C11N C 0.9287(4) 0.2932(2) 0.1924(2) 0.0514(12) Uani 1 d . . . C12N C 0.9309(5) 0.3543(2) 0.1930(3) 0.0695(15) Uani 1 d . . . H12A H 0.9284 0.3678 0.2341 0.083 Uiso 1 calc R . . H12B H 0.8662 0.3687 0.1669 0.083 Uiso 1 calc R . . H12C H 0.9997 0.3675 0.1783 0.083 Uiso 1 calc R . . C21N C 0.4300(4) 0.1118(2) 0.2240(2) 0.0575(13) Uani 1 d . . . C22N C 0.3552(5) 0.0804(3) 0.2598(3) 0.093(2) Uani 1 d . . . H22A H 0.2925 0.1042 0.2676 0.112 Uiso 1 calc R . . H22B H 0.3970 0.0689 0.2981 0.112 Uiso 1 calc R . . H22C H 0.3268 0.0471 0.2375 0.112 Uiso 1 calc R . . C31N C 0.2691(7) 0.2022(3) 0.6464(4) 0.121(3) Uani 1 d . . . C32N C 0.3653(6) 0.2230(4) 0.6723(3) 0.142(4) Uani 1 d . . . H32A H 0.4258 0.2117 0.6494 0.170 Uiso 1 calc R . . H32B H 0.3803 0.2089 0.7134 0.170 Uiso 1 calc R . . H32C H 0.3607 0.2639 0.6730 0.170 Uiso 1 calc R . . C41N C 0.4132(9) -0.0360(4) 0.1237(5) 0.122(3) Uani 1 d . . . C42N C 0.4815(10) -0.0766(3) 0.0996(4) 0.156(4) Uani 1 d . . . H42A H 0.5056 -0.1045 0.1305 0.187 Uiso 1 calc R . . H42B H 0.5472 -0.0583 0.0867 0.187 Uiso 1 calc R . . H42C H 0.4389 -0.0951 0.0652 0.187 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 Zn 0.0330(2) 0.0416(3) 0.0314(2) -0.0054(2) 0.00322(17) -0.0001(2) Cl 0.0422(6) 0.0753(9) 0.0594(8) -0.0147(6) 0.0112(5) 0.0102(6) Li1 0.048(4) 0.047(4) 0.037(4) 0.000(3) 0.008(3) -0.007(3) Li2 0.049(4) 0.039(4) 0.040(4) 0.006(3) 0.002(3) 0.002(3) Li3 0.044(4) 0.043(4) 0.038(4) 0.007(3) 0.012(3) -0.003(3) Li4 0.066(5) 0.047(5) 0.044(4) 0.007(4) 0.005(4) 0.006(4) O10 0.0424(17) 0.056(2) 0.0403(17) -0.0089(14) 0.0113(13) -0.0019(14) O11 0.0420(15) 0.0394(16) 0.0291(15) -0.0027(12) 0.0048(12) 0.0019(13) O20 0.111(3) 0.046(2) 0.0295(17) 0.0049(14) -0.0049(17) 0.0163(18) O21 0.0589(18) 0.0406(18) 0.0320(15) 0.0037(14) 0.0049(12) 0.0018(14) O30 0.0454(18) 0.0393(18) 0.070(2) 0.0158(15) 0.0167(16) 0.0013(14) O31 0.0403(16) 0.0402(16) 0.0335(15) 0.0010(13) 0.0104(12) -0.0088(13) O40 0.094(3) 0.047(2) 0.0326(17) 0.0070(14) -0.0022(16) 0.0085(18) O41 0.0349(15) 0.0502(18) 0.0351(15) 0.0049(13) 0.0039(12) 0.0037(13) O50 0.0344(16) 0.053(2) 0.101(3) 0.0059(19) 0.0082(16) -0.0032(15) O51 0.0352(14) 0.0419(17) 0.0449(16) -0.0044(14) 0.0022(12) -0.0041(13) C11 0.042(2) 0.061(3) 0.043(3) -0.002(2) 0.016(2) 0.005(2) C12 0.060(3) 0.088(4) 0.052(3) -0.022(3) 0.018(2) 0.005(3) C13 0.053(3) 0.052(3) 0.047(3) -0.015(2) 0.007(2) 0.008(2) C14 0.073(4) 0.073(4) 0.060(3) -0.030(3) 0.014(3) -0.002(3) C15 0.061(3) 0.071(4) 0.065(3) -0.031(3) 0.005(3) -0.015(3) C16 0.054(3) 0.050(3) 0.046(3) -0.007(2) 0.009(2) -0.010(2) C17 0.043(2) 0.034(2) 0.034(2) 0.0017(19) 0.0017(19) 0.0030(19) C18 0.040(2) 0.044(3) 0.037(2) -0.004(2) 0.0024(19) 0.007(2) C111 0.088(4) 0.086(4) 0.072(4) 0.022(3) 0.040(3) 0.010(3) C112 0.050(3) 0.120(5) 0.072(4) -0.003(4) 0.016(3) 0.011(3) C21 0.092(4) 0.068(4) 0.025(2) 0.012(2) 0.003(2) 0.021(3) C22 0.157(7) 0.077(4) 0.048(3) 0.018(3) 0.003(4) 0.042(4) C23 0.073(4) 0.055(3) 0.053(3) 0.018(3) 0.004(3) 0.015(3) C24 0.073(4) 0.056(4) 0.078(4) 0.024(3) 0.008(3) 0.012(3) C25 0.061(3) 0.036(3) 0.088(4) 0.008(3) 0.005(3) 0.004(2) C26 0.053(3) 0.048(3) 0.059(3) -0.001(2) -0.002(2) -0.002(2) C27 0.041(2) 0.042(3) 0.040(2) 0.006(2) 0.0022(19) 0.0064(19) C28 0.060(3) 0.044(3) 0.044(3) 0.008(2) 0.003(2) 0.010(2) C212 0.081(4) 0.124(5) 0.049(3) 0.000(3) -0.001(3) 0.008(4) C211 0.081(4) 0.099(5) 0.047(3) 0.029(3) 0.011(3) 0.015(3) C31 0.055(3) 0.039(3) 0.093(4) 0.016(3) 0.018(3) 0.005(2) C32 0.065(3) 0.054(3) 0.092(4) 0.028(3) 0.011(3) -0.002(3) C33 0.050(3) 0.053(3) 0.051(3) 0.011(2) 0.001(2) -0.017(2) C34 0.077(4) 0.075(4) 0.050(3) 0.004(3) 0.025(3) -0.028(3) C35 0.078(4) 0.071(4) 0.053(3) -0.018(3) 0.032(3) -0.024(3) C36 0.064(3) 0.047(3) 0.046(3) -0.016(2) 0.022(2) -0.016(2) C37 0.043(2) 0.047(3) 0.026(2) -0.0039(19) -0.0018(18) -0.015(2) C38 0.039(2) 0.044(3) 0.040(2) 0.005(2) 0.0012(19) -0.006(2) C311 0.069(4) 0.061(4) 0.297(12) 0.080(6) 0.061(6) 0.024(3) C312 0.148(7) 0.061(4) 0.097(5) -0.003(4) 0.026(5) -0.018(4) C41 0.114(5) 0.072(4) 0.035(3) 0.017(3) -0.013(3) -0.010(4) C42 0.110(5) 0.099(5) 0.073(4) 0.039(4) -0.040(4) -0.024(4) C43 0.053(3) 0.067(4) 0.079(4) 0.036(3) -0.011(3) -0.003(3) C44 0.049(3) 0.088(5) 0.142(6) 0.075(5) 0.015(4) 0.019(3) C45 0.073(4) 0.068(4) 0.149(7) 0.053(4) 0.062(4) 0.029(3) C46 0.055(3) 0.059(3) 0.087(4) 0.017(3) 0.038(3) 0.008(3) C47 0.032(2) 0.034(2) 0.061(3) 0.006(2) 0.007(2) -0.0015(19) C48 0.047(3) 0.045(3) 0.054(3) 0.014(2) -0.007(2) -0.003(2) C411 0.121(5) 0.102(5) 0.055(4) 0.031(3) -0.005(3) -0.023(4) C412 0.184(8) 0.117(6) 0.036(3) -0.009(3) 0.008(4) -0.045(5) C51 0.033(2) 0.091(4) 0.089(4) 0.001(3) 0.003(2) -0.013(3) C52 0.052(4) 0.100(5) 0.208(9) 0.006(5) 0.022(4) -0.027(4) C53 0.056(3) 0.059(4) 0.076(4) 0.004(3) 0.009(3) -0.019(3) C54 0.077(4) 0.066(4) 0.075(4) -0.009(3) 0.010(3) -0.032(3) C55 0.093(4) 0.043(3) 0.066(4) -0.009(3) 0.004(3) -0.009(3) C56 0.055(3) 0.052(3) 0.054(3) -0.013(2) 0.004(2) -0.005(2) C57 0.044(2) 0.040(3) 0.032(2) -0.0036(19) 0.0039(18) -0.007(2) C58 0.047(3) 0.055(3) 0.050(3) 0.002(2) 0.002(2) -0.013(2) C511 0.050(3) 0.193(8) 0.081(4) -0.005(5) 0.014(3) -0.034(4) C512 0.049(3) 0.131(6) 0.086(4) 0.000(4) -0.016(3) -0.007(3) N1 0.067(3) 0.048(3) 0.063(3) 0.006(2) 0.006(2) -0.005(2) N2 0.052(3) 0.068(3) 0.060(3) -0.006(2) 0.007(2) -0.006(2) N3 0.187(9) 0.159(8) 0.236(10) 0.016(7) -0.055(8) -0.050(7) N4 0.139(8) 0.164(9) 0.341(15) -0.131(9) -0.067(8) 0.021(6) C11N 0.049(3) 0.054(3) 0.053(3) 0.003(3) 0.013(2) -0.004(2) C12N 0.071(4) 0.045(3) 0.097(4) 0.003(3) 0.031(3) -0.003(3) C21N 0.040(3) 0.074(4) 0.057(3) -0.010(3) 0.000(2) -0.004(3) C22N 0.060(4) 0.148(6) 0.070(4) 0.013(4) 0.003(3) -0.036(4) C31N 0.085(5) 0.081(5) 0.180(8) 0.022(5) -0.059(5) -0.018(4) C32N 0.078(5) 0.250(11) 0.097(6) -0.014(6) 0.012(4) -0.057(6) C41N 0.128(8) 0.078(6) 0.149(8) -0.024(6) -0.034(6) -0.023(5) C42N 0.250(12) 0.076(6) 0.138(8) 0.016(5) 0.011(8) -0.041(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn O21 1.934(3) . ? Zn O51 1.945(3) . ? Zn O31 1.972(3) . ? Zn Cl 2.2231(12) . ? Zn Li4 3.078(8) . ? Zn Li2 3.296(7) . ? Li1 O41 1.889(7) . ? Li1 O11 1.993(7) . ? Li1 O10 2.006(7) . ? Li1 N1 2.018(8) . ? Li1 Li3 2.564(9) . ? Li1 C18 2.698(8) . ? Li1 C17 2.700(8) . ? Li1 Li2 3.280(10) . ? Li1 Li4 3.287(10) . ? Li2 O11 1.888(7) . ? Li2 O21 1.925(8) . ? Li2 O20 2.005(7) . ? Li2 N2 2.053(8) . ? Li2 C27 2.700(8) . ? Li2 C28 2.713(8) . ? Li2 C17 2.741(8) . ? Li2 Li3 2.879(10) . ? Li3 O11 1.890(7) . ? Li3 O41 1.927(7) . ? Li3 O30 1.960(7) . ? Li3 O31 1.983(7) . ? Li3 C38 2.667(8) . ? Li3 C37 2.682(8) . ? Li3 C47 2.766(8) . ? Li3 Li4 2.881(11) . ? Li4 O51 1.881(8) . ? Li4 O40 1.960(8) . ? Li4 O41 1.988(8) . ? Li4 O50 2.106(9) . ? Li4 C48 2.636(9) . ? Li4 C47 2.643(9) . ? Li4 C57 2.682(9) . ? Li4 C58 2.753(9) . ? O10 C18 1.372(5) . ? O10 C11 1.487(5) . ? O11 C17 1.334(5) . ? O20 C28 1.373(5) . ? O20 C21 1.490(5) . ? O21 C27 1.335(5) . ? O30 C38 1.385(5) . ? O30 C31 1.476(5) . ? O31 C37 1.340(5) . ? O40 C48 1.381(6) . ? O40 C41 1.479(5) . ? O41 C47 1.334(5) . ? O50 C58 1.368(5) . ? O50 C51 1.479(5) . ? O51 C57 1.326(5) . ? C11 C112 1.481(6) . ? C11 C111 1.498(7) . ? C11 C12 1.533(7) . ? C12 C13 1.498(6) . ? C13 C18 1.365(6) . ? C13 C14 1.375(6) . ? C14 C15 1.376(7) . ? C15 C16 1.395(6) . ? C16 C17 1.389(6) . ? C17 C18 1.391(6) . ? C21 C212 1.482(8) . ? C21 C211 1.491(7) . ? C21 C22 1.553(7) . ? C22 C23 1.492(7) . ? C23 C28 1.364(6) . ? C23 C24 1.383(7) . ? C24 C25 1.380(7) . ? C25 C26 1.402(7) . ? C26 C27 1.385(6) . ? C27 C28 1.376(6) . ? C31 C311 1.476(7) . ? C31 C312 1.517(8) . ? C31 C32 1.525(7) . ? C32 C33 1.501(7) . ? C33 C38 1.359(6) . ? C33 C34 1.377(7) . ? C34 C35 1.392(7) . ? C35 C36 1.392(6) . ? C36 C37 1.394(6) . ? C37 C38 1.383(6) . ? C41 C411 1.503(8) . ? C41 C412 1.504(8) . ? C41 C42 1.550(9) . ? C42 C43 1.498(8) . ? C43 C48 1.360(6) . ? C43 C44 1.405(9) . ? C44 C45 1.374(9) . ? C45 C46 1.375(7) . ? C46 C47 1.392(6) . ? C47 C48 1.378(6) . ? C51 C512 1.472(8) . ? C51 C511 1.483(8) . ? C51 C52 1.550(8) . ? C52 C53 1.506(8) . ? C53 C54 1.359(7) . ? C53 C58 1.371(6) . ? C54 C55 1.394(8) . ? C55 C56 1.394(6) . ? C56 C57 1.384(6) . ? C57 C58 1.390(6) . ? N1 C11N 1.126(6) . ? N2 C21N 1.116(6) . ? N3 C31N 1.153(10) . ? N4 C41N 1.062(11) . ? C11N C12N 1.434(7) . ? C21N C22N 1.453(7) . ? C31N C32N 1.303(9) . ? C41N C42N 1.393(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O21 Zn O51 110.75(12) . . ? O21 Zn O31 95.35(11) . . ? O51 Zn O31 95.05(11) . . ? O21 Zn Cl 111.09(9) . . ? O51 Zn Cl 119.13(9) . . ? O31 Zn Cl 122.38(8) . . ? O21 Zn Li4 100.13(17) . . ? O51 Zn Li4 35.74(17) . . ? O31 Zn Li4 61.50(16) . . ? Cl Zn Li4 147.35(15) . . ? O21 Zn Li2 31.24(14) . . ? O51 Zn Li2 119.33(15) . . ? O31 Zn Li2 65.25(14) . . ? Cl Zn Li2 119.57(13) . . ? Li4 Zn Li2 92.11(19) . . ? O41 Li1 O11 94.9(3) . . ? O41 Li1 O10 126.9(4) . . ? O11 Li1 O10 87.6(3) . . ? O41 Li1 N1 112.7(4) . . ? O11 Li1 N1 120.0(4) . . ? O10 Li1 N1 111.4(3) . . ? O41 Li1 Li3 48.4(2) . . ? O11 Li1 Li3 47.0(2) . . ? O10 Li1 Li3 118.8(4) . . ? N1 Li1 Li3 125.5(4) . . ? O41 Li1 C18 123.5(3) . . ? O11 Li1 C18 58.1(2) . . ? O10 Li1 C18 29.50(15) . . ? N1 Li1 C18 123.8(3) . . ? Li3 Li1 C18 94.2(3) . . ? O41 Li1 C17 110.5(3) . . ? O11 Li1 C17 28.21(15) . . ? O10 Li1 C17 59.4(2) . . ? N1 Li1 C17 127.6(3) . . ? Li3 Li1 C17 68.6(2) . . ? C18 Li1 C17 29.86(14) . . ? O41 Li1 Li2 101.6(3) . . ? O11 Li1 Li2 31.36(19) . . ? O10 Li1 Li2 106.8(3) . . ? N1 Li1 Li2 89.5(3) . . ? Li3 Li1 Li2 57.5(2) . . ? C18 Li1 Li2 79.9(2) . . ? C17 Li1 Li2 53.5(2) . . ? O41 Li1 Li4 32.9(2) . . ? O11 Li1 Li4 99.5(3) . . ? O10 Li1 Li4 158.7(4) . . ? N1 Li1 Li4 82.5(3) . . ? Li3 Li1 Li4 57.4(3) . . ? C18 Li1 Li4 150.7(3) . . ? C17 Li1 Li4 125.4(3) . . ? Li2 Li1 Li4 88.7(3) . . ? O11 Li2 O21 116.8(4) . . ? O11 Li2 O20 113.9(4) . . ? O21 Li2 O20 86.1(3) . . ? O11 Li2 N2 111.7(4) . . ? O21 Li2 N2 110.3(4) . . ? O20 Li2 N2 115.9(4) . . ? O11 Li2 C27 126.9(4) . . ? O21 Li2 C27 27.58(15) . . ? O20 Li2 C27 58.6(2) . . ? N2 Li2 C27 118.1(3) . . ? O11 Li2 C28 125.9(3) . . ? O21 Li2 C28 57.0(2) . . ? O20 Li2 C28 29.21(16) . . ? N2 Li2 C28 120.6(3) . . ? C27 Li2 C28 29.46(15) . . ? O11 Li2 C17 26.06(15) . . ? O21 Li2 C17 138.5(4) . . ? O20 Li2 C17 97.0(3) . . ? N2 Li2 C17 105.4(3) . . ? C27 Li2 C17 136.0(3) . . ? C28 Li2 C17 119.3(3) . . ? O11 Li2 Li3 40.4(2) . . ? O21 Li2 Li3 93.4(3) . . ? O20 Li2 Li3 149.3(4) . . ? N2 Li2 Li3 93.0(3) . . ? C27 Li2 Li3 117.8(3) . . ? C28 Li2 Li3 140.2(3) . . ? C17 Li2 Li3 63.7(2) . . ? O11 Li2 Li1 33.3(2) . . ? O21 Li2 Li1 86.3(3) . . ? O20 Li2 Li1 100.8(3) . . ? N2 Li2 Li1 140.0(3) . . ? C27 Li2 Li1 93.7(3) . . ? C28 Li2 Li1 99.0(3) . . ? C17 Li2 Li1 52.36(19) . . ? Li3 Li2 Li1 48.7(2) . . ? O11 Li2 Zn 104.8(3) . . ? O21 Li2 Zn 31.41(14) . . ? O20 Li2 Zn 117.2(3) . . ? N2 Li2 Zn 90.9(3) . . ? C27 Li2 Zn 58.58(16) . . ? C28 Li2 Zn 88.0(2) . . ? C17 Li2 Zn 130.9(3) . . ? Li3 Li2 Zn 69.5(2) . . ? Li1 Li2 Zn 85.6(2) . . ? O11 Li3 O41 97.1(3) . . ? O11 Li3 O30 128.8(4) . . ? O41 Li3 O30 117.7(4) . . ? O11 Li3 O31 115.3(4) . . ? O41 Li3 O31 109.3(4) . . ? O30 Li3 O31 88.5(3) . . ? O11 Li3 Li1 50.4(2) . . ? O41 Li3 Li1 47.2(2) . . ? O30 Li3 Li1 150.7(4) . . ? O31 Li3 Li1 119.1(4) . . ? O11 Li3 C38 135.3(4) . . ? O41 Li3 C38 127.4(3) . . ? O30 Li3 C38 30.17(16) . . ? O31 Li3 C38 58.6(2) . . ? Li1 Li3 C38 174.1(4) . . ? O11 Li3 C37 129.2(3) . . ? O41 Li3 C37 123.6(3) . . ? O30 Li3 C37 60.1(2) . . ? O31 Li3 C37 28.69(15) . . ? Li1 Li3 C37 147.7(4) . . ? C38 Li3 C37 29.95(14) . . ? O11 Li3 C47 112.6(3) . . ? O41 Li3 C47 25.94(15) . . ? O30 Li3 C47 92.2(3) . . ? O31 Li3 C47 116.4(3) . . ? Li1 Li3 C47 67.8(2) . . ? C38 Li3 C47 107.8(3) . . ? C37 Li3 C47 117.0(3) . . ? O11 Li3 Li2 40.3(2) . . ? O41 Li3 Li2 115.8(3) . . ? O30 Li3 Li2 126.6(3) . . ? O31 Li3 Li2 75.2(3) . . ? Li1 Li3 Li2 73.9(3) . . ? C38 Li3 Li2 109.7(3) . . ? C37 Li3 Li2 91.2(3) . . ? C47 Li3 Li2 140.7(3) . . ? O11 Li3 Li4 117.8(3) . . ? O41 Li3 Li4 43.4(2) . . ? O30 Li3 Li4 113.3(3) . . ? O31 Li3 Li4 65.9(3) . . ? Li1 Li3 Li4 74.0(3) . . ? C38 Li3 Li4 100.3(3) . . ? C37 Li3 Li4 83.2(3) . . ? C47 Li3 Li4 55.8(2) . . ? Li2 Li3 Li4 105.7(3) . . ? O51 Li4 O40 129.0(4) . . ? O51 Li4 O41 138.9(4) . . ? O40 Li4 O41 87.7(3) . . ? O51 Li4 O50 85.6(3) . . ? O40 Li4 O50 99.6(4) . . ? O41 Li4 O50 108.5(4) . . ? O51 Li4 C48 159.7(4) . . ? O40 Li4 C48 30.72(18) . . ? O41 Li4 C48 59.1(2) . . ? O50 Li4 C48 97.3(3) . . ? O51 Li4 C47 168.0(4) . . ? O40 Li4 C47 60.4(2) . . ? O41 Li4 C47 29.35(16) . . ? O50 Li4 C47 100.8(3) . . ? C48 Li4 C47 30.27(16) . . ? O51 Li4 C57 27.20(16) . . ? O40 Li4 C57 130.4(4) . . ? O41 Li4 C57 139.6(4) . . ? O50 Li4 C57 58.5(2) . . ? C48 Li4 C57 151.0(4) . . ? C47 Li4 C57 156.0(4) . . ? O51 Li4 C58 56.7(2) . . ? O40 Li4 C58 118.6(4) . . ? O41 Li4 C58 127.1(4) . . ? O50 Li4 C58 28.98(16) . . ? C48 Li4 C58 125.1(3) . . ? C47 Li4 C58 128.5(3) . . ? C57 Li4 C58 29.59(15) . . ? O51 Li4 Li3 109.6(4) . . ? O40 Li4 Li3 92.7(3) . . ? O41 Li4 Li3 41.8(2) . . ? O50 Li4 Li3 147.6(4) . . ? C48 Li4 Li3 78.4(3) . . ? C47 Li4 Li3 59.9(2) . . ? C57 Li4 Li3 130.6(3) . . ? C58 Li4 Li3 148.0(3) . . ? O51 Li4 Zn 37.16(17) . . ? O40 Li4 Zn 127.3(4) . . ? O41 Li4 Zn 108.6(3) . . ? O50 Li4 Zn 119.9(3) . . ? C48 Li4 Zn 142.5(3) . . ? C47 Li4 Zn 132.6(3) . . ? C57 Li4 Zn 62.38(18) . . ? C58 Li4 Zn 91.2(2) . . ? Li3 Li4 Zn 72.7(2) . . ? O51 Li4 Li1 110.0(3) . . ? O40 Li4 Li1 118.8(4) . . ? O41 Li4 Li1 31.13(19) . . ? O50 Li4 Li1 99.7(3) . . ? C48 Li4 Li1 89.4(3) . . ? C47 Li4 Li1 59.1(2) . . ? C57 Li4 Li1 109.2(3) . . ? C58 Li4 Li1 105.4(3) . . ? Li3 Li4 Li1 48.6(2) . . ? Zn Li4 Li1 89.1(2) . . ? C18 O10 C11 107.1(3) . . ? C18 O10 Li1 104.5(3) . . ? C11 O10 Li1 146.0(3) . . ? C17 O11 Li2 115.5(3) . . ? C17 O11 Li3 133.5(3) . . ? Li2 O11 Li3 99.3(3) . . ? C17 O11 Li1 106.8(3) . . ? Li2 O11 Li1 115.3(3) . . ? Li3 O11 Li1 82.6(3) . . ? C28 O20 C21 108.0(3) . . ? C28 O20 Li2 105.3(3) . . ? C21 O20 Li2 146.3(4) . . ? C27 O21 Li2 110.5(3) . . ? C27 O21 Zn 130.5(3) . . ? Li2 O21 Zn 117.3(2) . . ? C38 O30 C31 107.1(3) . . ? C38 O30 Li3 104.5(3) . . ? C31 O30 Li3 145.6(4) . . ? C37 O31 Zn 127.0(3) . . ? C37 O31 Li3 106.0(3) . . ? Zn O31 Li3 126.8(2) . . ? C48 O40 C41 107.8(4) . . ? C48 O40 Li4 102.8(3) . . ? C41 O40 Li4 148.5(4) . . ? C47 O41 Li1 134.4(3) . . ? C47 O41 Li3 114.8(3) . . ? Li1 O41 Li3 84.4(3) . . ? C47 O41 Li4 103.7(3) . . ? Li1 O41 Li4 115.9(3) . . ? Li3 O41 Li4 94.7(3) . . ? C58 O50 C51 108.2(4) . . ? C58 O50 Li4 102.8(3) . . ? C51 O50 Li4 147.8(4) . . ? C57 O51 Li4 112.4(4) . . ? C57 O51 Zn 132.3(3) . . ? Li4 O51 Zn 107.1(3) . . ? C112 C11 O10 106.8(4) . . ? C112 C11 C111 113.0(5) . . ? O10 C11 C111 106.0(4) . . ? C112 C11 C12 114.0(4) . . ? O10 C11 C12 103.9(4) . . ? C111 C11 C12 112.2(4) . . ? C13 C12 C11 103.6(4) . . ? C18 C13 C14 119.4(4) . . ? C18 C13 C12 107.5(4) . . ? C14 C13 C12 133.1(4) . . ? C13 C14 C15 118.1(4) . . ? C14 C15 C16 121.6(5) . . ? C17 C16 C15 121.2(4) . . ? O11 C17 C16 125.3(4) . . ? O11 C17 C18 119.9(4) . . ? C16 C17 C18 114.8(4) . . ? O11 C17 Li1 44.9(2) . . ? C16 C17 Li1 170.2(3) . . ? C18 C17 Li1 75.0(3) . . ? O11 C17 Li2 38.5(2) . . ? C16 C17 Li2 96.8(3) . . ? C18 C17 Li2 136.1(3) . . ? Li1 C17 Li2 74.1(2) . . ? C13 C18 O10 113.9(4) . . ? C13 C18 C17 124.9(4) . . ? O10 C18 C17 121.2(4) . . ? C13 C18 Li1 159.9(4) . . ? O10 C18 Li1 46.0(2) . . ? C17 C18 Li1 75.2(3) . . ? C212 C21 O20 106.8(4) . . ? C212 C21 C211 112.8(5) . . ? O20 C21 C211 106.4(4) . . ? C212 C21 C22 112.8(5) . . ? O20 C21 C22 104.8(4) . . ? C211 C21 C22 112.5(5) . . ? C23 C22 C21 104.2(4) . . ? C28 C23 C24 118.6(5) . . ? C28 C23 C22 108.6(5) . . ? C24 C23 C22 132.7(5) . . ? C25 C24 C23 118.5(5) . . ? C24 C25 C26 121.3(5) . . ? C27 C26 C25 120.7(5) . . ? O21 C27 C28 117.6(4) . . ? O21 C27 C26 126.8(4) . . ? C28 C27 C26 115.5(4) . . ? O21 C27 Li2 41.9(2) . . ? C28 C27 Li2 75.8(3) . . ? C26 C27 Li2 167.8(4) . . ? C23 C28 O20 114.4(4) . . ? C23 C28 C27 125.4(5) . . ? O20 C28 C27 120.1(4) . . ? C23 C28 Li2 159.5(4) . . ? O20 C28 Li2 45.5(2) . . ? C27 C28 Li2 74.7(3) . . ? O30 C31 C311 106.8(4) . . ? O30 C31 C312 105.6(4) . . ? C311 C31 C312 115.4(6) . . ? O30 C31 C32 104.6(4) . . ? C311 C31 C32 113.5(5) . . ? C312 C31 C32 109.9(5) . . ? C33 C32 C31 103.6(4) . . ? C38 C33 C34 119.1(5) . . ? C38 C33 C32 107.8(4) . . ? C34 C33 C32 133.1(4) . . ? C33 C34 C35 118.1(4) . . ? C36 C35 C34 121.2(5) . . ? C35 C36 C37 121.2(5) . . ? O31 C37 C38 119.5(4) . . ? O31 C37 C36 125.8(4) . . ? C38 C37 C36 114.7(4) . . ? O31 C37 Li3 45.3(2) . . ? C38 C37 Li3 74.4(3) . . ? C36 C37 Li3 169.7(4) . . ? C33 C38 C37 125.6(4) . . ? C33 C38 O30 113.5(4) . . ? C37 C38 O30 120.8(4) . . ? C33 C38 Li3 158.7(4) . . ? C37 C38 Li3 75.6(3) . . ? O30 C38 Li3 45.4(2) . . ? O40 C41 C411 106.1(4) . . ? O40 C41 C412 106.1(4) . . ? C411 C41 C412 113.2(6) . . ? O40 C41 C42 103.3(5) . . ? C411 C41 C42 112.4(5) . . ? C412 C41 C42 114.6(5) . . ? C43 C42 C41 103.9(4) . . ? C48 C43 C44 117.0(6) . . ? C48 C43 C42 107.6(5) . . ? C44 C43 C42 135.4(5) . . ? C45 C44 C43 119.0(5) . . ? C44 C45 C46 121.5(6) . . ? C45 C46 C47 121.3(6) . . ? O41 C47 C48 120.0(4) . . ? O41 C47 C46 125.0(4) . . ? C48 C47 C46 114.9(4) . . ? O41 C47 Li4 46.9(2) . . ? C48 C47 Li4 74.6(3) . . ? C46 C47 Li4 165.3(4) . . ? O41 C47 Li3 39.2(2) . . ? C48 C47 Li3 110.4(3) . . ? C46 C47 Li3 118.8(4) . . ? Li4 C47 Li3 64.3(2) . . ? C43 C48 C47 126.2(5) . . ? C43 C48 O40 113.8(5) . . ? C47 C48 O40 119.9(4) . . ? C43 C48 Li4 155.0(4) . . ? C47 C48 Li4 75.2(3) . . ? O40 C48 Li4 46.5(2) . . ? C512 C51 O50 107.7(4) . . ? C512 C51 C511 113.7(6) . . ? O50 C51 C511 106.2(4) . . ? C512 C51 C52 111.0(5) . . ? O50 C51 C52 104.9(4) . . ? C511 C51 C52 112.8(6) . . ? C53 C52 C51 104.3(4) . . ? C54 C53 C58 119.8(5) . . ? C54 C53 C52 132.9(5) . . ? C58 C53 C52 107.3(5) . . ? C53 C54 C55 118.2(5) . . ? C56 C55 C54 120.9(5) . . ? C57 C56 C55 121.7(5) . . ? O51 C57 C56 126.9(4) . . ? O51 C57 C58 118.3(4) . . ? C56 C57 C58 114.7(4) . . ? O51 C57 Li4 40.4(2) . . ? C56 C57 Li4 166.9(4) . . ? C58 C57 Li4 78.0(3) . . ? O50 C58 C53 114.8(4) . . ? O50 C58 C57 120.5(4) . . ? C53 C58 C57 124.6(5) . . ? O50 C58 Li4 48.3(2) . . ? C53 C58 Li4 162.5(4) . . ? C57 C58 Li4 72.4(3) . . ? C11N N1 Li1 171.5(5) . . ? C21N N2 Li2 157.6(5) . . ? N1 C11N C12N 177.8(5) . . ? N2 C21N C22N 179.3(6) . . ? N3 C31N C32N 170.7(13) . . ? N4 C41N C42N 178.4(13) . . ? _diffrn_measured_fraction_theta_max 0.498 _diffrn_reflns_theta_full 26.89 _diffrn_measured_fraction_theta_full 0.498 _refine_diff_density_max 0.587 _refine_diff_density_min -0.343 _refine_diff_density_rms 0.048 data_compound_2 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C96 H112 N8 Na8 O16' _chemical_formula_weight 1817.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 9.988(2) _cell_length_b 18.643(4) _cell_length_c 28.848(6) _cell_angle_alpha 84.29(3) _cell_angle_beta 84.32(3) _cell_angle_gamma 76.00(3) _cell_volume 5170.6(19) _cell_formula_units_Z 2 _cell_measurement_temperature 298(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 15 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.168 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.107 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Kuma KM4 automatic diffractometer' _diffrn_measurement_method 'profile data from omega-2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.4 _diffrn_reflns_number 7022 _diffrn_reflns_av_R_equivalents 0.0088 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.02 _reflns_number_total 6406 _reflns_number_gt 5403 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kuma KM4 software 1996' _computing_cell_refinement 'Kuma KM4 software 1996' _computing_data_reduction 'Kuma KM4 software 1996' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII, 1976' _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 w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+2.4630P] 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 6406 _refine_ls_number_parameters 1177 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.1183 _refine_ls_wR_factor_gt 0.1069 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.217 _refine_ls_shift/su_mean 0.026 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na 0.5643(2) 0.81217(10) 0.34840(7) 0.0740(5) Uani 1 d . . . Na2 Na 0.85843(18) 0.74024(10) 0.29709(7) 0.0643(5) Uani 1 d . . . Na3 Na 0.62634(19) 0.63730(9) 0.32444(7) 0.0705(5) Uani 1 d . . . Na4 Na 0.7893(2) 0.67839(10) 0.40532(7) 0.0762(5) Uani 1 d . . . Na5 Na 0.8857(2) 0.35213(10) 0.17283(8) 0.0811(6) Uani 1 d . . . Na6 Na 0.7273(2) 0.30001(10) 0.09331(7) 0.0795(6) Uani 1 d . . . Na7 Na 0.9311(2) 0.17314(10) 0.16094(7) 0.0718(5) Uani 1 d . . . Na8 Na 0.63973(19) 0.25928(10) 0.20462(7) 0.0687(5) Uani 1 d . . . O10 O 0.4237(4) 0.8398(2) 0.41859(13) 0.0922(11) Uani 1 d . . . O11 O 0.5563(4) 0.69870(17) 0.38995(12) 0.0762(10) Uani 1 d . . . O20 O 0.8380(4) 0.77961(17) 0.21657(11) 0.0677(9) Uani 1 d . . . O21 O 0.6271(3) 0.74896(16) 0.28176(12) 0.0670(9) Uani 1 d . . . O30 O 0.7414(4) 0.50873(16) 0.33085(14) 0.0868(11) Uani 1 d . . . O31 O 0.8659(3) 0.62731(17) 0.33445(12) 0.0738(9) Uani 1 d . . . O40 O 0.8405(5) 0.7541(2) 0.45967(13) 0.1120(14) Uani 1 d . . . O41 O 0.7908(3) 0.79460(17) 0.36577(11) 0.0717(9) Uani 1 d . . . O50 O 0.7716(4) 0.48557(17) 0.16255(13) 0.0877(11) Uani 1 d . . . O51 O 0.6477(4) 0.36604(17) 0.15941(13) 0.0843(11) Uani 1 d . . . O60 O 0.6639(4) 0.21842(17) 0.04558(12) 0.0876(11) Uani 1 d . . . O61 O 0.7088(4) 0.19311(17) 0.14078(11) 0.0722(9) Uani 1 d . . . O70 O 1.0711(4) 0.1274(2) 0.09582(13) 0.0934(11) Uani 1 d . . . O71 O 0.9583(4) 0.27847(18) 0.11207(12) 0.0787(10) Uani 1 d . . . O80 O 0.6522(4) 0.21819(17) 0.28609(11) 0.0680(9) Uani 1 d . . . O81 O 0.8694(3) 0.24792(17) 0.22227(12) 0.0684(9) Uani 1 d . . . N1 N 0.4640(8) 0.9285(3) 0.3045(2) 0.140(2) Uani 1 d . . . N2 N 1.0968(6) 0.7686(4) 0.2956(2) 0.127(2) Uani 1 d . . . N3 N 0.4223(7) 0.6068(4) 0.2952(3) 0.140(3) Uani 1 d . . . N4 N 0.8348(7) 0.5666(3) 0.4598(2) 0.133(2) Uani 1 d . . . N5 N 1.0894(8) 0.3843(4) 0.1990(3) 0.149(3) Uani 1 d . . . N6 N 0.6971(7) 0.4055(3) 0.0335(2) 0.131(2) Uani 1 d . . . N7 N 1.0096(8) 0.0615(3) 0.2126(2) 0.134(2) Uani 1 d . . . N8 N 0.4071(7) 0.2299(4) 0.2067(3) 0.140(3) Uani 1 d . . . C11N C 0.4457(8) 0.9554(4) 0.2698(3) 0.108(2) Uani 1 d . . . C12N C 0.4197(9) 0.9896(4) 0.2233(3) 0.154(3) Uani 1 d . . . H12A H 0.5062 0.9894 0.2055 0.185 Uiso 1 calc R . . H12B H 0.3673 1.0399 0.2253 0.185 Uiso 1 calc R . . H12C H 0.3684 0.9625 0.2083 0.185 Uiso 1 calc R . . C11 C 0.3518(7) 0.9027(3) 0.4459(2) 0.0953(18) Uani 1 d . . . C12 C 0.2898(9) 0.8683(4) 0.4910(2) 0.137(3) Uani 1 d . . . H12A H 0.3184 0.8853 0.5183 0.165 Uiso 1 calc R . . H12B H 0.1895 0.8807 0.4921 0.165 Uiso 1 calc R . . C13 C 0.3461(6) 0.7871(4) 0.4885(2) 0.0910(17) Uani 1 d . . . C14 C 0.3339(7) 0.7270(5) 0.5193(2) 0.103(2) Uani 1 d . . . H14 H 0.2853 0.7336 0.5483 0.124 Uiso 1 calc R . . C15 C 0.3948(7) 0.6580(4) 0.5060(2) 0.1018(19) Uani 1 d . . . H15 H 0.3864 0.6170 0.5263 0.122 Uiso 1 calc R . . C16 C 0.4694(6) 0.6467(3) 0.46283(19) 0.0851(15) Uani 1 d . . . H16 H 0.5094 0.5985 0.4551 0.102 Uiso 1 calc R . . C17 C 0.4858(5) 0.7056(3) 0.43096(18) 0.0706(13) Uani 1 d . . . C18 C 0.4196(5) 0.7749(3) 0.44641(18) 0.0733(14) Uani 1 d . . . C111 C 0.4561(7) 0.9444(4) 0.4525(3) 0.154(3) Uani 1 d . . . H11A H 0.4125 0.9876 0.4687 0.185 Uiso 1 calc R . . H11B H 0.4967 0.9591 0.4226 0.185 Uiso 1 calc R . . H11C H 0.5270 0.9134 0.4706 0.185 Uiso 1 calc R . . C112 C 0.2444(7) 0.9498(4) 0.4166(3) 0.145(3) Uani 1 d . . . H11D H 0.2018 0.9944 0.4315 0.175 Uiso 1 calc R . . H11E H 0.1755 0.9232 0.4130 0.175 Uiso 1 calc R . . H11F H 0.2867 0.9622 0.3865 0.175 Uiso 1 calc R . . C21N C 1.1360(7) 0.7620(4) 0.3302(3) 0.102(2) Uani 1 d . . . C22N C 1.1848(9) 0.7478(5) 0.3760(3) 0.180(4) Uani 1 d . . . H22A H 1.2073 0.7915 0.3849 0.216 Uiso 1 calc R . . H22B H 1.2658 0.7077 0.3759 0.216 Uiso 1 calc R . . H22C H 1.1139 0.7347 0.3978 0.216 Uiso 1 calc R . . C21 C 0.9078(6) 0.8170(3) 0.1778(2) 0.0811(17) Uani 1 d . . . C22 C 0.8190(6) 0.8230(3) 0.13690(19) 0.0892(17) Uani 1 d . . . H22A H 0.8089 0.8711 0.1195 0.107 Uiso 1 calc R . . H22B H 0.8587 0.7845 0.1159 0.107 Uiso 1 calc R . . C23 C 0.6836(6) 0.8133(3) 0.15991(19) 0.0680(14) Uani 1 d . . . C24 C 0.5546(7) 0.8239(3) 0.1435(2) 0.0802(16) Uani 1 d . . . H24 H 0.5389 0.8413 0.1127 0.096 Uiso 1 calc R . . C25 C 0.4514(7) 0.8079(3) 0.1741(3) 0.0887(19) Uani 1 d . . . H25 H 0.3637 0.8141 0.1638 0.106 Uiso 1 calc R . . C26 C 0.4728(6) 0.7827(3) 0.2204(2) 0.0769(15) Uani 1 d . . . H26 H 0.3987 0.7728 0.2400 0.092 Uiso 1 calc R . . C27 C 0.6018(6) 0.7715(2) 0.23862(18) 0.0613(13) Uani 1 d . . . C28 C 0.7032(5) 0.7880(2) 0.20550(17) 0.0567(12) Uani 1 d . . . C211 C 1.0506(7) 0.7707(5) 0.1697(2) 0.139(3) Uani 1 d . . . H21A H 1.0953 0.7905 0.1420 0.167 Uiso 1 calc R . . H21B H 1.0466 0.7208 0.1658 0.167 Uiso 1 calc R . . H21C H 1.1021 0.7711 0.1960 0.167 Uiso 1 calc R . . C212 C 0.9027(8) 0.8918(4) 0.1933(2) 0.142(3) Uani 1 d . . . H21D H 0.9348 0.9220 0.1678 0.170 Uiso 1 calc R . . H21E H 0.9607 0.8866 0.2187 0.170 Uiso 1 calc R . . H21F H 0.8091 0.9149 0.2036 0.170 Uiso 1 calc R . . C31N C 0.3494(10) 0.6067(4) 0.2692(4) 0.119(3) Uani 1 d . . . C32N C 0.2492(12) 0.6054(5) 0.2376(3) 0.202(5) Uani 1 d . . . H32A H 0.2935 0.5778 0.2117 0.242 Uiso 1 calc R . . H32B H 0.2072 0.6553 0.2265 0.242 Uiso 1 calc R . . H32C H 0.1794 0.5824 0.2534 0.242 Uiso 1 calc R . . C31 C 0.7128(7) 0.4341(3) 0.3331(2) 0.0853(17) Uani 1 d . . . C32 C 0.8431(8) 0.3795(3) 0.3468(4) 0.158(4) Uani 1 d . . . H32A H 0.8286 0.3547 0.3774 0.189 Uiso 1 calc R . . H32B H 0.8743 0.3425 0.3242 0.189 Uiso 1 calc R . . C33 C 0.9455(7) 0.4262(3) 0.3473(2) 0.0946(19) Uani 1 d . . . C34 C 1.0832(8) 0.4069(4) 0.3559(3) 0.115(2) Uani 1 d . . . H34 H 1.1303 0.3577 0.3613 0.137 Uiso 1 calc R . . C35 C 1.1478(7) 0.4641(4) 0.3561(3) 0.108(2) Uani 1 d . . . H35 H 1.2411 0.4531 0.3615 0.130 Uiso 1 calc R . . C36 C 1.0779(7) 0.5381(3) 0.3485(2) 0.0919(17) Uani 1 d . . . H36 H 1.1255 0.5751 0.3493 0.110 Uiso 1 calc R . . C37 C 0.9389(6) 0.5581(3) 0.33981(17) 0.0692(14) Uani 1 d . . . C38 C 0.8781(6) 0.4989(3) 0.33924(18) 0.0728(15) Uani 1 d . . . C311 C 0.5945(10) 0.4352(4) 0.3688(3) 0.164(4) Uani 1 d . . . H31A H 0.5733 0.3873 0.3727 0.197 Uiso 1 calc R . . H31B H 0.5151 0.4718 0.3588 0.197 Uiso 1 calc R . . H31C H 0.6186 0.4472 0.3980 0.197 Uiso 1 calc R . . C312 C 0.6769(9) 0.4251(3) 0.2856(2) 0.138(3) Uani 1 d . . . H31D H 0.7554 0.4260 0.2636 0.166 Uiso 1 calc R . . H31E H 0.6006 0.4649 0.2769 0.166 Uiso 1 calc R . . H31F H 0.6515 0.3786 0.2856 0.166 Uiso 1 calc R . . C41N C 0.8116(6) 0.5296(4) 0.4898(3) 0.0939(18) Uani 1 d . . . C42N C 0.7813(9) 0.4840(4) 0.5315(3) 0.151(3) Uani 1 d . . . H42A H 0.7993 0.4332 0.5243 0.182 Uiso 1 calc R . . H42B H 0.6858 0.5006 0.5424 0.182 Uiso 1 calc R . . H42C H 0.8389 0.4881 0.5554 0.182 Uiso 1 calc R . . C41 C 0.8543(9) 0.7545(4) 0.5104(2) 0.111(2) Uani 1 d . . . C42 C 0.8811(10) 0.8310(5) 0.5157(3) 0.157(3) Uani 1 d . . . H42A H 0.8156 0.8568 0.5391 0.188 Uiso 1 calc R . . H42B H 0.9742 0.8261 0.5246 0.188 Uiso 1 calc R . . C43 C 0.8627(6) 0.8715(4) 0.4687(2) 0.0959(19) Uani 1 d . . . C44 C 0.8650(7) 0.9428(4) 0.4533(3) 0.108(2) Uani 1 d . . . H44 H 0.8801 0.9757 0.4733 0.130 Uiso 1 calc R . . C45 C 0.8444(7) 0.9637(3) 0.4078(3) 0.107(2) Uani 1 d . . . H45 H 0.8475 1.0118 0.3963 0.128 Uiso 1 calc R . . C46 C 0.8186(5) 0.9151(3) 0.3773(2) 0.0845(16) Uani 1 d . . . H46 H 0.8035 0.9319 0.3463 0.101 Uiso 1 calc R . . C47 C 0.8153(5) 0.8426(3) 0.39241(18) 0.0671(13) Uani 1 d . . . C48 C 0.8393(5) 0.8238(3) 0.43955(19) 0.0745(14) Uani 1 d . . . C411 C 0.7245(8) 0.7424(5) 0.5343(2) 0.150(3) Uani 1 d . . . H41A H 0.7319 0.7370 0.5674 0.180 Uiso 1 calc R . . H41B H 0.7062 0.6982 0.5245 0.180 Uiso 1 calc R . . H41C H 0.6502 0.7840 0.5267 0.180 Uiso 1 calc R . . C412 C 0.9742(8) 0.6931(5) 0.5217(3) 0.154(3) Uani 1 d . . . H41D H 0.9827 0.6881 0.5548 0.185 Uiso 1 calc R . . H41E H 1.0570 0.7037 0.5057 0.185 Uiso 1 calc R . . H41F H 0.9607 0.6478 0.5119 0.185 Uiso 1 calc R . . C51N C 1.1701(10) 0.3914(4) 0.2201(3) 0.116(3) Uani 1 d . . . C52N C 1.2842(10) 0.4011(4) 0.2451(3) 0.160(3) Uani 1 d . . . H52A H 1.3461 0.3537 0.2515 0.192 Uiso 1 calc R . . H52B H 1.2481 0.4226 0.2739 0.192 Uiso 1 calc R . . H52C H 1.3334 0.4332 0.2262 0.192 Uiso 1 calc R . . C51 C 0.8026(7) 0.5599(3) 0.1592(2) 0.0924(18) Uani 1 d . . . C52 C 0.6734(8) 0.6140(3) 0.1422(3) 0.135(3) Uani 1 d . . . H52A H 0.6354 0.6507 0.1645 0.162 Uiso 1 calc R . . H52B H 0.6941 0.6392 0.1122 0.162 Uiso 1 calc R . . C53 C 0.5747(8) 0.5670(3) 0.1378(2) 0.0934(19) Uani 1 d . . . C54 C 0.4416(9) 0.5837(4) 0.1241(3) 0.123(3) Uani 1 d . . . H54 H 0.3955 0.6324 0.1161 0.148 Uiso 1 calc R . . C55 C 0.3799(8) 0.5261(4) 0.1225(3) 0.124(3) Uani 1 d . . . H55 H 0.2908 0.5361 0.1128 0.149 Uiso 1 calc R . . C56 C 0.4455(7) 0.4539(3) 0.1349(2) 0.102(2) Uani 1 d . . . H56 H 0.3980 0.4170 0.1339 0.123 Uiso 1 calc R . . C57 C 0.5792(6) 0.4339(3) 0.14887(18) 0.0763(15) Uani 1 d . . . C58 C 0.6390(7) 0.4949(3) 0.14990(19) 0.0781(16) Uani 1 d . . . C511 C 0.8317(10) 0.5729(3) 0.2068(3) 0.148(3) Uani 1 d . . . H51A H 0.8515 0.6208 0.2063 0.177 Uiso 1 calc R . . H51B H 0.9100 0.5354 0.2168 0.177 Uiso 1 calc R . . H51C H 0.7524 0.5707 0.2282 0.177 Uiso 1 calc R . . C512 C 0.9254(9) 0.5559(4) 0.1244(3) 0.153(3) Uani 1 d . . . H51D H 1.0029 0.5194 0.1358 0.183 Uiso 1 calc R . . H51E H 0.9481 0.6034 0.1198 0.183 Uiso 1 calc R . . H51F H 0.9039 0.5424 0.0952 0.183 Uiso 1 calc R . . C61N C 0.6982(7) 0.4603(4) 0.0168(2) 0.106(2) Uani 1 d . . . C62N C 0.6983(12) 0.5327(4) -0.0043(4) 0.216(5) Uani 1 d . . . H62A H 0.6207 0.5679 0.0089 0.259 Uiso 1 calc R . . H62B H 0.6917 0.5336 -0.0374 0.259 Uiso 1 calc R . . H62C H 0.7825 0.5455 0.0012 0.259 Uiso 1 calc R . . C61 C 0.6410(7) 0.2099(3) -0.0034(2) 0.0889(17) Uani 1 d . . . C62 C 0.5994(8) 0.1363(3) -0.0026(2) 0.114(2) Uani 1 d . . . H62A H 0.5047 0.1441 -0.0107 0.136 Uiso 1 calc R . . H62B H 0.6599 0.1042 -0.0243 0.136 Uiso 1 calc R . . C63 C 0.6139(5) 0.1036(3) 0.04628(19) 0.0721(14) Uani 1 d . . . C64 C 0.6556(5) 0.0742(2) 0.13936(19) 0.0760(14) Uani 1 d . . . H64 H 0.6688 0.0623 0.1709 0.091 Uiso 1 calc R . . C65 C 0.5970(5) 0.0371(3) 0.0679(2) 0.0785(15) Uani 1 d . . . H65 H 0.5716 0.0024 0.0516 0.094 Uiso 1 calc R . . C66 C 0.6185(6) 0.0237(3) 0.1139(2) 0.0857(16) Uani 1 d . . . H66 H 0.6080 -0.0213 0.1291 0.103 Uiso 1 calc R . . C67 C 0.6737(5) 0.1428(2) 0.11872(17) 0.0603(12) Uani 1 d . . . C68 C 0.6509(5) 0.1534(2) 0.07179(18) 0.0636(13) Uani 1 d . . . C611 C 0.5251(8) 0.2746(4) -0.0163(3) 0.131(3) Uani 1 d . . . H61A H 0.5091 0.2743 -0.0485 0.158 Uiso 1 calc R . . H61B H 0.5495 0.3199 -0.0115 0.158 Uiso 1 calc R . . H61C H 0.4426 0.2709 0.0030 0.158 Uiso 1 calc R . . C612 C 0.7726(8) 0.2135(5) -0.0311(2) 0.158(3) Uani 1 d . . . H61D H 0.7624 0.2101 -0.0635 0.189 Uiso 1 calc R . . H61E H 0.8452 0.1730 -0.0205 0.189 Uiso 1 calc R . . H61F H 0.7954 0.2596 -0.0273 0.189 Uiso 1 calc R . . C71N C 1.0285(7) 0.0329(4) 0.2488(3) 0.105(2) Uani 1 d . . . C72N C 1.0518(9) -0.0017(4) 0.2942(3) 0.152(3) Uani 1 d . . . H72A H 1.1203 -0.0476 0.2921 0.182 Uiso 1 calc R . . H72B H 0.9670 -0.0114 0.3091 0.182 Uiso 1 calc R . . H72C H 1.0839 0.0304 0.3123 0.182 Uiso 1 calc R . . C71 C 1.1285(6) 0.0573(3) 0.0738(2) 0.0938(18) Uani 1 d . . . C72 C 1.2042(7) 0.0770(4) 0.0281(2) 0.126(2) Uani 1 d . . . H72A H 1.3037 0.0609 0.0296 0.151 Uiso 1 calc R . . H72B H 1.1774 0.0550 0.0024 0.151 Uiso 1 calc R . . C73 C 1.1587(6) 0.1593(5) 0.0230(2) 0.0964(19) Uani 1 d . . . C74 C 1.1817(8) 0.2122(6) -0.0126(3) 0.133(3) Uani 1 d . . . H74 H 1.2321 0.1977 -0.0403 0.159 Uiso 1 calc R . . C75 C 1.1284(8) 0.2868(6) -0.0062(3) 0.136(3) Uani 1 d . . . H75 H 1.1422 0.3218 -0.0303 0.164 Uiso 1 calc R . . C76 C 1.0543(6) 0.3113(4) 0.0356(2) 0.113(2) Uani 1 d . . . H76 H 1.0225 0.3617 0.0391 0.136 Uiso 1 calc R . . C77 C 1.0285(5) 0.2598(4) 0.07190(19) 0.0795(15) Uani 1 d . . . C78 C 1.0844(5) 0.1847(4) 0.06317(18) 0.0790(15) Uani 1 d . . . C711 C 1.0054(6) 0.0264(4) 0.0669(3) 0.116(2) Uani 1 d . . . H71A H 1.0372 -0.0207 0.0539 0.140 Uiso 1 calc R . . H71B H 0.9465 0.0601 0.0459 0.140 Uiso 1 calc R . . H71C H 0.9545 0.0204 0.0964 0.140 Uiso 1 calc R . . C712 C 1.2224(7) 0.0073(4) 0.1079(3) 0.135(3) Uani 1 d . . . H71D H 1.2511 -0.0417 0.0973 0.162 Uiso 1 calc R . . H71E H 1.1734 0.0054 0.1382 0.162 Uiso 1 calc R . . H71F H 1.3024 0.0266 0.1098 0.162 Uiso 1 calc R . . C81N C 0.3627(7) 0.2234(4) 0.1746(3) 0.110(2) Uani 1 d . . . C82N C 0.3062(8) 0.2190(6) 0.1318(3) 0.215(5) Uani 1 d . . . H82A H 0.2070 0.2314 0.1362 0.258 Uiso 1 calc R . . H82B H 0.3375 0.1694 0.1221 0.258 Uiso 1 calc R . . H82C H 0.3361 0.2530 0.1082 0.258 Uiso 1 calc R . . C81 C 0.5797(6) 0.1813(3) 0.3241(2) 0.0802(17) Uani 1 d . . . C82 C 0.6638(6) 0.1751(3) 0.36579(19) 0.0891(17) Uani 1 d . . . H82A H 0.6237 0.2143 0.3863 0.107 Uiso 1 calc R . . H82B H 0.6708 0.1275 0.3835 0.107 Uiso 1 calc R . . C83 C 0.8024(6) 0.1830(3) 0.34360(19) 0.0702(15) Uani 1 d . . . C84 C 0.9291(8) 0.1709(3) 0.3611(2) 0.0912(18) Uani 1 d . . . H84 H 0.9410 0.1536 0.3921 0.109 Uiso 1 calc R . . C85 C 1.0382(7) 0.1848(3) 0.3316(3) 0.094(2) Uani 1 d . . . H85 H 1.1251 0.1767 0.3429 0.113 Uiso 1 calc R . . C86 C 1.0202(6) 0.2110(3) 0.2851(2) 0.0786(16) Uani 1 d . . . H86 H 1.0959 0.2203 0.2661 0.094 Uiso 1 calc R . . C87 C 0.8921(6) 0.2239(2) 0.26607(18) 0.0598(12) Uani 1 d . . . C88 C 0.7867(6) 0.2084(2) 0.29800(18) 0.0613(13) Uani 1 d . . . C811 C 0.4343(6) 0.2292(4) 0.3311(2) 0.129(3) Uani 1 d . . . H81A H 0.3868 0.2094 0.3581 0.154 Uiso 1 calc R . . H81B H 0.3852 0.2296 0.3041 0.154 Uiso 1 calc R . . H81C H 0.4387 0.2789 0.3356 0.154 Uiso 1 calc R . . C812 C 0.5811(8) 0.1064(3) 0.3090(2) 0.126(2) Uani 1 d . . . H81D H 0.5348 0.1123 0.2808 0.151 Uiso 1 calc R . . H81E H 0.5344 0.0800 0.3331 0.151 Uiso 1 calc R . . H81F H 0.6751 0.0791 0.3035 0.151 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 0.0883(14) 0.0663(11) 0.0637(13) -0.0048(9) 0.0002(10) -0.0136(10) Na2 0.0722(12) 0.0692(11) 0.0534(12) -0.0014(9) -0.0077(9) -0.0203(9) Na3 0.0789(13) 0.0608(11) 0.0729(14) -0.0065(9) -0.0035(10) -0.0187(9) Na4 0.0970(14) 0.0794(12) 0.0552(12) 0.0022(9) -0.0123(10) -0.0269(11) Na5 0.0949(15) 0.0633(11) 0.0877(16) -0.0078(10) -0.0111(12) -0.0212(11) Na6 0.1083(15) 0.0674(11) 0.0673(13) 0.0056(9) -0.0189(11) -0.0290(11) Na7 0.0862(13) 0.0654(11) 0.0600(12) -0.0095(9) 0.0029(10) -0.0118(10) Na8 0.0773(13) 0.0753(11) 0.0540(12) -0.0066(9) -0.0111(10) -0.0156(10) O10 0.116(3) 0.084(2) 0.070(3) -0.023(2) 0.017(2) -0.014(2) O11 0.090(2) 0.075(2) 0.061(2) -0.0069(17) 0.0099(19) -0.0218(18) O20 0.077(2) 0.080(2) 0.046(2) 0.0087(16) -0.0075(18) -0.0242(18) O21 0.078(2) 0.070(2) 0.055(2) 0.0030(17) -0.0086(17) -0.0219(17) O30 0.091(3) 0.051(2) 0.120(3) -0.0012(19) -0.025(2) -0.0161(19) O31 0.085(2) 0.061(2) 0.075(2) -0.0035(17) -0.0104(19) -0.0170(19) O40 0.179(4) 0.114(3) 0.056(3) -0.002(2) -0.032(3) -0.053(3) O41 0.097(3) 0.070(2) 0.055(2) -0.0099(16) -0.0098(18) -0.0304(19) O50 0.104(3) 0.054(2) 0.105(3) -0.0033(19) -0.016(2) -0.017(2) O51 0.107(3) 0.052(2) 0.093(3) -0.0050(18) -0.020(2) -0.0125(19) O60 0.141(3) 0.071(2) 0.056(2) -0.0040(18) -0.020(2) -0.030(2) O61 0.102(3) 0.067(2) 0.053(2) -0.0059(16) -0.0060(19) -0.0298(19) O70 0.113(3) 0.092(2) 0.072(3) -0.026(2) 0.019(2) -0.021(2) O71 0.095(3) 0.080(2) 0.062(2) 0.0001(18) 0.005(2) -0.0288(19) O80 0.067(2) 0.087(2) 0.052(2) -0.0036(17) -0.0130(18) -0.0198(18) O81 0.079(2) 0.071(2) 0.054(2) -0.0085(17) -0.0023(18) -0.0168(17) N1 0.197(6) 0.095(4) 0.113(5) 0.001(4) -0.027(5) 0.000(4) N2 0.095(5) 0.181(6) 0.109(6) -0.015(5) -0.020(4) -0.034(4) N3 0.108(6) 0.119(5) 0.200(9) -0.015(5) -0.033(5) -0.030(4) N4 0.160(5) 0.124(5) 0.102(5) 0.032(4) -0.013(4) -0.022(4) N5 0.129(6) 0.113(5) 0.211(9) -0.009(5) -0.048(5) -0.027(4) N6 0.179(6) 0.108(4) 0.103(5) 0.025(4) -0.025(4) -0.033(4) N7 0.197(6) 0.082(4) 0.110(5) -0.005(4) -0.019(5) -0.003(4) N8 0.100(5) 0.199(7) 0.124(6) -0.060(5) -0.013(4) -0.018(4) C11N 0.123(6) 0.092(5) 0.104(6) -0.006(4) -0.001(5) -0.016(4) C12N 0.181(8) 0.176(7) 0.114(6) 0.032(6) -0.014(6) -0.073(6) C11 0.091(4) 0.097(4) 0.095(5) -0.037(4) 0.006(4) -0.011(4) C12 0.163(7) 0.147(7) 0.090(5) -0.039(5) 0.032(5) -0.019(6) C13 0.083(4) 0.126(5) 0.067(4) -0.024(4) 0.002(3) -0.026(4) C14 0.103(5) 0.153(6) 0.058(4) -0.008(4) 0.012(4) -0.049(5) C15 0.111(5) 0.140(6) 0.066(4) 0.010(4) -0.005(4) -0.059(5) C16 0.095(4) 0.097(4) 0.067(4) 0.003(3) 0.004(3) -0.038(3) C17 0.069(3) 0.090(4) 0.056(3) -0.010(3) -0.003(3) -0.026(3) C18 0.079(4) 0.090(4) 0.054(3) -0.010(3) 0.000(3) -0.027(3) C111 0.111(6) 0.163(7) 0.205(9) -0.117(7) 0.005(6) -0.027(5) C112 0.110(6) 0.170(7) 0.139(7) -0.058(6) -0.021(5) 0.023(5) C21N 0.072(5) 0.142(6) 0.099(6) -0.030(5) -0.022(4) -0.025(4) C22N 0.142(7) 0.257(11) 0.145(8) -0.081(8) -0.054(6) -0.012(7) C21 0.082(4) 0.097(4) 0.067(4) 0.012(3) -0.003(3) -0.036(3) C22 0.107(5) 0.102(4) 0.057(4) 0.000(3) -0.003(4) -0.025(4) C23 0.094(4) 0.064(3) 0.049(3) -0.002(2) -0.015(3) -0.022(3) C24 0.102(5) 0.082(4) 0.065(4) 0.011(3) -0.045(4) -0.029(3) C25 0.088(4) 0.085(4) 0.103(6) 0.000(4) -0.041(4) -0.029(3) C26 0.079(4) 0.076(3) 0.081(4) 0.002(3) -0.020(3) -0.025(3) C27 0.075(4) 0.052(3) 0.058(3) -0.003(2) -0.014(3) -0.015(2) C28 0.060(3) 0.060(3) 0.053(3) -0.004(2) -0.014(3) -0.016(2) C211 0.091(5) 0.228(9) 0.083(5) 0.039(5) 0.002(4) -0.030(5) C212 0.210(8) 0.132(6) 0.117(6) 0.037(5) -0.050(5) -0.111(6) C31N 0.121(8) 0.086(4) 0.151(9) 0.003(5) -0.021(6) -0.024(5) C32N 0.276(13) 0.157(8) 0.179(10) -0.023(7) -0.120(10) -0.022(8) C31 0.109(5) 0.065(3) 0.088(5) 0.005(3) -0.015(4) -0.033(3) C32 0.141(6) 0.066(4) 0.271(11) 0.010(5) -0.073(7) -0.021(5) C33 0.107(5) 0.056(3) 0.117(5) 0.000(3) -0.029(4) -0.005(4) C34 0.114(6) 0.080(4) 0.140(7) 0.008(4) -0.036(5) 0.001(4) C35 0.083(4) 0.113(6) 0.116(6) -0.001(4) -0.023(4) 0.006(4) C36 0.083(4) 0.094(4) 0.100(5) -0.014(3) -0.016(4) -0.016(4) C37 0.085(4) 0.063(3) 0.058(3) -0.003(2) -0.006(3) -0.017(3) C38 0.080(4) 0.063(4) 0.073(4) 0.000(3) -0.013(3) -0.012(3) C311 0.224(9) 0.117(6) 0.144(8) 0.018(5) 0.045(7) -0.064(6) C312 0.256(9) 0.073(4) 0.101(5) -0.008(3) -0.043(6) -0.054(5) C41N 0.093(4) 0.092(4) 0.095(5) -0.002(4) -0.020(4) -0.016(4) C42N 0.184(8) 0.142(6) 0.141(7) 0.028(5) -0.022(6) -0.074(6) C41 0.124(6) 0.157(7) 0.059(4) -0.009(4) -0.031(4) -0.038(5) C42 0.222(9) 0.181(8) 0.089(6) -0.039(6) -0.043(6) -0.066(7) C43 0.093(4) 0.114(5) 0.089(5) -0.039(4) -0.012(4) -0.025(4) C44 0.091(5) 0.114(6) 0.132(7) -0.070(5) -0.004(5) -0.027(4) C45 0.097(5) 0.077(4) 0.153(7) -0.034(5) -0.001(5) -0.029(3) C46 0.091(4) 0.070(3) 0.096(4) -0.007(3) -0.012(3) -0.023(3) C47 0.063(3) 0.072(3) 0.070(4) -0.018(3) -0.002(3) -0.019(3) C48 0.085(4) 0.084(4) 0.060(4) -0.020(3) -0.010(3) -0.023(3) C411 0.121(6) 0.240(10) 0.088(5) -0.037(6) -0.009(5) -0.030(6) C412 0.122(6) 0.248(11) 0.092(6) -0.004(6) -0.029(5) -0.040(7) C51N 0.131(8) 0.095(5) 0.127(7) -0.011(4) -0.011(5) -0.035(5) C52N 0.202(9) 0.171(8) 0.129(7) -0.045(6) -0.040(6) -0.061(7) C51 0.117(5) 0.054(3) 0.104(5) 0.003(3) 0.000(4) -0.024(3) C52 0.159(7) 0.066(4) 0.175(8) 0.008(4) -0.030(6) -0.015(5) C53 0.114(5) 0.061(4) 0.097(5) 0.012(3) -0.013(4) -0.009(4) C54 0.132(7) 0.084(5) 0.134(7) 0.019(4) -0.016(5) 0.003(5) C55 0.102(5) 0.122(6) 0.138(7) 0.012(5) -0.033(5) -0.003(5) C56 0.092(5) 0.090(4) 0.122(5) 0.009(4) -0.032(4) -0.012(4) C57 0.101(5) 0.061(3) 0.061(3) -0.003(3) -0.013(3) -0.006(3) C58 0.101(5) 0.058(4) 0.070(4) 0.001(3) -0.006(3) -0.011(3) C511 0.263(10) 0.087(4) 0.112(6) -0.010(4) -0.028(6) -0.070(6) C512 0.177(8) 0.122(6) 0.149(8) 0.031(5) 0.027(7) -0.049(6) C61N 0.128(5) 0.084(4) 0.097(5) 0.006(4) -0.021(4) -0.007(4) C62N 0.292(12) 0.105(6) 0.268(13) 0.053(7) -0.112(11) -0.072(7) C61 0.111(5) 0.093(4) 0.057(4) -0.005(3) -0.019(3) -0.010(4) C62 0.173(6) 0.090(4) 0.084(5) -0.020(3) -0.031(4) -0.031(4) C63 0.076(4) 0.070(3) 0.072(4) -0.021(3) -0.013(3) -0.012(3) C64 0.087(4) 0.063(3) 0.078(4) 0.002(3) -0.001(3) -0.023(3) C65 0.079(4) 0.068(3) 0.095(5) -0.024(3) -0.007(3) -0.022(3) C66 0.094(4) 0.064(3) 0.103(5) -0.010(3) 0.002(4) -0.028(3) C67 0.059(3) 0.060(3) 0.061(3) -0.009(3) -0.003(2) -0.010(2) C68 0.071(3) 0.053(3) 0.063(4) -0.002(2) -0.005(3) -0.008(2) C611 0.148(6) 0.116(5) 0.138(7) 0.000(5) -0.063(5) -0.028(5) C612 0.154(7) 0.247(10) 0.084(5) -0.052(6) 0.021(5) -0.066(7) C71N 0.126(5) 0.077(4) 0.104(6) -0.010(4) -0.004(5) -0.011(4) C72N 0.176(7) 0.154(7) 0.117(7) 0.032(5) -0.011(6) -0.040(6) C71 0.084(4) 0.109(4) 0.087(5) -0.050(4) 0.007(4) -0.007(4) C72 0.113(5) 0.165(7) 0.099(5) -0.060(5) 0.016(4) -0.022(5) C73 0.077(4) 0.162(6) 0.054(4) -0.016(4) 0.000(3) -0.035(4) C74 0.090(5) 0.235(10) 0.065(5) -0.004(6) -0.005(4) -0.026(6) C75 0.100(6) 0.217(9) 0.078(6) 0.057(6) 0.002(4) -0.041(6) C76 0.105(5) 0.152(6) 0.083(5) 0.039(4) -0.011(4) -0.052(4) C77 0.067(4) 0.121(5) 0.057(4) 0.006(3) -0.008(3) -0.038(3) C78 0.074(4) 0.120(5) 0.047(3) -0.019(3) 0.004(3) -0.028(3) C711 0.091(5) 0.125(5) 0.137(6) -0.054(5) -0.011(4) -0.014(4) C712 0.107(5) 0.153(6) 0.127(6) -0.060(5) -0.019(5) 0.026(5) C81N 0.075(5) 0.147(6) 0.118(7) -0.043(5) -0.017(5) -0.028(4) C82N 0.120(7) 0.343(14) 0.178(9) -0.138(10) -0.069(7) 0.025(8) C81 0.087(4) 0.100(4) 0.061(4) 0.006(3) -0.009(3) -0.040(4) C82 0.107(5) 0.108(4) 0.055(4) 0.004(3) -0.013(3) -0.033(4) C83 0.087(4) 0.068(3) 0.061(4) 0.002(3) -0.025(3) -0.022(3) C84 0.119(6) 0.091(4) 0.072(4) 0.002(3) -0.028(4) -0.035(4) C85 0.090(5) 0.097(4) 0.101(6) 0.003(4) -0.051(4) -0.019(4) C86 0.068(4) 0.088(4) 0.084(4) -0.011(3) -0.008(3) -0.023(3) C87 0.070(4) 0.051(3) 0.059(3) -0.011(2) -0.013(3) -0.009(2) C88 0.077(4) 0.053(3) 0.055(3) -0.007(2) -0.010(3) -0.016(3) C811 0.083(5) 0.200(8) 0.096(5) -0.010(5) 0.009(4) -0.025(5) C812 0.170(7) 0.126(5) 0.107(5) -0.004(4) -0.028(5) -0.080(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 Na1 O41 2.305(4) . ? Na1 O21 2.309(4) . ? Na1 O11 2.340(4) . ? Na1 O10 2.373(4) . ? Na1 N1 2.441(6) . ? Na1 C17 3.111(5) . ? Na1 C47 3.111(5) . ? Na1 Na2 3.201(3) . ? Na1 Na3 3.298(3) . ? Na1 Na4 3.342(3) . ? Na2 O31 2.255(4) . ? Na2 O41 2.283(4) . ? Na2 O21 2.360(4) . ? Na2 O20 2.379(4) . ? Na2 N2 2.556(7) . ? Na2 C27 3.114(6) . ? Na2 Na4 3.286(3) . ? Na2 Na3 3.342(3) . ? Na3 O11 2.270(4) . ? Na3 O21 2.312(4) . ? Na3 O30 2.392(4) . ? Na3 O31 2.399(4) . ? Na3 N3 2.487(7) . ? Na3 Na4 3.223(3) . ? Na4 O31 2.323(4) . ? Na4 O11 2.345(4) . ? Na4 O41 2.349(4) . ? Na4 O40 2.380(4) . ? Na4 N4 2.459(6) . ? Na4 C17 2.980(5) . ? Na4 C37 3.081(5) . ? Na4 C47 3.117(5) . ? Na5 O71 2.287(4) . ? Na5 O81 2.322(4) . ? Na5 O51 2.394(4) . ? Na5 N5 2.461(8) . ? Na5 O50 2.475(4) . ? Na5 Na6 3.258(3) . ? Na5 Na7 3.305(3) . ? Na5 Na8 3.342(3) . ? Na6 O61 2.338(3) . ? Na6 O51 2.340(4) . ? Na6 O71 2.352(4) . ? Na6 O60 2.380(4) . ? Na6 N6 2.465(6) . ? Na6 C77 2.937(6) . ? Na6 C57 3.087(6) . ? Na6 C67 3.109(5) . ? Na6 Na8 3.307(3) . ? Na6 Na7 3.329(3) . ? Na7 O61 2.284(4) . ? Na7 O81 2.305(4) . ? Na7 O70 2.331(4) . ? Na7 O71 2.355(4) . ? Na7 N7 2.449(6) . ? Na7 C78 3.087(6) . ? Na7 C77 3.097(5) . ? Na7 Na8 3.170(3) . ? Na8 O61 2.276(4) . ? Na8 O51 2.282(4) . ? Na8 O81 2.354(4) . ? Na8 O80 2.404(4) . ? Na8 N8 2.507(7) . ? Na8 C87 3.127(6) . ? O10 C18 1.390(6) . ? O10 C11 1.476(6) . ? O11 C17 1.317(5) . ? O20 C28 1.383(5) . ? O20 C21 1.466(6) . ? O21 C27 1.302(6) . ? O30 C38 1.375(6) . ? O30 C31 1.480(6) . ? O31 C37 1.322(6) . ? O40 C48 1.367(6) . ? O40 C41 1.483(7) . ? O41 C47 1.316(5) . ? O50 C58 1.375(6) . ? O50 C51 1.483(6) . ? O51 C57 1.306(6) . ? O60 C68 1.390(5) . ? O60 C61 1.483(6) . ? O61 C67 1.315(5) . ? O70 C78 1.374(6) . ? O70 C71 1.474(6) . ? O71 C77 1.326(6) . ? O80 C88 1.384(6) . ? O80 C81 1.461(6) . ? O81 C87 1.321(6) . ? N1 C11N 1.088(8) . ? N2 C21N 1.092(8) . ? N3 C31N 1.098(10) . ? N4 C41N 1.095(7) . ? N5 C51N 1.096(9) . ? N6 C61N 1.087(7) . ? N7 C71N 1.133(8) . ? N8 C81N 1.095(8) . ? C11N C12N 1.446(10) . ? C11 C111 1.479(9) . ? C11 C112 1.487(9) . ? C11 C12 1.533(9) . ? C12 C13 1.488(9) . ? C13 C18 1.365(7) . ? C13 C14 1.380(8) . ? C14 C15 1.359(8) . ? C15 C16 1.394(8) . ? C16 C17 1.390(7) . ? C17 C18 1.396(7) . ? C21N C22N 1.432(10) . ? C21 C211 1.487(8) . ? C21 C212 1.495(8) . ? C21 C22 1.524(8) . ? C22 C23 1.490(7) . ? C23 C28 1.369(7) . ? C23 C24 1.379(7) . ? C24 C25 1.359(8) . ? C25 C26 1.391(8) . ? C26 C27 1.400(7) . ? C27 C28 1.391(7) . ? C31N C32N 1.423(11) . ? C31 C312 1.484(8) . ? C31 C311 1.488(9) . ? C31 C32 1.506(8) . ? C32 C33 1.495(9) . ? C33 C38 1.369(7) . ? C33 C34 1.377(8) . ? C34 C35 1.373(9) . ? C35 C36 1.394(8) . ? C36 C37 1.389(7) . ? C37 C38 1.385(7) . ? C41N C42N 1.452(9) . ? C41 C411 1.464(9) . ? C41 C412 1.479(10) . ? C41 C42 1.539(10) . ? C42 C43 1.489(9) . ? C43 C48 1.356(7) . ? C43 C44 1.364(9) . ? C44 C45 1.353(9) . ? C45 C46 1.408(8) . ? C46 C47 1.385(6) . ? C47 C48 1.399(7) . ? C51N C52N 1.463(11) . ? C51 C511 1.486(9) . ? C51 C512 1.499(9) . ? C51 C52 1.524(9) . ? C52 C53 1.489(9) . ? C53 C58 1.369(8) . ? C53 C54 1.379(9) . ? C54 C55 1.368(10) . ? C55 C56 1.376(8) . ? C56 C57 1.386(7) . ? C57 C58 1.410(7) . ? C61N C62N 1.426(9) . ? C61 C612 1.482(8) . ? C61 C611 1.501(8) . ? C61 C62 1.525(8) . ? C62 C63 1.485(8) . ? C63 C65 1.373(7) . ? C63 C68 1.376(6) . ? C64 C66 1.387(7) . ? C64 C67 1.401(6) . ? C65 C66 1.354(8) . ? C67 C68 1.382(6) . ? C71N C72N 1.418(10) . ? C71 C72 1.511(9) . ? C71 C711 1.515(8) . ? C71 C712 1.514(9) . ? C72 C73 1.488(9) . ? C73 C78 1.373(7) . ? C73 C74 1.393(10) . ? C74 C75 1.388(11) . ? C75 C76 1.406(10) . ? C76 C77 1.397(7) . ? C77 C78 1.414(8) . ? C81N C82N 1.426(10) . ? C81 C812 1.499(8) . ? C81 C82 1.513(7) . ? C81 C811 1.516(8) . ? C82 C83 1.501(8) . ? C83 C88 1.364(7) . ? C83 C84 1.367(8) . ? C84 C85 1.373(8) . ? C85 C86 1.395(8) . ? C86 C87 1.400(7) . ? C87 C88 1.394(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O41 Na1 O21 92.68(14) . . ? O41 Na1 O11 89.13(13) . . ? O21 Na1 O11 87.94(13) . . ? O41 Na1 O10 106.94(15) . . ? O21 Na1 O10 152.14(15) . . ? O11 Na1 O10 73.13(13) . . ? O41 Na1 N1 116.7(2) . . ? O21 Na1 N1 92.95(19) . . ? O11 Na1 N1 154.1(2) . . ? O10 Na1 N1 95.5(2) . . ? O41 Na1 C17 95.10(13) . . ? O21 Na1 C17 109.59(14) . . ? O11 Na1 C17 22.81(12) . . ? O10 Na1 C17 50.35(14) . . ? N1 Na1 C17 140.3(2) . . ? O41 Na1 C47 22.38(11) . . ? O21 Na1 C47 113.12(14) . . ? O11 Na1 C47 98.56(14) . . ? O10 Na1 C47 90.25(14) . . ? N1 Na1 C47 104.8(2) . . ? C17 Na1 C47 95.97(14) . . ? O41 Na1 Na2 45.47(10) . . ? O21 Na1 Na2 47.37(10) . . ? O11 Na1 Na2 91.05(11) . . ? O10 Na1 Na2 149.44(13) . . ? N1 Na1 Na2 108.52(19) . . ? C17 Na1 Na2 110.81(12) . . ? C47 Na1 Na2 65.92(10) . . ? O41 Na1 Na3 89.80(11) . . ? O21 Na1 Na3 44.50(9) . . ? O11 Na1 Na3 43.48(9) . . ? O10 Na1 Na3 114.42(12) . . ? N1 Na1 Na3 132.58(18) . . ? C17 Na1 Na3 65.64(11) . . ? C47 Na1 Na3 110.60(11) . . ? Na2 Na1 Na3 61.87(6) . . ? O41 Na1 Na4 44.62(9) . . ? O21 Na1 Na4 89.02(10) . . ? O11 Na1 Na4 44.55(10) . . ? O10 Na1 Na4 91.32(12) . . ? N1 Na1 Na4 161.3(2) . . ? C17 Na1 Na4 54.86(10) . . ? C47 Na1 Na4 57.64(10) . . ? Na2 Na1 Na4 60.24(6) . . ? Na3 Na1 Na4 58.07(6) . . ? O31 Na2 O41 90.56(13) . . ? O31 Na2 O21 89.49(13) . . ? O41 Na2 O21 91.92(14) . . ? O31 Na2 O20 129.61(14) . . ? O41 Na2 O20 135.37(13) . . ? O21 Na2 O20 72.70(13) . . ? O31 Na2 N2 108.9(2) . . ? O41 Na2 N2 90.9(2) . . ? O21 Na2 N2 161.4(2) . . ? O20 Na2 N2 92.6(2) . . ? O31 Na2 C27 104.78(13) . . ? O41 Na2 C27 107.94(14) . . ? O21 Na2 C27 22.59(12) . . ? O20 Na2 C27 50.11(13) . . ? N2 Na2 C27 141.1(2) . . ? O31 Na2 Na1 93.15(11) . . ? O41 Na2 Na1 46.03(10) . . ? O21 Na2 Na1 46.06(10) . . ? O20 Na2 Na1 105.22(11) . . ? N2 Na2 Na1 132.43(19) . . ? C27 Na2 Na1 62.86(11) . . ? O31 Na2 Na4 44.97(10) . . ? O41 Na2 Na4 45.63(9) . . ? O21 Na2 Na4 89.54(11) . . ? O20 Na2 Na4 162.01(12) . . ? N2 Na2 Na4 105.42(19) . . ? C27 Na2 Na4 112.12(11) . . ? Na1 Na2 Na4 62.01(6) . . ? O31 Na2 Na3 45.85(10) . . ? O41 Na2 Na3 89.08(10) . . ? O21 Na2 Na3 43.76(9) . . ? O20 Na2 Na3 105.08(11) . . ? N2 Na2 Na3 154.70(18) . . ? C27 Na2 Na3 61.84(10) . . ? Na1 Na2 Na3 60.49(6) . . ? Na4 Na2 Na3 58.19(6) . . ? O11 Na3 O21 89.58(13) . . ? O11 Na3 O30 119.84(15) . . ? O21 Na3 O30 143.46(15) . . ? O11 Na3 O31 92.34(15) . . ? O21 Na3 O31 87.21(13) . . ? O30 Na3 O31 71.57(13) . . ? O11 Na3 N3 108.7(2) . . ? O21 Na3 N3 100.5(2) . . ? O30 Na3 N3 90.50(19) . . ? O31 Na3 N3 157.5(2) . . ? O11 Na3 Na4 46.66(11) . . ? O21 Na3 Na4 91.95(11) . . ? O30 Na3 Na4 93.82(12) . . ? O31 Na3 Na4 45.98(10) . . ? N3 Na3 Na4 152.7(2) . . ? O11 Na3 Na1 45.18(9) . . ? O21 Na3 Na1 44.44(9) . . ? O30 Na3 Na1 155.38(13) . . ? O31 Na3 Na1 88.18(11) . . ? N3 Na3 Na1 112.18(18) . . ? Na4 Na3 Na1 61.65(6) . . ? O11 Na3 Na2 88.79(10) . . ? O21 Na3 Na2 44.91(10) . . ? O30 Na3 Na2 109.87(12) . . ? O31 Na3 Na2 42.42(9) . . ? N3 Na3 Na2 142.2(2) . . ? Na4 Na3 Na2 60.03(6) . . ? Na1 Na3 Na2 57.65(6) . . ? O31 Na4 O11 92.39(14) . . ? O31 Na4 O41 87.30(13) . . ? O11 Na4 O41 87.96(13) . . ? O31 Na4 O40 143.34(16) . . ? O11 Na4 O40 116.45(17) . . ? O41 Na4 O40 72.57(13) . . ? O31 Na4 N4 100.80(19) . . ? O11 Na4 N4 105.70(19) . . ? O41 Na4 N4 163.6(2) . . ? O40 Na4 N4 93.0(2) . . ? O31 Na4 C17 115.93(15) . . ? O11 Na4 C17 25.21(12) . . ? O41 Na4 C17 97.68(15) . . ? O40 Na4 C17 97.28(16) . . ? N4 Na4 C17 91.6(2) . . ? O31 Na4 C37 23.34(12) . . ? O11 Na4 C37 103.54(16) . . ? O41 Na4 C37 107.93(14) . . ? O40 Na4 C37 139.92(18) . . ? N4 Na4 C37 78.05(19) . . ? C17 Na4 C37 121.66(16) . . ? O31 Na4 C47 106.99(14) . . ? O11 Na4 C47 98.29(14) . . ? O41 Na4 C47 22.76(12) . . ? O40 Na4 C47 49.82(14) . . ? N4 Na4 C47 142.2(2) . . ? C17 Na4 C47 98.60(15) . . ? C37 Na4 C47 124.22(14) . . ? O31 Na4 Na3 47.95(10) . . ? O11 Na4 Na3 44.75(10) . . ? O41 Na4 Na3 90.87(10) . . ? O40 Na4 Na3 156.63(14) . . ? N4 Na4 Na3 105.14(18) . . ? C17 Na4 Na3 68.06(12) . . ? C37 Na4 Na3 60.28(12) . . ? C47 Na4 Na3 112.44(12) . . ? O31 Na4 Na2 43.32(9) . . ? O11 Na4 Na2 88.90(11) . . ? O41 Na4 Na2 44.01(9) . . ? O40 Na4 Na2 111.33(12) . . ? N4 Na4 Na2 142.63(18) . . ? C17 Na4 Na2 111.99(12) . . ? C37 Na4 Na2 65.00(11) . . ? C47 Na4 Na2 64.83(11) . . ? Na3 Na4 Na2 61.78(6) . . ? O31 Na4 Na1 88.38(11) . . ? O11 Na4 Na1 44.43(9) . . ? O41 Na4 Na1 43.57(10) . . ? O40 Na4 Na1 96.75(13) . . ? N4 Na4 Na1 149.53(18) . . ? C17 Na4 Na1 58.63(11) . . ? C37 Na4 Na1 110.77(12) . . ? C47 Na4 Na1 57.46(11) . . ? Na3 Na4 Na1 60.27(6) . . ? Na2 Na4 Na1 57.76(6) . . ? O71 Na5 O81 89.59(13) . . ? O71 Na5 O51 91.81(15) . . ? O81 Na5 O51 87.73(13) . . ? O71 Na5 N5 108.1(2) . . ? O81 Na5 N5 102.0(2) . . ? O51 Na5 N5 157.7(2) . . ? O71 Na5 O50 123.51(15) . . ? O81 Na5 O50 139.64(15) . . ? O51 Na5 O50 70.50(14) . . ? N5 Na5 O50 89.70(19) . . ? O71 Na5 Na6 46.20(11) . . ? O81 Na5 Na6 91.71(11) . . ? O51 Na5 Na6 45.83(11) . . ? N5 Na5 Na6 151.3(2) . . ? O50 Na5 Na6 96.06(12) . . ? O71 Na5 Na7 45.45(9) . . ? O81 Na5 Na7 44.21(9) . . ? O51 Na5 Na7 87.68(11) . . ? N5 Na5 Na7 113.33(18) . . ? O50 Na5 Na7 156.22(14) . . ? Na6 Na5 Na7 60.95(6) . . ? O71 Na5 Na8 88.72(10) . . ? O81 Na5 Na8 44.77(10) . . ? O51 Na5 Na8 43.06(9) . . ? N5 Na5 Na8 143.7(2) . . ? O50 Na5 Na8 107.83(12) . . ? Na6 Na5 Na8 60.11(6) . . ? Na7 Na5 Na8 56.97(6) . . ? O61 Na6 O51 87.06(13) . . ? O61 Na6 O71 88.31(13) . . ? O51 Na6 O71 91.55(15) . . ? O61 Na6 O60 72.85(12) . . ? O51 Na6 O60 141.49(16) . . ? O71 Na6 O60 119.51(16) . . ? O61 Na6 N6 165.0(2) . . ? O51 Na6 N6 98.55(18) . . ? O71 Na6 N6 105.30(19) . . ? O60 Na6 N6 94.62(18) . . ? O61 Na6 C77 97.40(16) . . ? O51 Na6 C77 116.37(17) . . ? O71 Na6 C77 26.16(13) . . ? O60 Na6 C77 98.90(16) . . ? N6 Na6 C77 92.5(2) . . ? O61 Na6 C57 107.02(15) . . ? O51 Na6 C57 23.01(12) . . ? O71 Na6 C57 103.16(16) . . ? O60 Na6 C57 137.17(17) . . ? N6 Na6 C57 76.38(18) . . ? C77 Na6 C57 122.95(18) . . ? O61 Na6 C67 22.79(12) . . ? O51 Na6 C67 105.99(14) . . ? O71 Na6 C67 100.19(13) . . ? O60 Na6 C67 50.06(12) . . ? N6 Na6 C67 143.87(19) . . ? C77 Na6 C67 99.62(15) . . ? C57 Na6 C67 122.10(15) . . ? O61 Na6 Na5 90.32(11) . . ? O51 Na6 Na5 47.20(11) . . ? O71 Na6 Na5 44.57(10) . . ? O60 Na6 Na5 158.37(12) . . ? N6 Na6 Na5 103.70(17) . . ? C77 Na6 Na5 69.25(13) . . ? C57 Na6 Na5 60.12(13) . . ? C67 Na6 Na5 112.43(12) . . ? O61 Na6 Na8 43.47(9) . . ? O51 Na6 Na8 43.63(9) . . ? O71 Na6 Na8 88.50(11) . . ? O60 Na6 Na8 110.36(11) . . ? N6 Na6 Na8 140.83(17) . . ? C77 Na6 Na8 111.90(13) . . ? C57 Na6 Na8 64.73(11) . . ? C67 Na6 Na8 63.78(10) . . ? Na5 Na6 Na8 61.20(6) . . ? O61 Na6 Na7 43.29(10) . . ? O51 Na6 Na7 87.99(11) . . ? O71 Na6 Na7 45.04(9) . . ? O60 Na6 Na7 98.24(11) . . ? N6 Na6 Na7 150.04(18) . . ? C77 Na6 Na7 58.85(12) . . ? C57 Na6 Na7 110.31(12) . . ? C67 Na6 Na7 58.31(10) . . ? Na5 Na6 Na7 60.22(6) . . ? Na8 Na6 Na7 57.08(6) . . ? O61 Na7 O81 93.43(14) . . ? O61 Na7 O70 105.61(15) . . ? O81 Na7 O70 153.95(15) . . ? O61 Na7 O71 89.50(13) . . ? O81 Na7 O71 88.33(13) . . ? O70 Na7 O71 74.49(14) . . ? O61 Na7 N7 115.3(2) . . ? O81 Na7 N7 92.90(18) . . ? O70 Na7 N7 94.74(19) . . ? O71 Na7 N7 155.0(2) . . ? O61 Na7 C78 100.14(14) . . ? O81 Na7 C78 135.37(16) . . ? O70 Na7 C78 24.71(14) . . ? O71 Na7 C78 49.89(15) . . ? N7 Na7 C78 118.1(2) . . ? O61 Na7 C77 94.26(13) . . ? O81 Na7 C77 110.93(16) . . ? O70 Na7 C77 51.11(16) . . ? O71 Na7 C77 23.47(14) . . ? N7 Na7 C77 141.0(2) . . ? C78 Na7 C77 26.44(15) . . ? O61 Na7 Na8 45.84(10) . . ? O81 Na7 Na8 47.77(10) . . ? O70 Na7 Na8 149.29(14) . . ? O71 Na7 Na8 91.76(11) . . ? N7 Na7 Na8 107.47(18) . . ? C78 Na7 Na8 132.74(14) . . ? C77 Na7 Na8 111.39(13) . . ? O61 Na7 Na5 90.10(11) . . ? O81 Na7 Na5 44.62(9) . . ? O70 Na7 Na5 116.39(12) . . ? O71 Na7 Na5 43.78(10) . . ? N7 Na7 Na5 133.25(17) . . ? C78 Na7 Na5 92.72(14) . . ? C77 Na7 Na5 66.84(14) . . ? Na8 Na7 Na5 62.10(6) . . ? O61 Na7 Na6 44.57(9) . . ? O81 Na7 Na6 90.23(11) . . ? O70 Na7 Na6 91.08(13) . . ? O71 Na7 Na6 44.95(10) . . ? N7 Na7 Na6 159.84(19) . . ? C78 Na7 Na6 71.67(13) . . ? C77 Na7 Na6 54.25(11) . . ? Na8 Na7 Na6 61.10(6) . . ? Na5 Na7 Na6 58.83(6) . . ? O61 Na8 O51 89.98(14) . . ? O61 Na8 O81 92.36(14) . . ? O51 Na8 O81 89.63(14) . . ? O61 Na8 O80 129.41(13) . . ? O51 Na8 O80 136.30(15) . . ? O81 Na8 O80 72.88(13) . . ? O61 Na8 N8 89.2(2) . . ? O51 Na8 N8 111.5(2) . . ? O81 Na8 N8 158.8(2) . . ? O80 Na8 N8 89.9(2) . . ? O61 Na8 C87 106.39(14) . . ? O51 Na8 C87 107.10(14) . . ? O81 Na8 C87 22.75(12) . . ? O80 Na8 C87 50.14(13) . . ? N8 Na8 C87 138.2(2) . . ? O61 Na8 Na7 46.06(10) . . ? O51 Na8 Na7 92.98(12) . . ? O81 Na8 Na7 46.47(9) . . ? O80 Na8 Na7 101.92(11) . . ? N8 Na8 Na7 129.69(18) . . ? C87 Na8 Na7 61.61(10) . . ? O61 Na8 Na6 44.97(9) . . ? O51 Na8 Na6 45.04(10) . . ? O81 Na8 Na6 89.94(11) . . ? O80 Na8 Na6 162.29(12) . . ? N8 Na8 Na6 105.8(2) . . ? C87 Na8 Na6 112.56(12) . . ? Na7 Na8 Na6 61.81(7) . . ? O61 Na8 Na5 89.32(11) . . ? O51 Na8 Na5 45.74(11) . . ? O81 Na8 Na5 43.99(9) . . ? O80 Na8 Na5 108.45(11) . . ? N8 Na8 Na5 157.2(2) . . ? C87 Na8 Na5 63.54(10) . . ? Na7 Na8 Na5 60.92(6) . . ? Na6 Na8 Na5 58.69(6) . . ? C18 O10 C11 107.6(4) . . ? C18 O10 Na1 110.3(3) . . ? C11 O10 Na1 141.6(3) . . ? C17 O11 Na3 150.6(3) . . ? C17 O11 Na1 113.6(3) . . ? Na3 O11 Na1 91.34(13) . . ? C17 O11 Na4 105.5(3) . . ? Na3 O11 Na4 88.59(14) . . ? Na1 O11 Na4 91.02(13) . . ? C28 O20 C21 106.8(4) . . ? C28 O20 Na2 110.3(3) . . ? C21 O20 Na2 140.2(3) . . ? C27 O21 Na1 129.5(3) . . ? C27 O21 Na3 131.6(3) . . ? Na1 O21 Na3 91.06(13) . . ? C27 O21 Na2 113.3(3) . . ? Na1 O21 Na2 86.57(14) . . ? Na3 O21 Na2 91.33(14) . . ? C38 O30 C31 107.1(4) . . ? C38 O30 Na3 111.4(3) . . ? C31 O30 Na3 141.2(3) . . ? C37 O31 Na2 145.3(3) . . ? C37 O31 Na4 112.5(3) . . ? Na2 O31 Na4 91.70(13) . . ? C37 O31 Na3 113.5(3) . . ? Na2 O31 Na3 91.72(14) . . ? Na4 O31 Na3 86.07(14) . . ? C48 O40 C41 107.8(5) . . ? C48 O40 Na4 111.0(3) . . ? C41 O40 Na4 140.5(4) . . ? C47 O41 Na2 144.0(3) . . ? C47 O41 Na1 115.8(3) . . ? Na2 O41 Na1 88.51(14) . . ? C47 O41 Na4 113.6(3) . . ? Na2 O41 Na4 90.36(13) . . ? Na1 O41 Na4 91.81(13) . . ? C58 O50 C51 107.6(4) . . ? C58 O50 Na5 110.5(3) . . ? C51 O50 Na5 141.3(4) . . ? C57 O51 Na8 144.1(4) . . ? C57 O51 Na6 112.5(3) . . ? Na8 O51 Na6 91.33(13) . . ? C57 O51 Na5 115.4(3) . . ? Na8 O51 Na5 91.21(14) . . ? Na6 O51 Na5 86.97(15) . . ? C68 O60 C61 107.3(4) . . ? C68 O60 Na6 110.2(3) . . ? C61 O60 Na6 142.3(3) . . ? C67 O61 Na8 140.4(3) . . ? C67 O61 Na7 119.1(3) . . ? Na8 O61 Na7 88.10(14) . . ? C67 O61 Na6 113.7(3) . . ? Na8 O61 Na6 91.56(13) . . ? Na7 O61 Na6 92.14(13) . . ? C78 O70 C71 107.8(4) . . ? C78 O70 Na7 110.1(3) . . ? C71 O70 Na7 140.6(4) . . ? C77 O71 Na5 154.6(3) . . ? C77 O71 Na6 102.4(3) . . ? Na5 O71 Na6 89.23(15) . . ? C77 O71 Na7 111.5(3) . . ? Na5 O71 Na7 90.77(14) . . ? Na6 O71 Na7 90.01(13) . . ? C88 O80 C81 106.8(4) . . ? C88 O80 Na8 109.5(3) . . ? C81 O80 Na8 141.0(3) . . ? C87 O81 Na7 123.3(3) . . ? C87 O81 Na5 137.3(3) . . ? Na7 O81 Na5 91.17(14) . . ? C87 O81 Na8 113.7(3) . . ? Na7 O81 Na8 85.75(14) . . ? Na5 O81 Na8 91.24(14) . . ? C11N N1 Na1 144.6(7) . . ? C21N N2 Na2 113.0(7) . . ? C31N N3 Na3 155.0(9) . . ? C41N N4 Na4 155.5(6) . . ? C51N N5 Na5 163.7(9) . . ? C61N N6 Na6 159.5(6) . . ? C71N N7 Na7 151.0(6) . . ? C81N N8 Na8 121.4(7) . . ? N1 C11N C12N 178.5(9) . . ? O10 C11 C111 106.6(5) . . ? O10 C11 C112 106.5(5) . . ? C111 C11 C112 109.5(7) . . ? O10 C11 C12 105.7(5) . . ? C111 C11 C12 115.1(7) . . ? C112 C11 C12 112.7(6) . . ? C13 C12 C11 104.0(5) . . ? C18 C13 C14 118.9(6) . . ? C18 C13 C12 108.9(6) . . ? C14 C13 C12 132.2(6) . . ? C15 C14 C13 118.3(6) . . ? C14 C15 C16 121.9(6) . . ? C17 C16 C15 121.8(6) . . ? O11 C17 C16 124.8(5) . . ? O11 C17 C18 121.7(5) . . ? C16 C17 C18 113.5(5) . . ? O11 C17 Na4 49.3(2) . . ? C16 C17 Na4 105.2(3) . . ? C18 C17 Na4 117.1(3) . . ? O11 C17 Na1 43.6(2) . . ? C16 C17 Na1 168.2(4) . . ? C18 C17 Na1 78.2(3) . . ? Na4 C17 Na1 66.52(12) . . ? C13 C18 O10 113.3(5) . . ? C13 C18 C17 125.6(5) . . ? O10 C18 C17 121.1(4) . . ? N2 C21N C22N 175.5(10) . . ? O20 C21 C211 107.5(5) . . ? O20 C21 C212 105.2(5) . . ? C211 C21 C212 113.7(6) . . ? O20 C21 C22 104.9(4) . . ? C211 C21 C22 113.7(6) . . ? C212 C21 C22 111.1(5) . . ? C23 C22 C21 103.4(5) . . ? C28 C23 C24 119.9(5) . . ? C28 C23 C22 107.8(5) . . ? C24 C23 C22 132.4(5) . . ? C25 C24 C23 117.4(5) . . ? C24 C25 C26 122.0(6) . . ? C25 C26 C27 122.5(6) . . ? O21 C27 C28 122.3(5) . . ? O21 C27 C26 125.0(5) . . ? C28 C27 C26 112.7(5) . . ? O21 C27 Na2 44.1(2) . . ? C28 C27 Na2 78.2(3) . . ? C26 C27 Na2 169.1(4) . . ? C23 C28 O20 113.1(5) . . ? C23 C28 C27 125.5(5) . . ? O20 C28 C27 121.4(4) . . ? N3 C31N C32N 176.5(12) . . ? O30 C31 C312 106.0(4) . . ? O30 C31 C311 105.6(5) . . ? C312 C31 C311 112.4(6) . . ? O30 C31 C32 106.6(5) . . ? C312 C31 C32 112.7(6) . . ? C311 C31 C32 112.8(6) . . ? C33 C32 C31 104.1(5) . . ? C38 C33 C34 120.9(6) . . ? C38 C33 C32 108.2(6) . . ? C34 C33 C32 130.9(6) . . ? C35 C34 C33 116.7(6) . . ? C34 C35 C36 122.1(6) . . ? C37 C36 C35 121.7(6) . . ? O31 C37 C38 121.2(5) . . ? O31 C37 C36 124.3(5) . . ? C38 C37 C36 114.5(5) . . ? O31 C37 Na4 44.2(2) . . ? C38 C37 Na4 115.7(4) . . ? C36 C37 Na4 108.2(4) . . ? C33 C38 O30 113.7(5) . . ? C33 C38 C37 124.2(6) . . ? O30 C38 C37 122.1(5) . . ? N4 C41N C42N 176.3(8) . . ? C411 C41 C412 112.3(7) . . ? C411 C41 O40 106.3(6) . . ? C412 C41 O40 106.2(6) . . ? C411 C41 C42 114.4(8) . . ? C412 C41 C42 112.4(7) . . ? O40 C41 C42 104.4(6) . . ? C43 C42 C41 104.8(6) . . ? C48 C43 C44 121.1(7) . . ? C48 C43 C42 107.7(6) . . ? C44 C43 C42 131.2(7) . . ? C45 C44 C43 117.3(6) . . ? C44 C45 C46 122.1(6) . . ? C47 C46 C45 121.2(6) . . ? O41 C47 C46 124.2(5) . . ? O41 C47 C48 121.7(4) . . ? C46 C47 C48 114.1(5) . . ? O41 C47 Na1 41.8(2) . . ? C46 C47 Na1 105.6(3) . . ? C48 C47 Na1 122.7(3) . . ? O41 C47 Na4 43.7(2) . . ? C46 C47 Na4 167.8(4) . . ? C48 C47 Na4 78.0(3) . . ? Na1 C47 Na4 64.90(11) . . ? C43 C48 O40 114.8(5) . . ? C43 C48 C47 124.1(6) . . ? O40 C48 C47 121.2(4) . . ? N5 C51N C52N 175.8(11) . . ? O50 C51 C511 106.8(5) . . ? O50 C51 C512 105.7(5) . . ? C511 C51 C512 113.0(7) . . ? O50 C51 C52 105.6(5) . . ? C511 C51 C52 112.7(6) . . ? C512 C51 C52 112.4(6) . . ? C53 C52 C51 104.7(5) . . ? C58 C53 C54 119.7(7) . . ? C58 C53 C52 108.0(6) . . ? C54 C53 C52 132.2(7) . . ? C55 C54 C53 117.6(7) . . ? C54 C55 C56 122.0(7) . . ? C55 C56 C57 122.9(6) . . ? O51 C57 C56 125.2(5) . . ? O51 C57 C58 121.6(5) . . ? C56 C57 C58 113.2(5) . . ? O51 C57 Na6 44.4(2) . . ? C56 C57 Na6 105.3(4) . . ? C58 C57 Na6 120.9(4) . . ? C53 C58 O50 114.0(6) . . ? C53 C58 C57 124.6(7) . . ? O50 C58 C57 121.4(5) . . ? N6 C61N C62N 179.0(9) . . ? C612 C61 O60 105.9(5) . . ? C612 C61 C611 112.0(6) . . ? O60 C61 C611 105.2(5) . . ? C612 C61 C62 115.0(6) . . ? O60 C61 C62 105.9(4) . . ? C611 C61 C62 111.9(6) . . ? C63 C62 C61 104.6(5) . . ? C65 C63 C68 119.3(5) . . ? C65 C63 C62 132.1(5) . . ? C68 C63 C62 108.6(5) . . ? C66 C64 C67 121.7(5) . . ? C66 C65 C63 117.5(5) . . ? C65 C66 C64 122.7(5) . . ? O61 C67 C68 122.2(4) . . ? O61 C67 C64 124.7(5) . . ? C68 C67 C64 113.1(4) . . ? O61 C67 Na6 43.5(2) . . ? C68 C67 Na6 78.6(3) . . ? C64 C67 Na6 168.3(4) . . ? C63 C68 C67 125.7(4) . . ? C63 C68 O60 113.2(4) . . ? C67 C68 O60 121.1(4) . . ? N7 C71N C72N 179.1(8) . . ? O70 C71 C72 106.4(5) . . ? O70 C71 C711 105.8(4) . . ? C72 C71 C711 112.6(6) . . ? O70 C71 C712 106.4(5) . . ? C72 C71 C712 113.4(6) . . ? C711 C71 C712 111.6(6) . . ? C73 C72 C71 102.8(5) . . ? C78 C73 C74 117.3(7) . . ? C78 C73 C72 109.8(6) . . ? C74 C73 C72 132.8(7) . . ? C75 C74 C73 119.2(7) . . ? C74 C75 C76 122.2(7) . . ? C77 C76 C75 120.1(7) . . ? O71 C77 C76 123.6(6) . . ? O71 C77 C78 121.3(5) . . ? C76 C77 C78 115.1(6) . . ? O71 C77 Na6 51.4(2) . . ? C76 C77 Na6 104.8(4) . . ? C78 C77 Na6 115.0(3) . . ? O71 C77 Na7 45.0(2) . . ? C76 C77 Na7 168.4(5) . . ? C78 C77 Na7 76.4(3) . . ? Na6 C77 Na7 66.90(12) . . ? C73 C78 O70 111.7(6) . . ? C73 C78 C77 126.1(6) . . ? O70 C78 C77 122.2(5) . . ? C73 C78 Na7 156.6(5) . . ? O70 C78 Na7 45.1(2) . . ? C77 C78 Na7 77.2(3) . . ? N8 C81N C82N 176.7(11) . . ? O80 C81 C812 106.5(5) . . ? O80 C81 C82 105.2(4) . . ? C812 C81 C82 111.5(5) . . ? O80 C81 C811 107.2(5) . . ? C812 C81 C811 112.4(5) . . ? C82 C81 C811 113.4(5) . . ? C83 C82 C81 102.8(5) . . ? C88 C83 C84 120.1(6) . . ? C88 C83 C82 107.8(5) . . ? C84 C83 C82 132.1(5) . . ? C83 C84 C85 118.3(6) . . ? C84 C85 C86 120.9(6) . . ? C85 C86 C87 122.3(5) . . ? O81 C87 C88 121.6(5) . . ? O81 C87 C86 124.9(5) . . ? C88 C87 C86 113.5(5) . . ? O81 C87 Na8 43.6(2) . . ? C88 C87 Na8 78.0(3) . . ? C86 C87 Na8 168.4(4) . . ? C83 C88 O80 112.7(5) . . ? C83 C88 C87 124.9(6) . . ? O80 C88 C87 122.4(5) . . ? _diffrn_measured_fraction_theta_max 0.351 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.351 _refine_diff_density_max 0.112 _refine_diff_density_min -0.113 _refine_diff_density_rms 0.024 data_COMPOUND_3 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C15 H16 Cl N O2 Zn' _chemical_formula_weight 343.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.855(4) _cell_length_b 8.836(5) _cell_length_c 18.068(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.99(4) _cell_angle_gamma 90.00 _cell_volume 1549.5(12) _cell_formula_units_Z 4 _cell_measurement_temperature 299(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 14 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 1.757 _exptl_absorpt_correction_type 'Absorb procedure' _exptl_absorpt_correction_T_min 0.759 _exptl_absorpt_correction_T_max 1.358 _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Kuma KM4 automatic diffractometer' _diffrn_measurement_method 'profile data from omega-2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.1 _diffrn_reflns_number 2650 _diffrn_reflns_av_R_equivalents 0.0111 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.51 _reflns_number_total 2505 _reflns_number_gt 1928 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kuma KM4 (Kuma, 1996)' _computing_cell_refinement 'Kuma KM4 (Kuma, 1996)' _computing_data_reduction 'Kuma KM4 (Kuma, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'OrtepII, 1976' _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 w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+0.4011P] 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 2505 _refine_ls_number_parameters 183 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0809 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.206 _refine_ls_shift/su_mean 0.011 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn 0.15550(3) 0.02827(4) 0.015084(19) 0.04176(12) Uani 1 d . . . Cl Cl 0.31872(9) -0.13908(11) 0.04150(5) 0.0711(3) Uani 1 d . . . O10 O 0.22709(19) 0.2005(2) 0.14250(11) 0.0476(5) Uani 1 d . . . O11 O -0.00324(19) 0.0476(2) 0.06654(11) 0.0482(5) Uani 1 d . . . N N 0.2047(2) 0.2226(3) -0.03217(13) 0.0435(5) Uani 1 d . . . C1 C 0.3152(3) 0.3151(4) 0.18799(19) 0.0560(8) Uani 1 d . . . C2 C 0.2483(4) 0.3413(4) 0.25662(19) 0.0621(9) Uani 1 d . . . H2A H 0.2958 0.2857 0.2997 0.075 Uiso 1 calc R . . H2B H 0.2476 0.4480 0.2692 0.075 Uiso 1 calc R . . C3 C 0.1030(3) 0.2819(3) 0.23186(16) 0.0461(7) Uani 1 d . . . C4 C -0.0149(3) 0.2880(4) 0.26355(17) 0.0539(8) Uani 1 d . . . H4 H -0.0170 0.3422 0.3074 0.065 Uiso 1 calc R . . C5 C -0.1291(3) 0.2111(4) 0.22788(18) 0.0579(8) Uani 1 d . . . H5 H -0.2096 0.2140 0.2482 0.069 Uiso 1 calc R . . C6 C -0.1278(3) 0.1298(4) 0.16287(18) 0.0516(7) Uani 1 d . . . H6 H -0.2069 0.0787 0.1406 0.062 Uiso 1 calc R . . C7 C -0.0106(3) 0.1227(3) 0.13000(16) 0.0413(6) Uani 1 d . . . C8 C 0.1036(3) 0.2011(3) 0.16771(15) 0.0391(6) Uani 1 d . . . C9 C 0.3066(5) 0.4561(4) 0.1396(2) 0.0864(14) Uani 1 d . . . H9A H 0.3626 0.5344 0.1662 0.104 Uiso 1 calc R . . H9B H 0.2127 0.4898 0.1282 0.104 Uiso 1 calc R . . H9C H 0.3392 0.4335 0.0937 0.104 Uiso 1 calc R . . C10 C 0.4578(4) 0.2506(6) 0.2048(3) 0.1046(17) Uani 1 d . . . H10A H 0.4574 0.1603 0.2343 0.125 Uiso 1 calc R . . H10B H 0.5191 0.3235 0.2323 0.125 Uiso 1 calc R . . H10C H 0.4885 0.2268 0.1585 0.125 Uiso 1 calc R . . C11 C 0.1107(3) 0.3282(4) -0.0543(2) 0.0663(10) Uani 1 d . . . H11 H 0.0195 0.3093 -0.0500 0.080 Uiso 1 calc R . . C12 C 0.1438(5) 0.4650(5) -0.0834(3) 0.0871(13) Uani 1 d . . . H12 H 0.0762 0.5375 -0.0984 0.105 Uiso 1 calc R . . C13 C 0.2772(5) 0.4918(5) -0.0897(2) 0.0827(13) Uani 1 d . . . H13 H 0.3022 0.5842 -0.1080 0.099 Uiso 1 calc R . . C14 C 0.3740(4) 0.3828(4) -0.0690(2) 0.0699(10) Uani 1 d . . . H14 H 0.4652 0.3984 -0.0742 0.084 Uiso 1 calc R . . C15 C 0.3340(3) 0.2498(4) -0.04045(19) 0.0525(7) Uani 1 d . . . H15 H 0.4001 0.1753 -0.0262 0.063 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 Zn 0.03203(17) 0.04134(19) 0.0514(2) 0.00296(16) 0.00576(13) -0.00381(14) Cl 0.0633(5) 0.0750(6) 0.0734(6) 0.0108(5) 0.0073(4) 0.0274(4) O10 0.0439(10) 0.0490(12) 0.0511(12) -0.0096(10) 0.0114(9) -0.0119(9) O11 0.0355(10) 0.0562(13) 0.0534(12) -0.0139(10) 0.0096(8) -0.0081(9) N 0.0403(12) 0.0415(13) 0.0488(14) 0.0015(11) 0.0080(10) -0.0042(10) C1 0.0497(17) 0.0560(19) 0.062(2) -0.0126(16) 0.0082(14) -0.0195(15) C2 0.0655(19) 0.067(2) 0.0524(19) -0.0121(16) 0.0056(15) -0.0195(17) C3 0.0523(16) 0.0459(17) 0.0390(15) 0.0023(13) 0.0048(12) -0.0022(13) C4 0.065(2) 0.059(2) 0.0393(16) -0.0014(14) 0.0138(14) 0.0064(16) C5 0.0481(17) 0.081(2) 0.0484(18) 0.0062(17) 0.0180(14) 0.0065(16) C6 0.0376(14) 0.065(2) 0.0515(18) 0.0025(15) 0.0062(13) -0.0033(14) C7 0.0390(14) 0.0409(16) 0.0434(16) 0.0043(12) 0.0055(12) 0.0011(12) C8 0.0395(14) 0.0373(14) 0.0403(15) 0.0037(12) 0.0063(11) 0.0010(11) C9 0.128(4) 0.065(3) 0.073(3) -0.014(2) 0.036(3) -0.049(3) C10 0.052(2) 0.128(4) 0.127(4) -0.042(3) -0.002(2) -0.012(2) C11 0.0494(18) 0.062(2) 0.085(3) 0.0183(19) 0.0035(17) 0.0034(16) C12 0.080(3) 0.067(3) 0.110(3) 0.037(2) 0.003(2) 0.011(2) C13 0.104(3) 0.066(3) 0.083(3) 0.025(2) 0.029(2) -0.014(2) C14 0.071(2) 0.064(2) 0.080(2) 0.010(2) 0.0307(19) -0.0139(19) C15 0.0480(16) 0.0498(18) 0.0627(19) 0.0006(15) 0.0179(14) -0.0045(14) _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 Zn O11 1.961(2) . ? Zn N 2.014(2) . ? Zn O11 2.027(2) 3 ? Zn Cl 2.1761(12) . ? Zn Zn 3.0595(14) 3 ? O10 C8 1.372(3) . ? O10 C1 1.485(3) . ? O11 C7 1.338(3) . ? O11 Zn 2.027(2) 3 ? N C11 1.326(4) . ? N C15 1.331(4) . ? C1 C10 1.498(5) . ? C1 C9 1.517(5) . ? C1 C2 1.520(5) . ? C2 C3 1.518(4) . ? C3 C8 1.362(4) . ? C3 C4 1.383(4) . ? C4 C5 1.375(5) . ? C5 C6 1.379(5) . ? C6 C7 1.389(4) . ? C7 C8 1.394(4) . ? C11 C12 1.380(5) . ? C12 C13 1.360(6) . ? C13 C14 1.361(6) . ? C14 C15 1.368(5) . ? 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 O11 Zn N 113.40(9) . . ? O11 Zn O11 79.81(9) . 3 ? N Zn O11 100.12(9) . 3 ? O11 Zn Cl 125.13(7) . . ? N Zn Cl 116.70(8) . . ? O11 Zn Cl 111.13(7) 3 . ? O11 Zn Zn 40.69(6) . 3 ? N Zn Zn 111.78(7) . 3 ? O11 Zn Zn 39.11(6) 3 3 ? Cl Zn Zn 127.42(4) . 3 ? C8 O10 C1 106.3(2) . . ? C7 O11 Zn 128.01(17) . . ? C7 O11 Zn 130.14(17) . 3 ? Zn O11 Zn 100.19(9) . 3 ? C11 N C15 118.1(3) . . ? C11 N Zn 121.4(2) . . ? C15 N Zn 120.5(2) . . ? O10 C1 C10 106.9(3) . . ? O10 C1 C9 105.8(3) . . ? C10 C1 C9 112.6(3) . . ? O10 C1 C2 105.1(2) . . ? C10 C1 C2 114.7(3) . . ? C9 C1 C2 110.9(3) . . ? C3 C2 C1 103.1(3) . . ? C8 C3 C4 120.0(3) . . ? C8 C3 C2 106.8(3) . . ? C4 C3 C2 133.0(3) . . ? C5 C4 C3 117.7(3) . . ? C4 C5 C6 121.9(3) . . ? C5 C6 C7 121.3(3) . . ? O11 C7 C6 124.2(3) . . ? O11 C7 C8 120.4(2) . . ? C6 C7 C8 115.4(3) . . ? C3 C8 O10 114.8(2) . . ? C3 C8 C7 123.7(3) . . ? O10 C8 C7 121.5(2) . . ? N C11 C12 122.1(3) . . ? C13 C12 C11 118.7(4) . . ? C12 C13 C14 119.7(4) . . ? C13 C14 C15 118.5(4) . . ? N C15 C14 122.8(3) . . ? _diffrn_measured_fraction_theta_max 0.813 _diffrn_reflns_theta_full 25.51 _diffrn_measured_fraction_theta_full 0.813 _refine_diff_density_max 0.321 _refine_diff_density_min -0.423 _refine_diff_density_rms 0.053